# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'R. Jones' _publ_contact_author_address ; Department of Chemistry University of Texas at Austin Austin Texas 778712-116 UNITED STATES OF AMERICA ; _publ_contact_author_email RAJONES@MAIL.UTEXAS.EDU _publ_section_title ; Reversible Guest Molecule Encapsulation in the 3-D Framework of a Heteropolynuclear Luminescent Zn4Eu2 Cage Complex ; loop_ _publ_author_name 'R. Jones' 'Benjamin P. Hahn' 'Keith J. Stevenson' 'J. Steven Swinnea' 'Qiaoyin Wu.' ; Xiaoping Yang ; # Attachment 'Complex-1(0702).CIF' data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 265078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H64 Br4 Eu2 N2 O34 Zn4' _chemical_formula_weight 2146.09 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' Br Br -0.2901 2.4595 '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' Zn Zn 0.2839 1.4301 '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 11.390(2) _cell_length_b 13.007(3) _cell_length_c 13.194(3) _cell_angle_alpha 102.47(3) _cell_angle_beta 104.01(3) _cell_angle_gamma 101.11(3) _cell_volume 1788.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 5.368 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.3356 _exptl_absorpt_correction_T_max 0.5219 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _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 12619 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8137 _reflns_number_gt 6104 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0397P)^2^+3.8114P] 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 SHELXL _refine_ls_extinction_coef 0.0031(4) _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 0.10(8) _refine_ls_number_reflns 8137 _refine_ls_number_parameters 447 _refine_ls_number_restraints 295 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.006 _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 0.510874(16) 0.233950(13) -0.009117(13) 0.01674(4) Uani 1 1 d U . . Zn2 Zn 0.78148(4) 0.13957(3) 0.05712(3) 0.01754(9) Uani 1 1 d U . . Zn1 Zn 0.60071(3) 0.05320(3) -0.20322(3) 0.01505(9) Uani 1 1 d U . . Br1 Br 1.18262(4) 0.67683(3) 0.20154(4) 0.03721(11) Uani 1 1 d U . . Br1' Br 0.41381(4) 0.34985(3) -0.59257(3) 0.03413(10) Uani 1 1 d U . . N1 N 0.4176(3) 0.3681(2) 0.1506(2) 0.0249(7) Uani 1 1 d U . . O1 O 0.9601(2) 0.27225(19) 0.1718(2) 0.0304(7) Uani 1 1 d U . . O2 O 0.7406(2) 0.28508(17) 0.06552(17) 0.0169(6) Uani 1 1 d U . . O3 O 0.6070(2) 0.41289(18) -0.03384(18) 0.0195(6) Uani 1 1 d U . . O1' O 0.5984(2) 0.10232(18) -0.36130(18) 