#Supplementary Material (ESI) for Chemical Communications #This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Prof. Guo-Yu Yang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 CHINA ; _publ_contact_author_email ygy@fjirsm.ac.cn _publ_contact_author_phone 86-591-83710051 _publ_contact_author_fax 86-591-83710051 _publ_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_section_title ;A Series of Luminescent Lanthanide-Cadmium-Organic Frameworks with Helical Channels and Tubes ; loop_ _publ_author_name 'Guo-Yu Yang' 'Yan-Qiong Sun' 'Jie Zhang' data_165 _database_code_depnum_ccdc_archive 'CCDC 602025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd N2 O11.50 S Tb' _chemical_formula_weight 584.52 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' Cd Cd -0.8075 1.2024 '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 P21/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 8.6257(7) _cell_length_b 10.4624(7) _cell_length_c 13.8439(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.284(3) _cell_angle_gamma 90.00 _cell_volume 1225.20(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3651 _cell_measurement_theta_min 3.0770 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 7.706 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.114 _exptl_absorpt_correction_T_max 0.214 _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 9101 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2808 _reflns_number_gt 2713 _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^)+(0.0213P)^2^+2.5390P] 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 2808 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 0.926367(18) 0.899276(15) 0.105986(11) 0.01191(6) Uani 1 1 d . . . Cd Cd 1.37636(3) 0.98168(2) 0.367023(16) 0.01195(7) Uani 1 1 d . . . S S 1.20375(10) 0.72349(8) 0.45967(6) 0.01562(17) Uani 1 1 d . . . C1 C 1.5320(4) 1.2370(3) 0.2713(2) 0.0176(7) Uani 1 1 d . . . H1A H 1.6119 1.2527 0.3256 0.021 Uiso 1 1 calc R . . C2 C 1.3353(4) 1.1490(3) 0.1748(2) 0.0102(6) Uani 1 1 d . . . C3 C 1.3823(4) 1.2557(3) 0.1280(2) 0.0119(6) Uani 1 1 d . . . C4 C 1.2101(4) 1.0542(3) 0.1472(2) 0.0116(6) Uani 1 1 d . . . C5 C 1.3246(4) 1.3184(3) 0.0309(2) 0.0124(6) Uani 1 1 d . . . N1 N 1.5079(3) 1.3100(3) 0.1904(2) 0.0147(6) Uani 1 1 d . . . N2 N 1.4311(3) 1.1395(3) 0.2671(2) 0.0139(6) Uani 1 1 d . . . O1 O 1.1728(3) 0.9826(2) 0.21325(17) 0.0158(5) Uani 1 1 d . . . O2 O 1.1358(3) 1.0430(2) 0.05919(17) 0.0152(5) Uani 1 1 d . . . O3 O 1.2224(3) 1.2696(3) -0.03368(19) 0.0247(6) Uani 1 1 d . . . O4 O 1.3863(3) 1.4259(2) 0.01844(17) 0.0177(5) Uani 1 1 d . . . O5 O 1.3702(3) 0.6976(3) 0.4974(2) 0.0302(7) Uani 1 1 d . . . O6 O 1.1827(3) 0.8501(3) 0.4099(2) 0.0267(6) Uani 1 1 d . . . O7 O 1.1376(3) 0.6255(3) 0.38544(18) 0.0212(6) Uani 1 1 d . . . O8 O 1.1141(3) 0.7246(2) 0.53983(18) 0.0208(5) Uani 1 1 d . . . O1W O 0.8693(7) 0.9349(4) 0.2717(3) 0.0809(17) Uani 1 1 d . . . O2W O 1.0031(4) 0.7180(3) 0.2055(2) 0.0339(7) Uani 1 1 d . . . O3W O 0.6376(4) 0.9411(4) 0.0994(3) 0.0527(10) Uani 1 1 d . . . O4W O 0.9601(9) 1.0076(7) 0.4293(6) 0.053(2) Uani 0.50 1 d P . . H11 H 0.8210 0.8728 0.2913 0.080 Uiso 1 1 d R . . H12 H 0.8048 0.9748 0.2279 0.080 Uiso 1 1 d R . . H21 H 1.0438 0.6799 0.1645 0.080 Uiso 1 1 d R . . H22 H 1.0739 0.7227 0.2659 0.080 Uiso 1 1 d R . . H31 H 0.5585 0.8720 0.0899 0.080 Uiso 1 1 d R . . H32 H 0.5880 1.0191 0.0756 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 0.01425(9) 0.01139(9) 0.00946(8) 0.00083(5) 0.00075(6) -0.00331(6) Cd 0.01454(13) 0.01073(12) 0.01016(11) 0.00111(8) 0.00141(9) 0.00186(9) S 0.0184(4) 0.0147(4) 0.0139(4) -0.0001(3) 0.0036(3) -0.0032(3) C1 0.0210(18) 0.0170(17) 0.0125(15) -0.0018(13) -0.0024(13) -0.0042(14) C2 0.0124(15) 0.0104(15) 0.0074(13) 0.0002(11) 0.0009(11) -0.0012(12) C3 0.0137(15) 0.0116(15) 0.0105(14) -0.0003(12) 0.0026(12) -0.0020(13) C4 0.0114(15) 0.0109(15) 0.0115(14) 0.0006(12) -0.0002(12) 0.0012(12) C5 0.0120(15) 0.0125(15) 0.0132(14) 0.0006(12) 0.0038(12) -0.0022(12) N1 0.0158(14) 0.0140(14) 0.0127(13) -0.0008(11) -0.0010(11) -0.0046(11) N2 0.0146(14) 0.0148(14) 0.0103(12) 0.0014(11) -0.0027(10) -0.0041(11) O1 0.0179(12) 0.0151(12) 0.0129(11) 0.0041(9) -0.0006(9) -0.0063(10) O2 0.0167(12) 0.0152(12) 0.0115(11) 0.0022(9) -0.0026(9) -0.0046(10) O3 0.0272(14) 0.0217(14) 0.0198(13) 0.0059(11) -0.0089(11) -0.0124(12) O4 0.0206(13) 0.0156(12) 0.0150(11) 0.0052(10) -0.0016(10) -0.0064(10) O5 0.0193(14) 0.0442(19) 0.0254(14) 0.0026(13) 0.0003(11) -0.0005(13) O6 0.0314(15) 0.0195(14) 0.0300(14) 0.0076(12) 0.0079(12) -0.0080(12) O7 0.0302(15) 0.0172(13) 0.0160(12) -0.0024(10) 0.0041(11) -0.0052(11) O8 0.0287(14) 0.0157(13) 0.0211(12) -0.0033(10) 0.0124(11) -0.0042(11) O1W 0.149(5) 0.044(2) 0.076(3) 0.026(2) 0.087(3) 0.024(3) O2W 0.050(2) 0.0296(17) 0.0190(13) 0.0100(12) -0.0019(13) 0.0037(14) O3W 0.0298(18) 0.036(2) 0.095(3) -0.012(2) 0.0204(19) -0.0079(16) O4W 0.052(5) 0.040(4) 0.072(5) -0.006(4) 0.024(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb O3 2.295(3) 3_775 ? Tb O2 2.324(2) 3_775 ? Tb O2W 2.362(3) . ? Tb O8 2.392(3) 4_575 ? Tb O7 2.438(3) 2_755 ? Tb O1W 2.466(4) . ? Tb O1 2.500(2) . ? Tb O3W 2.513(3) . ? Tb O2 2.530(2) . ? Tb C4 2.898(3) . ? Tb Tb 4.0157(4) 3_775 ? Tb H12 2.2947 . ? Tb H21 2.5744 . ? Cd N2 2.263(3) . ? Cd N1 2.273(3) 2_845 ? Cd O4 2.295(2) 4_586 ? Cd O6 2.329(3) . ? Cd O4 2.403(2) 2_845 ? Cd O1 2.480(2) . ? S O5 1.454(3) . ? S O8 1.471(3) . ? S O7 1.485(3) . ? S O6 1.488(3) . ? C1 N2 1.334(5) . ? C1 N1 1.337(4) . ? C1 H1A 0.9300 . ? C2 N2 1.383(4) . ? C2 C3 1.391(4) . ? C2 C4 1.461(4) . ? C3 N1 1.370(4) . ? C3 C5 1.490(4) . ? C4 O2 1.267(4) . ? C4 O1 1.270(4) . ? C5 O3 1.236(4) . ? C5 O4 1.271(4) . ? N1 Cd 2.273(3) 2_855 ? O2 Tb 2.324(2) 3_775 ? O3 Tb 2.295(3) 3_775 ? O4 Cd 2.295(2) 4_585 ? O4 Cd 2.403(2) 2_855 ? O7 Tb 2.438(3) 2_745 ? O8 Tb 2.392(3) 4_576 ? O1W H11 0.8443 . ? O1W H12 0.8481 . ? O2W H21 0.8250 . ? O2W H22 0.9358 . ? O3W H31 0.9844 . ? O3W H32 0.9501 . ? 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 O2 76.65(9) 3_775 3_775 ? O3 Tb O2W 72.85(10) 3_775 . ? O2 Tb O2W 140.07(10) 3_775 . ? O3 Tb O8 77.22(10) 3_775 4_575 ? O2 Tb O8 78.88(9) 3_775 4_575 ? O2W Tb O8 69.79(10) . 4_575 ? O3 Tb O7 130.98(10) 3_775 2_755 ? O2 Tb O7 77.58(8) 3_775 2_755 ? O2W Tb O7 142.34(9) . 2_755 ? O8 Tb O7 136.14(9) 4_575 2_755 ? O3 Tb O1W 108.99(14) 3_775 . ? O2 Tb O1W 145.71(13) 3_775 . ? O2W Tb O1W 70.32(12) . . ? O8 Tb O1W 135.33(13) 4_575 . ? O7 Tb O1W 73.74(11) 2_755 . ? O3 Tb O1 149.95(9) 3_775 . ? O2 Tb O1 119.97(8) 3_775 . ? O2W Tb O1 79.92(10) . . ? O8 Tb O1 81.70(9) 4_575 . ? O7 Tb O1 78.85(9) 2_755 . ? O1W Tb O1 72.31(15) . . ? O3 Tb O3W 69.66(11) 3_775 . ? O2 Tb O3W 83.27(12) 3_775 . ? O2W Tb O3W 108.90(13) . . ? O8 Tb O3W 145.18(11) 4_575 . ? O7 Tb O3W 66.47(11) 2_755 . ? O1W Tb O3W 68.34(17) . . ? O1 Tb O3W 133.04(11) . . ? O3 Tb O2 135.42(9) 3_775 . ? O2 Tb O2 68.44(9) 3_775 . ? O2W Tb O2 119.60(10) . . ? O8 Tb O2 69.71(9) 4_575 . ? O7 Tb O2 67.37(9) 2_755 . ? O1W Tb O2 115.51(14) . . ? O1 Tb O2 51.54(7) . . ? O3W Tb O2 129.74(11) . . ? O3 Tb C4 153.54(10) 3_775 . ? O2 Tb C4 94.13(9) 3_775 . ? O2W Tb C4 101.81(10) . . ? O8 Tb C4 76.67(9) 4_575 . ? O7 Tb C4 68.77(9) 2_755 . ? O1W Tb C4 92.68(15) . . ? O1 Tb C4 25.90(8) . . ? O3W Tb C4 134.65(11) . . ? O2 Tb C4 25.87(8) . . ? O3 Tb Tb 108.37(7) 3_775 3_775 ? O2 Tb Tb 35.88(6) 3_775 3_775 ? O2W Tb Tb 139.03(8) . 3_775 ? O8 Tb Tb 70.72(6) 4_575 3_775 ? O7 Tb Tb 68.47(6) 2_755 3_775 ? O1W Tb Tb 138.55(10) . 3_775 ? O1 Tb Tb 84.10(5) . 3_775 ? O3W Tb Tb 109.57(10) . 3_775 ? O2 Tb Tb 32.56(5) . 3_775 ? C4 Tb Tb 58.31(6) . 3_775 ? O3 Tb H12 106.8 3_775 . ? O2 Tb H12 125.7 3_775 . ? O2W Tb H12 87.9 . . ? O8 Tb H12 155.4 4_575 . ? O7 Tb H12 59.3 2_755 . ? O1W Tb H12 20.1 . . ? O1 Tb H12 84.3 . . ? O3W Tb H12 51.3 . . ? O2 Tb H12 115.8 . . ? C4 Tb H12 98.7 . . ? Tb Tb H12 127.7 3_775 . ? O3 Tb H21 66.6 3_775 . ? O2 Tb H21 122.8 3_775 . ? O2W Tb H21 18.6 . . ? O8 Tb H21 51.9 4_575 . ? O7 Tb H21 158.2 2_755 . ? O1W Tb H21 88.8 . . ? O1 Tb H21 83.5 . . ? O3W Tb H21 119.5 . . ? O2 Tb H21 110.7 . . ? C4 Tb H21 99.9 . . ? Tb Tb H21 122.4 3_775 . ? H12 Tb H21 106.5 . . ? N2 Cd N1 101.78(10) . 2_845 ? N2 Cd O4 106.03(10) . 4_586 ? N1 Cd O4 135.40(9) 2_845 4_586 ? N2 Cd O6 146.41(10) . . ? N1 Cd O6 90.46(11) 2_845 . ? O4 Cd O6 85.24(10) 4_586 . ? N2 Cd O4 109.13(10) . 2_845 ? N1 Cd O4 70.33(9) 2_845 2_845 ? O4 Cd O4 67.95(10) 4_586 2_845 ? O6 Cd O4 104.43(10) . 2_845 ? N2 Cd O1 70.71(9) . . ? N1 Cd O1 89.34(9) 2_845 . ? O4 Cd O1 132.54(8) 4_586 . ? O6 Cd O1 78.38(9) . . ? O4 Cd O1 159.37(8) 2_845 . ? O5 S O8 110.97(16) . . ? O5 S O7 109.81(17) . . ? O8 S O7 109.87(15) . . ? O5 S O6 110.76(18) . . ? O8 S O6 107.96(16) . . ? O7 S O6 107.39(16) . . ? N2 C1 N1 114.0(3) . . ? N2 C1 H1A 123.0 . . ? N1 C1 H1A 123.0 . . ? N2 C2 C3 108.2(3) . . ? N2 C2 C4 118.0(3) . . ? C3 C2 C4 133.8(3) . . ? N1 C3 C2 107.8(3) . . ? N1 C3 C5 118.1(3) . . ? C2 C3 C5 134.2(3) . . ? O2 C4 O1 119.1(3) . . ? O2 C4 C2 121.5(3) . . ? O1 C4 C2 119.4(3) . . ? O2 C4 Tb 60.65(17) . . ? O1 C4 Tb 59.28(16) . . ? C2 C4 Tb 169.7(2) . . ? O3 C5 O4 121.7(3) . . ? O3 C5 C3 122.4(3) . . ? O4 C5 C3 115.9(3) . . ? C1 N1 C3 105.4(3) . . ? C1 N1 Cd 137.5(2) . 2_855 ? C3 N1 Cd 117.0(2) . 2_855 ? C1 N2 C2 104.6(3) . . ? C1 N2 Cd 138.0(2) . . ? C2 N2 Cd 117.3(2) . . ? C4 O1 Cd 112.5(2) . . ? C4 O1 Tb 94.82(19) . . ? Cd O1 Tb 152.28(10) . . ? C4 O2 Tb 154.0(2) . 3_775 ? C4 O2 Tb 93.48(19) . . ? Tb O2 Tb 111.56(9) 3_775 . ? C5 O3 Tb 153.1(2) . 3_775 ? C5 O4 Cd 123.7(2) . 4_585 ? C5 O4 Cd 116.8(2) . 2_855 ? Cd O4 Cd 112.05(10) 4_585 2_855 ? S O6 Cd 128.01(17) . . ? S O7 Tb 134.18(15) . 2_745 ? S O8 Tb 141.22(15) . 4_576 ? Tb O1W H11 112.6 . . ? Tb O1W H12 68.4 . . ? H11 O1W H12 108.3 . . ? Tb O2W H21 95.4 . . ? Tb O2W H22 122.6 . . ? H21 O2W H22 110.5 . . ? Tb O3W H31 122.2 . . ? Tb O3W H32 122.5 . . ? H31 O3W H32 109.