# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Huabin Zhang' _publ_contact_author_email swdu@fjirsm.ac.cn loop_ _publ_author_name 'Huabin Zhang' 'Shaowu Du' 'Mingjian Zhang' 'Chong-Bin Tian' 'Ning Li' 'Zhi-Hua Li' data_1 _database_code_depnum_ccdc_archive 'CCDC 860628' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 H2 K O9 S2 Sm' _chemical_formula_weight 399.59 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' 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0693(15) _cell_length_b 8.4668(8) _cell_length_c 10.377(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.938(7) _cell_angle_gamma 90.00 _cell_volume 774.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2368 _cell_measurement_theta_min 3.3362 _cell_measurement_theta_max 27.4817 _exptl_crystal_description PRISM _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 8.683 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5969 _exptl_absorpt_correction_T_max 1.0000 _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 '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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4618 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1334 _reflns_number_gt 1287 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.4643P] 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 1334 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.76135(2) 0.15528(2) 0.03236(2) 0.01122(11) Uani 1 1 d . . . K1 K 1.28592(11) 0.18486(13) 0.30768(12) 0.0248(2) Uani 1 1 d . . . S1 S 0.98632(12) 0.18683(13) -0.10996(13) 0.0152(2) Uani 1 1 d . . . S2 S 0.54979(11) 0.13220(12) 0.17756(12) 0.0117(2) Uani 1 1 d . . . O1 O 1.0371(5) 0.2510(4) 0.0357(4) 0.0467(11) Uani 1 1 d . . . O2 O 0.8419(4) 0.1046(5) -0.1511(4) 0.0344(9) Uani 1 1 d . . . O3 O 0.9585(4) 0.3140(4) -0.2179(4) 0.0205(7) Uani 1 1 d . . . O4 O 1.0961(3) 0.0792(4) -0.1167(4) 0.0220(7) Uani 1 1 d . . . O5 O 0.5543(3) 0.2463(4) 0.0716(3) 0.0205(7) Uani 1 1 d . . . O6 O 0.6737(3) 0.0192(4) 0.2108(4) 0.0213(7) Uani 1 1 d . . . O7 O 0.4015(3) 0.0536(4) 0.1127(4) 0.0222(7) Uani 1 1 d . . . O8 O 0.5716(3) 0.2123(4) 0.3114(3) 0.0182(6) Uani 1 1 d . . . O9W O 0.8115(4) 0.4481(4) 0.0393(4) 0.0281(8) Uani 1 1 d . . . H1A H 0.8687 0.4836 0.0068 0.034 Uiso 1 1 d R . . H1B H 0.7712 0.5112 0.0742 0.034 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 Sm1 0.01196(15) 0.00910(15) 0.00808(17) -0.00029(7) 0.00126(11) 0.00091(7) K1 0.0224(5) 0.0283(5) 0.0210(6) -0.0014(4) 0.0083(4) -0.0035(4) S1 0.0202(5) 0.0153(5) 0.0106(6) 0.0046(4) 0.0077(4) 0.0082(4) S2 0.0118(5) 0.0137(5) 0.0082(6) -0.0033(4) 0.0037(4) -0.0030(4) O1 0.087(3) 0.032(2) 0.0109(19) 0.0004(16) 0.016(2) 0.025(2) O2 0.0276(19) 0.042(2) 0.043(2) 0.0105(18) 0.0241(18) 0.0009(16) O3 0.0249(16) 0.0180(15) 0.0143(17) 0.0059(13) 0.0059(14) 0.0043(13) O4 0.0238(16) 0.0178(16) 0.0253(19) 0.0031(13) 0.0126(14) 0.0100(13) O5 0.0249(16) 0.0229(16) 0.0158(17) 0.0046(13) 0.0115(14) 0.0014(13) O6 0.0186(15) 0.0189(16) 0.0250(18) -0.0012(14) 0.0095(14) 0.0037(12) O7 0.0166(15) 0.0245(16) 0.0226(18) -0.0108(14) 0.0071(13) -0.0086(12) O8 0.0191(15) 0.0232(16) 0.0104(16) -0.0066(13) 0.0057(13) -0.0055(13) O9W 0.0308(18) 0.0199(17) 0.037(2) -0.0045(15) 0.0194(16) -0.0071(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O4 2.357(3) 3_755 ? Sm1 O7 2.386(3) 3_655 ? Sm1 O3 2.397(3) 4_566 ? Sm1 O8 2.435(3) 4_565 ? Sm1 O5 2.435(3) . ? Sm1 O2 2.442(4) . ? Sm1 O9W 2.524(3) . ? Sm1 O6 2.667(3) . ? Sm1 O1 2.876(5) . ? K1 O1 2.777(4) . ? K1 O5 2.825(3) 4_666 ? K1 O8 2.868(3) 1_655 ? K1 O2 2.877(4) 3_755 ? K1 O6 2.879(3) 2_755 ? K1 O7 2.994(3) 1_655 ? K1 O9W 3.002(4) 2_745 ? K1 O4 3.117(3) 4_566 ? K1 O3 3.177(3) 4_566 ? S1 O1 1.447(4) . ? S1 O4 1.460(3) . ? S1 O2 1.477(4) . ? S1 O3 1.479(3) . ? S2 O8 1.463(3) . ? S2 O7 1.467(3) . ? S2 O6 1.475(3) . ? S2 O5 1.481(3) . ? O2 K1 2.877(4) 3_755 ? O3 Sm1 2.397(3) 4_565 ? O3 K1 3.177(3) 4_565 ? O4 Sm1 2.357(3) 3_755 ? O4 K1 3.117(3) 4_565 ? O5 K1 2.825(3) 4_465 ? O6 K1 2.879(3) 2_745 ? O7 Sm1 2.386(3) 3_655 ? O7 K1 2.994(3) 1_455 ? O8 Sm1 2.435(3) 4_566 ? O8 K1 2.868(3) 1_455 ? O9W K1 3.002(4) 2_755 ? O9W H1A 0.8500 . ? O9W H1B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sm1 O7 73.68(12) 3_755 3_655 ? O4 Sm1 O3 69.69(11) 3_755 4_566 ? O7 Sm1 O3 135.98(11) 3_655 4_566 ? O4 Sm1 O8 142.87(11) 3_755 4_565 ? O7 Sm1 O8 76.16(11) 3_655 4_565 ? O3 Sm1 O8 146.14(10) 4_566 4_565 ? O4 Sm1 O5 128.46(10) 3_755 . ? O7 Sm1 O5 87.55(10) 3_655 . ? O3 Sm1 O5 96.49(11) 4_566 . ? O8 Sm1 O5 70.52(10) 4_565 . ? O4 Sm1 O2 76.63(12) 3_755 . ? O7 Sm1 O2 76.36(12) 3_655 . ? O3 Sm1 O2 116.64(12) 4_566 . ? O8 Sm1 O2 75.63(11) 4_565 . ? O5 Sm1 O2 145.13(11) . . ? O4 Sm1 O9W 137.68(11) 3_755 . ? O7 Sm1 O9W 144.38(11) 3_655 . ? O3 Sm1 O9W 79.23(11) 4_566 . ? O8 Sm1 O9W 68.24(11) 4_565 . ? O5 Sm1 O9W 81.95(11) . . ? O2 Sm1 O9W 93.30(12) . . ? O4 Sm1 O6 74.04(10) 3_755 . ? O7 Sm1 O6 76.13(10) 3_655 . ? O3 Sm1 O6 71.05(10) 4_566 . ? O8 Sm1 O6 118.72(9) 4_565 . ? O5 Sm1 O6 54.78(9) . . ? O2 Sm1 O6 144.24(11) . . ? O9W Sm1 O6 122.24(10) . . ? O4 Sm1 O1 79.73(10) 3_755 . ? O7 Sm1 O1 125.53(10) 3_655 . ? O3 Sm1 O1 70.55(11) 4_566 . ? O8 Sm1 O1 101.21(10) 4_565 . ? O5 Sm1 O1 143.95(11) . . ? O2 Sm1 O1 51.38(11) . . ? O9W Sm1 O1 62.90(10) . . ? O6 Sm1 O1 139.02(10) . . ? O4 Sm1 S2 101.62(8) 3_755 . ? O7 Sm1 S2 80.71(8) 3_655 . ? O3 Sm1 S2 83.54(8) 4_566 . ? O8 Sm1 S2 94.30(7) 4_565 . ? O5 Sm1 S2 27.01(7) . . ? O2 Sm1 S2 156.55(9) . . ? O9W Sm1 S2 102.66(8) . . ? O6 Sm1 S2 27.77(6) . . ? O1 Sm1 S2 151.96(7) . . ? O4 Sm1 S1 78.76(8) 3_755 . ? O7 Sm1 S1 101.02(8) 3_655 . ? O3 Sm1 S1 95.03(8) 4_566 . ? O8 Sm1 S1 86.33(7) 4_565 . ? O5 Sm1 S1 152.74(7) . . ? O2 Sm1 S1 25.18(9) . . ? O9W Sm1 S1 76.06(8) . . ? O6 Sm1 S1 152.35(7) . . ? O1 Sm1 S1 26.34(7) . . ? S2 Sm1 S1 178.26(3) . . ? O4 Sm1 K1 63.65(8) 3_755 3_755 ? O7 Sm1 K1 40.02(8) 3_655 3_755 ? O3 Sm1 K1 130.54(8) 4_566 3_755 ? O8 Sm1 K1 79.33(8) 4_565 3_755 ? O5 Sm1 K1 124.91(8) . 3_755 ? O2 Sm1 K1 37.55(9) . 3_755 ? O9W Sm1 K1 127.48(8) . 3_755 ? O6 Sm1 K1 109.28(7) . 3_755 ? O1 Sm1 K1 85.59(7) . 3_755 ? S2 Sm1 K1 120.44(2) . 3_755 ? S1 Sm1 K1 61.27(3) . 3_755 ? O1 K1 O5 155.93(11) . 4_666 ? O1 K1 O8 113.77(12) . 1_655 ? O5 K1 O8 59.17(9) 4_666 1_655 ? O1 K1 O2 70.16(11) . 3_755 ? O5 K1 O2 132.84(11) 4_666 3_755 ? O8 K1 O2 104.38(9) 1_655 3_755 ? O1 K1 O6 79.70(11) . 2_755 ? O5 K1 O6 76.23(9) 4_666 2_755 ? O8 K1 O6 75.44(9) 1_655 2_755 ? O2 K1 O6 147.02(10) 3_755 2_755 ? O1 K1 O7 80.94(11) . 1_655 ? O5 K1 O7 103.26(9) 4_666 1_655 ? O8 K1 O7 47.43(8) 1_655 1_655 ? O2 K1 O7 61.07(9) 3_755 1_655 ? O6 K1 O7 101.92(9) 2_755 1_655 ? O1 K1 O9W 107.89(12) . 2_745 ? O5 K1 O9W 91.67(10) 4_666 2_745 ? O8 K1 O9W 129.01(10) 1_655 2_745 ? O2 K1 O9W 63.80(10) 3_755 2_745 ? O6 K1 O9W 141.67(10) 2_755 2_745 ? O7 K1 O9W 116.30(10) 1_655 2_745 ? O1 K1 O4 76.42(10) . 4_566 ? O5 K1 O4 92.25(9) 4_666 4_566 ? O8 K1 O4 132.72(9) 1_655 4_566 ? O2 K1 O4 121.78(9) 3_755 4_566 ? O6 K1 O4 60.66(9) 2_755 4_566 ? O7 K1 O4 153.45(10) 1_655 4_566 ? O9W K1 O4 84.12(9) 2_745 4_566 ? O1 K1 O3 61.65(11) . 4_566 ? O5 K1 O3 123.20(9) 4_666 4_566 ? O8 K1 O3 174.05(10) 1_655 4_566 ? O2 K1 O3 78.03(9) 3_755 4_566 ? O6 K1 O3 99.53(9) 2_755 4_566 ? O7 K1 O3 132.21(9) 1_655 4_566 ? O9W K1 O3 56.94(9) 2_745 4_566 ? O4 K1 O3 44.02(8) 4_566 4_566 ? O1 K1 S2 96.44(10) . 1_655 ? O5 K1 S2 81.57(7) 4_666 1_655 ? O8 K1 S2 23.49(6) 1_655 1_655 ? O2 K1 S2 83.73(7) 3_755 1_655 ? O6 K1 S2 86.70(7) 2_755 1_655 ? O7 K1 S2 24.11(6) 1_655 1_655 ? O9W K1 S2 127.94(7) 2_745 1_655 ? O4 K1 S2 147.26(7) 4_566 1_655 ? O3 K1 S2 155.21(7) 4_566 1_655 ? O1 K1 S1 74.83(9) . 4_566 ? O5 K1 S1 102.79(7) 4_666 4_566 ? O8 K1 S1 154.69(7) 1_655 4_566 ? O2 K1 S1 100.94(7) 3_755 4_566 ? O6 K1 S1 83.27(7) 2_755 4_566 ? O7 K1 S1 153.92(7) 1_655 4_566 ? O9W K1 S1 63.85(7) 2_745 4_566 ? O4 K1 S1 22.98(5) 4_566 4_566 ? O3 K1 S1 23.52(6) 4_566 4_566 ? S2 K1 S1 167.73(4) 1_655 4_566 ? O1 K1 S2 142.53(8) . 