# Electronic Supplementary Material (ESI) for Chemical Communications # 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_KIR1045 _audit_creation_date 2013-08-27T17:55:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H80 In2 N4 O2 S4' _chemical_formula_sum 'C54 H84 In2 N4 O2 Si4' _chemical_formula_weight 1163.25 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.335(3) _cell_length_b 14.576(4) _cell_length_c 20.959(6) _cell_angle_alpha 95.297(13) _cell_angle_beta 99.709(11) _cell_angle_gamma 95.859(12) _cell_volume 3076.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5021 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.01 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_unetI/netI 0.0609 _diffrn_reflns_number 34709 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.62 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 13984 _reflns_number_gt 9503 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0371P)^2^+1.0084P] 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_number_reflns 13984 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.458 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 In1 In -0.01037(2) 0.207946(16) 0.498810(11) 0.03813(8) Uani 1 1 d . . . Si1 Si -0.34169(9) 0.18070(8) 0.48251(5) 0.0494(3) Uani 1 1 d . . . Si2 Si 0.19921(10) 0.15289(8) 0.63355(5) 0.0500(3) Uani 1 1 d . . . O1 O 0.0223(2) 0.34284(16) 0.54808(11) 0.0464(6) Uani 1 1 d . . . C2 C 0.1267(3) 0.4042(2) 0.55813(15) 0.0372(7) Uani 1 1 d . . . C3 C 0.1407(3) 0.4813(2) 0.60757(15) 0.0398(8) Uani 1 1 d . . . C4 C 0.2547(4) 0.5422(3) 0.62035(18) 0.0540(10) Uani 1 1 d . . . H4 H 0.2636 0.5925 0.6536 0.065 Uiso 1 1 calc R . . C5 C 0.3579(4) 0.5325(3) 0.58603(19) 0.0593(10) Uani 1 1 d . . . H5 H 0.4374 0.574 0.5971 0.071 Uiso 1 1 calc R . . C6 C 0.3427(3) 0.4621(3) 0.53593(17) 0.0498(9) Uani 1 1 d . . . H6 H 0.4117 0.4568 0.5115 0.06 Uiso 1 1 calc R . . C7 C 0.2286(3) 0.3978(2) 0.51983(15) 0.0372(7) Uani 1 1 d . . . C8 C 0.2215(3) 0.3321(2) 0.46265(16) 0.0385(8) Uani 1 1 d . . . H8 H 0.2896 0.3436 0.4381 0.046 Uiso 1 1 calc R . . N9 N 0.1371(2) 0.26071(18) 0.44004(12) 0.0357(6) Uani 1 1 d . . . C10 C 0.1475(3) 0.2096(2) 0.37683(16) 0.0399(8) Uani 1 1 d . . . H10 H 0.2368 0.229 0.3667 0.048 Uiso 1 1 calc R . . C11 C 0.1329(3) 0.1060(2) 0.37944(17) 0.0454(8) Uani 1 1 d . . . H11A H 0.0466 0.0861 0.3915 0.054 Uiso 1 1 calc R . . H11B H 0.2034 0.0902 0.4134 0.054 Uiso 1 1 calc R . . C12 C 0.1414(4) 0.0544(3) 0.31466(19) 0.0575(10) Uani 1 1 d . . . H12A H 0.23 0.0712 0.3041 0.069 Uiso 1 1 calc R . . H12B H 0.1303 -0.0132 0.3178 0.069 Uiso 1 1 calc R . . N13 N 0.0399(3) 0.0764(2) 0.26221(14) 0.0498(7) Uani 1 1 d . . . C14 C 0.0527(4) 0.1760(3) 0.25796(17) 0.0502(9) Uani 1 1 d . . . H14A H -0.0176 0.1899 0.2232 0.06 Uiso 1 1 calc R . . H14B H 0.1391 0.1955 0.2458 0.06 Uiso 1 1 calc R . . C15 C 0.0430(3) 0.2318(2) 0.32174(15) 0.0427(8) Uani 1 1 d . . . H15A H -0.0461 0.2167 0.3323 0.051 Uiso 1 1 calc R . . H15B H 0.0557 0.2989 0.317 0.051 Uiso 1 1 calc R . . C16 C 0.0499(4) 0.0226(3) 0.2007(2) 0.0736(13) Uani 1 1 d . . . H16A H 0.0606 -0.0421 0.2091 0.088 Uiso 1 1 calc R . . H16B H 0.1306 0.0485 0.1858 0.088 Uiso 1 1 calc R . . C17 C -0.0662(5) 0.0214(3) 0.1467(2) 0.0641(11) Uani 1 1 d . . . C18 C -0.1908(6) -0.0122(5) 0.1527(3) 0.109(2) Uani 1 1 d . . . H18 H -0.206 -0.0316 0.1931 0.131 Uiso 1 1 calc R . . C19 C -0.2959(7) -0.0189(6) 0.1013(4) 0.140(3) Uani 1 1 d . . . H19 H -0.3816 -0.0443 0.1062 0.168 Uiso 1 1 calc R . . C20 C -0.2760(9) 0.0114(6) 0.0433(4) 0.142(3) Uani 1 1 d . . . H20 H -0.3476 0.0091 0.008 0.17 Uiso 1 1 calc R . . C21 C -0.1521(10) 0.0446(6) 0.0376(3) 0.151(3) Uani 1 1 d . . . H21 H -0.1359 0.0651 -0.0023 0.181 Uiso 1 1 calc R . . C22 C -0.0504(6) 0.0489(4) 0.0886(3) 0.1049(18) Uani 1 1 d . . . H22 H 0.0357 0.0723 0.083 0.126 Uiso 1 1 calc R . . C23 C -0.2022(3) 0.1964(3) 0.43880(17) 0.0486(9) Uani 1 1 d . . . H23A H -0.2091 0.2532 0.4164 0.058 Uiso 1 1 calc R . . H23B H -0.2103 0.1432 0.4049 0.058 Uiso 1 1 calc R . . C24 C -0.5022(4) 0.1652(4) 0.4251(2) 0.0873(16) Uani 1 1 d . . . H24A H -0.5747 0.1567 0.4495 0.131 Uiso 1 1 calc R . . H24B H -0.5059 0.1104 0.3937 0.131 Uiso 1 1 calc R . . H24C H -0.5105 0.2202 0.4019 0.131 Uiso 1 1 calc R . . C25 C -0.3371(4) 0.2861(3) 0.5416(2) 0.0789(13) Uani 1 1 d . . . H25A H -0.4111 0.278 0.5651 0.118 Uiso 1 1 calc R . . H25B H -0.3445 0.3407 0.5178 0.118 Uiso 1 1 calc R . . H25C H -0.2535 0.2947 0.5727 0.118 Uiso 1 1 calc R . . C26 C -0.3297(4) 0.0780(3) 0.5287(2) 0.0820(14) Uani 1 1 d . . . H26A H -0.4046 0.0706 0.5516 0.123 Uiso 1 1 calc R . . H26B H -0.2468 0.087 0.5603 0.123 Uiso 1 1 calc R . . H26C H -0.3314 0.0223 0.4984 0.123 Uiso 1 1 calc R . . C27 C 0.0766(3) 0.1101(3) 0.55877(18) 0.0541(10) Uani 1 1 d . . . H27A H 0.0034 0.0712 0.572 0.065 Uiso 1 1 calc R . . H27B H 0.1196 0.0686 0.531 0.065 Uiso 1 1 calc R . . C28 C 0.3448(4) 0.2204(3) 0.6125(2) 0.0721(13) Uani 1 1 d . . . H28A H 0.4084 0.2432 0.6524 0.108 Uiso 1 1 calc R . . H28B H 0.3166 0.2732 0.5903 0.108 Uiso 1 1 calc R . . H28C H 0.3865 0.1806 0.5837 0.108 Uiso 1 1 calc R . . C29 C 0.2602(4) 0.0533(3) 0.6750(2) 0.0813(14) Uani 1 1 d . . . H29A H 0.3239 0.077 0.7147 0.122 Uiso 1 1 calc R . . H29B H 0.3032 0.0154 0.6457 0.122 Uiso 1 1 calc R . . H29C H 0.1854 0.0152 0.6864 0.122 Uiso 1 1 calc R . . C30 C 0.1227(5) 0.2263(4) 0.6909(2) 0.1019(18) Uani 1 1 d . . . H30A H 0.1882 0.2484 0.7303 0.153 Uiso 1 1 calc R . . H30B H 0.0472 0.1896 0.7027 0.153 Uiso 1 1 calc R . . H30C H 0.0924 0.2796 0.6699 0.153 Uiso 1 1 calc R . . In2 In 0.25231(2) 0.575714(19) 0.843389(12) 0.04951(9) Uani 1 1 d . . . Si3 Si 0.46085(13) 0.40871(10) 0.86853(7) 0.0783(4) Uani 1 1 d . . . O31 O 0.1732(2) 0.5364(2) 0.74535(12) 0.0677(8) Uani 1 1 d . A . C32 C 0.0523(3) 0.5212(2) 0.71255(16) 0.0449(8) Uani 1 1 d . . . C33 C 0.0290(3) 0.4951(2) 0.64334(16) 0.0419(8) Uani 1 1 d . A . C34 C -0.0980(3) 0.4833(2) 0.60888(17) 0.0492(9) Uani 1 1 d . . . H34 H -0.1122 0.4679 0.563 0.059 Uiso 1 1 calc R A . C35 C -0.2070(3) 0.4935(3) 0.63923(19) 0.0550(10) Uani 1 1 d . A . H35 H -0.2939 0.4851 0.6143 0.066 Uiso 1 1 calc R . . C36 C -0.1870(3) 0.5155(3) 0.70505(18) 0.0508(9) Uani 1 1 d . . . H36 H -0.2614 0.5209 0.7257 0.061 Uiso 1 1 calc R A . C37 C -0.0599(3) 0.5305(2) 0.74323(16) 0.0434(8) Uani 1 1 d . A . C38 C -0.0545(3) 0.5577(3) 0.81170(18) 0.0489(9) Uani 1 1 d . . . H38 H -0.1386 0.5572 0.8244 0.059 Uiso 1 1 calc R A . N39 N 0.0439(3) 0.5825(2) 0.85855(13) 0.0430(7) Uani 1 1 d . A . C40 C 0.0095(3) 0.6123(2) 0.92283(16) 0.0441(8) Uani 1 1 d . . . H40 H -0.0659 0.5678 0.9297 0.053 Uiso 1 1 calc R A . C41 C 0.1227(3) 0.6119(3) 0.97883(16) 0.0489(9) Uani 1 1 d . A . H41A H 0.2003 0.6529 0.9717 0.059 Uiso 1 1 calc R . . H41B H 0.1477 0.5483 0.9802 0.059 Uiso 1 1 calc R . . C42 C 0.0855(4) 0.6451(3) 1.04351(17) 0.0527(9) Uani 1 1 d . . . H42A H 0.0122 0.6015 1.0522 0.063 Uiso 1 1 calc R A . H42B H 0.1622 0.6455 1.079 0.063 Uiso 1 1 calc R . . N43 N 0.0452(3) 0.7380(2) 1.04295(14) 0.0508(8) Uani 1 1 d . A . C44 C -0.0679(4) 0.7385(3) 0.99110(18) 0.0628(11) Uani 1 1 d . . . H44A H -0.095 0.8018 0.9915 0.075 Uiso 1 1 calc R A . H44B H -0.143 0.6959 0.9989 0.075 Uiso 1 1 calc R . . C45 C -0.0348(4) 0.7086(3) 0.92436(18) 0.0596(11) Uani 1 1 d . A . H45A H -0.1137 0.7083 0.8902 0.072 Uiso 1 1 calc R . . H45B H 0.0365 0.7534 0.9152 0.072 Uiso 1 1 calc R . . C46 C 0.0147(4) 0.7718(3) 1.10660(19) 0.0643(11) Uani 1 1 d . . . H46A H -0.0529 0.7262 1.1182 0.077 Uiso 1 1 calc R A . H46B H -0.0238 0.8309 1.1027 0.077 Uiso 1 1 calc R . . C47 C 0.1325(6) 0.7870(4) 1.1603(3) 0.0975(8) Uani 1 1 d . A . C48 C 0.1366(6) 0.7420(4) 1.2153(2) 0.0975(8) Uani 1 1 d . . . H48 H 0.0664 0.6964 1.2188 0.117 Uiso 1 1 calc R A . C49 C 0.2484(5) 0.7647(4) 1.2674(3) 0.0975(8) Uani 1 1 d . A . H49 H 0.2538 0.7342 1.3058 0.117 Uiso 1 1 calc R . . C50 C 0.3451(6) 0.8301(4) 1.2606(3) 0.0975(8) Uani 1 1 d . . . H50 H 0.4161 0.8476 1.2962 0.117 Uiso 1 1 calc R A . C51 C 0.3472(6) 0.8717(4) 1.2068(2) 0.0975(8) Uani 1 1 d . A . H51 H 0.4199 0.9149 1.2029 0.117 Uiso 1 1 calc R . . C52 C 0.2386(6) 0.8495(4) 1.1567(3) 0.0975(8) Uani 1 1 d . . . H52 H 0.238 0.879 1.1181 0.117 Uiso 1 1 calc R A . C53 C 0.3033(5) 0.4493(4) 0.8794(2) 0.0948(18) Uani 1 1 d . A . H53A H 0.3016 0.4558 0.9267 0.114 Uiso 1 1 calc R . . H53B H 0.2321 0.3996 0.8588 0.114 Uiso 1 1 calc R . . C54 C 0.4822(7) 0.3000(5) 0.9071(4) 0.176(4) Uani 1 1 d . A . H54A H 0.5674 0.2796 0.9015 0.264 Uiso 1 1 calc R . . H54B H 0.4106 0.2516 0.8865 0.264 Uiso 1 1 calc R . . H54C H 0.4797 0.3115 0.9537 0.264 Uiso 1 1 calc R . . C55 C 0.6009(5) 0.4963(4) 0.9097(3) 0.136(2) Uani 1 1 d . A . H55A H 0.6847 0.4741 0.9034 0.204 Uiso 1 1 calc R . . H55B H 0.5986 0.5059 0.9564 0.204 Uiso 1 1 calc R . . H55C H 0.5931 0.5551 0.891 0.204 Uiso 1 1 calc R . . C56 C 0.4705(6) 0.3928(5) 0.7808(3) 0.140(3) Uani 1 1 d . A . H56A H 0.5559 0.3722 0.7756 0.21 Uiso 1 1 calc R . . H56B H 0.462 0.4518 0.7625 0.21 Uiso 1 1 calc R . . H56C H 0.3989 0.346 0.758 0.21 Uiso 1 1 calc R . . Si4A Si 0.46000(11) 0.76139(9) 0.81241(6) 0.0641(3) Uani 0.714(4) 1 d P A 1 C57A