# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1747 data_yb14e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ' [YbL]2*12H2O (!centrosymmetric dimer!) ' _chemical_formula_sum 'C30 H52 N4 O12 P3 Yb' _chemical_formula_weight 926.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no.14)' 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 12.9699(9) _cell_length_b 19.961(2) _cell_length_c 15.784(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.184(9) _cell_angle_gamma 90.00 _cell_volume 3783.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 2.661 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min -- _exptl_absorpt_correction_T_max -- _exptl_special_details ; crystal coated by thin paraphine film due to a loss of solvate molecules ; _diffrn_ambient_temperature 170(1) _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 'CAD4 (Enraf-Nonius) ' _diffrn_measurement_method '.omega.-2.theta. ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 6.4 _diffrn_reflns_number 5547 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 22.98 _reflns_number_total 5243 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 program packet ' _computing_cell_refinement 'CAD4 program packet ' _computing_data_reduction 'JANA-98 (Petricek, 1998) ' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+10.7685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson + Fourier ' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00037(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5243 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 10.947 _refine_ls_shift/su_mean 0.048 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb Yb 0.669998(13) 0.607742(8) 0.031575(11) 0.01488(9) Uani 1 d . . . P1 P 0.89753(9) 0.62956(6) 0.22316(7) 0.0220(3) Uani 1 d . . . P2 P 0.56489(9) 0.74396(5) 0.09620(8) 0.0208(3) Uani 1 d . . . P3 P 0.40157(8) 0.56211(5) -0.07644(7) 0.0164(2) Uani 1 d . . . O11 O 0.8095(2) 0.58155(15) 0.16338(19) 0.0224(7) Uani 1 d . . . O12 O 0.8825(3) 0.66042(17) 0.3041(2) 0.0313(7) Uani 1 d . . . O21 O 0.6419(2) 0.68395(14) 0.12645(19) 0.0210(6) Uani 1 d . . . O22 O 0.6116(2) 0.80941(15) 0.1412(2) 0.0265(7) Uani 1 d . . . O31 O 0.4812(2) 0.60705(13) -0.00427(19) 0.0180(6) Uani 1 d . . . O32 O 0.3674(2) 0.49904(14) -0.04169(19) 0.0206(6) Uani 1 d . . . N1 N 0.8495(3) 0.67641(17) 0.0476(2) 0.0182(7) Uani 1 d . . . N2 N 0.6203(3) 0.72176(17) -0.0507(2) 0.0188(8) Uani 1 d . . . N3 N 0.5603(3) 0.59075(17) -0.1440(2) 0.0196(8) Uani 1 d . . . N4 N 0.7901(3) 0.54583(17) -0.0442(2) 0.0201(8) Uani 1 d . . . C1 C 0.8238(4) 0.7371(2) -0.0113(3) 0.0215(9) Uani 1 d . . . H011 H 0.814(4) 0.723(2) -0.073(3) 0.025(12) Uiso 1 d . . . H012 H 0.887(3) 0.769(2) 0.010(3) 0.014(10) Uiso 1 d . . . C2 C 0.7164(4) 0.7696(2) -0.0166(3) 0.0218(9) Uani 1 d . . . H021 H 0.703(4) 0.808(2) -0.059(3) 0.028(12) Uiso 1 d . . . H022 H 0.722(4) 0.785(2) 0.043(3) 0.022(11) Uiso 1 d . . . C3 C 0.5844(4) 0.7136(2) -0.1510(3) 0.0227(10) Uani 1 d . . . H031 H 0.552(3) 0.753(2) -0.181(3) 0.010(10) Uiso 1 d . . . H032 H 0.650(4) 0.709(2) -0.167(3) 0.027(12) Uiso 1 d . . . C4 C 0.5077(4) 0.6550(2) -0.1870(3) 0.0223(10) Uani 1 d . . . H041 H 0.491(3) 0.651(2) -0.247(3) 0.012(10) Uiso 1 d . . . H042 H 0.442(4) 0.659(2) -0.177(3) 0.026(12) Uiso 1 d . . . C5 C 0.6317(4) 0.5650(3) -0.1915(3) 0.0240(10) Uani 1 d . . . H051 H 0.588(4) 0.544(2) -0.241(3) 0.020(12) Uiso 1 d . . . H052 H 0.662(4) 0.600(2) -0.207(3) 0.015(11) Uiso 1 d . . . C6 C 0.7160(4) 0.5160(2) -0.1321(3) 0.0227(10) Uani 1 d . . . H061 H 0.682(4) 0.482(2) -0.117(3) 0.020(12) Uiso 1 d . . . H062 H 0.758(4) 0.500(2) -0.164(3) 0.026(12) Uiso 1 d . . . C7 C 0.8685(4) 0.5932(2) -0.0607(3) 0.0205(9) Uani 1 d . . . H071 H 0.829(3) 0.620(2) -0.109(3) 0.007(10) Uiso 1 d . . . H072 H 0.918(3) 0.568(2) -0.082(3) 0.008(10) Uiso 1 d . . . C8 C 0.9290(3) 0.6342(2) 0.0235(3) 0.0213(9) Uani 1 d . . . H081 H 0.981(4) 0.665(2) 0.009(3) 0.018(11) Uiso 1 d . . . H082 H 0.969(4) 0.604(2) 0.078(3) 0.021 Uiso 1 d . . . C10 C 0.9020(4) 0.6965(2) 0.1448(3) 0.0223(10) Uani 1 d . . . H101 H 0.976(4) 0.710(2) 0.157(3) 0.026(12) Uiso 1 d . . . H102 H 0.859(4) 0.730(2) 0.155(3) 0.022(12) Uiso 1 d . . . C11 C 1.0302(4) 0.5864(2) 0.2655(3) 0.0260(10) Uani 1 d . . . C12 C 1.0358(4) 0.5174(3) 0.2591(3) 0.0334(12) Uani 1 d . . . H12 H 0.972(5) 0.495(3) 0.231(4) 0.042(15) Uiso 1 d . . . C13 C 1.1361(5) 0.4841(3) 0.2997(4) 0.0407(13) Uani 1 d . . . H13 H 1.135(4) 0.442(3) 0.296(3) 0.027(14) Uiso 1 d . . . C14 C 1.2318(4) 0.5193(3) 0.3465(4) 0.0420(14) Uani 1 d . . . H14 H 1.297(5) 0.499(3) 0.372(4) 0.053(17) Uiso 1 d . . . C15 C 1.2274(4) 0.5879(3) 0.3524(4) 0.0426(14) Uani 1 d . . . H15 H 1.286(6) 0.608(3) 0.381(4) 0.06(2) Uiso 1 d . . . C16 C 1.1284(4) 0.6218(3) 0.3139(3) 0.0345(12) Uani 1 d . . . H16 H 1.125(4) 0.667(3) 0.315(3) 0.035(15) Uiso 1 d . . . C20 C 0.5282(4) 0.7503(2) -0.0272(3) 0.0213(9) Uani 1 d . . . H201 H 0.462(3) 0.7255(19) -0.058(3) 0.006(9) Uiso 1 d . . . H202 H 0.512(4) 0.794(3) -0.050(3) 0.036(14) Uiso 1 d . . . C21 C 0.4380(4) 0.7291(2) 0.1148(3) 0.0261(10) Uani 1 d . . . C22 C 0.3546(4) 0.7777(3) 0.0874(4) 0.0378(13) Uani 1 d . . . H22 H 0.366(5) 0.816(3) 0.051(4) 0.049(16) Uiso 1 d . . . C23 C 0.2601(5) 0.7699(4) 0.1084(5) 0.0583(19) Uani 1 d . . . H23 H 0.205(5) 0.805(3) 0.083(4) 0.056(18) Uiso 1 d . . . C24 C 0.2493(6) 0.7146(4) 0.1566(5) 0.068(2) Uani 1 d . . . H24 H 0.186(6) 0.712(4) 0.169(5) 0.08(2) Uiso 1 d . . . C25 C 0.3308(6) 0.6668(4) 0.1831(5) 0.060(2) Uani 1 d . . . H25 H 0.323(6) 0.634(4) 0.206(5) 0.06(2) Uiso 1 d . . . C26 C 0.4248(5) 0.6727(3) 0.1616(4) 0.0370(13) Uani 1 d . . . H26 H 0.480(4) 0.644(3) 0.180(3) 0.026(14) Uiso 1 d . . . C30 C 0.4714(3) 0.5408(2) -0.1536(3) 0.0210(9) Uani 1 d . . . H301 H 0.423(4) 0.537(2) -0.219(3) 0.027(12) Uiso 1 d . . . H302 H 0.508(3) 0.496(2) -0.128(3) 0.012(10) Uiso 1 d . . . C31 C 0.2759(3) 0.6082(2) -0.1389(3) 0.0232(10) Uani 1 d . . . C32 C 0.2104(4) 0.5935(3) -0.2290(3) 0.0323(12) Uani 1 d . . . H32 H 0.231(4) 0.564(2) -0.264(3) 0.024(13) Uiso 1 d . . . C33 C 0.1080(4) 0.6250(3) -0.2708(4) 0.0451(15) Uani 1 d . . . H33 H 0.070(5) 0.615(3) -0.324(4) 0.048(18) Uiso 1 d . . . C34 C 0.0699(5) 0.6681(3) -0.2215(5) 0.0502(18) Uani 1 d . . . H34 H 0.006(6) 0.681(3) -0.247(4) 0.056(18) Uiso 1 d . . . C35 C 0.1337(4) 0.6833(3) -0.1333(5) 0.0439(14) Uani 1 d . . . H35 H 0.116(5) 0.711(3) -0.102(4) 0.041(17) Uiso 1 d . . . C36 C 0.2382(4) 0.6543(2) -0.0913(4) 0.0304(11) Uani 1 d . . . H36 H 0.273(5) 0.662(3) -0.028(4) 0.043(16) Uiso 1 d . . . C40 C 0.8547(4) 0.4897(2) 0.0120(4) 0.0260(10) Uani 1 d . . . H401 H 0.904(4) 0.506(2) 0.068(3) 0.017(11) Uiso 1 d . . . H402 H 0.892(4) 0.466(2) -0.022(3) 0.019(11) Uiso 1 d . . . H403 H 0.808(4) 0.458(2) 0.022(3) 0.018(11) Uiso 1 d . . . O99 O 0.6867(9) 0.5857(7) 0.3168(8) 0.174(7) Uani 1 d . . . H992 H 0.694(16) 0.611(9) 0.297(13) 0.209 Uiso 1 d . . . H991 H 0.742(13) 0.569(9) 0.364(10) 0.209 Uiso 1 d . . . O98 O 0.5038(5) 0.9180(3) 0.0395(4) 0.0643(14) Uani 1 d . . . H981 H 0.552(8) 0.891(5) 0.079(7) 0.12(4) Uiso 1 d . . . H982 H 0.494(5) 0.940(3) 0.069(4) 0.04(2) Uiso 1 d . . . O97 O 0.9821(7) 0.6047(3) 0.4810(4) 0.129(4) Uani 1.000(18) d . . . O96 O 0.8184(3) 0.7965(2) 0.2779(3) 0.0381(16) Uani 1.000(18) d . . . H961 H 0.755(5) 0.798(2) 0.225(4) 0.032(14) Uiso 1 d . . . H962 H 0.824(6) 0.759(5) 0.278(5) 0.08(3) Uiso 1 d . . . O95 O 0.5336(7) 0.5409(4) 0.3868(5) 0.140(4) Uani 1.000(18) d . . . O94 O 0.8408(8) 0.4865(5) 0.4616(6) 0.171(6) Uani 1.00(2) d . . . QN N 0.7051 0.6337 -0.0478 0.050 Uiso 0.00 d P . . QO O 0.6356 0.5934 0.0818 0.050 Uiso 0.00 d P . . 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 Yb 0.01137(12) 0.01486(12) 0.01801(12) -0.00035(7) 0.00509(8) -0.00038(7) P1 0.0148(6) 0.0290(6) 0.0200(6) -0.0004(5) 0.0042(5) -0.0011(5) P2 0.0211(6) 0.0185(6) 0.0246(6) -0.0028(5) 0.0105(5) 0.0001(5) P3 0.0109(5) 0.0163(5) 0.0206(6) 0.0009(4) 0.0044(4) 0.0013(4) O11 0.0149(15) 0.0240(16) 0.0249(16) 0.0032(13) 0.0037(13) -0.0026(12) O12 0.0263(17) 0.042(2) 0.0249(17) -0.0023(15) 0.0085(14) 0.0016(15) O21 0.0217(15) 0.0206(15) 0.0206(15) -0.0020(12) 0.0078(12) -0.0001(12) O22 0.0281(17) 0.0220(16) 0.0312(17) -0.0060(13) 0.0132(14) -0.0023(13) O31 0.0130(14) 0.0179(15) 0.0235(16) 0.0002(12) 0.0073(12) 0.0006(11) O32 0.0130(14) 0.0196(15) 0.0271(16) 0.0006(13) 0.0049(12) 0.0004(12) N1 0.0138(17) 0.0193(18) 0.0222(18) -0.0015(15) 0.0075(15) -0.0012(14) N2 0.0172(18) 0.0192(19) 0.0215(19) -0.0007(15) 0.0090(15) -0.0013(15) N3 0.0157(18) 0.0213(19) 0.0228(19) -0.0005(15) 0.0085(15) -0.0007(15) N4 0.0158(18) 0.0202(19) 0.0242(19) 0.0004(15) 0.0076(15) 0.0015(15) C1 0.022(2) 0.020(2) 0.025(2) -0.0003(19) 0.0115(19) -0.0063(19) C2 0.025(2) 0.017(2) 0.025(2) 0.003(2) 0.012(2) 0.0008(19) C3 0.024(2) 0.022(2) 0.024(2) 0.006(2) 0.011(2) 0.001(2) C4 0.020(2) 0.028(3) 0.020(3) 0.0042(19) 0.009(2) 0.0024(19) C5 0.023(2) 0.031(3) 0.021(2) -0.008(2) 0.011(2) -0.006(2) C6 0.020(2) 0.024(3) 0.029(3) -0.007(2) 0.014(2) -0.002(2) C7 0.018(2) 0.023(2) 0.023(2) 0.002(2) 0.011(2) 0.0006(19) C8 0.014(2) 0.026(2) 0.028(2) 0.001(2) 0.011(2) 0.0002(19) C10 0.016(2) 0.025(2) 0.026(2) -0.0045(19) 0.0075(19) -0.004(2) C11 0.018(2) 0.038(3) 0.022(2) 0.003(2) 0.0070(19) 0.000(2) C12 0.029(3) 0.037(3) 0.032(3) 0.004(2) 0.010(2) -0.001(2) C13 0.037(3) 0.043(4) 0.040(3) 0.012(3) 0.013(3) 0.015(3) C14 0.025(3) 0.069(4) 0.032(3) 0.011(3) 0.010(2) 0.018(3) C15 0.019(3) 0.070(4) 0.031(3) 0.000(3) 0.000(2) -0.004(3) C16 0.021(3) 0.044(3) 0.034(3) -0.003(2) 0.005(2) -0.002(2) C20 0.020(2) 0.016(2) 0.029(2) 0.003(2) 0.010(2) 0.003(2) C21 0.026(2) 0.027(3) 0.028(2) -0.013(2) 0.015(2) -0.006(2) C22 0.026(3) 0.044(3) 0.046(3) -0.014(3) 0.015(2) 0.000(2) C23 0.030(3) 0.073(5) 0.077(5) -0.038(4) 0.027(3) -0.004(3) C24 0.054(4) 0.086(6) 0.090(5) -0.047(5) 0.058(4) -0.036(4) C25 0.078(5) 0.061(5) 0.069(5) -0.033(4) 0.058(4) -0.042(4) C26 0.048(3) 0.034(3) 0.039(3) -0.014(3) 0.029(3) -0.013(3) C30 0.016(2) 0.023(2) 0.020(2) -0.0030(19) 0.0036(19) -0.0008(19) C31 0.013(2) 0.023(2) 0.032(3) 0.0082(19) 0.008(2) 0.0007(18) C32 0.021(3) 0.042(3) 0.031(3) 0.008(2) 0.007(2) 0.000(2) C33 0.022(3) 0.060(4) 0.040(3) 0.028(3) -0.003(3) -0.001(3) C34 0.017(3) 0.047(4) 0.082(5) 0.038(4) 0.013(3) 0.014(3) C35 0.031(3) 0.031(3) 0.075(5) 0.013(3) 0.025(3) 0.012(2) C36 0.026(3) 0.024(3) 0.043(3) 0.006(2) 0.015(2) 0.005(2) C40 0.022(2) 0.021(2) 0.037(3) 0.003(2) 0.013(2) 0.003(2) O99 0.136(8) 0.262(15) 0.189(11) -0.142(11) 0.135(8) -0.126(10) O98 0.076(4) 0.041(3) 0.064(3) 0.010(3) 0.013(3) 0.010(3) O97 0.188(8) 0.139(7) 0.048(4) 0.008(3) 0.031(4) 0.052(5) O96 0.034(3) 0.040(3) 0.041(3) -0.0168(18) 0.015(2) -0.0078(18) O95 0.216(9) 0.115(6) 0.115(6) -0.034(4) 0.091(6) -0.083(6) O94 0.234(11) 0.158(9) 0.191(10) 0.056(6) 0.161(9) 0.069(7) _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 Yb QO 1.08535(19) . ? Yb QN 1.5732(2) . ? Yb O32 2.205(3) 3_665 ? Yb O11 2.243(3) . ? Yb O21 2.258(3) . ? Yb O31 2.296(3) . ? Yb N2 2.579(3) . ? Yb N4 2.605(3) . ? Yb N3 2.616(3) . ? Yb N1 2.631(3) . ? Yb P1 3.3621(12) . ? Yb P2 3.3678(11) . ? P1 O12 1.496(3) . ? P1 O11 1.516(3) . ? P1 C11 1.811(4) . ? P1 C10 1.836(5) . ? P2 O22 1.501(3) . ? P2 O21 1.517(3) . ? P2 C21 1.803(4) . ? P2 C20 1.827(5) . ? P3 O32 1.505(3) . ? P3 O31 1.510(3) . ? P3 C31 1.806(4) . ? P3 C30 1.822(4) . ? O32 Yb 2.205(3) 3_665 ? N1 C10 1.479(6) . ? N1 C1 1.487(5) . ? N1 C8 1.487(5) . ? N2 C3 1.481(5) . ? N2 C20 1.490(5) . ? N2 C2 1.499(5) . ? N3 C5 1.485(6) . ? N3 C30 1.488(5) . ? N3 C4 1.490(6) . ? N4 C40 1.479(6) . ? N4 C6 1.481(6) . ? N4 C7 1.482(5) . ? C1 C2 1.509(6) . ? C1 H011 0.97(5) . ? C1 H012 0.99(4) . ? C2 H021 0.98(5) . ? C2 H022 0.96(5) . ? C3 C4 1.502(6) . ? C3 H031 0.93(4) . ? C3 H032 0.99(5) . ? C4 H041 0.90(4) . ? C4 H042 0.94(5) . ? C5 C6 1.502(7) . ? C5 H051 0.88(5) . ? C5 H052 0.88(5) . ? C6 H061 0.88(5) . ? C6 H062 0.94(5) . ? C7 C8 1.506(6) . ? C7 H071 0.92(4) . ? C7 H072 0.97(4) . ? C8 H081 0.99(4) . ? C8 H082 1.02(5) . ? C10 H101 0.94(5) . ? C10 H102 0.92(5) . ? C11 C12 1.385(7) . ? C11 C16 1.403(7) . ? C12 C13 1.385(7) . ? C12 H12 0.90(6) . ? C13 C14 1.375(8) . ? C13 H13 0.85(5) . ? C14 C15 1.375(9) . ? C14 H14 0.89(6) . ? C15 C16 1.374(8) . ? C15 H15 0.83(7) . ? C16 H16 0.89(5) . ? C20 H201 0.96(4) . ? C20 H202 0.94(5) . ? C21 C26 1.392(7) . ? C21 C22 1.395(7) . ? C22 C23 1.394(8) . ? C22 H22 0.99(6) . ? C23 C24 1.377(11) . ? C23 H23 0.98(6) . ? C24 C25 1.366(11) . ? C24 H24 0.92(8) . ? C25 C26 1.387(8) . ? C25 H25 0.77(7) . ? C26 H26 0.88(5) . ? C30 H301 0.99(5) . ? C30 H302 1.02(4) . ? C31 C32 1.384(7) . ? C31 C36 1.389(7) . ? C32 C33 1.389(8) . ? C32 H32 0.91(5) . ? C33 C34 1.370(9) . ? C33 H33 0.82(6) . ? C34 C35 1.358(9) . ? C34 H34 0.82(7) . ? C35 C36 1.390(7) . ? C35 H35 0.84(6) . ? C36 H36 0.93(5) . ? C40 H401 0.93(5) . ? C40 H402 0.96(5) . ? C40 H403 0.93(5) . ? O99 H992 0.62(18) . ? O99 H991 0.88(16) . ? O98 H981 0.87(10) . ? O98 H982 0.68(6) . ? O96 H961 0.92(6) . ? O96 H962 0.76(9) . ? 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 QO Yb QN 172.436(14) . . ? QO Yb O32 61.92(7) . 3_665 ? QN Yb O32 120.93(7) . 3_665 ? QO Yb O11 70.77(7) . . ? QN Yb O11 116.16(7) . . ? O32 Yb O11 80.22(10) 3_665 . ? QO Yb O21 58.64(7) . . ? QN Yb O21 118.25(7) . . ? O32 Yb O21 120.53(10) 3_665 . ? O11 Yb O21 79.48(10) . . ? QO Yb O31 58.93(7) . . ? QN Yb O31 114.07(7) . . ? O32 Yb O31 76.62(9) 3_665 . ? O11 Yb O31 129.70(10) . . ? O21 Yb O31 75.14(10) . . ? QO Yb N2 120.50(7) . . ? QN Yb N2 53.18(7) . . ? O32 Yb N2 150.40(10) 3_665 . ? O11 Yb N2 129.31(10) . . ? O21 Yb N2 70.56(10) . . ? O31 Yb N2 80.82(10) . . ? QO Yb N4 133.80(8) . . ? QN Yb N4 52.28(8) . . ? O32 Yb N4 76.16(10) 3_665 . ? O11 Yb N4 84.42(11) . . ? O21 Yb N4 153.86(10) . . ? O31 Yb N4 130.60(10) . . ? N2 Yb N4 105.46(10) . . ? QO Yb N3 122.09(7) . . ? QN Yb N3 53.42(7) . . ? O32 Yb N3 84.55(11) 3_665 . ? O11 Yb N3 151.39(11) . . ? O21 Yb N3 129.09(10) . . ? O31 Yb N3 68.62(10) . . ? N2 Yb N3 69.40(11) . . ? N4 Yb N3 68.42(11) . . ? QO Yb N1 131.34(7) . . ? QN Yb N1 52.65(7) . . ? O32 Yb N1 135.05(10) 3_665 . ? O11 Yb N1 69.97(10) . . ? O21 Yb N1 86.77(10) . . ? O31 Yb N1 148.20(10) . . ? N2 Yb N1 68.45(10) . . ? N4 Yb N1 68.32(11) . . ? N3 Yb N1 106.08(10) . . ? QO Yb P1 80.80(2) . . ? QN Yb P1 104.71(2) . . ? O32 Yb P1 101.68(7) 3_665 . ? O11 Yb P1 21.47(8) . . ? O21 Yb P1 67.84(7) . . ? O31 Yb P1 135.62(7) . . ? N2 Yb P1 107.84(8) . . ? N4 Yb P1 90.03(8) . . ? N3 Yb P1 155.67(8) . . ? N1 Yb P1 53.23(8) . . ? QO Yb P2 70.53(2) . . ? QN Yb P2 104.29(2) . . ? O32 Yb P2 129.28(7) 3_665 . ? O11 Yb P2 100.61(8) . . ? O21 Yb P2 21.62(7) . . ? O31 Yb P2 64.11(7) . . ? N2 Yb P2 52.20(8) . . ? N4 Yb P2 154.47(8) . . ? N3 Yb P2 107.78(8) . . ? N1 Yb P2 89.71(8) . . ? P1 Yb P2 86.63(3) . . ? O12 P1 O11 118.77(18) . . ? O12 P1 C11 107.02(19) . . ? O11 P1 C11 108.5(2) . . ? O12 P1 C10 108.9(2) . . ? O11 P1 C10 104.38(18) . . ? C11 P1 C10 109.1(2) . . ? O12 P1 Yb 117.92(13) . . ? O11 P1 Yb 32.79(11) . . ? C11 P1 Yb 131.24(16) . . ? C10 P1 Yb 74.25(14) . . ? O22 P2 O21 115.98(17) . . ? O22 P2 C21 107.25(18) . . ? O21 P2 C21 110.63(19) . . ? O22 P2 C20 109.9(2) . . ? O21 P2 C20 105.40(18) . . ? C21 P2 C20 107.4(2) . . ? O22 P2 Yb 135.12(13) . . ? O21 P2 Yb 33.27(11) . . ? C21 P2 Yb 114.56(15) . . ? C20 P2 Yb 72.85(14) . . ? O32 P3 O31 115.69(16) . . ? O32 P3 C31 107.21(17) . . ? O31 P3 C31 109.18(18) . . ? O32 P3 C30 109.74(18) . . ? O31 P3 C30 105.76(18) . . ? C31 P3 C30 109.1(2) . . ? O32 P3 Yb 115.55(11) . . ? O31 P3 Yb 34.60(10) . . ? C31 P3 Yb 133.24(14) . . ? C30 P3 Yb 73.84(14) . . ? P1 O11 Yb 125.74(17) . . ? P2 O21 Yb 125.11(16) . . ? P3 O31 Yb 123.47(15) . . ? P3 O32 Yb 159.72(18) . 3_665 ? C10 N1 C1 109.5(3) . . ? C10 N1 C8 109.0(3) . . ? C1 N1 C8 108.4(3) . . ? C10 N1 Yb 106.6(2) . . ? C1 N1 Yb 112.5(2) . . ? C8 N1 Yb 110.8(2) . . ? C3 N2 C20 110.5(3) . . ? C3 N2 C2 109.7(3) . . ? C20 N2 C2 107.6(3) . . ? C3 N2 Yb 111.1(2) . . ? C20 N2 Yb 106.5(2) . . ? C2 N2 Yb 111.4(2) . . ? C5 N3 C30 108.9(3) . . ? C5 N3 C4 109.5(3) . . ? C30 N3 C4 109.0(3) . . ? C5 N3 Yb 112.7(3) . . ? C30 N3 Yb 106.5(2) . . ? C4 N3 Yb 110.0(3) . . ? C40 N4 C6 106.1(4) . . ? C40 N4 C7 108.5(3) . . ? C6 N4 C7 109.7(3) . . ? C40 N4 Yb 112.7(3) . . ? C6 N4 Yb 109.4(2) . . ? C7 N4 Yb 110.3(2) . . ? N1 C1 C2 111.7(3) . . ? N1 C1 H011 108(3) . . ? C2 C1 H011 107(3) . . ? N1 C1 H012 111(2) . . ? C2 C1 H012 111(2) . . ? H011 C1 H012 107(4) . . ? N2 C2 C1 111.8(3) . . ? N2 C2 H021 110(3) . . ? C1 C2 H021 107(3) . . ? N2 C2 H022 108(3) . . ? C1 C2 H022 111(3) . . ? H021 C2 H022 109(4) . . ? N2 C3 C4 112.7(4) . . ? N2 C3 H031 111(2) . . ? C4 C3 H031 111(2) . . ? N2 C3 H032 110(3) . . ? C4 C3 H032 110(3) . . ? H031 C3 H032 102(4) . . ? N3 C4 C3 112.0(4) . . ? N3 C4 H041 107(3) . . ? C3 C4 H041 109(3) . . ? N3 C4 H042 107(3) . . ? C3 C4 H042 112(3) . . ? H041 C4 H042 109(4) . . ? N3 C5 C6 110.8(4) . . ? N3 C5 H051 108(3) . . ? C6 C5 H051 108(3) . . ? N3 C5 H052 107(3) . . ? C6 C5 H052 113(3) . . ? H051 C5 H052 109(4) . . ? N4 C6 C5 112.6(4) . . ? N4 C6 H061 105(3) . . ? C5 C6 H061 110(3) . . ? N4 C6 H062 110(3) . . ? C5 C6 H062 109(3) . . ? H061 C6 H062 109(4) . . ? N4 C7 C8 110.8(3) . . ? N4 C7 H071 109(2) . . ? C8 C7 H071 111(2) . . ? N4 C7 H072 109(2) . . ? C8 C7 H072 113(2) . . ? H071 C7 H072 105(3) . . ? N1 C8 C7 110.7(3) . . ? N1 C8 H081 108(2) . . ? C7 C8 H081 108(2) . . ? N1 C8 H082 107(2) . . ? C7 C8 H082 111(2) . . ? H081 C8 H082 113(3) . . ? N1 C10 P1 112.5(3) . . ? N1 C10 H101 109(3) . . ? P1 C10 H101 111(3) . . ? N1 C10 H102 108(3) . . ? P1 C10 H102 104(3) . . ? H101 C10 H102 113(4) . . ? C12 C11 C16 118.6(5) . . ? C12 C11 P1 120.9(4) . . ? C16 C11 P1 120.1(4) . . ? C13 C12 C11 120.7(5) . . ? C13 C12 H12 121(4) . . ? C11 C12 H12 119(4) . . ? C14 C13 C12 120.2(6) . . ? C14 C13 H13 123(3) . . ? C12 C13 H13 117(3) . . ? C13 C14 C15 119.6(5) . . ? C13 C14 H14 121(4) . . ? C15 C14 H14 119(4) . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 121(4) . . ? C14 C15 H15 118(4) . . ? C15 C16 C11 119.9(6) . . ? C15 C16 H16 121(3) . . ? C11 C16 H16 119(3) . . ? N2 C20 P2 109.2(3) . . ? N2 C20 H201 109(2) . . ? P2 C20 H201 110(2) . . ? N2 C20 H202 110(3) . . ? P2 C20 H202 114(3) . . ? H201 C20 H202 105(4) . . ? C26 C21 C22 119.4(5) . . ? C26 C21 P2 121.5(4) . . ? C22 C21 P2 118.9(4) . . ? C23 C22 C21 119.7(6) . . ? C23 C22 H22 124(3) . . ? C21 C22 H22 116(3) . . ? C24 C23 C22 120.2(7) . . ? C24 C23 H23 126(4) . . ? C22 C23 H23 113(4) . . ? C25 C24 C23 120.0(6) . . ? C25 C24 H24 123(5) . . ? C23 C24 H24 117(5) . . ? C24 C25 C26 121.1(7) . . ? C24 C25 H25 121(5) . . ? C26 C25 H25 118(5) . . ? C25 C26 C21 119.5(6) . . ? C25 C26 H26 123(3) . . ? C21 C26 H26 117(3) . . ? N3 C30 P3 109.8(3) . . ? N3 C30 H301 108(3) . . ? P3 C30 H301 116(3) . . ? N3 C30 H302 109(2) . . ? P3 C30 H302 102(2) . . ? H301 C30 H302 112(3) . . ? C32 C31 C36 119.4(4) . . ? C32 C31 P3 122.0(4) . . ? C36 C31 P3 118.1(4) . . ? C31 C32 C33 119.9(6) . . ? C31 C32 H32 124(3) . . ? C33 C32 H32 117(3) . . ? C34 C33 C32 119.9(6) . . ? C34 C33 H33 122(4) . . ? C32 C33 H33 118(4) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 123(4) . . ? C33 C34 H34 116(4) . . ? C34 C35 C36 120.2(6) . . ? C34 C35 H35 124(4) . . ? C36 C35 H35 116(4) . . ? C31 C36 C35 119.7(5) . . ? C31 C36 H36 123(3) . . ? C35 C36 H36 116(3) . . ? N4 C40 H401 110(3) . . ? N4 C40 H402 109(3) . . ? H401 C40 H402 113(4) . . ? N4 C40 H403 111(3) . . ? H401 C40 H403 109(4) . . ? H402 C40 H403 105(4) . . ? H992 O99 H991 121(10) . . ? H981 O98 H982 100(8) . . ? H961 O96 H962 95(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag QO Yb P1 O12 -40.55(16) . . . . ? QN Yb P1 O12 134.16(16) . . . . ? O32 Yb P1 O12 -99.19(17) 3_665 . . . ? O11 Yb P1 O12 -100.6(3) . . . . ? O21 Yb P1 O12 19.23(17) . . . . ? O31 Yb P1 O12 -16.46(19) . . . . ? N2 Yb P1 O12 78.67(17) . . . . ? N4 Yb P1 O12 -175.06(17) . . . . ? N3 Yb P1 O12 158.0(2) . . . . ? N1 Yb P1 O12 122.43(18) . . . . ? P2 Yb P1 O12 30.26(16) . . . . ? QO Yb P1 O11 60.0(2) . . . . ? QN Yb P1 O11 -125.3(2) . . . . ? O32 Yb P1 O11 1.4(2) 3_665 . . . ? O21 Yb P1 O11 119.8(2) . . . . ? O31 Yb P1 O11 84.1(2) . . . . ? N2 Yb P1 O11 179.2(2) . . . . ? N4 Yb P1 O11 -74.5(2) . . . . ? N3 Yb P1 O11 -101.4(3) . . . . ? N1 Yb P1 O11 -137.0(2) . . . . ? P2 Yb P1 O11 130.8(2) . . . . ? QO Yb P1 C11 114.3(2) . . . . ? QN Yb P1 C11 -71.0(2) . . . . ? O32 Yb P1 C11 55.7(2) 3_665 . . . ? O11 Yb P1 C11 54.3(3) . . . . ? O21 Yb P1 C11 174.1(2) . . . . ? O31 Yb P1 C11 138.4(2) . . . . ? N2 Yb P1 C11 -126.5(2) . . . . ? N4 Yb P1 C11 -20.2(2) . . . . ? N3 Yb P1 C11 -47.1(3) . . . . ? N1 Yb P1 C11 -82.7(2) . . . . ? P2 Yb P1 C11 -174.9(2) . . . . ? QO Yb P1 C10 -143.89(16) . . . . ? QN Yb P1 C10 30.82(16) . . . . ? O32 Yb P1 C10 157.47(17) 3_665 . . . ? O11 Yb P1 C10 156.1(3) . . . . ? O21 Yb P1 C10 -84.11(18) . . . . ? O31 Yb P1 C10 -119.80(18) . . . . ? N2 Yb P1 C10 -24.68(18) . . . . ? N4 Yb P1 C10 81.59(17) . . . . ? N3 Yb P1 C10 54.7(3) . . . . ? N1 Yb P1 C10 19.08(18) . . . . ? P2 Yb P1 C10 -73.08(16) . . . . ? QO Yb P2 O22 119.17(18) . . . . ? QN Yb P2 O22 -66.59(18) . . . . ? O32 Yb P2 O22 140.1(2) 3_665 . . . ? O11 Yb P2 O22 54.1(2) . . . . ? O21 Yb P2 O22 66.5(3) . . . . ? O31 Yb P2 O22 -176.7(2) . . . . ? N2 Yb P2 O22 -78.0(2) . . . . ? N4 Yb P2 O22 -45.3(3) . . . . ? N3 Yb P2 O22 -122.3(2) . . . . ? N1 Yb P2 O22 -15.4(2) . . . . ? P1 Yb P2 O22 37.74(18) . . . . ? QO Yb P2 O21 52.7(2) . . . . ? QN Yb P2 O21 -133.1(2) . . . . ? O32 Yb P2 O21 73.6(2) 3_665 . . . ? O11 Yb P2 O21 -12.4(2) . . . . ? O31 Yb P2 O21 116.8(2) . . . . ? N2 Yb P2 O21 -144.5(2) . . . . ? N4 Yb P2 O21 -111.7(3) . . . . ? N3 Yb P2 O21 171.3(2) . . . . ? N1 Yb P2 O21 -81.9(2) . . . . ? P1 Yb P2 O21 -28.7(2) . . . . ? QO Yb P2 C21 -37.87(17) . . . . ? QN Yb P2 C21 136.36(17) . . . . ? O32 Yb P2 C21 -16.96(19) 3_665 . . . ? O11 Yb P2 C21 -102.94(18) . . . . ? O21 Yb P2 C21 -90.6(3) . . . . ? O31 Yb P2 C21 26.23(18) . . . . ? N2 Yb P2 C21 124.96(19) . . . . ? N4 Yb P2 C21 157.7(2) . . . . ? N3 Yb P2 C21 80.70(19) . . . . ? N1 Yb P2 C21 -172.49(18) . . . . ? P1 Yb P2 C21 -119.31(17) . . . . ? QO Yb P2 C20 -139.61(15) . . . . ? QN Yb P2 C20 34.63(15) . . . . ? O32 Yb P2 C20 -118.69(18) 3_665 . . . ? O11 Yb P2 C20 155.33(17) . . . . ? O21 Yb P2 C20 167.7(3) . . . . ? O31 Yb P2 C20 -75.51(17) . . . . ? N2 Yb P2 C20 23.23(18) . . . . ? N4 Yb P2 C20 56.0(2) . . . . ? N3 Yb P2 C20 -21.03(17) . . . . ? N1 Yb P2 C20 85.78(17) . . . . ? P1 Yb P2 C20 138.96(15) . . . . ? QO Yb P3 O32 -44.92(13) . . . . ? QN Yb P3 O32 140.47(13) . . . . ? O32 Yb P3 O32 22.5(2) 3_665 . . . ? O11 Yb P3 O32 -15.91(18) . . . . ? O21 Yb P3 O32 -98.06(15) . . . . ? O31 Yb P3 O32 -98.8(2) . . . . ? N2 Yb P3 O32 -168.23(15) . . . . ? N4 Yb P3 O32 86.03(15) . . . . ? N3 Yb P3 O32 126.77(17) . . . . ? N1 Yb P3 O32 164.9(2) . . . . ? P1 Yb P3 O32 -42.52(15) . . . . ? P2 Yb P3 O32 -116.02(13) . . . . ? QO Yb P3 O31 53.90(19) . . . . ? QN Yb P3 O31 -120.71(19) . . . . ? O32 Yb P3 O31 121.4(2) 3_665 . . . ? O11 Yb P3 O31 82.9(2) . . . . ? O21 Yb P3 O31 0.8(2) . . . . ? N2 Yb P3 O31 -69.4(2) . . . . ? N4 Yb P3 O31 -175.1(2) . . . . ? N3 Yb P3 O31 -134.4(2) . . . . ? N1 Yb P3 O31 -96.3(2) . . . . ? P1 Yb P3 O31 56.3(2) . . . . ? P2 Yb P3 O31 -17.20(19) . . . . ? QO Yb P3 C31 109.2(2) . . . . ? QN Yb P3 C31 -65.4(2) . . . . ? O32 Yb P3 C31 176.7(2) 3_665 . . . ? O11 Yb P3 C31 138.2(2) . . . . ? O21 Yb P3 C31 56.1(2) . . . . ? O31 Yb P3 C31 55.3(3) . . . . ? N2 Yb P3 C31 -14.1(2) . . . . ? N4 Yb P3 C31 -119.8(2) . . . . ? N3 Yb P3 C31 -79.1(2) . . . . ? N1 Yb P3 C31 -41.0(3) . . . . ? P1 Yb P3 C31 111.6(2) . . . . ? P2 Yb P3 C31 38.1(2) . . . . ? QO Yb P3 C30 -149.46(15) . . . . ? QN Yb P3 C30 35.92(15) . . . . ? O32 Yb P3 C30 -82.01(17) 3_665 . . . ? O11 Yb P3 C30 -120.45(19) . . . . ? O21 Yb P3 C30 157.39(17) . . . . ? O31 Yb P3 C30 156.6(2) . . . . ? N2 Yb P3 C30 87.22(17) . . . . ? N4 Yb P3 C30 -18.52(17) . . . . ? N3 Yb P3 C30 22.22(18) . . . . ? N1 Yb P3 C30 60.3(2) . . . . ? P1 Yb P3 C30 -147.07(16) . . . . ? P2 Yb P3 C30 139.43(15) . . . . ? O12 P1 O11 Yb 97.7(2) . . . . ? C11 P1 O11 Yb -139.9(2) . . . . ? C10 P1 O11 Yb -23.7(3) . . . . ? QO Yb O11 P1 -115.1(2) . . . . ? QN Yb O11 P1 61.6(2) . . . . ? O32 Yb O11 P1 -178.6(2) 3_665 . . . ? O21 Yb O11 P1 -54.8(2) . . . . ? O31 Yb O11 P1 -115.29(19) . . . . ? N2 Yb O11 P1 -1.0(3) . . . . ? N4 Yb O11 P1 104.5(2) . . . . ? N3 Yb O11 P1 122.5(2) . . . . ? N1 Yb O11 P1 35.54(19) . . . . ? P2 Yb O11 P1 -50.2(2) . . . . ? O22 P2 O21 Yb -133.97(19) . . . . ? C21 P2 O21 Yb 103.6(2) . . . . ? C20 P2 O21 Yb -12.2(3) . . . . ? QO Yb O21 P2 -118.6(2) . . . . ? QN Yb O21 P2 53.5(2) . . . . ? O32 Yb O21 P2 -120.44(19) 3_665 . . . ? O11 Yb O21 P2 167.6(2) . . . . ? O31 Yb O21 P2 -56.19(19) . . . . ? N2 Yb O21 P2 29.14(18) . . . . ? N4 Yb O21 P2 114.7(3) . . . . ? N3 Yb O21 P2 -10.7(3) . . . . ? N1 Yb O21 P2 97.4(2) . . . . ? P1 Yb O21 P2 148.8(2) . . . . ? O32 P3 O31 Yb 98.4(2) . . . . ? C31 P3 O31 Yb -140.64(19) . . . . ? C30 P3 O31 Yb -23.3(2) . . . . ? QO Yb O31 P3 -117.17(19) . . . . ? QN Yb O31 P3 66.08(19) . . . . ? O32 Yb O31 P3 -52.11(18) 3_665 . . . ? O11 Yb O31 P3 -116.98(19) . . . . ? O21 Yb O31 P3 -179.2(2) . . . . ? N2 Yb O31 P3 108.59(19) . . . . ? N4 Yb O31 P3 6.1(3) . . . . ? N3 Yb O31 P3 37.22(18) . . . . ? N1 Yb O31 P3 123.4(2) . . . . ? P1 Yb O31 P3 -145.23(13) . . . . ? P2 Yb O31 P3 160.9(2) . . . . ? O31 P3 O32 Yb -134.6(5) . . . 