# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Kee, Terence' _publ_contact_author_email t.p.kee@leeds.ac.uk _publ_section_title ; Asymmetric general base catalysis of the phospho-aldol reaction via dimeric aluminium hydroxides ; loop_ _publ_author_name T.Kee A.Gledhill N.Cosgrove T.Nixon C.Kilner J.Fisher # Attachment '- ACG29revised20100728.CIF' data_acg29revised20100728 _database_code_depnum_ccdc_archive 'CCDC 749040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H89 Al2 N4 O6, C7 H8' _chemical_formula_sum 'C67 H97 Al2 N4 O6' _chemical_formula_weight 1109.45 _chemical_absolute_configuration rmad 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 trigonal _symmetry_space_group_name_H-M 'P 32 2 1' _symmetry_space_group_name_Hall 'P 32 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 18.579(3) _cell_length_b 18.579(3) _cell_length_c 15.951(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4768.2(13) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8180 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.34 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1806 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8314 _exptl_absorpt_correction_T_max 0.9835 _exptl_absorpt_process_details ; See Sheldrick, G. M. (2002). SADABS. Version 2.03. University of Gottingen, Germany. ; _exptl_special_details ; The crystal temperature was held constant using an Oxford Cryosystems Cryostream 600 system. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Bruker Nonius FR591 rotating anode generator ; _diffrn_radiation_monochromator ; graphite model mounted in "parallel" mode ; _diffrn_measurement_device_type ; Mach3 kappa-type 4-circle goniostat. ; _diffrn_radiation_detector 'ApexII camera' _diffrn_measurement_method 'rotation images' _diffrn_detector_area_resol_mean ; 120 microns ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 69370 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.38 _reflns_number_total 3943 _reflns_number_gt 3671 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX 2 software, Bruker Nonius 2004 ; _computing_cell_refinement ; APEX 2 software, Bruker Nonius 2004 ; _computing_data_reduction ; SAINT - Bruker Integration program embedded in APEX 2 software, Bruker Nonius 2004 ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1990) XSeed v2.0 (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.) ; _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) XSeed v2.0 (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.) ; _computing_molecular_graphics 'ORTEP-III Version 1.08 (Farrugia, 2005)' _computing_publication_material ; enCIFer: A program for viewing, editing and visualising CIFs. F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler, J. Applied Cryst., 37, 331-334, 2004 ; _refine_special_details ; The structure solved in the trigonal spacegroup P3(2) 2 1 with the molecule of the title compound and a disordered toluene molecule, occupying a special position on a two-fold axis. Hydrogen atoms were placed in calculated positions and refined using a riding model. C-H distances: CH3, 0.98\A; CH2, 0.99\A; CH, 1.00\A; aromatic, 0.95\A. N-H distances: 0.93\A. All Uiso(H) values were constrained to be 1.2 times (1.5 for methyl) Ueq of the parent atom. The cifcheck report indicates an A alert because of high Ueq values for H atoms. These are associated with the pendant ethyl groups and are not unexpected. Other A alerts are associated with the disorder in the toluene molecule. The hydrogen atom, H3, bonded to O1 was found in the Fourier map and its parameters were freely refined resulting in a O1-H3 distance of 0.86\A. No corresponding hydrogen atom on the two-fold axis could be detected that was bonded to O2. The toluene molecule is disordered over two equally occupied positions with the plane of the phenyl ring approximately normal to the projection of the O1-H3 bond suggesting a O-H...pi interaction. The centroids of the phenyl rings of the disordered components are seperated by 0.733 Angstroms and the centroid-O1 distance, which is the same for both components, is 3.561 Angstroms. In terms of anomalous dispersion effects this is considered to be a 'light atom structure' since there are no Si or heavier atoms present and therefore Friedel pairs were merged. However the presence of chiral references establish the absolute configuration. C.Kilner 14 February 2007 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^)+(0.0703P)^2^+1.1580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3943 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.66349(3) 0.02742(3) 0.07631(2) 0.02071(10) Uani 1 1 d . . . O1 O 0.71121(8) 0.0000 0.1667 0.0230(3) Uani 1 2 d S . . C1 C 0.59116(10) 0.13652(10) 0.05141(10) 0.0252(3) Uani 1 1 d . . . H1 H 0.5542 0.1109 0.1011 0.030 Uiso 1 1 calc R . . O2 O 0.58213(8) 0.0000 0.1667 0.0217(3) Uani 1 2 d S . . C2 C 0.55749(13) 0.18425(12) 0.00104(12) 0.0371(4) Uani 1 1 d . . . H2A H 0.5006 0.1451 -0.0190 0.045 Uiso 1 1 calc R . . H2B H 0.5932 0.2106 -0.0485 0.045 Uiso 1 1 calc R . . C3 C 0.55613(15) 0.25166(14) 0.05684(14) 0.0444(5) Uani 1 1 d . . . H3A H 0.5367 0.2835 0.0233 0.053 Uiso 1 1 calc R . . H3B H 0.5165 0.2246 0.1035 0.053 Uiso 1 1 calc R . . C4 C 0.64311(16) 0.31182(14) 0.09294(13) 0.0454(5) Uani 1 1 d . . . H4A H 0.6393 0.3517 0.1313 0.054 Uiso 1 1 calc R . . H4B H 0.6813 0.3438 0.0466 0.054 Uiso 1 1 calc R . . C5 C 0.67852(13) 0.26409(12) 0.14092(12) 0.0368(4) Uani 1 1 d . . . H5A H 0.7358 0.3034 0.1598 0.044 Uiso 1 1 calc R . . H5B H 0.6441 0.2373 0.1911 0.044 Uiso 1 1 calc R . . C6 C 0.67910(11) 0.19742(10) 0.08380(10) 0.0263(3) Uani 1 1 d . . . H6 H 0.7141 0.2268 0.0339 0.032 Uiso 1 1 calc R . . N11 N 0.59571(8) 0.06894(9) 0.00471(8) 0.0244(3) Uani 1 1 d . . . H11 H 0.6252 0.0919 -0.0445 0.029 Uiso 1 1 calc R . . C12 C 0.51198(11) -0.00151(11) -0.01929(11) 0.0307(4) Uani 1 1 d . . . H12A H 0.4811 0.0207 -0.0503 0.037 Uiso 1 1 calc R . . H12B H 0.4802 -0.0289 0.0322 0.037 Uiso 1 1 calc R . . C13 C 0.51823(11) -0.06519(11) -0.07317(10) 0.0297(4) Uani 1 1 d . . . C14 C 0.47884(12) -0.08618(13) -0.15188(11) 0.0376(4) Uani 1 1 d . . . H14 H 0.4509 -0.0585 -0.1720 0.045 Uiso 1 1 calc R . . C15 C 0.48084(14) -0.14760(14) -0.20042(12) 0.0423(5) Uani 1 1 d . . . H15 H 0.4553 -0.1613 -0.2541 0.051 Uiso 1 1 calc R . . C16 C 0.52078(12) -0.18861(13) -0.16914(11) 0.0377(4) Uani 1 1 d . . . H16 H 0.5202 -0.2315 -0.2021 0.045 Uiso 1 1 calc R . . C17 C 0.56220(11) -0.16972(11) -0.09073(10) 0.0293(3) Uani 1 1 d . . . C18 C 0.56201(10) -0.10470(11) -0.04249(10) 0.0264(3) Uani 1 1 d . . . O19 O 0.59968(7) -0.08056(7) 0.03370(6) 0.0243(2) Uani 1 1 d . . . C20 C 0.59799(12) -0.22421(12) -0.05753(11) 0.0341(4) Uani 1 1 d . . . C21 C 0.68542(13) -0.17195(14) -0.01776(13) 0.0421(5) Uani 1 1 d . . . H21A H 0.6815 -0.1435 0.0323 0.063 Uiso 1 1 calc R . . H21B H 0.7231 -0.1307 -0.0584 0.063 Uiso 1 1 calc R . . H21C H 0.7070 -0.2086 -0.0021 0.063 Uiso 1 1 calc R . . C22 C 0.53645(14) -0.28293(14) 0.01005(12) 0.0421(5) Uani 1 1 d . . . H22A H 0.5285 -0.2498 0.0530 0.063 Uiso 1 1 calc R . . H22B H 0.5591 -0.3152 0.0361 0.063 Uiso 1 1 calc R . . H22C H 0.4830 -0.3209 -0.0163 0.063 Uiso 1 1 calc R . . C23 C 0.60325(16) -0.28124(16) -0.12588(14) 0.0494(5) Uani 1 1 d . . . H23A H 0.6169 -0.3204 -0.0978 0.059 Uiso 1 1 calc R . . H23B H 0.5475 -0.3146 -0.1512 0.059 Uiso 1 1 calc R . . C24 C 0.6651(2) -0.2387(2) -0.19592(17) 0.0750(9) Uani 1 1 d . . . H24A H 0.6511 -0.2016 -0.2264 0.112 Uiso 1 1 calc R . . H24B H 0.6633 -0.2807 -0.2345 0.112 Uiso 1 1 calc R . . H24C H 0.7212 -0.2064 -0.1723 0.112 Uiso 1 1 calc R . . N61 N 0.71534(8) 0.14944(8) 0.12339(8) 0.0227(3) Uani 1 1 d . . . H61 H 0.7024 0.1449 0.1802 0.027 Uiso 1 1 calc R . . C62 C 0.80853(10) 0.19398(11) 0.11701(10) 0.0277(3) Uani 1 1 d . . . H62A H 0.8296 0.1605 0.1446 0.033 Uiso 1 1 calc R . . H62B H 0.8323 0.2480 0.1465 0.033 Uiso 1 1 calc R . . C63 C 0.83630(10) 0.20870(11) 0.02627(10) 0.0279(3) Uani 1 1 d . . . C64 C 0.89274(12) 0.28937(12) -0.00026(12) 0.0358(4) Uani 1 1 d . . . H64 H 0.9126 0.3342 0.0384 0.043 Uiso 1 1 calc R . . C65 C 0.92015(13) 0.30440(13) -0.08332(12) 0.0431(5) Uani 1 1 d . . . H65 H 0.9580 0.3592 -0.1017 0.052 Uiso 1 1 calc R . . C66 C 0.89101(13) 0.23761(13) -0.13877(11) 0.0395(4) Uani 1 1 d . . . H66 H 0.9109 0.2483 -0.1948 0.047 Uiso 1 1 calc R . . C67 C 0.83357(11) 0.15497(12) -0.11598(10) 0.0346(4) Uani 1 1 d . . . C68 C 0.80368(10) 0.13992(11) -0.03041(10) 0.0276(3) Uani 1 1 d . . . O69 O 0.74705(7) 0.06325(8) -0.00299(6) 0.0271(3) Uani 1 1 d . . . C70 C 0.80743(15) 0.08307(15) -0.18022(12) 0.0544(7) Uani 1 1 d . . . C71 C 0.8499(2) 0.1179(2) -0.26734(15) 0.0980(15) Uani 1 1 d . . . H71A H 0.8341 0.1577 -0.2882 0.147 Uiso 1 1 calc R . . H71B H 0.8317 0.0720 -0.3073 0.147 Uiso 1 1 calc R . . H71C H 0.9104 0.1458 -0.2609 0.147 Uiso 1 1 calc R . . C72 C 0.8345(2) 0.02210(18) -0.14746(18) 0.0725(9) Uani 1 1 d . . . H72A H 0.8953 0.0494 -0.1477 0.109 Uiso 1 1 calc R . . H72B H 0.8115 -0.0270 -0.1837 0.109 Uiso 1 1 calc R . . H72C H 0.8139 0.0052 -0.0902 0.109 Uiso 1 1 calc R . . C73 C 0.71208(16) 0.03508(15) -0.19406(13) 0.0602(7) Uani 1 1 d . . . H73A H 0.6982 -0.0110 -0.2338 0.072 Uiso 1 1 calc R . . H73B H 0.6847 0.0101 -0.1401 0.072 Uiso 1 1 calc R . . C74 C 0.6778(2) 0.0851(2) -0.2262(2) 0.0850(10) Uani 1 1 d . . . H74A H 0.6906 0.1307 -0.1872 0.128 Uiso 1 1 calc R . . H74B H 0.6174 0.0502 -0.2320 0.128 Uiso 1 1 calc R . . H74C H 0.7023 0.1079 -0.2811 0.128 Uiso 1 1 calc R . . C1SA C 0.9337(3) 0.0421(4) 0.1190(3) 0.0491(11) Uani 0.50 1 d P . 1 C2SA C 0.8780(5) -0.0412(5) 0.0980(5) 0.0547(16) Uani 0.50 1 d P . 1 H2SA H 0.8676 -0.0555 0.0404 0.066 Uiso 0.50 1 calc PR . 1 C3SA C 0.8379(4) -0.1027(4) 0.1562(5) 0.0615(15) Uani 0.50 1 d P . 1 H3SA H 0.7947 -0.1591 0.1570 0.074 Uiso 0.50 1 calc PR . 1 C7SA C 0.9798(4) 0.1087(4) 0.0532(4) 0.0737(17) Uani 0.50 1 d P . 1 H7S1 H 1.0271 0.1045 0.0322 0.111 Uiso 0.50 1 calc PR . 1 H7S2 H 0.9999 0.1637 0.0783 0.111 Uiso 0.50 1 calc PR . 1 H7S3 H 0.9421 0.1011 0.0068 0.111 Uiso 0.50 1 calc PR . 1 C4SB C 0.9339(4) 0.0824(5) 0.0939(4) 0.0647(15) Uani 0.50 1 d P . 2 H4SB H 0.9432 0.1306 0.0643 0.078 Uiso 0.50 1 calc PR . 2 C5SB C 0.9056(6) 0.0010(6) 0.0704(5) 0.075(2) Uani 0.50 1 d P . 2 H5SB H 0.9003 -0.0126 0.0125 0.090 Uiso 0.50 1 calc PR . 2 C6SB C 0.8841(7) -0.0626(6) 0.1308(5) 0.067(2) Uani 0.50 1 d P . 2 H6SB H 0.8879 -0.1077 0.1076 0.081 Uiso 0.50 1 calc PR . 2 H3 H 0.7575 0.0000 0.1667 0.103(18) Uiso 1 2 d SR . . 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 0.0193(2) 0.0250(2) 0.01571(19) -0.00169(16) -0.00058(16) 0.00956(19) O1 0.0222(5) 0.0304(9) 0.0190(6) -0.0029(6) -0.0014(3) 0.0152(4) C1 0.0268(8) 0.0260(8) 0.0224(7) 0.0038(6) -0.0004(6) 0.0128(7) O2 0.0215(5) 0.0255(8) 0.0193(7) 0.0014(6) 0.0007(3) 0.0127(4) C2 0.0452(11) 0.0356(10) 0.0343(9) 0.0048(8) -0.0072(8) 0.0231(9) C3 0.0569(13) 0.0427(12) 0.0464(11) 0.0042(9) -0.0078(10) 0.0344(11) C4 0.0625(14) 0.0349(11) 0.0470(11) -0.0013(9) -0.0029(10) 0.0305(10) C5 0.0444(11) 0.0329(10) 0.0361(9) -0.0059(8) -0.0047(8) 0.0215(9) C6 0.0292(8) 0.0243(8) 0.0229(7) 0.0013(6) 0.0019(6) 0.0115(7) N11 0.0222(7) 0.0272(7) 0.0203(6) -0.0011(5) -0.0017(5) 0.0097(6) C12 0.0219(8) 0.0318(9) 0.0343(9) -0.0036(7) -0.0075(7) 0.0104(7) C13 0.0229(8) 0.0320(9) 0.0278(8) -0.0052(7) -0.0050(6) 0.0090(7) C14 0.0322(9) 0.0443(11) 0.0322(9) -0.0041(8) -0.0121(7) 0.0161(8) C15 0.0449(11) 0.0503(12) 0.0268(9) -0.0106(8) -0.0145(8) 0.0202(10) C16 0.0371(10) 0.0447(11) 0.0267(8) -0.0127(8) -0.0068(7) 0.0170(9) C17 0.0275(8) 0.0343(8) 0.0216(7) -0.0059(6) -0.0006(6) 0.0121(7) C18 0.0203(7) 0.0307(8) 0.0202(7) -0.0018(6) -0.0015(6) 0.0068(7) O19 0.0250(6) 0.0266(5) 0.0178(5) -0.0043(4) -0.0031(4) 0.0103(5) C20 0.0357(10) 0.0404(10) 0.0286(8) -0.0117(7) -0.0051(7) 0.0210(8) C21 0.0349(10) 0.0524(12) 0.0445(10) -0.0176(9) -0.0084(8) 0.0260(9) C22 0.0481(12) 0.0436(11) 0.0334(9) -0.0017(8) -0.0053(8) 0.0220(10) C23 0.0610(14) 0.0569(14) 0.0407(10) -0.0203(10) -0.0084(10) 0.0372(12) C24 0.0691(18) 0.100(2) 0.0561(14) -0.0264(16) 0.0083(14) 0.0425(18) N61 0.0211(6) 0.0264(6) 0.0171(5) -0.0004(5) 0.0016(5) 0.0092(5) C62 0.0220(8) 0.0308(8) 0.0223(7) -0.0051(6) 0.0002(6) 0.0072(7) C63 0.0219(8) 0.0348(9) 0.0207(7) -0.0029(6) 0.0038(6) 0.0095(7) C64 0.0288(9) 0.0327(9) 0.0347(9) -0.0060(7) 0.0072(7) 0.0069(8) C65 0.0391(11) 0.0351(10) 0.0402(10) 0.0030(8) 0.0187(9) 0.0074(9) C66 0.0363(10) 0.0433(11) 0.0267(8) 0.0016(8) 0.0123(7) 0.0107(9) C67 0.0290(9) 0.0389(10) 0.0243(8) -0.0032(7) 0.0058(7) 0.0084(8) C68 0.0208(8) 0.0328(9) 0.0232(7) -0.0014(6) 0.0030(6) 0.0091(7) O69 0.0238(5) 0.0295(6) 0.0207(5) -0.0029(4) 0.0036(4) 0.0078(5) C70 0.0563(13) 0.0507(13) 0.0239(8) -0.0105(9) 0.0149(9) 0.0026(11) C71 0.100(2) 0.0760(19) 0.0350(11) -0.0229(13) 0.0346(14) -0.0188(18) C72 0.088(2) 0.0584(16) 0.0660(16) -0.0181(13) 0.0284(15) 0.0333(15) C73 0.0631(15) 0.0466(12) 0.0276(9) 0.0014(9) -0.0035(10) -0.0051(11) C74 0.078(2) 0.0642(18) 0.0728(18) 0.0144(15) -0.0143(16) 0.0059(16) C1SA 0.035(2) 0.063(3) 0.051(3) 0.005(3) -0.004(2) 0.026(2) C2SA 0.055(4) 0.058(5) 0.058(5) -0.015(4) -0.015(3) 0.034(4) C3SA 0.048(3) 0.051(3) 0.080(4) 0.005(3) -0.005(3) 0.021(3) C7SA 0.062(4) 0.083(4) 0.067(4) 0.018(3) -0.007(3) 0.029(3) C4SB 0.069(4) 0.070(4) 0.070(4) 0.010(3) 0.001(3) 0.046(4) C5SB 0.100(6) 0.075(5) 0.054(4) -0.008(4) -0.021(4) 0.046(5) C6SB 0.099(7) 0.067(5) 0.059(5) -0.006(4) -0.014(4) 0.058(5) _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 O69 1.8493(12) . ? Al1 O19 1.8745(12) . ? Al1 O1 1.8906(10) . ? Al1 O2 1.9627(11) . ? Al1 N61 2.1088(14) . ? Al1 N11 2.1112(15) . ? O1 Al1 1.8906(10) 4 ? O1 H3 0.8603 . ? C1 N11 1.498(2) . ? C1 C6 1.539(2) . ? C1 C2 1.542(2) . ? C1 H1 1.0000 . ? O2 Al1 1.9627(11) 4 ? C2 C3 1.547(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.545(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.545(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.542(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N61 1.499(2) . ? C6 H6 1.0000 . ? N11 C12 1.498(2) . ? N11 H11 0.9300 . ? C12 C13 1.513(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.407(2) . ? C13 C18 1.427(2) . ? C14 C15 1.395(3) . ? C14 H14 0.9500 . ? C15 C16 1.395(3) . ? C15 H15 0.9500 . ? C16 C17 1.418(2) . ? C16 H16 0.9500 . ? C17 C18 1.434(2) . ? C17 C20 1.556(3) . ? C18 O19 1.3617(18) . ? C20 C21 1.551(3) . ? C20 C22 1.553(3) . ? C20 C23 1.557(3) . ? 