4_666 ? O5 K1 S2 19.87(6) 4_666 4_666 ? O8 K1 S2 75.28(7) 1_655 4_666 ? O2 K1 S2 145.49(8) 3_755 4_666 ? O6 K1 S2 67.21(7) 2_755 4_666 ? O7 K1 S2 121.71(7) 1_655 4_666 ? O9W K1 S2 89.17(7) 2_745 4_666 ? O4 K1 S2 72.39(6) 4_566 4_666 ? O3 K1 S2 105.92(7) 4_566 4_666 ? S2 K1 S2 98.63(4) 1_655 4_666 ? S1 K1 S2 84.01(4) 4_566 4_666 ? O1 S1 O4 113.0(2) . . ? O1 S1 O2 106.3(3) . . ? O4 S1 O2 110.7(2) . . ? O1 S1 O3 111.1(2) . . ? O4 S1 O3 106.79(19) . . ? O2 S1 O3 109.0(2) . . ? O1 S1 Sm1 61.9(2) . . ? O4 S1 Sm1 132.74(14) . . ? O2 S1 Sm1 44.72(16) . . ? O3 S1 Sm1 118.94(13) . . ? O1 S1 K1 102.5(2) . 4_565 ? O4 S1 K1 56.49(13) . 4_565 ? O2 S1 K1 151.20(16) . 4_565 ? O3 S1 K1 59.01(13) . 4_565 ? Sm1 S1 K1 163.41(4) . 4_565 ? O8 S2 O7 107.33(18) . . ? O8 S2 O6 110.94(19) . . ? O7 S2 O6 111.79(19) . . ? O8 S2 O5 110.98(18) . . ? O7 S2 O5 110.17(19) . . ? O6 S2 O5 105.67(18) . . ? O8 S2 Sm1 126.76(12) . . ? O7 S2 Sm1 125.54(14) . . ? O6 S2 Sm1 57.39(13) . . ? O5 S2 Sm1 48.28(12) . . ? O8 S2 K1 51.39(12) . 1_455 ? O7 S2 K1 56.47(13) . 1_455 ? O6 S2 K1 134.30(14) . 1_455 ? O5 S2 K1 119.93(13) . 1_455 ? Sm1 S2 K1 168.07(4) . 1_455 ? O8 S2 K1 118.84(13) . 4_465 ? O7 S2 K1 70.18(14) . 4_465 ? O6 S2 K1 127.00(14) . 4_465 ? O5 S2 K1 40.40(12) . 4_465 ? Sm1 S2 K1 78.18(3) . 4_465 ? K1 S2 K1 92.70(4) 1_455 4_465 ? S1 O1 K1 132.5(2) . . ? S1 O1 Sm1 91.8(2) . . ? K1 O1 Sm1 110.26(14) . . ? S1 O2 Sm1 110.1(2) . . ? S1 O2 K1 132.4(2) . 3_755 ? Sm1 O2 K1 111.30(12) . 3_755 ? S1 O3 Sm1 130.68(19) . 4_565 ? S1 O3 K1 97.47(14) . 4_565 ? Sm1 O3 K1 111.89(12) 4_565 4_565 ? S1 O4 Sm1 147.9(2) . 3_755 ? S1 O4 K1 100.53(15) . 4_565 ? Sm1 O4 K1 107.20(11) 3_755 4_565 ? S2 O5 Sm1 104.71(16) . . ? S2 O5 K1 119.73(17) . 4_465 ? Sm1 O5 K1 113.47(11) . 4_465 ? S2 O6 Sm1 94.83(15) . . ? S2 O6 K1 138.84(17) . 2_745 ? Sm1 O6 K1 105.90(10) . 2_745 ? S2 O7 Sm1 149.5(2) . 3_655 ? S2 O7 K1 99.42(15) . 1_455 ? Sm1 O7 K1 109.15(11) 3_655 1_455 ? S2 O8 Sm1 142.81(18) . 4_566 ? S2 O8 K1 105.12(15) . 1_455 ? Sm1 O8 K1 112.00(11) 4_566 1_455 ? Sm1 O9W K1 123.98(13) . 2_755 ? Sm1 O9W H1A 120.0 . . ? K1 O9W H1A 115.5 2_755 . ? Sm1 O9W H1B 120.0 . . ? K1 O9W H1B 8.1 2_755 . ? H1A O9W H1B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.045 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.156 #==END data_2 _database_code_depnum_ccdc_archive 'CCDC 860629' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 H2 Eu K O9 S2' _chemical_formula_weight 401.20 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M p2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.084(10) _cell_length_b 8.429(8) _cell_length_c 10.363(15) _cell_angle_alpha 90.00 _cell_angle_beta 119.023(16) _cell_angle_gamma 90.00 _cell_volume 770.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2414 _cell_measurement_theta_min 3.3416 _cell_measurement_theta_max 27.4758 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 9.248 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1924 _exptl_absorpt_correction_T_max 1.0000 _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 '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 5759 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1698 _reflns_number_gt 1482 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1698 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.74044(3) 0.15154(3) 0.46587(3) 0.01215(16) Uani 1 1 d . . . K1 K 0.78742(18) -0.18131(18) 0.80963(19) 0.0258(4) Uani 1 1 d . . . S1 S 0.94963(18) 0.13325(16) 0.32094(18) 0.0121(3) Uani 1 1 d . . . S2 S 0.49217(19) -0.19144(18) 0.39349(19) 0.0165(4) Uani 1 1 d . . . O1 O 1.0985(5) 0.0572(5) 0.3869(5) 0.0219(10) Uani 1 1 d . . . O2 O 0.9261(5) 0.2133(5) 0.1852(5) 0.0202(10) Uani 1 1 d . . . O3 O 0.9448(5) 0.2492(5) 0.4263(5) 0.0216(10) Uani 1 1 d . . . O4 O 0.8276(5) 0.0181(5) 0.2894(5) 0.0223(10) Uani 1 1 d . . . O5 O 0.5575(8) -0.2603(7) 0.5386(6) 0.064(2) Uani 1 1 d . . . O6 O 0.3514(6) -0.1090(6) 0.3636(7) 0.0398(15) Uani 1 1 d . . . O7 O 0.5970(5) -0.0818(5) 0.3802(5) 0.0216(10) Uani 1 1 d . . . O8 O 0.4555(5) -0.3156(5) 0.2809(5) 0.0186(10) Uani 1 1 d . . . O9W O 0.6819(6) 0.4391(5) 0.4544(5) 0.0284(12) Uani 1 1 d . . . H9WA H 0.6689 0.4818 0.5218 0.034 Uiso 1 1 d R . . H9WB H 0.6749 0.4948 0.3830 0.034 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0132(2) 0.00455(19) 0.0154(3) 0.00052(10) 0.00442(18) -0.00109(10) K1 0.0232(9) 0.0253(7) 0.0279(10) 0.0015(6) 0.0116(8) 0.0036(6) S1 0.0121(8) 0.0095(6) 0.0144(9) 0.0035(5) 0.0062(7) 0.0030(5) S2 0.0225(9) 0.0124(7) 0.0170(9) -0.0053(6) 0.0116(8) -0.0102(6) O1 0.018(2) 0.020(2) 0.028(3) 0.010(2) 0.011(2) 0.0067(18) O2 0.024(3) 0.019(2) 0.016(3) 0.0087(19) 0.008(2) 0.0065(19) O3 0.026(3) 0.018(2) 0.024(3) -0.0047(19) 0.015(2) 0.0002(19) O4 0.019(2) 0.014(2) 0.035(3) 0.002(2) 0.015(2) -0.0023(18) O5 0.118(6) 0.038(3) 0.012(3) 0.000(3) 0.012(4) -0.043(4) O6 0.032(3) 0.037(3) 0.068(5) -0.020(3) 0.038(3) -0.007(3) O7 0.023(3) 0.014(2) 0.031(3) -0.0045(19) 0.015(2) -0.0101(18) O8 0.017(2) 0.013(2) 0.022(3) -0.0078(18) 0.006(2) -0.0036(17) O9W 0.040(3) 0.013(2) 0.036(3) 0.003(2) 0.022(3) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O7 2.346(4) . ? Eu1 O8 2.370(5) 2_655 ? Eu1 O1 2.378(4) 3_756 ? Eu1 O6 2.387(6) 3_656 ? Eu1 O2 2.417(5) 4_566 ? Eu1 O3 2.432(5) . ? Eu1 O9W 2.484(5) . ? Eu1 O4 2.635(5) . ? Eu1 O5 3.120(9) 3_656 ? K1 O5 2.718(6) . ? K1 O3 2.820(5) 2_746 ? K1 O2 2.876(6) 3_756 ? K1 O4 2.890(5) 4_556 ? K1 O6 2.955(6) 3_656 ? K1 O1 2.973(5) 3_756 ? K1 O9W 3.017(5) 4_566 ? K1 O7 3.094(5) 4_556 ? K1 O8 3.214(6) 4_556 ? S1 O1 1.461(5) . ? S1 O4 1.474(4) . ? S1 O2 1.471(5) . ? S1 O3 1.483(5) . ? S2 O5 1.439(6) . ? S2 O7 1.460(4) . ? S2 O6 1.472(5) . ? S2 O8 1.475(5) . ? O1 Eu1 2.378(4) 3_756 ? O1 K1 2.973(5) 3_756 ? O2 Eu1 2.417(5) 4_565 ? O2 K1 2.876(6) 3_756 ? O3 K1 2.820(5) 2_756 ? O4 K1 2.890(5) 4 ? O5 Eu1 3.120(9) 3_656 ? O6 Eu1 2.387(6) 3_656 ? O6 K1 2.955(6) 3_656 ? O7 K1 3.094(5) 4 ? O8 Eu1 2.370(5) 2_645 ? O8 K1 3.214(6) 4 ? O9W K1 3.017(5) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Eu1 O8 69.58(16) . 2_655 ? O7 Eu1 O1 74.14(18) . 3_756 ? O8 Eu1 O1 136.97(15) 2_655 3_756 ? O7 Eu1 O6 76.39(17) . 3_656 ? O8 Eu1 O6 113.4(2) 2_655 3_656 ? O1 Eu1 O6 78.66(18) 3_756 3_656 ? O7 Eu1 O2 143.65(16) . 4_566 ? O8 Eu1 O2 145.05(15) 2_655 4_566 ? O1 Eu1 O2 76.64(17) 3_756 4_566 ? O6 Eu1 O2 77.1(2) 3_656 4_566 ? O7 Eu1 O3 129.60(15) . . ? O8 Eu1 O3 96.29(18) 2_655 . ? O1 Eu1 O3 89.29(17) 3_756 . ? O6 Eu1 O3 147.22(17) 3_656 . ? O2 Eu1 O3 70.48(17) 4_566 . ? O7 Eu1 O9W 135.35(16) . . ? O8 Eu1 O9W 77.31(16) 2_655 . ? O1 Eu1 O9W 145.57(17) 3_756 . ? O6 Eu1 O9W 90.76(17) 3_656 . ? O2 Eu1 O9W 69.05(16) 4_566 . ? O3 Eu1 O9W 82.13(16) . . ? O7 Eu1 O4 74.42(15) . . ? O8 Eu1 O4 71.64(18) 2_655 . ? O1 Eu1 O4 77.04(17) 3_756 . ? O6 Eu1 O4 146.07(16) 3_656 . ? O2 Eu1 O4 119.15(17) 4_566 . ? O3 Eu1 O4 55.39(14) . . ? O9W Eu1 O4 122.35(14) . . ? O7 Eu1 O5 80.10(16) . 3_656 ? O8 Eu1 O5 69.95(16) 2_655 3_656 ? O1 Eu1 O5 125.44(15) 3_756 3_656 ? O6 Eu1 O5 48.57(17) 3_656 3_656 ? O2 Eu1 O5 100.15(16) 4_566 3_656 ? O3 Eu1 O5 141.90(16) . 3_656 ? O9W Eu1 O5 60.51(15) . 3_656 ? O4 Eu1 O5 139.31(14) . 3_656 ? O7 Eu1 S1 102.26(12) . . ? O8 Eu1 S1 83.75(16) 2_655 . ? O1 Eu1 S1 82.07(13) 3_756 . ? O6 Eu1 S1 160.30(14) 3_656 . ? O2 Eu1 S1 94.57(15) 4_566 . ? O3 Eu1 S1 27.42(11) . . ? O9W Eu1 S1 103.00(12) . . ? O4 Eu1 S1 27.97(10) . . ? O5 Eu1 S1 151.09(10) 3_656 . ? O7 Eu1 S2 79.29(12) . 3_656 ? O8 Eu1 S2 93.73(16) 2_655 3_656 ? O1 Eu1 S2 101.59(13) 3_756 3_656 ? O6 Eu1 S2 23.23(14) 3_656 3_656 ? O2 Eu1 S2 85.95(15) 4_566 3_656 ? O3 Eu1 S2 151.11(11) . 3_656 ? O9W Eu1 S2 73.76(12) . 3_656 ? O4 Eu1 S2 153.03(10) . 3_656 ? O5 Eu1 S2 25.54(11) 3_656 3_656 ? S1 Eu1 S2 176.31(4) . 