# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Robert Davies' _publ_contact_author_address ; Dept of Chemistry Imperial College London Exhibition Road South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email R.DAVIES@IMPERIAL.AC.UK _publ_section_title ; Aluminium Complexes with Thio-Phosphorus Ligands: Syntheses and Characterisations of [Al2(CyPS3)2(CyPHS2)2] and [Al(S2PPh2)3] ; loop_ _publ_author_name 'Robert Davies' "Mar\'ia Gimenez" 'Laura Patel' 'Andrew J. P. White' # Attachment 'Structures123.cif' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 696777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H46 Al2 P4 S10, C7 H8' _chemical_formula_sum 'C31 H54 Al2 P4 S10' _chemical_formula_weight 925.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 13.8035(3) _cell_length_b 13.4034(3) _cell_length_c 11.7729(2) _cell_angle_alpha 90 _cell_angle_beta 90.7425(19) _cell_angle_gamma 90 _cell_volume 2177.97(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15125 _cell_measurement_theta_min 3.7168 _cell_measurement_theta_max 32.5803 _exptl_crystal_description cubes _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84525 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21647 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 32.65 _reflns_number_total 7459 _reflns_number_gt 5860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.8704P] 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 7459 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al 0.52274(5) 0.45331(4) 0.35396(5) 0.03564(13) Uani 1 1 d . . . P1 P 0.33388(4) 0.43993(4) 0.48502(4) 0.03309(11) Uani 1 1 d . . . S1 S 0.46553(4) 0.38390(3) 0.54130(4) 0.03286(10) Uani 1 1 d . . . S2 S 0.35300(4) 0.47480(4) 0.32009(4) 0.04212(13) Uani 1 1 d . . . S3 S 0.31261(4) 0.56064(4) 0.58419(4) 0.03966(12) Uani 1 1 d . . . P2 P 0.56130(5) 0.37213(4) 0.12645(4) 0.04198(14) Uani 1 1 d . . . H2 H 0.4962(19) 0.353(2) 0.048(2) 0.054(8) Uiso 1 1 d . . . S4 S 0.53094(5) 0.29284(4) 0.26711(4) 0.04700(15) Uani 1 1 d . . . S5 S 0.55858(4) 0.51809(4) 0.16904(4) 0.03947(12) Uani 1 1 d . . . C1 C 0.23925(14) 0.34639(14) 0.50147(15) 0.0327(4) Uani 1 1 d . . . H1A H 0.1782 0.3739 0.4672 0.039 Uiso 1 1 calc R . . C2 C 0.26418(17) 0.25044(16) 0.43757(17) 0.0420(5) Uani 1 1 d . . . H2A H 0.2738 0.2658 0.3562 0.050 Uiso 1 1 calc R . . H2B H 0.3253 0.2223 0.4686 0.050 Uiso 1 1 calc R . . C3 C 0.18300(19) 0.17394(17) 0.44923(18) 0.0472(5) Uani 1 1 d . . . H3A H 0.1239 0.1992 0.4104 0.057 Uiso 1 1 calc R . . H3B H 0.2022 0.1111 0.4116 0.057 Uiso 1 1 calc R . . C4 C 0.16070(18) 0.15300(16) 0.57278(18) 0.0443(5) Uani 1 1 d . . . H4A H 0.1045 0.1073 0.5770 0.053 Uiso 1 1 calc R . . H4B H 0.2170 0.1195 0.6092 0.053 Uiso 1 1 calc R . . C5 C 0.13838(18) 0.24814(17) 0.63648(19) 0.0459(5) Uani 1 1 d . . . H5A H 0.1283 0.2323 0.7176 0.055 Uiso 1 1 calc R . . H5B H 0.0776 0.2774 0.6058 0.055 Uiso 1 1 calc R . . C6 C 0.22003(17) 0.32436(16) 0.62661(16) 0.0407(4) Uani 1 1 d . . . H6A H 0.2796 0.2979 0.6634 0.049 Uiso 1 1 calc R . . H6B H 0.2018 0.3867 0.6660 0.049 Uiso 1 1 calc R . . C7 C 0.67432(19) 0.33470(17) 0.06265(18) 0.0470(5) Uani 1 1 d . . . H7A H 0.6687 0.2624 0.0425 0.056 Uiso 1 1 calc R . . C8 C 0.69260(19) 0.3923(2) -0.04707(19) 0.0541(6) Uani 1 1 d . . . H8A H 0.6382 0.3809 -0.1012 0.065 Uiso 1 1 calc R . . H8B H 0.6959 0.4646 -0.0304 0.065 Uiso 1 1 calc R . . C9 C 0.7869(2) 0.3587(3) -0.1005(2) 0.0650(7) Uani 1 1 d . . . H9A H 0.7804 0.2883 -0.1250 0.078 Uiso 1 1 calc R . . H9B H 0.7991 0.3996 -0.1689 0.078 Uiso 1 1 calc R . . C10 C 0.8722(2) 0.3680(2) -0.0192(3) 0.0626(7) Uani 1 1 d . . . H10A H 0.9310 0.3410 -0.0555 0.075 Uiso 1 1 calc R . . H10B H 0.8839 0.4393 -0.0018 0.075 Uiso 1 1 calc R . . C11 C 0.8537(3) 0.3121(2) 0.0894(3) 0.0715(8) Uani 1 1 d . . . H11A H 0.9086 0.3230 0.1429 0.086 Uiso 1 1 calc R . . H11B H 0.8499 0.2398 0.0729 0.086 Uiso 1 1 calc R . . C12 C 0.7599(2) 0.3457(2) 0.1451(2) 0.0549(6) Uani 1 1 d . . . H12A H 0.7484 0.3049 0.2137 0.066 Uiso 1 1 calc R . . H12B H 0.7660 0.4163 0.1688 0.066 Uiso 1 1 calc R . . C20 C -0.0150(9) 0.5126(9) 0.6857(10) 0.102(7) Uani 0.50 1 d P A -1 H20A H -0.0841 0.5095 0.7035 0.153 Uiso 0.50 1 calc PR A -1 H20B H 0.0116 0.5767 0.7115 0.153 Uiso 0.50 1 calc PR A -1 H20C H 0.0193 0.4581 0.7245 0.153 Uiso 0.50 1 calc PR A -1 C21 C -0.0023(3) 0.5030(4) 0.5611(4) 0.0572(13) Uani 0.50 1 d PG A -1 C22 C -0.0607(3) 0.4375(4) 0.4994(5) 0.079(5) Uani 0.50 1 d PG A -1 H22A H -0.1085 0.3991 0.5370 0.095 Uiso 0.50 1 calc PR A -1 C23 C -0.0492(4) 0.4280(4) 0.3828(5) 0.104(3) Uani 0.50 1 d PG A -1 H23A H -0.0891 0.3832 0.3407 0.125 Uiso 0.50 1 calc PR A -1 C24 C 0.0208(5) 0.4841(5) 0.3278(4) 0.087(6) Uani 0.50 1 d PG A -1 H24A H 0.0286 0.4776 0.2481 0.105 Uiso 0.50 1 calc PR A -1 C25 C 0.0791(4) 0.5497(4) 0.3894(4) 0.077(2) Uani 0.50 1 d PG A -1 H25A H 0.1269 0.5880 0.3519 0.092 Uiso 0.50 1 calc PR A -1 C26 C 0.0676(3) 0.5591(3) 0.5061(4) 0.079(4) Uani 0.50 1 d PG A -1 H26A H 0.1075 0.6039 0.5482 0.094 Uiso 0.50 1 calc PR A -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 Al 0.0494(3) 0.0328(3) 0.0245(2) 0.0035(2) -0.0065(2) -0.0139(2) P1 0.0439(3) 0.0311(2) 0.02413(19) 0.00475(16) -0.00694(18) -0.01230(19) S1 0.0443(2) 0.0293(2) 0.02484(18) 0.00594(15) -0.00651(16) -0.01134(17) S2 0.0506(3) 0.0499(3) 0.0256(2) 0.01237(19) -0.01087(19) -0.0189(2) S3 0.0515(3) 0.0306(2) 0.0365(2) 0.00070(18) -0.0099(2) -0.0076(2) P2 0.0611(3) 0.0393(3) 0.0254(2) 0.00162(19) -0.0041(2) -0.0199(2) S4 0.0785(4) 0.0333(2) 0.0292(2) 0.00139(18) -0.0010(2) -0.0223(2) S5 0.0536(3) 0.0361(2) 0.0286(2) 0.00749(17) -0.00268(19) -0.0129(2) C1 0.0385(9) 0.0326(8) 0.0270(8) 0.0029(6) -0.0044(7) -0.0087(7) C2 0.0552(12) 0.0398(10) 0.0313(9) -0.0075(8) 0.0078(8) -0.0176(9) C3 0.0641(14) 0.0410(11) 0.0367(10) -0.0061(8) 0.0046(9) -0.0241(10) C4 0.0559(13) 0.0360(10) 0.0410(10) 0.0054(8) 0.0028(9) -0.0148(9) C5 0.0543(13) 0.0448(11) 0.0389(10) -0.0016(9) 0.0108(9) -0.0166(10) C6 0.0543(12) 0.0393(10) 0.0285(8) -0.0033(7) 0.0057(8) -0.0141(9) C7 0.0705(15) 0.0369(10) 0.0337(9) -0.0029(8) 0.0004(9) -0.0144(10) C8 0.0534(13) 0.0743(17) 0.0344(10) 0.0096(11) -0.0048(9) -0.0166(12) C9 0.0681(17) 0.086(2) 0.0411(12) -0.0007(13) 0.0047(12) -0.0113(15) C10 0.0601(16) 0.0626(16) 0.0651(17) -0.0065(13) 0.0003(13) 0.0060(13) C11 0.086(2) 0.0632(17) 0.0650(17) -0.0069(14) -0.0093(15) 0.0292(16) C12 0.0755(17) 0.0511(13) 0.0380(11) 0.0034(10) -0.0090(11) 0.0121(12) C20 0.133(13) 0.104(14) 0.070(6) 0.007(7) 0.048(7) 0.038(10) C21 0.047(3) 0.053(3) 0.072(3) 0.011(3) 0.010(2) 0.014(2) C22 0.041(4) 0.080(7) 0.116(11) 0.006(6) 0.004(5) -0.043(4) C23 0.073(5) 0.111(7) 0.129(8) -0.047(6) -0.011(5) -0.025(5) C24 0.093(10) 0.099(13) 0.069(7) -0.007(7) -0.017(7) 0.037(9) C25 0.095(5) 0.054(3) 0.083(4) -0.003(3) 0.040(4) -0.005(3) C26 0.102(8) 0.051(5) 0.084(8) -0.016(5) 0.028(6) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al S3 2.3849(8) 3_666 ? Al S4 2.3849(8) . ? Al S2 2.3890(9) . ? Al S5 2.4012(7) . ? Al S1 2.5105(7) 3_666 ? Al S1 2.5296(7) . ? P1 C1 1.8226(18) . ? P1 S2 2.0178(6) . ? P1 S3 2.0189(7) . ? P1 S1 2.0674(7) . ? S1 Al 2.5105(7) 3_666 ? S3 Al 2.3849(8) 3_666 ? P2 C7 1.811(3) . ? P2 S4 2.0162(7) . ? P2 S5 2.0201(8) . ? C1 C6 1.529(3) . ? C1 C2 1.531(3) . ? C2 C3 1.526(3) . ? C3 C4 1.517(3) . ? C4 C5 1.513(3) . ? C5 C6 1.527(3) . ? C7 C12 1.526(3) . ? C7 C8 1.528(3) . ? C8 C9 1.521(4) . ? C9 C10 1.514(4) . ? C10 C11 1.506(4) . ? C11 C12 1.526(4) . ? C20 C21 1.486(10) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? 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 S3 Al S4 90.57(3) 3_666 . ? S3 Al S2 171.53(3) 3_666 . ? S4 Al S2 95.11(3) . . ? S3 Al S5 95.65(3) 3_666 . ? S4 Al S5 85.75(3) . . ? S2 Al S5 91.04(3) . . ? S3 Al S1 82.13(2) 3_666 3_666 ? S4 Al S1 172.45(4) . 3_666 ? S2 Al S1 91.95(3) . 3_666 ? S5 Al S1 96.80(2) . 3_666 ? S3 Al S1 90.68(2) 3_666 . ? S4 Al S1 93.39(2) . . ? S2 Al S1 82.72(3) . . ? S5 Al S1 173.61(3) . . ? S1 Al S1 84.85(2) 3_666 . ? C1 P1 S2 111.38(6) . . ? C1 P1 S3 112.33(7) . . ? S2 P1 S3 113.12(3) . . ? C1 P1 S1 110.14(7) . . ? S2 P1 S1 105.50(3) . . ? S3 P1 S1 103.86(3) . . ? P1 S1 Al 83.83(3) . 3_666 ? P1 S1 Al 82.53(2) . . ? Al S1 Al 95.15(2) 3_666 . ? P1 S2 Al 87.23(3) . . ? P1 S3 Al 88.20(3) . 3_666 ? C7 P2 S4 112.58(8) . . ? C7 P2 S5 112.96(7) . . ? S4 P2 S5 107.57(3) . . ? P2 S4 Al 83.58(3) . . ? P2 S5 Al 83.08(3) . . ? C6 C1 C2 110.74(16) . . ? C6 C1 P1 111.64(13) . . ? C2 C1 P1 111.07(14) . . ? C3 C2 C1 110.49(18) . . ? C4 C3 C2 111.64(17) . . ? C5 C4 C3 111.37(18) . . ? C4 C5 C6 111.78(18) . . ? C5 C6 C1 109.88(16) . . ? C12 C7 C8 110.7(2) . . ? C12 C7 P2 111.93(16) . . ? C8 C7 P2 111.30(18) . . ? C9 C8 C7 110.6(2) . . ? C10 C9 C8 112.2(2) . . ? C11 C10 C9 110.9(3) . . ? C10 C11 C12 111.8(2) . . ? C7 C12 C11 110.6(2) . . ? C22 C21 C26 120.0 . . ? C22 C21 C20 119.7(6) . . ? C26 C21 C20 120.3(6) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.407 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.070 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 696778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H54 Li2 N4 P2 S4' _chemical_formula_sum 'C24 H54 Li2 N4 P2 S4' _chemical_formula_weight 602.