# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_sm _database_code_depnum_ccdc_archive 'CCDC 918898' #TrackingRef '918898.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H86 Cd3 N6 O35 Sm2, 14(O)' _chemical_formula_sum 'C30 H86 Cd3 N6 O49 Sm2' _chemical_formula_weight 1952.95 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' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.064(3) _cell_length_b 14.808(3) _cell_length_c 14.846(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.89(3) _cell_angle_gamma 90.00 _cell_volume 3177.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6334 _cell_measurement_theta_min 3.0477 _cell_measurement_theta_max 27.5165 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 2.924 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724 (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12586 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5326 _reflns_number_gt 5294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.9296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(8) _refine_ls_number_reflns 5326 _refine_ls_number_parameters 415 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad 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 Sm Sm 0.782792(13) 0.508599(13) 0.676725(15) 0.02164(6) Uani 1 1 d . . . Cd1 Cd 0.78420(2) 0.83028(2) 0.62350(2) 0.02237(8) Uani 1 1 d . . . Cd2 Cd 1.0000 0.38361(3) 1.0000 0.02309(10) Uani 1 2 d SD . . C1 C 1.0281(4) 0.1755(3) 0.9705(4) 0.0351(12) Uani 1 1 d . . . H1A H 1.0933 0.1733 1.0166 0.042 Uiso 1 1 calc R . . H1B H 1.0135 0.1216 0.9293 0.042 Uiso 1 1 calc R . . C2 C 0.9234(3) 0.2494(3) 0.8137(4) 0.0279(10) Uani 1 1 d . . . H2A H 0.8776 0.2180 0.8282 0.033 Uiso 1 1 calc R . . H2B H 0.9334 0.2145 0.7640 0.033 Uiso 1 1 calc R . . C3 C 0.8867(3) 0.3420(3) 0.7714(3) 0.0250(9) Uani 1 1 d . . . C4 C 1.0892(4) 0.2724(4) 0.8818(4) 0.0341(11) Uani 1 1 d . . . H4A H 1.0679 0.3079 0.8209 0.041 Uiso 1 1 calc R . . H4B H 1.1117 0.2151 0.8694 0.041 Uiso 1 1 calc R . . C5 C 1.1690(3) 0.3220(4) 0.9650(4) 0.0358(12) Uani 1 1 d . . . C6 C 0.9948(4) 0.8593(5) 0.6947(4) 0.0420(14) Uani 1 1 d . . . C7 C 0.9926(3) 0.8236(4) 0.7878(4) 0.0344(11) Uani 1 1 d . . . H7A H 1.0066 0.7596 0.7929 0.041 Uiso 1 1 calc R . . H7B H 1.0410 0.8531 0.8452 0.041 Uiso 1 1 calc R . . C8 C 0.8599(3) 0.6775(3) 0.7879(4) 0.0246(9) Uani 1 1 d . . . C9 C 0.8865(3) 0.7640(3) 0.8494(3) 0.0285(10) Uani 1 1 d . . . H9A H 0.8369 0.7817 0.8663 0.034 Uiso 1 1 calc R . . H9B H 0.9416 0.7536 0.9112 0.034 Uiso 1 1 calc R . . C10 C 0.8983(4) 0.9278(3) 0.8324(4) 0.0325(11) Uani 1 1 d . . . H10A H 0.9314 0.9708 0.8108 0.039 Uiso 1 1 calc R . . H10B H 0.9285 0.9259 0.9050 0.039 Uiso 1 1 calc R . . C11 C 0.7993(4) 0.9604(4) 0.7980(4) 0.0341(11) Uani 1 1 d . . . H11A H 0.7673 0.9201 0.8239 0.041 Uiso 1 1 calc R . . H11B H 0.8000 1.0201 0.8252 0.041 Uiso 1 1 calc R . . C12 C 0.7765(4) 1.0406(3) 0.6447(4) 0.0295(10) Uani 1 1 d . . . H12A H 0.8421 1.0516 0.6839 0.035 Uiso 1 1 calc R . . H12B H 0.7434 1.0943 0.6482 0.035 Uiso 1 1 calc R . . C13 C 0.6476(4) 0.9639(4) 0.6548(4) 0.0358(11) Uani 1 1 d . . . H13A H 0.6175 0.9914 0.5890 0.043 Uiso 1 1 calc R . . H13B H 0.6339 1.0007 0.7007 0.043 Uiso 1 1 calc R . . C14 C 0.6078(4) 0.8706(4) 0.6502(4) 0.0368(12) Uani 1 1 d . . . C15 C 0.7570(3) 1.0233(3) 0.5363(3) 0.0243(9) Uani 1 1 d . . . N1 N 1.0107(3) 0.2555(3) 0.9056(3) 0.0263(8) Uani 1 1 d . . . N2 N 0.7483(3) 0.9639(3) 0.6873(3) 0.0290(8) Uani 1 1 d . . . N3 N 0.9040(3) 0.8366(3) 0.7926(3) 0.0262(8) Uani 1 1 d . . . O1 O 0.9171(2) 0.4117(2) 0.8238(2) 0.0270(7) Uani 1 1 d . . . O2 O 0.8222(3) 0.3472(3) 0.6844(3) 0.0339(8) Uani 