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.644 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.143 # Attachment '602026-Eu-Cd-(2)-191.cif' data_191 _database_code_depnum_ccdc_archive 'CCDC 602026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd Eu N2 O11.50 S' _chemical_formula_weight 577.56 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' Cd Cd -0.8075 1.2024 '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 P21/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 8.63050(10) _cell_length_b 10.3517(2) _cell_length_c 13.90690(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.6880(10) _cell_angle_gamma 90.00 _cell_volume 1216.69(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 89 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.68 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 7.103 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.198 _exptl_absorpt_correction_T_max 0.491 _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 6468 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2300 _reflns_number_gt 2254 _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^)+(0.0304P)^2^+19.9096P] 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 2300 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 0.92805(4) 0.89924(3) 0.10382(2) 0.01124(12) Uani 1 1 d . . . Cd Cd 1.37378(6) 0.98180(5) 0.36725(3) 0.01606(14) Uani 1 1 d . . . S S 1.2002(2) 0.72396(19) 0.45936(13) 0.0233(4) Uani 1 1 d . . . C1 C 1.5320(9) 1.2367(7) 0.2708(5) 0.0204(15) Uani 1 1 d . . . H1A H 1.6126 1.2522 0.3250 0.024 Uiso 1 1 calc R . . C2 C 1.3358(8) 1.1482(7) 0.1743(5) 0.0154(13) Uani 1 1 d . . . C3 C 1.3842(8) 1.2543(7) 0.1269(5) 0.0157(14) Uani 1 1 d . . . C4 C 1.2082(8) 1.0542(7) 0.1465(5) 0.0156(13) Uani 1 1 d . . . C5 C 1.3268(8) 1.3171(7) 0.0295(5) 0.0183(14) Uani 1 1 d . . . N1 N 1.5090(7) 1.3099(6) 0.1898(4) 0.0202(13) Uani 1 1 d . . . N2 N 1.4294(7) 1.1399(6) 0.2671(4) 0.0184(12) Uani 1 1 d . . . O1 O 1.1687(6) 0.9824(5) 0.2120(3) 0.0183(10) Uani 1 1 d . . . O2 O 1.1336(6) 1.0419(5) 0.0592(3) 0.0185(10) Uani 1 1 d . . . O3 O 1.2275(7) 1.2649(6) -0.0359(4) 0.0336(14) Uani 1 1 d . . . O4 O 1.3860(6) 1.4264(5) 0.0180(4) 0.0227(11) Uani 1 1 d . . . O5 O 1.3668(7) 0.7016(7) 0.4993(4) 0.0375(15) Uani 1 1 d . . . O6 O 1.1770(8) 0.8506(7) 0.4065(5) 0.0408(16) Uani 1 1 d . . . O7 O 1.1353(8) 0.6229(6) 0.3867(4) 0.0326(14) Uani 1 1 d . . . O8 O 1.1083(7) 0.7270(5) 0.5374(4) 0.0278(12) Uani 1 1 d . . . O1W O 0.8556(18) 0.9302(10) 0.2596(10) 0.135(7) Uani 1 1 d . . . O2W O 1.0062(9) 0.7213(7) 0.2040(4) 0.0432(17) Uani 1 1 d . . . O3W O 0.6397(12) 0.9446(10) 0.0940(11) 0.100(4) Uani 1 1 d . . . O4W O 0.941(2) 1.0033(15) 0.4120(14) 0.068(5) Uani 0.50 1 d P . . H11 H 0.8117 0.8725 0.2909 0.080 Uiso 1 1 d R . . H12 H 0.7894 0.9745 0.2275 0.080 Uiso 1 1 d R . . H21 H 1.0445 0.6736 0.1651 0.080 Uiso 1 1 d R . . H22 H 1.0746 0.7224 0.2656 0.080 Uiso 1 1 d R . . H31 H 0.5592 0.8717 0.0895 0.080 Uiso 1 1 d R . . H32 H 0.5887 1.0188 0.0752 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 0.01619(18) 0.01072(18) 0.00545(17) 0.00083(11) -0.00103(12) -0.00617(12) Cd 0.0187(3) 0.0172(3) 0.0118(2) 0.00152(18) 0.00201(19) 0.00325(19) S 0.0283(10) 0.0263(10) 0.0144(8) 0.0002(7) 0.0021(7) -0.0100(8) C1 0.021(4) 0.022(4) 0.014(3) -0.003(3) -0.004(3) -0.007(3) C2 0.015(3) 0.016(3) 0.014(3) -0.002(3) 0.001(3) 0.001(3) C3 0.016(3) 0.020(3) 0.010(3) -0.004(3) 0.000(3) -0.004(3) C4 0.019(3) 0.012(3) 0.016(3) 0.000(3) 0.004(3) 0.001(3) C5 0.014(3) 0.023(4) 0.018(3) 0.002(3) 0.002(3) -0.004(3) N1 0.024(3) 0.020(3) 0.015(3) 0.003(2) 0.002(2) -0.006(3) N2 0.021(3) 0.021(3) 0.011(3) 0.002(2) 0.000(2) -0.002(3) O1 0.019(2) 0.022(3) 0.013(2) 0.004(2) 0.0005(19) -0.004(2) O2 0.022(2) 0.021(3) 0.010(2) 0.003(2) -0.0017(19) -0.003(2) O3 0.038(3) 0.036(3) 0.020(3) 0.006(2) -0.010(2) -0.023(3) O4 0.025(3) 0.020(3) 0.021(3) 0.008(2) 0.001(2) -0.007(2) O5 0.027(3) 0.057(4) 0.026(3) 0.002(3) 0.001(2) -0.004(3) O6 0.046(4) 0.037(4) 0.034(3) 0.015(3) -0.005(3) -0.018(3) O7 0.046(4) 0.035(3) 0.019(3) -0.006(2) 0.012(3) -0.018(3) O8 0.038(3) 0.021(3) 0.027(3) -0.005(2) 0.012(2) -0.009(2) O1W 0.226(16) 0.076(7) 0.157(12) 0.071(8) 0.167(13) 0.066(9) O2W 0.066(5) 0.037(4) 0.021(3) 0.010(3) -0.003(3) -0.002(3) O3W 0.061(6) 0.069(6) 0.179(12) -0.046(8) 0.049(7) -0.019(5) O4W 0.072(11) 0.041(9) 0.104(14) -0.019(9) 0.048(11) 0.005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu O3 2.251(5) 3_775 ? Eu O2 2.303(5) 3_775 ? Eu O2W 2.325(6) . ? Eu O8 2.359(5) 4_575 ? Eu O7 2.389(6) 2_755 ? Eu O1W 2.395(10) . ? Eu O1 2.460(5) . ? Eu O2 2.482(5) . ? Eu O3W 2.509(10) . ? Eu C4 2.862(7) . ? Eu Eu 3.9606(6) 3_775 ? Eu H12 2.4153 . ? Eu H21 2.6161 . ? Cd N2 2.263(6) . ? Cd N1 2.269(6) 2_845 ? Cd O4 2.285(5) 4_586 ? Cd O6 2.325(6) . ? Cd O4 2.415(5) 2_845 ? Cd O1 2.499(5) . ? S O5 1.451(6) . ? S O8 1.469(6) . ? S O7 1.483(6) . ? S O6 1.496(6) . ? C1 N2 1.331(10) . ? C1 N1 1.338(9) . ? C1 H1A 0.9300 . ? C2 N2 1.380(9) . ? C2 C3 1.387(10) . ? C2 C4 1.462(10) . ? C3 N1 1.369(9) . ? C3 C5 1.494(9) . ? C4 O2 1.261(8) . ? C4 O1 1.274(8) . ? C5 O3 1.240(9) . ? C5 O4 1.265(9) . ? N1 Cd 2.269(6) 2_855 ? O2 Eu 2.303(5) 3_775 ? O3 Eu 2.251(5) 3_775 ? O4 Cd 2.285(5) 4_585 ? O4 Cd 2.415(5) 2_855 ? O7 Eu 2.389(6) 2_745 ? O8 Eu 2.359(5) 4_576 ? O1W H11 0.8694 . ? O1W H12 0.7955 . ? O2W H21 0.8471 . ? O2W H22 0.9366 . ? O3W H31 1.0180 . ? O3W H32 0.8980 . ? 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 Eu O2 77.71(19) 3_775 3_775 ? O3 Eu O2W 74.3(2) 3_775 . ? O2 Eu O2W 141.3(2) 3_775 . ? O3 Eu O8 78.6(2) 3_775 4_575 ? O2 Eu O8 78.48(19) 3_775 4_575 ? O2W Eu O8 70.2(2) . 4_575 ? O3 Eu O7 129.1(2) 3_775 2_755 ? O2 Eu O7 77.78(18) 3_775 2_755 ? O2W Eu O7 140.9(2) . 2_755 ? O8 Eu O7 137.3(2) 4_575 2_755 ? O3 Eu O1W 103.8(4) 3_775 . ? O2 Eu O1W 143.6(3) 3_775 . ? O2W Eu O1W 70.2(3) . . ? O8 Eu O1W 137.9(3) 4_575 . ? O7 Eu O1W 73.5(3) 2_755 . ? O3 Eu O1 151.5(2) 3_775 . ? O2 Eu O1 120.48(17) 3_775 . ? O2W Eu O1 78.7(2) . . ? O8 Eu O1 83.74(19) 4_575 . ? O7 Eu O1 78.5(2) 2_755 . ? O1W Eu O1 75.1(4) . . ? O3 Eu O2 137.72(19) 3_775 . ? O2 Eu O2 68.33(19) 3_775 . ? O2W Eu O2 119.1(2) . . ? O8 Eu O2 70.75(19) 4_575 . ? O7 Eu O2 67.66(19) 2_755 . ? O1W Eu O2 118.5(4) . . ? O1 Eu O2 52.19(16) . . ? O3 Eu O3W 67.5(3) 3_775 . ? O2 Eu O3W 82.4(4) 3_775 . ? O2W Eu O3W 110.2(4) . . ? O8 Eu O3W 143.9(3) 4_575 . ? O7 Eu O3W 65.6(3) 2_755 . ? O1W Eu O3W 65.6(5) . . ? O1 Eu O3W 132.3(3) . . ? O2 Eu O3W 128.8(3) . . ? O3 Eu C4 156.5(2) 3_775 . ? O2 Eu C4 94.19(18) 3_775 . ? O2W Eu C4 100.9(2) . . ? O8 Eu C4 78.2(2) 4_575 . ? O7 Eu C4 68.8(2) 2_755 . ? O1W Eu C4 95.8(4) . . ? O1 Eu C4 26.33(18) . . ? O2 Eu C4 26.06(17) . . ? O3W Eu C4 133.9(3) . . ? O3 Eu Eu 109.86(14) 3_775 3_775 ? O2 Eu Eu 35.61(12) 3_775 3_775 ? O2W Eu Eu 139.31(19) . 3_775 ? O8 Eu Eu 71.17(13) 4_575 3_775 ? O7 Eu Eu 68.82(14) 2_755 3_775 ? O1W Eu Eu 140.1(3) . 3_775 ? O1 Eu Eu 84.89(11) . 3_775 ? O2 Eu Eu 32.72(11) . 3_775 ? O3W Eu Eu 108.4(3) . 3_775 ? C4 Eu Eu 58.64(14) . 3_775 ? O3 Eu H12 101.7 3_775 . ? O2 Eu H12 124.5 3_775 . ? O2W Eu H12 87.4 . . ? O8 Eu H12 156.8 4_575 . ? O7 Eu H12 59.7 2_755 . ? O1W Eu H12 19.0 . . ? O1 Eu H12 86.0 . . ? O2 Eu H12 117.9 . . ? O3W Eu H12 49.4 . . ? C4 Eu H12 101.0 . . ? Eu Eu H12 128.5 3_775 . ? O3 Eu H21 67.7 3_775 . ? O2 Eu H21 123.6 3_775 . ? O2W Eu H21 18.6 . . ? O8 Eu H21 52.6 4_575 . ? O7 Eu H21 157.6 2_755 . ? O1W Eu H21 88.7 . . ? O1 Eu H21 83.8 . . ? O2 Eu H21 111.5 . . ? O3W Eu H21 119.7 . . ? C4 Eu H21 100.4 . . ? Eu Eu H21 123.5 3_775 . ? H12 Eu H21 105.6 . . ? N2 Cd N1 100.8(2) . 2_845 ? N2 Cd O4 106.7(2) . 4_586 ? N1 Cd O4 134.9(2) 2_845 4_586 ? N2 Cd O6 145.4(2) . . ? N1 Cd O6 91.3(3) 2_845 . ? O4 Cd O6 85.9(2) 4_586 . ? N2 Cd O4 108.5(2) . 2_845 ? N1 Cd O4 70.17(19) 2_845 2_845 ? O4 Cd O4 67.6(2) 4_586 2_845 ? O6 Cd O4 106.0(2) . 2_845 ? N2 Cd O1 70.60(19) . . ? N1 Cd O1 89.30(19) 2_845 . ? O4 Cd O1 133.22(17) 4_586 . ? O6 Cd O1 77.36(19) . . ? O4 Cd O1 159.11(17) 2_845 . ? O5 S O8 111.2(4) . . ? O5 S O7 110.9(4) . . ? O8 S O7 109.5(3) . . ? O5 S O6 110.6(4) . . ? O8 S O6 107.8(4) . . ? O7 S O6 106.8(4) . . ? N2 C1 N1 114.2(6) . . ? N2 C1 H1A 122.9 . . ? N1 C1 H1A 122.9 . . ? N2 C2 C3 108.6(6) . . ? N2 C2 C4 118.2(6) . . ? C3 C2 C4 133.2(6) . . ? N1 C3 C2 107.6(6) . . ? N1 C3 C5 118.0(6) . . ? C2 C3 C5 134.3(6) . . ? O2 C4 O1 118.1(6) . . ? O2 C4 C2 122.1(6) . . ? O1 C4 C2 119.8(6) . . ? O2 C4 Eu 59.9(4) . . ? O1 C4 Eu 58.9(3) . . ? C2 C4 Eu 171.0(5) . . ? O3 C5 O4 122.3(7) . . ? O3 C5 C3 121.9(7) . . ? O4 C5 C3 115.8(6) . . ? C1 N1 C3 105.2(6) . . ? C1 N1 Cd 137.5(5) . 2_855 ? C3 N1 Cd 117.1(4) . 2_855 ? C1 N2 C2 104.3(6) . . ? C1 N2 Cd 138.0(5) . . ? C2 N2 Cd 117.7(5) . . ? C4 O1 Eu 94.7(4) . . ? C4 O1 Cd 111.9(4) . . ? Eu O1 Cd 152.8(2) . . ? C4 O2 Eu 153.2(5) . 3_775 ? C4 O2 Eu 94.1(4) . . ? Eu O2 Eu 111.67(19) 3_775 . ? C5 O3 Eu 154.3(5) . 3_775 ? C5 O4 Cd 122.9(5) . 4_585 ? C5 O4 Cd 116.4(4) . 2_855 ? Cd O4 Cd 112.4(2) 4_585 2_855 ? S O6 Cd 126.6(4) . . ? S O7 Eu 134.8(3) . 2_745 ? S O8 Eu 140.8(3) . 4_576 ? Eu O1W H11 125.6 . . ? Eu O1W H12 81.9 . . ? H11 O1W H12 110.0 . . ? Eu O2W H21 100.5 . . ? Eu O2W H22 126.2 . . ? H21 O2W H22 109.6 . . ? Eu O3W H31 121.4 . . ? Eu O3W H32 126.7 . . ? H31 O3W H32 109.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.170 _refine_diff_density_min -1.930 _refine_diff_density_rms 0.215 # Attachment '602027-Dy-Cd(3)-163.cif' data_163 _database_code_depnum_ccdc_archive 'CCDC 602027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd Dy N2 O11.50 S' _chemical_formula_weight 588.10 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' Cd Cd -0.8075 1.2024 '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 P21/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 8.6178(2) _cell_length_b 10.4366(2) _cell_length_c 13.8568(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.3200(10) _cell_angle_gamma 90.00 _cell_volume 1222.04(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.67 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max .40 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 8.054 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.069 _exptl_absorpt_correction_T_max 0.299 _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 6409 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.67 _reflns_number_total 2315 _reflns_number_gt 2261 _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^)+(0.0206P)^2^+8.1719P] 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 2315 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.92658(2) 0.89928(2) 0.105530(15) 0.01237(8) Uani 1 1 d . . . Cd Cd 1.37562(4) 0.98154(3) 0.36704(2) 0.01240(9) Uani 1 1 d . . . S S 1.20282(14) 0.72340(11) 0.45958(8) 0.0164(2) Uani 1 1 d . . . C1 C 1.5323(6) 1.2368(5) 0.2710(3) 0.0168(10) Uani 1 1 d . . . H1A H 1.6126 1.2523 0.3252 0.020 Uiso 1 1 calc R . . C2 C 1.3357(5) 