Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Qingjin Meng' _publ_contact_author_address ; State Key Lab Nanjing University Coordination Chemistry Institute Nanjing 210093 CHINA ; _publ_contact_author_email MENGQJ@NJU.EDU.CN _publ_section_title ; Two Types of Novel Double Layer Framework Structures Assembled from 5-Sulfosalicylic Acid and Lanthanide Ions ; loop_ _publ_author_name 'Qingjin Meng.' 'Zhenda Lu.' 'Lili Wen.' 'Jing Yao.' 'Hui-Zhen Zhu.' # Attachment 'Dy1.cif' data_dy1 _database_code_depnum_ccdc_archive 'CCDC 618891' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 Dy O8 S, H2 O' _chemical_formula_sum 'C7 H9 Dy O9 S' _chemical_formula_weight 431.70 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' 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 8.7988(17) _cell_length_b 8.7709(17) _cell_length_c 14.151(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.771(4) _cell_angle_gamma 90.00 _cell_volume 1072.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 7.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.49 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5672 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2112 _reflns_number_gt 1751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0700P)^2^+1.7700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2112 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 C1 C 0.4658(9) 0.6672(9) -0.1457(6) 0.0290(18) Uani 1 1 d . . . C2 C 0.4496(10) 0.5215(10) -0.1889(6) 0.0316(18) Uani 1 1 d . . . C3 C 0.3537(10) 0.4181(10) -0.1532(6) 0.0331(19) Uani 1 1 d . . . H3A H 0.3372 0.3228 -0.1821 0.040 Uiso 1 1 calc R . . C4 C 0.2830(10) 0.4514(9) -0.0774(6) 0.0329(19) Uani 1 1 d . . . H4A H 0.2213 0.3791 -0.0548 0.039 Uiso 1 1 calc R . . C5 C 0.3041(10) 0.5942(11) -0.0346(6) 0.0352(19) Uani 1 1 d . . . C6 C 0.3932(10) 0.7006(11) -0.0689(6) 0.0347(19) Uani 1 1 d . . . H6A H 0.4055 0.7966 -0.0406 0.042 Uiso 1 1 calc R . . C7 C 0.5537(10) 0.7935(10) -0.1792(6) 0.0318(18) Uani 1 1 d . . . Dy1 Dy 0.26088(5) 0.95830(5) 0.21946(3) 0.03107(17) Uani 1 1 d . . . O1 O 0.5322(7) 0.9268(7) -0.1555(4) 0.0323(14) Uani 1 1 d . . . O2 O 0.6567(6) 0.7667(7) -0.2304(4) 0.0299(12) Uani 1 1 d . . . O3 O 0.5181(7) 0.4816(7) -0.2619(4) 0.0330(13) Uani 1 1 d . . . O4 O 0.2930(7) 0.7712(7) 0.1069(4) 0.0333(13) Uani 1 1 d . . . O5 O 0.1953(7) 0.5166(7) 0.1164(4) 0.0296(12) Uani 1 1 d . . . O6 O 0.0503(7) 0.6988(7) 0.0076(4) 0.0344(13) Uani 1 1 d . . . O7 O 0.4820(7) 0.8233(7) 0.2972(4) 0.0344(13) Uani 1 1 d . . . H7A H 0.4750 0.8082 0.3556 0.041 Uiso 1 1 d R . . H7B H 0.4878 0.7381 0.2695 0.041 Uiso 1 1 d R . . O8 O 0.1442(7) 1.0618(7) 0.0696(4) 0.0359(14) Uani 1 1 d . . . H8B H 0.2041 1.1287 0.0531 0.043 Uiso 1 1 d R . . H8C H 0.1292 0.9913 0.0277 0.043 Uiso 1 1 d R . . O9 O 0.2537(8) 0.0514(7) 0.9048(5) 0.0423(16) Uani 1 1 d . . . H9A H 0.1909 0.0972 0.8610 0.051 Uiso 1 1 d R . . H9B H 0.3413 0.0952 0.9128 0.051 Uiso 1 1 d R . . S1 S 0.2025(3) 0.6489(2) 0.05484(15) 0.0313(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(4) 0.028(4) 0.028(4) -0.004(3) -0.002(3) -0.009(3) C2 0.034(4) 0.028(4) 0.033(4) 0.005(4) 0.007(4) 0.006(4) C3 0.030(4) 0.031(4) 0.037(5) -0.005(4) 0.006(4) 0.003(3) C4 0.032(5) 0.031(5) 0.037(5) -0.001(4) 0.009(4) -0.008(4) C5 0.032(5) 0.036(5) 0.036(4) -0.006(4) 0.001(4) -0.001(4) C6 0.036(5) 0.032(5) 0.037(4) 0.000(4) 0.010(4) 0.003(4) C7 0.029(4) 0.031(4) 0.037(4) 0.000(4) 0.012(4) 0.001(3) Dy1 0.0354(3) 0.0283(2) 0.0296(2) -0.00054(17) 0.00622(16) -0.00072(16) O1 0.034(3) 0.034(3) 0.035(3) 0.004(2) 0.020(3) -0.001(2) O2 0.031(3) 0.030(3) 0.031(3) 0.003(2) 0.012(2) -0.002(2) O3 0.033(3) 0.033(3) 0.037(3) -0.004(3) 0.015(3) 0.000(3) O4 0.038(3) 0.031(3) 0.031(3) -0.003(3) 0.009(2) -0.004(3) O5 0.031(3) 0.031(3) 0.029(3) -0.002(2) 0.010(2) -0.002(2) O6 0.037(3) 0.032(3) 0.034(3) 0.001(3) 0.007(3) 0.004(3) O7 0.037(3) 0.033(3) 0.034(3) -0.005(3) 0.010(3) 0.003(3) O8 0.036(3) 0.035(3) 0.038(3) 0.001(3) 0.010(3) -0.002(3) O9 0.044(4) 0.050(4) 0.033(3) 0.001(3) 0.007(3) -0.004(3) S1 0.0361(11) 0.0295(11) 0.0285(10) -0.0002(8) 0.0063(8) 0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.391(12) . ? C1 C2 1.412(12) . ? C1 C7 1.479(11) . ? C2 O3 1.335(10) . ? C2 C3 1.396(12) . ? C3 C4 1.368(12) . ? C3 H3A 0.9300 . ? C4 C5 1.388(12) . ? C4 H4A 0.9300 . ? C5 C6 1.365(13) . ? C5 S1 1.748(9) . ? C6 H6A 0.9300 . ? C7 O1 1.240(10) . ? C7 O2 1.284(10) . ? C7 Dy1 2.841(9) 3_675 ? Dy1 O3 2.264(6) 4_576 ? Dy1 O5 2.338(6) 2 ? Dy1 O4 2.340(6) . ? Dy1 O2 2.342(6) 4_576 ? Dy1 O8 2.358(6) . ? Dy1 O7 2.366(6) . ? Dy1 O1 2.401(5) 3_675 ? Dy1 O2 2.515(6) 3_675 ? Dy1 C7 2.841(9) 3_675 ? O1 Dy1 2.401(5) 3_675 ? O2 Dy1 2.342(6) 4_675 ? O2 Dy1 2.515(6) 3_675 ? O3 Dy1 2.264(6) 4_675 ? O4 S1 1.453(6) . ? O5 S1 1.460(6) . ? O5 Dy1 2.338(6) 2_545 ? O6 S1 1.448(6) . ? O7 H7A 0.8499 . ? O7 H7B 0.8501 . ? O8 H8B 0.8499 . ? O8 H8C 0.8500 . ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 120.4(8) . . ? C6 C1 C7 115.9(8) . . ? C2 C1 C7 123.7(8) . . ? O3 C2 C3 120.0(8) . . ? O3 C2 C1 123.3(8) . . ? C3 C2 C1 116.7(8) . . ? C4 C3 C2 122.6(8) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 119.4(8) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 120.1(8) . . ? C6 C5 S1 118.4(7) . . ? C4 C5 S1 121.2(7) . . ? C5 C6 C1 120.8(8) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? O1 C7 O2 119.0(8) . . ? O1 C7 C1 120.3(7) . . ? O2 C7 C1 120.7(8) . . ? O1 C7 Dy1 56.9(4) . 3_675 ? O2 C7 Dy1 62.2(4) . 3_675 ? C1 C7 Dy1 173.0(6) . 3_675 ? O3 Dy1 O5 79.5(2) 4_576 2 ? O3 Dy1 O4 118.6(2) 4_576 . ? O5 Dy1 O4 144.2(2) 2 . ? O3 Dy1 O2 74.3(2) 4_576 4_576 ? O5 Dy1 O2 83.4(2) 2 4_576 ? O4 Dy1 O2 73.68(18) . 4_576 ? O3 Dy1 O8 75.7(2) 4_576 . ? O5 Dy1 O8 140.5(2) 2 . ? O4 Dy1 O8 75.3(2) . . ? O2 Dy1 O8 117.9(2) 4_576 . ? O3 Dy1 O7 140.8(2) 4_576 . ? O5 Dy1 O7 71.3(2) 2 . ? O4 Dy1 O7 76.8(2) . . ? O2 Dy1 O7 76.8(2) 4_576 . ? O8 Dy1 O7 142.4(2) . . ? O3 Dy1 O1 138.1(2) 4_576 3_675 ? O5 Dy1 O1 106.6(2) 2 3_675 ? O4 Dy1 O1 80.9(2) . 3_675 ? O2 Dy1 O1 146.7(2) 4_576 3_675 ? O8 Dy1 O1 74.5(2) . 3_675 ? O7 Dy1 O1 76.7(2) . 3_675 ? O3 Dy1 O2 92.1(2) 4_576 3_675 ? O5 Dy1 O2 74.75(19) 2 3_675 ? O4 Dy1 O2 130.11(18) . 3_675 ? O2 Dy1 O2 156.13(8) 4_576 3_675 ? O8 Dy1 O2 76.01(19) . 3_675 ? O7 Dy1 O2 104.40(19) . 3_675 ? O1 Dy1 O2 52.43(19) 3_675 3_675 ? O3 Dy1 C7 115.8(2) 4_576 3_675 ? O5 Dy1 C7 92.1(2) 2 3_675 ? O4 Dy1 C7 104.7(2) . 3_675 ? O2 Dy1 C7 168.1(2) 4_576 3_675 ? O8 Dy1 C7 72.2(2) . 3_675 ? O7 Dy1 C7 91.4(2) . 3_675 ? O1 Dy1 C7 25.6(2) 3_675 3_675 ? O2 Dy1 C7 26.9(2) 3_675 3_675 ? C7 O1 Dy1 97.4(5) . 3_675 ? C7 O2 Dy1 133.1(5) . 4_675 ? C7 O2 Dy1 90.9(5) . 