# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Yan Xu' _publ_contact_author_email YANXU@NJUT.EDU.CN _publ_section_title ; (C2H8N)9[Eu5(SO4)12]*2H2O: The first Europium Sulfate Open-framework Containing Two Kinds of Intersecting Extra-large 20-Membered Ring Channels ; loop_ _publ_author_name 'Yan Xu.' 'S. P. Elangovan' 'Xiaoliang Zhang.' 'Zhibin Zhang.' 'Lei Zheng.' ; Dunru Zhu ; # Attachment 'ZXL3.CIF' data_zxl3 _database_code_depnum_ccdc_archive 'CCDC 735455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C2 N H8)9 Eu5 (SO4)12] (H2O)2' _chemical_formula_sum 'C18 H76 Eu5 N9 O50 S12' _chemical_formula_weight 2363.40 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.5650(18) _cell_length_b 35.458(3) _cell_length_c 10.1333(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.9780(10) _cell_angle_gamma 90.00 _cell_volume 6698.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 65 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.50 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4616 _exptl_absorpt_coefficient_mu 5.102 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.5568 _exptl_absorpt_correction_T_max 0.5796 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _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 'Bruker Apex2 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 14002 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6447 _reflns_number_gt 5572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0913P)^2^+40.7210P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6447 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1481 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _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 0.0000 0.220318(17) 0.2500 0.01794(17) Uani 1 2 d S . . Eu2 Eu 0.24218(2) 0.192395(11) 0.49088(5) 0.01631(15) Uani 1 1 d . . . Eu3 Eu 0.36345(2) 0.031173(13) 0.52139(5) 0.02224(16) Uani 1 1 d . . . S1 S 0.13253(10) 0.26800(6) 0.5547(2) 0.0172(4) Uani 1 1 d . . . S2 S 0.29234(11) 0.11049(6) 0.4836(2) 0.0213(5) Uani 1 1 d . . . S3 S 0.15589(10) 0.25279(6) 0.1800(2) 0.0165(4) Uani 1 1 d . . . S4 S 0.44193(11) 0.03548(6) 0.8610(2) 0.0202(5) Uani 1 1 d . . . S5 S 0.09422(12) 0.15771(6) 0.4609(3) 0.0247(5) Uani 1 1 d . . . S6 S 0.24758(14) -0.02691(7) 0.6286(3) 0.0307(6) Uani 1 1 d . . . O20 O 0.0799(5) 0.1177(2) 0.4366(10) 0.051(2) Uani 1 1 d . . . O21 O 0.2301(6) -0.0658(3) 0.6004(11) 0.067(3) Uani 1 1 d . . . O22 O 0.2911(5) -0.0210(3) 0.7812(9) 0.051(2) Uani 1 1 d . . . O23 O 0.2876(4) -0.0134(2) 