Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Jun Okuda' _publ_contact_author_address ; Institute of Inorganic Chemistry RWTH Aachen University Professor-Pirlet-Strasse 1 Aachen 52074 GERMANY ; _publ_contact_author_phone '049 241 8094645' _publ_contact_author_fax '049 241 8092644' _publ_contact_author_email jun.okuda@ac.rwth-aachen.de _publ_section_title ; Aluminum alkyl complexes supported by [OSSO] type bisphenolato ligands: synthesis, characterization and living polymerization of rac-lactide ; loop_ _publ_author_name _publ_author_address H.Ma ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof. Pirlet-Str. 1 D-52056 Aachen Germany ; G.Melillo ; Dipartimento di Chimica Universita di Salerno Via S. Allende I-84081 Baronissi (SA) Italy ; L.Oliva ; Dipartimento di Chimica Universita di Salerno Via S. Allende I-84081 Baronissi (SA) Italy ; U.Englert ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof. Pirlet-Str. 1 D-52056 Aachen Germany ; T.P.Spaniol ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof. Pirlet-Str. 1 D-52056 Aachen Germany ; J.Okuda ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof. Pirlet-Str. 1 D-52056 Aachen Germany ; #============================================================================== data_hm10 _database_code_depnum_ccdc_archive 'CCDC 244970' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 Al O2 S2' _chemical_formula_weight 458.63 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 8.8288(13) _cell_length_b 15.074(2) _cell_length_c 18.759(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2496.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 29929 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 28.36 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8714 _exptl_absorpt_correction_T_max 0.9387 _exptl_absorpt_process_details 'Bruker area detector absorption correction' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ; Bruker AXS diffractometer with CCD area detector ; _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29929 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6235 _reflns_number_gt 5525 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction 'SAINT, SADABS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows, Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0481P)^2^+0.0498P] 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 noref _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 0.01(6) _refine_ls_number_reflns 6235 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 S1 S 0.74722(6) 0.77195(3) 0.60672(3) 0.02021(11) Uani 1 1 d . . . S2 S 0.58571(6) 0.85677(3) 0.75044(3) 0.02317(12) Uani 1 1 d . . . O1 O 0.99661(15) 0.88779(9) 0.60856(7) 0.0204(3) Uani 1 1 d . . . O2 O 0.75602(17) 0.98356(8) 0.66003(7) 0.0207(3) Uani 1 1 d . . . Al Al 0.86211(7) 0.88837(4) 0.67972(3) 0.01912(13) Uani 1 1 d . . . C1 C 0.9407(2) 0.88222(13) 0.54194(10) 0.0183(4) Uani 1 1 d . . . C2 C 0.8110(2) 0.83089(13) 0.53027(11) 0.0186(4) Uani 1 1 d . . . C3 C 0.7364(2) 0.82829(13) 0.46521(11) 0.0216(4) Uani 1 1 d . . . H3 H 0.6477 0.7933 0.4595 0.026 Uiso 1 1 calc R . . C4 C 0.7928(2) 0.87721(13) 0.40889(11) 0.0219(4) Uani 1 1 d . . . C5 C 0.9278(2) 0.92375(13) 0.41873(11) 0.0208(4) Uani 1 1 d . . . H5 H 0.9687 0.9548 0.3791 0.025 Uiso 1 1 calc R . . C6 C 1.0069(2) 0.92758(13) 0.48360(11) 0.0189(4) Uani 1 1 d . . . C7 C 0.7082(3) 0.88178(16) 0.33883(11) 0.0299(5) Uani 1 1 d . . . H7A H 0.6383 0.9323 0.3396 0.045 Uiso 1 1 calc R . . H7B H 0.6508 0.8268 0.3318 0.045 Uiso 1 1 calc R . . H7C H 0.7807 0.8892 0.2997 0.045 Uiso 1 1 calc R . . C8 C 1.1508(2) 0.98259(13) 0.49316(11) 0.0205(4) Uani 1 1 d . . . C9 C 1.1144(2) 1.06240(14) 0.54219(11) 0.0247(5) Uani 1 1 d . . . H9A H 1.0379 1.1000 0.5194 0.037 Uiso 1 1 calc R . . H9B H 1.2067 1.0970 0.5503 0.037 Uiso 1 1 calc R . . H9C H 1.0754 1.0407 0.5879 0.037 Uiso 1 1 calc R . . C10 C 1.2104(2) 1.01938(15) 0.42232(12) 0.0286(5) Uani 1 1 d . . . H10A H 1.1329 1.0570 0.4004 0.043 Uiso 1 1 calc R . . H10B H 1.2347 0.9701 0.3902 0.043 Uiso 1 1 calc R . . H10C H 1.3019 1.0546 0.4311 0.043 Uiso 1 1 calc R . . C11 C 1.2786(2) 0.92720(14) 0.52673(12) 0.0248(4) Uani 1 1 d . . . H11A H 1.3662 0.9654 0.5361 0.037 Uiso 1 1 calc R . . H11B H 1.3080 0.8797 0.4939 0.037 Uiso 1 1 calc R . . H11C H 1.2431 0.9012 0.5716 0.037 Uiso 1 1 calc R . . C12 C 0.5472(2) 0.79926(13) 0.61074(11) 0.0216(4) Uani 1 1 d . . . H12A H 0.5315 0.8618 0.5965 0.026 Uiso 1 1 calc R . . H12B H 0.4896 0.7609 0.5776 0.026 Uiso 1 1 calc R . . C13 C 0.4920(2) 0.78518(13) 0.68649(11) 0.0236(4) Uani 1 1 d . . . H13A H 0.5095 0.7226 0.7001 0.028 Uiso 1 1 calc R . . H13B H 0.3816 0.7963 0.6883 0.028 Uiso 1 1 calc R . . C14 C 0.5208(2) 0.96142(13) 0.72001(11) 0.0197(4) Uani 1 1 d . . . C15 C 0.6162(2) 1.01230(13) 0.67603(11) 0.0194(4) Uani 1 1 d . . . C16 C 0.5594(2) 1.09280(13) 0.64756(10) 0.0199(4) Uani 1 1 d . . . C17 C 0.4157(2) 1.11980(13) 0.66929(11) 0.0219(4) Uani 1 1 d . . . H17 H 0.3785 1.1748 0.6519 0.026 Uiso 1 1 calc R . . C18 C 0.3234(2) 1.07096(14) 0.71490(11) 0.0228(4) Uani 1 1 d . . . C19 C 0.3763(2) 0.99032(14) 0.73910(11) 0.0224(4) Uani 1 1 d . . . H19 H 0.3143 0.9544 0.7688 0.027 Uiso 1 1 calc R . . C20 C 0.1681(2) 1.10468(15) 0.73589(12) 0.0296(5) Uani 1 1 d . . . H20A H 0.1736 1.1324 0.7831 0.044 Uiso 1 1 calc R . . H20B H 0.0966 1.0550 0.7373 0.044 Uiso 1 1 calc R . . H20C H 0.1336 1.1485 0.7009 0.044 Uiso 1 1 calc R . . C21 C 0.6513(2) 1.14760(13) 0.59383(11) 0.0227(4) Uani 1 1 d . . . C22 C 0.5630(3) 1.22821(15) 0.56635(13) 0.0329(5) Uani 1 1 d . . . H22A H 0.5360 1.2666 0.6065 0.049 Uiso 1 1 calc R . . H22B H 0.4705 1.2081 0.5424 0.049 Uiso 1 1 calc R . . H22C H 0.6259 1.2614 0.5326 0.049 Uiso 1 1 calc R . . C23 C 0.6899(2) 1.09021(14) 0.52826(11) 0.0247(4) Uani 1 1 d . . . H23A H 0.5960 1.0694 0.5060 0.037 Uiso 1 1 calc R . . H23B H 0.7507 1.0391 0.5432 0.037 Uiso 1 1 calc R . . H23C H 0.7475 1.1257 0.4939 0.037 Uiso 1 1 calc R . . C24 C 0.7965(3) 1.18204(15) 0.62966(13) 0.0299(5) Uani 1 1 d . . . H24A H 0.8547 1.1318 0.6484 0.045 Uiso 1 1 calc R . . H24B H 0.7695 1.2221 0.6688 0.045 Uiso 1 1 calc R . . H24C H 0.8578 1.2142 0.5946 0.045 Uiso 1 1 calc R . . C25 C 0.9712(3) 0.86516(15) 0.76774(11) 0.0284(5) Uani 1 1 d . . . H25A H 0.9512 0.8042 0.7834 0.043 Uiso 1 1 calc R . . H25B H 0.9374 0.9067 0.8046 0.043 Uiso 1 1 calc R . . H25C H 1.0801 0.8728 0.7596 0.043 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 S1 0.0198(2) 0.0171(2) 0.0237(2) 0.00279(19) -0.0018(2) -0.0003(2) S2 0.0257(2) 0.0217(2) 0.0222(2) 0.0051(2) -0.0009(2) -0.00141(19) O1 0.0190(7) 0.0231(7) 0.0193(7) 0.0017(6) -0.0035(6) -0.0001(6) O2 0.0189(7) 0.0188(6) 0.0244(7) 0.0030(5) -0.0002(6) 0.0019(6) Al 0.0193(3) 0.0181(3) 0.0199(3) 0.0028(2) -0.0028(2) 0.0006(2) C1 0.0185(9) 0.0165(9) 0.0198(9) -0.0003(7) -0.0019(8) 0.0058(7) C2 0.0189(9) 0.0160(9) 0.0210(10) 0.0025(8) 0.0007(8) 0.0023(7) C3 0.0206(10) 0.0200(9) 0.0244(10) -0.0022(8) -0.0030(9) -0.0006(8) C4 0.0221(10) 0.0227(10) 0.0210(10) -0.0017(8) -0.0032(8) 0.0047(8) C5 0.0222(10) 0.0194(9) 0.0207(10) 0.0011(8) 0.0001(8) 0.0033(8) C6 0.0187(10) 0.0166(9) 0.0215(10) -0.0016(8) -0.0004(8) 0.0044(8) C7 0.0289(12) 0.0348(12) 0.0258(11) 0.0014(9) -0.0085(9) 0.0021(10) C8 0.0189(9) 0.0213(10) 0.0212(10) 0.0006(8) -0.0012(8) -0.0001(8) C9 0.0254(11) 0.0214(10) 0.0274(11) -0.0011(9) -0.0014(9) -0.0037(8) C10 0.0255(11) 0.0323(12) 0.0279(11) 0.0027(9) 0.0022(9) -0.0037(9) C11 0.0180(10) 0.0272(11) 0.0291(11) 0.0018(9) -0.0018(8) 0.0014(8) C12 0.0173(9) 0.0203(10) 0.0273(11) 0.0003(8) -0.0045(8) -0.0023(7) C13 0.0236(10) 0.0186(10) 0.0287(11) 0.0012(9) 0.0008(9) -0.0042(8) C14 0.0216(10) 0.0179(9) 0.0197(10) 0.0004(8) -0.0026(8) 0.0002(8) C15 0.0207(10) 0.0184(9) 0.0190(9) -0.0023(8) -0.0026(8) -0.0009(7) C16 0.0224(10) 0.0173(9) 0.0199(10) -0.0026(8) -0.0017(8) -0.0004(8) C17 0.0233(10) 0.0175(9) 0.0249(10) -0.0052(8) -0.0042(8) 0.0006(8) C18 0.0212(10) 0.0253(10) 0.0219(10) -0.0073(9) -0.0014(8) 0.0007(8) C19 0.0223(10) 0.0254(10) 0.0194(10) -0.0048(8) 0.0036(8) -0.0041(8) C20 0.0240(11) 0.0312(12) 0.0336(12) -0.0085(10) 0.0020(9) 0.0026(9) C21 0.0234(10) 0.0189(9) 0.0258(11) 0.0022(8) -0.0020(8) 0.0000(8) C22 0.0379(13) 0.0222(11) 0.0386(13) 0.0098(10) 0.0043(11) 0.0050(10) C23 0.0264(10) 0.0234(11) 0.0242(11) 0.0015(8) 0.0015(9) 0.0011(8) C24 0.0291(12) 0.0249(11) 0.0356(12) 0.0004(9) -0.0007(9) -0.0097(9) C25 0.0285(11) 0.0294(11) 0.0274(12) 0.0058(9) -0.0076(9) -0.0031(9) _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 S1 C2 1.778(2) . ? S1 C12 1.815(2) . ? S1 Al 2.4462(8) . ? S2 C14 1.773(2) . ? S2 C13 1.813(2) . ? S2 Al 2.8181(9) . ? O1 C1 1.346(2) . ? O1 Al 1.7866(15) . ? O2 C15 1.342(2) . ? O2 Al 1.7529(14) . ? Al C25 1.943(2) . ? C1 C2 1.399(3) . ? C1 C6 1.417(3) . ? C2 C3 1.387(3) . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.395(3) . ? C4 C7 1.513(3) . ? C5 C6 1.404(3) . ? C5 H5 0.9500 . ? C6 C8 1.528(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.533(3) . ? C8 C11 1.538(3) . ? C8 C9 1.548(3) . ? 