# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Pan, Mei' _publ_contact_author_name 'Pan, Mei' _publ_contact_author_email panm@mail.sysu.edu.cn _publ_section_title ; Lanthanide homometallic and d-f heterometallic MOFs from the same tripodal ligand: structural comparison, one photon (OP) vs. two photon (TP) luminescence and selective guest adsorption behavior ; # Attachment '- Compds.txt' data_1 _database_code_depnum_ccdc_archive 'CCDC 861079' #TrackingRef '- Compds.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 Eu N7 O6' _chemical_formula_weight 958.80 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P -3 c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z-1/2' 'x-y, -y, -z-1/2' '-x, -x+y, -z-1/2' _cell_length_a 18.7594(9) _cell_length_b 18.7594 _cell_length_c 15.4559(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4710.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.8060 _cell_measurement_theta_max 30.1296 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8739 _exptl_absorpt_correction_T_max 0.9728 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova (Agilent Technolies)' _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 11942 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3557 _reflns_number_gt 2150 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+10.3665P] 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 3557 _refine_ls_number_parameters 190 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1656 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.6667 0.3333 0.23627(7) 0.0219(4) Uani 0.50 3 d SPU . 1 Eu1' Eu 0.6667 0.3333 0.2336(2) 0.096(2) Uani 0.50 3 d SP . 2 O1 O 0.5847(3) 0.4024(3) 0.2588(3) 0.0524(12) Uani 1 1 d . . . O2 O 0.5600(3) 0.3002(3) 0.3468(3) 0.0563(13) Uani 1 1 d . . . N1 N 0.2756(3) 0.4467(3) 0.4411(4) 0.0552(15) Uani 1 1 d . . . N2 N 0.2542(4) 0.5256(4) 0.3486(4) 0.0570(16) Uani 1 1 d . . . N3 N 0.3333 0.6667 0.4387(7) 0.052(2) Uani 1 3 d S . . C1 C 0.5485(4) 0.3578(4) 0.3232(5) 0.0531(17) Uani 1 1 d . . . C2 C 0.4902(4) 0.3758(4) 0.3732(5) 0.0531(17) Uani 1 1 d . . . C3 C 0.4406(5) 0.3244(5) 0.4353(6) 0.067(2) Uani 1 1 d . . . H3 H 0.4433 0.2764 0.4484 0.081 Uiso 1 1 calc R . . C4 C 0.3864(5) 0.3396(4) 0.4799(5) 0.061(2) Uani 1 1 d . . . H4 H 0.3520 0.3021 0.5231 0.073 Uiso 1 1 calc R . . C5 C 0.3816(4) 0.4102(4) 0.4619(5) 0.0554(18) Uani 1 1 d . . . C6 C 0.4342(5) 0.4633(5) 0.3985(5) 0.0607(19) Uani 1 1 d . . . H6 H 0.4322 0.5115 0.3844 0.073 Uiso 1 1 calc R . . C7 C 0.4889(5) 0.4472(5) 0.3562(5) 0.0596(19) Uani 1 1 d . . . H7 H 0.5259 0.4854 0.3150 0.071 Uiso 1 1 calc R . . C8 C 0.3194(5) 0.4258(5) 0.5066(5) 0.060(2) Uani 1 1 d . . . H8A H 0.2796 0.3760 0.5389 0.072 Uiso 1 1 calc R . . H8B H 0.3475 0.4716 0.5483 0.072 Uiso 1 1 calc R . . C9 C 0.2223(5) 0.3949(5) 0.3795(5) 0.0609(19) Uani 1 1 d . . . C10 C 0.1858(6) 0.3112(5) 0.3700(7) 0.088(3) Uani 1 1 d . . . H10 H 0.1964 0.2781 0.4084 0.106 Uiso 1 1 calc R . . C11 C 0.1329(7) 0.2785(6) 0.3011(8) 0.111(4) Uani 1 1 d . . . H11 H 0.1067 0.2208 0.2916 0.133 Uiso 1 1 calc R . . C12 C 0.1150(7) 0.3268(6) 0.2428(7) 0.107(4) Uani 1 1 d . . . H12 H 0.0769 0.3012 0.1968 0.128 Uiso 1 1 calc R . . C13 C 0.1534(5) 0.4105(5) 0.2540(6) 0.078(2) Uani 1 1 d . . . H13 H 0.1427 0.4441 0.2164 0.093 Uiso 1 1 calc R . . C14 C 0.2081(4) 0.4441(4) 0.3217(5) 0.0581(19) Uani 1 1 d . . . C15 C 0.2932(4) 0.5251(4) 0.4194(5) 0.0528(17) Uani 1 1 d . . . C16 C 0.3460(5) 0.5998(5) 0.4708(5) 0.0606(19) Uani 1 1 d . . . H16A H 0.3311 0.5894 0.5328 0.073 Uiso 1 1 calc R . . H16B H 0.4045 0.6153 0.4645 0.073 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 0.0267(7) 0.0267(7) 0.0123(4) 0.000 0.000 0.0133(3) Eu1' 0.0502(17) 0.0502(17) 0.187(4) 0.000 0.000 0.0251(9) O1 0.049(3) 0.053(3) 0.059(3) 0.008(2) 0.006(2) 0.028(2) O2 0.043(3) 0.050(3) 0.080(3) 0.006(2) -0.002(2) 0.026(2) N1 0.051(3) 0.046(3) 0.071(4) 0.007(3) 0.001(3) 0.025(3) N2 0.055(4) 0.052(4) 0.059(4) 0.000(3) -0.001(3) 