Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name '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, GUOYU.YANG@HOTMAIL.COM' _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 ; _publ_section_title ; Organic-Inorganic Hybrid Materials Constructed from Inorganic Lanthanide Sulfate Skeletons and Organic 4,5-imidazoledicarboxylic acid: Syntheses, Structures and Photolum- inescence ; 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 # Attachment '5c-CCDC-601351(TbS).cif' data_171 _database_code_depnum_ccdc_archive 'CCDC 601351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H5 N O7 S Tb' _chemical_formula_weight 382.08 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' Tb Tb -0.1723 4.1537 '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 11.1805(11) _cell_length_b 6.4982(5) _cell_length_c 12.1319(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.818(5) _cell_angle_gamma 90.00 _cell_volume 839.14(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2333 _cell_measurement_theta_min 3.1339 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 8.694 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4044 _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 6211 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1905 _reflns_number_gt 1770 _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^)+(0.0364P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1905 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Tb Tb 0.160541(19) 0.14110(3) 0.605692(16) 0.00963(10) Uani 1 1 d . . . S S -0.16287(11) 0.32069(16) 0.45535(10) 0.0137(2) Uani 1 1 d . . . C1 C 0.5133(5) 0.2604(8) 0.5004(4) 0.0211(10) Uani 1 1 d . . . H1A H 0.5481 0.2771 0.4404 0.025 Uiso 1 1 calc R . . C2 C 0.4906(5) 0.2290(9) 0.6729(4) 0.0247(11) Uani 1 1 d . . . H2A H 0.5103 0.2202 0.7529 0.030 Uiso 1 1 calc R . . C3 C 0.3889(4) 0.2345(7) 0.4914(4) 0.0144(9) Uani 1 1 d . . . C4 C 0.2745(5) 0.2248(7) 0.3919(4) 0.0149(9) Uani 1 1 d . . . N1 N 0.5750(4) 0.2561(7) 0.6167(4) 0.0244(9) Uani 1 1 d . . . H1B H 0.6547 0.2688 0.6483 0.029 Uiso 1 1 calc R . . N2 N 0.3754(4) 0.2161(6) 0.6004(3) 0.0169(8) Uani 1 1 d . . . O1 O 0.2801(3) 0.2786(5) 0.2937(3) 0.0188(7) Uani 1 1 d . . . O2 O 0.1770(3) 0.1598(5) 0.4130(3) 0.0174(7) Uani 1 1 d . . . O3 O -0.1342(3) 0.5043(5) 0.3973(3) 0.0214(8) Uani 1 1 d . . . O4 O -0.1989(4) 0.3757(5) 0.5571(3) 0.0268(9) Uani 1 1 d . . . O5 O -0.2606(3) 0.1937(5) 0.3726(3) 0.0201(7) Uani 1 1 d . . . O6 O -0.0510(3) 0.1812(5) 0.4896(3) 0.0137(7) Uani 1 1 d . . . O1W O 0.0418(4) 0.0252(6) 0.7246(3) 0.0281(9) Uani 1 1 d . . . H11 H 0.0714 -0.0336 0.7892 0.080 Uiso 1 1 d R . . H12 H -0.0206 -0.0393 0.6847 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 Tb 0.01166(16) 0.00908(14) 0.00865(14) 0.00021(7) 0.00387(10) -0.00009(7) S 0.0144(6) 0.0091(5) 0.0171(6) -0.0005(4) 0.0040(5) 0.0007(4) C1 0.020(3) 0.026(3) 0.018(2) 0.0020(19) 0.007(2) -0.003(2) C2 0.025(3) 0.032(3) 0.016(2) 0.000(2) 0.004(2) -0.006(2) C3 0.016(3) 0.016(2) 0.012(2) 0.0009(17) 0.0049(19) 0.0000(19) C4 0.023(3) 0.011(2) 0.013(2) -0.0015(16) 0.0073(19) 0.0015(19) N1 0.015(2) 0.035(2) 0.021(2) -0.0008(18) 0.0021(18) -0.002(2) N2 0.014(2) 0.027(2) 0.0091(18) -0.0013(16) 0.0021(16) -0.0066(18) O1 0.0193(19) 0.0284(19) 0.0092(15) 0.0023(13) 0.0050(14) 0.0023(16) O2 0.0151(19) 0.0273(18) 0.0103(16) 0.0001(12) 0.0044(14) -0.0027(14) O3 0.024(2) 0.0107(16) 0.026(2) 0.0046(13) 0.0037(16) 0.0019(14) O4 0.034(2) 0.0251(19) 0.028(2) -0.0096(15) 0.019(2) 0.0008(16) O5 0.0159(19) 0.0158(15) 0.0237(18) -0.0046(14) -0.0011(15) 0.0005(15) O6 0.0096(17) 0.0114(14) 0.0180(17) -0.0003(12) 0.0012(14) 0.0006(13) O1W 0.028(2) 0.042(2) 0.0136(17) -0.0021(15) 0.0066(16) -0.0170(18) _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 Tb O3 2.322(3) 3_566 ? Tb O1 2.323(3) 4_566 ? Tb O1W 2.363(3) . ? Tb O6 2.367(3) . ? Tb O2 2.403(3) . ? Tb O5 2.423(3) 3_556 ? Tb N2 2.472(4) . ? Tb O6 2.521(3) 3_556 ? Tb S 3.0928(11) 3_556 ? S O4 1.456(4) . ? S O3 1.470(4) . ? S O5 1.487(4) . ? S O6 1.497(3) . ? S Tb 3.0928(11) 3_556 ? C1 N1 1.368(6) . ? C1 C3 1.372(7) . ? C1 H1A 0.9300 . ? C2 N2 1.321(7) . ? C2 N1 1.334(7) . ? C2 H2A 0.9300 . ? C3 N2 1.380(6) . ? C3 C4 1.468(7) . ? C4 O1 1.261(5) . ? C4 O2 1.266(6) . ? N1 H1B 0.8600 . ? O1 Tb 2.323(3) 4_565 ? O3 Tb 2.322(3) 3_566 ? O5 Tb 2.423(3) 3_556 ? O6 Tb 2.521(3) 3_556 ? O1W H11 0.8424 . ? O1W H12 0.8308 . ? 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 O3 Tb O1 79.90(12) 3_566 4_566 ? O3 Tb O1W 103.51(13) 3_566 . ? O1 Tb O1W 74.56(12) 4_566 . ? O3 Tb O6 77.44(12) 3_566 . ? O1 Tb O6 136.82(11) 4_566 . ? O1W Tb O6 75.70(12) . . ? O3 Tb O2 88.95(11) 3_566 . ? O1 Tb O2 138.73(12) 4_566 . ? O1W Tb O2 146.56(12) . . ? O6 Tb O2 77.03(12) . . ? O3 Tb O5 160.87(13) 3_566 3_556 ? O1 Tb O5 89.28(12) 4_566 3_556 ? O1W Tb O5 88.53(13) . 3_556 ? O6 Tb O5 120.47(11) . 3_556 ? O2 Tb O5 88.90(12) . 3_556 ? O3 Tb N2 85.62(13) 3_566 . ? O1 Tb N2 73.12(12) 4_566 . ? O1W Tb N2 144.19(13) . . ? O6 Tb N2 139.88(12) . . ? O2 Tb N2 66.45(12) . . ? O5 Tb N2 76.11(13) 3_556 . ? O3 Tb O6 140.86(12) 3_566 3_556 ? O1 Tb O6 133.60(12) 4_566 3_556 ? O1W Tb O6 74.35(12) . 3_556 ? O6 Tb O6 64.02(12) . 3_556 ? O2 Tb O6 76.52(11) . 3_556 ? O5 Tb O6 56.45(11) 3_556 3_556 ? N2 Tb O6 119.45(12) . 3_556 ? O3 Tb S 165.80(9) 3_566 3_556 ? O1 Tb S 114.11(9) 4_566 3_556 ? O1W Tb S 83.36(10) . 3_556 ? O6 Tb S 92.55(8) . 3_556 ? O2 Tb S 78.89(8) . 3_556 ? O5 Tb S 28.06(8) 3_556 3_556 ? N2 Tb S 96.06(10) . 3_556 ? O6 Tb S 28.69(8) 3_556 3_556 ? O4 S O3 111.4(2) . . ? O4 S O5 111.8(2) . . ? O3 S O5 110.5(2) . . ? O4 S O6 109.7(2) . . ? O3 S O6 109.8(2) . . ? O5 S O6 103.31(19) . . ? O4 S Tb 117.77(15) . 3_556 ? O3 S Tb 130.83(15) . 3_556 ? O5 S Tb 50.06(13) . 3_556 ? O6 S Tb 53.95(13) . 3_556 ? N1 C1 C3 104.9(4) . . ? N1 C1 H1A 127.5 . . ? C3 C1 H1A 127.5 . . ? N2 C2 N1 111.5(4) . . ? N2 C2 H2A 124.3 . . ? N1 C2 H2A 124.3 . . ? C1 C3 N2 109.9(4) . . ? C1 C3 C4 132.7(4) . . ? N2 C3 C4 117.4(4) . . ? O1 C4 O2 125.3(5) . . ? O1 C4 C3 118.9(4) . . ? O2 C4 C3 115.8(4) . . ? C2 N1 C1 108.5(4) . . ? C2 N1 H1B 125.7 . . ? C1 N1 H1B 125.7 . . ? C2 N2 C3 105.2(4) . . ? C2 N2 Tb 138.8(3) . . ? C3 N2 Tb 115.7(3) . . ? C4 O1 Tb 144.1(3) . 4_565 ? C4 O2 Tb 122.7(3) . . ? S O3 Tb 140.2(2) . 3_566 ? S O5 Tb 101.88(18) . 3_556 ? S O6 Tb 146.05(19) . . ? S O6 Tb 97.35(16) . 3_556 ? Tb O6 Tb 115.98(12) . 3_556 ? Tb O1W H11 125.3 . . ? Tb O1W H12 109.5 . . ? H11 O1W H12 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.076 _refine_diff_density_min -3.043 _refine_diff_density_rms 0.244 # Attachment '5b-CCDC-601352(GdS).cif' data_172 _database_code_depnum_ccdc_archive 'CCDC 601352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H5 Gd N2 O7 S' _chemical_formula_weight 382.41 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' Gd Gd -0.1653 3.9035 '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 11.2069(3) _cell_length_b 6.5254(2) _cell_length_c 12.1824(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.9100(10) _cell_angle_gamma 90.00 _cell_volume 847.72(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25.66 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max .30 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 8.091 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .3075 _exptl_absorpt_correction_T_max 1.0000 _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 'Siemems-Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.5 _diffrn_reflns_number 4311 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.66 _reflns_number_total 1595 _reflns_number_gt 1494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _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^)+(0.0480P)^2^+6.3914P] 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 0.0067(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1595 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _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 Gd Gd 0.16110(3) 0.14120(5) 0.60588(2) 0.01049(19) Uani 1 1 d . . . S S -0.16302(15) 0.3212(3) 0.45557(15) 0.0149(4) Uani 1 1 d . . . C1 C 0.5127(7) 0.2598(12) 0.5003(7) 0.0210(16) Uani 1 1 d . . . H1A H 0.5470 0.2743 0.4402 0.025 Uiso 1 1 calc R . . C2 C 0.4944(7) 0.2291(14) 0.6735(7) 0.0258(17) Uani 1 1 d . . . H2A H 0.5156 0.2194 0.7534 0.031 Uiso 1 1 calc R . . C3 C 0.3905(7) 0.2358(11) 0.4909(6) 0.0167(14) Uani 1 1 d . . . C4 C 0.2749(6) 0.2226(11) 0.3922(6) 0.0163(14) Uani 1 1 d . . . N1 N 0.5760(6) 0.2586(11) 0.6158(6) 0.0248(15) Uani 1 1 d . . . H1B H 0.6556 0.2742 0.6461 0.030 Uiso 1 1 calc R . . N2 N 0.3763(6) 0.2153(11) 0.6007(5) 0.0213(14) Uani 1 1 d . . . O1 O 0.2806(5) 0.2776(9) 0.2939(4) 0.0198(11) Uani 1 1 d . . . O2 O 0.1778(5) 0.1592(8) 0.4126(4) 0.0200(12) Uani 1 1 d . . . O3 O -0.1342(5) 0.5019(8) 0.3969(4) 0.0228(12) Uani 1 1 d . . . O4 O -0.1980(6) 0.3764(8) 0.5564(5) 0.0265(13) Uani 1 1 d . . . O5 O -0.2598(5) 0.1959(8) 0.3733(5) 0.0228(11) Uani 1 1 d . . . O6 O -0.0523(5) 0.1818(8) 0.4894(4) 0.0177(11) Uani 1 1 d . . . O1W O 0.0425(5) 0.0242(10) 0.7255(5) 0.0304(14) Uani 1 1 d . . . H11 H 0.0721 -0.0346 0.7900 0.080 Uiso 1 1 d R . . H12 H -0.0199 -0.0402 0.6856 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 Gd 0.0114(2) 0.0086(3) 0.0125(2) 0.00017(12) 0.00522(14) 0.00018(11) S 0.0130(8) 0.0088(8) 0.0223(9) -0.0006(7) 0.0044(7) 0.0009(6) C1 0.023(4) 0.023(4) 0.022(4) -0.002(3) 0.014(3) -0.001(3) C2 0.021(4) 0.031(5) 0.023(4) 0.007(3) 0.003(3) -0.001(3) C3 0.018(3) 0.016(4) 0.019(4) 0.005(3) 0.009(3) 0.004(3) C4 0.018(3) 0.012(3) 0.018(4) -0.003(3) 0.004(3) 0.001(3) N1 0.014(3) 0.031(4) 0.027(3) 0.003(3) 0.003(2) -0.001(3) N2 0.018(3) 0.032(4) 0.015(3) 0.002(3) 0.005(2) -0.005(3) O1 0.019(2) 0.029(3) 0.014(2) 0.005(2) 0.0084(19) -0.001(2) O2 0.014(2) 0.031(3) 0.016(3) -0.001(2) 0.006(2) -0.003(2) O3 0.027(3) 0.009(3) 0.029(3) 0.001(2) 0.003(2) 0.003(2) O4 0.027(3) 0.025(3) 0.032(3) -0.011(2) 0.017(2) -0.001(2) O5 0.021(3) 0.015(3) 0.028(3) -0.004(2) 0.001(2) -0.003(2) O6 0.015(2) 0.014(3) 0.023(3) 0.002(2) 0.004(2) 0.002(2) O1W 0.029(3) 0.046(4) 0.018(3) -0.002(3) 0.010(2) -0.021(3) _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 Gd O1 2.331(5) 4_566 ? Gd O3 2.347(5) 3_566 ? Gd O1W 2.380(5) . ? Gd O6 2.391(5) . ? Gd O2 2.421(5) . ? Gd O5 2.440(6) 3_556 ? Gd N2 2.479(6) . ? Gd O6 2.531(5) 3_556 ? Gd S 3.1105(18) 3_556 ? S O4 1.445(6) . ? S O3 1.465(6) . ? S O5 1.477(5) . ? S O6 1.491(5) . ? S Gd 3.1105(18) 3_556 ? C1 C3 1.348(10) . ? C1 N1 1.368(10) . ? C1 H1A 0.9300 . ? C2 N1 1.328(10) . ? C2 N2 1.351(9) . ? C2 H2A 0.9300 . ? C3 N2 1.401(9) . ? C3 C4 1.474(9) . ? C4 O2 1.258(9) . ? C4 O1 1.271(9) . ? N1 H1B 0.8600 . ? O1 Gd 2.331(5) 4_565 ? O3 Gd 2.347(5) 3_566 ? O5 Gd 2.440(6) 3_556 ? O6 Gd 2.531(5) 3_556 ? O1W H11 0.8454 . ? O1W H12 0.8328 . ? 