# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Raymundo Cea-Olivares' _publ_contact_author_address ; Inorganic Instituto de Quimica, Universidad Nacional Autonoma de Mexico Circuito Exterior, Ciudad Universit Mexico 04510 MEXICO ; _publ_contact_author_email CEA@SERVIDOR.UNAM.MX _publ_section_title ; Soluble, reactive and stable - unique alumosilicate ligands and a heterobimetallic derivative [LAl(SLi)(mu-O)Si(OLi.2thf)(OtBu)2]2 ; loop_ _publ_author_name 'Graciela Canseco Melchor' 'Vojteck Jancik' 'Fernando Rascon-Cruz' 'Ruben A. Toscano' data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 628448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H61 Al N2 O4 S Si, 1/3(C6 H14)' _chemical_formula_sum 'C39 H65.67 Al N2 O4 S Si' _chemical_formula_weight 713.73 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 Hexagonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall -R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 31.536(5) _cell_length_b 31.536(5) _cell_length_c 22.246(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19160(6) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6189 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.73 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6996 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9598 _exptl_absorpt_correction_T_max 0.9765 _exptl_absorpt_process_details 'Sadabs, Sheldrick 1996' _exptl_special_details ; The intensities were measured with Bruker Smart Appex 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 34889 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7499 _reflns_number_gt 5435 _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. ; _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^)+(0.0565P)^2^+27.3971P] 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 7499 _refine_ls_number_parameters 636 _refine_ls_number_restraints 479 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 0.988 _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 0.81917(3) 0.03735(3) 0.83743(3) 0.02209(19) Uani 1 1 d . . . Si1 Si 0.82601(3) 0.12378(3) 0.75747(3) 0.02633(19) Uani 1 1 d . . . O1 O 0.81595(6) 0.07146(6) 0.77915(8) 0.0279(4) Uani 1 1 d . . . N1 N 0.87857(7) 0.03622(7) 0.83819(9) 0.0252(5) Uani 1 1 d . . . C1 C 0.92766(10) -0.00202(12) 0.86608(15) 0.0452(8) Uani 1 1 d . . . H1A H 0.9531 0.0242 0.8416 0.068 Uiso 1 1 calc R . . H1B H 0.9243 -0.0335 0.8543 0.068 Uiso 1 1 calc R . . H1C H 0.9368 0.0042 0.9086 0.068 Uiso 1 1 calc R . . S1 S 0.80703(3) 0.06115(3) 0.92667(3) 0.0388(2) Uani 1 1 d . . . H1 H 0.8212(11) 0.1053(11) 0.9069(13) 0.058 Uiso 1 1 d . . . O2 O 0.84242(7) 0.15836(6) 0.81687(8) 0.0348(5) Uani 1 1 d . . . N2 N 0.77651(7) -0.03065(7) 0.82962(9) 0.0231(5) Uani 1 1 d . . . C2 C 0.87978(10) -0.00342(10) 0.85642(12) 0.0286(6) Uani 1 1 d . . . O3 O 0.77819(6) 0.12189(6) 0.72593(8) 0.0295(4) Uani 1 1 d . A . C3 C 0.83738(10) -0.04817(10) 0.86681(12) 0.0312(6) Uani 1 1 d . . . H3A H 0.8418(10) -0.0728(10) 0.8819(12) 0.037 Uiso 1 1 d . . . O4 O 0.86761(7) 0.14424(7) 0.70615(9) 0.0371(5) Uani 1 1 d D . . H2 H 0.8710(12) 0.1641(10) 0.6833(13) 0.056 Uiso 1 1 d D . . C4 C 0.78957(9) -0.06228(9) 0.85048(11) 0.0270(6) Uani 1 1 d . . . C5 C 0.75232(10) -0.11596(10) 0.85640(14) 0.0376(7) Uani 1 1 d . . . H5A H 0.7336 -0.1277 0.8189 0.056 Uiso 1 1 calc R . . H5B H 0.7300 -0.1207 0.8896 0.056 Uiso 1 1 calc R . . H5C H 0.7691 -0.1344 0.8645 0.056 Uiso 1 1 calc R . . C6 C 0.72727(9) -0.05097(9) 0.80439(11) 0.0247(6) Uani 1 1 d . . . C7 C 0.68734(9) -0.06286(9) 0.84242(12) 0.0278(6) Uani 1 1 d . . . C8 C 0.64127(10) -0.08258(10) 0.81563(13) 0.0359(7) Uani 1 1 d . . . H8A H 0.6136 -0.0904 0.8400 0.043 Uiso 1 1 calc R . . C9 C 0.63504(11) -0.09093(11) 0.75480(14) 0.0413(7) Uani 1 1 d . . . H9A H 0.6032 -0.1049 0.7378 0.050 Uiso 1 1 calc R . . C10 C 0.67477(10) -0.07910(10) 0.71821(13) 0.0363(7) Uani 1 1 d . . . H10A H 0.6700 -0.0851 0.6762 0.044 Uiso 1 1 calc R . . C11 C 0.72177(10) -0.05843(9) 0.74198(12) 0.0294(6) Uani 1 1 d . . . C12 C 0.76484(10) -0.04515(11) 0.70048(12) 0.0361(7) Uani 1 1 d . . . H12A H 0.7944 -0.0180 0.7204 0.043 Uiso 1 1 calc R . . C13 C 0.75990(15) -0.02613(16) 0.64017(16) 0.0737(12) Uani 1 1 d . . . H13A H 0.7908 -0.0131 0.6181 0.111 Uiso 1 1 calc R . . H13B H 0.7520 0.0000 0.6461 0.111 Uiso 1 1 calc R . . H13C H 0.7336 -0.0529 0.6171 0.111 Uiso 1 1 calc R . . C14 C 0.77447(18) -0.08702(16) 0.69249(19) 0.0876(15) Uani 1 1 d . . . H14A H 0.8025 -0.0770 0.6655 0.131 Uiso 1 1 calc R . . H14B H 0.7455 -0.1151 0.6751 0.131 Uiso 1 1 calc R . . H14C H 0.7818 -0.0962 0.7316 0.131 Uiso 1 1 calc R . . C15 C 0.69193(10) -0.05471(11) 0.90963(12) 0.0365(7) Uani 1 1 d . . . H15A H 0.7268 -0.0425 0.9209 0.044 Uiso 1 1 calc R . . C16 C 0.67925(12) -0.01555(13) 0.92751(15) 0.0532(9) Uani 1 1 d . . . H16A H 0.6981 0.0137 0.9027 0.080 Uiso 1 1 calc R . . H16B H 0.6874 -0.0070 0.9700 0.080 Uiso 1 1 calc R . . H16C H 0.6442 -0.0282 0.9214 0.080 Uiso 1 1 calc R . . C17 C 0.65983(12) -0.10187(13) 0.94536(15) 0.0607(10) Uani 1 1 d . . . H17A H 0.6670 -0.1274 0.9326 0.091 Uiso 1 1 calc R . . H17B H 0.6252 -0.1129 0.9379 0.091 Uiso 1 1 calc R . . H17C H 0.6668 -0.0954 0.9884 0.091 Uiso 1 1 calc R . . C18 C 0.92372(9) 0.07953(10) 0.82041(12) 0.0280(6) Uani 1 1 d . . . C19 C 0.95163(10) 0.11603(10) 0.86295(12) 0.0314(6) Uani 1 1 d . . . C20 C 0.99224(10) 0.15846(11) 0.84184(14) 0.0396(7) Uani 1 1 d . . . H20O H 1.0115 0.1839 0.8695 0.048 Uiso 1 1 calc R . . C21 C 1.00535(11) 0.16463(12) 0.78201(14) 0.0459(8) Uani 1 1 d . . . H21A H 1.0330 0.1942 0.7688 0.055 Uiso 1 1 calc R . . C22 C 0.97843(11) 0.12794(12) 0.74127(14) 0.0421(8) Uani 1 1 d . . . H22A H 0.9883 0.1320 0.7003 0.051 Uiso 1 1 calc R . . C23 C 0.93685(9) 0.08487(10) 0.75932(12) 0.0313(6) Uani 1 1 d . . . C24 C 0.90892(11) 0.04438(12) 0.71366(13) 0.0429(8) Uani 1 1 d . . . H24A H 0.8764 0.0209 0.7317 0.051 Uiso 1 1 calc R . . C25 C 0.89927(14) 0.06270(14) 0.65507(15) 0.0610(10) Uani 1 1 d . . . H25A H 0.8773 0.0347 0.6299 0.092 Uiso 1 1 calc R . . H25B H 0.9303 0.0827 0.6339 0.092 Uiso 1 1 calc R . . H25C H 0.8840 0.0825 0.6636 0.092 Uiso 1 1 calc R . . C26 C 0.9349(2) 0.01619(17) 0.7002(2) 0.0994(17) Uani 1 1 d . . . H26A H 0.9153 -0.0103 0.6719 0.149 Uiso 1 1 calc R . . H26B H 0.9392 0.0023 0.7375 0.149 Uiso 1 1 calc R . . H26C H 0.9670 0.0383 0.6824 0.149 Uiso 1 1 calc R . . C27 C 0.94104(10) 0.11030(11) 0.93017(12) 0.0364(7) Uani 1 1 d . . . H27A H 0.9102 0.0785 0.9368 0.044 Uiso 1 1 calc R . . C28 C 0.93374(12) 0.15107(11) 0.95596(15) 0.0490(8) Uani 1 1 d . . . H28A H 0.9080 0.1528 0.9334 0.073 Uiso 1 1 calc R . . H28B H 0.9644 0.1824 0.9527 0.073 Uiso 1 1 calc R . . H28C H 0.9242 0.1442 0.9983 0.073 Uiso 1 1 calc R . . C29 C 0.98237(12) 0.10882(14) 0.96491(15) 0.0572(10) Uani 1 1 d . . . H29A H 0.9883 0.0837 0.9475 0.086 Uiso 1 1 calc R . . H29B H 0.9729 0.1010 1.0072 0.086 Uiso 1 1 calc R . . H29C H 1.0123 0.1408 0.9623 0.086 Uiso 1 1 calc R . . C30 C 0.86792(11) 0.21097(10) 0.82398(13) 0.0401(7) Uani 1 1 d . . . C31 C 0.85308(14) 0.21955(12) 0.88558(15) 0.0566(9) Uani 1 1 d . . . H31A H 0.8606 0.2016 0.9158 0.085 Uiso 1 1 calc R . . H31B H 0.8179 0.2079 0.8859 0.085 Uiso 1 1 calc R . . H31C H 0.8712 0.2546 0.8948 0.085 Uiso 1 1 calc R . . C32 C 0.92252(12) 0.22935(13) 0.82174(18) 0.0634(10) Uani 1 1 d . . . H32A H 0.9311 0.2223 0.7821 0.095 Uiso 1 1 calc R . . H32B H 0.9310 0.2129 0.8528 0.095 Uiso 1 1 calc R . . H32C H 0.9406 0.2648 0.8288 0.095 Uiso 1 1 calc R . . C33 C 0.85326(14) 0.23465(11) 0.77553(15) 0.0564(10) Uani 1 1 d . . . H33A H 0.8638 0.2291 0.7363 0.085 Uiso 1 1 calc R . . H33B H 0.8689 0.2699 0.7832 0.085 Uiso 1 1 calc R . . H33C H 0.8176 0.2203 0.7757 0.085 Uiso 1 1 calc R . . C34 C 0.72793(10) 0.10010(10) 0.74680(12) 0.0323(6) Uani 1 1 d D . . C35 C 0.70348(19) 0.1200(2) 