# Electronic Supplementary Material (ESI) for CrystEngComm # 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_General #TrackingRef 'CIFLa.cif' _audit_creation_date 2010-06-16 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== data__TC6A-SO3-La #TrackingRef 'CIFLa.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H18 La2 O51 S12 ' _chemical_formula_moiety 'C36 H18 La2 O51 S12 ' _chemical_formula_weight 1929.04 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 13.9731(4) _cell_length_b 26.4604(7) _cell_length_c 19.5809(6) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 7239.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 44790 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792.00 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.785 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 66639 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Hydrogen atoms of all water molecules were unconsidered in the structure of 2. Several oxygen atoms of water molecules were disordered. Two disordered water molecules (O28 and O30) in the asymmetrical unit was refined with partial occupancy (0.5). Three water molecules including the coordinated water molecule indicated disordering at two positions(A and B sites).They were isotropically refined. The parts containing (O20A and O20B) were refined as the disordered water molecules,occupancy of which was fixed at 0.52 and 0.48. Also, the parts containing (O26A and O26B) were refined as the disordered water molecules, occupancy of which was fixed at 0.62 and 0.38. the parts containing (O29A and O29B) were refined as the disordered water molecules, occupancy of which was fixed at 0.70 and 0.30. ; _reflns_number_total 8439 _reflns_number_gt 7306 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1257 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8439 _refine_ls_number_parameters 461 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0604P)^2^+35.0181P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0080 _refine_diff_density_max 1.79 _refine_diff_density_min -1.92 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; La La -0.287 2.452 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 La(1) La 0.27683(2) 0.7500 0.833355(17) 0.01796(8) Uani 1.00 2 d S . . La(2) La 0.75083(3) 0.7500 1.02576(2) 0.02563(10) Uani 1.00 2 d S . . S(1) S 0.03311(7) 0.49391(4) 0.88460(6) 0.0217(2) Uani 1.00 1 d . . . S(2) S 0.39007(7) 0.50113(4) 0.76283(5) 0.0231(2) Uani 1.00 1 d . . . S(3) S 0.71709(8) 0.48140(4) 0.90059(6) 0.0272(2) Uani 1.00 1 d . . . S(4) S 0.13728(7) 0.65454(4) 0.72745(5) 0.0212(2) Uani 1.00 1 d . . . S(5) S 0.43653(7) 0.61368(4) 0.99684(5) 0.0220(2) Uani 1.00 1 d . . . S(6) S 0.91947(8) 0.65729(4) 0.93221(6) 0.0279(2) Uani 1.00 1 d . . . O(1) O 0.2273(2) 0.45559(12) 0.84644(17) 0.0269(6) Uani 1.00 1 d . . . O(2) O 0.5719(2) 0.46260(12) 0.79760(17) 0.0287(6) Uani 1.00 1 d . . . O(3) O 0.8143(2) 0.45440(11) 1.03163(16) 0.0248(6) Uani 1.00 1 d . . . O(4) O 0.0459(2) 0.66994(11) 0.75639(17) 0.0255(6) Uani 1.00 1 d . . . O(5) O 0.1350(2) 0.64764(13) 0.65423(16) 0.0328(7) Uani 1.00 1 d . . . O(6) O 0.2150(2) 0.68907(11) 0.74670(17) 0.0261(6) Uani 1.00 1 d . . . O(7) O 0.4697(2) 0.60101(12) 1.06467(17) 0.0293(6) Uani 1.00 1 d . . . O(8) O 0.3320(2) 0.61436(11) 0.99031(16) 0.0254(6) Uani 1.00 1 d . . . O(9) O 0.4767(2) 0.66177(12) 0.97249(17) 0.0281(6) Uani 1.00 1 d . . . O(10) O 0.8732(2) 0.69240(13) 0.9795(2) 0.0436(9) Uani 1.00 1 d . . . O(11) O 0.8847(3) 0.66194(14) 0.8632(2) 0.0446(9) Uani 1.00 1 d . . . O(12) O 1.0226(2) 0.66055(14) 0.9394(2) 0.0404(8) Uani 1.00 1 d . . . O(13) O 0.0925(3) 0.7500 0.8434(2) 0.0262(9) Uani 1.00 2 d S . . O(14) O 0.2139(2) 0.67650(14) 0.90642(19) 0.0354(8) Uani 1.00 1 d . . . O(15) O 0.3559(4) 0.7500 0.9560(3) 0.0383(11) Uani 1.00 2 d S . . O(16) O 0.4082(2) 0.81546(13) 0.83950(17) 0.0307(7) Uani 