# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Guo-Yu Yang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 CHINA ; _publ_contact_author_email ygy@fjirsm.ac.cn _publ_contact_author_phone 86-59183710051 _publ_contact_author_fax 86-59183710051 loop_ _publ_author_name _publ_author_address 'Yanqiong Sun' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 CHINA ; 'Jie Zhang' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 CHINA ; 'Guo-Yu Yang' ; State Key Lab of Structural Chemistry Fujian Institute of Reseach on the Structure of Matter, Chinese Academy of Sciences Fuzhou 350002 CHINA ; _publ_section_title ; Two novel luminescent lanthanide sulfate-carboxylates with unusual 2-D bamboo-raft-like structure based on the linkages of left- and right-handed helical tubes involving in-situ decarboxylation ; data_dy _database_code_depnum_ccdc_archive 'CCDC 293649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H5 Dy N2 O7 S' _chemical_formula_sum 'C4 H5 Dy N2 O7 S' _chemical_formula_weight 387.66 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.157(3) _cell_length_b 6.4786(15) _cell_length_c 12.087(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.8080(10) _cell_angle_gamma 90.00 _cell_volume 831.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2710 _cell_measurement_theta_min 1.7692 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.1300 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 9.256 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.259 _exptl_absorpt_correction_T_max 0.523 _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 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5902 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1836 _reflns_number_gt 1730 _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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1836 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 Dy Dy 0.160177(14) 0.14083(2) 0.605620(12) 0.00846(8) Uani 1 1 d . . . S S -0.16272(8) 0.32094(13) 0.45562(7) 0.01227(18) Uani 1 1 d . . . C1 C 0.5128(4) 0.2599(6) 0.5015(3) 0.0202(8) Uani 1 1 d . . . H1A H 0.5476 0.2764 0.4413 0.024 Uiso 1 1 calc R . . C2 C 0.4893(4) 0.2298(7) 0.6743(3) 0.0236(9) Uani 1 1 d . . . H2A H 0.5088 0.2232 0.7547 0.028 Uiso 1 1 calc R . . C3 C 0.3884(3) 0.2348(5) 0.4923(3) 0.0127(7) Uani 1 1 d . . . C4 C 0.2735(3) 0.2235(5) 0.3907(3) 0.0113(7) Uani 1 1 d . . . N1 N 0.5745(3) 0.2555(5) 0.6168(3) 0.0210(7) Uani 1 1 d . . . H1B H 0.6545 0.2671 0.6481 0.025 Uiso 1 1 calc R . . N2 N 0.3743(3) 0.2152(5) 0.6007(2) 0.0150(6) Uani 1 1 d . . . O1 O 0.2792(2) 0.2787(4) 0.2935(2) 0.0166(5) Uani 1 1 d . . . O2 O 0.1761(2) 0.1599(4) 0.4131(2) 0.0146(5) Uani 1 1 d . . . O3 O -0.1338(3) 0.5041(4) 0.3977(2) 0.0203(6) Uani 1 1 d . . . O4 O -0.1994(3) 0.3746(4) 0.5568(2) 0.0235(6) Uani 1 1 d . . . O5 O -0.2600(2) 0.1923(4) 0.3719(2) 0.0187(6) Uani 1 1 d . . . O6 O -0.0506(2) 0.1813(4) 0.4899(2) 0.0124(5) Uani 1 1 d . . . O1W O 0.0424(3) 0.0270(5) 0.7244(2) 0.0259(7) Uani 1 1 d . . . H11 H 0.0720 -0.0318 0.7889 0.080 Uiso 1 1 d R . . H12 H -0.0201 -0.0374 0.6844 0.080 Uiso 1 1 d 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 Dy 0.00842(10) 0.00903(12) 0.00594(10) 0.00022(5) -0.00075(6) -0.00021(6) S 0.0097(4) 0.0103(4) 0.0134(4) -0.0009(3) -0.0015(3) 0.0010(3) C1 0.0156(19) 0.027(2) 0.0167(19) 0.0003(15) 0.0028(15) -0.0026(16) C2 0.018(2) 0.033(2) 0.0152(18) 0.0009(16) -0.0016(15) -0.0055(17) C3 0.0134(17) 0.0151(18) 0.0087(16) 0.0007(13) 0.0020(13) -0.0020(14) C4 0.0133(17) 0.0102(17) 0.0084(15) -0.0006(12) 0.0004(13) 0.0013(13) N1 0.0090(15) 0.0304(19) 0.0199(16) 0.0000(13) -0.0012(12) -0.0018(13) N2 0.0117(15) 0.0222(16) 0.0085(14) 0.0020(12) -0.0007(11) -0.0037(13) O1 0.0164(13) 0.0255(14) 0.0066(11) 0.0025(10) 0.0017(10) 0.0024(11) O2 0.0112(13) 0.0209(14) 0.0093(11) 0.0012(9) -0.0006(9) -0.0028(10) O3 0.0219(15) 0.0125(13) 0.0220(14) 0.0028(10) 0.0003(11) 0.0033(11) O4 0.0262(16) 0.0235(15) 0.0233(15) -0.0073(11) 0.0113(12) 0.0012(12) O5 0.0126(13) 0.0149(12) 0.0228(14) -0.0036(11) -0.0033(11) -0.0004(11) O6 0.0101(12) 0.0092(11) 0.0124(12) 0.0002(9) -0.0048(9) 0.0021(9) O1W 0.0231(15) 0.0415(18) 0.0114(12) 0.0012(12) 0.0026(11) -0.0162(13) _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 Dy O1 2.313(2) 4_566 ? Dy O3 2.318(3) 3_566 ? Dy O1W 2.342(3) . ? Dy O6 2.355(2) . ? Dy O2 2.390(3) . ? Dy O5 2.405(3) 3_556 ? Dy N2 2.455(3) . ? Dy O6 2.514(2) 3_556 ? Dy S 3.0841(11) 3_556 ? S O4 1.446(3) . ? S O3 1.463(3) . ? S O5 1.492(3) . ? S O6 1.496(2) . ? S Dy 3.0841(11) 3_556 ? C1 N1 1.352(5) . ? C1 C3 1.367(5) . ? C1 H1A 0.9300 . ? C2 N2 1.322(5) . ? C2 N1 1.348(5) . ? C2 H2A 0.9300 . ? C3 N2 1.373(4) . ? C3 C4 1.481(4) . ? C4 O1 1.248(4) . ? C4 O2 1.267(4) . ? N1 H1B 0.8600 . ? O1 Dy 2.313(2) 4_565 ? O3 Dy 2.318(3) 3_566 ? O5 Dy 2.405(3) 3_556 ? O6 Dy 2.514(2) 3_556 ? O1W H11 0.8395 . ? O1W H12 0.8287 . ? 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 Dy O3 79.93(9) 4_566 3_566 ? O1 Dy O1W 74.36(9) 4_566 . ? O3 Dy O1W 103.36(10) 3_566 . ? O1 Dy O6 136.68(9) 4_566 . ? O3 Dy O6 77.33(9) 3_566 . ? O1W Dy O6 75.73(9) . . ? O1 Dy O2 138.86(9) 4_566 . ? O3 Dy O2 88.77(9) 3_566 . ? O1W Dy O2 146.66(9) . . ? O6 Dy O2 76.92(9) . . ? O1 Dy O5 89.10(9) 4_566 3_556 ? O3 Dy O5 160.78(9) 3_566 3_556 ? O1W Dy O5 88.60(10) . 3_556 ? O6 Dy O5 120.72(8) . 3_556 ? O2 Dy O5 89.25(9) . 3_556 ? O1 Dy N2 73.08(9) 4_566 . ? O3 Dy N2 85.66(10) 3_566 . ? O1W Dy N2 144.00(9) . . ? O6 Dy N2 140.01(9) . . ? O2 Dy N2 66.67(9) . . ? O5 Dy N2 76.02(10) 3_556 . ? O1 Dy O6 133.68(8) 4_566 3_556 ? O3 Dy O6 140.77(8) 3_566 3_556 ? O1W Dy O6 74.62(9) . 3_556 ? O6 Dy O6 64.06(9) . 