0.5460(8) 0.0365(17) Uani 1 1 d . . . O24 O 0.1818(5) -0.0052(3) 0.5846(13) 0.075(3) Uani 1 1 d . . . N1 N 0.5000 -0.0658(3) 0.7500 0.030(3) Uani 1 2 d S . . H1D H 0.4912 -0.0508 0.6726 0.036 Uiso 1 1 d R . . N2 N 0.2305(5) 0.3075(2) -0.0654(9) 0.0289(19) Uani 1 1 d . . . H2D H 0.2482 0.3005 -0.1290 0.035 Uiso 1 1 calc R . . H2E H 0.2048 0.2880 -0.0555 0.035 Uiso 1 1 calc R . . N3 N 0.1121(11) 0.0938(6) 0.1866(17) 0.123(8) Uani 1 1 d . . . H3D H 0.1071 0.1106 0.2480 0.148 Uiso 1 1 calc R . . H3E H 0.1595 0.0916 0.2119 0.148 Uiso 1 1 calc R . . N4 N -0.0041(11) 0.2433(7) 0.676(2) 0.055(6) Uani 0.50 1 d P . . H4D H -0.0460 0.2428 0.5958 0.066 Uiso 0.50 1 d PR . . H4E H 0.0312 0.2428 0.6457 0.066 Uiso 0.50 1 d PR . . N5 N 0.2039(16) -0.0671(6) 0.210(3) 0.173(13) Uani 1 1 d . . . H5D H 0.1956 -0.0767 0.1224 0.207 Uiso 1 1 calc R . . H5E H 0.2217 -0.0437 0.2153 0.207 Uiso 1 1 calc R . . N6 N 0.5000 0.1301(5) 0.7500 0.105(8) Uani 1 2 d S . . H6B H 0.4635 0.1151 0.6941 0.126 Uiso 1 1 d R . . C1 C 0.5642(8) -0.0876(5) 0.7788(19) 0.072(5) Uani 1 1 d . . . H1A H 0.6035 -0.0708 0.7952 0.109 Uiso 1 1 calc R . . H1B H 0.5564 -0.1034 0.6966 0.109 Uiso 1 1 calc R . . H1C H 0.5752 -0.1029 0.8636 0.109 Uiso 1 1 calc R . . C2 C 0.1827(7) 0.3398(4) -0.1252(14) 0.055(4) Uani 1 1 d . . . H2A H 0.1449 0.3330 -0.2174 0.082 Uiso 1 1 calc R . . H2B H 0.2095 0.3605 -0.1382 0.082 Uiso 1 1 calc R . . H2C H 0.1624 0.3470 -0.0593 0.082 Uiso 1 1 calc R . . C3 C 0.2913(7) 0.3152(3) 0.0782(14) 0.053(4) Uani 1 1 d . . . H3A H 0.3203 0.2930 0.1118 0.079 Uiso 1 1 calc R . . H3B H 0.2729 0.3223 0.1473 0.079 Uiso 1 1 calc R . . H3C H 0.3200 0.3354 0.0680 0.079 Uiso 1 1 calc R . . C4 C 0.0821(11) 0.1100(7) 0.049(3) 0.128(9) Uani 1 1 d . . . H4A H 0.1041 0.1340 0.0513 0.192 Uiso 1 1 calc R . . H4B H 0.0315 0.1133 0.0184 0.192 Uiso 1 1 calc R . . H4C H 0.0899 0.0937 -0.0192 0.192 Uiso 1 1 calc R . . C5 C 0.0888(13) 0.0588(7) 0.216(3) 0.127(10) Uani 1 1 d . . . H5A H 0.1154 0.0528 0.3172 0.191 Uiso 1 1 calc R . . H5B H 0.0966 0.0396 0.1575 0.191 Uiso 1 1 calc R . . H5C H 0.0386 0.0602 0.1937 0.191 Uiso 1 1 calc R . . C6 C 0.0000 0.2120(8) 0.7500 0.081(7) Uani 1 2 d S . . H6A H -0.0027 0.1902 0.6915 0.122 Uiso 0.50 1 d PR . . H6C H 0.0445 0.2116 0.8358 0.122 Uiso 0.50 1 d PR . . H6D H -0.0393 0.2116 0.7776 0.122 Uiso 0.50 1 d PR . . C7 C 0.0000 0.2800(6) 0.7500 0.057(5) Uani 1 2 d S . . H7A H -0.0030 0.3004 0.6855 0.085 Uiso 0.50 1 d PR . . H7B H -0.0393 0.2816 0.7773 0.085 Uiso 0.50 1 d PR . . H7C H 0.0445 