1 1 d . . . O3 O 1.1510(2) 0.3734(4) 1.0220(3) 0.0431(11) Uani 1 1 d . . . O4 O 1.2481(3) 0.3100(4) 0.9707(4) 0.0563(13) Uani 1 1 d . . . O5 O 0.9219(3) 0.8829(4) 0.6225(3) 0.0427(10) Uani 1 1 d . . . O6 O 1.0730(3) 0.8611(5) 0.6962(4) 0.077(2) Uani 1 1 d . . . O7 O 0.7714(3) 1.0856(2) 0.4876(3) 0.0306(7) Uani 1 1 d . . . O8 O 0.7288(2) 0.9467(2) 0.4975(3) 0.0280(7) Uani 1 1 d . . . O9 O 0.5286(3) 0.8662(3) 0.6474(4) 0.0511(11) Uani 1 1 d . . . O10 O 0.6541(3) 0.8015(3) 0.6475(4) 0.0409(9) Uani 1 1 d . . . O11 O 0.8297(2) 0.6814(2) 0.6930(3) 0.0269(7) Uani 1 1 d . . . O12 O 0.8657(3) 0.6035(2) 0.8313(3) 0.0317(8) Uani 1 1 d . . . O1W O 1.0000 0.5343(4) 1.0000 0.077(3) Uani 1 2 d SD . . H1W H 1.029(7) 0.5675(13) 0.977(8) 0.116 Uiso 1 1 d D . . O2W O 0.9331(2) 0.5201(3) 0.6699(3) 0.0331(8) Uani 1 1 d . . . H2WA H 0.9522 0.4675 0.6655 0.050 Uiso 1 1 d R . . H2WB H 0.9264 0.5510 0.6188 0.050 Uiso 1 1 d R . . O3W O 0.7333(2) 0.4500(3) 0.7998(3) 0.0356(8) Uani 1 1 d . . . H3WA H 0.7811 0.4379 0.8557 0.053 Uiso 1 1 d R . . H3WB H 0.6994 0.4897 0.8113 0.053 Uiso 1 1 d R . . O4W O 0.6331(2) 0.4372(3) 0.5762(3) 0.0379(9) Uani 1 1 d . . . H4WA H 0.6170 0.4030 0.6135 0.057 Uiso 1 1 d R . . H4WB H 0.5907 0.4783 0.5487 0.057 Uiso 1 1 d R . . O5W O 0.6620(3) 0.6133(3) 0.6778(4) 0.0439(10) Uani 1 1 d . . . H5WA H 0.6127 0.5838 0.6659 0.066 Uiso 1 1 d R . . H5WB H 0.6814 0.6385 0.7351 0.066 Uiso 1 1 d R . . O6W O 0.7670(3) 0.7537(3) 0.4867(3) 0.0366(9) Uani 1 1 d . . . H6WA H 0.7395 0.7030 0.4836 0.055 Uiso 1 1 d R . . H6WB H 0.7343 0.7849 0.4340 0.055 Uiso 1 1 d R . . O7W O 0.4513(8) 0.7008(11) 0.5810(11) 0.186(7) Uani 1 1 d . . . O8W O 0.4934(12) 0.5813(14) 0.6662(17) 0.285(12) Uani 1 1 d . . . O9W O 0.6458(4) 0.4756(5) 0.9624(5) 0.0779(18) Uani 1 1 d . . . O10W O 0.7278(5) 0.1142(5) 1.0345(5) 0.086(2) Uani 1 1 d . . . O11W O 1.1985(8) 0.6995(7) 0.7809(15) 0.221(8) Uani 1 1 d . . . O12W O 1.0857(7) 0.5846(9) 0.8357(6) 0.140(4) Uani 1 1 d . . . O13W O 0.9426(5) 0.6573(6) 0.5467(6) 0.103(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 Sm 0.02092(9) 0.02296(11) 0.02035(11) 0.00066(9) 0.00838(7) -0.00025(9) Cd1 0.02458(14) 0.02141(15) 0.02066(15) -0.00049(12) 0.00944(11) -0.00028(11) Cd2 0.0252(2) 0.0209(2) 0.0199(2) 0.000 0.00682(16) 0.000 C1 0.044(3) 0.017(2) 0.032(3) -0.0010(19) 0.006(2) 0.006(2) C2 0.036(2) 0.020(2) 0.020(2) -0.0045(18) 0.0047(18) 0.0018(18) C3 0.029(2) 0.025(2) 0.019(2) 0.0000(18) 0.0080(16) 0.0027(17) C4 0.035(2) 0.039(3) 0.026(3) -0.003(2) 0.012(2) 0.004(2) C5 0.031(2) 0.050(3) 0.028(2) 0.004(3) 0.0134(19) 0.008(2) C6 0.027(2) 0.064(4) 0.032(3) -0.002(3) 0.011(2) -0.016(2) C7 0.024(2) 0.049(3) 0.024(2) 0.002(2) 0.0057(17) -0.005(2) C8 0.0230(18) 0.024(2) 0.026(2) -0.0007(18) 0.0099(17) -0.0008(16) C9 0.035(2) 0.028(2) 0.019(2) -0.0014(19) 0.0080(18) -0.0036(18) C10 0.042(3) 0.025(2) 0.025(2) -0.003(2) 0.009(2) -0.005(2) C11 0.055(3) 0.027(2) 0.026(2) -0.004(2) 0.023(2) 0.001(2) C12 0.047(3) 0.020(2) 0.022(2) -0.0019(18) 0.015(2) 0.0018(18) C13 0.042(3) 0.034(3) 0.038(3) 0.001(2) 0.024(2) 0.010(2) C14 0.033(2) 0.042(3) 0.041(3) 0.008(2) 0.021(2) 0.008(2) C15 0.0279(19) 0.022(2) 0.022(2) -0.0009(18) 0.0101(16) 0.0010(17) N1 0.0285(18) 0.0242(19) 0.0193(19) -0.0009(16) 0.0039(15) 0.0021(15) N2 0.036(2) 0.026(2) 0.026(2) 0.0016(17) 0.0152(17) 0.0047(17) N3 0.0307(18) 0.0250(19) 0.0235(19) -0.0002(16) 0.0125(15) -0.0027(15) O1 0.0304(17) 0.0234(16) 0.0236(17) -0.0045(14) 0.0085(13) -0.0002(13) O2 0.041(2) 0.0277(18) 0.0215(17) -0.0027(15) 0.0029(14) 0.0042(15) O3 0.0254(17) 0.069(3) 0.033(2) -0.017(2) 0.0116(15) -0.0056(18) O4 0.036(2) 0.074(3) 