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 C24 1.512(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N61 C62 1.503(2) . ? N61 H61 0.9300 . ? C62 C63 1.515(2) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.398(3) . ? C63 C68 1.429(2) . ? C64 C65 1.397(3) . ? C64 H64 0.9500 . ? C65 C66 1.394(3) . ? C65 H65 0.9500 . ? C66 C67 1.411(3) . ? C66 H66 0.9500 . ? C67 C68 1.447(2) . ? C67 C70 1.556(3) . ? C68 O69 1.352(2) . ? C70 C72 1.542(4) . ? C70 C73 1.550(3) . ? C70 C71 1.569(3) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.457(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C1SA C2SA 1.405(9) . ? C1SA C3SA 1.415(9) 4 ? C1SA C7SA 1.519(8) . ? C1SA C2SA 1.874(10) 4 ? C1SA C1SA 2.036(12) 4 ? C2SA C3SA 1.367(11) . ? C2SA C1SA 1.874(10) 4 ? C2SA H2SA 0.9500 . ? C3SA C1SA 1.415(9) 4 ? C3SA H3SA 0.9500 . ? C7SA H7S1 0.9800 . ? C7SA H7S2 0.9800 . ? C7SA H7S3 0.9800 . ? C4SB C5SB 1.380(10) . ? C4SB C6SB 1.812(11) 4 ? C4SB H4SB 0.9500 . ? C5SB C6SB 1.419(10) . ? C5SB H5SB 0.9500 . ? C6SB C4SB 1.812(11) 4 ? C6SB H6SB 0.9500 . ? 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 O69 Al1 O19 96.03(5) . . ? O69 Al1 O1 101.31(6) . . ? O19 Al1 O1 96.83(4) . . ? O69 Al1 O2 174.14(5) . . ? O19 Al1 O2 89.75(4) . . ? O1 Al1 O2 76.96(5) . . ? O69 Al1 N61 90.38(5) . . ? O19 Al1 N61 169.77(6) . . ? O1 Al1 N61 89.68(4) . . ? O2 Al1 N61 84.03(4) . . ? O69 Al1 N11 92.59(5) . . ? O19 Al1 N11 91.22(5) . . ? O1 Al1 N11 163.06(5) . . ? O2 Al1 N11 88.24(5) . . ? N61 Al1 N11 80.51(5) . . ? Al1 O1 Al1 105.74(8) 4 . ? Al1 O1 H3 127.1 4 . ? Al1 O1 H3 127.1 . . ? N11 C1 C6 107.41(13) . . ? N11 C1 C2 115.59(13) . . ? C6 C1 C2 109.82(14) . . ? N11 C1 H1 107.9 . . ? C6 C1 H1 107.9 . . ? C2 C1 H1 107.9 . . ? Al1 O2 Al1 100.35(7) 4 . ? C1 C2 C3 109.95(14) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 111.45(18) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.16(17) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 110.13(15) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N61 C6 C1 109.37(13) . . ? N61 C6 C5 114.48(13) . . ? C1 C6 C5 110.97(15) . . ? N61 C6 H6 107.2 . . ? C1 C6 H6 107.2 . . ? C5 C6 H6 107.2 . . ? C12 N11 C1 112.98(13) . . ? C12 N11 Al1 111.56(10) . . ? C1 N11 Al1 109.34(9) . . ? C12 N11 H11 107.6 . . ? C1 N11 H11 107.6 . . ? Al1 N11 H11 107.6 . . ? N11 C12 C13 112.11(14) . . ? N11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C18 120.98(17) . . ? C14 C13 C12 119.42(17) . . ? C18 C13 C12 119.58(14) . . ? C15 C14 C13 119.96(18) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.17(16) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 123.48(18) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C16 C17 C18 116.89(17) . . ? C16 C17 C20 119.67(16) . . ? C18 C17 C20 123.20(14) . . ? O19 C18 C13 117.90(15) . . ? O19 C18 C17 122.62(15) . . ? C13 C18 C17 119.44(14) . . ? C18 O19 Al1 128.47(11) . . ? C21 C20 C22 109.18(16) . . ? C21 C20 C17 112.73(16) . . ? C22 C20 C17 106.81(15) . . ? C21 C20 C23 108.05(16) . . ? C22 C20 C23 106.42(17) . . ? C17 C20 C23 113.40(15) . . ? 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 . . ? C24 C23 C20 116.9(2) . . ? C24 C23 H23A 108.1 . . ? C20 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? C20 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C6 N61 C62 112.34(12) . . ? C6 N61 Al1 112.93(9) . . ? C62 N61 Al1 110.42(10) . . ? C6 N61 H61 106.9 . . ? C62 N61 H61 106.9 . . ? Al1 N61 H61 106.9 . . ? N61 C62 C63 111.02(13) . . ? N61 C62 H62A 109.4 . . ? C63 C62 H62A 109.4 . . ? N61 C62 H62B 109.4 . . ? C63 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C64 C63 C68 121.50(15) . . ? C64 C63 C62 119.22(15) . . ? C68 C63 C62 119.28(15) . . ? C65 C64 C63 120.32(17) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C66 C65 C64 118.91(18) . . ? C66 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? C65 C66 C67 123.44(16) . . ? C65 C66 H66 118.3 . . ? C67 C66 H66 118.3 . . ? C66 C67 C68 117.50(16) . . ? C66 C67 C70 120.41(15) . . ? C68 C67 C70 122.03(17) . . ? O69 C68 C63 119.73(13) . . ? O69 C68 C67 121.99(15) . . ? C63 C68 C67 118.27(15) . . ? C68 O69 Al1 132.17(11) . . ? C72 C70 C73 108.9(2) . . ? C72 C70 C67 109.32(19) . . ? C73 C70 C67 111.3(2) . . ? C72 C70 C71 108.8(2) . . ? C73 C70 C71 107.8(2) . . ? C67 C70 C71 110.63(18) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C70 115.0(2) . . ? C74 C73 H73A 108.5 . . ? C70 C73 H73A 108.5 . . ? C74 C73 H73B 108.5 . . ? C70 C73 H73B 108.5 . . ? H73A C73 H73B 107.5 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C2SA C1SA C3SA 139.1(6) . 4 ? C2SA C1SA C7SA 122.5(6) . . ? C3SA C1SA C7SA 90.8(6) 4 . ? C2SA C1SA C2SA 101.7(5) . 4 ? C3SA C1SA C2SA 46.6(4) 4 4 ? C7SA C1SA C2SA 135.3(6) . 4 ? C2SA C1SA C1SA 62.9(5) . 4 ? C3SA C1SA C1SA 88.2(4) 4 4 ? C7SA C1SA C1SA 170.2(4) . 4 ? C3SA C2SA C1SA 123.5(7) . . ? C3SA C2SA C1SA 48.7(5) . 4 ? C1SA C2SA C1SA 75.3(5) . 4 ? C3SA C2SA H2SA 118.2 . . ? C1SA C2SA H2SA 118.3 . . ? C1SA C2SA H2SA 164.9 4 . ? C2SA C3SA C1SA 84.7(6) . 4 ? C2SA C3SA H3SA 137.7 . . ? C1SA C3SA H3SA 137.7 4 . ? C5SB C4SB C6SB 93.2(6) . 4 ? C5SB C4SB H4SB 133.4 . . ? C6SB C4SB H4SB 133.4 4 . ? C4SB C5SB C6SB 121.5(8) . . ? C4SB C5SB H5SB 119.3 . . ? C6SB C5SB H5SB 119.3 . . ? C5SB C6SB C4SB 138.1(7) . 4 ? C5SB C6SB H6SB 111.0 . . ? C4SB C6SB H6SB 111.0 4 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O69 Al1 O1 Al1 174.27(5) . . . 4 ? O19 Al1 O1 Al1 -88.15(4) . . . 4 ? O2 Al1 O1 Al1 0.0 . . . 4 ? N61 Al1 O1 Al1 83.95(4) . . . 4 ? N11 Al1 O1 Al1 29.68(16) . . . 4 ? O19 Al1 O2 Al1 97.07(4) . . . 4 ? O1 Al1 O2 Al1 0.0 . . . 4 ? N61 Al1 O2 Al1 -91.06(4) . . . 4 ? N11 Al1 O2 Al1 -171.70(4) . . . 4 ? N11 C1 C2 C3 179.90(16) . . . . ? C6 C1 C2 C3 -58.4(2) . . . . ? C1 C2 C3 C4 56.6(2) . . . . ? C2 C3 C4 C5 -55.2(2) . . . . ? C3 C4 C5 C6 55.1(2) . . . . ? N11 C1 C6 N61 -46.61(15) . . . . ? C2 C1 C6 N61 -173.05(13) . . . . ? N11 C1 C6 C5 -173.84(13) . . . . ? C2 C1 C6 C5 59.71(18) . . . . ? C4 C5 C6 N61 177.85(16) . . . . ? C4 C5 C6 C1 -57.8(2) . . . . ? C6 C1 N11 C12 171.35(13) . . . . ? C2 C1 N11 C12 -65.68(18) . . . . ? C6 C1 N11 Al1 46.47(13) . . . . ? C2 C1 N11 Al1 169.43(12) . . . . ? O69 Al1 N11 C12 118.35(11) . . . . ? O19 Al1 N11 C12 22.25(11) . . . . ? O1 Al1 N11 C12 -96.31(19) . . . . ? O2 Al1 N11 C12 -67.45(10) . . . . ? N61 Al1 N11 C12 -151.69(11) . . . . ? O69 Al1 N11 C1 -115.94(10) . . . . ? O19 Al1 N11 C1 147.96(10) . . . . ? O1 Al1 N11 C1 29.4(2) . . . . ? O2 Al1 N11 C1 58.25(10) . . . . ? N61 Al1 N11 C1 -25.99(10) . . . . ? C1 N11 C12 C13 174.73(13) . . . . ? Al1 N11 C12 C13 -61.60(15) . . . . ? N11 C12 C13 C14 -124.28(18) . . . . ? N11 C12 C13 C18 57.4(2) . . . . ? C18 C13 C14 C15 1.3(3) . . . . ? C12 C13 C14 C15 -176.98(18) . . . . ? C13 C14 C15 C16 1.2(3) . . . . ? C14 C15 C16 C17 -1.9(3) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C15 C16 C17 C20 174.45(19) . . . . ? C14 C13 C18 O19 179.09(16) . . . . ? C12 C13 C18 O19 -2.6(2) . . . . ? C14 C13 C18 C17 -3.2(3) . . . . ? C12 C13 C18 C17 175.04(15) . . . . ? C16 C17 C18 O19 -179.88(16) . . . . ? C20 C17 C18 O19 5.8(3) . . . . ? C16 C17 C18 C13 2.6(2) . . . . ? C20 C17 C18 C13 -171.73(16) . . . . ? C13 C18 O19 Al1 -43.9(2) . . . . ? C17 C18 O19 Al1 138.55(14) . . . . ? O69 Al1 O19 C18 -62.74(14) . . . . ? O1 Al1 O19 C18 -164.94(13) . . . . ? O2 Al1 O19 C18 118.23(13) . . . . ? N61 Al1 O19 C18 65.8(3) . . . . ? N11 Al1 O19 C18 30.00(13) . . . . ? C16 C17 C20 C21 137.77(18) . . . . ? C18 C17 C20 C21 -48.1(2) . . . . ? C16 C17 C20 C22 -102.33(18) . . . . ? C18 C17 C20 C22 71.8(2) . . . . ? C16 C17 C20 C23 14.6(3) . . . . ? C18 C17 C20 C23 -171.29(17) . . . . ? C21 C20 C23 C24 -58.0(3) . . . . ? C22 C20 C23 C24 -175.1(2) . . . . ? C17 C20 C23 C24 67.7(3) . . . . ? C1 C6 N61 C62 150.98(12) . . . . ? C5 C6 N61 C62 -83.79(17) . . . . ? C1 C6 N61 Al1 25.28(15) . . . . ? C5 C6 N61 Al1 150.51(13) . . . . ? O69 Al1 N61 C6 92.55(10) . . . . ? O19 Al1 N61 C6 -36.4(3) . . . . ? O1 Al1 N61 C6 -166.14(10) . . . . ? O2 Al1 N61 C6 -89.22(10) . . . . ? N11 Al1 N61 C6 -0.01(10) . . . . ? O69 Al1 N61 C62 -34.18(10) . . . . ? O19 Al1 N61 C62 -163.1(3) . . . . ? O1 Al1 N61 C62 67.13(10) . . . . ? O2 Al1 N61 C62 144.05(10) . . . . ? N11 Al1 N61 C62 -126.74(10) . . . . ? C6 N61 C62 C63 -59.94(17) . . . . ? Al1 N61 C62 C63 67.12(15) . . . . ? N61 C62 C63 C64 125.73(18) . . . . ? N61 C62 C63 C68 -53.7(2) . . . . ? C68 C63 C64 C65 -1.4(3) . . . . ? C62 C63 C64 C65 179.15(19) . . . . ? C63 C64 C65 C66 -0.7(3) . . . . ? C64 C65 C66 C67 1.3(3) . . . . ? C65 C66 C67 C68 0.3(3) . . . . ? C65 C66 C67 C70 -176.8(2) . . . . ? C64 C63 C68 O69 -177.76(18) . . . . ? C62 C63 C68 O69 1.7(2) . . . . ? C64 C63 C68 C67 2.9(3) . . . . ? C62 C63 C68 C67 -177.63(16) . . . . ? C66 C67 C68 O69 178.37(18) . . . . ? C70 C67 C68 O69 -4.5(3) . . . . ? C66 C67 C68 C63 -2.3(3) . . . . ? C70 C67 C68 C63 174.78(19) . . . . ? C63 C68 O69 Al1 33.0(2) . . . . ? C67 C68 O69 Al1 -147.65(14) . . . . ? O19 Al1 O69 C68 157.76(14) . . . . ? O1 Al1 O69 C68 -104.01(14) . . . . ? N61 Al1 O69 C68 -14.26(14) . . . . ? N11 Al1 O69 C68 66.26(14) . . . . ? C66 C67 C70 C72 117.2(2) . . . . ? C68 C67 C70 C72 -59.8(3) . . . . ? C66 C67 C70 C73 -122.4(2) . . . . ? C68 C67 C70 C73 60.6(3) . . . . ? C66 C67 C70 C71 -2.5(4) . . . . ? C68 C67 C70 C71 -179.6(2) . . . . ? C72 C70 C73 C74 -179.2(2) . . . . ? C67 C70 C73 C74 60.1(3) . . . . ? C71 C70 C73 C74 -61.4(3) . . . . ? C3SA C1SA C2SA C3SA -42.5(11) 4 . . . ? C7SA C1SA C2SA C3SA 177.8(6) . . . . ? C2SA C1SA C2SA C3SA -9.0(9) 4 . . . ? C1SA C1SA C2SA C3SA 7.2(5) 4 . . . ? C3SA C1SA C2SA C1SA -49.8(9) 4 . . 4 ? C7SA C1SA C2SA C1SA 170.6(5) . . . 4 ? C2SA C1SA C2SA C1SA -16.2(5) 4 . . 4 ? C1SA C2SA C3SA C1SA -9.3(6) . . . 4 ? C6SB C4SB C5SB C6SB 10.9(8) 4 . . . ? C4SB C5SB C6SB C4SB 23.8(15) . . . 4 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.535 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.040 data_tdn310revised20100729 _database_code_depnum_ccdc_archive 'CCDC 749041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H82 Al2 N4 O6, 4(C6 H5 Cl)' _chemical_formula_sum 'C80 H102 Al2 Cl4 N4 O6' _chemical_formula_weight 1411.42 _chemical_absolute_configuration rmad 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.79800(10) _cell_length_b 31.2880(2) _cell_length_c 20.6198(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.3000(3) _cell_angle_gamma 90.00 _cell_volume 7488.85(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 143270 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type none _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _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 ; Nonius KappaCCD area-detector diffractometer ; _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; phi and omega scans to fill the asymmetric unit ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 90149 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 29189 _reflns_number_gt 25135 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'local program' _refine_special_details ; The structure solved in spacegroup P21 and the asymmetric unit contains two molecules of the title compound and eight molecules of chlorobenzene. Four of the eight chlorobenzene molecules displayed disorder. To eliminate the resulting unstable refinement, the atoms of these molecules were refined isotropically and subsequently fixed in position. All hydrogen atoms were positioned geometrically. C-H distances: aromatic, 0.95/A; CH3, 0.98/A; CH2, 0.99/A; CH, 1.00/A. N-H distance: 0.93/A. All Uiso(H) values were constrained to be 1.2 times Ueq of the parent atom. The absolute configuration was established since the molecule contained a chiral reference of known absolute configuration and this was confirmed by anomalous dispersion effects since the Flack parameter refined to 0.08(8). There is a high positive residual density of 1.82 e\A\^3 at 1.38 angstroms from C84S. All maxima greater than 0.33 e\A\^3 in the positive residual density function are associated with solvent molecules. C.Kilner 31 May 2007 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1562P)^2^+8.7164P] 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 0.08(8) _refine_ls_number_reflns 29189 _refine_ls_number_parameters 1502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.2457 _refine_ls_wR_factor_gt 0.2321 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.87086(10) 0.32638(7) 0.88784(6) 0.0238(3) Uani 1 1 d . . . Al2 Al 0.79073(11) 0.24230(7) 0.93188(6) 0.0247(3) Uani 1 1 d . . . Al3 Al 1.38913(11) 0.31120(7) 0.40878(6) 0.0251(3) Uani 1 1 d . . . Al4 Al 1.29769(11) 0.22199(7) 0.41196(6) 0.0262(3) Uani 1 1 d . . . C1A C 0.4938(4) 0.41350(18) 0.7713(2) 0.0399(11) Uani 1 1 d . . . C1B C 0.4908(4) 0.42754(19) 0.8417(2) 0.0408(12) Uani 1 1 d . . . C1C C 0.7495(5) 0.14213(19) 0.7157(2) 0.0416(12) Uani 1 1 d . . . C1D C 0.8779(5) 0.13558(18) 0.7377(3) 0.0425(12) Uani 1 1 d . . . C1E C 1.0175(4) 0.4135(2) 0.3346(3) 0.0464(13) Uani 1 1 d . . . C1F C 1.0153(5) 0.4141(2) 0.4091(3) 0.0493(14) Uani 1 1 d . . . C1G C 1.2432(5) 0.1608(2) 0.1626(3) 0.0515(15) Uani 1 1 d . . . C1H C 1.3710(5) 0.15045(19) 0.1818(2) 0.0423(12) Uani 1 1 d . . . C2A C 0.6184(4) 0.40578(16) 0.7609(2) 0.0330(10) Uani 1 1 d . . . C2B C 0.5505(3) 0.39514(12) 0.89149(16) 0.0332(10) Uani 1 1 d . . . C2C C 0.6878(4) 0.14802(17) 0.7749(2) 0.0373(11) Uani 1 1 d . . . C2D C 0.9302(5) 0.17297(18) 0.7800(2) 0.0396(11) Uani 1 1 d . . . C2E C 1.1407(4) 0.40830(16) 0.3212(3) 0.0357(10) Uani 1 1 d . . . C2F C 1.0724(4) 0.37403(18) 0.4424(3) 0.0399(11) Uani 1 1 d . . . C2G C 1.1816(5) 0.1575(2) 0.2216(2) 0.0424(12) Uani 1 1 d . . . C2H C 1.4282(4) 0.18031(18) 0.2369(2) 0.0375(11) Uani 1 1 d . . . C3A C 0.6760(4) 0.37281(15) 0.8095(2) 0.0281(9) Uani 1 1 d . . . C3B C 0.6723(4) 0.38706(15) 0.8808(2) 0.0278(9) Uani 1 1 d . . . C3C C 0.7408(4) 