# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Raymundo Cea-Olivares' _publ_contact_author_email CEA@SERVIDOR.UNAM.MX _publ_section_title ; Solubilizing Functionalized Molecular Aluminosilicates ; loop_ _publ_author_name 'Raymundo Cea-Olivares' "Ra\'ul Huerta-Lavorie" 'Vojteck Jancik' F.Rascon-Cruz ; R.A.Toscano ; # Attachment 'compound5.cif' data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 700777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H69 Al N2 O4 Si' _chemical_formula_sum 'C41 H69 Al N2 O4 Si' _chemical_formula_weight 709.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.061(2) _cell_length_b 19.621(3) _cell_length_c 18.028(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.40(2) _cell_angle_gamma 90.00 _cell_volume 4266(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7760 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details 'Sadabs, Sheldrick 1996' _exptl_special_details ; The intensities were measured with Bruker Apex CCD detector ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44647 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7485 _reflns_number_gt 5554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the Cs symmetry of the molecule and the value of the beta angle (90.40(2)\%), Orthorhombic system could be plausible for this structure. However, the Cs symmetry is not retained in the solid state, and thus the crystal system was identified as monoclinic and the space group P2(1)/c was used to solve and refine the structure. ; _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^)+(0.0551P)^2^+1.6630P] 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 7485 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.23355(6) 0.25032(3) 0.03686(4) 0.02211(18) Uani 1 1 d . . . H1 H 0.280(2) 0.2474(11) -0.0425(13) 0.033 Uiso 1 1 d . . . Si1 Si 0.46116(5) 0.24124(3) 0.11710(4) 0.02322(17) Uani 1 1 d . . . N1 N 0.13249(15) 0.32488(9) 0.04340(10) 0.0234(4) Uani 1 1 d . . . O1 O 0.33039(13) 0.25161(8) 0.10693(9) 0.0268(4) Uani 1 1 d . . . C1 C -0.0390(2) 0.13106(13) -0.01707(15) 0.0356(6) Uani 1 1 d . . . H1A H 0.0055 0.0956 -0.0410 0.053 Uiso 1 1 calc R . . H1B H -0.0972 0.1465 -0.0514 0.053 Uiso 1 1 calc R . . H1C H -0.0731 0.1125 0.0278 0.053 Uiso 1 1 calc R . . N2 N 0.12406(15) 0.18065(9) 0.04590(10) 0.0234(4) Uani 1 1 d . . . C2 C 0.03430(19) 0.19031(12) 0.00340(13) 0.0244(5) Uani 1 1 d . . . O2 O 0.51114(14) 0.28317(8) 0.18692(9) 0.0317(4) Uani 1 1 d . . . O3 O 0.51713(13) 0.26371(8) 0.03915(9) 0.0298(4) Uani 1 1 d . . . C3 C 0.0041(2) 0.25476(12) -0.02356(14) 0.0266(5) Uani 1 1 d . . . H3A H -0.054(2) 0.2554(12) -0.0569(14) 0.032 Uiso 1 1 d . . . C4 C 0.04182(19) 0.31807(12) 0.00136(13) 0.0255(5) Uani 1 1 d . . . O4 O 0.49750(13) 0.16260(8) 0.13131(9) 0.0268(4) Uani 1 1 d . . . C5 C -0.0255(2) 0.37943(13) -0.02100(15) 0.0347(6) Uani 1 1 d . . . H5A H -0.0317 0.4105 0.0213 0.052 Uiso 1 1 calc R . . H5B H -0.0997 0.3648 -0.0367 0.052 Uiso 1 1 calc R . . H5C H 0.0111 0.4029 -0.0621 0.052 Uiso 1 1 calc R . . C6 C 0.15994(19) 0.39074(11) 0.07483(13) 0.0253(5) Uani 1 1 d . . . C7 C 0.1285(2) 0.40497(12) 0.14852(14) 0.0294(6) Uani 1 1 d . . . C8 C 0.1559(2) 0.46834(12) 0.17752(15) 0.0340(6) Uani 1 1 d . . . H8A H 0.1350 0.4791 0.2269 0.041 Uiso 1 1 calc R . . C9 C 0.2126(2) 0.51600(13) 0.13633(15) 0.0378(7) Uani 1 1 d . . . H9A H 0.2302 0.5592 0.1572 0.045 Uiso 1 1 calc R . . C10 C 0.2437(2) 0.50083(13) 0.06509(15) 0.0352(6) Uani 1 1 d . . . H10A H 0.2837 0.5338 0.0374 0.042 Uiso 1 1 calc R . . C11 C 0.2181(2) 0.43810(12) 0.03214(14) 0.0280(6) Uani 1 1 d . . . C12 C 0.2565(2) 0.42456(13) -0.04645(14) 0.0331(6) Uani 1 1 d . . . H12A H 0.2218 0.3810 -0.0635 0.040 Uiso 1 1 calc R . . C13 C 0.2207(3) 0.48086(14) -0.10010(15) 0.0440(7) Uani 1 1 d . . . H13A H 0.1400 0.4864 -0.0981 0.066 Uiso 1 1 calc R . . H13B H 0.2423 0.4685 -0.1506 0.066 Uiso 1 1 calc R . . H13C H 0.2567 0.5238 -0.0860 0.066 Uiso 1 1 calc R . . C14 C 0.3821(2) 0.41531(16) -0.04785(16) 0.0467(8) Uani 1 1 d . . . H14A H 0.4028 0.3763 -0.0168 0.070 Uiso 1 1 calc R . . H14B H 0.4181 0.4566 -0.0287 0.070 Uiso 1 1 calc R . . H14C H 0.4060 0.4072 -0.0989 0.070 Uiso 1 1 calc R . . C15 C 0.0664(2) 0.35307(13) 0.19527(14) 0.0359(6) Uani 1 1 d . . . H15A H 0.0964 0.3070 0.1826 0.043 Uiso 1 1 calc R . . C16 C -0.0565(2) 0.35246(17) 0.17737(17) 0.0532(8) Uani 1 1 d . . . H16A H -0.0677 0.3395 0.1253 0.080 Uiso 1 1 calc R . . H16B H -0.0875 0.3980 0.1857 0.080 Uiso 1 1 calc R . . H16C H -0.0939 0.3195 0.2095 0.080 Uiso 1 1 calc R . . C17 C 0.0825(2) 0.36309(15) 0.27880(15) 0.0462(7) Uani 1 1 d . . . H17A H 0.1619 0.3651 0.2905 0.069 Uiso 1 1 calc R . . H17B H 0.0489 0.3249 0.3054 0.069 Uiso 1 1 calc R . . H17C H 0.0470 0.4057 0.2941 0.069 Uiso 1 1 calc R . . C18 C 0.13895(19) 0.11512(11) 0.08153(13) 0.0244(5) Uani 1 1 d . . . C19 C 0.0938(2) 0.10416(12) 0.15214(14) 0.0290(6) Uani 1 1 d . . . C20 C 0.1098(2) 0.04038(13) 0.18483(15) 0.0337(6) Uani 1 1 d . . . H20A H 0.0789 0.0318 0.2322 0.040 Uiso 1 1 calc R . . C21 C 0.1686(2) -0.01005(13) 0.15060(15) 0.0338(6) Uani 1 1 d . . . H21A H 0.1790 -0.0528 0.1745 0.041 Uiso 1 1 calc R . . C22 C 0.2126(2) 0.00132(12) 0.08142(14) 0.0318(6) Uani 1 1 d . . . H22A H 0.2538 -0.0338 0.0581 0.038 Uiso 1 1 calc R . . C23 C 0.1978(2) 0.06338(12) 0.04476(13) 0.0270(6) Uani 1 1 d . . . C24 C 0.2466(2) 0.07264(12) -0.03194(14) 0.0306(6) Uani 1 1 d . . . H24A H 0.2189 0.1170 -0.0522 0.037 Uiso 1 1 calc R . . C25 C 0.3725(2) 0.07656(14) -0.02756(15) 0.0404(7) Uani 1 1 d . . . H25A H 0.3943 0.1132 0.0065 0.061 Uiso 1 1 calc R . . H25B H 0.4022 0.0859 -0.0770 0.061 Uiso 1 1 calc R . . H25C H 0.4020 0.0331 -0.0093 0.061 Uiso 1 1 calc R . . C26 C 0.2100(2) 0.01633(13) -0.08504(14) 0.0373(7) Uani 1 1 d . . . H26A H 0.1288 0.0150 -0.0876 0.056 Uiso 1 1 calc R . . H26B H 0.2380 -0.0276 -0.0671 0.056 Uiso 1 1 calc R . . H26C H 0.2397 0.0254 -0.1345 0.056 Uiso 1 1 calc R . . C27 C 0.0294(2) 0.15852(13) 0.19334(14) 0.0360(6) Uani 1 1 d . . . H27A H 0.0352 0.2016 0.1641 0.043 Uiso 1 1 calc R . . C28 C 0.0772(3) 0.17245(19) 0.26941(18) 0.0717(11) Uani 1 1 d . . . H28A H 0.1546 0.1870 0.2648 0.108 Uiso 1 1 calc R . . H28B H 0.0737 0.1309 0.2994 0.108 Uiso 1 1 calc R . . H28C H 0.0343 0.2086 0.2934 0.108 Uiso 1 1 calc R . . C29 C -0.0933(3) 0.14058(17) 0.1985(2) 0.0663(10) Uani 1 1 d . . . H29A H -0.1244 0.1356 0.1484 0.099 Uiso 1 1 calc R . . H29B H -0.1325 0.1770 0.2247 0.099 Uiso 1 1 calc R . . H29C H -0.1017 0.0976 0.2256 0.099 Uiso 1 1 calc R . . C30 C 0.4967(2) 0.35096(13) 0.21519(15) 0.0376(7) Uani 1 1 d . . . C31 C 0.3965(3) 0.35053(18) 0.26435(19) 0.0646(10) Uani 1 1 d . . . H31A H 0.4087 0.3188 0.3056 0.097 Uiso 1 1 calc R . . H31B H 0.3314 0.3360 0.2356 0.097 Uiso 1 1 calc R . . H31C H 0.3840 0.3965 0.2839 0.097 Uiso 1 1 calc R . . C32 C 0.4816(3) 0.40123(14) 0.15183(18) 0.0580(9) Uani 1 1 d . . . H32A H 0.5433 0.3967 0.1171 0.087 Uiso 1 1 calc R . . H32B H 0.4801 0.4477 0.1716 0.087 Uiso 1 1 calc R . . H32C H 0.4116 0.3917 0.1259 0.087 Uiso 1 1 calc R . . C33 C 0.6015(3) 0.36642(16) 0.25919(19) 0.0600(10) Uani 1 1 d . . . H33A H 0.6653 0.3663 0.2258 0.090 Uiso 1 1 calc R . . H33B H 0.6121 0.3316 0.2976 0.090 Uiso 1 1 calc R . . H33C H 0.5948 0.4113 0.2825 0.090 Uiso 1 1 calc R . . C34 C 0.6268(2) 0.25263(13) 0.01002(15) 0.0339(6) Uani 1 1 d . . . C35 C 0.7133(2) 0.26308(18) 0.06991(18) 0.0585(9) Uani 1 1 d . . . H35A H 0.7004 0.2309 0.1105 0.088 Uiso 1 1 calc R . . H35B H 0.7086 0.3098 0.0888 0.088 Uiso 1 1 calc R . . H35C H 0.7872 0.2553 0.0493 0.088 Uiso 1 1 calc R . . C36 C 0.6391(3) 0.30392(18) -0.05162(19) 0.0658(10) Uani 1 1 d . . . H36A H 0.6320 0.3501 -0.0314 0.099 Uiso 1 1 calc R . . H36B H 0.5812 0.2963 -0.0891 0.099 Uiso 1 1 calc R . . H36C H 0.7122 0.2987 -0.0744 0.099 Uiso 1 1 calc R . . C37 C 0.6330(3) 0.18111(15) -0.02071(18) 0.0529(8) Uani 1 1 d . . . H37A H 0.6252 0.1482 0.0198 0.079 Uiso 1 1 calc R . . H37B H 0.7047 0.1744 -0.0449 0.079 Uiso 1 1 calc R . . H37C H 0.5732 0.1743 -0.0570 0.079 Uiso 1 1 calc R . . C38 C 0.4910(2) 0.12085(13) 0.19733(14) 0.0339(6) Uani 1 1 d . . . C39 C 0.4999(3) 0.04841(15) 0.16931(19) 0.0680(11) Uani 1 1 d . . . H39A H 0.5672 0.0436 0.1396 0.102 Uiso 1 1 calc R . . H39B H 0.4349 0.0376 0.1386 0.102 Uiso 1 1 calc R . . H39C H 0.5033 0.0170 0.2116 0.102 Uiso 1 1 calc R . . C40 C 