# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 O17 Pr S2' _chemical_formula_weight 860.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.4546(7) _cell_length_b 14.1658(6) _cell_length_c 9.8960(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.692(3) _cell_angle_gamma 90.00 _cell_volume 3271.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 4416 _cell_measurement_theta_min 2.9401 _cell_measurement_theta_max 29.1229 _exptl_crystal_description needle _exptl_crystal_colour lightgreen _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6963 _exptl_absorpt_correction_T_max 0.8487 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13564 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5756 _reflns_number_gt 4308 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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^+12.6827P] 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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5756 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 C14 C 0.7600(4) 0.7536(6) -0.4399(10) 0.060(3) Uani 1 1 d . . . H14A H 0.7475 0.8077 -0.4933 0.090 Uiso 1 1 calc R . . H14B H 0.7701 0.7038 -0.4989 0.090 Uiso 1 1 calc R . . H14C H 0.7928 0.7703 -0.3787 0.090 Uiso 1 1 calc R . . C2 C 0.4310(2) 0.6551(4) -0.0515(6) 0.0159(14) Uani 1 1 d . . . C26 C -0.1171(3) 0.3218(5) 0.5804(7) 0.0204(15) Uani 1 1 d . . . C1 C 0.3721(3) 0.6824(5) -0.0154(7) 0.0197(15) Uani 1 1 d . . . C5 C 0.5390(3) 0.6156(5) -0.1202(7) 0.0203(15) Uani 1 1 d . . . C23 C -0.0072(3) 0.3717(5) 0.5479(7) 0.0288(18) Uani 1 1 d . . . C27 C -0.1037(3) 0.3517(5) 0.4517(7) 0.0216(16) Uani 1 1 d . . . H27 H -0.1318 0.3540 0.3785 0.026 Uiso 1 1 calc R . . C30 C -0.1782(3) 0.2926(4) 0.5967(7) 0.0174(15) Uani 1 1 d . . . C17 C 0.1787(3) 0.4873(4) 0.1617(7) 0.0193(15) Uani 1 1 d . . . C25 C -0.0758(3) 0.3174(5) 0.6902(7) 0.0224(16) Uani 1 1 d . . . H25 H -0.0855 0.2975 0.7745 0.027 Uiso 1 1 calc R . . C7 C 0.4398(3) 0.6394(5) -0.1857(7) 0.0285(18) Uani 1 1 d . . . H7 H 0.4092 0.6425 -0.2528 0.034 Uiso 1 1 calc R . . C12 C 0.7147(3) 0.8762(5) -0.2550(7) 0.0270(17) Uani 1 1 d . . . H12 H 0.7488 0.8931 -0.2893 0.032 Uiso 1 1 calc R . . C20 C 0.1257(3) 0.3981(5) 0.3631(7) 0.0303(18) Uani 1 1 d . . . C15 C 0.7064(3) 1.0399(5) -0.1729(6) 0.0182(14) Uani 1 1 d . . . C4 C 0.5316(3) 0.6284(5) 0.0147(7) 0.0240(16) Uani 1 1 d . . . H4 H 0.5623 0.6237 0.0814 0.029 Uiso 1 1 calc R . . C11 C 0.6870(3) 0.9405(5) -0.1810(7) 0.0215(16) Uani 1 1 d . . . C16 C 0.2091(3) 0.5367(5) 0.0561(6) 0.0170(14) Uani 1 1 d . . . C6 C 0.4943(3) 0.6192(5) -0.2202(7) 0.0297(18) Uani 1 1 d . . . H6 H 0.5004 0.6082 -0.3102 0.036 Uiso 1 1 calc R . . C24 C -0.0198(3) 0.3431(5) 0.6733(7) 0.0263(17) Uani 1 1 d . . . H24 H 0.0086 0.3409 0.7459 0.032 Uiso 1 1 calc R . . C3 C 0.4768(3) 0.6488(5) 0.0483(7) 0.0228(16) Uani 1 1 d . . . H3 H 0.4708 0.6583 0.1387 0.027 Uiso 1 1 calc R . . C18 C 0.1984(3) 0.5004(5) 0.2970(7) 0.0233(16) Uani 1 1 d . . . H18 H 0.2301 0.5388 0.3196 0.028 Uiso 1 1 calc R . . C28 C -0.0478(3) 0.3778(5) 0.4367(7) 0.0266(17) Uani 1 1 d . . . C8 C 0.6424(3) 0.7627(5) -0.2267(8) 0.0286(18) Uani 1 1 d . . . C22 C 0.1321(3) 0.4286(5) 0.1283(7) 0.0306(18) Uani 1 1 d . . . H22 H 0.1189 0.4193 0.0375 0.037 Uiso 1 1 calc R . . C13 C 0.6928(3) 0.7867(5) -0.2794(8) 0.0311(19) Uani 1 1 d . . . C21 C 0.1048(3) 0.3834(5) 0.2288(8) 0.0320(18) Uani 1 1 d . . . H21 H 0.0733 0.3444 0.2065 0.038 Uiso 1 1 calc R . . C29 C -0.0717(3) 0.4375(6) 0.2114(8) 0.044(2) Uani 1 1 d . . . H29A H -0.0535 0.4629 0.1368 0.066 Uiso 1 1 calc R . . H29B H -0.0962 0.4846 0.2449 0.066 Uiso 1 1 calc R . . H29C H -0.0942 0.3835 0.1813 0.066 Uiso 1 1 calc R . . C19 C 0.1720(3) 0.4578(5) 0.3979(7) 0.0275(17) Uani 1 1 d . . . H19 H 0.1848 0.4685 0.4885 0.033 Uiso 1 1 calc R . . C10 C 0.6370(3) 0.9145(5) -0.1253(8) 0.0318(19) Uani 1 1 d . . . H10 H 0.6189 0.9568 -0.0716 0.038 Uiso 1 1 calc R . . C9 C 0.6143(3) 0.8250(5) -0.1507(8) 0.038(2) Uani 1 1 d . . . H9 H 0.5803 0.8075 -0.1165 0.046 Uiso 1 1 calc R . . O16 O -0.21517(17) 0.2999(3) 0.4976(5) 0.0199(10) Uani 1 1 d . . . O2 O 0.36603(18) 0.7002(3) 0.1057(5) 0.0248(11) Uani 1 1 d . . . O8 O 0.74814(18) 1.0683(3) -0.2335(5) 0.0229(11) Uani 1 1 d . . . O10 O 0.24178(19) 0.6018(3) 0.0821(5) 0.0249(11) Uani 1 1 d . . . O5 O 0.65023(18) 0.5967(3) -0.0585(6) 0.0359(13) Uani 1 1 d . . . O3 O 0.33239(17) 0.6867(3) -0.1098(5) 0.0247(11) Uani 1 1 d . . . O9 O 0.67893(17) 1.0991(3) -0.1048(4) 0.0186(10) Uani 1 1 d . . . O1 O 0.31992(17) 0.6194(3) 0.3345(5) 0.0236(11) Uani 1 1 d . . . H1A H 0.3036 0.6161 0.4073 0.035 Uiso 1 1 d R . . H1B H 0.3146 0.5683 0.2901 0.035 Uiso 1 1 d R . . O17 O -0.18850(17) 0.2639(3) 0.7124(5) 0.0233(11) Uani 1 1 d . . . O11 O 0.19728(19) 0.5016(3) -0.0666(5) 0.0248(11) Uani 1 1 d . . . H11 H 0.2172 0.5278 -0.1191 0.037 Uiso 1 1 calc R . . O4 O 0.60294(19) 0.5114(3) -0.2580(6) 0.0359(14) Uani 1 1 d . . . O6 O 0.61677(19) 0.6754(3) -0.2726(5) 0.0304(12) Uani 1 1 d . . . O14 O 0.04886(19) 0.4076(4) 0.5314(5) 0.0348(13) Uani 1 1 d . . . O12 O 0.1372(2) 0.3307(4) 0.6103(5) 0.0453(15) Uani 1 1 d . . . O15 O -0.02925(19) 0.4102(4) 0.3171(5) 0.0356(13) Uani 1 1 d . . . O7 O 0.7141(2) 0.7219(4) -0.3628(7) 0.0539(18) Uani 1 1 d . . . O13 O 0.0695(2) 0.2515(3) 0.4415(5) 0.0309(12) Uani 1 1 d . . . S1 S 0.60764(7) 0.59223(12) -0.1707(2) 0.0250(4) Uani 1 1 d . . . S2 S 0.09549(7) 0.33498(14) 0.4943(2) 0.0303(5) Uani 1 1 d . . . Pr1 Pr 0.277824(13) 0.75367(2) 0.19245(3) 0.01318(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 C14 0.044(5) 0.052(6) 0.089(8) -0.029(6) 0.036(5) -0.008(4) C2 0.017(3) 0.015(3) 0.017(4) 0.000(3) 0.006(3) 0.005(3) C26 0.017(3) 0.020(4) 0.025(4) -0.002(3) 0.011(3) -0.005(3) C1 0.017(3) 0.017(4) 0.026(4) 0.000(3) 0.008(3) -0.004(3) C5 0.015(3) 0.019(4) 0.029(4) -0.003(3) 0.009(3) 0.001(3) C23 0.014(3) 0.046(5) 0.028(4) -0.008(4) 0.010(3) -0.014(3) C27 0.019(3) 0.033(4) 0.013(4) -0.009(3) 0.002(3) -0.006(3) C30 0.020(3) 0.012(3) 0.021(4) -0.005(3) 0.010(3) 0.001(3) C17 0.020(3) 0.016(3) 0.022(4) 0.001(3) 0.007(3) -0.004(3) C25 0.021(3) 0.032(4) 0.014(4) 0.001(3) 0.004(3) -0.002(3) C7 0.016(3) 0.051(5) 0.018(4) -0.001(4) 0.001(3) 0.011(3) C12 0.024(4) 0.022(4) 0.036(5) -0.009(4) 0.009(3) -0.006(3) C20 0.021(4) 0.042(5) 0.029(4) 0.009(4) 0.006(3) -0.009(3) C15 0.024(3) 0.022(4) 0.008(3) 0.001(3) -0.001(3) -0.003(3) C4 0.017(3) 0.028(4) 0.026(4) -0.002(3) -0.002(3) 0.001(3) C11 0.022(3) 0.016(4) 0.028(4) -0.001(3) 0.008(3) 0.000(3) C16 0.019(3) 0.019(4) 0.014(4) 0.002(3) 0.007(3) 0.003(3) C6 0.024(4) 0.045(5) 0.022(4) -0.006(4) 0.012(3) 0.009(3) C24 0.018(3) 0.036(4) 0.025(4) -0.002(4) 0.005(3) -0.006(3) C3 0.023(4) 0.035(4) 0.011(4) -0.005(3) 0.002(3) -0.005(3) C18 0.023(3) 0.022(4) 0.025(4) -0.002(3) 0.003(3) -0.003(3) C28 0.026(4) 0.037(4) 0.019(4) 0.001(4) 0.013(3) -0.007(3) C8 0.029(4) 0.014(4) 0.044(5) 0.003(4) 0.011(3) -0.004(3) C22 0.029(4) 0.041(5) 0.023(4) -0.004(4) 0.007(3) -0.015(3) C13 0.032(4) 0.023(4) 0.043(5) -0.011(4) 0.022(4) 0.001(3) C21 0.030(4) 0.031(4) 0.035(5) -0.007(4) 0.004(3) -0.017(3) C29 0.049(5) 0.049(5) 0.035(5) 0.010(4) 0.010(4) -0.004(4) C19 0.028(4) 0.033(4) 0.022(4) 0.000(4) 0.007(3) -0.008(3) C10 0.031(4) 0.027(4) 0.039(5) -0.014(4) 0.014(4) 0.001(3) C9 0.030(4) 0.032(4) 0.058(6) -0.010(4) 0.029(4) -0.010(3) O16 0.013(2) 0.025(3) 0.023(3) -0.003(2) 0.005(2) -0.0010(19) O2 0.023(2) 0.030(3) 0.023(3) -0.008(2) 0.012(2) -0.002(2) O8 0.029(3) 0.017(2) 0.025(3) -0.004(2) 0.015(2) -0.003(2) O10 0.034(3) 0.021(3) 0.021(3) -0.006(2) 0.008(2) -0.012(2) O5 0.012(2) 0.031(3) 0.064(4) -0.008(3) -0.002(2) 0.004(2) O3 0.017(2) 0.033(3) 0.026(3) 0.010(2) 0.008(2) 0.006(2) O9 0.022(2) 0.018(2) 0.017(3) -0.002(2) 0.0088(19) -0.0018(19) O1 0.029(3) 0.021(3) 0.022(3) -0.003(2) 0.008(2) 0.007(2) O17 0.015(2) 0.033(3) 0.022(3) 0.005(2) 0.0058(19) -0.003(2) O11 0.031(3) 0.026(3) 0.020(3) -0.006(2) 0.013(2) -0.010(2) O4 0.031(3) 0.021(3) 0.058(4) -0.014(3) 0.019(3) 0.002(2) O6 0.029(3) 0.028(3) 0.036(3) -0.004(3) 0.014(2) -0.010(2) O14 0.025(3) 0.039(3) 0.041(3) -0.004(3) 0.009(2) -0.012(2) O12 0.030(3) 0.065(4) 0.039(3) 0.021(3) -0.008(2) -0.010(3) O15 0.029(3) 0.052(4) 0.027(3) 0.008(3) 0.009(2) -0.007(2) O7 0.042(3) 0.039(4) 0.084(5) -0.017(3) 0.026(3) -0.007(3) O13 0.036(3) 0.022(3) 0.035(3) 0.006(3) 0.009(2) -0.001(2) S1 0.0184(9) 0.0195(9) 0.0389(12) -0.0034(9) 0.0116(8) 0.0011(7) S2 0.0269(10) 0.0337(11) 0.0304(11) 0.0082(9) 0.0028(8) -0.0037(8) Pr1 0.01152(18) 0.0149(2) 0.0139(2) 0.00012(16) 0.00522(13) -0.00120(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 C14 O7 1.451(9) . ? C2 C7 1.382(9) . ? C2 C3 1.389(9) . ? C2 C1 1.511(8) . ? C26 C25 1.382(9) . ? C26 C27 1.407(9) . ? C26 C30 1.514(8) . ? C1 O2 1.247(8) . ? C1 O3 1.254(8) . ? C5 C6 1.369(9) . ? C5 C4 1.376(9) . ? C5 S1 1.765(6) . ? C23 C24 1.365(9) . ? C23 C28 1.385(10) . ? C23 O14 1.434(7) . ? C27 C28 1.385(8) . ? C30 O16 1.248(8) . ? C30 O17 1.261(7) . ? C17 C18 1.385(9) . ? C17 C22 1.388(9) . ? C17 C16 1.495(8) . ? C25 C24 1.390(8) . ? C7 C6 1.384(8) . ? C12 C11 1.372(9) . ? C12 C13 1.379(9) . ? C20 C21 1.386(10) . ? C20 C19 1.393(9) . ? C20 S2 1.781(7) . ? C15 O8 1.264(7) . ? C15 O9 1.288(7) . ? C15 C11 1.479(9) . ? C15 Pr1 2.956(7) 3_675 ? C4 C3 1.387(8) . ? C11 C10 1.395(9) . ? C16 O10 1.211(7) . ? C16 O11 1.316(7) . ? C18 C19 1.366(9) . ? C28 O15 1.379(8) . ? C8 C9 1.371(9) . ? C8 C13 1.380(9) . ? C8 O6 1.428(8) . ? C22 C21 1.391(9) . ? C13 O7 1.362(8) . ? C29 O15 1.425(9) . ? C10 C9 1.388(10) . ? O16 Pr1 2.362(5) 2_545 ? O2 Pr1 2.438(4) . ? O8 Pr1 2.635(4) 3_675 ? O10 Pr1 2.520(4) . ? O5 S1 1.420(5) . ? O3 Pr1 2.384(5) 4_575 ? O9 Pr1 2.511(4) 3_675 ? O1 Pr1 2.508(4) . ? O17 Pr1 2.394(4) 3_566 ? O4 S1 1.432(5) . ? O6 S1 1.579(5) . ? O14 S2 1.571(5) . ? O12 S2 1.434(5) . ? O13 S2 1.407(5) . ? Pr1 O16 2.362(5) 2 ? Pr1 O3 2.384(5) 4_576 ? Pr1 O17 2.394(4) 3_566 ? Pr1 O9 2.511(4) 3_675 ? Pr1 O8 2.635(4) 3_675 ? Pr1 C15 2.956(7) 3_675 ? 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 C7 C2 C3 119.6(6) . . ? C7 C2 C1 119.7(6) . . ? C3 C2 C1 120.6(6) . . ? C25 C26 C27 121.6(6) . . ? C25 C26 C30 120.0(6) . . ? C27 C26 C30 118.4(6) . . ? O2 C1 O3 124.0(6) . . ? O2 C1 C2 118.3(6) . . ? O3 C1 C2 117.7(6) . . ? C6 C5 C4 122.4(6) . . ? C6 C5 S1 117.2(5) . . ? C4 C5 S1 120.4(5) . . ? C24 C23 C28 123.2(6) . . ? C24 C23 O14 119.5(6) . . ? C28 C23 O14 117.0(6) . . ? C28 C27 C26 118.4(6) . . ? O16 C30 O17 124.0(6) . . ? O16 C30 C26 119.0(6) . . ? O17 C30 C26 117.0(6) . . ? C18 C17 C22 119.3(6) . . ? C18 C17 C16 118.5(6) . . ? C22 C17 C16 122.2(6) . . ? C26 C25 C24 119.4(6) . . ? C2 C7 C6 120.0(6) . . ? C11 C12 C13 121.0(6) . . ? C21 C20 C19 121.4(6) . . ? C21 C20 S2 119.7(5) . . ? C19 C20 S2 118.8(6) . . ? O8 C15 O9 119.5(6) . . ? O8 C15 C11 121.7(6) . . ? O9 C15 C11 118.8(5) . . ? O8 C15 Pr1 63.0(3) . 3_675 ? O9 C15 Pr1 57.5(3) . 3_675 ? C11 C15 Pr1 167.9(5) . 3_675 ? C5 C4 C3 117.9(6) . . ? C12 C11 C10 119.8(6) . . ? C12 C11 C15 120.1(6) . . ? C10 C11 C15 119.7(6) . . ? O10 C16 O11 123.7(6) . . ? O10 C16 C17 122.9(6) . . ? O11 C16 C17 113.4(5) . . ? C5 C6 C7 119.3(6) . . ? C23 C24 C25 118.6(6) . . ? C4 C3 C2 120.8(6) . . ? C19 C18 C17 121.0(6) . . ? O15 C28 C23 116.9(6) . . ? O15 C28 C27 124.3(6) . . ? C23 C28 C27 118.8(6) . . ? C9 C8 C13 121.6(6) . . ? C9 C8 O6 121.4(6) . . ? C13 C8 O6 116.3(6) . . ? C17 C22 C21 120.9(7) . . ? O7 C13 C12 124.9(6) . . ? O7 C13 C8 116.2(6) . . ? C12 C13 C8 118.6(6) . . ? C20 C21 C22 118.1(6) . . ? C18 C19 C20 119.1(7) . . ? C9 C10 C11 119.5(6) . . ? C8 C9 C10 119.4(6) . . ? C30 O16 Pr1 158.8(4) . 2_545 ? C1 O2 Pr1 125.7(4) . . ? C15 O8 Pr1 91.7(4) . 3_675 ? C16 O10 Pr1 157.0(4) . . ? C1 O3 Pr1 158.1(4) . 4_575 ? C15 O9 Pr1 96.9(3) . 3_675 ? C30 O17 Pr1 130.2(4) . 3_566 ? C8 O6 S1 121.5(5) . . ? C23 O14 S2 117.5(4) . . ? C28 O15 C29 117.6(5) . . ? C13 O7 C14 116.5(6) . . ? O5 S1 O4 120.9(3) . . ? O5 S1 O6 109.7(3) . . ? O4 S1 O6 102.6(3) . . ? O5 S1 C5 111.2(3) . . ? O4 S1 C5 107.6(3) . . ? O6 S1 C5 103.1(3) . . ? O13 S2 O12 119.9(3) . . ? O13 S2 O14 110.6(3) . . ? O12 S2 O14 106.1(3) . . ? O13 S2 C20 109.9(3) . . ? O12 S2 C20 108.4(3) . . ? O14 S2 C20 100.3(3) . . ? O16 Pr1 O3 142.77(16) 2 4_576 ? O16 Pr1 O17 80.93(14) 2 3_566 ? O3 Pr1 O17 97.67(14) 4_576 3_566 ? O16 Pr1 O2 106.77(15) 2 . ? O3 Pr1 O2 89.65(15) 4_576 . ? O17 Pr1 O2 155.89(16) 3_566 . ? O16 Pr1 O1 146.70(15) 2 . ? O3 Pr1 O1 70.08(15) 4_576 . ? O17 Pr1 O1 90.69(14) 3_566 . ? O2 Pr1 O1 70.19(15) . . ? O16 Pr1 O9 74.65(14) 2 3_675 ? O3 Pr1 O9 77.69(15) 4_576 3_675 ? O17 Pr1 O9 128.44(14) 3_566 3_675 ? O2 Pr1 O9 75.54(14) . 