3_675 ? Dy1 O2 Dy1 134.6(2) 4_675 3_675 ? C2 O3 Dy1 126.9(5) . 4_675 ? S1 O4 Dy1 137.6(4) . . ? S1 O5 Dy1 138.5(4) . 2_545 ? Dy1 O7 H7A 109.1 . . ? Dy1 O7 H7B 109.9 . . ? H7A O7 H7B 109.5 . . ? Dy1 O8 H8B 108.9 . . ? Dy1 O8 H8C 109.4 . . ? H8B O8 H8C 109.5 . . ? H9A O9 H9B 109.5 . . ? O6 S1 O4 112.5(4) . . ? O6 S1 O5 112.1(3) . . ? O4 S1 O5 111.4(3) . . ? O6 S1 C5 107.6(4) . . ? O4 S1 C5 105.3(4) . . ? O5 S1 C5 107.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.075 _refine_diff_density_min -2.308 _refine_diff_density_rms 0.218 # Attachment 'Eu1.cif' data_ff1 _database_code_depnum_ccdc_archive 'CCDC 618892' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 Eu O8 S, H2 O' _chemical_formula_sum 'C7 H9 Eu O9 S' _chemical_formula_weight 421.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.868(4) _cell_length_b 9.200(3) _cell_length_c 14.955(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2183.2(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 974 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.90 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 5.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.30 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10860 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _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 2.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2135 _reflns_number_gt 1901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2135 _refine_ls_number_parameters 168 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 1.023 _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 C1 C 0.5506(3) 0.8136(6) 0.3777(4) 0.0201(12) Uani 1 1 d . . . C2 C 0.5647(4) 0.9598(6) 0.3539(4) 0.0188(14) Uani 1 1 d . . . C3 C 0.4974(4) 1.0592(6) 0.3668(4) 0.0258(15) Uani 1 1 d . . . H3A H 0.5058 1.1562 0.3518 0.031 Uiso 1 1 calc R . . C4 C 0.4242(4) 1.0205(6) 0.3988(4) 0.0223(13) Uani 1 1 d . . . H4A H 0.3819 1.0893 0.4058 0.027 Uiso 1 1 calc R . . C5 C 0.4096(4) 0.8763(6) 0.4223(4) 0.0189(12) Uani 1 1 d . . . C6 C 0.4713(3) 0.7743(6) 0.4117(4) 0.0223(12) Uani 1 1 d . . . H6A H 0.4607 0.6781 0.4270 0.027 Uiso 1 1 calc R . . C7 C 0.6148(3) 0.6979(6) 0.3711(4) 0.0177(12) Uani 1 1 d . . . Eu1 Eu 0.227371(17) 1.05293(3) 0.644886(19) 0.01626(17) Uani 1 1 d . . . O1 O 0.5940(3) 0.5677(4) 0.3838(4) 0.0330(11) Uani 1 1 d . . . O2 O 0.6918(2) 0.7265(5) 0.3536(2) 0.0197(9) Uani 1 1 d . . . O3 O 0.6383(2) 1.0062(5) 0.3216(3) 0.0245(9) Uani 1 1 d . . . O4 O 0.2761(3) 0.9529(4) 0.5081(3) 0.0255(11) Uani 1 1 d . . . O5 O 0.2588(2) 0.7731(5) 0.3956(3) 0.0297(10) Uani 1 1 d . . . O6 O 0.3307(2) 0.7087(4) 0.5319(3) 0.0223(9) Uani 1 1 d . . . O7 O 0.1416(2) 1.2170(4) 0.7286(3) 0.0286(10) Uani 1 1 d . . . H7A H 0.1271 1.2875 0.6952 0.043 Uiso 1 1 d RD . . H7C H 0.1694 1.2491 0.7729 0.043 Uiso 1 1 d R . . O8 O 0.2084(3) 0.9695(5) 0.7952(3) 0.0347(11) Uani 1 1 d . . . H8A H 0.2346 0.8897 0.8022 0.052 Uiso 1 1 d R . . H8B H 0.2278 1.0325 0.8313 0.052 Uiso 1 1 d R . . O9 O 0.0636(5) 0.1011(8) 0.8882(6) 0.058(2) Uani 0.76 1 d P A 1 H9D H 0.0179 0.0527 0.8874 0.069 Uiso 0.76 1 d PR A 1 H9C H 0.0878 0.0940 0.8377 0.069 Uiso 0.76 1 d PR A 1 O10 O 0.0000 0.070(3) 0.7500 0.35(5) Uani 0.48 2 d SP B 2 H10D H 0.0402 0.1191 0.7317 0.420 Uiso 0.24 1 d PR B 2 H10B H -0.0211 0.0506 0.6991 0.525 Uiso 0.24 1 d PR B 2 S1 S 0.31192(8) 0.82272(15) 0.46726(9) 0.0179(3) 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 C1 0.018(3) 0.014(3) 0.028(3) -0.002(2) -0.004(2) 0.001(2) C2 0.015(3) 0.017(3) 0.024(3) 0.002(2) -0.001(2) 0.002(2) C3 0.023(3) 0.017(3) 0.038(4) 0.008(2) -0.002(3) 0.004(2) C4 0.020(3) 0.015(3) 0.032(4) 0.007(3) -0.001(2) 0.002(2) C5 0.020(3) 0.017(3) 0.020(3) 0.000(2) 0.002(2) 0.002(2) C6 0.022(3) 0.015(3) 0.030(3) 0.003(2) 0.003(2) 0.000(2) C7 0.021(3) 0.010(3) 0.022(3) 0.001(2) 0.000(2) 0.002(2) Eu1 0.0135(2) 0.0140(2) 0.0213(3) 0.00028(10) -0.00017(10) -0.00018(10) O1 0.018(2) 0.018(2) 0.063(3) -0.001(2) 0.004(2) -0.0008(17) O2 0.015(2) 0.016(2) 0.028(2) -0.0002(15) -0.0024(15) 0.0024(17) O3 0.015(2) 0.020(2) 0.039(2) 0.005(2) -0.003(2) -0.0032(18) O4 0.030(3) 0.016(3) 0.031(3) -0.0016(17) 0.0099(18) 0.0032(16) O5 0.022(2) 0.033(3) 0.034(3) -0.003(2) -0.0036(19) 0.0024(18) O6 0.0197(19) 0.022(2) 0.025(2) 0.0053(17) 0.0078(16) 0.0036(17) O7 0.032(2) 0.025(2) 0.029(2) 0.0035(18) 0.0053(18) 0.008(2) O8 0.050(3) 0.028(3) 0.025(2) -0.001(2) 0.001(2) 0.013(2) O9 0.057(5) 0.044(4) 0.071(5) -0.007(4) 0.030(4) -0.018(4) O10 0.14(4) 0.08(2) 0.82(14) 0.000 0.27(7) 0.000 S1 0.0167(7) 0.0164(7) 0.0206(7) -0.0002(5) 0.0041(5) 0.0026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.405(8) . ? C1 C2 1.410(8) . ? C1 C7 1.476(8) . ? C2 O3 1.333(8) . ? C2 C3 1.419(9) . ? C3 C4 1.305(9) . ? C3 H3A 0.9300 . ? C4 C5 1.392(8) . ? C4 H4A 0.9300 . ? C5 C6 1.366(8) . ? C5 S1 1.760(6) . ? C6 H6A 0.9300 . ? C7 O1 1.258(7) . ? C7 O2 1.277(7) . ? C7 Eu1 2.928(5) 4_566 ? Eu1 O3 2.257(4) 5_676 ? Eu1 O4 2.373(5) . ? Eu1 O7 2.387(4) . ? Eu1 O8 2.394(5) . ? Eu1 O6 2.399(4) 8_665 ? Eu1 O2 2.400(4) 5_676 ? Eu1 O1 2.428(4) 4_466 ? Eu1 O2 2.632(4) 4_466 ? Eu1 C7 2.928(5) 4_466 ? Eu1 H7A 2.7849 . ? Eu1 H7C 2.7873 . ? Eu1 H8A 2.7928 . ? Eu1 H8B 2.7937 . ? O1 Eu1 2.428(4) 4_566 ? O2 Eu1 2.400(4) 5_676 ? O2 Eu1 2.632(4) 4_566 ? O3 Eu1 2.257(4) 5_676 ? O4 S1 1.459(4) . ? O5 S1 1.437(4) . ? O6 S1 1.457(4) . ? O6 Eu1 2.399(4) 8_655 ? O7 H7A 0.8500 . ? O7 H7C 0.8500 . ? O8 H8A 0.8500 . ? O8 H8B 0.8501 . ? O9 H9D 0.8500 . ? O9 H9C 0.8500 . ? O10 H10D 0.8275 . ? O10 H10B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.6(5) . . ? C6 C1 C7 117.2(5) . . ? C2 C1 C7 124.2(5) . . ? O3 C2 C1 122.4(5) . . ? O3 C2 C3 120.1(5) . . ? C1 C2 C3 117.4(6) . . ? C4 C3 C2 122.9(6) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 S1 118.9(4) . . ? C4 C5 S1 120.8(4) . . ? C5 C6 C1 120.5(5) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? O1 C7 O2 118.6(5) . . ? O1 C7 C1 119.7(5) . . ? O2 C7 C1 121.7(5) . . ? O1 C7 Eu1 54.7(3) . 4_566 ? O2 C7 Eu1 64.0(3) . 4_566 ? C1 C7 Eu1 173.9(4) . 4_566 ? O3 Eu1 O4 77.90(16) 5_676 . ? O3 Eu1 O7 125.07(16) 5_676 . ? O4 Eu1 O7 152.02(14) . . ? O3 Eu1 O8 80.38(17) 5_676 . ? O4 Eu1 O8 136.56(15) . . ? O7 Eu1 O8 68.82(15) . . ? O3 Eu1 O6 131.55(14) 5_676 8_665 ? O4 Eu1 O6 75.50(14) . 8_665 ? O7 Eu1 O6 76.85(14) . 8_665 ? O8 Eu1 O6 143.54(15) . 8_665 ? O3 Eu1 O2 72.37(14) 5_676 5_676 ? O4 Eu1 O2 99.34(13) . 5_676 ? O7 Eu1 O2 76.40(14) . 5_676 ? O8 Eu1 O2 109.22(15) . 5_676 ? O6 Eu1 O2 72.95(12) 8_665 5_676 ? O3 Eu1 O1 138.82(14) 5_676 4_466 ? O4 Eu1 O1 87.39(17) . 4_466 ? O7 Eu1 O1 83.37(15) . 4_466 ? O8 Eu1 O1 84.81(18) . 