3_656 ? O7 Eu1 K1 64.79(13) . . ? O8 Eu1 K1 131.12(12) 2_655 . ? O1 Eu1 K1 39.91(11) 3_756 . ? O6 Eu1 K1 39.53(14) 3_656 . ? O2 Eu1 K1 78.94(14) 4_566 . ? O3 Eu1 K1 126.04(12) . . ? O9W Eu1 K1 126.43(12) . . ? O4 Eu1 K1 110.52(13) . . ? O5 Eu1 K1 85.62(11) 3_656 . ? S1 Eu1 K1 121.80(6) . . ? S2 Eu1 K1 61.89(6) 3_656 . ? O5 K1 O3 152.48(18) . 2_746 ? O5 K1 O2 110.0(2) . 3_756 ? O3 K1 O2 58.82(15) 2_746 3_756 ? O5 K1 O4 76.33(18) . 4_556 ? O3 K1 O4 76.37(14) 2_746 4_556 ? O2 K1 O4 74.60(13) 3_756 4_556 ? O5 K1 O6 70.12(18) . 3_656 ? O3 K1 O6 135.23(16) 2_746 3_656 ? O2 K1 O6 105.33(14) 3_756 3_656 ? O4 K1 O6 144.22(15) 4_556 3_656 ? O5 K1 O1 78.3(2) . 3_756 ? O3 K1 O1 103.37(16) 2_746 3_756 ? O2 K1 O1 47.67(12) 3_756 3_756 ? O4 K1 O1 100.47(13) 4_556 3_756 ? O6 K1 O1 61.26(14) 3_656 3_756 ? O5 K1 O9W 110.5(2) . 4_566 ? O3 K1 O9W 93.48(17) 2_746 4_566 ? O2 K1 O9W 130.36(14) 3_756 4_566 ? O4 K1 O9W 142.82(14) 4_556 4_566 ? O6 K1 O9W 64.17(16) 3_656 4_566 ? O1 K1 O9W 116.71(15) 3_756 4_566 ? O5 K1 O7 76.70(18) . 4_556 ? O3 K1 O7 92.78(15) 2_746 4_556 ? O2 K1 O7 131.93(13) 3_756 4_556 ? O4 K1 O7 60.52(13) 4_556 4_556 ? O6 K1 O7 120.84(15) 3_656 4_556 ? O1 K1 O7 151.62(14) 3_756 4_556 ? O9W K1 O7 84.85(14) 4_566 4_556 ? O5 K1 O8 64.8(2) . 4_556 ? O3 K1 O8 123.50(15) 2_746 4_556 ? O2 K1 O8 173.09(14) 3_756 4_556 ? O4 K1 O8 99.31(12) 4_556 4_556 ? O6 K1 O8 77.60(13) 3_656 4_556 ? O1 K1 O8 132.17(13) 3_756 4_556 ? O9W K1 O8 56.54(13) 4_566 4_556 ? O7 K1 O8 43.84(11) 4_556 4_556 ? O5 K1 S1 93.13(19) . 3_756 ? O3 K1 S1 81.52(14) 2_746 3_756 ? O2 K1 S1 23.79(9) 3_756 3_756 ? O4 K1 S1 85.83(10) 4_556 3_756 ? O6 K1 S1 83.97(12) 3_656 3_756 ? O1 K1 S1 24.00(9) 3_756 3_756 ? O9W K1 S1 128.58(11) 4_566 3_756 ? O7 K1 S1 146.18(10) 4_556 3_756 ? O8 K1 S1 154.98(11) 4_556 3_756 ? O5 K1 S2 77.78(18) . 4_556 ? O3 K1 S2 102.46(14) 2_746 4_556 ? O2 K1 S2 153.83(11) 3_756 4_556 ? O4 K1 S2 83.55(10) 4_556 4_556 ? O6 K1 S2 100.81(12) 3_656 4_556 ? O1 K1 S2 154.08(11) 3_756 4_556 ? O9W K1 S2 63.55(11) 4_566 4_556 ? O7 K1 S2 23.24(8) 4_556 4_556 ? O8 K1 S2 23.78(8) 4_556 4_556 ? S1 K1 S2 167.39(6) 3_756 4_556 ? O5 K1 S1 140.62(14) . 2_746 ? O3 K1 S1 19.96(9) 2_746 2_746 ? O2 K1 S1 74.79(12) 3_756 2_746 ? O4 K1 S1 67.23(11) 4_556 2_746 ? O6 K1 S1 148.29(12) 3_656 2_746 ? O1 K1 S1 121.66(13) 3_756 2_746 ? O9W K1 S1 91.12(14) 4_566 2_746 ? O7 K1 S1 72.82(12) 4_556 2_746 ? O8 K1 S1 106.13(11) 4_556 2_746 ? S1 K1 S1 98.46(11) 3_756 2_746 ? S2 K1 S1 83.66(10) 4_556 2_746 ? O1 S1 O4 111.9(3) . . ? O1 S1 O2 107.5(3) . . ? O4 S1 O2 111.1(3) . . ? O1 S1 O3 109.7(3) . . ? O4 S1 O3 106.0(3) . . ? O2 S1 O3 110.7(3) . . ? O1 S1 Eu1 125.1(2) . . ? O4 S1 Eu1 56.94(19) . . ? O2 S1 Eu1 127.0(2) . . ? O3 S1 Eu1 49.04(19) . . ? O1 S1 K1 55.84(19) . 3_756 ? O4 S1 K1 133.7(2) . 3_756 ? O2 S1 K1 52.05(19) . 3_756 ? O3 S1 K1 120.3(2) . 3_756 ? Eu1 S1 K1 169.29(6) . 3_756 ? O1 S1 K1 69.6(2) . 2_756 ? O4 S1 K1 126.7(2) . 2_756 ? O2 S1 K1 119.2(2) . 2_756 ? O3 S1 K1 40.47(19) . 2_756 ? Eu1 S1 K1 78.38(10) . 2_756 ? K1 S1 K1 93.00(11) 3_756 2_756 ? O5 S2 O7 111.6(3) . . ? O5 S2 O6 108.4(4) . . ? O7 S2 O6 110.5(3) . . ? O5 S2 O8 110.6(3) . . ? O7 S2 O8 106.9(3) . . ? O6 S2 O8 108.8(3) . . ? O5 S2 Eu1 69.2(3) . 3_656 ? O7 S2 Eu1 132.4(2) . 3_656 ? O6 S2 Eu1 39.7(2) . 3_656 ? O8 S2 Eu1 117.31(19) . 3_656 ? O5 S2 K1 96.7(3) . 4 ? O7 S2 K1 56.72(19) . 4 ? O6 S2 K1 154.8(3) . 4 ? O8 S2 K1 61.51(18) . 4 ? Eu1 S2 K1 165.01(6) 3_656 4 ? S1 O1 Eu1 148.4(3) . 3_756 ? S1 O1 K1 100.2(2) . 3_756 ? Eu1 O1 K1 109.21(17) 3_756 3_756 ? S1 O2 Eu1 143.8(3) . 4_565 ? S1 O2 K1 104.2(2) . 3_756 ? Eu1 O2 K1 111.99(17) 4_565 3_756 ? S1 O3 Eu1 103.5(2) . . ? S1 O3 K1 119.6(3) . 2_756 ? Eu1 O3 K1 113.4(2) . 2_756 ? S1 O4 Eu1 95.1(2) . . ? S1 O4 K1 139.6(2) . 4 ? Eu1 O4 K1 105.27(15) . 4 ? S2 O5 K1 135.2(3) . . ? S2 O5 Eu1 85.2(4) . 3_656 ? K1 O5 Eu1 106.0(2) . 3_656 ? S2 O6 Eu1 117.0(3) . 3_656 ? S2 O6 K1 130.0(3) . 3_656 ? Eu1 O6 K1 109.54(19) 3_656 3_656 ? S2 O7 Eu1 146.8(3) . . ? S2 O7 K1 100.0(2) . 4 ? Eu1 O7 K1 106.92(17) . 4 ? S2 O8 Eu1 134.0(3) . 2_645 ? S2 O8 K1 94.7(2) . 4 ? Eu1 O8 K1 112.61(18) 2_645 4 ? Eu1 O9W K1 123.45(18) . 4_565 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 3.049 _refine_diff_density_min -2.080 _refine_diff_density_rms 0.301 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 860630' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 H2 Gd K N0 O9 S2' _chemical_formula_weight 406.49 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' K K 0.2009 0.2494 '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 ? _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.129(5) _cell_length_b 8.391(3) _cell_length_c 10.357(7) _cell_angle_alpha 90.00 _cell_angle_beta 119.152(6) _cell_angle_gamma 90.00 _cell_volume 768.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2055 _cell_measurement_theta_min 3.311 _cell_measurement_theta_max 27.4719 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 9.734 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4036 _exptl_absorpt_correction_T_max 1.0000 _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 '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 4634 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1345 _reflns_number_gt 1289 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.5221P] 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 1345 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.25760(2) 0.14804(3) 0.03605(2) 0.00919(11) Uani 1 1 d . . . K1 K -0.21115(13) 0.32326(15) -0.18849(13) 0.0237(3) Uani 1 1 d . . . S1 S 0.50186(13) -0.19667(15) 0.10274(13) 0.0132(3) Uani 1 1 d . . . S2 S 0.05066(13) 0.13423(14) 0.18034(13) 0.0104(3) Uani 1 1 d . . . O1 O 0.4229(6) -0.2711(5) -0.0412(4) 0.0496(14) Uani 1 1 d . . . O2 O 0.6385(5) -0.1143(5) 0.1220(5) 0.0339(10) Uani 1 1 d . . . O3 O 0.5469(4) -0.3190(4) 0.2192(4) 0.0173(7) Uani 1 1 d . . . O4 O 0.4028(4) -0.0850(4) 0.1236(4) 0.0175(8) Uani 1 1 d . . . O5 O -0.0992(4) 0.0602(5) 0.1131(4) 0.0193(8) Uani 1 1 d . . . O6 O 0.0759(4) 0.2118(4) 0.3171(4) 0.0168(7) Uani 1 1 d . . . O7 O 0.0576(4) 0.2522(4) 0.0764(4) 0.0189(8) Uani 1 1 d . . . O8 O 0.1700(4) 0.0167(4) 0.2087(4) 0.0206(8) Uani 1 1 d . . . O9W O 0.3228(4) 0.4332(4) 0.0500(4) 0.0228(8) Uani 1 1 d . . . H1A H 0.2490 0.5070 0.0121 0.027 Uiso 1 1 d R . . H1B H 0.4203 0.4635 0.0930 0.027 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 Gd1 0.01021(16) 0.00747(17) 0.00914(16) -0.00041(8) 0.00412(11) 0.00097(8) K1 0.0213(6) 0.0295(7) 0.0216(6) 0.0000(5) 0.0113(5) 0.0021(5) S1 0.0179(6) 0.0138(6) 0.0115(6) 0.0047(5) 0.0099(5) 0.0079(5) S2 0.0100(5) 0.0130(6) 0.0106(6) -0.0024(4) 0.0068(5) -0.0024(4) O1 0.085(4) 0.034(3) 0.013(2) -0.0004(19) 0.011(2) 0.032(3) O2 0.032(2) 0.035(2) 0.053(3) 0.018(2) 0.036(2) 0.0098(19) O3 0.0199(17) 0.0149(18) 0.0139(17) 0.0041(14) 0.0059(14) 0.0012(15) O4 0.0191(17) 0.0137(19) 0.0231(19) 0.0015(15) 0.0129(15) 0.0077(15) O5 0.0136(16) 0.025(2) 0.0205(18) -0.0109(15) 0.0090(14) -0.0076(15) O6 0.0169(16) 0.021(2) 0.0150(17) -0.0071(15) 0.0100(14) -0.0062(15) O7 0.0198(16) 0.025(2) 0.0196(18) 0.0052(15) 0.0155(14) 0.0026(15) O8 0.0170(16) 0.018(2) 0.030(2) 0.0010(16) 0.0141(16) 0.0046(15) O9W 0.0218(18) 0.013(2) 0.034(2) 0.0003(16) 0.0135(16) -0.0040(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.347(3) . ? Gd1 O3 2.353(3) 2_655 ? Gd1 O2 2.355(4) 3_655 ? Gd1 O5 2.366(3) 3 ? Gd1 O6 2.418(3) 4_565 ? Gd1 O7 2.423(3) . ? Gd1 O9W 2.468(4) . ? Gd1 O8 2.597(4) . ? K1 O1 2.686(4) 2_554 ? K1 O7 2.831(4) . ? K1 O6 2.894(4) 4_565 ? K1 O8 2.905(4) 3 ? K1 O5 2.955(4) 4_565 ? K1 O9W 3.015(4) 3_565 ? K1 O2 3.037(5) 4_465 ? K1 O4 3.081(4) 3 ? K1 O3 3.258(4) 3 ? S1 O1 1.446(4) . ? S1 O4 1.463(3) . ? S1 O2 1.471(4) . ? S1 O3 1.476(4) . ? S2 O6 1.464(3) . ? S2 O5 1.465(3) . ? S2 O8 1.474(4) . ? S2 O7 1.489(4) . ? O1 K1 2.686(4) 2_544 ? O2 Gd1 2.355(4) 3_655 ? O2 K1 3.037(5) 4_666 ? O3 Gd1 2.353(3) 2_645 ? O3 K1 3.258(4) 3 ? O4 K1 3.081(4) 3 ? O5 Gd1 2.366(3) 3 ? O5 K1 2.955(4) 4_566 ? O6 Gd1 2.418(3) 4_566 ? O6 K1 2.894(4) 4_566 ? O8 K1 2.905(4) 3 ? O9W K1 3.015(4) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd1 O3 69.00(12) . 