0.5870(3) 0.13756(17) 0.24764(17) 0.0553(9) Uani 1 1 d . . . H40A H 0.5819 0.1853 0.2634 0.083 Uiso 1 1 calc R . . H40B H 0.6567 0.1305 0.2211 0.083 Uiso 1 1 calc R . . H40C H 0.5851 0.1079 0.2913 0.083 Uiso 1 1 calc R . . C41 C 0.3818(3) 0.13282(19) 0.23484(18) 0.0631(10) Uani 1 1 d . . . H41A H 0.3797 0.1794 0.2544 0.095 Uiso 1 1 calc R . . H41B H 0.3733 0.1003 0.2756 0.095 Uiso 1 1 calc R . . H41C H 0.3214 0.1266 0.1989 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0213(4) 0.0183(4) 0.0267(4) -0.0009(3) 0.0014(3) 0.0004(3) Si1 0.0213(4) 0.0206(4) 0.0277(4) -0.0004(3) -0.0007(3) -0.0001(3) N1 0.0236(11) 0.0205(10) 0.0260(11) -0.0004(8) -0.0012(9) 0.0012(8) O1 0.0221(9) 0.0260(9) 0.0323(9) -0.0009(7) -0.0005(7) 0.0004(7) C1 0.0307(15) 0.0325(15) 0.0436(16) -0.0001(12) -0.0065(12) -0.0063(12) N2 0.0226(11) 0.0195(10) 0.0281(11) -0.0014(8) 0.0004(9) -0.0006(8) C2 0.0231(13) 0.0257(13) 0.0246(13) -0.0039(10) 0.0036(10) -0.0025(10) O2 0.0310(10) 0.0272(9) 0.0370(10) -0.0077(8) -0.0069(8) 0.0032(8) O3 0.0256(9) 0.0306(10) 0.0331(10) 0.0041(8) 0.0019(7) 0.0006(7) C3 0.0219(13) 0.0320(14) 0.0259(13) -0.0002(11) -0.0024(10) 0.0023(11) C4 0.0229(13) 0.0261(13) 0.0275(14) 0.0019(10) 0.0031(11) 0.0022(10) O4 0.0308(10) 0.0204(9) 0.0291(9) 0.0031(7) 0.0011(7) 0.0025(7) C5 0.0311(15) 0.0288(14) 0.0442(16) 0.0001(12) -0.0060(12) 0.0045(11) C6 0.0243(13) 0.0173(12) 0.0342(14) -0.0028(10) -0.0029(11) 0.0038(10) C7 0.0280(14) 0.0256(13) 0.0345(15) -0.0031(11) -0.0002(11) 0.0064(11) C8 0.0409(16) 0.0260(14) 0.0351(15) -0.0057(12) -0.0007(12) 0.0064(12) C9 0.0442(17) 0.0246(14) 0.0444(17) -0.0086(12) -0.0072(13) -0.0002(12) C10 0.0354(16) 0.0238(14) 0.0463(17) 0.0013(12) -0.0029(13) -0.0015(11) C11 0.0276(14) 0.0206(13) 0.0356(15) -0.0005(11) -0.0029(11) 0.0042(10) C12 0.0410(16) 0.0241(13) 0.0341(15) 0.0023(11) 0.0013(12) -0.0012(11) C13 0.058(2) 0.0335(16) 0.0401(17) 0.0064(13) -0.0036(14) 0.0011(14) C14 0.0413(18) 0.057(2) 0.0421(18) 0.0031(14) 0.0070(14) 0.0073(14) C15 0.0433(17) 0.0288(14) 0.0357(15) -0.0059(12) 0.0077(12) 0.0012(12) C16 0.0451(19) 0.065(2) 0.0496(19) 0.0011(16) 0.0043(15) -0.0172(16) C17 0.0495(19) 0.0519(19) 0.0373(17) -0.0007(14) 0.0074(14) -0.0005(15) C18 0.0227(13) 0.0205(12) 0.0299(14) 0.0005(10) -0.0034(10) -0.0041(10) C19 0.0261(13) 0.0271(14) 0.0339(15) -0.0009(11) 0.0023(11) -0.0059(11) C20 0.0347(15) 0.0314(15) 0.0351(15) 0.0060(12) 0.0036(12) -0.0069(12) C21 0.0365(15) 0.0235(13) 0.0414(16) 0.0077(12) -0.0033(12) -0.0031(11) C22 0.0344(15) 0.0213(13) 0.0398(16) -0.0011(11) -0.0007(12) -0.0010(11) C23 0.0254(13) 0.0227(13) 0.0329(14) -0.0006(11) -0.0010(11) -0.0034(10) C24 0.0388(16) 0.0207(13) 0.0323(15) -0.0026(11) 0.0025(12) 0.0016(11) C25 0.0397(17) 0.0444(17) 0.0372(16) -0.0078(13) 0.0092(13) -0.0080(13) C26 0.0443(17) 0.0319(15) 0.0356(16) -0.0012(12) -0.0020(13) -0.0008(12) C27 0.0445(17) 0.0282(14) 0.0356(16) 0.0002(12) 0.0113(13) -0.0009(12) C28 0.079(3) 0.084(3) 0.052(2) -0.0288(19) -0.0047(19) 0.024(2) C29 0.044(2) 0.058(2) 0.097(3) -0.011(2) 0.0157(19) 0.0058(16) C30 0.0433(17) 0.0299(15) 0.0393(16) -0.0112(12) -0.0082(13) 0.0056(12) C31 0.062(2) 0.067(2) 0.064(2) -0.0304(19) 0.0055(18) 0.0129(18) C32 0.081(3) 0.0307(17) 0.062(2) -0.0092(15) -0.0189(18) 0.0048(16) C33 0.058(2) 0.0472(19) 0.075(2) -0.0256(17) -0.0319(18) 0.0066(16) C34 0.0243(13) 0.0400(16) 0.0376(15) 0.0020(12) 0.0064(11) -0.0011(12) C35 0.0266(16) 0.093(3) 0.056(2) -0.0174(18) 0.0032(14) -0.0035(16) C36 0.054(2) 0.072(2) 0.072(2) 0.0307(19) 0.0273(18) 0.0044(18) C37 0.0477(19) 0.052(2) 0.060(2) -0.0123(16) 0.0212(16) 0.0005(15) C38 0.0370(15) 0.0306(14) 0.0340(15) 0.0115(12) -0.0040(12) -0.0008(12) C39 0.104(3) 0.0303(17) 0.070(2) 0.0175(16) -0.015(2) 0.0011(18) C40 0.052(2) 0.059(2) 0.055(2) 0.0162(16) -0.0196(16) -0.0029(16) C41 0.0450(19) 0.095(3) 0.050(2) 0.0354(19) 0.0088(15) -0.0017(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7146(17) . ? Al1 N1 1.9083(19) . ? Al1 N2 1.9084(19) . ? Al1 H1 1.54(2) . ? Si1 O1 1.5995(17) . ? Si1 O2 1.6169(17) . ? Si1 O4 1.6238(16) . ? Si1 O3 1.6243(18) . ? N1 C4 1.333(3) . ? N1 C6 1.449(3) . ? C1 C2 1.505(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N2 C2 1.335(3) . ? N2 C18 1.448(3) . ? C2 C3 1.402(3) . ? O2 C30 1.435(3) . ? O3 C34 1.443(3) . ? C3 C4 1.396(3) . ? C3 H3A 0.92(3) . ? C4 C5 1.506(3) . ? O4 C38 1.448(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.398(3) . ? C6 C7 1.412(3) . ? C7 C8 1.388(3) . ? C7 C15 1.522(4) . ? C8 C9 1.379(4) . ? C8 H8A 0.9500 . ? C9 C10 1.373(4) . ? C9 H9A 0.9500 . ? C10 C11 1.400(3) . ? C10 H10A 0.9500 . ? C11 C12 1.517(3) . ? C12 C14 1.525(4) . ? C12 C13 1.529(3) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.516(4) . ? C15 C17 1.530(4) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.405(3) . ? C18 C23 1.407(3) . ? C19 C20 1.396(3) . ? C19 C27 1.517(3) . ? C20 C21 1.367(4) . ? C20 H20A 0.9500 . ? C21 C22 1.377(4) . ? C21 H21A 0.9500 . ? C22 C23 1.396(3) . ? C22 H22A 0.9500 . ? C23 C24 1.517(3) . ? C24 C25 1.522(3) . ? C24 C26 1.525(3) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.509(4) . ? C27 C29 1.525(4) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.504(4) . ? C30 C33 1.519(4) . ? C30 C32 1.519(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.507(4) . ? C34 C35 1.511(4) . ? C34 C37 1.511(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C40 1.502(4) . ? C38 C41 1.503(4) . ? C38 C39 1.512(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 N1 112.04(8) . . ? O1 Al1 N2 114.58(9) . . ? N1 Al1 N2 95.81(9) . . ? O1 Al1 H1 115.7(9) . . ? N1 Al1 H1 108.8(8) . . ? N2 Al1 H1 108.0(8) . . ? O1 Si1 O2 112.74(9) . . ? O1 Si1 O4 113.82(9) . . ? O2 Si1 O4 105.19(9) . . ? O1 Si1 O3 106.36(9) . . ? O2 Si1 O3 112.36(9) . . ? O4 Si1 O3 106.32(9) . . ? C4 N1 C6 119.75(19) . . ? C4 N1 Al1 114.20(15) . . ? C6 N1 Al1 124.31(15) . . ? Si1 O1 Al1 138.48(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 N2 C18 118.56(19) . . ? C2 N2 Al1 114.08(15) . . ? C18 N2 Al1 126.17(15) . . ? N2 C2 C3 122.3(2) . . ? N2 C2 C1 120.2(2) . . ? C3 C2 C1 117.5(2) . . ? C30 O2 Si1 134.62(16) . . ? C34 O3 Si1 131.41(15) . . ? C4 C3 C2 127.4(2) . . ? C4 C3 H3A 116.2(15) . . ? C2 C3 H3A 115.7(15) . . ? N1 C4 C3 122.4(2) . . ? N1 C4 C5 120.7(2) . . ? C3 C4 C5 116.8(2) . . ? C38 O4 Si1 130.65(15) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.7(2) . . ? C11 C6 N1 119.5(2) . . ? C7 C6 N1 118.8(2) . . ? C8 C7 C6 117.8(2) . . ? C8 C7 C15 120.5(2) . . ? C6 C7 C15 121.7(2) . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 121.8(2) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C6 C11 C10 117.4(2) . . ? C6 C11 C12 123.7(2) . . ? C10 C11 C12 118.8(2) . . ? C11 C12 C14 110.3(2) . . ? C11 C12 C13 112.2(2) . . ? C14 C12 C13 110.6(2) . . ? C11 C12 H12A 107.9 . . ? C14 C12 H12A 107.9 . . ? C13 C12 H12A 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C7 111.8(2) . . ? C16 C15 C17 109.1(2) . . ? C7 C15 C17 113.6(2) . . ? C16 C15 H15A 107.3 . . ? C7 C15 H15A 107.3 . . ? C17 C15 H15A 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.1(2) . . ? C19 C18 N2 119.4(2) . . ? C23 C18 N2 119.5(2) . . ? C20 C19 C18 117.8(2) . . ? C20 C19 C27 119.6(2) . . ? C18 C19 C27 122.6(2) . . ? C21 C20 C19 121.9(2) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? C20 C21 C22 119.7(2) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C21 C22 C23 121.4(2) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C22 C23 C18 118.0(2) . . ? C22 C23 C24 119.1(2) . . ? C18 C23 C24 122.9(2) . . ? C23 C24 C25 110.6(2) . . ? C23 C24 C26 111.9(2) . . ? C25 C24 C26 110.7(2) . . ? C23 C24 H24A 107.8 . . ? C25 C24 H24A 107.8 . . ? C26 C24 H24A 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C19 112.3(2) . . ? C28 C27 C29 110.5(3) . . ? C19 C27 C29 111.6(2) . . ? C28 C27 H27A 107.4 . . ? C19 C27 H27A 107.4 . . ? C29 C27 H27A 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O2 C30 C31 107.7(2) . . ? O2 C30 C33 105.5(2) . . ? C31 C30 C33 111.3(3) . . ? O2 C30 C32 110.4(2) . . ? C31 C30 C32 110.8(3) . . ? C33 C30 C32 111.0(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 C34 C36 105.3(2) . . ? O3 C34 C35 110.5(2) . . ? C36 C34 C35 111.4(3) . . ? O3 C34 C37 108.8(2) . . ? C36 C34 C37 110.1(3) . . ? C35 C34 C37 110.6(2) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O4 C38 C40 