3_665 ? C31 P3 O32 Yb 103.3(5) . . . 3_665 ? C30 P3 O32 Yb -15.1(6) . . . 3_665 ? Yb P3 O32 Yb -96.1(5) . . . 3_665 ? QO Yb N1 C10 -1.4(3) . . . . ? QN Yb N1 C10 170.3(3) . . . . ? O32 Yb N1 C10 -91.1(3) 3_665 . . . ? O11 Yb N1 C10 -39.5(3) . . . . ? O21 Yb N1 C10 40.5(3) . . . . ? O31 Yb N1 C10 95.2(3) . . . . ? N2 Yb N1 C10 110.9(3) . . . . ? N4 Yb N1 C10 -131.4(3) . . . . ? N3 Yb N1 C10 170.4(2) . . . . ? P1 Yb N1 C10 -24.1(2) . . . . ? P2 Yb N1 C10 62.0(3) . . . . ? QO Yb N1 C1 -121.5(2) . . . . ? QN Yb N1 C1 50.2(2) . . . . ? O32 Yb N1 C1 148.9(2) 3_665 . . . ? O11 Yb N1 C1 -159.5(3) . . . . ? O21 Yb N1 C1 -79.5(3) . . . . ? O31 Yb N1 C1 -24.9(4) . . . . ? N2 Yb N1 C1 -9.2(3) . . . . ? N4 Yb N1 C1 108.6(3) . . . . ? N3 Yb N1 C1 50.3(3) . . . . ? P1 Yb N1 C1 -144.1(3) . . . . ? P2 Yb N1 C1 -58.1(3) . . . . ? QO Yb N1 C8 117.1(2) . . . . ? QN Yb N1 C8 -71.3(2) . . . . ? O32 Yb N1 C8 27.4(3) 3_665 . . . ? O11 Yb N1 C8 79.0(3) . . . . ? O21 Yb N1 C8 159.0(3) . . . . ? O31 Yb N1 C8 -146.4(2) . . . . ? N2 Yb N1 C8 -130.6(3) . . . . ? N4 Yb N1 C8 -12.9(2) . . . . ? N3 Yb N1 C8 -71.1(3) . . . . ? P1 Yb N1 C8 94.4(3) . . . . ? P2 Yb N1 C8 -179.6(3) . . . . ? QO Yb N2 C3 -130.3(2) . . . . ? QN Yb N2 C3 44.7(2) . . . . ? O32 Yb N2 C3 -44.3(4) 3_665 . . . ? O11 Yb N2 C3 140.3(2) . . . . ? O21 Yb N2 C3 -162.3(3) . . . . ? O31 Yb N2 C3 -84.9(3) . . . . ? N4 Yb N2 C3 44.8(3) . . . . ? N3 Yb N2 C3 -14.4(2) . . . . ? N1 Yb N2 C3 103.4(3) . . . . ? P1 Yb N2 C3 140.0(2) . . . . ? P2 Yb N2 C3 -149.2(3) . . . . ? QO Yb N2 C20 -10.0(3) . . . . ? QN Yb N2 C20 165.0(3) . . . . ? O32 Yb N2 C20 76.1(3) 3_665 . . . ? O11 Yb N2 C20 -99.3(3) . . . . ? O21 Yb N2 C20 -41.9(2) . . . . ? O31 Yb N2 C20 35.5(2) . . . . ? N4 Yb N2 C20 165.2(2) . . . . ? N3 Yb N2 C20 106.0(3) . . . . ? N1 Yb N2 C20 -136.2(3) . . . . ? P1 Yb N2 C20 -99.7(2) . . . . ? P2 Yb N2 C20 -28.8(2) . . . . ? QO Yb N2 C2 107.1(2) . . . . ? QN Yb N2 C2 -77.9(2) . . . . ? O32 Yb N2 C2 -166.9(2) 3_665 . . . ? O11 Yb N2 C2 17.8(3) . . . . ? O21 Yb N2 C2 75.1(3) . . . . ? O31 Yb N2 C2 152.5(3) . . . . ? N4 Yb N2 C2 -77.7(3) . . . . ? N3 Yb N2 C2 -137.0(3) . . . . ? N1 Yb N2 C2 -19.2(2) . . . . ? P1 Yb N2 C2 17.4(3) . . . . ? P2 Yb N2 C2 88.3(3) . . . . ? QO Yb N3 C5 -137.8(3) . . . . ? QN Yb N3 C5 49.6(3) . . . . ? O32 Yb N3 C5 -86.0(3) 3_665 . . . ? O11 Yb N3 C5 -28.1(4) . . . . ? O21 Yb N3 C5 148.6(3) . . . . ? O31 Yb N3 C5 -163.7(3) . . . . ? N2 Yb N3 C5 108.3(3) . . . . ? N4 Yb N3 C5 -8.7(3) . . . . ? N1 Yb N3 C5 49.5(3) . . . . ? P1 Yb N3 C5 20.4(4) . . . . ? P2 Yb N3 C5 144.4(3) . . . . ? QO Yb N3 C30 -18.4(3) . . . . ? QN Yb N3 C30 169.0(3) . . . . ? O32 Yb N3 C30 33.5(2) 3_665 . . . ? O11 Yb N3 C30 91.3(3) . . . . ? O21 Yb N3 C30 -92.0(3) . . . . ? O31 Yb N3 C30 -44.3(2) . . . . ? N2 Yb N3 C30 -132.2(3) . . . . ? N4 Yb N3 C30 110.7(3) . . . . ? N1 Yb N3 C30 168.9(2) . . . . ? P1 Yb N3 C30 139.9(2) . . . . ? P2 Yb N3 C30 -96.1(2) . . . . ? QO Yb N3 C4 99.7(2) . . . . ? QN Yb N3 C4 -73.0(2) . . . . ? O32 Yb N3 C4 151.5(3) 3_665 . . . ? O11 Yb N3 C4 -150.6(3) . . . . ? O21 Yb N3 C4 26.0(3) . . . . ? O31 Yb N3 C4 73.7(3) . . . . ? N2 Yb N3 C4 -14.2(2) . . . . ? N4 Yb N3 C4 -131.2(3) . . . . ? N1 Yb N3 C4 -73.1(3) . . . . ? P1 Yb N3 C4 -102.1(3) . . . . ? P2 Yb N3 C4 21.9(3) . . . . ? QO Yb N4 C40 -23.7(3) . . . . ? QN Yb N4 C40 162.2(3) . . . . ? O32 Yb N4 C40 -48.5(3) 3_665 . . . ? O11 Yb N4 C40 32.8(3) . . . . ? O21 Yb N4 C40 84.8(4) . . . . ? O31 Yb N4 C40 -106.8(3) . . . . ? N2 Yb N4 C40 162.1(3) . . . . ? N3 Yb N4 C40 -138.1(3) . . . . ? N1 Yb N4 C40 103.4(3) . . . . ? P1 Yb N4 C40 53.5(3) . . . . ? P2 Yb N4 C40 135.8(3) . . . . ? QO Yb N4 C6 94.1(3) . . . . ? QN Yb N4 C6 -80.0(3) . . . . ? O32 Yb N4 C6 69.3(3) 3_665 . . . ? O11 Yb N4 C6 150.6(3) . . . . ? O21 Yb N4 C6 -157.4(3) . . . . ? O31 Yb N4 C6 11.0(3) . . . . ? N2 Yb N4 C6 -80.1(3) . . . . ? N3 Yb N4 C6 -20.2(3) . . . . ? N1 Yb N4 C6 -138.8(3) . . . . ? P1 Yb N4 C6 171.3(3) . . . . ? P2 Yb N4 C6 -106.4(3) . . . . ? QO Yb N4 C7 -145.2(2) . . . . ? QN Yb N4 C7 40.8(2) . . . . ? O32 Yb N4 C7 -170.0(3) 3_665 . . . ? O11 Yb N4 C7 -88.7(3) . . . . ? O21 Yb N4 C7 -36.7(4) . . . . ? O31 Yb N4 C7 131.7(3) . . . . ? N2 Yb N4 C7 40.6(3) . . . . ? N3 Yb N4 C7 100.5(3) . . . . ? N1 Yb N4 C7 -18.1(3) . . . . ? P1 Yb N4 C7 -67.9(3) . . . . ? P2 Yb N4 C7 14.3(4) . . . . ? C10 N1 C1 C2 -81.6(4) . . . . ? C8 N1 C1 C2 159.6(4) . . . . ? Yb N1 C1 C2 36.7(4) . . . . ? C3 N2 C2 C1 -76.6(4) . . . . ? C20 N2 C2 C1 163.1(4) . . . . ? Yb N2 C2 C1 46.8(4) . . . . ? N1 C1 C2 N2 -56.9(5) . . . . ? C20 N2 C3 C4 -75.1(4) . . . . ? C2 N2 C3 C4 166.4(4) . . . . ? Yb N2 C3 C4 42.8(4) . . . . ? C5 N3 C4 C3 -82.4(4) . . . . ? C30 N3 C4 C3 158.5(4) . . . . ? Yb N3 C4 C3 42.0(4) . . . . ? N2 C3 C4 N3 -59.0(5) . . . . ? C30 N3 C5 C6 -81.2(5) . . . . ? C4 N3 C5 C6 159.6(4) . . . . ? Yb N3 C5 C6 36.8(4) . . . . ? C40 N4 C6 C5 171.0(4) . . . . ? C7 N4 C6 C5 -72.0(5) . . . . ? Yb N4 C6 C5 49.1(4) . . . . ? N3 C5 C6 N4 -59.3(5) . . . . ? C40 N4 C7 C8 -75.7(4) . . . . ? C6 N4 C7 C8 168.7(4) . . . . ? Yb N4 C7 C8 48.2(4) . . . . ? C10 N1 C8 C7 159.8(4) . . . . ? C1 N1 C8 C7 -81.0(4) . . . . ? Yb N1 C8 C7 42.8(4) . . . . ? N4 C7 C8 N1 -62.9(5) . . . . ? C1 N1 C10 P1 162.3(3) . . . . ? C8 N1 C10 P1 -79.3(4) . . . . ? Yb N1 C10 P1 40.3(3) . . . . ? O12 P1 C10 N1 -145.0(3) . . . . ? O11 P1 C10 N1 -17.2(4) . . . . ? C11 P1 C10 N1 98.6(3) . . . . ? Yb P1 C10 N1 -30.3(3) . . . . ? O12 P1 C11 C12 115.1(4) . . . . ? O11 P1 C11 C12 -14.1(4) . . . . ? C10 P1 C11 C12 -127.2(4) . . . . ? Yb P1 C11 C12 -41.8(5) . . . . ? O12 P1 C11 C16 -58.3(4) . . . . ? O11 P1 C11 C16 172.5(4) . . . . ? C10 P1 C11 C16 59.4(4) . . . . ? Yb P1 C11 C16 144.8(3) . . . . ? C16 C11 C12 C13 0.0(7) . . . . ? P1 C11 C12 C13 -173.5(4) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C16 1.3(8) . . . . ? C14 C15 C16 C11 -1.7(8) . . . . ? C12 C11 C16 C15 1.0(7) . . . . ? P1 C11 C16 C15 174.5(4) . . . . ? C3 N2 C20 P2 168.7(3) . . . . ? C2 N2 C20 P2 -71.5(4) . . . . ? Yb N2 C20 P2 48.0(3) . . . . ? O22 P2 C20 N2 97.8(3) . . . . ? O21 P2 C20 N2 -27.9(3) . . . . ? C21 P2 C20 N2 -145.9(3) . . . . ? Yb P2 C20 N2 -34.8(2) . . . . ? O22 P2 C21 C26 -120.0(4) . . . . ? O21 P2 C21 C26 7.4(4) . . . . ? C20 P2 C21 C26 122.0(4) . . . . ? Yb P2 C21 C26 43.3(4) . . . . ? O22 P2 C21 C22 55.4(4) . . . . ? O21 P2 C21 C22 -177.2(3) . . . . ? C20 P2 C21 C22 -62.7(4) . . . . ? Yb P2 C21 C22 -141.3(3) . . . . ? C26 C21 C22 C23 1.1(7) . . . . ? P2 C21 C22 C23 -174.4(4) . . . . ? C21 C22 C23 C24 0.4(8) . . . . ? C22 C23 C24 C25 -0.7(10) . . . . ? C23 C24 C25 C26 -0.6(10) . . . . ? C24 C25 C26 C21 2.1(9) . . . . ? C22 C21 C26 C25 -2.3(7) . . . . ? P2 C21 C26 C25 173.0(4) . . . . ? C5 N3 C30 P3 167.9(3) . . . . ? C4 N3 C30 P3 -72.7(4) . . . . ? Yb N3 C30 P3 46.0(3) . . . . ? O32 P3 C30 N3 -145.8(3) . . . . ? O31 P3 C30 N3 -20.3(3) . . . . ? C31 P3 C30 N3 97.0(3) . . . . ? Yb P3 C30 N3 -33.9(2) . . . . ? O32 P3 C31 C32 -82.1(4) . . . . ? O31 P3 C31 C32 151.8(4) . . . . ? C30 P3 C31 C32 36.7(4) . . . . ? Yb P3 C31 C32 122.2(3) . . . . ? O32 P3 C31 C36 90.3(4) . . . . ? O31 P3 C31 C36 -35.7(4) . . . . ? C30 P3 C31 C36 -150.8(3) . . . . ? Yb P3 C31 C36 -65.3(4) . . . . ? C36 C31 C32 C33 0.1(7) . . . . ? P3 C31 C32 C33 172.5(4) . . . . ? C31 C32 C33 C34 -3.0(8) . . . . ? C32 C33 C34 C35 3.5(8) . . . . ? C33 C34 C35 C36 -1.1(8) . . . . ? C32 C31 C36 C35 2.3(7) . . . . ? P3 C31 C36 C35 -170.4(4) . . . . ? C34 C35 C36 C31 -1.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.441 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.088 data_la4e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[La(H2O)L]2*10H2O (!centrosymmetric dimer!) ' _chemical_formula_sum 'C30 H52 La N4 O12 P3' _chemical_formula_weight 892.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no. 14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2355(12) _cell_length_b 20.229(4) _cell_length_c 15.6591(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.221(8) _cell_angle_gamma 90.00 _cell_volume 3982.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min -- _exptl_absorpt_correction_T_max -- _exptl_special_details ; crystal coated by thin paraphine film due to a loss of solvate molecules ; _diffrn_ambient_temperature 298(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 'CAD4 (Enraf-Nonius) ' _diffrn_measurement_method '.omege.-2.theta. ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min ' _diffrn_standards_decay_% 7.8 _diffrn_reflns_number 6270 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.09 _reflns_number_total 6254 _reflns_number_gt 5496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 program packet' _computing_cell_refinement 'CAD4 program packet' _computing_data_reduction 'JANA-98 (Petricek, 1998)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+15.4985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson + Fourier ' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00060(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6254 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1514 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 9.846 _refine_ls_shift/su_mean 0.058 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La La 0.66514(2) 0.613575(15) 0.03013(2) 0.03371(16) Uani 1 d . . . P1 P 0.90720(13) 0.65895(9) 0.19591(11) 0.0470(4) Uani 1 d . . . P2 P 0.56380(14) 0.77559(8) 0.05260(12) 0.0473(4) Uani 1 d . . . P3 P 0.40192(11) 0.56239(7) -0.08258(10) 0.0349(3) Uani 1 d . . . O11 O 0.8233(4) 0.6059(2) 0.1594(3) 0.0544(12) Uani 1 d . . . O12 O 0.8964(4) 0.7022(3) 0.2690(3) 0.0627(13) Uani 1 d . . . O21 O 0.6286(3) 0.7167(2) 0.0991(3) 0.0473(10) Uani 1 d . . . O22 O 0.6149(4) 0.8420(2) 0.0784(4) 0.0643(13) Uani 1 d . . . O31 O 0.4694(3) 0.61077(19) -0.0157(3) 0.0413(10) Uani 1 d . . . O32 O 0.3697(3) 0.5007(2) -0.0448(3) 0.0413(9) Uani 1 d . . . N1 N 0.8483(4) 0.6795(3) 0.0120(3) 0.0417(11) Uani 1 d . . . N2 N 0.6239(4) 0.7230(2) -0.0859(3) 0.0420(11) Uani 1 d . . . N3 N 0.5641(4) 0.5851(3) -0.1536(3) 0.0389(11) Uani 1 d . . . N4 N 0.7889(4) 0.5413(3) -0.0532(4) 0.0435(12) Uani 1 d . . . C1 C 0.8201(5) 0.7307(3) -0.0598(5) 0.0514(16) Uani 1 d . . . H011 H 0.8124 0.7097 -0.1172 0.07(2) Uiso 1 calc R . . H012 H 0.8777 0.7624 -0.0486 0.08(3) Uiso 1 calc R . . C2 C 0.7186(5) 0.7669(3) -0.0653(5) 0.0513(16) Uani 1 d . . . H021 H 0.7272 0.7890 -0.0085 0.07(2) Uiso 1 calc R . . H022 H 0.7062 0.8006 -0.1115 0.049(18) Uiso 1 calc R . . C3 C 0.5918(5) 0.7036(3) -0.1815(4) 0.0492(15) Uani 1 d . . . H031 H 0.6550 0.6928 -0.1975 0.07(2) Uiso 1 calc R . . H032 H 0.5576 0.7410 -0.2180 0.049(18) Uiso 1 calc R . . C4 C 0.5172(5) 0.6455(3) -0.2032(4) 0.0465(15) Uani 1 d . . . H041 H 0.4531 0.6567 -0.1889 0.041(16) Uiso 1 calc R . . H042 H 0.4972 0.6367 -0.2672 0.08(3) Uiso 1 calc R . . C5 C 0.6376(5) 0.5534(3) -0.1962(4) 0.0480(15) Uani 1 d . . . H051 H 0.6764 0.5874 -0.2166 0.044(17) Uiso 1 calc R . . H052 H 0.5965 0.5284 -0.2484 0.038(15) Uiso 1 calc R . . C6 C 0.7157(5) 0.5079(3) -0.1320(4) 0.0488(16) Uani 1 d . . . H061 H 0.6763 0.4745 -0.1112 0.053(19) Uiso 1 calc R . . H062 H 0.7573 0.4854 -0.1643 0.042(16) Uiso 1 calc R . . C7 C 0.8649(5) 0.5826(3) -0.0806(4) 0.0476(15) Uani 1 d . . . H071 H 0.8272 0.6075 -0.1341 0.029(15) Uiso 1 calc R . . H072 H 0.9164 0.5545 -0.0954 0.039(16) Uiso 1 calc R . . C8 C 0.9226(5) 0.6301(4) -0.0065(5) 0.0482(15) Uani 1 d . . . H081 H 0.9568 0.6054 0.0479 0.035(16) Uiso 1 calc R . . H082 H 0.9775 0.6531 -0.0239 0.06(2) Uiso 1 calc R . . C10 C 0.9010(5) 0.7107(3) 0.0998(5) 0.0512(16) Uani 1 d . . . H101 H 0.8634 0.7511 0.1040 0.030(14) Uiso 1 calc R . . H102 H 0.9729 0.7227 0.1024 0.054(19) Uiso 1 calc R . . C11 C 1.0345(6) 0.6177(4) 0.2384(5) 0.0526(17) Uani 1 d . . . C12 C 1.0378(6) 0.5504(4) 0.2544(5) 0.067(2) Uani 1 d . . . H12 H 0.9758 0.5256 0.2346 0.05(2) Uiso 1 calc R . . C13 C 1.1324(8) 0.5202(5) 0.2995(6) 0.086(3) Uani 1 d . . . H13 H 1.1338 0.4749 0.3103 0.07(3) Uiso 1 calc R . . C14 C 1.2241(8) 0.5560(7) 0.3285(6) 0.095(4) Uani 1 d . . . H14 H 1.2874 0.5356 0.3610 0.08(3) Uiso 1 calc R . . C15 C 1.2226(7) 0.6218(6) 0.3096(7) 0.086(3) Uani 1 d . . . H15 H 1.2854 0.6460 0.3270 0.08(3) Uiso 1 calc R . . C16 C 1.1290(6) 0.6520(5) 0.2652(6) 0.070(2) Uani 1 d . . . H16 H 1.1289 0.6970 0.2527 0.06(2) Uiso 1 calc R . . C20 C 0.5360(5) 0.7592(3) -0.0670(4) 0.0470(15) Uani 1 d . . . H201 H 0.4712 0.7334 -0.0886 0.041(16) Uiso 1 calc R . . H202 H 0.5245 0.8008 -0.0994 0.043(17) Uiso 1 calc R . . C21 C 0.4364(6) 0.7767(4) 0.0710(5) 0.0583(19) Uani 1 d . . . C22 C 0.4012(7) 0.7224(5) 0.1090(6) 0.070(2) Uani 1 d . . . H22 H 0.4416 0.6839 0.1214 0.08(3) Uiso 1 calc R . . C23 C 0.3068(8) 0.7261(7) 0.1278(7) 0.096(3) Uani 1 d . . . H23 H 0.2840 0.6903 0.1543 0.11(4) Uiso 1 calc R . . C24 C 0.2461(9) 0.7819(9) 0.1080(9) 0.119(5) Uani 1 d . . . H24 H 0.1818 0.7837 0.1203 0.16(5) Uiso 1 calc R . . C25 C 0.2789(8) 0.8352(7) 0.0702(8) 0.108(4) Uani 1 d . . . H25 H 0.2375 0.8732 0.0575 0.10(3) Uiso 1 calc R . . C26 C 0.3731(7) 0.8324(6) 0.0510(6) 0.083(3) Uani 1 d . . . H26 H 0.3946 0.8685 0.0242 0.08(3) Uiso 1 calc R . . C30 C 0.4780(5) 0.5378(3) -0.1559(4) 0.0409(13) Uani 1 d . . . H301 H 0.5087 0.4945 -0.1379 0.035(15) Uiso 1 calc R . . H302 H 0.4305 0.5344 -0.2171 0.030(14) Uiso 1 calc R . . C31 C 0.2796(5) 0.6017(3) -0.1467(4) 0.0427(14) Uani 1 d . . . C32 C 0.2444(6) 0.6570(4) -0.1114(6) 0.0609(19) Uani 1 d . . . H32 H 0.2886 0.6780 -0.0605 0.07(2) Uiso 1 calc R . . C33 C 0.1431(7) 0.6801(5) -0.1531(7) 0.083(3) Uani 1 d . . . H33 H 0.1183 0.7160 -0.1282 0.044(17) Uiso 1 calc R . . C34 C 0.0789(7) 0.6523(6) -0.2286(8) 0.094(4) Uani 1 d . . . H34 H 0.0109 0.6689 -0.2555 0.10(3) Uiso 1 calc R . . C35 C 0.1141(7) 0.5997(5) -0.2656(7) 0.080(3) Uani 1 d . . . H35 H 0.0702 0.5810 -0.3185 0.14(5) Uiso 1 calc R . . C36 C 0.2137(6) 0.5740(4) -0.2256(5) 0.064(2) Uani 1 d . . . H36 H 0.2371 0.5380 -0.2514 0.05(2) Uiso 1 calc R . . C40 C 0.8495(5) 0.4899(3) 0.0093(5) 0.0533(17) Uani 1 d . . . H401 H 0.8012 0.4625 0.0281 0.08(3) Uiso 1 calc R . . H402 H 0.8985 0.5107 0.0610 0.06(2) Uiso 1 calc R . . H403 H 0.8882 0.4633 -0.0206 0.06(2) Uiso 1 calc R . . O99 O 0.6239(6) 0.6077(3) 0.1958(5) 0.086(3) Uani 1.00(2) d . . . O98 O 0.5707(15) 0.9551(7) -0.0222(13) 0.262(12) Uani 1.00(3) d . . . O97 O 0.941(4) 0.6169(18) 0.426(2) 0.62(5) Uani 1.00(6) d . . . O96 O 0.8062(5) 0.8315(3) 0.2219(4) 0.084(3) Uani 1.000(19) d . . . OW1 O 0.7156(19) 0.5460(9) 0.3597(11) 0.246(14) Uani 0.82(4) d P . . OW2 O 0.528(2) 0.0971(13) 0.205(2) 0.106(13) Uani 0.29(2) d P . . QN N 0.7063 0.6322 -0.0687 0.050 Uiso 0.00 d P . . QO O 0.6378 0.6081 0.0719 0.050 Uiso 0.00 d P . . 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 La 0.0281(2) 0.0328(2) 0.0406(2) 0.00050(13) 0.01125(15) 0.00080(12) P1 0.0365(8) 0.0588(10) 0.0448(9) -0.0026(8) 0.0113(7) -0.0050(7) P2 0.0456(9) 0.0407(9) 0.0536(10) -0.0028(7) 0.0127(8) 0.0065(7) P3 0.0273(7) 0.0344(8) 0.0425(8) 0.0018(6) 0.0100(6) 0.0038(6) O11 0.044(3) 0.061(3) 0.057(3) 0.008(2) 0.013(2) -0.008(2) O12 0.061(3) 0.075(3) 0.053(3) -0.008(2) 0.020(2) 0.007(3) O21 0.048(2) 0.043(2) 0.050(2) -0.0008(19) 0.013(2) 0.0043(19) O22 0.070(3) 0.040(3) 0.078(3) -0.008(2) 0.015(3) 0.002(2) O31 0.030(2) 0.044(2) 0.051(2) -0.0043(18) 0.0140(19) 0.0051(17) O32 0.032(2) 0.042(2) 0.051(2) 0.0053(19) 0.0135(18) 0.0039(17) N1 0.036(3) 0.045(3) 0.048(3) 0.001(2) 0.018(2) -0.003(2) N2 0.041(3) 0.039(3) 0.048(3) 0.002(2) 0.017(2) 0.000(2) N3 0.034(3) 0.046(3) 0.039(3) 0.000(2) 0.014(2) 0.002(2) N4 0.036(3) 0.047(3) 0.052(3) -0.001(2) 0.020(2) 0.008(2) C1 0.051(4) 0.052(4) 0.057(4) 0.008(3) 0.026(3) -0.007(3) C2 0.048(4) 0.046(4) 0.062(4) 0.011(3) 0.020(3) -0.001(3) C3 0.047(4) 0.057(4) 0.045(4) 0.006(3) 0.017(3) 0.000(3) C4 0.045(4) 0.052(4) 0.043(3) 0.003(3) 0.015(3) 0.003(3) C5 0.042(3) 0.058(4) 0.049(4) -0.014(3) 0.022(3) -0.003(3) C6 0.038(3) 0.055(4) 0.059(4) -0.011(3) 0.022(3) 0.005(3) C7 0.039(3) 0.060(4) 0.049(4) 0.002(3) 0.022(3) 0.008(3) C8 0.030(3) 0.064(4) 0.055(4) -0.001(3) 0.020(3) -0.002(3) C10 0.043(4) 0.053(4) 0.061(4) -0.010(3) 0.021(3) -0.010(3) C11 0.045(4) 0.067(5) 0.044(4) -0.007(3) 0.012(3) 0.000(3) C12 0.055(5) 0.080(6) 0.068(5) 0.009(4) 0.020(4) 0.007(4) C13 0.087(7) 0.089(7) 0.082(6) 0.023(5) 0.028(5) 0.029(6) C14 0.059(6) 0.157(11) 0.064(5) 0.000(6) 0.009(4) 0.042(7) C15 0.040(5) 0.139(10) 0.073(6) -0.024(6) 0.008(4) -0.001(5) C16 0.046(4) 0.086(6) 0.073(5) -0.015(4) 0.011(4) -0.011(4) C20 0.046(4) 0.041(3) 0.055(4) 0.003(3) 0.016(3) 0.004(3) C21 0.058(4) 0.067(5) 0.049(4) -0.013(3) 0.014(3) 0.018(4) C22 0.068(5) 0.074(6) 0.076(5) -0.011(4) 0.035(4) 0.000(4) C23 0.082(7) 0.123(9) 0.099(7) -0.012(7) 0.052(6) 0.003(7) C24 0.073(7) 0.181(15) 0.121(10) -0.019(9) 0.055(7) 0.013(8) C25 0.067(6) 0.152(12) 0.105(8) -0.012(8) 0.027(6) 0.054(7) C26 0.071(6) 0.108(8) 0.067(5) 0.007(5) 0.017(4) 0.033(5) C30 0.033(3) 0.041(3) 0.048(3) -0.001(3) 0.012(3) 0.001(2) C31 0.034(3) 0.040(3) 0.054(4) 0.012(3) 0.012(3) 0.005(3) C32 0.053(4) 0.056(4) 0.077(5) 0.009(4) 0.024(4) 0.016(3) C33 0.063(6) 0.078(6) 0.116(8) 0.036(6) 0.041(6) 0.041(5) C34 0.035(4) 0.112(8) 0.124(9) 0.061(7) 0.012(5) 0.022(5) C35 0.043(4) 0.081(6) 0.095(7) 0.025(5) -0.010(5) 0.000(4) C36 0.043(4) 0.072(5) 0.067(5) 0.002(4) 0.004(4) 0.000(4) C40 0.044(4) 0.051(4) 0.069(5) 0.006(4) 0.024(3) 0.017(3) O99 0.100(6) 0.081(5) 0.093(5) 0.004(3) 0.052(4) -0.004(3) O98 0.31(2) 0.133(11) 0.31(2) 0.077(12) 0.042(16) 0.030(11) O97 0.99(12) 0.63(7) 0.37(4) 0.03(4) 0.40(6) 0.46(7) O96 0.067(4) 0.087(5) 0.097(5) -0.028(4) 0.025(3) -0.011(3) OW1 0.32(3) 0.196(18) 0.151(14) -0.043(11) -0.020(14) 0.100(17) OW2 0.11(2) 0.098(19) 0.14(3) 0.039(16) 0.078(19) 0.024(15) _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 La QO 0.8485(3) . ? La QN 1.8337(4) . ? La O32 2.382(4) 3_665 ? La O11 2.419(5) . ? La O31 2.464(4) . ? La O21 2.466(4) . ? La N4 2.803(5) . ? La N2 2.806(5) . ? La O99 2.815(6) . ? La N3 2.827(5) . ? La N1 2.858(5) . ? P1 O12 1.483(5) . ? P1 O11 1.522(5) . ? P1 C11 1.810(7) . ? P1 C10 1.815(7) . ? P2 O22 1.501(5) . ? P2 O21 1.515(5) . ? P2 C21 1.798(8) . ? P2 C20 1.822(7) . ? P3 O32 1.499(4) . ? P3 O31 1.505(4) . ? P3 C31 1.802(6) . ? P3 C30 1.818(6) . ? O32 La 2.382(4) 3_665 ? N1 C10 1.474(8) . ? N1 C1 1.486(8) . ? N1 C8 1.493(8) . ? N2 C3 1.476(8) . ? N2 C20 1.481(8) . ? N2 C2 1.487(8) . ? N3 C4 1.477(8) . ? N3 C30 1.479(8) . ? N3 C5 1.486(7) . ? N4 C7 1.472(8) . ? N4 C6 1.474(8) . ? N4 C40 1.480(8) . ? C1 C2 1.509(9) . ? C1 H011 0.9700 . ? C1 H012 0.9700 . ? C2 H021 0.9700 . ? C2 H022 0.9700 . ? C3 C4 1.503(9) . ? C3 H031 0.9700 . ? C3 H032 0.9700 . ? C4 H041 0.9700 . ? C4 H042 0.9700 . ? C5 C6 1.509(9) . ? C5 H051 0.9700 . ? C5 H052 0.9700 . ? C6 H061 0.9700 . ? C6 H062 0.9700 . ? C7 C8 1.516(9) . ? C7 H071 0.9700 . ? C7 H072 0.9700 . ? C8 H081 0.9700 . ? C8 H082 0.9700 . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C11 C16 1.377(10) . ? C11 C12 1.381(11) . ? C12 C13 1.373(12) . ? C12 H12 0.9300 . ? C13 C14 1.364(15) . ? C13 H13 0.9300 . ? C14 C15 1.362(15) . ? C14 H14 0.9300 . ? C15 C16 1.361(13) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C20 H201 0.9700 . ? C20 H202 0.9700 . ? C21 C26 1.381(11) . ? C21 C22 1.395(12) . ? C22 C23 1.374(12) . ? C22 H22 0.9300 . ? C23 C24 1.363(17) . ? C23 H23 0.9300 . ? C24 C25 1.364(18) . ? C24 H24 0.9300 . ? C25 C26 1.373(14) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 C36 1.389(10) . ? C31 C32 1.391(10) . ? C32 C33 1.376(11) . ? C32 H32 0.9300 . ? C33 C34 1.345(15) . ? C33 H33 0.9300 . ? C34 C35 1.361(16) . ? C34 H34 0.9300 . ? C35 C36 1.374(11) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C40 H401 0.9600 . ? C40 H402 0.9600 . ? C40 H403 0.9600 . ? 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 QO La QN 171.53(3) . . ? QO La O32 69.95(10) . 3_665 ? QN La O32 113.50(10) . 3_665 ? QO La O11 79.16(12) . . ? QN La O11 108.17(12) . . ? O32 La O11 89.99(14) 3_665 . ? QO La O31 63.80(10) . . ? QN La O31 108.77(10) . . ? O32 La O31 77.76(13) 3_665 . ? O11 La O31 142.96(16) . . ? QO La O21 65.31(10) . . ? QN La O21 110.29(10) . . ? O32 La O21 135.08(14) 3_665 . ? O11 La O21 85.68(16) . . ? O31 La O21 79.31(14) . . ? QO La N4 138.04(11) . . ? QN La N4 48.95(11) . . ? O32 La N4 72.43(15) 3_665 . ? O11 La N4 82.96(16) . . ? O31 La N4 124.53(14) . . ? O21 La N4 150.27(15) . . ? QO La N2 123.94(10) . . ? QN La N2 48.74(10) . . ? O32 La N2 145.42(14) 3_665 . ? O11 La N2 122.33(15) . . ? O31 La N2 81.68(14) . . ? O21 La N2 65.88(14) . . ? N4 La N2 97.69(15) . . ? QO La O99 14.37(15) . . ? QN La O99 168.73(13) . . ? O32 La O99 76.78(16) 3_665 . ? O11 La O99 65.94(19) . . ? O31 La O99 77.21(18) . . ? O21 La O99 60.69(16) . . ? N4 La O99 135.79(18) . . ? N2 La O99 125.09(17) . . ? QO La N3 125.35(10) . . ? QN La N3 49.75(10) . . ? O32 La N3 81.73(14) 3_665 . ? O11 La N3 148.07(16) . . ? O31 La N3 65.09(14) . . ? O21 La N3 121.54(14) . . ? N4 La N3 65.14(15) . . ? N2 La N3 64.38(15) . . ? O99 La N3 139.72(18) . . ? QO La N1 135.82(11) . . ? QN La N1 48.30(10) . . ? O32 La N1 131.19(14) 3_665 . ? O11 La N1 64.83(15) . . ? O31 La N1 146.01(14) . . ? O21 La N1 86.41(15) . . ? N4 La N1 63.89(15) . . ? N2 La N1 64.33(15) . . ? O99 La N1 121.73(18) . . ? N3 La N1 98.04(14) . . ? O12 P1 O11 118.1(3) . . ? O12 P1 C11 107.0(3) . . ? O11 P1 C11 107.4(3) . . ? O12 P1 C10 108.1(3) . . ? O11 P1 C10 104.9(3) . . ? C11 P1 C10 111.5(3) . . ? O22 P2 O21 115.8(3) . . ? O22 P2 C21 108.2(3) . . ? O21 P2 C21 110.5(3) . . ? O22 P2 C20 111.6(3) . . ? O21 P2 C20 104.7(3) . . ? C21 P2 C20 105.6(3) . . ? O32 P3 O31 116.5(2) . . ? O32 P3 C31 105.7(3) . . ? O31 P3 C31 109.6(3) . . ? O32 P3 C30 107.7(3) . . ? O31 P3 C30 107.0(3) . . ? C31 P3 C30 110.3(3) . . ? P1 O11 La 127.4(3) . . ? P2 O21 La 127.8(2) . . ? P3 O31 La 124.0(2) . . ? P3 O32 La 159.0(3) . 