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0103(17) _cell_length_b 10.680(2) _cell_length_c 18.826(3) _cell_angle_alpha 95.329(15) _cell_angle_beta 101.726(14) _cell_angle_gamma 101.575(18) _cell_volume 1720.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25117 _cell_measurement_theta_min 2.4186 _cell_measurement_theta_max 70.6747 _exptl_crystal_description 'blocky needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 3.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90873 _exptl_absorpt_correction_T_max 1.10343 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36354 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0113 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 71.33 _reflns_number_total 6577 _reflns_number_gt 5862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+3.1233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6577 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Li1 Li 0.1893(6) 0.4882(5) 0.1591(3) 0.0388(11) Uani 1 1 d . . . Li2 Li 0.3148(6) 1.0336(5) 0.3453(3) 0.0385(11) Uani 1 1 d . . . P1 P 0.27781(8) 0.71267(7) 0.30123(4) 0.02826(16) Uani 1 1 d . . . P2 P 0.23216(8) 0.80091(7) 0.19746(4) 0.02886(16) Uani 1 1 d . . . S1 S 0.37354(9) 0.56541(7) 0.27757(4) 0.03577(18) Uani 1 1 d . . . S2 S 0.39866(9) 0.84672(7) 0.38499(4) 0.03636(18) Uani 1 1 d . . . S3 S 0.06474(9) 0.66700(7) 0.12796(4) 0.03662(18) Uani 1 1 d . . . S4 S 0.18896(9) 0.97538(7) 0.21589(4) 0.03646(18) Uani 1 1 d . . . N1 N 0.3054(3) 0.3930(3) 0.09476(14) 0.0393(6) Uani 1 1 d . . . N2 N 0.0112(3) 0.3212(2) 0.13616(14) 0.0386(6) Uani 1 1 d . . . N3 N 0.4949(3) 1.2002(2) 0.37367(14) 0.0356(5) Uani 1 1 d . . . N4 N 0.1925(3) 1.1286(2) 0.40869(14) 0.0355(5) Uani 1 1 d . . . C1 C 0.0836(3) 0.6454(3) 0.31560(16) 0.0330(6) Uani 1 1 d . . . H1A H 0.0250 0.5842 0.2706 0.040 Uiso 1 1 calc R . . C2 C -0.0114(4) 0.7456(3) 0.32697(19) 0.0412(7) Uani 1 1 d . . . H2A H -0.0233 0.7929 0.2841 0.049 Uiso 1 1 calc R . . H2B H 0.0440 0.8086 0.3709 0.049 Uiso 1 1 calc R . . C3 C -0.1721(4) 0.6808(4) 0.3368(2) 0.0523(9) Uani 1 1 d . . . H3A H -0.2295 0.7478 0.3469 0.063 Uiso 1 1 calc R . . H3B H -0.2316 0.6249 0.2908 0.063 Uiso 1 1 calc R . . C4 C -0.1594(4) 0.6002(4) 0.3992(2) 0.0528(9) Uani 1 1 d . . . H4A H -0.1112 0.6577 0.4461 0.063 Uiso 1 1 calc R . . H4B H -0.2649 0.5549 0.4019 0.063 Uiso 1 1 calc R . . C5 C -0.0627(4) 0.5020(3) 0.3887(2) 0.0518(9) Uani 1 1 d . . . H5A H -0.1168 0.4386 0.3447 0.062 Uiso 1 1 calc R . . H5B H -0.0513 0.4547 0.4316 0.062 Uiso 1 1 calc R . . C6 C 0.0980(4) 0.5671(3) 0.37966(18) 0.0417(7) Uani 1 1 d . . . H6A H 0.1571 0.5008 0.3707 0.050 Uiso 1 1 calc R . . H6B H 0.1559 0.6248 0.4253 0.050 Uiso 1 1 calc R . . C7 C 0.4124(3) 0.8120(3) 0.16442(16) 0.0333(6) Uani 1 1 d . . . H7A H 0.4288 0.7223 0.1571 0.040 Uiso 1 1 calc R . . C8 C 0.5592(4) 0.8937(3) 0.21735(18) 0.0429(7) Uani 1 1 d . . . H8A H 0.5480 0.9838 0.2262 0.052 Uiso 1 1 calc R . . H8B H 0.5729 0.8597 0.2648 0.052 Uiso 1 1 calc R . . C9 C 0.7011(4) 0.8911(4) 0.1857(2) 0.0533(9) Uani 1 1 d . . . H9A H 0.7938 0.9485 0.2193 0.064 Uiso 1 1 calc R . . H9B H 0.7186 0.8024 0.1823 0.064 Uiso 1 1 calc R . . C10 C 0.6823(4) 0.9341(4) 0.1105(2) 0.0559(9) Uani 1 1 d . . . H10A H 0.7733 0.9244 0.0903 0.067 Uiso 1 1 calc R . . H10B H 0.6789 1.0265 0.1149 0.067 Uiso 1 1 calc R . . C11 C 0.5344(4) 0.8553(4) 0.05822(19) 0.0500(8) Uani 1 1 d . . . H11A H 0.5438 0.7648 0.0487 0.060 Uiso 1 1 calc R . . H11B H 0.5213 0.8901 0.0110 0.060 Uiso 1 1 calc R . . C12 C 0.3918(4) 0.8583(3) 0.08947(17) 0.0417(7) Uani 1 1 d . . . H12A H 0.2985 0.8022 0.0556 0.050 Uiso 1 1 calc R . . H12B H 0.3756 0.9475 0.0941 0.050 Uiso 1 1 calc R . . C13 C 0.4733(4) 0.4066(4) 0.1217(2) 0.0552(9) Uani 1 1 d . . . H13A H 0.5131 0.3569 0.0864 0.083 Uiso 1 1 calc R . . H13B H 0.4928 0.3741 0.1690 0.083 Uiso 1 1 calc R . . H13C H 0.5263 0.4978 0.1278 0.083 Uiso 1 1 calc R . . C14 C 0.2776(4) 0.4427(4) 0.02476(18) 0.0482(8) Uani 1 1 d . . . H14A H 0.3296 0.4014 -0.0087 0.072 Uiso 1 1 calc R . . H14B H 0.3191 0.5362 0.0325 0.072 Uiso 1 1 calc R . . H14C H 0.1655 0.4237 0.0034 0.072 Uiso 1 1 calc R . . C15 C 0.2236(5) 0.2573(3) 0.0877(2) 0.0545(9) Uani 1 1 d . . . H15A H 0.2640 0.2208 0.1322 0.065 Uiso 1 1 calc R . . H15B H 0.2453 0.2079 0.0453 0.065 Uiso 1 1 calc R . . C16 C 0.0510(5) 0.2415(3) 0.07746(19) 0.0540(9) Uani 1 1 d . . . H16A H 0.0081 0.2664 0.0295 0.065 Uiso 1 1 calc R . . H16B H 0.0024 0.1496 0.0771 0.065 Uiso 1 1 calc R . . C17 C -0.1471(4) 0.3399(4) 0.1132(3) 0.0618(11) Uani 1 1 d . . . H17A H -0.2213 0.2562 0.1040 0.093 Uiso 1 1 calc R . . H17B H -0.1564 0.3801 0.0682 0.093 Uiso 1 1 calc R . . H17C H -0.1697 0.3960 0.1519 0.093 Uiso 1 1 calc R . . C18 C 0.0226(4) 0.2606(3) 0.20272(18) 0.0428(7) Uani 1 1 d . . . H18A H -0.0590 0.1813 0.1943 0.064 Uiso 1 1 calc R . . H18B H 0.0095 0.3202 0.2427 0.064 Uiso 1 1 calc R . . H18C H 0.1248 0.2397 0.2159 0.064 Uiso 1 1 calc R . . C19 C 0.5025(4) 1.2629(3) 0.30843(18) 0.0426(7) Uani 1 1 d . . . H19A H 0.5862 1.3411 0.3208 0.064 Uiso 1 1 calc R . . H19B H 0.4032 1.2859 0.2900 0.064 Uiso 1 1 calc R . . H19C H 0.5233 1.2037 0.2706 0.064 Uiso 1 1 calc R . . C20 C 0.6471(4) 1.1745(3) 0.4039(2) 0.0503(9) Uani 1 1 d . . . H20A H 0.7258 1.2558 0.4161 0.075 Uiso 1 1 calc R . . H20B H 0.6742 1.1165 0.3675 0.075 Uiso 1 1 calc R . . H20C H 0.6431 1.1338 0.4482 0.075 Uiso 1 1 calc R . . C21 C 0.4485(4) 1.2808(3) 0.42933(18) 0.0436(7) Uani 1 1 d . . . H21A H 0.4980 1.3726 0.4300 0.052 Uiso 1 1 calc R . . H21B H 0.4852 1.2566 0.4783 0.052 Uiso 1 1 calc R . . C22 C 0.2746(4) 1.2639(3) 0.41332(19) 0.0428(7) Uani 1 1 d . . . H22A H 0.2467 1.3170 0.4524 0.051 Uiso 1 1 calc R . . H22B H 0.2397 1.2957 0.3664 0.051 Uiso 1 1 calc R . . C23 C 0.2142(4) 1.0841(3) 0.48050(18) 0.0443(7) Uani 1 1 d . . . H23A H 0.1581 1.1271 0.5111 0.066 Uiso 1 1 calc R . . H23B H 0.3253 1.1048 0.5041 0.066 Uiso 1 1 calc R . . H23C H 0.1738 0.9905 0.4744 0.066 Uiso 1 1 calc R . . C24 C 0.0263(4) 1.1153(4) 0.3790(2) 0.0500(8) Uani 1 1 d . . . H24A H -0.0168 1.1634 0.4136 0.075 Uiso 1 1 calc R . . H24B H -0.0266 1.0239 0.3713 0.075 Uiso 1 1 calc R . . H24C H 0.0110 1.1496 0.3322 0.075 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 Li1 0.035(3) 0.037(3) 0.042(3) 0.001(2) 0.006(2) 0.006(2) Li2 0.037(3) 0.036(3) 0.042(3) 0.004(2) 0.009(2) 0.007(2) P1 0.0288(3) 0.0278(3) 0.0276(3) 0.0065(3) 0.0021(3) 0.0082(3) P2 0.0299(4) 0.0285(3) 0.0278(3) 0.0066(3) 0.0021(3) 0.0089(3) S1 0.0368(4) 0.0329(4) 0.0390(4) 0.0064(3) 0.0043(3) 0.0147(3) S2 0.0406(4) 0.0324(4) 0.0309(4) 0.0046(3) -0.0019(3) 0.0064(3) S3 0.0357(4) 0.0346(4) 0.0338(4) 0.0048(3) -0.0028(3) 0.0054(3) S4 0.0436(4) 0.0310(4) 0.0370(4) 0.0076(3) 0.0060(3) 0.0155(3) N1 0.0434(15) 0.0432(14) 0.0326(13) 0.0072(11) 0.0077(11) 0.0131(12) N2 0.0362(14) 0.0355(13) 0.0417(14) 0.0111(11) 0.0013(11) 0.0078(11) N3 0.0337(13) 0.0323(12) 0.0413(14) 0.0095(10) 0.0060(11) 0.0092(10) N4 0.0342(13) 0.0391(13) 0.0361(13) 0.0082(11) 0.0071(10) 0.0144(11) C1 0.0314(14) 0.0330(14) 0.0338(15) 0.0074(12) 0.0064(12) 0.0054(12) C2 0.0371(17) 0.0414(17) 0.0500(18) 0.0126(14) 0.0124(14) 0.0149(14) C3 0.0393(18) 0.061(2) 0.061(2) 0.0083(18) 0.0195(16) 0.0132(16) C4 0.052(2) 0.051(2) 0.057(2) 0.0029(17) 0.0274(18) 0.0016(16) C5 0.063(2) 0.0415(18) 0.055(2) 0.0111(16) 0.0288(18) 0.0032(16) C6 0.0481(19) 0.0375(16) 0.0437(17) 0.0123(14) 0.0155(15) 0.0111(14) C7 0.0329(15) 0.0342(15) 0.0342(15) 0.0078(12) 0.0073(12) 0.0097(12) C8 0.0350(16) 0.0475(18) 0.0427(17) 0.0066(14) 0.0049(14) 0.0048(14) C9 0.0345(18) 0.063(2) 0.061(2) 0.0121(18) 0.0131(16) 0.0047(16) C10 0.049(2) 0.058(2) 0.062(2) 0.0126(18) 0.0237(18) 0.0020(17) C11 0.058(2) 0.051(2) 0.0447(19) 0.0114(16) 0.0217(17) 0.0085(17) C12 0.0449(18) 0.0458(18) 0.0352(16) 0.0104(13) 0.0110(14) 0.0079(14) C13 0.049(2) 0.079(3) 0.0447(19) 0.0096(18) 0.0104(16) 0.0326(19) C14 0.053(2) 0.054(2) 0.0379(17) 0.0120(15) 0.0072(15) 0.0136(16) C15 0.079(3) 0.0421(19) 0.051(2) 0.0060(16) 0.0307(19) 0.0184(18) C16 0.070(3) 0.0405(18) 0.0408(18) -0.0001(14) 0.0102(17) -0.0063(17) C17 0.0376(19) 0.047(2) 0.092(3) 0.025(2) -0.0084(19) 0.0050(15) C18 0.0462(18) 0.0418(17) 0.0418(17) 0.0115(14) 0.0087(14) 0.0117(14) C19 0.0451(18) 0.0381(16) 0.0463(18) 0.0117(14) 0.0112(15) 0.0103(14) C20 0.0340(17) 0.0467(19) 0.068(2) 0.0183(17) 0.0028(16) 0.0077(14) C21 0.0490(19) 0.0343(16) 0.0436(18) 0.0025(13) 0.0080(15) 0.0043(14) C22 0.0506(19) 0.0380(16) 0.0468(18) 0.0078(14) 0.0176(15) 0.0187(14) C23 0.0493(19) 0.0451(18) 0.0391(17) 0.0089(14) 0.0074(14) 0.0133(15) C24 0.0394(18) 0.064(2) 0.051(2) 0.0134(17) 0.0073(15) 0.0222(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 Li1 N1 2.075(6) . ? Li1 N2 2.091(6) . ? Li1 S1 2.452(5) . ? Li1 S3 2.459(5) . ? Li2 N3 2.097(6) . ? Li2 N4 2.105(6) . ? Li2 S2 2.402(5) . ? Li2 S4 2.433(5) . ? Li2 C22 2.789(6) . ? P1 C1 1.837(3) . ? P1 S2 1.9948(11) . ? P1 S1 1.9966(11) . ? P1 P2 2.2460(10) . ? P2 C7 1.840(3) . ? P2 S4 1.9924(11) . ? P2 S3 2.0044(11) . ? N1 C14 1.459(4) . ? N1 C13 1.468(4) . ? N1 C15 1.469(4) . ? N2 C18 1.457(4) . ? N2 C17 1.464(4) . ? N2 C16 1.477(4) . ? N3 C19 1.459(4) . ? N3 C20 1.464(4) . ? N3 C21 1.472(4) . ? N4 C24 1.461(4) . ? N4 C23 1.463(4) . ? N4 C22 1.471(4) . ? C1 C2 1.524(4) . ? C1 C6 1.529(4) . ? C2 C3 1.529(5) . ? C3 C4 1.519(5) . ? C4 C5 1.516(5) . ? C5 C6 1.525(5) . ? C7 C12 1.526(4) . ? C7 C8 1.531(4) . ? C8 C9 1.520(5) . ? C9 C10 1.517(5) . ? C10 C11 1.522(5) . ? C11 C12 1.523(5) . ? C15 C16 1.500(6) . ? C21 C22 1.504(5) . ? 