0.023(3) N3 0.042(3) 0.042(3) 0.071(7) 0.000 0.000 0.0212(16) C1 0.036(3) 0.048(4) 0.075(5) -0.002(4) -0.007(3) 0.021(3) C2 0.045(4) 0.053(4) 0.065(4) 0.011(4) 0.002(3) 0.027(3) C3 0.055(5) 0.059(5) 0.099(6) 0.009(4) -0.006(4) 0.038(4) C4 0.054(4) 0.053(4) 0.079(5) 0.015(4) 0.000(4) 0.028(4) C5 0.051(4) 0.052(4) 0.060(4) 0.003(4) -0.002(4) 0.024(3) C6 0.062(5) 0.057(4) 0.072(5) 0.013(4) 0.004(4) 0.037(4) C7 0.053(4) 0.056(4) 0.067(5) 0.004(4) 0.007(4) 0.024(4) C8 0.061(5) 0.060(5) 0.066(5) 0.011(4) 0.010(4) 0.035(4) C9 0.051(4) 0.048(4) 0.076(5) 0.005(4) -0.004(4) 0.019(4) C10 0.102(7) 0.047(5) 0.101(7) 0.000(5) -0.035(6) 0.026(5) C11 0.133(10) 0.047(5) 0.129(9) -0.006(6) -0.037(8) 0.027(6) C12 0.111(9) 0.061(6) 0.115(8) 0.003(6) -0.044(7) 0.018(6) C13 0.073(5) 0.051(5) 0.096(6) 0.003(4) -0.019(5) 0.021(4) C14 0.050(4) 0.040(4) 0.071(5) -0.001(4) -0.008(4) 0.012(3) C15 0.041(4) 0.060(5) 0.057(4) 0.006(4) 0.007(3) 0.025(4) C16 0.053(4) 0.058(4) 0.072(5) 0.008(4) 0.006(4) 0.029(4) 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 O2 2.463(5) 2_655 ? Eu1 O2 2.463(5) 3_665 ? Eu1 O2 2.463(5) . ? Eu1 O1 2.481(5) 2_655 ? Eu1 O1 2.481(5) 3_665 ? Eu1 O1 2.481(5) . ? Eu1 N2 2.645(6) 12_656 ? Eu1 N2 2.645(6) 10_556 ? Eu1 N2 2.645(6) 11_666 ? Eu1 N3 2.704(11) 10_556 ? Eu1 C1 2.819(7) 2_655 ? Eu1 C1 2.819(7) 3_665 ? Eu1' O1 2.488(5) 2_655 ? Eu1' O1 2.488(5) 3_665 ? Eu1' O1 2.488(5) . ? Eu1' O2 2.492(6) 2_655 ? Eu1' O2 2.492(6) 3_665 ? Eu1' O2 2.492(6) . ? Eu1' N2 2.625(7) 12_656 ? Eu1' N2 2.625(7) 10_556 ? Eu1' N2 2.625(7) 11_666 ? Eu1' N3 2.662(12) 10_556 ? O1 C1 1.259(8) . ? O2 C1 1.257(8) . ? N1 C9 1.371(9) . ? N1 C15 1.377(9) . ? N1 C8 1.475(9) . ? N2 C15 1.320(9) . ? N2 C14 1.392(9) . ? N2 Eu1' 2.625(7) 10_556 ? N2 Eu1 2.645(6) 10_556 ? N3 C16 1.474(8) 3_565 ? N3 C16 1.474(8) 2_665 ? N3 C16 1.474(8) . ? N3 Eu1' 2.662(12) 10_556 ? N3 Eu1 2.704(11) 10_556 ? C1 C2 1.509(9) . ? C2 C3 1.348(10) . ? C2 C7 1.378(10) . ? C3 C4 1.371(11) . ? C4 C5 1.399(10) . ? C5 C6 1.393(10) . ? C5 C8 1.506(10) . ? C6 C7 1.371(10) . ? C9 C10 1.371(11) . ? C9 C14 1.402(11) . ? C10 C11 1.374(13) . ? C11 C12 1.431(14) . ? C12 C13 1.372(11) . ? C13 C14 1.377(11) . ? C15 C16 1.480(10) . ? 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 O2 Eu1 O2 77.18(18) 2_655 3_665 ? O2 Eu1 O2 77.18(18) 2_655 . ? O2 Eu1 O2 77.18(18) 3_665 . ? O2 Eu1 O1 52.94(15) 2_655 2_655 ? O2 Eu1 O1 126.25(16) 3_665 2_655 ? O2 Eu1 O1 73.73(16) . 2_655 ? O2 Eu1 O1 73.73(16) 2_655 3_665 ? O2 Eu1 O1 52.94(15) 3_665 3_665 ? O2 Eu1 O1 126.25(16) . 3_665 ? O1 Eu1 O1 118.07(5) 2_655 3_665 ? O2 Eu1 O1 126.25(16) 2_655 . ? O2 Eu1 O1 73.73(16) 3_665 . ? O2 Eu1 O1 52.94(15) . . ? O1 Eu1 O1 118.07(5) 2_655 . ? O1 Eu1 O1 118.07(5) 3_665 . ? O2 Eu1 N2 75.14(18) 2_655 12_656 ? O2 Eu1 N2 119.43(17) 3_665 12_656 ? O2 Eu1 N2 142.80(17) . 12_656 ? O1 Eu1 N2 69.85(16) 2_655 12_656 ? O1 Eu1 N2 67.88(16) 3_665 12_656 ? O1 Eu1 N2 158.31(19) . 12_656 ? O2 Eu1 N2 119.43(17) 2_655 10_556 ? O2 Eu1 N2 142.80(17) 3_665 10_556 ? O2 Eu1 N2 75.14(18) . 10_556 ? O1 Eu1 N2 67.88(16) 2_655 10_556 ? O1 Eu1 N2 158.31(19) 3_665 10_556 ? O1 Eu1 N2 69.85(16) . 10_556 ? N2 Eu1 N2 97.56(18) 12_656 10_556 ? O2 Eu1 N2 142.80(17) 2_655 11_666 ? O2 Eu1 N2 75.14(18) 3_665 11_666 ? O2 Eu1 N2 119.43(17) . 11_666 ? O1 Eu1 N2 158.31(19) 2_655 11_666 ? O1 Eu1 N2 69.85(16) 3_665 11_666 ? O1 Eu1 N2 67.88(16) . 11_666 ? N2 Eu1 N2 97.56(18) 12_656 11_666 ? N2 Eu1 N2 97.56(18) 10_556 11_666 ? O2 Eu1 N3 133.92(12) 2_655 10_556 ? O2 Eu1 N3 133.92(12) 3_665 10_556 ? O2 Eu1 N3 133.92(12) . 10_556 ? O1 Eu1 N3 98.05(11) 2_655 10_556 ? O1 Eu1 N3 98.05(11) 3_665 10_556 ? O1 Eu1 N3 98.05(11) . 10_556 ? N2 Eu1 N3 60.29(14) 12_656 10_556 ? N2 Eu1 N3 60.29(14) 10_556 10_556 ? N2 Eu1 N3 60.29(14) 11_666 10_556 ? O1 Eu1' O1 117.60(7) 2_655 3_665 ? O1 Eu1' O1 117.60(8) 2_655 . ? O1 Eu1' O1 117.60(7) 3_665 . ? O1 Eu1' O2 52.54(16) 2_655 2_655 ? O1 Eu1' O2 73.12(16) 3_665 2_655 ? O1 Eu1' O2 124.7(2) . 