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 Gd O3 79.71(19) 4_566 3_566 ? O1 Gd O1W 74.43(18) 4_566 . ? O3 Gd O1W 103.5(2) 3_566 . ? O1 Gd O6 136.53(18) 4_566 . ? O3 Gd O6 77.33(18) 3_566 . ? O1W Gd O6 75.76(19) . . ? O1 Gd O2 138.72(17) 4_566 . ? O3 Gd O2 89.18(19) 3_566 . ? O1W Gd O2 146.68(18) . . ? O6 Gd O2 77.27(17) . . ? O1 Gd O5 89.86(19) 4_566 3_556 ? O3 Gd O5 161.45(19) 3_566 3_556 ? O1W Gd O5 88.2(2) . 3_556 ? O6 Gd O5 120.03(17) . 3_556 ? O2 Gd O5 88.67(19) . 3_556 ? O1 Gd N2 73.22(19) 4_566 . ? O3 Gd N2 85.9(2) 3_566 . ? O1W Gd N2 144.0(2) . . ? O6 Gd N2 140.03(19) . . ? O2 Gd N2 66.37(18) . . ? O5 Gd N2 76.4(2) 3_556 . ? O1 Gd O6 133.63(18) 4_566 3_556 ? O3 Gd O6 141.07(17) 3_566 3_556 ? O1W Gd O6 74.49(19) . 3_556 ? O6 Gd O6 64.4(2) . 3_556 ? O2 Gd O6 76.41(17) . 3_556 ? O5 Gd O6 55.68(16) 3_556 3_556 ? N2 Gd O6 119.1(2) . 3_556 ? O1 Gd S 114.36(15) 4_566 3_556 ? O3 Gd S 165.78(13) 3_566 3_556 ? O1W Gd S 83.26(16) . 3_556 ? O6 Gd S 92.55(13) . 3_556 ? O2 Gd S 78.74(13) . 3_556 ? O5 Gd S 27.64(12) 3_556 3_556 ? N2 Gd S 95.99(17) . 3_556 ? O6 Gd S 28.34(11) 3_556 3_556 ? O4 S O3 111.8(3) . . ? O4 S O5 112.3(3) . . ? O3 S O5 109.9(3) . . ? O4 S O6 109.7(3) . . ? O3 S O6 109.6(3) . . ? O5 S O6 103.0(3) . . ? O4 S Gd 118.0(2) . 3_556 ? O3 S Gd 130.1(2) . 3_556 ? O5 S Gd 50.0(2) . 3_556 ? O6 S Gd 53.7(2) . 3_556 ? C3 C1 N1 106.1(6) . . ? C3 C1 H1A 126.9 . . ? N1 C1 H1A 126.9 . . ? N1 C2 N2 110.9(7) . . ? N1 C2 H2A 124.5 . . ? N2 C2 H2A 124.5 . . ? C1 C3 N2 110.0(6) . . ? C1 C3 C4 133.7(7) . . ? N2 C3 C4 116.3(6) . . ? O2 C4 O1 125.2(6) . . ? O2 C4 C3 117.0(6) . . ? O1 C4 C3 117.7(6) . . ? C2 N1 C1 108.8(6) . . ? C2 N1 H1B 125.6 . . ? C1 N1 H1B 125.6 . . ? C2 N2 C3 104.1(6) . . ? C2 N2 Gd 139.5(5) . . ? C3 N2 Gd 116.1(4) . . ? C4 O1 Gd 144.1(5) . 4_565 ? C4 O2 Gd 122.6(4) . . ? S O3 Gd 139.3(3) . 3_566 ? S O5 Gd 102.3(3) . 3_556 ? S O6 Gd 145.8(3) . . ? S O6 Gd 98.0(2) . 3_556 ? Gd O6 Gd 115.6(2) . 3_556 ? Gd O1W H11 125.5 . . ? Gd O1W H12 109.4 . . ? H11 O1W H12 109.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.623 _refine_diff_density_min -1.989 _refine_diff_density_rms 0.235 # Attachment '5e-CCDC-601353(ErS).cif' data_173 _database_code_depnum_ccdc_archive 'CCDC 601353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H5 Er N2 O7 S' _chemical_formula_weight 392.42 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' Er Er -0.2586 4.9576 '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 11.1469(3) _cell_length_b 6.447 _cell_length_c 12.0387(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.7710(10) _cell_angle_gamma 90.00 _cell_volume 823.88(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.64 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max .30 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 10.462 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .5525 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4196 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.64 _reflns_number_total 1559 _reflns_number_gt 1456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _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^)+(0.0358P)^2^+8.7029P] 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 0.0023(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1559 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_restrained_S_all 1.208 _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 Er Er 0.15956(3) 0.14091(5) 0.60546(3) 0.00983(17) Uani 1 1 d . . . S S -0.16234(17) 0.3204(3) 0.45559(17) 0.0142(4) Uani 1 1 d . . . C1 C 0.5117(8) 0.2601(13) 0.5025(8) 0.0213(17) Uani 1 1 d . . . H1A H 0.5474 0.2777 0.4426 0.026 Uiso 1 1 calc R . . C2 C 0.4857(7) 0.2300(15) 0.6748(7) 0.0237(18) Uani 1 1 d . . . H2A H 0.5037 0.2234 0.7554 0.028 Uiso 1 1 calc R . . C3 C 0.3881(7) 0.2344(12) 0.4922(7) 0.0169(16) Uani 1 1 d . . . C4 C 0.2728(7) 0.2243(12) 0.3912(7) 0.0144(15) Uani 1 1 d . . . N1 N 0.5727(7) 0.2545(12) 0.6197(6) 0.0232(15) Uani 1 1 d . . . H1B H 0.6527 0.2649 0.6523 0.028 Uiso 1 1 calc R . . N2 N 0.3725(6) 0.2165(11) 0.6009(6) 0.0188(14) Uani 1 1 d . . . O1 O 0.2785(5) 0.2788(9) 0.2928(4) 0.0169(11) Uani 1 1 d . . . O2 O 0.1738(5) 0.1593(8) 0.4136(5) 0.0160(11) Uani 1 1 d . . . O3 O -0.1341(5) 0.5063(9) 0.3974(5) 0.0203(12) Uani 1 1 d . . . O4 O -0.2004(6) 0.3740(9) 0.5569(5) 0.0243(13) Uani 1 1 d . . . O5 O -0.2594(5) 0.1899(9) 0.3711(5) 0.0197(12) Uani 1 1 d . . . O6 O -0.0496(5) 0.1804(8) 0.4898(5) 0.0143(11) Uani 1 1 d . . . O1W O 0.0428(5) 0.0286(10) 0.7233(5) 0.0272(14) Uani 1 1 d . . . H11 H 0.0724 -0.0302 0.7878 0.080 Uiso 1 1 d R . . H12 H -0.0196 -0.0358 0.6834 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 Er 0.0085(2) 0.0103(2) 0.0100(2) 0.00026(12) 0.00184(14) -0.00010(11) S 0.0106(9) 0.0101(9) 0.0194(9) -0.0006(7) 0.0008(7) 0.0003(7) C1 0.014(4) 0.028(5) 0.021(4) -0.001(3) 0.005(3) -0.002(3) C2 0.011(4) 0.036(5) 0.019(4) 0.004(4) -0.002(3) -0.004(3) C3 0.016(4) 0.015(4) 0.019(4) -0.001(3) 0.004(3) 0.000(3) C4 0.012(4) 0.011(4) 0.020(4) -0.007(3) 0.004(3) 0.001(3) N1 0.016(3) 0.030(4) 0.020(3) -0.001(3) -0.001(3) -0.001(3) N2 0.014(3) 0.025(4) 0.015(3) 0.001(3) 0.001(3) -0.003(3) O1 0.017(3) 0.026(3) 0.009(2) 0.005(2) 0.005(2) 0.002(2) O2 0.011(3) 0.022(3) 0.015(3) 0.001(2) 0.005(2) -0.002(2) O3 0.026(3) 0.009(3) 0.024(3) 0.005(2) 0.005(2) 0.003(2) O4 0.025(3) 0.024(3) 0.028(3) -0.008(3) 0.015(3) -0.002(2) O5 0.016(3) 0.016(3) 0.022(3) -0.003(2) -0.001(2) 0.001(2) O6 0.011(3) 0.011(3) 0.019(3) -0.001(2) 0.001(2) 0.002(2) O1W 0.022(3) 0.044(4) 0.013(3) 0.000(3) 0.001(2) -0.016(3) _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 Er O3 2.291(6) 3_566 ? Er O1 2.300(5) 4_566 ? Er O1W 2.315(6) . ? Er O6 2.336(5) . ? Er O2 2.366(5) . ? Er O5 2.382(6) 3_556 ? Er N2 2.440(7) . ? Er O6 2.500(5) 3_556 ? Er S 3.0659(19) 3_556 ? S O4 1.450(6) . ? S O3 1.470(6) . ? S O5 1.497(6) . ? S O6 1.499(5) . ? S Er 3.0659(19) 3_556 ? C1 C3 1.356(12) . ? C1 N1 1.367(11) . ? C1 H1A 0.9300 . ? C2 N2 1.306(10) . ? C2 N1 1.341(12) . ? C2 H2A 0.9300 . ? C3 N2 1.376(11) . ? C3 C4 1.477(10) . ? C4 O1 1.256(10) . ? C4 O2 1.284(10) . ? N1 H1B 0.8600 . ? O1 Er 2.300(5) 4_565 ? O3 Er 2.291(6) 3_566 ? O5 Er 2.382(6) 3_556 ? O6 Er 2.500(5) 3_556 ? O1W H11 0.8363 . ? O1W H12 0.8269 . ? 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 O3 Er O1 79.8(2) 3_566 4_566 ? O3 Er O1W 103.3(2) 3_566 . ? O1 Er O1W 74.50(19) 4_566 . ? O3 Er O6 77.68(19) 3_566 . ? O1 Er O6 137.05(19) 4_566 . ? O1W Er O6 75.8(2) . . ? O3 Er O2 88.9(2) 3_566 . ? O1 Er O2 139.10(19) 4_566 . ? O1W Er O2 146.29(19) . . ? O6 Er O2 76.40(18) . . ? O3 Er O5 160.4(2) 3_566 3_556 ? O1 Er O5 88.7(2) 4_566 3_556 ? O1W Er O5 88.7(2) . 3_556 ? O6 Er O5 120.87(18) . 3_556 ? O2 Er O5 89.6(2) . 3_556 ? O3 Er N2 85.3(2) 3_566 . ? O1 Er N2 72.7(2) 4_566 . ? O1W Er N2 144.0(2) . . ? O6 Er N2 140.0(2) . . ? O2 Er N2 67.2(2) . . ? O5 Er N2 76.1(2) 3_556 . ? O3 Er O6 140.77(19) 3_566 3_556 ? O1 Er O6 133.75(19) 4_566 3_556 ? O1W Er O6 74.5(2) . 3_556 ? O6 Er O6 63.7(2) . 3_556 ? O2 Er O6 76.31(18) . 3_556 ? O5 Er O6 57.21(17) 3_556 3_556 ? N2 Er O6 120.0(2) . 3_556 ? O3 Er S 165.86(14) 3_566 3_556 ? O1 Er S 114.10(15) 4_566 3_556 ? O1W Er S 83.81(17) . 3_556 ? O6 Er S 92.52(13) . 3_556 ? O2 Er S 78.82(14) . 3_556 ? O5 Er S 28.52(13) 3_556 3_556 ? N2 Er S 96.16(18) . 3_556 ? O6 Er S 29.05(12) 3_556 3_556 ? O4 S O3 111.5(3) . . ? O4 S O5 111.7(4) . . ? O3 S O5 110.5(3) . . ? O4 S O6 110.4(3) . . ? O3 S O6 109.8(3) . . ? O5 S O6 102.7(3) . . ? O4 S Er 117.4(2) . 3_556 ? O3 S Er 131.1(2) . 3_556 ? O5 S Er 49.5(2) . 3_556 ? O6 S Er 54.0(2) . 3_556 ? C3 C1 N1 105.2(8) . . ? C3 C1 H1A 127.4 . . ? N1 C1 H1A 127.4 . . ? N2 C2 N1 111.4(7) . . ? N2 C2 H2A 124.3 . . ? N1 C2 H2A 124.3 . . ? C1 C3 N2 110.1(7) . . ? C1 C3 C4 133.2(8) . . ? N2 C3 C4 116.6(7) . . ? O1 C4 O2 125.7(7) . . ? O1 C4 C3 118.9(7) . . ? O2 C4 C3 115.4(7) . . ? C2 N1 C1 107.9(7) . . ? C2 N1 H1B 126.1 . . ? C1 N1 H1B 126.1 . . ? C2 N2 C3 105.4(7) . . ? C2 N2 Er 137.9(6) . . ? C3 N2 Er 116.4(5) . . ? C4 O1 Er 143.9(5) . 4_565 ? C4 O2 Er 122.6(5) . . ? S O3 Er 140.6(4) . 3_566 ? S O5 Er 102.0(3) . 3_556 ? S O6 Er 146.1(3) . . ? S O6 Er 96.9(2) . 3_556 ? Er O6 Er 116.3(2) . 3_556 ? Er O1W H11 125.1 . . ? Er O1W H12 109.4 . . ? H11 O1W H12 109.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.124 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.222 data_la _database_code_depnum_ccdc_archive 'CCDC 604058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 La2 N4 O14 S' _chemical_formula_weight 718.08 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' La La -0.2871 2.4523 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 6.879(2) _cell_length_b 14.067(5) _cell_length_c 33.802(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3270.7(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8034 _cell_measurement_theta_min 1.5676 _cell_measurement_theta_max 28.2812 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 5.377 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.650 _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 dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 26109 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23843 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4052 _reflns_number_gt 3878 _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^)+(0.0137P)^2^+7.8266P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4052 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.004 _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 La1 La 0.37521(3) 1.030683(13) 0.084912(5) 0.00490(5) Uani 1 1 d . . . La2 La 0.20207(3) 0.806413(13) 0.170993(5) 0.00514(5) Uani 1 1 d . . . C1 C 0.2621(5) 0.6451(2) -0.00920(10) 0.0082(6) Uani 1 1 d . . . C2 C 0.2563(5) 0.7487(2) 0.03782(9) 0.0064(6) Uani 1 1 d . . . C3 C 0.2842(5) 0.7977(2) 0.00304(9) 0.0072(6) Uani 1 1 d . . . C4 C 0.3153(5) 0.8988(2) -0.00715(9) 0.0060(6) Uani 1 1 d . . . C5 C 0.2150(4) 0.7763(2) 0.07929(9) 0.0063(6) Uani 1 1 d . . . C6 C -0.1586(5) 0.4376(2) 0.23358(10) 0.0103(7) Uani 1 1 d . . . C7 C -0.1594(5) 0.5344(2) 0.28278(10) 0.0075(6) Uani 1 1 d . . . C8 C -0.1324(5) 0.5894(2) 0.24956(10) 0.0078(6) Uani 1 1 d . . . C9 C -0.0999(5) 0.6928(2) 0.24159(10) 0.0083(6) Uani 1 1 d . . . C10 C -0.1922(5) 0.5571(2) 0.32487(10) 0.0079(6) Uani 1 1 d . . . S S 0.69871(12) 0.84110(5) 0.12630(2) 0.00616(15) Uani 1 1 d . . . N1 N 0.2860(4) 0.73033(19) -0.02637(8) 0.0073(5) Uani 1 1 d . . . N2 N 0.2427(4) 0.65309(19) 0.02951(8) 0.0075(5) Uani 1 1 d . . . N3 N -0.1741(4) 0.43935(19) 0.27246(8) 0.0084(6) Uani 