0.065(3) -0.019(3) 0.028(2) 0.000(2) O5 0.0324(18) 0.063(3) 0.034(2) 0.010(2) 0.0164(16) -0.0106(19) O6 0.037(2) 0.142(6) 0.049(3) 0.014(3) 0.017(2) -0.022(3) O7 0.0439(19) 0.0238(17) 0.0241(17) 0.0024(14) 0.0149(15) 0.0014(14) O8 0.0374(18) 0.0243(17) 0.0238(17) -0.0038(14) 0.0147(14) -0.0007(13) O9 0.035(2) 0.055(3) 0.074(3) 0.010(2) 0.034(2) 0.0092(19) O10 0.0339(19) 0.0302(19) 0.066(3) 0.0011(19) 0.0284(19) 0.0003(15) O11 0.0315(16) 0.0277(17) 0.0209(17) 0.0006(14) 0.0110(14) 0.0016(13) O12 0.0355(18) 0.0257(18) 0.0268(18) 0.0053(14) 0.0070(14) 0.0023(14) O1W 0.095(6) 0.024(3) 0.047(4) 0.000 -0.030(4) 0.000 O2W 0.0285(15) 0.033(2) 0.0403(19) 0.0054(18) 0.0170(14) 0.0033(15) O3W 0.0296(16) 0.051(2) 0.0261(17) 0.0080(17) 0.0122(14) -0.0004(16) O4W 0.0310(17) 0.050(2) 0.031(2) -0.0008(17) 0.0127(15) -0.0150(16) O5W 0.0344(19) 0.035(2) 0.068(3) 0.000(2) 0.028(2) 0.0025(16) O6W 0.055(2) 0.0232(17) 0.028(2) 0.0011(15) 0.0146(16) 0.0006(17) O7W 0.146(9) 0.236(15) 0.212(12) -0.146(12) 0.111(9) -0.127(10) O8W 0.209(15) 0.30(2) 0.47(3) -0.17(2) 0.25(2) -0.144(15) O9W 0.062(3) 0.097(5) 0.070(3) 0.003(3) 0.026(3) 0.016(3) O10W 0.106(5) 0.089(5) 0.082(4) -0.020(4) 0.057(4) -0.024(4) O11W 0.143(9) 0.076(6) 0.50(3) -0.027(10) 0.190(14) -0.025(6) O12W 0.109(6) 0.226(11) 0.076(5) -0.019(6) 0.031(5) -0.048(7) O13W 0.103(5) 0.101(5) 0.145(7) 0.047(5) 0.093(5) 0.035(4) _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 Sm O3W 2.447(4) . ? Sm O4W 2.448(4) . ? Sm O2 2.463(4) . ? Sm O2W 2.467(3) . ? Sm O7 2.481(4) 4_646 ? Sm O5W 2.490(4) . ? Sm O12 2.519(4) . ? Sm O11 2.648(4) . ? Sm O8 2.673(4) 4_646 ? Sm O1 2.714(3) . ? Sm C15 2.949(5) 4_646 ? Sm C8 2.955(5) . ? Cd1 O6W 2.235(4) . ? Cd1 O10 2.307(4) . ? Cd1 O5 2.351(4) . ? Cd1 N2 2.371(4) . ? Cd1 N3 2.408(4) . ? Cd1 O11 2.409(4) . ? Cd1 O8 2.411(4) . ? Cd2 O1W 2.231(6) . ? Cd2 O3 2.306(4) 2_757 ? Cd2 O3 2.306(4) . ? Cd2 O1 2.397(3) 2_757 ? Cd2 O1 2.397(3) . ? Cd2 N1 2.409(4) . ? Cd2 N1 2.409(4) 2_757 ? C1 N1 1.473(7) . ? C1 C1 1.508(12) 2_757 ? C2 N1 1.473(6) . ? C2 C3 1.516(7) . ? C3 O2 1.256(6) . ? C3 O1 1.256(6) . ? C4 N1 1.473(7) . ? C4 C5 1.524(8) . ? C5 O4 1.249(6) . ? C5 O3 1.262(7) . ? C6 O5 1.244(7) . ? C6 O6 1.247(7) . ? C6 C7 1.495(8) . ? C7 N3 1.469(6) . ? C8 O12 1.254(6) . ? C8 O11 1.276(6) . ? C8 C9 1.521(7) . ? C9 N3 1.467(6) . ? C10 N3 1.493(6) . ? C10 C11 1.520(8) . ? C11 N2 1.484(7) . ? C12 N2 1.465(7) . ? C12 C15 1.520(7) . ? C13 N2 1.471(7) . ? C13 C14 1.512(8) . ? C14 O9 1.256(6) . ? C14 O10 1.276(7) . ? C15 O7 1.253(6) . ? C15 O8 1.264(6) . ? C15 Sm 2.949(5) 4_656 ? O7 Sm 2.481(4) 4_656 ? O8 Sm 2.673(4) 4_656 ? 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 O3W Sm O4W 75.47(13) . . ? O3W Sm O2 77.42(14) . . ? O4W Sm O2 76.92(14) . . ? O3W Sm O2W 134.28(12) . . ? O4W Sm O2W 136.35(13) . . ? O2 Sm O2W 80.36(14) . . ? O3W Sm O7 143.92(13) . 4_646 ? O4W Sm O7 76.67(13) . 4_646 ? O2 Sm O7 117.64(12) . 4_646 ? O2W Sm O7 81.77(13) . 4_646 ? O3W Sm O5W 73.04(14) . . ? O4W Sm O5W 73.25(15) . . ? O2 Sm O5W 142.18(14) . . ? O2W Sm O5W 137.46(13) . . ? O7 Sm O5W 77.31(14) 4_646 . ? O3W Sm O12 74.49(13) . . ? O4W Sm O12 141.62(13) . . ? O2 Sm O12 118.45(11) . . ? O2W Sm O12 82.04(13) . . ? O7 Sm O12 117.30(12) 4_646 . ? O5W Sm O12 75.53(14) . . ? O3W Sm O11 116.54(13) . . ? O4W Sm O11 129.58(13) . . ? O2 Sm O11 151.20(11) . . ? O2W Sm O11 72.07(12) . . ? O7 Sm O11 67.01(11) 4_646 . ? O5W Sm O11 65.74(12) . . ? O12 Sm O11 50.35(11) . . ? O3W Sm O8 133.85(13) . 4_646 ? O4W Sm O8 68.13(12) . 4_646 ? O2 Sm O8 67.65(11) . 4_646 ? O2W Sm O8 68.86(12) . 4_646 ? O7 Sm O8 50.17(11) 4_646 4_646 ? O5W Sm O8 119.65(14) . 