109.1(2) . . ? O4 C38 C41 109.5(2) . . ? C40 C38 C41 111.6(3) . . ? O4 C38 C39 104.7(2) . . ? C40 C38 C39 110.6(2) . . ? C41 C38 C39 111.2(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 N1 C4 -165.50(16) . . . . ? N2 Al1 N1 C4 -46.02(17) . . . . ? O1 Al1 N1 C6 29.6(2) . . . . ? N2 Al1 N1 C6 149.09(18) . . . . ? O2 Si1 O1 Al1 152.04(14) . . . . ? O4 Si1 O1 Al1 -88.26(16) . . . . ? O3 Si1 O1 Al1 28.47(17) . . . . ? N1 Al1 O1 Si1 -135.62(14) . . . . ? N2 Al1 O1 Si1 116.61(15) . . . . ? O1 Al1 N2 C2 163.54(15) . . . . ? N1 Al1 N2 C2 46.06(17) . . . . ? O1 Al1 N2 C18 -29.2(2) . . . . ? N1 Al1 N2 C18 -146.66(18) . . . . ? C18 N2 C2 C3 169.7(2) . . . . ? Al1 N2 C2 C3 -22.0(3) . . . . ? C18 N2 C2 C1 -10.1(3) . . . . ? Al1 N2 C2 C1 158.25(18) . . . . ? O1 Si1 O2 C30 -44.2(3) . . . . ? O4 Si1 O2 C30 -168.8(2) . . . . ? O3 Si1 O2 C30 76.0(2) . . . . ? O1 Si1 O3 C34 -165.51(19) . . . . ? O2 Si1 O3 C34 70.7(2) . . . . ? O4 Si1 O3 C34 -43.9(2) . . . . ? N2 C2 C3 C4 -16.3(4) . . . . ? C1 C2 C3 C4 163.5(2) . . . . ? C6 N1 C4 C3 -172.6(2) . . . . ? Al1 N1 C4 C3 21.7(3) . . . . ? C6 N1 C4 C5 6.9(3) . . . . ? Al1 N1 C4 C5 -158.71(18) . . . . ? C2 C3 C4 N1 16.5(4) . . . . ? C2 C3 C4 C5 -163.1(2) . . . . ? O1 Si1 O4 C38 -77.0(2) . . . . ? O2 Si1 O4 C38 46.8(2) . . . . ? O3 Si1 O4 C38 166.20(19) . . . . ? C4 N1 C6 C11 -84.1(3) . . . . ? Al1 N1 C6 C11 80.0(3) . . . . ? C4 N1 C6 C7 96.8(3) . . . . ? Al1 N1 C6 C7 -99.0(2) . . . . ? C11 C6 C7 C8 0.8(3) . . . . ? N1 C6 C7 C8 179.9(2) . . . . ? C11 C6 C7 C15 -179.2(2) . . . . ? N1 C6 C7 C15 -0.2(3) . . . . ? C6 C7 C8 C9 -0.5(4) . . . . ? C15 C7 C8 C9 179.6(2) . . . . ? C7 C8 C9 C10 -0.4(4) . . . . ? C8 C9 C10 C11 0.9(4) . . . . ? C7 C6 C11 C10 -0.4(3) . . . . ? N1 C6 C11 C10 -179.4(2) . . . . ? C7 C6 C11 C12 178.2(2) . . . . ? N1 C6 C11 C12 -0.8(3) . . . . ? C9 C10 C11 C6 -0.5(4) . . . . ? C9 C10 C11 C12 -179.2(2) . . . . ? C6 C11 C12 C14 -107.9(3) . . . . ? C10 C11 C12 C14 70.7(3) . . . . ? C6 C11 C12 C13 128.4(3) . . . . ? C10 C11 C12 C13 -53.0(3) . . . . ? C8 C7 C15 C16 99.3(3) . . . . ? C6 C7 C15 C16 -80.7(3) . . . . ? C8 C7 C15 C17 -24.8(3) . . . . ? C6 C7 C15 C17 155.3(2) . . . . ? C2 N2 C18 C19 -89.2(3) . . . . ? Al1 N2 C18 C19 104.0(2) . . . . ? C2 N2 C18 C23 90.5(3) . . . . ? Al1 N2 C18 C23 -76.3(3) . . . . ? C23 C18 C19 C20 0.3(3) . . . . ? N2 C18 C19 C20 -180.0(2) . . . . ? C23 C18 C19 C27 -179.7(2) . . . . ? N2 C18 C19 C27 -0.1(3) . . . . ? C18 C19 C20 C21 1.0(4) . . . . ? C27 C19 C20 C21 -179.0(2) . . . . ? C19 C20 C21 C22 -0.9(4) . . . . ? C20 C21 C22 C23 -0.5(4) . . . . ? C21 C22 C23 C18 1.7(4) . . . . ? C21 C22 C23 C24 -179.0(2) . . . . ? C19 C18 C23 C22 -1.6(3) . . . . ? N2 C18 C23 C22 178.7(2) . . . . ? C19 C18 C23 C24 179.1(2) . . . . ? N2 C18 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C25 -70.3(3) . . . . ? C18 C23 C24 C25 108.9(3) . . . . ? C22 C23 C24 C26 53.6(3) . . . . ? C18 C23 C24 C26 -127.2(2) . . . . ? C20 C19 C27 C28 55.2(3) . . . . ? C18 C19 C27 C28 -124.7(3) . . . . ? C20 C19 C27 C29 -69.5(3) . . . . ? C18 C19 C27 C29 110.5(3) . . . . ? Si1 O2 C30 C31 85.4(3) . . . . ? Si1 O2 C30 C33 -155.6(2) . . . . ? Si1 O2 C30 C32 -35.7(3) . . . . ? Si1 O3 C34 C36 -162.2(2) . . . . ? Si1 O3 C34 C35 -41.8(3) . . . . ? Si1 O3 C34 C37 79.8(3) . . . . ? Si1 O4 C38 C40 -80.4(3) . . . . ? Si1 O4 C38 C41 42.0(3) . . . . ? Si1 O4 C38 C39 161.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.352 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.050 # Attachment 'compound6.cif' data_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 700778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H69 Al N2 O4 S Si' _chemical_formula_sum 'C41 H69 Al N2 O4 S Si' _chemical_formula_weight 741.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.068(2) _cell_length_b 19.698(3) _cell_length_c 18.023(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.72(2) _cell_angle_gamma 90.00 _cell_volume 4284(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5944 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.33 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details 'Sadabs, Sheldrick 1996' _exptl_special_details ; The intensities were measured with Bruker Apex CCD area detector ; _diffrn_ambient_temperature 173(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 Smart Apex CCD diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34989 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.37 _reflns_number_total 7829 _reflns_number_gt 5461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_data_reduction 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Due to the Cs symmetry of the molecule and the value of the beta angle (90.40(2)\%), Orthorhombic system could be plausible for this structure. However, the Cs symmetry is not retained in the solid state, and thus the crystal system was identified as monoclinic and the space group P2(1)/c was used to solve and refine the structure. ; _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^)+(0.0577P)^2^+1.2512P] 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 7829 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Si1 Si 0.46480(6) 0.24331(3) 0.61755(4) 0.01960(18) Uani 1 1 d . . . O4 O 0.49901(14) 0.16516(8) 0.63388(9) 0.0237(4) Uani 1 1 d . . . Al1 Al 0.23442(6) 0.25155(4) 0.53796(4) 0.01739(18) Uani 1 1 d . . . O3 O 0.51487(14) 0.28677(8) 0.68622(10) 0.0265(4) Uani 1 1 d . . . S1 S 0.29918(7) 0.24834(4) 0.42298(4) 0.0337(2) Uani 1 1 d . . . H1 H 0.389(3) 0.2529(14) 0.4363(17) 0.051 Uiso 1 1 d . . . O2 O 0.52090(14) 0.26366(9) 0.53889(10) 0.0256(4) Uani 1 1 d . . . N2 N 0.13456(16) 0.32609(10) 0.54336(11) 0.0192(5) Uani 1 1 d . . . O1 O 0.33401(13) 0.25420(8) 0.60590(9) 0.0227(4) Uani 1 1 d . . . N1 N 0.12731(16) 0.18131(10) 0.54502(11) 0.0194(5) Uani 1 1 d . . . C7 C 0.1557(2) 0.46806(14) 0.67940(15) 0.0305(7) Uani 1 1 d . . . H7A H 0.1354 0.4779 0.7290 0.037 Uiso 1 1 calc R . . C8 C 0.1602(2) 0.39182(12) 0.57542(14) 0.0208(6) Uani 1 1 d . . . C9 C 0.0428(2) 0.31912(12) 0.50164(14) 0.0202(6) Uani 1 1 d . . . C10 C 0.1079(2) 0.04256(13) 0.68558(15) 0.0299(6) Uani 1 1 d . . . H10A H 0.0763 0.0349 0.7328 0.036 Uiso 1 1 calc R . . C11 C 0.2099(2) 0.51675(14) 0.63861(16) 0.0329(7) Uani 1 1 d . . . H11A H 0.2260 0.5598 0.6600 0.039 Uiso 1 1 calc R . . C12 C 0.1408(2) 0.11555(12) 0.58137(14) 0.0209(6) Uani 1 1 d . . . C13 C 0.0057(2) 0.25541(13) 0.47644(14) 0.0227(6) Uani 1 1 d . . . H13A H -0.055(2) 0.2584(12) 0.4426(15) 0.027 Uiso 1 1 d . . . C14 C 0.1983(2) 0.06276(13) 0.54578(14) 0.0236(6) Uani 1 1 d . . . C15 C 0.2166(2) 0.44098(13) 0.53321(14) 0.0242(6) Uani 1 1 d . . . C16 C 0.0364(2) 0.19109(13) 0.50243(14) 0.0215(6) Uani 1 1 d . . . C17 C 0.2107(2) 0.00143(13) 0.58351(15) 0.0274(6) Uani 1 1 d . . . H17A H 0.2513 -0.0343 0.5611 0.033 Uiso 1 1 calc R . . C18 C 0.5041(2) 0.35587(13) 0.71127(15) 0.0274(6) Uani 1 1 d . . . C19 C 0.1303(2) 0.40503(13) 0.64950(15) 0.0249(6) Uani 1 1 d . . . C20 C 0.1658(2) -0.00866(14) 0.65202(16) 0.0313(7) Uani 1 1 d . . . H20A H 0.1748 -0.0511 0.6763 0.038 Uiso 1 1 calc R . . C21 C 0.0946(2) 0.10583(13) 0.65159(15) 0.0260(6) Uani 1 1 d . . . C22 C 0.2405(2) 0.50304(13) 0.56711(16) 0.0308(7) Uani 1 1 d . . . H22A H 0.2790 0.5367 0.5399 0.037 Uiso 1 1 calc R . . C23 C 0.0715(2) 0.35202(13) 0.69609(15) 0.0296(6) Uani 1 1 d . . . H23A H 0.1028 0.3067 0.6829 0.035 Uiso 1 1 calc R . . C24 C -0.0360(2) 0.13230(14) 0.48156(16) 0.0302(7) Uani 1 1 d . . . H24A H -0.0096 0.0914 0.5071 0.045 Uiso 0.50 1 calc PR . . H24B H -0.0335 0.1252 0.4278 0.045 Uiso 0.50 1 calc PR . . H24C H -0.1124 0.1418 0.4961 0.045 Uiso 0.50 1 calc PR . . H24D H -0.0941 0.1476 0.4469 0.045 Uiso 0.50 1 calc PR . . H24E H -0.0702 0.1137 0.5262 0.045 Uiso 0.50 1 calc PR . . H24F H 0.0087 0.0971 0.4579 0.045 Uiso 0.50 1 calc PR . . C25 C -0.0258(2) 0.37943(13) 0.47982(16) 0.0305(7) Uani 1 1 d . . . H25A H -0.0211 0.4139 0.5190 0.046 Uiso 0.50 1 calc PR . . H25B H -0.1032 0.3654 0.4728 0.046 Uiso 0.50 1 calc PR . . H25C H 0.0020 0.3984 0.4334 0.046 Uiso 0.50 1 calc PR . . H25D H -0.0604 0.3713 0.4312 0.046 Uiso 0.50 1 calc PR . . H25E H 0.0216 0.4197 0.4773 0.046 Uiso 0.50 1 calc PR . . H25F H -0.0835 0.3867 0.5168 0.046 Uiso 0.50 1 calc PR . . C26 C 0.4907(2) 0.12475(13) 0.70051(15) 0.0283(6) Uani 1 1 d . . . C27 C 0.6306(2) 0.25109(14) 0.51076(15) 0.0295(6) Uani 