0.2816 0.8356 0.085 Uiso 0.50 1 d PR . . C8 C 0.4764(10) 0.1521(5) 0.843(3) 0.100(7) Uani 1 1 d . . . H8A H 0.4625 0.1354 0.9014 0.150 Uiso 1 1 calc R . . H8B H 0.4362 0.1675 0.7842 0.150 Uiso 1 1 calc R . . H8C H 0.5150 0.1680 0.9060 0.150 Uiso 1 1 calc R . . C9 C 0.1320(11) -0.0646(6) 0.224(2) 0.118(9) Uani 1 1 d . . . H9A H 0.0987 -0.0496 0.1458 0.177 Uiso 1 1 calc R . . H9B H 0.1399 -0.0531 0.3154 0.177 Uiso 1 1 calc R . . H9C H 0.1127 -0.0894 0.2196 0.177 Uiso 1 1 calc R . . C10 C 0.2545(8) -0.0891(5) 0.3159(18) 0.066(4) Uani 1 1 d . . . H10A H 0.2975 -0.0897 0.3005 0.099 Uiso 1 1 calc R . . H10B H 0.2363 -0.1142 0.3106 0.099 Uiso 1 1 calc R . . H10C H 0.2651 -0.0786 0.4101 0.099 Uiso 1 1 calc R . . O1 O 0.0336(4) 0.1788(2) 0.4658(8) 0.0345(17) Uani 1 1 d . . . O2 O 0.2017(3) 0.21887(16) 0.2527(7) 0.0184(13) Uani 1 1 d . . . O3 O 0.1850(3) 0.24742(16) 0.5122(7) 0.0201(13) Uani 1 1 d . . . O4 O 0.1512(3) 0.30778(16) 0.5533(7) 0.0229(14) Uani 1 1 d . . . O5 O 0.3993(4) 0.06487(18) 0.7572(7) 0.0280(15) Uani 1 1 d . . . O6 O 0.0593(3) 0.26133(19) 0.4429(7) 0.0274(15) Uani 1 1 d . . . O7 O 0.1632(3) 0.1640(2) 0.5894(7) 0.0300(16) Uani 1 1 d . . . O8 O 0.0833(3) 0.24678(18) 0.1699(7) 0.0258(15) Uani 1 1 d . . . O9 O 0.1055(3) 0.17600(18) 0.3367(7) 0.0274(15) Uani 1 1 d . . . O10 O 0.1874(3) 0.28703(18) 0.2657(7) 0.0250(15) Uani 1 1 d . . . O11 O 0.1389(4) 0.2561(2) 0.6968(8) 0.0312(16) Uani 1 1 d . . . O12 O 0.1526(3) 0.25672(19) 0.0353(7) 0.0256(15) Uani 1 1 d . . . O13 O 0.5165(3) 0.0490(2) 0.9400(7) 0.0307(16) Uani 1 1 d . . . O14 O 0.4147(4) 0.0269(2) 0.9697(7) 0.0301(16) Uani 1 1 d . . . O15 O 0.2608(3) 0.07430(19) 0.4988(8) 0.0300(16) Uani 1 1 d . . . O16 O 0.2409(4) 0.13220(18) 0.3584(7) 0.0298(16) Uani 1 1 d . . . O17 O 0.3083(3) 0.13501(17) 0.6101(7) 0.0239(14) Uani 1 1 d . . . O18 O 0.3580(3) 0.10007(18) 0.4693(8) 0.0309(16) Uani 1 1 d . . . O19 O 0.4362(4) 0.00267(18) 0.7691(8) 0.0311(16) Uani 1 1 d . . . O1W O 0.0329(6) -0.0086(4) 0.4026(13) 0.095(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0117(3) 0.0220(3) 0.0181(3) 0.000 0.0044(2) 0.000 Eu2 0.0146(2) 0.0155(2) 0.0168(2) 0.00001(15) 0.00463(18) 0.00114(15) Eu3 0.0191(2) 0.0209(3) 0.0243(3) -0.00363(17) 0.0069(2) 0.00301(16) S1 0.0122(9) 0.0202(10) 0.0190(11) -0.0039(8) 0.0063(8) -0.0012(8) S2 0.0199(10) 0.0160(10) 0.0241(12) 0.0003(8) 0.0055(9) 0.0036(8) S3 0.0116(9) 0.0220(10) 0.0144(10) -0.0002(8) 0.0041(8) 0.0004(8) S4 0.0169(10) 0.0257(11) 0.0173(11) 0.0041(8) 0.0066(9) -0.0013(8) S5 0.0224(11) 