# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1798 #Authors: Joseph W. Ziller, Jerome Gromada, Thomas Chenal, Andre Mortreux, #Jean-Francois Carpentier #contact email: Jean-Francois.Carpentier@ensc-lille.fr or #jziller@uci.edu #contact author: Jean-Francois Carpentier #Charge de recherche au CNRS #Laboratoire de Catalyse de Lille #UPRESA CNRS 8010 #ENSCL - BP 108 #59652 Villeneuve d'Ascq Cedex #France #phone: 33 (0)320 436 754 #email: carpentier@ensc-lille.fr data_rhodia1 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H105 Nd3 O12' _chemical_formula_weight 1307.04 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.0538(10) _cell_length_b 20.0343(12) _cell_length_c 17.7400(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6061.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description multi-faceted-polyhedra _exptl_crystal_colour pale_blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 2.581 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6132 _exptl_absorpt_correction_T_max 0.6398 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 38059 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7315 _reflns_number_gt 5589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+27.9838P] 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 7315 _refine_ls_number_parameters 213 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 0.011850(15) 0.287905(13) 0.148274(15) 0.02952(9) Uani 1 1 d . . . Nd2 Nd 0.0000 0.126072(17) 0.2500 0.02492(9) Uani 1 2 d S . . O1 O -0.07759(19) 0.23859(17) 0.23738(19) 0.0295(7) Uani 1 1 d . . . O2 O 0.0220(2) 0.17375(17) 0.12410(19) 0.0324(7) Uani 1 1 d . . . O3 O -0.0598(2) 0.32754(19) 0.0594(2) 0.0443(9) Uani 1 1 d . . . O4 O -0.0947(2) 0.05658(18) 0.2295(2) 0.0375(8) Uani 1 1 d . . . O5 O 0.0000 0.3662(2) 0.2500 0.0375(11) Uani 1 2 d S . . C1 C -0.1611(3) 0.2377(3) 0.2266(3) 0.0348(11) Uiso 1 1 d . . . C2 C -0.1993(4) 0.2008(3) 0.2922(3) 0.0449(13) Uiso 1 1 d . . . H2A H -0.1862 0.2233 0.3396 0.067 Uiso 1 1 calc R . . H2B H -0.1799 0.1548 0.2937 0.067 Uiso 1 1 calc R . . H2C H -0.2563 0.2005 0.2854 0.067 Uiso 1 1 calc R . . C3 C -0.1810(3) 0.2022(3) 0.1526(3) 0.0407(12) Uiso 1 1 d . . . H3A H -0.1571 0.2263 0.1105 0.061 Uiso 1 1 