# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Peter Roesky' _publ_contact_author_address ; Institut fur Chemie FU Beroin Fabechstr. 34-36 Berlin 14195 GERMANY ; _publ_contact_author_phone +49/(0)3083854004 _publ_contact_author_fax +49/(0)3083852440 _publ_contact_author_email ROESKY@CHEMIE.FU-BERLIN.DE _publ_section_title ; A pentanuclear yttrium hydroxo cluster as oxidation catalyst. Calaytic Oxidation of Aldehydes by air. ; loop_ _publ_author_name 'Peter Roesky' 'Graciela Canseco-Melchor' 'Agustino Zulys' data_grace2c _database_code_depnum_ccdc_archive 'CCDC 224900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C150 H115 O25 Y5' _chemical_formula_weight 2761.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7960 3.5670 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' _cell_length_a 19.466(4) _cell_length_b 19.466(4) _cell_length_c 18.530(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7021(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2819 _exptl_absorpt_coefficient_mu 2.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Stoe-IPDS _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30524 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.92 _reflns_number_total 6832 _reflns_number_gt 3378 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6832 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1867 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _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 C1 C 0.1652(3) -0.0109(3) 0.6107(4) 0.0644(17) Uani 1 1 d . . . C2 C 0.1240(4) -0.0357(4) 0.6659(5) 0.081(2) Uani 1 1 d . . . H2 H 0.1044 -0.0789 0.6594 0.097 Uiso 1 1 calc R . . C3 C 0.1094(3) -0.0015(3) 0.7301(4) 0.0695(19) Uani 1 1 d . . . C4 C 0.1752(3) -0.0509(3) 0.5417(4) 0.0704(19) Uani 1 1 d . . . C5 C 0.2130(4) -0.0217(4) 0.4862(5) 0.083(2) Uani 1 1 d . . . H5 H 0.2303 0.0225 0.4918 0.099 Uiso 1 1 calc R . . C6 C 0.2253(5) -0.0566(5) 0.4236(5) 0.098(3) Uani 1 1 d . . . H6 H 0.2507 -0.0361 0.3870 0.118 Uiso 1 1 calc R . . C7 C 0.1998(5) -0.1227(5) 0.4147(6) 0.107(3) Uani 1 1 d . . . H7 H 0.2083 -0.1467 0.3723 0.129 Uiso 1 1 calc R . . C8 C 0.1626(5) -0.1519(5) 0.4684(6) 0.108(3) Uani 1 1 d . . . H8 H 