1.1488(4) 0.1745(3) 0.0117(9) Uani 1 1 d . . . C3 C 1.3828(5) 1.2552(4) 0.1279(3) 0.0116(9) Uani 1 1 d . . . C4 C 1.2090(5) 1.0548(4) 0.1470(3) 0.0109(8) Uani 1 1 d . . . C5 C 1.3240(5) 1.3178(5) 0.0304(3) 0.0131(9) Uani 1 1 d . . . N1 N 1.5081(5) 1.3104(4) 0.1901(3) 0.0156(8) Uani 1 1 d . . . N2 N 1.4309(5) 1.1391(4) 0.2668(3) 0.0145(8) Uani 1 1 d . . . O1 O 1.1718(4) 0.9824(3) 0.2129(2) 0.0155(7) Uani 1 1 d . . . O2 O 1.1350(4) 1.0427(3) 0.0588(2) 0.0150(7) Uani 1 1 d . . . O3 O 1.2230(4) 1.2681(4) -0.0343(3) 0.0263(8) Uani 1 1 d . . . O4 O 1.3863(4) 1.4260(3) 0.0186(2) 0.0175(7) Uani 1 1 d . . . O5 O 1.3692(4) 0.6978(4) 0.4976(3) 0.0311(9) Uani 1 1 d . . . O6 O 1.1814(5) 0.8501(4) 0.4089(3) 0.0282(9) Uani 1 1 d . . . O7 O 1.1371(4) 0.6247(4) 0.3853(3) 0.0219(8) Uani 1 1 d . . . O8 O 1.1128(4) 0.7245(3) 0.5393(3) 0.0221(8) Uani 1 1 d . . . O1W O 0.8682(9) 0.9349(5) 0.2697(5) 0.086(2) Uani 1 1 d . . . O2W O 1.0029(5) 0.7194(4) 0.2050(3) 0.0336(10) Uani 1 1 d . . . O3W O 0.6388(6) 0.9408(5) 0.0982(5) 0.0570(15) Uani 1 1 d . . . O4W O 0.9565(13) 1.0062(10) 0.4276(8) 0.054(3) Uani 0.50 1 d P . . H11 H 0.8232 0.8735 0.2918 0.080 Uiso 1 1 d R . . H12 H 0.8070 0.9755 0.2284 0.080 Uiso 1 1 d R . . H21 H 1.0466 0.6809 0.1654 0.080 Uiso 1 1 d R . . H22 H 1.0767 0.7237 0.2668 0.080 Uiso 1 1 d R . . H31 H 0.5607 0.8727 0.0904 0.080 Uiso 1 1 d R . . H32 H 0.5902 1.0198 0.0761 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 0.01626(12) 0.01226(12) 0.00771(12) 0.00076(7) 0.00015(8) -0.00333(8) Cd 0.01641(17) 0.01163(17) 0.00853(17) 0.00094(12) 0.00088(12) 0.00204(12) S 0.0205(6) 0.0160(6) 0.0124(5) 0.0001(4) 0.0028(4) -0.0043(4) C1 0.018(2) 0.019(2) 0.011(2) -0.0008(18) -0.0034(18) -0.0049(19) C2 0.017(2) 0.011(2) 0.007(2) 0.0009(17) 0.0011(17) 0.0007(18) C3 0.012(2) 0.012(2) 0.010(2) -0.0019(17) 0.0008(17) -0.0017(17) C4 0.012(2) 0.011(2) 0.008(2) 0.0016(17) -0.0006(16) 0.0024(17) C5 0.013(2) 0.016(2) 0.010(2) 0.0023(18) 0.0008(17) -0.0013(18) N1 0.0182(19) 0.018(2) 0.0093(18) -0.0012(16) -0.0007(15) -0.0048(16) N2 0.0169(19) 0.0149(19) 0.0095(18) 0.0023(15) -0.0028(15) -0.0043(16) O1 0.0196(16) 0.0141(16) 0.0119(16) 0.0039(13) 0.0007(13) -0.0059(13) O2 0.0186(16) 0.0132(16) 0.0111(16) 0.0019(13) -0.0019(13) -0.0055(13) O3 0.031(2) 0.0236(19) 0.0183(18) 0.0064(15) -0.0106(15) -0.0114(16) O4 0.0210(17) 0.0151(17) 0.0147(17) 0.0067(13) -0.0007(13) -0.0072(14) O5 0.0206(18) 0.045(3) 0.027(2) 0.0005(18) 0.0006(16) -0.0020(17) O6 0.037(2) 0.022(2) 0.026(2) 0.0070(16) 0.0056(17) -0.0098(17) O7 0.0302(19) 0.0225(19) 0.0127(17) -0.0035(14) 0.0031(15) -0.0075(15) O8 0.0313(19) 0.0187(18) 0.0191(18) -0.0028(14) 0.0115(15) -0.0040(15) O1W 0.155(7) 0.046(3) 0.083(5) 0.031(3) 0.092(5) 0.030(4) O2W 0.053(3) 0.027(2) 0.0173(19) 0.0093(16) -0.0035(18) 0.0039(19) O3W 0.033(3) 0.042(3) 0.099(5) -0.016(3) 0.022(3) -0.007(2) O4W 0.063(7) 0.044(6) 0.058(7) -0.003(5) 0.023(5) 0.008(5) _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 O3 2.278(4) 3_775 ? Dy O2 2.314(3) 3_775 ? Dy O2W 2.346(4) . ? Dy O8 2.380(3) 4_575 ? Dy O7 2.425(4) 2_755 ? Dy O1W 2.453(6) . ? Dy O1 2.490(3) . ? Dy O3W 2.500(5) . ? Dy O2 2.519(3) . ? Dy C4 2.888(4) . ? Dy H12 2.2985 . ? Cd N2 2.263(4) . ? Cd N1 2.266(4) 2_845 ? Cd O4 2.297(3) 4_586 ? Cd O6 2.324(4) . ? Cd O4 2.404(3) 2_845 ? Cd O1 2.485(3) . ? S O5 1.452(4) . ? S O8 1.470(4) . ? S O7 1.487(4) . ? S O6 1.492(4) . ? C1 N2 1.336(6) . ? C1 N1 1.341(6) . ? C1 H1A 0.9300 . ? C2 N2 1.382(6) . ? C2 C3 1.385(6) . ? C2 C4 1.461(6) . ? C3 N1 1.369(6) . ? C3 C5 1.497(6) . ? C4 O2 1.270(5) . ? C4 O1 1.273(5) . ? C5 O3 1.235(6) . ? C5 O4 1.274(6) . ? N1 Cd 2.266(4) 2_855 ? O2 Dy 2.314(3) 3_775 ? O3 Dy 2.278(4) 3_775 ? O4 Cd 2.297(3) 4_585 ? O4 Cd 2.404(3) 2_855 ? O7 Dy 2.425(4) 2_745 ? O8 Dy 2.380(3) 4_576 ? O1W H11 0.8375 . ? O1W H12 0.8167 . ? O2W H21 0.8285 . ? O2W H22 0.9624 . ? O3W H31 0.9703 . ? O3W H32 0.9477 . ? 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 Dy O2 76.89(12) 3_775 3_775 ? O3 Dy O2W 73.16(14) 3_775 . ? O2 Dy O2W 140.46(13) 3_775 . ? O3 Dy O8 77.50(14) 3_775 4_575 ? O2 Dy O8 78.75(12) 3_775 4_575 ? O2W Dy O8 70.09(14) . 4_575 ? O3 Dy O7 130.71(13) 3_775 2_755 ? O2 Dy O7 77.71(12) 3_775 2_755 ? O2W Dy O7 141.81(13) . 2_755 ? O8 Dy O7 136.36(12) 4_575 2_755 ? O3 Dy O1W 108.5(2) 3_775 . ? O2 Dy O1W 145.43(18) 3_775 . ? O2W Dy O1W 70.19(17) . . ? O8 Dy O1W 135.75(18) 4_575 . ? O7 Dy O1W 73.41(15) 2_755 . ? O3 Dy O1 150.23(12) 3_775 . ? O2 Dy O1 120.03(11) 3_775 . ? O2W Dy O1 79.67(13) . . ? O8 Dy O1 82.06(12) 4_575 . ? O7 Dy O1 78.75(11) 2_755 . ? O1W Dy O1 72.4(2) . . ? O3 Dy O3W 69.08(16) 3_775 . ? O2 Dy O3W 83.11(17) 3_775 . ? O2W Dy O3W 108.92(18) . . ? O8 Dy O3W 144.79(16) 4_575 . ? O7 Dy O3W 66.48(15) 2_755 . ? O1W Dy O3W 68.2(2) . . ? O1 Dy O3W 133.08(15) . . ? O3 Dy O2 135.69(12) 3_775 . ? O2 Dy O2 68.22(12) 3_775 . ? O2W Dy O2 119.68(13) . . ? O8 Dy O2 69.79(12) 4_575 . ? O7 Dy O2 67.49(12) 2_755 . ? O1W Dy O2 115.78(19) . . ? O1 Dy O2 51.83(10) . . ? O3W Dy O2 129.66(15) . . ? O3 Dy C4 154.21(14) 3_775 . ? O2 Dy C4 94.04(11) 3_775 . ? O2W Dy C4 101.83(14) . . ? O8 Dy C4 77.06(12) 4_575 . ? O7 Dy C4 68.58(12) 2_755 . ? O1W Dy C4 92.8(2) . . ? O1 Dy C4 26.07(11) . . ? O3W Dy C4 134.52(15) . . ? O2 Dy C4 26.03(11) . . ? O3 Dy H12 106.8 3_775 . ? O2 Dy H12 126.0 3_775 . ? O2W Dy H12 87.5 . . ? O8 Dy H12 155.2 4_575 . ? O7 Dy H12 59.1 2_755 . ? O1W Dy H12 19.4 . . ? O1 Dy H12 83.6 . . ? O3W Dy H12 52.0 . . ? O2 Dy H12 115.5 . . ? C4 Dy H12 98.1 . . ? N2 Cd N1 101.42(14) . 2_845 ? N2 Cd O4 106.27(13) . 4_586 ? N1 Cd O4 135.22(13) 2_845 4_586 ? N2 Cd O6 146.19(14) . . ? N1 Cd O6 90.65(15) 2_845 . ? O4 Cd O6 85.50(13) 4_586 . ? N2 Cd O4 108.94(13) . 2_845 ? N1 Cd O4 70.19(12) 2_845 2_845 ? O4 Cd O4 67.86(13) 4_586 2_845 ? O6 Cd O4 104.87(13) . 2_845 ? N2 Cd O1 70.62(12) . . ? N1 Cd O1 89.37(12) 2_845 . ? O4 Cd O1 132.78(11) 4_586 . ? O6 Cd O1 78.14(12) . . ? O4 Cd O1 159.24(11) 2_845 . ? O5 S O8 111.0(2) . . ? O5 S O7 109.8(2) . . ? O8 S O7 109.9(2) . . ? O5 S O6 110.9(2) . . ? O8 S O6 108.2(2) . . ? O7 S O6 107.0(2) . . ? N2 C1 N1 114.1(4) . . ? N2 C1 H1A 123.0 . . ? N1 C1 H1A 123.0 . . ? N2 C2 C3 108.4(4) . . ? N2 C2 C4 118.0(4) . . ? C3 C2 C4 133.6(4) . . ? N1 C3 C2 108.1(4) . . ? N1 C3 C5 118.0(4) . . ? C2 C3 C5 133.8(4) . . ? O2 C4 O1 118.8(4) . . ? O2 C4 C2 121.7(4) . . ? O1 C4 C2 119.5(4) . . ? O2 C4 Dy 60.5(2) . . ? O1 C4 Dy 59.2(2) . . ? C2 C4 Dy 170.5(3) . . ? O3 C5 O4 122.3(4) . . ? O3 C5 C3 122.5(4) . . ? O4 C5 C3 115.2(4) . . ? C1 N1 C3 105.0(4) . . ? C1 N1 Cd 137.5(3) . 2_855 ? C3 N1 Cd 117.4(3) . 2_855 ? C1 N2 C2 104.4(4) . . ? C1 N2 Cd 138.0(3) . . ? C2 N2 Cd 117.6(3) . . ? C4 O1 Cd 112.5(3) . . ? C4 O1 Dy 94.7(3) . . ? Cd O1 Dy 152.40(14) . . ? C4 O2 Dy 153.7(3) . 3_775 ? C4 O2 Dy 93.4(3) . . ? Dy O2 Dy 111.78(12) 3_775 . ? C5 O3 Dy 153.6(3) . 3_775 ? C5 O4 Cd 123.2(3) . 4_585 ? C5 O4 Cd 117.1(3) . 2_855 ? Cd O4 Cd 112.14(13) 4_585 2_855 ? S O6 Cd 127.8(2) . . ? S O7 Dy 134.0(2) . 2_745 ? S O8 Dy 141.3(2) . 4_576 ? Dy O1W H11 114.7 . . ? Dy O1W H12 69.6 . . ? H11 O1W H12 111.8 . . ? Dy O2W H21 96.3 . . ? Dy O2W H22 123.0 . . ? H21 O2W H22 107.8 . . ? Dy O3W H31 122.6 . . ? Dy O3W H32 122.4 . . ? H31 O3W H32 110.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.609 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.134 # Attachment '602028-Gd-Cd(4)-180.cif' data_180 _database_code_depnum_ccdc_archive 'CCDC 602028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd Gd N2 O11.50 S' _chemical_formula_weight 582.85 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' Cd Cd -0.8075 1.2024 '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 P21/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 8.6194(6) _cell_length_b 10.4858(6) _cell_length_c 13.8468(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.168(4) _cell_angle_gamma 90.00 _cell_volume 1227.79(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3555 _cell_measurement_theta_min 2.4073 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 7.332 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.556 _exptl_absorpt_correction_T_min 0.3528 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 ; 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 9269 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2816 _reflns_number_gt 2644 _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^)+(0.0286P)^2^+1.5267P] 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 2816 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.92587(2) 0.899390(17) 0.106654(13) 0.01188(7) Uani 1 1 d . . . Cd Cd 1.37703(3) 0.98191(3) 0.367104(19) 0.01281(8) Uani 1 1 d . . . S S 1.20480(11) 0.72369(9) 0.45988(7) 0.01579(19) Uani 1 1 d . . . C1 C 1.5326(5) 1.2370(4) 0.2712(3) 0.0184(8) Uani 1 1 d . . . H1A H 1.6129 1.2523 0.3253 0.022 Uiso 1 1 calc R . . C2 C 1.3357(4) 1.1495(4) 0.1750(3) 0.0118(7) Uani 1 1 d . . . C3 C 1.3827(4) 1.2561(3) 0.1279(3) 0.0126(7) Uani 1 1 d . . . C4 C 1.2107(4) 1.0544(4) 0.1479(3) 0.0123(7) Uani 1 1 d . . . C5 C 1.3248(4) 1.3186(4) 0.0313(3) 0.0132(7) Uani 1 1 d . . . N1 N 1.5081(4) 1.3104(3) 0.1907(2) 0.0151(6) Uani 1 1 d . . . N2 N 1.4318(4) 1.1397(3) 0.2669(2) 0.0155(6) Uani 1 1 d . . . O1 O 1.1742(3) 0.9826(3) 0.21404(19) 0.0166(6) Uani 1 1 d . . . O2 O 1.1360(3) 1.0430(3) 0.05990(19) 0.0159(5) Uani 1 1 d . . . O3 O 1.2225(4) 1.2699(3) -0.0332(2) 0.0233(6) Uani 1 1 d . . . O4 O 1.3873(3) 1.4260(3) 0.0188(2) 0.0189(6) Uani 1 1 d . . . O5 O 1.3711(3) 0.6964(3) 0.4972(2) 0.0292(7) Uani 1 1 d . . . O6 O 1.1843(4) 0.8499(3) 0.4106(2) 0.0257(7) Uani 1 1 d . . . O7 O 1.1378(4) 0.6262(3) 0.3859(2) 0.0205(6) Uani 1 1 d . . . O8 O 1.1155(3) 0.7244(3) 0.5401(2) 0.0205(6) Uani 1 1 d . . . O1W O 0.8700(7) 0.9355(4) 0.2737(4) 0.0778(18) Uani 1 1 d . . . O2W O 1.0028(4) 0.7164(3) 0.2058(2) 0.0326(8) Uani 1 1 d . . . O3W O 0.6377(4) 0.9412(4) 0.0998(3) 0.0492(10) Uani 1 1 d . . . O4W O 0.9628(10) 1.0090(7) 0.4322(7) 0.054(2) Uani 0.50 1 d P . . H11 H 0.8218 0.8724 0.2913 0.080 Uiso 1 1 d R . . H12 H 0.8056 0.9744 0.2278 0.080 Uiso 1 1 d R . . H21 H 1.0445 0.6695 0.1644 0.080 Uiso 1 1 d R . . H22 H 1.0746 0.7223 0.2659 0.080 Uiso 1 1 d R . . H31 H 0.5593 0.8716 0.0898 0.080 Uiso 1 1 d R . . H32 H 0.5888 1.0187 0.0756 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 0.01334(10) 0.01226(11) 0.00876(10) 0.00093(6) -0.00100(7) -0.00294(7) Cd 0.01469(14) 0.01216(14) 0.01033(14) 