# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kuei Fang Hsu' _publ_contact_author_email HSUKF@MAIL.NCKU.EDU.TW _publ_section_title ; Five Related Metal-Organic Frameworks Constructed From [Ln2(SO4)2(H2O)n]2+ Units and Oxalate or Acetate Ligands ; loop_ _publ_author_name 'Kuei Fang Hsu' 'I-Han Chen' 'Anny Huang' 'Sin-Chiang Huang' ; Hsiao-Chan Liu ; # Attachment 'LnC2O4SO4_Cif.txt' data_Ce1 _database_code_depnum_ccdc_archive 'CCDC 708578' _chemical_formula_moiety NH4[Ce(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 Ce N O9 S' _chemical_formula_weight 360.26 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.93460(10) _cell_length_b 8.27310(10) _cell_length_c 14.3934(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.9980(10) _cell_angle_gamma 90.00 _cell_volume 823.749(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4673 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 28.52 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 5.813 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68285 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 8896 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 28.53 _reflns_number_total 2089 _reflns_number_gt 1926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+21.6906P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_number_reflns 2089 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.235 _refine_ls_restrained_S_all 1.235 _refine_ls_shift/su_max 0.012 _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 Ce1 Ce 0.25442(6) 0.21949(5) 0.41353(3) 0.01250(16) Uani 1 1 d . . . S1 S 0.2426(3) -0.1384(2) 0.49776(13) 0.0142(4) Uani 1 1 d . . . O1 O 0.2851(10) 0.0193(7) 0.5443(4) 0.0241(13) Uani 1 1 d . . . O2 O 0.4106(8) -0.2452(8) 0.5129(5) 0.0255(14) Uani 1 1 d . . . O3 O 0.2018(10) -0.1002(8) 0.3989(4) 0.0264(14) Uani 1 1 d . . . O4 O 0.0767(9) -0.2174(8) 0.5372(5) 0.0294(14) Uani 1 1 d . . . O5 O 0.4504(9) 0.1220(8) 0.2807(4) 0.0222(13) Uani 1 1 d . . . O6 O 0.4425(8) -0.0391(7) 0.1563(4) 0.0211(12) Uani 1 1 d . . . O7 O 0.0629(9) 0.1413(8) 0.2632(4) 0.0212(13) Uani 1 1 d . . . O8 O 0.0589(8) -0.0459(7) 0.1514(4) 0.0209(12) Uani 1 1 d . . . O9 O 0.2429(9) 0.4078(8) 0.5513(4) 0.0256(14) Uani 1 1 d . . . H9A H 0.1393 0.3912 0.5781 0.038 Uiso 1 1 d R . . H9B H 0.3398 0.3898 0.5893 0.038 Uiso 1 1 d R . . C1 C 0.3651(12) 0.0434(10) 0.2159(5) 0.0153(15) Uani 1 1 d . . . C2 C 0.1415(11) 0.0483(9) 0.2099(5) 0.0144(14) Uani 1 1 d . . . N1 N 0.7301(11) 0.3471(10) 0.2153(6) 0.0263(16) 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 Ce1 0.0123(2) 0.0117(2) 0.0137(2) 0.00003(17) 0.00222(13) -0.00108(17) S1 0.0111(8) 0.0133(9) 0.0183(9) 0.0028(7) 0.0014(6) -0.0002(7) O1 0.036(4) 0.014(3) 0.023(3) 0.001(2) 0.001(3) 0.000(3) O2 0.014(3) 0.019(3) 0.043(4) 0.008(3) -0.001(2) 0.002(2) O3 0.034(4) 0.024(3) 0.020(3) 0.002(3) -0.005(3) 0.002(3) O4 0.015(3) 0.024(3) 0.050(4) 0.005(3) 0.008(3) -0.001(3) O5 0.020(3) 0.024(3) 0.022(3) -0.010(3) 0.002(2) -0.005(2) O6 0.019(3) 0.019(3) 0.026(3) -0.006(2) 0.007(2) -0.003(2) O7 0.022(3) 0.022(3) 0.019(3) -0.008(2) -0.002(2) 0.006(2) O8 0.020(3) 0.017(3) 0.025(3) -0.008(2) -0.001(2) 0.003(2) O9 0.019(3) 0.029(4) 0.030(3) -0.014(3) 0.003(2) 0.000(3) C1 0.022(4) 0.012(4) 0.013(3) 0.000(3) 0.005(3) 0.000(3) C2 0.017(3) 0.009(4) 0.017(4) 0.002(3) 0.000(3) 0.004(3) N1 0.022(4) 0.027(4) 0.031(4) 0.006(3) 0.006(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O4 2.450(6) 3_556 ? Ce1 O2 2.494(6) 3_656 ? Ce1 O1 2.504(6) . ? Ce1 O9 2.527(6) . ? Ce1 O7 2.542(6) . ? Ce1 O8 2.547(6) 2 ? Ce1 O5 2.553(6) . ? Ce1 O6 2.583(6) 2 ? Ce1 O3 2.676(7) . ? Ce1 S1 3.203(2) . ? S1 O3 1.466(6) . ? S1 O2 1.466(6) . ? S1 O4 1.471(6) . ? S1 O1 1.487(6) . ? O2 Ce1 2.494(6) 3_656 ? O4 Ce1 2.450(6) 3_556 ? O5 C1 1.251(10) . ? O6 C1 1.246(9) . ? O6 Ce1 2.583(6) 2_545 ? O7 C2 1.240(9) . ? O8 C2 1.255(10) . ? O8 Ce1 2.547(6) 2_545 ? C1 C2 1.547(11) . ? 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 Ce1 O2 137.9(2) 3_556 3_656 ? O4 Ce1 O1 79.1(2) 3_556 . ? O2 Ce1 O1 73.1(2) 3_656 . ? O4 Ce1 O9 72.3(2) 3_556 . ? O2 Ce1 O9 72.2(2) 3_656 . ? O1 Ce1 O9 79.9(2) . . ? O4 Ce1 O7 78.5(2) 3_556 . ? O2 Ce1 O7 143.0(2) 3_656 . ? O1 Ce1 O7 118.9(2) . . ? O9 Ce1 O7 141.4(2) . . ? O4 Ce1 O8 128.5(2) 3_556 2 ? O2 Ce1 O8 66.96(19) 3_656 2 ? O1 Ce1 O8 139.6(2) . 2 ? O9 Ce1 O8 82.1(2) . 2 ? O7 Ce1 O8 97.5(2) . 2 ? O4 Ce1 O5 140.7(2) 3_556 . ? O2 Ce1 O5 79.4(2) 3_656 . ? O1 Ce1 O5 109.4(2) . . ? O9 Ce1 O5 146.1(2) . . ? O7 Ce1 O5 63.64(19) . . ? O8 Ce1 O5 69.8(2) 2 . ? O4 Ce1 O6 68.7(2) 3_556 2 ? O2 Ce1 O6 123.4(2) 3_656 2 ? O1 Ce1 O6 144.9(2) . 2 ? O9 Ce1 O6 77.5(2) . 2 ? O7 Ce1 O6 68.6(2) . 2 ? O8 Ce1 O6 62.37(19) 2 2 ? O5 Ce1 O6 104.3(2) . 2 ? O4 Ce1 O3 83.7(2) 3_556 . ? O2 Ce1 O3 103.6(2) 3_656 . ? O1 Ce1 O3 53.82(19) . . ? O9 Ce1 O3 131.3(2) . . ? O7 Ce1 O3 67.74(19) . . ? O8 Ce1 O3 142.6(2) 2 . ? O5 Ce1 O3 72.9(2) . . ? O6 Ce1 O3 131.91(19) 2 . ? O4 Ce1 S1 80.49(16) 3_556 . ? O2 Ce1 S1 88.04(14) 3_656 . ? O1 Ce1 S1 26.80(15) . . ? O9 Ce1 S1 105.66(17) . . ? O7 Ce1 S1 93.50(15) . . ? O8 Ce1 S1 150.54(14) 2 . ? O5 Ce1 S1 91.18(15) . . ? O6 Ce1 S1 146.65(14) 2 . ? O3 Ce1 S1 27.02(13) . . ? O3 S1 O2 111.8(4) . . ? O3 S1 O4 111.5(4) . . ? O2 S1 O4 108.0(4) . . ? O3 S1 O1 105.5(4) . . ? O2 S1 O1 109.3(4) . . ? O4 S1 O1 110.6(4) . . ? O3 S1 Ce1 56.1(3) . . ? O2 S1 Ce1 124.9(3) . . ? O4 S1 Ce1 126.7(3) . . ? O1 S1 Ce1 49.4(2) . . ? S1 O1 Ce1 103.8(3) . . ? S1 O2 Ce1 136.0(4) . 3_656 ? S1 O3 Ce1 96.9(3) . . ? S1 O4 Ce1 152.7(4) . 3_556 ? C1 O5 Ce1 118.3(5) . . ? C1 O6 Ce1 116.7(5) . 2_545 ? C2 O7 Ce1 117.3(5) . . ? C2 O8 Ce1 119.9(5) . 2_545 ? O6 C1 O5 126.4(8) . . ? O6 C1 C2 117.0(7) . . ? O5 C1 C2 116.6(7) . . ? O7 C2 O8 126.9(8) . . ? O7 C2 C1 117.7(7) . . ? O8 C2 C1 115.5(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.255 _refine_diff_density_min -1.987 _refine_diff_density_rms 0.247 #===END=============================================================== data_Nd2 _database_code_depnum_ccdc_archive 'CCDC 708579' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Nd(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 N Nd O9 S' _chemical_formula_weight 364.38 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' 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' Nd Nd -0.1943 3.0179 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1876(5) _cell_length_b 11.7787(7) _cell_length_c 9.2798(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.8850(10) _cell_angle_gamma 90.00 _cell_volume 851.69(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3972 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour light-purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 6.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.676430 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 6151 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2108 _reflns_number_gt 2026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 noref _refine_ls_number_reflns 2108 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.794 _refine_ls_restrained_S_all 0.794 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.880407(19) 0.588382(13) 0.153911(17) 0.01337(12) Uani 1 1 d . . . S1 S 0.77796(10) 0.63255(6) -0.21144(8) 0.01468(18) Uani 1 1 d . . . O1 O 0.9196(3) 0.5537(2) -0.1275(3) 0.0210(5) Uani 1 1 d . . . O2 O 0.7221(4) 0.6857(2) -0.0914(3) 0.0325(6) Uani 1 1 d . . . O3 O 0.6399(5) 0.5698(3) -0.3161(4) 0.0394(8) Uani 1 1 d . . . O4 O 0.8473(4) 0.7159(2) -0.2927(3) 0.0317(6) Uani 1 1 d . . . O5 O 0.5701(3) 0.6086(2) 0.1312(3) 0.0225(5) Uani 1 1 d . . . O6 O 0.3054(3) 0.5666(2) -0.0151(3) 0.0189(5) Uani 1 1 d . . . O7 O 0.8349(4) 0.4516(3) 0.3458(3) 0.0316(7) Uani 1 1 d . . . O8 O 0.9177(4) 0.3913(2) 0.5841(3) 0.0266(6) Uani 1 1 d . . . O9 O 1.1390(3) 0.6942(2) 0.1391(3) 0.0232(5) Uani 1 1 d . . . H9A H 1.1090 0.7594 0.1008 0.035 Uiso 1 1 d R . . H9B H 1.1864 0.6576 0.0838 0.035 Uiso 1 1 d R . . N1 N 0.4482(4) 0.6605(3) -0.5936(4) 0.0324(7) Uani 1 1 d . . . C1 C 0.4655(4) 0.5508(3) 0.0348(4) 0.0159(6) Uani 1 1 d . . . C2 C 0.9279(4) 0.4561(3) 0.4795(3) 0.0181(6) 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 Nd1 0.01149(16) 0.01415(16) 0.01392(16) -0.00073(4) 0.00312(10) 0.00017(4) S1 0.0147(4) 0.0141(4) 0.0140(3) 0.0027(3) 0.0027(3) 0.0018(3) O1 0.0217(13) 0.0179(11) 0.0221(12) 0.0065(10) 0.0049(10) 0.0071(10) O2 0.0403(16) 0.0380(16) 0.0215(12) 0.0046(11) 0.0129(12) 0.0233(13) O3 0.0357(19) 0.0336(16) 0.0345(18) 0.0008(13) -0.0106(14) -0.0097(13) O4 0.0356(15) 0.0214(12) 0.0409(16) 0.0154(11) 0.0159(13) 0.0007(11) O5 0.0123(11) 0.0283(12) 0.0270(14) -0.0127(10) 0.0064(10) -0.0025(10) O6 0.0130(11) 0.0198(10) 0.0232(12) -0.0007(9) 0.0045(10) 0.0017(9) O7 0.0320(16) 0.0421(17) 0.0148(12) 0.0033(12) -0.0014(11) -0.0224(13) O8 0.0284(15) 0.0286(12) 0.0195(12) 0.0034(10) 0.0022(11) -0.0111(11) O9 0.0242(13) 0.0190(12) 0.0311(12) 0.0013(9) 0.0152(11) 0.0019(9) N1 0.0284(17) 0.0344(18) 0.0314(17) -0.0031(14) 0.0047(14) -0.0093(14) C1 0.0130(14) 0.0187(15) 0.0176(14) -0.0019(12) 0.0069(12) -0.0026(12) C2 0.0217(16) 0.0196(16) 0.0129(14) 0.0006(11) 0.0051(13) -0.0029(12) _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 Nd1 O4 2.391(3) 4_576 ? Nd1 O1 2.406(2) 3_765 ? Nd1 O6 2.470(3) 3_665 ? Nd1 O5 2.495(3) . ? Nd1 O8 2.496(3) 3_766 ? Nd1 O9 2.497(2) . ? Nd1 O7 2.512(3) . ? Nd1 O2 2.523(3) . ? Nd1 O1 2.758(2) . ? Nd1 S1 3.2744(8) . ? S1 O3 1.447(3) . ? S1 O4 1.455(2) . ? S1 O2 1.468(2) . ? S1 O1 1.503(2) . ? O1 Nd1 2.406(2) 3_765 ? O4 Nd1 2.391(3) 4_575 ? O5 C1 1.235(4) . ? O6 C1 1.263(4) . ? O6 Nd1 2.470(3) 3_665 ? O7 C2 1.242(4) . ? O8 C2 1.257(4) . ? O8 Nd1 2.496(3) 3_766 ? C1 C1 1.547(6) 3_665 ? C2 C2 1.528(6) 3_766 ? 