0.1455 -0.1962 0.4626 0.130 Uiso 1 1 calc R . . C9 C 0.1498(4) -0.1170(4) 0.5305(5) 0.094(2) Uani 1 1 d . . . H9 H 0.1236 -0.1377 0.5663 0.113 Uiso 1 1 calc R . . C10 C 0.0575(4) -0.0287(4) 0.7825(5) 0.092(3) Uani 1 1 d . . . C11 C 0.0391(6) -0.0982(6) 0.7811(7) 0.136(4) Uiso 1 1 d . . . H11 H 0.0608 -0.1287 0.7499 0.163 Uiso 1 1 calc R . . C12 C -0.0139(8) -0.1212(8) 0.8288(8) 0.170(5) Uiso 1 1 d . . . H12 H -0.0283 -0.1667 0.8284 0.204 Uiso 1 1 calc R . . C13 C -0.0419(8) -0.0764(8) 0.8731(8) 0.168(5) Uiso 1 1 d . . . H13 H -0.0775 -0.0919 0.9024 0.202 Uiso 1 1 calc R . . C14 C -0.0229(7) -0.0085(7) 0.8796(7) 0.152(4) Uiso 1 1 d . . . H14 H -0.0414 0.0205 0.9144 0.183 Uiso 1 1 calc R . . C15 C 0.0272(5) 0.0137(5) 0.8291(6) 0.106(3) Uiso 1 1 d . . . H15 H 0.0393 0.0599 0.8285 0.128 Uiso 1 1 calc R . . C16 C 0.3475(3) 0.0771(3) 0.5999(4) 0.0571(15) Uani 1 1 d . . . C17 C 0.3569(3) 0.0153(3) 0.6331(4) 0.0684(18) Uani 1 1 d . . . H17 H 0.3833 -0.0174 0.6092 0.082 Uiso 1 1 calc R . . C18 C 0.3292(3) -0.0028(3) 0.7020(4) 0.0649(17) Uani 1 1 d . . . C19 C 0.3687(3) 0.0859(3) 0.5227(4) 0.0636(16) Uani 1 1 d . . . C20 C 0.3429(4) 0.1408(4) 0.4842(4) 0.082(2) Uani 1 1 d . . . H20 H 0.3152 0.1730 0.5072 0.098 Uiso 1 1 calc R . . C21 C 0.3581(5) 0.1482(5) 0.4111(5) 0.105(3) Uani 1 1 d . . . H21 H 0.3396 0.1848 0.3854 0.126 Uiso 1 1 calc R . . C22 C 0.3996(5) 0.1024(6) 0.3772(5) 0.107(3) Uani 1 1 d . . . H22 H 0.4093 0.1073 0.3283 0.128 Uiso 1 1 calc R . . C23 C 0.4268(5) 0.0493(5) 0.4151(6) 0.109(3) Uani 1 1 d . . . H23 H 0.4557 0.0181 0.3923 0.130 Uiso 1 1 calc R . . C24 C 0.4120(4) 0.0415(4) 0.4868(5) 0.085(2) Uani 1 1 d . . . H24 H 0.4317 0.0053 0.5121 0.103 Uiso 1 1 calc R . . C25 C 0.3518(4) -0.0688(4) 0.7361(5) 0.086(2) Uani 1 1 d . . . C26 C 0.4158(5) -0.0967(5) 0.7242(5) 0.104(3) Uiso 1 1 d . . . H26 H 0.4456 -0.0754 0.6920 0.125 Uiso 1 1 calc R . . C27 C 0.4367(7) -0.1572(6) 0.7601(7) 0.137(4) Uiso 1 1 d . . . H27 H 0.4812 -0.1743 0.7561 0.164 Uiso 1 1 calc R . . C28 C 0.3909(8) -0.1871(8) 0.7983(8) 0.166(5) Uiso 1 1 d . . . H28 H 0.4037 -0.2295 0.8170 0.200 Uiso 1 1 calc R . . C29 C 0.3249(9) -0.1659(9) 0.8162(10) 0.198(6) Uiso 1 1 d . . . H29 H 0.2952 -0.1905 