# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Miguel-Angel Munoz-Hernandez' _publ_contact_author_email MAMUND2@BUZON.UAEM.MX _publ_section_title ; Aluminum complexes incorporating tridentate thioetherbis(phenolate) ligands 2,2'-thiobis(2,6-di-tert-butylphenolate), Stdiol and 2,2'-thiobis(2,6-dimethylphenolate), Smdiol and thier activity in Diels-Alder catalysis ; loop_ _publ_author_name 'Miguel-Angel Munoz-Hernandez' 'Sara Cortes-Llamas' 'Alejandro-Jose Metta-Magana' ; V.Montiel-Palma ; 'Norma Tiempos-Flores' # Attachment 'complexes.cif' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 752747' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H53 Al O3 S' _chemical_formula_weight 556.79 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6785(12) _cell_length_b 12.1405(14) _cell_length_c 26.563(3) _cell_angle_alpha 90.00 _cell_angle_beta 81.097(2) _cell_angle_gamma 90.00 _cell_volume 3402.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9722 _exptl_absorpt_correction_T_max 0.9837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32208 _diffrn_reflns_av_R_equivalents 0.1599 _diffrn_reflns_av_sigmaI/netI 0.1680 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5993 _reflns_number_gt 2474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5993 _refine_ls_number_parameters 380 _refine_ls_number_restraints 173 _refine_ls_R_factor_all 0.2359 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3049 _refine_ls_wR_factor_gt 0.2447 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.022 _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 -0.1225(2) 0.8793(2) 0.74665(8) 0.0511(7) Uani 1 1 d . A . O1 O -0.0962(4) 0.8093(4) 0.68803(16) 0.0523(14) Uani 1 1 d . . . O2 O -0.1430(4) 0.8006(4) 0.80258(17) 0.0543(14) Uani 1 1 d . . . S1 S 0.11654(18) 0.81442(17) 0.74662(7) 0.0468(6) Uani 1 1 d . . . C1 C 0.0037(7) 0.7483(6) 0.6660(3) 0.0462(19) Uani 1 1 d . . . C2 C 0.1103(7) 0.7334(6) 0.6908(2) 0.0415(18) Uani 1 1 d . . . C3 C 0.0660(7) 0.7309(6) 0.8019(2) 0.0457(19) Uani 1 1 d . . . C4 C -0.0593(7) 0.7443(6) 0.8258(3) 0.0426(18) Uani 1 1 d . . . C5 C -0.0932(7) 0.6970(6) 0.8738(3) 0.0461(19) Uani 1 1 d . . . C6 C -0.0019(8) 0.6380(6) 0.8942(3) 0.054(2) Uani 1 1 d . . . H6A H -0.0256 0.6060 0.9269 0.065 Uiso 1 1 calc R . . C7 C 0.1223(8) 0.6222(6) 0.8701(3) 0.052(2) Uani 1 1 d . . . C8 C 0.1549(7) 0.6714(6) 0.8234(3) 0.0461(19) Uani 1 1 d . . . H8A H 0.2389 0.6646 0.8058 0.055 Uiso 1 1 calc R . . C9 C 0.2182(7) 0.5568(6) 0.8958(3) 0.071(2) Uani 1 1 d DU . . C10 C 0.2392(11) 0.6143(9) 0.9437(3) 0.134(4) Uani 1 1 d DU . . H10A H 0.3012 0.5731 0.9598 0.201 Uiso 1 1 calc R . . H10B H 0.1589 0.6186 0.9672 0.201 Uiso 1 1 calc R . . H10C H 0.2712 0.6888 0.9355 0.201 Uiso 1 1 calc R . . C11 C 0.3444(8) 0.5422(9) 0.8625(4) 0.117(3) Uani 1 1 d DU . . H11A H 0.4011 0.5001 0.8810 0.175 Uiso 1 1 calc R . . H11B H 0.3817 0.6146 0.8533 0.175 Uiso 1 1 calc R . . H11C H 0.3327 0.5024 0.8315 0.175 Uiso 1 1 calc R . . C12 C 0.1704(9) 0.4425(7) 0.9095(4) 0.119(4) Uani 1 1 d DU . . H12A H 0.2336 0.4023 0.9254 0.178 Uiso 1 1 calc R . . H12B H 0.1556 0.4038 0.8786 0.178 Uiso 1 1 calc R . . H12C H 0.0909 0.4470 0.9334 0.178 Uiso 1 1 calc R . . C13 C -0.2261(7) 0.7153(7) 0.9053(3) 0.059(2) Uani 1 1 d . . . C14 C -0.3277(8) 0.6670(8) 0.8770(4) 0.088(3) Uani 1 1 d . . . H14A H -0.3135 0.5877 0.8722 0.132 Uiso 1 1 calc R . . H14B H -0.3231 0.7029 0.8437 0.132 Uiso 1 1 calc R . . H14C H -0.4116 0.6795 0.8970 0.132 Uiso 1 1 calc R . . C15 C -0.2471(8) 0.8388(7) 0.9141(3) 0.074(3) Uani 1 1 d . . . H15A H -0.1818 0.8681 0.9326 0.111 Uiso 1 1 calc R . . H15B H -0.3310 0.8512 0.9341 0.111 Uiso 1 1 calc R . . H15C H -0.2419 0.8764 0.8812 0.111 Uiso 1 1 calc R . . C16 C -0.2396(9) 0.6589(8) 0.9579(3) 0.097(4) Uani 1 1 d . . . H16A H -0.1761 0.6887 0.9771 0.145 Uiso 1 1 calc R . . H16B H -0.2268 0.5794 0.9533 0.145 Uiso 1 1 calc R . . H16C H -0.3246 0.6728 0.9766 0.145 Uiso 1 1 calc R . . C17 C 0.0082(7) 0.7003(6) 0.6174(3) 0.0451(19) Uani 1 1 d . . . C18 C 0.1144(7) 0.6383(6) 0.5984(3) 0.047(2) Uani 1 1 d . . . H18A H 0.1175 0.6058 0.5657 0.057 Uiso 1 1 calc R . . C19 C 0.2157(7) 0.6207(6) 0.6240(3) 0.0438(18) Uani 1 1 d . . . C20 C 0.2133(6) 0.6713(6) 0.6704(3) 0.0439(19) Uani 1 1 d . . . H20A H 0.2830 0.6633 0.6885 0.053 Uiso 1 1 calc R . . C21 C 0.3299(8) 0.5500(7) 0.5999(3) 0.072(3) Uani 1 1 d DU . . C22 C 0.4060(11) 0.5087(10) 0.6375(4) 0.164(5) Uani 1 1 d DU . . H22A H 0.4770 0.4651 0.6201 0.247 Uiso 1 1 calc R . . H22B H 0.3530 0.4624 0.6624 0.247 Uiso 1 1 calc R . . H22C H 0.4387 0.5710 0.6549 0.247 Uiso 1 1 calc R . . C23 C 0.4170(10) 0.6173(9) 0.5641(4) 0.149(5) Uani 1 1 d DU . . H23A H 0.4897 0.5724 0.5493 0.223 Uiso 1 1 calc R . . H23B H 0.4466 0.6800 0.5823 0.223 Uiso 1 1 calc R . . H23C H 0.3725 0.6443 0.5369 0.223 Uiso 1 1 calc R . . C24 C 0.2943(10) 0.4548(9) 0.5715(5) 0.171(5) Uani 1 1 d DU . . H24A H 0.3706 0.4136 0.5573 0.256 Uiso 1 1 calc R . . H24B H 0.2508 0.4801 0.5437 0.256 Uiso 1 1 calc R . . H24C H 0.2375 0.4070 0.5944 0.256 Uiso 1 1 calc R . . C25 C -0.1008(7) 0.7173(7) 0.5864(3) 0.054(2) Uani 1 1 d . . . C26 C -0.2246(8) 0.6683(7) 0.6154(3) 0.079(3) Uani 1 1 d . . . H26A H -0.2449 0.7039 0.6487 0.119 Uiso 1 1 calc R . . H26B H -0.2137 0.5890 0.6200 0.119 Uiso 1 1 calc R . . H26C H -0.2938 0.6807 0.5957 0.119 Uiso 1 1 calc R . . C27 C -0.1165(8) 0.8396(7) 0.5764(3) 0.070(3) Uani 1 1 d . . . H27A H -0.0371 0.8690 0.5578 0.105 Uiso 1 1 calc R . . H27B H -0.1379 0.8785 0.6089 0.105 Uiso 1 1 calc R . . H27C H -0.1846 0.8500 0.5560 0.105 Uiso 1 1 calc R . . C28 C -0.0767(8) 0.6586(8) 0.5341(3) 0.083(3) Uani 1 1 d . . . H28A H 0.0009 0.6876 0.5140 0.124 Uiso 1 1 calc R . . H28B H -0.1485 0.6716 0.5159 0.124 Uiso 1 1 calc R . . H28C H -0.0672 0.5793 0.5393 0.124 Uiso 1 1 calc R . . C33 C -0.0875(8) 1.0369(7) 0.7509(3) 0.077(3) Uani 1 1 d . . . H33A H -0.1663 1.0785 0.7514 0.115 Uiso 1 1 calc R . . H33B H -0.0264 1.0592 0.7213 0.115 Uiso 1 1 calc R . . H33C H -0.0523 1.0519 0.7821 0.115 Uiso 1 1 calc R . . O3 O -0.3069(5) 0.8908(5) 0.7463(2) 0.0811(18) Uani 1 1 d DU . . C29A C -0.3535(11) 0.9282(12) 0.7006(4) 0.096(3) Uani 0.730(8) 1 d PDU A 1 H29A H -0.2798 0.9360 0.6732 0.115 Uiso 0.730(8) 1 calc PR A 1 H29B H -0.3902 1.0026 0.7075 0.115 Uiso 0.730(8) 1 calc PR A 1 C30A C -0.4483(14) 0.8601(14) 0.6808(6) 0.120(5) Uani 0.730(8) 1 d PDU A 1 H30A H -0.4731 0.8955 0.6507 0.180 Uiso 0.730(8) 1 calc PR A 1 H30B H -0.5229 0.8519 0.7071 0.180 Uiso 0.730(8) 1 calc PR A 1 H30C H -0.4122 0.7874 0.6715 0.180 Uiso 0.730(8) 1 calc PR A 1 C31A C -0.3829(10) 0.9358(13) 0.7923(4) 0.102(3) Uani 0.730(8) 1 d PDU A 1 H31A H -0.3288 0.9362 0.8194 0.123 Uiso 0.730(8) 1 calc PR A 1 H31B H -0.4012 1.0137 0.7851 0.123 Uiso 0.730(8) 1 calc PR A 1 C32A C -0.5018(13) 0.8844(16) 0.8133(6) 0.140(6) Uani 0.730(8) 1 d PDU A 1 H32A H -0.5395 0.9240 0.8441 0.210 Uiso 0.730(8) 1 calc PR A 1 H32B H -0.4866 0.8076 0.8219 0.210 Uiso 0.730(8) 1 calc PR A 1 H32C H -0.5598 0.8869 0.7881 0.210 Uiso 0.730(8) 1 calc PR A 1 C29B C -0.391(2) 0.815(2) 0.7255(13) 0.096(4) Uani 0.270(8) 1 d PDU A 2 H29C H -0.4404 0.7688 0.7524 0.115 Uiso 0.270(8) 1 calc PR A 2 H29D H -0.3445 0.7666 0.6988 0.115 Uiso 0.270(8) 1 calc PR A 2 C30B C -0.471(4) 0.895(3) 0.7042(16) 0.111(6) Uani 0.270(8) 1 d PDU A 2 H30D H -0.5312 0.8558 0.6860 0.166 Uiso 0.270(8) 1 calc PR A 2 H30E H -0.4182 0.9436 0.6804 0.166 Uiso 0.270(8) 1 calc PR A 2 H30F H -0.5185 0.9386 0.7318 0.166 Uiso 0.270(8) 1 calc PR A 2 C31B C -0.367(3) 0.9984(16) 0.7574(14) 0.098(4) Uani 0.270(8) 1 d PDU A 2 H31C H -0.3098 1.0490 0.7724 0.117 Uiso 0.270(8) 1 calc PR A 2 H31D H -0.3895 1.0323 0.7261 0.117 Uiso 0.270(8) 1 calc PR A 2 C32B C -0.480(3) 0.974(4) 0.7939(15) 0.117(7) Uani 0.270(8) 1 d PDU A 2 H32D H -0.5238 1.0424 0.8052 0.175 Uiso 0.270(8) 1 calc PR A 2 H32E H -0.4558 0.9353 0.8234 0.175 Uiso 0.270(8) 1 calc PR A 2 H32F H -0.5370 0.9267 0.7777 0.175 Uiso 0.270(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0452(14) 0.0655(17) 0.0430(14) -0.0054(13) -0.0079(11) 0.0164(13) O1 0.038(3) 0.077(4) 0.043(3) -0.011(3) -0.011(2) 0.016(3) O2 0.036(3) 0.075(4) 0.051(3) 0.005(3) -0.004(2) 0.012(3) S1 0.0452(11) 0.0627(13) 0.0334(10) -0.0028(10) -0.0093(8) -0.0013(10) C1 0.041(4) 0.056(5) 0.040(4) 0.003(4) -0.003(4) 0.002(4) C2 0.042(4) 0.054(5) 0.029(4) 0.002(3) -0.010(3) -0.003(4) C3 0.048(5) 0.055(5) 0.035(4) -0.007(4) -0.011(4) -0.001(4) C4 0.033(4) 0.058(5) 0.037(4) 0.001(4) -0.007(3) 0.000(4) C5 0.042(4) 0.044(5) 0.050(5) -0.001(4) -0.002(4) 0.008(4) C6 0.071(6) 0.039(5) 0.049(5) 0.007(4) 0.001(4) -0.007(4) C7 0.059(6) 0.059(5) 0.039(5) -0.002(4) -0.013(4) -0.002(4) C8 0.035(4) 0.057(5) 0.049(5) -0.006(4) -0.013(3) 0.007(4) C9 0.067(5) 0.076(5) 0.077(5) 0.012(4) -0.035(4) 0.015(5) C10 0.175(10) 0.133(8) 0.117(7) -0.028(6) -0.097(7) 0.061(8) C11 0.068(6) 0.155(9) 0.129(7) 0.035(7) -0.023(5) 0.042(6) C12 0.114(8) 0.091(6) 0.164(10) 0.050(6) -0.063(7) 0.002(6) C13 0.054(5) 0.064(6) 0.056(5) 0.000(4) 0.003(4) -0.004(5) C14 0.051(6) 0.086(7) 0.122(8) -0.004(6) 0.004(6) -0.008(5) C15 0.074(6) 0.064(7) 0.078(6) -0.005(5) 0.011(5) 0.009(5) C16 0.079(7) 0.105(8) 0.092(7) 0.032(6) 0.031(6) 0.019(6) C17 0.047(5) 0.049(5) 0.040(4) 0.003(4) -0.010(4) -0.001(4) C18 0.049(5) 0.056(5) 0.037(4) -0.016(4) -0.005(4) -0.001(4) C19 0.041(5) 0.053(5) 0.035(4) -0.002(4) 0.002(3) 0.002(4) C20 0.024(4) 0.056(5) 0.052(5) 0.001(4) -0.005(3) 0.006(4) C21 0.062(5) 0.081(6) 0.074(6) -0.019(5) -0.011(4) 0.032(5) C22 0.185(11) 0.210(12) 0.094(8) -0.001(8) -0.010(8) 0.146(10) C23 0.098(9) 0.130(10) 0.190(12) 0.013(9) 0.064(8) 0.027(8) C24 0.100(9) 0.153(11) 0.253(13) -0.132(10) -0.006(9) 0.032(8) C25 0.051(5) 0.061(6) 0.052(5) -0.005(4) -0.019(4) 0.002(4) C26 0.058(6) 0.089(7) 0.095(7) 0.001(6) -0.029(5) -0.001(5) C27 0.078(6) 0.077(7) 0.062(6) 0.002(5) -0.032(5) 0.004(5) C28 0.077(7) 0.112(8) 0.066(6) -0.023(6) -0.032(5) 0.008(6) C33 0.088(7) 0.071(6) 0.071(6) -0.002(5) -0.010(5) 0.017(5) O3 0.045(3) 0.126(5) 0.074(4) -0.010(3) -0.015(3) 0.043(3) C29A 0.056(6) 0.150(8) 0.083(5) 0.001(6) -0.016(5) 0.033(6) C30A 0.079(8) 0.192(11) 0.094(9) -0.043(9) -0.032(7) 0.039(8) C31A 0.067(6) 0.155(8) 0.084(5) -0.011(6) -0.005(5) 0.043(6) C32A 0.097(9) 0.192(14) 0.117(10) 0.010(11) 0.030(7) 0.030(9) C29B 0.057(7) 0.145(8) 0.087(8) -0.014(7) -0.017(6) 0.033(6) C30B 0.069(11) 0.179(13) 0.093(13) -0.017(11) -0.037(9) 0.043(10) C31B 0.064(7) 0.136(7) 0.092(8) -0.012(7) -0.006(7) 0.047(6) C32B 0.082(11) 0.154(14) 0.103(12) -0.025(12) 0.017(9) 0.046(10) _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 O2 1.752(5) . ? Al1 O1 1.759(5) . ? Al1 C33 1.955(9) . ? Al1 O3 1.975(6) . ? Al1 S1 2.671(3) . ? O1 C1 1.354(8) . ? O2 C4 1.349(8) . ? S1 C2 1.789(7) . ? S1 C3 1.797(7) . ? C1 C2 1.412(9) . ? C1 C17 1.412(9) . ? C2 C20 1.374(9) . ? C3 C8 1.385(9) . ? C3 C4 1.399(9) . ? C4 C5 1.394(9) . ? C5 C6 1.387(10) . ? C5 C13 1.547(10) . ? C6 C7 1.393(10) . ? C6 H6A 0.9500 . ? C7 C8 1.373(9) . ? C7 C9 1.537(10) . ? C8 H8A 0.9500 . ? C9 C10 1.498(8) . ? C9 C12 1.503(8) . ? C9 C11 1.504(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.529(10) . ? C13 C14 1.530(11) . ? C13 C16 1.540(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.389(9) . ? C17 C25 1.540(9) . ? C18 C19 1.380(9) . ? C18 H18A 0.9500 . ? C19 C20 1.374(9) . ? C19 C21 1.547(10) . ? C20 H20A 0.9500 . ? C21 C24 1.463(8) . ? C21 C22 1.468(8) . ? C21 C23 1.471(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C27 1.522(10) . ? C25 C26 1.542(11) . ? C25 C28 1.547(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O3 C29A 1.455(8) . ? O3 C29B 1.457(14) . ? O3 C31A 1.464(8) . ? O3 C31B 1.465(13) . ? C29A C30A 1.465(9) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C31A C32A 1.447(9) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C29B C30B 1.468(13) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31B C32B 1.462(13) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 O2 Al1 O1 118.0(3) . . ? O2 Al1 C33 119.0(3) . . ? O1 Al1 C33 121.2(3) . . ? O2 Al1 O3 92.8(3) . . ? O1 Al1 O3 93.0(2) . . ? C33 Al1 O3 97.5(3) . . ? O2 Al1 S1 80.41(17) . . ? O1 Al1 S1 80.53(17) . . ? C33 Al1 S1 95.6(3) . . ? O3 Al1 S1 166.9(2) . . ? C1 O1 Al1 130.8(4) . . ? C4 O2 Al1 131.3(4) . . ? C2 S1 C3 108.8(3) . . ? C2 S1 Al1 90.3(2) . . ? C3 S1 Al1 90.0(2) . . ? O1 C1 C2 120.5(6) . . ? O1 C1 C17 122.2(6) . . ? C2 C1 C17 117.3(7) . . ? C20 C2 C1 122.8(6) . . ? C20 C2 S1 119.9(5) . . ? C1 C2 S1 116.9(5) . . ? C8 C3 C4 122.7(7) . . ? C8 C3 S1 119.6(6) . . ? C4 C3 S1 116.8(5) . . ? O2 C4 C5 122.1(6) . . ? O2 C4 C3 120.4(6) . . ? C5 C4 C3 117.6(6) . . ? C6 C5 C4 118.1(7) . . ? C6 C5 C13 120.3(7) . . ? C4 C5 C13 121.5(6) . . ? C5 C6 C7 124.7(7) . . ? C5 C6 H6A 117.7 . . ? C7 C6 H6A 117.7 . . ? C8 C7 C6 116.4(7) . . ? C8 C7 C9 122.2(7) . . ? C6 C7 C9 121.3(7) . . ? C7 C8 C3 120.5(7) . . ? C7 C8 H8A 119.8 . . ? C3 C8 H8A 119.8 . . ? C10 C9 C12 108.3(7) . . ? C10 C9 C11 108.5(7) . . ? C12 C9 C11 105.9(7) . . ? C10 C9 C7 109.5(7) . . ? C12 C9 C7 111.0(7) . . ? C11 C9 C7 113.5(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 110.6(7) . . ? C15 C13 C16 107.9(7) . . ? C14 C13 C16 107.5(7) . . ? C15 C13 C5 108.9(6) . . ? C14 C13 C5 109.9(6) . . ? C16 C13 C5 112.1(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C1 117.8(6) . . ? C18 C17 C25 121.4(6) . . ? C1 C17 C25 120.8(7) . . ? C19 C18 C17 124.2(6) . . ? C19 C18 H18A 117.9 . . ? C17 C18 H18A 117.9 . . ? C20 C19 C18 117.8(7) . . ? C20 C19 C21 121.5(6) . . ? C18 C19 C21 120.6(6) . . ? C2 C20 C19 120.1(6) . . ? C2 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C24 C21 C22 107.2(7) . . ? C24 C21 C23 107.1(8) . . ? C22 C21 C23 105.6(8) . . ? C24 C21 C19 113.6(7) . . ? C22 C21 C19 113.1(7) . . ? C23 C21 C19 109.8(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C17 109.7(6) . . ? C27 C25 C26 110.8(7) . . ? C17 C25 C26 110.0(6) . . ? C27 C25 C28 107.5(7) . . ? C17 C25 C28 112.5(6) . . ? C26 C25 C28 106.3(7) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Al1 C33 H33A 109.5 . . ? Al1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Al1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29A O3 C29B 64.5(13) . . ? C29A O3 C31A 111.2(8) . . ? C29B O3 C31A 105.0(15) . . ? C29A O3 C31B 72.1(16) . . ? C29B O3 C31B 111.5(16) . . ? C31A O3 C31B 48.0(14) . . ? C29A O3 Al1 119.7(6) . . ? C29B O3 Al1 129.2(12) . . ? C31A O3 Al1 116.5(6) . . ? C31B O3 Al1 117.8(13) . . ? O3 C29A C30A 117.9(12) . . ? O3 C29A H29A 107.8 . . ? C30A C29A H29A 107.8 . . ? O3 C29A H29B 107.8 . . ? C30A C29A H29B 107.8 . . ? H29A C29A H29B 107.2 . . ? C29A C30A H30A 109.5 . . ? C29A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C29A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C32A C31A O3 120.0(12) . . ? C32A C31A H31A 107.3 . . ? O3 C31A H31A 107.3 . . ? C32A C31A H31B 107.3 . . ? O3 C31A H31B 107.3 . . ? H31A C31A H31B 106.9 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? O3 C29B C30B 99(2) . . ? O3 C29B H29C 112.0 . . ? C30B C29B H29C 112.0 . . ? O3 C29B H29D 112.0 . . ? C30B C29B H29D 112.0 . . ? H29C C29B H29D 109.6 . . ? C29B C30B H30D 109.5 . . ? C29B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C32B C31B O3 104(2) . . ? C32B C31B H31C 111.0 . . ? O3 C31B H31C 111.0 . . ? C32B C31B H31D 111.0 . . ? O3 C31B H31D 111.0 . . ? H31C C31B H31D 109.0 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 O1 C1 -67.9(7) . . . . ? C33 Al1 O1 C1 96.7(7) . . . . ? O3 Al1 O1 C1 -162.6(6) . . . . ? S1 Al1 O1 C1 5.9(6) . . . . ? O1 Al1 O2 C4 74.6(7) . . . . ? C33 Al1 O2 C4 -90.3(7) . . . . ? O3 Al1 O2 C4 169.5(6) . . . . ? S1 Al1 O2 C4 0.8(6) . . . . ? O2 Al1 S1 C2 113.1(3) . . . . ? O1 Al1 S1 C2 -7.5(3) . . . . ? C33 Al1 S1 C2 -128.3(3) . . . . ? O3 Al1 S1 C2 53.7(9) . . . . ? O2 Al1 S1 C3 4.4(3) . . . . ? O1 Al1 S1 C3 -116.3(3) . . . . ? C33 Al1 S1 C3 122.9(3) . . . . ? O3 Al1 S1 C3 -55.0(9) . . . . ? Al1 O1 C1 C2 -0.4(10) . . . . ? Al1 O1 C1 C17 -178.3(5) . . . . ? O1 C1 C2 C20 179.2(7) . . . . ? C17 C1 C2 C20 -2.8(11) . . . . ? O1 C1 C2 S1 -9.1(9) . . . . ? C17 C1 C2 S1 168.9(5) . . . . ? C3 S1 C2 C20 -88.1(6) . . . . ? Al1 S1 C2 C20 -178.2(6) . . . . ? C3 S1 C2 C1 100.0(6) . . . . ? Al1 S1 C2 C1 9.9(5) . . . . ? C2 S1 C3 C8 90.9(6) . . . . ? Al1 S1 C3 C8 -178.9(6) . . . . ? C2 S1 C3 C4 -99.5(6) . . . . ? Al1 S1 C3 C4 -9.2(5) . . . . ? Al1 O2 C4 C5 172.2(5) . . . . ? Al1 O2 C4 C3 -8.1(10) . . . . ? C8 C3 C4 O2 -178.2(7) . . . . ? S1 C3 C4 O2 12.5(9) . . . . ? C8 C3 C4 C5 1.4(11) . . . . ? S1 C3 C4 C5 -167.8(5) . . . . ? O2 C4 C5 C6 178.3(7) . . . . ? C3 C4 C5 C6 -1.4(10) . . . . ? O2 C4 C5 C13 -5.5(11) . . . . ? C3 C4 C5 C13 174.8(7) . . . . ? C4 C5 C6 C7 0.0(12) . . . . ? C13 C5 C6 C7 -176.3(7) . . . . ? C5 C6 C7 C8 1.5(12) . . . . ? C5 C6 C7 C9 179.2(7) . . . . ? C6 C7 C8 C3 -1.4(11) . . . . ? C9 C7 C8 C3 -179.1(7) . . . . ? C4 C3 C8 C7 0.0(11) . . . . ? S1 C3 C8 C7 169.0(6) . . . . ? C8 C7 C9 C10 115.0(9) . . . . ? C6 C7 C9 C10 -62.6(10) . . . . ? C8 C7 C9 C12 -125.4(8) . . . . ? C6 C7 C9 C12 57.0(10) . . . . ? C8 C7 C9 C11 -6.3(11) . . . . ? C6 C7 C9 C11 176.1(8) . . . . ? C6 C5 C13 C15 117.7(8) . . . . ? C4 C5 C13 C15 -58.4(9) . . . . ? C6 C5 C13 C14 -121.0(8) . . . . ? C4 C5 C13 C14 62.9(9) . . . . ? C6 C5 C13 C16 -1.6(11) . . . . ? C4 C5 C13 C16 -177.7(7) . . . . ? O1 C1 C17 C18 -179.3(7) . . . . ? C2 C1 C17 C18 2.7(10) . . . . ? O1 C1 C17 C25 1.1(11) . . . . ? C2 C1 C17 C25 -176.9(7) . . . . ? C1 C17 C18 C19 -0.1(11) . . . . ? C25 C17 C18 C19 179.4(7) . . . . ? C17 C18 C19 C20 -2.5(12) . . . . ? C17 C18 C19 C21 179.8(7) . . . . ? C1 C2 C20 C19 0.2(11) . . . . ? S1 C2 C20 C19 -171.3(6) . . . . ? C18 C19 C20 C2 2.4(11) . . . . ? C21 C19 C20 C2 -179.9(7) . . . . ? C20 C19 C21 C24 144.6(8) . . . . ? C18 C19 C21 C24 -37.8(11) . . . . ? C20 C19 C21 C22 22.1(11) . . . . ? C18 C19 C21 C22 -160.3(8) . . . . ? C20 C19 C21 C23 -95.6(9) . . . . ? C18 C19 C21 C23 82.1(9) . . . . ? C18 C17 C25 C27 -119.5(8) . . . . ? C1 C17 C25 C27 60.0(9) . . . . ? C18 C17 C25 C26 118.4(8) . . . . ? C1 C17 C25 C26 -62.1(9) . . . . ? C18 C17 C25 C28 0.1(10) . . . . ? C1 C17 C25 C28 179.6(7) . . . . ? O2 Al1 O3 C29A -165.7(8) . . . . ? O1 Al1 O3 C29A -47.5(8) . . . . ? C33 Al1 O3 C29A 74.6(8) . . . . ? S1 Al1 O3 C29A -107.5(11) . . . . ? O2 Al1 O3 C29B -85.7(19) . . . . ? O1 Al1 O3 C29B 32.5(19) . . . . ? C33 Al1 O3 C29B 154.6(19) . . . . ? S1 Al1 O3 C29B -27(2) . . . . ? O2 Al1 O3 C31A 55.6(9) . . . . ? O1 Al1 O3 C31A 173.8(9) . . . . ? C33 Al1 O3 C31A -64.2(9) . . . . ? S1 Al1 O3 C31A 113.7(11) . . . . ? O2 Al1 O3 C31B 109.9(17) . . . . ? O1 Al1 O3 C31B -131.9(17) . . . . ? C33 Al1 O3 C31B -9.8(17) . . . . ? S1 Al1 O3 C31B 168.1(18) . . . . ? C29B O3 C29A C30A 5.9(17) . . . . ? C31A O3 C29A C30A -91.1(14) . . . . ? C31B O3 C29A C30A -119.5(17) . . . . ? Al1 O3 C29A C30A 128.2(11) . . . . ? C29A O3 C31A C32A 81.6(16) . . . . ? C29B O3 C31A C32A 13.5(19) . . . . ? C31B O3 C31A C32A 119(2) . . . . ? Al1 O3 C31A C32A -136.3(12) . . . . ? C29A O3 C29B C30B -32(2) . . . . ? C31A O3 C29B C30B 75(3) . . . . ? C31B O3 C29B C30B 25(3) . . . . ? Al1 O3 C29B C30B -141(2) . . . . ? C29A O3 C31B C32B 111(3) . . . . ? C29B O3 C31B C32B 59(3) . . . . ? C31A O3 C31B C32B -32(2) . . . . ? Al1 O3 C31B C32B -134(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.576 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.072 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 752748' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H57 Al O3 S' _chemical_formula_weight 596.86 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 12.3409(9) _cell_length_b 14.9874(11) _cell_length_c 20.6407(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3817.