3_665 ? C10 N1 C1 110.0(5) . . ? C10 N1 C8 108.6(5) . . ? C1 N1 C8 110.1(5) . . ? C10 N1 La 106.0(3) . . ? C1 N1 La 112.3(4) . . ? C8 N1 La 109.7(4) . . ? C3 N2 C20 109.8(5) . . ? C3 N2 C2 109.5(5) . . ? C20 N2 C2 108.8(5) . . ? C3 N2 La 112.5(4) . . ? C20 N2 La 105.5(3) . . ? C2 N2 La 110.5(4) . . ? C4 N3 C30 109.2(5) . . ? C4 N3 C5 110.3(5) . . ? C30 N3 C5 108.5(5) . . ? C4 N3 La 110.7(4) . . ? C30 N3 La 105.8(3) . . ? C5 N3 La 112.1(3) . . ? C7 N4 C6 110.3(5) . . ? C7 N4 C40 108.2(5) . . ? C6 N4 C40 108.0(5) . . ? C7 N4 La 113.1(4) . . ? C6 N4 La 107.6(3) . . ? C40 N4 La 109.5(4) . . ? N1 C1 C2 112.9(5) . . ? N1 C1 H011 109.0 . . ? C2 C1 H011 109.0 . . ? N1 C1 H012 109.0 . . ? C2 C1 H012 109.0 . . ? H011 C1 H012 107.8 . . ? N2 C2 C1 113.4(5) . . ? N2 C2 H021 108.9 . . ? C1 C2 H021 108.9 . . ? N2 C2 H022 108.9 . . ? C1 C2 H022 108.9 . . ? H021 C2 H022 107.7 . . ? N2 C3 C4 113.4(5) . . ? N2 C3 H031 108.9 . . ? C4 C3 H031 108.9 . . ? N2 C3 H032 108.9 . . ? C4 C3 H032 108.9 . . ? H031 C3 H032 107.7 . . ? N3 C4 C3 113.0(5) . . ? N3 C4 H041 109.0 . . ? C3 C4 H041 109.0 . . ? N3 C4 H042 109.0 . . ? C3 C4 H042 109.0 . . ? H041 C4 H042 107.8 . . ? N3 C5 C6 111.8(5) . . ? N3 C5 H051 109.2 . . ? C6 C5 H051 109.2 . . ? N3 C5 H052 109.2 . . ? C6 C5 H052 109.2 . . ? H051 C5 H052 107.9 . . ? N4 C6 C5 114.3(5) . . ? N4 C6 H061 108.7 . . ? C5 C6 H061 108.7 . . ? N4 C6 H062 108.7 . . ? C5 C6 H062 108.7 . . ? H061 C6 H062 107.6 . . ? N4 C7 C8 111.3(5) . . ? N4 C7 H071 109.4 . . ? C8 C7 H071 109.4 . . ? N4 C7 H072 109.4 . . ? C8 C7 H072 109.4 . . ? H071 C7 H072 108.0 . . ? N1 C8 C7 111.6(5) . . ? N1 C8 H081 109.3 . . ? C7 C8 H081 109.3 . . ? N1 C8 H082 109.3 . . ? C7 C8 H082 109.3 . . ? H081 C8 H082 108.0 . . ? N1 C10 P1 114.4(4) . . ? N1 C10 H101 108.7 . . ? P1 C10 H101 108.7 . . ? N1 C10 H102 108.7 . . ? P1 C10 H102 108.7 . . ? H101 C10 H102 107.6 . . ? C16 C11 C12 117.9(8) . . ? C16 C11 P1 122.1(6) . . ? C12 C11 P1 119.6(6) . . ? C13 C12 C11 120.3(9) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 120.5(10) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.7(9) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 120.0(9) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 121.5(9) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? N2 C20 P2 112.1(4) . . ? N2 C20 H201 109.2 . . ? P2 C20 H201 109.2 . . ? N2 C20 H202 109.2 . . ? P2 C20 H202 109.2 . . ? H201 C20 H202 107.9 . . ? C26 C21 C22 118.7(8) . . ? C26 C21 P2 120.4(7) . . ? C22 C21 P2 120.9(6) . . ? C23 C22 C21 119.7(9) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 120.5(12) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.5(10) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.9(11) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.7(11) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? N3 C30 P3 112.5(4) . . ? N3 C30 H301 109.1 . . ? P3 C30 H301 109.1 . . ? N3 C30 H302 109.1 . . ? P3 C30 H302 109.1 . . ? H301 C30 H302 107.8 . . ? C36 C31 C32 118.9(6) . . ? C36 C31 P3 121.5(5) . . ? C32 C31 P3 119.2(5) . . ? C33 C32 C31 118.8(8) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C32 121.9(9) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 119.7(8) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 120.6(9) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 119.9(9) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? N4 C40 H401 109.5 . . ? N4 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? N4 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 La 94.5(4) . . . . ? C11 P1 O11 La -144.6(3) . . . . ? C10 P1 O11 La -25.9(4) . . . . ? QO La O11 P1 -117.0(4) . . . . ? QN La O11 P1 58.7(4) . . . . ? O32 La O11 P1 173.5(4) 3_665 . . . ? O31 La O11 P1 -117.2(3) . . . . ? O21 La O11 P1 -51.3(4) . . . . ? N4 La O11 P1 101.2(4) . . . . ? N2 La O11 P1 6.5(4) . . . . ? O99 La O11 P1 -111.0(4) . . . . ? N3 La O11 P1 99.3(4) . . . . ? N1 La O11 P1 36.8(3) . . . . ? O22 P2 O21 La -131.9(3) . . . . ? C21 P2 O21 La 104.7(4) . . . . ? C20 P2 O21 La -8.5(4) . . . . ? QO La O21 P2 -125.4(3) . . . . ? QN La O21 P2 46.7(3) . . . . ? O32 La O21 P2 -119.8(3) 3_665 . . . ? O11 La O21 P2 154.5(3) . . . . ? O31 La O21 P2 -59.5(3) . . . . ? N4 La O21 P2 86.9(4) . . . . ? N2 La O21 P2 26.1(3) . . . . ? O99 La O21 P2 -140.7(4) . . . . ? N3 La O21 P2 -7.7(4) . . . . ? N1 La O21 P2 89.5(3) . . . . ? O32 P3 O31 La 94.4(3) . . . . ? C31 P3 O31 La -145.6(3) . . . . ? C30 P3 O31 La -26.1(4) . . . . ? QO La O31 P3 -122.1(3) . . . . ? QN La O31 P3 62.3(3) . . . . ? O32 La O31 P3 -48.6(3) 3_665 . . . ? O11 La O31 P3 -121.9(3) . . . . ? O21 La O31 P3 170.3(3) . . . . ? N4 La O31 P3 9.8(4) . . . . ? N2 La O31 P3 103.4(3) . . . . ? O99 La O31 P3 -127.6(3) . . . . ? N3 La O31 P3 37.9(3) . . . . ? N1 La O31 P3 103.5(3) . . . . ? O31 P3 O32 La -137.7(6) . . . 3_665 ? C31 P3 O32 La 100.3(7) . . . 3_665 ? C30 P3 O32 La -17.6(7) . . . 3_665 ? QO La N1 C10 -1.1(5) . . . . ? QN La N1 C10 168.6(4) . . . . ? O32 La N1 C10 -105.4(4) 3_665 . . . ? O11 La N1 C10 -39.7(4) . . . . ? O31 La N1 C10 112.0(4) . . . . ? O21 La N1 C10 47.2(4) . . . . ? N4 La N1 C10 -134.3(4) . . . . ? N2 La N1 C10 112.1(4) . . . . ? O99 La N1 C10 -4.8(5) . . . . ? N3 La N1 C10 168.5(4) . . . . ? QO La N1 C1 -121.3(4) . . . . ? QN La N1 C1 48.5(4) . . . . ? O32 La N1 C1 134.4(4) 3_665 . . . ? O11 La N1 C1 -159.9(5) . . . . ? O31 La N1 C1 -8.1(5) . . . . ? O21 La N1 C1 -73.0(4) . . . . ? N4 La N1 C1 105.6(4) . . . . ? N2 La N1 C1 -8.1(4) . . . . ? O99 La N1 C1 -125.0(4) . . . . ? N3 La N1 C1 48.4(4) . . . . ? QO La N1 C8 115.9(4) . . . . ? QN La N1 C8 -74.4(4) . . . . ? O32 La N1 C8 11.6(5) 3_665 . . . ? O11 La N1 C8 77.3(4) . . . . ? O31 La N1 C8 -131.0(4) . . . . ? O21 La N1 C8 164.2(4) . . . . ? N4 La N1 C8 -17.3(4) . . . . ? N2 La N1 C8 -130.9(4) . . . . ? O99 La N1 C8 112.2(4) . . . . ? N3 La N1 C8 -74.4(4) . . . . ? QO La N2 C3 -128.5(4) . . . . ? QN La N2 C3 46.1(3) . . . . ? O32 La N2 C3 -24.2(5) 3_665 . . . ? O11 La N2 C3 132.4(4) . . . . ? O31 La N2 C3 -78.0(4) . . . . ? O21 La N2 C3 -160.0(4) . . . . ? N4 La N2 C3 45.9(4) . . . . ? O99 La N2 C3 -145.9(4) . . . . ? N3 La N2 C3 -11.8(4) . . . . ? N1 La N2 C3 102.0(4) . . . . ? QO La N2 C20 -8.8(4) . . . . ? QN La N2 C20 165.8(4) . . . . ? O32 La N2 C20 95.6(4) 3_665 . . . ? O11 La N2 C20 -107.9(4) . . . . ? O31 La N2 C20 41.7(4) . . . . ? O21 La N2 C20 -40.3(4) . . . . ? N4 La N2 C20 165.6(4) . . . . ? O99 La N2 C20 -26.2(4) . . . . ? N3 La N2 C20 108.0(4) . . . . ? N1 La N2 C20 -138.3(4) . . . . ? QO La N2 C2 108.7(4) . . . . ? QN La N2 C2 -76.7(4) . . . . ? O32 La N2 C2 -147.0(4) 3_665 . . . ? O11 La N2 C2 9.6(5) . . . . ? O31 La N2 C2 159.2(4) . . . . ? O21 La N2 C2 77.2(4) . . . . ? N4 La N2 C2 -76.9(4) . . . . ? O99 La N2 C2 91.3(4) . . . . ? N3 La N2 C2 -134.5(4) . . . . ? N1 La N2 C2 -20.8(4) . . . . ? QO La N3 C4 97.4(4) . . . . ? QN La N3 C4 -73.8(4) . . . . ? O32 La N3 C4 155.6(4) 3_665 . . . ? O11 La N3 C4 -127.9(4) . . . . ? O31 La N3 C4 75.3(4) . . . . ? O21 La N3 C4 17.0(4) . . . . ? N4 La N3 C4 -130.0(4) . . . . ? N2 La N3 C4 -17.3(3) . . . . ? O99 La N3 C4 97.5(4) . . . . ? N1 La N3 C4 -73.8(4) . . . . ? QO La N3 C30 -20.8(4) . . . . ? QN La N3 C30 168.0(4) . . . . ? O32 La N3 C30 37.4(3) 3_665 . . . ? O11 La N3 C30 113.9(4) . . . . ? O31 La N3 C30 -42.9(3) . . . . ? O21 La N3 C30 -101.3(4) . . . . ? N4 La N3 C30 111.8(4) . . . . ? N2 La N3 C30 -135.5(4) . . . . ? O99 La N3 C30 -20.7(5) . . . . ? N1 La N3 C30 168.0(3) . . . . ? QO La N3 C5 -138.9(4) . . . . ? QN La N3 C5 49.9(4) . . . . ? O32 La N3 C5 -80.8(4) 3_665 . . . ? O11 La N3 C5 -4.3(6) . . . . ? O31 La N3 C5 -161.0(4) . . . . ? O21 La N3 C5 140.6(4) . . . . ? N4 La N3 C5 -6.4(4) . . . . ? N2 La N3 C5 106.3(4) . . . . ? O99 La N3 C5 -138.8(4) . . . . ? N1 La N3 C5 49.9(4) . . . . ? QO La N4 C7 -144.9(3) . . . . ? QN La N4 C7 41.9(4) . . . . ? O32 La N4 C7 -172.0(4) 3_665 . . . ? O11 La N4 C7 -79.7(4) . . . . ? O31 La N4 C7 127.2(4) . . . . ? O21 La N4 C7 -11.4(6) . . . . ? N2 La N4 C7 42.1(4) . . . . ? O99 La N4 C7 -124.0(4) . . . . ? N3 La N4 C7 99.1(4) . . . . ? N1 La N4 C7 -14.4(4) . . . . ? QO La N4 C6 93.1(4) . . . . ? QN La N4 C6 -80.2(4) . . . . ? O32 La N4 C6 66.0(4) 3_665 . . . ? O11 La N4 C6 158.2(4) . . . . ? O31 La N4 C6 5.2(5) . . . . ? O21 La N4 C6 -133.5(4) . . . . ? N2 La N4 C6 -80.0(4) . . . . ? O99 La N4 C6 113.9(4) . . . . ? N3 La N4 C6 -22.9(4) . . . . ? N1 La N4 C6 -136.4(4) . . . . ? QO La N4 C40 -24.1(5) . . . . ? QN La N4 C40 162.7(5) . . . . ? O32 La N4 C40 -51.2(4) 3_665 . . . ? O11 La N4 C40 41.0(4) . . . . ? O31 La N4 C40 -112.0(4) . . . . ? O21 La N4 C40 109.4(5) . . . . ? N2 La N4 C40 162.8(4) . . . . ? O99 La N4 C40 -3.2(5) . . . . ? N3 La N4 C40 -140.1(5) . . . . ? N1 La N4 C40 106.4(4) . . . . ? C10 N1 C1 C2 -81.1(7) . . . . ? C8 N1 C1 C2 159.3(6) . . . . ? La N1 C1 C2 36.7(7) . . . . ? C3 N2 C2 C1 -74.2(7) . . . . ? C20 N2 C2 C1 165.7(6) . . . . ? La N2 C2 C1 50.3(6) . . . . ? N1 C1 C2 N2 -60.9(8) . . . . ? C20 N2 C3 C4 -76.4(7) . . . . ? C2 N2 C3 C4 164.2(5) . . . . ? La N2 C3 C4 40.8(6) . . . . ? C30 N3 C4 C3 162.3(5) . . . . ? C5 N3 C4 C3 -78.5(6) . . . . ? La N3 C4 C3 46.2(6) . . . . ? N2 C3 C4 N3 -61.0(7) . . . . ? C4 N3 C5 C6 159.2(5) . . . . ? C30 N3 C5 C6 -81.2(6) . . . . ? La N3 C5 C6 35.3(6) . . . . ? C7 N4 C6 C5 -69.8(6) . . . . ? C40 N4 C6 C5 172.1(5) . . . . ? La N4 C6 C5 54.0(6) . . . . ? N3 C5 C6 N4 -63.6(7) . . . . ? C6 N4 C7 C8 166.0(5) . . . . ? C40 N4 C7 C8 -76.1(7) . . . . ? La N4 C7 C8 45.4(6) . . . . ? C10 N1 C8 C7 163.6(5) . . . . ? C1 N1 C8 C7 -76.0(7) . . . . ? La N1 C8 C7 48.2(6) . . . . ? N4 C7 C8 N1 -65.3(7) . . . . ? C1 N1 C10 P1 164.1(4) . . . . ? C8 N1 C10 P1 -75.4(6) . . . . ? La N1 C10 P1 42.4(5) . . . . ? O12 P1 C10 N1 -145.3(5) . . . . ? O11 P1 C10 N1 -18.5(5) . . . . ? C11 P1 C10 N1 97.4(5) . . . . ? O12 P1 C11 C16 -61.1(7) . . . . ? O11 P1 C11 C16 171.2(6) . . . . ? C10 P1 C11 C16 56.8(7) . . . . ? O12 P1 C11 C12 111.3(6) . . . . ? O11 P1 C11 C12 -16.4(7) . . . . ? C10 P1 C11 C12 -130.8(6) . . . . ? C16 C11 C12 C13 3.0(12) . . . . ? P1 C11 C12 C13 -169.8(7) . . . . ? C11 C12 C13 C14 -0.4(14) . . . . ? C12 C13 C14 C15 -2.5(15) . . . . ? C13 C14 C15 C16 2.7(15) . . . . ? C14 C15 C16 C11 -0.1(14) . . . . ? C12 C11 C16 C15 -2.8(12) . . . . ? P1 C11 C16 C15 169.8(7) . . . . ? C3 N2 C20 P2 172.8(4) . . . . ? C2 N2 C20 P2 -67.3(6) . . . . ? La N2 C20 P2 51.3(4) . . . . ? O22 P2 C20 N2 92.8(5) . . . . ? O21 P2 C20 N2 -33.2(5) . . . . ? C21 P2 C20 N2 -149.9(5) . . . . ? O22 P2 C21 C26 38.9(7) . . . . ? O21 P2 C21 C26 166.6(6) . . . . ? C20 P2 C21 C26 -80.7(7) . . . . ? O22 P2 C21 C22 -138.5(6) . . . . ? O21 P2 C21 C22 -10.8(7) . . . . ? C20 P2 C21 C22 101.8(6) . . . . ? C26 C21 C22 C23 -1.8(12) . . . . ? P2 C21 C22 C23 175.7(7) . . . . ? C21 C22 C23 C24 1.4(15) . . . . ? C22 C23 C24 C25 -0.9(19) . . . . ? C23 C24 C25 C26 0.8(19) . . . . ? C24 C25 C26 C21 -1.2(17) . . . . ? C22 C21 C26 C25 1.7(13) . . . . ? P2 C21 C26 C25 -175.8(8) . . . . ? C4 N3 C30 P3 -73.7(5) . . . . ? C5 N3 C30 P3 166.0(4) . . . . ? La N3 C30 P3 45.5(4) . . . . ? O32 P3 C30 N3 -145.4(4) . . . . ? O31 P3 C30 N3 -19.4(5) . . . . ? C31 P3 C30 N3 99.7(4) . . . . ? O32 P3 C31 C36 -68.3(6) . . . . ? O31 P3 C31 C36 165.4(6) . . . . ? C30 P3 C31 C36 47.9(7) . . . . ? O32 P3 C31 C32 104.4(6) . . . . ? O31 P3 C31 C32 -22.0(6) . . . . ? C30 P3 C31 C32 -139.5(5) . . . . ? C36 C31 C32 C33 3.6(11) . . . . ? P3 C31 C32 C33 -169.2(6) . . . . ? C31 C32 C33 C34 -2.6(13) . . . . ? C32 C33 C34 C35 0.1(15) . . . . ? C33 C34 C35 C36 1.2(15) . . . . ? C34 C35 C36 C31 0.0(14) . . . . ? C32 C31 C36 C35 -2.4(11) . . . . ? P3 C31 C36 C35 170.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 24.09 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 2.087 _refine_diff_density_min -2.328 _refine_diff_density_rms 0.128 data_eu19e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[EuL]2*10H2O*4MeOH (!centrosymmetric dimer!) ' _chemical_formula_sum 'C32 H60 Eu N4 O13 P3' _chemical_formula_weight 953.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no.14) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2052(9) _cell_length_b 19.407(2) _cell_length_c 16.077(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.617(9) _cell_angle_gamma 90.00 _cell_volume 3856.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.819 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min --- _exptl_absorpt_correction_T_max --- _exptl_special_details ; crystal coated by thin paraphine film due to a loss of solvate molecules ; _diffrn_ambient_temperature 170(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 'CAD4 (Enraf-Nonius) ' _diffrn_measurement_method '.omega.-2.theta. ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min ' _diffrn_standards_decay_% '< 10 ' _diffrn_reflns_number 4959 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 21.99 _reflns_number_total 4724 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-program packet' _computing_cell_refinement 'CAD4-program packet' _computing_data_reduction 'JANA-98 (Petricek, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+11.9631P] 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 SHELXL _refine_ls_extinction_coef 0.00034(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4724 _refine_ls_number_parameters 646 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 8.284 _refine_ls_shift/su_mean 0.055 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.66842(2) 0.611644(14) 0.02195(2) 0.02930(17) Uani 1 d . . . P1 P 0.90088(14) 0.64471(9) 0.20081(13) 0.0419(5) Uani 1 d . . . P2 P 0.56978(15) 0.76749(9) 0.06589(16) 0.0531(6) Uani 1 d . . . P3 P 0.40392(12) 0.56352(8) -0.08167(12) 0.0317(4) Uani 1 d . . . O11 O 0.8135(3) 0.5932(2) 0.1541(3) 0.0394(11) Uani 1 d . . . O12 O 0.8892(4) 0.6834(3) 0.2769(4) 0.0573(14) Uani 1 d . . . O21 O 0.6389(3) 0.7037(2) 0.1048(3) 0.0465(12) Uani 1 d . . . O22 O 0.6207(4) 0.8356(2) 0.0998(5) 0.0735(19) Uani 1 d . . . O31 O 0.4786(3) 0.61247(18) -0.0150(3) 0.0326(10) Uani 1 d . . . O32 O 0.3704(3) 0.50018(19) -0.0436(3) 0.0320(10) Uani 1 d . . . N1 N 0.8495(4) 0.6790(3) 0.0238(4) 0.0367(13) Uani 1 d . . . N2 N 0.6252(4) 0.7260(3) -0.0746(4) 0.0427(15) Uani 1 d . . . N3 N 0.5624(4) 0.5858(3) -0.1504(4) 0.0329(12) Uani 1 d . . . N4 N 0.7868(4) 0.5389(2) -0.0509(3) 0.0291(11) Uani 1 d . . . C1 C 0.8241(6) 0.7362(4) -0.0414(7) 0.047(2) Uani 1 d . . . H011 H 0.822(5) 0.719(3) -0.093(4) 0.023(18) Uiso 1 d . . . H012 H 0.879(6) 0.770(4) -0.024(4) 0.042(18) Uiso 1 d . . . C2 C 0.7213(6) 0.7730(4) -0.0472(8) 0.054(2) Uani 1 d . . . H021 H 0.739(7) 0.795(4) 0.013(6) 0.07(3) Uiso 1 d . . . H022 H 0.713(4) 0.803(3) -0.084(4) 0.010(15) Uiso 1 d . . . C3 C 0.5914(6) 0.7108(4) -0.1699(6) 0.050(2) Uani 1 d . . . H031 H 0.652(6) 0.701(3) -0.186(4) 0.042(19) Uiso 1 d . . . H032 H 0.560(6) 0.749(4) -0.202(5) 0.05(2) Uiso 1 d . . . C4 C 0.5138(5) 0.6507(3) -0.1977(6) 0.0428(18) Uani 1 d . . . H041 H 0.445(6) 0.656(3) -0.180(4) 0.046(19) Uiso 1 d . . . H042 H 0.495(6) 0.644(4) -0.263(6) 0.07(3) Uiso 1 d . . . C5 C 0.6324(5) 0.5546(3) -0.1946(5) 0.0367(15) Uani 1 d . . . H051 H 0.679(4) 0.593(3) -0.210(3) 0.016(13) Uiso 1 d . . . H052 H 0.587(5) 0.528(3) -0.250(4) 0.033(16) Uiso 1 d . . . C6 C 0.7136(5) 0.5050(3) -0.1325(4) 0.0330(15) Uani 1 d . . . H061 H 0.676(4) 0.467(3) -0.113(3) 0.013(13) Uiso 1 d . . . H062 H 0.749(4) 0.481(3) -0.170(4) 0.020(14) Uiso 1 d . . . C7 C 0.8664(6) 0.5829(4) -0.0708(5) 0.0338(15) Uani 1 d . . . H071 H 0.828(5) 0.606(3) -0.113(4) 0.006(14) Uiso 1 d . . . H072 H 0.909(5) 0.558(3) -0.100(4) 0.035(17) Uiso 1 d . . . C8 C 0.9242(5) 0.6299(3) 0.0044(5) 0.0345(15) Uani 1 d . . . H081 H 0.972(5) 0.602(3) 0.069(4) 0.026(15) Uiso 1 d . . . H082 H 0.980(5) 0.656(3) -0.002(4) 0.022(14) Uiso 1 d . . . C10 C 0.9013(6) 0.7059(4) 0.1147(5) 0.0459(19) Uani 1 d . . . H101 H 0.856(6) 0.747(4) 0.125(5) 0.05(2) Uiso 1 d . . . H102 H 0.972(5) 0.720(3) 0.129(4) 0.032(16) Uiso 1 d . . . C11 C 1.0281(5) 0.5998(4) 0.2420(4) 0.0406(17) Uani 1 d . . . C12 C 1.0307(6) 0.5285(4) 0.2482(5) 0.0417(17) Uani 1 d . . . H12 H 0.972(5) 0.504(3) 0.229(4) 0.026(16) Uiso 1 d . . . C13 C 1.1254(7) 0.4937(5) 0.2904(5) 0.057(2) Uani 1 d . . . H13 H 1.127(5) 0.448(4) 0.293(4) 0.04(2) Uiso 1 d . . . C14 C 1.2214(7) 0.5304(6) 0.3265(5) 0.064(3) Uani 1 d . . . H14 H 1.273(8) 0.505(5) 0.356(6) 0.09(3) Uiso 1 d . . . C15 C 1.2220(6) 0.6003(6) 0.3186(6) 0.059(2) Uani 1 d . . . H15 H 1.287(8) 0.628(4) 0.346(6) 0.07(3) Uiso 1 d . . . C16 C 1.1263(6) 0.6354(5) 0.2772(5) 0.0489(19) Uani 1 d . . . H16 H 1.128(6) 0.682(4) 0.268(5) 0.06(2) Uiso 1 d . . . C20 C 0.5362(6) 0.7603(4) -0.0537(6) 0.047(2) Uani 1 d . . . H201 H 0.472(6) 0.729(4) -0.081(4) 0.044(19) Uiso 1 d . . . H202 H 0.525(6) 0.800(4) -0.075(5) 0.06(2) Uiso 1 d . . . C21 C 0.4425(5) 0.7622(4) 0.0845(6) 0.054(2) Uani 1 d . . . C22 C 0.3730(7) 0.8190(5) 0.0613(7) 0.068(3) Uani 1 d . . . H22 H 0.392(7) 0.855(4) 0.037(5) 0.06(3) Uiso 1 d . . . C23 C 0.2779(8) 0.8184(6) 0.0786(9) 0.093(4) Uani 1 d . . . H23 H 0.221(8) 0.856(5) 0.048(6) 0.09(3) Uiso 1 d . . . C24 C 0.2525(8) 0.7628(6) 0.1195(9) 0.086(3) Uani 1 d . . . H24 H 0.196(8) 0.760(5) 0.140(6) 0.09(3) Uiso 1 d . . . C25 C 0.3198(7) 0.7062(5) 0.1427(7) 0.069(3) Uani 1 d . . . H25 H 0.307(6) 0.667(4) 0.169(5) 0.05(2) Uiso 1 d . . . C26 C 0.4158(6) 0.7065(5) 0.1250(6) 0.057(2) Uani 1 d . . . H26 H 0.447(5) 0.666(4) 0.136(4) 0.035(18) Uiso 1 d . . . C30 C 0.4741(5) 0.5372(3) -0.1550(5) 0.0341(16) Uani 1 d . . . H301 H 0.499(4) 0.499(3) -0.140(3) 0.009(14) Uiso 1 d . . . H302 H 0.424(5) 0.530(3) -0.218(4) 0.028(16) Uiso 1 d . . . C31 C 0.2805(5) 0.6084(3) -0.1449(5) 0.0417(18) Uani 1 d . . . C32 C 0.2151(6) 0.5858(4) -0.2283(7) 0.057(2) Uani 1 d . . . H32 H 0.244(6) 0.557(4) -0.259(5) 0.04(2) Uiso 1 d . . . C33 C 0.1135(7) 0.6160(5) -0.2679(8) 0.075(3) Uani 1 d . . . H33 H 0.087(6) 0.596(4) -0.327(5) 0.05(2) Uiso 1 d . . . C34 C 0.0789(8) 0.6660(5) -0.2236(10) 0.078(4) Uani 1 d . . . H34 H 0.019(7) 0.683(4) -0.245(5) 0.05(2) Uiso 1 d . . . C35 C 0.1427(8) 0.6883(5) -0.1435(10) 0.072(3) Uani 1 d . . . H35 H 0.130(8) 0.719(5) -0.107(6) 0.07(3) Uiso 1 d . . . C36 C 0.2445(6) 0.6608(4) -0.1044(7) 0.050(2) Uani 1 d . . . H36 H 0.283(7) 0.670(4) -0.052(6) 0.06(3) Uiso 1 d . . . C4O C 0.8473(6) 0.4833(4) 0.0093(5) 0.0347(15) Uani 1 d . . . H4O1 H 0.800(5) 0.454(3) 0.025(4) 0.028(16) Uiso 1 d . . . H402 H 0.898(6) 0.501(4) 0.066(5) 0.05(2) Uiso 1 d . . . H403 H 0.883(6) 0.460(4) -0.018(4) 0.038(19) Uiso 1 d . . . O99 O 0.6540(9) 0.6164(4) 0.2503(9) 0.167(7) Uani 1.00(3) d . . . O96 O 0.8085(5) 0.6802(3) 0.7455(5) 0.081(3) Uani 1.000(18) d . . . O95 O 0.5616(12) 0.5530(4) 0.4839(8) 0.233(11) Uani 1.00(3) d . . . OW1 O 0.5326(8) 0.4084(5) -0.2951(7) 0.067(4) Uani 0.592(19) d P . . OW2 O 0.8579(12) 0.4964(8) 0.5023(10) 0.089(7) Uani 0.47(2) d P . . OM1 O -0.0032(11) 0.6036(5) 0.4636(6) 0.133(5) Uani 0.930(18) d P . . CM1 C -0.0895(10) 0.6064(5) 0.4121(9) 0.073(3) Uani 0.930(18) d P . . OM2 O 0.7365(11) 0.5179(7) 0.3812(10) 0.140(6) Uani 0.692(17) d P . . CM2 C 0.6396(12) 0.5261(7) 0.3875(9) 0.076(4) Uani 0.692(17) d P . . QN N 0.7060 0.6325 -0.0630 0.050 Uiso 0.00 d P . . QO O 0.6401 0.6023 0.0719 0.050 Uiso 0.00 d P . . 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 Eu 0.0189(2) 0.0161(2) 0.0520(3) -0.00623(13) 0.01135(16) -0.00085(11) P1 0.0258(9) 0.0403(11) 0.0607(12) -0.0220(9) 0.0165(8) -0.0071(8) P2 0.0296(10) 0.0229(9) 0.1053(17) -0.0188(10) 0.0218(10) 0.0005(8) P3 0.0183(8) 0.0168(8) 0.0562(11) -0.0010(7) 0.0084(8) 0.0012(6) O11 0.024(2) 0.033(2) 0.060(3) -0.010(2) 0.013(2) -0.0051(19) O12 0.038(3) 0.063(3) 0.077(4) -0.034(3) 0.028(3) -0.008(2) O21 0.026(2) 0.031(3) 0.077(3) -0.018(2) 0.011(2) 0.0000(19) O22 0.041(3) 0.027(3) 0.148(6) -0.038(3) 0.029(3) -0.005(2) O31 0.023(2) 0.016(2) 0.056(3) -0.0063(18) 0.012(2) 0.0010(16) O32 0.018(2) 0.018(2) 0.058(3) 0.0000(19) 0.0103(19) 0.0009(16) N1 0.023(3) 0.020(3) 0.065(4) -0.008(3) 0.014(3) -0.002(2) N2 0.026(3) 0.018(3) 0.082(5) 0.001(3) 0.016(3) 0.000(2) N3 0.024(3) 0.021(3) 0.052(3) 0.003(2) 0.011(2) 0.001(2) N4 0.022(3) 0.020(3) 0.044(3) 0.000(2) 0.010(2) 0.004(2) C1 0.032(4) 0.021(4) 0.091(7) 0.001(4) 0.024(4) -0.004(3) C2 0.034(4) 0.020(4) 0.110(8) 0.009(5) 0.027(5) -0.004(3) C3 0.038(4) 0.021(4) 0.093(7) 0.014(4) 0.025(4) 0.006(3) C4 0.029(4) 0.030(4) 0.068(5) 0.017(4) 0.014(4) 0.002(3) C5 0.031(4) 0.029(4) 0.049(4) 0.001(3) 0.013(3) -0.004(3) C6 0.026(3) 0.026(4) 0.046(4) -0.007(3) 0.012(3) -0.002(3) C7 0.027(4) 0.027(4) 0.046(4) 0.000(3) 0.011(4) 0.004(3) C8 0.016(3) 0.026(3) 0.063(5) -0.005(3) 0.016(3) -0.001(3) C10 0.029(4) 0.031(4) 0.079(5) -0.026(4) 0.020(4) -0.014(3) C11 0.027(4) 0.057(5) 0.039(4) -0.018(3) 0.014(3) -0.003(3) C12 0.031(4) 0.051(5) 0.040(4) 0.001(3) 0.009(3) -0.006(4) C13 0.053(6) 0.067(6) 0.048(5) 0.016(4) 0.015(4) 0.007(5) C14 0.038(5) 0.107(9) 0.045(5) 0.024(5) 0.012(4) 0.012(5) C15 0.027(5) 0.094(8) 0.053(5) -0.005(5) 0.010(4) -0.006(5) C16 0.031(4) 0.059(5) 0.055(5) -0.014(4) 0.012(4) -0.007(4) C20 0.033(4) 0.011(3) 0.097(6) 0.000(4) 0.022(4) 0.006(3) C21 0.029(4) 0.034(4) 0.096(6) -0.017(4) 0.019(4) 0.001(3) C22 0.038(5) 0.049(6) 0.115(8) -0.007(5) 0.023(5) 0.013(4) C23 0.053(6) 0.067(7) 0.170(11) -0.007(7) 0.051(7) 0.021(5) C24 0.044(6) 0.085(8) 0.140(10) -0.024(7) 0.045(6) 0.004(5) C25 0.045(5) 0.061(6) 0.107(8) -0.017(6) 0.033(5) -0.003(5) C26 0.035(4) 0.042(5) 0.093(6) -0.025(5) 0.022(4) -0.002(4) C30 0.029(4) 0.015(4) 0.053(5) 0.006(3) 0.007(3) 0.001(3) C31 0.020(4) 0.020(4) 0.079(5) 0.014(3) 0.010(4) 0.001(3) C32 0.023(4) 0.037(4) 0.097(7) 0.005(5) 0.004(4) -0.002(3) C33 0.027(5) 0.057(6) 0.109(9) 0.024(6) -0.015(5) -0.016(4) C34 0.029(5) 0.040(5) 0.165(12) 0.050(7) 0.033(7) 0.020(5) C35 0.042(6) 0.045(6) 0.133(10) 0.028(6) 0.035(7) 0.014(5) C36 0.036(5) 0.030(4) 0.089(7) 0.020(4) 0.026(5) 0.014(3) C4O 0.029(4) 0.027(4) 0.053(5) -0.001(3) 0.020(4) 0.007(3) O99 0.165(10) 0.107(8) 0.311(17) 0.086(8) 0.186(12) 0.059(6) O96 0.068(4) 0.068(4) 0.126(6) 0.048(4) 0.057(4) 0.022(3) O95 0.292(17) 0.065(6) 0.189(12) 0.034(6) -0.106(11) -0.063(8) OW1 0.062(7) 0.062(7) 0.077(7) -0.015(5) 0.025(5) -0.008(5) OW2 0.089(11) 0.108(13) 0.082(11) 0.007(9) 0.046(8) -0.006(9) OM1 0.172(11) 0.139(10) 0.073(6) -0.001(6) 0.025(7) -0.003(8) CM1 0.081(8) 0.060(7) 0.091(9) -0.002(6) 0.045(7) 0.009(5) OM2 0.125(11) 0.102(10) 0.188(15) -0.027(9) 0.048(10) -0.016(8) CM2 0.091(10) 0.081(10) 0.063(9) -0.017(7) 0.039(8) -0.010(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 Eu QO 1.0139(3) . ? Eu QN 1.6589(4) . ? Eu O32 2.284(4) 3_665 ? Eu O11 2.333(5) . ? Eu O21 2.341(4) . ? Eu O31 2.364(4) . ? Eu N2 2.652(5) . ? Eu N4 2.664(5) . ? Eu N3 2.675(5) . ? Eu N1 2.716(5) . ? Eu P3 3.4277(16) . ? Eu P1 3.4479(19) . ? P1 O12 1.489(5) . ? P1 O11 1.511(5) . ? P1 C11 1.799(7) . ? P1 C10 1.826(8) . ? P2 O22 1.495(5) . ? P2 O21 1.535(5) . ? P2 C21 1.811(7) . ? P2 C20 1.820(9) . ? P3 O32 1.508(4) . ? P3 O31 1.510(4) . ? P3 C30 1.811(7) . ? P3 C31 1.812(6) . ? O32 Eu 2.284(4) 3_665 ? N1 C10 1.474(9) . ? N1 C8 1.482(8) . ? N1 C1 1.481(10) . ? N2 C3 1.467(11) . ? N2 C20 1.489(9) . ? N2 C2 1.498(9) . ? N3 C30 1.480(8) . ? N3 C5 1.480(8) . ? N3 C4 1.494(8) . ? N4 C7 1.475(8) . ? N4 C6 1.482(8) . ? N4 C4O 1.483(8) . ? C1 C2 1.508(10) . ? C1 H011 0.88(6) . ? C1 H012 0.95(8) . ? C2 H021 1.01(8) . ? C2 H022 0.81(6) . ? C3 C4 1.512(10) . ? C3 H031 0.94(7) . ? C3 H032 0.92(8) . ? C4 H041 1.04(7) . ? C4 H042 1.00(8) . ? C5 C6 1.522(9) . ? C5 H051 1.05(6) . ? C5 H052 1.02(7) . ? C6 H061 1.00(5) . ? C6 H062 1.00(6) . ? C7 C8 1.491(10) . ? C7 H071 0.81(6) . ? C7 H072 0.98(7) . ? C8 H081 1.14(6) . ? C8 H082 0.94(6) . ? C10 H101 1.05(8) . ? C10 H102 0.92(7) . ? C11 C12 1.387(10) . ? C11 C16 1.401(10) . ? C12 C13 1.371(11) . ? C12 H12 0.87(6) . ? C13 C14 1.391(13) . ? C13 H13 0.88(7) . ? C14 C15 1.362(13) . ? C14 H14 0.83(10) . ? C15 C16 1.383(12) . ? C15 H15 0.98(9) . ? C16 H16 0.93(8) . ? C20 H201 1.02(7) . ? C20 H202 0.84(8) . ? C21 C26 1.370(12) . ? C21 C22 1.399(11) . ? C22 C23 1.378(13) . ? C22 H22 0.88(8) . ? C23 C24 1.365(16) . ? C23 H23 1.04(10) . ? C24 C25 1.380(14) . ? C24 H24 0.91(10) . ? C25 C26 1.394(11) . ? C25 H25 0.91(7) . ? C26 H26 0.88(7) . ? C30 H301 0.81(6) . ? C30 H302 1.00(6) . ? C31 C36 1.378(11) . ? C31 C32 1.386(12) . ? C32 C33 1.396(12) . ? C32 H32 0.92(7) . ? C33 C34 1.375(16) . ? C33 H33 0.97(7) . ? C34 C35 1.338(16) . ? C34 H34 0.82(8) . ? C35 C36 1.376(12) . ? C35 H35 0.88(9) . ? C36 H36 0.83(8) . ? C4O H4O1 0.94(7) . ? C4O H402 0.99(8) . ? C4O H403 0.88(7) . ? OM1 CM1 1.151(15) . ? OM2 CM2 1.329(18) . ? 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 QO Eu QN 174.70(3) . . ? QO Eu O32 62.91(11) . 3_665 ? QN Eu O32 120.37(11) . 