2_655 ? O1 Eu1' O2 124.7(2) 2_655 3_665 ? O1 Eu1' O2 52.54(16) 3_665 3_665 ? O1 Eu1' O2 73.12(16) . 3_665 ? O2 Eu1' O2 76.1(2) 2_655 3_665 ? O1 Eu1' O2 73.12(16) 2_655 . ? O1 Eu1' O2 124.7(2) 3_665 . ? O1 Eu1' O2 52.54(16) . . ? O2 Eu1' O2 76.1(2) 2_655 . ? O2 Eu1' O2 76.1(2) 3_665 . ? O1 Eu1' N2 70.10(16) 2_655 12_656 ? O1 Eu1' N2 68.12(16) 3_665 12_656 ? O1 Eu1' N2 160.1(2) . 12_656 ? O2 Eu1' N2 75.03(18) 2_655 12_656 ? O2 Eu1' N2 119.11(17) 3_665 12_656 ? O2 Eu1' N2 142.24(18) . 12_656 ? O1 Eu1' N2 68.12(16) 2_655 10_556 ? O1 Eu1' N2 160.1(2) 3_665 10_556 ? O1 Eu1' N2 70.10(16) . 10_556 ? O2 Eu1' N2 119.11(17) 2_655 10_556 ? O2 Eu1' N2 142.24(18) 3_665 10_556 ? O2 Eu1' N2 75.03(18) . 10_556 ? N2 Eu1' N2 98.6(2) 12_656 10_556 ? O1 Eu1' N2 160.1(2) 2_655 11_666 ? O1 Eu1' N2 70.10(16) 3_665 11_666 ? O1 Eu1' N2 68.12(16) . 11_666 ? O2 Eu1' N2 142.24(18) 2_655 11_666 ? O2 Eu1' N2 75.03(18) 3_665 11_666 ? O2 Eu1' N2 119.11(17) . 11_666 ? N2 Eu1' N2 98.6(2) 12_656 11_666 ? N2 Eu1' N2 98.6(2) 10_556 11_666 ? O1 Eu1' N3 99.01(14) 2_655 10_556 ? O1 Eu1' N3 99.01(14) 3_665 10_556 ? O1 Eu1' N3 99.01(14) . 10_556 ? O2 Eu1' N3 134.62(13) 2_655 10_556 ? O2 Eu1' N3 134.62(13) 3_665 10_556 ? O2 Eu1' N3 134.62(13) . 10_556 ? N2 Eu1' N3 61.08(16) 12_656 10_556 ? N2 Eu1' N3 61.08(16) 10_556 10_556 ? N2 Eu1' N3 61.08(16) 11_666 10_556 ? C1 O1 Eu1 91.9(4) . . ? C1 O1 Eu1' 92.6(4) . . ? Eu1 O1 Eu1' 0.95(10) . . ? C1 O2 Eu1 92.8(4) . . ? C1 O2 Eu1' 92.5(4) . . ? Eu1 O2 Eu1' 0.69(8) . . ? C9 N1 C15 106.7(6) . . ? C9 N1 C8 126.4(6) . . ? C15 N1 C8 125.7(6) . . ? C15 N2 C14 106.3(6) . . ? C15 N2 Eu1' 111.9(5) . 10_556 ? C14 N2 Eu1' 133.7(5) . 10_556 ? C15 N2 Eu1 112.5(5) . 10_556 ? C14 N2 Eu1 132.9(5) . 10_556 ? Eu1' N2 Eu1 0.79(9) 10_556 10_556 ? C16 N3 C16 109.2(5) 3_565 2_665 ? C16 N3 C16 109.2(5) 3_565 . ? C16 N3 C16 109.2(5) 2_665 . ? C16 N3 Eu1' 109.7(5) 3_565 10_556 ? C16 N3 Eu1' 109.7(5) 2_665 10_556 ? C16 N3 Eu1' 109.7(5) . 10_556 ? C16 N3 Eu1 109.7(5) 3_565 10_556 ? C16 N3 Eu1 109.7(5) 2_665 10_556 ? C16 N3 Eu1 109.7(5) . 10_556 ? Eu1' N3 Eu1 0.0 10_556 10_556 ? O1 C1 O2 122.3(7) . . ? O1 C1 C2 117.8(6) . . ? O2 C1 C2 119.9(7) . . ? O1 C1 Eu1 61.6(4) . . ? O2 C1 Eu1 60.8(4) . . ? C2 C1 Eu1 176.0(5) . . ? O1 C1 Eu1' 61.1(4) . . ? O2 C1 Eu1' 61.3(4) . . ? C2 C1 Eu1' 176.4(5) . . ? Eu1 C1 Eu1' 0.74(8) . . ? C3 C2 C7 119.3(7) . . ? C3 C2 C1 121.6(7) . . ? C7 C2 C1 119.2(6) . . ? C2 C3 C4 121.9(7) . . ? C3 C4 C5 120.0(7) . . ? C6 C5 C4 117.4(7) . . ? C6 C5 C8 121.6(7) . . ? C4 C5 C8 121.0(6) . . ? C7 C6 C5 121.2(7) . . ? C6 C7 C2 120.1(7) . . ? N1 C8 C5 109.0(6) . . ? C10 C9 N1 131.0(8) . . ? C10 C9 C14 122.3(8) . . ? N1 C9 C14 106.8(6) . . ? C9 C10 C11 115.5(9) . . ? C10 C11 C12 123.5(9) . . ? C13 C12 C11 119.3(9) . . ? C12 C13 C14 117.7(8) . . ? C13 C14 N2 129.9(7) . . ? C13 C14 C9 121.8(7) . . ? N2 C14 C9 108.3(6) . . ? N2 C15 N1 111.9(6) . . ? N2 C15 C16 123.3(7) . . ? N1 C15 C16 124.7(7) . . ? N3 C16 C15 108.0(6) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.778 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.121 data_2 _database_code_depnum_ccdc_archive 'CCDC 861080' #TrackingRef '- Compds.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H120 Cl4 Eu2 N18 O21 Zn2' _chemical_formula_weight 2630.72 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' Cl Cl 0.1484 0.1585 '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' 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 13.0720(10) _cell_length_b 14.3250(10) _cell_length_c 16.928(2) _cell_angle_alpha 96.764(2) _cell_angle_beta 112.235(12) _cell_angle_gamma 93.165(5) _cell_volume 2896.