# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 Eu2 N5 O26 P3' _chemical_formula_weight 1489.79 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' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2391(9) _cell_length_b 16.2140(9) _cell_length_c 18.1327(10) _cell_angle_alpha 106.807(5) _cell_angle_beta 103.456(6) _cell_angle_gamma 105.134(6) _cell_volume 3134.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour WHITE _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 2.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8145 _exptl_absorpt_correction_T_max 0.8145 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Brucker SMART APEX' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12301 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1464 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12301 _reflns_number_gt 8037 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material PUBLCIF _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. All H atoms were placed geometrically, with C---H = 0.93 (aromatic) , and refined using a riding-atom model, with Uiso(H) = 1.2Ueq(C). Structure refinement after modification of the data for the non-coordinate lattice solvent molecules with the SQUEEZE routine of PLATON led to better refinement and data convergence. In the final refinement of the crystal structures, all of the heavy metal atoms were refined anisotropically. The organic hydrogen atoms were generated geometrically. The hydrogen atoms were placed in idealised positions and refined using a riding model to the atom to which they were attached. In furthur, the two-fold disorder model of Cd3, O5 and O6 atoms in the crystal structure were set up with the total occupancy of 1. The O2, O5, O17, C3, C4, C7, C11, C15, C22, C35, C38, C39, C42 and coordinated aqua molecules were refined isotropically due to the instability of their anisotropic refinements. The atomic displacement parameters for the O5W, O6W and O7W positions were restrained. The plane of two cyclotriphosphazene rings were refined into the same plane separately .The missing hydrogen atoms and solvent molecules that cannot be located in the Fourier difference map and squeezedd out by PLATON routine were added to the formula in the final cycles of refinement. Calculated with EA and TGA data, the solvent molecules should be two aqua and DMF molecules. The whole formula should be C48 H56 Cd3 N5 O29 P3. Associated changes in formula weight, density, mu and F000 may account for the difference in calculated values and reported ones. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12301 _refine_ls_number_parameters 733 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2274 _refine_ls_wR_factor_gt 0.1950 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu -0.81833(5) 0.07511(3) -0.45961(3) 0.01800(17) Uani 1 1 d . . . Eu2 Eu 0.84623(5) 0.52050(4) 0.45226(3) 0.01843(17) Uani 1 1 d . . . P1 P -0.1372(3) 0.15872(19) -0.01103(17) 0.0228(6) Uani 1 1 d . . . P2 P 0.0962(3) 0.16759(19) 0.02424(16) 0.0198(6) Uani 1 1 d . . . P3 P 0.0358(3) 0.31337(19) -0.00191(17) 0.0267(7) Uani 1 1 d . . . O1 O -0.6605(7) 0.1524(5) -0.3194(5) 0.0285(19) Uani 1 1 d . . . O1W O -0.6608(8) 0.1481(6) -0.5065(5) 0.035(2) Uani 1 1 d U . . O2 O -0.6394(7) 0.0349(5) -0.4057(4) 0.0243(17) Uani 1 1 d . . . O2W O -0.7779(7) 0.2379(5) -0.4062(5) 0.0252(18) Uani 1 1 d . . . O3 O -0.2307(8) 0.0855(5) -0.0945(4) 0.031(2) Uani 1 1 d . . . O3W O 0.6718(10) 0.5476(8) 0.4905(6) 0.064(3) Uani 1 1 d . . . O4 O -0.0614(7) 0.4070(5) 0.4222(4) 0.0209(16) Uani 1 1 d . . . O4W O 0.8009(9) 0.6353(7) 0.4033(5) 0.046(2) Uani 1 1 d U . . O5 O 0.0646(8) 0.3334(5) 0.4274(4) 0.033(2) Uani 1 1 d . . . O6 O -0.2193(7) 0.1537(5) 0.0464(4) 0.0241(17) Uani 1 1 d . . . O7 O 0.7031(7) 0.4435(5) 0.3116(4) 0.0232(17) Uani 1 1 d . . . O8 O 0.6730(8) 0.3707(7) 0.3940(5) 0.051(3) Uani 1 1 d . . . O9 O 0.1662(7) 0.1732(5) 0.1111(4) 0.0248(18) Uani 1 1 d . . . O10 O 0.1259(7) -0.0359(5) -0.3971(4) 0.0246(18) Uani 1 1 d . . . O11 O -0.0698(7) -0.0908(5) -0.4183(4) 0.0215(17) Uani 1 1 d U . . O12 O 0.1506(7) 0.1040(5) -0.0287(4) 0.0199(16) Uani 1 1 d . . . O13 O 0.0074(7) 0.0861(5) -0.4247(4) 0.0260(18) Uani 1 1 d . . . O14 O -0.1847(7) 0.0574(5) -0.4376(4) 0.0286(18) Uani 1 1 d . . . O15 O 0.0438(9) 0.3472(5) -0.0748(5) 0.036(2) Uani 1 1 d . . . O16 O 0.1575(7) 0.5354(5) 0.4391(4) 0.0285(19) Uani 1 1 d . . . O17 O -0.0037(7) 0.5713(5) 0.3950(4) 0.0210(17) Uani 1 1 d . . . O18 O 0.0820(9) 0.4154(5) 0.0598(4) 0.037(2) Uani 1 1 d . . . N1 N -0.0375(8) 0.1172(6) 0.0096(5) 0.0187(19) Uani 1 1 d U . . N2 N 0.1292(8) 0.2647(6) 0.0151(5) 0.024(2) Uani 1 1 d . . . N3 N -0.0971(10) 0.2587(6) -0.0122(5) 0.028(2) Uani 1 1 d . . . C1 C -0.6061(9) 0.0958(7) -0.3343(7) 0.020(2) Uani 1 1 d . . . C2 C -0.5028(9) 0.1025(7) -0.2693(6) 0.020(2) Uani 1 1 d . . . C3 C -0.4752(10) 0.1531(8) -0.1906(7) 0.028(3) Uani 1 1 d . . . H3A H -0.5201 0.1893 -0.1759 0.034 Uiso 1 1 calc R . . C4 C -0.3800(12) 0.1537(9) -0.1287(7) 0.036(3) Uani 1 1 d . . . H4B H -0.3590 0.1925 -0.0746 0.044 Uiso 1 1 calc R . . C5 C -0.3199(10) 0.0962(8) -0.1504(7) 0.023(2) Uani 1 1 d . . . C6 C -0.3477(11) 0.0407(8) -0.2313(7) 0.033(3) Uani 1 1 d . . . H6B H -0.3069 0.0008 -0.2454 0.040 Uiso 1 1 calc R . . C7 C -0.4383(10) 0.0456(7) -0.2915(7) 0.021(2) Uani 1 1 d U . . H7A H -0.4554 0.0110 -0.3463 0.025 Uiso 1 1 calc R . . C8 C -0.0227(12) 0.3469(8) 0.3866(7) 0.031(3) Uani 1 1 d . . . C9 C -0.0764(10) 0.2930(7) 0.2964(6) 0.019(2) Uani 1 1 d U . . C10 C -0.1516(11) 0.3229(7) 0.2476(7) 0.029(3) Uani 1 1 d . . . H10A H -0.1710 0.3737 0.2714 0.034 Uiso 1 1 calc R . . C11 C -0.1972(11) 0.2757(8) 0.1632(7) 0.028(3) Uani 1 1 d . . . H11M H -0.2480 0.2944 0.1302 0.033 Uiso 1 1 calc R . . C12 C -0.1674(9) 0.2035(7) 0.1299(6) 0.018(2) Uani 1 1 d . . . C13 C -0.0895(10) 0.1730(7) 0.1772(6) 0.021(2) Uani 1 1 d . . . H13A H -0.0702 0.1225 0.1527 0.025 Uiso 1 1 calc R . . C14 C -0.0428(11) 0.2201(7) 0.2610(7) 0.026(3) Uani 1 1 d . . . H14A H 0.0109 0.2030 0.2933 0.031 Uiso 1 1 calc R . . C15 C 0.6346(12) 0.3813(9) 0.3260(7) 0.035(3) Uani 1 1 d . . . C16 C 0.5170(11) 0.3242(8) 0.2694(7) 0.034(3) Uani 1 1 d . . . C17 C 0.4295(12) 0.2810(10) 0.2945(8) 0.047(4) Uani 1 1 d . . . H17A H 0.4472 0.2857 0.3486 0.056 Uiso 1 1 calc R . . C18 C 0.3109(11) 0.2287(9) 0.2380(7) 0.037(3) Uani 1 1 d . . . H18A H 0.2516 0.1987 0.2550 0.044 Uiso 1 1 calc R . . C19 C 0.2854(9) 0.2229(7) 0.1596(6) 0.020(2) Uani 1 1 d . . . C20 C 0.3692(11) 0.2650(9) 0.1336(7) 0.033(3) Uani 1 1 d U . . H20A H 0.3495 0.2612 0.0796 0.039 Uiso 1 1 calc R . . C21 C 0.4881(10) 0.3156(8) 0.1881(7) 0.032(3) Uani 1 1 d . . . H21A H 0.5470 0.3430 0.1695 0.038 Uiso 1 1 calc R . . C22 C 0.0359(11) -0.0486(7) -0.3727(7) 0.022(2) Uani 1 1 d . . . C23 C 0.0623(10) -0.0100(7) -0.2808(6) 0.020(2) Uani 1 1 d . . . C24 C 0.1821(11) 0.0353(8) -0.2291(7) 0.027(3) Uani 1 1 d . . . H24A H 0.2440 0.0371 -0.2509 0.033 Uiso 1 1 calc R . . C25 C 0.2087(11) 0.0779(8) -0.1446(7) 0.027(3) Uani 1 1 d . . . H25A H 0.2874 0.1120 -0.1103 0.032 Uiso 1 1 calc R . . C26 C 0.1172(10) 0.0682(7) -0.1143(6) 0.019(2) Uani 1 1 d . . . C27 C -0.0037(10) 0.0213(7) -0.1642(7) 0.024(2) Uani 1 1 d . . . H27A H -0.0653 0.0161 -0.1420 0.029 Uiso 1 1 calc R . . C28 C -0.0277(11) -0.0170(8) -0.2482(7) 0.026(3) Uani 1 1 d . . . H28A H -0.1069 -0.0481 -0.2827 0.031 Uiso 1 1 calc R . . C29 C -0.0721(10) 0.1014(7) -0.3974(6) 0.017(2) Uani 1 1 d . . . C30 C -0.0405(10) 0.1694(7) -0.3134(6) 0.018(2) Uani 1 1 d U . . C31 C 0.0142(12) 0.2825(7) -0.1565(6) 0.025(3) Uani 1 1 d . . . C32 C -0.1048(12) 0.2447(8) -0.2063(7) 0.030(3) Uani 1 1 d . . . H32A H -0.1647 0.2577 -0.1868 0.036 Uiso 1 1 calc R . . C33 C -0.1309(12) 0.1883(8) -0.2841(7) 0.032(3) Uani 1 1 d . . . H33A H -0.2102 0.1617 -0.3189 0.038 Uiso 1 1 calc R . . C34 C 0.1058(11) 0.2667(7) -0.1815(6) 0.026(3) Uani 1 1 d . . . H34A H 0.1845 0.2933 -0.1457 0.031 Uiso 1 1 calc R . . C35 C 0.0790(10) 0.2106(8) -0.2606(7) 0.026(3) Uani 1 1 d . . . H35A H 0.1401 0.1997 -0.2797 0.032 Uiso 1 1 calc R . . C36 C 0.0792(10) 0.5419(7) 0.3841(6) 0.023(2) Uani 1 1 d . . . C37 C 0.1502(11) 0.4557(8) 0.2792(7) 0.031(3) Uani 1 1 d . . . H37A H 0.1961 0.4416 0.3191 0.037 Uiso 1 1 calc R . . C38 C 0.0853(10) 0.5112(7) 0.2994(6) 0.020(2) Uani 1 1 d . . . C39 C 0.0190(12) 0.5350(7) 0.2391(6) 0.032(3) Uani 1 1 d . . . H39A H -0.0225 0.5744 0.2530 0.038 Uiso 1 1 calc R . . C40 C 0.0162(13) 0.4994(8) 0.1594(7) 0.036(3) Uani 1 1 d . . . H40A H -0.0293 0.5126 0.1186 0.043 Uiso 1 1 calc R . . C41 C 0.0813(12) 0.4447(7) 0.1420(7) 0.029(3) Uani 1 1 d . . . C42 C 0.1467(11) 0.4208(8) 0.1986(7) 0.028(3) Uani 1 1 d . . . H42A H 0.1882 0.3817 0.1837 0.034 Uiso 1 1 calc R . . N4 N -0.6970(10) -0.1505(7) -0.4236(7) 0.041(3) Uani 1 1 d . . . H4A H -0.6443 -0.1112 -0.4323 0.049 Uiso 1 1 d R . . C43 C -0.6947(13) -0.1515(10) -0.3431(9) 0.051(4) Uani 1 1 d . . . H11A H -0.6293 -0.0990 -0.3018 0.076 Uiso 1 1 calc R . . H11B H -0.6842 -0.2068 -0.3391 0.076 Uiso 1 1 calc R . . H11C H -0.7690 -0.1492 -0.3354 0.076 Uiso 1 1 calc R . . C44 C -0.8099(14) -0.2286(9) -0.4922(10) 0.060(5) Uani 1 1 d . . . H11D H -0.8808 -0.2247 -0.4796 0.090 Uiso 1 1 calc R . . H11E H -0.8039 -0.2874 -0.4955 0.090 Uiso 1 1 calc R . . H11F H -0.8144 -0.2219 -0.5436 0.090 Uiso 1 1 calc R . . N6 N -0.5122(16) 0.3561(10) -0.3519(9) 0.083(5) Uani 1 1 d . . . H6A H -0.5686 0.3251 -0.3982 0.099 Uiso 1 1 d R . . C45 C -0.4983(15) 0.4448(14) -0.3052(13) 0.084(7) Uani 1 1 d . . . H11G H -0.5648 0.4602 -0.3295 0.127 Uiso 1 1 calc R . . H11H H -0.4249 0.4871 -0.3029 0.127 Uiso 1 1 calc R . . H11I H -0.4955 0.4487 -0.2509 0.127 Uiso 1 1 calc R . . C48 C -0.4331(17) 0.3175(11) -0.3173(11) 0.070(5) Uani 1 1 d . . . H11J H -0.4720 0.2519 -0.3369 0.105 Uiso 1 1 calc R . . H11K H -0.4110 0.3427 -0.2588 0.105 Uiso 1 1 calc R . . H11L H -0.3623 0.3315 -0.3325 0.105 Uiso 1 1 calc R . . O5W O 0.7309(11) 0.7333(9) 0.5788(7) 0.072(4) Uani 1 1 d . . . O6W O -0.7146(13) 0.4492(9) -0.2109(8) 0.091(4) Uiso 1 1 d . . . O7W O -0.4124(14) 0.3778(10) -0.4653(9) 0.100(4) Uiso 1 1 d . . . O8W O -0.6105(10) 0.3193(7) -0.1896(6) 0.062(3) Uani 1 1 d . . . 