3_665 ? QO Eu O11 70.44(11) . . ? QN Eu O11 113.52(11) . . ? O32 Eu O11 82.67(15) 3_665 . ? QO Eu O21 60.28(12) . . ? QN Eu O21 116.11(12) . . ? O32 Eu O21 123.14(16) 3_665 . ? O11 Eu O21 81.18(15) . . ? QO Eu O31 63.00(11) . . ? QN Eu O31 112.94(11) . . ? O32 Eu O31 76.68(13) 3_665 . ? O11 Eu O31 133.45(15) . . ? O21 Eu O31 76.31(14) . . ? QO Eu N2 123.36(13) . . ? QN Eu N2 51.60(13) . . ? O32 Eu N2 150.48(16) 3_665 . ? O11 Eu N2 126.83(16) . . ? O21 Eu N2 69.55(19) . . ? O31 Eu N2 81.78(15) . . ? QO Eu N4 133.65(11) . . ? QN Eu N4 51.36(10) . . ? O32 Eu N4 76.20(14) 3_665 . ? O11 Eu N4 84.17(15) . . ? O21 Eu N4 153.56(15) . . ? O31 Eu N4 128.88(14) . . ? N2 Eu N4 102.96(16) . . ? QO Eu N3 125.57(11) . . ? QN Eu N3 52.61(10) . . ? O32 Eu N3 85.16(15) 3_665 . ? O11 Eu N3 151.25(15) . . ? O21 Eu N3 126.95(16) . . ? O31 Eu N3 67.61(15) . . ? N2 Eu N3 67.95(17) . . ? N4 Eu N3 67.63(15) . . ? QO Eu N1 130.23(12) . . ? QN Eu N1 51.25(12) . . ? O32 Eu N1 134.40(14) 3_665 . ? O11 Eu N1 68.07(16) . . ? O21 Eu N1 87.07(15) . . ? O31 Eu N1 148.31(14) . . ? N2 Eu N1 67.08(16) . . ? N4 Eu N1 67.01(15) . . ? N3 Eu N1 103.86(16) . . ? QO Eu P3 74.90(3) . . ? QN Eu P3 102.44(3) . . ? O32 Eu P3 64.54(10) 3_665 . ? O11 Eu P3 140.37(11) . . ? O21 Eu P3 97.99(11) . . ? O31 Eu P3 21.70(10) . . ? N2 Eu P3 88.35(12) . . ? N4 Eu P3 107.28(11) . . ? N3 Eu P3 51.18(11) . . ? N1 Eu P3 151.50(12) . . ? QO Eu P1 80.86(4) . . ? QN Eu P1 101.80(3) . . ? O32 Eu P1 103.39(11) 3_665 . ? O11 Eu P1 20.73(11) . . ? O21 Eu P1 70.20(11) . . ? O31 Eu P1 139.65(11) . . ? N2 Eu P1 106.10(12) . . ? N4 Eu P1 88.71(11) . . ? N3 Eu P1 152.43(11) . . ? N1 Eu P1 51.66(13) . . ? P3 Eu P1 155.74(4) . . ? O12 P1 O11 117.4(3) . . ? O12 P1 C11 107.2(3) . . ? O11 P1 C11 108.3(3) . . ? O12 P1 C10 108.9(3) . . ? O11 P1 C10 105.0(3) . . ? C11 P1 C10 110.0(3) . . ? O12 P1 Eu 117.4(2) . . ? O11 P1 Eu 33.12(19) . . ? C11 P1 Eu 131.2(2) . . ? C10 P1 Eu 74.2(2) . . ? O22 P2 O21 116.0(3) . . ? O22 P2 C21 108.4(3) . . ? O21 P2 C21 109.9(3) . . ? O22 P2 C20 111.3(4) . . ? O21 P2 C20 104.9(3) . . ? C21 P2 C20 106.0(4) . . ? O22 P2 Eu 133.8(2) . . ? O21 P2 Eu 33.50(19) . . ? C21 P2 Eu 114.9(2) . . ? C20 P2 Eu 71.7(2) . . ? O32 P3 O31 115.8(3) . . ? O32 P3 C30 109.0(3) . . ? O31 P3 C30 106.5(3) . . ? O32 P3 C31 106.6(3) . . ? O31 P3 C31 109.2(3) . . ? C30 P3 C31 109.7(4) . . ? O32 P3 Eu 114.79(17) . . ? O31 P3 Eu 35.38(15) . . ? C30 P3 Eu 74.1(2) . . ? C31 P3 Eu 134.7(2) . . ? P1 O11 Eu 126.2(3) . . ? P2 O21 Eu 125.3(3) . . ? P3 O31 Eu 122.9(2) . . ? P3 O32 Eu 161.8(3) . 3_665 ? C10 N1 C8 109.0(5) . . ? C10 N1 C1 110.3(6) . . ? C8 N1 C1 109.6(6) . . ? C10 N1 Eu 106.3(4) . . ? C8 N1 Eu 109.7(4) . . ? C1 N1 Eu 112.0(4) . . ? C3 N2 C20 110.6(6) . . ? C3 N2 C2 110.2(7) . . ? C20 N2 C2 108.3(5) . . ? C3 N2 Eu 111.5(4) . . ? C20 N2 Eu 105.5(4) . . ? C2 N2 Eu 110.6(5) . . ? C30 N3 C5 109.2(5) . . ? C30 N3 C4 108.8(5) . . ? C5 N3 C4 109.2(5) . . ? C30 N3 Eu 106.7(4) . . ? C5 N3 Eu 112.7(4) . . ? C4 N3 Eu 110.1(4) . . ? C7 N4 C6 111.0(5) . . ? C7 N4 C4O 107.6(5) . . ? C6 N4 C4O 106.7(5) . . ? C7 N4 Eu 111.2(4) . . ? C6 N4 Eu 108.9(3) . . ? C4O N4 Eu 111.3(4) . . ? N1 C1 C2 111.9(7) . . ? N1 C1 H011 107(4) . . ? C2 C1 H011 113(4) . . ? N1 C1 H012 111(4) . . ? C2 C1 H012 105(4) . . ? H011 C1 H012 108(6) . . ? N2 C2 C1 112.3(6) . . ? N2 C2 H021 115(5) . . ? C1 C2 H021 104(5) . . ? N2 C2 H022 109(4) . . ? C1 C2 H022 106(4) . . ? H021 C2 H022 110(6) . . ? N2 C3 C4 112.9(6) . . ? N2 C3 H031 111(4) . . ? C4 C3 H031 108(4) . . ? N2 C3 H032 110(4) . . ? C4 C3 H032 110(4) . . ? H031 C3 H032 105(6) . . ? N3 C4 C3 112.0(6) . . ? N3 C4 H041 102(4) . . ? C3 C4 H041 114(4) . . ? N3 C4 H042 110(5) . . ? C3 C4 H042 108(5) . . ? H041 C4 H042 112(6) . . ? N3 C5 C6 111.0(5) . . ? N3 C5 H051 110(3) . . ? C6 C5 H051 105(3) . . ? N3 C5 H052 110(3) . . ? C6 C5 H052 109(3) . . ? H051 C5 H052 111(4) . . ? N4 C6 C5 112.9(5) . . ? N4 C6 H061 107(3) . . ? C5 C6 H061 111(3) . . ? N4 C6 H062 116(3) . . ? C5 C6 H062 105(3) . . ? H061 C6 H062 105(4) . . ? N4 C7 C8 112.2(6) . . ? N4 C7 H071 102(4) . . ? C8 C7 H071 109(4) . . ? N4 C7 H072 114(4) . . ? C8 C7 H072 118(4) . . ? H071 C7 H072 99(5) . . ? N1 C8 C7 112.1(5) . . ? N1 C8 H081 108(3) . . ? C7 C8 H081 114(3) . . ? N1 C8 H082 107(3) . . ? C7 C8 H082 116(3) . . ? H081 C8 H082 99(4) . . ? N1 C10 P1 113.4(4) . . ? N1 C10 H101 110(4) . . ? P1 C10 H101 103(4) . . ? N1 C10 H102 115(4) . . ? P1 C10 H102 106(4) . . ? H101 C10 H102 109(5) . . ? C12 C11 C16 117.8(7) . . ? C12 C11 P1 120.5(5) . . ? C16 C11 P1 121.4(6) . . ? C13 C12 C11 121.5(8) . . ? C13 C12 H12 117(4) . . ? C11 C12 H12 122(4) . . ? C12 C13 C14 119.5(9) . . ? C12 C13 H13 121(5) . . ? C14 C13 H13 119(5) . . ? C15 C14 C13 120.3(9) . . ? C15 C14 H14 127(7) . . ? C13 C14 H14 112(7) . . ? C14 C15 C16 120.1(8) . . ? C14 C15 H15 123(5) . . ? C16 C15 H15 117(5) . . ? C15 C16 C11 120.7(9) . . ? C15 C16 H16 119(5) . . ? C11 C16 H16 120(5) . . ? N2 C20 P2 110.8(5) . . ? N2 C20 H201 104(4) . . ? P2 C20 H201 111(4) . . ? N2 C20 H202 111(5) . . ? P2 C20 H202 108(5) . . ? H201 C20 H202 113(7) . . ? C26 C21 C22 119.6(8) . . ? C26 C21 P2 122.2(6) . . ? C22 C21 P2 118.1(7) . . ? C23 C22 C21 119.9(10) . . ? C23 C22 H22 121(6) . . ? C21 C22 H22 119(6) . . ? C24 C23 C22 120.0(10) . . ? C24 C23 H23 121(5) . . ? C22 C23 H23 117(5) . . ? C23 C24 C25 121.0(9) . . ? C23 C24 H24 126(6) . . ? C25 C24 H24 113(6) . . ? C24 C25 C26 119.2(10) . . ? C24 C25 H25 125(5) . . ? C26 C25 H25 116(5) . . ? C21 C26 C25 120.4(8) . . ? C21 C26 H26 129(4) . . ? C25 C26 H26 110(4) . . ? N3 C30 P3 111.2(4) . . ? N3 C30 H301 109(4) . . ? P3 C30 H301 109(4) . . ? N3 C30 H302 112(3) . . ? P3 C30 H302 113(3) . . ? H301 C30 H302 103(5) . . ? C36 C31 C32 119.3(7) . . ? C36 C31 P3 118.8(6) . . ? C32 C31 P3 121.4(6) . . ? C31 C32 C33 118.7(10) . . ? C31 C32 H32 118(5) . . ? C33 C32 H32 122(5) . . ? C34 C33 C32 120.1(11) . . ? C34 C33 H33 136(5) . . ? C32 C33 H33 104(5) . . ? C35 C34 C33 121.1(9) . . ? C35 C34 H34 118(5) . . ? C33 C34 H34 121(5) . . ? C34 C35 C36 119.8(11) . . ? C34 C35 H35 130(6) . . ? C36 C35 H35 110(7) . . ? C35 C36 C31 121.0(11) . . ? C35 C36 H36 122(6) . . ? C31 C36 H36 117(6) . . ? N4 C4O H4O1 111(4) . . ? N4 C4O H402 112(4) . . ? H4O1 C4O H402 105(5) . . ? N4 C4O H403 108(4) . . ? H4O1 C4O H403 110(6) . . ? H402 C4O H403 110(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag QO Eu P1 O12 -41.1(3) . . . . ? QN Eu P1 O12 134.3(3) . . . . ? O32 Eu P1 O12 -100.2(3) 3_665 . . . ? O11 Eu P1 O12 -98.9(4) . . . . ? O21 Eu P1 O12 20.5(3) . . . . ? O31 Eu P1 O12 -15.2(3) . . . . ? N2 Eu P1 O12 81.2(3) . . . . ? N4 Eu P1 O12 -175.7(3) . . . . ? N3 Eu P1 O12 154.2(3) . . . . ? N1 Eu P1 O12 123.0(3) . . . . ? P3 Eu P1 O12 -43.4(3) . . . . ? QO Eu P1 O11 57.8(3) . . . . ? QN Eu P1 O11 -126.8(3) . . . . ? O32 Eu P1 O11 -1.4(3) 3_665 . . . ? O21 Eu P1 O11 119.4(3) . . . . ? O31 Eu P1 O11 83.7(3) . . . . ? N2 Eu P1 O11 -180.0(3) . . . . ? N4 Eu P1 O11 -76.8(3) . . . . ? N3 Eu P1 O11 -106.9(4) . . . . ? N1 Eu P1 O11 -138.1(3) . . . . ? P3 Eu P1 O11 55.5(3) . . . . ? QO Eu P1 C11 112.4(3) . . . . ? QN Eu P1 C11 -72.3(3) . . . . ? O32 Eu P1 C11 53.2(3) 3_665 . . . ? O11 Eu P1 C11 54.6(4) . . . . ? O21 Eu P1 C11 174.0(3) . . . . ? O31 Eu P1 C11 138.3(3) . . . . ? N2 Eu P1 C11 -125.4(3) . . . . ? N4 Eu P1 C11 -22.3(3) . . . . ? N3 Eu P1 C11 -52.3(4) . . . . ? N1 Eu P1 C11 -83.6(3) . . . . ? P3 Eu P1 C11 110.1(3) . . . . ? QO Eu P1 C10 -144.5(2) . . . . ? QN Eu P1 C10 30.8(2) . . . . ? O32 Eu P1 C10 156.3(3) 3_665 . . . ? O11 Eu P1 C10 157.6(4) . . . . ? O21 Eu P1 C10 -83.0(3) . . . . ? O31 Eu P1 C10 -118.6(3) . . . . ? N2 Eu P1 C10 -22.3(3) . . . . ? N4 Eu P1 C10 80.8(3) . . . . ? N3 Eu P1 C10 50.7(3) . . . . ? N1 Eu P1 C10 19.5(3) . . . . ? P3 Eu P1 C10 -146.9(2) . . . . ? QO Eu P2 O22 116.0(4) . . . . ? QN Eu P2 O22 -66.7(4) . . . . ? O32 Eu P2 O22 140.7(4) 3_665 . . . ? O11 Eu P2 O22 50.4(4) . . . . ? O21 Eu P2 O22 69.4(5) . . . . ? O31 Eu P2 O22 -177.0(4) . . . . ? N2 Eu P2 O22 -78.4(4) . . . . ? N4 Eu P2 O22 -48.0(5) . . . . ? N3 Eu P2 O22 -120.8(4) . . . . ? N1 Eu P2 O22 -16.9(4) . . . . ? P3 Eu P2 O22 -168.8(4) . . . . ? P1 Eu P2 O22 34.8(4) . . . . ? QO Eu P2 O21 46.6(3) . . . . ? QN Eu P2 O21 -136.2(3) . . . . ? O32 Eu P2 O21 71.3(3) 3_665 . . . ? O11 Eu P2 O21 -19.1(3) . . . . ? O31 Eu P2 O21 113.6(3) . . . . ? N2 Eu P2 O21 -147.8(4) . . . . ? N4 Eu P2 O21 -117.4(4) . . . . ? N3 Eu P2 O21 169.8(3) . . . . ? N1 Eu P2 O21 -86.3(3) . . . . ? P3 Eu P2 O21 121.8(3) . . . . ? P1 Eu P2 O21 -34.6(3) . . . . ? QO Eu P2 C21 -42.1(3) . . . . ? QN Eu P2 C21 135.2(3) . . . . ? O32 Eu P2 C21 -17.4(4) 3_665 . . . ? O11 Eu P2 C21 -107.8(3) . . . . ? O21 Eu P2 C21 -88.7(4) . . . . ? O31 Eu P2 C21 24.9(3) . . . . ? N2 Eu P2 C21 123.5(4) . . . . ? N4 Eu P2 C21 153.9(4) . . . . ? N3 Eu P2 C21 81.1(3) . . . . ? N1 Eu P2 C21 -175.0(3) . . . . ? P3 Eu P2 C21 33.1(3) . . . . ? P1 Eu P2 C21 -123.3(3) . . . . ? QO Eu P2 C20 -141.6(3) . . . . ? QN Eu P2 C20 35.6(2) . . . . ? O32 Eu P2 C20 -116.9(3) 3_665 . . . ? O11 Eu P2 C20 152.7(3) . . . . ? O21 Eu P2 C20 171.8(4) . . . . ? O31 Eu P2 C20 -74.6(3) . . . . ? N2 Eu P2 C20 24.0(3) . . . . ? N4 Eu P2 C20 54.4(3) . . . . ? N3 Eu P2 C20 -18.5(3) . . . . ? N1 Eu P2 C20 85.5(3) . . . . ? P3 Eu P2 C20 -66.5(3) . . . . ? P1 Eu P2 C20 137.1(3) . . . . ? QO Eu P3 O32 -46.72(19) . . . . ? QN Eu P3 O32 138.00(19) . . . . ? O32 Eu P3 O32 20.1(3) 3_665 . . . ? O11 Eu P3 O32 -17.1(3) . . . . ? O21 Eu P3 O32 -102.9(2) . . . . ? O31 Eu P3 O32 -100.3(3) . . . . ? N2 Eu P3 O32 -172.0(2) . . . . ? N4 Eu P3 O32 84.9(2) . . . . ? N3 Eu P3 O32 125.3(2) . . . . ? N1 Eu P3 O32 158.4(3) . . . . ? P1 Eu P3 O32 -44.3(2) . . . . ? QO Eu P3 O31 53.6(3) . . . . ? QN Eu P3 O31 -121.7(3) . . . . ? O32 Eu P3 O31 120.4(3) 3_665 . . . ? O11 Eu P3 O31 83.2(3) . . . . ? O21 Eu P3 O31 -2.6(3) . . . . ? N2 Eu P3 O31 -71.7(3) . . . . ? N4 Eu P3 O31 -174.7(3) . . . . ? N3 Eu P3 O31 -134.4(3) . . . . ? N1 Eu P3 O31 -101.2(4) . . . . ? P1 Eu P3 O31 56.0(3) . . . . ? QO Eu P3 C30 -150.6(2) . . . . ? QN Eu P3 C30 34.1(2) . . . . ? O32 Eu P3 C30 -83.8(3) 3_665 . . . ? O11 Eu P3 C30 -121.0(3) . . . . ? O21 Eu P3 C30 153.2(3) . . . . ? O31 Eu P3 C30 155.8(4) . . . . ? N2 Eu P3 C30 84.1(3) . . . . ? N4 Eu P3 C30 -19.0(3) . . . . ? N3 Eu P3 C30 21.4(3) . . . . ? N1 Eu P3 C30 54.5(3) . . . . ? P1 Eu P3 C30 -148.2(2) . . . . ? QO Eu P3 C31 107.3(4) . . . . ? QN Eu P3 C31 -68.0(4) . . . . ? O32 Eu P3 C31 174.1(4) 3_665 . . . ? O11 Eu P3 C31 136.9(4) . . . . ? O21 Eu P3 C31 51.1(4) . . . . ? O31 Eu P3 C31 53.7(5) . . . . ? N2 Eu P3 C31 -18.0(4) . . . . ? N4 Eu P3 C31 -121.1(4) . . . . ? N3 Eu P3 C31 -80.7(4) . . . . ? N1 Eu P3 C31 -47.6(4) . . . . ? P1 Eu P3 C31 109.7(4) . . . . ? O12 P1 O11 Eu 98.8(4) . . . . ? C11 P1 O11 Eu -139.8(3) . . . . ? C10 P1 O11 Eu -22.3(4) . . . . ? QO Eu O11 P1 -117.5(3) . . . . ? QN Eu O11 P1 58.7(3) . . . . ? O32 Eu O11 P1 178.7(3) 3_665 . . . ? O21 Eu O11 P1 -56.0(3) . . . . ? O31 Eu O11 P1 -117.6(3) . . . . ? N2 Eu O11 P1 0.0(4) . . . . ? N4 Eu O11 P1 101.9(3) . . . . ? N3 Eu O11 P1 113.0(4) . . . . ? N1 Eu O11 P1 34.3(3) . . . . ? P3 Eu O11 P1 -147.9(2) . . . . ? O22 P2 O21 Eu -131.3(4) . . . . ? C21 P2 O21 Eu 105.4(4) . . . . ? C20 P2 O21 Eu -8.1(4) . . . . ? QO Eu O21 P2 -126.5(3) . . . . ? QN Eu O21 P2 49.1(3) . . . . ? O32 Eu O21 P2 -123.7(3) 3_665 . . . ? O11 Eu O21 P2 161.1(3) . . . . ? O31 Eu O21 P2 -60.0(3) . . . . ? N2 Eu O21 P2 26.2(3) . . . . ? N4 Eu O21 P2 103.9(4) . . . . ? N3 Eu O21 P2 -12.3(4) . . . . ? N1 Eu O21 P2 92.8(3) . . . . ? P3 Eu O21 P2 -59.0(3) . . . . ? P1 Eu O21 P2 142.9(3) . . . . ? O32 P3 O31 Eu 97.0(3) . . . . ? C30 P3 O31 Eu -24.3(4) . . . . ? C31 P3 O31 Eu -142.6(3) . . . . ? QO Eu O31 P3 -119.3(3) . . . . ? QN Eu O31 P3 64.5(3) . . . . ? O32 Eu O31 P3 -53.2(3) 3_665 . . . ? O11 Eu O31 P3 -119.3(3) . . . . ? O21 Eu O31 P3 177.3(3) . . . . ? N2 Eu O31 P3 106.5(3) . . . . ? N4 Eu O31 P3 6.5(4) . . . . ? N3 Eu O31 P3 37.0(3) . . . . ? N1 Eu O31 P3 117.0(3) . . . . ? P1 Eu O31 P3 -148.3(2) . . . . ? O31 P3 O32 Eu -135.6(7) . . . 3_665 ? C30 P3 O32 Eu -15.6(9) . . . 3_665 ? C31 P3 O32 Eu 102.6(8) . . . 3_665 ? Eu P3 O32 Eu -96.4(8) . . . 3_665 ? QO Eu N1 C10 -3.7(4) . . . . ? QN Eu N1 C10 169.7(4) . . . . ? O32 Eu N1 C10 -93.3(4) 3_665 . . . ? O11 Eu N1 C10 -39.2(4) . . . . ? O21 Eu N1 C10 42.4(4) . . . . ? O31 Eu N1 C10 100.1(5) . . . . ? N2 Eu N1 C10 111.4(4) . . . . ? N4 Eu N1 C10 -132.2(4) . . . . ? N3 Eu N1 C10 169.8(4) . . . . ? P3 Eu N1 C10 143.8(3) . . . . ? P1 Eu N1 C10 -24.5(3) . . . . ? QO Eu N1 C8 114.0(4) . . . . ? QN Eu N1 C8 -72.6(4) . . . . ? O32 Eu N1 C8 24.4(5) 3_665 . . . ? O11 Eu N1 C8 78.4(4) . . . . ? O21 Eu N1 C8 160.1(4) . . . . ? O31 Eu N1 C8 -142.2(4) . . . . ? N2 Eu N1 C8 -130.9(5) . . . . ? N4 Eu N1 C8 -14.5(4) . . . . ? N3 Eu N1 C8 -72.5(4) . . . . ? P3 Eu N1 C8 -98.5(4) . . . . ? P1 Eu N1 C8 93.2(4) . . . . ? QO Eu N1 C1 -124.2(5) . . . . ? QN Eu N1 C1 49.2(5) . . . . ? O32 Eu N1 C1 146.2(5) 3_665 . . . ? O11 Eu N1 C1 -159.7(5) . . . . ? O21 Eu N1 C1 -78.1(5) . . . . ? O31 Eu N1 C1 -20.4(6) . . . . ? N2 Eu N1 C1 -9.1(5) . . . . ? N4 Eu N1 C1 107.3(5) . . . . ? N3 Eu N1 C1 49.3(5) . . . . ? P3 Eu N1 C1 23.3(6) . . . . ? P1 Eu N1 C1 -145.0(5) . . . . ? QO Eu N2 C3 -132.7(4) . . . . ? QN Eu N2 C3 45.3(4) . . . . ? O32 Eu N2 C3 -39.5(6) 3_665 . . . ? O11 Eu N2 C3 137.7(4) . . . . ? O21 Eu N2 C3 -161.2(5) . . . . ? O31 Eu N2 C3 -82.9(4) . . . . ? N4 Eu N2 C3 45.3(4) . . . . ? N3 Eu N2 C3 -13.8(4) . . . . ? N1 Eu N2 C3 103.1(5) . . . . ? P3 Eu N2 C3 -62.1(4) . . . . ? P1 Eu N2 C3 137.7(4) . . . . ? QO Eu N2 C20 -12.7(5) . . . . ? QN Eu N2 C20 165.3(5) . . . . ? O32 Eu N2 C20 80.5(6) 3_665 . . . ? O11 Eu N2 C20 -102.2(4) . . . . ? O21 Eu N2 C20 -41.2(4) . . . . ? O31 Eu N2 C20 37.2(4) . . . . ? N4 Eu N2 C20 165.3(4) . . . . ? N3 Eu N2 C20 106.3(4) . . . . ? N1 Eu N2 C20 -136.8(5) . . . . ? P3 Eu N2 C20 58.0(4) . . . . ? P1 Eu N2 C20 -102.2(4) . . . . ? QO Eu N2 C2 104.2(5) . . . . ? QN Eu N2 C2 -77.8(5) . . . . ? O32 Eu N2 C2 -162.6(5) 3_665 . . . ? O11 Eu N2 C2 14.6(6) . . . . ? O21 Eu N2 C2 75.7(5) . . . . ? O31 Eu N2 C2 154.1(5) . . . . ? N4 Eu N2 C2 -77.8(5) . . . . ? N3 Eu N2 C2 -136.8(6) . . . . ? N1 Eu N2 C2 -19.9(5) . . . . ? P3 Eu N2 C2 174.9(5) . . . . ? P1 Eu N2 C2 14.7(5) . . . . ? QO Eu N3 C30 -17.2(4) . . . . ? QN Eu N3 C30 169.0(4) . . . . ? O32 Eu N3 C30 34.3(4) 3_665 . . . ? O11 Eu N3 C30 99.4(5) . . . . ? O21 Eu N3 C30 -94.2(4) . . . . ? O31 Eu N3 C30 -43.3(4) . . . . ? N2 Eu N3 C30 -133.3(4) . . . . ? N4 Eu N3 C30 111.4(4) . . . . ? N1 Eu N3 C30 168.9(4) . . . . ? P3 Eu N3 C30 -26.6(3) . . . . ? P1 Eu N3 C30 144.2(3) . . . . ? QO Eu N3 C5 -137.0(3) . . . . ? QN Eu N3 C5 49.1(3) . . . . ? O32 Eu N3 C5 -85.6(4) 3_665 . . . ? O11 Eu N3 C5 -20.4(6) . . . . ? O21 Eu N3 C5 145.9(4) . . . . ? O31 Eu N3 C5 -163.1(4) . . . . ? N2 Eu N3 C5 106.9(4) . . . . ? N4 Eu N3 C5 -8.5(4) . . . . ? N1 Eu N3 C5 49.1(4) . . . . ? P3 Eu N3 C5 -146.5(4) . . . . ? P1 Eu N3 C5 24.3(5) . . . . ? QO Eu N3 C4 100.7(4) . . . . ? QN Eu N3 C4 -73.1(4) . . . . ? O32 Eu N3 C4 152.2(4) 3_665 . . . ? O11 Eu N3 C4 -142.6(4) . . . . ? O21 Eu N3 C4 23.7(4) . . . . ? O31 Eu N3 C4 74.7(4) . . . . ? N2 Eu N3 C4 -15.3(4) . . . . ? N4 Eu N3 C4 -130.7(4) . . . . ? N1 Eu N3 C4 -73.1(4) . . . . ? P3 Eu N3 C4 91.3(4) . . . . ? P1 Eu N3 C4 -97.9(4) . . . . ? QO Eu N4 C7 -139.8(4) . . . . ? QN Eu N4 C7 42.5(4) . . . . ? O32 Eu N4 C7 -167.9(4) 3_665 . . . ? O11 Eu N4 C7 -84.0(4) . . . . ? O21 Eu N4 C7 -27.5(6) . . . . ? O31 Eu N4 C7 132.3(4) . . . . ? N2 Eu N4 C7 42.5(4) . . . . ? N3 Eu N4 C7 101.7(4) . . . . ? N1 Eu N4 C7 -15.4(4) . . . . ? P3 Eu N4 C7 134.8(4) . . . . ? P1 Eu N4 C7 -63.7(4) . . . . ? QO Eu N4 C6 97.6(4) . . . . ? QN Eu N4 C6 -80.1(4) . . . . ? O32 Eu N4 C6 69.5(4) 3_665 . . . ? O11 Eu N4 C6 153.3(4) . . . . ? O21 Eu N4 C6 -150.1(4) . . . . ? O31 Eu N4 C6 9.7(4) . . . . ? N2 Eu N4 C6 -80.2(4) . . . . ? N3 Eu N4 C6 -20.9(4) . . . . ? N1 Eu N4 C6 -138.0(4) . . . . ? P3 Eu N4 C6 12.2(4) . . . . ? P1 Eu N4 C6 173.6(4) . . . . ? QO Eu N4 C4O -19.8(5) . . . . ? QN Eu N4 C4O 162.5(4) . . . . ? O32 Eu N4 C4O -47.9(4) 3_665 . . . ? O11 Eu N4 C4O 35.9(4) . . . . ? O21 Eu N4 C4O 92.5(5) . . . . ? O31 Eu N4 C4O -107.7(4) . . . . ? N2 Eu N4 C4O 162.4(4) . . . . ? N3 Eu N4 C4O -138.3(4) . . . . ? N1 Eu N4 C4O 104.6(4) . . . . ? P3 Eu N4 C4O -105.2(4) . . . . ? P1 Eu N4 C4O 56.2(4) . . . . ? C10 N1 C1 C2 -80.6(8) . . . . ? C8 N1 C1 C2 159.5(7) . . . . ? Eu N1 C1 C2 37.6(8) . . . . ? C3 N2 C2 C1 -75.0(10) . . . . ? C20 N2 C2 C1 164.0(8) . . . . ? Eu N2 C2 C1 48.9(10) . . . . ? N1 C1 C2 N2 -59.7(11) . . . . ? C20 N2 C3 C4 -74.4(7) . . . . ? C2 N2 C3 C4 165.9(6) . . . . ? Eu N2 C3 C4 42.6(7) . . . . ? C30 N3 C4 C3 160.0(6) . . . . ? C5 N3 C4 C3 -80.9(8) . . . . ? Eu N3 C4 C3 43.4(7) . . . . ? N2 C3 C4 N3 -60.0(8) . . . . ? C30 N3 C5 C6 -81.7(6) . . . . ? C4 N3 C5 C6 159.5(5) . . . . ? Eu N3 C5 C6 36.8(6) . . . . ? C7 N4 C6 C5 -72.7(6) . . . . ? C4O N4 C6 C5 170.4(5) . . . . ? Eu N4 C6 C5 50.1(6) . . . . ? N3 C5 C6 N4 -60.5(7) . . . . ? C6 N4 C7 C8 166.9(5) . . . . ? C4O N4 C7 C8 -76.8(7) . . . . ? Eu N4 C7 C8 45.4(6) . . . . ? C10 N1 C8 C7 160.1(6) . . . . ? C1 N1 C8 C7 -79.1(7) . . . . ? Eu N1 C8 C7 44.1(6) . . . . ? N4 C7 C8 N1 -62.7(8) . . . . ? C8 N1 C10 P1 -76.1(6) . . . . ? C1 N1 C10 P1 163.6(5) . . . . ? Eu N1 C10 P1 42.0(5) . . . . ? O12 P1 C10 N1 -145.8(5) . . . . ? O11 P1 C10 N1 -19.3(5) . . . . ? C11 P1 C10 N1 97.0(5) . . . . ? Eu P1 C10 N1 -31.7(4) . . . . ? O12 P1 C11 C12 111.5(6) . . . . ? O11 P1 C11 C12 -16.0(6) . . . . ? C10 P1 C11 C12 -130.2(6) . . . . ? Eu P1 C11 C12 -43.9(7) . . . . ? O12 P1 C11 C16 -61.8(7) . . . . ? O11 P1 C11 C16 170.7(6) . . . . ? C10 P1 C11 C16 56.5(6) . . . . ? Eu P1 C11 C16 142.8(5) . . . . ? C16 C11 C12 C13 2.6(10) . . . . ? P1 C11 C12 C13 -170.9(6) . . . . ? C11 C12 C13 C14 -1.2(11) . . . . ? C12 C13 C14 C15 -1.3(12) . . . . ? C13 C14 C15 C16 2.3(13) . . . . ? C14 C15 C16 C11 -0.9(12) . . . . ? C12 C11 C16 C15 -1.5(11) . . . . ? P1 C11 C16 C15 172.0(6) . . . . ? C3 N2 C20 P2 171.3(4) . . . . ? C2 N2 C20 P2 -67.8(7) . . . . ? Eu N2 C20 P2 50.7(5) . . . . ? O22 P2 C20 N2 93.9(5) . . . . ? O21 P2 C20 N2 -32.3(5) . . . . ? C21 P2 C20 N2 -148.5(5) . . . . ? Eu P2 C20 N2 -37.0(4) . . . . ? O22 P2 C21 C26 -129.8(7) . . . . ? O21 P2 C21 C26 -2.1(8) . . . . ? C20 P2 C21 C26 110.7(7) . . . . ? Eu P2 C21 C26 33.8(8) . . . . ? O22 P2 C21 C22 46.2(8) . . . . ? O21 P2 C21 C22 173.8(7) . . . . ? C20 P2 C21 C22 -73.3(8) . . . . ? Eu P2 C21 C22 -150.2(6) . . . . ? C26 C21 C22 C23 -0.6(14) . . . . ? P2 C21 C22 C23 -176.6(8) . . . . ? C21 C22 C23 C24 1.0(17) . . . . ? C22 C23 C24 C25 -1.2(19) . . . . ? C23 C24 C25 C26 0.9(17) . . . . ? C22 C21 C26 C25 0.3(13) . . . . ? P2 C21 C26 C25 176.2(7) . . . . ? C24 C25 C26 C21 -0.4(14) . . . . ? C5 N3 C30 P3 167.3(4) . . . . ? C4 N3 C30 P3 -73.6(6) . . . . ? Eu N3 C30 P3 45.2(5) . . . . ? O32 P3 C30 N3 -144.7(4) . . . . ? O31 P3 C30 N3 -19.1(5) . . . . ? C31 P3 C30 N3 98.9(5) . . . . ? Eu P3 C30 N3 -33.5(4) . . . . ? O32 P3 C31 C36 94.9(6) . . . . ? O31 P3 C31 C36 -30.9(6) . . . . ? C30 P3 C31 C36 -147.2(5) . . . . ? Eu P3 C31 C36 -60.5(7) . . . . ? O32 P3 C31 C32 -76.8(7) . . . . ? O31 P3 C31 C32 157.4(6) . . . . ? C30 P3 C31 C32 41.0(7) . . . . ? Eu P3 C31 C32 127.8(5) . . . . ? C36 C31 C32 C33 -1.2(11) . . . . ? P3 C31 C32 C33 170.5(6) . . . . ? C31 C32 C33 C34 -1.6(13) . . . . ? C32 C33 C34 C35 2.3(14) . . . . ? C33 C34 C35 C36 -0.2(14) . . . . ? C34 C35 C36 C31 -2.7(13) . . . . ? C32 C31 C36 C35 3.4(11) . . . . ? P3 C31 C36 C35 -168.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.384 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.101 data_nd16e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ' [NdL]2*14H2O (!centrosymmetric dimer!) ' _chemical_formula_sum 'C30 H54 N4 Nd O13 P3' _chemical_formula_weight 915.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no. 14) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.112(3) _cell_length_b 19.758(5) _cell_length_c 15.928(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.38(2) _cell_angle_gamma 90.00 _cell_volume 3892.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 170(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _exptl_crystal_description prisms _exptl_crystal_colour 'pale pink ' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min -- _exptl_absorpt_correction_T_max -- _exptl_special_details ; crystal coated by thin paraphine film due to a loss of solvate molecules ; _diffrn_ambient_temperature 170(1) _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 ' CAD4 (Enraf-Nonius) ' _diffrn_measurement_method '.omega.-2.theta. ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min ' _diffrn_standards_decay_% 5.4 _diffrn_reflns_number 5670 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.01 _reflns_number_total 5405 _reflns_number_gt 4286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 program packet ' _computing_cell_refinement 'CAD4 program packet ' _computing_data_reduction 'JANA-98 (Petricek, 1998)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992) ' _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+22.3266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson + Fourier' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5405 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 5.249 _refine_ls_shift/su_mean 0.053 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd Nd 0.66692(3) 0.61352(2) 0.02499(3) 0.0393(2) Uani 1 d . . . P1 P 0.9037(2) 0.65244(16) 0.1978(2) 0.0629(8) Uani 1 d . . . P2 P 0.5651(2) 0.77215(14) 0.0597(2) 0.0629(8) Uani 1 d . . . P3 P 0.40223(17) 0.56312(12) -0.07959(17) 0.0408(6) Uani 1 d . . . O11 O 0.8168(5) 0.5997(3) 0.1563(5) 0.0548(17) Uani 1 d . . . O12 O 0.8895(6) 0.6936(4) 0.2725(5) 0.076(2) Uani 1 d . . . O21 O 0.6338(5) 0.7114(3) 0.1018(5) 0.0561(17) Uani 1 d . . . O22 O 0.6158(6) 0.8408(4) 0.0897(7) 0.089(3) Uani 1 d . . . O31 O 0.4744(4) 0.6114(3) -0.0139(4) 0.0388(13) Uani 1 d . . . O32 O 0.3699(4) 0.5005(3) -0.0422(4) 0.0439(15) Uani 1 d . . . N1 N 0.8489(6) 0.6816(4) 0.0175(6) 0.0479(19) Uani 1 d . . . N2 N 0.6217(6) 0.7263(4) -0.0803(7) 0.056(2) Uani 1 d . . . N3 N 0.5627(5) 0.5857(4) -0.1502(5) 0.0441(18) Uani 1 d . . . N4 N 0.7894(6) 0.5418(4) -0.0520(6) 0.0475(19) Uani 1 d . . . C1 C 0.8205(9) 0.7351(6) -0.0518(10) 0.064(3) Uani 1 d . . . H011 H 0.809(10) 0.712(7) -0.119(9) 0.09(4) Uiso 1 d . . . H012 H 0.876(11) 0.761(7) -0.027(8) 0.09(4) Uiso 1 d . . . C2 C 0.7176(9) 0.7715(5) -0.0581(10) 0.060(3) Uani 1 d . . . H021 H 0.721(6) 0.781(4) -0.003(5) 0.02(2) Uiso 1 d . . . H022 H 0.695(9) 0.812(6) -0.109(8) 0.09(4) Uiso 1 d . . . C3 C 0.5886(9) 0.7093(6) -0.1746(8) 0.061(3) Uani 1 d . . . H031 H 0.637(10) 0.699(7) -0.204(8) 0.09(4) Uiso 1 d . . . H032 H 0.548(7) 0.750(5) -0.217(6) 0.05(2) Uiso 1 d . . . C4 C 0.5130(8) 0.6492(5) -0.1985(8) 0.051(2) Uani 1 d . . . H041 H 0.460(6) 0.656(4) -0.166(4) 0.018(17) Uiso 1 d . . . H042 H 0.485(8) 0.643(5) -0.266(7) 0.06(3) Uiso 1 d . . . C5 C 0.6352(8) 0.5550(6) -0.1945(8) 0.052(2) Uani 1 d . . . H051 H 0.671(8) 0.599(5) -0.213(7) 0.06(3) Uiso 1 d . . . H052 H 0.589(8) 0.533(5) -0.242(7) 0.06(3) Uiso 1 d . . . C6 C 0.7173(8) 0.5090(6) -0.1311(8) 0.058(3) Uani 1 d . . . H061 H 0.684(5) 0.479(4) -0.118(4) 0.004(17) Uiso 1 d . . . H062 H 0.754(7) 0.486(5) -0.170(6) 0.05(2) Uiso 1 d . . . C7 C 0.8661(7) 0.5856(5) -0.0765(8) 0.049(2) Uani 1 d . . . H071 H 0.826(7) 0.606(4) -0.134(6) 0.04(2) Uiso 1 d . . . H072 H 0.925(6) 0.557(4) -0.093(4) 0.021(17) Uiso 1 d . . . C8 C 0.9235(7) 0.6324(5) -0.0024(8) 0.052(3) Uani 1 d . . . H081 H 0.953(7) 0.610(4) 0.050(6) 0.03(2) Uiso 1 d . . . H082 H 0.974(7) 0.662(4) -0.024(5) 0.04(2) Uiso 1 d . . . C10 C 0.9010(9) 0.7104(6) 0.1054(8) 0.062(3) Uani 1 d . . . H101 H 0.859(7) 0.748(5) 0.113(5) 0.03(2) Uiso 1 d . . . H102 H 0.973(10) 0.723(6) 0.124(8) 0.09(4) Uiso 1 d . . . C11 C 1.0327(8) 0.6090(6) 0.2394(7) 0.064(3) Uani 1 d . . . C12 C 1.0339(10) 0.5390(7) 0.2491(9) 0.076(3) Uani 1 d . . . H12 H 0.958(10) 0.520(6) 0.206(8) 0.09(4) Uiso 1 d . . . C13 C 1.1290(11) 0.5074(8) 0.2930(10) 0.087(4) Uani 1 d . . . H13 H 1.144(7) 0.453(5) 0.318(6) 0.05(3) Uiso 1 d . . . C14 C 1.2258(11) 0.5431(10) 0.3279(10) 0.095(5) Uani 1 d . . . H14 H 1.315(11) 0.530(7) 0.373(9) 0.11(4) Uiso 1 d . . . C15 C 1.2245(11) 0.6133(9) 0.3146(10) 0.087(4) Uani 1 d . . . H15 H 1.286(12) 0.629(7) 0.339(9) 0.09(4) Uiso 1 d . . . C16 C 0.1413(2) 0.68545(14) -0.1451(2) 0.080(4) Uani 1 d . . . H16 H 0.1160 0.7200 -0.1177 0.096 Uiso 1 calc R . . C20 C 0.5334(2) 0.75977(14) -0.0581(2) 0.060(3) Uani 1 d R . . H201 H 0.4638 0.7347 -0.0761 0.027(19) Uiso 1 d R . . H202 H 0.5169 0.7939 -0.0888 0.06(3) Uiso 1 d R . . C21 C 0.4382(2) 0.77006(14) 0.0808(2) 0.072(3) Uani 1 d R . . C22 C 0.3728(2) 0.82545(14) 0.0597(2) 0.093(5) Uani 1 d R . . H22 H 0.3915 0.8628 0.0323 0.112 Uiso 1 calc R . . C23 C 0.2746(2) 0.82492(14) 0.0805(2) 0.122(7) Uani 1 d R . . H23 H 0.2206 0.8710 0.0624 0.08(4) Uiso 1 d R . . C24 C 0.2478(2) 0.77256(14) 0.1187(2) 0.127(8) Uani 1 d R . . H24 H 0.2171 0.7676 0.1498 0.17(8) Uiso 1 d R . . C25 C 0.3135(2) 0.71503(14) 0.1389(2) 0.094(5) Uani 1 d R . . H25 H 0.3101 0.6656 0.1674 0.08(4) Uiso 1 d R . . C26 C 0.4078(2) 0.71593(14) 0.1181(2) 0.077(4) Uani 1 d R . . H26 H 0.4338 0.6794 0.1412 0.03(2) Uiso 1 d R . . C30 C 0.4760(2) 0.53854(14) -0.1528(2) 0.048(2) Uani 1 d R . . H301 H 0.4982 0.5028 -0.1406 0.018(19) Uiso 1 d R . . H302 H 0.4340 0.5399 -0.2033 0.03(2) Uiso 1 d R . . C31 C 0.2795(2) 0.60587(14) -0.1415(2) 0.049(2) Uani 1 d R . . C32 C 0.2124(2) 0.58209(14) -0.2229(2) 0.065(3) Uani 1 d R . . H32 H 0.2359 0.5474 -0.2514 0.078 Uiso 1 calc R . . C33 C 0.1118(2) 0.60939(14) -0.2616(2) 0.081(4) Uani 1 d R . . H33 H 0.0824 0.5967 -0.3090 0.07(4) Uiso 1 d R . . C34 C 0.0772(2) 0.66200(14) -0.2228(2) 0.088(5) Uani 1 d R . . H34 H 0.0143 0.6826 -0.2537 0.08(4) Uiso 1 d R . . C35 C 1.1300(2) 0.64237(14) 0.2749(2) 0.080(4) Uani 1 d R . . H35 H 1.1179 0.6788 0.2594 0.05(3) Uiso 1 d R . . C36 C 0.2444(2) 0.66043(14) -0.1034(2) 0.062(3) Uani 1 d R . . H36 H 0.2807 0.6730 -0.0520 0.06(3) Uiso 1 d R . . C40 C 0.8498(2) 0.48797(14) 0.0083(2) 0.055(3) Uani 1 d R . . H40A H 0.8988 0.5080 0.0613 0.05(3) Uiso 1 calc R . . H40B H 0.8899 0.4619 -0.0210 0.026(19) Uiso 1 calc R . . H40C H 0.8000 0.4590 0.0237 0.07(3) Uiso 1 calc R . . O99 O 0.6348(2) 0.60875(14) 0.2136(2) 0.180(8) Uani 1 d R . . O97 O 0.9840(2) 0.60952(14) 0.4437(2) 0.61(6) Uani 1.00(10) d R . . O96 O 0.8038(2) 0.82673(14) 0.2338(2) 0.097(4) Uani 1.00(3) d R . . O95 O 0.5657(2) 0.55005(14) 0.4779(2) 0.33(2) Uani 1.00(5) d R . . OW1 O 0.5233(2) 0.09286(14) 0.2040(2) 0.156(12) Uani 0.67(3) d PR . . OW2 O 0.2937(2) 0.03428(14) 0.1290(2) 0.42(4) Uani 1.00(6) d R . . OW3 O 0.0764(2) 0.10892(14) 0.0719(2) 0.28(5) Uani 0.43(6) d PR . . QN N 0.7053(2) 0.63400(14) -0.0661(2) 0.050 Uiso 0.00 d PR . . QO O 0.6388(2) 0.60573(14) 0.0718(2) 0.050 Uiso 0.00 d PR . . 