4_466 ? O6 Eu1 O1 79.27(15) 8_665 4_466 ? O2 Eu1 O1 148.60(13) 5_676 4_466 ? O3 Eu1 O2 87.99(13) 5_676 4_466 ? O4 Eu1 O2 72.45(13) . 4_466 ? O7 Eu1 O2 119.40(13) . 4_466 ? O8 Eu1 O2 69.61(14) . 4_466 ? O6 Eu1 O2 120.49(13) 8_665 4_466 ? O2 Eu1 O2 160.06(8) 5_676 4_466 ? O1 Eu1 O2 50.84(13) 4_466 4_466 ? O3 Eu1 C7 113.85(15) 5_676 4_466 ? O4 Eu1 C7 79.78(15) . 4_466 ? O7 Eu1 C7 101.15(15) . 4_466 ? O8 Eu1 C7 75.35(16) . 4_466 ? O6 Eu1 C7 100.32(14) 8_665 4_466 ? O2 Eu1 C7 173.16(14) 5_676 4_466 ? O1 Eu1 C7 25.00(14) 4_466 4_466 ? O2 Eu1 C7 25.86(14) 4_466 4_466 ? O3 Eu1 H7A 131.8 5_676 . ? O4 Eu1 H7A 136.0 . . ? O7 Eu1 H7A 16.7 . . ? O8 Eu1 H7A 85.6 . . ? O6 Eu1 H7A 60.5 8_665 . ? O2 Eu1 H7A 69.4 5_676 . ? O1 Eu1 H7A 84.5 4_466 . ? O2 Eu1 H7A 129.2 4_466 . ? C7 Eu1 H7A 106.5 4_466 . ? O3 Eu1 H7C 108.4 5_676 . ? O4 Eu1 H7C 162.0 . . ? O7 Eu1 H7C 16.7 . . ? O8 Eu1 H7C 61.4 . . ? O6 Eu1 H7C 88.3 8_665 . ? O2 Eu1 H7C 67.8 5_676 . ? O1 Eu1 H7C 97.5 4_466 . ? O2 Eu1 H7C 123.8 4_466 . ? C7 Eu1 H7C 111.4 4_466 . ? H7A Eu1 H7C 28.8 . . ? O3 Eu1 H8A 69.2 5_676 . ? O4 Eu1 H8A 120.3 . . ? O7 Eu1 H8A 85.5 . . ? O8 Eu1 H8A 16.7 . . ? O6 Eu1 H8A 158.4 8_665 . ? O2 Eu1 H8A 115.1 5_676 . ? O1 Eu1 H8A 86.5 4_466 . ? O2 Eu1 H8A 58.4 4_466 . ? C7 Eu1 H8A 70.7 4_466 . ? H7A Eu1 H8A 102.3 . . ? H7C Eu1 H8A 77.5 . . ? O3 Eu1 H8B 76.1 5_676 . ? O4 Eu1 H8B 146.4 . . ? O7 Eu1 H8B 61.4 . . ? O8 Eu1 H8B 16.7 . . ? O6 Eu1 H8B 138.1 8_665 . ? O2 Eu1 H8B 92.6 5_676 . ? O1 Eu1 H8B 98.5 4_466 . ? O2 Eu1 H8B 85.8 4_466 . ? C7 Eu1 H8B 91.7 4_466 . ? H7A Eu1 H8B 77.5 . . ? H7C Eu1 H8B 50.1 . . ? H8A Eu1 H8B 28.8 . . ? C7 O1 Eu1 100.3(4) . 4_566 ? C7 O2 Eu1 133.1(4) . 5_676 ? C7 O2 Eu1 90.1(3) . 4_566 ? Eu1 O2 Eu1 135.34(17) 5_676 4_566 ? C2 O3 Eu1 132.0(4) . 5_676 ? S1 O4 Eu1 143.7(3) . . ? S1 O6 Eu1 145.0(2) . 8_655 ? Eu1 O7 H7A 109.2 . . ? Eu1 O7 H7C 109.4 . . ? H7A O7 H7C 109.5 . . ? Eu1 O8 H8A 109.3 . . ? Eu1 O8 H8B 109.4 . . ? H8A O8 H8B 109.5 . . ? H9D O9 H9C 109.5 . . ? H10D O10 H10B 97.0 . . ? O5 S1 O6 112.7(3) . . ? O5 S1 O4 110.1(3) . . ? O6 S1 O4 113.1(3) . . ? O5 S1 C5 108.7(3) . . ? O6 S1 C5 106.0(3) . . ? O4 S1 C5 105.8(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.748 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.183 # Attachment 'Gd1.cif' data_81 _database_code_depnum_ccdc_archive 'CCDC 618893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 Gd O8 S, 0.5(H0.76 O0.38), 0.81(H2 O)' _chemical_formula_sum 'C7 H9 Gd O9 S' _chemical_formula_weight 426.45 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 Orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.874(4) _cell_length_b 9.161(2) _cell_length_c 14.936(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2172.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 803 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.59 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 6.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.39 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10832 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _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 2.57 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2138 _reflns_number_gt 1805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2138 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _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 0.272551(16) 0.44684(3) 0.356053(17) 0.01669(13) Uani 1 1 d . . . C1 C 0.0907(3) 0.6238(6) 0.5776(3) 0.0197(11) Uani 1 1 d . . . C2 C 0.0767(4) 0.4791(6) 0.6015(4) 0.0243(13) Uani 1 1 d . . . H2 H 0.1191 0.4100 0.5945 0.029 Uiso 1 1 calc R . . C3 C 0.0002(4) 0.4396(6) 0.6353(4) 0.0242(13) Uani 1 1 d . . . H3 H -0.0086 0.3428 0.6516 0.029 Uiso 1 1 calc R . . C4 C 0.0281(3) 0.7247(6) 0.5883(3) 0.0224(12) Uani 1 1 d . . . H4 H 0.0385 0.8214 0.5730 0.027 Uiso 1 1 calc R . . C5 C -0.0659(4) 0.5400(6) 0.6465(3) 0.0214(13) Uani 1 1 d . . . C6 C -0.0504(3) 0.6866(6) 0.6212(3) 0.0193(11) Uani 1 1 d . . . C7 C -0.1152(3) 0.8010(6) 0.6286(3) 0.0201(11) Uani 1 1 d . . . O1 O -0.0944(3) 0.9330(4) 0.6162(3) 0.0323(10) Uani 1 1 d . . . O2 O -0.1924(2) 0.7729(4) 0.6450(2) 0.0211(8) Uani 1 1 d . . . O3 O -0.1383(2) 0.4938(4) 0.6787(3) 0.0238(8) Uani 1 1 d . . . O4 O 0.2238(2) 0.5460(4) 0.4923(3) 0.0251(9) Uani 1 1 d . . . O5 O 0.2410(2) 0.7269(5) 0.6053(3) 0.0306(10) Uani 1 1 d . . . O6 O 0.1698(2) 0.7925(4) 0.4684(2) 0.0230(8) Uani 1 1 d . . . O7 O 0.2915(3) 0.5305(4) 0.2067(3) 0.0328(10) Uani 1 1 d . . . H7A H 0.2653 0.6106 0.1999 0.049 Uiso 1 1 d R . . H7C H 0.2720 0.4672 0.1706 0.049 Uiso 1 1 d R . . O8 O 0.3582(2) 0.2826(4) 0.2721(3) 0.0280(9) Uani 1 1 d . . . H8A H 0.3122 0.2565 0.2478 0.042 Uiso 1 1 d R . . H8C H 0.3628 0.2421 0.3231 0.042 Uiso 1 1 d R . . O9 O 0.4357(5) 0.4013(8) 0.1138(5) 0.073(2) Uani 0.81 1 d P A 1 H9D H 0.4297 0.4336 0.1668 0.088 Uiso 0.81 1 d PR A 1 H9A H 0.4842 0.4244 0.0944 0.110 Uiso 0.81 1 d PR A 1 O10 O 0.5000 0.431(2) 0.2500 0.089(8) Uani 0.38 2 d SP B 2 H10D H 0.4714 0.4727 0.2907 0.133 Uiso 0.19 1 d PR B 2 H10B H 0.5001 0.3393 0.2589 0.133 Uiso 0.19 1 d PR B 2 S1 S 0.18794(8) 0.67706(14) 0.53296(8) 0.0187(3) 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 0.01525(19) 0.01447(19) 0.02035(19) 0.00020(10) -0.00028(10) -0.00018(10) C1 0.018(3) 0.019(3) 0.023(3) 0.000(2) 0.004(2) -0.001(2) C2 0.022(3) 0.020(3) 0.032(3) 0.004(2) -0.001(3) 0.004(2) C3 0.022(3) 0.017(3) 0.033(3) 0.008(2) -0.002(2) 0.003(2) C4 0.026(3) 0.013(3) 0.028(3) 0.003(2) 0.002(2) 0.001(2) C5 0.022(3) 0.021(3) 0.021(3) -0.003(2) -0.003(2) 0.002(2) C6 0.018(3) 0.016(3) 0.024(3) -0.002(2) -0.002(2) -0.001(2) C7 0.024(3) 0.015(3) 0.022(3) 0.000(2) 0.000(2) 0.000(2) O1 0.020(2) 0.016(2) 0.060(3) 0.0015(19) 0.007(2) 0.0005(17) O2 0.0142(19) 0.019(2) 0.030(2) 0.0001(15) -0.0039(15) -0.0024(16) O3 0.0169(19) 0.0227(19) 0.032(2) 0.0040(17) -0.0002(19) -0.0025(17) O4 0.030(2) 0.022(2) 0.024(2) -0.0003(15) 0.0085(17) 0.0036(16) O5 0.027(2) 0.033(2) 0.033(3) -0.003(2) -0.0070(19) 0.0020(18) O6 0.0227(19) 0.023(2) 0.0236(19) 0.0049(15) 0.0074(16) 0.0002(17) O7 0.049(3) 0.028(2) 0.022(2) 0.0006(17) 0.001(2) 0.0094(19) O8 0.030(2) 0.027(2) 0.027(2) 0.0036(16) 0.0040(18) 0.0061(18) O9 0.068(5) 0.057(4) 0.094(5) -0.004(4) 0.044(5) -0.009(4) O10 0.065(15) 0.068(16) 0.13(2) 0.000 0.031(17) 0.000 S1 0.0187(6) 0.0179(7) 0.0196(6) 0.0002(5) 0.0032(5) 0.0025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.260(4) 5_566 ? Gd1 O4 2.359(4) . ? Gd1 O7 2.377(4) . ? Gd1 O6 2.378(3) 8_655 ? Gd1 O2 2.382(4) 5_566 ? Gd1 O8 2.385(4) . ? Gd1 O1 2.418(4) 4_566 ? Gd1 O2 2.627(4) 4_566 ? Gd1 C7 2.926(5) 4_566 ? Gd1 H8A 2.4594 . ? Gd1 H8C 2.4113 . ? C1 C4 1.366(7) . ? C1 C2 1.390(8) . ? C1 S1 1.751(5) . ? C2 C3 1.365(9) . ? C2 H2 0.9300 . ? C3 C5 1.405(8) . ? C3 H3 0.9300 . ? C4 C6 1.385(7) . ? C4 H4 0.9300 . ? C5 O3 1.316(7) . ? C5 C6 1.416(7) . ? C6 C7 1.472(7) . ? C7 O1 1.267(6) . ? C7 O2 1.275(7) . ? C7 Gd1 2.926(5) 4_466 ? O1 Gd1 2.418(4) 4_466 ? O2 Gd1 2.382(4) 5_566 ? O2 Gd1 2.627(4) 4_466 ? O3 Gd1 2.260(4) 5_566 ? O4 S1 1.461(4) . ? O5 S1 1.443(4) . ? O6 S1 1.460(4) . ? O6 Gd1 2.378(3) 8_665 ? O7 H7A 0.8500 . ? O7 H7C 0.8500 . ? O8 H8A 0.8501 . ? O8 H8C 0.8500 . ? O9 H9D 0.8501 . ? O9 H9A 0.8499 . ? O10 H10D 0.8500 . ? O10 H10B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O4 78.23(14) 5_566 . ? O3 Gd1 O7 80.01(15) 5_566 . ? O4 Gd1 O7 136.62(14) . . ? O3 Gd1 O6 131.91(13) 5_566 8_655 ? O4 Gd1 O6 75.30(13) . 