calc R . . H3B H -0.2381 0.2011 0.1461 0.061 Uiso 1 1 calc R . . H3C H -0.1606 0.1565 0.1541 0.061 Uiso 1 1 calc R . . C4 C -0.1903(4) 0.3097(3) 0.2230(4) 0.0500(14) Uiso 1 1 d . . . H4A H -0.1652 0.3327 0.1806 0.075 Uiso 1 1 calc R . . H4B H -0.1770 0.3327 0.2701 0.075 Uiso 1 1 calc R . . H4C H -0.2473 0.3100 0.2160 0.075 Uiso 1 1 calc R . . C5 C 0.0346(3) 0.1372(3) 0.0559(3) 0.0355(11) Uiso 1 1 d . . . C6 C 0.0823(4) 0.1800(3) 0.0018(4) 0.0508(15) Uiso 1 1 d . . . H6A H 0.0534 0.2211 -0.0095 0.076 Uiso 1 1 calc R . . H6B H 0.0916 0.1552 -0.0449 0.076 Uiso 1 1 calc R . . H6C H 0.1327 0.1914 0.0251 0.076 Uiso 1 1 calc R . . C7 C -0.0436(4) 0.1207(3) 0.0197(4) 0.0526(15) Uiso 1 1 d . . . H7A H -0.0715 0.1621 0.0076 0.079 Uiso 1 1 calc R . . H7B H -0.0752 0.0940 0.0547 0.079 Uiso 1 1 calc R . . H7C H -0.0347 0.0952 -0.0267 0.079 Uiso 1 1 calc R . . C8 C 0.0789(4) 0.0724(3) 0.0738(4) 0.0539(16) Uiso 1 1 d . . . H8A H 0.0477 0.0453 0.1086 0.081 Uiso 1 1 calc R . . H8B H 0.1295 0.0831 0.0970 0.081 Uiso 1 1 calc R . . H8C H 0.0877 0.0474 0.0270 0.081 Uiso 1 1 calc R . . C9 C -0.1078(4) 0.3513(4) -0.0005(4) 0.0555(16) Uiso 1 1 d . . . C10 C -0.1854(5) 0.3733(5) 0.0299(5) 0.084(3) Uiso 1 1 d . . . H10A H -0.2118 0.3354 0.0539 0.126 Uiso 1 1 calc R . . H10B H -0.2179 0.3903 -0.0114 0.126 Uiso 1 1 calc R . . H10C H -0.1773 0.4088 0.0673 0.126 Uiso 1 1 calc R . . C11 C -0.1175(7) 0.2980(5) -0.0574(6) 0.108(3) Uiso 1 1 d . . . H11A H -0.1426 0.2591 -0.0341 0.162 Uiso 1 1 calc R . . H11B H -0.0660 0.2851 -0.0772 0.162 Uiso 1 1 calc R . . H11C H -0.1503 0.3144 -0.0988 0.162 Uiso 1 1 calc R . . C12 C -0.0691(6) 0.4120(5) -0.0369(6) 0.092(3) Uiso 1 1 d . . . H12A H -0.0643 0.4478 0.0004 0.137 Uiso 1 1 calc R . . H12B H -0.1014 0.4274 -0.0792 0.137 Uiso 1 1 calc R . . H12C H -0.0169 0.3997 -0.0554 0.137 Uiso 1 1 calc R . . C13 C -0.1439(4) 0.0006(3) 0.2203(4) 0.0485(14) Uiso 1 1 d . . . C14 C -0.1265(6) -0.0515(5) 0.2819(5) 0.089(3) Uiso 1 1 d . . . H14A H -0.0726 -0.0676 0.2764 0.134 Uiso 1 1 calc R . . H14B H -0.1630 -0.0890 0.2769 0.134 Uiso 1 1 calc R . . H14C H -0.1330 -0.0309 0.3316 0.134 Uiso 1 1 calc R . . C15 C -0.1319(7) -0.0310(5) 0.1477(6) 0.108(3) Uiso 1 1 d . . . H15A H -0.1429 0.0012 0.1075 