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 Eu1 0.0171(3) 0.0257(3) 0.0090(3) 0.0017(2) 0.0020(2) 0.0116(2) Eu2 0.0159(3) 0.0283(3) 0.0119(3) 0.0068(2) 0.0033(2) 0.0111(2) P1 0.0278(17) 0.0283(15) 0.0083(14) 0.0018(11) -0.0006(13) 0.0152(13) P2 0.0235(16) 0.0245(14) 0.0081(14) 0.0034(11) 0.0018(12) 0.0092(12) P3 0.049(2) 0.0219(15) 0.0099(15) 0.0036(12) 0.0083(15) 0.0173(14) O1 0.028(5) 0.018(4) 0.031(5) 0.004(3) 0.000(4) 0.009(3) O1W 0.036(5) 0.049(5) 0.016(4) 0.015(4) 0.002(4) 0.011(4) O2 0.022(4) 0.035(4) 0.010(4) 0.001(3) -0.003(3) 0.015(4) O2W 0.027(5) 0.026(4) 0.023(4) 0.003(3) 0.007(4) 0.017(3) O3 0.037(5) 0.036(4) 0.008(4) -0.002(3) -0.010(4) 0.022(4) O3W 0.076(8) 0.116(9) 0.058(7) 0.060(7) 0.047(6) 0.073(7) O4 0.028(5) 0.022(4) 0.008(4) -0.002(3) 0.005(3) 0.009(3) O4W 0.049(5) 0.072(6) 0.021(4) 0.014(4) 0.002(4) 0.040(5) O5 0.054(6) 0.042(5) 0.008(4) 0.005(3) 0.004(4) 0.034(5) O6 0.019(4) 0.036(4) 0.007(4) -0.004(3) -0.001(3) 0.011(3) O7 0.016(4) 0.032(4) 0.011(4) 0.003(3) 0.000(3) 0.001(3) O8 0.034(6) 0.071(7) 0.028(5) 0.032(5) -0.006(4) -0.010(5) O9 0.021(4) 0.036(4) 0.007(4) 0.008(3) -0.001(3) 0.001(3) O10 0.032(5) 0.028(4) 0.013(4) 0.005(3) 0.004(4) 0.014(4) O11 0.020(4) 0.028(4) 0.007(4) 0.003(3) -0.006(3) 0.008(3) O12 0.023(4) 0.030(4) 0.005(4) 0.002(3) 0.000(3) 0.015(3) O13 0.034(5) 0.030(4) 0.015(4) 0.004(3) 0.011(4) 0.017(4) O14 0.027(5) 0.038(5) 0.013(4) -0.001(3) 0.001(4) 0.015(4) O15 0.070(7) 0.029(4) 0.015(4) 0.012(3) 0.016(4) 0.021(4) O16 0.026(5) 0.045(5) 0.011(4) 0.009(4) 0.000(4) 0.014(4) O17 0.028(5) 0.024(4) 0.012(4) 0.009(3) 0.006(4) 0.009(3) O18 0.082(7) 0.022(4) 0.009(4) 0.006(3) 0.019(4) 0.016(4) N1 0.021(5) 0.021(4) 0.007(4) 0.002(3) -0.004(3) 0.009(4) N2 0.019(5) 0.024(5) 0.017(5) 0.000(4) -0.003(4) 0.007(4) N3 0.047(7) 0.024(5) 0.012(5) 0.001(4) 0.005(5) 0.019(5) C1 0.012(6) 0.022(5) 0.018(6) 0.007(5) -0.001(5) 0.002(4) C2 0.013(6) 0.031(6) 0.013(6) 0.006(5) 0.001(5) 0.008(5) C3 0.025(7) 0.045(7) 0.022(7) 0.008(5) 0.008(5) 0.029(6) C4 0.044(9) 0.045(7) 0.016(7) -0.001(5) 0.005(6) 0.027(7) C5 0.015(6) 0.042(7) 0.013(6) 0.007(5) 0.002(5) 0.015(5) C6 0.029(7) 0.038(7) 0.016(6) -0.007(5) -0.005(6) 0.017(6) C7 0.019(4) 0.026(4) 0.012(4) 0.002(3) 0.001(3) 0.012(3) C8 0.047(8) 0.023(6) 0.022(7) 0.011(5) 0.013(6) 0.006(6) C9 0.030(6) 0.025(5) 0.011(5) 0.013(4) 0.008(4) 0.015(4) C10 0.043(8) 0.018(5) 0.016(6) -0.003(4) 0.005(6) 0.013(5) C11 0.033(7) 0.039(7) 0.018(6) 0.012(5) 0.011(6) 0.021(6) C12 0.010(5) 0.023(5) 0.009(5) -0.001(4) -0.004(4) 0.001(4) C13 0.032(7) 0.026(6) 0.012(6) 0.005(4) 0.009(5) 0.020(5) C14 0.040(7) 0.017(5) 0.022(6) 0.010(5) 0.006(6) 0.013(5) C15 0.030(7) 0.049(8) 0.012(6) 0.009(6) 0.001(6) 0.004(6) C16 0.025(7) 0.040(7) 0.029(7) 0.019(6) 0.002(6) 0.000(6) C17 0.023(7) 0.081(11) 0.015(7) 0.020(7) -0.004(6) -0.008(7) C18 0.018(6) 0.062(9) 0.019(7) 0.022(6) -0.004(5) 0.000(6) C19 0.011(5) 0.021(5) 0.014(6) -0.001(4) -0.005(5) 0.003(4) C20 0.026(6) 0.049(6) 0.014(5) 0.009(5) 0.003(5) 0.005(5) C21 0.013(6) 0.051(8) 0.013(6) 0.005(5) 0.000(5) -0.002(5) C22 0.031(7) 0.025(6) 0.019(6) 0.012(5) 0.011(6) 0.018(5) C23 0.032(7) 0.013(5) 0.013(6) 0.000(4) 0.007(5) 0.010(5) C24 0.028(7) 0.039(7) 0.011(6) 0.008(5) 0.005(5) 0.010(5) C25 0.031(7) 0.035(6) 0.015(6) 0.011(5) 0.005(5) 0.013(5) C26 0.027(6) 0.025(5) 0.014(6) 0.011(4) 0.006(5) 0.020(5) C27 0.024(6) 0.032(6) 0.018(6) 0.010(5) 0.004(5) 0.015(5) C28 0.025(7) 0.031(6) 0.022(7) 0.006(5) 0.007(5) 0.017(5) C29 0.026(6) 0.024(5) 0.012(6) 0.011(4) 0.012(5) 0.014(5) C30 0.020(5) 0.020(5) 0.006(5) 0.000(4) 0.004(4) 0.002(4) C31 0.047(8) 0.019(5) 0.008(6) 0.005(4) 0.011(6) 0.007(5) C32 0.051(9) 0.034(6) 0.018(6) 0.012(5) 0.016(6) 0.028(6) C33 0.031(7) 0.041(7) 0.024(7) 0.006(5) 0.008(6) 0.022(6) C34 0.039(8) 0.015(5) 0.013(6) -0.004(4) 0.003(5) 0.008(5) C35 0.017(6) 0.036(6) 0.018(6) 0.008(5) 0.001(5) 0.004(5) C36 0.027(7) 0.024(6) 0.011(6) 0.004(5) 0.005(5) 0.002(5) C37 0.038(8) 0.047(7) 0.017(6) 0.019(6) 0.005(6) 0.024(6) C38 0.021(6) 0.023(5) 0.019(6) 0.007(4) 0.010(5) 0.013(5) C39 0.062(9) 0.017(6) 0.012(6) 0.004(4) 0.006(6) 0.015(6) C40 0.065(10) 0.030(6) 0.013(6) 0.006(5) 0.005(6) 0.024(7) C41 0.055(9) 0.025(6) 0.013(6) 0.009(5) 0.019(6) 0.016(6) C42 0.030(7) 0.039(7) 0.021(7) 0.009(5) 0.017(6) 0.016(6) N4 0.040(7) 0.032(6) 0.042(7) 0.009(5) 0.016(6) 0.001(5) C43 0.048(10) 0.045(8) 0.063(10) 0.019(8) 0.041(9) 0.006(7) C44 0.053(10) 0.037(8) 0.088(13) 0.026(8) 0.011(10) 0.019(8) N6 0.104(14) 0.059(9) 0.061(10) 0.012(8) -0.010(9) 0.037(9) C45 0.030(10) 0.129(19) 0.123(18) 0.076(16) 0.027(11) 0.040(11) C48 0.077(13) 0.054(10) 0.078(13) 0.039(9) 0.009(11) 0.021(9) O5W 0.078(9) 0.143(11) 0.061(7) 0.073(8) 0.057(7) 0.073(8) O8W 0.059(8) 0.056(7) 0.054(7) 0.008(5) 0.011(6) 0.014(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 Eu1 O13 2.397(8) 1_455 ? Eu1 O2W 2.401(7) . ? Eu1 O14 2.419(8) 2_454 ? Eu1 O10 2.427(7) 1_455 ? Eu1 O11 2.436(7) 2_454 ? Eu1 O1W 2.449(8) . ? Eu1 O2 2.508(7) . ? Eu1 O1 2.525(8) . ? Eu1 O13 2.828(8) 2_454 ? Eu1 C1 2.894(10) . ? Eu1 C29 2.966(11) 2_454 ? Eu1 Eu1 4.1356(12) 2_354 ? Eu2 O17 2.392(7) 1_655 ? Eu2 O16 2.399(7) 2_666 ? Eu2 O4 2.399(7) 1_655 ? Eu2 O4W 2.414(9) . ? Eu2 O7 2.464(7) . ? Eu2 O5 2.474(8) 2_666 ? Eu2 O3W 2.497(10) . ? Eu2 O8 2.509(9) . ? Eu2 O4 2.747(7) 2_666 ? Eu2 C15 2.871(12) . ? Eu2 C8 2.972(12) 2_666 ? Eu2 Eu2 4.0678(11) 2_766 ? P1 N1 1.564(9) . ? P1 O3 1.567(8) . ? P1 N3 1.575(9) . ? P1 O6 1.609(8) . ? P2 N1 1.546(9) . ? P2 O9 1.572(7) . ? P2 O12 1.584(8) . ? P2 N2 1.587(9) . ? P3 O18 1.566(8) . ? P3 N2 1.573(9) . ? P3 N3 1.573(11) . ? P3 O15 1.584(7) . ? O1 C1 1.272(13) . ? O2 C1 1.274(13) . ? O3 C5 1.390(12) . ? O4 C8 1.269(14) . ? O4 Eu2 2.399(7) 1_455 ? O4 Eu2 2.747(7) 2_666 ? O5 C8 1.259(15) . ? O5 Eu2 2.474(8) 2_666 ? O6 C12 1.388(12) . ? O7 C15 1.266(14) . ? O8 C15 1.290(13) . ? O9 C19 1.390(12) . ? O10 C22 1.270(13) . ? O10 Eu1 2.427(7) 1_655 ? O11 C22 1.241(13) . ? O11 Eu1 2.436(7) 2_454 ? O12 C26 1.405(12) . ? O13 C29 1.237(13) . ? O13 Eu1 2.397(8) 1_655 ? O13 Eu1 2.828(8) 2_454 ? O14 C29 1.288(13) . ? O14 Eu1 2.419(8) 2_454 ? O15 C31 1.442(13) . ? O16 C36 1.263(13) . ? O16 Eu2 2.399(7) 2_666 ? O17 C36 1.260(14) . ? O17 Eu2 2.392(7) 1_455 ? O18 C41 1.431(12) . ? C1 C2 1.470(14) . ? C2 C3 1.333(15) . ? C2 C7 1.397(15) . ? C3 C4 1.412(16) . ? C3 H3A 0.9300 . ? C4 C5 1.359(16) . ? C4 H4B 0.9300 . ? C5 C6 1.387(15) . ? C6 C7 1.400(15) . ? C6 H6B 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.498(15) . ? C8 Eu2 2.972(12) 2_666 ? C9 C14 1.384(15) . ? C9 C10 1.402(15) . ? C10 C11 1.395(15) . ? C10 H10A 0.9300 . ? C11 C12 1.336(15) . ? C11 H11M 0.9300 . ? C12 C13 1.415(14) . ? C13 C14 1.383(15) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.431(17) . ? C16 C17 1.366(17) . ? C16 C21 1.388(15) . ? C17 C18 1.427(16) . ? C17 H17A 0.9300 . ? C18 C19 1.352(15) . ? C18 H18A 0.9300 . ? C19 C20 1.337(16) . ? C20 C21 1.416(16) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.521(15) . ? C23 C28 1.361(16) . ? C23 C24 1.403(16) . ? C24 C25 1.402(15) . ? C24 H24A 0.9300 . ? C25 C26 1.351(16) . ? C25 H25A 0.9300 . ? C26 C27 1.406(15) . ? C27 C28 1.392(15) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C30 1.489(14) . ? C29 Eu1 2.966(11) 2_454 ? C30 C33 1.398(16) . ? C30 C35 1.404(15) . ? C31 C34 1.359(17) . ? C31 C32 1.383(17) . ? C32 C33 1.350(16) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.365(15) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 C38 1.497(15) . ? C37 C38 1.376(16) . ? C37 C42 1.391(16) . ? C37 H37A 0.9300 . ? C38 C39 1.414(15) . ? C39 C40 1.381(16) . ? C39 H39A 0.9300 . ? C40 C41 1.359(17) . ? C40 H40A 0.9300 . ? C41 C42 1.362(16) . ? C42 H42A 0.9300 . ? N4 C43 1.459(16) . ? N4 C44 1.561(18) . ? N4 H4A 0.8589 . ? C43 H11A 0.9600 . ? C43 H11B 0.9600 . ? C43 H11C 0.9600 . ? C44 H11D 0.9600 . ? C44 H11E 0.9600 . ? C44 H11F 0.9600 . ? N6 C45 1.38(2) . ? N6 C48 1.41(2) . ? N6 H6A 0.8597 . ? C45 H11G 0.9600 . ? C45 H11H 0.9600 . ? C45 H11I 0.9600 . ? C48 H11J 0.9600 . ? C48 H11K 0.9600 . ? C48 H11L 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 O13 Eu1 O2W 76.5(3) 1_455 . ? O13 Eu1 O14 124.5(3) 1_455 2_454 ? O2W Eu1 O14 149.0(3) . 2_454 ? O13 Eu1 O10 71.8(3) 1_455 1_455 ? O2W Eu1 O10 128.5(3) . 1_455 ? O14 Eu1 O10 82.2(3) 2_454 1_455 ? O13 Eu1 O11 80.7(3) 1_455 2_454 ? O2W Eu1 O11 80.7(2) . 2_454 ? O14 Eu1 O11 80.8(2) 2_454 2_454 ? O10 Eu1 O11 130.7(2) 1_455 2_454 ? O13 Eu1 O1W 144.0(3) 1_455 . ? O2W Eu1 O1W 72.6(3) . . ? O14 Eu1 O1W 79.0(3) 2_454 . ? O10 Eu1 O1W 143.4(3) 1_455 . ? O11 Eu1 O1W 76.6(3) 2_454 . ? O13 Eu1 O2 137.0(2) 1_455 . ? O2W Eu1 O2 112.3(3) . . ? O14 Eu1 O2 69.8(2) 2_454 . ? O10 Eu1 O2 70.8(3) 1_455 . ? O11 Eu1 O2 141.1(3) 2_454 . ? O1W Eu1 O2 73.2(3) . . ? O13 Eu1 O1 100.1(3) 1_455 . ? O2W Eu1 O1 68.6(2) . . ? O14 Eu1 O1 121.8(2) 2_454 . ? O10 Eu1 O1 78.3(2) 1_455 . ? O11 Eu1 O1 148.0(2) 2_454 . ? O1W Eu1 O1 85.4(3) . . ? O2 Eu1 O1 52.0(2) . . ? O13 Eu1 O13 75.7(3) 1_455 2_454 ? O2W Eu1 O13 138.0(2) . 2_454 ? O14 Eu1 O13 49.2(3) 2_454 2_454 ? O10 Eu1 O13 69.6(2) 1_455 2_454 ? O11 Eu1 O13 64.3(2) 2_454 2_454 ? O1W Eu1 O13 117.4(2) . 2_454 ? O2 Eu1 O13 109.6(2) . 2_454 ? O1 Eu1 O13 147.3(2) . 2_454 ? O13 Eu1 C1 119.4(3) 1_455 . ? O2W Eu1 C1 91.1(3) . . ? O14 Eu1 C1 95.8(3) 2_454 . ? O10 Eu1 C1 71.5(3) 1_455 . ? O11 Eu1 C1 156.0(3) 2_454 . ? O1W Eu1 C1 79.4(3) . . ? O2 Eu1 C1 26.0(3) . . ? O1 Eu1 C1 26.0(3) . . ? O13 Eu1 C1 130.1(2) 2_454 . ? O13 Eu1 C29 100.2(3) 1_455 2_454 ? O2W Eu1 C29 148.2(2) . 2_454 ? O14 Eu1 C29 25.1(3) 2_454 2_454 ? O10 Eu1 C29 77.8(2) 1_455 2_454 ? O11 Eu1 C29 67.6(2) 2_454 2_454 ? O1W Eu1 C29 96.6(3) . 2_454 ? O2 Eu1 C29 91.9(3) . 2_454 ? O1 Eu1 C29 141.8(2) . 2_454 ? O13 Eu1 C29 24.5(3) 2_454 2_454 ? C1 Eu1 C29 116.8(3) . 2_454 ? O13 Eu1 Eu1 41.49(18) 1_455 2_354 ? O2W Eu1 Eu1 111.87(19) . 2_354 ? O14 Eu1 Eu1 83.2(2) 2_454 2_354 ? O10 Eu1 Eu1 65.19(18) 1_455 2_354 ? O11 Eu1 Eu1 67.05(18) 2_454 2_354 ? O1W Eu1 Eu1 141.57(18) . 2_354 ? O2 Eu1 Eu1 130.78(18) . 2_354 ? O1 Eu1 Eu1 132.62(19) . 2_354 ? O13 Eu1 Eu1 34.16(16) 2_454 2_354 ? C1 Eu1 Eu1 136.5(2) . 2_354 ? C29 Eu1 Eu1 58.7(2) 2_454 2_354 ? O17 Eu2 O16 134.5(3) 1_655 2_666 ? O17 Eu2 O4 71.2(2) 1_655 1_655 ? O16 Eu2 O4 78.3(3) 2_666 1_655 ? O17 Eu2 O4W 73.1(3) 1_655 . ? O16 Eu2 O4W 142.1(3) 2_666 . ? O4 Eu2 O4W 139.5(3) 1_655 . ? O17 Eu2 O7 87.3(2) 1_655 . ? O16 Eu2 O7 125.4(3) 2_666 . ? O4 Eu2 O7 88.8(2) 1_655 . ? O4W Eu2 O7 70.9(3) . . ? O17 Eu2 O5 91.5(3) 1_655 2_666 ? O16 Eu2 O5 79.0(3) 2_666 2_666 ? O4 Eu2 O5 124.9(3) 1_655 2_666 ? O4W Eu2 O5 74.3(3) . 2_666 ? O7 Eu2 O5 143.9(2) . 2_666 ? O17 Eu2 O3W 144.8(3) 1_655 . ? O16 Eu2 O3W 75.7(3) 2_666 . ? O4 Eu2 O3W 142.8(3) 1_655 . ? O4W Eu2 O3W 71.9(3) . . ? O7 Eu2 O3W 85.2(3) . . ? O5 Eu2 O3W 75.2(4) 2_666 . ? O17 Eu2 O8 128.2(3) 1_655 . ? O16 Eu2 O8 73.1(3) 2_666 . ? O4 Eu2 O8 76.4(3) 1_655 . ? O4W Eu2 O8 112.9(3) . . ? O7 Eu2 O8 52.3(2) . . ? O5 Eu2 O8 140.2(3) 2_666 . ? O3W Eu2 O8 70.8(4) . . ? O17 Eu2 O4 74.2(2) 1_655 2_666 ? O16 Eu2 O4 66.0(2) 2_666 2_666 ? O4 Eu2 O4 75.7(2) 1_655 2_666 ? O4W Eu2 O4 112.0(3) . 2_666 ? O7 Eu2 O4 158.9(2) . 2_666 ? O5 Eu2 O4 49.1(2) 2_666 2_666 ? O3W Eu2 O4 115.9(3) . 