C 0.3677(6) 0.7068(4) 0.8717(3) 0.0650(15) Uani 0.714(4) 1 d P A 1 H57A H 0.3083 0.7512 0.8852 0.078 Uiso 0.714(4) 1 calc PR A 1 H57B H 0.4332 0.7007 0.911 0.078 Uiso 0.714(4) 1 calc PR A 1 C58A C 0.5818(8) 0.8566(6) 0.8563(5) 0.127(3) Uani 0.714(4) 1 d P A 1 H58A H 0.5369 0.9007 0.8802 0.19 Uiso 0.714(4) 1 calc PR A 1 H58B H 0.6255 0.8884 0.825 0.19 Uiso 0.714(4) 1 calc PR A 1 H58C H 0.6479 0.8315 0.8869 0.19 Uiso 0.714(4) 1 calc PR A 1 C59A C 0.3366(8) 0.8026(6) 0.7495(4) 0.106(2) Uani 0.714(4) 1 d P A 1 H59A H 0.2729 0.7499 0.7278 0.159 Uiso 0.714(4) 1 calc PR A 1 H59B H 0.3819 0.8307 0.7174 0.159 Uiso 0.714(4) 1 calc PR A 1 H59C H 0.2898 0.8488 0.7703 0.159 Uiso 0.714(4) 1 calc PR A 1 C60A C 0.5416(5) 0.6754(4) 0.7669(3) 0.0978(17) Uani 0.714(4) 1 d P A 1 H60A H 0.4752 0.6249 0.7443 0.147 Uiso 0.714(4) 1 calc PR A 1 H60B H 0.6079 0.6502 0.7974 0.147 Uiso 0.714(4) 1 calc PR A 1 H60C H 0.5848 0.7059 0.7349 0.147 Uiso 0.714(4) 1 calc PR A 1 Si4B Si 0.46000(11) 0.76139(9) 0.81241(6) 0.0641(3) Uani 0.286(4) 1 d P A 2 C57B C 0.2989(14) 0.7254(10) 0.8205(8) 0.0650(15) Uani 0.286(4) 1 d P A 2 H57C H 0.2399 0.7333 0.7794 0.078 Uiso 0.286(4) 1 calc PR A 2 H57D H 0.2757 0.7676 0.8554 0.078 Uiso 0.286(4) 1 calc PR A 2 C58B C 0.5735(19) 0.7820(16) 0.8932(11) 0.127(3) Uani 0.286(4) 1 d P A 2 H58D H 0.6633 0.8027 0.887 0.19 Uiso 0.286(4) 1 calc PR A 2 H58E H 0.5734 0.7243 0.9138 0.19 Uiso 0.286(4) 1 calc PR A 2 H58F H 0.5432 0.8299 0.9213 0.19 Uiso 0.286(4) 1 calc PR A 2 C59B C 0.470(2) 0.8773(14) 0.7752(9) 0.106(2) Uani 0.286(4) 1 d P A 2 H59D H 0.5616 0.8958 0.7704 0.159 Uiso 0.286(4) 1 calc PR A 2 H59E H 0.4416 0.9252 0.8039 0.159 Uiso 0.286(4) 1 calc PR A 2 H59F H 0.4125 0.8699 0.7324 0.159 Uiso 0.286(4) 1 calc PR A 2 C60B C 0.5416(5) 0.6754(4) 0.7669(3) 0.0978(17) Uani 0.286(4) 1 d P A 2 H60D H 0.6292 0.7037 0.7621 0.147 Uiso 0.286(4) 1 calc PR A 2 H60E H 0.4877 0.6562 0.7237 0.147 Uiso 0.286(4) 1 calc PR A 2 H60F H 0.551 0.6212 0.7908 0.147 Uiso 0.286(4) 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 In1 0.02636(12) 0.04157(15) 0.04621(15) 0.00761(11) 0.00748(10) -0.00110(10) Si1 0.0263(4) 0.0571(7) 0.0645(7) 0.0146(5) 0.0064(4) 0.0002(4) Si2 0.0426(5) 0.0602(7) 0.0477(6) 0.0131(5) 0.0074(4) 0.0038(5) O1 0.0368(12) 0.0436(15) 0.0602(15) -0.0010(12) 0.0194(11) -0.0010(11) C2 0.0367(17) 0.0355(19) 0.0417(19) 0.0128(15) 0.0083(14) 0.0057(15) C3 0.0429(18) 0.041(2) 0.0372(18) 0.0073(15) 0.0081(15) 0.0066(15) C4 0.064(2) 0.050(2) 0.045(2) -0.0027(18) 0.0108(19) -0.0063(19) C5 0.055(2) 0.059(3) 0.058(2) -0.003(2) 0.0151(19) -0.0210(19) C6 0.044(2) 0.052(2) 0.053(2) 0.0039(19) 0.0223(17) -0.0125(17) C7 0.0349(17) 0.0392(19) 0.0377(18) 0.0060(15) 0.0082(14) 0.0007(14) C8 0.0317(16) 0.038(2) 0.048(2) 0.0074(16) 0.0161(15) 0.0020(14) N9 0.0307(13) 0.0356(16) 0.0410(15) 0.0041(12) 0.0085(11) 0.0019(12) C10 0.0311(16) 0.038(2) 0.051(2) 0.0034(16) 0.0124(15) 0.0011(14) C11 0.0407(18) 0.041(2) 0.055(2) 0.0083(17) 0.0047(16) 0.0124(16) C12 0.053(2) 0.044(2) 0.076(3) 0.000(2) 0.012(2) 0.0176(18) N13 0.0546(18) 0.0435(18) 0.0516(18) -0.0075(15) 0.0150(15) 0.0092(14) C14 0.052(2) 0.048(2) 0.051(2) 0.0002(18) 0.0140(17) 0.0060(17) C15 0.050(2) 0.0341(19) 0.045(2) 0.0031(16) 0.0111(16) 0.0073(15) C16 0.083(3) 0.064(3) 0.075(3) -0.018(2) 0.025(3) 0.020(2) C17 0.088(3) 0.048(3) 0.053(3) -0.016(2) 0.016(2) 0.009(2) C18 0.083(4) 0.169(6) 0.068(3) -0.005(4) 0.019(3) -0.008(4) C19 0.095(5) 0.196(8) 0.109(5) -0.052(5) 0.011(4) -0.005(5) C20 0.150(7) 0.167(8) 0.083(5) -0.035(5) -0.034(5) 0.028(6) C21 0.181(8) 0.176(8) 0.085(5) 0.040(5) -0.008(6) 0.001(7) C22 0.123(5) 0.100(5) 0.086(4) 0.028(3) 0.010(4) -0.015(4) C23 0.0304(17) 0.060(2) 0.054(2) 0.0063(18) 0.0058(15) 0.0000(16) C24 0.033(2) 0.120(4) 0.104(4) 0.024(3) -0.005(2) 0.001(2) C25 0.073(3) 0.079(3) 0.092(3) 0.006(3) 0.040(3) 0.004(2) C26 0.057(3) 0.077(3) 0.119(4) 0.043(3) 0.020(3) 0.004(2) C27 0.048(2) 0.050(2) 0.063(2) 0.0164(19) 0.0027(18) 0.0026(17) C28 0.048(2) 0.087(3) 0.082(3) 0.034(3) 0.005(2) 0.000(2) C29 0.075(3) 0.087(4) 0.078(3) 0.038(3) -0.006(2) -0.002(3) C30 0.102(4) 0.132(5) 0.074(3) -0.006(3) 0.026(3) 0.025(4) In2 0.03707(14) 0.05920(19) 0.05074(17) -0.00664(13) 0.01123(11) 0.00456(12) Si3 0.0629(8) 0.0831(10) 0.0958(10) 0.0053(8) 0.0212(7) 0.0343(7) O31 0.0406(14) 0.122(3) 0.0414(14) 0.0003(15) 0.0091(12) 0.0187(15) C32 0.0410(19) 0.050(2) 0.045(2) 0.0052(17) 0.0074(16) 0.0120(16) C33 0.0441(19) 0.041(2) 0.043(2) 0.0050(16) 0.0106(16) 0.0101(16) C34 0.053(2) 0.051(2) 0.044(2) 0.0024(17) 0.0026(17) 0.0189(18) C35 0.042(2) 0.064(3) 0.058(2) 0.000(2) 0.0043(18) 0.0183(18) C36 0.0419(19) 0.056(2) 0.057(2) 0.0025(19) 0.0138(17) 0.0147(17) C37 0.0431(19) 0.048(2) 0.041(2) 0.0041(16) 0.0098(15) 0.0136(16) C38 0.0395(19) 0.053(2) 0.060(2) 0.0082(19) 0.0191(18) 0.0127(17) N39 0.0405(16) 0.0476(18) 0.0436(17) 0.0016(14) 0.0127(13) 0.0121(13) C40 0.0446(19) 0.048(2) 0.043(2) 0.0014(17) 0.0148(16) 0.0142(16) C41 0.057(2) 0.048(2) 0.046(2) 0.0030(17) 0.0127(17) 0.0212(18) C42 0.067(2) 0.050(2) 0.047(2) 0.0058(18) 0.0153(18) 0.0236(19) N43 0.0579(19) 0.053(2) 0.0476(18) 0.0001(15) 0.0188(15) 0.0229(15) C44 0.068(3) 0.066(3) 0.059(3) -0.002(2) 0.012(2) 0.034(2) C45 0.070(3) 0.059(3) 0.056(2) 0.006(2) 0.017(2) 0.032(2) C46 0.070(3) 0.065(3) 0.064(3) -0.010(2) 0.029(2) 0.020(2) C47 0.1058(18) 0.114(2) 0.0778(14) -0.0021(14) 0.0130(14) 0.0540(15) C48 0.1058(18) 0.114(2) 0.0778(14) -0.0021(14) 0.0130(14) 0.0540(15) C49 0.1058(18) 0.114(2) 0.0778(14) -0.0021(14) 0.0130(14) 0.0540(15) C50 0.1058(18) 0.114(2) 0.0778(14) -0.0021(14) 0.0130(14) 0.0540(15) C51 0.1058(18) 0.114(2) 0.0778(14) -0.0021(14) 0.0130(14) 0.0540(15) C52 0.1058(18) 0.114(2) 0.0778(14) -0.0021(14) 0.0130(14) 0.0540(15) C53 0.084(3) 0.132(5) 0.093(4) 0.045(3) 0.041(3) 0.060(3) C54 0.141(6) 0.145(7) 0.292(10) 0.111(7) 0.093(7) 0.087(5) C55 0.078(4) 0.139(6) 0.174(6) 0.016(5) -0.030(4) 0.023(4) C56 0.151(6) 0.142(6) 0.135(6) -0.040(5) 0.074(5) 0.018(5) Si4A 0.0558(7) 0.0633(8) 0.0723(8) 0.0057(6) 0.0136(6) 0.0009(6) C57A 0.066(4) 0.059(4) 0.064(4) -0.010(3) 0.016(3) -0.009(3) C58A 0.097(5) 0.104(7) 0.162(8) -0.024(6) 0.035(5) -0.056(5) C59A 0.120(6) 0.108(6) 0.093(5) 0.018(5) 0.009(5) 0.040(5) C60A 0.073(3) 0.100(4) 0.124(5) -0.003(3) 0.039(3) 0.009(3) Si4B 0.0558(7) 0.0633(8) 0.0723(8) 0.0057(6) 0.0136(6) 0.0009(6) C57B 0.066(4) 0.059(4) 0.064(4) -0.010(3) 0.016(3) -0.009(3) C58B 0.097(5) 0.104(7) 0.162(8) -0.024(6) 0.035(5) -0.056(5) C59B 0.120(6) 0.108(6) 0.093(5) 0.018(5) 0.009(5) 0.040(5) C60B 0.073(3) 0.100(4) 0.124(5) -0.003(3) 0.039(3) 0.009(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 In1 O1 2.102(2) . ? In1 C23 2.143(3) . ? In1 C27 2.153(3) . ? In1 N9 2.236(2) . ? Si1 C23 1.840(3) . ? Si1 C24 1.857(4) . ? Si1 C26 1.859(4) . ? Si1 C25 1.873(5) . ? Si2 C28 1.852(4) . ? Si2 C27 1.855(4) . ? Si2 C30 1.863(5) . ? Si2 C29 1.870(4) . ? O1 C2 1.304(4) . ? C2 C7 1.434(4) . ? C2 C3 1.435(5) . ? C3 C4 1.372(5) . ? C3 C33 1.499(4) . ? C4 C5 1.395(5) . ? C4 H4 0.95 . ? C5 C6 1.376(5) . ? C5 H5 0.95 . ? C6 C7 1.401(4) . ? C6 H6 0.95 . ? C7 C8 1.450(4) . ? C8 N9 1.285(4) . ? C8 H8 0.95 . ? N9 C10 1.484(4) . ? C10 C11 1.510(4) . ? C10 C15 1.525(4) . ? C10 H10 1 . ? C11 C12 1.510(5) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 N13 1.469(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? N13 C14 1.456(4) . ? N13 C16 1.471(5) . ? C14 C15 1.523(5) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.500(6) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C22 1.347(6) . ? C17 C18 1.361(6) . ? C18 C19 1.384(8) . ? C18 H18 0.95 . ? C19 C20 1.371(9) . ? C19 H19 0.95 . ? C20 C21 1.350(9) . ? C20 H20 0.95 . ? C21 C22 1.358(8) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? In2 O31 2.083(3) . ? In2 C57A 2.125(5) . ? In2 C53 2.136(5) . ? In2 N39 2.240(3) . ? In2 C57B 2.297(15) . ? Si3 C53 1.830(4) . ? Si3 C56 1.852(6) . ? Si3 C54 1.861(6) . ? Si3 C55 1.863(6) . ? O31 C32 1.307(4) . ? C32 C37 1.430(4) . ? C32 C33 1.438(5) . ? C33 C34 1.373(4) . ? C34 C35 1.398(5) . ? C34 H34 0.95 . ? C35 C36 1.363(5) . ? C35 H35 0.95 . ? C36 C37 1.403(5) . ? C36 H36 0.95 . ? C37 C38 1.443(5) . ? C38 N39 1.285(4) . ? C38 H38 0.95 . ? N39 C40 1.488(4) . ? C40 C41 1.512(5) . ? C40 C45 1.519(5) . ? C40 H40 1 . ? C41 C42 1.520(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 N43 1.458(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? N43 C44 1.456(5) . ? N43 C46 1.475(4) . ? C44 C45 1.531(5) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 C47 1.495(6) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C47 C52 1.368(8) . ? C47 C48 1.374(7) . ? C48 C49 1.438(7) . ? C48 H48 0.95 . ? C49 C50 1.345(7) . ? C49 H49 0.95 . ? C50 C51 1.330(7) . ? C50 H50 0.95 . ? C51 C52 1.391(7) . ? C51 H51 0.95 . ? C52 H52 0.95 . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? Si4A C58A 1.836(7) . ? Si4A C60A 1.860(5) . ? Si4A C59A 1.860(7) . ? Si4A C57A 1.875(6) . ? C57A H57A 0.99 . ? C57A H57B 0.99 . ? C58A H58A 0.98 . ? C58A H58B 0.98 . ? C58A H58C 0.98 . ? C59A H59A 0.98 . ? C59A H59B 0.98 . ? C59A H59C 0.98 . ? C60A H60A 0.98 . ? C60A H60B 0.98 . ? C60A H60C 0.98 . ? C57B H57C 0.99 . ? C57B H57D 0.99 . ? C58B H58D 0.98 . ? C58B H58E 0.98 . ? C58B H58F 0.98 . ? C59B H59D 0.98 . ? C59B H59E 0.98 . ? C59B H59F 0.98 . ? 