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9575 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37254 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6737 _reflns_number_gt 4854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(12) _refine_ls_number_reflns 6737 _refine_ls_number_parameters 371 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 1.074 _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 0.79972(10) 0.66786(8) 0.91683(5) 0.0598(3) Uani 1 1 d . . . O1 O 0.8733(2) 0.76491(17) 0.89502(12) 0.0654(7) Uani 1 1 d . . . O2 O 0.8755(2) 0.58813(17) 0.96003(12) 0.0652(7) Uani 1 1 d . . . S1 S 0.90869(8) 0.60263(6) 0.81947(4) 0.0574(3) Uani 1 1 d . . . C1 C 0.9521(3) 0.7755(3) 0.85165(18) 0.0572(9) Uani 1 1 d . . . C2 C 0.9844(3) 0.7027(2) 0.81284(18) 0.0559(9) Uani 1 1 d . . . C3 C 1.0664(3) 0.7094(3) 0.76812(19) 0.0604(10) Uani 1 1 d . . . H3A H 1.0856 0.6587 0.7430 0.073 Uiso 1 1 calc R . . C4 C 1.1212(3) 0.7881(3) 0.75903(19) 0.0641(10) Uani 1 1 d . . . C5 C 1.0882(4) 0.8598(3) 0.7972(2) 0.0663(10) Uani 1 1 d . . . H5A H 1.1246 0.9151 0.7915 0.080 Uiso 1 1 calc R . . C6 C 1.0060(3) 0.8562(2) 0.84300(17) 0.0581(9) Uani 1 1 d . . . C7 C 1.2128(4) 0.7944(3) 0.7086(2) 0.0914(14) Uani 1 1 d DU . . C8 C 1.2757(7) 0.8750(5) 0.7155(6) 0.260(5) Uani 1 1 d DU . . H8A H 1.3326 0.8763 0.6824 0.391 Uiso 1 1 calc R . . H8B H 1.3089 0.8764 0.7586 0.391 Uiso 1 1 calc R . . H8C H 1.2284 0.9269 0.7102 0.391 Uiso 1 1 calc R . . C9 C 1.1695(6) 0.7995(7) 0.6437(3) 0.226(4) Uani 1 1 d DU . . H9A H 1.2292 0.8033 0.6126 0.339 Uiso 1 1 calc R . . H9B H 1.1236 0.8526 0.6399 0.339 Uiso 1 1 calc R . . H9C H 1.1262 0.7461 0.6348 0.339 Uiso 1 1 calc R . . C10 C 1.2854(5) 0.7189(4) 0.7108(4) 0.170(3) Uani 1 1 d DU . . H10A H 1.3416 0.7259 0.6777 0.255 Uiso 1 1 calc R . . H10B H 1.2446 0.6640 0.7027 0.255 Uiso 1 1 calc R . . H10C H 1.3194 0.7157 0.7537 0.255 Uiso 1 1 calc R . . C11 C 0.9758(4) 0.9396(3) 0.8835(2) 0.0699(11) Uani 1 1 d . . . C12 C 0.9961(5) 0.9211(3) 0.9549(2) 0.0919(15) Uani 1 1 d . . . H12A H 0.9769 0.9739 0.9804 0.138 Uiso 1 1 calc R . . H12B H 1.0729 0.9070 0.9615 0.138 Uiso 1 1 calc R . . H12C H 0.9517 0.8704 0.9688 0.138 Uiso 1 1 calc R . . C13 C 0.8580(4) 0.9636(3) 0.8728(3) 0.0897(15) Uani 1 1 d . . . H13A H 0.8396 1.0161 0.8989 0.135 Uiso 1 1 calc R . . H13B H 0.8121 0.9133 0.8856 0.135 Uiso 1 1 calc R . . H13C H 0.8462 0.9770 0.8268 0.135 Uiso 1 1 calc R . . C14 C 1.0433(5) 1.0210(3) 0.8643(3) 0.0904(15) Uani 1 1 d . . . H14A H 1.0225 1.0721 0.8911 0.136 Uiso 1 1 calc R . . H14B H 1.0305 1.0350 0.8185 0.136 Uiso 1 1 calc R . . H14C H 1.1204 1.0079 0.8708 0.136 Uiso 1 1 calc R . . C15 C 0.9489(3) 0.5311(3) 0.93828(19) 0.0579(9) Uani 1 1 d . . . C16 C 0.9836(3) 0.5336(2) 0.87315(18) 0.0546(9) Uani 1 1 d . . . C17 C 1.0649(3) 0.4805(2) 0.8495(2) 0.0610(10) Uani 1 1 d . . . H17A H 1.0855 0.4852 0.8053 0.073 Uiso 1 1 calc R . . C18 C 1.1172(3) 0.4206(3) 0.8891(2) 0.0694(11) Uani 1 1 d . . . C19 C 1.0796(4) 0.4159(3) 0.9531(2) 0.0749(12) Uani 1 1 d . . . H19A H 1.1148 0.3749 0.9812 0.090 Uiso 1 1 calc R . . C20 C 0.9962(4) 0.4653(3) 0.9786(2) 0.0662(10) Uani 1 1 d . . . C21 C 1.2111(4) 0.3631(3) 0.8669(2) 0.0961(15) Uani 1 1 d DU . . C22 C 1.2564(7) 0.3928(6) 0.8031(4) 0.221(4) Uani 1 1 d DU . . H22A H 1.1986 0.3929 0.7705 0.331 Uiso 1 1 calc R . . H22B H 1.3140 0.3518 0.7896 0.331 Uiso 1 1 calc R . . H22C H 1.2861 0.4531 0.8074 0.331 Uiso 1 1 calc R . . C23 C 1.1750(6) 0.2685(4) 0.8581(5) 0.197(4) Uani 1 1 d DU . . H23A H 1.1460 0.2457 0.8991 0.296 Uiso 1 1 calc R . . H23B H 1.2368 0.2318 0.8447 0.296 Uiso 1 1 calc R . . H23C H 1.1186 0.2659 0.8247 0.296 Uiso 1 1 calc R . . C24 C 1.3039(5) 0.3641(6) 0.9137(4) 0.189(4) Uani 1 1 d DU . . H24A H 1.2788 0.3438 0.9563 0.284 Uiso 1 1 calc R . . H24B H 1.3324 0.4249 0.9173 0.284 Uiso 1 1 calc R . . H24C H 1.3612 0.3242 0.8981 0.284 Uiso 1 1 calc R . . C25 C 0.9590(5) 0.4532(3) 1.0490(3) 0.0889(15) Uani 1 1 d . . . C26 C 1.0128(6) 0.3693(5) 1.0797(3) 0.142(3) Uani 1 1 d . . . H26A H 0.9880 0.3628 1.1246 0.213 Uiso 1 1 calc R . . H26B H 1.0917 0.3761 1.0790 0.213 Uiso 1 1 calc R . . H26C H 0.9923 0.3162 1.0549 0.213 Uiso 1 1 calc R . . C27 C 0.8381(5) 0.4404(4) 1.0516(3) 0.118(2) Uani 1 1 d . . . H27A H 0.8021 0.4929 1.0333 0.177 Uiso 1 1 calc R . . H27B H 0.8154 0.4325 1.0968 0.177 Uiso 1 1 calc R . . H27C H 0.8182 0.3874 1.0265 0.177 Uiso 1 1 calc R . . C28 C 0.9963(5) 0.5324(4) 1.0879(2) 0.1089(18) Uani 1 1 d . . . H28A H 0.9638 0.5869 1.0703 0.163 Uiso 1 1 calc R . . H28B H 1.0754 0.5369 1.0857 0.163 Uiso 1 1 calc R . . H28C H 0.9739 0.5250 1.1332 0.163 Uiso 1 1 calc R . . C29 C 0.6599(4) 0.6299(5) 0.8816(2) 0.1037(17) Uani 1 1 d U . . H29A H 0.6560 0.5645 0.8879 0.124 Uiso 1 1 calc R . . H29B H 0.6037 0.6563 0.9100 0.124 Uiso 1 1 calc R . . C30 C 0.6265(5) 0.6461(4) 0.8179(3) 0.136(2) Uani 1 1 d DU . . H30A H 0.6895 0.6365 0.7882 0.163 Uiso 1 1 calc R . . C31 C 0.5283(5) 0.5901(6) 0.7924(4) 0.161(3) Uani 1 1 d DU . . H31A H 0.5478 0.5267 0.7920 0.241 Uiso 1 1 calc R . . H31B H 0.5098 0.6093 0.7484 0.241 Uiso 1 1 calc R . . H31C H 0.4659 0.5991 0.8210 0.241 Uiso 1 1 calc R . . C32 C 0.5927(8) 0.7466(5) 0.8148(4) 0.181(3) Uani 1 1 d DU . . H32A H 0.6529 0.7838 0.8300 0.271 Uiso 1 1 calc R . . H32B H 0.5294 0.7564 0.8426 0.271 Uiso 1 1 calc R . . H32C H 0.5747 0.7626 0.7701 0.271 Uiso 1 1 calc R . . O3 O 0.7502(2) 0.72266(19) 0.99697(13) 0.0728(8) Uani 1 1 d DU . . C33 C 0.8113(4) 0.7300(3) 1.0556(2) 0.0876(13) Uani 1 1 d DU . . H33A H 0.8896 0.7359 1.0459 0.105 Uiso 1 1 calc R . . H33B H 0.8004 0.6766 1.0831 0.105 Uiso 1 1 calc R . . C34 C 0.7708(5) 0.8107(4) 1.0888(3) 0.1113(17) Uani 1 1 d DU . . H34A H 0.7241 0.7941 1.1258 0.134 Uiso 1 1 calc R . . H34B H 0.8320 0.8470 1.1051 0.134 Uiso 1 1 calc R . . C35 C 0.7097(6) 0.8601(4) 1.0413(3) 0.1165(17) Uani 1 1 d DU . . H35A H 0.7563 0.9049 1.0197 0.140 Uiso 1 1 calc R . . H35B H 0.6481 0.8912 1.0620 0.140 Uiso 1 1 calc R . . C36 C 0.6709(4) 0.7953(3) 0.9948(2) 0.0913(13) Uani 1 1 d DU . . H36A H 0.6673 0.8216 0.9508 0.110 Uiso 1 1 calc R . . H36B H 0.5979 0.7735 1.0069 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0569(7) 0.0666(7) 0.0559(6) -0.0022(6) 0.0017(5) 0.0081(6) O1 0.0759(18) 0.0590(15) 0.0612(15) -0.0030(12) 0.0118(14) 0.0142(13) O2 0.0763(18) 0.0613(16) 0.0579(15) 0.0037(13) 0.0070(13) 0.0102(14) S1 0.0610(5) 0.0565(5) 0.0548(5) -0.0040(4) -0.0044(5) 0.0063(5) C1 0.060(2) 0.056(2) 0.056(2) 0.0014(18) -0.0009(18) 0.0137(19) C2 0.061(2) 0.051(2) 0.056(2) 0.0022(17) -0.0076(19) 0.0125(17) C3 0.069(3) 0.052(2) 0.061(2) -0.0016(18) 0.005(2) 0.012(2) C4 0.062(2) 0.058(2) 0.073(3) 0.007(2) 0.008(2) 0.012(2) C5 0.072(3) 0.050(2) 0.076(2) 0.0107(18) 0.001(2) 0.004(2) C6 0.068(2) 0.051(2) 0.055(2) 0.0051(16) -0.003(2) 0.0113(19) C7 0.093(3) 0.071(3) 0.110(3) 0.013(3) 0.040(3) 0.015(2) C8 0.233(8) 0.156(5) 0.393(11) -0.102(7) 0.229(7) -0.084(6) C9 0.137(6) 0.430(12) 0.110(4) 0.107(6) 0.054(4) 0.056(7) C10 0.133(5) 0.153(5) 0.225(7) 0.062(6) 0.092(5) 0.069(5) C11 0.089(3) 0.052(2) 0.069(3) 0.0028(19) 0.001(2) 0.007(2) C12 0.130(4) 0.078(3) 0.068(3) -0.006(2) -0.001(3) 0.001(3) C13 0.110(4) 0.067(3) 0.092(3) -0.004(3) 0.004(3) 0.036(3) C14 0.124(4) 0.054(3) 0.093(3) -0.005(2) 0.014(3) 0.000(3) C15 0.057(2) 0.052(2) 0.065(2) -0.0002(18) 0.0006(18) -0.0026(19) C16 0.062(2) 0.0419(18) 0.060(2) -0.0014(16) -0.0050(18) -0.0037(18) C17 0.056(2) 0.059(2) 0.067(2) -0.0058(19) -0.0021(19) 0.0048(19) C18 0.067(3) 0.055(2) 0.086(3) -0.001(2) -0.004(2) 0.004(2) C19 0.080(3) 0.059(2) 0.087(3) 0.014(2) -0.011(3) 0.006(2) C20 0.070(3) 0.056(2) 0.072(3) 0.0081(19) 0.000(2) 0.002(2) C21 0.091(3) 0.085(3) 0.112(4) -0.007(3) -0.001(3) 0.036(3) C22 0.208(8) 0.265(8) 0.189(7) 0.056(7) 0.100(6) 0.163(7) C23 0.146(6) 0.110(4) 0.336(11) -0.093(6) 0.009(7) 0.033(5) C24 0.100(4) 0.248(9) 0.221(7) -0.078(7) -0.035(5) 0.079(5) C25 0.101(4) 0.086(3) 0.080(3) 0.027(3) 0.009(3) 0.013(3) C26 0.165(6) 0.146(6) 0.115(4) 0.075(4) 0.033(5) 0.039(5) C27 0.102(4) 0.128(5) 0.124(5) 0.050(4) 0.025(4) -0.002(4) C28 0.127(5) 0.130(5) 0.069(3) 0.010(3) 0.002(3) 0.004(4) C29 0.071(3) 0.160(5) 0.080(3) -0.022(3) 0.000(2) 0.008(3) C30 0.079(3) 0.231(6) 0.099(4) -0.034(5) 0.003(3) 0.017(4) C31 0.118(5) 0.211(7) 0.153(6) -0.084(6) -0.055(5) 0.038(5) C32 0.189(8) 0.201(7) 0.152(6) 0.054(6) -0.045(6) -0.035(6) O3 0.0764(18) 0.0774(17) 0.0646(16) -0.0053(14) 0.0041(13) 0.0161(15) C33 0.097(3) 0.099(3) 0.067(2) -0.007(2) -0.005(2) 0.015(3) C34 0.125(4) 0.120(4) 0.089(3) -0.035(3) -0.005(3) 0.020(3) C35 0.131(4) 0.100(3) 0.119(4) -0.029(3) 0.003(3) 0.031(3) C36 0.095(3) 0.090(3) 0.088(3) -0.010(2) 0.007(2) 0.030(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 O2 1.760(3) . ? Al1 O1 1.773(3) . ? Al1 O3 1.945(3) . ? Al1 C29 1.957(5) . ? Al1 S1 2.6082(15) . ? O1 C1 1.331(4) . ? O2 C15 1.325(5) . ? S1 C2 1.773(4) . ? S1 C16 1.776(4) . ? C1 C6 1.392(5) . ? C1 C2 1.412(5) . ? C2 C3 1.374(5) . ? C3 C4 1.372(6) . ? C3 H3A 0.9500 . ? C4 C5 1.393(5) . ? C4 C7 1.540(6) . ? C5 C6 1.387(5) . ? C5 H5A 0.9500 . ? C6 C11 1.549(5) . ? C7 C10 1.443(4) . ? C7 C8 1.443(4) . ? C7 C9 1.443(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.513(7) . ? C11 C12 1.520(6) . ? C11 C14 1.530(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C16 1.411(5) . ? C15 C20 1.416(5) . ? C16 C17 1.370(5) . ? C17 C18 1.375(5) . ? C17 H17A 0.9500 . ? C18 C19 1.401(6) . ? C18 C21 1.516(6) . ? C19 C20 1.373(6) . ? C19 H19A 0.9500 . ? C20 C25 1.533(6) . ? C21 C22 1.498(5) . ? C21 C23 1.498(5) . ? C21 C24 1.498(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C27 1.505(8) . ? C25 C28 1.506(8) . ? C25 C26 1.557(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.399(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.564(6) . ? C30 C32 1.565(6) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O3 C33 1.430(5) . ? O3 C36 1.464(5) . ? C33 C34 1.477(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.442(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.447(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al1 O1 114.44(14) . . ? O2 Al1 O3 91.30(13) . . ? O1 Al1 O3 91.74(13) . . ? O2 Al1 C29 117.4(2) . . ? O1 Al1 C29 126.5(2) . . ? O3 Al1 C29 99.33(18) . . ? O2 Al1 S1 82.07(9) . . ? O1 Al1 S1 81.25(9) . . ? O3 Al1 S1 167.26(11) . . ? C29 Al1 S1 93.39(15) . . ? C1 O1 Al1 130.0(2) . . ? C15 O2 Al1 129.1(2) . . ? C2 S1 C16 105.48(16) . . ? C2 S1 Al1 90.82(13) . . ? C16 S1 Al1 90.35(13) . . ? O1 C1 C6 122.6(3) . . ? O1 C1 C2 119.7(4) . . ? C6 C1 C2 117.6(3) . . ? C3 C2 C1 122.2(3) . . ? C3 C2 S1 120.2(3) . . ? C1 C2 S1 117.5(3) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 116.2(4) . . ? C3 C4 C7 120.4(4) . . ? C5 C4 C7 123.4(4) . . ? C6 C5 C4 124.7(4) . . ? C6 C5 H5A 117.6 . . ? C4 C5 H5A 117.6 . . ? C5 C6 C1 118.0(3) . . ? C5 C6 C11 120.9(4) . . ? C1 C6 C11 121.1(3) . . ? C10 C7 C8 108.6(5) . . ? C10 C7 C9 107.6(6) . . ? C8 C7 C9 104.2(6) . . ? C10 C7 C4 112.7(4) . . ? C8 C7 C4 112.3(5) . . ? C9 C7 C4 111.0(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 110.1(4) . . ? C13 C11 C14 107.2(4) . . ? C12 C11 C14 107.9(4) . . ? C13 C11 C6 110.1(4) . . ? C12 C11 C6 109.7(3) . . ? C14 C11 C6 111.8(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 120.9(3) . . ? O2 C15 C20 122.1(4) . . ? C16 C15 C20 117.0(4) . . ? C17 C16 C15 123.0(4) . . ? C17 C16 S1 119.9(3) . . ? C15 C16 S1 116.9(3) . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C19 115.9(4) . . ? C17 C18 C21 123.4(4) . . ? C19 C18 C21 120.7(4) . . ? C20 C19 C18 125.7(4) . . ? C20 C19 H19A 117.2 . . ? C18 C19 H19A 117.2 . . ? C19 C20 C15 117.3(4) . . ? C19 C20 C25 121.6(4) . . ? C15 C20 C25 121.1(4) . . ? C22 C21 C23 106.6(6) . . ? C22 C21 C24 106.2(6) . . ? C23 C21 C24 108.4(6) . . ? C22 C21 C18 112.5(4) . . ? C23 C21 C18 110.3(4) . . ? C24 C21 C18 112.5(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 112.6(5) . . ? C27 C25 C20 110.2(5) . . ? C28 C25 C20 108.8(4) . . ? C27 C25 C26 107.7(5) . . ? C28 C25 C26 106.8(5) . . ? C20 C25 C26 110.7(4) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Al1 124.0(4) . . ? C30 C29 H29A 106.3 . . ? Al1 C29 H29A 106.3 . . ? C30 C29 H29B 106.3 . . ? Al1 C29 H29B 106.3 . . ? H29A C29 H29B 106.4 . . ? C29 C30 C31 116.8(6) . . ? C29 C30 C32 106.4(5) . . ? C31 C30 C32 107.3(6) . . ? C29 C30 H30A 108.7 . . ? C31 C30 H30A 108.7 . . ? C32 C30 H30A 108.7 . . ? 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 . . ? C33 O3 C36 108.8(3) . . ? C33 O3 Al1 125.9(3) . . ? C36 O3 Al1 119.8(3) . . ? O3 C33 C34 106.1(4) . . ? O3 C33 H33A 110.5 . . ? C34 C33 H33A 110.5 . . ? O3 C33 H33B 110.5 . . ? C34 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? C35 C34 C33 106.4(4) . . ? C35 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? C35 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.6 . . ? C34 C35 C36 106.3(4) . . ? C34 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? C34 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C35 C36 O3 104.9(4) . . ? C35 C36 H36A 110.8 . . ? O3 C36 H36A 110.8 . . ? C35 C36 H36B 110.8 . . ? O3 C36 H36B 110.8 . . ? H36A C36 H36B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 O1 C1 70.6(3) . . . . ? O3 Al1 O1 C1 162.8(3) . . . . ? C29 Al1 O1 C1 -94.3(4) . . . . ? S1 Al1 O1 C1 -6.5(3) . . . . ? O1 Al1 O2 C15 -76.3(3) . . . . ? O3 Al1 O2 C15 -168.8(3) . . . . ? C29 Al1 O2 C15 90.0(4) . . . . ? S1 Al1 O2 C15 0.3(3) . . . . ? O2 Al1 S1 C2 -109.80(15) . . . . ? O1 Al1 S1 C2 6.57(14) . . . . ? O3 Al1 S1 C2 -50.6(5) . . . . ? C29 Al1 S1 C2 133.0(2) . . . . ? O2 Al1 S1 C16 -4.31(15) . . . . ? O1 Al1 S1 C16 112.06(15) . . . . ? O3 Al1 S1 C16 54.9(5) . . . . ? C29 Al1 S1 C16 -121.5(2) . . . . ? Al1 O1 C1 C6 -176.3(3) . . . . ? Al1 O1 C1 C2 3.0(5) . . . . ? O1 C1 C2 C3 -178.9(3) . . . . ? C6 C1 C2 C3 0.4(5) . . . . ? O1 C1 C2 S1 5.5(5) . . . . ? C6 C1 C2 S1 -175.2(3) . . . . ? C16 S1 C2 C3 86.2(3) . . . . ? Al1 S1 C2 C3 176.8(3) . . . . ? C16 S1 C2 C1 -98.1(3) . . . . ? Al1 S1 C2 C1 -7.5(3) . . . . ? C1 C2 C3 C4 0.0(6) . . . . ? S1 C2 C3 C4 175.5(3) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C2 C3 C4 C7 -179.9(4) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C7 C4 C5 C6 180.0(4) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? C4 C5 C6 C11 179.5(4) . . . . ? O1 C1 C6 C5 178.9(3) . . . . ? C2 C1 C6 C5 -0.3(5) . . . . ? O1 C1 C6 C11 -0.7(6) . . . . ? C2 C1 C6 C11 -180.0(3) . . . . ? C3 C4 C7 C10 -44.5(7) . . . . ? C5 C4 C7 C10 136.1(5) . . . . ? C3 C4 C7 C8 -167.5(6) . . . . ? C5 C4 C7 C8 13.1(7) . . . . ? C3 C4 C7 C9 76.3(6) . . . . ? C5 C4 C7 C9 -103.2(6) . . . . ? C5 C6 C11 C13 121.1(4) . . . . ? C1 C6 C11 C13 -59.3(5) . . . . ? C5 C6 C11 C12 -117.6(4) . . . . ? C1 C6 C11 C12 62.1(5) . . . . ? C5 C6 C11 C14 2.1(5) . . . . ? C1 C6 C11 C14 -178.3(4) . . . . ? Al1 O2 C15 C16 5.8(5) . . . . ? Al1 O2 C15 C20 -174.3(3) . . . . ? O2 C15 C16 C17 175.0(3) . . . . ? C20 C15 C16 C17 -4.9(6) . . . . ? O2 C15 C16 S1 -10.4(5) . . . . ? C20 C15 C16 S1 169.6(3) . . . . ? C2 S1 C16 C17 -86.2(3) . . . . ? Al1 S1 C16 C17 -177.1(3) . . . . ? C2 S1 C16 C15 99.1(3) . . . . ? Al1 S1 C16 C15 8.1(3) . . . . ? C15 C16 C17 C18 0.4(6) . . . . ? S1 C16 C17 C18 -174.0(3) . . . . ? C16 C17 C18 C19 2.1(6) . . . . ? C16 C17 C18 C21 -177.1(4) . . . . ? C17 C18 C19 C20 0.1(7) . . . . ? C21 C18 C19 C20 179.3(4) . . . . ? C18 C19 C20 C15 -4.6(7) . . . . ? C18 C19 C20 C25 178.3(5) . . . . ? O2 C15 C20 C19 -173.2(4) . . . . ? C16 C15 C20 C19 6.7(6) . . . . ? O2 C15 C20 C25 3.9(6) . . . . ? C16 C15 C20 C25 -176.2(4) . . . . ? C17 C18 C21 C22 12.9(7) . . . . ? C19 C18 C21 C22 -166.2(6) . . . . ? C17 C18 C21 C23 -106.0(6) . . . . ? C19 C18 C21 C23 74.9(6) . . . . ? C17 C18 C21 C24 132.9(6) . . . . ? C19 C18 C21 C24 -46.2(7) . . . . ? C19 C20 C25 C27 -129.4(5) . . . . ? C15 C20 C25 C27 53.6(6) . . . . ? C19 C20 C25 C28 106.8(5) . . . . ? C15 C20 C25 C28 -70.2(6) . . . . ? C19 C20 C25 C26 -10.3(7) . . . . ? C15 C20 C25 C26 172.8(5) . . . . ? O2 Al1 C29 C30 -132.1(5) . . . . ? O1 Al1 C29 C30 32.4(6) . . . . ? O3 Al1 C29 C30 131.6(5) . . . . ? S1 Al1 C29 C30 -49.3(6) . . . . ? Al1 C29 C30 C31 164.0(4) . . . . ? Al1 C29 C30 C32 -76.3(7) . . . . ? O2 Al1 O3 C33 34.2(4) . . . . ? O1 Al1 O3 C33 -80.3(4) . . . . ? C29 Al1 O3 C33 152.2(4) . . . . ? S1 Al1 O3 C33 -24.1(7) . . . . ? O2 Al1 O3 C36 -175.1(3) . . . . ? O1 Al1 O3 C36 70.4(3) . . . . ? C29 Al1 O3 C36 -57.1(4) . . . . ? S1 Al1 O3 C36 126.6(5) . . . . ? C36 O3 C33 C34 -1.9(6) . . . . ? Al1 O3 C33 C34 151.5(4) . . . . ? O3 C33 C34 C35 -15.1(7) . . . . ? C33 C34 C35 C36 26.5(7) . . . . ? C34 C35 C36 O3 -27.3(6) . . . . ? C33 O3 C36 C35 18.0(5) . . . . ? Al1 O3 C36 C35 -137.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.401 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.049 #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 752749' #TrackingRef 'complexes_cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H27 Al O3 S' _chemical_formula_weight 386.47 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.722(2) _cell_length_b 9.253(2) _cell_length_c 14.021(4) _cell_angle_alpha 88.920(4) _cell_angle_beta 75.986(4) _cell_angle_gamma 67.374(4) _cell_volume 1009.