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 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.517(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.394(3) . ? C14 C15 1.406(3) . ? C15 C16 1.417(3) . ? C16 C17 1.393(3) . ? C16 C21 1.535(3) . ? C17 C18 1.392(3) . ? C17 H17 0.9500 . ? C18 C19 1.379(3) . ? C18 C20 1.514(3) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.533(3) . ? C21 C24 1.537(3) . ? C21 C23 1.542(3) . ? 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 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 C2 S1 C12 103.19(10) . . ? C2 S1 Al 87.81(7) . . ? C12 S1 Al 102.56(7) . . ? C14 S2 C13 99.73(10) . . ? C14 S2 Al 88.74(7) . . ? C13 S2 Al 100.61(7) . . ? C1 O1 Al 116.75(12) . . ? C15 O2 Al 135.12(13) . . ? O2 Al O1 101.64(7) . . ? O2 Al C25 126.25(9) . . ? O1 Al C25 107.72(9) . . ? O2 Al S1 104.34(5) . . ? O1 Al S1 81.59(5) . . ? C25 Al S1 123.51(7) . . ? O2 Al S2 76.99(5) . . ? O1 Al S2 157.88(5) . . ? C25 Al S2 89.94(7) . . ? S1 Al S2 77.48(2) . . ? O1 C1 C2 118.68(17) . . ? O1 C1 C6 122.38(17) . . ? C2 C1 C6 118.93(18) . . ? C3 C2 C1 122.79(18) . . ? C3 C2 S1 123.04(15) . . ? C1 C2 S1 114.15(15) . . ? C4 C3 C2 119.14(19) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.37(18) . . ? C3 C4 C7 120.72(19) . . ? C5 C4 C7 120.89(19) . . ? C4 C5 C6 124.07(19) . . ? C4 C5 H5 118.0 . . ? C6 C5 H5 118.0 . . ? C5 C6 C1 116.37(18) . . ? C5 C6 C8 122.53(18) . . ? C1 C6 C8 120.96(17) . . ? 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 C10 112.34(17) . . ? C6 C8 C11 111.31(16) . . ? C10 C8 C11 107.41(17) . . ? C6 C8 C9 108.58(16) . . ? C10 C8 C9 107.77(17) . . ? C11 C8 C9 109.33(17) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S1 108.65(14) . . ? C13 C12 H12A 110.0 . . ? S1 C12 H12A 110.0 . . ? C13 C12 H12B 110.0 . . ? S1 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? C12 C13 S2 112.95(14) . . ? C12 C13 H13A 109.0 . . ? S2 C13 H13A 109.0 . . ? C12 C13 H13B 109.0 . . ? S2 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C19 C14 C15 121.86(18) . . ? C19 C14 S2 119.40(16) . . ? C15 C14 S2 118.72(15) . . ? O2 C15 C14 120.38(17) . . ? O2 C15 C16 121.15(18) . . ? C14 C15 C16 118.44(18) . . ? C17 C16 C15 117.50(19) . . ? C17 C16 C21 121.08(18) . . ? C15 C16 C21 121.41(18) . . ? C18 C17 C16 123.95(19) . . ? C18 C17 H17 118.0 . . ? C16 C17 H17 118.0 . . ? C19 C18 C17 118.03(19) . . ? C19 C18 C20 121.1(2) . . ? C17 C18 C20 120.82(19) . . ? C18 C19 C14 120.05(19) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C16 112.23(17) . . ? C22 C21 C24 107.67(18) . . ? C16 C21 C24 109.59(17) . . ? C22 C21 C23 106.79(17) . . ? C16 C21 C23 109.79(16) . . ? C24 C21 C23 110.75(18) . . ? 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 . . ? Al C25 H25A 109.5 . . ? Al C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 C15 O2 Al O1 157.15(17) . . . . ? C15 O2 Al C25 -80.4(2) . . . . ? C15 O2 Al S1 72.97(18) . . . . ? C15 O2 Al S2 -0.25(17) . . . . ? C1 O1 Al O2 -60.46(14) . . . . ? C1 O1 Al C25 165.15(14) . . . . ? C1 O1 Al S1 42.56(12) . . . . ? C1 O1 Al S2 23.6(2) . . . . ? C2 S1 Al O2 65.58(8) . . . . ? C12 S1 Al O2 -37.45(9) . . . . ? C2 S1 Al O1 -34.37(8) . . . . ? C12 S1 Al O1 -137.39(8) . . . . ? C2 S1 Al C25 -140.11(11) . . . . ? C12 S1 Al C25 116.87(11) . . . . ? C2 S1 Al S2 138.43(7) . . . . ? C12 S1 Al S2 35.40(7) . . . . ? C14 S2 Al O2 -0.93(8) . . . . ? C13 S2 Al O2 98.74(8) . . . . ? C14 S2 Al O1 -89.85(16) . . . . ? C13 S2 Al O1 9.82(16) . . . . ? C14 S2 Al C25 126.45(10) . . . . ? C13 S2 Al C25 -133.88(10) . . . . ? C14 S2 Al S1 -109.09(7) . . . . ? C13 S2 Al S1 -9.43(7) . . . . ? Al O1 C1 C2 -35.2(2) . . . . ? Al O1 C1 C6 143.74(15) . . . . ? O1 C1 C2 C3 173.33(17) . . . . ? C6 C1 C2 C3 -5.6(3) . . . . ? O1 C1 C2 S1 -5.0(2) . . . . ? C6 C1 C2 S1 176.08(14) . . . . ? C12 S1 C2 C3 -48.29(19) . . . . ? Al S1 C2 C3 -150.67(17) . . . . ? C12 S1 C2 C1 130.00(15) . . . . ? Al S1 C2 C1 27.61(14) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? S1 C2 C3 C4 179.07(15) . . . . ? C2 C3 C4 C5 3.4(3) . . . . ? C2 C3 C4 C7 -175.25(19) . . . . ? C3 C4 C5 C6 -3.2(3) . . . . ? C7 C4 C5 C6 175.5(2) . . . . ? C4 C5 C6 C1 -1.4(3) . . . . ? C4 C5 C6 C8 -177.24(18) . . . . ? O1 C1 C6 C5 -173.30(17) . . . . ? C2 C1 C6 C5 5.6(3) . . . . ? O1 C1 C6 C8 2.6(3) . . . . ? C2 C1 C6 C8 -178.46(17) . . . . ? C5 C6 C8 C10 -9.2(3) . . . . ? C1 C6 C8 C10 175.14(18) . . . . ? C5 C6 C8 C11 -129.7(2) . . . . ? C1 C6 C8 C11 54.6(2) . . . . ? C5 C6 C8 C9 109.9(2) . . . . ? C1 C6 C8 C9 -65.8(2) . . . . ? C2 S1 C12 C13 -157.76(14) . . . . ? Al S1 C12 C13 -67.07(13) . . . . ? S1 C12 C13 S2 62.27(16) . . . . ? C14 S2 C13 C12 64.68(16) . . . . ? Al S2 C13 C12 -25.86(15) . . . . ? C13 S2 C14 C19 80.32(18) . . . . ? Al S2 C14 C19 -179.13(16) . . . . ? C13 S2 C14 C15 -98.53(17) . . . . ? Al S2 C14 C15 2.02(15) . . . . ? Al O2 C15 C14 1.8(3) . . . . ? Al O2 C15 C16 -176.27(14) . . . . ? C19 C14 C15 O2 178.39(18) . . . . ? S2 C14 C15 O2 -2.8(3) . . . . ? C19 C14 C15 C16 -3.4(3) . . . . ? S2 C14 C15 C16 175.37(15) . . . . ? O2 C15 C16 C17 -177.26(17) . . . . ? C14 C15 C16 C17 4.6(3) . . . . ? O2 C15 C16 C21 3.7(3) . . . . ? C14 C15 C16 C21 -174.40(18) . . . . ? C15 C16 C17 C18 -2.5(3) . . . . ? C21 C16 C17 C18 176.55(18) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C16 C17 C18 C20 -179.79(19) . . . . ? C17 C18 C19 C14 2.4(3) . . . . ? C20 C18 C19 C14 -178.89(18) . . . . ? C15 C14 C19 C18 -0.2(3) . . . . ? S2 C14 C19 C18 -178.98(15) . . . . ? C17 C16 C21 C22 -3.1(3) . . . . ? C15 C16 C21 C22 175.85(19) . . . . ? C17 C16 C21 C24 116.4(2) . . . . ? C15 C16 C21 C24 -64.6(2) . . . . ? C17 C16 C21 C23 -121.7(2) . . . . ? C15 C16 C21 C23 57.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.405 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.055 #===END #================================================================= data_gm2 _database_code_depnum_ccdc_archive 'CCDC 244971' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H37 Al O2 S2' _chemical_formula_weight 472.66 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.952(4) _cell_length_b 15.202(6) _cell_length_c 18.987(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2583.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 248(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.3 _cell_measurement_theta_max 14.6 _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8810 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 248(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 Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15321 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5045 _reflns_number_gt 4305 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction 'XCAD4 (Harms, Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0421P)^2^+0.4353P] 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 noref _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 -0.02(7) _refine_ls_number_reflns 5045 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 S1 S 0.26389(7) 0.22578(4) 0.39397(4) 0.03956(16) Uani 1 1 d . . . S2 S 0.42083(8) 0.14299(4) 0.25106(4) 0.04446(17) Uani 1 1 d . . . O1 O 0.01714(19) 0.11091(11) 0.39196(9) 0.0378(4) Uani 1 1 d . . . O2 O 0.2519(2) 0.01617(10) 0.33805(9) 0.0380(4) Uani 1 1 d . . . Al Al 0.14778(9) 0.11181(5) 0.32098(4) 0.03502(18) Uani 1 1 d . . . C1 C 0.0711(3) 0.11693(15) 0.45794(13) 0.0336(5) Uani 1 1 d . . . C2 C 0.0064(3) 0.07314(15) 0.51510(13) 0.0348(5) Uani 1 1 d . . . C3 C 0.0813(3) 0.07863(16) 0.57959(14) 0.0388(6) Uani 1 1 d . . . H3 H 0.0396 0.0493 0.6185 0.047 Uiso 1 1 calc R . . C4 C 0.2142(3) 0.12507(16) 0.58971(14) 0.0410(6) Uani 1 1 d . . . C5 C 0.2712(3) 0.17233(16) 0.53405(14) 0.0399(6) Uani 1 1 d . . . H5 H 0.3573 0.2070 0.5398 0.048 Uiso 1 1 calc R . . C6 C 0.1997(3) 0.16803(15) 0.46948(14) 0.0344(5) Uani 1 1 d . . . C7 C 0.2946(4) 0.1237(2) 0.65947(15) 0.0593(8) Uani 1 1 d . . . H7A H 0.3695 0.0777 0.6591 0.089 Uiso 1 1 calc R . . H7B H 0.2234 0.1125 0.6969 0.089 Uiso 1 1 calc R . . H7C H 0.3425 0.1801 0.6673 0.089 Uiso 1 1 calc R . . C8 C -0.1379(3) 0.01915(16) 0.50619(14) 0.0390(6) Uani 1 1 d . . . C9 C -0.1039(3) -0.06041(18) 0.45831(16) 0.0493(7) Uani 1 1 d . . . H9A H -0.0286 -0.0971 0.4804 0.074 Uiso 1 1 calc R . . H9B H -0.0673 -0.0398 0.4132 0.074 Uiso 1 1 calc R . . H9C H -0.1944 -0.0944 0.4513 0.074 Uiso 1 1 calc R . . C10 C -0.1963(4) -0.0160(2) 0.57618(18) 0.0590(8) Uani 1 1 d . . . H10A H -0.1213 -0.0534 0.5976 0.089 Uiso 1 1 calc R . . H10B H -0.2867 -0.0497 0.5681 0.089 Uiso 1 1 calc R . . H10C H -0.2182 0.0329 0.6074 0.089 Uiso 1 1 calc R . . C11 C -0.2622(3) 0.07415(19) 0.47252(17) 0.0511(7) Uani 1 1 d . . . H11A H -0.3520 0.0388 0.4683 0.077 Uiso 1 1 calc R . . H11B H -0.2308 0.0934 0.4261 0.077 Uiso 1 1 calc R . . H11C H -0.2826 0.1251 0.5018 0.077 Uiso 1 1 calc R . . C12 C 0.4610(3) 0.19727(17) 0.38937(16) 0.0424(6) Uani 1 1 d . . . H12A H 0.5181 0.2339 0.4223 0.051 Uiso 1 1 calc R . . H12B H 0.4750 0.1355 0.4026 0.051 Uiso 1 1 calc R . . C13 C 0.5161(3) 0.21204(17) 0.31513(16) 0.0470(7) Uani 1 1 d . . . H13A H 0.6235 0.1999 0.3132 0.056 Uiso 1 1 calc R . . H13B H 0.5012 0.2739 0.3025 0.056 Uiso 1 1 calc R . . C14 C 0.4842(3) 0.03802(16) 0.27913(13) 0.0375(6) Uani 1 1 d . . . C15 C 0.3889(3) -0.01214(15) 0.32192(13) 0.0339(5) Uani 1 1 d . . . C16 C 0.4448(3) -0.09236(15) 0.34960(13) 0.0353(6) Uani 1 1 d . . . C17 C 0.5872(3) -0.11885(16) 0.32742(14) 0.0425(6) Uani 1 1 d . . . H17 H 0.6234 -0.1730 0.3442 0.051 Uiso 1 1 calc R . . C18 C 0.6786(3) -0.07113(19) 0.28270(15) 0.0442(6) Uani 1 1 d . . . C19 C 0.6259(3) 0.00960(18) 0.25939(15) 0.0425(6) Uani 1 1 d . . . H19 H 0.6859 0.0451 0.2303 0.051 Uiso 1 1 calc R . . C20 C 0.8326(4) -0.1043(2) 0.26122(18) 0.0613(8) Uani 1 1 d . . . H20A H 0.8358 -0.1122 0.2106 0.092 Uiso 1 1 calc R . . H20B H 0.8523 -0.1601 0.2843 0.092 Uiso 1 1 calc R . . H20C H 0.9077 -0.0618 0.2752 0.092 Uiso 1 1 calc R . . C21 C 0.3547(3) -0.14627(16) 0.40283(15) 0.0431(6) Uani 1 1 d . . . C22 C 0.4425(4) -0.2261(2) 0.43015(19) 0.0673(10) Uani 1 1 d . . . H22A H 0.4639 -0.2656 0.3913 0.101 Uiso 1 1 calc R . . H22B H 0.3836 -0.2567 0.4653 0.101 Uiso 1 1 calc R . . H22C H 0.5355 -0.2063 0.4511 0.101 Uiso 1 1 calc R . . C23 C 0.3176(4) -0.08903(18) 0.46708(15) 0.0479(7) Uani 1 1 d . . . H23A H 0.4095 -0.0687 0.4887 0.072 Uiso 1 1 calc R . . H23B H 0.2611 -0.1234 0.5009 0.072 Uiso 1 1 calc R . . H23C H 0.2587 -0.0388 0.4522 0.072 Uiso 1 1 calc R . . C24 C 0.2105(4) -0.1794(2) 0.36828(17) 0.0580(8) Uani 1 1 d . . . H24A H 0.1564 -0.1301 0.3483 0.087 Uiso 1 1 calc R . . H24B H 0.1487 -0.2082 0.4034 0.087 Uiso 1 1 calc R . . H24C H 0.2350 -0.2210 0.3313 0.087 Uiso 1 1 calc R . . C25 C 0.0276(3) 0.1400(2) 0.23858(15) 0.0502(7) Uani 1 1 d . . . H25A H -0.0610 0.1022 0.2408 0.060 Uiso 1 1 calc R . . H25B H -0.0078 0.2004 0.2451 0.060 Uiso 1 1 calc R . . C26 C 0.0852(5) 0.1343(3) 0.16389(17) 0.0769(11) Uani 1 1 d . . . H26A H 0.1564 0.1813 0.1556 0.115 Uiso 1 1 calc R . . H26B H 0.0024 0.1399 0.1312 0.115 Uiso 1 1 calc R . . H26C H 0.1339 0.0779 0.1569 0.115 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 S1 0.0389(4) 0.0312(3) 0.0486(4) 0.0051(3) -0.0055(3) -0.0026(3) S2 0.0464(4) 0.0451(4) 0.0419(4) 0.0132(3) -0.0028(3) -0.0053(3) O1 0.0334(9) 0.0445(9) 0.0354(9) 0.0027(8) -0.0075(8) -0.0026(8) O2 0.0344(9) 0.0346(8) 0.0450(11) 0.0088(7) 0.0008(8) -0.0004(8) Al 0.0360(4) 0.0340(4) 0.0350(4) 0.0074(3) -0.0062(3) -0.0017(3) C1 0.0358(13) 0.0299(11) 0.0352(13) 0.0005(10) -0.0052(11) 0.0067(10) C2 0.0391(14) 0.0299(11) 0.0353(13) -0.0018(10) -0.0018(11) 0.0052(10) C3 0.0454(14) 0.0353(12) 0.0358(13) 0.0020(10) -0.0009(12) 0.0065(11) C4 0.0449(16) 0.0392(13) 0.0388(15) -0.0051(11) -0.0123(12) 0.0107(11) C5 0.0347(14) 0.0355(12) 0.0495(16) -0.0086(11) -0.0090(13) 0.0042(11) C6 0.0349(13) 0.0285(11) 0.0398(14) 0.0005(10) -0.0054(11) 0.0024(10) C7 0.062(2) 0.071(2) 0.0454(17) -0.0058(14) -0.0187(15) 0.0089(16) C8 0.0381(14) 0.0383(13) 0.0405(15) 0.0020(11) 0.0011(12) -0.0001(11) C9 0.0546(19) 0.0401(14) 0.0532(18) -0.0036(12) 0.0005(15) -0.0115(13) C10 0.056(2) 0.067(2) 0.0547(19) 0.0090(15) 0.0072(16) -0.0108(15) C11 0.0369(15) 0.0526(15) 0.0638(19) 0.0046(13) -0.0057(15) -0.0017(13) C12 0.0342(14) 0.0414(14) 0.0515(16) 0.0029(12) -0.0089(13) -0.0055(11) C13 0.0405(15) 0.0365(14) 0.0639(19) 0.0067(13) 0.0036(14) -0.0101(11) C14 0.0399(14) 0.0396(13) 0.0329(13) 0.0028(10) -0.0050(12) -0.0060(11) C15 0.0369(14) 0.0342(12) 0.0306(12) -0.0025(10) -0.0057(11) -0.0042(10) C16 0.0387(14) 0.0318(12) 0.0356(13) -0.0058(9) -0.0033(11) -0.0018(10) C17 0.0487(16) 0.0355(13) 0.0434(15) -0.0096(11) -0.0045(13) 0.0034(12) C18 0.0388(15) 0.0524(16) 0.0413(15) -0.0155(12) 0.0000(12) -0.0016(12) C19 0.0428(15) 0.0509(15) 0.0338(14) -0.0041(11) 0.0015(12) -0.0104(12) C20 0.0546(19) 0.069(2) 0.060(2) -0.0161(16) 0.0057(16) 0.0101(16) C21 0.0513(16) 0.0315(12) 0.0464(16) 0.0040(11) -0.0018(14) 0.0019(12) C22 0.085(2) 0.0444(16) 0.072(2) 0.0207(15) 0.016(2) 0.0162(17) C23 0.0581(18) 0.0446(15) 0.0411(15) 0.0050(11) 0.0007(14) 0.0034(13) C24 0.064(2) 0.0501(16) 0.060(2) 0.0020(14) 0.0021(16) -0.0203(15) C25 0.0457(16) 0.0550(16) 0.0499(18) 0.0150(14) -0.0166(14) -0.0052(13) C26 0.092(3) 0.094(3) 0.0444(19) -0.0011(17) -0.020(2) 0.021(2) _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 S1 C6 1.777(3) . ? S1 C12 1.819(3) . ? S1 Al 2.4501(11) . ? S2 C14 1.775(3) . ? S2 C13 1.819(3) . ? S2 Al 2.8217(14) . ? O1 C1 1.346(3) . ? O1 Al 1.784(2) . ? O2 C15 1.336(3) . ? O2 Al 1.7572(18) . ? Al C25 1.947(3) . ? C1 C2 1.399(4) . ? C1 C6 1.405(4) . ? C2 C3 1.398(4) . ? C2 C8 1.539(4) . ? C3 C4 1.397(4) . ? C3 H3 0.9400 . ? C4 C5 1.376(4) . ? C4 C7 1.507(4) . ? C5 C6 1.385(4) . ? C5 H5 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C10 1.525(4) . ? C8 C11 1.532(4) . ? C8 C9 1.543(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.510(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C19 1.392(4) . ? C14 C15 1.403(4) . ? C15 C16 1.419(3) . ? C16 C17 1.402(4) . ? C16 C21 1.531(4) . ? C17 C18 1.384(4) . ? C17 H17 0.9400 . ? C18 C19 1.387(4) . ? C18 C20 1.524(4) . ? C19 H19 0.9400 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C24 1.534(4) . ? C21 C23 1.535(4) . ? C21 C22 1.536(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.512(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? 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 C6 S1 C12 103.58(13) . . ? C6 S1 Al 88.26(9) . . ? C12 S1 Al 102.47(10) . . ? C14 S2 C13 99.68(13) . . ? C14 S2 Al 89.10(10) . . ? C13 S2 Al 100.86(10) . . ? C1 O1 Al 117.85(16) . . ? C15 O2 Al 135.36(16) . . ? O2 Al O1 101.66(9) . . ? O2 Al C25 128.57(12) . . ? O1 Al C25 104.26(12) . . ? O2 Al S1 104.82(7) . . ? O1 Al S1 81.73(7) . . ? C25 Al S1 122.24(10) . . ? O2 Al S2 76.48(7) . . ? O1 Al S2 157.57(7) . . ? C25 Al S2 93.66(10) . . ? S1 Al S2 77.28(4) . . ? O1 C1 C2 122.7(2) . . ? O1 C1 C6 118.5(2) . . ? C2 C1 C6 118.8(2) . . ? C3 C2 C1 116.9(2) . . ? C3 C2 C8 122.0(2) . . ? C1 C2 C8 121.1(2) . . ? C4 C3 C2 124.0(3) . . ? C4 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C5 C4 C3 118.3(2) . . ? C5 C4 C7 120.3(3) . . ? C3 C4 C7 121.4(3) . . ? C4 C5 C6 118.9(2) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C1 122.9(2) . . ? C5 C6 S1 122.8(2) . . ? C1 C6 S1 114.34(19) . . ? 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 . . ? C10 C8 C11 107.8(2) . . ? C10 C8 C2 112.3(2) . . ? C11 C8 C2 111.4(2) . . ? C10 C8 C9 107.9(2) . . ? C11 C8 C9 109.0(2) . . ? C2 C8 C9 108.5(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S1 109.0(2) . . ? C13 C12 H12A 109.9 . . ? S1 C12 H12A 109.9 . . ? C13 C12 H12B 109.9 . . ? S1 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C12 C13 S2 112.66(18) . . ? C12 C13 H13A 109.1 . . ? S2 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? S2 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C19 C14 C15 122.8(2) . . ? C19 C14 S2 119.3(2) . . ? C15 C14 S2 117.9(2) . . ? O2 C15 C14 121.1(2) . . ? O2 C15 C16 121.0(2) . . ? C14 C15 C16 117.9(2) . . ? C17 C16 C15 117.1(2) . . ? C17 C16 C21 121.6(2) . . ? C15 C16 C21 121.3(2) . . ? C18 C17 C16 124.8(3) . . ? C18 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? C17 C18 C19 117.3(3) . . ? C17 C18 C20 121.7(3) . . ? C19 C18 C20 121.0(3) . . ? C18 C19 C14 119.9(3) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 C24 109.7(2) . . ? C16 C21 C23 109.6(2) . . ? C24 C21 C23 110.1(3) . . ? C16 C21 C22 112.1(2) . . ? C24 C21 C22 108.4(2) . . ? C23 C21 C22 106.9(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 . . ? C26 C25 Al 123.5(2) . . ? C26 C25 H25A 106.4 . . ? Al C25 H25A 106.4 . . ? C26 C25 H25B 106.4 . . ? Al C25 H25B 106.4 . . ? H25A C25 H25B 106.