Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_c79h119a _database_code_CSD 163151 _journal_coden_Cambridge 182 #============================================================================== #data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2001-05-23 10:27:12' _audit_creation_method 'PLATON option' _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Dr. B. Hessen ; _publ_contact_author_address # Address of author for correspondence ; Dutch Polymer Institute Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_email hessen@chem.rug.nl _publ_contact_author_fax '+31 50 3634441' _publ_contact_author_phone '+31 50 3634315' _publ_requested_journal ' Chemical Communication' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission : 2001-05-23 Consider this CIF submission for depostion of the X-ray structures of the manuscript entitled: Synthesis and structural characterisation of a boraluminoxane capable of activating a zirconocene ethene polymerisation catalyst to be submitted to : Chemical Communications Your Reference number : B103670J (Our Compound_Identification_Code : CP593) ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The reaction of Bu^t^~3~Al with ArB(OH)~2~ (Ar=2,6-dissopropylphenyl) leads, via the intermediate [Bu^t^~2~Al(O)BAr(OH)]~2~ (1), to the crystallographically characterised boraluminoxane Al(Bu^t^~2~Al)(Bu^t^Al)~2~(O~2~BAr)~4~ (3) which is able to activate Cp~2~ZrMe~2~ to effect catalytic ethene polymerisation. ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Richter, Bodo' ; Dutch Polymer Institute Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Meetsma, Auke' ; Dutch Polymer Institute Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Hessen, Bart' ; Dutch Polymer Institute Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Teuben, Jan H.' ; Dutch Polymer Institute Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; # Insert blank lines between references _publ_section_references ; Beurskens, P.T., Beurskens, G., Gelder, R. de Garc\'ia-Granda, S. Gould, R.O. Isra\"el, & Smits, J.M.M. (1999). The DIRDIF99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Bruker, (2000). SMART, SAINT, SADABS, XPREP and SHELXTL/NT. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (2001). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. SHELXL97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany, 1997. Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program. University of G\"ottingen, Germany, 2001 Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. Perspective PLUTO drawing of the molecule illustrating the configuration and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. Displacement ellipsoids for non-H are represented at the 50% probability level. The H-atoms are drawn with an arbitrary radius. ; #=============================================================================== #data_c79h119a #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H104 Al4 B4 O8, 2.5(C6 H6)' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C79 H119 Al4 B4 O8' _chemical_formula_weight 1347,96 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.0027(5) _cell_length_b 14.2483(5) _cell_length_c 22.7478(9) _cell_angle_alpha 79.888(1) _cell_angle_beta 86.886(1) _cell_angle_gamma 65.389(1) _cell_volume 4061.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 9078 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.29 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 9078 reflections after integration using the SAINT software package (Bruker, 2000). Intensity data were corrected for decay and absorption using SADABS (Sheldrick, 2000) ; _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.480 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1458 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_type 'Multi-Scan' _exptl_absorpt_process_details 'Sheldrick, Bruker, 2000)' _exptl_absorpt_correction_T_min 0.9482 _exptl_absorpt_correction_T_max 0.9872 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method 'phi and omega scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 38591 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 29.02 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.944 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001) Intensity data were corrected for Lorentz and polarization effects, scale variation, for absorption and reduced to F~o~^2^ ; # number of unique reflections _reflns_number_total 20435 _reflns_number_gt 13923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker Version 5.168, 2000' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2001) PLATON (Spek, 1994) ; _computing_publication_material ; PLATON (Spek, 1990) SHELXL (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; The structure was solved by Patterson methods and extension of the model was accomplished by direct methods applied to difference structure factors using the program DIRDIF. The positional and anisotropic displacement parameters for the non-hydrogen atoms were refined. Refinement was frustrated by a disorder problem: from the solution it was clear that one of the benzene solvent molecules was highly disordered. The electron density of the carbon atoms appeared to be spread out, indicating transformational disorder. This molecule was fitted to two partial occupied regular hexagons (with consequence of large a.d.p.s) The hydrogen atoms were included in the final refinement riding on their carrier atoms. 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^)+(0.0889P)^2^+0.5086P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 20435 _refine_ls_number_parameters 912 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.618 _refine_ls_shift/su_mean 0.044 _refine_diff_density_max 0.686 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.056 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Al1 Al Uani 0.30442(4) 0.95613(4) 0.27023(2) 1.000 0.0212(2) . . Al2 Al Uani 0.56154(4) 0.83274(4) 0.31351(3) 1.000 0.0282(2) . . Al3 Al Uani 0.19790(4) 1.09664(4) 0.17402(2) 1.000 0.0258(2) . . Al4 Al Uani 0.16283(4) 0.89936(4) 0.33023(2) 1.000 0.0252(2) . . O1 O Uani 0.44507(9) 0.93540(9) 0.26261(5) 1.000 0.0252(4) . . O2 O Uani 0.30941(9) 1.07771(9) 0.22014(5) 1.000 0.0243(3) . . O3 O Uani 0.09829(9) 1.15505(10) 0.22270(6) 1.000 0.0290(4) . . O4 O Uani 0.17791(9) 1.02521(9) 0.30709(5) 1.000 0.0235(3) . . O5 O Uani 0.30819(9) 0.84699(9) 0.32704(5) 1.000 0.0245(3) . . O6 O Uani 0.48259(10) 0.78506(11) 0.36132(6) 1.000 0.0336(4) . . O7 O Uani 0.23948(9) 0.95213(10) 0.20255(5) 1.000 0.0249(4) . . O8 O Uani 0.13892(10) 0.87302(11) 0.26111(6) 1.000 0.0313(4) . . C1 C Uani 0.48577(14) 1.08276(15) 0.18554(9) 1.000 0.0303(6) . . C2 C Uani 0.47023(16) 1.18361(17) 0.19383(10) 1.000 0.0398(7) . . C3 C Uani 0.5183(2) 1.2379(2) 0.15535(14) 1.000 0.0607(10) . . C4 C Uani 0.5795(2) 1.1945(2) 0.10947(14) 1.000 0.0669(11) . . C5 C Uani 0.59587(19) 1.0958(2) 0.10133(11) 1.000 0.0521(8) . . C6 C Uani 0.55085(15) 1.03812(17) 0.13913(9) 1.000 0.0358(6) . . C7 C Uani 0.40329(18) 1.23575(18) 0.24404(11) 1.000 0.0452(8) . . C8 C Uani 0.3016(2) 1.3279(2) 0.21931(15) 1.000 0.0698(10) . . C9 C Uani 0.4648(2) 1.2701(2) 0.28337(14) 1.000 0.0668(11) . . C10 C Uani 0.56817(17) 0.92966(18) 0.12882(10) 1.000 0.0423(7) . . C11 C Uani 0.6681(2) 0.8744(2) 0.09519(12) 1.000 0.0625(10) . . C12 C Uani 0.4751(2) 0.9308(3) 0.09704(14) 1.000 0.0698(11) . . C13 C Uani 0.03014(14) 1.20200(14) 0.32595(8) 1.000 0.0273(5) . . C14 C Uani 0.07598(15) 1.22442(15) 0.37267(9) 1.000 0.0314(6) . . C15 C Uani 0.01137(17) 1.28907(18) 0.41153(10) 1.000 0.0419(7) . . C16 C Uani -0.09651(18) 1.33173(19) 0.40463(11) 1.000 0.0482(8) . . C17 C Uani -0.14171(17) 1.31217(17) 0.35898(11) 1.000 0.0432(7) . . C18 C Uani -0.08081(14) 1.24817(15) 0.31888(9) 1.000 0.0313(6) . . C19 C Uani 0.19435(15) 1.18265(16) 0.38211(9) 1.000 0.0352(6) . . C20 C Uani 0.2300(2) 1.2678(2) 0.38884(14) 1.000 0.0593(10) . . C21 C Uani 0.2323(2) 1.0942(2) 0.43563(12) 1.000 0.0604(9) . . C22 C Uani -0.13535(15) 1.23258(17) 0.26761(9) 1.000 0.0359(6) . . C23 C Uani -0.1577(2) 1.3236(2) 0.21580(11) 1.000 0.0552(9) . . C24 C Uani -0.23701(17) 1.2197(2) 0.28540(12) 1.000 