# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Norbert Mitzel' 'Andreas Mix' 'Beate Neumann' 'Anja Nieland' 'Hans-Georg Stammler' _publ_contact_author_name 'Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-BIELEFELD.DE _publ_section_title ; Cationic rare-earth-metal methyl complexes: a new preparative access ; # Attachment 'compound1_6.CIF' #============================================================================== data_compound1 _database_code_depnum_ccdc_archive 'CCDC 764350' #TrackingRef 'compound1_6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C17 H35 O8 Y, 2(C4 H12 Al) ' _chemical_formula_sum 'C25 H59 Al2 O8 Y' _chemical_formula_weight 630.59 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9894(3) _cell_length_b 20.8592(7) _cell_length_c 14.4231(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.4476(17) _cell_angle_gamma 90.00 _cell_volume 3291.28(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 50071 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6047 _exptl_absorpt_correction_T_max 0.9637 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44359 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7526 _reflns_number_gt 5759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _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^)+(0.0266P)^2^+1.1131P] 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 7526 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Y1 Y 0.259047(18) 0.070043(10) 0.171022(14) 0.01782(6) Uani 1 1 d . . . O1 O 0.12293(12) 0.12927(7) 0.26704(10) 0.0220(3) Uani 1 1 d . . . O2 O 0.03928(12) 0.06047(7) 0.11439(10) 0.0214(3) Uani 1 1 d . . . O3 O 0.17138(13) 0.15242(8) 0.05400(10) 0.0263(4) Uani 1 1 d . . . O4 O 0.31558(13) 0.18298(7) 0.19466(10) 0.0241(4) Uani 1 1 d . . . O5 O 0.17167(12) -0.01119(8) 0.26230(10) 0.0217(3) Uani 1 1 d . . . O6 O 0.38120(12) -0.03054(8) 0.19640(10) 0.0236(4) Uani 1 1 d . . . O7 O 0.47949(13) 0.08394(7) 0.19041(10) 0.0229(4) Uani 1 1 d . . . O8 O 0.35371(12) 0.06566(7) 0.33823(10) 0.0211(3) Uani 1 1 d . . . C1 C -0.00576(18) 0.13568(12) 0.23553(15) 0.0247(5) Uani 1 1 d . . . H1A H -0.0192 0.1730 0.1934 0.030 Uiso 1 1 calc R . . H1B H -0.0544 0.1417 0.2892 0.030 Uiso 1 1 calc R . . C2 C -0.04208(18) 0.07507(12) 0.18509(15) 0.0234(5) Uani 1 1 d . . . H2A H -0.0406 0.0393 0.2302 0.028 Uiso 1 1 calc R . . H2B H -0.1267 0.0793 0.1554 0.028 Uiso 1 1 calc R . . C3 C 0.0006(2) 0.08501(12) 0.02206(15) 0.0272(6) Uani 1 1 d . . . H3A H -0.0898 0.0862 0.0131 0.033 Uiso 1 1 calc R . . H3B H 0.0295 0.0558 -0.0253 0.033 Uiso 1 1 calc R . . C4 C 0.05032(19) 0.15132(12) 0.00842(15) 0.0259(5) Uani 1 1 d . . . H4A H 0.0516 0.1607 -0.0588 0.031 Uiso 1 1 calc R . . H4B H -0.0012 0.1838 0.0359 0.031 Uiso 1 1 calc R . . C5 C 0.2401(2) 0.20837(12) 0.03591(16) 0.0293(6) Uani 1 1 d . . . H5A H 0.1913 0.2476 0.0437 0.035 Uiso 1 1 calc R . . H5B H 0.2648 0.2075 -0.0283 0.035 Uiso 1 1 calc R . . C6 C 0.3512(2) 0.20676(12) 0.10640(16) 0.0277(5) Uani 1 1 d . . . H6A H 0.4144 0.1784 0.0839 0.033 Uiso 1 1 calc R . . H6B H 0.3860 0.2504 0.1148 0.033 Uiso 1 1 calc R . . C7 C 0.2343(2) 0.22561(12) 0.23844(16) 0.0278(5) Uani 1 1 d . . . H7A H 0.1705 0.2426 0.1918 0.033 Uiso 1 1 calc R . . H7B H 0.2804 0.2621 0.2682 0.033 Uiso 1 1 calc R . . C8 C 0.1775(2) 0.18647(11) 0.31012(16) 0.0259(5) Uani 1 1 d . . . H8A H 0.2406 0.1743 0.3606 0.031 Uiso 1 1 calc R . . H8B H 0.1141 0.2120 0.3377 0.031 Uiso 1 1 calc R . . C9 C 0.19503(19) -0.07526(11) 0.23010(16) 0.0259(5) Uani 1 1 d . . . H9A H 0.1552 -0.0808 0.1661 0.031 Uiso 1 1 calc R . . H9B H 0.1588 -0.1068 0.2708 0.031 Uiso 1 1 calc R . . C10 C 0.33051(19) -0.08815(11) 0.23046(16) 0.0251(5) Uani 1 1 d . . . H10A H 0.3672 -0.0978 0.2943 0.030 Uiso 1 1 calc R . . H10B H 0.3453 -0.1249 0.1895 0.030 Uiso 1 1 calc R . . C11 C 0.51109(19) -0.03213(12) 0.19236(17) 0.0265(5) Uani 1 1 d . . . H11A H 0.5336 -0.0675 0.1515 0.032 Uiso 1 1 calc R . . H11B H 0.5533 -0.0389 0.2553 0.032 Uiso 1 1 calc R . . C12 C 0.5468(2) 0.03146(11) 0.15382(16) 0.0260(5) Uani 1 1 d . . . H12A H 0.6355 0.0384 0.1697 0.031 Uiso 1 1 calc R . . H12B H 0.5312 0.0307 0.0851 0.031 Uiso 1 1 calc R . . C13 C 0.53030(19) 0.11055(12) 0.27818(15) 0.0250(5) Uani 1 1 d . . . H13A H 0.5079 0.1564 0.2812 0.030 Uiso 1 1 calc R . . H13B H 0.6206 0.1076 0.2825 0.030 Uiso 1 1 calc R . . C14 C 0.48384(18) 0.07536(12) 0.35911(15) 0.0257(5) Uani 1 1 d . . . H14A H 0.5259 0.0336 0.3683 0.031 Uiso 1 1 calc R . . H14B H 0.4999 0.1008 0.4169 0.031 Uiso 1 1 calc R . . C15 C 0.3108(2) 0.01694(12) 0.39825(15) 0.0274(5) Uani 1 1 d . . . H15A H 0.3118 0.0336 0.4626 0.033 Uiso 1 1 calc R . . H15B H 0.3651 -0.0210 0.3992 0.033 Uiso 1 1 calc R . . C16 C 0.18250(19) -0.00183(12) 0.36220(14) 0.0262(5) Uani 1 1 d . . . H16A H 0.1599 -0.0420 0.3930 0.031 Uiso 1 1 calc R . . H16B H 0.1250 0.0321 0.3780 0.031 Uiso 1 1 calc R . . C17 C 0.2866(2) 0.02909(13) 0.01817(15) 0.0298(6) Uani 1 1 d . . . H17A H 0.3157 -0.0153 0.0234 0.045 Uiso 1 1 calc R . . H17B H 0.3468 0.0554 -0.0103 0.045 Uiso 1 1 calc R . . H17C H 0.2085 0.0305 -0.0207 0.045 Uiso 1 1 calc R . . Al1 Al 0.18156(6) 0.08757(4) 0.63467(5) 0.02350(16) Uani 1 1 d . . . C18 C 0.1412(2) 0.11179(13) 0.76394(16) 0.0316(6) Uani 1 1 d . . . H18A H 0.0866 0.0795 0.7868 0.047 Uiso 1 1 calc R . . H18B H 0.1008 0.1537 0.7619 0.047 Uiso 1 1 calc R . . H18C H 0.2167 0.1139 0.8058 0.047 Uiso 1 1 calc R . . C19 C 0.0583(2) 0.12565(13) 0.53833(17) 0.0333(6) Uani 1 1 d . . . H19A H 0.0922 0.1265 0.4779 0.050 Uiso 1 1 calc R . . H19B H 0.0387 0.1694 0.5566 0.050 Uiso 1 1 calc R . . H19C H -0.0162 0.0996 0.5335 0.050 Uiso 1 1 calc R . . C20 C 0.34942(19) 0.12012(12) 0.60924(16) 0.0258(5) Uani 1 1 d . . . H20A H 0.3865 0.1432 0.6640 0.039 Uiso 1 1 calc R . . H20B H 0.3413 0.1491 0.5556 0.039 Uiso 1 1 calc R . . H20C H 0.4014 0.0837 0.5959 0.039 Uiso 1 1 calc R . . C21 C 0.1841(2) -0.00886(11) 0.62727(16) 0.0277(5) Uani 1 1 d . . . H21A H 0.2341 -0.0222 0.5779 0.042 Uiso 1 1 calc R . . H21B H 0.1005 -0.0249 0.6133 0.042 Uiso 1 1 calc R . . H21C H 0.2190 -0.0264 0.6870 0.042 Uiso 1 1 calc R . . Al2 Al 0.67850(6) 0.25451(3) 0.46457(5) 0.02322(16) Uani 1 1 d . . . C22 C 0.6861(2) 0.16982(12) 0.53048(17) 0.0327(6) Uani 1 1 d . . . H22A H 0.7551 0.1698 0.5788 0.049 Uiso 1 1 calc R . . H22B H 0.6971 0.1355 0.4856 0.049 Uiso 1 1 calc R . . H22C H 0.6099 0.1628 0.5592 0.049 Uiso 1 1 calc R . . C23 C 0.51240(19) 0.26920(12) 0.39306(16) 0.0279(5) Uani 1 1 d . . . H23A H 0.4547 0.2367 0.4111 0.042 Uiso 1 1 calc R . . H23B H 0.5200 0.2661 0.3261 0.042 Uiso 1 1 calc R . . H23C H 0.4824 0.3119 0.4076 0.042 Uiso 1 1 calc R . . C24 C 0.8107(2) 0.25597(13) 0.37678(16) 0.0315(6) Uani 1 1 d . . . H24A H 0.8334 0.3005 0.3651 0.047 Uiso 1 1 calc R . . H24B H 0.7804 0.2356 0.3178 0.047 Uiso 1 1 calc R . . H24C H 0.8823 0.2326 0.4047 0.047 Uiso 1 1 calc R . . C25 C 0.7047(2) 0.32307(13) 0.56229(18) 0.0360(6) Uani 1 1 d . . . H25A H 0.6406 0.3202 0.6050 0.054 Uiso 1 1 calc R . . H25B H 0.7012 0.3653 0.5323 0.054 Uiso 1 1 calc R . . H25C H 0.7848 0.3172 0.5972 0.054 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 Y1 0.01804(10) 0.01879(12) 0.01701(10) 0.00026(9) 0.00369(7) 0.00113(9) O1 0.0194(7) 0.0230(9) 0.0236(8) -0.0033(7) 0.0024(6) 0.0021(6) O2 0.0202(7) 0.0261(10) 0.0181(7) 0.0000(7) 0.0025(6) 0.0006(6) O3 0.0236(8) 0.0254(10) 0.0293(9) 0.0069(7) -0.0003(7) 0.0005(7) O4 0.0217(8) 0.0211(9) 0.0299(9) 0.0011(7) 0.0043(6) 0.0015(7) O5 0.0208(8) 0.0243(9) 0.0201(8) 0.0018(7) 0.0014(6) -0.0015(7) O6 0.0221(8) 0.0214(9) 0.0279(8) 0.0050(7) 0.0057(7) 0.0016(7) O7 0.0189(7) 0.0241(9) 0.0260(8) -0.0013(7) 0.0048(6) 0.0027(6) O8 0.0185(7) 0.0253(9) 0.0195(7) -0.0006(7) 0.0019(6) -0.0010(7) C1 0.0183(11) 0.0308(14) 0.0255(12) -0.0016(10) 0.0051(9) 0.0036(10) C2 0.0155(10) 0.0326(15) 0.0225(11) 0.0020(10) 0.0047(8) -0.0003(10) C3 0.0256(12) 0.0363(16) 0.0190(11) 0.0000(10) -0.0018(9) 0.0009(10) C4 0.0229(11) 0.0325(15) 0.0221(12) 0.0043(10) 0.0003(9) 0.0057(10) C5 0.0289(12) 0.0269(15) 0.0328(13) 0.0084(11) 0.0072(10) 0.0005(11) C6 0.0271(12) 0.0227(14) 0.0343(13) 0.0074(11) 0.0084(10) -0.0014(10) C7 0.0247(12) 0.0229(14) 0.0354(13) -0.0065(11) 0.0011(10) 0.0049(10) C8 0.0254(12) 0.0246(14) 0.0273(12) -0.0101(10) 0.0005(10) 0.0051(10) C9 0.0283(12) 0.0203(13) 0.0284(12) 0.0009(10) -0.0012(10) -0.0050(10) C10 0.0266(12) 0.0189(13) 0.0299(12) 0.0031(10) 0.0023(10) 0.0008(10) C11 0.0210(11) 0.0269(14) 0.0324(13) 0.0006(11) 0.0063(10) 0.0064(10) C12 0.0217(11) 0.0276(14) 0.0297(13) -0.0017(11) 0.0081(10) 0.0046(10) C13 0.0173(11) 0.0241(14) 0.0334(13) -0.0036(11) 0.0012(9) -0.0008(9) C14 0.0194(11) 0.0336(15) 0.0235(11) -0.0028(11) -0.0009(9) 0.0008(10) C15 0.0325(13) 0.0330(15) 0.0167(11) 0.0057(10) 0.0028(9) -0.0015(11) C16 0.0272(12) 0.0332(15) 0.0191(11) 0.0035(10) 0.0062(9) -0.0014(10) C17 0.0257(12) 0.0388(16) 0.0253(12) 0.0005(11) 0.0041(10) 0.0115(11) Al1 0.0225(3) 0.0264(4) 0.0219(3) 0.0009(3) 0.0042(3) -0.0011(3) C18 0.0338(13) 0.0306(15) 0.0314(13) 0.0007(11) 0.0094(11) -0.0026(11) C19 0.0282(13) 0.0352(16) 0.0362(14) 0.0080(12) 0.0012(11) -0.0027(11) C20 0.0266(12) 0.0246(14) 0.0262(12) 0.0013(10) 0.0023(10) 0.0022(10) C21 0.0289(12) 0.0280(14) 0.0277(12) 0.0030(11) 0.0104(10) -0.0013(10) Al2 0.0205(3) 0.0231(4) 0.0261(4) -0.0013(3) 0.0024(3) 0.0007(3) C22 0.0282(13) 0.0313(15) 0.0379(14) 0.0064(12) -0.0004(11) -0.0011(11) C23 0.0264(12) 0.0262(14) 0.0314(13) -0.0005(11) 0.0035(10) 0.0008(10) C24 0.0275(12) 0.0377(16) 0.0296(13) 0.0039(12) 0.0040(10) 0.0013(11) C25 0.0243(12) 0.0377(17) 0.0462(16) -0.0144(13) 0.0049(11) -0.0033(11) _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 Y1 O5 2.4013(15) . ? Y1 C17 2.410(2) . ? Y1 O7 2.4294(14) . ? Y1 O4 2.4518(16) . ? Y1 O1 2.4647(14) . ? Y1 O2 2.4830(14) . ? Y1 O6 2.4988(15) . ? Y1 O3 2.5340(15) . ? Y1 O8 2.5358(14) . ? O1 C8 1.448(3) . ? O1 C1 1.450(2) . ? O2 C2 1.451(2) . ? O2 C3 1.452(3) . ? O3 C4 1.427(2) . ? O3 C5 1.427(3) . ? O4 C7 1.447(3) . ? O4 C6 1.454(3) . ? O5 C9 1.446(3) . ? O5 C16 1.448(2) . ? O6 C10 1.431(3) . ? O6 C11 1.435(2) . ? O7 C13 1.445(3) . ? O7 C12 1.449(3) . ? O8 C15 1.443(3) . ? O8 C14 1.447(2) . ? C1 C2 1.494(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.499(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.512(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.505(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.508(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? Al1 C19 2.010(2) . ? Al1 C21 2.015(2) . ? Al1 C18 2.021(2) . ? Al1 C20 2.031(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? Al2 C22 2.004(3) . ? Al2 C25 2.009(3) . ? Al2 C24 2.016(2) . ? Al2 C23 2.033(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Y1 C17 110.05(7) . . ? O5 Y1 O7 117.86(5) . . ? C17 Y1 O7 86.39(6) . . ? O5 Y1 O4 135.32(5) . . ? C17 Y1 O4 114.56(7) . . ? O7 Y1 O4 68.45(5) . . ? O5 Y1 O1 75.53(5) . . ? C17 Y1 O1 145.82(6) . . ? O7 Y1 O1 121.82(5) . . ? O4 Y1 O1 66.39(5) . . ? O5 Y1 O2 72.33(5) . . ? C17 Y1 O2 82.72(6) . . ? O7 Y1 O2 167.31(5) . . ? O4 Y1 O2 110.41(5) . . ? O1 Y1 O2 66.54(5) . . ? O5 Y1 O6 64.18(5) . . ? C17 Y1 O6 73.98(7) . . ? O7 Y1 O6 64.37(5) . . ? O4 Y1 O6 131.36(5) . . ? O1 Y1 O6 133.22(5) . . ? O2 Y1 O6 118.22(5) . . ? O5 Y1 O3 134.20(5) . . ? C17 Y1 O3 72.78(7) . . ? O7 Y1 O3 107.92(5) . . ? O4 Y1 O3 61.08(5) . . ? O1 Y1 O3 79.73(5) . . ? O2 Y1 O3 62.55(5) . . ? O6 Y1 O3 146.29(5) . . ? O5 Y1 O8 66.57(5) . . ? C17 Y1 O8 141.38(6) . . ? O7 Y1 O8 65.18(5) . . ? O4 Y1 O8 80.02(5) . . ? O1 Y1 O8 72.53(5) . . ? O2 Y1 O8 127.47(4) . . ? O6 Y1 O8 70.38(5) . . ? O3 Y1 O8 138.91(5) . . ? C8 O1 C1 114.21(16) . . ? C8 O1 Y1 113.92(11) . . ? C1 O1 Y1 119.74(12) . . ? C2 O2 C3 115.12(16) . . ? C2 O2 Y1 113.39(11) . . ? C3 O2 Y1 117.64(12) . . ? C4 O3 C5 114.52(17) . . ? C4 O3 Y1 125.08(13) . . ? C5 O3 Y1 120.13(12) . . ? C7 O4 C6 113.63(17) . . ? C7 O4 Y1 119.49(12) . . ? C6 O4 Y1 106.96(13) . . ? C9 O5 C16 116.36(17) . . ? C9 O5 Y1 112.57(12) . . ? C16 O5 Y1 116.82(13) . . ? C10 O6 C11 114.56(17) . . ? C10 O6 Y1 122.29(12) . . ? C11 O6 Y1 122.43(13) . . ? C13 O7 C12 116.17(16) . . ? C13 O7 Y1 116.41(11) . . ? C12 O7 Y1 113.97(12) . . ? C15 O8 C14 110.26(16) . . ? C15 O8 Y1 117.92(12) . . ? C14 O8 Y1 120.06(11) . . ? O1 C1 C2 106.39(17) . . ? O1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 111.46(17) . . ? O2 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? O2 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O2 C3 C4 111.44(18) . . ? O2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? O2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 106.74(18) . . ? O3 C4 H4A 110.4 . . ? C3 C4 H4A 110.4 . . ? O3 C4 H4B 110.4 . . ? C3 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? O3 C5 C6 105.43(18) . . ? O3 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? O3 C5 H5B 110.7 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? O4 C6 C5 109.20(17) . . ? O4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? O4 C7 C8 106.31(19) . . ? O4 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? O4 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? O1 C8 C7 109.59(17) . . ? O1 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O1 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O5 C9 C10 111.59(18) . . ? O5 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? O5 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O6 