# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Rudolf Wehmschulte' _publ_contact_author_name 'Rudolf Wehmschulte' _publ_contact_author_email RWEHMSCH@FIT.EDU _publ_section_title ; Synthesis of Aryloxyaluminum Hydrides and their Conversion into Aryloxyalumoxanes (ArOAlO)n ; # Attachment 'RJW_Aryloxy_hydrides.cif' data_bt964 _database_code_depnum_ccdc_archive 'CCDC 739385' # Compound 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Dipp-OAlH2.NMe3 _chemical_melting_point ? _chemical_formula_moiety 'C33 H48 Al N O' _chemical_formula_sum 'C33 H48 Al N O' _chemical_formula_weight 501.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.875(2) _cell_length_b 9.497(2) _cell_length_c 33.002(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.581(16) _cell_angle_gamma 90.00 _cell_volume 3074.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9184 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 30.10 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9414 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details 'SADABS-2004/1 ; Bruker, 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46931 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5581 _reflns_number_gt 5126 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker, 2001; SMART v. 5.630' _computing_cell_refinement 'Bruker, 2006; SAINT+ v. 7.23a' _computing_data_reduction 'Bruker, 2006; SAINT+ v. 7.23a' _computing_structure_solution 'Bruker, 2003; XS, SHELXTL v. 6.14' _computing_structure_refinement "Bruker, 2003; XL,SHELXTL v. 6.14'" _computing_molecular_graphics 'Bruker, 2003; XP, SHELXTL v. 6.14' _computing_publication_material 'Bruker, 2003; XCIF, SHELXTL v. 6.14' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+2.9225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5581 _refine_ls_number_parameters 355 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.83125(5) 0.29365(5) 0.144767(16) 0.01753(13) Uani 1 1 d . . . C1 C 0.71263(17) 0.56629(18) 0.11732(5) 0.0140(3) Uani 1 1 d . . . C2 C 0.75622(17) 0.70699(18) 0.11445(5) 0.0153(3) Uani 1 1 d . . . C3 C 0.66144(17) 0.81062(18) 0.10136(5) 0.0170(4) Uani 1 1 d . . . H3 H 0.6902 0.9056 0.0995 0.020 Uiso 1 1 calc R . . C4 C 0.52515(18) 0.77611(18) 0.09101(5) 0.0182(4) Uani 1 1 d . . . H4 H 0.4617 0.8465 0.0809 0.022 Uiso 1 1 calc R . . C5 C 0.48209(17) 0.63906(19) 0.09546(5) 0.0173(4) Uani 1 1 d . . . H5 H 0.3884 0.6165 0.0889 0.021 Uiso 1 1 calc R . . C6 C 0.57367(17) 0.53331(18) 0.10939(5) 0.0148(3) Uani 1 1 d . . . C7 C 0.52505(16) 0.38744(18) 0.11751(5) 0.0156(3) Uani 1 1 d . . . C8 C 0.52127(16) 0.34302(18) 0.15840(5) 0.0166(4) Uani 1 1 d . . . C9 C 0.48116(17) 0.20571(19) 0.16558(6) 0.0205(4) Uani 1 1 d . . . H9 H 0.4799 0.1740 0.1928 0.025 Uiso 1 1 calc R . . C10 C 0.44302(18) 0.11442(19) 0.13347(6) 0.0222(4) Uani 1 1 d . . . H10 H 0.4168 0.0206 0.1388 0.027 Uiso 1 1 calc R . . C11 C 0.44323(18) 0.16013(19) 0.09366(6) 0.0215(4) Uani 1 1 d . . . H11 H 0.4142 0.0977 0.0719 0.026 Uiso 1 1 calc R . . C12 C 0.48516(17) 0.29574(19) 0.08482(5) 0.0187(4) Uani 1 1 d . B . C13 C 0.90139(17) 0.74277(17) 0.12963(5) 0.0156(3) Uani 1 1 d . . . C14 C 0.93585(18) 0.76431(18) 0.17173(5) 0.0181(4) Uani 1 1 d . . . C15 C 1.07071(18) 0.79274(19) 0.18678(6) 0.0216(4) Uani 1 1 d . . . H15 H 1.0945 0.8071 0.2152 0.026 Uiso 1 1 calc R . . C16 C 1.17057(18) 0.80021(19) 0.16047(6) 0.0224(4) Uani 1 1 d . . . H16 H 1.2626 0.8184 0.1709 0.027 Uiso 1 1 calc R . . C17 C 1.13608(18) 0.78118(18) 0.11896(6) 0.0209(4) Uani 1 1 d . . . H17 H 1.2048 0.7886 0.1012 0.025 Uiso 1 1 calc R . . C18 C 1.00253(18) 0.75141(18) 0.10280(5) 0.0183(4) Uani 1 1 d . . . C19 C 0.96546(19) 0.7353(2) 0.05702(5) 0.0229(4) Uani 1 1 d . . . H19 H 0.8816 0.6758 0.0524 0.028 Uiso 1 1 calc R . . C20 C 0.9323(2) 0.8798(2) 0.03758(6) 0.0311(5) Uani 1 1 d . . . H20A H 0.8564 0.9225 0.0499 0.047 Uiso 1 1 calc R . . H20B H 0.9066 0.8684 0.0082 0.047 Uiso 1 1 calc R . . H20C H 1.0126 0.9409 0.0422 0.047 Uiso 1 1 calc R . . C21 C 1.0772(2) 0.6642(2) 0.03558(6) 0.0339(5) Uani 1 1 d . . . H21A H 1.1558 0.7274 0.0360 0.051 Uiso 1 1 calc R . . H21B H 1.0419 0.6433 0.0073 0.051 Uiso 1 1 calc R . . H21C H 1.1053 0.5765 0.0498 0.051 Uiso 1 1 calc R . . C22 C 0.82781(19) 0.7629(2) 0.20138(5) 0.0226(4) Uani 1 1 d . . . H22 H 0.7408 0.7286 0.1861 0.027 Uiso 1 1 calc R . . C23 C 0.8032(2) 0.9125(2) 0.21597(7) 0.0397(6) Uani 1 1 d . . . H23A H 0.8873 0.9493 0.2309 0.060 Uiso 1 1 calc R . . H23B H 0.7310 0.9112 0.2340 0.060 Uiso 1 1 calc R . . H23C H 0.7755 0.9728 0.1924 0.060 Uiso 1 1 calc R . . C24 C 0.8648(2) 0.6629(3) 0.23718(6) 0.0353(5) Uani 1 1 d . . . H24A H 0.9491 0.6950 0.2530 0.053 Uiso 1 1 calc R . . H24B H 0.8780 0.5678 0.2268 0.053 Uiso 1 1 calc R . . H24C H 0.7909 0.6619 0.2546 0.053 Uiso 1 1 calc R . . H25A H 0.5244 0.4344 0.0396 0.042 Uiso 0.60 1 d P A 1 C26A C 0.5950(5) 0.2389(6) 0.02289(19) 0.0382(15) Uani 0.60 1 d PD B 1 H26A H 0.5573 0.1434 0.0207 0.057 Uiso 0.60 1 calc PR B 1 H26B H 0.6814 0.2380 0.0408 0.057 Uiso 0.60 1 calc PR B 1 H26C H 0.6110 0.2723 -0.0043 0.057 Uiso 0.60 1 calc PR B 1 H25B H 0.5057 0.4389 0.0422 0.046 Uiso 0.40 1 d P C 2 C26B C 0.6240(6) 0.2878(8) 0.0237(3) 0.036(2) Uani 0.40 1 d PDU B 2 H26D H 0.6290 0.1848 0.0249 0.054 Uiso 0.40 1 calc PR B 2 H26E H 0.7039 0.3280 0.0400 0.054 Uiso 0.40 1 calc PR B 2 H26F H 0.6222 0.3188 -0.0047 0.054 Uiso 0.40 1 calc PR B 2 C25 C 0.49367(19) 0.3376(2) 0.04079(6) 0.0235(4) Uani 1 1 d D . . C27 C 0.3605(2) 0.3196(3) 0.01363(6) 0.0380(5) Uani 1 1 d . B . H27A H 0.3717 0.3515 -0.0140 0.057 Uiso 1 1 calc R . . H27B H 0.2894 0.3756 0.0244 0.057 Uiso 1 1 calc R . . H27C H 0.3342 0.2201 0.0129 0.057 Uiso 1 1 calc R . . C28 C 0.55627(18) 0.44528(19) 0.19388(5) 0.0190(4) Uani 1 1 d . . . H28 H 0.6383 0.5001 0.1881 0.023 Uiso 1 1 calc R . . C29 C 0.4396(2) 0.5504(2) 0.19634(6) 0.0262(4) Uani 1 1 d . . . H29A H 0.4190 0.5979 0.1700 0.039 Uiso 1 1 calc R . . H29B H 0.4668 0.6204 0.2175 0.039 Uiso 1 1 calc R . . H29C H 0.3585 0.5001 0.2031 0.039 Uiso 1 1 calc R . . C30 C 0.5901(2) 0.3746(2) 0.23543(5) 0.0250(4) Uani 1 1 d . . . H30A H 0.5079 0.3297 0.2435 0.037 Uiso 1 1 calc R . . H30B H 0.6231 0.4455 0.2558 0.037 Uiso 1 1 calc R . . H30C H 0.6608 0.3032 0.2336 0.037 Uiso 1 1 calc R . . C31 C 1.11350(19) 0.3837(2) 0.15089(6) 0.0273(4) Uani 1 1 d . . . H31A H 1.1155 0.3728 0.1805 0.041 Uiso 1 1 calc R . . H31B H 1.0801 0.4780 0.1429 0.041 Uiso 1 1 calc R . . H31C H 1.2057 0.3713 0.1432 0.041 Uiso 1 1 calc R . . C32 C 1.0199(2) 0.2914(2) 0.08519(6) 0.0300(5) Uani 1 1 d . . . H32A H 1.1130 0.2819 0.0779 0.045 Uiso 1 1 calc R . . H32B H 0.9838 0.3842 0.0767 0.045 Uiso 1 1 calc R . . H32C H 0.9621 0.2180 0.0713 0.045 Uiso 1 1 calc R . . C33 C 1.07103(19) 0.13307(19) 0.14230(6) 0.0244(4) Uani 1 1 d . . . H33A H 1.0099 0.0622 0.1285 0.037 Uiso 1 1 calc R . . H33B H 1.0728 0.1228 0.1719 0.037 Uiso 1 1 calc R . . H33C H 1.1632 0.1198 0.1346 0.037 Uiso 1 1 calc R . . N1 N 1.02131(14) 0.27613(16) 0.12987(4) 0.0192(3) Uani 1 1 d . . . O1 O 0.80602(12) 0.46806(12) 0.12903(4) 0.0192(3) Uani 1 1 d . . . H1 H 0.766(2) 0.178(2) 0.1187(6) 0.030(6) Uiso 1 1 d . . . H2 H 0.852(2) 0.283(2) 0.1893(6) 0.029(6) Uiso 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 0.0157(3) 0.0128(3) 0.0245(3) 0.0022(2) 0.0041(2) 0.0012(2) C1 0.0169(8) 0.0130(8) 0.0127(8) 0.0000(6) 0.0035(6) 0.0034(7) C2 0.0169(8) 0.0165(9) 0.0130(8) -0.0004(7) 0.0041(6) -0.0009(7) C3 0.0222(9) 0.0114(8) 0.0179(8) 0.0005(7) 0.0042(7) -0.0003(7) C4 0.0183(9) 0.0156(9) 0.0207(9) 0.0021(7) 0.0019(7) 0.0047(7) C5 0.0139(8) 0.0202(9) 0.0178(8) -0.0005(7) 0.0019(6) -0.0002(7) C6 0.0170(8) 0.0140(8) 0.0139(8) -0.0004(6) 0.0039(6) 0.0005(7) C7 0.0101(8) 0.0145(8) 0.0225(9) 0.0000(7) 0.0031(6) 0.0019(7) C8 0.0119(8) 0.0151(9) 0.0235(9) 0.0005(7) 0.0043(7) 0.0025(7) C9 0.0180(9) 0.0179(9) 0.0266(9) 0.0047(7) 0.0070(7) 0.0019(7) C10 0.0184(9) 0.0143(9) 0.0352(10) 0.0016(8) 0.0076(7) -0.0001(7) C11 0.0183(9) 0.0177(9) 0.0290(10) -0.0068(7) 0.0047(7) -0.0025(7) C12 0.0130(8) 0.0187(9) 0.0248(9) -0.0008(7) 0.0048(7) 0.0001(7) C13 0.0169(8) 0.0080(8) 0.0224(9) 0.0012(6) 0.0037(7) 0.0006(6) C14 0.0198(9) 0.0111(8) 0.0235(9) 0.0021(7) 0.0033(7) -0.0007(7) C15 0.0235(9) 0.0166(9) 0.0235(9) 0.0018(7) -0.0021(7) -0.0006(7) C16 0.0147(9) 0.0149(9) 0.0367(10) 0.0002(8) -0.0015(7) -0.0001(7) C17 0.0169(9) 0.0132(9) 0.0342(10) 0.0001(7) 0.0100(7) 0.0007(7) C18 0.0193(9) 0.0104(8) 0.0261(9) 0.0005(7) 0.0068(7) -0.0001(7) C19 0.0242(9) 0.0217(10) 0.0241(9) -0.0016(7) 0.0081(7) -0.0063(8) C20 0.0358(11) 0.0340(12) 0.0239(10) 0.0056(8) 0.0043(8) -0.0061(9) C21 0.0366(12) 0.0353(12) 0.0330(11) -0.0073(9) 0.0172(9) -0.0075(10) C22 0.0230(9) 0.0265(10) 0.0185(9) -0.0015(7) 0.0038(7) -0.0063(8) C23 0.0430(13) 0.0342(12) 0.0468(13) -0.0119(10) 0.0261(11) -0.0065(10) C24 0.0341(11) 0.0484(14) 0.0226(10) 0.0066(9) 0.0002(8) -0.0145(10) C26A 0.015(2) 0.078(4) 0.022(2) 0.008(3) 0.0066(18) 0.000(3) C26B 0.018(3) 0.056(4) 0.036(3) 0.014(3) 0.014(3) -0.003(3) C25 0.0253(10) 0.0237(10) 0.0218(9) -0.0037(8) 0.0041(7) -0.0079(8) C27 0.0270(11) 0.0582(15) 0.0283(11) 0.0091(10) 0.0017(8) 0.0004(10) C28 0.0200(9) 0.0175(9) 0.0199(9) 0.0010(7) 0.0041(7) -0.0034(7) C29 0.0345(11) 0.0223(10) 0.0223(9) -0.0036(8) 0.0060(8) 0.0045(8) C30 0.0261(10) 0.0284(10) 0.0209(9) 0.0032(8) 0.0047(7) -0.0014(8) C31 0.0177(9) 0.0199(10) 0.0434(12) 0.0008(8) 0.0001(8) -0.0022(8) C32 0.0296(11) 0.0333(11) 0.0291(10) 0.0029(9) 0.0116(8) 0.0036(9) C33 0.0199(9) 0.0174(9) 0.0359(11) 0.0015(8) 0.0031(8) 0.0046(7) N1 0.0161(7) 0.0166(8) 0.0249(8) 0.0007(6) 0.0028(6) 0.0011(6) O1 0.0144(6) 0.0135(6) 0.0297(7) 0.0028(5) 0.0020(5) 0.0008(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 O1 1.7452(13) . ? Al1 N1 2.0009(16) . ? Al1 H1 1.50(2) . ? Al1 H2 1.46(2) . ? C1 O1 1.337(2) . ? C1 C6 1.403(2) . ? C1 C2 1.410(2) . ? C2 C3 1.392(2) . ? C2 C13 1.502(2) . ? C3 C4 1.389(2) . ? C3 H3 0.9500 . ? C4 C5 1.382(2) . ? C4 H4 0.9500 . ? C5 C6 1.394(2) . ? C5 H5 0.9500 . ? C6 C7 1.500(2) . ? C7 C12 1.407(2) . ? C7 C8 1.418(2) . ? C8 C9 1.391(3) . ? C8 C28 1.530(2) . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 H11 0.9500 . ? C12 C25 1.518(2) . ? C13 C14 1.407(2) . ? C13 C18 1.411(2) . ? C14 C15 1.393(3) . ? C14 C22 1.528(2) . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.394(3) . ? C17 H17 0.9500 . ? C18 C19 1.521(3) . ? C19 C21 1.534(3) . ? C19 C20 1.534(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.527(3) . ? C22 C23 1.528(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26A C25 1.539(3) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C26B C25 1.538(3) . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C25 C27 1.514(3) . ? C25 H25A 0.9697 . ? C25 H25B 0.9696 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.529(2) . ? C28 C29 1.533(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N1 1.486(2) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N1 1.480(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N1 1.486(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 N1 96.42(6) . . ? O1 Al1 H1 119.2(8) . . ? N1 Al1 H1 98.8(8) . . ? O1 Al1 H2 111.2(8) . . ? N1 Al1 H2 102.5(8) . . ? H1 Al1 H2 121.9(12) . . ? O1 C1 C6 121.72(15) . . ? O1 C1 C2 118.34(15) . . ? C6 C1 C2 119.90(15) . . ? C3 C2 C1 119.41(15) . . ? C3 C2 C13 121.70(15) . . ? C1 C2 C13 118.60(15) . . ? C4 C3 C2 120.49(16) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.81(16) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.17(16) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.99(16) . . ? C5 C6 C7 121.02(15) . . ? C1 C6 C7 119.94(15) . . ? C12 C7 C8 120.64(16) . . ? C12 C7 C6 120.12(15) . . ? C8 C7 C6 119.23(15) . . ? C9 C8 C7 118.68(16) . . ? C9 C8 C28 120.55(16) . . ? C7 C8 C28 120.74(15) . . ? C10 C9 C8 120.89(17) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 119.95(17) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 121.41(17) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 118.38(16) . . ? C11 C12 C25 119.52(16) . . ? C7 C12 C25 122.01(16) . . ? C14 C13 C18 120.19(16) . . ? C14 C13 C2 118.41(15) . . ? C18 C13 C2 121.39(15) . . ? C15 C14 C13 119.55(16) . . ? C15 C14 C22 118.85(16) . . ? C13 C14 C22 121.56(15) . . ? C16 C15 C14 120.36(17) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.00(16) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 121.32(16) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 118.57(16) . . ? C17 C18 C19 120.67(16) . . ? C13 C18 C19 120.70(15) . . ? C18 C19 C21 113.48(16) . . ? C18 C19 C20 109.94(15) . . ? C21 C19 C20 109.36(16) . . ? C18 C19 H19 108.0 . . ? C21 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C14 112.24(16) . . ? C24 C22 C23 111.50(17) . . ? C14 C22 C23 109.96(15) . . ? C24 C22 H22 107.6 . . ? C14 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 C26A H26A 109.5 . . ? C25 C26A H26B 109.5 . . ? C25 C26A H26C 109.5 . . ? C25 C26B H26D 109.5 . . ? C25 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C27 C25 C12 113.41(16) . . ? C27 C25 C26B 117.1(4) . . ? C12 C25 C26B 114.2(5) . . ? C27 C25 C26A 105.2(3) . . ? C12 C25 C26A 108.5(3) . . ? C27 C25 H25A 109.8 . . ? C12 C25 H25A 109.8 . . ? C26B C25 H25A 89.9 . . ? C26A C25 H25A 110.0 . . ? C27 C25 H25B 103.5 . . ? C12 C25 H25B 103.5 . . ? C26B C25 H25B 102.7 . . ? C26A C25 H25B 122.8 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C8 114.49(15) . . ? C30 C28 C29 109.06(15) . . ? C8 C28 C29 110.40(14) . . ? C30 C28 H28 107.5 . . ? C8 C28 H28 107.5 . . ? C29 C28 H28 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N1 C32 H32A 109.5 . . ? N1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N1 C33 H33A 109.5 . . ? N1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 N1 C33 109.22(15) . . ? C32 N1 C31 109.44(15) . . ? C33 N1 C31 109.54(14) . . ? C32 N1 Al1 109.57(11) . . ? C33 N1 Al1 107.32(11) . . ? C31 N1 Al1 111.71(11) . . ? C1 O1 Al1 144.91(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.282 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.044 #===END data_bt1244 _database_code_depnum_ccdc_archive 'CCDC 739386' # Compound 6.3C7H8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(ROAl(O)DMSO)4 + 3toluene' _chemical_melting_point ? _chemical_formula_moiety 'C80 H140 Al4 O12 S4, 3(C7 H8)' _chemical_formula_sum 'C101 H164 Al4 O12 S4' _chemical_formula_weight 1806.48 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' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.9642(5) _cell_length_b 28.4632(10) _cell_length_c 50.1873(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21376.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 28.86 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7856 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS-2007/4 (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 318618 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.25 _reflns_number_total 19341 _reflns_number_gt 14920 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+27.9428P] 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 19341 _refine_ls_number_parameters 1138 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _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 0.24011(5) 0.36285(2) 0.902398(14) 0.01778(16) Uani 1 1 d . . . Al2 Al 0.11569(5) 0.27258(2) 0.886955(14) 0.01767(16) Uani 1 1 d . . . Al3 Al 0.26708(5) 0.23929(3) 0.843286(14) 0.01878(16) Uani 1 1 d . . . Al4 Al 0.40034(5) 0.32306(2) 0.863800(14) 0.01790(16) Uani 1 1 d . . . C2 C 0.22996(16) 0.37587(9) 0.96007(5) 0.0205(5) Uani 1 1 d . . . C3 C 0.15493(16) 0.39971(9) 0.97079(5) 0.0208(5) Uani 1 1 d . . . C4 C 0.12406(17) 0.38626(9) 0.99593(5) 0.0234(5) Uani 1 1 d . . . H4A H 0.0726 0.4014 1.0029 0.028 Uiso 1 1 calc R . . C5 C 0.16486(17) 0.35188(10) 1.01120(5) 0.0274(6) Uani 1 1 d . A . C6 C 0.24429(18) 0.33331(10) 1.00149(5) 0.0267(6) Uani 1 1 d . . . H6A H 0.2757 0.3113 1.0122 0.032 Uiso 1 1 calc R . . C7 C 0.28031(17) 0.34526(9) 0.97677(5) 0.0235(5) Uani 1 1 d . . . C8 C 0.37545(18) 0.32843(10) 0.96897(5) 0.0283(6) Uani 1 1 d . . . C9 C 0.37490(19) 0.29119(10) 0.94682(5) 0.0302(6) Uani 1 1 d . . . H9A H 0.3442 0.3037 0.9311 0.045 Uiso 1 1 calc R . . H9B H 0.3436 0.2630 0.9531 0.045 Uiso 1 1 calc R . . H9C H 0.4365 0.2830 0.9421 0.045 Uiso 1 1 calc R . . C10 C 0.43171(19) 0.37098(11) 0.96010(7) 0.0393(7) Uani 1 1 d . . . H10D H 0.4052 0.3849 0.9441 0.059 Uiso 1 1 calc R . . H10E H 0.4928 0.3607 0.9562 0.059 Uiso 1 1 calc R . . H10F H 0.4329 0.3944 0.9744 0.059 Uiso 1 1 calc R . . C11 C 0.42446(19) 0.30651(12) 0.99288(6) 0.0381(7) Uani 1 1 d . . . H11A H 0.4863 0.2993 0.9879 0.057 Uiso 1 1 calc R . . H11B H 0.3940 0.2775 0.9982 0.057 Uiso 1 1 calc R . . H11C H 0.4243 0.3287 1.0078 0.057 Uiso 1 1 calc R . . C12 C 0.12718(19) 0.33596(11) 1.03832(5) 0.0346(7) Uani 1 1 d D . . C13 C 0.1089(4) 0.28363(17) 1.03787(11) 0.0555(13) Uiso 0.769(4) 1 d P A 1 H13A H 0.0676 0.2763 1.0233 0.083 Uiso 0.769(4) 1 calc PR A 1 H13B H 0.0821 0.2741 1.0548 0.083 Uiso 0.769(4) 1 calc PR A 1 H13C H 0.1651 0.2666 1.0352 0.083 Uiso 0.769(4) 1 calc PR A 1 C14 C 0.1963(3) 0.34634(15) 1.06032(8) 0.0389(10) Uiso 0.769(4) 1 d P A 1 H14A H 0.2093 0.3801 1.0607 0.058 Uiso 0.769(4) 1 calc PR A 1 H14B H 0.2514 0.3289 1.0567 0.058 Uiso 0.769(4) 1 calc PR A 1 H14C H 0.1722 0.3366 1.0776 0.058 Uiso 0.769(4) 1 calc PR A 1 C15 C 0.0427(3) 0.36166(17) 1.04619(9) 0.0521(12) Uiso 0.769(4) 1 d P A 1 H15A H 0.0548 0.3954 1.0472 0.078 Uiso 0.769(4) 1 calc PR A 1 H15B H 0.0223 0.3503 1.0636 0.078 Uiso 0.769(4) 1 calc PR A 1 H15C H -0.0038 0.3558 1.0328 0.078 Uiso 0.769(4) 1 calc PR A 1 C13B C 0.1550(12) 0.2845(3) 1.0441(3) 0.050 Uiso 0.231(4) 1 d PD A 2 H13D H 0.2195 0.2831 1.0474 0.075 Uiso 0.231(4) 1 calc PR A 2 H13E H 0.1403 0.2647 1.0287 0.075 Uiso 0.231(4) 1 calc PR A 2 H13F H 0.1228 0.2730 1.0598 0.075 Uiso 0.231(4) 1 calc PR A 2 C14B C 0.1300(11) 0.3756(4) 1.0588(2) 0.050 Uiso 0.231(4) 1 d PD A 2 H14D H 0.0896 0.4008 1.0533 0.075 Uiso 0.231(4) 1 calc PR A 2 H14E H 0.1910 0.3878 1.0602 0.075 Uiso 0.231(4) 1 calc PR A 2 H14F H 0.1111 0.3635 1.0762 0.075 Uiso 0.231(4) 1 calc PR A 2 C15B C 0.0274(5) 0.3239(5) 1.0346(3) 0.050 Uiso 0.231(4) 1 d PD A 2 H15D H -0.0044 0.3515 1.0278 0.075 Uiso 0.231(4) 1 calc PR A 2 H15E H 0.0017 0.3145 1.0517 0.075 Uiso 0.231(4) 1 calc PR A 2 H15F H 0.0215 0.2980 1.0218 0.075 Uiso 0.231(4) 1 calc PR A 2 C16 C 0.10810(18) 0.44005(9) 0.95584(5) 0.0250(6) Uani 1 1 d . . . C17 C 0.0454(2) 0.46816(10) 0.97428(6) 0.0331(7) Uani 1 1 d . . . H17A H 0.0788 0.4789 0.9899 0.050 Uiso 1 1 calc R . . H17B H -0.0041 0.4481 0.9800 0.050 Uiso 1 1 calc R . . H17C H 0.0218 0.4954 0.9646 0.050 Uiso 1 1 calc R . . C18 C 0.1772(2) 0.47583(9) 0.94560(6) 0.0323(6) Uani 1 1 d . . . H18A H 0.2114 0.4883 0.9607 0.048 Uiso 1 1 calc R . . H18B H 0.1463 0.5016 0.9365 0.048 Uiso 1 1 calc R . . H18C H 0.2179 0.4603 0.9331 0.048 Uiso 1 1 calc R . . C19 C 0.05025(18) 0.42090(10) 