0.7067(2) 0.0560(14) Uani 0.891(9) 1 d PDU A 1 H35A H 0.7197 0.1557 0.7115 0.084 Uiso 0.891(9) 1 calc PR A 1 H35B H 0.6689 0.1053 0.7179 0.084 Uiso 0.891(9) 1 calc PR A 1 H35C H 0.7060 0.1120 0.6648 0.084 Uiso 0.891(9) 1 calc PR A 1 C36 C 0.70393(14) 0.04484(13) 0.7383(2) 0.0504(13) Uani 0.891(9) 1 d PDU A 1 H36A H 0.7083 0.0377 0.6967 0.076 Uiso 0.891(9) 1 calc PR A 1 H36B H 0.6689 0.0295 0.7473 0.076 Uiso 0.891(9) 1 calc PR A 1 H36C H 0.7191 0.0319 0.7656 0.076 Uiso 0.891(9) 1 calc PR A 1 C37 C 0.72562(15) 0.1115(2) 0.81233(18) 0.0539(13) Uani 0.891(9) 1 d PDU A 1 H37A H 0.7422 0.0982 0.8367 0.081 Uiso 0.891(9) 1 calc PR A 1 H37B H 0.6913 0.0965 0.8249 0.081 Uiso 0.891(9) 1 calc PR A 1 H37C H 0.7418 0.1470 0.8179 0.081 Uiso 0.891(9) 1 calc PR A 1 C36A C 0.6973(16) 0.0978(16) 0.6935(15) 0.068(12) Uani 0.109(9) 1 d PDU A 2 H36D H 0.7136 0.1292 0.6721 0.103 Uiso 0.109(9) 1 calc PR A 2 H36E H 0.6650 0.0911 0.7074 0.103 Uiso 0.109(9) 1 calc PR A 2 H36F H 0.6934 0.0716 0.6663 0.103 Uiso 0.109(9) 1 calc PR A 2 C37A C 0.7090(13) 0.0523(10) 0.7797(19) 0.065(9) Uani 0.109(9) 1 d PDU A 2 H37D H 0.7153 0.0300 0.7557 0.097 Uiso 0.109(9) 1 calc PR A 2 H37E H 0.6737 0.0377 0.7862 0.097 Uiso 0.109(9) 1 calc PR A 2 H37F H 0.7256 0.0582 0.8185 0.097 Uiso 0.109(9) 1 calc PR A 2 C35A C 0.7299(12) 0.1391(11) 0.7901(17) 0.063(9) Uani 0.109(9) 1 d PDU A 2 H35D H 0.7553 0.1469 0.8204 0.094 Uiso 0.109(9) 1 calc PR A 2 H35E H 0.6981 0.1264 0.8100 0.094 Uiso 0.109(9) 1 calc PR A 2 H35F H 0.7376 0.1687 0.7675 0.094 Uiso 0.109(9) 1 calc PR A 2 C101 C 0.8280(11) 0.4610(8) 0.7879(15) 0.100(6) Uani 0.1523(12) 1 d PDU B -1 H10B H 0.8164 0.4831 0.7750 0.149 Uiso 0.1523(12) 1 calc PR B -1 H10C H 0.8460 0.4564 0.7549 0.149 Uiso 0.1523(12) 1 calc PR B -1 H10D H 0.8498 0.4751 0.8226 0.149 Uiso 0.1523(12) 1 calc PR B -1 C102 C 0.7854(9) 0.4128(9) 0.8049(14) 0.096(5) Uani 0.1523(12) 1 d PDU B -1 H10E H 0.7616 0.3996 0.7714 0.115 Uiso 0.1523(12) 1 calc PR B -1 H10F H 0.7688 0.4164 0.8406 0.115 Uiso 0.1523(12) 1 calc PR B -1 C103 C 0.8044(8) 0.3787(8) 0.8187(15) 0.095(4) Uani 0.1523(12) 1 d PDU B -1 H10G H 0.8209 0.3750 0.7829 0.114 Uiso 0.1523(12) 1 calc PR B -1 H10H H 0.8284 0.3921 0.8519 0.114 Uiso 0.1523(12) 1 calc PR B -1 C104 C 0.7623(8) 0.3301(8) 0.8364(13) 0.094(5) Uani 0.1523(12) 1 d PDU B -1 H10I H 0.7395 0.3156 0.8020 0.112 Uiso 0.1523(12) 1 calc PR B -1 H10J H 0.7442 0.3343 0.8700 0.112 Uiso 0.1523(12) 1 calc PR B -1 C105 C 0.7806(9) 0.2964(9) 0.8552(14) 0.093(5) Uani 0.1523(12) 1 d PDU B -1 H10K H 0.7961 0.2895 0.8208 0.111 Uiso 0.1523(12) 1 calc PR B -1 H10L H 0.8051 0.3114 0.8877 0.111 Uiso 0.1523(12) 1 calc PR B -1 C106 C 0.7372(11) 0.2502(9) 0.8768(12) 0.096(6) Uani 0.1523(12) 1 d PDU B -1 H10M H 0.7477 0.2273 0.8903 0.144 Uiso 0.1523(12) 1 calc PR B -1 H10N H 0.7135 0.2354 0.8439 0.144 Uiso 0.1523(12) 1 calc PR B -1 H10O H 0.7218 0.2577 0.9103 0.144 Uiso 0.1523(12) 1 calc PR B -1 C201 C 0.828(3) 0.442(3) 0.778(4) 0.095(6) Uani 0.063(4) 1 d PDU C -2 H20A H 0.8600 0.4719 0.7835 0.143 Uiso 0.063(4) 1 calc PR C -2 H20B H 0.8148 0.4425 0.7387 0.143 Uiso 0.063(4) 1 calc PR C -2 H20C H 0.8326 0.4134 0.7809 0.143 Uiso 0.063(4) 1 calc PR C -2 C202 C 0.794(3) 0.439(2) 0.826(3) 0.096(5) Uani 0.063(4) 1 d PDU C -2 H20D H 0.7741 0.4536 0.8117 0.115 Uiso 0.063(4) 1 calc PR C -2 H20E H 0.8123 0.4573 0.8623 0.115 Uiso 0.063(4) 1 calc PR C -2 C203 C 0.7615(17) 0.386(2) 0.840(3) 0.095(5) Uani 0.063(4) 1 d PDU C -2 H20F H 0.7567 0.3813 0.8843 0.115 Uiso 0.063(4) 1 calc PR C -2 H20G H 0.7291 0.3735 0.8212 0.115 Uiso 0.063(4) 1 calc PR C -2 C204 C 0.785(3) 0.358(2) 0.817(2) 0.095(5) Uani 0.063(4) 1 d PDU C -2 H20H H 0.8172 0.3809 0.7997 0.114 Uiso 0.063(4) 1 calc PR C -2 H20I H 0.7642 0.3352 0.7853 0.114 Uiso 0.063(4) 1 calc PR C -2 C205 C 0.791(2) 0.330(2) 0.867(3) 0.094(5) Uani 0.063(4) 1 d PDU C -2 H20J H 0.8102 0.3144 0.8527 0.113 Uiso 0.063(4) 1 calc PR C -2 H20K H 0.8087 0.3514 0.9012 0.113 Uiso 0.063(4) 1 calc PR C -2 C206 C 0.741(3) 0.291(2) 0.886(3) 0.094(7) Uani 0.063(4) 1 d PDU C -2 H20L H 0.7438 0.2734 0.9209 0.141 Uiso 0.063(4) 1 calc PR C -2 H20M H 0.7253 0.2678 0.8529 0.141 Uiso 0.063(4) 1 calc PR C -2 H20N H 0.7218 0.3062 0.8967 0.141 Uiso 0.063(4) 1 calc PR C -2 C301 C 0.7514(12) 0.3976(16) 0.7710(16) 0.102(6) Uani 0.118(4) 1 d PDU D -3 H30A H 0.7369 0.3910 0.7307 0.153 Uiso 0.118(4) 1 calc PR D -3 H30B H 0.7370 0.4129 0.7957 0.153 Uiso 0.118(4) 1 calc PR D -3 H30C H 0.7449 0.3667 0.7897 0.153 Uiso 0.118(4) 1 calc PR D -3 C302 C 0.8054(13) 0.4312(13) 0.7665(18) 0.097(5) Uani 0.118(4) 1 d PDU D -3 H30D H 0.8141 0.4654 0.7755 0.116 Uiso 0.118(4) 1 calc PR D -3 H30E H 0.8174 0.4300 0.7257 0.116 Uiso 0.118(4) 1 calc PR D -3 C303 C 0.8267(11) 0.4123(13) 0.8128(16) 0.096(5) Uani 0.118(4) 1 d PDU D -3 H30F H 0.8523 0.4070 0.7943 0.115 Uiso 0.118(4) 1 calc PR D -3 H30G H 0.8417 0.4362 0.8459 0.115 Uiso 0.118(4) 1 calc PR D -3 C304 C 0.7859(12) 0.3649(14) 0.8364(16) 0.094(5) Uani 0.118(4) 1 d PDU D -3 H30H H 0.7738 0.3707 0.8748 0.113 Uiso 0.118(4) 1 calc PR D -3 H30I H 0.7584 0.3511 0.8073 0.113 Uiso 0.118(4) 1 calc PR D -3 C305 C 0.8036(13) 0.3293(14) 0.8461(16) 0.094(5) Uani 0.118(4) 1 d PDU D -3 H30J H 0.8013 0.3118 0.8082 0.112 Uiso 0.118(4) 1 calc PR D -3 H30K H 0.8382 0.3468 0.8593 0.112 Uiso 0.118(4) 1 calc PR D -3 C306 C 0.7721(17) 0.2940(14) 0.8930(19) 0.096(6) Uani 0.118(4) 1 d PDU D -3 H30L H 0.7928 0.2916 0.9242 0.144 Uiso 0.118(4) 1 calc PR D -3 H30M H 0.7516 0.2617 0.8748 0.144 Uiso 0.118(4) 1 calc PR D -3 H30N H 0.7511 0.3053 0.9111 0.144 Uiso 0.118(4) 1 calc PR D -3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0216(4) 0.0221(4) 0.0220(4) 0.0015(3) 0.0006(3) 0.0105(3) Si1 0.0271(4) 0.0252(4) 0.0263(4) 0.0039(3) 0.0010(3) 0.0128(3) O1 0.0288(10) 0.0242(10) 0.0311(10) 0.0024(8) -0.0005(8) 0.0135(8) N1 0.0238(12) 0.0265(12) 0.0249(11) -0.0001(9) -0.0005(9) 0.0122(10) C1 0.0334(17) 0.0459(19) 0.063(2) 0.0121(16) 0.0010(15) 0.0251(16) S1 0.0381(4) 0.0453(5) 0.0322(4) -0.0068(3) 0.0046(3) 0.0201(4) O2 0.0407(12) 0.0260(10) 0.0329(11) -0.0004(8) -0.0031(9) 0.0130(9) N2 0.0230(11) 0.0239(11) 0.0231(11) 0.0009(9) -0.0010(9) 0.0122(10) C2 0.0286(15) 0.0339(16) 0.0272(14) 0.0010(12) -0.0020(11) 0.0185(13) O3 0.0275(10) 0.0325(11) 0.0291(10) 0.0065(8) 0.0032(8) 0.0155(9) C3 0.0352(17) 0.0292(16) 0.0363(16) 0.0061(12) -0.0011(13) 0.0213(14) O4 0.0362(11) 0.0408(13) 0.0377(12) 0.0152(9) 0.0109(9) 0.0217(10) C4 0.0305(15) 0.0246(14) 0.0251(14) -0.0004(11) -0.0001(11) 0.0130(12) C5 0.0352(17) 0.0242(15) 0.0525(19) 0.0035(13) 0.0007(14) 0.0143(13) C6 0.0223(14) 0.0184(13) 0.0302(14) 0.0018(11) -0.0025(11) 0.0078(11) C7 0.0246(14) 0.0246(14) 0.0320(15) 0.0031(11) -0.0007(12) 0.0105(12) C8 0.0256(15) 0.0337(16) 0.0427(18) 0.0051(13) 0.0014(13) 0.0106(13) C9 0.0289(16) 0.0376(18) 0.0463(19) 0.0027(14) -0.0104(14) 0.0083(14) C10 0.0362(17) 0.0332(16) 0.0317(16) -0.0003(13) -0.0086(13) 0.0115(14) C11 0.0309(15) 0.0231(14) 0.0283(15) -0.0014(11) -0.0051(12) 0.0089(12) C12 0.0332(16) 0.0432(18) 0.0261(15) -0.0048(13) -0.0016(12) 0.0147(14) C13 0.080(3) 0.107(3) 0.047(2) 0.035(2) 0.026(2) 0.055(3) C14 0.126(4) 0.099(3) 0.077(3) 0.022(3) 0.046(3) 0.085(3) C15 0.0253(15) 0.0450(18) 0.0322(16) 0.0044(13) 0.0048(12) 0.0122(14) C16 0.0405(19) 0.071(2) 0.050(2) -0.0132(18) 0.0048(16) 0.0289(18) C17 0.047(2) 0.075(3) 0.044(2) 0.0225(18) 0.0105(16) 0.0183(19) C18 0.0218(14) 0.0291(15) 0.0337(15) 0.0021(12) 0.0013(12) 0.0131(12) C19 0.0240(15) 0.0344(16) 0.0369(16) 0.0001(13) -0.0011(12) 0.0155(13) C20 0.0255(16) 0.0386(17) 0.0444(18) -0.0029(14) -0.0003(13) 0.0084(14) C21 0.0286(17) 0.0406(19) 0.054(2) 0.0085(16) 0.0076(15) 0.0064(15) C22 0.0338(17) 0.053(2) 0.0346(17) 0.0091(15) 0.0084(13) 0.0182(16) C23 0.0236(14) 0.0371(16) 0.0319(15) 0.0028(12) 0.0018(12) 0.0141(13) C24 0.0401(18) 0.0470(19) 0.0323(17) -0.0002(14) 