1.00 1 d . . . O(17) O 0.3794(3) 0.7500 0.7217(2) 0.0213(8) Uani 1.00 2 d S . . O(18) O 0.5698(5) 0.7500 1.0501(4) 0.077(2) Uani 1.00 2 d S . . O(19) O 0.7059(5) 0.7500 0.8983(3) 0.0456(13) Uani 1.00 2 d S . . O(20A) O 0.7108(8) 0.7013(3) 1.1319(4) 0.038(3) Uiso 0.48 1 d P . . O(20B) O 0.7505(8) 0.6861(4) 1.1249(4) 0.047(3) Uiso 0.52 1 d P . . O(21) O 0.6739(2) 0.83476(15) 0.9888(2) 0.0467(9) Uani 1.00 1 d . . . O(22) O 0.9015(5) 0.7500 1.1053(4) 0.0719(19) Uani 1.00 2 d S . . O(23) O 0.6222(2) 0.61205(13) 0.15577(18) 0.0340(7) Uani 1.00 1 d . . . O(24) O 0.7366(6) 0.7500 0.4320(4) 0.084(2) Uani 1.00 2 d S . . O(25) O 0.6064(5) 0.3658(2) 0.6736(3) 0.0913(18) Uani 1.00 1 d . . . O(26A) O 0.4294(8) 0.3822(5) 0.7015(5) 0.092(4) Uiso 0.62 1 d P . . O(26B) O 0.4062(9) 0.3524(6) 0.7094(6) 0.055(5) Uiso 0.38 1 d P . . O(27) O 0.3535(10) 0.2500 0.7465(7) 0.154(4) Uiso 1.00 2 d S . . O(28) O 0.7347(7) 0.6502(4) 0.3860(6) 0.073(2) Uiso 0.50 1 d P . . O(29A) O 0.6236(10) 0.3599(5) 0.8116(7) 0.143(6) Uiso 0.70 1 d P . . O(29B) O 0.7029(15) 0.3872(8) 0.7897(11) 0.087(8) Uiso 0.30 1 d P . . O(30) O 0.4764(11) 0.7341(6) 0.1683(7) 0.124(5) Uiso 0.50 1 d P . . O(31) O 0.5586(5) 0.7500 0.4819(4) 0.071(2) Uani 1.00 2 d S . . C(1) C 0.1650(2) 0.59563(15) 0.7651(2) 0.0196(7) Uani 1.00 1 d . . . C(2) C 0.2550(2) 0.57570(16) 0.7539(2) 0.0211(8) Uani 1.00 1 d . . . C(3) C 0.2771(2) 0.52806(16) 0.7806(2) 0.0206(8) Uani 1.00 1 d . . . C(4) C 0.2105(3) 0.50198(15) 0.8200(2) 0.0210(8) Uani 1.00 1 d . . . C(5) C 0.1213(3) 0.52451(16) 0.8342(2) 0.0206(8) Uani 1.00 1 d . . . C(6) C 0.0989(2) 0.57105(15) 0.8061(2) 0.0193(7) Uani 1.00 1 d . . . C(7) C 0.4789(3) 0.56661(16) 0.9400(2) 0.0223(8) Uani 1.00 1 d . . . C(8) C 0.5705(3) 0.54573(16) 0.9479(2) 0.0234(8) Uani 1.00 1 d . . . C(9) C 0.6032(2) 0.51152(16) 0.8996(2) 0.0226(8) Uani 1.00 1 d . . . C(10) C 0.5451(3) 0.49719(16) 0.8454(2) 0.0211(8) Uani 1.00 1 d . . . C(11) C 0.4542(3) 0.51901(16) 0.8372(2) 0.0228(8) Uani 1.00 1 d . . . C(12) C 0.4221(3) 0.55423(16) 0.8845(2) 0.0220(8) Uani 1.00 1 d . . . C(13) C 0.8866(3) 0.59660(15) 0.9604(2) 0.0225(8) Uani 1.00 1 d . . . C(14) C 0.9301(3) 0.57705(15) 1.0192(2) 0.0229(8) Uani 1.00 1 d . . . C(15) C 0.9041(2) 0.52941(15) 1.0433(2) 0.0203(8) Uani 1.00 1 d . . . C(16) C 0.8348(2) 0.50096(15) 1.0080(2) 0.0200(8) Uani 1.00 1 d . . . C(17) C 0.7920(2) 0.52160(16) 0.9498(2) 0.0224(8) Uani 1.00 1 d . . . C(18) C 0.8174(3) 0.56926(16) 0.9266(2) 0.0242(8) Uani 1.00 1 d . . . H(1) H 0.2808 0.4451 0.8328 0.032 Uiso 1.00 1 c R . . H(2) H 0.6229 0.4485 0.8100 0.034 Uiso 1.00 1 c R . . H(3) H 0.7675 0.4426 1.0100 0.030 Uiso 1.00 1 c R . . H(4) H 0.3012 0.5940 0.7283 0.025 Uiso 1.00 1 c R . . H(5) H 0.0384 0.5861 0.8148 0.023 Uiso 1.00 1 c R . . H(6) H 0.6094 0.5549 0.9856 0.028 Uiso 1.00 1 c R . . H(7) H 0.3613 0.5698 0.8788 0.026 Uiso 1.00 1 c R . . H(8) H 0.9772 0.5962 1.0426 0.027 Uiso 1.00 1 c R . . H(9) H 0.7871 0.5831 0.8874 0.029 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 La(1) 0.01224(15) 0.01864(16) 0.02300(18) 0.0000 0.00088(12) 0.0000 La(2) 0.02412(19) 0.02625(19) 0.0265(2) 0.0000 0.00128(14) 0.0000 S(1) 0.0171(4) 0.0224(4) 0.0257(5) -0.0009(3) 0.0004(3) 0.0060(3) S(2) 0.0172(4) 0.0294(5) 0.0226(5) 0.0026(3) 0.0015(3) -0.0012(4) S(3) 0.0222(5) 0.0259(5) 0.0336(6) 0.0058(4) -0.0062(4) -0.0004(4) S(4) 0.0219(4) 0.0181(4) 0.0237(5) -0.0006(3) -0.0028(3) 0.0034(3) S(5) 0.0206(4) 0.0221(4) 0.0234(5) -0.0002(3) -0.0010(3) 0.0021(3) S(6) 0.0261(5) 0.0212(4) 0.0365(6) 0.0010(4) 0.0071(4) 0.0103(4) O(1) 0.0238(15) 0.0219(15) 0.0350(18) 0.0047(12) 0.0069(13) 0.0072(12) O(2) 0.0244(16) 0.0311(16) 0.0306(17) 0.0055(13) 0.0005(13) 0.0004(13) O(3) 0.0235(15) 0.0203(14) 0.0306(16) -0.0030(11) -0.0054(12) 0.0073(12) O(4) 0.0210(14) 0.0234(14) 0.0320(17) 0.0013(11) -0.0034(12) 0.0043(12) O(5) 0.0412(19) 0.0330(17) 0.0242(17) 