0.0208(6) Uani 1 1 d U . . O2' O 0.5278(2) 0.18479(16) -0.19542(16) 0.0136(5) Uani 1 1 d U . . O3' O 0.3629(2) 0.30811(17) -0.12868(17) 0.0175(6) Uani 1 1 d U . . O4 O 0.8931(2) 0.1132(2) -0.0309(2) 0.0353(7) Uani 1 1 d U . . O5 O 0.7711(2) 0.0474(2) -0.20382(19) 0.0258(6) Uani 1 1 d U . . O6 O 0.8071(2) 0.08084(18) 0.18166(18) 0.0207(6) Uani 1 1 d U . . O7 O 0.5245(2) 0.14789(17) 0.14064(17) 0.0169(6) Uani 1 1 d U . . O8 O 0.5325(2) 0.38976(19) 0.15477(19) 0.0262(6) Uani 1 1 d U . . O9 O 0.3459(2) 0.2839(2) 0.07893(19) 0.0243(6) Uani 1 1 d U . . O10 O 0.6639(2) -0.07536(17) 0.09254(18) 0.0184(6) Uani 1 1 d U . . O11 O 0.60845(19) 0.08040(17) -0.04658(16) 0.0133(5) Uani 1 1 d DU . . H11A H 0.5715 0.0293 -0.0275 0.016 Uiso 1 1 d RD . . O12 O 0.3782(3) 0.4282(2) 0.2119(2) 0.0355(7) Uani 1 1 d U . . O13 O 0.5285(2) 0.08272(17) 0.28389(17) 0.0175(6) Uani 1 1 d U . . C1 C 1.0807(4) 0.2531(4) 0.2103(5) 0.0610(16) Uani 1 1 d U . . H1A H 1.1205 0.2967 0.2841 0.092 Uiso 1 1 calc R . . H1B H 1.1316 0.2725 0.1656 0.092 Uiso 1 1 calc R . . H1C H 1.0709 0.1774 0.2072 0.092 Uiso 1 1 calc R . . C2 C 0.9559(3) 0.3704(3) 0.1515(3) 0.0224(9) Uani 1 1 d U . . C3 C 1.0586(3) 0.4585(3) 0.1818(3) 0.0256(9) Uani 1 1 d U . . H3A H 1.1378 0.4537 0.2172 0.031 Uiso 1 1 calc R . . C4 C 1.0413(3) 0.5559(3) 0.1581(3) 0.0240(9) Uani 1 1 d U . . C5 C 0.9276(3) 0.5623(3) 0.1024(3) 0.0239(9) Uani 1 1 d U . . H5A H 0.9184 0.6266 0.0852 0.029 Uiso 1 1 calc R . . C6 C 0.8226(3) 0.4712(3) 0.0703(3) 0.0188(8) Uani 1 1 d U . . C7 C 0.8359(3) 0.3736(3) 0.0956(3) 0.0171(8) Uani 1 1 d U . . C8 C 0.7079(3) 0.4822(3) 0.0041(3) 0.0198(8) Uani 1 1 d U . . H8A H 0.7103 0.5487 -0.0118 0.024 Uiso 1 1 calc R . . C1' C 0.6693(3) 0.0746(3) -0.4346(3) 0.0271(9) Uani 1 1 d U . . H1'A H 0.6139 0.0450 -0.5074 0.041 Uiso 1 1 calc R . . H1'B H 0.7113 0.0214 -0.4147 0.041 Uiso 1 1 calc R . . H1'C H 0.7301 0.1388 -0.4308 0.041 Uiso 1 1 calc R . . C2' C 0.5369(3) 0.1816(3) -0.3733(3) 0.0164(8) Uani 1 1 d U . . C3' C 0.5106(3) 0.2172(3) -0.4649(3) 0.0200(8) Uani 1 1 d U . . H3'A H 0.5344 0.1871 -0.5249 0.024 Uiso 1 1 calc R . . C4' C 0.4479(3) 0.2991(3) -0.4668(3) 0.0233(9) Uani 1 1 d U . . C5' C 0.4082(3) 0.3420(3) -0.3809(3) 0.0202(8) Uani 1 1 d U . . H5'A H 0.3673 0.3971 -0.3834 0.024 Uiso 1 1 calc R . . C6' C 0.4294(3) 0.3021(2) -0.2881(3) 0.0161(8) Uani 1 1 d U . . C7' C 0.4981(3) 0.2228(3) -0.2815(2) 0.0144(8) Uani 1 1 d U . . C8' C 0.3689(3) 0.3405(3) -0.2089(3) 0.0207(9) Uani 1 1 d U . . H8'A H 0.3301 0.3956 -0.2194 0.025 