0.0520(8) . . C25 C Uani 0.37221(14) 0.69640(14) 0.41888(8) 1.000 0.0263(5) . . C26 C Uani 0.37156(14) 0.70859(15) 0.47945(8) 1.000 0.0299(5) . . C27 C Uani 0.35922(16) 0.63380(17) 0.52382(9) 1.000 0.0377(6) . . C28 C Uani 0.34938(17) 0.54807(18) 0.51028(10) 1.000 0.0430(7) . . C29 C Uani 0.35138(17) 0.53463(16) 0.45128(10) 1.000 0.0395(7) . . C30 C Uani 0.36248(15) 0.60811(15) 0.40532(9) 1.000 0.0310(6) . . C31 C Uani 0.38857(16) 0.79946(16) 0.49653(9) 1.000 0.0356(6) . . C32 C Uani 0.3209(2) 0.8454(2) 0.54845(11) 1.000 0.0531(8) . . C33 C Uani 0.50451(18) 0.76472(19) 0.51184(11) 1.000 0.0460(8) . . C34 C Uani 0.37219(17) 0.58576(16) 0.34175(10) 1.000 0.0374(7) . . C35 C Uani 0.2855(2) 0.5561(2) 0.32480(13) 1.000 0.0593(10) . . C36 C Uani 0.47974(18) 0.50019(19) 0.33275(11) 1.000 0.0470(8) . . C37 C Uani 0.13271(16) 0.88098(16) 0.14711(9) 1.000 0.0334(6) . . C38 C Uani 0.20473(18) 0.81243(19) 0.11154(10) 1.000 0.0436(7) . . C39 C Uani 0.1684(2) 0.7960(2) 0.06008(11) 1.000 0.0573(10) . . C40 C Uani 0.0649(2) 0.8454(2) 0.04336(11) 1.000 0.0613(10) . . C41 C Uani -0.0060(2) 0.9137(2) 0.07705(11) 1.000 0.0531(9) . . C42 C Uani 0.02608(16) 0.93216(18) 0.12940(9) 1.000 0.0376(7) . . C43 C Uani -0.05539(16) 1.00627(19) 0.16584(10) 1.000 0.0416(7) . . C44 C Uani -0.1314(2) 1.1060(2) 0.12759(13) 1.000 0.0655(10) . . C45 C Uani -0.1152(2) 0.9520(3) 0.20419(14) 1.000 0.0696(11) . . C46 C Uani 0.3201(2) 0.7518(2) 0.13029(12) 1.000 0.0581(9) . . C47 C Uani 0.3936(3) 0.7254(3) 0.07745(17) 1.000 0.0896(16) . . C48 C Uani 0.3344(3) 0.6545(3) 0.17237(18) 1.000 0.1098(17) . . C49 C Uani 0.61611(16) 0.91290(18) 0.35492(9) 1.000 0.0381(7) . . C50 C Uani 0.5252(2) 0.9900(2) 0.38619(12) 1.000 0.0553(9) . . C51 C Uani 0.6987(2) 0.8378(2) 0.40307(11) 1.000 0.0559(9) . . C52 C Uani 0.6690(2) 0.9729(2) 0.31323(12) 1.000 0.0532(9) . . C53 C Uani 0.65869(17) 0.71296(17) 0.27610(10) 1.000 0.0433(7) . . C54 C Uani 0.7523(2) 0.7289(2) 0.24474(13) 1.000 0.0666(10) . . C55 C Uani 0.7047(2) 0.6198(2) 0.32790(13) 1.000 0.0626(9) . . C56 C Uani 0.6017(2) 0.6804(2) 0.23327(12) 1.000 0.0605(10) . . C57 C Uani 0.17910(16) 1.16111(17) 0.08958(9) 1.000 0.0360(6) . . C58 C Uani 0.2621(2) 1.2055(2) 0.07050(11) 1.000 0.0574(10) . . C59 C Uani 0.18355(19) 1.0867(2) 0.04725(9) 1.000 0.0459(8) . . C60 C Uani 0.0705(2) 1.2537(2) 0.08216(11) 1.000 0.0619(9) . . C61 C Uani 0.06621(15) 0.88443(16) 0.39281(9) 1.000 0.0327(6) . . C62 C Uani -0.04169(18) 0.9696(2) 0.37324(13) 1.000 0.0651(10) . . C63 C Uani 0.0631(3) 0.7778(2) 0.39820(16) 1.000 0.0802(13) . . C64 C Uani 0.0913(2) 0.8945(3) 0.45536(12) 1.000 0.0767(13) . . B1 B Uani 0.41866(16) 1.03007(16) 0.22297(9) 1.000 0.0246(6) . . B2 B Uani 0.10203(15) 1.12814(16) 0.28230(9) 1.000 0.0256(6) . . B3 B Uani 0.39259(16) 0.77740(16) 0.36801(9) 1.000 0.0252(6) . . B4 B Uani 0.17008(16) 0.89993(17) 0.20665(10) 1.000 0.0279(6) . . C65 C Uani 0.0148(3) 0.4803(4) 0.2448(4) 1.000 0.117(2) . . C66 C Uani 0.0358(3) 0.5502(6) 0.2728(2) 1.000 0.131(2) . . C67 C Uani 0.0471(3) 0.6336(4) 0.2359(4) 1.000 0.121(2) . . C68 C Uani 0.0380(4) 0.6437(5) 0.1806(3) 1.000 0.129(3) . . C69 C Uani 0.0169(5) 0.5804(6) 0.1549(3) 1.000 0.157(4) . . C70 C Uani 0.0070(4) 0.4982(4) 0.1872(4) 1.000 0.130(3) . . C71B C Uani 0.7243(5) 0.5128(6) -0.0434(2) 0.674(11) 0.218(9) . . C72B C Uani 0.8126(4) 0.4789(7) -0.0067(3) 0.674(11) 0.180(6) . . C73B C Uani 0.8022(4) 0.4707(10) 0.0549(3) 0.674(11) 0.355(12) . . C74B C Uani 0.7035(4) 0.4963(7) 0.0798(2) 0.674(11) 0.417(13) . . C75B C Uani 0.6151(4) 0.5302(5) 0.04306(19) 0.674(11) 0.64(3) . . C76B C Uani 0.6256(5) 0.5385(8) -0.01853(19) 0.674(11) 0.393(14) . . C77 C Uani 0.0692(2) 0.5229(2) 0.46222(13) 1.000 0.0606(10) . . C78 C Uani 0.1056(2) 0.4534(2) 0.51402(13) 1.000 0.0556(9) . . C79 C Uani -0.0361(2) 0.5695(2) 0.44813(13) 1.000 0.0616(10) . . C71A C Uani 0.7697(13) 0.4942(16) -0.0427(7) 0.326(11) 0.37(3) . . C72A C Uani 0.8439(12) 0.5146(15) -0.0155(7) 0.326(11) 0.72(10) . . C73A C Uani 0.8279(13) 0.5390(11) 0.0417(7) 0.326(11) 0.189(15) . . C74A C Uani 0.7376(15) 0.5430(11) 0.0719(7) 0.326(11) 0.226(17) . . C75A C Uani 0.6634(11) 0.5226(16) 0.0448(11) 0.326(11) 0.39(3) . . C76A C Uani 0.6794(10) 0.4982(17) -0.0125(11) 0.326(11) 0.51(5) . . H3 H Uiso 0.50867 1.30584 0.16093 1.000 0.0730 . . H4 H Uiso 0.61062 1.23305 0.08329 1.000 0.0802 . . H5 H Uiso 0.63836 1.06659 0.06956 1.000 0.0625 . . H7 H Uiso 0.38348 1.18258 0.27001 1.000 0.0543 . . H8 H Uiso 0.31849 1.37979 0.19187 1.000 0.1046 . . H8' H Uiso 0.26056 1.36016 0.25234 1.000 0.1046 . . H8" H Uiso 0.26049 1.30274 0.19788 1.000 0.1046 . . H9 H Uiso 0.52996 1.21002 0.29822 1.000 0.1000 . . H9' H Uiso 0.42190 1.29666 0.31723 1.000 0.1000 . . H9" H Uiso 0.48173 1.32542 0.25970 1.000 0.1000 . . H10 H Uiso 0.57501 0.88556 0.16908 1.000 0.0508 . . H11 H Uiso 0.66290 0.91340 0.05460 1.000 0.0938 . . H11' H Uiso 0.67644 0.80319 0.09328 1.000 0.0938 . . H11" H Uiso 0.72904 0.87110 0.11615 1.000 0.0938 . . H12 H Uiso 0.41191 0.95895 0.12063 1.000 0.1048 . . H12' H Uiso 0.48873 0.85929 0.09233 1.000 0.1048 . . H12" H Uiso 0.46458 0.97494 0.05761 1.000 0.1048 . . H15 H Uiso 0.04205 1.30379 0.44301 1.000 0.0503 . . H16 H Uiso -0.13962 1.37482 0.43165 1.000 0.0579 . . H17 H Uiso -0.21608 1.34279 0.35450 1.000 0.0517 . . H19 H Uiso 0.22847 1.15273 0.34588 1.000 0.0423 . . H20 H Uiso 0.20240 1.32553 0.35511 1.000 0.0891 . . H20' H Uiso 0.30694 1.23875 0.38952 1.000 0.0891 . . H20" H Uiso 0.20358 1.29388 0.42623 1.000 0.0891 . . H21 H Uiso 0.19693 1.12004 0.47160 1.000 0.0906 . . H21' H Uiso 0.30839 1.06910 0.44106 1.000 0.0906 . . H21" H Uiso 0.21589 1.03650 0.42861 1.000 0.0906 . . H22 H Uiso -0.08576 1.16721 0.25324 1.000 0.0431 . . H23 H Uiso -0.20345 1.38935 0.22920 1.000 0.0828 . . H23' H Uiso -0.19249 1.31300 0.18292 1.000 0.0828 . . H23" H Uiso -0.09140 1.32684 0.20203 1.000 0.0828 . . H24 H Uiso -0.22286 1.16390 0.32013 1.000 0.0780 . . H24' H Uiso -0.26316 1.20135 0.25196 1.000 0.0780 . . H24" H Uiso -0.28995 1.28555 0.29547 1.000 0.0780 . . H27 H Uiso 0.35757 0.64236 0.56440 1.000 0.0452 . . H28 H Uiso 0.34122 0.49800 0.54131 1.000 0.0516 . . H29 H Uiso 0.34513 0.47491 0.44206 1.000 0.0474 . . H31 H Uiso 0.36968 0.85644 0.46088 1.000 0.0428 . . H32 H Uiso 0.24795 0.85783 0.54118 1.000 0.0797 . . H32' H Uiso 0.32430 0.91164 0.55159 1.000 0.0797 . . H32" H Uiso 0.34737 0.79591 0.58575 1.000 0.0797 . . H33 H Uiso 0.52477 0.70974 0.54723 1.000 0.0690 . . H33' H Uiso 0.51581 0.82465 0.52001 1.000 0.0690 . . H33" H Uiso 0.54734 0.73747 0.47809 1.000 0.0690 . . H34 H Uiso 0.36555 0.65117 0.31415 1.000 0.0448 . . H35 H Uiso 0.28907 0.49304 0.35191 1.000 0.0889 . . H35' H Uiso 0.29498 0.54231 0.28367 1.000 0.0889 . . H35" H Uiso 0.21683 0.61377 0.32795 1.000 0.0889 . . H36 H Uiso 0.53467 0.52050 0.34315 1.000 0.0705 . . H36' H Uiso 0.48629 0.49056 0.29088 1.000 0.0705 . . H36" H Uiso 0.48745 0.43447 0.35843 1.000 0.0705 . . H39 H Uiso 0.21669 0.74958 0.03624 1.000 0.0688 . . H40 H Uiso 0.04160 0.83269 0.00833 1.000 0.0734 . . H41 H Uiso -0.07778 0.94869 0.06458 1.000 0.0637 . . H43 H Uiso -0.01701 1.02710 0.19325 1.000 0.0499 . . H44 H Uiso -0.17226 1.08836 0.10120 1.000 0.0983 . . H44' H Uiso -0.09190 1.14119 0.10348 1.000 0.0983 . . H44" H Uiso -0.17916 1.15272 0.15347 1.000 0.0983 . . H45 H Uiso -0.15279 0.92944 0.17855 1.000 0.1043 . . H45' H Uiso -0.16576 1.00059 0.22817 1.000 0.1043 . . H45" H Uiso -0.06589 0.89080 0.23071 1.000 0.1043 . . H46 H Uiso 0.34035 0.79635 0.15196 1.000 0.0696 . . H47 H Uiso 0.46656 0.69991 0.09128 1.000 0.1344 . . H47' H Uiso 0.37640 0.78840 0.04709 1.000 0.1344 . . H47" H Uiso 0.38482 0.67110 0.06016 1.000 0.1344 . . H48 H Uiso 0.28856 0.67225 0.20656 1.000 0.1643 . . H48' H Uiso 0.40778 0.61806 0.18640 1.000 0.1643 . . H48" H Uiso 0.31623 0.60882 0.15194 1.000 0.1643 . . H50 H Uiso 0.55237 1.02545 0.40963 1.000 0.0829 . . H50' H Uiso 0.49096 0.95188 0.41275 1.000 0.0829 . . H50" H Uiso 0.47413 1.04206 0.35621 1.000 0.0829 . . H51 H Uiso 0.75735 0.78682 0.38420 1.000 0.0838 . . H51' H Uiso 0.66657 0.80090 0.43219 1.000 0.0838 . . H51" H Uiso 0.72477 0.87799 0.42343 1.000 0.0838 . . H52 H Uiso 0.61849 1.02268 0.28229 1.000 0.0798 . . H52' H Uiso 0.72910 0.92338 0.29443 1.000 