8_655 ? O7 Gd1 O6 143.62(14) . 8_655 ? O3 Gd1 O2 72.40(13) 5_566 5_566 ? O4 Gd1 O2 98.97(12) . 5_566 ? O7 Gd1 O2 109.48(13) . 5_566 ? O6 Gd1 O2 73.03(12) 8_655 5_566 ? O3 Gd1 O8 124.68(14) 5_566 . ? O4 Gd1 O8 152.09(13) . . ? O7 Gd1 O8 68.77(13) . . ? O6 Gd1 O8 77.08(13) 8_655 . ? O2 Gd1 O8 76.58(13) 5_566 . ? O3 Gd1 O1 138.92(13) 5_566 4_566 ? O4 Gd1 O1 87.90(15) . 4_566 ? O7 Gd1 O1 84.46(16) . 4_566 ? O6 Gd1 O1 79.25(13) 8_655 4_566 ? O2 Gd1 O1 148.54(13) 5_566 4_566 ? O8 Gd1 O1 83.07(14) . 4_566 ? O3 Gd1 O2 87.91(13) 5_566 4_566 ? O4 Gd1 O2 72.47(12) . 4_566 ? O7 Gd1 O2 69.66(13) . 4_566 ? O6 Gd1 O2 120.25(12) 8_655 4_566 ? O2 Gd1 O2 159.92(7) 5_566 4_566 ? O8 Gd1 O2 119.50(12) . 4_566 ? O1 Gd1 O2 51.01(12) 4_566 4_566 ? O3 Gd1 C7 113.73(14) 5_566 4_566 ? O4 Gd1 C7 80.13(14) . 4_566 ? O7 Gd1 C7 75.04(14) . 4_566 ? O6 Gd1 C7 100.35(13) 8_655 4_566 ? O2 Gd1 C7 173.28(13) 5_566 4_566 ? O8 Gd1 C7 101.06(14) . 4_566 ? O1 Gd1 C7 25.19(14) 4_566 4_566 ? O2 Gd1 C7 25.84(13) 4_566 4_566 ? O3 Gd1 H8A 105.1 5_566 . ? O4 Gd1 H8A 157.5 . . ? O7 Gd1 H8A 65.1 . . ? O6 Gd1 H8A 86.8 8_655 . ? O2 Gd1 H8A 62.2 5_566 . ? O8 Gd1 H8A 20.1 . . ? O1 Gd1 H8A 102.2 4_566 . ? O2 Gd1 H8A 129.4 4_566 . ? C7 Gd1 H8A 117.1 4_566 . ? O3 Gd1 H8C 134.5 5_566 . ? O4 Gd1 H8C 132.1 . . ? O7 Gd1 H8C 89.1 . . ? O6 Gd1 H8C 56.8 8_655 . ? O2 Gd1 H8C 70.0 5_566 . ? O8 Gd1 H8C 20.4 . . ? O1 Gd1 H8C 82.5 4_566 . ? O2 Gd1 H8C 129.3 4_566 . ? C7 Gd1 H8C 105.5 4_566 . ? H8A Gd1 H8C 33.1 . . ? C4 C1 C2 119.9(5) . . ? C4 C1 S1 119.8(4) . . ? C2 C1 S1 120.2(4) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C5 122.3(5) . . ? C2 C3 H3 118.8 . . ? C5 C3 H3 118.8 . . ? C1 C4 C6 121.7(5) . . ? C1 C4 H4 119.1 . . ? C6 C4 H4 119.1 . . ? O3 C5 C3 119.0(5) . . ? O3 C5 C6 123.6(5) . . ? C3 C5 C6 117.4(5) . . ? C4 C6 C5 119.3(5) . . ? C4 C6 C7 118.4(5) . . ? C5 C6 C7 122.3(5) . . ? O1 C7 O2 118.1(5) . . ? O1 C7 C6 119.1(5) . . ? O2 C7 C6 122.8(5) . . ? O1 C7 Gd1 54.3(3) . 4_466 ? O2 C7 Gd1 63.9(3) . 4_466 ? C6 C7 Gd1 173.2(4) . 4_466 ? C7 O1 Gd1 100.5(3) . 4_466 ? C7 O2 Gd1 133.0(4) . 5_566 ? C7 O2 Gd1 90.3(3) . 4_466 ? Gd1 O2 Gd1 135.45(16) 5_566 4_466 ? C5 O3 Gd1 131.5(3) . 5_566 ? S1 O4 Gd1 143.4(2) . . ? S1 O6 Gd1 145.2(2) . 8_665 ? Gd1 O7 H7A 109.2 . . ? Gd1 O7 H7C 109.2 . . ? H7A O7 H7C 109.5 . . ? Gd1 O8 H8A 84.9 . . ? Gd1 O8 H8C 81.5 . . ? H8A O8 H8C 109.5 . . ? H9D O9 H9A 109.5 . . ? H10D O10 H10B 109.5 . . ? O5 S1 O6 112.3(2) . . ? O5 S1 O4 110.1(2) . . ? O6 S1 O4 113.5(2) . . ? O5 S1 C1 108.5(2) . . ? O6 S1 C1 106.2(2) . . ? O4 S1 C1 105.8(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.160 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.148 # Attachment 'Nd1.cif' data_dd1 _database_code_depnum_ccdc_archive 'CCDC 618894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 Nd O8 S, H2 O' _chemical_formula_sum 'C7 H9 Nd O9 S' _chemical_formula_weight 413.44 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.861(4) _cell_length_b 9.269(2) _cell_length_c 14.971(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2201.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 886 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 23.05 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 4.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.24 _exptl_absorpt_correction_T_max 0.37 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10991 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2167 _reflns_number_gt 1980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0711P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2167 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 1.0489(3) 0.6856(5) 0.6231(3) 0.0203(9) Uani 1 1 d . . . C2 C 1.0644(4) 0.5396(5) 0.6466(3) 0.0212(11) Uani 1 1 d . . . C3 C 0.9987(4) 0.4420(5) 0.6334(3) 0.0237(11) Uani 1 1 d . . . H3A H 1.0076 0.3460 0.6488 0.028 Uiso 1 1 calc R . . C4 C 0.9231(3) 0.4791(5) 0.5995(3) 0.0240(10) Uani 1 1 d . . . H4A H 0.8816 0.4096 0.5909 0.029 Uiso 1 1 calc R . . C5 C 0.9076(3) 0.6232(5) 0.5773(3) 0.0202(9) Uani 1 1 d . . . C6 C 0.9697(3) 0.7228(5) 0.5893(3) 0.0229(10) Uani 1 1 d . . . H6A H 0.9591 0.8186 0.5745 0.027 Uiso 1 1 calc R . . C7 C 1.1127(3) 0.8003(5) 0.6299(3) 0.0204(9) Uani 1 1 d . . . Nd1 Nd 0.726473(15) 0.44657(3) 0.352434(16) 0.01668(14) Uani 1 1 d . . . O1 O 1.0910(2) 0.9296(3) 0.6156(3) 0.0361(9) Uani 1 1 d . . . O2 O 1.1897(2) 0.7734(3) 0.64855(19) 0.0213(7) Uani 1 1 d . . . O3 O 1.1364(2) 0.4950(3) 0.6793(2) 0.0255(7) Uani 1 1 d . . . O4 O 0.8310(2) 0.7880(3) 0.4669(2) 0.0260(7) Uani 1 1 d . . . O5 O 0.7581(2) 0.7285(4) 0.6026(2) 0.0309(8) Uani 1 1 d . . . O6 O 0.7744(2) 0.5471(3) 0.4921(3) 0.0272(9) Uani 1 1 d . . . O7 O 0.7052(3) 0.5326(4) 0.2013(3) 0.0402(10) Uani 1 1 d . . . H7A H 0.7310 0.6121 0.1943 0.060 Uiso 1 1 d R . . H7B H 0.7246 0.4706 0.1648 0.060 Uiso 1 1 d R . . O8 O 0.6375(2) 0.2800(3) 0.2685(2) 0.0308(8) Uani 1 1 d . . . H8E H 0.6665 0.2085 0.2865 0.037 Uiso 1 1 d R . . H8C H 0.6651 0.2488 0.2238 0.046 Uiso 1 1 d R . . O9 O 0.5645(3) 0.3997(5) 0.1070(4) 0.0694(14) Uani 1 1 d . . . H9D H 0.5192 0.4487 0.1094 0.083 Uiso 1 1 d R . . H9C H 0.5898 0.4045 0.1570 0.104 Uiso 1 1 d R . . S1 S 0.81121(7) 0.67644(11) 0.53184(7) 0.0193(3) 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 C1 0.021(2) 0.016(2) 0.024(2) 0.0011(18) 0.0011(18) -0.0016(19) C2 0.024(3) 0.018(3) 0.021(2) -0.0010(16) 0.0022(18) 0.0013(19) C3 0.026(3) 0.014(2) 0.031(3) 0.0063(17) 0.001(2) -0.0029(18) C4 0.027(3) 0.015(2) 0.029(3) 0.003(2) 0.001(2) -0.0032(19) C5 0.022(2) 0.017(2) 0.021(2) 0.0008(17) -0.0006(18) -0.0002(18) C6 0.029(2) 0.012(2) 0.028(2) 0.0026(18) -0.0046(19) 0.0007(18) C7 0.024(2) 0.013(2) 0.024(2) 0.0018(17) 0.0001(18) -0.0004(19) Nd1 0.0167(2) 0.0127(2) 0.0207(2) 0.00054(8) 0.00020(8) 0.00026(8) O1 0.0220(19) 0.0154(18) 0.071(3) 0.0033(17) -0.003(2) -0.0004(14) O2 0.0187(18) 