1 1 d . . . N4 N -0.1327(4) 0.5257(2) 0.21876(8) 0.0095(6) Uani 1 1 d . . . O1 O 0.3294(3) 0.91917(16) -0.04346(7) 0.0078(5) Uani 1 1 d . . . O2 O 0.3254(4) 0.95712(16) 0.02051(7) 0.0112(5) Uani 1 1 d . . . O3 O 0.1433(3) 0.71160(16) 0.10085(7) 0.0087(5) Uani 1 1 d . . . O4 O 0.2462(4) 0.85874(16) 0.09271(7) 0.0084(5) Uani 1 1 d . . . O5 O -0.0404(4) 0.71245(17) 0.20711(7) 0.0118(5) Uani 1 1 d . . . O6 O -0.1314(4) 0.75233(17) 0.26807(7) 0.0133(5) Uani 1 1 d . . . O7 O -0.1744(4) 0.63950(17) 0.33774(7) 0.0132(5) Uani 1 1 d . . . O8 O -0.2445(4) 0.48716(16) 0.34665(7) 0.0094(5) Uani 1 1 d . . . O9 O 0.8829(4) 0.87021(18) 0.14527(7) 0.0128(5) Uani 1 1 d . . . O10 O 0.7188(4) 0.74803(17) 0.10726(7) 0.0119(5) Uani 1 1 d . . . O11 O 0.5445(3) 0.83831(17) 0.15645(7) 0.0109(5) Uani 1 1 d . . . O12 O 0.6518(4) 0.91275(17) 0.09557(7) 0.0104(5) Uani 1 1 d . . . O1W O 0.6461(4) 1.08451(17) 0.13555(7) 0.0108(5) Uani 1 1 d . . . O2W O 0.0067(3) 1.02713(17) 0.08434(7) 0.0130(5) Uani 1 1 d . . . H1A H 0.2527 0.5909 -0.0237 0.080 Uiso 1 1 d R . . H1 H 0.2883 0.7421 -0.0518 0.080 Uiso 1 1 d R . . H4 H -0.1178 0.5412 0.1944 0.080 Uiso 1 1 d R . . H6 H -0.1678 0.3834 0.2190 0.080 Uiso 1 1 d R . . H12 H 0.6690 1.1391 0.1305 0.080 Uiso 1 1 d R . . H11 H 0.7347 1.0570 0.1304 0.080 Uiso 1 1 d R . . H21 H -0.0330 0.9843 0.0915 0.080 Uiso 1 1 d R . . H22 H -0.0615 1.0447 0.0739 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 La1 0.00633(9) 0.00426(8) 0.00410(8) 0.00054(7) 0.00011(7) -0.00014(7) La2 0.00674(9) 0.00453(8) 0.00414(8) 0.00021(6) 0.00050(7) -0.00034(7) C1 0.0121(17) 0.0050(14) 0.0076(15) -0.0010(12) 0.0006(12) -0.0035(13) C2 0.0066(16) 0.0040(14) 0.0086(15) -0.0025(11) -0.0009(12) -0.0018(12) C3 0.0100(16) 0.0048(14) 0.0068(14) -0.0010(12) 0.0005(12) -0.0002(12) C4 0.0058(15) 0.0064(14) 0.0058(14) 0.0016(11) 0.0008(12) -0.0013(12) C5 0.0028(15) 0.0077(14) 0.0082(15) 0.0004(12) 0.0000(12) 0.0009(12) C6 0.0105(17) 0.0098(16) 0.0105(16) -0.0016(13) 0.0012(13) -0.0003(13) C7 0.0065(16) 0.0060(14) 0.0099(15) -0.0020(12) 0.0000(12) 0.0005(12) C8 0.0068(16) 0.0083(14) 0.0083(15) -0.0010(12) 0.0010(12) 0.0004(13) C9 0.0063(16) 0.0102(15) 0.0084(15) -0.0018(12) 0.0000(12) -0.0009(13) C10 0.0059(15) 0.0080(15) 0.0098(16) 0.0004(12) -0.0009(12) 0.0020(12) S 0.0070(4) 0.0058(3) 0.0057(4) 0.0008(3) 0.0006(3) 0.0006(3) N1 0.0116(14) 0.0058(12) 0.0045(12) -0.0006(10) 0.0014(11) -0.0008(11) N2 0.0102(14) 0.0057(13) 0.0065(13) -0.0008(10) 0.0013(11) -0.0021(11) N3 0.0107(14) 0.0069(13) 0.0075(13) -0.0007(10) -0.0008(11) 0.0009(11) N4 0.0133(15) 0.0106(13) 0.0045(12) -0.0003(11) 0.0015(11) 0.0007(12) O1 0.0087(12) 0.0078(11) 0.0068(11) 0.0018(9) 0.0002(9) -0.0005(9) O2 0.0198(13) 0.0059(11) 0.0080(11) 0.0001(9) -0.0002(10) -0.0022(10) O3 0.0124(12) 0.0070(11) 0.0067(11) -0.0004(9) 0.0014(9) -0.0013(9) O4 0.0137(12) 0.0057(11) 0.0056(11) 0.0002(8) -0.0001(9) -0.0008(9) O5 0.0143(13) 0.0116(12) 0.0094(11) 0.0021(9) 0.0023(10) -0.0042(10) O6 0.0198(14) 0.0073(11) 0.0129(12) -0.0017(9) 0.0049(10) 0.0004(10) O7 0.0232(15) 0.0076(11) 0.0089(12) -0.0030(9) -0.0013(10) 0.0045(10) O8 0.0126(12) 0.0096(11) 0.0061(11) 0.0011(9) 0.0023(9) 0.0006(9) O9 0.0068(12) 0.0180(13) 0.0135(12) -0.0003(10) -0.0018(10) -0.0010(10) O10 0.0192(13) 0.0075(11) 0.0089(11) 0.0000(9) 0.0003(10) 0.0023(10) O11 0.0071(12) 0.0170(12) 0.0087(11) -0.0015(9) 0.0033(9) -0.0011(10) O12 0.0138(13) 0.0079(11) 0.0096(11) 0.0027(9) 0.0008(9) 0.0012(10) O1W 0.0118(12) 0.0099(11) 0.0108(12) 0.0011(9) 0.0001(9) -0.0012(10) O2W 0.0089(12) 0.0137(12) 0.0163(12) 0.0055(10) -0.0009(10) 0.0002(10) _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 La1 O2 2.434(2) . ? La1 O2W 2.535(3) . ? La1 O12 2.550(2) . ? La1 O8 2.556(2) 3 ? La1 O1 2.567(2) 5_675 ? La1 O4 2.590(2) . ? La1 O3 2.604(2) 8_665 ? La1 O1W 2.641(2) . ? La1 N2 2.670(3) 8_665 ? La2 O11 2.448(2) . ? La2 O5 2.454(2) . ? La2 O6 2.477(2) 6_656 ? La2 O7 2.514(2) 6_656 ? La2 O9 2.526(3) 1_455 ? La2 O8 2.628(2) 3 ? La2 N3 2.681(3) 3 ? La2 O3 2.750(2) . ? La2 O4 2.763(2) . ? La2 C5 3.130(3) . ? C1 N2 1.320(4) . ? C1 N1 1.343(4) . ? C1 H1A 0.9083 . ? C2 C3 1.376(4) . ? C2 N2 1.378(4) . ? C2 C5 1.482(4) . ? C3 N1 1.374(4) . ? C3 C4 1.479(4) . ? C4 O2 1.246(4) . ? C4 O1 1.264(4) . ? C5 O4 1.264(4) . ? C5 O3 1.266(4) . ? C6 N3 1.319(4) . ? C6 N4 1.348(4) . ? C6 H6 0.9110 . ? C7 C8 1.377(5) . ? C7 N3 1.385(4) . ? C7 C10 1.475(4) . ? C8 N4 1.374(4) . ? C8 C9 1.495(4) . ? C9 O6 1.245(4) . ? C9 O5 1.266(4) . ? C10 O7 1.245(4) . ? C10 O8 1.280(4) . ? S O10 1.465(2) . ? S O11 1.471(2) . ? S O9 1.478(3) . ? S O12 1.483(2) . ? N1 H1 0.8744 . ? N2 La1 2.670(3) 8_655 ? N3 La2 2.681(3) 3_545 ? N4 H4 0.8575 . ? O1 La1 2.567(2) 5_675 ? O3 La1 2.604(2) 8_655 ? O6 La2 2.477(2) 6_556 ? O7 La2 2.514(2) 6_556 ? O8 La1 2.556(2) 3_545 ? O8 La2 2.628(2) 3_545 ? O9 La2 2.526(3) 1_655 ? O1W H12 0.8021 . ? O1W H11 0.7431 . ? O2W H21 0.7047 . ? O2W H22 0.6375 . ? 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 La1 O2W 81.03(8) . . ? O2 La1 O12 87.41(8) . . ? O2W La1 O12 137.24(8) . . ? O2 La1 O8 131.14(8) . 3 ? O2W La1 O8 69.55(8) . 3 ? O12 La1 O8 88.78(8) . 3 ? O2 La1 O1 74.94(8) . 5_675 ? O2W La1 O1 142.43(7) . 5_675 ? O12 La1 O1 70.45(8) . 5_675 ? O8 La1 O1 146.94(7) 3 5_675 ? O2 La1 O4 69.26(7) . . ? O2W La1 O4 68.89(8) . . ? O12 La1 O4 68.50(8) . . ? O8 La1 O4 64.13(7) 3 . ? O1 La1 O4 125.69(7) 5_675 . ? O2 La1 O3 126.40(7) . 8_665 ? O2W La1 O3 88.40(8) . 8_665 ? O12 La1 O3 130.01(8) . 8_665 ? O8 La1 O3 91.70(7) 3 8_665 ? O1 La1 O3 83.28(7) 5_675 8_665 ? O4 La1 O3 151.03(7) . 8_665 ? O2 La1 O1W 143.19(8) . . ? O2W La1 O1W 135.73(8) . . ? O12 La1 O1W 64.44(8) . . ? O8 La1 O1W 74.35(8) 3 . ? O1 La1 O1W 73.53(8) 5_675 . ? O4 La1 O1W 116.33(7) . . ? O3 La1 O1W 67.68(7) 8_665 . ? O2 La1 N2 66.68(8) . 8_665 ? O2W La1 N2 72.76(8) . 8_665 ? O12 La1 N2 138.19(8) . 8_665 ? O8 La1 N2 133.02(8) 3 8_665 ? O1 La1 N2 71.36(8) 5_675 8_665 ? O4 La1 N2 124.72(8) . 8_665 ? O3 La1 N2 60.01(8) 8_665 8_665 ? O1W La1 N2 118.95(8) . 8_665 ? O11 La2 O5 148.53(8) . . ? O11 La2 O6 77.18(8) . 6_656 ? O5 La2 O6 74.65(8) . 6_656 ? O11 La2 O7 79.77(8) . 6_656 ? O5 La2 O7 77.59(8) . 6_656 ? O6 La2 O7 69.78(8) 6_656 6_656 ? O11 La2 O9 134.60(8) . 1_455 ? O5 La2 O9 76.81(8) . 1_455 ? O6 La2 O9 142.88(8) 6_656 1_455 ? O7 La2 O9 125.81(8) 6_656 1_455 ? O11 La2 O8 70.74(8) . 3 ? O5 La2 O8 135.21(8) . 3 ? O6 La2 O8 115.76(8) 6_656 3 ? O7 La2 O8 147.07(8) 6_656 3 ? O9 La2 O8 71.02(8) 1_455 3 ? O11 La2 N3 94.84(8) . 3 ? O5 La2 N3 88.41(8) . 3 ? O6 La2 N3 69.79(8) 6_656 3 ? O7 La2 N3 139.40(8) 6_656 3 ? O9 La2 N3 86.28(8) 1_455 3 ? O8 La2 N3 59.66(8) 3 3 ? O11 La2 O3 93.28(7) . . ? O5 La2 O3 93.88(8) . . ? O6 La2 O3 129.49(8) 6_656 . ? O7 La2 O3 59.71(7) 6_656 . ? O9 La2 O3 75.39(8) 1_455 . ? O8 La2 O3 106.85(7) 3 . ? N3 La2 O3 160.45(8) 3 . ? O11 La2 O4 69.70(8) . . ? O5 La2 O4 134.00(8) . . ? O6 La2 O4 145.82(8) 6_656 . ? O7 La2 O4 95.69(7) 6_656 . ? O9 La2 O4 70.81(8) 1_455 . ? O8 La2 O4 60.84(7) 3 . ? N3 La2 O4 120.32(8) 3 . ? O3 La2 O4 47.14(7) . . ? O11 La2 C5 78.38(8) . . ? O5 La2 C5 116.04(8) . . ? O6 La2 C5 140.25(8) 6_656 . ? O7 La2 C5 75.38(8) 6_656 . ? O9 La2 C5 74.46(8) 1_455 . ? O8 La2 C5 84.44(8) 3 . ? N3 La2 C5 143.39(8) 3 . ? O3 La2 C5 23.75(7) . . ? O4 La2 C5 23.74(7) . . ? N2 C1 N1 111.4(3) . . ? N2 C1 H1A 126.8 . . ? N1 C1 H1A 121.7 . . ? C3 C2 N2 108.9(3) . . ? C3 C2 C5 134.8(3) . . ? N2 C2 C5 115.8(3) . . ? N1 C3 C2 105.9(3) . . ? N1 C3 C4 119.6(3) . . ? C2 C3 C4 134.5(3) . . ? O2 C4 O1 125.2(3) . . ? O2 C4 C3 117.8(3) . . ? O1 C4 C3 117.1(3) . . ? O4 C5 O3 121.3(3) . . ? O4 C5 C2 123.1(3) . . ? O3 C5 C2 115.6(3) . . ? O4 C5 La2 61.65(16) . . ? O3 C5 La2 61.06(16) . . ? C2 C5 La2 167.9(2) . . ? N3 C6 N4 111.3(3) . . ? N3 C6 H6 123.3 . . ? N4 C6 H6 125.3 . . ? C8 C7 N3 110.3(3) . . ? C8 C7 C10 133.3(3) . . ? N3 C7 C10 116.1(3) . . ? N4 C8 C7 104.5(3) . . ? N4 C8 C9 119.9(3) . . ? C7 C8 C9 135.6(3) . . ? O6 C9 O5 124.8(3) . . ? O6 C9 C8 119.9(3) . . ? O5 C9 C8 115.3(3) . . ? O7 C10 O8 122.9(3) . . ? O7 C10 C7 121.6(3) . . ? O8 C10 C7 115.6(3) . . ? O10 S O11 110.38(15) . . ? O10 S O9 110.94(15) . . ? O11 S O9 108.94(14) . . ? O10 S O12 108.68(14) . . ? O11 S O12 110.25(15) . . ? O9 S O12 107.60(14) . . ? C1 N1 C3 107.6(3) . . ? C1 N1 H1 126.6 . . ? C3 N1 H1 125.4 . . ? C1 N2 C2 106.2(3) . . ? C1 N2 La1 132.1(2) . 8_655 ? C2 N2 La1 120.5(2) . 8_655 ? C6 N3 C7 105.2(3) . . ? C6 N3 La2 134.7(2) . 3_545 ? C7 N3 La2 119.9(2) . 3_545 ? C6 N4 C8 108.6(3) . . ? C6 N4 H4 127.3 . . ? C8 N4 H4 124.2 . . ? C4 O1 La1 130.8(2) . 5_675 ? C4 O2 La1 163.5(2) . . ? C5 O3 La1 127.0(2) . 8_655 ? C5 O3 La2 95.19(19) . . ? La1 O3 La2 131.25(9) 8_655 . ? C5 O4 La1 151.5(2) . . ? C5 O4 La2 94.61(18) . . ? La1 O4 La2 112.58(8) . . ? C9 O5 La2 142.7(2) . . ? C9 O6 La2 152.3(2) . 6_556 ? C10 O7 La2 142.7(2) . 6_556 ? C10 O8 La1 115.8(2) . 3_545 ? C10 O8 La2 125.6(2) . 3_545 ? La1 O8 La2 118.44(9) 3_545 3_545 ? S O9 La2 142.74(15) . 1_655 ? S O11 La2 146.89(15) . . ? S O12 La1 134.74(14) . . ? La1 O1W H12 106.0 . . ? La1 O1W H11 106.0 . . ? H12 O1W H11 106.8 . . ? La1 O2W H21 113.7 . . ? La1 O2W H22 137.0 . . ? H21 O2W H22 103.