C10 C9 105.34(18) . . ? O6 C10 H10A 110.7 . . ? C9 C10 H10A 110.7 . . ? O6 C10 H10B 110.7 . . ? C9 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? O6 C11 C12 106.87(18) . . ? O6 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O6 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? O7 C12 C11 111.78(17) . . ? O7 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? O7 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? O7 C13 C14 111.09(18) . . ? O7 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? O7 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? O8 C14 C13 107.91(17) . . ? O8 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O8 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? O8 C15 C16 108.92(17) . . ? O8 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O8 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O5 C16 C15 111.35(16) . . ? O5 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? O5 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? Y1 C17 H17A 109.5 . . ? Y1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Y1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 Al1 C21 111.70(11) . . ? C19 Al1 C18 110.28(11) . . ? C21 Al1 C18 107.69(10) . . ? C19 Al1 C20 107.89(10) . . ? C21 Al1 C20 107.86(10) . . ? C18 Al1 C20 111.43(10) . . ? Al1 C18 H18A 109.5 . . ? Al1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al1 C19 H19A 109.5 . . ? Al1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al1 C20 H20A 109.5 . . ? Al1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 Al2 C25 107.34(12) . . ? C22 Al2 C24 108.13(11) . . ? C25 Al2 C24 111.48(11) . . ? C22 Al2 C23 111.63(10) . . ? C25 Al2 C23 108.08(10) . . ? C24 Al2 C23 110.17(10) . . ? Al2 C22 H22A 109.5 . . ? Al2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al2 C23 H23A 109.5 . . ? Al2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al2 C24 H24A 109.5 . . ? Al2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.415 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.066 #============================================================================== data_compound2 _database_code_depnum_ccdc_archive 'CCDC 764351' #TrackingRef 'compound1_6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H35 O8 Pr, 2(C4 H12 Al)' _chemical_formula_sum 'C25 H59 Al2 O8 Pr' _chemical_formula_weight 682.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.031(2) _cell_length_b 20.9866(15) _cell_length_c 14.514(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.581(15) _cell_angle_gamma 90.00 _cell_volume 3344.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 118 _cell_measurement_theta_min 3.052 _cell_measurement_theta_max 18.111 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_T_max 0.8360 _exptl_absorpt_process_details 'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87757 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9735 _reflns_number_gt 8163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _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^)+(0.0092P)^2^+3.2102P] 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 9735 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Pr1 Pr 0.252958(8) 0.067524(4) 0.165480(6) 0.01243(3) Uani 1 1 d . . . O1 O 0.11150(11) 0.13052(6) 0.26343(9) 0.0185(2) Uani 1 1 d . . . O2 O 0.02513(11) 0.06252(6) 0.10852(8) 0.0174(2) Uani 1 1 d . . . O3 O 0.16436(11) 0.15254(6) 0.04614(9) 0.0206(3) Uani 1 1 d . . . O4 O 0.30674(12) 0.18475(6) 0.19153(9) 0.0203(3) Uani 1 1 d . . . O5 O 0.17047(11) -0.01610(6) 0.26577(8) 0.0176(2) Uani 1 1 d . . . O6 O 0.38196(11) -0.03509(6) 0.19285(9) 0.0199(3) Uani 1 1 d . . . O7 O 0.48038(11) 0.08218(6) 0.19253(9) 0.0192(3) Uani 1 1 d . . . O8 O 0.35191(11) 0.06279(6) 0.33940(8) 0.0176(2) Uani 1 1 d . . . C1 C -0.01566(16) 0.13756(9) 0.23076(13) 0.0206(4) Uani 1 1 d . . . H1A H -0.0275 0.1748 0.1889 0.025 Uiso 1 1 calc R . . H1B H -0.0648 0.1440 0.2835 0.025 Uiso 1 1 calc R . . C2 C -0.05358(16) 0.07721(8) 0.17974(12) 0.0192(3) Uani 1 1 d . . . H2A H -0.0517 0.0414 0.2243 0.023 Uiso 1 1 calc R . . H2B H -0.1383 0.0818 0.1511 0.023 Uiso 1 1 calc R . . C3 C -0.01123(17) 0.08796(9) 0.01728(12) 0.0210(4) Uani 1 1 d . . . H3A H -0.1012 0.0904 0.0080 0.025 Uiso 1 1 calc R . . H3B H 0.0161 0.0587 -0.0300 0.025 Uiso 1 1 calc R . . C4 C 0.04156(17) 0.15338(9) 0.00396(13) 0.0217(4) Uani 1 1 d . . . H4A H 0.0400 0.1633 -0.0628 0.026 Uiso 1 1 calc R . . H4B H -0.0064 0.1861 0.0335 0.026 Uiso 1 1 calc R . . C5 C 0.23166(18) 0.20926(9) 0.03239(14) 0.0245(4) Uani 1 1 d . . . H5A H 0.1816 0.2474 0.0417 0.029 Uiso 1 1 calc R . . H5B H 0.2574 0.2104 -0.0311 0.029 Uiso 1 1 calc R . . C6 C 0.34151(18) 0.20720(9) 0.10334(14) 0.0245(4) Uani 1 1 d . . . H6A H 0.4039 0.1784 0.0816 0.029 Uiso 1 1 calc R . . H6B H 0.3774 0.2503 0.1110 0.029 Uiso 1 1 calc R . . C7 C 0.22406(17) 0.22628(9) 0.23433(14) 0.0235(4) Uani 1 1 d . . . H7A H 0.1604 0.2426 0.1874 0.028 Uiso 1 1 calc R . . H7B H 0.2687 0.2630 0.2639 0.028 Uiso 1 1 calc R . . C8 C 0.16750(18) 0.18722(9) 0.30571(13) 0.0231(4) Uani 1 1 d . . . H8A H 0.2308 0.1749 0.3556 0.028 Uiso 1 1 calc R . . H8B H 0.1052 0.2129 0.3336 0.028 Uiso 1 1 calc R . . C9 C 0.19976(17) -0.07988(8) 0.23705(14) 0.0228(4) Uani 1 1 d . . . H9A H 0.1592 -0.0878 0.1742 0.027 Uiso 1 1 calc R . . H9B H 0.1676 -0.1111 0.2797 0.027 Uiso 1 1 calc R . . C10 C 0.33518(17) -0.08997(8) 0.23622(13) 0.0220(4) Uani 1 1 d . . . H10A H 0.3743 -0.0946 0.3002 0.026 Uiso 1 1 calc R . . H10B H 0.3513 -0.1290 0.2011 0.026 Uiso 1 1 calc R . . C11 C 0.51255(17) -0.03314(9) 0.19596(14) 0.0234(4) Uani 1 1 d . . . H11A H 0.5422 -0.0683 0.1587 0.028 Uiso 1 1 calc R . . H11B H 0.5494 -0.0378 0.2606 0.028 Uiso 1 1 calc R . . C12 C 0.54727(17) 0.03034(9) 0.15710(13) 0.0223(4) Uani 1 1 d . . . H12A H 0.6355 0.0376 0.1728 0.027 Uiso 1 1 calc R . . H12B H 0.5315 0.0293 0.0888 0.027 Uiso 1 1 calc R . . C13 C 0.52719(17) 0.10899(9) 0.28045(13) 0.0220(4) Uani 1 1 d . . . H13A H 0.5030 0.1543 0.2827 0.026 Uiso 1 1 calc R . . H13B H 0.6173 0.1071 0.2863 0.026 Uiso 1 1 calc R . . C14 C 0.48040(16) 0.07388(9) 0.36084(13) 0.0216(4) Uani 1 1 d . . . H14A H 0.5238 0.0328 0.3710 0.026 Uiso 1 1 calc R . . H14B H 0.4947 0.0996 0.4180 0.026 Uiso 1 1 calc R . . C15 C 0.30768(18) 0.01604(9) 0.40064(12) 0.0232(4) Uani 1 1 d . . . H15A H 0.3072 0.0342 0.4636 0.028 Uiso 1 1 calc R . . H15B H 0.3618 -0.0217 0.4044 0.028 Uiso 1 1 calc R . . C16 C 0.18041(17) -0.00334(9) 0.36412(12) 0.0224(4) Uani 1 1 d . . . H16A H 0.1570 -0.0420 0.3972 0.027 Uiso 1 1 calc R . . H16B H 0.1230 0.0311 0.3767 0.027 Uiso 1 1 calc R . . C17 C 0.27914(18) 0.02500(10) 0.00894(13) 0.0252(4) Uani 1 1 d . . . H17A H 0.3050 -0.0196 0.0140 0.038 Uiso 1 1 calc R . . H17B H 0.3411 0.0500 -0.0190 0.038 Uiso 1 1 calc R . . H17C H 0.2016 0.0278 -0.0300 0.038 Uiso 1 1 calc R . . Al1 Al 0.17770(5) 0.08782(3) 0.63397(4) 0.01862(11) Uani 1 1 d . . . C18 C 0.13376(19) 0.11254(10) 0.76110(14) 0.0261(4) Uani 1 1 d . . . H18A H 0.0799 0.0801 0.7836 0.039 Uiso 1 1 calc R . . H18B H 0.0920 0.1538 0.7576 0.039 Uiso 1 1 calc R . . H18C H 0.2081 0.1157 0.8037 0.039 Uiso 1 1 calc R . . C19 C 0.05562(19) 0.12421(10) 0.53580(15) 0.0289(4) Uani 1 1 d . . . H19A H 0.0933 0.1285 0.4777 0.043 Uiso 1 1 calc R . . H19B H 0.0290 0.1662 0.5555 0.043 Uiso 1 1 calc R . . H19C H -0.0149 0.0957 0.5265 0.043 Uiso 1 1 calc R . . C20 C 0.34476(17) 0.12110(9) 0.60963(13) 0.0217(4) Uani 1 1 d . . . H20A H 0.3983 0.0851 0.5989 0.033 Uiso 1 1 calc R . . H20B H 0.3796 0.1455 0.6634 0.033 Uiso 1 1 calc R . . H20C H 0.3369 0.1487 0.5549 0.033 Uiso 1 1 calc R . . C21 C 0.18370(18) -0.00815(9) 0.62878(13) 0.0226(4) Uani 1 1 d . . . H21A H 0.1007 -0.0250 0.6181 0.034 Uiso 1 1 calc R . . H21B H 0.2225 -0.0246 0.6876 0.034 Uiso 1 1 calc R . . H21C H 0.2308 -0.0214 0.5782 0.034 Uiso 1 1 calc R . . Al2 Al 0.66939(5) 0.25318(3) 0.46191(4) 0.01875(11) Uani 1 1 d . . . C22 C 0.67975(19) 0.16866(10) 0.52701(15) 0.0288(4) Uani 1 1 d . . . H22A H 0.7479 0.1692 0.5757 0.043 Uiso 1 1 calc R . . H22B H 0.6928 0.1349 0.4824 0.043 Uiso 1 1 calc R . . H22C H 0.6037 0.1606 0.5547 0.043 Uiso 1 1 calc R . . C23 C 0.50399(17) 0.26729(9) 0.39090(14) 0.0246(4) Uani 1 1 d . . . H23A H 0.5113 0.2637 0.3244 0.037 Uiso 1 1 calc R . . H23B H 0.4741 0.3099 0.4047 0.037 Uiso 1 1 calc R . . H23C H 0.4466 0.2351 0.4094 0.037 Uiso 1 1 calc R . . C24 C 0.80173(18) 0.25564(10) 0.37523(14) 0.0269(4) Uani 1 1 d . . . H24A H 0.8737 0.2330 0.4034 0.040 Uiso 1 1 calc R . . H24B H 0.8232 0.3000 0.3636 0.040 Uiso 1 1 calc R . . H24C H 0.7725 0.2351 0.3166 0.040 Uiso 1 1 calc R . . C25 C 0.69422(19) 0.32088(10) 0.55991(16) 0.0331(5) Uani 1 1 d . . . H25A H 0.6313 0.3169 0.6028 0.050 Uiso 1 1 calc R . . H25B H 0.6887 0.3630 0.5307 0.050 Uiso 1 1 calc R . . H25C H 0.7748 0.3157 0.5940 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01327(4) 0.01180(4) 0.01226(4) 0.00033(3) 0.00140(3) 0.00125(4) O1 0.0168(6) 0.0187(6) 0.0198(6) -0.0047(5) 0.0007(5) 0.0023(5) O2 0.0162(6) 0.0207(6) 0.0152(6) 0.0002(5) 0.0009(4) 0.0003(5) O3 0.0191(6) 0.0175(6) 0.0243(7) 0.0061(5) -0.0026(5) 0.0006(5) O4 0.0197(6) 0.0148(6) 0.0261(7) -0.0001(5) 0.0009(5) 0.0019(5) O5 0.0177(6) 0.0175(6) 0.0173(6) 0.0021(5) -0.0003(5) -0.0014(5) O6 0.0201(6) 0.0161(6) 0.0238(6) 0.0051(5) 0.0037(5) 0.0040(5) O7 0.0158(6) 0.0204(6) 0.0217(6) -0.0006(5) 0.0033(5) 0.0015(5) O8 0.0163(6) 0.0208(6) 0.0156(6) 0.0007(5) 0.0002(4) -0.0010(5) C1 0.0152(8) 0.0248(9) 0.0220(9) -0.0025(7) 0.0017(7) 0.0052(7) C2 0.0143(8) 0.0239(9) 0.0198(8) 0.0002(7) 0.0038(6) 0.0000(7) C3 0.0188(9) 0.0287(9) 0.0147(8) 0.0011(7) -0.0029(7) 0.0006(7) C4 0.0188(9) 0.0269(9) 0.0187(8) 0.0051(7) -0.0012(7) 0.0063(7) C5 0.0246(9) 0.0186(9) 0.0307(10) 0.0093(7) 0.0055(8) -0.0001(7) C6 0.0234(9) 0.0168(8) 0.0337(10) 0.0065(8) 0.0053(8) -0.0017(7) C7 0.0224(9) 0.0146(8) 0.0331(10) -0.0074(7) -0.0002(8) 0.0038(7) C8 0.0233(9) 0.0221(9) 0.0231(9) -0.0090(7) -0.0009(7) 0.0041(7) C9 0.0227(9) 0.0155(8) 0.0292(10) 0.0020(7) -0.0029(8) -0.0044(7) C10 0.0263(10) 0.0133(8) 0.0261(9) 0.0038(7) 0.0001(8) 0.0006(7) C11 0.0192(9) 0.0228(9) 0.0284(10) 0.0012(7) 0.0041(7) 0.0076(7) C12 0.0178(9) 0.0250(9) 0.0251(9) -0.0006(7) 0.0076(7) 0.0041(7) C13 0.0171(8) 0.0218(9) 0.0265(9) -0.0029(7) -0.0014(7) -0.0014(7) C14 0.0150(8) 0.0287(10) 0.0203(8) -0.0028(7) -0.0031(6) 0.0004(7) C15 0.0267(10) 0.0289(10) 0.0136(8) 0.0038(7) 0.0009(7) -0.0037(8) C16 0.0244(9) 0.0273(9) 0.0161(8) 0.0044(7) 0.0049(7) -0.0030(7) C17 0.0263(10) 0.0290(10) 0.0202(9) -0.0018(8) 0.0023(8) 0.0077(8) Al1 0.0185(3) 0.0191(2) 0.0184(3) 0.0009(2) 0.0025(2) -0.0010(2) C18 0.0283(10) 0.0251(9) 0.0255(10) -0.0024(8) 0.0059(8) -0.0033(8) C19 0.0237(10) 0.0312(11) 0.0310(11) 0.0064(8) -0.0014(8) -0.0036(8) C20 0.0219(9) 0.0204(9) 0.0230(9) 0.0014(7) 0.0034(7) -0.0010(7) C21 0.0247(9) 0.0217(9) 0.0221(9) 0.0019(7) 0.0050(7) -0.0022(7) Al2 0.0172(3) 0.0164(2) 0.0224(3) -0.0009(2) 0.0011(2) -0.0006(2) C22 0.0251(10) 0.0278(10) 0.0320(11) 0.0094(8) -0.0049(8) -0.0035(8) C23 0.0219(9) 0.0208(9) 0.0305(10) -0.0011(8) -0.0007(8) 0.0016(7) C24 0.0236(10) 0.0296(10) 0.0275(10) 0.0033(8) 0.0025(8) 0.0018(8) C25 0.0216(10) 0.0336(11) 0.0436(13) -0.0157(10) 0.0012(9) -0.0030(8) _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 Pr1 C17 2.4838(19) . ? Pr1 O5 2.5068(12) . ? Pr1 O7 2.5200(13) . ? Pr1 O4 2.5503(12) . ? Pr1 O2 2.5702(13) . ? Pr1 O1 2.5758(12) . ? Pr1 O6 2.5904(12) . ? Pr1 O3 2.6095(12) . ? Pr1 O8 2.6528(13) . ? O1 C1 1.444(2) . ? O1 C8 1.449(2) . ? O2 C2 1.446(2) . ? O2 C3 1.448(2) . ? O3 C5 1.427(2) . ? O3 C4 1.431(2) . ? O4 C7 1.445(2) . ? O4 C6 1.450(2) . ? O5 C16 1.446(2) . ? O5 C9 1.448(2) . ? O6 C10 1.433(2) . ? O6 C11 1.437(2) . ? O7 C12 1.438(2) . ? O7 C13 1.443(2) . ? O8 C14 1.440(2) . ? O8 C15 1.440(2) . ? C1 C2 1.506(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.503(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.510(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.510(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.513(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? Al1 C19 2.013(2) . ? Al1 C21 2.0167(19) . ? Al1 C18 2.021(2) . ? Al1 C20 2.0335(19) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? Al2 C22 2.008(2) . ? Al2 C25 2.010(2) . ? Al2 C24 2.018(2) . ? Al2 C23 2.028(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pr1 O5 111.14(6) . . ? C17 Pr1 O7 89.07(6) . . ? O5 Pr1 O7 114.02(4) . . ? C17 Pr1 O4 115.86(6) . . ? O5 Pr1 O4 132.97(4) . . ? O7 Pr1 O4 69.23(4) . . ? C17 Pr1 O2 83.58(6) . . ? O5 Pr1 O2 76.08(4) . . ? O7 Pr1 O2 169.27(4) . . ? O4 Pr1 O2 107.05(4) . . ? C17 Pr1 O1 145.06(5) . . ? O5 Pr1 O1 76.42(4) . . ? O7 Pr1 O1 119.91(4) . . ? O4 Pr1 O1 64.39(4) . . ? O2 Pr1 O1 64.70(4) . . ? C17 Pr1 O6 74.37(5) . . ? O5 Pr1 O6 63.51(4) . . ? O7 Pr1 O6 63.50(4) . . ? O4 Pr1 O6 131.52(4) . . ? O2 Pr1 O6 121.38(4) . . ? O1 Pr1 O6 134.05(4) . . ? C17 Pr1 O3 73.02(5) . . ? O5 Pr1 O3 136.92(4) . . ? O7 Pr1 O3 108.84(4) . . ? O4 Pr1 O3 60.36(4) . . ? O2 Pr1 O3 61.51(4) . . ? O1 Pr1 O3 78.90(4) . . ? O6 Pr1 O3 146.60(4) . . ? C17 Pr1 O8 141.56(5) . . ? O5 Pr1 O8 63.91(4) . . ? O7 Pr1 O8 62.94(4) . . ? O4 Pr1 O8 80.03(4) . . ? O2 Pr1 O8 127.12(4) . . ? O1 Pr1 O8 73.10(4) . . ? O6 Pr1 O8 69.75(4) . . ? O3 Pr1 O8 138.60(4) . . ? C1 O1 C8 114.54(13) . . ? C1 O1 Pr1 119.52(10) . . ? C8 O1 Pr1 113.51(10) . . ? C2 