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 N1 Li1 N2 87.9(2) . . ? N1 Li1 S1 106.0(2) . . ? N2 Li1 S1 125.3(3) . . ? N1 Li1 S3 126.4(3) . . ? N2 Li1 S3 106.4(2) . . ? S1 Li1 S3 106.29(19) . . ? N3 Li2 N4 87.5(2) . . ? N3 Li2 S2 112.1(2) . . ? N4 Li2 S2 118.7(2) . . ? N3 Li2 S4 116.6(2) . . ? N4 Li2 S4 115.1(2) . . ? S2 Li2 S4 106.5(2) . . ? N3 Li2 C22 58.18(16) . . ? N4 Li2 C22 31.17(12) . . ? S2 Li2 C22 136.0(2) . . ? S4 Li2 C22 116.0(2) . . ? C1 P1 S2 110.39(10) . . ? C1 P1 S1 107.85(10) . . ? S2 P1 S1 116.99(5) . . ? C1 P1 P2 104.60(10) . . ? S2 P1 P2 110.67(4) . . ? S1 P1 P2 105.53(4) . . ? C7 P2 S4 110.51(10) . . ? C7 P2 S3 107.86(10) . . ? S4 P2 S3 116.85(5) . . ? C7 P2 P1 104.44(10) . . ? S4 P2 P1 111.60(4) . . ? S3 P2 P1 104.70(4) . . ? P1 S1 Li1 94.19(13) . . ? P1 S2 Li2 100.24(13) . . ? P2 S3 Li1 93.93(13) . . ? P2 S4 Li2 100.21(13) . . ? C14 N1 C13 109.1(3) . . ? C14 N1 C15 111.3(3) . . ? C13 N1 C15 110.2(3) . . ? C14 N1 Li1 105.1(3) . . ? C13 N1 Li1 117.9(3) . . ? C15 N1 Li1 103.1(2) . . ? C18 N2 C17 108.7(3) . . ? C18 N2 C16 110.9(3) . . ? C17 N2 C16 110.7(3) . . ? C18 N2 Li1 106.7(2) . . ? C17 N2 Li1 116.0(3) . . ? C16 N2 Li1 103.7(2) . . ? C19 N3 C20 109.2(3) . . ? C19 N3 C21 111.3(2) . . ? C20 N3 C21 110.0(3) . . ? C19 N3 Li2 108.5(2) . . ? C20 N3 Li2 113.5(2) . . ? C21 N3 Li2 104.3(2) . . ? C24 N4 C23 108.9(3) . . ? C24 N4 C22 109.6(3) . . ? C23 N4 C22 111.7(3) . . ? C24 N4 Li2 117.5(3) . . ? C23 N4 Li2 108.0(2) . . ? C22 N4 Li2 101.1(2) . . ? C2 C1 C6 110.5(3) . . ? C2 C1 P1 114.3(2) . . ? C6 C1 P1 109.7(2) . . ? C1 C2 C3 110.7(3) . . ? C4 C3 C2 111.3(3) . . ? C5 C4 C3 111.4(3) . . ? C4 C5 C6 111.1(3) . . ? C5 C6 C1 110.5(3) . . ? C12 C7 C8 110.9(3) . . ? C12 C7 P2 110.1(2) . . ? C8 C7 P2 115.1(2) . . ? C9 C8 C7 110.4(3) . . ? C10 C9 C8 112.0(3) . . ? C9 C10 C11 111.4(3) . . ? C10 C11 C12 111.5(3) . . ? C11 C12 C7 110.5(3) . . ? N1 C15 C16 112.4(3) . . ? N2 C16 C15 111.8(3) . . ? N3 C21 C22 110.9(3) . . ? N4 C22 C21 112.6(3) . . ? N4 C22 Li2 47.77(17) . . ? C21 C22 Li2 76.6(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 71.33 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.478 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.063 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 696779' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Al P3 S6' _chemical_formula_sum 'C36 H30 Al P3 S6' _chemical_formula_weight 774.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 34.8899(7) _cell_length_b 23.4002(5) _cell_length_c 18.2527(4) _cell_angle_alpha 90 _cell_angle_beta 90.923(2) _cell_angle_gamma 90 _cell_volume 14900.1(5) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22184 _cell_measurement_theta_min 2.2702 _cell_measurement_theta_max 62.8337 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6400 _exptl_absorpt_coefficient_mu 5.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55365 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31955 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 63.59 _reflns_number_total 31955 _reflns_number_gt 16747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31955 _refine_ls_number_parameters 1532 _refine_ls_number_restraints 2173 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.2026 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al 0.62344(6) 0.87550(8) 1.12983(11) 0.0320(5) Uani 1 1 d . . . P1 P 0.70847(5) 0.86214(8) 1.11566(10) 0.0328(4) Uani 1 1 d . . . P2 P 0.58516(5) 0.76627(8) 1.08471(10) 0.0340(4) Uani 1 1 d . . . P3 P 0.58173(6) 0.98180(8) 1.17611(10) 0.0343(5) Uani 1 1 d . . . S1 S 0.68066(5) 0.88985(8) 1.20499(10) 0.0365(4) Uani 1 1 d . . . S2 S 0.66849(5) 0.85762(8) 1.03478(9) 0.0367(4) Uani 1 1 d . . . S3 S 0.62037(5) 0.77743(7) 1.17215(9) 0.0343(4) Uani 1 1 d . . . S4 S 0.57105(6) 0.84438(8) 1.04780(10) 0.0421(5) Uani 1 1 d . . . S5 S 0.58285(5) 0.90676(7) 1.22908(10) 0.0371(5) Uani 1 1 d . . . S6 S 0.61607(6) 0.97386(8) 1.08904(10) 0.0414(5) Uani 1 1 d . . . C1 C 0.74620(12) 0.91001(16) 1.0908(2) 0.0348(18) Uani 1 1 d G . . C2 C 0.73767(11) 0.96784(18) 1.0846(2) 0.043(2) Uani 1 1 d G . . H2A H 0.7133 0.9816 1.0988 0.051 Uiso 1 1 calc R . . C3 C 0.76482(14) 1.00550(13) 1.0576(2) 0.047(2) Uani 1 1 d G . . H3A H 0.7590 1.0450 1.0533 0.056 Uiso 1 1 calc R . . C4 C 0.80051(12) 0.98532(17) 1.0368(2) 0.044(2) Uani 1 1 d G . . H4A H 0.8191 1.0111 1.0184 0.052 Uiso 1 1 calc R . . C5 C 0.80905(10) 0.92749(19) 1.0431(3) 0.049(2) Uani 1 1 d G . . H5A H 0.8334 0.9137 1.0289 0.059 Uiso 1 1 calc R . . C6 C 0.78189(13) 0.88983(13) 1.0701(3) 0.046(2) Uani 1 1 d G . . H6A H 0.7877 0.8503 1.0744 0.055 Uiso 1 1 calc R . . C7 C 0.73146(13) 0.79387(15) 1.1316(3) 0.0329(17) Uani 1 1 d G . . C8 C 0.75540(14) 0.78621(18) 1.1924(2) 0.051(2) Uani 1 1 d G . . H8A H 0.7592 0.8165 1.2264 0.061 Uiso 1 1 calc R . . C9 C 0.77384(13) 0.7342(2) 1.2035(2) 0.050(2) Uani 1 1 d G . . H9A H 0.7902 0.7290 1.2451 0.060 Uiso 1 1 calc R . . C10 C 0.76834(13) 0.68985(16) 1.1538(3) 0.048(2) Uani 1 1 d G . . H10A H 0.7809 0.6543 1.1614 0.057 Uiso 1 1 calc R . . C11 C 0.74439(14) 0.69750(16) 1.0930(3) 0.049(2) Uani 1 1 d G . . H11A H 0.7406 0.6672 1.0590 0.058 Uiso 1 1 calc R . . C12 C 0.72595(12) 0.74951(19) 1.0819(2) 0.044(2) Uani 1 1 d G . . H12A H 0.7096 0.7547 1.0403 0.052 Uiso 1 1 calc R . . C13 C 0.60827(14) 0.72437(19) 1.0148(2) 0.0368(18) Uani 1 1 d G . . C14 C 0.63733(14) 0.6858(2) 1.0322(2) 0.050(2) Uani 1 1 d G . . H14A H 0.6466 0.6828 1.0813 0.060 Uiso 1 1 calc R . . C15 C 0.65283(13) 0.6517(2) 0.9778(3) 0.059(2) Uani 1 1 d G . . H15A H 0.6727 0.6254 0.9898 0.071 Uiso 1 1 calc R . . C16 C 0.63927(15) 0.6561(2) 0.9060(2) 0.063(3) Uani 1 1 d G . . H16A H 0.6499 0.6328 0.8689 0.075 Uiso 1 1 calc R . . C17 C 0.61021(15) 0.6946(2) 0.88860(19) 0.048(2) Uani 1 1 d G . . H17A H 0.6009 0.6976 0.8395 0.058 Uiso 1 1 calc R . . C18 C 0.59471(12) 0.72877(19) 0.9430(3) 0.0420(19) Uani 1 1 d G . . H18A H 0.5748 0.7551 0.9310 0.050 Uiso 1 1 calc R . . C19 C 0.54410(12) 0.72443(19) 1.1104(2) 0.0395(18) Uani 1 1 d G . . C20 C 0.55042(11) 0.66969(19) 1.1376(3) 0.045(2) Uani 1 1 d G . . H20A H 0.5757 0.6548 1.1405 0.054 Uiso 1 1 calc R . . C21 C 0.51971(15) 0.63676(16) 1.1605(3) 0.051(2) Uani 1 1 d G . . H21A H 0.5240 0.5993 1.1791 0.062 Uiso 1 1 calc R . . C22 C 0.48268(13) 0.6586(2) 1.1563(3) 0.059(2) Uani 1 1 d G . . H22A H 0.4617 0.6360 1.1720 0.070 Uiso 1 1 calc R . . C23 C 0.47636(11) 0.7133(2) 1.1291(3) 0.057(2) Uani 1 1 d G . . H23A H 0.4511 0.7282 1.1262 0.068 Uiso 1 1 calc R . . C24 C 0.50708(15) 0.74624(17) 1.1061(2) 0.054(2) Uani 1 1 d G . . H24A H 0.5028 0.7836 1.0876 0.064 Uiso 1 1 calc R . . C25 C 0.53329(12) 1.0001(2) 1.1460(3) 0.0338(17) Uani 1 1 d GU . . C26 C 0.50173(16) 0.9785(2) 1.1825(2) 0.057(2) Uani 1 1 d G . . H26A H 0.5053 0.9543 1.2238 0.068 Uiso 1 1 calc R . . C27 C 0.46488(13) 0.9923(2) 1.1584(3) 0.073(3) Uani 1 1 d G . . H27A H 0.4433 0.9776 1.1832 0.087 Uiso 1 1 calc R . . C28 C 0.45960(13) 1.0277(2) 1.0978(3) 0.063(3) Uani 1 1 d G . . H28A H 0.4344 1.0371 1.0814 0.076 Uiso 1 1 calc R . . C29 C 0.49116(18) 1.0492(2) 1.0614(2) 0.060(2) Uani 1 1 d G . . H29A H 0.4876 1.0734 1.0201 0.073 Uiso 1 1 calc R . . C30 C 0.52801(14) 1.0354(2) 1.0855(3) 0.052(2) Uani 1 1 d G . . H30A H 0.5496 1.0502 1.0606 0.063 Uiso 1 1 calc R . . C31 C 0.59719(16) 1.03978(18) 1.2350(3) 0.044(2) Uani 1 1 d G . . C32 C 0.59970(17) 1.0946(2) 1.2061(2) 0.069(3) Uani 1 1 d GU . . H32A H 0.5929 1.1013 1.1562 0.083 Uiso 1 1 calc R . . C33 C 0.61209(18) 1.13958(17) 1.2502(3) 0.076(3) Uani 1 1 d GU . . H33A H 0.6138 1.1770 1.2304 0.091 Uiso 1 1 calc R . . C34 C 0.62198(16) 1.1298(2) 1.3232(3) 0.066(3) Uani 1 1 d G . . H34A H 0.6305 1.1605 1.3533 0.079 Uiso 1 1 calc R . . C35 C 0.61947(16) 1.0750(3) 1.3521(2) 0.061(2) Uani 1 1 d G . . H35A H 0.6262 1.0682 1.4020 0.073 Uiso 1 1 calc R . . C36 C 0.60708(16) 1.02996(18) 1.3080(3) 0.052(2) Uani 1 1 d G . . H36A H 0.6054 0.9925 1.3277 0.062 Uiso 1 1 calc R . . Al' Al 0.37087(6) 0.62265(8) 0.88849(11) 0.0323(5) Uani 1 1 d . . . P1' P 0.33635(5) 0.73525(8) 0.93394(10) 0.0311(4) Uani 1 1 d . . . P2' P 0.45700(5) 0.63263(7) 0.89556(10) 0.0309(4) Uani 1 1 d . . . P3' P 0.32514(6) 0.51763(8) 0.84874(10) 0.0355(5) Uani 1 1 d . . . S1' S 0.32202(5) 0.65821(7) 0.97255(10) 0.0382(5) Uani 1 1 d . . . S2' S 0.36914(5) 0.72094(7) 0.84583(9) 0.0320(4) Uani 1 1 d . . . S3' S 0.42075(5) 