0.0021(15) -0.0043(14) 0.0047(13) O(6) 0.0231(15) 0.0176(13) 0.0374(18) -0.0029(11) -0.0018(13) 0.0015(12) O(7) 0.0300(16) 0.0306(16) 0.0271(16) 0.0004(13) -0.0030(13) 0.0031(13) O(8) 0.0218(15) 0.0256(15) 0.0287(16) 0.0016(12) 0.0005(12) 0.0010(12) O(9) 0.0310(16) 0.0235(15) 0.0298(17) -0.0029(12) 0.0006(13) 0.0013(12) O(10) 0.045(2) 0.0214(16) 0.064(2) 0.0037(15) 0.0175(19) 0.0046(16) O(11) 0.054(2) 0.0365(19) 0.044(2) -0.0070(17) -0.0036(18) 0.0200(16) O(12) 0.0277(17) 0.0334(18) 0.060(2) -0.0072(14) 0.0091(16) 0.0122(17) O(13) 0.018(2) 0.024(2) 0.037(2) 0.0000 0.0014(18) 0.0000 O(14) 0.0218(15) 0.0400(19) 0.044(2) 0.0006(14) 0.0061(14) 0.0191(16) O(15) 0.042(2) 0.043(2) 0.030(2) 0.0000 -0.005(2) 0.0000 O(16) 0.0219(15) 0.0374(18) 0.0327(18) -0.0095(13) 0.0054(13) -0.0092(14) O(17) 0.021(2) 0.0199(19) 0.023(2) 0.0000 0.0012(16) 0.0000 O(18) 0.052(3) 0.115(4) 0.064(3) 0.0000 0.005(2) 0.0000 O(19) 0.068(3) 0.033(2) 0.036(2) 0.0000 -0.014(2) 0.0000 O(21) 0.041(2) 0.043(2) 0.057(2) 0.0206(17) -0.0103(18) -0.0060(18) O(22) 0.049(3) 0.113(4) 0.054(3) 0.0000 -0.009(2) 0.0000 O(23) 0.0307(16) 0.0330(16) 0.0382(18) 0.0046(13) -0.0007(13) 0.0047(13) O(24) 0.1(2) 0.0836 0.0836 0.0000 0.0000 0.0000 O(25) 0.09(15) 0.0913 0.0913 0.0000 0.0000 0.0000 O(31) 0.07(16) 0.0709 0.0709 0.0000 0.0000 0.0000 C(1) 0.0215(19) 0.0187(17) 0.0187(19) -0.0001(15) -0.0036(15) 0.0024(14) C(2) 0.0203(19) 0.0222(19) 0.021(2) -0.0024(15) -0.0021(15) 0.0018(16) C(3) 0.0170(18) 0.0245(19) 0.0205(19) 0.0033(15) -0.0011(15) -0.0012(15) C(4) 0.025(2) 0.0179(18) 0.020(2) 0.0007(15) -0.0013(16) 0.0028(15) C(5) 0.0186(19) 0.0227(19) 0.0206(19) -0.0021(15) 0.0025(15) 0.0007(15) C(6) 0.0185(18) 0.0197(18) 0.0197(19) -0.0010(14) -0.0024(15) -0.0009(15) C(7) 0.0208(19) 0.0217(19) 0.024(2) -0.0010(15) 0.0022(16) 0.0033(15) C(8) 0.022(2) 0.0233(19) 0.025(2) -0.0022(16) -0.0032(16) 0.0053(16) C(9) 0.0185(19) 0.0230(19) 0.026(2) 0.0013(15) -0.0001(16) 0.0088(16) C(10) 0.0202(19) 0.0216(19) 0.022(2) 0.0012(15) 0.0041(15) 0.0040(15) C(11) 0.021(2) 0.026(2) 0.021(2) -0.0027(16) -0.0006(16) 0.0047(16) C(12) 0.0185(18) 0.0224(19) 0.025(2) -0.0002(15) -0.0006(15) 0.0041(16) C(13) 0.0198(19) 0.0191(18) 0.029(2) 0.0036(15) 0.0065(16) 0.0069(16) C(14) 0.0190(19) 0.0200(19) 0.030(2) 0.0009(15) 0.0044(16) 0.0031(16) C(15) 0.0168(18) 0.0193(18) 0.025(2) 0.0036(14) 0.0028(15) 0.0046(15) C(16) 0.0159(18) 0.0196(18) 0.025(2) 0.0033(14) 0.0031(15) 0.0041(15) C(17) 0.0161(19) 0.024(2) 0.027(2) 0.0031(15) 0.0019(16) 0.0027(16) C(18) 0.022(2) 0.025(2) 0.026(2) 0.0072(16) 0.0032(16) 0.0062(16) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _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_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 La(1) O(6) 2.495(3) yes . . La(1) O(6) 2.495(3) yes . 3_565 La(1) O(13) 2.583(4) yes . . La(1) O(14) 2.570(3) yes . . La(1) O(14) 2.570(3) yes . 3_565 La(1) O(15) 2.643(5) yes . . La(1) O(16) 2.527(3) yes . . La(1) O(16) 2.527(3) yes . 3_565 La(1) O(17) 2.614(4) yes . . La(2) O(10) 2.463(3) yes . . La(2) O(10) 2.463(3) yes . 3_565 La(2) O(18) 2.574(7) yes . . La(2) O(19) 2.574(5) yes . . La(2) O(20A) 2.509(8) yes . . La(2) O(20A) 2.509(8) yes . 3_565 La(2) O(20B) 2.576(9) yes . . La(2) O(20B) 2.576(9) yes . 3_565 La(2) O(21) 2.590(3) yes . . La(2) O(21) 2.590(3) yes . 3_565 La(2) O(22) 2.619(7) yes . . S(1) C(5) 1.774(4) yes . . S(1) C(15) 1.772(4) yes . 5_667 S(2) C(3) 1.767(4) yes . . S(2) C(11) 1.774(4) yes . . S(3) C(9) 1.780(4) yes . . S(3) C(17) 1.776(4) yes . . S(4) O(4) 1.455(3) yes . . S(4) O(5) 1.446(3) yes . . S(4) O(6) 1.468(3) yes . . S(4) C(1) 1.767(4) yes . . S(5) O(7) 1.446(3) yes . . S(5) O(8) 1.466(3) yes . . S(5) O(9) 1.470(3) yes . . S(5) C(7) 1.772(4) yes . . S(6) O(10) 1.462(4) yes . . S(6) O(11) 1.441(4) yes . . S(6) O(12) 1.450(3) yes . . S(6) C(13) 1.759(4) yes . . O(1) C(4) 1.353(5) yes . . O(2) C(10) 1.361(5) yes . . O(3) C(16) 1.347(4) yes . . O(20A) O(20B) 0.699(15) yes . . O(26A) O(26B) 0.87(2) yes . . O(29A) O(29B) 1.39(2) yes . . O(30) O(30) 0.84(2) yes . 