# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # 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-Eu #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H27 Eu N0 O8 S2' _chemical_formula_weight 743.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.232(13) _cell_length_b 10.346(4) _cell_length_c 27.852(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.872(7) _cell_angle_gamma 90.00 _cell_volume 9164(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11384 _cell_measurement_theta_min 2.8641 _cell_measurement_theta_max 27.5204 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.4500 _exptl_crystal_size_min 0.3000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6167 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49132 _diffrn_reflns_av_R_equivalents 0.1496 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10465 _reflns_number_gt 6982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+100.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10465 _refine_ls_number_parameters 424 _refine_ls_number_restraints 405 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1836 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.212 _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 Eu1 Eu 0.555472(12) 0.10532(4) 0.009071(15) 0.03233(13) Uani 1 1 d . . . O1 O 0.1208(2) 0.6450(8) 0.0781(3) 0.072(2) Uani 1 1 d . . . O2 O 0.1259(2) 0.4928(10) 0.0265(3) 0.086(3) Uani 1 1 d . . . O3 O 0.4430(2) 0.9453(6) 0.4302(2) 0.0537(17) Uani 1 1 d . . . O4 O 0.49635(19) 0.8042(6) 0.4484(2) 0.0520(17) Uani 1 1 d . . . O5 O 0.4759(2) 0.0771(7) 0.0363(2) 0.0521(17) Uani 1 1 d . . . O6 O 0.5258(2) 0.2223(7) 0.0652(2) 0.0525(16) Uani 1 1 d . . . C1 C 0.1411(3) 0.5617(12) 0.0635(4) 0.061(3) Uani 1 1 d . . . C2 C 0.18621(16) 0.5389(10) 0.0941(3) 0.092(4) Uani 1 1 d GU . . C3 C 0.2072(2) 0.6384(8) 0.1249(4) 0.124(4) Uani 1 1 d GU . . H3A H 0.1928 0.7132 0.1284 0.149 Uiso 1 1 calc R . . C4 C 0.2497(2) 0.6263(8) 0.1503(3) 0.120(4) Uani 1 1 d GU . . H4A H 0.2637 0.6929 0.1708 0.144 Uiso 1 1 calc R . . C5 C 0.27124(16) 0.5146(9) 0.1449(3) 0.079(3) Uani 1 1 d GU . . C6 C 0.2503(2) 0.4151(8) 0.1142(4) 0.119(4) Uani 1 1 d GU . . H6A H 0.2647 0.3403 0.1106 0.143 Uiso 1 1 calc R . . C7 C 0.2078(2) 0.4272(8) 0.0888(4) 0.124(4) Uani 1 1 d GU . . H7A H 0.1937 0.3606 0.0683 0.149 Uiso 1 1 calc R . . C8 C 0.3185(3) 0.5112(12) 0.1700(3) 0.061(3) Uani 1 1 d . . . C9 C 0.3378(3) 0.5734(11) 0.2155(4) 0.066(3) Uani 1 1 d . . . H9A H 0.3215 0.6229 0.2307 0.079 Uiso 1 1 calc R . . C10 C 0.3813(3) 0.5625(11) 0.2388(3) 0.053(2) Uani 1 1 d . . . C11 C 0.4053(3) 0.5007(10) 0.2137(4) 0.055(3) Uani 1 1 d . . . H11A H 0.4344 0.5012 0.2277 0.066 Uiso 1 1 calc R . . C12 C 0.3885(3) 0.4362(10) 0.1676(3) 0.049(2) Uani 1 1 d . . . C13 C 0.3441(3) 0.4410(11) 0.1467(3) 0.058(3) Uani 1 1 d . . . H13A H 0.3317 0.3969 0.1170 0.069 Uiso 1 1 calc R . . C14 C 0.4008(3) 0.6369(11) 0.2863(3) 0.054(3) Uani 1 1 d . . . C15 C 0.3822(3) 0.7416(12) 0.2991(4) 0.074(4) Uani 1 1 d . . . H15A H 0.3565 0.7692 0.2780 0.089 Uiso 1 1 calc R . . C16 C 0.4009(3) 0.8112(12) 0.3439(4) 0.076(4) Uani 1 1 d . . . H16A H 0.3873 0.8825 0.3524 0.091 Uiso 1 1 calc R . . C17 C 0.4395(3) 0.7718(9) 0.3749(3) 0.045(2) Uani 1 1 d . . . C18 C 0.4584(3) 0.6653(10) 0.3618(4) 0.054(3) Uani 1 1 d . . . H18A H 0.4846 0.6392 0.3822 0.065 Uiso 1 1 calc R . . C19 C 0.4390(3) 0.5952(10) 0.3182(3) 0.053(3) Uani 1 1 d . . . H19A H 0.4516 0.5207 0.3106 0.063 Uiso 1 1 calc R . . C20 C 0.4618(3) 0.8466(9) 0.4215(3) 0.044(2) Uani 1 1 d . . . C21 C 0.4151(3) 0.3668(10) 0.1420(3) 0.049(2) Uani 1 1 d . . . C22 C 0.4542(3) 0.4115(10) 0.1438(4) 0.058(3) Uani 1 1 d . . . H22A H 0.4643 0.4861 0.1619 0.070 Uiso 1 1 calc R . . C23 C 0.4785(3) 0.3485(11) 0.1195(4) 0.061(3) Uani 1 1 d . . . H23A H 0.5052 0.3802 0.1218 0.073 Uiso 1 1 calc R . . C24 C 0.4643(3) 0.2378(9) 0.0912(3) 0.045(2) Uani 1 1 d . . . C25 C 0.4253(3) 0.1933(11) 0.0900(4) 0.063(3) Uani 1 1 d . . . H25A H 0.4152 0.1185 0.0721 0.076 Uiso 1 1 calc R . . C26 C 0.4002(3) 0.2585(11) 0.1152(4) 0.060(3) Uani 1 1 d . . . H26A H 0.3736 0.2275 0.1135 0.072 Uiso 1 1 calc R . . C27 C 0.4913(3) 0.1746(9) 0.0630(3) 0.043(2) Uani 1 1 d . . . O7 O 0.5755(3) 0.3300(8) 0.0041(3) 0.087(2) Uani 1 1 d DU . . O8 O 0.5804(3) 0.1254(9) -0.0635(3) 0.101(3) Uani 1 1 d DU . . S1 S 0.5718(3) 0.4468(6) 0.0344(3) 0.115(3) Uani 0.619(8) 1 d PDU A 1 C28 C 0.6042(8) 0.576(2) 0.0250(12) 0.149(8) Uani 0.619(8) 1 d PDU A 1 H28A H 0.6332 0.5520 0.0385 0.223 Uiso 0.619(8) 1 calc PR A 1 H28B H 0.5986 0.6517 0.0418 0.223 Uiso 0.619(8) 1 calc PR A 1 H28C H 0.5982 0.5928 -0.0102 0.223 Uiso 0.619(8) 1 calc PR A 1 C29 C 0.5191(5) 0.497(3) 0.0062(11) 0.127(6) Uani 0.619(8) 1 d PDU . 1 H29A H 0.5283 0.4212 0.0261 0.190 Uiso 0.619(8) 1 calc PR A 1 H29B H 0.5305 0.5725 0.0256 0.190 Uiso 0.619(8) 1 calc PR A 1 H29C H 0.5286 0.4941 -0.0231 0.190 Uiso 0.619(8) 1 calc PR A 1 S1B S 0.6129(4) 0.4073(14) 0.0312(6) 0.152(4) Uani 0.381(8) 1 d PDU A 2 C28B C 0.6157(15) 0.460(4) 0.0926(9) 0.127(9) Uani 0.381(8) 1 d PDU A 2 H28D H 0.6198 0.3865 0.1147 0.191 Uiso 0.381(8) 1 calc PR A 2 H28E H 0.5900 0.5028 0.0922 0.191 Uiso 0.381(8) 1 calc PR A 2 H28F H 0.6389 0.5185 0.1043 0.191 Uiso 0.381(8) 1 calc PR A 2 C29B C 0.6000(17) 0.544(3) -0.0087(12) 0.146(9) Uani 0.381(8) 1 d PDU A 2 H29D H 0.5983 0.5186 -0.0424 0.220 Uiso 0.381(8) 1 calc PR A 2 H29E H 0.6213 0.6087 0.0025 0.220 Uiso 0.381(8) 1 calc PR A 2 H29F H 0.5734 0.5778 -0.0078 0.220 Uiso 0.381(8) 1 calc PR A 2 S2 S 0.5695(6) 0.2016(16) -0.1111(5) 0.148(4) Uani 0.483(12) 1 d PDU A 1 C30 C 0.6254(10) 0.167(4) -0.1200(15) 0.144(9) Uani 0.483(12) 1 d PDU A 1 H30A H 0.6469 0.1997 -0.0916 0.216 Uiso 0.483(12) 1 calc PR A 1 H30B H 0.6275 0.2093 -0.1499 0.216 Uiso 0.483(12) 1 calc PR A 1 H30C H 0.6291 0.0757 -0.1229 0.216 Uiso 0.483(12) 1 calc PR A 1 C31 C 0.5378(12) 0.122(4) -0.1628(15) 0.169(10) Uani 0.483(12) 1 d PDU A 1 H31A H 0.5090 0.1282 -0.1627 0.253 Uiso 0.483(12) 1 calc PR A 1 H31B H 0.5459 0.0324 -0.1615 0.253 Uiso 0.483(12) 1 calc PR A 1 H31C H 0.5410 0.1604 -0.1928 0.253 Uiso 0.483(12) 1 calc PR A 1 S2B S 0.5922(5) 0.2375(10) -0.0905(5) 0.130(3) Uani 0.517(12) 1 d PDU A 2 C30B C 0.5902(11) 0.170(3) -0.1499(8) 0.133(8) Uani 0.517(12) 1 d PDU A 2 H30D H 0.5621 0.1413 -0.1663 0.200 Uiso 0.517(12) 1 calc PR A 2 H30E H 0.6092 0.0983 -0.1453 0.200 Uiso 0.517(12) 1 calc PR A 2 H30F H 0.5982 0.2347 -0.1702 0.200 Uiso 0.517(12) 1 calc PR A 2 C31B C 