0.0071(14) 0.0149(15) C25 0.082(3) 0.075(3) 0.043(2) -0.0171(18) -0.0161(18) 0.053(2) C26 0.168(5) 0.098(4) 0.081(3) -0.041(3) -0.050(3) 0.104(4) C27 0.0275(15) 0.0429(18) 0.0344(16) -0.0039(13) -0.0009(12) 0.0143(14) C28 0.0399(19) 0.0445(19) 0.054(2) -0.0145(16) 0.0011(15) 0.0145(16) C29 0.047(2) 0.089(3) 0.0398(19) -0.0010(18) -0.0049(16) 0.037(2) C30 0.0463(19) 0.0255(16) 0.0399(17) -0.0054(13) -0.0070(14) 0.0115(14) C31 0.076(3) 0.041(2) 0.047(2) -0.0122(16) -0.0092(18) 0.0260(19) C32 0.047(2) 0.045(2) 0.074(3) -0.0025(18) -0.0038(19) 0.0048(17) C33 0.083(3) 0.0296(18) 0.052(2) -0.0038(15) -0.0163(19) 0.0244(18) C34 0.0243(15) 0.0343(16) 0.0357(16) 0.0064(13) 0.0044(12) 0.0126(13) C35 0.032(3) 0.067(4) 0.074(3) 0.033(3) 0.013(2) 0.028(3) C36 0.036(2) 0.036(2) 0.072(3) 0.003(2) -0.002(2) 0.0125(17) C37 0.037(2) 0.068(3) 0.045(2) 0.000(2) 0.0166(18) 0.018(2) C36A 0.043(15) 0.064(19) 0.077(17) 0.037(16) 0.015(14) 0.010(16) C37A 0.041(14) 0.046(14) 0.095(18) 0.027(15) 0.016(15) 0.013(12) C35A 0.030(13) 0.075(17) 0.062(16) 0.001(14) 0.023(13) 0.010(14) C101 0.097(11) 0.158(12) 0.057(10) -0.049(9) -0.024(8) 0.074(9) C102 0.095(10) 0.157(12) 0.053(8) -0.051(8) -0.019(7) 0.077(9) C103 0.094(10) 0.157(12) 0.051(8) -0.052(8) -0.019(6) 0.077(8) C104 0.094(10) 0.158(12) 0.049(8) -0.051(8) -0.018(7) 0.078(8) C105 0.092(10) 0.159(12) 0.048(8) -0.051(8) -0.019(7) 0.079(9) C106 0.099(11) 0.159(13) 0.046(10) -0.049(9) -0.021(9) 0.077(9) C201 0.094(11) 0.156(13) 0.054(10) -0.051(10) -0.020(8) 0.076(10) C202 0.095(10) 0.158(12) 0.053(8) -0.051(9) -0.020(7) 0.076(9) C203 0.095(10) 0.158(12) 0.052(8) -0.051(8) -0.020(7) 0.077(9) C204 0.094(10) 0.158(12) 0.051(8) -0.051(8) -0.019(6) 0.076(9) C205 0.093(10) 0.158(12) 0.050(8) -0.052(8) -0.019(7) 0.077(9) C206 0.094(11) 0.159(13) 0.049(10) -0.051(9) -0.018(8) 0.078(10) C301 0.097(10) 0.159(14) 0.061(10) -0.046(11) -0.024(8) 0.073(10) C302 0.096(10) 0.157(12) 0.055(8) -0.050(8) -0.019(7) 0.077(9) C303 0.095(10) 0.158(12) 0.053(8) -0.051(8) -0.019(6) 0.076(9) C304 0.094(10) 0.157(12) 0.050(8) -0.052(8) -0.018(6) 0.077(8) C305 0.093(10) 0.158(12) 0.050(8) -0.052(8) -0.019(7) 0.077(9) C306 0.093(11) 0.160(13) 0.052(9) -0.049(9) -0.021(8) 0.077(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7195(18) . ? Al1 N2 1.885(2) . ? Al1 N1 1.891(2) . ? Al1 S1 2.2221(11) . ? Si1 O1 1.5914(18) . ? Si1 O4 1.611(2) . ? Si1 O2 1.6244(19) . ? Si1 O3 1.6370(18) . ? N1 C2 1.333(3) . ? N1 C18 1.451(3) . ? C1 C2 1.504(4) . ? O2 C30 1.446(3) . ? N2 C4 1.338(3) . ? N2 C6 1.463(3) . ? C2 C3 1.395(4) . ? O3 C34 1.453(3) . ? C3 C4 1.390(4) . ? C4 C5 1.508(4) . ? C6 C7 1.404(4) . ? C6 C11 1.404(4) . ? C7 C8 1.396(4) . ? C7 C15 1.512(4) . ? C8 C9 1.374(4) . ? C9 C10 1.380(4) . ? C10 C11 1.391(4) . ? C11 C12 1.518(4) . ? C12 C14 1.506(5) . ? C12 C13 1.509(4) . ? C15 C16 1.529(4) . ? C15 C17 1.537(4) . ? C18 C23 1.406(4) . ? C18 C19 1.408(4) . ? C19 C20 1.392(4) . ? C19 C27 1.523(4) . ? C20 C21 1.378(4) . ? C21 C22 1.378(4) . ? C22 C23 1.394(4) . ? C23 C24 1.521(4) . ? C24 C26 1.509(5) . ? C24 C25 1.517(4) . ? C27 C28 1.527(4) . ? C27 C29 1.536(4) . ? C30 C33 1.509(4) . ? C30 C31 1.516(4) . ? C30 C32 1.518(5) . ? C34 C37A 1.503(14) . ? C34 C35 1.506(5) . ? C34 C36A 1.508(14) . ? C34 C37 1.512(4) . ? C34 C36 1.525(4) . ? C34 C35A 1.538(14) . ? C101 C102 1.489(8) . ? C102 C103 1.499(8) . ? C103 C104 1.494(10) . ? C104 C105 1.500(8) . ? C105 C106 1.493(8) . ? C201 C202 1.490(11) . ? C202 C203 1.502(11) . ? C203 C204 1.491(14) . ? C204 C205 1.498(11) . ? C205 C206 1.490(11) . ? C301 C302 1.494(11) . ? C302 C303 1.505(11) . ? C303 C304 1.498(14) . ? C304 C305 1.497(11) . ? C305 C306 1.487(11) . ? 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 N2 114.22(9) . . ? O1 Al1 N1 112.78(9) . . ? N2 Al1 N1 97.45(9) . . ? O1 Al1 S1 112.85(7) . . ? N2 Al1 S1 108.72(7) . . ? N1 Al1 S1 109.74(7) . . ? O1 Si1 O4 109.28(10) . . ? O1 Si1 O2 106.31(10) . . ? O4 Si1 O2 112.67(11) . . ? O1 Si1 O3 112.93(10) . . ? O4 Si1 O3 105.19(10) . . ? O2 Si1 O3 110.58(10) . . ? Si1 O1 Al1 146.46(12) . . ? C2 N1 C18 119.4(2) . . ? C2 N1 Al1 120.90(17) . . ? C18 N1 Al1 119.67(16) . . ? C30 O2 Si1 131.84(17) . . ? C4 N2 C6 117.5(2) . . ? C4 N2 Al1 120.35(17) . . ? C6 N2 Al1 122.07(16) . . ? N1 C2 C3 122.5(2) . . ? N1 C2 C1 121.0(2) . . ? C3 C2 C1 116.5(2) . . ? C34 O3 Si1 130.36(16) . . ? C4 C3 C2 128.2(3) . . ? N2 C4 C3 122.7(2) . . ? N2 C4 C5 120.6(2) . . ? C3 C4 C5 116.6(2) . . ? C7 C6 C11 122.1(2) . . ? C7 C6 N2 120.0(2) . . ? C11 C6 N2 117.9(2) . . ? C8 C7 C6 117.2(2) . . ? C8 C7 C15 119.2(2) . . ? C6 C7 C15 123.6(2) . . ? C9 C8 C7 121.5(3) . . ? C8 C9 C10 120.4(3) . . ? C9 C10 C11 120.9(3) . . ? C10 C11 C6 117.9(3) . . ? C10 C11 C12 119.7(2) . . ? C6 C11 C12 122.5(2) . . ? C14 C12 C13 110.5(3) . . ? C14 C12 C11 112.0(3) . . ? C13 C12 C11 113.2(3) . . ? C7 C15 C16 110.7(2) . . ? C7 C15 C17 112.7(3) . . ? C16 C15 C17 109.6(3) . . ? C23 C18 C19 121.7(2) . . ? C23 C18 N1 117.9(2) . . ? C19 C18 N1 120.3(2) . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C27 119.1(3) . . ? C18 C19 C27 123.5(2) . . ? C21 C20 C19 121.9(3) . . ? C22 C21 C20 120.1(3) . . ? C21 C22 C23 120.9(3) . . ? C22 C23 C18 118.2(3) . . ? C22 C23 C24 119.6(3) . . ? C18 C23 C24 122.2(2) . . ? C26 C24 C25 109.0(3) . . ? C26 C24 C23 111.7(3) . . ? C25 C24 C23 113.4(3) . . ? C19 C27 C28 112.7(3) . . ? C19 C27 C29 111.0(2) . . ? C28 C27 C29 108.9(3) . . ? O2 C30 C33 110.9(2) . . ? O2 C30 C31 105.1(2) . . ? C33 C30 C31 111.0(3) . . ? O2 C30 C32 108.0(3) . . ? C33 C30 C32 110.9(3) . . ? C31 C30 C32 110.7(3) . . ? O3 C34 C37A 115.0(14) . . ? O3 C34 C35 106.2(3) . . ? C37A C34 C35 132.5(14) . . ? O3 C34 C36A 107(2) . . ? C37A C34 C36A 114.2(16) . . ? O3 C34 C37 111.5(2) . . ? C37A C34 C37 74.1(17) . . ? C35 C34 C37 112.1(3) . . ? C36A C34 C37 132(2) . . ? O3 C34 C36 107.6(2) . . ? C35 C34 C36 109.8(3) . . ? C36A C34 C36 84.7(16) . . ? C37 C34 C36 109.6(3) . . ? O3 C34 C35A 102.9(12) . . ? C37A C34 C35A 109.5(15) . . ? C35 C34 C35A 82.1(17) . . ? C36A C34 C35A 107.5(16) . . ? C36 C34 C35A 142.1(14) . . ? C101 C102 C103 107.7(10) . . ? C104 C103 C102 108.8(11) . . ? C103 C104 C105 110.0(11) . . ? C106 C105 C104 106.8(10) . . ? C201 C202 C203 106.5(14) . . ? C204 C203 C202 109.2(15) . . ? C203 C204 C205 110.6(16) . . ? C206 C205 C204 107.2(14) . . ? C301 C302 C303 104.3(12) . . ? C304 C303 C302 107.8(14) . . ? C305 C304 C303 110.0(15) . . ? C306 C305 C304 107.7(14) . . ? 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 1.31(3) 2.48(3) 3.632(2) 145.4(19) . O4 H2 O3 0.771(17) 2.136(19) 2.891(3) 166(3) 13_656 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.426 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.055 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 628449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H61 Al N2 O5 Si, C4 H8 O' _chemical_formula_sum 'C41 H69 Al N2 O6 Si' _chemical_formula_weight 741.05 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.504(1) _cell_length_b 22.740(2) _cell_length_c 20.130(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.87(2) _cell_angle_gamma 90.00 _cell_volume 4350.