3_675 ? O1 Pr1 O9 132.31(14) . 3_675 ? O16 Pr1 O10 74.71(15) 2 . ? O3 Pr1 O10 141.98(16) 4_576 . ? O17 Pr1 O10 79.20(15) 3_566 . ? O2 Pr1 O10 80.92(14) . . ? O1 Pr1 O10 72.07(15) . . ? O9 Pr1 O10 133.54(14) 3_675 . ? O16 Pr1 O8 73.88(15) 2 3_675 ? O3 Pr1 O8 69.37(15) 4_576 3_675 ? O17 Pr1 O8 79.29(14) 3_566 3_675 ? O2 Pr1 O8 124.66(14) . 3_675 ? O1 Pr1 O8 136.32(15) . 3_675 ? O9 Pr1 O8 50.65(12) 3_675 3_675 ? O10 Pr1 O8 144.19(15) . 3_675 ? O16 Pr1 C15 75.27(16) 2 3_675 ? O3 Pr1 C15 69.05(17) 4_576 3_675 ? O17 Pr1 C15 104.41(16) 3_566 3_675 ? O2 Pr1 C15 99.67(16) . 3_675 ? O1 Pr1 C15 137.86(16) . 3_675 ? O9 Pr1 C15 25.63(14) 3_675 3_675 ? O10 Pr1 C15 148.75(16) . 3_675 ? O8 Pr1 C15 25.30(14) 3_675 3_675 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.501 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 956810' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Eu O17 S2' _chemical_formula_weight 871.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.428(2) _cell_length_b 14.0753(13) _cell_length_c 9.8845(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.907(8) _cell_angle_gamma 90.00 _cell_volume 3247.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 1923 _cell_measurement_theta_min 2.8885 _cell_measurement_theta_max 29.1472 _exptl_crystal_description needle _exptl_crystal_colour lightpink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6061 _exptl_absorpt_correction_T_max 0.7833 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13629 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.1342 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5719 _reflns_number_gt 3639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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. SIMU 0.01 0.02 3.8 C30 C16 C1 C12 C3 C7 C20 C4 C17 C29 C5 C21 C2 C18 C11 C6 = C13 C15 C9 C26 C23 C14 C25 C22 C19 C24 C10 C27 C8 C28 SIMU 0.01 0.02 3.8 O17 O5 O3 O16 O11 O4 O2 O1 O6 O12 O14 O7 O8 O10 O9 O15 O13 ISOR 0.005 0.001 C2 C3 C9 C12 ISOR 0.01 0.001 C25 C30 ; _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^)+(0.0294P)^2^+0.6934P] 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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5719 _refine_ls_number_parameters 455 _refine_ls_number_restraints 660 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.016 _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 C30 C -0.2611(5) 0.7578(8) 0.9422(11) 0.050(3) Uani 1 1 d U . . H30A H -0.2950 0.7678 0.8824 0.075 Uiso 1 1 calc R . . H30B H -0.2498 0.8166 0.9859 0.075 Uiso 1 1 calc R . . H30C H -0.2686 0.7115 1.0096 0.075 Uiso 1 1 calc R . . C16 C 0.1302(4) 0.6818(6) 0.5239(9) 0.0187(18) Uani 1 1 d U . . C1 C 0.3196(4) 0.7073(6) 0.0942(8) 0.0148(16) Uani 1 1 d U . . C12 C 0.6780(4) 0.5115(6) -0.3382(8) 0.0174(16) Uani 1 1 d U . . C3 C 0.4205(3) 0.6825(6) 0.1888(8) 0.0181(16) Uani 1 1 d U . . H3 H 0.4102 0.7024 0.2731 0.022 Uiso 1 1 calc R . . C7 C 0.3945(4) 0.6483(6) -0.0488(8) 0.0165(16) Uani 1 1 d U . . H7 H 0.3667 0.6450 -0.1218 0.020 Uiso 1 1 calc R . . C20 C -0.0396(4) 0.6144(6) 0.6178(9) 0.0203(16) Uani 1 1 d U . . C4 C 0.4774(4) 0.6552(6) 0.1721(9) 0.0205(17) Uani 1 1 d U . . H4 H 0.5051 0.6558 0.2454 0.025 Uiso 1 1 calc R . . C17 C 0.0714(4) 0.6561(6) 0.5562(8) 0.0204(16) Uani 1 1 d U . . C29 C -0.2062(4) 1.0424(7) 0.6666(9) 0.0242(18) Uani 1 1 d U . . C5 C 0.4911(4) 0.6282(7) 0.0479(9) 0.0219(17) Uani 1 1 d U . . C21 C -0.0297(4) 0.6273(6) 0.4862(9) 0.0229(18) Uani 1 1 d U . . H21 H -0.0595 0.6222 0.4180 0.028 Uiso 1 1 calc R . . C2 C 0.3803(4) 0.6794(6) 0.0783(8) 0.0173(16) Uani 1 1 d U . . C18 C 0.0597(4) 0.6404(7) 0.6894(9) 0.0245(17) Uani 1 1 d U . . H18 H 0.0895 0.6434 0.7577 0.029 Uiso 1 1 calc R . . C11 C 0.6987(4) 0.4996(6) -0.2031(8) 0.0198(17) Uani 1 1 d U . . H11 H 0.7304 0.4612 -0.1809 0.024 Uiso 1 1 calc R . . C6 C 0.4512(4) 0.6221(6) -0.0646(8) 0.0205(16) Uani 1 1 d U . . C13 C 0.6314(4) 0.5695(6) -0.3713(9) 0.0223(17) Uani 1 1 d U . . H13 H 0.6178 0.5772 -0.4619 0.027 Uiso 1 1 calc R . . C15 C 0.7091(4) 0.4617(7) -0.4422(9) 0.0198(17) Uani 1 1 d U . . C9 C 0.6250(4) 0.6028(7) -0.1370(9) 0.0221(17) Uani 1 1 d U . . C26 C -0.1876(4) 0.9431(7) 0.6758(9) 0.0258(17) Uani 1 1 d U . . C23 C -0.1435(4) 0.7623(7) 0.7253(10) 0.0299(18) Uani 1 1 d U . . C14 C 0.6051(4) 0.6153(6) -0.2726(8) 0.0223(17) Uani 1 1 d U . . H14 H 0.5740 0.6549 -0.2957 0.027 Uiso 1 1 calc R . . C25 C -0.2159(4) 0.8774(7) 0.7511(9) 0.0307(18) Uani 1 1 d U . . H25 H -0.2502 0.8937 0.7857 0.037 Uiso 1 1 calc R . . C22 C 0.0258(4) 0.6486(6) 0.4538(9) 0.0227(17) Uani 1 1 d U . . H22 H 0.0328 0.6579 0.3635 0.027 Uiso 1 1 calc R . . C19 C 0.0047(4) 0.6204(7) 0.7237(9) 0.0266(17) Uani 1 1 d U . . H19 H -0.0027 0.6113 0.8137 0.032 Uiso 1 1 calc R . . C24 C -0.1928(4) 0.7876(7) 0.7746(10) 0.0327(18) Uani 1 1 d U . . C10 C 0.6721(4) 0.5449(6) -0.1024(9) 0.0205(17) Uani 1 1 d U . . H10 H 0.6855 0.5369 -0.0118 0.025 Uiso 1 1 calc R . . C27 C -0.1381(4) 0.9159(7) 0.6219(10) 0.0331(18) Uani 1 1 d U . . H27 H -0.1200 0.9583 0.5674 0.040 Uiso 1 1 calc R . . C8 C 0.4288(4) 0.5605(7) -0.2897(9) 0.033(3) Uani 1 1 d U . . H8A H 0.4475 0.5294 -0.3601 0.050 Uiso 1 1 calc R . . H8B H 0.4086 0.6154 -0.3264 0.050 Uiso 1 1 calc R . . H8C H 0.4022 0.5175 -0.2536 0.050 Uiso 1 1 calc R . . C28 C -0.1137(4) 0.8247(7) 0.6471(9) 0.0317(17) Uani 1 1 d U . . H28 H -0.0794 0.8072 0.6130 0.038 Uiso 1 1 calc R . . O17 O -0.2485(2) 1.0704(4) 0.7306(5) 0.0185(14) Uani 1 1 d U . . O5 O 0.2836(2) 0.7012(4) -0.0065(5) 0.0171(14) Uani 1 1 d U . . O3 O 0.1680(2) 0.6855(4) 0.6200(6) 0.0227(15) Uani 1 1 d U . . O16 O -0.1787(2) 1.1009(4) 0.6011(5) 0.0154(13) Uani 1 1 d U . . O11 O 0.7422(3) 0.3946(4) -0.4163(6) 0.0234(15) Uani 1 1 d U . . O4 O 0.3078(2) 0.7367(4) 0.2093(5) 0.0199(14) Uani 1 1 d U . . O2 O 0.1383(2) 0.7001(4) 0.4031(5) 0.0189(14) Uani 1 1 d U . . O1 O 0.1827(2) 0.6209(4) 0.1718(6) 0.0210(15) Uani 1 1 d U . . H1A H 0.1515 0.5984 0.2043 0.032 Uiso 1 1 d R . . H1B H 0.1735 0.6393 0.0876 0.032 Uiso 1 1 d R . . O6 O 0.4707(2) 0.5893(5) -0.1836(6) 0.0261(15) Uani 1 1 d U . . O12 O -0.1044(3) 0.5098(5) 0.7529(7) 0.0400(19) Uani 1 1 d U . . O14 O -0.1192(3) 0.6750(5) 0.7689(7) 0.0380(17) Uani 1 1 d U . . O7 O 0.5468(2) 0.5922(4) 0.0316(6) 0.0253(15) Uani 1 1 d U . . O8 O 0.5677(3) 0.7509(4) -0.0584(6) 0.0285(15) Uani 1 1 d U . . O10 O 0.6974(3) 0.4944(4) -0.5659(5) 0.0248(16) Uani 1 1 d U . . H10A H 0.7164 0.4655 -0.6184 0.037 Uiso 1 1 calc R . . O9 O 0.6353(3) 0.6712(5) 0.1099(6) 0.0343(18) Uani 1 1 d U . . O15 O -0.2146(3) 0.7235(5) 0.8632(8) 0.059(2) Uani 1 1 d U . . S1 S 0.59428(10) 0.66575(18) -0.0059(2) 0.0242(6) Uani 1 1 d . . . S2 S -0.10793(11) 0.59129(18) 0.6662(3) 0.0288(6) Uani 1 1 d . . . Eu1 Eu 0.222031(17) 0.75456(3) 0.30961(4) 0.01227(14) Uani 1 1 d . . . O13 O -0.1502(2) 0.5972(4) 0.5551(7) 0.0350(19) Uani 1 1 d U . . 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 C30 0.050(3) 0.050(3) 0.050(3) 0.0000(10) 0.0049(10) 0.0004(10) C16 0.018(4) 0.021(4) 0.019(4) -0.002(3) 0.008(3) -0.002(3) C1 0.014(3) 0.012(3) 0.018(3) -0.001(3) 0.002(3) 0.003(3) C12 0.020(3) 0.014(3) 0.019(3) -0.005(3) 0.004(3) 0.001(3) C3 0.015(3) 0.023(3) 0.016(3) -0.003(3) 0.005(3) -0.001(3) C7 0.017(3) 0.019(3) 0.014(3) 0.002(3) 0.004(3) 0.002(3) C20 0.018(3) 0.019(3) 0.025(3) 0.001(3) 0.009(3) -0.002(3) C4 0.019(3) 0.023(3) 0.020(3) 0.001(3) 0.002(3) 0.004(3) C17 0.019(3) 0.024(4) 0.020(3) 0.001(3) 0.007(3) -0.004(3) C29 0.025(4) 0.019(4) 0.029(4) 0.002(3) 0.004(3) 0.007(3) C5 0.018(3) 0.025(3) 0.023(3) -0.002(3) 0.006(3) 0.005(3) C21 0.021(4) 0.026(4) 0.021(3) 0.001(3) 0.002(3) -0.005(3) C2 0.015(3) 0.019(3) 0.019(3) 0.004(3) 0.007(3) 0.001(3) C18 0.019(3) 0.033(4) 0.022(3) 0.001(3) 0.006(3) -0.002(3) C11 0.020(3) 0.019(3) 0.021(3) -0.001(3) 0.005(3) 0.001(3) C6 0.022(3) 0.022(3) 0.019(3) 0.001(3) 0.009(3) 0.003(3) C13 0.024(3) 0.025(4) 0.019(3) -0.002(3) 0.004(3) 0.002(3) C15 0.020(4) 0.019(4) 0.021(3) -0.003(3) 0.004(3) -0.004(3) C9 0.022(3) 0.024(3) 0.021(3) -0.005(3) 0.007(3) 0.005(3) C26 0.027(4) 0.021(4) 0.031(4) 0.002(3) 0.012(3) 0.003(3) C23 0.031(4) 0.021(4) 0.040(4) 0.004(3) 0.015(3) 0.003(3) C14 0.025(3) 0.022(4) 0.021(3) -0.003(3) 0.006(3) 0.006(3) C25 0.028(3) 0.027(3) 0.039(3) 0.008(3) 0.015(3) 0.009(3) C22 0.023(3) 0.028(4) 0.018(3) 0.004(3) 0.009(3) -0.003(3) C19 0.025(3) 0.032(4) 0.023(3) 0.002(3) 0.007(3) -0.004(3) C24 0.034(4) 0.024(4) 0.043(4) 0.011(3) 0.018(3) 0.003(3) C10 0.021(3) 0.021(4) 0.020(3) -0.002(3) 0.004(3) 0.000(3) C27 0.037(4) 0.023(4) 0.042(4) 0.010(3) 0.018(3) 0.004(3) C8 0.044(6) 0.029(6) 0.028(5) -0.008(4) 0.007(5) 0.006(5) C28 0.033(4) 0.025(4) 0.039(3) 0.006(3) 0.018(3) 0.006(3) O17 0.021(3) 0.018(3) 0.017(3) 0.007(3) 0.003(3) 0.008(3) O5 0.013(3) 0.024(3) 0.016(3) 0.002(3) 0.005(3) 0.004(3) O3 0.016(3) 0.029(4) 0.023(3) -0.009(3) 0.002(3) -0.006(3) O16 0.016(3) 0.015(3) 0.017(3) 0.001(3) 0.010(3) 0.004(3) O11 0.030(4) 0.019(4) 0.022(3) -0.005(3) 0.007(3) 0.009(3) O4 0.014(3) 0.027(4) 0.019(3) -0.005(3) 0.002(2) 0.003(3) O2 0.012(3) 0.026(3) 0.018(3) 0.004(3) 0.003(3) -0.004(3) O1 0.023(3) 0.023(4) 0.019(3) 0.001(3) 0.008(3) -0.009(3) O6 0.018(3) 0.040(4) 0.022(3) -0.008(3) 0.007(3) 0.003(3) O12 0.041(4) 0.022(4) 0.061(5) 0.016(4) 0.026(4) 0.001(3) O14 0.043(4) 0.026(4) 0.048(4) 0.008(3) 0.021(3) 0.014(3) O7 0.017(3) 0.026(4) 0.034(3) -0.001(3) 0.009(3) 0.003(3) O8 0.035(4) 0.023(4) 0.029(3) -0.005(3) 0.011(3) 0.002(3) O10 0.037(4) 0.027(4) 0.013(3) 0.005(3) 0.011(3) 0.011(3) O9 0.031(4) 0.044(4) 0.028(4) -0.017(3) 0.002(3) 0.008(4) O15 0.054(5) 0.048(5) 0.078(5) 0.010(4) 0.030(4) 0.009(4) S1 0.0201(14) 0.0282(15) 0.0247(13) -0.0058(12) 0.0035(11) 0.0000(12) S2 0.0265(15) 0.0192(14) 0.0430(16) 0.0018(12) 0.0158(13) -0.0020(12) Eu1 0.0112(2) 0.0151(3) 0.0112(2) 0.0002(2) 0.00463(16) 0.0006(2) O13 0.007(3) 0.022(4) 0.074(5) 0.020(4) -0.009(3) -0.002(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 C30 O15 1.475(13) . ? C16 O3 1.242(9) . ? C16 O2 1.251(10) . ? C16 C17 1.485(12) . ? C1 O5 1.252(8) . ? C1 O4 1.263(10) . ? C1 C2 1.497(11) . ? C12 C13 1.380(11) . ? C12 C11 1.391(10) . ? C12 C15 1.486(12) . ? C3 C2 1.381(10) . ? C3 C4 1.411(11) . ? C7 C2 1.398(11) . ? C7 C6 1.400(12) . ? C20 C21 1.354(12) . ? C20 C19 1.413(11) . ? C20 S2 1.740(9) . ? C4 C5 1.350(12) . ? C17 C18 1.385(12) . ? C17 C22 1.412(11) . ? C29 O16 1.259(11) . ? C29 O17 1.283(11) . ? C29 C26 1.464(12) . ? C29 Eu1 2.894(9) 3_576 ? C5 C6 1.393(11) . ? C5 O7 1.422(10) . ? C21 C22 1.398(12) . ? C18 C19 1.388(12) . ? C11 C10 1.375(12) . ? C6 O6 1.377(10) . ? C13 C14 1.360(12) . ? C15 O11 1.235(10) . ? C15 O10 1.313(9) . ? C9 C10 1.391(11) . ? C9 C14 1.392(11) . ? C9 S1 1.772(9) . ? C26 C27 1.373(13) . ? C26 C25 1.390(13) . ? C23 C24 1.340(13) . ? C23 C28 1.396(13) . ? C23 O14 1.406(11) . ? C25 C24 1.386(13) . ? C24 O15 1.385(12) . ? C27 C28 1.418(12) . ? C8 O6 1.432(9) . ? O17 Eu1 2.580(6) 3_576 ? O5 Eu1 2.306(5) 4_575 ? O3 Eu1 2.329(5) 4_576 ? O16 Eu1 2.470(6) 3_576 ? O11 Eu1 2.463(6) 3_665 ? O4 Eu1 2.328(6) . ? O2 Eu1 2.367(6) . ? O1 Eu1 2.456(5) . ? O12 S2 1.429(7) . ? O14 S2 1.591(7) . ? O7 S1 1.587(7) . ? O8 S1 1.428(6) . ? O9 S1 1.432(6) . ? S2 O13 1.417(6) . ? Eu1 O5 2.306(5) 4_576 ? Eu1 O3 2.329(5) 4_575 ? Eu1 O11 2.463(6) 3_665 ? Eu1 O16 2.470(6) 3_576 ? Eu1 O17 2.580(6) 3_576 ? Eu1 C29 2.894(10) 3_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C16 O2 124.4(9) . . ? O3 C16 C17 117.3(8) . . ? O2 C16 C17 118.3(8) . . ? O5 C1 O4 123.7(8) . . ? O5 C1 C2 118.7(8) . . ? O4 C1 C2 117.6(7) . . ? C13 C12 C11 120.2(8) . . ? C13 C12 C15 122.7(7) . . ? C11 C12 C15 117.2(8) . . ? C2 C3 C4 119.1(8) . . ? C2 C7 C6 118.9(8) . . ? C21 C20 C19 121.9(9) . . ? C21 C20 S2 121.8(7) . . ? C19 C20 S2 116.3(7) . . ? C5 C4 C3 118.9(8) . . ? C18 C17 C22 118.0(9) . . ? C18 C17 C16 120.4(8) . . ? C22 C17 C16 121.6(8) . . ? O16 C29 O17 120.3(8) . . ? O16 C29 C26 119.6(9) . . ? O17 C29 C26 120.0(9) . . ? O16 C29 Eu1 58.0(5) . 3_576 ? O17 C29 Eu1 63.1(5) . 3_576 ? C26 C29 Eu1 167.7(6) . 