2_666 ? O8 Eu2 O4 134.1(2) . 2_666 ? O17 Eu2 C15 110.3(3) 1_655 . ? O16 Eu2 C15 99.5(3) 2_666 . ? O4 Eu2 C15 85.0(3) 1_655 . ? O4W Eu2 C15 89.8(3) . . ? O7 Eu2 C15 26.0(3) . . ? O5 Eu2 C15 148.2(4) 2_666 . ? O3W Eu2 C15 73.7(4) . . ? O8 Eu2 C15 26.7(3) . . ? O4 Eu2 C15 157.8(3) 2_666 . ? O17 Eu2 C8 86.5(3) 1_655 2_666 ? O16 Eu2 C8 66.6(3) 2_666 2_666 ? O4 Eu2 C8 100.5(3) 1_655 2_666 ? O4W Eu2 C8 95.8(3) . 2_666 ? O7 Eu2 C8 166.5(3) . 2_666 ? O5 Eu2 C8 24.6(3) 2_666 2_666 ? O3W Eu2 C8 93.0(4) . 2_666 ? O8 Eu2 C8 139.2(3) . 2_666 ? O4 Eu2 C8 25.3(3) 2_666 2_666 ? C15 Eu2 C8 163.2(3) . 2_666 ? O17 Eu2 Eu2 68.06(17) 1_655 2_766 ? O16 Eu2 Eu2 66.8(2) 2_666 2_766 ? O4 Eu2 Eu2 40.88(17) 1_655 2_766 ? O4W Eu2 Eu2 134.6(2) . 2_766 ? O7 Eu2 Eu2 128.11(19) . 2_766 ? O5 Eu2 Eu2 83.99(19) 2_666 2_766 ? O3W Eu2 Eu2 139.8(2) . 2_766 ? O8 Eu2 Eu2 109.4(2) . 2_766 ? O4 Eu2 Eu2 34.86(15) 2_666 2_766 ? C15 Eu2 Eu2 125.0(3) . 2_766 ? C8 Eu2 Eu2 59.8(3) 2_666 2_766 ? N1 P1 O3 104.8(4) . . ? N1 P1 N3 117.7(5) . . ? O3 P1 N3 112.6(5) . . ? N1 P1 O6 111.7(4) . . ? O3 P1 O6 99.6(4) . . ? N3 P1 O6 109.0(5) . . ? N1 P2 O9 105.3(4) . . ? N1 P2 O12 112.1(4) . . ? O9 P2 O12 98.8(4) . . ? N1 P2 N2 116.6(5) . . ? O9 P2 N2 112.7(4) . . ? O12 P2 N2 109.9(4) . . ? O18 P3 N2 112.0(5) . . ? O18 P3 N3 112.4(5) . . ? N2 P3 N3 116.0(5) . . ? O18 P3 O15 90.8(4) . . ? N2 P3 O15 110.6(5) . . ? N3 P3 O15 112.4(5) . . ? C1 O1 Eu1 93.4(6) . . ? C1 O2 Eu1 94.1(6) . . ? C5 O3 P1 128.8(7) . . ? C8 O4 Eu2 164.1(7) . 1_455 ? C8 O4 Eu2 87.3(7) . 2_666 ? Eu2 O4 Eu2 104.3(2) 1_455 2_666 ? C8 O5 Eu2 100.4(7) . 2_666 ? C12 O6 P1 119.2(7) . . ? C15 O7 Eu2 95.2(6) . . ? C15 O8 Eu2 92.5(7) . . ? C19 O9 P2 129.6(7) . . ? C22 O10 Eu1 124.1(6) . 1_655 ? C22 O11 Eu1 130.6(6) . 2_454 ? C26 O12 P2 126.8(6) . . ? C29 O13 Eu1 171.5(8) . 1_655 ? C29 O13 Eu1 84.0(6) . 2_454 ? Eu1 O13 Eu1 104.3(3) 1_655 2_454 ? C29 O14 Eu1 101.9(6) . 2_454 ? C31 O15 P3 121.2(6) . . ? C36 O16 Eu2 134.8(7) . 2_666 ? C36 O17 Eu2 129.6(6) . 1_455 ? C41 O18 P3 126.2(7) . . ? P2 N1 P1 123.1(5) . . ? P3 N2 P2 123.6(6) . . ? P1 N3 P3 122.6(6) . . ? O1 C1 O2 120.2(9) . . ? O1 C1 C2 119.6(10) . . ? O2 C1 C2 120.2(10) . . ? O1 C1 Eu1 60.6(5) . . ? O2 C1 Eu1 59.8(5) . . ? C2 C1 Eu1 176.7(7) . . ? C3 C2 C7 119.1(10) . . ? C3 C2 C1 123.5(10) . . ? C7 C2 C1 117.0(10) . . ? C2 C3 C4 122.4(10) . . ? C2 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? C5 C4 C3 118.2(11) . . ? C5 C4 H4B 120.9 . . ? C3 C4 H4B 120.9 . . ? C4 C5 C6 121.2(11) . . ? C4 C5 O3 123.6(10) . . ? C6 C5 O3 115.1(10) . . ? C5 C6 C7 118.9(11) . . ? C5 C6 H6B 120.5 . . ? C7 C6 H6B 120.5 . . ? C2 C7 C6 120.0(10) . . ? C2 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? O5 C8 O4 119.5(11) . . ? O5 C8 C9 118.9(11) . . ? O4 C8 C9 121.6(11) . . ? O5 C8 Eu2 55.0(6) . 2_666 ? O4 C8 Eu2 67.4(6) . 2_666 ? C9 C8 Eu2 160.4(8) . 2_666 ? C14 C9 C10 120.5(10) . . ? C14 C9 C8 120.1(10) . . ? C10 C9 C8 119.1(10) . . ? C11 C10 C9 119.4(10) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C12 C11 C10 119.6(10) . . ? C12 C11 H11M 120.2 . . ? C10 C11 H11M 120.2 . . ? C11 C12 O6 118.9(9) . . ? C11 C12 C13 122.4(10) . . ? O6 C12 C13 118.6(9) . . ? C14 C13 C12 118.4(10) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C9 C14 C13 119.7(10) . . ? C9 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? O7 C15 O8 118.2(11) . . ? O7 C15 C16 121.5(10) . . ? O8 C15 C16 120.3(11) . . ? O7 C15 Eu2 58.7(6) . . ? O8 C15 Eu2 60.8(6) . . ? C16 C15 Eu2 168.3(10) . . ? C17 C16 C21 118.5(11) . . ? C17 C16 C15 121.2(11) . . ? C21 C16 C15 120.2(10) . . ? C16 C17 C18 120.3(11) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C19 C18 C17 119.6(11) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C20 C19 C18 121.3(10) . . ? C20 C19 O9 124.2(10) . . ? C18 C19 O9 114.5(10) . . ? C19 C20 C21 120.0(11) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C16 C21 C20 120.2(11) . . ? C16 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? O11 C22 O10 124.5(10) . . ? O11 C22 C23 119.0(10) . . ? O10 C22 C23 116.6(10) . . ? C28 C23 C24 119.7(10) . . ? C28 C23 C22 121.4(10) . . ? C24 C23 C22 118.9(10) . . ? C25 C24 C23 120.1(11) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 118.4(11) . . ? C26 C25 H25A 120.8 . . ? C24 C25 H25A 120.8 . . ? C25 C26 C27 122.8(10) . . ? C25 C26 O12 115.6(10) . . ? C27 C26 O12 121.5(10) . . ? C28 C27 C26 117.4(11) . . ? C28 C27 H27A 121.3 . . ? C26 C27 H27A 121.3 . . ? C23 C28 C27 121.4(11) . . ? C23 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? O13 C29 O14 122.7(10) . . ? O13 C29 C30 120.7(10) . . ? O14 C29 C30 116.6(9) . . ? O13 C29 Eu1 71.5(6) . 2_454 ? O14 C29 Eu1 52.9(5) . 2_454 ? C30 C29 Eu1 160.1(7) . 2_454 ? C33 C30 C35 119.0(10) . . ? C33 C30 C29 120.2(10) . . ? C35 C30 C29 120.7(10) . . ? C34 C31 C32 124.0(10) . . ? C34 C31 O15 117.9(11) . . ? C32 C31 O15 118.0(11) . . ? C33 C32 C31 117.6(12) . . ? C33 C32 H32A 121.2 . . ? C31 C32 H32A 121.2 . . ? C32 C33 C30 121.1(12) . . ? C32 C33 H33A 119.5 . . ? C30 C33 H33A 119.5 . . ? C31 C34 C35 118.1(11) . . ? C31 C34 H34A 121.0 . . ? C35 C34 H34A 121.0 . . ? C34 C35 C30 120.3(11) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? O17 C36 O16 125.0(10) . . ? O17 C36 C38 118.0(10) . . ? O16 C36 C38 117.0(10) . . ? C38 C37 C42 119.6(10) . . ? C38 C37 H37A 120.2 . . ? C42 C37 H37A 120.2 . . ? C37 C38 C39 120.0(10) . . ? C37 C38 C36 120.0(10) . . ? C39 C38 C36 119.9(10) . . ? C40 C39 C38 119.6(11) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C41 C40 C39 118.5(11) . . ? C41 C40 H40A 120.8 . . ? C39 C40 H40A 120.8 . . ? C40 C41 C42 123.4(11) . . ? C40 C41 O18 116.0(10) . . ? C42 C41 O18 120.5(11) . . ? C41 C42 C37 118.8(11) . . ? C41 C42 H42A 120.6 . . ? C37 C42 H42A 120.6 . . ? C43 N4 C44 111.2(11) . . ? C43 N4 H4A 124.6 . . ? C44 N4 H4A 124.2 . . ? N4 C43 H11A 109.5 . . ? N4 C43 H11B 109.5 . . ? H11A C43 H11B 109.5 . . ? N4 C43 H11C 109.5 . . ? H11A C43 H11C 109.5 . . ? H11B C43 H11C 109.5 . . ? N4 C44 H11D 109.5 . . ? N4 C44 H11E 109.5 . . ? H11D C44 H11E 109.5 . . ? N4 C44 H11F 109.5 . . ? H11D C44 H11F 109.5 . . ? H11E C44 H11F 109.5 . . ? C45 N6 C48 116.3(14) . . ? C45 N6 H6A 121.9 . . ? C48 N6 H6A 121.8 . . ? N6 C45 H11G 109.5 . . ? N6 C45 H11H 109.5 . . ? H11G C45 H11H 109.5 . . ? N6 C45 H11I 109.5 . . ? H11G C45 H11I 109.5 . . ? H11H C45 H11I 109.5 . . ? N6 C48 H11J 109.5 . . ? N6 C48 H11K 109.5 . . ? H11J C48 H11K 109.5 . . ? N6 C48 H11L 109.5 . . ? H11J C48 H11L 109.5 . . ? H11K C48 H11L 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 6.096 _refine_diff_density_min -1.199 _refine_diff_density_rms 0.269 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.646 0.000 447.9 20.4 2 0.500 1.000 0.500 46.2 -3.6 3 0.452 0.148 0.373 9.5 2.4 4 0.547 0.852 0.627 9.5 3.5 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 926681' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H51 Eu2 N4 O28 P3' _chemical_formula_weight 1480.56 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 Orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 34.882(4) _cell_length_b 12.059(2) _cell_length_c 15.391(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6474.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 2.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6820 _exptl_absorpt_correction_T_max 0.8195 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Brucker SMART APEX' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6182 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1905 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6182 _reflns_number_gt 3241 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics diamond _computing_publication_material PUBLCIF _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. All H atoms were placed geometrically, with C---H = 0.93 (aromatic) , and refined using a riding-atom model, with Uiso(H) = 1.2Ueq(C). Structure refinement after modification of the data for the non-coordinate lattice solvent molecules with the SQUEEZE routine of PLATON led to better refinement and data convergence. In the final refinement of the crystal structures, all of the heavy metal atoms were refined anisotropically. The organic hydrogen atoms were generated geometrically. The hydrogen atoms were placed in idealised positions and refined using a riding model to the atom to which they were attached. In furthur, the two-fold disorder model of Cd3, O5 and O6 atoms in the crystal structure were set up with the total occupancy of 1. The O2, O5, O17, C3, C4, C7, C11, C15, C22, C35, C38, C39, C42 and coordinated aqua molecules were refined isotropically due to the instability of their anisotropic refinements. The atomic displacement parameters for the O5W, O6W and O7W positions were restrained. The plane of two cyclotriphosphazene rings were refined into the same plane separately .The missing hydrogen atoms and solvent molecules that cannot be located in the Fourier difference map and squeezedd out by PLATON routine were added to the formula in the final cycles of refinement. Calculated with EA and TGA data, the solvent molecules should be two aqua and DMF molecules. The whole formula should be C48 H56 Cd3 N5 O29 P3. Associated changes in formula weight, density, mu and F000 may account for the difference in calculated values and reported ones. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6182 _refine_ls_number_parameters 367 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1892 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.018927(15) 0.17364(5) 0.28539(4) 0.0234(2) Uani 1 1 d . . . P2 P 0.2500 0.7500 0.3306(3) 0.0279(11) Uani 1 2 d S . . P1 P 0.23884(8) 0.6411(3) 0.1743(2) 0.0264(8) Uani 1 1 d . . . O10 O -0.0058(2) 0.0144(6) 0.2068(5) 0.031(2) Uani 1 1 d . . . O8 O 0.04405(19) 0.6283(6) 0.3440(5) 0.0275(19) Uani 1 1 d . . . O11 O 0.0391(2) 0.0182(6) 0.3726(5) 0.033(2) Uani 1 1 d . . . O2 O 0.09348(19) 0.2485(6) 0.3303(5) 0.033(2) Uani 1 1 d . . . O13 O 0.0220(2) 0.2413(6) 0.4347(5) 0.039(2) Uani 1 1 d U . . C7 C 0.0857(3) 0.3297(10) 0.2828(8) 0.027(3) Uani 1 1 d . . . O9 O 0.03899(19) 0.8062(6) 0.3130(6) 0.035(2) Uani 1 1 d . . . O3 O 0.0502(2) 0.3466(6) 0.2570(5) 0.034(2) Uani 1 1 d . . . O4 O 0.26028(18) 0.5375(6) 0.1344(5) 0.0277(19) Uani 1 1 d . . . N1 N 0.2427(2) 0.6400(7) 0.2771(6) 0.025(2) Uani 1 1 d . . . O7 O 0.21783(18) 0.7703(7) 0.4020(5) 0.029(2) Uani 1 1 d . . . O1 O 0.19698(18) 0.6137(6) 0.1420(5) 0.0284(19) Uani 1 1 d U . . C21 C 0.0590(3) 0.7266(10) 0.3380(8) 0.029(3) Uani 1 1 d . . . O6 O 0.4336(2) 0.3934(6) 0.1890(6) 0.036(2) Uani 1 1 d . . . C5 C 0.1062(3) 0.5009(9) 0.2023(8) 0.032(3) Uani 1 1 d . . . H5A H 0.0806 0.5194 0.1952 0.039 Uiso 1 1 calc R . . O14 O -0.0103(3) 0.2395(8) 0.1510(5) 0.063(3) Uani 1 1 d . . . C1 C 0.1710(3) 0.5404(9) 0.1800(8) 0.023(3) Uani 1 1 d U . . O5 O 0.4434(2) 0.5550(7) 0.1222(6) 0.051(3) Uani 1 1 d . . . C6 C 0.1330(3) 0.5701(10) 0.1683(8) 0.032(3) Uani 1 1 d . . . H6A H 0.1261 0.6343 0.1386 0.038 Uiso 1 1 calc R . . C16 C 0.1617(3) 0.6590(10) 0.4028(8) 0.035(3) Uani 1 1 d . . . H16A H 0.1760 0.6008 0.4254 0.042 Uiso 1 1 calc R . . C20 C 0.1590(3) 0.8482(8) 0.3537(9) 0.033(3) Uani 1 1 d . . . H20A H 0.1718 0.9149 0.3448 0.040 Uiso 1 1 calc R . . C2 C 0.1811(3) 0.4474(9) 0.2255(7) 0.026(3) Uani 1 1 d U . . H2A H 0.2069 0.4302 0.2336 0.031 Uiso 1 1 calc R . . N2 N 0.2500 0.7500 0.1253(9) 0.036(4) Uani 1 2 d S . . C13 C 0.3151(3) 0.4421(9) 0.1905(8) 0.031(3) Uani 1 1 d . . . H13A H 0.2990 0.3961 0.2225 0.037 Uiso 1 1 calc R . . C15 C 0.1782(3) 0.7577(9) 0.3819(7) 0.023(3) Uani 1 1 d U . . C19 C 0.1193(3) 0.8400(10) 0.3379(9) 0.037(3) Uani 1 1 d . . . H19A H 0.1055 0.8997 0.3159 0.044 Uiso 1 1 calc R . . C3 C 0.1533(3) 0.3796(9) 0.2590(8) 0.029(3) Uani 1 1 d . . . H3A H 0.1603 0.3166 0.2901 0.034 Uiso 1 1 calc R . . C4 C 0.1148(3) 0.4042(9) 0.2469(7) 0.024(3) Uani 1 1 d . . . C8 C 0.3006(3) 0.5255(10) 0.1395(9) 0.036(3) Uani 1 1 d . . . C17 C 0.1219(3) 0.6488(9) 0.3888(9) 0.038(4) Uani 1 1 d . . . H17A H 0.1095 0.5823 0.4011 0.046 Uiso 1 1 calc R . . C18 C 0.1012(3) 0.7384(10) 0.3565(8) 0.029(3) Uani 1 1 d U . . C9 C 0.3241(3) 0.5915(11) 0.0911(8) 0.040(4) Uani 1 1 d . . . H9A H 0.3137 0.6450 0.0545 0.048 Uiso 1 1 calc R . . C10 C 0.3635(3) 0.5785(11) 0.0967(9) 0.043(4) Uani 1 1 d . . . H10A H 0.3797 0.6257 0.0662 0.051 Uiso 1 1 calc R . . C12 C 0.3548(3) 0.4289(9) 0.1925(8) 0.029(3) Uani 1 1 d . . . H12A H 0.3653 0.3721 0.2259 0.035 Uiso 1 1 calc R . . C11 C 0.3784(3) 0.4959(10) 0.1475(8) 0.029(3) Uani 1 1 d . . . C14 C 0.4219(3) 0.4785(11) 0.1526(8) 0.035(3) Uani 1 1 d . . . O1W O 0.0565(2) 0.0402(6) 0.5425(5) 0.040(2) Uani 1 1 d . . . N3 N 0.1216(4) 0.2500 0.5000 0.055(5) Uani 1 2 d S . . H3B H 0.0969 0.2500 0.5000 0.066 Uiso 1 2 calc SR . . C22 C 0.1447(4) 0.1513(11) 0.4873(11) 0.069(5) Uani 1 1 d . . . H22A H 0.1283 0.0885 0.4785 0.104 Uiso 1 1 calc R . . H22B H 0.1604 0.1392 0.5376 0.104 Uiso 1 1 calc R . . H22C H 0.1608 0.1611 0.4372 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0156(3) 0.0213(3) 0.0334(4) 0.0016(3) -0.0006(3) -0.0011(3) P2 0.010(2) 0.038(3) 0.036(3) 0.000 0.000 -0.0007(19) P1 0.0117(15) 0.0298(17) 0.0376(19) 0.0040(16) 0.0007(15) -0.0030(13) O10 0.025(4) 0.031(5) 0.038(5) -0.006(4) 0.000(4) -0.006(4) O8 0.018(4) 0.025(4) 0.040(5) -0.006(4) -0.009(4) -0.002(3) O11 0.044(5) 0.021(4) 0.034(5) 0.007(4) -0.008(4) 0.010(4) O2 0.019(4) 0.026(4) 0.052(6) 0.018(5) -0.001(4) -0.001(4) O13 0.035(3) 0.025(3) 0.057(4) -0.002(3) -0.031(3) -0.005(3) C7 0.017(6) 0.039(7) 0.025(7) -0.001(7) 0.003(6) -0.003(6) O9 0.014(4) 0.029(5) 0.061(6) 0.009(5) 0.001(4) 0.003(4) O3 0.024(5) 0.024(4) 0.053(6) 0.004(4) 0.009(4) -0.003(4) O4 0.010(4) 0.034(5) 0.038(5) -0.005(4) 0.002(4) 0.002(3) N1 0.026(5) 0.025(5) 0.024(5) -0.003(5) -0.003(5) 0.004(4) O7 0.013(4) 0.053(5) 0.022(4) 0.001(4) 0.003(4) 0.000(4) O1 0.009(3) 0.034(4) 0.043(5) 0.009(4) 0.002(3) -0.010(3) C21 0.005(5) 0.041(8) 0.041(8) -0.008(7) 0.002(6) -0.005(5) O6 0.024(4) 0.025(5) 0.060(6) 0.018(5) -0.009(4) 0.009(4) C5 0.023(6) 0.031(7) 0.044(9) -0.014(7) -0.009(6) 0.005(5) O14 0.101(8) 0.065(7) 0.023(5) 0.004(5) -0.016(5) 0.024(6) C1 0.009(5) 0.026(6) 0.035(6) -0.001(5) 0.007(5) -0.001(4) O5 0.030(5) 0.056(6) 0.068(7) 0.022(6) 0.012(5) -0.003(5) C6 0.017(6) 0.025(6) 0.053(9) 0.008(7) -0.002(6) -0.015(5) C16 0.019(6) 0.031(7) 0.056(9) 0.009(7) 0.006(6) 0.008(5) C20 0.013(6) 0.013(6) 0.074(10) -0.002(7) 0.011(6) -0.002(5) C2 0.012(5) 0.031(6) 0.034(6) -0.008(5) -0.009(5) -0.001(4) N2 0.020(7) 0.058(11) 0.032(9) 0.000 0.000 -0.009(7) C13 0.029(7) 0.025(7) 0.038(8) 0.003(6) -0.004(6) -0.010(6) C15 0.012(5) 0.032(6) 0.024(6) 0.010(5) 0.006(5) -0.002(5) C19 0.023(6) 0.027(7) 0.061(10) 0.012(7) 0.013(7) 0.005(5) C3 0.032(7) 0.016(6) 0.039(8) -0.003(6) -0.005(6) 0.005(5) C4 0.019(6) 0.024(6) 0.030(7) 0.006(6) 0.000(5) -0.007(5) C8 0.018(6) 0.034(7) 0.055(9) -0.016(7) 0.010(6) -0.012(6) C17 0.031(7) 0.013(6) 0.071(10) 0.010(7) 0.006(7) 0.002(5) C18 0.017(5) 0.031(6) 0.039(6) 0.003(6) 0.015(5) -0.005(5) C9 0.025(7) 0.054(9) 0.042(9) 0.022(7) 0.009(6) 0.018(6) C10 0.023(7) 0.036(8) 0.069(11) 0.001(8) 0.009(7) -0.003(6) C12 0.023(6) 0.025(6) 0.039(9) 0.006(6) 0.008(6) -0.005(5) C11 0.024(6) 0.034(7) 0.031(7) 0.015(6) -0.007(6) 0.007(6) C14 0.028(7) 0.045(8) 0.032(8) -0.014(7) 0.010(6) -0.011(7) O1W 0.038(5) 0.036(5) 0.046(6) 0.012(5) 0.005(4) 0.013(4) N3 0.045(10) 0.035(10) 0.085(14) -0.014(10) 0.000 0.000 C22 0.078(11) 0.051(10) 0.078(13) 0.007(10) 0.006(10) 0.014(9) _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 Eu1 O6 2.367(7) 2 ? Eu1 O3 2.393(7) . ? Eu1 O11 2.411(7) . ? Eu1 O10 2.428(7) . ? Eu1 O8 2.437(7) 8 ? Eu1 O14 2.439(8) . ? Eu1 O13 2.441(8) . ? Eu1 O9 2.611(7) 8 ? Eu1 O2 2.838(7) . ? Eu1 C21 2.908(10) 8 ? Eu1 C7 2.994(11) . ? P2 N1 1.581(9) 2_565 ? P2 N1 1.581(9) . ? P2 O7 1.590(7) 2_565 ? P2 O7 1.590(7) . ? P1 N2 1.564(7) . ? P1 O1 1.577(7) . ? P1 O4 1.580(7) . ? P1 N1 1.588(9) . ? O8 C21 1.300(13) . ? O8 Eu1 2.437(7) 8_565 ? O2 C7 1.251(13) . ? C7 O3 1.317(12) . ? C7 C4 1.466(15) . ? O9 C21 1.248(13) . ? O9 Eu1 2.611(7) 8_565 ? O4 C8 1.418(12) . ? O7 C15 1.424(12) . ? O1 C1 1.394(12) . ? C21 C18 1.507(14) . ? C21 Eu1 2.908(10) 8_565 ? O6 C14 1.238(14) . ? O6 Eu1 2.367(7) 2 ? C5 C6 1.357(15) . ? C5 C4 1.386(15) . ? C5 H5A 0.9300 . ? C1 C2 1.368(15) . ? C1 C6 1.388(14) . ? O5 C14 1.278(13) . ? C6 H6A 0.9300 . ? C16 C15 1.362(15) . ? C16 C17 1.409(15) . ? C16 H16A 0.9300 . ? C20 C15 1.353(14) . ? C20 C19 1.408(14) . ? C20 H20A 0.9300 . ? C2 C3 1.370(15) . ? C2 H2A 0.9300 . ? N2 P1 1.564(7) 2_565 ? C13 C8 1.371(16) . ? C13 C12 1.397(15) . ? C13 H13A 0.9300 . ? C19 C18 1.407(14) . ? C19 H19A 0.9300 . ? C3 C4 1.388(14) . ? C3 H3A 0.9300 . ? C8 C9 1.363(16) . ? C17 C18 1.391(15) . ? C17 H17A 0.9300 . ? C9 C10 1.386(15) . ? C9 H9A 0.9300 . ? C10 C11 1.368(15) . ? C10 H10A 0.9300 . ? C12 C11 1.345(14) . ? C12 H12A 0.9300 . ? C11 C14 1.533(15) . ? N3 C22 1.452(14) 4_556 ? N3 C22 1.452(14) . ? N3 H3B 0.8600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 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 O6 Eu1 O3 82.2(3) 2 . ? O6 Eu1 O11 83.0(3) 2 . ? O3 Eu1 O11 130.3(3) . . ? O6 Eu1 O10 70.5(2) 2 . ? O3 Eu1 O10 139.5(3) . . ? O11 Eu1 O10 76.5(3) . . ? O6 Eu1 O8 141.9(3) 2 8 ? O3 Eu1 O8 132.3(2) . 8 ? O11 Eu1 O8 83.2(3) . 8 ? O10 Eu1 O8 71.7(2) . 8 ? O6 Eu1 O14 82.7(3) 2 . ? O3 Eu1 O14 75.6(3) . . ? O11 Eu1 O14 147.9(3) . . ? O10 Eu1 O14 71.7(3) . . ? O8 Eu1 O14 90.6(3) 8 . ? O6 Eu1 O13 132.3(3) 2 . ? O3 Eu1 O13 82.0(3) . . ? O11 Eu1 O13 73.9(3) . . ? O10 Eu1 O13 138.5(3) . . ? O8 Eu1 O13 76.5(3) 8 . ? O14 Eu1 O13 135.1(3) . . ? O6 Eu1 O9 148.6(3) 2 8 ? O3 Eu1 O9 81.3(2) . 8 ? O11 Eu1 O9 127.7(3) . 8 ? O10 Eu1 O9 106.9(2) . 8 ? O8 Eu1 O9 51.7(2) 8 8 ? O14 Eu1 O9 67.4(3) . 8 ? O13 Eu1 O9 71.1(3) . 8 ? O6 Eu1 O2 67.6(2) 2 . ? O3 Eu1 O2 49.5(2) . . ? O11 Eu1 O2 81.1(2) . . ? O10 Eu1 O2 134.3(2) . . ? O8 Eu1 O2 143.8(2) 8 . ? O14 Eu1 O2 119.0(3) . . ? O13 Eu1 O2 67.9(2) . . ? O9 Eu1 O2 118.3(2) 8 . ? O6 Eu1 C21 154.7(3) 2 8 ? O3 Eu1 C21 106.6(3) . 8 ? O11 Eu1 C21 106.8(3) . 8 ? O10 Eu1 C21 88.9(3) . 8 ? O8 Eu1 C21 26.3(3) 8 8 ? O14 Eu1 C21 76.9(3) . 8 ? O13 Eu1 C21 72.9(3) . 8 ? O9 Eu1 C21 25.4(3) 8 8 ? O2 Eu1 C21 136.0(3) . 8 ? O6 Eu1 C7 70.2(3) 2 . ? O3 Eu1 C7 25.3(3) . . ? O11 Eu1 C7 105.6(3) . . ? O10 Eu1 C7 140.1(3) . . ? O8 Eu1 C7 147.9(3) 8 . ? O14 Eu1 C7 96.3(3) . . ? O13 Eu1 C7 76.6(3) . . ? O9 Eu1 C7 102.6(3) 8 . ? O2 Eu1 C7 24.6(2) . . ? C21 Eu1 C7 126.3(3) 8 . ? N1 P2 N1 117.3(7) 2_565 . ? N1 P2 O7 112.0(4) 2_565 2_565 ? N1 P2 O7 110.1(4) . 2_565 ? N1 P2 O7 110.1(4) 2_565 . ? N1 P2 O7 112.0(4) . . ? O7 P2 O7 92.5(6) 2_565 . ? N2 P1 O1 104.7(4) . . ? N2 P1 O4 111.0(4) . . ? O1 P1 O4 98.6(4) . . ? N2 P1 N1 117.8(6) . . ? O1 P1 N1 113.1(5) . . ? O4 P1 N1 109.9(5) . . ? C21 O8 Eu1 97.5(6) . 8_565 ? C7 O2 Eu1 84.7(6) . . ? O2 C7 O3 120.1(10) . . ? O2 C7 C4 123.3(10) . . ? O3 C7 C4 116.3(10) . . ? O2 C7 Eu1 70.7(6) . . ? O3 C7 Eu1 50.9(5) . . ? C4 C7 Eu1 158.4(8) . . ? C21 O9 Eu1 90.7(6) . 8_565 ? C7 O3 Eu1 103.8(7) . . ? C8 O4 P1 121.9(7) . . ? P2 N1 P1 121.7(6) . . ? C15 O7 P2 121.2(7) . . ? C1 O1 P1 126.9(7) . . ? O9 C21 O8 119.9(9) . . ? O9 C21 C18 122.2(11) . . ? O8 C21 C18 117.7(10) . . ? O9 C21 Eu1 63.9(5) . 8_565 ? O8 C21 Eu1 56.2(5) . 8_565 ? C18 C21 Eu1 170.8(8) . 8_565 ? C14 O6 Eu1 142.9(8) . 2 ? C6 C5 C4 124.1(11) . . ? C6 C5 H5A 117.9 . . ? C4 C5 H5A 117.9 . . ? C2 C1 C6 121.7(10) . . ? C2 C1 O1 124.6(9) . . ? C6 C1 O1 113.7(10) . . ? C5 C6 C1 116.6(11) . . ? C5 C6 H6A 121.7 . . ? C1 C6 H6A 121.7 . . ? C15 C16 C17 117.3(11) . . ? C15 C16 H16A 121.4 . . ? C17 C16 H16A 121.4 . . ? C15 C20 C19 119.1(10) . . ? C15 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? C1 C2 C3 120.0(10) . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? P1 N2 P1 122.3(9) 2_565 . ? C8 C13 C12 117.4(11) . . ? C8 C13 H13A 121.3 . . ? C12 C13 H13A 121.3 . . ? C20 C15 C16 124.8(10) . . ? C20 C15 O7 117.8(10) . . ? C16 C15 O7 116.9(10) . . ? C18 C19 C20 117.8(11) . . ? C18 C19 H19A 121.1 . . ? C20 C19 H19A 121.1 . . ? C2 C3 C4 120.5(11) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 117.1(10) . . ? C5 C4 C7 123.6(10) . . ? C3 C4 C7 119.3(10) . . ? C9 C8 C13 121.4(11) . . ? C9 C8 O4 120.5(12) . . ? C13 C8 O4 118.1(11) . . ? C18 C17 C16 119.7(10) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 121.1(10) . . ? C17 C18 C21 120.0(10) . . ? C19 C18 C21 118.8(11) . . ? C8 C9 C10 119.7(12) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 119.6(12) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C11 C12 C13 121.8(11) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C12 C11 C10 120.0(11) . . ? C12 C11 C14 119.7(10) . . ? C10 C11 C14 120.3(11) . . ? O6 C14 O5 124.8(11) . . ? O6 C14 C11 117.5(11) . . ? O5 C14 C11 117.6(12) . . ? C22 N3 C22 112.4(16) 4_556 . ? C22 N3 H3B 123.8 4_556 . ? C22 N3 H3B 123.8 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 O6 Eu1 O2 C7 91.2(7) 2 . . . ? O3 Eu1 O2 C7 -8.0(6) . . . . ? O11 Eu1 O2 C7 177.3(7) . . . . ? O10 Eu1 O2 C7 116.3(7) . . . . ? O8 Eu1 O2 C7 -117.4(7) 8 . . . ? O14 Eu1 O2 C7 23.9(7) . . . . ? O13 Eu1 O2 C7 -106.5(7) . . . . ? O9 Eu1 O2 C7 -54.5(7) 8 . . . ? C21 Eu1 O2 C7 -77.8(8) 8 . . . ? Eu1 O2 C7 O3 12.8(10) . . . . ? Eu1 O2 C7 C4 -161.6(11) . . . . ? O6 Eu1 C7 O2 -79.2(7) 2 . . . ? O3 Eu1 C7 O2 165.7(11) . . . . ? O11 Eu1 C7 O2 -2.8(7) . . . . ? O10 Eu1 C7 O2 -90.2(7) . . . . ? O8 Eu1 C7 O2 99.7(8) 8 . . . ? O14 Eu1 C7 O2 -159.1(6) . . . . ? O13 Eu1 C7 O2 66.0(6) . . . . ? O9 Eu1 C7 O2 132.7(6) 8 . . . ? C21 Eu1 C7 O2 122.5(7) 8 . . . ? O6 Eu1 C7 O3 115.1(7) 2 . . . ? O11 Eu1 C7 O3 -168.5(7) . . . . ? O10 Eu1 C7 O3 104.1(7) . . . . ? O8 Eu1 C7 O3 -66.0(9) 8 . . . ? O14 Eu1 C7 O3 35.2(7) . . . . ? O13 Eu1 C7 O3 -99.7(7) . . . . ? O9 Eu1 C7 O3 -33.0(7) 8 . . . ? O2 Eu1 C7 O3 -165.7(11) . . . . ? C21 Eu1 C7 O3 -43.2(8) 8 . . . ? O6 Eu1 C7 C4 55(2) 2 . . . ? O3 Eu1 C7 C4 -60(2) . . . . ? O11 Eu1 C7 C4 131(2) . . . . ? O10 Eu1 C7 C4 44(2) . . . . ? O8 Eu1 C7 C4 -126(2) 8 . . . ? O14 Eu1 C7 C4 -25(2) . . . . ? O13 Eu1 C7 C4 -160(2) . . . . ? O9 Eu1 C7 C4 -93(2) 8 . . . ? O2 Eu1 C7 C4 134(3) . . . . ? C21 Eu1 C7 C4 -103(2) 8 . . . ? O2 C7 O3 Eu1 -15.6(13) . . . . ? C4 C7 O3 Eu1 159.2(8) . . . . ? O6 Eu1 O3 C7 -59.3(7) 2 . . . ? O11 Eu1 O3 C7 14.6(8) . . . . ? O10 Eu1 O3 C7 -106.7(7) . . . . ? O8 Eu1 O3 C7 138.9(6) 8 . . . ? O14 Eu1 O3 C7 -143.7(7) . . . . ? O13 Eu1 O3 C7 75.5(7) . . . . ? O9 Eu1 O3 C7 147.5(7) 8 . . . ? O2 Eu1 O3 C7 7.8(6) . . . . ? C21 Eu1 O3 C7 144.9(7) 8 . . . ? N2 P1 O4 C8 65.8(10) . . . . ? O1 P1 O4 C8 175.3(9) . . . . ? N1 P1 O4 C8 -66.3(10) . . . . ? N1 P2 N1 P1 -5.7(4) 2_565 . . . ? O7 P2 N1 P1 -135.5(6) 2_565 . . . ? O7 P2 N1 P1 123.1(6) . . . . ? N2 P1 N1 P2 11.3(8) . . . . ? O1 P1 N1 P2 -111.1(6) . . . . ? O4 P1 N1 P2 139.7(5) . . . . ? N1 P2 O7 C15 86.7(9) 2_565 . . . ? N1 P2 O7 C15 -45.8(9) . . . . ? O7 P2 O7 C15 -158.7(10) 2_565 . . . ? N2 P1 O1 C1 -164.3(9) . . . . ? O4 P1 O1 C1 81.2(9) . . . . ? N1 P1 O1 C1 -34.9(10) . . . . ? Eu1 O9 C21 O8 -3.9(11) 8_565 . . . ? Eu1 O9 C21 C18 172.2(10) 8_565 . . . ? Eu1 O8 C21 O9 4.2(12) 8_565 . . . ? Eu1 O8 C21 C18 -172.0(9) 8_565 . . . ? P1 O1 C1 C2 -30.1(16) . . . . ? P1 O1 C1 C6 149.6(9) . . . . ? C4 C5 C6 C1 -0.1(19) . . . . ? C2 C1 C6 C5 -1.6(18) . . . . ? O1 C1 C6 C5 178.7(10) . . . . ? C6 C1 C2 C3 1.5(18) . . . . ? O1 C1 C2 C3 -178.8(10) . . . . ? O1 P1 N2 P1 121.1(4) . . . 2_565 ? O4 P1 N2 P1 -133.4(4) . . . 2_565 ? N1 P1 N2 P1 -5.4(4) . . . 2_565 ? C19 C20 C15 C16 -5(2) . . . . ? C19 C20 C15 O7 -176.5(11) . . . . ? C17 C16 C15 C20 4(2) . . . . ? C17 C16 C15 O7 175.6(10) . . . . ? P2 O7 C15 C20 -90.8(12) . . . . ? P2 O7 C15 C16 97.0(11) . . . . ? C15 C20 C19 C18 3.0(19) . . . . ? C1 C2 C3 C4 0.3(18) . . . . ? C6 C5 C4 C3 1.8(19) . . . . ? C6 C5 C4 C7 -179.6(12) . . . . ? C2 C3 C4 C5 -1.9(18) . . . . ? C2 C3 C4 C7 179.4(11) . . . . ? O2 C7 C4 C5 -172.8(11) . . . . ? O3 C7 C4 C5 12.5(18) . . . . ? Eu1 C7 C4 C5 61(3) . . . . ? O2 C7 C4 C3 5.8(18) . . . . ? O3 C7 C4 C3 -168.8(11) . . . . ? Eu1 C7 C4 C3 -120(2) . . . . ? C12 C13 C8 C9 1.4(19) . . . . ? C12 C13 C8 O4 177.8(10) . . . . ? P1 O4 C8 C9 -71.4(15) . . . . ? P1 O4 C8 C13 112.1(11) . . . . ? C15 C16 C17 C18 -1.2(19) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C16 C17 C18 C21 177.5(11) . . . . ? C20 C19 C18 C17 -0.5(19) . . . . ? C20 C19 C18 C21 -178.4(11) . . . . ? O9 C21 C18 C17 176.4(12) . . . . ? O8 C21 C18 C17 -7.4(17) . . . . ? Eu1 C21 C18 C17 -54(6) 8_565 . . . ? O9 C21 C18 C19 -5.6(18) . . . . ? O8 C21 C18 C19 170.5(11) . . . . ? Eu1 C21 C18 C19 124(5) 8_565 . . . ? C13 C8 C9 C10 -4(2) . . . . ? O4 C8 C9 C10 -179.9(11) . . . . ? C8 C9 C10 C11 3(2) . . . . ? C8 C13 C12 C11 1.0(18) . . . . ? C13 C12 C11 C10 -1.3(19) . . . . ? C13 C12 C11 C14 179.4(11) . . . . ? C9 C10 C11 C12 -1(2) . . . . ? C9 C10 C11 C14 178.4(12) . . . . ? Eu1 O6 C14 O5 38(2) 2 . . . ? Eu1 O6 C14 C11 -138.9(10) 2 . . . ? C12 C11 C14 O6 9.5(18) . . . . ? C10 C11 C14 O6 -169.8(12) . . . . ? C12 C11 C14 O5 -167.6(12) . . . . ? C10 C11 C14 O5 13.1(18) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 3.503 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.188 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.001 -0.001 -0.028 1800.7 128.2 2 0.569 0.250 1.000 29.0 1.1 3 0.931 0.250 0.000 27.8 0.6 4 0.069 0.750 0.000 29.0 1.3 5 0.431 0.750 1.000 27.8 0.7 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 926682' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H38 Eu2 N5 O24 P3' _chemical_formula_weight 1453.65 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2371(3) _cell_length_b 9.8604(3) _cell_length_c 30.4599(10) _cell_angle_alpha 96.869(3) _cell_angle_beta 92.323(2) _cell_angle_gamma 92.071(2) _cell_volume 2749.81(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6417 _exptl_absorpt_correction_T_max 0.7928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Brucker SMART APEX' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25951 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10521 _reflns_number_gt 8846 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material PUBLCIF _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. All H atoms were placed geometrically, with C---H = 0.93 (aromatic) , and refined using a riding-atom model, with Uiso(H) = 1.2Ueq(C). Structure refinement after modification of the data for the non-coordinate lattice solvent molecules with the SQUEEZE routine of PLATON led to better refinement and data convergence. In the final refinement of the crystal structures, all of the heavy metal atoms were refined anisotropically. The organic hydrogen atoms were generated geometrically. The hydrogen atoms were placed in idealised positions and refined using a riding model to the atom to which they were attached. In furthur, the two-fold disorder model of Cd3, O5 and O6 atoms in the crystal structure were set up with the total occupancy of 1. The O2, O5, O17, C3, C4, C7, C11, C15, C22, C35, C38, C39, C42 and coordinated aqua molecules were refined isotropically due to the instability of their anisotropic refinements. The atomic displacement parameters for the O5W, O6W and O7W positions were restrained. The plane of two cyclotriphosphazene rings were refined into the same plane separately .The missing hydrogen atoms and solvent molecules that cannot be located in the Fourier difference map and squeezedd out by PLATON routine were added to the formula in the final cycles of refinement. Calculated with EA and TGA data, the solvent molecules should be two aqua and DMF molecules. The whole formula should be C48 H56 Cd3 N5 O29 P3. Associated changes in formula weight, density, mu and F000 may account for the difference in calculated values and reported ones. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+21.1965P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10521 _refine_ls_number_parameters 724 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.18795(3) 0.50347(3) 0.470884(10) 0.01451(10) Uani 1 1 d . . . Eu2 Eu 0.02599(6) 0.16442(5) -0.034497(13) 0.05001(16) Uani 1 1 d . . . P3 P 0.25395(19) 0.07681(19) 0.24155(6) 0.0220(4) Uani 1 1 d . . . P1 P 0.04911(19) -0.03370(18) 0.29240(6) 0.0202(4) Uani 1 1 d . . . P2 P 0.00729(19) 0.21460(19) 0.26244(6) 0.0210(4) Uani 1 1 d . . . O3 O 0.0837(5) 0.2838(5) 0.47403(15) 0.0220(10) Uani 1 1 d . . . O9 O -0.2963(5) 0.5296(5) 0.45593(15) 0.0208(10) Uani 1 1 d . . . O1 O 0.0956(5) -0.0624(5) 0.34062(15) 0.0224(10) Uani 1 1 d . . . O8 O -0.0616(5) 0.5069(5) 0.45191(14) 0.0176(10) Uani 1 1 d . . . O7 O 0.0051(5) 0.3617(5) 0.28944(15) 0.0224(10) Uani 1 1 d . . . O1W O 0.4288(5) 0.6257(5) 0.47496(16) 0.0238(11) Uani 1 1 d . . . O2 O -0.1511(5) 0.2744(5) 0.49013(16) 0.0241(11) Uani 1 1 d . . . O15 O 0.2348(5) 0.3792(5) 0.39833(15) 0.0268(11) Uani 1 1 d . . . O14 O 0.3884(5) 0.3384(5) 0.45170(16) 0.0266(11) Uani 1 1 d . . . O4 O -0.0566(6) -0.1646(5) 0.27846(16) 0.0292(12) Uani 1 1 d . . . O13 O 0.4163(5) 0.1199(5) 0.25845(16) 0.0294(12) Uani 1 1 d . . . C21 C -0.1862(7) 0.5120(6) 0.4332(2) 0.0163(13) Uani 1 1 d . . . O19 O 0.1768(6) 0.6578(5) 0.41604(17) 0.0303(12) Uani 1 1 d . . . O16 O 0.2827(5) 0.0114(5) 0.19305(15) 0.0284(12) Uani 1 1 d . . . O10 O -0.1181(5) 0.2129(5) 0.22497(14) 0.0254(11) Uani 1 1 d . . . C17 C -0.2030(7) 0.4899(6) 0.3843(2) 0.0158(13) Uani 1 1 d . . . C30 C 0.6033(7) 0.1189(7) 0.3132(2) 0.0260(16) Uani 1 1 d . . . H30A H 0.6607 0.0790 0.2912 0.031 Uiso 1 1 calc R . . C14 C -0.1459(11) -0.2010(9) 0.1180(3) 0.043(2) Uani 1 1 d . . . C35 C 0.3480(7) 0.3246(7) 0.4118(2) 0.0210(14) Uani 1 1 d . . . C3 C -0.0604(7) 0.0942(7) 0.4417(2) 0.0197(14) Uani 1 1 d . . . C7 C -0.0409(7) 0.2271(7) 0.4713(2) 0.0209(14) Uani 1 1 d . . . N3 N 0.1607(7) 0.2091(6) 0.24194(19) 0.0257(13) Uani 1 1 d . . . C33 C 0.4351(7) 0.2452(7) 0.3777(2) 0.0204(14) Uani 1 1 d . . . C1 C 0.0032(7) -0.0442(7) 0.3769(2) 0.0177(14) Uani 1 1 d . . . C16 C -0.0902(7) 0.4387(6) 0.3594(2) 0.0162(13) Uani 1 1 d . . . H16A H -0.0015 0.4229 0.3729 0.019 Uiso 1 1 calc R . . C2 C 0.0223(7) 0.0750(7) 0.4050(2) 0.0195(14) Uani 1 1 d . . . H2A H 0.0902 0.1420 0.3994 0.023 Uiso 1 1 calc R . . C6 C -0.0925(8) -0.1476(7) 0.3844(2) 0.0244(15) Uani 1 1 d . . . H6A H -0.1012 -0.2287 0.3653 0.029 Uiso 1 1 calc R . . C32 C 0.5726(8) 0.2068(7) 0.3885(2) 0.0256(16) Uani 1 1 d . . . H32A H 0.6087 0.2224 0.4177 0.031 Uiso 1 1 calc R . . C34 C 0.3787(7) 0.2180(7) 0.3348(2) 0.0240(15) Uani 1 1 d . . . H34A H 0.2856 0.2432 0.3274 0.029 Uiso 1 1 calc R . . O18 O 0.1192(9) 0.0392(8) 0.0341(2) 0.0655(15) Uani 1 1 d . . . C29 C 0.4632(7) 0.1523(7) 0.3030(2) 0.0238(15) Uani 1 1 d . . . N2 N 0.1923(6) -0.0437(6) 0.26544(19) 0.0240(13) Uani 1 1 d . . . O6 O -0.0138(7) -0.1722(7) 0.11389(18) 0.0477(16) Uani 1 1 d . . . O12 O -0.1561(9) 0.0319(7) 0.06461(19) 0.0573(19) Uani 1 1 d . . . C9 C -0.1034(9) -0.1739(8) 0.1994(2) 0.0309(17) Uani 1 1 d . . . H9A H -0.0052 -0.1592 0.1951 0.037 Uiso 1 1 calc R . . C5 C -0.1754(8) -0.1278(7) 0.4211(2) 0.0283(16) Uani 1 1 d . . . H5A H -0.2418 -0.1961 0.4267 0.034 Uiso 1 1 calc R . . O5 O -0.2308(8) -0.2332(7) 0.08430(19) 0.0583(19) Uani 1 1 d . . . C4 C -0.1609(7) -0.0076(7) 0.4496(2) 0.0246(15) Uani 1 1 d . . . H4A H -0.2182 0.0052 0.4741 0.030 Uiso 1 1 calc R . . C15 C -0.1120(7) 0.4118(7) 0.3141(2) 0.0192(14) Uani 1 1 d . . . O3W O -0.2209(9) 0.2182(8) -0.0588(2) 0.071(2) Uani 1 1 d . . . N1 N -0.0383(6) 0.1013(6) 0.29201(18) 0.0204(12) Uani 1 1 d . . . C20 C -0.2419(8) 0.4381(8) 0.2927(2) 0.0298(17) Uani 1 1 d . . . H20A H -0.2545 0.4194 0.2621 0.036 Uiso 1 1 calc R . . C22 C -0.0981(8) 0.2733(8) 0.1859(2) 0.0288(17) Uani 1 1 d . . . C31 C 0.6570(8) 0.1451(8) 0.3560(2) 0.0276(16) Uani 1 1 d . . . H31A H 0.7507 0.1212 0.3633 0.033 Uiso 1 1 calc R . . C8 C -0.1522(8) -0.1756(8) 0.2415(2) 0.0273(16) Uani 1 1 d . . . C42 C 0.2158(12) 0.1314(11) 0.0433(3) 0.051(3) Uani 1 1 d . . . O11 O -0.1118(9) 0.2138(7) 0.02966(19) 0.066(2) Uani 1 1 d . . . C10 C -0.2025(9) -0.1944(9) 0.1633(3) 0.0360(19) Uani 1 1 d . . . C23 C -0.1165(9) 0.1900(8) 0.1465(2) 