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 Nd 0.0286(3) 0.0268(3) 0.0661(4) -0.0011(2) 0.0205(2) 0.00126(18) P1 0.0443(15) 0.0641(18) 0.086(2) -0.0132(16) 0.0289(14) -0.0062(13) P2 0.0445(14) 0.0428(15) 0.103(2) -0.0135(15) 0.0274(15) 0.0081(12) P3 0.0269(11) 0.0339(12) 0.0643(15) 0.0032(11) 0.0190(10) 0.0045(9) O11 0.042(4) 0.049(4) 0.074(4) 0.000(3) 0.019(3) 0.000(3) O12 0.059(5) 0.091(6) 0.089(6) -0.023(5) 0.038(4) -0.003(4) O21 0.039(3) 0.049(4) 0.082(5) -0.012(3) 0.024(3) 0.001(3) O22 0.062(5) 0.043(4) 0.160(9) -0.034(5) 0.034(5) 0.001(4) O31 0.031(3) 0.027(3) 0.063(4) 0.004(3) 0.021(3) 0.008(2) O32 0.025(3) 0.037(3) 0.075(4) -0.001(3) 0.022(3) 0.002(2) N1 0.037(4) 0.027(4) 0.085(6) -0.002(4) 0.026(4) -0.002(3) N2 0.043(4) 0.028(4) 0.105(7) 0.013(4) 0.035(5) 0.003(3) N3 0.030(4) 0.038(4) 0.066(5) 0.003(4) 0.019(3) 0.002(3) N4 0.030(4) 0.041(4) 0.078(5) -0.005(4) 0.027(4) 0.001(3) C1 0.045(6) 0.040(6) 0.117(11) 0.006(6) 0.041(6) -0.004(5) C2 0.052(6) 0.033(6) 0.103(10) -0.001(6) 0.035(6) -0.003(5) C3 0.048(6) 0.059(7) 0.083(8) 0.028(6) 0.030(6) 0.014(5) C4 0.045(5) 0.044(6) 0.068(7) 0.010(5) 0.025(5) 0.005(4) C5 0.034(5) 0.060(7) 0.067(7) -0.017(6) 0.024(5) -0.006(5) C6 0.035(5) 0.058(7) 0.091(8) -0.012(6) 0.033(6) -0.001(5) C7 0.033(5) 0.049(6) 0.072(7) 0.000(5) 0.027(5) 0.001(4) C8 0.030(5) 0.051(6) 0.083(8) 0.008(6) 0.031(5) 0.004(4) C10 0.042(6) 0.051(7) 0.101(9) -0.018(6) 0.032(6) -0.009(5) C11 0.045(6) 0.083(9) 0.066(7) -0.020(6) 0.020(5) -0.011(5) C12 0.057(7) 0.078(9) 0.096(9) -0.001(7) 0.030(7) 0.000(6) C13 0.066(8) 0.101(11) 0.099(10) 0.025(9) 0.033(7) 0.021(8) C14 0.063(9) 0.137(16) 0.083(9) -0.002(9) 0.023(7) 0.019(9) C15 0.044(8) 0.115(14) 0.097(10) -0.019(9) 0.018(7) -0.002(8) C16 0.059(7) 0.077(9) 0.118(11) 0.035(8) 0.046(7) 0.037(7) C20 0.043(5) 0.037(6) 0.103(9) 0.007(6) 0.027(5) 0.008(4) C21 0.051(6) 0.061(7) 0.117(10) -0.029(7) 0.045(7) 0.006(6) C22 0.060(7) 0.123(12) 0.095(9) 0.005(9) 0.023(7) 0.051(8) C23 0.064(9) 0.18(2) 0.125(13) -0.018(13) 0.042(9) 0.039(11) C24 0.058(8) 0.21(2) 0.134(14) -0.048(14) 0.058(10) 0.009(11) C25 0.065(8) 0.117(13) 0.115(11) -0.027(10) 0.049(8) 0.005(8) C26 0.052(7) 0.074(9) 0.110(10) -0.027(8) 0.032(7) 0.008(6) C30 0.038(5) 0.036(6) 0.068(7) 0.008(5) 0.015(5) 0.007(4) C31 0.032(5) 0.046(6) 0.072(7) 0.010(5) 0.022(5) -0.003(4) C32 0.045(6) 0.061(7) 0.091(8) 0.012(6) 0.025(6) 0.004(5) C33 0.044(6) 0.078(9) 0.101(11) 0.039(8) -0.001(7) -0.006(6) C34 0.039(6) 0.080(9) 0.147(13) 0.054(9) 0.032(7) 0.020(6) C35 0.047(7) 0.090(11) 0.103(10) -0.024(8) 0.027(6) -0.013(7) C36 0.049(6) 0.057(7) 0.084(8) 0.020(6) 0.027(6) 0.020(5) C40 0.043(5) 0.036(5) 0.097(8) -0.002(5) 0.039(6) 0.007(4) O99 0.129(10) 0.067(7) 0.40(3) 0.032(10) 0.164(14) 0.015(6) O97 0.82(12) 0.72(11) 0.39(6) -0.23(5) 0.36(7) -0.03(6) O96 0.074(6) 0.101(8) 0.130(9) -0.034(6) 0.052(6) -0.018(5) O95 0.32(3) 0.088(13) 0.44(5) -0.014(18) -0.05(3) -0.034(15) OW1 0.19(2) 0.128(17) 0.19(2) 0.072(15) 0.111(18) 0.035(14) OW2 0.53(6) 0.19(3) 0.40(5) 0.14(3) -0.05(4) -0.07(3) OW3 0.60(10) 0.019(14) 0.46(9) -0.04(2) 0.48(9) -0.06(2) _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 Nd QO 0.948(3) . ? Nd QN 1.734(3) . ? Nd O32 2.340(6) 3_665 ? Nd O11 2.362(7) . ? Nd O31 2.392(5) . ? Nd O21 2.403(6) . ? Nd N4 2.720(7) . ? Nd N3 2.725(8) . ? Nd N2 2.732(8) . ? Nd N1 2.776(7) . ? P1 O12 1.504(8) . ? P1 O11 1.525(7) . ? P1 C11 1.814(12) . ? P1 C10 1.856(13) . ? P2 O22 1.516(8) . ? P2 O21 1.517(7) . ? P2 C20 1.799(4) . ? P2 C21 1.804(4) . ? P3 O32 1.493(6) . ? P3 O31 1.498(6) . ? P3 C31 1.794(3) . ? P3 C30 1.811(3) . ? O32 Nd 2.340(6) 3_665 ? N1 C10 1.454(14) . ? N1 C1 1.483(15) . ? N1 C8 1.486(12) . ? N2 C3 1.458(15) . ? N2 C20 1.475(8) . ? N2 C2 1.487(13) . ? N3 C30 1.459(7) . ? N3 C5 1.488(12) . ? N3 C4 1.504(12) . ? N4 C6 1.453(14) . ? N4 C7 1.473(12) . ? N4 C40 1.475(8) . ? C1 C2 1.503(14) . ? C1 H011 1.13(13) . ? C1 H012 0.87(13) . ? C2 H021 0.88(8) . ? C2 H022 1.10(12) . ? C3 C4 1.512(15) . ? C3 H031 0.92(13) . ? C3 H032 1.06(10) . ? C4 H041 1.00(7) . ? C4 H042 1.02(10) . ? C5 C6 1.510(16) . ? C5 H051 1.08(11) . ? C5 H052 0.91(10) . ? C6 H061 0.81(7) . ? C6 H062 1.00(10) . ? C7 C8 1.491(15) . ? C7 H071 0.97(9) . ? C7 H072 1.06(7) . ? C8 H081 0.91(8) . ? C8 H082 1.01(9) . ? C10 H101 0.96(9) . ? C10 H102 0.92(12) . ? C11 C35 1.379(11) . ? C11 C12 1.391(17) . ? C12 C13 1.362(17) . ? C12 H12 1.07(12) . ? C13 C14 1.40(2) . ? C13 H13 1.13(10) . ? C14 C15 1.40(2) . ? C14 H14 1.18(14) . ? C15 C35 1.322(14) . ? C15 H15 0.83(14) . ? C16 C34 1.3269 . ? C16 C36 1.3845 . ? C16 H16 0.9300 . ? C20 H201 0.9932 . ? C20 H202 0.8187 . ? C21 C26 1.3458 . ? C21 C22 1.3618 . ? C22 C23 1.4328 . ? C22 H22 0.9300 . ? C23 C24 1.3060 . ? C23 H23 1.1310 . ? C24 C25 1.3984 . ? C24 H24 0.7402 . ? C25 C26 1.3821 . ? C25 H25 1.0837 . ? C26 H26 0.8309 . ? C30 H301 0.7641 . ? C30 H302 0.8102 . ? C31 C32 1.3858 . ? C31 C36 1.3881 . ? C32 C33 1.3680 . ? C32 H32 0.9300 . ? C33 C34 1.3615 . ? C33 H33 0.7665 . ? C34 H34 0.9048 . ? C35 H35 0.7614 . ? C36 H36 0.8370 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? O97 OW3 0.746(5) 2_655 ? OW3 O97 0.746(5) 2_645 ? 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 QO Nd QN 173.2(2) . . ? QO Nd O32 66.5(2) . 3_665 ? QN Nd O32 116.85(18) . 3_665 ? QO Nd O11 73.2(2) . . ? QN Nd O11 112.37(19) . . ? O32 Nd O11 85.9(2) 3_665 . ? QO Nd O31 63.1(2) . . ? QN Nd O31 111.23(17) . . ? O32 Nd O31 76.84(18) 3_665 . ? O11 Nd O31 136.3(2) . . ? QO Nd O21 63.1(2) . . ? QN Nd O21 112.94(19) . . ? O32 Nd O21 129.5(2) 3_665 . ? O11 Nd O21 83.1(2) . . ? O31 Nd O21 78.0(2) . . ? QO Nd N4 135.4(2) . . ? QN Nd N4 50.61(19) . . ? O32 Nd N4 74.2(2) 3_665 . ? O11 Nd N4 84.1(2) . . ? O31 Nd N4 127.2(2) . . ? O21 Nd N4 151.9(2) . . ? QO Nd N3 125.4(2) . . ? QN Nd N3 51.44(17) . . ? O32 Nd N3 82.7(2) 3_665 . ? O11 Nd N3 150.5(2) . . ? O31 Nd N3 66.7(2) . . ? O21 Nd N3 124.7(2) . . ? N4 Nd N3 66.7(2) . . ? QO Nd N2 123.6(2) . . ? QN Nd N2 50.2(2) . . ? O32 Nd N2 147.8(2) 3_665 . ? O11 Nd N2 125.8(2) . . ? O31 Nd N2 81.9(2) . . ? O21 Nd N2 67.5(3) . . ? N4 Nd N2 100.9(2) . . ? N3 Nd N2 66.6(3) . . ? QO Nd N1 132.6(3) . . ? QN Nd N1 50.1(2) . . ? O32 Nd N1 133.29(19) 3_665 . ? O11 Nd N1 67.7(2) . . ? O31 Nd N1 147.8(2) . . ? O21 Nd N1 86.3(2) . . ? N4 Nd N1 65.7(2) . . ? N3 Nd N1 101.5(2) . . ? N2 Nd N1 66.0(2) . . ? O12 P1 O11 116.2(4) . . ? O12 P1 C11 108.2(5) . . ? O11 P1 C11 107.9(5) . . ? O12 P1 C10 108.6(5) . . ? O11 P1 C10 105.3(5) . . ? C11 P1 C10 110.6(5) . . ? O22 P2 O21 115.8(4) . . ? O22 P2 C20 112.0(5) . . ? O21 P2 C20 104.5(3) . . ? O22 P2 C21 107.3(3) . . ? O21 P2 C21 110.4(3) . . ? C20 P2 C21 106.4(2) . . ? O32 P3 O31 116.5(4) . . ? O32 P3 C31 106.7(3) . . ? O31 P3 C31 109.1(3) . . ? O32 P3 C30 108.5(3) . . ? O31 P3 C30 105.8(3) . . ? C31 P3 C30 110.2(2) . . ? P1 O11 Nd 126.0(4) . . ? P2 O21 Nd 126.4(4) . . ? P3 O31 Nd 124.0(3) . . ? P3 O32 Nd 160.3(4) . 3_665 ? C10 N1 C1 111.0(9) . . ? C10 N1 C8 109.2(8) . . ? C1 N1 C8 109.1(8) . . ? C10 N1 Nd 106.5(6) . . ? C1 N1 Nd 111.7(6) . . ? C8 N1 Nd 109.2(5) . . ? C3 N2 C20 111.2(7) . . ? C3 N2 C2 108.8(9) . . ? C20 N2 C2 110.0(7) . . ? C3 N2 Nd 112.0(6) . . ? C20 N2 Nd 104.3(4) . . ? C2 N2 Nd 110.5(7) . . ? C30 N3 C5 109.9(7) . . ? C30 N3 C4 108.5(6) . . ? C5 N3 C4 109.5(8) . . ? C30 N3 Nd 106.2(4) . . ? C5 N3 Nd 112.7(6) . . ? C4 N3 Nd 109.9(6) . . ? C6 N4 C7 109.6(9) . . ? C6 N4 C40 107.3(7) . . ? C7 N4 C40 109.3(6) . . ? C6 N4 Nd 108.2(5) . . ? C7 N4 Nd 111.7(5) . . ? C40 N4 Nd 110.6(4) . . ? N1 C1 C2 112.9(9) . . ? N1 C1 H011 110(6) . . ? C2 C1 H011 107(6) . . ? N1 C1 H012 97(9) . . ? C2 C1 H012 110(9) . . ? H011 C1 H012 120(10) . . ? N2 C2 C1 113.4(9) . . ? N2 C2 H021 97(5) . . ? C1 C2 H021 106(5) . . ? N2 C2 H022 105(6) . . ? C1 C2 H022 115(6) . . ? H021 C2 H022 119(8) . . ? N2 C3 C4 112.7(9) . . ? N2 C3 H031 123(8) . . ? C4 C3 H031 102(8) . . ? N2 C3 H032 113(5) . . ? C4 C3 H032 107(5) . . ? H031 C3 H032 98(9) . . ? N3 C4 C3 112.9(8) . . ? N3 C4 H041 96(4) . . ? C3 C4 H041 106(4) . . ? N3 C4 H042 113(6) . . ? C3 C4 H042 110(6) . . ? H041 C4 H042 119(7) . . ? N3 C5 C6 110.8(9) . . ? N3 C5 H051 102(5) . . ? C6 C5 H051 113(5) . . ? N3 C5 H052 103(6) . . ? C6 C5 H052 114(6) . . ? H051 C5 H052 112(8) . . ? N4 C6 C5 115.2(9) . . ? N4 C6 H061 111(5) . . ? C5 C6 H061 107(5) . . ? N4 C6 H062 116(5) . . ? C5 C6 H062 104(5) . . ? H061 C6 H062 102(7) . . ? N4 C7 C8 111.3(8) . . ? N4 C7 H071 107(5) . . ? C8 C7 H071 117(5) . . ? N4 C7 H072 112(4) . . ? C8 C7 H072 108(4) . . ? H071 C7 H072 101(6) . . ? N1 C8 C7 112.3(8) . . ? N1 C8 H081 103(5) . . ? C7 C8 H081 112(5) . . ? N1 C8 H082 104(5) . . ? C7 C8 H082 108(5) . . ? H081 C8 H082 117(7) . . ? N1 C10 P1 113.7(7) . . ? N1 C10 H101 108(5) . . ? P1 C10 H101 104(5) . . ? N1 C10 H102 121(8) . . ? P1 C10 H102 99(8) . . ? H101 C10 H102 109(9) . . ? C35 C11 C12 117.0(10) . . ? C35 C11 P1 123.2(8) . . ? C12 C11 P1 119.1(9) . . ? C13 C12 C11 119.2(13) . . ? C13 C12 H12 131(7) . . ? C11 C12 H12 108(7) . . ? C12 C13 C14 121.9(15) . . ? C12 C13 H13 130(5) . . ? C14 C13 H13 108(5) . . ? C13 C14 C15 118.4(14) . . ? C13 C14 H14 136(7) . . ? C15 C14 H14 106(7) . . ? C35 C15 C14 117.7(13) . . ? C35 C15 H15 132(10) . . ? C14 C15 H15 110(10) . . ? C34 C16 C36 122.6 . . ? C34 C16 H16 118.7 . . ? C36 C16 H16 118.7 . . ? N2 C20 P2 112.5(4) . . ? N2 C20 H201 115.2 . . ? P2 C20 H201 104.0 . . ? N2 C20 H202 107.4 . . ? P2 C20 H202 115.8 . . ? H201 C20 H202 101.7 . . ? C26 C21 C22 119.6 . . ? C26 C21 P2 121.77(13) . . ? C22 C21 P2 118.65(13) . . ? C21 C22 C23 118.5 . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 121.0 . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 118.0 . . ? C23 C24 C25 120.7 . . ? C23 C24 H24 134.9 . . ? C25 C24 H24 99.7 . . ? C26 C25 C24 117.8 . . ? C26 C25 H25 106.1 . . ? C24 C25 H25 136.1 . . ? C21 C26 C25 122.4 . . ? C21 C26 H26 138.5 . . ? C25 C26 H26 98.6 . . ? N3 C30 P3 112.8(4) . . ? N3 C30 H301 110.8 . . ? P3 C30 H301 108.8 . . ? N3 C30 H302 106.0 . . ? P3 C30 H302 107.3 . . ? H301 C30 H302 111.0 . . ? C32 C31 C36 118.2 . . ? C32 C31 P3 121.99(12) . . ? C36 C31 P3 119.51(12) . . ? C33 C32 C31 120.4 . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.9 . . ? C34 C33 H33 124.2 . . ? C32 C33 H33 114.1 . . ? C16 C34 C33 119.1 . . ? C16 C34 H34 122.1 . . ? C33 C34 H34 118.5 . . ? C15 C35 C11 125.6(9) . . ? C15 C35 H35 128.9 . . ? C11 C35 H35 104.7 . . ? C16 C36 C31 118.7 . . ? C16 C36 H36 120.7 . . ? C31 C36 H36 119.7 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 Nd 97.4(6) . . . . ? C11 P1 O11 Nd -141.0(5) . . . . ? C10 P1 O11 Nd -22.8(6) . . . . ? QO Nd O11 P1 -118.5(5) . . . . ? QN Nd O11 P1 57.4(5) . . . . ? O32 Nd O11 P1 174.8(5) 3_665 . . . ? O31 Nd O11 P1 -119.2(4) . . . . ? O21 Nd O11 P1 -54.6(5) . . . . ? N4 Nd O11 P1 100.3(5) . . . . ? N3 Nd O11 P1 107.5(5) . . . . ? N2 Nd O11 P1 1.2(6) . . . . ? N1 Nd O11 P1 34.2(4) . . . . ? O22 P2 O21 Nd -132.2(5) . . . . ? C20 P2 O21 Nd -8.5(5) . . . . ? C21 P2 O21 Nd 105.6(4) . . . . ? QO Nd O21 P2 -125.4(5) . . . . ? QN Nd O21 P2 48.6(5) . . . . ? O32 Nd O21 P2 -121.2(4) 3_665 . . . ? O11 Nd O21 P2 160.0(5) . . . . ? O31 Nd O21 P2 -59.6(4) . . . . ? N4 Nd O21 P2 96.5(6) . . . . ? N3 Nd O21 P2 -9.4(6) . . . . ? N2 Nd O21 P2 26.5(4) . . . . ? N1 Nd O21 P2 92.1(5) . . . . ? O32 P3 O31 Nd 95.9(4) . . . . ? C31 P3 O31 Nd -143.3(3) . . . . ? C30 P3 O31 Nd -24.7(4) . . . . ? QO Nd O31 P3 -120.8(4) . . . . ? QN Nd O31 P3 63.3(4) . . . . ? O32 Nd O31 P3 -50.7(4) 3_665 . . . ? O11 Nd O31 P3 -120.1(4) . . . . ? O21 Nd O31 P3 173.5(4) . . . . ? N4 Nd O31 P3 7.3(5) . . . . ? N3 Nd O31 P3 36.9(4) . . . . ? N2 Nd O31 P3 104.9(4) . . . . ? N1 Nd O31 P3 110.9(5) . . . . ? O31 P3 O32 Nd -136.4(10) . . . 3_665 ? C31 P3 O32 Nd 101.5(10) . . . 3_665 ? C30 P3 O32 Nd -17.2(11) . . . 3_665 ? QO Nd N1 C10 -2.7(7) . . . . ? QN Nd N1 C10 169.0(7) . . . . ? O32 Nd N1 C10 -99.8(6) 3_665 . . . ? O11 Nd N1 C10 -39.4(6) . . . . ? O31 Nd N1 C10 105.2(7) . . . . ? O21 Nd N1 C10 44.7(6) . . . . ? N4 Nd N1 C10 -133.0(7) . . . . ? N3 Nd N1 C10 169.4(6) . . . . ? N2 Nd N1 C10 111.7(7) . . . . ? QO Nd N1 C1 -124.1(7) . . . . ? QN Nd N1 C1 47.6(7) . . . . ? O32 Nd N1 C1 138.9(7) 3_665 . . . ? O11 Nd N1 C1 -160.7(8) . . . . ? O31 Nd N1 C1 -16.2(9) . . . . ? O21 Nd N1 C1 -76.6(7) . . . . ? N4 Nd N1 C1 105.7(7) . . . . ? N3 Nd N1 C1 48.1(7) . . . . ? N2 Nd N1 C1 -9.7(7) . . . . ? QO Nd N1 C8 115.1(7) . . . . ? QN Nd N1 C8 -73.2(7) . . . . ? O32 Nd N1 C8 18.0(8) 3_665 . . . ? O11 Nd N1 C8 78.4(7) . . . . ? O31 Nd N1 C8 -137.0(6) . . . . ? O21 Nd N1 C8 162.5(7) . . . . ? N4 Nd N1 C8 -15.2(6) . . . . ? N3 Nd N1 C8 -72.8(7) . . . . ? N2 Nd N1 C8 -130.5(7) . . . . ? QO Nd N2 C3 -130.9(6) . . . . ? QN Nd N2 C3 45.5(6) . . . . ? O32 Nd N2 C3 -31.9(8) 3_665 . . . ? O11 Nd N2 C3 136.1(6) . . . . ? O31 Nd N2 C3 -80.9(6) . . . . ? O21 Nd N2 C3 -161.2(6) . . . . ? N4 Nd N2 C3 45.6(6) . . . . ? N3 Nd N2 C3 -12.9(6) . . . . ? N1 Nd N2 C3 102.6(6) . . . . ? QO Nd N2 C20 -10.6(5) . . . . ? QN Nd N2 C20 165.9(6) . . . . ? O32 Nd N2 C20 88.5(6) 3_665 . . . ? O11 Nd N2 C20 -103.5(4) . . . . ? O31 Nd N2 C20 39.5(4) . . . . ? O21 Nd N2 C20 -40.8(4) . . . . ? N4 Nd N2 C20 166.0(4) . . . . ? N3 Nd N2 C20 107.5(5) . . . . ? N1 Nd N2 C20 -137.0(5) . . . . ? QO Nd N2 C2 107.6(7) . . . . ? QN Nd N2 C2 -75.9(7) . . . . ? O32 Nd N2 C2 -153.3(6) 3_665 . . . ? O11 Nd N2 C2 14.7(8) . . . . ? O31 Nd N2 C2 157.7(7) . . . . ? O21 Nd N2 C2 77.4(7) . . . . ? N4 Nd N2 C2 -75.8(7) . . . . ? N3 Nd N2 C2 -134.3(7) . . . . ? N1 Nd N2 C2 -18.8(7) . . . . ? QO Nd N3 C30 -17.8(4) . . . . ? QN Nd N3 C30 169.8(5) . . . . ? O32 Nd N3 C30 36.6(4) 3_665 . . . ? O11 Nd N3 C30 104.6(5) . . . . ? O31 Nd N3 C30 -42.2(3) . . . . ? O21 Nd N3 C30 -97.1(4) . . . . ? N4 Nd N3 C30 112.4(4) . . . . ? N2 Nd N3 C30 -133.4(4) . . . . ? N1 Nd N3 C30 169.3(3) . . . . ? QO Nd N3 C5 -138.1(6) . . . . ? QN Nd N3 C5 49.4(6) . . . . ? O32 Nd N3 C5 -83.8(6) 3_665 . . . ? O11 Nd N3 C5 -15.8(9) . . . . ? O31 Nd N3 C5 -162.6(7) . . . . ? O21 Nd N3 C5 142.5(6) . . . . ? N4 Nd N3 C5 -7.9(6) . . . . ? N2 Nd N3 C5 106.3(6) . . . . ? N1 Nd N3 C5 49.0(6) . . . . ? QO Nd N3 C4 99.4(6) . . . . ? QN Nd N3 C4 -73.0(5) . . . . ? O32 Nd N3 C4 153.8(5) 3_665 . . . ? O11 Nd N3 C4 -138.2(6) . . . . ? O31 Nd N3 C4 75.0(5) . . . . ? O21 Nd N3 C4 20.1(6) . . . . ? N4 Nd N3 C4 -130.4(6) . . . . ? N2 Nd N3 C4 -16.2(5) . . . . ? N1 Nd N3 C4 -73.5(5) . . . . ? QO Nd N4 C6 96.6(8) . . . . ? QN Nd N4 C6 -79.2(7) . . . . ? O32 Nd N4 C6 68.0(7) 3_665 . . . ? O11 Nd N4 C6 155.4(7) . . . . ? O31 Nd N4 C6 8.8(8) . . . . ? O21 Nd N4 C6 -141.4(7) . . . . ? N3 Nd N4 C6 -20.8(7) . . . . ? N2 Nd N4 C6 -79.3(7) . . . . ? N1 Nd N4 C6 -136.5(8) . . . . ? QO Nd N4 C7 -142.6(6) . . . . ? QN Nd N4 C7 41.6(6) . . . . ? O32 Nd N4 C7 -171.2(7) 3_665 . . . ? O11 Nd N4 C7 -83.9(6) . . . . ? O31 Nd N4 C7 129.6(6) . . . . ? O21 Nd N4 C7 -20.6(9) . . . . ? N3 Nd N4 C7 100.0(7) . . . . ? N2 Nd N4 C7 41.5(7) . . . . ? N1 Nd N4 C7 -15.7(6) . . . . ? QO Nd N4 C40 -20.6(5) . . . . ? QN Nd N4 C40 163.6(5) . . . . ? O32 Nd N4 C40 -49.2(4) 3_665 . . . ? O11 Nd N4 C40 38.2(4) . . . . ? O31 Nd N4 C40 -108.4(4) . . . . ? O21 Nd N4 C40 101.4(6) . . . . ? N3 Nd N4 C40 -138.0(5) . . . . ? N2 Nd N4 C40 163.5(4) . . . . ? N1 Nd N4 C40 106.3(5) . . . . ? C10 N1 C1 C2 -80.8(12) . . . . ? C8 N1 C1 C2 158.8(10) . . . . ? Nd N1 C1 C2 38.0(12) . . . . ? C3 N2 C2 C1 -75.6(13) . . . . ? C20 N2 C2 C1 162.3(10) . . . . ? Nd N2 C2 C1 47.7(13) . . . . ? N1 C1 C2 N2 -60.0(16) . . . . ? C20 N2 C3 C4 -74.6(9) . . . . ? C2 N2 C3 C4 164.1(8) . . . . ? Nd N2 C3 C4 41.7(9) . . . . ? C30 N3 C4 C3 160.6(8) . . . . ? C5 N3 C4 C3 -79.4(11) . . . . ? Nd N3 C4 C3 44.9(10) . . . . ? N2 C3 C4 N3 -60.7(11) . . . . ? C30 N3 C5 C6 -82.9(9) . . . . ? C4 N3 C5 C6 158.0(9) . . . . ? Nd N3 C5 C6 35.3(10) . . . . ? C7 N4 C6 C5 -71.2(10) . . . . ? C40 N4 C6 C5 170.2(8) . . . . ? Nd N4 C6 C5 50.9(10) . . . . ? N3 C5 C6 N4 -61.0(12) . . . . ? C6 N4 C7 C8 166.4(8) . . . . ? C40 N4 C7 C8 -76.3(9) . . . . ? Nd N4 C7 C8 46.5(9) . . . . ? C10 N1 C8 C7 162.2(9) . . . . ? C1 N1 C8 C7 -76.3(11) . . . . ? Nd N1 C8 C7 46.1(10) . . . . ? N4 C7 C8 N1 -64.9(11) . . . . ? C1 N1 C10 P1 163.5(7) . . . . ? C8 N1 C10 P1 -76.1(9) . . . . ? Nd N1 C10 P1 41.6(8) . . . . ? O12 P1 C10 N1 -144.1(7) . . . . ? O11 P1 C10 N1 -19.0(8) . . . . ? C11 P1 C10 N1 97.3(8) . . . . ? O12 P1 C11 C35 -58.7(10) . . . . ? O11 P1 C11 C35 174.8(7) . . . . ? C10 P1 C11 C35 60.2(10) . . . . ? O12 P1 C11 C12 111.1(10) . . . . ? O11 P1 C11 C12 -15.4(11) . . . . ? C10 P1 C11 C12 -130.1(10) . . . . ? C35 C11 C12 C13 0.6(18) . . . . ? P1 C11 C12 C13 -169.8(10) . . . . ? C11 C12 C13 C14 -1(2) . . . . ? C12 C13 C14 C15 -2(2) . . . . ? C13 C14 C15 C35 5(2) . . . . ? C3 N2 C20 P2 172.8(6) . . . . ? C2 N2 C20 P2 -66.5(9) . . . . ? Nd N2 C20 P2 52.0(4) . . . . ? O22 P2 C20 N2 92.4(5) . . . . ? O21 P2 C20 N2 -33.7(5) . . . . ? C21 P2 C20 N2 -150.6(3) . . . . ? O22 P2 C21 C26 -135.5(4) . . . . ? O21 P2 C21 C26 -8.5(4) . . . . ? C20 P2 C21 C26 104.42(18) . . . . ? O22 P2 C21 C22 43.4(5) . . . . ? O21 P2 C21 C22 170.4(3) . . . . ? C20 P2 C21 C22 -76.74(19) . . . . ? C26 C21 C22 C23 1.9 . . . . ? P2 C21 C22 C23 -176.97(16) . . . . ? C21 C22 C23 C24 -0.2 . . . . ? C22 C23 C24 C25 -1.1 . . . . ? C23 C24 C25 C26 0.7 . . . . ? C22 C21 C26 C25 -2.4 . . . . ? P2 C21 C26 C25 176.46(16) . . . . ? C24 C25 C26 C21 1.1 . . . . ? C5 N3 C30 P3 166.9(6) . . . . ? C4 N3 C30 P3 -73.4(7) . . . . ? Nd N3 C30 P3 44.8(4) . . . . ? O32 P3 C30 N3 -144.9(4) . . . . ? O31 P3 C30 N3 -19.2(4) . . . . ? C31 P3 C30 N3 98.6(4) . . . . ? O32 P3 C31 C32 -73.1(3) . . . . ? O31 P3 C31 C32 160.3(2) . . . . ? C30 P3 C31 C32 44.5(2) . . . . ? O32 P3 C31 C36 100.3(3) . . . . ? O31 P3 C31 C36 -26.4(3) . . . . ? C30 P3 C31 C36 -142.14(12) . . . . ? C36 C31 C32 C33 -3.8 . . . . ? P3 C31 C32 C33 169.63(13) . . . . ? C31 C32 C33 C34 2.6 . . . . ? C36 C16 C34 C33 2.8 . . . . ? C32 C33 C34 C16 -2.0 . . . . ? C14 C15 C35 C11 -5.1(18) . . . . ? C12 C11 C35 C15 2.5(15) . . . . ? P1 C11 C35 C15 172.4(9) . . . . ? C34 C16 C36 C31 -4.2 . . . . ? C32 C31 C36 C16 4.5 . . . . ? P3 C31 C36 C16 -169.10(12) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.911 _refine_diff_density_min -1.346 _refine_diff_density_rms 0.155 data_tb24e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[TbL]2*12H2O (!centrosymmetric dimer!)' _chemical_formula_sum 'C30 H52 N4 O12 P3 Tb' _chemical_formula_weight 912.59 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no. 14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.047(3) _cell_length_b 20.238(6) _cell_length_c 15.841(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.19(2) _cell_angle_gamma 90.00 _cell_volume 3873.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.66 _exptl_crystal_size_min 0.49 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 2.011 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min -- _exptl_absorpt_correction_T_max -- _exptl_special_details ; crystal coated by thin paraphine film due to a loss of solvent molecules ; _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 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method '.omega.-2.theta.