0.0237(11) 0.0243(12) 0.0051(9) 0.0063(9) -0.0034(9) S6 0.0345(13) 0.0328(13) 0.0260(13) -0.0024(10) 0.0141(11) -0.0070(10) O20 0.055(5) 0.017(4) 0.070(6) 0.004(4) 0.014(5) -0.001(3) O21 0.093(8) 0.052(6) 0.062(6) -0.022(5) 0.040(6) -0.041(5) O22 0.062(6) 0.063(5) 0.028(4) 0.006(4) 0.020(4) -0.023(4) O23 0.037(4) 0.045(4) 0.029(4) 0.004(3) 0.015(3) -0.006(3) O24 0.047(6) 0.100(8) 0.087(8) 0.011(7) 0.036(6) 0.016(5) N1 0.041(7) 0.027(6) 0.023(6) 0.000 0.015(5) 0.000 N2 0.037(5) 0.030(5) 0.023(4) -0.008(3) 0.016(4) -0.002(3) N3 0.146(17) 0.150(16) 0.066(10) -0.052(11) 0.038(11) -0.101(14) N4 0.026(10) 0.090(17) 0.034(11) -0.003(11) -0.002(9) 0.007(10) N5 0.32(3) 0.127(16) 0.18(2) 0.094(16) 0.21(3) 0.11(2) N6 0.097(17) 0.041(11) 0.17(3) 0.000 0.051(17) 0.000 C1 0.058(9) 0.076(10) 0.085(12) 0.015(9) 0.032(9) 0.028(8) C2 0.053(8) 0.052(7) 0.038(7) -0.014(6) -0.001(6) 0.018(6) C3 0.057(8) 0.041(6) 0.039(7) -0.011(5) 0.001(6) 0.008(6) C4 0.082(14) 0.125(19) 0.16(2) -0.007(17) 0.030(15) 0.055(14) C5 0.122(19) 0.14(2) 0.16(2) -0.084(18) 0.103(19) -0.046(16) C6 0.060(14) 0.080(17) 0.09(2) 0.000 0.021(14) 0.000 C7 0.027(8) 0.101(16) 0.042(11) 0.000 0.014(8) 0.000 C8 0.068(11) 0.063(11) 0.15(2) -0.023(12) 0.028(12) -0.013(9) C9 0.091(15) 0.118(17) 0.089(14) -0.036(13) -0.018(12) 0.041(13) C10 0.068(10) 0.069(10) 0.077(11) -0.031(9) 0.046(9) -0.015(8) O1 0.023(3) 0.047(4) 0.037(4) 0.005(3) 0.015(3) 0.004(3) O2 0.015(3) 0.020(3) 0.022(3) 0.002(2) 0.010(3) 0.002(2) O3 0.015(3) 0.023(3) 0.025(3) 0.002(2) 0.011(3) 0.004(2) O4 0.022(3) 0.017(3) 0.034(4) -0.004(3) 0.016(3) 0.000(2) O5 0.031(4) 0.028(3) 0.025(4) 0.000(3) 0.011(3) 0.010(3) O6 0.014(3) 0.034(4) 0.028(4) -0.005(3) 0.002(3) -0.001(3) O7 0.022(3) 0.044(4) 0.022(4) 0.007(3) 0.007(3) 0.002(3) O8 0.009(3) 0.038(4) 0.026(4) 0.006(3) 0.003(3) 0.002(2) O9 0.025(3) 0.025(3) 0.027(4) 0.006(3) 0.007(3) -0.001(3) O10 0.022(3) 0.025(3) 0.021(3) 0.001(3) 0.003(3) 0.001(3) O11 0.029(4) 0.039(4) 0.028(4) -0.005(3) 0.013(3) -0.002(3) O12 0.024(3) 0.034(4) 0.015(3) 0.002(3) 0.005(3) -0.001(3) O13 0.016(3) 0.039(4) 0.030(4) 0.004(3) 0.003(3) -0.010(3) O14 0.031(4) 0.042(4) 0.022(4) 0.003(3) 0.016(3) -0.011(3) O15 0.028(4) 0.023(3) 0.041(4) 0.003(3) 0.017(3) -0.002(3) O16 0.029(3) 0.025(3) 0.024(4) -0.001(3) 0.001(3) 0.005(3) O17 0.031(3) 0.019(3) 0.016(3) 0.001(2) 0.004(3) 0.006(3) O18 0.026(3) 0.025(3) 0.042(4) 0.001(3) 0.014(3) 0.003(3) O19 0.034(4) 0.026(3) 0.029(4) -0.003(3) 0.009(3) 0.004(3) O1W 0.075(8) 0.148(12) 0.066(7) 0.026(8) 