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 In1 C23 105.89(12) . . ? O1 In1 C27 111.45(12) . . ? C23 In1 C27 129.46(14) . . ? O1 In1 N9 85.39(9) . . ? C23 In1 N9 107.46(11) . . ? C27 In1 N9 108.30(12) . . ? C23 Si1 C24 111.00(19) . . ? C23 Si1 C26 110.50(19) . . ? C24 Si1 C26 109.1(2) . . ? C23 Si1 C25 109.15(18) . . ? C24 Si1 C25 108.5(2) . . ? C26 Si1 C25 108.5(2) . . ? C28 Si2 C27 110.23(19) . . ? C28 Si2 C30 110.0(3) . . ? C27 Si2 C30 110.1(2) . . ? C28 Si2 C29 107.1(2) . . ? C27 Si2 C29 110.4(2) . . ? C30 Si2 C29 108.9(2) . . ? C2 O1 In1 130.3(2) . . ? O1 C2 C7 121.4(3) . . ? O1 C2 C3 120.2(3) . . ? C7 C2 C3 118.3(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 C33 121.1(3) . . ? C2 C3 C33 119.3(3) . . ? C3 C4 C5 122.1(3) . . ? C3 C4 H4 119 . . ? C5 C4 H4 119 . . ? C6 C5 C4 119.0(3) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.0(3) . . ? C5 C6 H6 119 . . ? C7 C6 H6 119 . . ? C6 C7 C2 118.8(3) . . ? C6 C7 C8 116.0(3) . . ? C2 C7 C8 125.2(3) . . ? N9 C8 C7 129.9(3) . . ? N9 C8 H8 115 . . ? C7 C8 H8 115 . . ? C8 N9 C10 118.4(3) . . ? C8 N9 In1 120.5(2) . . ? C10 N9 In1 120.87(19) . . ? N9 C10 C11 111.6(3) . . ? N9 C10 C15 111.4(2) . . ? C11 C10 C15 108.5(3) . . ? N9 C10 H10 108.4 . . ? C11 C10 H10 108.4 . . ? C15 C10 H10 108.4 . . ? C10 C11 C12 111.3(3) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108 . . ? N13 C12 C11 111.6(3) . . ? N13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108 . . ? C14 N13 C12 110.1(3) . . ? C14 N13 C16 112.4(3) . . ? C12 N13 C16 109.5(3) . . ? N13 C14 C15 112.5(3) . . ? N13 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N13 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C10 110.4(3) . . ? C14 C15 H15A 109.6 . . ? C10 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C10 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N13 C16 C17 114.8(3) . . ? N13 C16 H16A 108.6 . . ? C17 C16 H16A 108.6 . . ? N13 C16 H16B 108.6 . . ? C17 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? C22 C17 C18 116.8(5) . . ? C22 C17 C16 121.3(5) . . ? C18 C17 C16 121.8(4) . . ? C17 C18 C19 121.5(6) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C20 C19 C18 119.8(7) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 118.3(7) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C22 120.6(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C17 C22 C21 122.9(6) . . ? C17 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? Si1 C23 In1 114.90(18) . . ? Si1 C23 H23A 108.5 . . ? In1 C23 H23A 108.5 . . ? Si1 C23 H23B 108.5 . . ? In1 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 In1 119.61(19) . . ? Si2 C27 H27A 107.4 . . ? In1 C27 H27A 107.4 . . ? Si2 C27 H27B 107.4 . . ? In1 C27 H27B 107.4 . . ? H27A C27 H27B 106.9 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O31 In2 C57A 119.42(19) . . ? O31 In2 C53 103.91(18) . . ? C57A In2 C53 124.3(2) . . ? O31 In2 N39 86.73(10) . . ? C57A In2 N39 110.85(18) . . ? C53 In2 N39 104.46(14) . . ? O31 In2 C57B 89.5(4) . . ? C57A In2 C57B 32.6(4) . . ? C53 In2 C57B 153.9(4) . . ? N39 In2 C57B 98.5(4) . . ? C53 Si3 C56 110.1(3) . . ? C53 Si3 C54 110.4(3) . . ? C56 Si3 C54 111.7(3) . . ? C53 Si3 C55 110.1(3) . . ? C56 Si3 C55 107.7(3) . . ? C54 Si3 C55 106.8(3) . . ? C32 O31 In2 133.2(2) . . ? O31 C32 C37 122.0(3) . . ? O31 C32 C33 120.0(3) . . ? C37 C32 C33 117.9(3) . . ? C34 C33 C32 119.6(3) . . ? C34 C33 C3 119.0(3) . . ? C32 C33 C3 121.5(3) . . ? C33 C34 C35 122.0(3) . . ? C33 C34 H34 119 . . ? C35 C34 H34 119 . . ? C36 C35 C34 119.2(3) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 122.0(3) . . ? C35 C36 H36 119 . . ? C37 C36 H36 119 . . ? C36 C37 C32 119.3(3) . . ? C36 C37 C38 115.4(3) . . ? C32 C37 C38 125.3(3) . . ? N39 C38 C37 131.4(3) . . ? N39 C38 H38 114.3 . . ? C37 C38 H38 114.3 . . ? C38 N39 C40 115.7(3) . . ? C38 N39 In2 121.2(2) . . ? C40 N39 In2 123.1(2) . . ? N39 C40 C41 112.7(3) . . ? N39 C40 C45 111.2(3) . . ? C41 C40 C45 108.8(3) . . ? N39 C40 H40 108 . . ? C41 C40 H40 108 . . ? C45 C40 H40 108 . . ? C40 C41 C42 111.4(3) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108 . . ? N43 C42 C41 111.1(3) . . ? N43 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? N43 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108 . . ? C44 N43 C42 110.1(3) . . ? C44 N43 C46 110.9(3) . . ? C42 N43 C46 111.1(3) . . ? N43 C44 C45 111.3(3) . . ? N43 C44 H44A 109.4 . . ? C45 C44 H44A 109.4 . . ? N43 C44 H44B 109.4 . . ? C45 C44 H44B 109.4 . . ? H44A C44 H44B 108 . . ? C40 C45 C44 110.4(3) . . ? C40 C45 H45A 109.6 . . ? C44 C45 H45A 109.6 . . ? C40 C45 H45B 109.6 . . ? C44 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? N43 C46 C47 113.5(3) . . ? N43 C46 H46A 108.9 . . ? C47 C46 H46A 108.9 . . ? N43 C46 H46B 108.9 . . ? C47 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C52 C47 C48 118.0(6) . . ? C52 C47 C46 120.2(5) . . ? C48 C47 C46 121.8(6) . . ? C47 C48 C49 119.3(6) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C50 C49 C48 118.4(6) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C51 C50 C49 123.8(6) . . ? C51 C50 H50 118.1 . . ? C49 C50 H50 118.1 . . ? C50 C51 C52 117.3(6) . . ? C50 C51 H51 121.3 . . ? C52 C51 H51 121.3 . . ? C47 C52 C51 123.1(6) . . ? C47 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? Si3 C53 In2 119.6(3) . . ? Si3 C53 H53A 107.4 . . ? In2 C53 H53A 107.4 . . ? Si3 C53 H53B 107.4 . . ? In2 C53 H53B 107.4 . . ? H53A C53 H53B 106.9 . . ? Si3 C54 H54A 109.5 . . ? Si3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si3 C55 H55A 109.5 . . ? Si3 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si3 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si3 C56 H56A 109.5 . . ? Si3 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si3 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58A Si4A C60A 110.8(3) . . ? C58A Si4A C59A 112.1(4) . . ? C60A Si4A C59A 105.1(3) . . ? C58A Si4A C57A 109.2(3) . . ? C60A Si4A C57A 112.0(3) . . ? C59A Si4A C57A 107.6(3) . . ? Si4A C57A In2 119.6(3) . . ? Si4A C57A H57A 107.4 . . ? In2 C57A H57A 107.4 . . ? Si4A C57A H57B 107.4 . . ? In2 C57A H57B 107.4 . . ? H57A C57A H57B 107 . . ? Si4A C58A H58A 109.5 . . ? Si4A C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? Si4A C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? Si4A C59A H59A 109.5 . . ? Si4A C59A H59B 109.5 . . ? H59A C59A H59B 109.5 . . ? Si4A C59A H59C 109.5 . . ? H59A C59A H59C 109.5 . . ? H59B C59A H59C 109.5 . . ? Si4A C60A H60A 109.5 . . ? Si4A C60A H60B 109.5 . . ? H60A C60A H60B 109.5 . . ? Si4A C60A H60C 109.5 . . ? H60A C60A H60C 109.5 . . ? H60B C60A H60C 109.5 . . ? In2 C57B H57C 107.9 . . ? In2 C57B H57D 107.9 . . ? H57C C57B H57D 107.2 . . ? H58D C58B H58E 109.5 . . ? H58D C58B H58F 109.5 . . ? H58E C58B H58F 109.5 . . ? H59D C59B H59E 109.5 . . ? H59D C59B H59F 109.5 . . ? H59E C59B H59F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 In1 O1 C2 -135.1(3) . . . . ? C27 In1 O1 C2 79.6(3) . . . . ? N9 In1 O1 C2 -28.2(3) . . . . ? In1 O1 C2 C7 18.3(4) . . . . ? In1 O1 C2 C3 -162.8(2) . . . . ? O1 C2 C3 C4 176.0(3) . . . . ? C7 C2 C3 C4 -5.1(5) . . . . ? O1 C2 C3 C33 -5.4(4) . . . . ? C7 C2 C3 C33 173.5(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C33 C3 C4 C5 -177.6(3) . . . . ? C3 C4 C5 C6 2.8(6) . . . . ? C4 C5 C6 C7 -2.3(6) . . . . ? C5 C6 C7 C2 -2.0(5) . . . . ? C5 C6 C7 C8 175.1(3) . . . . ? O1 C2 C7 C6 -175.5(3) . . . . ? C3 C2 C7 C6 5.6(4) . . . . ? O1 C2 C7 C8 7.8(5) . . . . ? C3 C2 C7 C8 -171.2(3) . . . . ? C6 C7 C8 N9 172.4(3) . . . . ? C2 C7 C8 N9 -10.8(5) . . . . ? C7 C8 N9 C10 175.0(3) . . . . ? C7 C8 N9 In1 -10.2(5) . . . . ? O1 In1 N9 C8 22.4(2) . . . . ? C23 In1 N9 C8 127.6(2) . . . . ? C27 In1 N9 C8 -88.7(3) . . . . ? O1 In1 N9 C10 -162.9(2) . . . . ? C23 In1 N9 C10 -57.7(2) . . . . ? C27 In1 N9 C10 86.0(2) . . . . ? C8 N9 C10 C11 135.0(3) . . . . ? In1 N9 C10 C11 -39.7(3) . . . . ? C8 N9 C10 C15 -103.5(3) . . . . ? In1 N9 C10 C15 81.8(3) . . . . ? N9 C10 C11 C12 179.1(3) . . . . ? C15 C10 C11 C12 55.9(3) . . . . ? C10 C11 C12 N13 -58.2(4) . . . . ? C11 C12 N13 C14 57.6(4) . . . . ? C11 C12 N13 C16 -178.4(3) . . . . ? C12 N13 C14 C15 -57.4(4) . . . . ? C16 N13 C14 C15 -179.8(3) . . . . ? N13 C14 C15 C10 57.0(4) . . . . ? N9 C10 C15 C14 -178.0(3) . . . . ? C11 C10 C15 C14 -54.7(4) . . . . ? C14 N13 C16 C17 -70.8(5) . . . . ? C12 N13 C16 C17 166.5(4) . . . . ? N13 C16 C17 C22 124.4(5) . . . . ? N13 C16 C17 C18 -59.5(6) . . . . ? C22 C17 C18 C19 0.7(9) . . . . ? C16 C17 C18 C19 -175.6(5) . . . . ? C17 C18 C19 C20 -1.9(11) . . . . ? C18 C19 C20 C21 1.9(12) . . . . ? C19 C20 C21 C22 -0.9(13) . . . . ? C18 C17 C22 C21 0.4(9) . . . . ? C16 C17 C22 C21 176.8(6) . . . . ? C20 C21 C22 C17 -0.3(12) . . . . ? C24 Si1 C23 In1 -176.9(2) . . . . ? C26 Si1 C23 In1 -55.7(3) . . . . ? C25 Si1 C23 In1 63.6(3) . . . . ? O1 In1 C23 Si1 -76.2(2) . . . . ? C27 In1 C23 Si1 60.4(3) . . . . ? N9 In1 C23 Si1 -166.30(17) . . . . ? C28 Si2 C27 In1 -60.9(3) . . . . ? C30 Si2 C27 In1 