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9427 _exptl_absorpt_correction_T_max 0.9613 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5633 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3500 _reflns_number_gt 2916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3500 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.229 _refine_ls_shift/su_mean 0.005 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 0.74612(10) 0.38342(9) 0.14131(6) 0.0216(3) Uani 1 1 d . . . O1 O 0.7446(2) 0.5736(2) 0.15347(14) 0.0264(5) Uani 1 1 d . . . O2 O 0.7163(2) 0.2879(2) 0.25040(13) 0.0257(5) Uani 1 1 d . . . O3 O 0.9953(2) 0.2914(2) 0.11606(14) 0.0297(5) Uani 1 1 d . . . S1 S 0.40159(8) 0.55134(8) 0.22211(5) 0.0226(3) Uani 1 1 d . . . C1 C 0.6184(3) 0.7071(3) 0.2016(2) 0.0237(6) Uani 1 1 d . . . C2 C 0.4483(3) 0.7200(3) 0.23961(19) 0.0225(6) Uani 1 1 d . . . C3 C 0.3192(4) 0.8587(3) 0.2904(2) 0.0256(6) Uani 1 1 d . . . H3 H 0.2053 0.8645 0.3149 0.031 Uiso 1 1 calc R . . C4 C 0.3573(4) 0.9882(3) 0.3051(2) 0.0285(7) Uani 1 1 d . . . C5 C 0.5279(4) 0.9742(3) 0.2660(2) 0.0267(6) Uani 1 1 d . . . H5 H 0.5551 1.0624 0.2746 0.032 Uiso 1 1 calc R . . C6 C 0.6577(4) 0.8376(3) 0.2159(2) 0.0263(6) Uani 1 1 d . . . C7 C 0.2227(4) 1.1396(4) 0.3610(2) 0.0369(8) Uani 1 1 d . . . H7A H 0.1554 1.2021 0.3170 0.055 Uiso 1 1 calc R . . H7B H 0.2791 1.1993 0.3853 0.055 Uiso 1 1 calc R . . H7C H 0.1465 1.1156 0.4169 0.055 Uiso 1 1 calc R . . C8 C 0.8404(4) 0.8268(4) 0.1780(2) 0.0351(7) Uani 1 1 d . . . H8A H 0.8411 0.9323 0.1804 0.053 Uiso 1 1 calc R . . H8B H 0.8865 0.7799 0.1098 0.053 Uiso 1 1 calc R . . H8C H 0.9116 0.7613 0.2193 0.053 Uiso 1 1 calc R . . C9 C 0.5832(3) 0.3324(3) 0.33156(19) 0.0213(6) Uani 1 1 d . . . C10 C 0.4260(3) 0.4566(3) 0.33341(19) 0.0224(6) Uani 1 1 d . . . C11 C 0.2893(3) 0.5026(3) 0.41845(19) 0.0241(6) Uani 1 1 d . . . H11 H 0.1843 0.5870 0.4176 0.029 Uiso 1 1 calc R . . C12 C 0.3056(4) 0.4262(3) 0.5038(2) 0.0262(6) Uani 1 1 d . . . C13 C 0.4611(4) 0.3006(4) 0.5008(2) 0.0270(6) Uani 1 1 d . . . H13 H 0.4731 0.2457 0.5583 0.032 Uiso 1 1 calc R . . C14 C 0.5997(3) 0.2522(3) 0.4173(2) 0.0254(6) Uani 1 1 d . . . C15 C 0.1601(4) 0.4743(4) 0.5966(2) 0.0343(7) Uani 1 1 d . . . H15A H 0.1734 0.5492 0.6391 0.051 Uiso 1 1 calc R . . H15B H 0.1624 0.3813 0.6318 0.051 Uiso 1 1 calc R . . H15C H 0.0502 0.5236 0.5790 0.051 Uiso 1 1 calc R . . C16 C 0.7659(4) 0.1150(4) 0.4177(2) 0.0359(8) Uani 1 1 d . . . H16A H 0.7618 0.0820 0.4847 0.054 Uiso 1 1 calc R . . H16B H 0.8627 0.1470 0.3950 0.054 Uiso 1 1 calc R . . H16C H 0.7806 0.0272 0.3734 0.054 Uiso 1 1 calc R . . C17 C 1.0899(4) 0.1216(3) 0.1145(2) 0.0318(7) Uani 1 1 d . . . H17A H 1.0480 0.0638 0.0753 0.038 Uiso 1 1 calc R . . H17B H 1.0764 0.0874 0.1822 0.038 Uiso 1 1 calc R . . C18 C 1.2755(4) 0.0926(4) 0.0673(2) 0.0320(7) Uani 1 1 d . . . H18A H 1.3033 0.0705 -0.0050 0.038 Uiso 1 1 calc R . . H18B H 1.3537 0.0032 0.0949 0.038 Uiso 1 1 calc R . . C19 C 1.2898(4) 0.2468(4) 0.0933(2) 0.0376(8) Uani 1 1 d . . . H19A H 1.3305 0.2403 0.1539 0.045 Uiso 1 1 calc R . . H19B H 1.3708 0.2703 0.0387 0.045 Uiso 1 1 calc R . . C20 C 1.1112(4) 0.3710(4) 0.1089(3) 0.0431(8) Uani 1 1 d . . . H20A H 1.0803 0.4385 0.1702 0.052 Uiso 1 1 calc R . . H20B H 1.1042 0.4380 0.0529 0.052 Uiso 1 1 calc R . . C21 C 0.7196(4) 0.3036(4) 0.0204(2) 0.0331(7) Uani 1 1 d . . . H21A H 0.7040 0.2047 0.0315 0.050 Uiso 1 1 calc R . . H21B H 0.8225 0.2854 -0.0331 0.050 Uiso 1 1 calc R . . H21C H 0.6190 0.3808 0.0026 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0216(5) 0.0226(5) 0.0213(5) 0.0033(3) -0.0038(3) -0.0103(4) O1 0.0246(10) 0.0232(11) 0.0309(11) 0.0031(8) -0.0031(8) -0.0113(8) O2 0.0222(10) 0.0278(11) 0.0247(10) 0.0069(8) -0.0036(8) -0.0089(8) O3 0.0248(10) 0.0242(11) 0.0403(12) 0.0028(9) -0.0037(9) -0.0127(9) S1 0.0253(4) 0.0233(4) 0.0230(4) 0.0043(3) -0.0077(3) -0.0126(3) C1 0.0275(15) 0.0236(15) 0.0223(14) 0.0067(11) -0.0082(11) -0.0115(12) C2 0.0297(15) 0.0205(14) 0.0225(14) 0.0083(11) -0.0112(11) -0.0130(12) C3 0.0283(15) 0.0283(16) 0.0227(14) 0.0061(11) -0.0087(12) -0.0127(12) C4 0.0373(17) 0.0225(15) 0.0242(15) 0.0045(11) -0.0076(12) -0.0105(13) C5 0.0362(16) 0.0239(15) 0.0279(15) 0.0072(12) -0.0125(13) -0.0177(13) C6 0.0311(15) 0.0293(16) 0.0254(14) 0.0096(12) -0.0104(12) -0.0176(13) C7 0.0394(18) 0.0260(16) 0.0401(18) -0.0009(13) -0.0050(14) -0.0101(14) C8 0.0391(18) 0.0337(17) 0.0386(18) 0.0060(13) -0.0038(14) -0.0244(14) C9 0.0181(13) 0.0217(14) 0.0257(14) 0.0046(11) -0.0079(11) -0.0084(11) C10 0.0281(15) 0.0223(14) 0.0230(14) 0.0023(11) -0.0062(11) -0.0166(12) C11 0.0230(14) 0.0252(15) 0.0281(15) 0.0018(11) -0.0060(12) -0.0139(12) C12 0.0277(15) 0.0323(16) 0.0240(14) 0.0003(12) -0.0042(12) -0.0190(13) C13 0.0333(16) 0.0366(17) 0.0198(14) 0.0052(12) -0.0080(12) -0.0222(14) C14 0.0251(15) 0.0284(15) 0.0279(15) 0.0064(12) -0.0102(12) -0.0142(12) C15 0.0321(17) 0.0422(18) 0.0276(16) 0.0032(13) -0.0032(13) -0.0161(14) C16 0.0285(16) 0.0425(19) 0.0326(16) 0.0149(14) -0.0117(13) -0.0075(14) C17 0.0287(15) 0.0232(16) 0.0397(17) 0.0021(13) -0.0032(13) -0.0094(13) C18 0.0243(15) 0.0333(17) 0.0334(16) 0.0065(13) -0.0059(12) -0.0068(13) C19 0.0272(16) 0.0444(19) 0.0469(19) 0.0109(15) -0.0103(14) -0.0200(15) C20 0.0284(17) 0.0391(19) 0.069(2) 0.0092(17) -0.0143(16) -0.0201(15) C21 0.0297(16) 0.0439(19) 0.0278(15) -0.0035(13) -0.0046(12) -0.0180(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.766(2) . ? Al1 O2 1.7668(19) . ? Al1 O3 1.947(2) . ? Al1 C21 1.959(3) . ? Al1 S1 2.7482(12) . ? O1 C1 1.348(3) . ? O2 C9 1.350(3) . ? O3 C20 1.447(3) . ? O3 C17 1.464(3) . ? S1 C10 1.793(3) . ? S1 C2 1.792(3) . ? C1 C6 1.406(4) . ? C1 C2 1.408(4) . ? C2 C3 1.398(4) . ? C3 C4 1.392(4) . ? C3 H3 0.9500 . ? C4 C5 1.411(4) . ? C4 C7 1.512(4) . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 C8 1.517(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.404(4) . ? C9 C14 1.409(4) . ? C10 C11 1.402(4) . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C12 C13 1.398(4) . ? C12 C15 1.513(4) . ? C13 C14 1.397(4) . ? C13 H13 0.9500 . ? C14 C16 1.517(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.512(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.537(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.504(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 O2 117.29(10) . . ? O1 Al1 O3 90.60(9) . . ? O2 Al1 O3 93.32(9) . . ? O1 Al1 C21 121.37(12) . . ? O2 Al1 C21 119.38(12) . . ? O3 Al1 C21 99.90(11) . . ? O1 Al1 S1 80.03(7) . . ? O2 Al1 S1 79.93(7) . . ? O3 Al1 S1 164.16(7) . . ? C21 Al1 S1 95.89(9) . . ? C1 O1 Al1 129.98(17) . . ? C9 O2 Al1 129.69(16) . . ? C20 O3 C17 109.9(2) . . ? C20 O3 Al1 128.30(18) . . ? C17 O3 Al1 121.36(16) . . ? C10 S1 C2 102.57(12) . . ? C10 S1 Al1 88.33(9) . . ? C2 S1 Al1 88.75(9) . . ? O1 C1 C6 119.1(2) . . ? O1 C1 C2 122.3(2) . . ? C6 C1 C2 118.6(3) . . ? C3 C2 C1 121.6(3) . . ? C3 C2 S1 120.6(2) . . ? C1 C2 S1 117.8(2) . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C7 122.1(3) . . ? C5 C4 C7 120.2(3) . . ? C6 C5 C4 123.0(3) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C1 119.0(3) . . ? C5 C6 C8 121.0(3) . . ? C1 C6 C8 120.0(3) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 122.0(2) . . ? O2 C9 C14 119.8(2) . . ? C10 C9 C14 118.2(2) . . ? C11 C10 C9 121.4(2) . . ? C11 C10 S1 120.5(2) . . ? C9 C10 S1 118.1(2) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 117.6(3) . . ? C11 C12 C15 121.6(3) . . ? C13 C12 C15 120.8(3) . . ? C14 C13 C12 123.0(3) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C9 119.0(3) . . ? C13 C14 C16 121.1(3) . . ? C9 C14 C16 119.9(2) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 105.4(2) . . ? O3 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? O3 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C17 C18 C19 103.9(2) . . ? C17 C18 H18A 111.0 . . ? C19 C18 H18A 111.0 . . ? C17 C18 H18B 111.0 . . ? C19 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C20 C19 C18 105.2(2) . . ? C20 C19 H19A 110.7 . . ? C18 C19 H19A 110.7 . . ? C20 C19 H19B 110.7 . . ? C18 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? O3 C20 C19 107.4(3) . . ? O3 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? O3 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 O1 C1 -62.3(2) . . . . ? O3 Al1 O1 C1 -156.3(2) . . . . ? C21 Al1 O1 C1 101.7(2) . . . . ? S1 Al1 O1 C1 10.8(2) . . . . ? O1 Al1 O2 C9 59.3(2) . . . . ? O3 Al1 O2 C9 151.7(2) . . . . ? C21 Al1 O2 C9 -105.0(2) . . . . ? S1 Al1 O2 C9 -13.9(2) . . . . ? O1 Al1 O3 C20 -2.2(3) . . . . ? O2 Al1 O3 C20 -119.6(2) . . . . ? C21 Al1 O3 C20 119.8(3) . . . . ? S1 Al1 O3 C20 -55.5(4) . . . . ? O1 Al1 O3 C17 169.4(2) . . . . ? O2 Al1 O3 C17 52.1(2) . . . . ? C21 Al1 O3 C17 -68.5(2) . . . . ? S1 Al1 O3 C17 116.1(3) . . . . ? O1 Al1 S1 C10 -109.92(10) . . . . ? O2 Al1 S1 C10 10.35(10) . . . . ? O3 Al1 S1 C10 -55.4(3) . . . . ? C21 Al1 S1 C10 129.20(13) . . . . ? O1 Al1 S1 C2 -7.30(10) . . . . ? O2 Al1 S1 C2 112.97(11) . . . . ? O3 Al1 S1 C2 47.2(3) . . . . ? C21 Al1 S1 C2 -128.18(12) . . . . ? Al1 O1 C1 C6 168.46(18) . . . . ? Al1 O1 C1 C2 -10.7(4) . . . . ? O1 C1 C2 C3 179.3(2) . . . . ? C6 C1 C2 C3 0.2(4) . . . . ? O1 C1 C2 S1 -0.1(4) . . . . ? C6 C1 C2 S1 -179.17(18) . . . . ? C10 S1 C2 C3 -86.0(2) . . . . ? Al1 S1 C2 C3 -174.1(2) . . . . ? C10 S1 C2 C1 93.3(2) . . . . ? Al1 S1 C2 C1 5.3(2) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? S1 C2 C3 C4 178.90(19) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C2 C3 C4 C7 -178.9(3) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C7 C4 C5 C6 178.7(3) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C4 C5 C6 C8 -178.1(2) . . . . ? O1 C1 C6 C5 -179.5(2) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? O1 C1 C6 C8 -0.5(4) . . . . ? C2 C1 C6 C8 178.6(2) . . . . ? Al1 O2 C9 C10 12.1(4) . . . . ? Al1 O2 C9 C14 -168.56(18) . . . . ? O2 C9 C10 C11 -179.4(2) . . . . ? C14 C9 C10 C11 1.2(4) . . . . ? O2 C9 C10 S1 2.7(3) . . . . ? C14 C9 C10 S1 -176.64(19) . . . . ? C2 S1 C10 C11 85.0(2) . . . . ? Al1 S1 C10 C11 173.4(2) . . . . ? C2 S1 C10 C9 -97.1(2) . . . . ? Al1 S1 C10 C9 -8.76(19) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? S1 C10 C11 C12 177.81(19) . . . . ? C10 C11 C12 C13 -1.3(4) . . . . ? C10 C11 C12 C15 179.6(2) . . . . ? C11 C12 C13 C14 1.4(4) . . . . ? C15 C12 C13 C14 -179.5(2) . . . . ? C12 C13 C14 C9 -0.2(4) . . . . ? C12 C13 C14 C16 -179.9(3) . . . . ? O2 C9 C14 C13 179.5(2) . . . . ? C10 C9 C14 C13 -1.1(4) . . . . ? O2 C9 C14 C16 -0.8(4) . . . . ? C10 C9 C14 C16 178.6(2) . . . . ? C20 O3 C17 C18 -21.3(3) . . . . ? Al1 O3 C17 C18 165.62(17) . . . . ? O3 C17 C18 C19 28.4(3) . . . . ? C17 C18 C19 C20 -25.4(3) . . . . ? C17 O3 C20 C19 5.0(3) . . . . ? Al1 O3 C20 C19 177.42(19) . . . . ? C18 C19 C20 O3 13.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.496 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.086 #===END data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 752750' #TrackingRef 'complexes_cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 Al Cl O3 S' _chemical_formula_weight 575.19 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' 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' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.463(2) _cell_length_b 11.788(3) _cell_length_c 26.013(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.027(5) _cell_angle_gamma 90.00 _cell_volume 3190.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9178 _exptl_absorpt_correction_T_max 0.9599 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12212 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5185 _reflns_number_gt 3809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5185 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.59135(8) 0.40238(7) 0.23981(3) 0.0188(2) Uani 1 1 d . . . O1 O 0.63335(17) 0.32593(16) 0.29686(7) 0.0198(5) Uani 1 1 d . . . O2 O 0.58393(17) 0.32871(16) 0.18117(7) 0.0200(5) Uani 1 1 d . . . O3 O 0.76294(16) 0.44829(16) 0.23416(7) 0.0203(5) Uani 1 1 d . . . S1 S 0.37074(6) 0.31082(6) 0.24577(3) 0.01852(19) Uani 1 1 d . . . C1 C 0.5598(3) 0.2530(2) 0.32091(11) 0.0186(7) Uani 1 1 d . . . C2 C 0.4346(3) 0.2287(2) 0.29995(11) 0.0181(6) Uani 1 1 d . . . C3 C 0.3558(3) 0.1538(2) 0.32382(11) 0.0193(7) Uani 1 1 d . . . H3 H 0.2709 0.1394 0.3086 0.023 Uiso 1 1 calc R . . C4 C 0.4006(3) 0.1006(2) 0.36935(11) 0.0209(7) Uani 1 1 d . . . C5 C 0.5262(3) 0.1265(2) 0.38991(11) 0.0210(7) Uani 1 1 d . . . H5 H 0.5579 0.0904 0.4213 0.025 Uiso 1 1 calc R . . C6 C 0.6079(3) 0.2007(2) 0.36812(11) 0.0196(7) Uani 1 1 d . . . C7 C 0.3200(3) 0.0177(2) 0.39837(11) 0.0235(7) Uani 1 1 d . . . C8 C 0.1852(3) 0.0058(3) 0.37149(12) 0.0315(8) Uani 1 1 d . . . H8A H 0.1368 -0.0483 0.3905 0.047 Uiso 1 1 calc R . . H8B H 0.1893 -0.0217 0.3362 0.047 Uiso 1 1 calc R . . H8C H 0.1422 0.0798 0.3704 0.047 Uiso 1 1 calc R . . C9 C 0.3846(3) -0.0994(3) 0.40153(13) 0.0355(8) Uani 1 1 d . . . H9A H 0.3336 -0.1517 0.4204 0.053 Uiso 1 1 calc R . . H9B H 0.4712 -0.0927 0.4197 0.053 Uiso 1 1 calc R . . H9C H 0.3902 -0.1284 0.3665 0.053 Uiso 1 1 calc R . . C10 C 0.3104(3) 0.0625(3) 0.45330(12) 0.0334(8) Uani 1 1 d . . . H10A H 0.2689 0.1371 0.4514 0.050 Uiso 1 1 calc R . . H10B H 0.3968 0.0692 0.4716 0.050 Uiso 1 1 calc R . . H10C H 0.2594 0.0097 0.4719 0.050 Uiso 1 1 calc R . . C11 C 0.7434(3) 0.2260(2) 0.39417(11) 0.0197(7) Uani 1 1 d . . . C12 C 0.8421(3) 0.1845(3) 0.35837(12) 0.0278(8) Uani 1 1 d . . . H12A H 0.9288 0.2059 0.3731 0.042 Uiso 1 1 calc R . . H12B H 0.8236 0.2195 0.3242 0.042 Uiso 1 1 calc R . . H12C H 0.8367 0.1018 0.3550 0.042 Uiso 1 1 calc R . . C13 C 0.7605(3) 0.3538(2) 0.40459(11) 0.0246(7) Uani 1 1 d . . . H13A H 0.7010 0.3783 0.4291 0.037 Uiso 1 1 calc R . . H13B H 0.7424 0.3957 0.3721 0.037 Uiso 1 1 calc R . . H13C H 0.8491 0.3688 0.4192 0.037 Uiso 1 1 calc R . . C14 C 0.7709(3) 0.1649(3) 0.44559(11) 0.0282(7) Uani 1 1 d . . . H14A H 0.7093 0.1899 0.4692 0.042 Uiso 1 1 calc R . . H14B H 0.8584 0.1827 0.4607 0.042 Uiso 1 1 calc R . . H14C H 0.7626 0.0829 0.4401 0.042 Uiso 1 1 calc R . . C15 C 0.4920(3) 0.2553(2) 0.16167(11) 0.0180(7) Uani 1 1 d . . . C16 C 0.3867(3) 0.2305(2) 0.18865(11) 0.0174(6) Uani 1 1 d . . . C17 C 0.2896(2) 0.1566(2) 0.16952(11) 0.0180(6) Uani 1 1 d . . . H17 H 0.2181 0.1437 0.1885 0.022 Uiso 1 1 calc R . . C18 C 0.2969(3) 0.1019(2) 0.12294(11) 0.0187(7) Uani 1 1 d . . . C19 C 0.4032(2) 0.1267(2) 0.09634(11) 0.0192(7) Uani 1 1 d . . . H19 H 0.4093 0.0891 0.0644 0.023 Uiso 1 1 calc R . . C20 C 0.5002(3) 0.2024(2) 0.11336(11) 0.0184(7) Uani 1 1 d . . . C21 C 0.1985(3) 0.0135(3) 0.10085(12) 0.0255(7) Uani 1 1 d . . . C22 C 0.2620(3) -0.1046(3) 0.10560(13) 0.0359(8) Uani 1 1 d . . . H22A H 0.2867 -0.1220 0.1421 0.054 Uiso 1 1 calc R . . H22B H 0.3386 -0.1051 0.0869 0.054 Uiso 1 1 calc R . . H22C H 0.2010 -0.1619 0.0907 0.054 Uiso 1 1 calc R . . C23 C 0.1570(3) 0.0368(3) 0.04392(12) 0.0398(9) Uani 1 1 d . . . H23A H 0.0956 -0.0213 0.0303 0.060 Uiso 1 1 calc R . . H23B H 0.2325 0.0351 0.0246 0.060 Uiso 1 1 calc R . . H23C H 0.1164 0.1117 0.0403 0.060 Uiso 1 1 calc R . . C24 C 0.0799(3) 0.0111(3) 0.13010(13) 0.0394(9) Uani 1 1 d . . . H24A H 0.0382 0.0856 0.1278 0.059 Uiso 1 1 calc R . . H24B H 0.1053 -0.0075 0.1665 0.059 Uiso 1 1 calc R . . H24C H 0.0197 -0.0465 0.1149 0.059 Uiso 1 1 calc R . . C25 C 0.6118(3) 0.2266(2) 0.08041(11) 0.0217(7) Uani 1 1 d . . . C26 C 0.5947(3) 0.1650(3) 0.02800(11) 0.0283(8) Uani 1 1 d . . . H26A H 0.6671 0.1831 0.0084 0.042 Uiso 1 1 calc R . . H26B H 0.5144 0.1897 0.0084 0.042 Uiso 1 1 calc R . . H26C H 0.5917 0.0829 0.0337 0.042 Uiso 1 1 calc R . . C27 C 0.6197(3) 0.3538(2) 0.06923(12) 0.0280(7) Uani 1 1 d . . . H27A H 0.6363 0.3954 0.1019 0.042 Uiso 1 1 calc R . . H27B H 0.5382 0.3795 0.0509 0.042 Uiso 1 1 calc R . . H27C H 0.6896 0.3679 0.0478 0.042 Uiso 1 1 calc R . . C28 C 0.7383(3) 0.1845(3) 0.10863(12) 0.0260(7) Uani 1 1 d . . . H28A H 0.8101 0.2120 0.0907 0.039 Uiso 1 1 calc R . . H28B H 0.7388 0.1014 0.1091 0.039 Uiso 1 1 calc R . . H28C H 0.7472 0.2133 0.1442 0.039 Uiso 1 1 calc R . . C29 C 0.8575(3) 0.3710(3) 0.21434(12) 0.0279(8) Uani 1 1 d . . . H29A H 0.8545 0.3770 0.1763 0.034 Uiso 1 1 calc R . . H29B H 0.8400 0.2914 0.2235 0.034 Uiso 1 1 calc R . . C30 C 0.9867(3) 0.4087(3) 0.23991(12) 0.0326(8) Uani 1 1 d . . . H30A H 1.0269 0.4650 0.2184 0.039 Uiso 1 1 calc R . . H30B H 1.0456 0.3434 0.2467 0.039 Uiso 1 1 calc R . . C31 C 0.9524(3) 0.4615(3) 0.29013(12) 0.0279(8) Uani 1 1 d . . . H31A H 0.9384 0.4025 0.3161 0.033 Uiso 1 1 calc R . . H31B H 1.0203 0.5142 0.3048 0.033 Uiso 1 1 calc R . . C32 C 0.8300(3) 0.5237(3) 0.27298(12) 0.0263(7) Uani 1 1 d . . . H32A H 0.7784 0.5358 0.3023 0.032 Uiso 1 1 calc R . . H32B H 0.8482 0.5981 0.2577 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.51925(7) 0.57251(6) 0.24635(3) 0.0250(2) 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 0.0223(5) 0.0168(5) 0.0175(5) -0.0005(4) 0.0036(4) -0.0021(3) O1 0.0218(10) 0.0202(11) 0.0176(11) 0.0043(9) 0.0039(9) -0.0043(8) O2 0.0224(10) 0.0206(11) 0.0175(11) -0.0034(9) 0.0049(9) -0.0030(8) O3 0.0220(11) 0.0204(11) 0.0190(12) -0.0041(9) 0.0040(9) -0.0043(8) S1 0.0213(4) 0.0180(4) 0.0165(4) 0.0002(3) 0.0033(3) 0.0007(3) C1 0.0255(16) 0.0140(15) 0.0174(17) -0.0027(13) 0.0077(13) -0.0013(12) C2 0.0241(15) 0.0166(15) 0.0143(16) 0.0018(12) 0.0052(13) 0.0022(12) C3 0.0229(15) 0.0158(15) 0.0196(17) -0.0034(13) 0.0044(13) 0.0016(12) C4 0.0285(16) 0.0173(16) 0.0179(17) -0.0012(13) 0.0073(13) -0.0003(12) C5 0.0272(16) 0.0198(16) 0.0161(17) -0.0022(13) 0.0032(13) 0.0015(12) C6 0.0253(16) 0.0154(15) 0.0185(17) -0.0037(13) 0.0038(13) 0.0032(12) C7 0.0304(17) 0.0215(17) 0.0200(18) 0.0008(14) 0.0093(14) -0.0069(13) C8 0.0358(18) 0.0329(19) 0.027(2) 0.0050(16) 0.0071(15) -0.0126(14) C9 0.046(2) 0.0244(18) 0.038(2) 0.0043(16) 0.0141(17) -0.0082(15) C10 0.048(2) 0.0309(19) 0.0241(19) 0.0012(16) 0.0145(16) -0.0103(16) C11 0.0236(15) 0.0180(15) 0.0175(17) -0.0009(13) 0.0032(13) -0.0001(12) C12 0.0242(16) 0.0272(18) 0.032(2) -0.0030(15) 0.0009(14) 0.0022(13) C13 0.0294(16) 0.0222(17) 0.0218(18) -0.0023(14) 0.0010(14) -0.0003(13) C14 0.0326(17) 0.0245(18) 0.0263(19) 0.0035(14) -0.0029(14) -0.0018(13) C15 0.0201(15) 0.0131(15) 0.0203(17) 0.0031(13) -0.0006(13) 0.0011(11) C16 0.0231(15) 0.0160(15) 0.0137(16) 0.0003(12) 0.0050(13) 0.0026(12) C17 0.0179(14) 0.0182(15) 0.0179(17) 0.0038(13) 0.0028(12) 0.0010(11) C18 0.0223(15) 0.0145(15) 0.0194(17) 0.0027(13) 0.0026(13) 0.0012(11) C19 0.0257(16) 0.0193(16) 0.0131(16) -0.0008(13) 0.0044(13) 0.0008(12) C20 0.0237(15) 0.0160(15) 0.0157(17) 0.0019(13) 0.0034(13) -0.0003(12) C21 0.0305(17) 0.0259(18) 0.0201(18) -0.0038(14) 0.0025(14) -0.0076(13) C22 0.046(2) 0.0262(19) 0.036(2) -0.0033(16) 0.0038(16) -0.0114(15) C23 0.043(2) 0.048(2) 0.027(2) 0.0004(17) -0.0065(16) -0.0154(17) C24 0.0360(19) 0.043(2) 0.040(2) -0.0133(18) 0.0091(17) -0.0176(16) C25 0.0248(16) 0.0221(16) 0.0193(17) -0.0015(13) 0.0073(13) -0.0017(12) C26 0.0320(17) 0.0312(19) 0.0235(19) -0.0045(15) 0.0110(14) -0.0030(14) C27 0.0371(18) 0.0230(17) 0.0262(19) 0.0015(14) 0.0137(15) -0.0012(14) C28 0.0245(16) 0.0269(18) 0.0280(19) -0.0057(15) 0.0090(14) -0.0025(13) C29 0.0258(16) 0.0250(18) 0.035(2) -0.0044(15) 0.0108(14) -0.0014(13) C30 0.0228(16) 0.035(2) 0.040(2) -0.0051(16) 0.0053(15) -0.0046(13) C31 0.0294(17) 0.0282(18) 0.0250(19) 0.0012(15) -0.0015(14) -0.0079(13) C32 0.0334(18) 0.0213(17) 0.0243(19) -0.0061(14) 0.0030(14) -0.0063(13) Cl1 0.0314(4) 0.0179(4) 0.0264(5) -0.0009(3) 0.0067(3) 0.0001(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 O2 1.750(2) . ? Al1 O1 1.752(2) . ? Al1 O3 1.8956(19) . ? Al1 Cl1 2.1556(12) . ? Al1 S1 2.5676(12) . ? O1 C1 1.350(3) . ? O2 C15 1.352(3) . ? O3 C32 1.467(3) . ? O3 C29 1.477(3) . ? S1 C2 1.781(3) . ? S1 C16 1.785(3) . ? C1 C2 1.395(4) . ? C1 C6 1.418(4) . ? C2 C3 1.398(4) . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.399(4) . ? C4 C7 1.539(4) . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 C11 1.536(4) . ? C7 C8 1.513(4) . ? C7 C9 1.536(4) . ? C7 C10 1.536(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.520(4) . ? C11 C13 1.537(4) . ? C11 C12 1.541(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C16 1.398(4) . ? C15 C20 1.414(4) . ? C16 C17 1.391(4) . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 C19 1.401(4) . ? C18 C21 1.534(4) . ? C19 C20 1.389(4) . ? C19 H19 0.9500 . ? C20 C25 1.545(4) . ? C21 C24 1.522(4) . ? C21 C23 1.524(4) . ? C21 C22 1.542(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C28 1.528(4) . ? C25 C27 1.531(4) . ? C25 C26 1.539(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.509(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.524(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.502(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al1 O1 117.85(10) . . ? O2 Al1 O3 91.70(9) . . ? O1 Al1 O3 93.28(9) . . ? O2 Al1 Cl1 123.13(8) . . ? O1 Al1 Cl1 118.07(8) . . ? O3 Al1 Cl1 94.74(7) . . ? O2 Al1 S1 83.46(7) . . ? O1 Al1 S1 83.10(7) . . ? O3 Al1 S1 171.69(7) . . ? Cl1 Al1 S1 93.56(4) . . ? C1 O1 Al1 127.96(17) . . ? C15 O2 Al1 127.53(18) . . ? C32 O3 C29 108.93(19) . . ? C32 O3 Al1 120.51(16) . . ? C29 O3 Al1 121.72(16) . . ? C2 S1 C16 108.09(13) . . ? C2 S1 Al1 90.64(9) . . ? C16 S1 Al1 90.53(10) . . ? O1 C1 C2 120.5(3) . . ? O1 C1 C6 120.7(2) . . ? C2 C1 C6 118.8(2) . . ? C1 C2 C3 122.0(3) . . ? C1 C2 S1 117.2(2) . . ? C3 C2 S1 120.4(2) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 116.7(3) . . ? C3 C4 C7 123.8(3) . . ? C5 C4 C7 119.5(3) . . ? C6 C5 C4 125.2(3) . . ? C6 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? C5 C6 C1 116.8(2) . . ? C5 C6 C11 121.5(3) . . ? C1 C6 C11 121.7(2) . . ? C8 C7 C9 109.0(3) . . ? C8 C7 C10 108.2(2) . . ? C9 C7 C10 109.3(3) . . ? C8 C7 C4 111.4(2) . . ? C9 C7 C4 109.6(2) . . ? C10 C7 C4 109.3(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C6 112.1(2) . . ? C14 C11 C13 107.5(2) . . ? C6 C11 C13 110.7(2) . . ? C14 C11 C12 107.7(2) . . ? C6 C11 C12 108.6(2) . . ? C13 C11 C12 110.1(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 120.8(3) . . ? O2 C15 C20 120.6(2) . . ? C16 C15 C20 118.6(2) . . ? C17 C16 C15 122.4(3) . . ? C17 C16 S1 120.1(2) . . ? C15 C16 S1 117.0(2) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 117.1(2) . . ? C17 C18 C21 123.3(3) . . ? C19 C18 C21 119.6(3) . . ? C20 C19 C18 124.6(3) . . ? C20 C19 H19 117.7 . . ? C18 C19 H19 117.7 . . ? C19 C20 C15 117.2(3) . . ? C19 C20 C25 120.8(3) . . ? C15 C20 C25 122.1(2) . . ? C24 C21 C23 109.0(3) . . ? C24 C21 C18 112.1(2) . . ? C23 C21 C18 110.6(2) . . ? C24 C21 C22 108.1(3) . . ? C23 C21 C22 108.5(3) . . ? C18 C21 C22 108.4(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 110.3(2) . . ? C28 C25 C26 106.7(2) . . ? C27 C25 C26 107.3(2) . . ? C28 C25 C20 109.9(2) . . ? C27 C25 C20 110.2(2) . . ? C26 C25 C20 112.3(2) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 105.5(2) . . ? O3 C29 H29A 110.7 . . ? C30 C29 H29A 110.7 . . ? O3 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C31 102.6(2) . . ? C29 C30 H30A 111.3 . . ? C31 C30 H30A 111.3 . . ? C29 C30 H30B 111.3 . . ? C31 C30 H30B 111.3 . . ? H30A C30 H30B 109.2 . . ? C32 C31 C30 102.4(2) . . ? C32 C31 H31A 111.3 . . ? C30 C31 H31A 111.3 . . ? C32 C31 H31B 111.3 . . ? C30 C31 H31B 111.3 . . ? H31A C31 H31B 109.2 . . ? O3 C32 C31 103.9(2) . . ? O3 C32 H32A 111.0 . . ? C31 C32 H32A 111.0 . . ? O3 C32 H32B 111.0 . . ? C31 C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 O1 C1 -75.5(2) . . . . ? O3 Al1 O1 C1 -169.2(2) . . . . ? Cl1 Al1 O1 C1 93.7(2) . . . . ? S1 Al1 O1 C1 3.3(2) . . . . ? O1 Al1 O2 C15 74.2(2) . . . . ? O3 Al1 O2 C15 168.8(2) . . . . ? Cl1 Al1 O2 C15 -94.4(2) . . . . ? S1 Al1 O2 C15 -4.4(2) . . . . ? O2 Al1 O3 C32 176.68(19) . . . . ? O1 Al1 O3 C32 -65.3(2) . . . . ? Cl1 Al1 O3 C32 53.23(19) . . . . ? S1 Al1 O3 C32 -129.1(5) . . . . ? O2 Al1 O3 C29 -39.5(2) . . . . ? O1 Al1 O3 C29 78.5(2) . . . . ? Cl1 Al1 O3 C29 -162.98(19) . . . . ? S1 Al1 O3 C29 14.7(6) . . . . ? O2 Al1 S1 C2 113.75(11) . . . . ? O1 Al1 S1 C2 -5.43(11) . . . . ? O3 Al1 S1 C2 59.1(5) . . . . ? Cl1 Al1 S1 C2 -123.29(10) . . . . ? O2 Al1 S1 C16 5.65(11) . . . . ? O1 Al1 S1 C16 -113.53(11) . . . . ? O3 Al1 S1 C16 -49.0(5) . . . . ? Cl1 Al1 S1 C16 128.61(9) . . . . ? Al1 O1 C1 C2 1.5(4) . . . . ? Al1 O1 C1 C6 -177.88(19) . . . . ? O1 C1 C2 C3 -180.0(2) . . . . ? C6 C1 C2 C3 -0.6(4) . . . . ? O1 C1 C2 S1 -7.9(4) . . . . ? C6 C1 C2 S1 171.5(2) . . . . ? C16 S1 C2 C1 98.6(2) . . . . ? Al1 S1 C2 C1 7.8(2) . . . . ? C16 S1 C2 C3 -89.2(2) . . . . ? Al1 S1 C2 C3 -180.0(2) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? S1 C2 C3 C4 -172.1(2) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C2 C3 C4 C7 179.5(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C7 C4 C5 C6 -179.0(3) . . . . ? C4 C5 C6 C1 -0.8(4) . . . . ? C4 C5 C6 C11 178.6(3) . . . . ? O1 C1 C6 C5 -179.6(2) . . . . ? C2 C1 C6 C5 1.1(4) . . . . ? O1 C1 C6 C11 1.0(4) . . . . ? C2 C1 C6 C11 -178.3(3) . . . . ? C3 C4 C7 C8 -1.9(4) . . . . ? C5 C4 C7 C8 176.9(3) . . . . ? C3 C4 C7 C9 118.8(3) . . . . ? C5 C4 C7 C9 -62.4(3) . . . . ? C3 C4 C7 C10 -121.5(3) . . . . ? C5 C4 C7 C10 57.3(4) . . . . ? C5 C6 C11 C14 -2.3(4) . . . . ? C1 C6 C11 C14 177.0(3) . . . . ? C5 C6 C11 C13 -122.4(3) . . . . ? C1 C6 C11 C13 57.0(3) . . . . ? C5 C6 C11 C12 116.6(3) . . . . ? C1 C6 C11 C12 -64.0(3) . . . . ? Al1 O2 C15 C16 0.3(4) . . . . ? Al1 O2 C15 C20 -179.94(19) . . . . ? O2 C15 C16 C17 179.2(2) . . . . ? C20 C15 C16 C17 -0.6(4) . . . . ? O2 C15 C16 S1 6.6(3) . . . . ? C20 C15 C16 S1 -173.2(2) . . . . ? C2 S1 C16 C17 89.1(2) . . . . ? Al1 S1 C16 C17 179.9(2) . . . . ? C2 S1 C16 C15 -98.2(2) . . . . ? Al1 S1 C16 C15 -7.3(2) . . . . ? C15 C16 C17 C18 2.0(4) . . . . ? S1 C16 C17 C18 174.4(2) . . . . ? C16 C17 C18 C19 -1.5(4) . . . . ? C16 C17 C18 C21 176.0(3) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? C21 C18 C19 C20 -178.0(3) . . . . ? C18 C19 C20 C15 1.7(4) . . . . ? C18 C19 C20 C25 -178.3(3) . . . . ? O2 C15 C20 C19 179.0(2) . . . . ? C16 C15 C20 C19 -1.2(4) . . . . ? O2 C15 C20 C25 -1.0(4) . . . . ? C16 C15 C20 C25 178.8(2) . . . . ? C17 C18 C21 C24 11.5(4) . . . . ? C19 C18 C21 C24 -171.0(3) . . . . ? C17 C18 C21 C23 133.4(3) . . . . ? C19 C18 C21 C23 -49.1(4) . . . . ? C17 C18 C21 C22 -107.7(3) . . . . ? C19 C18 C21 C22 69.8(3) . . . . ? C19 C20 C25 C28 -114.8(3) . . . . ? C15 C20 C25 C28 65.2(3) . . . . ? C19 C20 C25 C27 123.4(3) . . . . ? C15 C20 C25 C27 -56.6(3) . . . . ? C19 C20 C25 C26 3.8(4) . . . . ? C15 C20 C25 C26 -176.2(3) . . . . ? C32 O3 C29 C30 -4.2(3) . . . . ? Al1 O3 C29 C30 -151.62(19) . . . . ? O3 C29 C30 C31 27.3(3) . . . . ? C29 C30 C31 C32 -40.0(3) . . . . ? C29 O3 C32 C31 -21.1(3) . . . . ? Al1 O3 C32 C31 126.8(2) . . . . ? C30 C31 C32 O3 37.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.354 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.058 #===END data_complex_8 _database_code_depnum_ccdc_archive 'CCDC 752751' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H86 Al2 O4 S2' _chemical_formula_weight 965.35 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.976(3) _cell_length_b 25.200(11) _cell_length_c 26.683(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.599(18) _cell_angle_gamma 90.00 _cell_volume 5968(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9524 _exptl_absorpt_correction_T_max 0.9704 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48004 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 23.00 _reflns_number_total 8303 _reflns_number_gt 7750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+36.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8303 _refine_ls_number_parameters 628 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_gt 0.1348 _refine_ls_wR_factor_ref 0.2680 _refine_ls_wR_factor_gt 0.2643 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.9352(2) 0.74118(8) 0.25490(7) 0.0366(5) Uani 1 1 d . . . Al2 Al 0.9296(3) 0.85814(9) 0.25233(9) 0.0515(6) Uani 1 1 d . . . S1 S 1.14291(19) 0.73954(7) 0.32643(6) 0.0376(4) Uani 1 1 d . . . S2 S 0.72751(19) 0.73594(7) 0.18291(6) 0.0368(4) Uani 1 1 d . . . O1 O 0.8708(5) 0.80247(17) 0.29127(16) 0.0398(11) Uani 1 1 d . . . O2 O 0.8440(5) 0.69536(18) 0.29248(16) 0.0413(12) Uani 1 1 d . . . O3 O 1.0270(5) 0.69408(18) 0.21877(16) 0.0384(11) Uani 1 1 d . . . O4 O 0.9960(5) 0.80117(17) 0.21631(16) 0.0418(12) Uani 1 1 d . . . C1 C 0.9086(8) 0.8047(3) 0.3442(3) 0.0424(18) Uani 1 1 d . . . C2 C 0.8178(9) 0.8292(3) 0.3759(3) 0.0445(18) Uani 1 1 d . . . C3 C 0.8866(9) 0.8376(3) 0.4256(3) 0.0493(19) Uani 1 1 d . . . H3 H 0.8305 0.8562 0.4475 0.059 Uiso 1 1 calc R . . C4 C 1.0334(9) 0.8207(3) 0.4461(3) 0.0465(19) Uani 1 1 d . . . C5 C 1.1083(8) 0.7911(3) 0.4151(3) 0.0421(17) Uani 1 1 d . . . H5 H 1.2040 0.7765 0.4279 0.051 Uiso 1 1 calc R . . C6 C 1.0454(8) 0.7819(3) 0.3644(2) 0.0388(17) Uani 1 1 d . . . C7 C 0.6543(9) 0.8457(3) 0.3591(3) 0.054(2) Uani 1 1 d D . . C8 C 0.5700(12) 0.8048(5) 0.3235(4) 0.113(2) Uani 1 1 d D . . H8A H 0.5774 0.7700 0.3400 0.170 Uiso 1 1 calc R . . H8B H 0.6146 0.8031 0.2922 0.170 Uiso 1 1 calc R . . H8C H 0.4638 0.8151 0.3155 0.170 Uiso 1 1 calc R . . C9 C 0.6443(12) 0.8991(4) 0.3324(5) 0.113(2) Uani 1 1 d D . . H9A H 0.5397 0.9115 0.3275 0.170 Uiso 1 1 calc R . . H9B H 0.6786 0.8954 0.2994 0.170 Uiso 1 1 calc R . . H9C H 0.7083 0.9248 0.3531 0.170 Uiso 1 1 calc R . . C10 C 0.5684(12) 0.8517(5) 0.4036(4) 0.113(2) Uani 1 1 d D . . H10A H 0.6058 0.8829 0.4236 0.170 Uiso 1 1 calc R . . H10B H 0.5832 0.8199 0.4250 0.170 Uiso 1 1 calc R . . H10C H 0.4609 0.8562 0.3911 0.170 Uiso 1 1 calc R . . C11 C 1.1032(11) 0.8369(3) 0.5007(3) 0.061(2) Uani 1 1 d . . . C12 C 1.1289(13) 0.8965(4) 0.5018(4) 0.093(3) Uani 1 1 d . . . H12A H 1.1662 0.9078 0.5366 0.139 Uiso 1 1 calc R . . H12B H 1.0338 0.9147 0.4897 0.139 Uiso 1 1 calc R . . H12C H 1.2034 0.9055 0.4798 0.139 Uiso 1 1 calc R . . C13 C 0.9935(12) 0.8227(4) 0.5383(3) 0.083(3) Uani 1 1 d . . . H13A H 0.9826 0.7841 0.5399 0.125 Uiso 1 1 calc R . . H13B H 0.8949 0.8388 0.5268 0.125 Uiso 1 1 calc R . . H13C H 1.0335 0.8364 0.5721 0.125 Uiso 1 1 calc R . . C14 C 1.2513(12) 0.8079(5) 0.5176(4) 0.100(4) Uani 1 1 d . . . H14A H 1.3227 0.8163 0.4943 0.150 Uiso 1 1 calc R . . H14B H 1.2331 0.7696 0.5174 0.150 Uiso 1 1 calc R . . H14C H 1.2933 0.8192 0.5520 0.150 Uiso 1 1 calc R . . C15 C 0.9285(8) 0.6624(3) 0.3249(2) 0.0377(17) Uani 1 1 d . . . C16 C 1.0765(7) 0.6766(3) 0.3457(2) 0.0317(15) Uani 1 1 d . . . C17 C 1.1695(8) 0.6442(3) 0.3785(2) 0.0394(17) Uani 1 1 d . . . H17 H 1.2688 0.6555 0.3914 0.047 Uiso 1 1 calc R . . C18 C 1.1193(7) 0.5959(3) 0.3926(3) 0.0400(17) Uani 1 1 d . . . C19 C 0.9705(8) 0.5828(3) 0.3730(3) 0.0449(18) Uani 1 1 d . . . H19 H 0.9337 0.5498 0.3833 0.054 Uiso 1 1 calc R . . C20 C 0.8716(8) 0.6134(3) 0.3399(2) 0.0381(16) Uani 1 1 d . . . C21 C 0.7093(8) 0.5952(3) 0.3203(3) 0.0460(18) Uani 1 1 d . . . C22 C 0.6949(10) 0.5849(4) 0.2627(3) 0.071(3) Uani 1 1 d . . . H22A H 0.7141 0.6179 0.2453 0.106 Uiso 1 1 calc R . . H22B H 0.5929 0.5723 0.2500 0.106 Uiso 1 1 calc R . . H22C H 0.7684 0.5580 0.2562 0.106 Uiso 1 1 calc R . . C23 C 0.5947(8) 0.6368(3) 0.3314(4) 0.064(2) Uani 1 1 d . . . H23A H 0.6085 0.6441 0.3679 0.096 Uiso 1 1 calc R . . H23B H 0.4925 0.6235 0.3205 0.096 Uiso 1 1 calc R . . H23C H 0.6098 0.6696 0.3130 0.096 Uiso 1 1 calc R . . C24 C 0.6707(10) 0.5426(3) 0.3443(4) 0.072(3) Uani 1 1 d . . . H24A H 0.7389 0.5148 0.3358 0.107 Uiso 1 1 calc R . . H24B H 0.5664 0.5328 0.3314 0.107 Uiso 1 1 calc R . . H24C H 0.6822 0.5467 0.3812 0.107 Uiso 1 1 calc R . . C25 C 1.2136(8) 0.5567(3) 0.4271(3) 0.056(2) Uani 1 1 d D . . C26 C 1.2481(14) 0.5089(4) 0.3966(4) 0.123(3) Uani 1 1 d D . . H26A H 1.3214 0.4862 0.4174 0.184 Uiso 1 1 calc R . . H26B H 1.2899 0.5206 0.3665 0.184 Uiso 1 1 calc R . . H26C H 1.1552 0.4888 0.3859 0.184 Uiso 1 1 calc R . . C27 C 1.3668(12) 0.5779(5) 0.4486(5) 0.123(3) Uani 1 1 d D . . H27A H 1.3556 0.6064 0.4727 0.184 Uiso 1 1 calc R . . H27B H 1.4167 0.5918 0.4211 0.184 Uiso 1 1 calc R . . H27C H 1.4278 0.5493 0.4660 0.184 Uiso 1 1 calc R . . C28 C 1.1388(13) 0.5371(5) 0.4703(4) 0.123(3) Uani 1 1 d D . . H28A H 1.2067 0.5127 0.4913 0.184 Uiso 1 1 calc R . . H28B H 1.0455 0.5184 0.4569 0.184 Uiso 1 1 calc R . . H28C H 1.1153 0.5673 0.4909 0.184 Uiso 1 1 calc R . . C29 C 0.9461(7) 0.6598(3) 0.1869(2) 0.0345(16) Uani 1 1 d . . . C30 C 0.7969(8) 0.6725(3) 0.1657(2) 0.0374(16) Uani 1 1 d . . . C31 C 0.7063(8) 0.6388(3) 0.1330(2) 0.0426(18) Uani 1 1 d . . . H31 H 0.6064 0.6490 0.1196 0.051 Uiso 1 1 calc R . . C32 C 0.7619(8) 0.5901(3) 0.1199(3) 0.0415(17) Uani 1 1 d . A . C33 C 0.9085(7) 0.5779(3) 0.1409(3) 0.0397(17) Uani 1 1 d . . . H33 H 0.9473 0.5446 0.1322 0.048 Uiso 1 1 calc R . . C34 C 1.0038(8) 0.6102(3) 0.1737(2) 0.0398(17) Uani 1 1 d . . . C35 C 1.1652(8) 0.5927(3) 0.1949(3) 0.0436(18) Uani 1 1 d . . . C36 C 1.2791(9) 0.6348(3) 0.1817(3) 0.064(2) Uani 1 1 d . . . H36A H 1.2642 0.6406 0.1450 0.095 Uiso 1 1 calc R . . H36B H 1.3820 0.6222 0.1929 0.095 Uiso 1 1 calc R . . H36C H 1.2630 0.6682 0.1989 0.095 Uiso 1 1 calc R . . C37 C 1.1800(10) 0.5856(4) 0.2520(3) 0.071(3) Uani 1 1 d . . . H37A H 1.1727 0.6202 0.2681 0.106 Uiso 1 1 calc R . . H37B H 1.2778 0.5694 0.2646 0.106 Uiso 1 1 calc R . . H37C H 1.0990 0.5624 0.2600 0.106 Uiso 1 1 calc R . . C38 C 1.2073(9) 0.5397(3) 0.1721(3) 0.066(2) Uani 1 1 d . . . H38A H 1.1394 0.5118 0.1807 0.100 Uiso 1 1 calc R . . H38B H 1.3114 0.5305 0.1860 0.100 Uiso 1 1 calc R . . H38C H 1.1980 0.5431 0.1352 0.100 Uiso 1 1 calc R . . C39 C 0.6653(8) 0.5510(3) 0.0846(3) 0.050(2) Uani 1 1 d D . . C40 C 0.5107(16) 0.5737(7) 0.0635(7) 0.086(5) Uani 0.616(8) 1 d PDU A 1 H40A H 0.4528 0.5470 0.0420 0.129 Uiso 0.616(8) 1 calc PR A 1 H40B H 0.5235 0.6054 0.0433 0.129 Uiso 0.616(8) 1 calc PR A 1 H40C H 0.4567 0.5831 0.0915 0.129 Uiso 0.616(8) 1 calc PR A 1 C41 C 0.647(2) 0.5003(5) 0.1145(6) 0.088(5) Uani 0.616(8) 1 d PDU A 1 H41A H 0.5840 0.4750 0.0928 0.132 Uiso 0.616(8) 1 calc PR A 1 H41B H 0.5984 0.5087 0.1441 0.132 Uiso 0.616(8) 1 calc PR A 1 H41C H 0.7459 0.4845 0.1257 0.132 Uiso 0.616(8) 1 calc PR A 1 C42 C 0.7477(18) 0.5381(7) 0.0397(6) 0.080(4) Uani 0.616(8) 1 d PDU A 1 H42A H 0.8484 0.5243 0.0523 0.120 Uiso 0.616(8) 1 calc PR A 1 H42B H 0.7568 0.5704 0.0199 0.120 Uiso 0.616(8) 1 calc PR A 1 H42C H 0.6906 0.5114 0.0181 0.120 Uiso 0.616(8) 1 calc PR A 1 C40B C 0.521(3) 0.5385(11) 0.1052(11) 0.090(6) Uani 0.384(8) 1 d PDU A 2 H40D H 0.4578 0.5154 0.0814 0.135 Uiso 0.384(8) 1 calc PR A 2 H40E H 0.4671 0.5716 0.1097 0.135 Uiso 0.384(8) 1 calc PR A 2 H40F H 0.5454 0.5205 0.1380 0.135 Uiso 0.384(8) 1 calc PR A 2 C41B C 0.613(3) 0.5780(10) 0.0343(8) 0.090(6) Uani 0.384(8) 1 d PDU A 2 H41D H 0.7001 0.5839 0.0166 0.134 Uiso 0.384(8) 1 calc PR A 2 H41E H 0.5666 0.6121 0.0402 0.134 Uiso 0.384(8) 1 calc PR A 2 H41F H 0.5397 0.5553 0.0135 0.134 Uiso 0.384(8) 1 calc PR A 2 C42B C 0.745(3) 0.5010(9) 0.0727(12) 0.087(6) Uani 0.384(8) 1 d PDU A 2 H42D H 0.7386 0.4745 0.0992 0.130 Uiso 0.384(8) 1 calc PR A 2 H42E H 0.8516 0.5089 0.0713 0.130 Uiso 0.384(8) 1 calc PR A 2 H42F H 0.6982 0.4870 0.0399 0.130 Uiso 0.384(8) 1 calc PR A 2 C43 C 0.9606(9) 0.8003(3) 0.1635(2) 0.0399(17) Uani 1 1 d . . . C44 C 0.8238(7) 0.7773(3) 0.1431(2) 0.0363(16) Uani 1 1 d . . . C45 C 0.7641(8) 0.7830(3) 0.0926(2) 0.0399(17) Uani 1 1 d . . . H45 H 0.6694 0.7676 0.0800 0.048 Uiso 1 1 calc R . . C46 C 0.8421(9) 0.8114(3) 0.0603(3) 0.0458(18) Uani 1 1 d . . . C47 C 0.9845(10) 0.8292(3) 0.0810(3) 0.055(2) Uani 1 1 d . . . H47 H 1.0413 0.8471 0.0588 0.066 Uiso 1 1 calc R . . C48 C 1.0514(8) 0.8233(3) 0.1311(3) 0.0454(18) Uani 1 1 d . A . C49 C 1.2165(10) 0.8410(3) 0.1480(3) 0.061(2) Uani 1 1 d D . . C50 C 1.2227(19) 0.8895(6) 0.1832(7) 0.088(3) Uani 0.616(8) 1 d PD A 2 H50A H 1.1509 0.9163 0.1680 0.132 Uiso 0.616(8) 1 calc PR A 2 H50B H 1.3247 0.9044 0.1881 0.132 Uiso 0.616(8) 1 calc PR A 2 H50C H 1.1965 0.8786 0.2161 0.132 Uiso 0.616(8) 1 calc PR A 2 C51 C 1.2999(19) 0.8564(8) 0.1040(6) 0.088(3) Uani 0.616(8) 1 d PD A 2 H51A H 1.2891 0.8280 0.0787 0.132 Uiso 0.616(8) 1 calc PR A 2 H51B H 1.4069 0.8619 0.1168 0.132 Uiso 0.616(8) 1 calc PR A 2 H51C H 1.2569 0.8893 0.0885 0.132 Uiso 0.616(8) 1 calc PR A 2 C52 C 1.3021(19) 0.7956(6) 0.1777(7) 0.088(3) Uani 0.616(8) 1 d PD A 2 H52A H 1.2552 0.7876 0.2077 0.132 Uiso 0.616(8) 1 calc PR A 2 H52B H 1.4072 0.8061 0.1883 0.132 Uiso 0.616(8) 1 calc PR A 2 H52C H 1.2986 0.7640 0.1561 0.132 Uiso 0.616(8) 1 calc PR A 2 C50B C 1.308(3) 0.8210(12) 0.1075(10) 0.088(3) Uani 0.384(8) 1 d PD A 1 H50D H 1.4092 0.8368 0.1135 0.132 Uiso 0.384(8) 1 calc PR A 1 H50E H 1.2575 0.8314 0.0739 0.132 Uiso 0.384(8) 1 calc PR A 1 H50F H 1.3165 0.7823 0.1094 0.132 Uiso 0.384(8) 1 calc PR A 1 C51B C 1.293(3) 0.8171(12) 0.1983(9) 0.088(3) Uani 0.384(8) 1 d PD A 1 H51D H 1.2709 0.7790 0.1989 0.132 Uiso 0.384(8) 1 calc PR A 1 H51E H 1.2547 0.8346 0.2266 0.132 Uiso 0.384(8) 1 calc PR A 1 H51F H 1.4022 0.8223 0.2015 0.132 Uiso 0.384(8) 1 calc PR A 1 C52B C 1.221(3) 0.9017(8) 0.1511(12) 0.088(3) Uani 0.384(8) 1 d PD A 1 H52D H 1.1311 0.9147 0.1637 0.132 Uiso 0.384(8) 1 calc PR A 1 H52E H 1.2252 0.9164 0.1173 0.132 Uiso 0.384(8) 1 calc PR A 1 H52F H 1.3113 0.9128 0.1742 0.132 Uiso 0.384(8) 1 calc PR A 1 C53 C 0.7752(10) 0.8249(3) 0.0056(3) 0.054(2) Uani 1 1 d . . . C54 C 0.7452(11) 0.8849(4) 0.0021(3) 0.076(3) Uani 1 1 d . . . H54A H 0.7097 0.8946 -0.0332 0.114 Uiso 1 1 calc R . . H54B H 0.8386 0.9041 0.0142 0.114 Uiso 1 1 calc R . . H54C H 0.6683 0.8942 0.0230 0.114 Uiso 1 1 calc R . . C55 C 0.8860(12) 0.8112(4) -0.0312(3) 0.083(3) Uani 1 1 d . . . H55A H 0.9052 0.7729 -0.0303 0.125 Uiso 1 1 calc R . . H55B H 0.9809 0.8303 -0.0211 0.125 Uiso 1 1 calc R . . H55C H 0.8425 0.8217 -0.0656 0.125 Uiso 1 1 calc R . . C56 C 0.6279(12) 0.7947(4) -0.0115(3) 0.091(3) Uani 1 1 d . . . H56A H 0.5534 0.8044 0.0103 0.136 Uiso 1 1 calc R . . H56B H 0.6470 0.7564 -0.0089 0.136 Uiso 1 1 calc R . . H56C H 0.5893 0.8039 -0.0467 0.136 Uiso 1 1 calc R . . C57 C 0.7692(13) 0.8940(4) 0.2067(3) 0.087(3) Uani 1 1 d . . . H57A H 0.6786 0.8718 0.2021 0.130 Uiso 1 1 calc R . . H57B H 0.8024 0.8999 0.1738 0.130 Uiso 1 1 calc R . . H57C H 0.7466 0.9281 0.2214 0.130 Uiso 1 1 calc R . . C58 C 1.0817(13) 0.8994(4) 0.2960(4) 0.090(3) Uani 1 1 d . . . H58A H 1.0465 0.9064 0.3284 0.135 Uiso 1 1 calc R . . H58B H 1.0985 0.9331 0.2795 0.135 Uiso 1 1 calc R . . H58C H 1.1762 0.8793 0.3020 0.135 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0466(12) 0.0336(11) 0.0290(10) -0.0010(9) 0.0035(9) -0.0010(10) Al2 0.0787(17) 0.0363(12) 0.0393(12) -0.0001(10) 0.0079(11) -0.0033(12) S1 0.0400(10) 0.0393(10) 0.0331(9) -0.0016(8) 0.0047(8) -0.0093(8) S2 0.0419(10) 0.0360(10) 0.0323(9) -0.0001(7) 0.0051(8) 0.0028(8) O1 0.055(3) 0.033(3) 0.029(3) -0.003(2) 0.001(2) -0.001(2) O2 0.045(3) 0.041(3) 0.036(3) 0.005(2) 0.000(2) -0.005(2) O3 0.037(3) 