0.6452(7) 0.285(4) -0.0623(12) 0.156(8) Uani 0.517(12) 1 d PDU A 2 H31D H 0.6475 0.3256 -0.0307 0.234 Uiso 0.517(12) 1 calc PR A 2 H31E H 0.6537 0.3441 -0.0839 0.234 Uiso 0.517(12) 1 calc PR A 2 H31F H 0.6630 0.2097 -0.0570 0.234 Uiso 0.517(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02417(19) 0.0390(2) 0.0327(2) 0.00065(16) 0.00659(15) 0.00234(17) O1 0.035(4) 0.086(6) 0.080(5) -0.014(4) -0.007(4) 0.005(4) O2 0.032(4) 0.155(9) 0.065(5) -0.032(5) 0.004(3) 0.010(5) O3 0.048(4) 0.056(4) 0.048(4) -0.022(3) 0.000(3) 0.006(3) O4 0.046(4) 0.054(4) 0.043(3) -0.014(3) -0.008(3) -0.003(3) O5 0.059(4) 0.056(4) 0.045(3) -0.015(3) 0.021(3) -0.001(3) O6 0.052(4) 0.058(4) 0.054(4) -0.013(3) 0.024(3) 0.001(3) C1 0.021(4) 0.087(8) 0.068(7) -0.008(6) 0.003(4) -0.002(5) C2 0.033(5) 0.130(8) 0.097(7) -0.057(6) -0.004(5) 0.025(5) C3 0.059(6) 0.155(9) 0.124(8) -0.078(7) -0.029(6) 0.026(7) C4 0.054(6) 0.160(9) 0.118(8) -0.067(7) -0.017(6) 0.018(7) C5 0.037(4) 0.114(8) 0.072(6) -0.067(5) -0.006(4) 0.015(5) C6 0.046(6) 0.157(9) 0.128(8) -0.069(7) -0.017(6) 0.030(6) C7 0.050(6) 0.160(9) 0.132(8) -0.071(7) -0.021(6) 0.026(6) C8 0.028(4) 0.102(9) 0.049(5) -0.036(6) 0.004(4) 0.000(5) C9 0.034(5) 0.095(8) 0.057(6) -0.045(6) -0.008(4) 0.013(5) C10 0.036(5) 0.071(7) 0.046(5) -0.017(5) 0.003(4) 0.004(5) C11 0.030(4) 0.067(7) 0.057(6) -0.023(5) -0.003(4) 0.011(4) C12 0.034(4) 0.064(6) 0.051(5) -0.016(5) 0.013(4) 0.007(4) C13 0.030(4) 0.091(8) 0.046(5) -0.033(5) 0.001(4) -0.001(5) C14 0.032(4) 0.080(7) 0.046(5) -0.028(5) 0.002(4) 0.006(5) C15 0.047(6) 0.101(10) 0.053(6) -0.028(6) -0.019(5) 0.023(6) C16 0.060(6) 0.082(8) 0.064(6) -0.043(6) -0.016(5) 0.022(6) C17 0.032(4) 0.053(6) 0.043(5) -0.019(4) 0.000(4) -0.003(4) C18 0.044(5) 0.063(7) 0.051(5) -0.012(5) 0.006(4) 0.011(5) C19 0.039(5) 0.069(7) 0.043(5) -0.023(5) 0.000(4) 0.009(5) C20 0.033(4) 0.055(6) 0.038(4) -0.008(4) 0.002(4) 0.001(4) C21 0.043(5) 0.058(6) 0.045(5) -0.018(4) 0.013(4) 0.005(4) C22 0.036(5) 0.070(7) 0.069(7) -0.037(5) 0.016(5) 0.000(5) C23 0.044(5) 0.076(8) 0.066(6) -0.030(6) 0.021(5) -0.010(5) C24 0.039(5) 0.052(6) 0.041(5) -0.013(4) 0.005(4) 0.004(4) C25 0.053(6) 0.065(7) 0.082(7) -0.042(6) 0.034(5) -0.018(5) C26 0.038(5) 0.074(7) 0.076(7) -0.025(6) 0.028(5) -0.004(5) C27 0.045(5) 0.045(5) 0.044(5) 0.002(4) 0.019(4) 0.007(4) O7 0.093(5) 0.063(5) 0.114(6) 0.005(4) 0.044(5) -0.007(4) O8 0.140(7) 0.096(6) 0.102(6) 0.027(5) 0.091(5) 0.007(5) S1 0.126(6) 0.064(4) 0.142(6) -0.005(4) 0.017(5) -0.002(4) C28 0.159(15) 0.108(14) 0.173(16) 0.004(14) 0.038(15) -0.012(14) C29 0.134(10) 0.092(9) 0.148(10) -0.006(9) 0.031(10) -0.003(10) S1B 0.158(8) 0.118(8) 0.178(8) -0.004(7) 0.044(8) -0.006(7) C28B 0.149(16) 0.093(15) 0.138(16) -0.018(15) 0.038(15) -0.002(15) C29B 0.158(15) 0.114(15) 0.149(16) -0.003(15) 0.016(15) -0.005(15) S2 0.169(9) 0.138(8) 0.149(8) 0.025(7) 0.064(7) 0.010(7) C30 0.154(16) 0.151(16) 0.153(16) 0.007(15) 0.086(14) 0.016(15) C31 0.195(18) 0.159(18) 0.151(17) 0.002(16) 0.048(17) 0.013(17) S2B 0.165(8) 0.123(7) 0.124(7) 0.028(6) 0.077(6) -0.014(6) C30B 0.172(16) 0.143(15) 0.116(14) 0.002(14) 0.090(13) 0.011(15) C31B 0.162(14) 0.139(14) 0.178(14) 0.011(13) 0.067(13) 0.002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O5 2.340(6) 5_655 ? Eu1 O3 2.357(6) 2_645 ? Eu1 O4 2.379(5) 6_565 ? Eu1 O6 2.404(6) . ? Eu1 O8 2.406(7) . ? Eu1 O7 2.434(8) . ? Eu1 O1 2.481(6) 3_545 ? Eu1 O2 2.530(7) 3_545 ? Eu1 C1 2.844(9) 3_545 ? Eu1 O5 2.970(7) . ? Eu1 C27 3.029(9) . ? O1 C1 1.234(12) . ? O1 Eu1 2.481(6) 3_455 ? O2 C1 1.234(12) . ? O2 Eu1 2.530(7) 3_455 ? O3 C20 1.255(10) . ? O3 Eu1 2.357(6) 2_665 ? O4 C20 1.254(10) . ? O4 Eu1 2.379(5) 6_566 ? O5 C27 1.271(11) . ? O5 Eu1 2.340(6) 5_655 ? O6 C27 1.231(10) . ? C1 C2 1.514(10) . ? C1 Eu1 2.844(9) 3_455 ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 C8 1.523(9) . ? C6 C7 1.3900 . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.400(11) . ? C8 C13 1.413(12) . ? C9 C10 1.405(12) . ? C9 H9A 0.9300 . ? C10 C11 1.364(12) . ? C10 C14 1.505(12) . ? C11 C12 1.410(12) . ? C11 H11A 0.9300 . ? C12 C13 1.421(11) . ? C12 C21 1.472(12) . ? C13 H13A 0.9300 . ? C14 C15 1.345(14) . ? C14 C19 1.391(12) . ? C15 C16 1.419(12) . ? C15 H15A 0.9300 . ? C16 C17 1.384(12) . ? C16 H16A 0.9300 . ? C17 C18 1.370(12) . ? C17 C20 1.508(11) . ? C18 C19 1.402(12) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.365(13) . ? C21 C26 1.359(13) . ? C22 C23 1.362(12) . ? C22 H22A 0.9300 . ? C23 C24 1.392(12) . ? C23 H23A 0.9300 . ? C24 C25 1.364(12) . ? C24 C27 1.504(12) . ? C25 C26 1.410(12) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? O7 S1B 1.485(9) . ? O7 S1 1.500(8) . ? O8 S2 1.493(9) . ? O8 S2B 1.496(8) . ? S1 C29 1.779(13) . ? S1 C28 1.778(14) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C29 1.21(3) 5_665 ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? S1B C28B 1.770(14) . ? S1B C29B 1.771(14) . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? S2 C31 1.73(4) . ? S2 C30 1.98(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? S2B C31B 1.776(14) . ? S2B C30B 1.777(14) . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? 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 Eu1 O3 74.6(2) 5_655 2_645 ? O5 Eu1 O4 77.7(2) 5_655 6_565 ? O3 Eu1 O4 128.8(2) 2_645 6_565 ? O5 Eu1 O6 123.7(2) 5_655 . ? O3 Eu1 O6 79.3(2) 2_645 . ? O4 Eu1 O6 81.6(2) 6_565 . ? O5 Eu1 O8 79.9(3) 5_655 . ? O3 Eu1 O8 136.3(3) 2_645 . ? O4 Eu1 O8 77.6(3) 6_565 . ? O6 Eu1 O8 144.1(3) . . ? O5 Eu1 O7 145.7(3) 5_655 . ? O3 Eu1 O7 139.7(3) 2_645 . ? O4 Eu1 O7 76.5(3) 6_565 . ? O6 Eu1 O7 74.2(3) . . ? O8 Eu1 O7 72.7(3) . . ? O5 Eu1 O1 134.7(3) 5_655 3_545 ? O3 Eu1 O1 74.2(3) 2_645 3_545 ? O4 Eu1 O1 147.3(3) 6_565 3_545 ? O6 Eu1 O1 81.1(2) . 3_545 ? O8 Eu1 O1 101.5(3) . 3_545 ? O7 Eu1 O1 72.2(3) . 3_545 ? O5 Eu1 O2 88.5(3) 5_655 3_545 ? O3 Eu1 O2 73.4(3) 2_645 3_545 ? O4 Eu1 O2 147.5(2) 6_565 3_545 ? O6 Eu1 O2 129.7(2) . 3_545 ? O8 Eu1 O2 71.1(3) . 3_545 ? O7 Eu1 O2 101.3(3) . 3_545 ? O1 Eu1 O2 51.3(3) 3_545 3_545 ? O5 Eu1 C1 112.3(3) 5_655 3_545 ? O3 Eu1 C1 72.3(3) 2_645 3_545 ? O4 Eu1 C1 158.9(3) 6_565 3_545 ? O6 Eu1 C1 105.6(3) . 3_545 ? O8 Eu1 C1 85.8(3) . 3_545 ? O7 Eu1 C1 86.2(3) . 