0.8457 0.238 Uiso 1 1 calc R . . C30 C 0.3081(6) -0.1000(6) 0.7826(6) 0.131(4) Uiso 1 1 d . . . H30 H 0.2664 -0.0791 0.7933 0.157 Uiso 1 1 calc R . . C31 C 0.1461(8) 0.3834(8) 0.9500(9) 0.078(4) Uiso 0.50 1 d P . . C32A C 0.3171(7) 0.3816(7) 0.9405(8) 0.068(3) Uiso 0.50 1 d P A 1 C33A C 0.3090(4) 0.4578(5) 0.9520(6) 0.108(8) Uiso 0.50 1 d PG A 1 C34A C 0.3586(4) 0.5070(7) 0.9676(9) 0.129(7) Uiso 0.50 1 d PG A 1 H34A H 0.4049 0.4952 0.9669 0.155 Uiso 0.50 1 calc PR A 1 C35A C 0.3391(7) 0.5739(6) 0.9841(7) 0.145(8) Uiso 0.50 1 d PG A 1 H35A H 0.3723 0.6068 0.9945 0.174 Uiso 0.50 1 calc PR A 1 C36A C 0.2699(7) 0.5915(4) 0.9851(8) 0.153(9) Uiso 0.50 1 d PG A 1 H36A H 0.2568 0.6363 0.9961 0.184 Uiso 0.50 1 calc PR A 1 C37A C 0.2203(5) 0.5424(4) 0.9696(8) 0.145(8) Uiso 0.50 1 d PG A 1 H37A H 0.1740 0.5542 0.9702 0.173 Uiso 0.50 1 calc PR A 1 C38A C 0.2398(4) 0.4755(4) 0.9530(4) 0.055(3) Uiso 0.50 1 d PG A 1 H38A H 0.2066 0.4426 0.9427 0.066 Uiso 0.50 1 calc PR A 1 C32B C 0.2158(5) 0.3967(4) 0.9421(6) 0.063(3) Uiso 0.50 1 d PG A 2 C33B C 0.2449(2) 0.45962(11) 0.98026(14) 0.136(8) Uiso 0.50 1 d PG A 2 C34B C 0.3092(2) 0.47426(11) 0.95159(14) 0.140(11) Uiso 0.50 1 d PG A 2 H34B H 0.3349 0.4396 0.9300 0.167 Uiso 0.50 1 calc PR A 2 C35B C 0.3352(2) 0.54067(12) 0.95526(17) 0.162(10) Uiso 0.50 1 d PG A 2 H35B H 0.3783 0.5505 0.9361 0.194 Uiso 0.50 1 calc PR A 2 C36B C 0.2969(3) 0.59245(12) 0.98759(19) 0.111(6) Uiso 0.50 1 d PG A 2 H36B H 0.3143 0.6369 0.9900 0.133 Uiso 0.50 1 calc PR A 2 C37B C 0.2325(3) 0.57781(12) 1.01626(19) 0.122(7) Uiso 0.50 1 d PG A 2 H37B H 0.2069 0.6125 1.0379 0.147 Uiso 0.50 1 calc PR A 2 C38B C 0.2065(2) 0.51140(13) 1.01260(17) 0.109(6) Uiso 0.50 1 d PG A 2 H38B H 0.1635 0.5016 1.0318 0.131 Uiso 0.50 1 calc PR A 2 O1 O 0.19456(7) 0.04683(4) 0.61280(5) 0.0646(11) Uani 1 1 d G . . O2 O 0.13472(8) 0.05668(7) 0.74725(8) 0.0680(12) Uani 1 1 d G . . O3 O 0.31817(6) 0.13039(8) 0.63036(8) 0.0546(10) Uani 1 1 d G . . O4 O 0.28572(9) 0.03145(5) 0.73644(9) 0.0647(11) Uani 1 1 d G . . O5 O 0.26293(15) 0.35128(9) 0.92119(9) 0.0720(12) Uani 1 1 d G . . O6 O 0.25000(11) 0.25000(4) 0.67180(5) 0.0528(18) Uani 1 4 d SG . . O7 O 0.30253(5) 0.16543(6) 0.78089(7) 0.0521(9) Uani 1 1 d G . . Y1 Y 0.21864(3) 0.12476(2) 0.70093(3) 0.05200(19) Uani 1 1 d G A . Y2 Y 0.25000(10) 0.25000(6) 0.85711(5) 0.0530(3) Uani 1 4 d SG . . 