O2 C3 116.29(13) . . ? C2 O2 Pr1 113.43(10) . . ? C3 O2 Pr1 117.02(10) . . ? C5 O3 C4 114.42(14) . . ? C5 O3 Pr1 119.79(11) . . ? C4 O3 Pr1 124.75(10) . . ? C7 O4 C6 114.56(14) . . ? C7 O4 Pr1 119.88(10) . . ? C6 O4 Pr1 105.08(10) . . ? C16 O5 C9 117.24(14) . . ? C16 O5 Pr1 116.53(10) . . ? C9 O5 Pr1 112.10(10) . . ? C10 O6 C11 114.32(13) . . ? C10 O6 Pr1 121.31(10) . . ? C11 O6 Pr1 121.00(10) . . ? C12 O7 C13 117.34(14) . . ? C12 O7 Pr1 112.94(10) . . ? C13 O7 Pr1 116.77(10) . . ? C14 O8 C15 111.22(13) . . ? C14 O8 Pr1 120.32(10) . . ? C15 O8 Pr1 118.68(10) . . ? O1 C1 C2 106.85(14) . . ? O1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 111.93(14) . . ? O2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? O2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? O2 C3 C4 112.09(14) . . ? O2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 107.13(14) . . ? O3 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O3 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? O3 C5 C6 105.90(14) . . ? O3 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? O3 C5 H5B 110.6 . . ? C6 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? O4 C6 C5 110.31(15) . . ? O4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O4 C7 C8 106.79(14) . . ? O4 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O4 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O1 C8 C7 110.14(15) . . ? O1 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O1 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O5 C9 C10 112.37(14) . . ? O5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? O5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? O6 C10 C9 106.84(14) . . ? O6 C10 H10A 110.4 . . ? C9 C10 H10A 110.4 . . ? O6 C10 H10B 110.4 . . ? C9 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? O6 C11 C12 107.64(14) . . ? O6 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O6 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O7 C12 C11 112.11(14) . . ? O7 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? O7 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O7 C13 C14 111.86(15) . . ? O7 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? O7 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? O8 C14 C13 108.33(14) . . ? O8 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? O8 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? O8 C15 C16 109.06(14) . . ? O8 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O8 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O5 C16 C15 112.07(14) . . ? O5 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? O5 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? Pr1 C17 H17A 109.5 . . ? Pr1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pr1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 Al1 C21 112.00(9) . . ? C19 Al1 C18 110.21(9) . . ? C21 Al1 C18 107.59(8) . . ? C19 Al1 C20 107.56(8) . . ? C21 Al1 C20 107.64(8) . . ? C18 Al1 C20 111.86(8) . . ? Al1 C18 H18A 109.5 . . ? Al1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al1 C19 H19A 109.5 . . ? Al1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al1 C20 H20A 109.5 . . ? Al1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 Al2 C25 107.09(10) . . ? C22 Al2 C24 107.72(9) . . ? C25 Al2 C24 111.47(9) . . ? C22 Al2 C23 112.05(8) . . ? C25 Al2 C23 108.08(9) . . ? C24 Al2 C23 110.42(9) . . ? Al2 C22 H22A 109.5 . . ? Al2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al2 C23 H23A 109.5 . . ? Al2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al2 C24 H24A 109.5 . . ? Al2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.655 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.081 #============================================================================== data_compound3 _database_code_depnum_ccdc_archive 'CCDC 764352' #TrackingRef 'compound1_6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H39 O7 Y, 2(C4 H12 Al, C4 H8 O) ' _chemical_formula_sum 'C31 H71 Al2 O8 Y' _chemical_formula_weight 714.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6170(3) _cell_length_b 11.1132(2) _cell_length_c 15.3071(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.9190(14) _cell_angle_gamma 90.00 _cell_volume 1968.90(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 46851 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7877 _exptl_absorpt_correction_T_max 0.9119 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40037 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8804 _reflns_number_gt 8109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Disorder of C1 and C10 on two positions (76:24) Disorder of C11 on two positions (63:37) Disorder of O8 on two positions (64:36) 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^)+(0.0362P)^2^+0.7411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(3) _refine_ls_number_reflns 8804 _refine_ls_number_parameters 387 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Y1 Y 0.671675(15) 0.86196(2) 0.716813(12) 0.02155(6) Uani 1 1 d . A . O1 O 0.77530(12) 0.8570(2) 0.58433(9) 0.0337(3) Uani 1 1 d . . . O2 O 0.85794(16) 0.96356(17) 0.72690(13) 0.0377(4) Uani 1 1 d . . . O3 O 0.68677(13) 1.05776(14) 0.79792(11) 0.0249(3) Uani 1 1 d . . . O4 O 0.48619(13) 0.94846(14) 0.74597(11) 0.0253(3) Uani 1 1 d . . . O5 O 0.57834(15) 0.97281(18) 0.59578(12) 0.0347(4) Uani 1 1 d . . . O6 O 0.81139(15) 0.70959(16) 0.75005(12) 0.0298(4) Uani 1 1 d . . . O7 O 0.64299(13) 0.81205(14) 0.86347(11) 0.0253(3) Uani 1 1 d . . . C1A C 0.8810(3) 0.9177(4) 0.5786(3) 0.0404(10) Uiso 0.755(6) 1 d P A 1 H1A1 H 0.8663 0.9982 0.5523 0.049 Uiso 0.755(6) 1 calc PR A 1 H1A2 H 0.9298 0.8719 0.5404 0.049 Uiso 0.755(6) 1 calc PR A 1 C1B C 0.9020(8) 0.8569(14) 0.5983(6) 0.030(2) Uiso 0.245(6) 1 d P A 2 H1B1 H 0.9292 0.7735 0.6101 0.037 Uiso 0.245(6) 1 calc PR A 2 H1B2 H 0.9345 0.8847 0.5441 0.037 Uiso 0.245(6) 1 calc PR A 2 C2 C 0.9431(2) 0.9310(3) 0.66828(18) 0.0402(7) Uani 1 1 d . A . H2A H 0.9809 0.8543 0.6871 0.048 Uiso 0.755(6) 1 calc PR A 1 H2B H 1.0030 0.9942 0.6679 0.048 Uiso 0.755(6) 1 calc PR A 1 H2C H 0.9746 1.0055 0.6441 0.048 Uiso 0.245(6) 1 calc PR A 2 H2D H 1.0075 0.8892 0.7023 0.048 Uiso 0.245(6) 1 calc PR A 2 C3 C 0.8892(2) 1.0533(2) 0.79231(19) 0.0307(6) Uani 1 1 d . A . H3A H 0.9577 1.0990 0.7770 0.037 Uiso 1 1 calc R . . H3B H 0.9069 1.0153 0.8504 0.037 Uiso 1 1 calc R . . C4 C 0.7864(2) 1.1344(2) 0.79337(18) 0.0311(5) Uani 1 1 d . A . H4A H 0.7951 1.1886 0.8448 0.037 Uiso 1 1 calc R . . H4B H 0.7781 1.1841 0.7395 0.037 Uiso 1 1 calc R . . C5 C 0.5830(2) 1.1271(2) 0.80481(17) 0.0289(5) Uani 1 1 d . A . H5A H 0.5660 1.1771 0.7517 0.035 Uiso 1 1 calc R . . H5B H 0.5920 1.1808 0.8566 0.035 Uiso 1 1 calc R . . C6 C 0.4874(2) 1.0383(2) 0.81408(17) 0.0280(5) Uani 1 1 d . A . H6A H 0.4985 0.9988 0.8722 0.034 Uiso 1 1 calc R . . H6B H 0.4123 1.0809 0.8103 0.034 Uiso 1 1 calc R . . C7 C 0.4067(2) 0.9692(2) 0.66887(17) 0.0306(5) Uani 1 1 d . A . H7A H 0.3408 1.0186 0.6849 0.037 Uiso 1 1 calc R . . H7B H 0.3760 0.8914 0.6456 0.037 Uiso 1 1 calc R . . C8 C 0.4688(2) 1.0336(2) 0.59925(18) 0.0316(6) Uani 1 1 d . A . H8A H 0.4231 1.0290 0.5417 0.038 Uiso 1 1 calc R . . H8B H 0.4810 1.1193 0.6150 0.038 Uiso 1 1 calc R . . C9 C 0.6241(2) 0.9750(3) 0.51077(17) 0.0346(6) Uani 1 1 d . A . H9A H 0.6712 1.0482 0.5047 0.042 Uiso 0.755(6) 1 calc PR A 1 H9B H 0.5602 0.9750 0.4636 0.042 Uiso 0.755(6) 1 calc PR A 1 H9C H 0.5993 1.0497 0.4793 0.042 Uiso 0.245(6) 1 calc PR A 2 H9D H 0.5938 0.9056 0.4754 0.042 Uiso 0.245(6) 1 calc PR A 2 C10A C 0.6979(3) 0.8632(4) 0.5045(2) 0.0338(8) Uiso 0.755(6) 1 d P A 1 H10A H 0.6485 0.7906 0.4989 0.041 Uiso 0.755(6) 1 calc PR A 1 H10B H 0.7429 0.8682 0.4526 0.041 Uiso 0.755(6) 1 calc PR A 1 C10B C 0.7521(9) 0.9695(10) 0.5223(7) 0.035(3) Uiso 0.245(6) 1 d P A 2 H10C H 0.7849 1.0437 0.5502 0.043 Uiso 0.245(6) 1 calc PR A 2 H10D H 0.7852 0.9574 0.4655 0.043 Uiso 0.245(6) 1 calc PR A 2 C11A C 0.8357(5) 0.6128(5) 0.6900(4) 0.0318(15) Uiso 0.627(16) 1 d P A 1 H11A H 0.8780 0.6434 0.6411 0.038 Uiso 0.627(16) 1 calc PR A 1 H11B H 0.7634 0.5737 0.6656 0.038 Uiso 0.627(16) 1 calc PR A 1 C11B C 0.8041(9) 0.5823(9) 0.7151(7) 0.038(3) Uiso 0.373(16) 1 d P A 2 H11C H 0.7371 0.5398 0.7364 0.045 Uiso 0.373(16) 1 calc PR A 2 H11D H 0.7960 0.5824 0.6502 0.045 Uiso 0.373(16) 1 calc PR A 2 C12 C 0.9107(3) 0.5247(3) 0.7475(2) 0.0546(9) Uani 1 1 d . . . H12A H 0.8630 0.4707 0.7810 0.065 Uiso 0.627(16) 1 calc PR A 1 H12B H 0.9609 0.4759 0.7122 0.065 Uiso 0.627(16) 1 calc PR A 1 H12C H 0.9553 0.5017 0.6978 0.065 Uiso 0.373(16) 1 calc PR A 2 H12D H 0.8938 0.4509 0.7802 0.065 Uiso 0.373(16) 1 calc PR A 2 C13 C 0.9804(3) 0.6111(3) 0.8071(2) 0.0507(8) Uani 1 1 d . A . H13A H 1.0137 0.5701 0.8609 0.061 Uiso 1 1 calc R . . H13B H 1.0435 0.6481 0.7768 0.061 Uiso 1 1 calc R . . C14 C 0.8930(3) 0.7025(3) 0.8277(2) 0.0355(6) Uani 1 1 d . A . H14A H 0.8533 0.6776 0.8795 0.043 Uiso 1 1 calc R . . H14B H 0.9303 0.7816 0.8402 0.043 Uiso 1 1 calc R . . C15 C 0.5546(2) 0.7241(2) 0.88380(18) 0.0334(6) Uani 1 1 d . A . H15A H 0.5707 0.6444 0.8586 0.040 Uiso 1 1 calc R . . H15B H 0.4769 0.7508 0.8599 0.040 Uiso 1 1 calc R . . C16 C 0.5616(3) 0.7176(3) 0.98302(19) 0.0419(7) Uani 1 1 d . . . H16A H 0.5492 0.6342 1.0030 0.050 Uiso 1 1 calc R A . H16B H 0.5033 0.7708 1.0066 0.050 Uiso 1 1 calc R . . C17 C 0.6833(3) 0.7601(3) 1.01182(19) 0.0486(8) Uani 1 1 d . A . H17A H 0.6882 0.7933 1.0720 0.058 Uiso 1 1 calc R . . H17B H 0.7401 0.6941 1.0091 0.058 Uiso 1 1 calc R . . C18 C 0.7017(2) 0.8557(3) 0.94587(15) 0.0367(5) Uani 1 1 d . A . H18A H 0.6681 0.9330 0.9632 0.044 Uiso 1 1 calc R . . H18B H 0.7852 0.8674 0.9400 0.044 Uiso 1 1 calc R . . C19 C 0.5570(2) 0.6952(2) 0.6592(2) 0.0373(6) Uani 1 1 d . . . H19A H 0.5665 0.6271 0.6999 0.056 Uiso 1 1 calc R A . H19B H 0.5822 0.6716 0.6022 0.056 Uiso 1 1 calc R . . H19C H 0.4754 0.7189 0.6521 0.056 Uiso 1 1 calc R . . Al1 Al 0.81244(6) 0.33777(7) 1.01376(5) 0.0348(2) Uani 1 1 d . . . C20 C 0.7001(2) 0.4225(2) 0.9270(2) 0.0413(7) Uani 1 1 d . . . H20A H 0.6228 0.4206 0.9481 0.062 Uiso 1 1 calc R . . H20B H 0.6983 0.3818 0.8701 0.062 Uiso 1 1 calc R . . H20C H 0.7244 0.5062 0.9206 0.062 Uiso 1 1 calc R . . C21 C 0.7605(3) 0.1667(3) 1.0312(2) 0.0412(7) Uani 1 1 d . . . H21A H 0.7606 0.1500 1.0940 0.062 Uiso 1 1 calc R . . H21B H 0.8134 0.1113 1.0050 0.062 Uiso 1 1 calc R . . H21C H 0.6823 0.1560 1.0029 0.062 Uiso 1 1 calc R . . C22 C 0.9697(2) 0.3347(3) 0.96724(19) 0.0428(7) Uani 1 1 d . . . H22A H 1.0101 0.4103 0.9821 0.064 Uiso 1 1 calc R . . H22B H 0.9609 0.3250 0.9034 0.064 Uiso 1 1 calc R . . H22C H 1.0146 0.2672 0.9936 0.064 Uiso 1 1 calc R . . C23 C 0.8162(3) 0.4255(3) 1.1283(2) 0.0547(9) Uani 1 1 d . . . H23A H 0.8419 0.5085 1.1204 0.082 Uiso 1 1 calc R . . H23B H 0.8698 0.3850 1.1717 0.082 Uiso 1 1 calc R . . H23C H 0.7386 0.4260 1.1490 0.082 Uiso 1 1 calc R . . Al2 Al 0.82039(6) 0.32363(7) 0.51281(5) 0.02960(17) Uani 1 1 d . . . C24 C 0.8393(2) 0.4982(3) 0.47911(18) 0.0332(6) Uani 1 1 d . . . H24A H 0.7789 0.5465 0.5030 0.050 Uiso 1 1 calc R . . H24B H 0.8330 0.5054 0.4151 0.050 Uiso 1 1 calc R . . H24C H 0.9154 0.5271 0.5029 0.050 Uiso 1 1 calc R . . C25 C 0.6703(2) 0.3030(3) 0.5683(2) 0.0395(6) Uani 1 1 d . . . H25A H 0.6719 0.2271 0.6009 0.059 Uiso 1 1 calc R . . H25B H 0.6060 0.3017 0.5224 0.059 Uiso 1 1 calc R . . H25C H 0.6600 0.3701 0.6084 0.059 Uiso 1 1 calc R . . C26 C 0.8231(3) 0.2181(3) 0.40548(19) 0.0410(7) Uani 1 1 d . . . H26A H 0.8155 0.2684 0.3527 0.061 Uiso 1 1 calc R . . H26B H 0.7587 0.1610 0.4037 0.061 Uiso 1 1 calc R . . H26C H 0.8962 0.1739 0.4080 0.061 Uiso 1 1 calc R . . C27 C 0.9519(3) 0.2721(3) 0.5995(2) 0.0451(7) Uani 1 1 d . . . H27A H 0.9241 0.2647 0.6579 0.068 Uiso 1 1 calc R . . H27B H 1.0137 0.3324 0.6010 0.068 Uiso 1 1 calc R . . H27C H 0.9818 0.1943 0.5816 0.068 Uiso 1 1 calc R . . O8A O 0.3670(3) 0.2830(3) 0.7032(3) 0.0323(11) Uiso 0.638(11) 1 d P B 1 O8B O 0.3725(5) 0.2793(5) 0.7471(6) 0.032(2) Uiso 0.362(11) 1 d P B 2 C28 C 0.4190(2) 0.3883(3) 0.7447(2) 0.0477(8) Uani 1 1 d . . . H28A H 0.4689 0.4278 0.7040 0.057 Uiso 0.638(11) 1 calc PR B 1 H28B H 0.4684 0.3638 0.7976 0.057 Uiso 0.638(11) 1 calc PR B 1 H28C H 0.4407 0.4063 0.6849 0.057 Uiso 0.362(11) 1 calc PR B 2 H28D H 0.4892 0.3931 0.7860 0.057 Uiso 0.362(11) 1 calc PR B 2 C29 C 0.3329(3) 0.4735(3) 0.7695(3) 0.0587(10) Uani 1 1 d . B . H29A H 0.3344 0.5476 0.7337 0.070 Uiso 1 1 calc R . . H29B H 0.3472 0.4955 0.8322 0.070 Uiso 1 1 calc R . . C30 C 0.2178(3) 0.4097(3) 0.7527(2) 0.0459(8) Uani 1 1 d . . . H30A H 0.1703 0.4474 0.7033 0.055 Uiso 1 1 calc R B . H30B H 0.1743 0.4115 0.8055 0.055 Uiso 1 1 calc R . . C31 C 0.2500(2) 0.2811(3) 0.7302(2) 0.0395(7) Uani 1 1 d . B . H31A H 0.2461 0.2283 0.7820 0.047 Uiso 0.638(11) 1 calc PR B 1 H31B H 0.1957 0.2497 0.6821 0.047 Uiso 0.638(11) 1 calc PR B 1 H31C H 0.2132 0.2224 0.7678 0.047 Uiso 0.362(11) 1 calc PR B 2 H31D H 0.2266 0.2626 0.6679 0.047 Uiso 0.362(11) 1 calc PR B 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 Y1 0.01983(9) 0.02261(9) 0.02228(9) -0.00069(10) 0.00221(6) 0.00130(10) O1 0.0271(7) 0.0501(10) 0.0241(7) 0.0004(11) 0.0048(6) 0.0066(11) O2 0.0297(10) 0.0372(11) 0.0482(11) -0.0104(9) 0.0152(8) -0.0078(8) O3 0.0217(8) 0.0226(8) 0.0304(9) -0.0024(7) 0.0027(7) 0.0001(6) O4 0.0205(8) 0.0251(8) 0.0305(9) -0.0008(7) 0.0024(7) 0.0035(6) O5 0.0262(9) 