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 C15 O2 Al O1 -156.0(2) . . . . ? C15 O2 Al C25 84.9(3) . . . . ? C15 O2 Al S1 -71.6(2) . . . . ? C15 O2 Al S2 1.0(2) . . . . ? C1 O1 Al O2 62.46(17) . . . . ? C1 O1 Al C25 -162.35(17) . . . . ? C1 O1 Al S1 -41.06(15) . . . . ? C1 O1 Al S2 -20.3(3) . . . . ? C6 S1 Al O2 -66.95(10) . . . . ? C12 S1 Al O2 36.58(12) . . . . ? C6 S1 Al O1 33.00(10) . . . . ? C12 S1 Al O1 136.53(11) . . . . ? C6 S1 Al C25 134.69(14) . . . . ? C12 S1 Al C25 -121.78(15) . . . . ? C6 S1 Al S2 -139.04(8) . . . . ? C12 S1 Al S2 -35.51(10) . . . . ? C14 S2 Al O2 0.68(10) . . . . ? C13 S2 Al O2 -99.00(11) . . . . ? C14 S2 Al O1 88.52(19) . . . . ? C13 S2 Al O1 -11.2(2) . . . . ? C14 S2 Al C25 -128.17(13) . . . . ? C13 S2 Al C25 132.15(13) . . . . ? C14 S2 Al S1 109.58(9) . . . . ? C13 S2 Al S1 9.90(9) . . . . ? Al O1 C1 C2 -144.9(2) . . . . ? Al O1 C1 C6 33.8(3) . . . . ? O1 C1 C2 C3 174.4(2) . . . . ? C6 C1 C2 C3 -4.3(3) . . . . ? O1 C1 C2 C8 -3.6(4) . . . . ? C6 C1 C2 C8 177.6(2) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C8 C2 C3 C4 178.4(2) . . . . ? C2 C3 C4 C5 3.7(4) . . . . ? C2 C3 C4 C7 -176.1(3) . . . . ? C3 C4 C5 C6 -3.6(3) . . . . ? C7 C4 C5 C6 176.2(2) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C4 C5 C6 S1 -179.67(19) . . . . ? O1 C1 C6 C5 -174.3(2) . . . . ? C2 C1 C6 C5 4.5(4) . . . . ? O1 C1 C6 S1 5.1(3) . . . . ? C2 C1 C6 S1 -176.15(18) . . . . ? C12 S1 C6 C5 50.3(2) . . . . ? Al S1 C6 C5 152.7(2) . . . . ? C12 S1 C6 C1 -129.07(19) . . . . ? Al S1 C6 C1 -26.66(17) . . . . ? C3 C2 C8 C10 7.2(3) . . . . ? C1 C2 C8 C10 -174.8(2) . . . . ? C3 C2 C8 C11 128.2(3) . . . . ? C1 C2 C8 C11 -53.9(3) . . . . ? C3 C2 C8 C9 -111.9(3) . . . . ? C1 C2 C8 C9 66.1(3) . . . . ? C6 S1 C12 C13 158.64(17) . . . . ? Al S1 C12 C13 67.40(17) . . . . ? S1 C12 C13 S2 -61.9(2) . . . . ? C14 S2 C13 C12 -65.7(2) . . . . ? Al S2 C13 C12 25.2(2) . . . . ? C13 S2 C14 C19 -79.9(2) . . . . ? Al S2 C14 C19 179.2(2) . . . . ? C13 S2 C14 C15 98.8(2) . . . . ? Al S2 C14 C15 -2.11(19) . . . . ? Al O2 C15 C14 -3.0(4) . . . . ? Al O2 C15 C16 174.68(18) . . . . ? C19 C14 C15 O2 -178.0(2) . . . . ? S2 C14 C15 O2 3.4(3) . . . . ? C19 C14 C15 C16 4.3(4) . . . . ? S2 C14 C15 C16 -174.36(18) . . . . ? O2 C15 C16 C17 177.3(2) . . . . ? C14 C15 C16 C17 -5.0(3) . . . . ? O2 C15 C16 C21 -4.2(4) . . . . ? C14 C15 C16 C21 173.5(2) . . . . ? C15 C16 C17 C18 2.3(4) . . . . ? C21 C16 C17 C18 -176.1(2) . . . . ? C16 C17 C18 C19 1.4(4) . . . . ? C16 C17 C18 C20 179.8(2) . . . . ? C17 C18 C19 C14 -2.3(4) . . . . ? C20 C18 C19 C14 179.3(2) . . . . ? C15 C14 C19 C18 -0.5(4) . . . . ? S2 C14 C19 C18 178.1(2) . . . . ? C17 C16 C21 C24 -117.2(3) . . . . ? C15 C16 C21 C24 64.4(3) . . . . ? C17 C16 C21 C23 121.8(3) . . . . ? C15 C16 C21 C23 -56.6(3) . . . . ? C17 C16 C21 C22 3.3(4) . . . . ? C15 C16 C21 C22 -175.1(3) . . . . ? O2 Al C25 C26 -52.1(3) . . . . ? O1 Al C25 C26 -170.1(3) . . . . ? S1 Al C25 C26 100.8(3) . . . . ? S2 Al C25 C26 23.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.287 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.047 #============================================================================== #===END data_hm11 _database_code_depnum_ccdc_archive 'CCDC 244972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H39 Al O2 S2' _chemical_formula_weight 534.72 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C mc21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.001(2) _cell_length_b 17.967(2) _cell_length_c 10.0090(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3057.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20943 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 28.33 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9006 _exptl_absorpt_correction_T_max 0.9776 _exptl_absorpt_process_details 'Bruker area detector absorption detection' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ; Bruker AXS diffractometer with CCD area detector ; _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20943 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3933 _reflns_number_gt 3664 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction 'SAINT, SADABS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0442P)^2^+0.9481P] 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 noref _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 0.09(8) _refine_ls_number_reflns 3933 _refine_ls_number_parameters 177 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 S S 0.39733(2) 0.93497(2) 0.13957(5) 0.02048(10) Uani 1 1 d . . . O O 0.42338(7) 0.77712(7) 0.08960(14) 0.0231(3) Uani 1 1 d . . . Al Al 0.5000 0.82712(4) 0.16539(7) 0.01619(16) Uani 1 2 d S . . C1 C 0.34810(10) 0.79628(10) 0.07295(18) 0.0189(4) Uani 1 1 d . . . C2 C 0.32424(10) 0.86989(10) 0.09434(19) 0.0196(4) Uani 1 1 d . . . C3 C 0.24688(11) 0.89300(11) 0.0751(2) 0.0230(4) Uani 1 1 d . . . H3 H 0.2324 0.9432 0.0920 0.028 Uiso 1 1 calc R . . C4 C 0.19147(11) 0.84251(12) 0.0312(2) 0.0251(4) Uani 1 1 d . . . C5 C 0.21510(11) 0.76937(12) 0.0094(2) 0.0244(4) Uani 1 1 d . . . H5 H 0.1768 0.7349 -0.0213 0.029 Uiso 1 1 calc R . . C6 C 0.29140(11) 0.74357(10) 0.03000(19) 0.0202(4) Uani 1 1 d . . . C7 C 0.10662(12) 0.86621(13) 0.0104(3) 0.0355(5) Uani 1 1 d . . . H7A H 0.0752 0.8513 0.0880 0.053 Uiso 1 1 calc R . . H7B H 0.0857 0.8422 -0.0701 0.053 Uiso 1 1 calc R . . H7C H 0.1042 0.9204 -0.0001 0.053 Uiso 1 1 calc R . . C8 C 0.31486(12) 0.66229(11) 0.0051(2) 0.0254(4) Uani 1 1 d . . . C9 C 0.34764(13) 0.62799(11) 0.1342(2) 0.0358(5) Uani 1 1 d . . . H9A H 0.3958 0.6542 0.1601 0.054 Uiso 1 1 calc R . . H9B H 0.3595 0.5753 0.1192 0.054 Uiso 1 1 calc R . . H9C H 0.3085 0.6326 0.2056 0.054 Uiso 1 1 calc R . . C10 C 0.24406(14) 0.61516(12) -0.0382(2) 0.0330(5) Uani 1 1 d . . . H10A H 0.2037 0.6166 0.0317 0.049 Uiso 1 1 calc R . . H10B H 0.2609 0.5636 -0.0525 0.049 Uiso 1 1 calc R . . H10C H 0.2223 0.6352 -0.1214 0.049 Uiso 1 1 calc R . . C11 C 0.37624(14) 0.65868(13) -0.1072(3) 0.0343(5) Uani 1 1 d . . . H11A H 0.3533 0.6781 -0.1900 0.051 Uiso 1 1 calc R . . H11B H 0.3925 0.6069 -0.1207 0.051 Uiso 1 1 calc R . . H11C H 0.4221 0.6888 -0.0826 0.051 Uiso 1 1 calc R . . C12 C 0.41321(11) 0.97952(10) -0.0246(2) 0.0237(4) Uani 1 1 d . . . H12A H 0.3616 0.9914 -0.0652 0.028 Uiso 1 1 calc R . . H12B H 0.4420 1.0269 -0.0117 0.028 Uiso 1 1 calc R . . C13 C 0.45851(11) 0.93095(10) -0.11726(19) 0.0214(4) Uani 1 1 d . . . C14 C 0.41881(12) 0.88282(11) -0.2028(2) 0.0262(4) Uani 1 1 d . . . H14 H 0.3629 0.8832 -0.2045 0.031 Uiso 1 1 calc R . . C15 C 0.45916(14) 0.83463(12) -0.2850(2) 0.0316(5) Uani 1 1 d . . . H15 H 0.4312 0.8015 -0.3416 0.038 Uiso 1 1 calc R . . C16 C 0.5000 0.82386(17) 0.3600(3) 0.0269(6) Uani 1 2 d S . . H16A H 0.5000 0.771(2) 0.383(4) 0.054(12) Uiso 1 2 d S . . H16B H 0.5483(15) 0.8470(15) 0.396(3) 0.039(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S 0.01759(18) 0.02007(19) 0.0238(2) -0.00420(19) 0.00113(19) -0.00041(16) O 0.0152(6) 0.0219(6) 0.0321(7) -0.0078(6) -0.0044(5) 0.0006(5) Al 0.0151(3) 0.0169(3) 0.0165(4) -0.0025(3) 0.000 0.000 C1 0.0168(8) 0.0238(9) 0.0163(8) -0.0014(7) -0.0007(7) -0.0004(7) C2 0.0175(8) 0.0219(8) 0.0192(8) -0.0013(7) 0.0002(7) -0.0029(7) C3 0.0203(9) 0.0259(9) 0.0227(9) 0.0016(8) 0.0029(7) 0.0021(7) C4 0.0128(9) 0.0369(11) 0.0256(10) 0.0024(9) -0.0007(7) -0.0010(7) C5 0.0192(9) 0.0316(10) 0.0224(9) 0.0029(8) -0.0020(7) -0.0071(7) C6 0.0189(8) 0.0215(9) 0.0200(9) -0.0011(7) 0.0000(7) -0.0035(7) C7 0.0169(9) 0.0459(13) 0.0437(13) 0.0016(11) -0.0035(9) 0.0015(9) C8 0.0260(10) 0.0227(10) 0.0276(10) -0.0019(8) -0.0047(8) -0.0058(8) C9 0.0446(12) 0.0246(9) 0.0382(12) 0.0030(10) -0.0128(12) -0.0021(8) C10 0.0340(12) 0.0278(10) 0.0371(13) -0.0060(9) -0.0037(10) -0.0099(9) C11 0.0321(11) 0.0299(11) 0.0408(12) -0.0122(10) 0.0037(10) -0.0039(9) C12 0.0199(9) 0.0195(9) 0.0318(10) 0.0062(8) 0.0027(8) 0.0014(7) C13 0.0216(10) 0.0201(9) 0.0225(9) 0.0082(7) 0.0003(8) -0.0003(7) C14 0.0260(10) 0.0292(10) 0.0234(10) 0.0073(8) -0.0043(8) -0.0035(8) C15 0.0456(13) 0.0309(11) 0.0182(8) 0.0009(8) -0.0071(9) -0.0059(9) C16 0.0363(17) 0.0227(14) 0.0216(14) 0.0008(11) 0.000 0.000 _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 S C2 1.7652(18) . ? S C12 1.848(2) . ? S Al 2.6209(7) . ? O C1 1.336(2) . ? O Al 1.7549(13) . ? Al O 1.7549(13) 3_655 ? Al C16 1.948(3) . ? Al S 2.6209(7) 3_655 ? C1 C2 1.400(2) . ? C1 C6 1.418(2) . ? C2 C3 1.393(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 C7 1.518(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C8 1.534(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.534(3) . ? C8 C11 1.535(3) . ? C8 C9 1.536(3) . ? 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 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.488(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.391(3) . ? C13 C13 1.411(4) 3_655 ? C14 C15 1.377(3) . ? C14 H14 0.9500 . ? C15 C15 1.389(5) 3_655 ? C15 H15 0.9500 . ? C16 H16A 0.99(4) . ? C16 H16B 0.99(3) . ? 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 C2 S C12 99.31(9) . . ? C2 S Al 90.25(6) . . ? C12 S Al 108.10(6) . . ? C1 O Al 129.29(12) . . ? O Al O 95.86(9) . 3_655 ? O Al C16 114.63(8) . . ? O Al C16 114.63(8) 3_655 . ? O Al S 80.88(4) . . ? O Al S 146.13(6) 3_655 . ? C16 Al S 96.93(7) . . ? O Al S 146.13(6) . 3_655 ? O Al S 80.88(4) 3_655 3_655 ? C16 Al S 96.93(7) . 3_655 ? S Al S 83.52(3) . 3_655 ? O C1 C2 120.14(16) . . ? O C1 C6 121.12(16) . . ? C2 C1 C6 118.71(16) . . ? C3 C2 C1 122.29(17) . . ? C3 C2 S 120.18(14) . . ? C1 C2 S 117.46(13) . . ? C4 C3 C2 119.53(18) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.28(17) . . ? C3 C4 C7 120.53(19) . . ? C5 C4 C7 121.18(18) . . ? C4 C5 C6 124.07(18) . . ? C4 C5 H5 118.0 . . ? C6 C5 H5 118.0 . . ? C5 C6 C1 117.10(17) . . ? C5 C6 C8 122.34(17) . . ? C1 C6 C8 120.55(16) . . ? 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 . . ? C10 C8 C6 111.55(17) . . ? C10 C8 C11 107.66(17) . . ? C6 C8 C11 109.64(17) . . ? C10 C8 C9 107.49(16) . . ? C6 C8 C9 109.84(17) . . ? C11 C8 C9 110.63(18) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S 112.08(12) . . ? C13 C12 H12A 109.2 . . ? S C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? S C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C13 119.02(12) . 