0.93292(5) 0.0283(6) Uani 1 1 d . . . H19A H 0.0268 0.4472 0.9224 0.042 Uiso 1 1 calc R . . H19B H 0.0005 0.4027 0.9403 0.042 Uiso 1 1 calc R . . H19C H 0.0867 0.4006 0.9215 0.042 Uiso 1 1 calc R . . C21 C 0.1979(2) 0.48317(12) 0.84946(7) 0.0471(9) Uani 1 1 d . . . H21A H 0.1505 0.4671 0.8395 0.071 Uiso 1 1 calc R . . H21B H 0.2332 0.5025 0.8372 0.071 Uiso 1 1 calc R . . H21C H 0.1711 0.5033 0.8631 0.071 Uiso 1 1 calc R . . C22 C 0.3347(2) 0.47958(12) 0.88404(6) 0.0417(8) Uani 1 1 d . . . H22A H 0.3710 0.4613 0.8966 0.063 Uiso 1 1 calc R . . H22B H 0.2960 0.5012 0.8940 0.063 Uiso 1 1 calc R . . H22C H 0.3740 0.4976 0.8722 0.063 Uiso 1 1 calc R . . C24 C -0.06212(16) 0.26828(9) 0.86177(5) 0.0200(5) Uani 1 1 d . . . C25 C -0.10862(17) 0.22504(9) 0.86051(5) 0.0230(5) Uani 1 1 d . . . C26 C -0.16756(17) 0.21757(10) 0.83917(5) 0.0267(6) Uani 1 1 d . . . H26A H -0.1971 0.1881 0.8380 0.032 Uiso 1 1 calc R . . C27 C -0.18476(17) 0.25084(10) 0.81992(5) 0.0281(6) Uani 1 1 d . . . C28 C -0.14498(17) 0.29466(10) 0.82328(5) 0.0266(6) Uani 1 1 d . . . H28A H -0.1586 0.3187 0.8108 0.032 Uiso 1 1 calc R . . C29 C -0.08629(16) 0.30511(9) 0.84399(5) 0.0209(5) Uani 1 1 d . . . C30 C -0.05544(15) 0.35629(9) 0.84840(5) 0.0247(6) Uani 1 1 d D . . C31 C -0.10517(19) 0.39063(10) 0.82991(6) 0.0347(7) Uani 1 1 d D . . H31A H -0.0889 0.3842 0.8114 0.052 Uiso 1 1 calc R . . H31B H -0.0885 0.4230 0.8344 0.052 Uiso 1 1 calc R . . H31C H -0.1698 0.3867 0.8322 0.052 Uiso 1 1 calc R . . C32 C 0.04491(16) 0.36377(9) 0.84300(6) 0.0272(6) Uani 1 1 d D . . H32A H 0.0573 0.3583 0.8241 0.041 Uiso 1 1 calc R . . H32B H 0.0798 0.3417 0.8538 0.041 Uiso 1 1 calc R . . H32C H 0.0614 0.3960 0.8477 0.041 Uiso 1 1 calc R . . C33 C -0.07737(19) 0.37093(10) 0.87728(5) 0.0316(6) Uani 1 1 d D . . H33A H -0.0447 0.3507 0.8897 0.047 Uiso 1 1 calc R . . H33B H -0.1417 0.3677 0.8804 0.047 Uiso 1 1 calc R . . H33C H -0.0597 0.4037 0.8801 0.047 Uiso 1 1 calc R . . C34 C -0.24543(19) 0.24263(11) 0.79553(5) 0.0346(7) Uani 1 1 d . . . C35 C -0.1883(2) 0.24852(12) 0.77036(6) 0.0386(7) Uani 1 1 d . . . H35A H -0.1398 0.2254 0.7705 0.058 Uiso 1 1 calc R . . H35B H -0.1630 0.2803 0.7699 0.058 Uiso 1 1 calc R . . H35C H -0.2256 0.2436 0.7546 0.058 Uiso 1 1 calc R . . C36 C -0.32114(19) 0.27896(14) 0.79519(6) 0.0460(9) Uani 1 1 d . . . H36A H -0.2957 0.3106 0.7941 0.069 Uiso 1 1 calc R . . H36B H -0.3565 0.2761 0.8115 0.069 Uiso 1 1 calc R . . H36C H -0.3596 0.2734 0.7797 0.069 Uiso 1 1 calc R . . C37 C -0.2854(2) 0.19344(13) 0.79537(6) 0.0518(9) Uani 1 1 d . . . H37A H -0.2372 0.1701 0.7953 0.078 Uiso 1 1 calc R . . H37B H -0.3223 0.1894 0.7794 0.078 Uiso 1 1 calc R . . H37C H -0.3225 0.1891 0.8113 0.078 Uiso 1 1 calc R . . C38 C -0.09566(18) 0.18635(9) 0.88176(5) 0.0275(6) Uani 1 1 d . . . C39 C -0.00460(19) 0.16239(10) 0.87810(6) 0.0332(7) Uani 1 1 d . . . H39A H -0.0031 0.1463 0.8608 0.050 Uiso 1 1 calc R . . H39B H 0.0046 0.1394 0.8924 0.050 Uiso 1 1 calc R . . H39C H 0.0428 0.1861 0.8787 0.050 Uiso 1 1 calc R . . C40 C -0.10491(19) 0.20717(10) 0.90988(5) 0.0300(6) Uani 1 1 d . . . H40A H -0.0971 0.1822 0.9231 0.045 Uiso 1 1 calc R . . H40B H -0.1644 0.2212 0.9119 0.045 Uiso 1 1 calc R . . H40C H -0.0592 0.2314 0.9125 0.045 Uiso 1 1 calc R . . C41 C -0.1667(2) 0.14773(10) 0.87952(6) 0.0344(7) Uani 1 1 d . . . H41A H -0.1604 0.1316 0.8624 0.052 Uiso 1 1 calc R . . H41B H -0.2263 0.1618 0.8807 0.052 Uiso 1 1 calc R . . H41C H -0.1587 0.1251 0.8940 0.052 Uiso 1 1 calc R . . C43 C 0.05594(19) 0.28984(10) 0.95600(5) 0.0312(6) Uani 1 1 d . . . H43A H 0.0405 0.3152 0.9436 0.047 Uiso 1 1 calc R . . H43B H 0.0708 0.3032 0.9734 0.047 Uiso 1 1 calc R . . H43C H 0.0049 0.2685 0.9579 0.047 Uiso 1 1 calc R . . C44 C 0.1484(2) 0.20989(11) 0.96614(6) 0.0419(8) Uani 1 1 d . . . H44A H 0.1946 0.1872 0.9610 0.063 Uiso 1 1 calc R . . H44B H 0.0897 0.1946 0.9656 0.063 Uiso 1 1 calc R . . H44C H 0.1604 0.2213 0.9842 0.063 Uiso 1 1 calc R . . C46 C 0.36336(16) 0.14827(8) 0.84381(5) 0.0205(5) Uani 1 1 d . . . C47 C 0.37513(18) 0.12633(9) 0.86901(5) 0.0242(6) Uani 1 1 d . . . C48 C 0.44627(18) 0.09516(9) 0.87210(6) 0.0286(6) Uani 1 1 d . . . H48A H 0.4552 0.0812 0.8891 0.034 Uiso 1 1 calc R . . C49 C 0.50472(19) 0.08346(9) 0.85167(6) 0.0301(6) Uani 1 1 d . B . C50 C 0.48828(18) 0.10309(9) 0.82690(6) 0.0275(6) Uani 1 1 d . . . H50A H 0.5260 0.0945 0.8125 0.033 Uiso 1 1 calc R . . C51 C 0.41900(17) 0.13493(9) 0.82208(5) 0.0236(5) Uani 1 1 d . . . C52 C 0.40559(17) 0.15528(9) 0.79380(5) 0.0235(5) Uani 1 1 d . . . C53 C 0.30884(18) 0.14689(10) 0.78453(5) 0.0279(6) Uani 1 1 d . . . H53A H 0.2961 0.1131 0.7847 0.042 Uiso 1 1 calc R . . H53B H 0.3013 0.1591 0.7664 0.042 Uiso 1 1 calc R . . H53C H 0.2676 0.1631 0.7966 0.042 Uiso 1 1 calc R . . C54 C 0.42946(18) 0.20775(9) 0.79360(5) 0.0256(6) Uani 1 1 d . . . H54A H 0.4926 0.2117 0.7983 0.038 Uiso 1 1 calc R . . H54B H 0.3921 0.2244 0.8066 0.038 Uiso 1 1 calc R . . H54C H 0.4189 0.2207 0.7758 0.038 Uiso 1 1 calc R . . C55 C 0.46665(19) 0.13165(10) 0.77311(5) 0.0310(6) Uani 1 1 d . . . H55A H 0.5293 0.1382 0.7775 0.047 Uiso 1 1 calc R . . H55B H 0.4531 0.1440 0.7553 0.047 Uiso 1 1 calc R . . H55C H 0.4566 0.0976 0.7733 0.047 Uiso 1 1 calc R . . C56 C 0.58444(18) 0.05082(9) 0.85705(6) 0.0358(7) Uani 1 1 d D . . C57A C 0.6403(5) 0.0398(3) 0.83249(13) 0.050(2) Uiso 0.50 1 d PD B 1 H57A H 0.6707 0.0684 0.8265 0.075 Uiso 0.50 1 calc PR B 1 H57B H 0.6014 0.0281 0.8183 0.075 Uiso 0.50 1 calc PR B 1 H57C H 0.6849 0.0158 0.8369 0.075 Uiso 0.50 1 calc PR B 1 C58A C 0.6432(4) 0.0733(2) 0.87886(12) 0.0350(16) Uiso 0.50 1 d PD B 1 H58A H 0.6631 0.1045 0.8730 0.052 Uiso 0.50 1 calc PR B 1 H58B H 0.6954 0.0534 0.8822 0.052 Uiso 0.50 1 calc PR B 1 H58C H 0.6085 0.0765 0.8953 0.052 Uiso 0.50 1 calc PR B 1 C59A C 0.5501(5) 0.00386(19) 0.86832(15) 0.0326(18) Uiso 0.50 1 d PD B 1 H59A H 0.5114 -0.0114 0.8551 0.049 Uiso 0.50 1 calc PR B 1 H59B H 0.5161 0.0097 0.8847 0.049 Uiso 0.50 1 calc PR B 1 H59C H 0.6009 -0.0167 0.8723 0.049 Uiso 0.50 1 calc PR B 1 C57B C 0.6672(9) 0.0709(7) 0.8424(4) 0.040 Uiso 0.15 1 d PD B 2 H57D H 0.6819 0.1019 0.8498 0.060 Uiso 0.15 1 calc PR B 2 H57E H 0.6541 0.0739 0.8234 0.060 Uiso 0.15 1 calc PR B 2 H57F H 0.7181 0.0497 0.8449 0.060 Uiso 0.15 1 calc PR B 2 C58B C 0.6260(15) 0.0588(9) 0.8849(2) 0.040 Uiso 0.15 1 d PD B 2 H58D H 0.6295 0.0926 0.8885 0.060 Uiso 0.15 1 calc PR B 2 H58E H 0.6862 0.0453 0.8854 0.060 Uiso 0.15 1 calc PR B 2 H58F H 0.5887 0.0437 0.8985 0.060 Uiso 0.15 1 calc PR B 2 C59B C 0.5793(15) 0.0049(4) 0.8413(4) 0.040 Uiso 0.15 1 d PD B 2 H59D H 0.5832 0.0117 0.8222 0.060 Uiso 0.15 1 calc PR B 2 H59E H 0.5224 -0.0109 0.8451 0.060 Uiso 0.15 1 calc PR B 2 H59F H 0.6289 -0.0157 0.8465 0.060 Uiso 0.15 1 calc PR B 2 C57C C 0.6175(7) 0.0284(4) 0.83070(13) 0.032(2) Uiso 0.35 1 d PD B 3 H57G H 0.6411 0.0529 0.8190 0.049 Uiso 0.35 1 calc PR B 3 H57H H 0.5676 0.0124 0.8219 0.049 Uiso 0.35 1 calc PR B 3 H57I H 0.6647 0.0055 0.8346 0.049 Uiso 0.35 1 calc PR B 3 C58C C 0.6634(4) 0.0807(3) 0.86645(19) 0.035(2) Uiso 0.35 1 d PD B 3 H58G H 0.6786 0.1037 0.8527 0.053 Uiso 0.35 1 calc PR B 3 H58H H 0.7151 0.0603 0.8698 0.053 Uiso 0.35 1 calc PR B 3 H58I H 0.6472 0.0971 0.8829 0.053 Uiso 0.35 1 calc PR B 3 C59C C 0.5588(7) 0.0091(4) 0.8760(2) 0.039(3) Uiso 0.35 1 d P B 3 H59G H 0.5448 0.0214 0.8938 0.058 Uiso 0.35 1 calc PR B 3 H59H H 0.6091 -0.0128 0.8773 0.058 Uiso 0.35 1 calc PR B 3 H59I H 0.5065 -0.0073 0.8689 0.058 Uiso 0.35 1 calc PR B 3 C60 C 0.31376(18) 0.13683(9) 0.89296(5) 0.0260(6) Uani 1 1 d . . . C61 C 0.3295(2) 0.10293(11) 0.91642(6) 0.0362(7) Uani 1 1 d . . . H61A H 0.3197 0.0705 0.9105 0.054 Uiso 1 1 calc R . . H61B H 0.2877 0.1103 0.9309 0.054 Uiso 1 1 calc R . . H61C H 0.3910 0.1063 0.9229 0.054 Uiso 1 1 calc R . . C62 C 0.21492(18) 0.13092(10) 0.88536(5) 0.0296(6) Uani 1 1 d . . . H62A H 0.2003 0.1523 0.8707 0.044 Uiso 1 1 calc R . . H62B H 0.1773 0.1382 0.9008 0.044 Uiso 1 1 calc R . . H62C H 0.2041 0.0984 0.8797 0.044 Uiso 1 1 calc R . . C63 C 0.33217(19) 0.18680(9) 0.90360(5) 0.0293(6) Uani 1 1 d . . . H63A H 0.3259 0.2095 0.8890 0.044 Uiso 1 1 calc R . . H63B H 0.3930 0.1883 0.9108 0.044 Uiso 1 1 calc R . . H63C H 0.2893 0.1943 0.9177 0.044 Uiso 1 1 calc R . . C64 C 0.0922(2) 0.27523(11) 0.77615(5) 0.0346(7) Uani 1 1 d . . . H64A H 0.1233 0.3044 0.7715 0.052 Uiso 1 1 calc R . . H64B H 0.0278 0.2793 0.7734 0.052 Uiso 1 1 calc R . . H64C H 0.1140 0.2496 0.7648 0.052 Uiso 1 1 calc R . . C65 C 0.05606(19) 0.20678(10) 0.81121(6) 0.0321(6) Uani 1 1 d . . . H65A H 0.0688 0.1910 0.8281 0.048 Uiso 1 1 calc R . . H65B H 0.0763 0.1870 0.7964 0.048 Uiso 1 1 calc R . . H65C H -0.0084 0.2122 0.8096 0.048 Uiso 1 1 calc R . . C67 C 0.46148(16) 0.40546(9) 0.83281(5) 0.0211(5) Uani 1 1 d . . . C68 C 0.51625(17) 0.44074(10) 0.84442(5) 0.0268(6) Uani 1 1 d . . . C69 C 0.51010(18) 0.48649(10) 0.83477(5) 0.0294(6) Uani 1 1 d . . . H69A H 0.5448 0.5102 0.8432 0.035 Uiso 1 1 calc R . . C70 C 0.45609(17) 0.49918(9) 0.81359(5) 0.0243(6) Uani 1 1 d . . . C71 C 0.40924(17) 0.46343(9) 0.80114(5) 0.0232(5) Uani 1 1 d . . . H71A H 0.3737 0.4711 0.7861 0.028 Uiso 1 1 calc R . . C72 C 0.41149(16) 0.41678(9) 0.80960(5) 0.0206(5) Uani 1 1 d . . . C73 C 0.36017(18) 0.37916(9) 0.79347(5) 0.0250(6) Uani 1 1 d . . . C74 C 0.3310(2) 0.39788(10) 0.76596(5) 0.0336(7) Uani 1 1 d . . . H74A H 0.3834 0.4097 0.7564 0.050 Uiso 1 1 calc R . . H74B H 0.2878 0.4234 0.7683 0.050 Uiso 1 1 calc R . . H74C H 0.3035 