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6840 _exptl_absorpt_correction_T_max 0.7345 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Oxford Germin S Ultra' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13834 _diffrn_reflns_av_R_equivalents 0.1402 _diffrn_reflns_av_sigmaI/netI 0.1488 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.23 _reflns_number_total 8853 _reflns_number_gt 4880 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0510P)^2^+70.0000P] 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 8853 _refine_ls_number_parameters 655 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1605 _refine_ls_R_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.2618 _refine_ls_wR_factor_gt 0.2179 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.002 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 0.35827(5) -0.40667(4) -0.09680(4) 0.04506(16) Uani 1 1 d . . . Zn2 Zn 0.37768(9) 0.22269(8) 0.36722(7) 0.0373(3) Uani 1 1 d . . . Cl1 Cl 0.24922(18) 0.23343(17) 0.42789(14) 0.0362(6) Uani 1 1 d . . . Cl2 Cl 0.53892(18) -0.40822(15) -0.14280(13) 0.0336(6) Uani 1 1 d . . . N1 N 0.4130(6) 0.0849(5) 0.3696(4) 0.034(2) Uani 1 1 d . . . N2 N 0.5332(6) -0.0223(5) 0.3858(4) 0.030(2) Uani 1 1 d . . . N3 N 0.3017(6) 0.2364(5) 0.2405(4) 0.028(2) Uani 1 1 d U . . N4 N 0.2811(6) 0.2104(5) 0.1037(4) 0.030(2) Uani 1 1 d . . . N5 N 0.5111(6) 0.3190(5) 0.4435(4) 0.027(2) Uani 1 1 d . . . N6 N 0.6580(6) 0.4181(5) 0.4686(5) 0.036(2) Uani 1 1 d . . . N7 N 0.5199(5) 0.2074(4) 0.3076(4) 0.0218(18) Uani 1 1 d . . . C1 C 0.5661(7) -0.3691(7) 0.1129(5) 0.036(3) Uani 1 1 d . . . C2 C 0.5823(7) -0.2888(6) 0.1848(5) 0.031(2) Uani 1 1 d . . . C3 C 0.6574(7) -0.2931(6) 0.2669(5) 0.030(2) Uani 1 1 d . . . H3A H 0.6991 -0.3458 0.2770 0.037 Uiso 1 1 calc R . . C4 C 0.6736(8) -0.2229(7) 0.3346(6) 0.039(3) Uani 1 1 d . . . H4A H 0.7259 -0.2274 0.3908 0.047 Uiso 1 1 calc R . . C5 C 0.6118(7) -0.1438(6) 0.3201(5) 0.030(2) Uani 1 1 d . . . C6 C 0.5395(8) -0.1399(6) 0.2356(5) 0.034(3) Uani 1 1 d . . . H6A H 0.5006 -0.0858 0.2236 0.041 Uiso 1 1 calc R . . C7 C 0.5229(7) -0.2109(7) 0.1700(5) 0.035(3) Uani 1 1 d . . . H7A H 0.4704 -0.2072 0.1137 0.042 Uiso 1 1 calc R . . C8 C 0.6332(8) -0.0679(7) 0.3936(5) 0.036(3) Uani 1 1 d . . . H8A H 0.6599 -0.0950 0.4481 0.043 Uiso 1 1 calc R . . H8B H 0.6923 -0.0199 0.3962 0.043 Uiso 1 1 calc R . . C9 C 0.4404(7) -0.0645(6) 0.3968(5) 0.030(2) Uani 1 1 d U . . C10 C 0.4170(9) -0.1539(7) 0.4118(6) 0.042(3) Uani 1 1 d . . . H10A H 0.4685 -0.1995 0.4181 0.051 Uiso 1 1 calc R . . C11 C 0.3165(9) -0.1749(7) 0.4173(6) 0.049(3) Uani 1 1 d . . . H11A H 0.2985 -0.2356 0.4288 0.059 Uiso 1 1 calc R . . C12 C 0.2387(8) -0.1066(7) 0.4060(6) 0.044(3) Uani 1 1 d . . . H12A H 0.1693 -0.1228 0.4096 0.053 Uiso 1 1 calc R . . C13 C 0.2622(8) -0.0180(7) 0.3901(6) 0.039(3) Uani 1 1 d . . . H13A H 0.2097 0.0270 0.3819 0.047 Uiso 1 1 calc R . . C14 C 0.3676(8) 0.0047(6) 0.3863(5) 0.035(3) Uani 1 1 d . . . C15 C 0.5091(8) 0.0662(6) 0.3698(5) 0.031(3) Uani 1 1 d . . . C16 C 0.5878(7) 0.1345(6) 0.3498(5) 0.030(2) Uani 1 1 d . . . H16A H 0.6502 0.1637 0.4036 0.037 Uiso 1 1 calc R . . H16B H 0.6185 0.1005 0.3108 0.037 Uiso 1 1 calc R . . C17 C 0.4611(7) 0.1772(7) 0.2129(5) 0.033(3) Uani 1 1 d . . . H17A H 0.4547 0.1074 0.1990 0.040 Uiso 1 1 calc R . . H17B H 0.5028 0.2052 0.1818 0.040 Uiso 1 1 calc R . . C18 C 0.3481(7) 0.2102(6) 0.1862(5) 0.031(3) Uani 1 1 d . . . C19 C 0.1938(7) 0.2607(6) 0.1899(5) 0.030(2) Uani 1 1 d . . . C20 C 0.1103(7) 0.2933(6) 0.2122(6) 0.035(3) Uani 1 1 d . . . H20A H 0.1191 0.3052 0.2710 0.042 Uiso 1 1 calc R . . C21 C 0.0124(8) 0.3086(7) 0.1464(6) 0.042(3) Uani 1 1 d . . . H21A H -0.0462 0.3329 0.1599 0.050 Uiso 1 1 calc R . . C22 C 0.0007(8) 0.2879(8) 0.0603(7) 0.055(4) Uani 1 1 d . . . H22A H -0.0675 0.2974 0.0163 0.066 Uiso 1 1 calc R . . C23 C 0.0833(8) 0.2545(7) 0.0361(6) 0.041(3) Uani 1 1 d . . . H23A H 0.0739 0.2408 -0.0227 0.049 Uiso 1 1 calc R . . C24 C 0.1803(8) 0.2424(6) 0.1028(6) 0.035(3) Uani 1 1 d . . . C25 C 0.3077(8) 0.1872(6) 0.0279(5) 0.034(3) Uani 1 1 d . . . H25A H 0.3824 0.2188 0.0399 0.041 Uiso 1 1 calc R . . H25B H 0.2537 0.2133 -0.0209 0.041 Uiso 1 1 calc R . . C26 C 0.3060(7) 0.0801(6) 0.0001(5) 0.032(3) Uani 1 1 d . . . C27 C 0.2542(9) 0.0108(7) 0.0248(7) 0.049(3) Uani 1 1 d . . . H27A