2_655 ? O4 Gd1 O2 76.12(13) . 3_655 ? O3 Gd1 O2 109.66(15) 2_655 3_655 ? O4 Gd1 O5 74.63(13) . 3 ? O3 Gd1 O5 137.53(13) 2_655 3 ? O2 Gd1 O5 81.24(14) 3_655 3 ? O4 Gd1 O6 144.59(12) . 4_565 ? O3 Gd1 O6 144.09(12) 2_655 4_565 ? O2 Gd1 O6 78.50(13) 3_655 4_565 ? O5 Gd1 O6 77.45(13) 3 4_565 ? O4 Gd1 O7 130.80(12) . . ? O3 Gd1 O7 96.16(12) 2_655 . ? O2 Gd1 O7 149.07(13) 3_655 . ? O5 Gd1 O7 91.22(12) 3 . ? O6 Gd1 O7 70.59(11) 4_565 . ? O4 Gd1 O9W 133.29(12) . . ? O3 Gd1 O9W 76.23(12) 2_655 . ? O2 Gd1 O9W 87.71(14) 3_655 . ? O5 Gd1 O9W 146.23(12) 3 . ? O6 Gd1 O9W 69.08(12) 4_565 . ? O7 Gd1 O9W 82.07(12) . . ? O4 Gd1 O8 74.97(11) . . ? O3 Gd1 O8 72.46(12) 2_655 . ? O2 Gd1 O8 147.76(13) 3_655 . ? O5 Gd1 O8 77.64(12) 3 . ? O6 Gd1 O8 119.52(11) 4_565 . ? O7 Gd1 O8 55.90(11) . . ? O9W Gd1 O8 122.84(12) . . ? O4 Gd1 S2 103.03(9) . . ? O3 Gd1 S2 84.11(10) 2_655 . ? O2 Gd1 S2 164.28(12) 3_655 . ? O5 Gd1 S2 83.41(9) 3 . ? O6 Gd1 S2 94.89(9) 4_565 . ? O7 Gd1 S2 27.80(8) . . ? O9W Gd1 S2 103.37(9) . . ? O8 Gd1 S2 28.11(8) . . ? O4 Gd1 K1 65.97(9) . 2_544 ? O3 Gd1 K1 131.28(9) 2_655 2_544 ? O2 Gd1 K1 41.84(11) 3_655 2_544 ? O5 Gd1 K1 39.83(8) 3 2_544 ? O6 Gd1 K1 78.64(9) 4_565 2_544 ? O7 Gd1 K1 127.30(9) . 2_544 ? O9W Gd1 K1 125.00(9) . 2_544 ? O8 Gd1 K1 111.60(9) . 2_544 ? S2 Gd1 K1 123.14(3) . 2_544 ? O4 Gd1 K1 42.59(9) . 3 ? O3 Gd1 K1 84.23(9) 2_655 3 ? O2 Gd1 K1 107.80(11) 3_655 3 ? O5 Gd1 K1 53.79(10) 3 3 ? O6 Gd1 K1 127.78(9) 4_565 3 ? O7 Gd1 K1 91.03(9) . 3 ? O9W Gd1 K1 158.37(9) . 3 ? O8 Gd1 K1 39.99(8) . 3 ? S2 Gd1 K1 64.95(3) . 3 ? K1 Gd1 K1 75.21(4) 2_544 3 ? O4 Gd1 K1 142.61(9) . . ? O3 Gd1 K1 130.96(9) 2_655 . ? O2 Gd1 K1 113.92(11) 3_655 . ? O5 Gd1 K1 71.82(9) 3 . ? O6 Gd1 K1 37.74(8) 4_565 . ? O7 Gd1 K1 36.17(9) . . ? O9W Gd1 K1 84.02(9) . . ? O8 Gd1 K1 82.13(8) . . ? S2 Gd1 K1 57.36(4) . . ? K1 Gd1 K1 96.78(3) 2_544 . ? K1 Gd1 K1 102.42(3) 3 . ? O1 K1 O7 148.28(14) 2_554 . ? O1 K1 O6 105.99(15) 2_554 4_565 ? O7 K1 O6 58.47(10) . 4_565 ? O1 K1 O8 72.86(13) 2_554 3 ? O7 K1 O8 76.07(11) . 3 ? O6 K1 O8 73.97(10) 4_565 3 ? O1 K1 O5 75.82(13) 2_554 4_565 ? O7 K1 O5 103.30(11) . 4_565 ? O6 K1 O5 47.61(9) 4_565 4_565 ? O8 K1 O5 99.08(11) 3 4_565 ? O1 K1 O9W 113.67(15) 2_554 3_565 ? O7 K1 O9W 95.04(11) . 3_565 ? O6 K1 O9W 131.68(11) 4_565 3_565 ? O8 K1 O9W 143.13(11) 3 3_565 ? O5 K1 O9W 117.79(11) 4_565 3_565 ? O1 K1 O2 70.68(13) 2_554 4_465 ? O7 K1 O2 137.58(12) . 4_465 ? O6 K1 O2 106.10(11) 4_565 4_465 ? O8 K1 O2 141.95(11) 3 4_465 ? O5 K1 O2 61.71(10) 4_565 4_465 ? O9W K1 O2 64.92(11) 3_565 4_465 ? O1 K1 O4 76.58(12) 2_554 3 ? O7 K1 O4 93.58(10) . 3 ? O6 K1 O4 131.55(10) 4_565 3 ? O8 K1 O4 60.41(10) 3 3 ? O5 K1 O4 149.60(11) 4_565 3 ? O9W K1 O4 85.06(10) 3_565 3 ? O2 K1 O4 119.47(10) 4_465 3 ? O1 K1 O3 68.25(14) 2_554 3 ? O7 K1 O3 123.86(10) . 3 ? O6 K1 O3 172.47(11) 4_565 3 ? O8 K1 O3 99.30(10) 3 3 ? O5 K1 O3 132.20(9) 4_565 3 ? O9W K1 O3 55.84(10) 3_565 3 ? O2 K1 O3 76.99(10) 4_465 3 ? O4 K1 O3 43.55(9) 3 3 ? O1 K1 S2 89.83(12) 2_554 4_565 ? O7 K1 S2 81.18(9) . 4_565 ? O6 K1 S2 23.72(7) 4_565 4_565 ? O8 K1 S2 84.88(8) 3 4_565 ? O5 K1 S2 23.99(6) 4_565 4_565 ? O9W K1 S2 129.73(8) 3_565 4_565 ? O2 K1 S2 84.52(8) 4_465 4_565 ? O4 K1 S2 145.01(8) 3 4_565 ? O3 K1 S2 154.93(7) 3 4_565 ? O1 K1 S1 80.64(12) 2_554 3 ? O7 K1 S1 102.31(9) . 3 ? O6 K1 S1 153.29(8) 4_565 3 ? O8 K1 S1 83.80(8) 3 3 ? O5 K1 S1 154.16(8) 4_565 3 ? O9W K1 S1 62.90(8) 3_565 3 ? O2 K1 S1 100.51(8) 4_465 3 ? O4 K1 S1 23.46(6) 3 3 ? O3 K1 S1 24.02(6) 3 3 ? S2 K1 S1 166.94(5) 4_565 3 ? O1 K1 S2 137.81(11) 2_554 . ? O7 K1 S2 20.25(7) . . ? O6 K1 S2 74.54(8) 4_565 . ? O8 K1 S2 66.79(8) 3 . ? O5 K1 S2 121.59(8) 4_565 . ? O9W K1 S2 92.57(9) 3_565 . ? O2 K1 S2 151.06(9) 4_465 . ? O4 K1 S2 73.35(7) 3 . ? O3 K1 S2 106.21(7) 3 . ? S2 K1 S2 98.18(6) 4_565 . ? S1 K1 S2 83.29(5) 3 . ? O1 S1 O4 110.7(2) . . ? O1 S1 O2 110.7(3) . . ? O4 S1 O2 110.3(2) . . ? O1 S1 O3 109.7(3) . . ? O4 S1 O3 106.6(2) . . ? O2 S1 O3 108.7(2) . . ? O1 S1 K1 91.1(2) . 3 ? O4 S1 K1 56.95(15) . 3 ? O2 S1 K1 158.0(2) . 3 ? O3 S1 K1 63.93(14) . 3 ? O6 S2 O5 107.5(2) . . ? O6 S2 O8 111.4(2) . . ? O5 S2 O8 111.8(2) . . ? O6 S2 O7 110.9(2) . . ? O5 S2 O7 110.0(2) . . ? O8 S2 O7 105.4(2) . . ? O6 S2 Gd1 127.38(14) . . ? O5 S2 Gd1 124.89(15) . . ? O8 S2 Gd1 56.09(14) . . ? O7 S2 Gd1 49.35(13) . . ? O6 S2 K1 52.67(13) . 4_566 ? O5 S2 K1 55.10(14) . 4_566 ? O8 S2 K1 133.33(15) . 4_566 ? O7 S2 K1 121.23(14) . 4_566 ? Gd1 S2 K1 170.58(5) . 4_566 ? O6 S2 K1 119.84(16) . . ? O5 S2 K1 69.08(16) . . ? O8 S2 K1 125.86(15) . . ? O7 S2 K1 41.14(13) . . ? Gd1 S2 K1 78.70(5) . . ? K1 S2 K1 93.31(6) 4_566 . ? S1 O1 K1 135.0(2) . 2_544 ? S1 O2 Gd1 124.0(3) . 3_655 ? S1 O2 K1 127.4(2) . 4_666 ? Gd1 O2 K1 107.01(14) 3_655 4_666 ? S1 O3 Gd1 136.5(2) . 2_645 ? S1 O3 K1 92.05(15) . 3 ? Gd1 O3 K1 113.24(13) 2_645 3 ? S1 O4 Gd1 145.3(2) . . ? S1 O4 K1 99.59(17) . 3 ? Gd1 O4 K1 106.37(12) . 3 ? S2 O5 Gd1 147.1(2) . 3 ? S2 O5 K1 100.91(17) . 4_566 ? Gd1 O5 K1 109.31(12) 3 4_566 ? S2 O6 Gd1 144.87(19) . 4_566 ? S2 O6 K1 103.61(16) . 4_566 ? Gd1 O6 K1 111.52(12) 4_566 4_566 ? S2 O7 Gd1 102.85(18) . . ? S2 O7 K1 118.61(18) . . ? Gd1 O7 K1 113.50(13) . . ? S2 O8 Gd1 95.80(17) . . ? S2 O8 K1 140.8(2) . 3 ? Gd1 O8 K1 104.95(12) . 3 ? Gd1 O9W K1 122.25(13) . 3_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.807 _refine_diff_density_min -1.419 _refine_diff_density_rms 0.218 #==END data_4 _database_code_depnum_ccdc_archive 'CCDC 860631' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 H2 K O9 S2 Tb' _chemical_formula_weight 408.16 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' 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' K K 0.2009 0.2494 '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 ? _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.128(3) _cell_length_b 8.3268(11) _cell_length_c 10.344(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.305(16) _cell_angle_gamma 90.00 _cell_volume 760.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2396 _cell_measurement_theta_min 3.3584 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 10.415 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5128 _exptl_absorpt_correction_T_max 1.0000 _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 '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 4628 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1309 _reflns_number_gt 1268 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+1.5250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0065(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1309 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0474 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.75631(2) 0.14546(2) 0.53701(2) 0.00945(12) Uani 1 1 d . . . K1 K 0.28985(12) 0.32704(14) 0.31303(13) 0.0238(3) Uani 1 1 d . . . S1 S 0.99878(12) -0.19946(13) 0.60068(12) 0.0122(2) Uani 1 1 d . . . S2 S 0.55123(12) 0.13587(12) 0.68117(12) 0.0106(2) Uani 1 1 d . . . O1 O 0.9148(4) -0.2770(4) 0.4574(4) 0.0347(9) Uani 1 1 d . . . O2 O 1.1340(4) -0.1161(4) 0.6147(4) 0.0261(8) Uani 1 1 d . . . O3 O 1.0489(3) -0.3205(4) 0.7199(4) 0.0173(7) Uani 1 1 d . . . O4 O 0.9028(3) -0.0861(4) 0.6255(3) 0.0170(7) Uani 1 1 d . . . O5 O 0.3999(3) 0.0624(4) 0.6130(4) 0.0193(7) Uani 1 1 d . . . O6 O 0.5591(3) 0.2545(4) 0.5779(3) 0.0187(7) Uani 1 1 d . . . O7 O 0.6688(3) 0.0160(4) 0.7073(4) 0.0202(7) Uani 1 1 d . . . O8 O 0.5772(3) 0.2134(4) 0.8182(3) 0.0169(7) Uani 1 1 d . . . O9W O 0.8256(4) 0.4277(4) 0.5522(4) 0.0219(7) Uani 1 1 d . . . H9WA H 0.7571 0.4993 0.5166 0.026 Uiso 1 1 d R . . H9WB H 0.9184 0.4545 0.5930 0.026 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 Tb1 0.00863(15) 0.01113(16) 0.00694(17) -0.00025(7) 0.00252(12) 0.00085(7) K1 0.0196(5) 0.0341(6) 0.0170(6) -0.0001(5) 0.0083(5) 0.0019(5) S1 