0.63984(7) 0.98002(9) 0.0338(4) Uani 1 1 d . . . S4' S 0.42490(5) 0.60406(8) 0.81017(10) 0.0357(4) Uani 1 1 d . . . S5' S 0.36157(6) 0.52704(8) 0.93456(10) 0.0420(5) Uani 1 1 d . . . S6' S 0.32807(5) 0.59037(7) 0.79104(10) 0.0367(5) Uani 1 1 d . . . C1' C 0.29553(12) 0.77880(18) 0.9073(2) 0.0352(17) Uani 1 1 d G . . C2' C 0.25856(14) 0.75666(17) 0.9055(2) 0.048(2) Uani 1 1 d G . . H2'A H 0.2540 0.7188 0.9221 0.057 Uiso 1 1 calc R . . C3' C 0.22828(11) 0.7899(2) 0.8792(3) 0.060(2) Uani 1 1 d G . . H3'A H 0.2030 0.7747 0.8779 0.072 Uiso 1 1 calc R . . C4' C 0.23498(13) 0.8452(2) 0.8549(3) 0.061(3) Uani 1 1 d G . . H4'A H 0.2143 0.8679 0.8369 0.073 Uiso 1 1 calc R . . C5' C 0.27195(16) 0.86733(16) 0.8567(2) 0.056(2) Uani 1 1 d G . . H5'A H 0.2765 0.9051 0.8401 0.067 Uiso 1 1 calc R . . C6' C 0.30223(11) 0.83414(19) 0.8830(3) 0.046(2) Uani 1 1 d G . . H6'A H 0.3275 0.8493 0.8843 0.055 Uiso 1 1 calc R . . C7' C 0.36162(13) 0.77745(18) 1.0024(2) 0.0331(17) Uani 1 1 d G . . C8' C 0.34983(12) 0.77428(18) 1.0747(3) 0.0407(19) Uani 1 1 d G . . H8'A H 0.3289 0.7504 1.0872 0.049 Uiso 1 1 calc R . . C9' C 0.36863(15) 0.8061(2) 1.12862(19) 0.049(2) Uani 1 1 d G . . H9'A H 0.3606 0.8039 1.1780 0.059 Uiso 1 1 calc R . . C10' C 0.39923(15) 0.8410(2) 1.1103(2) 0.056(2) Uani 1 1 d G . . H10B H 0.4121 0.8627 1.1472 0.067 Uiso 1 1 calc R . . C11' C 0.41103(12) 0.84418(19) 1.0380(3) 0.050(2) Uani 1 1 d G . . H11B H 0.4319 0.8681 1.0255 0.060 Uiso 1 1 calc R . . C12' C 0.39222(14) 0.8124(2) 0.98409(19) 0.044(2) Uani 1 1 d G . . H12B H 0.4003 0.8146 0.9347 0.053 Uiso 1 1 calc R . . C13' C 0.47971(13) 0.70003(15) 0.8756(3) 0.0349(18) Uani 1 1 d G . . C14' C 0.47307(12) 0.7477(2) 0.9190(2) 0.0422(19) Uani 1 1 d G . . H14B H 0.4562 0.7451 0.9592 0.051 Uiso 1 1 calc R . . C15' C 0.49105(15) 0.79923(16) 0.9034(3) 0.048(2) Uani 1 1 d G . . H15B H 0.4865 0.8318 0.9330 0.058 Uiso 1 1 calc R . . C16' C 0.51566(14) 0.80303(17) 0.8445(3) 0.054(2) Uani 1 1 d G . . H16B H 0.5279 0.8382 0.8338 0.065 Uiso 1 1 calc R . . C17' C 0.52230(13) 0.7553(2) 0.8011(2) 0.054(2) Uani 1 1 d G . . H17B H 0.5391 0.7579 0.7608 0.064 Uiso 1 1 calc R . . C18' C 0.50432(14) 0.70383(18) 0.8167(2) 0.043(2) Uani 1 1 d G . . H18B H 0.5089 0.6712 0.7870 0.052 Uiso 1 1 calc R . . C19' C 0.49611(11) 0.58610(17) 0.9163(2) 0.0310(17) Uani 1 1 d G . . C20' C 0.52651(13) 0.60652(14) 0.9589(2) 0.0416(19) Uani 1 1 d G . . H20B H 0.5270 0.6454 0.9738 0.050 Uiso 1 1 calc R . . C21' C 0.55617(11) 0.57003(19) 0.9798(2) 0.050(2) Uani 1 1 d G . . H21B H 0.5769 0.5840 1.0089 0.060 Uiso 1 1 calc R . . C22' C 0.55543(11) 0.51311(18) 0.9580(3) 0.047(2) Uani 1 1 d G . . H22B H 0.5757 0.4882 0.9723 0.056 Uiso 1 1 calc R . . C23' C 0.52503(14) 0.49269(14) 0.9154(3) 0.051(2) Uani 1 1 d G . . H23B H 0.5245 0.4538 0.9005 0.061 Uiso 1 1 calc R . . C24' C 0.49537(11) 0.52918(18) 0.8946(2) 0.0418(19) Uani 1 1 d G . . H24B H 0.4746 0.5152 0.8654 0.050 Uiso 1 1 calc R . . C25' C 0.33881(15) 0.45541(16) 0.7969(3) 0.0383(18) Uani 1 1 d G . . C26' C 0.37315(14) 0.45747(18) 0.7594(3) 0.077(3) Uani 1 1 d G . . H26B H 0.3877 0.4917 0.7589 0.092 Uiso 1 1 calc R . . C27' C 0.38616(13) 0.4094(2) 0.7227(3) 0.082(3) Uani 1 1 d G . . H27B H 0.4096 0.4108 0.6971 0.098 Uiso 1 1 calc R . . C28' C 0.36484(16) 0.35920(18) 0.7235(3) 0.056(2) Uani 1 1 d G . . H28B H 0.3737 0.3263 0.6984 0.067 Uiso 1 1 calc R . . C29' C 0.33049(15) 0.35714(16) 0.7609(3) 0.054(2) Uani 1 1 d G . . H29B H 0.3159 0.3229 0.7615 0.065 Uiso 1 1 calc R . . C30' C 0.31748(12) 0.4052(2) 0.7977(3) 0.051(2) Uani 1 1 d G . . H30B H 0.2940 0.4038 0.8233 0.061 Uiso 1 1 calc R . . C31' C 0.27721(11) 0.5025(2) 0.8787(3) 0.0383(19) Uani 1 1 d G . . C32' C 0.27226(13) 0.46637(19) 0.9382(2) 0.045(2) Uani 1 1 d G . . H32B H 0.2940 0.4518 0.9641 0.054 Uiso 1 1 calc R . . C33' C 0.23555(16) 0.45159(18) 0.9598(2) 0.051(2) Uani 1 1 d G . . H33B H 0.2322 0.4269 1.0005 0.061 Uiso 1 1 calc R . . C34' C 0.20379(12) 0.4730(2) 0.9219(3) 0.062(2) Uani 1 1 d G . . H34B H 0.1787 0.4629 0.9367 0.074 Uiso 1 1 calc R . . C35' C 0.20874(12) 0.5091(2) 0.8624(3) 0.069(3) Uani 1 1 d G . . H35B H 0.1870 0.5237 0.8365 0.083 Uiso 1 1 calc R . . C36' C 0.24545(15) 0.52389(19) 0.8408(2) 0.053(2) Uani 1 1 d G . . H36B H 0.2488 0.5486 0.8001 0.064 Uiso 1 1 calc R . . Al" Al 0.88144(7) 0.61727(9) 0.86566(11) 0.0386(6) Uani 1 1 d . . . P1" P 0.84071(6) 0.72138(8) 0.92041(10) 0.0391(5) Uani 1 1 d D . . P2" P 0.96720(6) 0.63188(8) 0.87434(11) 0.0414(5) Uani 1 1 d D . . P3" P 0.83877(6) 0.51229(8) 0.81424(10) 0.0382(5) Uani 1 1 d . . . S1" S 0.83453(6) 0.64117(9) 0.95688(11) 0.0515(6) Uani 1 1 d . A . S2" S 0.87226(6) 0.71719(7) 0.82934(9) 0.0380(5) Uani 1 1 d . A . S3" S 0.92996(6) 0.63574(9) 0.95708(10) 0.0464(5) Uani 1 1 d . B . S4" S 0.93581(6) 0.60658(9) 0.78638(10) 0.0443(5) Uani 1 1 d . B . S5" S 0.87591(6) 0.51652(8) 0.89965(11) 0.0509(6) Uani 1 1 d . . . S6" S 0.83758(6) 0.59008(8) 0.76733(10) 0.0424(5) Uani 1 1 d . . . C1" C 0.79236(19) 0.7451(4) 0.9050(6) 0.052(3) Uani 0.538(11) 1 d PGDU A 1 C2" C 0.7634(2) 0.7075(4) 0.8837(6) 0.061(3) Uani 0.538(11) 1 d PGDU A 1 H2"A H 0.7690 0.6682 0.8766 0.073 Uiso 0.538(11) 1 calc PR A 1 C3" C 0.7262(2) 0.7274(5) 0.8730(6) 0.063(3) Uani 0.538(11) 1 d PGU A 1 H3"A H 0.7064 0.7017 0.8585 0.075 Uiso 0.538(11) 1 calc PR A 1 C4" C 0.7180(2) 0.7849(6) 0.8834(6) 0.064(3) Uani 0.538(11) 1 d PGU A 1 H4"A H 0.6925 0.7985 0.8761 0.077 Uiso 0.538(11) 1 calc PR A 1 C5" C 0.7469(3) 0.8225(4) 0.9046(6) 0.060(3) Uani 0.538(11) 1 d PGU A 1 H5"A H 0.7413 0.8618 0.9118 0.072 Uiso 0.538(11) 1 calc PR A 1 C6" C 0.7841(2) 0.8026(4) 0.9154(6) 0.056(3) Uani 0.538(11) 1 d PGDU A 1 H6"A H 0.8039 0.8283 0.9299 0.067 Uiso 0.538(11) 1 calc PR A 1 C1C C 0.7970(2) 0.7616(4) 0.9034(8) 0.049(3) Uiso 0.462(11) 1 d PGDU A 2 C2C C 0.7627(3) 0.7319(4) 0.8957(9) 0.060(4) Uiso 0.462(11) 1 d PGDU A 2 H2CA H 0.7625 0.6914 0.8985 0.072 Uiso 0.462(11) 1 calc PR A 2 C3C C 0.7286(2) 0.7616(6) 0.8839(8) 0.062(4) Uiso 0.462(11) 1 d PGU A 2 H3CA H 0.7051 0.7414 0.8786 0.075 Uiso 0.462(11) 1 calc PR A 2 C4C C 0.7289(3) 0.8209(6) 0.8797(7) 0.058(3) Uiso 0.462(11) 1 d PGU A 2 H4CA H 0.7057 0.8412 0.8716 0.070 Uiso 0.462(11) 1 calc PR A 2 C5C C 0.7633(4) 0.8506(4) 0.8874(7) 0.069(4) Uiso 0.462(11) 1 d PGU A 2 H5CA H 0.7635 0.8911 0.8845 0.083 Uiso 0.462(11) 1 calc PR A 2 C6C C 0.7973(3) 0.8209(4) 0.8992(7) 0.059(4) Uiso 0.462(11) 1 d PGDU A 2 H6CA H 0.8208 0.8411 0.9045 0.071 Uiso 0.462(11) 1 calc PR A 2 C7" C 0.86366(14) 0.76658(19) 0.9889(2) 0.0380(18) Uani 1 1 d G A . C8" C 0.85009(12) 0.76491(19) 1.0601(3) 0.042(2) Uani 1 1 d G . . H8"A H 0.8293 0.7405 1.0718 0.051 Uiso 1 1 calc R A . C9" C 0.86694(16) 0.7989(2) 1.11411(19) 0.052(2) Uani 1 1 d G A . H9"A H 0.8577 0.7978 1.1627 0.062 Uiso 1 1 calc R . . C10" C 0.89737(16) 0.8346(2) 1.0970(3) 0.061(3) Uani 1 1 d G . . H10C H 0.9089 0.8578 1.1339 0.073 Uiso 1 1 calc R A . C11" C 0.91094(13) 0.8362(2) 1.0258(3) 0.061(3) Uani 1 1 d G A . H11C H 0.9317 0.8606 1.0141 0.073 Uiso 1 1 calc R . . C12" C 0.89409(14) 0.8023(2) 0.9718(2) 0.048(2) Uani 1 1 d G . . H12C H 0.9034 0.8034 0.9232 0.058 Uiso 1 1 calc R A . C13" C 0.99014(14) 0.70000(17) 0.8590(3) 0.042(2) Uani 1 1 d G B . C14" C 0.98301(13) 0.7457(2) 0.9055(2) 0.054(2) Uani 1 1 d G . . H14C H 0.9665 0.7409 0.9459 0.064 Uiso 1 1 calc R B . C15" C 1.00003(16) 0.79839(19) 0.8929(3) 0.065(3) Uani 1 1 d G B . H15C H 0.9952 0.8296 0.9247 0.078 Uiso 1 1 calc R . . C16" C 1.02418(15) 0.80543(18) 0.8337(3) 0.057(2) Uani 1 1 d G . . H16C H 1.0358 0.8415 0.8251 0.068 Uiso 1 1 calc R B . C17" C 1.03130(13) 0.7598(2) 0.7872(2) 0.062(3) Uani 1 1 d G B . H17C H 1.0478 0.7646 0.7468 0.075 Uiso 1 1 calc R . . C18" C 1.01428(15) 0.7070(2) 0.7998(3) 0.055(2) Uani 1 1 d G . . H18C H 1.0191 0.6758 0.7680 0.066 Uiso 1 1 calc R B . C19" C 1.0033(3) 0.5822(3) 0.9009(7) 0.052(3) Uani 0.50 1 d PGDU B 1 C20" C 1.0401(3) 0.6011(3) 0.9181(8) 0.051(3) Uani 0.50 1 d PGDU B 1 H20C H 1.0471 0.6397 0.9090 0.061 Uiso 0.50 1 calc PR B 1 C21" C 1.0668(2) 0.5636(5) 0.9488(7) 0.061(3) Uani 0.50 1 d PGU B 1 H21C H 1.0919 0.5765 0.9606 0.074 Uiso 0.50 1 calc PR B 1 C22" C 1.0566(3) 0.5072(4) 0.9623(6) 0.051(3) Uani 0.50 1 d PGU B 1 H22C H 1.0748 0.4815 0.9833 0.062 Uiso 0.50 1 calc PR B 1 C23" C 1.0198(3) 0.4883(3) 0.9450(6) 0.055(3) Uani 0.50 1 d PGU B 1 H23C H 1.0128 0.4497 0.9542 0.066 Uiso 0.50 1 calc PR B 1 C24" C 0.9931(2) 0.5258(4) 0.9143(6) 0.053(3) Uani 0.50 1 d PGDU B 1 H24C H 0.9680 0.5129 0.9025 0.064 Uiso 0.50 1 calc PR B 1 C19C C 1.0075(3) 0.5833(4) 0.8915(7) 0.050(3) Uani 0.50 1 d PGDU B 2 C20C C 1.0385(3) 0.6025(4) 0.9336(8) 0.052(3) Uani 0.50 1 d PGDU B 2 H20E H 1.0391 0.6409 0.9508 0.062 Uiso 0.50 1 calc PR B 2 C21C C 1.0686(3) 0.5657(5) 0.9506(7) 0.062(3) Uani 0.50 1 d PGU B 2 H21E H 1.0897 0.5788 0.9793 0.074 Uiso 0.50 1 calc PR B 2 C22C C 1.0677(3) 0.5096(4) 0.9255(6) 0.062(3) Uani 0.50 1 d PGU B 2 H22E H 1.0883 0.4844 0.9371 0.074 Uiso 0.50 1 calc PR B 2 C23C C 1.0368(3) 0.4904(3) 0.8834(6) 0.062(3) Uani 0.50 1 d PGU B 2 H23E H 1.0362 0.4521 