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 Nd1 O1 144.66(9) 4_576 3_765 ? O4 Nd1 O6 136.87(9) 4_576 3_665 ? O1 Nd1 O6 76.26(8) 3_765 3_665 ? O4 Nd1 O5 75.42(9) 4_576 . ? O1 Nd1 O5 139.90(9) 3_765 . ? O6 Nd1 O5 65.07(8) 3_665 . ? O4 Nd1 O8 77.83(10) 4_576 3_766 ? O1 Nd1 O8 84.14(9) 3_765 3_766 ? O6 Nd1 O8 134.12(9) 3_665 3_766 ? O5 Nd1 O8 115.18(10) . 3_766 ? O4 Nd1 O9 71.47(9) 4_576 . ? O1 Nd1 O9 74.11(8) 3_765 . ? O6 Nd1 O9 137.47(8) 3_665 . ? O5 Nd1 O9 143.75(8) . . ? O8 Nd1 O9 71.76(9) 3_766 . ? O4 Nd1 O7 114.86(10) 4_576 . ? O1 Nd1 O7 83.11(10) 3_765 . ? O6 Nd1 O7 72.20(9) 3_665 . ? O5 Nd1 O7 75.64(10) . . ? O8 Nd1 O7 64.47(8) 3_766 . ? O9 Nd1 O7 132.22(9) . . ? O4 Nd1 O2 71.90(9) 4_576 . ? O1 Nd1 O2 113.66(8) 3_765 . ? O6 Nd1 O2 78.56(9) 3_665 . ? O5 Nd1 O2 69.69(9) . . ? O8 Nd1 O2 146.97(9) 3_766 . ? O9 Nd1 O2 86.15(9) . . ? O7 Nd1 O2 141.62(10) . . ? O4 Nd1 O1 113.13(9) 4_576 . ? O1 Nd1 O1 61.29(9) 3_765 . ? O6 Nd1 O1 68.20(8) 3_665 . ? O5 Nd1 O1 110.23(8) . . ? O8 Nd1 O1 134.57(9) 3_766 . ? O9 Nd1 O1 71.01(8) . . ? O7 Nd1 O1 131.44(9) . . ? O2 Nd1 O1 52.39(7) . . ? O4 Nd1 S1 92.98(7) 4_576 . ? O1 Nd1 S1 88.34(6) 3_765 . ? O6 Nd1 S1 69.91(6) 3_665 . ? O5 Nd1 S1 88.12(7) . . ? O8 Nd1 S1 151.12(6) 3_766 . ? O9 Nd1 S1 79.37(6) . . ? O7 Nd1 S1 142.11(6) . . ? O2 Nd1 S1 25.34(6) . . ? O1 Nd1 S1 27.17(5) . . ? O3 S1 O4 110.2(2) . . ? O3 S1 O2 111.5(2) . . ? O4 S1 O2 111.56(17) . . ? O3 S1 O1 110.57(18) . . ? O4 S1 O1 108.89(16) . . ? O2 S1 O1 103.96(14) . . ? O3 S1 Nd1 120.86(16) . . ? O4 S1 Nd1 128.83(12) . . ? O2 S1 Nd1 47.36(10) . . ? O1 S1 Nd1 56.90(9) . . ? S1 O1 Nd1 144.90(15) . 3_765 ? S1 O1 Nd1 95.93(11) . . ? Nd1 O1 Nd1 118.71(9) 3_765 . ? S1 O2 Nd1 107.30(13) . . ? S1 O4 Nd1 147.67(18) . 4_575 ? C1 O5 Nd1 118.0(2) . . ? C1 O6 Nd1 119.1(2) . 3_665 ? C2 O7 Nd1 120.2(2) . . ? C2 O8 Nd1 120.8(2) . 3_766 ? O5 C1 O6 126.5(3) . . ? O5 C1 C1 117.9(4) . 3_665 ? O6 C1 C1 115.6(3) . 3_665 ? O7 C2 O8 125.5(3) . . ? O7 C2 C2 117.8(3) . 3_766 ? O8 C2 C2 116.7(4) . 3_766 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.119 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.158 #===END=============================================================== data_Eu3 _database_code_depnum_ccdc_archive 'CCDC 708580' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Eu(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 Eu N O9 S' _chemical_formula_weight 372.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.10830(10) _cell_length_b 11.7568(2) _cell_length_c 9.29830(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.5190(10) _cell_angle_gamma 90.00 _cell_volume 840.49(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5467 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.44 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 7.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725676 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 9323 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28.49 _reflns_number_total 2122 _reflns_number_gt 1983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+12.5823P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_number_reflns 2122 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _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 Eu1 Eu 0.87814(3) 0.59014(2) 0.16032(3) 0.01580(11) Uani 1 1 d . . . S1 S 0.78112(17) 0.62961(11) -0.21210(14) 0.0146(3) Uani 1 1 d . . . O1 O 0.9237(6) 0.5493(4) -0.1395(5) 0.0281(10) Uani 1 1 d . . . O2 O 0.7350(6) 0.6805(4) -0.0855(5) 0.0310(10) Uani 1 1 d . . . O3 O 0.6342(7) 0.5700(4) -0.3148(6) 0.0386(12) Uani 1 1 d . . . O4 O 0.8439(6) 0.7172(4) -0.2921(5) 0.0304(10) Uani 1 1 d . . . O5 O 0.5688(5) 0.6114(4) 0.1297(5) 0.0228(9) Uani 1 1 d . . . O6 O 0.3007(5) 0.5632(3) -0.0164(4) 0.0188(8) Uani 1 1 d . . . O7 O 0.8263(6) 0.4577(5) 0.3455(5) 0.0352(12) Uani 1 1 d . . . O8 O 0.9196(6) 0.3881(4) 0.5811(5) 0.0275(10) Uani 1 1 d . . . O9 O 1.1326(6) 0.6913(3) 0.1364(5) 0.0236(9) Uani 1 1 d . . . H9A H 1.1010 0.7555 0.0945 0.035 Uiso 1 1 d R . . H9B H 1.1786 0.6522 0.0822 0.035 Uiso 1 1 d R . . C1 C 0.4639(7) 0.5504(5) 0.0337(6) 0.0163(10) Uani 1 1 d . . . C2 C 0.9259(8) 0.4562(5) 0.4786(6) 0.0212(11) Uani 1 1 d . . . N1 N 0.4510(8) 0.6631(5) -0.5962(6) 0.0338(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01246(16) 0.01469(16) 0.01904(15) -0.00065(10) 0.00330(10) 0.00005(10) S1 0.0134(6) 0.0144(6) 0.0143(5) 0.0022(4) 0.0022(5) 0.0012(5) O1 0.021(2) 0.021(2) 0.041(2) 0.0101(19) 0.0077(19) 0.0094(18) O2 0.038(3) 0.035(3) 0.022(2) 0.0000(18) 0.0124(19) 0.011(2) O3 0.030(3) 0.039(3) 0.034(2) -0.003(2) -0.008(2) -0.009(2) O4 0.035(3) 0.023(2) 0.036(2) 0.0113(19) 0.014(2) -0.0015(19) O5 0.018(2) 0.023(2) 0.029(2) -0.0100(17) 0.0093(17) -0.0041(17) O6 0.0128(18) 0.0189(19) 0.0237(19) -0.0019(15) 0.0045(15) 0.0023(15) O7 0.033(3) 0.049(3) 0.018(2) 0.002(2) 0.0005(18) -0.021(2) O8 0.030(2) 0.025(2) 0.024(2) 0.0042(17) 0.0038(18) -0.0089(19) O9 0.025(2) 0.0157(19) 0.035(2) 0.0033(17) 0.0163(18) 0.0033(16) C1 0.014(2) 0.018(3) 0.018(2) 0.002(2) 0.0065(19) -0.001(2) C2 0.024(3) 0.022(3) 0.017(2) -0.004(2) 0.006(2) -0.006(2) N1 0.031(3) 0.036(3) 0.031(3) -0.004(2) 0.005(2) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.342(4) 4_576 ? Eu1 O1 2.346(4) 3_765 ? Eu1 O6 2.431(4) 3_665 ? Eu1 O5 2.446(4) . ? Eu1 O9 2.452(4) . ? Eu1 O2 2.452(4) . ? Eu1 O7 2.455(5) . ? Eu1 O8 2.456(4) 3_766 ? Eu1 O1 2.965(5) . ? Eu1 C1 3.221(5) . ? Eu1 C1 3.240(5) 3_665 ? Eu1 C2 3.265(6) . ? S1 O3 1.449(5) . ? S1 O4 1.453(4) . ? S1 O2 1.471(4) . ? S1 O1 1.479(4) . ? O1 Eu1 2.346(4) 3_765 ? O4 Eu1 2.342(4) 4_575 ? O5 C1 1.245(7) . ? O6 C1 1.265(7) . ? O6 Eu1 2.431(4) 3_665 ? O7 C2 1.245(7) . ? O8 C2 1.258(7) . ? O8 Eu1 2.456(4) 3_766 ? C1 C1 1.541(11) 3_665 ? C1 Eu1 3.240(5) 3_665 ? C2 C2 1.536(11) 3_766 ? 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 Eu1 O1 144.77(17) 4_576 3_765 ? O4 Eu1 O6 137.36(15) 4_576 3_665 ? O1 Eu1 O6 75.00(15) 3_765 3_665 ? O4 Eu1 O5 75.20(15) 4_576 . ? O1 Eu1 O5 139.98(15) 3_765 . ? O6 Eu1 O5 66.49(13) 3_665 . ? O4 Eu1 O9 72.63(15) 4_576 . ? O1 Eu1 O9 73.34(15) 3_765 . ? O6 Eu1 O9 132.98(14) 3_665 . ? O5 Eu1 O9 143.25(14) . . ? O4 Eu1 O2 73.00(16) 4_576 . ? O1 Eu1 O2 111.07(15) 3_765 . ? O6 Eu1 O2 77.61(15) 3_665 . ? O5 Eu1 O2 71.52(15) . . ? O9 Eu1 O2 82.40(16) . . ? O4 Eu1 O7 115.09(17) 4_576 . ? O1 Eu1 O7 83.64(17) 3_765 . ? O6 Eu1 O7 73.17(14) 3_665 . ? O5 Eu1 O7 75.44(16) . . ? O9 Eu1 O7 135.07(15) . . ? O2 Eu1 O7 142.44(16) . . ? O4 Eu1 O8 78.26(16) 4_576 3_766 ? O1 Eu1 O8 83.78(16) 3_765 3_766 ? O6 Eu1 O8 135.40(14) 3_665 3_766 ? O5 Eu1 O8 116.39(15) . 3_766 ? O9 Eu1 O8 73.69(14) . 3_766 ? O2 Eu1 O8 146.99(15) . 3_766 ? O7 Eu1 O8 65.74(14) . 3_766 ? O4 Eu1 O1 113.09(14) 4_576 . ? O1 Eu1 O1 61.05(16) 3_765 . ? O6 Eu1 O1 65.98(13) 3_665 . ? O5 Eu1 O1 109.66(13) . . ? O9 Eu1 O1 68.51(14) . . ? O2 Eu1 O1 50.02(13) . . ? O7 Eu1 O1 131.05(15) . . ? O8 Eu1 O1 133.92(14) 3_766 . ? O4 Eu1 C1 92.12(15) 4_576 . ? O1 Eu1 C1 122.05(15) 3_765 . ? O6 Eu1 C1 47.22(13) 3_665 . ? O5 Eu1 C1 20.00(13) . . ? O9 Eu1 C1 147.88(14) . . ? O2 Eu1 C1 65.95(15) . . ? O7 Eu1 C1 76.89(15) . . ? O8 Eu1 C1 131.86(14) 3_766 . ? O1 Eu1 C1 93.42(13) . . ? O4 Eu1 C1 117.83(15) 4_576 3_665 ? O1 Eu1 C1 94.90(15) 3_765 3_665 ? O6 Eu1 C1 19.93(13) 3_665 3_665 ? O5 Eu1 C1 47.35(13) . 3_665 ? O9 Eu1 C1 142.45(13) . 3_665 ? O2 Eu1 C1 68.53(15) . 3_665 ? O7 Eu1 C1 76.12(14) . 3_665 ? O8 Eu1 C1 141.76(14) 3_766 3_665 ? O1 Eu1 C1 74.57(13) . 3_665 ? C1 Eu1 C1 27.59(19) . 3_665 ? O4 Eu1 C2 106.39(15) 4_576 . ? O1 Eu1 C2 81.43(15) 3_765 . ? O6 Eu1 C2 91.12(14) 3_665 . ? O5 Eu1 C2 88.67(15) . . ? O9 Eu1 C2 117.09(15) . . ? O2 Eu1 C2 159.80(16) . . ? O7 Eu1 C2 19.22(14) . . ? O8 Eu1 C2 46.57(14) 3_766 . ? O1 Eu1 C2 139.44(13) . . ? C1 Eu1 C2 94.07(14) . . ? C1 Eu1 C2 95.33(13) 3_665 . ? O3 S1 O4 110.7(3) . . ? O3 S1 O2 111.1(3) . . ? O4 S1 O2 109.9(3) . . ? O3 S1 O1 110.6(3) . . ? O4 S1 O1 109.6(3) . . ? O2 S1 O1 104.8(3) . . ? O3 S1 Eu1 119.4(2) . . ? O4 S1 Eu1 128.7(2) . . ? O2 S1 Eu1 42.33(18) . . ? O1 S1 Eu1 62.89(19) . . ? S1 O1 Eu1 149.9(3) . 3_765 ? S1 O1 Eu1 90.7(2) . . ? Eu1 O1 Eu1 118.95(16) 3_765 . ? S1 O2 Eu1 113.8(2) . . ? S1 O4 Eu1 149.7(3) . 4_575 ? C1 O5 Eu1 117.8(3) . . ? C1 O6 Eu1 119.1(3) . 3_665 ? C2 O7 Eu1 120.3(4) . . ? C2 O8 Eu1 120.0(4) . 3_766 ? O5 C1 O6 126.3(5) . . ? O5 C1 C1 118.2(6) . 3_665 ? O6 C1 C1 115.4(6) . 3_665 ? O5 C1 Eu1 42.2(3) . . ? O6 C1 Eu1 164.9(4) . . ? C1 C1 Eu1 76.9(4) 3_665 . ? O5 C1 Eu1 164.0(4) . 3_665 ? O6 C1 Eu1 40.9(3) . 3_665 ? C1 C1 Eu1 75.5(4) 3_665 3_665 ? Eu1 C1 Eu1 152.41(19) . 3_665 ? O7 C2 O8 126.3(6) . . ? O7 C2 C2 117.1(6) . 3_766 ? O8 C2 C2 116.5(6) . 