0.0144(16) 0.0308(18) -0.0001(12) 0.0016(12) 0.0022(14) O3 0.0205(17) 0.0183(16) 0.0376(19) 0.0055(15) 0.0039(15) 0.0027(14) O4 0.0278(17) 0.0221(16) 0.0282(17) 0.0078(13) -0.0088(13) -0.0042(14) O5 0.0267(18) 0.033(2) 0.033(2) -0.0050(17) 0.0054(15) -0.0029(15) O6 0.031(2) 0.0174(19) 0.033(2) 0.0003(13) -0.0100(15) -0.0043(13) O7 0.067(3) 0.029(2) 0.025(2) 0.0019(15) -0.006(2) -0.0169(19) O8 0.038(2) 0.0223(17) 0.0316(18) 0.0021(14) -0.0088(15) -0.0070(15) O9 0.063(3) 0.059(3) 0.086(4) -0.008(3) -0.032(3) 0.016(3) S1 0.0212(6) 0.0155(5) 0.0211(5) 0.0007(4) -0.0040(4) -0.0029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.398(6) . ? C1 C2 1.420(6) . ? C1 C7 1.471(6) . ? C2 O3 1.309(6) . ? C2 C3 1.394(7) . ? C3 C4 1.348(8) . ? C3 H3A 0.9300 . ? C4 C5 1.398(6) . ? C4 H4A 0.9300 . ? C5 C6 1.362(6) . ? C5 S1 1.745(5) . ? C6 H6A 0.9300 . ? C7 O1 1.265(5) . ? C7 O2 1.278(6) . ? C7 Nd1 2.972(4) 4_566 ? Nd1 O3 2.291(3) 5_766 ? Nd1 O6 2.412(4) . ? Nd1 O7 2.423(4) . ? Nd1 O2 2.434(3) 5_766 ? Nd1 O4 2.435(3) 8_755 ? Nd1 O8 2.440(3) . ? Nd1 O1 2.482(4) 4_466 ? Nd1 O2 2.660(3) 4_466 ? Nd1 C7 2.972(4) 4_466 ? Nd1 H8E 2.5982 . ? O1 Nd1 2.482(4) 4_566 ? O2 Nd1 2.434(3) 5_766 ? O2 Nd1 2.660(3) 4_566 ? O3 Nd1 2.291(3) 5_766 ? O4 S1 1.453(3) . ? O4 Nd1 2.435(3) 8_765 ? O5 S1 1.438(4) . ? O6 S1 1.461(3) . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 H8E 0.8500 . ? O8 H8C 0.8500 . ? O9 H9D 0.8501 . ? O9 H9C 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.7(4) . . ? C6 C1 C7 117.7(4) . . ? C2 C1 C7 123.6(4) . . ? O3 C2 C3 120.0(4) . . ? O3 C2 C1 123.0(4) . . ? C3 C2 C1 117.0(5) . . ? C4 C3 C2 123.6(4) . . ? C4 C3 H3A 118.2 . . ? C2 C3 H3A 118.2 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 119.3(4) . . ? C6 C5 S1 119.6(3) . . ? C4 C5 S1 121.1(4) . . ? C5 C6 C1 122.0(4) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O1 C7 O2 118.7(4) . . ? O1 C7 C1 119.1(4) . . ? O2 C7 C1 122.1(4) . . ? O1 C7 Nd1 55.4(2) . 4_566 ? O2 C7 Nd1 63.5(2) . 4_566 ? C1 C7 Nd1 173.9(3) . 4_566 ? O3 Nd1 O6 77.81(12) 5_766 . ? O3 Nd1 O7 82.01(14) 5_766 . ? O6 Nd1 O7 136.59(12) . . ? O3 Nd1 O2 71.25(11) 5_766 5_766 ? O6 Nd1 O2 99.02(10) . 5_766 ? O7 Nd1 O2 110.24(12) . 5_766 ? O3 Nd1 O4 130.09(12) 5_766 8_755 ? O6 Nd1 O4 74.99(11) . 8_755 ? O7 Nd1 O4 143.50(13) . 8_755 ? O2 Nd1 O4 72.73(10) 5_766 8_755 ? O3 Nd1 O8 126.29(12) 5_766 . ? O6 Nd1 O8 150.84(11) . . ? O7 Nd1 O8 69.30(12) . . ? O2 Nd1 O8 77.43(11) 5_766 . ? O4 Nd1 O8 76.36(11) 8_755 . ? O3 Nd1 O1 138.77(11) 5_766 4_466 ? O6 Nd1 O1 85.82(13) . 4_466 ? O7 Nd1 O1 84.68(16) . 4_466 ? O2 Nd1 O1 149.44(11) 5_766 4_466 ? O4 Nd1 O1 79.59(12) 8_755 4_466 ? O8 Nd1 O1 83.77(12) . 4_466 ? O3 Nd1 O2 88.63(11) 5_766 4_466 ? O6 Nd1 O2 72.36(10) . 4_466 ? O7 Nd1 O2 69.10(11) . 4_466 ? O2 Nd1 O2 159.55(6) 5_766 4_466 ? O4 Nd1 O2 120.71(10) 8_755 4_466 ? O8 Nd1 O2 119.20(10) . 4_466 ? O1 Nd1 O2 50.23(10) 4_466 4_466 ? O3 Nd1 C7 114.09(12) 5_766 4_466 ? O6 Nd1 C7 79.01(12) . 4_466 ? O7 Nd1 C7 74.85(13) . 4_466 ? O2 Nd1 C7 173.48(11) 5_766 4_466 ? O4 Nd1 C7 100.75(11) 8_755 4_466 ? O8 Nd1 C7 101.20(12) . 4_466 ? O1 Nd1 C7 24.79(11) 4_466 4_466 ? O2 Nd1 C7 25.47(11) 4_466 4_466 ? O3 Nd1 H8E 118.0 5_766 . ? O6 Nd1 H8E 140.6 . . ? O7 Nd1 H8E 82.7 . . ? O2 Nd1 H8E 59.1 5_766 . ? O4 Nd1 H8E 67.5 8_755 . ? O8 Nd1 H8E 19.1 . . ? O1 Nd1 H8E 98.6 4_466 . ? O2 Nd1 H8E 138.3 4_466 . ? C7 Nd1 H8E 118.8 4_466 . ? C7 O1 Nd1 99.8(3) . 4_566 ? C7 O2 Nd1 133.2(3) . 5_766 ? C7 O2 Nd1 91.0(3) . 4_566 ? Nd1 O2 Nd1 134.25(14) 5_766 4_566 ? C2 O3 Nd1 132.5(3) . 5_766 ? S1 O4 Nd1 145.0(2) . 8_765 ? S1 O6 Nd1 142.8(2) . . ? Nd1 O7 H7A 109.4 . . ? Nd1 O7 H7B 109.1 . . ? H7A O7 H7B 109.5 . . ? Nd1 O8 H8E 91.0 . . ? Nd1 O8 H8C 108.9 . . ? H8E O8 H8C 72.9 . . ? H9D O9 H9C 109.5 . . ? O5 S1 O4 112.4(2) . . ? O5 S1 O6 110.0(2) . . ? O4 S1 O6 113.5(2) . . ? O5 S1 C5 108.7(2) . . ? O4 S1 C5 105.8(2) . . ? O6 S1 C5 106.1(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.911 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.134 # Attachment 'Sm1.cif' data_91 _database_code_depnum_ccdc_archive 'CCDC 618895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '8(C7 H7 O8 S Sm), 4(H), 8(H2 O)' _chemical_formula_sum 'C56 H72 O72 S8 Sm8' _chemical_formula_weight 3356.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.877(4) _cell_length_b 9.203(2) _cell_length_c 14.958(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2185.5(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 761 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.66 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 5.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 0.57 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10956 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2156 _reflns_number_gt 1576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2156 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 O9 O 0.4359(4) 0.3992(6) 0.3909(4) 0.0412(17) Uani 0.86 1 d P A 1 O10 O 0.5000 0.425(3) 0.2500 0.061(9) Uani 0.28 2 d SP B 2 Sm1 Sm 0.77286(2) -0.05328(3) 0.35423(2) 0.01806(12) Uani 1 1 d . . . C1 C 0.5911(4) 0.1242(7) 0.5768(4) 0.0184(15) Uani 1 1 d . . . C2 C 0.5765(5) -0.0199(7) 0.6000(4) 0.0248(17) Uani 1 1 d . . . H2 H 0.6186 -0.0891 0.5923 0.030 Uiso 1 1 calc R . . C3 C 0.5005(4) -0.0593(7) 0.6339(5) 0.0248(16) Uani 1 1 d . . . H3 H 0.4918 -0.1560 0.6493 0.030 Uiso 1 1 calc R . . C4 C 0.5286(4) 0.2238(7) 0.5883(5) 0.0228(17) Uani 1 1 d . . . H4 H 0.5386 0.3201 0.5728 0.027 Uiso 1 1 calc R . . C5 C 0.4346(4) 0.0404(7) 0.6465(4) 0.0232(15) Uani 1 1 d . . . C6 C 0.4503(4) 0.1857(7) 0.6225(4) 0.0213(16) Uani 1 1 d . . . C7 C 0.3867(4) 0.3013(7) 0.6291(4) 0.0214(16) Uani 1 1 d . . . O1 O 0.4071(3) 0.4330(5) 0.6170(3) 0.0316(13) Uani 1 1 d . . . O2 O 0.3092(3) 0.2738(5) 0.6460(3) 0.0235(11) Uani 1 1 d . . . O3 O 0.3621(3) -0.0053(5) 0.6787(3) 0.0239(11) Uani 1 1 d . . . O4 O 0.7242(3) 0.0468(4) 0.4919(3) 0.0274(11) Uani 1 1 d . . . O5 O 0.6688(3) 0.2905(4) 0.4675(3) 0.0254(11) Uani 1 1 d . . . O6 O 0.7416(3) 0.2277(5) 0.6037(3) 0.0311(12) Uani 1 1 d . . . O7 O 0.7922(3) 0.0310(5) 0.2038(3) 0.0358(14) Uani 1 1 d . . . H7A H 0.7660 0.1107 0.1968 0.054 Uiso 1 1 d R . . H7C H 0.7730 -0.0320 0.1676 0.054 Uiso 1 1 d R . . O8 O 0.8600(3) -0.2178(4) 0.2693(3) 0.0306(12) Uani 1 1 d . . . H8A H 0.8140 -0.2435 0.2449 0.046 Uiso 1 1 d R . . H8C H 0.8644 -0.2585 0.3202 0.046 Uiso 1 1 d R . . H9D H 0.4829 0.4506 0.3909 0.037 Uiso 0.86 1 d PR C 1 H9B H 0.4113 0.4103 0.3437 0.046 Uiso 0.86 1 d PR D 1 H10D H 0.5300 0.4730 0.2924 0.037 Uiso 0.14 1 d PR E 2 H10A H 0.5258 0.4431 0.2015 0.046 Uiso 0.14 1 d PR F 2 S1 S 