1 1 d . . . C28 C 0.0289(2) 0.16033(14) 0.69146(15) 0.0306(7) Uani 1 1 d . . . H28A H 0.0349 0.2032 0.6621 0.037 Uiso 1 1 calc R . . C29 C 0.2537(2) 0.42963(13) 0.45358(14) 0.0264(6) Uani 1 1 d . . . H29A H 0.2236 0.3850 0.4362 0.032 Uiso 1 1 calc R . . C30 C 0.6331(3) 0.17984(16) 0.47973(19) 0.0463(8) Uani 1 1 d . . . H30A H 0.6272 0.1471 0.5204 0.069 Uiso 1 1 calc R . . H30B H 0.7029 0.1726 0.4537 0.069 Uiso 1 1 calc R . . H30C H 0.5707 0.1736 0.4450 0.069 Uiso 1 1 calc R . . C31 C 0.2099(3) 0.48515(14) 0.40150(16) 0.0391(7) Uani 1 1 d . . . H31A H 0.1290 0.4873 0.4045 0.059 Uiso 1 1 calc R . . H31B H 0.2312 0.4747 0.3505 0.059 Uiso 1 1 calc R . . H31C H 0.2416 0.5290 0.4162 0.059 Uiso 1 1 calc R . . C32 C -0.0524(2) 0.35009(17) 0.67879(17) 0.0449(8) Uani 1 1 d . . . H32A H -0.0882 0.3171 0.7113 0.067 Uiso 1 1 calc R . . H32B H -0.0643 0.3368 0.6269 0.067 Uiso 1 1 calc R . . H32C H -0.0843 0.3952 0.6870 0.067 Uiso 1 1 calc R . . C33 C 0.6442(3) 0.30195(18) 0.44881(19) 0.0538(9) Uani 1 1 d . . . H33A H 0.6339 0.3479 0.4682 0.081 Uiso 1 1 calc R . . H33B H 0.5890 0.2931 0.4097 0.081 Uiso 1 1 calc R . . H33C H 0.7188 0.2978 0.4283 0.081 Uiso 1 1 calc R . . C34 C 0.3734(2) 0.07091(15) 0.47373(16) 0.0348(7) Uani 1 1 d . . . H34A H 0.3975 0.1075 0.5070 0.052 Uiso 1 1 calc R . . H34B H 0.4034 0.0786 0.4242 0.052 Uiso 1 1 calc R . . H34C H 0.4004 0.0273 0.4930 0.052 Uiso 1 1 calc R . . C35 C 0.0884(3) 0.36192(16) 0.77945(15) 0.0398(8) Uani 1 1 d . . . H35A H 0.0590 0.3225 0.8059 0.060 Uiso 1 1 calc R . . H35B H 0.0493 0.4029 0.7953 0.060 Uiso 1 1 calc R . . H35C H 0.1676 0.3667 0.7907 0.060 Uiso 1 1 calc R . . C36 C 0.2470(2) 0.06969(13) 0.46913(14) 0.0258(6) Uani 1 1 d . . . H36A H 0.2217 0.1140 0.4479 0.031 Uiso 1 1 calc R . . C37 C 0.0760(3) 0.17393(19) 0.76854(18) 0.0591(10) Uani 1 1 d . . . H37A H 0.1529 0.1895 0.7646 0.089 Uiso 1 1 calc R . . H37B H 0.0738 0.1321 0.7979 0.089 Uiso 1 1 calc R . . H37C H 0.0318 0.2090 0.7928 0.089 Uiso 1 1 calc R . . C38 C 0.2075(2) 0.01329(14) 0.41682(15) 0.0339(7) Uani 1 1 d . . . H38A H 0.1263 0.0127 0.4150 0.051 Uiso 1 1 calc R . . H38B H 0.2349 -0.0306 0.4350 0.051 Uiso 1 1 calc R . . H38C H 0.2360 0.0216 0.3670 0.051 Uiso 1 1 calc R . . C39 C 0.4942(3) 0.40350(15) 0.64543(17) 0.0474(9) Uani 1 1 d . . . H39A H 0.5585 0.3978 0.6134 0.071 Uiso 1 1 calc R . . H39B H 0.4911 0.4505 0.6631 0.071 Uiso 1 1 calc R . . H39C H 0.4263 0.3930 0.6172 0.071 Uiso 1 1 calc R . . C40 C 0.3798(2) 0.42658(15) 0.45097(16) 0.0371(7) Uani 1 1 d . . . H40A H 0.4065 0.3895 0.4827 0.056 Uiso 1 1 calc R . . H40B H 0.4108 0.4697 0.4687 0.056 Uiso 1 1 calc R . . H40C H 0.4030 0.4186 0.3998 0.056 Uiso 1 1 calc R . . C41 C 0.6080(3) 0.37020(18) 0.7562(2) 0.0617(11) Uani 1 1 d . . . H41A H 0.6729 0.3660 0.7244 0.093 Uiso 1 1 calc R . . H41B H 0.6140 0.3375 0.7971 0.093 Uiso 1 1 calc R . . H41C H 0.6045 0.4163 0.7764 0.093 Uiso 1 1 calc R . . C42 C 0.7174(2) 0.26043(18) 0.57056(18) 0.0503(9) Uani 1 1 d . . . H42A H 0.7022 0.2296 0.6119 0.075 Uiso 1 1 calc R . . H42B H 0.7158 0.3074 0.5883 0.075 Uiso 1 1 calc R . . H42C H 0.7906 0.2503 0.5504 0.075 Uiso 1 1 calc R . . C43 C -0.0931(3) 0.14213(17) 0.6962(2) 0.0540(9) Uani 1 1 d . . . H43A H -0.1234 0.1350 0.6461 0.081 Uiso 1 1 calc R . . H43B H -0.1332 0.1792 0.7202 0.081 Uiso 1 1 calc R . . H43C H -0.1014 0.1004 0.7252 0.081 Uiso 1 1 calc R . . C44 C 0.4014(3) 0.36031(17) 0.75779(18) 0.0507(9) Uani 1 1 d . . . H44A H 0.3366 0.3475 0.7277 0.076 Uiso 1 1 calc R . . H44B H 0.3924 0.4069 0.7757 0.076 Uiso 1 1 calc R . . H44C H 0.4085 0.3294 0.8002 0.076 Uiso 1 1 calc R . . C45 C 0.3801(3) 0.1380(2) 0.73652(18) 0.0584(10) Uani 1 1 d . . . H45A H 0.3781 0.1849 0.7549 0.088 Uiso 1 1 calc R . . H45B H 0.3704 0.1066 0.7781 0.088 Uiso 1 1 calc R . . H45C H 0.3204 0.1313 0.6999 0.088 Uiso 1 1 calc R . . C46 C 0.5854(3) 0.14182(18) 0.75230(18) 0.0518(9) Uani 1 1 d . . . H46A H 0.6558 0.1316 0.7281 0.078 Uiso 1 1 calc R . . H46B H 0.5794 0.1148 0.7977 0.078 Uiso 1 1 calc R . . H46C H 0.5828 0.1902 0.7648 0.078 Uiso 1 1 calc R . . C47 C 0.4983(3) 0.05210(15) 0.6748(2) 0.0619(11) Uani 1 1 d . . . H47A H 0.5670 0.0457 0.6472 0.093 Uiso 1 1 calc R . . H47B H 0.4346 0.0416 0.6425 0.093 Uiso 1 1 calc R . . H47C H 0.4982 0.0218 0.7179 0.093 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 Si1 0.0180(4) 0.0188(4) 0.0219(4) 0.0003(3) -0.0025(3) 0.0001(3) O4 0.0258(10) 0.0218(10) 0.0234(10) 0.0027(8) 0.0003(8) 0.0023(8) Al1 0.0172(4) 0.0150(4) 0.0199(4) -0.0007(3) 0.0001(3) 0.0001(3) O3 0.0295(10) 0.0217(10) 0.0282(10) -0.0028(8) -0.0069(8) -0.0003(8) S1 0.0457(5) 0.0278(4) 0.0279(4) -0.0007(3) 0.0114(3) 0.0005(3) O2 0.0209(9) 0.0279(10) 0.0279(10) 0.0048(8) -0.0010(8) -0.0006(8) N2 0.0183(11) 0.0169(11) 0.0223(12) -0.0002(9) -0.0025(9) 0.0019(9) O1 0.0204(9) 0.0234(10) 0.0243(9) -0.0018(8) -0.0011(7) 0.0002(8) N1 0.0217(11) 0.0151(11) 0.0213(12) -0.0002(9) -0.0014(9) 0.0007(9) C7 0.0363(16) 0.0277(16) 0.0273(15) -0.0067(12) -0.0017(12) 0.0040(13) C8 0.0193(13) 0.0187(13) 0.0244(14) -0.0022(11) -0.0042(11) 0.0046(11) C9 0.0184(13) 0.0212(14) 0.0210(14) 0.0005(11) 0.0019(11) 0.0025(11) C10 0.0323(16) 0.0306(16) 0.0269(15) 0.0063(13) 0.0026(12) -0.0047(13) C11 0.0400(17) 0.0214(15) 0.0371(18) -0.0083(13) -0.0070(14) -0.0012(13) C12 0.0196(13) 0.0183(13) 0.0247(14) 0.0023(11) -0.0052(11) -0.0045(11) C13 0.0181(13) 0.0287(15) 0.0212(14) -0.0002(12) -0.0046(11) 0.0030(11) C14 0.0233(14) 0.0190(14) 0.0284(15) -0.0014(11) -0.0021(11) -0.0048(11) C15 0.0255(14) 0.0180(13) 0.0288(15) 0.0007(11) -0.0061(12) 0.0034(11) C16 0.0189(13) 0.0234(14) 0.0223(14) -0.0015(11) 0.0001(11) -0.0029(11) C17 0.0282(15) 0.0191(14) 0.0346(16) 0.0009(12) -0.0027(12) -0.0006(11) C18 0.0311(15) 0.0209(14) 0.0301(16) -0.0048(12) -0.0058(12) -0.0019(12) C19 0.0229(14) 0.0240(14) 0.0278(15) -0.0007(12) -0.0035(11) 0.0042(11) C20 0.0357(16) 0.0217(15) 0.0363(17) 0.0079(13) -0.0033(13) -0.0043(12) C21 0.0261(14) 0.0224(14) 0.0295(16) -0.0012(12) -0.0014(12) -0.0051(11) C22 0.0345(16) 0.0205(15) 0.0374(17) -0.0008(13) -0.0019(13) -0.0035(12) C23 0.0371(16) 0.0227(15) 0.0290(16) -0.0050(12) 0.0052(12) 0.0022(12) C24 0.0250(15) 0.0284(16) 0.0370(17) -0.0019(13) -0.0068(12) -0.0047(12) C25 0.0278(15) 0.0263(15) 0.0372(17) 0.0015(13) -0.0066(13) 0.0051(12) C26 0.0327(15) 0.0260(15) 0.0261(15) 0.0073(12) -0.0039(12) -0.0008(12) C27 0.0197(14) 0.0378(17) 0.0311(15) 0.0020(13) 0.0065(11) -0.0028(12) C28 0.0382(17) 0.0259(15) 0.0280(16) 0.0022(12) 0.0080(13) -0.0024(13) C29 0.0328(16) 0.0201(14) 0.0263(15) -0.0005(11) -0.0014(12) -0.0035(12) C30 0.0362(18) 0.048(2) 0.055(2) -0.0100(17) 0.0141(16) 0.0014(15) C31 0.052(2) 0.0313(17) 0.0337(17) 0.0059(14) -0.0039(14) -0.0003(15) C32 0.0401(18) 0.057(2) 0.0373(18) -0.0005(16) 0.0034(14) -0.0123(16) C33 0.044(2) 0.064(2) 0.053(2) 0.0227(19) 0.0157(16) -0.0047(18) C34 0.0341(17) 0.0371(17) 0.0332(17) -0.0014(14) 0.0071(13) -0.0029(14) C35 0.0455(19) 0.0440(19) 0.0301(17) -0.0005(14) 0.0038(14) -0.0015(15) C36 0.0303(15) 0.0187(14) 0.0284(15) -0.0004(12) 0.0003(12) 0.0022(11) C37 0.068(2) 0.065(2) 0.044(2) -0.0227(18) -0.0059(18) 0.020(2) C38 0.0433(18) 0.0269(15) 0.0314(16) -0.0033(13) 0.0001(14) 0.0014(13) C39 0.074(2) 0.0271(17) 0.0411(19) -0.0014(15) 0.0029(17) -0.0004(16) C40 0.0414(18) 0.0388(18) 0.0312(17) -0.0024(14) 0.0051(14) -0.0031(14) C41 0.056(2) 0.046(2) 0.083(3) -0.028(2) -0.033(2) 0.0029(18) C42 0.0233(16) 0.080(3) 0.047(2) -0.0078(18) 0.0016(14) -0.0008(16) C43 0.0418(19) 0.044(2) 0.077(3) -0.0093(19) 0.0137(18) 0.0045(16) C44 0.058(2) 0.043(2) 0.051(2) -0.0119(17) 0.0136(17) -0.0015(17) C45 0.045(2) 0.086(3) 0.044(2) 0.033(2) 0.0113(16) 0.0055(19) C46 0.052(2) 0.055(2) 0.047(2) 0.0195(17) -0.0234(17) -0.0041(17) C47 0.105(3) 0.0264(18) 0.054(2) 0.0116(16) -0.007(2) 0.0026(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O1 1.6041(18) . ? Si1 O3 1.6157(18) . ? Si1 O4 1.6197(18) . ? Si1 O2 1.6288(19) . ? O4 C26 1.445(3) . ? Al1 O1 1.7058(18) . ? Al1 N1 1.899(2) . ? Al1 N2 1.903(2) . ? Al1 S1 2.2248(11) . ? O3 C18 1.441(3) . ? S1 H1 1.11(3) . ? O2 C27 1.445(3) . ? N2 C9 1.337(3) . ? N2 C8 1.450(3) . ? N1 C16 1.345(3) . ? N1 C12 1.460(3) . ? C7 C11 1.378(4) . ? C7 C19 1.386(4) . ? C7 H7A 0.9500 . ? C8 C19 1.411(4) . ? C8 C15 1.412(4) . ? C9 C13 1.406(4) . ? C9 C25 1.498(3) . ? C10 C20 1.372(4) . ? C10 