3_565 C(1) C(2) 1.381(5) yes . . C(1) C(6) 1.386(5) yes . . C(2) C(3) 1.400(5) yes . . C(3) C(4) 1.392(5) yes . . C(4) C(5) 1.409(5) yes . . C(5) C(6) 1.385(5) yes . . C(7) C(8) 1.402(5) yes . . C(7) C(12) 1.386(6) yes . . C(8) C(9) 1.386(6) yes . . C(9) C(10) 1.390(5) yes . . C(10) C(11) 1.403(6) yes . . C(11) C(12) 1.389(6) yes . . C(13) C(14) 1.400(6) yes . . C(13) C(18) 1.377(5) yes . . C(14) C(15) 1.394(5) yes . . C(15) C(16) 1.408(5) yes . . C(16) C(17) 1.398(6) yes . . C(17) C(18) 1.386(6) yes . . O(1) H(1) 0.840 no . . O(2) H(2) 0.840 no . . O(3) H(3) 0.840 no . . C(2) H(4) 0.950 no . . C(6) H(5) 0.950 no . . C(8) H(6) 0.950 no . . C(12) H(7) 0.950 no . . C(14) H(8) 0.950 no . . C(18) H(9) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(6) La(1) O(6) 80.51(10) yes . . 3_565 O(6) La(1) O(13) 72.93(9) yes . . . O(6) La(1) O(14) 76.76(10) yes . . . O(6) La(1) O(14) 138.52(10) yes . . 3_565 O(6) La(1) O(15) 139.69(7) yes . . . O(6) La(1) O(16) 136.63(10) yes . . . O(6) La(1) O(16) 80.86(10) yes . . 3_565 O(6) La(1) O(17) 67.74(9) yes . . . O(6) La(1) O(13) 72.93(9) yes 3_565 . . O(6) La(1) O(14) 138.52(10) yes 3_565 . . O(6) La(1) O(14) 76.76(10) yes 3_565 . 3_565 O(6) La(1) O(15) 139.69(7) yes 3_565 . . O(6) La(1) O(16) 80.86(10) yes 3_565 . . O(6) La(1) O(16) 136.63(10) yes 3_565 . 3_565 O(6) La(1) O(17) 67.74(9) yes 3_565 . . O(13) La(1) O(14) 67.44(8) yes . . . O(13) La(1) O(14) 67.44(8) yes . . 3_565 O(13) La(1) O(15) 110.34(15) yes . . . O(13) La(1) O(16) 136.13(7) yes . . . O(13) La(1) O(16) 136.13(7) yes . . 3_565 O(13) La(1) O(17) 127.61(12) yes . . . O(14) La(1) O(14) 98.38(11) yes . . 3_565 O(14) La(1) O(15) 68.73(10) yes . . . O(14) La(1) O(16) 137.81(10) yes . . . O(14) La(1) O(16) 72.74(10) yes . . 3_565 O(14) La(1) O(17) 130.79(8) yes . . . O(14) La(1) O(15) 68.73(10) yes 3_565 . . O(14) La(1) O(16) 72.74(10) yes 3_565 . . O(14) La(1) O(16) 137.81(10) yes 3_565 . 3_565 O(14) La(1) O(17) 130.79(8) yes 3_565 . . O(15) La(1) O(16) 69.70(11) yes . . . O(15) La(1) O(16) 69.70(11) yes . . 3_565 O(15) La(1) O(17) 122.05(15) yes . . . O(16) La(1) O(16) 86.53(10) yes . . 3_565 O(16) La(1) O(17) 68.99(9) yes . . . O(16) La(1) O(17) 68.99(9) yes 3_565 . . O(10) La(2) O(10) 76.46(12) yes . . 3_565 O(10) La(2) O(18) 138.61(10) yes . . . O(10) La(2) O(19) 79.20(15) yes . . . O(10) La(2) O(20A) 98.1(2) yes . . . O(10) La(2) O(20A) 141.0(2) yes . . 3_565 O(10) La(2) O(20B) 82.7(2) yes . . . O(10) La(2) O(20B) 133.3(2) yes . . 3_565 O(10) La(2) O(21) 136.15(13) yes . . . O(10) La(2) O(21) 69.48(12) yes . . 3_565 O(10) La(2) O(22) 70.17(15) yes . . . O(10) La(2) O(18) 138.61(10) yes 3_565 . . O(10) La(2) O(19) 79.20(15) yes 3_565 . . O(10) La(2) O(20A) 141.0(2) yes 3_565 . . O(10) La(2) O(20A) 98.1(2) yes 3_565 . 3_565 O(10) La(2) O(20B) 133.3(2) yes 3_565 . . O(10) La(2) O(20B) 82.7(2) yes 3_565 . 3_565 O(10) La(2) O(21) 69.48(12) yes 3_565 . . O(10) La(2) O(21) 136.15(13) yes 3_565 . 3_565 O(10) La(2) O(22) 70.17(15) yes 3_565 . . O(18) La(2) O(19) 86.6(2) yes . . . O(18) La(2) O(20A) 68.1(2) yes . . . O(18) La(2) O(20A) 68.1(2) yes . . 3_565 O(18) La(2) O(20B) 81.9(2) yes . . . O(18) La(2) O(20B) 81.9(2) yes . . 3_565 O(18) La(2) O(21) 69.14(10) yes . . . O(18) La(2) O(21) 69.14(10) yes . . 3_565 O(18) La(2) O(22) 132.8(2) yes . . . O(19) La(2) O(20A) 138.5(2) yes . . . O(19) La(2) O(20A) 138.5(2) yes . . 3_565 O(19) La(2) O(20B) 136.9(2) yes . . . O(19) La(2) O(20B) 136.9(2) yes . . 3_565 O(19) La(2) O(21) 68.17(10) yes . . . O(19) La(2) O(21) 68.17(10) yes . . 3_565 O(19) La(2) O(22) 140.6(2) yes . . . O(20A) La(2) O(20A) 61.8(3) yes . . 3_565 O(20A) La(2) O(20B) 15.7(3) yes . . . O(20A) La(2) O(20B) 73.3(3) yes . . 