H 0.2149 0.0291 0.0601 0.059 Uiso 1 1 calc R . . C28 C 0.2557(9) -0.0839(8) 0.0015(6) 0.054(3) Uani 1 1 d . . . H28A H 0.2172 -0.1299 0.0193 0.065 Uiso 1 1 calc R . . C29 C 0.3129(7) -0.1099(6) -0.0472(5) 0.031(3) Uani 1 1 d . . . C30 C 0.3651(11) -0.0439(7) -0.0744(7) 0.060(4) Uani 1 1 d . . . H30A H 0.4033 -0.0631 -0.1103 0.072 Uiso 1 1 calc R . . C31 C 0.3626(9) 0.0522(7) -0.0496(7) 0.056(3) Uani 1 1 d . . . H31A H 0.4008 0.0982 -0.0677 0.068 Uiso 1 1 calc R . . C32 C 0.3244(8) -0.2153(6) -0.0687(6) 0.043(3) Uani 1 1 d . . . C33 C 0.5852(7) 0.2997(6) 0.3303(5) 0.026(2) Uani 1 1 d . . . H33A H 0.5519 0.3396 0.2851 0.031 Uiso 1 1 calc R . . H33B H 0.6622 0.2922 0.3355 0.031 Uiso 1 1 calc R . . C34 C 0.5854(7) 0.3439(6) 0.4130(5) 0.027(2) Uani 1 1 d . . . C35 C 0.5349(7) 0.3811(6) 0.5221(5) 0.026(2) Uani 1 1 d . . . C36 C 0.4845(8) 0.3808(6) 0.5797(5) 0.032(3) Uani 1 1 d . . . H36A H 0.4234 0.3357 0.5703 0.039 Uiso 1 1 calc R . . C37 C 0.5274(8) 0.4504(6) 0.6536(6) 0.036(3) Uani 1 1 d . . . H37A H 0.4925 0.4553 0.6938 0.043 Uiso 1 1 calc R . . C38 C 0.6214(8) 0.5125(6) 0.6677(6) 0.042(3) Uani 1 1 d . . . H38A H 0.6504 0.5578 0.7187 0.050 Uiso 1 1 calc R . . C39 C 0.6731(8) 0.5100(6) 0.6104(5) 0.036(3) Uani 1 1 d . . . H39A H 0.7356 0.5535 0.6199 0.043 Uiso 1 1 calc R . . C40 C 0.6293(8) 0.4404(6) 0.5373(5) 0.036(3) Uani 1 1 d . . . C41 C 0.7476(7) 0.4705(7) 0.4508(6) 0.039(3) Uani 1 1 d . . . H41A H 0.7239 0.5321 0.4339 0.047 Uiso 1 1 calc R . . H41B H 0.7585 0.4338 0.4018 0.047 Uiso 1 1 calc R . . C42 C 0.8573(7) 0.4872(6) 0.5289(6) 0.035(3) Uani 1 1 d . . . C43 C 0.8941(8) 0.4204(7) 0.5815(7) 0.047(3) Uani 1 1 d . . . H43A H 0.8539 0.3595 0.5681 0.057 Uiso 1 1 calc R . . C44 C 0.9927(8) 0.4437(7) 0.6558(7) 0.049(3) Uani 1 1 d . . . H44A H 1.0147 0.4005 0.6961 0.059 Uiso 1 1 calc R . . C45 C 1.0578(7) 0.5282(7) 0.6712(6) 0.036(3) Uani 1 1 d . . . C46 C 1.0233(7) 0.5921(7) 0.6131(6) 0.036(3) Uani 1 1 d . . . H46A H 1.0696 0.6489 0.6212 0.043 Uiso 1 1 calc R . . C47 C 0.9216(7) 0.5737(6) 0.5431(6) 0.035(3) Uani 1 1 d . . . H47A H 0.8962 0.6191 0.5055 0.042 Uiso 1 1 calc R . . C48 C 1.1655(7) 0.5542(7) 0.7491(6) 0.040(3) Uani 1 1 d . . . O1 O 0.4910(6) -0.3691(5) 0.0413(4) 0.051(2) Uani 1 1 d . . . O2 O 0.6276(5) -0.4338(4) 0.1319(4) 0.044(2) Uani 1 1 d . . . O3 O 0.3944(5) -0.2374(4) -0.1033(4) 0.0392(18) Uani 1 1 d . . . O4 O 0.2668(5) -0.2790(4) -0.0532(4) 0.0386(18) Uani 1 1 d . . . O5 O 1.2426(5) 0.6072(5) 0.7511(4) 0.046(2) Uani 1 1 d . . . O6 O 1.1678(5) 0.5166(5) 0.8145(4) 0.046(2) Uani 1 1 d . . . O7 O 0.2908(5) -0.4909(5) -0.0047(4) 0.0421(19) Uani 1 1 d . . . O8 O 0.1813(6) 0.3360(5) 0.8857(5) 0.060(3) Uani 1 1 d . . . O9 O 0.1627(13) 0.7832(11) 0.5654(10) 0.060(4) Uiso 0.50 1 d P . . N9 N 0.0868(5) 1.0104(4) 0.7509(5) 0.183(9) Uiso 1 1 d D . . O11 O 0.1895(10) 0.9682(12) 0.6727(9) 0.220(9) Uiso 1 1 d D . . C53 C 0.1037(17) 0.8391(5) 0.7242(13) 0.221(14) Uiso 1 1 d D . . H53A H 0.0820 0.8336 0.7730 0.332 Uiso 1 1 calc R . . H53B H 0.1706 0.8072 0.7320 0.332 Uiso 1 1 calc R . . H53C H 0.0432 0.8095 0.6705 0.332 Uiso 1 1 calc R . . C54 C 0.1262(8) 0.9365(4) 0.7200(8) 0.300 Uiso 1 1 d D . . C55 C 0.0144(7) 0.9885(13) 0.7953(7) 0.171(10) Uiso 1 1 d D . . H55A H -0.0028 0.9198 0.7880 0.257 Uiso 1 1 calc R . . H55B H -0.0546 1.0177 0.7709 0.257 Uiso 1 1 calc R . . H55C H 0.0520 1.0134 0.8569 0.257 Uiso 1 1 calc R . . C56 C 0.1201(12) 1.1054(5) 0.7396(10) 0.124(7) Uiso 1 1 d D . . H56A H 0.1924 1.1295 0.7855 0.186 Uiso 1 1 calc R . . H56B H 0.0645 1.1474 0.7425 0.186 Uiso 1 1 calc R . . H56C H 0.1258 1.1030 0.6833 0.186 Uiso 1 1 calc R . . N8 N 0.1999(7) 0.7090(6) 0.1748(8) 0.115(5) Uiso 1 1 d D . . O10 O 0.0372(7) 0.7195(7) 0.1884(6) 0.092(3) Uiso 1 1 d D . . C49 C 0.0959(13) 0.5576(7) 0.1589(11) 0.111(6) Uiso 1 1 d D . . H49A H 0.1093 0.5340 0.1073 0.167 Uiso 1 1 calc R . . H49B H 0.0191 0.5371 0.1500 0.167 Uiso 1 1 calc R . . H49C H 0.1471 0.5326 0.2088 0.167 Uiso 1 1 calc R . . C50 C 0.1136(9) 0.6592(7) 0.1743(10) 0.105(6) Uiso 1 1 d D . . C51 C 0.2847(8) 0.6549(9) 0.1624(8) 0.079(4) Uiso 1 1 d D . . H51A H 0.2632 0.5874 0.1584 0.119 Uiso 1 1 calc R . . H51B H 0.3557 0.6740 0.2114 0.119 Uiso 1 1 calc R . . H51C H 0.2926 0.6669 0.1091 0.119 Uiso 1 1 calc R . . C52 C 0.2031(12) 0.8131(7) 0.1853(9) 0.089(5) Uiso 1 1 d D . . H52A H 0.1419 0.8314 0.1367 0.133 Uiso 1 1 calc R . . H52B H 0.2741 0.8408 0.1868 0.133 Uiso 1 1 calc R . . H52C H 0.1952 0.8361 0.2394 0.133 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 0.0464(3) 0.0392(3) 0.0396(3) -0.0023(2) 0.0086(2) -0.0002(2) Zn2 0.0390(5) 0.0366(6) 0.0310(5) 0.0000(4) 0.0098(4) 0.0003(5) Cl1 0.0361(10) 0.0465(13) 0.0299(10) 0.0062(9) 0.0165(8) 0.0079(10) Cl2 0.0355(11) 0.0317(11) 0.0271(10) 0.0025(9) 0.0060(9) 0.0016(9) N1 0.028(4) 0.036(4) 0.029(4) -0.005(3) 0.007(3) -0.014(3) N2 0.035(4) 0.024(4) 0.021(3) 0.000(3) 0.003(3) -0.002(3) N3 0.030(4) 0.036(4) 0.006(3) -0.002(3) -0.005(3) -0.004(3) N4 0.029(3) 0.035(4) 0.024(3) 0.005(3) 0.007(3) 0.005(3) N5 0.028(3) 0.026(4) 0.020(3) 0.004(3) 0.000(3) 0.005(3) N6 0.030(4) 0.028(4) 0.034(4) 0.000(3) -0.001(3) -0.008(3) N7 0.022(3) 0.021(3) 0.017(3) 0.003(3) 0.003(3) -0.002(3) C1 0.031(5) 0.048(5) 0.016(4) -0.010(4) 0.000(4) -0.008(4) C2 0.047(5) 0.020(4) 0.028(4) 0.000(3) 0.018(4) 0.004(4) C3 0.042(4) 0.032(4) 0.023(4) 0.003(3) 0.018(3) 0.014(4) C4 0.041(5) 0.046(5) 0.019(4) -0.005(4) 0.002(4) 0.010(4) C5 0.031(4) 0.038(5) 0.011(4) 0.003(3) -0.004(3) 0.003(4) C6 0.050(5) 0.023(4) 0.019(4) -0.008(3) 0.005(4) 0.000(4) C7 0.027(4) 0.055(6) 0.016(4) 0.015(4) -0.001(3) 0.016(4) C8 0.038(5) 0.040(5) 0.020(4) 0.004(4) 0.001(4) 0.013(4) C9 0.040(4) 0.025(4) 0.012(4) -0.009(3) -0.003(3) 0.015(4) C10 0.053(6) 0.030(5) 0.026(5) 0.005(4) -0.004(4) 0.000(5) C11 0.054(6) 0.039(5) 0.039(5) 0.002(4) 0.003(5) -0.007(5) C12 0.041(5) 0.044(6) 0.042(5) 0.005(4) 0.012(4) -0.003(5) C13 0.035(5) 0.039(5) 0.028(5) 0.004(4) -0.005(4) 0.002(4) C14 0.048(5) 0.020(4) 0.013(4) -0.005(3) -0.011(4) -0.004(4) C15 0.049(5) 0.025(4) 0.008(4) 0.000(3) 0.001(4) -0.006(4) C16 0.028(4) 0.040(5) 0.019(4) 0.002(4) 0.005(3) 0.001(4) C17 0.035(4) 0.039(5) 0.021(4) 0.000(4) 0.009(4) 0.002(4) C18 0.037(5) 0.027(4) 0.024(4) 0.006(3) 0.006(4) -0.003(4) C19 0.029(4) 0.036(5) 0.018(4) -0.010(3) 0.006(3) -0.007(4) C20 0.035(4) 0.032(5) 0.034(5) -0.006(4) 0.012(4) 0.004(4) C21 0.032(5) 0.055(6) 0.031(5) 0.000(4) 0.006(4) 0.001(5) C22 0.033(5) 0.062(7) 0.056(7) -0.005(5) 0.007(5) 0.003(5) C23 0.033(5) 0.054(6) 0.022(4) -0.009(4) 0.000(4) -0.005(5) C24 0.039(5) 0.027(4) 0.031(5) -0.005(4) 0.009(4) -0.012(4) C25 0.046(5) 0.024(4) 0.025(4) 0.005(3) 0.005(4) 0.000(4) C26 0.034(4) 0.029(4) 0.024(4) 0.002(4) 0.004(4) -0.005(4) C27 0.059(6) 0.028(5) 0.068(6) 0.007(4) 0.034(5) 0.000(5) C28 0.082(6) 0.046(6) 0.048(5) 0.010(4) 0.043(5) -0.018(5) C29 0.022(4) 0.035(5) 0.024(4) 0.010(4) -0.005(4) -0.009(4) C30 0.096(8) 0.024(5) 0.066(7) 0.004(5) 0.039(6) 0.000(5) C31 0.087(6) 0.027(5) 0.077(6) 0.004(5) 0.058(5) 0.001(5) C32 0.045(6) 0.030(5) 0.029(5) 0.011(4) -0.014(4) 0.008(4) C33 0.030(4) 0.031(4) 0.019(4) -0.001(3) 0.011(3) 0.004(4) C34 0.027(4) 0.026(4) 0.021(4) 0.004(3) 0.002(3) 0.002(4) C35 0.033(4) 0.020(4) 0.024(4) 0.012(3) 0.004(3) 0.007(3) C36 0.040(5) 0.019(4) 0.026(4) 0.000(3) -0.001(4) 0.008(4) C37 0.045(5) 0.034(5) 0.030(4) 0.001(4) 0.015(4) 0.010(4) C38 0.050(6) 0.023(4) 0.029(5) -0.008(4) -0.007(4) 0.002(4) C39 0.049(5) 0.027(4) 0.019(4) -0.006(4) 0.002(4) 0.001(4) C40 0.045(5) 0.032(5) 0.016(4) 0.001(4) -0.005(4) -0.001(4) C41 0.032(5) 0.037(5) 0.036(5) -0.003(4) 0.003(4) -0.008(4) C42 0.029(4) 0.027(4) 0.037(5) -0.002(4) 0.003(4) -0.008(4) C43 0.042(5) 0.036(5) 0.052(6) 0.002(5) 0.010(5) -0.010(5) C44 0.035(5) 0.048(6) 0.043(6) 0.012(5) -0.006(5) -0.014(5) C45 0.026(4) 0.038(5) 0.036(5) -0.003(4) 0.004(4) 0.007(4) C46 0.031(4) 0.034(5) 0.040(5) -0.007(4) 0.015(4) -0.005(4) C47 0.034(5) 0.031(5) 0.033(5) 0.003(4) 