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9924 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.31 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 55277 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7629 _reflns_number_gt 5747 _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. ; _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^)+(0.1120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7629 _refine_ls_number_parameters 529 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1700 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.84929(10) 0.47367(4) 0.24810(5) 0.0263(2) Uani 1 1 d D . . Al1 Al 0.73399(10) 0.34942(4) 0.25671(5) 0.0212(2) Uani 1 1 d D . . N1 N 0.6232(3) 0.31543(11) 0.32383(12) 0.0221(6) Uani 1 1 d . . . O1 O 0.7304(2) 0.42465(9) 0.25811(12) 0.0274(5) Uani 1 1 d . . . C1 C 0.4992(4) 0.23811(16) 0.12808(17) 0.0362(9) Uani 1 1 d . . . H1A H 0.4841 0.2671 0.0927 0.054 Uiso 1 1 calc R . . H1B H 0.4095 0.2193 0.1387 0.054 Uiso 1 1 calc R . . H1C H 0.5660 0.2082 0.1132 0.054 Uiso 1 1 calc R . . N2 N 0.6357(3) 0.31685(11) 0.18287(13) 0.0225(6) Uani 1 1 d . . . O2 O 1.0049(2) 0.44392(10) 0.25149(14) 0.0342(6) Uani 1 1 d D . . H2 H 1.0040(10) 0.4110(4) 0.254(2) 0.051 Uiso 1 1 d D . . C2 C 0.5574(4) 0.26824(14) 0.18864(16) 0.0236(8) Uani 1 1 d . . . O3 O 0.8399(3) 0.52639(10) 0.30221(13) 0.0390(7) Uani 1 1 d . . . C3 C 0.5211(4) 0.24413(14) 0.25003(16) 0.0270(7) Uani 1 1 d . . . H3A H 0.4757 0.2069 0.2486 0.032 Uiso 1 1 calc R . . C4 C 0.5436(4) 0.26826(14) 0.31313(16) 0.0250(8) Uani 1 1 d . . . O4 O 0.8166(3) 0.50462(11) 0.17678(13) 0.0407(7) Uani 1 1 d . . . O5 O 0.9081(2) 0.32969(10) 0.26021(13) 0.0315(6) Uani 1 1 d D . . H5 H 0.9164(8) 0.2974(5) 0.261(2) 0.047 Uiso 1 1 d D . . C5 C 0.4683(4) 0.23953(16) 0.37001(17) 0.0351(9) Uani 1 1 d . . . H5A H 0.5345 0.2336 0.4072 0.053 Uiso 1 1 calc R . . H5B H 0.4306 0.2014 0.3556 0.053 Uiso 1 1 calc R . . H5C H 0.3910 0.2649 0.3842 0.053 Uiso 1 1 calc R . . C6 C 0.6286(4) 0.34108(14) 0.39003(16) 0.0251(8) Uani 1 1 d . . . C7 C 0.7304(4) 0.32115(15) 0.43560(16) 0.0271(8) Uani 1 1 d . . . C8 C 0.7334(4) 0.34751(16) 0.49848(18) 0.0371(9) Uani 1 1 d . . . H8A H 0.8012 0.3349 0.5306 0.045 Uiso 1 1 calc R . . C9 C 0.6407(5) 0.39111(17) 0.51463(18) 0.0388(10) Uani 1 1 d . . . H9A H 0.6445 0.4082 0.5577 0.047 Uiso 1 1 calc R . . C10 C 0.5428(4) 0.41008(16) 0.46920(18) 0.0367(9) Uani 1 1 d . . . H10I H 0.4791 0.4403 0.4812 0.044 Uiso 1 1 calc R . . C11 C 0.5341(4) 0.38593(14) 0.40525(17) 0.0278(8) Uani 1 1 d . . . C12 C 0.4224(4) 0.40788(16) 0.35612(19) 0.0362(9) Uani 1 1 d . . . H12A H 0.4372 0.3870 0.3131 0.043 Uiso 1 1 calc R . . C13 C 0.4374(5) 0.47319(18) 0.3431(2) 0.0557(12) Uani 1 1 d . . . H13A H 0.3692 0.4852 0.3087 0.084 Uiso 1 1 calc R . . H13B H 0.5330 0.4815 0.3280 0.084 Uiso 1 1 calc R . . H13C H 0.4199 0.4950 0.3841 0.084 Uiso 1 1 calc R . . C14 C 0.2762(5) 0.3936(2) 0.3786(3) 0.0752(17) Uani 1 1 d . . . H14A H 0.2077 0.4070 0.3450 0.113 Uiso 1 1 calc R . . H14B H 0.2585 0.4135 0.4208 0.113 Uiso 1 1 calc R . . H14C H 0.2672 0.3510 0.3845 0.113 Uiso 1 1 calc R . . C15 C 0.8362(4) 0.27352(16) 0.41969(19) 0.0349(9) Uani 1 1 d . . . H15A H 0.8202 0.2615 0.3724 0.042 Uiso 1 1 calc R . . C16 C 0.8157(5) 0.21857(17) 0.4634(2) 0.0449(11) Uani 1 1 d . . . H16A H 0.8886 0.1895 0.4535 0.067 Uiso 1 1 calc R . . H16B H 0.7228 0.2015 0.4541 0.067 Uiso 1 1 calc R . . H16C H 0.8227 0.2297 0.5104 0.067 Uiso 1 1 calc R . . C17 C 0.9859(4) 0.2956(2) 0.4262(2) 0.0508(11) Uani 1 1 d . . . H17A H 1.0000 0.3283 0.3953 0.076 Uiso 1 1 calc R . . H17B H 1.0513 0.2637 0.4159 0.076 Uiso 1 1 calc R . . H17C H 1.0035 0.3093 0.4718 0.076 Uiso 1 1 calc R . . C18 C 0.6531(4) 0.34205(14) 0.11730(16) 0.0262(8) Uani 1 1 d . . . C19 C 0.7570(4) 0.32039(15) 0.07538(17) 0.0324(9) Uani 1 1 d . . . C20 C 0.7656(5) 0.34510(17) 0.01192(18) 0.0431(11) Uani 1 1 d . . . H20I H 0.8351 0.3313 -0.0177 0.052 Uiso 1 1 calc R . . C21 C 0.6755(5) 0.38884(18) -0.00838(19) 0.0506(12) Uani 1 1 d . . . H21A H 0.6813 0.4040 -0.0522 0.061 Uiso 1 1 calc R . . C22 C 0.5768(5) 0.41098(17) 0.03430(19) 0.0431(10) Uani 1 1 d . . . H22A H 0.5164 0.4418 0.0197 0.052 Uiso 1 1 calc R . . C23 C 0.5639(4) 0.38901(15) 0.09868(18) 0.0319(9) Uani 1 1 d . . . C24 C 0.4546(4) 0.41359(16) 0.14502(19) 0.0357(9) Uani 1 1 d . . . H24A H 0.4915 0.4076 0.1913 0.043 Uiso 1 1 calc R . . C25 C 0.4327(5) 0.47917(18) 0.1362(2) 0.0586(13) Uani 1 1 d . . . H25A H 0.3699 0.4937 0.1707 0.088 Uiso 1 1 calc R . . H25B H 0.3904 0.4868 0.0923 0.088 Uiso 1 1 calc R . . H25C H 0.5235 0.4994 0.1398 0.088 Uiso 1 1 calc R . . C26 C 0.3172(5) 0.3812(2) 0.1399(3) 0.0702(15) Uani 1 1 d . . . H26A H 0.3326 0.3395 0.1498 0.105 Uiso 1 1 calc R . . H26B H 0.2781 0.3853 0.0948 0.105 Uiso 1 1 calc R . . H26C H 0.2510 0.3977 0.1718 0.105 Uiso 1 1 calc R . . C27 C 0.8605(4) 0.27320(16) 0.09618(18) 0.0358(9) Uani 1 1 d . . . H27A H 0.8335 0.2592 0.1413 0.043 Uiso 1 1 calc R . . C28 C 0.8562(5) 0.21966(17) 0.0491(2) 0.0516(12) Uani 1 1 d . . . H28A H 0.9184 0.1888 0.0667 0.077 Uiso 1 1 calc R . . H28B H 0.8877 0.2315 0.0050 0.077 Uiso 1 1 calc R . . H28C H 0.7597 0.2046 0.0459 0.077 Uiso 1 1 calc R . . C29 C 1.0093(5) 0.2972(2) 0.1014(2) 0.0568(12) Uani 1 1 d . . . H29A H 1.0097 0.3329 0.1287 0.085 Uiso 1 1 calc R . . H29B H 1.0431 0.3066 0.0569 0.085 Uiso 1 1 calc R . . H29C H 1.0710 0.2677 0.1220 0.085 Uiso 1 1 calc R . . C30 C 0.8978(4) 0.53055(17) 0.36892(19) 0.0378(9) Uani 1 1 d . . . C31 C 0.8057(5) 0.5751(2) 0.4042(2) 0.0619(14) Uani 1 1 d . . . H31A H 0.8011 0.6114 0.3781 0.093 Uiso 1 1 calc R . . H31B H 0.8458 0.5835 0.4483 0.093 Uiso 1 1 calc R . . H31C H 0.7107 0.5589 0.4088 0.093 Uiso 1 1 calc R . . C32 C 1.0469(5) 0.5531(2) 0.3636(3) 0.0586(13) Uani 1 1 d . . . H32A H 1.1046 0.5237 0.3410 0.088 Uiso 1 1 calc R . . H32B H 1.0859 0.5603 0.4082 0.088 Uiso 1 1 calc R . . H32C H 1.0469 0.5898 0.3381 0.088 Uiso 1 1 calc R . . C33 C 0.8918(5) 0.47174(19) 0.4042(2) 0.0528(12) Uani 1 1 d . . . H33A H 0.9518 0.4434 0.3814 0.079 Uiso 1 1 calc R . . H33B H 0.7946 0.4574 0.4039 0.079 Uiso 1 1 calc R . . H33C H 0.9251 0.4764 0.4502 0.079 Uiso 1 1 calc R . . C34 C 0.9092(5) 0.53014(16) 0.1293(2) 0.0421(10) Uani 1 1 d . . . C35 C 1.0144(6) 0.5701(2) 0.1640(3) 0.0786(18) Uani 1 1 d . . . H35A H 1.0732 0.5468 0.1946 0.118 Uiso 1 1 calc R . . H35B H 0.9641 0.6003 0.1890 0.118 Uiso 1 1 calc R . . H35C H 1.0740 0.5890 0.1309 0.118 Uiso 1 1 calc R . . C36 C 0.8154(6) 0.5636(2) 0.0810(2) 0.0737(17) Uani 1 1 d . . . H36A H 0.7450 0.5368 0.0618 0.111 Uiso 1 1 calc R . . H36B H 0.8726 0.5801 0.0455 0.111 Uiso 1 1 calc R . . H36C H 0.7677 0.5954 0.1045 0.111 Uiso 1 1 calc R . . C37 C 0.9856(6) 0.4818(2) 0.0927(2) 0.0608(14) Uani 1 1 d . . . H37A H 0.9171 0.4533 0.0752 0.091 Uiso 1 1 calc R . . H37B H 1.0512 0.4620 0.1233 0.091 Uiso 1 1 calc R . . H37C H 1.0380 0.4990 0.0558 0.091 Uiso 1 1 calc R . . O6 O 0.9848(14) 0.2107(5) 0.2458(7) 0.070(3) Uani 0.473(12) 1 d PDU A 1 C100 C 1.1206(15) 0.1880(6) 0.2448(9) 0.077(3) Uani 0.473(12) 1 d PDU A 1 H10A H 1.1837 0.2113 0.2742 0.092 Uiso 0.473(12) 1 calc PR A 1 H10B H 1.1577 0.1892 0.1992 0.092 Uiso 0.473(12) 1 calc PR A 1 C101 C 1.1121(12) 0.1254(5) 0.2690(10) 0.082(3) Uani 0.473(12) 1 d PDU A 1 H10C H 1.1632 0.0988 0.2388 0.099 Uiso 0.473(12) 1 calc PR A 1 H10D H 1.1541 0.1219 0.3142 0.099 Uiso 0.473(12) 1 calc PR A 1 C102 C 0.9589(12) 0.1099(5) 0.2699(10) 0.081(3) Uani 0.473(12) 1 d PDU A 1 H10E H 0.9367 0.0788 0.2369 0.098 Uiso 0.473(12) 1 calc PR A 1 H10F H 0.9310 0.0962 0.3145 0.098 Uiso 0.473(12) 1 calc PR A 1 C103 C 0.8875(15) 0.1654(6) 0.2523(13) 0.073(3) Uani 0.473(12) 1 d PDU A 1 H10G H 0.8347 0.1604 0.2099 0.088 Uiso 0.473(12) 1 calc PR A 1 H10H H 0.8195 0.1757 0.2872 0.088 Uiso 0.473(12) 1 calc PR A 1 O6B O 0.9830(13) 0.2089(4) 0.2756(6) 0.067(2) Uani 0.527(12) 1 d PDU A 2 C200 C 1.1190(14) 0.1892(5) 0.2756(8) 0.078(3) Uani 0.527(12) 1 d PDU A 2 H20A H 1.1501 0.1793 0.3214 0.093 Uiso 0.527(12) 1 calc PR A 2 H20B H 1.1819 0.2201 0.2583 0.093 Uiso 0.527(12) 1 calc PR A 2 C201 C 1.1258(11) 0.1357(6) 0.2324(8) 0.087(3) Uani 0.527(12) 1 d PDU A 2 H20C H 1.1604 0.1457 0.1877 0.105 Uiso 0.527(12) 1 calc PR A 2 H20D H 1.1880 0.1054 0.2525 0.105 Uiso 0.527(12) 1 calc PR A 2 C202 C 0.9769(12) 0.1151(5) 0.2291(8) 0.083(3) Uani 0.527(12) 1 d PDU A 2 H20E H 0.9677 0.0757 0.2497 0.099 Uiso 0.527(12) 1 calc PR A 2 H20F H 0.9428 0.1129 0.1824 0.099 Uiso 0.527(12) 1 calc PR A 2 C203 C 0.8962(14) 0.1599(6) 0.2670(11) 