0.8663 0.074 Uiso 0.50 1 calc PR B 2 C24C C 1.0067(2) 0.5273(4) 0.8664(6) 0.057(3) Uani 0.50 1 d PGDU B 2 H24E H 0.9855 0.5141 0.8377 0.068 Uiso 0.50 1 calc PR B 2 C25" C 0.85286(16) 0.45683(18) 0.7508(2) 0.0382(18) Uani 1 1 d G . . C26" C 0.85688(18) 0.4013(2) 0.7767(2) 0.071(3) Uani 1 1 d G . . H26C H 0.8530 0.3932 0.8271 0.085 Uiso 1 1 calc R . . C27" C 0.86656(18) 0.35748(16) 0.7290(3) 0.073(3) Uani 1 1 d G . . H27C H 0.8693 0.3195 0.7468 0.087 Uiso 1 1 calc R . . C28" C 0.87222(16) 0.36924(19) 0.6553(3) 0.050(2) Uani 1 1 d G . . H28C H 0.8788 0.3393 0.6227 0.060 Uiso 1 1 calc R . . C29" C 0.86820(15) 0.4248(2) 0.6294(2) 0.055(2) Uani 1 1 d G . . H29C H 0.8721 0.4328 0.5790 0.066 Uiso 1 1 calc R . . C30" C 0.85853(15) 0.46858(16) 0.6771(3) 0.047(2) Uani 1 1 d G . . H30C H 0.8558 0.5066 0.6593 0.056 Uiso 1 1 calc R . . C31" C 0.79181(12) 0.4912(2) 0.8425(3) 0.0407(19) Uani 1 1 d GU . . C32" C 0.78781(14) 0.4598(2) 0.9066(3) 0.046(2) Uani 1 1 d G . . H32C H 0.8098 0.4505 0.9357 0.055 Uiso 1 1 calc R . . C33" C 0.75170(17) 0.44190(19) 0.9281(2) 0.056(2) Uani 1 1 d G . . H33C H 0.7490 0.4204 0.9718 0.068 Uiso 1 1 calc R . . C34" C 0.71958(13) 0.4554(2) 0.8855(3) 0.062(3) Uani 1 1 d G . . H34C H 0.6949 0.4432 0.9001 0.074 Uiso 1 1 calc R . . C35" C 0.72358(13) 0.4868(2) 0.8214(3) 0.079(3) Uani 1 1 d G . . H35C H 0.7016 0.4961 0.7923 0.095 Uiso 1 1 calc R . . C36" C 0.75969(17) 0.5047(2) 0.7999(2) 0.058(2) Uani 1 1 d G . . H36C H 0.7624 0.5262 0.7561 0.070 Uiso 1 1 calc R . . Al* Al 0.86966(6) 0.38137(9) 0.37710(11) 0.0366(5) Uani 1 1 d . . . P1* P 0.90598(6) 0.27069(8) 0.42797(10) 0.0366(5) Uani 1 1 d D . . P2* P 0.78336(5) 0.37270(8) 0.37813(10) 0.0338(4) Uani 1 1 d . . . P3* P 0.91406(6) 0.48582(8) 0.33345(12) 0.0487(6) Uani 1 1 d D . . S1* S 0.91793(6) 0.34934(8) 0.46604(10) 0.0442(5) Uani 1 1 d . C . S2* S 0.87287(5) 0.28187(7) 0.33804(9) 0.0370(5) Uani 1 1 d . C . S3* S 0.81924(5) 0.36737(8) 0.46531(10) 0.0368(4) Uani 1 1 d . . . S4* S 0.81621(5) 0.39798(8) 0.29420(10) 0.0406(5) Uani 1 1 d . . . S5* S 0.87870(6) 0.47856(8) 0.41915(11) 0.0486(5) Uani 1 1 d . D . S6* S 0.91335(6) 0.41071(8) 0.28133(10) 0.0441(5) Uani 1 1 d . D . C1* C 0.94790(19) 0.2273(4) 0.4071(5) 0.046(3) Uani 0.603(15) 1 d PGDU C 1 C2* C 0.9845(2) 0.2507(4) 0.4086(6) 0.052(3) Uani 0.603(15) 1 d PGDU C 1 H2*A H 0.9883 0.2890 0.4245 0.062 Uiso 0.603(15) 1 calc PR C 1 C3* C 1.01563(17) 0.2182(5) 0.3867(5) 0.050(3) Uani 0.603(15) 1 d PGU C 1 H3*A H 1.0406 0.2342 0.3877 0.060 Uiso 0.603(15) 1 calc PR C 1 C4* C 1.0101(2) 0.1622(4) 0.3635(6) 0.055(3) Uani 0.603(15) 1 d PGU C 1 H4*A H 1.0314 0.1399 0.3485 0.066 Uiso 0.603(15) 1 calc PR C 1 C5* C 0.9735(3) 0.1387(3) 0.3620(7) 0.054(3) Uani 0.603(15) 1 d PGU C 1 H5*A H 0.9698 0.1005 0.3461 0.065 Uiso 0.603(15) 1 calc PR C 1 C6* C 0.9424(2) 0.1713(3) 0.3838(6) 0.049(3) Uani 0.603(15) 1 d PGDU C 1 H6*A H 0.9174 0.1552 0.3828 0.059 Uiso 0.603(15) 1 calc PR C 1 C1D C 0.9504(2) 0.2369(5) 0.4089(9) 0.045(4) Uiso 0.397(15) 1 d PGDU C 2 C2D C 0.9829(3) 0.2683(5) 0.3916(9) 0.052(4) Uiso 0.397(15) 1 d PGDU C 2 H2DA H 0.9815 0.3087 0.3883 0.062 Uiso 0.397(15) 1 calc PR C 2 C3D C 1.0174(3) 0.2404(6) 0.3791(8) 0.055(4) Uiso 0.397(15) 1 d PGU C 2 H3DA H 1.0396 0.2619 0.3673 0.066 Uiso 0.397(15) 1 calc PR C 2 C4D C 1.0194(3) 0.1812(7) 0.3840(8) 0.053(4) Uiso 0.397(15) 1 d PGU C 2 H4DA H 1.0430 0.1622 0.3755 0.063 Uiso 0.397(15) 1 calc PR C 2 C5D C 0.9870(4) 0.1499(5) 0.4013(10) 0.055(4) Uiso 0.397(15) 1 d PGU C 2 H5DA H 0.9884 0.1094 0.4046 0.066 Uiso 0.397(15) 1 calc PR C 2 C6D C 0.9525(3) 0.1777(5) 0.4137(9) 0.048(4) Uiso 0.397(15) 1 d PGDU C 2 H6DA H 0.9303 0.1562 0.4256 0.058 Uiso 0.397(15) 1 calc PR C 2 C7* C 0.88227(13) 0.22761(18) 0.4958(2) 0.0338(17) Uani 1 1 d G C . C8* C 0.89621(11) 0.22875(18) 0.5676(2) 0.0377(18) Uani 1 1 d G . . H8*A H 0.9179 0.2515 0.5800 0.045 Uiso 1 1 calc R C . C9* C 0.87842(14) 0.1965(2) 0.62123(19) 0.045(2) Uani 1 1 d GU C . H9*A H 0.8879 0.1973 0.6703 0.054 Uiso 1 1 calc R . . C10* C 0.84669(14) 0.1632(2) 0.6031(2) 0.055(2) Uani 1 1 d G . . H10D H 0.8345 0.1412 0.6398 0.066 Uiso 1 1 calc R C . C11* C 0.83275(12) 0.16203(19) 0.5314(3) 0.055(2) Uani 1 1 d G C . H11D H 0.8111 0.1392 0.5190 0.066 Uiso 1 1 calc R . . C12* C 0.85054(14) 0.1942(2) 0.4777(2) 0.0422(19) Uani 1 1 d G . . H12D H 0.8410 0.1935 0.4287 0.051 Uiso 1 1 calc R C . C13* C 0.76123(13) 0.30465(15) 0.3595(2) 0.0306(17) Uani 1 1 d G . . C14* C 0.76879(12) 0.25813(19) 0.4049(2) 0.0410(19) Uani 1 1 d G . . H14D H 0.7854 0.2624 0.4463 0.049 Uiso 1 1 calc R . . C15* C 0.75211(14) 0.20544(16) 0.3895(2) 0.049(2) Uani 1 1 d G . . H15D H 0.7573 0.1736 0.4205 0.059 Uiso 1 1 calc R . . C16* C 0.72788(13) 0.19926(15) 0.3288(3) 0.044(2) Uani 1 1 d G . . H16D H 0.7165 0.1632 0.3184 0.052 Uiso 1 1 calc R . . C17* C 0.72033(12) 0.2458(2) 0.2835(2) 0.046(2) Uani 1 1 d G . . H17D H 0.7038 0.2416 0.2420 0.055 Uiso 1 1 calc R . . C18* C 0.73700(14) 0.29847(16) 0.2988(2) 0.047(2) Uani 1 1 d G . . H18D H 0.7318 0.3303 0.2679 0.056 Uiso 1 1 calc R . . C19* C 0.74380(12) 0.42097(18) 0.3925(3) 0.0392(19) Uani 1 1 d G . . C20* C 0.71298(15) 0.40208(16) 0.4333(3) 0.051(2) Uani 1 1 d G . . H20D H 0.7128 0.3643 0.4523 0.061 Uiso 1 1 calc R . . C21* C 0.68234(12) 0.4385(2) 0.4463(3) 0.068(3) Uani 1 1 d G . . H21D H 0.6613 0.4256 0.4742 0.082 Uiso 1 1 calc R . . C22* C 0.68253(14) 0.4938(2) 0.4184(3) 0.070(3) Uani 1 1 d G . . H22D H 0.6616 0.5186 0.4273 0.084 Uiso 1 1 calc R . . C23* C 0.71335(17) 0.51266(16) 0.3776(3) 0.068(3) Uani 1 1 d G . . H23D H 0.7135 0.5504 0.3586 0.082 Uiso 1 1 calc R . . C24* C 0.74398(14) 0.4763(2) 0.3647(3) 0.054(2) Uani 1 1 d G . . H24D H 0.7650 0.4892 0.3368 0.064 Uiso 1 1 calc R . . C25* C 0.9034(3) 0.5503(3) 0.2853(5) 0.061(3) Uani 0.50 1 d PGDU D 1 C26* C 0.9252(3) 0.5996(4) 0.2937(5) 0.063(3) Uani 0.50 1 d PGDU D 1 H26D H 0.9468 0.5998 0.3262 0.076 Uiso 0.50 1 calc PR D 1 C27* C 0.9155(3) 0.6486(3) 0.2547(6) 0.068(3) Uani 0.50 1 d PGU D 1 H27D H 0.9304 0.6823 0.2605 0.081 Uiso 0.50 1 calc PR D 1 C28* C 0.8840(4) 0.6484(3) 0.2072(6) 0.069(3) Uani 0.50 1 d PGU D 1 H28D H 0.8773 0.6819 0.1806 0.082 Uiso 0.50 1 calc PR D 1 C29* C 0.8621(3) 0.5990(4) 0.1988(5) 0.080(3) Uani 0.50 1 d PGU D 1 H29D H 0.8406 0.5988 0.1664 0.096 Uiso 0.50 1 calc PR D 1 C30* C 0.8719(3) 0.5500(4) 0.2378(6) 0.076(3) Uani 0.50 1 d PGDU D 1 H30D H 0.8569 0.5163 0.2321 0.091 Uiso 0.50 1 calc PR D 1 C25D C 0.8937(4) 0.5395(4) 0.2693(4) 0.060(3) Uani 0.50 1 d PGDU D 2 C26D C 0.8753(4) 0.5868(4) 0.2984(4) 0.073(3) Uani 0.50 1 d PGDU D 2 H26E H 0.8698 0.5881 0.3492 0.088 Uiso 0.50 1 calc PR D 2 C27D C 0.8648(3) 0.6321(4) 0.2531(6) 0.076(3) Uani 0.50 1 d PGU D 2 H27E H 0.8522 0.6645 0.2730 0.092 Uiso 0.50 1 calc PR D 2 C28D C 0.8728(4) 0.6302(4) 0.1788(6) 0.074(3) Uani 0.50 1 d PGU D 2 H28E H 0.8656 0.6612 0.1479 0.089 Uiso 0.50 1 calc PR D 2 C29D C 0.8912(4) 0.5829(4) 0.1497(4) 0.067(3) Uani 0.50 1 d PGU D 2 H29E H 0.8967 0.5816 0.0990 0.081 Uiso 0.50 1 calc PR D 2 C30D C 0.9017(3) 0.5375(4) 0.1950(5) 0.064(3) Uani 0.50 1 d PGDU D 2 H30E H 0.9143 0.5052 0.1751 0.077 Uiso 0.50 1 calc PR D 2 C31* C 0.9616(2) 0.5008(7) 0.3725(7) 0.053(3) Uani 0.50 1 d PGDU D 1 C32* C 0.9651(3) 0.5360(8) 0.4336(8) 0.062(3) Uani 0.50 1 d PGDU D 1 H32* H 0.9428 0.5485 0.4581 0.074 Uiso 0.50 1 calc PR D 1 C33* C 1.0012(3) 0.5528(7) 0.4588(6) 0.060(3) Uani 0.50 1 d PGU D 1 H33* H 1.0036 0.5769 0.5005 0.072 Uiso 0.50 1 calc PR D 1 C34* C 1.0338(2) 0.5345(6) 0.4228(6) 0.058(3) Uani 0.50 1 d PGU D 1 H34* H 1.0584 0.5460 0.4400 0.070 Uiso 0.50 1 calc PR D 1 C35* C 1.0303(2) 0.4993(5) 0.3617(6) 0.060(3) Uani 0.50 1 d PGU D 1 H35* H 1.0526 0.4868 0.3372 0.072 Uiso 0.50 1 calc PR D 1 C36* C 0.9942(3) 0.4825(5) 0.3365(6) 0.055(3) Uani 0.50 1 d PGDU D 1 H36* H 0.9918 0.4584 0.2948 0.066 Uiso 0.50 1 calc PR D 1 C31D C 0.9617(2) 0.5091(7) 0.3553(7) 0.051(3) Uani 0.50 1 d PGDU D 2 C32D C 0.9683(3) 0.5417(8) 0.4180(7) 0.060(3) Uani 0.50 1 d PGDU D 2 H32E H 0.9476 0.5508 0.4492 0.072 Uiso 0.50 1 calc PR D 2 C33D C 1.0050(3) 0.5609(7) 0.4350(6) 0.062(4) Uani 0.50 1 d PGU D 2 H33E H 1.0095 0.5831 0.4778 0.074 Uiso 0.50 1 calc PR D 2 C34D C 1.0353(2) 0.5476(6) 0.3893(7) 0.058(3) Uani 0.50 1 d PGU D 2 H34E H 1.0604 0.5607 0.4009 0.069 Uiso 0.50 1 calc PR D 2 C35D C 1.0287(2) 0.5150(5) 0.3266(6) 0.062(3) Uani 0.50 1 d PGU D 2 H35E H 1.0494 0.5059 0.2954 0.074 Uiso 0.50 1 calc PR D 2 C36D C 0.9919(3) 0.4958(6) 0.3096(6) 0.064(4) Uani 0.50 1 d PGDU D 2 H36E H 0.9875 0.4736 0.2668 0.076 Uiso 0.50 1 calc PR D 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 Al 0.0406(13) 0.0235(11) 0.0320(12) -0.0001(9) 0.0021(10) 0.0035(10) P1 0.0400(11) 0.0257(10) 0.0329(11) -0.0021(8) 0.0039(9) 0.0015(8) P2 0.0390(11) 0.0289(10) 0.0337(11) -0.0033(8) -0.0087(9) 0.0011(9) P3 0.0461(12) 0.0236(10) 0.0334(11) 0.0011(8) 0.0051(9) 0.0021(9) S1 0.0435(11) 0.0331(10) 0.0331(10) -0.0059(8) 0.0029(9) -0.0023(8) S2 0.0431(11) 0.0354(10) 0.0314(10) -0.0037(8) -0.0003(8) 0.0040(9) S3 0.0464(11) 0.0230(9) 0.0334(10) 0.0000(8) -0.0066(9) -0.0006(8) S4 