3_556 ? O2 Dy O6 76.49(8) . 3_556 ? O5 Dy O6 56.66(8) 3_556 3_556 ? N2 Dy O6 119.46(9) . 3_556 ? O1 Dy S 114.19(7) 4_566 3_556 ? O3 Dy S 165.68(6) 3_566 3_556 ? O1W Dy S 83.67(8) . 3_556 ? O6 Dy S 92.65(6) . 3_556 ? O2 Dy S 78.91(6) . 3_556 ? O5 Dy S 28.24(6) 3_556 3_556 ? N2 Dy S 95.97(8) . 3_556 ? O6 Dy S 28.76(6) 3_556 3_556 ? O4 S O3 111.76(16) . . ? O4 S O5 111.89(17) . . ? O3 S O5 110.48(15) . . ? O4 S O6 109.90(16) . . ? O3 S O6 109.56(15) . . ? O5 S O6 102.89(14) . . ? O4 S Dy 117.51(11) . 3_556 ? O3 S Dy 130.73(12) . 3_556 ? O5 S Dy 49.71(10) . 3_556 ? O6 S Dy 53.95(9) . 3_556 ? N1 C1 C3 105.4(3) . . ? N1 C1 H1A 127.3 . . ? C3 C1 H1A 127.3 . . ? N2 C2 N1 110.7(3) . . ? N2 C2 H2A 124.6 . . ? N1 C2 H2A 124.6 . . ? C1 C3 N2 110.1(3) . . ? C1 C3 C4 132.3(3) . . ? N2 C3 C4 117.6(3) . . ? O1 C4 O2 126.0(3) . . ? O1 C4 C3 119.1(3) . . ? O2 C4 C3 114.9(3) . . ? C2 N1 C1 108.5(3) . . ? C2 N1 H1B 125.7 . . ? C1 N1 H1B 125.7 . . ? C2 N2 C3 105.3(3) . . ? C2 N2 Dy 138.5(3) . . ? C3 N2 Dy 116.0(2) . . ? C4 O1 Dy 144.1(2) . 4_565 ? C4 O2 Dy 123.3(2) . . ? S O3 Dy 140.17(17) . 3_566 ? S O5 Dy 102.06(13) . 3_556 ? S O6 Dy 146.14(14) . . ? S O6 Dy 97.30(12) . 3_556 ? Dy O6 Dy 115.94(9) . 3_556 ? Dy O1W H11 125.2 . . ? Dy O1W H12 109.3 . . ? H11 O1W H12 109.5 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.067 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.144 # Attachment 'CCDC-293650.cif' data_eu _database_code_depnum_ccdc_archive 'CCDC 293650' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H5 Eu N2 O7 S' _chemical_formula_sum 'C4 H5 Eu N2 O7 S' _chemical_formula_weight 377.12 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 P_1_21/c_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.209(2) _cell_length_b 6.5406(11) _cell_length_c 12.203(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.922(2) _cell_angle_gamma 90.00 _cell_volume 851.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2968 _cell_measurement_theta_min 1.7539 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.2300 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 7.635 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.416 _exptl_absorpt_correction_T_max 0.543 _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 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6227 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1946 _reflns_number_gt 1853 _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^)+(0.0355P)^2^+0.1842P] 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 1946 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0189 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.351 _refine_ls_restrained_S_all 1.351 _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 Eu Eu 0.161464(15) 0.14159(3) 0.605979(13) 0.00810(9) Uani 1 1 d . . . S