3_576 ? C4 C5 C6 123.2(9) . . ? C4 C5 O7 119.7(8) . . ? C6 C5 O7 116.6(8) . . ? C20 C21 C22 119.3(8) . . ? C3 C2 C7 121.5(8) . . ? C3 C2 C1 120.0(8) . . ? C7 C2 C1 118.5(7) . . ? C17 C18 C19 121.9(8) . . ? C10 C11 C12 119.8(8) . . ? O6 C6 C5 116.9(8) . . ? O6 C6 C7 124.8(7) . . ? C5 C6 C7 118.2(8) . . ? C14 C13 C12 120.5(8) . . ? O11 C15 O10 122.6(9) . . ? O11 C15 C12 123.6(8) . . ? O10 C15 C12 113.7(8) . . ? C10 C9 C14 120.2(8) . . ? C10 C9 S1 118.4(6) . . ? C14 C9 S1 121.2(7) . . ? C27 C26 C25 118.6(9) . . ? C27 C26 C29 120.0(9) . . ? C25 C26 C29 121.0(9) . . ? C24 C23 C28 121.4(10) . . ? C24 C23 O14 117.4(9) . . ? C28 C23 O14 120.7(9) . . ? C13 C14 C9 119.8(8) . . ? C24 C25 C26 120.0(10) . . ? C21 C22 C17 120.9(8) . . ? C18 C19 C20 118.1(9) . . ? C23 C24 O15 115.6(9) . . ? C23 C24 C25 121.2(10) . . ? O15 C24 C25 122.8(10) . . ? C11 C10 C9 119.5(8) . . ? C26 C27 C28 121.7(10) . . ? C23 C28 C27 117.0(10) . . ? C29 O17 Eu1 90.6(5) . 3_576 ? C1 O5 Eu1 160.3(6) . 4_575 ? C16 O3 Eu1 158.9(6) . 4_576 ? C29 O16 Eu1 96.4(6) . 3_576 ? C15 O11 Eu1 157.7(6) . 3_665 ? C1 O4 Eu1 133.0(5) . . ? C16 O2 Eu1 129.6(5) . . ? C6 O6 C8 117.6(7) . . ? C23 O14 S2 122.4(6) . . ? C5 O7 S1 117.6(6) . . ? C24 O15 C30 116.7(8) . . ? O8 S1 O9 119.2(4) . . ? O8 S1 O7 109.8(4) . . ? O9 S1 O7 106.5(4) . . ? O8 S1 C9 110.2(4) . . ? O9 S1 C9 109.0(4) . . ? O7 S1 C9 100.4(4) . . ? O13 S2 O12 120.8(4) . . ? O13 S2 O14 107.9(4) . . ? O12 S2 O14 102.5(4) . . ? O13 S2 C20 112.0(4) . . ? O12 S2 C20 107.9(4) . . ? O14 S2 C20 104.1(4) . . ? O5 Eu1 O4 82.02(19) 4_576 . ? O5 Eu1 O3 142.8(2) 4_576 4_575 ? O4 Eu1 O3 97.2(2) . 4_575 ? O5 Eu1 O2 105.23(19) 4_576 . ? O4 Eu1 O2 154.9(2) . . ? O3 Eu1 O2 91.13(19) 4_575 . ? O5 Eu1 O1 145.43(19) 4_576 . ? O4 Eu1 O1 88.70(19) . . ? O3 Eu1 O1 71.3(2) 4_575 . ? O2 Eu1 O1 71.6(2) . . ? O5 Eu1 O11 74.11(19) 4_576 3_665 ? O4 Eu1 O11 79.4(2) . 3_665 ? O3 Eu1 O11 142.6(2) 4_575 3_665 ? O2 Eu1 O11 79.6(2) . 3_665 ? O1 Eu1 O11 71.47(18) . 3_665 ? O5 Eu1 O16 75.20(18) 4_576 3_576 ? O4 Eu1 O16 129.6(2) . 3_576 ? O3 Eu1 O16 77.11(19) 4_575 3_576 ? O2 Eu1 O16 75.35(19) . 3_576 ? O1 Eu1 O16 133.07(18) . 3_576 ? O11 Eu1 O16 133.15(18) 3_665 3_576 ? O5 Eu1 O17 73.82(18) 4_576 3_576 ? O4 Eu1 O17 79.1(2) . 3_576 ? O3 Eu1 O17 69.59(19) 4_575 3_576 ? O2 Eu1 O17 126.0(2) . 3_576 ? O1 Eu1 O17 136.89(18) . 3_576 ? O11 Eu1 O17 143.36(18) 3_665 3_576 ? O16 Eu1 O17 51.70(19) 3_576 3_576 ? O5 Eu1 C29 75.2(2) 4_576 3_576 ? O4 Eu1 C29 105.2(3) . 3_576 ? O3 Eu1 C29 69.1(2) 4_575 3_576 ? O2 Eu1 C29 99.9(3) . 3_576 ? O1 Eu1 C29 139.2(2) . 3_576 ? O11 Eu1 C29 148.0(2) 3_665 3_576 ? O16 Eu1 C29 25.6(2) 3_576 3_576 ? O17 Eu1 C29 26.3(2) 3_576 3_576 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.147 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.175 _database_code_depnum_ccdc_archive 'CCDC 956811' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Gd O17 S2' _chemical_formula_weight 876.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.4006(7) _cell_length_b 14.1988(5) _cell_length_c 9.9356(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.468(3) _cell_angle_gamma 90.00 _cell_volume 3291.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 5385 _cell_measurement_theta_min 2.5021 _cell_measurement_theta_max 29.1376 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5554 _exptl_absorpt_correction_T_max 0.8084 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13237 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5785 _reflns_number_gt 4520 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _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. SIMU 0.01 0.02 3.8 C19 C23 C24 C7 C25 C1 C13 C20 C17 C26 C9 C8 C16 C4 C6 C18 = C3 C28 C14 C22 C10 C27 C5 C21 C30 C2 C11 C29 C12 C15 SIMU 0.01 0.02 3.8 O10 O5 O14 O12 O1 O2 O11 O3 O16 O15 O4 O17 O6 O13 O9 O7 O8 ; _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^)+(0.0315P)^2^+13.2044P] 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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5785 _refine_ls_number_parameters 455 _refine_ls_number_restraints 624 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.040 _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 C19 C 0.1161(3) 0.1721(5) 0.3544(8) 0.0526(15) Uani 1 1 d U . . H19 H 0.0817 0.1900 0.3877 0.063 Uiso 1 1 calc R . . C23 C 0.2637(4) 0.2406(6) 0.0656(11) 0.078(3) Uani 1 1 d U . . H23A H 0.2728 0.2895 0.0042 0.117 Uiso 1 1 calc R . . H23B H 0.2503 0.1860 0.0154 0.117 Uiso 1 1 calc R . . H23C H 0.2973 0.2246 0.1226 0.117 Uiso 1 1 calc R . . C24 C 0.0411(3) 0.3814(5) 0.3803(7) 0.0359(13) Uani 1 1 d U . . C7 C 0.4179(3) -0.1831(5) 0.6807(7) 0.0368(13) Uani 1 1 d U . . H7 H 0.4069 -0.2015 0.7647 0.044 Uiso 1 1 calc R . . C25 C 0.0299(3) 0.3698(5) 0.5124(7) 0.0397(14) Uani 1 1 d U . . H25 H 0.0592 0.3752 0.5807 0.048 Uiso 1 1 calc R . . C1 C 0.3169(2) -0.2095(4) 0.5881(6) 0.0281(12) Uani 1 1 d U . . C13 C 0.6990(3) 0.0006(5) 0.2999(7) 0.0393(14) Uani 1 1 d U . . H13 H 0.7311 0.0375 0.3233 0.047 Uiso 1 1 calc R . . C20 C 0.1456(3) 0.2339(5) 0.2803(8) 0.0475(15) Uani 1 1 d U . . C17 C 0.1883(3) 0.0543(5) 0.3251(7) 0.0389(14) Uani 1 1 d U . . C26 C -0.0255(3) 0.3500(5) 0.5435(7) 0.0382(13) Uani 1 1 d U . . H26 H -0.0332 0.3411 0.6330 0.046 Uiso 1 1 calc R . . C9 C 0.6251(3) -0.1005(5) 0.3633(7) 0.0441(14) Uani 1 1 d U . . C8 C 0.4276(4) -0.0622(7) 0.2070(8) 0.072(2) Uani 1 1 d U . . H8A H 0.4469 -0.0412 0.1307 0.108 Uiso 1 1 calc R . . H8B H 0.4051 -0.0116 0.2389 0.108 Uiso 1 1 calc R . . H8C H 0.4031 -0.1143 0.1808 0.108 Uiso 1 1 calc R . . C16 C 0.2062(3) -0.0453(5) 0.3318(7) 0.0355(13) Uani 1 1 d U . . C4 C 0.4489(3) -0.1235(5) 0.4303(7) 0.0392(13) Uani 1 1 d U . . C6 C 0.4750(3) -0.1578(5) 0.6672(7) 0.0421(14) Uani 1 1 d U . . H6 H 0.5026 -0.1605 0.7397 0.051 Uiso 1 1 calc R . . C18 C 0.1381(3) 0.0821(5) 0.3797(8) 0.0509(15) Uani 1 1 d U . . H18 H 0.1191 0.0406 0.4332 0.061 Uiso 1 1 calc R . . C3 C 0.3926(3) -0.1499(5) 0.4453(7) 0.0361(13) Uani 1 1 d U . . H3 H 0.3651 -0.1467 0.3727 0.043 Uiso 1 1 calc R . . C28 C -0.0577(3) 0.3586(5) 0.3099(7) 0.0434(14) Uani 1 1 d U . . H28 H -0.0873 0.3559 0.2419 0.052 Uiso 1 1 calc R . . C14 C 0.6707(3) -0.0437(5) 0.3995(7) 0.0439(14) Uani 1 1 d U . . H14 H 0.6826 -0.0347 0.4901 0.053 Uiso 1 1 calc R . . C22 C 0.2169(3) 0.1190(5) 0.2526(7) 0.0431(14) Uani 1 1 d U . . H22 H 0.2511 0.1013 0.2178 0.052 Uiso 1 1 calc R . . C10 C 0.6051(3) -0.1129(5) 0.2297(7) 0.0481(15) Uani 1 1 d U . . H10 H 0.5735 -0.1510 0.2067 0.058 Uiso 1 1 calc R . . C27 C -0.0691(2) 0.3433(4) 0.4435(6) 0.0319(13) Uani 1 1 d U . . C5 C 0.4883(3) -0.1284(5) 0.5403(7) 0.0399(14) Uani 1 1 d U . . C21 C 0.1969(3) 0.2089(5) 0.2297(8) 0.0484(15) Uani 1 1 d U . . C30 C -0.1293(2) 0.3173(4) 0.4750(6) 0.0298(12) Uani 1 1 d U . . C2 C 0.3780(2) -0.1813(5) 0.5719(6) 0.0304(12) Uani 1 1 d U . . C11 C 0.6333(3) -0.0673(5) 0.1308(7) 0.0450(15) Uani 1 1 d U . . H11 H 0.6208 -0.0752 0.0403 0.054 Uiso 1 1 calc R . . C29 C -0.0024(3) 0.3777(5) 0.2783(7) 0.0464(15) Uani 1 1 d U . . H29 H 0.0054 0.3880 0.1891 0.056 Uiso 1 1 calc R . . C12 C 0.6798(3) -0.0099(5) 0.1662(7) 0.0366(13) Uani 1 1 d U . . C15 C 0.7114(3) 0.0409(5) 0.0633(6) 0.0356(13) Uani 1 1 d U . . O10 O 0.6994(2) 0.0100(3) -0.0603(5) 0.0468(13) Uani 1 1 d U . . H10A H 0.7199 0.0368 -0.1116 0.070 Uiso 1 1 calc R . . O5 O 0.30467(17) -0.2350(3) 0.7034(4) 0.0366(11) Uani 1 1 d U . . O14 O 0.1083(2) 0.4841(3) 0.2505(6) 0.0669(17) Uani 1 1 d U . . O12 O 0.2195(3) 0.2730(4) 0.1475(7) 0.0815(19) Uani 1 1 d U . . O1 O 0.18104(19) -0.3772(3) 0.1707(4) 0.0437(12) Uani 1 1 d . . . H1A H 0.1503 -0.4001 0.2038 0.066 Uiso 1 1 d R . . H1B H 0.1716 -0.3584 0.0881 0.066 Uiso 1 1 d R . . O2 O 0.17810(17) -0.1036(3) 0.3985(4) 0.0325(10) Uani 1 1 d U . . O11 O 0.7445(2) 0.1047(3) 0.0896(5) 0.0425(12) Uani 1 1 d U . . O3 O 0.24750(18) -0.0737(3) 0.2677(4) 0.0344(10) Uani 1 1 d U . . O16 O -0.16691(17) 0.3140(3) 0.3789(4) 0.0391(11) Uani 1 1 d U . . O15 O 0.1511(2) 0.3983(4) 0.4480(6) 0.0674(17) Uani 1 1 d U . . O4 O 0.28176(17) -0.2051(3) 0.4880(4) 0.0364(10) Uani 1 1 d U . . O17 O -0.13781(16) 0.2997(3) 0.5944(4) 0.0340(10) Uani 1 1 d U . . O6 O 0.4689(2) -0.0911(4) 0.3118(5) 0.0600(14) Uani 1 1 d U . . O13 O 0.1216(2) 0.3218(4) 0.2353(6) 0.0594(14) Uani 1 1 d U . . O9 O 0.6321(2) -0.1688(5) 0.6075(6) 0.0718(17) Uani 1 1 d U . . O7 O 0.54470(19) -0.0931(4) 0.5242(5) 0.0550(13) Uani 1 1 d U . . O8 O 0.5680(2) -0.2486(3) 0.4379(6) 0.0567(14) Uani 1 1 d U . . S2 S 0.11054(7) 0.40375(12) 0.3352(2) 0.0438(5) Uani 1 1 d . . . S1 S 0.59252(8) -0.16503(14) 0.4915(2) 0.0471(5) Uani 1 1 d . . . Gd1 Gd 0.220160(11) -0.245825(19) 0.30741(3) 0.02134(11) 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 C19 0.051(3) 0.044(3) 0.066(3) 0.006(3) 0.028(3) 0.011(3) C23 0.065(5) 0.072(6) 0.101(7) 0.019(5) 0.038(5) 0.000(4) C24 0.029(3) 0.040(3) 0.040(3) 0.001(3) 0.013(2) 0.000(2) C7 0.028(3) 0.052(3) 0.031(3) 0.004(3) 0.008(2) -0.007(3) C25 0.028(3) 0.055(3) 0.037(3) 0.002(3) 0.002(2) -0.004(3) C1 0.024(3) 0.037(3) 0.025(3) -0.004(2) 0.008(2) 0.000(2) C13 0.041(3) 0.041(3) 0.037(3) -0.005(3) 0.012(3) -0.014(3) C20 0.045(3) 0.036(3) 0.064(3) 0.005(3) 0.021(3) 0.007(3) C17 0.039(3) 0.031(3) 0.049(3) 0.001(3) 0.016(3) 0.004(2) C26 0.031(3) 0.052(3) 0.032(3) 0.004(3) 0.008(2) -0.003(3) C9 0.042(3) 0.054(3) 0.039(3) 0.001(3) 0.013(3) -0.011(3) C8 0.076(5) 0.086(6) 0.053(5) 0.018(5) 0.007(4) -0.015(5) C16 0.038(3) 0.030(3) 0.040(3) 0.002(3) 0.013(3) 0.005(3) C4 0.033(3) 0.053(3) 0.034(3) -0.001(3) 0.015(2) -0.008(3) C6 0.030(3) 0.057(3) 0.039(3) 0.002(3) 0.002(2) -0.007(3) C18 0.055(3) 0.038(3) 0.063(3) 0.013(3) 0.028(3) 0.007(3) C3 0.031(3) 0.048(3) 0.031(3) -0.003(3) 0.009(2) -0.006(2) C28 0.032(3) 0.065(3) 0.034(3) 0.006(3) 0.005(2) -0.011(3) C14 0.044(3) 0.051(3) 0.038(3) -0.002(3) 0.011(3) -0.014(3) C22 0.040(3) 0.034(3) 0.058(3) 0.008(3) 0.022(3) 0.005(3) C10 0.047(3) 0.053(3) 0.046(3) 0.000(3) 0.011(3) -0.019(3) C27 0.026(3) 0.038(3) 0.032(3) 0.000(2) 0.009(2) -0.008(2) C5 0.025(3) 0.055(3) 0.041(3) -0.003(3) 0.011(2) -0.012(3) C21 0.045(3) 0.036(3) 0.067(3) 0.008(3) 0.024(3) 0.003(3) C30 0.026(3) 0.035(3) 0.029(3) 0.001(2) 0.007(2) -0.002(2) C2 0.026(3) 0.041(3) 0.026(3) 0.000(2) 0.007(2) -0.005(2) C11 0.048(3) 0.053(3) 0.036(3) -0.002(3) 0.010(3) -0.019(3) C29 0.035(3) 0.067(3) 0.039(3) 0.009(3) 0.013(3) -0.009(3) C12 0.040(3) 0.039(3) 0.034(3) -0.003(3) 0.016(2) -0.007(2) C15 0.040(3) 0.037(3) 0.032(3) -0.002(3) 0.017(3) -0.008(3) O10 0.060(3) 0.050(3) 0.032(3) -0.003(2) 0.019(2) -0.021(2) O5 0.021(2) 0.061(3) 0.029(2) 0.006(2) 0.0105(18) -0.005(2) O14 0.054(3) 0.038(3) 0.114(5) 0.022(3) 0.041(3) 0.000(2) O12 0.079(4) 0.052(3) 0.120(5) 0.022(4) 0.048(4) 0.004(3) O1 0.055(3) 0.049(3) 0.029(3) -0.006(2) 0.015(2) -0.019(2) O2 0.037(2) 0.031(2) 0.031(2) 0.0037(19) 0.0156(19) 0.0010(19) O11 0.056(3) 0.035(3) 0.039(3) -0.005(2) 0.020(2) -0.021(2) O3 0.039(2) 0.030(2) 0.036(2) 0.0032(19) 0.015(2) 0.0034(19) O16 0.027(2) 0.054(3) 0.037(3) -0.007(2) 0.008(2) -0.011(2) O15 0.027(3) 0.068(4) 0.106(5) 0.008(3) -0.001(3) -0.007(3) O4 0.028(2) 0.050(3) 0.032(2) 0.002(2) 0.0071(19) -0.0058(19) O17 0.026(2) 0.045(3) 0.032(2) 0.007(2) 0.0140(18) -0.005(2) O6 0.046(3) 0.087(4) 0.049(3) 0.016(3) 0.020(2) -0.013(3) O13 0.062(3) 0.044(3) 0.077(4) 0.011(3) 0.032(3) 0.015(3) O9 0.056(3) 0.103(5) 0.055(3) 0.032(3) -0.005(3) -0.011(3) O7 0.037(3) 0.065(3) 0.065(3) -0.010(3) 0.017(2) -0.017(2) O8 0.060(3) 0.045(3) 0.069(4) 0.011(3) 0.026(3) -0.005(2) S2 0.0320(9) 0.0323(9) 0.0696(13) 0.0048(9) 0.0196(9) -0.0020(7) S1 0.0385(10) 0.0510(12) 0.0527(12) 0.0144(10) 0.0091(9) -0.0019(9) Gd1 0.01904(16) 0.02668(18) 0.01930(16) 0.00037(13) 0.00793(11) 0.00109(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 C19 C20 1.365(9) . ? C19 C18 1.393(10) . ? C23 O12 1.440(10) . ? C24 C25 1.368(9) . ? C24 C29 1.381(9) . ? C24 S2 1.748(6) . ? C7 C2 1.372(8) . ? C7 C6 1.400(8) . ? C25 C26 1.384(8) . ? C1 O4 1.241(7) . ? C1 O5 1.256(7) . ? C1 C2 1.507(8) . ? C13 C12 1.377(9) . ? C13 C14 1.384(9) . ? C20 C21 1.383(9) . ? C20 O13 1.427(8) . ? C17 C22 1.374(9) . ? C17 C18 1.390(9) . ? C17 C16 1.475(9) . ? C26 C27 1.371(9) . ? C9 C14 1.364(9) . ? C9 C10 1.384(10) . ? C9 S1 1.787(7) . ? C8 O6 1.424(9) . ? C16 O3 1.265(7) . ? C16 O2 1.274(7) . ? C16 Gd1 2.878(6) . ? C4 C5 1.376(9) . ? C4 O6 1.378(7) . ? C4 C3 1.389(8) . ? C6 C5 1.385(9) . ? C3 C2 1.402(8) . ? C28 C29 1.382(9) . ? C28 C27 1.391(8) . ? C22 C21 1.374(9) . ? C10 C11 1.386(9) . ? C27 C30 1.514(8) . ? C5 O7 1.433(7) . ? C21 O12 1.357(9) . ? C30 O17 1.244(7) . ? C30 O16 1.247(7) . ? C11 C12 1.385(9) . ? C12 C15 1.492(8) . ? C15 O11 1.207(7) . ? C15 O10 1.314(7) . ? O5 Gd1 2.317(4) 4_556 ? O14 S2 1.417(5) . ? O1 Gd1 2.443(4) . ? O2 Gd1 2.450(4) . ? O11 Gd1 2.471(4) 2_655 ? O3 Gd1 2.564(4) . ? O16 Gd1 2.312(4) 2 ? O15 S2 1.412(6) . ? O4 Gd1 2.287(4) . ? O17 Gd1 2.354(4) 3_556 ? O13 S2 1.564(5) . ? O9 S1 1.421(6) . ? O7 S1 1.568(5) . ? O8 S1 1.405(5) . ? Gd1 O16 2.312(4) 2_545 ? Gd1 O5 2.317(4) 4 ? Gd1 O17 2.354(4) 3_556 ? Gd1 O11 2.471(4) 2_645 ? 