0.163 Uiso 1 1 calc R . . H15B H -0.1672 -0.0693 0.1428 0.163 Uiso 1 1 calc R . . H15C H -0.0774 -0.0462 0.1437 0.163 Uiso 1 1 calc R . . C16 C -0.2260(7) 0.0181(6) 0.2366(6) 0.114(4) Uiso 1 1 d . . . H16A H -0.2443 0.0512 0.1999 0.172 Uiso 1 1 calc R . . H16B H -0.2297 0.0369 0.2875 0.172 Uiso 1 1 calc R . . H16C H -0.2587 -0.0220 0.2333 0.172 Uiso 1 1 calc R . . C17 C 0.0000 0.4382(4) 0.2500 0.0415(17) Uiso 1 2 d S . . C18 C -0.0502(8) 0.4652(7) 0.1822(8) 0.054(3) Uiso 0.50 1 d P . . C19 C 0.0800(11) 0.4630(9) 0.2496(10) 0.081(5) Uiso 0.50 1 d P . . C20 C -0.0492(9) 0.4592(8) 0.3201(9) 0.068(4) Uiso 0.50 1 d P . . O6 O 0.1351(3) 0.3390(2) 0.0766(2) 0.0515(11) Uani 1 1 d D . . C21 C 0.2178(7) 0.3663(7) 0.0942(8) 0.055(3) Uiso 0.50 1 d PD A 1 H21A H 0.2590 0.3324 0.0853 0.066 Uiso 0.50 1 calc PR A 1 H21B H 0.2218 0.3832 0.1465 0.066 Uiso 0.50 1 calc PR A 1 C22 C 0.2217(10) 0.4248(9) 0.0346(9) 0.073(4) Uiso 0.50 1 d PD A 1 H22A H 0.2069 0.4678 0.0581 0.087 Uiso 0.50 1 calc PR A 1 H22B H 0.2753 0.4289 0.0137 0.087 Uiso 0.50 1 calc PR A 1 C23 C 0.1679(8) 0.4074(7) -0.0226(8) 0.051(3) Uiso 0.50 1 d PD A 1 H23A H 0.1955 0.4049 -0.0716 0.062 Uiso 0.50 1 calc PR A 1 H23B H 0.1269 0.4422 -0.0264 0.062 Uiso 0.50 1 calc PR A 1 C24 C 0.1306(7) 0.3419(6) -0.0059(7) 0.050(3) Uiso 0.50 1 d PD A 1 H24A H 0.0755 0.3407 -0.0235 0.060 Uiso 0.50 1 calc PR A 1 H24B H 0.1600 0.3047 -0.0294 0.060 Uiso 0.50 1 calc PR A 1 C21B C 0.2110(10) 0.3246(9) 0.0590(10) 0.075(4) Uiso 0.50 1 d P A 2 H21C H 0.2127 0.2892 0.0202 0.090 Uiso 0.50 1 calc PR A 2 H21D H 0.2387 0.3082 0.1044 0.090 Uiso 0.50 1 calc PR A 2 C22B C 0.2505(9) 0.3859(8) 0.0301(9) 0.062(4) Uiso 0.50 1 d P A 2 H22C H 0.2872 0.3750 -0.0114 0.075 Uiso 0.50 1 calc PR A 2 H22D H 0.2796 0.4090 0.0707 0.075 Uiso 0.50 1 calc PR A 2 C23B C 0.183(3) 0.428(3) 0.002(3) 0.26(3) Uiso 0.50 1 d P A 2 H23C H 0.1898 0.4753 0.0165 0.316 Uiso 0.50 1 calc PR A 2 H23D H 0.1781 0.4251 -0.0535 0.316 Uiso 0.50 1 calc PR A 2 C24B C 0.1170(12) 0.4015(9) 0.0365(11) 0.086(5) Uiso 0.50 1 d P A 2 H24C H 0.0763 0.3927 -0.0021 0.104 Uiso 0.50 1 calc PR A 2 H24D H 0.0955 0.4344 0.0727 0.104 Uiso 0.50 1 calc PR A 2 O40 O -0.0972(18) 0.3213(13) -0.3195(17) 0.110(11) Uiso 0.25 1 d PD B 1 C41 C -0.107(3) 0.2466(17) -0.338(3) 0.14(2) Uiso 0.25 1 d PD B 1 C42 C -0.0373(17) 0.2109(12) -0.2952(16) 0.062(7) Uiso 0.25 1 d PD . 