0.68813(11) 0.17695(17) 0.53240(11) 0.0201(4) 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 O9 0.038(4) 0.040(4) 0.046(4) 0.000(3) -0.025(3) -0.009(3) O10 0.06(2) 0.06(2) 0.06(2) 0.000 -0.002(18) 0.000 Sm1 0.01591(19) 0.01548(18) 0.0228(2) -0.00060(15) 0.00019(17) -0.00025(17) C1 0.021(4) 0.019(4) 0.016(4) -0.001(3) -0.002(3) -0.005(3) C2 0.022(4) 0.023(4) 0.029(4) 0.001(3) -0.002(3) 0.007(3) C3 0.026(4) 0.012(3) 0.036(4) -0.004(3) -0.001(3) -0.003(3) C4 0.026(4) 0.013(3) 0.029(5) -0.001(3) -0.004(3) -0.001(3) C5 0.022(4) 0.026(4) 0.022(4) 0.002(3) 0.003(3) 0.001(3) C6 0.023(4) 0.018(4) 0.022(4) 0.001(3) 0.001(3) 0.002(3) C7 0.022(4) 0.020(4) 0.023(4) 0.002(3) 0.003(3) -0.001(3) O1 0.018(3) 0.015(2) 0.061(4) -0.005(2) -0.007(2) 0.002(2) O2 0.015(2) 0.019(2) 0.036(3) 0.001(2) 0.000(2) -0.001(2) O3 0.017(3) 0.021(2) 0.034(3) -0.008(2) 0.004(2) -0.003(2) O4 0.033(3) 0.019(2) 0.030(3) -0.002(2) -0.007(2) 0.003(3) O5 0.024(3) 0.021(2) 0.032(3) -0.006(2) -0.006(2) 0.001(2) O6 0.026(3) 0.038(3) 0.029(3) 0.006(2) 0.005(2) -0.002(2) O7 0.055(4) 0.029(3) 0.023(3) 0.002(2) 0.001(2) 0.013(3) O8 0.033(3) 0.030(3) 0.029(3) -0.007(2) 0.001(2) 0.007(2) S1 0.0201(9) 0.0178(8) 0.0224(9) -0.0003(7) -0.0025(8) 0.0022(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O9 H9D 0.8833 . ? O9 H9B 0.8131 . ? O10 H10D 0.9080 . ? O10 H10A 0.8496 . ? Sm1 O3 2.264(5) 5_656 ? Sm1 O4 2.384(5) . ? Sm1 O7 2.400(5) . ? Sm1 O5 2.408(5) 8_755 ? Sm1 O2 2.411(4) 5_656 ? Sm1 O8 2.413(4) . ? Sm1 O1 2.440(5) 4_556 ? Sm1 O2 2.636(4) 4_556 ? Sm1 C7 2.951(7) 4_556 ? Sm1 H8A 2.4834 . ? Sm1 H8C 2.4370 . ? C1 C4 1.362(9) . ? C1 C2 1.390(8) . ? C1 S1 1.747(7) . ? C2 C3 1.358(9) . ? C2 H2 0.9300 . ? C3 C5 1.405(9) . ? C3 H3 0.9300 . ? C4 C6 1.389(9) . ? C4 H4 0.9300 . ? C5 O3 1.316(8) . ? C5 C6 1.408(9) . ? C6 C7 1.470(9) . ? C7 O1 1.268(8) . ? C7 O2 1.282(8) . ? C7 Sm1 2.951(7) 4_456 ? O1 Sm1 2.440(5) 4_456 ? O2 Sm1 2.411(4) 5_656 ? O2 Sm1 2.636(4) 4_456 ? O3 Sm1 2.264(5) 5_656 ? O4 S1 1.460(4) . ? O5 S1 1.458(5) . ? O5 Sm1 2.408(5) 8_765 ? O6 S1 1.441(5) . ? O7 H7A 0.8500 . ? O7 H7C 0.8500 . ? O8 H8A 0.8500 . ? O8 H8C 0.8501 . ? 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 H9D O9 H9B 109.8 . . ? H10D O10 H10A 104.3 . . ? O3 Sm1 O4 77.85(16) 5_656 . ? O3 Sm1 O7 80.80(17) 5_656 . ? O4 Sm1 O7 136.59(15) . . ? O3 Sm1 O5 131.26(16) 5_656 8_755 ? O4 Sm1 O5 75.36(14) . 8_755 ? O7 Sm1 O5 143.49(16) . 8_755 ? O3 Sm1 O2 71.88(15) 5_656 5_656 ? O4 Sm1 O2 98.71(15) . 5_656 ? O7 Sm1 O2 109.86(16) . 5_656 ? O5 Sm1 O2 72.91(15) 8_755 5_656 ? O3 Sm1 O8 125.30(16) 5_656 . ? O4 Sm1 O8 151.97(16) . . ? O7 Sm1 O8 68.65(16) . . ? O5 Sm1 O8 76.99(16) 8_755 . ? O2 Sm1 O8 77.33(15) 5_656 . ? O3 Sm1 O1 139.20(16) 5_656 4_556 ? O4 Sm1 O1 87.42(16) . 4_556 ? O7 Sm1 O1 84.66(17) . 4_556 ? O5 Sm1 O1 79.10(16) 8_755 4_556 ? O2 Sm1 O1 148.65(16) 5_656 4_556 ? O8 Sm1 O1 82.92(15) . 4_556 ? O3 Sm1 O2 88.52(15) 5_656 4_556 ? O4 Sm1 O2 72.25(14) . 4_556 ? O7 Sm1 O2 69.83(15) . 4_556 ? O5 Sm1 O2 119.98(14) 8_755 4_556 ? O2 Sm1 O2 159.93(8) 5_656 4_556 ? O8 Sm1 O2 119.10(14) . 4_556 ? O1 Sm1 O2 50.69(15) 4_556 4_556 ? O3 Sm1 C7 114.25(17) 5_656 4_556 ? O4 Sm1 C7 79.74(17) . 4_556 ? O7 Sm1 C7 75.32(17) . 4_556 ? O5 Sm1 C7 100.05(16) 8_755 4_556 ? O2 Sm1 C7 172.94(16) 5_656 4_556 ? O8 Sm1 C7 100.75(17) . 4_556 ? O1 Sm1 C7 24.97(16) 4_556 4_556 ? O2 Sm1 C7 25.74(15) 4_556 4_556 ? O3 Sm1 H8A 105.9 5_656 . ? O4 Sm1 H8A 157.9 . . ? O7 Sm1 H8A 65.0 . . ? O5 Sm1 H8A 86.6 8_755 . ? O2 Sm1 H8A 63.1 5_656 . ? O8 Sm1 H8A 19.9 . . ? O1 Sm1 H8A 101.9 4_556 . ? O2 Sm1 H8A 129.0 4_556 . ? C7 Sm1 H8A 116.6 4_556 . ? O3 Sm1 H8C 134.7 5_656 . ? O4 Sm1 H8C 132.3 . . ? O7 Sm1 H8C 88.7 . . ? O5 Sm1 H8C 57.0 8_755 . ? O2 Sm1 H8C 70.7 5_656 . ? O8 Sm1 H8C 20.2 . . ? O1 Sm1 H8C 82.4 4_556 . ? O2 Sm1 H8C 128.7 4_556 . ? C7 Sm1 H8C 105.1 4_556 . ? H8A Sm1 H8C 32.8 . . ? C4 C1 C2 119.3(6) . . ? C4 C1 S1 120.3(5) . . ? C2 C1 S1 120.4(5) . . ? C3 C2 C1 119.7(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C5 122.6(6) . . ? C2 C3 H3 118.7 . . ? C5 C3 H3 118.7 . . ? C1 C4 C6 122.0(6) . . ? C1 C4 H4 119.0 . . ? C6 C4 H4 119.0 . . ? O3 C5 C3 119.5(6) . . ? O3 C5 C6 123.5(6) . . ? C3 C5 C6 117.0(6) . . ? C4 C6 C5 119.5(6) . . ? C4 C6 C7 117.2(6) . . ? C5 C6 C7 123.2(6) . . ? O1 C7 O2 117.5(6) . . ? O1 C7 C6 120.4(6) . . ? O2 C7 C6 122.0(6) . . ? O1 C7 Sm1 54.3(3) . 4_456 ? O2 C7 Sm1 63.3(3) . 4_456 ? C6 C7 Sm1 174.3(5) . 4_456 ? C7 O1 Sm1 100.7(4) . 4_456 ? C7 O2 Sm1 133.2(4) . 5_656 ? C7 O2 Sm1 91.0(4) . 4_456 ? Sm1 O2 Sm1 134.68(19) 5_656 4_456 ? C5 O3 Sm1 132.2(4) . 5_656 ? S1 O4 Sm1 143.4(3) . . ? S1 O5 Sm1 144.6(3) . 8_765 ? Sm1 O7 H7A 109.4 . . ? Sm1 O7 H7C 109.3 . . ? H7A O7 H7C 109.5 . . ? Sm1 O8 H8A 84.7 . . ? Sm1 O8 H8C 81.5 . . ? H8A O8 H8C 109.5 . . ? O6 S1 O5 112.6(3) . . ? O6 S1 O4 110.0(3) . . ? O5 S1 O4 113.2(3) . . ? O6 S1 C1 109.2(3) . . ? O5 S1 C1 105.5(3) . . ? O4 S1 C1 106.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.123 _refine_diff_density_min -1.785 _refine_diff_density_rms 0.171 # Attachment 'Tb1.cif' data_a1 _database_code_depnum_ccdc_archive 'CCDC 618896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 O8 S Tb, H2 O' _chemical_formula_sum 'C7 H9 O9 S Tb' _chemical_formula_weight 428.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.882(4) _cell_length_b 9.212(2) _cell_length_c 14.969(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2190.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 6.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.26 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10902 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2159 _reflns_number_gt 1908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2159 _refine_ls_number_parameters 169 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5502(3) 0.1861(6) 0.6219(4) 0.0184(12) Uani 1 1 d . . . C2 C 0.5652(4) 0.0391(6) 0.6463(4) 0.0200(14) Uani 1 1 d . . . C3 C 0.4981(4) -0.0587(6) 0.6331(4) 0.0231(14) Uani 1 1 d . . . H3A H 0.5065 -0.1555 0.6482 0.028 Uiso 1 1 calc R . . C4 C 0.4243(4) -0.0208(6) 0.6007(4) 0.0227(13) Uani 1 1 d . . . H4A H 0.3824 -0.0902 0.5932 0.027 Uiso 1 1 calc R . . C5 C 0.4089(3) 0.1236(6) 0.5776(4) 0.0171(11) Uani 1 1 d . . . C6 C 0.4708(3) 0.2236(6) 0.5890(4) 0.0203(12) Uani 1 1 d . . . H6A H 0.4600 0.3200 0.5744 0.024 Uiso 1 1 calc R . . C7 C 0.6138(3) 0.3011(6) 0.6293(4) 0.0180(12) Uani 1 1 d . . . O1 O 0.5936(3) 0.4308(4) 0.6157(4) 0.0322(11) Uani 1 1 d . . . O2 O 0.6917(2) 0.2738(4) 0.6463(2) 0.0190(9) Uani 1 1 d . . . O3 O 0.6376(2) -0.0054(4) 0.6787(3) 0.0230(9) Uani 1 1 d . . . O4 O 0.2755(2) 0.0474(4) 0.4924(3) 0.0241(10) Uani 