S -0.16314(8) 0.32110(14) 0.45557(8) 0.01219(19) Uani 1 1 d . . . C1 C 0.5136(4) 0.2604(7) 0.4992(3) 0.0179(8) Uani 1 1 d . . . H1A H 0.5474 0.2777 0.4391 0.022 Uiso 1 1 calc R . . C2 C 0.4931(4) 0.2288(8) 0.6715(3) 0.0231(9) Uani 1 1 d . . . H2A H 0.5136 0.2209 0.7513 0.028 Uiso 1 1 calc R . . C3 C 0.3909(3) 0.2337(6) 0.4911(3) 0.0125(7) Uani 1 1 d . . . C4 C 0.2756(3) 0.2231(6) 0.3916(3) 0.0115(7) Uani 1 1 d . . . N1 N 0.5766(3) 0.2563(6) 0.6144(3) 0.0222(7) Uani 1 1 d . . . H1B H 0.6563 0.2691 0.6451 0.027 Uiso 1 1 calc R . . N2 N 0.3782(3) 0.2147(6) 0.6001(2) 0.0158(6) Uani 1 1 d . . . O1 O 0.2818(3) 0.2769(5) 0.2946(2) 0.0177(6) Uani 1 1 d . . . O2 O 0.1784(3) 0.1591(4) 0.4123(2) 0.0155(6) Uani 1 1 d . . . O3 O -0.1344(3) 0.5017(5) 0.3979(2) 0.0213(6) Uani 1 1 d . . . O4 O -0.1988(3) 0.3765(4) 0.5569(3) 0.0249(7) Uani 1 1 d . . . O5 O -0.2617(3) 0.1958(4) 0.3734(3) 0.0194(6) Uani 1 1 d . . . O6 O -0.0514(2) 0.1819(4) 0.4893(2) 0.0137(5) Uani 1 1 d . . . O1W O 0.0422(3) 0.0239(5) 0.7252(2) 0.0269(7) Uani 1 1 d . . . H11 H 0.0718 -0.0349 0.7897 0.080 Uiso 1 1 d R . . H12 H -0.0202 -0.0405 0.6853 0.080 Uiso 1 1 d 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 Eu 0.00807(12) 0.00823(13) 0.00700(12) -0.00009(5) 0.00083(8) -0.00011(6) S 0.0093(4) 0.0087(4) 0.0162(4) -0.0011(3) 0.0004(3) 0.0011(3) C1 0.0147(17) 0.024(2) 0.0155(17) 0.0008(15) 0.0050(14) -0.0014(16) C2 0.021(2) 0.032(3) 0.0136(18) 0.0014(17) 0.0013(15) -0.0068(19) C3 0.0122(16) 0.0153(19) 0.0092(16) 0.0020(14) 0.0023(13) 0.0010(14) C4 0.0129(16) 0.0105(17) 0.0107(16) -0.0021(13) 0.0031(13) 0.0020(14) N1 0.0107(15) 0.030(2) 0.0214(17) -0.0008(15) -0.0010(13) -0.0033(15) N2 0.0129(15) 0.0245(18) 0.0083(14) 0.0007(13) 0.0007(12) -0.0037(14) O1 0.0172(13) 0.0257(16) 0.0101(12) 0.0026(11) 0.0040(10) 0.0023(12) O2 0.0124(13) 0.0230(15) 0.0091(12) -0.0014(10) 0.0002(10) -0.0037(10) O3 0.0231(14) 0.0112(15) 0.0257(15) 0.0032(11) 0.0018(12) 0.0018(12) O4 0.0257(17) 0.0255(17) 0.0265(16) -0.0102(12) 0.0123(14) -0.0007(13) O5 0.0139(13) 0.0125(13) 0.0256(14) -0.0035(12) -0.0028(11) -0.0001(11) O6 0.0093(12) 0.0107(12) 0.0175(13) -0.0003(10) -0.0009(10) 0.0027(10) O1W 0.0232(15) 0.044(2) 0.0126(13) -0.0005(13) 0.0037(11) -0.0181(14) _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 O1 2.344(3) 4_566 ? Eu O3 2.351(3) 3_566 ? Eu O1W 2.386(3) . ? Eu O6 2.387(3) . ? Eu O2 2.431(3) . ? Eu O5 2.453(3) 3_556 ? Eu N2 2.499(3) . ? Eu O6 2.543(3) 3_556 ? Eu S 3.1195(11) 3_556 ? Eu Eu 4.1786(6) 3_556 ? Eu H12 2.7778 . ? S O4 1.457(3) . ? S O3 1.460(3) . ? S O5 1.489(3) . ? S O6 1.500(3) . ? S Eu 3.1195(11) 3_556 ? C1 C3 1.361(5) . ? C1 N1 1.366(5) . ? C1 H1A 0.9300 . ? C2 N2 1.318(5) . ? C2 N1 1.340(5) . ? C2 H2A 0.9300 . ? C3 N2 1.385(4) . ? C3 C4 1.478(5) . ? C4 O1 1.256(4) . ? C4 O2 1.264(5) . ? N1 H1B 0.8600 . ? O1 Eu 2.344(3) 4_565 ? O3 Eu 2.351(3) 3_566 ? O5 Eu 2.453(3) 3_556 ? O6 Eu 2.543(3) 3_556 ? O1W H11 0.8468 . ? O1W H12 0.8336 . ? 