0.040(3) 0.036(3) -0.003(2) -0.003(2) -0.007(2) O4 0.057(3) 0.036(3) 0.032(3) -0.001(2) 0.006(2) -0.003(2) C1 0.056(5) 0.031(4) 0.039(4) 0.006(3) 0.000(4) -0.014(3) C2 0.070(5) 0.033(4) 0.034(4) -0.006(3) 0.017(4) 0.003(4) C3 0.070(6) 0.044(4) 0.037(4) -0.006(3) 0.021(4) 0.000(4) C4 0.067(5) 0.033(4) 0.042(4) -0.003(3) 0.016(4) -0.012(4) C5 0.049(4) 0.034(4) 0.044(4) -0.003(3) 0.009(4) -0.003(3) C6 0.054(5) 0.033(4) 0.030(4) -0.003(3) 0.010(3) -0.022(3) C7 0.046(5) 0.058(5) 0.058(5) -0.012(4) 0.004(4) 0.010(4) C8 0.074(4) 0.140(7) 0.126(6) 0.007(5) 0.019(4) 0.034(4) C9 0.074(4) 0.140(7) 0.126(6) 0.007(5) 0.019(4) 0.034(4) C10 0.074(4) 0.140(7) 0.126(6) 0.007(5) 0.019(4) 0.034(4) C11 0.083(6) 0.062(5) 0.038(4) -0.009(4) 0.005(4) -0.011(5) C12 0.126(9) 0.078(7) 0.070(7) -0.023(5) 0.001(6) -0.037(7) C13 0.120(9) 0.092(7) 0.040(5) -0.014(5) 0.018(5) -0.034(6) C14 0.104(9) 0.120(9) 0.064(7) -0.026(6) -0.027(6) 0.016(7) C15 0.050(4) 0.031(4) 0.035(4) -0.006(3) 0.016(3) -0.004(3) C16 0.032(4) 0.037(4) 0.026(3) -0.003(3) 0.004(3) -0.005(3) C17 0.038(4) 0.044(4) 0.035(4) -0.002(3) 0.002(3) -0.009(3) C18 0.029(4) 0.054(5) 0.038(4) 0.005(3) 0.009(3) 0.001(3) C19 0.061(5) 0.030(4) 0.045(4) 0.002(3) 0.014(4) 0.001(3) C20 0.038(4) 0.043(4) 0.036(4) -0.004(3) 0.016(3) -0.001(3) C21 0.047(4) 0.047(4) 0.044(4) 0.001(3) 0.006(3) -0.008(4) C22 0.063(6) 0.090(7) 0.061(6) -0.008(5) 0.012(5) -0.032(5) C23 0.032(4) 0.063(5) 0.095(7) -0.006(5) 0.006(4) -0.006(4) C24 0.059(6) 0.066(6) 0.087(7) 0.009(5) 0.003(5) -0.021(5) C25 0.049(5) 0.054(5) 0.067(5) 0.014(4) 0.013(4) 0.008(4) C26 0.109(6) 0.135(7) 0.121(6) 0.064(5) 0.006(5) 0.029(5) C27 0.109(6) 0.135(7) 0.121(6) 0.064(5) 0.006(5) 0.029(5) C28 0.109(6) 0.135(7) 0.121(6) 0.064(5) 0.006(5) 0.029(5) C29 0.036(4) 0.045(4) 0.021(3) 0.001(3) -0.002(3) -0.005(3) C30 0.043(4) 0.044(4) 0.028(4) 0.001(3) 0.012(3) -0.007(3) C31 0.038(4) 0.055(5) 0.035(4) 0.006(3) 0.004(3) -0.006(4) C32 0.056(5) 0.033(4) 0.036(4) -0.009(3) 0.007(3) 0.003(3) C33 0.036(4) 0.038(4) 0.044(4) -0.003(3) 0.003(3) 0.006(3) C34 0.054(5) 0.032(4) 0.032(4) 0.000(3) 0.001(3) 0.003(3) C35 0.035(4) 0.058(5) 0.037(4) 0.002(3) 0.001(3) 0.006(3) C36 0.049(5) 0.068(6) 0.076(6) -0.005(5) 0.014(4) 0.012(4) C37 0.062(6) 0.095(7) 0.047(5) 0.009(5) -0.015(4) 0.031(5) C38 0.055(5) 0.060(5) 0.082(6) -0.020(5) 0.004(5) 0.021(4) C39 0.046(5) 0.049(5) 0.051(5) -0.016(4) -0.008(4) -0.003(4) C40 0.078(10) 0.080(10) 0.091(11) -0.040(9) -0.015(9) -0.004(8) C41 0.098(11) 0.052(8) 0.104(11) 0.009(8) -0.016(9) -0.040(8) C42 0.088(10) 0.077(10) 0.077(10) -0.046(8) 0.018(8) -0.021(8) C40B 0.090(13) 0.077(12) 0.098(13) -0.030(11) 0.000(12) -0.043(11) C41B 0.091(13) 0.088(12) 0.084(13) -0.035(11) -0.005(11) -0.030(11) C42B 0.094(13) 0.064(12) 0.095(14) -0.040(11) -0.011(12) -0.020(11) C43 0.067(5) 0.029(4) 0.023(4) 0.000(3) 0.006(3) 0.003(3) C44 0.039(4) 0.033(4) 0.034(4) -0.005(3) -0.004(3) 0.006(3) C45 0.044(4) 0.036(4) 0.037(4) -0.001(3) -0.005(3) 0.002(3) C46 0.064(5) 0.037(4) 0.035(4) 0.003(3) 0.003(4) 0.009(4) C47 0.080(6) 0.051(5) 0.037(4) 0.005(4) 0.014(4) 0.001(4) C48 0.053(5) 0.042(4) 0.043(4) 0.000(3) 0.013(4) -0.011(4) C49 0.077(6) 0.055(5) 0.052(5) 0.001(4) 0.016(4) -0.016(5) C50 0.069(5) 0.100(7) 0.096(7) 0.011(6) 0.019(5) -0.034(5) C51 0.069(5) 0.100(7) 0.096(7) 0.011(6) 0.019(5) -0.034(5) C52 0.069(5) 0.100(7) 0.096(7) 0.011(6) 0.019(5) -0.034(5) C50B 0.069(5) 0.100(7) 0.096(7) 0.011(6) 0.019(5) -0.034(5) C51B 0.069(5) 0.100(7) 0.096(7) 0.011(6) 0.019(5) -0.034(5) C52B 0.069(5) 0.100(7) 0.096(7) 0.011(6) 0.019(5) -0.034(5) C53 0.089(6) 0.039(4) 0.032(4) 0.003(3) 0.009(4) 0.002(4) C54 0.092(7) 0.066(6) 0.064(6) 0.004(5) -0.004(5) 0.013(5) C55 0.127(9) 0.087(7) 0.038(5) 0.012(5) 0.023(5) 0.039(6) C56 0.122(9) 0.105(8) 0.036(5) 0.007(5) -0.019(5) -0.026(7) C57 0.133(9) 0.067(6) 0.059(6) 0.012(5) 0.011(6) 0.030(6) C58 0.128(9) 0.061(6) 0.081(7) -0.014(5) 0.018(6) -0.049(6) _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 1.804(5) . ? Al1 O2 1.804(5) . ? Al1 O4 1.952(5) . ? Al1 O1 1.957(5) . ? Al1 S1 2.461(3) . ? Al1 S2 2.472(3) . ? Al1 Al2 2.949(3) . ? Al2 O1 1.868(5) . ? Al2 O4 1.874(5) . ? Al2 C58 1.956(9) . ? Al2 C57 1.961(9) . ? S1 C6 1.788(7) . ? S1 C16 1.797(6) . ? S2 C44 1.799(7) . ? S2 C30 1.799(7) . ? O1 C1 1.402(8) . ? O2 C15 1.349(8) . ? O3 C29 1.346(7) . ? O4 C43 1.398(7) . ? C1 C6 1.390(10) . ? C1 C2 1.403(10) . ? C2 C3 1.395(10) . ? C2 C7 1.526(11) . ? C3 C4 1.415(11) . ? C3 H3 0.9500 . ? C4 C5 1.364(10) . ? C4 C11 1.552(10) . ? C5 C6 1.404(9) . ? C5 H5 0.9500 . ? C7 C9 1.518(9) . ? C7 C10 1.518(9) . ? C7 C8 1.523(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.520(12) . ? C11 C14 1.525(13) . ? C11 C13 1.549(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C16 1.407(9) . ? C15 C20 1.416(9) . ? C16 C17 1.383(9) . ? C17 C18 1.368(9) . ? C17 H17 0.9500 . ? C18 C19 1.399(10) . ? C18 C25 1.518(10) . ? C19 C20 1.389(10) . ? C19 H19 0.9500 . ? C20 C21 1.542(10) . ? C21 C23 1.529(10) . ? C21 C24 1.535(10) . ? C21 C22 1.545(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C28 1.503(9) . ? C25 C27 1.506(9) . ? C25 C26 1.512(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.410(9) . ? C29 C34 1.417(9) . ? C30 C31 1.392(9) . ? C31 C32 1.388(10) . ? C31 H31 0.9500 . ? C32 C33 1.385(9) . ? C32 C39 1.536(9) . ? C33 C34 1.391(9) . ? C33 H33 0.9500 . ? C34 C35 1.539(9) . ? C35 C37 1.520(10) . ? C35 C38 1.537(10) . ? C35 C36 1.550(11) . ? 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 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C42B 1.510(16) . ? C39 C40B 1.513(17) . ? C39 C41B 1.515(17) . ? C39 C40 1.528(11) . ? C39 C41 1.529(10) . ? C39 C42 1.536(10) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43 C44 1.393(10) . ? C43 C48 1.400(10) . ? C44 C45 1.381(9) . ? C45 C46 1.387(10) . ? C45 H45 0.9500 . ? C46 C47 1.388(11) . ? C46 C53 1.532(10) . ? C47 C48 1.389(10) . ? C47 H47 0.9500 . ? C48 C49 1.549(11) . ? C49 C52 1.531(12) . ? C49 C52B 1.533(18) . ? C49 C51 1.534(12) . ? C49 C51B 1.536(18) . ? C49 C50B 1.537(18) . ? C49 C50 1.538(12) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? C51B H51D 0.9800 . ? C51B H51E 0.9800 . ? C51B H51F 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53 C56 1.534(12) . ? C53 C54 1.536(11) . ? C53 C55 1.538(11) . ? 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 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 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 O3 Al1 O2 99.1(2) . . ? O3 Al1 O4 92.4(2) . . ? O2 Al1 O4 167.0(2) . . ? O3 Al1 O1 167.6(2) . . ? O2 Al1 O1 92.1(2) . . ? O4 Al1 O1 77.1(2) . . ? O3 Al1 S1 92.87(17) . . ? O2 Al1 S1 84.96(17) . . ? O4 Al1 S1 100.56(17) . . ? O1 Al1 S1 82.79(15) . . ? O3 Al1 S2 84.33(16) . . ? O2 Al1 S2 92.61(17) . . ? O4 Al1 S2 82.48(16) . . ? O1 Al1 S2 100.53(16) . . ? S1 Al1 S2 175.98(11) . . ? O3 Al1 Al2 130.77(18) . . ? O2 Al1 Al2 130.16(18) . . ? O4 Al1 Al2 38.63(14) . . ? O1 Al1 Al2 38.49(14) . . ? S1 Al1 Al2 92.48(9) . . ? S2 Al1 Al2 91.54(9) . . ? O1 Al2 O4 81.3(2) . . ? O1 Al2 C58 107.3(3) . . ? O4 Al2 C58 117.7(4) . . ? O1 Al2 C57 116.7(4) . . ? O4 Al2 C57 107.1(3) . . ? C58 Al2 C57 120.5(5) . . ? O1 Al2 Al1 40.69(15) . . ? O4 Al2 Al1 40.57(15) . . ? C58 Al2 Al1 120.6(3) . . ? C57 Al2 Al1 118.9(3) . . ? C6 S1 C16 98.8(3) . . ? C6 S1 Al1 93.0(2) . . ? C16 S1 Al1 89.5(2) . . ? C44 S2 C30 98.5(3) . . ? C44 S2 Al1 93.1(2) . . ? C30 S2 Al1 89.7(2) . . ? C1 O1 Al2 118.9(4) . . ? C1 O1 Al1 119.0(4) . . ? Al2 O1 Al1 100.8(2) . . ? C15 O2 Al1 119.5(4) . . ? C29 O3 Al1 120.9(4) . . ? C43 O4 Al2 119.2(4) . . ? C43 O4 Al1 118.7(4) . . ? Al2 O4 Al1 100.8(2) . . ? C6 C1 O1 116.3(6) . . ? C6 C1 C2 120.4(6) . . ? O1 C1 C2 123.3(7) . . ? C3 C2 C1 115.2(7) . . ? C3 C2 C7 120.5(6) . . ? C1 C2 C7 124.3(6) . . ? C2 C3 C4 125.2(7) . . ? C2 C3 H3 117.4 . . ? C4 C3 H3 117.4 . . ? C5 C4 C3 116.5(7) . . ? C5 C4 C11 123.2(8) . . ? C3 C4 C11 120.3(7) . . ? C4 C5 C6 120.7(7) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 120.7(7) . . ? C1 C6 S1 120.3(5) . . ? C5 C6 S1 119.0(6) . . ? C9 C7 C10 106.2(8) . . ? C9 C7 C8 108.6(8) . . ? C10 C7 C8 107.0(8) . . ? C9 C7 C2 111.4(7) . . ? C10 C7 C2 112.1(7) . . ? C8 C7 C2 111.4(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 110.2(9) . . ? C12 C11 C13 109.0(8) . . ? C14 C11 C13 108.0(8) . . ? C12 C11 C4 108.4(7) . . ? C14 C11 C4 111.3(7) . . ? C13 C11 C4 109.9(7) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 120.2(6) . . ? O2 C15 C20 121.7(6) . . ? C16 C15 C20 118.0(6) . . ? C17 C16 C15 123.0(6) . . ? C17 C16 S1 120.5(5) . . ? C15 C16 S1 116.5(5) . . ? C18 C17 C16 120.4(6) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 116.3(6) . . ? C17 C18 C25 124.6(6) . . ? C19 C18 C25 119.2(6) . . ? C20 C19 C18 126.2(7) . . ? C20 C19 H19 116.9 . . ? C18 C19 H19 116.9 . . ? C19 C20 C15 116.1(6) . . ? C19 C20 C21 122.2(6) . . ? C15 C20 C21 121.8(6) . . ? C23 C21 C24 108.1(7) . . ? C23 C21 C20 111.0(6) . . ? C24 C21 C20 112.1(6) . . ? C23 C21 C22 110.5(7) . . ? C24 C21 C22 106.3(7) . . ? C20 C21 C22 108.7(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 108.1(9) . . ? C28 C25 C26 107.5(9) . . ? C27 C25 C26 103.9(9) . . ? C28 C25 C18 114.0(7) . . ? C27 C25 C18 113.3(7) . . ? C26 C25 C18 109.5(7) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 119.8(6) . . ? O3 C29 C34 122.7(6) . . ? C30 C29 C34 117.5(6) . . ? C31 C30 C29 122.9(6) . . ? C31 C30 S2 120.7(5) . . ? C29 C30 S2 116.4(5) . . ? C32 C31 C30 120.0(7) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 116.7(6) . . ? C33 C32 C39 121.4(6) . . ? C31 C32 C39 121.9(6) . . ? C32 C33 C34 125.6(6) . . ? C32 C33 H33 117.2 . . ? C34 C33 H33 117.2 . . ? C33 C34 C29 117.3(6) . . ? C33 C34 C35 121.3(6) . . ? C29 C34 C35 121.4(6) . . ? C37 C35 C38 107.6(7) . . ? C37 C35 C34 109.8(6) . . ? C38 C35 C34 112.2(6) . . ? C37 C35 C36 110.3(7) . . ? C38 C35 C36 107.2(6) . . ? C34 C35 C36 109.7(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C42B C39 C40B 111.3(17) . . ? C42B C39 C41B 106.3(17) . . ? C40B C39 C41B 104.4(17) . . ? C42B C39 C40 132.0(12) . . ? C40B C39 C40 55.5(13) . . ? C41B C39 C40 50.4(12) . . ? C42B C39 C41 60.2(14) . . ? C40B C39 C41 58.0(13) . . ? C41B C39 C41 142.5(12) . . ? C40 C39 C41 109.9(11) . . ? C42B C39 C42 50.0(13) . . ? C40B C39 C42 141.1(12) . . ? C41B C39 C42 61.5(13) . . ? C40 C39 C42 107.9(11) . . ? C41 C39 C42 109.4(11) . . ? C42B C39 C32 114.9(10) . . ? C40B C39 C32 110.3(10) . . ? C41B C39 C32 109.1(10) . . ? C40 C39 C32 112.7(7) . . ? C41 C39 C32 108.2(7) . . ? C42 C39 C32 108.7(7) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? C39 C40B H40D 109.5 . . ? C39 C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39 C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C39 C41B H41D 109.5 . . ? C39 C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C39 C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C39 C42B H42D 109.5 . . ? C39 C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C39 C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C44 C43 O4 117.0(6) . . ? C44 C43 C48 119.5(6) . . ? O4 C43 C48 123.4(6) . . ? C45 C44 C43 121.9(6) . . ? C45 C44 S2 119.1(5) . . ? C43 C44 S2 118.9(5) . . ? C44 C45 C46 120.1(7) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 116.1(6) . . ? C45 C46 C53 122.9(7) . . ? C47 C46 C53 120.9(7) . . ? C46 C47 C48 126.0(7) . . ? C46 C47 H47 117.0 . . ? C48 C47 H47 117.0 . . ? C47 C48 C43 115.5(7) . . ? C47 C48 C49 120.5(7) . . ? C43 C48 C49 124.0(6) . . ? C52 C49 C52B 135.2(15) . . ? C52 C49 C51 108.7(11) . . ? C52B C49 C51 76.9(13) . . ? C52 C49 C51B 29.6(13) . . ? C52B C49 C51B 109.8(17) . . ? C51 C49 C51B 124.2(15) . . ? C52 C49 C50B 80.8(14) . . ? C52B C49 C50B 110.5(16) . . ? C51 C49 C50B 34.0(11) . . ? C51B C49 C50B 105.6(17) . . ? C52 C49 C50 108.0(11) . . ? C52B C49 C50 34.5(11) . . ? C51 C49 C50 106.8(10) . . ? C51B C49 C50 78.9(14) . . ? C50B C49 C50 135.6(13) . . ? C52 C49 C48 108.7(8) . . ? C52B C49 C48 108.7(12) . . ? C51 C49 C48 113.9(9) . . ? C51B C49 C48 115.2(12) . . ? C50B C49 C48 106.9(12) . . ? C50 C49 C48 110.6(9) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C50B H50D 109.5 . . ? C49 C50B H50E 109.5 . . ? C49 C50B H50F 109.5 . . ? C49 C51B H51D 109.5 . . ? C49 C51B H51E 109.5 . . ? C49 C51B H51F 109.5 . . ? C49 C52B H52D 109.5 . . ? C49 C52B H52E 109.5 . . ? C49 C52B H52F 109.5 . . ? C46 C53 C56 111.8(7) . . ? C46 C53 C54 108.5(6) . . ? C56 C53 C54 109.6(8) . . ? C46 C53 C55 111.1(7) . . ? C56 C53 C55 108.1(7) . . ? C54 C53 C55 107.8(7) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Al2 C57 H57A 109.5 . . ? Al2 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? Al2 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Al2 C58 H58A 109.5 . . ? Al2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? Al2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Al1 Al2 O1 -171.1(3) . . . . ? O2 Al1 Al2 O1 10.3(3) . . . . ? O4 Al1 Al2 O1 -179.0(3) . . . . ? S1 Al1 Al2 O1 -75.1(2) . . . . ? S2 Al1 Al2 O1 105.1(2) . . . . ? O3 Al1 Al2 O4 7.9(3) . . . . ? O2 Al1 Al2 O4 -170.6(3) . . . . ? O1 Al1 Al2 O4 179.0(3) . . . . ? S1 Al1 Al2 O4 103.9(2) . . . . ? S2 Al1 Al2 O4 -75.9(2) . . . . ? O3 Al1 Al2 C58 -90.2(4) . . . . ? O2 Al1 Al2 C58 91.3(4) . . . . ? O4 Al1 Al2 C58 -98.1(4) . . . . ? O1 Al1 Al2 C58 80.9(4) . . . . ? S1 Al1 Al2 C58 5.8(4) . . . . ? S2 Al1 Al2 C58 -174.0(4) . . . . ? O3 Al1 Al2 C57 90.6(4) . . . . ? O2 Al1 Al2 C57 -88.0(4) . . . . ? O4 Al1 Al2 C57 82.7(4) . . . . ? O1 Al1 Al2 C57 -98.3(4) . . . . ? S1 Al1 Al2 C57 -173.5(4) . . . . ? S2 Al1 Al2 C57 6.8(4) . . . . ? O3 Al1 S1 C6 -175.5(3) . . . . ? O2 Al1 S1 C6 -76.6(3) . . . . ? O4 Al1 S1 C6 91.5(3) . . . . ? O1 Al1 S1 C6 16.1(2) . . . . ? S2 Al1 S1 C6 -129.6(16) . . . . ? Al2 Al1 S1 C6 53.5(2) . . . . ? O3 Al1 S1 C16 -76.7(3) . . . . ? O2 Al1 S1 C16 22.2(3) . . . . ? O4 Al1 S1 C16 -169.7(3) . . . . ? O1 Al1 S1 C16 115.0(3) . . . . ? S2 Al1 S1 C16 -30.8(17) . . . . ? Al2 Al1 S1 C16 152.3(2) . . . . ? O3 Al1 S2 C44 -76.8(3) . . . . ? O2 Al1 S2 C44 -175.6(3) . . . . ? O4 Al1 S2 C44 16.4(3) . . . . ? O1 Al1 S2 C44 91.7(3) . . . . ? S1 Al1 S2 C44 -122.9(16) . . . . ? Al2 Al1 S2 C44 54.1(2) . . . . ? O3 Al1 S2 C30 21.8(3) . . . . ? O2 Al1 S2 C30 -77.1(3) . . . . ? O4 Al1 S2 C30 114.9(3) . . . . ? O1 Al1 S2 C30 -169.7(3) . . . . ? S1 Al1 S2 C30 -24.4(17) . . . . ? Al2 Al1 S2 C30 152.6(2) . . . . ? O4 Al2 O1 C1 131.4(5) . . . . ? C58 Al2 O1 C1 15.0(6) . . . . ? C57 Al2 O1 C1 -123.7(6) . . . . ? Al1 Al2 O1 C1 132.1(6) . . . . ? O4 Al2 O1 Al1 -0.6(2) . . . . ? C58 Al2 O1 Al1 -117.1(4) . . . . ? C57 Al2 O1 Al1 104.2(4) . . . . ? O3 Al1 O1 C1 -98.8(11) . . . . ? O2 Al1 O1 C1 55.9(5) . . . . ? O4 Al1 O1 C1 -131.4(5) . . . . ? S1 Al1 O1 C1 -28.8(4) . . . . ? S2 Al1 O1 C1 148.9(4) . . . . ? Al2 Al1 O1 C1 -132.0(6) . . . . ? O3 Al1 O1 Al2 33.2(11) . . . . ? O2 Al1 O1 Al2 -172.1(2) . . . . ? O4 Al1 O1 Al2 0.6(2) . . . . ? S1 Al1 O1 Al2 103.2(2) . . . . ? S2 Al1 O1 Al2 -79.1(2) . . . . ? O3 Al1 O2 C15 62.4(5) . . . . ? O4 Al1 O2 C15 -145.6(9) . . . . ? O1 Al1 O2 C15 -112.2(5) . . . . ? S1 Al1 O2 C15 -29.7(4) . . . . ? S2 Al1 O2 C15 147.1(4) . . . . ? Al2 Al1 O2 C15 -118.7(4) . . . . ? O2 Al1 O3 C29 62.9(5) . . . . ? O4 Al1 O3 C29 -111.0(5) . . . . ? O1 Al1 O3 C29 -142.7(10) . . . . ? S1 Al1 O3 C29 148.2(4) . . . . ? S2 Al1 O3 C29 -28.9(4) . . . . ? Al2 Al1 O3 C29 -116.0(4) . . . . ? O1 Al2 O4 C43 132.5(5) . . . . ? C58 Al2 O4 C43 -122.5(6) . . . . ? C57 Al2 O4 C43 17.1(6) . . . . ? Al1 Al2 O4 C43 131.8(6) . . . . ? O1 Al2 O4 Al1 0.6(2) . . . . ? C58 Al2 O4 Al1 105.7(4) . . . . ? C57 Al2 O4 Al1 -114.7(4) . . . . ? O3 Al1 O4 C43 53.8(5) . . . . ? O2 Al1 O4 C43 -98.5(11) . . . . ? O1 Al1 O4 C43 -132.8(5) . . . . ? S1 Al1 O4 C43 147.2(4) . . . . ? S2 Al1 O4 C43 -30.1(5) . . . . ? Al2 Al1 O4 C43 -132.2(6) . . . . ? O3 Al1 O4 Al2 -174.0(2) . . . . ? O2 Al1 O4 Al2 33.7(11) . . . . ? O1 Al1 O4 Al2 -0.6(2) . . . . ? S1 Al1 O4 Al2 -80.6(2) . . . . ? S2 Al1 O4 Al2 102.0(2) . . . . ? Al2 O1 C1 C6 -90.5(6) . . . . ? Al1 O1 C1 C6 33.0(7) . . . . ? Al2 O1 C1 C2 88.2(7) . . . . ? Al1 O1 C1 C2 -148.3(5) . . . . ? C6 C1 C2 C3 11.7(10) . . . . ? O1 C1 C2 C3 -166.9(6) . . . . ? C6 C1 C2 C7 -167.6(6) . . . . ? O1 C1 C2 C7 13.8(11) . . . . ? C1 C2 C3 C4 -3.9(11) . . . . ? C7 C2 C3 C4 175.4(7) . . . . ? C2 C3 C4 C5 -4.2(11) . . . . ? C2 C3 C4 C11 174.4(7) . . . . ? C3 C4 C5 C6 4.7(10) . . . . ? C11 C4 C5 C6 -173.8(7) . . . . ? O1 C1 C6 C5 167.1(6) . . . . ? C2 C1 C6 C5 -11.6(10) . . . . ? O1 C1 C6 S1 -13.8(8) . . . . ? C2 C1 C6 S1 167.5(5) . . . . ? C4 C5 C6 C1 2.8(10) . . . . ? C4 C5 C6 S1 -176.3(5) . . . . ? C16 S1 C6 C1 -95.9(6) . . . . ? Al1 S1 C6 C1 -5.9(5) . . . . ? C16 S1 C6 C5 83.3(6) . . . . ? Al1 S1 C6 C5 173.2(5) . . . . ? C3 C2 C7 C9 98.1(9) . . . . ? C1 C2 C7 C9 -82.6(9) . . . . ? C3 C2 C7 C10 -20.7(11) . . . . ? C1 C2 C7 C10 158.6(8) . . . . ? C3 C2 C7 C8 -140.4(8) . . . . ? C1 C2 C7 C8 38.8(11) . . . . ? C5 C4 C11 C12 111.6(9) . . . . ? C3 C4 C11 C12 -66.9(10) . . . . ? C5 C4 C11 C14 -9.8(11) . . . . ? C3 C4 C11 C14 171.7(8) . . . . ? C5 C4 C11 C13 -129.4(8) . . . . ? C3 C4 C11 C13 52.1(10) . . . . ? Al1 O2 C15 C16 26.6(8) . . . . ? Al1 O2 C15 C20 -154.5(5) . . . . ? O2 C15 C16 C17 -179.0(6) . . . . ? C20 C15 C16 C17 2.1(10) . . . . ? O2 C15 C16 S1 -0.1(8) . . . . ? C20 C15 C16 S1 -179.1(5) . . . . ? C6 S1 C16 C17 -104.6(6) . . . . ? Al1 S1 C16 C17 162.4(5) . . . . ? C6 S1 C16 C15 76.5(5) . . . . ? Al1 S1 C16 C15 -16.5(5) . . . . ? C15 C16 C17 C18 -0.3(10) . . . . ? S1 C16 C17 C18 -179.1(5) . . . . ? C16 C17 C18 C19 -1.5(10) . . . . ? C16 C17 C18 C25 178.0(6) . . . . ? C17 C18 C19 C20 1.7(11) . . . . ? C25 C18 C19 C20 -177.9(7) . . . . ? C18 C19 C20 C15 0.0(10) . . . . ? C18 C19 C20 C21 179.9(7) . . . . ? O2 C15 C20 C19 179.2(6) . . . . ? C16 C15 C20 C19 -1.9(9) . . . . ? O2 C15 C20 C21 -0.6(9) . . . . ? C16 C15 C20 C21 178.3(6) . . . . ? C19 C20 C21 C23 124.8(7) . . . . ? C15 C20 C21 C23 -55.4(9) . . . . ? C19 C20 C21 C24 3.8(10) . . . . ? C15 C20 C21 C24 -176.4(7) . . . . ? C19 C20 C21 C22 -113.4(8) . . . . ? C15 C20 C21 C22 66.4(9) . . . . ? C17 C18 C25 C28 129.3(9) . . . . ? C19 C18 C25 C28 -51.2(11) . . . . ? C17 C18 C25 C27 5.1(11) . . . . ? C19 C18 C25 C27 -175.4(8) . . . . ? C17 C18 C25 C26 -110.3(9) . . . . ? C19 C18 C25 C26 69.2(9) . . . . ? Al1 O3 C29 C30 25.2(8) . . . . ? Al1 O3 C29 C34 -153.9(5) . . . . ? O3 C29 C30 C31 -179.2(6) . . . . ? C34 C29 C30 C31 -0.1(10) . . . . ? O3 C29 C30 S2 1.3(8) . . . . ? C34 C29 C30 S2 -179.6(5) . . . . ? C44 S2 C30 C31 -103.3(6) . . . . ? Al1 S2 C30 C31 163.6(5) . . . . ? C44 S2 C30 C29 76.3(5) . . . . ? Al1 S2 C30 C29 -16.8(5) . . . . ? C29 C30 C31 C32 0.1(10) . . . . ? S2 C30 C31 C32 179.6(5) . . . . ? C30 C31 C32 C33 0.0(10) . . . . ? C30 C31 C32 C39 178.9(6) . . . . ? C31 C32 C33 C34 -0.2(11) . . . . ? C39 C32 C33 C34 -179.1(7) . . . . ? C32 C33 C34 C29 0.2(11) . . . . ? C32 C33 C34 C35 180.0(7) . . . . ? O3 C29 C34 C33 179.0(6) . . . . ? C30 C29 C34 C33 -0.1(9) . . . . ? O3 C29 C34 C35 -0.7(10) . . . . ? C30 C29 C34 C35 -179.8(6) . . . . ? C33 C34 C35 C37 -114.8(8) . . . . ? C29 C34 C35 C37 64.9(9) . . . . ? C33 C34 C35 C38 4.9(10) . . . . ? C29 C34 C35 C38 -175.4(7) . . . . ? C33 C34 C35 C36 123.8(7) . . . . ? C29 C34 C35 C36 -56.5(8) . . . . ? C33 C32 C39 C42B -3.5(17) . . . . ? C31 C32 C39 C42B 177.7(16) . . . . ? C33 C32 C39 C40B 123.2(15) . . . . ? C31 C32 C39 C40B -55.6(16) . . . . ? C33 C32 C39 C41B -122.7(15) . . . . ? C31 C32 C39 C41B 58.5(16) . . . . ? C33 C32 C39 C40 -176.8(11) . . . . ? C31 C32 C39 C40 4.3(13) . . . . ? C33 C32 C39 C41 61.4(12) . . . . ? C31 C32 C39 C41 -117.4(11) . . . . ? C33 C32 C39 C42 -57.3(11) . . . . ? C31 C32 C39 C42 123.9(10) . . . . ? Al2 O4 C43 C44 -87.6(6) . . . . ? Al1 O4 C43 C44 35.8(8) . . . . ? Al2 O4 C43 C48 89.1(7) . . . . ? Al1 O4 C43 C48 -147.5(6) . . . . ? O4 C43 C44 C45 167.4(6) . . . . ? C48 C43 C44 C45 -9.4(10) . . . . ? O4 C43 C44 S2 -16.1(8) . . . . ? C48 C43 C44 S2 167.1(5) . . . . ? C30 S2 C44 C45 81.4(6) . . . . ? Al1 S2 C44 C45 171.7(5) . . . . ? C30 S2 C44 C43 -95.2(6) . . . . ? Al1 S2 C44 C43 -5.0(5) . . . . ? C43 C44 C45 C46 1.4(10) . . . . ? S2 C44 C45 C46 -175.1(5) . . . . ? C44 C45 C46 C47 4.7(10) . . . . ? C44 C45 C46 C53 -172.7(6) . . . . ? C45 C46 C47 C48 -3.2(12) . . . . ? C53 C46 C47 C48 174.3(7) . . . . ? C46 C47 C48 C43 -4.3(12) . . . . ? C46 C47 C48 C49 174.8(7) . . . . ? C44 C43 C48 C47 10.4(10) . . . . ? O4 C43 C48 C47 -166.2(6) . . . . ? C44 C43 C48 C49 -168.7(7) . . . . ? O4 C43 C48 C49 14.7(11) . . . . ? C47 C48 C49 C52 -130.1(10) . . . . ? C43 C48 C49 C52 48.9(12) . . . . ? C47 C48 C49 C52B 74.9(15) . . . . ? C43 C48 C49 C52B -106.1(14) . . . . ? C47 C48 C49 C51 -8.7(13) . . . . ? C43 C48 C49 C51 170.3(11) . . . . ? C47 C48 C49 C51B -161.4(15) . . . . ? C43 C48 C49 C51B 17.7(17) . . . . ? C47 C48 C49 C50B -44.4(15) . . . . ? C43 C48 C49 C50B 134.7(14) . . . . ? C47 C48 C49 C50 111.5(10) . . . . ? C43 C48 C49 C50 -69.4(11) . . . . ? C45 C46 C53 C56 -10.9(11) . . . . ? C47 C46 C53 C56 171.8(8) . . . . ? C45 C46 C53 C54 110.1(8) . . . . ? C47 C46 C53 C54 -67.3(10) . . . . ? C45 C46 C53 C55 -131.6(8) . . . . ? C47 C46 C53 C55 51.0(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.438 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.061 #===END data_complex_9 _database_code_depnum_ccdc_archive 'CCDC 752752' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H98 Al2 O4 S2' _chemical_formula_weight 1049.50 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0701(7) _cell_length_b 16.2602(12) _cell_length_c 21.6729(16) _cell_angle_alpha 91.4670(10) _cell_angle_beta 101.7900(10) _cell_angle_gamma 90.2190(10) _cell_volume 3127.