1 1 d . . . O5 O 0.3305(2) 0.2904(4) 0.4683(3) 0.0219(9) Uani 1 1 d . . . O6 O 0.2591(2) 0.2276(5) 0.6049(3) 0.0287(10) Uani 1 1 d . . . O7 O 0.2079(3) 0.0311(5) 0.2037(3) 0.0345(11) Uani 1 1 d . . . H7A H 0.2342 0.1106 0.1967 0.052 Uiso 1 1 d R . . H7B H 0.2272 -0.0319 0.1676 0.052 Uiso 1 1 d R . . O8 O 0.1408(2) -0.2182(4) 0.2708(3) 0.0276(10) Uani 1 1 d . . . H8A H 0.1265 -0.2889 0.3039 0.041 Uiso 1 1 d RD . . H8C H 0.1687 -0.2497 0.2264 0.041 Uiso 1 1 d R . . O9 O 0.5640(5) 0.5981(8) 0.8886(6) 0.065(2) Uani 0.86 1 d P A 1 H9D H 0.5185 0.5498 0.8877 0.079 Uiso 0.86 1 d PR A 1 H9C H 0.5881 0.5919 0.8379 0.098 Uiso 0.86 1 d PR A 1 O10 O 0.5000 0.577(3) 0.7500 0.090(14) Uani 0.28 2 d SP B 2 H10D H 0.5281 0.5342 0.7096 0.107 Uiso 0.14 1 d PR B 2 H10B H 0.4538 0.5329 0.7584 0.134 Uiso 0.14 1 d PR B 2 S2 S 0.31189(8) 0.17715(14) 0.53307(9) 0.0173(3) Uani 1 1 d . . . Tb1 Tb 0.227150(17) -0.05275(3) 0.354863(19) 0.01879(17) 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 C1 0.015(3) 0.014(3) 0.026(3) -0.003(2) 0.002(2) -0.001(2) C2 0.020(3) 0.019(3) 0.021(3) 0.001(2) 0.003(2) 0.000(2) C3 0.023(3) 0.013(3) 0.033(4) 0.009(2) 0.002(3) 0.000(2) C4 0.025(3) 0.014(3) 0.030(4) 0.004(3) 0.001(3) -0.003(2) C5 0.018(3) 0.015(3) 0.018(3) 0.003(2) -0.002(2) 0.001(2) C6 0.028(3) 0.012(3) 0.021(3) 0.000(2) -0.003(2) 0.003(2) C7 0.022(3) 0.009(3) 0.023(3) 0.001(2) -0.001(2) 0.003(2) O1 0.017(2) 0.019(2) 0.061(3) 0.002(2) -0.004(2) -0.0017(17) O2 0.014(2) 0.016(2) 0.027(2) -0.0007(16) 0.0017(15) -0.0002(16) O3 0.018(2) 0.019(2) 0.032(2) 0.0061(19) 0.001(2) 0.0034(17) O4 0.028(3) 0.018(2) 0.026(3) 0.0001(17) -0.0093(18) -0.0047(15) O5 0.0239(19) 0.0191(19) 0.023(2) 0.0058(17) -0.0068(17) -0.0013(17) O6 0.025(2) 0.031(2) 0.030(3) -0.004(2) 0.006(2) -0.0033(18) O7 0.054(3) 0.028(2) 0.022(2) -0.001(2) -0.003(2) -0.014(2) O8 0.034(2) 0.022(2) 0.026(2) 0.0045(18) -0.0037(19) -0.0102(19) O9 0.062(4) 0.048(4) 0.086(6) -0.004(4) 0.036(4) -0.014(4) O10 0.043(18) 0.06(2) 0.17(4) 0.000 0.04(2) 0.000 S2 0.0178(7) 0.0159(7) 0.0180(7) 0.0011(5) -0.0036(5) -0.0025(5) Tb1 0.0176(2) 0.0166(2) 0.0222(2) 0.00051(10) 0.00031(10) 0.00005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.397(8) . ? C1 C2 1.422(8) . ? C1 C7 1.468(8) . ? C2 O3 1.313(8) . ? C2 C3 1.410(9) . ? C3 C4 1.316(9) . ? C3 H3A 0.9300 . ? C4 C5 1.396(8) . ? C4 H4A 0.9300 . ? C5 C6 1.358(8) . ? C5 S2 1.750(5) . ? C6 H6A 0.9300 . ? C7 O1 1.254(6) . ? C7 O2 1.288(7) . ? C7 Tb1 2.945(5) 4_556 ? O1 Tb1 2.441(4) 4_556 ? O2 Tb1 2.410(4) 5_656 ? O2 Tb1 2.631(4) 4_556 ? O3 Tb1 2.271(4) 5_656 ? O4 S2 1.460(4) . ? O4 Tb1 2.384(5) . ? O5 S2 1.455(4) . ? O5 Tb1 2.410(4) 8_665 ? O6 S2 1.440(4) . ? O7 Tb1 2.410(5) . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 Tb1 2.406(4) . ? O8 H8A 0.8501 . ? O8 H8C 0.8500 . ? O9 H9D 0.8499 . ? O9 H9C 0.8501 . ? O10 H10D 0.8500 . ? O10 H10B 0.8500 . ? Tb1 O3 2.271(4) 5_656 ? Tb1 O5 2.410(4) 8_655 ? Tb1 O2 2.410(4) 5_656 ? Tb1 O1 2.441(4) 4_456 ? Tb1 O2 2.631(4) 4_456 ? Tb1 C7 2.945(5) 4_456 ? 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 C6 C1 C2 118.5(5) . . ? C6 C1 C7 118.0(5) . . ? C2 C1 C7 123.5(5) . . ? O3 C2 C3 120.9(5) . . ? O3 C2 C1 122.6(5) . . ? C3 C2 C1 116.4(6) . . ? C4 C3 C2 123.8(5) . . ? C4 C3 H3A 118.1 . . ? C2 C3 H3A 118.1 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 119.3(5) . . ? C6 C5 S2 119.6(4) . . ? C4 C5 S2 121.1(4) . . ? C5 C6 C1 122.0(5) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O1 C7 O2 117.7(5) . . ? O1 C7 C1 119.9(5) . . ? O2 C7 C1 122.3(5) . . ? O1 C7 Tb1 54.5(3) . 4_556 ? O2 C7 Tb1 63.3(3) . 4_556 ? C1 C7 Tb1 174.2(4) . 4_556 ? C7 O1 Tb1 100.7(4) . 4_556 ? C7 O2 Tb1 132.6(4) . 5_656 ? C7 O2 Tb1 90.8(3) . 4_556 ? Tb1 O2 Tb1 135.30(16) 5_656 4_556 ? C2 O3 Tb1 132.3(4) . 5_656 ? S2 O4 Tb1 143.5(3) . . ? S2 O5 Tb1 145.4(2) . 8_665 ? Tb1 O7 H7A 109.3 . . ? Tb1 O7 H7B 109.4 . . ? H7A O7 H7B 109.5 . . ? Tb1 O8 H8A 109.4 . . ? Tb1 O8 H8C 109.1 . . ? H8A O8 H8C 109.5 . . ? H9D O9 H9C 109.5 . . ? H10D O10 H10B 109.5 . . ? O6 S2 O5 112.6(3) . . ? O6 S2 O4 110.2(3) . . ? O5 S2 O4 113.0(3) . . ? O6 S2 C5 108.6(3) . . ? O5 S2 C5 106.1(2) . . ? O4 S2 C5 106.0(2) . . ? O3 Tb1 O4 78.15(15) 5_656 . ? O3 Tb1 O8 124.97(15) 5_656 . ? O4 Tb1 O8 151.75(14) . . ? O3 Tb1 O5 131.04(14) 5_656 8_655 ? O4 Tb1 O5 75.26(14) . 8_655 ? O8 Tb1 O5 76.85(14) . 8_655 ? O3 Tb1 O7 80.60(17) 5_656 . ? O4 Tb1 O7 136.71(15) . . ? O8 Tb1 O7 68.87(15) . . ? O5 Tb1 O7 143.65(15) 8_655 . ? O3 Tb1 O2 72.05(14) 5_656 5_656 ? O4 Tb1 O2 99.25(13) . 5_656 ? O8 Tb1 O2 76.46(14) . 5_656 ? O5 Tb1 O2 72.64(12) 8_655 5_656 ? O7 Tb1 O2 109.37(15) . 5_656 ? O3 Tb1 O1 138.92(14) 5_656 4_456 ? O4 Tb1 O1 86.92(17) . 4_456 ? O8 Tb1 O1 83.71(15) . 4_456 ? O5 Tb1 O1 79.56(14) 8_655 4_456 ? O7 Tb1 O1 84.93(18) . 4_456 ? O2 Tb1 O1 148.77(13) 5_656 4_456 ? O3 Tb1 O2 88.31(13) 5_656 4_456 ? O4 Tb1 O2 72.35(13) . 4_456 ? O8 Tb1 O2 119.56(13) . 4_456 ? O5 Tb1 O2 120.60(13) 8_655 4_456 ? O7 Tb1 O2 69.73(14) . 4_456 ? O2 Tb1 O2 160.01(7) 5_656 4_456 ? O1 Tb1 O2 50.62(13) 4_456 4_456 ? O3 Tb1 C7 114.22(15) 5_656 4_456 ? O4 Tb1 C7 79.81(15) . 4_456 ? O8 Tb1 C7 101.09(15) . 4_456 ? O5 Tb1 C7 100.56(14) 8_655 4_456 ? O7 Tb1 C7 75.26(16) . 4_456 ? O2 Tb1 C7 173.10(14) 5_656 4_456 ? O1 Tb1 C7 24.74(14) 4_456 4_456 ? O2 Tb1 C7 25.93(14) 4_456 4_456 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.416 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.161 # Attachment 'Yb1.cif' data_b1 _database_code_depnum_ccdc_archive 'CCDC 618897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 O8 S Yb, H2 O' _chemical_formula_sum 'C7 H9 O9 S Yb' _chemical_formula_weight 442.24 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' S S 0.1246 0.1234 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 8.782(2) _cell_length_b 8.701(2) _cell_length_c 14.038(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.730(5) _cell_angle_gamma 90.00 _cell_volume 1053.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 777 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.41 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 9.