0.0497(11) 0.0287(9) 0.0123(8) 0.0051(7) 0.0091(8) O6 0.0296(9) 0.0299(9) 0.0287(9) -0.0081(7) -0.0042(7) 0.0082(7) O7 0.0234(8) 0.0264(8) 0.0261(9) 0.0026(6) 0.0030(6) -0.0012(6) C2 0.0221(12) 0.0628(19) 0.0371(15) -0.0021(13) 0.0096(11) 0.0083(12) C3 0.0255(13) 0.0310(14) 0.0350(15) 0.0001(11) -0.0001(11) -0.0039(10) C4 0.0265(12) 0.0241(12) 0.0424(15) 0.0002(11) 0.0006(10) -0.0061(10) C5 0.0270(12) 0.0229(12) 0.0368(14) -0.0035(10) 0.0024(10) 0.0061(9) C6 0.0266(12) 0.0275(12) 0.0307(13) -0.0031(10) 0.0071(10) 0.0048(9) C7 0.0195(11) 0.0364(14) 0.0354(14) 0.0029(11) -0.0015(10) 0.0006(10) C8 0.0241(12) 0.0360(14) 0.0341(14) 0.0073(11) -0.0015(10) 0.0056(10) C9 0.0313(13) 0.0463(16) 0.0265(13) 0.0081(11) 0.0041(10) -0.0002(11) C12 0.0541(19) 0.0420(18) 0.065(2) -0.0182(16) -0.0122(16) 0.0219(15) C13 0.0422(16) 0.0493(18) 0.058(2) -0.0075(16) -0.0086(14) 0.0170(14) C14 0.0384(15) 0.0326(14) 0.0337(15) 0.0002(12) -0.0067(12) 0.0080(12) C15 0.0286(13) 0.0323(13) 0.0400(15) 0.0088(11) 0.0056(11) -0.0046(10) C16 0.0507(17) 0.0393(15) 0.0386(16) 0.0050(12) 0.0210(13) 0.0027(13) C17 0.067(2) 0.0522(18) 0.0273(15) -0.0003(13) 0.0065(14) -0.0006(15) C18 0.0436(13) 0.0394(13) 0.0262(11) -0.0019(15) -0.0028(9) -0.0045(16) C19 0.0306(14) 0.0330(14) 0.0473(17) -0.0086(12) -0.0024(12) 0.0009(11) Al1 0.0267(3) 0.0353(5) 0.0414(4) -0.0059(3) -0.0029(3) 0.0008(3) C20 0.0313(14) 0.0267(13) 0.065(2) 0.0045(13) -0.0034(13) -0.0011(11) C21 0.0409(16) 0.0405(16) 0.0412(16) 0.0074(13) -0.0028(13) 0.0004(12) C22 0.0324(13) 0.054(2) 0.0411(15) 0.0022(13) -0.0031(11) 0.0005(12) C23 0.0411(17) 0.061(2) 0.061(2) -0.0207(17) -0.0047(15) 0.0044(15) Al2 0.0236(3) 0.0347(4) 0.0310(4) -0.0031(3) 0.0053(3) -0.0019(3) C24 0.0259(12) 0.0406(15) 0.0333(14) 0.0010(11) 0.0039(10) -0.0022(11) C25 0.0346(14) 0.0398(15) 0.0462(17) 0.0009(13) 0.0150(12) -0.0033(12) C26 0.0410(16) 0.0475(17) 0.0354(16) -0.0093(13) 0.0092(12) -0.0067(13) C27 0.0433(16) 0.0446(16) 0.0463(18) -0.0090(14) -0.0023(13) 0.0085(13) C28 0.0314(13) 0.055(2) 0.0563(19) -0.0207(15) 0.0021(12) -0.0007(12) C29 0.0456(19) 0.0325(16) 0.100(3) -0.0038(17) 0.019(2) 0.0023(14) C30 0.0363(16) 0.0486(17) 0.054(2) 0.0108(14) 0.0099(14) 0.0141(13) C31 0.0305(14) 0.0440(16) 0.0434(17) 0.0020(13) 0.0000(12) 0.0017(12) _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 Y1 O7 2.3636(16) . ? Y1 O6 2.3704(17) . ? Y1 O5 2.4043(17) . ? Y1 C19 2.405(3) . ? Y1 O2 2.4338(18) . ? Y1 O4 2.4354(15) . ? Y1 O1 2.4460(14) . ? Y1 O3 2.5039(16) . ? O1 C1A 1.411(4) . ? O1 C10A 1.455(3) . ? O1 C1B 1.469(9) . ? O1 C10B 1.579(11) . ? O2 C3 1.437(3) . ? O2 C2 1.438(3) . ? O3 C5 1.443(3) . ? O3 C4 1.443(3) . ? O4 C6 1.443(3) . ? O4 C7 1.453(3) . ? O5 C8 1.446(3) . ? O5 C9 1.447(3) . ? O6 C11A 1.458(5) . ? O6 C14 1.458(3) . ? O6 C11B 1.512(9) . ? O7 C18 1.464(3) . ? O7 C15 1.471(3) . ? C1A C2 1.502(5) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C1B C2 1.402(11) . ? C1B H1B1 0.9900 . ? C1B H1B2 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.497(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.502(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.516(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10B 1.484(11) . ? C9 C10A 1.517(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 H9C 0.9900 . ? C9 H9D 0.9900 . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11A C12 1.536(6) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C11B C12 1.443(8) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12 C13 1.510(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? C13 C14 1.490(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.516(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.520(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.493(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Al1 C23 2.004(3) . ? Al1 C20 2.014(3) . ? Al1 C22 2.017(3) . ? Al1 C21 2.019(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Al2 C25 2.017(3) . ? Al2 C27 2.018(3) . ? Al2 C26 2.021(3) . ? Al2 C24 2.024(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O8A C28 1.440(4) . ? O8A C31 1.454(4) . ? O8B C28 1.328(6) . ? O8B C31 1.425(6) . ? C28 C29 1.451(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 H28C 0.9900 . ? C28 H28D 0.9900 . ? C29 C30 1.516(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.524(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 H31C 0.9900 . ? C31 H31D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Y1 O6 77.19(6) . . ? O7 Y1 O5 139.56(6) . . ? O6 Y1 O5 141.87(6) . . ? O7 Y1 C19 92.78(9) . . ? O6 Y1 C19 82.87(8) . . ? O5 Y1 C19 85.03(9) . . ? O7 Y1 O2 104.22(6) . . ? O6 Y1 O2 74.28(7) . . ? O5 Y1 O2 98.68(7) . . ? C19 Y1 O2 147.38(8) . . ? O7 Y1 O4 73.71(6) . . ? O6 Y1 O4 147.45(6) . . ? O5 Y1 O4 65.88(6) . . ? C19 Y1 O4 84.27(8) . . ? O2 Y1 O4 126.95(6) . . ? O7 Y1 O1 154.36(6) . . ? O6 Y1 O1 77.59(7) . . ? O5 Y1 O1 66.07(6) . . ? C19 Y1 O1 88.58(9) . . ? O2 Y1 O1 64.22(6) . . ? O4 Y1 O1 131.83(6) . . ? O7 Y1 O3 75.08(5) . . ? O6 Y1 O3 119.79(6) . . ? O5 Y1 O3 86.82(6) . . ? C19 Y1 O3 149.80(8) . . ? O2 Y1 O3 62.70(6) . . ? O4 Y1 O3 65.89(5) . . ? O1 Y1 O3 114.35(7) . . ? C1A O1 C10A 113.8(3) . . ? C1A O1 C1B 31.0(5) . . ? C10A O1 C1B 131.4(4) . . ? C1A O1 C10B 71.8(4) . . ? C10A O1 C10B 52.9(5) . . ? C1B O1 C10B 101.8(7) . . ? C1A O1 Y1 122.24(19) . . ? C10A O1 Y1 112.48(14) . . ? C1B O1 Y1 115.9(4) . . ? C10B O1 Y1 114.2(4) . . ? C3 O2 C2 117.6(2) . . ? C3 O2 Y1 122.40(15) . . ? C2 O2 Y1 119.94(17) . . ? C5 O3 C4 111.53(17) . . ? C5 O3 Y1 118.50(13) . . ? C4 O3 Y1 120.74(14) . . ? C6 O4 C7 116.30(18) . . ? C6 O4 Y1 116.87(13) . . ? C7 O4 Y1 115.12(13) . . ? C8 O5 C9 114.66(19) . . ? C8 O5 Y1 123.45(14) . . ? C9 O5 Y1 121.70(14) . . ? C11A O6 C14 109.1(2) . . ? C11A O6 C11B 25.1(4) . . ? C14 O6 C11B 104.5(4) . . ? C11A O6 Y1 123.9(2) . . ? C14 O6 Y1 126.79(15) . . ? C11B O6 Y1 125.2(3) . . ? C18 O7 C15 108.68(19) . . ? C18 O7 Y1 130.33(15) . . ? C15 O7 Y1 120.99(14) . . ? O1 C1A C2 110.0(3) . . ? O1 C1A H1A1 109.7 . . ? C2 C1A H1A1 109.7 . . ? O1 C1A H1A2 109.7 . . ? C2 C1A H1A2 109.7 . . ? H1A1 C1A H1A2 108.2 . . ? C2 C1B O1 112.5(7) . . ? C2 C1B H1B1 109.1 . . ? O1 C1B H1B1 109.1 . . ? C2 C1B H1B2 109.1 . . ? O1 C1B H1B2 109.1 . . ? H1B1 C1B H1B2 107.8 . . ? C1B C2 O2 114.7(4) . . ? C1B C2 C1A 30.5(5) . . ? O2 C2 C1A 107.1(2) . . ? C1B C2 H2A 80.2 . . ? O2 C2 H2A 110.3 . . ? C1A C2 H2A 110.3 . . ? C1B C2 H2B 127.3 . . ? O2 C2 H2B 110.3 . . ? C1A C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? C1B C2 H2C 108.6 . . ? O2 C2 H2C 108.6 . . ? C1A C2 H2C 84.6 . . ? H2A C2 H2C 131.3 . . ? H2B C2 H2C 28.4 . . ? C1B C2 H2D 108.6 . . ? O2 C2 H2D 108.6 . . ? C1A C2 H2D 135.8 . . ? H2A C2 H2D 31.5 . . ? H2B C2 H2D 80.6 . . ? H2C C2 H2D 107.6 . . ? O2 C3 C4 105.7(2) . . ? O2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O3 C4 C3 106.8(2) . . ? O3 C4 H4A 110.4 . . ? C3 C4 H4A 110.4 . . ? O3 C4 H4B 110.4 . . ? C3 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? O3 C5 C6 106.57(18) . . ? O3 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O3 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? O4 C6 C5 110.35(19) . . ? O4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O4 C7 C8 109.75(19) . . ? O4 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O4 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O5 C8 C7 106.2(2) . . ? O5 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O5 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? O5 C9 C10B 109.5(5) . . ? O5 C9 C10A 107.2(2) . . ? C10B C9 C10A 53.6(5) . . ? O5 C9 H9A 110.3 . . ? C10B C9 H9A 59.2 . . ? C10A C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10B C9 H9B 140.1 . . ? C10A C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? O5 C9 H9C 109.8 . . ? C10B C9 H9C 109.8 . . ? C10A C9 H9C 142.9 . . ? H9A C9 H9C 53.5 . . ? H9B C9 H9C 58.5 . . ? O5 C9 H9D 109.8 . . ? C10B C9 H9D 109.8 . . ? C10A C9 H9D 60.2 . . ? H9A C9 H9D 139.8 . . ? H9B C9 H9D 52.6 . . ? H9C C9 H9D 108.2 . . ? O1 C10A C9 107.4(3) . . ? O1 C10A H10A 110.2 . . ? C9 C10A H10A 110.2 . . ? O1 C10A H10B 110.2 . . ? C9 C10A H10B 110.2 . . ? H10A C10A H10B 108.5 . . ? C9 C10B O1 102.8(7) . . ? C9 C10B H10C 111.2 . . ? O1 C10B H10C 111.2 . . ? C9 C10B H10D 111.2 . . ? O1 C10B H10D 111.2 . . ? H10C C10B H10D 109.1 . . ? O6 C11A C12 103.9(3) . . ? O6 C11A H11A 111.0 . . ? C12 C11A H11A 111.0 . . ? O6 C11A H11B 111.0 . . ? C12 C11A H11B 111.0 . . ? H11A C11A H11B 109.0 . . ? C12 C11B O6 105.8(5) . . ? C12 C11B H11C 110.6 . . ? O6 C11B H11C 110.6 . . ? C12 C11B H11D 110.6 . . ? O6 C11B H11D 110.6 . . ? H11C C11B H11D 108.7 . . ? C11B C12 C13 109.0(4) . . ? C11B C12 C11A 24.9(4) . . ? C13 C12 C11A 100.9(3) . . ? C11B C12 H12A 86.9 . . ? C13 C12 H12A 111.6 . . ? C11A C12 H12A 111.6 . . ? C11B C12 H12B 125.6 . . ? C13 C12 H12B 111.6 . . ? C11A C12 H12B 111.6 . . ? H12A C12 H12B 109.4 . . ? C11B C12 H12C 109.9 . . ? C13 C12 H12C 109.9 . . ? C11A C12 H12C 91.9 . . ? H12A C12 H12C 126.4 . . ? H12B C12 H12C 21.2 . . ? C11B C12 H12D 109.9 . . ? C13 C12 H12D 109.9 . . ? C11A C12 H12D 133.7 . . ? H12A C12 H12D 24.6 . . ? H12B C12 H12D 88.5 . . ? H12C C12 H12D 108.3 . . ? C14 C13 C12 102.8(2) . . ? C14 C13 H13A 111.2 . . ? C12 C13 H13A 111.2 . . ? C14 C13 H13B 111.2 . . ? C12 C13 H13B 111.2 . . ? H13A C13 H13B 109.1 . . ? O6 C14 C13 105.7(2) . . ? O6 C14 H14A 110.6 . . ? C13 C14 H14A 110.6 . . ? O6 C14 H14B 110.6 . . ? C13 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? O7 C15 C16 105.4(2) . . ? O7 C15 H15A 110.7 . . ? C16 C15 H15A 110.7 . . ? O7 C15 H15B 110.7 . . ? C16 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C15 C16 C17 104.1(2) . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16B 110.9 . . ? C17 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? C18 C17 C16 102.1(2) . . ? C18 C17 H17A 111.4 . . ? C16 C17 H17A 111.4 . . ? C18 C17 H17B 111.4 . . ? C16 C17 H17B 111.4 . . ? H17A C17 H17B 109.2 . . ? O7 C18 C17 105.3(3) . . ? O7 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? O7 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? Y1 C19 H19A 109.5 . . ? Y1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Y1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 Al1 C20 108.29(14) . . ? C23 Al1 C22 111.41(13) . . ? C20 Al1 C22 109.31(13) . . ? C23 Al1 C21 109.08(15) . . ? C20 Al1 C21 110.06(12) . . ? C22 Al1 C21 108.69(13) . . ? Al1 C20 H20A 109.5 . . ? Al1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Al1 C22 H22A 109.5 . . ? Al1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al1 C23 H23A 109.5 . . ? Al1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 Al2 C27 108.91(14) . . ? C25 Al2 C26 110.50(13) . . ? C27 Al2 C26 107.84(13) . . ? C25 Al2 C24 109.46(12) . . ? C27 Al2 C24 110.27(13) . . ? C26 Al2 C24 109.83(12) . . ? Al2 C24 H24A 109.5 . . ? Al2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Al2 C26 H26A 109.5 . . ? Al2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Al2 C27 H27A 109.5 . . ? Al2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 O8A C31 104.7(3) . . ? C28 O8B C31 112.6(4) . . ? O8B C28 O8A 27.7(3) . . ? O8B C28 C29 107.3(3) . . ? O8A C28 C29 111.9(3) . . ? O8B C28 H28A 133.2 . . ? O8A C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? O8B C28 H28B 86.2 . . ? O8A C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? O8B C28 H28C 110.3 . . ? O8A C28 H28C 83.5 . . ? C29 C28 H28C 110.3 . . ? H28A C28 H28C 28.3 . . ? H28B C28 H28C 129.5 . . ? O8B C28 H28D 110.3 . . ? O8A C28 H28D 128.1 . . ? C29 C28 H28D 110.3 . . ? H28A C28 H28D 83.2 . . ? H28B C28 H28D 26.4 . . ? H28C C28 H28D 108.5 . . ? C28 C29 C30 105.5(3) . . ? C28 C29 H29A 110.6 . . ? C30 C29 H29A 110.6 . . ? C28 C29 H29B 110.6 . . ? C30 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C31 104.3(3) . . ? C29 C30 H30A 110.9 . . ? C31 C30 H30A 110.9 . . ? C29 C30 H30B 110.9 . . ? C31 C30 H30B 110.9 . . ? H30A C30 H30B 108.9 . . ? O8B C31 O8A 27.0(3) . . ? O8B C31 C30 103.4(3) . . ? O8A C31 C30 107.7(3) . . ? O8B C31 H31A 87.7 . . ? O8A C31 H31A 110.2 . . ? C30 C31 H31A 110.2 . . ? O8B C31 H31B 133.9 . . ? O8A C31 H31B 110.2 . . ? C30 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? O8B C31 H31C 111.1 . . ? O8A C31 H31C 129.5 . . ? C30 C31 H31C 111.1 . . ? H31A C31 H31C 25.0 . . ? H31B C31 H31C 85.5 . . ? O8B C31 H31D 111.1 . . ? O8A C31 H31D 85.1 . . ? C30 C31 H31D 111.1 . . ? H31A C31 H31D 128.4 . . ? H31B C31 H31D 26.8 . . ? H31C C31 H31D 109.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.416 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.055 #============================================================================== data_compound4 _database_code_depnum_ccdc_archive 'CCDC 764353' #TrackingRef 'compound1_6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 O10 Pr, 3(C4 H12 Al)' _chemical_formula_sum 'C32 H76 Al3 O10 Pr' _chemical_formula_weight 842.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 22.697(4) _cell_length_b 11.4073(7) _cell_length_c 16.757(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4338.