60.7(3) . . . . ? C29 Si2 C27 In1 -179.0(2) . . . . ? O1 In1 C27 Si2 -14.9(2) . . . . ? C23 In1 C27 Si2 -149.66(18) . . . . ? N9 In1 C27 Si2 77.4(2) . . . . ? C57A In2 O31 C32 -114.1(4) . . . . ? C53 In2 O31 C32 102.2(4) . . . . ? N39 In2 O31 C32 -1.9(3) . . . . ? C57B In2 O31 C32 -100.4(5) . . . . ? In2 O31 C32 C37 -0.1(6) . . . . ? In2 O31 C32 C33 179.4(3) . . . . ? O31 C32 C33 C34 -177.2(3) . . . . ? C37 C32 C33 C34 2.4(5) . . . . ? O31 C32 C33 C3 2.2(5) . . . . ? C37 C32 C33 C3 -178.3(3) . . . . ? C4 C3 C33 C34 136.0(4) . . . . ? C2 C3 C33 C34 -42.6(4) . . . . ? C4 C3 C33 C32 -43.4(5) . . . . ? C2 C3 C33 C32 138.0(3) . . . . ? C32 C33 C34 C35 -1.8(5) . . . . ? C3 C33 C34 C35 178.8(3) . . . . ? C33 C34 C35 C36 -0.1(6) . . . . ? C34 C35 C36 C37 1.5(6) . . . . ? C35 C36 C37 C32 -0.9(6) . . . . ? C35 C36 C37 C38 177.1(4) . . . . ? O31 C32 C37 C36 178.5(3) . . . . ? C33 C32 C37 C36 -1.0(5) . . . . ? O31 C32 C37 C38 0.7(6) . . . . ? C33 C32 C37 C38 -178.8(3) . . . . ? C36 C37 C38 N39 -174.7(4) . . . . ? C32 C37 C38 N39 3.2(6) . . . . ? C37 C38 N39 C40 175.8(4) . . . . ? C37 C38 N39 In2 -6.2(5) . . . . ? O31 In2 N39 C38 4.6(3) . . . . ? C57A In2 N39 C38 124.9(3) . . . . ? C53 In2 N39 C38 -98.9(3) . . . . ? C57B In2 N39 C38 93.6(5) . . . . ? O31 In2 N39 C40 -177.6(3) . . . . ? C57A In2 N39 C40 -57.2(3) . . . . ? C53 In2 N39 C40 78.9(3) . . . . ? C57B In2 N39 C40 -88.6(5) . . . . ? C38 N39 C40 C41 162.4(3) . . . . ? In2 N39 C40 C41 -15.6(4) . . . . ? C38 N39 C40 C45 -75.2(4) . . . . ? In2 N39 C40 C45 106.8(3) . . . . ? N39 C40 C41 C42 178.5(3) . . . . ? C45 C40 C41 C42 54.7(4) . . . . ? C40 C41 C42 N43 -57.8(4) . . . . ? C41 C42 N43 C44 59.2(4) . . . . ? C41 C42 N43 C46 -177.6(3) . . . . ? C42 N43 C44 C45 -59.7(4) . . . . ? C46 N43 C44 C45 177.0(3) . . . . ? N39 C40 C45 C44 -179.2(3) . . . . ? C41 C40 C45 C44 -54.5(4) . . . . ? N43 C44 C45 C40 58.1(5) . . . . ? C44 N43 C46 C47 -171.0(4) . . . . ? C42 N43 C46 C47 66.2(5) . . . . ? N43 C46 C47 C52 60.5(6) . . . . ? N43 C46 C47 C48 -121.8(5) . . . . ? C52 C47 C48 C49 2.4(7) . . . . ? C46 C47 C48 C49 -175.3(4) . . . . ? C47 C48 C49 C50 0.5(7) . . . . ? C48 C49 C50 C51 -3.8(8) . . . . ? C49 C50 C51 C52 3.9(8) . . . . ? C48 C47 C52 C51 -2.4(8) . . . . ? C46 C47 C52 C51 175.3(4) . . . . ? C50 C51 C52 C47 -0.6(8) . . . . ? C56 Si3 C53 In2 -58.4(4) . . . . ? C54 Si3 C53 In2 177.8(4) . . . . ? C55 Si3 C53 In2 60.2(4) . . . . ? O31 In2 C53 Si3 83.2(3) . . . . ? C57A In2 C53 Si3 -58.3(4) . . . . ? N39 In2 C53 Si3 173.3(3) . . . . ? C57B In2 C53 Si3 -35.9(10) . . . . ? C58A Si4A C57A In2 -165.5(4) . . . . ? C60A Si4A C57A In2 -42.4(4) . . . . ? C59A Si4A C57A In2 72.6(4) . . . . ? O31 In2 C57A Si4A -27.2(4) . . . . ? C53 In2 C57A Si4A 108.8(3) . . . . ? N39 In2 C57A Si4A -125.5(3) . . . . ? C57B In2 C57A Si4A -53.1(7) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 959435' ####################################################################### # # 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_sq _audit_creation_date 2011-09-06T13:44:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C336 H416 Al16 N32 O16' _chemical_formula_sum 'C336 H416 Al16 N32 O16' _chemical_formula_weight 5590.69 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F 2 d d' _symmetry_space_group_name_Hall 'F -2d 2' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x+1/4, -y+1/4, z+1/4' 'x+1/4, y+1/4, -z+1/4' 'x, y+1/2, z+1/2' 'x, -y+1/2, -z+1/2' 'x+1/4, -y+3/4, z+3/4' 'x+1/4, y+3/4, -z+3/4' 'x+1/2, y, z+1/2' 'x+1/2, -y, -z+1/2' 'x+3/4, -y+1/4, z+3/4' 'x+3/4, y+1/4, -z+3/4' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+3/4, -y+3/4, z+1/4' 'x+3/4, y+3/4, -z+1/4' _cell_length_a 15.3906(12) _cell_length_b 41.213(3) _cell_length_c 55.854(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 35428(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5217 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 19.6 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11968 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.992 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.659 0.000 0.000 17 1 ' ' 2 0.447 0.000 0.250 674 243 ' ' 3 0.159 0.000 0.500 17 1 ' ' 4 0.947 0.000 0.750 674 243 ' ' 5 0.364 0.105 0.342 13 2 ' ' 6 0.864 0.105 0.842 13 2 ' ' 7 0.523 0.250 0.000 673 243 ' ' 8 0.023 0.250 0.500 673 243 ' ' 9 0.114 0.145 0.092 13 2 ' ' 10 0.614 0.145 0.592 13 2 ' ' 11 0.909 0.250 0.250 17 1 ' ' 12 0.409 0.250 0.750 17 1 ' ' 13 0.114 0.355 0.408 13 2 ' ' 14 0.614 0.355 0.908 13 2 ' ' 15 0.761 0.500 0.250 674 243 ' ' 16 0.261 0.500 0.750 674 243 ' ' 17 0.364 0.395 0.158 13 2 ' ' 18 0.864 0.395 0.658 13 2 ' ' 19 0.159 0.500 0.000 17 1 ' ' 20 0.659 0.500 0.500 17 1 ' ' 21 0.864 0.605 0.342 13 2 ' ' 22 0.364 0.605 0.842 13 2 ' ' 23 0.023 0.750 0.000 673 243 ' ' 24 0.523 0.750 0.500 673 243 ' ' 25 0.614 0.645 0.092 13 2 ' ' 26 0.114 0.645 0.592 13 2 ' ' 27 0.409 0.750 0.250 17 1 ' ' 28 0.909 0.750 0.750 17 1 ' ' 29 0.614 0.855 0.408 13 2 ' ' 30 0.114 0.855 0.908 13 2 ' ' 31 0.864 0.895 0.158 13 2 ' ' 32 0.364 0.895 0.658 13 2 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_unetI/netI 0.1405 _diffrn_reflns_number 76390 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -53 _diffrn_reflns_limit_k_max 53 _diffrn_reflns_limit_l_min -72 _diffrn_reflns_limit_l_max 72 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 18553 _reflns_number_gt 9492 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0744P)^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_number_reflns 18553 _refine_ls_number_parameters 909 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.10(17) _refine_diff_density_max 0.622 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.68146(9) -0.21496(3) -0.14550(2) 0.0317(3) Uani 1 1 d . . . Al2 Al 1.11372(9) -0.20479(3) -0.22320(2) 0.0346(3) Uani 1 1 d . . . N1 N 0.6223(2) -0.25065(8) -0.16249(6) 0.0311(8) Uani 1 1 d . . . N2 N 1.1542(2) -0.16612(8) -0.20551(6) 0.0302(9) Uani 1 1 d . . . N3 N 0.8317(2) -0.13966(8) -0.20190(6) 0.0358(9) Uani 1 1 d . . . N4 N 1.3862(2) -0.07003(8) -0.15882(6) 0.0304(9) Uani 1 1 d . . . O1 O 0.78218(19) -0.22111(6) -0.16005(5) 0.0349(7) Uani 1 1 d . . . O2 O 1.0221(2) -0.21127(7) -0.20442(5) 0.0405(8) Uani 1 1 d . . . C1 C 0.6297(3) -0.17329(10) -0.15368(8) 0.0412(12) Uani 1 1 d . . . H1A H 0.6701 -0.1558 -0.1495 0.062 Uiso 1 1 calc R . . H1B H 0.5754 -0.1705 -0.1447 0.062 Uiso 1 1 calc R . . H1C H 0.6174 -0.1726 -0.1709 0.062 Uiso 1 1 calc R . . C2 C 0.6976(4) -0.22303(13) -0.11079(8) 0.0519(14) Uani 1 1 d . . . H2A H 0.7188 -0.2452 -0.1084 0.078 Uiso 1 1 calc R . . H2B H 0.642 -0.2203 -0.1025 0.078 Uiso 1 1 calc R . . H2C H 0.7401 -0.2076 -0.1044 0.078 Uiso 1 1 calc R . . C3 C 0.5266(3) -0.25713(10) -0.15952(7) 0.0319(10) Uani 1 1 d . . . H3 H 0.5138 -0.2792 -0.1661 0.038 Uiso 1 1 calc R . . C4 C 0.5028(3) -0.25706(11) -0.13327(7) 0.0362(11) Uani 1 1 d . . . H4A H 0.5178 -0.2359 -0.1261 0.043 Uiso 1 1 calc R . . H4B H 0.5356 -0.2742 -0.1248 0.043 Uiso 1 1 calc R . . C5 C 0.4059(3) -0.26319(11) -0.13084(8) 0.0362(11) Uani 1 1 d . . . H5A H 0.3914 -0.2847 -0.1376 0.043 Uiso 1 1 calc R . . H5B H 0.3894 -0.2631 -0.1137 0.043 Uiso 1 1 calc R . . C6 C 0.4728(3) -0.23265(11) -0.17311(7) 0.0340(11) Uani 1 1 d . . . H6A H 0.487 -0.2105 -0.1675 0.041 Uiso 1 1 calc R . . H6B H 0.4868 -0.2339 -0.1904 0.041 Uiso 1 1 calc R . . C7 C 0.3780(3) -0.23910(11) -0.16944(8) 0.0386(11) Uani 1 1 d . . . H7A H 0.3433 -0.2225 -0.178 0.046 Uiso 1 1 calc R . . H7B H 0.3629 -0.2607 -0.176 0.046 Uiso 1 1 calc R . . C8 C 0.2628(3) -0.24247(12) -0.13986(8) 0.0432(12) Uani 1 1 d . . . H8A H 0.2466 -0.2652 -0.1435 0.052 Uiso 1 1 calc R . . H8B H 0.2308 -0.2281 -0.151 0.052 Uiso 1 1 calc R . . C9 C 0.2373(3) -0.23459(14) -0.11448(9) 0.0486(13) Uani 1 1 d . . . C10 C 0.1837(4) -0.25432(17) -0.10172(11) 0.0747(19) Uani 1 1 d . . . H10 H 0.1656 -0.2744 -0.1085 0.09 Uiso 1 1 calc R . . C11 C 0.1547(5) -0.2458(3) -0.07899(14) 0.103(3) Uani 1 1 d . . . H11 H 0.1155 -0.2596 -0.0707 0.124 Uiso 1 1 calc R . . C12 C 0.1813(7) -0.2185(3) -0.06881(15) 0.127(4) Uani 1 1 d . . . H12 H 0.1608 -0.2127 -0.0534 0.152 Uiso 1 1 calc R . . C13 C 0.2413(6) -0.19781(19) -0.08120(14) 0.111(3) Uani 1 1 d . . . H13 H 0.2646 -0.1789 -0.0739 0.134 Uiso 1 1 calc R . . C14 C 0.2636(5) -0.20674(15) -0.10422(11) 0.076(2) Uani 1 1 d . . . H14 H 0.2994 -0.1925 -0.1133 0.092 Uiso 1 1 calc R . . C15 C 0.6639(3) -0.26973(10) -0.17639(7) 0.0304(10) Uani 1 1 d . . . H15 H 0.6305 -0.2862 -0.1839 0.037 Uiso 1 1 calc R . . C16 C 0.7541(3) -0.26939(10) -0.18209(7) 0.0312(10) Uani 1 1 d . . . C17 C 0.7868(4) -0.29409(11) -0.19677(8) 0.0421(12) Uani 1 1 d . . . H17 H 0.7484 -0.31 -0.203 0.051 Uiso 1 1 calc R . . C18 C 0.8748(4) -0.29568(11) -0.20229(8) 0.0466(13) Uani 1 1 d . . . H18 H 0.8964 -0.3122 -0.2126 0.056 Uiso 1 1 calc R . . C19 C 0.9298(3) -0.27293(11) -0.19261(7) 0.0379(11) Uani 1 1 d . . . H19 H 0.99 -0.2742 -0.1963 0.045 Uiso 1 1 calc R . . C20 C 0.9009(3) -0.24810(10) -0.17766(7) 0.0301(10) Uani 1 1 d . . . C21 C 0.8128(3) -0.24558(10) -0.17293(7) 0.0308(11) Uani 1 1 d . . . C22 C 0.9643(3) -0.22504(10) -0.16660(7) 0.0319(10) Uani 1 