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 C20 C19 C18 119.5(6) . . ? C25 C24 C29 121.0(6) . . ? C25 C24 S2 121.3(5) . . ? C29 C24 S2 117.7(5) . . ? C2 C7 C6 121.0(6) . . ? C24 C25 C26 119.4(6) . . ? O4 C1 O5 124.2(5) . . ? O4 C1 C2 118.4(5) . . ? O5 C1 C2 117.4(5) . . ? C12 C13 C14 120.2(6) . . ? C19 C20 C21 121.4(7) . . ? C19 C20 O13 121.9(6) . . ? C21 C20 O13 116.2(6) . . ? C22 C17 C18 118.5(6) . . ? C22 C17 C16 121.1(6) . . ? C18 C17 C16 120.0(6) . . ? C27 C26 C25 120.6(6) . . ? C14 C9 C10 121.8(6) . . ? C14 C9 S1 118.9(6) . . ? C10 C9 S1 119.2(5) . . ? O3 C16 O2 120.0(6) . . ? O3 C16 C17 120.6(6) . . ? O2 C16 C17 119.4(5) . . ? O3 C16 Gd1 63.0(3) . . ? O2 C16 Gd1 57.9(3) . . ? C17 C16 Gd1 168.1(5) . . ? C5 C4 O6 116.4(6) . . ? C5 C4 C3 118.9(6) . . ? O6 C4 C3 124.7(6) . . ? C5 C6 C7 116.6(6) . . ? C17 C18 C19 120.1(7) . . ? C4 C3 C2 118.7(6) . . ? C29 C28 C27 120.0(6) . . ? C9 C14 C13 119.2(7) . . ? C21 C22 C17 122.3(6) . . ? C9 C10 C11 118.5(6) . . ? C26 C27 C28 119.6(6) . . ? C26 C27 C30 121.3(6) . . ? C28 C27 C30 119.1(6) . . ? C4 C5 C6 123.7(6) . . ? C4 C5 O7 117.3(6) . . ? C6 C5 O7 118.7(6) . . ? O12 C21 C22 125.3(6) . . ? O12 C21 C20 116.0(6) . . ? C22 C21 C20 118.2(6) . . ? O17 C30 O16 124.6(5) . . ? O17 C30 C27 117.8(6) . . ? O16 C30 C27 117.6(5) . . ? C7 C2 C3 121.0(5) . . ? C7 C2 C1 120.3(5) . . ? C3 C2 C1 118.7(6) . . ? C12 C11 C10 120.2(7) . . ? C24 C29 C28 119.3(6) . . ? C13 C12 C11 120.0(6) . . ? C13 C12 C15 117.9(6) . . ? C11 C12 C15 122.2(6) . . ? O11 C15 O10 122.7(6) . . ? O11 C15 C12 123.9(6) . . ? O10 C15 C12 113.4(6) . . ? C1 O5 Gd1 134.7(4) . 4_556 ? C21 O12 C23 117.2(6) . . ? C16 O2 Gd1 96.0(3) . . ? C15 O11 Gd1 157.4(4) . 2_655 ? C16 O3 Gd1 91.0(4) . . ? C30 O16 Gd1 158.5(4) . 2 ? C1 O4 Gd1 162.5(5) . . ? C30 O17 Gd1 131.1(4) . 3_556 ? C4 O6 C8 117.7(6) . . ? C20 O13 S2 122.2(5) . . ? C5 O7 S1 118.3(4) . . ? O15 S2 O14 120.5(4) . . ? O15 S2 O13 109.2(3) . . ? O14 S2 O13 102.9(3) . . ? O15 S2 C24 111.5(3) . . ? O14 S2 C24 107.8(3) . . ? O13 S2 C24 103.4(3) . . ? O8 S1 O9 119.8(4) . . ? O8 S1 O7 110.6(3) . . ? O9 S1 O7 106.7(4) . . ? O8 S1 C9 110.3(3) . . ? O9 S1 C9 108.1(3) . . ? O7 S1 C9 99.5(3) . . ? O4 Gd1 O16 143.43(17) . 2_545 ? O4 Gd1 O5 82.62(15) . 4 ? O16 Gd1 O5 96.41(14) 2_545 4 ? O4 Gd1 O17 104.09(14) . 3_556 ? O16 Gd1 O17 92.50(14) 2_545 3_556 ? O5 Gd1 O17 154.31(16) 4 3_556 ? O4 Gd1 O1 144.62(17) . . ? O16 Gd1 O1 71.34(16) 2_545 . ? O5 Gd1 O1 87.62(15) 4 . ? O17 Gd1 O1 72.48(15) 3_556 . ? O4 Gd1 O2 75.45(15) . . ? O16 Gd1 O2 77.64(15) 2_545 . ? O5 Gd1 O2 129.98(15) 4 . ? O17 Gd1 O2 75.48(14) 3_556 . ? O1 Gd1 O2 133.68(15) . . ? O4 Gd1 O11 73.84(16) . 2_645 ? O16 Gd1 O11 142.18(17) 2_545 2_645 ? O5 Gd1 O11 79.28(15) 4 2_645 ? O17 Gd1 O11 78.93(15) 3_556 2_645 ? O1 Gd1 O11 70.95(17) . 2_645 ? O2 Gd1 O11 133.32(14) . 2_645 ? O4 Gd1 O3 74.35(15) . . ? O16 Gd1 O3 69.62(15) 2_545 . ? O5 Gd1 O3 79.12(14) 4 . ? O17 Gd1 O3 126.54(14) 3_556 . ? O1 Gd1 O3 136.81(15) . . ? O2 Gd1 O3 51.96(12) . . ? O11 Gd1 O3 143.39(15) 2_645 . ? O4 Gd1 C16 75.69(18) . . ? O16 Gd1 C16 69.26(18) 2_545 . ? O5 Gd1 C16 105.08(17) 4 . ? O17 Gd1 C16 100.62(16) 3_556 . ? O1 Gd1 C16 139.62(18) . . ? O2 Gd1 C16 26.12(14) . . ? O11 Gd1 C16 148.37(18) 2_645 . ? O3 Gd1 C16 26.07(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.229 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.119 _database_code_depnum_ccdc_archive 'CCDC 956812' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 O17 S2 Tb' _chemical_formula_weight 878.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.3952(15) _cell_length_b 14.0348(11) _cell_length_c 9.8470(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.930(6) _cell_angle_gamma 90.00 _cell_volume 3221.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 3627 _cell_measurement_theta_min 2.5282 _cell_measurement_theta_max 29.1277 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5959 _exptl_absorpt_correction_T_max 0.7777 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12160 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5681 _reflns_number_gt 4318 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _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. SIMU 0.01 0.01 3.8 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C14 C16 C17 C18 = C19 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32 ISOR 0.005 0.001 O6 ; _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^)+(0.0367P)^2^+18.7921P] 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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5681 _refine_ls_number_parameters 458 _refine_ls_number_restraints 540 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.002 _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 0.2067(3) 0.4560(5) 0.3336(7) 0.0210(14) Uani 1 1 d U . . C2 C 0.1882(3) 0.5571(5) 0.3264(7) 0.0254(14) Uani 1 1 d U . . C3 C 0.2168(3) 0.6203(6) 0.2500(8) 0.0310(15) Uani 1 1 d U . . H3 H 0.252(3) 0.614(6) 0.228(7) 0.037 Uiso 1 1 d . . . C4 C 0.1953(3) 0.7120(6) 0.2254(9) 0.0340(15) Uani 1 1 d U . . C5 C 0.1447(3) 0.7372(6) 0.2780(8) 0.0316(15) Uani 1 1 d U . . C6 C 0.1155(3) 0.6746(6) 0.3558(8) 0.0345(15) Uani 1 1 d U . . H6 H 0.0812 0.6925 0.3897 0.041 Uiso 1 1 calc R . . C7 C 0.1386(3) 0.5838(6) 0.3826(8) 0.0330(15) Uani 1 1 d U . . H7 H 0.1206 0.5416 0.4381 0.040 Uiso 1 1 calc R . . C8 C 0.2621(4) 0.7417(7) 0.0603(10) 0.048(2) Uani 1 1 d U . . H8A H 0.2696 0.7878 -0.0079 0.071 Uiso 1 1 calc R . . H8B H 0.2506 0.6826 0.0171 0.071 Uiso 1 1 calc R . . H8C H 0.2962 0.7319 0.1202 0.071 Uiso 1 1 calc R . . C9 C 0.0390(3) 0.8837(5) 0.3809(7) 0.0218(13) Uani 1 1 d U . . C10 C 0.0285(3) 0.8710(5) 0.5135(7) 0.0218(13) Uani 1 1 d U . . H10 H 0.0583 0.8756 0.5822 0.026 Uiso 1 1 calc R . . C11 C -0.0267(3) 0.8513(5) 0.5454(7) 0.0211(13) Uani 1 1 d U . . H11 H -0.0343 0.8433 0.6359 0.025 Uiso 1 1 calc R . . C12 C -0.0712(3) 0.8435(5) 0.4412(7) 0.0173(13) Uani 1 1 d U . . C14 C -0.0590(3) 0.8593(6) 0.3080(7) 0.0250(14) Uani 1 1 d U . . H14 H -0.0886 0.8565 0.2388 0.030 Uiso 1 1 calc R . . C16 C -0.0043(3) 0.8789(6) 0.2755(7) 0.0238(14) Uani 1 1 d U . . H16 H 0.0035 0.8887 0.1855 0.029 Uiso 1 1 calc R . . C17 C -0.1307(3) 0.8174(5) 0.4735(7) 0.0174(13) Uani 1 1 d U . . C18 C 0.3186(3) 0.2919(5) 0.5948(6) 0.0136(13) Uani 1 1 d U . . C19 C 0.3795(3) 0.3203(5) 0.5780(6) 0.0155(12) Uani 1 1 d U . . C20 C 0.4199(3) 0.3177(5) 0.6884(7) 0.0188(13) Uani 1 1 d U . . H20 H 0.4093 0.2985 0.7732 0.023 Uiso 1 1 calc R . . C21 C 0.4766(3) 0.3437(5) 0.6734(7) 0.0201(13) Uani 1 1 d U . . H21 H 0.5043 0.3414 0.7469 0.024 Uiso 1 1 calc R . . C22 C 0.4902(3) 0.3727(5) 0.5471(7) 0.0229(13) Uani 1 1 d U . . C23 C 0.4504(3) 0.3772(5) 0.4349(6) 0.0194(13) Uani 1 1 d U . . C24 C 0.3941(3) 0.3517(5) 0.4494(7) 0.0185(13) Uani 1 1 d U . . H24 H 0.3665 0.3550 0.3758 0.022 Uiso 1 1 calc R . . C25 C 0.4290(3) 0.4378(6) 0.2099(7) 0.0283(16) Uani 1 1 d U . . H25A H 0.4481 0.4607 0.1338 0.043 Uiso 1 1 calc R . . H25B H 0.4058 0.4878 0.2428 0.043 Uiso 1 1 calc R . . H25C H 0.4051 0.3846 0.1818 0.043 Uiso 1 1 calc R . . C26 C 0.6250(3) 0.3974(5) 0.3644(7) 0.0221(14) Uani 1 1 d U . . C27 C 0.6718(3) 0.4543(5) 0.4001(7) 0.0216(14) Uani 1 1 d U . . H27 H 0.6851 0.4621 0.4912 0.026 Uiso 1 1 calc R . . C28 C 0.6988(3) 0.5003(5) 0.2980(7) 0.0202(13) Uani 1 1 d U . . H28 H 0.7308 0.5383 0.3205 0.024 Uiso 1 1 calc R . . C29 C 0.6780(3) 0.4895(5) 0.1627(7) 0.0183(13) Uani 1 1 d U . . C30 C 0.6312(3) 0.4304(5) 0.1281(7) 0.0209(13) Uani 1 1 d U . . H30 H 0.6184 0.4213 0.0370 0.025 Uiso 1 1 calc R . . C31 C 0.6041(3) 0.3858(5) 0.2282(7) 0.0239(14) Uani 1 1 d U . . H31 H 0.5719 0.3481 0.2058 0.029 Uiso 1 1 calc R . . C32 C 0.7092(3) 0.5402(5) 0.0572(7) 0.0165(13) Uani 1 1 d U . . O1 O 0.18344(19) 0.1230(3) 0.1740(4) 0.0196(11) Uani 1 1 d . . . H1A H 0.1548 0.0968 0.2110 0.029 Uiso 1 1 d R . . H1B H 0.1712 0.1429 0.0931 0.029 Uiso 1 1 d R . . O2 O 0.17886(18) 0.3971(3) 0.4003(4) 0.0161(10) Uani 1 1 d . . . O3 O 0.24874(19) 0.4277(3) 0.2712(4) 0.0186(11) Uani 1 1 d . . . O4 O 0.2168(3) 0.7758(5) 0.1376(7) 0.060(2) Uani 1 1 d . . . O5 O 0.1202(2) 0.8252(4) 0.2329(5) 0.0356(14) Uani 1 1 d . . . O6 O 0.1497(2) 0.9032(4) 0.4486(5) 0.0374(14) Uani 1 1 d U . . O7 O 0.1052(2) 0.9903(4) 0.2479(6) 0.0409(15) Uani 1 1 d . . . O8 O -0.16857(19) 0.8145(4) 0.3755(5) 0.0223(11) Uani 1 1 d . . . O9 O -0.13920(19) 0.7994(4) 0.5943(4) 0.0196(11) Uani 1 1 d . . . O10 O 0.28253(18) 0.2972(3) 0.4929(4) 0.0162(10) Uani 1 1 d . . . O11 O 0.30643(19) 0.2644(3) 0.7097(4) 0.0188(11) Uani 1 1 d . . . O12 O 0.4706(2) 0.4087(4) 0.3160(5) 0.0300(13) Uani 1 1 d . . . O14 O 0.54648(19) 0.4069(4) 0.5321(5) 0.0271(12) Uani 1 1 d . . . O15 O 0.5674(2) 0.2492(4) 0.4412(5) 0.0271(12) Uani 1 1 d . . . O16 O 0.6347(2) 0.3290(4) 0.6107(5) 0.0333(14) Uani 1 1 d . . . O17 O 0.6970(2) 0.5074(4) -0.0664(5) 0.0235(12) Uani 1 1 d . . . H17 H 0.7188 0.5312 -0.1178 0.035 Uiso 1 1 calc R . . O18 O 0.74273(19) 0.6051(3) 0.0833(4) 0.0194(11) Uani 1 1 d . . . S1 S 0.10844(8) 0.90829(14) 0.3348(2) 0.0275(5) Uani 1 1 d . . . S2 S 0.59377(8) 0.33354(14) 0.49467(19) 0.0246(4) Uani 1 1 d . . . Tb1 Tb 0.221825(12) 0.25448(2) 0.31095(3) 0.01107(11) 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 0.022(3) 0.018(3) 0.024(3) 0.007(3) 0.008(3) 0.004(3) C2 0.029(3) 0.019(3) 0.031(3) 0.005(3) 0.015(3) 0.006(3) C3 0.028(3) 0.024(3) 0.043(3) 0.009(3) 0.018(3) 0.007(3) C4 0.032(3) 0.026(3) 0.046(3) 0.010(3) 0.020(3) 0.005(3) C5 0.034(3) 0.023(3) 0.040(3) 0.009(3) 0.015(3) 0.005(3) C6 0.032(3) 0.029(3) 0.045(3) 0.010(3) 0.019(3) 0.008(3) C7 0.036(3) 0.025(3) 0.042(3) 0.014(3) 0.021(3) 0.005(3) C8 0.041(4) 0.043(4) 0.061(4) 0.013(4) 0.017(4) 0.005(4) C9 0.019(3) 0.021(3) 0.027(3) 0.004(3) 0.010(2) -0.002(2) C10 0.016(3) 0.027(3) 0.022(3) 0.002(3) 0.003(2) -0.002(3) C11 0.020(3) 0.024(3) 0.019(3) 0.003(3) 0.007(2) -0.002(3) C12 0.017(3) 0.018(3) 0.018(3) 0.000(3) 0.006(2) -0.002(2) C14 0.021(3) 0.033(3) 0.021(3) 0.003(3) 0.002(2) -0.008(3) C16 0.019(3) 0.032(3) 0.020(3) 0.005(3) 0.005(2) -0.006(3) C17 0.017(3) 0.018(3) 0.019(3) -0.003(3) 0.008(2) -0.003(3) C18 0.012(3) 0.013(3) 0.016(3) -0.003(2) 0.001(2) -0.001(2) C19 0.014(3) 0.018(3) 0.016(3) 0.000(2) 0.007(2) -0.002(2) C20 0.016(3) 0.025(3) 0.017(3) 0.002(3) 0.005(2) -0.004(3) C21 0.015(3) 0.026(3) 0.018(3) 0.001(3) 0.000(2) -0.005(3) C22 0.018(3) 0.028(3) 0.023(3) -0.002(3) 0.005(2) -0.005(3) C23 0.018(3) 0.026(3) 0.016(3) 0.000(3) 0.007(2) -0.006(2) C24 0.017(3) 0.024(3) 0.015(3) -0.002(2) 0.005(2) -0.004(2) C25 0.029(3) 0.033(4) 0.023(3) 0.010(3) 0.006(3) -0.006(3) C26 0.021(3) 0.025(3) 0.021(3) 0.004(3) 0.005(2) -0.003(3) C27 0.020(3) 0.026(3) 0.019(3) 0.003(3) 0.004(2) -0.003(3) C28 0.019(3) 0.022(3) 0.020(3) -0.001(3) 0.006(2) -0.003(3) C29 0.019(3) 0.020(3) 0.017(3) 0.002(3) 0.008(2) 0.001(2) C30 0.019(3) 0.027(3) 0.017(3) 0.001(3) 0.005(2) -0.004(3) C31 0.024(3) 0.024(3) 0.024(3) 0.001(3) 0.003(3) -0.006(3) C32 0.014(3) 0.017(3) 0.019(3) 0.000(3) 0.005(2) 0.001(3) O1 0.028(3) 0.021(3) 0.011(2) -0.001(2) 0.006(2) -0.009(2) O2 0.019(2) 0.015(3) 0.015(2) 0.000(2) 0.0080(19) 0.004(2) O3 0.022(3) 0.017(3) 0.018(2) 0.004(2) 0.009(2) 0.001(2) O4 0.052(4) 0.048(4) 0.083(5) 0.017(4) 0.032(4) 0.008(3) O5 0.041(3) 0.025(3) 0.043(3) 0.004(3) 0.017(3) 0.010(3) O6 0.0349(16) 0.0369(16) 0.0403(16) 0.0018(9) 0.0025(9) -0.0011(9) O7 0.032(3) 0.022(3) 0.072(4) 0.009(3) 0.023(3) -0.002(3) O8 0.018(2) 0.031(3) 0.019(2) -0.007(2) 0.006(2) -0.008(2) O9 0.018(2) 0.023(3) 0.019(2) 0.003(2) 0.007(2) -0.001(2) O10 0.011(2) 0.021(3) 0.016(2) 0.000(2) 0.0032(19) -0.003(2) O11 