0.006(4) -0.005(4) C48 0.038(4) 0.058(6) 0.035(5) 0.010(4) 0.022(4) 0.019(4) O1 0.060(4) 0.053(4) 0.032(3) -0.006(3) 0.011(3) 0.011(4) O2 0.051(3) 0.029(3) 0.057(4) -0.002(3) 0.028(3) 0.008(3) O3 0.046(3) 0.027(3) 0.052(3) -0.003(3) 0.030(3) 0.000(3) O4 0.038(3) 0.035(3) 0.043(3) -0.013(3) 0.023(3) -0.008(3) O5 0.031(3) 0.039(4) 0.048(4) 0.000(3) -0.002(3) -0.017(3) O6 0.018(3) 0.070(5) 0.038(4) -0.001(3) -0.001(3) -0.001(3) O7 0.048(3) 0.044(4) 0.036(3) 0.003(3) 0.021(3) -0.001(3) O8 0.058(5) 0.043(4) 0.059(5) 0.011(4) 0.000(4) 0.004(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 O1 2.302(6) . ? Eu1 O2 2.328(6) 2_645 ? Eu1 O4 2.432(6) . ? Eu1 O7 2.456(7) . ? Eu1 O3 2.468(6) . ? Eu1 O6 2.478(6) 1_444 ? Eu1 O5 2.483(7) 1_444 ? Eu1 Cl2 2.753(3) . ? Eu1 C32 2.815(9) . ? Eu1 C48 2.827(8) 1_444 ? Zn2 N3 2.033(6) . ? Zn2 N1 2.054(8) . ? Zn2 N5 2.055(6) . ? Zn2 Cl1 2.279(3) . ? Zn2 N7 2.435(7) . ? N1 C15 1.297(13) . ? N1 C14 1.370(12) . ? N2 C15 1.357(11) . ? N2 C9 1.411(13) . ? N2 C8 1.461(12) . ? N3 C18 1.311(13) . ? N3 C19 1.434(11) . ? N4 C18 1.339(10) . ? N4 C24 1.415(12) . ? N4 C25 1.459(12) . ? N5 C34 1.312(12) . ? N5 C35 1.427(10) . ? N6 C40 1.362(13) . ? N6 C34 1.377(10) . ? N6 C41 1.499(13) . ? N7 C33 1.461(10) . ? N7 C16 1.479(11) . ? N7 C17 1.490(10) . ? C1 O1 1.238(10) . ? C1 O2 1.252(12) . ? C1 C2 1.516(12) . ? C2 C3 1.375(11) . ? C2 C7 1.388(13) . ? C3 C4 1.375(12) . ? C4 C5 1.419(13) . ? C5 C6 1.394(11) . ? C5 C8 1.483(12) . ? C6 C7 1.356(12) . ? C9 C10 1.375(13) . ? C9 C14 1.392(13) . ? C10 C11 1.371(16) . ? C11 C12 1.427(15) . ? C12 C13 1.370(14) . ? C13 C14 1.426(15) . ? C15 C16 1.537(13) . ? C17 C18 1.494(13) . ? C19 C20 1.371(14) . ? C19 C24 1.406(13) . ? C20 C21 1.391(12) . ? C21 C22 1.400(15) . ? C22 C23 1.382(16) . ? C23 C24 1.378(12) . ? C25 C26 1.548(12) . ? C26 C31 1.356(16) . ? C26 C27 1.362(15) . ? C27 C28 1.370(15) . ? C28 C29 1.344(15) . ? C29 C30 1.356(15) . ? C29 C32 1.540(13) . ? C30 C31 1.397(14) . ? C32 O4 1.264(12) . ? C32 O3 1.294(14) . ? C33 C34 1.465(12) . ? C35 C36 1.368(14) . ? C35 C40 1.379(13) . ? C36 C37 1.410(11) . ? C37 C38 1.401(14) . ? C38 C39 1.375(16) . ? C39 C40 1.402(11) . ? C41 C42 1.521(11) . ? C42 C43 1.365(14) . ? C42 C47 1.401(13) . ? C43 C44 1.408(13) . ? C44 C45 1.379(14) . ? C45 C46 1.389(14) . ? C45 C48 1.511(11) . ? C46 C47 1.391(11) . ? C48 O5 1.216(12) . ? C48 O6 1.278(13) . ? C48 Eu1 2.827(8) 1_666 ? O2 Eu1 2.328(6) 2_645 ? O5 Eu1 2.483(7) 1_666 ? O6 Eu1 2.478(6) 1_666 ? N9 C54 1.340(8) . ? N9 C55 1.456(8) . ? N9 C56 1.462(8) . ? O11 C54 1.440(16) . ? C53 C54 1.425(8) . ? N8 C50 1.297(13) . ? N8 C51 1.452(13) . ? N8 C52 1.477(12) . ? O10 C50 1.425(14) . ? C49 C50 1.437(13) . ? 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 O1 Eu1 O2 102.9(2) . 2_645 ? O1 Eu1 O4 84.7(2) . . ? O2 Eu1 O4 152.1(2) 2_645 . ? O1 Eu1 O7 73.6(2) . . ? O2 Eu1 O7 73.8(2) 2_645 . ? O4 Eu1 O7 83.0(2) . . ? O1 Eu1 O3 83.8(2) . . ? O2 Eu1 O3 152.6(3) 2_645 . ? O4 Eu1 O3 53.9(2) . . ? O7 Eu1 O3 133.1(2) . . ? O1 Eu1 O6 144.7(3) . 1_444 ? O2 Eu1 O6 72.8(2) 2_645 1_444 ? O4 Eu1 O6 85.5(2) . 1_444 ? O7 Eu1 O6 71.6(2) . 1_444 ? O3 Eu1 O6 116.5(2) . 1_444 ? O1 Eu1 O5 160.1(2) . 1_444 ? O2 Eu1 O5 92.4(2) 2_645 1_444 ? O4 Eu1 O5 87.8(2) . 1_444 ? O7 Eu1 O5 123.7(2) . 1_444 ? O3 Eu1 O5 76.9(2) . 1_444 ? O6 Eu1 O5 52.3(2) 1_444 1_444 ? O1 Eu1 Cl2 83.9(2) . . ? O2 Eu1 Cl2 75.35(19) 2_645 . ? O4 Eu1 Cl2 132.49(16) . . ? O7 Eu1 Cl2 136.14(17) . . ? O3 Eu1 Cl2 79.05(17) . . ? O6 Eu1 Cl2 126.35(18) 1_444 . ? O5 Eu1 Cl2 87.74(18) 1_444 . ? O1 Eu1 C32 82.3(2) . . ? O2 Eu1 C32 174.8(2) 2_645 . ? O4 Eu1 C32 26.6(3) . . ? O7 Eu1 C32 107.6(3) . . ? O3 Eu1 C32 27.4(3) . . ? O6 Eu1 C32 102.7(3) 1_444 . ? O5 Eu1 C32 82.7(2) 1_444 . ? Cl2 Eu1 C32 106.0(2) . . ? O1 Eu1 C48 168.8(3) . 1_444 ? O2 Eu1 C48 81.9(3) 2_645 1_444 ? O4 Eu1 C48 86.6(2) . 1_444 ? O7 Eu1 C48 98.4(3) . 1_444 ? O3 Eu1 C48 96.7(3) . 1_444 ? O6 Eu1 C48 26.9(3) 1_444 1_444 ? O5 Eu1 C48 25.4(3) 1_444 1_444 ? Cl2 Eu1 C48 107.2(2) . 