0.0133(5) 0.0152(5) 0.0087(6) 0.0026(4) 0.0060(5) 0.0055(4) S2 0.0087(5) 0.0162(6) 0.0075(6) -0.0027(4) 0.0043(5) -0.0025(4) O1 0.048(2) 0.033(2) 0.0111(19) -0.0022(16) 0.0045(19) 0.0154(18) O2 0.0247(19) 0.0280(18) 0.036(2) 0.0116(17) 0.0231(19) 0.0041(15) O3 0.0165(16) 0.0182(16) 0.0115(18) 0.0062(14) 0.0024(15) 0.0038(13) O4 0.0167(16) 0.0184(17) 0.0171(18) 0.0012(14) 0.0094(15) 0.0062(13) O5 0.0129(16) 0.0264(18) 0.0183(19) -0.0098(14) 0.0075(15) -0.0074(13) O6 0.0173(16) 0.0260(18) 0.0171(18) 0.0049(14) 0.0118(15) 0.0024(13) O7 0.0167(16) 0.0197(16) 0.0247(19) 0.0015(15) 0.0104(16) 0.0046(13) O8 0.0166(16) 0.0266(18) 0.0089(17) -0.0079(14) 0.0073(14) -0.0070(14) O9W 0.0172(17) 0.0165(17) 0.030(2) 0.0017(15) 0.0103(16) -0.0010(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.330(3) . ? Tb1 O3 2.332(3) 2_756 ? Tb1 O2 2.338(4) 3_756 ? Tb1 O5 2.346(3) 3_656 ? Tb1 O8 2.403(3) 4_565 ? Tb1 O6 2.412(3) . ? Tb1 O9W 2.435(3) . ? Tb1 O7 2.565(3) . ? K1 O1 2.682(4) 2_655 ? K1 O6 2.828(3) . ? K1 O8 2.904(3) 4_565 ? K1 O7 2.910(3) 3_656 ? K1 O5 2.937(3) 4_565 ? K1 O9W 3.013(3) 3_666 ? K1 O2 3.054(4) 4_465 ? K1 O4 3.074(3) 3_656 ? K1 O3 3.279(3) 3_656 ? S1 O1 1.451(4) . ? S1 O4 1.465(3) . ? S1 O2 1.477(4) . ? S1 O3 1.477(3) . ? S2 O8 1.460(3) . ? S2 O5 1.471(3) . ? S2 O7 1.474(3) . ? S2 O6 1.486(3) . ? O1 K1 2.682(4) 2_645 ? O2 Tb1 2.338(4) 3_756 ? O2 K1 3.054(4) 4_666 ? O3 Tb1 2.332(3) 2_746 ? O3 K1 3.279(3) 3_656 ? O4 K1 3.074(3) 3_656 ? O5 Tb1 2.346(3) 3_656 ? O5 K1 2.937(3) 4_566 ? O7 K1 2.910(3) 3_656 ? O8 Tb1 2.403(3) 4_566 ? O8 K1 2.904(3) 4_566 ? O9W K1 3.013(3) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tb1 O3 68.71(11) . 2_756 ? O4 Tb1 O2 75.93(11) . 3_756 ? O3 Tb1 O2 107.91(13) 2_756 3_756 ? O4 Tb1 O5 75.11(12) . 3_656 ? O3 Tb1 O5 138.04(11) 2_756 3_656 ? O2 Tb1 O5 82.36(12) 3_756 3_656 ? O4 Tb1 O8 144.77(11) . 4_565 ? O3 Tb1 O8 143.74(11) 2_756 4_565 ? O2 Tb1 O8 78.85(12) 3_756 4_565 ? O5 Tb1 O8 77.51(12) 3_656 4_565 ? O4 Tb1 O6 131.70(10) . . ? O3 Tb1 O6 95.80(11) 2_756 . ? O2 Tb1 O6 149.70(11) 3_756 . ? O5 Tb1 O6 92.62(11) 3_656 . ? O8 Tb1 O6 70.90(10) 4_565 . ? O4 Tb1 O9W 131.71(11) . . ? O3 Tb1 O9W 75.43(11) 2_756 . ? O2 Tb1 O9W 85.82(11) 3_756 . ? O5 Tb1 O9W 146.52(11) 3_656 . ? O8 Tb1 O9W 69.50(11) 4_565 . ? O6 Tb1 O9W 82.11(11) . . ? O4 Tb1 O7 75.52(10) . . ? O3 Tb1 O7 72.82(11) 2_756 . ? O2 Tb1 O7 148.74(10) 3_756 . ? O5 Tb1 O7 78.27(11) 3_656 . ? O8 Tb1 O7 119.79(10) 4_565 . ? O6 Tb1 O7 56.20(10) . . ? O9W Tb1 O7 123.15(10) . . ? O4 Tb1 S2 103.75(8) . . ? O3 Tb1 S2 84.06(9) 2_756 . ? O2 Tb1 S2 166.54(10) 3_756 . ? O5 Tb1 S2 84.57(8) 3_656 . ? O8 Tb1 S2 95.22(8) 4_565 . ? O6 Tb1 S2 27.96(8) . . ? O9W Tb1 S2 103.55(8) . . ? O7 Tb1 S2 28.25(7) . . ? O4 Tb1 K1 66.96(8) . 2_645 ? O3 Tb1 K1 131.68(8) 2_756 2_645 ? O2 Tb1 K1 42.77(9) 3_756 2_645 ? O5 Tb1 K1 39.85(7) 3_656 2_645 ? O8 Tb1 K1 77.81(8) 4_565 2_645 ? O6 Tb1 K1 128.18(8) . 2_645 ? O9W Tb1 K1 123.71(8) . 2_645 ? O7 Tb1 K1 112.67(8) . 2_645 ? S2 Tb1 K1 124.38(3) . 2_645 ? O4 Tb1 K1 42.95(8) . 3_656 ? O3 Tb1 K1 84.65(8) 2_756 3_656 ? O2 Tb1 K1 108.37(8) 3_756 3_656 ? O5 Tb1 K1 53.96(9) 3_656 3_656 ? O8 Tb1 K1 128.06(8) 4_565 3_656 ? O6 Tb1 K1 92.03(8) . 3_656 ? O9W Tb1 K1 158.48(8) . 3_656 ? O7 Tb1 K1 40.47(7) . 3_656 ? S2 Tb1 K1 65.73(3) . 3_656 ? K1 Tb1 K1 75.93(3) 2_645 3_656 ? O4 Tb1 K1 143.76(8) . . ? O3 Tb1 K1 130.63(8) 2_756 . ? O2 Tb1 K1 115.10(10) 3_756 . ? O5 Tb1 K1 72.64(8) 3_656 . ? O8 Tb1 K1 38.08(7) 4_565 . ? O6 Tb1 K1 36.21(8) . . ? O9W Tb1 K1 84.46(8) . . ? O7 Tb1 K1 82.11(7) . . ? S2 Tb1 K1 57.33(4) . . ? K1 Tb1 K1 97.00(3) 2_645 . ? K1 Tb1 K1 102.99(2) 3_656 . ? O1 K1 O6 145.90(12) 2_655 . ? O1 K1 O8 103.76(12) 2_655 4_565 ? O6 K1 O8 58.31(9) . 4_565 ? O1 K1 O7 70.88(11) 2_655 3_656 ? O6 K1 O7 75.87(10) . 3_656 ? O8 K1 O7 73.08(9) 4_565 3_656 ? O1 K1 O5 74.51(11) 2_655 4_565 ? O6 K1 O5 103.35(10) . 4_565 ? O8 K1 O5 47.70(9) 4_565 4_565 ? O7 K1 O5 97.99(10) 3_656 4_565 ? O1 K1 O9W 115.13(12) 2_655 3_666 ? O6 K1 O9W 96.03(10) . 3_666 ? O8 K1 O9W 133.04(10) 4_565 3_666 ? O7 K1 O9W 143.25(10) 3_656 3_666 ? O5 K1 O9W 118.71(10) 4_565 3_666 ? O1 K1 O2 70.89(11) 2_655 4_465 ? O6 K1 O2 139.08(10) . 4_465 ? O8 K1 O2 106.73(9) 4_565 4_465 ? O7 K1 O2 140.41(10) 3_656 4_465 ? O5 K1 O2 61.93(9) 4_565 4_465 ? O9W K1 O2 65.57(10) 3_666 4_465 ? O1 K1 O4 76.12(10) 2_655 3_656 ? O6 K1 O4 93.96(9) . 3_656 ? O8 K1 O4 130.71(9) 4_565 3_656 ? O7 K1 O4 60.18(8) 3_656 3_656 ? O5 K1 O4 148.03(10) 4_565 3_656 ? O9W K1 O4 85.26(9) 3_666 3_656 ? O2 K1 O4 118.79(9) 4_465 3_656 ? O1 K1 O3 69.58(11) 2_655 3_656 ? O6 K1 O3 124.14(9) . 3_656 ? O8 K1 O3 171.28(10) 4_565 3_656 ? O7 K1 O3 99.02(9) 3_656 3_656 ? O5 K1 O3 132.12(9) 4_565 3_656 ? O9W K1 O3 55.65(9) 3_666 3_656 ? O2 K1 O3 76.85(9) 4_465 3_656 ? O4 K1 O3 43.34(8) 3_656 3_656 ? O1 K1 S2 88.19(10) 2_655 4_565 ? O6 K1 S2 80.98(8) . 4_565 ? O8 K1 S2 23.70(6) 4_565 4_565 ? O7 K1 S2 84.05(7) 3_656 4_565 ? O5 K1 S2 24.07(6) 4_565 4_565 ? O9W K1 S2 130.75(7) 3_666 4_565 ? O2 K1 S2 84.87(7) 4_465 4_565 ? O4 K1 S2 143.87(7) 3_656 4_565 ? O3 K1 S2 154.78(7) 3_656 4_565 ? O1 K1 S1 81.76(9) 2_655 3_656 ? O6 K1 S1 102.20(8) . 3_656 ? O8 K1 S1 152.50(8) 4_565 3_656 ? O7 K1 S1 83.78(7) 3_656 3_656 ? O5 K1 S1 154.03(7) 4_565 3_656 ? O9W K1 S1 62.63(7) 3_666 3_656 ? O2 K1 S1 100.55(7) 4_465 3_656 ? O4 K1 S1 23.63(6) 3_656 3_656 ? O3 K1 S1 24.16(6) 3_656 3_656 ? S2 K1 S1 166.23(4) 4_565 3_656 ? O1 K1 S2 136.06(9) 2_655 . ? O6 K1 S2 20.35(6) . . ? O8 K1 S2 74.34(7) 4_565 . ? O7 K1 S2 66.63(7) 3_656 . ? O5 K1 S2 121.57(7) 4_565 . ? O9W K1 S2 93.35(8) 3_666 . ? O2 K1 S2 152.76(8) 4_465 . ? O4 K1 S2 73.63(7) 3_656 . ? O3 K1 S2 106.26(7) 3_656 . ? S2 K1 S2 97.97(5) 4_565 . ? S1 K1 S2 83.05(4) 3_656 . ? O1 S1 O4 111.0(2) . . ? O1 S1 O2 111.2(2) . . ? O4 S1 O2 110.1(2) . . ? O1 S1 O3 109.8(2) . . ? O4 S1 O3 106.25(19) . . ? O2 S1 O3 108.4(2) . . ? O1 S1 K1 88.92(18) . 3_656 ? O4 S1 K1 57.24(13) . 3_656 ? O2 S1 K1 159.70(16) . 3_656 ? O3 S1 K1 65.29(13) . 3_656 ? O8 S2 O5 107.42(18) . . ? O8 S2 O7 112.1(2) . . ? O5 S2 O7 111.40(19) . . ? O8 S2 O6 110.89(19) . . ? O5 S2 O6 110.03(19) . . ? O7 S2 O6 105.04(18) . . ? O8 S2 Tb1 127.76(13) . . ? O5 S2 Tb1 124.59(14) . . ? O7 S2 Tb1 55.49(13) . . ? O6 S2 Tb1 49.56(12) . . ? O8 S2 K1 53.09(12) . 4_566 ? O5 S2 K1 54.53(13) . 4_566 ? O7 S2 K1 132.73(14) . 4_566 ? O6 S2 K1 122.23(13) . 4_566 ? Tb1 S2 K1 171.74(4) . 4_566 ? O8 S2 K1 119.90(14) . . ? O5 S2 K1 68.86(14) . . ? O7 S2 K1 125.24(14) . . ? O6 S2 K1 41.43(12) . . ? Tb1 S2 K1 78.88(4) . . ? K1 S2 K1 93.71(5) 4_566 . ? S1 O1 K1 133.6(2) . 2_645 ? S1 O2 Tb1 127.4(2) . 3_756 ? S1 O2 K1 125.86(19) . 4_666 ? Tb1 O2 K1 105.90(12) 3_756 4_666 ? S1 O3 Tb1 138.31(19) . 2_746 ? S1 O3 K1 90.56(14) . 3_656 ? Tb1 O3 K1 113.56(12) 2_746 3_656 ? S1 O4 Tb1 144.47(19) . . ? S1 O4 K1 99.13(15) . 3_656 ? Tb1 O4 K1 105.96(10) . 3_656 ? S2 O5 Tb1 146.23(19) . 3_656 ? S2 O5 K1 101.40(16) . 4_566 ? Tb1 O5 K1 109.38(11) 3_656 4_566 ? S2 O6 Tb1 102.49(16) . . ? S2 O6 K1 118.22(16) . . ? Tb1 O6 K1 113.52(12) . . ? S2 O7 Tb1 96.26(16) . . ? S2 O7 K1 141.60(18) . 3_656 ? Tb1 O7 K1 104.62(11) . 3_656 ? S2 O8 Tb1 145.57(18) . 4_566 ? S2 O8 K1 103.21(15) . 4_566 ? Tb1 O8 K1 111.22(11) 4_566 4_566 ? Tb1 O9W K1 121.26(12) . 3_666 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.861 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.140 #==END data_5 _database_code_depnum_ccdc_archive 'CCDC 860632' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 Dy H2 K O9 S2 ' _chemical_formula_weight 411.74 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' 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' K K 0.2009 0.2494 '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 ? _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.107(4) _cell_length_b 8.290(3) _cell_length_c 10.306(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.318(3) _cell_angle_gamma 90.00 _cell_volume 752.