0.0798 . . H52" H Uiso 0.69343 1.01098 0.33630 1.000 0.0798 . . H54 H Uiso 0.79526 0.66735 0.22664 1.000 0.0998 . . H54' H Uiso 0.79503 0.73823 0.27402 1.000 0.0998 . . H54" H Uiso 0.72625 0.79115 0.21359 1.000 0.0998 . . H55 H Uiso 0.64734 0.60647 0.34887 1.000 0.0939 . . H55' H Uiso 0.74388 0.63640 0.35582 1.000 0.0939 . . H55" H Uiso 0.75190 0.55725 0.31189 1.000 0.0939 . . H56 H Uiso 0.65131 0.61659 0.21936 1.000 0.0908 . . H56' H Uiso 0.57296 0.73672 0.19895 1.000 0.0908 . . H56" H Uiso 0.54431 0.66706 0.25413 1.000 0.0908 . . H58 H Uiso 0.33223 1.14778 0.07335 1.000 0.0861 . . H58' H Uiso 0.25910 1.25406 0.09686 1.000 0.0861 . . H58" H Uiso 0.24738 1.24256 0.02920 1.000 0.0861 . . H59 H Uiso 0.13148 1.05795 0.05902 1.000 0.0689 . . H59' H Uiso 0.25389 1.02942 0.04941 1.000 0.0689 . . H59" H Uiso 0.16813 1.12524 0.00627 1.000 0.0689 . . H60 H Uiso 0.05881 1.28820 0.04032 1.000 0.0929 . . H60' H Uiso 0.06723 1.30384 0.10751 1.000 0.0929 . . H60" H Uiso 0.01610 1.22801 0.09392 1.000 0.0929 . . H62 H Uiso -0.09385 0.96290 0.40219 1.000 0.0976 . . H62' H Uiso -0.06020 0.96242 0.33384 1.000 0.0976 . . H62" H Uiso -0.04058 1.03847 0.37105 1.000 0.0976 . . H63 H Uiso 0.00448 0.77641 0.42334 1.000 0.1204 . . H63' H Uiso 0.12924 0.72334 0.41632 1.000 0.1204 . . H63" H Uiso 0.05364 0.76507 0.35842 1.000 0.1204 . . H64 H Uiso 0.08742 0.96492 0.45490 1.000 0.1151 . . H64' H Uiso 0.16229 0.84243 0.46777 1.000 0.1151 . . H64" H Uiso 0.04039 0.88262 0.48351 1.000 0.1151 . . H65 H Uiso 0.00665 0.42157 0.26750 1.000 0.1399 . . H66 H Uiso 0.04203 0.54089 0.31504 1.000 0.1577 . . H67 H Uiso 0.06169 0.68283 0.25274 1.000 0.1459 . . H68 H Uiso 0.04703 0.70071 0.15622 1.000 0.1558 . . H69 H Uiso 0.00852 0.59288 0.11271 1.000 0.1886 . . H70 H Uiso -0.00625 0.45115 0.16743 1.000 0.1553 . . H71B H Uiso 0.73141 0.51845 -0.08552 0.674(11) 0.2608 . . H72B H Uiso 0.88007 0.46138 -0.02375 0.674(11) 0.2165 . . H73B H Uiso 0.86253 0.44750 0.07993 0.674(11) 0.4273 . . H74B H Uiso 0.69634 0.49070 0.12184 0.674(11) 0.4959 . . H75B H Uiso 0.54767 0.54777 0.06007 0.674(11) 0.7701 . . H76B H Uiso 0.56521 0.56165 -0.04361 0.674(11) 0.4698 . . H77 H Uiso 0.11716 0.53896 0.43574 1.000 0.0727 . . H78 H Uiso 0.17864 0.42127 0.52370 1.000 0.0668 . . H79 H Uiso -0.06083 0.61790 0.41204 1.000 0.0738 . . H71 H Uiso 0.78061 0.47756 -0.08184 0.326(11) 0.4462 . . H72 H Uiso 0.90565 0.51191 -0.03616 0.326(11) 0.8638 . . H73 H Uiso 0.87870 0.55295 0.06030 0.326(11) 0.2279 . . H74 H Uiso 0.72670 0.55965 0.11107 0.326(11) 0.2705 . . H75 H Uiso 0.60165 0.52530 0.06538 0.326(11) 0.4744 . . H76 H Uiso 0.62861 0.48425 -0.03107 0.326(11) 0.6195 . . 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 0.0199(2) 0.0230(3) 0.0209(3) -0.0037(2) 0.0007(2) -0.0092(2) Al2 0.0206(3) 0.0309(3) 0.0309(3) -0.0018(2) -0.0011(2) -0.0095(2) Al3 0.0231(3) 0.0313(3) 0.0214(3) -0.0020(2) -0.0005(2) -0.0105(2) Al4 0.0235(3) 0.0277(3) 0.0249(3) -0.0028(2) 0.0022(2) -0.0119(2) O1 0.0209(6) 0.0264(7) 0.0277(7) -0.0027(5) 0.0003(5) -0.0099(5) O2 0.0222(6) 0.0255(6) 0.0264(6) -0.0021(5) -0.0002(5) -0.0118(5) O3 0.0227(6) 0.0312(7) 0.0266(7) -0.0019(5) 0.0000(5) -0.0060(5) O4 0.0225(6) 0.0237(6) 0.0234(6) -0.0047(5) 0.0030(5) -0.0087(5) O5 0.0224(6) 0.0234(6) 0.0256(6) -0.0013(5) -0.0001(5) -0.0085(5) O6 0.0273(7) 0.0400(8) 0.0311(7) 0.0037(6) -0.0030(5) -0.0150(6) O7 0.0246(6) 0.0303(7) 0.0226(6) -0.0062(5) 0.0007(5) -0.0134(5) O8 0.0324(7) 0.0391(8) 0.0290(7) -0.0061(6) 0.0006(5) -0.0210(6) C1 0.0234(9) 0.0340(10) 0.0323(10) 0.0010(8) -0.0014(7) -0.0130(8) C2 0.0337(10) 0.0360(11) 0.0518(13) -0.0016(10) 0.0039(9) -0.0190(9) C3 0.0559(15) 0.0443(14) 0.086(2) -0.0004(14) 0.0167(14) -0.0306(13) C4 0.0599(17) 0.0633(18) 0.077(2) 0.0080(15) 0.0223(15) -0.0351(15) C5 0.0429(13) 0.0605(16) 0.0480(14) 0.0023(12) 0.0155(11) -0.0228(12) C6 0.0277(10) 0.0435(12) 0.0326(11) 0.0015(9) 0.0019(8) -0.0145(9) C7 0.0425(12) 0.0371(12) 0.0646(16) -0.0158(11) 0.0083(11) -0.0228(10) C8 0.0512(16) 0.0548(17) 0.093(2) -0.0205(16) 0.0090(15) -0.0096(13) C9 0.0671(18) 0.0617(18) 0.094(2) -0.0335(16) 0.0058(16) -0.0410(15) C10 0.0404(12) 0.0493(13) 0.0358(12) -0.0103(10) 0.0122(9) -0.0172(10) C11 0.0575(16) 0.0728(19) 0.0512(16) -0.0191(14) 0.0254(13) -0.0206(14) C12 0.0639(18) 0.084(2) 0.074(2) -0.0338(17) 0.0078(15) -0.0357(17) C13 0.0272(9) 0.0239(9) 0.0287(10) -0.0043(7) 0.0035(7) -0.0089(7) C14 0.0320(10) 0.0287(10) 0.0325(10) -0.0073(8) 0.0029(8) -0.0110(8) C15 0.0419(12) 0.0428(12) 0.0411(12) -0.0189(10) 0.0065(9) -0.0137(10) C16 0.0398(12) 0.0518(14) 0.0532(14) -0.0287(12) 0.0152(10) -0.0130(11) C17 0.0293(10) 0.0386(12) 0.0556(14) -0.0163(10) 0.0089(10) -0.0059(9) C18 0.0264(9) 0.0279(10) 0.0357(11) -0.0056(8) 0.0033(8) -0.0077(8) C19 0.0318(10) 0.0367(11) 0.0375(11) -0.0151(9) 0.0013(8) -0.0111(9) C20 0.0470(14) 0.0596(16) 0.083(2) -0.0276(15) 0.0044(13) -0.0277(13) C21 0.0498(15) 0.0617(17) 0.0546(16) 0.0024(13) -0.0122(12) -0.0115(13) C22 0.0248(9) 0.0395(11) 0.0405(12) -0.0079(9) 0.0028(8) -0.0102(8) C23 0.0556(15) 0.0572(16) 0.0476(14) 0.0022(12) -0.0096(12) -0.0212(13) C24 0.0305(11) 0.0653(16) 0.0633(16) -0.0183(13) 0.0051(10) -0.0203(11) C25 0.0233(8) 0.0250(9) 0.0273(9) -0.0013(7) -0.0014(7) -0.0078(7) C26 0.0268(9) 0.0317(10) 0.0261(9) -0.0028(8) 0.0012(7) -0.0081(8) C27 0.0367(11) 0.0430(12) 0.0274(10) 0.0012(9) 0.0024(8) -0.0137(9) C28 0.0399(12) 0.0399(12) 0.0425(13) 0.0109(10) 0.0016(9) -0.0171(10) C29 0.0397(11) 0.0286(10) 0.0487(13) 0.0025(9) -0.0042(10) -0.0156(9) C30 0.0312(10) 0.0258(10) 0.0338(10) -0.0022(8) -0.0036(8) -0.0102(8) C31 0.0430(11) 0.0347(11) 0.0264(10) -0.0064(8) -0.0004(8) -0.0128(9) C32 0.0551(15) 0.0637(16) 0.0412(13) -0.0266(12) 0.0050(11) -0.0187(13) C33 0.0472(13) 0.0504(14) 0.0463(13) -0.0096(11) -0.0020(10) -0.0250(11) C34 0.0473(12) 0.0262(10) 0.0389(12) -0.0059(9) -0.0062(9) -0.0145(9) C35 0.0506(14) 0.0673(18) 0.0668(18) -0.0299(14) -0.0075(13) -0.0229(13) C36 0.0480(13) 0.0437(13) 0.0496(14) -0.0142(11) 0.0039(11) -0.0171(11) C37 0.0364(10) 0.0407(11) 0.0310(10) -0.0082(9) -0.0005(8) -0.0227(9) C38 0.0448(12) 0.0529(14) 0.0416(12) -0.0194(11) 0.0007(10) -0.0241(11) C39 0.0625(16) 0.0756(19) 0.0446(14) -0.0337(13) 0.0054(12) -0.0304(14) C40 0.0689(17) 0.084(2) 0.0410(14) -0.0239(14) -0.0130(12) -0.0344(16) C41 0.0520(14) 0.0688(17) 0.0448(14) -0.0133(12) -0.0133(11) -0.0279(13) C42 0.0394(11) 0.0482(13) 0.0337(11) -0.0070(9) -0.0041(9) -0.0258(10) C43 0.0314(10) 0.0563(14) 0.0416(12) -0.0135(10) -0.0037(9) -0.0200(10) C44 0.0511(15) 0.0677(19) 0.0648(18) -0.0119(15) -0.0073(13) -0.0106(14) C45 0.0596(17) 0.086(2) 0.0709(19) -0.0138(16) 0.0194(14) -0.0396(17) C46 0.0452(14) 0.0665(18) 0.0641(17) -0.0403(15) -0.0006(12) -0.0131(12) C47 0.063(2) 0.116(3) 0.103(3) -0.061(2) 0.0243(18) -0.036(2) C48 0.080(3) 0.117(3) 0.094(3) 0.026(2) -0.025(2) -0.017(2) C49 0.0332(10) 0.0474(13) 0.0385(12) -0.0052(10) -0.0039(9) -0.0216(10) C50 0.0573(15) 0.0591(16) 0.0580(16) -0.0233(13) 0.0019(12) -0.0273(13) C51 0.0486(14) 0.0717(18) 0.0498(15) 0.0011(13) -0.0163(11) -0.0297(13) C52 0.0517(14) 0.0640(16) 0.0572(15) -0.0005(12) -0.0067(12) -0.0397(13) C53 0.0345(11) 0.0365(12) 0.0469(13) -0.0041(10) 0.0018(9) -0.0043(9) C54 0.0375(13) 0.0713(19) 0.0700(19) -0.0137(15) 0.0156(12) -0.0031(13) C55 0.0590(16) 0.0378(14) 0.0679(18) -0.0008(12) -0.0062(14) 0.0002(12) C56 0.0790(19) 0.0432(14) 0.0563(16) -0.0140(12) -0.0012(14) -0.0199(14) C57 0.0369(11) 0.0443(12) 0.0251(10) 0.0002(9) -0.0015(8) -0.0171(9) C58 0.0739(18) 0.0726(18) 0.0371(13) 0.0078(12) -0.0038(12) -0.0476(15) C59 0.0513(13) 0.0656(16) 0.0258(11) -0.0036(10) -0.0022(9) -0.0303(12) C60 0.0583(16) 0.0605(17) 0.0403(14) 0.0076(12) -0.0094(12) -0.0036(13) C61 0.0280(9) 0.0344(11) 0.0334(10) -0.0035(8) 0.0088(8) -0.0126(8) C62 0.0316(12) 0.0684(18) 0.0742(19) 0.0133(15) 0.0105(12) -0.0111(12) C63 0.089(2) 0.0555(18) 0.106(3) -0.0209(17) 0.061(2) -0.0437(17) C64 0.0591(18) 0.129(3) 0.0474(16) -0.0306(18) 0.0192(13) -0.0401(19) B1 0.0254(10) 0.0292(11) 0.0216(10) -0.0064(8) 0.0008(7) -0.0130(8) B2 0.0215(9) 0.0267(10) 0.0282(10) -0.0051(8) 0.0017(8) -0.0094(8) B3 0.0274(10) 0.0228(10) 0.0232(10) -0.0060(8) 0.0003(8) -0.0075(8) B4 0.0255(10) 0.0300(11) 