0.0325(18) Uani 1 1 d . . . H23A H -0.1367 0.0968 0.1463 0.039 Uiso 1 1 calc R . . C36 C 0.3369(8) 0.0814(9) 0.1595(2) 0.0342(19) Uani 1 1 d . . . C28 C -0.1282(12) 0.1554(11) 0.0636(3) 0.050(2) Uani 1 1 d . . . C24 C -0.1047(10) 0.2458(9) 0.1069(2) 0.037(2) Uani 1 1 d . . . C13 C -0.2984(10) -0.1918(11) 0.2490(3) 0.050(3) Uani 1 1 d . . . H13A H -0.3301 -0.1925 0.2776 0.060 Uiso 1 1 calc R . . O2W O 0.0335(13) 0.4074(9) -0.0213(3) 0.102(4) Uani 1 1 d . . . C27 C -0.0673(11) 0.4101(10) 0.1872(3) 0.047(2) Uani 1 1 d . . . H27A H -0.0569 0.4653 0.2142 0.057 Uiso 1 1 calc R . . C12 C -0.3972(10) -0.2072(14) 0.2125(3) 0.068(3) Uani 1 1 d . . . H12A H -0.4961 -0.2170 0.2167 0.082 Uiso 1 1 calc R . . C11 C -0.3482(11) -0.2078(11) 0.1705(3) 0.054(3) Uani 1 1 d . . . H11A H -0.4148 -0.2175 0.1464 0.065 Uiso 1 1 calc R . . C18 C -0.3339(7) 0.5182(7) 0.3632(2) 0.0231(15) Uani 1 1 d . . . H18A H -0.4088 0.5545 0.3797 0.028 Uiso 1 1 calc R . . C19 C -0.3516(8) 0.4923(8) 0.3177(2) 0.0328(18) Uani 1 1 d . . . H19A H -0.4385 0.5116 0.3037 0.039 Uiso 1 1 calc R . . O17 O 0.2394(9) 0.2185(8) 0.0174(2) 0.0655(15) Uani 1 1 d . . . C37 C 0.2514(9) 0.0747(9) 0.1205(2) 0.0349(19) Uani 1 1 d . . . H37A H 0.1617 0.0278 0.1177 0.042 Uiso 1 1 calc R . . C38 C 0.3026(10) 0.1390(10) 0.0858(3) 0.044(2) Uani 1 1 d . . . C25 C -0.0733(12) 0.3820(10) 0.1073(3) 0.053(3) Uani 1 1 d . . . H25A H -0.0664 0.4193 0.0808 0.064 Uiso 1 1 calc R . . C26 C -0.0513(13) 0.4665(10) 0.1479(3) 0.060(3) Uani 1 1 d . . . H26A H -0.0264 0.5590 0.1484 0.072 Uiso 1 1 calc R . . C45 C 0.2585(12) 0.6952(13) 0.3891(4) 0.067(3) Uani 1 1 d . . . H45A H 0.2583 0.6354 0.3631 0.081 Uiso 1 1 calc R . . C43 C 0.4318(12) 0.8358(13) 0.3548(4) 0.074(4) Uani 1 1 d . . . H43A H 0.4197 0.7671 0.3297 0.111 Uiso 1 1 calc R . . H43B H 0.5317 0.8432 0.3651 0.111 Uiso 1 1 calc R . . H43C H 0.4032 0.9221 0.3465 0.111 Uiso 1 1 calc R . . C39 C 0.4367(13) 0.2031(15) 0.0899(3) 0.078(4) Uani 1 1 d . . . H39A H 0.4709 0.2450 0.0664 0.093 Uiso 1 1 calc R . . C44 C 0.3530(14) 0.8972(12) 0.4299(5) 0.080(4) Uani 1 1 d . . . H44A H 0.2905 0.8655 0.4513 0.120 Uiso 1 1 calc R . . H44B H 0.3233 0.9847 0.4230 0.120 Uiso 1 1 calc R . . H44C H 0.4511 0.9053 0.4418 0.120 Uiso 1 1 calc R . . N4 N 0.3438(9) 0.7988(10) 0.3893(3) 0.059(2) Uani 1 1 d . . . C41 C 0.4715(10) 0.1429(14) 0.1635(3) 0.069(4) Uani 1 1 d . . . H41A H 0.5293 0.1429 0.1892 0.083 Uiso 1 1 calc R . . C40 C 0.5213(12) 0.2070(17) 0.1274(4) 0.092(5) Uani 1 1 d . . . H40A H 0.6121 0.2518 0.1295 0.111 Uiso 1 1 calc R . . O5W O -0.2936(11) 0.3436(10) -0.1362(6) 0.165(7) Uani 1 1 d . . . N5 N -0.7125(12) -0.4211(12) 0.1946(4) 0.087(3) Uani 1 1 d U . . H5B H -0.7281 -0.3625 0.1763 0.105 Uiso 1 1 calc R . . O4W O -0.5023(12) 0.1113(15) -0.0355(4) 0.134(4) Uani 1 1 d . . . C46 C -0.7529(18) -0.399(2) 0.2405(5) 0.122(7) Uani 1 1 d . . . H46A H -0.7960 -0.3120 0.2461 0.183 Uiso 1 1 calc R . . H46B H -0.6680 -0.4007 0.2597 0.183 Uiso 1 1 calc R . . H46C H -0.8212 -0.4701 0.2460 0.183 Uiso 1 1 calc R . . C47 C -0.642(2) -0.5522(16) 0.1815(6) 0.130(7) Uani 1 1 d U . . H47A H -0.6217 -0.5591 0.1507 0.195 Uiso 1 1 calc R . . H47B H -0.7065 -0.6271 0.1865 0.195 Uiso 1 1 calc R . . H47C H -0.5538 -0.5552 0.1989 0.195 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.00965(16) 0.02076(18) 0.01240(17) -0.00106(12) -0.00006(11) 0.00157(12) Eu2 0.0933(4) 0.0433(3) 0.0136(2) 0.00358(18) 0.0006(2) 0.0060(3) P3 0.0204(9) 0.0322(10) 0.0139(9) 0.0019(7) 0.0050(7) 0.0054(8) P1 0.0220(9) 0.0256(9) 0.0130(9) 0.0001(7) 0.0029(7) 0.0043(7) P2 0.0212(9) 0.0294(10) 0.0130(9) 0.0032(7) 0.0027(7) 0.0069(7) O3 0.020(2) 0.023(2) 0.023(3) 0.001(2) 0.0019(19) 0.003(2) O9 0.010(2) 0.034(3) 0.019(2) 0.003(2) 0.0003(18) 0.0041(19) O1 0.023(3) 0.027(3) 0.017(2) 0.001(2) 0.0051(19) 0.007(2) O8 0.013(2) 0.025(2) 0.015(2) 0.0001(19) -0.0001(17) -0.0009(18) O7 0.023(2) 0.029(3) 0.016(2) 0.001(2) 0.0044(19) 0.002(2) O1W 0.013(2) 0.030(3) 0.029(3) 0.006(2) 0.0013(19) 0.000(2) O2 0.027(3) 0.023(3) 0.022(3) -0.001(2) 0.007(2) -0.003(2) O15 0.022(3) 0.041(3) 0.017(3) -0.001(2) 0.001(2) 0.015(2) O14 0.019(2) 0.040(3) 0.018(3) -0.004(2) -0.0021(19) 0.005(2) O4 0.034(3) 0.034(3) 0.018(3) 0.004(2) 0.001(2) -0.006(2) O13 0.023(3) 0.043(3) 0.021(3) 0.000(2) 0.005(2) 0.002(2) C21 0.013(3) 0.016(3) 0.020(3) 0.003(3) 0.000(3) 0.002(2) O19 0.028(3) 0.041(3) 0.025(3) 0.017(2) 0.001(2) 0.000(2) O16 0.029(3) 0.042(3) 0.016(3) 0.003(2) 0.006(2) 0.012(2) O10 0.029(3) 0.039(3) 0.008(2) 0.003(2) -0.0009(19) 0.011(2) C17 0.016(3) 0.016(3) 0.015(3) 0.002(2) 0.001(2) -0.001(2) C30 0.019(4) 0.029(4) 0.030(4) 0.000(3) 0.011(3) 0.004(3) C14 0.064(6) 0.046(5) 0.020(4) 0.008(4) -0.003(4) -0.011(5) C35 0.019(3) 0.022(4) 0.020(4) -0.003(3) 0.003(3) -0.002(3) C3 0.019(3) 0.026(4) 0.015(3) 0.005(3) -0.003(3) 0.002(3) C7 0.023(4) 0.021(3) 0.019(4) 0.003(3) 0.002(3) -0.001(3) N3 0.029(3) 0.031(3) 0.020(3) 0.006(3) 0.010(2) 0.009(3) C33 0.018(3) 0.019(3) 0.024(4) 0.002(3) 0.003(3) -0.002(3) C1 0.015(3) 0.026(4) 0.014(3) 0.006(3) 0.004(2) 0.007(3) C16 0.018(3) 0.018(3) 0.013(3) 0.004(3) 0.000(2) 0.001(3) C2 0.023(4) 0.022(3) 0.014(3) 0.005(3) 0.002(3) -0.001(3) C6 0.035(4) 0.013(3) 0.024(4) -0.001(3) 0.000(3) 0.003(3) C32 0.023(4) 0.032(4) 0.020(4) -0.001(3) -0.005(3) -0.003(3) C34 0.016(3) 0.025(4) 0.031(4) 0.002(3) 0.004(3) 0.004(3) O18 0.102(4) 0.069(3) 0.024(2) 0.012(2) -0.014(3) -0.013(3) C29 0.021(4) 0.031(4) 0.019(4) 0.001(3) 0.003(3) -0.002(3) N2 0.027(3) 0.029(3) 0.018(3) 0.003(2) 0.005(2) 0.010(3) O6 0.056(4) 0.070(4) 0.017(3) 0.006(3) 0.000(3) -0.009(3) O12 0.103(6) 0.051(4) 0.018(3) 0.004(3) 0.010(3) 0.009(4) C9 0.034(4) 0.037(4) 0.022(4) 0.005(3) 0.005(3) -0.001(3) C5 0.036(4) 0.023(4) 0.025(4) -0.002(3) 0.006(3) -0.003(3) O5 0.077(5) 0.074(5) 0.020(3) 0.000(3) -0.014(3) -0.015(4) C4 0.022(4) 0.033(4) 0.020(4) 0.007(3) 0.007(3) 0.000(3) C15 0.019(3) 0.022(3) 0.017(3) 0.001(3) 0.007(3) 0.004(3) O3W 0.104(6) 0.077(5) 0.039(4) 0.020(4) 0.015(4) 0.028(5) N1 0.020(3) 0.029(3) 0.013(3) 0.003(2) 0.002(2) 0.004(2) C20 0.040(4) 0.040(4) 0.010(3) 0.003(3) -0.001(3) 0.010(4) C22 0.038(4) 0.038(4) 0.013(4) 0.008(3) 0.005(3) 0.012(3) C31 0.015(3) 0.034(4) 0.033(4) -0.002(3) 0.001(3) 0.007(3) C8 0.031(4) 0.028(4) 0.021(4) 0.002(3) -0.003(3) -0.007(3) C42 0.078(7) 0.062(6) 0.015(4) 0.006(4) 0.001(4) 0.008(6) O11 0.125(7) 0.058(4) 0.018(3) 0.012(3) 0.015(4) 0.030(4) C10 0.042(5) 0.039(5) 0.026(4) 0.002(3) -0.002(3) -0.005(4) C23 0.045(5) 0.034(4) 0.019(4) 0.005(3) 0.000(3) 0.016(4) C36 0.028(4) 0.056(5) 0.021(4) 0.011(4) 0.009(3) 0.011(4) C28 0.077(7) 0.056(6) 0.020(5) 0.009(4) 0.007(4) 0.017(5) C24 0.054(5) 0.043(5) 0.017(4) 0.005(3) 0.005(4) 0.020(4) C13 0.037(5) 0.082(7) 0.028(5) -0.005(5) 0.007(4) -0.018(5) O2W 0.202(11) 0.067(5) 0.039(5) 0.020(4) 0.011(6) -0.022(6) C27 0.078(7) 0.046(5) 0.020(4) 0.009(4) -0.002(4) 0.008(5) C12 0.028(5) 0.127(11) 0.047(6) 0.003(6) 0.000(4) -0.019(6) C11 0.052(6) 0.080(7) 0.027(5) 0.003(5) -0.010(4) -0.011(5) C18 0.019(3) 0.030(4) 0.019(4) -0.001(3) -0.001(3) 0.007(3) C19 0.026(4) 0.048(5) 0.025(4) 0.003(3) -0.006(3) 0.017(4) O17 0.102(4) 0.069(3) 0.024(2) 0.012(2) -0.014(3) -0.013(3) C37 0.043(5) 0.046(5) 0.015(4) -0.001(3) 0.004(3) 0.005(4) C38 0.050(5) 0.067(6) 0.017(4) 0.009(4) 0.007(4) 0.005(5) C25 0.089(8) 0.054(6) 0.020(5) 0.017(4) 0.000(5) 0.009(5) C26 0.098(9) 0.043(6) 0.041(6) 0.019(5) -0.001(5) -0.009(5) C45 0.050(6) 0.074(8) 0.088(9) 0.049(7) -0.005(6) 0.011(6) C43 0.055(7) 0.087(9) 0.092(9) 0.056(7) 0.008(6) -0.002(6) C39 0.064(7) 0.141(12) 0.033(6) 0.039(7) 0.006(5) -0.024(7) C44 0.081(9) 0.056(7) 0.097(10) -0.012(7) -0.004(7) 0.001(6) N4 0.044(5) 0.068(6) 0.075(6) 0.046(5) 0.017(4) 0.011(4) C41 0.034(5) 0.141(11) 0.039(6) 0.039(7) 0.003(4) -0.004(6) C40 0.042(6) 0.191(16) 0.050(7) 0.056(9) -0.002(5) -0.033(8) O5W 0.081(7) 0.073(6) 0.345(19) 0.085(9) -0.107(10) -0.021(5) N5 0.087(6) 0.087(6) 0.087(7) 0.005(5) 0.014(5) -0.003(5) O4W 0.099(8) 0.196(13) 0.099(8) -0.015(8) 0.025(6) -0.001(8) C46 0.105(12) 0.164(17) 0.082(11) -0.049(11) 0.031(9) -0.026(11) C47 0.188(19) 0.084(10) 0.135(15) 0.054(10) 0.053(13) 0.048(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.353(5) . ? Eu1 O8 2.356(4) . ? Eu1 O19 2.392(5) . ? Eu1 O2 2.406(5) 2_566 ? Eu1 O15 2.458(5) . ? Eu1 O9 2.469(4) 2_566 ? Eu1 O1W 2.483(5) . ? Eu1 O14 2.549(5) . ? Eu1 O8 2.678(4) 2_566 ? Eu1 C35 2.860(7) . ? Eu1 C21 2.943(6) 2_566 ? Eu1 Eu1 3.9646(6) 2_566 ? Eu2 O2W 2.379(8) . ? Eu2 O18 2.375(8) 2 ? Eu2 O11 2.386(7) . ? Eu2 O12 2.422(7) 2 ? Eu2 O6 2.427(5) 2 ? Eu2 O3W 2.464(8) . ? Eu2 O17 2.477(7) . ? Eu2 O5 2.593(7) 2 ? Eu2 O18 2.679(6) . ? Eu2 C14 2.871(9) 2 ? Eu2 C42 2.946(9) . ? Eu2 Eu2 4.0940(9) 2 ? P3 N2 1.567(6) . ? P3 O16 1.576(5) . ? P3 N3 1.588(6) . ? P3 O13 1.592(5) . ? P1 O1 1.574(5) . ? P1 N1 1.583(6) . ? P1 N2 1.585(6) . ? P1 O4 1.595(5) . ? P2 N3 1.572(6) . ? P2 N1 1.573(6) . ? P2 O7 1.581(5) . ? P2 O10 1.591(5) . ? O3 C7 1.257(8) . ? O9 C21 1.258(8) . ? O9 Eu1 2.469(4) 2_566 ? O1 C1 1.422(8) . ? O8 C21 1.269(7) . ? O8 Eu1 2.678(4) 2_566 ? O7 C15 1.413(8) . ? O2 C7 1.265(8) . ? O2 Eu1 2.406(5) 2_566 ? O15 C35 1.268(8) . ? O14 C35 1.248(8) . ? O4 C8 1.393(8) . ? O13 C29 1.402(8) . ? C21 C17 1.480(9) . ? C21 Eu1 2.943(6) 2_566 ? O19 C45 1.216(12) . ? O16 C36 1.398(9) . ? O10 C22 1.409(8) . ? C17 C16 1.389(9) . ? C17 C18 1.400(9) . ? C30 C31 1.368(10) . ? C30 C29 1.379(10) . ? C30 H30A 0.9300 . ? C14 O6 1.257(11) . ? C14 O5 1.268(10) . ? C14 C10 1.490(12) . ? C14 Eu2 2.871(9) 2 ? C35 C33 1.502(9) . ? C3 C2 1.378(9) . ? C3 C4 1.392(10) . ? C3 C7 1.500(9) . ? C33 C32 1.377(9) . ? C33 C34 1.379(10) . ? C1 C2 1.370(9) . ? C1 C6 1.371(10) . ? C16 C15 1.377(9) . ? C16 H16A 0.9300 . ? C2 H2A 0.9300 . ? C6 C5 1.377(10) . ? C6 H6A 0.9300 . ? C32 C31 1.383(10) . ? C32 H32A 0.9300 . ? C34 C29 1.385(10) . ? C34 H34A 0.9300 . ? O18 C42 1.250(12) . ? O18 Eu2 2.375(8) 2 ? O6 Eu2 2.427(5) 2 ? O12 C28 1.241(12) . ? O12 Eu2 2.422(7) 2 ? C9 C8 1.379(10) . ? C9 C10 1.394(11) . ? C9 H9A 0.9300 . ? C5 C4 1.383(10) . ? C5 H5A 0.9300 . ? O5 Eu2 2.593(7) 2 ? C4 H4A 0.9300 . ? C15 C20 1.389(10) . ? C20 C19 1.376(10) . ? C20 H20A 0.9300 . ? C22 C27 1.365(12) . ? C22 C23 1.371(10) . ? C31 H31A 0.9300 . ? C8 C13 1.386(11) . ? C42 O17 1.253(11) . ? C42 C38 1.489(12) . ? O11 C28 1.252(11) . ? C10 C11 1.377(13) . ? C23 C24 1.391(11) . ? C23 H23A 0.9300 . ? C36 C41 1.358(13) . ? C36 C37 1.394(11) . ? C28 C24 1.505(12) . ? C24 C25 1.362(13) . ? C13 C12 1.400(13) . ? C13 H13A 0.9300 . ? C27 C26 1.390(12) . ? C27 H27A 0.9300 . ? C12 C11 1.375(14) . ? C12 H12A 0.9300 . ? C11 H11A 0.9300 . ? C18 C19 1.380(10) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C37 C38 1.386(12) . ? C37 H37A 0.9300 . ? C38 C39 1.365(14) . ? C25 C26 1.408(14) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C45 N4 1.267(14) . ? C45 H45A 0.9300 . ? C43 N4 1.428(13) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C39 C40 1.354(15) . ? C39 H39A 0.9300 . ? C44 N4 1.474(15) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C41 C40 1.416(14) . ? C41 H41A 0.9300 . ? C40 H40A 0.9300 . ? N5 C46 1.455(17) . ? N5 C47 1.485(17) . ? N5 H5B 0.8600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 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 O3 Eu1 O8 71.63(15) . . ? O3 Eu1 O19 132.86(17) . . ? O8 Eu1 O19 76.30(17) . . ? O3 Eu1 O2 133.88(16) . 