3_766 ? O7 C2 Eu1 40.5(3) . . ? O8 C2 Eu1 166.4(4) . . ? C2 C2 Eu1 76.7(4) 3_766 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.856 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.161 #===END=============================================================== data_Gd4 _database_code_depnum_ccdc_archive 'CCDC 708581' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Gd(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 Gd N O9 S' _chemical_formula_weight 377.39 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0845(7) _cell_length_b 11.75440(10) _cell_length_c 9.33230(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.8460(10) _cell_angle_gamma 90.00 _cell_volume 839.29(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9028 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 34.96 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 8.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859507 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 16969 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2031 _reflns_number_gt 1946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+7.3680P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2031 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.400 _refine_ls_restrained_S_all 1.400 _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 0.87722(4) 0.09095(3) 0.16291(4) 0.01572(15) Uani 1 1 d . . . S1 S 0.7818(2) 0.12840(13) -0.21251(18) 0.0137(3) Uani 1 1 d . . . O1 O 0.9254(7) 0.0477(5) -0.1442(7) 0.0287(12) Uani 1 1 d . . . O2 O 0.7384(8) 0.1777(5) -0.0840(6) 0.0289(12) Uani 1 1 d . . . O3 O 0.6322(8) 0.0698(6) -0.3142(8) 0.0368(15) Uani 1 1 d . . . O4 O 0.8432(8) 0.2169(5) -0.2914(7) 0.0292(12) Uani 1 1 d . . . O5 O 0.5674(7) 0.1119(4) 0.1296(6) 0.0217(11) Uani 1 1 d . . . O6 O 0.2984(6) 0.0618(4) -0.0178(6) 0.0182(10) Uani 1 1 d . . . O7 O 0.8227(8) -0.0399(6) 0.3455(6) 0.0335(14) Uani 1 1 d . . . O8 O 0.9211(8) -0.1132(5) 0.5791(6) 0.0268(12) Uani 1 1 d . . . O9 O 1.1305(7) 0.1905(4) 0.1360(6) 0.0226(11) Uani 1 1 d . . . H9A H 1.0990 0.2303 0.0556 0.034 Uiso 1 1 d R . . H9B H 1.2065 0.1421 0.1308 0.034 Uiso 1 1 d R . . N1 N 0.4524(10) 0.1641(7) 0.4030(8) 0.0328(16) Uani 1 1 d . . . C1 C 0.4625(9) 0.0505(6) 0.0335(8) 0.0148(12) Uani 1 1 d . . . C2 C 0.9248(9) -0.0436(6) 0.4776(8) 0.0208(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0129(2) 0.0142(2) 0.0188(2) -0.00039(12) 0.00331(14) 0.00029(12) S1 0.0119(7) 0.0135(7) 0.0139(8) 0.0023(6) 0.0017(6) 0.0008(6) O1 0.019(3) 0.020(2) 0.042(3) 0.008(2) 0.003(2) 0.007(2) O2 0.036(3) 0.031(3) 0.021(3) 0.001(2) 0.012(3) 0.010(2) O3 0.027(3) 0.039(3) 0.034(3) -0.001(3) -0.006(3) -0.009(3) O4 0.033(3) 0.022(3) 0.035(3) 0.010(2) 0.015(3) -0.002(2) O5 0.016(2) 0.022(2) 0.027(3) -0.007(2) 0.007(2) -0.001(2) O6 0.011(2) 0.019(2) 0.022(3) -0.002(2) 0.001(2) 0.0024(18) O7 0.028(3) 0.047(4) 0.019(3) 0.003(3) -0.001(2) -0.020(3) O8 0.030(3) 0.025(3) 0.021(3) 0.006(2) 0.002(2) -0.008(2) O9 0.024(3) 0.016(2) 0.030(3) 0.004(2) 0.013(2) 0.005(2) N1 0.030(4) 0.039(4) 0.026(4) -0.007(3) 0.003(3) -0.009(3) C1 0.014(3) 0.016(3) 0.016(3) 0.003(3) 0.007(3) 0.002(2) C2 0.021(3) 0.021(3) 0.021(4) -0.005(3) 0.007(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.326(5) 3_755 ? Gd1 O4 2.331(5) 4_566 ? Gd1 O6 2.414(5) 3_655 ? Gd1 O5 2.434(5) . ? Gd1 O2 2.437(6) . ? Gd1 O7 2.440(6) . ? Gd1 O9 2.441(5) . ? Gd1 O8 2.447(6) 3_756 ? S1 O3 1.448(6) . ? S1 O4 1.452(5) . ? S1 O2 1.473(6) . ? S1 O1 1.475(5) . ? O1 Gd1 2.326(5) 3_755 ? O4 Gd1 2.331(5) 4_565 ? O5 C1 1.246(9) . ? O6 C1 1.264(8) . ? O6 Gd1 2.414(5) 3_655 ? O7 C2 1.243(10) . ? O8 C2 1.259(9) . ? O8 Gd1 2.447(6) 3_756 ? C1 C1 1.553(13) 3_655 ? C2 C2 1.542(14) 3_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O4 144.8(2) 3_755 4_566 ? O1 Gd1 O6 74.36(18) 3_755 3_655 ? O4 Gd1 O6 137.75(19) 4_566 3_655 ? O1 Gd1 O5 139.76(18) 3_755 . ? O4 Gd1 O5 75.42(19) 4_566 . ? O6 Gd1 O5 67.00(16) 3_655 . ? O1 Gd1 O2 109.9(2) 3_755 . ? O4 Gd1 O2 73.9(2) 4_566 . ? O6 Gd1 O2 76.88(19) 3_655 . ? O5 Gd1 O2 72.32(19) . . ? O1 Gd1 O7 83.9(2) 3_755 . ? O4 Gd1 O7 115.1(2) 4_566 . ? O6 Gd1 O7 73.54(18) 3_655 . ? O5 Gd1 O7 75.1(2) . . ? O2 Gd1 O7 142.4(2) . . ? O1 Gd1 O9 73.13(18) 3_755 . ? O4 Gd1 O9 72.94(18) 4_566 . ? O6 Gd1 O9 131.27(17) 3_655 . ? O5 Gd1 O9 143.23(17) . . ? O2 Gd1 O9 81.23(19) . . ? O7 Gd1 O9 136.16(19) . . ? O1 Gd1 O8 83.9(2) 3_755 3_756 ? O4 Gd1 O8 78.3(2) 4_566 3_756 ? O6 Gd1 O8 135.67(17) 3_655 3_756 ? O5 Gd1 O8 116.47(19) . 3_756 ? O2 Gd1 O8 147.44(19) . 3_756 ? O7 Gd1 O8 65.99(18) . 3_756 ? O9 Gd1 O8 74.68(18) . 3_756 ? O3 S1 O4 111.0(4) . . ? O3 S1 O2 110.6(4) . . ? O4 S1 O2 110.0(4) . . ? O3 S1 O1 110.6(4) . . ? O4 S1 O1 109.2(3) . . ? O2 S1 O1 105.2(3) . . ? S1 O1 Gd1 151.8(4) . 3_755 ? S1 O2 Gd1 116.6(3) . . ? S1 O4 Gd1 150.1(4) . 4_565 ? C1 O5 Gd1 117.8(4) . . ? C1 O6 Gd1 119.3(4) . 3_655 ? C2 O7 Gd1 120.2(5) . . ? C2 O8 Gd1 120.1(5) . 3_756 ? O5 C1 O6 126.8(6) . . ? O5 C1 C1 118.0(7) . 3_655 ? O6 C1 C1 115.2(7) . 3_655 ? O7 C2 O8 126.8(7) . . ? O7 C2 C2 117.3(8) . 3_756 ? O8 C2 C2 115.9(8) . 3_756 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.461 _refine_diff_density_min -1.383 _refine_diff_density_rms 0.181 #===END=============================================================== data_Gd5 _database_code_depnum_ccdc_archive 'CCDC 708582' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Gd(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 Gd N O9 S' _chemical_formula_weight 377.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5902(3) _cell_length_b 8.6100(4) _cell_length_c 13.8089(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.1330(10) _cell_angle_gamma 90.00 _cell_volume 782.37(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2319 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 30.52 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 8.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.662440 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5811 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.99 _reflns_number_total 1895 _reflns_number_gt 1611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.6929P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1895 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.24576(3) 0.24062(2) 0.910902(16) 0.00900(11) Uani 1 1 d . . . S1 S 0.23941(17) -0.16665(13) 0.97472(8) 0.0106(2) Uani 1 1 d . . . O1 O 0.2494(5) 0.0026(4) 0.9939(3) 0.0173(8) Uani 1 1 d . . . O2 O 0.4379(5) -0.2376(3) 1.0012(3) 0.0161(7) Uani 1 1 d . . . O3 O 0.1860(6) -0.1946(5) 0.8730(3) 0.0235(8) Uani 1 1 d . . . O4 O 0.0874(6) -0.2353(4) 1.0355(3) 0.0221(9) Uani 1 1 d . . . O5 O 0.4476(5) 0.4450(4) 0.8415(2) 0.0156(7) Uani 1 1 d . . . O6 O 0.0457(5) 0.4442(4) 0.8284(2) 0.0142(7) Uani 1 1 d . . . O7 O 0.0458(5) 0.6058(4) 0.7005(2) 0.0150(7) Uani 1 1 d . . . O8 O 0.4528(5) 0.6220(4) 0.7231(2) 0.0155(7) Uani 1 1 d . . . O9 O 0.2344(5) 0.4203(4) 1.0446(3) 0.0220(8) Uani 1 1 d . . . H9A H 0.2993 0.3821 1.0940 0.033 Uiso 1 1 d R . . H9B H 0.2889 0.5057 1.0293 0.033 Uiso 1 1 d R . . C1 C 0.3651(7) 0.5333(5) 0.7783(3) 0.0125(9) Uani 1 1 d . . . C2 C 0.1311(7) 0.5288(5) 0.7682(3) 0.0114(9) Uani 1 1 d . . . N1 N 0.7327(7) 0.3432(5) 0.6908(4) 0.0247(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.00837(14) 0.00870(14) 0.00990(15) -0.00002(8) 0.00020(9) -0.00003(8) S1 0.0083(5) 0.0104(5) 0.0130(6) 0.0014(4) -0.0004(4) -0.0003(4) O1 0.0202(18) 0.0098(15) 0.022(2) -0.0008(14) 0.0032(15) -0.0002(14) O2 0.0124(17) 0.0147(17) 0.021(2) -0.0006(13) -0.0033(15) 0.0048(13) O3 0.030(2) 0.0278(19) 0.0111(18) -0.0041(16) -0.0080(16) 0.0018(17) O4 0.020(2) 0.0167(18) 0.031(2) 0.0049(15) 0.0107(17) -0.0007(14) O5 0.0118(16) 0.0163(16) 0.0185(19) 0.0065(14) -0.0011(13) -0.0024(13) O6 0.0132(16) 0.0141(16) 0.0155(18) 0.0054(13) 0.0023(13) 0.0003(13) O7 0.0091(15) 0.0202(17) 0.0157(18) 0.0047(14) -0.0004(13) 0.0004(13) O8 0.0118(16) 0.0179(17) 0.0167(18) 0.0050(14) -0.0007(14) -0.0029(13) O9 0.0204(19) 0.0241(19) 0.021(2) -0.0061(16) -0.0039(15) 0.0010(15) C1 0.015(2) 0.013(2) 0.011(2) -0.0023(18) 0.0012(18) 0.0018(18) C2 0.012(2) 0.010(2) 0.012(2) 0.0005(17) 0.0019(18) 0.0023(17) N1 0.017(2) 0.024(2) 0.033(3) -0.003(2) -0.003(2) 0.0068(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.347(3) . ? Gd1 O2 2.355(4) 3_657 ? Gd1 O4 2.355(4) 3_557 ? Gd1 O9 2.414(3) . ? Gd1 O7 2.415(3) 2_546 ? Gd1 O8 2.432(3) 2_546 ? Gd1 O5 2.434(3) . ? Gd1 O6 2.438(3) . ? S1 O3 1.450(4) . ? S1 O4 1.466(4) . ? S1 O2 1.471(4) . ? S1 O1 1.482(3) . ? O2 Gd1 2.355(4) 3_657 ? O4 Gd1 2.355(4) 3_557 ? O5 C1 1.258(6) . ? O6 C2 1.261(5) . ? O7 C2 1.253(6) . ? O7 Gd1 2.415(3) 2_556 ? O8 C1 1.243(5) . ? O8 Gd1 2.432(3) 2_556 ? C1 C2 1.542(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O2 75.73(12) . 3_657 ? O1 Gd1 O4 79.31(12) . 3_557 ? O2 Gd1 O4 130.69(14) 3_657 3_557 ? O1 Gd1 O9 100.73(12) . . ? O2 Gd1 O9 71.09(12) 3_657 . ? O4 Gd1 O9 72.76(13) 3_557 . ? O1 Gd1 O7 84.29(11) . 2_546 ? O2 Gd1 O7 78.75(12) 3_657 2_546 ? O4 Gd1 O7 139.75(12) 3_557 2_546 ? O9 Gd1 O7 146.94(12) . 2_546 ? O1 Gd1 O8 89.75(12) . 2_546 ? O2 Gd1 O8 144.31(11) 3_657 2_546 ? O4 Gd1 O8 76.06(13) 3_557 2_546 ? O9 Gd1 O8 144.44(11) . 2_546 ? O7 Gd1 O8 67.32(11) 2_546 2_546 ? O1 Gd1 O5 146.32(11) . . ? O2 Gd1 O5 73.94(12) 3_657 . ? O4 Gd1 O5 132.58(11) 3_557 . ? O9 Gd1 O5 83.00(12) . . ? O7 Gd1 O5 75.79(11) 2_546 . ? O8 Gd1 O5 106.66(12) 2_546 . ? O1 Gd1 O6 147.85(11) . . ? O2 Gd1 O6 133.60(11) 3_657 . ? O4 Gd1 O6 70.81(12) 3_557 . ? O9 Gd1 O6 81.84(12) . . ? O7 Gd1 O6 111.08(11) 2_546 . ? O8 Gd1 O6 72.04(11) 2_546 . ? O5 Gd1 O6 65.76(11) . . ? O3 S1 O4 110.5(2) . . ? O3 S1 O2 109.7(2) . . ? O4 S1 O2 108.4(2) . . ? O3 S1 O1 110.0(2) . . ? O4 S1 O1 108.6(2) . . ? O2 S1 O1 109.5(2) . . ? S1 O1 Gd1 140.6(2) . . ? S1 O2 Gd1 151.9(2) . 