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 11.8 _diffrn_reflns_number 6233 _diffrn_reflns_av_R_equivalents 0.2310 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.01 _reflns_number_total 5945 _reflns_number_gt 4986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 program packet' _computing_cell_refinement 'CAD4 program packet' _computing_data_reduction 'JANA-98 (Petricek, 1998)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992) _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson + Fourier' _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 5945 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.2677 _refine_ls_wR_factor_gt 0.2475 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _refine_ls_shift/su_max 4.680 _refine_ls_shift/su_mean 0.033 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb Tb 0.66897(3) 0.60853(2) 0.03474(3) 0.0188(3) Uani 1 d . . . P1 P 0.9014(2) 0.63380(16) 0.22575(17) 0.0317(6) Uani 1 d . . . O11 O 0.8137(6) 0.5849(4) 0.1711(5) 0.0341(16) Uani 1 d . . . O12 O 0.8884(7) 0.6673(4) 0.3055(5) 0.047(2) Uani 1 d . . . P2 P 0.5618(2) 0.74651(14) 0.09480(17) 0.0288(6) Uani 1 d . . . O21 O 0.6375(5) 0.6864(3) 0.1272(4) 0.0293(15) Uani 1 d . . . O22 O 0.6090(6) 0.8108(4) 0.1393(5) 0.0379(18) Uani 1 d . . . P3 P 0.39949(18) 0.56270(12) -0.07839(16) 0.0216(6) Uani 1 d . . . O31 O 0.4780(5) 0.6063(3) -0.0050(4) 0.0237(16) Uani 1 d . . . O32 O 0.3660(5) 0.4991(3) -0.0460(5) 0.0316(16) Uani 1 d . . . N1 N 0.8499(6) 0.6772(4) 0.0481(5) 0.0271(17) Uani 1 d . . . N2 N 0.6195(6) 0.7228(4) -0.0501(5) 0.0251(17) Uani 1 d . . . N3 N 0.5594(7) 0.5929(4) -0.1433(5) 0.0242(17) Uani 1 d . . . N4 N 0.7888(7) 0.5477(4) -0.0438(5) 0.0277(18) Uani 1 d . . . C1 C 0.8234(7) 0.7351(6) -0.0108(7) 0.028(2) Uani 1 d . . . H011 H 0.8190 0.7223 -0.0711 0.034 Uiso 1 calc R . . H012 H 0.8827 0.7672 0.0131 0.034 Uiso 1 calc R . . C2 C 0.7152(9) 0.7670(5) -0.0186(7) 0.034(2) Uani 1 d . . . H021 H 0.7232 0.7844 0.0406 0.041 Uiso 1 calc R . . H022 H 0.7007 0.8040 -0.0604 0.041 Uiso 1 calc R . . C3 C 0.5852(9) 0.7138(5) -0.1510(7) 0.035(2) Uani 1 d . . . H031 H 0.6504 0.7073 -0.1654 0.042 Uiso 1 calc R . . H032 H 0.5479 0.7535 -0.1820 0.042 Uiso 1 calc R . . C4 C 0.5085(8) 0.6552(5) -0.1847(6) 0.027(2) Uani 1 d . . . H041 H 0.4426 0.6626 -0.1716 0.033 Uiso 1 calc R . . H042 H 0.4859 0.6520 -0.2504 0.033 Uiso 1 calc R . . C5 C 0.6327(8) 0.5668(6) -0.1892(7) 0.035(2) Uani 1 d . . . H051 H 0.5876 0.5453 -0.2458 0.042 Uiso 1 calc R . . H052 H 0.6712 0.6033 -0.2038 0.042 Uiso 1 calc R . . C6 C 0.7158(8) 0.5184(6) -0.1296(7) 0.036(2) Uani 1 d . . . H061 H 0.6770 0.4813 -0.1166 0.043 Uiso 1 calc R . . H062 H 0.7601 0.5017 -0.1622 0.043 Uiso 1 calc R . . C7 C 0.8680(8) 0.5942(5) -0.0605(7) 0.032(2) Uani 1 d . . . H071 H 0.8284 0.6228 -0.1115 0.038 Uiso 1 calc R . . H072 H 0.9223 0.5693 -0.0757 0.038 Uiso 1 calc R . . C8 C 0.9265(8) 0.6357(5) 0.0243(7) 0.032(2) Uani 1 d . . . H081 H 0.9653 0.6067 0.0751 0.038 Uiso 1 calc R . . H082 H 0.9811 0.6636 0.0139 0.038 Uiso 1 calc R . . C11 C 1.0324(8) 0.5896(7) 0.2670(7) 0.037(3) Uani 1 d . . . C12 C 1.0365(11) 0.5235(7) 0.2599(8) 0.050(3) Uani 1 d . . . H12 H 0.9719 0.4998 0.2298 0.060 Uiso 1 calc R . . C13 C 1.1406(12) 0.4896(9) 0.2985(9) 0.065(4) Uani 1 d . . . H13 H 1.1448 0.4441 0.2920 0.078 Uiso 1 calc R . . C14 C 1.2335(12) 0.5257(11) 0.3450(11) 0.080(6) Uani 1 d . . . H14 H 1.3007 0.5040 0.3734 0.096 Uiso 1 calc R . . C15 C 1.2292(13) 0.5926(11) 0.3506(13) 0.079(5) Uani 1 d . . . H151 H 1.2939 0.6164 0.3803 0.094 Uiso 1 calc R . . C16 C 1.1308(11) 0.6252(9) 0.3129(10) 0.057(4) Uani 1 d . . . H16 H 1.1287 0.6709 0.3174 0.068 Uiso 1 calc R . . C21 C 0.4338(9) 0.7340(5) 0.1109(7) 0.032(2) Uani 1 d . . . C22 C 0.4194(11) 0.6767(7) 0.1564(9) 0.055(3) Uani 1 d . . . H22 H 0.4733 0.6439 0.1749 0.066 Uiso 1 calc R . . C23 C 0.3211(14) 0.6708(9) 0.1729(11) 0.073(5) Uani 1 d . . . H23 H 0.3071 0.6334 0.2009 0.088 Uiso 1 calc R . . C24 C 0.2439(17) 0.7237(12) 0.1454(17) 0.106(8) Uani 1 d . . . H24 H 0.1809 0.7215 0.1593 0.127 Uiso 1 calc R . . C25 C 0.2577(12) 0.7751(10) 0.1018(11) 0.073(4) Uani 1 d . . . H25 H 0.2031 0.8075 0.0823 0.087 Uiso 1 calc R . . C26 C 0.3525(10) 0.7819(7) 0.0843(9) 0.055(3) Uani 1 d . . . H26 H 0.3621 0.8194 0.0541 0.066 Uiso 1 calc R . . C31 C 0.2732(9) 0.6068(5) -0.1413(7) 0.028(2) Uani 1 d . . . C32 C 0.2099(10) 0.5900(8) -0.2297(9) 0.050(3) Uani 1 d . . . H32 H 0.2345 0.5585 -0.2605 0.060 Uiso 1 calc R . . C33 C 0.1059(12) 0.6217(9) -0.2730(12) 0.072(5) Uani 1 d . . . H33 H 0.0637 0.6136 -0.3341 0.086 Uiso 1 calc R . . C34 C 0.0676(11) 0.6652(8) -0.2231(12) 0.072(5) Uani 1 d . . . H34 H -0.0028 0.6835 -0.2494 0.086 Uiso 1 calc R . . C35 C 0.1345(12) 0.6810(7) -0.1343(12) 0.068(4) Uani 1 d . . . H35 H 0.1095 0.7105 -0.1013 0.082 Uiso 1 calc R . . C36 C 0.2356(9) 0.6537(6) -0.0955(9) 0.044(3) Uani 1 d . . . H36 H 0.2813 0.6665 -0.0369 0.053 Uiso 1 calc R . . C10 C 0.9048(8) 0.6982(5) 0.1457(6) 0.031(2) Uani 1 d . . . H101 H 0.8680 0.7373 0.1556 0.037 Uiso 1 calc R . . H102 H 0.9812 0.7097 0.1578 0.037 Uiso 1 calc R . . C20 C 0.5274(9) 0.7503(5) -0.0288(7) 0.033(2) Uani 1 d . . . H201 H 0.4604 0.7252 -0.0604 0.039 Uiso 1 calc R . . H202 H 0.5142 0.7958 -0.0494 0.039 Uiso 1 calc R . . C30 C 0.4715(7) 0.5428(5) -0.1541(6) 0.024(2) Uani 1 d . . . H301 H 0.5045 0.4992 -0.1396 0.029 Uiso 1 calc R . . H302 H 0.4191 0.5423 -0.2168 0.029 Uiso 1 calc R . . C40 C 0.8543(10) 0.4933(6) 0.0124(8) 0.042(3) Uani 1 d . . . H401 H 0.9037 0.5103 0.0699 0.062 Uiso 1 calc R . . H402 H 0.8964 0.4725 -0.0185 0.062 Uiso 1 calc R . . H403 H 0.8055 0.4614 0.0224 0.062 Uiso 1 calc R . . O99 O 0.6809(18) 0.5939(13) 0.3077(15) 0.199(16) Uani 1.00(6) d . . . O98 O 0.5117(13) 0.9216(7) 0.0420(10) 0.111(7) Uani 1.00(4) d . . . O97 O 0.977(3) 0.6084(10) 0.4789(15) 0.21(2) Uani 1.00(8) d . . . O96 O 0.8163(8) 0.7988(5) 0.2758(6) 0.065(4) Uani 1.00(3) d . . . O95 O 0.543(2) 0.5405(11) 0.3898(16) 0.195(14) Uani 1.00(5) d . . . O94 O 0.845(2) 0.4845(17) 0.4611(19) 0.24(2) Uani 1.00(6) d . . . QN N 0.7046 0.6350 -0.0470 0.050 Uiso 0.00 d P . . QO O 0.6409 0.5945 0.0851 0.050 Uiso 0.00 d P . . 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 Tb 0.0162(4) 0.0262(4) 0.0183(4) 0.00012(15) 0.0116(3) -0.00045(15) P1 0.0215(13) 0.0520(17) 0.0228(13) -0.0011(12) 0.0097(11) -0.0041(12) O11 0.026(4) 0.046(4) 0.023(4) 0.009(3) 0.001(3) -0.003(3) O12 0.039(4) 0.075(6) 0.030(4) 0.001(4) 0.015(3) 0.008(4) P2 0.0271(13) 0.0369(15) 0.0279(13) -0.0067(11) 0.0167(11) -0.0002(11) O21 0.033(4) 0.038(4) 0.018(3) 0.005(3) 0.011(3) 0.005(3) O22 0.040(4) 0.037(4) 0.042(4) -0.013(3) 0.022(4) -0.012(3) P3 0.0147(11) 0.0308(13) 0.0219(12) 0.0015(10) 0.0098(9) 0.0011(9) O31 0.017(3) 0.038(4) 0.018(3) 0.000(2) 0.008(3) -0.002(2) O32 0.023(3) 0.034(4) 0.037(4) 0.010(3) 0.010(3) 0.002(3) N1 0.025(4) 0.040(5) 0.021(4) -0.003(4) 0.014(3) -0.004(4) N2 0.023(4) 0.033(4) 0.025(4) 0.003(3) 0.016(3) 0.002(3) N3 0.019(4) 0.043(5) 0.016(4) -0.005(4) 0.012(3) -0.007(3) N4 0.024(4) 0.036(5) 0.026(4) 0.003(4) 0.013(3) -0.006(4) C1 0.017(5) 0.053(7) 0.025(5) 0.005(5) 0.020(4) -0.005(4) C2 0.041(6) 0.040(6) 0.032(5) 0.000(5) 0.025(5) -0.012(5) C3 0.031(5) 0.048(6) 0.028(5) 0.002(5) 0.015(4) -0.003(5) C4 0.033(5) 0.038(5) 0.015(4) 0.012(4) 0.014(4) 0.005(4) C5 0.023(5) 0.055(7) 0.033(6) 0.002(5) 0.016(4) 0.005(5) C6 0.026(5) 0.044(6) 0.046(6) -0.004(5) 0.023(5) -0.002(4) C7 0.020(5) 0.047(6) 0.032(6) -0.008(5) 0.014(4) -0.004(4) C8 0.030(5) 0.039(6) 0.033(5) -0.008(5) 0.019(4) -0.008(5) C11 0.015(5) 0.081(8) 0.015(5) 0.005(5) 0.005(4) -0.001(5) C12 0.045(7) 0.059(8) 0.045(7) 0.003(6) 0.015(6) 0.012(6) C13 0.051(9) 0.098(11) 0.048(8) 0.021(8) 0.023(7) 0.027(8) C14 0.044(9) 0.142(17) 0.064(9) 0.031(10) 0.032(8) 0.051(10) C15 0.024(8) 0.128(16) 0.068(11) -0.010(11) 0.000(7) 0.002(9) C16 0.031(7) 0.089(10) 0.049(8) -0.005(8) 0.012(6) -0.022(7) C21 0.032(5) 0.046(6) 0.025(5) -0.016(5) 0.019(4) -0.014(5) C22 0.060(8) 0.070(9) 0.056(8) -0.017(7) 0.046(7) -0.018(7) C23 0.079(11) 0.097(12) 0.068(10) -0.025(9) 0.055(9) -0.046(10) C24 0.084(14) 0.134(18) 0.141(19) -0.069(16) 0.091(14) -0.038(13) C25 0.045(8) 0.103(13) 0.078(11) -0.009(10) 0.032(8) 0.001(8) C26 0.033(6) 0.072(9) 0.064(8) -0.026(7) 0.022(6) 0.002(6) C31 0.023(5) 0.038(6) 0.026(6) 0.012(4) 0.013(4) 0.000(4) C32 0.018(6) 0.076(8) 0.047(8) 0.017(7) 0.003(5) -0.003(6) C33 0.024(7) 0.107(13) 0.066(10) 0.049(9) -0.003(7) 0.010(7) C34 0.031(7) 0.084(11) 0.108(13) 0.058(10) 0.034(8) 0.026(7) C35 0.042(8) 0.056(8) 0.103(12) 0.030(8) 0.023(8) 0.025(7) C36 0.030(6) 0.047(7) 0.058(7) 0.005(6) 0.020(5) 0.011(5) C10 0.022(5) 0.046(6) 0.019(5) -0.013(4) 0.003(4) -0.015(4) C20 0.042(6) 0.025(5) 0.035(6) -0.001(5) 0.019(5) 0.007(4) C30 0.017(4) 0.042(6) 0.008(4) -0.014(4) -0.001(3) -0.003(4) C40 0.044(6) 0.045(7) 0.048(7) -0.002(5) 0.032(6) 0.002(5) O99 0.140(19) 0.37(4) 0.16(2) -0.062(18) 0.137(17) -0.078(17) O98 0.127(13) 0.076(10) 0.112(12) 0.030(8) 0.027(9) 0.027(8) O97 0.31(4) 0.21(3) 0.102(18) 0.014(13) 0.07(2) 0.051(19) O96 0.053(6) 0.092(8) 0.055(6) -0.031(5) 0.028(5) -0.018(5) O95 0.29(3) 0.19(2) 0.17(2) -0.057(16) 0.15(2) -0.13(2) O94 0.25(4) 0.31(4) 0.23(4) 0.04(2) 0.18(3) 0.06(2) _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 Tb QO 1.0357(4) . ? Tb QN 1.6241(5) . ? Tb O32 2.247(7) 3_665 ? Tb O21 2.292(7) . ? Tb O11 2.319(7) . ? Tb O31 2.328(7) . ? Tb N2 2.629(8) . ? Tb N4 2.641(8) . ? Tb N3 2.655(8) . ? Tb N1 2.678(8) . ? P1 O12 1.499(8) . ? P1 O11 1.514(8) . ? P1 C11 1.817(11) . ? P1 C10 1.830(11) . ? P2 O22 1.497(7) . ? P2 O21 1.528(7) . ? P2 C21 1.799(10) . ? P2 C20 1.838(10) . ? P3 O32 1.510(7) . ? P3 O31 1.510(7) . ? P3 C31 1.807(10) . ? P3 C30 1.826(9) . ? O32 Tb 2.247(7) 3_665 ? N1 C8 1.459(13) . ? N1 C1 1.456(13) . ? N1 C10 1.499(11) . ? N2 C2 1.461(12) . ? N2 C20 1.475(12) . ? N2 C3 1.500(12) . ? N3 C4 1.461(12) . ? N3 C30 1.492(12) . ? N3 C5 1.498(12) . ? N4 C6 1.459(13) . ? N4 C40 1.471(14) . ? N4 C7 1.492(13) . ? C1 C2 1.515(14) . ? C1 H011 0.9700 . ? C1 H012 0.9700 . ? C2 H021 0.9700 . ? C2 H022 0.9700 . ? C3 C4 1.512(14) . ? C3 H031 0.9700 . ? C3 H032 0.9700 . ? C4 H041 0.9700 . ? C4 H042 0.9700 . ? C5 C6 1.501(15) . ? C5 H051 0.9700 . ? C5 H052 0.9700 . ? C6 H061 0.9700 . ? C6 H062 0.9700 . ? C7 C8 1.523(14) . ? C7 H071 0.9700 . ? C7 H072 0.9700 . ? C8 H081 0.9700 . ? C8 H082 0.9700 . ? C11 C12 1.345(18) . ? C11 C16 1.411(17) . ? C12 C13 1.436(18) . ? C12 H12 0.9300 . ? C13 C14 1.37(2) . ? C13 H13 0.9300 . ? C14 C15 1.36(2) . ? C14 H14 0.9300 . ? C15 C16 1.36(2) . ? C15 H151 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.381(17) . ? C21 C22 1.415(17) . ? C22 C23 1.407(19) . ? C22 H22 0.9300 . ? C23 C24 1.42(3) . ? C23 H23 0.9300 . ? C24 C25 1.30(3) . ? C24 H24 0.9300 . ? C25 C26 1.373(19) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.392(16) . ? C31 C32 1.373(18) . ? C32 C33 1.422(19) . ? C32 H32 0.9300 . ? C33 C34 1.40(3) . ? C33 H33 0.9300 . ? C34 C35 1.38(2) . ? C34 H34 0.9300 . ? C35 C36 1.345(17) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C20 H201 0.9700 . ? C20 H202 0.9700 . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C40 H401 0.9600 . ? C40 H402 0.9600 . ? C40 H403 0.9600 . ? 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 QO Tb QN 175.20(4) . . ? QO Tb O32 62.08(18) . 3_665 ? QN Tb O32 120.76(18) . 3_665 ? QO Tb O21 59.64(17) . . ? QN Tb O21 117.22(17) . . ? O32 Tb O21 121.7(2) 3_665 . ? QO Tb O11 68.03(18) . . ? QN Tb O11 115.68(18) . . ? O32 Tb O11 81.0(3) 3_665 . ? O21 Tb O11 80.0(3) . . ? QO Tb O31 63.22(16) . . ? QN Tb O31 112.99(16) . . ? O32 Tb O31 77.0(2) 3_665 . ? O21 Tb O31 75.8(2) . . ? O11 Tb O31 131.2(2) . . ? QO Tb N2 123.00(16) . . ? QN Tb N2 52.50(16) . . ? O32 Tb N2 151.1(2) 3_665 . ? O21 Tb N2 69.7(2) . . ? O11 Tb N2 127.9(3) . . ? O31 Tb N2 81.2(2) . . ? QO Tb N4 132.86(18) . . ? QN Tb N4 51.60(17) . . ? O32 Tb N4 76.1(3) 3_665 . ? O21 Tb N4 154.5(2) . . ? O11 Tb N4 85.7(3) . . ? O31 Tb N4 128.8(2) . . ? N2 Tb N4 104.1(2) . . ? QO Tb N3 125.51(17) . . ? QN Tb N3 52.68(17) . . ? O32 Tb N3 85.7(3) 3_665 . ? O21 Tb N3 127.3(2) . . ? O11 Tb N3 152.5(3) . . ? O31 Tb N3 67.6(2) . . ? N2 Tb N3 68.4(3) . . ? N4 Tb N3 67.7(2) . . ? QO Tb N1 129.71(16) . . ? QN Tb N1 51.83(16) . . ? O32 Tb N1 134.1(2) 3_665 . ? O21 Tb N1 87.6(2) . . ? O11 Tb N1 69.5(2) . . ? O31 Tb N1 148.5(2) . . ? N2 Tb N1 67.8(2) . . ? N4 Tb N1 67.5(2) . . ? N3 Tb N1 104.5(2) . . ? O12 P1 O11 118.4(5) . . ? O12 P1 C11 108.0(5) . . ? O11 P1 C11 106.8(5) . . ? O12 P1 C10 107.6(5) . . ? O11 P1 C10 106.3(4) . . ? C11 P1 C10 109.5(5) . . ? P1 O11 Tb 124.9(4) . . ? O22 P2 O21 115.8(4) . . ? O22 P2 C21 107.2(4) . . ? O21 P2 C21 110.9(5) . . ? O22 P2 C20 110.9(5) . . ? O21 P2 C20 104.9(4) . . ? C21 P2 C20 106.9(5) . . ? P2 O21 Tb 125.6(3) . . ? O32 P3 O31 115.9(4) . . ? O32 P3 C31 106.7(4) . . ? O31 P3 C31 110.4(4) . . ? O32 P3 C30 108.8(4) . . ? O31 P3 C30 105.5(4) . . ? C31 P3 C30 109.6(5) . . ? P3 O31 Tb 124.4(4) . . ? P3 O32 Tb 161.3(5) . 3_665 ? C8 N1 C1 108.5(7) . . ? C8 N1 C10 108.8(8) . . ? C1 N1 C10 109.8(8) . . ? C8 N1 Tb 110.5(6) . . ? C1 N1 Tb 112.2(5) . . ? C10 N1 Tb 106.9(5) . . ? C2 N2 C20 110.8(8) . . ? C2 N2 C3 108.1(7) . . ? C20 N2 C3 110.3(8) . . ? C2 N2 Tb 110.5(6) . . ? C20 N2 Tb 106.2(5) . . ? C3 N2 Tb 110.8(6) . . ? C4 N3 C30 109.7(7) . . ? C4 N3 C5 110.5(7) . . ? C30 N3 C5 108.0(7) . . ? C4 N3 Tb 110.2(5) . . ? C30 N3 Tb 106.6(5) . . ? C5 N3 Tb 111.8(6) . . ? C6 N4 C40 106.5(8) . . ? C6 N4 C7 110.1(8) . . ? C40 N4 C7 107.2(8) . . ? C6 N4 Tb 109.5(6) . . ? C40 N4 Tb 112.1(6) . . ? C7 N4 Tb 111.3(6) . . ? N1 C1 C2 112.5(7) . . ? N1 C1 H011 109.1 . . ? C2 C1 H011 109.1 . . ? N1 C1 H012 109.1 . . ? C2 C1 H012 109.1 . . ? H011 C1 H012 107.8 . . ? N2 C2 C1 114.6(8) . . ? N2 C2 H021 108.6 . . ? C1 C2 H021 108.6 . . ? N2 C2 H022 108.6 . . ? C1 C2 H022 108.6 . . ? H021 C2 H022 107.6 . . ? N2 C3 C4 111.3(8) . . ? N2 C3 H031 109.4 . . ? C4 C3 H031 109.4 . . ? N2 C3 H032 109.4 . . ? C4 C3 H032 109.4 . . ? H031 C3 H032 108.0 . . ? N3 C4 C3 113.0(8) . . ? N3 C4 H041 109.0 . . ? C3 C4 H041 109.0 . . ? N3 C4 H042 109.0 . . ? C3 C4 H042 109.0 . . ? H041 C4 H042 107.8 . . ? C6 C5 N3 111.5(8) . . ? C6 C5 H051 109.3 . . ? N3 C5 H051 109.3 . . ? C6 C5 H052 109.3 . . ? N3 C5 H052 109.3 . . ? H051 C5 H052 108.0 . . ? N4 C6 C5 112.5(9) . . ? N4 C6 H061 109.1 . . ? C5 C6 H061 109.1 . . ? N4 C6 H062 109.1 . . ? C5 C6 H062 109.1 . . ? H061 C6 H062 107.8 . . ? N4 C7 C8 110.0(8) . . ? N4 C7 H071 109.7 . . ? C8 C7 H071 109.7 . . ? N4 C7 H072 109.7 . . ? C8 C7 H072 109.7 . . ? H071 C7 H072 108.2 . . ? N1 C8 C7 112.4(8) . . ? N1 C8 H081 109.1 . . ? C7 C8 H081 109.1 . . ? N1 C8 H082 109.1 . . ? C7 C8 H082 109.1 . . ? H081 C8 H082 107.9 . . ? C12 C11 C16 119.5(13) . . ? C12 C11 P1 121.4(9) . . ? C16 C11 P1 119.0(11) . . ? C11 C12 C13 120.1(13) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 118.5(15) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 121.2(14) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 120.5(16) . . ? C14 C15 H151 119.7 . . ? C16 C15 H151 119.7 . . ? C15 C16 C11 120.2(16) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C26 C21 C22 119.7(11) . . ? C26 C21 P2 120.4(9) . . ? C22 C21 P2 119.8(9) . . ? C23 C22 C21 118.1(15) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 117.9(15) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 122.9(15) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.6 . . ? C24 C25 C26 120.2(17) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.1(15) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C36 C31 C32 120.4(11) . . ? C36 C31 P3 118.5(8) . . ? C32 C31 P3 120.8(9) . . ? C31 C32 C33 118.5(15) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C34 C33 C32 119.5(16) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 119.8(12) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C34 120.2(15) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C31 121.3(13) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? N1 C10 P1 112.7(7) . . ? N1 C10 H101 109.1 . . ? P1 C10 H101 109.1 . . ? N1 C10 H102 109.0 . . ? P1 C10 H102 109.0 . . ? H101 C10 H102 107.8 . . ? N2 C20 P2 109.6(7) . . ? N2 C20 H201 109.8 . . ? P2 C20 H201 109.8 . . ? N2 C20 H202 109.7 . . ? P2 C20 H202 109.8 . . ? H201 C20 H202 108.2 . . ? N3 C30 P3 109.8(6) . . ? N3 C30 H301 109.7 . . ? P3 C30 H301 109.7 . . ? N3 C30 H302 109.7 . . ? P3 C30 H302 109.7 . . ? H301 C30 H302 108.2 . . ? N4 C40 H401 109.5 . . ? N4 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? N4 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 Tb 98.6(6) . . . . ? C11 P1 O11 Tb -139.3(5) . . . . ? C10 P1 O11 Tb -22.4(6) . . . . ? QO Tb O11 P1 -118.5(5) . . . . ? QN Tb O11 P1 58.2(6) . . . . ? O32 Tb O11 P1 178.1(6) 3_665 . . . ? O21 Tb O11 P1 -57.3(5) . . . . ? O31 Tb O11 P1 -118.2(5) . . . . ? N2 Tb O11 P1 -3.0(7) . . . . ? N4 Tb O11 P1 101.5(5) . . . . ? N3 Tb O11 P1 116.0(6) . . . . ? N1 Tb O11 P1 33.9(5) . . . . ? O22 P2 O21 Tb -133.5(5) . . . . ? C21 P2 O21 Tb 104.2(5) . . . . ? C20 P2 O21 Tb -10.9(6) . . . . ? QO Tb O21 P2 -124.7(5) . . . . ? QN Tb O21 P2 51.2(5) . . . . ? O32 Tb O21 P2 -122.2(5) 3_665 . . . ? O11 Tb O21 P2 165.0(5) . . . . ? O31 Tb O21 P2 -57.6(5) . . . . ? N2 Tb O21 P2 28.1(4) . . . . ? N4 Tb O21 P2 108.3(6) . . . . ? N3 Tb O21 P2 -11.1(6) . . . . ? N1 Tb O21 P2 95.4(5) . . . . ? O32 P3 O31 Tb 97.4(5) . . . . ? C31 P3 O31 Tb -141.2(5) . . . . ? C30 P3 O31 Tb -22.9(5) . . . . ? QO Tb O31 P3 -118.7(4) . . . . ? QN Tb O31 P3 64.6(4) . . . . ? O32 Tb O31 P3 -53.6(4) 3_665 . . . ? O21 Tb O31 P3 178.4(5) . . . . ? O11 Tb O31 P3 -119.0(5) . . . . ? N2 Tb O31 P3 107.3(4) . . . . ? N4 Tb O31 P3 6.2(6) . . . . ? N3 Tb O31 P3 37.1(4) . . . . ? N1 Tb O31 P3 118.2(5) . . . . ? O31 P3 O32 Tb -131.5(12) . . . 3_665 ? C31 P3 O32 Tb 105.2(13) . . . 3_665 ? C30 P3 O32 Tb -12.9(14) . . . 3_665 ? QO Tb N1 C8 114.0(6) . . . . ? QN Tb N1 C8 -71.8(6) . . . . ? O32 Tb N1 C8 26.5(8) 3_665 . . . ? O21 Tb N1 C8 160.2(6) . . . . ? O11 Tb N1 C8 80.0(6) . . . . ? O31 Tb N1 C8 -142.4(6) . . . . ? N2 Tb N1 C8 -130.7(7) . . . . ? N4 Tb N1 C8 -13.8(6) . . . . ? N3 Tb N1 C8 -71.7(6) . . . . ? QO Tb N1 C1 -124.7(6) . . . . ? QN Tb N1 C1 49.5(5) . . . . ? O32 Tb N1 C1 147.8(6) 3_665 . . . ? O21 Tb N1 C1 -78.5(6) . . . . ? O11 Tb N1 C1 -158.7(7) . . . . ? O31 Tb N1 C1 -21.1(8) . . . . ? N2 Tb N1 C1 -9.4(6) . . . . ? N4 Tb N1 C1 107.5(6) . . . . ? N3 Tb N1 C1 49.5(6) . . . . ? QO Tb N1 C10 -4.2(7) . . . . ? QN Tb N1 C10 169.9(7) . . . . ? O32 Tb N1 C10 -91.8(7) 3_665 . . . ? O21 Tb N1 C10 41.9(6) . . . . ? O11 Tb N1 C10 -38.2(6) . . . . ? O31 Tb N1 C10 99.3(7) . . . . ? N2 Tb N1 C10 111.0(6) . . . . ? N4 Tb N1 C10 -132.1(7) . . . . ? N3 Tb N1 C10 170.0(6) . . . . ? QO Tb N2 C2 106.1(6) . . . . ? QN Tb N2 C2 -75.9(6) . . . . ? O32 Tb N2 C2 -162.7(6) 3_665 . . . ? O21 Tb N2 C2 78.1(6) . . . . ? O11 Tb N2 C2 19.6(7) . . . . ? O31 Tb N2 C2 156.1(6) . . . . ? N4 Tb N2 C2 -75.9(6) . . . . ? N3 Tb N2 C2 -134.7(6) . . . . ? N1 Tb N2 C2 -17.8(6) . . . . ? QO Tb N2 C20 -14.2(6) . . . . ? QN Tb N2 C20 163.8(7) . . . . ? O32 Tb N2 C20 77.0(8) 3_665 . . . ? O21 Tb N2 C20 -42.2(6) . . . . ? O11 Tb N2 C20 -100.7(6) . . . . ? O31 Tb N2 C20 35.8(6) . . . . ? N4 Tb N2 C20 163.8(6) . . . . ? N3 Tb N2 C20 105.0(6) . . . . ? N1 Tb N2 C20 -138.1(6) . . . . ? QO Tb N2 C3 -134.0(5) . . . . ? QN Tb N2 C3 44.0(5) . . . . ? O32 Tb N2 C3 -42.8(8) 3_665 . . . ? O21 Tb N2 C3 -162.1(6) . . . . ? O11 Tb N2 C3 139.4(6) . . . . ? O31 Tb N2 C3 -84.1(6) . . . . ? N4 Tb N2 C3 43.9(6) . . . . ? N3 Tb N2 C3 -14.8(6) . . . . ? N1 Tb N2 C3 102.0(6) . . . . ? QO Tb N3 C4 101.3(6) . . . . ? QN Tb N3 C4 -73.2(5) . . . . ? O32 Tb N3 C4 152.2(6) 3_665 . . . ? O21 Tb N3 C4 25.0(7) . . . . ? O11 Tb N3 C4 -146.7(6) . . . . ? O31 Tb N3 C4 74.5(6) . . . . ? N2 Tb N3 C4 -14.7(5) . . . . ? N4 Tb N3 C4 -131.1(6) . . . . ? N1 Tb N3 C4 -73.2(6) . . . . ? QO Tb N3 C30 -17.6(6) . . . . ? QN Tb N3 C30 167.9(6) . . . . ? O32 Tb N3 C30 33.3(6) 3_665 . . . ? O21 Tb N3 C30 -93.9(6) . . . . ? O11 Tb N3 C30 94.4(7) . . . . ? O31 Tb N3 C30 -44.4(5) . . . . ? N2 Tb N3 C30 -133.6(6) . . . . ? N4 Tb N3 C30 110.0(6) . . . . ? N1 Tb N3 C30 167.8(5) . . . . ? QO Tb N3 C5 -135.4(6) . . . . ? QN Tb N3 C5 50.1(6) . . . . ? O32 Tb N3 C5 -84.5(7) 3_665 . . . ? O21 Tb N3 C5 148.3(6) . . . . ? O11 Tb N3 C5 -23.4(10) . . . . ? O31 Tb N3 C5 -162.1(7) . . . . ? N2 Tb N3 C5 108.7(7) . . . . ? N4 Tb N3 C5 -7.7(6) . . . . ? N1 Tb N3 C5 50.1(7) . . . . ? QO Tb N4 C6 96.9(6) . . . . ? QN Tb N4 C6 -80.8(6) . . . . ? O32 Tb N4 C6 69.5(6) 3_665 . . . ? O21 Tb N4 C6 -153.1(6) . . . . ? O11 Tb N4 C6 151.3(6) . . . . ? O31 Tb N4 C6 9.3(7) . . . . ? N2 Tb N4 C6 -80.8(6) . . . . ? N3 Tb N4 C6 -21.6(6) . . . . ? N1 Tb N4 C6 -139.1(7) . . . . ? QO Tb N4 C40 -21.1(8) . . . . ? QN Tb N4 C40 161.2(8) . . . . ? O32 Tb N4 C40 -48.5(7) 3_665 . . . ? O21 Tb N4 C40 89.0(8) . . . . ? O11 Tb N4 C40 33.3(7) . . . . ? O31 Tb N4 C40 -108.7(7) . . . . ? N2 Tb N4 C40 161.3(7) . . . . ? N3 Tb N4 C40 -139.5(7) . . . . ? N1 Tb N4 C40 102.9(7) . . . . ? QO Tb N4 C7 -141.1(6) . . . . ? QN Tb N4 C7 41.2(6) . . . . ? O32 Tb N4 C7 -168.6(7) 3_665 . . . ? O21 Tb N4 C7 -31.1(10) . . . . ? O11 Tb N4 C7 -86.8(6) . . . . ? O31 Tb N4 C7 131.3(6) . . . . ? N2 Tb N4 C7 41.2(7) . . . . ? N3 Tb N4 C7 100.4(7) . . . . ? N1 Tb N4 C7 -17.1(6) . . . . ? C8 N1 C1 C2 157.8(8) . . . . ? C10 N1 C1 C2 -83.4(10) . . . . ? Tb N1 C1 C2 35.3(10) . . . . ? C20 N2 C2 C1 162.3(8) . . . . ? C3 N2 C2 C1 -76.6(10) . . . . ? Tb N2 C2 C1 44.8(9) . . . . ? N1 C1 C2 N2 -56.1(11) . . . . ? C2 N2 C3 C4 164.4(8) . . . . ? C20 N2 C3 C4 -74.3(10) . . . . ? Tb N2 C3 C4 43.1(9) . . . . ? C30 N3 C4 C3 160.9(8) . . . . ? C5 N3 C4 C3 -80.2(9) . . . . ? Tb N3 C4 C3 43.9(8) . . . . ? N2 C3 C4 N3 -60.8(10) . . . . ? C4 N3 C5 C6 159.3(8) . . . . ? C30 N3 C5 C6 -80.7(10) . . . . ? Tb N3 C5 C6 36.2(10) . . . . ? C40 N4 C6 C5 172.2(8) . . . . ? C7 N4 C6 C5 -71.9(11) . . . . ? Tb N4 C6 C5 50.7(9) . . . . ? N3 C5 C6 N4 -60.5(11) . . . . ? C6 N4 C7 C8 167.6(8) . . . . ? C40 N4 C7 C8 -76.9(11) . . . . ? Tb N4 C7 C8 46.0(10) . . . . ? C1 N1 C8 C7 -79.5(10) . . . . ? C10 N1 C8 C7 161.1(9) . . . . ? Tb N1 C8 C7 44.0(10) . . . . ? N4 C7 C8 N1 -62.5(12) . . . . ? O12 P1 C11 C12 118.0(10) . . . . ? O11 P1 C11 C12 -10.4(11) . . . . ? C10 P1 C11 C12 -125.1(10) . . . . ? O12 P1 C11 C16 -57.8(11) . . . . ? O11 P1 C11 C16 173.8(9) . . . . ? C10 P1 C11 C16 59.1(11) . . . . ? C16 C11 C12 C13 -0.1(18) . . . . ? P1 C11 C12 C13 -175.9(9) . . . . ? C11 C12 C13 C14 2.3(19) . . . . ? C12 C13 C14 C15 -4(2) . . . . ? C13 C14 C15 C16 3(3) . . . . ? C14 C15 C16 C11 0(3) . . . . ? C12 C11 C16 C15 -1(2) . . . . ? P1 C11 C16 C15 175.0(13) . . . . ? O22 P2 C21 C26 54.1(10) . . . . ? O21 P2 C21 C26 -178.7(8) . . . . ? C20 P2 C21 C26 -64.9(10) . . . . ? O22 P2 C21 C22 -121.7(8) . . . . ? O21 P2 C21 C22 5.5(10) . . . . ? C20 P2 C21 C22 119.4(9) . . . . ? C26 C21 C22 C23 0.1(17) . . . . ? P2 C21 C22 C23 175.9(10) . . . . ? C21 C22 C23 C24 -2(2) . . . . ? C22 C23 C24 C25 4(3) . . . . ? C23 C24 C25 C26 -3(3) . . . . ? C24 C25 C26 C21 1(2) . . . . ? C22 C21 C26 C25 0.3(17) . . . . ? P2 C21 C26 C25 -175.4(10) . . . . ? O32 P3 C31 C36 94.3(9) . . . . ? O31 P3 C31 C36 -32.3(9) . . . . ? C30 P3 C31 C36 -148.1(8) . . . . ? O32 P3 C31 C32 -79.4(10) . . . . ? O31 P3 C31 C32 154.0(9) . . . . ? C30 P3 C31 C32 38.2(10) . . . . ? C36 C31 C32 C33 0.2(18) . . . . ? P3 C31 C32 C33 173.8(10) . . . . ? C31 C32 C33 C34 -4(2) . . . . ? C32 C33 C34 C35 5(2) . . . . ? C33 C34 C35 C36 -1(2) . . . . ? C34 C35 C36 C31 -3(2) . . . . ? C32 C31 C36 C35 3.8(18) . . . . ? P3 C31 C36 C35 -169.9(10) . . . . ? C8 N1 C10 P1 -79.7(9) . . . . ? C1 N1 C10 P1 161.8(6) . . . . ? Tb N1 C10 P1 39.8(8) . . . . ? O12 P1 C10 N1 -144.9(7) . . . . ? O11 P1 C10 N1 -17.1(8) . . . . ? C11 P1 C10 N1 98.0(8) . . . . ? C2 N2 C20 P2 -70.7(9) . . . . ? C3 N2 C20 P2 169.6(7) . . . . ? Tb N2 C20 P2 49.4(7) . . . . ? O22 P2 C20 N2 95.8(7) . . . . ? O21 P2 C20 N2 -29.9(8) . . . . ? C21 P2 C20 N2 -147.7(7) . . . . ? C4 N3 C30 P3 -72.4(8) . . . . ? C5 N3 C30 P3 167.1(6) . . . . ? Tb N3 C30 P3 46.9(6) . . . . ? O32 P3 C30 N3 -146.2(6) . . . . ? O31 P3 C30 N3 -21.3(7) . . . . ? C31 P3 C30 N3 97.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 24.01 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 4.362 _refine_diff_density_min -4.372 _refine_diff_density_rms 0.306 data_er16e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[ErL]2*10H2O (!centrosymmetric dimer!)' _chemical_formula_sum 'C30 H50 Er N4 O11 P3' _chemical_formula_weight 902.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no. 14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.048(16) _cell_length_b 19.56(6) _cell_length_c 16.535(15) _cell_angle_alpha 90.00 _cell_angle_beta 111.32(9) _cell_angle_gamma 90.00 _cell_volume 3932(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 2.314 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min -- _exptl_absorpt_correction_T_max -- _exptl_special_details ; crystal coated by thin paraphine film due to a loss of solvate molecules ; _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 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method '.omega.-2.theta.