1_444 ? C32 Eu1 C48 92.9(3) . 1_444 ? N3 Zn2 N1 106.1(3) . . ? N3 Zn2 N5 117.9(3) . . ? N1 Zn2 N5 113.3(3) . . ? N3 Zn2 Cl1 108.1(2) . . ? N1 Zn2 Cl1 104.1(2) . . ? N5 Zn2 Cl1 106.4(2) . . ? N3 Zn2 N7 74.3(3) . . ? N1 Zn2 N7 74.1(3) . . ? N5 Zn2 N7 72.9(3) . . ? Cl1 Zn2 N7 177.39(17) . . ? C15 N1 C14 106.0(8) . . ? C15 N1 Zn2 117.6(6) . . ? C14 N1 Zn2 135.3(7) . . ? C15 N2 C9 105.4(8) . . ? C15 N2 C8 129.9(8) . . ? C9 N2 C8 124.7(7) . . ? C18 N3 C19 106.5(7) . . ? C18 N3 Zn2 120.2(6) . . ? C19 N3 Zn2 132.9(6) . . ? C18 N4 C24 107.6(8) . . ? C18 N4 C25 127.0(8) . . ? C24 N4 C25 125.3(7) . . ? C34 N5 C35 107.1(7) . . ? C34 N5 Zn2 119.0(5) . . ? C35 N5 Zn2 132.9(6) . . ? C40 N6 C34 109.2(8) . . ? C40 N6 C41 126.2(7) . . ? C34 N6 C41 124.3(8) . . ? C33 N7 C16 111.4(6) . . ? C33 N7 C17 113.5(7) . . ? C16 N7 C17 111.6(6) . . ? C33 N7 Zn2 106.5(5) . . ? C16 N7 Zn2 106.3(5) . . ? C17 N7 Zn2 107.0(5) . . ? O1 C1 O2 124.3(8) . . ? O1 C1 C2 118.9(9) . . ? O2 C1 C2 116.7(7) . . ? C3 C2 C7 119.0(8) . . ? C3 C2 C1 119.4(8) . . ? C7 C2 C1 121.6(7) . . ? C4 C3 C2 121.6(9) . . ? C3 C4 C5 119.6(8) . . ? C6 C5 C4 117.3(8) . . ? C6 C5 C8 124.0(8) . . ? C4 C5 C8 118.5(7) . . ? C7 C6 C5 122.1(9) . . ? C6 C7 C2 120.3(8) . . ? N2 C8 C5 111.7(7) . . ? C10 C9 C14 123.7(10) . . ? C10 C9 N2 131.3(9) . . ? C14 C9 N2 105.0(8) . . ? C11 C10 C9 117.6(10) . . ? C10 C11 C12 120.8(10) . . ? C13 C12 C11 121.2(10) . . ? C12 C13 C14 118.1(9) . . ? N1 C14 C9 109.8(9) . . ? N1 C14 C13 131.5(9) . . ? C9 C14 C13 118.6(8) . . ? N1 C15 N2 113.8(8) . . ? N1 C15 C16 124.4(8) . . ? N2 C15 C16 121.8(9) . . ? N7 C16 C15 106.0(7) . . ? N7 C17 C18 107.7(7) . . ? N3 C18 N4 113.1(8) . . ? N3 C18 C17 123.6(7) . . ? N4 C18 C17 123.2(9) . . ? C20 C19 C24 120.8(8) . . ? C20 C19 N3 132.0(8) . . ? C24 C19 N3 107.2(8) . . ? C19 C20 C21 118.1(9) . . ? C20 C21 C22 119.7(10) . . ? C23 C22 C21 123.3(9) . . ? C24 C23 C22 115.6(9) . . ? C23 C24 C19 122.4(10) . . ? C23 C24 N4 131.9(9) . . ? C19 C24 N4 105.6(7) . . ? N4 C25 C26 114.5(8) . . ? C31 C26 C27 117.1(9) . . ? C31 C26 C25 118.6(9) . . ? C27 C26 C25 124.2(9) . . ? C26 C27 C28 123.7(11) . . ? C29 C28 C27 118.1(10) . . ? C28 C29 C30 120.6(10) . . ? C28 C29 C32 119.8(9) . . ? C30 C29 C32 119.5(10) . . ? C29 C30 C31 120.1(12) . . ? C26 C31 C30 120.2(11) . . ? O4 C32 O3 120.6(8) . . ? O4 C32 C29 121.0(10) . . ? O3 C32 C29 118.5(9) . . ? O4 C32 Eu1 59.5(5) . . ? O3 C32 Eu1 61.2(5) . . ? C29 C32 Eu1 175.9(6) . . ? N7 C33 C34 107.6(7) . . ? N5 C34 N6 109.6(8) . . ? N5 C34 C33 123.6(7) . . ? N6 C34 C33 126.8(9) . . ? C36 C35 C40 122.8(8) . . ? C36 C35 N5 129.3(8) . . ? C40 C35 N5 107.6(8) . . ? C35 C36 C37 116.9(9) . . ? C38 C37 C36 120.0(10) . . ? C39 C38 C37 122.3(8) . . ? C38 C39 C40 116.9(9) . . ? N6 C40 C35 106.4(7) . . ? N6 C40 C39 132.7(9) . . ? C35 C40 C39 120.8(10) . . ? N6 C41 C42 112.0(8) . . ? C43 C42 C47 121.0(8) . . ? C43 C42 C41 122.2(8) . . ? C47 C42 C41 116.8(8) . . ? C42 C43 C44 118.7(9) . . ? C45 C44 C43 121.1(10) . . ? C44 C45 C46 119.0(8) . . ? C44 C45 C48 122.4(9) . . ? C46 C45 C48 118.6(8) . . ? C45 C46 C47 120.6(9) . . ? C46 C47 C42 119.1(9) . . ? O5 C48 O6 122.4(8) . . ? O5 C48 C45 124.0(9) . . ? O6 C48 C45 113.6(9) . . ? O5 C48 Eu1 61.2(5) . 1_666 ? O6 C48 Eu1 61.2(4) . 1_666 ? C45 C48 Eu1 174.8(8) . 1_666 ? C1 O1 Eu1 166.2(7) . . ? C1 O2 Eu1 144.3(5) . 2_645 ? C32 O3 Eu1 91.4(5) . . ? C32 O4 Eu1 93.8(6) . . ? C48 O5 Eu1 93.3(6) . 1_666 ? C48 O6 Eu1 92.0(5) . 1_666 ? C54 N9 C55 116.0(10) . . ? C54 N9 C56 118.9(9) . . ? C55 N9 C56 125.1(11) . . ? N9 C54 C53 127.5(12) . . ? N9 C54 O11 109.6(9) . . ? C53 C54 O11 122.7(13) . . ? C50 N8 C51 115.3(10) . . ? C50 N8 C52 118.9(11) . . ? C51 N8 C52 125.8(11) . . ? N8 C50 O10 110.3(9) . . ? N8 C50 C49 124.9(12) . . ? O10 C50 C49 124.7(12) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 24.23 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.935 _refine_diff_density_min -2.998 _refine_diff_density_rms 0.247