1 d . . . C23 C 0.9686(3) -0.22175(10) -0.14179(8) 0.0339(11) Uani 1 1 d . . . H23 H 0.9283 -0.2334 -0.1322 0.041 Uiso 1 1 calc R . . C24 C 1.0279(3) -0.20251(11) -0.13075(7) 0.0399(12) Uani 1 1 d . . . H24 H 1.0312 -0.2017 -0.1138 0.048 Uiso 1 1 calc R . . C25 C 1.0831(3) -0.18417(10) -0.14451(7) 0.0312(10) Uani 1 1 d . . . H25 H 1.1222 -0.1696 -0.1369 0.037 Uiso 1 1 calc R . . C26 C 1.0830(3) -0.18658(10) -0.16961(7) 0.0273(9) Uani 1 1 d . . . C27 C 1.0235(3) -0.20828(10) -0.18059(7) 0.0303(10) Uani 1 1 d . . . C28 C 1.1379(3) -0.16463(10) -0.18300(7) 0.0321(10) Uani 1 1 d . . . H28 H 1.1644 -0.1475 -0.1743 0.039 Uiso 1 1 calc R . . C29 C 1.2070(3) -0.13956(10) -0.21598(7) 0.0309(10) Uani 1 1 d . . . H29 H 1.2306 -0.1261 -0.2026 0.037 Uiso 1 1 calc R . . C30 C 1.1504(3) -0.11814(12) -0.23154(9) 0.0473(13) Uani 1 1 d . . . H30A H 1.1243 -0.1313 -0.2445 0.057 Uiso 1 1 calc R . . H30B H 1.1025 -0.109 -0.2218 0.057 Uiso 1 1 calc R . . C31 C 1.2027(4) -0.09106(12) -0.24218(9) 0.0560(15) Uani 1 1 d . . . H31A H 1.1652 -0.0775 -0.2525 0.067 Uiso 1 1 calc R . . H31B H 1.2264 -0.0772 -0.2293 0.067 Uiso 1 1 calc R . . C32 C 1.2823(3) -0.15248(10) -0.23034(8) 0.0387(11) Uani 1 1 d . . . H32A H 1.2607 -0.1673 -0.2429 0.046 Uiso 1 1 calc R . . H32B H 1.3219 -0.1649 -0.2198 0.046 Uiso 1 1 calc R . . C33 C 1.3313(3) -0.12435(11) -0.24182(8) 0.0483(13) Uani 1 1 d . . . H33A H 1.3572 -0.1107 -0.2291 0.058 Uiso 1 1 calc R . . H33B H 1.3792 -0.133 -0.2518 0.058 Uiso 1 1 calc R . . C34 C 1.3225(4) -0.07897(12) -0.26860(9) 0.0582(15) Uani 1 1 d . . . H34A H 1.3714 -0.0884 -0.2778 0.07 Uiso 1 1 calc R . . H34B H 1.3467 -0.0637 -0.2567 0.07 Uiso 1 1 calc R . . C35 C 1.2590(5) -0.06042(15) -0.28600(11) 0.0735(18) Uani 1 1 d . . . C36 C 1.2200(4) -0.07494(17) -0.30626(11) 0.079(2) Uani 1 1 d . . . H36 H 1.2285 -0.0974 -0.3092 0.095 Uiso 1 1 calc R . . C37 C 1.1712(5) -0.0575(2) -0.32149(12) 0.088(2) Uani 1 1 d . . . H37 H 1.1484 -0.0676 -0.3354 0.106 Uiso 1 1 calc R . . C38 C 1.1538(4) -0.02526(17) -0.31727(14) 0.079(2) Uani 1 1 d . . . H38 H 1.1165 -0.0137 -0.3278 0.095 Uiso 1 1 calc R . . C39 C 1.1876(5) -0.01042(17) -0.29909(13) 0.081(2) Uani 1 1 d . . . H39 H 1.1755 0.0119 -0.2966 0.097 Uiso 1 1 calc R . . C40 C 1.2418(5) -0.02693(15) -0.28305(12) 0.082(2) Uani 1 1 d . . . H40 H 1.2673 -0.0155 -0.27 0.099 Uiso 1 1 calc R . . C41 C 1.0728(4) -0.19660(11) -0.25548(7) 0.0472(13) Uani 1 1 d . . . H41A H 1.0507 -0.2168 -0.2624 0.071 Uiso 1 1 calc R . . H41B H 1.1209 -0.1884 -0.2653 0.071 Uiso 1 1 calc R . . H41C H 1.0262 -0.1804 -0.2551 0.071 Uiso 1 1 calc R . . C42 C 1.2044(4) -0.23708(11) -0.21721(8) 0.0470(13) Uani 1 1 d . . . H42A H 1.1994 -0.2451 -0.2007 0.07 Uiso 1 1 calc R . . H42B H 1.2616 -0.2271 -0.2195 0.07 Uiso 1 1 calc R . . H42C H 1.1975 -0.2552 -0.2284 0.07 Uiso 1 1 calc R . . Al3 Al 0.87989(10) -0.10287(3) -0.21953(2) 0.0405(4) Uani 1 1 d . . . Al4 Al 1.32442(9) -0.10727(3) -0.14452(2) 0.0351(3) Uani 1 1 d . . . N5 N 0.3578(2) -0.23815(8) -0.14351(6) 0.0348(9) Uani 1 1 d . . . N6 N 1.2746(3) -0.10473(9) -0.25649(7) 0.0522(12) Uani 1 1 d . . . N7 N 0.6524(2) -0.18636(8) -0.24942(6) 0.0354(9) Uani 1 1 d . . . N8 N 1.6517(2) -0.08098(8) -0.13739(6) 0.0324(9) Uani 1 1 d . . . O3 O 0.9721(2) -0.09882(7) -0.20078(5) 0.0424(8) Uani 1 1 d . . . O4 O 1.22190(19) -0.09644(7) -0.15640(5) 0.0357(8) Uani 1 1 d . . . C51 C 0.9143(4) -0.11325(14) -0.25234(9) 0.0599(15) Uani 1 1 d . . . H51A H 0.9497 -0.0955 -0.2588 0.09 Uiso 1 1 calc R . . H51B H 0.8623 -0.1161 -0.2622 0.09 Uiso 1 1 calc R . . H51C H 0.9483 -0.1334 -0.2524 0.09 Uiso 1 1 calc R . . C52 C 0.8017(3) -0.06586(11) -0.21512(9) 0.0526(14) Uani 1 1 d . . . H52A H 0.7847 -0.0644 -0.1982 0.079 Uiso 1 1 calc R . . H52B H 0.7498 -0.0688 -0.225 0.079 Uiso 1 1 calc R . . H52C H 0.8315 -0.0459 -0.2199 0.079 Uiso 1 1 calc R . . C53 C 0.7627(3) -0.16162(10) -0.21130(8) 0.0368(11) Uani 1 1 d . . . H53 H 0.7407 -0.1751 -0.1977 0.044 Uiso 1 1 calc R . . C54 C 0.7977(3) -0.18465(11) -0.23076(8) 0.0393(11) Uani 1 1 d . . . H54A H 0.8224 -0.1719 -0.2442 0.047 Uiso 1 1 calc R . . H54B H 0.8443 -0.1984 -0.224 0.047 Uiso 1 1 calc R . . C55 C 0.7245(3) -0.20559(11) -0.23975(8) 0.0454(13) Uani 1 1 d . . . H55A H 0.7468 -0.2202 -0.2524 0.054 Uiso 1 1 calc R . . H55B H 0.7028 -0.2192 -0.2264 0.054 Uiso 1 1 calc R . . C56 C 0.6868(3) -0.14228(10) -0.22135(8) 0.0376(11) Uani 1 1 d . . . H56A H 0.6618 -0.1285 -0.2086 0.045 Uiso 1 1 calc R . . H56B H 0.7076 -0.1279 -0.2344 0.045 Uiso 1 1 calc R . . C57 C 0.6176(3) -0.16475(11) -0.23094(8) 0.0423(12) Uani 1 1 d . . . H57A H 0.5937 -0.1779 -0.2176 0.051 Uiso 1 1 calc R . . H57B H 0.5695 -0.1517 -0.2378 0.051 Uiso 1 1 calc R . . C58 C 0.5844(3) -0.20731(10) -0.25883(8) 0.0446(12) Uani 1 1 d . . . H58A H 0.5564 -0.2187 -0.2453 0.054 Uiso 1 1 calc R . . H58B H 0.6117 -0.224 -0.2691 0.054 Uiso 1 1 calc R . . C59 C 0.5157(3) -0.19035(10) -0.27301(7) 0.0336(11) Uani 1 1 d . . . C60 C 0.4315(4) -0.20219(12) -0.27276(8) 0.0489(13) Uani 1 1 d . . . H60 H 0.4171 -0.22 -0.2627 0.059 Uiso 1 1 calc R . . C61 C 0.3679(4) -0.18823(14) -0.28716(9) 0.0583(15) Uani 1 1 d . . . H61 H 0.3109 -0.197 -0.2874 0.07 Uiso 1 1 calc R . . C62 C 0.3874(4) -0.16223(15) -0.30074(9) 0.0582(15) Uani 1 1 d . . . H62 H 0.3432 -0.1526 -0.3103 0.07 Uiso 1 1 calc R . . C63 C 0.4694(4) -0.14925(13) -0.30117(9) 0.0588(16) Uani 1 1 d . . . H63 H 0.4819 -0.1309 -0.3108 0.071 Uiso 1 1 calc R . . C64 C 0.5346(4) -0.16359(11) -0.28707(8) 0.0485(13) Uani 1 1 d . . . H64 H 0.5917 -0.1549 -0.2872 0.058 Uiso 1 1 calc R . . C65 C 0.8553(3) -0.14449(10) -0.17979(8) 0.0376(11) Uani 1 1 d . . . H65 H 0.8282 -0.162 -0.1716 0.045 Uiso 1 1 calc R . . C66 C 0.9173(3) -0.12633(11) -0.16668(8) 0.0407(12) Uani 1 1 d . . . C67 C 0.9215(3) -0.13169(11) -0.14124(8) 0.0430(12) Uani 1 1 d . . . H67 H 0.8826 -0.1465 -0.1339 0.052 Uiso 1 1 calc R . . C68 C 0.9811(3) -0.11549(12) -0.12771(9) 0.0445(13) Uani 1 1 d . . . H68 H 0.9816 -0.1178 -0.1108 0.053 Uiso 1 1 calc R . . C69 C 1.0421(3) -0.09522(11) -0.13920(9) 0.0447(13) Uani 1 1 d . . . H69 H 1.0856 -0.085 -0.1298 0.054 Uiso 1 1 calc R . . C70 C 1.0415(3) -0.08960(11) -0.16364(9) 0.0401(12) Uani 1 1 d . . . C71 C 0.9742(3) -0.10453(11) -0.17757(8) 0.0371(11) Uani 1 1 d . . . C72 C 1.1054(3) -0.06730(10) -0.17432(8) 0.0371(11) Uani 1 1 d . . . C73 C 1.0815(3) -0.04197(11) -0.18896(9) 0.0458(13) Uani 1 1 d . . . H73 H 1.0218 -0.0398 -0.193 0.055 Uiso 1 1 calc R . . C74 C 1.1397(4) -0.01948(12) -0.19808(10) 0.0548(14) Uani 1 1 d . . . H74 H 1.1203 -0.0022 -0.208 0.066 Uiso 1 1 calc R . . C75 C 1.2261(4) -0.02281(12) -0.19245(9) 0.0512(14) Uani 1 1 d . . . H75 H 1.2663 -0.0073 -0.1984 0.061 Uiso 1 1 calc R . . C76 C 1.2569(3) -0.04836(10) -0.17824(8) 0.0337(11) Uani 1 1 d . . . C77 C 1.1953(3) -0.07149(11) -0.16897(8) 0.0393(12) Uani 1 1 d . . . C78 C 1.3468(3) -0.04932(10) -0.17226(7) 0.0347(11) Uani 1 1 d . . . H78 H 1.3819 -0.0327 -0.179 0.042 Uiso 1 1 calc R . . C79 C 1.4799(3) -0.06423(10) -0.15469(8) 0.0346(11) Uani 1 1 d . . . H79 H 1.4937 -0.0422 -0.1612 0.042 Uiso 1 1 calc R . . C80 C 1.5382(3) -0.08870(11) -0.16773(8) 0.0388(12) Uani 1 1 d . . . H80A H 1.5255 -0.1109 -0.162 0.047 Uiso 1 1 calc R . . H80B H 1.5269 -0.0878 -0.1852 0.047 Uiso 1 1 calc R . . C81 C 1.6335(3) -0.08023(11) -0.16266(8) 0.0384(11) Uani 1 1 d . . . H81A H 1.6717 -0.0959 -0.171 0.046 Uiso 1 1 calc R . . H81B H 1.6463 -0.0583 -0.169 0.046 Uiso 1 1 calc R . . C82 C 1.5029(3) -0.06389(11) -0.12833(7) 0.0360(11) Uani 1 1 d . . . H82A H 1.4683 -0.047 -0.1201 0.043 Uiso 1 1 calc R . . H82B H 1.4882 -0.0851 -0.1211 0.043 Uiso 1 1 calc R . . C83 C 1.5982(3) -0.05712(11) -0.12474(8) 0.0381(12) Uani 1 1 d . . . H83A H 1.6119 -0.0351 -0.1307 0.046 Uiso 1 1 calc R . . H83B H 1.6119 -0.0578 -0.1074 0.046 Uiso 1 1 calc R . . C84 C 1.7420(3) -0.07402(12) -0.13276(8) 0.0419(12) Uani 1 1 d . . . H84A H 1.7518 -0.0505 -0.1353 0.05 Uiso 1 1 calc R . . H84B H 1.7776 -0.0858 -0.1447 0.05 Uiso 1 1 calc R . . C85 C 1.7741(3) -0.08278(13) -0.10821(9) 0.0495(14) Uani 1 1 d . . . C86 C 1.7512(4) -0.11202(14) -0.09829(10) 0.0680(18) Uani 1 1 d . . . H86 H 1.7141 -0.1263 -0.1069 0.082 Uiso 1 1 calc R . . C87 C 1.7816(6) -0.12112(17) -0.07566(12) 0.092(2) Uani 1 1 d . . . H87 H 1.7636 -0.141 -0.0686 0.11 Uiso 1 1 calc R . . C88 C 1.8381(5) -0.1008(2) -0.06378(11) 0.085(2) Uani 1 1 d . . . H88 H 1.8618 -0.1072 -0.0488 0.101 Uiso 1 1 calc R . . C89 C 1.8604(5) -0.0713(2) -0.07344(11) 0.082(2) Uani 1 1 d . . . H89 H 1.8979 -0.0571 -0.0649 0.098 Uiso 1 1 calc R . . C90 C 1.8281(4) -0.06221(15) -0.09582(10) 0.0616(15) Uani 1 1 d . . . H90 H 1.8435 -0.0418 -0.1025 0.074 Uiso 1 1 calc R . . C91 C 1.3657(3) -0.14704(10) -0.15913(9) 0.0449(12) Uani 1 1 d . . . H91A H 1.3168 -0.1619 -0.1615 0.067 Uiso 1 1 calc R . . H91B H 1.4088 -0.1573 -0.1486 0.067 Uiso 1 1 calc R . . H91C H 1.3926 -0.1421 -0.1746 0.067 Uiso 1 1 calc R . . C92 C 1.3155(4) -0.10483(14) -0.10970(8) 0.0563(15) Uani 1 1 d . . . H92A H 1.321 -0.0822 -0.1046 0.084 Uiso 1 1 calc R . . H92B H 1.362 -0.1177 -0.1024 0.084 Uiso 1 1 calc R . . H92C H 1.259 -0.1134 -0.1046 0.084 