0.00105(10) -0.00070(10) 0.00190(10) S 0.0174(5) 0.0159(5) 0.0137(5) 0.0000(4) 0.0021(3) -0.0028(4) C1 0.020(2) 0.020(2) 0.0110(18) -0.0026(15) -0.0050(14) -0.0045(16) C2 0.0119(17) 0.0134(17) 0.0092(17) 0.0010(14) -0.0001(13) -0.0021(14) C3 0.0144(18) 0.0130(18) 0.0104(17) -0.0025(14) 0.0025(13) -0.0028(14) C4 0.0127(17) 0.0126(17) 0.0103(17) -0.0018(14) -0.0009(13) -0.0005(14) C5 0.0129(17) 0.0138(18) 0.0125(17) 0.0007(14) 0.0017(13) -0.0015(14) N1 0.0138(16) 0.0163(16) 0.0128(16) -0.0016(13) -0.0031(12) -0.0049(13) N2 0.0183(16) 0.0161(16) 0.0096(15) 0.0003(13) -0.0031(12) -0.0035(13) O1 0.0189(14) 0.0172(14) 0.0115(13) 0.0046(10) -0.0025(10) -0.0064(11) O2 0.0170(14) 0.0181(14) 0.0104(13) 0.0020(11) -0.0030(10) -0.0027(11) O3 0.0266(16) 0.0207(15) 0.0170(15) 0.0047(12) -0.0098(12) -0.0099(13) O4 0.0198(15) 0.0173(14) 0.0167(14) 0.0037(11) -0.0037(11) -0.0087(12) O5 0.0161(15) 0.043(2) 0.0259(17) 0.0021(14) -0.0016(12) -0.0013(14) O6 0.0318(18) 0.0182(15) 0.0273(17) 0.0054(13) 0.0062(13) -0.0070(13) O7 0.0312(17) 0.0161(14) 0.0129(14) -0.0045(11) 0.0010(11) -0.0063(12) O8 0.0257(16) 0.0186(14) 0.0195(15) -0.0039(11) 0.0098(12) -0.0043(12) O1W 0.145(5) 0.042(2) 0.070(3) 0.022(2) 0.078(4) 0.021(3) O2W 0.049(2) 0.0280(18) 0.0162(15) 0.0065(13) -0.0044(14) 0.0034(16) O3W 0.0246(19) 0.035(2) 0.091(3) -0.008(2) 0.0170(19) -0.0059(16) O4W 0.053(5) 0.037(4) 0.073(6) -0.004(4) 0.016(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O3 2.306(3) 3_775 ? Gd O2 2.343(3) 3_775 ? Gd O2W 2.378(3) . ? Gd O8 2.406(3) 4_575 ? Gd O7 2.448(3) 2_755 ? Gd O1W 2.481(4) . ? Gd O3W 2.506(4) . ? Gd O1 2.514(3) . ? Gd O2 2.534(3) . ? Gd C4 2.908(4) . ? Gd Gd 4.0338(4) 3_775 ? Gd H12 2.2768 . ? Cd N2 2.267(3) . ? Cd N1 2.273(3) 2_845 ? Cd O4 2.298(3) 4_586 ? Cd O6 2.330(3) . ? Cd O4 2.392(3) 2_845 ? Cd O1 2.473(3) . ? S O5 1.455(3) . ? S O8 1.469(3) . ? S O7 1.483(3) . ? S O6 1.484(3) . ? C1 N2 1.333(5) . ? C1 N1 1.337(5) . ? C1 H1A 0.9300 . ? C2 N2 1.381(5) . ? C2 C3 1.393(5) . ? C2 C4 1.463(5) . ? C3 N1 1.373(5) . ? C3 C5 1.486(5) . ? C4 O2 1.269(4) . ? C4 O1 1.272(4) . ? C5 O3 1.237(5) . ? C5 O4 1.275(4) . ? N1 Cd 2.273(3) 2_855 ? O2 Gd 2.343(3) 3_775 ? O3 Gd 2.306(3) 3_775 ? O4 Cd 2.298(3) 4_585 ? O4 Cd 2.392(3) 2_855 ? O7 Gd 2.448(3) 2_745 ? O8 Gd 2.406(3) 4_576 ? O1W H11 0.8421 . ? O1W H12 0.8606 . ? O2W H21 0.8830 . ? O2W H22 0.9370 . ? O3W H31 0.9866 . ? O3W H32 0.9463 . ? 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 Gd O2 76.30(9) 3_775 3_775 ? O3 Gd O2W 72.69(11) 3_775 . ? O2 Gd O2W 139.56(10) 3_775 . ? O3 Gd O8 77.03(11) 3_775 4_575 ? O2 Gd O8 78.70(9) 3_775 4_575 ? O2W Gd O8 69.61(11) . 4_575 ? O3 Gd O7 131.07(10) 3_775 2_755 ? O2 Gd O7 77.36(9) 3_775 2_755 ? O2W Gd O7 143.07(10) . 2_755 ? O8 Gd O7 135.65(10) 4_575 2_755 ? O3 Gd O1W 109.72(14) 3_775 . ? O2 Gd O1W 146.09(14) 3_775 . ? O2W Gd O1W 70.58(13) . . ? O8 Gd O1W 135.09(14) 4_575 . ? O7 Gd O1W 74.14(11) 2_755 . ? O3 Gd O3W 69.95(12) 3_775 . ? O2 Gd O3W 83.26(13) 3_775 . ? O2W Gd O3W 109.08(13) . . ? O8 Gd O3W 145.26(12) 4_575 . ? O7 Gd O3W 66.59(11) 2_755 . ? O1W Gd O3W 68.82(18) . . ? O3 Gd O1 149.76(10) 3_775 . ? O2 Gd O1 119.87(9) 3_775 . ? O2W Gd O1 80.11(10) . . ? O8 Gd O1 81.38(10) 4_575 . ? O7 Gd O1 79.04(9) 2_755 . ? O1W Gd O1 72.09(16) . . ? O3W Gd O1 133.29(12) . . ? O3 Gd O2 135.04(10) 3_775 . ? O2 Gd O2 68.48(10) 3_775 . ? O2W Gd O2 119.60(11) . . ? O8 Gd O2 69.56(9) 4_575 . ? O7 Gd O2 67.08(10) 2_755 . ? O1W Gd O2 115.14(14) . . ? O3W Gd O2 129.67(11) . . ? O1 Gd O2 51.40(8) . . ? O3 Gd C4 153.14(11) 3_775 . ? O2 Gd C4 94.11(10) 3_775 . ? O2W Gd C4 101.96(11) . . ? O8 Gd C4 76.49(10) 4_575 . ? O7 Gd C4 68.66(10) 2_755 . ? O1W Gd C4 92.34(15) . . ? O3W Gd C4 134.64(11) . . ? O1 Gd C4 25.85(9) . . ? O2 Gd C4 25.81(9) . . ? O3 Gd Gd 107.88(7) 3_775 3_775 ? O2 Gd Gd 35.76(6) 3_775 3_775 ? O2W Gd Gd 138.80(9) . 3_775 ? O8 Gd Gd 70.53(6) 4_575 3_775 ? O7 Gd Gd 68.17(7) 2_755 3_775 ? O1W Gd Gd 138.51(10) . 3_775 ? O3W Gd Gd 109.44(10) . 3_775 ? O1 Gd Gd 84.11(6) . 3_775 ? O2 Gd Gd 32.71(6) . 3_775 ? C4 Gd Gd 58.40(7) . 3_775 ? O3 Gd H12 107.3 3_775 . ? O2 Gd H12 126.0 3_775 . ? O2W Gd H12 88.2 . . ? O8 Gd H12 155.3 4_575 . ? O7 Gd H12 59.7 2_755 . ? O1W Gd H12 20.3 . . ? O3W Gd H12 51.5 . . ? O1 Gd H12 84.3 . . ? O2 Gd H12 115.7 . . ? C4 Gd H12 98.6 . . ? Gd Gd H12 127.8 3_775 . ? N2 Cd N1 101.87(12) . 2_845 ? N2 Cd O4 106.07(11) . 4_586 ? N1 Cd O4 135.43(10) 2_845 4_586 ? N2 Cd O6 146.66(11) . . ? N1 Cd O6 90.12(11) 2_845 . ? O4 Cd O6 85.20(11) 4_586 . ? N2 Cd O4 109.40(11) . 2_845 ? N1 Cd O4 70.51(10) 2_845 2_845 ? O4 Cd O4 67.79(11) 4_586 2_845 ? O6 Cd O4 103.92(11) . 2_845 ? N2 Cd O1 70.72(10) . . ? N1 Cd O1 89.11(10) 2_845 . ? O4 Cd O1 132.67(9) 4_586 . ? O6 Cd O1 78.59(10) . . ? O4 Cd O1 159.36(9) 2_845 . ? O5 S O8 110.91(18) . . ? O5 S O7 109.55(19) . . ? O8 S O7 109.59(17) . . ? O5 S O6 111.13(19) . . ? O8 S O6 108.06(18) . . ? O7 S O6 107.53(17) . . ? N2 C1 N1 114.0(3) . . ? N2 C1 H1A 123.0 . . ? N1 C1 H1A 123.0 . . ? N2 C2 C3 108.3(3) . . ? N2 C2 C4 117.8(3) . . ? C3 C2 C4 133.8(3) . . ? N1 C3 C2 107.5(3) . . ? N1 C3 C5 118.3(3) . . ? C2 C3 C5 134.3(3) . . ? O2 C4 O1 119.0(3) . . ? O2 C4 C2 121.5(3) . . ? O1 C4 C2 119.4(3) . . ? O2 C4 Gd 60.43(19) . . ? O1 C4 Gd 59.52(19) . . ? C2 C4 Gd 169.6(3) . . ? O3 C5 O4 121.8(3) . . ? O3 C5 C3 122.4(3) . . ? O4 C5 C3 115.8(3) . . ? C1 N1 C3 105.5(3) . . ? C1 N1 Cd 137.7(3) . 2_855 ? C3 N1 Cd 116.6(2) . 2_855 ? C1 N2 C2 104.7(3) . . ? C1 N2 Cd 137.9(3) . . ? C2 N2 Cd 117.3(2) . . ? C4 O1 Cd 112.7(2) . . ? C4 O1 Gd 94.6(2) . . ? Cd O1 Gd 152.33(11) . . ? C4 O2 Gd 153.8(3) . 3_775 ? C4 O2 Gd 93.8(2) . . ? Gd O2 Gd 111.52(10) 3_775 . ? C5 O3 Gd 153.2(3) . 3_775 ? C5 O4 Cd 123.6(2) . 4_585 ? C5 O4 Cd 117.0(2) . 2_855 ? Cd O4 Cd 112.21(11) 4_585 2_855 ? S O6 Cd 128.41(19) . . ? S O7 Gd 134.50(16) . 2_745 ? S O8 Gd 141.38(17) . 4_576 ? Gd O1W H11 110.2 . . ? Gd O1W H12 66.4 . . ? H11 O1W H12 107.6 . . ? Gd O2W H21 100.2 . . ? Gd O2W H22 121.4 . . ? H21 O2W H22 109.3 . . ? Gd O3W H31 121.6 . . ? Gd O3W H32 122.3 . . ? H31 O3W H32 109.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.836 _refine_diff_density_min -1.381 _refine_diff_density_rms 0.153 # Attachment '602029-Er-Cd(5)-142.cif' data_142 _database_code_depnum_ccdc_archive 'CCDC 602029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd Er N2 O11.50 S' _chemical_formula_weight 592.86 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' Cd Cd -0.8075 1.2024 '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 P21/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 8.6197(6) _cell_length_b 10.3244(5) _cell_length_c 13.8885(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.714(2) _cell_angle_gamma 90.00 _cell_volume 1210.24(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3615 _cell_measurement_theta_min 3.0863 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 8.892 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.169 _exptl_absorpt_correction_T_min 0.080 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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_radiation_detector CCD _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 9095 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2764 _reflns_number_gt 2614 _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^)+(0.0484P)^2^+4.3996P] 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 2764 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.92800(3) 0.89928(2) 0.103639(15) 0.01409(10) Uani 1 1 d . . . Cd Cd 1.37354(4) 0.98199(3) 0.36730(2) 0.01249(11) Uani 1 1 d . . . S S 1.19992(17) 0.72450(13) 0.45912(9) 0.0198(3) Uani 1 1 d . . . C1 C 1.5321(6) 1.2379(5) 0.2716(4) 0.0171(10) Uani 1 1 d . . . H1A H 1.6118 1.2544 0.3262 0.020 Uiso 1 1 calc R . . C2 C 1.3352(6) 1.1483(5) 0.1744(3) 0.0111(9) Uani 1 1 d . . . C3 C 1.3838(6) 1.2546(5) 0.1266(3) 0.0128(9) Uani 1 1 d . . . C4 C 1.2079(6) 1.0537(5) 0.1465(4) 0.0118(9) Uani 1 1 d . . . C5 C 1.3269(6) 1.3161(5) 0.0295(4) 0.0137(9) Uani 1 1 d . . . N1 N 1.5094(5) 1.3100(4) 0.1894(3) 0.0166(9) Uani 1 1 d . . . N2 N 1.4297(5) 1.1408(4) 0.2674(3) 0.0148(8) Uani 1 1 d . . . O1 O 1.1687(4) 0.9828(3) 0.2123(3) 0.0148(7) Uani 1 1 d . . . O2 O 1.1332(4) 1.0421(3) 0.0584(2) 0.0141(7) Uani 1 1 d . . . O3 O 1.2284(5) 1.2649(4) -0.0362(3) 0.0298(10) Uani 1 1 d . . . O4 O 1.3854(4) 1.4267(4) 0.0179(3) 0.0177(8) Uani 1 1 d . . . O5 O 1.3658(5) 0.7034(5) 0.4993(3) 0.0322(10) Uani 1 1 d . . . O6 O 1.1769(6) 0.8509(5) 0.4071(3) 0.0366(11) Uani 1 1 d . . . O7 O 1.1371(6) 0.6227(4) 0.3868(3) 0.0293(10) Uani 1 1 d . . . O8 O 1.1077(5) 0.7273(4) 0.5373(3) 0.0235(9) Uani 1 1 d . . . O1W O 0.8550(13) 0.9310(7) 0.2607(7) 0.126(5) Uani 1 1 d . . . O2W O 1.0068(6) 0.7216(5) 0.2042(3) 0.0392(12) Uani 1 1 d . . . O3W O 0.6411(9) 0.9452(8) 0.0953(7) 0.091(3) Uani 1 1 d . . . O4W O 0.9428(15) 1.0032(10) 0.4093(11) 0.062(4) Uani 0.50 1 d P . . H11 H 0.8121 0.8737 0.2903 0.080 Uiso 1 1 d R . . H12 H 0.7859 0.9757 0.2269 0.080 Uiso 1 1 d R . . H21 H 1.0446 0.6806 0.1637 0.080 Uiso 1 1 d R . . H22 H 1.0746 0.7234 0.2651 0.080 Uiso 1 1 d R . . H31 H 0.5696 0.8829 0.0899 0.080 Uiso 1 1 d R . . H32 H 0.5941 1.0200 0.0746 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 0.01836(16) 0.01303(14) 0.00831(14) 0.00089(7) -0.00333(10) -0.00667(8) Cd 0.0140(2) 0.01352(19) 0.00862(18) 0.00154(12) -0.00092(14) 0.00337(13) S 0.0244(7) 0.0224(7) 0.0109(6) 0.0003(5) -0.0006(5) -0.0113(5) C1 0.018(3) 0.021(3) 0.008(2) 0.0014(19) -0.0085(19) -0.007(2) C2 0.009(2) 0.015(2) 0.007(2) 0.0015(18) -0.0025(17) 0.0000(18) C3 0.015(2) 0.013(2) 0.009(2) -0.0010(18) -0.0005(18) -0.0040(18) C4 0.013(2) 0.010(2) 0.011(2) -0.0010(18) -0.0006(18) -0.0015(18) C5 0.012(2) 0.017(2) 0.011(2) 0.0024(18) 0.0005(18) -0.0025(18) N1 0.017(2) 0.019(2) 0.010(2) 0.0009(16) -0.0044(16) -0.0063(17) N2 0.014(2) 0.020(2) 0.0079(19) 0.0016(16) -0.0048(16) -0.0051(17) O1 0.0157(18) 0.0172(17) 0.0096(16) 0.0020(13) -0.0017(14) -0.0072(14) O2 0.0148(17) 0.0157(17) 0.0087(16) 0.0016(13) -0.0049(13) -0.0053(14) O3 0.032(2) 0.032(2) 0.017(2) 0.0075(17) -0.0143(17) -0.0240(19) O4 0.0178(19) 0.0191(18) 0.0132(18) 0.0063(15) -0.0038(15) -0.0063(15) O5 0.020(2) 0.050(3) 0.023(2) 0.005(2) -0.0032(17) -0.003(2) O6 0.041(3) 0.032(2) 0.032(3) 0.015(2) -0.004(2) -0.016(2) O7 0.037(3) 0.035(2) 0.015(2) -0.0086(17) 0.0036(18) -0.021(2) O8 0.032(2) 0.0192(19) 0.020(2) -0.0047(15) 0.0071(17) -0.0050(16) O1W 0.204(12) 0.077(5) 0.145(9) 0.067(6) 0.148(10) 0.059(7) O2W 0.057(3) 0.035(3) 0.018(2) 0.0130(19) -0.010(2) -0.002(2) O3W 0.058(4) 0.070(5) 0.154(8) -0.042(5) 0.041(5) -0.021(4) O4W 0.062(8) 0.039(6) 0.096(10) -0.020(6) 0.040(8) 0.002(5) _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 2.248(4) 3_775 ? Er O2 2.287(3) 3_775 ? Er O2W 2.322(4) . ? Er O8 2.353(4) 4_575 ? Er O7 2.384(4) 2_755 ? Er O1W 2.412(7) . ? Er O1 2.461(4) . ? Er O2 2.480(3) . ? Er O3W 2.497(7) . ? Er C4 2.852(5) . ? Er Er 3.9503(4) 3_775 ? Er H12 2.4293 . ? Er H21 2.5426 . ? Cd N1 2.261(4) 2_845 ? Cd N2 2.263(4) . ? Cd O4 2.277(4) 4_586 ? Cd O6 2.322(4) . ? Cd O4 2.417(4) 2_845 ? Cd O1 2.491(4) . ? S O5 1.442(4) . ? S O8 1.470(4) . ? S O7 1.479(4) . ? S O6 1.485(5) . ? C1 N2 1.329(7) . ? C1 N1 1.343(6) . ? C1 H1A 0.9300 . ? C2 N2 1.382(6) . ? C2 C3 1.391(6) . ? C2 C4 1.461(7) . ? C3 N1 1.370(6) . ? C3 C5 1.481(7) . ? C4 O2 1.267(6) . ? C4 O1 1.269(6) . ? C5 O3 1.233(6) . ? C5 O4 1.272(6) . ? N1 Cd 2.261(4) 2_855 ? O2 Er 2.287(3) 3_775 ? O3 Er 2.248(4) 3_775 ? O4 Cd 2.277(4) 4_585 ? O4 Cd 2.417(4) 2_855 ? O7 Er 2.384(4) 2_745 ? O8 Er 2.353(4) 4_576 ? O1W H11 0.8473 . ? O1W H12 0.8207 . ? O2W H21 0.8234 . ? O2W H22 0.9258 . ? O3W H31 0.8834 . ? O3W H32 0.8919 . ? 