3_657 ? S1 O4 Gd1 150.0(2) . 3_557 ? C1 O5 Gd1 119.0(3) . . ? C2 O6 Gd1 118.3(3) . . ? C2 O7 Gd1 118.8(3) . 2_556 ? C1 O8 Gd1 118.4(3) . 2_556 ? O8 C1 O5 126.8(5) . . ? O8 C1 C2 117.1(4) . . ? O5 C1 C2 116.1(4) . . ? O7 C2 O6 126.8(4) . . ? O7 C2 C1 117.4(4) . . ? O6 C2 C1 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.987 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.183 #===END=============================================================== data_Tb6 _database_code_depnum_ccdc_archive 'CCDC 708583' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Tb(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 N O9 S Tb' _chemical_formula_weight 379.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5786(3) _cell_length_b 8.6025(3) _cell_length_c 13.7919(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.0150(10) _cell_angle_gamma 90.00 _cell_volume 779.44(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5195 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 28.34 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 9.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.734703 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5740 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1931 _reflns_number_gt 1915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+3.4291P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0188(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1931 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.005 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 0.24568(2) 0.240422(16) 0.910547(10) 0.00726(8) Uani 1 1 d . . . S1 S 0.24003(10) -0.16655(8) 0.97480(5) 0.00837(15) Uani 1 1 d . . . O1 O 0.2491(4) 0.0032(3) 0.99337(17) 0.0155(5) Uani 1 1 d . . . O2 O 0.4386(4) -0.2376(3) 1.0019(2) 0.0162(5) Uani 1 1 d . . . O3 O 0.1869(4) -0.1958(3) 0.87239(18) 0.0222(5) Uani 1 1 d . . . O4 O 0.0858(4) -0.2358(3) 1.0358(2) 0.0210(6) Uani 1 1 d . . . O5 O 0.4475(4) 0.4443(3) 0.84116(17) 0.0151(5) Uani 1 1 d . . . O6 O 0.0446(3) 0.4437(3) 0.82790(17) 0.0138(4) Uani 1 1 d . . . O7 O 0.0458(3) 0.6054(3) 0.70034(16) 0.0137(4) Uani 1 1 d . . . O8 O 0.4539(3) 0.6214(3) 0.72188(17) 0.0152(5) Uani 1 1 d . . . O9 O 0.2363(4) 0.4209(3) 1.04350(18) 0.0186(5) Uani 1 1 d . . . H9A H 0.3016 0.3831 1.0928 0.028 Uiso 1 1 d R . . H9B H 0.2911 0.5061 1.0276 0.028 Uiso 1 1 d R . . C1 C 0.3646(5) 0.5328(4) 0.7779(2) 0.0105(5) Uani 1 1 d . . . C2 C 0.1307(5) 0.5280(4) 0.7681(2) 0.0108(5) Uani 1 1 d . . . N1 N 0.7328(5) 0.3410(4) 0.6908(2) 0.0229(6) 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 Tb1 0.00805(11) 0.00565(11) 0.00803(11) -0.00005(4) -0.00009(6) 0.00003(4) S1 0.0072(3) 0.0072(3) 0.0106(3) 0.0008(2) -0.0008(2) 0.0000(2) O1 0.0188(11) 0.0077(10) 0.0199(11) 0.0009(9) 0.0011(9) -0.0001(8) O2 0.0125(12) 0.0135(12) 0.0220(13) 0.0006(8) -0.0044(10) 0.0024(8) O3 0.0289(14) 0.0229(13) 0.0137(11) -0.0023(10) -0.0086(10) 0.0049(11) O4 0.0164(13) 0.0151(12) 0.0325(16) 0.0052(10) 0.0113(12) -0.0009(9) O5 0.0138(11) 0.0158(12) 0.0154(11) 0.0067(9) -0.0029(8) -0.0010(9) O6 0.0129(10) 0.0130(11) 0.0155(11) 0.0040(9) 0.0014(8) 0.0001(8) O7 0.0128(10) 0.0150(11) 0.0132(11) 0.0051(9) -0.0016(8) 0.0016(8) O8 0.0139(11) 0.0163(11) 0.0154(11) 0.0063(9) -0.0007(8) -0.0031(9) O9 0.0183(12) 0.0187(12) 0.0186(12) -0.0085(10) -0.0010(9) 0.0013(9) C1 0.0143(14) 0.0087(13) 0.0083(13) -0.0007(10) -0.0008(10) -0.0012(11) C2 0.0160(14) 0.0078(13) 0.0087(13) -0.0012(10) 0.0010(10) 0.0005(11) N1 0.0193(15) 0.0232(16) 0.0257(16) -0.0042(12) -0.0034(12) 0.0015(12) _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 2.339(3) 3_557 ? Tb1 O1 2.338(2) . ? Tb1 O2 2.347(3) 3_657 ? Tb1 O7 2.406(2) 2_546 ? Tb1 O9 2.406(2) . ? Tb1 O8 2.420(2) 2_546 ? Tb1 O5 2.426(2) . ? Tb1 O6 2.439(2) . ? S1 O3 1.459(3) . ? S1 O2 1.473(3) . ? S1 O4 1.478(3) . ? S1 O1 1.483(2) . ? O2 Tb1 2.347(3) 3_657 ? O4 Tb1 2.339(3) 3_557 ? O5 C1 1.260(4) . ? O6 C2 1.255(4) . ? O7 C2 1.254(4) . ? O7 Tb1 2.406(2) 2_556 ? O8 C1 1.253(4) . ? O8 Tb1 2.420(2) 2_556 ? C1 C2 1.538(4) . ? 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 O1 79.40(9) 3_557 . ? O4 Tb1 O2 130.66(11) 3_557 3_657 ? O1 Tb1 O2 75.77(8) . 3_657 ? O4 Tb1 O7 139.88(9) 3_557 2_546 ? O1 Tb1 O7 84.15(8) . 2_546 ? O2 Tb1 O7 78.67(9) 3_657 2_546 ? O4 Tb1 O9 73.04(9) 3_557 . ? O1 Tb1 O9 101.01(8) . . ? O2 Tb1 O9 70.85(9) 3_657 . ? O7 Tb1 O9 146.54(8) 2_546 . ? O4 Tb1 O8 75.73(10) 3_557 2_546 ? O1 Tb1 O8 89.45(8) . 2_546 ? O2 Tb1 O8 144.53(8) 3_657 2_546 ? O7 Tb1 O8 67.72(8) 2_546 2_546 ? O9 Tb1 O8 144.45(8) . 2_546 ? O4 Tb1 O5 132.48(8) 3_557 . ? O1 Tb1 O5 146.31(8) . . ? O2 Tb1 O5 73.89(8) 3_657 . ? O7 Tb1 O5 75.89(8) 2_546 . ? O9 Tb1 O5 82.57(9) . . ? O8 Tb1 O5 107.13(8) 2_546 . ? O4 Tb1 O6 70.63(9) 3_557 . ? O1 Tb1 O6 147.70(8) . . ? O2 Tb1 O6 133.73(8) 3_657 . ? O7 Tb1 O6 111.24(8) 2_546 . ? O9 Tb1 O6 81.86(8) . . ? O8 Tb1 O6 72.02(8) 2_546 . ? O5 Tb1 O6 65.92(8) . . ? O3 S1 O2 109.77(16) . . ? O3 S1 O4 110.21(18) . . ? O2 S1 O4 108.33(16) . . ? O3 S1 O1 110.01(15) . . ? O2 S1 O1 109.74(14) . . ? O4 S1 O1 108.74(15) . . ? S1 O1 Tb1 140.86(15) . . ? S1 O2 Tb1 152.13(15) . 3_657 ? S1 O4 Tb1 150.04(17) . 3_557 ? C1 O5 Tb1 118.9(2) . . ? C2 O6 Tb1 118.0(2) . . ? C2 O7 Tb1 118.9(2) . 2_556 ? C1 O8 Tb1 118.0(2) . 2_556 ? O5 C1 O8 126.5(3) . . ? O5 C1 C2 116.0(3) . . ? O8 C1 C2 117.5(3) . . ? O6 C2 O7 126.7(3) . . ? O6 C2 C1 116.2(3) . . ? O7 C2 C1 117.1(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.440 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.161 #===END=============================================================== data_Dy7 _database_code_depnum_ccdc_archive 'CCDC 708584' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Dy(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 Dy N O9 S' _chemical_formula_weight 382.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5535(3) _cell_length_b 8.5529(4) _cell_length_c 13.7537(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.9210(10) _cell_angle_gamma 90.00 _cell_volume 769.91(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4213 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 28.44 _exptl_crystal_description columnar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 10.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.514287 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5841 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.44 _reflns_number_total 1941 _reflns_number_gt 1855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+1.8460P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0072(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1941 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.24569(2) 0.240414(15) 0.910162(9) 0.00785(8) Uani 1 1 d . . . S1 S 0.24021(11) -0.16652(8) 0.97484(5) 0.00893(15) Uani 1 1 d . . . O1 O 0.2488(4) 0.0040(3) 0.99279(17) 0.0152(4) Uani 1 1 d . . . O2 O 0.4394(4) -0.2379(3) 1.0026(2) 0.0159(5) Uani 1 1 d . . . O3 O 0.1889(4) -0.1969(3) 0.87235(18) 0.0227(5) Uani 1 1 d . . . O4 O 0.0847(4) -0.2356(3) 1.0356(2) 0.0208(6) Uani 1 1 d . . . O5 O 0.4473(3) 0.4431(3) 0.84081(16) 0.0152(5) Uani 1 1 d . . . O6 O 0.0446(3) 0.4428(3) 0.82778(16) 0.0141(4) Uani 1 1 d . . . O7 O 0.0453(3) 0.6055(3) 0.70010(16) 0.0141(4) Uani 1 1 d . . . O8 O 0.4536(3) 0.6204(3) 0.72105(16) 0.0147(4) Uani 1 1 d . . . O9 O 0.2379(4) 0.4210(3) 1.04255(17) 0.0186(5) Uani 1 1 d . . . H9A H 0.1146 0.4372 1.0563 0.028 Uiso 1 1 d R . . H9B H 0.2923 0.5067 1.0263 0.028 Uiso 1 1 d R . . C1 C 0.3651(5) 0.5320(3) 0.7776(2) 0.0110(5) Uani 1 1 d . . . C2 C 0.1306(5) 0.5276(3) 0.7675(2) 0.0106(5) Uani 1 1 d . . . N1 N 0.7332(5) 0.3404(4) 0.6903(2) 0.0222(6) 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 Dy1 0.00723(11) 0.00777(10) 0.00849(10) -0.00002(4) -0.00029(6) 0.00006(4) S1 0.0064(3) 0.0095(3) 0.0107(3) 0.0009(2) -0.0010(2) 0.0000(2) O1 0.0172(11) 0.0085(10) 0.0199(11) 0.0019(8) 0.0003(9) -0.0004(8) O2 0.0094(12) 0.0164(12) 0.0214(13) -0.0001(8) -0.0038(10) 0.0026(8) O3 0.0296(14) 0.0227(13) 0.0148(11) -0.0025(10) -0.0088(10) 0.0045(11) O4 0.0143(13) 0.0153(12) 0.0338(16) 0.0054(9) 0.0102(12) -0.0009(8) O5 0.0121(10) 0.0176(11) 0.0155(11) 0.0058(9) -0.0035(8) -0.0013(9) O6 0.0114(10) 0.0150(11) 0.0161(11) 0.0050(8) 0.0019(8) -0.0006(9) O7 0.0114(10) 0.0170(11) 0.0137(10) 0.0048(8) -0.0024(8) 0.0010(9) O8 0.0113(10) 0.0172(11) 0.0154(11) 0.0056(9) -0.0009(8) -0.0038(9) O9 0.0147(11) 0.0199(12) 0.0211(12) -0.0087(9) 0.0001(9) 0.0008(9) C1 0.0120(13) 0.0103(13) 0.0106(13) -0.0013(11) -0.0015(10) -0.0011(11) C2 0.0125(14) 0.0093(13) 0.0101(13) -0.0017(10) 0.0014(11) -0.0004(11) N1 0.0169(14) 0.0268(16) 0.0226(15) -0.0036(12) -0.0019(12) 0.0021(12) _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 O1 2.319(2) . ? Dy1 O4 2.326(3) 3_557 ? Dy1 O2 2.334(3) 3_657 ? Dy1 O9 2.390(2) . ? Dy1 O7 2.391(2) 2_546 ? Dy1 O8 2.403(2) 2_546 ? Dy1 O5 2.406(2) . ? Dy1 O6 2.422(2) . ? S1 O3 1.456(3) . ? S1 O2 1.474(3) . ? S1 O4 1.474(3) . ? S1 O1 1.480(2) . ? O2 Dy1 2.334(3) 3_657 ? O4 Dy1 2.326(3) 3_557 ? O5 C1 1.255(4) . ? O6 C2 1.257(4) . ? O7 C2 1.250(4) . ? O7 Dy1 2.391(2) 2_556 ? O8 C1 1.249(4) . ? O8 Dy1 2.403(2) 2_556 ? C1 C2 1.536(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O4 79.20(8) . 3_557 ? O1 Dy1 O2 75.79(8) . 3_657 ? O4 Dy1 O2 130.41(11) 3_557 3_657 ? O1 Dy1 O9 100.95(8) . . ? O4 Dy1 O9 73.18(9) 3_557 . ? O2 Dy1 O9 70.56(8) 3_657 . ? O1 Dy1 O7 84.21(8) . 