Uiso 1 1 calc R . . C9 C 0.8752(3) 0.0804(3) -0.1317(3) 0.0267(9) Uani 1 1 d U . . C10 C 0.9919(4) 0.0852(4) -0.1683(4) 0.0458(13) Uani 1 1 d U . . H10B H 1.0620 0.0913 -0.1078 0.069 Uiso 1 1 calc R . . H10C H 1.0078 0.1474 -0.1959 0.069 Uiso 1 1 calc R . . H10D H 0.9798 0.0200 -0.2245 0.069 Uiso 1 1 calc R . . C11 C 0.7438(3) -0.0126(2) 0.1777(3) 0.0154(8) Uani 1 1 d U . . C12 C 0.7694(3) -0.0451(3) 0.2813(3) 0.0217(9) Uani 1 1 d U . . H12B H 0.7657 -0.1214 0.2656 0.032 Uiso 1 1 calc R . . H12C H 0.7078 -0.0307 0.3170 0.032 Uiso 1 1 calc R . . H12D H 0.8512 -0.0039 0.3279 0.032 Uiso 1 1 calc R . . C13 C 0.5682(3) 0.1544(3) 0.2395(3) 0.0160(8) Uani 1 1 d U . . C14 C 0.6739(3) 0.2503(3) 0.3102(3) 0.0233(9) Uani 1 1 d U . . H14A H 0.7192 0.2313 0.3718 0.035 Uiso 1 1 calc R . . H14B H 0.6409 0.3105 0.3347 0.035 Uiso 1 1 calc R . . H14C H 0.7293 0.2707 0.2693 0.035 Uiso 1 1 calc R . . C15 C 0.9005(8) 0.5308(8) 0.3940(7) 0.139(4) Uani 1 1 d U . . H15A H 0.9500 0.4816 0.3760 0.208 Uiso 1 1 calc R . . H15B H 0.8319 0.5221 0.3312 0.208 Uiso 1 1 calc R . . H15C H 0.8686 0.5151 0.4515 0.208 Uiso 1 1 calc R . . C16 C 0.9770(8) 0.6410(7) 0.4289(8) 0.133(4) Uani 1 1 d U . . H16A H 1.0460 0.6506 0.4929 0.160 Uiso 1 1 calc R . . H16B H 1.0116 0.6567 0.3719 0.160 Uiso 1 1 calc R . . C17 C 0.9555(8) 0.8091(6) 0.5037(9) 0.154(5) Uani 1 1 d U . . H17A H 0.9990 0.8423 0.4594 0.184 Uiso 1 1 calc R . . H17B H 1.0183 0.8106 0.5689 0.184 Uiso 1 1 calc R . . C18 C 0.8719(6) 0.8777(5) 0.5362(5) 0.083(2) Uani 1 1 d U . . H18A H 0.9214 0.9503 0.5758 0.125 Uiso 1 1 calc R . . H18B H 0.8291 0.8467 0.5813 0.125 Uiso 1 1 calc R . . H18C H 0.8115 0.8799 0.4723 0.125 Uiso 1 1 calc R . . O1W O 0.9027(6) 0.7125(6) 0.4529(5) 0.168(3) Uani 1 1 d U . . 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 0.01593(8) 0.01797(8) 0.01665(7) 0.00740(6) 0.00386(6) 0.00344(6) Zn2 0.01391(18) 0.01785(17) 0.02069(18) 0.00965(14) 0.00101(14) 0.00406(15) Zn1 0.01533(17) 0.01625(17) 0.01514(16) 0.00630(14) 0.00520(14) 0.00460(14) Br1 0.0269(2) 0.02562(19) 0.0450(2) 0.00813(17) 0.00151(17) -0.01218(17) Br1' 0.0416(2) 0.0508(2) 0.02272(16) 0.02545(15) 0.01111(15) 0.02175(17) N1 0.0331(15) 0.0333(14) 0.0220(13) 0.0201(11) 0.0145(12) 0.0181(13) O1 0.0128(12) 0.0214(11) 0.0510(15) 0.0217(11) -0.0068(11) -0.0017(10) O2 0.0154(11) 0.0125(10) 0.0187(11) 0.0054(9) 0.0006(9) -0.0017(9) O3 0.0171(11) 0.0179(11) 0.0226(11) 0.0084(9) 0.0040(9) 0.0015(9) O1' 0.0280(11) 0.0237(11) 0.0201(10) 0.0117(9) 0.0147(9) 0.0124(10) O2' 0.0163(10) 0.0150(10) 