4_646 ? O12 Sm O8 149.15(12) . 4_646 ? O11 Sm O8 108.42(11) . 4_646 ? O3W Sm O1 67.35(12) . . ? O4W Sm O1 119.11(13) . . ? O2 Sm O1 49.60(11) . . ? O2W Sm O1 67.76(12) . . ? O7 Sm O1 148.04(12) 4_646 . ? O5W Sm O1 132.22(14) . . ? O12 Sm O1 69.12(11) . . ? O11 Sm O1 110.05(10) . . ? O8 Sm O1 107.00(10) 4_646 . ? O3W Sm C15 146.92(12) . 4_646 ? O4W Sm C15 71.51(13) . 4_646 ? O2 Sm C15 93.00(13) . 4_646 ? O2W Sm C15 73.04(12) . 4_646 ? O7 Sm C15 24.82(12) 4_646 4_646 ? O5W Sm C15 98.98(15) . 4_646 ? O12 Sm C15 135.79(12) . 4_646 ? O11 Sm C15 86.90(12) . 4_646 ? O8 Sm C15 25.38(11) 4_646 4_646 ? O1 Sm C15 128.77(11) . 4_646 ? O3W Sm C8 94.40(14) . . ? O4W Sm C8 140.04(14) . . ? O2 Sm C8 139.40(12) . . ? O2W Sm C8 77.60(13) . . ? O7 Sm C8 92.41(13) 4_646 . ? O5W Sm C8 66.85(13) . . ? O12 Sm C8 24.89(12) . . ? O11 Sm C8 25.59(12) . . ? O8 Sm C8 131.75(12) 4_646 . ? O1 Sm C8 90.33(12) . . ? C15 Sm C8 112.23(13) 4_646 . ? O6W Cd1 O10 106.60(16) . . ? O6W Cd1 O5 84.57(16) . . ? O10 Cd1 O5 168.52(16) . . ? O6W Cd1 N2 146.20(14) . . ? O10 Cd1 N2 72.42(15) . . ? O5 Cd1 N2 96.86(17) . . ? O6W Cd1 N3 133.83(14) . . ? O10 Cd1 N3 102.23(15) . . ? O5 Cd1 N3 70.61(14) . . ? N2 Cd1 N3 76.95(14) . . ? O6W Cd1 O11 79.56(13) . . ? O10 Cd1 O11 83.72(13) . . ? O5 Cd1 O11 101.30(15) . . ? N2 Cd1 O11 132.40(14) . . ? N3 Cd1 O11 68.55(13) . . ? O6W Cd1 O8 78.48(13) . . ? O10 Cd1 O8 101.51(14) . . ? O5 Cd1 O8 77.73(14) . . ? N2 Cd1 O8 68.97(13) . . ? N3 Cd1 O8 129.61(13) . . ? O11 Cd1 O8 158.02(12) . . ? O1W Cd2 O3 93.77(13) . 2_757 ? O1W Cd2 O3 93.77(13) . . ? O3 Cd2 O3 172.5(3) 2_757 . ? O1W Cd2 O1 79.99(8) . 2_757 ? O3 Cd2 O1 102.43(13) 2_757 2_757 ? O3 Cd2 O1 78.91(13) . 2_757 ? O1W Cd2 O1 79.99(8) . . ? O3 Cd2 O1 78.91(13) 2_757 . ? O3 Cd2 O1 102.43(13) . . ? O1 Cd2 O1 159.99(16) 2_757 . ? O1W Cd2 N1 141.97(10) . . ? O3 Cd2 N1 101.74(16) 2_757 . ? O3 Cd2 N1 72.11(15) . . ? O1 Cd2 N1 128.65(12) 2_757 . ? O1 Cd2 N1 69.47(12) . . ? O1W Cd2 N1 141.97(10) . 2_757 ? O3 Cd2 N1 72.11(15) 2_757 2_757 ? O3 Cd2 N1 101.74(16) . 2_757 ? O1 Cd2 N1 69.47(12) 2_757 2_757 ? O1 Cd2 N1 128.65(12) . 2_757 ? N1 Cd2 N1 76.1(2) . 2_757 ? N1 C1 C1 112.9(4) . 2_757 ? N1 C2 C3 111.7(4) . . ? O2 C3 O1 120.7(4) . . ? O2 C3 C2 118.5(4) . . ? O1 C3 C2 120.7(4) . . ? O2 C3 Sm 54.7(3) . . ? O1 C3 Sm 66.2(2) . . ? C2 C3 Sm 170.1(3) . . ? N1 C4 C5 113.1(4) . . ? O4 C5 O3 124.4(5) . . ? O4 C5 C4 117.1(5) . . ? O3 C5 C4 118.4(4) . . ? O5 C6 O6 124.9(6) . . ? O5 C6 C7 120.2(5) . . ? O6 C6 C7 114.9(5) . . ? N3 C7 C6 114.4(4) . . ? O12 C8 O11 120.9(4) . . ? O12 C8 C9 119.3(4) . . ? O11 C8 C9 119.8(4) . . ? O12 C8 Sm 57.7(2) . . ? O11 C8 Sm 63.7(2) . . ? C9 C8 Sm 170.8(3) . . ? N3 C9 C8 110.3(4) . . ? N3 C10 C11 113.0(4) . . ? N2 C11 C10 112.0(4) . . ? N2 C12 C15 111.5(4) . . ? N2 C13 C14 113.5(4) . . ? O9 C14 O10 123.7(6) . . ? O9 C14 C13 116.8(5) . . ? O10 C14 C13 119.5(4) . . ? O7 C15 O8 121.1(4) . . ? O7 C15 C12 118.8(4) . . ? O8 C15 C12 120.1(4) . . ? O7 C15 Sm 56.2(2) . 4_656 ? O8 C15 Sm 65.0(2) . 4_656 ? C12 C15 Sm 174.5(3) . 4_656 ? C2 N1 C4 110.9(4) . . ? C2 N1 C1 112.9(4) . . ? C4 N1 C1 110.9(4) . . ? C2 N1 Cd2 107.8(3) . . ? C4 N1 Cd2 107.0(3) . . ? C1 N1 Cd2 107.1(3) . . ? C12 N2 C13 111.2(4) . . ? C12 N2 C11 112.4(4) . . ? C13 N2 C11 111.1(4) . . ? C12 N2 Cd1 107.4(3) . . ? C13 N2 Cd1 107.0(3) . . ? C11 N2 Cd1 107.4(3) . . ? C9 N3 C7 111.4(4) . . ? C9 N3 C10 112.0(4) . . ? C7 N3 C10 111.5(4) . . ? C9 N3 Cd1 107.7(3) . . ? C7 N3 Cd1 107.1(3) . . ? C10 N3 Cd1 106.8(3) . . ? C3 O1 Cd2 114.4(3) . . ? C3 O1 Sm 88.8(3) . . ? Cd2 O1 Sm 146.89(15) . . ? C3 O2 Sm 100.7(3) . . ? C5 O3 Cd2 118.7(3) . . ? C6 O5 Cd1 115.8(4) . . ? C15 O7 Sm 99.0(3) . 