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 Eu O3 79.97(10) 4_566 3_566 ? O1 Eu O1W 74.66(10) 4_566 . ? O3 Eu O1W 103.86(12) 3_566 . ? O1 Eu O6 136.73(10) 4_566 . ? O3 Eu O6 77.26(10) 3_566 . ? O1W Eu O6 75.79(10) . . ? O1 Eu O2 138.64(10) 4_566 . ? O3 Eu O2 88.94(10) 3_566 . ? O1W Eu O2 146.51(9) . . ? O6 Eu O2 77.17(10) . . ? O1 Eu O5 89.82(10) 4_566 3_556 ? O3 Eu O5 161.18(10) 3_566 3_556 ? O1W Eu O5 88.39(12) . 3_556 ? O6 Eu O5 120.16(9) . 3_556 ? O2 Eu O5 88.39(10) . 3_556 ? O1 Eu N2 73.38(10) 4_566 . ? O3 Eu N2 85.98(11) 3_566 . ? O1W Eu N2 144.23(10) . . ? O6 Eu N2 139.82(10) . . ? O2 Eu N2 66.14(10) . . ? O5 Eu N2 75.91(11) 3_556 . ? O1 Eu O6 133.64(10) 4_566 3_556 ? O3 Eu O6 140.79(9) 3_566 3_556 ? O1W Eu O6 74.14(10) . 3_556 ? O6 Eu O6 64.15(10) . 3_556 ? O2 Eu O6 76.50(9) . 3_556 ? O5 Eu O6 56.01(9) 3_556 3_556 ? N2 Eu O6 119.01(10) . 3_556 ? O1 Eu S 114.39(8) 4_566 3_556 ? O3 Eu S 165.47(7) 3_566 3_556 ? O1W Eu S 83.10(9) . 3_556 ? O6 Eu S 92.44(7) . 3_556 ? O2 Eu S 78.68(7) . 3_556 ? O5 Eu S 27.84(6) 3_556 3_556 ? N2 Eu S 95.78(9) . 3_556 ? O6 Eu S 28.45(6) 3_556 3_556 ? O1 Eu Eu 146.72(7) 4_566 3_556 ? O3 Eu Eu 110.22(7) 3_566 3_556 ? O1W Eu Eu 72.14(7) . 3_556 ? O6 Eu Eu 33.21(6) . 3_556 ? O2 Eu Eu 74.40(7) . 3_556 ? O5 Eu Eu 86.96(6) 3_556 3_556 ? N2 Eu Eu 137.02(7) . 3_556 ? O6 Eu Eu 30.94(6) 3_556 3_556 ? S Eu Eu 59.284(17) 3_556 3_556 ? O1 Eu H12 91.0 4_566 . ? O3 Eu H12 109.2 3_566 . ? O1W Eu H12 16.4 . . ? O6 Eu H12 63.2 . . ? O2 Eu H12 130.1 . . ? O5 Eu H12 86.6 3_556 . ? N2 Eu H12 156.3 . . ? O6 Eu H12 59.9 3_556 . ? S Eu H12 74.2 3_556 . ? Eu Eu H12 55.8 3_556 . ? O4 S O3 111.47(18) . . ? O4 S O5 111.59(19) . . ? O3 S O5 110.41(17) . . ? O4 S O6 110.00(18) . . ? O3 S O6 109.53(17) . . ? O5 S O6 103.55(16) . . ? O4 S Eu 117.98(13) . 3_556 ? O3 S Eu 130.55(13) . 3_556 ? O5 S Eu 50.34(11) . 3_556 ? O6 S Eu 53.90(11) . 3_556 ? C3 C1 N1 105.2(3) . . ? C3 C1 H1A 127.4 . . ? N1 C1 H1A 127.4 . . ? N2 C2 N1 111.2(3) . . ? N2 C2 H2A 124.4 . . ? N1 C2 H2A 124.4 . . ? C1 C3 N2 110.0(3) . . ? C1 C3 C4 132.4(3) . . ? N2 C3 C4 117.6(3) . . ? O1 C4 O2 125.6(3) . . ? O1 C4 C3 118.2(3) . . ? O2 C4 C3 116.1(3) . . ? C2 N1 C1 108.4(3) . . ? C2 N1 H1B 125.8 . . ? C1 N1 H1B 125.8 . . ? C2 N2 C3 105.1(3) . . ? C2 N2 Eu 139.0(3) . . ? C3 N2 Eu 115.6(2) . . ? C4 O1 Eu 143.8(2) . 4_565 ? C4 O2 Eu 122.7(2) . . ? S O3 Eu 140.02(19) . 3_566 ? S O5 Eu 101.82(14) . 3_556 ? S O6 Eu 145.86(16) . . ? S O6 Eu 97.65(13) . 3_556 ? Eu O6 Eu 115.85(10) . 3_556 ? Eu O1W H11 125.5 . . ? Eu O1W H12 109.5 . . ? H11 O1W H12 109.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.932 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.218