2_546 ? O4 Dy1 O7 140.12(9) 3_557 2_546 ? O2 Dy1 O7 78.55(8) 3_657 2_546 ? O9 Dy1 O7 146.11(8) . 2_546 ? O1 Dy1 O8 89.24(8) . 2_546 ? O4 Dy1 O8 75.77(9) 3_557 2_546 ? O2 Dy1 O8 144.54(8) 3_657 2_546 ? O9 Dy1 O8 144.69(8) . 2_546 ? O7 Dy1 O8 67.95(7) 2_546 2_546 ? O1 Dy1 O5 146.22(8) . . ? O4 Dy1 O5 132.73(8) 3_557 . ? O2 Dy1 O5 73.83(8) 3_657 . ? O9 Dy1 O5 82.53(8) . . ? O7 Dy1 O5 75.67(8) 2_546 . ? O8 Dy1 O5 107.36(8) 2_546 . ? O1 Dy1 O6 147.51(8) . . ? O4 Dy1 O6 70.69(8) 3_557 . ? O2 Dy1 O6 133.87(8) 3_657 . ? O9 Dy1 O6 82.08(8) . . ? O7 Dy1 O6 111.33(8) 2_546 . ? O8 Dy1 O6 72.05(8) 2_546 . ? O5 Dy1 O6 66.18(8) . . ? O3 S1 O2 109.56(16) . . ? O3 S1 O4 110.19(18) . . ? O2 S1 O4 108.40(16) . . ? O3 S1 O1 110.03(15) . . ? O2 S1 O1 109.83(14) . . ? O4 S1 O1 108.80(14) . . ? S1 O1 Dy1 141.10(14) . . ? S1 O2 Dy1 152.32(15) . 3_657 ? S1 O4 Dy1 150.52(17) . 3_557 ? C1 O5 Dy1 119.1(2) . . ? C2 O6 Dy1 117.99(19) . . ? C2 O7 Dy1 118.60(19) . 2_556 ? C1 O8 Dy1 118.32(19) . 2_556 ? O8 C1 O5 127.0(3) . . ? O8 C1 C2 116.9(3) . . ? O5 C1 C2 116.1(3) . . ? O7 C2 O6 126.7(3) . . ? O7 C2 C1 117.5(3) . . ? O6 C2 C1 115.8(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.036 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.167 #===END=============================================================== data_Er8 _database_code_depnum_ccdc_archive 'CCDC 708585' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Er(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 Er N O9 S' _chemical_formula_weight 387.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.4752(9) _cell_length_b 8.4502(12) _cell_length_c 13.627(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.028(3) _cell_angle_gamma 90.00 _cell_volume 744.56(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 831 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 23.42 _exptl_crystal_description columnar _exptl_crystal_colour light-pink _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 11.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653054 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5723 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 28.57 _reflns_number_total 1896 _reflns_number_gt 1357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1896 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.24576(6) 0.24042(4) 0.90952(3) 0.00975(16) Uani 1 1 d . . . S1 S 0.2418(3) -0.1668(2) 0.97529(17) 0.0106(5) Uani 1 1 d . . . O1 O 0.2514(9) 0.0066(7) 0.9922(5) 0.0144(14) Uani 1 1 d . . . O2 O 0.4411(9) -0.2369(7) 1.0042(5) 0.0180(14) Uani 1 1 d . . . O3 O 0.1938(11) -0.1980(8) 0.8719(5) 0.0246(16) Uani 1 1 d . . . O4 O 0.0849(9) -0.2349(7) 1.0357(5) 0.0213(15) Uani 1 1 d . . . O5 O 0.4491(9) 0.4423(7) 0.8402(5) 0.0152(14) Uani 1 1 d . . . O6 O 0.0455(9) 0.4417(7) 0.8274(5) 0.0143(14) Uani 1 1 d . . . O7 O 0.0456(10) 0.6049(7) 0.7000(5) 0.0135(14) Uani 1 1 d . . . O8 O 0.4528(10) 0.6179(7) 0.7194(5) 0.0172(15) Uani 1 1 d . . . O9 O 0.2369(11) 0.4210(8) 1.0403(5) 0.0223(16) Uani 1 1 d . . . H9A H 0.3037 0.3831 1.0903 0.033 Uiso 1 1 d R . . H9B H 0.2921 0.5076 1.0237 0.033 Uiso 1 1 d R . . C1 C 0.3615(14) 0.5300(10) 0.7754(8) 0.015(2) Uani 1 1 d . . . C2 C 0.1314(14) 0.5273(10) 0.7669(7) 0.0131(19) Uani 1 1 d . . . N1 N 0.7328(12) 0.3392(9) 0.6894(6) 0.0205(19) 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 0.0089(2) 0.0089(2) 0.0115(2) 0.00007(18) 0.00076(13) 0.00012(16) S1 0.0095(10) 0.0095(10) 0.0129(12) 0.0006(9) 0.0003(9) 0.0000(8) O1 0.019(3) 0.006(3) 0.018(4) 0.002(3) 0.000(3) 0.004(2) O2 0.008(3) 0.019(3) 0.027(4) -0.003(3) -0.003(3) 0.005(3) O3 0.027(4) 0.029(4) 0.016(4) -0.007(3) -0.010(3) -0.006(3) O4 0.013(3) 0.017(3) 0.035(4) 0.009(3) 0.012(3) -0.001(3) O5 0.011(3) 0.016(3) 0.018(4) 0.003(3) -0.003(3) -0.002(2) O6 0.013(3) 0.020(3) 0.011(3) 0.001(3) 0.005(3) -0.001(2) O7 0.015(3) 0.014(3) 0.011(3) 0.005(3) 0.004(3) 0.004(2) O8 0.014(3) 0.020(3) 0.018(4) 0.004(3) -0.001(3) -0.006(3) O9 0.027(4) 0.020(4) 0.020(4) -0.005(3) -0.002(3) 0.001(3) C1 0.013(5) 0.006(4) 0.028(6) -0.003(4) 0.003(4) -0.003(3) C2 0.017(5) 0.005(4) 0.018(5) -0.004(4) 0.008(4) -0.004(3) N1 0.015(4) 0.019(4) 0.028(5) -0.008(4) 0.002(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.274(6) . ? Er1 O2 2.290(6) 3_657 ? Er1 O4 2.305(6) 3_557 ? Er1 O9 2.349(6) . ? Er1 O8 2.361(7) 2_546 ? Er1 O7 2.361(6) 2_546 ? Er1 O5 2.380(6) . ? Er1 O6 2.382(6) . ? S1 O3 1.451(7) . ? S1 O2 1.455(6) . ? S1 O4 1.459(6) . ? S1 O1 1.484(6) . ? O2 Er1 2.290(6) 3_657 ? O4 Er1 2.305(6) 3_557 ? O5 C1 1.265(11) . ? O6 C2 1.249(10) . ? O7 C2 1.232(11) . ? O7 Er1 2.361(6) 2_556 ? O8 C1 1.237(10) . ? O8 Er1 2.361(7) 2_556 ? C1 C2 1.488(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O2 75.1(2) . 3_657 ? O1 Er1 O4 79.2(2) . 3_557 ? O2 Er1 O4 130.2(2) 3_657 3_557 ? O1 Er1 O9 100.9(2) . . ? O2 Er1 O9 71.1(2) 3_657 . ? O4 Er1 O9 73.0(2) 3_557 . ? O1 Er1 O8 88.9(2) . 2_546 ? O2 Er1 O8 144.0(2) 3_657 2_546 ? O4 Er1 O8 75.7(2) 3_557 2_546 ? O9 Er1 O8 144.6(2) . 2_546 ? O1 Er1 O7 84.1(2) . 2_546 ? O2 Er1 O7 78.3(2) 3_657 2_546 ? O4 Er1 O7 140.1(2) 3_557 2_546 ? O9 Er1 O7 146.3(2) . 2_546 ? O8 Er1 O7 67.9(2) 2_546 2_546 ? O1 Er1 O5 145.5(2) . . ? O2 Er1 O5 73.7(2) 3_657 . ? O4 Er1 O5 133.3(2) 3_557 . ? O9 Er1 O5 82.6(2) . . ? O8 Er1 O5 108.1(2) 2_546 . ? O7 Er1 O5 75.5(2) 2_546 . ? O1 Er1 O6 147.9(2) . . ? O2 Er1 O6 134.1(2) 3_657 . ? O4 Er1 O6 71.0(2) 3_557 . ? O9 Er1 O6 81.8(2) . . ? O8 Er1 O6 72.7(2) 2_546 . ? O7 Er1 O6 111.4(2) 2_546 . ? O5 Er1 O6 66.5(2) . . ? O3 S1 O2 109.3(4) . . ? O3 S1 O4 110.9(4) . . ? O2 S1 O4 108.7(4) . . ? O3 S1 O1 109.6(4) . . ? O2 S1 O1 109.3(4) . . ? O4 S1 O1 109.1(4) . . ? S1 O1 Er1 141.4(4) . . ? S1 O2 Er1 153.2(4) . 3_657 ? S1 O4 Er1 151.3(4) . 3_557 ? C1 O5 Er1 117.4(6) . . ? C2 O6 Er1 118.2(6) . . ? C2 O7 Er1 118.4(6) . 2_556 ? C1 O8 Er1 117.6(6) . 2_556 ? O8 C1 O5 124.8(9) . . ? O8 C1 C2 118.1(9) . . ? O5 C1 C2 117.1(8) . . ? O7 C2 O6 126.7(9) . . ? O7 C2 C1 117.4(8) . . ? O6 C2 C1 115.9(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.57 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.728 _refine_diff_density_min -1.708 _refine_diff_density_rms 0.337 #===END=============================================================== data_Yb9 _database_code_depnum_ccdc_archive 'CCDC 708586' _audit_creation_method SHELXL-97 _chemical_formula_moiety NH4[Yb(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H6 N O9 S Yb' _chemical_formula_weight 393.18 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.4884(5) _cell_length_b 8.4666(6) _cell_length_c 13.6830(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.6630(10) _cell_angle_gamma 90.00 _cell_volume 750.86(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2536 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 28.40 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 12.770 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.542923 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5701 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 28.49 _reflns_number_total 1904 _reflns_number_gt 1662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.8218P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1904 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.006 _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 Yb1 Yb 0.24567(3) 0.24019(3) 0.908906(18) 0.00911(12) Uani 1 1 d . . . S1 S 0.2414(2) -0.16651(16) 0.97457(10) 0.0099(3) Uani 1 1 d . . . O1 O 0.2480(6) 0.0069(5) 0.9901(3) 0.0158(9) Uani 1 1 d . . . O2 O 0.4412(7) -0.2372(5) 1.0047(4) 0.0171(9) Uani 1 1 d . . . O3 O 0.1947(8) -0.2001(6) 0.8719(4) 0.0228(10) Uani 1 1 d . . . O4 O 0.0819(7) -0.2350(5) 1.0350(4) 0.0212(11) Uani 1 1 d . . . O5 O 0.4490(7) 0.4406(5) 0.8392(3) 0.0160(9) Uani 1 1 d . . . O6 O 0.0427(6) 0.4399(5) 0.8270(3) 0.0156(9) Uani 1 1 d . . . O7 O 0.0441(6) 0.6049(5) 0.6997(3) 0.0151(9) Uani 1 1 d . . . O8 O 0.4559(6) 0.6175(5) 0.7182(3) 0.0149(9) Uani 1 1 d . . . O9 O 0.2380(7) 0.4233(6) 1.0377(3) 0.0215(10) Uani 1 1 d . . . H9A H 0.2055 0.3766 1.0888 0.032 Uiso 1 1 d R . . H9B H 0.3551 0.4663 1.0454 0.032 Uiso 1 1 d R . . C1 C 0.3661(9) 0.5293(7) 0.7754(4) 0.0129(11) Uani 1 1 d . . . C2 C 0.1303(9) 0.5251(7) 0.7666(4) 0.0128(11) Uani 1 1 d . . . N1 N 0.7349(8) 0.3359(7) 0.6890(4) 0.0231(12) 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 Yb1 0.00899(16) 0.00784(16) 0.01062(17) -0.00021(9) 0.00183(9) -0.00001(8) S1 0.0079(6) 0.0098(6) 0.0121(7) 0.0003(5) 0.0012(5) -0.0003(5) O1 0.017(2) 0.0094(19) 0.022(2) -0.0005(17) 0.0039(17) -0.0003(16) O2 0.010(2) 0.018(2) 0.023(2) -0.0025(18) -0.0033(18) 0.0011(16) O3 0.028(3) 0.022(2) 0.017(2) -0.003(2) -0.007(2) 0.004(2) O4 0.016(2) 0.015(2) 0.033(3) 0.0068(19) 0.014(2) -0.0012(16) O5 0.017(2) 0.015(2) 0.015(2) 0.0053(18) -0.0007(16) -0.0011(17) O6 0.0150(19) 0.015(2) 0.017(2) 0.0063(18) 0.0030(16) -0.0008(16) O7 0.0120(19) 0.019(2) 0.015(2) 0.0032(18) 0.0001(16) 0.0005(16) O8 0.015(2) 0.015(2) 0.014(2) 0.0038(17) 0.0010(17) -0.0043(16) O9 0.017(2) 0.024(2) 0.024(3) -0.010(2) 0.0021(18) 0.0021(18) C1 0.013(3) 0.012(3) 0.013(3) -0.005(2) 0.000(2) -0.001(2) C2 0.015(3) 0.010(3) 0.014(3) -0.002(2) 0.004(2) 0.001(2) N1 0.016(3) 0.025(3) 0.028(3) -0.001(3) -0.004(2) 0.002(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 Yb1 O4 2.294(5) 3_557 ? Yb1 O1 2.266(4) . ? Yb1 O2 2.303(5) 3_657 ? Yb1 O7 2.360(4) 2_546 ? Yb1 O9 2.350(4) . ? Yb1 O5 2.376(4) . ? Yb1 O8 2.367(4) 2_546 ? Yb1 O6 2.390(4) . ? Yb1 C2 3.148(6) 2_546 ? Yb1 C1 3.173(6) . ? Yb1 C1 3.147(6) 2_546 ? Yb1 C2 3.168(6) . ? S1 O3 1.451(5) . ? S1 O2 1.470(5) . ? S1 O4 1.473(5) . ? S1 O1 1.484(4) . ? O2 Yb1 2.303(5) 3_657 ? O4 Yb1 2.294(5) 3_557 ? O5 C1 1.254(7) . ? O6 C2 1.253(7) . ? O7 C2 1.249(7) . ? O7 Yb1 2.360(4) 2_556 ? O8 C1 1.246(7) . ? O8 Yb1 2.367(4) 2_556 ? C1 C2 1.529(8) . ? C1 Yb1 3.147(6) 2_556 ? C2 Yb1 3.148(6) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Yb1 O1 78.73(15) 3_557 . ? O4 Yb1 O2 129.60(18) 3_557 3_657 ? O1 Yb1 O2 75.72(15) . 