0.014(2) 0.026(3) 0.017(2) 0.005(2) 0.0069(19) -0.002(2) O12 0.023(3) 0.045(4) 0.022(3) 0.008(3) 0.005(2) -0.007(3) O14 0.016(3) 0.031(3) 0.035(3) -0.002(3) 0.008(2) -0.006(2) O15 0.028(3) 0.022(3) 0.032(3) 0.004(2) 0.011(2) -0.004(2) O16 0.025(3) 0.045(4) 0.028(3) 0.020(3) -0.006(2) -0.004(3) O17 0.030(3) 0.023(3) 0.020(3) -0.002(2) 0.015(2) -0.008(2) O18 0.026(3) 0.016(3) 0.018(2) -0.002(2) 0.007(2) -0.009(2) S1 0.0243(10) 0.0177(10) 0.0423(12) 0.0009(9) 0.0129(9) 0.0004(8) S2 0.0204(9) 0.0270(11) 0.0265(10) 0.0077(9) 0.0034(8) -0.0009(8) Tb1 0.00966(17) 0.01376(19) 0.01031(17) 0.00006(14) 0.00378(12) 0.00071(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 C1 O3 1.267(8) . ? C1 O2 1.271(8) . ? C1 C2 1.483(10) . ? C1 Tb1 2.862(7) . ? C2 C3 1.373(10) . ? C2 C7 1.380(10) . ? C3 C4 1.396(11) . ? C4 O4 1.370(10) . ? C4 C5 1.379(10) . ? C5 C6 1.383(10) . ? C5 O5 1.417(9) . ? C6 C7 1.401(11) . ? C8 O4 1.438(10) . ? C9 C10 1.360(9) . ? C9 C16 1.389(10) . ? C9 S1 1.758(7) . ? C10 C11 1.384(9) . ? C11 C12 1.401(9) . ? C12 C14 1.384(9) . ? C12 C17 1.501(9) . ? C14 C16 1.373(9) . ? C17 O9 1.249(7) . ? C17 O8 1.253(8) . ? C18 O11 1.251(7) . ? C18 O10 1.256(7) . ? C18 C19 1.501(8) . ? C19 C20 1.379(9) . ? C19 C24 1.411(9) . ? C20 C21 1.396(9) . ? C21 C22 1.372(9) . ? C22 C23 1.384(9) . ? C22 O14 1.420(8) . ? C23 O12 1.373(8) . ? C23 C24 1.385(9) . ? C25 O12 1.425(8) . ? C26 C27 1.376(10) . ? C26 C31 1.398(9) . ? C26 S2 1.773(7) . ? C27 C28 1.392(9) . ? C28 C29 1.387(9) . ? C29 C30 1.392(9) . ? C29 C32 1.500(9) . ? C30 C31 1.370(9) . ? C32 O18 1.214(8) . ? C32 O17 1.309(8) . ? O1 Tb1 2.413(4) . ? O2 Tb1 2.438(4) . ? O3 Tb1 2.549(5) . ? O5 S1 1.577(6) . ? O6 S1 1.417(6) . ? O7 S1 1.432(6) . ? O8 Tb1 2.289(5) 2 ? O9 Tb1 2.343(4) 3_566 ? O10 Tb1 2.270(4) . ? O11 Tb1 2.307(4) 4_566 ? O14 S2 1.578(5) . ? O15 S2 1.416(5) . ? O16 S2 1.428(5) . ? O18 Tb1 2.453(5) 2_655 ? Tb1 O8 2.289(5) 2_545 ? Tb1 O11 2.307(4) 4_565 ? Tb1 O9 2.343(4) 3_566 ? Tb1 O18 2.453(5) 2_645 ? 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 C1 O2 120.0(6) . . ? O3 C1 C2 120.9(6) . . ? O2 C1 C2 119.1(6) . . ? O3 C1 Tb1 63.0(4) . . ? O2 C1 Tb1 57.9(3) . . ? C2 C1 Tb1 168.3(5) . . ? C3 C2 C7 120.7(7) . . ? C3 C2 C1 119.3(6) . . ? C7 C2 C1 119.5(7) . . ? C2 C3 C4 120.4(7) . . ? O4 C4 C5 116.4(7) . . ? O4 C4 C3 124.5(7) . . ? C5 C4 C3 118.6(7) . . ? C4 C5 C6 121.8(7) . . ? C4 C5 O5 116.3(7) . . ? C6 C5 O5 121.4(7) . . ? C5 C6 C7 118.8(7) . . ? C2 C7 C6 119.7(7) . . ? C10 C9 C16 122.0(6) . . ? C10 C9 S1 121.4(6) . . ? C16 C9 S1 116.6(5) . . ? C9 C10 C11 119.6(7) . . ? C10 C11 C12 119.9(6) . . ? C14 C12 C11 118.8(6) . . ? C14 C12 C17 120.7(6) . . ? C11 C12 C17 120.5(6) . . ? C16 C14 C12 121.7(7) . . ? C14 C16 C9 118.0(6) . . ? O9 C17 O8 124.5(6) . . ? O9 C17 C12 118.5(6) . . ? O8 C17 C12 116.9(6) . . ? O11 C18 O10 123.4(6) . . ? O11 C18 C19 118.2(6) . . ? O10 C18 C19 118.4(6) . . ? C20 C19 C24 120.9(6) . . ? C20 C19 C18 119.9(6) . . ? C24 C19 C18 119.1(6) . . ? C19 C20 C21 120.2(6) . . ? C22 C21 C20 118.1(6) . . ? C21 C22 C23 123.0(6) . . ? C21 C22 O14 119.0(6) . . ? C23 C22 O14 117.9(6) . . ? O12 C23 C22 116.0(6) . . ? O12 C23 C24 124.9(6) . . ? C22 C23 C24 119.1(6) . . ? C23 C24 C19 118.7(6) . . ? C27 C26 C31 121.2(6) . . ? C27 C26 S2 118.5(5) . . ? C31 C26 S2 120.2(5) . . ? C26 C27 C28 119.0(6) . . ? C29 C28 C27 120.0(7) . . ? C28 C29 C30 120.3(6) . . ? C28 C29 C32 117.5(6) . . ? C30 C29 C32 122.2(6) . . ? C31 C30 C29 120.0(6) . . ? C30 C31 C26 119.4(7) . . ? O18 C32 O17 123.1(6) . . ? O18 C32 C29 123.6(6) . . ? O17 C32 C29 113.4(6) . . ? C1 O2 Tb1 95.8(4) . . ? C1 O3 Tb1 90.8(4) . . ? C4 O4 C8 116.3(7) . . ? C5 O5 S1 122.2(5) . . ? C17 O8 Tb1 158.4(5) . 2 ? C17 O9 Tb1 130.5(4) . 3_566 ? C18 O10 Tb1 161.2(4) . . ? C18 O11 Tb1 134.2(4) . 4_566 ? C23 O12 C25 116.9(5) . . ? C22 O14 S2 118.6(5) . . ? C32 O18 Tb1 156.8(4) . 2_655 ? O6 S1 O7 120.7(4) . . ? O6 S1 O5 108.8(3) . . ? O7 S1 O5 102.6(3) . . ? O6 S1 C9 111.6(3) . . ? O7 S1 C9 108.0(3) . . ? O5 S1 C9 103.5(3) . . ? O15 S2 O16 120.0(3) . . ? O15 S2 O14 109.9(3) . . ? O16 S2 O14 106.2(3) . . ? O15 S2 C26 110.3(3) . . ? O16 S2 C26 108.1(3) . . ? O14 S2 C26 100.4(3) . . ? O10 Tb1 O8 142.83(18) . 2_545 ? O10 Tb1 O11 82.52(15) . 4_565 ? O8 Tb1 O11 97.10(15) 2_545 4_565 ? O10 Tb1 O9 104.64(15) . 3_566 ? O8 Tb1 O9 91.56(16) 2_545 3_566 ? O11 Tb1 O9 154.55(17) 4_565 3_566 ? O10 Tb1 O1 145.17(16) . . ? O8 Tb1 O1 71.48(17) 2_545 . ? O11 Tb1 O1 87.85(15) 4_565 . ? O9 Tb1 O1 72.26(15) 3_566 . ? O10 Tb1 O2 75.37(15) . . ? O8 Tb1 O2 76.98(16) 2_545 . ? O11 Tb1 O2 130.25(16) 4_565 . ? O9 Tb1 O2 75.01(16) 3_566 . ? O1 Tb1 O2 133.20(15) . . ? O10 Tb1 O18 74.04(16) . 2_645 ? O8 Tb1 O18 142.70(17) 2_545 2_645 ? O11 Tb1 O18 79.27(15) 4_565 2_645 ? O9 Tb1 O18 79.37(16) 3_566 2_645 ? O1 Tb1 O18 71.30(16) . 2_645 ? O2 Tb1 O18 133.10(14) . 2_645 ? O10 Tb1 O3 73.93(15) . . ? O8 Tb1 O3 69.57(16) 2_545 . ? O11 Tb1 O3 79.10(15) 4_565 . ? O9 Tb1 O3 126.30(15) 3_566 . ? O1 Tb1 O3 136.76(15) . . ? O2 Tb1 O3 52.24(14) . . ? O18 Tb1 O3 143.22(15) 2_645 . ? O10 Tb1 C1 75.55(18) . . ? O8 Tb1 C1 68.69(19) 2_545 . ? O11 Tb1 C1 105.27(18) 4_565 . ? O9 Tb1 C1 100.17(18) 3_566 . ? O1 Tb1 C1 139.21(18) . . ? O2 Tb1 C1 26.23(16) . . ? O18 Tb1 C1 148.34(18) 2_645 . ? O3 Tb1 C1 26.27(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.914 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.155 _database_code_depnum_ccdc_archive 'CCDC 956813' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Dy O17 S2' _chemical_formula_weight 882.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.3391(5) _cell_length_b 14.0385(4) _cell_length_c 9.8581(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.703(2) _cell_angle_gamma 90.00 _cell_volume 3219.09(14) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 4048 _cell_measurement_theta_min 2.8961 _cell_measurement_theta_max 29.0482 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 2.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5375 _exptl_absorpt_correction_T_max 0.7343 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12334 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5676 _reflns_number_gt 4199 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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. SIMU 0.01 0.02 3.8 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 = C17 C18 C19 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 ISOR 0.01 0.001 O5 ; _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^)+(0.0368P)^2^+13.6100P] 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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5676 _refine_ls_number_parameters 459 _refine_ls_number_restraints 540 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 0.998 _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 0.3688(3) 0.1824(4) 0.9713(8) 0.0159(13) Uani 1 1 d U . . C2 C 0.4287(3) 0.1562(5) 0.9409(8) 0.0171(13) Uani 1 1 d U . . C3 C 0.4728(3) 0.1497(5) 1.0453(8) 0.0210(14) Uani 1 1 d U . . H3 H 0.4648 0.1586 1.1353 0.025 Uiso 1 1 calc R . . C4 C 0.5285(3) 0.1298(5) 1.0144(8) 0.0215(14) Uani 1 1 d U . . H4 H 0.5582 0.1258 1.0832 0.026 Uiso 1 1 calc R . . C5 C 0.5391(3) 0.1162(5) 0.8819(8) 0.0198(13) Uani 1 1 d U . . C6 C 0.4961(3) 0.1203(5) 0.7766(9) 0.0270(15) Uani 1 1 d U . . H6 H 0.5044 0.1101 0.6871 0.032 Uiso 1 1 calc R . . C7 C 0.4403(3) 0.1398(5) 0.8071(8) 0.0241(14) Uani 1 1 d U . . H7 H 0.4107 0.1419 0.7379 0.029 Uiso 1 1 calc R . . C8 C 0.6451(3) 0.2628(5) 0.7802(9) 0.0303(15) Uani 1 1 d U . . C9 C 0.6162(3) 0.3249(5) 0.8575(9) 0.0337(15) Uani 1 1 d U . . H9 H 0.5820 0.3067 0.8925 0.040 Uiso 1 1 calc R . . C10 C 0.6387(3) 0.4156(5) 0.8827(9) 0.0336(16) Uani 1 1 d U . . H10 H 0.6201 0.4578 0.9371 0.040 Uiso 1 1 calc R . . C11 C 0.6887(3) 0.4435(5) 0.8272(8) 0.0246(15) Uani 1 1 d U . . C12 C 0.7167(3) 0.3787(5) 0.7494(9) 0.0282(15) Uani 1 1 d U . . H12 H 0.7507 0.3966 0.7131 0.034 Uiso 1 1 calc R . . C13 C 0.6952(3) 0.2887(5) 0.7250(9) 0.0304(15) Uani 1 1 d U . . C14 C 0.7628(4) 0.2594(6) 0.5609(11) 0.052(3) Uani 1 1 d U . . H14A H 0.7731 0.2104 0.4993 0.078 Uiso 1 1 calc R . . H14B H 0.7957 0.2755 0.6214 0.078 Uiso 1 1 calc R . . H14C H 0.7500 0.3148 0.5100 0.078 Uiso 1 1 calc R . . C15 C 0.7074(3) 0.5445(5) 0.8344(8) 0.0233(15) Uani 1 1 d U . . C16 C 0.1823(3) 0.2918(5) 0.9080(8) 0.0144(13) Uani 1 1 d U . . C17 C 0.1214(3) 0.3201(5) 0.9226(7) 0.0160(13) Uani 1 1 d U . . C18 C 0.1061(3) 0.3508(5) 1.0495(8) 0.0195(14) Uani 1 1 d U . . H18 H 0.1337 0.3535 1.1229 0.023 Uiso 1 1 calc R . . C19 C 0.0501(3) 0.3772(5) 1.0666(8) 0.0210(14) Uani 1 1 d U . . C20 C 0.0105(3) 0.3732(5) 0.9539(8) 0.0212(14) Uani 1 1 d U . . C21 C 0.0245(3) 0.3431(5) 0.8271(8) 0.0203(14) Uani 1 1 d U . . H21 H -0.0033 0.3399 0.7540 0.024 Uiso 1 1 calc R . . C22 C 0.0810(3) 0.3177(5) 0.8118(8) 0.0187(13) Uani 1 1 d U . . H22 H 0.0917 0.2990 0.7270 0.022 Uiso 1 1 calc R . . C23 C 0.0713(3) 0.4376(6) 1.2904(9) 0.033(2) Uani 1 1 d U . . H23A H 0.0944 0.4882 1.2584 0.050 Uiso 1 1 calc R . . H23B H 0.0955 0.3846 1.3179 0.050 Uiso 1 1 calc R . . H23C H 0.0519 0.4596 1.3667 0.050 Uiso 1 1 calc R . . C24 C -0.1251(3) 0.3975(5) 1.1368(8) 0.0228(14) Uani 1 1 d U . . C25 C -0.1039(3) 0.3850(5) 1.2706(8) 0.0235(14) Uani 1 1 d U . . H25 H -0.0720 0.3466 1.2929 0.028 Uiso 1 1 calc R . . C26 C -0.1318(3) 0.4320(5) 1.3716(8) 0.0233(14) Uani 1 1 d U . . H26 H -0.1188 0.4241 1.4626 0.028 Uiso 1 1 calc R . . C27 C -0.1784(3) 0.4898(5) 1.3373(8) 0.0179(13) Uani 1 1 d U . . C28 C -0.1986(3) 0.5001(5) 1.2019(9) 0.0210(14) Uani 1 1 d U . . C29 C -0.1721(3) 0.4547(5) 1.0996(8) 0.0224(14) Uani 1 1 d U . . H29 H -0.1853 0.4624 1.0087 0.027 Uiso 1 1 calc R . . C30 C -0.2095(3) 0.5405(5) 1.4421(8) 0.0182(14) Uani 1 1 d U . . O1 O 0.19466(19) 0.2358(3) 1.2912(5) 0.0167(11) Uani 1 1 d . . . O2 O 0.3177(2) 0.1252(3) 1.3273(5) 0.0207(12) Uani 1 1 d . . . H2A H 0.2924 0.1048 1.3781 0.031 Uiso 1 1 d R . . H2B H 0.3273 0.0801 1.2756 0.031 Uiso 1 1 d R . . O3 O 0.36005(19) 0.2010(3) 1.0932(5) 0.0190(11) Uani 1 1 d . . . O4 O 0.33110(19) 0.1844(3) 0.8747(5) 0.0213(12) Uani 1 1 d . . . O5 O 0.6500(2) 0.0975(4) 0.9511(6) 0.0350(14) Uani 1 1 d U . . O6 O 0.6058(2) 0.0095(4) 0.7502(7) 0.0421(17) Uani 1 1 d . . . O7 O 0.6207(2) 0.1739(4) 0.7342(6) 0.0361(15) Uani 1 1 d . . . O8 O 0.7171(3) 0.2254(4) 0.6392(8) 0.057(2) Uani 1 1 d . . . O9 O 0.7494(2) 0.5732(3) 0.7718(5) 0.0190(12) Uani 1 1 d . . . O10 O 0.67901(19) 0.6032(3) 0.9013(5) 0.0156(11) Uani 1 1 d . . . O11 O 0.21816(18) 0.2965(3) 1.0085(5) 0.0170(11) Uani 1 1 d . . . O12 O 0.0298(2) 0.4086(4) 1.1838(6) 0.0309(13) Uani 1 1 d . . . O13 O -0.0457(2) 0.4067(3) 0.9685(6) 0.0267(13) Uani 1 1 d . . . O14 O -0.1345(2) 0.3287(4) 0.8887(6) 0.0337(14) Uani 1 1 d . . . O15 O -0.0673(2) 0.2493(3) 1.0596(6) 0.0262(13) Uani 1 1 d . . . O16 O -0.2431(2) 0.6062(3) 1.4150(5) 0.0192(11) Uani 1 1 d . . . O17 O -0.1976(2) 0.5083(3) 1.5660(5) 0.0244(12) Uani 1 1 d . . . H17 H -0.2174 0.5363 1.6183 0.037 Uiso 1 1 calc R . . S1 S 0.60887(8) 0.09159(13) 0.8362(2) 0.0275(5) Uani 1 1 d . . . S2 S -0.09366(8) 0.33356(13) 1.0051(2) 0.0253(5) Uani 1 1 d . . . Dy1 Dy 0.278359(12) 0.25479(2) 1.18921(3) 0.01128(12) Uani 1 1 d . . . H28 H -0.227(3) 0.522(5) 1.176(8) 0.03(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(3) 0.013(3) 0.017(3) 0.002(3) 0.006(3) -0.001(2) C2 0.013(3) 0.017(3) 0.022(3) -0.003(3) 0.004(3) 0.001(2) C3 0.018(3) 0.024(3) 0.021(3) -0.005(3) 0.006(3) -0.001(2) C4 0.018(3) 0.023(3) 0.023(3) -0.004(3) 0.001(3) 0.001(2) C5 0.017(3) 0.019(3) 0.024(3) -0.004(3) 0.006(3) -0.001(2) C6 0.022(3) 0.034(3) 0.025(3) -0.004(3) 0.009(3) 0.005(3) C7 0.021(3) 0.032(3) 0.020(3) -0.004(3) 0.003(3) 0.004(3) C8 0.028(3) 0.022(3) 0.043(4) -0.005(3) 0.015(3) -0.008(3) C9 0.032(3) 0.026(3) 0.046(3) -0.007(3) 0.019(3) -0.007(3) C10 0.035(3) 0.024(3) 0.044(4) -0.011(3) 0.018(3) -0.005(3) C11 0.026(3) 0.017(3) 0.032(3) -0.004(3) 0.010(3) -0.008(2) C12 0.023(3) 0.025(3) 0.039(3) -0.006(3) 0.016(3) -0.007(3) C13 0.026(3) 0.022(3) 0.045(4) -0.010(3) 0.017(3) -0.003(3) C14 0.037(5) 0.055(5) 0.067(7) -0.008(5) 0.025(5) -0.002(4) C15 0.026(3) 0.016(3) 0.029(4) -0.003(3) 0.008(3) -0.004(3) C16 0.012(3) 0.015(3) 0.016(3) 0.005(3) 0.004(3) 0.004(2) C17 0.014(3) 0.020(3) 0.016(3) 0.002(3) 0.007(2) 0.004(2) C18 0.014(3) 0.025(3) 0.019(3) 