0.18594(16) 0.8171(2) 0.0321(9) Uani 1 1 d . . . C3D C 0.8682(4) 0.17918(15) 0.8387(2) 0.0306(9) Uani 1 1 d . . . C3E C 1.1970(4) 0.36786(16) 0.3539(2) 0.0303(9) Uani 1 1 d . . . C3F C 1.1940(4) 0.36875(16) 0.4280(2) 0.0307(9) Uani 1 1 d . . . C3G C 1.2388(4) 0.18770(15) 0.2774(2) 0.0309(9) Uani 1 1 d . . . C3H C 1.3684(4) 0.17719(15) 0.2965(2) 0.0311(9) Uani 1 1 d . . . C5A C 0.8180(4) 0.34317(15) 0.7442(2) 0.0280(9) Uani 1 1 d . . . C5B C 0.7835(4) 0.37376(16) 0.9929(2) 0.0292(9) Uani 1 1 d . . . C5C C 0.5664(3) 0.20417(12) 0.86517(16) 0.0334(10) Uani 1 1 d R . . C5D C 1.0199(4) 0.20229(16) 0.9315(2) 0.0317(9) Uani 1 1 d . . . C5E C 1.3420(4) 0.35790(17) 0.2811(2) 0.0348(10) Uani 1 1 d . . . C5F C 1.3038(4) 0.33709(16) 0.5307(2) 0.0313(9) Uani 1 1 d . . . C5G C 1.0687(4) 0.19835(16) 0.3322(2) 0.0335(10) Uani 1 1 d . . . C5H C 1.5210(4) 0.18477(17) 0.3939(2) 0.0351(10) Uani 1 1 d . . . C6A C 0.9443(4) 0.34175(15) 0.7416(2) 0.0277(9) Uani 1 1 d . . . C6B C 0.8601(4) 0.41137(15) 0.9869(2) 0.0295(9) Uani 1 1 d . . . C6C C 0.5235(4) 0.20924(16) 0.9288(2) 0.0324(10) Uani 1 1 d . . . C6D C 0.9955(4) 0.16889(15) 0.9787(2) 0.0304(9) Uani 1 1 d . . . C6E C 1.4690(4) 0.35769(16) 0.2801(2) 0.0315(9) Uani 1 1 d . . . C6F C 1.3876(4) 0.37389(16) 0.5413(2) 0.0300(9) Uani 1 1 d . . . C6G C 1.0252(4) 0.19113(16) 0.3958(2) 0.0347(10) Uani 1 1 d . . . C6H C 1.4950(5) 0.14333(17) 0.4242(2) 0.0386(11) Uani 1 1 d . . . C7A C 0.9864(4) 0.36253(16) 0.6918(2) 0.0313(9) Uani 1 1 d . . . C7B C 0.8390(4) 0.45007(17) 1.0166(2) 0.0350(10) Uani 1 1 d . . . C7C C 0.4340(4) 0.18288(17) 0.9430(3) 0.0385(11) Uani 1 1 d . . . C7D C 1.0674(4) 0.13241(16) 0.9876(2) 0.0347(10) Uani 1 1 d . . . C7E C 1.5176(4) 0.38875(17) 0.2451(2) 0.0378(11) Uani 1 1 d . . . C7F C 1.3698(4) 0.40617(17) 0.5850(2) 0.0367(10) Uani 1 1 d . . . C7G C 0.9331(4) 0.16392(17) 0.3979(2) 0.0373(11) Uani 1 1 d . . . C7H C 1.5639(5) 0.1082(2) 0.4184(3) 0.0496(13) Uani 1 1 d . . . C8A C 1.1029(5) 0.36011(16) 0.6886(2) 0.0371(11) Uani 1 1 d . . . C8B C 0.9044(5) 0.48514(16) 1.0108(3) 0.0400(11) Uani 1 1 d . . . C8C C 0.3874(4) 0.19032(17) 0.9985(3) 0.0378(11) Uani 1 1 d . . . C8D C 1.0543(4) 0.10149(16) 1.0341(3) 0.0375(11) Uani 1 1 d . . . C8E C 1.6289(5) 0.38719(17) 0.2407(3) 0.0408(11) Uani 1 1 d . . . C8F C 1.4490(5) 0.43926(17) 0.5993(2) 0.0405(11) Uani 1 1 d . . . C8G C 0.8918(4) 0.15809(18) 0.4555(3) 0.0411(11) Uani 1 1 d . . . C8H C 1.5456(6) 0.0700(2) 0.4500(4) 0.0650(19) Uani 1 1 d . . . C9A C 1.1759(4) 0.33701(16) 0.7359(2) 0.0328(10) Uani 1 1 d . . . C9B C 0.9962(4) 0.48168(17) 0.9769(3) 0.0389(11) Uani 1 1 d . . . C9C C 0.4301(4) 0.22360(16) 1.0403(2) 0.0344(10) Uani 1 1 d . . . C9D C 0.9697(4) 0.10789(17) 1.0718(3) 0.0378(11) Uani 1 1 d . . . C9E C 1.6986(4) 0.35400(18) 0.2710(2) 0.0387(11) Uani 1 1 d . . . C9F C 1.5478(5) 0.43834(16) 0.5722(2) 0.0367(11) Uani 1 1 d . . . C9G C 0.9405(4) 0.18119(18) 0.5108(3) 0.0392(11) Uani 1 1 d . . . C9H C 1.4598(6) 0.06736(19) 0.4870(3) 0.0529(15) Uani 1 1 d . . . C10A C 1.1372(4) 0.31591(15) 0.7885(2) 0.0311(9) Uani 1 1 d . . . C10B C 1.0215(4) 0.44381(15) 0.9465(2) 0.0317(9) Uani 1 1 d . . . C10C C 0.5202(4) 0.25051(15) 1.0298(2) 0.0294(9) Uani 1 1 d . . . C10D C 0.8945(4) 0.14257(16) 1.0645(2) 0.0325(10) Uani 1 1 d . . . C10E C 1.6563(4) 0.32225(17) 0.3077(2) 0.0315(9) Uani 1 1 d . . . C10F C 1.5694(4) 0.40684(16) 0.5278(2) 0.0318(9) Uani 1 1 d . . . C10G C 1.0331(4) 0.20922(16) 0.5121(2) 0.0330(10) Uani 1 1 d . . . C10H C 1.3868(5) 0.10186(16) 0.4934(2) 0.0393(11) Uani 1 1 d . . . C11A C 1.0185(4) 0.31945(14) 0.7920(2) 0.0265(9) Uani 1 1 d . . . C11B C 0.9506(4) 0.40726(15) 0.9514(2) 0.0280(9) Uani 1 1 d . . . C11C C 0.5711(4) 0.24115(15) 0.9734(2) 0.0271(8) Uani 1 1 d . . . C11D C 0.9067(4) 0.17375(15) 1.0148(2) 0.0293(9) Uani 1 1 d . . . C11E C 1.5384(4) 0.32566(15) 0.3153(2) 0.0276(9) Uani 1 1 d . . . C11F C 1.4822(4) 0.37416(15) 0.5099(2) 0.0297(9) Uani 1 1 d . . . C11G C 1.0791(4) 0.21279(15) 0.4539(2) 0.0298(9) Uani 1 1 d . . . C11H C 1.4030(4) 0.14080(17) 0.4601(2) 0.0361(10) Uani 1 1 d . . . C11S C 0.4352(5) 0.99498(18) 0.9535(3) 0.0458(13) Uani 1 1 d . . . C12A C 1.2218(4) 0.28795(16) 0.8354(2) 0.0337(10) Uani 1 1 d . . . C12B C 1.1259(4) 0.44195(16) 0.9116(2) 0.0349(10) Uani 1 1 d . . . C12C C 0.5518(4) 0.28938(15) 1.0734(2) 0.0294(9) Uani 1 1 d . . . C12D C 0.8032(5) 0.14744(18) 1.1084(3) 0.0439(12) Uani 1 1 d . . . C12E C 1.7320(4) 0.28342(17) 0.3321(2) 0.0360(10) Uani 1 1 d . . . C12F C 1.6822(4) 0.40737(18) 0.5004(3) 0.0393(11) Uani 1 1 d . . . C12G C 1.0696(4) 0.23926(17) 0.5716(2) 0.0333(10) Uani 1 1 d . . . C12H C 1.2917(5) 0.09648(18) 0.5336(3) 0.0468(13) Uani 1 1 d . . . C12S C 0.3572(5) 1.0255(2) 0.9258(4) 0.0583(16) Uani 1 1 d . . . C13A C 1.2157(4) 0.29500(18) 0.9087(2) 0.0399(11) Uani 1 1 d . . . C13B C 1.2161(5) 0.41166(19) 0.9513(3) 0.0465(13) Uani 1 1 d . . . C13C C 0.4899(4) 0.29114(18) 1.1332(2) 0.0374(10) Uani 1 1 d . . . C13D C 0.8215(6) 0.1899(2) 1.1462(3) 0.0525(14) Uani 1 1 d . . . C13E C 1.8561(4) 0.2888(2) 0.3213(3) 0.0509(14) Uani 1 1 d . . . C13F C 1.7672(5) 0.44106(19) 0.5335(3) 0.0488(13) Uani 1 1 d . . . C13G C 1.2011(4) 0.23832(18) 0.5981(2) 0.0372(10) Uani 1 1 d . . . C13H C 1.1722(6) 0.1015(2) 0.4892(4) 0.0610(17) Uani 1 1 d . . . C13S C 0.3533(7) 1.0641(2) 0.9589(5) 0.073(2) Uani 1 1 d . . . C14A C 1.3476(5) 0.2946(2) 0.8287(3) 0.0537(15) Uani 1 1 d . . . C14B C 1.1842(4) 0.48586(17) 0.9083(3) 0.0414(12) Uani 1 1 d . . . C14C C 0.6813(4) 0.29261(17) 1.1005(2) 0.0334(10) Uani 1 1 d . . . C14D C 0.8115(6) 0.1121(2) 1.1611(4) 0.0648(19) Uani 1 1 d . . . C14E C 1.6817(5) 0.24431(18) 0.2930(2) 0.0399(11) Uani 1 1 d . . . C14F C 1.7431(5) 0.3645(2) 0.5149(3) 0.0525(14) Uani 1 1 d . . . C14G C 1.0120(5) 0.2283(2) 0.6313(3) 0.0467(13) Uani 1 1 d . . . C14H C 1.2914(7) 0.0530(2) 0.5665(4) 0.0665(18) Uani 1 1 d . . . C14S C 0.4252(9) 1.0702(2) 1.0181(5) 0.086(3) Uani 1 1 d . . . C15A C 1.1903(5) 0.24093(17) 0.8176(3) 0.0412(11) Uani 1 1 d . . . C15B C 1.0918(5) 0.42684(18) 0.8400(3) 0.0434(12) Uani 1 1 d . . . C15C C 0.5128(4) 0.32940(16) 1.0313(2) 0.0337(10) Uani 1 1 d . . . C15D C 0.6820(5) 0.1457(2) 1.0673(3) 0.0547(15) Uani 1 1 d . . . C15E C 1.7388(4) 0.27496(19) 0.4067(3) 0.0423(12) Uani 1 1 d . . . C15F C 1.6567(5) 0.4159(2) 0.4263(3) 0.0508(14) Uani 1 1 d . . . C15G C 1.0333(4) 0.28399(17) 0.5489(2) 0.0377(11) Uani 1 1 d . . . C15H C 1.3042(7) 0.1292(2) 0.5884(3) 0.0579(16) Uani 1 1 d . . . C15S C 0.5044(7) 1.0382(2) 1.0450(4) 0.0705(19) Uani 1 1 d . . . C16S C 0.5072(6) 1.0006(2) 1.0123(3) 0.0539(15) Uani 1 1 d . . . C21S C -0.0117(5) 0.8403(2) 0.8656(3) 0.0531(15) Uani 1 1 d . . . C22S C -0.0929(6) 0.8535(3) 0.9013(3) 0.0629(18) Uani 1 1 d . . . C23S C -0.1586(5) 0.8244(3) 0.9277(3) 0.0647(18) Uani 1 1 d . . . C24S C -0.1418(5) 0.7809(3) 0.9187(3) 0.0618(17) Uani 1 1 d . . . C25S C -0.0591(6) 0.7670(3) 0.8859(3) 0.0609(16) Uani 1 1 d . . . C26S C 0.0063(5) 0.7963(2) 0.8582(3) 0.0578(16) Uani 1 1 d . . . C31S C 0.2262(8) 0.5161(3) 0.6905(4) 0.081(2) Uani 1 1 d . . . C32S C 0.1724(12) 0.4747(3) 0.6760(7) 0.116(4) Uani 1 1 d . . . C33S C 0.0832(9) 0.4697(3) 0.6168(7) 0.113(4) Uani 1 1 d . . . C34S C 0.0515(8) 0.5052(3) 0.5797(8) 0.127(5) Uani 1 1 d . . . C35S C 0.1086(9) 0.5433(3) 0.5928(7) 0.112(4) Uani 1 1 d . . . C36S C 0.1900(8) 0.5497(3) 0.6482(6) 0.095(3) Uani 1 1 d . . . C41S C 0.7428 0.5294 0.7890 0.101(3) Uiso 1 1 d . . . C42S C 0.8618 0.5253 0.7968 0.104(3) Uiso 1 1 d . . . C43S C 0.9168 0.5316 0.7433 0.146(5) Uiso 1 1 d . . . C44S C 0.8529 0.5421 0.6820 0.202(8) Uiso 1 1 d . . . C45S C 0.7339 0.5462 0.6742 0.134(4) Uiso 1 1 d . . . C46S C 0.6789 0.5398 0.7277 0.109(3) Uiso 1 1 d . . . C51S C 0.5518(5) 0.2628(2) 0.6378(3) 0.0488(14) Uani 1 1 d . . . C52S C 0.5132(5) 0.2207(2) 0.6307(3) 0.0553(15) Uani 1 1 d . . . C53S C 0.5619(6) 0.1941(3) 0.5912(3) 0.0629(17) Uani 1 1 d . . . C54S C 0.6489(6) 0.2098(3) 0.5587(3) 0.067(2) Uani 1 1 d . . . C55S C 0.6857(6) 0.2507(3) 0.5671(3) 0.067(2) Uani 1 1 d . . . C56S C 0.6337(6) 0.2777(3) 0.6056(3) 0.0616(17) Uani 1 1 d . . . C61S C 0.2896 0.0832 0.7584 0.081(2) Uiso 1 1 d . . . C62S C 0.1850 0.0629 0.7363 0.140(5) Uiso 1 1 d . . . C63S C 0.1825 0.0198 0.7201 0.235(10) Uiso 1 1 d . . . C64S C 0.2848 -0.0031 0.7260 0.133(4) Uiso 1 1 d . . . C65S C 0.3894 0.0171 0.7481 0.132(4) Uiso 1 1 d . . . C66S C 0.3919 0.0603 0.7643 0.162(6) Uiso 1 1 d . . . C71S C 0.8137 0.0229 0.6069 0.080(2) Uiso 1 1 d . . . C72S C 0.7404 -0.0007 0.5599 0.073(2) Uiso 1 1 d . . . C73S C 0.6396 -0.0178 0.5749 0.081(2) Uiso 1 1 d . . . C74S C 0.6120 -0.0114 0.6370 0.0591(16) Uiso 1 1 d . . . C75S C 0.6853 0.0122 0.6840 0.104(3) Uiso 1 1 d . . . C76S C 0.7861 0.0293 0.6690 0.084(2) Uiso 1 1 d . . . C81S C 0.8943 0.0136 0.8498 0.145(5) Uiso 1 1 d . . . C82S C 0.8959 0.0521 0.8835 0.085(2) Uiso 1 1 d . . . C83S C 0.8045 0.0630 0.9145 0.124(4) Uiso 1 1 d . . . C84S C 0.7115 0.0354 0.9117 0.185(7) Uiso 1 1 d . . . C85S C 0.7099 -0.0032 0.8780 0.137(5) Uiso 1 1 d . . . C86S C 0.8013 -0.0140 0.8471 0.167(6) Uiso 1 1 d . . . Cl1S Cl 0.44213(17) 0.94677(7) 0.91121(10) 0.0681(5) Uani 1 1 d . . . Cl2S Cl 0.07276(16) 0.87702(8) 0.83444(8) 0.0688(5) Uani 1 1 d . . . Cl3S Cl 0.3370(4) 0.52207(11) 0.75615(14) 0.1353(13) Uani 1 1 d . . . Cl4S Cl 0.6811 0.5271 0.8535 0.1417(12) Uiso 1 1 d . . . Cl5S Cl 0.49093(16) 0.29794(9) 0.68836(9) 0.0739(5) Uani 1 1 d . . . Cl6S Cl 0.2744 0.1362 0.7749 0.1314(11) Uiso 1 1 d . . . Cl7S Cl 0.9380 0.0456 0.5941 0.1361(11) Uiso 1 1 d . . . Cl8S Cl 1.0009 0.0012 0.8097 0.219(2) Uiso 1 1 d . . . H1A H 0.4576 0.4358 0.7403 0.048 Uiso 1 1 calc R . . H1B H 0.4487 0.3869 0.7617 0.048 Uiso 1 1 calc R . . H1D H 0.4097 0.4309 0.8474 0.049 Uiso 1 1 calc R . . H1E H 0.5294 0.4556 0.8499 0.049 Uiso 1 1 calc R . . H1G H 0.7165 0.1171 0.6896 0.050 Uiso 1 1 calc R . . H1H H 0.7362 0.1677 0.6870 0.050 Uiso 1 1 calc R . . H1J H 0.9153 0.1331 0.6985 0.051 Uiso 1 1 calc R . . H1K H 0.8918 0.1087 0.7632 0.051 Uiso 1 1 calc R . . H1M H 0.9692 0.3897 0.3137 0.056 Uiso 1 1 calc R . . H1N H 0.9844 0.4405 0.3145 0.056 Uiso 1 1 calc R . . H1R H 1.0562 0.4397 0.4293 0.059 Uiso 1 1 calc R . . H1S H 0.9345 0.4156 0.4161 0.059 Uiso 1 1 calc R . . H1U H 1.2071 0.1408 0.1278 0.062 Uiso 1 1 calc R . . H1V H 1.2341 0.1901 0.1444 0.062 Uiso 1 1 calc R . . H1X H 1.4087 0.1537 0.1429 0.051 Uiso 1 1 calc R . . H1Y H 1.3805 0.1204 0.1970 0.051 Uiso 1 1 calc R . . H2A H 0.6178 0.3956 0.7153 0.040 Uiso 1 1 calc R . . H2B H 0.6623 0.4329 0.7671 0.040 Uiso 1 1 calc R . . H2D H 0.5523 0.4061 0.9367 0.040 Uiso 1 1 calc R . . H2E H 0.5067 0.3680 0.8868 0.040 Uiso 1 1 calc R . . H2G H 0.6047 0.1533 0.7590 0.045 Uiso 1 1 calc R . . H2H H 0.6955 0.1217 0.8019 0.045 Uiso 1 1 calc R . . H2J H 0.9235 0.1994 0.7531 0.047 Uiso 1 1 calc R . . H2K H 1.0130 0.1675 0.7964 0.047 Uiso 1 1 calc R . . H2M H 1.1389 0.4068 0.2731 0.043 Uiso 1 1 calc R . . H2N H 1.1872 0.4335 0.3385 0.043 Uiso 1 1 calc R . . H2R H 1.0756 0.3761 0.4906 0.048 Uiso 1 1 calc R . . H2S H 1.0257 0.3486 0.4262 0.048 Uiso 1 1 calc R . . H2U H 1.1853 0.1277 0.2379 0.051 Uiso 1 1 calc R . . H2V H 1.0996 0.1654 0.2079 0.051 Uiso 1 1 calc R . . H2X H 1.5105 0.1725 0.2501 0.045 Uiso 1 1 calc R . . H2Y H 1.4243 0.2101 0.2206 0.045 Uiso 1 1 calc R . . H3A H 0.6311 0.3456 0.8012 0.034 Uiso 1 1 calc R . . H3D H 0.7147 0.4148 0.8881 0.033 Uiso 1 1 calc R . . H3G H 1.2312 0.2177 0.2604 0.037 Uiso 1 1 calc R . . H3H H 0.7296 0.2122 0.7891 0.039 Uiso 1 1 calc R . . H3J H 0.8781 0.1522 0.8650 0.037 Uiso 1 1 calc R . . H3M H 1.1529 0.3424 0.3338 0.036 Uiso 1 1 calc R . . H3R H 1.2387 0.3945 0.4465 0.037 Uiso 1 1 calc R . . H3X H 1.3749 0.1469 0.3122 0.037 Uiso 1 1 calc R . . H4A H 0.8383 0.3888 0.8104 0.030 Uiso 1 1 calc R . . H4B H 0.6865 0.3337 0.9328 0.031 Uiso 1 1 calc R . . H4C H 0.7030 0.1695 0.9024 0.035 Uiso 1 1 calc R . . H4D H 0.9372 0.2361 0.8578 0.035 Uiso 1 1 calc R . . H4E H 1.3588 0.3869 0.3666 0.033 Uiso 1 1 calc R . . H4F H 1.2051 0.3085 0.4555 0.033 Uiso 1 1 calc R . . H4G H 1.1976 0.1578 0.3533 0.036 Uiso 1 1 calc R . . H4H H 1.4411 0.2296 0.3355 0.034 Uiso 1 1 calc R . . H5A H 0.7771 0.3600 0.7064 0.034 Uiso 1 1 calc R . . H5B H 0.7862 0.3138 0.7407 0.034 Uiso 1 1 calc R . . H5D H 0.8276 0.3517 1.0212 0.035 Uiso 1 1 calc R . . H5E H 0.7184 0.3829 1.0140 0.035 Uiso 1 1 calc R . . H5G H 0.5234 0.1810 0.8388 0.040 Uiso 1 1 d R . . H5H H 0.5524 0.2311 0.8396 0.040 Uiso 1 1 d R . . H5J H 1.0523 0.2279 0.9564 0.038 Uiso 1 1 calc R . . H5K H 1.0784 0.1914 0.9067 0.038 Uiso 1 1 calc R . . H5M H 1.3052 0.3819 0.2539 0.042 Uiso 1 1 calc R . . H5N H 1.3072 0.3310 0.2618 0.042 Uiso 1 1 calc R . . H5R H 1.3430 0.3107 0.5492 0.038 Uiso 1 1 calc R . . H5S H 1.2392 0.3428 0.5542 0.038 Uiso 1 1 calc R . . H5U H 1.0224 0.1812 0.2967 0.040 Uiso 1 1 calc R . . H5V H 1.0594 0.2289 0.3196 0.040 Uiso 1 1 calc R . . H5X H 1.5536 0.2049 0.4293 0.042 Uiso 1 1 calc R . . H5Y H 1.5799 0.1799 0.3660 0.042 Uiso 1 1 calc R . . H7A H 0.9358 0.3785 0.6597 0.038 Uiso 1 1 calc R . . H7C H 0.4060 0.1600 0.9142 0.046 Uiso 1 1 calc R . . H7D H 0.7782 0.4519 1.0411 0.042 Uiso 1 1 calc R . . H7J H 1.1255 0.1290 0.9615 0.042 Uiso 1 1 calc R . . H7M H 1.4710 0.4113 0.2243 0.045 Uiso 1 1 calc R . . H7R H 1.3033 0.4056 0.6050 0.044 Uiso 1 1 calc R . . H7U H 0.8983 0.1492 0.3591 0.045 Uiso 1 1 calc R . . H7X H 1.6233 0.1101 0.3929 0.059 Uiso 1 1 calc R . . H8A H 1.1322 0.3742 0.6543 0.045 Uiso 1 1 calc R . . H8C H 0.3267 0.1729 1.0082 0.045 Uiso 1 1 calc R . . H8D H 0.8878 0.5116 1.0295 0.048 Uiso 1 1 calc R . . H8J H 1.1017 0.0768 1.0398 0.045 Uiso 1 1 calc R . . H8M H 1.6610 0.4086 0.2169 0.049 Uiso 1 1 calc R . . H8R H 1.4353 0.4621 0.6272 0.049 Uiso 1 1 calc R . . H8U H 0.8309 0.1385 0.4573 0.049 Uiso 1 1 calc R . . H8X H 1.5925 0.0459 0.4460 0.078 Uiso 1 1 calc R . . H9A H 1.2551 0.3352 0.7329 0.039 Uiso 1 1 calc R . . H9B H 1.0434 0.5060 0.9743 0.047 Uiso 1 1 calc R . . H9G H 0.3963 0.2284 1.0782 0.041 Uiso 1 1 calc R . . H9J H 0.9626 0.0873 1.1047 0.045 Uiso 1 1 calc R . . H9M H 1.7773 0.3531 0.2665 0.046 Uiso 1 1 calc R . . H9R H 1.6037 0.4601 0.5843 0.044 Uiso 1 1 calc R . . H9U H 0.9093 0.1778 0.5499 0.047 Uiso 1 