C21 1.397(4) . ? C10 H10A 0.9500 . ? C11 C22 1.372(4) . ? C11 H11A 0.9500 . ? C12 C21 1.403(4) . ? C12 C14 1.409(3) . ? C13 C16 1.399(4) . ? C13 H13A 0.95(3) . ? C14 C17 1.393(4) . ? C14 C36 1.514(4) . ? C15 C22 1.395(4) . ? C15 C29 1.525(4) . ? C16 C24 1.496(3) . ? C17 C20 1.369(4) . ? C17 H17A 0.9500 . ? C18 C44 1.508(4) . ? C18 C41 1.511(4) . ? C18 C39 1.516(4) . ? C19 C23 1.521(4) . ? C20 H20A 0.9500 . ? C21 C28 1.520(4) . ? C22 H22A 0.9500 . ? C23 C32 1.524(4) . ? C23 C35 1.526(4) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? C26 C46 1.505(4) . ? C26 C47 1.508(4) . ? C26 C45 1.514(4) . ? C27 C42 1.505(4) . ? C27 C33 1.511(4) . ? C27 C30 1.511(4) . ? C28 C43 1.518(4) . ? C28 C37 1.518(4) . ? C28 H28A 1.0000 . ? C29 C40 1.524(4) . ? C29 C31 1.531(4) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.527(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.529(4) . ? C36 H36A 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 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 Si1 O3 112.79(10) . . ? O1 Si1 O4 113.52(9) . . ? O3 Si1 O4 105.80(9) . . ? O1 Si1 O2 105.79(9) . . ? O3 Si1 O2 112.38(10) . . ? O4 Si1 O2 106.51(9) . . ? C26 O4 Si1 130.85(16) . . ? O1 Al1 N1 116.63(9) . . ? O1 Al1 N2 112.37(9) . . ? N1 Al1 N2 97.28(9) . . ? O1 Al1 S1 114.64(7) . . ? N1 Al1 S1 106.80(7) . . ? N2 Al1 S1 107.45(7) . . ? C18 O3 Si1 134.96(16) . . ? Al1 S1 H1 98.6(16) . . ? C27 O2 Si1 130.99(16) . . ? C9 N2 C8 119.1(2) . . ? C9 N2 Al1 114.35(16) . . ? C8 N2 Al1 125.26(15) . . ? Si1 O1 Al1 140.64(12) . . ? C16 N1 C12 118.0(2) . . ? C16 N1 Al1 114.10(16) . . ? C12 N1 Al1 127.19(16) . . ? C11 C7 C19 121.3(3) . . ? C11 C7 H7A 119.3 . . ? C19 C7 H7A 119.3 . . ? C19 C8 C15 120.9(2) . . ? C19 C8 N2 119.1(2) . . ? C15 C8 N2 120.0(2) . . ? N2 C9 C13 122.1(2) . . ? N2 C9 C25 121.2(2) . . ? C13 C9 C25 116.7(2) . . ? C20 C10 C21 121.3(3) . . ? C20 C10 H10A 119.4 . . ? C21 C10 H10A 119.4 . . ? C22 C11 C7 119.9(3) . . ? C22 C11 H11A 120.0 . . ? C7 C11 H11A 120.0 . . ? C21 C12 C14 120.9(2) . . ? C21 C12 N1 118.9(2) . . ? C14 C12 N1 120.2(2) . . ? C16 C13 C9 128.2(2) . . ? C16 C13 H13A 118.0(15) . . ? C9 C13 H13A 113.2(15) . . ? C17 C14 C12 117.9(2) . . ? C17 C14 C36 118.9(2) . . ? C12 C14 C36 123.2(2) . . ? C22 C15 C8 117.6(2) . . ? C22 C15 C29 118.6(2) . . ? C8 C15 C29 123.8(2) . . ? N1 C16 C13 122.1(2) . . ? N1 C16 C24 120.2(2) . . ? C13 C16 C24 117.7(2) . . ? C20 C17 C14 121.7(3) . . ? C20 C17 H17A 119.2 . . ? C14 C17 H17A 119.2 . . ? O3 C18 C44 107.9(2) . . ? O3 C18 C41 105.5(2) . . ? C44 C18 C41 111.9(3) . . ? O3 C18 C39 110.2(2) . . ? C44 C18 C39 110.0(3) . . ? C41 C18 C39 111.2(3) . . ? C7 C19 C8 118.4(2) . . ? C7 C19 C23 120.2(2) . . ? C8 C19 C23 121.5(2) . . ? C17 C20 C10 120.0(3) . . ? C17 C20 H20A 120.0 . . ? C10 C20 H20A 120.0 . . ? C10 C21 C12 118.2(2) . . ? C10 C21 C28 118.7(2) . . ? C12 C21 C28 123.1(2) . . ? C11 C22 C15 121.8(3) . . ? C11 C22 H22A 119.1 . . ? C15 C22 H22A 119.1 . . ? C19 C23 C32 111.6(2) . . ? C19 C23 C35 113.5(2) . . ? C32 C23 C35 108.8(2) . . ? C19 C23 H23A 107.6 . . ? C32 C23 H23A 107.6 . . ? C35 C23 H23A 107.6 . . ? C16 C24 H24A 109.5 . . ? C16 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C16 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C16 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? C16 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C16 C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C9 C25 H25A 109.5 . . ? C9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C9 C25 H25D 109.5 . . ? H25A C25 H25D 141.1 . . ? H25B C25 H25D 56.3 . . ? H25C C25 H25D 56.3 . . ? C9 C25 H25E 109.5 . . ? H25A C25 H25E 56.3 . . ? H25B C25 H25E 141.1 . . ? H25C C25 H25E 56.3 . . ? H25D C25 H25E 109.5 . . ? C9 C25 H25F 109.5 . . ? H25A C25 H25F 56.3 . . ? H25B C25 H25F 56.3 . . ? H25C C25 H25F 141.1 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? O4 C26 C46 109.4(2) . . ? O4 C26 C47 105.2(2) . . ? C46 C26 C47 110.7(3) . . ? O4 C26 C45 109.4(2) . . ? C46 C26 C45 111.3(3) . . ? C47 C26 C45 110.7(3) . . ? O2 C27 C42 111.1(2) . . ? O2 C27 C33 104.8(2) . . ? C42 C27 C33 111.5(3) . . ? O2 C27 C30 108.2(2) . . ? C42 C27 C30 111.2(3) . . ? C33 C27 C30 109.8(3) . . ? C43 C28 C37 110.0(3) . . ? C43 C28 C21 111.8(2) . . ? C37 C28 C21 111.4(2) . . ? C43 C28 H28A 107.8 . . ? C37 C28 H28A 107.8 . . ? C21 C28 H28A 107.8 . . ? C40 C29 C15 109.9(2) . . ? C40 C29 C31 110.2(2) . . ? C15 C29 C31 111.7(2) . . ? C40 C29 H29A 108.3 . . ? C15 C29 H29A 108.3 . . ? C31 C29 H29A 108.3 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 C32 H32A 109.5 . . ? C23 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C23 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 H34A 109.5 . . ? C36 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C36 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C23 C35 H35A 109.5 . . ? C23 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C23 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C14 C36 C34 110.5(2) . . ? C14 C36 C38 112.0(2) . . ? C34 C36 C38 110.4(2) . . ? C14 C36 H36A 107.9 . . ? C34 C36 H36A 107.9 . . ? C38 C36 H36A 107.9 . . ? C28 C37 H37A 109.5 . . ? C28 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C28 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C18 C39 H39A 109.5 . . ? C18 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C18 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C29 C40 H40A 109.5 . . ? C29 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C29 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C18 C41 H41A 109.5 . . ? C18 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C18 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C27 C42 H42A 109.5 . . ? C27 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C27 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C28 C43 H43A 109.5 . . ? C28 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C28 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C18 C44 H44A 109.5 . . ? C18 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C18 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C26 C45 H45A 109.5 . . ? C26 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C26 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C26 C46 H46A 109.5 . . ? C26 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C26 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C26 C47 H47A 109.5 . . ? C26 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C26 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 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 O1 Si1 O4 C26 -76.9(2) . . . . ? O3 Si1 O4 C26 47.3(2) . . . . ? O2 Si1 O4 C26 167.1(2) . . . . ? O1 Si1 O3 C18 -46.3(3) . . . . ? O4 Si1 O3 C18 -170.9(2) . . . . ? O2 Si1 O3 C18 73.2(2) . . . . ? O1 Si1 O2 C27 -165.4(2) . . . . ? O3 Si1 O2 C27 71.1(2) . . . . ? O4 Si1 O2 C27 -44.3(2) . . . . ? O1 Al1 N2 C9 -166.90(16) . . . . ? N1 Al1 N2 C9 -44.13(18) . . . . ? S1 Al1 N2 C9 66.09(18) . . . . ? O1 Al1 N2 C8 26.1(2) . . . . ? N1 Al1 N2 C8 148.84(19) . . . . ? S1 Al1 N2 C8 -100.94(19) . . . . ? O3 Si1 O1 Al1 152.77(16) . . . . ? O4 Si1 O1 Al1 -86.90(18) . . . . ? O2 Si1 O1 Al1 29.54(19) . . . . ? N1 Al1 O1 Si1 112.48(17) . . . . ? N2 Al1 O1 Si1 -136.44(16) . . . . ? S1 Al1 O1 Si1 -13.4(2) . . . . ? O1 Al1 N1 C16 164.07(16) . . . . ? N2 Al1 N1 C16 44.51(18) . . . . ? S1 Al1 N1 C16 -66.24(17) . . . . ? O1 Al1 N1 C12 -26.1(2) . . . . ? N2 Al1 N1 C12 -145.6(2) . . . . ? S1 Al1 N1 C12 103.61(19) . . . . ? C9 N2 C8 C19 97.1(3) . . . . ? Al1 N2 C8 C19 -96.4(2) . . . . ? C9 N2 C8 C15 -84.3(3) . . . . ? Al1 N2 C8 C15 82.1(3) . . . . ? C8 N2 C9 C13 -172.0(2) . . . . ? Al1 N2 C9 C13 20.1(3) . . . . ? C8 N2 C9 C25 7.7(3) . . . . ? Al1 N2 C9 C25 -160.23(19) . . . . ? C19 C7 C11 C22 -0.5(4) . . . . ? C16 N1 C12 C21 -88.3(3) . . . . ? Al1 N1 C12 C21 102.2(2) . . . . ? C16 N1 C12 C14 90.9(3) . . . . ? Al1 N1 C12 C14 -78.6(3) . . . . ? N2 C9 C13 C16 16.7(4) . . . . ? C25 C9 C13 C16 -163.0(3) . . . . ? C21 C12 C14 C17 -2.0(4) . . . . ? N1 C12 C14 C17 178.8(2) . . . . ? C21 C12 C14 C36 178.2(2) . . . . ? N1 C12 C14 C36 -1.1(4) . . . . ? C19 C8 C15 C22 -0.6(4) . . . . ? N2 C8 C15 C22 -179.2(2) . . . . ? C19 C8 C15 C29 178.6(2) . . . . ? N2 C8 C15 C29 0.0(4) . . . . ? C12 N1 C16 C13 168.1(2) . . . . ? Al1 N1 C16 C13 -21.0(3) . . . . ? C12 N1 C16 C24 -11.6(3) . . . . ? Al1 