3_655 ? C14 C13 C12 119.79(17) . . ? C13 C13 C12 121.16(10) 3_655 . ? C15 C14 C13 121.10(19) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C15 119.87(12) . 3_655 ? C14 C15 H15 120.1 . . ? C15 C15 H15 120.1 3_655 . ? Al C16 H16A 105(2) . . ? Al C16 H16B 110.4(15) . . ? H16A C16 H16B 109(2) . . ? 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 C1 O Al O -160.24(13) . . . 3_655 ? C1 O Al C16 79.23(19) . . . . ? C1 O Al S -14.26(16) . . . . ? C1 O Al S -77.88(19) . . . 3_655 ? C2 S Al O 10.18(8) . . . . ? C12 S Al O -89.70(8) . . . . ? C2 S Al O 97.11(11) . . . 3_655 ? C12 S Al O -2.77(11) . . . 3_655 ? C2 S Al C16 -103.75(9) . . . . ? C12 S Al C16 156.37(9) . . . . ? C2 S Al S 160.01(6) . . . 3_655 ? C12 S Al S 60.14(7) . . . 3_655 ? Al O C1 C2 12.8(3) . . . . ? Al O C1 C6 -168.93(14) . . . . ? O C1 C2 C3 178.36(17) . . . . ? C6 C1 C2 C3 0.1(3) . . . . ? O C1 C2 S 1.4(2) . . . . ? C6 C1 C2 S -176.88(14) . . . . ? C12 S C2 C3 -76.75(17) . . . . ? Al S C2 C3 174.86(16) . . . . ? C12 S C2 C1 100.28(16) . . . . ? Al S C2 C1 -8.11(15) . . . . ? C1 C2 C3 C4 -1.2(3) . . . . ? S C2 C3 C4 175.73(15) . . . . ? C2 C3 C4 C5 0.9(3) . . . . ? C2 C3 C4 C7 179.54(19) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C7 C4 C5 C6 -178.22(19) . . . . ? C4 C5 C6 C1 -1.4(3) . . . . ? C4 C5 C6 C8 179.84(19) . . . . ? O C1 C6 C5 -177.10(17) . . . . ? C2 C1 C6 C5 1.2(3) . . . . ? O C1 C6 C8 1.6(3) . . . . ? C2 C1 C6 C8 179.91(17) . . . . ? C5 C6 C8 C10 -2.3(3) . . . . ? C1 C6 C8 C10 178.99(18) . . . . ? C5 C6 C8 C11 116.8(2) . . . . ? C1 C6 C8 C11 -61.8(2) . . . . ? C5 C6 C8 C9 -121.4(2) . . . . ? C1 C6 C8 C9 59.9(2) . . . . ? C2 S C12 C13 -74.47(15) . . . . ? Al S C12 C13 18.86(15) . . . . ? S C12 C13 C14 91.44(19) . . . . ? S C12 C13 C13 -86.51(12) . . . 3_655 ? C13 C13 C14 C15 1.2(2) 3_655 . . . ? C12 C13 C14 C15 -176.82(18) . . . . ? C13 C14 C15 C15 -1.2(2) . . . 3_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.359 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.055 #============================================================================== data_gm1 _database_code_depnum_ccdc_archive 'CCDC 248947' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H70 Al2 O4 S4' _chemical_formula_weight 917.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Al Al 0.0640 0.0510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 10.7048(17) _cell_length_b 16.380(3) _cell_length_c 28.722(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5036.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 50262 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 28.32 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8573 _exptl_absorpt_correction_T_max 0.9248 _exptl_absorpt_process_details 'Bruker area detector absorption detection' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker AXS diffractometer with CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50262 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6270 _reflns_number_gt 5520 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction 'SAINT, SADABS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows, Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0611P)^2^+2.2698P] 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 6270 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Al Al -0.03725(4) 0.64120(3) 0.362317(15) 0.01908(11) Uani 1 1 d . . . O1 O -0.08788(9) 0.66552(6) 0.30552(3) 0.0209(2) Uani 1 1 d . . . O2 O -0.08725(9) 0.67763(6) 0.41748(3) 0.0198(2) Uani 1 1 d . . . S1 S 0.08427(3) 0.77529(2) 0.352761(12) 0.02002(9) Uani 1 1 d . . . S2 S -0.24885(3) 0.56548(2) 0.369066(11) 0.01834(9) Uani 1 1 d . . . C1 C -0.01992(13) 0.70947(8) 0.27513(5) 0.0198(3) Uani 1 1 d . . . C2 C 0.06238(13) 0.76961(8) 0.29167(5) 0.0198(3) Uani 1 1 d . . . C3 C 0.12939(14) 0.82001(8) 0.26150(5) 0.0231(3) Uani 1 1 d . . . H3 H 0.1851 0.8599 0.2736 0.028 Uiso 1 1 calc R . . C4 C 0.11436(14) 0.81170(9) 0.21411(5) 0.0258(3) Uani 1 1 d . . . C5 C 0.03686(15) 0.74920(10) 0.19785(5) 0.0270(3) Uani 1 1 d . . . H5 H 0.0289 0.7425 0.1651 0.032 Uiso 1 1 calc R . . C6 C -0.02941(14) 0.69610(9) 0.22654(5) 0.0236(3) Uani 1 1 d . . . C7 C 0.18056(17) 0.86769(11) 0.18051(6) 0.0344(4) Uani 1 1 d . . . H7A H 0.1191 0.9019 0.1645 0.052 Uiso 1 1 calc R . . H7B H 0.2264 0.8350 0.1576 0.052 Uiso 1 1 calc R . . H7C H 0.2392 0.9025 0.1976 0.052 Uiso 1 1 calc R . . C8 C -0.10485(17) 0.62418(10) 0.20689(5) 0.0309(4) Uani 1 1 d . . . C9 C -0.1004(2) 0.62125(14) 0.15353(6) 0.0518(6) Uani 1 1 d . . . H9A H -0.0132 0.6182 0.1432 0.078 Uiso 1 1 calc R . . H9B H -0.1392 0.6706 0.1408 0.078 Uiso 1 1 calc R . . H9C H -0.1459 0.5731 0.1425 0.078 Uiso 1 1 calc R . . C10 C -0.0475(2) 0.54428(11) 0.22480(7) 0.0441(5) Uani 1 1 d . . . H10A H 0.0396 0.5405 0.2146 0.066 Uiso 1 1 calc R . . H10B H -0.0948 0.4979 0.2124 0.066 Uiso 1 1 calc R . . H10C H -0.0509 0.5434 0.2589 0.066 Uiso 1 1 calc R . . C11 C -0.24246(19) 0.62835(13) 0.22143(7) 0.0434(5) Uani 1 1 d . . . H11A H -0.2881 0.5827 0.2074 0.065 Uiso 1 1 calc R . . H11B H -0.2786 0.6801 0.2108 0.065 Uiso 1 1 calc R . . H11C H -0.2486 0.6249 0.2554 0.065 Uiso 1 1 calc R . . C12 C -0.01852(13) 0.85979(8) 0.36945(5) 0.0201(3) Uani 1 1 d . . . H12A H -0.0126 0.8682 0.4035 0.024 Uiso 1 1 calc R . . H12B H 0.0108 0.9104 0.3541 0.024 Uiso 1 1 calc R . . C13 C -0.14694(13) 0.62786(8) 0.44757(5) 0.0183(3) Uani 1 1 d . . . C14 C -0.23424(13) 0.57149(8) 0.43030(5) 0.0183(3) Uani 1 1 d . . . C15 C -0.30164(13) 0.51993(8) 0.45956(5) 0.0199(3) Uani 1 1 d . . . H15 H -0.3596 0.4820 0.4469 0.024 Uiso 1 1 calc R . . C16 C -0.28365(13) 0.52427(9) 0.50732(5) 0.0214(3) Uani 1 1 d . . . C17 C -0.19436(14) 0.57885(9) 0.52419(5) 0.0215(3) Uani 1 1 d . . . H17 H -0.1810 0.5808 0.5569 0.026 Uiso 1 1 calc R . . C18 C -0.12356(13) 0.63061(8) 0.49613(5) 0.0194(3) Uani 1 1 d . . . C19 C -0.35683(15) 0.47074(10) 0.54019(5) 0.0272(3) Uani 1 1 d . . . H19A H -0.4241 0.4434 0.5231 0.041 Uiso 1 1 calc R . . H19B H -0.3927 0.5043 0.5650 0.041 Uiso 1 1 calc R . . H19C H -0.3012 0.4297 0.5538 0.041 Uiso 1 1 calc R . . C20 C -0.02281(14) 0.68651(9) 0.51654(5) 0.0232(3) Uani 1 1 d . . . C21 C -0.05457(17) 0.77622(9) 0.50741(6) 0.0326(4) Uani 1 1 d . . . H21A H -0.0623 0.7853 0.4738 0.049 Uiso 1 1 calc R . . H21B H 0.0120 0.8110 0.5199 0.049 Uiso 1 1 calc R . . H21C H -0.1337 0.7898 0.5227 0.049 Uiso 1 1 calc R . . C22 C 0.10414(15) 0.66540(11) 0.49470(6) 0.0333(4) Uani 1 1 d . . . H22A H 0.1207 0.6070 0.4986 0.050 Uiso 1 1 calc R . . H22B H 0.1700 0.6970 0.5101 0.050 Uiso 1 1 calc R . . H22C H 0.1027 0.6788 0.4615 0.050 Uiso 1 1 calc R . . C23 C -0.0093(2) 0.67539(12) 0.56914(6) 0.0399(4) Uani 1 1 d . . . H23A H -0.0890 0.6878 0.5844 0.060 Uiso 1 1 calc R . . H23B H 0.0554 0.7124 0.5809 0.060 Uiso 1 1 calc R . . H23C H 0.0145 0.6188 0.5759 0.060 Uiso 1 1 calc R . . C24 C -0.34690(13) 0.65453(8) 0.35663(5) 0.0190(3) Uani 1 1 d . . . H24A H -0.3149 0.7021 0.3742 0.023 Uiso 1 1 calc R . . H24B H -0.3414 0.6676 0.3230 0.023 Uiso 1 1 calc R . . C25 C 0.09118(16) 0.55735(10) 0.36425(6) 0.0311(3) Uani 1 1 d . . . H25A H 0.1727 0.5820 0.3578 0.047 Uiso 1 1 calc R . . H25B H 0.0730 0.5156 0.3408 0.047 Uiso 1 1 calc R . . H25C H 0.0925 0.5322 0.3952 0.047 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 Al 0.0213(2) 0.0165(2) 0.0194(2) 0.00155(15) 0.00257(15) 0.00149(15) O1 0.0244(5) 0.0205(5) 0.0176(5) 0.0015(4) 0.0035(4) -0.0045(4) O2 0.0254(5) 0.0162(4) 0.0176(4) 0.0024(4) 0.0020(4) -0.0020(4) S1 0.01894(17) 0.01926(17) 0.02185(17) 0.00026(12) -0.00031(12) -0.00003(12) S2 0.02299(18) 0.01495(17) 0.01708(17) 0.00025(11) 0.00083(12) 0.00109(12) C1 0.0236(7) 0.0158(6) 0.0200(7) 0.0012(5) 0.0049(5) 0.0002(5) C2 0.0218(6) 0.0176(6) 0.0199(6) 0.0001(5) 0.0027(5) 0.0017(5) C3 0.0236(7) 0.0165(6) 0.0292(7) 0.0025(5) 0.0027(6) -0.0009(5) C4 0.0279(7) 0.0217(7) 0.0279(7) 0.0059(6) 0.0063(6) -0.0013(6) C5 0.0357(8) 0.0254(7) 0.0199(7) 0.0025(6) 0.0050(6) -0.0027(6) C6 0.0312(8) 0.0192(6) 0.0202(7) -0.0009(5) 0.0051(5) -0.0036(6) C7 0.0388(9) 0.0326(9) 0.0317(8) 0.0118(7) 0.0044(7) -0.0089(7) C8 0.0462(10) 0.0265(8) 0.0201(7) -0.0055(6) 0.0086(6) -0.0131(7) C9 0.0819(16) 0.0511(12) 0.0225(8) -0.0100(8) 0.0067(9) -0.0329(11) C10 0.0654(13) 0.0224(8) 0.0445(11) -0.0088(7) 0.0139(9) -0.0101(8) C11 0.0409(10) 0.0472(11) 0.0423(10) -0.0168(8) 0.0010(8) -0.0175(9) C12 0.0224(7) 0.0164(6) 0.0216(7) -0.0028(5) -0.0004(5) -0.0008(5) C13 0.0214(6) 0.0145(6) 0.0189(6) 0.0030(5) 0.0019(5) 0.0029(5) C14 0.0219(6) 0.0166(6) 0.0164(6) 0.0015(5) 0.0005(5) 0.0031(5) C15 0.0209(6) 0.0167(6) 0.0221(7) 0.0022(5) 0.0000(5) 0.0004(5) C16 0.0229(7) 0.0196(6) 0.0216(7) 0.0048(5) 0.0026(5) 0.0011(5) C17 0.0259(7) 0.0207(6) 0.0181(6) 0.0024(5) -0.0006(5) 0.0021(5) C18 0.0228(7) 0.0156(6) 0.0197(6) 0.0013(5) -0.0007(5) 0.0024(5) C19 0.0280(7) 0.0302(8) 0.0233(7) 0.0077(6) 0.0022(6) -0.0040(6) C20 0.0283(7) 0.0196(7) 0.0216(7) 0.0006(5) -0.0037(5) -0.0024(6) C21 0.0399(9) 0.0183(7) 0.0396(9) -0.0027(6) -0.0069(7) 0.0003(6) C22 0.0245(8) 0.0331(8) 0.0423(9) -0.0047(7) -0.0049(7) -0.0009(6) C23 0.0534(11) 0.0412(10) 0.0252(8) 0.0027(7) -0.0118(8) -0.0171(8) C24 0.0208(6) 0.0159(6) 0.0202(6) 0.0036(5) 0.0006(5) 0.0008(5) C25 0.0282(8) 0.0248(8) 0.0404(9) -0.0015(6) -0.0012(7) 0.0080(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 Al O1 1.7645(11) . ? Al O2 1.7755(11) . ? Al C25 1.9441(16) . ? Al S1 2.5673(6) . ? Al S2 2.5897(6) . ? O1 C1 1.3452(16) . ? O2 C13 1.3490(16) . ? S1 C2 1.7727(15) . ? S1 C12 1.8320(14) . ? S2 C14 1.7685(14) . ? S2 C24 1.8321(14) . ? C1 C2 1.404(2) . ? C1 C6 1.416(2) . ? C2 C3 1.3954(19) . ? C3 C4 1.377(2) . ? C3 H3 0.9500 . ? C4 C5 1.398(2) . ? C4 C7 1.508(2) . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? C6 C8 1.536(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C11 1.533(3) . ? C8 C10 1.534(3) . ? C8 C9 1.534(2) . ? 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 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C24 1.505(2) 2_465 ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.4042(19) . ? C13 C18 1.4180(19) . ? C14 C15 1.3928(19) . ? C15 C16 1.3872(19) . ? C15 H15 0.9500 . ? C16 C17 1.395(2) . ? C16 C19 1.5078(19) . ? C17 C18 1.394(2) . ? C17 H17 0.9500 . ? C18 C20 1.531(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C23 1.529(2) . ? C20 C21 1.531(2) . ? C20 C22 1.536(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C12 1.505(2) 2_465 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 Al O2 131.03(5) . . ? O1 Al C25 113.77(7) . . ? O2 Al C25 115.16(7) . . ? O1 Al S1 82.16(4) . . ? O2 Al S1 87.74(4) . . ? C25 Al S1 104.42(6) . . ? O1 Al S2 84.76(4) . . ? O2 Al S2 80.24(4) . . ? C25 Al S2 106.15(6) . . ? S1 Al S2 149.42(2) . . ? C1 O1 Al 123.69(9) . . ? C13 O2 Al 120.75(9) . . ? C2 S1 C12 102.67(6) . . ? C2 S1 Al 89.66(5) . . ? C12 S1 Al 108.30(5) . . ? C14 S2 C24 101.56(6) . . ? C14 S2 Al 88.31(5) . . ? C24 S2 Al 96.04(5) . . ? O1 C1 C2 119.67(12) . . ? O1 C1 C6 121.19(12) . . ? C2 C1 C6 119.13(13) . . ? C3 C2 C1 121.83(13) . . ? C3 C2 S1 121.05(11) . . ? C1 C2 S1 117.04(10) . . ? C4 C3 C2 119.68(14) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.15(13) . . ? C3 C4 C7 121.16(14) . . ? C5 C4 C7 120.69(14) . . ? C6 C5 C4 124.21(14) . . ? C6 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C5 C6 C1 116.74(13) . . ? C5 C6 C8 121.99(13) . . ? C1 C6 C8 121.22(13) . . ? 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 . . ? C11 C8 C10 109.33(15) . . ? C11 C8 C9 107.68(16) . . ? C10 C8 C9 107.20(16) . . ? C11 C8 C6 111.79(13) . . ? C10 C8 C6 108.72(15) . . ? C9 C8 C6 112.00(13) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C24 C12 S1 113.14(9) 2_465 . ? C24 C12 H12A 109.0 2_465 . ? S1 C12 H12A 109.0 . . ? C24 C12 H12B 109.0 2_465 . ? S1 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O2 C13 C14 119.10(12) . . ? O2 C13 C18 121.83(12) . . ? C14 C13 C18 119.06(12) . . ? C15 C14 C13 122.03(12) . . ? C15 C14 S2 121.36(11) . . ? C13 C14 S2 116.53(10) . . ? C16 C15 C14 119.58(13) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 118.11(13) . . ? C15 C16 C19 121.15(13) . . ? C17 C16 C19 120.74(13) . . ? C18 C17 C16 124.16(13) . . ? C18 C17 H17 117.9 . . ? C16 C17 H17 117.9 . . ? C17 C18 C13 116.96(13) . . ? C17 C18 C20 121.70(12) . . ? C13 C18 C20 121.32(12) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 C21 107.74(13) . . ? C23 C20 C18 111.95(12) . . ? C21 C20 C18 110.61(12) . . ? C23 C20 C22 107.03(14) . . ? C21 C20 C22 110.04(14) . . ? C18 C20 C22 109.40(12) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C12 C24 S2 112.12(9) 2_465 . ? C12 C24 H24A 109.2 2_465 . ? S2 C24 H24A 109.2 . . ? C12 C24 H24B 109.2 2_465 . ? S2 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? Al C25 H25A 109.5 . . ? Al C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 Al O1 C1 108.40(11) . . . . ? C25 Al O1 C1 -74.03(12) . . . . ? S1 Al O1 C1 28.33(10) . . . . ? S2 Al O1 C1 -179.38(10) . . . . ? O1 Al O2 C13 112.45(10) . . . . ? C25 Al O2 C13 -65.09(12) . . . . ? S1 Al O2 C13 -169.97(10) . . . . ? S2 Al O2 C13 38.27(9) . . . . ? O1 Al S1 C2 -17.52(6) . . . . ? O2 Al S1 C2 -149.48(6) . . . . ? C25 Al S1 C2 95.10(7) . . . . ? S2 Al S1 C2 -83.06(6) . . . . ? O1 Al S1 C12 85.72(6) . . . . ? O2 Al S1 C12 -46.24(6) . . . . ? C25 Al S1 C12 -161.66(7) . . . . ? S2 Al S1 C12 20.18(7) . . . . ? O1 Al S2 C14 -159.34(6) . . . . ? O2 Al S2 C14 -26.13(5) . . . . ? C25 Al S2 C14 87.41(7) . . . . ? S1 Al S2 C14 -94.44(6) . . . . ? O1 Al S2 C24 -57.89(6) . . . . ? O2 Al S2 C24 75.32(6) . . . . ? C25 Al S2 C24 -171.15(7) . . . . ? S1 Al S2 C24 7.00(6) . . . . ? Al O1 C1 C2 -30.70(17) . . . . ? Al O1 C1 C6 149.11(11) . . . . ? O1 C1 C2 C3 -176.18(13) . . . . ? C6 C1 C2 C3 4.0(2) . . . . ? O1 C1 C2 S1 7.16(18) . . . . ? C6 C1 C2 S1 -172.65(11) . . . . ? C12 S1 C2 C3 83.90(13) . . . . ? Al S1 C2 C3 -167.41(11) . . . . ? C12 S1 C2 C1 -99.41(12) . . . . ? Al S1 C2 C1 9.29(11) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? S1 C2 C3 C4 177.17(11) . . . . ? C2 C3 C4 C5 -3.6(2) . . . . ? C2 C3 C4 C7 177.09(14) . . . . ? C3 C4 C5 C6 2.0(2) . . . . ? C7 C4 C5 C6 -178.64(16) . . . . ? C4 C5 C6 C1 2.5(2) . . . . ? C4 C5 C6 C8 -174.97(16) . . . . ? O1 C1 C6 C5 174.81(13) . . . . ? C2 C1 C6 C5 -5.4(2) . . . . ? O1 C1 C6 C8 -7.7(2) . . . . ? C2 C1 C6 C8 172.12(14) . . . . ? C5 C6 C8 C11 -122.78(17) . . . . ? C1 C6 C8 C11 59.8(2) . . . . ? C5 C6 C8 C10 116.43(17) . . . . ? C1 C6 C8 C10 -60.94(19) . . . . ? C5 C6 C8 C9 -1.8(2) . . . . ? C1 C6 C8 C9 -179.21(17) . . . . ? C2 S1 C12 C24 58.93(11) . . . 2_465 ? Al S1 C12 C24 -34.97(11) . . . 2_465 ? Al O2 C13 C14 -38.93(16) . . . . ? Al O2 C13 C18 140.77(11) . . . . ? O2 C13 C14 C15 -178.17(12) . . . . ? C18 C13 C14 C15 2.1(2) . . . . ? O2 C13 C14 S2 4.92(17) . . . . ? C18 C13 C14 S2 -174.78(10) . . . . ? C24 S2 C14 C15 103.78(12) . . . . ? Al S2 C14 C15 -160.40(11) . . . . ? C24 S2 C14 C13 -79.29(11) . . . . ? Al S2 C14 C13 16.53(10) . . . . ? C13 C14 C15 C16 0.6(2) . . . . ? S2 C14 C15 C16 177.32(11) . . . . ? C14 C15 C16 C17 -2.2(2) . . . . ? C14 C15 C16 C19 178.69(13) . . . . ? C15 C16 C17 C18 1.3(2) . . . . ? C19 C16 C17 C18 -179.61(14) . . . . ? C16 C17 C18 C13 1.3(2) . . . . ? C16 C17 C18 C20 -177.25(13) . . . . ? O2 C13 C18 C17 177.34(12) . . . . ? C14 C13 C18 C17 -2.96(19) . . . . ? O2 C13 C18 C20 -4.1(2) . . . . ? C14 C13 C18 C20 175.61(12) . . . . ? C17 C18 C20 C23 1.9(2) . . . . ? C13 C18 C20 C23 -176.60(14) . . . . ? C17 C18 C20 C21 -118.27(15) . . . . ? C13 C18 C20 C21 63.23(18) . . . . ? C17 C18 C20 C22 120.37(15) . . . . ? C13 C18 C20 C22 -58.14(17) . . . . ? C14 S2 C24 C12 -75.62(11) . . . 2_465 ? Al S2 C24 C12 -165.12(9) . . . 2_465 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.504 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.070 #============================================================================== #============================================================================== #===END data_gm3 _database_code_depnum_ccdc_archive 'CCDC 254740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H47 Al O3 S2' _chemical_formula_weight 702.91 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 14.766(7) _cell_length_b 11.823(6) _cell_length_c 22.170(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.260(10) _cell_angle_gamma 90.00 _cell_volume 3767(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 47730 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 25.20 _exptl_crystal_description colourless _exptl_crystal_colour plate _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 0.9839 _exptl_absorpt_process_details 'Bruker area detector absorption detection' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ; Bruker AXS diffractometer with CCD area detector ; _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47730 _diffrn_reflns_av_R_equivalents 0.2207 _diffrn_reflns_av_sigmaI/netI 0.1395 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.20 _reflns_number_total 6727 _reflns_number_gt 3699 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction 'SAINT, SADABS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.1007P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6727 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2104 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 S1 S 0.20522(8) 0.84846(10) 0.26459(6) 0.0311(3) Uani 1 1 d . . . S2 S 0.00989(9) 0.71957(10) 0.23233(6) 0.0335(3) Uani 1 1 d . . . O1 O 0.3235(2) 0.6591(2) 0.30771(15) 0.0323(8) Uani 1 1 d . . . O2 O 0.1544(2) 0.5939(3) 0.32215(14) 0.0326(8) Uani 1 1 d . . . O3 O 0.1921(2) 0.6037(3) 0.19412(15) 0.0361(8) Uani 1 1 d . . . Al Al 0.20741(10) 0.64894(11) 0.26715(7) 0.0302(4) Uani 1 1 d . . . C1 C 0.3599(3) 0.7551(4) 0.3352(2) 0.0323(11) Uani 1 1 d . . . C2 C 0.3118(3) 0.8571(4) 0.3192(2) 0.0300(11) Uani 1 1 d . . . C3 C 0.3464(3) 0.9593(4) 0.3441(2) 0.0341(12) Uani 1 1 d . . . H3 H 0.3123 1.0268 0.3315 0.041 Uiso 1 1 calc R . . C4 C 0.4284(3) 0.9643(4) 0.3863(2) 0.0325(11) Uani 1 1 d . . . C5 C 0.4767(3) 0.8629(4) 0.4030(2) 0.0333(12) Uani 1 1 d . . . H5 H 0.5344 0.8659 0.4327 0.040 Uiso 1 1 calc R . . C6 C 0.4449(3) 0.7579(4) 0.3784(2) 0.0340(12) Uani 1 1 d . . . C7 C 0.4680(4) 1.0739(4) 0.4143(2) 0.0422(13) Uani 1 1 d . . . H7A H 0.5213 1.0950 0.3973 0.063 Uiso 1 1 calc R . . H7B H 0.4882 1.0654 0.4594 0.063 Uiso 1 1 calc R . . H7C H 0.4203 1.1330 0.4046 0.063 Uiso 1 1 calc R . . C8 C 0.5002(3) 0.6498(4) 0.3981(2) 0.0381(12) Uani 1 1 d . . . C9 C 0.4408(4) 0.5670(4) 0.4253(3) 0.0463(14) Uani 1 1 d . . . H9A H 0.4290 0.5983 0.4637 0.069 Uiso 1 1 calc R . . H9B H 0.4738 0.4948 0.4342 0.069 Uiso 1 1 calc R . . H9C H 0.3815 0.5547 0.3954 0.069 Uiso 1 1 calc R . . C10 C 0.5284(4) 0.5976(4) 0.3425(3) 0.0460(14) Uani 1 1 d . . . H10A H 0.4727 0.5826 0.3098 0.069 Uiso 1 1 calc R . . H10B H 0.5616 0.5265 0.3549 0.069 Uiso 1 1 calc R . . H10C H 0.5692 0.6500 0.3270 0.069 Uiso 1 1 calc R . . C11 C 0.5887(4) 0.6730(5) 0.4477(3) 0.0543(16) Uani 1 1 d . . . H11A H 0.6293 0.7238 0.4309 0.081 Uiso 1 1 calc R . . H11B H 0.6213 0.6016 0.4602 0.081 Uiso 1 1 calc R . . H11C H 0.5724 0.7084 0.4837 0.081 Uiso 1 1 calc R . . C12 C 0.1207(3) 0.8727(4) 0.3113(2) 0.0335(12) Uani 1 1 d . . . H12A H 0.1315 0.8193 0.3466 0.040 Uiso 1 1 calc R . . H12B H 0.1270 0.9507 0.3279 0.040 Uiso 1 1 calc R . . C13 C 0.0250(3) 0.8555(4) 0.2710(2) 0.0339(12) Uani 1 1 d . . . H13A H 0.0123 0.9161 0.2393 0.041 Uiso 1 1 calc R . . H13B H -0.0212 0.8627 0.2968 0.041 Uiso 1 1 calc R . . C14 C -0.0086(3) 0.6306(4) 0.2923(2) 0.0284(11) Uani 1 1 d . . . C15 C 0.0680(3) 0.5771(4) 0.3303(2) 0.0291(11) Uani 1 1 d . . . C16 C 0.0533(3) 0.5055(4) 0.3778(2) 0.0297(11) Uani 1 1 d . . . C17 C -0.0371(3) 0.4915(4) 0.3833(2) 0.0342(12) Uani 1 1 d . . . H17 H -0.0475 0.4420 0.4147 0.041 Uiso 1 1 calc R . . C18 C -0.1143(3) 0.5443(4) 0.3463(2) 0.0330(12) Uani 1 1 d . . . C19 C -0.0966(3) 0.6140(4) 0.3003(2) 0.0327(12) Uani 1 1 d . . . H19 H -0.1472 0.6514 0.2735 0.039 Uiso 1 1 calc R . . C20 C -0.2091(3) 0.5293(4) 0.3573(2) 0.0406(13) Uani 1 1 d . . . H20A H -0.2161 0.5773 0.3920 0.061 Uiso 1 1 calc R . . H20B H -0.2181 0.4499 0.3672 0.061 Uiso 1 1 calc R . . H20C H -0.2555 0.5508 0.3199 0.061 Uiso 1 1 calc R . . C21 C 0.1353(3) 0.4500(4) 0.4237(2) 0.0340(12) Uani 1 1 d . . . C22 C 0.1024(4) 0.3726(4) 0.4693(2) 0.0409(13) Uani 1 1 d . . . H22A H 0.0622 0.3134 0.4464 0.061 Uiso 1 1 calc R . . H22B H 0.0675 0.4168 0.4937 0.061 Uiso 1 1 calc R . . H22C H 0.1564 0.3376 0.4970 0.061 Uiso 1 1 calc R . . C23 C 0.1954(3) 0.3797(4) 0.3911(2) 0.0381(12) Uani 1 1 d . . . H23A H 0.2442 0.3421 0.4220 0.057 Uiso 1 1 calc R . . H23B H 0.2240 0.4289 0.3651 0.057 Uiso 1 1 calc R . . H23C H 0.1569 0.3226 0.3651 0.057 Uiso 1 1 calc R . . C24 C 0.1932(4) 0.5444(4) 0.4610(2) 0.0392(13) Uani 1 1 d . . . H24A H 0.2457 0.5113 0.4910 0.059 Uiso 1 1 calc R . . H24B H 0.1543 0.5878 0.4830 0.059 Uiso 1 1 calc R . . H24C H 0.2166 0.5945 0.4328 0.059 Uiso 1 1 calc R . . C25 C 0.2129(3) 0.5191(4) 0.1549(2) 0.0301(11) Uani 1 1 d . . . C26 C 0.2840(3) 0.4388(4) 0.1953(2) 0.0307(11) Uani 1 1 d . . . C27 C 0.2561(3) 0.3746(4) 0.2402(2) 0.0342(12) Uani 1 1 d . . . H27 H 0.1930 0.3770 0.2433 0.041 Uiso 1 1 calc R . . C28 C 0.3189(4) 0.3075(4) 0.2802(2) 0.0404(13) Uani 1 1 d . . . H28 H 0.2989 0.2634 0.3106 0.048 Uiso 1 1 calc R . . C29 C 0.4102(4) 0.3043(4) 0.2763(2) 0.0419(13) Uani 1 1 d . . . H29 H 0.4535 0.2576 0.3036 0.050 Uiso 1 1 calc R . . C30 C 0.4384(4) 0.3687(5) 0.2329(2) 0.0447(14) Uani 1 1 d . . . H30 H 0.5018 0.3678 0.2306 0.054 Uiso 1 1 calc R . . C31 C 0.3754(3) 0.4353(4) 0.1923(2) 0.0367(12) Uani 1 1 d . . . H31 H 0.3958 0.4790 0.1619 0.044 Uiso 1 1 calc R . . C32 C 0.1221(3) 0.4623(4) 0.1229(2) 0.0308(11) Uani 1 1 d . . . C33 C 0.0450(3) 0.5297(4) 0.1030(2) 0.0343(12) Uani 1 1 d . . . H33 H 0.0491 0.6081 0.1127 0.041 Uiso 1 1 calc R . . C34 C -0.0375(3) 0.4867(4) 0.0694(2) 0.0386(13) Uani 1 1 d . . . H34 H -0.0894 0.5352 0.0557 0.046 Uiso 1 1 calc R . . C35 C -0.0450(4) 0.3708(4) 0.0556(2) 0.0373(12) Uani 1 1 d . . . H35 H -0.1015 0.3397 0.0323 0.045 Uiso 1 1 calc R . . C36 C 0.0314(3) 0.3038(4) 0.0766(2) 0.0379(12) Uani 1 1 d . . . H36 H 0.0268 0.2249 0.0684 0.045 Uiso 1 1 calc R . . C37 C 0.1146(3) 0.3478(4) 0.1093(2) 0.0332(11) Uani 1 1 d . . . H37 H 0.1669 0.2996 0.1225 0.040 Uiso 1 1 calc R . . C38 C 0.2515(3) 0.5734(4) 0.1041(2) 0.0361(12) Uani 1 1 d . . . C39 C 0.2739(4) 0.6868(4) 0.1049(3) 0.0430(14) Uani 1 1 d . . . H39 H 0.2688 0.7324 0.1392 0.052 Uiso 1 1 calc R . . C40 C 0.3038(4) 0.7341(5) 0.0560(3) 0.0546(16) Uani 1 1 d . . . H40 H 0.3192 0.8123 0.0573 0.065 Uiso 1 1 calc R . . C41 C 0.3118(4) 0.6720(5) 0.0062(3) 0.0535(16) Uani 1 1 d . . . H41 H 0.3308 0.7067 -0.0276 0.064 Uiso 1 1 calc R . . C42 C 0.2919(4) 0.5580(5) 0.0048(3) 0.0518(16) Uani 1 1 d . . . H42 H 0.2992 0.5129 -0.0292 0.062 Uiso 1 1 calc R . . C43 C 0.2618(3) 0.5102(5) 0.0529(2) 0.0422(13) Uani 1 1 d . . . H43 H 0.2474 0.4317 0.0514 0.051 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 S1 0.0336(7) 0.0229(6) 0.0373(7) 0.0017(5) 0.0089(5) 0.0010(5) S2 0.0388(7) 0.0230(6) 0.0393(7) 0.0023(5) 0.0102(6) 0.0003(5) O1 0.0383(19) 0.0161(17) 0.0429(19) 0.0007(14) 0.0101(15) 0.0004(14) O2 0.034(2) 0.0259(18) 0.0389(19) 0.0044(15) 0.0107(15) -0.0013(14) O3 0.046(2) 0.0217(18) 0.040(2) -0.0049(15) 0.0090(17) 0.0078(14) Al 0.0335(8) 0.0212(7) 0.0365(8) 0.0016(6) 0.0091(6) 0.0008(6) C1 0.036(3) 0.024(3) 0.040(3) 0.003(2) 0.015(2) 0.000(2) C2 0.033(3) 0.021(3) 0.040(3) 0.004(2) 0.015(2) 0.000(2) C3 0.038(3) 0.024(3) 0.043(3) 0.000(2) 0.017(2) -0.003(2) C4 0.034(3) 0.029(3) 0.036(3) -0.005(2) 0.014(2) -0.004(2) C5 0.032(3) 0.030(3) 0.038(3) -0.001(2) 0.008(2) -0.002(2) C6 0.032(3) 0.034(3) 0.038(3) 0.008(2) 0.010(2) 0.003(2) C7 0.043(3) 0.035(3) 0.049(3) -0.007(2) 0.012(3) -0.009(2) C8 0.035(3) 0.033(3) 0.047(3) 0.003(2) 0.011(2) 0.007(2) C9 0.050(3) 0.035(3) 0.054(4) 0.012(3) 0.011(3) 0.005(2) C10 0.043(3) 0.036(3) 0.059(4) 0.006(3) 0.013(3) 0.013(2) C11 0.041(3) 0.047(4) 0.069(4) 0.010(3) -0.001(3) 0.007(3) C12 0.040(3) 0.020(3) 0.043(3) 0.001(2) 0.013(2) 0.003(2) C13 0.037(3) 0.015(2) 0.051(3) 0.000(2) 0.013(2) 0.002(2) C14 0.030(3) 0.019(2) 0.036(3) -0.005(2) 0.007(2) -0.0004(19) C15 0.030(3) 0.020(2) 0.040(3) -0.009(2) 0.012(2) -0.005(2) C16 0.038(3) 0.018(2) 0.035(3) -0.005(2) 0.011(2) -0.001(2) C17 0.042(3) 0.024(3) 0.039(3) -0.005(2) 0.016(2) -0.003(2) C18 0.037(3) 0.020(3) 0.042(3) -0.008(2) 0.011(2) -0.002(2) C19 0.036(3) 0.020(2) 0.042(3) -0.005(2) 0.011(2) 0.001(2) C20 0.042(3) 0.034(3) 0.049(3) -0.008(2) 0.016(3) -0.003(2) C21 0.043(3) 0.022(3) 0.038(3) -0.004(2) 0.010(2) -0.004(2) C22 0.049(3) 0.031(3) 0.044(3) 0.006(2) 0.014(3) 0.000(2) C23 0.042(3) 0.028(3) 0.043(3) 0.004(2) 0.007(2) 0.003(2) C24 0.050(3) 0.024(3) 0.042(3) 0.000(2) 0.007(3) -0.001(2) C25 0.037(3) 0.023(3) 0.031(3) 0.001(2) 0.010(2) 0.004(2) C26 0.037(3) 0.020(2) 0.036(3) -0.004(2) 0.011(2) 0.003(2) C27 0.038(3) 0.026(3) 0.042(3) 0.001(2) 0.016(2) 0.002(2) C28 0.056(4) 0.026(3) 0.041(3) 0.007(2) 0.016(3) 0.007(2) C29 0.053(4) 0.029(3) 0.044(3) 0.004(2) 0.011(3) 0.013(2) C30 0.043(3) 0.047(4) 0.046(3) 0.000(3) 0.013(3) 0.016(3) C31 0.043(3) 0.031(3) 0.039(3) -0.001(2) 0.016(2) 0.008(2) C32 0.034(3) 0.028(3) 0.033(3) 0.000(2) 0.014(2) -0.002(2) C33 0.036(3) 0.029(3) 0.040(3) 0.002(2) 0.013(2) 0.004(2) C34 0.032(3) 0.039(3) 0.047(3) 0.008(3) 0.014(2) 0.006(2) C35 0.044(3) 0.033(3) 0.034(3) -0.002(2) 0.007(2) -0.005(2) C36 0.043(3) 0.030(3) 0.043(3) 0.000(2) 0.014(3) -0.001(2) C37 0.047(3) 0.023(3) 0.032(3) -0.001(2) 0.014(2) 0.002(2) C38 0.030(3) 0.036(3) 0.044(3) 0.008(2) 0.012(2) 0.004(2) C39 0.048(3) 0.026(3) 0.060(4) 0.007(3) 0.023(3) 0.003(2) C40 0.053(4) 0.038(3) 0.080(5) 0.021(3) 0.030(3) 0.014(3) C41 0.044(3) 0.063(4) 0.058(4) 0.033(3) 0.021(3) 0.013(3) C42 0.038(3) 0.073(5) 0.045(3) 0.011(3) 0.010(3) 0.004(3) C43 0.039(3) 0.052(4) 0.037(3) 0.006(3) 0.012(2) 0.000(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 S1 C2 1.755(5) . ? S1 C12 1.817(5) . ? S1 Al 2.360(2) . ? S2 C14 1.764(5) . ? S2 C13 1.811(5) . ? S2 Al 2.961(2) . ? O1 C1 1.341(5) . ? O1 Al 1.748(3) . ? O2 C15 1.345(5) . ? O2 Al 1.721(3) . ? O3 C25 1.404(5) . ? O3 Al 1.670(3) . ? C1 C6 1.394(6) . ? C1 C2 1.402(6) . ? C2 C3 1.377(6) . ? C3 C4 1.351(6) . ? C3 H3 0.9500 . ? C4 C5 1.401(7) . ? C4 C7 1.497(6) . ? C5 C6 1.393(6) . ? C5 H5 0.9500 . ? C6 C8 1.526(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.519(7) . ? C8 C11 1.527(7) . ? C8 C9 1.528(7) . ? 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 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.502(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.367(6) . ? C14 C15 1.397(6) . ? C15 C16 1.406(6) . ? C16 C17 1.377(6) . ? C16 C21 1.539(6) . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.381(7) . ? C18 C20 1.486(7) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.515(7) . ? C21 C22 1.522(7) . ? C21 C24 1.527(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 C38 1.517(7) . ? C25 C32 1.522(6) . ? C25 C26 1.540(6) . ? C26 C31 1.367(6) . ? C26 C27 1.386(6) . ? C27 C28 1.379(6) . ? C27 H27 0.9500 . ? C28 C29 1.372(7) . ? C28 H28 0.9500 . ? C29 C30 1.365(7) . ? C29 H29 0.9500 . ? C30 C31 1.383(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.377(6) . ? C32 C37 1.387(6) . ? C33 C34 1.371(7) . ? C33 H33 0.9500 . ? C34 C35 1.403(7) . ? C34 H34 0.9500 . ? C35 C36 1.369(7) . ? C35 H35 0.9500 . ? C36 C37 1.377(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.379(7) . ? C38 C43 1.397(7) . ? C39 C40 1.379(7) . ? C39 H39 0.9500 . ? C40 C41 1.354(8) . ? C40 H40 0.9500 . ? C41 C42 1.378(8) . ? C41 H41 0.9500 . ? C42 C43 1.369(7) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 S1 C12 102.9(2) . . ? C2 S1 Al 92.09(16) . . ? C12 S1 Al 98.72(16) . . ? C14 S2 C13 101.3(2) . . ? C14 S2 Al 87.05(15) . . ? C13 S2 Al 96.87(15) . . ? C1 O1 Al 122.4(3) . . ? C15 O2 Al 138.7(3) . . ? C25 O3 Al 145.8(3) . . ? O3 Al O2 125.70(18) . . ? O3 Al O1 114.78(17) . . ? O2 Al O1 102.31(16) . . ? O3 Al S1 107.37(13) . . ? O2 Al S1 112.91(13) . . ? O1 Al S1 87.13(11) . . ? O3 Al S2 86.08(12) . . ? O2 Al S2 73.18(12) . . ? O1 Al S2 154.95(12) . . ? S1 Al S2 72.82(5) . . ? O1 C1 C6 122.4(4) . . ? O1 C1 C2 119.1(4) . . ? C6 C1 C2 118.5(4) . . ? C3 C2 C1 122.2(4) . . ? C3 C2 S1 121.3(4) . . ? C1 C2 S1 116.5(4) . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 117.9(4) . . ? C3 C4 C7 121.9(4) . . ? C5 C4 C7 120.3(4) . . ? C6 C5 C4 123.6(4) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C5 C6 C1 117.4(4) . . ? C5 C6 C8 121.6(4) . . ? C1 C6 C8 121.0(4) . . ? 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 . . ? C10 C8 C6 109.7(4) . . ? C10 C8 C11 107.9(4) . . ? C6 C8 C11 111.7(4) . . ? C10 C8 C9 110.4(4) . . ? C6 C8 C9 109.4(4) . . ? C11 C8 C9 107.8(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S1 108.4(3) . . ? C13 C12 H12A 110.0 . . ? S1 C12 H12A 110.0 . . ? C13 C12 H12B 110.0 . . ? S1 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C12 C13 S2 113.5(3) . . ? C12 C13 H13A 108.9 . . ? S2 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? S2 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C19 C14 C15 121.3(5) . . ? C19 C14 S2 120.0(4) . . ? C15 C14 S2 118.8(4) . . ? O2 C15 C14 120.9(4) . . ? O2 C15 C16 120.3(4) . . ? C14 C15 C16 118.8(4) . . ? C17 C16 C15 117.2(4) . . ? C17 C16 C21 121.5(4) . . ? C15 C16 C21 121.3(4) . . ? C16 C17 C18 125.1(5) . . ? C16 C17 H17 117.5 . . ? C18 C17 H17 117.5 . . ? C19 C18 C17 115.8(5) . . ? C19 C18 C20 122.4(4) . . ? C17 C18 C20 121.7(5) . . ? C14 C19 C18 121.8(5) . . ? C14 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 107.3(4) . . ? C23 C21 C24 110.0(4) . . ? C22 C21 C24 107.8(4) . . ? C23 C21 C16 112.1(4) . . ? C22 C21 C16 111.9(4) . . ? C24 C21 C16 107.7(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 . . ? O3 C25 C38 109.3(4) . . ? O3 C25 C32 108.0(4) . . ? C38 C25 C32 106.3(4) . . ? O3 C25 C26 107.2(4) . . ? C38 C25 C26 111.8(4) . . ? C32 C25 C26 114.1(4) . . ? C31 C26 C27 118.5(5) . . ? C31 C26 C25 122.6(4) . . ? C27 C26 C25 118.6(4) . . ? C28 C27 C26 120.7(5) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 120.0(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 119.6(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.5(5) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C26 C31 C30 120.7(5) . . ? C26 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C37 118.5(4) . . ? C33 C32 C25 118.0(4) . . ? C37 C32 C25 123.4(4) . . ? C34 C33 C32 121.7(5) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 119.7(5) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 118.3(5) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C35 C36 C37 121.8(5) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C32 120.0(5) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C39 C38 C43 117.4(5) . . ? C39 C38 C25 122.2(5) . . ? C43 C38 C25 120.4(5) . . ? C40 C39 C38 120.3(5) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 121.6(6) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 119.3(5) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C43 C42 C41 119.6(6) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C38 121.8(5) . . ? C42 C43 H43 119.1 . . ? C38 C43 H43 119.1 . . ? 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 C25 O3 Al O2 -75.4(6) . . . . ? C25 O3 Al O1 53.0(6) . . . . ? C25 O3 Al S1 147.9(5) . . . . ? C25 O3 Al S2 -141.4(6) . . . . ? C15 O2 Al O3 -58.9(5) . . . . ? C15 O2 Al O1 167.8(4) . . . . ? C15 O2 Al S1 75.7(4) . . . . ? C15 O2 Al S2 13.3(4) . . . . ? C1 O1 Al O3 124.8(3) . . . . ? C1 O1 Al O2 -95.9(4) . . . . ? C1 O1 Al S1 16.9(3) . . . . ? C1 O1 Al S2 -19.3(5) . . . . ? C2 S1 Al O3 -127.2(2) . . . . ? C12 S1 Al O3 129.5(2) . . . . ? C2 S1 Al O2 90.1(2) . . . . ? C12 S1 Al O2 -13.3(2) . . . . ? C2 S1 Al O1 -12.08(19) . . . . ? C12 S1 Al O1 -115.4(2) . . . . ? C2 S1 Al S2 152.72(16) . . . . ? C12 S1 Al S2 49.35(16) . . . . ? C14 S2 Al O3 121.84(19) . . . . ? C13 S2 Al O3 -137.1(2) . . . . ? C14 S2 Al O2 -7.34(18) . . . . ? C13 S2 Al O2 93.7(2) . . . . ? C14 S2 Al O1 -90.4(3) . . . . ? C13 S2 Al O1 10.7(3) . . . . ? C14 S2 Al S1 -128.62(15) . . . . ? C13 S2 Al S1 -27.54(17) . . . . ? Al O1 C1 C6 165.6(3) . . . . ? Al O1 C1 C2 -15.6(6) . . . . ? O1 C1 C2 C3 -178.0(4) . . . . ? C6 C1 C2 C3 0.8(7) . . . . ? O1 C1 C2 S1 1.2(6) . . . . ? C6 C1 C2 S1 -179.9(3) . . . . ? C12 S1 C2 C3 -73.0(4) . . . . ? Al S1 C2 C3 -172.4(4) . . . . ? C12 S1 C2 C1 107.7(4) . . . . ? Al S1 C2 C1 8.3(4) . . . . ? C1 C2 C3 C4 -1.1(7) . . . . ? S1 C2 C3 C4 179.6(4) . . . . ? C2 C3 C4 C5 0.7(7) . . . . ? C2 C3 C4 C7 180.0(4) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C7 C4 C5 C6 -179.2(5) . . . . ? C4 C5 C6 C1 -0.4(7) . . . . ? C4 C5 C6 C8 180.0(4) . . . . ? O1 C1 C6 C5 178.7(4) . . . . ? C2 C1 C6 C5 -0.1(7) . . . . ? O1 C1 C6 C8 -1.6(7) . . . . ? C2 C1 C6 C8 179.6(4) . . . . ? C5 C6 C8 C10 -117.6(5) . . . . ? C1 C6 C8 C10 62.7(6) . . . . ? C5 C6 C8 C11 1.9(7) . . . . ? C1 C6 C8 C11 -177.7(4) . . . . ? C5 C6 C8 C9 121.2(5) . . . . ? C1 C6 C8 C9 -58.4(6) . . . . ? C2 S1 C12 C13 -174.2(3) . . . . ? Al S1 C12 C13 -80.0(3) . . . . ? S1 C12 C13 S2 54.2(4) . . . . ? C14 S2 C13 C12 79.8(4) . . . . ? Al S2 C13 C12 -8.5(4) . . . . ? C13 S2 C14 C19 89.0(4) . . . . ? Al S2 C14 C19 -174.6(4) . . . . ? C13 S2 C14 C15 -91.8(4) . . . . ? Al S2 C14 C15 4.7(3) . . . . ? Al O2 C15 C14 -14.3(7) . . . . ? Al O2 C15 C16 166.1(3) . . . . ? C19 C14 C15 O2 -180.0(4) . . . . ? S2 C14 C15 O2 0.8(6) . . . . ? C19 C14 C15 C16 -0.4(7) . . . . ? S2 C14 C15 C16 -179.6(3) . . . . ? O2 C15 C16 C17 -179.5(4) . . . . ? C14 C15 C16 C17 0.9(6) . . . . ? O2 C15 C16 C21 3.4(6) . . . . ? C14 C15 C16 C21 -176.2(4) . . . . ? C15 C16 C17 C18 -1.4(7) . . . . ? C21 C16 C17 C18 175.7(4) . . . . ? C16 C17 C18 C19 1.2(7) . . . . ? C16 C17 C18 C20 -176.7(4) . . . . ? C15 C14 C19 C18 0.3(7) . . . . ? S2 C14 C19 C18 179.5(4) . . . . ? C17 C18 C19 C14 -0.7(7) . . . . ? C20 C18 C19 C14 177.3(4) . . . . ? C17 C16 C21 C23 126.0(5) . . . . ? C15 C16 C21 C23 -57.0(6) . . . . ? C17 C16 C21 C22 5.4(6) . . . . ? C15 C16 C21 C22 -177.6(4) . . . . ? C17 C16 C21 C24 -112.9(5) . . . . ? C15 C16 C21 C24 64.1(5) . . . . ? Al O3 C25 C38 -127.2(5) . . . . ? Al O3 C25 C32 117.5(5) . . . . ? Al O3 C25 C26 -5.9(7) . . . . ? O3 C25 C26 C31 -108.2(5) . . . . ? C38 C25 C26 C31 11.6(6) . . . . ? C32 C25 C26 C31 132.3(5) . . . . ? O3 C25 C26 C27 66.1(5) . . . . ? C38 C25 C26 C27 -174.1(4) . . . . ? C32 C25 C26 C27 -53.4(6) . . . . ? C31 C26 C27 C28 -0.9(7) . . . . ? C25 C26 C27 C28 -175.5(4) . . . . ? C26 C27 C28 C29 0.5(7) . . . . ? C27 C28 C29 C30 0.6(8) . . . . ? C28 C29 C30 C31 -1.2(8) . . . . ? C27 C26 C31 C30 0.3(7) . . . . ? C25 C26 C31 C30 174.6(4) . . . . ? C29 C30 C31 C26 0.8(8) . . . . ? O3 C25 C32 C33 40.2(6) . . . . ? C38 C25 C32 C33 -76.9(5) . . . . ? C26 C25 C32 C33 159.4(4) . . . . ? O3 C25 C32 C37 -144.0(4) . . . . ? C38 C25 C32 C37 98.8(5) . . . . ? C26 C25 C32 C37 -24.9(6) . . . . ? C37 C32 C33 C34 -1.1(7) . . . . ? C25 C32 C33 C34 174.8(4) . . . . ? C32 C33 C34 C35 1.0(7) . . . . ? C33 C34 C35 C36 0.3(7) . . . . ? C34 C35 C36 C37 -1.5(7) . . . . ? C35 C36 C37 C32 1.4(7) . . . . ? C33 C32 C37 C36 -0.1(7) . . . . ? C25 C32 C37 C36 -175.8(4) . . . . ? O3 C25 C38 C39 8.8(6) . . . . ? C32 C25 C38 C39 125.2(5) . . . . ? C26 C25 C38 C39 -109.7(5) . . . . ? O3 C25 C38 C43 -168.3(4) . . . . ? C32 C25 C38 C43 -52.0(6) . . . . ? C26 C25 C38 C43 73.2(5) . . . . ? C43 C38 C39 C40 0.9(7) . . . . ? C25 C38 C39 C40 -176.3(5) . . . . ? C38 C39 C40 C41 0.2(8) . . . . ? C39 C40 C41 C42 -1.8(8) . . . . ? C40 C41 C42 C43 2.1(8) . . . . ? C41 C42 C43 C38 -0.9(8) . . . . ? C39 C38 C43 C42 -0.6(7) . . . . ? C25 C38 C43 C42 176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.701 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.086 #============================================================================== #===END