2_566 ? O8 Eu1 O2 83.87(16) . 2_566 ? O19 Eu1 O2 73.70(18) . 2_566 ? O3 Eu1 O15 76.29(17) . . ? O8 Eu1 O15 91.36(15) . . ? O19 Eu1 O15 70.83(18) . . ? O2 Eu1 O15 144.33(17) 2_566 . ? O3 Eu1 O9 83.20(16) . 2_566 ? O8 Eu1 O9 126.20(15) . 2_566 ? O19 Eu1 O9 143.92(17) . 2_566 ? O2 Eu1 O9 80.75(16) 2_566 2_566 ? O15 Eu1 O9 128.21(15) . 2_566 ? O3 Eu1 O1W 140.54(15) . . ? O8 Eu1 O1W 147.15(15) . . ? O19 Eu1 O1W 73.88(16) . . ? O2 Eu1 O1W 74.86(16) 2_566 . ? O15 Eu1 O1W 91.64(17) . . ? O9 Eu1 O1W 75.15(15) 2_566 . ? O3 Eu1 O14 74.41(16) . . ? O8 Eu1 O14 134.99(15) . . ? O19 Eu1 O14 108.10(17) . . ? O2 Eu1 O14 141.03(16) 2_566 . ? O15 Eu1 O14 52.02(15) . . ? O9 Eu1 O14 76.87(15) 2_566 . ? O1W Eu1 O14 68.81(16) . . ? O3 Eu1 O8 69.72(15) . 2_566 ? O8 Eu1 O8 76.28(15) . 2_566 ? O19 Eu1 O8 133.60(16) . 2_566 ? O2 Eu1 O8 66.76(15) 2_566 2_566 ? O15 Eu1 O8 145.94(16) . 2_566 ? O9 Eu1 O8 50.27(14) 2_566 2_566 ? O1W Eu1 O8 115.98(14) . 2_566 ? O14 Eu1 O8 117.79(15) . 2_566 ? O3 Eu1 C35 74.88(18) . . ? O8 Eu1 C35 114.78(17) . . ? O19 Eu1 C35 88.73(19) . . ? O2 Eu1 C35 150.96(18) 2_566 . ? O15 Eu1 C35 26.22(17) . . ? O9 Eu1 C35 102.58(17) 2_566 . ? O1W Eu1 C35 78.15(17) . . ? O14 Eu1 C35 25.85(17) . . ? O8 Eu1 C35 136.95(17) 2_566 . ? O3 Eu1 C21 77.56(17) . 2_566 ? O8 Eu1 C21 101.81(16) . 2_566 ? O19 Eu1 C21 143.50(18) . 2_566 ? O2 Eu1 C21 69.87(17) 2_566 2_566 ? O15 Eu1 C21 145.15(17) . 2_566 ? O9 Eu1 C21 24.96(15) 2_566 2_566 ? O1W Eu1 C21 94.12(17) . 2_566 ? O14 Eu1 C21 98.74(16) . 2_566 ? O8 Eu1 C21 25.53(15) 2_566 2_566 ? C35 Eu1 C21 123.10(18) . 2_566 ? O3 Eu1 Eu1 65.07(11) . 2_566 ? O8 Eu1 Eu1 41.02(11) . 2_566 ? O19 Eu1 Eu1 108.97(13) . 2_566 ? O2 Eu1 Eu1 70.73(11) 2_566 2_566 ? O15 Eu1 Eu1 125.02(12) . 2_566 ? O9 Eu1 Eu1 85.36(10) 2_566 2_566 ? O1W Eu1 Eu1 142.67(11) . 2_566 ? O14 Eu1 Eu1 137.32(12) . 2_566 ? O8 Eu1 Eu1 35.26(9) 2_566 2_566 ? C35 Eu1 Eu1 137.97(14) . 2_566 ? C21 Eu1 Eu1 60.79(12) 2_566 2_566 ? O2W Eu2 O18 145.6(3) . 2 ? O2W Eu2 O11 75.7(3) . . ? O18 Eu2 O11 77.1(3) 2 . ? O2W Eu2 O12 144.4(3) . 2 ? O18 Eu2 O12 69.8(3) 2 2 ? O11 Eu2 O12 133.9(2) . 2 ? O2W Eu2 O6 90.9(2) . 2 ? O18 Eu2 O6 97.5(2) 2 2 ? O11 Eu2 O6 141.5(2) . 2 ? O12 Eu2 O6 75.4(2) 2 2 ? O2W Eu2 O3W 77.8(3) . . ? O18 Eu2 O3W 73.9(3) 2 . ? O11 Eu2 O3W 71.8(2) . . ? O12 Eu2 O3W 125.1(3) 2 . ? O6 Eu2 O3W 70.2(2) 2 . ? O2W Eu2 O17 76.7(3) . . ? O18 Eu2 O17 121.3(2) 2 . ? O11 Eu2 O17 84.8(3) . . ? O12 Eu2 O17 85.9(3) 2 . ? O6 Eu2 O17 127.6(2) 2 . ? O3W Eu2 O17 148.8(3) . . ? O2W Eu2 O5 77.3(3) . 2 ? O18 Eu2 O5 132.9(2) 2 2 ? O11 Eu2 O5 149.7(2) . 2 ? O12 Eu2 O5 68.3(2) 2 2 ? O6 Eu2 O5 51.8(2) 2 2 ? O3W Eu2 O5 115.4(2) . 2 ? O17 Eu2 O5 75.8(2) . 2 ? O2W Eu2 O18 115.0(3) . . ? O18 Eu2 O18 72.0(3) 2 . ? O11 Eu2 O18 66.8(2) . . ? O12 Eu2 O18 73.0(2) 2 . ? O6 Eu2 O18 148.3(2) 2 . ? O3W Eu2 O18 130.7(3) . . ? O17 Eu2 O18 49.8(2) . . ? O5 Eu2 O18 113.9(2) 2 . ? O2W Eu2 C14 85.6(3) . 2 ? O18 Eu2 C14 115.1(2) 2 2 ? O11 Eu2 C14 158.2(2) . 2 ? O12 Eu2 C14 67.7(2) 2 2 ? O6 Eu2 C14 25.8(2) 2 2 ? O3W Eu2 C14 93.7(3) . 2 ? O17 Eu2 C14 101.9(3) . 2 ? O5 Eu2 C14 26.2(2) 2 2 ? O18 Eu2 C14 132.9(3) . 2 ? O2W Eu2 C42 94.6(3) . . ? O18 Eu2 C42 97.0(3) 2 . ? O11 Eu2 C42 72.5(3) . . ? O12 Eu2 C42 80.6(2) 2 . ? O6 Eu2 C42 145.5(3) 2 . ? O3W Eu2 C42 144.2(3) . . ? O17 Eu2 C42 24.8(3) . . ? O5 Eu2 C42 96.3(3) 2 . ? O18 Eu2 C42 25.1(2) . . ? C14 Eu2 C42 120.8(3) 2 . ? O2W Eu2 Eu2 139.01(18) . 2 ? O18 Eu2 Eu2 38.47(15) 2 2 ? O11 Eu2 Eu2 67.23(16) . 2 ? O12 Eu2 Eu2 66.91(16) 2 2 ? O6 Eu2 Eu2 129.22(16) 2 2 ? O3W Eu2 Eu2 105.40(19) . 2 ? O17 Eu2 Eu2 83.05(16) . 2 ? O5 Eu2 Eu2 131.32(17) 2 2 ? O18 Eu2 Eu2 33.48(17) . 2 ? C14 Eu2 Eu2 133.76(19) 2 2 ? C42 Eu2 Eu2 58.6(2) . 2 ? N2 P3 O16 105.4(3) . . ? N2 P3 N3 117.5(3) . . ? O16 P3 N3 112.0(3) . . ? N2 P3 O13 111.3(3) . . ? O16 P3 O13 99.3(3) . . ? N3 P3 O13 109.7(3) . . ? O1 P1 N1 112.6(3) . . ? O1 P1 N2 105.6(3) . . ? N1 P1 N2 117.3(3) . . ? O1 P1 O4 98.9(3) . . ? N1 P1 O4 110.0(3) . . ? N2 P1 O4 110.8(3) . . ? N3 P2 N1 118.6(3) . . ? N3 P2 O7 104.7(3) . . ? N1 P2 O7 110.8(3) . . ? N3 P2 O10 111.2(3) . . ? N1 P2 O10 106.2(3) . . ? O7 P2 O10 104.8(3) . . ? C7 O3 Eu1 137.8(4) . . ? C21 O9 Eu1 99.1(4) . 2_566 ? C1 O1 P1 123.3(4) . . ? C21 O8 Eu1 167.3(4) . . ? C21 O8 Eu1 89.0(4) . 2_566 ? Eu1 O8 Eu1 103.72(15) . 2_566 ? C15 O7 P2 124.7(4) . . ? C7 O2 Eu1 130.5(4) . 2_566 ? C35 O15 Eu1 94.9(4) . . ? C35 O14 Eu1 91.2(4) . . ? C8 O4 P1 122.6(5) . . ? C29 O13 P3 125.0(4) . . ? O9 C21 O8 120.6(6) . . ? O9 C21 C17 119.8(5) . . ? O8 C21 C17 119.6(6) . . ? O9 C21 Eu1 55.9(3) . 2_566 ? O8 C21 Eu1 65.5(3) . 2_566 ? C17 C21 Eu1 167.2(4) . 2_566 ? C45 O19 Eu1 135.7(6) . . ? C36 O16 P3 125.7(5) . . ? C22 O10 P2 122.1(5) . . ? C16 C17 C18 119.7(6) . . ? C16 C17 C21 120.3(5) . . ? C18 C17 C21 120.0(6) . . ? C31 C30 C29 119.3(6) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? O6 C14 O5 121.0(8) . . ? O6 C14 C10 118.9(7) . . ? O5 C14 C10 120.1(9) . . ? O6 C14 Eu2 57.0(4) . 2 ? O5 C14 Eu2 64.6(5) . 2 ? C10 C14 Eu2 170.2(6) . 2 ? O14 C35 O15 121.7(6) . . ? O14 C35 C33 120.6(6) . . ? O15 C35 C33 117.7(6) . . ? O14 C35 Eu1 63.0(3) . . ? O15 C35 Eu1 58.9(3) . . ? C33 C35 Eu1 173.1(5) . . ? C2 C3 C4 119.6(6) . . ? C2 C3 C7 118.3(6) . . ? C4 C3 C7 122.1(6) . . ? O3 C7 O2 125.8(6) . . ? O3 C7 C3 116.4(6) . . ? O2 C7 C3 117.8(6) . . ? P2 N3 P3 121.2(4) . . ? C32 C33 C34 120.4(6) . . ? C32 C33 C35 120.5(6) . . ? C34 C33 C35 119.0(6) . . ? C2 C1 C6 122.6(6) . . ? C2 C1 O1 117.1(6) . . ? C6 C1 O1 120.1(6) . . ? C15 C16 C17 118.9(6) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C1 C6 C5 118.1(6) . . ? C1 C6 H6A 120.9 . . ? C5 C6 H6A 120.9 . . ? C33 C32 C31 120.0(6) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C34 C29 118.8(6) . . ? C33 C34 H34A 120.6 . . ? C29 C34 H34A 120.6 . . ? C42 O18 Eu2 162.4(6) . 2 ? C42 O18 Eu2 89.5(5) . . ? Eu2 O18 Eu2 108.0(3) 2 . ? C30 C29 C34 121.1(7) . . ? C30 C29 O13 115.5(6) . . ? C34 C29 O13 123.3(6) . . ? P3 N2 P1 122.8(4) . . ? C14 O6 Eu2 97.3(5) . 2 ? C28 O12 Eu2 129.6(7) . 2 ? C8 C9 C10 119.5(8) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C6 C5 C4 120.8(7) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C14 O5 Eu2 89.2(6) . 2 ? C5 C4 C3 119.8(7) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C16 C15 C20 121.8(6) . . ? C16 C15 O7 117.7(6) . . ? C20 C15 O7 120.4(6) . . ? P2 N1 P1 121.1(4) . . ? C19 C20 C15 118.8(6) . . ? C19 C20 H20A 120.6 . . ? C15 C20 H20A 120.6 . . ? C27 C22 C23 121.5(7) . . ? C27 C22 O10 121.2(7) . . ? C23 C22 O10 117.3(7) . . ? C30 C31 C32 120.3(6) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C9 C8 C13 121.5(7) . . ? C9 C8 O4 121.6(7) . . ? C13 C8 O4 116.9(7) . . ? O17 C42 O18 120.9(8) . . ? O17 C42 C38 119.6(10) . . ? O18 C42 C38 119.6(9) . . ? O17 C42 Eu2 56.2(5) . . ? O18 C42 Eu2 65.4(5) . . ? C38 C42 Eu2 169.8(7) . . ? C28 O11 Eu2 133.2(6) . . ? C11 C10 C9 119.3(8) . . ? C11 C10 C14 122.4(8) . . ? C9 C10 C14 118.3(8) . . ? C22 C23 C24 119.5(8) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C41 C36 C37 121.7(8) . . ? C41 C36 O16 121.4(7) . . ? C37 C36 O16 116.7(7) . . ? O12 C28 O11 126.5(9) . . ? O12 C28 C24 118.1(8) . . ? O11 C28 C24 115.4(9) . . ? C25 C24 C23 120.1(8) . . ? C25 C24 C28 120.1(8) . . ? C23 C24 C28 119.8(8) . . ? C8 C13 C12 118.4(8) . . ? C8 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C22 C27 C26 119.6(8) . . ? C22 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C11 C12 C13 120.0(9) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C11 C10 121.2(8) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C20 C19 C18 120.7(6) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C42 O17 Eu2 99.0(6) . . ? C38 C37 C36 118.8(8) . . ? C38 C37 H37A 120.6 . . ? C36 C37 H37A 120.6 . . ? C39 C38 C37 119.7(8) . . ? C39 C38 C42 119.9(9) . . ? C37 C38 C42 120.3(9) . . ? C24 C25 C26 120.1(8) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C27 C26 C25 119.2(9) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? O19 C45 N4 133.1(13) . . ? O19 C45 H45A 113.4 . . ? N4 C45 H45A 113.4 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C39 C38 121.6(10) . . ? C40 C39 H39A 119.2 . . ? C38 C39 H39A 119.2 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C45 N4 C43 128.6(12) . . ? C45 N4 C44 116.9(11) . . ? C43 N4 C44 114.5(10) . . ? C36 C41 C40 118.2(9) . . ? C36 C41 H41A 120.9 . . ? C40 C41 H41A 120.9 . . ? C39 C40 C41 120.0(10) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C46 N5 C47 115.1(13) . . ? C46 N5 H5B 122.4 . . ? C47 N5 H5B 122.4 . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 C47 H47A 109.5 . . ? N5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 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 O8 Eu1 O3 C7 -7.6(6) . . . . ? O19 Eu1 O3 C7 -57.1(7) . . . . ? O2 Eu1 O3 C7 54.1(7) 2_566 . . . ? O15 Eu1 O3 C7 -103.7(7) . . . . ? O9 Eu1 O3 C7 124.2(7) 2_566 . . . ? O1W Eu1 O3 C7 -179.2(6) . . . . ? O14 Eu1 O3 C7 -157.6(7) . . . . ? O8 Eu1 O3 C7 74.2(6) 2_566 . . . ? C35 Eu1 O3 C7 -130.7(7) . . . . ? C21 Eu1 O3 C7 99.5(7) 2_566 . . . ? Eu1 Eu1 O3 C7 36.2(6) 2_566 . . . ? N1 P1 O1 C1 41.7(6) . . . . ? N2 P1 O1 C1 170.9(5) . . . . ? O4 P1 O1 C1 -74.5(5) . . . . ? O3 Eu1 O8 C21 -111.2(19) . . . . ? O19 Eu1 O8 C21 33.8(19) . . . . ? O2 Eu1 O8 C21 108.4(19) 2_566 . . . ? O15 Eu1 O8 C21 -36.1(19) . . . . ? O9 Eu1 O8 C21 -177.8(19) 2_566 . . . ? O1W Eu1 O8 C21 59(2) . . . . ? O14 Eu1 O8 C21 -68(2) . . . . ? O8 Eu1 O8 C21 176(2) 2_566 . . . ? C35 Eu1 O8 C21 -48(2) . . . . ? C21 Eu1 O8 C21 176.4(18) 2_566 . . . ? Eu1 Eu1 O8 C21 176(2) 2_566 . . . ? O3 Eu1 O8 Eu1 72.85(17) . . . 2_566 ? O19 Eu1 O8 Eu1 -142.2(2) . . . 2_566 ? O2 Eu1 O8 Eu1 -67.52(17) 2_566 . . 2_566 ? O15 Eu1 O8 Eu1 147.92(17) . . . 2_566 ? O9 Eu1 O8 Eu1 6.3(2) 2_566 . . 2_566 ? O1W Eu1 O8 Eu1 -116.9(3) . . . 2_566 ? O14 Eu1 O8 Eu1 115.8(2) . . . 2_566 ? O8 Eu1 O8 Eu1 0.0 2_566 . . 2_566 ? C35 Eu1 O8 Eu1 135.71(18) . . . 2_566 ? C21 Eu1 O8 Eu1 0.39(19) 2_566 . . 