1 calc R . . H9X H 1.4497 0.0413 0.5089 0.064 Uiso 1 1 calc R . . H10 H 1.0716 0.2921 0.5123 0.045 Uiso 1 1 calc R . . H12A H 0.9443 0.2904 0.9985 0.033 Uiso 1 1 calc R . . H12B H 0.7091 0.2776 0.8168 0.032 Uiso 1 1 calc R . . H12S H 0.3073 1.0204 0.8851 0.070 Uiso 1 1 calc R . . H13 H 0.3013 1.0860 0.9406 0.088 Uiso 1 1 calc R . . H13A H 1.2714 0.2763 0.9360 0.048 Uiso 1 1 calc R . . H13B H 1.1379 0.2884 0.9162 0.048 Uiso 1 1 calc R . . H13C H 1.2340 0.3249 0.9205 0.048 Uiso 1 1 calc R . . H13D H 1.2837 0.4099 0.9298 0.056 Uiso 1 1 calc R . . H13E H 1.1825 0.3831 0.9531 0.056 Uiso 1 1 calc R . . H13F H 1.2394 0.4227 0.9962 0.056 Uiso 1 1 calc R . . H13G H 0.5139 0.3169 1.1591 0.045 Uiso 1 1 calc R . . H13H H 0.5102 0.2658 1.1608 0.045 Uiso 1 1 calc R . . H13I H 0.4064 0.2919 1.1178 0.045 Uiso 1 1 calc R . . H13J H 0.7633 0.1929 1.1744 0.063 Uiso 1 1 calc R . . H13K H 0.8143 0.2137 1.1147 0.063 Uiso 1 1 calc R . . H13L H 0.8985 0.1903 1.1735 0.063 Uiso 1 1 calc R . . H13M H 1.8562 0.2942 0.2745 0.061 Uiso 1 1 calc R . . H13N H 1.8997 0.2627 0.3350 0.061 Uiso 1 1 calc R . . H13O H 1.8918 0.3130 0.3475 0.061 Uiso 1 1 calc R . . H13R H 1.8374 0.4401 0.5142 0.059 Uiso 1 1 calc R . . H13S H 1.7867 0.4352 0.5808 0.059 Uiso 1 1 calc R . . H13T H 1.7321 0.4695 0.5265 0.059 Uiso 1 1 calc R . . H13U H 1.2193 0.2575 0.6362 0.045 Uiso 1 1 calc R . . H13V H 1.2424 0.2477 0.5635 0.045 Uiso 1 1 calc R . . H13W H 1.2247 0.2091 0.6116 0.045 Uiso 1 1 calc R . . H13X H 1.1118 0.0977 0.5157 0.073 Uiso 1 1 calc R . . H13Y H 1.1632 0.0799 0.4542 0.073 Uiso 1 1 calc R . . H13Z H 1.1658 0.1301 0.4694 0.073 Uiso 1 1 calc R . . H14 H 0.4217 1.0963 1.0414 0.103 Uiso 1 1 calc R . . H14A H 1.3970 0.2759 0.8598 0.064 Uiso 1 1 calc R . . H14B H 1.3693 0.3244 0.8383 0.064 Uiso 1 1 calc R . . H14C H 1.3571 0.2876 0.7836 0.064 Uiso 1 1 calc R . . H14D H 1.2494 0.4830 0.8851 0.050 Uiso 1 1 calc R . . H14E H 1.2119 0.4963 0.9531 0.050 Uiso 1 1 calc R . . H14F H 1.1283 0.5062 0.8847 0.050 Uiso 1 1 calc R . . H14G H 0.6966 0.3182 1.1281 0.040 Uiso 1 1 calc R . . H14H H 0.7235 0.2946 1.0637 0.040 Uiso 1 1 calc R . . H14I H 0.7067 0.2672 1.1268 0.040 Uiso 1 1 calc R . . H14J H 0.7518 0.1165 1.1879 0.078 Uiso 1 1 calc R . . H14K H 0.8876 0.1130 1.1894 0.078 Uiso 1 1 calc R . . H14L H 0.8004 0.0841 1.1394 0.078 Uiso 1 1 calc R . . H14M H 1.6771 0.2498 0.2458 0.048 Uiso 1 1 calc R . . H14N H 1.6044 0.2386 0.3021 0.048 Uiso 1 1 calc R . . H14O H 1.7314 0.2195 0.3060 0.048 Uiso 1 1 calc R . . H14R H 1.8151 0.3646 0.4975 0.063 Uiso 1 1 calc R . . H14S H 1.6931 0.3415 0.4939 0.063 Uiso 1 1 calc R . . H14T H 1.7602 0.3598 0.5627 0.063 Uiso 1 1 calc R . . H14U H 1.0396 0.2481 0.6675 0.056 Uiso 1 1 calc R . . H14V H 1.0318 0.1989 0.6456 0.056 Uiso 1 1 calc R . . H14W H 0.9282 0.2309 0.6185 0.056 Uiso 1 1 calc R . . H14X H 1.2285 0.0518 0.5917 0.080 Uiso 1 1 calc R . . H14Y H 1.3651 0.0486 0.5964 0.080 Uiso 1 1 calc R . . H14Z H 1.2806 0.0306 0.5328 0.080 Uiso 1 1 calc R . . H15 H 0.5553 1.0429 1.0856 0.085 Uiso 1 1 calc R . . H15A H 1.2426 0.2220 0.8467 0.049 Uiso 1 1 calc R . . H15B H 1.1976 0.2356 0.7717 0.049 Uiso 1 1 calc R . . H15C H 1.1108 0.2355 0.8232 0.049 Uiso 1 1 calc R . . H15D H 1.1602 0.4263 0.8191 0.052 Uiso 1 1 calc R . . H15E H 1.0347 0.4465 0.8159 0.052 Uiso 1 1 calc R . . H15F H 1.0587 0.3981 0.8392 0.052 Uiso 1 1 calc R . . H15G H 0.5320 0.3551 1.0582 0.040 Uiso 1 1 calc R . . H15H H 0.4293 0.3282 1.0158 0.040 Uiso 1 1 calc R . . H15I H 0.5522 0.3302 0.9934 0.040 Uiso 1 1 calc R . . H15J H 0.6251 0.1487 1.0963 0.066 Uiso 1 1 calc R . . H15K H 0.6708 0.1182 1.0442 0.066 Uiso 1 1 calc R . . H15L H 0.6724 0.1690 1.0350 0.066 Uiso 1 1 calc R . . H15M H 1.7875 0.2499 0.4198 0.051 Uiso 1 1 calc R . . H15N H 1.6613 0.2696 0.4157 0.051 Uiso 1 1 calc R . . H15O H 1.7719 0.3000 0.4318 0.051 Uiso 1 1 calc R . . H15R H 1.7291 0.4163 0.4092 0.061 Uiso 1 1 calc R . . H15S H 1.6181 0.4436 0.4180 0.061 Uiso 1 1 calc R . . H15T H 1.6067 0.3933 0.4042 0.061 Uiso 1 1 calc R . . H15U H 1.0552 0.3040 0.5855 0.045 Uiso 1 1 calc R . . H15V H 0.9496 0.2848 0.5343 0.045 Uiso 1 1 calc R . . H15X H 1.2430 0.1251 0.6143 0.070 Uiso 1 1 calc R . . H15Y H 1.2983 0.1580 0.5694 0.070 Uiso 1 1 calc R . . H15Z H 1.3794 0.1258 0.6170 0.070 Uiso 1 1 calc R . . H16S H 0.5586 0.9785 1.0303 0.065 Uiso 1 1 calc R . . H22S H -0.1037 0.8832 0.9079 0.075 Uiso 1 1 calc R . . H23S H -0.2153 0.8338 0.9519 0.078 Uiso 1 1 calc R . . H24S H -0.1890 0.7607 0.9357 0.074 Uiso 1 1 calc R . . H25S H -0.0460 0.7372 0.8819 0.073 Uiso 1 1 calc R . . H26S H 0.0631 0.7867 0.8342 0.069 Uiso 1 1 calc R . . H32S H 0.1946 0.4511 0.7044 0.139 Uiso 1 1 calc R . . H33S H 0.0488 0.4427 0.6048 0.136 Uiso 1 1 calc R . . H34E H 1.2237 0.2783 0.3183 0.032 Uiso 1 1 calc R . . H34F H 1.4572 0.2556 0.4976 0.033 Uiso 1 1 calc R . . H34S H -0.0115 0.5036 0.5440 0.152 Uiso 1 1 calc R . . H35S H 0.0909 0.5662 0.5622 0.135 Uiso 1 1 calc R . . H36S H 0.2218 0.5774 0.6577 0.114 Uiso 1 1 calc R . . H42S H 0.9056 0.5181 0.8387 0.124 Uiso 1 1 calc R . . H43S H 0.9981 0.5288 0.7487 0.175 Uiso 1 1 calc R . . H44S H 0.8905 0.5465 0.6455 0.242 Uiso 1 1 calc R . . H45S H 0.6901 0.5534 0.6324 0.161 Uiso 1 1 calc R . . H46S H 0.5975 0.5426 0.7224 0.131 Uiso 1 1 calc R . . H52S H 0.4542 0.2107 0.6528 0.066 Uiso 1 1 calc R . . H53S H 0.5375 0.1651 0.5856 0.076 Uiso 1 1 calc R . . H54S H 0.6821 0.1915 0.5305 0.080 Uiso 1 1 calc R . . H55S H 0.7468 0.2607 0.5467 0.080 Uiso 1 1 calc R . . H56S H 0.6556 0.3070 0.6095 0.074 Uiso 1 1 calc R . . H62S H 0.1151 0.0786 0.7322 0.169 Uiso 1 1 calc R . . H63S H 0.1110 0.0060 0.7051 0.282 Uiso 1 1 calc R . . H64S H 0.2831 -0.0326 0.7150 0.160 Uiso 1 1 calc R . . H65S H 0.4593 0.0014 0.7522 0.158 Uiso 1 1 calc R . . H66S H 0.4634 0.0741 0.7794 0.194 Uiso 1 1 calc R . . H72S H 0.7593 -0.0051 0.5175 0.088 Uiso 1 1 calc R . . H73S H 0.5895 -0.0339 0.5428 0.097 Uiso 1 1 calc R . . H74S H 0.5431 -0.0231 0.6472 0.071 Uiso 1 1 calc R . . H75S H 0.6664 0.0166 0.7264 0.125 Uiso 1 1 calc R . . H76S H 0.8362 0.0454 0.7011 0.101 Uiso 1 1 calc R . . H82S H 0.9594 0.0710 0.8854 0.102 Uiso 1 1 calc R . . H83S H 0.8056 0.0894 0.9375 0.149 Uiso 1 1 calc R . . H84S H 0.6491 0.0428 0.9329 0.222 Uiso 1 1 calc R . . H85S H 0.6464 -0.0221 0.8761 0.164 Uiso 1 1 calc R . . H86S H 0.8002 -0.0404 0.8240 0.200 Uiso 1 1 calc R . . N4A N 0.7991(3) 0.36289(12) 0.80663(17) 0.0254(7) Uani 1 1 d . . . N4B N 0.7379(3) 0.35517(13) 0.92661(17) 0.0258(7) Uani 1 1 d . . . N4C N 0.6927(3) 0.19428(13) 0.87716(18) 0.0296(8) Uani 1 1 d . . . N4D N 0.9146(3) 0.21473(13) 0.88419(18) 0.0289(8) Uani 1 1 d . . . N4E N 1.3205(3) 0.36235(13) 0.34909(18) 0.0279(7) Uani 1 1 d . . . N4F N 1.2578(3) 0.33084(13) 0.45871(17) 0.0277(8) Uani 1 1 d . . . N4G N 1.1922(3) 0.18611(13) 0.33923(18) 0.0303(8) Uani 1 1 d . . . N4H N 1.4169(3) 0.20451(13) 0.35289(17) 0.0281(8) Uani 1 1 d . . . O11A O 0.9734(3) 0.30137(11) 0.84112(14) 0.0273(6) Uani 1 1 d . . . O11B O 0.9687(2) 0.36986(11) 0.92332(14) 0.0270(6) Uani 1 1 d . . . O11C O 0.6612(2) 0.26380(11) 0.95909(15) 0.0275(6) Uani 1 1 d . . . O11D O 0.8354(3) 0.20721(11) 1.00349(15) 0.0290(6) Uani 1 1 d . . . O11E O 1.4894(2) 0.29765(11) 0.35218(14) 0.0278(6) Uani 1 1 d . . . O11F O 1.4927(3) 0.34465(11) 0.46411(15) 0.0303(7) Uani 1 1 d . . . O11G O 1.1723(3) 0.23751(11) 0.44925(15) 0.0285(6) Uani 1 1 d . . . O11H O 1.3356(3) 0.17459(12) 0.46360(16) 0.0338(7) Uani 1 1 d . . . O12A O 0.8923(3) 0.28766(11) 0.95787(14) 0.0272(6) Uani 1 1 d . . . O12B O 0.7618(2) 0.28040(11) 0.85725(14) 0.0264(6) Uani 1 1 d . . . O34E O 1.2757(2) 0.27316(11) 0.35833(14) 0.0264(6) Uani 1 1 d . . . O34F O 1.4051(3) 0.26076(11) 0.45760(14) 0.0273(6) 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 Al1 0.0257(6) 0.0230(6) 0.0227(6) 0.0005(5) 0.0044(5) 0.0001(5) Al2 0.0290(6) 0.0218(6) 0.0235(6) 0.0005(5) 0.0049(5) -0.0010(5) Al3 0.0269(6) 0.0252(6) 0.0230(6) -0.0009(5) 0.0038(5) -0.0007(5) Al4 0.0287(6) 0.0266(6) 0.0232(6) 0.0000(5) 0.0043(5) 0.0004(5) C1A 0.041(3) 0.048(3) 0.031(2) 0.011(2) 0.005(2) 0.013(2) C1B 0.035(3) 0.054(3) 0.035(3) 0.009(2) 0.011(2) 0.020(2) C1C 0.045(3) 0.048(3) 0.031(2) -0.011(2) 0.007(2) 0.006(2) C1D 0.052(3) 0.040(3) 0.036(3) -0.009(2) 0.012(2) 0.003(2) C1E 0.034(3) 0.048(3) 0.058(3) 0.015(3) 0.010(2) 0.011(2) C1F 0.033(3) 0.064(4) 0.057(3) 0.010(3) 0.021(2) 0.018(2) C1G 0.057(3) 0.070(4) 0.030(3) -0.014(3) 0.014(2) -0.019(3) C1H 0.056(3) 0.045(3) 0.028(2) -0.011(2) 0.014(2) -0.008(2) C2A 0.039(2) 0.035(2) 0.025(2) 0.0075(18) 0.0048(18) 0.008(2) C2B 0.032(2) 0.037(2) 0.031(2) 0.0028(19) 0.0087(18) 0.0051(19) C2C 0.043(3) 0.036(3) 0.031(2) -0.007(2) 0.003(2) -0.002(2) C2D 0.045(3) 0.043(3) 0.031(2) -0.005(2) 0.010(2) 0.002(2) C2E 0.031(2) 0.035(2) 0.041(3) 0.009(2) 0.0050(19) 0.0024(19) C2F 0.029(2) 0.044(3) 0.048(3) 0.005(2) 0.012(2) 0.006(2) C2G 0.046(3) 0.053(3) 0.030(2) -0.014(2) 0.012(2) -0.009(2) C2H 0.041(3) 0.040(3) 0.032(2) -0.002(2) 0.008(2) -0.004(2) C3A 0.025(2) 0.028(2) 0.032(2) 0.0047(18) 0.0075(17) 0.0055(17) C3B 0.027(2) 0.028(2) 0.028(2) 0.0045(17) 0.0047(17) 0.0008(17) C3C 0.037(2) 0.028(2) 0.031(2) -0.0016(18) 0.0062(19) -0.0007(18) C3D 0.038(2) 0.024(2) 0.029(2) -0.0027(17) 0.0053(18) -0.0029(18) C3E 0.024(2) 0.032(2) 0.034(2) 0.0036(18) 0.0014(17) 0.0001(17) C3F 0.030(2) 0.033(2) 0.030(2) 0.0027(18) 0.0079(17) -0.0018(18) C3G 0.038(2) 0.026(2) 0.028(2) -0.0025(17) 0.0069(18) -0.0066(18) C3H 0.038(2) 0.028(2) 0.027(2) -0.0005(17) 0.0039(18) 0.0030(18) C5A 0.031(2) 0.033(2) 0.021(2) -0.0050(17) 0.0054(16) -0.0003(17) C5B 0.028(2) 0.034(2) 0.025(2) -0.0007(18) 0.0049(17) -0.0017(18) C5C 0.032(2) 0.032(2) 0.034(2) -0.0032(19) 0.0017(19) -0.0018(19) C5D 0.032(2) 0.032(2) 0.030(2) -0.0041(18) 0.0024(18) 0.0016(18) C5E 0.033(2) 0.041(3) 0.030(2) 0.004(2) 0.0041(18) 0.004(2) C5F 0.033(2) 0.037(2) 0.025(2) -0.0017(18) 0.0092(18) -0.0006(19) C5G 0.034(2) 0.034(2) 0.031(2) -0.0035(18) 0.0001(18) 0.0049(19) C5H 0.032(2) 0.043(3) 0.030(2) 0.004(2) 0.0054(19) 0.007(2) C6A 0.029(2) 0.031(2) 0.025(2) -0.0056(17) 0.0092(17) 0.0009(17) C6B 0.036(2) 0.030(2) 0.023(2) -0.0029(17) 0.0047(17) 0.0014(18) C6C 0.026(2) 0.035(2) 0.035(2) 0.0032(19) 0.0022(18) -0.0020(18) C6D 0.034(2) 0.029(2) 0.027(2) -0.0034(17) 0.0007(17) -0.0001(18) C6E 0.033(2) 0.035(2) 0.027(2) -0.0012(18) 0.0072(18) 0.0065(19) C6F 0.034(2) 0.035(2) 0.019(2) 0.0000(17) -0.0002(16) -0.0018(19) C6G 0.037(2) 0.028(2) 0.037(2) 0.0009(19) 0.0005(19) 0.0026(19) C6H 0.048(3) 0.035(3) 0.030(2) 0.0033(19) -0.002(2) 0.008(2) C7A 0.038(2) 0.033(2) 0.023(2) -0.0034(17) 0.0056(17) 0.0015(19) C7B 0.033(2) 0.037(3) 0.037(3) -0.007(2) 0.012(2) 0.0012(19) C7C 0.033(2) 0.033(2) 0.048(3) 0.002(2) 0.003(2) -0.0061(19) C7D 0.033(2) 0.033(2) 0.038(3) -0.0038(19) 0.0050(19) 0.0056(19) C7E 0.045(3) 0.037(3) 0.033(2) 0.003(2) 0.010(2) 0.009(2) C7F 0.041(3) 0.040(3) 0.030(2) -0.004(2) 0.0097(19) -0.004(2) C7G 0.035(2) 0.039(3) 0.037(3) -0.007(2) 0.006(2) -0.005(2) C7H 0.053(3) 0.046(3) 0.051(3) 0.000(3) 0.014(3) 0.015(3) C8A 0.052(3) 0.031(2) 0.034(2) 0.0004(19) 0.022(2) -0.003(2) C8B 0.050(3) 0.028(2) 0.045(3) -0.015(2) 0.016(2) -0.005(2) C8C 0.030(2) 0.040(3) 0.046(3) 0.007(2) 0.010(2) -0.0055(19) C8D 0.042(3) 0.026(2) 0.042(3) -0.0055(19) 0.000(2) 0.0053(19) C8E 0.052(3) 0.032(2) 0.040(3) 0.004(2) 0.014(2) -0.006(2) C8F 0.057(3) 0.035(3) 0.029(2) -0.009(2) 0.008(2) -0.004(2) C8G 0.034(2) 0.041(3) 0.048(3) 0.001(2) 0.009(2) -0.008(2) C8H 0.079(5) 0.038(3) 0.077(5) 0.016(3) 0.012(4) 0.032(3) C9A 0.032(2) 0.036(2) 0.033(2) -0.0010(19) 0.0122(18) -0.0005(19) C9B 0.038(3) 0.030(2) 0.050(3) -0.005(2) 0.012(2) -0.007(2) C9C 0.035(2) 0.031(2) 0.039(3) 0.004(2) 0.0120(19) -0.0028(19) C9D 0.043(3) 0.031(2) 0.039(3) 0.006(2) 0.006(2) -0.001(2) C9E 0.035(3) 0.044(3) 0.038(3) -0.004(2) 0.011(2) -0.002(2) C9F 0.050(3) 0.032(2) 0.027(2) -0.0015(18) 0.003(2) -0.006(2) C9G 0.038(3) 0.042(3) 0.040(3) -0.003(2) 0.014(2) -0.005(2) C9H 0.070(4) 0.034(3) 0.054(3) 0.013(2) 0.009(3) 0.012(3) C10A 0.037(2) 0.023(2) 0.034(2) 0.0006(17) 0.0089(19) -0.0022(17) C10B 0.033(2) 0.029(2) 0.033(2) -0.0015(18) 0.0042(18) -0.0062(18) C10C 0.029(2) 0.029(2) 0.031(2) 0.0046(17) 0.0057(17) -0.0027(17) C10D 0.039(2) 0.028(2) 0.030(2) 0.0002(17) 0.0042(19) 0.0025(18) C10E 0.028(2) 0.039(2) 0.028(2) -0.0016(18) 0.0074(17) 0.0000(18) C10F 0.032(2) 0.036(2) 0.026(2) 0.0006(18) 0.0030(17) -0.0087(19) C10G 0.032(2) 0.031(2) 0.036(2) 0.0021(19) 0.0046(19) -0.0019(18) C10H 0.050(3) 0.029(2) 0.036(3) 0.0043(19) 0.001(2) 0.002(2) C11A 0.030(2) 0.026(2) 0.0230(19) -0.0045(16) 0.0040(16) -0.0041(17) C11B 0.028(2) 0.026(2) 0.029(2) -0.0016(17) 0.0030(17) 0.0008(17) C11C 0.026(2) 0.027(2) 0.028(2) 0.0061(17) 0.0033(16) 0.0004(17) C11D 0.031(2) 0.024(2) 0.032(2) -0.0012(17) 0.0019(17) 0.0000(17) C11E 0.031(2) 0.031(2) 0.0222(19) -0.0035(17) 0.0080(16) -0.0042(17) C11F 0.034(2) 0.025(2) 0.028(2) -0.0001(17) 0.0003(17) -0.0024(17) C11G 0.029(2) 0.027(2) 0.034(2) 0.0009(17) 0.0064(18) 0.0012(17) C11H 0.039(3) 0.035(3) 0.031(2) 0.0017(19) -0.0007(19) 0.004(2) C11S 0.049(3) 0.039(3) 0.055(3) 0.004(2) 0.024(3) -0.001(2) C12A 0.029(2) 0.033(2) 0.041(3) -0.002(2) 0.0101(19) 0.0029(18) C12B 0.042(3) 0.030(2) 0.034(2) -0.0016(19) 0.010(2) -0.007(2) C12C 0.033(2) 0.027(2) 0.030(2) 0.0002(18) 0.0104(18) -0.0053(18) C12D 0.048(3) 0.036(3) 0.052(3) 0.019(2) 0.022(2) 0.009(2) C12E 0.033(2) 0.039(3) 0.037(3) -0.001(2) 0.011(2) 0.001(2) C12F 0.035(3) 0.042(3) 0.041(3) -0.009(2) 0.008(2) -0.010(2) C12G 0.030(2) 0.042(3) 0.031(2) 0.002(2) 0.0114(18) -0.0043(19) C12H 0.055(3) 0.033(3) 0.052(3) 0.007(2) 0.010(3) 0.002(2) C12S 0.049(3) 0.055(4) 0.074(4) 0.014(3) 0.020(3) 0.000(3) C13A 0.037(3) 0.044(3) 0.037(3) -0.006(2) 0.000(2) 0.007(2) C13B 0.037(3) 0.042(3) 0.062(4) 0.004(3) 0.015(2) -0.001(2) C13C 0.035(2) 0.045(3) 0.032(2) -0.001(2) 0.0089(19) -0.003(2) C13D 0.067(4) 0.052(3) 0.043(3) 0.009(3) 0.021(3) 0.014(3) C13E 0.030(3) 0.056(3) 0.069(4) 0.008(3) 0.017(3) 0.005(2) C13F 0.045(3) 0.041(3) 0.058(3) -0.002(3) 0.004(3) -0.017(2) C13G 0.030(2) 0.048(3) 0.034(2) -0.001(2) 0.0063(19) -0.005(2) C13H 0.062(4) 0.047(3) 0.072(4) 0.009(3) 0.008(3) -0.008(3) C13S 0.068(4) 0.045(4) 0.108(6) 