0.0118(9) 0.0080(8) 0.0034(8) 0.0057(9) O3' 0.0173(11) 0.0203(11) 0.0172(10) 0.0082(9) 0.0049(9) 0.0067(9) O4 0.0198(12) 0.0599(17) 0.0272(13) 0.0090(12) 0.0053(10) 0.0178(12) O5 0.0186(11) 0.0340(13) 0.0291(12) 0.0100(10) 0.0110(10) 0.0099(10) O6 0.0144(11) 0.0180(11) 0.0255(12) 0.0104(9) -0.0009(9) -0.0019(9) O7 0.0216(11) 0.0177(10) 0.0120(10) 0.0072(8) 0.0044(9) 0.0041(9) O8 0.0334(13) 0.0206(12) 0.0226(12) 0.0028(10) 0.0103(10) 0.0038(11) O9 0.0216(12) 0.0299(12) 0.0198(11) 0.0065(10) 0.0038(10) 0.0066(10) O10 0.0179(11) 0.0157(10) 0.0188(11) 0.0054(9) 0.0028(9) 0.0003(9) O11 0.0113(10) 0.0146(10) 0.0159(10) 0.0093(8) 0.0046(8) 0.0010(8) O12 0.0548(15) 0.0417(14) 0.0259(12) 0.0163(11) 0.0210(11) 0.0296(12) O13 0.0213(11) 0.0166(10) 0.0139(10) 0.0062(8) 0.0054(9) 0.0009(9) C1 0.022(2) 0.038(2) 0.112(4) 0.041(2) -0.014(2) 0.0013(19) C2 0.0179(17) 0.0177(16) 0.0291(17) 0.0112(14) 0.0018(14) 0.0000(14) C3 0.0152(17) 0.0239(17) 0.0319(19) 0.0103(15) -0.0004(15) -0.0016(15) C4 0.0214(17) 0.0158(16) 0.0281(18) 0.0030(14) 0.0052(14) -0.0046(14) C5 0.0277(18) 0.0175(16) 0.0257(17) 0.0095(13) 0.0071(14) 0.0008(14) C6 0.0176(16) 0.0133(15) 0.0229(16) 0.0064(13) 0.0032(13) 0.0001(13) C7 0.0172(15) 0.0148(15) 0.0167(15) 0.0039(12) 0.0053(12) -0.0015(13) C8 0.0258(17) 0.0175(15) 0.0172(15) 0.0068(13) 0.0066(13) 0.0059(14) C1' 0.0274(17) 0.0366(19) 0.0237(17) 0.0094(15) 0.0134(14) 0.0147(16) C2' 0.0163(16) 0.0148(15) 0.0141(15) 0.0049(12) -0.0013(12) 0.0012(13) C3' 0.0190(16) 0.0255(17) 0.0155(15) 0.0070(13) 0.0058(13) 0.0036(14) C4' 0.0264(18) 0.0288(17) 0.0180(15) 0.0159(13) 0.0067(13) 0.0042(15) C5' 0.0209(16) 0.0209(15) 0.0219(16) 0.0129(13) 0.0039(13) 0.0079(14) C6' 0.0173(15) 0.0140(14) 0.0170(15) 0.0064(12) 0.0039(12) 0.0031(13) C7' 0.0108(14) 0.0194(15) 0.0141(14) 0.0105(12) 0.0011(12) 0.0032(12) C8' 0.0173(16) 0.0205(16) 0.0229(17) 0.0102(13) 0.0012(13) 0.0029(14) C9 0.0196(16) 0.0236(17) 0.044(2) 0.0120(15) 0.0147(15) 0.0127(14) C10 0.0236(18) 0.062(3) 0.055(3) 0.009(2) 0.0222(18) 0.015(2) C11 0.0107(14) 0.0148(14) 0.0220(15) 0.0071(12) 0.0033(12) 0.0062(12) C12 0.0157(16) 0.0248(17) 0.0242(16) 0.0121(14) 0.0044(13) 0.0003(14) C13 0.0169(15) 0.0168(15) 0.0174(15) 0.0067(12) 0.0061(12) 0.0081(13) C14 0.0242(18) 0.0243(17) 0.0209(16) 0.0096(14) 0.0053(14) 0.0035(15) C15 0.136(7) 0.171(8) 0.087(6) -0.017(6) 0.022(5) 0.061(6) C16 0.119(6) 0.135(6) 0.120(7) -0.029(5) 0.022(5) 0.064(5) C17 0.091(6) 0.068(5) 0.233(12) -0.018(6) -0.027(7) 0.024(4) C18 0.087(5) 0.059(3) 0.080(4) 