3_565 O(20A) La(2) O(21) 125.7(2) yes . . . O(20A) La(2) O(21) 72.2(2) yes . . 3_565 O(20A) La(2) O(22) 71.7(2) yes . . . O(20A) La(2) O(20B) 73.3(3) yes 3_565 . . O(20A) La(2) O(20B) 15.7(3) yes 3_565 . 3_565 O(20A) La(2) O(21) 72.2(2) yes 3_565 . . O(20A) La(2) O(21) 125.7(2) yes 3_565 . 3_565 O(20A) La(2) O(22) 71.7(2) yes 3_565 . . O(20B) La(2) O(20B) 82.1(3) yes . . 3_565 O(20B) La(2) O(21) 141.1(2) yes . . . O(20B) La(2) O(21) 68.9(2) yes . . 3_565 O(20B) La(2) O(22) 63.5(2) yes . . . O(20B) La(2) O(21) 68.9(2) yes 3_565 . . O(20B) La(2) O(21) 141.1(2) yes 3_565 . 3_565 O(20B) La(2) O(22) 63.5(2) yes 3_565 . . O(21) La(2) O(21) 119.99(12) yes . . 3_565 O(21) La(2) O(22) 119.97(8) yes . . . O(21) La(2) O(22) 119.97(8) yes 3_565 . . C(5) S(1) C(15) 104.95(19) yes . . 5_667 C(3) S(2) C(11) 100.5(2) yes . . . C(9) S(3) C(17) 105.34(19) yes . . . O(4) S(4) O(5) 113.7(2) yes . . . O(4) S(4) O(6) 112.00(18) yes . . . O(4) S(4) C(1) 106.09(18) yes . . . O(5) S(4) O(6) 110.5(2) yes . . . O(5) S(4) C(1) 107.89(19) yes . . . O(6) S(4) C(1) 106.23(18) yes . . . O(7) S(5) O(8) 113.70(18) yes . . . O(7) S(5) O(9) 112.11(19) yes . . . O(7) S(5) C(7) 107.86(19) yes . . . O(8) S(5) O(9) 109.95(18) yes . . . O(8) S(5) C(7) 106.65(18) yes . . . O(9) S(5) C(7) 106.11(19) yes . . . O(10) S(6) O(11) 112.9(2) yes . . . O(10) S(6) O(12) 109.9(2) yes . . . O(10) S(6) C(13) 105.4(2) yes . . . O(11) S(6) O(12) 114.9(2) yes . . . O(11) S(6) C(13) 106.5(2) yes . . . O(12) S(6) C(13) 106.5(2) yes . . . La(1) O(6) S(4) 146.39(19) yes . . . La(2) O(10) S(6) 158.9(2) yes . . . La(2) O(20A) O(20B) 87.6(10) yes . . . La(2) O(20B) O(20A) 76.7(10) yes . . . S(4) C(1) C(2) 118.1(3) yes . . . S(4) C(1) C(6) 120.6(3) yes . . . C(2) C(1) C(6) 121.3(3) yes . . . C(1) C(2) C(3) 119.0(3) yes . . . S(2) C(3) C(2) 119.1(3) yes . . . S(2) C(3) C(4) 120.5(3) yes . . . C(2) C(3) C(4) 120.5(3) yes . . . O(1) C(4) C(3) 123.1(3) yes . . . O(1) C(4) C(5) 117.6(3) yes . . . C(3) C(4) C(5) 119.4(3) yes . . . S(1) C(5) C(4) 122.1(3) yes . . . S(1) C(5) C(6) 118.1(3) yes . . . C(4) C(5) C(6) 119.8(3) yes . . . C(1) C(6) C(5) 119.8(3) yes . . . S(5) C(7) C(8) 120.9(3) yes . . . S(5) C(7) C(12) 117.9(3) yes . . . C(8) C(7) C(12) 121.0(3) yes . . . C(7) C(8) C(9) 119.0(3) yes . . . S(3) C(9) C(8) 125.5(3) yes . . . S(3) C(9) C(10) 114.1(3) yes . . . C(8) C(9) C(10) 120.4(3) yes . . . O(2) C(10) C(9) 123.2(3) yes . . . O(2) C(10) C(11) 116.5(3) yes . . . C(9) C(10) C(11) 120.3(3) yes . . . S(2) C(11) C(10) 116.2(3) yes . . . S(2) C(11) C(12) 124.3(3) yes . . . C(10) C(11) C(12) 119.5(3) yes . . . C(7) C(12) C(11) 119.8(3) yes . . . S(6) C(13) C(14) 118.8(3) yes . . . S(6) C(13) C(18) 120.8(3) yes . . . C(14) C(13) C(18) 120.4(3) yes . . . C(13) C(14) C(15) 120.0(3) yes . . . S(1) C(15) C(14) 117.1(3) yes 5_667 . . S(1) C(15) C(16) 123.1(3) yes 5_667 . . C(14) C(15) C(16) 119.7(3) yes . . . O(3) C(16) C(15) 117.8(3) yes . . . O(3) C(16) C(17) 123.1(3) yes . . . C(15) C(16) C(17) 119.1(3) yes . . . S(3) C(17) C(16) 117.4(3) yes . . . S(3) C(17) C(18) 121.2(3) yes . . . C(16) C(17) C(18) 120.8(3) yes . . . C(13) C(18) C(17) 120.1(4) yes . . . C(4) O(1) H(1) 109.5 no . . . C(10) O(2) H(2) 109.5 no . . . C(16) O(3) H(3) 109.5 no . . . C(1) C(2) H(4) 120.5 no . . . C(3) C(2) H(4) 120.5 no . . . C(1) C(6) H(5) 120.1 no . . . C(5) C(6) H(5) 120.1 no . . . C(7) C(8) H(6) 120.5 no . . . C(9) C(8) H(6) 120.5 no . . . C(7) C(12) H(7) 120.1 no . . . C(11) C(12) H(7) 120.1 no . . . C(13) C(14) H(8) 120.0 no . . . C(15) C(14) H(8) 120.0 no . . . C(13) C(18) H(9) 120.0 no . . . C(17) C(18) H(9) 120.0 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(6) La(1) O(6) S(4) 101.5(3) ? . . 3_565 3_565 O(6) La(1) O(6) S(4) -101.5(3) ? 3_565 . . . O(13) La(1) O(6) S(4) -26.6(3) ? . . . . O(14) La(1) O(6) S(4) 43.6(3) ? . . . . O(14) La(1) O(6) S(4) -44.1(4) ? 