0.072(3) Uani 0.527(12) 1 d PDU A 2 H20G H 0.8096 0.1710 0.2421 0.087 Uiso 0.527(12) 1 calc PR A 2 H20H H 0.8691 0.1439 0.3107 0.087 Uiso 0.527(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0332(5) 0.0180(4) 0.0278(5) 0.0006(4) 0.0011(5) -0.0024(4) Al1 0.0301(5) 0.0174(5) 0.0162(5) -0.0003(4) 0.0013(4) -0.0017(4) N1 0.0330(17) 0.0206(14) 0.0126(14) -0.0010(11) 0.0014(12) -0.0011(12) O1 0.0344(13) 0.0176(11) 0.0304(13) 0.0001(10) 0.0025(11) -0.0008(10) C1 0.052(3) 0.031(2) 0.025(2) -0.0050(16) 0.0000(18) -0.0077(18) N2 0.0313(16) 0.0203(14) 0.0159(14) -0.0012(11) 0.0030(12) -0.0006(12) O2 0.0385(14) 0.0235(12) 0.0408(15) -0.0005(13) 0.0021(13) -0.0020(10) C2 0.033(2) 0.0198(17) 0.0183(17) -0.0023(13) -0.0028(15) 0.0014(15) O3 0.0508(17) 0.0257(13) 0.0404(15) -0.0090(12) -0.0061(13) 0.0023(12) C3 0.041(2) 0.0210(16) 0.0192(17) -0.0016(15) 0.0026(17) -0.0063(14) C4 0.034(2) 0.0221(18) 0.0191(17) 0.0032(14) 0.0011(15) -0.0015(15) O4 0.0421(16) 0.0398(15) 0.0403(16) 0.0168(13) 0.0074(12) 0.0001(13) O5 0.0366(14) 0.0217(11) 0.0362(15) 0.0032(12) 0.0015(12) 0.0000(10) C5 0.050(2) 0.036(2) 0.0191(18) -0.0012(16) 0.0066(17) -0.0185(18) C6 0.035(2) 0.0237(18) 0.0166(17) 0.0004(14) 0.0023(15) -0.0097(15) C7 0.039(2) 0.0246(18) 0.0177(17) -0.0004(14) -0.0003(15) -0.0057(16) C8 0.051(3) 0.039(2) 0.0209(19) 0.0024(16) -0.0072(18) -0.011(2) C9 0.058(3) 0.036(2) 0.023(2) -0.0099(16) 0.0051(19) -0.010(2) C10 0.050(3) 0.030(2) 0.030(2) -0.0078(16) 0.0088(18) -0.0038(18) C11 0.035(2) 0.0224(18) 0.0264(19) -0.0009(15) 0.0059(16) -0.0044(15) C12 0.043(2) 0.034(2) 0.032(2) -0.0057(17) -0.0006(17) 0.0093(18) C13 0.064(3) 0.041(2) 0.063(3) 0.016(2) 0.005(2) 0.013(2) C14 0.041(3) 0.078(4) 0.107(5) 0.028(3) -0.011(3) -0.011(3) C15 0.045(2) 0.035(2) 0.0253(19) 0.0031(16) -0.0069(17) 0.0034(18) C16 0.058(3) 0.035(2) 0.041(2) 0.0049(18) -0.012(2) -0.002(2) C17 0.043(3) 0.052(3) 0.057(3) 0.008(2) -0.007(2) 0.003(2) C18 0.040(2) 0.0201(17) 0.0185(17) 0.0003(13) -0.0014(15) -0.0030(15) C19 0.051(2) 0.0251(18) 0.0210(18) -0.0042(14) 0.0070(17) -0.0051(17) C20 0.071(3) 0.036(2) 0.0223(19) 0.0009(16) 0.015(2) -0.004(2) C21 0.093(4) 0.040(2) 0.018(2) 0.0073(18) 0.004(2) -0.004(2) C22 0.068(3) 0.031(2) 0.031(2) 0.0094(17) -0.007(2) 0.002(2) C23 0.043(2) 0.0250(19) 0.027(2) 0.0005(15) -0.0048(17) -0.0021(16) C24 0.040(2) 0.036(2) 0.031(2) 0.0027(17) -0.0059(17) 0.0088(18) C25 0.074(3) 0.038(2) 0.064(3) 0.001(2) 0.009(3) 0.013(2) C26 0.055(3) 0.057(3) 0.099(4) -0.002(3) 0.012(3) 0.007(3) C27 0.049(2) 0.036(2) 0.0226(19) 0.0027(16) 0.0124(17) 0.0064(18) C28 0.084(3) 0.030(2) 0.041(2) -0.0008(18) 0.022(2) 0.007(2) C29 0.047(3) 0.062(3) 0.061(3) -0.002(2) 0.013(2) 0.006(2) C30 0.045(2) 0.034(2) 0.035(2) -0.0108(17) -0.0005(18) -0.0032(18) C31 0.070(3) 0.059(3) 0.057(3) -0.029(2) 0.004(3) 0.004(3) C32 0.055(3) 0.053(3) 0.067(3) -0.015(2) -0.001(2) -0.017(2) C33 0.073(3) 0.050(3) 0.035(2) 0.001(2) -0.004(2) -0.008(2) C34 0.062(3) 0.028(2) 0.037(2) 0.0089(17) 0.018(2) -0.0016(19) C35 0.106(5) 0.059(3) 0.072(4) 0.003(3) 0.029(3) -0.039(3) C36 0.097(4) 0.067(3) 0.059(3) 0.036(3) 0.030(3) 0.032(3) C37 0.089(4) 0.054(3) 0.039(3) 0.003(2) 0.012(2) 0.020(3) O6 0.066(3) 0.038(3) 0.107(7) 0.012(4) -0.001(5) 0.009(2) C100 0.069(3) 0.054(4) 0.107(7) 0.009(5) 0.004(5) 0.012(3) C101 0.081(4) 0.052(3) 0.113(7) 0.013(4) 0.000(5) 0.019(3) C102 0.086(4) 0.044(3) 0.115(7) 0.013(5) 0.005(5) 0.009(3) C103 0.073(3) 0.041(4) 0.105(7) 0.010(4) -0.001(5) 0.005(3) O6B 0.067(3) 0.035(3) 0.099(6) -0.001(4) 0.008(5) 0.008(2) C200 0.069(3) 0.056(4) 0.108(7) -0.003(4) -0.007(5) 0.010(3) C201 0.086(4) 0.065(4) 0.110(7) -0.007(5) 0.013(5) 0.024(4) C202 0.093(4) 0.044(3) 0.111(7) -0.007(4) -0.002(5) 0.007(3) C203 0.073(3) 0.038(3) 0.107(7) 0.012(4) 0.008(4) 0.003(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 Si1 O1 1.602(2) . ? Si1 O3 1.623(3) . ? Si1 O4 1.625(3) . ? Si1 O2 1.627(3) . ? Al1 O1 1.711(2) . ? Al1 O5 1.715(3) . ? Al1 N1 1.891(3) . ? Al1 N2 1.894(3) . ? N1 C4 1.329(4) . ? N1 C6 1.455(4) . ? C1 C2 1.497(5) . ? N2 C2 1.338(4) . ? N2 C18 1.451(4) . ? C2 C3 1.400(5) . ? O3 C30 1.447(5) . ? C3 C4 1.397(5) . ? C4 C5 1.508(4) . ? O4 C34 1.432(4) . ? C6 C11 1.396(5) . ? C6 C7 1.398(5) . ? C7 C8 1.401(5) . ? C7 C15 1.516(5) . ? C8 C9 1.369(6) . ? C9 C10 1.365(6) . ? C10 C11 1.401(5) . ? C11 C12 1.524(5) . ? C12 C14 1.503(6) . ? C12 C13 1.515(5) . ? C15 C17 1.513(6) . ? C15 C16 1.542(5) . ? C18 C19 1.399(5) . ? C18 C23 1.411(5) . ? C19 C20 1.399(5) . ? C19 C27 1.511(5) . ? C20 C21 1.370(6) . ? C21 C22 1.377(6) . ? C22 C23 1.396(5) . ? C23 C24 1.514(5) . ? C24 C26 1.502(6) . ? C24 C25 1.516(5) . ? C27 C29 1.518(6) . ? C27 C28 1.542(5) . ? C30 C32 1.512(6) . ? C30 C33 1.516(6) . ? C30 C31 1.521(6) . ? C34 C36 1.514(6) . ? C34 C35 1.514(7) . ? C34 C37 1.515(6) . ? O6 C100 1.390(11) . ? O6 C103 1.391(11) . ? C100 C101 1.508(13) . ? C101 C102 1.498(8) . ? C102 C103 1.474(13) . ? O6B C200 1.368(10) . ? O6B C203 1.395(10) . ? C200 C201 1.496(12) . ? C201 C202 1.492(8) . ? C202 C203 1.492(14) . ? 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 112.54(14) . . ? O1 Si1 O4 106.67(14) . . ? O3 Si1 O4 105.15(14) . . ? O1 Si1 O2 110.37(12) . . ? O3 Si1 O2 109.76(14) . . ? O4 Si1 O2 112.24(15) . . ? O1 Al1 O5 106.29(11) . . ? O1 Al1 N1 112.67(12) . . ? O5 Al1 N1 114.28(13) . . ? O1 Al1 N2 113.20(12) . . ? O5 Al1 N2 113.20(13) . . ? N1 Al1 N2 97.33(11) . . ? C4 N1 C6 119.0(3) . . ? C4 N1 Al1 122.4(2) . . ? C6 N1 Al1 118.6(2) . . ? Si1 O1 Al1 132.76(14) . . ? C2 N2 C18 118.4(3) . . ? C2 N2 Al1 121.5(2) . . ? C18 N2 Al1 119.9(2) . . ? N2 C2 C3 123.0(3) . . ? N2 C2 C1 120.4(3) . . ? C3 C2 C1 116.5(3) . . ? C30 O3 Si1 130.3(2) . . ? C4 C3 C2 127.8(3) . . ? N1 C4 C3 122.9(3) . . ? N1 C4 C5 120.1(3) . . ? C3 C4 C5 116.9(3) . . ? C34 O4 Si1 130.9(3) . . ? C11 C6 C7 122.3(3) . . ? C11 C6 N1 118.7(3) . . ? C7 C6 N1 119.0(3) . . ? C6 C7 C8 117.3(3) . . ? C6 C7 C15 123.2(3) . . ? C8 C7 C15 119.5(3) . . ? C9 C8 C7 121.4(4) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 121.5(4) . . ? C6 C11 C10 117.3(3) . . ? C6 C11 C12 122.8(3) . . ? C10 C11 C12 119.9(3) . . ? C14 C12 C13 110.7(4) . . ? C14 C12 C11 111.8(3) . . ? C13 C12 C11 111.5(3) . . ? C17 C15 C7 111.7(3) . . ? C17 C15 C16 110.3(3) . . ? C7 C15 C16 111.6(3) . . ? C19 C18 C23 122.2(3) . . ? C19 C18 N2 120.1(3) . . ? C23 C18 N2 117.7(3) . . ? C18 C19 C20 117.4(4) . . ? C18 C19 C27 123.1(3) . . ? C20 C19 C27 119.5(3) . . ? C21 C20 C19 121.3(4) . . ? C20 C21 C22 120.5(4) . . ? C21 C22 C23 121.3(4) . . ? C22 C23 C18 117.2(3) . . ? C22 C23 C24 120.7(3) . . ? C18 C23 C24 122.1(3) . . ? C26 C24 C23 112.4(3) . . ? C26 C24 C25 110.9(4) . . ? C23 C24 C25 112.7(3) . . ? C19 C27 C29 111.4(3) . . ? C19 C27 C28 112.3(3) . . ? C29 C27 C28 110.1(3) . . ? O3 C30 C32 107.5(3) . . ? O3 C30 C33 111.2(3) . . ? C32 C30 C33 112.0(4) . . ? O3 C30 C31 105.2(3) . . ? C32 C30 C31 110.8(3) . . ? C33 C30 C31 110.0(4) . . ? O4 C34 C36 105.7(4) . . ? O4 C34 C35 110.1(3) . . ? C36 C34 C35 111.9(4) . . ? O4 C34 C37 109.6(3) . . ? C36 C34 C37 109.5(4) . . ? C35 C34 C37 110.0(4) . . ? C100 O6 C103 110.2(9) . . ? O6 C100 C101 106.9(9) . . ? C102 C101 C100 106.4(8) . . ? C103 C102 C101 103.9(9) . . ? O6 C103 C102 110.6(9) . . ? C200 O6B C203 107.1(8) . . ? O6B C200 C201 108.4(9) . . ? C202 C201 C200 103.4(8) . . ? C201 C202 C203 104.9(8) . . ? O6B C203 C202 107.6(9) . . ? 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 O6 0.739(9) 2.101(16) 2.819(11) 164(3) . O5 H5 O6B 0.739(9) 2.128(13) 2.854(10) 167(2) . O2 H2 O5 0.751(9) 2.066(12) 2.762(3) 154.5(9) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.443 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.057 #===END data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 628450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H150 Al2 Li4 N4 O12 S2 Si2, C4 H8 O' _chemical_formula_sum 'C94 H158 Al2 Li4 N4 O13 S2 Si2' _chemical_formula_weight 1754.26 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' Li Li -0.0003 0.0001 '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)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.248(2) _cell_length_b 23.568(4) _cell_length_c 16.509(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.91(3) _cell_angle_gamma 90.00 _cell_volume 5061.