0.006(4) 0.019(4) 0.003(3) C14A 0.031(3) 0.069(4) 0.063(4) 0.025(3) 0.013(2) 0.005(3) C14B 0.037(3) 0.034(3) 0.055(3) -0.009(2) 0.013(2) -0.012(2) C14C 0.029(2) 0.039(3) 0.032(2) 0.001(2) 0.0039(18) -0.0008(19) C14D 0.077(4) 0.064(4) 0.064(4) 0.032(3) 0.043(4) 0.019(3) C14E 0.042(3) 0.045(3) 0.032(2) -0.005(2) 0.007(2) 0.009(2) C14F 0.031(3) 0.051(3) 0.075(4) -0.008(3) 0.008(3) -0.006(2) C14G 0.048(3) 0.062(4) 0.031(3) 0.008(2) 0.010(2) -0.008(3) C14H 0.092(5) 0.051(4) 0.061(4) 0.015(3) 0.024(4) 0.004(3) C14S 0.114(7) 0.047(4) 0.105(7) -0.017(4) 0.042(6) -0.005(4) C15A 0.052(3) 0.029(2) 0.041(3) 0.001(2) 0.004(2) 0.006(2) C15B 0.055(3) 0.040(3) 0.042(3) -0.006(2) 0.027(2) -0.017(2) C15C 0.037(2) 0.027(2) 0.036(2) -0.0019(19) 0.0048(19) 0.0032(19) C15D 0.042(3) 0.053(3) 0.073(4) 0.018(3) 0.022(3) 0.001(3) C15E 0.033(2) 0.053(3) 0.037(3) -0.003(2) -0.003(2) 0.008(2) C15F 0.045(3) 0.071(4) 0.040(3) 0.003(3) 0.016(2) -0.010(3) C15G 0.042(3) 0.040(3) 0.031(2) -0.004(2) 0.009(2) -0.002(2) C15H 0.085(5) 0.045(3) 0.051(3) 0.010(3) 0.031(3) 0.002(3) C15S 0.085(5) 0.062(4) 0.064(4) -0.008(3) 0.013(4) -0.009(4) C16S 0.056(3) 0.041(3) 0.064(4) 0.005(3) 0.008(3) -0.004(3) C21S 0.043(3) 0.082(4) 0.031(3) 0.001(3) -0.002(2) 0.007(3) C22S 0.054(4) 0.083(5) 0.052(4) -0.014(3) 0.010(3) 0.014(3) C23S 0.044(3) 0.099(6) 0.053(4) -0.017(4) 0.012(3) 0.001(3) C24S 0.040(3) 0.091(5) 0.053(4) -0.007(3) 0.003(3) -0.012(3) C25S 0.049(3) 0.070(4) 0.063(4) -0.003(3) 0.005(3) 0.002(3) C26S 0.047(3) 0.077(4) 0.049(3) -0.001(3) 0.008(3) 0.013(3) C31S 0.106(6) 0.069(5) 0.080(5) 0.022(4) 0.048(5) 0.026(4) C32S 0.173(11) 0.050(5) 0.155(10) 0.038(6) 0.110(9) 0.026(6) C33S 0.095(7) 0.052(5) 0.199(13) 0.030(7) 0.047(8) 0.012(5) C34S 0.066(6) 0.086(7) 0.222(15) 0.048(8) 0.008(7) -0.010(5) C35S 0.099(7) 0.063(5) 0.169(11) 0.042(6) 0.007(7) 0.001(5) C36S 0.075(5) 0.061(5) 0.155(9) 0.031(5) 0.035(6) 0.012(4) C51S 0.040(3) 0.076(4) 0.032(3) -0.003(3) 0.011(2) -0.003(3) C52S 0.036(3) 0.085(5) 0.042(3) 0.001(3) -0.001(2) -0.005(3) C53S 0.051(4) 0.071(4) 0.059(4) -0.002(3) -0.013(3) 0.002(3) C54S 0.051(4) 0.113(6) 0.030(3) -0.008(3) -0.009(2) 0.018(4) C55S 0.051(4) 0.115(6) 0.034(3) -0.003(3) 0.004(3) 0.001(4) C56S 0.054(4) 0.089(5) 0.040(3) 0.003(3) 0.004(3) -0.019(3) Cl1S 0.0788(11) 0.0456(8) 0.0880(13) -0.0112(8) 0.0370(10) -0.0057(8) Cl2S 0.0698(10) 0.0850(12) 0.0538(9) 0.0117(8) 0.0175(8) 0.0070(9) Cl3S 0.211(4) 0.109(2) 0.0805(16) -0.0009(14) 0.0115(19) 0.073(2) Cl5S 0.0676(10) 0.1002(14) 0.0557(9) -0.0297(9) 0.0161(8) -0.0121(9) N4A 0.0280(18) 0.0245(17) 0.0245(17) -0.0019(14) 0.0071(14) -0.0019(14) N4B 0.0262(17) 0.0290(18) 0.0222(17) 0.0003(14) 0.0040(14) -0.0023(14) N4C 0.035(2) 0.0265(18) 0.0267(18) 0.0015(14) 0.0054(15) -0.0016(15) N4D 0.0334(19) 0.0249(18) 0.0289(18) 0.0000(14) 0.0065(15) -0.0020(15) N4E 0.0294(18) 0.0269(18) 0.0281(18) 0.0001(14) 0.0072(14) 0.0005(14) N4F 0.0255(17) 0.0314(19) 0.0262(18) -0.0075(15) 0.0043(14) -0.0010(15) N4G 0.035(2) 0.0261(18) 0.0301(19) -0.0001(15) 0.0062(15) -0.0010(15) N4H 0.0302(19) 0.0274(18) 0.0258(18) 0.0026(15) 0.0025(14) 0.0030(15) O11A 0.0309(15) 0.0257(15) 0.0255(14) -0.0013(12) 0.0055(12) 0.0024(12) O11B 0.0296(15) 0.0230(14) 0.0291(15) -0.0021(12) 0.0073(12) -0.0004(12) O11C 0.0261(15) 0.0265(15) 0.0306(16) 0.0006(12) 0.0070(12) -0.0030(12) O11D 0.0314(16) 0.0260(15) 0.0301(16) 0.0010(12) 0.0069(12) 0.0027(12) O11E 0.0266(15) 0.0291(15) 0.0276(15) 0.0006(12) 0.0051(12) 0.0022(12) O11F 0.0313(16) 0.0311(16) 0.0279(15) -0.0054(12) 0.0038(12) -0.0011(12) O11G 0.0308(15) 0.0267(15) 0.0295(15) -0.0020(12) 0.0098(12) -0.0029(12) O11H 0.0373(17) 0.0316(17) 0.0318(16) 0.0013(13) 0.0047(13) 0.0030(14) O12A 0.0293(15) 0.0250(15) 0.0263(15) 0.0001(12) 0.0017(12) -0.0017(12) O12B 0.0283(15) 0.0280(15) 0.0222(14) 0.0010(11) 0.0023(11) -0.0031(12) O34E 0.0282(15) 0.0283(15) 0.0220(14) 0.0004(11) 0.0026(11) 0.0009(12) O34F 0.0302(15) 0.0285(15) 0.0217(14) 0.0012(12) 0.0009(11) 0.0023(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 Al2 2.9911(17) . ? Al1 N4A 2.078(4) . ? Al1 N4B 2.088(4) . ? Al1 O11A 1.849(3) . ? Al1 O11B 1.848(3) . ? Al1 O12A 1.867(3) . ? Al1 O12B 1.958(3) . ? Al2 N4C 2.098(4) . ? Al2 N4D 2.088(4) . ? Al2 O11C 1.847(3) . ? Al2 O11D 1.840(3) . ? Al2 O12A 1.873(3) . ? Al2 O12B 1.928(3) . ? Al3 Al4 2.9974(18) . ? Al3 N4E 2.092(4) . ? Al3 N4F 2.099(4) . ? Al3 O11F 1.841(3) . ? Al3 O34E 1.947(3) . ? Al4 N4G 2.095(4) . ? Al4 N4H 2.091(4) . ? Al4 O11G 1.850(3) . ? Al4 O11H 1.834(3) . ? Al4 O34E 1.937(3) . ? C1A C1B 1.522(7) . ? C1A C2A 1.543(7) . ? C1A H1A 0.9900 . ? C1A H1B 0.9900 . ? C1B H1D 0.9900 . ? C1B H1E 0.9900 . ? C1C H1G 0.9900 . ? C1C H1H 0.9900 . ? C1D C1C 1.516(8) . ? C1D C2D 1.523(7) . ? C1D H1J 0.9900 . ? C1D H1K 0.9900 . ? C1E H1M 0.9900 . ? C1E H1N 0.9900 . ? C1F C1E 1.543(8) . ? C1F H1R 0.9900 . ? C1F H1S 0.9900 . ? C1G C1H 1.524(9) . ? C1G H1U 0.9900 . ? C1G H1V 0.9900 . ? C1H H1X 0.9900 . ? C1H H1Y 0.9900 . ? C2A H2A 0.9900 . ? C2A H2B 0.9900 . ? C2B C1B 1.523(6) . ? C2B H2D 0.9900 . ? C2B H2E 0.9900 . ? C2C C1C 1.540(7) . ? C2C H2G 0.9900 . ? C2C H2H 0.9900 . ? C2D H2J 0.9900 . ? C2D H2K 0.9900 . ? C2E C1E 1.536(7) . ? C2E C3E 1.528(6) . ? C2E H2M 0.9900 . ? C2E H2N 0.9900 . ? C2F C1F 1.526(7) . ? C2F H2R 0.9900 . ? C2F H2S 0.9900 . ? C2G C1G 1.527(7) . ? C2G C3G 1.546(6) . ? C2G H2U 0.9900 . ? C2G H2V 0.9900 . ? C2H C1H 1.531(7) . ? C2H C3H 1.526(6) . ? C2H H2X 0.9900 . ? C2H H2Y 0.9900 . ? C3A C2A 1.512(6) . ? C3A H3A 1.0000 . ? C3B C2B 1.513(5) . ? C3B C3A 1.544(6) . ? C3B H3D 1.0000 . ? C3C C2C 1.536(6) . ? C3C C3D 1.504(7) . ? C3C H3H 1.0000 . ? C3D C2D 1.534(7) . ? C3D H3J 1.0000 . ? C3E H3M 1.0000 . ? C3F C2F 1.525(6) . ? C3F C3E 1.537(6) . ? C3F H3R 1.0000 . ? C3G C3H 1.545(6) . ? C3G H3G 1.0000 . ? C3H H3X 1.0000 . ? C5A H5A 0.9900 . ? C5A H5B 0.9900 . ? C5B C6B 1.502(6) . ? C5B H5D 0.9900 . ? C5B H5E 0.9900 . ? C5C C6C 1.497(6) . ? C5C H5G 0.9900 . ? C5C H5H 0.9901 . ? C5D H5J 0.9900 . ? C5D H5K 0.9900 . ? C5E H5M 0.9900 . ? C5E H5N 0.9900 . ? C5F C6F 1.508(6) . ? C5F H5R 0.9900 . ? C5F H5S 0.9900 . ? C5G H5U 0.9900 . ? C5G H5V 0.9900 . ? C5H H5X 0.9900 . ? C5H H5Y 0.9900 . ? C6A C5A 1.501(6) . ? C6A C7A 1.381(6) . ? C6A C11A 1.417(6) . ? C6B C11B 1.405(6) . ? C6D C5D 1.491(7) . ? C6D C7D 1.415(6) . ? C6D C11D 1.397(7) . ? C6E C5E 1.502(6) . ? C6E C7E 1.393(7) . ? C6F C7F 1.394(7) . ? C6G C5G 1.509(7) . ? C6G C7G 1.387(7) . ? C6H C5H 1.495(7) . ? C6H C7H 1.385(7) . ? C6H C11H 1.420(8) . ? C7A C8A 1.390(7) . ? C7A H7A 0.9500 . ? C7B C6B 1.399(6) . ? C7B C8B 1.360(7) . ? C7B H7D 0.9500 . ? C7C C6C 1.411(7) . ? C7C H7C 0.9500 . ? C7D H7J 0.9500 . ? C7E C8E 1.333(8) . ? C7E H7M 0.9500 . ? C7F H7R 0.9500 . ? C7G C8G 1.374(7) . ? C7G H7U 0.9500 . ? C7H C8H 1.396(9) . ? C7H H7X 0.9500 . ? C8A H8A 0.9500 . ? C8B C9B 1.394(7) . ? C8B H8D 0.9500 . ? C8C C7C 1.376(8) . ? C8C H8C 0.9500 . ? C8D C7D 1.389(7) . ? C8D C9D 1.384(8) . ? C8D H8J 0.9500 . ? C8E H8M 0.9500 . ? C8F C7F 1.391(7) . ? C8F H8R 0.9500 . ? C8G C9G 1.385(7) . ? C8G H8U 0.9500 . ? C8H H8X 0.9500 . ? C9A C8A 1.383(7) . ? C9A C10A 1.414(6) . ? C9A H9A 0.9500 . ? C9B H9B 0.9500 . ? C9C C8C 1.387(7) . ? C9C H9G 0.9500 . ? C9D C10D 1.392(7) . ? C9D H9J 0.9500 . ? C9E C8E 1.401(7) . ? C9E C10E 1.393(7) . ? C9E H9M 0.9500 . ? C9F C8F 1.379(8) . ? C9F C10F 1.400(7) . ? C9F H9R 0.9500 . ? C9G H9U 0.9500 . ? C9H C8H 1.374(10) . ? C9H H9X 0.9500 . ? C10A C11A 1.419(6) . ? C10A C12A 1.534(6) . ? C10B C9B 1.397(7) . ? C10B C11B 1.431(6) . ? C10B C12B 1.535(7) . ? C10C C9C 1.403(6) . ? C10C C11C 1.432(6) . ? C10C C12C 1.518(6) . ? C10E C11E 1.432(6) . ? C10E C12E 1.538(7) . ? C10F C12F 1.536(7) . ? C10G C9G 1.397(7) . ? C10G C12G 1.544(7) . ? C10H C9H 1.401(8) . ? C10H C12H 1.520(8) . ? C11C C6C 1.405(6) . ? C11D C10D 1.442(6) . ? C11E C6E 1.410(6) . ? C11F C6F 1.387(7) . ? C11F C10F 1.450(6) . ? C11G C6G 1.423(6) . ? C11G C10G 1.408(7) . ? C11H C10H 1.428(7) . ? C11S C12S 1.378(9) . ? C11S C16S 1.361(9) . ? C12A C13A 1.541(7) . ? C12A C14A 1.528(7) . ? C12A C15A 1.545(7) . ? C12B C13B 1.546(7) . ? C12B C14B 1.543(6) . ? C12B C15B 1.533(7) . ? C12C C13C 1.543(6) . ? C12C C14C 1.534(6) . ? C12C C15C 1.546(6) . ? C12D C10D 1.534(7) . ? C12D C13D 1.536(9) . ? C12D C14D 1.541(7) . ? C12D C15D 1.528(9) . ? C12F C14F 1.527(8) . ? C12F C15F 1.527(8) . ? C12H C13H 1.546(9) . ? C12H C14H 1.520(8) . ? C12H C15H 1.513(9) . ? C12S C13S 1.391(11) . ? C12S H12S 0.9500 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C13C H13G 0.9800 . ? C13C H13H 0.9800 . ? C13C H13I 0.9800 . ? C13D H13J 0.9800 . ? C13D H13K 0.9800 . ? C13D H13L 0.9800 . ? C13E C12E 1.529(7) . ? C13E H13M 0.9800 . ? C13E H13N 0.9800 . ? C13E H13O 0.9800 . ? C13F C12F 1.529(7) . ? C13F H13R 0.9800 . ? C13F H13S 0.9800 . ? C13F H13T 0.9800 . ? C13G C12G 1.551(6) . ? C13G H13U 0.9800 . ? C13G H13V 0.9800 . ? C13G H13W 0.9800 . ? C13H H13X 0.9800 . ? C13H H13Y 0.9800 . ? C13H H13Z 0.9800 . ? C13S H13 0.9500 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C14C H14G 0.9800 . ? C14C H14H 0.9800 . ? C14C H14I 0.9800 . ? C14D H14J 0.9800 . ? C14D H14K 0.9800 . ? C14D H14L 0.9800 . ? C14E C12E 1.526(7) . ? C14E H14M 0.9800 . ? C14E H14N 0.9800 . ? C14E H14O 0.9800 . ? C14F H14R 0.9800 . ? C14F H14S 0.9800 . ? C14F H14T 0.9800 . ? C14G C12G 1.547(7) . ? C14G H14U 0.9800 . ? C14G H14V 0.9800 . ? C14G H14W 0.9800 . ? C14H H14X 0.9800 . ? C14H H14Y 0.9800 . ? C14H H14Z 0.9800 . ? C14S C13S 1.370(13) . ? C14S C15S 1.414(12) . ? C14S H14 0.9500 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C15C H15G 0.9800 . ? C15C H15H 0.9800 . ? C15C H15I 0.9800 . ? C15D H15J 0.9800 . ? C15D H15K 0.9800 . ? C15D H15L 0.9800 . ? C15E C12E 1.548(7) . ? C15E H15M 0.9800 . ? C15E H15N 0.9800 . ? C15E H15O 0.9800 . ? C15F H15R 0.9800 . ? C15F H15S 0.9800 . ? C15F H15T 0.9800 . ? C15G C12G 1.513(7) . ? C15G H10 0.9800 . ? C15G H15U 0.9800 . ? C15G H15V 0.9800 . ? C15H H15X 0.9800 . ? C15H H15Y 0.9800 . ? C15H H15Z 0.9800 . ? C15S H15 0.9500 . ? C16S C15S 1.360(10) . ? C16S H16S 0.9500 . ? C22S C21S 1.373(9) . ? C22S C23S 1.370(11) . ? C22S H22S 0.9500 . ? C23S C24S 1.392(11) . ? C23S H23S 0.9500 . ? C24S C25S 1.355(10) . ? C24S H24S 0.9500 . ? C25S H25S 0.9500 . ? C26S C21S 1.406(10) . ? C26S C25S 1.386(10) . ? C26S H26S 0.9500 . ? C31S C32S 1.451(15) . ? C31S C36S 1.383(12) . ? C32S H32S 0.9500 . ? C33S C32S 1.471(18) . ? C33S C34S 1.362(14) . ? C33S H33S 0.9500 . ? C34S C35S 1.372(14) . ? C34S H34S 0.9500 . ? C35S C36S 1.370(16) . ? C35S H35S 0.9500 . ? C36S H36S 0.9500 . ? C41S C42S 1.3901 . ? C41S C46S 1.3899 . ? C42S C43S 1.3898 . ? C42S H42S 0.9500 . ? C43S C44S 1.3899 . ? C43S H43S 0.9500 . ? C44S C45S 1.3901 . ? C44S H44S 0.9500 . ? C45S C46S 1.3900 . ? C45S H45S 0.9500 . ? C46S H46S 0.9500 . ? C51S C52S 1.393(10) . ? C51S C56S 1.351(9) . ? C52S H52S 0.9500 . ? C53S C52S 1.361(10) . ? C53S C54S 1.413(11) . ? C53S H53S 0.9500 . ? C54S C55S 1.352(12) . ? C54S H54S 0.9500 . ? C55S H55S 0.9500 . ? C56S C55S 1.376(10) . ? C56S H56S 0.9500 . ? C61S C62S 1.3899 . ? C61S C66S 1.3904 . ? C62S C63S 1.3899 . ? C62S H62S 0.9500 . ? C63S C64S 1.3900 . ? C63S H63S 0.9500 . ? C64S C65S 1.3899 . ? C64S H64S 0.9500 . ? C65S C66S 1.3900 . ? C65S H65S 0.9500 . ? C66S H66S 0.9500 . ? C71S C72S 1.3903 . ? C71S C76S 1.3905 . ? C72S C73S 1.3897 . ? C72S H72S 0.9500 . ? C73S C74S 1.3899 . ? C73S H73S 0.9500 . ? C74S C75S 1.3901 . ? C74S H74S 0.9500 . ? C75S C76S 1.3896 . ? C75S H75S 0.9500 . ? C76S H76S 0.9500 . ? C81S C82S 1.3901 . ? C81S C86S 1.3900 . ? C82S C83S 1.3897 . ? C82S H82S 0.9500 . ? C83S C84S 1.3902 . ? C83S H83S 0.9500 . ? C84S C85S 1.3904 . ? C84S H84S 0.9500 . ? C85S C86S 1.3899 . ? C85S H85S 0.9500 . ? C86S H86S 0.9500 . ? Cl1S C11S 1.752(6) . ? Cl2S C21S 1.720(7) . ? Cl3S C31S 1.716(11) . ? Cl4S C41S 1.6290 . ? Cl5S C51S 1.755(6) . ? Cl6S C61S 1.7090 . ? Cl7S C71S 1.6919 . ? Cl8S C81S 1.6694 . ? N4A C3A 1.497(5) . ? N4A C5A 1.480(5) . ? N4A H4A 0.9300 . ? N4B C3B 1.492(5) . ? N4B C5B 1.494(5) . ? N4B H4B 0.9300 . ? N4C C3C 1.475(6) . ? N4C C5C 1.498(5) . ? N4C H4C 0.9300 . ? N4D C3D 1.494(5) . ? N4D C5D 1.488(6) . ? N4D H4D 0.9300 . ? N4E C3E 1.488(6) . ? N4E C5E 1.475(6) . ? N4E H4E 0.9300 . ? N4F C3F 1.484(6) . ? N4F C5F 1.500(5) . ? N4F H4F 0.9300 . ? N4G C3G 1.476(6) . ? N4G C5G 1.489(6) . ? N4G H4G 0.9300 . ? N4H C3H 1.473(6) . ? N4H C5H 1.494(6) . ? N4H H4H 0.9300 . ? O11A C11A 1.350(5) . ? O11B C11B 1.340(5) . ? O11C C11C 1.353(5) . ? O11D C11D 1.337(5) . ? O11E Al3 1.853(3) . ? O11E C11E 1.356(5) . ? O11F C11F 1.342(5) . ? O11G C11G 1.361(5) . ? O11H C11H 1.332(6) . ? O12A H12A 0.9500 . ? O12B H12B 0.9500 . ? O34E H34E 0.9500 . ? O34F Al3 1.863(3) . ? O34F Al4 1.881(3) . ? O34F H34F 0.9500 . ? 