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2251 _cell_measurement_theta_min 2.2667 _cell_measurement_theta_max 27.4895 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 11.055 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7152 _exptl_absorpt_correction_T_max 1.0000 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4467 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1315 _reflns_number_gt 1286 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+1.9301P] 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 1315 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_restrained_S_all 1.260 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.74434(2) 0.14401(2) 0.46242(2) 0.00582(10) Uani 1 1 d . . . K1 K 0.79005(13) -0.17061(14) 0.81356(12) 0.0203(3) Uani 1 1 d . . . S1 S 0.94849(13) 0.13595(13) 0.31866(12) 0.0074(2) Uani 1 1 d . . . S2 S 0.49723(12) 0.20140(14) 0.59955(12) 0.0077(2) Uani 1 1 d . . . O1 O 0.9397(4) 0.2561(4) 0.4210(4) 0.0157(7) Uani 1 1 d . . . O2 O 1.1004(4) 0.0631(4) 0.3877(4) 0.0150(7) Uani 1 1 d . . . O3 O 0.9219(4) 0.2137(4) 0.1807(3) 0.0139(7) Uani 1 1 d . . . O4 O 0.8315(4) 0.0151(4) 0.2921(4) 0.0161(7) Uani 1 1 d . . . O5 O 0.6312(4) 0.1170(4) 0.6101(4) 0.0197(8) Uani 1 1 d . . . O6 O 0.4112(4) 0.2800(4) 0.4569(4) 0.0228(8) Uani 1 1 d . . . O7 O 0.5504(4) 0.3211(4) 0.7205(4) 0.0139(7) Uani 1 1 d . . . O8 O 0.4031(4) 0.0863(4) 0.6271(4) 0.0133(7) Uani 1 1 d . . . O9W O 0.6723(4) 0.4247(4) 0.4461(4) 0.0159(7) Uani 1 1 d . . . H1A H 0.6535 0.4679 0.5156 0.019 Uiso 1 1 d R . . H1B H 0.6642 0.4860 0.3704 0.019 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 Dy1 0.00475(14) 0.00496(14) 0.00702(13) 0.00011(7) 0.00231(10) -0.00056(7) K1 0.0164(6) 0.0267(6) 0.0178(6) 0.0001(5) 0.0082(5) 0.0014(5) S1 0.0046(6) 0.0096(6) 0.0086(5) 0.0023(4) 0.0038(4) 0.0015(4) S2 0.0085(5) 0.0068(5) 0.0082(5) -0.0021(4) 0.0046(4) -0.0039(4) O1 0.0152(17) 0.0197(18) 0.0161(17) -0.0060(14) 0.0108(14) -0.0025(14) O2 0.0076(17) 0.0191(18) 0.0175(17) 0.0094(14) 0.0055(14) 0.0065(14) O3 0.0114(17) 0.0201(19) 0.0114(16) 0.0070(14) 0.0064(14) 0.0069(14) O4 0.0108(17) 0.0131(17) 0.0265(19) 0.0004(14) 0.0108(15) -0.0022(14) O5 0.019(2) 0.0211(19) 0.031(2) -0.0076(16) 0.0213(17) -0.0035(15) O6 0.029(2) 0.0186(19) 0.0124(17) 0.0027(14) 0.0042(16) -0.0064(16) O7 0.0135(17) 0.0112(16) 0.0115(16) -0.0041(13) 0.0019(14) -0.0018(14) O8 0.0125(18) 0.0129(17) 0.0175(16) -0.0024(14) 0.0097(14) -0.0082(14) O9W 0.0204(19) 0.0099(17) 0.0211(18) 0.0006(14) 0.0130(15) 0.0023(15) _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 Dy1 O7 2.314(3) 4_565 ? Dy1 O8 2.318(3) 3_656 ? Dy1 O5 2.319(4) . ? Dy1 O2 2.329(3) 3_756 ? Dy1 O3 2.391(3) 4_566 ? Dy1 O1 2.402(3) . ? Dy1 O9W 2.419(3) . ? Dy1 O4 2.552(4) . ? K1 O6 2.679(4) 3_656 ? K1 O1 2.828(4) 2_746 ? K1 O3 2.905(4) 3_756 ? K1 O4 2.911(4) 4_556 ? K1 O2 2.928(4) 3_756 ? K1 O9W 3.004(4) 4_566 ? K1 O5 3.060(4) . ? K1 O8 3.068(4) 2_646 ? K1 O7 3.284(4) 2_646 ? S1 O3 1.461(3) . ? S1 O4 1.470(3) . ? S1 O2 1.469(3) . ? S1 O1 1.484(3) . ? S2 O6 1.446(4) . ? S2 O8 1.470(3) . ? S2 O7 1.474(3) . ? S2 O5 1.480(4) . ? O1 K1 2.828(4) 2_756 ? O2 Dy1 2.329(3) 3_756 ? O2 K1 2.928(4) 3_756 ? O3 Dy1 2.391(3) 4_565 ? O3 K1 2.905(4) 3_756 ? O4 K1 2.911(4) 4 ? O6 K1 2.679(4) 3_656 ? O7 Dy1 2.314(3) 4_566 ? O7 K1 3.284(4) 2_656 ? O8 Dy1 2.318(3) 3_656 ? O8 K1 3.068(4) 2_656 ? O9W K1 3.004(4) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Dy1 O8 68.52(12) 4_565 3_656 ? O7 Dy1 O5 106.80(14) 4_565 . ? O8 Dy1 O5 75.77(12) 3_656 . ? O7 Dy1 O2 138.32(12) 4_565 3_756 ? O8 Dy1 O2 75.49(12) 3_656 3_756 ? O5 Dy1 O2 83.26(13) . 3_756 ? O7 Dy1 O3 143.25(12) 4_565 4_566 ? O8 Dy1 O3 145.17(11) 3_656 4_566 ? O5 Dy1 O3 79.30(13) . 4_566 ? O2 Dy1 O3 77.78(12) 3_756 4_566 ? O7 Dy1 O1 95.55(12) 4_565 . ? O8 Dy1 O1 132.23(11) 3_656 . ? O5 Dy1 O1 150.04(12) . . ? O2 Dy1 O1 93.28(12) 3_756 . ? O3 Dy1 O1 70.90(11) 4_566 . ? O7 Dy1 O9W 74.77(11) 4_565 . ? O8 Dy1 O9W 130.69(12) 3_656 . ? O5 Dy1 O9W 84.85(12) . . ? O2 Dy1 O9W 146.88(12) 3_756 . ? O3 Dy1 O9W 69.68(11) 4_566 . ? O1 Dy1 O9W 82.02(12) . . ? O7 Dy1 O4 72.97(12) 4_565 . ? O8 Dy1 O4 75.67(11) 3_656 . ? O5 Dy1 O4 149.11(11) . . ? O2 Dy1 O4 78.45(12) 3_756 . ? O3 Dy1 O4 120.05(11) 4_566 . ? O1 Dy1 O4 56.57(11) . . ? O9W Dy1 O4 123.24(11) . . ? O7 Dy1 S1 84.16(10) 4_565 . ? O8 Dy1 S1 104.05(9) 3_656 . ? O5 Dy1 S1 167.73(10) . . ? O2 Dy1 S1 84.84(9) 3_756 . ? O3 Dy1 S1 95.30(9) 4_566 . ? O1 Dy1 S1 28.19(8) . . ? O9W Dy1 S1 103.73(8) . . ? O4 Dy1 S1 28.39(8) . . ? O7 Dy1 K1 131.90(9) 4_565 . ? O8 Dy1 K1 67.55(8) 3_656 . ? O5 Dy1 K1 43.38(10) . . ? O2 Dy1 K1 40.06(8) 3_756 . ? O3 Dy1 K1 77.62(9) 4_566 . ? O1 Dy1 K1 128.72(8) . . ? O9W Dy1 K1 123.16(8) . . ? O4 Dy1 K1 113.21(8) . . ? S1 Dy1 K1 124.87(3) . . ? O7 Dy1 K1 84.98(9) 4_565 4 ? O8 Dy1 K1 43.10(9) 3_656 4 ? O5 Dy1 K1 108.56(9) . 4 ? O2 Dy1 K1 53.92(9) 3_756 4 ? O3 Dy1 K1 128.37(8) 4_566 4 ? O1 Dy1 K1 92.76(8) . 4 ? O9W Dy1 K1 158.42(8) . 4 ? O4 Dy1 K1 40.75(8) . 4 ? S1 Dy1 K1 66.13(3) . 4 ? K1 Dy1 K1 76.21(3) . 4 ? O7 Dy1 K1 130.44(9) 4_565 2_756 ? O8 Dy1 K1 144.49(9) 3_656 2_756 ? O5 Dy1 K1 115.82(10) . 2_756 ? O2 Dy1 K1 73.02(9) 3_756 2_756 ? O3 Dy1 K1 38.15(8) 4_566 2_756 ? O1 Dy1 K1 36.27(8) . 2_756 ? O9W Dy1 K1 84.74(8) . 2_756 ? O4 Dy1 K1 82.29(8) . 2_756 ? S1 Dy1 K1 57.34(4) . 2_756 ? K1 Dy1 K1 97.14(2) . 2_756 ? K1 Dy1 K1 103.40(2) 4 2_756 ? O6 K1 O1 144.63(12) 3_656 2_746 ? O6 K1 O3 102.86(12) 3_656 3_756 ? O1 K1 O3 57.99(10) 2_746 3_756 ? O6 K1 O4 69.70(11) 3_656 4_556 ? O1 K1 O4 75.86(10) 2_746 4_556 ? O3 K1 O4 72.59(10) 3_756 4_556 ? O6 K1 O2 73.97(11) 3_656 3_756 ? O1 K1 O2 103.26(10) 2_746 3_756 ? O3 K1 O2 47.85(9) 3_756 3_756 ? O4 K1 O2 97.26(10) 4_556 3_756 ? O6 K1 O9W 115.75(12) 3_656 4_566 ? O1 K1 O9W 96.67(10) 2_746 4_566 ? O3 K1 O9W 133.64(10) 3_756 4_566 ? O4 K1 O9W 143.51(10) 4_556 4_566 ? O2 K1 O9W 119.14(10) 3_756 4_566 ? O6 K1 O5 71.00(11) 3_656 . ? O1 K1 O5 139.87(11) 2_746 . ? O3 K1 O5 107.12(10) 3_756 . ? O4 K1 O5 139.41(10) 4_556 . ? O2 K1 O5 62.04(10) 3_756 . ? O9W K1 O5 65.86(10) 4_566 . ? O6 K1 O8 75.64(11) 3_656 2_646 ? O1 K1 O8 94.21(10) 2_746 2_646 ? O3 K1 O8 130.11(10) 3_756 2_646 ? O4 K1 O8 60.00(9) 4_556 2_646 ? O2 K1 O8 147.07(10) 3_756 2_646 ? O9W K1 O8 85.57(10) 4_566 2_646 ? O5 K1 O8 118.47(10) . 2_646 ? O6 K1 O7 70.09(11) 3_656 2_646 ? O1 K1 O7 124.35(10) 2_746 2_646 ? O3 K1 O7 170.68(10) 3_756 2_646 ? O4 K1 O7 98.83(9) 4_556 2_646 ? O2 K1 O7 132.11(9) 3_756 2_646 ? O9W K1 O7 55.63(9) 4_566 2_646 ? O5 K1 O7 76.83(9) . 2_646 ? O8 K1 O7 43.28(8) 2_646 2_646 ? O6 K1 S1 87.51(10) 3_656 3_756 ? O1 K1 S1 80.77(8) 2_746 3_756 ? O3 K1 S1 23.83(6) 3_756 3_756 ? O4 K1 S1 83.55(8) 4_556 3_756 ? O2 K1 S1 24.07(6) 3_756 3_756 ? O9W K1 S1 131.19(8) 4_566 3_756 ? O5 K1 S1 85.00(8) . 3_756 ? O8 K1 S1 143.17(7) 2_646 3_756 ? O7 K1 S1 154.70(7) 2_646 3_756 ? O6 K1 S2 82.22(9) 3_656 2_646 ? O1 K1 S2 102.20(8) 2_746 2_646 ? O3 K1 S2 152.00(8) 3_756 2_646 ? O4 K1 S2 83.86(8) 4_556 2_646 ? O2 K1 S2 154.00(8) 3_756 2_646 ? O9W K1 S2 62.53(7) 4_566 2_646 ? O5 K1 S2 100.60(8) . 2_646 ? O8 K1 S2 23.87(6) 2_646 2_646 ? O7 K1 S2 24.22(6) 2_646 2_646 ? S1 K1 S2 165.92(5) 3_756 2_646 ? O6 K1 S1 134.90(9) 3_656 2_746 ? O1 K1 S1 20.47(7) 2_746 2_746 ? O3 K1 S1 73.98(7) 3_756 2_746 ? O4 K1 S1 66.52(7) 4_556 2_746 ? O2 K1 S1 121.43(8) 3_756 2_746 ? O9W K1 S1 94.05(8) 4_566 2_746 ? O5 K1 S1 153.88(8) . 2_746 ? O8 K1 S1 73.76(7) 2_646 2_746 ? O7 K1 S1 106.36(7) 2_646 2_746 ? S1 K1 S1 97.73(5) 3_756 2_746 ? S2 K1 S1 82.97(4) 2_646 2_746 ? O3 S1 O4 111.8(2) . . ? O3 S1 O2 107.7(2) . . ? O4 S1 O2 111.4(2) . . ? O3 S1 O1 110.4(2) . . ? O4 S1 O1 105.5(2) . . ? O2 S1 O1 110.1(2) . . ? O3 S1 Dy1 127.75(14) . . ? O4 S1 Dy1 55.65(14) . . ? O2 S1 Dy1 124.34(14) . . ? O1 S1 Dy1 49.84(14) . . ? O3 S1 K1 53.42(14) . 3_756 ? O4 S1 K1 132.08(15) . 3_756 ? O2 S1 K1 54.41(14) . 3_756 ? O1 S1 K1 122.46(15) . 