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 12.8 _diffrn_reflns_number 4806 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 21.99 _reflns_number_total 4806 _reflns_number_gt 3698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 program packet ' _computing_cell_refinement 'CAD4 program packet ' _computing_data_reduction 'JANA-98 (Petricek, 1998) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.1231P)^2^+187.2630P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson + Fourier ' _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 4806 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.2947 _refine_ls_wR_factor_gt 0.2516 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 4.136 _refine_ls_shift/su_mean 0.029 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er Er 0.66195(7) 0.61325(5) 0.01445(6) 0.0346(4) Uani 1 d . . . P1 P 0.8891(5) 0.6505(4) 0.1894(4) 0.0533(17) Uani 1 d . . . P2 P 0.5564(5) 0.7610(4) 0.0602(5) 0.0522(17) Uani 1 d . . . P3 P 0.3980(4) 0.5585(3) -0.0795(4) 0.0396(14) Uani 1 d . . . O11 O 0.8036(12) 0.5990(8) 0.1415(10) 0.049(4) Uani 1 d . . . O12 O 0.8765(14) 0.6878(10) 0.2634(11) 0.069(5) Uani 1 d . . . O21 O 0.6293(12) 0.6990(7) 0.0935(10) 0.047(4) Uani 1 d . . . O22 O 0.6040(16) 0.8287(10) 0.0930(14) 0.083(6) Uani 1 d . . . O31 O 0.4769(11) 0.6105(5) -0.0161(7) 0.027(3) Uani 1 d . . . O32 O 0.3680(9) 0.4944(7) -0.0420(9) 0.036(3) Uani 1 d . . . N1 N 0.8354(14) 0.6850(10) 0.0165(13) 0.048(5) Uani 1 d . . . N2 N 0.6099(16) 0.7229(9) -0.0789(12) 0.046(5) Uani 1 d . . . N3 N 0.5538(15) 0.5852(11) -0.1493(12) 0.051(5) Uani 1 d . . . N4 N 0.7841(15) 0.5424(11) -0.0519(13) 0.050(5) Uani 1 d . . . C1 C 0.8094(19) 0.7391(13) -0.0497(18) 0.055(7) Uani 1 d . . . H011 H 0.8031 0.7202 -0.1056 0.066 Uiso 1 calc R . . H012 H 0.8663 0.7738 -0.0335 0.066 Uiso 1 calc R . . C2 C 0.703(2) 0.7682(12) -0.053(2) 0.062(8) Uani 1 d . . . H021 H 0.7130 0.7865 0.0034 0.075 Uiso 1 calc R . . H022 H 0.6856 0.8064 -0.0937 0.075 Uiso 1 calc R . . C3 C 0.571(2) 0.7066(15) -0.1719(16) 0.062(7) Uani 1 d . . . H031 H 0.6342 0.6977 -0.1880 0.074 Uiso 1 calc R . . H032 H 0.5332 0.7463 -0.2045 0.074 Uiso 1 calc R . . C4 C 0.4955(18) 0.6468(13) -0.1975(15) 0.050(6) Uani 1 d . . . H041 H 0.4303 0.6556 -0.1840 0.060 Uiso 1 calc R . . H042 H 0.4727 0.6391 -0.2595 0.060 Uiso 1 calc R . . C5 C 0.6262(17) 0.5532(13) -0.1928(15) 0.049(6) Uani 1 d . . . H051 H 0.5812 0.5273 -0.2431 0.059 Uiso 1 calc R . . H052 H 0.6634 0.5889 -0.2123 0.059 Uiso 1 calc R . . C6 C 0.7102(19) 0.5068(15) -0.1303(17) 0.062(8) Uani 1 d . . . H061 H 0.6722 0.4705 -0.1127 0.075 Uiso 1 calc R . . H062 H 0.7542 0.4859 -0.1599 0.075 Uiso 1 calc R . . C7 C 0.8650(16) 0.5896(14) -0.0722(17) 0.056(7) Uani 1 d . . . H071 H 0.9202 0.5626 -0.0840 0.067 Uiso 1 calc R . . H072 H 0.8261 0.6167 -0.1233 0.067 Uiso 1 calc R . . C8 C 0.9177(19) 0.6345(13) 0.0015(19) 0.061(7) Uani 1 d . . . H081 H 0.9756 0.6601 -0.0086 0.073 Uiso 1 calc R . . H082 H 0.9512 0.6071 0.0533 0.073 Uiso 1 calc R . . C10 C 0.8853(18) 0.7133(12) 0.1047(15) 0.046(6) Uani 1 d . . . H101 H 0.8436 0.7531 0.1098 0.055 Uiso 1 calc R . . H102 H 0.9597 0.7282 0.1141 0.055 Uiso 1 calc R . . C11 C 1.0219(19) 0.6106(13) 0.2317(16) 0.052(6) Uani 1 d . . . C12 C 1.026(2) 0.5392(16) 0.2388(18) 0.068(8) Uani 1 d . . . H12 H 0.9624 0.5134 0.2159 0.081 Uiso 1 calc R . . C13 C 1.131(3) 0.506(2) 0.282(2) 0.090(11) Uani 1 d . . . H13 H 1.1369 0.4585 0.2850 0.108 Uiso 1 calc R . . C14 C 1.221(2) 0.548(3) 0.318(2) 0.108(16) Uani 1 d . . . H14 H 1.2887 0.5277 0.3496 0.129 Uiso 1 calc R . . C15 C 1.215(3) 0.616(2) 0.310(2) 0.089(11) Uani 1 d . . . H15 H 1.2788 0.6423 0.3340 0.107 Uiso 1 calc R . . C16 C 1.118(2) 0.648(2) 0.268(2) 0.097(12) Uani 1 d . . . H16 H 1.1158 0.6958 0.2636 0.117 Uiso 1 calc R . . C20 C 0.5164(19) 0.7556(12) -0.0600(16) 0.054(7) Uani 1 d . . . H201 H 0.4501 0.7284 -0.0848 0.064 Uiso 1 calc R . . H202 H 0.5020 0.8009 -0.0853 0.064 Uiso 1 calc R . . C21 C 0.4299(19) 0.7517(14) 0.0811(17) 0.054(7) Uani 1 d . . . C22 C 0.355(3) 0.805(2) 0.062(2) 0.098(12) Uani 1 d . . . H22 H 0.3686 0.8429 0.0340 0.117 Uiso 1 calc R . . C23 C 0.265(2) 0.805(3) 0.081(3) 0.133(18) Uani 1 d . . . H23 H 0.2185 0.8426 0.0687 0.160 Uiso 1 calc R . . C24 C 0.243(3) 0.743(3) 0.123(3) 0.113(15) Uani 1 d . . . H24 H 0.1781 0.7380 0.1334 0.135 Uiso 1 calc R . . C25 C 0.321(3) 0.693(3) 0.145(3) 0.136(19) Uani 1 d . . . H25 H 0.3113 0.6551 0.1755 0.163 Uiso 1 calc R . . C26 C 0.410(2) 0.6956(17) 0.1259(19) 0.076(9) Uani 1 d . . . H26 H 0.4605 0.6599 0.1422 0.091 Uiso 1 calc R . . C30 C 0.4684(17) 0.5324(12) -0.1529(14) 0.042(5) Uani 1 d . . . H301 H 0.5032 0.4882 -0.1353 0.050 Uiso 1 calc R . . H302 H 0.4156 0.5284 -0.2118 0.050 Uiso 1 calc R . . C31 C 0.2731(17) 0.6005(12) -0.1424(15) 0.045(6) Uani 1 d . . . C32 C 0.206(2) 0.5797(15) -0.2255(19) 0.063(7) Uani 1 d . . . H32 H 0.2294 0.5455 -0.2536 0.075 Uiso 1 calc R . . C33 C 0.106(2) 0.609(2) -0.266(2) 0.096(12) Uani 1 d . . . H33 H 0.0614 0.5940 -0.3206 0.115 Uiso 1 calc R . . C34 C 0.068(3) 0.661(2) -0.227(3) 0.092(11) Uani 1 d . . . H34 H -0.0007 0.6805 -0.2545 0.110 Uiso 1 calc R . . C35 C 0.135(2) 0.6830(16) -0.146(2) 0.077(9) Uani 1 d . . . H35 H 0.1114 0.7182 -0.1189 0.093 Uiso 1 calc R . . C36 C 0.2378(19) 0.6541(14) -0.1026(19) 0.063(7) Uani 1 d . . . H36 H 0.2825 0.6700 -0.0483 0.075 Uiso 1 calc R . . C40 C 0.848(2) 0.4892(13) 0.005(2) 0.067(8) Uani 1 d . . . H401 H 0.8982 0.5094 0.0575 0.101 Uiso 1 calc R . . H402 H 0.8894 0.4648 -0.0235 0.101 Uiso 1 calc R . . H403 H 0.8001 0.4582 0.0188 0.101 Uiso 1 calc R . . O99 O 0.665(3) 0.620(2) 0.260(2) 0.18(2) Uani 1.00(8) d . . . O98 O 0.561(6) 0.945(2) -0.012(4) 0.29(5) Uani 0.95(10) d P . . O97 O 0.957(17) 0.614(8) 0.430(8) 0.9(2) Uani 1.0(2) d . . . O96 O 0.790(2) 0.8226(13) 0.2405(15) 0.102(11) Uani 1.00(6) d . . . O95 O 0.498(4) 0.589(3) 0.316(3) 0.13(3) Uani 0.56(7) d P . . QN N 0.6960 0.6338 -0.0659 0.050 Uiso 0.00 d P . . QO O 0.6355 0.6035 0.0653 0.050 Uiso 0.00 d P . . 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 Er 0.0253(6) 0.0408(7) 0.0429(6) 0.0005(5) 0.0185(4) -0.0006(4) P1 0.032(3) 0.076(5) 0.055(4) -0.007(4) 0.019(3) -0.002(3) P2 0.036(3) 0.060(4) 0.070(4) -0.005(3) 0.031(3) 0.006(3) P3 0.014(3) 0.062(4) 0.046(3) 0.001(3) 0.014(2) 0.003(3) O11 0.030(8) 0.061(11) 0.063(10) 0.000(8) 0.024(8) -0.007(7) O12 0.052(11) 0.097(15) 0.061(11) -0.015(10) 0.023(9) -0.011(10) O21 0.055(10) 0.035(9) 0.058(10) -0.016(7) 0.028(8) 0.001(7) O22 0.071(13) 0.065(13) 0.113(16) -0.019(12) 0.033(12) 0.019(10) O31 0.062(9) 0.000(6) 0.013(6) -0.004(5) 0.006(6) 0.003(6) O32 0.011(6) 0.042(8) 0.056(9) 0.013(7) 0.013(6) 0.006(6) N1 0.028(10) 0.051(12) 0.067(13) 0.006(10) 0.020(9) -0.009(9) N2 0.056(12) 0.043(11) 0.050(12) 0.006(9) 0.031(10) 0.000(10) N3 0.033(10) 0.080(15) 0.054(12) -0.010(11) 0.032(10) -0.010(10) N4 0.034(11) 0.072(14) 0.056(12) -0.001(11) 0.029(10) 0.010(10) C1 0.047(14) 0.050(15) 0.082(18) 0.025(14) 0.040(13) 0.005(12) C2 0.058(16) 0.044(15) 0.11(2) 0.013(14) 0.059(16) -0.007(13) C3 0.058(16) 0.09(2) 0.051(16) 0.016(14) 0.031(13) 0.001(15) C4 0.030(12) 0.078(18) 0.042(13) 0.019(13) 0.012(10) 0.013(12) C5 0.030(12) 0.074(17) 0.053(14) -0.018(13) 0.027(11) -0.008(12) C6 0.035(13) 0.09(2) 0.068(17) -0.042(16) 0.033(13) -0.006(14) C7 0.011(10) 0.09(2) 0.086(19) 0.026(16) 0.042(12) 0.012(12) C8 0.026(13) 0.062(17) 0.09(2) 0.001(15) 0.021(13) 0.020(12) C10 0.035(12) 0.048(14) 0.061(15) -0.015(12) 0.026(11) -0.011(11) C11 0.040(15) 0.058(16) 0.063(16) 0.007(13) 0.027(12) -0.006(12) C12 0.031(14) 0.10(2) 0.073(19) 0.007(17) 0.023(13) -0.010(14) C13 0.07(2) 0.12(3) 0.08(2) 0.03(2) 0.029(19) 0.05(2) C14 0.030(17) 0.24(5) 0.050(18) -0.03(3) 0.006(14) 0.02(3) C15 0.06(2) 0.11(3) 0.09(3) -0.02(2) 0.024(18) 0.00(2) C16 0.032(17) 0.15(3) 0.09(2) -0.03(2) 0.005(15) 0.009(19) C20 0.045(14) 0.039(14) 0.074(17) 0.011(12) 0.017(13) 0.024(11) C21 0.039(14) 0.067(17) 0.072(17) -0.008(14) 0.039(13) 0.012(13) C22 0.08(2) 0.15(4) 0.07(2) 0.02(2) 0.041(18) 0.02(2) C23 0.027(17) 0.19(5) 0.19(5) 0.05(4) 0.05(2) 0.04(2) C24 0.06(2) 0.19(5) 0.13(3) -0.02(3) 0.08(2) 0.02(3) C25 0.10(3) 0.24(6) 0.10(3) -0.04(3) 0.07(3) -0.07(4) C26 0.056(18) 0.11(3) 0.09(2) -0.001(19) 0.051(17) 0.032(17) C30 0.038(13) 0.051(14) 0.040(13) -0.013(11) 0.018(10) 0.006(11) C31 0.021(11) 0.064(16) 0.054(15) 0.006(12) 0.017(11) -0.005(11) C32 0.040(16) 0.073(19) 0.08(2) -0.001(15) 0.031(15) -0.019(14) C33 0.030(17) 0.14(3) 0.09(2) 0.03(2) -0.012(16) -0.024(19) C34 0.045(19) 0.11(3) 0.12(3) 0.05(2) 0.02(2) 0.01(2) C35 0.059(19) 0.08(2) 0.10(3) 0.006(19) 0.044(19) 0.007(17) C36 0.037(14) 0.068(18) 0.09(2) 0.013(16) 0.035(14) 0.016(13) C40 0.061(17) 0.051(16) 0.11(2) 0.001(15) 0.057(17) 0.015(14) O99 0.12(3) 0.31(6) 0.14(3) -0.03(3) 0.09(2) -0.01(3) O98 0.48(11) 0.08(3) 0.28(7) 0.01(3) 0.10(6) 0.04(4) O97 1.7(5) 0.9(3) 0.44(17) 0.11(15) 0.7(3) 0.6(3) O96 0.11(2) 0.12(2) 0.098(18) -0.011(14) 0.062(15) -0.009(15) O95 0.09(4) 0.19(6) 0.14(5) -0.05(4) 0.05(3) -0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er QO 1.0357(12) . ? Er QN 1.5971(16) . ? Er O32 2.220(15) 3_665 ? Er O11 2.254(16) . ? Er O21 2.261(14) . ? Er O31 2.280(14) . ? Er N2 2.584(19) . ? Er N3 2.616(19) . ? Er N4 2.634(18) . ? Er N1 2.652(17) . ? P1 O12 1.483(19) . ? P1 O11 1.498(17) . ? P1 C11 1.80(2) . ? P1 C10 1.85(2) . ? P2 O22 1.48(2) . ? P2 O21 1.516(16) . ? P2 C21 1.81(2) . ? P2 C20 1.86(3) . ? P3 O32 1.512(15) . ? P3 O31 1.552(13) . ? P3 C31 1.78(2) . ? P3 C30 1.84(2) . ? O32 Er 2.220(15) 3_665 ? N1 C1 1.47(3) . ? N1 C10 1.47(3) . ? N1 C8 1.54(3) . ? N2 C2 1.44(3) . ? N2 C3 1.47(3) . ? N2 C20 1.51(3) . ? N3 C4 1.49(3) . ? N3 C30 1.50(3) . ? N3 C5 1.52(3) . ? N4 C40 1.45(3) . ? N4 C6 1.48(3) . ? N4 C7 1.53(3) . ? C1 C2 1.48(3) . ? C1 H011 0.9700 . ? C1 H012 0.9700 . ? C2 H021 0.9700 . ? C2 H022 0.9700 . ? C3 C4 1.49(3) . ? C3 H031 0.9700 . ? C3 H032 0.9700 . ? C4 H041 0.9700 . ? C4 H042 0.9700 . ? C5 C6 1.51(4) . ? C5 H051 0.9700 . ? C5 H052 0.9700 . ? C6 H061 0.9700 . ? C6 H062 0.9700 . ? C7 C8 1.46(4) . ? C7 H071 0.9700 . ? C7 H072 0.9700 . ? C8 H081 0.9700 . ? C8 H082 0.9700 . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C11 C16 1.39(4) . ? C11 C12 1.40(4) . ? C12 C13 1.44(4) . ? C12 H12 0.9300 . ? C13 C14 1.38(5) . ? C13 H13 0.9300 . ? C14 C15 1.35(5) . ? C14 H14 0.9300 . ? C15 C16 1.36(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C20 H201 0.9700 . ? C20 H202 0.9700 . ? C21 C22 1.38(4) . ? C21 C26 1.40(4) . ? C22 C23 1.31(4) . ? C22 H22 0.9300 . ? C23 C24 1.48(6) . ? C23 H23 0.9300 . ? C24 C25 1.36(6) . ? C24 H24 0.9300 . ? C25 C26 1.31(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 C32 1.40(4) . ? C31 C36 1.40(4) . ? C32 C33 1.36(4) . ? C32 H32 0.9300 . ? C33 C34 1.38(5) . ? C33 H33 0.9300 . ? C34 C35 1.38(5) . ? C34 H34 0.9300 . ? C35 C36 1.39(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C40 H401 0.9600 . ? C40 H402 0.9600 . ? C40 H403 0.9600 . ? 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 QO Er QN 175.12(8) . . ? QO Er O32 61.5(4) . 3_665 ? QN Er O32 122.2(4) . 3_665 ? QO Er O11 67.9(4) . . ? QN Er O11 115.1(4) . . ? O32 Er O11 80.6(5) 3_665 . ? QO Er O21 58.6(4) . . ? QN Er O21 117.5(4) . . ? O32 Er O21 120.1(5) 3_665 . ? O11 Er O21 79.4(6) . . ? QO Er O31 62.4(3) . . ? QN Er O31 114.4(3) . . ? O32 Er O31 76.8(4) 3_665 . ? O11 Er O31 130.3(5) . . ? O21 Er O31 74.8(5) . . ? QO Er N2 123.0(4) . . ? QN Er N2 52.2(4) . . ? O32 Er N2 151.9(6) 3_665 . ? O11 Er N2 127.4(6) . . ? O21 Er N2 70.5(6) . . ? O31 Er N2 81.9(5) . . ? QO Er N3 126.0(4) . . ? QN Er N3 53.2(4) . . ? O32 Er N3 86.8(6) 3_665 . ? O11 Er N3 152.8(6) . . ? O21 Er N3 127.6(6) . . ? O31 Er N3 68.7(5) . . ? N2 Er N3 68.3(6) . . ? QO Er N4 132.2(5) . . ? QN Er N4 52.7(5) . . ? O32 Er N4 76.4(6) 3_665 . ? O11 Er N4 84.7(6) . . ? O21 Er N4 154.3(6) . . ? O31 Er N4 130.4(5) . . ? N2 Er N4 104.8(6) . . ? N3 Er N4 68.8(6) . . ? QO Er N1 128.4(5) . . ? QN Er N1 51.9(4) . . ? O32 Er N1 135.4(5) 3_665 . ? O11 Er N1 69.3(6) . . ? O21 Er N1 86.5(6) . . ? O31 Er N1 147.7(5) . . ? N2 Er N1 66.8(6) . . ? N3 Er N1 105.1(6) . . ? N4 Er N1 69.0(6) . . ? O12 P1 O11 118.9(10) . . ? O12 P1 C11 105.9(11) . . ? O11 P1 C11 109.9(11) . . ? O12 P1 C10 108.5(11) . . ? O11 P1 C10 103.7(10) . . ? C11 P1 C10 109.9(11) . . ? O22 P2 O21 117.3(10) . . ? O22 P2 C21 108.0(12) . . ? O21 P2 C21 110.2(11) . . ? O22 P2 C20 111.0(12) . . ? O21 P2 C20 103.8(9) . . ? C21 P2 C20 106.0(12) . . ? O32 P3 O31 118.3(8) . . ? O32 P3 C31 107.6(9) . . ? O31 P3 C31 109.5(10) . . ? O32 P3 C30 107.8(10) . . ? O31 P3 C30 105.1(9) . . ? C31 P3 C30 108.2(11) . . ? P1 O11 Er 127.6(10) . . ? P2 O21 Er 127.5(9) . . ? P3 O31 Er 123.6(7) . . ? P3 O32 Er 164.2(9) . 3_665 ? C1 N1 C10 111(2) . . ? C1 N1 C8 109.0(19) . . ? C10 N1 C8 108.5(18) . . ? C1 N1 Er 114.0(13) . . ? C10 N1 Er 106.3(12) . . ? C8 N1 Er 107.5(14) . . ? C2 N2 C3 111.9(19) . . ? C2 N2 C20 109.9(19) . . ? C3 N2 C20 108.1(19) . . ? C2 N2 Er 109.1(15) . . ? C3 N2 Er 111.2(15) . . ? C20 N2 Er 106.6(13) . . ? C4 N3 C30 107.9(17) . . ? C4 N3 C5 111.4(18) . . ? C30 N3 C5 106.2(18) . . ? C4 N3 Er 111.2(14) . . ? C30 N3 Er 107.4(12) . . ? C5 N3 Er 112.5(13) . . ? C40 N4 C6 106(2) . . ? C40 N4 C7 107.1(17) . . ? C6 N4 C7 112.0(19) . . ? C40 N4 Er 113.8(14) . . ? C6 N4 Er 108.2(12) . . ? C7 N4 Er 110.1(14) . . ? N1 C1 C2 105.5(18) . . ? N1 C1 H011 110.6 . . ? C2 C1 H011 110.6 . . ? N1 C1 H012 110.6 . . ? C2 C1 H012 110.6 . . ? H011 C1 H012 108.8 . . ? N2 C2 C1 117(2) . . ? N2 C2 H021 108.0 . . ? C1 C2 H021 108.0 . . ? N2 C2 H022 108.1 . . ? C1 C2 H022 108.1 . . ? H021 C2 H022 107.3 . . ? N2 C3 C4 114.1(19) . . ? N2 C3 H031 108.7 . . ? C4 C3 H031 108.7 . . ? N2 C3 H032 108.7 . . ? C4 C3 H032 108.7 . . ? H031 C3 H032 107.6 . . ? N3 C4 C3 109.1(19) . . ? N3 C4 H041 109.9 . . ? C3 C4 H041 109.9 . . ? N3 C4 H042 109.9 . . ? C3 C4 H042 109.9 . . ? H041 C4 H042 108.3 . . ? C6 C5 N3 110.3(19) . . ? C6 C5 H051 109.6 . . ? N3 C5 H051 109.6 . . ? C6 C5 H052 109.6 . . ? N3 C5 H052 109.6 . . ? H051 C5 H052 108.1 . . ? N4 C6 C5 113(2) . . ? N4 C6 H061 108.9 . . ? C5 C6 H061 108.9 . . ? N4 C6 H062 108.9 . . ? C5 C6 H062 108.9 . . ? H061 C6 H062 107.7 . . ? C8 C7 N4 110(2) . . ? C8 C7 H071 109.8 . . ? N4 C7 H071 109.8 . . ? C8 C7 H072 109.8 . . ? N4 C7 H072 109.8 . . ? H071 C7 H072 108.2 . . ? C7 C8 N1 112.1(19) . . ? C7 C8 H081 109.2 . . ? N1 C8 H081 109.2 . . ? C7 C8 H082 109.2 . . ? N1 C8 H082 109.2 . . ? H081 C8 H082 107.9 . . ? N1 C10 P1 112.3(15) . . ? N1 C10 H101 109.2 . . ? P1 C10 H101 109.1 . . ? N1 C10 H102 109.1 . . ? P1 C10 H102 109.1 . . ? H101 C10 H102 107.9 . . ? C16 C11 C12 119(3) . . ? C16 C11 P1 122(2) . . ? C12 C11 P1 118.1(18) . . ? C11 C12 C13 120(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 117(4) . . ? C14 C13 H13 121.5 . . ? C12 C13 H13 121.6 . . ? C15 C14 C13 122(3) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C16 121(4) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 120(4) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? N2 C20 P2 108.1(15) . . ? N2 C20 H201 110.1 . . ? P2 C20 H201 110.1 . . ? N2 C20 H202 110.1 . . ? P2 C20 H202 110.1 . . ? H201 C20 H202 108.4 . . ? C22 C21 C26 117(2) . . ? C22 C21 P2 120(2) . . ? C26 C21 P2 122.4(19) . . ? C23 C22 C21 125(4) . . ? C23 C22 H22 117.7 . . ? C21 C22 H22 117.7 . . ? C22 C23 C24 117(4) . . ? C22 C23 H23 121.6 . . ? C24 C23 H23 121.6 . . ? C25 C24 C23 117(3) . . ? C25 C24 H24 121.4 . . ? C23 C24 H24 121.3 . . ? C26 C25 C24 123(5) . . ? C26 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C25 C26 C21 121(4) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? N3 C30 P3 108.8(14) . . ? N3 C30 H301 109.9 . . ? P3 C30 H301 109.9 . . ? N3 C30 H302 109.9 . . ? P3 C30 H302 109.9 . . ? H301 C30 H302 108.3 . . ? C32 C31 C36 119(2) . . ? C32 C31 P3 124(2) . . ? C36 C31 P3 117.2(19) . . ? C33 C32 C31 121(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 121(3) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 118(3) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C34 C35 C36 122(3) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 119(3) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.4 . . ? N4 C40 H401 109.5 . . ? N4 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? N4 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 Er 99.4(14) . . . . ? C11 P1 O11 Er -138.4(11) . . . . ? C10 P1 O11 Er -21.0(13) . . . . ? QO Er O11 P1 -116.5(11) . . . . ? QN Er O11 P1 59.2(12) . . . . ? O32 Er O11 P1 -179.5(12) 3_665 . . . ? O21 Er O11 P1 -56.3(11) . . . . ? O31 Er O11 P1 -115.7(10) . . . . ? N2 Er O11 P1 -1.1(14) . . . . ? N3 Er O11 P1 116.8(14) . . . . ? N4 Er O11 P1 103.5(11) . . . . ? N1 Er O11 P1 34.0(10) . . . . ? O22 P2 O21 Er -130.2(13) . . . . ? C21 P2 O21 Er 105.7(13) . . . . ? C20 P2 O21 Er -7.3(14) . . . . ? QO Er O21 P2 -127.2(12) . . . . ? QN Er O21 P2 49.4(12) . . . . ? O32 Er O21 P2 -125.1(10) 3_665 . . . ? O11 Er O21 P2 162.3(12) . . . . ? O31 Er O21 P2 -60.6(11) . . . . ? N2 Er O21 P2 26.1(10) . . . . ? N3 Er O21 P2 -13.7(14) . . . . ? N4 Er O21 P2 109.7(15) . . . . ? N1 Er O21 P2 92.7(11) . . . . ? O32 P3 O31 Er 96.0(9) . . . . ? C31 P3 O31 Er -140.3(9) . . . . ? C30 P3 O31 Er -24.3(11) . . . . ? QO Er O31 P3 -118.2(8) . . . . ? QN Er O31 P3 66.0(8) . . . . ? O32 Er O31 P3 -53.7(8) 3_665 . . . ? O11 Er O31 P3 -119.0(8) . . . . ? O21 Er O31 P3 179.7(9) . . . . ? N2 Er O31 P3 107.9(9) . . . . ? N3 Er O31 P3 38.1(8) . . . . ? N4 Er O31 P3 5.2(11) . . . . ? N1 Er O31 P3 122.8(10) . . . . ? O31 P3 O32 Er -129(3) . . . 3_665 ? C31 P3 O32 Er 107(3) . . . 3_665 ? C30 P3 O32 Er -10(3) . . . 3_665 ? QO Er N1 C1 -126.9(15) . . . . ? QN Er N1 C1 46.9(15) . . . . ? O32 Er N1 C1 146.7(15) 3_665 . . . ? O11 Er N1 C1 -162.4(18) . . . . ? O21 Er N1 C1 -82.5(17) . . . . ? O31 Er N1 C1 -28(2) . . . . ? N2 Er N1 C1 -12.3(15) . . . . ? N3 Er N1 C1 45.6(17) . . . . ? N4 Er N1 C1 105.3(17) . . . . ? QO Er N1 C10 -3.8(16) . . . . ? QN Er N1 C10 170.0(16) . . . . ? O32 Er N1 C10 -90.2(15) 3_665 . . . ? O11 Er N1 C10 -39.3(13) . . . . ? O21 Er N1 C10 40.6(14) . . . . ? O31 Er N1 C10 94.8(15) . . . . ? N2 Er N1 C10 110.9(15) . . . . ? N3 Er N1 C10 168.7(13) . . . . ? N4 Er N1 C10 -131.6(15) . . . . ? QO Er N1 C8 112.2(14) . . . . ? QN Er N1 C8 -74.0(15) . . . . ? O32 Er N1 C8 25.8(18) 3_665 . . . ? O11 Er N1 C8 76.7(15) . . . . ? O21 Er N1 C8 156.7(15) . . . . ? O31 Er N1 C8 -149.2(13) . . . . ? N2 Er N1 C8 -133.1(16) . . . . ? N3 Er N1 C8 -75.3(16) . . . . ? N4 Er N1 C8 -15.6(15) . . . . ? QO Er N2 C2 104.3(15) . . . . ? QN Er N2 C2 -76.5(15) . . . . ? O32 Er N2 C2 -165.3(14) 3_665 . . . ? O11 Er N2 C2 18.2(17) . . . . ? O21 Er N2 C2 77.1(15) . . . . ? O31 Er N2 C2 153.8(15) . . . . ? N3 Er N2 C2 -136.1(16) . . . . ? N4 Er N2 C2 -76.5(16) . . . . ? N1 Er N2 C2 -17.6(15) . . . . ? QO Er N2 C3 -131.9(13) . . . . ? QN Er N2 C3 47.3(13) . . . . ? O32 Er N2 C3 -41(2) 3_665 . . . ? O11 Er N2 C3 142.0(14) . . . . ? O21 Er N2 C3 -159.1(16) . . . . ? O31 Er N2 C3 -82.4(14) . . . . ? N3 Er N2 C3 -12.2(14) . . . . ? N4 Er N2 C3 47.3(15) . . . . ? N1 Er N2 C3 106.2(15) . . . . ? QO Er N2 C20 -14.3(16) . . . . ? QN Er N2 C20 164.9(16) . . . . ? O32 Er N2 C20 76.2(18) 3_665 . . . ? O11 Er N2 C20 -100.4(15) . . . . ? O21 Er N2 C20 -41.5(14) . . . . ? O31 Er N2 C20 35.2(14) . . . . ? N3 Er N2 C20 105.4(15) . . . . ? N4 Er N2 C20 164.9(14) . . . . ? N1 Er N2 C20 -136.2(16) . . . . ? QO Er N3 C4 98.7(13) . . . . ? QN Er N3 C4 -75.3(13) . . . . ? O32 Er N3 C4 149.6(13) 3_665 . . . ? O11 Er N3 C4 -148.0(13) . . . . ? O21 Er N3 C4 23.4(15) . . . . ? O31 Er N3 C4 72.5(13) . . . . ? N2 Er N3 C4 -17.1(12) . . . . ? N4 Er N3 C4 -133.8(14) . . . . ? N1 Er N3 C4 -74.0(13) . . . . ? QO Er N3 C30 -19.1(15) . . . . ? QN Er N3 C30 166.9(16) . . . . ? O32 Er N3 C30 31.8(13) 3_665 . . . ? O11 Er N3 C30 94.1(16) . . . . ? O21 Er N3 C30 -94.4(15) . . . . ? O31 Er N3 C30 -45.3(12) . . . . ? N2 Er N3 C30 -134.9(14) . . . . ? N4 Er N3 C30 108.4(15) . . . . ? N1 Er N3 C30 168.2(13) . . . . ? QO Er N3 C5 -135.5(14) . . . . ? QN Er N3 C5 50.4(14) . . . . ? O32 Er N3 C5 -84.6(15) 3_665 . . . ? O11 Er N3 C5 -22(2) . . . . ? O21 Er N3 C5 149.2(14) . . . . ? O31 Er N3 C5 -161.7(17) . . . . ? N2 Er N3 C5 108.6(16) . . . . ? N4 Er N3 C5 -8.0(15) . . . . ? N1 Er N3 C5 51.7(17) . . . . ? QO Er N4 C40 -18.0(19) . . . . ? QN Er N4 C40 162.8(19) . . . . ? O32 Er N4 C40 -46.1(17) 3_665 . . . ? O11 Er N4 C40 35.5(17) . . . . ? O21 Er N4 C40 87(2) . . . . ? O31 Er N4 C40 -105.2(17) . . . . ? N2 Er N4 C40 162.8(17) . . . . ? N3 Er N4 C40 -138.0(18) . . . . ? N1 Er N4 C40 105.4(18) . . . . ? QO Er N4 C6 99.1(16) . . . . ? QN Er N4 C6 -80.0(16) . . . . ? O32 Er N4 C6 71.0(16) 3_665 . . . ? O11 Er N4 C6 152.6(17) . . . . ? O21 Er N4 C6 -155.7(16) . . . . ? O31 Er N4 C6 11.9(19) . . . . ? N2 Er N4 C6 -80.1(17) . . . . ? N3 Er N4 C6 -20.9(16) . . . . ? N1 Er N4 C6 -137.5(18) . . . . ? QO Er N4 C7 -138.2(13) . . . . ? QN Er N4 C7 42.7(13) . . . . ? O32 Er N4 C7 -166.3(15) 3_665 . . . ? O11 Er N4 C7 -84.7(15) . . . . ? O21 Er N4 C7 -33(2) . . . . ? O31 Er N4 C7 134.6(13) . . . . ? N2 Er N4 C7 42.6(15) . . . . ? N3 Er N4 C7 101.8(15) . . . . ? N1 Er N4 C7 -14.8(14) . . . . ? C10 N1 C1 C2 -82(2) . . . . ? C8 N1 C1 C2 159(2) . . . . ? Er N1 C1 C2 39(3) . . . . ? C3 N2 C2 C1 -73(3) . . . . ? C20 N2 C2 C1 167(2) . . . . ? Er N2 C2 C1 51(3) . . . . ? N1 C1 C2 N2 -62(3) . . . . ? C2 N2 C3 C4 165(2) . . . . ? C20 N2 C3 C4 -74(3) . . . . ? Er N2 C3 C4 42(2) . . . . ? C30 N3 C4 C3 161.9(18) . . . . ? C5 N3 C4 C3 -82(2) . . . . ? Er N3 C4 C3 44(2) . . . . ? N2 C3 C4 N3 -60(3) . . . . ? C4 N3 C5 C6 162(2) . . . . ? C30 N3 C5 C6 -81(2) . . . . ? Er N3 C5 C6 36(2) . . . . ? C40 N4 C6 C5 172.7(19) . . . . ? C7 N4 C6 C5 -71(2) . . . . ? Er N4 C6 C5 50(2) . . . . ? N3 C5 C6 N4 -60(3) . . . . ? C40 N4 C7 C8 -78(2) . . . . ? C6 N4 C7 C8 167.0(19) . . . . ? Er N4 C7 C8 47(2) . . . . ? N4 C7 C8 N1 -66(3) . . . . ? C1 N1 C8 C7 -75(3) . . . . ? C10 N1 C8 C7 163(2) . . . . ? Er N1 C8 C7 49(2) . . . . ? C1 N1 C10 P1 166.7(14) . . . . ? C8 N1 C10 P1 -73.3(19) . . . . ? Er N1 C10 P1 42.0(16) . . . . ? O12 P1 C10 N1 -147.5(15) . . . . ? O11 P1 C10 N1 -20.2(17) . . . . ? C11 P1 C10 N1 97.2(17) . . . . ? O12 P1 C11 C16 -60(3) . . . . ? O11 P1 C11 C16 171(2) . . . . ? C10 P1 C11 C16 57(3) . . . . ? O12 P1 C11 C12 111(2) . . . . ? O11 P1 C11 C12 -18(2) . . . . ? C10 P1 C11 C12 -132(2) . . . . ? C16 C11 C12 C13 -1(4) . . . . ? P1 C11 C12 C13 -173(2) . . . . ? C11 C12 C13 C14 3(4) . . . . ? C12 C13 C14 C15 -4(5) . . . . ? C13 C14 C15 C16 3(6) . . . . ? C14 C15 C16 C11 0(6) . . . . ? C12 C11 C16 C15 0(5) . . . . ? P1 C11 C16 C15 171(3) . . . . ? C2 N2 C20 P2 -68(2) . . . . ? C3 N2 C20 P2 169.4(16) . . . . ? Er N2 C20 P2 49.7(16) . . . . ? O22 P2 C20 N2 95.3(17) . . . . ? O21 P2 C20 N2 -31.6(18) . . . . ? C21 P2 C20 N2 -147.7(16) . . . . ? O22 P2 C21 C22 46(3) . . . . ? O21 P2 C21 C22 175(2) . . . . ? C20 P2 C21 C22 -73(3) . . . . ? O22 P2 C21 C26 -126(2) . . . . ? O21 P2 C21 C26 3(3) . . . . ? C20 P2 C21 C26 115(2) . . . . ? C26 C21 C22 C23 -2(6) . . . . ? P2 C21 C22 C23 -174(3) . . . . ? C21 C22 C23 C24 -2(7) . . . . ? C22 C23 C24 C25 6(6) . . . . ? C23 C24 C25 C26 -5(6) . . . . ? C24 C25 C26 C21 1(6) . . . . ? C22 C21 C26 C25 3(5) . . . . ? P2 C21 C26 C25 175(3) . . . . ? C4 N3 C30 P3 -73.9(19) . . . . ? C5 N3 C30 P3 166.6(15) . . . . ? Er N3 C30 P3 46.1(16) . . . . ? O32 P3 C30 N3 -146.7(14) . . . . ? O31 P3 C30 N3 -19.7(17) . . . . ? C31 P3 C30 N3 97.2(17) . . . . ? O32 P3 C31 C32 -78(2) . . . . ? O31 P3 C31 C32 152.6(19) . . . . ? C30 P3 C31 C32 39(2) . . . . ? O32 P3 C31 C36 97.6(19) . . . . ? O31 P3 C31 C36 -32(2) . . . . ? C30 P3 C31 C36 -146.2(18) . . . . ? C36 C31 C32 C33 -3(4) . . . . ? P3 C31 C32 C33 172(2) . . . . ? C31 C32 C33 C34 1(5) . . . . ? C32 C33 C34 C35 1(5) . . . . ? C33 C34 C35 C36 -1(5) . . . . ? C34 C35 C36 C31 -1(4) . . . . ? C32 C31 C36 C35 3(4) . . . . ? P3 C31 C36 C35 -173(2) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 3.029 _refine_diff_density_min -4.676 _refine_diff_density_rms 0.296 data_ct13e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ce(H2O)L]2*8H2O*2MeOH ' _chemical_formula_sum 'C32 H60 Ce N4 O13 P3' _chemical_formula_weight 941.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (no. 14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.194(3) _cell_length_b 19.990(4) _cell_length_c 15.534(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.21(3) _cell_angle_gamma 90.00 _cell_volume 3913.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 170(1) _cell_measurement_reflns_used 4926 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 21.9 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.353 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min -- _exptl_absorpt_correction_T_max -- _exptl_special_details ; crystal covered by APIEZON mull due to a loss of solvate molecules ; _diffrn_ambient_temperature 170(1) _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 'KUMA (Poland) ' _diffrn_measurement_method '.omega.