3_545 ? O1 Eu1 C1 25.6(3) 3_545 3_545 ? O2 Eu1 C1 25.7(3) 3_545 3_545 ? O5 Eu1 O5 76.6(2) 5_655 . ? O3 Eu1 O5 65.3(2) 2_645 . ? O4 Eu1 O5 66.8(2) 6_565 . ? O6 Eu1 O5 47.1(2) . . ? O8 Eu1 O5 140.6(3) . . ? O7 Eu1 O5 112.8(2) . . ? O1 Eu1 O5 117.5(2) 3_545 . ? O2 Eu1 O5 138.4(3) 3_545 . ? C1 Eu1 O5 132.5(3) 3_545 . ? O5 Eu1 C27 101.0(2) 5_655 . ? O3 Eu1 C27 71.4(2) 2_645 . ? O4 Eu1 C27 72.8(2) 6_565 . ? O6 Eu1 C27 22.7(2) . . ? O8 Eu1 C27 149.3(3) . . ? O7 Eu1 C27 92.7(3) . . ? O1 Eu1 C27 99.2(3) 3_545 . ? O2 Eu1 C27 139.3(3) 3_545 . ? C1 Eu1 C27 120.8(3) 3_545 . ? O5 Eu1 C27 24.4(2) . . ? O5 Eu1 Eu1 43.66(16) 5_655 5_655 ? O3 Eu1 Eu1 63.60(15) 2_645 5_655 ? O4 Eu1 Eu1 66.55(16) 6_565 5_655 ? O6 Eu1 Eu1 80.03(16) . 5_655 ? O8 Eu1 Eu1 116.7(3) . 5_655 ? O7 Eu1 Eu1 137.5(2) . 5_655 ? O1 Eu1 Eu1 136.2(2) 3_545 5_655 ? O2 Eu1 Eu1 121.1(2) 3_545 5_655 ? C1 Eu1 Eu1 133.7(2) 3_545 5_655 ? O5 Eu1 Eu1 32.96(12) . 5_655 ? C27 Eu1 Eu1 57.39(18) . 5_655 ? C1 O1 Eu1 93.9(6) . 3_455 ? C1 O2 Eu1 91.5(6) . 3_455 ? C20 O3 Eu1 143.2(5) . 2_665 ? C20 O4 Eu1 135.3(6) . 6_566 ? C27 O5 Eu1 175.9(6) . 5_655 ? C27 O5 Eu1 80.4(5) . . ? Eu1 O5 Eu1 103.4(2) 5_655 . ? C27 O6 Eu1 108.5(6) . . ? O1 C1 O2 123.2(9) . . ? O1 C1 C2 118.0(9) . . ? O2 C1 C2 118.7(10) . . ? O1 C1 Eu1 60.5(5) . 3_455 ? O2 C1 Eu1 62.8(5) . 3_455 ? C2 C1 Eu1 178.0(8) . 3_455 ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.0(7) . . ? C7 C2 C1 121.7(7) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 C8 122.1(6) . . ? C4 C5 C8 117.7(7) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C9 C8 C13 118.2(8) . . ? C9 C8 C5 123.0(8) . . ? C13 C8 C5 118.7(7) . . ? C8 C9 C10 121.3(9) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 118.6(8) . . ? C11 C10 C14 121.5(8) . . ? C9 C10 C14 119.1(8) . . ? C10 C11 C12 123.4(8) . . ? C10 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 116.5(8) . . ? C11 C12 C21 122.5(8) . . ? C13 C12 C21 121.0(8) . . ? C8 C13 C12 121.5(8) . . ? C8 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C15 C14 C19 118.9(8) . . ? C15 C14 C10 122.1(8) . . ? C19 C14 C10 119.0(9) . . ? C14 C15 C16 121.7(9) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C17 C16 C15 119.3(9) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C18 C17 C16 119.0(8) . . ? C18 C17 C20 119.6(8) . . ? C16 C17 C20 121.4(8) . . ? C17 C18 C19 121.0(9) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C14 120.0(9) . . ? C18 C19 H19A 120.0 . . ? C14 C19 H19A 120.0 . . ? O3 C20 O4 126.1(8) . . ? O3 C20 C17 115.8(7) . . ? O4 C20 C17 118.0(8) . . ? C22 C21 C26 119.3(9) . . ? C22 C21 C12 121.0(9) . . ? C26 C21 C12 119.7(9) . . ? C21 C22 C23 121.0(9) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C22 C23 C24 121.5(9) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C25 C24 C23 117.1(9) . . ? C25 C24 C27 123.1(8) . . ? C23 C24 C27 119.8(9) . . ? C24 C25 C26 121.4(9) . . ? C24 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? C21 C26 C25 119.7(9) . . ? C21 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? O6 C27 O5 124.0(8) . . ? O6 C27 C24 119.2(8) . . ? O5 C27 C24 116.7(8) . . ? O6 C27 Eu1 48.8(4) . . ? O5 C27 Eu1 75.2(5) . . ? C24 C27 Eu1 167.2(7) . . ? S1B O7 S1 58.1(7) . . ? S1B O7 Eu1 133.4(8) . . ? S1 O7 Eu1 132.0(6) . . ? S2 O8 S2B 34.4(7) . . ? S2 O8 Eu1 137.5(8) . . ? S2B O8 Eu1 133.9(7) . . ? O7 S1 C29 102.7(12) . . ? O7 S1 C28 111.7(12) . . ? C29 S1 C28 106.0(11) . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 C29 S1 162(4) 5_665 . ? C29 C29 H29A 109.5 5_665 . ? S1 C29 H29A 52.9 . . ? C29 C29 H29B 109.5 5_665 . ? S1 C29 H29B 79.2 . . ? H29A C29 H29B 109.5 . . ? C29 C29 H29C 109.5 5_665 . ? S1 C29 H29C 80.7 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 S1B C28B 117.4(19) . . ? O7 S1B C29B 95.5(19) . . ? C28B S1B C29B 107.3(12) . . ? S1B C28B H28D 109.5 . . ? S1B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? S1B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? S1B C29B H29D 109.5 . . ? S1B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? S1B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? O8 S2 C31 114.7(19) . . ? O8 S2 C30 91.3(14) . . ? C31 S2 C30 100.2(17) . . ? S2 C30 H30A 109.5 . . ? S2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? S2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? S2 C31 H31A 109.5 . . ? S2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O8 S2B C31B 111.1(16) . . ? O8 S2B C30B 102.7(14) . . ? C31B S2B C30B 106.5(11) . . ? S2B C30B H30D 109.5 . . ? S2B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? S2B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? S2B C31B H31D 109.5 . . ? S2B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? S2B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.754 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.177 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.198 0.211 -0.001 3535.7 172.8 2 0.000 0.158 0.250 15.1 3.3 3 0.500 0.658 0.250 15.1 3.3 4 0.000 0.842 0.750 15.1 2.4 5 0.500 0.342 0.750 15.1 2.4 _platon_squeeze_details ; ? ; _database_code_depnum_ccdc_archive 'CCDC 930171' ####################################################################### # # 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-Gd #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H27 Gd O8 S2' _chemical_formula_sum 'C31 H27 Gd N0 O8 S2' _chemical_formula_weight 748.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.226(7) _cell_length_b 10.372(2) _cell_length_c 27.776(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.061(4) _cell_angle_gamma 90.00 _cell_volume 9151(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11109 _cell_measurement_theta_min 3.0019 _cell_measurement_theta_max 27.4758 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 1.573 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8118 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34389 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10336 _reflns_number_gt 8742 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+60.