0.036(7) 0.027(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.326(6) . ? Eu1 O6 2.326(6) 2 ? Eu1 O8 2.376(7) 2 ? Eu1 O8 2.376(7) . ? Eu1 O1 2.481(7) 2 ? Eu1 O1 2.481(7) . ? Eu1 O9 2.518(6) 2 ? Eu1 O9 2.518(6) . ? Eu1 S5 3.123(2) 2 ? Eu1 S5 3.123(2) . ? Eu2 O3 2.335(6) . ? Eu2 O10 2.387(6) 7_556 ? Eu2 O2 2.388(6) . ? Eu2 O4 2.417(6) 7_556 ? Eu2 O7 2.453(7) . ? Eu2 O17 2.462(6) . ? Eu2 O16 2.515(7) . ? Eu2 O3 2.615(6) 7_556 ? Eu2 O9 2.640(6) . ? Eu2 S2 3.093(2) . ? Eu2 S1 3.135(2) 7_556 ? Eu2 S5 3.175(2) . ? Eu3 O22 2.282(8) 6 ? Eu3 O23 2.308(7) . ? Eu3 O13 2.415(7) 2_656 ? Eu3 O14 2.469(7) 6 ? Eu3 O5 2.489(7) . ? Eu3 O18 2.492(7) . ? Eu3 O19 2.528(7) . ? Eu3 O15 2.538(7) . ? Eu3 S2 3.118(2) . ? Eu3 S4 3.127(2) . ? S1 O11 1.453(8) . ? S1 O4 1.463(6) . ? S1 O6 1.472(6) . ? S1 O3 1.507(6) . ? S1 Eu2 3.135(2) 7_556 ? S2 O18 1.465(7) . ? S2 O17 1.468(6) . ? S2 O15 1.475(7) . ? S2 O16 1.479(6) . ? S3 O12 1.446(7) . ? S3 O8 1.468(6) . ? S3 O10 1.474(6) . ? S3 O2 1.513(6) . ? S4 O14 1.463(7) . ? S4 O19 1.463(7) . ? S4 O5 1.477(7) . ? S4 O13 1.479(6) . ? S5 O20 1.450(7) . ? S5 O1 1.473(7) . ? S5 O7 1.483(7) . ? S5 O9 1.519(7) . ? S6 O21 1.423(9) . ? S6 O22 1.438(8) . ? S6 O24 1.454(10) . ? S6 O23 1.479(8) . ? O22 Eu3 2.282(8) 6_556 ? N1 C1 1.450(14) 2_656 ? N1 C1 1.450(14) . ? N1 H1D 0.9002 . ? N2 C2 1.462(14) . ? N2 C3 1.490(14) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? N3 C4 1.39(3) . ? N3 C5 1.40(3) . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 C6 1.32(3) . ? N4 N4 1.44(4) 2_556 ? N4 C7 1.49(3) . ? N4 H4D 0.9000 . ? N4 H4E 0.9000 . ? N5 C10 1.38(3) . ? N5 C9 1.55(3) . ? N5 H5D 0.9000 . ? N5 H5E 0.9000 . ? N6 C8 1.46(2) . ? N6 C8 1.46(2) 2_656 ? N6 H6B 0.8999 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N4 1.32(3) 2_556 ? C6 H6A 0.9601 . ? C6 H6C 0.9600 . ? C6 H6D 0.9599 . ? C7 N4 1.49(3) 2_556 ? C7 H7A 0.9601 . ? C7 H7B 0.9601 . ? C7 H7C 0.9601 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O3 Eu2 2.615(6) 7_556 ? O4 Eu2 2.417(6) 7_556 ? O10 Eu2 2.387(6) 7_556 ? O13 Eu3 2.415(7) 2_656 ? O14 Eu3 2.469(7) 6_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O6 102.6(3) . 2 ? O6 Eu1 O8 70.4(2) . 2 ? O6 Eu1 O8 80.9(2) 2 2 ? O6 Eu1 O8 80.9(2) . . ? O6 Eu1 O8 70.4(2) 2 . ? O8 Eu1 O8 133.5(3) 2 . ? O6 Eu1 O1 164.6(2) . 2 ? O6 Eu1 O1 77.2(2) 2 2 ? O8 Eu1 O1 124.3(2) 2 2 ? O8 Eu1 O1 84.6(2) . 2 ? O6 Eu1 O1 77.2(2) . . ? O6 Eu1 O1 164.6(2) 2 . ? O8 Eu1 O1 84.6(2) 2 . ? O8 Eu1 O1 124.3(2) . . ? O1 Eu1 O1 107.2(4) 2 . ? O6 Eu1 O9 138.8(2) . 