4_656 ? C15 O8 Cd1 110.5(3) . . ? C15 O8 Sm 89.6(3) . 4_656 ? Cd1 O8 Sm 147.37(15) . 4_656 ? C14 O10 Cd1 115.9(3) . . ? C8 O11 Cd1 114.3(3) . . ? C8 O11 Sm 90.8(3) . . ? Cd1 O11 Sm 145.53(15) . . ? C8 O12 Sm 97.4(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.872 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.109 data_eu _database_code_depnum_ccdc_archive 'CCDC 918899' #TrackingRef '918899.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H74 Cd3 N6 O35 Eu2, 14(O)' _chemical_formula_sum 'C30 H86 Cd3 Eu2 N6 O49' _chemical_formula_weight 1956.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.9222(8) _cell_length_b 14.8017(4) _cell_length_c 14.7923(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.882(7) _cell_angle_gamma 90.00 _cell_volume 3136.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10360 _cell_measurement_theta_min 3.3181 _cell_measurement_theta_max 76.0845 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 23.159 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21632 _diffrn_reflns_av_R_equivalents 0.2331 _diffrn_reflns_av_sigmaI/netI 0.1157 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 76.27 _reflns_number_total 5614 _reflns_number_gt 4693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(6) _refine_ls_number_reflns 5614 _refine_ls_number_parameters 379 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.2604 _refine_ls_wR_factor_gt 0.2458 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad 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 Eu Eu 0.28125(5) 0.31605(5) 0.67648(7) 0.0437(3) Uani 1 1 d . . . Cd1 Cd 0.21667(6) 0.13633(7) 0.37599(9) 0.0463(3) Uani 1 1 d . . . Cd2 Cd 0.5000 0.19217(9) 1.0000 0.0459(4) Uani 1 2 d SD . . C1 C 0.2001(18) 0.2668(13) 0.192(2) 0.079(6) Uani 1 1 d . . . H1A H 0.1979 0.3258 0.1628 0.095 Uiso 1 1 calc R . . H1B H 0.2318 0.2253 0.1667 0.095 Uiso 1 1 calc R . . C2 C 0.1040(16) 0.2340(11) 0.1673(16) 0.060(4) Uani 1 1 d D . . H2A H 0.0750 0.2763 0.1951 0.072 Uiso 1 1 calc R . . H2B H 0.0682 0.2352 0.0948 0.072 Uiso 1 1 calc R . . C3 C 0.0078(10) 0.1319(15) 0.2074(14) 0.064(5) Uani 1 1 d . . . H3A H -0.0409 0.1613 0.1497 0.077 Uiso 1 1 calc R . . H3B H -0.0059 0.0678 0.2019 0.077 Uiso 1 1 calc R . . C4 C 0.0039(13) 0.1653(17) 0.297(2) 0.095(10) Uani 1 1 d . . . C5 C 0.1135(13) 0.0692(13) 0.1469(15) 0.059(4) Uani 1 1 d . . . H5A H 0.1618 0.0858 0.1268 0.071 Uiso 1 1 calc R . . H5B H 0.0568 0.0567 0.0867 0.071 Uiso 1 1 calc R . . C6 C 0.1433(10) -0.0153(11) 0.2126(13) 0.052(4) Uani 1 1 d . . . C7 C 0.3595(16) 0.2645(16) 0.3474(19) 0.072(5) Uani 1 1 d . . . H7A H 0.3768 0.2995 0.3027 0.087 Uiso 1 1 calc R . . H7B H 0.3897 0.2921 0.4134 0.087 Uiso 1 1 calc R . . C8 C 0.3956(12) 0.1769(14) 0.3539(17) 0.059(4) Uani 1 1 d . . . C9 C 0.2225(14) 0.3475(9) 0.3546(11) 0.050(4) Uani 1 1 d . . . H9A H 0.1559 0.3563 0.3159 0.060 Uiso 1 1 calc R . . H9B H 0.2535 0.4024 0.3496 0.060 Uiso 1 1 calc R . . C10 C 0.2436(10) 0.3320(9) 0.4646(13) 0.047(3) Uani 1 1 d . . . C11 C 0.4717(11) -0.0153(10) 1.0299(12) 0.045(3) Uani 1 1 d . . . H11A H 0.4059 -0.0167 0.9835 0.054 Uiso 1 1 calc R . . H11B H 0.4856 -0.0701 1.0699 0.054 Uiso 1 1 calc R . . C12 C 0.4085(12) 0.0843(13) 1.1162(12) 0.054(4) Uani 1 1 d . . . H12A H 0.4313 0.1227 1.1752 0.065 Uiso 1 1 calc R . . H12B H 0.3832 0.0300 1.1317 0.065 Uiso 1 1 calc R . . C13 C 0.5761(10) 0.0598(9) 1.1838(14) 0.050(4) Uani 1 1 d . . . H13A H 0.6231 0.0326 1.1674 0.060 Uiso 1 1 calc R . . H13B H 0.5692 0.0211 1.2331 0.060 Uiso 1 1 calc R . . C14 C 0.3294(14) 0.1342(14) 1.0282(17) 0.067(5) Uani 1 1 d . . . C15 C 0.3870(11) 0.1501(11) 