3_565 . . . O(15) La(1) O(6) S(4) 75.0(4) ? . . . . O(16) La(1) O(6) S(4) -167.2(2) ? . . . . O(16) La(1) O(6) S(4) 117.8(3) ? 3_565 . . . O(17) La(1) O(6) S(4) -171.2(3) ? . . . . O(13) La(1) O(6) S(4) 26.6(3) ? . . 3_565 3_565 O(14) La(1) O(6) S(4) 44.1(4) ? . . 3_565 3_565 O(14) La(1) O(6) S(4) -43.6(3) ? 3_565 . 3_565 3_565 O(15) La(1) O(6) S(4) -75.0(4) ? . . 3_565 3_565 O(16) La(1) O(6) S(4) -117.8(3) ? . . 3_565 3_565 O(16) La(1) O(6) S(4) 167.2(2) ? 3_565 . 3_565 3_565 O(17) La(1) O(6) S(4) 171.2(3) ? . . 3_565 3_565 O(10) La(2) O(10) S(6) 101.8(6) ? . . 3_565 3_565 O(10) La(2) O(10) S(6) -101.8(6) ? 3_565 . . . O(18) La(2) O(10) S(6) 51.5(7) ? . . . . O(19) La(2) O(10) S(6) -20.5(6) ? . . . . O(10) La(2) O(20A) O(20B) 10.2(12) ? . . . . O(20A) La(2) O(10) S(6) 117.5(6) ? . . . . O(10) La(2) O(20A) O(20B) 68.3(12) ? . . 3_565 3_565 O(20A) La(2) O(10) S(6) 172.0(6) ? 3_565 . . . O(10) La(2) O(20B) O(20A) -169.8(12) ? . . . . O(20B) La(2) O(10) S(6) 120.3(6) ? . . . . O(10) La(2) O(20B) O(20A) -126.6(11) ? . . 3_565 3_565 O(20B) La(2) O(10) S(6) -167.8(6) ? 3_565 . . . O(21) La(2) O(10) S(6) -62.3(6) ? . . . . O(21) La(2) O(10) S(6) 50.1(6) ? 3_565 . . . O(22) La(2) O(10) S(6) -175.3(6) ? . . . . O(18) La(2) O(10) S(6) -51.5(7) ? . . 3_565 3_565 O(19) La(2) O(10) S(6) 20.5(6) ? . . 3_565 3_565 O(10) La(2) O(20A) O(20B) -68.3(12) ? 3_565 . . . O(20A) La(2) O(10) S(6) -172.0(6) ? . . 3_565 3_565 O(10) La(2) O(20A) O(20B) -10.2(12) ? 3_565 . 3_565 3_565 O(20A) La(2) O(10) S(6) -117.5(6) ? 3_565 . 3_565 3_565 O(10) La(2) O(20B) O(20A) 126.6(11) ? 3_565 . . . O(20B) La(2) O(10) S(6) 167.8(6) ? . . 3_565 3_565 O(10) La(2) O(20B) O(20A) 169.8(12) ? 3_565 . 3_565 3_565 O(20B) La(2) O(10) S(6) -120.3(6) ? 3_565 . 3_565 3_565 O(21) La(2) O(10) S(6) -50.1(6) ? . . 3_565 3_565 O(21) La(2) O(10) S(6) 62.3(6) ? 3_565 . 3_565 3_565 O(22) La(2) O(10) S(6) 175.3(6) ? . . 3_565 3_565 O(18) La(2) O(20A) O(20B) 149.6(12) ? . . . . O(18) La(2) O(20A) O(20B) -149.6(12) ? . . 3_565 3_565 O(18) La(2) O(20B) O(20A) -28.4(11) ? . . . . O(18) La(2) O(20B) O(20A) 28.4(11) ? . . 3_565 3_565 O(19) La(2) O(20A) O(20B) 93.1(12) ? . . . . O(19) La(2) O(20A) O(20B) -93.1(12) ? . . 3_565 3_565 O(19) La(2) O(20B) O(20A) -104.4(11) ? . . . . O(19) La(2) O(20B) O(20A) 104.4(11) ? . . 3_565 3_565 O(20A) La(2) O(20A) O(20B) 134.3(12) ? . . 3_565 3_565 O(20A) La(2) O(20A) O(20B) -134.3(12) ? 3_565 . . . O(20A) La(2) O(20B) O(20A) -41.2(11) ? . . 3_565 3_565 O(20B) La(2) O(20A) O(20B) -122.7(12) ? 3_565 . . . O(21) La(2) O(20A) O(20B) -170.0(10) ? . . . . O(21) La(2) O(20A) O(20B) 75.5(11) ? 3_565 . . . O(22) La(2) O(20A) O(20B) -55.7(11) ? . . . . O(20A) La(2) O(20B) O(20A) 41.2(11) ? 3_565 . . . O(20B) La(2) O(20A) O(20B) 122.7(12) ? . . 3_565 3_565 O(21) La(2) O(20A) O(20B) -75.5(11) ? . . 3_565 3_565 O(21) La(2) O(20A) O(20B) 170.0(10) ? 3_565 . 3_565 3_565 O(22) La(2) O(20A) O(20B) 55.7(11) ? . . 3_565 3_565 O(20B) La(2) O(20B) O(20A) -54.5(12) ? . . 3_565 3_565 O(20B) La(2) O(20B) O(20A) 54.5(12) ? 3_565 . . . O(21) La(2) O(20B) O(20A) 13.0(14) ? . . . . O(21) La(2) O(20B) O(20A) -99.1(12) ? 3_565 . . . O(22) La(2) O(20B) O(20A) 118.7(12) ? . . . . O(21) La(2) O(20B) O(20A) 99.1(12) ? . . 3_565 3_565 O(21) La(2) O(20B) O(20A) -13.0(14) ? 3_565 . 3_565 3_565 O(22) La(2) O(20B) O(20A) -118.7(12) ? . . 3_565 3_565 C(5) S(1) C(15) C(14) -140.6(3) ? . . 5_667 5_667 C(5) S(1) C(15) C(16) 43.3(4) ? . . 5_667 5_667 C(15) S(1) C(5) C(4) 46.4(3) ? 5_667 . . . C(15) S(1) C(5) C(6) -136.3(3) ? 