N1 C16 C24 159.25(19) . . . . ? C9 C13 C16 N1 -16.1(4) . . . . ? C9 C13 C16 C24 163.6(3) . . . . ? C12 C14 C17 C20 2.1(4) . . . . ? C36 C14 C17 C20 -178.1(2) . . . . ? Si1 O3 C18 C44 84.7(3) . . . . ? Si1 O3 C18 C41 -155.5(2) . . . . ? Si1 O3 C18 C39 -35.4(3) . . . . ? C11 C7 C19 C8 -0.7(4) . . . . ? C11 C7 C19 C23 179.4(2) . . . . ? C15 C8 C19 C7 1.3(4) . . . . ? N2 C8 C19 C7 179.8(2) . . . . ? C15 C8 C19 C23 -178.8(2) . . . . ? N2 C8 C19 C23 -0.3(4) . . . . ? C14 C17 C20 C10 -0.7(4) . . . . ? C21 C10 C20 C17 -0.8(4) . . . . ? C20 C10 C21 C12 0.8(4) . . . . ? C20 C10 C21 C28 179.6(2) . . . . ? C14 C12 C21 C10 0.6(4) . . . . ? N1 C12 C21 C10 179.8(2) . . . . ? C14 C12 C21 C28 -178.1(2) . . . . ? N1 C12 C21 C28 1.1(4) . . . . ? C7 C11 C22 C15 1.2(4) . . . . ? C8 C15 C22 C11 -0.6(4) . . . . ? C29 C15 C22 C11 -179.9(2) . . . . ? C7 C19 C23 C32 99.2(3) . . . . ? C8 C19 C23 C32 -80.7(3) . . . . ? C7 C19 C23 C35 -24.2(4) . . . . ? C8 C19 C23 C35 155.9(2) . . . . ? Si1 O4 C26 C46 -79.8(3) . . . . ? Si1 O4 C26 C47 161.2(2) . . . . ? Si1 O4 C26 C45 42.3(3) . . . . ? Si1 O2 C27 C42 -40.4(3) . . . . ? Si1 O2 C27 C33 -160.9(2) . . . . ? Si1 O2 C27 C30 81.9(3) . . . . ? C10 C21 C28 C43 -67.8(3) . . . . ? C12 C21 C28 C43 110.9(3) . . . . ? C10 C21 C28 C37 55.8(3) . . . . ? C12 C21 C28 C37 -125.5(3) . . . . ? C22 C15 C29 C40 67.5(3) . . . . ? C8 C15 C29 C40 -111.7(3) . . . . ? C22 C15 C29 C31 -55.1(3) . . . . ? C8 C15 C29 C31 125.7(3) . . . . ? C17 C14 C36 C34 -69.8(3) . . . . ? C12 C14 C36 C34 110.1(3) . . . . ? C17 C14 C36 C38 53.8(3) . . . . ? C12 C14 C36 C38 -126.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A S1 H1 O2 1.11(3) 2.43(3) 3.387(2) 143(2) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.437 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.055 # Attachment 'compound7.cif' data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 700779' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H69 Al N2 O4.92 Si' _chemical_formula_sum 'C41 H69 Al N2 O4.92 Si' _chemical_formula_weight 723.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.061(2) _cell_length_b 19.651(3) _cell_length_c 18.008(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.24(2) _cell_angle_gamma 90.00 _cell_volume 4268(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.31 _exptl_crystal_description plate _exptl_crystal_colour colorles _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1581 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details 'Sadabs, Sheldrick 1996' _exptl_special_details ; The intensities were measured with Bruker Apex CCD area detector ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44646 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7520 _reflns_number_gt 5827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the Cs symmetry of the molecule and the value of the beta angle (90.40(2)\%), Orthorhombic system could be plausible for this structure. However, the Cs symmetry is not retained in the solid state, and thus the crystal system was identified as monoclinic and the space group P2(1)/c was used to solve and refine the structure. The methyl groups (C35, C36, C37) from the tBu moiety are disordered over two positions and refined with the ocupancy ratio (0.727:0.263). The OH group attached to the aluminum center is disordered with residual hydridic atom, which could not be localized, owing to its low ocupancy (0.079). ; _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^)+(0.0706P)^2^+1.1654P] 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 7520 _refine_ls_number_parameters 517 _refine_ls_number_restraints 140 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.23370(5) 0.74920(3) 0.03967(3) 0.02034(16) Uani 1 1 d . . . N1 N 0.13278(13) 0.67497(8) 0.04354(9) 0.0224(4) Uani 1 1 d . A . O1 O 0.32900(11) 0.74729(6) 0.11075(8) 0.0261(3) Uani 1 1 d . A . C1 C -0.03700(18) 0.86878(11) -0.01778(13) 0.0348(5) Uani 1 1 d . A . H1A H 0.0084 0.9037 -0.0419 0.052 Uiso 1 1 calc R . . H1B H -0.0709 0.8879 0.0270 0.052 Uiso 1 1 calc R . . H1C H -0.0953 0.8537 -0.0520 0.052 Uiso 1 1 calc R . . N2 N 0.12497(13) 0.81899(8) 0.04560(9) 0.0217(4) Uani 1 1 d . A . O5 O 0.29073(14) 0.75248(8) -0.04677(9) 0.0347(6) Uani 0.921(6) 1 d PD A 1 H5 H 0.3595(9) 0.7490(13) -0.0505(17) 0.052 Uiso 0.921(6) 1 d PD A 1 C2 C 0.03458(16) 0.80946(10) 0.00305(11) 0.0235(4) Uani 1 1 d . . . C3 C 0.00283(17) 0.74515(10) -0.02230(12) 0.0253(5) Uani 1 1 d . A . H3A H -0.0569(19) 0.7440(10) -0.0578(12) 0.030 Uiso 1 1 d . . . O4 O 0.51415(11) 0.73748(7) 0.03939(8) 0.0276(3) Uani 1 1 d . . . C4 C 0.04134(16) 0.68182(10) 0.00159(11) 0.0247(4) Uani 1 1 d . . . O2 O 0.49654(11) 0.83659(7) 0.13369(7) 0.0260(3) Uani 1 1 d . . . C5 C -0.02587(18) 0.62040(11) -0.02056(13) 0.0343(5) Uani 1 1 d . A . H5A H -0.0346 0.5903 0.0224 0.051 Uiso 1 1 calc R . . H5B H 0.0123 0.5959 -0.0603 0.051 Uiso 1 1 calc R . . H5C H -0.0991 0.6351 -0.0382 0.051 Uiso 1 1 calc R . . C6 C 0.15926(16) 0.60922(10) 0.07485(11) 0.0246(4) Uani 1 1 d . . . C7 C 0.12782(17) 0.59550(10) 0.14876(12) 0.0283(5) Uani 1 1 d . A . C8 C 0.15421(18) 0.53208(11) 0.17787(12) 0.0338(5) Uani 1 1 d . . . H8A H 0.1328 0.5215 0.2272 0.041 Uiso 1 1 calc R A . C9 C 0.21070(19) 0.48416(11) 0.13696(13) 0.0357(5) Uani 1 1 d . A . H9A H 0.2276 0.4411 0.1581 0.043 Uiso 1 1 calc R . . C10 C 0.24257(18) 0.49882(11) 0.06562(13) 0.0327(5) Uani 1 1 d . . . H10A H 0.2825 0.4658 0.0381 0.039 Uiso 1 1 calc R A . C11 C 0.21747(16) 0.56128(10) 0.03275(11) 0.0272(5) Uani 1 1 d . A . C12 C 0.25635(17) 0.57468(11) -0.04630(12) 0.0305(5) Uani 1 1 d . . . H12A H 0.2244 0.6190 -0.0631 0.037 Uiso 1 1 calc R A . C13 C 0.38330(19) 0.58047(13) -0.04753(13) 0.0424(6) Uani 1 1 d . A . H13A H 0.4069 0.6175 -0.0147 0.064 Uiso 1 1 calc R . . H13B H 0.4079 0.5900 -0.0983 0.064 Uiso 1 1 calc R . . H13C H 0.4161 0.5376 -0.0304 0.064 Uiso 1 1 calc R . . C14 C 0.2176(2) 0.51912(12) -0.09988(13) 0.0420(6) Uani 1 1 d . A . H14A H 0.1368 0.5146 -0.0970 0.063 Uiso 1 1 calc R . . H14B H 0.2524 0.4758 -0.0863 0.063 Uiso 1 1 calc R . . H14C H 0.2387 0.5314 -0.1506 0.063 Uiso 1 1 calc R . . C15 C 0.06611(19) 0.64761(11) 0.19538(12) 0.0352(5) Uani 1 1 d . . . H15A H 0.0961 0.6935 0.1825 0.042 Uiso 1 1 calc R A . C16 C 0.0820(2) 0.63758(13) 0.27894(13) 0.0456(6) Uani 1 1 d . A . H16A H 0.1614 0.6351 0.2905 0.068 Uiso 1 1 calc R . . H16B H 0.0458 0.5952 0.2943 0.068 Uiso 1 1 calc R . . H16C H 0.0490 0.6760 0.3056 0.068 Uiso 1 1 calc R . . C17 C -0.0575(2) 0.64803(15) 0.17784(15) 0.0536(7) Uani 1 1 d . A . H17A H -0.0688 0.6598 0.1255 0.080 Uiso 1 1 calc R . . H17B H -0.0946 0.6817 0.2092 0.080 Uiso 1 1 calc R . . H17C H -0.0886 0.6028 0.1875 0.080 Uiso 1 1 calc R . . C18 C 0.14003(16) 0.88487(10) 0.08080(11) 0.0233(4) Uani 1 1 d . . . C19 C 0.09439(17) 0.89551(10) 0.15166(11) 0.0276(5) Uani 1 1 d . A . C20 C 0.10932(18) 0.95917(11) 0.18455(12) 0.0329(5) Uani 1 1 d . . . H20A H 0.0779 0.9677 0.2319 0.040 Uiso 1 1 calc R A . C21 C 0.16851(18) 1.01003(11) 0.14999(12) 0.0332(5) Uani 1 1 d . A . H21A H 0.1785 1.0528 0.1737 0.040 Uiso 1 1 calc R . . C22 C 0.21315(18) 0.99839(10) 0.08082(12) 0.0304(5) Uani 1 1 d . . . H22A H 0.2544 1.0335 0.0574 0.037 Uiso 1 1 calc R A . C23 C 0.19914(16) 0.93634(10) 0.04440(11) 0.0259(5) Uani 1 1 d . A . C24 C 0.24890(17) 0.92722(10) -0.03237(11) 0.0283(5) Uani 1 1 d . . . H24A H 0.2231 0.8825 -0.0524 0.034 Uiso 1 1 calc R A . C25 C 0.37523(18) 0.92545(12) -0.02757(13) 0.0381(6) Uani 1 1 d . A . H25A H 0.3983 0.8895 0.0069 0.057 Uiso 1 1 calc R . . H25B H 0.4026 0.9695 -0.0097 0.057 Uiso 1 1 calc R . . H25C H 0.4059 0.9162 -0.0769 0.057 Uiso 1 1 calc R . . C26 C 0.2106(2) 0.98299(11) -0.08603(12) 0.0364(5) Uani 1 1 d . A . H26A H 0.1294 0.9840 -0.0878 0.055 Uiso 1 1 calc R . . H26B H 0.2395 0.9735 -0.1358 0.055 Uiso 1 1 calc R . . H26C H 0.2383 1.0272 -0.0689 0.055 Uiso 1 1 calc R . . C27 C 0.02908(19) 0.84107(11) 0.19251(12) 0.0354(5) Uani 1 1 d . . . H27A H 0.0363 0.7976 0.1640 0.042 Uiso 1 1 calc R A . C28 C 0.0746(3) 0.82897(18) 0.26966(16) 0.0742(10) Uani 1 1 d . A . H28A H 0.1517 0.8136 0.2663 0.111 Uiso 1 1 calc R . . H28B H 0.0301 0.7941 0.2945 0.111 Uiso 1 1 calc R . . H28C H 0.0714 0.8714 0.2982 0.111 Uiso 1 1 calc R . . C29 C -0.0932(2) 0.85896(15) 0.19609(19) 0.0652(9) Uani 1 1 d . A . H29A H -0.1224 0.8648 0.1456 0.098 