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9575 _exptl_absorpt_correction_T_max 0.9739 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22555 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10917 _reflns_number_gt 10376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10917 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.1780 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.71848(13) 0.75025(7) 0.25403(5) 0.0143(2) Uani 1 1 d . . . Al2 Al 0.75165(13) 0.61125(7) 0.33874(5) 0.0158(2) Uani 1 1 d . . . O1 O 0.6356(3) 0.63909(15) 0.26023(12) 0.0151(5) Uani 1 1 d . . . O2 O 0.5821(3) 0.76905(16) 0.18331(12) 0.0152(5) Uani 1 1 d . . . O3 O 0.8272(3) 0.84409(16) 0.25663(12) 0.0162(6) Uani 1 1 d . . . O4 O 0.8370(3) 0.71462(15) 0.33210(12) 0.0152(5) Uani 1 1 d . . . S1 S 0.86098(10) 0.68012(6) 0.18526(4) 0.0145(2) Uani 1 1 d . . . S2 S 0.58687(10) 0.82822(6) 0.32588(4) 0.0142(2) Uani 1 1 d . . . C1 C 0.6258(4) 0.5864(2) 0.20809(17) 0.0147(8) Uani 1 1 d . . . C2 C 0.5089(5) 0.5281(2) 0.18888(18) 0.0194(8) Uani 1 1 d . . . C3 C 0.5295(5) 0.4711(2) 0.14229(19) 0.0217(9) Uani 1 1 d . . . H3 H 0.4550 0.4293 0.1304 0.026 Uiso 1 1 calc R . . C4 C 0.6507(5) 0.4704(2) 0.11162(18) 0.0204(8) Uani 1 1 d . . . C5 C 0.7546(4) 0.5343(2) 0.12667(18) 0.0173(8) Uani 1 1 d . . . H5 H 0.8353 0.5390 0.1051 0.021 Uiso 1 1 calc R . . C6 C 0.7394(4) 0.5914(2) 0.17372(18) 0.0153(8) Uani 1 1 d . . . C7 C 0.3621(5) 0.5283(3) 0.21466(19) 0.0243(9) Uani 1 1 d . . . C8 C 0.2976(6) 0.6151(3) 0.2113(3) 0.0540(16) Uani 1 1 d . . . H8A H 0.2023 0.6151 0.2260 0.081 Uiso 1 1 calc R . . H8B H 0.2799 0.6333 0.1677 0.081 Uiso 1 1 calc R . . H8C H 0.3693 0.6528 0.2382 0.081 Uiso 1 1 calc R . . C9 C 0.3917(6) 0.4976(4) 0.2819(2) 0.0547(17) Uani 1 1 d . . . H9A H 0.2967 0.4952 0.2967 0.082 Uiso 1 1 calc R . . H9B H 0.4619 0.5353 0.3095 0.082 Uiso 1 1 calc R . . H9C H 0.4356 0.4425 0.2828 0.082 Uiso 1 1 calc R . . C10 C 0.2413(5) 0.4725(3) 0.1745(2) 0.0388(12) Uani 1 1 d . . . H10A H 0.2730 0.4151 0.1790 0.058 Uiso 1 1 calc R . . H10B H 0.2276 0.4874 0.1302 0.058 Uiso 1 1 calc R . . H10C H 0.1461 0.4794 0.1887 0.058 Uiso 1 1 calc R . . C11 C 0.6681(5) 0.4006(3) 0.0645(2) 0.0259(9) Uani 1 1 d . . . C12 C 0.7173(6) 0.3235(3) 0.1026(2) 0.0339(11) Uani 1 1 d . . . H12A H 0.8141 0.3343 0.1314 0.051 Uiso 1 1 calc R . . H12B H 0.7280 0.2775 0.0737 0.051 Uiso 1 1 calc R . . H12C H 0.6413 0.3093 0.1269 0.051 Uiso 1 1 calc R . . C13 C 0.5193(6) 0.3827(3) 0.0180(2) 0.0337(11) Uani 1 1 d . . . H13A H 0.4414 0.3683 0.0413 0.051 Uiso 1 1 calc R . . H13B H 0.5329 0.3367 -0.0104 0.051 Uiso 1 1 calc R . . H13C H 0.4886 0.4316 -0.0067 0.051 Uiso 1 1 calc R . . C14 C 0.7868(6) 0.4223(3) 0.0262(2) 0.0357(11) Uani 1 1 d . . . H14A H 0.7592 0.4738 0.0043 0.054 Uiso 1 1 calc R . . H14B H 0.7916 0.3780 -0.0048 0.054 Uiso 1 1 calc R . . H14C H 0.8853 0.4290 0.0546 0.054 Uiso 1 1 calc R . . C15 C 0.6302(4) 0.7773(2) 0.12897(17) 0.0140(7) Uani 1 1 d . . . C16 C 0.7631(4) 0.7386(2) 0.12089(17) 0.0143(8) Uani 1 1 d . . . C17 C 0.8214(4) 0.7448(2) 0.06698(17) 0.0159(8) Uani 1 1 d . . . H17 H 0.9121 0.7174 0.0639 0.019 Uiso 1 1 calc R . . C18 C 0.7469(4) 0.7909(2) 0.01766(17) 0.0166(8) Uani 1 1 d . . . C19 C 0.6135(4) 0.8283(2) 0.02536(18) 0.0178(8) Uani 1 1 d . . . H19 H 0.5614 0.8600 -0.0084 0.021 Uiso 1 1 calc R . . C20 C 0.5510(4) 0.8229(2) 0.07851(17) 0.0164(8) Uani 1 1 d . . . C21 C 0.4019(4) 0.8663(2) 0.08273(18) 0.0185(8) Uani 1 1 d . . . C22 C 0.4314(5) 0.9353(3) 0.1329(2) 0.0257(9) Uani 1 1 d . . . H22A H 0.5032 0.9750 0.1222 0.039 Uiso 1 1 calc R . . H22B H 0.4734 0.9121 0.1740 0.039 Uiso 1 1 calc R . . H22C H 0.3367 0.9631 0.1348 0.039 Uiso 1 1 calc R . . C23 C 0.2885(5) 0.8040(3) 0.0989(2) 0.0262(9) Uani 1 1 d . . . H23A H 0.1927 0.8315 0.0992 0.039 Uiso 1 1 calc R . . H23B H 0.3282 0.7818 0.1405 0.039 Uiso 1 1 calc R . . H23C H 0.2723 0.7591 0.0672 0.039 Uiso 1 1 calc R . . C24 C 0.3291(5) 0.9043(3) 0.0199(2) 0.0262(9) Uani 1 1 d . . . H24A H 0.2342 0.9303 0.0239 0.039 Uiso 1 1 calc R . . H24B H 0.3092 0.8611 -0.0132 0.039 Uiso 1 1 calc R . . H24C H 0.3974 0.9456 0.0088 0.039 Uiso 1 1 calc R . . C25 C 0.8111(5) 0.8051(3) -0.04138(18) 0.0214(9) Uani 1 1 d . . . C26 C 0.9272(7) 0.7411(4) -0.0494(3) 0.0583(18) Uani 1 1 d . . . H26A H 1.0091 0.7425 -0.0121 0.087 Uiso 1 1 calc R . . H26B H 0.9679 0.7531 -0.0868 0.087 Uiso 1 1 calc R . . H26C H 0.8798 0.6865 -0.0546 0.087 Uiso 1 1 calc R . . C27 C 0.6897(6) 0.8048(4) -0.1005(2) 0.0489(15) Uani 1 1 d . . . H27A H 0.6317 0.7533 -0.1039 0.073 Uiso 1 1 calc R . . H27B H 0.7361 0.8093 -0.1374 0.073 Uiso 1 1 calc R . . H27C H 0.6225 0.8514 -0.0987 0.073 Uiso 1 1 calc R . . C28 C 0.8900(7) 0.8890(4) -0.0329(2) 0.0521(16) Uani 1 1 d . . . H28A H 0.8168 0.9318 -0.0287 0.078 Uiso 1 1 calc R . . H28B H 0.9340 0.8995 -0.0696 0.078 Uiso 1 1 calc R . . H28C H 0.9699 0.8893 0.0052 0.078 Uiso 1 1 calc R . . C29 C 0.7667(4) 0.9171(2) 0.26520(17) 0.0154(8) Uani 1 1 d . . . C30 C 0.6470(4) 0.9225(2) 0.29692(17) 0.0151(8) Uani 1 1 d . . . C31 C 0.5763(4) 0.9956(2) 0.30745(17) 0.0153(8) Uani 1 1 d . . . H31 H 0.4956 0.9958 0.3293 0.018 Uiso 1 1 calc R . . C32 C 0.6250(4) 1.0683(2) 0.28562(17) 0.0170(8) Uani 1 1 d . . . C33 C 0.7454(4) 1.0636(2) 0.25489(17) 0.0173(8) Uani 1 1 d . . . H33 H 0.7798 1.1132 0.2402 0.021 Uiso 1 1 calc R . . C34 C 0.8191(4) 0.9911(2) 0.24408(17) 0.0167(8) Uani 1 1 d . . . C35 C 0.9522(4) 0.9927(2) 0.20962(18) 0.0194(8) Uani 1 1 d . . . C36 C 0.9086(5) 0.9467(3) 0.14566(19) 0.0257(9) Uani 1 1 d . . . H36A H 0.8217 0.9734 0.1197 0.039 Uiso 1 1 calc R . . H36B H 0.8827 0.8895 0.1523 0.039 Uiso 1 1 calc R . . H36C H 0.9937 0.9479 0.1242 0.039 Uiso 1 1 calc R . . C37 C 0.9984(5) 1.0799(3) 0.19729(19) 0.0234(9) Uani 1 1 d . . . H37A H 1.0872 1.0780 0.1780 0.035 Uiso 1 1 calc R . . H37B H 1.0226 1.1115 0.2372 0.035 Uiso 1 1 calc R . . H37C H 0.9154 1.1062 0.1687 0.035 Uiso 1 1 calc R . . C38 C 1.0911(4) 0.9513(3) 0.2500(2) 0.0246(9) Uani 1 1 d . . . H38A H 1.1746 0.9518 0.2276 0.037 Uiso 1 1 calc R . . H38B H 1.0657 0.8943 0.2577 0.037 Uiso 1 1 calc R . . H38C H 1.1209 0.9815 0.2904 0.037 Uiso 1 1 calc R . . C39 C 0.5492(4) 1.1504(2) 0.29672(18) 0.0192(8) Uani 1 1 d . . . C40 C 0.3777(5) 1.1404(3) 0.2780(2) 0.0246(9) Uani 1 1 d . . . H40A H 0.3496 1.1215 0.2339 0.037 Uiso 1 1 calc R . . H40B H 0.3301 1.1934 0.2833 0.037 Uiso 1 1 calc R . . H40C H 0.3438 1.1000 0.3050 0.037 Uiso 1 1 calc R . . C41 C 0.5960(5) 1.2192(2) 0.2574(2) 0.0257(9) Uani 1 1 d . . . H41A H 0.7044 1.2299 0.2709 0.039 Uiso 1 1 calc R . . H41B H 0.5405 1.2693 0.2635 0.039 Uiso 1 1 calc R . . H41C H 0.5731 1.2023 0.2128 0.039 Uiso 1 1 calc R . . C42 C 0.5937(5) 1.1755(3) 0.3671(2) 0.0270(9) Uani 1 1 d . . . H42A H 0.5678 1.1308 0.3925 0.041 Uiso 1 1 calc R . . H42B H 0.5391 1.2252 0.3751 0.041 Uiso 1 1 calc R . . H42C H 0.7023 1.1864 0.3783 0.041 Uiso 1 1 calc R . . C43 C 0.8628(4) 0.7697(2) 0.38292(17) 0.0156(8) Uani 1 1 d . . . C44 C 0.9999(4) 0.7758(2) 0.42610(18) 0.0166(8) Uani 1 1 d . . . C45 C 0.9960(4) 0.8194(2) 0.48247(18) 0.0174(8) Uani 1 1 d . . . H45 H 1.0856 0.8212 0.5141 0.021 Uiso 1 1 calc R . . C46 C 0.8715(4) 0.8599(2) 0.49546(18) 0.0190(8) Uani 1 1 d . . . C47 C 0.7435(4) 0.8623(2) 0.44710(18) 0.0176(8) Uani 1 1 d . . . H47 H 0.6586 0.8937 0.4524 0.021 Uiso 1 1 calc R . . C48 C 0.7418(4) 0.8184(2) 0.39153(17) 0.0153(8) Uani 1 1 d . . . C49 C 1.1506(4) 0.7397(2) 0.41648(18) 0.0191(8) Uani 1 1 d . . . C50 C 1.1531(5) 0.7177(3) 0.34709(19) 0.0260(9) Uani 1 1 d . . . H50A H 1.2555 0.7025 0.3435 0.039 Uiso 1 1 calc R . . H50B H 1.1211 0.7653 0.3210 0.039 Uiso 1 1 calc R . . H50C H 1.0843 0.6713 0.3326 0.039 Uiso 1 1 calc R . . C51 C 1.1868(5) 0.6635(3) 0.4559(2) 0.0284(10) Uani 1 1 d . . . H51A H 1.1961 0.6786 0.5006 0.043 Uiso 1 1 calc R . . H51B H 1.2819 0.6402 0.4492 0.043 Uiso 1 1 calc R . . H51C H 1.1057 0.6227 0.4433 0.043 Uiso 1 1 calc R . . C52 C 1.2765(5) 0.8044(3) 0.4379(2) 0.0269(10) Uani 1 1 d . . . H52A H 1.2873 0.8165 0.4831 0.040 Uiso 1 1 calc R . . H52B H 1.2507 0.8550 0.4145 0.040 Uiso 1 1 calc R . . H52C H 1.3717 0.7830 0.4296 0.040 Uiso 1 1 calc R . . C53 C 0.8764(5) 0.8995(3) 0.56122(19) 0.0232(9) Uani 1 1 d . . . C54 C 0.8931(5) 0.8294(3) 0.60872(19) 0.0285(10) Uani 1 1 d . . . H54A H 0.8980 0.8526 0.6513 0.043 Uiso 1 1 calc R . . H54B H 0.9857 0.7990 0.6075 0.043 Uiso 1 1 calc R . . H54C H 0.8063 0.7919 0.5975 0.043 Uiso 1 1 calc R . . C55 C 1.0113(5) 0.9579(3) 0.5804(2) 0.0298(10) Uani 1 1 d . . . H55A H 0.9969 1.0060 0.5536 0.045 Uiso 1 1 calc R . . H55B H 1.1033 0.9294 0.5754 0.045 Uiso 1 1 calc R . . H55C H 1.0204 0.9756 0.6246 0.045 Uiso 1 1 calc R . . C56 C 0.7329(5) 0.9473(3) 0.5634(2) 0.0293(10) Uani 1 1 d . . . H56A H 0.7212 0.9910 0.5325 0.044 Uiso 1 1 calc R . . H56B H 0.7395 0.9716 0.6057 0.044 Uiso 1 1 calc R . . H56C H 0.6458 0.9099 0.5533 0.044 Uiso 1 1 calc R . . C57 C 0.8947(4) 0.5248(2) 0.32475(19) 0.0199(8) Uani 1 1 d . . . H57A H 0.9413 0.5423 0.2896 0.024 Uiso 1 1 calc R . . H57B H 0.9760 0.5241 0.3629 0.024 Uiso 1 1 calc R . . C58 C 0.8391(5) 0.4359(2) 0.30987(19) 0.0215(9) Uani 1 1 d . . . H58 H 0.7518 0.4361 0.2732 0.026 Uiso 1 1 calc R . . C59 C 0.9628(5) 0.3820(3) 0.2919(2) 0.0334(11) Uani 1 1 d . . . H59A H 0.9930 0.4041 0.2546 0.050 Uiso 1 1 calc R . . H59B H 0.9245 0.3257 0.2825 0.050 Uiso 1 1 calc R . . H59C H 1.0500 0.3819 0.3271 0.050 Uiso 1 1 calc R . . C60 C 0.7860(5) 0.3990(3) 0.3660(2) 0.0287(10) Uani 1 1 d . . . H60A H 0.8701 0.3987 0.4025 0.043 Uiso 1 1 calc R . . H60B H 0.7500 0.3425 0.3551 0.043 Uiso 1 1 calc R . . H60C H 0.7040 0.4322 0.3764 0.043 Uiso 1 1 calc R . . C61 C 0.6360(4) 0.6190(2) 0.40695(18) 0.0193(8) Uani 1 1 d . . . H61A H 0.5658 0.6656 0.3976 0.023 Uiso 1 1 calc R . . H61B H 0.5737 0.5684 0.4042 0.023 Uiso 1 1 calc R . . C62 C 0.7206(5) 0.6303(3) 0.47595(18) 0.0211(9) Uani 1 1 d . . . H62 H 0.7911 0.6782 0.4785 0.025 Uiso 1 1 calc R . . C63 C 0.6135(5) 0.6481(3) 0.5207(2) 0.0301(10) Uani 1 1 d . . . H63A H 0.5391 0.6035 0.5169 0.045 Uiso 1 1 calc R . . H63B H 0.5616 0.7001 0.5096 0.045 Uiso 1 1 calc R . . H63C H 0.6711 0.6523 0.5641 0.045 Uiso 1 1 calc R . . C64 C 0.8133(5) 0.5547(3) 0.4978(2) 0.0293(10) Uani 1 1 d . . . H64A H 0.8679 0.5640 0.5414 0.044 Uiso 1 1 calc R . . H64B H 0.8854 0.5445 0.4705 0.044 Uiso 1 1 calc R . . H64C H 0.7462 0.5068 0.4957 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0164(6) 0.0144(6) 0.0118(5) 0.0002(4) 0.0025(4) -0.0009(4) Al2 0.0185(6) 0.0152(6) 0.0138(6) 0.0012(4) 0.0036(5) -0.0003(4) O1 0.0179(13) 0.0138(13) 0.0134(13) -0.0002(10) 0.0026(10) -0.0026(10) O2 0.0124(13) 0.0197(14) 0.0139(13) 0.0019(10) 0.0035(10) 0.0017(10) O3 0.0169(13) 0.0166(14) 0.0155(13) -0.0005(10) 0.0045(11) -0.0011(11) O4 0.0178(13) 0.0150(13) 0.0125(13) -0.0012(10) 0.0025(10) -0.0025(10) S1 0.0140(5) 0.0150(5) 0.0138(5) 0.0013(3) 0.0011(4) 0.0005(3) S2 0.0147(5) 0.0146(5) 0.0136(4) 0.0012(3) 0.0038(4) -0.0012(3) C1 0.0167(19) 0.0118(18) 0.0154(19) 0.0004(14) 0.0024(15) 0.0034(14) C2 0.024(2) 0.018(2) 0.0159(19) 0.0021(15) 0.0019(16) -0.0020(16) C3 0.025(2) 0.017(2) 0.020(2) 0.0011(16) -0.0021(17) -0.0076(16) C4 0.025(2) 0.018(2) 0.018(2) 0.0018(16) 0.0021(16) 0.0024(16) C5 0.021(2) 0.0144(19) 0.0170(19) 0.0006(15) 0.0041(16) 0.0035(15) C6 0.0140(18) 0.0108(18) 0.0188(19) -0.0007(14) -0.0015(15) -0.0007(14) C7 0.020(2) 0.032(2) 0.021(2) -0.0006(18) 0.0051(17) -0.0110(18) C8 0.031(3) 0.043(3) 0.094(5) -0.014(3) 0.030(3) -0.005(2) C9 0.030(3) 0.106(5) 0.029(3) 0.018(3) 0.007(2) -0.026(3) C10 0.027(2) 0.053(3) 0.038(3) -0.015(2) 0.011(2) -0.018(2) C11 0.032(2) 0.019(2) 0.027(2) -0.0048(17) 0.0060(19) -0.0027(18) C12 0.042(3) 0.021(2) 0.039(3) -0.004(2) 0.009(2) 0.002(2) C13 0.044(3) 0.027(2) 0.029(2) -0.0133(19) 0.007(2) -0.005(2) C14 0.048(3) 0.026(2) 0.038(3) -0.013(2) 0.019(2) -0.001(2) C15 0.0150(18) 0.0144(18) 0.0123(18) -0.0045(14) 0.0027(14) -0.0037(14) C16 0.0153(18) 0.0149(18) 0.0105(18) 0.0003(14) -0.0020(14) -0.0030(14) C17 0.0172(19) 0.0129(18) 0.0179(19) -0.0031(15) 0.0051(15) -0.0028(15) C18 0.020(2) 0.0164(19) 0.0139(19) -0.0020(15) 0.0045(15) -0.0029(15) C19 0.022(2) 0.0160(19) 0.0133(19) 0.0000(15) -0.0018(15) -0.0004(15) C20 0.0169(19) 0.0156(19) 0.0156(19) -0.0040(15) 0.0008(15) -0.0005(15) C21 0.019(2) 0.017(2) 0.019(2) 0.0017(16) 0.0029(16) 0.0021(16) C22 0.023(2) 0.025(2) 0.027(2) -0.0029(18) 0.0014(18) 0.0071(17) C23 0.015(2) 0.029(2) 0.034(2) 0.0049(19) 0.0039(18) 0.0034(17) C24 0.021(2) 0.027(2) 0.030(2) 0.0084(18) 0.0035(18) 0.0083(17) C25 0.022(2) 0.029(2) 0.0145(19) 0.0034(16) 0.0062(16) 0.0023(17) C26 0.076(4) 0.077(4) 0.033(3) 0.022(3) 0.035(3) 0.040(4) C27 0.034(3) 0.094(5) 0.020(2) 0.008(3) 0.008(2) -0.009(3) C28 0.068(4) 0.066(4) 0.030(3) -0.007(3) 0.027(3) -0.035(3) C29 0.0176(19) 0.018(2) 0.0082(17) -0.0002(14) -0.0016(14) 0.0002(15) C30 0.0158(19) 0.0160(19) 0.0120(18) 0.0029(14) -0.0010(15) -0.0021(15) C31 0.0135(18) 0.020(2) 0.0116(18) -0.0012(15) 0.0011(14) 0.0000(15) C32 0.0182(19) 0.018(2) 0.0129(18) -0.0012(15) -0.0007(15) -0.0030(15) C33 0.018(2) 0.018(2) 0.0147(19) 0.0030(15) 0.0003(15) -0.0038(15) C34 0.0175(19) 0.021(2) 0.0100(18) -0.0014(15) -0.0004(15) -0.0049(15) C35 0.020(2) 0.020(2) 0.018(2) -0.0031(16) 0.0061(16) -0.0027(16) C36 0.030(2) 0.028(2) 0.022(2) -0.0072(18) 0.0110(18) -0.0103(18) C37 0.024(2) 0.027(2) 0.020(2) 0.0009(17) 0.0068(17) -0.0076(17) C38 0.017(2) 0.029(2) 0.031(2) 0.0023(18) 0.0117(18) -0.0037(17) C39 0.023(2) 0.018(2) 0.017(2) -0.0009(15) 0.0028(16) -0.0008(16) C40 0.022(2) 0.023(2) 0.029(2) 0.0059(18) 0.0055(18) 0.0035(17) C41 0.031(2) 0.018(2) 0.028(2) 0.0036(17) 0.0058(19) -0.0004(17) C42 0.031(2) 0.023(2) 0.027(2) -0.0023(18) 0.0076(19) 0.0001(18) C43 0.0180(19) 0.0180(19) 0.0104(18) 0.0028(15) 0.0022(15) -0.0050(15) C44 0.020(2) 0.0147(19) 0.0158(19) 0.0022(15) 0.0045(15) -0.0049(15) C45 0.0164(19) 0.019(2) 0.0146(19) 0.0008(15) -0.0010(15) -0.0025(15) C46 0.022(2) 0.018(2) 0.016(2) 0.0019(15) 0.0037(16) -0.0048(16) C47 0.020(2) 0.0166(19) 0.0179(19) 0.0013(15) 0.0076(16) -0.0003(15) C48 0.0175(19) 0.0154(19) 0.0122(18) 0.0050(14) 0.0008(15) -0.0067(15) C49 0.018(2) 0.019(2) 0.020(2) -0.0004(16) 0.0028(16) -0.0039(16) C50 0.020(2) 0.037(3) 0.022(2) -0.0045(18) 0.0066(17) 0.0020(18) C51 0.024(2) 0.027(2) 0.034(2) 0.0069(19) 0.0052(19) 0.0043(18) C52 0.018(2) 0.029(2) 0.033(2) -0.0014(19) 0.0050(18) -0.0034(17) C53 0.027(2) 0.026(2) 0.016(2) -0.0029(17) 0.0039(17) -0.0050(18) C54 0.038(3) 0.031(2) 0.017(2) 0.0004(18) 0.0069(19) -0.003(2) C55 0.039(3) 0.030(2) 0.020(2) -0.0075(18) 0.0047(19) -0.009(2) C56 0.038(3) 0.033(2) 0.016(2) -0.0065(18) 0.0050(19) 0.003(2) C57 0.022(2) 0.016(2) 0.021(2) 0.0022(16) 0.0044(17) 0.0025(16) C58 0.021(2) 0.021(2) 0.022(2) -0.0006(16) 0.0036(17) 0.0012(16) C59 0.033(3) 0.019(2) 0.050(3) -0.002(2) 0.015(2) 0.0005(19) C60 0.040(3) 0.018(2) 0.030(2) 0.0000(18) 0.011(2) -0.0030(18) C61 0.020(2) 0.020(2) 0.018(2) 0.0015(16) 0.0057(16) -0.0028(16) C62 0.022(2) 0.024(2) 0.019(2) 0.0028(16) 0.0072(17) -0.0038(17) C63 0.029(2) 0.044(3) 0.018(2) 0.0049(19) 0.0065(18) 0.008(2) C64 0.031(2) 0.033(3) 0.024(2) 0.0063(19) 0.0041(19) 0.0058(19) _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 O2 1.796(3) . ? Al1 O3 1.807(3) . ? Al1 O4 1.915(3) . ? Al1 O1 1.973(3) . ? Al1 S1 2.4298(14) . ? Al1 S2 2.4754(14) . ? Al1 Al2 2.9260(16) . ? Al2 O4 1.869(3) . ? Al2 O1 1.876(3) . ? Al2 C57 1.976(4) . ? Al2 C61 1.982(4) . ? O1 C1 1.388(4) . ? O2 C15 1.347(4) . ? O3 C29 1.334(5) . ? O4 C43 1.383(4) . ? S1 C16 1.791(4) . ? S1 C6 1.793(4) . ? S2 C48 1.795(4) . ? S2 C30 1.796(4) . ? C1 C6 1.393(5) . ? C1 C2 1.411(5) . ? C2 C3 1.394(6) . ? C2 C7 1.545(6) . ? C3 C4 1.396(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 C11 1.537(6) . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C7 C9 1.525(6) . ? C7 C8 1.528(7) . ? C7 C10 1.531(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.533(6) . ? C11 C14 1.533(6) . ? C11 C12 1.536(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C16 1.401(5) . ? C15 C20 1.410(5) . ? C16 C17 1.383(5) . ? C17 C18 1.382(5) . ? C17 H17 0.9500 . ? C18 C19 1.395(5) . ? C18 C25 1.533(5) . ? C19 C20 1.388(5) . ? C19 H19 0.9500 . ? C20 C21 1.546(5) . ? C21 C22 1.526(5) . ? C21 C24 1.533(5) . ? C21 C23 1.537(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C27 1.509(6) . ? C25 C26 1.515(6) . ? C25 C28 1.527(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.401(5) . ? C29 C34 1.413(5) . ? C30 C31 1.388(5) . ? C31 C32 1.389(5) . ? C31 H31 0.9500 . ? C32 C33 1.392(5) . ? C32 C39 1.539(5) . ? C33 C34 1.395(6) . ? C33 H33 0.9500 . ? C34 C35 1.544(5) . ? C35 C37 1.522(5) . ? C35 C36 1.536(5) . ? C35 C38 1.547(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.532(5) . ? C39 C40 1.532(6) . ? C39 C42 1.539(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.396(5) . ? C43 C44 1.397(5) . ? C44 C45 1.403(5) . ? C44 C49 1.540(5) . ? C45 C46 1.383(6) . ? C45 H45 0.9500 . ? C46 C47 1.398(5) . ? C46 C53 1.541(5) . ? C47 C48 1.382(5) . ? C47 H47 0.9500 . ? C49 C51 1.522(6) . ? C49 C50 1.542(5) . ? C49 C52 1.542(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C56 1.527(6) . ? C53 C55 1.528(6) . ? C53 C54 1.543(6) . ? 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 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.534(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.532(6) . ? C58 C60 1.532(6) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.541(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C64 1.522(6) . ? C62 C63 1.530(6) . ? C62 H62 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 O2 Al1 O3 97.99(13) . . ? O2 Al1 O4 169.07(13) . . ? O3 Al1 O4 92.50(12) . . ? O2 Al1 O1 91.77(12) . . ? O3 Al1 O1 169.14(13) . . ? O4 Al1 O1 78.05(11) . . ? O2 Al1 S1 85.73(9) . . ? O3 Al1 S1 92.71(9) . . ? O4 Al1 S1 96.86(9) . . ? O1 Al1 S1 83.24(9) . . ? O2 Al1 S2 95.91(9) . . ? O3 Al1 S2 83.78(9) . . ? O4 Al1 S2 82.15(9) . . ? O1 Al1 S2 100.01(9) . . ? S1 Al1 S2 176.29(6) . . ? O2 Al1 Al2 130.79(10) . . ? O3 Al1 Al2 131.22(10) . . ? O4 Al1 Al2 38.79(8) . . ? O1 Al1 Al2 39.30(8) . . ? S1 Al1 Al2 91.48(5) . . ? S2 Al1 Al2 89.96(5) . . ? O4 Al2 O1 81.66(11) . . ? O4 Al2 C57 109.36(15) . . ? O1 Al2 C57 108.34(15) . . ? O4 Al2 C61 107.84(15) . . ? O1 Al2 C61 112.29(15) . . ? C57 Al2 C61 127.71(17) . . ? O4 Al2 Al1 39.92(8) . . ? O1 Al2 Al1 41.78(8) . . ? C57 Al2 Al1 116.77(13) . . ? C61 Al2 Al1 115.40(13) . . ? C1 O1 Al2 120.6(2) . . ? C1 O1 Al1 116.9(2) . . ? Al2 O1 Al1 98.92(12) . . ? C15 O2 Al1 118.6(2) . . ? C29 O3 Al1 121.0(2) . . ? C43 O4 Al2 120.5(2) . . ? C43 O4 Al1 118.1(2) . . ? Al2 O4 Al1 101.29(12) . . ? C16 S1 C6 98.05(17) . . ? C16 S1 Al1 89.10(13) . . ? C6 S1 Al1 93.45(13) . . ? C48 S2 C30 97.43(17) . . ? C48 S2 Al1 92.43(13) . . ? C30 S2 Al1 89.39(13) . . ? O1 C1 C6 117.6(3) . . ? O1 C1 C2 123.6(3) . . ? C6 C1 C2 118.8(3) . . ? C3 C2 C1 115.9(4) . . ? C3 C2 C7 120.9(4) . . ? C1 C2 C7 123.1(3) . . ? C2 C3 C4 125.4(4) . . ? C2 C3 H3 117.3 . . ? C4 C3 H3 117.3 . . ? C5 C4 C3 116.9(4) . . ? C5 C4 C11 122.3(4) . . ? C3 C4 C11 120.8(4) . . ? C4 C5 C6 119.3(4) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C1 122.8(3) . . ? C5 C6 S1 118.1(3) . . ? C1 C6 S1 118.8(3) . . ? C9 C7 C8 111.3(5) . . ? C9 C7 C10 107.8(4) . . ? C8 C7 C10 106.5(4) . . ? C9 C7 C2 110.5(4) . . ? C8 C7 C2 109.3(4) . . ? C10 C7 C2 111.4(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 107.8(4) . . ? C13 C11 C12 109.4(4) . . ? C14 C11 C12 109.4(4) . . ? C13 C11 C4 111.3(4) . . ? C14 C11 C4 111.3(3) . . ? C12 C11 C4 107.6(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 119.8(3) . . ? O2 C15 C20 122.6(3) . . ? C16 C15 C20 117.6(3) . . ? C17 C16 C15 123.5(3) . . ? C17 C16 S1 119.6(3) . . ? C15 C16 S1 116.9(3) . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 116.9(3) . . ? C17 C18 C25 122.2(3) . . ? C19 C18 C25 120.8(3) . . ? C20 C19 C18 125.1(4) . . ? C20 C19 H19 117.5 . . ? C18 C19 H19 117.5 . . ? C19 C20 C15 117.3(3) . . ? C19 C20 C21 121.5(3) . . ? C15 C20 C21 121.2(3) . . ? C22 C21 C24 107.9(3) . . ? C22 C21 C23 109.9(3) . . ? C24 C21 C23 107.3(3) . . ? C22 C21 C20 110.0(3) . . ? C24 C21 C20 111.5(3) . . ? C23 C21 C20 110.2(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 108.7(4) . . ? C27 C25 C28 109.1(4) . . ? C26 C25 C28 107.7(5) . . ? C27 C25 C18 112.1(3) . . ? C26 C25 C18 111.7(3) . . ? C28 C25 C18 107.4(3) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 119.8(3) . . ? O3 C29 C34 122.8(3) . . ? C30 C29 C34 117.3(3) . . ? C31 C30 C29 123.8(3) . . ? C31 C30 S2 119.6(3) . . ? C29 C30 S2 116.5(3) . . ? C30 C31 C32 119.2(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C33 117.3(4) . . ? C31 C32 C39 120.5(3) . . ? C33 C32 C39 122.3(3) . . ? C32 C33 C34 124.7(4) . . ? C32 C33 H33 117.6 . . ? C34 C33 H33 117.6 . . ? C33 C34 C29 117.6(3) . . ? C33 C34 C35 120.5(3) . . ? C29 C34 C35 121.8(3) . . ? C37 C35 C36 107.7(3) . . ? C37 C35 C34 112.3(3) . . ? C36 C35 C34 110.0(3) . . ? C37 C35 C38 107.5(3) . . ? C36 C35 C38 109.3(3) . . ? C34 C35 C38 109.9(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C40 107.8(3) . . ? C41 C39 C32 111.9(3) . . ? C40 C39 C32 109.7(3) . . ? C41 C39 C42 109.1(3) . . ? C40 C39 C42 109.3(3) . . ? C32 C39 C42 109.0(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 C43 C48 116.9(3) . . ? O4 C43 C44 123.2(3) . . ? C48 C43 C44 119.9(3) . . ? C43 C44 C45 115.5(4) . . ? C43 C44 C49 125.7(3) . . ? C45 C44 C49 118.9(3) . . ? C46 C45 C44 124.9(4) . . ? C46 C45 H45 117.5 . . ? C44 C45 H45 117.5 . . ? C45 C46 C47 117.3(4) . . ? C45 C46 C53 120.3(4) . . ? C47 C46 C53 122.4(4) . . ? C48 C47 C46 119.2(4) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C43 121.9(3) . . ? C47 C48 S2 120.2(3) . . ? C43 C48 S2 117.9(3) . . ? C51 C49 C44 109.6(3) . . ? C51 C49 C50 109.3(3) . . ? C44 C49 C50 113.7(3) . . ? C51 C49 C52 109.1(3) . . ? C44 C49 C52 109.1(3) . . ? C50 C49 C52 105.9(3) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C56 C53 C55 108.6(4) . . ? C56 C53 C46 111.5(3) . . ? C55 C53 C46 111.2(3) . . ? C56 C53 C54 109.6(4) . . ? C55 C53 C54 108.4(4) . . ? C46 C53 C54 107.4(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 Al2 119.9(3) . . ? C58 C57 H57A 107.3 . . ? Al2 C57 H57A 107.3 . . ? C58 C57 H57B 107.3 . . ? Al2 C57 H57B 107.3 . . ? H57A C57 H57B 106.9 . . ? C59 C58 C60 109.5(4) . . ? C59 C58 C57 111.0(3) . . ? C60 C58 C57 111.1(3) . . ? C59 C58 H58 108.4 . . ? C60 C58 H58 108.4 . . ? C57 C58 H58 108.4 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 Al2 119.6(3) . . ? C62 C61 H61A 107.4 . . ? Al2 C61 H61A 107.4 . . ? C62 C61 H61B 107.4 . . ? Al2 C61 H61B 107.4 . . ? H61A C61 H61B 107.0 . . ? C64 C62 C63 109.2(3) . . ? C64 C62 C61 111.1(3) . . ? C63 C62 C61 112.1(3) . . ? C64 C62 H62 108.1 . . ? C63 C62 H62 108.1 . . ? C61 C62 H62 108.1 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 Al2 O4 -175.23(18) . . . . ? O3 Al1 Al2 O4 4.22(17) . . . . ? O1 Al1 Al2 O4 176.57(18) . . . . ? S1 Al1 Al2 O4 99.13(13) . . . . ? S2 Al1 Al2 O4 -77.45(13) . . . . ? O2 Al1 Al2 O1 8.20(17) . . . . ? O3 Al1 Al2 O1 -172.35(18) . . . . ? O4 Al1 Al2 O1 -176.57(18) . . . . ? S1 Al1 Al2 O1 -77.44(13) . . . . ? S2 Al1 Al2 O1 105.98(13) . . . . ? O2 Al1 Al2 C57 96.16(19) . . . . ? O3 Al1 Al2 C57 -84.38(19) . . . . ? O4 Al1 Al2 C57 -88.60(19) . . . . ? O1 Al1 Al2 C57 87.96(19) . . . . ? S1 Al1 Al2 C57 10.53(15) . . . . ? S2 Al1 Al2 C57 -166.06(14) . . . . ? O2 Al1 Al2 C61 -87.46(18) . . . . ? O3 Al1 Al2 C61 91.99(18) . . . . ? O4 Al1 Al2 C61 87.77(18) . . . . ? O1 Al1 Al2 C61 -95.66(18) . . . . ? S1 Al1 Al2 C61 -173.10(14) . . . . ? S2 Al1 Al2 C61 10.32(14) . . . . ? O4 Al2 O1 C1 126.4(3) . . . . ? C57 Al2 O1 C1 18.7(3) . . . . ? C61 Al2 O1 C1 -127.6(3) . . . . ? Al1 Al2 O1 C1 128.7(3) . . . . ? O4 Al2 O1 Al1 -2.23(12) . . . . ? C57 Al2 O1 Al1 -109.94(16) . . . . ? C61 Al2 O1 Al1 103.71(16) . . . . ? O2 Al1 O1 C1 55.1(2) . . . . ? O3 Al1 O1 C1 -99.0(7) . . . . ? O4 Al1 O1 C1 -128.9(2) . . . . ? S1 Al1 O1 C1 -30.4(2) . . . . ? S2 Al1 O1 C1 151.4(2) . . . . ? Al2 Al1 O1 C1 -131.1(3) . . . . ? O2 Al1 O1 Al2 -173.80(13) . . . . ? O3 Al1 O1 Al2 32.1(7) . . . . ? O4 Al1 O1 Al2 2.20(12) . . . . ? S1 Al1 O1 Al2 100.71(10) . . . . ? S2 Al1 O1 Al2 -77.48(11) . . . . ? O3 Al1 O2 C15 61.6(3) . . . . ? O4 Al1 O2 C15 -134.7(6) . . . . ? O1 Al1 O2 C15 -113.6(3) . . . . ? S1 Al1 O2 C15 -30.5(2) . . . . ? S2 Al1 O2 C15 146.2(2) . . . . ? Al2 Al1 O2 C15 -118.8(2) . . . . ? O2 Al1 O3 C29 65.2(3) . . . . ? O4 Al1 O3 C29 -111.8(3) . . . . ? O1 Al1 O3 C29 -141.0(6) . . . . ? S1 Al1 O3 C29 151.2(2) . . . . ? S2 Al1 O3 C29 -30.0(2) . . . . ? Al2 Al1 O3 C29 -114.4(2) . . . . ? O1 Al2 O4 C43 134.8(3) . . . . ? C57 Al2 O4 C43 -118.6(3) . . . . ? C61 Al2 O4 C43 24.0(3) . . . . ? Al1 Al2 O4 C43 132.5(3) . . . . ? O1 Al2 O4 Al1 2.31(12) . . . . ? C57 Al2 O4 Al1 108.91(16) . . . . ? C61 Al2 O4 Al1 -108.51(16) . . . . ? O2 Al1 O4 C43 -114.5(7) . . . . ? O3 Al1 O4 C43 49.3(3) . . . . ? O1 Al1 O4 C43 -136.1(3) . . . . ? S1 Al1 O4 C43 142.3(2) . . . . ? S2 Al1 O4 C43 -34.1(2) . . . . ? Al2 Al1 O4 C43 -133.9(3) . . . . ? O2 Al1 O4 Al2 19.4(7) . . . . ? O3 Al1 O4 Al2 -176.82(13) . . . . ? O1 Al1 O4 Al2 -2.22(12) . . . . ? S1 Al1 O4 Al2 -83.79(11) . . . . ? S2 Al1 O4 Al2 99.82(11) . . . . ? O2 Al1 S1 C16 22.90(15) . . . . ? O3 Al1 S1 C16 -74.92(15) . . . . ? O4 Al1 S1 C16 -167.77(14) . . . . ? O1 Al1 S1 C16 115.20(14) . . . . ? S2 Al1 S1 C16 -93.5(9) . . . . ? Al2 Al1 S1 C16 153.70(12) . . . . ? O2 Al1 S1 C6 -75.11(15) . . . . ? O3 Al1 S1 C6 -172.93(15) . . . . ? O4 Al1 S1 C6 94.22(15) . . . . ? O1 Al1 S1 C6 17.18(14) . . . . ? S2 Al1 S1 C6 168.5(9) . . . . ? Al2 Al1 S1 C6 55.68(12) . . . . ? O2 Al1 S2 C48 -172.29(15) . . . . ? O3 Al1 S2 C48 -74.86(14) . . . . ? O4 Al1 S2 C48 18.55(14) . . . . ? O1 Al1 S2 C48 94.86(14) . . . . ? S1 Al1 S2 C48 -56.2(9) . . . . ? Al2 Al1 S2 C48 56.66(12) . . . . ? O2 Al1 S2 C30 -74.88(15) . . . . ? O3 Al1 S2 C30 22.55(15) . . . . ? O4 Al1 S2 C30 115.95(14) . . . . ? O1 Al1 S2 C30 -167.73(14) . . . . ? S1 Al1 S2 C30 41.2(9) . . . . ? Al2 Al1 S2 C30 154.07(12) . . . . ? Al2 O1 C1 C6 -84.6(4) . . . . ? Al1 O1 C1 C6 35.6(4) . . . . ? Al2 O1 C1 C2 94.6(4) . . . . ? Al1 O1 C1 C2 -145.3(3) . . . . ? O1 C1 C2 C3 -169.6(3) . . . . ? C6 C1 C2 C3 9.6(5) . . . . ? O1 C1 C2 C7 13.4(6) . . . . ? C6 C1 C2 C7 -167.5(4) . . . . ? C1 C2 C3 C4 -3.6(6) . . . . ? C7 C2 C3 C4 173.6(4) . . . . ? C2 C3 C4 C5 -3.5(6) . . . . ? C2 C3 C4 C11 175.3(4) . . . . ? C3 C4 C5 C6 4.5(5) . . . . ? C11 C4 C5 C6 -174.3(4) . . . . ? C4 C5 C6 C1 1.7(6) . . . . ? C4 C5 C6 S1 -172.4(3) . . . . ? O1 C1 C6 C5 170.1(3) . . . . ? C2 C1 C6 C5 -9.1(6) . . . . ? O1 C1 C6 S1 -15.8(4) . . . . ? C2 C1 C6 S1 165.0(3) . . . . ? C16 S1 C6 C5 78.8(3) . . . . ? Al1 S1 C6 C5 168.4(3) . . . . ? C16 S1 C6 C1 -95.5(3) . . . . ? Al1 S1 C6 C1 -6.0(3) . . . . ? C3 C2 C7 C9 108.9(5) . . . . ? C1 C2 C7 C9 -74.2(5) . . . . ? C3 C2 C7 C8 -128.3(4) . . . . ? C1 C2 C7 C8 48.6(5) . . . . ? C3 C2 C7 C10 -10.9(6) . . . . ? C1 C2 C7 C10 166.0(4) . . . . ? C5 C4 C11 C13 -134.3(4) . . . . ? C3 C4 C11 C13 46.9(5) . . . . ? C5 C4 C11 C14 -14.0(6) . . . . ? C3 C4 C11 C14 167.2(4) . . . . ? C5 C4 C11 C12 105.8(4) . . . . ? C3 C4 C11 C12 -72.9(5) . . . . ? Al1 O2 C15 C16 27.1(4) . . . . ? Al1 O2 C15 C20 -153.7(3) . . . . ? O2 C15 C16 C17 -179.1(3) . . . . ? C20 C15 C16 C17 1.6(5) . . . . ? O2 C15 C16 S1 -0.1(5) . . . . ? C20 C15 C16 S1 -179.4(3) . . . . ? C6 S1 C16 C17 -104.6(3) . . . . ? Al1 S1 C16 C17 162.0(3) . . . . ? C6 S1 C16 C15 76.4(3) . . . . ? Al1 S1 C16 C15 -17.0(3) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? S1 C16 C17 C18 -179.1(3) . . . . ? C16 C17 C18 C19 -0.8(5) . . . . ? C16 C17 C18 C25 175.6(3) . . . . ? C17 C18 C19 C20 0.2(6) . . . . ? C25 C18 C19 C20 -176.2(4) . . . . ? C18 C19 C20 C15 1.2(6) . . . . ? C18 C19 C20 C21 -179.7(4) . . . . ? O2 C15 C20 C19 178.7(3) . . . . ? C16 C15 C20 C19 -2.1(5) . . . . ? O2 C15 C20 C21 -0.4(5) . . . . ? C16 C15 C20 C21 178.9(3) . . . . ? C19 C20 C21 C22 -112.8(4) . . . . ? C15 C20 C21 C22 66.2(5) . . . . ? C19 C20 C21 C24 6.8(5) . . . . ? C15 C20 C21 C24 -174.1(3) . . . . ? C19 C20 C21 C23 125.9(4) . . . . ? C15 C20 C21 C23 -55.1(5) . . . . ? C17 C18 C25 C27 142.7(4) . . . . ? C19 C18 C25 C27 -41.0(5) . . . . ? C17 C18 C25 C26 20.4(6) . . . . ? C19 C18 C25 C26 -163.3(4) . . . . ? C17 C18 C25 C28 -97.5(5) . . . . ? C19 C18 C25 C28 78.8(5) . . . . ? Al1 O3 C29 C30 26.0(4) . . . . ? Al1 O3 C29 C34 -154.7(3) . . . . ? O3 C29 C30 C31 -179.4(3) . . . . ? C34 C29 C30 C31 1.3(5) . . . . ? O3 C29 C30 S2 1.6(5) . . . . ? C34 C29 C30 S2 -177.8(3) . . . . ? C48 S2 C30 C31 -104.4(3) . . . . ? Al1 S2 C30 C31 163.2(3) . . . . ? C48 S2 C30 C29 74.6(3) . . . . ? Al1 S2 C30 C29 -17.7(3) . . . . ? C29 C30 C31 C32 0.1(6) . . . . ? S2 C30 C31 C32 179.1(3) . . . . ? C30 C31 C32 C33 -1.0(5) . . . . ? C30 C31 C32 C39 -179.8(3) . . . . ? C31 C32 C33 C34 0.6(6) . . . . ? C39 C32 C33 C34 179.4(3) . . . . ? C32 C33 C34 C29 0.8(6) . . . . ? C32 C33 C34 C35 -179.8(3) . . . . ? O3 C29 C34 C33 179.0(3) . . . . ? C30 C29 C34 C33 -1.6(5) . . . . ? O3 C29 C34 C35 -0.4(5) . . . . ? C30 C29 C34 C35 178.9(3) . . . . ? C33 C34 C35 C37 6.3(5) . . . . ? C29 C34 C35 C37 -174.3(3) . . . . ? C33 C34 C35 C36 -113.6(4) . . . . ? C29 C34 C35 C36 65.8(5) . . . . ? C33 C34 C35 C38 126.0(4) . . . . ? C29 C34 C35 C38 -54.6(5) . . . . ? C31 C32 C39 C41 -167.9(3) . . . . ? C33 C32 C39 C41 13.4(5) . . . . ? C31 C32 C39 C40 -48.3(5) . . . . ? C33 C32 C39 C40 133.0(4) . . . . ? C31 C32 C39 C42 71.3(4) . . . . ? C33 C32 C39 C42 -107.4(4) . . . . ? Al2 O4 C43 C48 -84.1(4) . . . . ? Al1 O4 C43 C48 40.8(4) . . . . ? Al2 O4 C43 C44 93.4(4) . . . . ? Al1 O4 C43 C44 -141.7(3) . . . . ? O4 C43 C44 C45 -165.0(3) . . . . ? C48 C43 C44 C45 12.4(5) . . . . ? O4 C43 C44 C49 15.3(6) . . . . ? C48 C43 C44 C49 -167.3(3) . . . . ? C43 C44 C45 C46 -4.5(6) . . . . ? C49 C44 C45 C46 175.2(4) . . . . ? C44 C45 C46 C47 -4.7(6) . . . . ? C44 C45 C46 C53 174.7(4) . . . . ? C45 C46 C47 C48 6.0(5) . . . . ? C53 C46 C47 C48 -173.4(3) . . . . ? C46 C47 C48 C43 1.9(6) . . . . ? C46 C47 C48 S2 -173.9(3) . . . . ? O4 C43 C48 C47 165.9(3) . . . . ? C44 C43 C48 C47 -11.6(5) . . . . ? O4 C43 C48 S2 -18.2(4) . . . . ? C44 C43 C48 S2 164.3(3) . . . . ? C30 S2 C48 C47 80.9(3) . . . . ? Al1 S2 C48 C47 170.6(3) . . . . ? C30 S2 C48 C43 -95.1(3) . . . . ? Al1 S2 C48 C43 -5.4(3) . . . . ? C43 C44 C49 C51 -105.0(4) . . . . ? C45 C44 C49 C51 75.3(4) . . . . ? C43 C44 C49 C50 17.6(5) . . . . ? C45 C44 C49 C50 -162.0(3) . . . . ? C43 C44 C49 C52 135.6(4) . . . . ? C45 C44 C49 C52 -44.1(5) . . . . ? C45 C46 C53 C56 174.9(4) . . . . ? C47 C46 C53 C56 -5.8(5) . . . . ? C45 C46 C53 C55 53.4(5) . . . . ? C47 C46 C53 C55 -127.2(4) . . . . ? C45 C46 C53 C54 -65.1(5) . . . . ? C47 C46 C53 C54 114.3(4) . . . . ? O4 Al2 C57 C58 -163.5(3) . . . . ? O1 Al2 C57 C58 -76.1(3) . . . . ? C61 Al2 C57 C58 63.5(4) . . . . ? Al1 Al2 C57 C58 -120.7(3) . . . . ? Al2 C57 C58 C59 172.2(3) . . . . ? Al2 C57 C58 C60 -65.7(4) . . . . ? O4 Al2 C61 C62 -69.4(3) . . . . ? O1 Al2 C61 C62 -157.5(3) . . . . ? C57 Al2 C61 C62 64.2(4) . . . . ? Al1 Al2 C61 C62 -111.7(3) . . . . ? Al2 C61 C62 C64 -66.3(4) . . . . ? Al2 C61 C62 C63 171.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.484 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.075 #===END data_complex_10 _database_code_depnum_ccdc_archive 'CCDC 752753' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 Al2 O4 S2' _chemical_formula_weight 812.99 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.577(3) _cell_length_b 10.5990(18) _cell_length_c 24.049(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.405(7) _cell_angle_gamma 90.00 _cell_volume 4319.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9273 _exptl_absorpt_correction_T_max 0.9676 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17642 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6031 _reflns_number_gt 3991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+17.1637P] 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 6031 _refine_ls_number_parameters 517 _refine_ls_number_restraints 212 _refine_ls_R_factor_all 0.1464 _refine_ls_R_factor_gt 0.1086 _refine_ls_wR_factor_ref 0.2196 _refine_ls_wR_factor_gt 0.2076 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.030 _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 0.24777(13) 0.1325(2) 0.05401(10) 0.0254(6) Uani 1 1 d . . . Al2 Al 0.18971(13) 0.3509(2) -0.01557(10) 0.0281(6) Uani 1 1 d . . . O1 O 0.2207(3) -0.0096(5) 0.0837(2) 0.0251(12) Uani 1 1 d . . . O2 O 0.1554(3) 0.1936(5) 0.00385(19) 0.0232(12) Uani 1 1 d . . . O3 O 0.2785(3) 0.3083(5) 0.0443(2) 0.0247(12) Uani 1 1 d . . . O4 O 0.2924(3) 0.0639(5) 0.0030(2) 0.0272(13) Uani 1 1 d . . . S1 S 0.17264(11) 0.22233(19) 0.12847(8) 0.0255(5) Uani 1 1 d . . . S2 S 0.37961(11) 0.12486(19) 0.12147(8) 0.0265(5) Uani 1 1 d . . . C1 C 0.2083(4) -0.0258(8) 0.1352(3) 0.0265(19) Uani 1 1 d . . . C2 C 0.1833(4) 0.0743(8) 0.1640(3) 0.0240(19) Uani 1 1 d . . . C3 C 0.1682(4) 0.0595(8) 0.2173(4) 0.031(2) Uani 1 1 d . . . H3 H 0.1517 0.1298 0.2356 0.037 Uiso 1 1 calc R . . C4 C 0.1769(4) -0.0567(8) 0.2438(3) 0.033(2) Uani 1 1 d . . . C5 C 0.2011(4) -0.1571(8) 0.2149(3) 0.032(2) Uani 1 1 d . . . H5 H 0.2072 -0.2377 0.2328 0.039 Uiso 1 1 calc R . . C6 C 0.2165(4) -0.1456(7) 0.1623(3) 0.0279(19) Uani 1 1 d . . . C7 C 0.1626(5) -0.0752(9) 0.3026(4) 0.043(2) Uani 1 1 d . . . H7A H 0.2104 -0.0530 0.3325 0.065 Uiso 1 1 calc R . . H7B H 0.1491 -0.1636 0.3071 0.065 Uiso 1 1 calc R . . H7C H 0.1190 -0.0209 0.3061 0.065 Uiso 1 1 calc R . . C8 C 0.2432(5) -0.2550(7) 0.1320(4) 0.040(2) Uani 1 1 d . . . H8A H 0.2557 -0.3272 0.1583 0.060 Uiso 1 1 calc R . . H8B H 0.2903 -0.2305 0.1201 0.060 Uiso 1 1 calc R . . H8C H 0.2010 -0.2782 0.0979 0.060 Uiso 1 1 calc R . . C9 C 0.0836(4) 0.1849(7) 0.0184(4) 0.028(2) Uani 1 1 d . . . C10 C 0.0818(4) 0.1949(7) 0.0748(3) 0.0220(18) Uani 1 1 d . . . C11 C 0.0113(4) 0.1879(7) 0.0885(4) 0.030(2) Uani 1 1 d . . . H11 H 0.0101 0.1972 0.1275 0.036 Uiso 1 1 calc R . . C12 C -0.0583(4) 0.1675(7) 0.0465(4) 0.029(2) Uani 1 1 d . . . C13 C -0.0540(4) 0.1569(7) -0.0100(3) 0.0290(19) Uani 1 1 d . . . H13 H -0.1015 0.1429 -0.0393 0.035 Uiso 1 1 calc R . . C14 C 0.0153(4) 0.1656(7) -0.0260(3) 0.029(2) Uani 1 1 d . . . C15 C 0.0168(4) 0.1571(8) -0.0878(3) 0.038(2) Uani 1 1 d . . . H15A H -0.0348 0.1288 -0.1112 0.057 Uiso 1 1 calc R . . H15B H 0.0574 0.0966 -0.0914 0.057 Uiso 1 1 calc R . . H15C H 0.0288 0.2402 -0.1011 0.057 Uiso 1 1 calc R . . C16 C -0.1365(5) 0.1576(8) 0.0611(4) 0.041(2) Uani 1 1 d . . . H16A H -0.1680 0.0903 0.0381 0.062 Uiso 1 1 calc R . . H16B H -0.1648 0.2379 0.0525 0.062 Uiso 1 1 calc R . . H16C H -0.1273 0.1383 0.1022 0.062 Uiso 1 1 calc R . . C17 C 0.3551(4) 0.3493(7) 0.0624(3) 0.0233(18) Uani 1 1 d . . . C18 C 0.3765(4) 0.4684(7) 0.0496(3) 0.029(2) Uani 1 1 d . . . C19 C 0.4554(5) 0.5020(8) 0.0689(3) 0.034(2) Uani 1 1 d . . . H19 H 0.4710 0.5828 0.0588 0.041 Uiso 1 1 calc R . . C20 C 0.5129(5) 0.4229(8) 0.1024(3) 0.031(2) Uani 1 1 d . . . C21 C 0.4887(4) 0.3076(8) 0.1165(3) 0.028(2) Uani 1 1 d . . . H21 H 0.5263 0.2517 0.1396 0.034 Uiso 1 1 calc R . . C22 