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 C1 0.059(4) 0.047(3) 0.087(5) -0.007(3) -0.018(3) -0.003(3) C2 0.089(5) 0.055(4) 0.098(6) 0.001(4) -0.009(5) -0.017(3) C3 0.059(4) 0.059(4) 0.091(6) 0.015(4) -0.005(4) -0.009(3) C4 0.062(4) 0.054(4) 0.095(6) -0.010(4) -0.021(4) 0.000(3) C5 0.091(5) 0.067(4) 0.091(6) -0.012(4) -0.013(5) -0.002(4) C6 0.117(7) 0.094(6) 0.084(6) -0.012(5) -0.012(5) -0.002(5) C7 0.125(8) 0.097(7) 0.099(8) -0.033(6) -0.023(6) 0.018(6) C8 0.119(7) 0.080(6) 0.125(9) -0.041(6) -0.017(6) -0.009(5) C9 0.097(6) 0.067(4) 0.117(7) -0.017(5) -0.009(5) -0.015(4) C10 0.092(5) 0.077(5) 0.109(7) 0.019(5) -0.008(5) -0.031(4) C16 0.045(3) 0.053(3) 0.074(5) -0.014(3) -0.002(3) 0.006(2) C17 0.068(4) 0.054(4) 0.084(5) -0.008(3) 0.003(4) 0.010(3) C18 0.066(4) 0.049(3) 0.080(5) -0.005(3) -0.015(4) 0.007(3) C19 0.063(4) 0.061(4) 0.067(5) -0.005(3) 0.001(3) -0.001(3) C20 0.086(5) 0.091(5) 0.068(5) -0.010(4) 0.006(4) 0.016(4) C21 0.107(7) 0.120(7) 0.087(7) 0.018(6) -0.002(5) 0.010(5) C22 0.118(7) 0.127(8) 0.075(6) -0.021(6) 0.027(5) -0.003(6) C23 0.133(8) 0.094(6) 0.098(8) -0.024(6) 0.034(6) 0.004(6) C24 0.097(6) 0.072(4) 0.087(6) -0.014(4) 0.024(5) 0.004(4) C25 0.102(6) 0.071(4) 0.084(6) 0.005(4) 0.004(5) 0.021(4) O1 0.064(2) 0.051(2) 0.079(3) -0.010(2) -0.009(2) -0.0072(19) O2 0.067(3) 0.059(2) 0.078(3) 0.006(2) 0.002(2) -0.013(2) O3 0.052(2) 0.049(2) 0.063(3) -0.0049(19) 0.0047(19) 0.0001(17) O4 0.072(3) 0.048(2) 0.074(3) 0.001(2) 0.002(2) 0.008(2) O5 0.066(3) 0.072(3) 0.078(3) -0.021(2) 0.001(2) -0.003(2) O6 0.050(3) 0.050(3) 0.059(5) 0.000 0.000 0.000 O7 0.049(2) 0.049(2) 0.058(2) 0.0025(18) -0.0002(18) -0.0010(16) Y1 0.0473(3) 0.0446(3) 0.0641(4) -0.0018(3) -0.0001(3) -0.0011(2) Y2 0.0511(4) 0.0511(4) 0.0569(8) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.262(6) . ? C1 C2 1.386(10) . ? C1 C4 1.511(10) . ? C2 C3 1.394(11) . ? C3 O2 1.276(7) . ? C3 C10 1.497(10) . ? C4 C5 1.385(11) . ? C4 C9 1.394(9) . ? C5 C6 1.365(11) . ? C6 C7 1.388(12) . ? C7 C8 1.356(13) . ? C8 C9 