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 Al1 N4A H4A 106.7 . . ? Al1 N4B H4B 107.1 . . ? Al1 O12A Al2 106.21(15) . . ? Al1 O12A H12A 126.9 . . ? Al1 O12B H12B 129.7 . . ? Al2 N4C H4C 106.9 . . ? Al2 N4D H4D 106.1 . . ? Al2 O12A H12A 126.9 . . ? Al2 O12B Al1 100.64(14) . . ? Al2 O12B H12B 129.7 . . ? Al3 N4E H4E 107.0 . . ? Al3 N4F H4F 106.7 . . ? Al3 O34E H34E 129.5 . . ? Al3 O34F Al4 106.37(15) . . ? Al3 O34F H34F 126.8 . . ? Al4 N4G H4G 106.7 . . ? Al4 N4H H4H 106.8 . . ? Al4 O34E Al3 101.02(14) . . ? Al4 O34E H34E 129.5 . . ? Al4 O34F H34F 126.8 . . ? C1A C1B C2B 111.3(4) . . ? C1A C1B H1D 109.4 . . ? C1A C1B H1E 109.4 . . ? C1A C2A H2A 109.7 . . ? C1A C2A H2B 109.7 . . ? C1B C1A C2A 111.3(4) . . ? C1B C1A H1A 109.4 . . ? C1B C1A H1B 109.4 . . ? C1B C2B H2D 109.6 . . ? C1B C2B H2E 109.6 . . ? C1C C1D C2D 110.4(4) . . ? C1C C1D H1J 109.6 . . ? C1C C1D H1K 109.6 . . ? C1C C2C H2G 109.7 . . ? C1C C2C H2H 109.7 . . ? C1D C1C C2C 111.6(4) . . ? C1D C1C H1G 109.3 . . ? C1D C1C H1H 109.3 . . ? C1D C2D C3D 110.4(4) . . ? C1D C2D H2J 109.6 . . ? C1D C2D H2K 109.6 . . ? C1E C1F H1R 109.5 . . ? C1E C1F H1S 109.5 . . ? C1E C2E H2M 109.4 . . ? C1E C2E H2N 109.4 . . ? C1F C1E H1M 109.3 . . ? C1F C1E H1N 109.3 . . ? C1F C2F H2R 109.5 . . ? C1F C2F H2S 109.5 . . ? C1G C1H C2H 110.3(4) . . ? C1G C1H H1X 109.6 . . ? C1G C1H H1Y 109.6 . . ? C1G C2G C3G 110.2(4) . . ? C1G C2G H2U 109.6 . . ? C1G C2G H2V 109.6 . . ? C1H C1G C2G 111.6(5) . . ? C1H C1G H1U 109.3 . . ? C1H C1G H1V 109.3 . . ? C1H C2H H2X 109.5 . . ? C1H C2H H2Y 109.5 . . ? C2A C1A H1A 109.4 . . ? C2A C1A H1B 109.4 . . ? C2A C3A C3B 110.4(4) . . ? C2A C3A H3A 107.7 . . ? C2B C1B H1D 109.4 . . ? C2B C1B H1E 109.4 . . ? C2B C3B C3A 112.1(3) . . ? C2B C3B H3D 107.2 . . ? C2C C1C H1G 109.3 . . ? C2C C1C H1H 109.3 . . ? C2C C3C H3H 108.0 . . ? C2D C1D H1J 109.6 . . ? C2D C1D H1K 109.6 . . ? C2D C3D H3J 107.1 . . ? C2E C1E C1F 111.4(4) . . ? C2E C1E H1M 109.3 . . ? C2E C1E H1N 109.3 . . ? C2E C3E C3F 109.7(4) . . ? C2E C3E H3M 108.9 . . ? C2F C1F C1E 110.8(5) . . ? C2F C1F H1R 109.5 . . ? C2F C1F H1S 109.5 . . ? C2F C3F C3E 112.7(4) . . ? C2F C3F H3R 106.8 . . ? C2G C1G H1U 109.3 . . ? C2G C1G H1V 109.3 . . ? C2G C3G H3G 108.1 . . ? C2H C1H H1X 109.6 . . ? C2H C1H H1Y 109.6 . . ? C2H C3H C3G 111.1(4) . . ? C2H C3H H3X 107.4 . . ? C3A C2A C1A 109.9(4) . . ? C3A C2A H2A 109.7 . . ? C3A C2A H2B 109.7 . . ? C3A C3B H3D 107.2 . . ? C3A N4A Al1 109.9(3) . . ? C3A N4A H4A 106.7 . . ? C3B C2B C1B 110.4(3) . . ? C3B C2B H2D 109.6 . . ? C3B C2B H2E 109.6 . . ? C3B C3A H3A 107.7 . . ? C3B N4B Al1 112.7(3) . . ? C3B N4B C5B 112.4(3) . . ? C3B N4B H4B 107.1 . . ? C3C C2C C1C 109.8(4) . . ? C3C C2C H2G 109.7 . . ? C3C C2C H2H 109.7 . . ? C3C C3D C2D 112.1(4) . . ? C3C C3D H3J 107.1 . . ? C3C N4C Al2 108.7(3) . . ? C3C N4C C5C 114.7(3) . . ? C3C N4C H4C 106.9 . . ? C3D C2D H2J 109.6 . . ? C3D C2D H2K 109.6 . . ? C3D C3C C2C 110.1(4) . . ? C3D C3C H3H 108.0 . . ? C3D N4D Al2 113.2(3) . . ? C3D N4D H4D 106.1 . . ? C3E C2E C1E 111.1(4) . . ? C3E C2E H2M 109.4 . . ? C3E C2E H2N 109.4 . . ? C3E C3F H3R 106.8 . . ? C3E N4E Al3 109.3(3) . . ? C3E N4E H4E 107.0 . . ? C3F C2F C1F 110.9(4) . . ? C3F C2F H2R 109.5 . . ? C3F C2F H2S 109.5 . . ? C3F C3E H3M 108.9 . . ? C3F N4F Al3 112.8(3) . . ? C3F N4F C5F 112.6(3) . . ? C3F N4F H4F 106.7 . . ? C3G C2G H2U 109.6 . . ? C3G C2G H2V 109.6 . . ? C3G C3H H3X 107.4 . . ? C3G N4G Al4 109.6(3) . . ? C3G N4G C5G 114.6(4) . . ? C3G N4G H4G 106.7 . . ? C3H C2H C1H 110.6(4) . . ? C3H C2H H2X 109.5 . . ? C3H C2H H2Y 109.5 . . ? C3H C3G C2G 109.9(4) . . ? C3H C3G H3G 108.1 . . ? C3H N4H Al4 113.9(3) . . ? C3H N4H C5H 111.7(3) . . ? C3H N4H H4H 106.8 . . ? C5A N4A Al1 111.7(3) . . ? C5A N4A C3A 114.7(3) . . ? C5A N4A H4A 106.7 . . ? C5B N4B Al1 110.2(3) . . ? C5B N4B H4B 107.1 . . ? C5C N4C Al2 112.2(2) . . ? C5C N4C H4C 106.9 . . ? C5D N4D Al2 111.8(3) . . ? C5D N4D C3D 112.7(3) . . ? C5D N4D H4D 106.1 . . ? C5E N4E Al3 111.9(3) . . ? C5E N4E C3E 114.2(3) . . ? C5E N4E H4E 107.0 . . ? C5F N4F Al3 110.8(3) . . ? C5F N4F H4F 106.7 . . ? C5G N4G Al4 112.2(3) . . ? C5G N4G H4G 106.7 . . ? C5H N4H Al4 110.4(3) . . ? C5H N4H H4H 106.8 . . ? C6A C5A H5A 109.6 . . ? C6A C5A H5B 109.6 . . ? C6A C7A C8A 120.0(4) . . ? C6A C7A H7A 120.0 . . ? C6A C11A C10A 119.2(4) . . ? C6B C5B H5D 109.5 . . ? C6B C5B H5E 109.5 . . ? C6B C7B H7D 119.6 . . ? C6B C11B C10B 118.2(4) . . ? C6C C5C H5G 109.8 . . ? C6C C5C H5H 109.0 . . ? C6C C5C N4C 111.1(3) . . ? C6C C7C H7C 120.0 . . ? C6C C11C C10C 120.1(4) . . ? C6D C5D H5J 109.2 . . ? C6D C5D H5K 109.2 . . ? C6D C7D H7J 119.6 . . ? C6D C11D C10D 119.0(4) . . ? C6E C5E H5M 109.5 . . ? C6E C5E H5N 109.5 . . ? C6E C7E H7M 119.6 . . ? C6E C11E C10E 118.8(4) . . ? C6F C5F H5R 109.5 . . ? C6F C5F H5S 109.5 . . ? C6F C7F H7R 119.9 . . ? C6F C11F C10F 118.6(4) . . ? C6G C5G H5U 109.5 . . ? C6G C5G H5V 109.5 . . ? C6G C7G H7U 119.7 . . ? C6H C5H H5X 109.1 . . ? C6H C5H H5Y 109.1 . . ? C6H C7H C8H 119.7(6) . . ? C6H C7H H7X 120.2 . . ? C6H C11H C10H 118.5(4) . . ? C7A C6A C5A 120.2(4) . . ? C7A C6A C11A 121.3(4) . . ? C7A C8A H8A 120.3 . . ? C7B C6B C5B 119.1(4) . . ? C7B C6B C11B 121.2(4) . . ? C7B C8B C9B 119.1(4) . . ? C7B C8B H8D 120.4 . . ? C7C C6C C5C 120.2(4) . . ? C7C C8C C9C 119.3(4) . . ? C7C C8C H8C 120.4 . . ? C7D C6D C5D 118.0(4) . . ? C7D C8D H8J 121.1 . . ? C7E C6E C5E 120.6(4) . . ? C7E C6E C11E 120.5(4) . . ? C7E C8E C9E 120.2(5) . . ? C7E C8E H8M 119.9 . . ? C7F C6F C5F 118.5(4) . . ? C7F C8F H8R 120.6 . . ? C7G C6G C5G 120.6(4) . . ? C7G C6G C11G 120.1(5) . . ? C7G C8G C9G 118.9(5) . . ? C7G C8G H8U 120.6 . . ? C7H C6H C5H 119.0(5) . . ? C7H C6H C11H 121.1(5) . . ? C7H C8H H8X 119.9 . . ? C8A C7A H7A 120.0 . . ? C8A C9A C10A 122.7(4) . . ? C8A C9A H9A 118.7 . . ? C8B C7B C6B 120.7(4) . . ? C8B C7B H7D 119.6 . . ? C8B C9B C10B 122.5(4) . . ? C8B C9B H9B 118.7 . . ? C8C C7C C6C 119.9(5) . . ? C8C C7C H7C 120.0 . . ? C8C C9C C10C 123.7(4) . . ? C8C C9C H9G 118.1 . . ? C8D C7D C6D 120.9(5) . . ? C8D C7D H7J 119.6 . . ? C8D C9D C10D 124.2(5) . . ? C8D C9D H9J 117.9 . . ? C8E C7E C6E 120.8(5) . . ? C8E C7E H7M 119.6 . . ? C8E C9E H9M 118.9 . . ? C8F C7F C6F 120.2(5) . . ? C8F C7F H7R 119.9 . . ? C8F C9F C10F 123.1(5) . . ? C8F C9F H9R 118.5 . . ? C8G C7G C6G 120.6(5) . . ? C8G C7G H7U 119.7 . . ? C8G C9G C10G 123.5(5) . . ? C8G C9G H9U 118.2 . . ? C8H C7H H7X 120.2 . . ? C8H C9H C10H 122.0(5) . . ? C8H C9H H9X 119.0 . . ? C9A C8A C7A 119.4(4) . . ? C9A C8A H8A 120.3 . . ? C9A C10A C11A 117.3(4) . . ? C9A C10A C12A 119.1(4) . . ? C9B C8B H8D 120.4 . . ? C9B C10B C11B 118.1(4) . . ? C9B C10B C12B 119.7(4) . . ? C9C C8C H8C 120.4 . . ? C9C C10C C11C 116.2(4) . . ? C9C C10C C12C 120.1(4) . . ? C9D C8D C7D 117.8(4) . . ? C9D C8D H8J 121.1 . . ? C9D C10D C11D 117.5(4) . . ? C9D C10D C12D 121.0(4) . . ? C9E C8E H8M 119.9 . . ? C9E C10E C11E 117.1(4) . . ? C9E C10E C12E 119.8(4) . . ? C9F C8F C7F 118.9(5) . . ? C9F C8F H8R 120.6 . . ? C9F C10F C11F 117.3(4) . . ? C9F C10F C12F 120.3(4) . . ? C9G C8G H8U 120.6 . . ? C9G C10G C11G 116.9(4) . . ? C9G C10G C12G 120.3(4) . . ? C9H C8H C7H 120.2(5) . . ? C9H C8H H8X 119.9 . . ? C9H C10H C11H 118.4(5) . . ? C9H C10H C12H 119.5(5) . . ? C10A C9A H9A 118.7 . . ? C10A C12A C13A 113.4(4) . . ? C10A C12A C15A 106.9(4) . . ? C10B C9B H9B 118.7 . . ? C10B C12B C13B 108.0(4) . . ? C10B C12B C14B 112.8(4) . . ? C10C C9C H9G 118.1 . . ? C10C C12C C13C 113.6(4) . . ? C10C C12C C14C 113.0(4) . . ? C10C C12C C15C 107.5(4) . . ? C10D C9D H9J 117.9 . . ? C10D C12D C13D 109.6(4) . . ? C10D C12D C14D 112.4(4) . . ? C10E C9E C8E 122.2(5) . . ? C10E C9E H9M 118.9 . . ? C10E C12E C15E 112.6(4) . . ? C10F C9F H9R 118.5 . . ? C10G C9G H9U 118.2 . . ? C10G C11G C6G 119.8(4) . . ? C10G C12G C13G 112.9(4) . . ? C10G C12G C14G 113.4(4) . . ? C10H C9H H9X 119.0 . . ? C10H C12H C13H 110.5(5) . . ? C10H C12H C14H 113.8(5) . . ? C11A C6A C5A 118.4(4) . . ? C11A C10A C12A 123.4(4) . . ? C11A O11A Al1 126.6(3) . . ? C11B C6B C5B 119.7(4) . . ? C11B C10B C12B 122.1(4) . . ? C11B O11B Al1 132.7(3) . . ? C11C C6C C5C 119.4(4) . . ? C11C C6C C7C 120.4(4) . . ? C11C C10C C12C 123.4(4) . . ? C11C O11C Al2 126.9(3) . . ? C11D C6D C5D 121.5(4) . . ? C11D C6D C7D 120.5(4) . . ? C11D C10D C12D 121.5(4) . . ? C11D O11D Al2 133.5(3) . . ? C11E C6E C5E 118.9(4) . . ? C11E C10E C12E 122.8(4) . . ? C11E O11E Al3 126.1(3) . . ? C11F C6F C5F 119.9(4) . . ? C11F C6F C7F 121.6(4) . . ? C11F C10F C12F 122.4(4) . . ? C11F O11F Al3 133.8(3) . . ? C11G C6G C5G 119.4(4) . . ? C11G C10G C12G 122.3(4) . . ? C11G O11G Al4 126.6(3) . . ? C11H C6H C5H 119.9(4) . . ? C11H C10H C12H 122.2(4) . . ? C11H O11H Al4 134.1(3) . . ? C11S C12S C13S 118.5(7) . . ? C11S C12S H12S 120.8 . . ? C11S C16S H16S 120.4 . . ? C12A C13A H13A 109.5 . . ? C12A C13A H13B 109.5 . . ? C12A C13A H13C 109.5 . . ? C12A C14A H14A 109.5 . . ? C12A C14A H14B 109.5 . . ? C12A C14A H14C 109.5 . . ? C12A C15A H15A 109.5 . . ? C12A C15A H15B 109.5 . . ? C12A C15A H15C 109.5 . . ? C12B C13B H13D 109.5 . . ? C12B C13B H13E 109.5 . . ? C12B C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? C12B C15B H15D 109.5 . . ? C12B C15B H15E 109.5 . . ? C12B C15B H15F 109.5 . . ? C12C C13C H13G 109.5 . . ? C12C C13C H13H 109.5 . . ? C12C C13C H13I 109.5 . . ? C12C C14C H14G 109.5 . . ? C12C C14C H14H 109.5 . . ? C12C C14C H14I 109.5 . . ? C12C C15C H15G 109.5 . . ? C12C C15C H15H 109.5 . . ? C12C C15C H15I 109.5 . . ? C12D C13D H13J 109.5 . . ? C12D C13D H13K 109.5 . . ? C12D C13D H13L 109.5 . . ? C12D C14D H14J 109.5 . . ? C12D C14D H14K 109.5 . . ? C12D C14D H14L 109.5 . . ? C12D C15D H15J 109.5 . . ? C12D C15D H15K 109.5 . . ? C12D C15D H15L 109.5 . . ? C12E C13E H13M 109.5 . . ? C12E C13E H13N 109.5 . . ? C12E C13E H13O 109.5 . . ? C12E C14E H14M 109.5 . . ? C12E C14E H14N 109.5 . . ? C12E C14E H14O 109.5 . . ? C12E C15E H15M 109.5 . . ? C12E C15E H15N 109.5 . . ? C12E C15E H15O 109.5 . . ? C12F C13F H13R 109.5 . . ? C12F C13F H13S 109.5 . . ? C12F C13F H13T 109.5 . . ? C12F C14F H14R 109.5 . . ? C12F C14F H14S 109.5 . . ? C12F C14F H14T 109.5 . . ? C12F C15F H15R 109.5 . . ? C12F C15F H15S 109.5 . . ? C12F C15F H15T 109.5 . . ? C12G C13G H13U 109.5 . . ? C12G C13G H13V 109.5 . . ? C12G C13G H13W 109.5 . . ? C12G C14G H14U 109.5 . . ? C12G C14G H14V 109.5 . . ? C12G C14G H14W 109.5 . . ? C12G C15G H10 109.5 . . ? C12G C15G H15U 109.5 . . ? C12G C15G H15V 109.5 . . ? C12H C13H H13X 109.5 . . ? C12H C13H H13Y 109.5 . . ? C12H C13H H13Z 109.5 . . ? C12H C14H H14X 109.5 . . ? C12H C14H H14Y 109.5 . . ? C12H C14H H14Z 109.5 . . ? C12H C15H H15X 109.5 . . ? C12H C15H H15Y 109.5 . . ? C12H C15H H15Z 109.5 . . ? C12S C11S Cl1S 118.6(5) . . ? C12S C13S H13 120.4 . . ? C13A C12A C15A 108.5(4) . . ? C13C C12C C15C 106.5(4) . . ? C13D C12D C14D 106.2(5) . . ? C13E C12E C10E 112.3(4) . . ? C13E C12E C15E 106.4(4) . . ? C13F C12F C10F 112.7(4) . . ? C13S C12S H12S 120.8 . . ? C13S C14S C15S 120.7(7) . . ? C13S C14S H14 119.6 . . ? C14A C12A C10A 113.5(4) . . ? C14A C12A C13A 106.6(4) . . ? C14A C12A C15A 107.7(4) . . ? C14B C12B C13B 107.4(4) . . ? C14C C12C C13C 106.8(4) . . ? C14C C12C C15C 109.2(4) . . ? C14E C12E C10E 108.2(4) . . ? C14E C12E C13E 107.6(4) . . ? C14E C12E C15E 109.5(4) . . ? C14F C12F C10F 109.1(4) . . ? C14F C12F C13F 105.7(4) . . ? C14F C12F C15F 110.6(5) . . ? C14G C12G C13G 105.6(4) . . ? C14H C12H C13H 106.3(5) . . ? C14S C13S C12S 119.2(7) . . ? C14S C13S H13 120.4 . . ? C14S C15S H15 120.3 . . ? C15B C12B C10B 111.6(4) . . ? C15B C12B C13B 111.0(4) . . ? C15B C12B C14B 106.0(4) . . ? C15D C12D C10D 110.8(5) . . ? C15D C12D C13D 110.2(5) . . ? C15D C12D C14D 107.5(5) . . ? C15F C12F C10F 109.9(4) . . ? C15F C12F C13F 108.7(5) . . ? C15G C12G C10G 107.1(4) . . ? C15G C12G C13G 109.7(4) . . ? C15G C12G C14G 108.1(4) . . ? C15H C12H C10H 110.4(5) . . ? C15H C12H C13H 109.3(5) . . ? C15H C12H C14H 106.3(5) . . ? C15S C14S H14 119.6 . . ? C15S C16S C11S 119.1(6) . . ? C15S C16S H16S 120.4 . . ? C16S C11S C12S 122.9(6) . . ? C16S C11S Cl1S 118.5(5) . . ? C16S C15S C14S 119.4(7) . . ? C16S C15S H15 120.3 . . ? C21S C22S H22S 119.6 . . ? C21S C26S H26S 120.1 . . ? C22S C21S C26S 119.2(7) . . ? C22S C21S Cl2S 120.4(6) . . ? C22S C23S C24S 119.5(6) . . ? C22S C23S H23S 120.2 . . ? C23S C22S C21S 120.7(7) . . ? C23S C22S H22S 119.6 . . ? C23S C24S H24S 119.5 . . ? C24S C23S H23S 120.2 . . ? C24S C25S C26S 119.8(7) . . ? C24S C25S H25S 120.1 . . ? C25S C24S C23S 120.9(7) . . ? C25S C24S H24S 119.5 . . ? C25S C26S C21S 119.8(6) . . ? C25S C26S H26S 120.1 . . ? C26S C21S Cl2S 120.3(5) . . ? C26S C25S H25S 120.1 . . ? C31S C32S C33S 119.1(8) . . ? C31S C32S H32S 120.4 . . ? C31S C36S H36S 119.8 . . ? C32S C31S Cl3S 120.1(8) . . ? C32S C33S H33S 121.2 . . ? C33S C32S H32S 120.4 . . ? C33S C34S C35S 121.5(12) . . ? C33S C34S H34S 119.2 . . ? C34S C33S C32S 117.6(10) . . ? C34S C33S H33S 121.2 . . ? C34S C35S C36S 122.5(10) . . ? C34S C35S H35S 118.8 . . ? C35S C34S H34S 119.2 . . ? C35S C36S C31S 120.4(9) . . ? C35S C36S H36S 119.8 . . ? C36S C31S C32S 118.4(10) . . ? C36S C31S Cl3S 121.4(8) . . ? C36S C35S H35S 118.8 . . ? C41S C42S H42S 120.0 . . ? C41S C46S C45S 120.008(1) . . ? C41S C46S H46S 120.0 . . ? C42S C41S Cl4S 119.447(2) . . ? C42S C43S C44S 120.014(1) . . ? C42S C43S H43S 120.0 . . ? C43S C42S C41S 119.999(3) . . ? C43S C42S H42S 120.0 . . ? C43S C44S C45S 119.992(1) . . ? C43S C44S H44S 120.0 . . ? C44S C43S H43S 120.0 . . ? C44S C45S H45S 120.0 . . ? C45S C44S H44S 120.0 . . ? C45S C46S H46S 120.0 . . ? C46S C41S C42S 119.991(2) . . ? C46S C41S Cl4S 120.215(1) . . ? C46S C45S C44S 119.996(1) . . ? C46S C45S H45S 120.0 . . ? C51S C52S H52S 120.8 . . ? C51S C56S C55S 120.2(7) . . ? C51S C56S H56S 119.9 . . ? C52S C51S Cl5S 119.7(4) . . ? C52S C53S C54S 119.4(7) . . ? C52S C53S H53S 120.3 . . ? C53S C52S C51S 118.5(6) . . ? C53S C52S H52S 120.8 . . ? C53S C54S H54S 119.6 . . ? C54S C53S H53S 120.3 . . ? C54S C55S C56S 119.3(7) . . ? C54S C55S H55S 120.3 . . ? C55S C54S C53S 120.9(7) . . ? C55S C54S H54S 119.6 . . ? C55S C56S H56S 119.9 . . ? C56S C51S C52S 121.6(6) . . ? C56S C51S Cl5S 118.7(6) . . ? C56S C55S H55S 120.3 . . ? C61S C62S C63S 120.0 . . ? C61S C62S H62S 120.0 . . ? C61S C66S H66S 120.0 . . ? C62S C61S C66S 119.993(1) . . ? C62S C61S Cl6S 112.9 . . ? C62S C63S C64S 120.0 . . ? C62S C63S H63S 120.0 . . ? C63S C62S H62S 120.0 . . ? C63S C64S H64S 120.0 . . ? C64S C63S H63S 120.0 . . ? C64S C65S C66S 120.0 . . ? C64S C65S H65S 120.0 . . ? C65S C64S C63S 119.995(1) . . ? C65S C64S H64S 120.0 . . ? C65S C66S C61S 120.0 . . ? C65S C66S H66S 120.0 . . ? C66S C61S Cl6S 127.1 . . ? C66S C65S H65S 120.0 . . ? C71S C72S H72S 120.0 . . ? C71S C76S H76S 120.0 . . ? C72S C71S C76S 119.988(1) . . ? C72S C71S Cl7S 124.189(1) . . ? C72S C73S C74S 120.0 . . ? C72S C73S H73S 120.0 . . ? C73S C72S C71S 120.004(1) . . ? C73S C72S H72S 120.0 . . ? C73S C74S C75S 120.009(1) . . ? C73S C74S H74S 120.0 . . ? C74S C73S H73S 120.0 . . ? C74S C75S H75S 120.0 . . ? C75S C74S H74S 120.0 . . ? C75S C76S C71S 119.989(1) . . ? C75S C76S H76S 120.0 . . ? C76S C71S Cl7S 115.8 . . ? C76S C75S C74S 120.010(1) . . ? C76S C75S H75S 120.0 . . ? C81S C82S H82S 120.0 . . ? C81S C86S H86S 120.0 . . ? C82S C81S Cl8S 120.343(1) . . ? C82S C83S C84S 120.010(1) . . ? C82S C83S H83S 120.0 . . ? C83S C82S C81S 120.000(1) . . ? C83S C82S H82S 120.0 . . ? C83S C84S C85S 119.996(1) . . ? C83S C84S H84S 120.0 . . ? C84S C83S H83S 120.0 . . ? C84S C85S H85S 120.0 . . ? C85S C84S H84S 120.0 . . ? C85S C86S C81S 120.0 . . ? C85S C86S H86S 120.0 . . ? C86S C81S C82S 120.0 . . ? C86S C81S Cl8S 