2 ? O6 Eu1 O9 91.6(2) 2 2 ? O8 Eu1 O9 74.1(2) 2 2 ? O8 Eu1 O9 140.1(2) . 2 ? O1 Eu1 O9 56.2(2) 2 2 ? O1 Eu1 O9 79.3(2) . 2 ? O6 Eu1 O9 91.6(2) . . ? O6 Eu1 O9 138.8(2) 2 . ? O8 Eu1 O9 140.1(2) 2 . ? O8 Eu1 O9 74.1(2) . . ? O1 Eu1 O9 79.3(2) 2 . ? O1 Eu1 O9 56.2(2) . . ? O9 Eu1 O9 102.8(3) 2 . ? O6 Eu1 S5 166.72(18) . 2 ? O6 Eu1 S5 85.16(17) 2 2 ? O8 Eu1 S5 100.72(15) 2 2 ? O8 Eu1 S5 112.04(17) . 2 ? O1 Eu1 S5 27.54(17) 2 2 ? O1 Eu1 S5 92.45(18) . 2 ? O9 Eu1 S5 28.77(16) 2 2 ? O9 Eu1 S5 89.39(15) . 2 ? O6 Eu1 S5 85.16(17) . . ? O6 Eu1 S5 166.72(18) 2 . ? O8 Eu1 S5 112.04(17) 2 . ? O8 Eu1 S5 100.72(15) . . ? O1 Eu1 S5 92.45(18) 2 . ? O1 Eu1 S5 27.54(17) . . ? O9 Eu1 S5 89.39(15) 2 . ? O9 Eu1 S5 28.77(16) . . ? S5 Eu1 S5 89.40(9) 2 . ? O3 Eu2 O10 76.0(2) . 7_556 ? O3 Eu2 O2 77.9(2) . . ? O10 Eu2 O2 136.5(2) 7_556 . ? O3 Eu2 O4 123.5(2) . 7_556 ? O10 Eu2 O4 89.5(2) 7_556 7_556 ? O2 Eu2 O4 76.7(2) . 7_556 ? O3 Eu2 O7 81.9(2) . . ? O10 Eu2 O7 85.5(2) 7_556 . ? O2 Eu2 O7 124.4(2) . . ? O4 Eu2 O7 152.0(2) 7_556 . ? O3 Eu2 O17 147.2(2) . . ? O10 Eu2 O17 77.1(2) 7_556 . ? O2 Eu2 O17 134.9(2) . . ? O4 Eu2 O17 74.5(2) 7_556 . ? O7 Eu2 O17 77.5(2) . . ? O3 Eu2 O16 150.0(2) . . ? O10 Eu2 O16 132.5(2) 7_556 . ? O2 Eu2 O16 82.7(2) . . ? O4 Eu2 O16 72.8(2) 7_556 . ? O7 Eu2 O16 90.5(2) . . ? O17 Eu2 O16 55.9(2) . . ? O3 Eu2 O3 68.5(2) . 7_556 ? O10 Eu2 O3 70.3(2) 7_556 7_556 ? O2 Eu2 O3 67.9(2) . 7_556 ? O4 Eu2 O3 55.29(19) 7_556 7_556 ? O7 Eu2 O3 145.2(2) . 7_556 ? O17 Eu2 O3 118.7(2) . 7_556 ? O16 Eu2 O3 124.3(2) . 7_556 ? O3 Eu2 O9 77.7(2) . . ? O10 Eu2 O9 135.1(2) 7_556 . ? O2 Eu2 O9 70.0(2) . . ? O4 Eu2 O9 135.4(2) 7_556 . ? O7 Eu2 O9 55.1(2) . . ? O17 Eu2 O9 109.7(2) . . ? O16 Eu2 O9 74.2(2) . . ? O3 Eu2 O9 130.14(19) 7_556 . ? O3 Eu2 S2 166.62(16) . . ? O10 Eu2 S2 104.42(15) 7_556 . ? O2 Eu2 S2 108.80(15) . . ? O4 Eu2 S2 69.83(14) 7_556 . ? O7 Eu2 S2 84.80(17) . . ? O17 Eu2 S2 27.78(15) . . ? O16 Eu2 S2 28.25(15) . . ? O3 Eu2 S2 124.56(13) 7_556 . ? O9 Eu2 S2 93.53(15) . . ? O3 Eu2 S1 96.72(15) . 7_556 ? O10 Eu2 S1 80.66(17) 7_556 7_556 ? O2 Eu2 S1 68.44(14) . 7_556 ? O4 Eu2 S1 26.78(14) 7_556 7_556 ? O7 Eu2 S1 166.00(16) . 7_556 ? O17 Eu2 S1 97.17(16) . 7_556 ? O16 Eu2 S1 97.22(17) . 7_556 ? O3 Eu2 S1 28.61(14) 7_556 7_556 ? O9 Eu2 S1 138.34(15) . 7_556 ? S2 Eu2 S1 96.54(6) . 7_556 ? O3 Eu2 S5 80.36(15) . . ? O10 Eu2 S5 110.83(17) 7_556 . ? O2 Eu2 S5 98.32(14) . . ? O4 Eu2 S5 152.78(15) 7_556 . ? O7 Eu2 S5 26.82(16) . . ? O17 Eu2 S5 91.99(16) . . ? O16 Eu2 S5 80.01(17) . . ? O3 Eu2 S5 147.74(13) 7_556 . ? O9 Eu2 S5 28.43(15) . . ? S2 Eu2 S5 87.13(6) . . ? S1 Eu2 S5 166.75(6) 7_556 . ? O22 Eu3 O23 80.8(3) 6 . ? O22 Eu3 O13 112.1(3) 6 2_656 ? O23 Eu3 O13 148.6(3) . 