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.109 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.129 # Attachment '2-CCDC-604059-122(GdS).cif' data_122 _database_code_depnum_ccdc_archive 'CCDC 604059' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H10 Gd2 N2 O16 S2' _chemical_formula_weight 732.77 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 9.4691(6) _cell_length_b 13.4407(7) _cell_length_c 12.7749(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.155(3) _cell_angle_gamma 90.00 _cell_volume 1569.33(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4766 _cell_measurement_theta_min 3.1005 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 8.739 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.190 _exptl_absorpt_correction_T_min 0.174 _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 dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11768 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3563 _reflns_number_gt 3331 _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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3563 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0434 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Gd1 Gd 0.921600(16) 0.221957(11) 0.202722(13) 0.00418(5) Uani 1 1 d . . . Gd2 Gd 0.308833(17) 0.142974(12) -0.119809(14) 0.00511(5) Uani 1 1 d . . . S1 S 1.01727(9) 0.25705(6) 0.48922(7) 0.00599(16) Uani 1 1 d . . . S2 S 0.60639(8) 0.12606(6) 0.12339(7) 0.00623(16) Uani 1 1 d . . . N1 N 0.7646(3) 0.3726(2) 0.1746(2) 0.0067(6) Uani 1 1 d . . . N2 N 0.5948(3) 0.4882(2) 0.1313(2) 0.0069(6) Uani 1 1 d . . . H1 H 0.501(5) 0.518(4) 0.104(4) 0.046(15) Uiso 1 1 d . . . C1 C 0.6232(4) 0.3903(2) 0.1331(3) 0.0080(7) Uani 1 1 d . . . H1A H 0.5530 0.3413 0.1085 0.010 Uiso 1 1 calc R . . C2 C 0.8288(3) 0.4646(2) 0.2025(3) 0.0055(6) Uani 1 1 d . . . C3 C 0.7236(3) 0.5378(2) 0.1753(3) 0.0070(7) Uani 1 1 d . . . C4 C 0.9900(3) 0.4686(2) 0.2508(3) 0.0070(7) Uani 1 1 d . . . C5 C 0.7199(4) 0.6470(2) 0.1765(3) 0.0076(7) Uani 1 1 d . . . O1 O 1.0566(2) 0.54981(17) 0.2621(2) 0.0090(5) Uani 1 1 d . . . O2 O 1.0514(2) 0.38454(17) 0.27929(19) 0.0065(5) Uani 1 1 d . . . O3 O 0.6062(2) 0.68624(18) 0.1172(2) 0.0117(5) Uani 1 1 d . . . O4 O 0.8257(2) 0.70005(17) 0.23015(19) 0.0069(5) Uani 1 1 d . . . O12 O 0.4638(2) 0.16378(18) 0.0621(2) 0.0089(5) Uani 1 1 d . . . O11 O 0.7191(2) 0.15412(18) 0.0658(2) 0.0089(5) Uani 1 1 d . . . O10 O 0.6565(3) 0.17437(18) 0.2310(2) 0.0100(5) Uani 1 1 d . . . O9 O 0.6013(2) 0.01796(18) 0.1357(2) 0.0101(5) Uani 1 1 d . . . O8 O 0.9886(2) 0.35331(17) 0.5369(2) 0.0093(5) Uani 1 1 d . . . O7 O 0.9139(3) 0.23947(18) 0.3825(2) 0.0100(5) Uani 1 1 d . . . O6 O 1.1690(2) 0.25453(18) 0.4803(2) 0.0087(5) Uani 1 1 d . . . O5 O 0.9937(3) 0.17980(18) 0.5657(2) 0.0105(5) Uani 1 1 d . . . O1W O 0.7122(3) 0.4465(2) -0.0876(3) 0.0161(6) Uani 1 1 d . . . H11 H 0.706(5) 0.408(4) -0.134(4) 0.021(13) Uiso 1 1 d . . . H12 H 0.777(6) 0.424(4) -0.044(5) 0.050(19) Uiso 1 1 d . . . O2W O 0.5594(3) 0.1562(2) -0.1476(2) 0.0115(5) Uani 1 1 d . . . H21 H 0.622(6) 0.166(4) -0.096(5) 0.044(18) Uiso 1 1 d . . . H22 H 0.568(6) 0.211(5) -0.187(5) 0.056(19) Uiso 1 1 d . . . O3W O 0.2100(3) 0.0355(2) -0.0047(2) 0.0113(5) Uani 1 1 d . . . H31 H 0.150(6) 0.050(5) 0.023(5) 0.07(2) Uiso 1 1 d . . . H32 H 0.203(6) -0.016(5) -0.017(5) 0.05(2) Uiso 1 1 d . . . O4W O 0.3036(3) 0.1293(2) -0.3115(2) 0.0135(6) Uani 1 1 d . . . H41 H 0.258(5) 0.161(4) -0.354(4) 0.025(14) Uiso 1 1 d . . . H42 H 0.291(6) 0.064(5) -0.334(5) 0.07(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.00446(8) 0.00377(9) 0.00387(9) 0.00005(6) 0.00027(6) 0.00055(5) Gd2 0.00433(8) 0.00447(9) 0.00583(9) -0.00004(6) 0.00010(7) 0.00005(5) S1 0.0056(4) 0.0080(4) 0.0043(4) 0.0001(3) 0.0013(3) -0.0008(3) S2 0.0050(4) 0.0053(4) 0.0073(4) -0.0001(3) -0.0002(3) 0.0005(3) N1 0.0068(13) 0.0061(14) 0.0064(15) -0.0017(11) 0.0005(12) -0.0013(10) N2 0.0050(13) 0.0054(14) 0.0109(16) -0.0002(12) 0.0029(12) 0.0010(10) C1 0.0092(15) 0.0050(16) 0.0091(18) 0.0005(13) 0.0012(14) -0.0010(12) C2 0.0068(15) 0.0043(15) 0.0059(17) 0.0005(13) 0.0027(13) -0.0021(12) C3 0.0042(14) 0.0076(17) 0.0089(18) -0.0023(13) 0.0008(13) -0.0011(12) C4 0.0088(16) 0.0087(17) 0.0047(17) -0.0010(13) 0.0038(14) 0.0007(12) C5 0.0078(15) 0.0079(17) 0.0085(18) 0.0002(13) 0.0048(14) 0.0012(12) O1 0.0066(11) 0.0051(12) 0.0153(14) -0.0001(10) 0.0028(10) -0.0010(9) O2 0.0062(11) 0.0052(11) 0.0073(12) 0.0002(9) 0.0000(10) 0.0019(8) O3 0.0063(11) 0.0064(12) 0.0203(15) 0.0011(11) -0.0004(10) 0.0012(9) O4 0.0078(11) 0.0067(11) 0.0065(12) -0.0007(9) 0.0024(10) -0.0013(9) O12 0.0061(11) 0.0105(12) 0.0089(13) 0.0005(10) 0.0000(10) 0.0013(9) O11 0.0061(11) 0.0112(12) 0.0096(13) -0.0006(10) 0.0025(10) -0.0021(9) O10 0.0127(12) 0.0067(12) 0.0085(13) -0.0024(10) -0.0010(10) -0.0010(9) O9 0.0091(11) 0.0074(12) 0.0132(13) -0.0001(10) 0.0017(10) -0.0008(9) O8 0.0093(12) 0.0092(13) 0.0103(13) -0.0017(10) 0.0043(10) -0.0002(9) O7 0.0075(11) 0.0172(13) 0.0034(13) -0.0006(10) -0.0018(10) -0.0040(9) O6 0.0062(11) 0.0085(12) 0.0110(13) -0.0035(10) 0.0016(10) 0.0001(9) O5 0.0162(13) 0.0084(13) 0.0075(13) 0.0019(10) 0.0044(11) 0.0005(9) O1W 0.0188(15) 0.0162(15) 0.0127(15) -0.0007(13) 0.0029(13) 0.0042(11) O2W 0.0094(13) 0.0132(14) 0.0114(15) 0.0001(11) 0.0019(12) -0.0019(10) O3W 0.0124(13) 0.0075(14) 0.0147(15) 0.0002(11) 0.0047(11) -0.0003(10) O4W 0.0127(13) 0.0169(15) 0.0091(14) 0.0002(12) -0.0004(11) 0.0075(11) _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 Gd1 O7 2.329(2) . ? Gd1 O4 2.340(2) 2_745 ? Gd1 O1 2.356(2) 2_745 ? Gd1 O11 2.412(2) . ? Gd1 O5 2.429(2) 4_565 ? Gd1 N1 2.482(3) . ? Gd1 O2 2.572(2) . ? Gd1 O8 2.573(2) 4_565 ? Gd1 O10 2.704(2) . ? Gd1 S1 3.1034(9) 4_565 ? Gd1 S2 3.1648(8) . ? Gd2 O9 2.352(2) 3_655 ? Gd2 O3W 2.417(3) . ? Gd2 O12 2.418(2) . ? Gd2 O3 2.430(2) 3_665 ? Gd2 O4W 2.443(3) . ? Gd2 O2 2.470(2) 4_465 ? Gd2 O6 2.485(2) 4_465 ? Gd2 O2W 2.496(3) . ? Gd2 O4 2.669(2) 3_665 ? Gd2 C5 2.909(3) 3_665 ? S1 O6 1.471(2) . ? S1 O7 1.474(3) . ? S1 O5 1.482(3) . ? S1 O8 1.485(2) . ? S1 Gd1 3.1034(9) 4_566 ? S2 O12 1.463(2) . ? S2 O9 1.464(2) . ? S2 O10 1.481(3) . ? S2 O11 1.495(2) . ? N1 C1 1.326(4) . ? N1 C2 1.383(4) . ? N2 C1 1.343(4) . ? N2 C3 1.375(4) . ? N2 H1 0.95(5) . ? C1 H1A 0.9300 . ? C2 C3 1.378(4) . ? C2 C4 1.490(4) . ? C3 C5 1.468(5) . ? C4 O1 1.250(4) . ? C4 O2 1.279(4) . ? C5 O3 1.259(4) . ? C5 O4 1.274(4) . ? C5 Gd2 2.909(3) 3_665 ? O1 Gd1 2.356(2) 2_755 ? O2 Gd2 2.470(2) 4_666 ? O3 Gd2 2.430(2) 3_665 ? O4 Gd1 2.340(2) 2_755 ? O4 Gd2 2.669(2) 3_665 ? O9 Gd2 2.352(2) 3_655 ? O8 Gd1 2.573(2) 4_566 ? O6 Gd2 2.485(2) 4_666 ? O5 Gd1 2.429(2) 4_566 ? O1W H11 0.77(5) . ? O1W H12 0.78(6) . ? O2W H21 0.77(6) . ? O2W H22 0.91(6) . ? O3W H31 0.77(6) . ? O3W H32 0.70(6) . ? O4W H41 0.73(5) . ? O4W H42 0.93(7) . ? 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 O7 Gd1 O4 86.78(8) . 2_745 ? O7 Gd1 O1 86.26(9) . 2_745 ? O4 Gd1 O1 77.06(8) 2_745 2_745 ? O7 Gd1 O11 122.00(8) . . ? O4 Gd1 O11 139.58(8) 2_745 . ? O1 Gd1 O11 77.33(8) 2_745 . ? O7 Gd1 O5 137.99(8) . 4_565 ? O4 Gd1 O5 83.08(8) 2_745 4_565 ? O1 Gd1 O5 130.12(8) 2_745 4_565 ? O11 Gd1 O5 90.15(8) . 4_565 ? O7 Gd1 N1 83.58(9) . . ? O4 Gd1 N1 132.24(9) 2_745 . ? O1 Gd1 N1 148.01(8) 2_745 . ? O11 Gd1 N1 82.58(8) . . ? O5 Gd1 N1 73.92(9) 4_565 . ? O7 Gd1 O2 70.97(8) . . ? O4 Gd1 O2 68.06(8) 2_745 . ? O1 Gd1 O2 138.82(8) 2_745 . ? O11 Gd1 O2 143.85(8) . . ? O5 Gd1 O2 67.41(8) 4_565 . ? N1 Gd1 O2 64.56(8) . . ? O7 Gd1 O8 158.44(8) . 4_565 ? O4 Gd1 O8 78.67(8) 2_745 4_565 ? O1 Gd1 O8 75.09(8) 2_745 4_565 ? O11 Gd1 O8 64.81(8) . 4_565 ? O5 Gd1 O8 56.21(8) 4_565 4_565 ? N1 Gd1 O8 117.98(8) . 4_565 ? O2 Gd1 O8 116.82(7) . 4_565 ? O7 Gd1 O10 67.86(8) . . ? O4 Gd1 O10 144.81(8) 2_745 . ? O1 Gd1 O10 77.32(7) 2_745 . ? O11 Gd1 O10 54.38(8) . . ? O5 Gd1 O10 132.09(8) 4_565 . ? N1 Gd1 O10 70.75(8) . . ? O2 Gd1 O10 121.20(7) . . ? O8 Gd1 O10 117.02(7) 4_565 . ? O7 Gd1 S1 161.64(6) . 4_565 ? O4 Gd1 S1 80.10(6) 2_745 4_565 ? O1 Gd1 S1 103.05(6) 2_745 4_565 ? O11 Gd1 S1 75.89(6) . 4_565 ? O5 Gd1 S1 27.81(6) 4_565 4_565 ? N1 Gd1 S1 95.76(7) . 4_565 ? O2 Gd1 S1 92.11(5) . 4_565 ? O8 Gd1 S1 28.40(5) 4_565 4_565 ? O10 Gd1 S1 129.28(5) . 4_565 ? O7 Gd1 S2 95.00(6) . . ? O4 Gd1 S2 148.72(6) 2_745 . ? O1 Gd1 S2 71.91(6) 2_745 . ? O11 Gd1 S2 27.02(6) . . ? O5 Gd1 S2 114.19(6) 4_565 . ? N1 Gd1 S2 78.85(6) . . ? O2 Gd1 S2 141.69(5) . . ? O8 Gd1 S2 89.50(5) 4_565 . ? O10 Gd1 S2 27.85(5) . . ? S1 Gd1 S2 102.89(2) 4_565 . ? O9 Gd2 O3W 73.09(9) 3_655 . ? O9 Gd2 O12 92.70(8) 3_655 . ? O3W Gd2 O12 73.68(9) . . ? O9 Gd2 O3 138.08(8) 3_655 3_665 ? O3W Gd2 O3 137.36(10) . 3_665 ? O12 Gd2 O3 76.23(8) . 3_665 ? O9 Gd2 O4W 75.95(9) 3_655 . ? O3W Gd2 O4W 130.91(10) . . ? O12 Gd2 O4W 145.08(8) . . ? O3 Gd2 O4W 90.28(10) 3_665 . ? O9 Gd2 O2 98.46(8) 3_655 4_465 ? O3W Gd2 O2 75.02(8) . 4_465 ? O12 Gd2 O2 141.91(8) . 4_465 ? O3 Gd2 O2 115.26(8) 3_665 4_465 ? O4W Gd2 O2 72.97(8) . 4_465 ? O9 Gd2 O6 143.87(8) 3_655 4_465 ? O3W Gd2 O6 71.04(9) . 4_465 ? O12 Gd2 O6 73.28(8) . 4_465 ? O3 Gd2 O6 71.83(8) 3_665 4_465 ? O4W Gd2 O6 133.15(9) . 4_465 ? O2 Gd2 O6 76.43(8) 4_465 4_465 ? O9 Gd2 O2W 70.99(8) 3_655 . ? O3W Gd2 O2W 131.49(9) . . ? O12 Gd2 O2W 76.57(9) . . ? O3 Gd2 O2W 67.12(8) 3_665 . ? O4W Gd2 O2W 68.51(9) . . ? O2 Gd2 O2W 141.45(9) 4_465 . ? O6 Gd2 O2W 133.50(8) 4_465 . ? O9 Gd2 O4 144.56(8) 3_655 3_665 ? O3W Gd2 O4 125.90(8) . 3_665 ? O12 Gd2 O4 120.14(8) . 3_665 ? O3 Gd2 O4 51.03(7) 3_665 3_665 ? O4W Gd2 O4 69.41(8) . 3_665 ? O2 Gd2 O4 64.71(7) 4_465 3_665 ? O6 Gd2 O4 65.71(7) 4_465 3_665 ? O2W Gd2 O4 102.07(8) . 3_665 ? O9 Gd2 C5 152.02(9) 3_655 3_665 ? O3W Gd2 C5 134.86(10) . 3_665 ? O12 Gd2 C5 96.93(9) . 3_665 ? O3 Gd2 C5 25.29(8) 3_665 3_665 ? O4W Gd2 C5 81.23(10) . 3_665 ? O2 Gd2 C5 90.00(8) 4_465 3_665 ? O6 Gd2 C5 64.05(9) 4_465 3_665 ? O2W Gd2 C5 85.78(9) . 3_665 ? O4 Gd2 C5 25.94(8) 3_665 3_665 ? O6 S1 O7 110.53(15) . . ? O6 S1 O5 110.69(14) . . ? O7 S1 O5 108.61(14) . . ? O6 S1 O8 109.77(14) . . ? O7 S1 O8 111.75(14) . . ? O5 S1 O8 105.38(15) . . ? O6 S1 Gd1 125.82(11) . 4_566 ? O7 S1 Gd1 123.46(10) . 4_566 ? O5 S1 Gd1 49.87(10) . 4_566 ? O8 S1 Gd1 55.53(10) . 4_566 ? O12 S2 O9 110.50(14) . . ? O12 S2 O10 111.82(14) . . ? O9 S2 O10 110.29(15) . . ? O12 S2 O11 109.08(14) . . ? O9 S2 O11 110.56(14) . . ? O10 S2 O11 104.44(14) . . ? O12 S2 Gd1 133.74(10) . . ? O9 S2 Gd1 115.11(10) . . ? O10 S2 Gd1 58.51(10) . . ? O11 S2 Gd1 47.15(9) . . ? C1 N1 C2 105.8(3) . . ? C1 N1 Gd1 135.1(2) . . ? C2 N1 Gd1 119.1(2) . . ? C1 N2 C3 108.5(3) . . ? C1 N2 H1 126(3) . . ? C3 N2 H1 126(3) . . ? N1 C1 N2 111.1(3) . . ? N1 C1 H1A 124.5 . . ? N2 C1 H1A 124.5 . . ? C3 C2 N1 109.5(3) . . ? C3 C2 C4 132.3(3) . . ? N1 C2 C4 118.2(3) . . ? N2 C3 C2 105.2(3) . . ? N2 C3 C5 117.9(3) . . ? C2 C3 C5 136.8(3) . . ? O1 C4 O2 124.1(3) . . ? O1 C4 C2 120.7(3) . . ? O2 C4 C2 115.2(3) . . ? O3 C5 O4 121.2(3) . . ? O3 C5 C3 115.5(3) . . ? O4 C5 C3 123.2(3) . . ? O3 C5 Gd2 55.55(17) . 3_665 ? O4 C5 Gd2 66.46(18) . 3_665 ? C3 C5 Gd2 165.5(3) . 3_665 ? C4 O1 Gd1 153.7(2) . 2_755 ? C4 O2 Gd2 126.4(2) . 4_666 ? C4 O2 Gd1 120.4(2) . . ? Gd2 O2 Gd1 112.31(9) 4_666 . ? C5 O3 Gd2 99.2(2) . 3_665 ? C5 O4 Gd1 148.5(2) . 2_755 ? C5 O4 Gd2 87.60(19) . 3_665 ? Gd1 O4 Gd2 113.29(9) 2_755 3_665 ? S2 O12 Gd2 135.84(15) . . ? S2 O11 Gd1 105.83(13) . . ? S2 O10 Gd1 93.64(12) . . ? S2 O9 Gd2 151.74(15) . 3_655 ? S1 O8 Gd1 96.07(12) . 4_566 ? S1 O7 Gd1 138.05(14) . . ? S1 O6 Gd2 133.61(14) . 4_666 ? S1 O5 Gd1 102.32(13) . 