3_756 ? Dy1 S1 K1 172.19(4) . 3_756 ? O3 S1 K1 119.80(15) . 2_756 ? O4 S1 K1 125.68(15) . 2_756 ? O2 S1 K1 68.56(14) . 2_756 ? O1 S1 K1 41.77(14) . 2_756 ? Dy1 S1 K1 79.11(4) . 2_756 ? K1 S1 K1 93.73(5) 3_756 2_756 ? O6 S2 O8 111.4(2) . . ? O6 S2 O7 110.2(2) . . ? O8 S2 O7 106.0(2) . . ? O6 S2 O5 111.1(2) . . ? O8 S2 O5 109.6(2) . . ? O7 S2 O5 108.3(2) . . ? O6 S2 K1 87.91(17) . 2_656 ? O8 S2 K1 57.64(14) . 2_656 ? O7 S2 K1 66.07(15) . 2_656 ? O5 S2 K1 160.62(16) . 2_656 ? S1 O1 Dy1 101.97(17) . . ? S1 O1 K1 117.76(18) . 2_756 ? Dy1 O1 K1 113.58(13) . 2_756 ? S1 O2 Dy1 146.1(2) . 3_756 ? S1 O2 K1 101.51(16) . 3_756 ? Dy1 O2 K1 109.16(12) 3_756 3_756 ? S1 O3 Dy1 146.0(2) . 4_565 ? S1 O3 K1 102.75(16) . 3_756 ? Dy1 O3 K1 111.28(12) 4_565 3_756 ? S1 O4 Dy1 95.96(16) . . ? S1 O4 K1 141.93(19) . 4 ? Dy1 O4 K1 104.34(12) . 4 ? S2 O5 Dy1 129.3(2) . . ? S2 O5 K1 125.0(2) . . ? Dy1 O5 K1 105.24(13) . . ? S2 O6 K1 132.7(2) . 3_656 ? S2 O7 Dy1 139.6(2) . 4_566 ? S2 O7 K1 89.71(15) . 2_656 ? Dy1 O7 K1 113.79(13) 4_566 2_656 ? S2 O8 Dy1 144.0(2) . 3_656 ? S2 O8 K1 98.49(17) . 2_656 ? Dy1 O8 K1 105.83(12) 3_656 2_656 ? Dy1 O9W K1 120.77(13) . 4_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.634 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.169 #==END data_6 _database_code_depnum_ccdc_archive 'CCDC 860633' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 Ho K O9 S2' _chemical_formula_weight 414.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.079(4) _cell_length_b 8.257(3) _cell_length_c 10.280(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.285(5) _cell_angle_gamma 90.00 _cell_volume 746.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2589 _cell_measurement_theta_min 2.3168 _cell_measurement_theta_max 27.4778 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 11.743 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4837 _exptl_absorpt_correction_T_max 1.0000 _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 '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 6079 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1682 _reflns_number_gt 1527 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1457P)^2^+1.3511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0079(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1682 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.24480(3) -0.14334(3) 0.46233(3) 0.0083(2) Uani 1 1 d . . . K1 K 0.2905(2) 0.3307(2) 0.3137(2) 0.0225(4) Uani 1 1 d . . . S1 S 0.4484(2) -0.13609(19) 0.3190(2) 0.0100(4) Uani 1 1 d . . . S2 S -0.00306(19) -0.2980(2) 0.0990(2) 0.0099(4) Uani 1 1 d . . . O1 O 0.4399(6) -0.2560(7) 0.4234(6) 0.0156(11) Uani 1 1 d . . . O2 O 0.3326(6) -0.0160(7) 0.2940(6) 0.0192(11) Uani 1 1 d . . . O3 O 0.6017(6) -0.0643(7) 0.3866(6) 0.0172(11) Uani 1 1 d . . . O4 O 0.4211(6) -0.2155(7) 0.1826(6) 0.0154(11) Uani 1 1 d . . . O5 O 0.0511(7) -0.1783(7) 0.2212(6) 0.0176(11) Uani 1 1 d . . . O6 O 0.1302(7) -0.3836(7) 0.1065(7) 0.0184(12) Uani 1 1 d . . . O7 O -0.0985(6) -0.4116(7) 0.1229(6) 0.0161(11) Uani 1 1 d . . . O8 O -0.0929(7) -0.2191(7) -0.0444(6) 0.0199(12) Uani 1 1 d . . . O9W O 0.1736(7) -0.4220(7) 0.4467(8) 0.0238(13) Uani 1 1 d . . . H9WA H 0.1249 -0.4674 0.3620 0.029 Uiso 1 1 d R . . H9WB H 0.1963 -0.4754 0.5256 0.029 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 Ho1 0.0074(3) 0.0086(3) 0.0076(3) -0.00007(9) 0.0028(2) 0.00048(8) K1 0.0193(9) 0.0295(9) 0.0180(9) -0.0005(7) 0.0085(8) 0.0012(7) S1 0.0077(9) 0.0133(9) 0.0095(9) -0.0030(6) 0.0046(7) -0.0034(5) S2 0.0094(8) 0.0102(8) 0.0100(8) -0.0012(6) 0.0047(7) -0.0015(6) O1 0.016(2) 0.023(3) 0.013(3) 0.010(2) 0.011(2) 0.003(2) O2 0.018(3) 0.016(3) 0.019(3) 0.001(2) 0.005(2) 0.003(2) O3 0.011(2) 0.027(3) 0.015(3) -0.011(2) 0.008(2) -0.007(2) O4 0.014(2) 0.022(3) 0.006(2) -0.010(2) 0.002(2) -0.005(2) O5 0.023(3) 0.014(2) 0.006(3) 0.006(2) -0.001(2) 0.003(2) O6 0.018(3) 0.022(3) 0.018(3) -0.002(2) 0.011(2) 0.004(2) O7 0.016(3) 0.014(3) 0.015(3) 0.002(2) 0.005(2) -0.007(2) O8 0.026(3) 0.021(3) 0.008(3) 0.006(2) 0.004(2) -0.002(2) O9W 0.026(3) 0.014(3) 0.034(4) 0.000(2) 0.016(3) -0.004(2) _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 Ho1 O6 2.292(6) 4_556 ? Ho1 O5 2.303(6) . ? Ho1 O7 2.311(5) 2 ? Ho1 O3 2.323(5) 3_656 ? Ho1 O1 2.379(5) . ? Ho1 O9W 2.392(5) . ? Ho1 O4 2.389(5) 4_556 ? Ho1 O2 2.526(6) . ? K1 O8 2.662(6) 3 ? K1 O1 2.808(6) 3_656 ? K1 O3 2.891(6) 2_655 ? K1 O2 2.915(6) . ? K1 O4 2.913(6) 2_655 ? K1 O9W 3.001(6) 1_565 ? K1 O6 3.057(6) 1_565 ? K1 O7 3.067(6) 2 ? K1 O5 3.284(6) 2 ? S1 O4 1.447(5) . ? S1 O2 1.456(6) . ? S1 O3 1.474(5) . ? S1 O1 1.493(5) . ? S2 O7 1.448(5) . ? S2 O8 1.453(5) . ? S2 O5 1.477(6) . ? S2 O6 1.486(6) . ? O1 K1 2.808(6) 3_656 ? O3 Ho1 2.323(5) 3_656 ? O3 K1 2.891(6) 2_645 ? O4 Ho1 2.389(5) 4 ? O4 K1 2.913(6) 2_645 ? O5 K1 3.284(6) 2_545 ? O6 Ho1 2.292(6) 4 ? O6 K1 3.057(6) 1_545 ? O7 Ho1 2.311(5) 2_545 ? O7 K1 3.067(6) 2_545 ? O8 K1 2.662(6) 3 ? O9W K1 3.001(6) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ho1 O5 106.2(2) 4_556 . ? O6 Ho1 O7 74.6(2) 4_556 2 ? O5 Ho1 O7 69.4(2) . 2 ? O6 Ho1 O3 83.0(2) 4_556 3_656 ? O5 Ho1 O3 138.5(2) . 3_656 ? O7 Ho1 O3 74.6(2) 2 3_656 ? O6 Ho1 O1 149.98(19) 4_556 . ? O5 Ho1 O1 96.0(2) . . ? O7 Ho1 O1 133.36(19) 2 . ? O3 Ho1 O1 93.79(19) 3_656 . ? O6 Ho1 O9W 84.7(2) 4_556 . ? O5 Ho1 O9W 74.9(2) . . ? O7 Ho1 O9W 131.01(19) 2 . ? O3 Ho1 O9W 146.6(2) 3_656 . ? O1 Ho1 O9W 81.9(2) . . ? O6 Ho1 O4 79.1(2) 4_556 4_556 ? O5 Ho1 O4 143.58(19) . 4_556 ? O7 Ho1 O4 143.53(19) 2 4_556 ? O3 Ho1 O4 77.5(2) 3_656 4_556 ? O1 Ho1 O4 71.10(18) . 4_556 ? O9W Ho1 O4 69.7(2) . 4_556 ? O6 Ho1 O2 149.16(19) 4_556 . ? O5 Ho1 O2 73.2(2) . . ? O7 Ho1 O2 76.59(19) 2 . ? O3 Ho1 O2 78.98(19) 3_656 . ? O1 Ho1 O2 56.79(17) . . ? O9W Ho1 O2 123.3(2) . . ? O4 Ho1 O2 120.34(18) 4_556 . ? O6 Ho1 S1 168.27(15) 4_556 . ? O5 Ho1 S1 84.20(16) . . ? O7 Ho1 S1 104.80(15) 2 . ? O3 Ho1 S1 85.60(14) 3_656 . ? O1 Ho1 S1 28.57(13) . . ? O9W Ho1 S1 103.69(15) . . ? O4 Ho1 S1 95.92(13) 4_556 . ? O2 Ho1 S1 28.23(13) . . ? O6 Ho1 K1 43.59(15) 4_556 4_566 ? O5 Ho1 K1 132.00(15) . 4_566 ? O7 Ho1 K1 66.75(14) 2 4_566 ? O3 Ho1 K1 39.50(14) 3_656 4_566 ? O1 Ho1 K1 128.42(14) . 4_566 ? O9W Ho1 K1 122.82(16) . 4_566 ? O4 Ho1 K1 76.77(14) 4_556 4_566 ? O2 Ho1 K1 113.46(14) . 4_566 ? S1 Ho1 K1 125.09(5) . 4_566 ? O6 Ho1 K1 108.44(15) 4_556 . ? O5 Ho1 K1 85.04(14) . . ? O7 Ho1 K1 43.30(15) 2 . ? O3 Ho1 K1 54.17(15) 3_656 . ? O1 Ho1 K1 93.15(13) . . ? O9W Ho1 K1 158.56(17) . . ? O4 Ho1 K1 128.37(14) 4_556 . ? O2 Ho1 K1 40.94(13) . . ? S1 Ho1 K1 66.28(4) . . ? K1 Ho1 K1 76.42(3) 4_566 . ? O6 Ho1 K1 116.29(16) 4_556 3_656 ? O5 Ho1 K1 130.44(16) . 3_656 ? O7 Ho1 K1 144.48(14) 2 3_656 ? O3 Ho1 K1 73.58(14) 3_656 3_656 ? O1 Ho1 K1 35.81(13) . 3_656 ? O9W Ho1 K1 84.49(15) . 3_656 ? O4 Ho1 K1 38.65(13) 4_556 3_656 ? O2 Ho1 K1 82.19(13) . 3_656 ? S1 Ho1 K1 57.42(5) . 3_656 ? K1 Ho1 K1 97.11(3) 4_566 3_656 ? K1 Ho1 K1 103.63(4) . 3_656 ? O8 K1 O1 143.56(19) 3 3_656 ? O8 K1 O3 73.36(18) 3 2_655 ? O1 K1 O3 103.15(16) 3_656 2_655 ? O8 K1 O2 69.41(17) 3 . ? O1 K1 O2 75.28(16) 3_656 . ? O3 K1 O2 97.30(17) 2_655 . ? O8 K1 O4 101.68(18) 3 2_655 ? O1 K1 O4 57.93(15) 3_656 2_655 ? O3 K1 O4 47.82(15) 2_655 2_655 ? O2 K1 O4 72.21(17) . 2_655 ? O8 K1 O9W 116.67(19) 3 1_565 ? O1 K1 O9W 96.98(18) 3_656 1_565 ? O3 K1 O9W 119.25(17) 2_655 1_565 ? O2 K1 O9W 143.37(18) . 1_565 ? O4 K1 O9W 134.00(17) 2_655 1_565 ? O8 K1 O6 70.79(17) 3 1_565 ? O1 K1 O6 140.61(18) 3_656 1_565 ? O3 K1 O6 61.77(16) 2_655 1_565 ? O2 K1 O6 139.00(17) . 1_565 ? O4 K1 O6 107.09(17) 2_655 1_565 ? O9W K1 O6 66.49(18) 1_565 1_565 ? O8 K1 O7 76.51(17) 3 2 ? O1 K1 O7 93.79(16) 3_656 2 ? O3 K1 O7 147.46(18) 2_655 2 ? O2 K1 O7 60.17(15) . 2 ? O4 K1 O7 129.88(16) 2_655 2 ? O9W K1 O7 85.27(15) 1_565 2 ? O6 K1 O7 118.57(16) 1_565 2 ? O8 K1 O5 70.59(17) 3 2 ? O1 K1 O5 124.71(16) 3_656 2 ? O3 K1 O5 131.94(16) 2_655 2 ? O2 K1 O5 98.66(16) . 