3_657 ? O4 Yb1 O7 140.66(16) 3_557 2_546 ? O1 Yb1 O7 83.95(15) . 2_546 ? O2 Yb1 O7 78.21(16) 3_657 2_546 ? O4 Yb1 O9 73.10(17) 3_557 . ? O1 Yb1 O9 101.97(16) . . ? O2 Yb1 O9 70.80(16) 3_657 . ? O7 Yb1 O9 145.64(15) 2_546 . ? O4 Yb1 O5 133.50(15) 3_557 . ? O1 Yb1 O5 145.89(15) . . ? O2 Yb1 O5 73.76(16) 3_657 . ? O7 Yb1 O5 75.29(15) 2_546 . ? O9 Yb1 O5 82.02(16) . . ? O4 Yb1 O8 75.45(17) 3_557 2_546 ? O1 Yb1 O8 88.20(15) . 2_546 ? O2 Yb1 O8 144.73(15) 3_657 2_546 ? O7 Yb1 O8 68.91(14) 2_546 2_546 ? O9 Yb1 O8 144.16(15) . 2_546 ? O5 Yb1 O8 108.46(15) . 2_546 ? O4 Yb1 O6 70.82(15) 3_557 . ? O1 Yb1 O6 146.89(14) . . ? O2 Yb1 O6 134.60(15) 3_657 . ? O7 Yb1 O6 111.72(15) 2_546 . ? O9 Yb1 O6 81.65(16) . . ? O5 Yb1 O6 67.09(14) . . ? O8 Yb1 O6 72.08(15) 2_546 . ? O4 Yb1 C2 121.21(17) 3_557 2_546 ? O1 Yb1 C2 82.75(15) . 2_546 ? O2 Yb1 C2 97.72(16) 3_657 2_546 ? O7 Yb1 C2 20.48(15) 2_546 2_546 ? O9 Yb1 C2 165.68(15) . 2_546 ? O5 Yb1 C2 86.59(15) . 2_546 ? O8 Yb1 C2 48.52(15) 2_546 2_546 ? O6 Yb1 C2 101.89(15) . 2_546 ? O4 Yb1 C1 117.65(15) 3_557 . ? O1 Yb1 C1 163.40(14) . . ? O2 Yb1 C1 93.94(16) 3_657 . ? O7 Yb1 C1 81.20(15) 2_546 . ? O9 Yb1 C1 86.40(16) . . ? O5 Yb1 C1 20.30(15) . . ? O8 Yb1 C1 93.32(15) 2_546 . ? O6 Yb1 C1 47.89(14) . . ? C2 Yb1 C1 85.90(14) 2_546 . ? O4 Yb1 C1 94.30(17) 3_557 2_546 ? O1 Yb1 C1 83.93(15) . 2_546 ? O2 Yb1 C1 124.75(15) 3_657 2_546 ? O7 Yb1 C1 48.58(15) 2_546 2_546 ? O9 Yb1 C1 164.45(15) . 2_546 ? O5 Yb1 C1 101.26(15) . 2_546 ? O8 Yb1 C1 20.50(14) 2_546 2_546 ? O6 Yb1 C1 85.65(15) . 2_546 ? C2 Yb1 C1 28.12(15) 2_546 2_546 ? C1 Yb1 C1 91.72(6) . 2_546 ? O4 Yb1 C2 91.37(15) 3_557 . ? O1 Yb1 C2 163.98(16) . . ? O2 Yb1 C2 120.08(15) 3_657 . ? O7 Yb1 C2 96.31(15) 2_546 . ? O9 Yb1 C2 86.90(16) . . ? O5 Yb1 C2 47.88(15) . . ? O8 Yb1 C2 77.05(15) 2_546 . ? O6 Yb1 C2 20.56(14) . . ? C2 Yb1 C2 91.90(6) 2_546 . ? C1 Yb1 C2 27.91(15) . . ? C1 Yb1 C2 84.29(15) 2_546 . ? O3 S1 O2 109.5(3) . . ? O3 S1 O4 110.2(3) . . ? O2 S1 O4 108.4(3) . . ? O3 S1 O1 109.6(3) . . ? O2 S1 O1 110.1(2) . . ? O4 S1 O1 109.0(2) . . ? S1 O1 Yb1 142.5(3) . . ? S1 O2 Yb1 153.4(3) . 3_657 ? S1 O4 Yb1 151.8(3) . 3_557 ? C1 O5 Yb1 118.6(4) . . ? C2 O6 Yb1 117.4(4) . . ? C2 O7 Yb1 118.2(4) . 2_556 ? C1 O8 Yb1 117.8(4) . 2_556 ? O5 C1 O8 126.7(6) . . ? O5 C1 C2 115.9(5) . . ? O8 C1 C2 117.4(5) . . ? O5 C1 Yb1 41.1(3) . . ? O8 C1 Yb1 163.5(4) . . ? C2 C1 Yb1 75.8(3) . . ? O5 C1 Yb1 166.7(4) . 2_556 ? O8 C1 Yb1 41.7(3) . 2_556 ? C2 C1 Yb1 76.0(3) . 2_556 ? Yb1 C1 Yb1 147.7(2) . 2_556 ? O6 C2 O7 126.4(6) . . ? O6 C2 C1 116.4(5) . . ? O7 C2 C1 117.2(5) . . ? O6 C2 Yb1 167.4(4) . 2_556 ? O7 C2 Yb1 41.4(3) . 2_556 ? C1 C2 Yb1 75.9(3) . 2_556 ? O6 C2 Yb1 42.1(3) . . ? O7 C2 Yb1 161.3(4) . . ? C1 C2 Yb1 76.2(3) . . ? Yb1 C2 Yb1 147.97(19) 2_556 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.449 _refine_diff_density_min -1.915 _refine_diff_density_rms 0.256 #===END=============================================================== data_Gd10 _database_code_depnum_ccdc_archive 'CCDC 708587' _audit_creation_method SHELXL-97 _chemical_formula_moiety '[Gd(CH3CO2)(H2O)2(SO4)]' _chemical_formula_sum 'C2 H7 Gd O8 S' _chemical_formula_weight 348.39 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7281(3) _cell_length_b 6.8746(3) _cell_length_c 8.6645(4) _cell_angle_alpha 109.6850(10) _cell_angle_beta 90.7580(10) _cell_angle_gamma 107.5040(10) _cell_volume 356.93(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4078 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.17 _exptl_crystal_description quadrilateral-plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 326 _exptl_absorpt_coefficient_mu 9.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.500933 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 4259 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.17 _reflns_number_total 1736 _reflns_number_gt 1729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.9657P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0305(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1736 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0453 _refine_ls_wR_factor_gt 0.0452 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.11949(2) 0.34883(2) 0.130296(18) 0.00863(8) Uani 1 1 d . . . S1 S 0.29858(12) 0.40768(13) -0.24744(10) 0.00985(16) Uani 1 1 d . . . O1 O 0.2131(4) 0.2731(4) -0.1458(3) 0.0141(5) Uani 1 1 d . . . O2 O 0.1618(4) 0.5357(4) -0.2592(3) 0.0151(5) Uani 1 1 d . . . O3 O 0.3082(4) 0.2615(5) -0.4141(3) 0.0172(5) Uani 1 1 d . . . O4 O 0.5113(4) 0.5562(4) -0.1707(3) 0.0159(5) Uani 1 1 d . . . O5 O 0.1731(4) 0.6785(4) 0.0802(3) 0.0142(5) Uani 1 1 d . . . O6 O 0.1799(4) 0.9760(4) 0.0387(3) 0.0148(5) Uani 1 1 d . . . O7 O 0.0084(4) 0.1709(4) 0.3323(3) 0.0188(5) Uani 1 1 d . . . H7A H 0.1164 0.1789 0.3894 0.028 Uiso 1 1 d R . . H7B H -0.0655 0.0396 0.2830 0.028 Uiso 1 1 d R . . O8 O 0.2548(4) 0.6121(5) 0.4092(3) 0.0201(6) Uani 1 1 d . . . H8A H 0.1535 0.6269 0.4635 0.031 Uiso 1 1 d R . . H8B H 0.3341 0.5681 0.4567 0.031 Uiso 1 1 d R . . C1 C 0.2595(5) 0.8815(5) 0.1143(4) 0.0114(6) Uani 1 1 d . . . C2 C 0.4491(6) 1.0037(6) 0.2384(5) 0.0201(7) Uani 1 1 d . . . H2A H 0.4855 0.9058 0.2817 0.030 Uiso 1 1 d R . . H2B H 0.5637 1.0674 0.1870 0.030 Uiso 1 1 d R . . H2C H 0.4206 1.1171 0.3266 0.030 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 0.00831(10) 0.00907(11) 0.00845(10) 0.00335(6) 0.00070(6) 0.00249(6) S1 0.0086(3) 0.0118(4) 0.0097(4) 0.0040(3) 0.0013(3) 0.0038(3) O1 0.0165(12) 0.0151(12) 0.0136(11) 0.0079(10) 0.0048(9) 0.0059(9) O2 0.0133(11) 0.0193(13) 0.0177(12) 0.0092(10) 0.0044(9) 0.0090(10) O3 0.0187(12) 0.0226(13) 0.0097(11) 0.0024(10) 0.0011(9) 0.0095(10) O4 0.0086(11) 0.0172(12) 0.0193(12) 0.0052(10) -0.0004(9) 0.0022(9) O5 0.0150(11) 0.0127(11) 0.0147(12) 0.0054(9) 0.0016(9) 0.0038(9) O6 0.0148(11) 0.0130(11) 0.0171(12) 0.0060(10) -0.0006(9) 0.0047(9) O7 0.0212(13) 0.0190(13) 0.0176(12) 0.0096(10) 0.0003(10) 0.0053(10) O8 0.0146(12) 0.0243(14) 0.0137(12) 0.0019(10) 0.0008(10) 0.0011(10) C1 0.0129(15) 0.0111(15) 0.0114(14) 0.0037(12) 0.0038(12) 0.0058(12) C2 0.0183(17) 0.0172(17) 0.0216(18) 0.0062(14) -0.0072(14) 0.0027(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 Gd1 O4 2.359(2) 2_665 ? Gd1 O5 2.373(3) . ? Gd1 O1 2.406(2) . ? Gd1 O2 2.413(2) 2_565 ? Gd1 O8 2.439(3) . ? Gd1 O7 2.459(3) . ? Gd1 O6 2.490(3) 2_565 ? Gd1 O6 2.575(3) 1_545 ? Gd1 O5 2.586(3) 2_565 ? Gd1 C1 2.944(3) 2_565 ? S1 O3 1.470(3) . ? S1 O4 1.474(3) . ? S1 O2 1.476(3) . ? S1 O1 1.484(2) . ? O2 Gd1 2.413(2) 2_565 ? O4 Gd1 2.359(2) 2_665 ? O5 C1 1.266(4) . ? O5 Gd1 2.586(3) 2_565 ? O6 C1 1.275(4) . ? O6 Gd1 2.490(3) 2_565 ? O6 Gd1 2.575(3) 1_565 ? C1 C2 1.483(5) . ? C1 Gd1 2.944(3) 2_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 O5 86.95(9) 2_665 . ? O4 Gd1 O1 76.61(9) 2_665 . ? O5 Gd1 O1 75.00(8) . . ? O4 Gd1 O2 140.32(9) 2_665 2_565 ? O5 Gd1 O2 79.10(9) . 2_565 ? O1 Gd1 O2 132.97(9) . 2_565 ? O4 Gd1 O8 70.34(9) 2_665 . ? O5 Gd1 O8 80.24(9) . . ? O1 Gd1 O8 139.39(9) . . ? O2 Gd1 O8 70.77(9) 2_565 . ? O4 Gd1 O7 102.68(9) 2_665 . ? O5 Gd1 O7 143.35(9) . . ? O1 Gd1 O7 141.51(9) . . ? O2 Gd1 O7 70.98(9) 2_565 . ? O8 Gd1 O7 70.38(9) . . ? O4 Gd1 O6 136.58(9) 2_665 2_565 ? O5 Gd1 O6 117.71(8) . 2_565 ? O1 Gd1 O6 76.50(9) . 2_565 ? O2 Gd1 O6 81.96(9) 2_565 2_565 ? O8 Gd1 O6 144.08(9) . 2_565 ? O7 Gd1 O6 79.03(9) . 2_565 ? O4 Gd1 O6 76.72(9) 2_665 1_545 ? O5 Gd1 O6 146.27(8) . 1_545 ? O1 Gd1 O6 72.61(8) . 1_545 ? O2 Gd1 O6 131.23(8) 2_565 1_545 ? O8 Gd1 O6 119.97(9) . 1_545 ? O7 Gd1 O6 69.91(9) . 1_545 ? O6 Gd1 O6 63.00(10) 2_565 1_545 ? O4 Gd1 O5 139.35(9) 2_665 2_565 ? O5 Gd1 O5 67.15(10) . 2_565 ? O1 Gd1 O5 66.96(8) . 2_565 ? O2 Gd1 O5 66.97(8) 2_565 2_565 ? O8 Gd1 O5 130.20(9) . 2_565 ? O7 Gd1 O5 116.91(9) . 2_565 ? O6 Gd1 O5 50.82(8) 2_565 2_565 ? O6 Gd1 O5 107.50(8) 1_545 2_565 ? O4 Gd1 C1 145.02(9) 2_665 2_565 ? O5 Gd1 C1 92.43(9) . 2_565 ? O1 Gd1 C1 69.51(9) . 2_565 ? O2 Gd1 C1 73.17(9) 2_565 2_565 ? O8 Gd1 C1 143.93(9) . 2_565 ? O7 Gd1 C1 98.50(9) . 2_565 ? O6 Gd1 C1 25.39(9) 2_565 2_565 ? O6 Gd1 C1 84.98(9) 1_545 2_565 ? O5 Gd1 C1 25.44(9) 2_565 2_565 ? O3 S1 O4 109.69(15) . . ? O3 S1 O2 109.35(16) . . ? O4 S1 O2 109.73(15) . . ? O3 S1 O1 108.66(16) . . ? O4 S1 O1 109.10(15) . . ? O2 S1 O1 110.30(15) . . ? S1 O1 Gd1 134.83(15) . . ? S1 O2 Gd1 140.67(15) . 2_565 ? S1 O4 Gd1 153.62(17) . 2_665 ? C1 O5 Gd1 153.1(2) . . ? C1 O5 Gd1 93.3(2) . 2_565 ? Gd1 O5 Gd1 112.85(10) . 2_565 ? C1 O6 Gd1 97.7(2) . 2_565 ? C1 O6 Gd1 133.3(2) . 1_565 ? Gd1 O6 Gd1 117.00(10) 2_565 1_565 ? O5 C1 O6 118.2(3) . . ? O5 C1 C2 120.3(3) . . ? O6 C1 C2 121.5(3) . . ? O5 C1 Gd1 61.28(18) . 2_565 ? O6 C1 Gd1 56.95(17) . 2_565 ? C2 C1 Gd1 178.3(2) . 