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 O2 77.92(13) 3_775 3_775 ? O3 Er O2W 74.48(17) 3_775 . ? O2 Er O2W 141.48(15) 3_775 . ? O3 Er O8 78.75(16) 3_775 4_575 ? O2 Er O8 78.48(13) 3_775 4_575 ? O2W Er O8 70.23(16) . 4_575 ? O3 Er O7 128.67(17) 3_775 2_755 ? O2 Er O7 77.80(13) 3_775 2_755 ? O2W Er O7 140.72(16) . 2_755 ? O8 Er O7 137.76(15) 4_575 2_755 ? O3 Er O1W 103.6(3) 3_775 . ? O2 Er O1W 143.5(2) 3_775 . ? O2W Er O1W 70.2(2) . . ? O8 Er O1W 138.0(2) 4_575 . ? O7 Er O1W 73.17(19) 2_755 . ? O3 Er O1 151.55(14) 3_775 . ? O2 Er O1 120.55(12) 3_775 . ? O2W Er O1 78.50(15) . . ? O8 Er O1 83.96(14) 4_575 . ? O7 Er O1 78.78(14) 2_755 . ? O1W Er O1 74.9(3) . . ? O3 Er O2 137.83(14) 3_775 . ? O2 Er O2 68.12(14) 3_775 . ? O2W Er O2 119.05(16) . . ? O8 Er O2 70.78(13) 4_575 . ? O7 Er O2 68.09(14) 2_755 . ? O1W Er O2 118.6(3) . . ? O1 Er O2 52.47(11) . . ? O3 Er O3W 67.6(2) 3_775 . ? O2 Er O3W 82.8(3) 3_775 . ? O2W Er O3W 110.1(3) . . ? O8 Er O3W 144.2(2) 4_575 . ? O7 Er O3W 65.0(2) 2_755 . ? O1W Er O3W 65.1(4) . . ? O1 Er O3W 131.7(2) . . ? O2 Er O3W 128.8(2) . . ? O3 Er C4 156.73(16) 3_775 . ? O2 Er C4 94.23(13) 3_775 . ? O2W Er C4 100.62(16) . . ? O8 Er C4 78.22(14) 4_575 . ? O7 Er C4 69.28(15) 2_755 . ? O1W Er C4 95.8(3) . . ? O1 Er C4 26.35(12) . . ? O2 Er C4 26.32(12) . . ? O3W Er C4 133.74(19) . . ? O3 Er Er 110.13(10) 3_775 3_775 ? O2 Er Er 35.63(9) 3_775 3_775 ? O2W Er Er 139.26(14) . 3_775 ? O8 Er Er 71.20(9) 4_575 3_775 ? O7 Er Er 69.11(10) 2_755 3_775 ? O1W Er Er 139.97(19) . 3_775 ? O1 Er Er 84.95(8) . 3_775 ? O2 Er Er 32.49(8) . 3_775 ? O3W Er Er 108.7(2) . 3_775 ? C4 Er Er 58.67(10) . 3_775 ? O3 Er H12 101.1 3_775 . ? O2 Er H12 124.0 3_775 . ? O2W Er H12 87.7 . . ? O8 Er H12 157.3 4_575 . ? O7 Er H12 59.2 2_755 . ? O1W Er H12 19.5 . . ? O1 Er H12 86.4 . . ? O2 Er H12 118.2 . . ? O3W Er H12 48.3 . . ? C4 Er H12 101.4 . . ? Er Er H12 128.3 3_775 . ? O3 Er H21 68.3 3_775 . ? O2 Er H21 123.7 3_775 . ? O2W Er H21 18.8 . . ? O8 Er H21 52.2 4_575 . ? O7 Er H21 157.3 2_755 . ? O1W Er H21 89.0 . . ? O1 Er H21 83.2 . . ? O2 Er H21 110.9 . . ? O3W Er H21 120.4 . . ? C4 Er H21 99.6 . . ? Er Er H21 123.0 3_775 . ? H12 Er H21 106.2 . . ? N1 Cd N2 100.91(16) 2_845 . ? N1 Cd O4 134.82(15) 2_845 4_586 ? N2 Cd O4 106.74(15) . 4_586 ? N1 Cd O6 91.38(18) 2_845 . ? N2 Cd O6 145.67(16) . . ? O4 Cd O6 85.49(16) 4_586 . ? N1 Cd O4 70.11(14) 2_845 2_845 ? N2 Cd O4 108.26(15) . 2_845 ? O4 Cd O4 67.64(15) 4_586 2_845 ? O6 Cd O4 106.06(15) . 2_845 ? N1 Cd O1 89.42(14) 2_845 . ? N2 Cd O1 70.73(13) . . ? O4 Cd O1 133.14(12) 4_586 . ? O6 Cd O1 77.54(14) . . ? O4 Cd O1 159.13(12) 2_845 . ? O5 S O8 111.0(3) . . ? O5 S O7 110.7(3) . . ? O8 S O7 109.7(2) . . ? O5 S O6 110.2(3) . . ? O8 S O6 107.6(3) . . ? O7 S O6 107.4(3) . . ? N2 C1 N1 113.6(4) . . ? N2 C1 H1A 123.2 . . ? N1 C1 H1A 123.2 . . ? N2 C2 C3 108.2(4) . . ? N2 C2 C4 118.6(4) . . ? C3 C2 C4 133.1(4) . . ? N1 C3 C2 107.6(4) . . ? N1 C3 C5 118.3(4) . . ? C2 C3 C5 134.2(5) . . ? O2 C4 O1 118.9(4) . . ? O2 C4 C2 121.8(4) . . ? O1 C4 C2 119.3(4) . . ? O2 C4 Er 60.2(2) . . ? O1 C4 Er 59.4(2) . . ? C2 C4 Er 170.7(3) . . ? O3 C5 O4 121.5(5) . . ? O3 C5 C3 122.8(5) . . ? O4 C5 C3 115.7(4) . . ? C1 N1 C3 105.6(4) . . ? C1 N1 Cd 137.1(4) . 2_855 ? C3 N1 Cd 117.2(3) . 2_855 ? C1 N2 C2 105.0(4) . . ? C1 N2 Cd 138.0(3) . . ? C2 N2 Cd 117.0(3) . . ? C4 O1 Er 94.3(3) . . ? C4 O1 Cd 112.3(3) . . ? Er O1 Cd 152.88(15) . . ? C4 O2 Er 153.6(3) . 3_775 ? C4 O2 Er 93.5(3) . . ? Er O2 Er 111.88(14) 3_775 . ? C5 O3 Er 153.7(4) . 3_775 ? C5 O4 Cd 122.9(3) . 4_585 ? C5 O4 Cd 116.0(3) . 2_855 ? Cd O4 Cd 112.36(14) 4_585 2_855 ? S O6 Cd 126.6(3) . . ? S O7 Er 135.1(3) . 2_745 ? S O8 Er 140.9(2) . 4_576 ? Er O1W H11 124.3 . . ? Er O1W H12 81.4 . . ? H11 O1W H12 109.5 . . ? Er O2W H21 95.9 . . ? Er O2W H22 126.0 . . ? H21 O2W H22 111.7 . . ? Er O3W H31 122.2 . . ? Er O3W H32 124.0 . . ? H31 O3W H32 109.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.485 _refine_diff_density_min -3.234 _refine_diff_density_rms 0.249 # Attachment '602030-Yb-Cd(6)-190.cif' data_190 _database_code_depnum_ccdc_archive 'CCDC 602030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd N2 O11.50 S Yb' _chemical_formula_weight 598.64 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.63880(10) _cell_length_b 10.2591(2) _cell_length_c 13.9386(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.9910(10) _cell_angle_gamma 90.00 _cell_volume 1208.37(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 95 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.75 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 9.700 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.068 _exptl_absorpt_correction_T_max 0.144 _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 6431 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.75 _reflns_number_total 2293 _reflns_number_gt 2241 _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^)+(0.0262P)^2^+8.0088P] 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 2293 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _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 Yb Yb 0.92917(3) 0.89897(2) 0.102039(15) 0.01719(9) Uani 1 1 d . . . Cd Cd 1.37198(4) 0.98189(3) 0.36732(2) 0.01365(10) Uani 1 1 d . . . S S 1.19756(18) 0.72500(15) 0.45877(9) 0.0250(3) Uani 1 1 d . . . C1 C 1.5309(6) 1.2378(5) 0.2712(4) 0.0188(11) Uani 1 1 d . . . H1A H 1.6106 1.2543 0.3259 0.023 Uiso 1 1 calc R . . C2 C 1.3344(6) 1.1483(5) 0.1745(3) 0.0134(10) Uani 1 1 d . . . C3 C 1.3850(6) 1.2536(5) 0.1270(4) 0.0145(10) Uani 1 1 d . . . C4 C 1.2053(5) 1.0530(5) 0.1462(3) 0.0120(9) Uani 1 1 d . . . C5 C 1.3284(6) 1.3148(5) 0.0285(4) 0.0162(10) Uani 1 1 d . . . N1 N 1.5099(5) 1.3098(4) 0.1893(3) 0.0186(9) Uani 1 1 d . . . N2 N 1.4280(5) 1.1406(4) 0.2674(3) 0.0172(9) Uani 1 1 d . . . O1 O 1.1657(4) 0.9832(3) 0.2116(3) 0.0169(7) Uani 1 1 d . . . O2 O 1.1329(4) 1.0417(4) 0.0582(3) 0.0170(7) Uani 1 1 d . . . O3 O 1.2314(5) 1.2614(4) -0.0381(3) 0.0292(10) Uani 1 1 d . . . O4 O 1.3849(4) 1.4270(4) 0.0176(3) 0.0191(8) Uani 1 1 d . . . O5 O 1.3644(5) 0.7060(5) 0.5006(3) 0.0346(10) Uani 1 1 d . . . O6 O 1.1714(6) 0.8511(5) 0.4049(4) 0.0485(15) Uani 1 1 d . . . O7 O 1.1373(6) 0.6201(5) 0.3878(3) 0.0413(13) Uani 1 1 d . . . O8 O 1.1041(5) 0.7292(4) 0.5355(3) 0.0257(9) Uani 1 1 d . . . O1W O 0.8721(17) 0.9402(11) 0.2695(9) 0.047(3) Uani 0.50 1 d P . . O1W' O 0.7963(16) 0.9058(16) 0.2233(10) 0.061(4) Uani 0.50 1 d P . . O2W O 1.0108(7) 0.7240(5) 0.2044(3) 0.0469(14) Uani 1 1 d . . . O3W O 0.6352(10) 0.9542(10) 0.0861(9) 0.120(4) Uani 1 1 d . . . O4W O 0.9337(15) 1.0008(11) 0.3996(11) 0.066(4) Uani 0.50 1 d P . . 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 Yb 0.02488(14) 0.01465(13) 0.01004(13) 0.00127(8) -0.00102(9) -0.00934(9) Cd 0.01622(19) 0.01407(19) 0.01048(18) 0.00198(13) 0.00238(14) 0.00409(13) S 0.0327(8) 0.0284(7) 0.0119(6) 0.0017(5) 0.0003(5) -0.0169(6) C1 0.020(3) 0.022(3) 0.012(2) 0.004(2) -0.001(2) -0.006(2) C2 0.017(2) 0.015(2) 0.008(2) 0.0006(19) 0.0028(18) 0.000(2) C3 0.015(2) 0.017(2) 0.011(2) -0.0027(19) 0.0008(19) -0.0030(19) C4 0.011(2) 0.014(2) 0.011(2) -0.0006(19) 0.0036(18) 0.0020(18) C5 0.013(2) 0.019(3) 0.017(2) 0.005(2) 0.0026(19) -0.005(2) N1 0.021(2) 0.020(2) 0.013(2) -0.0013(17) -0.0015(17) -0.0073(18) N2 0.018(2) 0.021(2) 0.011(2) 0.0017(17) -0.0007(17) -0.0059(18) O1 0.0184(18) 0.0186(18) 0.0138(17) 0.0040(14) 0.0031(14) -0.0055(14) O2 0.0198(18) 0.0193(18) 0.0102(17) 0.0005(14) -0.0011(14) -0.0059(15) O3 0.032(2) 0.034(2) 0.017(2) 0.0059(17) -0.0076(17) -0.0226(19) O4 0.0214(19) 0.0193(19) 0.0158(18) 0.0042(15) 0.0018(15) -0.0063(15) O5 0.030(2) 0.049(3) 0.023(2) 0.002(2) 0.0030(18) -0.006(2) O6 0.050(3) 0.051(3) 0.035(3) 0.027(2) -0.013(2) -0.031(3) O7 0.055(3) 0.054(3) 0.019(2) -0.014(2) 0.017(2) -0.035(3) O8 0.038(2) 0.0181(19) 0.023(2) -0.0047(16) 0.0096(18) -0.0081(17) O1W 0.072(9) 0.037(6) 0.040(7) 0.001(5) 0.030(6) -0.011(6) O1W' 0.046(7) 0.104(12) 0.041(7) 0.026(7) 0.024(6) -0.017(7) O2W 0.068(4) 0.039(3) 0.025(2) 0.018(2) -0.011(2) -0.008(3) O3W 0.077(6) 0.104(7) 0.195(11) -0.058(7) 0.063(7) -0.025(5) O4W 0.066(8) 0.036(6) 0.111(11) -0.036(7) 0.053(8) -0.008(5) _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 Yb O3 2.216(4) 3_775 ? Yb O1W' 2.232(12) . ? Yb O2 2.269(3) 3_775 ? Yb O2W 2.310(4) . ? Yb O8 2.335(4) 4_575 ? Yb O7 2.352(5) 2_755 ? Yb O1 2.440(4) . ? Yb O2 2.462(4) . ? Yb O1W 2.520(11) . ? Yb O3W 2.566(9) . ? Yb C4 2.820(5) . ? Yb Yb 3.9157(4) 3_775 ? Cd N2 2.259(4) . ? Cd N1 2.262(4) 2_845 ? Cd O4 2.276(4) 4_586 ? Cd O6 2.335(5) . ? Cd O4 2.429(4) 2_845 ? Cd O1 2.506(4) . ? S O5 1.451(5) . ? S O8 1.469(4) . ? S O7 1.481(4) . ? S O6 1.490(5) . ? C1 N2 1.330(7) . ? C1 N1 1.340(7) . ? C1 H1A 0.9300 . ? C2 N2 1.379(6) . ? C2 C3 1.384(7) . ? C2 C4 1.474(7) . ? C3 N1 1.364(6) . ? C3 C5 1.496(7) . ? C4 O2 1.260(6) . ? C4 O1 1.262(6) . ? C5 O3 1.242(6) . ? C5 O4 1.272(6) . ? N1 Cd 2.262(4) 2_855 ? O2 Yb 2.269(3) 3_775 ? O3 Yb 2.216(4) 3_775 ? O4 Cd 2.276(4) 4_585 ? O4 Cd 2.429(4) 2_855 ? O7 Yb 2.352(5) 2_745 ? O8 Yb 2.335(4) 4_576 ? 