0.0299(11) -0.0089(9) 0.0001(8) -0.0117(8) C65 0.054(2) 0.078(3) 0.188(6) 0.038(4) 0.000(3) -0.021(2) C66 0.053(2) 0.178(6) 0.093(3) 0.000(4) -0.022(2) 0.014(3) C67 0.067(2) 0.082(3) 0.211(6) -0.054(4) -0.049(3) -0.009(2) C68 0.104(4) 0.130(5) 0.175(6) 0.016(4) -0.004(4) -0.084(3) C69 0.173(6) 0.220(8) 0.121(5) -0.059(5) 0.065(4) -0.119(6) C70 0.138(4) 0.089(3) 0.188(6) -0.072(4) 0.050(4) -0.059(3) C71B 0.37(2) 0.225(17) 0.115(8) 0.029(9) -0.026(12) -0.198(17) C72B 0.167(10) 0.213(13) 0.094(7) -0.020(7) 0.018(7) -0.017(9) C73B 0.144(11) 0.42(3) 0.212(15) 0.156(18) -0.011(10) 0.085(14) C74B 0.25(2) 0.49(3) 0.188(15) 0.152(18) -0.076(15) 0.09(2) C75B 0.25(3) 0.86(6) 0.38(4) -0.19(4) 0.11(3) 0.22(3) C76B 0.28(2) 0.32(2) 0.36(3) -0.21(2) -0.14(2) 0.166(19) C77 0.0588(16) 0.0511(16) 0.0720(19) -0.0072(14) 0.0143(14) -0.0256(13) C78 0.0482(14) 0.0464(14) 0.0704(18) -0.0100(13) -0.0087(13) -0.0165(12) C79 0.0676(18) 0.0512(16) 0.0572(17) 0.0026(13) -0.0025(14) -0.0202(14) C71A 0.157(19) 0.13(2) 0.78(8) -0.23(3) -0.26(4) 0.079(15) C72A 1.4(3) 0.080(18) 0.51(9) -0.06(3) -0.44(13) -0.09(6) C73A 0.24(3) 0.117(16) 0.19(3) 0.107(17) -0.11(2) -0.091(18) C74A 0.21(3) 0.107(13) 0.36(4) -0.104(19) 0.21(3) -0.064(16) C75A 0.088(14) 0.60(9) 0.35(5) -0.24(5) 0.15(2) 0.04(3) C76A 0.124(19) 0.55(7) 1.06(13) -0.73(9) 0.21(4) -0.12(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 Al4 2.6650(8) . . yes Al1 O1 1.8688(15) . . yes Al1 O2 1.9244(13) . . yes Al1 O4 1.8671(14) . . yes Al1 O5 1.8233(13) . . yes Al1 O7 1.8511(13) . . yes Al1 B1 2.376(2) . . yes Al2 O1 1.9400(14) . . yes Al2 O6 1.7612(16) . . yes Al2 C49 1.990(2) . . yes Al2 C53 1.984(2) . . yes Al3 O2 1.8274(14) . . yes Al3 O3 1.7474(15) . . yes Al3 O7 1.8903(14) . . yes Al3 C57 1.959(2) . . yes Al4 O4 1.8732(13) . . yes Al4 O5 1.8555(15) . . yes Al4 O8 1.7590(15) . . yes Al4 C61 1.956(2) . . yes O1 B1 1.401(2) . . yes O2 B1 1.391(3) . . yes O3 B2 1.340(2) . . yes O4 B2 1.440(2) . . yes O5 B3 1.438(3) . . yes O6 B3 1.308(3) . . yes O7 B4 1.440(3) . . yes O8 B4 1.336(3) . . yes C1 C2 1.406(3) . . no C1 C6 1.414(3) . . no C1 B1 1.565(3) . . yes C2 C3 1.396(4) . . no C2 C7 1.529(3) . . no C3 C4 1.376(4) . . no C4 C5 1.372(4) . . no C5 C6 1.392(3) . . no C6 C10 1.520(3) . . no C7 C8 1.529(4) . . no C7 C9 1.540(4) . . no C10 C11 1.530(4) . . no C10 C12 1.517(4) . . no C13 C14 1.417(3) . . no C13 C18 1.418(3) . . no C13 B2 1.576(3) . . yes C14 C15 1.398(3) . . no C14 C19 1.523(3) . . no C15 C16 1.380(4) . . no C16 C17 1.370(4) . . no C17 C18 1.397(3) . . no C18 C22 1.524(3) . . no C19 C20 1.524(4) . . no C19 C21 1.525(3) . . no C22 C23 1.528(3) . . no C22 C24 1.534(4) . . no C25 C26 1.418(3) . . no C25 C30 1.407(3) . . no C25 B3 1.588(3) . . yes C26 C27 1.393(3) . . no C26 C31 1.526(3) . . no C27 C28 1.372(3) . . no C28 C29 1.386(3) . . no C29 C30 1.395(3) . . no C30 C34 1.522(3) . . no C31 C32 1.534(3) . . no C31 C33 1.528(4) . . no C34 C35 1.528(4) . . no C34 C36 1.524(3) . . no C37 C38 1.412(3) . . no C37 C42 1.407(3) . . no C37 B4 1.582(3) . . yes C38 C39 1.394(4) . . no C38 C46 1.524(4) . . no C39 C40 1.363(4) . . no C40 C41 1.376(4) . . no C41 C42 1.398(3) . . no C42 C43 1.518(3) . . no C43 C44 1.522(4) . . no C43 C45 1.511(4) . . no C46 C47 1.532(5) . . no C46 C48 1.484(5) . . no C49 C50 1.531(4) . . no C49 C51 1.542(3) . . no C49 C52 1.531(4) . . no C53 C54 1.539(4) . . no C53 C55 1.545(4) . . no C53 C56 1.534(4) . . no C57 C58 1.549(4) . . no C57 C59 1.534(3) . . no C57 C60 1.536(4) . . no C61 C62 1.520(4) . . no C61 C63 1.521(4) . . no C61 C64 1.529(4) . . no C3 H3 0.9508 . . no C4 H4 0.9500 . . no C5 H5 0.9498 . . no C7 H7 1.0000 . . no C8 H8 0.9797 . . no C8 H8' 0.9800 . . no C8 H8" 0.9804 . . no C9 H9 0.9802 . . no C9 H9' 0.9798 . . no C9 H9" 0.9799 . . no C10 H10 1.0000 . . no C11 H11 0.9798 . . no C11 H11' 0.9804 . . no C11 H11" 0.9801 . . no C12 H12 0.9799 . . no C12 H12' 0.9799 . . no C12 H12" 0.9802 . . no C15 H15 0.9500 . . no C16 H16 0.9501 . . no C17 H17 0.9501 . . no C19 H19 1.0001 . . no C20 H20 0.9801 . . no C20 H20' 0.9800 . . no C20 H20" 0.9801 . . no C21 H21 0.9799 . . no C21 H21' 0.9797 . . no C21 H21" 0.9806 . . no C22 H22 1.0001 . . no C23 H23 0.9799 . . no C23 H23' 0.9798 . . no C23 H23" 0.9804 . . no C24 H24 0.9802 . . no C24 H24' 0.9803 . . no C24 H24" 0.9798 . . no C27 H27 0.9500 . . no C28 H28 0.9500 . . no C29 H29 0.9499 . . no C31 H31 1.0000 . . no C32 H32 0.9796 . . no C32 H32' 0.9796 . . no C32 H32" 0.9803 . . no C33 H33 0.9801 . . no C33 H33' 0.9799 . . no C33 H33" 0.9801 . . no C34 H34 1.0001 . . no C35 H35 0.9805 . . no C35 H35' 0.9803 . . no C35 H35" 0.9798 . . no C36 H36 0.9801 . . no C36 H36' 0.9800 . . no C36 H36" 0.9800 . . no C39 H39 0.9499 . . no C40 H40 0.9499 . . no C41 H41 0.9504 . . no C43 H43 1.0000 . . no C44 H44 0.9803 . . no C44 H44' 0.9796 . . no C44 H44" 0.9803 . . no C45 H45 0.9801 . . no C45 H45' 0.9801 . . no C45 H45" 0.9799 . . no C46 H46 1.0006 . . no C47 H47 0.9800 . . no C47 H47' 0.9803 . . no C47 H47" 0.9797 . . no C48 H48 0.9800 . . no C48 H48' 0.9800 . . no C48 H48" 0.9805 . . no C50 H50 0.9802 . . no C50 H50' 0.9799 . . no C50 H50" 0.9799 . . no C51 H51 0.9801 . . no C51 H51' 0.9798 . . no C51 H51" 0.9805 . . no C52 H52 0.9796 . . no C52 H52' 0.9804 . . no C52 H52" 0.9803 . . no C54 H54 0.9803 . . no C54 H54' 0.9798 . . no C54 H54" 0.9797 . . no C55 H55 0.9810 . . no C55 H55' 0.9793 . . no C55 H55" 0.9803 . . no C56 H56 0.9800 . . no C56 H56' 0.9801 . . no C56 H56" 0.9804 . . no C58 H58 0.9800 . . no C58 H58' 0.9792 . . no C58 H58" 0.9799 . . no C59 H59 0.9799 . . no C59 H59' 0.9799 . . no C59 H59" 0.9801 . . no C60 H60 0.9798 . . no C60 H60' 0.9796 . . no C60 H60" 0.9806 . . no C62 H62 0.9798 . . no C62 H62' 0.9800 . . no C62 H62" 0.9804 . . no C63 H63 0.9797 . . no C63 H63' 0.9800 . . no C63 H63" 0.9798 . . no C64 H64 0.9802 . . no C64 H64' 0.9803 . . no C64 H64" 0.9797 . . no C65 C66 1.404(9) . . no C65 C70 1.292(13) . . no C66 C67 1.391(9) . . no C67 C68 1.248(11) . . no C68 C69 1.292(10) . . no C69 C70 1.324(10) . . no C65 H65 0.9494 . . no C66 H66 0.9504 . . no C67 H67 0.9501 . . no C68 H68 0.9503 . . no C69 H69 0.9494 . . no C70 H70 0.9511 . . no C71B C72B 1.390(10) . . no C71B C76B 1.389(11) . . no C72B C73B 1.390(10) . . no C73B C74B 1.390(11) . . no C74B C75B 1.392(9) . . no C75B C76B 1.390(6) . . no C71B H71B 0.9506 . . no C72B H72B 0.9503 . . no C73B H73B 0.9490 . . no C74B H74B 0.9489 . . no C75B H75B 0.9494 . . no C76B H76B 0.9505 . . no C77 C78 1.365(4) . . no C77 C79 1.371(4) . . no C78 C79 1.367(4) . 2_566 no C77 H77 0.9497 . . no C78 H78 0.9504 . . no C79 H79 0.9501 . . no C71A C72A 1.39(3) . . no C71A C76A 1.39(3) . . no C72A C73A 1.39(2) . . no C73A C74A 1.39(3) . . no C74A C75A 1.39(3) . . no C75A C76A 1.39(3) . . no C71A H71 0.9494 . . no C72A H72 0.9511 . . no C73A H73 0.9511 . . no C74A H74 0.9502 . . no C75A H75 0.9502 . . no C76A H76 0.9506 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Al4 Al1 O1 147.57(4) . . . yes Al4 Al1 O2 138.55(5) . . . yes Al4 Al1 O4 44.65(4) . . . yes Al4 Al1 O5 44.06(5) . . . yes Al4 Al1 O7 85.30(5) . . . yes Al4 Al1 B1 171.42(6) . . . yes O1 Al1 O2 71.86(6) . . . yes O1 Al1 O4 145.24(6) . . . yes O1 Al1 O5 104.00(6) . . . yes O1 Al1 O7 116.00(6) . . . yes O1 Al1 B1 36.11(6) . . . yes O2 Al1 O4 97.24(6) . . . yes O2 Al1 O5 170.85(6) . . . yes O2 Al1 O7 81.48(6) . . . yes O2 Al1 B1 35.85(7) . . . yes O4 Al1 O5 81.54(6) . . . yes O4 Al1 O7 93.89(6) . . . yes O4 Al1 B1 127.08(7) . . . yes O5 Al1 O7 107.63(6) . . . yes O5 Al1 B1 139.92(7) . . . yes O7 Al1 B1 98.52(7) . . . yes O1 Al2 O6 94.56(7) . . . yes O1 Al2 C49 106.53(8) . . . yes O1 Al2 C53 114.94(8) . . . yes O6 Al2 C49 110.79(8) . . . yes O6 Al2 C53 105.98(9) . . . yes C49 Al2 C53 120.87(11) . . . yes O2 Al3 O3 97.69(6) . . . yes O2 Al3 O7 83.03(6) . . . yes O2 Al3 C57 123.29(9) . . . yes O3 Al3 O7 102.75(6) . . . yes O3 Al3 C57 117.73(9) . . . yes O7 Al3 C57 124.81(8) . . . yes Al1 Al4 O4 44.47(4) . . . yes Al1 Al4 O5 43.10(4) . . . yes Al1 Al4 O8 84.15(5) . . . yes Al1 Al4 C61 160.77(7) . . . yes O4 Al4 O5 80.54(6) . . . yes O4 Al4 O8 101.69(6) . . . yes O4 Al4 C61 121.65(8) . . . yes O5 Al4 O8 98.16(7) . . . yes O5 Al4 C61 133.09(8) . . . yes O8 