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 138 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7653 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details 'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93846 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.99 _reflns_number_total 12629 _reflns_number_gt 9884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; racemic twin BASF 0.40544 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^)+(0.0370P)^2^+4.0392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.405(9) _chemical_absolute_configuration 'merohedral twin' _refine_ls_number_reflns 12629 _refine_ls_number_parameters 428 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 Pr1 Pr 0.124524(7) 0.236153(10) 0.799816(17) 0.01248(4) Uani 1 1 d . . . Al1 Al 0.11863(4) 0.72722(9) 0.54880(8) 0.0229(2) Uani 1 1 d . . . Al2 Al 0.34708(5) 0.23965(8) 0.57840(7) 0.0186(2) Uani 1 1 d . . . Al3 Al 0.37475(4) 0.74966(6) 0.7941(2) 0.0191(3) Uani 1 1 d . . . O1 O 0.06653(9) 0.43290(18) 0.8063(2) 0.0312(6) Uani 1 1 d . . . O2 O 0.01453(9) 0.23224(18) 0.76272(14) 0.0198(5) Uani 1 1 d . . . O3 O 0.07577(9) 0.03418(18) 0.77993(13) 0.0192(5) Uani 1 1 d . . . O4 O 0.08846(10) 0.1151(2) 0.92650(13) 0.0228(5) Uani 1 1 d . . . O5 O 0.10910(12) 0.3452(3) 0.94036(17) 0.0270(7) Uani 1 1 d . . . O6 O 0.12277(10) 0.3606(3) 0.66915(16) 0.0201(6) Uani 1 1 d . . . O7 O 0.13938(11) 0.1374(2) 0.65930(14) 0.0239(5) Uani 1 1 d . . . O8 O 0.20184(9) 0.06796(17) 0.78372(13) 0.0188(5) Uani 1 1 d . . . O9 O 0.21285(9) 0.23426(18) 0.89252(13) 0.0171(4) Uani 1 1 d . . . O10 O 0.19985(9) 0.39579(17) 0.78516(13) 0.0196(5) Uani 1 1 d . . . C1 C 0.01178(15) 0.4396(3) 0.7623(2) 0.0283(8) Uani 1 1 d . . . H1A H 0.0201 0.4469 0.7045 0.034 Uiso 1 1 calc R . . H1B H -0.0108 0.5094 0.7794 0.034 Uiso 1 1 calc R . . C2 C -0.02330(14) 0.3313(3) 0.7775(2) 0.0251(8) Uani 1 1 d . . . H2A H -0.0374 0.3302 0.8335 0.030 Uiso 1 1 calc R . . H2B H -0.0580 0.3287 0.7417 0.030 Uiso 1 1 calc R . . C3 C -0.01905(14) 0.1245(3) 0.7613(2) 0.0244(7) Uani 1 1 d . . . H3A H -0.0526 0.1315 0.7238 0.029 Uiso 1 1 calc R . . H3B H -0.0347 0.1068 0.8151 0.029 Uiso 1 1 calc R . . C4 C 0.02173(15) 0.0301(3) 0.7348(2) 0.0262(8) Uani 1 1 d . . . H4A H 0.0026 -0.0472 0.7423 0.031 Uiso 1 1 calc R . . H4B H 0.0305 0.0398 0.6773 0.031 Uiso 1 1 calc R . . C5 C 0.08185(15) -0.0498(3) 0.8435(2) 0.0234(7) Uani 1 1 d . . . H5A H 0.1237 -0.0725 0.8492 0.028 Uiso 1 1 calc R . . H5B H 0.0588 -0.1211 0.8308 0.028 Uiso 1 1 calc R . . C6 C 0.06041(15) 0.0020(3) 0.9191(2) 0.0243(7) Uani 1 1 d . . . H6A H 0.0170 0.0109 0.9179 0.029 Uiso 1 1 calc R . . H6B H 0.0711 -0.0487 0.9649 0.029 Uiso 1 1 calc R . . C7 C 0.07642(17) 0.1667(3) 1.0029(2) 0.0315(8) Uani 1 1 d . . . H7A H 0.0841 0.1094 1.0460 0.038 Uiso 1 1 calc R . . H7B H 0.0347 0.1917 1.0060 0.038 Uiso 1 1 calc R . . C8 C 0.11640(17) 0.2701(4) 1.0110(2) 0.0282(9) Uani 1 1 d . . . H8A H 0.1064 0.3146 1.0599 0.034 Uiso 1 1 calc R . . H8B H 0.1578 0.2436 1.0152 0.034 Uiso 1 1 calc R . . C9 C 0.06660(17) 0.4344(4) 0.9497(2) 0.0356(10) Uani 1 1 d . . . H9A H 0.0750 0.4816 0.9979 0.043 Uiso 1 1 calc R . . H9B H 0.0267 0.4003 0.9548 0.043 Uiso 1 1 calc R . . C10 C 0.07067(17) 0.5084(3) 0.8767(2) 0.0336(9) Uani 1 1 d . . . H10A H 0.0383 0.5666 0.8762 0.040 Uiso 1 1 calc R . . H10B H 0.1086 0.5513 0.8763 0.040 Uiso 1 1 calc R . . C11 C 0.09981(18) 0.3031(3) 0.5994(2) 0.0243(8) Uani 1 1 d . . . H11A H 0.1021 0.3565 0.5530 0.029 Uiso 1 1 calc R . . H11B H 0.0579 0.2823 0.6080 0.029 Uiso 1 1 calc R . . C12 C 0.13481(17) 0.1951(3) 0.5835(2) 0.0276(8) Uani 1 1 d . . . H12A H 0.1145 0.1444 0.5442 0.033 Uiso 1 1 calc R . . H12B H 0.1743 0.2153 0.5626 0.033 Uiso 1 1 calc R . . C13 C 0.16628(15) 0.0229(3) 0.6540(2) 0.0246(7) Uani 1 1 d . . . H13A H 0.1786 0.0075 0.5983 0.030 Uiso 1 1 calc R . . H13B H 0.1375 -0.0380 0.6697 0.030 Uiso 1 1 calc R . . C14 C 0.21836(15) 0.0183(3) 0.7077(2) 0.0250(7) Uani 1 1 d . . . H14A H 0.2313 -0.0639 0.7148 0.030 Uiso 1 1 calc R . . H14B H 0.2514 0.0634 0.6842 0.030 Uiso 1 1 calc R . . C15 C 0.24923(14) 0.0533(3) 0.8404(2) 0.0218(7) Uani 1 1 d . . . H15A H 0.2864 0.0857 0.8186 0.026 Uiso 1 1 calc R . . H15B H 0.2553 -0.0309 0.8523 0.026 Uiso 1 1 calc R . . C16 C 0.23205(15) 0.1170(3) 0.9136(2) 0.0246(7) Uani 1 1 d . . . H16A H 0.1997 0.0747 0.9409 0.030 Uiso 1 1 calc R . . H16B H 0.2660 0.1214 0.9506 0.030 Uiso 1 1 calc R . . C17 C 0.26091(14) 0.3139(3) 0.8844(2) 0.0226(7) Uani 1 1 d . . . H17A H 0.2910 0.2808 0.8481 0.027 Uiso 1 1 calc R . . H17B H 0.2795 0.3278 0.9370 0.027 Uiso 1 1 calc R . . C18 C 0.23773(15) 0.4262(3) 0.8514(2) 0.0232(7) Uani 1 1 d . . . H18A H 0.2152 0.4691 0.8927 0.028 Uiso 1 1 calc R . . H18B H 0.2706 0.4765 0.8330 0.028 Uiso 1 1 calc R . . C19 C 0.19311(17) 0.4882(3) 0.7273(2) 0.0275(8) Uani 1 1 d . . . H19A H 0.2310 0.5293 0.7192 0.033 Uiso 1 1 calc R . . H19B H 0.1635 0.5458 0.7459 0.033 Uiso 1 1 calc R . . C20 C 0.17343(16) 0.4328(3) 0.6519(2) 0.0260(8) Uani 1 1 d . . . H20A H 0.1629 0.4938 0.6124 0.031 Uiso 1 1 calc R . . H20B H 0.2055 0.3842 0.6294 0.031 Uiso 1 1 calc R . . C21 C 0.06247(18) 0.6964(4) 0.6388(3) 0.0451(11) Uani 1 1 d . . . H21A H 0.0588 0.7670 0.6717 0.068 Uiso 1 1 calc R . . H21B H 0.0774 0.6317 0.6715 0.068 Uiso 1 1 calc R . . H21C H 0.0238 0.6755 0.6171 0.068 Uiso 1 1 calc R . . C22 C 0.09364(16) 0.8746(3) 0.4914(2) 0.0327(9) Uani 1 1 d . . . H22A H 0.1283 0.9122 0.4676 0.049 Uiso 1 1 calc R . . H22B H 0.0751 0.9285 0.5294 0.049 Uiso 1 1 calc R . . H22C H 0.0654 0.8546 0.4492 0.049 Uiso 1 1 calc R . . C23 C 0.11481(16) 0.5958(3) 0.4677(2) 0.0297(8) Uani 1 1 d . . . H23A H 0.0748 0.5634 0.4664 0.045 Uiso 1 1 calc R . . H23B H 0.1427 0.5340 0.4827 0.045 Uiso 1 1 calc R . . H23C H 0.1251 0.6263 0.4149 0.045 Uiso 1 1 calc R . . C24 C 0.20041(16) 0.7403(3) 0.5962(2) 0.0229(7) Uani 1 1 d . . . H24A H 0.2212 0.8065 0.5717 0.034 Uiso 1 1 calc R . . H24B H 0.2223 0.6678 0.5859 0.034 Uiso 1 1 calc R . . H24C H 0.1974 0.7530 0.6539 0.034 Uiso 1 1 calc R . . C25 C 0.31449(16) 0.3794(3) 0.5209(2) 0.0287(8) Uani 1 1 d . . . H25A H 0.3299 0.4513 0.5453 0.043 Uiso 1 1 calc R . . H25B H 0.2714 0.3790 0.5247 0.043 Uiso 1 1 calc R . . H25C H 0.3263 0.3764 0.4647 0.043 Uiso 1 1 calc R . . C26 C 0.30992(15) 0.0956(3) 0.5318(2) 0.0275(8) Uani 1 1 d . . . H26A H 0.2669 0.1039 0.5328 0.041 Uiso 1 1 calc R . . H26B H 0.3214 0.0270 0.5633 0.041 Uiso 1 1 calc R . . H26C H 0.3232 0.0856 0.4766 0.041 Uiso 1 1 calc R . . C27 C 0.43528(15) 0.2318(3) 0.5631(2) 0.0262(7) Uani 1 1 d . . . H27A H 0.4443 0.2239 0.5062 0.039 Uiso 1 1 calc R . . H27B H 0.4510 0.1641 0.5921 0.039 Uiso 1 1 calc R . . H27C H 0.4534 0.3037 0.5838 0.039 Uiso 1 1 calc R . . C28 C 0.32724(15) 0.2579(3) 0.69401(19) 0.0200(7) Uani 1 1 d . . . H28A H 0.3434 0.3321 0.7138 0.030 Uiso 1 1 calc R . . H28B H 0.3442 0.1926 0.7243 0.030 Uiso 1 1 calc R . . H28C H 0.2843 0.2579 0.7006 0.030 Uiso 1 1 calc R . . C29 C 0.37530(16) 0.8980(3) 0.7295(2) 0.0258(7) Uani 1 1 d . . . H29A H 0.3416 0.8982 0.6930 0.039 Uiso 1 1 calc R . . H29B H 0.4119 0.9025 0.6987 0.039 Uiso 1 1 calc R . . H29C H 0.3726 0.9657 0.7654 0.039 Uiso 1 1 calc R . . C30 C 0.44803(17) 0.7464(3) 0.8626(2) 0.0301(9) Uani 1 1 d . . . H30A H 0.4468 0.8114 0.9008 0.045 Uiso 1 1 calc R . . H30B H 0.4829 0.7541 0.8286 0.045 Uiso 1 1 calc R . . H30C H 0.4499 0.6719 0.8917 0.045 Uiso 1 1 calc R . . C31 C 0.30457(18) 0.7390(3) 0.8674(2) 0.0322(9) Uani 1 1 d . . . H31A H 0.3062 0.6652 0.8973 0.048 Uiso 1 1 calc R . . H31B H 0.2683 0.7415 0.8357 0.048 Uiso 1 1 calc R . . H31C H 0.3051 0.8051 0.9047 0.048 Uiso 1 1 calc R . . C32 C 0.37435(17) 0.6118(3) 0.7196(2) 0.0299(8) Uani 1 1 d . . . H32A H 0.3705 0.5393 0.7505 0.045 Uiso 1 1 calc R . . H32B H 0.4113 0.6102 0.6894 0.045 Uiso 1 1 calc R . . H32C H 0.3411 0.6188 0.6827 0.045 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 Pr1 0.00910(6) 0.01457(6) 0.01378(6) -0.0005(2) -0.00091(7) -0.00006(5) Al1 0.0206(6) 0.0250(5) 0.0231(5) 0.0055(5) 0.0042(4) 0.0036(4) Al2 0.0166(6) 0.0235(5) 0.0156(5) 0.0000(4) 0.0011(4) 0.0002(4) Al3 0.0182(3) 0.0178(3) 0.0212(8) -0.0006(6) -0.0005(4) 0.0024(3) O1 0.0180(10) 0.0273(11) 0.0481(16) -0.0196(16) -0.0114(15) 0.0094(8) O2 0.0120(10) 0.0224(10) 0.0250(12) -0.0036(10) -0.0011(9) -0.0005(8) O3 0.0161(10) 0.0183(10) 0.0233(13) 0.0010(8) -0.0037(8) -0.0038(8) O4 0.0238(13) 0.0273(12) 0.0174(12) 0.0006(10) 0.0016(10) -0.0036(10) O5 0.0201(13) 0.0313(16) 0.0296(16) -0.0133(13) 0.0051(12) 0.0015(12) O6 0.0187(13) 0.0222(13) 0.0194(13) 0.0035(10) -0.0034(10) -0.0006(10) O7 0.0360(14) 0.0221(12) 0.0136(12) 0.0018(9) 0.0018(10) 0.0070(10) O8 0.0157(10) 0.0201(10) 0.0207(15) -0.0024(9) -0.0019(9) 0.0021(8) O9 0.0134(10) 0.0201(10) 0.0178(11) 0.0014(9) -0.0026(9) 0.0002(8) O10 0.0171(10) 0.0191(10) 0.0226(15) 0.0023(9) -0.0056(9) -0.0024(8) C1 0.0193(18) 0.0258(18) 0.040(2) -0.0040(16) -0.0127(16) 0.0071(14) C2 0.0122(14) 0.0328(17) 0.030(2) -0.0049(13) -0.0024(12) 0.0090(12) C3 0.0162(16) 0.0304(18) 0.0267(18) 0.0013(14) -0.0033(14) -0.0064(13) C4 0.0201(18) 0.0269(18) 0.031(2) -0.0012(15) -0.0083(15) -0.0069(14) C5 0.0222(17) 0.0199(16) 0.0283(18) 0.0076(14) -0.0013(14) -0.0012(13) C6 0.0227(18) 0.0262(17) 0.0240(18) 0.0075(14) -0.0003(14) -0.0047(14) C7 0.034(2) 0.041(2) 0.0192(17) -0.0038(15) 0.0037(16) -0.0050(17) C8 0.029(2) 0.039(3) 0.0168(18) -0.0044(17) 0.0028(15) -0.0052(17) C9 0.0212(19) 0.045(2) 0.040(2) -0.024(2) 0.0037(17) 0.0019(16) C10 0.0262(19) 0.0232(18) 0.051(3) -0.0219(17) -0.0077(18) 0.0094(14) C11 0.032(2) 0.0226(18) 0.0187(18) 0.0046(14) -0.0077(16) -0.0029(16) C12 0.040(2) 0.0258(18) 0.0172(17) 0.0023(14) 0.0030(15) 0.0001(16) C13 0.0300(19) 0.0209(16) 0.0231(18) -0.0051(14) 0.0024(15) 0.0050(14) C14 0.0224(18) 0.0222(17) 0.0304(19) -0.0089(14) 0.0010(15) 0.0047(13) C15 0.0159(16) 0.0224(16) 0.0271(18) 0.0055(14) -0.0043(14) 0.0023(13) C16 0.0202(17) 0.0260(18) 0.0276(19) 0.0092(14) -0.0025(14) 0.0013(13) C17 0.0182(16) 0.0323(18) 0.0173(16) 0.0037(14) -0.0027(13) -0.0067(13) C18 0.0209(17) 0.0213(17) 0.0275(18) -0.0055(14) -0.0044(15) -0.0034(13) C19 0.029(2) 0.0168(16) 0.037(2) 0.0085(14) -0.0066(16) -0.0029(13) C20 0.0241(18) 0.0270(18) 0.0270(19) 0.0110(15) -0.0053(15) -0.0080(14) C21 0.035(2) 0.051(3) 0.049(3) 0.019(2) 0.017(2) 0.0090(19) C22 0.026(2) 0.0313(19) 0.041(2) 0.0059(17) -0.0034(17) 0.0094(15) C23 0.027(2) 0.0328(19) 0.030(2) 0.0035(15) -0.0068(15) -0.0040(14) C24 0.0317(19) 0.0185(15) 0.0185(17) -0.0025(12) -0.0008(14) 0.0025(12) C25 0.0267(19) 0.0349(19) 0.0246(19) 0.0097(15) -0.0013(15) 0.0001(15) C26 0.0220(18) 0.036(2) 0.0241(18) -0.0098(15) 0.0017(14) -0.0010(14) C27 0.0184(17) 0.0365(19) 0.0237(18) -0.0004(15) 0.0011(13) -0.0005(14) C28 0.0170(16) 0.0258(17) 0.0172(15) -0.0014(12) 0.0020(12) 0.0003(11) C29 0.0216(17) 0.0248(16) 0.0309(18) 0.0042(14) 0.0000(15) 0.0012(14) C30 0.0252(19) 0.032(2) 0.033(2) -0.0010(14) -0.0053(16) 0.0053(14) C31 0.031(2) 0.0273(18) 0.038(2) -0.0004(15) 0.0098(17) 0.0006(14) C32 0.030(2) 0.0290(18) 0.0303(19) -0.0042(15) -0.0024(16) 0.0053(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 Pr1 O10 2.510(2) . ? Pr1 O9 2.536(2) . ? Pr1 O2 2.573(2) . ? Pr1 O3 2.578(2) . ? Pr1 O1 2.604(2) . ? Pr1 O6 2.610(3) . ? Pr1 O8 2.614(2) . ? Pr1 O7 2.632(2) . ? Pr1 O4 2.661(2) . ? Pr1 O5 2.686(3) . ? Al1 C21 2.005(4) . ? Al1 C22 2.018(4) . ? Al1 C23 2.025(4) . ? Al1 C24 2.025(4) . ? Al2 C28 2.000(3) . ? Al2 C26 2.005(3) . ? Al2 C25 2.004(3) . ? Al2 C27 2.020(3) . ? Al3 C31 2.014(5) . ? Al3 C30 2.021(4) . ? Al3 C32 2.007(4) . ? Al3 C29 2.009(4) . ? O1 C1 1.447(4) . ? O1 C10 1.464(4) . ? O2 C2 1.441(4) . ? O2 C3 1.446(4) . ? O3 C5 1.439(4) . ? O3 C4 1.442(4) . ? O4 C7 1.434(4) . ? O4 C6 1.444(4) . ? O5 C9 1.411(5) . ? O5 C8 1.470(5) . ? O6 C11 1.437(4) . ? O6 C20 1.444(4) . ? O7 C12 1.435(4) . ? O7 C13 1.444(4) . ? O8 C15 1.445(4) . ? O8 C14 1.444(4) . ? O9 C17 1.426(4) . ? O9 C16 1.451(4) . ? O10 C19 1.440(4) . ? O10 C18 1.446(4) . ? C1 C2 1.491(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.488(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.481(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.495(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.488(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.490(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.486(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.478(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.491(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.482(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 O10 Pr1 O9 61.81(7) . . ? O10 Pr1 O2 130.53(7) . . ? O9 Pr1 O2 156.17(7) . . ? O10 Pr1 O3 158.17(7) . . ? O9 Pr1 O3 114.26(7) . . ? O2 Pr1 O3 62.40(7) . . ? O10 Pr1 O1 73.92(7) . . ? O9 Pr1 O1 112.42(7) . . ? O2 Pr1 O1 62.26(7) . . ? O3 Pr1 O1 123.97(7) . . ? O10 Pr1 O6 62.20(7) . . ? O9 Pr1 O6 122.04(7) . . ? O2 Pr1 O6 77.99(7) . . ? O3 Pr1 O6 111.79(8) . . ? O1 Pr1 O6 63.80(10) . . ? O10 Pr1 O8 93.74(7) . . ? O9 Pr1 O8 61.73(7) . . ? O2 Pr1 O8 127.85(7) . . ? O3 Pr1 O8 67.59(7) . . ? O1 Pr1 O8 167.47(7) . . ? O6 Pr1 O8 108.83(8) . . ? O10 Pr1 O7 97.81(8) . . ? O9 Pr1 O7 116.30(7) . . ? O2 Pr1 O7 84.30(7) . . ? O3 Pr1 O7 63.68(7) . . ? O1 Pr1 O7 118.10(9) . . ? O6 Pr1 O7 58.95(9) . . ? O8 Pr1 O7 60.49(7) . . ? O10 Pr1 O4 131.60(7) . . ? O9 Pr1 O4 75.53(7) . . ? O2 Pr1 O4 83.41(7) . . ? O3 Pr1 O4 60.49(7) . . ? O1 Pr1 O4 104.98(9) . . ? O6 Pr1 O4 161.21(7) . . ? O8 Pr1 O4 84.72(7) . . ? O7 Pr1 O4 122.07(7) . . ? O10 Pr1 O5 80.72(8) . . ? O9 Pr1 O5 64.53(8) . . ? O2 Pr1 O5 95.36(8) . . ? O3 Pr1 O5 118.11(8) . . ? O1 Pr1 O5 59.91(10) . . ? O6 Pr1 O5 118.81(8) . . ? O8 Pr1 O5 121.18(8) . . ? O7 Pr1 O5 