4_566 ? H11 O1W H12 100(5) . . ? Gd2 O2W H21 116(4) . . ? Gd2 O2W H22 112(3) . . ? H21 O2W H22 100(5) . . ? Gd2 O3W H31 126(5) . . ? Gd2 O3W H32 119(5) . . ? H31 O3W H32 108(6) . . ? Gd2 O4W H41 123(4) . . ? Gd2 O4W H42 110(4) . . ? H41 O4W H42 109(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.647 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.156 # Attachment '3a-CCDC-604060-164(GdS).cif' data_164 _database_code_depnum_ccdc_archive 'CCDC 604060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H10 Gd2 N2 O16 S2' _chemical_formula_weight 732.79 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 6.6363(2) _cell_length_b 13.3817(5) _cell_length_c 18.9960(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.7120(10) _cell_angle_gamma 90.00 _cell_volume 1615.69(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 69 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 26.23 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .35 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 8.488 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.142 _exptl_absorpt_correction_T_max 0.428 _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 'Siemems-Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.5 _diffrn_reflns_number 8525 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.03 _reflns_number_total 3198 _reflns_number_gt 2777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _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^)+(0.0227P)^2^+15.4675P] 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 3198 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.000 _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 Gd1 Gd 0.45501(5) -0.30401(2) -0.290679(16) 0.01212(10) Uani 1 1 d . . . Gd2 Gd -0.19441(5) -0.16680(2) -0.101373(16) 0.01146(10) Uani 1 1 d . . . S1 S 0.0310(3) -0.28495(14) -0.23929(10) 0.0221(4) Uani 1 1 d . . . S2 S 0.2483(2) -0.40058(11) -0.44346(8) 0.0120(3) Uani 1 1 d . . . O2 O 0.5865(7) -0.1422(3) -0.2296(2) 0.0165(10) Uani 1 1 d . . . O5 O 0.1600(10) -0.3762(5) -0.2324(3) 0.0450(16) Uani 1 1 d . . . O6 O 0.0253(8) -0.2488(4) -0.1658(3) 0.0229(11) Uani 1 1 d . . . O7 O -0.1835(7) -0.3015(4) -0.2861(3) 0.0230(11) Uani 1 1 d . . . O8 O 0.1413(9) -0.2102(5) -0.2728(3) 0.0416(16) Uani 1 1 d . . . O9 O 0.1511(7) -0.3517(3) -0.5150(2) 0.0162(9) Uani 1 1 d . . . O10 O 0.4720(7) -0.3702(4) -0.4136(2) 0.0174(10) Uani 1 1 d . . . O11 O 0.1447(7) -0.3635(4) -0.3872(2) 0.0180(10) Uani 1 1 d . . . O12 O 0.2297(8) -0.5094(3) -0.4516(3) 0.0207(10) Uani 1 1 d . . . N1 N 0.4048(9) -0.1528(4) -0.3746(3) 0.0190(12) Uani 1 1 d . . . N2 N 0.2728(9) -0.0368(4) -0.4589(3) 0.0198(12) Uani 1 1 d . . . H2A H 0.2170 -0.0098 -0.5011 0.07(3) Uiso 1 1 d R . . C1 C 0.3166(12) -0.1347(5) -0.4462(4) 0.0209(15) Uani 1 1 d . . . H1A H 0.2894 -0.1835 -0.4825 0.015(18) Uiso 1 1 d R . . C2 C 0.3332(10) 0.0125(5) -0.3923(3) 0.0144(13) Uani 1 1 d . . . C3 C 0.4153(10) -0.0611(5) -0.3403(3) 0.0129(13) Uani 1 1 d . . . O1W O -0.1446(12) -0.0355(7) -0.3903(4) 0.075(3) Uani 1 1 d . . . H11 H -0.2707 -0.0140 -0.3814 0.800 Uiso 1 1 d R . . H12 H -0.1620 -0.0971 -0.4145 0.800 Uiso 1 1 d R . . O2W O -0.5634(8) -0.1483(5) -0.1042(3) 0.0357(14) Uani 1 1 d . . . H21 H -0.6787 -0.1816 -0.1303 0.800 Uiso 1 1 d R . . H22 H -0.6079 -0.0851 -0.0936 0.800 Uiso 1 1 d R . . O3W O -0.2407(8) -0.2005(4) 0.0213(3) 0.0263(11) Uani 1 1 d . . . H31 H -0.1297 -0.1823 0.0589 0.800 Uiso 1 1 d R . . H32 H -0.3585 -0.1794 0.0303 0.800 Uiso 1 1 d R . . O4W O 0.0000(8) -0.0435(4) -0.1581(3) 0.0278(12) Uani 1 1 d . . . H41 H 0.0006 0.0232 -0.1702 0.800 Uiso 1 1 d R . . H42 H 0.0248 -0.0795 -0.1967 0.800 Uiso 1 1 d R . . C5 C 0.2817(10) 0.1204(5) -0.3898(3) 0.0149(13) Uani 1 1 d . . . O3 O 0.1355(8) 0.1542(4) -0.4415(3) 0.0244(11) Uani 1 1 d . . . O4 O 0.3864(7) 0.1779(3) -0.3376(2) 0.0172(10) Uani 1 1 d . . . C4 C 0.5083(10) -0.0579(4) -0.2586(3) 0.0121(12) Uani 1 1 d . . . O1 O 0.5080(8) 0.0198(3) -0.2230(2) 0.0185(10) 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 Gd1 0.01271(17) 0.00903(16) 0.01116(17) 0.00014(11) -0.00207(12) -0.00106(11) Gd2 0.01050(16) 0.01061(16) 0.01148(16) -0.00200(11) 0.00029(12) -0.00025(11) S1 0.0128(8) 0.0325(10) 0.0197(9) -0.0112(7) 0.0027(7) -0.0007(7) S2 0.0133(7) 0.0105(7) 0.0099(7) 0.0005(6) -0.0003(6) -0.0028(6) O2 0.019(2) 0.012(2) 0.017(2) 0.0004(18) 0.0014(19) 0.0010(19) O5 0.041(4) 0.052(4) 0.034(3) -0.015(3) -0.001(3) 0.019(3) O6 0.019(2) 0.030(3) 0.019(2) -0.011(2) 0.004(2) 0.001(2) O7 0.011(2) 0.034(3) 0.022(3) -0.007(2) 0.002(2) -0.003(2) O8 0.032(3) 0.050(4) 0.050(4) -0.019(3) 0.023(3) -0.023(3) O9 0.016(2) 0.018(2) 0.012(2) 0.0010(18) -0.0012(18) -0.0034(19) O10 0.010(2) 0.022(2) 0.018(2) -0.0005(19) 0.0007(18) -0.0044(19) O11 0.017(2) 0.021(2) 0.014(2) -0.0021(19) 0.0013(18) 0.001(2) O12 0.029(3) 0.011(2) 0.019(2) -0.0021(19) 0.003(2) -0.003(2) N1 0.026(3) 0.016(3) 0.012(3) 0.001(2) 0.001(2) 0.001(2) N2 0.028(3) 0.015(3) 0.011(3) -0.002(2) -0.003(2) -0.004(2) C1 0.035(4) 0.011(3) 0.010(3) -0.003(3) -0.003(3) -0.003(3) C2 0.015(3) 0.010(3) 0.015(3) -0.001(2) -0.001(3) -0.001(2) C3 0.022(3) 0.007(3) 0.009(3) -0.001(2) 0.003(2) -0.001(2) O1W 0.048(5) 0.113(7) 0.066(5) 0.033(5) 0.020(4) -0.001(5) O2W 0.011(2) 0.067(4) 0.027(3) -0.014(3) 0.002(2) 0.000(3) O3W 0.024(3) 0.031(3) 0.025(3) 0.002(2) 0.008(2) 0.003(2) O4W 0.030(3) 0.021(3) 0.031(3) 0.004(2) 0.007(2) 0.002(2) C5 0.018(3) 0.013(3) 0.013(3) 0.001(3) 0.003(3) -0.004(3) O3 0.029(3) 0.020(3) 0.016(3) -0.001(2) -0.007(2) 0.002(2) O4 0.018(2) 0.014(2) 0.014(2) -0.0024(18) -0.0035(18) -0.0027(19) C4 0.012(3) 0.008(3) 0.016(3) 0.001(2) 0.003(2) -0.007(2) O1 0.025(3) 0.013(2) 0.014(2) -0.0018(19) 0.0009(19) -0.0018(19) _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 Gd1 O4 2.372(4) 2_644 ? Gd1 O7 2.376(5) 1_655 ? Gd1 O1 2.378(4) 2_644 ? Gd1 O11 2.463(4) . ? Gd1 O2 2.492(4) . ? Gd1 O10 2.531(4) . ? Gd1 O8 2.536(6) . ? Gd1 N1 2.538(6) . ? Gd1 O5 2.691(7) . ? Gd1 S2 3.1121(15) . ? Gd1 S1 3.2430(17) . ? Gd2 O12 2.374(5) 2_554 ? Gd2 O9 2.418(4) 4_556 ? Gd2 O6 2.419(5) . ? Gd2 O2W 2.446(5) . ? Gd2 O2 2.474(4) 1_455 ? Gd2 O3W 2.478(5) . ? Gd2 O4W 2.519(5) . ? Gd2 O3 2.525(5) 2_544 ? Gd2 O4 2.537(5) 2_544 ? Gd2 C5 2.902(6) 2_544 ? S1 O7 1.462(5) . ? S1 O5 1.475(6) . ? S1 O8 1.487(6) . ? S1 O6 1.489(5) . ? S2 O12 1.466(5) . ? S2 O9 1.478(5) . ? S2 O10 1.485(4) . ? S2 O11 1.510(5) . ? O2 C4 1.296(8) . ? O2 Gd2 2.474(4) 1_655 ? O7 Gd1 2.376(5) 1_455 ? O9 Gd2 2.418(4) 4 ? O12 Gd2 2.374(5) 2_544 ? N1 C1 1.338(9) . ? N1 C3 1.381(8) . ? N2 C1 1.349(9) . ? N2 C2 1.380(8) . ? N2 H2A 0.8600 . ? C1 H1A 0.9300 . ? C2 C3 1.391(9) . ? C2 C5 1.487(9) . ? C3 C4 1.497(9) . ? O1W H11 0.9457 . ? O1W H12 0.9344 . ? O2W H21 0.9015 . ? O2W H22 0.9366 . ? O3W H31 0.9001 . ? O3W H32 0.8927 . ? O4W H41 0.9216 . ? O4W H42 0.9310 . ? C5 O3 1.250(8) . ? C5 O4 1.290(8) . ? C5 Gd2 2.902(6) 2_554 ? O3 Gd2 2.525(5) 2_554 ? O4 Gd1 2.372(4) 2_654 ? O4 Gd2 2.537(5) 2_554 ? C4 O1 1.241(8) . ? O1 Gd1 2.378(4) 2_654 ? 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 O4 Gd1 O7 79.55(17) 2_644 1_655 ? O4 Gd1 O1 77.60(15) 2_644 2_644 ? O7 Gd1 O1 86.46(17) 1_655 2_644 ? O4 Gd1 O11 139.53(16) 2_644 . ? O7 Gd1 O11 130.62(16) 1_655 . ? O1 Gd1 O11 78.37(16) 2_644 . ? O4 Gd1 O2 67.55(15) 2_644 . ? O7 Gd1 O2 75.89(16) 1_655 . ? O1 Gd1 O2 143.08(15) 2_644 . ? O11 Gd1 O2 137.17(15) . . ? O4 Gd1 O10 141.98(15) 2_644 . ? O7 Gd1 O10 74.11(15) 1_655 . ? O1 Gd1 O10 73.91(15) 2_644 . ? O11 Gd1 O10 56.57(14) . . ? O2 Gd1 O10 129.14(15) . . ? O4 Gd1 O8 92.98(18) 2_644 . ? O7 Gd1 O8 147.93(18) 1_655 . ? O1 Gd1 O8 122.64(18) 2_644 . ? O11 Gd1 O8 73.56(17) . . ? O2 Gd1 O8 72.46(16) . . ? O10 Gd1 O8 123.56(17) . . ? O4 Gd1 N1 131.75(17) 2_644 . ? O7 Gd1 N1 87.76(19) 1_655 . ? O1 Gd1 N1 148.23(16) 2_644 . ? O11 Gd1 N1 81.92(17) . . ? O2 Gd1 N1 64.22(16) . . ? O10 Gd1 N1 74.46(17) . . ? O8 Gd1 N1 74.0(2) . . ? O4 Gd1 O5 72.60(17) 2_644 . ? O7 Gd1 O5 146.77(18) 1_655 . ? O1 Gd1 O5 70.34(18) 2_644 . ? O11 Gd1 O5 68.85(16) . . ? O2 Gd1 O5 108.59(17) . . ? O10 Gd1 O5 119.02(16) . . ? O8 Gd1 O5 53.14(19) . . ? N1 Gd1 O5 124.40(19) . . ? O4 Gd1 S2 149.52(11) 2_644 . ? O7 Gd1 S2 102.11(12) 1_655 . ? O1 Gd1 S2 72.17(11) 2_644 . ? O11 Gd1 S2 28.51(11) . . ? O2 Gd1 S2 142.77(11) . . ? O10 Gd1 S2 28.19(10) . . ? O8 Gd1 S2 99.88(14) . . ? N1 Gd1 S2 78.60(13) . . ? O5 Gd1 S2 93.28(13) . . ? O4 Gd1 S1 82.29(12) 2_644 . ? O7 Gd1 S1 160.45(12) 1_655 . ? O1 Gd1 S1 96.69(12) 2_644 . ? O11 Gd1 S1 68.76(11) . . ? O2 Gd1 S1 90.54(11) . . ? O10 Gd1 S1 125.32(10) . . ? O8 Gd1 S1 26.37(14) . . ? N1 Gd1 S1 99.07(14) . . ? O5 Gd1 S1 26.78(14) . . ? S2 Gd1 S1 97.21(4) . . ? O12 Gd2 O9 79.13(16) 2_554 4_556 ? O12 Gd2 O6 139.80(17) 2_554 . ? O9 Gd2 O6 78.34(15) 4_556 . ? O12 Gd2 O2W 72.49(19) 2_554 . ? O9 Gd2 O2W 138.77(16) 4_556 . ? O6 Gd2 O2W 141.26(17) . . ? O12 Gd2 O2 101.41(15) 2_554 1_455 ? O9 Gd2 O2 146.00(15) 4_556 1_455 ? O6 Gd2 O2 80.29(15) . 1_455 ? O2W Gd2 O2 70.35(17) . 1_455 ? O12 Gd2 O3W 73.08(17) 2_554 . ? O9 Gd2 O3W 74.34(16) 4_556 . ? O6 Gd2 O3W 130.45(17) . . ? O2W Gd2 O3W 69.20(18) . . ? O2 Gd2 O3W 138.89(16) 1_455 . ? O12 Gd2 O4W 74.07(17) 2_554 . ? O9 Gd2 O4W 73.80(16) 4_556 . ? O6 Gd2 O4W 67.87(17) . . ? O2W Gd2 O4W 123.8(2) . . ? O2 Gd2 O4W 73.76(16) 1_455 . ? O3W Gd2 O4W 137.62(17) . . ? O12 Gd2 O3 136.87(16) 2_554 2_544 ? O9 Gd2 O3 81.33(15) 4_556 2_544 ? O6 Gd2 O3 70.92(17) . 2_544 ? O2W Gd2 O3 99.5(2) . 2_544 ? O2 Gd2 O3 115.89(15) 1_455 2_544 ? O3W Gd2 O3 64.73(16) . 2_544 ? O4W Gd2 O3 135.12(17) . 2_544 ? O12 Gd2 O4 145.32(16) 2_554 2_544 ? O9 Gd2 O4 130.35(15) 4_556 2_544 ? O6 Gd2 O4 72.18(16) . 2_544 ? O2W Gd2 O4 72.85(18) . 2_544 ? O2 Gd2 O4 65.35(14) 1_455 2_544 ? O3W Gd2 O4 95.67(16) . 2_544 ? O4W Gd2 O4 126.35(16) . 2_544 ? O3 Gd2 O4 51.76(14) 2_544 2_544 ? O12 Gd2 C5 148.50(17) 2_554 2_544 ? O9 Gd2 C5 105.91(17) 4_556 2_544 ? O6 Gd2 C5 70.43(18) . 2_544 ? O2W Gd2 C5 85.2(2) . 2_544 ? O2 Gd2 C5 91.28(16) 1_455 2_544 ? O3W Gd2 C5 78.40(17) . 2_544 ? O4W Gd2 C5 137.42(17) . 2_544 ? O3 Gd2 C5 25.45(16) 2_544 2_544 ? O4 Gd2 C5 26.35(16) 2_544 2_544 ? O7 S1 O5 111.5(3) . . ? O7 S1 O8 110.8(3) . . ? O5 S1 O8 104.5(4) . . ? O7 S1 O6 109.7(3) . . ? O5 S1 O6 110.9(3) . . ? O8 S1 O6 109.4(3) . . ? O7 S1 Gd1 125.6(2) . . ? O5 S1 Gd1 55.3(3) . . ? O8 S1 Gd1 49.2(3) . . ? O6 S1 Gd1 124.5(2) . . ? O12 S2 O9 110.0(3) . . ? O12 S2 O10 110.9(3) . . ? O9 S2 O10 110.7(3) . . ? O12 S2 O11 111.1(3) . . ? O9 S2 O11 109.7(3) . . ? O10 S2 O11 104.4(3) . . ? O12 S2 Gd1 120.8(2) . . ? O9 S2 Gd1 129.19(19) . . ? O10 S2 Gd1 53.60(18) . . ? O11 S2 Gd1 51.13(18) . . ? C4 O2 Gd2 125.7(4) . 1_655 ? C4 O2 Gd1 121.0(4) . . ? Gd2 O2 Gd1 111.78(17) 1_655 . ? S1 O5 Gd1 98.0(4) . . ? S1 O6 Gd2 143.5(3) . . ? S1 O7 Gd1 145.2(3) . 1_455 ? S1 O8 Gd1 104.4(3) . . ? S2 O9 Gd2 138.3(3) . 4 ? S2 O10 Gd1 98.2(2) . . ? S2 O11 Gd1 100.4(2) . . ? S2 O12 Gd2 148.4(3) . 2_544 ? C1 N1 C3 105.5(5) . . ? C1 N1 Gd1 136.2(5) . . ? C3 N1 Gd1 115.6(4) . . ? C1 N2 C2 108.0(5) . . ? C1 N2 H2A 126.0 . . ? C2 N2 H2A 126.0 . . ? N1 C1 N2 111.5(6) . . ? N1 C1 H1A 124.2 . . ? N2 C1 H1A 124.3 . . ? N2 C2 C3 105.3(5) . . ? N2 C2 C5 118.9(6) . . ? C3 C2 C5 135.4(6) . . ? N1 C3 C2 109.8(5) . . ? N1 C3 C4 117.7(5) . . ? C2 C3 C4 132.6(6) . . ? H11 O1W H12 111.4 . . ? Gd2 O2W H21 130.4 . . ? Gd2 O2W H22 117.6 . . ? H21 O2W H22 107.1 . . ? Gd2 O3W H31 113.7 . . ? Gd2 O3W H32 118.3 . . ? H31 O3W H32 108.9 . . ? Gd2 O4W H41 141.3 . . ? Gd2 O4W H42 103.1 . . ? H41 O4W H42 106.9 . . ? O3 C5 O4 120.9(6) . . ? O3 C5 C2 117.4(6) . . ? O4 C5 C2 121.7(6) . . ? O3 C5 Gd2 60.2(3) . 