0.7670(14) 0.052(4) Uani 1 1 d . . . N1 N 0.0969(9) 0.1452(9) 0.2021(8) 0.046(3) Uani 1 1 d D . . N2 N 0.2527(11) 0.2723(9) 0.3102(13) 0.057(4) Uani 1 1 d . . . N3 N 0.4882(9) 0.0591(10) 1.0936(12) 0.057(4) Uani 1 1 d . . . O1 O 0.0770(11) 0.1904(12) 0.3737(11) 0.067(3) Uani 1 1 d . . . O2 O -0.0777(12) 0.159(2) 0.3070(16) 0.120(10) Uani 1 1 d . . . O3 O 0.1705(7) -0.0102(8) 0.3066(9) 0.051(3) Uani 1 1 d . . . O4 O 0.1358(9) -0.0920(8) 0.1669(9) 0.058(3) Uani 1 1 d . . . O5 O 0.3477(10) 0.1079(9) 0.3569(15) 0.085(6) Uani 1 1 d . . . O6 O 0.4772(11) 0.1693(10) 0.3576(17) 0.084(5) Uani 1 1 d . . . O7 O 0.2707(9) 0.2541(8) 0.5026(9) 0.057(3) Uani 1 1 d . . . O8 O 0.2275(9) 0.3922(8) 0.5093(8) 0.053(3) Uani 1 1 d . . . O9 O 0.3476(10) 0.1825(12) 0.9740(12) 0.072(4) Uani 1 1 d . . . O10 O 0.2479(10) 0.1216(13) 1.0281(16) 0.087(5) Uani 1 1 d . . . O11 O 0.4158(8) 0.2208(7) 0.8195(8) 0.047(3) Uani 1 1 d . . . O12 O 0.3214(9) 0.1533(7) 0.6812(10) 0.063(4) Uani 1 1 d . . . O1W O 0.2358(11) 0.0596(8) 0.5182(12) 0.068(4) Uani 1 1 d . . . H1WA H 0.2575 0.0044 0.5187 0.102 Uiso 1 1 d R . . H1WB H 0.2759 0.0875 0.5731 0.102 Uiso 1 1 d R . . O2W O 0.4344(8) 0.3257(11) 0.6721(12) 0.070(4) Uani 1 1 d . . . H2WA H 0.4552 0.2713 0.6594 0.104 Uiso 1 1 d R . . H2WB H 0.4326 0.3648 0.6231 0.104 Uiso 1 1 d R . . O3W O 0.2330(10) 0.2577(10) 0.8018(11) 0.066(3) Uani 1 1 d . . . H3WA H 0.2837 0.2408 0.8662 0.099 Uiso 1 1 d R . . H3WB H 0.1961 0.2998 0.8198 0.099 Uiso 1 1 d R . . O4W O 0.1572(10) 0.4198(10) 0.6710(14) 0.071(4) Uani 1 1 d . . . H4WA H 0.1115 0.3905 0.6815 0.106 Uiso 1 1 d R . . H4WB H 0.1800 0.4638 0.7189 0.106 Uiso 1 1 d R . . O5W O 0.1319(10) 0.2436(11) 0.5798(15) 0.079(4) Uani 1 1 d . . . H5WA H 0.1275 0.2014 0.5226 0.118 Uiso 1 1 d R . . H5WB H 0.1034 0.2016 0.6159 0.118 Uiso 1 1 d R . . O6W O 0.5000 0.3436(11) 1.0000 0.108(12) Uani 1 2 d SD . . H6W H 0.50(3) 0.3767(17) 0.951(11) 0.162 Uiso 1 1 d D . . O7W O 0.585(3) 0.415(3) 0.836(3) 0.211(19) Uiso 1 1 d . . . O8W O 0.5000 0.083(15) 0.5000 0.57(12) Uiso 1 2 d S . . O9W O 0.530(3) -0.033(3) 0.388(3) 0.165(12) Uiso 1 1 d . . . O10W O 0.236(4) -0.084(4) 1.037(4) 0.24(2) Uiso 1 1 d . . . O11W O 0.1500(18) 0.2925(16) 0.9567(18) 0.109(7) Uiso 1 1 d . . . O12W O -0.201(3) 0.001(3) 0.205(3) 0.174(14) Uiso 1 1 d . . . O13W O 0.4490(16) 0.4728(17) 0.5472(18) 0.107(6) Uiso 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 Eu 0.0282(4) 0.0381(4) 0.0578(5) 0.0006(4) 0.0124(3) -0.0002(3) Cd1 0.0334(5) 0.0371(5) 0.0594(6) 0.0006(4) 0.0120(4) -0.0001(4) Cd2 0.0361(7) 0.0360(6) 0.0552(8) 0.000 0.0101(6) 0.000 C1 0.083(14) 0.036(8) 0.113(18) -0.003(10) 0.037(13) -0.010(9) C2 0.078(12) 0.048(9) 0.068(11) 0.002(8) 0.045(10) 0.012(9) C3 0.028(6) 0.077(11) 0.064(10) -0.034(9) -0.002(6) 0.004(7) C4 0.027(7) 0.083(15) 0.13(2) -0.026(14) -0.010(10) 0.010(8) C5 0.051(9) 0.058(10) 0.068(10) -0.002(9) 0.025(8) 0.007(8) C6 0.032(6) 0.049(8) 0.054(8) 0.022(7) 0.000(6) 0.000(6) C7 0.061(11) 0.076(13) 0.079(13) -0.014(11) 0.030(10) -0.015(10) C8 0.038(7) 0.064(10) 0.084(12) -0.013(9) 0.035(8) 0.004(7) C9 0.086(12) 0.029(6) 0.037(6) 0.022(5) 0.029(7) 0.013(6) C10 0.034(6) 0.032(6) 0.064(9) -0.012(6) 0.011(6) -0.005(5) C11 0.047(7) 0.039(6) 0.048(7) 0.008(6) 0.021(7) -0.011(6) C12 0.053(9) 0.061(9) 0.043(7) 0.007(7) 0.016(6) -0.006(7) C13 0.037(7) 0.028(6) 0.071(10) -0.001(6) 0.009(7) 0.004(5) C14 0.057(10) 0.053(9) 0.075(12) -0.004(10) 0.013(9) 0.003(9) C15 0.035(7) 0.045(8) 0.070(10) -0.001(7) 0.015(7) 0.003(6) N1 0.042(6) 0.061(7) 0.034(5) -0.010(6) 0.017(4) 0.009(6) N2 0.065(9) 0.030(6) 0.070(9) 0.005(6) 0.026(7) -0.010(6) N3 0.034(6) 0.051(7) 