2 ? O4 K1 O5 169.97(17) 2_655 2 ? O9W K1 O5 55.99(15) 1_565 2 ? O6 K1 O5 76.88(16) 1_565 2 ? O7 K1 O5 43.23(14) 2 2 ? O8 K1 S1 86.83(15) 3 2_655 ? O1 K1 S1 80.50(12) 3_656 2_655 ? O3 K1 S1 24.15(11) 2_655 2_655 ? O2 K1 S1 83.57(13) . 2_655 ? O4 K1 S1 23.70(10) 2_655 2_655 ? O9W K1 S1 131.20(13) 1_565 2_655 ? O6 K1 S1 84.85(13) 1_565 2_655 ? O7 K1 S1 143.41(12) 2 2_655 ? O5 K1 S1 154.55(12) 2 2_655 ? O8 K1 S2 82.70(14) 3 2 ? O1 K1 S2 102.35(12) 3_656 2 ? O3 K1 S2 153.85(13) 2_655 2 ? O2 K1 S2 83.63(13) . 2 ? O4 K1 S2 151.71(13) 2_655 2 ? O9W K1 S2 62.77(12) 1_565 2 ? O6 K1 S2 100.76(13) 1_565 2 ? O7 K1 S2 23.50(10) 2 2 ? O5 K1 S2 24.30(11) 2 2 ? S1 K1 S2 165.69(8) 2_655 2 ? O8 K1 S1 134.35(14) 3 3_656 ? O1 K1 S1 20.61(11) 3_656 3_656 ? O3 K1 S1 121.53(13) 2_655 3_656 ? O2 K1 S1 66.08(12) . 3_656 ? O4 K1 S1 74.12(11) 2_655 3_656 ? O9W K1 S1 94.07(14) 1_565 3_656 ? O6 K1 S1 154.71(13) 1_565 3_656 ? O7 K1 S1 73.20(11) 2 3_656 ? O5 K1 S1 106.38(12) 2 3_656 ? S1 K1 S1 97.73(7) 2_655 3_656 ? S2 K1 S1 82.87(7) 2 3_656 ? O4 S1 O2 112.4(3) . . ? O4 S1 O3 107.3(3) . . ? O2 S1 O3 112.0(3) . . ? O4 S1 O1 110.2(3) . . ? O2 S1 O1 104.8(3) . . ? O3 S1 O1 110.1(3) . . ? O4 S1 Ho1 127.1(2) . . ? O2 S1 Ho1 55.2(2) . . ? O3 S1 Ho1 125.2(2) . . ? O1 S1 Ho1 49.6(2) . . ? O4 S1 K1 54.0(2) . 2_645 ? O2 S1 K1 132.3(3) . 2_645 ? O3 S1 K1 53.4(2) . 2_645 ? O1 S1 K1 123.0(2) . 2_645 ? Ho1 S1 K1 172.47(7) . 2_645 ? O4 S1 K1 119.3(2) . 3_656 ? O2 S1 K1 125.2(3) . 3_656 ? O3 S1 K1 68.9(3) . 3_656 ? O1 S1 K1 41.4(2) . 3_656 ? Ho1 S1 K1 79.16(6) . 3_656 ? K1 S1 K1 93.87(7) 2_645 3_656 ? O7 S2 O8 109.0(3) . . ? O7 S2 O5 106.9(3) . . ? O8 S2 O5 110.5(3) . . ? O7 S2 O6 110.0(3) . . ? O8 S2 O6 111.4(4) . . ? O5 S2 O6 109.0(3) . . ? O7 S2 K1 57.6(2) . 2_545 ? O8 S2 K1 86.7(2) . 2_545 ? O5 S2 K1 66.2(2) . 2_545 ? O6 S2 K1 161.5(3) . 2_545 ? O7 S2 K1 86.3(2) . 3 ? O8 S2 K1 31.0(2) . 3 ? O5 S2 K1 139.4(2) . 3 ? O6 S2 K1 101.5(2) . 3 ? K1 S2 K1 91.86(6) 2_545 3 ? S1 O1 Ho1 101.8(3) . . ? S1 O1 K1 118.0(3) . 3_656 ? Ho1 O1 K1 114.5(2) . 3_656 ? S1 O2 Ho1 96.6(3) . . ? S1 O2 K1 142.0(3) . . ? Ho1 O2 K1 104.5(2) . . ? S1 O3 Ho1 144.5(3) . 3_656 ? S1 O3 K1 102.5(3) . 2_645 ? Ho1 O3 K1 109.8(2) 3_656 2_645 ? S1 O4 Ho1 147.2(3) . 4 ? S1 O4 K1 102.3(3) . 2_645 ? Ho1 O4 K1 110.54(19) 4 2_645 ? S2 O5 Ho1 139.9(3) . . ? S2 O5 K1 89.5(3) . 2_545 ? Ho1 O5 K1 113.9(2) . 2_545 ? S2 O6 Ho1 130.5(4) . 4 ? S2 O6 K1 124.0(3) . 1_545 ? Ho1 O6 K1 105.3(2) 4 1_545 ? S2 O7 Ho1 145.7(4) . 2_545 ? S2 O7 K1 98.9(3) . 2_545 ? Ho1 O7 K1 105.6(2) 2_545 2_545 ? S2 O8 K1 132.7(3) . 3 ? Ho1 O9W K1 120.9(2) . 1_545 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.341 _refine_diff_density_min -1.585 _refine_diff_density_rms 0.314 #==END data_7 _database_code_depnum_ccdc_archive 'CCDC 860634' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Er4 K4 O36 S8' _chemical_formula_weight 1666.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Er Er -0.2586 4.9576 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0682(12) _cell_length_b 8.2344(8) _cell_length_c 10.2663(12) _cell_angle_alpha 90.00 _cell_angle_beta 119.382(10) _cell_angle_gamma 90.00 _cell_volume 741.65(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2389 _cell_measurement_theta_min 2.2767 _cell_measurement_theta_max 27.4700 _exptl_crystal_description PRISM _exptl_crystal_colour PINK _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 12.463 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4845 _exptl_absorpt_correction_T_max 1.00 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5002 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.38 _reflns_number_total 1584 _reflns_number_gt 1580 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+22.5578P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0261(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1584 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.25505(4) -0.14288(5) -0.46235(4) 0.00687(19) Uani 1 1 d . . . S1 S 0.0521(2) -0.1364(3) -0.3185(2) 0.0082(4) Uani 1 1 d . . . S2 S 0.5035(2) -0.2022(3) -0.5991(2) 0.0083(4) Uani 1 1 d . . . O1 O -0.1021(7) -0.0636(9) -0.3876(7) 0.0147(13) Uani 1 1 d . . . O2 O 0.0789(8) -0.2153(9) -0.1806(7) 0.0166(14) Uani 1 1 d . . . O3 O 0.0620(8) -0.2563(9) -0.4221(7) 0.0157(13) Uani 1 1 d . . . O4 O 0.1691(8) -0.0128(9) -0.2924(8) 0.0177(14) Uani 1 1 d . . . O5 O 0.5923(9) -0.2828(9) -0.4567(8) 0.0192(15) Uani 1 1 d . . . O6 O 0.3700(8) -0.1181(9) -0.6068(8) 0.0162(14) Uani 1 1 d . . . O7 O 0.4477(8) -0.3217(8) -0.7221(7) 0.0131(13) Uani 1 1 d . . . O8 O 0.5980(7) -0.0870(8) -0.6272(7) 0.0130(13) Uani 1 1 d . . . O9W O 0.3292(8) -0.4206(9) -0.4461(8) 0.0159(14) Uani 1 1 d . . . H1A H 0.2577 -0.4989 -0.4836 0.019 Uiso 1 1 d R . . H1C H 0.4286 -0.4470 -0.4025 0.019 Uiso 1 1 d R . . K1 K -0.2095(3) -0.3318(3) -0.6860(2) 0.0210(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0057(2) 0.0065(2) 0.0066(2) 0.00023(12) 0.00169(16) -0.00029(12) S1 0.0061(9) 0.0102(9) 0.0063(9) 0.0032(7) 0.0016(7) 0.0020(7) S2 0.0082(9) 0.0081(9) 0.0070(9) -0.0020(7) 0.0024(7) -0.0026(7) O1 0.010(3) 0.019(3) 0.013(3) 0.009(3) 0.003(2) 0.009(3) O2 0.015(3) 0.023(4) 0.011(3) 0.007(3) 0.005(3) 0.005(3) O3 0.017(3) 0.017(3) 0.015(3) -0.005(3) 0.010(3) -0.003(3) O4 0.011(3) 0.015(3) 0.024(4) -0.001(3) 0.006(3) -0.002(3) O5 0.023(4) 0.018(3) 0.012(3) 0.002(3) 0.005(3) -0.002(3) O6 0.015(3) 0.019(3) 0.023(3) -0.002(3) 0.017(3) 0.000(3) O7 0.014(3) 0.012(3) 0.009(3) -0.004(2) 0.002(2) -0.001(3) O8 0.013(3) 0.013(3) 0.017(3) 0.000(3) 0.011(3) -0.006(3) O9W 0.017(3) 0.012(3) 0.022(3) 0.003(3) 0.013(3) 0.004(3) K1 0.0171(10) 0.0267(11) 0.0171(10) 0.0005(8) 0.0066(8) -0.0009(9) _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 Er1 O7 2.288(6) 4_556 ? Er1 O6 2.294(7) . ? Er1 O8 2.298(7) 3_654 ? Er1 O1 2.304(6) 3_554 ? Er1 O3 2.369(7) . ? Er1 O2 2.373(6) 4 ? Er1 O9W 2.386(7) . ? Er1 O4 2.534(8) . ? S1 O2 1.458(7) . ? S1 O4 1.478(7) . ? S1 O1 1.481(6) . ? S1 O3 1.490(7) . ? S2 O5 1.447(7) . ? S2 O8 1.469(7) . ? S2 O7 1.477(7) . ? S2 O6 1.480(7) . ? O1 Er1 2.304(6) 3_554 ? O2 Er1 2.373(6) 4_556 ? O7 Er1 2.288(6) 4 ? O8 Er1 2.298(7) 3_654 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Er1 O6 106.1(3) 4_556 . ? O7 Er1 O8 68.6(2) 4_556 3_654 ? O6 Er1 O8 75.8(2) . 3_654 ? O7 Er1 O1 138.6(2) 4_556 3_554 ? O6 Er1 O1 83.4(3) . 3_554 ? O8 Er1 O1 75.4(3) 3_654 3_554 ? O7 Er1 O3 95.5(2) 4_556 . ? O6 Er1 O3 149.9(2) . . ? O8 Er1 O3 132.6(2) 3_654 . ? O1 Er1 O3 94.1(2) 3_554 . ? O7 Er1 O2 143.2(3) 4_556 4 ? O6 Er1 O2 79.3(3) . 4 ? O8 Er1 O2 145.0(2) 3_654 4 ? O1 Er1 O2 77.7(3) 3_554 4 ? O3 Er1 O2 70.9(2) . 4 ? O7 Er1 O9W 74.4(2) 4_556 . ? O6 Er1 O9W 83.7(2) . . ? O8 Er1 O9W 130.1(2) 3_654 . ? O1 Er1 O9W 146.9(2) 3_554 . ? O3 Er1 O9W 82.3(2) . . ? O2 Er1 O9W 70.0(2) 4 . ? O7 Er1 O4 73.0(2) 4_556 . ? O6 Er1 O4 149.1(2) . . ? O8 Er1 O4 75.3(2) 3_654 . ? O1 Er1 O4 78.9(2) 3_554 . ? O3 Er1 O4 57.3(2) . . ? O2 Er1 O4 120.6(2) 4 . ? O9W Er1 O4 123.9(2) . . ? O7 Er1 S1 84.01(18) 4_556 . ? O6 Er1 S1 168.72(19) . . ? O8 Er1 S1 104.15(17) 3_654 . ? O1 Er1 S1 85.66(17) 3_554 . ? O3 Er1 S1 28.49(17) . . ? O2 Er1 S1 95.60(17) 4 . ? O9W Er1 S1 104.10(17) . . ? O4 Er1 S1 28.82(16) . . ? O2 S1 O4 112.3(4) . . ? O2 S1 O1 107.2(4) . . ? O4 S1 O1 111.3(4) . . ? O2 S1 O3 110.7(4) . . ? O4 S1 O3 105.1(4) . . ? O1 S1 O3 110.4(4) . . ? O2 S1 Er1 127.8(3) . . ? O4 S1 Er1 55.7(3) . . ? O1 S1 Er1 124.7(3) . . ? O3 S1 Er1 49.3(3) . . ? O5 S2 O8 110.8(4) . . ? O5 S2 O7 110.2(4) . . ? O8 S2 O7 105.9(4) . . ? O5 S2 O6 111.3(4) . . ? O8 S2 O6 110.2(4) . . ? O7 S2 O6 108.2(4) . . ? S1 O1 Er1 144.9(4) . 3_554 ? S1 O2 Er1 146.4(4) . 4_556 ? S1 O3 Er1 102.2(4) . . ? S1 O4 Er1 95.4(3) . . ? S2 O6 Er1 131.1(4) . . ? S2 O7 Er1 140.5(4) . 4 ? S2 O8 Er1 143.6(4) . 3_654 ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.960 _refine_diff_density_min -1.597 _refine_diff_density_rms 0.287