2_554 ? O4 C5 Gd2 60.9(3) . 2_554 ? C2 C5 Gd2 174.1(4) . 2_554 ? C5 O3 Gd2 94.4(4) . 2_554 ? C5 O4 Gd1 146.4(4) . 2_654 ? C5 O4 Gd2 92.8(4) . 2_554 ? Gd1 O4 Gd2 113.70(18) 2_654 2_554 ? O1 C4 O2 124.1(6) . . ? O1 C4 C3 121.6(6) . . ? O2 C4 C3 114.3(5) . . ? C4 O1 Gd1 151.0(4) . 2_654 ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.930 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.180 # Attachment '3b-CCDC-604061-147(EuS).cif' data_147 _database_code_depnum_ccdc_archive 'CCDC 604061' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H10 Eu2 N2 O16 S2' _chemical_formula_weight 722.21 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' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 6.6022(5) _cell_length_b 13.3235(9) _cell_length_c 18.8797(12) _cell_angle_alpha 90.00 _cell_angle_beta 106.618(3) _cell_angle_gamma 90.00 _cell_volume 1591.38(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4557 _cell_measurement_theta_min 3.0585 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.1800 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 8.166 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.442 _exptl_absorpt_correction_T_min 0.390 _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 dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12133 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3631 _reflns_number_gt 3417 _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^)+(0.0415P)^2^+3.3841P] 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 3631 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.45137(4) -0.304522(17) -0.290493(12) 0.01100(8) Uani 1 1 d . . . Eu2 Eu -0.19537(3) -0.166995(17) -0.101465(12) 0.01080(8) Uani 1 1 d . . . S1 S 0.02948(19) -0.28462(10) -0.24005(7) 0.0174(3) Uani 1 1 d . . . S2 S 0.24717(17) -0.40069(8) -0.44357(6) 0.0115(2) Uani 1 1 d . . . O2 O 0.5845(5) -0.1425(3) -0.23011(18) 0.0157(7) Uani 1 1 d . . . O5 O 0.1604(7) -0.3753(3) -0.2332(2) 0.0308(9) Uani 1 1 d . . . O6 O 0.0253(6) -0.2495(3) -0.16599(19) 0.0215(8) Uani 1 1 d . . . O7 O -0.1858(6) -0.3031(3) -0.2867(2) 0.0214(8) Uani 1 1 d . . . O8 O 0.1357(7) -0.2085(3) -0.2744(2) 0.0329(10) Uani 1 1 d . . . O9 O 0.1509(5) -0.3515(3) -0.51506(18) 0.0149(7) Uani 1 1 d . . . O10 O 0.4694(5) -0.3704(3) -0.41401(18) 0.0173(7) Uani 1 1 d . . . O11 O 0.1428(5) -0.3643(3) -0.38778(18) 0.0158(7) Uani 1 1 d . . . O12 O 0.2284(6) -0.5095(3) -0.45172(19) 0.0198(8) Uani 1 1 d . . . N1 N 0.4040(7) -0.1531(3) -0.3754(2) 0.0154(8) Uani 1 1 d . . . N2 N 0.2729(7) -0.0369(3) -0.4586(2) 0.0191(9) Uani 1 1 d . . . H2A H 0.2148 -0.0098 -0.5009 0.029(17) Uiso 1 1 d R . . C1 C 0.3209(9) -0.1346(4) -0.4462(3) 0.0206(11) Uani 1 1 d . . . H1A H 0.2979 -0.1831 -0.4831 0.06(3) Uiso 1 1 d R . . C2 C 0.3325(7) 0.0119(4) -0.3922(3) 0.0139(9) Uani 1 1 d . . . C3 C 0.4143(7) -0.0611(4) -0.3407(2) 0.0128(9) Uani 1 1 d . . . O1W O -0.1429(9) -0.0338(5) -0.3897(3) 0.0685(18) Uani 1 1 d . . . O2W O -0.5661(6) -0.1475(4) -0.1050(2) 0.0361(11) Uani 1 1 d . . . O3W O -0.2430(6) -0.2007(3) 0.0214(2) 0.0258(9) Uani 1 1 d . . . O4W O -0.0008(6) -0.0439(3) -0.1592(2) 0.0252(8) Uani 1 1 d . . . H11 H -0.2696 -0.0106 -0.3813 0.800 Uiso 1 1 d R . . H12 H -0.1609 -0.0937 -0.4144 0.800 Uiso 1 1 d R . . H21 H -0.6767 -0.1825 -0.1312 0.800 Uiso 1 1 d R . . H22 H -0.6059 -0.0860 -0.0944 0.800 Uiso 1 1 d R . . H31 H -0.1283 -0.1832 0.0578 0.800 Uiso 1 1 d R . . H32 H -0.3571 -0.1803 0.0292 0.800 Uiso 1 1 d R . . H41 H 0.0013 0.0223 -0.1706 0.800 Uiso 1 1 d R . . H42 H 0.0255 -0.0804 -0.1971 0.800 Uiso 1 1 d R . . C5 C 0.2825(7) 0.1194(3) -0.3903(2) 0.0129(9) Uani 1 1 d . . . O3 O 0.1353(6) 0.1541(3) -0.44151(19) 0.0224(8) Uani 1 1 d . . . O4 O 0.3876(6) 0.1766(3) -0.33808(19) 0.0159(7) Uani 1 1 d . . . C4 C 0.5057(7) -0.0586(3) -0.2592(3) 0.0121(9) Uani 1 1 d . . . O1 O 0.5064(6) 0.0195(3) -0.22303(18) 0.0171(7) 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 0.00965(13) 0.01151(13) 0.00963(13) 0.00014(8) -0.00081(9) -0.00084(8) Eu2 0.00841(13) 0.01304(13) 0.00980(13) -0.00192(8) 0.00078(9) -0.00025(8) S1 0.0094(6) 0.0258(6) 0.0168(6) -0.0084(5) 0.0033(5) -0.0013(5) S2 0.0109(5) 0.0129(5) 0.0087(5) 0.0009(4) -0.0003(4) -0.0016(4) O2 0.0165(18) 0.0155(16) 0.0115(16) -0.0005(13) -0.0017(13) 0.0000(13) O5 0.030(2) 0.035(2) 0.024(2) -0.0082(17) 0.0036(17) 0.0112(18) O6 0.0193(19) 0.028(2) 0.0174(18) -0.0088(15) 0.0054(15) -0.0003(15) O7 0.0065(17) 0.037(2) 0.0179(18) -0.0074(15) -0.0013(14) -0.0030(14) O8 0.030(2) 0.038(2) 0.036(2) -0.0066(19) 0.0168(19) -0.0159(19) O9 0.0113(16) 0.0204(17) 0.0093(15) 0.0033(13) -0.0026(13) -0.0001(13) O10 0.0093(16) 0.0277(19) 0.0124(16) 0.0015(14) -0.0010(13) -0.0052(14) O11 0.0135(17) 0.0222(18) 0.0113(16) -0.0045(13) 0.0030(13) 0.0017(14) O12 0.029(2) 0.0138(17) 0.0142(16) 0.0012(13) 0.0030(15) -0.0038(15) N1 0.019(2) 0.0132(19) 0.0115(19) -0.0016(15) 0.0009(16) -0.0033(16) N2 0.027(2) 0.015(2) 0.012(2) 0.0001(15) 0.0004(17) -0.0002(17) C1 0.030(3) 0.015(2) 0.015(2) -0.0009(19) 0.003(2) 0.000(2) C2 0.010(2) 0.016(2) 0.013(2) -0.0009(17) 0.0004(17) 0.0021(17) C3 0.013(2) 0.014(2) 0.009(2) 0.0002(17) 0.0000(17) -0.0027(17) O1W 0.045(3) 0.107(5) 0.056(4) 0.026(3) 0.019(3) -0.001(3) O2W 0.0105(19) 0.071(3) 0.026(2) -0.012(2) 0.0036(16) 0.0018(19) O3W 0.024(2) 0.033(2) 0.023(2) 0.0014(16) 0.0110(17) 0.0016(16) O4W 0.026(2) 0.0204(19) 0.031(2) 0.0069(15) 0.0102(17) 0.0027(15) C5 0.012(2) 0.014(2) 0.011(2) -0.0016(17) 0.0009(17) -0.0029(17) O3 0.027(2) 0.0184(18) 0.0140(18) -0.0006(13) -0.0064(15) 0.0026(15) O4 0.0153(18) 0.0172(17) 0.0127(16) -0.0046(13) -0.0002(14) 0.0009(13) C4 0.010(2) 0.011(2) 0.015(2) 0.0002(17) 0.0034(18) -0.0025(17) O1 0.0201(18) 0.0163(17) 0.0138(16) -0.0007(13) 0.0030(14) 0.0015(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 Eu1 O1 2.366(3) 2_644 ? Eu1 O4 2.368(3) 2_644 ? Eu1 O7 2.376(4) 1_655 ? Eu1 O11 2.453(3) . ? Eu1 O2 2.481(3) . ? Eu1 O10 2.526(3) . ? Eu1 O8 2.537(5) . ? Eu1 N1 2.539(4) . ? Eu1 O5 2.634(5) . ? Eu1 S2 3.0957(11) . ? Eu1 S1 3.2021(13) . ? Eu1 Eu2 4.0954(4) 1_655 ? Eu2 O12 2.363(3) 2_554 ? Eu2 O9 2.412(3) 4_556 ? Eu2 O6 2.415(4) . ? Eu2 O2W 2.443(4) . ? Eu2 O3W 2.469(4) . ? Eu2 O2 2.470(3) 1_455 ? Eu2 O3 2.513(4) 2_544 ? Eu2 O4W 2.516(4) . ? Eu2 O4 2.535(3) 2_544 ? Eu2 C5 2.899(5) 2_544 ? Eu2 Eu1 4.0954(4) 1_455 ? S1 O7 1.463(4) . ? S1 O5 1.470(4) . ? S1 O6 1.482(4) . ? S1 O8 1.483(4) . ? S2 O12 1.459(4) . ? S2 O10 1.470(3) . ? S2 O9 1.471(3) . ? S2 O11 1.495(3) . ? O2 C4 1.288(6) . ? O2 Eu2 2.470(3) 1_655 ? O7 Eu1 2.376(4) 1_455 ? O9 Eu2 2.412(3) 4 ? O12 Eu2 2.363(3) 2_544 ? N1 C1 1.316(6) . ? N1 C3 1.382(6) . ? N2 C1 1.344(6) . ? N2 C2 1.367(6) . ? N2 H2A 0.8599 . ? C1 H1A 0.9302 . ? C2 C3 1.372(6) . ? C2 C5 1.473(6) . ? C3 C4 1.484(6) . ? O1W H11 0.9468 . ? O1W H12 0.9148 . ? O2W H21 0.8881 . ? O2W H22 0.9001 . ? O3W H31 0.8959 . ? O3W H32 0.8528 . ? O4W H41 0.9095 . ? O4W H42 0.9215 . ? C5 O3 1.247(6) . ? C5 O4 1.281(6) . ? C5 Eu2 2.899(5) 2_554 ? O3 Eu2 2.513(4) 2_554 ? O4 Eu1 2.368(3) 2_654 ? O4 Eu2 2.535(3) 2_554 ? C4 O1 1.244(6) . ? O1 Eu1 2.366(3) 2_654 ? 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 O4 77.27(11) 2_644 2_644 ? O1 Eu1 O7 85.28(13) 2_644 1_655 ? O4 Eu1 O7 79.43(13) 2_644 1_655 ? O1 Eu1 O11 78.82(12) 2_644 . ? O4 Eu1 O11 140.00(12) 2_644 . ? O7 Eu1 O11 129.75(12) 1_655 . ? O1 Eu1 O2 142.84(11) 2_644 . ? O4 Eu1 O2 68.00(11) 2_644 . ? O7 Eu1 O2 75.98(12) 1_655 . ? O11 Eu1 O2 137.36(11) . . ? O1 Eu1 O10 73.76(12) 2_644 . ? O4 Eu1 O10 141.57(12) 2_644 . ? O7 Eu1 O10 73.58(11) 1_655 . ? O11 Eu1 O10 56.25(11) . . ? O2 Eu1 O10 128.47(11) . . ? O1 Eu1 O8 124.22(13) 2_644 . ? O4 Eu1 O8 94.24(14) 2_644 . ? O7 Eu1 O8 148.01(13) 1_655 . ? O11 Eu1 O8 73.67(12) . . ? O2 Eu1 O8 72.62(12) . . ? O10 Eu1 O8 122.90(12) . . ? O1 Eu1 N1 147.63(12) 2_644 . ? O4 Eu1 N1 132.02(12) 2_644 . ? O7 Eu1 N1 87.37(14) 1_655 . ? O11 Eu1 N1 81.92(12) . . ? O2 Eu1 N1 64.06(12) . . ? O10 Eu1 N1 73.92(12) . . ? O8 Eu1 N1 73.62(14) . . ? O1 Eu1 O5 71.23(12) 2_644 . ? O4 Eu1 O5 72.99(12) 2_644 . ? O7 Eu1 O5 146.90(13) 1_655 . ? O11 Eu1 O5 69.15(12) . . ? O2 Eu1 O5 109.08(12) . . ? O10 Eu1 O5 119.16(12) . . ? O8 Eu1 O5 53.89(13) . . ? N1 Eu1 O5 124.81(13) . . ? O1 Eu1 S2 72.36(8) 2_644 . ? O4 Eu1 S2 149.41(9) 2_644 . ? O7 Eu1 S2 101.40(9) 1_655 . ? O11 Eu1 S2 28.35(8) . . ? O2 Eu1 S2 142.32(8) . . ? O10 Eu1 S2 28.04(8) . . ? O8 Eu1 S2 99.64(10) . . ? N1 Eu1 S2 78.32(9) . . ? O5 Eu1 S2 93.50(9) . . ? O1 Eu1 S1 97.80(9) 2_644 . ? O4 Eu1 S1 82.97(9) 2_644 . ? O7 Eu1 S1 161.01(9) 1_655 . ? O11 Eu1 S1 69.07(8) . . ? O2 Eu1 S1 90.87(9) . . ? O10 Eu1 S1 125.32(8) . . ? O8 Eu1 S1 26.90(10) . . ? N1 Eu1 S1 99.28(10) . . ? O5 Eu1 S1 26.99(9) . . ? S2 Eu1 S1 97.37(3) . . ? O1 Eu1 Eu2 109.22(8) 2_644 1_655 ? O4 Eu1 Eu2 34.68(8) 2_644 1_655 ? O7 Eu1 Eu2 69.64(9) 1_655 1_655 ? O11 Eu1 Eu2 160.34(8) . 1_655 ? O2 Eu1 Eu2 34.09(8) . 1_655 ? O10 Eu1 Eu2 142.59(8) . 1_655 ? O8 Eu1 Eu2 87.27(10) . 1_655 ? N1 Eu1 Eu2 97.54(9) . 1_655 ? O5 Eu1 Eu2 95.91(9) . 1_655 ? S2 Eu1 Eu2 170.45(2) . 1_655 ? S1 Eu1 Eu2 91.77(2) . 1_655 ? O12 Eu2 O9 78.86(12) 2_554 4_556 ? O12 Eu2 O6 139.56(13) 2_554 . ? O9 Eu2 O6 78.21(11) 4_556 . ? O12 Eu2 O2W 72.77(15) 2_554 . ? O9 Eu2 O2W 139.12(12) 4_556 . ? O6 Eu2 O2W 141.16(13) . . ? O12 Eu2 O3W 73.17(13) 2_554 . ? O9 Eu2 O3W 74.58(13) 4_556 . ? O6 Eu2 O3W 130.41(13) . . ? O2W Eu2 O3W 69.46(14) . . ? O12 Eu2 O2 101.59(12) 2_554 1_455 ? O9 Eu2 O2 146.02(12) 4_556 1_455 ? O6 Eu2 O2 80.46(12) . 1_455 ? O2W Eu2 O2 69.88(13) . 1_455 ? O3W Eu2 O2 138.63(13) . 1_455 ? O12 Eu2 O3 136.93(12) 2_554 2_544 ? O9 Eu2 O3 81.21(12) 4_556 2_544 ? O6 Eu2 O3 70.65(13) . 2_544 ? O2W Eu2 O3 100.01(15) . 2_544 ? O3W Eu2 O3 64.84(13) . 2_544 ? O2 Eu2 O3 115.90(11) 1_455 2_544 ? O12 Eu2 O4W 74.10(13) 2_554 . ? O9 Eu2 O4W 73.97(12) 4_556 . ? O6 Eu2 O4W 67.76(13) . . ? O2W Eu2 O4W 123.42(15) . . ? O3W Eu2 O4W 138.06(13) . . ? O2 Eu2 O4W 73.59(12) 1_455 . ? O3 Eu2 O4W 134.86(13) 2_544 . ? O12 Eu2 O4 145.69(13) 2_554 2_544 ? O9 Eu2 O4 130.11(11) 4_556 2_544 ? O6 Eu2 O4 72.26(12) . 2_544 ? O2W Eu2 O4 72.92(14) . 2_544 ? O3W Eu2 O4 95.24(12) . 2_544 ? O2 Eu2 O4 65.64(11) 1_455 2_544 ? O3 Eu2 O4 51.54(11) 2_544 2_544 ? O4W Eu2 O4 126.34(12) . 2_544 ? O12 Eu2 C5 148.61(13) 2_554 2_544 ? O9 Eu2 C5 105.78(12) 4_556 2_544 ? O6 Eu2 C5 70.42(13) . 2_544 ? O2W Eu2 C5 85.46(16) . 2_544 ? O3W Eu2 C5 78.18(13) . 2_544 ? O2 Eu2 C5 91.41(12) 1_455 2_544 ? O3 Eu2 C5 25.38(12) 2_544 2_544 ? O4W Eu2 C5 137.27(13) . 