1.359(12) . ? C10 C15 1.333(12) . ? C10 C11 1.399(13) . ? C11 C12 1.430(17) . ? C12 C13 1.316(18) . ? C13 C14 1.378(17) . ? C14 C15 1.418(15) . ? C16 O3 1.311(6) . ? C16 C17 1.363(9) . ? C16 C19 1.499(9) . ? C17 C18 1.432(10) . ? C18 O4 1.251(7) . ? C18 C25 1.497(9) . ? C19 C24 1.377(9) . ? C19 C20 1.379(10) . ? C20 C21 1.395(11) . ? C21 C22 1.357(12) . ? C22 C23 1.357(13) . ? C23 C24 1.367(12) . ? C25 C30 1.354(13) . ? C25 C26 1.377(11) . ? C26 C27 1.413(14) . ? C27 C28 1.280(16) . ? C28 C29 1.389(19) . ? C29 C30 1.463(19) . ? C31 C32B 1.389(17) . ? C31 C32A 1.411(19) 2 ? C32A O5 1.260(14) . ? C32A C31 1.411(19) 4 ? C32A C33A 1.508(16) . ? C33A C34A 1.3900 . ? C33A C38A 1.3900 . ? C34A C35A 1.3900 . ? C35A C36A 1.3900 . ? C36A C37A 1.3900 . ? C37A C38A 1.3900 . ? C32B O5 1.331(11) . ? C32B C33B 1.523(8) . ? C33B C34B 1.3900 . ? C33B C38B 1.3900 . ? C34B C35B 1.3900 . ? C35B C36B 1.3900 . ? C36B C37B 1.3900 . ? C37B C38B 1.3900 . ? O1 Y1 2.2777 . ? O2 Y1 2.2720 . ? O3 Y1 2.3402 . ? O3 Y1 2.428(3) 2 ? O4 Y1 2.3318 . ? O5 Y2 2.3151 . ? O6 Y1 2.5705 2 ? O6 Y1 2.5705 . ? O6 Y1 2.5705 3 ? O6 Y1 2.5705 4 ? O7 Y1 2.296(2) 2 ? O7 Y1 2.3428 . ? O7 Y2 2.3979 . ? Y1 O7 2.2959(14) 4 ? Y1 O3 2.4280(14) 4 ? Y1 Y1 3.554(3) 2 ? Y1 Y1 3.554(3) 4 ? Y1 Y2 3.8328 . ? Y2 O5 2.315(3) 2 ? Y2 O5 2.315(3) 3 ? Y2 O5 2.315(3) 4 ? Y2 O7 2.398(2) 3 ? Y2 O7 2.3979(13) 4 ? Y2 O7 2.3979(15) 2 ? Y2 Y1 3.8328 4 ? Y2 Y1 3.8328 3 ? Y2 Y1 3.8328 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 123.4(6) . . ? O1 C1 C4 115.2(6) . . ? C2 C1 C4 121.3(6) . . ? C1 C2 C3 125.6(6) . . ? O2 C3 C2 123.9(6) . . ? O2 C3 C10 114.5(7) . . ? C2 C3 C10 121.5(6) . . ? C5 C4 C9 117.1(8) . . ? C5 C4 C1 119.1(6) . . ? C9 C4 C1 123.7(8) . . ? C6 C5 C4 121.3(8) . . ? C5 C6 C7 119.9(10) . . ? C8 C7 C6 119.5(9) . . ? C7 C8 C9 120.6(9) . . ? C8 C9 C4 121.5(9) . . ? C15 C10 C11 119.8(9) . . ? C15 C10 C3 120.0(8) . . ? C11 C10 C3 120.2(9) . . ? C10 C11 C12 118.4(13) . . ? C13 C12 C11 118.5(16) . . ? C12 C13 C14 125.3(17) . . ? C13 C14 C15 114.8(13) . . ? C10 C15 C14 122.9(11) . . ? O3 C16 C17 124.2(6) . . ? O3 C16 C19 116.2(5) . . ? C17 C16 C19 119.6(6) . . ? C16 C17 C18 124.7(6) . . ? O4 C18 C17 125.3(5) . . ? O4 C18 