0.3724 0.7557 0.050 Uiso 1 1 calc R . . C75 C 0.27409(18) 0.36512(10) 0.80805(6) 0.0294(6) Uani 1 1 d . . . H75A H 0.2887 0.3545 0.8261 0.044 Uiso 1 1 calc R . . H75B H 0.2446 0.3396 0.7983 0.044 Uiso 1 1 calc R . . H75C H 0.2340 0.3923 0.8091 0.044 Uiso 1 1 calc R . . C76 C 0.4189(2) 0.33578(9) 0.78808(5) 0.0304(6) Uani 1 1 d . . . H76A H 0.4738 0.3455 0.7790 0.046 Uiso 1 1 calc R . . H76B H 0.3861 0.3136 0.7768 0.046 Uiso 1 1 calc R . . H76C H 0.4340 0.3206 0.8050 0.046 Uiso 1 1 calc R . . C77 C 0.44803(18) 0.55089(9) 0.80471(5) 0.0279(6) Uani 1 1 d . . . C78 C 0.4108(3) 0.55522(11) 0.77648(6) 0.0489(9) Uani 1 1 d . . . H78A H 0.4487 0.5375 0.7641 0.073 Uiso 1 1 calc R . . H78B H 0.4099 0.5884 0.7712 0.073 Uiso 1 1 calc R . . H78C H 0.3499 0.5426 0.7760 0.073 Uiso 1 1 calc R . . C79 C 0.3843(2) 0.57630(11) 0.82387(7) 0.0455(8) Uani 1 1 d . . . H79A H 0.3806 0.6096 0.8190 0.068 Uiso 1 1 calc R . . H79B H 0.4068 0.5735 0.8421 0.068 Uiso 1 1 calc R . . H79C H 0.3248 0.5621 0.8227 0.068 Uiso 1 1 calc R . . C80 C 0.5389(2) 0.57573(10) 0.80530(7) 0.0393(7) Uani 1 1 d . . . H80A H 0.5808 0.5591 0.7937 0.059 Uiso 1 1 calc R . . H80B H 0.5620 0.5759 0.8236 0.059 Uiso 1 1 calc R . . H80C H 0.5318 0.6081 0.7990 0.059 Uiso 1 1 calc R . . C81 C 0.5877(2) 0.42845(11) 0.86587(6) 0.0391(8) Uani 1 1 d . . . C82 C 0.6478(2) 0.47120(14) 0.87244(8) 0.0627(12) Uani 1 1 d . . . H82A H 0.6932 0.4619 0.8855 0.094 Uiso 1 1 calc R . . H82B H 0.6111 0.4965 0.8798 0.094 Uiso 1 1 calc R . . H82C H 0.6772 0.4822 0.8561 0.094 Uiso 1 1 calc R . . C83 C 0.6486(2) 0.39057(13) 0.85390(7) 0.0508(9) Uani 1 1 d . . . H83A H 0.6132 0.3625 0.8498 0.076 Uiso 1 1 calc R . . H83B H 0.6955 0.3824 0.8667 0.076 Uiso 1 1 calc R . . H83C H 0.6761 0.4025 0.8375 0.076 Uiso 1 1 calc R . . C84 C 0.5474(2) 0.41236(11) 0.89235(6) 0.0414(8) Uani 1 1 d . . . H84A H 0.5028 0.3879 0.8890 0.062 Uiso 1 1 calc R . . H84B H 0.5188 0.4391 0.9012 0.062 Uiso 1 1 calc R . . H84C H 0.5947 0.3998 0.9038 0.062 Uiso 1 1 calc R . . C85 C 0.5503(2) 0.20930(10) 0.86902(6) 0.0374(7) Uani 1 1 d . . . H85A H 0.4940 0.2006 0.8604 0.056 Uiso 1 1 calc R . . H85B H 0.5469 0.2020 0.8881 0.056 Uiso 1 1 calc R . . H85C H 0.5995 0.1915 0.8610 0.056 Uiso 1 1 calc R . . C86 C 0.66743(19) 0.27609(11) 0.88488(6) 0.0351(7) Uani 1 1 d . . . H86A H 0.6821 0.3094 0.8870 0.053 Uiso 1 1 calc R . . H86B H 0.7174 0.2599 0.8763 0.053 Uiso 1 1 calc R . . H86C H 0.6564 0.2621 0.9024 0.053 Uiso 1 1 calc R . . C87 C 0.7117(3) 0.47792(16) 0.78767(7) 0.0658(11) Uani 1 1 d . . . H87A H 0.6714 0.4776 0.8031 0.099 Uiso 1 1 calc R . . H87B H 0.7445 0.5077 0.7872 0.099 Uiso 1 1 calc R . . H87C H 0.7541 0.4518 0.7891 0.099 Uiso 1 1 calc R . . C88 C 0.6587(2) 0.47279(13) 0.76274(6) 0.0459(8) Uani 1 1 d . . . C89 C 0.6615(2) 0.50658(11) 0.74287(6) 0.0412(8) Uani 1 1 d . . . H89 H 0.6964 0.5341 0.7453 0.049 Uiso 1 1 calc R . . C90 C 0.6138(3) 0.50046(12) 0.71938(7) 0.0516(9) Uani 1 1 d . . . H90 H 0.6154 0.5241 0.7060 0.062 Uiso 1 1 calc R . . C91 C 0.5645(3) 0.46053(14) 0.71537(8) 0.0571(10) Uani 1 1 d . . . H91 H 0.5326 0.4562 0.6992 0.069 Uiso 1 1 calc R . . C92 C 0.5616(2) 0.42665(14) 0.73511(9) 0.0597(10) Uani 1 1 d . . . H92 H 0.5278 0.3988 0.7325 0.072 Uiso 1 1 calc R . . C93 C 0.6072(2) 0.43306(13) 0.75835(8) 0.0534(9) Uani 1 1 d . . . H93 H 0.6035 0.4098 0.7719 0.064 Uiso 1 1 calc R . . C94 C 0.8210(3) 0.03136(16) 0.98200(12) 0.0952(10) Uani 1 1 d . . . H94A H 0.7983 0.0620 0.9878 0.143 Uiso 1 1 calc R . . H94B H 0.8304 0.0112 0.9976 0.143 Uiso 1 1 calc R . . H94C H 0.7774 0.0166 0.9700 0.143 Uiso 1 1 calc R . . C95 C 0.9083(3) 0.03793(14) 0.96747(9) 0.0686(12) Uani 1 1 d . . . C96 C 0.9323(3) 0.08082(13) 0.95754(7) 0.0563(10) Uani 1 1 d . . . H96 H 0.8931 0.1068 0.9596 0.068 Uiso 1 1 calc R . . C97 C 1.0121(3) 0.08677(14) 0.94464(8) 0.0623(11) Uani 1 1 d . . . H97 H 1.0277 0.1169 0.9380 0.075 Uiso 1 1 calc R . . C98 C 1.0700(3) 0.04975(14) 0.94122(7) 0.0579(10) Uani 1 1 d . . . H98 H 1.1248 0.0541 0.9320 0.070 Uiso 1 1 calc R . . C99 C 1.0484(4) 0.00742(16) 0.95109(12) 0.0952(10) Uani 1 1 d . . . H99 H 1.0883 -0.0183 0.9491 0.114 Uiso 1 1 calc R . . C100 C 0.9685(3) 0.00119(16) 0.96409(12) 0.0952(10) Uani 1 1 d . . . H100 H 0.9540 -0.0290 0.9709 0.114 Uiso 1 1 calc R . . C101 C 0.8111(3) 0.3150(2) 0.94603(9) 0.0853(16) Uani 1 1 d . . . H10A H 0.8520 0.3316 0.9340 0.128 Uiso 1 1 calc R . . H10B H 0.7578 0.3053 0.9362 0.128 Uiso 1 1 calc R . . H10C H 0.8410 0.2873 0.9534 0.128 Uiso 1 1 calc R . . C102 C 0.7846(2) 0.34696(15) 0.96816(7) 0.0533(9) Uani 1 1 d . . . C103 C 0.6955(2) 0.35880(14) 0.97213(7) 0.0526(9) Uani 1 1 d . . . H103 H 0.6512 0.3463 0.9606 0.063 Uiso 1 1 calc R . . C104 C 0.6703(2) 0.38856(13) 0.99269(7) 0.0503(9) Uani 1 1 d . . . H104 H 0.6091 0.3963 0.9951 0.060 Uiso 1 1 calc R . . C105 C 0.7342(2) 0.40700(12) 1.00961(7) 0.0487(8) Uani 1 1 d . . . H105 H 0.7173 0.4274 1.0237 0.058 Uiso 1 1 calc R . . C106 C 0.8224(2) 0.39535(14) 1.00575(7) 0.0509(9) Uani 1 1 d . . . H106 H 0.8670 0.4079 1.0172 0.061 Uiso 1 1 calc R . . C107 C 0.8464(2) 0.36580(15) 0.98551(7) 0.0577(10) Uani 1 1 d . . . H107 H 0.9077 0.3580 0.9833 0.069 Uiso 1 1 calc R . . O1 O 0.25650(11) 0.38377(6) 0.93491(3) 0.0207(4) Uani 1 1 d . . . O2 O 0.20456(11) 0.41785(6) 0.88510(3) 0.0222(4) Uani 1 1 d . . . O3 O 0.15478(11) 0.32350(6) 0.90068(3) 0.0196(4) Uani 1 1 d . . . O4 O 0.00096(11) 0.27558(6) 0.88032(3) 0.0204(4) Uani 1 1 d . . . O5 O 0.11551(12) 0.23509(6) 0.91758(3) 0.0232(4) Uani 1 1 d . . . O6 O 0.17269(11) 0.24512(6) 0.86231(3) 0.0212(4) Uani 1 1 d . . . O7 O 0.29902(11) 0.18049(6) 0.84029(3) 0.0216(4) Uani 1 1 d . . . O8 O 0.21308(11) 0.24849(6) 0.80981(3) 0.0214(4) Uani 1 1 d . . . O9 O 0.35482(11) 0.27636(6) 0.84735(3) 0.0213(4) Uani 1 1 d . . . O10 O 0.46002(11) 0.36158(6) 0.84300(3) 0.0213(4) Uani 1 1 d . . . O11 O 0.49720(11) 0.29478(6) 0.88149(3) 0.0233(4) Uani 1 1 d . . . O12 O 0.33929(11) 0.35212(6) 0.88694(3) 0.0218(4) Uani 1 1 d . . . S1 S 0.26815(5) 0.44100(2) 0.864816(13) 0.02580(15) Uani 1 1 d . . . S2 S 0.14950(4) 0.25822(2) 0.943472(13) 0.02603(15) Uani 1 1 d . . . S3 S 0.11298(4) 0.26138(2) 0.810203(12) 0.02280(14) Uani 1 1 d . . . S4 S 0.56969(4) 0.27037(2) 0.864782(13) 0.02496(15) 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 0.0180(4) 0.0173(4) 0.0179(4) -0.0004(3) 0.0022(3) -0.0005(3) Al2 0.0171(4) 0.0171(4) 0.0188(4) 0.0009(3) 0.0006(3) -0.0004(3) Al3 0.0202(4) 0.0166(4) 0.0195(4) 0.0003(3) 0.0007(3) 0.0029(3) Al4 0.0164(4) 0.0183(4) 0.0191(4) 0.0006(3) 0.0016(3) 0.0017(3) C2 0.0197(13) 0.0225(13) 0.0195(12) -0.0033(10) -0.0011(10) -0.0066(10) C3 0.0190(12) 0.0226(13) 0.0208(12) -0.0040(10) -0.0019(10) -0.0018(10) C4 0.0198(13) 0.0291(14) 0.0213(13) -0.0037(11) 0.0001(10) -0.0030(11) C5 0.0229(14) 0.0377(16) 0.0216(13) -0.0002(11) -0.0030(11) -0.0025(12) C6 0.0251(14) 0.0315(15) 0.0236(13) 0.0033(11) -0.0061(11) 0.0021(12) C7 0.0202(13) 0.0266(14) 0.0239(13) -0.0055(11) -0.0018(10) -0.0001(11) C8 0.0219(14) 0.0360(16) 0.0269(14) -0.0026(12) -0.0027(11) 0.0044(12) C9 0.0265(14) 0.0355(16) 0.0285(14) 0.0012(12) -0.0008(12) 0.0086(12) C10 0.0182(14) 0.0454(18) 0.054(2) -0.0038(15) 0.0019(13) -0.0020(13) C11 0.0265(15) 0.056(2) 0.0319(16) -0.0063(14) -0.0063(12) 0.0140(14) C12 0.0315(16) 0.0498(18) 0.0225(14) 0.0090(13) 0.0004(12) 0.0014(14) C16 0.0275(14) 0.0246(14) 0.0229(13) -0.0010(11) 0.0055(11) 0.0042(11) C17 0.0396(17) 0.0307(15) 0.0290(15) -0.0007(12) 0.0069(13) 0.0114(13) C18 0.0410(17) 0.0221(14) 0.0338(16) -0.0002(12) 0.0101(13) 0.0017(12) C19 0.0278(14) 0.0342(15) 0.0228(13) 0.0026(11) 0.0016(11) 0.0092(12) C21 0.0383(18) 0.0455(19) 0.058(2) 0.0312(17) -0.0087(16) -0.0084(15) C22 0.0337(17) 0.0491(19) 0.0423(18) 0.0042(15) 0.0013(14) -0.0161(15) C24 0.0168(12) 0.0249(13) 0.0183(12) -0.0048(10) 0.0025(10) 0.0002(10) C25 0.0201(13) 0.0259(14) 0.0230(13) -0.0023(10) 0.0036(10) -0.0019(11) C26 0.0218(13) 0.0307(15) 0.0278(14) -0.0060(11) 0.0063(11) -0.0076(11) C27 0.0198(13) 0.0444(17) 0.0202(13) -0.0041(12) 0.0027(10) -0.0054(12) C28 0.0219(14) 0.0360(15) 0.0220(13) 0.0020(11) 0.0018(11) -0.0012(12) C29 0.0146(12) 0.0263(13) 0.0218(13) -0.0012(10) 0.0035(10) -0.0003(10) C30 0.0222(13) 0.0237(14) 0.0282(14) 0.0024(11) -0.0030(11) 0.0031(11) C31 0.0320(16) 0.0313(16) 0.0410(17) 0.0061(13) -0.0028(13) 0.0060(13) C32 0.0260(14) 0.0192(13) 0.0366(15) 0.0035(11) -0.0029(12) -0.0016(11) C33 0.0331(15) 0.0263(15) 0.0354(16) -0.0060(12) 0.0005(13) 0.0059(12) C34 0.0274(15) 0.0541(19) 0.0221(14) -0.0046(13) 0.0011(12) -0.0117(14) C35 0.0295(15) 0.062(2) 0.0245(15) -0.0079(14) 0.0006(12) -0.0098(15) C36 0.0238(15) 0.090(3) 0.0247(15) -0.0054(16) -0.0021(12) -0.0017(16) C37 0.048(2) 0.077(3) 0.0302(17) -0.0053(16) -0.0063(15) -0.0300(19) C38 0.0249(14) 0.0237(14) 0.0337(15) 0.0006(11) 0.0004(11) -0.0061(11) C39 0.0333(16) 0.0245(15) 0.0419(17) 0.0041(12) 0.0009(13) -0.0024(12) C40 0.0295(15) 0.0325(15) 0.0281(14) 0.0068(12) 0.0011(12) -0.0069(12) C41 0.0348(16) 0.0288(15) 0.0397(17) 0.0022(13) 0.0012(13) -0.0115(13) C43 0.0346(16) 0.0330(16) 0.0259(14) -0.0051(12) 0.0047(12) -0.0029(13) C44 0.052(2) 0.0456(19) 0.0284(16) 0.0139(14) 0.0014(14) 0.0030(16) C46 0.0221(13) 0.0133(12) 0.0261(13) -0.0020(10) -0.0049(10) 0.0018(10) C47 0.0286(14) 0.0153(12) 0.0285(14) -0.0027(10) -0.0047(11) 0.0004(10) C48 0.0342(15) 0.0207(13) 0.0308(15) 0.0000(11) -0.0112(12) 0.0051(12) C49 0.0311(15) 0.0203(14) 0.0390(16) -0.0039(12) -0.0072(12) 0.0060(11) C50 