Al4 C61 114.19(9) . . . yes Al1 O1 Al2 126.10(7) . . . yes Al1 O1 B1 92.06(12) . . . yes Al2 O1 B1 139.80(14) . . . yes Al1 O2 Al3 92.52(6) . . . yes Al1 O2 B1 90.05(11) . . . yes Al3 O2 B1 141.53(12) . . . yes Al3 O3 B2 125.92(13) . . . yes Al1 O4 Al4 90.88(6) . . . yes Al1 O4 B2 122.87(11) . . . yes Al4 O4 B2 130.40(13) . . . yes Al1 O5 Al4 92.84(6) . . . yes Al1 O5 B3 128.38(13) . . . yes Al4 O5 B3 134.17(12) . . . yes Al2 O6 B3 146.31(14) . . . yes Al1 O7 Al3 92.88(6) . . . yes Al1 O7 B4 120.77(12) . . . yes Al3 O7 B4 124.18(12) . . . yes Al4 O8 B4 129.56(15) . . . yes C2 C1 C6 119.3(2) . . . no C2 C1 B1 118.14(18) . . . yes C6 C1 B1 122.05(18) . . . yes C1 C2 C3 119.1(2) . . . no C1 C2 C7 122.3(2) . . . no C3 C2 C7 118.6(2) . . . no C2 C3 C4 121.0(2) . . . no C3 C4 C5 120.4(3) . . . no C4 C5 C6 120.7(2) . . . no C1 C6 C5 119.5(2) . . . no C1 C6 C10 120.42(19) . . . no C5 C6 C10 120.0(2) . . . no C2 C7 C8 111.2(2) . . . no C2 C7 C9 111.9(2) . . . no C8 C7 C9 111.0(2) . . . no C6 C10 C11 114.6(2) . . . no C6 C10 C12 112.2(2) . . . no C11 C10 C12 108.8(2) . . . no C14 C13 C18 118.88(18) . . . no C14 C13 B2 120.15(18) . . . yes C18 C13 B2 120.97(17) . . . yes C13 C14 C15 119.6(2) . . . no C13 C14 C19 122.75(18) . . . no C15 C14 C19 117.61(19) . . . no C14 C15 C16 120.7(2) . . . no C15 C16 C17 120.3(2) . . . no C16 C17 C18 121.4(2) . . . no C13 C18 C17 119.14(19) . . . no C13 C18 C22 121.81(18) . . . no C17 C18 C22 119.0(2) . . . no C14 C19 C20 112.85(19) . . . no C14 C19 C21 110.98(19) . . . no C20 C19 C21 110.3(2) . . . no C18 C22 C23 109.87(19) . . . no C18 C22 C24 113.75(18) . . . no C23 C22 C24 110.0(2) . . . no C26 C25 C30 119.13(17) . . . no C26 C25 B3 119.67(17) . . . yes C30 C25 B3 121.03(16) . . . yes C25 C26 C27 119.02(18) . . . no C25 C26 C31 120.97(17) . . . no C27 C26 C31 119.96(17) . . . no C26 C27 C28 121.55(19) . . . no C27 C28 C29 119.9(2) . . . no C28 C29 C30 120.5(2) . . . no C25 C30 C29 119.85(18) . . . no C25 C30 C34 121.54(18) . . . no C29 C30 C34 118.44(18) . . . no C26 C31 C32 113.8(2) . . . no C26 C31 C33 109.86(18) . . . no C32 C31 C33 109.68(19) . . . no C30 C34 C35 112.4(2) . . . no C30 C34 C36 110.75(19) . . . no C35 C34 C36 110.17(19) . . . no C38 C37 C42 119.2(2) . . . no C38 C37 B4 121.0(2) . . . yes C42 C37 B4 119.79(19) . . . yes C37 C38 C39 119.3(2) . . . no C37 C38 C46 121.1(2) . . . no C39 C38 C46 119.6(2) . . . no C38 C39 C40 121.2(2) . . . no C39 C40 C41 120.2(2) . . . no C40 C41 C42 120.9(3) . . . no C37 C42 C41 119.2(2) . . . no C37 C42 C43 121.81(19) . . . no C41 C42 C43 119.0(2) . . . no C42 C43 C44 112.97(19) . . . no C42 C43 C45 110.9(2) . . . no C44 C43 C45 110.2(2) . . . no C38 C46 C47 113.3(2) . . . no C38 C46 C48 109.8(3) . . . no C47 C46 C48 110.0(3) . . . no Al2 C49 C50 108.86(17) . . . yes Al2 C49 C51 110.02(16) . . . yes Al2 C49 C52 113.67(15) . . . yes C50 C49 C51 107.90(19) . . . no C50 C49 C52 109.3(2) . . . no C51 C49 C52 106.9(2) . . . no Al2 C53 C54 114.50(16) . . . yes Al2 C53 C55 105.74(16) . . . yes Al2 C53 C56 112.52(17) . . . yes C54 C53 C55 106.8(2) . . . no C54 C53 C56 109.9(2) . . . no C55 C53 C56 106.8(2) . . . no Al3 C57 C58 110.96(16) . . . yes Al3 C57 C59 113.73(15) . . . yes Al3 C57 C60 107.38(15) . . . yes C58 C57 C59 108.79(19) . . . no C58 C57 C60 107.5(2) . . . no C59 C57 C60 108.3(2) . . . no Al4 C61 C62 106.38(15) . . . yes Al4 C61 C63 110.04(18) . . . yes Al4 C61 C64 116.05(18) . . . yes C62 C61 C63 109.3(2) . . . no C62 C61 C64 108.5(2) . . . no C63 C61 C64 106.5(2) . . . no C2 C3 H3 119.53 . . . no C4 C3 H3 119.49 . . . no C3 C4 H4 119.85 . . . no C5 C4 H4 119.79 . . . no C4 C5 H5 119.63 . . . no C6 C5 H5 119.70 . . . no C2 C7 H7 107.50 . . . no C8 C7 H7 107.53 . . . no C9 C7 H7 107.52 . . . no C7 C8 H8 109.50 . . . no C7 C8 H8' 109.47 . . . no C7 C8 H8" 109.46 . . . no H8 C8 H8' 109.50 . . . no H8 C8 H8" 109.47 . . . no H8' C8 H8" 109.43 . . . no C7 C9 H9' 109.47 . . . no C7 C9 H9" 109.48 . . . no H9 C9 H9' 109.47 . . . no H9 C9 H9" 109.46 . . . no H9' C9 H9" 109.49 . . . no C7 C9 H9 109.46 . . . no C11 C10 H10 106.95 . . . no C12 C10 H10 106.92 . . . no C6 C10 H10 106.93 . . . no C10 C11 H11' 109.48 . . . no C10 C11 H11" 109.49 . . . no H11 C11 H11' 109.45 . . . no H11 C11 H11" 109.47 . . . no H11' C11 H11" 109.44 . . . no C10 C11 H11 109.50 . . . no C10 C12 H12 109.47 . . . no C10 C12 H12' 109.47 . . . no C10 C12 H12" 109.45 . . . no H12 C12 H12' 109.50 . . . no H12 C12 H12" 109.47 . . . no H12' C12 H12" 109.47 . . . no C14 C15 H15 119.66 . . . no C16 C15 H15 119.67 . . . no C15 C16 H16 119.88 . . . no C17 C16 H16 119.87 . . . no C16 C17 H17 119.30 . . . no C18 C17 H17 119.29 . . . no C14 C19 H19 107.47 . . . no C20 C19 H19 107.47 . . . no C21 C19 H19 107.48 . . . no C19 C20 H20 109.47 . . . no H20 C20 H20' 109.48 . . . no H20 C20 H20" 109.47 . . . no H20' C20 H20" 109.46 . . . no C19 C20 H20" 109.47 . . . no C19 C20 H20' 109.47 . . . no C19 C21 H21' 109.52 . . . no C19 C21 H21 109.50 . . . no H21 C21 H21" 109.42 . . . no C19 C21 H21" 109.45 . . . no H21 C21 H21' 109.50 . . . no H21' C21 H21" 109.44 . . . no C23 C22 H22 107.69 . . . no C24 C22 H22 107.68 . . . no C18 C22 H22 107.68 . . . no C22 C23 H23" 109.46 . . . no C22 C23 H23 109.49 . . . no C22 C23 H23' 109.49 . . . no H23 C23 H23' 109.49 . . . no H23 C23 H23" 109.45 . . . no H23' C23 H23" 109.45 . . . no C22 C24 H24 109.47 . . . no C22 C24 H24' 109.47 . . . no C22 C24 H24" 109.49 . . . no H24 C24 H24' 109.45 . . . no H24 C24 H24" 109.47 . . . no H24' C24 H24" 109.48 . . . no C26 C27 H27 119.23 . . . no C28 C27 H27 119.23 . . . no C27 C28 H28 120.04 . . . no C29 C28 H28 120.05 . . . no C28 C29 H29 119.72 . . . no C30 C29 H29 119.74 . . . no C32 C31 H31 107.77 . . . no C33 C31 H31 107.79 . . . no C26 C31 H31 107.78 . . . no C31 C32 H32' 109.46 . . . no C31 C32 H32" 109.42 . . . no C31 C32 H32 109.47 . . . no H32 C32 H32" 109.47 . . . no H32' C32 H32" 109.48 . . . no H32 C32 H32' 109.53 . . . no C31 C33 H33' 109.48 . . . no C31 C33 H33" 109.47 . . . no H33 C33 H33' 109.48 . . . no H33 C33 H33" 109.47 . . . no H33' C33 H33" 109.46 . . . no C31 C33 H33 109.47 . . . no C30 C34 H34 107.78 . . . no C35 C34 H34 107.78 . . . no C36 C34 H34 107.79 . . . no C34 C35 H35 109.49 . . . no C34 C35 H35' 109.50 . . . no C34 C35 H35" 109.53 . . . no H35 C35 H35' 109.40 . . . no H35 C35 H35" 109.43 . . . no H35' C35 H35" 109.47 . . . no C34 C36 H36 109.47 . . . no C34 C36 H36' 109.47 . . . no C34 C36 H36" 109.48 . . . no H36 C36 H36' 109.47 . . . no H36 C36 H36" 109.47 . . . no H36' C36 H36" 109.47 . . . no C38 C39 H39 119.39 . . . no C40 C39 H39 119.43 . . . no C39 C40 H40 119.90 . . . no C41 C40 H40 119.89 . . . no C42 C41 H41 119.57 . . . no C40 C41 H41 119.50 . . . no C45 C43 H43 107.50 . . . no C44 C43 H43 107.50 . . . no C42 C43 H43 107.51 . . . no C43 C44 H44 109.47 . . . no C43 C44 H44' 109.52 . . . no C43 C44 H44" 109.48 . . . no H44' C44 H44" 109.46 . . . no H44 C44 H44' 109.48 . . . no H44 C44 H44" 109.41 . . . no C43 C45 H45 109.47 . . . no C43 C45 H45' 109.47 . . . no C43 C45 H45" 109.48 . . . no H45 C45 H45' 109.45 . . . no H45 C45 H45" 109.47 . . . no H45' C45 H45" 109.48 . . . no C38 C46 H46 107.86 . . . no C47 C46 H46 107.82 . . . no C48 C46 H46 107.86 . . . no C46 C47 H47 109.49 . . . no C46 C47 H47' 109.46 . . . no C46 C47 H47" 109.47 . . . no H47 C47 H47' 109.45 . . . no H47 C47 H47" 109.50 . . . no H47' C47 H47" 109.46 . . . no C46 C48 H48 109.49 . . . no C46 C48 H48' 109.54 . . . no C46 C48 H48" 109.46 . . . no H48 C48 H48' 109.47 . . . no H48' C48 H48" 109.44 . . . no H48 C48 H48" 109.43 . . . no C49 C50 H50' 109.48 . . . no C49 C50 H50" 109.48 . . . no H50 C50 H50' 109.47 . . . no H50 C50 H50" 109.45 . . . no H50' C50 H50" 109.49 . . . no C49 C50 H50 109.45 . . . no C49 C51 H51 109.48 . . . no C49 C51 H51" 109.46 . . . no H51 C51 H51' 109.49 . . . no H51 C51 H51" 109.43 . . . no H51' C51 H51" 109.46 . . . no C49 C51 H51' 109.50 . . . no C49 C52 H52 109.52 . . . no C49 C52 H52' 109.47 . . . no C49 C52 H52" 109.48 . . . no H52 C52 H52' 109.47 . . . no H52 C52 H52" 109.48 . . . no H52' C52 H52" 109.41 . . . no C53 C54 H54 109.44 . . . no C53 C54 H54' 109.47 . . . no C53 C54 H54" 109.48 . . . no H54 C54 H54' 109.45 . . . no H54 C54 H54" 109.47 . . . no H54' C54 H54" 109.51 . . . no C53 C55 H55 109.45 . . . no C53 C55 H55' 109.55 . . . no C53 C55 H55" 109.49 . . . no H55 C55 H55' 109.46 . . . no H55 C55 H55" 109.37 . . . no H55' C55 H55" 109.51 . . . no C53 C56 H56" 109.48 . . . no H56 C56 H56' 109.47 . . . no H56 C56 H56" 109.44 . . . no H56' C56 H56" 109.43 . . . no C53 C56 H56' 109.51 . . . no C53 C56 H56 109.51 . . . no C57 C58 H58" 109.41 . . . no C57 C58 H58 109.40 . . . no C57 C58 H58' 109.45 . . . no H58' C58 H58" 109.55 . . . no H58 C58 H58' 109.54 . . . no H58 C58 H58" 109.48 . . . no C57 C59 H59 109.47 . . . no H59 C59 H59' 109.49 . . . no C57 C59 H59' 109.46 . . . no C57 C59 H59" 109.45 . . . no H59 C59 H59" 109.49 . . . no H59' C59 H59" 109.47 . . . no C57 C60 H60 109.48 . . . no C57 C60 H60' 109.50 . . . no C57 C60 H60" 109.44 . . . no H60 C60 H60' 109.52 . . . no H60 C60 H60" 109.43 . . . no H60' C60 H60" 109.46 . . . no C61 C62 H62 109.49 . . . no C61 C62 H62' 109.48 . . . no C61 C62 H62" 109.46 . . . no H62 C62 H62' 109.48 . . . no H62 C62 H62" 109.47 . . . no H62' C62 H62" 109.45 . . . no C61 C63 H63 109.43 . . . no C61 C63 H63" 109.45 . . . no H63 C63 H63' 109.50 . . . no H63 C63 H63" 109.53 . . . no H63' C63 H63" 109.49 . . . no C61 C63 H63' 109.42 . . . no C61 C64 H64 109.48 . . . no C61 C64 H64" 109.50 . . . no H64 C64 H64' 109.42 . . . no C61 C64 H64' 109.46 . . . no H64' C64 H64" 109.48 . . . no H64 C64 H64" 109.48 . . . no C66 C65 C70 118.0(6) . . . no C65 C66 C67 116.9(6) . . . no C66 C67 C68 119.9(6) . . . no C67 C68 C69 123.2(7) . . . no C68 C69 C70 120.2(7) . . . no C65 C70 C69 121.7(6) . . . no C66 C65 H65 121.02 . . . no C70 C65 H65 120.96 . . . no C65 C66 H66 121.49 . . . no C67 C66 H66 121.56 . . . no C66 C67 H67 120.08 . . . no C68 C67 H67 120.05 . . . no C67 C68 H68 118.43 . . . no C69 C68 H68 118.40 . . . no C68 C69 H69 119.85 . . . no C70 C69 H69 119.94 . . . no C65 C70 H70 119.19 . . . no C69 C70 H70 119.06 . . . no C72B C71B C76B 120.0(5) . . . no C71B C72B C73B 120.0(7) . . . no C72B C73B C74B 120.0(7) . . . no C73B C74B C75B 120.0(5) . . . no C74B C75B C76B 120.0(6) . . . no C71B C76B C75B 120.0(6) . . . no C76B C71B H71B 119.98 . . . no C72B C71B H71B 120.02 . . . no C71B C72B H72B 119.95 . . . no C73B C72B H72B 120.03 . . . no C74B C73B H73B 120.03 . . . no C72B C73B H73B 119.97 . . . no C73B C74B H74B 120.04 . . . no C75B C74B H74B 119.97 . . . no C74B C75B H75B 119.98 . . . no C76B C75B H75B 120.06 . . . no C71B C76B H76B 120.03 . . . no C75B C76B H76B 119.94 . . . no C78 C77 C79 120.4(3) . . . no C77 C78 C79 119.5(3) . . 2_566 no C77 C79 C78 120.1(3) . . 2_566 no C78 C77 H77 119.79 . . . no C79 C77 H77 119.78 . . . no C77 C78 H78 120.25 . . . no C79 C78 H78 120.29 2_566 . . no C77 C79 H79 119.92 . . . no C78 C79 H79 119.96 2_566 . . no C72A C71A C76A 119.9(17) . . . no C71A C72A C73A 120.1(17) . . . no C72A C73A C74A 120.0(17) . . . no C73A C74A C75A 120.0(16) . . . no C74A C75A C76A 120.0(18) . . . no C71A C76A C75A 120.0(17) . . . no C72A C71A H71 120.09 . . . no C76A C71A H71 120.02 . . . no C71A C72A H72 119.90 . . . no C73A C72A H72 120.02 . . . no C74A C73A H73 119.92 . . . no C72A C73A H73 120.05 . . . no C75A C74A H74 120.02 . . . no C73A C74A H74 120.01 . . . no C74A C75A H75 120.07 . . . no C76A C75A H75 119.92 . . . no C71A C76A H76 119.95 . . . no C75A C76A H76 120.03 . . . no Al1 B1 O1 51.83(9) . . . yes Al1 B1 O2 54.10(9) . . . yes Al1 B1 C1 173.62(15) . . . yes O1 B1 O2 105.75(17) . . . yes O1 B1 C1 133.03(19) . . . yes O2 B1 C1 121.22(17) . . . yes O4 B2 C13 118.92(15) . . . yes O3 B2 C13 124.17(17) . . . yes O3 B2 O4 116.91(16) . . . yes O5 B3 C25 118.94(18) . . . yes O6 B3 C25 123.47(18) . . . yes O5 B3 O6 117.59(17) . . . yes O8 B4 C37 124.0(2) . . . yes O7 B4 O8 117.19(18) . . . yes O7 B4 C37 118.74(18) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 Al4 O4 125.93(10) . . . . no O1 Al1 Al4 O5 -12.23(10) . . . . no O1 Al1 Al4 O8 -120.79(10) . . . . no O2 Al1 Al4 O4 -28.91(8) . . . . no O2 Al1 Al4 O5 -167.06(9) . . . . no O2 Al1 Al4 O8 84.38(8) . . . . no O4 Al1 Al4 O5 -138.16(8) . . . . no O4 Al1 Al4 O8 113.28(7) . . . . no O5 Al1 Al4 O4 138.16(8) . . . . no O5 Al1 Al4 O8 -108.56(8) . . . . no O7 Al1 Al4 O4 -100.38(7) . . . . no O7 Al1 Al4 O5 121.47(7) . . . . no O7 Al1 Al4 O8 12.91(7) . . . . no Al4 Al1 O1 Al2 0.25(14) . . . . no Al4 Al1 O1 B1 -166.20(10) . . . . no O2 Al1 O1 Al2 163.02(9) . . . . no O2 Al1 O1 B1 -3.43(10) . . . . no O4 Al1 O1 Al2 86.89(12) . . . . no O4 Al1 O1 B1 -79.57(14) . . . . no O5 Al1 O1 Al2 -8.48(9) . . . . no O5 Al1 O1 B1 -174.93(10) . . . . no O7 Al1 O1 Al2 -126.45(8) . . . . no O7 Al1 O1 B1 67.10(11) . . . . no B1 Al1 O1 Al2 166.45(15) . . . . no Al4 Al1 O2 Al3 -48.83(8) . . . . no Al4 Al1 O2 B1 169.57(9) . . . . no O1 Al1 O2 Al3 145.06(6) . . . . no O1 Al1 O2 B1 3.45(10) . . . . no O4 Al1 O2 Al3 -68.85(6) . . . . no O4 Al1 O2 B1 149.54(10) . . . . no O7 Al1 O2 Al3 24.02(6) . . . . no O7 Al1 O2 B1 -117.59(11) . . . . no B1 Al1 O2 Al3 141.61(12) . . . . no Al4 Al1 O4 B2 -141.41(16) . . . . no O1 Al1 O4 Al4 -130.38(9) . . . . no O1 Al1 O4 B2 88.21(16) . . . . no O2 Al1 O4 Al4 161.18(5) . . . . no O2 Al1 O4 B2 19.77(14) . . . . no O5 Al1 O4 Al4 -27.97(6) . . . . no O5 Al1 O4 B2 -169.38(14) . . . . no O7 Al1 O4 Al4 79.29(6) . . . . no O7 Al1 O4 B2 -62.12(14) . . . . no B1 Al1 O4 Al4 -176.97(7) . . . . no B1 Al1 O4 B2 41.62(17) . . . . no Al4 Al1 O5 B3 -158.29(16) . . . . no O1 Al1 O5 Al4 173.28(5) . . . . no O1 Al1 O5 B3 14.98(15) . . . . no O4 Al1 O5 Al4 28.29(6) . . . . no O4 Al1 O5 B3 -130.00(14) . . . . no O7 Al1 O5 Al4 -63.12(7) . . . . no O7 Al1 O5 B3 138.58(14) . . . . no B1 Al1 O5 Al4 168.64(9) . . . . no B1 Al1 O5 B3 10.35(19) . . . . no Al4 Al1 O7 Al3 117.42(5) . . . . no Al4 Al1 O7 B4 -15.79(14) . . . . no O1 Al1 O7 Al3 -88.14(7) . . . . no O1 Al1 O7 B4 138.65(14) . . . . no O2 Al1 O7 Al3 -23.18(6) . . . . no O2 Al1 O7 B4 -156.39(15) . . . . no O4 Al1 O7 Al3 73.56(6) . . . . no O4 Al1 O7 B4 -59.65(14) . . . . no O5 Al1 O7 Al3 155.91(6) . . . . no O5 Al1 O7 B4 22.70(15) . . . . no B1 Al1 O7 Al3 -54.84(7) . . . . no B1 Al1 O7 B4 171.95(14) . . . . no O1 Al1 B1 O2 -174.43(16) . . . . no O2 Al1 B1 O1 174.43(16) . . . . no O4 Al1 B1 O1 135.36(10) . . . . no O4 Al1 B1 O2 -39.07(13) . . . . no O5 Al1 B1 O1 7.65(15) . . . . no O5 Al1 B1 O2 -166.78(10) . . . . no O7 Al1 B1 O1 -123.16(10) . . . . no O7 Al1 B1 O2 62.41(10) . . . . no O6 Al2 O1 Al1 -2.09(9) . . . . no O6 Al2 O1 B1 156.64(18) . . . . no C49 Al2 O1 Al1 -115.36(10) . . . . no C49 Al2 O1 B1 43.4(2) . . . . no C53 Al2 O1 Al1 107.88(11) . . . . no C53 Al2 O1 B1 -93.38(19) . . . . no O1 Al2 O6 B3 19.7(3) . . . . no C49 Al2 O6 B3 129.3(3) . . . . no C53 Al2 O6 B3 -97.8(3) . . . . no O1 Al2 C49 C50 53.91(16) . . . . no O1 Al2 C49 C51 171.95(15) . . . . no O1 Al2 C49 C52 -68.15(19) . . . . no O6 Al2 C49 C50 -47.71(17) . . . . no O6 Al2 C49 C51 70.34(18) . . . . no O6 Al2 C49 C52 -169.77(16) . . . . no C53 Al2 C49 C50 -172.46(15) . . . . no C53 Al2 C49 C51 -54.42(19) . . . . no C53 Al2 C49 C52 65.5(2) . . . . no O1 Al2 C53 C54 91.44(19) . . . . no O1 Al2 C53 C55 -151.21(16) . . . . no O1 Al2 C53 C56 -35.02(19) . . . . no O6 Al2 C53 C54 -165.60(17) . . . . no O6 Al2 C53 C55 -48.25(19) . . . . no O6 Al2 C53 C56 67.94(18) . . . . no C49 Al2 C53 C54 -38.6(2) . . . . no C49 Al2 C53 C55 78.72(19) . . . . no C49 Al2 C53 C56 -165.09(16) . . . . no O3 Al3 O2 Al1 78.59(6) . . . . no O3 Al3 O2 B1 171.85(19) . . . . no O7 Al3 O2 Al1 -23.40(5) . . . . no O7 Al3 O2 B1 69.86(19) . . . . no C57 Al3 O2 Al1 -150.83(9) . . . . no C57 Al3 O2 B1 -57.6(2) . . . . no O2 Al3 O3 B2 -38.98(17) . . . . no O7 Al3 O3 B2 45.57(17) . . . . no C57 Al3 O3 B2 -173.15(16) . . . . no O2 Al3 O7 Al1 24.40(6) . . . . no O2 Al3 O7 B4 155.20(14) . . . . no O3 Al3 O7 Al1 -71.96(7) . . . . no O3 Al3 O7 B4 58.85(15) . . . . no C57 Al3 O7 Al1 150.45(10) . . . . no C57 Al3 O7 B4 -78.75(17) . . . . no O2 Al3 C57 C58 -7.3(2) . . . . no O2 Al3 C57 C59 115.76(18) . . . . no O2 Al3 C57 C60 -124.50(16) . . . . no O3 Al3 C57 C58 114.47(16) . . . . no O3 Al3 C57 C59 -122.49(17) . . . . no O3 Al3 C57 C60 -2.7(2) . . . . no O7 Al3 C57 C58 -113.52(16) . . . . no O7 Al3 C57 