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 0.0246(9) 0.0307(7) 0.0397(7) -0.0017(6) 0.0000(6) 0.0004(6) Al2 0.0342(9) 0.0424(7) 0.0271(6) -0.0038(6) 0.0000(6) -0.0034(7) N1 0.026(2) 0.0302(18) 0.0368(19) 0.0018(15) 0.0038(17) -0.0002(17) N2 0.024(2) 0.036(2) 0.0305(19) -0.0019(15) 0.0040(15) -0.0018(16) N3 0.026(2) 0.040(2) 0.042(2) -0.0033(17) 0.0033(18) -0.0030(17) N4 0.024(2) 0.036(2) 0.0313(19) -0.0106(16) -0.0026(17) 0.0014(17) O1 0.022(2) 0.0286(15) 0.0536(19) -0.0087(14) 0.0049(14) -0.0037(13) O2 0.035(2) 0.0513(19) 0.0352(17) -0.0063(14) -0.0009(14) -0.0088(16) C1 0.035(3) 0.034(2) 0.054(3) -0.005(2) 0.000(2) 0.004(2) C2 0.042(4) 0.061(3) 0.053(3) 0.007(3) -0.008(3) -0.001(3) C3 0.029(3) 0.027(2) 0.039(2) 0.0010(18) 0.000(2) -0.007(2) C4 0.027(3) 0.038(3) 0.043(3) 0.014(2) 0.004(2) 0.008(2) C5 0.025(3) 0.042(3) 0.042(2) 0.004(2) 0.001(2) -0.001(2) C6 0.026(3) 0.044(3) 0.032(2) -0.003(2) -0.002(2) -0.002(2) C7 0.025(3) 0.045(3) 0.046(3) -0.003(2) -0.005(2) -0.004(2) C8 0.023(3) 0.053(3) 0.054(3) -0.008(2) 0.005(2) 0.002(2) C9 0.030(3) 0.064(4) 0.052(3) 0.009(3) 0.004(2) 0.013(3) C10 0.035(4) 0.116(5) 0.073(4) 0.028(4) 0.008(3) 0.015(4) C11 0.062(6) 0.172(9) 0.075(5) 0.065(5) 0.039(4) 0.053(6) C12 0.148(10) 0.155(9) 0.077(6) 0.015(6) 0.032(6) 0.102(8) C13 0.159(9) 0.091(6) 0.084(5) -0.006(4) 0.038(5) 0.059(6) C14 0.096(6) 0.066(4) 0.067(4) -0.002(3) 0.017(4) 0.030(4) C15 0.034(3) 0.028(2) 0.029(2) -0.0058(18) -0.003(2) -0.004(2) C16 0.025(3) 0.032(2) 0.037(2) 0.0011(19) 0.006(2) -0.004(2) C17 0.044(4) 0.037(3) 0.046(3) -0.014(2) -0.003(2) -0.005(2) C18 0.035(4) 0.048(3) 0.057(3) -0.018(2) 0.005(3) -0.002(3) C19 0.024(3) 0.046(3) 0.044(3) -0.005(2) 0.011(2) 0.001(2) C20 0.025(3) 0.028(2) 0.038(2) 0.0029(19) -0.002(2) -0.0007(19) C21 0.029(3) 0.028(2) 0.035(2) -0.0009(18) -0.001(2) 0.005(2) C22 0.025(3) 0.034(2) 0.037(2) -0.0023(19) 0.002(2) 0.008(2) C23 0.028(3) 0.034(2) 0.039(3) 0.001(2) 0.003(2) 0.000(2) C24 0.048(4) 0.048(3) 0.024(2) 0.000(2) 0.005(2) 0.002(3) C25 0.028(3) 0.037(2) 0.028(2) 0.0005(19) 0.001(2) 0.001(2) C26 0.010(2) 0.037(2) 0.036(2) -0.0039(19) -0.0019(19) 0.0023(19) C27 0.024(3) 0.034(2) 0.032(2) -0.0024(19) 0.003(2) 0.004(2) C28 0.023(3) 0.037(2) 0.036(2) -0.0035(19) 0.000(2) -0.002(2) C29 0.028(3) 0.033(2) 0.031(2) 0.0002(18) 0.0040(19) 0.000(2) C30 0.037(4) 0.052(3) 0.053(3) 0.000(2) 0.009(2) 0.012(2) C31 0.079(4) 0.043(3) 0.045(3) 0.012(2) 0.026(3) 0.016(3) C32 0.036(3) 0.043(3) 0.037(2) -0.002(2) 0.006(2) -0.006(2) C33 0.045(4) 0.043(3) 0.057(3) 0.000(2) 0.028(3) 0.001(3) C34 0.080(5) 0.041(3) 0.054(3) 0.012(2) 0.017(3) -0.015(3) C35 0.087(5) 0.067(4) 0.067(4) 0.004(3) 0.020(4) -0.019(4) C36 0.074(5) 0.090(5) 0.075(4) 0.002(4) -0.002(4) -0.017(4) C37 0.084(6) 0.116(6) 0.065(4) 0.031(4) -0.018(4) -0.022(5) C38 0.061(5) 0.067(4) 0.110(6) 0.026(4) -0.010(4) 0.001(4) C39 0.081(6) 0.067(4) 0.096(5) 0.015(4) -0.021(4) 0.012(4) C40 0.085(6) 0.070(4) 0.092(5) 0.009(4) 0.019(4) 0.000(4) C41 0.057(4) 0.053(3) 0.032(2) -0.004(2) 0.000(2) -0.003(3) C42 0.057(4) 0.037(3) 0.047(3) -0.010(2) -0.016(3) 0.000(2) Al3 0.0343(10) 0.0402(8) 0.0470(8) -0.0012(6) 0.0028(7) -0.0023(7) Al4 0.0293(9) 0.0384(8) 0.0375(7) 0.0001(6) -0.0014(6) -0.0040(6) N5 0.029(3) 0.039(2) 0.036(2) 0.0002(16) -0.0017(17) -0.0020(18) N6 0.072(3) 0.041(2) 0.044(2) 0.0093(19) 0.023(2) 0.015(2) N7 0.032(3) 0.0314(19) 0.042(2) -0.0073(17) -0.0063(18) -0.0004(18) N8 0.017(2) 0.039(2) 0.041(2) -0.0062(16) 0.0056(16) 0.0045(17) O3 0.037(2) 0.053(2) 0.0380(18) -0.0041(15) 0.0045(15) -0.0060(16) O4 0.023(2) 0.0369(17) 0.0476(18) 0.0004(15) -0.0037(14) -0.0025(14) C51 0.054(4) 0.070(4) 0.056(3) -0.001(3) 0.000(3) 0.000(3) C52 0.046(4) 0.040(3) 0.072(3) -0.003(2) 0.013(3) 0.005(3) C53 0.027(3) 0.035(2) 0.049(3) 0.001(2) -0.002(2) 0.002(2) C54 0.028(3) 0.039(3) 0.051(3) -0.006(2) -0.003(2) 0.007(2) C55 0.052(4) 0.034(3) 0.050(3) -0.002(2) -0.002(3) 0.004(2) C56 0.031(3) 0.040(3) 0.042(3) -0.012(2) -0.004(2) 0.003(2) C57 0.036(3) 0.046(3) 0.045(3) -0.005(2) 0.003(2) -0.004(2) C58 0.051(4) 0.026(2) 0.057(3) 0.001(2) -0.003(2) -0.008(2) C59 0.037(3) 0.028(2) 0.036(2) -0.0043(18) -0.007(2) -0.002(2) C60 0.052(4) 0.051(3) 0.043(3) -0.007(2) 0.000(3) -0.007(3) C61 0.051(4) 0.066(4) 0.058(3) -0.021(3) -0.010(3) -0.002(3) C62 0.048(4) 0.078(4) 0.049(3) -0.013(3) -0.014(3) 0.011(3) C63 0.080(5) 0.050(3) 0.046(3) 0.003(2) 0.008(3) 0.023(3) C64 0.057(4) 0.048(3) 0.040(3) -0.004(2) 0.006(3) 0.007(3) C65 0.031(3) 0.033(2) 0.049(3) 0.002(2) 0.005(2) 0.003(2) C66 0.032(3) 0.041(3) 0.049(3) -0.006(2) -0.003(2) 0.005(2) C67 0.033(3) 0.043(3) 0.053(3) 0.001(2) 0.007(2) 0.004(2) C68 0.031(3) 0.052(3) 0.051(3) -0.010(2) 0.001(2) 0.007(3) C69 0.030(3) 0.044(3) 0.060(3) -0.022(2) 0.000(2) 0.004(2) C70 0.024(3) 0.043(3) 0.053(3) -0.014(2) 0.003(2) 0.011(2) C71 0.030(3) 0.037(2) 0.045(3) -0.003(2) 0.002(2) 0.008(2) C72 0.024(3) 0.034(2) 0.054(3) -0.017(2) -0.001(2) 0.000(2) C73 0.025(3) 0.037(3) 0.075(3) -0.005(2) -0.012(3) -0.001(2) C74 0.036(4) 0.049(3) 0.080(4) 0.005(3) -0.015(3) 0.005(3) C75 0.043(4) 0.043(3) 0.067(3) 0.006(3) 0.001(3) -0.005(3) C76 0.022(3) 0.036(2) 0.043(3) -0.004(2) 0.001(2) 0.000(2) C77 0.040(4) 0.041(3) 0.038(2) -0.011(2) -0.002(2) 0.002(2) C78 0.029(3) 0.035(2) 0.041(2) -0.009(2) 0.004(2) -0.001(2) C79 0.026(3) 0.034(2) 0.044(3) -0.003(2) 0.002(2) -0.003(2) C80 0.041(3) 0.039(3) 0.036(2) -0.013(2) 0.004(2) -0.001(2) C81 0.025(3) 0.046(3) 0.044(3) -0.008(2) 0.007(2) -0.003(2) C82 0.026(3) 0.049(3) 0.033(2) -0.010(2) 0.004(2) 0.002(2) C83 0.025(3) 0.047(3) 0.042(3) -0.014(2) -0.002(2) 0.003(2) C84 0.023(3) 0.050(3) 0.053(3) -0.006(2) 0.002(2) 0.008(2) C85 0.039(4) 0.065(4) 0.045(3) -0.007(3) -0.004(2) 0.014(3) C86 0.092(6) 0.056(4) 0.056(4) 0.004(3) -0.006(3) 0.011(3) C87 0.123(7) 0.072(5) 0.080(5) 0.015(4) -0.013(5) 0.023(4) C88 0.093(6) 0.114(6) 0.046(3) -0.015(4) -0.014(4) 0.063(5) C89 0.068(5) 0.118(6) 0.060(4) -0.037(4) -0.005(4) 0.026(5) C90 0.044(4) 0.073(4) 0.068(4) -0.015(3) -0.008(3) 0.002(3) C91 0.025(3) 0.038(3) 0.072(3) 0.001(2) -0.005(3) -0.004(2) C92 0.043(4) 0.076(4) 0.049(3) 0.008(3) -0.009(3) -0.013(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.769(3) . ? Al1 C1 1.948(4) . ? Al1 N1 1.973(4) . ? Al1 C2 1.983(5) . ? Al2 O2 1.778(3) . ? Al2 C41 1.939(4) . ? Al2 C42 1.957(5) . ? Al2 N2 1.975(4) . ? N1 C15 1.277(5) . ? N1 C3 1.507(6) . ? N2 C28 1.283(5) . ? N2 C29 1.484(5) . ? N3 C65 1.303(5) . ? N3 C53 1.491(6) . ? N3 Al3 1.954(4) . ? N4 C78 1.289(5) . ? N4 C79 1.479(5) . ? N4 Al4 1.975(4) . ? O1 C21 1.325(5) . ? O2 C27 1.337(5) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 C6 1.510(6) . ? C3 C4 1.511(5) . ? C3 H3 1 . ? C4 C5 1.518(6) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 N5 1.454(5) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.497(6) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 N5 1.482(5) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N5 1.487(6) . ? C8 C9 1.507(6) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C14 1.345(8) . ? C9 C10 1.360(8) . ? C10 C11 1.391(9) . ? C10 H10 0.95 . ? C11 C12 1.325(12) . ? C11 H11 0.95 . ? C12 C13 1.435(13) . ? C12 H12 0.95 . ? C13 C14 1.381(8) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 C16 1.423(6) . ? C15 H15 0.95 . ? C16 C17 1.401(6) . ? C16 C21 1.429(6) . ? C17 C18 1.389(7) . ? C17 H17 0.95 . ? C18 C19 1.374(6) . ? C18 H18 0.95 . ? C19 C20 1.394(6) . ? C19 H19 0.95 . ? C20 C21 1.385(6) . ? C20 C22 1.497(6) . ? C22 C27 1.385(6) . ? C22 C23 1.394(6) . ? C23 C24 1.358(6) . ? C23 H23 0.95 . ? C24 C25 1.373(6) . ? C24 H24 0.95 . ? C25 C26 1.405(5) . ? C25 H25 0.95 . ? C26 C27 1.419(6) . ? C26 C28 1.446(6) . ? C28 H28 0.95 . ? C29 C32 1.507(6) . ? C29 C30 1.515(6) . ? C29 H29 1 . ? C30 C31 1.499(7) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 N6 1.477(6) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.524(6) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 N6 1.444(6) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 N6 1.459(6) . ? C34 C35 1.576(8) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 C36 1.414(8) . ? C35 C40 1.415(8) . ? C36 C37 1.344(8) . ? C36 H36 0.95 . ? C37 C38 1.375(9) . ? C37 H37 0.95 . ? C38 C39 1.294(9) . ? C38 H38 0.95 . ? C39 C40 1.400(9) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? Al3 O3 1.771(4) . ? Al3 C51 1.955(5) . ? Al3 C52 1.958(5) . ? Al4 O4 1.769(3) . ? Al4 C91 1.938(5) . ? Al4 C92 1.953(5) . ? N7 C58 1.455(5) . ? N7 C57 1.465(5) . ? N7 C55 1.467(6) . ? N8 C81 1.439(5) . ? N8 C84 1.443(6) . ? N8 C83 1.465(5) . ? O3 C71 1.318(5) . ? O4 C77 1.311(5) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 C56 1.522(6) . ? C53 C54 1.541(6) . ? C53 H53 1 . ? C54 C55 1.505(6) . ? C54 H54A 0.99 . ? C54 H54B 0.99 . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 C57 1.510(6) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 C59 1.495(6) . ? C58 H58A 0.99 . ? C58 H58B 0.99 . ? C59 C64 1.385(6) . ? C59 C60 1.384(7) . ? C60 C61 1.391(7) . ? C60 H60 0.95 . ? C61 C62 1.347(7) . ? C61 H61 0.95 . ? C62 C63 1.370(8) . ? C62 H62 0.95 . ? C63 C64 1.406(7) . ? C63 H63 0.95 . ? C64 H64 0.95 . ? C65 C66 1.417(6) . ? C65 H65 0.95 . ? C66 C71 1.394(7) . ? C66 C67 1.439(6) . ? C67 C68 1.364(7) . ? C67 H67 0.95 . ? C68 C69 1.411(7) . ? C68 H68 0.95 . ? C69 C70 1.385(6) . ? C69 H69 0.95 . ? C70 C71 1.434(7) . ? C70 C72 1.472(6) . ? C72 C73 1.376(6) . ? C72 C77 1.426(6) . ? C73 C74 1.387(7) . ? C73 H73 0.95 . ? C74 C75 1.373(7) . ? C74 H74 0.95 . ? C75 C76 1.401(6) . ? C75 H75 0.95 . ? C76 C78 1.424(6) . ? C76 C77 1.441(6) . ? C78 H78 0.95 . ? C79 C82 1.515(6) . ? C79 C80 1.534(6) . ? C79 H79 1 . ? C80 C81 1.534(6) . ? C80 H80A 0.99 . ? C80 H80B 0.99 . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C82 C83 1.506(6) . ? C82 H82A 0.99 . ? C82 H82B 0.99 . ? C83 H83A 0.99 . ? C83 H83B 0.99 . ? C84 C85 1.501(6) . ? C84 H84A 0.99 . ? C84 H84B 0.99 . ? C85 C86 1.372(7) . ? C85 C90 1.375(7) . ? C86 C87 1.399(8) . ? C86 H86 0.95 . ? C87 C88 1.378(10) . ? C87 H87 0.95 . ? C88 C89 1.372(9) . ? C88 H88 0.95 . ? C89 C90 1.397(8) . ? C89 H89 0.95 . ? C90 H90 0.95 . ? C91 H91A 0.98 . ? C91 H91B 0.98 . ? C91 H91C 0.98 . ? C92 H92A 0.98 . ? C92 H92B 0.98 . ? C92 H92C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 C1 112.16(19) . . ? O1 Al1 N1 94.40(15) . . ? C1 Al1 N1 110.84(18) . . ? O1 Al1 C2 108.4(2) . . ? C1 Al1 C2 115.4(2) . . ? N1 Al1 C2 113.78(19) . . ? O2 Al2 C41 108.5(2) . . ? O2 Al2 C42 111.2(2) . . ? C41 Al2 C42 120.6(2) . . ? O2 Al2 N2 94.36(14) . . ? C41 Al2 N2 115.28(18) . . ? C42 Al2 N2 103.80(18) . . ? C15 N1 C3 116.7(3) . . ? C15 N1 Al1 121.3(3) . . ? C3 N1 Al1 122.0(3) . . ? C28 N2 C29 117.2(3) . . ? C28 N2 Al2 117.9(3) . . ? C29 N2 Al2 124.8(3) . . ? C65 N3 C53 116.1(4) . . ? C65 N3 Al3 119.4(3) . . ? C53 N3 Al3 124.3(3) . . ? C78 N4 C79 116.3(4) . . ? C78 N4 Al4 121.5(3) . . ? C79 N4 Al4 122.1(3) . . ? C21 O1 Al1 132.0(3) . . ? C27 O2 Al2 124.1(3) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C6 111.2(3) . . ? N1 C3 C4 110.1(3) . . ? C6 C3 C4 110.7(4) . . ? N1 C3 H3 108.2 . . ? C6 C3 H3 108.2 . . ? C4 C3 H3 108.2 . . ? C3 C4 C5 109.0(4) . . ? C3 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N5 C5 C4 109.7(3) . . ? N5 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? N5 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C7 C6 C3 110.3(4) . . ? C7 C6 H6A 109.6 . . ? C3 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? C3 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N5 C7 C6 109.5(4) . . ? N5 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N5 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N5 C8 C9 111.1(4) . . ? N5 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N5 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108 . . ? C14 C9 C10 118.0(6) . . ? C14 C9 C8 120.4(5) . . ? C10 C9 C8 121.5(5) . . ? C9 C10 C11 121.4(7) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 120.5(8) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.8(8) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 116.8(8) . . ? C14 C13 H13 121.6 . . ? C12 C13 H13 121.6 . . ? C9 C14 C13 123.3(7) . . ? C9 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? N1 C15 C16 128.2(4) . . ? N1 C15 H15 115.9 . . ? C16 C15 H15 115.9 . . ? C17 C16 C15 118.3(4) . . ? C17 C16 C21 118.8(4) . . ? C15 C16 C21 122.9(4) . . ? C18 C17 C16 121.0(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 122.7(5) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C21 C20 C19 118.8(4) . . ? C21 C20 C22 120.9(4) . . ? C19 C20 C22 120.3(4) . . ? O1 C21 C20 120.5(4) . . ? O1 C21 C16 119.5(4) . . ? C20 C21 C16 119.9(4) . . ? C27 C22 C23 118.8(4) . . ? C27 C22 C20 120.9(4) . . ? C23 C22 C20 120.2(4) . . ? C24 C23 C22 122.7(4) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 118.9(4) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C24 C25 C26 121.2(4) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 118.5(4) . . ? C25 C26 C28 118.1(4) . . ? C27 C26 C28 123.2(4) . . ? O2 C27 C22 120.3(4) . . ? O2 C27 C26 120.0(4) . . ? C22 C27 C26 119.7(4) . . ? N2 C28 C26 126.2(4) . . ? N2 C28 H28 116.9 . . ? C26 C28 H28 116.9 . . ? N2 C29 C32 111.8(3) . . ? N2 C29 C30 109.9(4) . . ? C32 C29 C30 110.1(4) . . ? N2 C29 H29 108.3 . . ? C32 C29 H29 108.3 . . ? C30 C29 H29 108.3 . . ? C31 C30 C29 110.6(4) . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? N6 C31 C30 109.5(4) . . ? N6 C31 H31A 109.8 . . ? C30 C31 H31A 109.8 . . ? N6 C31 H31B 109.8 . . ? C30 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? C29 C32 C33 109.6(4) . . ? C29 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C29 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? N6 C33 C32 111.4(4) . . ? N6 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? N6 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108 . . ? N6 C34 C35 109.0(5) . . ? N6 C34 H34A 109.9 . . ? C35 C34 H34A 109.9 . . ? N6 C34 H34B 109.9 . . ? C35 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? C36 C35 C40 115.3(7) . . ? C36 C35 C34 123.5(6) . . ? C40 C35 C34 121.1(6) . . ? C37 C36 C35 121.1(7) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 121.1(7) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C37 120.9(7) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 120.8(7) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C39 C40 C35 120.7(7) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? Al2 C41 H41A 109.5 . . ? Al2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Al2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Al2 C42 H42A 109.5 . . ? Al2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Al2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3 Al3 N3 94.55(16) . . ? O3 Al3 C51 110.9(2) . . ? N3 Al3 C51 113.9(2) . . ? O3 Al3 C52 110.2(2) . . ? N3 Al3 C52 107.9(2) . . ? C51 Al3 C52 117.1(2) . . ? O4 Al4 C91 110.38(18) . . ? O4 Al4 C92 107.3(2) . . ? C91 Al4 C92 119.1(2) . . ? O4 Al4 N4 94.70(15) . . ? C91 Al4 N4 109.20(18) . . ? C92 Al4 N4 113.4(2) . . ? C5 N5 C7 110.5(3) . . ? C5 N5 C8 110.4(3) . . ? C7 N5 C8 109.7(3) . . ? C33 N6 C34 111.4(4) . . ? C33 N6 C31 111.1(4) . . ? C34 N6 C31 110.6(4) . . ? C58 N7 C57 110.6(4) . . ? C58 N7 C55 110.9(3) . . ? C57 N7 C55 110.2(3) . . ? C81 N8 C84 111.0(3) . . ? C81 N8 C83 110.5(3) . . ? C84 N8 C83 108.8(3) . . ? C71 O3 Al3 125.8(3) . . ? C77 O4 Al4 132.7(3) . . ? Al3 C51 H51A 109.5 . . ? Al3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Al3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Al3 C52 H52A 109.5 . . ? Al3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Al3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N3 C53 C56 111.1(3) . . ? N3 C53 C54 111.9(4) . . ? C56 C53 C54 109.3(4) . . ? N3 C53 H53 108.1 . . ? C56 C53 H53 108.1 . . ? C54 C53 H53 108.1 . . ? C55 C54 C53 109.1(4) . . ? C55 C54 H54A 109.9 . . ? C53 C54 H54A 109.9 . . ? C55 C54 H54B 109.9 . . ? C53 C54 H54B 109.9 . . ? H54A C54 H54B 108.3 . . ? N7 C55 C54 112.3(4) . . ? N7 C55 H55A 109.1 . . ? C54 C55 H55A 109.1 . . ? N7 C55 H55B 109.1 . . ? C54 C55 H55B 109.1 . . ? H55A C55 H55B 107.9 . . ? C57 C56 C53 110.6(4) . . ? C57 C56 H56A 109.5 . . ? C53 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 108.1 . . ? N7 C57 C56 111.4(4) . . ? N7 C57 H57A 109.4 . . ? C56 C57 H57A 109.4 . . ? N7 C57 H57B 109.4 . . ? C56 C57 H57B 109.4 . . ? H57A C57 H57B 108 . . ? N7 C58 C59 115.0(3) . . ? N7 C58 H58A 108.5 . . ? C59 C58 H58A 108.5 . . ? N7 C58 H58B 108.5 . . ? C59 C58 H58B 108.5 . . ? H58A C58 H58B 107.5 . . ? C64 C59 C60 118.9(5) . . ? C64 C59 C58 121.6(4) . . ? C60 C59 C58 119.5(4) . . ? C59 C60 C61 120.4(5) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C62 C61 C60 119.9(6) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C61 C62 C63 121.7(6) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C62 C63 C64 118.9(5) . . ? C62 C63 H63 120.5 . . ? C64 C63 H63 120.6 . . ? C59 C64 C63 120.2(5) . . ? C59 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? N3 C65 C66 126.7(4) . . ? N3 C65 H65 116.7 . . ? C66 C65 H65 116.7 . . ? C71 C66 C65 122.5(4) . . ? C71 C66 C67 120.1(4) . . ? C65 C66 C67 117.3(4) . . ? C68 C67 C66 120.1(5) . . ? C68 C67 H67 119.9 . . ? C66 C67 H67 119.9 . . ? C67 C68 C69 119.1(5) . . ? C67 C68 H68 120.5 . . ? C69 C68 H68 120.5 . . ? C70 C69 C68 122.9(5) . . ? C70 C69 H69 118.6 . . ? C68 C69 H69 118.6 . . ? C69 C70 C71 117.9(5) . . ? C69 C70 C72 119.9(4) . . ? C71 C70 C72 122.0(4) . . ? O3 C71 C66 121.9(4) . . ? O3 C71 C70 118.4(4) . . ? C66 C71 C70 119.5(4) . . ? C73 C72 C77 118.4(4) . . ? C73 C72 C70 122.4(4) . . ? C77 C72 C70 119.2(4) . . ? C72 C73 C74 123.5(5) . . ? C72 C73 H73 118.2 . . ? C74 C73 H73 118.2 . . ? C75 C74 C73 118.4(5) . . ? C75 C74 H74 120.8 . . ? C73 C74 H74 120.8 . . ? C74 C75 C76 122.1(5) . . ? C74 C75 H75 118.9 . . ? C76 C75 H75 118.9 . . ? C75 C76 C78 118.8(4) . . ? C75 C76 C77 118.6(4) . . ? C78 C76 C77 122.5(4) . . ? O4 C77 C72 120.7(4) . . ? O4 C77 C76 120.4(4) . . ? C72 C77 C76 118.9(4) . . ? N4 C78 C76 127.8(4) . . ? N4 C78 H78 116.1 . . ? C76 C78 H78 116.1 . . ? N4 C79 C82 112.4(3) . . ? N4 C79 C80 113.0(3) . . ? C82 C79 C80 109.3(4) . . ? N4 C79 H79 107.3 . . ? C82 C79 H79 107.3 . . ? C80 C79 H79 107.3 . . ? C81 C80 C79 108.8(4) . . ? C81 C80 H80A 109.9 . . ? C79 C80 H80A 109.9 . . ? C81 C80 H80B 