0.013(3) -0.005(4) 0.010(3) O1W 0.150(5) 0.169(5) 0.127(5) -0.048(4) -0.025(4) 0.093(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 Eu1 O10 2.409(2) 2_655 ? Eu1 O2 2.461(2) . ? Eu1 O7 2.461(2) . ? Eu1 O2' 2.467(2) . ? Eu1 O11 2.483(2) . ? Eu1 O3 2.498(2) . ? Eu1 O3' 2.501(2) . ? Eu1 O8 2.550(2) . ? Eu1 O9 2.550(3) . ? Eu1 N1 2.971(3) . ? Eu1 Zn2 3.5197(10) . ? Eu1 Zn1 3.5679(12) . ? Zn2 O6 1.940(2) . ? Zn2 O4 1.947(3) . ? Zn2 O11 2.001(2) . ? Zn2 O2 2.021(2) . ? Zn2 O1 2.331(3) . ? Zn1 O5 1.958(2) . ? Zn1 O13 1.962(2) 2_655 ? Zn1 O11 1.997(2) . ? Zn1 O2' 2.036(2) . ? Zn1 O1' 2.305(2) . ? Br1 C4 1.892(3) . ? Br1' C4' 1.897(4) . ? N1 O12 1.227(4) . ? N1 O9 1.263(3) . ? N1 O8 1.269(4) . ? O1 C2 1.367(4) . ? O1 C1 1.434(5) . ? O2 C7 1.331(4) . ? O3 C8 1.229(4) . ? O1' C2' 1.369(4) . ? O1' C1' 1.434(4) . ? O2' C7' 1.330(4) . ? O3' C8' 1.232(4) . ? O4 C9 1.258(5) . ? O5 C9 1.256(4) . ? O6 C11 1.272(4) . ? O7 C13 1.257(4) . ? O10 C11 1.257(4) . ? O10 Eu1 2.409(2) 2_655 ? O11 H11A 0.8355 . ? O13 C13 1.272(4) . ? O13 Zn1 1.962(2) 2_655 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.379(5) . ? C2 C7 1.401(5) . ? C3 C4 1.407(5) . ? C3 H3A 0.9300 . ? C4 C5 1.354(5) . ? C5 C6 1.416(5) . ? C5 H5A 0.9300 . ? C6 C7 1.407(5) . ? C6 C8 1.436(5) . ? C8 H8A 0.9300 . ? C1' H1'A 0.9600 . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C2' C3' 1.372(5) . ? C2' C7' 1.421(5) . ? C3' C4' 1.393(5) . ? C3' H3'A 0.9300 . ? C4' C5' 1.368(5) . ? C5' C6' 1.416(5) . ? C5' H5'A 0.9300 . ? C6' C7' 1.415(5) . ? C6' C8' 1.440(5) . ? C8' H8'A 0.9300 . ? C9 C10 1.515(5) . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 H10D 0.9600 . ? C11 C12 1.495(5) . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C13 C14 1.500(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.437(12) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O1W 1.410(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O1W 1.241(9) . ? C17 C18 1.499(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 O10 Eu1 O2 140.88(8) 2_655 . ? O10 Eu1 O7 79.64(8) 2_655 . ? O2 Eu1 O7 82.25(8) . . ? O10 Eu1 O2' 79.41(8) 2_655 . ? O2 Eu1 O2' 90.42(8) . . ? O7 Eu1 O2' 136.07(7) . . ? O10 Eu1 O11 75.57(8) 2_655 . ? O2 Eu1 O11 65.83(7) . . ? O7 Eu1 O11 71.39(8) . . ? O2' Eu1 O11 66.18(8) . . ? O10 Eu1 O3 142.13(8) 2_655 . ? O2 Eu1 O3 68.28(8) . . ? O7 Eu1 O3 137.02(7) . . ? O2' Eu1 O3 76.58(8) . . ? O11 Eu1 O3 119.14(8) . . ? O10 Eu1 O3' 79.31(8) 2_655 . ? O2 Eu1 O3' 132.64(8) . . ? O7 Eu1 O3' 140.92(8) . . ? O2' Eu1 O3' 70.52(8) . . ? O11 Eu1 O3' 