1 C43 C -0.038(2) 0.2550(14) -0.2359(16) 0.100 Uiso 0.25 1 d PD . 1 C44 C -0.036(2) 0.3254(13) -0.2642(19) 0.075(10) Uiso 0.25 1 d PD . 1 O41 O -0.0741(12) 0.2505(10) -0.2942(15) 0.096(8) Uiso 0.25 1 d PD . 2 C45 C 0.0000 0.2268(12) -0.2500 0.111(11) Uiso 0.50 2 d SPD . 2 C46 C 0.0357(12) 0.2944(11) -0.2220(13) 0.042(5) Uiso 0.25 1 d PD . 2 C47 C -0.0189(12) 0.3416(10) -0.2436(16) 0.048(6) Uiso 0.25 1 d PD . 2 C48 C -0.0841(14) 0.3214(11) -0.2914(16) 0.047(6) Uiso 0.25 1 d PD . 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 Nd1 0.03148(14) 0.02784(14) 0.02924(14) 0.00439(10) 0.00397(10) 0.00252(10) Nd2 0.02644(17) 0.02453(17) 0.02381(17) 0.000 0.00163(12) 0.000 O1 0.0259(16) 0.0278(16) 0.0347(19) 0.0001(14) 0.0030(13) -0.0012(13) O2 0.0395(19) 0.0318(18) 0.0258(16) -0.0002(14) 0.0025(14) 0.0052(15) O3 0.048(2) 0.041(2) 0.044(2) 0.0138(18) -0.0001(17) 0.0085(17) O4 0.0346(18) 0.0341(19) 0.044(2) -0.0053(16) -0.0001(15) -0.0082(15) O5 0.043(3) 0.027(2) 0.043(3) 0.000 0.003(2) 0.000 O6 0.053(2) 0.050(3) 0.052(3) 0.015(2) 0.011(2) -0.0054(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.147(4) . ? Nd1 O2 2.333(3) . ? Nd1 O5 2.399(3) . ? Nd1 O1 2.409(3) . ? Nd1 O1 2.520(3) 3 ? Nd1 O6 2.661(4) . ? Nd1 Nd1 3.6318(6) 3 ? Nd1 Nd2 3.7161(4) . ? Nd2 O4 2.163(3) 3 ? Nd2 O4 2.163(3) . ? Nd2 O2 2.458(3) 3 ? Nd2 O2 2.458(3) . ? Nd2 O1 2.624(3) 3 ? Nd2 O1 2.624(3) . ? Nd2 Nd1 3.7161(4) 3 ? O1 C1 1.437(6) . ? O1 Nd1 2.520(3) 3 ? O2 C5 1.429(6) . ? O3 C9 1.422(8) . ? O4 C13 1.410(7) . ? O5 C17 1.442(10) . ? O5 Nd1 2.399(3) 3 ? C1 C2 1.525(8) . ? C1 C4 1.528(8) . ? C1 C3 1.531(8) . ? C5 C7 1.518(8) . ? C5 C6 1.522(8) . ? C5 C8 1.535(8) . ? C9 C11 1.479(12) . ? C9 C10 1.497(11) . ? C9 C12 1.526(11) . ? C13 C15 1.449(12) . ? C13 C16 1.473(13) . ? C13 C14 1.539(11) . ? C17 C19 1.451(19) . ? C17 C19 1.451(19) 3 ? C17 C20 1.559(16) 3 ? C17 C20 1.559(16) . ? C17 C18 1.572(14) 3 ? C17 C18 1.572(14) . ? C18 C19 1.31(2) 3 ? C18 C20 1.70(2) 3 ? C19 C18 1.31(2) 3 ? C19 C20 1.35(2) 3 ? C20 C19 1.35(2) 3 ? C20 C18 1.70(2) 3 ? O6 C21B 1.362(17) . ? O6 C24 1.467(12) . ? O6 C24B 