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 Yb O1W' 87.1(4) 3_775 . ? O3 Yb O2 78.65(13) 3_775 3_775 ? O1W' Yb O2 133.1(4) . 3_775 ? O3 Yb O2W 75.93(17) 3_775 . ? O1W' Yb O2W 72.3(4) . . ? O2 Yb O2W 142.74(16) 3_775 . ? O3 Yb O8 79.92(16) 3_775 4_575 ? O1W' Yb O8 142.6(4) . 4_575 ? O2 Yb O8 78.49(14) 3_775 4_575 ? O2W Yb O8 70.61(18) . 4_575 ? O3 Yb O7 126.87(19) 3_775 2_755 ? O1W' Yb O7 75.8(4) . 2_755 ? O2 Yb O7 77.85(14) 3_775 2_755 ? O2W Yb O7 139.41(17) . 2_755 ? O8 Yb O7 138.88(16) 4_575 2_755 ? O3 Yb O1 152.51(14) 3_775 . ? O1W' Yb O1 90.6(4) . . ? O2 Yb O1 121.13(12) 3_775 . ? O2W Yb O1 77.29(15) . . ? O8 Yb O1 85.48(14) 4_575 . ? O7 Yb O1 78.70(16) 2_755 . ? O3 Yb O2 139.63(14) 3_775 . ? O1W' Yb O2 132.5(4) . . ? O2 Yb O2 68.37(14) 3_775 . ? O2W Yb O2 118.23(16) . . ? O8 Yb O2 71.44(14) 4_575 . ? O7 Yb O2 68.73(16) 2_755 . ? O1 Yb O2 52.84(11) . . ? O3 Yb O1W 105.7(3) 3_775 . ? O1W' Yb O1W 20.5(4) . . ? O2 Yb O1W 144.6(3) 3_775 . ? O2W Yb O1W 69.6(3) . . ? O8 Yb O1W 136.9(3) 4_575 . ? O7 Yb O1W 71.7(3) 2_755 . ? O1 Yb O1W 70.2(3) . . ? O2 Yb O1W 114.7(3) . . ? O3 Yb O3W 66.6(2) 3_775 . ? O1W' Yb O3W 53.4(4) . . ? O2 Yb O3W 80.1(3) 3_775 . ? O2W Yb O3W 113.2(3) . . ? O8 Yb O3W 143.2(2) 4_575 . ? O7 Yb O3W 62.8(3) 2_755 . ? O1 Yb O3W 131.4(2) . . ? O2 Yb O3W 126.4(3) . . ? O1W Yb O3W 70.3(4) . . ? O3 Yb C4 159.07(16) 3_775 . ? O1W' Yb C4 111.2(4) . . ? O2 Yb C4 94.63(13) 3_775 . ? O2W Yb C4 99.49(17) . . ? O8 Yb C4 79.32(14) 4_575 . ? O7 Yb C4 69.65(17) 2_755 . ? O1 Yb C4 26.51(13) . . ? O2 Yb C4 26.51(13) . . ? O1W Yb C4 91.3(3) . . ? O3W Yb C4 132.2(2) . . ? O3 Yb Yb 111.41(10) 3_775 3_775 ? O1W' Yb Yb 145.2(4) . 3_775 ? O2 Yb Yb 35.77(9) 3_775 3_775 ? O2W Yb Yb 139.35(15) . 3_775 ? O8 Yb Yb 71.59(10) 4_575 3_775 ? O7 Yb Yb 69.51(11) 2_755 3_775 ? O1 Yb Yb 85.40(8) . 3_775 ? O2 Yb Yb 32.60(8) . 3_775 ? O1W Yb Yb 137.3(3) . 3_775 ? O3W Yb Yb 105.9(3) . 3_775 ? C4 Yb Yb 58.94(10) . 3_775 ? N2 Cd N1 100.22(17) . 2_845 ? N2 Cd O4 107.18(15) . 4_586 ? N1 Cd O4 134.64(14) 2_845 4_586 ? N2 Cd O6 144.70(16) . . ? N1 Cd O6 92.3(2) 2_845 . ? O4 Cd O6 85.79(17) 4_586 . ? N2 Cd O4 107.91(15) . 2_845 ? N1 Cd O4 70.03(14) 2_845 2_845 ? O4 Cd O4 67.49(15) 4_586 2_845 ? O6 Cd O4 107.39(15) . 2_845 ? N2 Cd O1 70.57(13) . . ? N1 Cd O1 89.60(14) 2_845 . ? O4 Cd O1 133.26(13) 4_586 . ? O6 Cd O1 76.70(14) . . ? O4 Cd O1 159.18(12) 2_845 . ? O5 S O8 111.2(3) . . ? O5 S O7 110.7(3) . . ? O8 S O7 109.7(2) . . ? O5 S O6 110.7(3) . . ? O8 S O6 107.0(3) . . ? O7 S O6 107.4(3) . . ? N2 C1 N1 114.1(5) . . ? N2 C1 H1A 122.9 . . ? N1 C1 H1A 122.9 . . ? N2 C2 C3 108.2(4) . . ? N2 C2 C4 118.5(4) . . ? C3 C2 C4 133.3(5) . . ? N1 C3 C2 108.2(4) . . ? N1 C3 C5 118.1(4) . . ? C2 C3 C5 133.7(5) . . ? O2 C4 O1 119.8(4) . . ? O2 C4 C2 121.1(4) . . ? O1 C4 C2 119.1(4) . . ? O2 C4 Yb 60.7(2) . . ? O1 C4 Yb 59.7(2) . . ? C2 C4 Yb 171.3(3) . . ? O3 C5 O4 121.7(5) . . ? O3 C5 C3 122.9(5) . . ? O4 C5 C3 115.4(4) . . ? C1 N1 C3 105.0(4) . . ? C1 N1 Cd 137.4(4) . 2_855 ? C3 N1 Cd 117.5(3) . 2_855 ? C1 N2 C2 104.5(4) . . ? C1 N2 Cd 138.0(4) . . ? C2 N2 Cd 117.5(3) . . ? C4 O1 Yb 93.8(3) . . ? C4 O1 Cd 112.2(3) . . ? Yb O1 Cd 153.17(16) . . ? C4 O2 Yb 154.3(3) . 3_775 ? C4 O2 Yb 92.8(3) . . ? Yb O2 Yb 111.63(14) 3_775 . ? C5 O3 Yb 153.8(4) . 3_775 ? C5 O4 Cd 122.4(3) . 4_585 ? C5 O4 Cd 115.6(3) . 2_855 ? Cd O4 Cd 112.51(15) 4_585 2_855 ? S O6 Cd 124.8(3) . . ? S O7 Yb 135.8(3) . 2_745 ? S O8 Yb 140.5(2) . 4_576 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.706 _refine_diff_density_min -1.821 _refine_diff_density_rms 0.161 # Attachment '602031-Y-Cd(7)-178.cif' data_178 _database_code_depnum_ccdc_archive 'CCDC 602031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd N2 O11.50 S Y' _chemical_formula_weight 514.51 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.6115(6) _cell_length_b 10.3674(7) _cell_length_c 13.8626(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.547(4) _cell_angle_gamma 90.00 _cell_volume 1212.59(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3241 _cell_measurement_theta_min 3.0863 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.2500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 6.764 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.184 _exptl_absorpt_correction_T_min 0.151 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 9195 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2772 _reflns_number_gt 2580 _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^)+(0.0289P)^2^+2.1268P] 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 2772 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Y Y 0.92730(4) 0.89920(3) 0.10467(2) 0.01336(9) Uani 1 1 d . . . Cd Cd 1.37440(3) 0.98157(2) 0.367112(16) 0.01322(8) Uani 1 1 d . . . S S 1.20119(10) 0.72357(9) 0.45929(6) 0.01842(18) Uani 1 1 d . . . C1 C 1.5324(4) 1.2367(3) 0.2712(3) 0.0192(7) Uani 1 1 d . . . H1A H 1.6126 1.2523 0.3257 0.023 Uiso 1 1 calc R . . C2 C 1.3353(4) 1.1484(3) 0.1745(2) 0.0123(6) Uani 1 1 d . . . C3 C 1.3840(4) 1.2548(3) 0.1273(2) 0.0134(6) Uani 1 1 d . . . C4 C 1.2085(4) 1.0544(3) 0.1467(2) 0.0129(6) Uani 1 1 d . . . C5 C 1.3259(4) 1.3173(3) 0.0300(2) 0.0153(6) Uani 1 1 d . . . N1 N 1.5090(3) 1.3097(3) 0.1900(2) 0.0162(6) Uani 1 1 d . . . N2 N 1.4300(3) 1.1395(3) 0.26662(19) 0.0153(6) Uani 1 1 d . . . O1 O 1.1701(3) 0.9826(2) 0.21220(17) 0.0161(5) Uani 1 1 d . . . O2 O 1.1345(3) 1.0421(2) 0.05843(16) 0.0156(5) Uani 1 1 d . . . O3 O 1.2257(3) 1.2658(3) -0.03513(19) 0.0285(6) Uani 1 1 d . . . O4 O 1.3857(3) 1.4256(2) 0.01828(17) 0.0195(5) Uani 1 1 d . . . O5 O 1.3677(3) 0.7002(3) 0.4981(2) 0.0325(7) Uani 1 1 d . . . O6 O 1.1775(3) 0.8499(3) 0.4078(2) 0.0316(7) Uani 1 1 d . . . O7 O 1.1360(3) 0.6232(3) 0.38602(18) 0.0254(6) Uani 1 1 d . . . O8 O 1.1099(3) 0.7257(2) 0.53804(18) 0.0226(6) Uani 1 1 d . . . O1W O 0.8641(7) 0.9331(4) 0.2666(4) 0.104(2) Uani 1 1 d . . . O2W O 1.0059(4) 0.7203(3) 0.2049(2) 0.0370(7) Uani 1 1 d . . . O3W O 0.6393(4) 0.9428(4) 0.0977(4) 0.0706(13) Uani 1 1 d . . . O4W O 0.9489(10) 1.0028(7) 0.4198(7) 0.063(2) Uani 0.50 1 d P . . H11 H 0.8125 0.8744 0.2913 0.080 Uiso 1 1 d R . . H12 H 0.8063 0.9764 0.2279 0.080 Uiso 1 1 d R . . H21 H 1.0453 0.6715 0.1695 0.080 Uiso 1 1 d R . . H22 H 1.0754 0.7243 0.2660 0.080 Uiso 1 1 d R . . H31 H 0.5700 0.8736 0.0909 0.080 Uiso 1 1 d R . . H32 H 0.5895 1.0207 0.0756 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 Y 0.01670(16) 0.01418(17) 0.00841(16) 0.00079(11) 0.00060(12) -0.00452(12) Cd 0.01564(13) 0.01430(13) 0.00956(12) 0.00122(8) 0.00211(9) 0.00245(9) S 0.0225(4) 0.0208(5) 0.0122(4) 0.0001(3) 0.0038(3) -0.0073(3) C1 0.0217(17) 0.0214(18) 0.0122(16) -0.0001(13) -0.0022(13) -0.0049(14) C2 0.0133(15) 0.0133(16) 0.0099(15) 0.0022(11) 0.0015(12) -0.0020(12) C3 0.0128(15) 0.0142(16) 0.0131(16) 0.0002(12) 0.0021(12) -0.0033(12) C4 0.0115(15) 0.0146(16) 0.0121(15) 0.0009(12) 0.0012(12) 0.0032(12) C5 0.0145(15) 0.0191(17) 0.0126(16) 0.0018(12) 0.0036(12) -0.0022(13) N1 0.0179(14) 0.0200(15) 0.0095(13) -0.0006(10) -0.0002(11) -0.0063(12) N2 0.0168(14) 0.0180(15) 0.0097(13) 0.0026(10) -0.0007(10) -0.0041(11) O1 0.0177(12) 0.0177(12) 0.0123(11) 0.0040(9) 0.0016(9) -0.0055(9) O2 0.0161(11) 0.0177(13) 0.0116(11) 0.0007(9) -0.0006(9) -0.0052(9) O3 0.0329(15) 0.0285(15) 0.0183(13) 0.0077(11) -0.0084(11) -0.0158(12) O4 0.0228(13) 0.0190(13) 0.0152(12) 0.0047(9) -0.0001(10) -0.0071(10) O5 0.0242(14) 0.0471(19) 0.0248(15) 0.0015(13) 0.0012(11) -0.0037(13) O6 0.0379(16) 0.0274(16) 0.0285(15) 0.0094(12) 0.0039(12) -0.0130(13) O7 0.0346(15) 0.0270(15) 0.0153(13) -0.0052(10) 0.0068(11) -0.0110(12) O8 0.0314(14) 0.0206(13) 0.0196(13) -0.0052(10) 0.0138(11) -0.0059(11) O1W 0.187(6) 0.058(3) 0.103(4) 0.040(3) 0.120(4) 0.037(3) O2W 0.056(2) 0.0327(17) 0.0195(14) 0.0100(12) 0.0002(13) 0.0023(14) O3W 0.040(2) 0.054(3) 0.124(4) -0.024(3) 0.031(2) -0.0121(19) O4W 0.066(5) 0.033(4) 0.096(7) -0.009(4) 0.034(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y O3 2.255(3) 3_775 ? Y O2 2.299(2) 3_775 ? Y O2W 2.335(3) . ? Y O8 2.363(2) 4_575 ? Y O7 2.395(3) 2_755 ? Y O1W 2.438(4) . ? Y O1 2.469(2) . ? Y O2 2.499(2) . ? Y O3W 2.504(4) . ? Y C4 2.868(3) . ? Y Y 3.9765(6) 3_775 ? Y H12 2.3148 . ? Cd N2 2.262(3) . ? Cd N1 2.265(3) 2_845 ? Cd O4 2.290(2) 4_586 ? Cd O6 2.333(3) . ? Cd O4 2.411(2) 2_845 ? Cd O1 2.489(2) . ? S O5 1.448(3) . ? S O8 1.468(2) . ? S O7 1.484(3) . ? S O6 1.486(3) . ? C1 N2 1.332(4) . ? C1 N1 1.338(4) . ? C1 H1A 0.9300 . ? C2 N2 1.373(4) . ? C2 C3 1.390(4) . ? C2 C4 1.457(4) . ? C3 N1 1.365(4) . ? C3 C5 1.489(4) . ? C4 O1 1.268(4) . ? C4 O2 1.268(4) . ? C5 O3 1.238(4) . ? C5 O4 1.260(4) . ? N1 Cd 2.265(3) 2_855 ? O2 Y 2.299(2) 3_775 ? O3 Y 2.255(3) 3_775 ? O4 Cd 2.290(2) 4_585 ? O4 Cd 2.411(2) 2_855 ? O7 Y 2.395(3) 2_745 ? O8 Y 2.363(2) 4_576 ? O1W H11 0.8641 . ? O1W H12 0.7933 . ? O2W H21 0.8232 . ? O2W H22 0.9347 . ? O3W H31 0.9254 . ? O3W H32 0.9368 . ? 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 Y O2 77.30(9) 3_775 3_775 ? O3 Y O2W 74.13(10) 3_775 . ? O2 Y O2W 141.08(10) 3_775 . ? O3 Y O8 78.15(10) 3_775 4_575 ? O2 Y O8 78.56(8) 3_775 4_575 ? O2W Y O8 70.19(10) . 4_575 ? O3 Y O7 129.72(10) 3_775 2_755 ? O2 Y O7 77.63(8) 3_775 2_755 ? O2W Y O7 141.28(10) . 2_755 ? O8 Y O7 136.80(9) 4_575 2_755 ? O3 Y O1W 106.50(16) 3_775 . ? O2 Y O1W 144.77(14) 3_775 . ? O2W Y O1W 70.02(13) . . ? O8 Y O1W 136.66(14) 4_575 . ? O7 Y O1W 73.47(12) 2_755 . ? O3 Y O1 151.13(9) 3_775 . ? O2 Y O1 120.16(8) 3_775 . ? O2W Y O1 79.01(9) . . ? O8 Y O1 83.02(9) 4_575 . ? O7 Y O1 78.60(9) 2_755 . ? O1W Y O1 73.25(16) . . ? O3 Y O2 136.55(9) 3_775 . ? O2 Y O2 68.11(9) 3_775 . ? O2W Y O2 119.12(10) . . ? O8 Y O2 70.08(8) 4_575 . ? O7 Y O2 67.74(9) 2_755 . ? O1W Y O2 116.94(15) . . ? O1 Y O2 52.08(7) . . ? O3 Y O3W 68.35(12) 3_775 . ? O2 Y O3W 83.21(14) 3_775 . ? O2W Y O3W 109.47(14) . . ? O8 Y O3W 144.62(12) 4_575 . ? O7 Y O3W 65.95(12) 2_755 . ? O1W Y O3W 66.90(19) . . ? O1 Y O3W 132.29(12) . . ? O2 Y O3W 129.47(12) . . ? O3 Y C4 155.46(10) 3_775 . ? O2 Y C4 94.07(8) 3_775 . ? O2W Y C4 101.09(10) . . ? O8 Y C4 77.63(9) 4_575 . ? O7 Y C4 68.74(9) 2_755 . ? O1W Y C4 93.85(16) . . ? O1 Y C4 26.14(8) . . ? O2 Y C4 26.19(8) . . ? O3W Y C4 134.12(11) . . ? O3 Y Y 109.22(7) 3_775 3_775 ? O2 Y Y 35.67(6) 3_775 3_775 ? O2W Y Y 139.08(8) . 3_775 ? O8 Y Y 70.81(6) 4_575 3_775 ? O7 Y Y 68.78(6) 2_755 3_775 ? O1W Y Y 139.19(11) . 3_775 ? O1 Y Y 84.50(5) . 3_775 ? O2 Y Y 32.44(5) . 3_775 ? O3W Y Y 109.34(12) . 