119.606(1) . . ? C86S C85S C84S 120.0 . . ? C86S C85S H85S 120.0 . . ? H1A C1A H1B 108.0 . . ? H1D C1B H1E 108.0 . . ? H1G C1C H1H 108.0 . . ? H1J C1D H1K 108.1 . . ? H1M C1E H1N 108.0 . . ? H1R C1F H1S 108.1 . . ? H1U C1G H1V 108.0 . . ? H1X C1H H1Y 108.1 . . ? H2A C2A H2B 108.2 . . ? H2D C2B H2E 108.1 . . ? H2G C2C H2H 108.2 . . ? H2J C2D H2K 108.1 . . ? H2M C2E H2N 108.0 . . ? H2R C2F H2S 108.0 . . ? H2U C2G H2V 108.1 . . ? H2X C2H H2Y 108.1 . . ? H5A C5A H5B 108.1 . . ? H5D C5B H5E 108.1 . . ? H5G C5C H5H 108.0 . . ? H5J C5D H5K 107.9 . . ? H5M C5E H5N 108.1 . . ? H5R C5F H5S 108.1 . . ? H5U C5G H5V 108.1 . . ? H5X C5H H5Y 107.8 . . ? H13A C13A H13B 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? H13D C13B H13E 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? H13G C13C H13H 109.5 . . ? H13G C13C H13I 109.5 . . ? H13H C13C H13I 109.5 . . ? H13J C13D H13K 109.5 . . ? H13J C13D H13L 109.5 . . ? H13K C13D H13L 109.5 . . ? H13M C13E H13N 109.5 . . ? H13M C13E H13O 109.5 . . ? H13N C13E H13O 109.5 . . ? H13R C13F H13S 109.5 . . ? H13R C13F H13T 109.5 . . ? H13S C13F H13T 109.5 . . ? H13U C13G H13V 109.5 . . ? H13U C13G H13W 109.5 . . ? H13V C13G H13W 109.5 . . ? H13X C13H H13Y 109.5 . . ? H13X C13H H13Z 109.5 . . ? H13Y C13H H13Z 109.5 . . ? H14A C14A H14B 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? H14D C14B H14E 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? H14G C14C H14H 109.5 . . ? H14G C14C H14I 109.5 . . ? H14H C14C H14I 109.5 . . ? H14J C14D H14K 109.5 . . ? H14J C14D H14L 109.5 . . ? H14K C14D H14L 109.5 . . ? H14M C14E H14N 109.5 . . ? H14M C14E H14O 109.5 . . ? H14N C14E H14O 109.5 . . ? H14R C14F H14S 109.5 . . ? H14R C14F H14T 109.5 . . ? H14S C14F H14T 109.5 . . ? H14U C14G H14V 109.5 . . ? H14U C14G H14W 109.5 . . ? H14V C14G H14W 109.5 . . ? H14X C14H H14Y 109.5 . . ? H14X C14H H14Z 109.5 . . ? H14Y C14H H14Z 109.5 . . ? H15A C15A H15B 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? H15D C15B H15E 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? H15G C15C H15H 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? H15J C15D H15K 109.5 . . ? H15J C15D H15L 109.5 . . ? H15K C15D H15L 109.5 . . ? H15M C15E H15N 109.5 . . ? H15M C15E H15O 109.5 . . ? H15N C15E H15O 109.5 . . ? H15R C15F H15S 109.5 . . ? H15R C15F H15T 109.5 . . ? H15S C15F H15T 109.5 . . ? H15U C15G H10 109.5 . . ? H15U C15G H15V 109.5 . . ? H15V C15G H10 109.5 . . ? H15X C15H H15Y 109.5 . . ? H15X C15H H15Z 109.5 . . ? H15Y C15H H15Z 109.5 . . ? N4A Al1 Al2 128.52(11) . . ? N4A Al1 N4B 81.14(14) . . ? N4A C3A C2A 116.1(4) . . ? N4A C3A C3B 106.9(3) . . ? N4A C3A H3A 107.7 . . ? N4A C5A C6A 110.3(3) . . ? N4A C5A H5A 109.6 . . ? N4A C5A H5B 109.6 . . ? N4B Al1 Al2 87.90(11) . . ? N4B C3B C2B 114.7(3) . . ? N4B C3B C3A 108.1(3) . . ? N4B C3B H3D 107.2 . . ? N4B C5B C6B 110.7(4) . . ? N4B C5B H5D 109.5 . . ? N4B C5B H5E 109.5 . . ? N4C Al2 Al1 129.82(11) . . ? N4C C3C C2C 115.7(4) . . ? N4C C3C C3D 106.8(4) . . ? N4C C3C H3H 108.0 . . ? N4C C5C H5G 109.6 . . ? N4C C5C H5H 109.2 . . ? N4D Al2 Al1 86.25(11) . . ? N4D Al2 N4C 79.39(15) . . ? N4D C3D C2D 114.6(4) . . ? N4D C3D C3C 108.4(4) . . ? N4D C3D H3J 107.1 . . ? N4D C5D C6D 112.0(4) . . ? N4D C5D H5J 109.2 . . ? N4D C5D H5K 109.2 . . ? N4E Al3 Al4 128.49(11) . . ? N4E Al3 N4F 79.80(15) . . ? N4E C3E C2E 114.9(4) . . ? N4E C3E C3F 105.4(3) . . ? N4E C3E H3M 108.9 . . ? N4E C5E C6E 110.8(4) . . ? N4E C5E H5M 109.5 . . ? N4E C5E H5N 109.5 . . ? N4F Al3 Al4 87.81(11) . . ? N4F C3F C2F 115.3(4) . . ? N4F C3F C3E 108.0(4) . . ? N4F C3F H3R 106.8 . . ? N4F C5F C6F 110.8(4) . . ? N4F C5F H5R 109.5 . . ? N4F C5F H5S 109.5 . . ? N4G Al4 Al3 130.79(12) . . ? N4G C3G C2G 116.2(4) . . ? N4G C3G C3H 106.0(4) . . ? N4G C3G H3G 108.1 . . ? N4G C5G C6G 110.8(4) . . ? N4G C5G H5U 109.5 . . ? N4G C5G H5V 109.5 . . ? N4H Al4 Al3 87.06(11) . . ? N4H Al4 N4G 79.52(15) . . ? N4H C3H C2H 115.3(4) . . ? N4H C3H C3G 107.8(3) . . ? N4H C3H H3X 107.4 . . ? N4H C5H C6H 112.7(4) . . ? N4H C5H H5X 109.1 . . ? N4H C5H H5Y 109.1 . . ? O11A Al1 Al2 93.30(10) . . ? O11A Al1 N4A 91.31(14) . . ? O11A Al1 N4B 171.16(15) . . ? O11A Al1 O12A 96.75(14) . . ? O11A Al1 O12B 88.56(14) . . ? O11A C11A C6A 118.8(4) . . ? O11A C11A C10A 122.0(4) . . ? O11B Al1 Al2 137.40(11) . . ? O11B Al1 N4A 92.86(14) . . ? O11B Al1 N4B 89.41(14) . . ? O11B Al1 O11A 95.59(14) . . ? O11B Al1 O12A 100.54(14) . . ? O11B Al1 O12B 175.07(15) . . ? O11B C11B C6B 120.0(4) . . ? O11B C11B C10B 121.8(4) . . ? O11C Al2 Al1 95.48(10) . . ? O11C Al2 N4C 91.01(15) . . ? O11C Al2 N4D 168.67(15) . . ? O11C Al2 O12A 99.14(14) . . ? O11C Al2 O12B 88.79(14) . . ? O11C C11C C6C 117.8(4) . . ? O11C C11C C10C 122.0(4) . . ? O11D Al2 Al1 135.06(11) . . ? O11D Al2 N4C 93.18(15) . . ? O11D Al2 N4D 90.43(15) . . ? O11D Al2 O11C 96.15(14) . . ? O11D Al2 O12A 98.39(14) . . ? O11D Al2 O12B 173.68(15) . . ? O11D C11D C6D 120.1(4) . . ? O11D C11D C10D 121.0(4) . . ? O11E Al3 Al4 94.21(11) . . ? O11E Al3 N4E 91.60(14) . . ? O11E Al3 N4F 170.32(15) . . ? O11E Al3 O34E 88.78(13) . . ? O11E Al3 O34F 97.58(14) . . ? O11E C11E C6E 118.8(4) . . ? O11E C11E C10E 122.2(4) . . ? O11F Al3 Al4 135.82(12) . . ? O11F Al3 N4E 94.24(15) . . ? O11F Al3 N4F 89.76(14) . . ? O11F Al3 O11E 95.33(14) . . ? O11F Al3 O34E 174.14(15) . . ? O11F Al3 O34F 98.90(14) . . ? O11F C11F C6F 120.5(4) . . ? O11F C11F C10F 120.9(4) . . ? O11G Al4 Al3 94.73(11) . . ? O11G Al4 N4G 91.22(15) . . ? O11G Al4 N4H 169.04(15) . . ? O11G Al4 O34E 89.13(14) . . ? O11G Al4 O34F 98.07(14) . . ? O11G C11G C6G 117.1(4) . . ? O11G C11G C10G 123.0(4) . . ? O11H Al4 Al3 135.59(12) . . ? O11H Al4 N4G 91.97(15) . . ? O11H Al4 N4H 90.39(15) . . ? O11H Al4 O11G 95.81(15) . . ? O11H Al4 O34E 173.68(16) . . ? O11H Al4 O34F 99.11(15) . . ? O11H C11H C6H 120.2(4) . . ? O11H C11H C10H 121.2(5) . . ? O12A Al1 Al2 36.96(9) . . ? O12A Al1 N4A 163.57(15) . . ? O12A Al1 N4B 89.47(14) . . ? O12A Al1 O12B 76.27(13) . . ? O12A Al2 Al1 36.83(9) . . ? O12A Al2 N4C 163.66(15) . . ? O12A Al2 N4D 88.97(14) . . ? O12A Al2 O12B 76.88(13) . . ? O12B Al1 Al2 39.32(9) . . ? O12B Al1 N4A 89.70(14) . . ? O12B Al1 N4B 86.83(14) . . ? O12B Al2 Al1 40.05(9) . . ? O12B Al2 N4C 90.66(14) . . ? O12B Al2 N4D 85.34(14) . . ? O34E Al3 Al4 39.36(9) . . ? O34E Al3 N4E 89.80(14) . . ? O34E Al3 N4F 86.79(14) . . ? O34E Al4 Al3 39.62(9) . . ? O34E Al4 N4G 91.86(14) . . ? O34E Al4 N4H 85.36(14) . . ? O34F Al3 Al4 37.01(9) . . ? O34F Al3 N4E 163.16(15) . . ? O34F Al3 N4F 89.73(15) . . ? O34F Al3 O34E 76.37(13) . . ? O34F Al4 Al3 36.61(9) . . ? O34F Al4 N4G 164.70(15) . . ? O34F Al4 N4H 89.82(14) . . ? O34F Al4 O34E 76.23(13) . . ? 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 Al1 Al2 N4C C3C 47.2(3) . . . . ? Al1 Al2 N4C C5C -80.7(3) . . . . ? Al1 Al2 N4D C3D -130.1(3) . . . . ? Al1 Al2 N4D C5D 101.3(3) . . . . ? Al1 Al2 O11C C11C 166.1(3) . . . . ? Al1 Al2 O11D C11D -93.5(4) . . . . ? Al1 N4A C3A C2A 169.1(3) . . . . ? Al1 N4A C3A C3B 45.5(4) . . . . ? Al1 N4A C5A C6A -64.1(4) . . . . ? Al1 N4B C3B C2B 155.8(3) . . . . ? Al1 N4B C3B C3A 29.9(4) . . . . ? Al1 N4B C5B C6B 68.6(4) . . . . ? Al1 O11A C11A C6A -45.9(5) . . . . ? Al1 O11A C11A C10A 135.6(4) . . . . ? Al1 O11B C11B C6B 31.3(6) . . . . ? Al1 O11B C11B C10B -148.8(3) . . . . ? Al2 Al1 N4A C3A 56.8(3) . . . . ? Al2 Al1 N4A C5A -71.8(3) . . . . ? Al2 Al1 N4B C3B -133.8(3) . . . . ? Al2 Al1 N4B C5B 99.8(3) . . . . ? Al2 Al1 O11A C11A 159.4(3) . . . . ? Al2 Al1 O11B C11B -96.3(4) . . . . ? Al2 N4C C3C C2C 173.4(3) . . . . ? Al2 N4C C3C C3D 50.5(4) . . . . ? Al2 N4C C5C C6C -59.2(4) . . . . ? Al2 N4D C3D C2D 151.2(3) . . . . ? Al2 N4D C3D C3C 25.2(4) . . . . ? Al2 N4D C5D C6D 63.0(4) . . . . ? Al2 O11C C11C C6C -46.9(5) . . . . ? Al2 O11C C11C C10C 136.7(4) . . . . ? Al2 O11D C11D C6D 24.3(6) . . . . ? Al2 O11D C11D C10D -156.5(3) . . . . ? Al3 Al4 N4G C3G 49.9(3) . . . . ? Al3 Al4 N4G C5G -78.6(3) . . . . ? Al3 Al4 N4H C3H -134.0(3) . . . . ? Al3 Al4 N4H C5H 99.4(3) . . . . ? Al3 Al4 O11G C11G 167.0(3) . . . . ? Al3 Al4 O11H C11H -92.3(4) . . . . ? Al3 N4E C3E C2E 171.0(3) . . . . ? Al3 N4E C3E C3F 50.1(4) . . . . ? Al3 N4E C5E C6E -61.8(4) . . . . ? Al3 N4F C3F C2F 156.4(3) . . . . ? Al3 N4F C3F C3E 29.4(4) . . . . ? Al3 N4F C5F C6F 66.1(4) . . . . ? Al3 O11E C11E C6E -45.1(5) . . . . ? Al3 O11E C11E C10E 138.7(4) . . . . ? Al3 O11F C11F C6F 24.5(6) . . . . ? Al3 O11F C11F C10F -155.7(3) . . . . ? Al3 O34F Al4 N4G 39.8(6) . . . . ? Al3 O34F Al4 N4H 85.31(17) . . . . ? Al3 O34F Al4 O11G -87.06(17) . . . . ? Al3 O34F Al4 O11H 175.68(16) . . . . ? Al3 O34F Al4 O34E 0.04(15) . . . . ? Al4 Al3 N4E C3E 51.5(3) . . . . ? Al4 Al3 N4E C5E -76.0(3) . . . . ? Al4 Al3 N4F C3F -131.6(3) . . . . ? Al4 Al3 N4F C5F 101.2(3) . . . . ? Al4 Al3 O11F C11F -95.7(4) . . . . ? Al4 N4G C3G C2G 171.3(4) . . . . ? Al4 N4G C3G C3H 48.9(4) . . . . ? Al4 N4G C5G C6G -60.5(4) . . . . ? Al4 N4H C3H C2H 152.8(3) . . . . ? Al4 N4H C3H C3G 28.1(4) . . . . ? Al4 N4H C5H C6H 65.4(4) . . . . ? Al4 O11G C11G C6G -48.2(5) . . . . ? Al4 O11G C11G C10G 134.0(4) . . . . ? Al4 O11H C11H C6H 23.9(7) . . . . ? Al4 O11H C11H C10H -157.8(4) . . . . ? Al4 O34F Al3 N4E 35.5(6) . . . . ? Al4 O34F Al3 N4F 86.72(16) . . . . ? Al4 O34F Al3 O11E -86.93(16) . . . . ? Al4 O34F Al3 O11F 176.43(15) . . . . ? Al4 O34F Al3 O34E -0.04(15) . . . . ? C1B C1A C2A C3A 57.2(6) . . . . ? C1C C1D C2D C3D 55.7(6) . . . . ? C1E C2E C3E C3F -55.8(5) . . . . ? C1E C2E C3E N4E -174.3(4) . . . . ? C1G C2G C3G C3H -56.3(6) . . . . ? C1G C2G C3G N4G -176.7(5) . . . . ? C1H C2H C3H C3G -57.3(5) . . . . ? C1H C2H C3H N4H 179.7(4) . . . . ? C2A C1A C1B C2B -56.5(6) . . . . ? C2B C3B C3A C2A 56.9(5) . . . . ? C2B C3B C3A N4A -176.0(3) . . . . ? C2C C3C C3D C2D 57.3(5) . . . . ? C2C C3C C3D N4D -175.2(4) . . . . ? C2D C1D C1C C2C -57.0(6) . . . . ? C2F C1F C1E C2E -55.6(6) . . . . ? C2F C3F C3E C2E 56.1(5) . . . . ? C2F C3F C3E N4E -179.7(4) . . . . ? C2G C1G C1H C2H -57.5(6) . . . . ? C2G C3G C3H C2H 56.9(5) . . . . ? C2G C3G C3H N4H -175.9(4) . . . . ? C3A C3B C2B C1B -55.4(5) . . . . ? C3A N4A C5A C6A 170.0(3) . . . . ? C3B C2B C1B C1A 55.1(5) . . . . ? C3B C3A C2A C1A -56.5(5) . . . . ? C3B N4B C5B C6B -58.0(4) . . . . ? C3C C2C C1C C1D 57.2(6) . . . . ? C3C C3D C2D C1D -56.9(5) . . . . ? C3C N4C C5C C6C 176.2(3) . . . . ? C3D C3C C2C C1C -56.6(5) . . . . ? C3D N4D C5D C6D -65.9(5) . . . . ? C3E C2E C1E C1F 56.6(6) . . . . ? C3E C3F C2F C1F -55.9(6) . . . . ? C3E N4E C5E C6E 173.3(4) . . . . ? C3F C2F C1F C1E 54.6(6) . . . . ? C3F N4F C5F C6F -61.3(5) . . . . ? C3G C2G C1G C1H 57.4(6) . . . . ? C3G N4G C5G C6G 173.7(4) . . . . ? C3H C2H C1H C1G 57.0(6) . . . . ? C3H N4H C5H C6H -62.4(5) . . . . ? C5A C6A C7A C8A -178.2(4) . . . . ? C5A C6A C11A C10A 176.8(4) . . . . ? C5A C6A C11A O11A -1.7(6) . . . . ? C5A N4A C3A C2A -64.1(5) . . . . ? C5A N4A C3A C3B 172.3(3) . . . . ? C5B C6B C11B C10B 179.7(4) . . . . ? C5B C6B C11B O11B -0.4(6) . . . . ? C5B N4B C3B C2B -78.9(4) . . . . ? C5B N4B C3B C3A 155.2(3) . . . . ? C5C N4C C3C C2C -60.2(5) . . . . ? C5C N4C C3C C3D 176.9(3) . . . . ? C5D C6D C7D C8D 175.7(4) . . . . ? C5D C6D C11D C10D -173.7(4) . . . . ? C5D C6D C11D O11D 5.5(6) . . . . ? C5D N4D C3D C2D -80.6(5) . . . . ? C5D N4D C3D C3C 153.4(4) . . . . ? C5E C6E C7E C8E -175.8(5) . . . . ? C5E N4E C3E C2E -62.8(5) . . . . ? C5E N4E C3E C3F 176.3(4) . . . . ? C5F C6F C7F C8F 175.9(4) . . . . ? C5F N4F C3F C2F -77.3(5) . . . . ? C5F N4F C3F C3E 155.7(3) . . . . ? C5G C6G C7G C8G -178.5(5) . . . . ? C5G N4G C3G C2G -61.6(5) . . . . ? C5G N4G C3G C3H 176.0(4) . . . . ? C5H C6H C7H C8H 175.8(6) . . . . ? C5H C6H C11H C10H -174.5(4) . . . . ? C5H C6H C11H O11H 3.8(7) . . . . ? C5H N4H C3H C2H -81.3(5) . . . . ? C5H N4H C3H C3G 154.0(4) . . . . ? C6A C7A C8A C9A -0.4(7) . . . . ? C6B C7B C8B C9B -2.5(8) . . . . ? C6D C11D C10D C9D -2.9(6) . . . . ? C6D C11D C10D C12D 176.5(4) . . . . ? C6E C7E C8E C9E 0.2(8) . . . . ? C6F C11F C10F C9F -4.9(6) . . . . ? C6F C11F C10F C12F 174.4(4) . . . . ? C6G C7G C8G C9G 2.7(8) . . . . ? C6G C11G C10G C9G 5.1(7) . . . . ? C6G C11G C10G C12G -166.0(4) . . . . ? C6H C7H C8H C9H -0.2(10) . . . . ? C6H C11H C10H C9H -2.4(7) . . . . ? C6H C11H C10H C12H 179.2(5) . . . . ? C7A C6A C5A N4A -120.1(4) . . . . ? C7A C6A C11A C10A -4.5(6) . . . . ? C7A C6A C11A O11A 177.0(4) . . . . ? C7B C6B C11B C10B 0.3(6) . . . . ? C7B C6B C11B O11B -179.8(4) . . . . ? C7B C8B C9B C10B 2.3(8) . . . . ? C7D C6D C5D N4D 130.5(4) . . . . ? C7D C6D C11D C10D 4.4(6) . . . . ? C7D C6D C11D O11D -176.5(4) . . . . ? C7D C8D C9D C10D 2.3(8) . . . . ? C7E C6E C5E N4E -119.9(5) . . . . ? C7G C6G C5G N4G -121.2(5) . . . . ? C7G C8G C9G C10G -2.5(8) . . . . ? C7H C6H C5H N4H 130.8(5) . . . . ? C7H C6H C11H C10H 3.6(7) . . . . ? C7H C6H C11H O11H -178.1(5) . . . . ? C8A C9A C10A C11A -0.5(7) . . . . ? C8A C9A C10A C12A 175.0(4) . . . . ? C8B C7B C6B C5B -178.2(5) . . . . ? C8B C7B C6B C11B 1.3(7) . . . . ? C8C C7C C6C C5C -173.8(4) . . . . ? C8C C7C C6C C11C 4.6(7) . . . . ? C8D C9D C10D C11D -0.4(7) . . . . ? C8D C9D C10D C12D -179.8(5) . . . . ? C8E C9E C10E C11E -2.2(7) . . . . ? C8E C9E C10E C12E 171.9(5) . . . . ? C8F C9F C10F C11F 0.3(7) . . . . ? C8F C9F C10F C12F -179.0(5) . . . . ? C9A C10A C11A C6A 3.1(6) . . . . ? C9A C10A C11A O11A -178.4(4) . . . . ? C9A C10A C12A C13A 135.4(5) . . . . ? C9A C10A C12A C14A 13.5(6) . . . . ? C9A C10A C12A C15A -105.1(5) . . . . ? C9B C10B C11B C6B -0.5(6) . . . . ? C9B C10B C11B O11B 179.6(4) . . . . ? C9B C10B C12B C13B 112.1(5) . . . . ? C9B C10B C12B C14B -6.4(7) . . . . ? C9B C10B C12B C15B -125.6(5) . . . . ? C9C C8C C7C C6C -0.6(7) . . . . ? C9C C10C C11C C6C 5.9(6) . . . . ? C9C C10C C11C O11C -177.8(4) . . . . ? C9C C10C C12C C13C 8.9(6) . . . . ? C9C C10C C12C C14C 130.9(4) . . . . ? C9C C10C C12C C15C -108.6(5) . . . . ? C9D C8D C7D C6D -0.9(7) . . . . ? C9E C10E C11E C6E 6.7(6) . . . . ? C9E C10E C11E O11E -177.2(4) . . . . ? C9E C10E C12E C13E 9.4(7) . . . . ? C9E C10E C12E C14E -109.3(5) . . . . ? C9E C10E C12E C15E 129.5(5) . . . . ? C9F C8F C7F C6F -3.3(7) . . . . ? C9F C10F C12F C13F 7.2(7) . . . . ? C9F C10F C12F C14F 124.3(5) . . . . ? C9F