C 0.4108(4) 0.2706(7) 0.0978(3) 0.0248(18) Uani 1 1 d . . . C23 C 0.3179(5) 0.5638(7) 0.0166(3) 0.033(2) Uani 1 1 d . . . H23A H 0.2990 0.5374 -0.0238 0.049 Uiso 1 1 calc R . . H23B H 0.3435 0.6464 0.0186 0.049 Uiso 1 1 calc R . . H23C H 0.2732 0.5695 0.0337 0.049 Uiso 1 1 calc R . . C24 C 0.5989(5) 0.4609(8) 0.1227(4) 0.049(3) Uani 1 1 d . . . H24A H 0.6060 0.5198 0.1551 0.074 Uiso 1 1 calc R . . H24B H 0.6148 0.5018 0.0911 0.074 Uiso 1 1 calc R . . H24C H 0.6314 0.3857 0.1352 0.074 Uiso 1 1 calc R . . C25 C 0.3589(4) -0.0032(7) 0.0203(3) 0.030(2) Uani 1 1 d . . . C26 C 0.3822(4) -0.0885(7) -0.0163(3) 0.0276(19) Uani 1 1 d . . . C27 C 0.4528(5) -0.1510(7) 0.0040(4) 0.031(2) Uani 1 1 d . . . H27 H 0.4679 -0.2093 -0.0210 0.038 Uiso 1 1 calc R . . C28 C 0.5035(4) -0.1345(8) 0.0588(4) 0.033(2) Uani 1 1 d . . . C29 C 0.4799(5) -0.0516(8) 0.0951(4) 0.033(2) Uani 1 1 d . . . H29 H 0.5121 -0.0384 0.1332 0.040 Uiso 1 1 calc R . . C30 C 0.4090(4) 0.0127(7) 0.0759(3) 0.0261(19) Uani 1 1 d . . . C31 C 0.3319(5) -0.1102(8) -0.0766(3) 0.037(2) Uani 1 1 d . . . H31A H 0.2982 -0.1841 -0.0772 0.055 Uiso 1 1 calc R . . H31B H 0.3658 -0.1248 -0.1024 0.055 Uiso 1 1 calc R . . H31C H 0.2988 -0.0359 -0.0897 0.055 Uiso 1 1 calc R . . C32 C 0.5815(5) -0.2031(8) 0.0772(4) 0.042(2) Uani 1 1 d . . . H32A H 0.6244 -0.1446 0.0765 0.063 Uiso 1 1 calc R . . H32B H 0.5817 -0.2732 0.0507 0.063 Uiso 1 1 calc R . . H32C H 0.5891 -0.2360 0.1164 0.063 Uiso 1 1 calc R . . C33 C 0.1209(5) 0.4783(8) 0.0044(4) 0.042(2) Uani 1 1 d . . . H33A H 0.1330 0.4861 0.0464 0.064 Uiso 1 1 calc R . . H33B H 0.0657 0.4529 -0.0110 0.064 Uiso 1 1 calc R . . H33C H 0.1296 0.5596 -0.0123 0.064 Uiso 1 1 calc R . . C34 C 0.2121(5) 0.3428(8) -0.0907(3) 0.036(2) Uani 1 1 d . . . H34A H 0.2144 0.4285 -0.1054 0.054 Uiso 1 1 calc R . . H34B H 0.1703 0.2953 -0.1176 0.054 Uiso 1 1 calc R . . H34C H 0.2629 0.3007 -0.0867 0.054 Uiso 1 1 calc R . . C35 C 0.6580(6) 0.2347(11) 0.2612(5) 0.088(3) Uani 1 1 d DU . . C36 C 0.5790(6) 0.2157(12) 0.2580(4) 0.084(3) Uani 1 1 d DU . . H36 H 0.5567 0.1348 0.2471 0.101 Uiso 1 1 calc R . . C37 C 0.5310(7) 0.3105(11) 0.2700(5) 0.091(3) Uani 1 1 d DU . . H37 H 0.4772 0.2931 0.2676 0.109 Uiso 1 1 calc R . . C38 C 0.5611(7) 0.4304(12) 0.2855(5) 0.097(3) Uani 1 1 d DU . . H38 H 0.5284 0.4970 0.2922 0.116 Uiso 1 1 calc R . . C39 C 0.6412(7) 0.4487(12) 0.2907(5) 0.101(3) Uani 1 1 d DU . . H39 H 0.6638 0.5287 0.3030 0.121 Uiso 1 1 calc R . . C40 C 0.6892(7) 0.3541(11) 0.2787(5) 0.098(3) Uani 1 1 d DU . . H40 H 0.7434 0.3706 0.2823 0.117 Uiso 1 1 calc R . . C41 C 0.7081(7) 0.1409(12) 0.2498(5) 0.111(4) Uani 1 1 d DU . . H41A H 0.6770 0.0658 0.2345 0.167 Uiso 1 1 calc R . . H41B H 0.7477 0.1191 0.2856 0.167 Uiso 1 1 calc R . . H41C H 0.7344 0.1723 0.2214 0.167 Uiso 1 1 calc R . . C42 C 0.4648(5) 0.9361(9) 0.2943(4) 0.072(2) Uani 1 1 d DU . . C43 C 0.5449(5) 0.9226(10) 0.3209(5) 0.078(3) Uani 1 1 d DU . . H43 H 0.5677 0.9668 0.3557 0.094 Uiso 1 1 calc R . . C44 C 0.5920(6) 0.8451(10) 0.2973(5) 0.081(3) Uani 1 1 d DU . . H44 H 0.6468 0.8396 0.3157 0.097 Uiso 1 1 calc R . . C45 C 0.5607(6) 0.7754(11) 0.2475(5) 0.082(3) Uani 1 1 d DU . . H45 H 0.5934 0.7230 0.2316 0.098 Uiso 1 1 calc R . . C46 C 0.4807(6) 0.7847(11) 0.2219(5) 0.081(3) Uani 1 1 d DU . . H46 H 0.4573 0.7358 0.1886 0.097 Uiso 1 1 calc R . . C47 C 0.4343(6) 0.8651(9) 0.2445(4) 0.074(2) Uani 1 1 d DU . . H47 H 0.3797 0.8721 0.2255 0.088 Uiso 1 1 calc R . . C48 C 0.4152(7) 1.0160(11) 0.3159(6) 0.105(4) Uani 1 1 d DU . . H48A H 0.4165 0.9904 0.3553 0.158 Uiso 1 1 calc R . . H48B H 0.3611 1.0097 0.2914 0.158 Uiso 1 1 calc R . . H48C H 0.4336 1.1033 0.3161 0.158 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0214(12) 0.0280(14) 0.0264(13) 0.0017(11) 0.0055(10) -0.0004(11) Al2 0.0225(13) 0.0313(15) 0.0301(14) 0.0045(12) 0.0061(11) -0.0008(11) O1 0.024(3) 0.025(3) 0.026(3) -0.005(2) 0.008(2) 0.002(2) O2 0.026(3) 0.026(3) 0.016(3) 0.002(2) 0.004(2) 0.003(2) O3 0.023(3) 0.027(3) 0.026(3) 0.005(2) 0.009(2) -0.003(2) O4 0.019(3) 0.032(3) 0.028(3) 0.003(3) 0.003(2) 0.000(3) S1 0.0244(11) 0.0295(12) 0.0222(11) 0.0011(9) 0.0056(9) -0.0027(9) S2 0.0251(11) 0.0318(12) 0.0239(11) 0.0015(9) 0.0085(9) -0.0008(10) C1 0.013(4) 0.041(5) 0.027(5) -0.012(4) 0.008(4) -0.004(4) C2 0.015(4) 0.045(5) 0.012(4) 0.005(4) 0.003(3) -0.001(4) C3 0.019(4) 0.029(5) 0.045(6) -0.001(4) 0.007(4) -0.002(4) C4 0.022(4) 0.044(6) 0.029(5) 0.005(4) 0.001(4) 0.005(4) C5 0.033(5) 0.031(5) 0.032(5) 0.011(4) 0.008(4) -0.004(4) C6 0.023(4) 0.022(5) 0.035(5) 0.005(4) 0.002(4) -0.008(4) C7 0.043(5) 0.050(6) 0.038(5) 0.003(5) 0.015(5) -0.001(5) C8 0.044(5) 0.027(5) 0.045(6) 0.004(4) 0.004(4) 0.001(4) C9 0.020(4) 0.019(4) 0.049(6) 0.002(4) 0.017(4) 0.003(3) C10 0.012(4) 0.025(5) 0.033(5) 0.001(4) 0.011(3) 0.001(3) C11 0.032(5) 0.023(5) 0.040(5) 0.003(4) 0.015(4) 0.007(4) C12 0.013(4) 0.019(4) 0.058(6) 0.011(4) 0.013(4) 0.006(3) C13 0.025(5) 0.027(5) 0.033(5) 0.003(4) 0.004(4) 0.001(4) C14 0.027(5) 0.025(5) 0.031(5) 0.010(4) 0.001(4) 0.000(4) C15 0.025(5) 0.038(5) 0.044(6) -0.005(4) -0.002(4) -0.003(4) C16 0.034(5) 0.038(6) 0.049(6) 0.009(5) 0.007(4) 0.003(4) C17 0.015(4) 0.038(5) 0.020(4) -0.008(4) 0.011(3) -0.011(4) C18 0.027(5) 0.030(5) 0.032(5) -0.003(4) 0.011(4) -0.006(4) C19 0.048(6) 0.024(5) 0.035(5) -0.002(4) 0.018(4) -0.008(4) C20 0.031(5) 0.028(5) 0.035(5) 0.000(4) 0.009(4) -0.002(4) C21 0.028(5) 0.035(5) 0.024(5) -0.010(4) 0.010(4) 0.007(4) C22 0.023(4) 0.036(5) 0.018(4) -0.007(4) 0.011(4) -0.002(4) C23 0.035(5) 0.026(5) 0.039(5) -0.003(4) 0.011(4) -0.013(4) C24 0.039(5) 0.033(6) 0.068(7) 0.000(5) 0.002(5) -0.009(4) C25 0.027(5) 0.027(5) 0.036(5) 0.005(4) 0.011(4) -0.003(4) C26 0.027(5) 0.021(4) 0.039(5) 0.000(4) 0.015(4) -0.004(4) C27 0.035(5) 0.027(5) 0.041(5) -0.003(4) 0.024(4) -0.003(4) C28 0.025(5) 0.028(5) 0.048(6) 0.003(4) 0.016(4) -0.005(4) C29 0.030(5) 0.040(5) 0.031(5) 0.007(4) 0.009(4) -0.006(4) C30 0.021(4) 0.030(5) 0.031(5) 0.006(4) 0.014(4) 0.001(4) C31 0.038(5) 0.040(6) 0.039(5) 0.000(4) 0.020(4) 0.002(4) C32 0.035(5) 0.041(6) 0.054(6) 0.009(5) 0.018(5) 0.005(4) C33 0.034(5) 0.031(5) 0.063(7) 0.014(5) 0.014(5) 0.007(4) C34 0.035(5) 0.056(6) 0.017(4) 0.008(4) 0.005(4) -0.004(4) C35 0.092(5) 0.115(6) 0.061(6) 0.027(6) 0.026(5) 0.021(5) C36 0.089(5) 0.119(6) 0.046(5) 0.029(5) 0.020(5) 0.017(5) C37 0.096(6) 0.122(7) 0.056(6) 0.029(6) 0.024(5) 0.020(5) C38 0.113(6) 0.117(6) 0.064(6) 0.029(6) 0.029(6) 0.018(6) C39 0.116(6) 0.113(6) 0.074(6) 0.026(6) 0.028(6) 0.010(5) C40 0.106(6) 0.116(7) 0.073(6) 0.031(6) 0.027(6) 0.009(5) C41 0.120(9) 0.141(9) 0.077(8) 0.027(8) 0.035(8) 0.050(8) C42 0.055(4) 0.056(5) 0.103(6) 0.025(4) 0.017(4) -0.012(4) C43 0.060(5) 0.072(6) 0.095(6) 0.020(5) 0.007(4) -0.010(4) C44 0.059(5) 0.087(7) 0.092(6) 0.034(5) 0.010(5) 0.002(5) C45 0.077(5) 0.090(6) 0.084(6) 0.032(5) 0.030(5) -0.001(5) C46 0.079(5) 0.085(6) 0.077(6) 0.025(5) 0.018(5) -0.016(5) C47 0.057(5) 0.069(6) 0.088(6) 0.036(4) 0.008(4) -0.014(4) C48 0.081(7) 0.066(8) 0.174(11) 0.007(7) 0.045(8) -0.006(6) _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 1.785(5) . ? Al1 O4 1.778(5) . ? Al1 O2 1.863(5) . ? Al1 O3 1.971(5) . ? Al1 S2 2.452(3) . ? Al1 S1 2.667(3) . ? Al2 O2 1.874(5) . ? Al2 O3 1.876(5) . ? Al2 C34 1.950(7) . ? Al2 C33 1.955(8) . ? O1 C1 1.324(8) . ? O2 C9 1.399(8) . ? O3 C17 1.371(8) . ? O4 C25 1.337(9) . ? S1 C2 1.773(8) . ? S1 C10 1.789(7) . ? S2 C30 1.783(8) . ? S2 C22 1.782(8) . ? C1 C2 1.400(10) . ? C1 C6 1.417(11) . ? C2 C3 1.385(10) . ? C3 C4 1.376(11) . ? C3 H3 0.9500 . ? C4 C5 1.397(11) . ? C4 C7 1.514(11) . ? C5 C6 1.367(10) . ? C5 H5 0.9500 . ? C6 C8 1.510(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.369(10) . ? C9 C14 1.393(10) . ? C10 C11 1.367(9) . ? C11 C12 1.380(11) . ? C11 H11 0.9500 . ? C12 C13 1.386(11) . ? C12 C16 1.510(10) . ? C13 C14 1.375(10) . ? C13 H13 0.9500 . ? C14 C15 1.496(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.376(10) . ? C17 C22 1.391(10) . ? C18 C19 1.387(11) . ? C18 C23 1.508(11) . ? C19 C20 1.393(11) . ? C19 H19 0.9500 . ? C20 C21 1.367(11) . ? C20 C24 1.513(11) . ? C21 C22 1.380(10) . ? C21 H21 0.9500 . ? 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 1.396(11) . ? C25 C30 1.403(10) . ? C26 C27 1.376(10) . ? C26 C31 1.504(11) . ? C27 C28 1.391(11) . ? C27 H27 0.9500 . ? C28 C29 1.378(11) . ? C28 C32 1.512(11) . ? C29 C30 1.388(10) . ? C29 H29 0.9500 . ? 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 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.385(7) . ? C35 C40 1.398(7) . ? C35 C41 1.401(7) . ? C36 C37 1.392(7) . ? C36 H36 0.9500 . ? C37 C38 1.388(8) . ? C37 H37 0.9500 . ? C38 C39 1.394(8) . ? C38 H38 0.9500 . ? C39 C40 1.389(8) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.391(7) . ? C42 C47 1.394(7) . ? C42 C48 1.409(7) . ? C43 C44 1.390(7) . ? C43 H43 0.9500 . ? C44 C45 1.391(7) . ? C44 H44 0.9500 . ? C45 C46 1.381(7) . ? C45 H45 0.9500 . ? C46 C47 1.387(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O4 98.3(3) . . ? O1 Al1 O2 105.8(2) . . ? O4 Al1 O2 99.4(2) . . ? O1 Al1 O3 162.8(2) . . ? O4 Al1 O3 96.9(2) . . ? O2 Al1 O3 79.3(2) . . ? O1 Al1 S2 90.76(18) . . ? O4 Al1 S2 86.00(18) . . ? O2 Al1 S2 161.4(2) . . ? O3 Al1 S2 82.48(17) . . ? O1 Al1 S1 78.46(17) . . ? O4 Al1 S1 175.8(2) . . ? O2 Al1 S1 78.98(16) . . ? O3 Al1 S1 86.66(16) . . ? S2 Al1 S1 96.72(10) . . ? O2 Al2 O3 81.5(2) . . ? O2 Al2 C34 110.4(3) . . ? O3 Al2 C34 111.7(3) . . ? O2 Al2 C33 107.0(3) . . ? O3 Al2 C33 114.9(3) . . ? C34 Al2 C33 123.2(4) . . ? C1 O1 Al1 127.7(5) . . ? C9 O2 Al1 120.3(4) . . ? C9 O2 Al2 119.5(4) . . ? Al1 O2 Al2 100.8(2) . . ? C17 O3 Al2 135.5(5) . . ? C17 O3 Al1 122.6(5) . . ? Al2 O3 Al1 96.9(2) . . ? C25 O4 Al1 120.9(5) . . ? C2 S1 C10 99.4(3) . . ? C2 S1 Al1 90.0(2) . . ? C10 S1 Al1 87.9(2) . . ? C30 S2 C22 102.6(3) . . ? C30 S2 Al1 89.6(3) . . ? C22 S2 Al1 94.4(3) . . ? O1 C1 C2 121.0(7) . . ? O1 C1 C6 121.6(7) . . ? C2 C1 C6 117.3(7) . . ? C3 C2 C1 122.3(7) . . ? C3 C2 S1 121.7(6) . . ? C1 C2 S1 116.0(5) . . ? C4 C3 C2 120.3(8) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 117.6(7) . . ? C3 C4 C7 121.5(8) . . ? C5 C4 C7 120.9(8) . . ? C6 C5 C4 123.6(8) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C5 C6 C1 119.0(7) . . ? C5 C6 C8 122.8(7) . . ? C1 C6 C8 118.2(7) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 121.9(7) . . ? C10 C9 O2 120.1(7) . . ? C14 C9 O2 117.9(7) . . ? C11 C10 C9 119.7(7) . . ? C11 C10 S1 121.8(6) . . ? C9 C10 S1 118.5(5) . . ? C10 C11 C12 121.1(8) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 117.6(7) . . ? C11 C12 C16 121.6(8) . . ? C13 C12 C16 120.8(7) . . ? C14 C13 C12 123.4(7) . . ? C14 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C13 C14 C9 116.3(7) . . ? C13 C14 C15 121.6(7) . . ? C9 C14 C15 122.1(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 121.6(7) . . ? O3 C17 C22 118.4(7) . . ? C18 C17 C22 119.8(7) . . ? C17 C18 C19 118.0(7) . . ? C17 C18 C23 122.9(7) . . ? C19 C18 C23 119.1(7) . . ? C18 C19 C20 123.2(8) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 117.1(7) . . ? C21 C20 C24 120.5(8) . . ? C19 C20 C24 122.4(7) . . ? C20 C21 C22 121.4(8) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C17 120.3(7) . . ? C21 C22 S2 120.3(6) . . ? C17 C22 S2 119.3(5) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 C26 121.8(7) . . ? O4 C25 C30 120.5(7) . . ? C26 C25 C30 117.7(7) . . ? C25 C26 C27 118.4(8) . . ? C25 C26 C31 120.7(7) . . ? C27 C26 C31 120.9(7) . . ? C28 C27 C26 124.5(8) . . ? C28 C27 H27 117.8 . . ? C26 C27 H27 117.8 . . ? C29 C28 C27 117.1(7) . . ? C29 C28 C32 121.6(8) . . ? C27 C28 C32 121.3(8) . . ? C28 C29 C30 119.8(8) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 122.5(7) . . ? C29 C30 S2 120.3(6) . . ? C25 C30 S2 117.1(6) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Al2 C33 H33A 109.5 . . ? Al2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Al2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al2 C34 H34A 109.5 . . ? Al2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Al2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 117.1(10) . . ? C36 C35 C41 123.9(11) . . ? C40 C35 C41 119.0(10) . . ? C35 C36 C37 122.5(11) . . ? C35 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 120.5(11) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 117.1(11) . . ? C37 C38 H38 121.4 . . ? C39 C38 H38 121.4 . . ? C40 C39 C38 122.4(12) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C39 C40 C35 120.3(11) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? C35 C41 H41A 109.5 . . ? C35 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C35 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 116.8(9) . . ? C43 C42 C48 122.7(10) . . ? C47 C42 C48 120.5(9) . . ? C44 C43 C42 120.8(10) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C43 121.6(10) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C46 C45 C44 118.0(10) . . ? C46 C45 H45 121.0 . . ? C44 C45 H45 121.0 . . ? C45 C46 C47 120.2(10) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C42 122.5(9) . . ? C46 C47 H47 118.7 . . ? C42 C47 H47 118.7 . . ? C42 C48 H48A 109.5 . . ? C42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Al1 O1 C1 156.1(6) . . . . ? O2 Al1 O1 C1 -101.5(6) . . . . ? O3 Al1 O1 C1 3.7(12) . . . . ? S2 Al1 O1 C1 70.1(6) . . . . ? S1 Al1 O1 C1 -26.7(5) . . . . ? O1 Al1 O2 C9 38.8(5) . . . . ? O4 Al1 O2 C9 140.3(5) . . . . ? O3 Al1 O2 C9 -124.4(5) . . . . ? S2 Al1 O2 C9 -113.9(7) . . . . ? S1 Al1 O2 C9 -35.7(5) . . . . ? O1 Al1 O2 Al2 172.6(2) . . . . ? O4 Al1 O2 Al2 -85.9(3) . . . . ? O3 Al1 O2 Al2 9.4(2) . . . . ? S2 Al1 O2 Al2 19.9(7) . . . . ? S1 Al1 O2 Al2 98.0(2) . . . . ? O3 Al2 O2 C9 124.4(5) . . . . ? C34 Al2 O2 C9 -125.6(5) . . . . ? C33 Al2 O2 C9 10.9(6) . . . . ? O3 Al2 O2 Al1 -9.8(2) . . . . ? C34 Al2 O2 Al1 100.2(3) . . . . ? C33 Al2 O2 Al1 -123.3(3) . . . . ? O2 Al2 O3 C17 163.1(6) . . . . ? C34 Al2 O3 C17 54.4(7) . . . . ? C33 Al2 O3 C17 -92.1(7) . . . . ? O2 Al2 O3 Al1 9.2(2) . . . . ? C34 Al2 O3 Al1 -99.5(3) . . . . ? C33 Al2 O3 Al1 114.0(3) . . . . ? O1 Al1 O3 C17 83.1(9) . . . . ? O4 Al1 O3 C17 -69.5(5) . . . . ? O2 Al1 O3 C17 -167.8(5) . . . . ? S2 Al1 O3 C17 15.5(5) . . . . ? S1 Al1 O3 C17 112.8(5) . . . . ? O1 Al1 O3 Al2 -118.4(8) . . . . ? O4 Al1 O3 Al2 89.1(2) . . . . ? O2 Al1 O3 Al2 -9.3(2) . . . . ? S2 Al1 O3 Al2 174.1(2) . . . . ? S1 Al1 O3 Al2 -88.69(19) . . . . ? O1 Al1 O4 C25 -66.2(6) . . . . ? O2 Al1 O4 C25 -173.9(5) . . . . ? O3 Al1 O4 C25 105.9(5) . . . . ? S2 Al1 O4 C25 24.0(5) . . . . ? S1 Al1 O4 C25 -106(3) . . . . ? O1 Al1 S1 C2 17.5(3) . . . . ? O4 Al1 S1 C2 58(3) . . . . ? O2 Al1 S1 C2 126.4(3) . . . . ? O3 Al1 S1 C2 -153.9(3) . . . . ? S2 Al1 S1 C2 -71.9(2) . . . . ? O1 Al1 S1 C10 -81.9(3) . . . . ? O4 Al1 S1 C10 -41(3) . . . . ? O2 Al1 S1 C10 27.0(3) . . . . ? O3 Al1 S1 C10 106.7(3) . . . . ? S2 Al1 S1 C10 -171.3(3) . . . . ? O1 Al1 S2 C30 80.5(3) . . . . ? O4 Al1 S2 C30 -17.8(3) . . . . ? O2 Al1 S2 C30 -125.7(6) . . . . ? O3 Al1 S2 C30 -115.3(3) . . . . ? S1 Al1 S2 C30 159.0(3) . . . . ? O1 Al1 S2 C22 -176.9(3) . . . . ? O4 Al1 S2 C22 84.8(3) . . . . ? O2 Al1 S2 C22 -23.1(6) . . . . ? O3 Al1 S2 C22 -12.7(3) . . . . ? S1 Al1 S2 C22 -98.4(2) . . . . ? Al1 O1 C1 C2 27.0(10) . . . . ? Al1 O1 C1 C6 -155.7(5) . . . . ? O1 C1 C2 C3 178.5(7) . . . . ? C6 C1 C2 C3 1.1(11) . . . . ? O1 C1 C2 S1 -1.9(9) . . . . ? C6 C1 C2 S1 -179.3(5) . . . . ? C10 S1 C2 C3 -104.4(6) . . . . ? Al1 S1 C2 C3 167.7(6) . . . . ? C10 S1 C2 C1 76.0(6) . . . . ? Al1 S1 C2 C1 -11.9(5) . . . . ? C1 C2 C3 C4 -0.5(11) . . . . ? S1 C2 C3 C4 179.9(6) . . . . ? C2 C3 C4 C5 0.0(11) . . . . ? C2 C3 C4 C7 178.6(7) . . . . ? C3 C4 C5 C6 0.0(12) . . . . ? C7 C4 C5 C6 -178.6(7) . . . . ? C4 C5 C6 C1 0.5(12) . . . . ? C4 C5 C6 C8 179.5(7) . . . . ? O1 C1 C6 C5 -178.5(7) . . . . ? C2 C1 C6 C5 -1.0(11) . . . . ? O1 C1 C6 C8 2.5(11) . . . . ? C2 C1 C6 C8 179.9(7) . . . . ? Al1 O2 C9 C10 33.5(9) . . . . ? Al2 O2 C9 C10 -91.9(7) . . . . ? Al1 O2 C9 C14 -146.2(6) . . . . ? Al2 O2 C9 C14 88.4(7) . . . . ? C14 C9 C10 C11 -1.1(12) . . . . ? O2 C9 C10 C11 179.2(6) . . . . ? C14 C9 C10 S1 -178.9(6) . . . . ? O2 C9 C10 S1 1.3(10) . . . . ? C2 S1 C10 C11 71.6(7) . . . . ? Al1 S1 C10 C11 161.3(6) . . . . ? C2 S1 C10 C9 -110.5(6) . . . . ? Al1 S1 C10 C9 -20.9(6) . . . . ? C9 C10 C11 C12 1.8(12) . . . . ? S1 C10 C11 C12 179.6(6) . . . . ? C10 C11 C12 C13 -1.2(11) . . . . ? C10 C11 C12 C16 179.1(7) . . . . ? C11 C12 C13 C14 0.0(12) . . . . ? C16 C12 C13 C14 179.7(7) . . . . ? C12 C13 C14 C9 0.7(12) . . . . ? C12 C13 C14 C15 -178.3(8) . . . . ? C10 C9 C14 C13 -0.1(11) . . . . ? O2 C9 C14 C13 179.6(6) . . . . ? C10 C9 C14 C15 178.9(7) . . . . ? O2 C9 C14 C15 -1.4(11) . . . . ? Al2 O3 C17 C18 23.9(10) . . . . ? Al1 O3 C17 C18 172.7(5) . . . . ? Al2 O3 C17 C22 -160.6(5) . . . . ? Al1 O3 C17 C22 -11.8(8) . . . . ? O3 C17 C18 C19 -179.3(6) . . . . ? C22 C17 C18 C19 5.3(11) . . . . ? O3 C17 C18 C23 1.9(11) . . . . ? C22 C17 C18 C23 -173.6(7) . . . . ? C17 C18 C19 C20 -2.7(12) . . . . ? C23 C18 C19 C20 176.3(7) . . . . ? C18 C19 C20 C21 -0.3(12) . . . . ? C18 C19 C20 C24 179.6(8) . . . . ? C19 C20 C21 C22 0.7(11) . . . . ? C24 C20 C21 C22 -179.3(7) . . . . ? C20 C21 C22 C17 2.0(11) . . . . ? C20 C21 C22 S2 -175.1(6) . . . . ? O3 C17 C22 C21 179.3(6) . . . . ? C18 C17 C22 C21 -5.1(11) . . . . ? O3 C17 C22 S2 -3.5(9) . . . . ? C18 C17 C22 S2 172.1(6) . . . . ? C30 S2 C22 C21 -80.1(6) . . . . ? Al1 S2 C22 C21 -170.6(6) . . . . ? C30 S2 C22 C17 102.8(6) . . . . ? Al1 S2 C22 C17 12.2(6) . . . . ? Al1 O4 C25 C26 160.1(6) . . . . ? Al1 O4 C25 C30 -21.5(9) . . . . ? O4 C25 C26 C27 177.9(7) . . . . ? C30 C25 C26 C27 -0.5(11) . . . . ? O4 C25 C26 C31 -1.3(11) . . . . ? C30 C25 C26 C31 -179.7(7) . . . . ? C25 C26 C27 C28 -0.5(12) . . . . ? C31 C26 C27 C28 178.7(7) . . . . ? C26 C27 C28 C29 1.3(12) . . . . ? C26 C27 C28 C32 -177.6(7) . . . . ? C27 C28 C29 C30 -1.1(11) . . . . ? C32 C28 C29 C30 177.8(7) . . . . ? C28 C29 C30 C25 0.2(12) . . . . ? C28 C29 C30 S2 -177.6(6) . . . . ? O4 C25 C30 C29 -177.8(7) . . . . ? C26 C25 C30 C29 0.7(11) . . . . ? O4 C25 C30 S2 0.1(10) . . . . ? C26 C25 C30 S2 178.5(5) . . . . ? C22 S2 C30 C29 96.6(7) . . . . ? Al1 S2 C30 C29 -169.0(6) . . . . ? C22 S2 C30 C25 -81.3(6) . . . . ? Al1 S2 C30 C25 13.1(6) . . . . ? C40 C35 C36 C37 1.4(18) . . . . ? C41 C35 C36 C37 179.4(11) . . . . ? C35 C36 C37 C38 0.7(18) . . . . ? C36 C37 C38 C39 -2.8(18) . . . . ? C37 C38 C39 C40 2.9(19) . . . . ? C38 C39 C40 C35 -1(2) . . . . ? C36 C35 C40 C39 -1.4(19) . . . . ? C41 C35 C40 C39 -179.5(11) . . . . ? C47 C42 C43 C44 2.3(16) . . . . ? C48 C42 C43 C44 -178.4(11) . . . . ? C42 C43 C44 C45 -2.1(18) . . . . ? C43 C44 C45 C46 -0.3(17) . . . . ? C44 C45 C46 C47 2.3(17) . . . . ? C45 C46 C47 C42 -2.1(17) . . . . ? C43 C42 C47 C46 -0.3(16) . . . . ? C48 C42 C47 C46 -179.6(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.582 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.079 #===END