177.76(9) . . ? O4 Pr1 O5 60.04(9) . . ? C21 Al1 C22 109.01(17) . . ? C21 Al1 C23 110.32(18) . . ? C22 Al1 C23 106.55(17) . . ? C21 Al1 C24 107.50(17) . . ? C22 Al1 C24 112.55(15) . . ? C23 Al1 C24 110.91(14) . . ? C28 Al2 C26 111.56(14) . . ? C28 Al2 C25 107.43(15) . . ? C26 Al2 C25 108.04(16) . . ? C28 Al2 C27 110.51(15) . . ? C26 Al2 C27 109.37(15) . . ? C25 Al2 C27 109.88(15) . . ? C31 Al3 C30 107.7(3) . . ? C31 Al3 C32 109.15(16) . . ? C30 Al3 C32 110.01(15) . . ? C31 Al3 C29 112.58(15) . . ? C30 Al3 C29 108.45(15) . . ? C32 Al3 C29 108.9(2) . . ? C1 O1 C10 115.8(3) . . ? C1 O1 Pr1 117.27(19) . . ? C10 O1 Pr1 120.5(2) . . ? C2 O2 C3 110.8(2) . . ? C2 O2 Pr1 121.53(18) . . ? C3 O2 Pr1 122.02(18) . . ? C5 O3 C4 116.6(2) . . ? C5 O3 Pr1 117.26(17) . . ? C4 O3 Pr1 117.52(18) . . ? C7 O4 C6 111.0(3) . . ? C7 O4 Pr1 123.9(2) . . ? C6 O4 Pr1 122.08(18) . . ? C9 O5 C8 114.1(3) . . ? C9 O5 Pr1 121.3(2) . . ? C8 O5 Pr1 114.9(2) . . ? C11 O6 C20 112.7(3) . . ? C11 O6 Pr1 116.1(2) . . ? C20 O6 Pr1 117.77(19) . . ? C12 O7 C13 113.0(3) . . ? C12 O7 Pr1 125.9(2) . . ? C13 O7 Pr1 119.77(19) . . ? C15 O8 C14 110.0(2) . . ? C15 O8 Pr1 121.12(17) . . ? C14 O8 Pr1 123.59(18) . . ? C17 O9 C16 112.4(2) . . ? C17 O9 Pr1 122.75(18) . . ? C16 O9 Pr1 113.23(18) . . ? C19 O10 C18 113.8(2) . . ? C19 O10 Pr1 121.64(18) . . ? C18 O10 Pr1 120.25(18) . . ? O1 C1 C2 109.1(3) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 107.6(3) . . ? O2 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O2 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O2 C3 C4 107.0(3) . . ? O2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? O2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? O3 C4 C3 110.4(3) . . ? O3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? O3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? O3 C5 C6 109.7(3) . . ? O3 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O3 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O4 C6 C5 106.5(3) . . ? O4 C6 H6A 110.4 . . ? C5 C6 H6A 110.4 . . ? O4 C6 H6B 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O4 C7 C8 106.8(3) . . ? O4 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O4 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O5 C8 C7 108.5(3) . . ? O5 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O5 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O5 C9 C10 106.0(3) . . ? O5 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O5 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O1 C10 C9 109.0(3) . . ? O1 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O1 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O6 C11 C12 109.2(3) . . ? O6 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O6 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? O7 C12 C11 105.0(3) . . ? O7 C12 H12A 110.7 . . ? C11 C12 H12A 110.7 . . ? O7 C12 H12B 110.7 . . ? C11 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? O7 C13 C14 109.3(3) . . ? O7 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? O7 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? O8 C14 C13 108.3(3) . . ? O8 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? O8 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? O8 C15 C16 107.0(3) . . ? O8 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? O8 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.6 . . ? O9 C16 C15 109.3(3) . . ? O9 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O9 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O9 C17 C18 108.2(3) . . ? O9 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? O9 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? O10 C18 C17 106.8(3) . . ? O10 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? O10 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? O10 C19 C20 107.1(3) . . ? O10 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O10 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? O6 C20 C19 108.2(3) . . ? O6 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O6 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Al1 C22 H22A 109.5 . . ? Al1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al1 C23 H23A 109.5 . . ? Al1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al1 C24 H24A 109.5 . . ? Al1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Al2 C26 H26A 109.5 . . ? Al2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Al2 C27 H27A 109.5 . . ? Al2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Al2 C28 H28A 109.5 . . ? Al2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Al2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Al3 C29 H29A 109.5 . . ? Al3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Al3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Al3 C30 H30A 109.5 . . ? Al3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Al3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Al3 C31 H31A 109.5 . . ? Al3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Al3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Al3 C32 H32A 109.5 . . ? Al3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Al3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.358 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.095 #============================================================================== data_compound5 _database_code_depnum_ccdc_archive 'CCDC 764354' #TrackingRef 'compound1_6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H35 O7 Y, 2(C4 H12 Al), C4 H8 O' _chemical_formula_sum 'C29 H67 Al2 O8 Y' _chemical_formula_weight 686.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.32730(10) _cell_length_b 30.0819(3) _cell_length_c 11.65110(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.4467(6) _cell_angle_gamma 90.00 _cell_volume 3743.59(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 87508 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6382 _exptl_absorpt_correction_T_max 0.7239 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71869 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8569 _reflns_number_gt 7219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Disorder of C(3)/C(4) on two positions (50:50). 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^)+(0.0332P)^2^+1.4615P] 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 8569 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.736601(14) 0.146057(5) 0.225454(14) 0.01783(5) Uani 1 1 d . A . O1 O 0.59011(11) 0.08953(4) 0.11855(11) 0.0276(3) Uani 1 1 d . A . O2 O 0.57648(11) 0.13387(4) 0.31147(11) 0.0290(3) Uani 1 1 d . . . O3 O 0.72501(11) 0.20089(4) 0.36896(11) 0.0254(3) Uani 1 1 d . . . O4 O 0.88249(10) 0.20734(4) 0.24790(10) 0.0217(2) Uani 1 1 d . . . O5 O 0.94209(11) 0.13432(4) 0.38289(10) 0.0230(2) Uani 1 1 d . . . O6 O 0.78543(11) 0.07058(4) 0.30611(11) 0.0249(3) Uani 1 1 d . . . O7 O 0.84995(11) 0.12234(4) 0.10291(10) 0.0255(3) Uani 1 1 d . . . C1 C 0.46842(17) 0.09475(6) 0.13155(17) 0.0308(4) Uani 1 1 d . . . H1A H 0.4164 0.0683 0.0981 0.037 Uiso 1 1 calc R A . H1B H 0.4260 0.1211 0.0848 0.037 Uiso 1 1 calc R . . C2 C 0.48103(17) 0.10042(6) 0.26372(17) 0.0321(4) Uani 1 1 d . A . H2A H 0.4006 0.1102 0.2716 0.038 Uiso 1 1 calc R . . H2B H 0.5062 0.0721 0.3083 0.038 Uiso 1 1 calc R . . C3A C 0.5466(5) 0.16103(12) 0.3902(4) 0.0227(10) Uiso 0.502(9) 1 d P A 1 H3A1 H 0.5218 0.1433 0.4500 0.027 Uiso 0.502(9) 1 calc PR A 1 H3A2 H 0.4759 0.1806 0.3458 0.027 Uiso 0.502(9) 1 calc PR A 1 C4A C 0.6604(4) 0.18825(17) 0.4536(4) 0.0257(10) Uiso 0.502(9) 1 d P A 1 H4A1 H 0.6354 0.2153 0.4880 0.031 Uiso 0.502(9) 1 calc PR A 1 H4A2 H 0.7178 0.1709 0.5216 0.031 Uiso 0.502(9) 1 calc PR A 1 C3B C 0.5919(5) 0.15587(13) 0.4311(4) 0.0249(11) Uiso 0.498(9) 1 d P A 2 H3B1 H 0.5110 0.1557 0.4464 0.030 Uiso 0.498(9) 1 calc PR A 2 H3B2 H 0.6537 0.1392 0.4976 0.030 Uiso 0.498(9) 1 calc PR A 2 C4B C 0.6352(4) 0.20228(17) 0.4292(4) 0.0246(10) Uiso 0.498(9) 1 d P A 2 H4B1 H 0.5643 0.2218 0.3849 0.029 Uiso 0.498(9) 1 calc PR A 2 H4B2 H 0.6734 0.2137 0.5132 0.029 Uiso 0.498(9) 1 calc PR A 2 C5 C 0.79237(17) 0.24243(6) 0.38691(16) 0.0266(4) Uani 1 1 d . A . H5A H 0.8654 0.2415 0.4628 0.032 Uiso 1 1 calc R . . H5B H 0.7373 0.2673 0.3926 0.032 Uiso 1 1 calc R . . C6 C 0.83479(17) 0.24851(5) 0.27831(16) 0.0253(4) Uani 1 1 d . A . H6A H 0.7635 0.2588 0.2079 0.030 Uiso 1 1 calc R . . H6B H 0.9010 0.2715 0.2967 0.030 Uiso 1 1 calc R . . C7 C 1.01328(16) 0.19863(6) 0.31312(17) 0.0281(4) Uani 1 1 d . A . H7A H 1.0583 0.2271 0.3378 0.034 Uiso 1 1 calc R . . H7B H 1.0508 0.1829 0.2590 0.034 Uiso 1 1 calc R . . C8 C 1.02814(16) 0.17070(6) 0.42439(17) 0.0275(4) Uani 1 1 d . A . H8A H 1.1151 0.1596 0.4594 0.033 Uiso 1 1 calc R . . H8B H 1.0075 0.1882 0.4871 0.033 Uiso 1 1 calc R . . C9 C 0.94372(17) 0.10220(5) 0.47483(15) 0.0249(4) Uani 1 1 d . A . H9A H 0.8895 0.1120 0.5213 0.030 Uiso 1 1 calc R . . H9B H 1.0299 0.0981 0.5321 0.030 Uiso 1 1 calc R . . C10 C 0.89538(17) 0.05969(6) 0.40824(16) 0.0266(4) Uani 1 1 d . A . H10A H 0.9599 0.0460 0.3794 0.032 Uiso 1 1 calc R . . H10B H 0.8737 0.0384 0.4628 0.032 Uiso 1 1 calc R . . C11 C 0.71290(18) 0.03181(6) 0.25233(17) 0.0308(4) Uani 1 1 d . A . H11A H 0.6582 0.0229 0.2992 0.037 Uiso 1 1 calc R . . H11B H 0.7689 0.0066 0.2516 0.037 Uiso 1 1 calc R . . C12 C 0.63490(19) 0.04451(6) 0.12355(17) 0.0332(4) Uani 1 1 d . . . H12A H 0.6861 0.0415 0.0697 0.040 Uiso 1 1 calc R A . H12B H 0.5627 0.0240 0.0936 0.040 Uiso 1 1 calc R . . C13 C 0.59690(16) 0.19045(6) 0.06562(15) 0.0248(4) Uani 1 1 d . . . H13A H 0.6439 0.2147 0.0447 0.037 Uiso 1 1 calc R A . H13B H 0.5311 0.2029 0.0933 0.037 Uiso 1 1 calc R . . H13C H 0.5588 0.1718 -0.0063 0.037 Uiso 1 1 calc R . . C14 C 0.8354(2) 0.14524(7) -0.01214(19) 0.0451(6) Uani 1 1 d . A . H14A H 0.8798 0.1741 0.0032 0.054 Uiso 1 1 calc R . . H14B H 0.7458 0.1506 -0.0579 0.054 Uiso 1 1 calc R . . C15 C 0.8908(2) 0.11522(7) -0.08093(19) 0.0461(6) Uani 1 1 d . . . H15A H 0.9231 0.1322 -0.1370 0.055 Uiso 1 1 calc R A . H15B H 0.8287 0.0932 -0.1284 0.055 Uiso 1 1 calc R . . C16 C 0.9959(2) 0.09282(8) 0.01742(19) 0.0404(5) Uani 1 1 d . A . H16A H 1.0155 0.0635 -0.0101 0.048 Uiso 1 1 calc R . . H16B H 1.0724 0.1114 0.0415 0.048 Uiso 1 1 calc R . . C17 C 0.94563(19) 0.08793(7) 0.12079(18) 0.0361(5) Uani 1 1 d . A . H17A H 0.9087 0.0581 0.1197 0.043 Uiso 1 1 calc R . . H17B H 1.0133 0.0921 0.1998 0.043 Uiso 1 1 calc R . . Al1 Al 0.79239(5) 0.246583(18) 0.76545(5) 0.02335(11) Uani 1 1 d . . . C18 C 0.83508(17) 0.26903(7) 0.93818(16) 0.0310(4) Uani 1 1 d . . . H18A H 0.9200 0.2595 0.9861 0.046 Uiso 1 1 calc R . . H18B H 0.7753 0.2569 0.9744 0.046 Uiso 1 1 calc R . . H18C H 0.8307 0.3016 0.9377 0.046 Uiso 1 1 calc R . . C19 C 0.74283(17) 0.29924(6) 0.65085(17) 0.0283(4) Uani 1 1 d . . . H19A H 0.8098 0.3056 0.6175 0.042 Uiso 1 1 calc R . . H19B H 0.7292 0.3253 0.6954 0.042 Uiso 1 1 calc R . . H19C H 0.6655 0.2923 0.5842 0.042 Uiso 1 1 calc R . . C20 C 0.94080(18) 0.21550(7) 0.74069(19) 0.0366(5) Uani 1 1 d . . . H20A H 0.9901 0.2371 0.7127 0.055 Uiso 1 1 calc R . . H20B H 0.9109 0.1920 0.6796 0.055 Uiso 1 1 calc R . . H20C H 0.9932 0.2024 0.8178 0.055 Uiso 1 1 calc R . . C21 C 0.64930(16) 0.20290(6) 0.73385(15) 0.0239(4) Uani 1 1 d . . . H21A H 0.6746 0.1741 0.7101 0.036 Uiso 1 1 calc R . . H21B H 0.5764 0.2141 0.6682 0.036 Uiso 1 1 calc R . . H21C H 0.6276 0.1993 0.8080 0.036 Uiso 1 1 calc R . . Al2 Al 0.78046(5) 0.00556(2) 0.68054(5) 0.03171(13) Uani 1 1 d . . . C22 C 0.7371(2) -0.00560(8) 0.8322(2) 0.0483(6) Uani 1 1 d . . . H22A H 0.7782 0.0167 0.8938 0.072 Uiso 1 1 calc R . . H22B H 0.7658 -0.0353 0.8638 0.072 Uiso 1 1 calc R . . H22C H 0.6462 -0.0036 0.8130 0.072 Uiso 1 1 calc R . . C23 C 0.95767(16) 0.02842(6) 0.72858(16) 0.0266(4) Uani 1 1 d . . . H23A H 0.9897 0.0242 0.6609 0.040 Uiso 1 1 calc R . . H23B H 1.0104 0.0121 0.8000 0.040 Uiso 1 1 calc R . . H23C H 0.9590 0.0601 0.7482 0.040 Uiso 1 1 calc R . . C24 C 0.6649(2) 0.05234(9) 0.5816(2) 0.0480(6) Uani 1 1 d . . . H24A H 0.5791 0.0409 0.5526 0.072 Uiso 1 1 calc R . . H24B H 0.6904 0.0603 0.5117 0.072 Uiso 1 1 calc R . . H24C H 0.6688 0.0787 0.6320 0.072 Uiso 1 1 calc R . . C25 C 0.7621(2) -0.05030(8) 0.5801(2) 0.0473(6) Uani 1 1 d . . . H25A H 0.6735 -0.0586 0.5471 0.071 Uiso 1 1 calc R . . H25B H 0.8095 -0.0744 0.6315 0.071 Uiso 1 1 calc R . . H25C H 0.7943 -0.0450 0.5130 0.071 Uiso 1 1 calc R . . O8 O 0.87665(12) 0.43697(4) 0.35006(13) 0.0346(3) Uani 1 1 d . . . C26 C 0.76214(18) 0.41297(7) 0.3257(2) 0.0371(5) Uani 1 1 d . . . H26A H 0.6944 0.4274 0.2593 0.045 Uiso 1 1 calc R . . H26B H 0.7370 0.4118 0.3993 0.045 Uiso 1 1 calc R . . C27 C 0.78730(19) 0.36674(7) 0.28873(19) 0.0365(5) Uani 1 1 d . . . H27A H 0.7095 0.3522 0.2366 0.044 Uiso 1 1 calc R . . H27B H 0.8277 0.3478 0.3606 0.044 Uiso 1 1 calc R . . C28 C 0.8757(2) 0.37660(7) 0.21836(19) 0.0384(5) Uani 1 1 d . . . H28A H 0.9289 0.3506 0.2176 0.046 Uiso 1 1 calc R . . H28B H 0.8290 0.3855 0.1335 0.046 Uiso 1 1 calc R . . C29 C 0.9528(2) 0.41484(7) 0.2901(2) 0.0413(5) Uani 1 1 d . . . H29A H 1.0308 0.4036 0.3508 0.050 Uiso 1 1 calc R . . H29B H 0.9753 0.4357 0.2349 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01880(8) 0.01731(8) 0.01797(8) 0.00018(6) 0.00692(6) -0.00024(6) O1 0.0303(7) 0.0228(6) 0.0267(6) -0.0005(5) 0.0055(5) -0.0055(5) O2 0.0251(6) 0.0399(7) 0.0245(6) -0.0035(5) 0.0115(5) -0.0094(5) O3 0.0336(7) 0.0208(6) 0.0289(6) -0.0021(5) 