C10F C12F C15F -114.2(5) . . . . ? C9G C10G C12G C13G 131.6(5) . . . . ? C9G C10G C12G C14G 11.6(6) . . . . ? C9G C10G C12G C15G -107.6(5) . . . . ? C9H C10H C12H C13H -116.3(6) . . . . ? C9H C10H C12H C14H 3.2(8) . . . . ? C9H C10H C12H C15H 122.6(6) . . . . ? C10A C9A C8A C7A -0.9(7) . . . . ? C10C C9C C8C C7C -0.6(7) . . . . ? C10C C11C C6C C5C 171.0(4) . . . . ? C10C C11C C6C C7C -7.3(7) . . . . ? C10E C9E C8E C7E -1.4(8) . . . . ? C10E C11E C6E C5E 172.3(4) . . . . ? C10E C11E C6E C7E -8.0(7) . . . . ? C10F C9F C8F C7F 3.8(8) . . . . ? C10F C11F C6F C5F -171.8(4) . . . . ? C10F C11F C6F C7F 5.6(6) . . . . ? C10G C11G C6G C5G 174.5(4) . . . . ? C10G C11G C6G C7G -5.1(7) . . . . ? C10H C9H C8H C7H 1.3(11) . . . . ? C11A C6A C5A N4A 58.7(5) . . . . ? C11A C6A C7A C8A 3.1(7) . . . . ? C11A C10A C12A C13A -49.5(6) . . . . ? C11A C10A C12A C14A -171.3(5) . . . . ? C11A C10A C12A C15A 70.1(5) . . . . ? C11B C10B C9B C8B -0.8(8) . . . . ? C11B C10B C12B C13B -65.4(6) . . . . ? C11B C10B C12B C14B 176.1(4) . . . . ? C11B C10B C12B C15B 56.9(6) . . . . ? C11C C10C C9C C8C -2.0(7) . . . . ? C11C C10C C12C C13C -176.9(4) . . . . ? C11C C10C C12C C14C -55.0(6) . . . . ? C11C C10C C12C C15C 65.5(5) . . . . ? C11D C6D C5D N4D -51.4(5) . . . . ? C11D C6D C7D C8D -2.5(7) . . . . ? C11E C6E C5E N4E 59.7(6) . . . . ? C11E C6E C7E C8E 4.5(7) . . . . ? C11E C10E C12E C13E -176.9(5) . . . . ? C11E C10E C12E C14E 64.4(6) . . . . ? C11E C10E C12E C15E -56.8(6) . . . . ? C11E O11E Al3 Al4 161.1(3) . . . . ? C11E O11E Al3 N4E 32.3(3) . . . . ? C11E O11E Al3 O11F -62.1(3) . . . . ? C11E O11E Al3 O34E 122.1(3) . . . . ? C11E O11E Al3 O34F -161.8(3) . . . . ? C11F C6F C7F C8F -1.4(7) . . . . ? C11F C10F C12F C13F -172.1(4) . . . . ? C11F C10F C12F C14F -55.0(6) . . . . ? C11F C10F C12F C15F 66.5(6) . . . . ? C11G C6G C5G N4G 59.3(5) . . . . ? C11G C6G C7G C8G 1.0(7) . . . . ? C11G C10G C9G C8G -1.4(8) . . . . ? C11G C10G C12G C13G -57.5(6) . . . . ? C11G C10G C12G C14G -177.5(4) . . . . ? C11G C10G C12G C15G 63.3(5) . . . . ? C11H C6H C5H N4H -51.1(6) . . . . ? C11H C6H C7H C8H -2.3(9) . . . . ? C11H C10H C9H C8H 0.1(9) . . . . ? C11H C10H C12H C13H 62.1(7) . . . . ? C11H C10H C12H C14H -178.4(5) . . . . ? C11H C10H C12H C15H -59.0(7) . . . . ? C11S C12S C13S C14S -1.1(11) . . . . ? C11S C16S C15S C14S 1.5(11) . . . . ? C12A C10A C11A C6A -172.2(4) . . . . ? C12A C10A C11A O11A 6.3(6) . . . . ? C12B C10B C9B C8B -178.4(5) . . . . ? C12B C10B C11B C6B 177.1(4) . . . . ? C12B C10B C11B O11B -2.9(7) . . . . ? C12C C10C C9C C8C 172.6(4) . . . . ? C12C C10C C11C C6C -168.5(4) . . . . ? C12C C10C C11C O11C 7.8(6) . . . . ? C12E C10E C11E C6E -167.2(4) . . . . ? C12E C10E C11E O11E 9.0(7) . . . . ? C12G C10G C9G C8G 169.9(5) . . . . ? C12H C10H C9H C8H 178.5(6) . . . . ? C12S C11S C16S C15S -1.4(10) . . . . ? C13D C12D C10D C9D 121.2(5) . . . . ? C13D C12D C10D C11D -58.2(6) . . . . ? C13S C14S C15S C16S -1.5(13) . . . . ? C14D C12D C10D C9D 3.3(8) . . . . ? C14D C12D C10D C11D -176.1(5) . . . . ? C15D C12D C10D C9D -117.0(5) . . . . ? C15D C12D C10D C11D 63.6(6) . . . . ? C15S C14S C13S C12S 1.3(13) . . . . ? C16S C11S C12S C13S 1.2(10) . . . . ? C21S C22S C23S C24S 0.7(10) . . . . ? C21S C26S C25S C24S 1.5(10) . . . . ? C22S C23S C24S C25S 2.0(10) . . . . ? C23S C22S C21S C26S -2.2(9) . . . . ? C23S C22S C21S Cl2S -178.4(5) . . . . ? C23S C24S C25S C26S -3.0(10) . . . . ? C25S C26S C21S C22S 1.1(9) . . . . ? C25S C26S C21S Cl2S 177.3(5) . . . . ? C32S C31S C36S C35S -2.5(14) . . . . ? C32S C33S C34S C35S 6.7(19) . . . . ? C33S C34S C35S C36S -9(2) . . . . ? C34S C33S C32S C31S -2.9(16) . . . . ? C34S C35S C36S C31S 6.4(19) . . . . ? C36S C31S C32S C33S 0.9(13) . . . . ? C41S C42S C43S C44S 0.0 . . . . ? C42S C41S C46S C45S -0.037(2) . . . . ? C42S C43S C44S C45S -0.001(1) . . . . ? C43S C44S C45S C46S -0.017(1) . . . . ? C44S C45S C46S C41S 0.0 . . . . ? C46S C41S C42S C43S 0.019(2) . . . . ? C51S C56S C55S C54S 4.1(9) . . . . ? C52S C51S C56S C55S -3.4(9) . . . . ? C52S C53S C54S C55S 1.1(9) . . . . ? C53S C54S C55S C56S -3.0(9) . . . . ? C54S C53S C52S C51S -0.4(9) . . . . ? C56S C51S C52S C53S 1.5(9) . . . . ? C61S C62S C63S C64S -0.059(1) . . . . ? C62S C61S C66S C65S 0.0 . . . . ? C62S C63S C64S C65S 0.036(1) . . . . ? C63S C64S C65S C66S 0.0 . . . . ? C64S C65S C66S C61S 0.0 . . . . ? C66S C61S C62S C63S 0.1 . . . . ? C71S C72S C73S C74S 0.0 . . . . ? C72S C71S C76S C75S 0.0 . . . . ? C72S C73S C74S C75S 0.0 . . . . ? C73S C74S C75S C76S 0.0 . . . . ? C74S C75S C76S C71S 0.0 . . . . ? C76S C71S C72S C73S 0.0 . . . . ? C81S C82S C83S C84S 0.043(6) . . . . ? C82S C81S C86S C85S -0.003(2) . . . . ? C82S C83S C84S C85S -0.033(6) . . . . ? C83S C84S C85S C86S 0.006(4) . . . . ? C84S C85S C86S C81S 0.012(2) . . . . ? C86S C81S C82S C83S -0.025(4) . . . . ? Cl1S C11S C12S C13S -178.9(5) . . . . ? Cl1S C11S C16S C15S 178.7(5) . . . . ? Cl3S C31S C32S C33S -175.8(8) . . . . ? Cl3S C31S C36S C35S 174.1(9) . . . . ? Cl4S C41S C42S C43S -173.237(1) . . . . ? Cl4S C41S C46S C45S 173.167(1) . . . . ? Cl5S C51S C52S C53S -180.0(5) . . . . ? Cl5S C51S C56S C55S 178.1(5) . . . . ? Cl6S C61S C62S C63S 179.5 . . . . ? Cl6S C61S C66S C65S -179.4 . . . . ? Cl7S C71S C72S C73S -179.5 . . . . ? Cl7S C71S C76S C75S 179.6 . . . . ? Cl8S C81S C82S C83S 177.288(1) . . . . ? Cl8S C81S C86S C85S -177.335(1) . . . . ? N4A Al1 Al2 N4C 25.0(2) . . . . ? N4A Al1 Al2 N4D 97.86(17) . . . . ? N4A Al1 Al2 O11C -70.90(17) . . . . ? N4A Al1 Al2 O11D -175.30(19) . . . . ? N4A Al1 Al2 O12A -168.8(2) . . . . ? N4A Al1 Al2 O12B 10.65(19) . . . . ? N4A Al1 N4B C3B -4.3(3) . . . . ? N4A Al1 N4B C5B -130.7(3) . . . . ? N4A Al1 O11A C11A 30.7(3) . . . . ? N4A Al1 O11B C11B 71.0(4) . . . . ? N4A Al1 O12A Al2 32.4(6) . . . . ? N4A Al1 O12B Al2 -171.69(15) . . . . ? N4A C3A C2A C1A -178.2(4) . . . . ? N4B Al1 Al2 N4C 101.93(18) . . . . ? N4B Al1 Al2 N4D 174.78(14) . . . . ? N4B Al1 Al2 O11C 6.02(14) . . . . ? N4B Al1 Al2 O11D -98.38(18) . . . . ? N4B Al1 Al2 O12A -91.92(19) . . . . ? N4B Al1 Al2 O12B 87.56(17) . . . . ? N4B Al1 N4A C3A -23.4(3) . . . . ? N4B Al1 N4A C5A -151.9(3) . . . . ? N4B Al1 O11B C11B -10.1(4) . . . . ? N4B Al1 O12A Al2 87.20(16) . . . . ? N4B Al1 O12B Al2 -90.55(15) . . . . ? N4B C3B C2B C1B -179.1(4) . . . . ? N4B C3B C3A C2A -175.7(3) . . . . ? N4B C3B C3A N4A -48.7(4) . . . . ? N4B C5B C6B C7B 127.9(4) . . . . ? N4B C5B C6B C11B -51.6(5) . . . . ? N4C Al2 N4D C3D 1.6(3) . . . . ? N4C Al2 N4D C5D -127.0(3) . . . . ? N4C Al2 O11C C11C 35.9(3) . . . . ? N4C Al2 O11D C11D 71.0(4) . . . . ? N4C Al2 O12A Al1 40.8(6) . . . . ? N4C Al2 O12B Al1 -169.01(15) . . . . ? N4C C3C C2C C1C -177.8(4) . . . . ? N4C C3C C3D C2D -176.4(4) . . . . ? N4C C3C C3D N4D -48.9(4) . . . . ? N4C C5C C6C C7C -121.7(4) . . . . ? N4C C5C C6C C11C 60.0(5) . . . . ? N4D Al2 N4C C3C -28.8(3) . . . . ? N4D Al2 N4C C5C -156.7(3) . . . . ? N4D Al2 O11C C11C 67.8(9) . . . . ? N4D Al2 O11D C11D -8.4(4) . . . . ? N4D Al2 O12A Al1 85.11(17) . . . . ? N4D Al2 O12B Al1 -89.71(15) . . . . ? N4D C3D C2D C1D 178.9(4) . . . . ? N4E Al3 Al4 N4G 25.3(2) . . . . ? N4E Al3 Al4 N4H 98.76(17) . . . . ? N4E Al3 Al4 O11G -70.40(18) . . . . ? N4E Al3 Al4 O11H -173.7(2) . . . . ? N4E Al3 Al4 O34E 12.49(19) . . . . ? N4E Al3 Al4 O34F -167.6(2) . . . . ? N4E Al3 N4F C3F -1.8(3) . . . . ? N4E Al3 N4F C5F -129.0(3) . . . . ? N4E Al3 O11F C11F 70.7(4) . . . . ? N4E Al3 O34E Al4 -170.26(15) . . . . ? N4F Al3 Al4 N4G 100.42(18) . . . . ? N4F Al3 Al4 N4H 173.88(14) . . . . ? N4F Al3 Al4 O11G 4.71(14) . . . . ? N4F Al3 Al4 O11H -98.6(2) . . . . ? N4F Al3 Al4 O34E 87.60(17) . . . . ? N4F Al3 Al4 O34F -92.46(19) . . . . ? N4F Al3 N4E C3E -27.3(3) . . . . ? N4F Al3 N4E C5E -154.9(3) . . . . ? N4F Al3 O11F C11F -9.1(4) . . . . ? N4F Al3 O34E Al4 -90.46(15) . . . . ? N4F C3F C2F C1F 179.5(4) . . . . ? N4F C3F C3E C2E -175.4(3) . . . . ? N4F C3F C3E N4E -51.2(4) . . . . ? N4F C5F C6F C7F 127.1(4) . . . . ? N4F C5F C6F C11F -55.5(5) . . . . ? N4G Al4 N4H C3H -1.6(3) . . . . ? N4G Al4 N4H C5H -128.2(3) . . . . ? N4G Al4 O11G C11G 35.9(3) . . . . ? N4G Al4 O11H C11H 73.5(4) . . . . ? N4G Al4 O34E Al3 -170.32(15) . . . . ? N4G C3G C3H C2H -176.8(4) . . . . ? N4G C3G C3H N4H -49.5(4) . . . . ? N4H Al4 N4G C3G -26.9(3) . . . . ? N4H Al4 N4G C5G -155.4(3) . . . . ? N4H Al4 O11G C11G 68.0(9) . . . . ? N4H Al4 O11H C11H -6.1(4) . . . . ? N4H Al4 O34E Al3 -90.99(15) . . . . ? O11A Al1 Al2 N4C -69.30(18) . . . . ? O11A Al1 Al2 N4D 3.55(14) . . . . ? O11A Al1 Al2 O11C -165.22(14) . . . . ? O11A Al1 Al2 O11D 90.39(18) . . . . ? O11A Al1 Al2 O12A 96.85(19) . . . . ? O11A Al1 Al2 O12B -83.67(17) . . . . ? O11A Al1 N4A C3A 152.0(3) . . . . ? O11A Al1 N4A C5A 23.5(3) . . . . ? O11A Al1 O11B C11B 162.6(4) . . . . ? O11A Al1 O12A Al2 -86.51(17) . . . . ? O11A Al1 O12B Al2 96.99(15) . . . . ? O11B Al1 Al2 N4C -171.2(2) . . . . ? O11B Al1 Al2 N4D -98.39(19) . . . . ? O11B Al1 Al2 O11C 92.85(19) . . . . ? O11B Al1 Al2 O11D -11.5(2) . . . . ? O11B Al1 Al2 O12A -5.1(2) . . . . ? O11B Al1 Al2 O12B 174.4(2) . . . . ? O11B Al1 N4A C3A -112.3(3) . . . . ? O11B Al1 N4A C5A 119.2(3) . . . . ? O11B Al1 N4B C3B 88.7(3) . . . . ? O11B Al1 N4B C5B -37.7(3) . . . . ? O11B Al1 O11A C11A -62.3(3) . . . . ? O11B Al1 O12A Al2 176.50(15) . . . . ? O11C Al2 N4C C3C 145.2(3) . . . . ? O11C Al2 N4C C5C 17.2(3) . . . . ? O11C Al2 N4D C3D -30.9(9) . . . . ? O11C Al2 N4D C5D -159.5(7) . . . . ? O11C Al2 O11D C11D 162.4(4) . . . . ? O11C Al2 O12A Al1 -86.94(17) . . . . ? O11C Al2 O12B Al1 99.99(15) . . . . ? O11C C11C C6C C5C -5.4(6) . . . . ? O11C C11C C6C C7C 176.2(4) . . . . ? O11D Al2 N4C C3C -118.6(3) . . . . ? O11D Al2 N4C C5C 113.5(3) . . . . ? O11D Al2 N4D C3D 94.8(3) . . . . ? O11D Al2 N4D C5D -33.9(3) . . . . ? O11D Al2 O11C C11C -57.4(3) . . . . ? O11D Al2 O12A Al1 175.39(15) . . . . ? O11D C11D C10D C9D 177.9(4) . . . . ? O11D C11D C10D C12D -2.7(7) . . . . ? O11E Al3 Al4 N4G -70.09(18) . . . . ? O11E Al3 Al4 N4H 3.36(14) . . . . ? O11E Al3 Al4 O11G -165.81(14) . . . . ? O11E Al3 Al4 O11H 90.9(2) . . . . ? O11E Al3 Al4 O34E -82.92(17) . . . . ? O11E Al3 Al4 O34F 97.02(19) . . . . ? O11E Al3 N4E C3E 148.2(3) . . . . ? O11E Al3 N4E C5E 20.6(3) . . . . ? O11E Al3 O11F C11F 162.7(4) . . . . ? O11E Al3 O34E Al4 98.14(15) . . . . ? O11E C11E C6E C5E -3.9(6) . . . . ? O11E C11E C6E C7E 175.7(4) . . . . ? O11F Al3 Al4 N4G -172.2(2) . . . . ? O11F Al3 Al4 N4H -98.73(19) . . . . ? O11F Al3 Al4 O11G 92.11(19) . . . . ? O11F Al3 Al4 O11H -11.2(2) . . . . ? O11F Al3 Al4 O34E 175.0(2) . . . . ? O11F Al3 Al4 O34F -5.1(2) . . . . ? O11F Al3 N4E C3E -116.3(3) . . . . ? O11F Al3 N4E C5E 116.1(3) . . . . ? O11F Al3 N4F C3F 92.6(3) . . . . ? O11F Al3 N4F C5F -34.7(3) . . . . ? O11F C11F C6F C5F 8.1(6) . . . . ? O11F C11F C6F C7F -174.6(4) . . . . ? O11F C11F C10F C9F 175.2(4) . . . . ? O11F C11F C10F C12F -5.5(7) . . . . ? O11G Al4 N4G C3G 147.2(3) . . . . ? O11G Al4 N4G C5G 18.7(3) . . . . ? O11G Al4 N4H C3H -34.3(10) . . . . ? O11G Al4 N4H C5H -160.9(7) . . . . ? O11G Al4 O11H C11H 164.9(4) . . . . ? O11G Al4 O34E Al3 98.49(15) . . . . ? O11G C11G C6G C5G -3.3(6) . . . . ? O11G C11G C6G C7G 177.1(4) . . . . ? O11G C11G C10G C9G -177.2(4) . . . . ? O11G C11G C10G C12G 11.6(7) . . . . ? O11H Al4 N4G C3G -117.0(3) . . . . ? O11H Al4 N4G C5G 114.6(3) . . . . ? O11H Al4 N4H C3H 90.4(3) . . . . ? O11H Al4 N4H C5H -36.3(3) . . . . ? O11H Al4 O11G C11G -56.2(3) . . . . ? O11H C11H C10H C9H 179.3(5) . . . . ? O11H C11H C10H C12H 0.9(7) . . . . ? O12A Al1 Al2 N4C -166.1(2) . . . . ? O12A Al1 Al2 N4D -93.30(19) . . . . ? O12A Al1 Al2 O11C 97.94(19) . . . . ? O12A Al1 Al2 O11D -6.5(2) . . . . ? O12A Al1 Al2 O12B 179.5(2) . . . . ? O12A Al1 N4A C3A 32.5(7) . . . . ? O12A Al1 N4A C5A -96.1(6) . . . . ? O12A Al1 N4B C3B -170.7(3) . . . . ? O12A Al1 N4B C5B 62.8(3) . . . . ? O12A Al1 O11A C11A -163.6(3) . . . . ? O12A Al1 O11B C11B -99.4(4) . . . . ? O12A Al1 O12B Al2 -0.32(14) . . . . ? O12A Al2 N4C C3C 16.5(7) . . . . ? O12A Al2 N4C C5C -111.4(5) . . . . ? O12A Al2 N4D C3D -166.8(3) . . . . ? O12A Al2 N4D C5D 64.5(3) . . . . ? O12A Al2 O11C C11C -156.9(3) . . . . ? O12A Al2 O11D C11D -97.4(4) . . . . ? O12A Al2 O12B Al1 0.32(14) . . . . ? O12B Al1 Al2 N4C 14.4(2) . . . . ? O12B Al1 Al2 N4D 87.22(18) . . . . ? O12B Al1 Al2 O11C -81.55(17) . . . . ? O12B Al1 Al2 O11D 174.1(2) . . . . ? O12B Al1 Al2 O12A -179.5(2) . . . . ? O12B Al1 N4A C3A 63.5(3) . . . . ? O12B Al1 N4A C5A -65.0(3) . . . . ? O12B Al1 N4B C3B -94.5(3) . . . . ? O12B Al1 N4B C5B 139.1(3) . . . . ? O12B Al1 O11A C11A 120.4(3) . . . . ? O12B Al1 O12A Al2 0.34(15) . . . . ? O12B Al2 N4C C3C 56.4(3) . . . . ? O12B Al2 N4C C5C -71.6(3) . . . . ? O12B Al2 N4D C3D -89.9(3) . . . . ? O12B Al2 N4D C5D 141.4(3) . . . . ? O12B Al2 O11C C11C 126.6(3) . . . . ? O12B Al2 O12A Al1 -0.34(15) . . . . ? O34E Al3 Al4 N4G 12.8(2) . . . . ? O34E Al3 Al4 N4H 86.27(17) . . . . ? O34E Al3 Al4 O11G -82.89(17) . . . . ? O34E Al3 Al4 O11H 173.8(2) . . . . ? O34E Al3 Al4 O34F 179.9(2) . . . . ? O34E Al3 N4E C3E 59.4(3) . . . . ? O34E Al3 N4E C5E -68.1(3) . . . . ? O34E Al3 N4F C3F -92.2(3) . . . . ? O34E Al3 N4F C5F 140.6(3) . . . . ? O34E Al4 N4G C3G 58.0(3) . . . . ? O34E Al4 N4G C5G -70.4(3) . . . . ? O34E Al4 N4H C3H -94.3(3) . . . . ? O34E Al4 N4H C5H 139.0(3) . . . . ? O34E Al4 O11G C11G 127.8(3) . . . . ? O34F Al3 Al4 N4G -167.1(2) . . . . ? O34F Al3 Al4 N4H -93.66(19) . . . . ? O34F Al3 Al4 O11G 97.17(19) . . . . ? O34F Al3 Al4 O11H -6.1(2) . . . . ? O34F Al3 Al4 O34E -179.9(2) . . . . ? O34F Al3 N4E C3E 25.0(7) . . . . ? O34F Al3 N4E C5E -102.6(6) . . . . ? O34F Al3 N4F C3F -168.5(3) . . . . ? O34F Al3 N4F C5F 64.2(3) . . . . ? O34F Al3 O11F C11F -98.8(4) . . . . ? O34F Al3 O34E Al4 0.04(14) . . . . ? O34F Al4 N4G C3G 19.6(7) . . . . ? O34F Al4 N4G C5G -108.9(6) . . . . ? O34F Al4 N4H C3H -170.5(3) . . . . ? O34F Al4 N4H C5H 62.8(3) . . . . ? O34F Al4 O11G C11G -156.3(3) . . . . ? O34F Al4 O11H C11H -96.0(4) . . . . ? O34F Al4 O34E Al3 -0.04(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.819 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.093 #################EOF#######################