2_566 ? N3 P2 O7 C15 -179.2(5) . . . . ? N1 P2 O7 C15 -50.3(6) . . . . ? O10 P2 O7 C15 63.8(5) . . . . ? O3 Eu1 O15 C35 -83.5(4) . . . . ? O8 Eu1 O15 C35 -154.3(4) . . . . ? O19 Eu1 O15 C35 130.8(4) . . . . ? O2 Eu1 O15 C35 124.4(4) 2_566 . . . ? O9 Eu1 O15 C35 -13.9(5) 2_566 . . . ? O1W Eu1 O15 C35 58.5(4) . . . . ? O14 Eu1 O15 C35 -2.8(4) . . . . ? O8 Eu1 O15 C35 -87.1(5) 2_566 . . . ? C21 Eu1 O15 C35 -41.2(6) 2_566 . . . ? Eu1 Eu1 O15 C35 -129.1(4) 2_566 . . . ? O3 Eu1 O14 C35 87.4(4) . . . . ? O8 Eu1 O14 C35 45.3(5) . . . . ? O19 Eu1 O14 C35 -43.3(4) . . . . ? O2 Eu1 O14 C35 -129.5(4) 2_566 . . . ? O15 Eu1 O14 C35 2.8(4) . . . . ? O9 Eu1 O14 C35 173.9(4) 2_566 . . . ? O1W Eu1 O14 C35 -107.2(4) . . . . ? O8 Eu1 O14 C35 143.8(4) 2_566 . . . ? C21 Eu1 O14 C35 161.8(4) 2_566 . . . ? Eu1 Eu1 O14 C35 105.9(4) 2_566 . . . ? O1 P1 O4 C8 166.0(5) . . . . ? N1 P1 O4 C8 47.9(6) . . . . ? N2 P1 O4 C8 -83.5(6) . . . . ? N2 P3 O13 C29 -52.3(6) . . . . ? O16 P3 O13 C29 -163.0(5) . . . . ? N3 P3 O13 C29 79.4(6) . . . . ? Eu1 O9 C21 O8 -11.0(7) 2_566 . . . ? Eu1 O9 C21 C17 165.8(5) 2_566 . . . ? Eu1 O8 C21 O9 -166.1(15) . . . . ? Eu1 O8 C21 O9 10.0(6) 2_566 . . . ? Eu1 O8 C21 C17 17(2) . . . . ? Eu1 O8 C21 C17 -166.8(5) 2_566 . . . ? Eu1 O8 C21 Eu1 -176(2) . . . 2_566 ? O3 Eu1 O19 C45 -105.4(11) . . . . ? O8 Eu1 O19 C45 -153.4(11) . . . . ? O2 Eu1 O19 C45 119.0(11) 2_566 . . . ? O15 Eu1 O19 C45 -57.1(11) . . . . ? O9 Eu1 O19 C45 72.3(11) 2_566 . . . ? O1W Eu1 O19 C45 40.5(11) . . . . ? O14 Eu1 O19 C45 -20.1(11) . . . . ? O8 Eu1 O19 C45 151.2(10) 2_566 . . . ? C35 Eu1 O19 C45 -37.5(11) . . . . ? C21 Eu1 O19 C45 115.1(11) 2_566 . . . ? Eu1 Eu1 O19 C45 -178.6(11) 2_566 . . . ? N2 P3 O16 C36 179.4(5) . . . . ? N3 P3 O16 C36 50.5(6) . . . . ? O13 P3 O16 C36 -65.3(6) . . . . ? N3 P2 O10 C22 -32.4(6) . . . . ? N1 P2 O10 C22 -162.7(5) . . . . ? O7 P2 O10 C22 80.1(5) . . . . ? O9 C21 C17 C16 -164.7(6) . . . . ? O8 C21 C17 C16 12.2(9) . . . . ? Eu1 C21 C17 C16 -98.0(19) 2_566 . . . ? O9 C21 C17 C18 14.2(9) . . . . ? O8 C21 C17 C18 -169.0(6) . . . . ? Eu1 C21 C17 C18 81(2) 2_566 . . . ? Eu1 O14 C35 O15 -5.0(7) . . . . ? Eu1 O14 C35 C33 173.3(6) . . . . ? Eu1 O15 C35 O14 5.3(7) . . . . ? Eu1 O15 C35 C33 -173.1(5) . . . . ? O3 Eu1 C35 O14 -85.4(4) . . . . ? O8 Eu1 C35 O14 -146.4(4) . . . . ? O19 Eu1 C35 O14 139.3(4) . . . . ? O2 Eu1 C35 O14 87.5(5) 2_566 . . . ? O15 Eu1 C35 O14 -175.0(7) . . . . ? O9 Eu1 C35 O14 -6.1(4) 2_566 . . . ? O1W Eu1 C35 O14 65.5(4) . . . . ? O8 Eu1 C35 O14 -50.0(5) 2_566 . . . ? C21 Eu1 C35 O14 -21.7(5) 2_566 . . . ? Eu1 Eu1 C35 O14 -103.2(4) 2_566 . . . ? O3 Eu1 C35 O15 89.6(4) . . . . ? O8 Eu1 C35 O15 28.6(5) . . . . ? O19 Eu1 C35 O15 -45.7(4) . . . . ? O2 Eu1 C35 O15 -97.5(5) 2_566 . . . ? O9 Eu1 C35 O15 168.9(4) 2_566 . . . ? O1W Eu1 C35 O15 -119.5(4) . . . . ? O14 Eu1 C35 O15 175.0(7) . . . . ? O8 Eu1 C35 O15 125.0(4) 2_566 . . . ? C21 Eu1 C35 O15 153.3(4) 2_566 . . . ? Eu1 Eu1 C35 O15 71.8(5) 2_566 . . . ? O3 Eu1 C35 C33 151(4) . . . . ? O8 Eu1 C35 C33 90(4) . . . . ? O19 Eu1 C35 C33 16(4) . . . . ? O2 Eu1 C35 C33 -36(4) 2_566 . . . ? O15 Eu1 C35 C33 62(4) . . . . ? O9 Eu1 C35 C33 -129(4) 2_566 . . . ? O1W Eu1 C35 C33 -58(4) . . . . ? O14 Eu1 C35 C33 -123(4) . . . . ? O8 Eu1 C35 C33 -173(4) 2_566 . . . ? C21 Eu1 C35 C33 -145(4) 2_566 . . . ? Eu1 Eu1 C35 C33 134(4) 2_566 . . . ? Eu1 O3 C7 O2 -44.5(11) . . . . ? Eu1 O3 C7 C3 133.0(5) . . . . ? Eu1 O2 C7 O3 9.8(10) 2_566 . . . ? Eu1 O2 C7 C3 -167.6(4) 2_566 . . . ? C2 C3 C7 O3 -31.4(9) . . . . ? C4 C3 C7 O3 150.2(6) . . . . ? C2 C3 C7 O2 146.3(6) . . . . ? C4 C3 C7 O2 -32.2(9) . . . . ? N1 P2 N3 P3 13.6(6) . . . . ? O7 P2 N3 P3 137.6(4) . . . . ? O10 P2 N3 P3 -109.8(4) . . . . ? N2 P3 N3 P2 -4.4(6) . . . . ? O16 P3 N3 P2 117.9(4) . . . . ? O13 P3 N3 P2 -132.8(4) . . . . ? O14 C35 C33 C32 -11.3(10) . . . . ? O15 C35 C33 C32 167.0(7) . . . . ? Eu1 C35 C33 C32 109(4) . . . . ? O14 C35 C33 C34 172.2(7) . . . . ? O15 C35 C33 C34 -9.4(10) . . . . ? Eu1 C35 C33 C34 -68(4) . . . . ? P1 O1 C1 C2 -98.6(6) . . . . ? P1 O1 C1 C6 86.1(7) . . . . ? C18 C17 C16 C15 -2.5(10) . . . . ? C21 C17 C16 C15 176.3(6) . . . . ? C6 C1 C2 C3 -1.9(10) . . . . ? O1 C1 C2 C3 -177.0(5) . . . . ? C4 C3 C2 C1 0.3(9) . . . . ? C7 C3 C2 C1 -178.2(6) . . . . ? C2 C1 C6 C5 2.1(10) . . . . ? O1 C1 C6 C5 177.1(6) . . . . ? C34 C33 C32 C31 2.4(11) . . . . ? C35 C33 C32 C31 -174.0(7) . . . . ? C32 C33 C34 C29 -0.5(11) . . . . ? C35 C33 C34 C29 176.0(6) . . . . ? O2W Eu2 O18 C42 -38.0(7) . . . . ? O18 Eu2 O18 C42 178.3(8) 2 . . . ? O11 Eu2 O18 C42 -98.3(6) . . . . ? O12 Eu2 O18 C42 104.6(6) 2 . . . ? O6 Eu2 O18 C42 103.8(7) 2 . . . ? O3W Eu2 O18 C42 -133.4(6) . . . . ? O17 Eu2 O18 C42 5.3(6) . . . . ? O5 Eu2 O18 C42 48.6(7) 2 . . . ? C14 Eu2 O18 C42 70.5(7) 2 . . . ? Eu2 Eu2 O18 C42 178.3(8) 2 . . . ? O2W Eu2 O18 Eu2 143.6(4) . . . 2 ? O18 Eu2 O18 Eu2 0.0 2 . . 2 ? O11 Eu2 O18 Eu2 83.4(4) . . . 2 ? O12 Eu2 O18 Eu2 -73.7(3) 2 . . 2 ? O6 Eu2 O18 Eu2 -74.5(5) 2 . . 2 ? O3W Eu2 O18 Eu2 48.3(4) . . . 2 ? O17 Eu2 O18 Eu2 -173.1(5) . . . 2 ? O5 Eu2 O18 Eu2 -129.7(3) 2 . . 2 ? C14 Eu2 O18 Eu2 -107.8(4) 2 . . 2 ? C42 Eu2 O18 Eu2 -178.3(8) . . . 2 ? C31 C30 C29 C34 3.2(11) . . . . ? C31 C30 C29 O13 -179.0(7) . . . . ? C33 C34 C29 C30 -2.4(11) . . . . ? C33 C34 C29 O13 -180.0(6) . . . . ? P3 O13 C29 C30 147.9(6) . . . . ? P3 O13 C29 C34 -34.4(10) . . . . ? O16 P3 N2 P1 -130.2(4) . . . . ? N3 P3 N2 P1 -4.6(6) . . . . ? O13 P3 N2 P1 123.1(4) . . . . ? O1 P1 N2 P3 -122.3(4) . . . . ? N1 P1 N2 P3 4.0(6) . . . . ? O4 P1 N2 P3 131.5(4) . . . . ? O5 C14 O6 Eu2 9.3(10) . . . 2 ? C10 C14 O6 Eu2 -169.6(7) . . . 2 ? C1 C6 C5 C4 -0.8(11) . . . . ? O6 C14 O5 Eu2 -8.7(9) . . . 2 ? C10 C14 O5 Eu2 170.2(8) . . . 2 ? C6 C5 C4 C3 -0.8(11) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? C7 C3 C4 C5 179.5(6) . . . . ? C17 C16 C15 C20 1.9(10) . . . . ? C17 C16 C15 O7 179.1(6) . . . . ? P2 O7 C15 C16 114.5(6) . . . . ? P2 O7 C15 C20 -68.2(8) . . . . ? N3 P2 N1 P1 -14.2(6) . . . . ? O7 P2 N1 P1 -135.2(4) . . . . ? O10 P2 N1 P1 111.6(4) . . . . ? O1 P1 N1 P2 128.4(4) . . . . ? N2 P1 N1 P2 5.6(5) . . . . ? O4 P1 N1 P2 -122.3(4) . . . . ? C16 C15 C20 C19 -0.1(11) . . . . ? O7 C15 C20 C19 -177.3(7) . . . . ? P2 O10 C22 C27 -61.9(9) . . . . ? P2 O10 C22 C23 120.5(7) . . . . ? C29 C30 C31 C32 -1.2(11) . . . . ? C33 C32 C31 C30 -1.5(11) . . . . ? C10 C9 C8 C13 -2.6(12) . . . . ? C10 C9 C8 O4 175.7(7) . . . . ? P1 O4 C8 C9 61.5(9) . . . . ? P1 O4 C8 C13 -120.2(7) . . . . ? Eu2 O18 C42 O17 165.5(18) 2 . . . ? Eu2 O18 C42 O17 -9.3(10) . . . . ? Eu2 O18 C42 C38 -15(3) 2 . . . ? Eu2 O18 C42 C38 169.9(8) . . . . ? Eu2 O18 C42 Eu2 175(3) 2 . . . ? O2W Eu2 C42 O17 -43.7(7) . . . . ? O18 Eu2 C42 O17 168.8(6) 2 . . . ? O11 Eu2 C42 O17 -117.1(7) . . . . ? O12 Eu2 C42 O17 100.7(6) 2 . . . ? O6 Eu2 C42 O17 54.5(8) 2 . . . ? O3W Eu2 C42 O17 -119.1(7) . . . . ? O5 Eu2 C42 O17 34.0(7) 2 . . . ? O18 Eu2 C42 O17 170.4(11) . . . . ? C14 Eu2 C42 O17 43.9(7) 2 . . . ? Eu2 Eu2 C42 O17 169.3(7) 2 . . . ? O2W Eu2 C42 O18 145.9(6) . . . . ? O18 Eu2 C42 O18 -1.6(8) 2 . . . ? O11 Eu2 C42 O18 72.5(6) . . . . ? O12 Eu2 C42 O18 -69.7(6) 2 . . . ? O6 Eu2 C42 O18 -115.9(7) 2 . . . ? O3W Eu2 C42 O18 70.5(8) . . . . ? O17 Eu2 C42 O18 -170.4(11) . . . . ? O5 Eu2 C42 O18 -136.4(6) 2 . . . ? C14 Eu2 C42 O18 -126.5(6) 2 . . . ? Eu2 Eu2 C42 O18 -1.1(5) 2 . . . ? O2W Eu2 C42 C38 25(4) . . . . ? O18 Eu2 C42 C38 -123(4) 2 . . . ? O11 Eu2 C42 C38 -49(4) . . . . ? O12 Eu2 C42 C38 169(4) 2 . . . ? O6 Eu2 C42 C38 123(4) 2 . . . ? O3W Eu2 C42 C38 -51(4) . . . . ? O17 Eu2 C42 C38 68(4) . . . . ? O5 Eu2 C42 C38 102(4) 2 . . . ? O18 Eu2 C42 C38 -121(4) . . . . ? C14 Eu2 C42 C38 112(4) 2 . . . ? Eu2 Eu2 C42 C38 -122(4) 2 . . . ? O2W Eu2 O11 C28 -145.4(11) . . . . ? O18 Eu2 O11 C28 55.9(10) 2 . . . ? O12 Eu2 O11 C28 11.4(12) 2 . . . ? O6 Eu2 O11 C28 141.8(9) 2 . . . ? O3W Eu2 O11 C28 132.9(11) . . . . ? O17 Eu2 O11 C28 -67.9(10) . . . . ? O5 Eu2 O11 C28 -117.8(10) 2 . . . ? O18 Eu2 O11 C28 -19.7(10) . . . . ? C14 Eu2 O11 C28 -177.1(9) 2 . . . ? C42 Eu2 O11 C28 -45.8(10) . . . . ? Eu2 Eu2 O11 C28 16.7(10) 2 . . . ? C8 C9 C10 C11 3.8(13) . . . . ? C8 C9 C10 C14 -176.1(7) . . . . ? O6 C14 C10 C11 171.8(9) . . . . ? O5 C14 C10 C11 -7.1(14) . . . . ? Eu2 C14 C10 C11 109(4) 2 . . . ? O6 C14 C10 C9 -8.2(13) . . . . ? O5 C14 C10 C9 172.8(8) . . . . ? Eu2 C14 C10 C9 -71(4) 2 . . . ? C27 C22 C23 C24 -0.6(13) . . . . ? O10 C22 C23 C24 177.0(7) . . . . ? P3 O16 C36 C41 62.8(11) . . . . ? P3 O16 C36 C37 -122.6(7) . . . . ? Eu2 O12 C28 O11 56.6(15) 2 . . . ? Eu2 O12 C28 C24 -120.5(8) 2 . . . ? Eu2 O11 C28 O12 -48.2(17) . . . . ? Eu2 O11 C28 C24 129.0(8) . . . . ? C22 C23 C24 C25 0.9(13) . . . . ? C22 C23 C24 C28 -178.6(8) . . . . ? O12 C28 C24 C25 179.8(10) . . . . ? O11 C28 C24 C25 2.3(14) . . . . ? O12 C28 C24 C23 -0.8(14) . . . . ? O11 C28 C24 C23 -178.3(9) . . . . ? C9 C8 C13 C12 0.2(15) . . . . ? O4 C8 C13 C12 -178.1(9) . . . . ? C23 C22 C27 C26 -1.2(14) . . . . ? O10 C22 C27 C26 -178.6(9) . . . . ? C8 C13 C12 C11 0.9(18) . . . . ? C13 C12 C11 C10 0.4(19) . . . . ? C9 C10 C11 C12 -2.8(16) . . . . ? C14 C10 C11 C12 177.2(10) . . . . ? C16 C17 C18 C19 1.5(10) . . . . ? C21 C17 C18 C19 -177.3(7) . . . . ? C15 C20 C19 C18 -1.0(12) . . . . ? C17 C18 C19 C20 0.3(12) . . . . ? O18 C42 O17 Eu2 10.2(11) . . . . ? C38 C42 O17 Eu2 -169.0(8) . . . . ? O2W Eu2 O17 C42 135.0(7) . . . . ? O18 Eu2 O17 C42 -13.0(7) 2 . . . ? O11 Eu2 O17 C42 58.5(6) . . . . ? O12 Eu2 O17 C42 -76.4(6) 2 . . . ? O6 Eu2 O17 C42 -144.4(6) 2 . . . ? O3W Eu2 O17 C42 99.2(7) . . . . ? O5 Eu2 O17 C42 -145.0(7) 2 . . . ? O18 Eu2 O17 C42 -5.3(6) . . . . ? C14 Eu2 O17 C42 -142.5(6) 2 . . . ? Eu2 Eu2 O17 C42 -9.2(6) 2 . . . ? C41 C36 C37 C38 -3.6(14) . . . . ? O16 C36 C37 C38 -178.1(7) . . . . ? C36 C37 C38 C39 2.3(14) . . . . ? C36 C37 C38 C42 178.6(8) . . . . ? O17 C42 C38 C39 -24.1(16) . . . . ? O18 C42 C38 C39 156.7(11) . . . . ? Eu2 C42 C38 C39 -87(4) . . . . ? O17 C42 C38 C37 159.6(9) . . . . ? O18 C42 C38 C37 -19.6(14) . . . . ? Eu2 C42 C38 C37 97(4) . . . . ? C23 C24 C25 C26 0.6(15) . . . . ? C28 C24 C25 C26 -180.0(10) . . . . ? C22 C27 C26 C25 2.6(16) . . . . ? C24 C25 C26 C27 -2.3(17) . . . . ? Eu1 O19 C45 N4 -97.4(14) . . . . ? C37 C38 C39 C40 -1(2) . . . . ? C42 C38 C39 C40 -177.2(13) . . . . ? O19 C45 N4 C43 -177.3(10) . . . . ? O19 C45 N4 C44 1.3(16) . . . . ? C37 C36 C41 C40 3.1(18) . . . . ? O16 C36 C41 C40 177.4(11) . . . . ? C38 C39 C40 C41 0(2) . . . . ? C36 C41 C40 C39 -2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 3.156 _refine_diff_density_min -3.640 _refine_diff_density_rms 0.159 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.500 0.000 145.3 -0.1 _platon_squeeze_details ; ; #_eof #End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 926683'