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.33 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5482 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2056 _reflns_number_gt 1707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2056 _refine_ls_number_parameters 163 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.284 _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 C1 C 0.5305(12) 0.3318(12) 0.1452(8) 0.018(2) Uani 1 1 d . . . C2 C 0.5475(11) 0.4787(12) 0.1887(8) 0.016(2) Uani 1 1 d . . . C3 C 0.6466(12) 0.5855(12) 0.1535(8) 0.022(3) Uani 1 1 d . . . H3 H 0.6620 0.6822 0.1820 0.027 Uiso 1 1 calc R . . C4 C 0.7195(12) 0.5488(12) 0.0789(8) 0.021(2) Uani 1 1 d . . . H4 H 0.7847 0.6198 0.0574 0.025 Uiso 1 1 calc R . . C5 C 0.6969(11) 0.4079(12) 0.0356(7) 0.016(2) Uani 1 1 d . . . C6 C 0.6054(12) 0.3008(13) 0.0681(8) 0.021(2) Uani 1 1 d . . . H6 H 0.5927 0.2051 0.0381 0.025 Uiso 1 1 calc R . . C7 C 0.4416(12) 0.2072(13) 0.1788(7) 0.019(2) Uani 1 1 d . . . O1 O 0.4624(8) 0.0718(8) 0.1556(6) 0.0229(18) Uani 1 1 d . . . O2 O 0.3376(8) 0.2341(8) 0.2302(5) 0.0210(17) Uani 1 1 d . . . O3 O 0.4795(8) 0.5188(8) 0.2625(5) 0.0202(17) Uani 1 1 d . . . O4 O 0.8048(8) 0.4834(8) -0.1178(5) 0.0206(17) Uani 1 1 d . . . O5 O 0.9498(8) 0.3023(8) -0.0075(5) 0.0224(17) Uani 1 1 d . . . O6 O 0.7078(8) 0.2262(8) -0.1080(5) 0.0224(17) Uani 1 1 d . . . O7 O 0.3553(8) 0.5612(8) 0.4238(5) 0.029(2) Uani 1 1 d . . . H7C H 0.4533 0.5518 0.4334 0.034 Uiso 1 1 d RD . . H7B H 0.3274 0.6546 0.4157 0.043 Uiso 1 1 d RD . . O8 O 0.0200(8) 0.3282(9) 0.2054(5) 0.0238(18) Uani 1 1 d . . . H8A H 0.0245 0.3140 0.1461 0.036 Uiso 1 1 d R . . H8B H 0.0154 0.2418 0.2330 0.036 Uiso 1 1 d R . . O9 O 0.2417(10) 0.5486(10) 0.5998(6) 0.044(2) Uani 1 1 d . . . H9D H 0.2772 0.5505 0.5475 0.052 Uiso 1 1 d RD . . H9A H 0.3050 0.5931 0.6445 0.065 Uiso 1 1 d R . . S1 S 0.7973(3) 0.3501(3) -0.05524(19) 0.0155(6) Uani 1 1 d . . . Yb1 Yb 0.23957(5) 0.45778(5) 0.28048(3) 0.01576(17) 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 C1 0.019(5) 0.016(6) 0.020(6) -0.002(5) 0.005(5) 0.001(5) C2 0.011(5) 0.016(6) 0.020(6) 0.003(5) 0.000(4) 0.003(4) C3 0.024(6) 0.019(6) 0.026(7) -0.007(5) 0.010(5) -0.011(5) C4 0.019(5) 0.016(6) 0.031(7) -0.001(5) 0.012(5) -0.005(5) C5 0.017(5) 0.019(6) 0.014(6) 0.005(4) 0.007(4) 0.006(4) C6 0.020(6) 0.018(6) 0.026(6) -0.002(5) 0.006(5) 0.002(5) C7 0.021(6) 0.017(6) 0.017(6) -0.002(5) -0.001(5) 0.002(5) O1 0.028(4) 0.014(4) 0.032(5) 0.000(3) 0.021(4) -0.003(3) O2 0.021(4) 0.018(4) 0.028(4) 0.004(3) 0.016(3) 0.000(3) O3 0.017(4) 0.019(4) 0.027(4) -0.008(3) 0.010(3) 0.003(3) O4 0.026(4) 0.019(4) 0.019(4) 0.001(3) 0.011(3) -0.004(3) O5 0.018(4) 0.023(4) 0.026(4) 0.001(4) 0.003(3) 0.004(3) O6 0.027(4) 0.019(4) 0.025(4) -0.004(3) 0.014(4) -0.004(3) O7 0.026(4) 0.026(5) 0.035(5) -0.005(4) 0.008(4) 0.000(4) O8 0.030(4) 0.024(5) 0.018(4) 0.004(3) 0.006(3) -0.001(3) O9 0.053(6) 0.051(6) 0.028(5) -0.010(4) 0.009(4) -0.011(5) S1 0.0162(13) 0.0150(14) 0.0164(14) 0.0000(11) 0.0057(11) -0.0011(11) Yb1 0.0170(3) 0.0145(3) 0.0173(3) 0.0004(2) 0.00735(18) 0.0009(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 C1 C6 1.394(14) . ? C1 C2 1.413(14) . ? C1 C7 1.464(15) . ? C2 O3 1.335(12) . ? C2 C3 1.423(14) . ? C3 C4 1.363(15) . ? C3 H3 0.9300 . ? C4 C5 1.366(15) . ? C4 H4 0.9300 . ? C5 C6 1.363(14) . ? C5 S1 1.754(10) . ? C6 H6 0.9300 . ? C7 O1 1.245(12) . ? C7 O2 1.287(12) . ? C7 Yb1 2.812(11) 2_545 ? O1 Yb1 2.350(7) 2_545 ? O2 Yb1 2.292(7) . ? O2 Yb1 2.495(7) 2_545 ? O3 Yb1 2.232(7) . ? O4 S1 1.464(7) . ? O4 Yb1 2.301(7) 3_665 ? O5 S1 1.442(7) . ? O6 S1 1.453(7) . ? O6 Yb1 2.292(7) 4_665 ? O7 Yb1 2.265(7) . ? O7 H7C 0.8500 . ? O7 H7B 0.8499 . ? O8 Yb1 2.312(7) . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? O9 H9D 0.8500 . ? O9 H9A 0.8501 . ? Yb1 O6 2.292(7) 4_566 ? Yb1 O4 2.301(7) 3_665 ? Yb1 O1 2.350(7) 2 ? Yb1 O2 2.495(7) 2 ? Yb1 C7 2.812(11) 2 ? Yb1 H7C 2.7018 . ? Yb1 H7B 2.5661 . ? Yb1 H8A 2.7136 . ? Yb1 H8B 2.7131 . ? 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 C6 C1 C2 118.9(10) . . ? C6 C1 C7 117.6(10) . . ? C2 C1 C7 123.4(10) . . ? O3 C2 C1 123.1(9) . . ? O3 C2 C3 119.3(9) . . ? C1 C2 C3 117.6(10) . . ? C4 C3 C2 121.2(10) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.2(10) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.7(10) . . ? C6 C5 S1 117.0(8) . . ? C4 C5 S1 122.0(8) . . ? C5 C6 C1 121.3(10) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? O1 C7 O2 118.2(10) . . ? O1 C7 C1 120.3(10) . . ? O2 C7 C1 121.5(10) . . ? O1 C7 Yb1 55.8(5) . 2_545 ? O2 C7 Yb1 62.5(6) . 2_545 ? C1 C7 Yb1 173.0(7) . 2_545 ? C7 O1 Yb1 98.2(7) . 2_545 ? C7 O2 Yb1 132.4(7) . . ? C7 O2 Yb1 90.2(6) . 2_545 ? Yb1 O2 Yb1 136.3(3) . 2_545 ? C2 O3 Yb1 126.4(6) . . ? S1 O4 Yb1 138.9(4) . 3_665 ? S1 O6 Yb1 138.0(4) . 4_665 ? Yb1 O7 H7C 112.1 . . ? Yb1 O7 H7B 101.0 . . ? H7C O7 H7B 111.8 . . ? Yb1 O8 H8A 109.3 . . ? Yb1 O8 H8B 109.2 . . ? H8A O8 H8B 109.5 . . ? H9D O9 H9A 109.5 . . ? O5 S1 O6 113.0(4) . . ? O5 S1 O4 111.5(4) . . ? O6 S1 O4 111.2(4) . . ? O5 S1 C5 107.1(4) . . ? O6 S1 C5 106.6(5) . . ? O4 S1 C5 107.1(5) . . ? O3 Yb1 O7 74.3(3) . . ? O3 Yb1 O2 75.6(3) . . ? O7 Yb1 O2 118.6(3) . . ? O3 Yb1 O6 118.7(3) . 4_566 ? O7 Yb1 O6 76.3(3) . 4_566 ? O2 Yb1 O6 73.6(2) . 4_566 ? O3 Yb1 O4 79.9(3) . 3_665 ? O7 Yb1 O4 139.3(3) . 3_665 ? O2 Yb1 O4 83.5(3) . 3_665 ? O6 Yb1 O4 144.4(3) 4_566 3_665 ? O3 Yb1 O8 142.1(3) . . ? O7 Yb1 O8 142.9(3) . . ? O2 Yb1 O8 77.0(3) . . ? O6 Yb1 O8 76.9(3) 4_566 . ? O4 Yb1 O8 71.5(2) 3_665 . ? O3 Yb1 O1 137.5(3) . 2 ? O7 Yb1 O1 74.9(3) . 2 ? O2 Yb1 O1 146.0(2) . 2 ? O6 Yb1 O1 80.7(2) 4_566 2 ? O4 Yb1 O1 106.5(3) 3_665 2 ? O8 Yb1 O1 75.8(3) . 2 ? O3 Yb1 O2 90.9(2) . 2 ? O7 Yb1 O2 75.1(2) . 2 ? O2 Yb1 O2 155.95(10) . 2 ? O6 Yb1 O2 130.4(2) 4_566 2 ? O4 Yb1 O2 74.5(2) 3_665 2 ? O8 Yb1 O2 104.4(2) . 2 ? O1 Yb1 O2 53.2(2) 2 2 ? O3 Yb1 C7 114.9(3) . 2 ? O7 Yb1 C7 71.9(3) . 2 ? O2 Yb1 C7 167.7(3) . 2 ? O6 Yb1 C7 104.8(3) 4_566 2 ? O4 Yb1 C7 91.9(3) 3_665 2 ? O8 Yb1 C7 90.8(3) . 2 ? O1 Yb1 C7 26.0(3) 2 2 ? O2 Yb1 C7 27.2(3) 2 2 ? O3 Yb1 H7C 59.1 . . ? O7 Yb1 H7C 17.0 . . ? O2 Yb1 H7C 104.9 . . ? O6 Yb1 H7C 79.9 4_566 . ? O4 Yb1 H7C 133.2 3_665 . ? O8 Yb1 H7C 155.1 . . ? O1 Yb1 H7C 91.8 2 . ? O2 Yb1 H7C 84.1 2 . ? C7 Yb1 H7C 86.6 2 . ? O3 Yb1 H7B 76.4 . . ? O7 Yb1 H7B 19.0 . . ? O2 Yb1 H7B 135.7 . . ? O6 Yb1 H7B 91.1 4_566 . ? O4 Yb1 H7B 123.9 3_665 . ? O8 Yb1 H7B 140.6 . . ? O1 Yb1 H7B 65.2 2 . ? O2 Yb1 H7B 56.1 2 . ? C7 Yb1 H7B 55.8 2 . ? H7C Yb1 H7B 30.9 . . ? O3 Yb1 H8A 125.5 . . ? O7 Yb1 H8A 160.0 . . ? O2 Yb1 H8A 69.3 . . ? O6 Yb1 H8A 89.7 4_566 . ? O4 Yb1 H8A 56.3 3_665 . ? O8 Yb1 H8A 17.2 . . ? O1 Yb1 H8A 89.0 2 . ? O2 Yb1 H8A 104.8 2 . ? C7 Yb1 H8A 98.6 2 . ? H7C Yb1 H8A 169.3 . . ? H7B Yb1 H8A 153.7 . . ? O3 Yb1 H8B 142.5 . . ? O7 Yb1 H8B 132.7 . . ? O2 Yb1 H8B 68.5 . . ? O6 Yb1 H8B 60.6 4_566 . ? O4 Yb1 H8B 85.9 3_665 . ? O8 Yb1 H8B 17.2 . . ? O1 Yb1 H8B 79.7 2 . ? O2 Yb1 H8B 118.4 2 . ? C7 Yb1 H8B 99.9 2 . ? H7C Yb1 H8B 140.3 . . ? H7B Yb1 H8B 138.4 . . ? H8A Yb1 H8B 29.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.873 _refine_diff_density_min -1.933 _refine_diff_density_rms 0.239