C59 9.5(2) . . . . no O7 Al3 C57 C60 129.26(15) . . . . no Al1 Al4 O4 B2 136.54(16) . . . . no O5 Al4 O4 Al1 27.53(5) . . . . no O5 Al4 O4 B2 164.07(15) . . . . no O8 Al4 O4 Al1 -68.93(7) . . . . no O8 Al4 O4 B2 67.61(15) . . . . no C61 Al4 O4 Al1 162.82(8) . . . . no C61 Al4 O4 B2 -60.64(17) . . . . no Al1 Al4 O5 B3 156.16(18) . . . . no O4 Al4 O5 Al1 -28.28(5) . . . . no O4 Al4 O5 B3 127.88(16) . . . . no O8 Al4 O5 Al1 72.30(7) . . . . no O8 Al4 O5 B3 -131.53(16) . . . . no C61 Al4 O5 Al1 -153.20(10) . . . . no C61 Al4 O5 B3 3.0(2) . . . . no Al1 Al4 O8 B4 -12.68(18) . . . . no O4 Al4 O8 B4 28.40(19) . . . . no O5 Al4 O8 B4 -53.55(19) . . . . no C61 Al4 O8 B4 161.27(18) . . . . no O4 Al4 C61 C62 56.70(18) . . . . no O4 Al4 C61 C63 174.94(18) . . . . no O4 Al4 C61 C64 -64.1(2) . . . . no O5 Al4 C61 C62 164.88(13) . . . . no O5 Al4 C61 C63 -76.9(2) . . . . no O5 Al4 C61 C64 44.1(2) . . . . no O8 Al4 C61 C62 -65.84(17) . . . . no O8 Al4 C61 C63 52.4(2) . . . . no O8 Al4 C61 C64 173.41(19) . . . . no Al1 O1 B1 O2 4.69(14) . . . . no Al1 O1 B1 C1 -174.6(2) . . . . no Al2 O1 B1 Al1 -162.95(18) . . . . no Al2 O1 B1 O2 -158.26(12) . . . . no Al2 O1 B1 C1 22.5(3) . . . . no Al1 O2 B1 O1 -4.55(13) . . . . no Al1 O2 B1 C1 174.80(17) . . . . no Al3 O2 B1 Al1 -94.12(17) . . . . no Al3 O2 B1 O1 -98.67(19) . . . . no Al3 O2 B1 C1 80.7(3) . . . . no Al3 O3 B2 O4 -20.0(3) . . . . no Al3 O3 B2 C13 159.32(15) . . . . no Al1 O4 B2 O3 29.2(2) . . . . no Al1 O4 B2 C13 -150.13(14) . . . . no Al4 O4 B2 O3 -95.8(2) . . . . no Al4 O4 B2 C13 84.8(2) . . . . no Al1 O5 B3 O6 -6.9(2) . . . . no Al1 O5 B3 C25 172.65(12) . . . . no Al4 O5 B3 O6 -155.95(13) . . . . no Al4 O5 B3 C25 23.6(3) . . . . no Al2 O6 B3 O5 -16.8(4) . . . . no Al2 O6 B3 C25 163.66(17) . . . . no Al1 O7 B4 O8 12.6(2) . . . . no Al1 O7 B4 C37 -169.19(14) . . . . no Al3 O7 B4 O8 -105.75(18) . . . . no Al3 O7 B4 C37 72.4(2) . . . . no Al4 O8 B4 O7 4.8(3) . . . . no Al4 O8 B4 C37 -173.31(15) . . . . no C6 C1 C2 C3 1.0(3) . . . . no C6 C1 C2 C7 -178.4(2) . . . . no B1 C1 C2 C3 -171.3(2) . . . . no B1 C1 C2 C7 9.4(3) . . . . no C2 C1 C6 C5 -1.9(3) . . . . no C2 C1 C6 C10 -179.4(2) . . . . no B1 C1 C6 C5 170.0(2) . . . . no B1 C1 C6 C10 -7.5(3) . . . . no C2 C1 B1 O1 -123.2(2) . . . . no C2 C1 B1 O2 57.7(3) . . . . no C6 C1 B1 O1 64.8(3) . . . . no C6 C1 B1 O2 -114.4(2) . . . . no C1 C2 C3 C4 0.5(4) . . . . no C7 C2 C3 C4 179.9(3) . . . . no C1 C2 C7 C8 -110.6(3) . . . . no C1 C2 C7 C9 124.6(2) . . . . no C3 C2 C7 C8 70.0(3) . . . . no C3 C2 C7 C9 -54.7(3) . . . . no C2 C3 C4 C5 -1.1(5) . . . . no C3 C4 C5 C6 0.1(4) . . . . no C4 C5 C6 C1 1.4(4) . . . . no C4 C5 C6 C10 178.9(2) . . . . no C1 C6 C10 C11 -158.0(2) . . . . no C1 C6 C10 C12 77.3(3) . . . . no C5 C6 C10 C11 24.6(3) . . . . no C5 C6 C10 C12 -100.2(3) . . . . no C18 C13 C14 C15 1.6(3) . . . . no C18 C13 C14 C19 -177.14(18) . . . . no B2 C13 C14 C15 -179.26(19) . . . . no B2 C13 C14 C19 2.0(3) . . . . no C14 C13 C18 C17 -1.6(3) . . . . no C14 C13 C18 C22 176.53(18) . . . . no B2 C13 C18 C17 179.25(19) . . . . no B2 C13 C18 C22 -2.6(3) . . . . no C14 C13 B2 O3 -124.8(2) . . . . no C14 C13 B2 O4 54.5(3) . . . . no C18 C13 B2 O3 54.3(3) . . . . no C18 C13 B2 O4 -126.3(2) . . . . no C13 C14 C15 C16 -0.4(3) . . . . no C19 C14 C15 C16 178.4(2) . . . . no C13 C14 C19 C20 130.1(2) . . . . no C13 C14 C19 C21 -105.5(2) . . . . no C15 C14 C19 C20 -48.7(3) . . . . no C15 C14 C19 C21 75.8(2) . . . . no C14 C15 C16 C17 -0.8(4) . . . . no C15 C16 C17 C18 0.8(4) . . . . no C16 C17 C18 C13 0.4(3) . . . . no C16 C17 C18 C22 -177.7(2) . . . . no C13 C18 C22 C23 -94.8(2) . . . . no C13 C18 C22 C24 141.4(2) . . . . no C17 C18 C22 C23 83.3(3) . . . . no C17 C18 C22 C24 -40.4(3) . . . . no C30 C25 C26 C27 -1.3(3) . . . . no C30 C25 C26 C31 176.2(2) . . . . no B3 C25 C26 C27 -176.6(2) . . . . no B3 C25 C26 C31 0.9(3) . . . . no C26 C25 C30 C29 0.6(3) . . . . no C26 C25 C30 C34 -174.6(2) . . . . no B3 C25 C30 C29 175.9(2) . . . . no B3 C25 C30 C34 0.7(3) . . . . no C26 C25 B3 O5 -111.9(2) . . . . no C26 C25 B3 O6 67.7(3) . . . . no C30 C25 B3 O5 72.8(3) . . . . no C30 C25 B3 O6 -107.6(2) . . . . no C25 C26 C27 C28 1.0(3) . . . . no C31 C26 C27 C28 -176.5(2) . . . . no C25 C26 C31 C32 142.3(2) . . . . no C25 C26 C31 C33 -94.3(2) . . . . no C27 C26 C31 C32 -40.3(3) . . . . no C27 C26 C31 C33 83.1(2) . . . . no C26 C27 C28 C29 -0.2(4) . . . . no C27 C28 C29 C30 -0.5(4) . . . . no C28 C29 C30 C25 0.3(4) . . . . no C28 C29 C30 C34 175.6(2) . . . . no C25 C30 C34 C35 -134.1(2) . . . . no C25 C30 C34 C36 102.2(2) . . . . no C29 C30 C34 C35 50.7(3) . . . . no C29 C30 C34 C36 -73.0(3) . . . . no C42 C37 C38 C39 -0.8(3) . . . . no C42 C37 C38 C46 -177.4(2) . . . . no B4 C37 C38 C39 178.6(2) . . . . no B4 C37 C38 C46 2.0(3) . . . . no C38 C37 C42 C41 0.1(3) . . . . no C38 C37 C42 C43 179.6(2) . . . . no B4 C37 C42 C41 -179.3(2) . . . . no B4 C37 C42 C43 0.2(3) . . . . no C38 C37 B4 O7 66.4(3) . . . . no C38 C37 B4 O8 -115.6(3) . . . . no C42 C37 B4 O7 -114.2(2) . . . . no C42 C37 B4 O8 63.8(3) . . . . no C37 C38 C39 C40 0.4(4) . . . . no C46 C38 C39 C40 177.1(2) . . . . no C37 C38 C46 C47 -152.4(3) . . . . no C37 C38 C46 C48 84.2(3) . . . . no C39 C38 C46 C47 31.0(4) . . . . no C39 C38 C46 C48 -92.4(3) . . . . no C38 C39 C40 C41 0.6(4) . . . . no C39 C40 C41 C42 -1.2(4) . . . . no C40 C41 C42 C37 0.9(4) . . . . no C40 C41 C42 C43 -178.6(2) . . . . no C37 C42 C43 C44 136.3(2) . . . . no C37 C42 C43 C45 -99.4(3) . . . . no C41 C42 C43 C44 -44.2(3) . . . . no C41 C42 C43 C45 80.1(3) . . . . no C70 C65 C66 C67 -0.3(8) . . . . no C66 C65 C70 C69 -0.9(9) . . . . no C65 C66 C67 C68 0.3(9) . . . . no C66 C67 C68 C69 0.9(10) . . . . no C67 C68 C69 C70 -2.1(12) . . . . no C68 C69 C70 C65 2.1(11) . . . . no C76B C71B C72B C73B 0.0(14) . . . . no C72B C71B C76B C75B -0.1(13) . . . . no C71B C72B C73B C74B 0.1(16) . . . . no C72B C73B C74B C75B 0.0(16) . . . . no C73B C74B C75B C76B 0.0(13) . . . . no C74B C75B C76B C71B 0.1(13) . . . . no C79 C77 C78 C79 0.0(4) . . . 2_566 no C78 C77 C79 C78 0.0(4) . . . 2_566 no C77 C78 C79 C77 0.0(4) . . 2_566 2_566 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Al4 C30 4.040(2) . . no Al1 H19 3.3093 . . no Al2 H10 3.2525 . . no Al3 H12 3.1383 . . no Al3 H43 3.5238 . . no Al3 H8" 3.5272 . . no Al4 H21" 3.5077 . . no O1 C10 3.412(3) . . no O2 C7 3.173(3) . . no O3 C22 3.161(3) . . no O3 C23 3.376(3) . . no O4 C19 3.133(2) . . no O5 C34 3.404(2) . . no O6 C31 3.285(2) . . no O6 C33 3.405(3) . . no O7 C46 3.299(3) . . no O8 C43 3.255(3) . . no O1 H10 2.7158 . . no O2 H7 2.5708 . . no O3 H22 2.5750 . . no O3 H23" 2.7539 . . no O4 H21" 2.8874 . . no O4 H19 2.5067 . . no O5 H34 2.6289 . . no O6 H50' 2.8732 . . no O6 H31 2.7828 . . no O6 H33" 2.7303 . . no O6 H55 2.6777 . . no O7 H46 2.5209 . . no O8 H43 2.6746 . . no O8 H45" 2.8838 . . no C7 O2 3.173(3) . . no C10 O1 3.412(3) . . no C12 B1 3.328(4) . . no C19 O4 3.133(2) . . no C22 O3 3.161(3) . . no C23 O3 3.376(3) . . no C30 Al4 4.040(2) . . no C31 O6 3.285(2) . . no C33 O6 3.405(3) . . no C34 O5 3.404(2) . . no C43 O8 3.255(3) . . no C46 O7 3.299(3) . . no C47 C75B 3.359(8) . . no C48 B4 3.492(5) . . no C75B C47 3.359(8) . . no C1 H12 2.9937 . . no C1 H52 2.7364 . . no C2 H52 2.9130 . . no C3 H9" 2.7977 . . no C3 H8 2.8690 . . no C5 H11 2.7559 . . no C5 H11" 2.9254 . . no C8 H3 3.0396 . . no C9 H3 2.8233 . . no C10 H54" 2.8288 . . no C10 H56' 2.9026 . . no C11 H54" 2.7633 . . no C11 H5 2.5550 . . no C12 H58 2.8690 . . no C12 H59' 2.9913 . . no C13 H65 3.0649 . 1_565 no C13 H62" 2.9042 . . no C15 H20" 2.7604 . . no C15 H21 2.9046 . . no C17 H24" 2.7774 . . no C17 H24 3.0495 . . no C17 H23 3.0029 . . no C18 H62" 2.8423 . . no C20 H15 2.7301 . . no C21 H31 3.0847 . . no C21 H15 3.0894 . . no C23 H74B 3.0081 . 2_576 no C24 H17 2.6606 . . no C25 H64' 3.0935 . . no C26 H64' 2.7471 . . no C27 H33 3.0420 . . no C27 H32" 2.8540 . . no C27 H32 3.0010 . . no C28 H16 2.9966 . 2_576 no C29 H35 2.7088 . . no C29 H36" 2.9128 . . no C30 H63' 3.0024 . . no C31 H64' 3.0514 . . no C32 H64' 2.9751 . . no C32 H27 2.6794 . . no C33 H51' 2.9829 . . no C35 H48 2.9084 . . no C35 H29 2.7394 . . no C36 H29 3.0996 . . no C37 H59 2.9270 . . no C37 H48 2.9898 . . no C39 H47' 2.8700 . . no C39 H47" 2.8033 . . no C40 H68 3.0668 . . no C41 H68 3.0584 . . no C41 H44 2.7259 . . no C41 H45 2.9814 . . no C42 H59 2.9821 . . no C44 H41 2.6929 . . no C45 H52' 3.0156 . 