0.0487(12) 0.0323(11) 0.0451(12) 0.0011(9) -0.0109(9) 0.0057(9) S5 0.0481(12) 0.0247(10) 0.0388(11) 0.0060(8) 0.0071(9) 0.0044(8) S6 0.0598(13) 0.0285(10) 0.0364(11) 0.0048(8) 0.0136(10) 0.0070(9) C1 0.049(5) 0.025(4) 0.031(4) 0.003(3) 0.007(3) 0.001(3) C2 0.061(5) 0.026(4) 0.042(5) 0.004(3) 0.014(4) 0.002(4) C3 0.065(6) 0.028(4) 0.048(5) 0.008(4) 0.013(4) 0.003(4) C4 0.053(5) 0.031(4) 0.048(5) 0.002(4) 0.007(4) -0.010(4) C5 0.038(5) 0.045(5) 0.064(6) -0.002(4) 0.013(4) 0.003(4) C6 0.049(5) 0.026(4) 0.063(5) 0.007(4) 0.011(4) 0.003(4) C7 0.034(4) 0.028(4) 0.037(4) 0.001(3) 0.003(3) 0.000(3) C8 0.068(6) 0.044(5) 0.042(5) 0.001(4) -0.004(4) 0.010(4) C9 0.053(5) 0.059(6) 0.038(5) 0.002(4) -0.006(4) 0.012(4) C10 0.052(5) 0.033(5) 0.059(5) 0.013(4) 0.009(4) 0.008(4) C11 0.062(6) 0.028(4) 0.056(5) -0.010(4) 0.001(4) 0.003(4) C12 0.062(5) 0.026(4) 0.043(5) 0.001(4) -0.005(4) 0.007(4) C13 0.035(4) 0.034(4) 0.041(5) 0.000(4) -0.007(4) 0.000(3) C14 0.062(6) 0.047(5) 0.041(5) -0.007(4) -0.005(4) 0.011(4) C15 0.062(6) 0.050(6) 0.065(6) -0.007(5) 0.002(5) 0.022(5) C16 0.064(6) 0.065(6) 0.059(6) -0.024(5) 0.008(5) -0.007(5) C17 0.051(5) 0.061(6) 0.032(5) 0.002(4) -0.006(4) -0.002(4) C18 0.044(5) 0.040(5) 0.042(5) -0.001(4) -0.002(4) 0.005(4) C19 0.050(5) 0.038(5) 0.030(4) -0.006(3) -0.007(4) -0.006(4) C20 0.050(5) 0.037(5) 0.049(5) -0.020(4) 0.005(4) -0.011(4) C21 0.060(6) 0.033(5) 0.061(6) -0.010(4) 0.002(4) -0.014(4) C22 0.051(6) 0.057(6) 0.067(6) -0.021(5) 0.006(5) -0.025(5) C23 0.048(5) 0.061(6) 0.061(6) -0.005(5) 0.001(4) -0.005(5) C24 0.053(5) 0.058(6) 0.049(5) -0.013(4) -0.012(4) -0.003(5) C25 0.043(4) 0.021(3) 0.037(3) -0.005(3) 0.001(3) 0.005(3) C26 0.062(6) 0.053(6) 0.056(6) 0.006(4) 0.011(5) 0.011(5) C27 0.058(7) 0.084(8) 0.077(7) 0.015(6) 0.013(5) 0.010(5) C28 0.077(7) 0.051(6) 0.062(6) -0.008(5) -0.010(5) 0.028(5) C29 0.072(7) 0.046(6) 0.063(6) 0.003(5) 0.002(5) 0.007(5) C30 0.063(6) 0.034(5) 0.060(6) 0.013(4) -0.004(5) -0.003(4) C31 0.055(5) 0.027(4) 0.049(5) -0.006(4) 0.012(4) -0.006(4) C32 0.120(7) 0.040(5) 0.046(5) 0.004(4) -0.004(5) -0.021(5) C33 0.118(7) 0.048(5) 0.061(5) 0.003(4) 0.004(5) -0.028(5) C34 0.057(6) 0.059(6) 0.082(7) -0.030(5) 0.010(5) -0.022(5) C35 0.071(6) 0.064(6) 0.049(6) -0.010(5) -0.009(5) -0.002(5) C36 0.064(6) 0.037(5) 0.053(5) -0.006(4) -0.009(5) 0.005(4) Al' 0.0382(13) 0.0229(11) 0.0356(13) 0.0013(9) -0.0037(10) -0.0018(9) P1' 0.0381(11) 0.0272(10) 0.0281(10) 0.0018(8) 0.0015(8) -0.0002(8) P2' 0.0358(11) 0.0247(10) 0.0319(10) 0.0007(8) -0.0054(8) 0.0008(8) P3' 0.0437(12) 0.0221(10) 0.0403(12) 0.0021(8) -0.0102(9) -0.0027(8) S1' 0.0447(12) 0.0289(10) 0.0413(11) 0.0044(8) 0.0077(9) -0.0040(8) S2' 0.0424(11) 0.0235(9) 0.0301(10) 0.0014(7) 0.0027(8) 0.0020(8) S3' 0.0387(11) 0.0302(10) 0.0323(10) 0.0001(8) -0.0044(8) -0.0042(8) S4' 0.0386(11) 0.0341(11) 0.0342(10) -0.0050(8) -0.0081(8) 0.0033(8) S5' 0.0543(13) 0.0270(10) 0.0442(12) 0.0066(8) -0.0169(10) -0.0050(9) S6' 0.0441(11) 0.0254(10) 0.0402(11) 0.0040(8) -0.0109(9) -0.0052(8) C1' 0.033(4) 0.039(4) 0.034(4) 0.003(3) 0.002(3) 0.009(3) C2' 0.052(5) 0.051(5) 0.040(5) 0.006(4) 0.003(4) 0.003(4) C3' 0.045(5) 0.079(7) 0.055(6) 0.004(5) 0.001(4) 0.010(5) C4' 0.055(6) 0.070(7) 0.057(6) -0.006(5) -0.005(5) 0.030(5) C5' 0.067(6) 0.046(5) 0.054(6) -0.002(4) -0.006(5) 0.023(5) C6' 0.051(5) 0.036(4) 0.050(5) -0.003(4) -0.008(4) 0.015(4) C7' 0.042(4) 0.021(4) 0.037(4) 0.001(3) -0.004(4) -0.001(3) C8' 0.044(5) 0.037(5) 0.041(5) -0.001(4) 0.004(4) 0.005(4) C9' 0.067(6) 0.048(5) 0.032(5) -0.003(4) 0.008(4) 0.001(4) C10' 0.078(7) 0.040(5) 0.050(6) -0.014(4) -0.004(5) -0.005(5) C11' 0.054(5) 0.040(5) 0.056(6) -0.013(4) -0.005(4) -0.013(4) C12' 0.056(5) 0.036(5) 0.040(5) 0.003(4) 0.006(4) -0.001(4) C13' 0.037(4) 0.030(4) 0.038(4) 0.003(3) 0.003(3) -0.003(3) C14' 0.046(5) 0.033(4) 0.048(5) 0.005(4) 0.004(4) -0.002(4) C15' 0.063(6) 0.029(4) 0.053(5) 0.001(4) -0.006(4) -0.001(4) C16' 0.066(6) 0.034(5) 0.063(6) 0.011(4) -0.011(5) -0.011(4) C17' 0.068(6) 0.051(6) 0.043(5) 0.023(4) 0.003(4) -0.009(5) C18' 0.054(5) 0.033(4) 0.042(5) -0.001(4) -0.008(4) 0.001(4) C19' 0.024(4) 0.030(4) 0.039(4) 0.011(3) -0.003(3) 0.002(3) C20' 0.045(5) 0.027(4) 0.053(5) 0.003(4) -0.014(4) 0.005(3) C21' 0.039(5) 0.045(5) 0.065(6) -0.001(4) -0.014(4) -0.009(4) C22' 0.043(5) 0.039(5) 0.059(5) 0.000(4) -0.008(4) 0.004(4) C23' 0.048(5) 0.030(4) 0.076(6) 0.001(4) -0.014(5) 0.000(4) C24' 0.038(5) 0.029(4) 0.058(5) -0.001(4) -0.017(4) -0.001(3) C25' 0.048(5) 0.026(4) 0.041(5) 0.003(3) -0.006(4) -0.002(3) C26' 0.098(8) 0.025(5) 0.109(8) -0.015(5) 0.045(7) -0.008(5) C27' 0.101(8) 0.046(6) 0.100(8) 0.002(6) 0.043(7) -0.004(6) C28' 0.070(6) 0.034(5) 0.065(6) -0.011(4) 0.006(5) 0.012(4) C29' 0.088(7) 0.026(4) 0.047(5) -0.001(4) -0.002(5) -0.009(4) C30' 0.075(6) 0.030(4) 0.046(5) 0.001(4) -0.001(4) -0.007(4) C31' 0.051(5) 0.023(4) 0.040(5) -0.010(3) -0.009(4) 0.001(3) C32' 0.056(5) 0.030(4) 0.050(5) 0.005(4) 0.004(4) 0.001(4) C33' 0.073(6) 0.025(4) 0.055(5) 0.011(4) 0.014(5) -0.002(4) C34' 0.058(6) 0.063(6) 0.064(6) -0.002(5) 0.005(5) -0.012(5) C35' 0.052(6) 0.078(7) 0.077(7) 0.017(6) -0.001(5) -0.011(5) C36' 0.053(6) 0.060(6) 0.048(5) 0.007(4) 0.006(4) -0.009(5) Al" 0.0517(15) 0.0319(13) 0.0318(13) 0.0006(10) -0.0081(11) -0.0065(11) P1" 0.0447(12) 0.0434(12) 0.0291(11) -0.0013(9) 0.0020(9) 0.0022(10) P2" 0.0528(13) 0.0341(11) 0.0371(12) 0.0002(9) -0.0099(10) -0.0050(10) P3" 0.0504(13) 0.0295(11) 0.0342(11) 0.0005(9) -0.0095(9) -0.0033(9) S1" 0.0663(15) 0.0488(13) 0.0396(12) -0.0001(10) 0.0088(10) -0.0209(11) S2" 0.0567(13) 0.0294(10) 0.0282(10) -0.0001(8) 0.0054(9) 0.0009(9) S3" 0.0606(14) 0.0453(12) 0.0329(11) 0.0010(9) -0.0110(10) -0.0132(10) S4" 0.0503(13) 0.0482(13) 0.0341(11) -0.0085(9) -0.0089(9) 0.0070(10) S5" 0.0688(15) 0.0370(11) 0.0461(13) 0.0068(9) -0.0254(11) -0.0110(10) S6" 0.0554(13) 0.0302(11) 0.0411(12) 0.0029(9) -0.0130(9) -0.0034(9) C1" 0.054(5) 0.064(6) 0.038(5) 0.003(5) -0.001(5) 0.002(5) C2" 0.056(5) 0.072(6) 0.054(5) 0.000(5) 0.000(5) 0.001(5) C3" 0.062(5) 0.073(6) 0.053(5) -0.001(5) -0.007(5) 0.003(5) C4" 0.066(6) 0.070(6) 0.056(5) 0.011(5) 0.000(5) 0.015(5) C5" 0.060(5) 0.069(5) 0.052(5) 0.005(5) 0.004(5) 0.012(5) C6" 0.055(5) 0.067(6) 0.046(5) 0.002(5) 0.005(5) 0.009(5) C7" 0.043(5) 0.033(4) 0.037(4) 0.005(3) -0.005(4) 0.007(4) C8" 0.056(5) 0.038(4) 0.033(4) -0.003(4) 0.008(4) 0.005(4) C9" 0.071(6) 0.056(6) 0.029(5) -0.004(4) 0.003(4) 0.013(5) C10" 0.078(7) 0.052(6) 0.052(6) -0.014(5) -0.014(5) 0.008(5) C11" 0.081(7) 0.042(5) 0.060(6) -0.011(5) 0.004(5) -0.011(5) C12" 0.063(6) 0.038(5) 0.043(5) 0.005(4) 0.008(4) -0.003(4) C13" 0.049(5) 0.037(5) 0.040(5) 0.007(4) -0.011(4) -0.005(4) C14" 0.053(5) 0.042(5) 0.066(6) 0.005(4) 0.008(4) 0.001(4) C15" 0.059(6) 0.041(5) 0.095(8) -0.011(5) 0.011(5) -0.006(4) C16" 0.057(6) 0.053(6) 0.060(6) 0.014(5) -0.007(5) -0.004(5) C17" 0.067(6) 0.082(7) 0.038(5) 0.013(5) -0.003(4) -0.013(5) C18" 0.077(7) 0.045(5) 0.043(5) 0.007(4) -0.003(5) -0.015(5) C19" 0.055(6) 0.041(5) 0.058(6) 0.008(5) -0.026(5) -0.005(5) C20" 0.057(6) 0.037(5) 0.058(6) 0.010(5) -0.017(5) -0.010(5) C21" 0.065(6) 0.048(6) 0.071(6) 0.009(5) -0.028(5) -0.007(5) C22" 0.056(6) 0.043(5) 0.054(6) 0.015(5) -0.021(5) -0.004(5) C23" 0.062(6) 0.037(5) 0.064(6) 0.011(5) -0.018(5) -0.008(5) C24" 0.058(6) 0.048(5) 0.054(6) 0.009(5) -0.023(5) -0.008(5) C19C 0.054(6) 0.038(5) 0.058(6) 0.016(5) -0.024(5) -0.005(5) C20C 0.057(6) 0.040(5) 0.059(6) 0.015(5) -0.019(5) -0.010(5) C21C 0.066(6) 0.048(6) 0.071(6) 0.008(5) -0.027(5) -0.005(5) C22C 0.064(6) 0.049(6) 0.071(6) 0.021(6) -0.032(5) 0.000(5) C23C 0.067(6) 0.045(6) 0.073(6) 0.008(6) -0.021(6) -0.007(5) C24C 0.058(6) 0.044(5) 0.068(6) 0.008(6) -0.025(5) -0.006(5) C25" 0.047(5) 0.028(4) 0.040(5) -0.001(3) -0.004(4) 0.003(3) C26" 0.144(10) 0.035(5) 0.035(5) 0.004(4) 0.008(5) 0.025(6) C27" 0.129(9) 0.033(5) 0.056(6) 0.011(4) 0.002(6) 0.025(5) C28" 0.058(6) 0.043(5) 0.048(5) -0.006(4) 0.002(4) 0.007(4) C29" 0.046(5) 0.057(6) 0.061(6) -0.006(5) 0.006(4) 0.003(4) C30" 0.066(6) 0.042(5) 0.032(5) 0.004(4) 0.000(4) -0.001(4) C31" 0.055(5) 0.026(4) 0.041(4) -0.012(3) -0.003(4) -0.003(3) C32" 0.057(6) 0.035(4) 0.045(5) -0.001(4) 0.010(4) 0.002(4) C33" 0.084(7) 0.028(4) 0.057(6) -0.001(4) 0.010(5) -0.008(5) C34" 0.070(7) 0.043(5) 0.072(7) -0.004(5) 0.000(5) -0.014(5) C35" 0.059(7) 0.071(7) 0.106(9) 0.002(6) -0.021(6) -0.008(5) C36" 0.054(6) 0.051(5) 0.069(6) 0.011(5) -0.008(5) -0.009(5) Al* 0.0409(13) 0.0319(12) 0.0374(13) 0.0008(10) 0.0080(11) -0.0005(10) P1* 0.0422(12) 0.0363(11) 0.0313(11) -0.0002(9) -0.0003(9) 0.0026(9) P2* 0.0383(11) 0.0280(10) 0.0352(11) -0.0005(8) 0.0044(9) -0.0007(8) P3* 0.0521(14) 0.0278(11) 0.0671(15) 0.0045(10) 0.0246(12) 0.0032(10) S1* 0.0494(12) 0.0432(12) 0.0399(12) -0.0050(9) -0.0021(9) -0.0094(9) S2* 0.0467(12) 0.0316(10) 0.0327(10) -0.0003(8) -0.0051(9) 0.0063(9) S3* 0.0436(11) 0.0344(11) 0.0327(10) -0.0029(8) 0.0052(9) -0.0070(9) S4* 0.0432(12) 0.0402(11) 0.0386(11) 0.0087(9) 0.0057(9) 0.0022(9) S5* 0.0546(13) 0.0348(11) 