0.076(9) 0.020(7) 0.015(6) -0.005(5) O1 0.067(8) 0.066(8) 0.064(8) 0.001(7) 0.025(6) 0.006(7) O2 0.044(8) 0.20(3) 0.099(12) -0.036(15) 0.015(8) 0.031(11) O3 0.038(5) 0.045(6) 0.063(7) 0.003(5) 0.015(5) 0.002(4) O4 0.055(7) 0.039(5) 0.057(6) 0.002(5) 0.004(5) 0.017(5) O5 0.046(7) 0.040(6) 0.134(14) 0.016(7) 0.006(8) -0.004(5) O6 0.057(8) 0.058(8) 0.138(15) -0.001(9) 0.043(9) -0.010(6) O7 0.064(7) 0.040(5) 0.050(6) 0.009(5) 0.009(5) 0.006(5) O8 0.059(7) 0.056(6) 0.040(5) 0.006(5) 0.020(5) -0.013(5) O9 0.052(7) 0.089(10) 0.079(9) 0.040(9) 0.032(7) 0.022(7) O10 0.050(7) 0.081(10) 0.131(15) 0.013(10) 0.040(8) -0.008(7) O11 0.046(6) 0.046(5) 0.046(5) 0.026(5) 0.016(5) 0.014(4) O12 0.056(7) 0.028(5) 0.071(8) -0.008(5) -0.004(6) -0.003(4) O1W 0.083(9) 0.040(6) 0.079(9) -0.027(6) 0.034(7) -0.003(6) O2W 0.041(6) 0.060(7) 0.086(9) 0.007(7) 0.008(6) 0.012(6) O3W 0.056(7) 0.069(8) 0.062(7) 0.001(6) 0.017(6) 0.021(6) O4W 0.051(7) 0.058(7) 0.116(12) -0.010(7) 0.048(8) 0.012(5) O5W 0.050(7) 0.066(9) 0.113(12) -0.009(8) 0.029(8) 0.003(6) O6W 0.16(3) 0.025(7) 0.066(12) 0.000 -0.023(14) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu O5W 2.425(15) . ? Eu O3W 2.452(17) . ? Eu O2W 2.472(15) . ? Eu O4W 2.475(12) . ? Eu O12 2.486(11) . ? Eu O8 2.504(11) . ? Eu O4 2.509(12) 4_556 ? Eu O11 2.663(9) . ? Eu O3 2.665(11) 4_556 ? Eu O7 2.667(14) . ? Eu C10 2.933(18) . ? Eu C6 2.940(14) 4_556 ? Cd1 O5 2.263(19) . ? Cd1 O1W 2.291(16) . ? Cd1 O1 2.350(16) . ? Cd1 O3 2.374(12) . ? Cd1 N2 2.411(13) . ? Cd1 O7 2.424(12) . ? Cd1 N1 2.447(11) . ? Cd2 O6W 2.241(16) . ? Cd2 O9 2.289(14) 2_657 ? Cd2 O9 2.289(14) . ? Cd2 O11 2.446(10) 2_657 ? Cd2 O11 2.446(10) . ? Cd2 N3 2.462(14) 2_657 ? Cd2 N3 2.462(14) . ? C1 C2 1.49(3) . ? C1 N2 1.57(3) . ? C2 N1 1.435(16) . ? C3 C4 1.44(4) . ? C3 N1 1.47(2) . ? C4 O1 1.28(3) . ? C4 O2 1.38(3) . ? C5 N1 1.48(2) . ? C5 C6 1.53(2) . ? C6 O3 1.27(2) . ? C6 O4 1.30(2) . ? C6 Eu 2.940(14) 4_546 ? C7 C8 1.40(3) . ? C7 N2 1.55(3) . ? C8 O6 1.28(2) . ? C8 O5 1.29(2) . ? C9 N2 1.48(2) . ? C9 C10 1.53(2) . ? C10 O8 1.20(2) . ? C10 O7 1.273(19) . ? C11 N3 1.40(2) . ? C11 C11 1.51(3) 2_657 ? C12 N3 1.49(3) . ? C12 C14 1.55(2) . ? C13 N3 1.452(19) . ? C13 C15 1.51(2) 2_657 ? C14 O9 1.20(3) . ? C14 O10 1.31(3) . ? C15 O12 1.24(2) . ? C15 O11 1.26(2) . ? C15 C13 1.51(2) 2_657 ? O3 Eu 2.665(11) 4_546 ? O4 Eu 2.509(12) 4_546 ? 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 O5W Eu O3W 74.9(6) . . ? O5W Eu O2W 137.3(6) . . ? O3W Eu O2W 132.7(5) . . ? O5W Eu O4W 72.1(5) . . ? O3W Eu O4W 74.6(5) . . ? O2W Eu O4W 138.2(5) . . ? O5W Eu O12 76.2(5) . . ? O3W Eu O12 78.4(5) . . ? O2W Eu O12 79.2(5) . . ? O4W Eu O12 142.5(5) . . ? O5W Eu O8 78.0(5) . . ? O3W Eu O8 145.1(4) . . ? O2W Eu O8 82.2(5) . . ? O4W Eu O8 76.4(5) . . ? O12 Eu O8 115.9(5) . . ? O5W Eu O4 140.4(6) . 4_556 ? O3W Eu O4 72.9(5) . 4_556 ? O2W Eu O4 82.2(5) . 4_556 ? O4W Eu O4 77.5(5) . 4_556 ? O12 Eu O4 118.3(4) . 4_556 ? O8 Eu O4 118.9(4) . 4_556 ? O5W Eu O11 118.4(5) . . ? O3W Eu O11 67.8(4) . . ? O2W Eu O11 65.8(4) . . ? O4W Eu O11 135.1(5) . . ? O12 Eu O11 50.0(4) . . ? O8 Eu O11 146.3(4) . . ? O4 Eu O11 68.7(4) 4_556 . ? O5W Eu O3 130.6(4) . 4_556 ? O3W Eu O3 116.2(4) . 4_556 ? O2W Eu O3 72.5(4) . 4_556 ? O4W Eu O3 66.3(4) . 4_556 ? O12 Eu O3 150.8(4) . 4_556 ? O8 Eu O3 67.6(4) . 4_556 ? O4 Eu O3 51.3(4) 4_556 4_556 ? O11 Eu O3 109.7(4) . 4_556 ? O5W Eu O7 69.3(6) . . ? O3W Eu O7 134.4(5) . . ? O2W Eu O7 69.0(5) . . ? O4W Eu O7 117.9(5) . . ? O12 Eu O7 66.5(4) . . ? O8 Eu O7 49.6(4) . . ? O4 Eu O7 149.7(5) 4_556 . ? O11 Eu O7 105.9(4) . . ? O3 Eu O7 108.5(4) 4_556 . ? O5W Eu C10 73.5(6) . . ? O3W Eu C10 148.3(4) . . ? O2W Eu C10 73.2(5) . . ? O4W Eu C10 97.3(5) . . ? O12 Eu C10 92.2(5) . . ? O8 Eu C10 23.9(4) . . ? O4 Eu C10 136.3(4) 4_556 . ? O11 Eu C10 127.6(4) . . ? O3 Eu C10 86.5(4) 4_556 . ? O7 Eu C10 25.7(4) . . ? O5W Eu C6 139.6(5) . 