1.473(19) . ? O6 C21 1.546(13) . ? C21 C22 1.580(19) . ? C22 C23 1.41(2) . ? C23 C24 1.488(17) . ? C21B C22B 1.49(2) . ? C22B C23B 1.52(5) . ? C23B C24B 1.38(5) . ? O40 C44 1.44(2) . ? O40 C41 1.54(2) . ? C41 C42 1.59(2) . ? C42 C43 1.37(2) . ? C42 C43 1.65(4) 3_554 ? C42 C42 2.05(6) 3_554 ? C43 C43 1.39(8) 3_554 ? C43 C44 1.50(2) . ? C43 C42 1.65(4) 3_554 ? C43 C44 1.89(4) 3_554 ? C44 C44 1.32(6) 3_554 ? C44 C43 1.89(4) 3_554 ? O41 C46 1.13(3) 3_554 ? O41 C48 1.431(19) . ? O41 C45 1.561(18) . ? C45 O41 1.561(18) 3_554 ? C45 C46 1.57(2) . ? C45 C46 1.57(2) 3_554 ? C46 C48 1.02(3) 3_554 ? C46 O41 1.13(3) 3_554 ? C46 C47 1.16(3) 3_554 ? C46 C47 1.38(2) . ? C46 C46 1.57(4) 3_554 ? C47 C47 0.68(4) 3_554 ? C47 C46 1.16(3) 3_554 ? C47 C48 1.46(2) . ? C47 C48 1.91(4) 3_554 ? C48 C46 1.02(3) 3_554 ? C48 C47 1.91(4) 3_554 ? 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 O3 Nd1 O2 105.66(14) . . ? O3 Nd1 O5 105.23(13) . . ? O2 Nd1 O5 141.74(12) . . ? O3 Nd1 O1 105.86(13) . . ? O2 Nd1 O1 76.45(11) . . ? O5 Nd1 O1 73.81(11) . . ? O3 Nd1 O1 171.71(13) . 3 ? O2 Nd1 O1 74.37(11) . 3 ? O5 Nd1 O1 71.83(10) . 3 ? O1 Nd1 O1 65.96(13) . 3 ? O3 Nd1 O6 87.50(14) . . ? O2 Nd1 O6 103.31(13) . . ? O5 Nd1 O6 100.06(12) . . ? O1 Nd1 O6 166.29(13) . . ? O1 Nd1 O6 100.61(12) 3 . ? O3 Nd1 Nd1 131.80(11) . 3 ? O2 Nd1 Nd1 101.01(8) . 3 ? O5 Nd1 Nd1 40.82(9) . 3 ? O1 Nd1 Nd1 43.72(8) . 3 ? O1 Nd1 Nd1 41.36(7) 3 3 ? O6 Nd1 Nd1 124.25(10) . 3 ? O3 Nd1 Nd2 130.42(11) . . ? O2 Nd1 Nd2 40.37(8) . . ? O5 Nd1 Nd2 101.56(9) . . ? O1 Nd1 Nd2 44.68(8) . . ? O1 Nd1 Nd2 44.86(8) 3 . ? O6 Nd1 Nd2 127.62(10) . . ? Nd1 Nd1 Nd2 60.748(5) 3 . ? O4 Nd2 O4 99.9(2) 3 . ? O4 Nd2 O2 102.21(13) 3 3 ? O4 Nd2 O2 106.78(13) . 3 ? O4 Nd2 O2 106.78(13) 3 . ? O4 Nd2 O2 102.21(13) . . ? O2 Nd2 O2 134.27(16) 3 . ? O4 Nd2 O1 99.32(12) 3 3 ? O4 Nd2 O1 160.73(13) . 3 ? O2 Nd2 O1 70.47(10) 3 3 ? O2 Nd2 O1 70.52(11) . 3 ? O4 Nd2 O1 160.73(13) 3 . ? O4 Nd2 O1 99.32(12) . . ? O2 Nd2 O1 70.52(11) 3 . ? O2 Nd2 O1 70.47(10) . . ? O1 Nd2 O1 61.53(14) 3 . ? O4 Nd2 Nd1 121.36(10) 3 3 ? O4 Nd2 Nd1 127.05(10) . 3 ? O2 Nd2 Nd1 37.95(8) 3 3 ? O2 Nd2 Nd1 96.35(8) . 3 ? O1 Nd2 Nd1 40.21(7) 3 3 ? O1 Nd2 Nd1 42.64(7) . 