0.0197(5) -0.0005(5) O4 0.0213(6) 0.0191(6) 0.0258(6) 0.0001(5) 0.0094(5) -0.0004(5) O5 0.0237(6) 0.0211(6) 0.0227(6) 0.0019(5) 0.0056(5) -0.0015(5) O6 0.0297(6) 0.0176(6) 0.0243(6) 0.0020(5) 0.0046(5) -0.0008(5) O7 0.0324(7) 0.0244(6) 0.0233(6) 0.0044(5) 0.0141(5) 0.0096(5) C1 0.0236(9) 0.0284(9) 0.0344(10) 0.0060(8) 0.0016(8) -0.0072(7) C2 0.0234(9) 0.0339(10) 0.0383(10) 0.0070(8) 0.0095(8) -0.0065(8) C5 0.0274(9) 0.0227(8) 0.0293(9) -0.0061(7) 0.0087(7) 0.0005(7) C6 0.0264(9) 0.0177(8) 0.0311(9) -0.0010(7) 0.0086(7) 0.0000(7) C7 0.0194(8) 0.0273(9) 0.0386(10) 0.0007(8) 0.0109(8) -0.0018(7) C8 0.0198(8) 0.0248(9) 0.0334(10) -0.0006(7) 0.0028(7) -0.0022(7) C9 0.0284(9) 0.0233(9) 0.0216(8) 0.0047(7) 0.0065(7) 0.0038(7) C10 0.0307(9) 0.0222(9) 0.0251(9) 0.0037(7) 0.0067(7) 0.0034(7) C11 0.0349(10) 0.0178(9) 0.0360(10) -0.0018(7) 0.0069(8) -0.0059(7) C12 0.0401(11) 0.0239(9) 0.0320(10) -0.0057(8) 0.0069(8) -0.0047(8) C13 0.0239(9) 0.0271(9) 0.0237(8) 0.0012(7) 0.0084(7) 0.0001(7) C14 0.0684(15) 0.0450(12) 0.0336(11) 0.0189(9) 0.0327(11) 0.0260(11) C15 0.0749(16) 0.0388(11) 0.0385(11) 0.0112(9) 0.0375(12) 0.0217(11) C16 0.0401(11) 0.0479(13) 0.0390(11) -0.0056(9) 0.0209(9) 0.0070(10) C17 0.0420(11) 0.0357(11) 0.0330(10) 0.0047(8) 0.0157(9) 0.0211(9) Al1 0.0204(2) 0.0276(3) 0.0222(3) 0.0014(2) 0.0072(2) -0.0020(2) C18 0.0262(9) 0.0394(11) 0.0269(9) -0.0014(8) 0.0082(8) -0.0100(8) C19 0.0310(9) 0.0269(9) 0.0293(9) -0.0008(7) 0.0132(8) -0.0025(7) C20 0.0279(10) 0.0429(12) 0.0423(11) 0.0129(9) 0.0161(9) 0.0050(9) C21 0.0253(9) 0.0267(9) 0.0200(8) 0.0005(7) 0.0078(7) -0.0019(7) Al2 0.0253(3) 0.0377(3) 0.0320(3) -0.0087(2) 0.0094(2) -0.0039(2) C22 0.0521(14) 0.0482(13) 0.0531(14) -0.0062(11) 0.0288(12) -0.0216(11) C23 0.0281(9) 0.0244(9) 0.0267(9) -0.0021(7) 0.0083(7) 0.0006(7) C24 0.0316(11) 0.0740(16) 0.0382(12) -0.0017(11) 0.0115(9) 0.0116(11) C25 0.0315(11) 0.0541(14) 0.0528(14) -0.0237(11) 0.0092(10) -0.0075(10) O8 0.0344(7) 0.0255(7) 0.0421(8) -0.0026(6) 0.0102(6) 0.0021(6) C26 0.0281(10) 0.0351(11) 0.0430(11) -0.0023(9) 0.0050(9) 0.0055(8) C27 0.0348(11) 0.0279(10) 0.0408(12) 0.0026(8) 0.0043(9) 0.0019(8) C28 0.0476(12) 0.0304(11) 0.0357(11) 0.0012(8) 0.0118(9) 0.0097(9) C29 0.0408(12) 0.0394(12) 0.0472(12) 0.0028(9) 0.0194(10) 0.0043(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 Y1 O7 2.3274(11) . ? Y1 O2 2.3746(12) . ? Y1 O3 2.3831(11) . ? Y1 C13 2.4068(17) . ? Y1 O1 2.4125(12) . ? Y1 O4 2.4311(11) . ? Y1 O6 2.4490(11) . ? Y1 O5 2.4626(12) . ? O1 C12 1.441(2) . ? O1 C1 1.444(2) . ? O2 C3A 1.352(4) . ? O2 C2 1.446(2) . ? O2 C3B 1.500(4) . ? O3 C4B 1.416(4) . ? O3 C5 1.443(2) . ? O3 C4A 1.461(4) . ? O4 C6 1.4419(19) . ? O4 C7 1.446(2) . ? O5 C8 1.438(2) . ? O5 C9 1.4382(19) . ? O6 C11 1.444(2) . ? O6 C10 1.445(2) . ? O7 C17 1.462(2) . ? O7 C14 1.467(2) . ? C1 C2 1.508(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3A C4A 1.498(6) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C3B C4B 1.482(6) . ? C3B H3B1 0.9900 . ? C3B H3B2 0.9900 . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C5 C6 1.507(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.506(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.501(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.515(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.479(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.501(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? Al1 C18 2.0229(18) . ? Al1 C21 2.0229(17) . ? Al1 C20 2.0264(19) . ? Al1 C19 2.0268(18) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? Al2 C24 2.005(2) . ? Al2 C22 2.014(2) . ? Al2 C23 2.0168(18) . ? Al2 C25 2.019(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O8 C26 1.428(2) . ? O8 C29 1.441(2) . ? C26 C27 1.511(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.519(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.516(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Y1 O2 150.05(4) . . ? O7 Y1 O3 144.40(4) . . ? O2 Y1 O3 65.32(4) . . ? O7 Y1 C13 92.88(5) . . ? O2 Y1 C13 90.82(5) . . ? O3 Y1 C13 89.04(5) . . ? O7 Y1 O1 83.81(4) . . ? O2 Y1 O1 67.57(4) . . ? O3 Y1 O1 131.37(4) . . ? C13 Y1 O1 80.19(5) . . ? O7 Y1 O4 78.72(4) . . ? O2 Y1 O4 131.23(4) . . ? O3 Y1 O4 66.04(4) . . ? C13 Y1 O4 84.88(5) . . ? O1 Y1 O4 156.36(4) . . ? O7 Y1 O6 81.43(4) . . ? O2 Y1 O6 78.56(4) . . ? O3 Y1 O6 115.50(4) . . ? C13 Y1 O6 144.84(5) . . ? O1 Y1 O6 64.74(4) . . ? O4 Y1 O6 127.10(4) . . ? O7 Y1 O5 80.52(4) . . ? O2 Y1 O5 109.20(4) . . ? O3 Y1 O5 80.55(4) . . ? C13 Y1 O5 150.55(5) . . ? O1 Y1 O5 126.92(4) . . ? O4 Y1 O5 65.70(4) . . ? O6 Y1 O5 62.91(4) . . ? C12 O1 C1 115.68(14) . . ? C12 O1 Y1 117.99(10) . . ? C1 O1 Y1 112.68(10) . . ? C3A O2 C2 111.0(2) . . ? C3A O2 C3B 23.28(18) . . ? C2 O2 C3B 120.37(18) . . ? C3A O2 Y1 126.26(17) . . ? C2 O2 Y1 121.56(10) . . ? C3B O2 Y1 117.07(17) . . ? C4B O3 C5 109.6(2) . . ? C4B O3 C4A 21.36(19) . . ? C5 O3 C4A 119.16(19) . . ? C4B O3 Y1 125.80(17) . . ? C5 O3 Y1 123.45(9) . . ? C4A O3 Y1 116.79(18) . . ? C6 O4 C7 115.39(13) . . ? C6 O4 Y1 112.39(9) . . ? C7 O4 Y1 117.38(9) . . ? C8 O5 C9 114.94(12) . . ? C8 O5 Y1 120.54(9) . . ? C9 O5 Y1 115.19(9) . . ? C11 O6 C10 112.58(13) . . ? C11 O6 Y1 124.00(10) . . ? C10 O6 Y1 123.29(10) . . ? C17 O7 C14 108.36(13) . . ? C17 O7 Y1 131.57(10) . . ? C14 O7 Y1 119.97(10) . . ? O1 C1 C2 110.49(14) . . ? O1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? O1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? O2 C2 C1 106.02(14) . . ? O2 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? O2 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? O2 C3A C4A 107.2(3) . . ? O2 C3A H3A1 110.3 . . ? C4A C3A H3A1 110.3 . . ? O2 C3A H3A2 110.3 . . ? C4A C3A H3A2 110.3 . . ? H3A1 C3A H3A2 108.5 . . ? O3 C4A C3A 110.6(3) . . ? O3 C4A H4A1 109.5 . . ? C3A C4A H4A1 109.5 . . ? O3 C4A H4A2 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 108.1 . . ? C4B C3B O2 109.8(3) . . ? C4B C3B H3B1 109.7 . . ? O2 C3B H3B1 109.7 . . ? C4B C3B H3B2 109.7 . . ? O2 C3B H3B2 109.7 . . ? H3B1 C3B H3B2 108.2 . . ? O3 C4B C3B 106.0(3) . . ? O3 C4B H4B1 110.5 . . ? C3B C4B H4B1 110.5 . . ? O3 C4B H4B2 110.5 . . ? C3B C4B H4B2 110.5 . . ? H4B1 C4B H4B2 108.7 . . ? O3 C5 C6 106.53(13) . . ? O3 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O3 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? O4 C6 C5 110.64(14) . . ? O4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O4 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? O4 C7 C8 110.77(13) . . ? O4 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? O4 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O5 C8 C7 105.42(14) . . ? O5 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? O5 C8 H8B 110.7 . . ? C7 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? O5 C9 C10 105.98(13) . . ? O5 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O5 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O6 C10 C9 107.37(13) . . ? O6 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O6 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O6 C11 C12 106.62(14) . . ? O6 C11 H11A 110.4 . . ? C12 C11 H11A 110.4 . . ? O6 C11 H11B 110.4 . . ? C12 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? O1 C12 C11 111.01(15) . . ? O1 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? O1 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? Y1 C13 H13A 109.5 . . ? Y1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Y1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O7 C14 C15 105.64(15) . . ? O7 C14 H14A 110.6 . . ? C15 C14 H14A 110.6 . . ? O7 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? C14 C15 C16 103.36(17) . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C17 C16 C15 103.84(16) . . ? C17 C16 H16A 111.0 . . ? C15 C16 H16A 111.0 . . ? C17 C16 H16B 111.0 . . ? C15 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? O7 C17 C16 106.11(15) . . ? O7 C17 H17A 110.5 . . ? C16 C17 H17A 110.5 . . ? O7 C17 H17B 110.5 . . ? C16 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? C18 Al1 C21 108.04(7) . . ? C18 Al1 C20 111.15(8) . . ? C21 Al1 C20 109.07(8) . . ? C18 Al1 C19 108.46(8) . . ? C21 Al1 C19 111.00(7) . . ? C20 Al1 C19 109.13(8) . . ? Al1 C18 H18A 109.5 . . ? Al1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al1 C19 H19A 109.5 . . ? Al1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al1 C20 H20A 109.5 . . ? Al1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 Al2 C22 108.59(10) . . ? C24 Al2 C23 108.61(9) . . ? C22 Al2 C23 108.92(9) . . ? C24 Al2 C25 109.23(10) . . ? C22 Al2 C25 111.21(10) . . ? C23 Al2 C25 110.23(8) . . ? Al2 C22 H22A 109.5 . . ? Al2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al2 C23 H23A 109.5 . . ? Al2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al2 C24 H24A 109.5 . . ? Al2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 O8 C29 108.71(15) . . ? O8 C26 C27 106.08(16) . . ? O8 C26 H26A 110.5 . . ? C27 C26 H26A 110.5 . . ? O8 C26 H26B 110.5 . . ? C27 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? C26 C27 C28 101.24(16) . . ? C26 C27 H27A 111.5 . . ? C28 C27 H27A 111.5 . . ? C26 C27 H27B 111.5 . . ? C28 C27 H27B 111.5 . . ? H27A C27 H27B 109.3 . . ? C29 C28 C27 102.30(16) . . ? C29 C28 H28A 111.3 . . ? C27 C28 H28A 111.3 . . ? C29 C28 H28B 111.3 . . ? C27 C28 H28B 111.3 . . ? H28A C28 H28B 109.2 . . ? O8 C29 C28 106.84(16) . . ? O8 C29 H29A 110.4 . . ? C28 C29 H29A 110.4 . . ? O8 C29 H29B 110.4 . . ? C28 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.473 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.050 #============================================================================== data_compound6 _database_code_depnum_ccdc_archive 'CCDC 764355' #TrackingRef 'compound1_6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H43 O8 Pr, 2(C4 H12 Al)' _chemical_formula_sum 'C29 H67 Al2 O8 Pr' _chemical_formula_weight 738.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.86100(10) _cell_length_b 14.7330(2) _cell_length_c 21.8646(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.5470(7) _cell_angle_gamma 90.00 _cell_volume 3817.02(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 77585 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6855 _exptl_absorpt_correction_T_max 0.8989 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80699 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8736 _reflns_number_gt 7629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _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^)+(0.0276P)^2^+3.2168P] 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 8736 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Pr1 Pr 0.351845(9) 0.236937(7) 0.165022(5) 0.01863(4) Uani 1 1 d . . . Al1 Al 0.83641(6) 0.18915(5) -0.02209(3) 0.03157(16) Uani 1 1 d . . . Al2 Al 0.84720(6) 0.14670(5) 0.35115(3) 0.02791(15) Uani 1 1 d . . . O1 O 0.16615(13) 0.17438(11) 0.20501(7) 0.0284(3) Uani 1 1 d . . . O2 O 0.34972(13) 0.19244(11) 0.27849(7) 0.0289(3) Uani 1 1 d . . . O3 O 0.53219(14) 0.27399(11) 0.23558(7) 0.0316(4) Uani 1 1 d . . . O4 O 0.51141(14) 0.33576(13) 0.12083(8) 0.0365(4) Uani 1 1 d . . . O5 O 0.41971(14) 0.20013(11) 0.05608(7) 0.0308(4) Uani 1 1 d . . . O6 O 0.25128(13) 0.10247(10) 0.10489(7) 0.0275(3) Uani 1 1 d . . . O7 O 0.19276(13) 0.30435(10) 0.09457(7) 0.0268(3) Uani 1 1 d . . . O8 O 0.47458(12) 0.09269(10) 0.18136(7) 0.0255(3) Uani 1 1 d . . . C1 C 0.1527(2) 0.18797(19) 0.26974(11) 0.0365(6) Uani 1 1 d . . . H1A H 0.0836 0.1567 0.2823 0.044 Uiso 1 1 calc R . . H1B H 0.1445 0.2536 0.2783 0.044 Uiso 1 1 calc R . . C2 C 0.2533(2) 0.15132(18) 0.30557(11) 0.0336(5) Uani 1 1 d . . . H2A H 0.2504 0.1681 0.3493 0.040 Uiso 1 1 calc R . . H2B H 0.2566 0.0844 0.3023 0.040 Uiso 1 1 calc R . . C3 C 0.4538(2) 0.18391(18) 0.31411(10) 0.0341(5) Uani 1 1 d . . . H3A H 0.4944 0.1282 0.3024 0.041 Uiso 1 1 calc R . . H3B H 0.4391 0.1806 0.3583 0.041 Uiso 1 1 calc R . . C4 C 0.5226(2) 0.26668(18) 0.30089(11) 0.0363(6) Uani 1 1 d . . . H4A H 0.4855 0.3215 0.3167 0.044 Uiso 1 1 calc R . . H4B H 0.5985 0.2615 0.3213 0.044 Uiso 1 1 calc R . . C5 C 0.5924(2) 0.35503(18) 0.22046(13) 0.0419(6) Uani 1 1 d . . . H5A H 0.6635 0.3594 0.2458 0.050 Uiso 1 1 calc R . . H5B H 0.5460 0.4093 0.2283 0.050 Uiso 1 1 calc R . . C6 C 0.6174(2) 0.34999(19) 0.15433(13) 0.0428(7) Uani 1 1 d . . . H6A H 0.6529 0.4071 0.1411 0.051 Uiso 1 1 calc R . . H6B H 0.6698 0.2992 0.1470 0.051 Uiso 1 1 calc R . . C7 C 0.5238(2) 0.3360(2) 0.05557(12) 0.0416(6) Uani 1 1 d . . . H7A H 0.5961 0.3649 0.0459 0.050 Uiso 1 1 calc R . . H7B H 0.4616 0.3710 0.0352 0.050 Uiso 1 1 calc R . . C8 C 0.5213(2) 0.2412(2) 0.03322(12) 0.0410(7) Uani 1 1 d . . . H8A H 0.5191 0.2398 -0.0121 0.049 Uiso 1 1 calc R . . H8B H 0.5892 0.2080 0.0488 0.049 Uiso 1 1 calc R . . C9 C 0.3967(2) 0.11086(17) 0.03350(11) 0.0384(6) Uani 1 1 d . . . H9A H 0.4427 0.0658 0.0571 0.046 Uiso 1 1 calc R . . H9B H 0.4151 0.1065 -0.0101 0.046 Uiso 1 1 calc R . . C10 C 0.2751(2) 0.09319(16) 0.04050(10) 0.0368(6) Uani 1 1 d . . . H10A H 0.2293 0.1371 0.0157 0.044 Uiso 1 1 calc R . . H10B H 0.2558 0.0312 0.0261 0.044 Uiso 1 1 calc R . . C11 C 0.1348(2) 0.08629(17) 0.11519(12) 0.0370(6) Uani 1 1 d . . . H11A H 0.1115 0.0263 0.0985 0.044 Uiso 1 1 calc R . . H11B H 0.0873 0.1336 0.0947 0.044 Uiso 1 1 calc R . . C12 C 0.1214(2) 0.08879(16) 0.18237(13) 0.0375(6) Uani 