5_667 . . . C(3) S(2) C(11) C(10) 170.8(3) ? . . . . C(3) S(2) C(11) C(12) -12.4(4) ? . . . . C(11) S(2) C(3) C(2) 96.0(3) ? . . . . C(11) S(2) C(3) C(4) -84.8(3) ? . . . . C(9) S(3) C(17) C(16) 121.3(3) ? . . . . C(9) S(3) C(17) C(18) -67.3(3) ? . . . . C(17) S(3) C(9) C(8) -23.6(4) ? . . . . C(17) S(3) C(9) C(10) 157.7(3) ? . . . . O(4) S(4) O(6) La(1) 27.8(3) ? . . . . O(4) S(4) C(1) C(2) -171.0(3) ? . . . . O(4) S(4) C(1) C(6) 7.4(3) ? . . . . O(5) S(4) O(6) La(1) 155.7(3) ? . . . . O(5) S(4) C(1) C(2) 66.8(3) ? . . . . O(5) S(4) C(1) C(6) -114.8(3) ? . . . . O(6) S(4) C(1) C(2) -51.6(3) ? . . . . O(6) S(4) C(1) C(6) 126.7(3) ? . . . . C(1) S(4) O(6) La(1) -87.6(3) ? . . . . O(7) S(5) C(7) C(8) -38.3(4) ? . . . . O(7) S(5) C(7) C(12) 147.1(3) ? . . . . O(8) S(5) C(7) C(8) -160.8(3) ? . . . . O(8) S(5) C(7) C(12) 24.6(3) ? . . . . O(9) S(5) C(7) C(8) 82.0(3) ? . . . . O(9) S(5) C(7) C(12) -92.6(3) ? . . . . O(11) S(6) O(10) La(2) 22.5(7) ? . . . . O(12) S(6) O(10) La(2) 152.3(5) ? . . . . O(10) S(6) C(13) C(14) -74.8(3) ? . . . . O(10) S(6) C(13) C(18) 103.4(3) ? . . . . C(13) S(6) O(10) La(2) -93.4(6) ? . . . . O(11) S(6) C(13) C(14) 165.0(3) ? . . . . O(11) S(6) C(13) C(18) -16.8(4) ? . . . . O(12) S(6) C(13) C(14) 41.9(4) ? . . . . O(12) S(6) C(13) C(18) -139.9(3) ? . . . . S(4) C(1) C(2) C(3) -177.2(3) ? . . . . S(4) C(1) C(6) C(5) 178.9(3) ? . . . . C(2) C(1) C(6) C(5) -2.8(6) ? . . . . C(6) C(1) C(2) C(3) 4.5(6) ? . . . . C(1) C(2) C(3) S(2) 176.9(3) ? . . . . C(1) C(2) C(3) C(4) -2.3(6) ? . . . . S(2) C(3) C(4) O(1) -0.1(4) ? . . . . S(2) C(3) C(4) C(5) 179.2(3) ? . . . . C(2) C(3) C(4) O(1) 179.1(3) ? . . . . C(2) C(3) C(4) C(5) -1.6(6) ? . . . . O(1) C(4) C(5) S(1) -0.1(4) ? . . . . O(1) C(4) C(5) C(6) -177.3(3) ? . . . . C(3) C(4) C(5) S(1) -179.5(3) ? . . . . C(3) C(4) C(5) C(6) 3.3(6) ? . . . . S(1) C(5) C(6) C(1) -178.5(3) ? . . . . C(4) C(5) C(6) C(1) -1.2(6) ? . . . . S(5) C(7) C(8) C(9) -175.7(3) ? . . . . S(5) C(7) C(12) C(11) 177.4(3) ? . . . . C(8) C(7) C(12) C(11) 2.8(6) ? . . . . C(12) C(7) C(8) C(9) -1.2(6) ? . . . . C(7) C(8) C(9) S(3) 179.7(3) ? . . . . C(7) C(8) C(9) C(10) -1.7(6) ? . . . . S(3) C(9) C(10) O(2) 0.9(5) ? . . . . S(3) C(9) C(10) C(11) -178.2(3) ? . . . . C(8) C(9) C(10) O(2) -177.8(3) ? . . . . C(8) C(9) C(10) C(11) 3.0(6) ? . . . . O(2) C(10) C(11) S(2) -3.6(5) ? . . . . O(2) C(10) C(11) C(12) 179.4(3) ? . . . . C(9) C(10) C(11) S(2) 175.7(3) ? . . . . C(9) C(10) C(11) C(12) -1.4(6) ? . . . . S(2) C(11) C(12) C(7) -178.2(3) ? . . . . C(10) C(11) C(12) C(7) -1.4(6) ? . . . . S(6) C(13) C(14) C(15) 178.9(3) ? . . . . S(6) C(13) C(18) C(17) -179.6(3) ? . . . . C(14) C(13) C(18) C(17) -1.5(6) ? . . . . C(18) C(13) C(14) C(15) 0.7(6) ? . . . . C(13) C(14) C(15) S(1) 176.8(3) ? . . . 5_667 C(13) C(14) C(15) C(16) 0.6(6) ? . . . . S(1) C(15) C(16) O(3) 1.7(5) ? 5_667 . . . S(1) C(15) C(16) C(17) -177.1(3) ? 5_667 . . . C(14) C(15) C(16) O(3) 177.6(3) ? . . . . C(14) C(15) C(16) C(17) -1.2(6) ? . . . . O(3) C(16) C(17) S(3) -6.8(5) ? . . . . O(3) C(16) C(17) C(18) -178.3(3) ? . . . . C(15) C(16) C(17) S(3) 171.9(3) ? . . . . C(15) C(16) C(17) C(18) 0.4(6) ? . . . . S(3) C(17) C(18) C(13) -170.2(3) ? . . . . C(16) C(17) C(18) C(13) 0.9(6) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S(1) S(2) 3.5164(14) ? . 8_456 S(2) S(1) 3.5164(14) ? . 8_556 S(2) O(23) 3.397(3) ? . 5_666 S(2) O(26A) 3.414(14) ? . . S(3) O(28) 3.559(11) ? . 4_665 S(3) O(29B) 3.31(2) ? . . S(4) O(16) 3.548(3) ? . 6_466 S(6) O(31) 3.553(5) ? . 6_566 O(1) O(2) 3.565(4) ? . 8_456 O(1) O(23) 2.761(4) ? . 5_666 O(1) O(25) 2.941(7) ? . 8_456 O(1) O(29B) 3.24(2) ? . 8_456 O(2) O(1) 3.565(4) ? . 8_556 O(2) O(23) 3.477(4) ? . 5_666 O(2) O(25) 3.561(7) ? . . O(2) O(26A) 3.470(13) ? . . O(2) O(29A) 2.825(14) ? . . O(2) O(29B) 2.71(2) ? . . O(2) C(4) 3.185(5) ? . 8_556 O(2) C(5) 3.134(5) ? . 8_556 O(2) C(6) 3.535(5) ? . 8_556 O(4) O(11) 3.082(5) ? . 1_455 O(4) O(16) 2.716(4) ? . 6_466 O(4) O(17) 3.176(4) ? . 6_466 O(5) O(9) 3.345(4) ? . 8_456 O(5) O(11) 3.526(5) ? . 8_456 O(5) O(16) 3.317(4) ? . 6_466 O(5) O(19) 3.062(4) ? . 6_466 O(5) O(21) 2.892(5) ? . 6_466 O(5) C(7) 3.572(5) ? . 8_456 O(5) C(8) 3.476(5) ? . 8_456 O(6) O(11) 3.282(5) ? . 8_456 O(6) O(19) 3.268(6) ? . 6_466 O(7) O(23) 2.795(4) ? . 