3 ? O4 Nd2 Nd1 127.05(10) 3 . ? O4 Nd2 Nd1 121.36(10) . . ? O2 Nd2 Nd1 96.35(8) 3 . ? O2 Nd2 Nd1 37.95(8) . . ? O1 Nd2 Nd1 42.64(7) 3 . ? O1 Nd2 Nd1 40.21(7) . . ? Nd1 Nd2 Nd1 58.505(11) 3 . ? C1 O1 Nd1 123.1(3) . . ? C1 O1 Nd1 123.6(3) . 3 ? Nd1 O1 Nd1 94.92(11) . 3 ? C1 O1 Nd2 120.0(3) . . ? Nd1 O1 Nd2 95.11(11) . . ? Nd1 O1 Nd2 92.51(11) 3 . ? C5 O2 Nd1 131.9(3) . . ? C5 O2 Nd2 126.4(3) . . ? Nd1 O2 Nd2 101.68(12) . . ? C9 O3 Nd1 177.8(4) . . ? C13 O4 Nd2 167.3(4) . . ? C17 O5 Nd1 130.82(9) . 3 ? C17 O5 Nd1 130.82(9) . . ? Nd1 O5 Nd1 98.37(18) 3 . ? O1 C1 C2 109.2(4) . . ? O1 C1 C4 108.4(4) . . ? C2 C1 C4 110.6(5) . . ? O1 C1 C3 109.8(4) . . ? C2 C1 C3 109.5(4) . . ? C4 C1 C3 109.3(5) . . ? O2 C5 C7 109.8(4) . . ? O2 C5 C6 109.0(4) . . ? C7 C5 C6 109.0(5) . . ? O2 C5 C8 109.4(4) . . ? C7 C5 C8 109.5(5) . . ? C6 C5 C8 110.1(5) . . ? O3 C9 C11 109.5(7) . . ? O3 C9 C10 109.7(6) . . ? C11 C9 C10 111.1(7) . . ? O3 C9 C12 109.5(6) . . ? C11 C9 C12 109.5(7) . . ? C10 C9 C12 107.4(7) . . ? O4 C13 C15 111.5(6) . . ? O4 C13 C16 110.7(7) . . ? C15 C13 C16 114.4(8) . . ? O4 C13 C14 110.0(6) . . ? C15 C13 C14 108.0(7) . . ? C16 C13 C14 101.8(7) . . ? O5 C17 C19 110.0(8) . . ? O5 C17 C19 110.0(8) . 3 ? C19 C17 C19 140.0(16) . 3 ? O5 C17 C20 105.7(7) . 3 ? C19 C17 C20 53.0(9) . 3 ? C19 C17 C20 114.6(9) 3 3 ? O5 C17 C20 105.7(7) . . ? C19 C17 C20 114.6(9) . . ? C19 C17 C20 53.0(9) 3 . ? C20 C17 C20 148.6(13) 3 . ? O5 C17 C18 110.1(6) . 3 ? C19 C17 C18 51.3(8) . 3 ? C19 C17 C18 112.9(9) 3 3 ? C20 C17 C18 103.0(8) 3 3 ? C20 C17 C18 65.7(8) . 3 ? O5 C17 C18 110.1(6) . . ? C19 C17 C18 112.9(9) . . ? C19 C17 C18 51.3(8) 3 . ? C20 C17 C18 65.7(8) 3 . ? C20 C17 C18 103.0(8) . . ? C18 C17 C18 139.8(11) 3 . ? C19 C18 C17 59.6(10) 3 . ? C19 C18 C20 113.9(13) 3 3 ? C17 C18 C20 56.8(7) . 3 ? C18 C19 C20 134.3(18) 3 3 ? C18 C19 C17 69.1(11) 3 . ? C20 C19 C17 67.6(11) 3 . ? C19 C20 C17 59.4(10) 3 . ? C19 C20 C18 111.3(14) 3 3 ? C17 C20 C18 57.5(7) . 3 ? C21B O6 C24 80.2(9) . . ? C21B O6 C24B 105.5(11) . . ? C24 O6 C24B 58.2(9) . . ? C21B O6 C21 41.7(8) . . ? C24 O6 C21 103.6(7) . . ? C24B O6 C21 89.3(9) . . ? C21B O6 Nd1 141.2(8) . . ? C24 O6 Nd1 116.8(6) . . ? C24B O6 Nd1 113.1(8) . . ? C21 O6 Nd1 139.5(6) . . ? O6 C21 C22 99.6(10) . . ? C23 C22 C21 105.7(11) . . ? C22 C23 C24 110.7(11) . . ? O6 C24 C23 102.2(9) . . ? O6 C21B C22B 109.6(13) . . ? C21B C22B C23B 103(2) . . ? C24B C23B C22B 105(4) . . ? C23B C24B O6 112(3) . . ? C44 O40 C41 106.6(16) . . ? O40 C41 C42 104.4(17) . . ? C43 C42 C41 94.1(18) . . ? C43 C42 C43 54(3) . 