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7391 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.31 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9647 _exptl_absorpt_correction_T_max 0.9771 _exptl_absorpt_process_details 'Sadabs, Sheldrick 1996' _exptl_special_details ; The intensities were measured with Bruker Smart Appex 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 39473 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.38 _reflns_number_total 9260 _reflns_number_gt 6312 _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. ; _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^)+(0.0540P)^2^+0.9348P] 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 9260 _refine_ls_number_parameters 679 _refine_ls_number_restraints 561 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 0.995 _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 0.93754(5) -0.02492(3) 0.59672(4) 0.03012(16) Uani 1 1 d . . . Si1 Si 0.90319(5) 0.15189(3) 0.58308(4) 0.02848(18) Uani 1 1 d . . . Al1 Al 0.92461(5) 0.03809(3) 0.69159(4) 0.02565(18) Uani 1 1 d . . . O1 O 0.91089(13) 0.10742(7) 0.65907(10) 0.0310(4) Uani 1 1 d . . . N1 N 0.81520(15) 0.01877(8) 0.75076(12) 0.0283(5) Uani 1 1 d . . . C1 C 0.7482(2) -0.03771(13) 0.85632(17) 0.0430(7) Uani 1 1 d . . . H1A H 0.6854 -0.0159 0.8369 0.064 Uiso 0.50 1 calc PR . . H1B H 0.7668 -0.0350 0.9165 0.064 Uiso 0.50 1 calc PR . . H1C H 0.7365 -0.0775 0.8402 0.064 Uiso 0.50 1 calc PR . . H1D H 0.7738 -0.0698 0.8922 0.064 Uiso 0.50 1 calc PR . . H1E H 0.6923 -0.0506 0.8126 0.064 Uiso 0.50 1 calc PR . . H1F H 0.7226 -0.0081 0.8889 0.064 Uiso 0.50 1 calc PR . . Li1 Li 0.9426(3) 0.04752(18) 0.4950(3) 0.0371(10) Uani 1 1 d . . . O2 O 0.94233(13) 0.12487(7) 0.50613(10) 0.0318(4) Uani 1 1 d . A . N2 N 1.03383(15) 0.03378(8) 0.78764(12) 0.0268(5) Uani 1 1 d . . . Li2 Li 1.0475(4) 0.1343(2) 0.4461(3) 0.0411(11) Uani 1 1 d . . . O3 O 0.78460(13) 0.17720(7) 0.55957(10) 0.0350(4) Uani 1 1 d . . . C2 C 0.83480(19) -0.01404(10) 0.81812(15) 0.0298(6) Uani 1 1 d . . . C3 C 0.9345(2) -0.02727(11) 0.85939(16) 0.0337(6) Uani 1 1 d . . . H3A H 0.936(2) -0.0532(11) 0.9046(16) 0.040 Uiso 1 1 d . . . O4 O 0.96960(13) 0.20783(7) 0.62285(11) 0.0352(4) Uani 1 1 d . . . C4 C 1.02655(19) -0.00123(11) 0.84974(15) 0.0297(6) Uani 1 1 d . . . C5 C 1.1191(2) -0.01383(12) 0.91712(15) 0.0379(7) Uani 1 1 d . . . H5A H 1.1582 0.0212 0.9319 0.057 Uiso 1 1 calc R . . H5B H 1.1630 -0.0420 0.8971 0.057 Uiso 1 1 calc R . . H5C H 1.0956 -0.0288 0.9658 0.057 Uiso 1 1 calc R . . C6 C 1.12801(19) 0.06678(11) 0.79464(14) 0.0296(6) Uani 1 1 d . . . C7 C 1.21446(19) 0.04393(11) 0.76951(15) 0.0329(6) Uani 1 1 d . . . C8 C 1.3044(2) 0.07631(13) 0.78177(17) 0.0435(7) Uani 1 1 d . . . H8A H 1.3643 0.0613 0.7658 0.052 Uiso 1 1 calc R . . C9 C 1.3082(2) 0.12978(13) 0.81657(18) 0.0476(8) Uani 1 1 d . . . H9A H 1.3698 0.1513 0.8239 0.057 Uiso 1 1 calc R . . C10 C 1.2221(2) 0.15170(12) 0.84060(17) 0.0444(7) Uani 1 1 d . . . H10A H 1.2251 0.1885 0.8643 0.053 Uiso 1 1 calc R . . C11 C 1.1304(2) 0.12093(11) 0.83089(15) 0.0353(6) Uani 1 1 d . . . C12 C 1.0400(2) 0.14475(11) 0.86429(17) 0.0401(7) Uani 1 1 d . . . H12A H 0.9789 0.1205 0.8430 0.048 Uiso 1 1 calc R . . C13 C 1.0135(2) 0.20528(12) 0.83601(19) 0.0512(8) Uani 1 1 d . . . H13A H 0.9961 0.2064 0.7756 0.077 Uiso 1 1 calc R . . H13B H 1.0727 0.2300 0.8552 0.077 Uiso 1 1 calc R . . H13C H 0.9546 0.2185 0.8589 0.077 Uiso 1 1 calc R . . C14 C 1.0607(3) 0.14114(15) 0.9580(2) 0.0656(10) Uani 1 1 d . . . H14A H 1.0722 0.1015 0.9751 0.098 Uiso 1 1 calc R . . H14B H 1.0014 0.1561 0.9788 0.098 Uiso 1 1 calc R . . H14C H 1.1219 0.1636 0.9806 0.098 Uiso 1 1 calc R . . C15 C 1.2153(2) -0.01451(11) 0.73026(16) 0.0354(6) Uani 1 1 d . . . H15A H 1.1484 -0.0334 0.7328 0.042 Uiso 1 1 calc R . . C16 C 1.3019(2) -0.05266(13) 0.77480(19) 0.0528(8) Uani 1 1 d . . . H16A H 1.2950 -0.0906 0.7501 0.079 Uiso 1 1 calc R . . H16B H 1.2976 -0.0553 0.8333 0.079 Uiso 1 1 calc R . . H16C H 1.3684 -0.0364 0.7695 0.079 Uiso 1 1 calc R . . C17 C 1.2233(2) -0.00890(12) 0.63923(16) 0.0423(7) Uani 1 1 d . . . H17A H 1.1695 0.0167 0.6114 0.063 Uiso 1 1 calc R . . H17B H 1.2147 -0.0463 0.6129 0.063 Uiso 1 1 calc R . . H17C H 1.2909 0.0065 0.6352 0.063 Uiso 1 1 calc R . . C18 C 0.70840(18) 0.03526(11) 0.72091(15) 0.0296(6) Uani 1 1 d . . . C19 C 0.64078(19) -0.00192(11) 0.67143(15) 0.0321(6) Uani 1 1 d . . . C20 C 0.5388(2) 0.01557(12) 0.64478(17) 0.0377(7) Uani 1 1 d . . . H20A H 0.4916 -0.0092 0.6115 0.045 Uiso 1 1 calc R . . C21 C 0.5055(2) 0.06807(12) 0.66605(17) 0.0401(7) Uani 1 1 d . . . H21A H 0.4361 0.0793 0.6472 0.048 Uiso 1 1 calc R . . C22 C 0.5732(2) 0.10420(12) 0.71466(17) 0.0401(7) Uani 1 1 d . . . H22A H 0.5496 0.1401 0.7294 0.048 Uiso 1 1 calc R . . C23 C 0.6760(2) 0.08900(11) 0.74266(16) 0.0340(6) Uani 1 1 d . . . C24 C 0.7489(2) 0.13044(12) 0.79566(17) 0.0414(7) Uani 1 1 d . . . H24A H 0.8201 0.1215 0.7876 0.050 Uiso 1 1 calc R . . C25 C 0.7275(3) 0.19225(12) 0.7713(2) 0.0563(9) Uani 1 1 d . . . H25A H 0.7296 0.1971 0.7127 0.084 Uiso 1 1 calc R . . H25B H 0.7799 0.2164 0.8044 0.084 Uiso 1 1 calc R . . H25C H 0.6594 0.2030 0.7812 0.084 Uiso 1 1 calc R . . C26 C 0.7470(3) 0.12268(15) 0.88689(19) 0.0724(11) Uani 1 1 d . . . H26A H 0.7671 0.0837 0.9034 0.109 Uiso 1 1 calc R . . H26B H 0.6775 0.1300 0.8966 0.109 Uiso 1 1 calc R . . H26C H 0.7952 0.1493 0.9194 0.109 Uiso 1 1 calc R . . C27 C 0.6715(2) -0.05997(11) 0.64294(16) 0.0371(6) Uani 1 1 d . . . H27A H 0.7454 -0.0665 0.6679 0.045 Uiso 1 1 calc R . . C28 C 0.6609(2) -0.06156(12) 0.54965(17) 0.0432(7) Uani 1 1 d . . . H28A H 0.7025 -0.0312 0.5320 0.065 Uiso 1 1 calc R . . H28B H 0.5887 -0.0562 0.5238 0.065 Uiso 1 1 calc R . . H28C H 0.6849 -0.0983 0.5330 0.065 Uiso 1 1 calc R . . C29 C 0.6079(2) -0.10832(12) 0.67114(19) 0.0505(8) Uani 1 1 d . . . H29A H 0.6108 -0.1055 0.7308 0.076 Uiso 1 1 calc R . . H29B H 0.6362 -0.1450 0.6583 0.076 Uiso 1 1 calc R . . H29C H 0.5363 -0.1053 0.6423 0.076 Uiso 1 1 calc R . . C30 C 0.69531(19) 0.15814(11) 0.50284(16) 0.0344(6) Uani 1 1 d . . . C31 C 0.6768(2) 0.09550(11) 0.51631(17) 0.0389(7) Uani 1 1 d . . . H31A H 0.6630 0.0898 0.5720 0.058 Uiso 1 1 calc R . . H31B H 0.7379 0.0737 0.5100 0.058 Uiso 1 1 calc R . . H31C H 0.6176 0.0825 0.4756 0.058 Uiso 1 1 calc R . . C32 C 0.7095(2) 0.16942(12) 0.41528(17) 0.0438(7) Uani 1 1 d . . . H32A H 0.7244 0.2098 0.4091 0.066 Uiso 1 1 calc R . . H32B H 0.6465 0.1592 0.3766 0.066 Uiso 1 1 calc R . . H32C H 0.7669 0.1466 0.4036 0.066 Uiso 1 1 calc R . . C33 C 0.6057(2) 0.19339(13) 0.52234(18) 0.0475(8) Uani 1 1 d . . . H33A H 0.6201 0.2338 0.5163 0.071 Uiso 1 1 calc R . . H33B H 0.5974 0.1858 0.5791 0.071 Uiso 1 1 calc R . . H33C H 0.5424 0.1831 0.4841 0.071 Uiso 1 1 calc R . . C34 C 0.9619(2) 0.26696(11) 0.59944(18) 0.0427(7) Uani 1 1 d . . . C35 C 0.8704(3) 0.29369(13) 0.6282(2) 0.0645(10) Uani 1 1 d . . . H35A H 0.8068 0.2760 0.5990 0.097 Uiso 1 1 calc R . . H35B H 0.8687 0.3345 0.6163 0.097 Uiso 1 1 calc R . . H35C H 0.8766 0.2878 0.6877 0.097 Uiso 1 1 calc R . . C36 C 1.0604(3) 0.29494(13) 0.6442(2) 0.0642(10) Uani 1 1 d . . . H36A H 1.1196 0.2778 0.6258 0.096 Uiso 1 1 calc R . . H36B H 1.0668 0.2894 0.7038 0.096 Uiso 1 1 calc R . . H36C H 1.0582 0.3356 0.6317 0.096 Uiso 1 1 calc R . . C37 C 0.9526(3) 0.27304(13) 0.5065(2) 0.0610(9) Uani 1 1 d . . . H37A H 0.8898 0.2541 0.4785 0.091 