3_775 ? C4 Y Y 58.47(6) . 3_775 ? O3 Y H12 105.5 3_775 . ? O2 Y H12 125.8 3_775 . ? O2W Y H12 87.4 . . ? O8 Y H12 155.7 4_575 . ? O7 Y H12 58.9 2_755 . ? O1W Y H12 19.0 . . ? O1 Y H12 83.4 . . ? O2 Y H12 115.7 . . ? O3W Y H12 51.5 . . ? C4 Y H12 98.2 . . ? Y Y H12 127.7 3_775 . ? N2 Cd N1 101.00(10) . 2_845 ? N2 Cd O4 106.49(10) . 4_586 ? N1 Cd O4 135.23(9) 2_845 4_586 ? N2 Cd O6 145.73(10) . . ? N1 Cd O6 91.08(11) 2_845 . ? O4 Cd O6 85.65(10) 4_586 . ? N2 Cd O4 108.71(9) . 2_845 ? N1 Cd O4 70.10(9) 2_845 2_845 ? O4 Cd O4 67.94(10) 4_586 2_845 ? O6 Cd O4 105.56(9) . 2_845 ? N2 Cd O1 70.47(9) . . ? N1 Cd O1 89.31(9) 2_845 . ? O4 Cd O1 132.92(8) 4_586 . ? O6 Cd O1 77.81(9) . . ? O4 Cd O1 159.06(8) 2_845 . ? O5 S O8 111.34(16) . . ? O5 S O7 110.35(18) . . ? O8 S O7 109.52(15) . . ? O5 S O6 110.91(17) . . ? O8 S O6 107.55(17) . . ? O7 S O6 107.04(16) . . ? N2 C1 N1 113.6(3) . . ? N2 C1 H1A 123.2 . . ? N1 C1 H1A 123.2 . . ? N2 C2 C3 108.2(3) . . ? N2 C2 C4 118.4(3) . . ? C3 C2 C4 133.4(3) . . ? N1 C3 C2 107.7(3) . . ? N1 C3 C5 118.3(3) . . ? C2 C3 C5 133.9(3) . . ? O1 C4 O2 118.7(3) . . ? O1 C4 C2 119.5(3) . . ? O2 C4 C2 121.9(3) . . ? O1 C4 Y 59.06(16) . . ? O2 C4 Y 60.44(16) . . ? C2 C4 Y 170.6(2) . . ? O3 C5 O4 122.2(3) . . ? O3 C5 C3 122.1(3) . . ? O4 C5 C3 115.6(3) . . ? C1 N1 C3 105.5(3) . . ? C1 N1 Cd 137.4(2) . 2_855 ? C3 N1 Cd 117.0(2) . 2_855 ? C1 N2 C2 104.9(3) . . ? C1 N2 Cd 137.5(2) . . ? C2 N2 Cd 117.5(2) . . ? C4 O1 Y 94.80(19) . . ? C4 O1 Cd 112.3(2) . . ? Y O1 Cd 152.44(10) . . ? C4 O2 Y 153.5(2) . 3_775 ? C4 O2 Y 93.37(19) . . ? Y O2 Y 111.89(9) 3_775 . ? C5 O3 Y 154.3(2) . 3_775 ? C5 O4 Cd 123.3(2) . 4_585 ? C5 O4 Cd 116.6(2) . 2_855 ? Cd O4 Cd 112.06(10) 4_585 2_855 ? S O6 Cd 126.55(17) . . ? S O7 Y 134.61(15) . 2_745 ? S O8 Y 141.28(15) . 4_576 ? Y O1W H11 119.5 . . ? Y O1W H12 71.7 . . ? H11 O1W H12 111.3 . . ? Y O2W H21 103.8 . . ? Y O2W H22 124.0 . . ? H21 O2W H22 107.6 . . ? Y O3W H31 118.5 . . ? Y O3W H32 123.6 . . ? H31 O3W H32 113.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.913 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.124 # Attachment '602032-Nd-Cd(8)-177.cif' data_177 _database_code_depnum_ccdc_archive 'CCDC 602032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd N2 Nd O11.50 S' _chemical_formula_weight 569.84 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.71200(10) _cell_length_b 10.5288(2) _cell_length_c 13.9024(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.0330(10) _cell_angle_gamma 90.00 _cell_volume 1251.65(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 81 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.67 _exptl_crystal_description purple _exptl_crystal_colour prism _exptl_crystal_size_max .40 _exptl_crystal_size_mid .31 _exptl_crystal_size_min .26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 6.041 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.122 _exptl_absorpt_correction_T_max 0.208 _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 6643 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.67 _reflns_number_total 2377 _reflns_number_gt 2309 _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^)+(0.0197P)^2^+8.4700P] 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 2377 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Nd Nd 0.92557(3) 0.89871(2) 0.107945(16) 0.01154(8) Uani 1 1 d . . . Cd Cd 1.37914(4) 0.98282(3) 0.36717(2) 0.01141(9) Uani 1 1 d . . . S S 1.20810(13) 0.72590(11) 0.46066(8) 0.0151(2) Uani 1 1 d . . . C1 C 1.5322(5) 1.2380(5) 0.2706(3) 0.0167(9) Uani 1 1 d . . . H1A H 1.6121 1.2534 0.3241 0.020 Uiso 1 1 calc R . . C2 C 1.3368(5) 1.1512(4) 0.1760(3) 0.0119(8) Uani 1 1 d . . . C3 C 1.3834(5) 1.2567(4) 0.1295(3) 0.0107(8) Uani 1 1 d . . . C4 C 1.2126(5) 1.0565(4) 0.1496(3) 0.0116(8) Uani 1 1 d . . . C5 C 1.3269(5) 1.3196(4) 0.0325(3) 0.0120(9) Uani 1 1 d . . . N1 N 1.5073(4) 1.3106(4) 0.1911(3) 0.0150(8) Uani 1 1 d . . . N2 N 1.4326(4) 1.1407(4) 0.2674(3) 0.0141(8) Uani 1 1 d . . . O1 O 1.1784(4) 0.9847(3) 0.2160(2) 0.0161(7) Uani 1 1 d . . . O2 O 1.1372(4) 1.0453(3) 0.0622(2) 0.0145(6) Uani 1 1 d . . . O3 O 1.2240(4) 1.2706(3) -0.0312(2) 0.0241(8) Uani 1 1 d . . . O4 O 1.3888(4) 1.4257(3) 0.0196(2) 0.0166(7) Uani 1 1 d . . . O5 O 1.3728(4) 0.6980(4) 0.4976(3) 0.0302(9) Uani 1 1 d . . . O6 O 1.1887(4) 0.8523(3) 0.4119(3) 0.0258(8) Uani 1 1 d . . . O7 O 1.1423(4) 0.6292(3) 0.3867(2) 0.0207(7) Uani 1 1 d . . . O8 O 1.1194(4) 0.7266(3) 0.5405(3) 0.0226(8) Uani 1 1 d . . . O1W O 0.8710(10) 0.9348(5) 0.2786(5) 0.089(3) Uani 1 1 d . . . O2W O 1.0049(5) 0.7118(4) 0.2072(3) 0.0349(10) Uani 1 1 d . . . O3W O 0.6332(5) 0.9417(4) 0.1004(4) 0.0494(13) Uani 1 1 d . . . O4W O 0.9626(11) 1.0067(8) 0.4347(7) 0.045(2) Uani 0.50 1 d P . . H11 H 0.8219 0.8633 0.2915 0.080 Uiso 1 1 d R . . H12 H 0.8157 0.9753 0.2281 0.080 Uiso 1 1 d R . . H21 H 1.0448 0.6806 0.1646 0.080 Uiso 1 1 d R . . H22 H 1.0749 0.7034 0.2660 0.080 Uiso 1 1 d R . . H31 H 0.5594 0.8725 0.0901 0.080 Uiso 1 1 d R . . H32 H 0.5889 1.0196 0.0758 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 Nd 0.01266(13) 0.01201(13) 0.00937(13) 0.00121(8) 0.00062(9) -0.00337(9) Cd 0.01289(17) 0.01127(16) 0.00965(16) 0.00115(11) 0.00109(12) 0.00200(12) S 0.0155(5) 0.0149(5) 0.0155(5) 0.0003(4) 0.0044(4) -0.0023(4) C1 0.016(2) 0.020(2) 0.012(2) 0.0000(18) -0.0047(17) -0.0064(19) C2 0.012(2) 0.014(2) 0.0098(19) 0.0013(17) 0.0013(16) -0.0012(17) C3 0.012(2) 0.011(2) 0.009(2) -0.0012(16) 0.0018(16) -0.0032(17) C4 0.0068(19) 0.013(2) 0.014(2) 0.0014(17) 0.0005(16) 0.0003(16) C5 0.010(2) 0.013(2) 0.014(2) 0.0037(17) 0.0032(17) -0.0007(17) N1 0.0147(19) 0.0160(19) 0.0133(18) -0.0005(15) 0.0002(15) -0.0047(16) N2 0.0155(18) 0.0154(19) 0.0096(17) 0.0027(15) -0.0022(14) -0.0032(16) O1 0.0170(16) 0.0174(16) 0.0132(15) 0.0042(13) 0.0006(13) -0.0052(13) O2 0.0126(15) 0.0166(16) 0.0123(15) 0.0020(13) -0.0027(12) -0.0054(13) O3 0.0278(19) 0.0225(18) 0.0169(17) 0.0056(14) -0.0089(14) -0.0129(15) O4 0.0163(16) 0.0155(16) 0.0164(16) 0.0063(13) -0.0011(13) -0.0061(13) O5 0.0166(18) 0.043(2) 0.030(2) 0.0008(18) 0.0015(15) -0.0012(17) O6 0.031(2) 0.0174(18) 0.030(2) 0.0067(15) 0.0083(16) -0.0050(16) O7 0.0273(19) 0.0164(17) 0.0173(17) -0.0031(13) 0.0013(14) -0.0026(15) O8 0.0282(19) 0.0196(18) 0.0235(18) -0.0047(14) 0.0138(15) -0.0050(15) O1W 0.177(8) 0.041(3) 0.079(4) 0.012(3) 0.100(5) 0.005(4) O2W 0.049(3) 0.029(2) 0.0227(19) 0.0080(16) -0.0021(18) 0.0048(19) O3W 0.026(2) 0.031(2) 0.095(4) -0.009(3) 0.023(2) -0.0047(19) O4W 0.048(6) 0.036(5) 0.049(6) -0.006(4) 0.005(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O3 2.342(3) 3_775 ? Nd O2 2.397(3) 3_775 ? Nd O2W 2.427(4) . ? Nd O8 2.465(3) 4_575 ? Nd O7 2.502(3) 2_755 ? Nd O1W 2.536(5) . ? Nd O3W 2.569(4) . ? Nd O2 2.576(3) . ? Nd O1 2.581(3) . ? Nd C4 2.965(4) . ? Nd Nd 4.0901(4) 3_775 ? Nd H12 2.2290 . ? Nd H21 2.5805 . ? Cd N2 2.270(4) . ? Cd N1 2.287(4) 2_845 ? Cd O4 2.314(3) 4_586 ? Cd O6 2.329(4) . ? Cd O4 2.390(3) 2_845 ? Cd O1 2.463(3) . ? S O5 1.459(4) . ? S O8 1.469(3) . ? S O7 1.483(3) . ? S O6 1.488(4) . ? C1 N1 1.327(6) . ? C1 N2 1.338(6) . ? C1 H1A 0.9300 . ? C2 N2 1.385(6) . ? C2 C3 1.385(6) . ? C2 C4 1.465(6) . ? C3 N1 1.367(6) . ? C3 C5 1.498(6) . ? C4 O1 1.272(5) . ? C4 O2 1.272(5) . ? C5 O3 1.244(6) . ? C5 O4 1.268(5) . ? N1 Cd 2.287(4) 2_855 ? O2 Nd 2.397(3) 3_775 ? O3 Nd 2.342(3) 3_775 ? O4 Cd 2.314(3) 4_585 ? O4 Cd 2.390(3) 2_855 ? O7 Nd 2.502(3) 2_745 ? O8 Nd 2.465(3) 4_576 ? O1W H11 0.9011 . ? O1W H12 0.8813 . ? O2W H21 0.8117 . ? O2W H22 0.9262 . ? O3W H31 0.9644 . ? O3W H32 0.9419 . ? O4W O4W 1.813(19) 3_776 ? 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 Nd O2 74.65(11) 3_775 3_775 ? O3 Nd O2W 73.43(13) 3_775 . ? O2 Nd O2W 138.31(12) 3_775 . ? O3 Nd O8 77.37(13) 3_775 4_575 ? O2 Nd O8 78.46(11) 3_775 4_575 ? O2W Nd O8 68.97(13) . 4_575 ? O3 Nd O7 129.63(12) 3_775 2_755 ? O2 Nd O7 77.31(11) 3_775 2_755 ? O2W Nd O7 144.36(12) . 2_755 ? O8 Nd O7 135.50(11) 4_575 2_755 ? O3 Nd O1W 110.67(18) 3_775 . ? O2 Nd O1W 146.94(19) 3_775 . ? O2W Nd O1W 70.94(17) . . ? O8 Nd O1W 134.5(2) 4_575 . ? O7 Nd O1W 74.88(15) 2_755 . ? O3 Nd O3W 69.79(14) 3_775 . ? O2 Nd O3W 83.05(15) 3_775 . ? O2W Nd O3W 109.77(16) . . ? O8 Nd O3W 145.56(14) 4_575 . ? O7 Nd O3W 65.94(13) 2_755 . ? O1W Nd O3W 69.5(2) . . ? O3 Nd O2 134.89(11) 3_775 . ? O2 Nd O2 69.38(11) 3_775 . ? O2W Nd O2 119.15(13) . . ? O8 Nd O2 69.63(11) 4_575 . ? O7 Nd O2 67.08(11) 2_755 . ? O1W Nd O2 114.36(18) . . ? O3W Nd O2 129.43(13) . . ? O3 Nd O1 150.55(12) 3_775 . ? O2 Nd O1 119.76(10) 3_775 . ? O2W Nd O1 80.51(12) . . ? O8 Nd O1 80.70(12) 4_575 . ? O7 Nd O1 79.79(11) 2_755 . ? O1W Nd O1 72.2(2) . . ? O3W Nd O1 133.71(14) . . ? O2 Nd O1 50.37(10) . . ? O3 Nd C4 152.93(13) 3_775 . ? O2 Nd C4 94.57(11) 3_775 . ? O2W Nd C4 101.87(13) . . ? O8 Nd C4 76.15(12) 4_575 . ? O7 Nd C4 69.27(12) 2_755 . ? O1W Nd C4 92.0(2) . . ? O3W Nd C4 134.55(13) . . ? O2 Nd C4 25.30(11) . . ? O1 Nd C4 25.31(11) . . ? O3 Nd Nd 106.82(9) 3_775 3_775 ? O2 Nd Nd 36.12(7) 3_775 3_775 ? O2W Nd Nd 138.11(11) . 3_775 ? O8 Nd Nd 70.34(8) 4_575 3_775 ? O7 Nd Nd 68.04(8) 2_755 3_775 ? O1W Nd Nd 138.67(13) . 3_775 ? O3W Nd Nd 109.21(12) . 3_775 ? O2 Nd Nd 33.26(7) . 3_775 ? O1 Nd Nd 83.64(7) . 3_775 ? C4 Nd Nd 58.49(8) . 3_775 ? O3 Nd H12 109.6 3_775 . ? O2 Nd H12 126.9 3_775 . ? O2W Nd H12 89.0 . . ? O8 Nd H12 154.4 4_575 . ? O7 Nd H12 59.3 2_755 . ? O1W Nd H12 20.0 . . ? O3W Nd H12 53.3 . . ? O2 Nd H12 113.5 . . ? O1 Nd H12 83.0 . . ? C4 Nd H12 96.8 . . ? Nd Nd H12 127.1 3_775 . ? O3 Nd H21 67.6 3_775 . ? O2 Nd H21 121.5 3_775 . ? O2W Nd H21 18.3 . . ? O8 Nd H21 51.3 4_575 . ? O7 Nd H21 159.6 2_755 . ? O1W Nd H21 89.1 . . ? O3W Nd H21 120.5 . . ? O2 Nd H21 110.1 . . ? O1 Nd H21 83.4 . . ? C4 Nd H21 99.4 . . ? Nd Nd H21 121.5 3_775 . ? H12 Nd H21 107.4 . . ? N2 Cd N1 102.15(14) . 2_845 ? N2 Cd O4 106.21(13) . 4_586 ? N1 Cd O4 135.40(12) 2_845 4_586 ? N2 Cd O6 146.67(13) . . ? N1 Cd O6 90.32(14) 2_845 . ? O4 Cd O6 84.48(13) 4_586 . ? N2 Cd O4 109.90(13) . 2_845 ? N1 Cd O4 70.42(12) 2_845 2_845 ? O4 Cd O4 67.90(13) 4_586 2_845 ? O6 Cd O4 103.39(13) . 