3_554 ? C41 C42 C43 120(2) . 3_554 ? C43 C42 C42 53.6(18) . 3_554 ? C41 C42 C42 147.6(19) . 3_554 ? C43 C42 C42 41.9(14) 3_554 3_554 ? C42 C43 C43 74(2) . 3_554 ? C42 C43 C44 110(2) . . ? C43 C43 C44 82(2) 3_554 . ? C42 C43 C42 85(3) . 3_554 ? C43 C43 C42 53(2) 3_554 3_554 ? C44 C43 C42 126(3) . 3_554 ? C42 C43 C44 118(3) . 3_554 ? C43 C43 C44 51.6(16) 3_554 3_554 ? C44 C43 C44 44.0(19) . 3_554 ? C42 C43 C44 83(2) 3_554 3_554 ? C44 C44 O40 159(5) 3_554 . ? C44 C44 C43 84.1(18) 3_554 . ? O40 C44 C43 98.9(17) . . ? C44 C44 C43 51.9(15) 3_554 3_554 ? O40 C44 C43 116(2) . 3_554 ? C43 C44 C43 47(3) . 3_554 ? C46 O41 C48 44.8(14) 3_554 . ? C46 O41 C45 68.9(15) 3_554 . ? C48 O41 C45 112.4(15) . . ? O41 C45 O41 145(2) 3_554 . ? O41 C45 C46 42.5(11) 3_554 . ? O41 C45 C46 102.2(15) . . ? O41 C45 C46 102.2(15) 3_554 3_554 ? O41 C45 C46 42.5(11) . 3_554 ? C46 C45 C46 60.3(16) . 3_554 ? C48 C46 O41 83(2) 3_554 3_554 ? C48 C46 C47 84(2) 3_554 3_554 ? O41 C46 C47 155(3) 3_554 3_554 ? C48 C46 C47 104(3) 3_554 . ? O41 C46 C47 172(2) 3_554 . ? C47 C46 C47 30(2) 3_554 . ? C48 C46 C45 148(2) 3_554 . ? O41 C46 C45 68.6(14) 3_554 . ? C47 C46 C45 116(2) 3_554 . ? C47 C46 C45 104.0(15) . . ? C48 C46 C46 141(3) 3_554 3_554 ? O41 C46 C46 127.4(15) 3_554 3_554 ? C47 C46 C46 58.4(15) 3_554 3_554 ? C47 C46 C46 45.8(13) . 3_554 ? C45 C46 C46 59.9(8) . 3_554 ? C47 C47 C46 93(3) 3_554 3_554 ? C47 C47 C46 57(3) 3_554 . ? C46 C47 C46 76(2) 3_554 . ? C47 C47 C48 122(5) 3_554 . ? C46 C47 C48 43.9(14) 3_554 . ? C46 C47 C48 119.1(17) . . ? C47 C47 C48 40(4) 3_554 3_554 ? C46 C47 C48 103.0(17) 3_554 3_554 ? C46 C47 C48 31.1(12) . 3_554 ? C48 C47 C48 146.6(18) . 3_554 ? C46 C48 O41 51.9(17) 3_554 . ? C46 C48 C47 52.5(19) 3_554 . ? O41 C48 C47 101.8(15) . . ? C46 C48 C47 44.6(18) 3_554 3_554 ? O41 C48 C47 96.4(14) . 3_554 ? C47 C48 C47 17.7(19) . 3_554 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.505 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.137