2_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.263 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.153 #===END=============================================================== data_KDy _database_code_depnum_ccdc_archive 'CCDC 708588' _audit_creation_method SHELXL-97 _chemical_formula_moiety K[Dy(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H2 Dy K O9 S' _chemical_formula_weight 403.70 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.6007(3) _cell_length_b 8.6186(4) _cell_length_c 13.8238(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.0830(10) _cell_angle_gamma 90.00 _cell_volume 785.28(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4816 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.31 _exptl_crystal_description columnar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 10.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.475558 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5825 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 28.11 _reflns_number_total 1897 _reflns_number_gt 1591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00079(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1897 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.022 _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 0.24545(3) 0.24027(2) 0.912215(15) 0.00927(9) Uani 1 1 d . . . K1 K -0.26909(18) 0.34341(15) 0.69807(9) 0.0289(3) Uani 1 1 d . . . S1 S 0.23559(17) -0.16430(13) 0.97620(8) 0.0113(2) Uani 1 1 d . . . O1 O 0.2449(5) 0.0063(4) 0.9971(3) 0.0166(7) Uani 1 1 d . . . O2 O 0.4386(5) -0.2363(4) 0.9984(3) 0.0177(8) Uani 1 1 d . . . O3 O 0.1697(6) -0.1895(5) 0.8730(3) 0.0240(8) Uani 1 1 d . . . O4 O 0.0898(5) -0.2366(4) 1.0411(3) 0.0206(8) Uani 1 1 d . . . O5 O 0.4480(5) 0.4435(4) 0.8438(2) 0.0155(7) Uani 1 1 d . . . O6 O 0.0455(5) 0.4448(4) 0.8275(2) 0.0156(7) Uani 1 1 d . . . O7 O 0.0450(5) 0.6083(4) 0.6989(2) 0.0160(7) Uani 1 1 d . . . O8 O 0.4567(5) 0.6237(4) 0.7243(2) 0.0155(7) Uani 1 1 d . . . O9 O 0.2351(5) 0.4086(4) 1.0514(2) 0.0198(8) Uani 1 1 d . . . H9B H 0.2436 0.5024 1.0331 0.030 Uiso 1 1 d R . . H9C H 0.1238 0.3952 1.0785 0.030 Uiso 1 1 d R . . C1 C 0.3665(7) 0.5347(5) 0.7797(3) 0.0113(9) Uani 1 1 d . . . C2 C 0.1310(7) 0.5303(5) 0.7677(3) 0.0126(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.00887(13) 0.00906(13) 0.00992(13) -0.00010(8) 0.00067(8) 0.00005(8) K1 0.0185(6) 0.0339(7) 0.0337(7) -0.0121(6) -0.0044(5) 0.0021(5) S1 0.0086(6) 0.0116(6) 0.0138(6) 0.0015(4) 0.0009(5) -0.0006(4) O1 0.0169(18) 0.0116(17) 0.0210(19) -0.0007(14) 0.0001(15) -0.0007(14) O2 0.0121(18) 0.0152(19) 0.026(2) 0.0010(14) -0.0014(15) 0.0024(13) O3 0.023(2) 0.030(2) 0.0186(19) -0.0009(17) -0.0089(16) 0.0011(17) O4 0.0139(18) 0.019(2) 0.030(2) 0.0047(15) 0.0104(16) 0.0003(14) O5 0.0125(17) 0.0160(18) 0.0179(18) 0.0052(14) 0.0003(14) 0.0005(14) O6 0.0130(18) 0.0154(18) 0.0184(18) 0.0074(14) 0.0019(14) 0.0000(13) O7 0.0125(17) 0.0200(19) 0.0156(17) 0.0038(14) 0.0026(14) 0.0027(14) O8 0.0126(18) 0.0151(18) 0.0187(18) 0.0056(14) -0.0004(14) -0.0043(13) O9 0.0155(19) 0.024(2) 0.0207(19) -0.0075(15) 0.0028(15) 0.0017(15) C1 0.014(2) 0.005(2) 0.015(2) -0.0019(18) 0.0003(19) -0.0007(17) C2 0.017(2) 0.010(2) 0.011(2) -0.0014(18) 0.0012(19) 0.0017(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.333(3) . ? Dy1 O4 2.339(4) 3_557 ? Dy1 O2 2.366(4) 3_657 ? Dy1 O7 2.407(3) 2_546 ? Dy1 O9 2.414(3) . ? Dy1 O5 2.426(3) . ? Dy1 O6 2.461(3) . ? Dy1 O8 2.466(3) 2_546 ? Dy1 K1 4.0231(13) 4_666 ? Dy1 K1 4.4730(13) . ? K1 O3 2.785(4) 2_456 ? K1 O6 2.807(3) . ? K1 O5 2.949(4) 1_455 ? K1 O8 2.958(3) 2_546 ? K1 O9 2.972(4) 4_565 ? K1 O8 3.052(4) 1_455 ? K1 O1 3.071(4) 4_565 ? K1 O7 3.084(4) . ? K1 O7 3.119(4) 2_446 ? K1 C1 3.173(5) 1_455 ? K1 C2 3.197(5) . ? K1 Dy1 4.0231(13) 4_565 ? S1 O3 1.485(4) . ? S1 O4 1.487(4) . ? S1 O2 1.494(3) . ? S1 O1 1.499(3) . ? O1 K1 3.071(4) 4_666 ? O2 Dy1 2.366(3) 3_657 ? O3 K1 2.785(4) 2_446 ? O4 Dy1 2.339(4) 3_557 ? O5 C1 1.281(5) . ? O5 K1 2.949(4) 1_655 ? O6 C2 1.263(5) . ? O7 C2 1.273(6) . ? O7 Dy1 2.407(3) 2_556 ? O7 K1 3.119(4) 2_456 ? O8 C1 1.256(5) . ? O8 Dy1 2.466(3) 2_556 ? O8 K1 2.958(3) 2_556 ? O8 K1 3.052(4) 1_655 ? O9 K1 2.972(4) 4_666 ? C1 C2 1.555(7) . ? C1 K1 3.173(5) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O4 79.77(12) . 3_557 ? O1 Dy1 O2 75.53(11) . 3_657 ? O4 Dy1 O2 132.54(13) 3_557 3_657 ? O1 Dy1 O7 85.94(12) . 2_546 ? O4 Dy1 O7 138.98(12) 3_557 2_546 ? O2 Dy1 O7 78.81(12) 3_657 2_546 ? O1 Dy1 O9 96.76(12) . . ? O4 Dy1 O9 73.75(12) 3_557 . ? O2 Dy1 O9 69.79(12) 3_657 . ? O7 Dy1 O9 146.58(11) 2_546 . ? O1 Dy1 O5 146.71(11) . . ? O4 Dy1 O5 131.83(11) 3_557 . ? O2 Dy1 O5 74.06(11) 3_657 . ? O7 Dy1 O5 75.21(11) 2_546 . ? O9 Dy1 O5 85.22(12) . . ? O1 Dy1 O6 147.47(11) . . ? O4 Dy1 O6 69.49(11) 3_557 . ? O2 Dy1 O6 133.95(11) 3_657 . ? O7 Dy1 O6 110.29(11) 2_546 . ? O9 Dy1 O6 84.90(12) . . ? O5 Dy1 O6 65.80(11) . . ? O1 Dy1 O8 91.00(11) . 2_546 ? O4 Dy1 O8 74.02(12) 3_557 2_546 ? O2 Dy1 O8 145.00(11) 3_657 2_546 ? O7 Dy1 O8 67.97(11) 2_546 2_546 ? O9 Dy1 O8 144.84(11) . 2_546 ? O5 Dy1 O8 106.41(11) . 2_546 ? O6 Dy1 O8 70.93(11) . 2_546 ? O1 Dy1 K1 49.48(9) . 4_666 ? O4 Dy1 K1 69.73(10) 3_557 4_666 ? O2 Dy1 K1 63.34(9) 3_657 4_666 ? O7 Dy1 K1 125.95(8) 2_546 4_666 ? O9 Dy1 K1 47.28(9) . 4_666 ? O5 Dy1 K1 123.72(8) . 4_666 ? O6 Dy1 K1 123.73(8) . 4_666 ? O8 Dy1 K1 129.66(8) 2_546 4_666 ? O1 Dy1 K1 118.87(8) . . ? O4 Dy1 K1 59.29(10) 3_557 . ? O2 Dy1 K1 164.78(9) 3_657 . ? O7 Dy1 K1 96.51(8) 2_546 . ? O9 Dy1 K1 110.79(8) . . ? O5 Dy1 K1 90.76(8) . . ? O6 Dy1 K1 34.30(8) . . ? O8 Dy1 K1 38.19(8) 2_546 . ? K1 Dy1 K1 128.92(3) 4_666 . ? O3 K1 O6 155.83(11) 2_456 . ? O3 K1 O5 69.31(10) 2_456 1_455 ? O6 K1 O5 86.98(10) . 1_455 ? O3 K1 O8 133.86(11) 2_456 2_546 ? O6 K1 O8 59.38(10) . 2_546 ? O5 K1 O8 113.21(10) 1_455 2_546 ? O3 K1 O9 74.24(11) 2_456 4_565 ? O6 K1 O9 128.96(10) . 4_565 ? O5 K1 O9 135.16(10) 1_455 4_565 ? O8 K1 O9 75.39(10) 2_546 4_565 ? O3 K1 O8 64.20(10) 2_456 1_455 ? O6 K1 O8 95.79(10) . 1_455 ? O5 K1 O8 44.43(9) 1_455 1_455 ? O8 K1 O8 150.44(6) 2_546 1_455 ? O9 K1 O8 133.38(10) 4_565 1_455 ? O3 K1 O1 78.33(10) 2_456 4_565 ? O6 K1 O1 112.85(10) . 4_565 ? O5 K1 O1 123.07(10) 1_455 4_565 ? O8 K1 O1 122.94(10) 2_546 4_565 ? O9 K1 O1 71.90(9) 4_565 4_565 ? O8 K1 O1 79.66(9) 1_455 4_565 ? O3 K1 O7 134.59(11) 2_456 . ? O6 K1 O7 45.00(9) . . ? O5 K1 O7 103.38(10) 1_455 . ? O8 K1 O7 90.98(9) 2_546 . ? O9 K1 O7 120.85(10) 4_565 . ? O8 K1 O7 79.42(9) 1_455 . ? O1 K1 O7 68.80(9) 4_565 . ? O3 K1 O7 61.87(10) 2_456 2_446 ? O6 K1 O7 109.95(10) . 2_446 ? O5 K1 O7 58.07(10) 1_455 2_446 ? O8 K1 O7 80.30(10) 2_546 2_446 ? O9 K1 O7 82.17(9) 4_565 2_446 ? O8 K1 O7 95.47(9) 1_455 2_446 ? O1 K1 O7 137.19(10) 4_565 2_446 ? O7 K1 O7 152.65(5) . 2_446 ? O3 K1 C1 56.98(12) 2_456 1_455 ? O6 K1 C1 99.23(11) . 1_455 ? O5 K1 C1 23.80(10) 1_455 1_455 ? O8 K1 C1 136.93(11) 2_546 1_455 ? O9 K1 C1 131.09(11) 4_565 1_455 ? O8 K1 C1 23.18(10) 1_455 1_455 ? O1 K1 C1 99.37(11) 4_565 1_455 ? O7 K1 C1 97.83(11) . 1_455 ? O7 K1 C1 72.71(11) 2_446 1_455 ? O3 K1 C2 155.58(13) 2_456 . ? O6 K1 C2 23.13(10) . . ? O5 K1 C2 100.96(11) 1_455 . ? O8 K1 C2 70.42(11) 2_546 . ? O9 K1 C2 122.40(11) 4_565 . ? O8 K1 C2 92.91(11) 1_455 . ? O1 K1 C2 89.74(11) 4_565 . ? O7 K1 C2 23.30(10) . . ? O7 K1 C2 133.07(11) 2_446 . ? C1 K1 C2 105.11(12) 1_455 . ? O3 K1 Dy1 72.99(8) 2_456 4_565 ? O6 K1 Dy1 128.77(8) . 4_565 ? O5 K1 Dy1 140.62(7) 1_455 4_565 ? O8 K1 Dy1 100.87(7) 2_546 4_565 ? O9 K1 Dy1 36.63(7) 4_565 4_565 ? O8 K1 Dy1 107.72(7) 1_455 4_565 ? O1 K1 Dy1 35.27(6) 4_565 4_565 ? O7 K1 Dy1 94.87(7) . 4_565 ? O7 K1 Dy1 112.17(7) 2_446 4_565 ? C1 K1 Dy1 120.07(9) 1_455 4_565 ? C2 K1 Dy1 108.85(9) . 4_565 ? O3 S1 O4 110.6(2) . . ? O3 S1 O2 110.5(2) . . ? O4 S1 O2 107.7(2) . . ? O3 S1 O1 109.6(2) . . ? O4 S1 O1 108.4(2) . . ? O2 S1 O1 109.9(2) . . ? S1 O1 Dy1 138.8(2) . . ? S1 O1 K1 125.79(18) . 4_666 ? Dy1 O1 K1 95.24(11) . 4_666 ? S1 O2 Dy1 150.4(2) . 3_657 ? S1 O3 K1 123.2(2) . 2_446 ? S1 O4 Dy1 145.6(2) . 3_557 ? C1 O5 Dy1 119.6(3) . . ? C1 O5 K1 88.0(3) . 1_655 ? Dy1 O5 K1 115.97(13) . 1_655 ? C2 O6 Dy1 118.8(3) . . ? C2 O6 K1 96.1(3) . . ? Dy1 O6 K1 116.09(13) . . ? C2 O7 Dy1 118.6(3) . 2_556 ? C2 O7 K1 83.4(3) . . ? Dy1 O7 K1 139.17(14) 2_556 . ? C2 O7 K1 104.5(3) . 2_456 ? Dy1 O7 K1 110.74(12) 2_556 2_456 ? K1 O7 K1 94.22(9) . 2_456 ? C1 O8 Dy1 117.4(3) . 2_556 ? C1 O8 K1 120.9(3) . 2_556 ? Dy1 O8 K1 110.79(11) 2_556 2_556 ? C1 O8 K1 83.8(3) . 1_655 ? Dy1 O8 K1 122.10(13) 2_556 1_655 ? K1 O8 K1 98.25(9) 2_556 1_655 ? Dy1 O9 K1 96.09(12) . 4_666 ? O8 C1 O5 127.0(4) . . ? O8 C1 C2 117.0(4) . . ? O5 C1 C2 116.0(4) . . ? O8 C1 K1 73.0(3) . 1_655 ? O5 C1 K1 68.2(2) . 1_655 ? C2 C1 K1 136.2(3) . 1_655 ? O6 C2 O7 126.9(4) . . ? O6 C2 C1 115.1(4) . . ? O7 C2 C1 118.0(4) . . ? O6 C2 K1 60.8(2) . . ? O7 C2 K1 73.3(3) . . ? C1 C2 K1 148.1(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.961 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.190 #===END=============================================================== data_CsDy _database_code_depnum_ccdc_archive 'CCDC 708589' _audit_creation_method SHELXL-97 _chemical_formula_moiety Cs[Dy(SO4)(H2O)(C2O4)] _chemical_formula_sum 'C2 H2 Cs Dy O9 S' _chemical_formula_weight 497.