Uiso 1 1 calc R . . H37B H 1.0124 0.2556 0.4895 0.091 Uiso 1 1 calc R . . H37C H 0.9496 0.3134 0.4918 0.091 Uiso 1 1 calc R . . O5 O 1.1749(17) 0.1716(11) 0.5010(10) 0.0449(18) Uani 0.594(11) 1 d PDU A 1 C38 C 1.2189(14) 0.1617(8) 0.5870(10) 0.0454(17) Uani 0.594(11) 1 d PDU A 1 H38A H 1.2337 0.1208 0.5971 0.054 Uiso 0.594(11) 1 calc PR A 1 H38B H 1.1711 0.1743 0.6228 0.054 Uiso 0.594(11) 1 calc PR A 1 C39 C 1.3175(7) 0.1962(4) 0.6039(5) 0.0545(19) Uani 0.594(11) 1 d PDU A 1 H39A H 1.3772 0.1727 0.5969 0.065 Uiso 0.594(11) 1 calc PR A 1 H39B H 1.3299 0.2119 0.6606 0.065 Uiso 0.594(11) 1 calc PR A 1 C40 C 1.2987(6) 0.2434(3) 0.5401(4) 0.0556(16) Uani 0.594(11) 1 d PDU A 1 H40A H 1.2619 0.2757 0.5595 0.067 Uiso 0.594(11) 1 calc PR A 1 H40B H 1.3640 0.2571 0.5263 0.067 Uiso 0.594(11) 1 calc PR A 1 C41 C 1.2329(9) 0.2139(6) 0.4673(5) 0.0476(16) Uani 0.594(11) 1 d PDU A 1 H41A H 1.1863 0.2414 0.4337 0.057 Uiso 0.594(11) 1 calc PR A 1 H41B H 1.2766 0.1961 0.4319 0.057 Uiso 0.594(11) 1 calc PR A 1 O5A O 1.172(2) 0.1715(16) 0.5105(15) 0.046(2) Uani 0.406(11) 1 d PDU A 2 C38A C 1.210(2) 0.1577(12) 0.5955(15) 0.047(2) Uani 0.406(11) 1 d PDU A 2 H38C H 1.2349 0.1181 0.6007 0.057 Uiso 0.406(11) 1 calc PR A 2 H38D H 1.1543 0.1618 0.6278 0.057 Uiso 0.406(11) 1 calc PR A 2 C39A C 1.2973(10) 0.1989(6) 0.6270(7) 0.050(2) Uani 0.406(11) 1 d PDU A 2 H39C H 1.3534 0.1800 0.6658 0.060 Uiso 0.406(11) 1 calc PR A 2 H39D H 1.2727 0.2320 0.6546 0.060 Uiso 0.406(11) 1 calc PR A 2 C40A C 1.3324(7) 0.2163(6) 0.5473(6) 0.0520(18) Uani 0.406(11) 1 d PDU A 2 H40C H 1.3651 0.2543 0.5526 0.062 Uiso 0.406(11) 1 calc PR A 2 H40D H 1.3810 0.1884 0.5315 0.062 Uiso 0.406(11) 1 calc PR A 2 C41A C 1.2313(13) 0.2170(9) 0.4857(8) 0.050(2) Uani 0.406(11) 1 d PDU A 2 H41C H 1.1956 0.2538 0.4876 0.060 Uiso 0.406(11) 1 calc PR A 2 H41D H 1.2433 0.2108 0.4289 0.060 Uiso 0.406(11) 1 calc PR A 2 O6 O 1.0275(6) 0.1747(7) 0.3376(4) 0.0450(12) Uani 0.751(12) 1 d PDU A 1 C42 C 1.0940(5) 0.1630(6) 0.2795(4) 0.0465(13) Uani 0.751(12) 1 d PDU A 1 H42A H 1.1132 0.1223 0.2809 0.056 Uiso 0.751(12) 1 calc PR A 1 H42B H 1.1574 0.1861 0.2921 0.056 Uiso 0.751(12) 1 calc PR A 1 C43 C 1.0310(5) 0.1788(3) 0.1958(3) 0.0524(13) Uani 0.751(12) 1 d PDU A 1 H43A H 1.0323 0.2202 0.1860 0.063 Uiso 0.751(12) 1 calc PR A 1 H43B H 1.0552 0.1586 0.1505 0.063 Uiso 0.751(12) 1 calc PR A 1 C44 C 0.9250(4) 0.1588(3) 0.2055(4) 0.0522(13) Uani 0.751(12) 1 d PDU A 1 H44A H 0.9172 0.1175 0.1960 0.063 Uiso 0.751(12) 1 calc PR A 1 H44B H 0.8705 0.1790 0.1669 0.063 Uiso 0.751(12) 1 calc PR A 1 C45 C 0.9216(4) 0.1738(3) 0.2946(3) 0.0575(14) Uani 0.751(12) 1 d PDU A 1 H45A H 0.8893 0.2114 0.2978 0.069 Uiso 0.751(12) 1 calc PR A 1 H45B H 0.8818 0.1451 0.3191 0.069 Uiso 0.751(12) 1 calc PR A 1 O6A O 1.039(2) 0.177(2) 0.3388(13) 0.047(2) Uani 0.249(12) 1 d PDU A 2 C42A C 1.0791(15) 0.1609(19) 0.2663(14) 0.048(2) Uani 0.249(12) 1 d PDU A 2 H42C H 1.0965 0.1200 0.2679 0.058 Uiso 0.249(12) 1 calc PR A 2 H42D H 1.1420 0.1829 0.2637 0.058 Uiso 0.249(12) 1 calc PR A 2 C43A C 0.9960(16) 0.1738(11) 0.1920(10) 0.052(2) Uani 0.249(12) 1 d PDU A 2 H43C H 1.0057 0.2117 0.1687 0.062 Uiso 0.249(12) 1 calc PR A 2 H43D H 0.9937 0.1447 0.1484 0.062 Uiso 0.249(12) 1 calc PR A 2 C44A C 0.9005(12) 0.1719(8) 0.2299(12) 0.055(2) Uani 0.249(12) 1 d PDU A 2 H44C H 0.8798 0.1325 0.2395 0.066 Uiso 0.249(12) 1 calc PR A 2 H44D H 0.8421 0.1921 0.1956 0.066 Uiso 0.249(12) 1 calc PR A 2 C45A C 0.9402(12) 0.2029(9) 0.3103(9) 0.054(2) Uani 0.249(12) 1 d PDU A 2 H45C H 0.9476 0.2441 0.3009 0.065 Uiso 0.249(12) 1 calc PR A 2 H45D H 0.8939 0.1973 0.3502 0.065 Uiso 0.249(12) 1 calc PR A 2 O7 O 0.6156(4) 0.0155(2) -0.0025(3) 0.0768(13) Uani 0.50 1 d PDU B -1 C46 C 0.5688(9) -0.0380(5) 0.0029(10) 0.087(3) Uani 0.50 1 d PDU B -1 H46A H 0.6148 -0.0629 0.0418 0.104 Uiso 0.50 1 calc PR B -1 H46B H 0.5545 -0.0566 -0.0519 0.104 Uiso 0.50 1 calc PR B -1 C47 C 0.4702(9) -0.0276(4) 0.0332(9) 0.097(3) Uani 0.50 1 d PDU B -1 H47A H 0.4137 -0.0511 0.0024 0.116 Uiso 0.50 1 calc PR B -1 H47B H 0.4784 -0.0362 0.0927 0.116 Uiso 0.50 1 calc PR B -1 C48 C 0.4493(10) 0.0344(5) 0.0170(11) 0.098(3) Uani 0.50 1 d PDU B -1 H48A H 0.4500 0.0550 0.0694 0.117 Uiso 0.50 1 calc PR B -1 H48B H 0.3815 0.0399 -0.0193 0.117 Uiso 0.50 1 calc PR B -1 C49 C 0.5341(8) 0.0554(4) -0.0244(9) 0.088(2) Uani 0.50 1 d PDU B -1 H49A H 0.5108 0.0568 -0.0850 0.106 Uiso 0.50 1 calc PR B -1 H49B H 0.5566 0.0938 -0.0044 0.106 Uiso 0.50 1 calc PR B -1 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 0.0351(4) 0.0279(3) 0.0278(3) -0.0019(3) 0.0071(3) -0.0017(3) Si1 0.0319(4) 0.0254(4) 0.0273(4) 0.0003(3) 0.0033(3) 0.0010(3) Al1 0.0262(4) 0.0268(4) 0.0231(4) -0.0006(3) 0.0025(3) -0.0009(3) O1 0.0347(10) 0.0284(9) 0.0291(10) 0.0016(7) 0.0036(8) 0.0005(8) N1 0.0284(11) 0.0303(12) 0.0255(11) -0.0009(9) 0.0031(9) -0.0017(9) C1 0.0409(16) 0.0559(19) 0.0328(16) 0.0063(14) 0.0086(13) -0.0087(14) Li1 0.043(3) 0.032(2) 0.036(3) -0.0004(19) 0.006(2) 0.004(2) O2 0.0363(10) 0.0280(9) 0.0308(10) 0.0020(8) 0.0058(8) 0.0016(8) N2 0.0274(11) 0.0290(11) 0.0235(11) -0.0014(9) 0.0035(9) -0.0023(9) Li2 0.040(3) 0.042(3) 0.041(3) 0.005(2) 0.009(2) -0.004(2) O3 0.0339(10) 0.0324(10) 0.0361(10) -0.0016(8) 0.0002(8) 0.0059(8) C2 0.0339(14) 0.0297(14) 0.0256(14) -0.0021(11) 0.0046(11) -0.0049(11) C3 0.0382(16) 0.0340(15) 0.0281(14) 0.0058(12) 0.0045(12) -0.0021(12) O4 0.0403(10) 0.0255(9) 0.0376(10) 0.0013(8) 0.0017(8) -0.0033(8) C4 0.0312(14) 0.0313(14) 0.0259(14) -0.0015(11) 0.0033(11) 0.0027(11) C5 0.0385(16) 0.0429(17) 0.0293(15) 0.0076(12) -0.0013(12) 0.0017(13) C6 0.0314(14) 0.0327(14) 0.0225(13) 0.0011(11) -0.0002(11) -0.0057(11) C7 0.0313(14) 0.0412(16) 0.0243(13) -0.0004(11) 0.0003(11) -0.0037(12) C8 0.0345(16) 0.057(2) 0.0389(17) -0.0035(14) 0.0073(13) -0.0051(14) C9 0.0378(17) 0.0539(19) 0.0507(19) -0.0091(15) 0.0072(14) -0.0178(15) C10 0.0491(18) 0.0409(17) 0.0418(17) -0.0102(14) 0.0049(14) -0.0155(14) C11 0.0400(16) 0.0370(16) 0.0261(14) -0.0011(12) -0.0009(12) -0.0052(13) C12 0.0406(16) 0.0340(16) 0.0448(17) -0.0094(13) 0.0062(13) -0.0050(13) C13 0.057(2) 0.0479(19) 0.0459(19) -0.0049(15) 0.0015(15) 0.0073(16) C14 0.093(3) 0.059(2) 0.053(2) 0.0064(17) 0.0350(19) 0.022(2) C15 0.0326(14) 0.0386(16) 0.0347(15) -0.0036(12) 0.0056(12) 0.0004(12) C16 0.0491(19) 0.052(2) 0.054(2) -0.0021(15) 0.0029(15) 0.0136(15) C17 0.0388(16) 0.0486(18) 0.0392(17) -0.0081(14) 0.0070(13) -0.0018(14) C18 0.0259(13) 0.0366(15) 0.0266(13) 0.0030(11) 0.0059(11) -0.0011(11) C19 0.0296(14) 0.0363(15) 0.0302(14) 0.0032(12) 0.0055(11) -0.0025(12) C20 0.0274(14) 0.0449(17) 0.0392(16) 0.0024(13) 0.0025(12) -0.0052(12) C21 0.0266(15) 0.0519(18) 0.0415(17) 0.0015(14) 0.0059(12) 0.0035(13) C22 0.0373(16) 0.0418(17) 0.0430(17) -0.0019(13) 0.0120(13) 0.0071(13) C23 0.0319(14) 0.0389(16) 0.0317(15) -0.0030(12) 0.0072(12) -0.0011(12) C24 0.0358(16) 0.0425(17) 0.0442(17) -0.0112(13) 0.0030(13) 0.0052(13) C25 0.061(2) 0.0446(19) 0.061(2) -0.0096(16) 0.0061(17) -0.0043(16) C26 0.107(3) 0.061(2) 0.042(2) -0.0079(17) -0.0040(19) -0.015(2) C27 0.0316(15) 0.0343(15) 0.0414(16) 0.0013(12) -0.0033(12) -0.0047(12) C28 0.0435(17) 0.0437(17) 0.0409(17) -0.0065(13) 0.0042(13) -0.0025(14) C29 0.059(2) 0.0429(18) 0.0471(18) 0.0032(14) 0.0026(15) -0.0101(15) C30 0.0338(15) 0.0343(15) 0.0328(15) 0.0005(12) 0.0004(12) 0.0048(12) C31 0.0365(16) 0.0383(16) 0.0389(16) 0.0013(13) -0.0007(12) -0.0007(13) C32 0.0458(17) 0.0444(17) 0.0399(17) 0.0072(13) 0.0044(13) 0.0052(14) C33 0.0419(17) 0.056(2) 0.0431(17) 0.0035(14) 0.0042(14) 0.0133(15) C34 0.0556(19) 0.0251(14) 0.0465(18) -0.0018(13) 0.0074(14) -0.0045(13) C35 0.075(2) 0.0332(18) 0.088(3) -0.0122(17) 0.022(2) 0.0037(17) C36 0.075(2) 0.0390(19) 0.075(2) -0.0021(17) 0.0058(19) -0.0163(17) C37 0.089(3) 0.0375(18) 0.057(2) 0.0107(15) 0.0148(19) -0.0020(17) O5 