0.001(3) 0.003(3) 0.005(2) C19 0.021(3) 0.026(3) 0.018(3) 0.002(3) 0.011(3) 0.005(2) C20 0.015(3) 0.028(3) 0.022(3) -0.001(3) 0.006(3) 0.009(2) C21 0.018(3) 0.026(3) 0.018(3) -0.001(3) 0.004(3) 0.007(2) C22 0.018(3) 0.023(3) 0.016(3) -0.001(3) 0.007(3) 0.006(2) C23 0.035(4) 0.038(4) 0.027(5) -0.007(4) 0.009(4) 0.003(4) C24 0.019(3) 0.027(3) 0.023(3) 0.000(3) 0.007(3) 0.006(2) C25 0.020(3) 0.027(3) 0.024(3) 0.002(3) 0.002(3) 0.006(2) C26 0.022(3) 0.027(3) 0.021(3) -0.002(3) 0.003(3) 0.003(2) C27 0.019(3) 0.016(3) 0.019(3) -0.001(3) 0.007(3) 0.000(2) C28 0.019(3) 0.021(3) 0.023(3) 0.002(3) 0.003(3) 0.002(3) C29 0.022(3) 0.027(3) 0.019(3) 0.003(3) 0.003(3) 0.004(2) C30 0.016(3) 0.019(3) 0.020(3) 0.004(3) 0.005(3) -0.003(2) O1 0.011(2) 0.025(3) 0.014(3) 0.005(2) 0.004(2) -0.0007(19) O2 0.026(3) 0.019(3) 0.019(3) 0.000(2) 0.012(2) 0.009(2) O3 0.013(2) 0.026(3) 0.018(3) -0.005(2) 0.003(2) 0.0007(19) O4 0.013(3) 0.031(3) 0.020(3) 0.003(2) 0.003(2) 0.008(2) O5 0.0330(16) 0.0344(16) 0.0375(16) -0.0021(9) 0.0018(10) 0.0010(9) O6 0.035(3) 0.020(3) 0.073(5) -0.015(3) 0.018(3) -0.002(2) O7 0.032(3) 0.030(3) 0.050(4) -0.006(3) 0.018(3) -0.014(2) O8 0.052(4) 0.039(4) 0.086(6) -0.010(4) 0.033(4) -0.001(3) O9 0.021(3) 0.013(2) 0.024(3) -0.006(2) 0.010(2) -0.0038(19) O10 0.022(3) 0.009(2) 0.018(3) -0.001(2) 0.009(2) -0.0020(18) O11 0.009(2) 0.023(3) 0.020(3) 0.002(2) 0.002(2) 0.0030(18) O12 0.023(3) 0.047(3) 0.023(3) -0.005(3) 0.007(3) 0.003(2) O13 0.017(3) 0.030(3) 0.033(4) 0.003(3) 0.005(2) 0.009(2) O14 0.022(3) 0.046(3) 0.032(4) -0.019(3) -0.004(3) 0.008(2) O15 0.030(3) 0.021(3) 0.028(3) -0.007(2) 0.009(3) 0.004(2) O16 0.024(3) 0.014(2) 0.020(3) 0.003(2) 0.007(2) 0.006(2) O17 0.031(3) 0.028(3) 0.016(3) 0.003(2) 0.014(2) 0.011(2) S1 0.0224(10) 0.0186(9) 0.0431(14) -0.0013(10) 0.0119(10) -0.0004(7) S2 0.0206(10) 0.0276(10) 0.0279(12) -0.0080(9) 0.0031(9) 0.0007(8) Dy1 0.00903(17) 0.01405(18) 0.0113(2) -0.00007(15) 0.00399(13) -0.00063(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 C1 O4 1.243(8) . ? C1 O3 1.262(8) . ? C1 C2 1.502(9) . ? C2 C7 1.387(10) . ? C2 C3 1.397(10) . ? C3 C4 1.388(9) . ? C4 C5 1.362(10) . ? C5 C6 1.385(10) . ? C5 S1 1.760(7) . ? C6 C7 1.387(10) . ? C8 C9 1.371(10) . ? C8 C13 1.378(10) . ? C8 O7 1.430(9) . ? C9 C10 1.393(10) . ? C10 C11 1.385(10) . ? C11 C12 1.388(10) . ? C11 C15 1.484(9) . ? C12 C13 1.375(10) . ? C13 O8 1.355(9) . ? C14 O8 1.449(10) . ? C15 O9 1.265(8) . ? C15 O10 1.275(8) . ? C15 Dy1 2.848(7) 3_667 ? C16 O11 1.245(8) . ? C16 O1 1.270(8) 4_565 ? C16 C17 1.495(9) . ? C17 C22 1.384(10) . ? C17 C18 1.398(10) . ? C18 C19 1.381(9) . ? C19 O12 1.358(8) . ? C19 C20 1.387(10) . ? C20 C21 1.384(10) . ? C20 O13 1.410(8) . ? C21 C22 1.386(9) . ? C23 O12 1.429(9) . ? C24 C25 1.382(10) . ? C24 C29 1.384(10) . ? C24 S2 1.785(7) . ? C25 C26 1.399(10) . ? C26 C27 1.377(9) . ? C27 C28 1.386(11) . ? C27 C30 1.492(9) . ? C28 C29 1.382(10) . ? C30 O16 1.225(8) . ? C30 O17 1.311(8) . ? O1 C16 1.270(8) 4_566 ? O1 Dy1 2.285(4) . ? O2 Dy1 2.408(5) . ? O3 Dy1 2.323(4) . ? O4 Dy1 2.284(5) 4_565 ? O5 S1 1.426(6) . ? O6 S1 1.429(6) . ? O7 S1 1.571(6) . ? O9 Dy1 2.538(4) 3_667 ? O10 Dy1 2.430(4) 3_667 ? O11 Dy1 2.254(5) . ? O13 S2 1.583(5) . ? O14 S2 1.432(6) . ? O15 S2 1.419(5) . ? O16 Dy1 2.438(4) 2_557 ? Dy1 O4 2.284(5) 4_566 ? Dy1 O10 2.430(4) 3_667 ? Dy1 O16 2.438(4) 2_547 ? Dy1 O9 2.538(4) 3_667 ? Dy1 C15 2.848(7) 3_667 ? 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 C1 O3 124.5(6) . . ? O4 C1 C2 117.7(6) . . ? O3 C1 C2 117.8(7) . . ? C7 C2 C3 120.1(6) . . ? C7 C2 C1 119.2(7) . . ? C3 C2 C1 120.7(7) . . ? C4 C3 C2 119.9(7) . . ? C5 C4 C3 119.0(7) . . ? C4 C5 C6 122.4(7) . . ? C4 C5 S1 121.1(6) . . ? C6 C5 S1 116.4(6) . . ? C5 C6 C7 118.8(7) . . ? C2 C7 C6 119.8(7) . . ? C9 C8 C13 121.6(7) . . ? C9 C8 O7 122.0(7) . . ? C13 C8 O7 115.7(7) . . ? C8 C9 C10 119.0(7) . . ? C11 C10 C9 120.4(7) . . ? C10 C11 C12 119.0(7) . . ? C10 C11 C15 120.4(7) . . ? C12 C11 C15 120.1(6) . . ? C13 C12 C11 121.1(7) . . ? O8 C13 C12 124.2(7) . . ? O8 C13 C8 116.7(7) . . ? C12 C13 C8 118.9(7) . . ? O9 C15 O10 120.2(6) . . ? O9 C15 C11 121.1(6) . . ? O10 C15 C11 118.6(6) . . ? O9 C15 Dy1 63.0(3) . 3_667 ? O10 C15 Dy1 58.1(3) . 3_667 ? C11 C15 Dy1 167.7(6) . 3_667 ? O11 C16 O1 123.4(6) . 4_565 ? O11 C16 C17 119.5(6) . . ? O1 C16 C17 117.1(6) 4_565 . ? C22 C17 C18 120.4(6) . . ? C22 C17 C16 120.7(6) . . ? C18 C17 C16 118.9(7) . . ? C19 C18 C17 120.4(7) . . ? O12 C19 C18 126.2(7) . . ? O12 C19 C20 116.0(6) . . ? C18 C19 C20 117.9(7) . . ? C21 C20 C19 123.0(6) . . ? C21 C20 O13 118.9(7) . . ? C19 C20 O13 118.0(6) . . ? C20 C21 C22 118.3(7) . . ? C17 C22 C21 120.1(7) . . ? C25 C24 C29 122.8(7) . . ? C25 C24 S2 119.6(5) . . ? C29 C24 S2 117.6(6) . . ? C24 C25 C26 117.9(7) . . ? C27 C26 C25 120.6(7) . . ? C26 C27 C28 119.8(7) . . ? C26 C27 C30 122.1(7) . . ? C28 C27 C30 118.0(6) . . ? C29 C28 C27 121.1(7) . . ? C28 C29 C24 117.8(8) . . ? O16 C30 O17 123.1(7) . . ? O16 C30 C27 123.2(7) . . ? O17 C30 C27 113.7(6) . . ? C16 O1 Dy1 134.4(4) 4_566 . ? C1 O3 Dy1 131.0(5) . . ? C1 O4 Dy1 157.4(4) . 4_565 ? C8 O7 S1 121.7(6) . . ? C13 O8 C14 116.6(6) . . ? C15 O9 Dy1 90.6(4) . 3_667 ? C15 O10 Dy1 95.4(4) . 3_667 ? C16 O11 Dy1 161.8(4) . . ? C19 O12 C23 117.2(6) . . ? C20 O13 S2 119.2(4) . . ? C30 O16 Dy1 157.4(5) . 2_557 ? O5 S1 O6 121.1(3) . . ? O5 S1 O7 108.9(3) . . ? O6 S1 O7 102.5(3) . . ? O5 S1 C5 111.2(4) . . ? O6 S1 C5 107.9(3) . . ? O7 S1 C5 103.6(3) . . ? O15 S2 O14 120.2(3) . . ? O15 S2 O13 109.5(3) . . ? O14 S2 O13 106.6(3) . . ? O15 S2 C24 109.6(3) . . ? O14 S2 C24 108.7(3) . . ? O13 S2 C24 100.4(3) . . ? O11 Dy1 O4 142.73(17) . 4_566 ? O11 Dy1 O1 82.99(16) . . ? O4 Dy1 O1 96.63(16) 4_566 . ? O11 Dy1 O3 103.98(17) . . ? O4 Dy1 O3 92.35(17) 4_566 . ? O1 Dy1 O3 154.32(16) . . ? O11 Dy1 O2 145.77(17) . . ? O4 Dy1 O2 71.00(17) 4_566 . ? O1 Dy1 O2 87.87(16) . . ? O3 Dy1 O2 72.39(16) . . ? O11 Dy1 O10 75.18(16) . 3_667 ? O4 Dy1 O10 77.15(17) 4_566 3_667 ? O1 Dy1 O10 130.39(15) . 3_667 ? O3 Dy1 O10 75.08(15) . 3_667 ? O2 Dy1 O10 132.75(16) . 3_667 ? O11 Dy1 O16 73.86(16) . 2_547 ? O4 Dy1 O16 142.94(17) 4_566 2_547 ? O1 Dy1 O16 79.29(16) . 2_547 ? O3 Dy1 O16 79.07(16) . 2_547 ? O2 Dy1 O16 72.04(17) . 2_547 ? O10 Dy1 O16 132.93(16) 3_667 2_547 ? O11 Dy1 O9 73.87(16) . 3_667 ? O4 Dy1 O9 69.56(17) 4_566 3_667 ? O1 Dy1 O9 78.84(15) . 3_667 ? O3 Dy1 O9 126.81(15) . 3_667 ? O2 Dy1 O9 136.34(16) . 3_667 ? O10 Dy1 O9 52.58(14) 3_667 3_667 ? O16 Dy1 O9 142.78(16) 2_547 3_667 ? O11 Dy1 C15 75.4(2) . 3_667 ? O4 Dy1 C15 68.7(2) 4_566 3_667 ? O1 Dy1 C15 105.13(18) . 3_667 ? O3 Dy1 C15 100.55(19) . 3_667 ? O2 Dy1 C15 138.8(2) . 3_667 ? O10 Dy1 C15 26.47(17) 3_667 3_667 ? O16 Dy1 C15 148.1(2) 2_547 3_667 ? O9 Dy1 C15 26.37(17) 3_667 3_667 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.986 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.163 _database_code_depnum_ccdc_archive 'CCDC 956814' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Ho O17 S2' _chemical_formula_weight 884.53 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.327(2) _cell_length_b 14.0248(11) _cell_length_c 9.8469(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.653(7) _cell_angle_gamma 90.00 _cell_volume 3210.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 1413 _cell_measurement_theta_min 3.0281 _cell_measurement_theta_max 29.0200 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 2.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5544 _exptl_absorpt_correction_T_max 0.7757 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12179 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.1987 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5655 _reflns_number_gt 3028 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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. SIMU 0.01 0.02 3.8 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 = C17 C18 C19 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 ISOR 0.01 0.001 O12 ; _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^)+(0.0055P)^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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5655 _refine_ls_number_parameters 455 _refine_ls_number_restraints 534 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 0.976 _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 0.3179(6) 0.7920(9) 0.5925(11) 0.019(2) Uani 1 1 d U . . C2 C 0.3786(5) 0.8201(9) 0.5763(11) 0.017(2) Uani 1 1 d U . . C3 C 0.4180(5) 0.8168(9) 0.6872(11) 0.020(2) Uani 1 1 d U . . H3 H 0.4066 0.7977 0.7713 0.024 Uiso 1 1 calc R . . C4 C 0.4755(5) 0.8420(8) 0.6742(11) 0.018(2) Uani 1 1 d U . . H4 H 0.5029 0.8397 0.7481 0.022 Uiso 1 1 calc R . . C5 C 0.4895(6) 0.8707(9) 0.5460(12) 0.021(2) Uani 1 1 d U . . C6 C 0.4494(6) 0.8771(9) 0.4343(11) 0.020(2) Uani 1 1 d U . . C7 C 0.3919(6) 0.8509(9) 0.4481(11) 0.019(2) Uani 1 1 d U . . H7 H 0.3641 0.8541 0.3750 0.023 Uiso 1 1 calc R . . C8 C 0.4292(6) 0.9389(10) 0.2096(11) 0.032(3) Uani 1 1 d U . . H8A H 0.4489 0.9696 0.1398 0.048 Uiso 1 1 calc R . . H8B H 0.4031 0.9832 0.2462 0.048 Uiso 1 1 calc R . . H8C H 0.4081 0.8852 0.1716 0.048 Uiso 1 1 calc R . . C9 C 0.2907(6) 0.5396(9) 0.4392(12) 0.019(2) Uani 1 1 d U . . C10 C 0.3212(5) 0.4920(9) 0.3381(11) 0.020(2) Uani 1 1 d U . . C11 C 0.3689(6) 0.4327(9) 0.3711(11) 0.023(2) Uani 1 1 d U . . H11 H 0.3820 0.4240 0.4620 0.028 Uiso 1 1 calc R . . C12 C 0.3963(6) 0.3877(9) 0.2719(11) 0.024(2) Uani 1 1 d U . . H12 H 0.4292 0.3516 0.2943 0.029 Uiso 1 1 calc R . . C13 C 0.3742(6) 0.3967(9) 0.1352(11) 0.020(2) Uani 1 1 d U . . C14 C 0.3280(6) 0.4533(9) 0.1004(12) 0.023(2) Uani 1 1 d U . . H14 H 0.3155 0.4613 0.0090 0.027 Uiso 1 1 calc R . . C15 C 0.2992(5) 0.4991(9) 0.1994(11) 0.019(2) Uani 1 1 d U . . H15 H 0.2661 0.5341 0.1754 0.023 Uiso 1 1 calc R . . C16 C 0.1307(6) 0.6827(9) 0.5266(11) 0.018(2) Uani 1 1 d U . . C17 C 0.0712(6) 0.6548(9) 0.5583(11) 0.017(2) Uani 1 1 d U . . C18 C 0.0276(6) 0.6490(9) 0.4559(11) 0.019(2) Uani 1 1 d U . . H18 H 0.0356 0.6591 0.3660 0.023 Uiso 1 1 calc R . . C19 C -0.0283(6) 0.6283(9) 0.4850(11) 0.020(2) Uani 1 1 d U . . H19 H -0.0575 0.6228 0.4154 0.024 Uiso 1 1 calc R . . C20 C -0.0396(6) 0.6162(9) 0.6190(11) 0.0191(19) Uani 1 1 d U . . C21 C 0.0041(6) 0.6195(9) 0.7224(11) 0.021(2) Uani 1 1 d U . . H21 H -0.0035 0.6081 0.8122 0.025 Uiso 1 1 calc R . . C22 C 0.0574(6) 0.6394(9) 0.6909(11) 0.024(2) Uani 1 1 d U . . H22 H 0.0866 0.6431 0.7610 0.029 Uiso 1 1 calc R . . C23 C -0.1452(6) 0.7624(10) 0.7201(12) 0.029(2) Uani 1 1 d U . . C24 C -0.1164(6) 0.8245(9) 0.6409(12) 0.030(2) Uani 1 1 d U . . H24 H -0.0823 0.8066 0.6050 0.036 Uiso 1 1 calc R . . C25 C -0.1401(6) 0.9157(10) 0.6164(12) 0.030(2) Uani 1 1 d U . . H25 H -0.1219 0.9580 0.5613 0.037 Uiso 1 1 calc R . . C26 C -0.1886(6) 0.9433(10) 0.6706(12) 0.026(2) Uani 1 1 d U . . C27 C -0.2172(6) 0.8799(9) 0.7481(12) 0.029(2) Uani 1 1 d U . . H27 H -0.2512 0.8980 0.7844 0.035 Uiso 1 1 calc R . . C28 C -0.1954(6) 0.7894(10) 0.7716(13) 0.029(2) Uani 1 1 d U . . C29 C -0.2639(6) 0.7593(11) 0.9391(13) 0.050(4) Uani 1 1 d U . . H29A H -0.2978 0.7719 0.8799 0.075 Uiso 1 1 calc R . . H29B H -0.2517 0.8169 0.9858 0.075 Uiso 1 1 calc R . . H29C H -0.2723 0.7116 1.0045 0.075 Uiso 1 1 calc R . . C30 C -0.2064(6) 1.0459(10) 0.6668(13) 0.027(2) Uani 1 1 d U . . O1 O 0.1406(3) 0.7010(6) 0.4072(7) 0.016(2) Uani 1 1 d . . . O2 O 0.1835(4) 0.6257(6) 0.1736(7) 0.022(2) Uani 1 1 d . . . H2A H 0.1609 0.5912 0.2189 0.033 Uiso 1 1 d R . . H2B H 0.1641 0.6477 0.1017 0.033 Uiso 1 1 d R . . O3 O 0.2558(4) 0.6063(6) 0.4144(7) 0.023(2) Uani 1 1 d . . . O4 O 0.3046(3) 0.7361(6) 0.2095(7) 0.017(2) Uani 1 1 d . . . O5 O 0.2816(3) 0.7952(6) 0.4909(7) 0.016(2) Uani 1 1 d . . . O6 O 0.4703(4) 0.9071(7) 0.3163(8) 0.036(3) Uani 1 1 d . . . O7 O 0.3030(4) 0.5099(7) 0.5657(7) 0.030(3) Uani 1 1 d . . . H7A H 0.2935 0.5507 0.6191 0.045 Uiso 1 1 calc R . . O8 O 0.4543(4) 0.4063(7) -0.0324(8) 0.031(2) Uani 1 1 d . . . O9 O 0.4325(4) 0.2485(7) 0.0567(7) 0.030(2) Uani 1 1 d . . . O10 O 0.3665(4) 0.3296(7) -0.1127(8) 0.040(3) Uani 1 1 d . . . O11 O 0.1692(4) 0.6865(6) 0.6264(7) 0.020(2) Uani 1 1 d . . . O12 O -0.1500(4) 0.5961(7) 0.5477(8) 0.037(3) Uani 1 1 d U . . O13 O -0.1209(4) 0.6743(7) 0.7635(8) 0.032(3) Uani 1 1 d . . . O14 O -0.1071(4) 0.5093(6) 0.7504(10) 