0.0269(14) 0.0213(13) 0.0343(15) -0.0057(11) 0.0015(12) 0.0034(11) C51 0.0243(13) 0.0179(13) 0.0286(14) -0.0034(10) -0.0025(11) 0.0002(11) C52 0.0259(14) 0.0200(13) 0.0245(13) -0.0037(10) 0.0004(11) 0.0018(11) C53 0.0293(15) 0.0280(14) 0.0263(14) -0.0024(11) -0.0008(11) 0.0008(12) C54 0.0251(14) 0.0245(14) 0.0273(14) -0.0015(11) 0.0023(11) -0.0007(11) C55 0.0356(16) 0.0265(14) 0.0310(15) -0.0034(12) 0.0043(12) 0.0029(12) C56 0.0318(16) 0.0267(15) 0.0490(18) -0.0033(13) -0.0092(14) 0.0103(12) C60 0.0312(15) 0.0243(14) 0.0225(13) 0.0029(11) -0.0034(11) 0.0039(11) C61 0.0466(18) 0.0349(16) 0.0269(15) 0.0051(12) -0.0044(13) 0.0063(14) C62 0.0338(15) 0.0276(14) 0.0273(14) 0.0044(11) 0.0016(12) -0.0007(12) C63 0.0329(15) 0.0303(15) 0.0249(14) -0.0056(11) -0.0039(12) 0.0065(12) C64 0.0331(16) 0.0435(18) 0.0272(15) 0.0107(13) -0.0079(12) -0.0003(13) C65 0.0300(15) 0.0306(15) 0.0357(16) -0.0036(12) 0.0028(12) -0.0062(12) C67 0.0174(12) 0.0230(13) 0.0228(13) 0.0016(10) 0.0070(10) -0.0014(10) C68 0.0207(13) 0.0327(15) 0.0269(14) 0.0056(11) 0.0006(11) -0.0061(11) C69 0.0282(15) 0.0301(15) 0.0298(15) 0.0000(12) 0.0013(12) -0.0108(12) C70 0.0242(13) 0.0222(13) 0.0267(14) 0.0009(11) 0.0066(11) -0.0026(11) C71 0.0222(13) 0.0239(13) 0.0236(13) 0.0010(11) 0.0038(10) 0.0016(11) C72 0.0189(12) 0.0214(13) 0.0214(13) 0.0008(10) 0.0028(10) 0.0014(10) C73 0.0302(14) 0.0189(13) 0.0260(14) 0.0003(10) -0.0033(11) 0.0016(11) C74 0.0469(18) 0.0250(15) 0.0290(15) 0.0009(12) -0.0086(13) -0.0012(13) C75 0.0291(15) 0.0244(14) 0.0347(15) 0.0024(12) -0.0045(12) -0.0031(11) C76 0.0425(17) 0.0229(14) 0.0257(14) -0.0026(11) -0.0008(12) 0.0038(12) C77 0.0318(15) 0.0221(14) 0.0299(14) 0.0030(11) 0.0052(12) -0.0031(11) C78 0.074(2) 0.0262(16) 0.0462(19) 0.0168(14) -0.0125(18) -0.0124(16) C79 0.0458(19) 0.0265(16) 0.064(2) 0.0096(15) 0.0227(17) 0.0044(14) C80 0.0363(17) 0.0236(15) 0.058(2) 0.0035(14) 0.0076(15) -0.0061(13) C81 0.0296(16) 0.0457(19) 0.0421(17) 0.0169(14) -0.0123(13) -0.0179(14) C82 0.052(2) 0.069(3) 0.067(3) 0.031(2) -0.0350(19) -0.037(2) C83 0.0212(15) 0.069(2) 0.062(2) 0.0302(19) -0.0070(15) -0.0030(16) C84 0.0445(19) 0.0420(18) 0.0378(17) 0.0079(14) -0.0168(14) -0.0177(15) C85 0.0367(17) 0.0303(16) 0.0453(18) -0.0067(13) -0.0094(14) 0.0061(13) C86 0.0249(15) 0.0389(17) 0.0415(17) -0.0013(13) -0.0093(13) 0.0056(13) C87 0.059(2) 0.088(3) 0.050(2) 0.003(2) -0.0025(19) 0.021(2) C88 0.0396(18) 0.060(2) 0.0380(18) 0.0030(16) 0.0106(14) 0.0181(17) C89 0.0461(19) 0.0366(17) 0.0408(18) -0.0042(14) 0.0073(15) 0.0067(14) C90 0.072(3) 0.043(2) 0.0396(19) -0.0020(15) 0.0100(18) 0.0190(19) C91 0.056(2) 0.065(3) 0.050(2) -0.0171(19) 0.0018(18) 0.009(2) C92 0.045(2) 0.057(2) 0.077(3) -0.011(2) 0.018(2) -0.0057(18) C93 0.047(2) 0.051(2) 0.062(2) 0.0121(18) 0.0249(19) 0.0029(17) C94 0.094(2) 0.0509(15) 0.141(3) 0.0088(16) 0.057(2) 0.0137(15) C95 0.072(3) 0.051(2) 0.083(3) 0.003(2) 0.026(2) 0.010(2) C96 0.076(3) 0.041(2) 0.052(2) -0.0013(17) -0.010(2) 0.0146(19) C97 0.077(3) 0.053(2) 0.056(2) 0.0063(19) -0.008(2) -0.006(2) C98 0.070(3) 0.057(2) 0.048(2) -0.0066(18) 0.0022(19) -0.004(2) C99 0.094(2) 0.0509(15) 0.141(3) 0.0088(16) 0.057(2) 0.0137(15) C100 0.094(2) 0.0509(15) 0.141(3) 0.0088(16) 0.057(2) 0.0137(15) C101 0.041(2) 0.145(5) 0.070(3) -0.041(3) 0.000(2) -0.008(3) C102 0.0363(19) 0.079(3) 0.045(2) -0.0086(18) -0.0006(15) -0.0049(18) C103 0.0362(19) 0.071(3) 0.051(2) -0.0005(18) -0.0068(16) -0.0034(17) C104 0.0383(19) 0.053(2) 0.059(2) 0.0083(18) -0.0001(16) 0.0029(16) C105 0.056(2) 0.043(2) 0.048(2) 0.0046(16) 0.0004(17) 0.0007(17) C106 0.0383(19) 0.073(3) 0.0416(19) -0.0036(18) -0.0034(15) -0.0034(18) C107 0.0360(19) 0.086(3) 0.051(2) -0.011(2) -0.0029(16) -0.0011(19) O1 0.0200(9) 0.0228(9) 0.0192(8) -0.0020(7) 0.0027(7) -0.0022(7) O2 0.0219(9) 0.0215(9) 0.0233(9) 0.0031(7) 0.0046(7) 0.0008(7) O3 0.0188(9) 0.0194(9) 0.0205(9) -0.0001(7) 0.0013(7) -0.0009(7) O4 0.0176(8) 0.0214(9) 0.0223(9) -0.0013(7) -0.0008(7) -0.0014(7) O5 0.0276(10) 0.0215(9) 0.0206(9) 0.0019(7) -0.0007(7) -0.0012(8) O6 0.0232(9) 0.0197(9) 0.0206(9) 0.0006(7) 0.0020(7) 0.0015(7) O7 0.0228(9) 0.0182(9) 0.0238(9) -0.0002(7) -0.0005(7) 0.0041(7) O8 0.0195(9) 0.0239(9) 0.0207(9) 0.0008(7) 0.0011(7) 0.0024(7) O9 0.0235(9) 0.0198(9) 0.0208(9) -0.0008(7) 0.0013(7) 0.0014(7) O10 0.0191(9) 0.0225(9) 0.0222(9) 0.0040(7) 0.0024(7) 0.0005(7) O11 0.0219(9) 0.0280(10) 0.0200(9) 0.0011(7) 0.0013(7) 0.0063(8) O12 0.0195(9) 0.0230(9) 0.0227(9) -0.0032(7) 0.0028(7) -0.0007(7) S1 0.0302(4) 0.0229(3) 0.0243(3) 0.0026(3) 0.0080(3) -0.0010(3) S2 0.0263(3) 0.0313(4) 0.0205(3) 0.0041(3) -0.0017(3) -0.0030(3) S3 0.0211(3) 0.0229(3) 0.0244(3) -0.0010(3) -0.0013(3) 0.0039(3) S4 0.0219(3) 0.0297(4) 0.0232(3) -0.0014(3) -0.0008(3) 0.0068(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.7006(18) . ? Al1 O12 1.7024(18) . ? Al1 O1 1.7543(17) . ? Al1 O2 1.8673(18) . ? Al2 O6 1.6934(18) . ? Al2 O3 1.7082(18) . ? Al2 O4 1.7510(18) . ? Al2 O5 1.8711(18) . ? Al3 O9 1.6967(18) . ? Al3 O6 1.7131(18) . ? Al3 O7 1.7469(17) . ? Al3 O8 1.8826(18) . ? Al4 O12 1.6934(17) . ? Al4 O9 1.7065(18) . ? Al4 O10 1.7578(18) . ? Al4 O11 1.8808(18) . ? C2 O1 1.343(3) . ? C2 C3 1.418(3) . ? C2 C7 1.424(4) . ? C3 C4 1.397(3) . ? C3 C16 1.540(4) . ? C4 C5 1.385(4) . ? C4 H4A 0.9500 . ? C5 C6 1.389(4) . ? C5 C12 1.541(4) . ? C6 C7 1.395(4) . ? C6 H6A 0.9500 . ? C7 C8 1.552(4) . ? C8 C9 1.536(4) . ? C8 C11 1.539(4) . ? C8 C10 1.541(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.514(5) . ? C12 C13 1.515(6) . ? C12 C14B 1.527(5) . ? C12 C14 1.542(5) . ? C12 C15B 1.544(5) . ? C12 C13B 1.551(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16 C19 1.539(4) . ? C16 C18 1.540(4) . ? C16 C17 1.541(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 S1 1.772(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 S1 1.769(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 O4 1.342(3) . ? C24 C25 1.415(3) . ? C24 C29 1.423(4) . ? C25 C26 1.403(4) . ? C25 C38 1.545(4) . ? C26 C27 1.377(4) . ? C26 H26A 0.9500 . ? C27 C28 1.392(4) . ? C27 C34 1.542(4) . ? C28 C29 1.393(4) . ? C28 H28A 0.9500 . ? C29 C30 1.544(4) . ? C30 C31 1.540(3) . ? C30 C32 1.541(3) . ? C30 C33 1.544(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C37 1.523(4) . ? C34 C36 1.534(5) . ? C34 C35 1.534(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C41 1.533(4) . ? C38 C39 1.535(4) . ? C38 C40 1.537(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C43 S2 1.779(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 S2 1.785(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C46 O7 1.341(3) . ? C46 C47 1.422(4) . ? C46 C51 1.424(4) . ? C47 C48 1.394(4) . ? C47 C60 1.542(4) . ? C48 C49 1.388(4) . ? C48 H48A 0.9500 . ? C49 C50 1.385(4) . ? C49 C56 1.536(4) . ? C50 C51 1.398(4) . ? C50 H50A 0.9500 . ? C51 C52 1.546(4) . ? C52 C54 1.536(4) . ? C52 C55 1.538(4) . ? C52 C53 1.539(4) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57A 1.523(4) . ? C56 C58C 1.530(3) . ? C56 C59B 1.531(5) . ? C56 C59A 1.540(4) . ? C56 C58A 1.544(4) . ? C56 C58B 1.548(5) . ? C56 C57B 1.549(5) . ? C56 C57C 1.550(5) . ? C56 C59C 1.569(10) . ? C57A H57A 0.9800 . ? C57A H57B 0.9800 . ? C57A H57C 0.9800 . ? C58A H58A 0.9800 . ? C58A H58B 0.9800 . ? C58A H58C 0.9800 . ? C59A H59A 0.9800 . ? C59A H59B 0.9800 . ? C59A H59C 0.9800 . ? C57B H57D 0.9800 . ? C57B H57E 0.9800 . ? C57B H57F 0.9800 . ? C58B H58D 0.9800 . ? C58B H58E 0.9800 . ? C58B H58F 0.9800 . ? C59B H59D 0.9800 . ? C59B H59E 0.9800 . ? C59B H59F 0.9800 . ? C57C H57G 0.9800 . ? C57C H57H 0.9800 . ? C57C H57I 0.9800 . ? C58C H58G 0.9800 . ? C58C H58H 0.9800 . ? C58C H58I 0.9800 . ? C59C H59G 0.9800 . ? C59C H59H 0.9800 . ? C59C H59I 0.9800 . ? C60 C62 1.537(4) . ? C60 C61 1.540(4) . ? C60 C63 1.544(4) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 S3 1.782(3) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 S3 1.773(3) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C67 O10 1.350(3) . ? C67 C68 1.421(4) . ? C67 C72 1.422(3) . ? C68 C69 1.392(4) . ? C68 C81 1.557(4) . ? C69 C70 1.383(4) . ? C69 H69A 0.9500 . ? C70 C71 1.385(4) . ? C70 C77 1.542(4) . ? C71 C72 1.394(4) . ? C71 H71A 0.9500 . ? C72 C73 1.546(4) . ? C73 C75 1.534(4) . ? C73 C76 1.539(4) . ? C73 C74 1.542(4) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.528(4) . ? C77 C80 1.532(4) . ? C77 C79 1.535(4) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C84 1.530(4) . ? C81 C83 1.534(5) . ? C81 C82 1.548(4) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 S4 1.775(3) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 S4 1.784(3) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.489(5) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 C93 1.386(5) . ? C88 C89 1.386(5) . ? C89 C90 1.389(5) . ? C89 H89 0.9500 . ? C90 C91 1.370(5) . ? C90 H90 0.9500 . ? C91 C92 1.383(6) . ? C91 H91 0.9500 . ? C92 C93 1.363(5) . ? C92 H92 0.9500 . ? C93 H93 0.9500 . ? C94 C95 1.508(6) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 C96 1.367(5) . ? C95 C100 1.391(6) . ? C96 C97 1.369(6) . ? C96 H96 0.9500 . ? C97 C98 1.375(6) . ? C97 H97 0.9500 . ? C98 C99 1.342(6) . ? C98 H98 0.9500 . ? C99 C100 1.373(6) . ? C99 H99 0.9500 . ? C100 H100 0.9500 . ? C101 C102 1.489(5) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C107 1.379(5) . ? C102 C103 1.390(5) . ? C103 C104 1.387(5) . ? C103 H103 0.9500 . ? C104 C105 1.382(5) . ? C104 H104 0.9500 . ? C105 C106 1.376(5) . ? C105 H105 0.9500 . ? C106 C107 1.366(5) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? O2 S1 1.5415(17) . ? O5 S2 1.5430(18) . ? O8 S3 1.5423(17) . ? O11 S4 1.5370(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O12 120.89(9) . . ? O3 Al1 O1 112.06(8) . . ? O12 Al1 O1 111.27(9) . . ? O3 Al1 O2 108.34(8) . . ? O12 Al1 O2 100.77(8) . . ? O1 Al1 O2 100.82(8) . . ? O6 Al2 O3 120.91(9) . . ? O6 Al2 O4 112.18(9) . . ? O3 Al2 O4 111.78(9) . . ? O6 Al2 O5 109.72(8) . . ? O3 Al2 O5 98.81(8) . . ? O4 Al2 O5 100.52(8) . . ? O9 Al3 O6 120.72(9) . . ? O9 Al3 O7 113.23(9) . . ? O6 Al3 O7 111.49(9) . . ? O9 Al3 O8 110.67(8) . . ? O6 Al3 O8 97.48(8) . . ? O7 Al3 O8 100.01(8) . . ? O12 Al4 O9 119.81(9) . . ? O12 Al4 O10 112.13(9) . . ? O9 Al4 O10 113.66(9) . . ? O12 Al4 O11 107.52(9) . . ? O9 Al4 O11 101.69(9) . . ? O10 Al4 O11 98.96(8) . . ? O1 C2 C3 120.7(2) . . ? O1 C2 C7 119.9(2) . . ? C3 C2 C7 119.2(2) . . ? C4 C3 C2 118.2(2) . . ? C4 C3 C16 119.6(2) . . ? C2 C3 C16 122.2(2) . . ? C5 C4 C3 123.2(2) . . ? C5 C4 H4A 118.4 . . ? C3 C4 H4A 118.4 . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C12 122.4(2) . . ? C6 C5 C12 120.7(2) . . ? C5 C6 C7 123.4(2) . . ? C5 C6 H6A 118.3 . . ? C7 C6 H6A 118.3 . . ? C6 C7 C2 117.9(2) . . ? C6 C7 C8 120.2(2) . . ? C2 C7 C8 121.7(2) . . ? C9 C8 C11 106.7(2) . . ? C9 C8 C10 109.7(2) . . ? C11 C8 C10 106.5(2) . . ? C9 C8 C7 113.0(2) . . ? C11 C8 C7 111.5(2) . . ? C10 C8 C7 109.4(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10D 109.5 . . ? C8 C10 H10E 109.5 . . ? H10D C10 H10E 109.5 . . ? C8 C10 H10F 109.5 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 109.2(3) . . ? C15 C12 C14B 59.4(6) . . ? C13 C12 C14B 137.8(7) . . ? C15 C12 C5 113.2(3) . . ? C13 C12 C5 110.0(3) . . ? C14B C12 C5 111.6(6) . . ? C15 C12 C14 106.3(3) . . ? C13 C12 C14 108.7(3) . . ? C14B C12 C14 50.0(6) . . ? C5 C12 C14 109.3(3) . . ? C15 C12 C15B 48.0(6) . . ? C13 C12 C15B 66.7(6) . . ? C14B C12 C15B 105.8(9) . . ? C5 C12 C15B 108.2(6) . . ? C14 C12 C15B 141.2(6) . . ? C15 C12 C13B 129.2(7) . . ? C14B C12 C13B 124.3(9) . . ? C5 C12 C13B 110.2(6) . . ? C14 C12 C13B 82.3(7) . . ? C15B C12 C13B 94.1(9) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? C12 C13B H13D 109.5 . . ? C12 C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12 C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12 C14B H14D 109.5 . . ? C12 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C12 C15B H15D 109.5 . . ? C12 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C12 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C19 C16 C18 111.3(2) . . ? C19 C16 C3 110.8(2) . . ? C18 C16 C3 110.5(2) . . ? C19 C16 C17 106.9(2) . . ? C18 C16 C17 105.4(2) . . ? C3 C16 C17 111.8(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S1 C21 H21A 109.5 . . ? S1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S1 C22 H22A 109.5 . . ? S1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C24 C25 120.8(2) . . ? O4 C24 C29 120.0(2) . . ? C25 C24 C29 119.2(2) . . ? C26 C25 C24 118.4(2) . . ? C26 C25 C38 119.8(2) . . ? C24 C25 C38 121.8(2) . . ? C27 C26 C25 123.3(2) . . ? C27 C26 H26A 118.4 . . ? C25 C26 H26A 118.4 . . ? C26 C27 C28 116.8(2) . . ? C26 C27 C34 124.3(3) . . ? C28 C27 C34 118.9(3) . . ? C27 C28 C29 123.5(3) . . ? C27 C28 H28A 118.3 . . ? C29 C28 H28A 118.3 . . ? C28 C29 C24 118.1(2) . . ? C28 C29 C30 119.8(2) . . ? C24 C29 C30 121.9(2) . . ? C31 C30 C32 106.1(2) . . ? C31 C30 C33 107.0(2) . . ? C32 C30 C33 109.6(2) . . ? C31 C30 C29 111.6(2) . . ? C32 C30 C29 113.4(2) . . ? C33 C30 C29 109.0(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C37 C34 C36 109.2(3) . . ? C37 C34 C35 108.4(3) . . ? C36 C34 C35 109.2(3) . . ? C37 C34 C27 112.0(3) . . ? C36 C34 C27 110.0(2) . . ? C35 C34 C27 108.0(2) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C41 C38 C39 106.7(2) . . ? C41 C38 C40 106.3(2) . . ? C39 C38 C40 111.2(2) . . ? C41 C38 C25 111.9(2) . . ? C39 C38 C25 110.2(2) . . ? C40 C38 C25 110.4(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S2 C43 H43A 109.5 . . ? S2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? S2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? S2 C44 H44A 109.5 . . ? S2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? S2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O7 C46 C47 120.4(2) . . ? O7 C46 C51 120.1(2) . . ? C47 C46 C51 119.5(2) . . ? C48 C47 C46 118.2(2) . . ? C48 C47 C60 119.4(2) . . ? C46 C47 C60 122.3(2) . . ? C49 C48 C47 123.5(3) . . ? C49 C48 H48A 118.3 . . ? C47 C48 H48A 118.3 . . ? C50 C49 C48 117.0(2) . . ? C50 C49 C56 122.7(3) . . ? C48 C49 C56 120.3(2) . . ? C49 C50 C51 123.3(3) . . ? C49 C50 H50A 118.4 . . ? C51 C50 H50A 118.4 . . ? C50 C51 C46 118.3(2) . . ? C50 C51 C52 119.9(2) . . ? C46 C51 C52 121.8(2) . . ? C54 C52 C55 106.4(2) . . ? C54 C52 C53 111.6(2) . . ? C55 C52 C53 106.7(2) . . ? C54 C52 C51 109.9(2) . . ? C55 C52 C51 112.3(2) . . ? C53 C52 C51 110.0(2) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57A C56 C58C 86.5(5) . . ? C57A C56 C59B 55.5(9) . . ? C58C C56 C59B 132.3(9) . . ? C57A C56 C49 114.1(4) . . ? C58C C56 C49 108.6(4) . . ? C59B C56 C49 112.7(8) . . ? C57A C56 C59A 107.6(5) . . ? C58C C56 C59A 128.8(5) . . ? C59B C56 C59A 55.3(9) . . ? C49 C56 C59A 109.3(3) . . ? C57A C56 C58A 110.3(5) . . ? C59B C56 C58A 138.6(9) . . ? C49 C56 C58A 108.4(3) . . ? C59A C56 C58A 106.9(4) . . ? C57A C56 C58B 122.8(10) . . ? C58C C56 C58B 47.9(10) . . ? C59B C56 C58B 127.8(12) . . ? C49 C56 C58B 112.5(9) . . ? C59A C56 C58B 86.0(10) . . ? C59B C56 C57B 96.4(12) . . ? C49 C56 C57B 108.3(8) . . ? C59A C56 C57B 139.6(9) . . ? C58A C56 C57B 74.1(9) . . ? C58B C56 C57B 93.0(13) . . ? C58C C56 C57C 104.2(6) . . ? C49 C56 C57C 110.3(4) . . ? C59A C56 C57C 93.6(5) . . ? C58A C56 C57C 126.5(5) . . ? C58B C56 C57C 134.7(10) . . ? C57B C56 C57C 59.6(9) . . ? C57A C56 C59C 118.0(6) . . ? C58C C56 C59C 115.0(6) . . ? C59B C56 C59C 69.8(10) . . ? C49 C56 C59C 112.0(5) . . ? C58A C56 C59C 91.3(5) . . ? C58B C56 C59C 70.2(11) . . ? C57B C56 C59C 139.6(9) . . ? C57C C56 C59C 106.5(6) . . ? C56 C57A H57A 109.5 . . ? C56 C57A H57B 109.5 . . ? C56 C57A H57C 109.5 . . ? C56 C58A H58A 109.5 . . ? C56 C58A H58B 109.5 . . ? C56 C58A H58C 109.5 . . ? C56 C59A H59A 109.5 . . ? C56 C59A H59B 109.5 . . ? C56 C59A H59C 109.5 . . ? C56 C57B H57D 109.5 . . ? C56 C57B H57E 109.5 . . ? H57D C57B H57E 109.5 . . ? C56 C57B H57F 109.5 . . ? H57D C57B H57F 109.5 . . ? H57E C57B H57F 109.5 . . ? C56 C58B H58D 109.5 . . ? C56 C58B H58E 109.5 . . ? H58D C58B H58E 109.5 . . ? C56 C58B H58F 109.5 . . ? H58D C58B H58F 109.5 . . ? H58E C58B H58F 109.5 . . ? C56 C59B H59D 109.5 . . ? C56 C59B H59E 109.5 . . ? H59D C59B H59E 109.5 . . ? C56 C59B H59F 109.5 . . ? H59D C59B H59F 109.5 . . ? H59E C59B H59F 109.5 . . ? C56 C57C H57G 109.5 . . ? C56 C57C H57H 109.5 . . ? C56 C57C H57I 109.5 . . ? C56 C58C H58G 109.5 . . ? C56 C58C H58H 109.5 . . ? C56 C58C H58I 109.5 . . ? C56 C59C H59G 109.5 . . ? C56 C59C H59H 109.5 . . ? C56 C59C H59I 109.5 . . ? C62 C60 C61 105.5(2) . . ? C62 C60 C47 111.0(2) . . ? C61 C60 C47 112.5(2) . . ? C62 C60 C63 111.0(2) . . ? C61 C60 C63 106.6(2) . . ? C47 C60 C63 110.0(2) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? S3 C64 H64A 109.5 . . ? S3 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? S3 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? S3 C65 H65A 109.5 . . ? S3 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? S3 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O10 C67 C68 120.5(2) . . ? O10 C67 C72 120.8(2) . . ? C68 C67 C72 118.6(2) . . ? C69 C68 C67 118.7(2) . . ? C69 C68 C81 119.7(2) . . ? C67 C68 C81 121.4(2) . . ? C70 C69 C68 123.4(3) . . ? C70 C69 H69A 118.3 . . ? C68 C69 H69A 118.3 . . ? C69 C70 C71 116.8(2) . . ? C69 C70 C77 121.1(2) . . ? C71 C70 C77 122.1(2) . . ? C70 C71 C72 123.4(2) . . ? C70 C71 H71A 118.3 . . ? C72 C71 H71A 118.3 . . ? C71 C72 C67 118.6(2) . . ? C71 C72 C73 119.2(2) . . ? C67 C72 C73 122.2(2) . . ? C75 C73 C76 110.7(2) . . ? C75 C73 C74 106.2(2) . . ? C76 C73 C74 106.3(2) . . ? C75 C73 C72 110.3(2) . . ? C76 C73 C72 111.3(2) . . ? C74 C73 C72 111.7(2) . . ? 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 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C80 107.7(2) . . ? C78 C77 C79 108.4(3) . . ? C80 C77 C79 108.8(2) . . ? C78 C77 C70 111.9(2) . . ? C80 C77 C70 111.4(2) . . ? C79 C77 C70 108.5(2) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C84 C81 C83 111.4(3) . . ? C84 C81 C82 106.2(3) . . ? C83 C81 C82 106.9(3) . . ? C84 C81 C68 113.4(2) . . ? C83 C81 C68 107.2(3) . . ? C82 C81 C68 111.7(2) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? S4 C85 H85A 109.5 . . ? S4 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? S4 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? S4 C86 H86A 109.5 . . ? S4 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? S4 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C93 C88 C89 118.0(3) . . ? C93 C88 C87 120.7(3) . . ? C89 C88 C87 121.3(4) . . ? C88 C89 C90 120.5(3) . . ? C88 C89 H89 119.7 . . ? C90 C89 H89 119.7 . . ? C91 C90 C89 120.4(3) . . ? C91 C90 H90 119.8 . . ? C89 C90 H90 119.8 . . ? C90 C91 C92 119.3(4) . . ? C90 C91 H91 120.3 . . ? C92 C91 H91 120.3 . . ? C93 C92 C91 120.3(4) . . ? C93 C92 H92 119.9 . . ? C91 C92 H92 119.9 . . ? C92 C93 C88 121.6(3) . . ? C92 C93 H93 119.2 . . ? C88 C93 H93 119.2 . . ? C95 C94 H94A 109.5 . . ? C95 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C95 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C96 C95 C100 117.2(4) . . ? C96 C95 C94 121.0(4) . . ? C100 C95 C94 121.8(4) . . ? C95 C96 C97 120.8(4) . . ? C95 C96 H96 119.6 . . ? C97 C96 H96 119.6 . . ? C96 C97 C98 120.9(4) . . ? C96 C97 H97 119.5 . . ? C98 C97 H97 119.5 . . ? C99 C98 C97 119.3(4) . . ? C99 C98 H98 120.3 . . ? C97 C98 H98 120.3 . . ? C98 C99 C100 120.1(4) . . ? C98 C99 H99 120.0 . . ? C100 C99 H99 120.0 . . ? C99 C100 C95 121.7(4) . . ? C99 C100 H100 119.2 . . ? C95 C100 H100 119.2 . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C107 C102 C103 117.3(3) . . ? C107 C102 C101 122.0(3) . . ? C103 C102 C101 120.7(3) . . ? C104 C103 C102 121.0(3) . . ? C104 C103 H103 119.5 . . ? C102 C103 H103 119.5 . . ? C105 C104 C103 120.1(3) . . ? C105 C104 H104 120.0 . . ? C103 C104 H104 120.0 . . ? C106 C105 C104 119.1(3) . . ? C106 C105 H105 120.5 . . ? C104 C105 H105 120.5 . . ? C107 C106 C105 120.3(3) . . ? C107 C106 H106 119.8 . . ? C105 C106 H106 119.8 . . ? C106 C107 C102 122.2(3) . . ? C106 C107 H107 118.9 . . ? C102 C107 H107 118.9 . . ? C2 O1 Al1 140.95(16) . . ? S1 O2 Al1 119.31(10) . . ? Al1 O3 Al2 146.76(11) . . ? C24 O4 Al2 144.50(16) . . ? S2 O5 Al2 116.62(10) . . ? Al2 O6 Al3 150.12(11) . . ? C46 O7 Al3 147.14(16) . . ? S3 O8 Al3 116.01(10) . . ? Al3 O9 Al4 148.36(11) . . ? C67 O10 Al4 144.14(16) . . ? S4 O11 Al4 118.67(10) . . ? Al4 O12 Al1 150.51(11) . . ? O2 S1 C22 104.64(12) . . ? O2 S1 C21 102.16(13) . . ? C22 S1 C21 98.67(17) . . ? O5 S2 C43 104.71(12) . . ? O5 S2 C44 101.82(13) . . ? C43 S2 C44 99.06(15) . . ? O8 S3 C65 104.98(12) . . ? O8 S3 C64 102.13(12) . . ? C65 S3 C64 97.89(14) . . ? O11 S4 C85 105.20(13) . . ? O11 S4 C86 103.23(12) . . ? C85 S4 C86 98.94(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.636 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.059 #===END data_bt1044 _database_code_depnum_ccdc_archive 'CCDC 739387' # Compound 7a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Bert*OH + DMSO' _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 O, C2 H6 O S' _chemical_formula_sum 'C38 H56 O2 S' _chemical_formula_weight 576.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7515(5) _cell_length_b 16.8969(6) _cell_length_c 16.9967(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.505(1) _cell_angle_gamma 90.00 _cell_volume 3511.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8760 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.01 _exptl_crystal_description fragment _exptl_crystal_colour 'clear colorless' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.954 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS-2004/1 ; Bruker, 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54056 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6371 _reflns_number_gt 5653 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker, 2006; SMART v. 5.632' _computing_cell_refinement 'Bruker, 2006; SAINT+ v. 7.23a' _computing_data_reduction 'Bruker, 2006; SAINT+ v. 7.23a' _computing_structure_solution 'Bruker, 2003; XS, SHELXTL v. 6.14' _computing_structure_refinement "Bruker, 2003; XL,SHELXTL v. 6.14'" _computing_molecular_graphics 'Bruker, 2003; XP, SHELXTL v. 6.14' _computing_publication_material 'Bruker, 2001; XCIF, SHELXTL, v. 6.14' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.9775P] 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 6371 _refine_ls_number_parameters 396 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.14183(11) 0.29036(8) 0.19932(8) 0.0174(3) Uani 1 1 d . . . C2 C 0.24273(11) 0.30090(8) 0.25838(8) 0.0171(3) Uani 1 1 d . . . C3 C 0.26860(11) 0.25150(8) 0.32694(8) 0.0195(3) Uani 1 1 d . . . H3 H 0.3357 0.2589 0.3684 0.023 Uiso 1 1 calc R . . C4 C 0.19803(11) 0.19180(8) 0.33568(8) 0.0211(3) Uani 1 1 d . . . H4 H 0.2167 0.1588 0.3829 0.025 Uiso 1 1 calc R . . C5 C 0.10023(11) 0.18059(8) 0.27517(8) 0.0197(3) Uani 1 1 d . . . H5 H 0.0529 0.1388 0.2805 0.024 Uiso 1 1 calc R . . C6 C 0.07042(11) 0.22977(8) 0.20655(8) 0.0176(3) Uani 1 1 d . . . C7 C -0.03714(11) 0.22042(8) 0.14258(8) 0.0182(3) Uani 1 1 d . A . C8 C -0.13226(11) 0.25082(9) 0.15735(9) 0.0213(3) Uani 1 1 d D . . C9 C -0.23201(11) 0.23995(9) 0.09831(9) 0.0234(3) Uani 1 1 d . A . H9 H -0.2962 0.2613 0.1080 0.028 Uiso 1 1 calc R . . C10 C -0.24138(11) 0.19915(9) 0.02574(9) 0.0222(3) Uani 1 1 d . . . C11 C -0.14599(11) 0.17055(8) 0.01176(8) 0.0213(3) Uani 1 1 d . A . H11 H -0.1506 0.1428 -0.0377 0.026 Uiso 1 1 calc R . . C12 C -0.04359(11) 0.18150(8) 0.06833(8) 0.0192(3) Uani 1 1 d . . . C13 C 0.31937(11) 0.36352(8) 0.24535(8) 0.0178(3) Uani 1 1 d . . . C14 C 0.32630(11) 0.43731(8) 0.28498(8) 0.0201(3) Uani 1 1 d . . . C15 C 0.39445(11) 0.49527(8) 0.26796(9) 0.0213(3) Uani 1 1 d . . . H15 H 0.3992 0.5450 0.2948 0.026 Uiso 1 1 calc R . . C16 C 0.45576(11) 0.48306(8) 0.21318(8) 0.0204(3) Uani 1 1 d . . . C17 C 0.44839(11) 0.40950(8) 0.17535(8) 0.0209(3) Uani 1 1 d . . . H17 H 0.4905 0.3998 0.1383 0.025 Uiso 1 1 calc R . . C18 C 0.38113(11) 0.34948(8) 0.19002(8) 0.0189(3) Uani 1 1 d . . . C19 C 0.37644(12) 0.27077(8) 0.14538(9) 0.0215(3) Uani 1 1 d . . . H19 H 0.3289 0.2341 0.1663 0.026 Uiso 1 1 calc R . . C20 C 0.32530(14) 0.28018(10) 0.05289(9) 0.0314(4) Uani 1 1 d . . . H20A H 0.2527 0.3042 0.0425 0.047 Uiso 1 1 calc R . . H20B H 0.3185 0.2281 0.0265 0.047 Uiso 1 1 calc R . . H20C H 0.3719 0.3142 0.0304 0.047 Uiso 1 1 calc R . . C21 C 0.48976(13) 0.23310(9) 0.16342(10) 0.0302(4) Uani 1 1 d . . . H21A H 0.5377 0.2673 0.1424 0.045 Uiso 1 1 calc R . . H21B H 0.4837 0.1813 0.1366 0.045 Uiso 1 1 calc R . . H21C H 0.5206 0.2266 0.2228 0.045 Uiso 1 1 calc R . . C22 C 0.52959(12) 0.54900(9) 0.19864(9) 0.0240(3) Uani 1 1 d . . . H22 H 0.4899 0.6001 0.1981 0.029 Uiso 1 1 calc R . . C23 C 0.55648(14) 0.54231(10) 0.11684(10) 0.0317(4) Uani 1 1 d . . . H23A H 0.5945 0.5903 0.1076 0.048 Uiso 1 1 calc R . . H23B H 0.4886 0.5361 0.0723 0.048 Uiso 1 1 calc R . . H23C H 0.6036 0.4962 0.1181 0.048 Uiso 1 1 calc R . . C24 C 0.63502(12) 0.55290(9) 0.26961(10) 0.0288(3) Uani 1 1 d . . . H24A H 0.6767 0.5039 0.2712 0.043 Uiso 1 1 calc R . . H24B H 0.6167 0.5593 0.3215 0.043 Uiso 1 1 calc R . . H24C H 0.6791 0.5980 0.2615 0.043 Uiso 1 1 calc R . . C25 C 0.26175(12) 0.45439(9) 0.34577(9) 0.0259(3) Uani 1 1 d . . . H25 H 0.2108 0.4089 0.3436 0.031 Uiso 1 1 calc R . . C26 C 0.19251(17) 0.52906(11) 0.32436(13) 0.0452(5) Uani 1 1 d . . . H26A H 0.1495 0.5359 0.3634 0.068 Uiso 1 1 calc R . . H26B H 0.1431 0.5243 0.2687 0.068 Uiso 1 1 calc R . . H26C H 0.2404 0.5750 0.3272 0.068 Uiso 1 1 calc R . . C27 C 0.33846(16) 0.45854(13) 0.43301(10) 0.0436(5) Uani 1 1 d . . . H27A H 0.3802 0.4092 0.4458 0.065 Uiso 1 1 calc R . . H27B H 0.2954 0.4661 0.4719 0.065 Uiso 1 1 calc R . . H27C H 0.3890 0.5031 0.4373 0.065 Uiso 1 1 calc R . . C28A C -0.12891(17) 0.29118(10) 0.23811(11) 0.0219(4) Uiso 0.861(3) 1 d PD A 1 H28A H -0.0504 0.2990 0.2693 0.026 Uiso 0.861(3) 1 calc PR A 1 C29A C -0.18341(17) 0.37270(12) 0.22457(13) 0.0369(5) Uiso 0.861(3) 1 d PD A 1 H29A H -0.1728 0.3991 0.2776 0.055 Uiso 0.861(3) 1 calc PR A 1 H29B H -0.2618 0.3665 0.1977 0.055 Uiso 0.861(3) 1 calc PR A 1 H29C H -0.1505 0.4047 0.1897 0.055 Uiso 0.861(3) 1 calc PR A 1 C30A C -0.18063(16) 0.23881(12) 0.28965(12) 0.0313(5) Uiso 0.861(3) 1 d PD A 1 H30A H -0.1462 0.1865 0.2959 0.047 Uiso 0.861(3) 1 calc PR A 1 H30B H -0.2591 0.2334 0.2624 0.047 Uiso 0.861(3) 1 calc PR A 1 H30C H -0.1700 0.2628 0.3438 0.047 Uiso 0.861(3) 1 calc PR A 1 C28B C -0.1252(10) 0.3094(5) 0.2287(6) 0.0219(4) Uiso 0.139(3) 1 d PD A 2 H28B H -0.0534 0.2966 0.2692 0.026 Uiso 0.139(3) 1 calc PR A 2 C29B C -0.1181(11) 0.3965(6) 0.2141(8) 0.0369(5) Uiso 0.139(3) 1 d PD A 2 H29D H -0.1045 0.4249 0.2663 0.055 Uiso 0.139(3) 1 calc PR A 2 H29E H -0.1870 0.4149 0.1763 0.055 Uiso 0.139(3) 1 calc PR A 2 H29F H -0.0580 0.4067 0.1901 0.055 Uiso 0.139(3) 1 calc PR A 2 C30B C -0.2093(9) 0.2837(7) 0.2719(7) 0.0313(5) Uiso 0.139(3) 1 d PD A 2 H30D H -0.1813 0.2952 0.3307 0.047 Uiso 0.139(3) 1 calc PR A 2 H30E H -0.2228 0.2268 0.2639 0.047 Uiso 0.139(3) 1 calc PR A 2 H30F H -0.2777 0.3127 0.2489 0.047 Uiso 0.139(3) 1 calc PR A 2 C31 C -0.35468(12) 0.18944(9) -0.03500(9) 0.0269(3) Uani 1 1 d . A . H31 H -0.4052 0.1730 -0.0025 0.032 Uiso 1 1 calc R . . C32 C -0.36250(13) 0.12680(10) -0.10008(10) 0.0331(4) Uani 1 1 d . . . H32A H -0.4392 0.1198 -0.1317 0.050 Uiso 1 1 calc R A . H32B H -0.3336 0.0766 -0.0738 0.050 Uiso 1 1 calc R . . H32C H -0.3198 0.1434 -0.1369 0.050 Uiso 1 1 calc R . . C33 C -0.39591(13) 0.26913(10) -0.07443(11) 0.0341(4) Uani 1 1 d . . . H33A H -0.3453 0.2892 -0.1036 0.051 Uiso 1 1 calc R A . H33B H -0.4002 0.3069 -0.0317 0.051 Uiso 1 1 calc R . . H33C H -0.4686 0.2623 -0.1132 0.051 Uiso 1 1 calc R . . C34 C 0.06000(11) 0.14943(9) 0.05206(9) 0.0226(3) Uani 1 1 d . A . H34 H 0.1219 0.1839 0.0826 0.027 Uiso 1 1 calc R . . C35 C 0.08386(13) 0.06572(9) 0.08709(10) 0.0305(4) Uani 1 1 d . . . H35A H 0.0215 0.0313 0.0621 0.046 Uiso 1 1 calc R A . H35B H 0.0960 0.0672 0.1466 0.046 Uiso 1 1 calc R . . H35C H 0.1494 0.0451 0.0749 0.046 Uiso 1 1 calc R . . C36 C 0.05728(13) 0.15195(10) -0.03864(9) 0.0278(3) Uani 1 1 d . . . H36A H 0.1289 0.1364 -0.0442 0.042 Uiso 1 1 calc R A . H36B H 0.0399 0.2058 -0.0598 0.042 Uiso 1 1 calc R . . H36C H 0.0013 0.1153 -0.0699 0.042 Uiso 1 1 calc R . . O1 O 0.10971(8) 0.33642(6) 0.13104(6) 0.0249(2) Uani 1 1 d . . . H1A