132.94(7) . . ? O3 Eu1 O3' 65.28(8) . . ? O10 Eu1 O8 126.14(9) 2_655 . ? O2 Eu1 O8 81.77(9) . . ? O7 Eu1 O8 76.23(8) . . ? O2' Eu1 O8 145.57(8) . . ? O11 Eu1 O8 136.42(8) . . ? O3 Eu1 O8 69.36(8) . . ? O3' Eu1 O8 90.38(8) . . ? O10 Eu1 O9 77.26(8) 2_655 . ? O2 Eu1 O9 129.83(7) . . ? O7 Eu1 O9 74.17(8) . . ? O2' Eu1 O9 136.39(8) . . ? O11 Eu1 O9 139.16(8) . . ? O3 Eu1 O9 100.98(8) . . ? O3' Eu1 O9 69.28(8) . . ? O8 Eu1 O9 50.09(8) . . ? O10 Eu1 N1 101.87(8) 2_655 . ? O2 Eu1 N1 106.23(8) . . ? O7 Eu1 N1 74.46(8) . . ? O2' Eu1 N1 147.91(8) . . ? O11 Eu1 N1 145.66(8) . . ? O3 Eu1 N1 84.27(8) . . ? O3' Eu1 N1 78.17(8) . . ? O8 Eu1 N1 25.13(8) . . ? O9 Eu1 N1 24.99(7) . . ? O10 Eu1 Zn2 106.94(6) 2_655 . ? O2 Eu1 Zn2 34.02(5) . . ? O7 Eu1 Zn2 66.12(6) . . ? O2' Eu1 Zn2 83.93(6) . . ? O11 Eu1 Zn2 33.64(5) . . ? O3 Eu1 Zn2 99.19(6) . . ? O3' Eu1 Zn2 152.31(6) . . ? O8 Eu1 Zn2 105.91(7) . . ? O9 Eu1 Zn2 138.17(6) . . ? N1 Eu1 Zn2 124.90(6) . . ? O10 Eu1 Zn1 73.27(6) 2_655 . ? O2 Eu1 Zn1 77.55(6) . . ? O7 Eu1 Zn1 103.09(6) . . ? O2' Eu1 Zn1 33.55(5) . . ? O11 Eu1 Zn1 32.72(5) . . ? O3 Eu1 Zn1 100.32(6) . . ? O3' Eu1 Zn1 101.82(6) . . ? O8 Eu1 Zn1 159.18(6) . . ? O9 Eu1 Zn1 150.37(5) . . ? N1 Eu1 Zn1 174.98(6) . . ? Zn2 Eu1 Zn1 56.66(3) . . ? O6 Zn2 O4 114.46(12) . . ? O6 Zn2 O11 113.59(9) . . ? O4 Zn2 O11 105.19(10) . . ? O6 Zn2 O2 121.51(10) . . ? O4 Zn2 O2 113.11(12) . . ? O11 Zn2 O2 83.82(9) . . ? O6 Zn2 O1 81.31(9) . . ? O4 Zn2 O1 82.41(11) . . ? O11 Zn2 O1 156.98(9) . . ? O2 Zn2 O1 73.26(9) . . ? O6 Zn2 Eu1 116.86(8) . . ? O4 Zn2 Eu1 127.59(9) . . ? O11 Zn2 Eu1 43.44(6) . . ? O2 Zn2 Eu1 42.94(6) . . ? O1 Zn2 Eu1 114.82(7) . . ? O5 Zn1 O13 114.56(10) . 2_655 ? O5 Zn1 O11 103.91(10) . . ? O13 Zn1 O11 107.76(9) 2_655 . ? O5 Zn1 O2' 127.73(10) . . ? O13 Zn1 O2' 111.37(9) 2_655 . ? O11 Zn1 O2' 84.15(9) . . ? O5 Zn1 O1' 82.02(10) . . ? O13 Zn1 O1' 91.25(9) 2_655 . ? O11 Zn1 O1' 154.75(8) . . ? O2' Zn1 O1' 73.30(9) . . ? O5 Zn1 Eu1 127.33(7) . . ? O13 Zn1 Eu1 114.40(8) 2_655 . ? O11 Zn1 Eu1 42.22(7) . . ? O2' Zn1 Eu1 42.04(6) . . ? O1' Zn1 Eu1 114.96(6) . . ? O12 N1 O9 121.9(3) . . ? O12 N1 O8 121.1(3) . . ? O9 N1 O8 117.0(3) . . ? O12 N1 Eu1 175.6(2) . . ? O9 N1 Eu1 58.54(17) . . ? O8 N1 Eu1 58.54(16) . . ? C2 O1 C1 118.0(3) . . ? C2 O1 Zn2 109.24(19) . . ? C1 O1 Zn2 124.9(2) . . ? C7 O2 Zn2 117.7(2) . . ? C7 O2 Eu1 138.7(2) . . ? Zn2 O2 Eu1 103.04(9) . . ? C8 O3 Eu1 137.3(2) . . ? C2' O1' C1' 118.0(3) . . ? C2' O1' Zn1 112.9(2) . . ? C1' O1' Zn1 128.1(2) . . ? C7' O2' Zn1 120.9(2) . . ? C7' O2' Eu1 134.7(2) . . ? Zn1 O2' Eu1 104.41(9) . . ? C8' O3' Eu1 131.5(2) . . ? C9 O4 Zn2 133.0(2) . . ? C9 O5 Zn1 133.4(3) . . ? C11 O6 Zn2 122.0(2) . . ? C13 O7 Eu1 149.2(2) . . ? N1 O8 Eu1 96.33(17) . . ? N1 O9 Eu1 96.5(2) . . ? C11 O10 Eu1 148.3(2) . 