2_656 ? O22 Eu3 O14 77.7(3) 6 6 ? O23 Eu3 O14 79.6(3) . 6 ? O13 Eu3 O14 75.8(2) 2_656 6 ? O22 Eu3 O5 153.6(2) 6 . ? O23 Eu3 O5 99.5(3) . . ? O13 Eu3 O5 81.4(2) 2_656 . ? O14 Eu3 O5 128.6(2) 6 . ? O22 Eu3 O18 88.8(3) 6 . ? O23 Eu3 O18 136.3(2) . . ? O13 Eu3 O18 74.3(2) 2_656 . ? O14 Eu3 O18 139.3(2) 6 . ? O5 Eu3 O18 72.6(2) . . ? O22 Eu3 O19 147.3(3) 6 . ? O23 Eu3 O19 76.3(2) . . ? O13 Eu3 O19 78.9(2) 2_656 . ? O14 Eu3 O19 75.5(2) 6 . ? O5 Eu3 O19 55.1(2) . . ? O18 Eu3 O19 123.9(2) . . ? O22 Eu3 O15 81.7(3) 6 . ? O23 Eu3 O15 81.3(2) . . ? O13 Eu3 O15 127.7(2) 2_656 . ? O14 Eu3 O15 153.8(2) 6 . ? O5 Eu3 O15 72.3(2) . . ? O18 Eu3 O15 55.2(2) . . ? O19 Eu3 O15 116.8(2) . . ? O22 Eu3 S2 87.2(2) 6 . ? O23 Eu3 S2 109.1(2) . . ? O13 Eu3 S2 100.25(17) 2_656 . ? O14 Eu3 S2 161.21(17) 6 . ? O5 Eu3 S2 67.58(15) . . ? O18 Eu3 S2 27.50(16) . . ? O19 Eu3 S2 122.20(16) . . ? O15 Eu3 S2 27.90(15) . . ? O22 Eu3 S4 169.2(3) 6 . ? O23 Eu3 S4 88.46(19) . . ? O13 Eu3 S4 77.98(17) 2_656 . ? O14 Eu3 S4 101.88(16) 6 . ? O5 Eu3 S4 27.61(15) . . ? O18 Eu3 S4 98.13(17) . . ? O19 Eu3 S4 27.46(15) . . ? O15 Eu3 S4 95.34(17) . . ? S2 Eu3 S4 95.08(6) . . ? O11 S1 O4 112.0(4) . . ? O11 S1 O6 110.6(4) . . ? O4 S1 O6 109.5(4) . . ? O11 S1 O3 111.5(4) . . ? O4 S1 O3 104.0(4) . . ? O6 S1 O3 109.0(4) . . ? O11 S1 Eu2 122.7(3) . 7_556 ? O4 S1 Eu2 48.1(3) . 7_556 ? O6 S1 Eu2 126.6(3) . 7_556 ? O3 S1 Eu2 56.2(2) . 7_556 ? O18 S2 O17 111.2(4) . . ? O18 S2 O15 104.8(4) . . ? O17 S2 O15 111.7(4) . . ? O18 S2 O16 113.7(4) . . ? O17 S2 O16 104.8(4) . . ? O15 S2 O16 110.8(4) . . ? O18 S2 Eu2 124.7(3) . . ? O17 S2 Eu2 51.4(2) . . ? O15 S2 Eu2 130.4(3) . . ? O16 S2 Eu2 53.6(3) . . ? O18 S2 Eu3 51.7(3) . . ? O17 S2 Eu3 120.5(3) . . ? O15 S2 Eu3 53.6(3) . . ? O16 S2 Eu3 134.7(3) . . ? Eu2 S2 Eu3 171.02(8) . . ? O12 S3 O8 109.4(4) . . ? O12 S3 O10 109.8(4) . . ? O8 S3 O10 110.0(4) . . ? O12 S3 O2 108.9(4) . . ? O8 S3 O2 108.9(4) . . ? O10 S3 O2 109.8(3) . . ? O14 S4 O19 111.2(4) . . ? O14 S4 O5 112.4(4) . . ? O19 S4 O5 104.1(4) . . ? O14 S4 O13 107.4(4) . . ? O19 S4 O13 112.9(4) . . ? O5 S4 O13 108.9(4) . . ? O14 S4 Eu3 129.4(3) . . ? O19 S4 Eu3 52.8(3) . . ? O5 S4 Eu3 51.4(3) . . ? O13 S4 Eu3 123.2(3) . . ? O20 S5 O1 112.8(5) . . ? O20 S5 O7 110.3(5) . . ? O1 S5 O7 113.8(4) . . ? O20 S5 O9 111.6(5) . . ? O1 S5 O9 103.9(4) . . ? O7 S5 O9 