Uiso 1 1 calc R . . H29B H -0.1026 0.9014 0.2240 0.098 Uiso 1 1 calc R . . H29C H -0.1336 0.8222 0.2210 0.098 Uiso 1 1 calc R . . C30 C 0.49762(19) 0.64768(11) 0.21561(13) 0.0364(5) Uani 1 1 d . B . C31 C 0.3968(2) 0.64828(16) 0.26457(16) 0.0645(8) Uani 1 1 d . . . H31A H 0.4082 0.6806 0.3053 0.097 Uiso 1 1 calc R . . H31B H 0.3848 0.6026 0.2849 0.097 Uiso 1 1 calc R . . H31C H 0.3319 0.6620 0.2353 0.097 Uiso 1 1 calc R . . C32 C 0.4817(2) 0.59765(12) 0.15260(15) 0.0548(7) Uani 1 1 d . . . H32A H 0.4117 0.6074 0.1269 0.082 Uiso 1 1 calc R . . H32B H 0.4799 0.5512 0.1725 0.082 Uiso 1 1 calc R . . H32C H 0.5433 0.6019 0.1176 0.082 Uiso 1 1 calc R . . C33 C 0.6019(2) 0.63208(14) 0.25961(16) 0.0582(8) Uani 1 1 d . . . H33A H 0.6131 0.6672 0.2975 0.087 Uiso 1 1 calc R . . H33B H 0.6657 0.6313 0.2261 0.087 Uiso 1 1 calc R . . H33C H 0.5943 0.5876 0.2837 0.087 Uiso 1 1 calc R . . Si1 Si 0.46014(4) 0.75819(3) 0.11904(3) 0.02146(15) Uani 1 1 d D A . O3 O 0.51324(11) 0.71525(7) 0.18707(8) 0.0300(4) Uani 1 1 d . . . C34 C 0.6240(8) 0.7479(5) 0.0102(5) 0.0315(11) Uani 0.73(3) 1 d PDU B 1 C35 C 0.6348(9) 0.7003(5) -0.0556(6) 0.0485(18) Uani 0.73(3) 1 d PDU B 1 H35A H 0.5804 0.7128 -0.0938 0.073 Uiso 0.73(3) 1 calc PR B 1 H35B H 0.6214 0.6534 -0.0394 0.073 Uiso 0.73(3) 1 calc PR B 1 H35C H 0.7097 0.7038 -0.0761 0.073 Uiso 0.73(3) 1 calc PR B 1 C36 C 0.7115(11) 0.7311(7) 0.0687(6) 0.0461(18) Uani 0.73(3) 1 d PDU B 1 H36A H 0.7011 0.7605 0.1121 0.069 Uiso 0.73(3) 1 calc PR B 1 H36B H 0.7855 0.7387 0.0480 0.069 Uiso 0.73(3) 1 calc PR B 1 H36C H 0.7041 0.6834 0.0837 0.069 Uiso 0.73(3) 1 calc PR B 1 C37 C 0.6373(12) 0.8213(4) -0.0150(7) 0.0441(18) Uani 0.73(3) 1 d PDU B 1 H37A H 0.6340 0.8515 0.0283 0.066 Uiso 0.73(3) 1 calc PR B 1 H37B H 0.5774 0.8329 -0.0497 0.066 Uiso 0.73(3) 1 calc PR B 1 H37C H 0.7089 0.8267 -0.0397 0.066 Uiso 0.73(3) 1 calc PR B 1 C34A C 0.628(2) 0.7475(12) 0.0135(12) 0.035(3) Uani 0.27(3) 1 d PDU B 2 C35A C 0.646(3) 0.6856(12) -0.0349(17) 0.050(4) Uani 0.27(3) 1 d PDU B 2 H35D H 0.6429 0.6444 -0.0043 0.075 Uiso 0.27(3) 1 calc PR B 2 H35E H 0.7193 0.6887 -0.0584 0.075 Uiso 0.27(3) 1 calc PR B 2 H35F H 0.5887 0.6836 -0.0734 0.075 Uiso 0.27(3) 1 calc PR B 2 C36A C 0.710(3) 0.7514(14) 0.0771(13) 0.039(4) Uani 0.27(3) 1 d PDU B 2 H36D H 0.6939 0.7911 0.1080 0.059 Uiso 0.27(3) 1 calc PR B 2 H36E H 0.7856 0.7555 0.0571 0.059 Uiso 0.27(3) 1 calc PR B 2 H36F H 0.7053 0.7100 0.1072 0.059 Uiso 0.27(3) 1 calc PR B 2 C37A C 0.624(3) 0.8128(13) -0.0311(17) 0.045(4) Uani 0.27(3) 1 d PDU B 2 H37D H 0.6036 0.8507 0.0016 0.067 Uiso 0.27(3) 1 calc PR B 2 H37E H 0.5680 0.8085 -0.0707 0.067 Uiso 0.27(3) 1 calc PR B 2 H37F H 0.6964 0.8215 -0.0531 0.067 Uiso 0.27(3) 1 calc PR B 2 C38 C 0.49026(18) 0.87794(11) 0.19953(12) 0.0336(5) Uani 1 1 d . B . C39 C 0.5861(2) 0.86109(14) 0.25014(15) 0.0533(7) Uani 1 1 d . . . H39A H 0.5823 0.8130 0.2644 0.080 Uiso 1 1 calc R B . H39B H 0.5825 0.8896 0.2947 0.080 Uiso 1 1 calc R . . H39C H 0.6560 0.8697 0.2242 0.080 Uiso 1 1 calc R . . C40 C 0.4985(3) 0.95038(13) 0.17204(17) 0.0734(10) Uani 1 1 d . . . H40A H 0.5674 0.9561 0.1440 0.110 Uiso 1 1 calc R B . H40B H 0.4986 0.9816 0.2145 0.110 Uiso 1 1 calc R . . H40C H 0.4350 0.9605 0.1398 0.110 Uiso 1 1 calc R . . C41 C 0.3812(2) 0.86612(18) 0.23723(16) 0.0708(10) Uani 1 1 d . . . H41A H 0.3791 0.8198 0.2572 0.106 Uiso 1 1 calc R B . H41B H 0.3207 0.8720 0.2012 0.106 Uiso 1 1 calc R . . H41C H 0.3724 0.8989 0.2778 0.106 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0185(3) 0.0184(3) 0.0240(3) 0.0009(2) -0.0005(2) -0.0005(2) N1 0.0206(9) 0.0192(8) 0.0274(9) 0.0013(7) -0.0023(7) -0.0023(7) O1 0.0213(7) 0.0271(8) 0.0299(8) 0.0017(6) -0.0022(6) -0.0016(6) C1 0.0273(12) 0.0316(12) 0.0455(14) 0.0001(10) -0.0095(10) 0.0069(9) N2 0.0195(8) 0.0194(8) 0.0263(9) 0.0003(7) -0.0011(7) 0.0011(7) O5 0.0333(10) 0.0386(11) 0.0322(10) 0.0013(7) 0.0039(8) 0.0011(8) C2 0.0209(10) 0.0256(11) 0.0240(10) 0.0027(8) -0.0001(8) 0.0019(8) C3 0.0191(10) 0.0297(12) 0.0270(11) -0.0004(9) -0.0050(9) -0.0008(8) O4 0.0211(7) 0.0324(8) 0.0293(8) -0.0043(6) 0.0011(6) -0.0011(6) C4 0.0219(10) 0.0257(11) 0.0264(11) -0.0014(8) 0.0011(8) -0.0036(8) O2 0.0275(8) 0.0226(8) 0.0278(8) -0.0025(6) -0.0002(6) -0.0024(6) C5 0.0296(12) 0.0295(12) 0.0436(13) -0.0012(10) -0.0088(10) -0.0063(9) C6 0.0232(10) 0.0189(10) 0.0316(11) 0.0022(8) -0.0065(9) -0.0045(8) C7 0.0267(11) 0.0263(11) 0.0318(12) 0.0039(9) -0.0029(9) -0.0055(9) C8 0.0383(13) 0.0282(12) 0.0347(12) 0.0079(10) -0.0026(10) -0.0054(10) C9 0.0403(13) 0.0213(11) 0.0454(14) 0.0093(10) -0.0089(11) -0.0007(10) C10 0.0341(12) 0.0213(11) 0.0427(13) -0.0003(9) -0.0026(10) 0.0029(9) C11 0.0250(11) 0.0229(11) 0.0337(12) 0.0001(9) -0.0050(9) -0.0043(9) C12 0.0347(12) 0.0239(11) 0.0329(12) -0.0011(9) -0.0007(10) 0.0002(9) C13 0.0399(14) 0.0473(15) 0.0400(14) -0.0014(11) 0.0041(11) -0.0061(11) C14 0.0552(16) 0.0347(13) 0.0361(13) -0.0059(10) -0.0035(11) -0.0019(11) C15 0.0439(14) 0.0283(12) 0.0334(12) 0.0056(10) 0.0073(10) -0.0006(10) C16 0.0497(15) 0.0494(16) 0.0378(14) 0.0016(11) 0.0075(11) -0.0019(12) C17 0.0443(15) 0.0689(19) 0.0477(16) 0.0013(14) 0.0062(12) 0.0205(14) C18 0.0204(10) 0.0204(10) 0.0291(11) -0.0010(8) -0.0030(8) 0.0055(8) C19 0.0242(11) 0.0263(11) 0.0324(12) 0.0000(9) 0.0001(9) 0.0056(9) C20 0.0328(12) 0.0329(12) 0.0331(12) -0.0073(10) 0.0014(10) 0.0079(10) C21 0.0348(12) 0.0240(11) 0.0408(13) -0.0083(10) -0.0073(10) 0.0031(9) C22 0.0303(12) 0.0225(11) 0.0384(12) -0.0005(9) -0.0026(10) 0.0017(9) C23 0.0230(10) 0.0233(11) 0.0314(11) 0.0008(9) -0.0045(9) 0.0037(8) C24 0.0334(12) 0.0215(11) 0.0299(11) 0.0013(9) 0.0002(9) -0.0005(9) C25 0.0348(13) 0.0419(14) 0.0377(13) 0.0061(11) 0.0049(10) 0.0043(10) C26 0.0436(14) 0.0302(12) 0.0354(13) 0.0040(10) -0.0030(11) 0.0003(10) C27 0.0414(14) 0.0282(12) 0.0366(13) -0.0035(10) 0.0106(10) 0.0012(10) C28 0.079(2) 0.090(2) 0.0534(18) 0.0343(17) -0.0070(16) -0.0280(19) C29 0.0402(16) 0.0586(19) 0.097(2) 0.0133(17) 0.0144(15) -0.0083(14) C30 0.0401(13) 0.0290(12) 0.0401(13) 0.0137(10) -0.0113(11) -0.0054(10) C31 0.0589(18) 0.075(2) 0.0597(18) 0.0303(16) 0.0027(15) -0.0100(15) C32 0.076(2) 0.0295(14) 0.0585(17) 0.0081(12) -0.0222(15) -0.0076(13) C33 0.0594(18) 0.0456(16) 0.0695(19) 0.0238(14) -0.0324(15) -0.0046(13) Si1 0.0186(3) 0.0208(3) 0.0249(3) 0.0000(2) -0.0029(2) -0.0003(2) O3 0.0286(8) 0.0272(8) 0.0341(8) 0.0068(6) -0.0079(6) -0.0018(6) C34 0.019(2) 0.039(2) 0.037(2) -0.0024(18) 0.0047(19) 0.002(2) C35 0.044(3) 0.056(4) 0.045(4) -0.011(3) 0.015(3) 0.003(3) C36 0.025(2) 0.064(5) 0.049(3) 0.001(3) 0.002(2) 0.005(4) C37 0.038(4) 0.045(2) 0.049(4) 0.002(2) 0.009(3) -0.006(2) C34A 0.025(5) 0.042(5) 0.039(5) -0.003(4) 0.008(5) -0.001(5) C35A 0.039(7) 0.057(6) 0.053(9) -0.015(6) 0.013(8) 0.007(6) C36A 0.020(5) 0.049(9) 0.049(6) -0.002(6) 0.003(5) 0.005(7) C37A 0.028(7) 0.052(6) 0.053(9) 0.010(6) 0.006(7) -0.004(7) C38 0.0349(12) 0.0304(12) 0.0354(12) -0.0110(10) -0.0057(10) 0.0005(10) C39 0.0514(16) 0.0578(17) 0.0505(16) -0.0186(13) -0.0224(13) 0.0058(13) C40 0.116(3) 0.0328(16) 0.071(2) -0.0177(14) -0.0196(19) 0.0009(16) C41 0.0439(16) 0.110(3) 0.0584(18) -0.0482(18) 0.0055(14) 0.0018(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O5 1.7057(18) . ? Al1 O1 1.7171(15) . ? Al1 N2 1.9009(16) . ? Al1 N1 1.9012(16) . ? N1 C4 1.341(2) . ? N1 C6 1.445(2) . ? O1 Si1 1.6025(15) . ? C1 C2 1.497(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N2 C2 1.343(2) . ? N2 C18 1.452(2) . ? O5 H5 0.835(10) . ? C2 C3 1.397(3) . ? C3 C4 1.396(3) . ? C3 H3A 0.96(2) . ? O4 C34 1.441(10) . ? O4 C34A 1.46(3) . ? O4 Si1 1.6296(15) . ? C4 C5 1.507(3) . ? O2 C38 1.440(2) . ? O2 Si1 1.6233(14) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.400(3) . ? C6 C7 1.411(3) . ? C7 C8 1.389(3) . ? C7 C15 1.521(3) . ? C8 C9 1.378(3) . ? C8 H8A 0.9500 . ? C9 C10 1.373(3) . ? C9 H9A 0.9500 . ? C10 C11 1.395(3) . ? C10 H10A 0.9500 . ? C11 C12 1.524(3) . ? C12 C14 1.529(3) . ? C12 C13 1.536(3) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.522(3) . ? C15 C16 1.529(3) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.402(3) . ? C18 C19 1.408(3) . ? C19 C20 1.395(3) . ? C19 C27 1.520(3) . ? C20 C21 1.378(3) . ? C20 H20A 0.9500 . ? C21 C22 1.378(3) . ? C21 H21A 0.9500 . ? C22 C23 1.394(3) . ? C22 H22A 0.9500 . ? C23 C24 1.520(3) . ? C24 C25 1.526(3) . ? C24 C26 1.531(3) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.511(4) . ? C27 C29 1.518(3) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O3 1.437(2) . ? C30 C31 1.505(4) . ? C30 C32 1.513(3) . ? C30 C33 1.515(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Si1 O3 1.6175(15) . ? C34 C35 1.515(6) . ? C34 C37 1.521(7) . ? C34 C36 1.524(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C34A C35A 1.513(13) . ? C34A C37A 1.515(14) . ? C34A C36A 1.518(14) . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? C38 C41 1.501(4) . ? C38 C39 1.506(3) . ? C38 C40 1.511(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? 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 O5 Al1 O1 114.20(8) . . ? O5 Al1 N2 107.75(8) . . ? O1 Al1 N2 115.70(7) . . ? O5 Al1 N1 108.85(8) . . ? O1 Al1 N1 112.49(7) . . ? N2 Al1 N1 96.29(8) . . ? C4 N1 C6 119.30(16) . . ? C4 N1 Al1 115.32(13) . . ? C6 N1 Al1 124.04(12) . . ? Si1 O1 Al1 136.37(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 N2 C18 118.23(15) . . ? C2 N2 Al1 115.21(13) . . ? C18 N2 Al1 125.63(12) . . ? Al1 O5 H5 118(2) . . ? N2 C2 C3 122.24(17) . . ? N2 C2 C1 120.01(18) . . ? C3 C2 C1 117.74(18) . . ? C4 C3 C2 128.00(19) . . ? C4 C3 H3A 115.6(12) . . ? C2 C3 H3A 116.2(12) . . ? C34 O4 Si1 131.1(4) . . ? C34A O4 Si1 128.7(9) . . ? N1 C4 C3 122.34(18) . . ? N1 C4 C5 120.61(18) . . ? C3 C4 C5 117.05(18) . . ? C38 O2 Si1 130.87(13) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.29(18) . . ? C11 C6 N1 120.07(18) . . ? C7 C6 N1 118.62(18) . . ? C8 C7 C6 117.7(2) . . ? C8 C7 C15 120.52(19) . . ? C6 C7 C15 121.74(18) . . ? C9 C8 C7 121.6(2) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 121.4(2) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C6 118.08(19) . . ? C10 C11 C12 118.77(19) . . ? C6 C11 C12 123.13(18) . . ? C11 C12 C14 111.82(18) . . ? C11 C12 C13 109.70(17) . . ? C14 C12 C13 110.25(19) . . ? C11 C12 H12A 108.3 . . ? C14 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C15 C17 111.72(19) . . ? C7 C15 C16 113.39(19) . . ? C17 C15 C16 108.87(19) . . ? C7 C15 H15A 107.5 . . ? C17 C15 H15A 107.5 . . ? C16 C15 H15A 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.23(18) . . ? C23 C18 N2 120.13(17) . . ? C19 C18 N2 118.64(17) . . ? C20 C19 C18 117.88(19) . . ? C20 C19 C27 119.45(19) . . ? C18 C19 C27 122.66(18) . . ? C21 C20 C19 121.6(2) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 119.5(2) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C21 C22 C23 121.5(2) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C22 C23 C18 118.15(19) . . ? C22 C23 C24 118.90(18) . . ? C18 C23 C24 122.94(18) . . ? C23 C24 C25 110.43(17) . . ? C23 C24 C26 111.73(17) . . ? C25 C24 C26 110.52(18) . . ? C23 C24 H24A 108.0 . . ? C25 C24 H24A 108.0 . . ? C26 C24 H24A 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 110.3(2) . . ? C28 C27 C19 111.6(2) . . ? C29 C27 C19 111.29(19) . . ? C28 C27 H27A 107.8 . . ? C29 C27 H27A 107.8 . . ? C19 C27 H27A 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O3 C30 C31 108.1(2) . . ? O3 C30 C32 110.41(18) . . ? C31 C30 C32 110.1(2) . . ? O3 C30 C33 105.32(18) . . ? C31 C30 C33 111.5(2) . . ? C32 C30 C33 111.3(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O1 Si1 O3 112.85(8) . . ? O1 Si1 O2 114.09(7) . . ? O3 Si1 O2 105.43(7) . . ? O1 Si1 O4 106.42(8) . . ? O3 Si1 O4 112.21(8) . . ? O2 Si1 O4 105.74(7) . . ? C30 O3 Si1 134.51(13) . . ? O4 C34 C35 106.3(7) . . ? O4 C34 C37 109.9(8) . . ? C35 C34 C37 110.0(6) . . ? O4 C34 C36 110.6(8) . . ? C35 C34 C36 110.2(5) . . ? C37 C34 C36 109.7(6) . . ? O4 C34A C35A 103(2) . . ? O4 C34A C37A 105(2) . . ? C35A C34A C37A 112.4(15) . . ? O4 C34A C36A 112(2) . . ? C35A C34A C36A 112.1(14) . . ? C37A C34A C36A 112.2(16) . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C34A C36A H36D 109.5 . . ? C34A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C34A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? C34A C37A H37D 109.5 . . ? C34A C37A H37E 109.5 . . ? H37D C37A H37E 109.5 . . ? C34A C37A H37F 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? O2 C38 C41 109.53(18) . . ? O2 C38 C39 109.35(18) . . ? C41 C38 C39 111.4(2) . . ? O2 C38 C40 104.97(19) . . ? C41 C38 C40 110.7(2) . . ? C39 C38 C40 110.7(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? 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 O5 Al1 N1 C4 -67.87(16) . . . . ? O1 Al1 N1 C4 164.53(13) . . . . ? N2 Al1 N1 C4 43.33(15) . . . . ? O5 Al1 N1 C6 98.78(16) . . . . ? O1 Al1 N1 C6 -28.81(17) . . . . ? N2 Al1 N1 C6 -150.01(15) . . . . ? O5 Al1 O1 Si1 10.71(15) . . . . ? N2 Al1 O1 Si1 -115.26(13) . . . . ? N1 Al1 O1 Si1 135.42(12) . . . . ? O5 Al1 N2 C2 68.51(15) . . . . ? O1 Al1 N2 C2 -162.31(13) . . . . ? N1 Al1 N2 C2 -43.61(15) . . . . ? O5 Al1 N2 C18 -100.18(16) . . . . ? O1 Al1 N2 C18 29.00(18) . . . . ? N1 Al1 N2 C18 147.70(15) . . . . ? C18 N2 C2 C3 -168.55(18) . . . . ? Al1 N2 C2 C3 21.9(2) . . . . ? C18 N2 C2 C1 10.5(3) . . . . ? Al1 N2 C2 C1 -159.06(15) . . . . ? N2 C2 C3 C4 13.5(3) . . . . ? C1 C2 C3 C4 -165.6(2) . . . . ? C6 N1 C4 C3 171.41(18) . . . . ? Al1 N1 C4 C3 -21.3(2) . . . . ? C6 N1 C4 C5 -7.4(3) . . . . ? Al1 N1 C4 C5 159.98(15) . . . . ? C2 C3 C4 N1 -13.8(3) . . . . ? C2 C3 C4 C5 165.0(2) . . . . ? C4 N1 C6 C11 84.7(2) . . . . ? Al1 N1 C6 C11 -81.5(2) . . . . ? C4 N1 C6 C7 -96.9(2) . . . . ? Al1 N1 C6 C7 96.90(19) . . . . ? C11 C6 C7 C8 -1.5(3) . . . . ? N1 C6 C7 C8 -179.88(18) . . . . ? C11 C6 C7 C15 179.05(19) . . . . ? N1 C6 C7 C15 0.7(3) . . . . ? C6 C7 C8 C9 1.0(3) . . . . ? C15 C7 C8 C9 -179.6(2) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 -1.0(3) . . . . ? C9 C10 C11 C6 0.5(3) . . . . ? C9 C10 C11 C12 179.32(19) . . . . ? C7 C6 C11 C10 0.8(3) . . . . ? N1 C6 C11 C10 179.12(17) . . . . ? C7 C6 C11 C12 -177.97(18) . . . . ? N1 C6 C11 C12 0.3(3) . . . . ? C10 C11 C12 C14 54.4(3) . . . . ? C6 C11 C12 C14 -126.9(2) . . . . ? C10 C11 C12 C13 -68.3(2) . . . . ? C6 C11 C12 C13 110.5(2) . . . . ? C8 C7 C15 C17 -98.5(2) . . . . ? C6 C7 C15 C17 80.9(3) . . . . ? C8 C7 C15 C16 25.0(3) . . . . ? C6 C7 C15 C16 -155.6(2) . . . . ? C2 N2 C18 C23 -90.7(2) . . . . ? Al1 N2 C18 C23 77.6(2) . . . . ? C2 N2 C18 C19 89.4(2) . . . . ? Al1 N2 C18 C19 -102.24(19) . . . . ? C23 C18 C19 C20 0.3(3) . . . . ? N2 C18 C19 C20 -179.79(17) . . . . ? C23 C18 C19 C27 179.52(19) . . . . ? N2 C18 C19 C27 -0.6(3) . . . . ? C18 C19 C20 C21 -1.2(3) . . . . ? C27 C19 C20 C21 179.5(2) . . . . ? C19 C20 C21 C22 0.8(3) . . . . ? C20 C21 C22 C23 0.5(3) . . . . ? C21 C22 C23 C18 -1.4(3) . . . . ? C21 C22 C23 C24 178.99(19) . . . . ? C19 C18 C23 C22 1.0(3) . . . . ? N2 C18 C23 C22 -178.93(17) . . . . ? C19 C18 C23 C24 -179.46(18) . . . . ? N2 C18 C23 C24 0.7(3) . . . . ? C22 C23 C24 C25 69.0(2) . . . . ? C18 C23 C24 C25 -110.6(2) . . . . ? C22 C23 C24 C26 -54.5(2) . . . . ? C18 C23 C24 C26 125.9(2) . . . . ? C20 C19 C27 C28 -53.9(3) . . . . ? C18 C19 C27 C28 126.9(2) . . . . ? C20 C19 C27 C29 69.8(3) . . . . ? C18 C19 C27 C29 -109.4(2) . . . . ? Al1 O1 Si1 O3 -151.09(11) . . . . ? Al1 O1 Si1 O2 88.60(13) . . . . ? Al1 O1 Si1 O4 -27.60(14) . . . . ? C38 O2 Si1 O1 75.72(18) . . . . ? C38 O2 Si1 O3 -48.66(18) . . . . ? C38 O2 Si1 O4 -167.69(16) . . . . ? C34 O4 Si1 O1 168.0(5) . . . . ? C34A O4 Si1 O1 170.1(12) . . . . ? C34 O4 Si1 O3 -68.1(5) . . . . ? C34A O4 Si1 O3 -66.0(12) . . . . ? C34 O4 Si1 O2 46.3(5) . . . . ? C34A O4 Si1 O2 48.4(12) . . . . ? C31 C30 O3 Si1 -81.9(3) . . . . ? C32 C30 O3 Si1 38.6(3) . . . . ? C33 C30 O3 Si1 158.87(18) . . . . ? O1 Si1 O3 C30 41.3(2) . . . . ? O2 Si1 O3 C30 166.50(19) . . . . ? O4 Si1 O3 C30 -78.9(2) . . . . ? C34A O4 C34 C35 128(26) . . . . ? Si1 O4 C34 C35 163.6(5) . . . . ? C34A O4 C34 C37 -113(26) . . . . ? Si1 O4 C34 C37 -77.3(8) . . . . ? C34A O4 C34 C36 8(25) . . . . ? Si1 O4 C34 C36 44.0(9) . . . . ? C34 O4 C34A C35A -68(25) . . . . ? Si1 O4 C34A C35A 146.2(13) . . . . ? C34 O4 C34A C37A 49(25) . . . . ? Si1 O4 C34A C37A -96.4(18) . . . . ? C34 O4 C34A C36A 171(26) . . . . ? Si1 O4 C34A C36A 26(2) . . . . ? Si1 O2 C38 C41 -42.1(3) . . . . ? Si1 O2 C38 C39 80.2(2) . . . . ? Si1 O2 C38 C40 -160.92(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O4 0.835(10) 2.48(2) 3.118(2) 134(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.363 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.051