0.042(3) Uani 1 1 d . . . O15 O -0.2177(5) 0.7250(8) 0.8579(10) 0.063(4) Uani 1 1 d . . . O16 O -0.2492(4) 1.0741(6) 0.7282(7) 0.021(2) Uani 1 1 d . . . O17 O -0.1780(3) 1.1032(6) 0.5995(7) 0.016(2) Uani 1 1 d . . . S1 S 0.40644(16) 0.3343(3) 0.0043(3) 0.0263(9) Uani 1 1 d . . . S2 S -0.10925(16) 0.5920(3) 0.6636(3) 0.0269(9) Uani 1 1 d . . . Ho1 Ho 0.22145(2) 0.75449(5) 0.31041(5) 0.01193(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 0.017(5) 0.019(4) 0.022(4) -0.001(4) 0.007(4) -0.005(4) C2 0.018(4) 0.016(4) 0.018(4) 0.001(4) 0.006(4) -0.003(4) C3 0.022(4) 0.021(4) 0.017(4) 0.002(4) 0.007(4) 0.000(4) C4 0.019(4) 0.017(4) 0.019(4) 0.002(4) 0.003(4) -0.003(4) C5 0.018(5) 0.021(4) 0.023(4) -0.002(4) -0.001(4) -0.005(4) C6 0.020(4) 0.020(4) 0.019(4) 0.001(4) 0.007(4) -0.003(4) C7 0.019(4) 0.022(4) 0.018(4) -0.001(4) 0.007(4) -0.001(4) C8 0.032(8) 0.041(8) 0.022(6) 0.009(6) -0.005(6) -0.020(7) C9 0.020(5) 0.021(5) 0.019(4) 0.000(4) 0.009(4) 0.000(4) C10 0.017(4) 0.024(5) 0.019(4) -0.003(4) 0.012(4) 0.002(4) C11 0.025(5) 0.026(5) 0.019(4) 0.001(4) 0.005(4) 0.003(4) C12 0.023(4) 0.029(5) 0.021(4) -0.001(4) 0.009(4) 0.005(4) C13 0.017(5) 0.025(5) 0.019(4) -0.005(4) 0.007(4) 0.005(4) C14 0.023(5) 0.027(5) 0.019(4) -0.003(4) 0.006(4) 0.002(4) C15 0.018(4) 0.023(4) 0.018(4) -0.002(4) 0.006(4) 0.002(4) C16 0.027(5) 0.012(4) 0.015(4) 0.003(4) 0.007(4) -0.007(4) C17 0.022(4) 0.014(4) 0.016(4) -0.005(4) 0.008(4) -0.007(4) C18 0.026(4) 0.017(4) 0.016(4) -0.002(4) 0.011(4) -0.006(4) C19 0.025(4) 0.018(4) 0.016(4) -0.006(4) 0.005(4) -0.002(4) C20 0.023(4) 0.014(4) 0.022(4) -0.001(4) 0.014(3) -0.006(4) C21 0.023(4) 0.023(4) 0.017(4) -0.001(4) 0.012(4) -0.008(4) C22 0.028(4) 0.024(4) 0.021(4) -0.001(4) 0.009(4) -0.008(4) C23 0.033(4) 0.019(4) 0.037(4) 0.005(4) 0.013(4) 0.005(4) C24 0.034(4) 0.021(4) 0.037(4) 0.008(4) 0.017(4) 0.005(4) C25 0.034(5) 0.023(4) 0.036(4) 0.015(4) 0.016(4) 0.003(4) C26 0.029(5) 0.021(4) 0.030(4) 0.005(4) 0.015(4) 0.004(4) C27 0.030(5) 0.021(4) 0.038(4) 0.008(4) 0.015(4) 0.005(4) C28 0.031(5) 0.022(4) 0.038(4) 0.012(4) 0.019(4) 0.001(4) C29 0.043(8) 0.047(8) 0.063(8) 0.010(8) 0.024(7) 0.005(8) C30 0.031(5) 0.023(5) 0.030(4) 0.007(4) 0.014(4) 0.001(4) O1 0.013(5) 0.026(6) 0.010(4) 0.004(4) 0.000(4) 0.001(4) O2 0.036(6) 0.019(5) 0.011(4) 0.001(4) 0.004(4) -0.004(5) O3 0.030(6) 0.018(5) 0.020(5) -0.003(4) 0.002(4) 0.001(5) O4 0.021(5) 0.015(5) 0.014(4) 0.003(4) 0.004(4) 0.001(5) O5 0.007(5) 0.024(5) 0.017(4) -0.004(4) 0.002(4) -0.004(4) O6 0.024(6) 0.044(7) 0.038(6) 0.010(5) -0.002(5) -0.007(6) O7 0.045(7) 0.035(7) 0.011(4) 0.000(4) 0.007(5) 0.012(6) O8 0.009(5) 0.040(7) 0.043(6) 0.008(5) 0.008(4) 0.005(5) O9 0.034(6) 0.027(6) 0.032(5) -0.004(5) 0.014(4) 0.015(6) O10 0.032(7) 0.044(7) 0.043(6) -0.025(5) -0.006(5) -0.004(6) O11 0.019(6) 0.032(6) 0.009(4) -0.008(4) 0.002(4) -0.004(5) O12 0.036(3) 0.036(3) 0.037(3) 0.0005(10) 0.0024(10) -0.0007(10) O13 0.036(7) 0.024(6) 0.037(5) -0.002(5) 0.012(5) -0.001(5) O14 0.034(7) 0.010(6) 0.086(8) 0.011(5) 0.020(6) -0.004(5) O15 0.047(8) 0.073(10) 0.072(7) 0.008(7) 0.023(6) 0.011(7) O16 0.019(6) 0.019(5) 0.026(5) -0.005(4) 0.009(4) 0.001(5) O17 0.015(5) 0.014(5) 0.019(4) -0.006(4) 0.009(4) 0.000(4) S1 0.025(2) 0.025(2) 0.0292(19) -0.0078(18) 0.0018(17) 0.0015(19) S2 0.025(2) 0.023(2) 0.034(2) 0.0004(18) 0.0109(17) -0.0005(19) Ho1 0.0106(3) 0.0155(3) 0.0102(3) -0.0006(3) 0.0035(2) 0.0006(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 C1 O5 1.259(13) . ? C1 O4 1.279(12) 4_576 ? C1 C2 1.491(16) . ? C2 C3 1.369(16) . ? C2 C7 1.393(14) . ? C3 C4 1.403(16) . ? C3 H3 0.9300 . ? C4 C5 1.389(14) . ? C4 H4 0.9300 . ? C5 C6 1.389(16) . ? C5 O8 1.420(14) 2_655 ? C6 O6 1.363(12) . ? C6 C7 1.407(16) . ? C7 H7 0.9300 . ? C8 O6 1.435(13) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O3 1.250(14) . ? C9 O7 1.324(13) . ? C9 C10 1.434(15) . ? C10 C11 1.408(17) . ? C10 C15 1.422(15) . ? C11 C12 1.364(15) . ? C11 H11 0.9300 . ? C12 C13 1.408(15) . ? C12 H12 0.9300 . ? C13 C14 1.360(17) . ? C13 S1 1.774(12) . ? C14 C15 1.385(14) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.243(11) . ? C16 O11 1.278(14) . ? C16 C17 1.498(16) . ? C17 C18 1.377(16) . ? C17 C22 1.386(14) . ? C18 C19 1.387(16) . ? C18 H18 0.9300 . ? C19 C20 1.376(14) . ? C19 H19 0.9300 . ? C20 C21 1.381(17) . ? C20 S2 1.752(13) . ? C21 C22 1.337(16) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.366(17) . ? C23 C24 1.379(16) . ? C23 O13 1.411(15) . ? C24 C25 1.407(17) . ? C24 H24 0.9300 . ? C25 C26 1.347(17) . ? C25 H25 0.9300 . ? C26 C27 1.379(16) . ? C26 C30 1.497(17) . ? C27 C28 1.380(17) . ? C27 H27 0.9300 . ? C28 O15 1.372(15) . ? C29 O15 1.474(14) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O17 1.262(14) . ? C30 O16 1.271(14) . ? C30 Ho1 2.832(14) 3_576 ? O1 Ho1 2.306(7) . ? O2 Ho1 2.381(7) . ? O2 H2A 0.8657 . ? O2 H2B 0.8655 . ? O3 Ho1 2.424(8) . ? O4 C1 1.279(12) 4_575 ? O4 Ho1 2.266(7) . ? O5 Ho1 2.247(7) . ? O7 H7A 0.8200 . ? O8 C5 1.420(14) 2_645 ? O8 S1 1.569(9) . ? O9 S1 1.426(9) . ? O10 S1 1.424(9) . ? O11 Ho1 2.257(7) 4_576 ? O12 S2 1.427(9) . ? O13 S2 1.555(9) . ? O14 S2 1.439(9) . ? O16 Ho1 2.527(8) 3_576 ? O17 Ho1 2.438(7) 3_576 ? Ho1 O11 2.257(7) 4_575 ? Ho1 O17 2.438(7) 3_576 ? Ho1 O16 2.527(8) 3_576 ? Ho1 C30 2.832(14) 3_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 C1 O4 122.1(12) . 4_576 ? O5 C1 C2 119.3(10) . . ? O4 C1 C2 118.6(11) 4_576 . ? C3 C2 C7 123.3(12) . . ? C3 C2 C1 119.1(10) . . ? C7 C2 C1 117.5(11) . . ? C2 C3 C4 120.2(11) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 117.0(12) . . ? C5 C4 H4 121.5 . . ? C3 C4 H4 121.5 . . ? C6 C5 C4 123.1(12) . . ? C6 C5 O8 118.1(11) . 2_655 ? C4 C5 O8 118.4(11) . 2_655 ? O6 C6 C5 115.5(12) . . ? O6 C6 C7 125.0(11) . . ? C5 C6 C7 119.5(11) . . ? C2 C7 C6 116.9(12) . . ? C2 C7 H7 121.5 . . ? C6 C7 H7 121.5 . . ? O6 C8 H8A 109.5 . . ? O6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 O7 120.5(11) . . ? O3 C9 C10 124.3(12) . . ? O7 C9 C10 115.1(12) . . ? C11 C10 C15 118.6(11) . . ? C11 C10 C9 122.9(11) . . ? C15 C10 C9 118.3(12) . . ? C12 C11 C10 121.1(11) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 119.1(13) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 120.9(11) . . ? C14 C13 S1 118.6(9) . . ? C12 C13 S1 120.4(10) . . ? C13 C14 C15 120.9(12) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 119.1(12) . . ? C14 C15 H15 120.5 . . ? C10 C15 H15 120.5 . . ? O1 C16 O11 123.1(12) . . ? O1 C16 C17 119.9(11) . . ? O11 C16 C17 117.1(10) . . ? C18 C17 C22 117.8(12) . . ? C18 C17 C16 120.3(10) . . ? C22 C17 C16 121.8(11) . . ? C17 C18 C19 120.8(11) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 118.7(12) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 121.0(12) . . ? C19 C20 S2 121.2(10) . . ? C21 C20 S2 117.7(9) . . ? C22 C21 C20 118.7(11) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C17 122.9(13) . . ? C21 C22 H22 118.6 . . ? C17 C22 H22 118.6 . . ? C28 C23 C24 120.4(14) . . ? C28 C23 O13 117.7(12) . . ? C24 C23 O13 121.4(12) . . ? C23 C24 C25 117.9(13) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? C26 C25 C24 121.6(13) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C27 119.6(13) . . ? C25 C26 C30 120.4(13) . . ? C27 C26 C30 119.3(12) . . ? C26 C27 C28 119.8(13) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C23 C28 O15 115.3(13) . . ? C23 C28 C27 120.6(13) . . ? O15 C28 C27 123.8(13) . . ? O15 C29 H29A 109.5 . . ? O15 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O15 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O17 C30 O16 121.2(13) . . ? O17 C30 C26 118.0(12) . . ? O16 C30 C26 120.8(12) . . ? O17 C30 Ho1 59.1(7) . 3_576 ? O16 C30 Ho1 63.2(7) . 3_576 ? C26 C30 Ho1 169.7(11) . 3_576 ? C16 O1 Ho1 132.8(8) . . ? Ho1 O2 H2A 110.3 . . ? Ho1 O2 H2B 109.8 . . ? H2A O2 H2B 108.6 . . ? C9 O3 Ho1 155.7(8) . . ? C1 O4 Ho1 135.1(8) 4_575 . ? C1 O5 Ho1 163.1(9) . . ? C6 O6 C8 117.1(10) . . ? C9 O7 H7A 109.5 . . ? C5 O8 S1 118.3(9) 2_645 . ? C16 O11 Ho1 158.9(9) . 4_576 ? C23 O13 S2 123.1(8) . . ? C28 O15 C29 116.8(12) . . ? C30 O16 Ho1 90.2(8) . 3_576 ? C30 O17 Ho1 94.5(7) . 3_576 ? O10 S1 O9 119.0(6) . . ? O10 S1 O8 106.0(5) . . ? O9 S1 O8 109.7(5) . . ? O10 S1 C13 108.8(6) . . ? O9 S1 C13 110.3(5) . . ? O8 S1 C13 101.6(6) . . ? O12 S2 O14 119.8(6) . . ? O12 S2 O13 109.6(6) . . ? O14 S2 O13 102.9(5) . . ? O12 S2 C20 111.3(6) . . ? O14 S2 C20 108.5(6) . . ? O13 S2 C20 103.2(6) . . ? O5 Ho1 O11 143.5(3) . 4_575 ? O5 Ho1 O4 82.7(3) . . ? O11 Ho1 O4 96.7(3) 4_575 . ? O5 Ho1 O1 103.6(3) . . ? O11 Ho1 O1 92.5(3) 4_575 . ? O4 Ho1 O1 154.5(3) . . ? O5 Ho1 O2 145.1(3) . . ? O11 Ho1 O2 70.8(3) 4_575 . ? O4 Ho1 O2 87.6(3) . . ? O1 Ho1 O2 73.0(3) . . ? O5 Ho1 O3 73.7(3) . . ? O11 Ho1 O3 142.4(3) 4_575 . ? O4 Ho1 O3 79.7(3) . . ? O1 Ho1 O3 78.5(3) . . ? O2 Ho1 O3 71.6(3) . . ? O5 Ho1 O17 75.8(3) . 3_576 ? O11 Ho1 O17 77.2(3) 4_575 3_576 ? O4 Ho1 O17 130.5(3) . 3_576 ? O1 Ho1 O17 74.8(3) . 3_576 ? O2 Ho1 O17 132.9(3) . 3_576 ? O3 Ho1 O17 132.9(2) . 3_576 ? O5 Ho1 O16 74.1(3) . 3_576 ? O11 Ho1 O16 70.0(3) 4_575 3_576 ? O4 Ho1 O16 78.7(3) . 3_576 ? O1 Ho1 O16 126.9(3) . 3_576 ? O2 Ho1 O16 136.4(2) . 3_576 ? O3 Ho1 O16 143.1(3) . 3_576 ? O17 Ho1 O16 52.7(2) 3_576 3_576 ? O5 Ho1 C30 76.1(4) . 3_576 ? O11 Ho1 C30 68.8(3) 4_575 3_576 ? O4 Ho1 C30 105.3(3) . 3_576 ? O1 Ho1 C30 100.3(3) . 3_576 ? O2 Ho1 C30 138.7(3) . 3_576 ? O3 Ho1 C30 148.5(3) . 3_576 ? O17 Ho1 C30 26.4(3) 3_576 3_576 ? O16 Ho1 C30 26.7(3) 3_576 3_576 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.302 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.229 _database_code_depnum_ccdc_archive 'CCDC 956815' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Er O17 S2' _chemical_formula_weight 886.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.318(2) _cell_length_b 14.0046(15) _cell_length_c 9.8371(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.552(9) _cell_angle_gamma 90.00 _cell_volume 3202.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 124(2) _cell_measurement_reflns_used 1609 _cell_measurement_theta_min 2.9031 _cell_measurement_theta_max 29.1305 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5043 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 124(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13502 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_sigmaI/netI 0.2007 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5646 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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. SIMU 0.01 0.02 3.8 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 = C17 C18 C19 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 ISOR 0.01 0.001 O1 O2 O3 O9 C2 C3 C6 C7 C9 C15 C16 C25 C27 C30 ISOR 0.005 0.001 C1 C10 C23 C24 C29 ; _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^)+(0.0108P)^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 Constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5646 _refine_ls_number_parameters 455 _refine_ls_number_restraints 666 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 0.994 _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 0.2066(5) 0.5447(9) 0.8340(13) 0.024(2) Uani 1 1 d U . . C2 C 0.1889(5) 0.4447(9) 0.8273(14) 0.026(2) Uani 1 1 d U . . C3 C 0.1404(5) 0.4158(9) 0.8889(13) 0.029(2) Uani 1 1 d U . . H3 H 0.1235 0.4557 0.9498 0.035 Uiso 1 1 calc R . . C4 C 0.1170(5) 0.3242(9) 0.8576(13) 0.028(2) Uani 1 1 d U . . H4 H 0.0816 0.3068 0.8876 0.034 Uiso 1 1 calc R . . C5 C 0.1466(5) 0.2619(10) 0.7837(13) 0.030(2) Uani 1 1 d U . . C6 C 0.1969(5) 0.2905(10) 0.7316(14) 0.030(2) Uani 1 1 d U . . C7 C 0.2179(5) 0.3797(9) 0.7518(13) 0.026(2) Uani 1 1 d U . . H7 H 0.2518 0.3975 0.7150 0.031 Uiso 1 1 calc R . . C8 C 0.2637(5) 0.2613(11) 0.5592(14) 0.052(4) Uani 1 1 d U . . H8A H 0.2679 0.2195 0.4834 0.078 Uiso 1 1 calc R . . H8B H 0.2991 0.2636 0.6158 0.078 Uiso 1 1 calc R . . H8C H 0.2541 0.3243 0.5262 0.078 Uiso 1 1 calc R . . C9 C 0.0382(5) 0.1150(9) 0.8819(13) 0.0215(19) Uani 1 1 d U . . C10 C 0.0284(5) 0.1275(9) 1.0142(13) 0.024(2) Uani 1 1 d U . . H10 H 0.0580 0.1219 1.0829 0.028 Uiso 1 1 calc R . . C11 C -0.0282(5) 0.1495(9) 1.0446(12) 0.020(2) Uani 1 1 d U . . H11 H -0.0363 0.1596 1.1346 0.024 Uiso 1 1 calc R . . C12 C -0.0708(5) 0.1559(9) 0.9429(12) 0.020(2) Uani 1 1 d U . . C13 C -0.0588(5) 0.1383(9) 0.8092(13) 0.025(2) Uani 1 1 d U . . H13 H -0.0887 0.1382 0.7409 0.030 Uiso 1 1 calc R . . C14 C -0.0026(5) 0.1208(9) 0.7753(13) 0.023(2) Uani 1 1 d U . . H14 H 0.0063 0.1136 0.6854 0.028 Uiso 1 1 calc R . . C15 C -0.1324(5) 0.1824(9) 0.9721(13) 0.018(2) Uani 1 1 d U . . C16 C 0.2890(5) 0.9573(9) 0.9356(13) 0.019(2) Uani 1 1 d U . . C17 C 0.3206(5) 1.0117(9) 0.8355(13) 0.019(2) Uani 1 1 d U . . C18 C 0.3014(5) 0.9994(9) 0.7020(13) 0.0214(18) Uani 1 1 d U . . H18 H 0.2704 0.9591 0.6792 0.026 Uiso 1 1 calc R . . C19 C 0.3278(5) 1.0467(8) 0.6000(13) 0.0196(18) Uani 1 1 d U . . H19 H 0.3135 1.0411 0.5095 0.023 Uiso 1 1 calc R . . C20 C 0.3744(5) 1.1007(9) 0.6337(13) 0.022(2) Uani 1 1 d U . . C21 C 0.3964(5) 1.1129(9) 0.7693(12) 0.024(2) Uani 1 1 d U . . H21 H 0.4287 1.1509 0.7901 0.029 Uiso 1 1 calc R . . C22 C 0.3691(5) 1.0671(8) 0.8731(13) 0.021(2) Uani 1 1 d U . . H22 H 0.3829 1.0733 0.9640 0.025 Uiso 1 1 calc R . . C23 C 0.3162(5) 0.7917(9) 0.5924(12) 0.0161(18) Uani 1 1 d U . . C24 C 0.3768(5) 0.8200(9) 0.5761(12) 0.0166(18) Uani 1 1 d U . . C25 C 0.3935(5) 0.8502(8) 0.4507(12) 0.0196(19) Uani 1 1 d U . . H25 H 0.3663 0.8524 0.3763 0.024 Uiso 1 1 calc R . . C26 C 0.4495(5) 0.8769(9) 0.4340(12) 0.0190(19) Uani 1 1 d U . . C27 C 0.4888(5) 0.8717(9) 0.5443(13) 0.019(2) Uani 1 1 d U . . C28 C 0.4749(5) 0.8435(8) 0.6708(13) 0.022(2) Uani 1 1 d U . . H28 H 0.5025 0.8413 0.7443 0.026 Uiso 1 1 calc R . . C29 C 0.4176(5) 0.8180(8) 0.6860(12) 0.0175(18) Uani 1 1 d U . . H29 H 0.4069 0.7994 0.7711 0.021 Uiso 1 1 calc R . . C30 C 0.4286(5) 0.9370(10) 0.2080(13) 0.034(3) Uani 1 1 d U . . H30A H 0.4478 0.9565 0.1298 0.052 Uiso 1 1 calc R . . H30B H 0.4065 0.9893 0.2390 0.052 Uiso 1 1 calc R . . H30C H 0.4035 0.8843 0.1838 0.052 Uiso 1 1 calc R . . O1 O 0.2814(3) 0.7043(6) 0.9903(7) 0.0132(19) Uani 1 1 d U . . O2 O 0.2558(3) 0.8936(6) 0.9138(8) 0.023(2) Uani 1 1 d U . . O3 O 0.3038(3) 0.7639(6) 0.7080(7) 0.019(2) Uani 1 1 d U . . O4 O 0.1844(3) 0.8742(6) 0.6747(8) 0.025(2) Uani 1 1 d . . . H4A H 0.1734 0.8535 0.5957 0.038 Uiso 1 1 d R . . H4B H 0.1559 0.8987 0.7111 0.038 Uiso 1 1 d R . . O5 O 0.2490(3) 0.5739(6) 0.7727(8) 0.019(2) Uani 1 1 d . . . O6 O 0.1788(3) 0.6050(5) 0.9002(8) 0.016(2) Uani 1 1 d . . . O7 O 0.2171(4) 0.2253(7) 0.6399(10) 0.051(3) Uani 1 1 d . . . O8 O 0.1219(3) 0.1738(6) 0.7367(9) 0.031(2) Uani 1 1 d . . . O9 O 0.1509(3) 0.0977(7) 0.9545(9) 0.033(2) Uani 1 1 d U . . O10 O 0.1067(4) 0.0100(6) 0.7513(10) 0.046(3) Uani 1 1 d . . . O11 O -0.1696(3) 0.1854(6) 0.8700(8) 0.021(2) Uani 1 1 d . . . O12 O -0.1416(3) 0.2018(6) 1.0907(8) 0.019(2) Uani 1 1 d . . . O13 O 0.3029(3) 0.9888(6) 1.0659(8) 0.028(2) Uani 1 1 d . . . H13A H 0.2780 0.9720 1.1152 0.042 Uiso 1 1 calc R . . O14 O 0.4704(3) 0.9085(7) 0.3144(9) 0.035(3) Uani 1 1 d . . . O15 O 0.5456(3) 0.9070(6) 0.5311(8) 0.026(2) Uani 1 1 d . . . O16 O 0.6328(3) 0.8292(7) 0.6113(9) 0.038(3) Uani 1 1 d . . . O17 O 0.5671(3) 0.7478(6) 0.4418(8) 0.025(2) Uani 1 1 d . . . S1 S 0.10919(14) 0.0921(3) 0.8380(4) 0.0279(9) Uani 1 1 d . . . S2 S 0.59328(14) 0.8334(3) 0.4951(4) 0.0279(9) Uani 1 1 d . . . Er1 Er 0.22137(2) 0.74532(4) 0.81085(5) 0.01239(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 0.026(3) 0.021(3) 0.023(4) -0.002(3) 0.004(3) -0.005(3) C2 0.030(4) 0.019(4) 0.030(4) -0.002(4) 0.009(3) -0.002(4) C3 0.031(4) 0.023(4) 0.034(4) -0.005(4) 0.011(3) -0.005(4) C4 0.029(4) 0.023(4) 0.034(4) -0.002(4) 0.011(3) -0.004(4) C5 0.031(4) 0.023(4) 0.037(4) -0.004(4) 0.007(4) -0.004(4) C6 0.031(4) 0.027(4) 0.034(4) -0.006(4) 0.014(3) -0.001(4) C7 0.028(4) 0.020(4) 0.032(4) -0.002(3) 0.013(3) -0.002(3) C8 0.050(7) 0.046(8) 0.062(8) -0.015(7) 0.018(7) -0.008(7) C9 0.018(3) 0.022(4) 0.025(4) -0.001(3) 0.007(3) 0.006(3) C10 0.019(3) 0.027(4) 0.024(4) 0.002(3) 0.001(3) 0.007(3) C11 0.017(4) 0.025(4) 0.019(4) 0.001(4) 0.007(3) 0.008(4) C12 0.016(4) 0.025(4) 0.021(4) 0.000(4) 0.007(3) 0.008(4) C13 0.021(4) 0.032(4) 0.023(4) 0.000(4) 0.005(4) 0.006(4) C14 0.017(4) 0.029(4) 0.024(4) 0.001(4) 0.005(4) 0.008(4) C15 0.018(4) 0.022(4) 0.016(4) 0.000(4) 0.011(4) 0.005(4) C16 0.020(4) 0.017(4) 0.021(4) -0.007(4) 0.005(4) 0.003(4) C17 0.021(4) 0.015(4) 0.022(4) -0.003(4) 0.007(4) -0.001(4) C18 0.021(3) 0.019(3) 0.025(3) -0.004(3) 0.004(3) -0.003(3) C19 0.022(3) 0.017(3) 0.020(3) -0.003(3) 0.005(3) -0.001(3) C20 0.024(4) 0.019(4) 0.023(4) -0.002(4) 0.007(4) -0.005(4) C21 0.024(4) 0.020(4) 0.027(4) -0.004(4) 0.003(4) -0.004(4) C22 0.025(4) 0.018(4) 0.021(4) -0.002(4) 0.004(4) -0.004(4) C23 0.015(3) 0.015(3) 0.018(3) -0.001(3) 0.004(3) -0.002(3) C24 0.014(3) 0.017(3) 0.019(3) 0.001(3) 0.003(3) -0.002(3) C25 0.022(3) 0.017(3) 0.020(3) 0.001(3) 0.002(3) 0.000(3) C26 0.020(4) 0.020(4) 0.018(4) 0.002(4) 0.003(3) -0.005(4) C27 0.017(4) 0.019(4) 0.022(4) 0.004(3) 0.007(3) -0.002(3) C28 0.024(4) 0.018(4) 0.024(4) 0.002(4) 0.003(4) 0.001(4) C29 0.018(3) 0.016(3) 0.019(3) 0.003(3) 0.007(3) -0.002(3) C30 0.035(3) 0.035(3) 0.034(3) 0.0001(10) 0.0029(10) -0.0001(10) O1 0.012(4) 0.018(4) 0.009(4) 0.002(4) -0.004(3) 0.000(4) O2 0.031(5) 0.013(4) 0.028(5) 0.000(4) 0.015(4) -0.009(4) O3 0.022(4) 0.025(5) 0.011(4) 0.006(4) 0.007(3) -0.007(4) O4 0.036(5) 0.025(5) 0.016(5) 0.001(5) 0.015(5) 0.017(5) O5 0.023(5) 0.022(5) 0.012(5) -0.001(4) 0.008(4) 0.002(4) O6 0.018(4) 0.013(5) 0.019(5) 0.006(4) 0.004(4) 0.009(4) O7 0.057(7) 0.031(7) 0.068(8) -0.006(6) 0.026(6) 0.000(6) O8 0.032(5) 0.029(6) 0.033(6) -0.012(5) 0.008(5) -0.002(5) O9 0.033(2) 0.033(3) 0.034(3) -0.0005(10) 0.0021(10) 0.0002(10) O10 0.052(6) 0.020(6) 0.071(8) 0.003(6) 0.035(6) 0.007(6) O11 0.027(5) 0.026(5) 0.012(5) 0.009(4) 0.007(4) 0.002(5) O12 0.014(4) 0.029(5) 0.016(5) 0.002(4) 0.003(4) 0.005(4) O13 0.034(6) 0.031(6) 0.020(6) -0.003(5) 0.013(5) -0.006(5) O14 0.031(5) 0.053(7) 0.021(6) 0.008(5) -0.002(5) -0.006(5) O15 0.013(4) 0.027(6) 0.040(6) -0.006(5) 0.006(4) -0.012(4) O16 0.031(6) 0.048(7) 0.034(6) 0.021(6) 0.005(5) 0.008(5) O17 0.031(5) 0.015(5) 0.029(5) 0.005(5) 0.011(4) -0.012(5) S1 0.0255(19) 0.021(2) 0.039(2) -0.0046(19) 0.0124(18) -0.0045(18) S2 0.026(2) 0.028(2) 0.030(2) 0.0107(19) 0.0035(18) -0.0012(19) Er1 0.0120(3) 0.0145(3) 0.0112(3) -0.0001(3) 0.0047(2) 0.0002(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 C1 O5 1.266(12) . ? C1 O6 1.274(13) . ? C1 C2 1.460(16) . ? C1 Er1 2.842(13) . ? C2 C7 1.384(15) . ? C2 C3 1.386(14) . ? C3 C4 1.419(16) . ? C3 H3 0.9300 . ? C4 C5 1.358(15) . ? C4 H4 0.9300 . ? C5 C6 1.378(14) . ? C5 O8 1.423(15) . ? C6 C7 1.350(17) . ? C6 O7 1.392(14) . ? C7 H7 0.9300 . ? C8 O7 1.483(12) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.350(14) . ? C9 C14 1.361(17) . ? C9 S1 1.773(10) . ? C10 C11 1.410(13) . ? C10 H10 0.9300 . ? C11 C12 1.355(17) . ? C11 H11 0.9300 . ? C12 C13 1.388(14) . ? C12 C15 1.534(14) . ? C13 C14 1.399(13) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O12 1.233(12) . ? C15 O11 1.274(14) . ? C16 O2 1.189(13) . ? C16 O13 1.370(14) . ? C16 C17 1.486(15) . ? C17 C18 1.365(16) . ? C17 C22 1.397(16) . ? C18 C19 1.387(14) . ? C18 H18 0.9300 . ? C19 C20 1.343(16) . ? C19 H19 0.9300 . ? C20 C21 1.401(17) . ? C20 S2 1.782(11) 3_676 ? C21 C22 1.401(14) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O1 1.242(14) 4_575 ? C23 O3 1.258(12) . ? C23 C24 1.488(14) . ? C24 C29 1.381(17) . ? C24 C25 1.388(14) . ? C25 C26 1.382(14) . ? C25 H25 0.9300 . ? C26 C27 1.367(17) . ? C26 O14 1.380(12) . ? C27 C28 1.369(14) . ? C27 O15 1.429(12) . ? C28 C29 1.402(14) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O14 1.428(15) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? O1 C23 1.242(14) 4_576 ? O1 Er1 2.239(8) . ? O2 Er1 2.419(8) . ? O3 Er1 2.258(6) . ? O4 Er1 2.369(8) . ? O4 H4A 0.8499 . ? O4 H4B 0.8504 . ? O5 Er1 2.521(8) . ? O6 Er1 2.400(7) . ? O8 S1 1.562(9) . ? O9 S1 1.445(9) . ? O10 S1 1.430(10) . ? O11 Er1 2.234(8) 2_546 ? O12 Er1 2.288(6) 3_567 ? O13 H13A 0.8200 . ? O15 S2 1.577(8) . ? O16 S2 1.411(10) . ? O17 S2 1.426(9) . ? S2 C20 1.782(12) 3_676 ? Er1 O11 2.234(8) 2_556 ? Er1 O12 2.288(6) 3_567 ? 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 O5 C1 O6 118.5(11) . . ? O5 C1 C2 121.1(11) . . ? O6 C1 C2 120.4(10) . . ? O5 C1 Er1 62.5(6) . . ? O6 C1 Er1 57.0(6) . . ? C2 C1 Er1 168.6(11) . . ? C7 C2 C3 119.5(12) . . ? C7 C2 C1 120.5(10) . . ? C3 C2 C1 119.9(11) . . ? C2 C3 C4 118.9(11) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.6(11) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 119.8(13) . . ? C4 C5 O8 121.4(10) . . ? C6 C5 O8 117.8(11) . . ? C7 C6 C5 121.5(12) . . ? C7 C6 O7 124.5(10) . . ? C5 C6 O7 113.1(12) . . ? C6 C7 C2 120.1(11) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O7 C8 H8A 109.5 . . ? O7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 124.9(11) . . ? C10 C9 S1 119.4(10) . . ? C14 C9 S1 115.6(9) . . ? C9 C10 C11 117.8(12) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? C12 C11 C10 120.0(11) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 119.8(10) . . ? C11 C12 C15 121.3(10) . . ? C13 C12 C15 118.9(11) . . ? C12 C13 C14 121.3(12) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C9 C14 C13 115.9(11) . . ? C9 C14 H14 122.0 . . ? C13 C14 H14 122.0 . . ? O12 C15 O11 125.6(10) . . ? O12 C15 C12 117.8(11) . . ? O11 C15 C12 116.6(10) . . ? O2 C16 O13 120.9(11) . . ? O2 C16 C17 128.0(12) . . ? O13 C16 C17 111.1(11) . . ? C18 C17 C22 121.4(11) . . ? C18 C17 C16 115.5(12) . . ? C22 C17 C16 122.9(12) . . ? C17 C18 C19 120.3(12) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.2(12) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 122.1(11) . . ? C19 C20 S2 119.7(10) . 3_676 ? C21 C20 S2 118.0(10) . 3_676 ? C22 C21 C20 118.9(12) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C17 C22 C21 117.9(12) . . ? C17 C22 H22 121.1 . . ? C21 C22 H22 121.1 . . ? O1 C23 O3 124.2(10) 4_575 . ? O1 C23 C24 117.8(10) 4_575 . ? O3 C23 C24 117.9(11) . . ? C29 C24 C25 118.6(10) . . ? C29 C24 C23 120.7(10) . . ? C25 C24 C23 120.7(11) . . ? C26 C25 C24 121.4(12) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C27 C26 O14 115.7(10) . . ? C27 C26 C25 118.2(11) . . ? O14 C26 C25 126.1(12) . . ? C26 C27 C28 123.0(11) . . ? C26 C27 O15 118.5(10) . . ? C28 C27 O15 118.2(11) . . ? C27 C28 C29 117.9(12) . . ? C27 C28 H28 121.1 . . ? C29 C28 H28 121.1 . . ? C24 C29 C28 120.9(11) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? O14 C30 H30A 109.5 . . ? O14 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O14 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 O1 Er1 162.6(9) 4_576 . ? C16 O2 Er1 155.4(7) . . ? C23 O3 Er1 134.9(7) . . ? Er1 O4 H4A 109.0 . . ? Er1 O4 H4B 109.3 . . ? H4A O4 H4B 109.5 . . ? C1 O5 Er1 91.1(7) . . ? C1 O6 Er1 96.5(7) . . ? C6 O7 C8 115.0(10) . . ? C5 O8 S1 121.3(8) . . ? C15 O11 Er1 158.6(9) . 2_546 ? C15 O12 Er1 132.8(8) . 3_567 ? C16 O13 H13A 109.5 . . ? C26 O14 C30 116.6(9) . . ? C27 O15 S2 117.9(8) . . ? O10 S1 O9 120.7(6) . . ? O10 S1 O8 102.1(5) . . ? O9 S1 O8 108.5(5) . . ? O10 S1 C9 107.2(6) . . ? O9 S1 C9 112.3(6) . . ? O8 S1 C9 104.5(5) . . ? O16 S2 O17 119.7(6) . . ? O16 S2 O15 105.8(5) . . ? O17 S2 O15 110.1(5) . . ? O16 S2 C20 108.2(6) . 3_676 ? O17 S2 C20 111.5(5) . 3_676 ? O15 S2 C20 99.6(5) . 3_676 ? O11 Er1 O1 142.8(3) 2_556 . ? O11 Er1 O3 96.5(3) 2_556 . ? O1 Er1 O3 83.2(3) . . ? O11 Er1 O12 93.0(3) 2_556 3_567 ? O1 Er1 O12 103.2(3) . 3_567 ? O3 Er1 O12 154.5(3) . 3_567 ? O11 Er1 O4 71.7(3) 2_556 . ? O1 Er1 O4 144.9(3) . . ? O3 Er1 O4 86.8(3) . . ? O12 Er1 O4 73.8(3) 3_567 . ? O11 Er1 O6 76.7(3) 2_556 . ? O1 Er1 O6 75.6(3) . . ? O3 Er1 O6 130.5(3) . . ? O12 Er1 O6 74.7(3) 3_567 . ? O4 Er1 O6 133.5(3) . . ? O11 Er1 O2 142.8(3) 2_556 . ? O1 Er1 O2 74.0(3) . . ? O3 Er1 O2 79.8(3) . . ? O12 Er1 O2 78.4(3) 3_567 . ? O4 Er1 O2 71.1(3) . . ? O6 Er1 O2 133.1(3) . . ? O11 Er1 O5 69.6(3) 2_556 . ? O1 Er1 O5 73.9(3) . . ? O3 Er1 O5 78.8(3) . . ? O12 Er1 O5 126.6(3) 3_567 . ? O4 Er1 O5 136.7(3) . . ? O6 Er1 O5 52.6(2) . . ? O2 Er1 O5 143.1(3) . . ? O11 Er1 C1 68.3(4) 2_556 . ? O1 Er1 C1 75.8(3) . . ? O3 Er1 C1 105.2(3) . . ? O12 Er1 C1 100.2(3) 3_567 . ? O4 Er1 C1 139.3(3) . . ? O6 Er1 C1 26.4(2) . . ? O2 Er1 C1 148.6(3) . . ? O5 Er1 C1 26.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.757 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.244 _database_code_depnum_ccdc_archive 'CCDC 956816'