4_556 ? O3W Eu C6 93.7(6) . 4_556 ? O2W Eu C6 78.3(5) . 4_556 ? O4W Eu C6 67.5(5) . 4_556 ? O12 Eu C6 140.3(4) . 4_556 ? O8 Eu C6 92.8(5) . 4_556 ? O4 Eu C6 26.1(5) 4_556 4_556 ? O11 Eu C6 90.8(4) . 4_556 ? O3 Eu C6 25.5(5) 4_556 4_556 ? O7 Eu C6 132.0(5) . 4_556 ? C10 Eu C6 111.8(5) . 4_556 ? O5 Cd1 O1W 105.2(6) . . ? O5 Cd1 O1 168.4(6) . . ? O1W Cd1 O1 85.9(5) . . ? O5 Cd1 O3 84.5(5) . . ? O1W Cd1 O3 80.6(4) . . ? O1 Cd1 O3 101.1(5) . . ? O5 Cd1 N2 73.1(5) . . ? O1W Cd1 N2 145.6(5) . . ? O1 Cd1 N2 95.8(6) . . ? O3 Cd1 N2 132.1(5) . . ? O5 Cd1 O7 101.2(5) . . ? O1W Cd1 O7 77.7(4) . . ? O1 Cd1 O7 77.3(5) . . ? O3 Cd1 O7 158.3(4) . . ? N2 Cd1 O7 69.2(5) . . ? O5 Cd1 N1 102.5(6) . . ? O1W Cd1 N1 136.2(5) . . ? O1 Cd1 N1 70.6(5) . . ? O3 Cd1 N1 69.0(4) . . ? N2 Cd1 N1 75.2(5) . . ? O7 Cd1 N1 128.6(4) . . ? O6W Cd2 O9 93.6(5) . 2_657 ? O6W Cd2 O9 93.6(5) . . ? O9 Cd2 O9 172.9(9) 2_657 . ? O6W Cd2 O11 80.0(3) . 2_657 ? O9 Cd2 O11 78.0(5) 2_657 2_657 ? O9 Cd2 O11 103.3(5) . 2_657 ? O6W Cd2 O11 80.0(3) . . ? O9 Cd2 O11 103.3(5) 2_657 . ? O9 Cd2 O11 78.0(5) . . ? O11 Cd2 O11 160.0(6) 2_657 . ? O6W Cd2 N3 143.1(4) . 2_657 ? O9 Cd2 N3 73.1(5) 2_657 2_657 ? O9 Cd2 N3 101.0(6) . 2_657 ? O11 Cd2 N3 127.8(5) 2_657 2_657 ? O11 Cd2 N3 70.4(5) . 2_657 ? O6W Cd2 N3 143.1(4) . . ? O9 Cd2 N3 101.0(6) 2_657 . ? O9 Cd2 N3 73.1(5) . . ? O11 Cd2 N3 70.4(5) 2_657 . ? O11 Cd2 N3 127.8(5) . . ? N3 Cd2 N3 73.7(9) 2_657 . ? C2 C1 N2 106(2) . . ? N1 C2 C1 116.3(17) . . ? C4 C3 N1 115.8(14) . . ? O1 C4 O2 117(3) . . ? O1 C4 C3 122(2) . . ? O2 C4 C3 120.2(18) . . ? N1 C5 C6 110.7(17) . . ? O3 C6 O4 122.3(13) . . ? O3 C6 C5 120.7(17) . . ? O4 C6 C5 116.9(16) . . ? O3 C6 Eu 65.0(8) . 4_546 ? O4 C6 Eu 58.1(7) . 4_546 ? C5 C6 Eu 171.3(15) . 4_546 ? C8 C7 N2 116.5(17) . . ? O6 C8 O5 122.3(18) . . ? O6 C8 C7 117.5(19) . . ? O5 C8 C7 120.2(16) . . ? N2 C9 C10 113.4(11) . . ? O8 C10 O7 122.7(17) . . ? O8 C10 C9 118.3(13) . . ? O7 C10 C9 118.7(14) . . ? O8 C10 Eu 57.6(9) . . ? O7 C10 Eu 65.4(10) . . ? C9 C10 Eu 175.9(9) . . ? N3 C11 C11 114.1(11) . 2_657 ? N3 C12 C14 112.9(16) . . ? N3 C13 C15 117.7(13) . 2_657 ? O9 C14 O10 127.6(19) . . ? O9 C14 C12 120.1(18) . . ? O10 C14 C12 112(2) . . ? O12 C15 O11 120.8(15) . . ? O12 C15 C13 120.1(15) . 2_657 ? O11 C15 C13 118.4(15) . 2_657 ? O12 C15 Eu 56.4(8) . . ? O11 C15 Eu 64.6(8) . . ? C13 C15 Eu 168.4(12) 2_657 . ? C2 N1 C3 111.7(15) . . ? C2 N1 C5 116.0(14) . . ? C3 N1 C5 109.7(14) . . ? C2 N1 Cd1 106.2(11) . . ? C3 N1 Cd1 105.3(10) . . ? C5 N1 Cd1 107.1(10) . . ? C9 N2 C7 114.8(15) . . ? C9 N2 C1 114.4(14) . . ? C7 N2 C1 111.2(18) . . ? C9 N2 Cd1 105.6(10) . . ? C7 N2 Cd1 102.3(12) . . ? C1 N2 Cd1 107.4(10) . . ? C11 N3 C13 116.6(14) . . ? C11 N3 C12 114.8(13) . . ? C13 N3 C12 111.4(16) . . ? C11 N3 Cd2 106.8(11) . . ? C13 N3 Cd2 103.4(10) . . ? C12 N3 Cd2 101.9(10) . . ? C4 O1 Cd1 113.7(16) . . ? C6 O3 Cd1 115.0(10) . . ? C6 O3 Eu 89.5(10) . 4_546 ? Cd1 O3 Eu 144.9(5) . 4_546 ? C6 O4 Eu 95.8(9) . 4_546 ? C8 O5 Cd1 116.7(12) . . ? C10 O7 Cd1 111.9(10) . . ? C10 O7 Eu 88.9(10) . . ? Cd1 O7 Eu 147.6(6) . . ? C10 O8 Eu 98.5(10) . . ? C14 O9 Cd2 118.1(12) . . ? C15 O11 Cd2 113.9(10) . . ? C15 O11 Eu 90.0(9) . . ? Cd2 O11 Eu 145.7(5) . . ? C15 O12 Eu 99.0(10) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 76.27 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 3.114 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.248