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10336 _refine_ls_number_parameters 423 _refine_ls_number_restraints 399 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.555626(5) 0.105065(18) 0.009306(7) 0.02999(6) Uani 1 1 d . . . O1 O 0.12027(10) 0.6462(3) 0.07913(13) 0.0624(10) Uani 1 1 d . . . O2 O 0.12574(10) 0.4974(5) 0.02601(13) 0.0782(13) Uani 1 1 d . . . O3 O 0.44253(9) 0.9455(3) 0.42982(11) 0.0504(8) Uani 1 1 d . . . O4 O 0.49621(9) 0.8049(3) 0.44910(10) 0.0467(7) Uani 1 1 d . . . O5 O 0.47569(9) 0.0750(3) 0.03662(11) 0.0466(7) Uani 1 1 d . . . O6 O 0.52577(9) 0.2182(3) 0.06531(11) 0.0465(7) Uani 1 1 d . . . C1 C 0.14146(13) 0.5641(5) 0.06465(18) 0.0528(12) Uani 1 1 d . . . C2 C 0.18707(7) 0.5426(4) 0.09458(15) 0.0644(15) Uani 1 1 d GU . . C3 C 0.20816(10) 0.6413(4) 0.12569(17) 0.125(3) Uani 1 1 d GU . . H3A H 0.1937 0.7153 0.1298 0.150 Uiso 1 1 calc R . . C4 C 0.25086(10) 0.6295(4) 0.15067(17) 0.123(3) Uani 1 1 d GU . . H4A H 0.2650 0.6956 0.1715 0.148 Uiso 1 1 calc R . . C5 C 0.27248(7) 0.5190(4) 0.14453(15) 0.0667(16) Uani 1 1 d GU . . C6 C 0.25139(11) 0.4202(4) 0.11341(17) 0.121(3) Uani 1 1 d GU . . H6A H 0.2659 0.3462 0.1093 0.145 Uiso 1 1 calc R . . C7 C 0.20869(10) 0.4320(4) 0.08844(17) 0.120(3) Uani 1 1 d GU . . H7A H 0.1946 0.3659 0.0676 0.144 Uiso 1 1 calc R . . C8 C 0.31926(13) 0.5118(5) 0.16897(17) 0.0558(13) Uani 1 1 d . . . C9 C 0.33799(13) 0.5741(5) 0.21456(17) 0.0573(14) Uani 1 1 d . . . H9A H 0.3212 0.6204 0.2299 0.069 Uiso 1 1 calc R . . C10 C 0.38106(13) 0.5687(5) 0.23753(16) 0.0484(12) Uani 1 1 d . . . C11 C 0.40587(13) 0.5005(5) 0.21355(16) 0.0506(12) Uani 1 1 d . . . H11A H 0.4348 0.4967 0.2284 0.061 Uiso 1 1 calc R . . C12 C 0.38812(13) 0.4377(5) 0.16770(16) 0.0488(11) Uani 1 1 d . . . C13 C 0.34466(13) 0.4436(5) 0.14642(17) 0.0555(13) Uani 1 1 d . . . H13A H 0.3324 0.4006 0.1163 0.067 Uiso 1 1 calc R . . C14 C 0.40090(13) 0.6358(5) 0.28623(16) 0.0497(12) Uani 1 1 d . . . C15 C 0.38245(15) 0.7428(6) 0.30030(19) 0.0756(19) Uani 1 1 d . . . H15A H 0.3567 0.7715 0.2795 0.091 Uiso 1 1 calc R . . C16 C 0.40113(15) 0.8088(6) 0.34448(19) 0.0698(17) Uani 1 1 d . . . H16A H 0.3876 0.8796 0.3532 0.084 Uiso 1 1 calc R . . C17 C 0.43971(13) 0.7700(4) 0.37563(15) 0.0426(10) Uani 1 1 d . . . C18 C 0.45831(13) 0.6634(5) 0.36242(16) 0.0507(12) Uani 1 1 d . . . H18A H 0.4841 0.6351 0.3833 0.061 Uiso 1 1 calc R . . C19 C 0.43912(13) 0.5971(5) 0.31826(16) 0.0522(12) Uani 1 1 d . . . H19A H 0.4523 0.5248 0.3101 0.063 Uiso 1 1 calc R . . C20 C 0.46104(13) 0.8463(4) 0.42220(15) 0.0424(10) Uani 1 1 d . . . C21 C 0.41500(13) 0.3669(5) 0.14230(16) 0.0476(11) Uani 1 1 d . . . C22 C 0.45499(13) 0.4113(5) 0.14443(18) 0.0545(13) Uani 1 1 d . . . H22A H 0.4656 0.4849 0.1630 0.065 Uiso 1 1 calc R . . C23 C 0.47918(13) 0.3469(5) 0.11920(18) 0.0512(12) Uani 1 1 d . . . H23A H 0.5058 0.3778 0.1209 0.061 Uiso 1 1 calc R . . C24 C 0.46428(12) 0.2373(4) 0.09152(15) 0.0394(9) Uani 1 1 d . . . C25 C 0.42473(14) 0.1928(5) 0.08937(18) 0.0523(12) Uani 1 1 d . . . H25A H 0.4143 0.1192 0.0707 0.063 Uiso 1 1 calc R . . C26 C 0.40032(14) 0.2562(5) 0.11467(19) 0.0567(13) Uani 1 1 d . . . H26A H 0.3738 0.2243 0.1131 0.068 Uiso 1 1 calc R . . C27 C 0.49038(13) 0.1725(4) 0.06282(14) 0.0381(9) Uani 1 1 d . . . O7 O 0.57566(12) 0.3282(3) 0.00410(15) 0.0697(10) Uani 1 1 d DU . . O8 O 0.57969(14) 0.1255(4) -0.06392(15) 0.0822(12) Uani 1 1 d DU . . S1 S 0.57133(13) 0.4453(3) 0.03507(15) 0.1134(15) Uani 0.614(5) 1 d PDU A 1 C28 C 0.6025(4) 0.5708(13) 0.0208(6) 0.155(6) Uani 0.614(5) 1 d PDU A 1 H28A H 0.6317 0.5492 0.0340 0.232 Uiso 0.614(5) 1 calc PR A 1 H28B H 0.5970 0.6499 0.0357 0.232 Uiso 0.614(5) 1 calc PR A 1 H28C H 0.5955 0.5811 -0.0151 0.232 Uiso 0.614(5) 1 calc PR A 1 C29 C 0.5188(3) 0.5034(14) 0.0060(6) 0.129(4) Uani 0.614(5) 1 d PDU . 1 H29A H 0.5306 0.4392 0.0310 0.193 Uiso 0.614(5) 1 calc PR A 1 H29B H 0.5275 0.5875 0.0195 0.193 Uiso 0.614(5) 1 calc PR A 1 H29C H 0.5283 0.4891 -0.0230 0.193 Uiso 0.614(5) 1 calc PR A 1 S1B S 0.6124(2) 0.4073(7) 0.0306(3) 0.142(3) Uani 0.386(5) 1 d PDU A 2 C28B C 0.6101(7) 0.4411(18) 0.0926(5) 0.118(6) Uani 0.386(5) 1 d PDU A 2 H28D H 0.6147 0.3631 0.1121 0.177 Uiso 0.386(5) 1 calc PR A 2 H28E H 0.5830 0.4758 0.0910 0.177 Uiso 0.386(5) 1 calc PR A 2 H28F H 0.6316 0.5027 0.1083 0.177 Uiso 0.386(5) 1 calc PR A 2 C29B C 0.5917(10) 0.5511(18) -0.0025(8) 0.165(9) Uani 0.386(5) 1 d PDU A 2 H29D H 0.5884 0.5397 -0.0377 0.247 Uiso 0.386(5) 1 calc PR A 2 H29E H 0.6106 0.6214 0.0102 0.247 Uiso 0.386(5) 1 calc PR A 2 H29F H 0.5648 0.5697 0.0022 0.247 Uiso 0.386(5) 1 calc PR A 2 S2 S 0.5717(3) 0.2079(9) -0.1090(3) 0.135(3) Uani 0.509(9) 1 d PDU A 1 C30 C 0.6259(6) 0.202(3) -0.1194(9) 0.172(7) Uani 0.509(9) 1 d PDU A 1 H30A H 0.6466 0.2358 -0.0902 0.258 Uiso 0.509(9) 1 calc PR A 1 H30B H 0.6257 0.2530 -0.1483 0.258 Uiso 0.509(9) 1 calc PR A 1 H30C H 0.6328 0.1144 -0.1248 0.258 Uiso 0.509(9) 1 calc PR A 1 C31 C 0.5423(7) 0.130(2) -0.1605(7) 0.190(8) Uani 0.509(9) 1 d PDU A 1 H31A H 0.5132 0.1353 -0.1617 0.285 Uiso 0.509(9) 1 calc PR A 1 H31B H 0.5508 0.0418 -0.1591 0.285 Uiso 0.509(9) 1 calc PR A 1 H31C H 0.5462 0.1702 -0.1900 0.285 Uiso 0.509(9) 1 calc PR A 1 S2B S 0.5916(3) 0.2380(7) -0.0899(3) 0.131(2) Uani 0.491(9) 1 d PDU A 2 C30B C 0.5949(8) 0.168(2) -0.1472(5) 0.155(6) Uani 0.491(9) 1 d PDU A 2 H30D H 0.5677 0.1361 -0.1661 0.232 Uiso 0.491(9) 1 calc PR A 2 H30E H 0.6147 0.0976 -0.1397 0.232 Uiso 0.491(9) 1 calc PR A 2 H30F H 0.6042 0.2315 -0.1666 0.232 Uiso 0.491(9) 1 calc PR A 2 C31B C 0.6445(4) 0.282(2) -0.0591(7) 0.175(7) Uani 0.491(9) 1 d PDU A 2 H31D H 0.6460 0.3232 -0.0276 0.262 Uiso 0.491(9) 1 calc PR A 2 H31E H 0.6541 0.3412 -0.0800 0.262 Uiso 0.491(9) 1 calc PR A 2 H31F H 0.6619 0.2067 -0.0531 0.262 Uiso 0.491(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02248(9) 0.03584(10) 0.02975(9) 0.00075(8) 0.00470(7) 0.00258(7) O1 0.0318(17) 0.066(2) 0.077(2) -0.0149(19) -0.0030(16) 0.0061(15) O2 0.0312(17) 0.133(4) 0.060(2) -0.033(2) -0.0031(15) 0.011(2) O3 0.0436(17) 0.0513(18) 0.0452(16) -0.0211(14) -0.0044(13) 0.0049(14) O4 0.0352(15) 0.0511(18) 0.0429(16) -0.0144(14) -0.0054(12) -0.0012(13) O5 0.0497(18) 0.0477(18) 0.0412(15) -0.0149(13) 0.0117(13) 0.0028(14) O6 0.0376(16) 0.0526(18) 0.0547(18) -0.0110(15) 0.0220(14) 0.0010(14) C1 0.026(2) 0.075(3) 0.053(3) -0.006(2) 0.0053(19) -0.001(2) C2 0.027(2) 0.096(4) 0.061(3) -0.028(3) -0.001(2) 0.009(2) C3 0.043(3) 0.169(6) 0.132(5) -0.084(5) -0.022(3) 0.033(4) C4 0.047(3) 0.165(6) 0.125(5) -0.093(4) -0.027(3) 0.033(4) C5 0.027(2) 0.102(4) 0.059(3) -0.043(3) -0.006(2) 0.014(2) C6 0.047(3) 0.163(6) 0.128(5) -0.085(5) -0.015(3) 0.031(4) C7 0.047(3) 0.161(6) 0.123(5) -0.083(5) -0.018(3) 0.022(4) C8 0.025(2) 0.084(4) 0.050(3) -0.031(2) -0.0006(18) 0.007(2) C9 0.031(2) 0.085(4) 0.049(3) -0.033(2) 0.0010(19) 0.011(2) C10 0.029(2) 0.069(3) 0.042(2) -0.025(2) 0.0010(17) 0.008(2) C11 0.024(2) 0.073(3) 0.049(2) -0.024(2) 0.0003(17) 0.007(2) C12 0.028(2) 0.069(3) 0.046(2) -0.024(2) 0.0057(18) 0.006(2) C13 0.030(2) 0.081(4) 0.049(3) -0.033(2) 0.0007(19) 0.005(2) C14 0.031(2) 0.069(3) 0.042(2) -0.022(2) -0.0012(17) 0.008(2) C15 0.042(3) 