109.9 . . ? C79 C80 H80B 109.9 . . ? H80A C80 H80B 108.3 . . ? N8 C81 C80 111.2(4) . . ? N8 C81 H81A 109.4 . . ? C80 C81 H81A 109.4 . . ? N8 C81 H81B 109.4 . . ? C80 C81 H81B 109.4 . . ? H81A C81 H81B 108 . . ? C83 C82 C79 111.0(4) . . ? C83 C82 H82A 109.4 . . ? C79 C82 H82A 109.4 . . ? C83 C82 H82B 109.4 . . ? C79 C82 H82B 109.4 . . ? H82A C82 H82B 108 . . ? N8 C83 C82 111.0(3) . . ? N8 C83 H83A 109.4 . . ? C82 C83 H83A 109.4 . . ? N8 C83 H83B 109.4 . . ? C82 C83 H83B 109.4 . . ? H83A C83 H83B 108 . . ? N8 C84 C85 115.7(4) . . ? N8 C84 H84A 108.4 . . ? C85 C84 H84A 108.4 . . ? N8 C84 H84B 108.4 . . ? C85 C84 H84B 108.4 . . ? H84A C84 H84B 107.4 . . ? C86 C85 C90 119.6(5) . . ? C86 C85 C84 119.7(5) . . ? C90 C85 C84 120.7(5) . . ? C85 C86 C87 121.0(6) . . ? C85 C86 H86 119.5 . . ? C87 C86 H86 119.5 . . ? C88 C87 C86 118.9(7) . . ? C88 C87 H87 120.6 . . ? C86 C87 H87 120.6 . . ? C89 C88 C87 120.4(6) . . ? C89 C88 H88 119.8 . . ? C87 C88 H88 119.8 . . ? C88 C89 C90 120.1(6) . . ? C88 C89 H89 120 . . ? C90 C89 H89 120 . . ? C85 C90 C89 120.0(6) . . ? C85 C90 H90 120 . . ? C89 C90 H90 120 . . ? Al4 C91 H91A 109.5 . . ? Al4 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? Al4 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? Al4 C92 H92A 109.5 . . ? Al4 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? Al4 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 N1 C15 6.1(3) . . . . ? C1 Al1 N1 C15 121.8(3) . . . . ? C2 Al1 N1 C15 -106.2(4) . . . . ? O1 Al1 N1 C3 -174.8(3) . . . . ? C1 Al1 N1 C3 -59.1(3) . . . . ? C2 Al1 N1 C3 72.9(3) . . . . ? O2 Al2 N2 C28 30.3(3) . . . . ? C41 Al2 N2 C28 143.1(3) . . . . ? C42 Al2 N2 C28 -82.8(4) . . . . ? O2 Al2 N2 C29 -153.8(3) . . . . ? C41 Al2 N2 C29 -41.0(4) . . . . ? C42 Al2 N2 C29 93.1(3) . . . . ? C1 Al1 O1 C21 -129.4(4) . . . . ? N1 Al1 O1 C21 -14.8(4) . . . . ? C2 Al1 O1 C21 102.1(4) . . . . ? C41 Al2 O2 C27 -159.8(3) . . . . ? C42 Al2 O2 C27 65.3(4) . . . . ? N2 Al2 O2 C27 -41.3(3) . . . . ? C15 N1 C3 C6 -105.2(4) . . . . ? Al1 N1 C3 C6 75.7(4) . . . . ? C15 N1 C3 C4 131.7(4) . . . . ? Al1 N1 C3 C4 -47.4(4) . . . . ? N1 C3 C4 C5 179.3(3) . . . . ? C6 C3 C4 C5 55.8(5) . . . . ? C3 C4 C5 N5 -59.1(5) . . . . ? N1 C3 C6 C7 -178.7(3) . . . . ? C4 C3 C6 C7 -55.9(5) . . . . ? C3 C6 C7 N5 57.6(5) . . . . ? N5 C8 C9 C14 49.5(6) . . . . ? N5 C8 C9 C10 -133.9(5) . . . . ? C14 C9 C10 C11 1.7(9) . . . . ? C8 C9 C10 C11 -174.9(5) . . . . ? C9 C10 C11 C12 -2.4(11) . . . . ? C10 C11 C12 C13 -0.8(13) . . . . ? C11 C12 C13 C14 4.3(13) . . . . ? C10 C9 C14 C13 2.2(10) . . . . ? C8 C9 C14 C13 178.8(6) . . . . ? C12 C13 C14 C9 -5.2(11) . . . . ? C3 N1 C15 C16 -179.1(4) . . . . ? Al1 N1 C15 C16 0.0(6) . . . . ? N1 C15 C16 C17 176.1(4) . . . . ? N1 C15 C16 C21 -1.9(7) . . . . ? C15 C16 C17 C18 -177.8(4) . . . . ? C21 C16 C17 C18 0.4(7) . . . . ? C16 C17 C18 C19 1.5(7) . . . . ? C17 C18 C19 C20 -0.7(7) . . . . ? C18 C19 C20 C21 -2.1(7) . . . . ? C18 C19 C20 C22 176.8(4) . . . . ? Al1 O1 C21 C20 -164.4(3) . . . . ? Al1 O1 C21 C16 16.0(6) . . . . ? C19 C20 C21 O1 -175.7(4) . . . . ? C22 C20 C21 O1 5.4(6) . . . . ? C19 C20 C21 C16 3.9(6) . . . . ? C22 C20 C21 C16 -174.9(4) . . . . ? C17 C16 C21 O1 176.5(4) . . . . ? C15 C16 C21 O1 -5.4(6) . . . . ? C17 C16 C21 C20 -3.1(6) . . . . ? C15 C16 C21 C20 174.9(4) . . . . ? C21 C20 C22 C27 -127.7(4) . . . . ? C19 C20 C22 C27 53.5(6) . . . . ? C21 C20 C22 C23 56.6(6) . . . . ? C19 C20 C22 C23 -122.2(5) . . . . ? C27 C22 C23 C24 0.7(7) . . . . ? C20 C22 C23 C24 176.5(4) . . . . ? C22 C23 C24 C25 3.5(7) . . . . ? C23 C24 C25 C26 -4.2(7) . . . . ? C24 C25 C26 C27 0.7(6) . . . . ? C24 C25 C26 C28 175.0(4) . . . . ? Al2 O2 C27 C22 -154.8(3) . . . . ? Al2 O2 C27 C26 28.4(5) . . . . ? C23 C22 C27 O2 179.0(4) . . . . ? C20 C22 C27 O2 3.3(6) . . . . ? C23 C22 C27 C26 -4.2(6) . . . . ? C20 C22 C27 C26 -180.0(4) . . . . ? C25 C26 C27 O2 -179.7(4) . . . . ? C28 C26 C27 O2 6.3(6) . . . . ? C25 C26 C27 C22 3.6(6) . . . . ? C28 C26 C27 C22 -170.5(4) . . . . ? C29 N2 C28 C26 175.4(4) . . . . ? Al2 N2 C28 C26 -8.4(6) . . . . ? C25 C26 C28 N2 170.5(4) . . . . ? C27 C26 C28 N2 -15.4(7) . . . . ? C28 N2 C29 C32 128.9(4) . . . . ? Al2 N2 C29 C32 -47.0(5) . . . . ? C28 N2 C29 C30 -108.5(4) . . . . ? Al2 N2 C29 C30 75.5(4) . . . . ? N2 C29 C30 C31 179.8(3) . . . . ? C32 C29 C30 C31 -56.7(5) . . . . ? C29 C30 C31 N6 58.5(5) . . . . ? N2 C29 C32 C33 176.9(4) . . . . ? C30 C29 C32 C33 54.4(5) . . . . ? C29 C32 C33 N6 -56.6(5) . . . . ? N6 C34 C35 C36 -65.2(7) . . . . ? N6 C34 C35 C40 119.0(6) . . . . ? C40 C35 C36 C37 0.8(9) . . . . ? C34 C35 C36 C37 -175.2(6) . . . . ? C35 C36 C37 C38 -3.4(11) . . . . ? C36 C37 C38 C39 3.5(11) . . . . ? C37 C38 C39 C40 -0.9(11) . . . . ? C38 C39 C40 C35 -1.7(11) . . . . ? C36 C35 C40 C39 1.7(9) . . . . ? C34 C35 C40 C39 177.8(6) . . . . ? C65 N3 Al3 O3 21.5(4) . . . . ? C53 N3 Al3 O3 -164.0(3) . . . . ? C65 N3 Al3 C51 136.8(4) . . . . ? C53 N3 Al3 C51 -48.7(4) . . . . ? C65 N3 Al3 C52 -91.4(4) . . . . ? C53 N3 Al3 C52 83.1(4) . . . . ? C78 N4 Al4 O4 -1.8(3) . . . . ? C79 N4 Al4 O4 178.0(3) . . . . ? C78 N4 Al4 C91 111.7(3) . . . . ? C79 N4 Al4 C91 -68.5(3) . . . . ? C78 N4 Al4 C92 -113.0(3) . . . . ? C79 N4 Al4 C92 66.8(4) . . . . ? C4 C5 N5 C7 62.5(4) . . . . ? C4 C5 N5 C8 -176.0(3) . . . . ? C6 C7 N5 C5 -61.6(5) . . . . ? C6 C7 N5 C8 176.5(4) . . . . ? C9 C8 N5 C5 70.1(5) . . . . ? C9 C8 N5 C7 -167.9(4) . . . . ? C32 C33 N6 C34 -176.6(4) . . . . ? C32 C33 N6 C31 59.6(5) . . . . ? C35 C34 N6 C33 175.1(4) . . . . ? C35 C34 N6 C31 -60.9(6) . . . . ? C30 C31 N6 C33 -60.2(6) . . . . ? C30 C31 N6 C34 175.5(4) . . . . ? N3 Al3 O3 C71 -33.9(4) . . . . ? C51 Al3 O3 C71 -151.7(4) . . . . ? C52 Al3 O3 C71 77.0(4) . . . . ? C91 Al4 O4 C77 -116.2(4) . . . . ? C92 Al4 O4 C77 112.6(4) . . . . ? N4 Al4 O4 C77 -3.7(4) . . . . ? C65 N3 C53 C56 125.4(4) . . . . ? Al3 N3 C53 C56 -49.2(5) . . . . ? C65 N3 C53 C54 -112.1(4) . . . . ? Al3 N3 C53 C54 73.2(4) . . . . ? N3 C53 C54 C55 -178.9(4) . . . . ? C56 C53 C54 C55 -55.5(5) . . . . ? C58 N7 C55 C54 177.6(4) . . . . ? C57 N7 C55 C54 -59.5(5) . . . . ? C53 C54 C55 N7 58.2(5) . . . . ? N3 C53 C56 C57 179.7(4) . . . . ? C54 C53 C56 C57 55.7(5) . . . . ? C58 N7 C57 C56 -178.7(4) . . . . ? C55 N7 C57 C56 58.3(5) . . . . ? C53 C56 C57 N7 -57.6(5) . . . . ? C57 N7 C58 C59 67.9(5) . . . . ? C55 N7 C58 C59 -169.5(4) . . . . ? N7 C58 C59 C64 33.9(6) . . . . ? N7 C58 C59 C60 -148.2(4) . . . . ? C64 C59 C60 C61 2.6(7) . . . . ? C58 C59 C60 C61 -175.3(4) . . . . ? C59 C60 C61 C62 -2.6(7) . . . . ? C60 C61 C62 C63 1.2(8) . . . . ? C61 C62 C63 C64 0.1(8) . . . . ? C60 C59 C64 C63 -1.3(6) . . . . ? C58 C59 C64 C63 176.6(4) . . . . ? C62 C63 C64 C59 -0.1(7) . . . . ? C53 N3 C65 C66 -178.0(4) . . . . ? Al3 N3 C65 C66 -3.1(6) . . . . ? N3 C65 C66 C71 -13.2(7) . . . . ? N3 C65 C66 C67 168.2(4) . . . . ? C71 C66 C67 C68 -0.1(7) . . . . ? C65 C66 C67 C68 178.5(4) . . . . ? C66 C67 C68 C69 -4.3(7) . . . . ? C67 C68 C69 C70 3.5(7) . . . . ? C68 C69 C70 C71 1.6(7) . . . . ? C68 C69 C70 C72 178.0(4) . . . . ? Al3 O3 C71 C66 26.8(6) . . . . ? Al3 O3 C71 C70 -158.0(3) . . . . ? C65 C66 C71 O3 1.9(7) . . . . ? C67 C66 C71 O3 -179.6(4) . . . . ? C65 C66 C71 C70 -173.3(4) . . . . ? C67 C66 C71 C70 5.3(7) . . . . ? C69 C70 C71 O3 178.7(4) . . . . ? C72 C70 C71 O3 2.5(6) . . . . ? C69 C70 C71 C66 -5.9(6) . . . . ? C72 C70 C71 C66 177.8(4) . . . . ? C69 C70 C72 C73 -127.7(5) . . . . ? C71 C70 C72 C73 48.5(6) . . . . ? C69 C70 C72 C77 50.9(6) . . . . ? C71 C70 C72 C77 -132.9(4) . . . . ? C77 C72 C73 C74 -2.6(7) . . . . ? C70 C72 C73 C74 176.0(4) . . . . ? C72 C73 C74 C75 0.7(8) . . . . ? C73 C74 C75 C76 1.1(8) . . . . ? C74 C75 C76 C78 -177.1(5) . . . . ? C74 C75 C76 C77 -1.0(7) . . . . ? Al4 O4 C77 C72 -173.8(3) . . . . ? Al4 O4 C77 C76 8.1(6) . . . . ? C73 C72 C77 O4 -175.6(4) . . . . ? C70 C72 C77 O4 5.8(6) . . . . ? C73 C72 C77 C76 2.6(6) . . . . ? C70 C72 C77 C76 -176.1(4) . . . . ? C75 C76 C77 O4 177.3(4) . . . . ? C78 C76 C77 O4 -6.8(6) . . . . ? C75 C76 C77 C72 -0.8(6) . . . . ? C78 C76 C77 C72 175.1(4) . . . . ? C79 N4 C78 C76 -177.1(4) . . . . ? Al4 N4 C78 C76 2.7(6) . . . . ? C75 C76 C78 N4 177.3(4) . . . . ? C77 C76 C78 N4 1.4(7) . . . . ? C78 N4 C79 C82 127.3(4) . . . . ? Al4 N4 C79 C82 -52.6(4) . . . . ? C78 N4 C79 C80 -108.5(4) . . . . ? Al4 N4 C79 C80 71.7(4) . . . . ? N4 C79 C80 C81 179.0(3) . . . . ? C82 C79 C80 C81 -55.0(5) . . . . ? C84 N8 C81 C80 178.2(4) . . . . ? C83 N8 C81 C80 -61.1(5) . . . . ? C79 C80 C81 N8 59.0(5) . . . . ? N4 C79 C82 C83 -178.6(3) . . . . ? C80 C79 C82 C83 55.1(5) . . . . ? C81 N8 C83 C82 59.7(5) . . . . ? C84 N8 C83 C82 -178.2(4) . . . . ? C79 C82 C83 N8 -57.1(5) . . . . ? C81 N8 C84 C85 -164.1(4) . . . . ? C83 N8 C84 C85 74.1(5) . . . . ? N8 C84 C85 C86 43.9(6) . . . . ? N8 C84 C85 C90 -137.9(5) . . . . ? C90 C85 C86 C87 0.4(9) . . . . ? C84 C85 C86 C87 178.6(6) . . . . ? C85 C86 C87 C88 -2.6(10) . . . . ? C86 C87 C88 C89 3.4(11) . . . . ? C87 C88 C89 C90 -2.1(10) . . . . ? C86 C85 C90 C89 1.0(8) . . . . ? C84 C85 C90 C89 -177.2(5) . . . . ? C88 C89 C90 C85 -0.2(9) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 959436'