103.8(4) . . ? O20 S5 Eu1 123.8(4) . . ? O1 S5 Eu1 51.2(3) . . ? O7 S5 Eu1 125.5(3) . . ? O9 S5 Eu1 52.9(3) . . ? O20 S5 Eu2 120.9(4) . . ? O1 S5 Eu2 126.2(3) . . ? O7 S5 Eu2 48.3(3) . . ? O9 S5 Eu2 55.8(2) . . ? Eu1 S5 Eu2 94.74(6) . . ? O21 S6 O22 110.3(6) . . ? O21 S6 O24 109.2(7) . . ? O22 S6 O24 109.2(7) . . ? O21 S6 O23 110.7(5) . . ? O22 S6 O23 108.6(5) . . ? O24 S6 O23 108.8(6) . . ? S6 O22 Eu3 162.4(6) . 6_556 ? S6 O23 Eu3 147.7(5) . . ? C1 N1 C1 115.5(16) 2_656 . ? C1 N1 H1D 108.0 2_656 . ? C1 N1 H1D 108.7 . . ? C2 N2 C3 113.6(8) . . ? C2 N2 H2D 108.9 . . ? C3 N2 H2D 108.9 . . ? C2 N2 H2E 108.9 . . ? C3 N2 H2E 108.9 . . ? H2D N2 H2E 107.7 . . ? C4 N3 C5 122.1(19) . . ? C4 N3 H3D 106.8 . . ? C5 N3 H3D 106.8 . . ? C4 N3 H3E 106.8 . . ? C5 N3 H3E 106.8 . . ? H3D N3 H3E 106.7 . . ? C6 N4 N4 57.1(11) . 2_556 ? C6 N4 C7 118.1(18) . . ? N4 N4 C7 61.1(10) 2_556 . ? C6 N4 H4D 107.6 . . ? N4 N4 H4D 126.0 2_556 . ? C7 N4 H4D 107.6 . . ? C6 N4 H4E 107.9 . . ? N4 N4 H4E 126.7 2_556 . ? C7 N4 H4E 107.9 . . ? H4D N4 H4E 107.2 . . ? C10 N5 C9 113.7(15) . . ? C10 N5 H5D 108.8 . . ? C9 N5 H5D 108.8 . . ? C10 N5 H5E 108.8 . . ? C9 N5 H5E 108.8 . . ? H5D N5 H5E 107.7 . . ? C8 N6 C8 115(2) . 2_656 ? C8 N6 H6B 107.9 . . ? C8 N6 H6B 109.0 2_656 . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N4 66(2) . 2_556 ? N4 C6 H6A 110.5 . . ? N4 C6 H6A 176.3 2_556 . ? N4 C6 H6C 109.5 . . ? N4 C6 H6C 71.9 2_556 . ? H6A C6 H6C 109.5 . . ? N4 C6 H6D 108.4 . . ? N4 C6 H6D 72.9 2_556 . ? H6A C6 H6D 109.5 . . ? H6C C6 H6D 109.5 . . ? N4 C7 N4 58(2) 2_556 . ? N4 C7 H7A 167.9 2_556 . ? N4 C7 H7A 110.0 . . ? N4 C7 H7B 77.4 2_556 . ? N4 C7 H7B 108.7 . . ? H7A C7 H7B 109.4 . . ? N4 C7 H7C 76.5 2_556 . ? N4 C7 H7C 109.7 . . ? H7A C7 H7C 109.4 . . ? H7B C7 H7C 109.5 . . ? N6 C8 H8A 109.5 . . ? N6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S5 O1 Eu1 101.3(4) . . ? S3 O2 Eu2 133.2(4) . . ? S1 O3 Eu2 151.7(4) . . ? S1 O3 Eu2 95.2(3) . 7_556 ? Eu2 O3 Eu2 111.5(2) . 7_556 ? S1 O4 Eu2 105.1(3) . 7_556 ? S4 O5 Eu3 101.0(3) . . ? S1 O6 Eu1 138.6(4) . . ? S5 O7 Eu2 104.9(4) . . ? S3 O8 Eu1 153.1(4) . . ? S5 O9 Eu1 98.3(3) . . ? S5 O9 Eu2 95.8(3) . . ? Eu1 O9 Eu2 127.9(3) . . ? S3 O10 Eu2 141.7(4) . 7_556 ? S4 O13 Eu3 139.3(4) . 2_656 ? S4 O14 Eu3 131.7(4) . 6_556 ? S2 O15 Eu3 98.5(3) . . ? S2 O16 Eu2 98.1(3) . . ? S2 O17 Eu2 100.8(3) . . ? S2 O18 Eu3 100.8(3) . . ? S4 O19 Eu3 99.7(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.993 _refine_diff_density_min -2.495 _refine_diff_density_rms 0.199