0.101(4) 0.063(3) -0.043(3) -0.019(2) 0.031(3) C16 0.046(3) 0.085(4) 0.062(3) -0.039(3) -0.011(2) 0.025(3) C17 0.031(2) 0.050(2) 0.040(2) -0.0146(19) -0.0001(17) -0.0004(18) C18 0.035(2) 0.063(3) 0.043(2) -0.014(2) -0.0074(18) 0.011(2) C19 0.039(2) 0.059(3) 0.048(2) -0.018(2) -0.0026(19) 0.015(2) C20 0.034(2) 0.047(2) 0.040(2) -0.0099(18) 0.0018(17) -0.0063(18) C21 0.030(2) 0.067(3) 0.044(2) -0.023(2) 0.0088(18) 0.005(2) C22 0.034(2) 0.064(3) 0.065(3) -0.033(2) 0.013(2) -0.003(2) C23 0.030(2) 0.062(3) 0.063(3) -0.025(2) 0.016(2) -0.006(2) C24 0.032(2) 0.044(2) 0.042(2) -0.0108(18) 0.0099(17) 0.0024(17) C25 0.039(2) 0.056(3) 0.062(3) -0.030(2) 0.016(2) -0.007(2) C26 0.037(2) 0.069(3) 0.068(3) -0.029(3) 0.021(2) -0.008(2) C27 0.035(2) 0.043(2) 0.035(2) -0.0018(17) 0.0095(16) 0.0071(18) O7 0.071(2) 0.048(2) 0.090(3) 0.0028(19) 0.024(2) -0.0146(18) O8 0.111(3) 0.082(3) 0.077(3) 0.018(2) 0.065(2) 0.008(2) S1 0.118(3) 0.0600(17) 0.141(3) -0.0115(18) 0.006(2) -0.0041(17) C28 0.161(12) 0.094(9) 0.171(12) -0.003(9) -0.010(10) -0.069(8) C29 0.136(9) 0.092(7) 0.140(8) 0.008(7) 0.012(8) 0.004(8) S1B 0.138(6) 0.116(5) 0.164(5) 0.005(4) 0.031(4) -0.032(4) C28B 0.141(13) 0.093(11) 0.116(11) -0.059(9) 0.032(10) -0.012(10) C29B 0.175(15) 0.135(14) 0.144(15) 0.021(13) -0.017(14) -0.011(14) S2 0.168(6) 0.145(5) 0.108(4) 0.036(4) 0.064(4) 0.045(4) C30 0.160(13) 0.228(15) 0.158(14) 0.022(13) 0.092(11) -0.018(13) C31 0.226(16) 0.214(16) 0.116(12) -0.013(13) 0.028(13) 0.046(15) S2B 0.173(6) 0.127(4) 0.116(5) 0.032(4) 0.077(4) -0.012(4) C30B 0.202(15) 0.201(14) 0.088(10) 0.010(11) 0.084(10) -0.011(14) C31B 0.158(12) 0.185(13) 0.197(13) 0.016(12) 0.077(11) -0.023(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 Gd1 O5 2.328(3) 5_655 ? Gd1 O3 2.354(3) 2_645 ? Gd1 O4 2.372(3) 6_565 ? Gd1 O6 2.385(3) . ? Gd1 O8 2.403(3) . ? Gd1 O7 2.425(3) . ? Gd1 O1 2.472(3) 3_545 ? Gd1 O2 2.501(3) 3_545 ? Gd1 C1 2.847(4) 3_545 ? Gd1 C27 3.048(4) . ? O1 C1 1.245(6) . ? O1 Gd1 2.472(3) 3_455 ? O2 C1 1.255(6) . ? O2 Gd1 2.501(3) 3_455 ? O3 C20 1.248(5) . ? O3 Gd1 2.354(3) 2_665 ? O4 C20 1.263(5) . ? O4 Gd1 2.372(3) 6_566 ? O5 C27 1.258(5) . ? O5 Gd1 2.328(3) 5_655 ? O6 C27 1.251(5) . ? C1 C2 1.516(5) . ? C1 Gd1 2.847(4) 3_455 ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 C8 1.504(4) . ? C6 C7 1.3900 . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.384(6) . ? C8 C9 1.395(6) . ? C9 C10 1.387(6) . ? C9 H9A 0.9300 . ? C10 C11 1.395(6) . ? C10 C14 1.492(5) . ? C11 C12 1.397(5) . ? C11 H11A 0.9300 . ? C12 C13 1.392(6) . ? C12 C21 1.485(6) . ? C13 H13A 0.9300 . ? C14 C15 1.379(6) . ? C14 C19 1.379(6) . ? C15 C16 1.383(6) . ? C15 H15A 0.9300 . ? C16 C17 1.379(6) . ? C16 H16A 0.9300 . ? C17 C18 1.369(6) . ? C17 C20 1.504(5) . ? C18 C19 1.388(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C26 1.387(6) . ? C21 C22 1.391(6) . ? C22 C23 1.384(6) . ? C22 H22A 0.9300 . ? C23 C24 1.380(6) . ? C23 H23A 0.9300 . ? C24 C25 1.378(6) . ? C24 C27 1.498(5) . ? C25 C26 1.386(6) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? O7 S1B 1.476(6) . ? O7 S1 1.519(4) . ? O8 S2 1.473(6) . ? O8 S2B 1.484(6) . ? S1 C28 1.779(9) . ? S1 C29 1.800(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C29 1.194(18) 5_665 ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? S1B C29B 1.781(10) . ? S1B C28B 1.782(10) . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? S2 C31 1.68(2) . ? S2 C30 1.908(19) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? S2B C31B 1.775(10) . ? S2B C30B 1.783(10) . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? 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 Gd1 O3 75.09(11) 5_655 2_645 ? O5 Gd1 O4 77.51(11) 5_655 6_565 ? O3 Gd1 O4 128.60(10) 2_645 6_565 ? O5 Gd1 O6 123.22(10) 5_655 . ? O3 Gd1 O6 78.80(12) 2_645 . ? O4 Gd1 O6 81.18(11) 6_565 . ? O5 Gd1 O8 79.24(13) 5_655 . ? O3 Gd1 O8 136.46(13) 2_645 . ? O4 Gd1 O8 77.49(13) 6_565 . ? O6 Gd1 O8 144.49(13) . . ? O5 Gd1 O7 145.06(12) 5_655 . ? O3 Gd1 O7 139.85(12) 2_645 . ? O4 Gd1 O7 76.62(12) 6_565 . ? O6 Gd1 O7 75.10(12) . . ? O8 Gd1 O7 72.54(13) . . ? O5 Gd1 O1 135.57(11) 5_655 3_545 ? O3 Gd1 O1 74.01(11) 2_645 3_545 ? O4 Gd1 O1 146.80(11) 6_565 3_545 ? O6 Gd1 O1 80.51(11) . 3_545 ? O8 Gd1 O1 102.74(14) . 3_545 ? O7 Gd1 O1 72.02(13) . 3_545 ? O5 Gd1 O2 89.17(12) 5_655 3_545 ? O3 Gd1 O2 74.12(13) 2_645 3_545 ? O4 Gd1 O2 147.53(12) 6_565 3_545 ? O6 Gd1 O2 129.93(11) . 3_545 ? O8 Gd1 O2 70.93(14) . 3_545 ? O7 Gd1 O2 100.39(14) . 3_545 ? O1 Gd1 O2 51.98(11) 3_545 3_545 ? O5 Gd1 C1 113.07(13) 5_655 3_545 ? O3 Gd1 C1 72.33(13) 2_645 3_545 ? O4 Gd1 C1 159.07(13) 6_565 3_545 ? O6 Gd1 C1 105.29(12) . 3_545 ? O8 Gd1 C1 86.61(15) . 3_545 ? O7 Gd1 C1 85.74(14) . 3_545 ? O1 Gd1 C1 25.86(12) 3_545 3_545 ? O2 Gd1 C1 26.13(12) 3_545 3_545 ? O5 Gd1 C27 100.60(11) 5_655 . ? O3 Gd1 C27 71.55(11) 2_645 . ? O4 Gd1 C27 71.91(11) 6_565 . ? O6 Gd1 C27 22.69(10) . . ? O8 Gd1 C27 148.58(13) . . ? O7 Gd1 C27 93.26(12) . . ? O1 Gd1 C27 98.99(11) 3_545 . ? O2 Gd1 C27 140.28(12) 3_545 . ? C1 Gd1 C27 120.94(12) 3_545 . ? C1 O1 Gd1 94.1(3) . 3_455 ? C1 O2 Gd1 92.5(3) . 3_455 ? C20 O3 Gd1 142.3(3) . 2_665 ? C20 O4 Gd1 135.9(3) . 6_566 ? C27 O5 Gd1 175.8(3) . 5_655 ? C27 O6 Gd1 110.0(3) . . ? O1 C1 O2 121.4(4) . . ? O1 C1 C2 119.5(4) . . ? O2 C1 C2 119.1(4) . . ? O1 C1 Gd1 60.0(2) . 3_455 ? O2 C1 Gd1 61.4(2) . 3_455 ? C2 C1 Gd1 179.5(3) . 3_455 ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.2(3) . . ? C7 C2 C1 121.6(3) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 C8 120.6(3) . . ? C4 C5 C8 119.2(3) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C13 C8 C9 118.6(4) . . ? C13 C8 C5 120.5(4) . . ? C9 C8 C5 120.9(4) . . ? C10 C9 C8 121.6(4) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C11 118.4(4) . . ? C9 C10 C14 121.3(4) . . ? C11 C10 C14 120.3(4) . . ? C10 C11 C12 121.4(4) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C13 C12 C11 118.3(4) . . ? C13 C12 C21 120.9(4) . . ? C11 C12 C21 120.8(4) . . ? C8 C13 C12 121.6(4) . . ? C8 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C15 C14 C19 117.0(4) . . ? C15 C14 C10 121.2(4) . . ? C19 C14 C10 121.8(4) . . ? C14 C15 C16 121.9(4) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C17 C16 C15 120.4(4) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C18 C17 C16 118.5(4) . . ? C18 C17 C20 121.3(4) . . ? C16 C17 C20 120.2(4) . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C14 C19 C18 121.5(4) . . ? C14 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? O3 C20 O4 126.6(4) . . ? O3 C20 C17 116.6(4) . . ? O4 C20 C17 116.8(4) . . ? C26 C21 C22 118.3(4) . . ? C26 C21 C12 120.6(4) . . ? C22 C21 C12 121.1(4) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C25 C24 C23 118.8(4) . . ? C25 C24 C27 121.4(4) . . ? C23 C24 C27 119.8(4) . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C25 C26 C21 120.7(4) . . ? C25 C26 H26A 119.6 . . ? C21 C26 H26A 119.6 . . ? O6 C27 O5 122.4(4) . . ? O6 C27 C24 118.8(4) . . ? O5 C27 C24 118.8(4) . . ? O6 C27 Gd1 47.33(19) . . ? O5 C27 Gd1 75.2(2) . . ? C24 C27 Gd1 165.5(3) . . ? S1B O7 S1 58.4(4) . . ? S1B O7 Gd1 134.6(4) . . ? S1 O7 Gd1 131.0(3) . . ? S2 O8 S2B 30.6(4) . . ? S2 O8 Gd1 138.4(4) . . ? S2B O8 Gd1 133.0(4) . . ? O7 S1 C28 107.5(7) . . ? O7 S1 C29 104.7(6) . . ? C28 S1 C29 101.9(6) . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 C29 S1 154.3(18) 5_665 . ? C29 C29 H29A 109.5 5_665 . ? S1 C29 H29A 45.9 . . ? C29 C29 H29B 109.5 5_665 . ? S1 C29 H29B 89.2 . . ? H29A C29 H29B 109.5 . . ? C29 C29 H29C 109.5 5_665 . ? S1 C29 H29C 78.9 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 S1B C29B 94.0(11) . . ? O7 S1B C28B 109.1(8) . . ? C29B S1B C28B 102.3(7) . . ? S1B C28B H28D 109.5 . . ? S1B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? S1B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? S1B C29B H29D 109.5 . . ? S1B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? S1B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? O8 S2 C31 111.2(11) . . ? O8 S2 C30 99.6(9) . . ? C31 S2 C30 101.2(9) . . ? S2 C30 H30A 109.5 . . ? S2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? S2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? S2 C31 H31A 109.5 . . ? S2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O8 S2B C31B 109.7(9) . . ? O8 S2B C30B 102.0(8) . . ? C31B S2B C30B 102.9(7) . . ? S2B C30B H30D 109.5 . . ? S2B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? S2B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? S2B C31B H31D 109.5 . . ? S2B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? S2B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.612 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.097 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.198 0.213 -0.002 3554.5 223.8 2 0.000 0.152 0.250 14.1 3.6 3 0.500 0.652 0.250 14.1 3.6 4 0.000 0.848 0.750 14.1 2.9 5 0.500 0.348 0.750 14.1 2.9 _platon_squeeze_details ; ? ; _database_code_depnum_ccdc_archive 'CCDC 930172' ####################################################################### # # 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-Tb #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H27 O8 S2 Tb' _chemical_formula_sum 'C31 H27 N0 O8 S2 Tb' _chemical_formula_weight 750.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.182(9) _cell_length_b 10.296(2) _cell_length_c 27.814(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.238(4) _cell_angle_gamma 90.00 _cell_volume 9076(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10885 _cell_measurement_theta_min 2.8663 _cell_measurement_theta_max 27.5089 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 1.683 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6321 _exptl_absorpt_correction_T_max 0.7295 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 20668 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48265 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10375 _reflns_number_gt 8941 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+80.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10375 _refine_ls_number_parameters 423 _refine_ls_number_restraints 393 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.104 _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 Tb1 Tb 0.555382(6) 0.10622(2) 0.009470(7) 0.03077(6) Uani 1 1 d . . . O1 O 0.12006(11) 0.6493(4) 0.07696(16) 0.0663(11) Uani 1 1 d . . . O2 O 0.12437(11) 0.4915(5) 0.02684(15) 0.0788(14) Uani 1 1 d . . . O3 O 0.44338(10) 0.9509(3) 0.42876(12) 0.0493(8) Uani 1 1 d . . . O4 O 0.49648(10) 0.8075(3) 0.44841(12) 0.0470(8) Uani 1 1 d . . . O5 O 0.47439(10) 0.0756(3) 0.03539(12) 0.0460(8) Uani 1 1 d . . . O6 O 0.52464(10) 0.2203(3) 0.06367(12) 0.0467(8) Uani 1 1 d . . . C1 C 0.14046(14) 0.5617(6) 0.0643(2) 0.0560(14) Uani 1 1 d . . . C2 C 0.18552(8) 0.5420(5) 0.09373(16) 0.0688(16) Uani 1 1 d GU . . C3 C 0.20706(12) 0.6441(4) 0.12294(19) 0.113(3) Uani 1 1 d GU . . H3A H 0.1929 0.7205 0.1254 0.136 Uiso 1 1 calc R . . C4 C 0.24977(11) 0.6319(4) 0.14844(18) 0.114(3) Uani 1 1 d GU . . H4A H 0.2642 0.7003 0.1680 0.136 Uiso 1 1 calc R . . C5 C 0.27096(8) 0.5177(4) 0.14472(15) 0.0599(15) Uani 1 1 d GU . . C6 C 0.24943(12) 0.4156(4) 0.11551(18) 0.110(3) Uani 1 1 d GU . . H6A H 0.2636 0.3391 0.1130 0.132 Uiso 1 1 calc R . . C7 C 0.20671(11) 0.4277(4) 0.09001(18) 0.108(3) Uani 1 1 d GU . . H7A H 0.1923 0.3594 0.0705 0.129 Uiso 1 1 calc R . . C8 C 0.31884(14) 0.5115(6) 0.16921(19) 0.0581(15) Uani 1 1 d . . . C9 C 0.33748(14) 0.5755(6) 0.21432(19) 0.0587(15) Uani 1 1 d . . . H9A H 0.3206 0.6221 0.2296 0.070 Uiso 1 1 calc R . . C10 C 0.38087(14) 0.5710(5) 0.23700(18) 0.0502(13) Uani 1 1 d . . . C11 C 0.40547(14) 0.5019(5) 0.21288(18) 0.0519(13) Uani 1 1 d . . . H11A H 0.4346 0.4989 0.2274 0.062 Uiso 1 1 calc R . . C12 C 0.38753(14) 0.4372(5) 0.16743(18) 0.0504(13) Uani 1 1 d . . . C13 C 0.34408(15) 0.4427(6) 0.14625(19) 0.0587(15) Uani 1 1 d . . . H13A H 0.3316 0.3995 0.1161 0.070 Uiso 1 1 calc R . . C14 C 0.40082(14) 0.6390(5) 0.28543(17) 0.0482(12) Uani 1 1 d . . . C15 C 0.38274(16) 0.7490(6) 0.2988(2) 0.0698(19) Uani 1 1 d . . . H15A H 0.3571 0.7784 0.2777 0.084 Uiso 1 1 calc R . . C16 C 0.40185(16) 0.8161(6) 0.3425(2) 0.0635(16) Uani 1 1 d . . . H16A H 0.3890 0.8898 0.3506 0.076 Uiso 1 1 calc R . . C17 C 0.44003(13) 0.7743(5) 0.37443(17) 0.0426(10) Uani 1 1 d . . . C18 C 0.45839(14) 0.6658(5) 0.36154(17) 0.0495(12) Uani 1 1 d . . . H18A H 0.4842 0.6372 0.3824 0.059 Uiso 1 1 calc R . . C19 C 0.43895(14) 0.5984(5) 0.31789(18) 0.0511(13) Uani 1 1 d . . . H19A H 0.4518 0.5242 0.3102 0.061 Uiso 1 1 calc R . . C20 C 0.46159(13) 0.8504(5) 0.42111(16) 0.0407(10) Uani 1 1 d . . . C21 C 0.41435(14) 0.3674(5) 0.14175(18) 0.0482(12) Uani 1 1 d . . . C22 C 0.45439(14) 0.4123(6) 0.1438(2) 0.0551(14) Uani 1 1 d . . . H22A H 0.4651 0.4860 0.1626 0.066 Uiso 1 1 calc R . . C23 C 0.47840(14) 0.3488(5) 0.11831(19) 0.0509(13) Uani 1 1 d . . . H23A H 0.5051 0.3802 0.1201 0.061 Uiso 1 1 calc R . . C24 C 0.46332(14) 0.2389(5) 0.09018(17) 0.0413(10) Uani 1 1 d . . . C25 C 0.42385(15) 0.1933(5) 0.0881(2) 0.0540(13) Uani 1 1 d . . . H25A H 0.4133 0.1196 0.0692 0.065 Uiso 1 1 calc R . . C26 C 0.39964(15) 0.2560(6) 0.1139(2) 0.0589(15) Uani 1 1 d . . . H26A H 0.3732 0.2231 0.1126 0.071 Uiso 1 1 calc R . . C27 C 0.48928(14) 0.1742(4) 0.06131(15) 0.0383(9) Uani 1 1 d . . . O7 O 0.57482(13) 0.3295(4) 0.00366(17) 0.0727(11) Uani 1 1 d DU . . O8 O 0.58105(16) 0.1263(5) -0.06163(17) 0.0841(13) Uani 1 1 d DU . . S1 S 0.57011(15) 0.4458(4) 0.03530(19) 0.1118(18) Uani 0.562(6) 1 d PDU A 1 C28 C 0.6044(6) 0.5735(17) 0.0328(9) 0.156(7) Uani 0.562(6) 1 d PDU A 1 H28A H 0.6331 0.5452 0.0467 0.235 Uiso 0.562(6) 1 calc PR A 1 H28B H 0.5991 0.6458 0.0519 0.235 Uiso 0.562(6) 1 calc PR A 1 H28C H 0.5997 0.5994 -0.0016 0.235 Uiso 0.562(6) 1 calc PR A 1 C29 C 0.5187(3) 0.5060(16) 0.0058(7) 0.125(5) Uani 0.562(6) 1 d PDU . 