0.0571(14) -0.0117(10) 0.0200(11) -0.0098(9) S6* 0.0494(13) 0.0339(11) 0.0494(13) 0.0013(9) 0.0152(10) 0.0005(9) C1* 0.040(5) 0.054(5) 0.044(5) 0.005(5) 0.002(4) 0.005(5) C2* 0.052(5) 0.050(5) 0.053(5) 0.005(5) 0.005(5) 0.006(5) C3* 0.043(5) 0.049(5) 0.057(5) 0.002(5) -0.003(5) 0.006(5) C4* 0.049(5) 0.054(5) 0.062(5) 0.010(5) 0.003(5) 0.011(5) C5* 0.057(5) 0.045(5) 0.060(5) 0.004(5) -0.001(5) 0.008(5) C6* 0.046(5) 0.046(5) 0.054(5) 0.005(5) -0.002(5) 0.009(5) C7* 0.042(4) 0.024(4) 0.035(4) -0.006(3) 0.000(4) 0.007(3) C8* 0.044(5) 0.039(5) 0.030(4) 0.002(4) -0.006(4) 0.003(4) C9* 0.063(5) 0.048(5) 0.023(4) 0.004(3) -0.008(4) 0.003(4) C10* 0.065(6) 0.046(5) 0.053(6) 0.008(4) 0.005(5) -0.001(5) C11* 0.066(6) 0.045(5) 0.053(6) -0.001(4) -0.003(5) -0.009(4) C12* 0.057(5) 0.033(4) 0.036(5) 0.000(4) -0.006(4) 0.002(4) C13* 0.043(4) 0.019(4) 0.030(4) 0.001(3) 0.003(3) 0.002(3) C14* 0.041(4) 0.037(5) 0.044(5) 0.002(4) -0.014(4) -0.004(4) C15* 0.054(5) 0.034(5) 0.060(6) 0.006(4) -0.004(4) 0.004(4) C16* 0.058(5) 0.027(4) 0.045(5) 0.000(4) 0.008(4) 0.004(4) C17* 0.049(5) 0.047(5) 0.041(5) -0.008(4) -0.004(4) -0.006(4) C18* 0.074(6) 0.029(4) 0.038(5) 0.004(4) 0.000(4) 0.006(4) C19* 0.046(5) 0.027(4) 0.045(5) -0.010(3) 0.010(4) 0.005(3) C20* 0.041(5) 0.033(4) 0.077(6) -0.011(4) 0.006(4) 0.000(4) C21* 0.052(6) 0.064(6) 0.089(7) -0.015(6) 0.021(5) 0.000(5) C22* 0.059(6) 0.050(6) 0.102(8) -0.018(6) -0.006(6) 0.015(5) C23* 0.083(7) 0.031(5) 0.090(7) 0.001(5) 0.000(6) 0.014(5) C24* 0.071(6) 0.033(5) 0.058(6) -0.004(4) 0.009(5) 0.003(4) C25* 0.094(7) 0.028(6) 0.060(6) 0.007(5) -0.003(6) 0.006(6) C26* 0.103(7) 0.028(5) 0.059(6) -0.008(5) 0.000(6) 0.004(6) C27* 0.104(7) 0.036(6) 0.062(6) -0.002(5) -0.003(6) 0.003(6) C28* 0.103(7) 0.030(6) 0.073(7) 0.000(5) 0.001(6) 0.002(6) C29* 0.112(7) 0.044(6) 0.083(7) 0.000(6) -0.019(6) 0.001(6) C30* 0.110(7) 0.039(6) 0.079(7) 0.003(6) -0.012(6) 0.003(6) C25D 0.095(7) 0.027(5) 0.057(6) 0.001(5) -0.007(6) 0.003(6) C26D 0.112(7) 0.046(6) 0.063(6) -0.003(5) -0.003(6) 0.016(6) C27D 0.114(7) 0.047(6) 0.068(7) -0.008(6) -0.011(6) 0.016(6) C28D 0.105(7) 0.041(6) 0.077(7) 0.010(6) -0.011(6) -0.008(6) C29D 0.095(7) 0.043(6) 0.064(6) 0.006(5) 0.002(6) 0.005(6) C30D 0.093(7) 0.036(6) 0.063(6) 0.014(5) 0.005(6) 0.007(6) C31* 0.053(5) 0.029(6) 0.079(7) 0.002(6) 0.027(5) -0.010(5) C32* 0.057(5) 0.043(6) 0.085(7) -0.002(6) 0.025(6) -0.011(5) C33* 0.060(6) 0.038(6) 0.083(7) -0.002(6) 0.027(6) -0.012(5) C34* 0.053(5) 0.041(6) 0.081(7) 0.003(6) 0.028(6) -0.018(5) C35* 0.057(5) 0.048(6) 0.076(7) 0.005(6) 0.030(6) -0.012(5) C36* 0.053(5) 0.041(6) 0.073(7) 0.003(6) 0.026(5) -0.015(5) C31D 0.050(5) 0.032(6) 0.074(7) 0.003(6) 0.028(5) -0.008(5) C32D 0.056(5) 0.041(6) 0.085(7) 0.003(6) 0.023(5) -0.009(5) C33D 0.064(6) 0.037(6) 0.086(7) -0.005(6) 0.025(6) -0.015(5) C34D 0.057(5) 0.038(6) 0.080(7) 0.004(6) 0.026(6) -0.015(5) C35D 0.057(5) 0.044(6) 0.085(7) 0.002(6) 0.026(6) -0.010(5) C36D 0.060(6) 0.046(6) 0.085(7) -0.002(6) 0.025(6) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al S2 2.396(3) . ? Al S3 2.424(3) . ? Al S1 2.427(3) . ? Al S5 2.430(3) . ? Al S6 2.431(3) . ? Al S4 2.455(3) . ? P1 C1 1.792(4) . ? P1 C7 1.809(4) . ? P1 S2 2.017(3) . ? P1 S1 2.018(2) . ? P2 C19 1.803(4) . ? P2 C13 1.810(4) . ? P2 S4 2.007(3) . ? P2 S3 2.015(3) . ? P3 C31 1.808(4) . ? P3 C25 1.819(4) . ? P3 S5 2.005(2) . ? P3 S6 2.014(3) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? Al' S5' 2.414(3) . ? Al' S4' 2.423(3) . ? Al' S6' 2.425(3) . ? Al' S3' 2.426(3) . ? Al' S2' 2.429(3) . ? Al' S1' 2.457(3) . ? P1' C7' 1.811(4) . ? P1' C1' 1.811(4) . ? P1' S1' 2.002(2) . ? P1' S2' 2.016(2) . ? P2' C19' 1.782(3) . ? P2' C13' 1.805(4) . ? P2' S3' 2.017(2) . ? P2' S4' 2.019(2) . ? P3' C31' 1.803(4) . ? P3' C25' 1.805(4) . ? P3' S6' 2.005(2) . ? P3' S5' 2.013(3) . ? C1' C2' 1.3900 . ? C1' C6' 1.3900 . ? C2' C3' 1.3900 . ? C3' C4' 1.3900 . ? C4' C5' 1.3900 . ? C5' C6' 1.3900 . ? C7' C8' 1.3900 . ? C7' C12' 1.3900 . ? C8' C9' 1.3900 . ? C9' C10' 1.3900 . ? C10' C11' 1.3900 . ? C11' C12' 1.3900 . ? C13' C14' 1.3900 . ? C13' C18' 1.3900 . ? C14' C15' 1.3900 . ? C15' C16' 1.3900 . ? C16' C17' 1.3900 . ? C17' C18' 1.3900 . ? C19' C20' 1.3900 . ? C19' C24' 1.3900 . ? C20' C21' 1.3900 . ? C21' C22' 1.3900 . ? C22' C23' 1.3900 . ? C23' C24' 1.3900 . ? C25' C26' 1.3900 . ? C25' C30' 1.3900 . ? C26' C27' 1.3900 . ? C27' C28' 1.3900 . ? C28' C29' 1.3900 . ? C29' C30' 1.3900 . ? C31' C32' 1.3900 . ? C31' C36' 1.3900 . ? C32' C33' 1.3900 . ? C33' C34' 1.3900 . ? C34' C35' 1.3900 . ? C35' C36' 1.3900 . ? Al" S3" 2.397(3) . ? Al" S4" 2.417(3) . ? Al" S1" 2.419(3) . ? Al" S6" 2.425(3) . ? Al" S5" 2.446(3) . ? Al" S2" 2.450(3) . ? P1" C1" 1.794(6) . ? P1" C1C 1.813(7) . ? P1" C7" 1.815(4) . ? P1" S1" 2.004(3) . ? P1" S2" 2.011(3) . ? P2" C19" 1.775(6) . ? P2" C13" 1.807(4) . ? P2" C19C 1.832(6) . ? P2" S3" 2.010(3) . ? P2" S4" 2.018(3) . ? P3" C31" 1.795(4) . ? P3" C25" 1.813(4) . ? P3" S6" 2.012(3) . ? P3" S5" 2.013(3) . ? C1" C2" 1.3900 . ? C1" C6" 1.3900 . ? C2" C3" 1.3900 . ? C3" C4" 1.3900 . ? C4" C5" 1.3900 . ? C5" C6" 1.3900 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C2C C3C 1.3900 . ? C3C C4C 1.3900 . ? C4C C5C 1.3900 . ? C5C C6C 1.3900 . ? C7" C8" 1.3900 . ? C7" C12" 1.3900 . ? C8" C9" 1.3900 . ? C9" C10" 1.3900 . ? C10" C11" 1.3900 . ? C11" C12" 1.3900 . ? C13" C14" 1.3900 . ? C13" C18" 1.3900 . ? C14" C15" 1.3900 . ? C15" C16" 1.3900 . ? C16" C17" 1.3900 . ? C17" C18" 1.3900 . ? C19" C20" 1.3900 . ? C19" C24" 1.3900 . ? C20" C21" 1.3900 . ? C21" C22" 1.3900 . ? C22" C23" 1.3900 . ? C23" C24" 1.3900 . ? C19C C20C 1.3900 . ? C19C C24C 1.3900 . ? C20C C21C 1.3900 . ? C21C C22C 1.3900 . ? C22C C23C 1.3900 . ? C23C C24C 1.3900 . ? C25" C26" 1.3900 . ? C25" C30" 1.3900 . ? C26" C27" 1.3900 . ? C27" C28" 1.3900 . ? C28" C29" 1.3900 . ? C29" C30" 1.3900 . ? C31" C32" 1.3900 . ? C31" C36" 1.3900 . ? C32" C33" 1.3900 . ? C33" C34" 1.3900 . ? C34" C35" 1.3900 . ? C35" C36" 1.3900 . ? Al* S4* 2.414(3) . ? Al* S5* 2.419(3) . ? Al* S3* 2.426(3) . ? Al* S6* 2.436(3) . ? Al* S2* 2.438(3) . ? Al* S1* 2.438(3) . ? P1* C1D 1.781(7) . ? P1* C7* 1.808(4) . ? P1* C1* 1.826(5) . ? P1* S1* 2.009(3) . ? P1* S2* 2.009(3) . ? P2* C13* 1.800(4) . ? P2* C19* 1.806(4) . ? P2* S3* 2.013(3) . ? P2* S4* 2.017(2) . ? P3* C25* 1.782(6) . ? P3* C31D 1.789(7) . ? P3* C31* 1.829(7) . ? P3* C25D 1.851(6) . ? P3* S6* 1.999(3) . ? P3* S5* 2.015(3) . ? C1* C2* 1.3900 . ? C1* C6* 1.3900 . ? C2* C3* 1.3900 . ? C3* C4* 1.3900 . ? C4* C5* 1.3900 . ? C5* C6* 1.3900 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C2D C3D 1.3900 . ? C3D C4D 1.3900 . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? C7* C8* 1.3900 . ? C7* C12* 1.3900 . ? C8* C9* 1.3900 . ? C9* C10* 1.3900 . ? C10* C11* 1.3900 . ? C11* C12* 1.3900 . ? C13* C14* 1.3900 . ? C13* C18* 1.3900 . ? C14* C15* 1.3900 . ? C15* C16* 1.3900 . ? C16* C17* 1.3900 . ? C17* C18* 1.3900 . ? C19* C20* 1.3900 . ? C19* C24* 1.3900 . ? C20* C21* 1.3900 . ? C21* C22* 1.3900 . ? C22* C23* 1.3900 . ? C23* C24* 1.3900 . ? C25* C26* 1.3900 . ? C25* C30* 1.3900 . ? C26* C27* 1.3900 . ? C27* C28* 1.3900 . ? C28* C29* 1.3900 . ? C29* C30* 1.3900 . ? C25D C26D 1.3900 . ? C25D C30D 1.3900 . ? C26D C27D 1.3900 . ? C27D C28D 1.3900 . ? C28D C29D 1.3900 . ? C29D C30D 1.3900 . ? C31* C32* 1.3900 . ? C31* C36* 1.3900 . ? C32* C33* 1.3900 . ? C33* C34* 1.3900 . ? C34* C35* 1.3900 . ? C35* C36* 1.3900 . ? C31D C32D 1.3900 . ? C31D C36D 1.3900 . ? C32D C33D 1.3900 . ? C33D C34D 1.3900 . ? C34D C35D 1.3900 . ? C35D C36D 1.3900 . ? 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 S2 Al S3 95.64(9) . . ? S2 Al S1 83.70(9) . . ? S3 Al S1 89.49(9) . . ? S2 Al S5 171.54(11) . . ? S3 Al S5 91.04(9) . . ? S1 Al S5 91.20(9) . . ? S2 Al S6 90.63(9) . . ? S3 Al S6 171.35(12) . . ? S1 Al S6 97.13(10) . . ? S5 Al S6 83.29(8) . . ? S2 Al S4 89.84(9) . . ? S3 Al S4 82.95(9) . . ? S1 Al S4 169.54(11) . . ? S5 Al S4 96.13(10) . . ? S6 Al S4 91.14(9) . . ? C1 P1 C7 105.5(2) . . ? C1 P1 S2 110.48(18) . . ? C7 P1 S2 111.77(18) . . ? C1 P1 S1 111.60(18) . . ? C7 P1 S1 111.80(18) . . ? S2 P1 S1 105.80(11) . . ? C19 P2 C13 104.7(2) . . ? C19 P2 S4 113.0(2) . . ? C13 P2 S4 111.49(19) . . ? C19 P2 S3 109.96(18) . . ? C13 P2 S3 110.86(19) . . ? S4 P2 S3 106.92(11) . . ? C31 P3 C25 105.7(3) . . ? C31 P3 S5 111.6(2) . . ? C25 P3 S5 111.23(19) . . ? C31 P3 S6 111.3(2) . . ? C25 P3 S6 110.19(19) . . ? S5 P3 S6 107.00(11) . . ? P1 S1 Al 84.30(9) . . ? P1 S2 Al 85.12(9) . . ? P2 S3 Al 84.26(9) . . ? P2 S4 Al 83.63(9) . . ? P3 S5 Al 84.91(9) . . ? P3 S6 Al 84.67(9) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 118.2(3) . . ? C6 C1 P1 121.4(3) . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 120.1(3) . . ? C12 C7 P1 119.9(3) . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 P2 121.4(3) . . ? C18 C13 P2 118.4(3) . . ? C15 C14 C13 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 118.1(3) . . ? C24 C19 P2 121.9(3) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 P3 120.7(3) . . ? C30 C25 P3 119.3(3) . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C25 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P3 119.1(3) . . ? C36 C31 P3 120.8(3) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? S5' Al' S4' 98.59(10) . . ? S5' Al' S6' 83.23(9) . . ? S4' Al' S6' 89.25(9) . . ? S5' Al' S3' 90.73(9) . . ? S4' Al' S3' 83.10(9) . . ? S6' Al' S3' 169.47(11) . . ? S5' Al' S2' 170.62(12) . . ? S4' Al' S2' 89.80(9) . . ? S6' Al' S2' 92.76(9) . . ? S3' Al' S2' 94.45(9) . . ? S5' Al' S1' 89.87(9) . . ? S4' Al' S1' 169.50(11) . . ? S6' Al' S1' 97.96(10) . . ? S3' Al' S1' 90.62(9) . . ? S2' Al' S1' 82.27(8) . . ? C7' P1' C1' 104.5(2) . . ? C7' P1' S1' 111.70(18) . . ? C1' P1' S1' 113.66(19) . . ? C7' P1' S2' 111.41(18) . . ? C1' P1' S2' 109.47(17) . . ? S1' P1' S2' 106.22(11) . . ? C19' P2' C13' 103.9(2) . . ? C19' P2' S3' 112.09(18) . . ? C13' P2' S3' 111.35(18) . . ? C19' P2' S4' 112.05(18) . . ? C13' P2' S4' 111.93(18) . . ? S3' P2' S4' 105.71(11) . . ? C31' P3' C25' 104.8(2) . . ? C31' P3' S6' 112.40(19) . . ? C25' P3' S6' 113.16(19) . . ? C31' P3' S5' 111.27(19) . . ? C25' P3' S5' 109.1(2) . . ? S6' P3' S5' 106.20(11) . . ? P1' S1' Al' 84.57(9) . . ? P1' S2' Al' 85.01(9) . . ? P2' S3' Al' 84.92(9) . . ? P2' S4' Al' 84.97(9) . . ? P3' S5' Al' 85.24(9) . . ? P3' S6' Al' 85.13(9) . . ? C2' C1' C6' 120.0 . . ? C2' C1' P1' 121.5(3) . . ? C6' C1' P1' 118.3(3) . . ? C3' C2' C1' 120.0 . . ? C4' C3' C2' 120.0 . . ? C3' C4' C5' 120.0 . . ? C6' C5' C4' 120.0 . . ? C5' C6' C1' 120.0 . . ? C8' C7' C12' 120.0 . . ? C8' C7' P1' 118.5(3) . . ? C12' C7' P1' 121.5(3) . . ? C7' C8' C9' 120.0 . . ? C10' C9' C8' 120.0 . . ? C11' C10' C9' 120.0 . . ? C12' C11' C10' 120.0 . . ? C11' C12' C7' 120.0 . . ? C14' C13' C18' 120.0 . . ? C14' C13' P2' 120.6(3) . . ? C18' C13' P2' 119.4(3) . . ? C15' C14' C13' 120.0 . . ? C16' C15' C14' 120.0 . . ? C15' C16' C17' 120.0 . . ? C18' C17' C16' 120.0 . . ? C17' C18' C13' 120.0 . . ? C20' C19' C24' 120.0 . . ? C20' C19' P2' 118.9(3) . . ? C24' C19' P2' 120.9(3) . . ? C21' C20' C19' 120.0 . . ? C20' C21' C22' 120.0 . . ? C23' C22' C21' 120.0 . . ? C22' C23' C24' 120.0 . . ? C23' C24' C19' 120.0 . . ? C26' C25' C30' 120.0 . . ? C26' C25' P3' 117.8(3) . . ? C30' C25' P3' 122.0(3) . . ? C25' C26' C27' 120.0 . . ? C28' C27' C26' 120.0 . . ? C27' C28' C29' 120.0 . . ? C30' C29' C28' 120.0 . . ? C29' C30' C25' 120.0 . . ? C32' C31' C36' 120.0 . . ? C32' C31' P3' 118.9(3) . . ? C36' C31' P3' 121.0(3) . . ? C33' C32' C31' 120.0 . . ? C32' C33' C34' 120.0 . . ? C33' C34' C35' 120.0 . . ? C36' C35' C34' 120.0 . . ? C35' C36' C31' 120.0 . . ? S3" Al" S4" 83.29(10) . . ? S3" Al" S1" 87.55(10) . . ? S4" Al" S1" 169.15(12) . . ? S3" Al" S6" 173.10(13) . . ? S4" Al" S6" 91.24(10) . . ? S1" Al" S6" 98.30(11) . . ? S3" Al" S5" 93.15(10) . . ? S4" Al" S5" 96.77(11) . . ? S1" Al" S5" 89.49(10) . . ? S6" Al" S5" 83.30(9) . . ? S3" Al" S2" 95.97(10) . . ? S4" Al" S2" 92.13(10) . . ? S1" Al" S2" 83.04(10) . . ? S6" Al" S2" 88.40(9) . . ? S5" Al" S2" 167.94(13) . . ? C1" P1" C7" 109.4(4) . . ? C1C P1" C7" 100.1(4) . . ? C1" P1" S1" 103.6(4) . . ? C1C P1" S1" 116.6(4) . . ? C7" P1" S1" 111.44(19) . . ? C1" P1" S2" 114.3(4) . . ? C1C P1" S2" 110.7(5) . . ? C7" P1" S2" 110.92(19) . . ? S1" P1" S2" 106.99(12) . . ? C19" P2" C13" 107.8(4) . . ? C13" P2" C19C 103.5(4) . . ? C19" P2" S3" 106.8(4) . . ? C13" P2" S3" 111.7(2) . . ? C19C P2" S3" 113.8(4) . . ? C19" P2" S4" 113.5(4) . . ? C13" P2" S4" 111.8(2) . . ? C19C P2" S4" 111.1(3) . . ? S3" P2" S4" 105.18(12) . . ? C31" P3" C25" 104.2(2) . . ? C31" P3" S6" 111.0(2) . . ? C25" P3" S6" 112.31(19) . . ? C31" P3" S5" 111.7(2) . . ? C25" P3" S5" 110.6(2) . . ? S6" P3" S5" 107.08(12) . . ? P1" S1" Al" 84.85(10) . . ? P1" S2" Al" 83.90(10) . . ? P2" S3" Al" 85.80(10) . . ? P2" S4" Al" 85.10(10) . . ? P3" S5" Al" 84.45(10) . . ? P3" S6" Al" 85.07(10) . . ? C2" C1" C6" 120.0 . . ? C2" C1" P1" 121.7(5) . . ? C6" C1" P1" 118.3(5) . . ? C1" C2" C3" 120.0 . . ? C4" C3" C2" 120.0 . . ? C5" C4" C3" 120.0 . . ? C4" C5" C6" 120.0 . . ? C5" C6" C1" 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C P1" 118.7(5) . . ? C6C C1C P1" 121.3(5) . . ? C3C C2C C1C 120.0 . . ? C2C C3C C4C 120.0 . . ? C5C C4C C3C 120.0 . . ? C4C C5C C6C 120.0 . . ? C5C C6C C1C 120.0 . . ? C8" C7" C12" 120.0 . . ? C8" C7" P1" 118.3(3) . . ? C12" C7" P1" 121.7(3) . . ? C7" C8" C9" 120.0 . . ? C8" C9" C10" 120.0 . . ? C11" C10" C9" 120.0 . . ? C10" C11" C12" 120.0 . . ? C11" C12" C7" 120.0 . . ? C14" C13" C18" 120.0 . . ? C14" C13" P2" 120.0(3) . . ? C18" C13" P2" 120.0(3) . . ? C15" C14" C13" 120.0 . . ? C16" C15" C14" 120.0 . . ? C15" C16" C17" 120.0 . . ? C18" C17" C16" 120.0 . . ? C17" C18" C13" 120.0 . . ? C20" C19" C24" 120.0 . . ? C20" C19" P2" 120.1(5) . . ? C24" C19" P2" 119.2(5) . . ? C19" C20" C21" 120.0 . . ? C20" C21" C22" 120.0 . . ? C23" C22" C21" 120.0 . . ? C22" C23" C24" 120.0 . . ? C23" C24" C19" 120.0 . . ? C20C C19C C24C 120.0 . . ? C20C C19C P2" 118.8(5) . . ? C24C C19C P2" 121.1(5) . . ? C19C C20C C21C 120.0 . . ? C20C C21C C22C 120.0 . . ? C21C C22C C23C 120.0 . . ? C24C C23C C22C 120.0 . . ? C23C C24C C19C 120.0 . . ? C26" C25" C30" 120.0 . . ? C26" C25" P3" 118.6(3) . . ? C30" C25" P3" 121.4(3) . . ? C27" C26" C25" 120.0 . . ? C26" C27" C28" 120.0 . . ? C29" C28" C27" 120.0 . . ? C30" C29" C28" 120.0 . . ? C29" C30" C25" 120.0 . . ? C32" C31" C36" 120.0 . . ? C32" C31" P3" 119.5(3) . . ? C36" C31" P3" 120.5(3) . . ? C33" C32" C31" 120.0 . . ? C32" C33" C34" 120.0 . . ? C35" C34" C33" 120.0 . . ? C34" C35" C36" 120.0 . . ? C35" C36" C31" 120.0 . . ? S4* Al* S5* 98.22(10) . . ? S4* Al* S3* 82.91(9) . . ? S5* Al* S3* 90.49(9) . . ? S4* Al* S6* 89.48(10) . . ? S5* Al* S6* 83.28(9) . . ? S3* Al* S6* 169.40(12) . . ? S4* Al* S2* 90.52(10) . . ? S5* Al* S2* 169.78(13) . . ? S3* Al* S2* 95.87(10) . . ? S6* Al* S2* 91.55(9) . . ? S4* Al* S1* 170.10(12) . . ? S5* Al* S1* 89.58(10) . . ? S3* Al* S1* 90.98(9) . . ? S6* Al* S1* 97.52(10) . . ? S2* Al* S1* 82.34(9) . . ? C1D P1* C7* 107.2(4) . . ? C7* P1* C1* 102.1(3) . . ? C1D P1* S1* 107.3(4) . . ? C7* P1* S1* 111.64(18) . . ? C1* P1* S1* 114.8(3) . . ? C1D P1* S2* 112.9(5) . . ? C7* P1* S2* 111.65(19) . . ? C1* P1* S2* 110.7(3) . . ? S1* P1* S2* 106.06(12) . . ? C13* P2* C19* 104.7(2) . . ? C13* P2* S3* 110.72(18) . . ? C19* P2* S3* 113.01(19) . . ? C13* P2* S4* 111.31(18) . . ? C19* P2* S4* 111.84(19) . . ? S3* P2* S4* 105.36(11) . . ? C25* P3* C31* 102.1(7) . . ? C31D P3* C25D 106.2(7) . . ? C25* P3* S6* 120.6(3) . . ? C31D P3* S6* 112.3(5) . . ? C31* P3* S6* 111.0(5) . . ? C25D P3* S6* 107.1(3) . . ? C25* P3* S5* 109.2(4) . . ? C31D P3* S5* 115.6(4) . . ? C31* P3* S5* 106.1(4) . . ? C25D P3* S5* 108.3(3) . . ? S6* P3* S5* 107.00(12) . . ? P1* S1* Al* 85.07(10) . . ? P1* S2* Al* 85.07(10) . . ? P2* S3* Al* 85.15(10) . . ? P2* S4* Al* 85.38(10) . . ? P3* S5* Al* 84.90(10) . . ? P3* S6* Al* 84.80(10) . . ? C2* C1* C6* 120.0 . . ? C2* C1* P1* 121.0(4) . . ? C6* C1* P1* 118.8(4) . . ? C3* C2* C1* 120.0 . . ? C4* C3* C2* 120.0 . . ? C3* C4* C5* 120.0 . . ? C6* C5* C4* 120.0 . . ? C5* C6* C1* 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D P1* 121.7(6) . . ? C6D C1D P1* 118.3(6) . . ? C3D C2D C1D 120.0 . . ? C2D C3D C4D 120.0 . . ? C5D C4D C3D 120.0 . . ? C4D C5D C6D 120.0 . . ? C5D C6D C1D 120.0 . . ? C8* C7* C12* 120.0 . . ? C8* C7* P1* 118.5(3) . . ? C12* C7* P1* 121.5(3) . . ? C7* C8* C9* 120.0 . . ? C8* C9* C10* 120.0 . . ? C11* C10* C9* 120.0 . . ? C12* C11* C10* 120.0 . . ? C11* C12* C7* 120.0 . . ? C14* C13* C18* 120.0 . . ? C14* C13* P2* 120.3(3) . . ? C18* C13* P2* 119.7(3) . . ? C15* C14* C13* 120.0 . . ? C14* C15* C16* 120.0 . . ? C17* C16* C15* 120.0 . . ? C16* C17* C18* 120.0 . . ? C17* C18* C13* 120.0 . . ? C20* C19* C24* 120.0 . . ? C20* C19* P2* 118.6(3) . . ? C24* C19* P2* 121.4(3) . . ? C21* C20* C19* 120.0 . . ? C20* C21* C22* 120.0 . . ? C23* C22* C21* 120.0 . . ? C22* C23* C24* 120.0 . . ? C23* C24* C19* 120.0 . . ? C26* C25* C30* 120.0 . . ? C26* C25* P3* 122.6(5) . . ? C30* C25* P3* 117.4(5) . . ? C27* C26* C25* 120.0 . . ? C26* C27* C28* 120.0 . . ? C29* C28* C27* 120.0 . . ? C28* C29* C30* 120.0 . . ? C29* C30* C25* 120.0 . . ? C26D C25D C30D 120.0 . . ? C26D C25D P3* 118.3(5) . . ? C30D C25D P3* 120.9(5) . . ? C27D C26D C25D 120.0 . . ? C26D C27D C28D 120.0 . . ? C29D C28D C27D 120.0 . . ? C28D C29D C30D 120.0 . . ? C29D C30D C25D 120.0 . . ? C32* C31* C36* 120.0 . . ? C32* C31* P3* 119.5(5) . . ? C36* C31* P3* 120.1(5) . . ? C31* C32* C33* 120.0 . . ? C34* C33* C32* 120.0 . . ? C33* C34* C35* 120.0 . . ? C36* C35* C34* 120.0 . . ? C35* C36* C31* 120.0 . . ? C32D C31D C36D 120.0 . . ? C32D C31D P3* 119.4(5) . . ? C36D C31D P3* 120.6(5) . . ? C33D C32D C31D 120.0 . . ? C32D C33D C34D 120.0 . . ? C35D C34D C33D 120.0 . . ? C36D C35D C34D 120.0 . . ? C35D C36D C31D 120.0 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 63.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.775 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.156 #===END