2_576 no C47 H39 2.5617 . . no C47 H75B 2.6319 . . no C47 H12' 2.8144 . . no C48 H35' 2.9038 . . no C50 H21' 3.0459 . . no C51 H55' 3.0475 . . no C52 H9 3.0839 . . no C52 H45' 3.0429 . 1_655 no C53 H10 3.0257 . . no C54 H52' 3.0614 . . no C54 H10 2.9338 . . no C56 H10 2.9099 . . no C59 H11 3.0738 . 2_675 no C60 H73B 3.0622 . 2_576 no C62 H24 2.9780 . . no C63 H35" 3.0655 . . no C64 H32 2.8369 . . no C69 H71 3.0827 . 1_545 no C72A H69 3.0923 . 2_665 no C73A H58" 3.0148 . 2_675 no C74B H23' 3.0816 . 2_665 no C75B H47 2.8055 . . no C75B H47" 3.0538 . . no B1 C12 3.328(4) . . no B4 C48 3.492(5) . . no B1 H12 2.7180 . . no B1 H7 2.4449 . . no B1 H10 2.7158 . . no B2 H19 2.5144 . . no B2 H22 2.5499 . . no B3 H31 2.5090 . . no B3 H34 2.5041 . . no B4 H48 2.9657 . . no B4 H46 2.6081 . . no B4 H43 2.4856 . . no H3 H9" 2.3040 . . no H3 C9 2.8233 . . no H3 H8 2.5332 . . no H3 C8 3.0396 . . no H5 H11" 2.5803 . . no H5 H11 2.1498 . . no H5 C11 2.5550 . . no H7 B1 2.4449 . . no H7 O2 2.5708 . . no H7 H50" 2.4980 . . no H8 H3 2.5332 . . no H8 H71B 2.5595 . 2_675 no H8 H9" 2.5873 . . no H8 C3 2.8690 . . no H8' H20 2.4688 . . no H8' H9' 2.5084 . . no H8" Al3 3.5272 . . no H8" H58' 2.5175 . . no H9 C52 3.0839 . . no H9 H52 2.5155 . . no H9' H8' 2.5084 . . no H9' H20' 2.5137 . . no H9" H3 2.3040 . . no H9" C3 2.7977 . . no H9" H8 2.5873 . . no H9" H36' 2.5999 . 2_675 no H10 C56 2.9099 . . no H10 O1 2.7158 . . no H10 H56' 2.1219 . . no H10 Al2 3.2525 . . no H10 C54 2.9338 . . no H10 B1 2.7158 . . no H10 H54" 2.1683 . . no H10 C53 3.0257 . . no H11 H59" 2.5778 . 2_675 no H11 H5 2.1498 . . no H11 C5 2.7559 . . no H11 C59 3.0738 . 2_675 no H11 H12" 2.5412 . . no H11' H12' 2.4080 . . no H11" H5 2.5803 . . no H11" H54" 2.3137 . . no H11" C5 2.9254 . . no H12 B1 2.7180 . . no H12 C1 2.9937 . . no H12 Al3 3.1383 . . no H12 H58 2.5009 . . no H12 H59' 2.5489 . . no H12' H11' 2.4080 . . no H12' C47 2.8144 . . no H12' H47 2.4209 . . no H12' H47' 2.5333 . . no H12" H11 2.5412 . . no H12" H58 2.4625 . . no H15 H20" 2.2228 . . no H15 C21 3.0894 . . no H15 C20 2.7301 . . no H16 C28 2.9966 . 2_576 no H17 C24 2.6606 . . no H17 H24" 2.1855 . . no H19 Al1 3.3093 . . no H19 O4 2.5067 . . no H19 B2 2.5144 . . no H20 H8' 2.4688 . . no H20' H9' 2.5137 . . no H20' H21' 2.4869 . . no H20" H21 2.5481 . . no H20" C15 2.7604 . . no H20" H15 2.2228 . . no H21 H20" 2.5481 . . no H21 C15 2.9046 . . no H21' H50' 2.5263 . . no H21' C50 3.0459 . . no H21' H20' 2.4869 . . no H21" H31 2.5821 . . no H21" H64 2.4148 . . no H21" Al4 3.5077 . . no H21" O4 2.8874 . . no H22 H43 2.4469 . . no H22 B2 2.5499 . . no H22 O3 2.5750 . . no H23 C17 3.0029 . . no H23 H24" 2.5373 . . no H23' C74B 3.0816 . 1_465 no H23' H44" 2.4223 . . no H23' H24' 2.4983 . . no H23' H74B 2.5458 . 2_576 no H23" H70 2.5191 . 1_565 no H23" O3 2.7539 . . no H24 C17 3.0495 . . no H24 C62 2.9780 . . no H24' H23' 2.4983 . . no H24' H44" 2.5423 . . no H24" H17 2.1855 . . no H24" C17 2.7774 . . no H24" H23 2.5373 . . no H27 H36" 2.5980 . 2_666 no H27 H32" 2.2690 . . no H27 C32 2.6794 . . no H29 H35 2.1699 . . no H29 C35 2.7394 . . no H29 H33 2.4761 . 2_666 no H29 C36 3.0996 . . no H31 B3 2.5090 . . no H31 C21 3.0847 . . no H31 O6 2.7828 . . no H31 H21" 2.5821 . . no H32 C64 2.8369 . . no H32 C27 3.0010 . . no H32 H64' 2.2002 . . no H32' H33' 2.5649 . . no H32' H50 2.5093 . 1_545 no H32" C27 2.8540 . . no H32" H27 2.2690 . . no H32" H33 2.4590 . . no H33 C27 3.0420 . . no H33 H32" 2.4590 . . no H33 H29 2.4761 . 2_666 no H33' H32' 2.5649 . . no H33" H51' 2.3303 . . no H33" O6 2.7303 . . no H34 O5 2.6289 . . no H34 B3 2.5041 . . no H35 C29 2.7088 . . no H35 H29 2.1699 . . no H35 H36" 2.5506 . . no H35' H36' 2.4712 . . no H35' C48 2.9038 . . no H35' H48 2.2915 . . no H35" H67 2.5781 . . no H35" C63 3.0655 . . no H35" H63" 2.5689 . . no H36 H55 2.3863 . . no H36' H9" 2.5999 . 1_545 no H36' H35' 2.4712 . . no H36" H35 2.5506 . . no H36" C29 2.9128 . . no H36" H27 2.5980 . 2_666 no H39 H47' 2.5508 . . no H39 H47" 2.1959 . . no H39 C47 2.5617 . . no H41 C44 2.6929 . . no H41 H44 2.1619 . . no H43 Al3 3.5238 . . no H43 H22 2.4469 . . no H43 O8 2.6746 . . no H43 B4 2.4856 . . no H44 H41 2.1619 . . no H44 C41 2.7259 . . no H44 H45 2.5370 . . no H44' H60" 2.3006 . . no H44" H24' 2.5423 . . no H44" H45' 2.4543 . . no H44" H23' 2.4223 . . no H45 C41 2.9814 . . no H45 H44 2.5370 . . no H45' H52' 2.4850 . 2_576 no H45' C52 3.0429 . 1_455 no H45' H44" 2.4543 . . no H45" O8 2.8838 . . no H46 B4 2.6081 . . no H46 O7 2.5209 . . no H47 H75B 2.2125 . . no H47 H75 2.5669 . . no H47 H48' 2.5376 . . no H47 C75B 2.8055 . . no H47 H12' 2.4209 . . no H47' H12' 2.5333 . . no H47' C39 2.8700 . . no H47' H39 2.5508 . . no H47" C39 2.8033 . . no H47" H76 2.4995 . 1_545 no H47" H39 2.1959 . . no H47" H48" 2.4311 . . no H47" H75B 2.2251 . . no H47" C75B 3.0538 . . no H48 C35 2.9084 . . no H48 H35' 2.2915 . . no H48 C37 2.9898 . . no H48 B4 2.9657 . . no H48' H47 2.5376 . . no H48" H47" 2.4311 . . no H50 H32' 2.5093 . 1_545 no H50 H52" 2.4799 . . no H50 H51" 2.4427 . . no H50' O6 2.8732 . . no H50' H21' 2.5263 . . no H50' H51' 2.4996 . . no H50" H7 2.4980 . . no H50" H52 2.5137 . . no H51 H55' 2.4252 . . no H51 H52' 2.4827 . . no H51' H50' 2.4996 . . no H51' H33" 2.3303 . . no H51' C33 2.9829 . . no H51" H52" 2.4072 . . no H51" H50 2.4427 . . no H52 H50" 2.5137 . . no H52 H9 2.5155 . . no H52 C1 2.7364 . . no H52 C2 2.9130 . . no H52' H45' 2.4850 . 1_655 no H52' H54' 2.5263 . . no H52' H51 2.4827 . . no H52' C45 3.0156 . 1_655 no H52' C54 3.0614 . . no H52" H51" 2.4072 . . no H52" H50 2.4799 . . no H54 H55" 2.4875 . . no H54 H56 2.4302 . . no H54' H52' 2.5263 . . no H54' H55' 2.4194 . . no H54" H11" 2.3137 . . no H54" C11 2.7633 . . no H54" H10 2.1683 . . no H54" C10 2.8288 . . no H55 O6 2.6777 . . no H55 H36 2.3863 . . no H55 H56" 2.4735 . . no H55' C51 3.0475 . . no H55' H51 2.4252 . . no H55' H54' 2.4194 . . no H55" H56 2.4155 . . no H55" H54 2.4875 . . no H56 H54 2.4302 . . no H56 H55" 2.4155 . . no H56' C10 2.9026 . . no H56' H10 2.1219 . . no H56" H55 2.4735 . . no H58 H59' 2.5044 . . no H58 H12" 2.4625 . . no H58 H12 2.5009 . . no H58 C12 2.8690 . . no H58' H60' 2.4865 . . no H58' H8" 2.5175 . . no H58" H60 2.4524 . . no H58" H59" 2.4924 . . no H58" C73A 3.0148 . 2_675 no H59 C42 2.9821 . . no H59 C37 2.9270 . . no H59 H60" 2.5273 . . no H59' H12 2.5489 . . no H59' C12 2.9913 . . no H59' H58 2.5044 . . no H59" H11 2.5778 . 2_675 no H59" H60 2.4242 . . no H59" H58" 2.4924 . . no H60 H58" 2.4524 . . no H60 H59" 2.4242 . . no H60' H58' 2.4865 . . no H60' H70 2.5250 . 1_565 no H60" H44' 2.3006 . . no H60" H59 2.5273 . . no H62 H64" 2.4714 . . no H62 H63 2.4007 . . no H62' H63" 2.5636 . . no H62" H64 2.4605 . . no H62" C13 2.9042 . . no H62" C18 2.8423 . . no H63 H64" 2.4192 . . no H63 H62 2.4007 . . no H63' C30 3.0024 . . no H63' H64' 2.4235 . . no H63" H35" 2.5689 . . no H63" H62' 2.5636 . . no H64 H62" 2.4605 . . no H64 H21" 2.4148 . . no H64' C32 2.9751 . . no H64' C31 3.0514 . . no H64' C25 3.0935 . . no H64' C26 2.7471 . . no H64' H32 2.2002 . . no H64' H63' 2.4235 . . no H64" H62 2.4714 . . no H64" H63 2.4192 . . no H65 C13 3.0649 . 1_545 no H67 H35" 2.5781 . . no H68 C40 3.0668 . . no H68 C41 3.0584 . . no H69 H72B 2.5156 . 2_665 no H69 H73 2.5268 . 2_665 no H69 H72 2.4284 . 1_545 no H69 C72A 3.0923 . 2_665 no H70 H60' 2.5250 . 1_545 no H70 H23" 2.5191 . 1_545 no H71 C69 3.0827 . 2_665 no H71B H8 2.5595 . 2_675 no H72 H69 2.4284 . 2_665 no H72B H69 2.5156 . 2_665 no H73 H69 2.5268 . 2_665 no H73B C60 3.0622 . 1_645 no H74B C23 3.0081 . 1_645 no H74B H23' 2.5458 . 2_665 no H75 H47 2.5669 . . no H75B H47" 2.2251 . . no H75B C47 2.6319 . . no H75B H47 2.2125 . . no H76 H47" 2.4995 . 2_665 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C7 H7 O2 1.0000 2.5708 3.173(3) 118.56 . yes C19 H19 O4 1.0001 2.5067 3.133(2) 120.32 . yes C22 H22 O3 1.0001 2.5750 3.161(3) 117.27 . yes C46 H46 O7 1.0006 2.5209 3.299(3) 134.39 . yes # End of Crystallographic Information File