2_655 ? Zn1 O11 Zn2 114.59(11) . . ? Zn1 O11 Eu1 105.07(10) . . ? Zn2 O11 Eu1 102.92(9) . . ? Zn1 O11 H11A 117.6 . . ? Zn2 O11 H11A 107.7 . . ? Eu1 O11 H11A 107.8 . . ? C13 O13 Zn1 123.41(19) . 2_655 ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.2(3) . . ? O1 C2 C7 113.4(3) . . ? C3 C2 C7 122.4(3) . . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 121.1(3) . . ? C5 C4 Br1 120.6(3) . . ? C3 C4 Br1 118.3(3) . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 120.3(3) . . ? C7 C6 C8 123.2(3) . . ? C5 C6 C8 116.2(3) . . ? O2 C7 C2 119.9(3) . . ? O2 C7 C6 122.6(3) . . ? C2 C7 C6 117.5(3) . . ? O3 C8 C6 126.8(3) . . ? O3 C8 H8A 116.6 . . ? C6 C8 H8A 116.6 . . ? O1' C1' H1'A 109.5 . . ? O1' C1' H1'B 109.5 . . ? H1'A C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'A C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C2' C3' 124.7(3) . . ? O1' C2' C7' 113.2(3) . . ? C3' C2' C7' 122.0(3) . . ? C2' C3' C4' 119.2(3) . . ? C2' C3' H3'A 120.4 . . ? C4' C3' H3'A 120.4 . . ? C5' C4' C3' 121.4(3) . . ? C5' C4' Br1' 119.4(3) . . ? C3' C4' Br1' 119.2(3) . . ? C4' C5' C6' 119.9(3) . . ? C4' C5' H5'A 120.1 . . ? C6' C5' H5'A 120.1 . . ? C7' C6' C5' 120.0(3) . . ? C7' C6' C8' 123.9(3) . . ? C5' C6' C8' 115.9(3) . . ? O2' C7' C6' 124.1(3) . . ? O2' C7' C2' 118.6(3) . . ? C6' C7' C2' 117.3(3) . . ? O3' C8' C6' 127.0(3) . . ? O3' C8' H8'A 116.5 . . ? C6' C8' H8'A 116.5 . . ? O5 C9 O4 126.3(4) . . ? O5 C9 C10 117.7(4) . . ? O4 C9 C10 116.0(3) . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10D 109.5 . . ? H10B C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? O10 C11 O6 122.9(3) . . ? O10 C11 C12 121.0(3) . . ? O6 C11 C12 116.1(3) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? O7 C13 O13 123.4(3) . . ? O7 C13 C14 119.3(3) . . ? O13 C13 C14 117.3(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1W C16 C15 108.9(8) . . ? O1W C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? O1W C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O1W C17 C18 115.8(8) . . ? O1W C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? O1W C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 O1W C16 118.7(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.285 _refine_diff_density_min -1.575 _refine_diff_density_rms 0.170