1 1 d . . . H12A H 0.0407 0.0834 0.1915 0.045 Uiso 1 1 calc R . . H12B H 0.1629 0.0377 0.2023 0.045 Uiso 1 1 calc R . . C13 C 0.3020(2) 0.38445(16) 0.21206(11) 0.0318(5) Uani 1 1 d . . . H13A H 0.2203 0.3870 0.2169 0.048 Uiso 1 1 calc R . . H13B H 0.3246 0.4343 0.1855 0.048 Uiso 1 1 calc R . . H13C H 0.3414 0.3902 0.2522 0.048 Uiso 1 1 calc R . . C14 C 0.2225(2) 0.36952(16) 0.04770(11) 0.0324(5) Uani 1 1 d . . . H14A H 0.2493 0.3378 0.0112 0.039 Uiso 1 1 calc R . . H14B H 0.2828 0.4108 0.0636 0.039 Uiso 1 1 calc R . . C15 C 0.1154(2) 0.42201(17) 0.03181(11) 0.0374(6) Uani 1 1 d . . . H15A H 0.0685 0.3907 -0.0003 0.045 Uiso 1 1 calc R . . H15B H 0.1324 0.4843 0.0179 0.045 Uiso 1 1 calc R . . C16 C 0.0583(2) 0.42290(16) 0.09238(11) 0.0339(5) Uani 1 1 d . . . H16A H 0.0928 0.4684 0.1208 0.041 Uiso 1 1 calc R . . H16B H -0.0236 0.4352 0.0867 0.041 Uiso 1 1 calc R . . C17 C 0.0802(2) 0.32767(16) 0.11478(12) 0.0326(5) Uani 1 1 d . . . H17A H 0.0782 0.3248 0.1600 0.039 Uiso 1 1 calc R . . H17B H 0.0228 0.2854 0.0969 0.039 Uiso 1 1 calc R . . C18 C 0.4313(2) 0.00557(16) 0.20087(12) 0.0336(5) Uani 1 1 d . . . H18A H 0.3821 -0.0215 0.1680 0.040 Uiso 1 1 calc R . . H18B H 0.3867 0.0132 0.2378 0.040 Uiso 1 1 calc R . . C19 C 0.5315(2) -0.05421(18) 0.21484(13) 0.0417(6) Uani 1 1 d . . . H19A H 0.5187 -0.1160 0.1982 0.050 Uiso 1 1 calc R . . H19B H 0.5481 -0.0584 0.2595 0.050 Uiso 1 1 calc R . . C20 C 0.6261(3) -0.00746(19) 0.1835(2) 0.0669(11) Uani 1 1 d . . . H20A H 0.6981 -0.0150 0.2076 0.080 Uiso 1 1 calc R . . H20B H 0.6348 -0.0335 0.1422 0.080 Uiso 1 1 calc R . . C21 C 0.5962(2) 0.0874(2) 0.17897(17) 0.0563(9) Uani 1 1 d . . . H21A H 0.6212 0.1132 0.1400 0.068 Uiso 1 1 calc R . . H21B H 0.6327 0.1219 0.2133 0.068 Uiso 1 1 calc R . . C22 C 0.8081(2) 0.1196(2) 0.05500(12) 0.0451(7) Uani 1 1 d . . . H22A H 0.8218 0.1593 0.0906 0.068 Uiso 1 1 calc R . . H22B H 0.8590 0.0673 0.0581 0.068 Uiso 1 1 calc R . . H22C H 0.7297 0.0985 0.0538 0.068 Uiso 1 1 calc R . . C23 C 0.9986(3) 0.1680(3) -0.04072(13) 0.0582(9) Uani 1 1 d . . . H23A H 1.0148 0.1976 -0.0795 0.087 Uiso 1 1 calc R . . H23B H 1.0125 0.1027 -0.0441 0.087 Uiso 1 1 calc R . . H23C H 1.0475 0.1934 -0.0077 0.087 Uiso 1 1 calc R . . C24 C 0.8119(2) 0.32366(18) -0.01198(12) 0.0383(6) Uani 1 1 d . . . H24A H 0.8227 0.3399 0.0313 0.057 Uiso 1 1 calc R . . H24B H 0.7350 0.3394 -0.0264 0.057 Uiso 1 1 calc R . . H24C H 0.8662 0.3570 -0.0359 0.057 Uiso 1 1 calc R . . C25 C 0.7315(3) 0.14813(18) -0.09157(13) 0.0485(7) Uani 1 1 d . . . H25A H 0.6588 0.1792 -0.0891 0.073 Uiso 1 1 calc R . . H25B H 0.7201 0.0824 -0.0888 0.073 Uiso 1 1 calc R . . H25C H 0.7646 0.1628 -0.1306 0.073 Uiso 1 1 calc R . . C26 C 0.8488(2) 0.1753(2) 0.26081(11) 0.0399(6) Uani 1 1 d . . . H26A H 0.7778 0.2049 0.2477 0.060 Uiso 1 1 calc R . . H26B H 0.8574 0.1190 0.2377 0.060 Uiso 1 1 calc R . . H26C H 0.9121 0.2160 0.2532 0.060 Uiso 1 1 calc R . . C27 C 0.7168(2) 0.06472(18) 0.36892(13) 0.0402(6) Uani 1 1 d . . . H27A H 0.7349 0.0298 0.4062 0.060 Uiso 1 1 calc R . . H27B H 0.7028 0.0230 0.3345 0.060 Uiso 1 1 calc R . . H27C H 0.6492 0.1015 0.3747 0.060 Uiso 1 1 calc R . . C28 C 0.98975(19) 0.08649(17) 0.38500(11) 0.0310(5) Uani 1 1 d . . . H28A H 1.0495 0.1321 0.3906 0.047 Uiso 1 1 calc R . . H28B H 1.0136 0.0399 0.3563 0.047 Uiso 1 1 calc R . . H28C H 0.9754 0.0583 0.4245 0.047 Uiso 1 1 calc R . . C29 C 0.8313(2) 0.26552(17) 0.39453(11) 0.0352(5) Uani 1 1 d . . . H29A H 0.8216 0.2545 0.4382 0.053 Uiso 1 1 calc R . . H29B H 0.7654 0.2981 0.3771 0.053 Uiso 1 1 calc R . . H29C H 0.8993 0.3021 0.3895 0.053 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 Pr1 0.01835(6) 0.01954(6) 0.01800(6) 0.00039(4) 0.00087(4) -0.00011(4) Al1 0.0318(4) 0.0365(4) 0.0260(3) -0.0050(3) -0.0028(3) 0.0065(3) Al2 0.0231(3) 0.0338(4) 0.0267(3) -0.0051(3) 0.0001(3) -0.0005(3) O1 0.0254(8) 0.0294(8) 0.0308(8) 0.0073(7) 0.0048(6) -0.0012(6) O2 0.0313(9) 0.0338(9) 0.0214(8) 0.0033(6) 0.0000(6) -0.0022(7) O3 0.0327(9) 0.0310(9) 0.0301(9) 0.0026(7) -0.0090(7) -0.0109(7) O4 0.0265(9) 0.0492(11) 0.0338(9) 0.0104(8) 0.0009(7) -0.0100(8) O5 0.0331(9) 0.0345(9) 0.0252(8) 0.0018(7) 0.0074(7) 0.0094(7) O6 0.0302(8) 0.0233(8) 0.0284(8) -0.0021(6) -0.0056(6) 0.0019(6) O7 0.0259(8) 0.0258(8) 0.0287(8) 0.0022(6) -0.0002(6) 0.0060(6) O8 0.0201(8) 0.0273(8) 0.0290(8) 0.0051(6) 0.0006(6) 0.0029(6) C1 0.0319(13) 0.0452(15) 0.0332(13) 0.0108(11) 0.0122(10) 0.0091(11) C2 0.0351(13) 0.0384(14) 0.0281(12) 0.0097(10) 0.0098(10) 0.0037(11) C3 0.0393(14) 0.0416(14) 0.0207(11) -0.0005(10) -0.0065(10) -0.0004(11) C4 0.0415(15) 0.0390(14) 0.0271(12) -0.0020(10) -0.0137(11) -0.0046(11) C5 0.0385(15) 0.0330(13) 0.0528(16) 0.0059(12) -0.0126(12) -0.0154(11) C6 0.0284(13) 0.0397(15) 0.0594(18) 0.0143(13) -0.0055(12) -0.0140(11) C7 0.0307(13) 0.0569(18) 0.0376(14) 0.0170(12) 0.0070(11) -0.0037(12) C8 0.0260(12) 0.0699(19) 0.0278(12) 0.0130(12) 0.0099(10) 0.0139(12) C9 0.0570(17) 0.0350(14) 0.0235(12) 0.0020(10) 0.0049(11) 0.0192(12) C10 0.0633(18) 0.0221(12) 0.0238(11) -0.0029(9) -0.0118(11) 0.0035(11) C11 0.0296(13) 0.0266(12) 0.0536(16) -0.0021(11) -0.0113(11) -0.0026(10) C12 0.0232(12) 0.0244(12) 0.0652(18) 0.0082(11) 0.0044(11) -0.0029(9) C13 0.0390(14) 0.0263(12) 0.0301(12) -0.0019(9) 0.0001(10) 0.0011(10) C14 0.0409(14) 0.0293(12) 0.0272(12) 0.0049(9) 0.0045(10) 0.0064(10) C15 0.0447(15) 0.0315(13) 0.0357(13) 0.0065(10) -0.0037(11) 0.0100(11) C16 0.0331(13) 0.0262(12) 0.0417(14) -0.0019(10) -0.0042(11) 0.0077(10) C17 0.0251(12) 0.0308(12) 0.0418(14) 0.0039(10) 0.0016(10) 0.0071(10) C18 0.0306(13) 0.0235(12) 0.0459(14) 0.0026(10) -0.0054(11) -0.0023(10) C19 0.0395(15) 0.0338(14) 0.0520(16) 0.0077(12) 0.0041(12) 0.0109(11) C20 0.0340(16) 0.0297(15) 0.138(3) 0.0002(18) 0.0191(18) 0.0080(12) C21 0.0245(14) 0.0576(19) 0.088(2) 0.0354(17) 0.0156(14) 0.0131(13) C22 0.0472(17) 0.0510(17) 0.0376(15) 0.0011(12) 0.0064(12) 0.0086(13) C23 0.0478(18) 0.094(3) 0.0334(15) 0.0197(15) 0.0069(13) 0.0323(17) C24 0.0376(14) 0.0385(14) 0.0385(14) -0.0110(11) -0.0013(11) -0.0042(11) C25 0.068(2) 0.0292(13) 0.0459(16) -0.0014(12) -0.0228(14) 0.0026(13) C26 0.0291(13) 0.0570(17) 0.0330(13) -0.0063(12) -0.0041(10) 0.0056(12) C27 0.0236(12) 0.0357(14) 0.0612(17) -0.0063(12) 0.0020(11) -0.0002(10) C28 0.0259(12) 0.0377(13) 0.0297(12) -0.0008(10) 0.0029(9) -0.0038(10) C29 0.0393(14) 0.0362(13) 0.0300(12) -0.0031(10) -0.0011(10) -0.0020(11) _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 Pr1 C13 2.487(2) . ? Pr1 O2 2.5673(15) . ? Pr1 O1 2.5761(15) . ? Pr1 O7 2.5809(14) . ? Pr1 O8 2.5917(15) . ? Pr1 O5 2.6050(15) . ? Pr1 O4 2.6072(16) . ? Pr1 O6 2.6339(15) . ? Pr1 O3 2.6383(15) . ? Al1 C23 2.008(3) . ? Al1 C25 2.013(3) . ? Al1 C22 2.013(3) . ? Al1 C24 2.016(3) . ? Al2 C29 2.004(3) . ? Al2 C27 2.014(3) . ? Al2 C28 2.020(2) . ? Al2 C26 2.021(3) . ? O1 C1 1.445(3) . ? O1 C12 1.447(3) . ? O2 C3 1.436(3) . ? O2 C2 1.444(3) . ? O3 C5 1.437(3) . ? O3 C4 1.441(3) . ? O4 C7 1.441(3) . ? O4 C6 1.442(3) . ? O5 C9 1.427(3) . ? O5 C8 1.456(3) . ? O6 C11 1.430(3) . ? O6 C10 1.455(3) . ? O7 C14 1.459(3) . ? O7 C17 1.466(3) . ? O8 C21 1.448(3) . ? O8 C18 1.453(3) . ? C1 C2 1.499(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.502(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.491(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.479(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.480(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.485(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.514(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.514(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.505(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.499(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.507(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.444(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Pr1 O2 79.09(7) . . ? C13 Pr1 O1 87.12(7) . . ? O2 Pr1 O1 62.32(5) . . ? C13 Pr1 O7 74.31(6) . . ? O2 Pr1 O7 129.55(5) . . ? O1 Pr1 O7 74.14(5) . . ? C13 Pr1 O8 143.33(6) . . ? O2 Pr1 O8 71.76(5) . . ? O1 Pr1 O8 98.24(5) . . ? O7 Pr1 O8 142.10(5) . . ? C13 Pr1 O5 130.45(7) . . ? O2 Pr1 O5 147.91(5) . . ? O1 Pr1 O5 122.64(5) . . ? O7 Pr1 O5 77.40(5) . . ? O8 Pr1 O5 76.16(5) . . ? C13 Pr1 O4 81.67(7) . . ? O2 Pr1 O4 122.63(5) . . ? O1 Pr1 O4 166.22(5) . . ? O7 Pr1 O4 95.01(5) . . ? O8 Pr1 O4 95.54(5) . . ? O5 Pr1 O4 61.22(6) . . ? C13 Pr1 O6 138.85(7) . . ? O2 Pr1 O6 105.47(5) . . ? O1 Pr1 O6 61.65(5) . . ? O7 Pr1 O6 71.86(5) . . ? O8 Pr1 O6 72.01(5) . . ? O5 Pr1 O6 62.51(5) . . ? O4 Pr1 O6 123.72(5) . . ? C13 Pr1 O3 77.23(7) . . ? O2 Pr1 O3 61.98(5) . . ? O1 Pr1 O3 123.97(5) . . ? O7 Pr1 O3 145.25(5) . . ? O8 Pr1 O3 69.71(5) . . ? O5 Pr1 O3 107.60(5) . . ? O4 Pr1 O3 61.19(5) . . ? O6 Pr1 O3 141.72(5) . . ? C23 Al1 C25 111.45(14) . . ? C23 Al1 C22 106.73(12) . . ? C25 Al1 C22 111.01(13) . . ? C23 Al1 C24 108.58(14) . . ? C25 Al1 C24 106.90(11) . . ? C22 Al1 C24 112.21(12) . . ? C29 Al2 C27 110.09(11) . . ? C29 Al2 C28 107.74(11) . . ? C27 Al2 C28 107.66(11) . . ? C29 Al2 C26 106.58(12) . . ? C27 Al2 C26 110.77(12) . . ? C28 Al2 C26 113.92(10) . . ? C1 O1 C12 113.65(19) . . ? C1 O1 Pr1 114.57(14) . . ? C12 O1 Pr1 120.12(14) . . ? C3 O2 C2 114.74(17) . . ? C3 O2 Pr1 120.09(13) . . ? C2 O2 Pr1 123.05(13) . . ? C5 O3 C4 110.60(18) . . ? C5 O3 Pr1 115.82(13) . . ? C4 O3 Pr1 117.78(14) . . ? C7 O4 C6 112.21(19) . . ? C7 O4 Pr1 118.40(14) . . ? C6 O4 Pr1 121.59(14) . . ? C9 O5 C8 114.37(19) . . ? C9 O5 Pr1 116.49(13) . . ? C8 O5 Pr1 121.42(14) . . ? C11 O6 C10 111.54(18) . . ? C11 O6 Pr1 117.79(13) . . ? C10 O6 Pr1 116.80(13) . . ? C14 O7 C17 108.03(16) . . ? C14 O7 Pr1 118.63(13) . . ? C17 O7 Pr1 124.19(13) . . ? C21 O8 C18 109.17(18) . . ? C21 O8 Pr1 126.41(15) . . ? C18 O8 Pr1 124.14(13) . . ? O1 C1 C2 110.02(19) . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O2 C2 C1 105.13(18) . . ? O2 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O2 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? O2 C3 C4 106.60(19) . . ? O2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? O2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? O3 C4 C3 108.59(18) . . ? O3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O3 C5 C6 107.7(2) . . ? O3 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? O3 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? O4 C6 C5 107.1(2) . . ? O4 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? O4 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? O4 C7 C8 108.9(2) . . ? O4 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O5 C8 C7 106.5(2) . . ? O5 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? O5 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? O5 C9 C10 107.38(19) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O6 C10 C9 108.38(19) . . ? O6 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O6 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? O6 C11 C12 107.33(19) . . ? O6 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O6 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O1 C12 C11 107.85(19) . . ? O1 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O1 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.5 . . ? Pr1 C13 H13A 109.5 . . ? Pr1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Pr1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O7 C14 C15 105.69(19) . . ? O7 C14 H14A 110.6 . . ? C15 C14 H14A 110.6 . . ? O7 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? C14 C15 C16 101.97(19) . . ? C14 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? C14 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.2 . . ? C17 C16 C15 101.48(19) . . ? C17 C16 H16A 111.5 . . ? C15 C16 H16A 111.5 . . ? C17 C16 H16B 111.5 . . ? C15 C16 H16B 111.5 . . ? H16A C16 H16B 109.3 . . ? O7 C17 C16 105.47(19) . . ? O7 C17 H17A 110.6 . . ? C16 C17 H17A 110.6 . . ? O7 C17 H17B 110.6 . . ? C16 C17 H17B 110.6 . . ? H17A C17 H17B 108.8 . . ? O8 C18 C19 106.96(19) . . ? O8 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? O8 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C18 C19 C20 103.8(2) . . ? C18 C19 H19A 111.0 . . ? C20 C19 H19A 111.0 . . ? C18 C19 H19B 111.0 . . ? C20 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? C21 C20 C19 106.7(2) . . ? C21 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? C21 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C20 C21 O8 106.9(2) . . ? C20 C21 H21A 110.3 . . ? O8 C21 H21A 110.3 . . ? C20 C21 H21B 110.3 . . ? O8 C21 H21B 110.3 . . ? H21A C21 H21B 108.6 . . ? Al1 C22 H22A 109.5 . . ? Al1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al1 C23 H23A 109.5 . . ? Al1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al1 C24 H24A 109.5 . . ? Al1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al1 C25 H25A 109.5 . . ? Al1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Al2 C26 H26A 109.5 . . ? Al2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Al2 C27 H27A 109.5 . . ? Al2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Al2 C28 H28A 109.5 . . ? Al2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Al2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Al2 C29 H29A 109.5 . . ? Al2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Al2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.882 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.069 #===END