0.045(3) 0.044(2) 0.043(4) 0.005(3) 0.002(3) -0.011(2) C38 0.050(4) 0.041(3) 0.043(4) 0.006(3) 0.003(3) -0.004(2) C39 0.052(4) 0.053(3) 0.052(4) 0.007(3) -0.006(3) -0.012(3) C40 0.061(3) 0.048(3) 0.054(3) 0.009(3) 0.001(3) -0.017(3) C41 0.051(3) 0.046(3) 0.047(3) 0.003(3) 0.010(3) -0.012(2) O5A 0.045(3) 0.044(3) 0.045(4) 0.001(4) 0.001(4) -0.011(3) C38A 0.048(4) 0.047(4) 0.043(4) 0.003(3) -0.001(3) -0.006(3) C39A 0.043(4) 0.055(4) 0.049(4) -0.002(4) -0.001(3) -0.004(3) C40A 0.048(3) 0.051(4) 0.055(4) -0.008(4) 0.004(3) -0.015(3) C41A 0.051(3) 0.048(4) 0.048(4) 0.002(4) 0.004(4) -0.013(3) O6 0.051(2) 0.048(2) 0.0365(16) 0.0070(16) 0.0091(15) 0.003(3) C42 0.053(2) 0.049(3) 0.037(3) 0.005(3) 0.0085(19) -0.003(3) C43 0.063(3) 0.052(3) 0.040(2) 0.0023(19) 0.005(2) -0.008(3) C44 0.053(3) 0.055(3) 0.045(3) 0.003(2) 0.003(2) 0.002(2) C45 0.052(2) 0.068(3) 0.051(3) 0.004(3) 0.0066(19) 0.010(2) O6A 0.048(4) 0.053(4) 0.041(3) 0.007(4) 0.010(3) 0.003(4) C42A 0.054(4) 0.050(4) 0.040(4) 0.000(4) 0.006(4) 0.001(4) C43A 0.058(5) 0.054(5) 0.041(4) 0.006(4) 0.002(4) -0.001(5) C44A 0.054(4) 0.060(5) 0.049(5) 0.006(4) 0.002(4) 0.002(4) C45A 0.052(4) 0.059(5) 0.050(4) 0.004(4) 0.005(4) 0.007(4) O7 0.062(3) 0.094(3) 0.078(3) 0.000(3) 0.021(3) 0.008(3) C46 0.079(5) 0.103(4) 0.081(6) 0.027(5) 0.021(5) 0.005(3) C47 0.074(5) 0.118(5) 0.101(6) 0.017(6) 0.024(4) -0.007(5) C48 0.067(5) 0.123(5) 0.108(7) 0.017(6) 0.029(5) 0.010(4) C49 0.070(5) 0.099(5) 0.101(5) 0.010(5) 0.030(4) 0.015(4) _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 Al1 2.1885(10) . ? S1 Li1 2.404(4) . ? S1 Li1 2.452(5) 3_756 ? S1 Li2 2.689(5) 3_756 ? Si1 O2 1.5929(18) . ? Si1 O1 1.6229(17) . ? Si1 O4 1.6508(18) . ? Si1 O3 1.6565(18) . ? Si1 Li1 2.954(4) . ? Al1 O1 1.7188(18) . ? Al1 N2 1.936(2) . ? Al1 N1 1.949(2) . ? N1 C2 1.339(3) . ? N1 C18 1.460(3) . ? C1 C2 1.516(4) . ? Li1 O2 1.832(5) . ? Li1 S1 2.452(5) 3_756 ? Li1 Li2 2.682(6) . ? Li1 Li1 2.695(9) 3_756 ? O2 Li2 1.870(5) . ? N2 C4 1.334(3) . ? N2 C6 1.456(3) . ? Li2 O5 1.967(11) . ? Li2 O5A 1.988(16) . ? Li2 O6 2.001(12) . ? Li2 O6A 2.02(4) . ? Li2 S1 2.689(5) 3_756 ? O3 C30 1.435(3) . ? C2 C3 1.402(4) . ? C3 C4 1.401(4) . ? O4 C34 1.445(3) . ? C4 C5 1.520(3) . ? C6 C7 1.398(4) . ? C6 C11 1.407(4) . ? C7 C8 1.397(4) . ? C7 C15 1.523(4) . ? C8 C9 1.382(4) . ? C9 C10 1.377(4) . ? C10 C11 1.398(4) . ? C11 C12 1.517(4) . ? C12 C13 1.521(4) . ? C12 C14 1.522(4) . ? C15 C16 1.532(4) . ? C15 C17 1.532(4) . ? C18 C19 1.400(3) . ? C18 C23 1.405(4) . ? C19 C20 1.402(4) . ? C19 C27 1.527(4) . ? C20 C21 1.381(4) . ? C21 C22 1.379(4) . ? C22 C23 1.399(4) . ? C23 C24 1.527(4) . ? C24 C26 1.522(4) . ? C24 C25 1.523(4) . ? C27 C28 1.520(4) . ? C27 C29 1.541(4) . ? C30 C32 1.516(4) . ? C30 C31 1.520(4) . ? C30 C33 1.532(4) . ? C34 C35 1.520(4) . ? C34 C36 1.522(4) . ? C34 C37 1.522(4) . ? O5 C41 1.433(8) . ? O5 C38 1.449(8) . ? C38 C39 1.519(8) . ? C39 C40 1.519(8) . ? C40 C41 1.513(9) . ? O5A C41A 1.436(11) . ? O5A C38A 1.436(11) . ? C38A C39A 1.527(11) . ? C39A C40A 1.533(9) . ? C40A C41A 1.520(12) . ? O6 C42 1.446(6) . ? O6 C45 1.447(7) . ? C42 C43 1.519(6) . ? C43 C44 1.518(6) . ? C44 C45 1.521(6) . ? O6A C45A 1.445(14) . ? O6A C42A 1.446(13) . ? C42A C43A 1.517(13) . ? C43A C44A 1.515(11) . ? C44A C45A 1.519(12) . ? O7 C46 1.414(11) . ? O7 C49 1.426(9) . ? C46 C47 1.505(11) . ? C47 C48 1.501(11) . ? C48 C49 1.505(11) . ? 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 Al1 S1 Li1 91.96(11) . . ? Al1 S1 Li1 137.48(11) . 3_756 ? Li1 S1 Li1 67.42(17) . 3_756 ? Al1 S1 Li2 149.08(10) . 3_756 ? Li1 S1 Li2 118.94(14) . 3_756 ? Li1 S1 Li2 62.68(14) 3_756 3_756 ? O2 Si1 O1 112.09(9) . . ? O2 Si1 O4 114.01(10) . . ? O1 Si1 O4 104.92(9) . . ? O2 Si1 O3 113.24(9) . . ? O1 Si1 O3 109.37(10) . . ? O4 Si1 O3 102.47(9) . . ? O1 Si1 Li1 81.47(11) . . ? O4 Si1 Li1 136.93(11) . . ? O3 Si1 Li1 115.63(11) . . ? O1 Al1 N2 108.92(9) . . ? O1 Al1 N1 109.51(9) . . ? N2 Al1 N1 95.08(9) . . ? O1 Al1 S1 116.08(7) . . ? N2 Al1 S1 113.75(7) . . ? N1 Al1 S1 111.50(7) . . ? Si1 O1 Al1 147.43(11) . . ? C2 N1 C18 117.2(2) . . ? C2 N1 Al1 120.37(17) . . ? C18 N1 Al1 122.25(15) . . ? O2 Li1 S1 129.5(2) . . ? O2 Li1 S1 107.0(2) . 3_756 ? S1 Li1 S1 112.58(17) . 3_756 ? O2 Li1 Li2 44.15(15) . . ? S1 Li1 Li2 146.7(2) . . ? S1 Li1 Li2 63.00(15) 3_756 . ? O2 Li1 Li1 146.3(3) . 3_756 ? S1 Li1 Li1 57.12(16) . 3_756 ? S1 Li1 Li1 55.45(16) 3_756 3_756 ? Li2 Li1 Li1 109.5(3) . 3_756 ? O2 Li1 Si1 28.15(9) . . ? S1 Li1 Si1 102.52(15) . . ? S1 Li1 Si1 132.88(18) 3_756 . ? Li2 Li1 Si1 70.33(15) . . ? Li1 Li1 Si1 144.3(3) 3_756 . ? Si1 O2 Li1 118.99(17) . . ? Si1 O2 Li2 139.76(18) . . ? Li1 O2 Li2 92.8(2) . . ? C4 N2 C6 117.1(2) . . ? C4 N2 Al1 120.69(16) . . ? C6 N2 Al1 122.22(15) . . ? O2 Li2 O5 118.0(8) . . ? O2 Li2 O5A 113.2(11) . . ? O5 Li2 O5A 4.9(15) . . ? O2 Li2 O6 123.0(3) . . ? O5 Li2 O6 99.0(6) . . ? O5A Li2 O6 103.0(8) . . ? O2 Li2 O6A 126.9(7) . . ? O5 Li2 O6A 94.8(13) . . ? O5A Li2 O6A 98.9(14) . . ? O6 Li2 O6A 4.4(13) . . ? O2 Li2 Li1 43.04(14) . . ? O5 Li2 Li1 130.6(5) . . ? O5A Li2 Li1 126.9(7) . . ? O6 Li2 Li1 130.1(5) . . ? O6A Li2 Li1 134.0(13) . . ? O2 Li2 S1 97.19(19) . 3_756 ? O5 Li2 S1 116.8(10) . 3_756 ? O5A Li2 S1 117.9(14) . 3_756 ? O6 Li2 S1 103.0(4) . 3_756 ? O6A Li2 S1 103.7(12) . 3_756 ? Li1 Li2 S1 54.32(13) . 3_756 ? C30 O3 Si1 131.95(16) . . ? N1 C2 C3 123.3(2) . . ? N1 C2 C1 121.0(2) . . ? C3 C2 C1 115.7(2) . . ? C4 C3 C2 127.4(2) . . ? C34 O4 Si1 131.22(17) . . ? N2 C4 C3 123.4(2) . . ? N2 C4 C5 121.2(2) . . ? C3 C4 C5 115.4(2) . . ? C7 C6 C11 121.4(2) . . ? C7 C6 N2 120.6(2) . . ? C11 C6 N2 117.9(2) . . ? C8 C7 C6 118.1(2) . . ? C8 C7 C15 118.8(2) . . ? C6 C7 C15 123.1(2) . . ? C9 C8 C7 121.4(3) . . ? C10 C9 C8 119.7(3) . . ? C9 C10 C11 121.4(3) . . ? C10 C11 C6 117.9(3) . . ? C10 C11 C12 119.7(2) . . ? C6 C11 C12 122.3(2) . . ? C11 C12 C13 112.8(2) . . ? C11 C12 C14 110.3(2) . . ? C13 C12 C14 110.6(2) . . ? C7 C15 C16 113.0(2) . . ? C7 C15 C17 110.3(2) . . ? C16 C15 C17 109.7(2) . . ? C19 C18 C23 121.4(2) . . ? C19 C18 N1 120.2(2) . . ? C23 C18 N1 118.5(2) . . ? C18 C19 C20 118.1(2) . . ? C18 C19 C27 124.2(2) . . ? C20 C19 C27 117.7(2) . . ? C21 C20 C19 121.3(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 121.3(3) . . ? C22 C23 C18 118.1(2) . . ? C22 C23 C24 119.7(2) . . ? C18 C23 C24 122.2(2) . . ? C26 C24 C25 109.8(2) . . ? C26 C24 C23 111.3(2) . . ? C25 C24 C23 113.3(2) . . ? C28 C27 C19 110.8(2) . . ? C28 C27 C29 109.7(2) . . ? C19 C27 C29 112.1(2) . . ? O3 C30 C32 109.4(2) . . ? O3 C30 C31 110.1(2) . . ? C32 C30 C31 111.3(2) . . ? O3 C30 C33 105.6(2) . . ? C32 C30 C33 110.3(2) . . ? C31 C30 C33 110.1(2) . . ? O4 C34 C35 109.6(2) . . ? O4 C34 C36 106.1(2) . . ? C35 C34 C36 109.3(3) . . ? O4 C34 C37 110.4(2) . . ? C35 C34 C37 111.0(3) . . ? C36 C34 C37 110.3(3) . . ? C41 O5 C38 110.4(7) . . ? C41 O5 Li2 127.5(9) . . ? C38 O5 Li2 122.0(9) . . ? O5 C38 C39 105.4(6) . . ? C38 C39 C40 104.0(6) . . ? C41 C40 C39 102.1(6) . . ? O5 C41 C40 106.3(7) . . ? C41A O5A C38A 109.9(10) . . ? C41A O5A Li2 128.4(14) . . ? C38A O5A Li2 121.5(13) . . ? O5A C38A C39A 106.9(9) . . ? C38A C39A C40A 102.3(9) . . ? C41A C40A C39A 101.8(8) . . ? O5A C41A C40A 105.2(11) . . ? C42 O6 C45 109.2(5) . . ? C42 O6 Li2 120.6(7) . . ? C45 O6 Li2 112.6(8) . . ? O6 C42 C43 104.9(5) . . ? C44 C43 C42 100.8(4) . . ? C43 C44 C45 103.2(4) . . ? O6 C45 C44 105.9(4) . . ? C45A O6A C42A 107.0(14) . . ? C45A O6A Li2 113(2) . . ? C42A O6A Li2 129(3) . . ? O6A C42A C43A 107.1(12) . . ? C44A C43A C42A 101.2(11) . . ? C43A C44A C45A 99.7(11) . . ? O6A C45A C44A 102.7(14) . . ? C46 O7 C49 106.6(8) . . ? O7 C46 C47 107.0(8) . . ? C48 C47 C46 104.0(7) . . ? C47 C48 C49 105.9(8) . . ? O7 C49 C48 105.2(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.354 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.048