-scan (0.5.degree.) ' _diffrn_detector_area_resol_mean '16.7 pixels/mm ' _diffrn_standards_number -- _diffrn_standards_interval_count -- _diffrn_standards_interval_time -- _diffrn_standards_decay_% -- _diffrn_reflns_number 28519 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.67 _reflns_number_total 9815 _reflns_number_gt 7669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA program packet' _computing_cell_refinement 'KUMA program packet' _computing_data_reduction 'KUMA program packet' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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 w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+17.4923P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson + Fourier' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9815 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 9.527 _refine_ls_shift/su_mean 0.033 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce Ce 0.66963(2) 0.611976(14) 0.030845(19) 0.02401(13) Uani 1 d . . . P1 P 0.90732(11) 0.65166(7) 0.19869(9) 0.0281(3) Uani 1 d . . . P2 P 0.57465(11) 0.77666(7) 0.06075(10) 0.0288(3) Uani 1 d . . . P3 P 0.40710(10) 0.56560(7) -0.07861(9) 0.0245(3) Uani 1 d . . . O11 O 0.8237(3) 0.5991(2) 0.1579(3) 0.0306(8) Uani 1 d . . . O12 O 0.8920(3) 0.6947(2) 0.2734(3) 0.0353(9) Uani 1 d . . . O21 O 0.6382(3) 0.71600(19) 0.1056(3) 0.0298(8) Uani 1 d . . . O22 O 0.6243(3) 0.8440(2) 0.0875(3) 0.0357(9) Uani 1 d . . . O31 O 0.4766(3) 0.61332(17) -0.0117(3) 0.0251(7) Uani 1 d . . . O32 O 0.3714(3) 0.50312(19) -0.0415(3) 0.0287(8) Uani 1 d . . . N1 N 0.8557(3) 0.6776(2) 0.0162(3) 0.0285(9) Uani 1 d . . . N2 N 0.6356(3) 0.7246(2) -0.0801(3) 0.0275(9) Uani 1 d . . . N3 N 0.5701(3) 0.5856(2) -0.1519(3) 0.0279(9) Uani 1 d . . . N4 N 0.7910(4) 0.5384(2) -0.0532(3) 0.0288(9) Uani 1 d . . . C1 C 0.8313(4) 0.7297(3) -0.0546(4) 0.0304(11) Uani 1 d . . . H011 H 0.8235 0.7088 -0.1126 0.036 Uiso 1 calc R . . H012 H 0.8904 0.7607 -0.0431 0.036 Uiso 1 calc R . . C2 C 0.7301(4) 0.7686(3) -0.0590(4) 0.0325(11) Uani 1 d . . . H021 H 0.7384 0.7904 -0.0015 0.039 Uiso 1 calc R . . H022 H 0.7194 0.8030 -0.1047 0.039 Uiso 1 calc R . . C3 C 0.6042(4) 0.7062(3) -0.1766(4) 0.0297(11) Uani 1 d . . . H031 H 0.6672 0.6941 -0.1930 0.036 Uiso 1 calc R . . H032 H 0.5729 0.7450 -0.2121 0.036 Uiso 1 calc R . . C4 C 0.5264(4) 0.6491(3) -0.2002(4) 0.0305(11) Uani 1 d . . . H041 H 0.4626 0.6614 -0.1851 0.037 Uiso 1 calc R . . H042 H 0.5069 0.6413 -0.2647 0.037 Uiso 1 calc R . . C5 C 0.6416(4) 0.5531(3) -0.1967(4) 0.0311(11) Uani 1 d . . . H051 H 0.6816 0.5871 -0.2171 0.037 Uiso 1 calc R . . H052 H 0.5995 0.5288 -0.2491 0.037 Uiso 1 calc R . . C6 C 0.7185(4) 0.5049(3) -0.1334(4) 0.0312(11) Uani 1 d . . . H061 H 0.6780 0.4709 -0.1133 0.037 Uiso 1 calc R . . H062 H 0.7606 0.4825 -0.1665 0.037 Uiso 1 calc R . . C7 C 0.8693(4) 0.5797(3) -0.0801(4) 0.0309(11) Uani 1 d . . . H071 H 0.8332 0.6054 -0.1333 0.037 Uiso 1 calc R . . H072 H 0.9202 0.5506 -0.0956 0.037 Uiso 1 calc R . . C8 C 0.9280(4) 0.6272(3) -0.0051(4) 0.0289(11) Uani 1 d . . . H081 H 0.9618 0.6015 0.0487 0.035 Uiso 1 calc R . . H082 H 0.9832 0.6502 -0.0231 0.035 Uiso 1 calc R . . C10 C 0.9087(4) 0.7072(3) 0.1055(4) 0.0302(11) Uani 1 d . . . H101 H 0.8735 0.7487 0.1116 0.036 Uiso 1 calc R . . H102 H 0.9817 0.7176 0.1092 0.036 Uiso 1 calc R . . C11 C 1.0332(5) 0.6086(3) 0.2421(4) 0.0292(11) Uani 1 d . . . C12 C 1.0333(5) 0.5395(3) 0.2561(4) 0.0369(12) Uani 1 d . . . H12 H 0.9707 0.5153 0.2338 0.044 Uiso 1 calc R . . C13 C 1.1264(6) 0.5064(4) 0.3033(4) 0.0449(15) Uani 1 d . . . H13 H 1.1260 0.4605 0.3127 0.054 Uiso 1 calc R . . C14 C 1.2191(5) 0.5425(4) 0.3359(5) 0.0502(17) Uani 1 d . . . H14 H 1.2810 0.5210 0.3686 0.060 Uiso 1 calc R . . C15 C 1.2205(5) 0.6109(4) 0.3201(5) 0.0439(17) Uani 1 d . . . H15 H 1.2836 0.6347 0.3410 0.053 Uiso 1 calc R . . C16 C 1.1280(5) 0.6439(3) 0.2733(4) 0.0386(13) Uani 1 d . . . H16 H 1.1294 0.6896 0.2627 0.046 Uiso 1 calc R . . C20 C 0.5470(4) 0.7619(3) -0.0607(4) 0.0290(10) Uani 1 d . . . H201 H 0.4818 0.7366 -0.0827 0.035 Uiso 1 calc R . . H202 H 0.5372 0.8045 -0.0921 0.035 Uiso 1 calc R . . C21 C 0.4470(4) 0.7761(3) 0.0812(4) 0.0342(12) Uani 1 d . . . C22 C 0.4125(5) 0.7213(3) 0.1215(4) 0.0393(13) Uani 1 d . . . H22 H 0.4535 0.6827 0.1349 0.047 Uiso 1 calc R . . C23 C 0.3157(6) 0.7253(4) 0.1412(5) 0.0511(17) Uani 1 d . . . H23 H 0.2928 0.6895 0.1690 0.061 Uiso 1 calc R . . C24 C 0.2538(6) 0.7825(5) 0.1196(6) 0.059(2) Uani 1 d . . . H24 H 0.1893 0.7846 0.1324 0.071 Uiso 1 calc R . . C25 C 0.2868(6) 0.8359(4) 0.0795(6) 0.057(2) Uani 1 d . . . H25 H 0.2447 0.8741 0.0661 0.068 Uiso 1 calc R . . C26 C 0.3828(5) 0.8341(4) 0.0585(5) 0.0456(15) Uani 1 d . . . H26 H 0.4041 0.8701 0.0302 0.055 Uiso 1 calc R . . C30 C 0.4809(4) 0.5396(3) -0.1564(4) 0.0297(11) Uani 1 d . . . H301 H 0.5081 0.4947 -0.1411 0.036 Uiso 1 calc R . . H302 H 0.4333 0.5388 -0.2174 0.036 Uiso 1 calc R . . C31 C 0.2868(4) 0.6096(3) -0.1393(4) 0.0274(11) Uani 1 d . . . C32 C 0.2182(5) 0.5821(3) -0.2183(4) 0.0383(13) Uani 1 d . . . H32 H 0.2389 0.5456 -0.2461 0.046 Uiso 1 calc R . . C33 C 0.1180(5) 0.6110(3) -0.2541(5) 0.0428(17) Uani 1 d . . . H33 H 0.0719 0.5938 -0.3069 0.051 Uiso 1 calc R . . C34 C 0.0871(5) 0.6641(4) -0.2124(5) 0.0486(18) Uani 1 d . . . H34 H 0.0191 0.6815 -0.2359 0.058 Uiso 1 calc R . . C35 C 0.1547(5) 0.6921(4) -0.1363(5) 0.0461(16) Uani 1 d . . . H35 H 0.1334 0.7288 -0.1092 0.055 Uiso 1 calc R . . C36 C 0.2560(5) 0.6649(3) -0.1002(4) 0.0349(12) Uani 1 d . . . H36 H 0.3030 0.6842 -0.0494 0.042 Uiso 1 calc R . . C40 C 0.8494(5) 0.4845(3) 0.0083(4) 0.0339(12) Uani 1 d . . . H401 H 0.7998 0.4573 0.0270 0.051 Uiso 1 calc R . . H402 H 0.8987 0.5044 0.0603 0.051 Uiso 1 calc R . . H403 H 0.8873 0.4573 -0.0227 0.051 Uiso 1 calc R . . O99 O 0.6248(4) 0.6050(2) 0.1994(4) 0.0449(18) Uani 1.00(2) d . . . O98 O 0.5714(8) 0.9541(4) -0.0257(7) 0.119(5) Uani 1.00(3) d . . . O96 O 0.8154(4) 0.6714(2) -0.2731(3) 0.0452(17) Uani 1.000(18) d . . . OW1 O 0.7182(7) 0.5359(4) 0.3583(5) 0.090(4) Uani 0.95(2) d P . . OW2 O 0.5385(7) 0.0967(4) 0.2063(6) 0.056(3) Uani 0.67(2) d P . . OM1 O 0.1002(6) 0.3901(3) 0.5849(5) 0.052(2) Uani 0.840(18) d P . . CM1 C -0.0051(11) 0.3954(6) 0.5274(7) 0.073(4) Uani 0.840(18) d P . . QN N 0.7131 0.6315 -0.0673 0.050 Uiso 0.00 d P . . QO O 0.6343 0.6063 0.0733 0.050 Uiso 0.00 d P . . 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 Ce 0.02071(18) 0.02441(19) 0.02601(19) 0.00024(10) 0.00551(12) 0.00117(9) P1 0.0251(6) 0.0309(7) 0.0271(7) 0.0008(5) 0.0056(5) 0.0002(5) P2 0.0266(6) 0.0282(7) 0.0306(7) 0.0004(5) 0.0069(5) 0.0057(5) P3 0.0209(6) 0.0254(6) 0.0265(6) -0.0003(5) 0.0059(5) 0.0002(5) O11 0.0260(18) 0.033(2) 0.030(2) 0.0034(16) 0.0037(15) -0.0013(15) O12 0.039(2) 0.038(2) 0.029(2) 0.0016(17) 0.0098(17) 0.0070(18) O21 0.0273(18) 0.0286(19) 0.031(2) 0.0005(15) 0.0051(15) 0.0033(15) O22 0.035(2) 0.029(2) 0.038(2) -0.0054(16) 0.0030(17) 0.0001(16) O31 0.0205(17) 0.0266(19) 0.0278(19) -0.0023(13) 0.0067(14) 0.0012(13) O32 0.0255(17) 0.0294(19) 0.0288(19) 0.0019(15) 0.0040(14) 0.0004(14) N1 0.025(2) 0.033(2) 0.028(2) 0.0029(18) 0.0076(17) 0.0032(17) N2 0.026(2) 0.028(2) 0.029(2) 0.0006(17) 0.0096(17) 0.0015(17) N3 0.0208(19) 0.034(2) 0.027(2) -0.0011(18) 0.0045(16) -0.0002(17) N4 0.025(2) 0.033(2) 0.029(2) -0.0017(18) 0.0084(18) -0.0003(18) C1 0.028(2) 0.035(3) 0.028(3) 0.003(2) 0.008(2) 0.000(2) C2 0.031(3) 0.038(3) 0.028(3) 0.001(2) 0.007(2) -0.004(2) C3 0.029(3) 0.034(3) 0.025(2) 0.001(2) 0.007(2) 0.002(2) C4 0.027(2) 0.036(3) 0.026(3) 0.005(2) 0.004(2) 0.002(2) C5 0.029(2) 0.039(3) 0.028(3) -0.004(2) 0.011(2) -0.003(2) C6 0.026(2) 0.040(3) 0.027(3) -0.005(2) 0.008(2) -0.002(2) C7 0.027(2) 0.035(3) 0.036(3) -0.001(2) 0.016(2) -0.004(2) C8 0.022(2) 0.037(3) 0.027(3) -0.002(2) 0.006(2) 0.005(2) C10 0.028(2) 0.031(3) 0.032(3) -0.003(2) 0.008(2) -0.004(2) C11 0.029(3) 0.032(3) 0.024(3) -0.0012(19) 0.004(2) -0.001(2) C12 0.034(3) 0.038(3) 0.037(3) 0.006(2) 0.008(2) 0.005(2) C13 0.047(4) 0.048(4) 0.039(3) 0.009(3) 0.010(3) 0.015(3) C14 0.035(3) 0.071(5) 0.044(4) 0.001(3) 0.010(3) 0.021(3) C15 0.021(3) 0.069(5) 0.038(3) -0.008(3) 0.003(2) 0.004(3) C16 0.034(3) 0.043(3) 0.036(3) -0.010(3) 0.005(2) -0.001(2) C20 0.025(2) 0.032(3) 0.029(3) 0.004(2) 0.006(2) 0.006(2) C21 0.024(2) 0.043(3) 0.033(3) -0.004(2) 0.004(2) 0.001(2) C22 0.043(3) 0.041(3) 0.035(3) -0.003(2) 0.014(3) 0.003(3) C23 0.050(4) 0.064(5) 0.047(4) -0.003(3) 0.025(3) -0.003(3) C24 0.035(3) 0.079(6) 0.069(5) -0.005(4) 0.024(3) 0.009(3) C25 0.037(3) 0.067(5) 0.064(5) 0.000(4) 0.012(3) 0.019(3) C26 0.041(3) 0.051(4) 0.044(4) -0.003(3) 0.010(3) 0.016(3) C30 0.027(2) 0.032(3) 0.031(3) -0.002(2) 0.011(2) 0.001(2) C31 0.020(2) 0.029(3) 0.031(3) 0.0034(19) 0.004(2) 0.0015(18) C32 0.035(3) 0.039(3) 0.036(3) 0.006(2) 0.002(2) -0.005(2) C33 0.025(3) 0.044(4) 0.047(4) 0.020(3) -0.008(3) -0.007(2) C34 0.026(3) 0.050(4) 0.069(5) 0.027(3) 0.013(3) 0.017(3) C35 0.032(3) 0.051(4) 0.056(4) 0.020(3) 0.014(3) 0.018(3) C36 0.029(3) 0.037(3) 0.037(3) 0.005(2) 0.008(2) 0.008(2) C40 0.031(3) 0.034(3) 0.039(3) 0.004(2) 0.013(2) 0.006(2) O99 0.053(3) 0.038(3) 0.049(3) 0.0002(19) 0.024(2) 0.001(2) O98 0.112(7) 0.066(5) 0.142(9) 0.020(5) -0.022(6) 0.005(5) O96 0.040(3) 0.046(3) 0.049(3) 0.007(2) 0.013(2) 0.000(2) OW1 0.104(7) 0.079(6) 0.072(5) -0.008(4) 0.004(4) -0.001(4) OW2 0.048(5) 0.057(5) 0.066(6) 0.011(4) 0.022(4) -0.001(4) OM1 0.061(4) 0.051(4) 0.047(4) 0.007(3) 0.018(3) 0.005(3) CM1 0.078(8) 0.095(9) 0.037(5) 0.002(5) 0.002(5) 0.027(6) _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 Ce QO 0.9207(4) . ? Ce QN 1.8225(5) . ? Ce O32 2.380(4) 3_665 ? Ce O11 2.392(4) . ? Ce O31 2.434(4) . ? Ce O21 2.476(4) . ? Ce N4 2.769(5) . ? Ce N2 2.789(5) . ? Ce N3 2.802(5) . ? Ce N1 2.851(5) . ? Ce O99 2.854(5) . ? P1 O12 1.506(4) . ? P1 O11 1.520(4) . ? P1 C11 1.814(6) . ? P1 C10 1.828(6) . ? P2 O22 1.501(4) . ? P2 O21 1.521(4) . ? P2 C21 1.805(6) . ? P2 C20 1.836(6) . ? P3 O31 1.506(4) . ? P3 O32 1.509(4) . ? P3 C31 1.815(5) . ? P3 C30 1.837(5) . ? O32 Ce 2.380(4) 3_665 ? N1 C1 1.479(7) . ? N1 C10 1.481(7) . ? N1 C8 1.490(7) . ? N2 C3 1.478(7) . ? N2 C2 1.481(7) . ? N2 C20 1.492(7) . ? N3 C5 1.478(7) . ? N3 C30 1.479(7) . ? N3 C4 1.500(7) . ? N4 C7 1.476(7) . ? N4 C6 1.487(7) . ? N4 C40 1.493(7) . ? C1 C2 1.529(8) . ? C1 H011 0.9700 . ? C1 H012 0.9700 . ? C2 H021 0.9700 . ? C2 H022 0.9700 . ? C3 C4 1.506(8) . ? C3 H031 0.9700 . ? C3 H032 0.9700 . ? C4 H041 0.9700 . ? C4 H042 0.9700 . ? C5 C6 1.528(8) . ? C5 H051 0.9700 . ? C5 H052 0.9700 . ? C6 H061 0.9700 . ? C6 H062 0.9700 . ? C7 C8 1.526(8) . ? C7 H071 0.9700 . ? C7 H072 0.9700 . ? C8 H081 0.9700 . ? C8 H082 0.9700 . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C11 C16 1.392(8) . ? C11 C12 1.400(8) . ? C12 C13 1.397(8) . ? C12 H12 0.9300 . ? C13 C14 1.381(11) . ? C13 H13 0.9300 . ? C14 C15 1.390(11) . ? C14 H14 0.9300 . ? C15 C16 1.388(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C20 H201 0.9700 . ? C20 H202 0.9700 . ? C21 C22 1.402(9) . ? C21 C26 1.416(9) . ? C22 C23 1.403(9) . ? C22 H22 0.9300 . ? C23 C24 1.386(11) . ? C23 H23 0.9300 . ? C24 C25 1.371(12) . ? C24 H24 0.9300 . ? C25 C26 1.399(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 C36 1.381(8) . ? C31 C32 1.402(8) . ? C32 C33 1.398(9) . ? C32 H32 0.9300 . ? C33 C34 1.368(11) . ? C33 H33 0.9300 . ? C34 C35 1.372(11) . ? C34 H34 0.9300 . ? C35 C36 1.398(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C40 H401 0.9600 . ? C40 H402 0.9600 . ? C40 H403 0.9600 . ? OM1 CM1 1.416(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag QO Ce QN 167.71(3) . . ? QO Ce O32 70.00(9) . 3_665 ? QN Ce O32 113.56(9) . 3_665 ? QO Ce O11 83.24(10) . . ? QN Ce O11 108.19(10) . . ? O32 Ce O11 89.63(13) 3_665 . ? QO Ce O31 59.02(9) . . ? QN Ce O31 109.46(9) . . ? O32 Ce O31 77.80(12) 3_665 . ? O11 Ce O31 142.26(13) . . ? QO Ce O21 64.92(9) . . ? QN Ce O21 110.48(9) . . ? O32 Ce O21 134.92(13) 3_665 . ? O11 Ce O21 85.59(13) . . ? O31 Ce O21 79.11(12) . . ? QO Ce N4 139.35(10) . . ? QN Ce N4 49.53(10) . . ? O32 Ce N4 72.20(13) 3_665 . ? O11 Ce N4 82.11(14) . . ? O31 Ce N4 125.60(13) . . ? O21 Ce N4 150.20(13) . . ? QO Ce N2 121.27(9) . . ? QN Ce N2 48.92(9) . . ? O32 Ce N2 145.53(13) 3_665 . ? O11 Ce N2 122.62(13) . . ? O31 Ce N2 81.90(13) . . ? O21 Ce N2 66.02(13) . . ? N4 Ce N2 98.45(13) . . ? QO Ce N3 121.20(9) . . ? QN Ce N3 50.40(9) . . ? O32 Ce N3 80.83(13) 3_665 . ? O11 Ce N3 147.65(14) . . ? O31 Ce N3 65.66(13) . . ? O21 Ce N3 122.65(13) . . ? N4 Ce N3 65.53(13) . . ? N2 Ce N3 65.43(14) . . ? QO Ce N1 138.10(10) . . ? QN Ce N1 48.93(9) . . ? O32 Ce N1 131.98(13) 3_665 . ? O11 Ce N1 64.79(13) . . ? O31 Ce N1 146.03(12) . . ? O21 Ce N1 85.35(13) . . ? N4 Ce N1 64.85(14) . . ? N2 Ce N1 64.17(13) . . ? N3 Ce N1 99.32(13) . . ? QO Ce O99 18.16(11) . . ? QN Ce O99 168.45(10) . . ? O32 Ce O99 77.06(13) 3_665 . ? O11 Ce O99 66.04(15) . . ? O31 Ce O99 76.44(14) . . ? O21 Ce O99 60.10(13) . . ? N4 Ce O99 135.43(14) . . ? N2 Ce O99 124.57(13) . . ? N3 Ce O99 139.29(14) . . ? N1 Ce O99 120.87(14) . . ? O12 P1 O11 118.0(2) . . ? O12 P1 C11 107.5(2) . . ? O11 P1 C11 107.4(2) . . ? O12 P1 C10 107.4(3) . . ? O11 P1 C10 105.4(2) . . ? C11 P1 C10 111.1(3) . . ? O22 P2 O21 116.8(2) . . ? O22 P2 C21 108.1(3) . . ? O21 P2 C21 109.4(3) . . ? O22 P2 C20 111.5(3) . . ? O21 P2 C20 105.0(2) . . ? C21 P2 C20 105.5(3) . . ? O31 P3 O32 117.1(2) . . ? O31 P3 C31 108.2(2) . . ? O32 P3 C31 106.0(2) . . ? O31 P3 C30 107.4(2) . . ? O32 P3 C30 107.7(2) . . ? C31 P3 C30 110.3(3) . . ? P1 O11 Ce 127.2(2) . . ? P2 O21 Ce 126.9(2) . . ? P3 O31 Ce 123.7(2) . . ? P3 O32 Ce 158.4(2) . 3_665 ? C1 N1 C10 110.8(4) . . ? C1 N1 C8 108.9(4) . . ? C10 N1 C8 108.8(4) . . ? C1 N1 Ce 112.4(3) . . ? C10 N1 Ce 106.7(3) . . ? C8 N1 Ce 109.2(3) . . ? C3 N2 C2 109.7(4) . . ? C3 N2 C20 109.1(4) . . ? C2 N2 C20 108.4(4) . . ? C3 N2 Ce 111.8(3) . . ? C2 N2 Ce 111.8(3) . . ? C20 N2 Ce 105.7(3) . . ? C5 N3 C30 108.3(4) . . ? C5 N3 C4 110.0(4) . . ? C30 N3 C4 108.7(4) . . ? C5 N3 Ce 112.7(3) . . ? C30 N3 Ce 107.0(3) . . ? C4 N3 Ce 110.1(3) . . ? C7 N4 C6 110.2(4) . . ? C7 N4 C40 108.2(4) . . ? C6 N4 C40 107.1(4) . . ? C7 N4 Ce 112.8(3) . . ? C6 N4 Ce 108.4(3) . . ? C40 N4 Ce 110.0(3) . . ? N1 C1 C2 112.7(4) . . ? N1 C1 H011 109.1 . . ? C2 C1 H011 109.1 . . ? N1 C1 H012 109.1 . . ? C2 C1 H012 109.1 . . ? H011 C1 H012 107.8 . . ? N2 C2 C1 112.0(5) . . ? N2 C2 H021 109.2 . . ? C1 C2 H021 109.2 . . ? N2 C2 H022 109.2 . . ? C1 C2 H022 109.2 . . ? H021 C2 H022 107.9 . . ? N2 C3 C4 113.7(4) . . ? N2 C3 H031 108.8 . . ? C4 C3 H031 108.8 . . ? N2 C3 H032 108.8 . . ? C4 C3 H032 108.8 . . ? H031 C3 H032 107.7 . . ? N3 C4 C3 112.7(4) . . ? N3 C4 H041 109.0 . . ? C3 C4 H041 109.0 . . ? N3 C4 H042 109.0 . . ? C3 C4 H042 109.0 . . ? H041 C4 H042 107.8 . . ? N3 C5 C6 111.7(4) . . ? N3 C5 H051 109.3 . . ? C6 C5 H051 109.3 . . ? N3 C5 H052 109.3 . . ? C6 C5 H052 109.3 . . ? H051 C5 H052 107.9 . . ? N4 C6 C5 113.3(5) . . ? N4 C6 H061 108.9 . . ? C5 C6 H061 108.9 . . ? N4 C6 H062 108.9 . . ? C5 C6 H062 108.9 . . ? H061 C6 H062 107.7 . . ? N4 C7 C8 111.8(4) . . ? N4 C7 H071 109.3 . . ? C8 C7 H071 109.3 . . ? N4 C7 H072 109.3 . . ? C8 C7 H072 109.3 . . ? H071 C7 H072 107.9 . . ? N1 C8 C7 112.1(4) . . ? N1 C8 H081 109.2 . . ? C7 C8 H081 109.2 . . ? N1 C8 H082 109.2 . . ? C7 C8 H082 109.2 . . ? H081 C8 H082 107.9 . . ? N1 C10 P1 112.8(4) . . ? N1 C10 H101 109.0 . . ? P1 C10 H101 109.0 . . ? N1 C10 H102 109.0 . . ? P1 C10 H102 109.0 . . ? H101 C10 H102 107.8 . . ? C16 C11 C12 119.2(6) . . ? C16 C11 P1 121.3(4) . . ? C12 C11 P1 119.0(4) . . ? C13 C12 C11 120.6(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.4(7) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.4(6) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.3(6) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.1(6) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? N2 C20 P2 111.0(3) . . ? N2 C20 H201 109.4 . . ? P2 C20 H201 109.4 . . ? N2 C20 H202 109.4 . . ? P2 C20 H202 109.4 . . ? H201 C20 H202 108.0 . . ? C22 C21 C26 120.1(6) . . ? C22 C21 P2 121.7(5) . . ? C26 C21 P2 118.1(5) . . ? C21 C22 C23 119.3(6) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.2(7) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 121.1(7) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C21 118.6(7) . . ? C25 C26 H26 120.7 . . ? C21 C26 H26 120.7 . . ? N3 C30 P3 111.2(4) . . ? N3 C30 H301 109.4 . . ? P3 C30 H301 109.4 . . ? N3 C30 H302 109.4 . . ? P3 C30 H302 109.4 . . ? H301 C30 H302 108.0 . . ? C36 C31 C32 120.1(5) . . ? C36 C31 P3 119.0(4) . . ? C32 C31 P3 120.2(4) . . ? C33 C32 C31 118.4(6) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C34 C33 C32 120.8(7) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 121.0(6) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 119.2(7) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C31 C36 C35 120.4(6) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? N4 C40 H401 109.5 . . ? N4 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? N4 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 Ce 91.2(3) . . . . ? C11 P1 O11 Ce -147.1(3) . . . . ? C10 P1 O11 Ce -28.6(3) . . . . ? QO Ce O11 P1 -113.5(3) . . . . ? QN Ce O11 P1 61.8(3) . . . . ? O32 Ce O11 P1 176.6(3) 3_665 . . . ? O31 Ce O11 P1 -114.2(3) . . . . ? O21 Ce O11 P1 -48.3(3) . . . . ? N4 Ce O11 P1 104.5(3) . . . . ? N2 Ce O11 P1 9.5(4) . . . . ? N3 Ce O11 P1 104.5(3) . . . . ? N1 Ce O11 P1 38.6(3) . . . . ? O99 Ce O11 P1 -107.5(3) . . . . ? O22 P2 O21 Ce -133.6(3) . . . . ? C21 P2 O21 Ce 103.3(3) . . . . ? C20 P2 O21 Ce -9.5(3) . . . . ? QO Ce O21 P2 -119.2(3) . . . . ? QN Ce O21 P2 48.4(3) . . . . ? O32 Ce O21 P2 -118.8(3) 3_665 . . . ? O11 Ce O21 P2 156.2(3) . . . . ? O31 Ce O21 P2 -58.5(3) . . . . ? N4 Ce O21 P2 90.5(4) . . . . ? N2 Ce O21 P2 27.4(2) . . . . ? N3 Ce O21 P2 -6.9(3) . . . . ? N1 Ce O21 P2 91.2(3) . . . . ? O99 Ce O21 P2 -139.0(3) . . . . ? O32 P3 O31 Ce 94.2(3) . . . . ? C31 P3 O31 Ce -146.2(2) . . . . ? C30 P3 O31 Ce -27.1(3) . . . . ? QO Ce O31 P3 -121.1(3) . . . . ? QN Ce O31 P3 63.7(2) . . . . ? O32 Ce O31 P3 -47.3(2) 3_665 . . . ? O11 Ce O31 P3 -120.4(3) . . . . ? O21 Ce O31 P3 171.7(3) . . . . ? N4 Ce O31 P3 10.1(3) . . . . ? N2 Ce O31 P3 104.7(3) . . . . ? N3 Ce O31 P3 38.1(2) . . . . ? N1 Ce O31 P3 107.4(3) . . . . ? O99 Ce O31 P3 -126.7(3) . . . . ? O31 P3 O32 Ce -138.4(6) . . . 3_665 ? C31 P3 O32 Ce 100.8(6) . . . 3_665 ? C30 P3 O32 Ce -17.3(7) . . . 3_665 ? QO Ce N1 C1 -118.1(3) . . . . ? QN Ce N1 C1 47.6(3) . . . . ? O32 Ce N1 C1 133.6(3) 3_665 . . . ? O11 Ce N1 C1 -162.1(4) . . . . ? O31 Ce N1 C1 -12.2(5) . . . . ? O21 Ce N1 C1 -74.8(4) . . . . ? N4 Ce N1 C1 104.8(4) . . . . ? N2 Ce N1 C1 -9.2(3) . . . . ? N3 Ce N1 C1 47.6(4) . . . . ? O99 Ce N1 C1 -125.7(3) . . . . ? QO Ce N1 C10 3.4(4) . . . . ? QN Ce N1 C10 169.2(4) . . . . ? O32 Ce N1 C10 -104.8(3) 3_665 . . . ? O11 Ce N1 C10 -40.5(3) . . . . ? O31 Ce N1 C10 109.4(3) . . . . ? O21 Ce N1 C10 46.8(3) . . . . ? N4 Ce N1 C10 -133.6(4) . . . . ? N2 Ce N1 C10 112.3(3) . . . . ? N3 Ce N1 C10 169.1(3) . . . . ? O99 Ce N1 C10 -4.1(4) . . . . ? QO Ce N1 C8 120.9(3) . . . . ? QN Ce N1 C8 -73.4(3) . . . . ? O32 Ce N1 C8 12.6(4) 3_665 . . . ? O11 Ce N1 C8 76.9(3) . . . . ? O31 Ce N1 C8 -133.2(3) . . . . ? O21 Ce N1 C8 164.2(3) . . . . ? N4 Ce N1 C8 -16.2(3) . . . . ? N2 Ce N1 C8 -130.2(3) . . . . ? N3 Ce N1 C8 -73.4(3) . . . . ? O99 Ce N1 C8 113.3(3) . . . . ? QO Ce N2 C3 -124.9(3) . . . . ? QN Ce N2 C3 45.9(3) . . . . ? O32 Ce N2 C3 -24.6(4) 3_665 . . . ? O11 Ce N2 C3 132.1(3) . . . . ? O31 Ce N2 C3 -78.9(3) . . . . ? O21 Ce N2 C3 -160.5(4) . . . . ? N4 Ce N2 C3 46.1(3) . . . . ? N3 Ce N2 C3 -12.0(3) . . . . ? N1 Ce N2 C3 102.8(3) . . . . ? O99 Ce N2 C3 -146.2(3) . . . . ? QO Ce N2 C2 111.6(3) . . . . ? QN Ce N2 C2 -77.6(3) . . . . ? O32 Ce N2 C2 -148.1(3) 3_665 . . . ? O11 Ce N2 C2 8.6(4) . . . . ? O31 Ce N2 C2 157.6(4) . . . . ? O21 Ce N2 C2 76.0(3) . . . . ? N4 Ce N2 C2 -77.4(3) . . . . ? N3 Ce N2 C2 -135.5(4) . . . . ? N1 Ce N2 C2 -20.7(3) . . . . ? O99 Ce N2 C2 90.3(4) . . . . ? QO Ce N2 C20 -6.2(3) . . . . ? QN Ce N2 C20 164.6(4) . . . . ? O32 Ce N2 C20 94.1(4) 3_665 . . . ? O11 Ce N2 C20 -109.2(3) . . . . ? O31 Ce N2 C20 39.8(3) . . . . ? O21 Ce N2 C20 -41.8(3) . . . . ? N4 Ce N2 C20 164.8(3) . . . . ? N3 Ce N2 C20 106.7(3) . . . . ? N1 Ce N2 C20 -138.5(3) . . . . ? O99 Ce N2 C20 -27.5(4) . . . . ? QO Ce N3 C5 -140.9(3) . . . . ? QN Ce N3 C5 50.2(3) . . . . ? O32 Ce N3 C5 -81.1(4) 3_665 . . . ? O11 Ce N3 C5 -6.6(5) . . . . ? O31 Ce N3 C5 -161.7(4) . . . . ? O21 Ce N3 C5 140.7(3) . . . . ? N4 Ce N3 C5 -6.5(3) . . . . ? N2 Ce N3 C5 106.2(4) . . . . ? N1 Ce N3 C5 50.2(4) . . . . ? O99 Ce N3 C5 -138.7(3) . . . . ? QO Ce N3 C30 -22.0(3) . . . . ? QN Ce N3 C30 169.1(4) . . . . ? O32 Ce N3 C30 37.9(3) 3_665 . . . ? O11 Ce N3 C30 112.4(3) . . . . ? O31 Ce N3 C30 -42.8(3) . . . . ? O21 Ce N3 C30 -100.4(3) . . . . ? N4 Ce N3 C30 112.4(3) . . . . ? N2 Ce N3 C30 -134.9(3) . . . . ? N1 Ce N3 C30 169.2(3) . . . . ? O99 Ce N3 C30 -19.8(4) . . . . ? QO Ce N3 C4 96.0(3) . . . . ? QN Ce N3 C4 -73.0(3) . . . . ? O32 Ce N3 C4 155.8(3) 3_665 . . . ? O11 Ce N3 C4 -129.7(3) . . . . ? O31 Ce N3 C4 75.1(3) . . . . ? O21 Ce N3 C4 17.5(4) . . . . ? N4 Ce N3 C4 -129.7(3) . . . . ? N2 Ce N3 C4 -17.0(3) . . . . ? N1 Ce N3 C4 -72.9(3) . . . . ? O99 Ce N3 C4 98.2(4) . . . . ? QO Ce N4 C7 -150.6(3) . . . . ? QN Ce N4 C7 41.5(3) . . . . ? O32 Ce N4 C7 -172.8(4) 3_665 . . . ? O11 Ce N4 C7 -80.7(4) . . . . ? O31 Ce N4 C7 127.4(3) . . . . ? O21 Ce N4 C7 -14.1(5) . . . . ? N2 Ce N4 C7 41.3(4) . . . . ? N3 Ce N4 C7 99.3(4) . . . . ? N1 Ce N4 C7 -14.9(3) . . . . ? O99 Ce N4 C7 -124.2(4) . . . . ? QO Ce N4 C6 87.1(4) . . . . ? QN Ce N4 C6 -80.8(3) . . . . ? O32 Ce N4 C6 64.8(3) 3_665 . . . ? O11 Ce N4 C6 157.0(4) . . . . ? O31 Ce N4 C6 5.0(4) . . . . ? O21 Ce N4 C6 -136.5(3) . . . . ? N2 Ce N4 C6 -81.0(3) . . . . ? N3 Ce N4 C6 -23.0(3) . . . . ? N1 Ce N4 C6 -137.2(4) . . . . ? O99 Ce N4 C6 113.5(4) . . . . ? QO Ce N4 C40 -29.6(4) . . . . ? QN Ce N4 C40 162.4(4) . . . . ? O32 Ce N4 C40 -51.9(3) 3_665 . . . ? O11 Ce N4 C40 40.2(3) . . . . ? O31 Ce N4 C40 -111.7(3) . . . . ? O21 Ce N4 C40 106.8(4) . . . . ? N2 Ce N4 C40 162.2(3) . . . . ? N3 Ce N4 C40 -139.8(4) . . . . ? N1 Ce N4 C40 106.0(4) . . . . ? O99 Ce N4 C40 -3.3(4) . . . . ? C10 N1 C1 C2 -81.1(5) . . . . ? C8 N1 C1 C2 159.4(5) . . . . ? Ce N1 C1 C2 38.2(5) . . . . ? C3 N2 C2 C1 -74.8(6) . . . . ? C20 N2 C2 C1 166.0(4) . . . . ? Ce N2 C2 C1 49.8(5) . . . . ? N1 C1 C2 N2 -61.1(6) . . . . ? C2 N2 C3 C4 166.1(5) . . . . ? C20 N2 C3 C4 -75.2(6) . . . . ? Ce N2 C3 C4 41.5(5) . . . . ? C5 N3 C4 C3 -78.9(5) . . . . ? C30 N3 C4 C3 162.8(4) . . . . ? Ce N3 C4 C3 45.9(5) . . . . ? N2 C3 C4 N3 -61.5(6) . . . . ? C30 N3 C5 C6 -82.8(5) . . . . ? C4 N3 C5 C6 158.6(4) . . . . ? Ce N3 C5 C6 35.4(5) . . . . ? C7 N4 C6 C5 -70.8(6) . . . . ? C40 N4 C6 C5 171.8(4) . . . . ? Ce N4 C6 C5 53.1(5) . . . . ? N3 C5 C6 N4 -62.3(6) . . . . ? C6 N4 C7 C8 166.7(5) . . . . ? C40 N4 C7 C8 -76.5(6) . . . . ? Ce N4 C7 C8 45.4(5) . . . . ? C1 N1 C8 C7 -76.7(6) . . . . ? C10 N1 C8 C7 162.5(4) . . . . ? Ce N1 C8 C7 46.3(5) . . . . ? N4 C7 C8 N1 -64.4(6) . . . . ? C1 N1 C10 P1 163.8(4) . . . . ? C8 N1 C10 P1 -76.6(5) . . . . ? Ce N1 C10 P1 41.2(4) . . . . ? O12 P1 C10 N1 -142.9(4) . . . . ? O11 P1 C10 N1 -16.2(4) . . . . ? C11 P1 C10 N1 99.8(4) . . . . ? O12 P1 C11 C16 -60.4(6) . . . . ? O11 P1 C11 C16 171.6(5) . . . . ? C10 P1 C11 C16 56.8(6) . . . . ? O12 P1 C11 C12 110.6(5) . . . . ? O11 P1 C11 C12 -17.4(5) . . . . ? C10 P1 C11 C12 -132.2(5) . . . . ? C16 C11 C12 C13 2.1(9) . . . . ? P1 C11 C12 C13 -169.1(5) . . . . ? C11 C12 C13 C14 -0.3(10) . . . . ? C12 C13 C14 C15 -1.5(10) . . . . ? C13 C14 C15 C16 1.6(11) . . . . ? C14 C15 C16 C11 0.2(10) . . . . ? C12 C11 C16 C15 -2.0(9) . . . . ? P1 C11 C16 C15 169.0(5) . . . . ? C3 N2 C20 P2 172.7(4) . . . . ? C2 N2 C20 P2 -67.8(5) . . . . ? Ce N2 C20 P2 52.3(4) . . . . ? O22 P2 C20 N2 94.6(4) . . . . ? O21 P2 C20 N2 -32.8(4) . . . . ? C21 P2 C20 N2 -148.3(4) . . . . ? O22 P2 C21 C22 -136.5(5) . . . . ? O21 P2 C21 C22 -8.3(6) . . . . ? C20 P2 C21 C22 104.1(5) . . . . ? O22 P2 C21 C26 41.2(6) . . . . ? O21 P2 C21 C26 169.4(5) . . . . ? C20 P2 C21 C26 -78.2(5) . . . . ? C26 C21 C22 C23 -1.9(9) . . . . ? P2 C21 C22 C23 175.8(5) . . . . ? C21 C22 C23 C24 1.2(11) . . . . ? C22 C23 C24 C25 -0.7(13) . . . . ? C23 C24 C25 C26 0.7(13) . . . . ? C24 C25 C26 C21 -1.3(12) . . . . ? C22 C21 C26 C25 1.9(10) . . . . ? P2 C21 C26 C25 -175.8(6) . . . . ? C5 N3 C30 P3 165.5(4) . . . . ? C4 N3 C30 P3 -75.1(5) . . . . ? Ce N3 C30 P3 43.7(4) . . . . ? O31 P3 C30 N3 -17.3(4) . . . . ? O32 P3 C30 N3 -144.3(4) . . . . ? C31 P3 C30 N3 100.5(4) . . . . ? O31 P3 C31 C36 -23.0(5) . . . . ? O32 P3 C31 C36 103.5(5) . . . . ? C30 P3 C31 C36 -140.2(5) . . . . ? O31 P3 C31 C32 166.4(5) . . . . ? O32 P3 C31 C32 -67.2(5) . . . . ? C30 P3 C31 C32 49.1(5) . . . . ? C36 C31 C32 C33 -1.8(9) . . . . ? P3 C31 C32 C33 168.8(5) . . . . ? C31 C32 C33 C34 -1.0(9) . . . . ? C32 C33 C34 C35 2.5(10) . . . . ? C33 C34 C35 C36 -1.3(10) . . . . ? C32 C31 C36 C35 3.0(9) . . . . ? P3 C31 C36 C35 -167.7(5) . . . . ? C34 C35 C36 C31 -1.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.790 _diffrn_reflns_theta_full 30.67 _diffrn_measured_fraction_theta_full 0.790 _refine_diff_density_max 4.514 _refine_diff_density_min -1.923 _refine_diff_density_rms 0.297