C25 116.2(6) . . ? C17 C18 C25 118.5(6) . . ? C24 C19 C20 117.4(7) . . ? C24 C19 C16 123.9(6) . . ? C20 C19 C16 118.7(6) . . ? C19 C20 C21 120.3(7) . . ? C22 C21 C20 120.5(9) . . ? C23 C22 C21 119.5(9) . . ? C22 C23 C24 120.4(8) . . ? C23 C24 C19 121.9(8) . . ? C30 C25 C26 119.5(9) . . ? C30 C25 C18 118.0(8) . . ? C26 C25 C18 122.5(8) . . ? C25 C26 C27 121.0(10) . . ? C28 C27 C26 116.0(13) . . ? C27 C28 C29 129.9(17) . . ? C28 C29 C30 111.5(16) . . ? C25 C30 C29 121.6(13) . . ? C32B C31 C32A 122.1(12) . 2 ? O5 C32A C31 128.5(12) . 4 ? O5 C32A C33A 114.5(10) . . ? C31 C32A C33A 117.0(11) 4 . ? C34A C33A C38A 120.0 . . ? C34A C33A C32A 129.4(7) . . ? C38A C33A C32A 110.3(7) . . ? C33A C34A C35A 120.0 . . ? C36A C35A C34A 120.0 . . ? C37A C36A C35A 120.0 . . ? C36A C37A C38A 120.0 . . ? C37A C38A C33A 120.0 . . ? O5 C32B C31 125.4(9) . . ? O5 C32B C33B 114.4(7) . . ? C31 C32B C33B 117.6(10) . . ? C34B C33B C38B 120.0 . . ? C34B C33B C32B 108.8(4) . . ? C38B C33B C32B 125.7(4) . . ? C35B C34B C33B 120.0 . . ? C36B C35B C34B 120.0 . . ? C35B C36B C37B 120.0 . . ? C38B C37B C36B 120.0 . . ? C37B C38B C33B 120.0 . . ? C1 O1 Y1 135.1(4) . . ? C3 O2 Y1 134.6(4) . . ? C16 O3 Y1 124.3(3) . . ? C16 O3 Y1 126.3(3) . 2 ? Y1 O3 Y1 96.4 . 2 ? C18 O4 Y1 130.5(3) . . ? C32A O5 C32B 100.5(7) . . ? C32A O5 Y2 129.5(6) . . ? C32B O5 Y2 129.8(4) . . ? Y1 O6 Y1 87.47(8) 2 . ? Y1 O6 Y1 87.47(8) 2 3 ? Y1 O6 Y1 155.8 . 3 ? Y1 O6 Y1 155.8 2 4 ? Y1 O6 Y1 87.47(8) . 4 ? Y1 O6 Y1 87.47(8) 3 4 ? Y1 O7 Y1 100.0 2 . ? Y1 O7 Y2 109.47(7) 2 . ? Y1 O7 Y2 107.9 . . ? O2 Y1 O1 74.6 . . ? O2 Y1 O7 78.0 . 4 ? O1 Y1 O7 141.3 . 4 ? O2 Y1 O4 80.9 . . ? O1 Y1 O4 78.4 . . ? O7 Y1 O4 123.4 4 . ? O2 Y1 O3 146.5 . . ? O1 Y1 O3 78.5 . . ? O7 Y1 O3 134.9 4 . ? O4 Y1 O3 74.4 . . ? O2 Y1 O7 117.3 . . ? O1 Y1 O7 145.3 . . ? O7 Y1 O7 72.4 4 . ? O4 Y1 O7 72.2 . . ? O3 Y1 O7 76.1 . . ? O2 Y1 O3 87.81(5) . 4 ? O1 Y1 O3 76.87(5) . 4 ? O7 Y1 O3 75.31(6) 4 4 ? O4 Y1 O3 154.77(6) . 4 ? O3 Y1 O3 105.3 . 4 ? O7 Y1 O3 132.78(6) . 4 ? O2 Y1 O6 143.5 . . ? O1 Y1 O6 122.0 . . ? O7 Y1 O6 70.0 4 . ? O4 Y1 O6 131.7 . . ? O3 Y1 O6 69.0 . . ? O7 Y1 O6 69.3 . . ? O3 Y1 O6 67.73(6) 4 . ? O2 Y1 Y1 156.4 . 2 ? O1 Y1 Y1 121.3 . 