2_544 ? O4 Eu2 C5 26.20(11) 2_544 2_544 ? O12 Eu2 Eu1 131.97(9) 2_554 1_455 ? O9 Eu2 Eu1 145.96(8) 4_556 1_455 ? O6 Eu2 Eu1 68.41(8) . 1_455 ? O2W Eu2 Eu1 72.99(10) . 1_455 ? O3W Eu2 Eu1 122.90(10) . 1_455 ? O2 Eu2 Eu1 34.28(8) 1_455 1_455 ? O3 Eu2 Eu1 81.65(8) 2_544 1_455 ? O4W Eu2 Eu1 98.51(9) . 1_455 ? O4 Eu2 Eu1 32.11(7) 2_544 1_455 ? C5 Eu2 Eu1 57.25(9) 2_544 1_455 ? O7 S1 O5 111.1(2) . . ? O7 S1 O6 110.1(2) . . ? O5 S1 O6 110.2(2) . . ? O7 S1 O8 110.6(3) . . ? O5 S1 O8 105.1(3) . . ? O6 S1 O8 109.6(2) . . ? O7 S1 Eu1 125.82(16) . . ? O5 S1 Eu1 54.43(19) . . ? O6 S1 Eu1 124.00(15) . . ? O8 S1 Eu1 50.70(19) . . ? O12 S2 O10 111.0(2) . . ? O12 S2 O9 110.1(2) . . ? O10 S2 O9 110.4(2) . . ? O12 S2 O11 110.7(2) . . ? O10 S2 O11 104.8(2) . . ? O9 S2 O11 109.7(2) . . ? O12 S2 Eu1 120.72(15) . . ? O10 S2 Eu1 53.89(14) . . ? O9 S2 Eu1 129.10(15) . . ? O11 S2 Eu1 51.20(13) . . ? C4 O2 Eu2 125.9(3) . 1_655 ? C4 O2 Eu1 120.8(3) . . ? Eu2 O2 Eu1 111.63(13) 1_655 . ? S1 O5 Eu1 98.6(2) . . ? S1 O6 Eu2 142.8(2) . . ? S1 O7 Eu1 144.8(2) . 1_455 ? S1 O8 Eu1 102.4(2) . . ? S2 O9 Eu2 138.0(2) . 4 ? S2 O10 Eu1 98.07(17) . . ? S2 O11 Eu1 100.45(17) . . ? S2 O12 Eu2 148.5(2) . 2_544 ? C1 N1 C3 105.3(4) . . ? C1 N1 Eu1 137.0(3) . . ? C3 N1 Eu1 115.2(3) . . ? C1 N2 C2 108.0(4) . . ? C1 N2 H2A 126.1 . . ? C2 N2 H2A 125.9 . . ? N1 C1 N2 111.6(4) . . ? N1 C1 H1A 124.2 . . ? N2 C1 H1A 124.2 . . ? N2 C2 C3 105.3(4) . . ? N2 C2 C5 118.5(4) . . ? C3 C2 C5 135.9(4) . . ? C2 C3 N1 109.7(4) . . ? C2 C3 C4 132.8(4) . . ? N1 C3 C4 117.5(4) . . ? H11 O1W H12 112.2 . . ? Eu2 O2W H21 128.1 . . ? Eu2 O2W H22 116.4 . . ? H21 O2W H22 110.8 . . ? Eu2 O3W H31 111.5 . . ? Eu2 O3W H32 117.4 . . ? H31 O3W H32 112.2 . . ? Eu2 O4W H41 141.2 . . ? Eu2 O4W H42 103.1 . . ? H41 O4W H42 108.0 . . ? O3 C5 O4 120.5(4) . . ? O3 C5 C2 118.1(4) . . ? O4 C5 C2 121.4(4) . . ? O3 C5 Eu2 59.8(3) . 2_554 ? O4 C5 Eu2 60.9(2) . 2_554 ? C2 C5 Eu2 174.9(3) . 2_554 ? C5 O3 Eu2 94.9(3) . 2_554 ? C5 O4 Eu1 146.8(3) . 2_654 ? C5 O4 Eu2 92.9(3) . 2_554 ? Eu1 O4 Eu2 113.22(13) 2_654 2_554 ? O1 C4 O2 123.7(4) . . ? O1 C4 C3 121.6(4) . . ? O2 C4 C3 114.7(4) . . ? C4 O1 Eu1 150.5(3) . 2_654 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.885 _refine_diff_density_min -2.341 _refine_diff_density_rms 0.198 # Attachment '4-CCDC-604062-160(EuCu).cif' data_syq-160 _database_code_depnum_ccdc_archive 'CCDC 604062' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 Cu Eu6 N8 O54 S6' _chemical_formula_weight 2420.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 6.6280(5) _cell_length_b 9.4648(7) _cell_length_c 21.5033(15) _cell_angle_alpha 96.778(2) _cell_angle_beta 94.307(4) _cell_angle_gamma 97.886(4) _cell_volume 1321.14(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3751 _cell_measurement_theta_min 3.0910 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1147 _exptl_absorpt_coefficient_mu 7.791 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.459 _exptl_absorpt_correction_T_min 0.256 _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 dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10190 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5932 _reflns_number_gt 5340 _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^)+(0.0388P)^2^+3.1974P] 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 5932 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.93626(4) 0.11837(3) 0.321871(11) 0.01092(7) Uani 1 1 d . . . Eu2 Eu 0.65242(4) -0.29082(2) 0.422202(11) 0.01019(7) Uani 1 1 d . . . Eu3 Eu 1.67536(4) -0.01347(3) 0.138756(12) 0.01554(8) Uani 1 1 d . . . Cu Cu 1.0000 0.5000 0.0000 0.0180(2) Uani 1 2 d S . . S1 S 1.2323(2) 0.06525(15) 0.18550(6) 0.0182(3) Uani 1 1 d . . . S2 S 1.33150(19) 0.35751(13) 0.43562(5) 0.0110(2) Uani 1 1 d . . . S3 S 1.15329(19) -0.18125(13) 0.37622(6) 0.0125(2) Uani 1 1 d . . . C1 C 1.0796(9) 0.6167(6) 0.1493(3) 0.0208(11) Uani 1 1 d . . . H1A H 1.1444 0.7105 0.1498 0.025 Uiso 1 1 calc R . . C2 C 0.9280(8) 0.4011(5) 0.1174(2) 0.0143(10) Uani 1 1 d . . . C3 C 0.9421(8) 0.4170(6) 0.1822(2) 0.0149(10) Uani 1 1 d . . . C4 C 0.8903(8) 0.3198(5) 0.2303(2) 0.0147(10) Uani 1 1 d . . . C5 C 0.8214(8) 0.2886(5) 0.0675(2) 0.0155(10) Uani 1 1 d . . . C6 C 0.4776(8) -0.5286(5) 0.2819(2) 0.0166(11) Uani 1 1 d . . . H6A H 0.4311 -0.6049 0.3032 0.020 Uiso 1 1 calc R . . C7 C 0.5516(8) -0.4047(5) 0.2044(2) 0.0134(10) Uani 1 1 d . . . C8 C 0.6018(8) -0.3187(5) 0.2612(2) 0.0135(10) Uani 1 1 d . . . C9 C 0.5662(8) -0.3836(6) 0.1374(2) 0.0160(10) Uani 1 1 d . . . C10 C 0.7015(7) -0.1688(5) 0.2806(2) 0.0121(9) Uani 1 1 d . . . N1 N 1.0159(7) 0.5261(5) 0.0975(2) 0.0170(9) Uani 1 1 d . . . N2 N 1.0379(7) 0.5548(5) 0.2008(2) 0.0173(9) Uani 1 1 d . . . H2A H 1.0666 0.5950 0.2390 0.021 Uiso 1 1 calc R . . N3 N 0.4743(7) -0.5370(5) 0.2190(2) 0.0163(9) Uani 1 1 d . . . H3A H 0.4311 -0.6125 0.1925 0.020 Uiso 1 1 calc R . . N4 N 0.5549(7) -0.3986(4) 0.30956(19) 0.0138(9) Uani 1 1 d . . . O1 O 0.9510(6) 0.3646(4) 0.28647(18) 0.0224(9) Uani 1 1 d . . . O2 O 0.7955(6) 0.1929(4) 0.21474(17) 0.0160(7) Uani 1 1 d . . . O3 O 0.7257(7) 0.1748(4) 0.08115(19) 0.0245(9) Uani 1 1 d . . . O4 O 0.8271(6) 0.3147(4) 0.01171(17) 0.0216(9) Uani 1 1 d . . . O5 O 0.5301(7) -0.4940(4) 0.09811(18) 0.0238(9) Uani 1 1 d . . . O6 O 0.6156(7) -0.2597(4) 0.12448(18) 0.0258(9) Uani 1 1 d . . . O7 O 0.7708(6) -0.0866(4) 0.24256(16) 0.0146(7) Uani 1 1 d . . . O8 O 0.7221(5) -0.1254(4) 0.33919(16) 0.0143(7) Uani 1 1 d . . . O9 O 1.1905(6) 0.1247(4) 0.24923(18) 0.0223(9) Uani 1 1 d . . . O10 O 1.3346(10) 0.1772(6) 0.1542(2) 0.0603(19) Uani 1 1 d . . . O11 O 1.3701(7) -0.0432(6) 0.1923(2) 0.0441(13) Uani 1 1 d . . . O12 O 1.0418(6) -0.0032(5) 0.14949(18) 0.0252(9) Uani 1 1 d . . . O13 O 1.4908(6) 0.2846(4) 0.46372(19) 0.0227(8) Uani 1 1 d . . . O14 O 1.4127(6) 0.4994(4) 0.42151(18) 0.0203(8) Uani 1 1 d . . . O15 O 1.2281(6) 0.2709(4) 0.37810(16) 0.0181(8) Uani 1 1 d . . . O16 O 1.1811(6) 0.3705(4) 0.48352(16) 0.0158(7) Uani 1 1 d . . . O17 O 1.0088(6) -0.2047(5) 0.42445(19) 0.0234(9) Uani 1 1 d . . . O18 O 1.1528(6) -0.0336(4) 0.3602(2) 0.0300(10) Uani 1 1 d . . . O19 O 1.3586(6) -0.1873(4) 0.40534(19) 0.0226(8) Uani 1 1 d . . . O20 O 1.0970(7) -0.2856(5) 0.3212(2) 0.0365(11) Uani 1 1 d . . . O1W O 0.8425(6) -0.4977(4) 0.39729(18) 0.0252(9) Uani 1 1 d . . . O2W O 0.5713(6) 0.1353(5) 0.32367(19) 0.0253(9) Uani 1 1 d . . . O3W O 1.3964(7) -0.0690(4) 0.05513(19) 0.0259(9) Uani 1 1 d . . . O4W O 1.2634(7) 0.3867(5) 0.00165(19) 0.0317(10) Uani 1 1 d . . . O5W O 0.7250(7) -0.0579(4) 0.48745(19) 0.0280(10) Uani 1 1 d . . . O6W O 1.8267(8) -0.0951(5) 0.0340(2) 0.0343(11) Uani 1 1 d . . . O7W O 0.8475(6) 0.1856(4) 0.42874(18) 0.0202(8) Uani 1 1 d . . . H11 H 0.9044 -0.5114 0.4314 0.080 Uiso 1 1 d R . . H12 H 0.9193 -0.5131 0.3672 0.080 Uiso 1 1 d R . . H21 H 0.4949 0.1209 0.2873 0.080 Uiso 1 1 d R . . H22 H 0.4997 0.0817 0.3528 0.080 Uiso 1 1 d R . . H31 H 1.2749 -0.0692 0.0757 0.080 Uiso 1 1 d R . . H32 H 1.3996 0.0102 0.0321 0.080 Uiso 1 1 d R . . H41 H 1.3419 0.4212 0.0382 0.080 Uiso 1 1 d R . . H42 H 1.3437 0.3931 -0.0310 0.080 Uiso 1 1 d R . . H51 H 0.7929 0.0180 0.4789 0.080 Uiso 1 1 d R . . H52 H 0.6770 -0.0388 0.5227 0.080 Uiso 1 1 d R . . H61 H 1.7687 -0.1800 0.0222 0.080 Uiso 1 1 d R . . H62 H 1.9450 -0.0965 0.0488 0.080 Uiso 1 1 d R . . H72 H 0.9254 0.2489 0.4575 0.080 Uiso 1 1 d R . . H71 H 0.7201 0.2052 0.4280 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 Eu1 0.01037(13) 0.01428(12) 0.00768(12) -0.00170(9) 0.00249(9) 0.00211(9) Eu2 0.01023(13) 0.01337(12) 0.00671(12) -0.00094(9) 0.00237(9) 0.00182(9) Eu3 0.01839(15) 0.01679(13) 0.00953(13) 0.00147(9) 0.00009(10) -0.00328(10) Cu 0.0244(5) 0.0184(4) 0.0098(4) 0.0002(3) 0.0042(4) -0.0019(4) S1 0.0133(6) 0.0276(7) 0.0109(6) -0.0055(5) 0.0052(5) -0.0017(5) S2 0.0113(6) 0.0150(5) 0.0062(5) -0.0003(4) 0.0023(4) 0.0001(4) S3 0.0103(6) 0.0157(6) 0.0116(6) -0.0004(4) 0.0029(5) 0.0034(4) C1 0.019(3) 0.019(3) 0.024(3) -0.001(2) 0.004(2) 0.002(2) C2 0.015(3) 0.015(2) 0.013(2) 0.0000(19) 0.004(2) 0.0035(19) C3 0.014(3) 0.020(2) 0.011(2) -0.0015(19) 0.0031(19) 0.004(2) C4 0.018(3) 0.018(2) 0.009(2) -0.0005(19) 0.003(2) 0.005(2) C5 0.022(3) 0.016(2) 0.010(2) 0.0010(18) 0.007(2) 0.006(2) C6 0.026(3) 0.013(2) 0.011(2) 0.0011(18) 0.007(2) 0.001(2) C7 0.018(3) 0.015(2) 0.006(2) -0.0064(18) -0.0006(19) 0.0062(19) C8 0.016(3) 0.014(2) 0.011(2) 0.0028(18) 0.0025(19) 0.0025(19) C9 0.018(3) 0.020(3) 0.009(2) -0.0046(19) 0.002(2) 0.006(2) C10 0.010(2) 0.015(2) 0.010(2) -0.0009(18) 0.0005(18) 0.0022(18) N1 0.021(2) 0.017(2) 0.012(2) 0.0003(16) 0.0034(18) -0.0007(18) N2 0.023(2) 0.018(2) 0.010(2) -0.0028(16) 0.0020(18) 0.0039(18) N3 0.018(2) 0.018(2) 0.009(2) -0.0045(16) 0.0019(17) -0.0019(18) N4 0.019(2) 0.017(2) 0.0045(19) 0.0033(15) 0.0043(16) -0.0028(17) O1 0.033(2) 0.0202(19) 0.0123(19) -0.0014(15) -0.0010(16) 0.0030(17) O2 0.0199(19) 0.0159(17) 0.0113(17) -0.0009(14) 0.0045(15) -0.0007(15) O3 0.035(2) 0.0205(19) 0.016(2) 0.0040(15) 0.0068(17) -0.0053(17) O4 0.032(2) 0.0199(19) 0.0086(18) -0.0027(14) 0.0031(16) -0.0068(17) O5 0.034(2) 0.024(2) 0.0113(18) -0.0039(15) 0.0028(17) 0.0014(17) O6 0.042(3) 0.0209(19) 0.0138(19) 0.0009(15) 0.0077(18) 0.0027(18) O7 0.0162(18) 0.0168(17) 0.0097(17) 0.0016(13) 0.0021(14) -0.0023(14) O8 0.0172(18) 0.0170(17) 0.0078(17) -0.0002(13) 0.0013(14) 0.0007(14) O9 0.018(2) 0.036(2) 0.0110(18) -0.0094(16) 0.0075(15) 0.0040(17) O10 0.087(4) 0.048(3) 0.028(3) -0.015(2) 0.023(3) -0.045(3) O11 0.034(3) 0.081(4) 0.020(2) -0.009(2) 0.000(2) 0.034(3) O12 0.014(2) 0.042(2) 0.016(2) -0.0084(17) 0.0010(15) -0.0006(17) O13 0.017(2) 0.028(2) 0.025(2) 0.0056(17) 0.0030(16) 0.0084(16) O14 0.029(2) 0.0168(18) 0.0131(18) 0.0016(14) 0.0028(16) -0.0040(16) O15 0.020(2) 0.0241(19) 0.0072(17) -0.0061(14) 0.0040(14) -0.0023(15) O16 0.0164(19) 0.0261(19) 0.0052(16) 0.0007(14) 0.0068(14) 0.0020(15) O17 0.0130(19) 0.040(2) 0.018(2) 0.0076(17) 0.0064(16) 0.0029(17) O18 0.018(2) 0.023(2) 0.051(3) 0.013(2) 0.001(2) 0.0043(17) O19 0.0114(19) 0.034(2) 0.024(2) 0.0050(17) 0.0019(16) 0.0093(16) O20 0.034(3) 0.044(3) 0.025(2) -0.019(2) 0.000(2) 0.006(2) O1W 0.031(2) 0.032(2) 0.015(2) -0.0005(16) 0.0052(17) 0.0136(18) O2W 0.019(2) 0.038(2) 0.020(2) -0.0004(17) 0.0014(16) 0.0113(18) O3W 0.031(2) 0.028(2) 0.016(2) -0.0020(16) -0.0039(17) 0.0007(18) O4W 0.029(2) 0.045(3) 0.015(2) -0.0070(18) 0.0065(18) -0.007(2) O5W 0.037(3) 0.024(2) 0.020(2) -0.0038(16) 0.0142(18) -0.0063(18) O6W 0.043(3) 0.033(2) 0.026(2) -0.0036(19) 0.008(2) 0.008(2) O7W 0.0161(19) 0.026(2) 0.0153(19) -0.0077(15) 0.0036(15) 0.0010(16) _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 O18 2.340(4) . ? Eu1 O9 2.382(4) . ? Eu1 O15 2.400(4) . ? Eu1 O7W 2.448(4) . ? Eu1 O2W 2.449(4) . ? Eu1 O7 2.496(3) . ? Eu1 O1 2.527(4) . ? Eu1 O8 2.619(3) . ? Eu1 O2 2.630(4) . ? Eu1 C4 2.925(5) . ? Eu1 C10 2.943(5) . ? Eu1 Eu3 4.1566(4) 1_455 ? Eu2 O19 2.320(4) 1_455 ? Eu2 O14 2.364(4) 1_445 ? Eu2 O17 2.386(4) . ? Eu2 O5W 2.437(4) . ? Eu2 O16 2.480(4) 2_756 ? Eu2 O1W 2.498(4) . ? Eu2 N4 2.515(4) . ? Eu2 O8 2.537(3) . ? Eu2 O13 2.693(4) 2_756 ? Eu2 S2 3.1909(12) 2_756 ? Eu3 O3 2.289(4) 1_655 ? Eu3 O6 2.290(4) 1_655 ? Eu3 O2 2.397(3) 1_655 ? Eu3 O11 2.402(5) . ? Eu3 O12 2.410(4) 1_655 ? Eu3 O3W 2.437(4) . ? Eu3 O7 2.477(3) 1_655 ? Eu3 O6W 2.612(5) . ? Eu3 O10 3.091(7) . ? Eu3 S1 3.3253(14) . ? Eu3 Eu1 4.1566(4) 1_655 ? Cu O4 2.012(4) . ? Cu O4 2.012(4) 2_765 ? Cu N1 2.075(4) 2_765 ? Cu N1 2.075(4) . ? Cu O4W 2.171(5) . ? Cu O4W 2.171(5) 2_765 ? S1 O10 1.441(5) . ? S1 O12 1.457(4) . ? S1 O11 1.477(5) . ? S1 O9 1.479(4) . ? S2 O14 1.452(4) . ? S2 O15 1.466(4) . ? S2 O13 1.470(4) . ? S2 O16 1.493(4) . ? S2 Eu2 3.1909(12) 2_756 ? S3 O20 1.439(4) . ? S3 O19 1.466(4) . ? S3 O18 1.479(4) . ? S3 O17 1.479(4) . ? C1 N1 1.326(7) . ? C1 N2 1.342(7) . ? C1 H1A 0.9300 . ? C2 N1 1.375(6) . ? C2 C3 1.380(7) . ? C2 C5 1.481(7) . ? C3 N2 1.370(6) . ? C3 C4 1.492(7) . ? C4 O1 1.248(6) . ? C4 O2 1.271(6) . ? C5 O3 1.251(6) . ? C5 O4 1.256(6) . ? C6 N4 1.319(6) . ? C6 N3 1.343(6) . ? C6 H6A 0.9300 . ? C7 N3 1.368(7) . ? C7 C8 1.376(7) . ? C7 C9 1.487(7) . ? C8 N4 1.386(6) . ? C8 C10 1.478(7) . ? C9 O6 1.242(7) . ? C9 O5 1.247(6) . ? C10 O7 1.263(6) . ? C10 O8 1.269(6) . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? O2 Eu3 2.397(3) 1_455 ? O3 Eu3 2.289(4) 1_455 ? O6 Eu3 2.290(4) 1_455 ? O7 Eu3 2.477(3) 1_455 ? O12 Eu3 2.410(4) 1_455 ? O13 Eu2 2.693(4) 2_756 ? O14 Eu2 2.364(4) 1_665 ? O16 Eu2 2.480(4) 2_756 ? O19 Eu2 2.320(4) 1_655 ? O1W H11 0.8447 . ? O1W H12 0.8635 . ? O2W H21 0.8858 . ? O2W H22 0.9632 . ? O3W H31 0.9475 . ? O3W H32 0.9453 . ? O4W H41 0.9083 . ? O4W H42 0.9142 . ? O5W H51 0.8411 . ? O5W H52 0.8539 . ? O6W H61 0.8425 . ? O6W H62 0.8265 . ? O7W H72 0.8874 . ? O7W H71 0.8887 . ? 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 O18 Eu1 O9 77.99(16) . . ? O18 Eu1 O15 73.38(14) . . ? O9 Eu1 O15 75.41(12) . . ? O18 Eu1 O7W 89.92(16) . . ? O9 Eu1 O7W 147.98(13) . . ? O15 Eu1 O7W 72.73(12) . . ? O18 Eu1 O2W 134.87(15) . . ? O9 Eu1 O2W 139.02(14) . . ? O15 Eu1 O2W 130.02(14) . . ? O7W Eu1 O2W 68.36(13) . . ? O18 Eu1 O7 88.73(14) . . ? O9 Eu1 O7 81.31(12) . . ? O15 Eu1 O7 153.02(13) . . ? O7W Eu1 O7 128.47(12) . . ? O2W Eu1 O7 76.86(13) . . ? O18 Eu1 O1 140.42(14) . . ? O9 Eu1 O1 75.59(14) . . ? O15 Eu1 O1 71.79(13) . . ? O7W Eu1 O1 97.16(13) . . ? O2W Eu1 O1 83.10(14) . . ? O7 Eu1 O1 115.44(12) . . ? O18 Eu1 O8 69.98(13) . . ? O9 Eu1 O8 120.96(13) . . ? O15 Eu1 O8 134.34(12) . . ? O7W Eu1 O8 80.84(12) . . ? O2W Eu1 O8 67.85(13) . . ? O7 Eu1 O8 50.68(11) . . ? O1 Eu1 O8 149.58(13) . . ? O18 Eu1 O2 140.18(15) . . ? O9 Eu1 O2 69.03(13) . . ? O15 Eu1 O2 116.97(12) . . ? O7W Eu1 O2 129.76(13) . . ? O2W Eu1 O2 70.41(13) . . ? O7 Eu1 O2 65.27(11) . . ? O1 Eu1 O2 50.19(11) . . ? O8 Eu1 O2 108.60(11) . . ? O18 Eu1 C4 143.80(15) . . ? O9 Eu1 C4 66.15(15) . . ? O15 Eu1 C4 92.32(14) . . ? O7W Eu1 C4 117.95(14) . . ? O2W Eu1 C4 79.73(15) . . ? O7 Eu1 C4 90.55(13) . . ? O1 Eu1 C4 25.14(13) . . ? O8 Eu1 C4 133.21(13) . . ? O2 Eu1 C4 25.76(12) . . ? O18 Eu1 C10 77.58(14) . . ? O9 Eu1 C10 100.89(14) . . ? O15 Eu1 C10 150.87(14) . . ? O7W Eu1 C10 105.31(13) . . ? O2W Eu1 C10 71.41(14) . . ? O7 Eu1 C10 25.18(12) . . ? O1 Eu1 C10 136.12(13) . . ? O8 Eu1 C10 25.53(12) . . ? O2 Eu1 C10 87.16(12) . . ? C4 Eu1 C10 112.91(14) . . ? O18 Eu1 Eu3 114.54(12) . 1_455 ? O9 Eu1 Eu3 68.94(9) . 1_455 ? O15 Eu1 Eu3 140.13(9) . 1_455 ? O7W Eu1 Eu3 141.99(9) . 1_455 ? O2W Eu1 Eu3 73.89(10) . 1_455 ? O7 Eu1 Eu3 33.15(8) . 1_455 ? O1 Eu1 Eu3 82.39(8) . 1_455 ? O8 Eu1 Eu3 81.08(7) . 1_455 ? O2 Eu1 Eu3 32.44(8) . 1_455 ? C4 Eu1 Eu3 57.41(10) . 1_455 ? C10 Eu1 Eu3 56.82(10) . 1_455 ? O19 Eu2 O14 82.57(14) 1_455 1_445 ? O19 Eu2 O17 133.62(14) 1_455 . ? O14 Eu2 O17 143.41(15) 1_445 . ? O19 Eu2 O5W 75.78(15) 1_455 . ? O14 Eu2 O5W 134.66(14) 1_445 . ? O17 Eu2 O5W 71.62(15) . . ? O19 Eu2 O16 132.84(13) 1_455 2_756 ? O14 Eu2 O16 84.46(13) 1_445 2_756 ? O17 Eu2 O16 73.73(12) . 2_756 ? O5W Eu2 O16 82.04(14) . 2_756 ? O19 Eu2 O1W 148.37(14) 1_455 . ? O14 Eu2 O1W 74.08(14) 1_445 . ? O17 Eu2 O1W 70.38(14) . . ? O5W Eu2 O1W 135.82(15) . . ? O16 Eu2 O1W 66.39(12) 2_756 . ? O19 Eu2 N4 81.96(15) 1_455 . ? O14 Eu2 N4 72.08(13) 1_445 . ? O17 Eu2 N4 103.50(14) . . ? O5W Eu2 N4 140.67(14) . . ? O16 Eu2 N4 135.38(13) 2_756 . ? O1W Eu2 N4 70.83(14) . . ? O19 Eu2 O8 73.60(13) 1_455 . ? O14 Eu2 O8 131.53(12) 1_445 . ? O17 Eu2 O8 68.69(13) . . ? O5W Eu2 O8 79.31(12) . . ? O16 Eu2 O8 141.66(11) 2_756 . ? O1W Eu2 O8 106.50(13) . . ? N4 Eu2 O8 63.35(12) . . ? O19 Eu2 O13 78.81(13) 1_455 2_756 ? O14 Eu2 O13 71.93(13) 1_445 2_756 ? O17 Eu2 O13 114.43(13) . 2_756 ? O5W Eu2 O13 65.11(13) . 2_756 ? O16 Eu2 O13 54.07(12) 2_756 2_756 ? O1W Eu2 O13 112.65(13) . 2_756 ? N4 Eu2 O13 140.92(13) . 2_756 ? O8 Eu2 O13 139.27(12) . 2_756 ? O19 Eu2 S2 106.05(10) 1_455 2_756 ? O14 Eu2 S2 74.55(9) 1_445 2_756 ? O17 Eu2 S2 95.70(10) . 2_756 ? O5W Eu2 S2 73.98(10) . 2_756 ? O16 Eu2 S2 26.98(8) 2_756 2_756 ? O1W Eu2 S2 88.19(9) . 2_756 ? N4 Eu2 S2 144.29(9) . 2_756 ? O8 Eu2 S2 152.33(8) . 2_756 ? O13 Eu2 S2 27.28(9) 2_756 2_756 ? O3 Eu3 O6 139.85(14) 1_655 1_655 ? O3 Eu3 O2 75.08(13) 1_655 1_655 ? O6 Eu3 O2 143.68(13) 1_655 1_655 ? O3 Eu3 O11 118.16(17) 1_655 . ? O6 Eu3 O11 82.32(18) 1_655 . ? O2 Eu3 O11 87.40(15) 1_655 . ? O3 Eu3 O12 87.04(15) 1_655 1_655 ? O6 Eu3 O12 93.61(16) 1_655 1_655 ? O2 Eu3 O12 75.39(13) 1_655 1_655 ? O11 Eu3 O12 144.91(15) . 1_655 ? O3 Eu3 O3W 76.26(14) 1_655 . ? O6 Eu3 O3W 76.75(15) 1_655 . ? O2 Eu3 O3W 133.68(14) 1_655 . ? O11 Eu3 O3W 75.15(15) . . ? O12 Eu3 O3W 137.97(14) 1_655 . ? O3 Eu3 O7 142.17(12) 1_655 1_655 ? O6 Eu3 O7 74.53(13) 1_655 1_655 ? O2 Eu3 O7 69.15(12) 1_655 1_655 ? O11 Eu3 O7 72.70(14) . 1_655 ? O12 Eu3 O7 72.63(13) 1_655 1_655 ? O3W Eu3 O7 139.10(13) . 1_655 ? O3 Eu3 O6W 69.94(15) 1_655 . ? O6 Eu3 O6W 73.67(14) 1_655 . ? O2 Eu3 O6W 128.50(13) 1_655 . ? O11 Eu3 O6W 142.56(16) . . ? O12 Eu3 O6W 66.35(14) 1_655 . ? O3W Eu3 O6W 71.70(15) . . ? O7 Eu3 O6W 125.32(14) 1_655 . ? O3 Eu3 O10 69.33(14) 1_655 . ? O6 Eu3 O10 123.67(14) 1_655 . ? O2 Eu3 O10 70.21(13) 1_655 . ? O11 Eu3 O10 49.03(16) . . ? O12 Eu3 O10 142.10(13) 1_655 . ? O3W Eu3 O10 65.94(14) . . ? O7 Eu3 O10 108.23(13) 1_655 . ? O6W Eu3 O10 126.38(15) . . ? O3 Eu3 S1 94.63(12) 1_655 . ? O6 Eu3 S1 101.48(12) 1_655 . ? O2 Eu3 S1 79.96(9) 1_655 . ? O11 Eu3 S1 23.54(14) . . ? O12 Eu3 S1 153.99(10) 1_655 . ? O3W Eu3 S1 66.95(11) . . ? O7 Eu3 S1 91.00(9) 1_655 . ? O6W Eu3 S1 138.28(11) . . ? O10 Eu3 S1 25.63(9) . . ? O3 Eu3 Eu1 109.28(10) 1_655 1_655 ? O6 Eu3 Eu1 107.71(10) 1_655 1_655 ? O2 Eu3 Eu1 36.07(9) 1_655 1_655 ? O11 Eu3 Eu1 81.32(11) . 1_655 ? O12 Eu3 Eu1 66.69(9) 1_655 1_655 ? O3W Eu3 Eu1 155.29(10) . 1_655 ? O7 Eu3 Eu1 33.44(8) 1_655 1_655 ? O6W Eu3 Eu1 133.00(11) . 1_655 ? O10 Eu3 Eu1 92.92(9) . 1_655 ? S1 Eu3 Eu1 88.43(2) . 1_655 ? O4 Cu O4 180.0(2) . 2_765 ? O4 Cu N1 98.85(15) . 2_765 ? O4 Cu N1 81.15(15) 2_765 2_765 ? O4 Cu N1 81.15(15) . . ? O4 Cu N1 98.85(15) 2_765 . ? N1 Cu N1 180.0(2) 2_765 . ? O4 Cu O4W 88.04(17) . . ? O4 Cu O4W 91.96(17) 2_765 . ? N1 Cu O4W 89.22(17) 2_765 . ? N1 Cu O4W 90.78(17) . . ? O4 Cu O4W 91.96(17) . 2_765 ? O4 Cu O4W 88.04(17) 2_765 2_765 ? N1 Cu O4W 90.78(17) 2_765 2_765 ? N1 Cu O4W 89.22(17) . 2_765 ? O4W Cu O4W 180.0 . 2_765 ? O10 S1 O12 111.1(3) . . ? O10 S1 O11 108.2(4) . . ? O12 S1 O11 109.4(3) . . ? O10 S1 O9 110.2(3) . . ? O12 S1 O9 109.9(2) . . ? O11 S1 O9 108.0(3) . . ? O10 S1 Eu3 68.1(3) . . ? O12 S1 Eu3 119.47(17) . . ? O11 S1 Eu3 40.5(2) . . ? O9 S1 Eu3 127.57(17) . . ? O14 S2 O15 109.4(2) . . ? O14 S2 O13 112.2(2) . . ? O15 S2 O13 110.8(2) . . ? O14 S2 O16 109.8(2) . . ? O15 S2 O16 109.0(2) . . ? O13 S2 O16 105.6(2) . . ? O14 S2 Eu2 120.04(16) . 2_756 ? O15 S2 Eu2 130.10(16) . 2_756 ? O13 S2 Eu2 57.14(17) . 2_756 ? O16 S2 Eu2 48.91(15) . 2_756 ? O20 S3 O19 112.5(3) . . ? O20 S3 O18 110.8(3) . . ? O19 S3 O18 107.0(2) . . ? O20 S3 O17 110.8(3) . . ? O19 S3 O17 107.3(2) . . ? O18 S3 O17 108.3(3) . . ? N1 C1 N2 110.9(5) . . ? N1 C1 H1A 124.6 . . ? N2 C1 H1A 124.6 . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C5 116.0(4) . . ? C3 C2 C5 134.0(5) . . ? N2 C3 C2 105.1(4) . . ? N2 C3 C4 119.9(4) . . ? C2 C3 C4 134.9(5) . . ? O1 C4 O2 120.7(5) . . ? O1 C4 C3 117.8(5) . . ? O2 C4 C3 121.4(4) . . ? O1 C4 Eu1 59.3(3) . . ? O2 C4 Eu1 64.0(3) . . ? C3 C4 Eu1 160.3(4) . . ? O3 C5 O4 122.1(5) . . ? O3 C5 C2 120.8(5) . . ? O4 C5 C2 117.1(4) . . ? N4 C6 N3 111.5(4) . . ? N4 C6 H6A 124.2 . . ? N3 C6 H6A 124.2 . . ? N3 C7 C8 105.5(4) . . ? N3 C7 C9 119.5(4) . . ? C8 C7 C9 135.0(5) . . ? C7 C8 N4 109.4(4) . . ? C7 C8 C10 134.7(5) . . ? N4 C8 C10 115.8(4) . . ? O6 C9 O5 124.9(5) . . ? O6 C9 C7 118.6(4) . . ? O5 C9 C7 116.5(5) . . ? O7 C10 O8 119.9(4) . . ? O7 C10 C8 123.5(4) . . ? O8 C10 C8 116.6(4) . . ? O7 C10 Eu1 57.2(2) . . ? O8 C10 Eu1 62.8(2) . . ? C8 C10 Eu1 174.6(4) . . ? C1 N1 C2 105.9(4) . . ? C1 N1 Cu 144.7(4) . . ? C2 N1 Cu 109.4(3) . . ? C1 N2 C3 108.6(4) . . ? C1 N2 H2A 125.7 . . ? C3 N2 H2A 125.7 . . ? C6 N3 C7 108.1(4) . . ? C6 N3 H3A 125.9 . . ? C7 N3 H3A 125.9 . . ? C6 N4 C8 105.5(4) . . ? C6 N4 Eu2 133.9(3) . . ? C8 N4 Eu2 120.3(3) . . ? C4 O1 Eu1 95.6(3) . . ? C4 O2 Eu3 151.9(3) . 1_455 ? C4 O2 Eu1 90.2(3) . . ? Eu3 O2 Eu1 111.49(14) 1_455 . ? C5 O3 Eu3 154.1(4) . 1_455 ? C5 O4 Cu 115.6(3) . . ? C9 O6 Eu3 158.3(4) . 1_455 ? C10 O7 Eu3 140.4(3) . 1_455 ? C10 O7 Eu1 97.6(3) . . ? Eu3 O7 Eu1 113.41(13) 1_455 . ? C10 O8 Eu2 123.3(3) . . ? C10 O8 Eu1 91.6(3) . . ? Eu2 O8 Eu1 142.05(14) . . ? S1 O9 Eu1 142.9(2) . . ? S1 O10 Eu3 86.3(3) . . ? S1 O11 Eu3 116.0(3) . . ? S1 O12 Eu3 145.3(3) . 1_455 ? S2 O13 Eu2 95.58(19) . 2_756 ? S2 O14 Eu2 158.0(3) . 1_665 ? S2 O15 Eu1 151.1(2) . . ? S2 O16 Eu2 104.11(19) . 2_756 ? S3 O17 Eu2 135.0(2) . . ? S3 O18 Eu1 142.1(2) . . ? S3 O19 Eu2 154.8(3) . 1_655 ? Eu2 O1W H11 107.0 . . ? Eu2 O1W H12 129.0 . . ? H11 O1W H12 108.7 . . ? Eu1 O2W H21 117.9 . . ? Eu1 O2W H22 116.1 . . ? H21 O2W H22 108.2 . . ? Eu3 O3W H31 105.4 . . ? Eu3 O3W H32 108.0 . . ? H31 O3W H32 104.6 . . ? Cu O4W H41 107.0 . . ? Cu O4W H42 117.1 . . ? H41 O4W H42 108.6 . . ? Eu2 O5W H51 127.5 . . ? Eu2 O5W H52 124.3 . . ? H51 O5W H52 108.0 . . ? Eu3 O6W H61 105.7 . . ? Eu3 O6W H62 97.9 . . ? H61 O6W H62 109.5 . . ? Eu1 O7W H72 124.5 . . ? Eu1 O7W H71 110.5 . . ? H72 O7W H71 108.6 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.156 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.212