2_845 ? N2 Cd O1 70.61(12) . . ? N1 Cd O1 89.35(12) 2_845 . ? O4 Cd O1 132.31(11) 4_586 . ? O6 Cd O1 78.87(12) . . ? O4 Cd O1 159.57(11) 2_845 . ? O5 S O8 111.1(2) . . ? O5 S O7 109.2(2) . . ? O8 S O7 109.8(2) . . ? O5 S O6 111.0(2) . . ? O8 S O6 108.0(2) . . ? O7 S O6 107.7(2) . . ? N1 C1 N2 114.3(4) . . ? N1 C1 H1A 122.9 . . ? N2 C1 H1A 122.9 . . ? N2 C2 C3 108.2(4) . . ? N2 C2 C4 117.5(4) . . ? C3 C2 C4 134.2(4) . . ? N1 C3 C2 107.9(4) . . ? N1 C3 C5 117.7(4) . . ? C2 C3 C5 134.4(4) . . ? O1 C4 O2 119.3(4) . . ? O1 C4 C2 119.2(4) . . ? O2 C4 C2 121.5(4) . . ? O1 C4 Nd 60.2(2) . . ? O2 C4 Nd 60.0(2) . . ? C2 C4 Nd 170.0(3) . . ? O3 C5 O4 122.2(4) . . ? O3 C5 C3 121.6(4) . . ? O4 C5 C3 116.2(4) . . ? C1 N1 C3 105.5(4) . . ? C1 N1 Cd 137.6(3) . 2_855 ? C3 N1 Cd 116.8(3) . 2_855 ? C1 N2 C2 104.1(4) . . ? C1 N2 Cd 138.4(3) . . ? C2 N2 Cd 117.4(3) . . ? C4 O1 Cd 113.4(3) . . ? C4 O1 Nd 94.5(3) . . ? Cd O1 Nd 151.79(14) . . ? C4 O2 Nd 154.0(3) . 3_775 ? C4 O2 Nd 94.7(3) . . ? Nd O2 Nd 110.62(11) 3_775 . ? C5 O3 Nd 154.4(3) . 3_775 ? C5 O4 Cd 123.7(3) . 4_585 ? C5 O4 Cd 117.2(3) . 2_855 ? Cd O4 Cd 112.10(13) 4_585 2_855 ? S O6 Cd 128.7(2) . . ? S O7 Nd 135.1(2) . 2_745 ? S O8 Nd 141.5(2) . 4_576 ? Nd O1W H11 104.0 . . ? Nd O1W H12 59.9 . . ? H11 O1W H12 110.8 . . ? Nd O2W H21 91.6 . . ? Nd O2W H22 130.3 . . ? H21 O2W H22 107.7 . . ? Nd O3W H31 120.0 . . ? Nd O3W H32 120.2 . . ? H31 O3W H32 112.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.742 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.138 # Attachment '602033-Pr-Cd(9)-176.cif' data_176 _database_code_depnum_ccdc_archive 'CCDC 602033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Cd N2 O11.50 Pr S' _chemical_formula_weight 566.51 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.75380(10) _cell_length_b 10.5445(2) _cell_length_c 13.9138(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.0100(10) _cell_angle_gamma 90.00 _cell_volume 1260.67(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.68 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max .35 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 5.744 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_T_max 0.563 _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 6707 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2388 _reflns_number_gt 2136 _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^)+(0.0172P)^2^+16.5562P] 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 2388 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _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 Pr Pr 0.92567(4) 0.89838(4) 0.10825(3) 0.01571(12) Uani 1 1 d . . . Cd Cd 1.37977(6) 0.98288(5) 0.36720(4) 0.01394(14) Uani 1 1 d . . . S S 1.2092(2) 0.72680(18) 0.46123(13) 0.0190(4) Uani 1 1 d . . . C1 C 1.5329(9) 1.2377(7) 0.2717(5) 0.0209(16) Uani 1 1 d . . . H1A H 1.6125 1.2525 0.3251 0.025 Uiso 1 1 calc R . . C2 C 1.3374(8) 1.1508(7) 0.1762(5) 0.0145(14) Uani 1 1 d . . . C3 C 1.3834(8) 1.2574(7) 0.1283(5) 0.0140(14) Uani 1 1 d . . . C4 C 1.2138(7) 1.0564(6) 0.1503(5) 0.0110(13) Uani 1 1 d . . . C5 C 1.3271(8) 1.3197(7) 0.0318(5) 0.0147(14) Uani 1 1 d . . . N1 N 1.5073(7) 1.3110(6) 0.1906(4) 0.0176(13) Uani 1 1 d . . . N2 N 1.4322(7) 1.1414(6) 0.2673(4) 0.0154(12) Uani 1 1 d . . . O1 O 1.1802(6) 0.9847(5) 0.2168(4) 0.0192(11) Uani 1 1 d . . . O2 O 1.1371(6) 1.0452(5) 0.0631(4) 0.0200(11) Uani 1 1 d . . . O3 O 1.2254(7) 1.2714(5) -0.0312(4) 0.0291(13) Uani 1 1 d . . . O4 O 1.3891(6) 1.4252(5) 0.0193(4) 0.0187(11) Uani 1 1 d . . . O5 O 1.3725(6) 0.6991(6) 0.4973(4) 0.0342(14) Uani 1 1 d . . . O6 O 1.1900(7) 0.8530(5) 0.4121(4) 0.0292(13) Uani 1 1 d . . . O7 O 1.1425(6) 0.6298(5) 0.3866(4) 0.0254(12) Uani 1 1 d . . . O8 O 1.1202(6) 0.7276(5) 0.5413(4) 0.0263(12) Uani 1 1 d . . . O1W O 0.8716(15) 0.9351(8) 0.2805(7) 0.104(4) Uani 1 1 d . . . O2W O 1.0046(8) 0.7106(6) 0.2091(4) 0.0410(16) Uani 1 1 d . . . O3W O 0.6314(8) 0.9418(7) 0.1000(7) 0.057(2) Uani 1 1 d . . . O4W O 0.9593(18) 1.0053(14) 0.4335(11) 0.060(4) Uani 0.50 1 d P . . H11 H 0.8260 0.8727 0.2977 0.080 Uiso 1 1 d R . . H12 H 0.8098 0.9747 0.2343 0.080 Uiso 1 1 d R . . H21 H 1.0494 0.6800 0.1712 0.080 Uiso 1 1 d R . . H22 H 1.0795 0.7228 0.2727 0.080 Uiso 1 1 d R . . H31 H 0.5635 0.8819 0.0823 0.080 Uiso 1 1 d R . . H32 H 0.5930 1.0170 0.0820 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 Pr 0.0172(2) 0.0154(2) 0.0133(2) 0.00140(16) 0.00000(14) -0.00435(16) Cd 0.0161(3) 0.0135(3) 0.0118(3) 0.0012(2) 0.00131(19) 0.0021(2) S 0.0213(9) 0.0186(9) 0.0179(9) 0.0006(7) 0.0057(7) -0.0030(7) C1 0.022(4) 0.025(4) 0.014(4) 0.000(3) -0.001(3) -0.003(3) C2 0.013(3) 0.016(3) 0.013(3) 0.004(3) 0.000(3) -0.001(3) C3 0.015(3) 0.014(3) 0.013(3) 0.000(3) 0.002(3) -0.005(3) C4 0.008(3) 0.015(3) 0.009(3) -0.002(3) -0.001(2) 0.000(3) C5 0.012(3) 0.018(4) 0.014(3) 0.002(3) 0.003(3) 0.004(3) N1 0.022(3) 0.016(3) 0.014(3) -0.002(2) 0.002(2) -0.006(3) N2 0.015(3) 0.018(3) 0.011(3) 0.002(2) -0.003(2) -0.007(2) O1 0.021(3) 0.020(3) 0.016(3) 0.006(2) 0.003(2) -0.008(2) O2 0.019(3) 0.022(3) 0.018(3) 0.005(2) 0.001(2) -0.006(2) O3 0.034(3) 0.030(3) 0.017(3) 0.004(2) -0.012(2) -0.013(3) O4 0.020(3) 0.016(3) 0.019(3) 0.007(2) 0.000(2) -0.007(2) O5 0.019(3) 0.048(4) 0.032(3) 0.000(3) -0.002(2) -0.002(3) O6 0.035(3) 0.018(3) 0.035(3) 0.007(2) 0.008(3) -0.005(2) O7 0.037(3) 0.017(3) 0.021(3) -0.006(2) 0.003(2) -0.007(2) O8 0.033(3) 0.026(3) 0.022(3) -0.002(2) 0.011(2) -0.004(2) O1W 0.206(13) 0.048(5) 0.092(7) 0.014(5) 0.112(8) 0.012(7) O2W 0.052(4) 0.037(4) 0.030(3) 0.009(3) -0.001(3) -0.003(3) O3W 0.031(4) 0.038(4) 0.106(7) -0.012(4) 0.025(4) -0.007(3) O4W 0.062(10) 0.049(9) 0.068(10) 0.001(8) 0.008(8) 0.010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr O3 2.358(5) 3_775 ? Pr O2 2.417(5) 3_775 ? Pr O2W 2.448(6) . ? Pr O8 2.478(5) 4_575 ? Pr O7 2.516(5) 2_755 ? Pr O1W 2.560(8) . ? Pr O2 2.581(5) . ? Pr O3W 2.597(7) . ? Pr O1 2.605(5) . ? Pr C4 2.986(6) . ? Pr Pr 4.1059(8) 3_775 ? Pr H12 2.3299 . ? Pr H21 2.6230 . ? Cd N2 2.275(6) . ? Cd N1 2.283(6) 2_845 ? Cd O4 2.315(5) 4_586 ? Cd O6 2.328(5) . ? Cd O4 2.395(5) 2_845 ? Cd O1 2.457(5) . ? S O5 1.452(6) . ? S O8 1.476(5) . ? S O6 1.491(6) . ? S O7 1.495(5) . ? C1 N2 1.339(9) . ? C1 N1 1.350(9) . ? C1 H1A 0.9300 . ? C2 N2 1.380(9) . ? C2 C3 1.404(10) . ? C2 C4 1.463(9) . ? C3 N1 1.375(9) . ? C3 C5 1.492(9) . ? C4 O1 1.272(8) . ? C4 O2 1.275(8) . ? C5 O3 1.233(8) . ? C5 O4 1.264(9) . ? N1 Cd 2.283(6) 2_855 ? O2 Pr 2.417(5) 3_775 ? O3 Pr 2.358(5) 3_775 ? O4 Cd 2.315(5) 4_585 ? O4 Cd 2.395(5) 2_855 ? O7 Pr 2.516(5) 2_745 ? O8 Pr 2.478(5) 4_576 ? O1W H11 0.8282 . ? O1W H12 0.8644 . ? O2W H21 0.7841 . ? O2W H22 1.0040 . ? O3W H31 0.8700 . ? O3W H32 0.8785 . ? 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 Pr O2 74.71(17) 3_775 3_775 ? O3 Pr O2W 73.7(2) 3_775 . ? O2 Pr O2W 138.6(2) 3_775 . ? O3 Pr O8 77.8(2) 3_775 4_575 ? O2 Pr O8 78.68(18) 3_775 4_575 ? O2W Pr O8 69.1(2) . 4_575 ? O3 Pr O7 129.34(19) 3_775 2_755 ? O2 Pr O7 77.23(17) 3_775 2_755 ? O2W Pr O7 144.1(2) . 2_755 ? O8 Pr O7 135.58(18) 4_575 2_755 ? O3 Pr O1W 110.6(3) 3_775 . ? O2 Pr O1W 147.0(3) 3_775 . ? O2W Pr O1W 70.6(3) . . ? O8 Pr O1W 134.2(3) 4_575 . ? O7 Pr O1W 74.9(2) 2_755 . ? O3 Pr O2 135.30(18) 3_775 . ? O2 Pr O2 69.56(18) 3_775 . ? O2W Pr O2 119.18(19) . . ? O8 Pr O2 69.74(18) 4_575 . ? O7 Pr O2 67.05(17) 2_755 . ? O1W Pr O2 114.0(3) . . ? O3 Pr O3W 69.4(2) 3_775 . ? O2 Pr O3W 82.9(2) 3_775 . ? O2W Pr O3W 109.7(2) . . ? O8 Pr O3W 145.6(2) 4_575 . ? O7 Pr O3W 65.9(2) 2_755 . ? O1W Pr O3W 69.9(4) . . ? O2 Pr O3W 129.4(2) . . ? O3 Pr O1 150.65(18) 3_775 . ? O2 Pr O1 119.61(16) 3_775 . ? O2W Pr O1 80.43(19) . . ? O8 Pr O1 80.33(17) 4_575 . ? O7 Pr O1 79.99(17) 2_755 . ? O1W Pr O1 72.3(3) . . ? O2 Pr O1 50.04(15) . . ? O3W Pr O1 134.1(2) . . ? O3 Pr C4 153.1(2) 3_775 . ? O2 Pr C4 94.62(17) 3_775 . ? O2W Pr C4 101.8(2) . . ? O8 Pr C4 75.97(18) 4_575 . ? O7 Pr C4 69.47(18) 2_755 . ? O1W Pr C4 91.9(3) . . ? O2 Pr C4 25.15(16) . . ? O3W Pr C4 134.7(2) . . ? O1 Pr C4 25.13(16) . . ? O3 Pr Pr 106.95(13) 3_775 3_775 ? O2 Pr Pr 36.09(12) 3_775 3_775 ? O2W Pr Pr 138.44(17) . 3_775 ? O8 Pr Pr 70.54(13) 4_575 3_775 ? O7 Pr Pr 67.96(12) 2_755 3_775 ? O1W Pr Pr 138.5(2) . 3_775 ? O2 Pr Pr 33.48(11) . 3_775 ? O3W Pr Pr 109.04(19) . 3_775 ? O1 Pr Pr 83.52(11) . 3_775 ? C4 Pr Pr 58.56(12) . 3_775 ? O3 Pr H12 108.5 3_775 . ? O2 Pr H12 127.4 3_775 . ? O2W Pr H12 87.9 . . ? O8 Pr H12 153.8 4_575 . ? O7 Pr H12 60.3 2_755 . ? O1W Pr H12 19.6 . . ? O2 Pr H12 114.3 . . ? O3W Pr H12 53.3 . . ? O1 Pr H12 83.7 . . ? C4 Pr H12 97.6 . . ? Pr Pr H12 128.1 3_775 . ? O3 Pr H21 69.2 3_775 . ? O2 Pr H21 123.2 3_775 . ? O2W Pr H21 17.3 . . ? O8 Pr H21 52.1 4_575 . ? O7 Pr H21 157.9 2_755 . ? O1W Pr H21 87.6 . . ? O2 Pr H21 109.8 . . ? O3W Pr H21 120.8 . . ? O1 Pr H21 81.9 . . ? C4 Pr H21 98.3 . . ? Pr Pr H21 122.3 3_775 . ? H12 Pr H21 105.2 . . ? N2 Cd N1 102.5(2) . 2_845 ? N2 Cd O4 105.9(2) . 4_586 ? N1 Cd O4 135.46(19) 2_845 4_586 ? N2 Cd O6 146.4(2) . . ? N1 Cd O6 90.4(2) 2_845 . ? O4 Cd O6 84.5(2) 4_586 . ? N2 Cd O4 110.23(19) . 2_845 ? N1 Cd O4 70.29(18) 2_845 2_845 ? O4 Cd O4 68.03(19) 4_586 2_845 ? O6 Cd O4 103.29(19) . 2_845 ? N2 Cd O1 70.59(18) . . ? N1 Cd O1 89.48(19) 2_845 . ? O4 Cd O1 132.12(17) 4_586 . ? O6 Cd O1 78.78(18) . . ? O4 Cd O1 159.59(17) 2_845 . ? O5 S O8 111.5(3) . . ? O5 S O6 110.9(4) . . ? O8 S O6 108.1(3) . . ? O5 S O7 109.3(4) . . ? O8 S O7 109.6(3) . . ? O6 S O7 107.3(3) . . ? N2 C1 N1 113.2(6) . . ? N2 C1 H1A 123.4 . . ? N1 C1 H1A 123.4 . . ? N2 C2 C3 108.5(6) . . ? N2 C2 C4 117.6(6) . . ? C3 C2 C4 133.9(6) . . ? N1 C3 C2 107.0(6) . . ? N1 C3 C5 118.2(6) . . ? C2 C3 C5 134.8(6) . . ? O1 C4 O2 119.0(6) . . ? O1 C4 C2 119.2(6) . . ? O2 C4 C2 121.8(6) . . ? O1 C4 Pr 60.5(3) . . ? O2 C4 Pr 59.4(3) . . ? C2 C4 Pr 170.0(5) . . ? O3 C5 O4 122.4(6) . . ? O3 C5 C3 121.8(6) . . ? O4 C5 C3 115.7(6) . . ? C1 N1 C3 106.0(6) . . ? C1 N1 Cd 137.3(5) . 2_855 ? C3 N1 Cd 116.5(4) . 2_855 ? C1 N2 C2 105.2(6) . . ? C1 N2 Cd 137.5(5) . . ? C2 N2 Cd 117.3(4) . . ? C4 O1 Cd 113.5(4) . . ? C4 O1 Pr 94.4(4) . . ? Cd O1 Pr 151.8(2) . . ? C4 O2 Pr 153.6(5) . 3_775 ? C4 O2 Pr 95.5(4) . . ? Pr O2 Pr 110.44(18) 3_775 . ? C5 O3 Pr 154.4(5) . 3_775 ? C5 O4 Cd 123.6(4) . 4_585 ? C5 O4 Cd 117.6(4) . 2_855 ? Cd O4 Cd 111.97(19) 4_585 2_855 ? S O6 Cd 128.6(3) . . ? S O7 Pr 135.0(3) . 2_745 ? S O8 Pr 141.3(3) . 4_576 ? Pr O1W H11 109.6 . . ? Pr O1W H12 65.0 . . ? H11 O1W H12 109.3 . . ? Pr O2W H21 94.0 . . ? Pr O2W H22 117.8 . . ? H21 O2W H22 108.5 . . ? Pr O3W H31 120.2 . . ? Pr O3W H32 119.6 . . ? H31 O3W H32 111.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.290 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.172