H 0.1371 0.3811 0.1382 0.037 Uiso 0.91 1 d P B 1 H1B H 0.0552 0.3667 0.1115 0.037 Uiso 0.09 1 d P B 2 S1A S 0.18475(4) 0.55428(2) 0.08248(3) 0.03027(14) Uani 0.9148(10) 1 d PD B 1 O2A O 0.12353(11) 0.49140(7) 0.11349(8) 0.0364(3) Uani 0.9148(10) 1 d PD B 1 C37A C 0.08264(16) 0.61734(11) 0.01997(13) 0.0395(5) Uani 0.9148(10) 1 d PD B 1 H37A H 0.0298 0.5855 -0.0210 0.059 Uiso 0.9148(10) 1 calc PR B 1 H37B H 0.1171 0.6558 -0.0079 0.059 Uiso 0.9148(10) 1 calc PR B 1 H37C H 0.0448 0.6454 0.0544 0.059 Uiso 0.9148(10) 1 calc PR B 1 C38A C 0.2272(2) 0.50960(15) 0.00125(15) 0.0530(6) Uani 0.9148(10) 1 d PD B 1 H38A H 0.2811 0.4682 0.0238 0.079 Uiso 0.9148(10) 1 calc PR B 1 H38B H 0.2600 0.5499 -0.0259 0.079 Uiso 0.9148(10) 1 calc PR B 1 H38C H 0.1637 0.4863 -0.0387 0.079 Uiso 0.9148(10) 1 calc PR B 1 S1B S 0.1613(5) 0.5769(4) -0.0019(4) 0.045 Uiso 0.0852(10) 1 d PD B 2 O2B O 0.0587(11) 0.5700(9) -0.0705(8) 0.045 Uiso 0.0852(10) 1 d PD B 2 C37B C 0.1146(18) 0.6047(13) 0.0831(11) 0.045 Uiso 0.0852(10) 1 d PD B 2 H37D H 0.0561 0.6440 0.0654 0.068 Uiso 0.0852(10) 1 calc PR B 2 H37E H 0.1754 0.6276 0.1260 0.068 Uiso 0.0852(10) 1 calc PR B 2 H37F H 0.0867 0.5580 0.1047 0.068 Uiso 0.0852(10) 1 calc PR B 2 C38B C 0.205(2) 0.4803(10) 0.0276(15) 0.045 Uiso 0.0852(10) 1 d PD B 2 H38D H 0.2094 0.4502 -0.0206 0.068 Uiso 0.0852(10) 1 calc PR B 2 H38E H 0.1529 0.4547 0.0521 0.068 Uiso 0.0852(10) 1 calc PR B 2 H38F H 0.2773 0.4819 0.0679 0.068 Uiso 0.0852(10) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0192(7) 0.0180(6) 0.0154(6) 0.0000(5) 0.0053(5) 0.0030(5) C2 0.0166(6) 0.0187(7) 0.0172(6) -0.0032(5) 0.0065(5) 0.0011(5) C3 0.0163(6) 0.0255(7) 0.0156(6) -0.0013(5) 0.0028(5) 0.0016(5) C4 0.0215(7) 0.0250(7) 0.0169(7) 0.0035(5) 0.0058(6) 0.0032(6) C5 0.0199(7) 0.0211(7) 0.0199(7) 0.0000(5) 0.0087(6) -0.0009(5) C6 0.0172(7) 0.0197(7) 0.0169(7) -0.0029(5) 0.0065(5) 0.0012(5) C7 0.0181(7) 0.0188(7) 0.0174(7) 0.0024(5) 0.0045(5) -0.0014(5) C8 0.0198(7) 0.0244(7) 0.0198(7) 0.0006(6) 0.0059(6) -0.0014(6) C9 0.0174(7) 0.0296(8) 0.0239(7) -0.0005(6) 0.0068(6) 0.0012(6) C10 0.0203(7) 0.0252(7) 0.0199(7) 0.0012(6) 0.0036(6) -0.0024(6) C11 0.0228(7) 0.0231(7) 0.0173(7) -0.0009(5) 0.0044(6) -0.0020(6) C12 0.0200(7) 0.0190(7) 0.0189(7) 0.0021(5) 0.0057(5) -0.0006(5) C13 0.0144(6) 0.0213(7) 0.0156(6) 0.0010(5) 0.0008(5) 0.0009(5) C14 0.0178(7) 0.0227(7) 0.0185(7) -0.0008(5) 0.0033(5) 0.0008(5) C15 0.0214(7) 0.0193(7) 0.0215(7) -0.0026(5) 0.0033(6) -0.0006(5) C16 0.0172(7) 0.0223(7) 0.0196(7) 0.0028(5) 0.0018(5) -0.0005(5) C17 0.0193(7) 0.0246(7) 0.0195(7) 0.0003(6) 0.0067(5) -0.0002(6) C18 0.0169(6) 0.0215(7) 0.0169(7) 0.0003(5) 0.0027(5) 0.0010(5) C19 0.0232(7) 0.0208(7) 0.0229(7) -0.0021(6) 0.0103(6) -0.0019(6) C20 0.0388(9) 0.0311(8) 0.0243(8) -0.0077(6) 0.0087(7) -0.0027(7) C21 0.0290(8) 0.0250(8) 0.0393(9) -0.0007(7) 0.0141(7) 0.0028(6) C22 0.0246(7) 0.0209(7) 0.0272(8) 0.0006(6) 0.0083(6) -0.0026(6) C23 0.0351(9) 0.0309(8) 0.0317(9) 0.0014(7) 0.0136(7) -0.0096(7) C24 0.0256(8) 0.0270(8) 0.0333(9) -0.0008(6) 0.0076(7) -0.0067(6) C25 0.0286(8) 0.0249(8) 0.0279(8) -0.0069(6) 0.0140(7) -0.0048(6) C26 0.0514(11) 0.0397(10) 0.0557(12) -0.0020(9) 0.0334(10) 0.0114(9) C27 0.0461(10) 0.0613(12) 0.0275(9) -0.0104(8) 0.0174(8) -0.0119(9) C31 0.0203(7) 0.0351(8) 0.0235(7) 0.0000(6) 0.0034(6) -0.0036(6) C32 0.0274(8) 0.0357(9) 0.0305(8) -0.0014(7) -0.0008(7) -0.0069(7) C33 0.0238(8) 0.0364(9) 0.0350(9) 0.0018(7) -0.0028(7) 0.0009(7) C34 0.0194(7) 0.0267(7) 0.0213(7) -0.0046(6) 0.0049(6) 0.0000(6) C35 0.0321(8) 0.0308(8) 0.0263(8) -0.0023(6) 0.0045(7) 0.0086(7) C36 0.0268(8) 0.0335(8) 0.0255(8) -0.0035(6) 0.0112(6) 0.0012(6) O1 0.0251(5) 0.0240(5) 0.0219(5) 0.0065(4) 0.0007(4) -0.0016(4) S1A 0.0301(2) 0.0231(2) 0.0299(2) 0.00540(16) -0.00398(18) -0.00315(17) O2A 0.0416(7) 0.0251(6) 0.0367(7) 0.0091(5) 0.0017(6) -0.0041(5) C37A 0.0358(10) 0.0286(9) 0.0439(11) 0.0130(8) -0.0050(9) -0.0015(8) C38A 0.0531(14) 0.0562(14) 0.0514(14) 0.0029(11) 0.0177(11) 0.0032(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.3603(16) . ? C1 C6 1.3985(19) . ? C1 C2 1.4004(19) . ? C2 C3 1.3946(19) . ? C2 C13 1.4988(19) . ? C3 C4 1.388(2) . ? C3 H3 0.9500 . ? C4 C5 1.386(2) . ? C4 H4 0.9500 . ? C5 C6 1.3941(19) . ? C5 H5 0.9500 . ? C6 C7 1.4970(18) . ? C7 C8 1.404(2) . ? C7 C12 1.4045(19) . ? C8 C9 1.390(2) . ? C8 C28A 1.522(2) . ? C8 C28B 1.549(8) . ? C9 C10 1.388(2) . ? C9 H9 0.9500 . ? C10 C11 1.391(2) . ? C10 C31 1.527(2) . ? C11 C12 1.397(2) . ? C11 H11 0.9500 . ? C12 C34 1.5240(19) . ? C13 C18 1.4077(19) . ? C13 C14 1.4079(19) . ? C14 C15 1.393(2) . ? C14 C25 1.5204(19) . ? C15 C16 1.391(2) . ? C15 H15 0.9500 . ? C16 C17 1.390(2) . ? C16 C22 1.5235(19) . ? C17 C18 1.396(2) . ? C17 H17 0.9500 . ? C18 C19 1.5239(19) . ? C19 C21 1.528(2) . ? C19 C20 1.530(2) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.528(2) . ? C22 C24 1.531(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.524(2) . ? C25 C27 1.528(2) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28A C30A 1.521(2) . ? C28A C29A 1.531(3) . ? C28A H28A 1.0000 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C28B C29B 1.500(8) . ? C28B C30B 1.524(8) . ? C28B H28B 1.0000 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31 C32 1.514(2) . ? C31 C33 1.529(2) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.531(2) . ? C34 C36 1.533(2) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O1 H1A 0.8254 . ? O1 H1B 0.8505 . ? S1A O2A 1.5000(13) . ? S1A C37A 1.7814(18) . ? S1A C38A 1.787(2) . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? S1B O2B 1.490(13) . ? S1B C38B 1.752(15) . ? S1B C37B 1.773(15) . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 116.62(12) . . ? O1 C1 C2 122.10(12) . . ? C6 C1 C2 121.24(12) . . ? C3 C2 C1 118.29(12) . . ? C3 C2 C13 122.45(12) . . ? C1 C2 C13 119.26(12) . . ? C4 C3 C2 121.20(12) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.61(13) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.90(13) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 118.71(12) . . ? C5 C6 C7 121.37(12) . . ? C1 C6 C7 119.90(12) . . ? C8 C7 C12 119.93(12) . . ? C8 C7 C6 119.43(12) . . ? C12 C7 C6 120.64(12) . . ? C9 C8 C7 118.84(13) . . ? C9 C8 C28A 119.70(14) . . ? C7 C8 C28A 121.38(14) . . ? C9 C8 C28B 119.2(5) . . ? C7 C8 C28B 120.9(5) . . ? C10 C9 C8 122.48(13) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 117.76(13) . . ? C9 C10 C31 118.69(13) . . ? C11 C10 C31 123.54(13) . . ? C10 C11 C12 121.90(13) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 119.03(13) . . ? C11 C12 C34 121.13(12) . . ? C7 C12 C34 119.80(12) . . ? C18 C13 C14 119.86(13) . . ? C18 C13 C2 119.45(12) . . ? C14 C13 C2 120.63(12) . . ? C15 C14 C13 118.77(13) . . ? C15 C14 C25 119.84(12) . . ? C13 C14 C25 121.38(12) . . ? C16 C15 C14 122.49(13) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C17 C16 C15 117.73(13) . . ? C17 C16 C22 122.85(13) . . ? C15 C16 C22 119.40(13) . . ? C16 C17 C18 122.09(13) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C13 119.06(13) . . ? C17 C18 C19 118.97(12) . . ? C13 C18 C19 121.97(12) . . ? C18 C19 C21 111.25(12) . . ? C18 C19 C20 111.47(12) . . ? C21 C19 C20 110.62(12) . . ? C18 C19 H19 107.8 . . ? C21 C19 H19 107.8 . . ? C20 C19 H19 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 C23 113.73(12) . . ? C16 C22 C24 110.38(12) . . ? C23 C22 C24 110.26(13) . . ? C16 C22 H22 107.4 . . ? C23 C22 H22 107.4 . . ? C24 C22 H22 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C25 C26 112.57(13) . . ? C14 C25 C27 110.32(13) . . ? C26 C25 C27 111.19(15) . . ? C14 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30A C28A C8 110.67(14) . . ? C30A C28A C29A 110.94(16) . . ? C8 C28A C29A 111.86(15) . . ? C30A C28A H28A 107.7 . . ? C8 C28A H28A 107.7 . . ? C29A C28A H28A 107.7 . . ? C29B C28B C30B 116.3(9) . . ? C29B C28B C8 119.3(8) . . ? C30B C28B C8 107.6(7) . . ? C29B C28B H28B 103.8 . . ? C30B C28B H28B 103.8 . . ? C8 C28B H28B 103.8 . . ? C28B C29B H29D 109.5 . . ? C28B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C28B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C28B C30B H30D 109.5 . . ? C28B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C28B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C32 C31 C10 114.99(13) . . ? C32 C31 C33 110.64(13) . . ? C10 C31 C33 110.06(12) . . ? C32 C31 H31 106.9 . . ? C10 C31 H31 106.9 . . ? C33 C31 H31 106.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C12 C34 C35 110.15(12) . . ? C12 C34 C36 113.56(12) . . ? C35 C34 C36 111.22(12) . . ? C12 C34 H34 107.2 . . ? C35 C34 H34 107.2 . . ? C36 C34 H34 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 O1 H1A 112.6 . . ? C1 O1 H1B 133.8 . . ? H1A O1 H1B 76.9 . . ? O2A S1A C37A 105.55(8) . . ? O2A S1A C38A 105.92(10) . . ? C37A S1A C38A 97.02(11) . . ? O2B S1B C38B 106.8(10) . . ? O2B S1B C37B 103.6(10) . . ? C38B S1B C37B 99.6(11) . . ? S1B C37B H37D 109.5 . . ? S1B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? S1B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? S1B C38B H38D 109.5 . . ? S1B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? S1B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? 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 O1 H1A O2A 0.83 1.91 2.6471(15) 148.4 . O1 H1B O2B 0.85 1.78 2.629(14) 179.9 3_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.352 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.041 #===END