2 ? O7 Y1 Y1 94.0 4 2 ? O4 Y1 Y1 85.4 . 2 ? O3 Y1 Y1 42.8 . 2 ? O7 Y1 Y1 39.5 . 2 ? O3 Y1 Y1 111.8 4 2 ? O6 Y1 Y1 46.3 . 2 ? O2 Y1 Y1 97.5 . 4 ? O1 Y1 Y1 117.7 . 4 ? O7 Y1 Y1 40.5 4 4 ? O4 Y1 Y1 162.9 . 4 ? O3 Y1 Y1 112.7 . 4 ? O7 Y1 Y1 93.9 . 4 ? O3 Y1 Y1 40.9 4 4 ? O6 Y1 Y1 46.3 . 4 ? Y1 Y1 Y1 90.0 2 4 ? O2 Y1 Y2 101.6 . . ? O1 Y1 Y2 176.2 . . ? O7 Y1 Y2 36.1 4 . ? O4 Y1 Y2 101.1 . . ? O3 Y1 Y2 105.1 . . ? O7 Y1 Y2 36.5 . . ? O3 Y1 Y2 103.20(5) 4 . ? O6 Y1 Y2 61.2 . . ? Y1 Y1 Y2 62.4 2 . ? Y1 Y1 Y2 62.4 4 . ? O5 Y2 O5 74.75(8) 2 . ? O5 Y2 O5 74.75(6) 2 3 ? O5 Y2 O5 118.3 . 3 ? O5 Y2 O5 118.3 2 4 ? O5 Y2 O5 74.75(7) . 4 ? O5 Y2 O5 74.75(6) 3 4 ? O5 Y2 O7 82.20(13) 2 3 ? O5 Y2 O7 76.3 . 3 ? O5 Y2 O7 147.17(17) 3 3 ? O5 Y2 O7 137.72(14) 4 3 ? O5 Y2 O7 76.3 2 4 ? O5 Y2 O7 137.7 . 4 ? O5 Y2 O7 82.20(11) 3 4 ? O5 Y2 O7 147.17(8) 4 4 ? O7 Y2 O7 69.70(5) 3 4 ? O5 Y2 O7 147.17(13) 2 2 ? O5 Y2 O7 82.20(7) . 2 ? O5 Y2 O7 137.72(16) 3 2 ? O5 Y2 O7 76.34(9) 4 2 ? O7 Y2 O7 69.70(5) 3 2 ? O7 Y2 O7 107.8 4 2 ? O5 Y2 O7 137.72(8) 2 . ? O5 Y2 O7 147.2 . . ? O5 Y2 O7 76.34(9) 3 . ? O5 Y2 O7 82.20(6) 4 . ? O7 Y2 O7 107.8 3 . ? O7 Y2 O7 69.7 4 . ? O7 Y2 O7 69.70(8) 2 . ? O5 Y2 Y1 80.1 2 4 ? O5 Y2 Y1 108.71(5) . 4 ? O5 Y2 Y1 116.98(10) 3 4 ? O5 Y2 Y1 161.12(6) 4 4 ? O7 Y2 Y1 34.4 3 4 ? O7 Y2 Y1 35.6 4 4 ? O7 Y2 Y1 85.6 2 4 ? O7 Y2 Y1 86.3 . 4 ? O5 Y2 Y1 116.98(12) 2 3 ? O5 Y2 Y1 80.1 . 3 ? O5 Y2 Y1 161.12(6) 3 3 ? O5 Y2 Y1 108.71(11) 4 3 ? O7 Y2 Y1 35.6 3 3 ? O7 Y2 Y1 86.3 4 3 ? O7 Y2 Y1 34.39(7) 2 3 ? O7 Y2 Y1 85.64(6) . 3 ? Y1 Y2 Y1 55.2 4 3 ? O5 Y2 Y1 108.71(6) 2 . ? O5 Y2 Y1 161.1 . . ? O5 Y2 Y1 80.1 3 . ? O5 Y2 Y1 116.98(6) 4 . ? O7 Y2 Y1 85.6 3 . ? O7 Y2 Y1 34.4 4 . ? O7 Y2 Y1 86.32(6) 2 . ? O7 Y2 Y1 35.6 . . ? Y1 Y2 Y1 55.2 4 . ? Y1 Y2 Y1 81.9 3 . ? O5 Y2 Y1 161.1 2 2 ? O5 Y2 Y1 116.98(5) . 2 ? O5 Y2 Y1 108.71(10) 3 2 ? O5 Y2 Y1 80.1 4 2 ? O7 Y2 Y1 86.3 3 2 ? O7 Y2 Y1 85.6 4 2 ? O7 Y2 Y1 35.6 2 2 ? O7 Y2 Y1 34.39(5) . 2 ? Y1 Y2 Y1 81.9 4 2 ? Y1 Y2 Y1 55.2 3 2 ? Y1 Y2 Y1 55.2 . 2 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.899 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.094 #==============================================================================