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cs Cs -0.3680 2.1192 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1421(7) _cell_length_b 11.9078(10) _cell_length_c 9.3459(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.7910(10) _cell_angle_gamma 90.00 _cell_volume 862.79(13) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5151 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.42 _exptl_crystal_description plate _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 13.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723525 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 6583 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.42 _reflns_number_total 2166 _reflns_number_gt 2105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0072(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2166 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _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 Dy1 Dy 0.36697(2) 0.091526(14) 0.17346(2) 0.01050(13) Uani 1 1 d . . . Cs1 Cs -0.05489(4) 0.32366(3) -0.09275(4) 0.02484(14) Uani 1 1 d . . . S1 S 0.29306(12) 0.12267(8) -0.21176(10) 0.0103(2) Uani 1 1 d . . . O1 O 0.2619(5) 0.1620(3) -0.0730(4) 0.0214(7) Uani 1 1 d . . . O2 O 0.4452(4) 0.0478(3) -0.1680(4) 0.0259(8) Uani 1 1 d . . . O3 O 0.1447(5) 0.0636(4) -0.3069(5) 0.0311(8) Uani 1 1 d . . . O4 O 0.3327(5) 0.2205(3) -0.2913(4) 0.0246(7) Uani 1 1 d . . . O5 O 0.2000(4) -0.0606(3) 0.0233(4) 0.0172(6) Uani 1 1 d . . . O6 O -0.0595(4) -0.1120(3) -0.1264(4) 0.0156(6) Uani 1 1 d . . . O7 O 0.5662(5) 0.1185(3) 0.4243(4) 0.0203(6) Uani 1 1 d . . . O8 O 0.6905(4) 0.0296(3) 0.6419(4) 0.0249(7) Uani 1 1 d . . . O9 O 0.6136(4) 0.1833(3) 0.1253(4) 0.0191(6) Uani 1 1 d . . . H9A H 0.7047 0.1476 0.1704 0.029 Uiso 1 1 d R . . H9B H 0.5988 0.1839 0.0318 0.029 Uiso 1 1 d R . . C1 C 0.0406(5) -0.0490(3) -0.0301(5) 0.0141(8) Uani 1 1 d . . . C2 C 0.5749(5) 0.0431(4) 0.5199(5) 0.0161(8) 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 Dy1 0.01115(17) 0.00833(16) 0.01126(16) -0.00016(5) 0.00227(10) 0.00094(5) Cs1 0.0253(2) 0.0242(2) 0.0232(2) 0.00664(11) 0.00475(14) 0.00704(10) S1 0.0119(4) 0.0080(4) 0.0102(4) 0.0007(3) 0.0019(3) 0.0000(3) O1 0.0282(17) 0.0249(17) 0.0133(15) 0.0020(12) 0.0095(13) 0.0093(13) O2 0.0227(16) 0.0185(17) 0.032(2) -0.0014(14) 0.0025(14) 0.0134(13) O3 0.031(2) 0.0274(18) 0.027(2) -0.0051(16) -0.0034(16) -0.0143(16) O4 0.0365(19) 0.0145(16) 0.0265(17) 0.0085(13) 0.0151(15) -0.0016(13) O5 0.0130(13) 0.0157(14) 0.0212(16) -0.0065(13) 0.0027(11) 0.0007(11) O6 0.0151(15) 0.0151(14) 0.0166(15) -0.0014(12) 0.0051(12) -0.0015(11) O7 0.0256(16) 0.0190(15) 0.0133(15) 0.0023(13) 0.0016(12) -0.0080(13) O8 0.0232(16) 0.0308(18) 0.0174(16) 0.0065(13) 0.0014(13) -0.0123(14) O9 0.0169(14) 0.0182(16) 0.0238(17) -0.0005(12) 0.0085(13) 0.0025(11) C1 0.0157(18) 0.0116(19) 0.0178(19) 0.0034(15) 0.0093(15) 0.0009(14) C2 0.0173(19) 0.0144(19) 0.0143(19) 0.0004(15) 0.0015(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 O2 2.267(3) 3_655 ? Dy1 O4 2.291(3) 4_566 ? Dy1 O1 2.353(3) . ? Dy1 O8 2.403(3) 3_656 ? Dy1 O6 2.418(3) 3 ? Dy1 O7 2.430(3) . ? Dy1 O5 2.436(3) . ? Dy1 O9 2.445(3) . ? Dy1 Cs1 4.5173(4) . ? Dy1 Cs1 4.6548(5) 4_666 ? Dy1 Cs1 4.7094(5) 4_566 ? Cs1 O3 2.987(4) 4_566 ? Cs1 O3 3.027(4) 2_554 ? Cs1 O6 3.136(3) 2_554 ? Cs1 O9 3.145(4) 4_465 ? Cs1 O1 3.178(3) . ? Cs1 O6 3.202(3) 3 ? Cs1 O7 3.212(3) 4_465 ? Cs1 C1 3.457(4) 3 ? Cs1 O5 3.479(3) 3 ? Cs1 O4 3.570(4) 4_566 ? Cs1 C2 3.828(4) 4_465 ? Cs1 S1 3.8664(10) 4_566 ? S1 O3 1.445(4) . ? S1 O4 1.470(3) . ? S1 O1 1.472(3) . ? S1 O2 1.479(3) . ? S1 Cs1 3.8664(10) 4_565 ? O2 Dy1 2.267(3) 3_655 ? O3 Cs1 2.987(4) 4_565 ? O3 Cs1 3.027(4) 2_544 ? O4 Dy1 2.291(3) 4_565 ? O4 Cs1 3.570(4) 4_565 ? O5 C1 1.248(5) . ? O5 Cs1 3.479(3) 3 ? O6 C1 1.261(6) . ? O6 Dy1 2.418(3) 3 ? O6 Cs1 3.136(3) 2_544 ? O6 Cs1 3.202(3) 3 ? O7 C2 1.254(6) . ? O7 Cs1 3.212(3) 4_666 ? O8 C2 1.247(6) . ? O8 Dy1 2.403(3) 3_656 ? O9 Cs1 3.145(4) 4_666 ? C1 C1 1.530(8) 3 ? C1 Cs1 3.457(4) 3 ? C1 Cs1 3.871(4) 2_544 ? C2 C2 1.550(8) 3_656 ? C2 Cs1 3.828(4) 4_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 O2 Dy1 O4 146.13(14) 3_655 4_566 ? O2 Dy1 O1 106.56(13) 3_655 . ? O4 Dy1 O1 76.64(13) 4_566 . ? O2 Dy1 O8 81.80(14) 3_655 3_656 ? O4 Dy1 O8 115.10(14) 4_566 3_656 ? O1 Dy1 O8 145.57(12) . 3_656 ? O2 Dy1 O6 137.52(12) 3_655 3 ? O4 Dy1 O6 76.31(12) 4_566 3 ? O1 Dy1 O6 74.91(12) . 3 ? O8 Dy1 O6 76.87(12) 3_656 3 ? O2 Dy1 O7 82.08(13) 3_655 . ? O4 Dy1 O7 78.86(13) 4_566 . ? O1 Dy1 O7 146.41(12) . . ? O8 Dy1 O7 66.77(11) 3_656 . ? O6 Dy1 O7 120.72(12) 3 . ? O2 Dy1 O5 72.82(12) 3_655 . ? O4 Dy1 O5 137.57(12) 4_566 . ? O1 Dy1 O5 74.27(13) . . ? O8 Dy1 O5 76.73(12) 3_656 . ? O6 Dy1 O5 66.77(10) 3 . ? O7 Dy1 O5 138.13(12) . . ? O2 Dy1 O9 74.08(12) 3_655 . ? O4 Dy1 O9 74.49(12) 4_566 . ? O1 Dy1 O9 74.58(12) . . ? O8 Dy1 O9 138.73(12) 3_656 . ? O6 Dy1 O9 141.65(11) 3 . ? O7 Dy1 O9 76.98(12) . . ? O5 Dy1 O9 124.85(11) . . ? O2 Dy1 Cs1 147.14(10) 3_655 . ? O4 Dy1 Cs1 51.41(10) 4_566 . ? O1 Dy1 Cs1 41.83(8) . . ? O8 Dy1 Cs1 118.74(9) 3_656 . ? O6 Dy1 Cs1 42.91(8) 3 . ? O7 Dy1 Cs1 128.43(9) . . ? O5 Dy1 Cs1 86.62(8) . . ? O9 Dy1 Cs1 98.86(8) . . ? O2 Dy1 Cs1 64.97(10) 3_655 4_666 ? O4 Dy1 Cs1 82.56(10) 4_566 4_666 ? O1 Dy1 Cs1 113.28(9) . 4_666 ? O8 Dy1 Cs1 100.61(8) 3_656 4_666 ? O6 Dy1 Cs1 154.93(8) 3 4_666 ? O7 Dy1 Cs1 40.29(8) . 4_666 ? O5 Dy1 Cs1 137.57(7) . 4_666 ? O9 Dy1 Cs1 38.74(8) . 4_666 ? Cs1 Dy1 Cs1 127.985(6) . 4_666 ? O2 Dy1 Cs1 139.45(10) 3_655 4_566 ? O4 Dy1 Cs1 65.53(9) 4_566 4_566 ? O1 Dy1 Cs1 106.21(8) . 4_566 ? O8 Dy1 Cs1 57.71(10) 3_656 4_566 ? O6 Dy1 Cs1 37.00(8) 3 4_566 ? O7 Dy1 Cs1 83.72(9) . 4_566 ? O5 Dy1 Cs1 93.96(7) . 4_566 ? O9 Dy1 Cs1 138.21(8) . 4_566 ? Cs1 Dy1 Cs1 65.460(7) . 4_566 ? Cs1 Dy1 Cs1 120.798(9) 4_666 4_566 ? O3 Cs1 O3 82.34(11) 4_566 2_554 ? O3 Cs1 O6 114.77(11) 4_566 2_554 ? O3 Cs1 O6 67.38(10) 2_554 2_554 ? O3 Cs1 O9 148.67(10) 4_566 4_465 ? O3 Cs1 O9 72.61(10) 2_554 4_465 ? O6 Cs1 O9 72.77(8) 2_554 4_465 ? O3 Cs1 O1 90.58(10) 4_566 . ? O3 Cs1 O1 134.82(10) 2_554 . ? O6 Cs1 O1 75.73(8) 2_554 . ? O9 Cs1 O1 120.41(9) 4_465 . ? O3 Cs1 O6 79.00(10) 4_566 3 ? O3 Cs1 O6 159.55(10) 2_554 3 ? O6 Cs1 O6 128.69(9) 2_554 3 ? O9 Cs1 O6 121.51(8) 4_465 3 ? O1 Cs1 O6 54.11(8) . 3 ? O3 Cs1 O7 97.33(10) 4_566 4_465 ? O3 Cs1 O7 70.62(11) 2_554 4_465 ? O6 Cs1 O7 121.63(8) 2_554 4_465 ? O9 Cs1 O7 57.01(8) 4_465 4_465 ? O1 Cs1 O7 154.38(10) . 4_465 ? O6 Cs1 O7 103.48(9) 3 4_465 ? O3 Cs1 C1 100.02(11) 4_566 3 ? O3 Cs1 C1 167.61(10) 2_554 3 ? O6 Cs1 C1 121.39(9) 2_554 3 ? O9 Cs1 C1 100.75(10) 4_465 3 ? O1 Cs1 C1 57.54(9) . 3 ? O6 Cs1 C1 21.38(10) 3 3 ? O7 Cs1 C1 96.99(9) 4_465 3 ? O3 Cs1 O5 111.14(10) 4_566 3 ? O3 Cs1 O5 147.61(10) 2_554 3 ? O6 Cs1 O5 125.52(8) 2_554 3 ? O9 Cs1 O5 83.05(8) 4_465 3 ? O1 Cs1 O5 76.09(8) . 3 ? O6 Cs1 O5 38.79(8) 3 3 ? O7 Cs1 O5 78.33(9) 4_465 3 ? C1 Cs1 O5 20.73(9) 3 3 ? O3 Cs1 O4 41.60(9) 4_566 4_566 ? O3 Cs1 O4 117.08(10) 2_554 4_566 ? O6 Cs1 O4 106.23(8) 2_554 4_566 ? O9 Cs1 O4 169.42(8) 4_465 4_566 ? O1 Cs1 O4 50.12(8) . 4_566 ? O6 Cs1 O4 50.56(8) 3 4_566 ? O7 Cs1 O4 128.57(8) 4_465 4_566 ? C1 Cs1 O4 70.51(9) 3 4_566 ? O5 Cs1 O4 89.35(8) 3 4_566 ? O3 Cs1 C2 80.02(10) 4_566 4_465 ? O3 Cs1 C2 63.76(11) 2_554 4_465 ? O6 Cs1 C2 126.09(9) 2_554 4_465 ? O9 Cs1 C2 72.24(9) 4_465 4_465 ? O1 Cs1 C2 158.19(9) . 4_465 ? O6 Cs1 C2 104.48(9) 3 4_465 ? O7 Cs1 C2 17.92(9) 4_465 4_465 ? C1 Cs1 C2 104.49(9) 3 4_465 ? O5 Cs1 C2 88.91(8) 3 4_465 ? O4 Cs1 C2 115.13(8) 4_566 4_465 ? O3 Cs1 S1 19.43(7) 4_566 4_566 ? O3 Cs1 S1 99.72(8) 2_554 4_566 ? O6 Cs1 S1 114.13(6) 2_554 4_566 ? O9 Cs1 S1 167.37(6) 4_465 4_566 ? O1 Cs1 S1 72.15(6) . 4_566 ? O6 Cs1 S1 63.44(6) 3 4_566 ? O7 Cs1 S1 111.32(6) 4_465 4_566 ? C1 Cs1 S1 84.82(8) 3 4_566 ? O5 Cs1 S1 99.91(6) 3 4_566 ? O4 Cs1 S1 22.35(5) 4_566 4_566 ? C2 Cs1 S1 95.46(7) 4_465 4_566 ? O3 S1 O4 110.2(2) . . ? O3 S1 O1 111.1(2) . . ? O4 S1 O1 108.5(2) . . ? O3 S1 O2 110.4(3) . . ? O4 S1 O2 108.8(2) . . ? O1 S1 O2 107.7(2) . . ? O3 S1 Cs1 43.44(17) . 4_565 ? O4 S1 Cs1 67.41(16) . 4_565 ? O1 S1 Cs1 118.93(14) . 4_565 ? O2 S1 Cs1 132.08(15) . 4_565 ? O3 S1 Cs1 86.22(19) . . ? O4 S1 Cs1 87.21(15) . . ? O1 S1 Cs1 42.11(13) . . ? O2 S1 Cs1 149.79(16) . . ? Cs1 S1 Cs1 77.374(19) 4_565 . ? S1 O1 Dy1 129.80(19) . . ? S1 O1 Cs1 119.79(17) . . ? Dy1 O1 Cs1 108.58(11) . . ? S1 O2 Dy1 161.6(2) . 3_655 ? S1 O3 Cs1 117.1(2) . 4_565 ? S1 O3 Cs1 136.7(3) . 2_544 ? Cs1 O3 Cs1 97.66(11) 4_565 2_544 ? S1 O4 Dy1 154.4(2) . 4_565 ? S1 O4 Cs1 90.24(17) . 4_565 ? Dy1 O4 Cs1 98.48(12) 4_565 4_565 ? C1 O5 Dy1 118.5(3) . . ? C1 O5 Cs1 78.7(2) . 3 ? Dy1 O5 Cs1 136.36(13) . 3 ? C1 O6 Dy1 118.5(3) . 3 ? C1 O6 Cs1 116.8(2) . 2_544 ? Dy1 O6 Cs1 115.36(12) 3 2_544 ? C1 O6 Cs1 90.8(3) . 3 ? Dy1 O6 Cs1 106.15(11) 3 3 ? Cs1 O6 Cs1 103.89(9) 2_544 3 ? C2 O7 Dy1 117.9(3) . . ? C2 O7 Cs1 110.1(3) . 4_666 ? Dy1 O7 Cs1 110.41(12) . 4_666 ? C2 O8 Dy1 118.4(3) . 3_656 ? Dy1 O9 Cs1 112.15(12) . 4_666 ? O5 C1 O6 125.9(4) . . ? O5 C1 C1 116.8(5) . 3 ? O6 C1 C1 117.3(5) . 3 ? O5 C1 Cs1 80.6(2) . 3 ? O6 C1 Cs1 67.8(2) . 3 ? C1 C1 Cs1 125.0(3) 3 3 ? O5 C1 Cs1 90.2(2) . 2_544 ? O6 C1 Cs1 46.3(2) . 2_544 ? C1 C1 Cs1 140.4(4) 3 2_544 ? Cs1 C1 Cs1 85.66(9) 3 2_544 ? O8 C2 O7 127.3(4) . . ? O8 C2 C2 117.0(5) . 3_656 ? O7 C2 C2 115.7(5) . 3_656 ? O8 C2 Cs1 82.3(2) . 4_666 ? O7 C2 Cs1 52.0(2) . 4_666 ? C2 C2 Cs1 146.8(4) 3_656 4_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.248 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.170 #===END===============================================================