1 H29A H 0.5318 0.4267 0.0207 0.187 Uiso 0.562(6) 1 calc PR A 1 H29B H 0.5271 0.5755 0.0297 0.187 Uiso 0.562(6) 1 calc PR A 1 H29C H 0.5271 0.5256 -0.0236 0.187 Uiso 0.562(6) 1 calc PR A 1 S1B S 0.6084(3) 0.4187(10) 0.0329(4) 0.220(4) Uani 0.438(6) 1 d PDU A 2 C28B C 0.6134(8) 0.451(2) 0.0965(6) 0.159(7) Uani 0.438(6) 1 d PDU A 2 H28D H 0.6174 0.3709 0.1150 0.238 Uiso 0.438(6) 1 calc PR A 2 H28E H 0.5882 0.4930 0.0990 0.238 Uiso 0.438(6) 1 calc PR A 2 H28F H 0.6372 0.5067 0.1102 0.238 Uiso 0.438(6) 1 calc PR A 2 C29B C 0.6009(10) 0.5691(17) 0.0022(8) 0.155(8) Uani 0.438(6) 1 d PDU A 2 H29D H 0.5985 0.5568 -0.0327 0.232 Uiso 0.438(6) 1 calc PR A 2 H29E H 0.6245 0.6246 0.0174 0.232 Uiso 0.438(6) 1 calc PR A 2 H29F H 0.5755 0.6085 0.0052 0.232 Uiso 0.438(6) 1 calc PR A 2 S2 S 0.5675(5) 0.1882(14) -0.1122(4) 0.205(4) Uani 0.455(9) 1 d PDU A 1 C30 C 0.6255(7) 0.192(3) -0.1203(11) 0.156(7) Uani 0.455(9) 1 d PDU A 1 H30A H 0.6450 0.2265 -0.0902 0.234 Uiso 0.455(9) 1 calc PR A 1 H30B H 0.6254 0.2468 -0.1484 0.234 Uiso 0.455(9) 1 calc PR A 1 H30C H 0.6338 0.1060 -0.1262 0.234 Uiso 0.455(9) 1 calc PR A 1 C31 C 0.5412(9) 0.127(3) -0.1683(11) 0.195(9) Uani 0.455(9) 1 d PDU A 1 H31A H 0.5115 0.1283 -0.1722 0.292 Uiso 0.455(9) 1 calc PR A 1 H31B H 0.5501 0.0388 -0.1706 0.292 Uiso 0.455(9) 1 calc PR A 1 H31C H 0.5470 0.1778 -0.1944 0.292 Uiso 0.455(9) 1 calc PR A 1 S2B S 0.5888(2) 0.2360(5) -0.0924(2) 0.119(2) Uani 0.545(9) 1 d PDU A 2 C30B C 0.5925(8) 0.158(2) -0.1474(6) 0.160(7) Uani 0.545(9) 1 d PDU A 2 H30D H 0.5652 0.1259 -0.1663 0.239 Uiso 0.545(9) 1 calc PR A 2 H30E H 0.6119 0.0865 -0.1383 0.239 Uiso 0.545(9) 1 calc PR A 2 H30F H 0.6023 0.2184 -0.1676 0.239 Uiso 0.545(9) 1 calc PR A 2 C31B C 0.6411(5) 0.280(3) -0.0593(8) 0.201(8) Uani 0.545(9) 1 d PDU A 2 H31D H 0.6416 0.3202 -0.0280 0.301 Uiso 0.545(9) 1 calc PR A 2 H31E H 0.6516 0.3395 -0.0792 0.301 Uiso 0.545(9) 1 calc PR A 2 H31F H 0.6585 0.2035 -0.0527 0.301 Uiso 0.545(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02384(10) 0.03554(11) 0.03085(10) 0.00052(8) 0.00489(7) 0.00206(8) O1 0.0326(18) 0.068(3) 0.083(3) -0.017(2) -0.0059(18) 0.0029(18) O2 0.0319(18) 0.129(4) 0.065(2) -0.036(3) -0.0015(17) 0.010(2) O3 0.0439(18) 0.049(2) 0.0448(18) -0.0196(15) -0.0021(14) 0.0049(15) O4 0.0375(17) 0.0499(19) 0.0420(17) -0.0122(15) -0.0060(13) -0.0002(15) O5 0.0497(19) 0.0454(19) 0.0411(17) -0.0147(14) 0.0109(14) 0.0043(15) O6 0.0388(17) 0.051(2) 0.0546(19) -0.0098(16) 0.0207(15) 0.0017(15) C1 0.027(2) 0.080(4) 0.057(3) -0.006(3) 0.005(2) 0.000(2) C2 0.035(3) 0.094(4) 0.067(3) -0.029(3) 0.001(2) 0.010(3) C3 0.046(3) 0.141(6) 0.127(5) -0.068(5) -0.015(3) 0.027(4) C4 0.046(3) 0.152(6) 0.111(5) -0.063(5) -0.025(3) 0.008(4) C5 0.036(2) 0.087(4) 0.044(2) -0.044(3) -0.0083(19) 0.013(2) C6 0.048(3) 0.136(6) 0.129(5) -0.050(5) -0.002(4) 0.029(4) C7 0.049(3) 0.133(6) 0.116(5) -0.063(5) -0.014(3) 0.014(4) C8 0.025(2) 0.088(4) 0.053(3) -0.031(3) 0.000(2) 0.007(2) C9 0.030(2) 0.088(4) 0.052(3) -0.033(3) 0.002(2) 0.012(2) C10 0.028(2) 0.073(4) 0.043(2) -0.025(2) 0.0001(18) 0.007(2) C11 0.027(2) 0.072(4) 0.050(3) -0.026(3) 0.0022(19) 0.006(2) C12 0.031(2) 0.069(3) 0.048(3) -0.027(2) 0.0061(19) 0.003(2) C13 0.033(2) 0.085(4) 0.051(3) -0.037(3) 0.003(2) 0.003(2) C14 0.029(2) 0.066(3) 0.043(2) -0.022(2) 0.0011(18) 0.007(2) C15 0.038(3) 0.094(5) 0.058(3) -0.039(3) -0.015(2) 0.026(3) C16 0.044(3) 0.073(4) 0.058(3) -0.031(3) -0.009(2) 0.022(3) C17 0.032(2) 0.050(3) 0.039(2) -0.015(2) -0.0011(18) 0.000(2) C18 0.035(2) 0.059(3) 0.043(2) -0.011(2) -0.0076(19) 0.012(2) C19 0.038(2) 0.059(3) 0.046(3) -0.018(2) -0.004(2) 0.013(2) C20 0.032(2) 0.047(3) 0.037(2) -0.0091(19) 0.0013(18) -0.0032(19) C21 0.032(2) 0.065(3) 0.047(3) -0.024(2) 0.0096(19) 0.002(2) C22 0.035(2) 0.065(3) 0.063(3) -0.034(3) 0.010(2) -0.005(2) C23 0.033(2) 0.062(3) 0.059(3) -0.026(3) 0.015(2) -0.008(2) C24 0.034(2) 0.047(3) 0.043(2) -0.015(2) 0.0114(18) 0.0024(19) C25 0.040(3) 0.057(3) 0.066(3) -0.031(3) 0.019(2) -0.007(2) C26 0.034(2) 0.073(4) 0.072(3) -0.033(3) 0.020(2) -0.012(2) C27 0.038(2) 0.042(2) 0.034(2) -0.0014(18) 0.0094(17) 0.0080(19) O7 0.068(2) 0.052(2) 0.100(3) 0.002(2) 0.029(2) -0.014(2) O8 0.111(3) 0.086(3) 0.079(3) 0.019(2) 0.064(3) 0.011(3) S1 0.104(3) 0.061(2) 0.149(4) -0.015(2) 0.004(3) -0.004(2) C28 0.150(12) 0.142(13) 0.186(15) 0.004(12) 0.063(12) -0.032(11) C29 0.126(9) 0.092(8) 0.149(9) -0.002(8) 0.030(9) 0.006(9) S1B 0.195(8) 0.198(8) 0.241(8) -0.004(7) 0.026(7) -0.010(7) C28B 0.175(14) 0.150(14) 0.158(14) -0.048(13) 0.059(13) 0.002(13) C29B 0.171(14) 0.090(11) 0.162(15) 0.007(12) -0.013(14) -0.056(11) S2 0.208(8) 0.191(8) 0.210(8) 0.010(7) 0.054(7) 0.026(7) C30 0.148(14) 0.192(15) 0.157(14) 0.020(13) 0.091(12) -0.003(14) C31 0.216(17) 0.188(16) 0.170(16) -0.022(15) 0.041(15) 0.036(16) S2B 0.168(5) 0.103(4) 0.119(4) 0.038(3) 0.092(4) 0.009(3) C30B 0.225(15) 0.181(14) 0.106(11) 0.009(11) 0.099(11) 0.008(14) C31B 0.182(13) 0.205(14) 0.224(14) 0.014(13) 0.074(12) 0.004(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O5 2.304(3) 5_655 ? Tb1 O3 2.339(3) 2_645 ? Tb1 O4 2.351(3) 6_565 ? Tb1 O6 2.367(3) . ? Tb1 O8 2.383(4) . ? Tb1 O7 2.406(4) . ? Tb1 O1 2.437(3) 3_545 ? Tb1 O2 2.493(4) 3_545 ? Tb1 C1 2.820(5) 3_545 ? O1 C1 1.240(6) . ? O1 Tb1 2.437(3) 3_455 ? O2 C1 1.249(6) . ? O2 Tb1 2.493(4) 3_455 ? O3 C20 1.248(5) . ? O3 Tb1 2.339(3) 2_665 ? O4 C20 1.261(5) . ? O4 Tb1 2.351(3) 6_566 ? O5 C27 1.258(5) . ? O5 Tb1 2.304(3) 5_655 ? O6 C27 1.249(5) . ? C1 C2 1.491(5) . ? C1 Tb1 2.820(5) 3_455 ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 C8 1.533(5) . ? C6 C7 1.3900 . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.389(6) . ? C8 C9 1.390(6) . ? C9 C10 1.391(6) . ? C9 H9A 0.9300 . ? C10 C11 1.395(6) . ? C10 C14 1.488(6) . ? C11 C12 1.396(6) . ? C11 H11A 0.9300 . ? C12 C13 1.388(6) . ? C12 C21 1.482(6) . ? C13 H13A 0.9300 . ? C14 C15 1.383(7) . ? C14 C19 1.383(6) . ? C15 C16 1.380(7) . ? C15 H15A 0.9300 . ? C16 C17 1.382(6) . ? C16 H16A 0.9300 . ? C17 C18 1.371(6) . ? C17 C20 1.503(6) . ? C18 C19 1.381(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.392(6) . ? C21 C26 1.389(7) . ? C22 C23 1.378(6) . ? C22 H22A 0.9300 . ? C23 C24 1.382(6) . ? C23 H23A 0.9300 . ? C24 C25 1.377(6) . ? C24 C27 1.497(6) . ? C25 C26 1.385(6) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? O7 S1B 1.486(7) . ? O7 S1 1.521(5) . ? O8 S2B 1.485(5) . ? O8 S2 1.487(8) . ? S1 C28 1.754(10) . ? S1 C29 1.773(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C29 1.19(2) 5_665 ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? S1B C29B 1.749(10) . ? S1B C28B 1.760(10) . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? S2 C31 1.67(3) . ? S2 C30 2.00(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? S2B C31B 1.762(11) . ? S2B C30B 1.767(10) . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? 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 Tb1 O3 75.73(12) 5_655 2_645 ? O5 Tb1 O4 77.55(12) 5_655 6_565 ? O3 Tb1 O4 128.24(11) 2_645 6_565 ? O5 Tb1 O6 123.47(11) 5_655 . ? O3 Tb1 O6 77.80(13) 2_645 . ? O4 Tb1 O6 81.35(12) 6_565 . ? O5 Tb1 O8 79.76(15) 5_655 . ? O3 Tb1 O8 137.40(15) 2_645 . ? O4 Tb1 O8 78.04(15) 6_565 . ? O6 Tb1 O8 144.39(14) . . ? O5 Tb1 O7 145.14(14) 5_655 . ? O3 Tb1 O7 139.12(14) 2_645 . ? O4 Tb1 O7 76.85(13) 6_565 . ? O6 Tb1 O7 75.12(13) . . ? O8 Tb1 O7 72.10(15) . . ? O5 Tb1 O1 134.71(12) 5_655 3_545 ? O3 Tb1 O1 74.85(13) 2_645 3_545 ? O4 Tb1 O1 147.32(13) 6_565 3_545 ? O6 Tb1 O1 82.33(12) . 3_545 ? O8 Tb1 O1 100.01(17) . 3_545 ? O7 Tb1 O1 71.68(15) . 3_545 ? O5 Tb1 O2 86.66(13) 5_655 3_545 ? O3 Tb1 O2 73.63(14) 2_645 3_545 ? O4 Tb1 O2 146.96(13) 6_565 3_545 ? O6 Tb1 O2 130.99(12) . 3_545 ? O8 Tb1 O2 70.63(16) . 3_545 ? O7 Tb1 O2 102.53(16) . 3_545 ? O1 Tb1 O2 52.29(13) 3_545 3_545 ? O5 Tb1 C1 111.13(15) 5_655 3_545 ? O3 Tb1 C1 72.24(14) 2_645 3_545 ? O4 Tb1 C1 159.51(14) 6_565 3_545 ? O6 Tb1 C1 106.73(14) . 3_545 ? O8 Tb1 C1 85.17(17) . 3_545 ? O7 Tb1 C1 86.93(16) . 3_545 ? O1 Tb1 C1 26.00(14) 3_545 3_545 ? O2 Tb1 C1 26.29(14) 3_545 3_545 ? C1 O1 Tb1 94.5(3) . 3_455 ? C1 O2 Tb1 91.6(3) . 3_455 ? C20 O3 Tb1 142.0(3) . 2_665 ? C20 O4 Tb1 136.2(3) . 6_566 ? C27 O5 Tb1 176.9(3) . 5_655 ? C27 O6 Tb1 110.7(3) . . ? O1 C1 O2 121.5(5) . . ? O1 C1 C2 119.1(5) . . ? O2 C1 C2 119.4(5) . . ? O1 C1 Tb1 59.5(2) . 3_455 ? O2 C1 Tb1 62.1(3) . 3_455 ? C2 C1 Tb1 178.4(4) . 3_455 ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.5(4) . . ? C7 C2 C1 121.4(4) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C8 118.8(3) . . ? C6 C5 C8 120.9(3) . . ? C7 C6 C5 120.0 . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C13 C8 C9 119.3(4) . . ? C13 C8 C5 120.2(4) . . ? C9 C8 C5 120.5(4) . . ? C8 C9 C10 121.2(4) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C11 118.3(4) . . ? C9 C10 C14 121.2(4) . . ? C11 C10 C14 120.6(4) . . ? C12 C11 C10 121.7(4) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C13 C12 C11 118.4(4) . . ? C13 C12 C21 120.8(4) . . ? C11 C12 C21 120.8(4) . . ? C8 C13 C12 121.2(4) . . ? C8 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C15 C14 C19 117.2(4) . . ? C15 C14 C10 121.1(4) . . ? C19 C14 C10 121.6(4) . . ? C16 C15 C14 121.6(5) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C18 C17 C16 118.7(4) . . ? C18 C17 C20 121.1(4) . . ? C16 C17 C20 120.2(4) . . ? C17 C18 C19 120.8(4) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C18 C19 C14 121.4(4) . . ? C18 C19 H19A 119.3 . . ? C14 C19 H19A 119.3 . . ? O3 C20 O4 126.3(4) . . ? O3 C20 C17 116.6(4) . . ? O4 C20 C17 117.1(4) . . ? C22 C21 C26 118.0(4) . . ? C22 C21 C12 121.5(4) . . ? C26 C21 C12 120.5(4) . . ? C23 C22 C21 120.8(5) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 120.8(4) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C25 C24 C23 118.9(4) . . ? C25 C24 C27 121.2(4) . . ? C23 C24 C27 119.9(4) . . ? C24 C25 C26 120.7(5) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.8(5) . . ? C25 C26 H26A 119.6 . . ? C21 C26 H26A 119.6 . . ? O6 C27 O5 122.7(4) . . ? O6 C27 C24 118.9(4) . . ? O5 C27 C24 118.4(4) . . ? S1B O7 S1 52.2(5) . . ? S1B O7 Tb1 136.6(5) . . ? S1 O7 Tb1 129.6(3) . . ? S2B O8 S2 35.4(6) . . ? S2B O8 Tb1 135.2(3) . . ? S2 O8 Tb1 137.7(6) . . ? O7 S1 C28 112.8(9) . . ? O7 S1 C29 104.9(7) . . ? C28 S1 C29 105.4(8) . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 C29 S1 151(2) 5_665 . ? C29 C29 H29A 109.5 5_665 . ? S1 C29 H29A 41.4 . . ? C29 C29 H29B 109.5 5_665 . ? S1 C29 H29B 84.0 . . ? H29A C29 H29B 109.5 . . ? C29 C29 H29C 109.5 5_665 . ? S1 C29 H29C 89.0 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 S1B C29B 107.8(10) . . ? O7 S1B C28B 119.9(12) . . ? C29B S1B C28B 106.2(8) . . ? S1B C28B H28D 109.5 . . ? S1B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? S1B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? S1B C29B H29D 109.5 . . ? S1B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? S1B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? O8 S2 C31 130.5(16) . . ? O8 S2 C30 94.9(10) . . ? C31 S2 C30 98.9(12) . . ? S2 C30 H30A 109.5 . . ? S2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? S2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? S2 C31 H31A 109.5 . . ? S2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O8 S2B C31B 101.9(10) . . ? O8 S2B C30B 102.7(8) . . ? C31B S2B C30B 105.0(8) . . ? S2B C30B H30D 109.5 . . ? S2B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? S2B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? S2B C31B H31D 109.5 . . ? S2B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? S2B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.083 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.105 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.216 0.079 0.028 3454.3 132.7 2 0.000 0.150 0.250 12.7 2.8 3 0.500 0.650 0.250 12.7 2.8 4 0.000 0.850 0.750 12.7 1.8 5 0.500 0.350 0.750 12.7 1.8 _platon_squeeze_details ; ? ; #==END _database_code_depnum_ccdc_archive 'CCDC 930173'