1_556 O(7) O(29A) 2.939(14) ? . 5_667 O(8) O(28) 2.935(11) ? . 8_456 O(9) O(5) 3.345(4) ? . 8_556 O(10) O(31) 3.099(8) ? . 6_566 O(11) O(4) 3.082(5) ? . 1_655 O(11) O(5) 3.526(5) ? . 8_556 O(11) O(6) 3.282(5) ? . 8_556 O(11) O(17) 2.864(4) ? . 6_566 O(12) O(13) 3.176(4) ? . 1_655 O(12) O(14) 2.782(4) ? . 1_655 O(12) O(31) 2.869(5) ? . 6_566 O(13) O(12) 3.176(4) ? . 1_455 O(13) O(12) 3.176(4) ? . 3_465 O(13) O(17) 3.239(5) ? . 6_466 O(13) O(31) 3.454(8) ? . 6_466 O(14) O(12) 2.782(4) ? . 1_455 O(15) O(24) 2.755(10) ? . 6_466 O(16) S(4) 3.548(3) ? . 6_566 O(16) O(4) 2.716(4) ? . 6_566 O(16) O(5) 3.317(4) ? . 6_566 O(17) O(4) 3.176(4) ? . 6_566 O(17) O(4) 3.176(4) ? . 8_556 O(17) O(11) 2.864(4) ? . 6_466 O(17) O(11) 2.864(4) ? . 8_456 O(17) O(13) 3.239(5) ? . 6_566 O(17) O(19) 3.376(7) ? . 6_466 O(18) O(30) 2.691(16) ? . 1_556 O(18) O(30) 2.691(16) ? . 3_566 O(19) O(5) 3.062(4) ? . 6_566 O(19) O(5) 3.062(4) ? . 8_556 O(19) O(6) 3.268(6) ? . 6_566 O(19) O(6) 3.268(6) ? . 8_556 O(19) O(17) 3.376(7) ? . 6_566 O(20A) O(23) 2.707(10) ? . 1_556 O(20A) O(25) 3.217(12) ? . 4_665 O(20A) O(27) 2.851(16) ? . 5_667 O(20A) O(30) 3.464(19) ? . 1_556 O(20B) O(23) 2.722(11) ? . 1_556 O(20B) O(25) 2.607(13) ? . 4_665 O(20B) O(27) 3.363(16) ? . 5_667 O(21) O(5) 2.892(5) ? . 6_566 O(22) O(25) 3.346(7) ? . 2_655 O(22) O(25) 3.346(7) ? . 4_665 O(22) O(31) 2.781(10) ? . 6_566 O(23) S(2) 3.397(3) ? . 5_666 O(23) O(1) 2.761(4) ? . 5_666 O(23) O(2) 3.477(4) ? . 5_666 O(23) O(7) 2.795(4) ? . 1_554 O(23) O(20A) 2.707(10) ? . 1_554 O(23) O(20B) 2.722(11) ? . 1_554 O(23) O(26A) 2.891(11) ? . 5_666 O(23) O(26B) 2.830(13) ? . 5_666 O(23) O(29A) 3.572(15) ? . 5_666 O(23) O(29B) 3.58(2) ? . 4_664 O(24) O(15) 2.755(10) ? . 6_566 O(24) O(28) 2.789(12) ? . . O(24) O(28) 2.789(12) ? . 3_565 O(24) O(31) 2.673(12) ? . . O(25) O(1) 2.941(7) ? . 8_556 O(25) O(2) 3.561(7) ? . . O(25) O(20A) 3.217(12) ? . 4_664 O(25) O(20B) 2.607(13) ? . 4_664 O(25) O(22) 3.346(7) ? . 2_644 O(25) O(26A) 2.569(13) ? . . O(25) O(26B) 2.905(14) ? . . O(25) O(29A) 2.717(15) ? . . O(25) O(29B) 2.70(2) ? . . O(25) C(14) 3.419(8) ? . 4_664 O(26A) S(2) 3.414(14) ? . . O(26A) O(2) 3.470(13) ? . . O(26A) O(23) 2.891(11) ? . 5_666 O(26A) O(25) 2.569(13) ? . . O(26A) O(28) 2.988(16) ? . 5_666 O(26A) O(29A) 3.516(18) ? . . O(26A) O(29B) 3.17(2) ? . 8_456 O(26B) O(23) 2.830(13) ? . 5_666 O(26B) O(25) 2.905(14) ? . . O(26B) O(27) 2.900(16) ? . . O(26B) O(28) 2.716(17) ? . 5_666 O(26B) O(29B) 2.99(2) ? . 8_456 O(27) O(20A) 2.851(16) ? . 5_667 O(27) O(20A) 2.851(16) ? . 7_647 O(27) O(20B) 3.363(16) ? . 5_667 O(27) O(20B) 3.363(16) ? . 7_647 O(27) O(26B) 2.900(16) ? . . O(27) O(26B) 2.900(16) ? . 3_555 O(27) O(30) 2.93(2) ? . 5_666 O(27) O(30) 2.93(2) ? . 7_646 O(28) S(3) 3.559(11) ? . 4_664 O(28) O(8) 2.935(11) ? . 8_556 O(28) O(24) 2.789(12) ? . . O(28) O(26A) 2.988(16) ? . 5_666 O(28) O(26B) 2.716(17) ? . 5_666 O(28) O(29A) 2.472(18) ? . 4_664 O(28) O(29B) 2.30(2) ? . 4_664 O(29A) O(2) 2.825(14) ? . . O(29A) O(7) 2.939(14) ? . 5_667 O(29A) O(23) 3.572(15) ? . 5_666 O(29A) O(25) 2.717(15) ? . . O(29A) O(26A) 3.516(18) ? . . O(29A) O(28) 2.472(18) ? . 4_665 O(29A) O(30) 2.88(2) ? . 5_666 O(29B) S(3) 3.31(2) ? . . O(29B) O(1) 3.24(2) ? . 8_556 O(29B) O(2) 2.71(2) ? . . O(29B) O(23) 3.58(2) ? . 4_665 O(29B) O(25) 2.70(2) ? . . O(29B) O(26A) 3.17(2) ? . 8_556 O(29B) O(26B) 2.99(2) ? . 8_556 O(29B) O(28) 2.30(2) ? . 4_665 O(30) O(18) 2.691(16) ? . 1_554 O(30) O(20A) 3.464(19) ? . 1_554 O(30) O(27) 2.93(2) ? . 5_666 O(30) O(29A) 2.88(2) ? . 5_666 O(31) S(6) 3.553(5) ? . 6_466 O(31) S(6) 3.553(5) ? . 8_456 O(31) O(10) 3.099(8) ? . 6_466 O(31) O(10) 3.099(8) ? . 8_456 O(31) O(12) 2.869(5) ? . 6_466 O(31) O(12) 2.869(5) ? . 8_456 O(31) O(13) 3.454(8) ? . 6_566 O(31) O(22) 2.781(10) ? . 6_466 O(31) O(24) 2.673(12) ? . . C(4) O(2) 3.185(5) ? . 8_456 C(5) O(2) 3.134(5) ? . 8_456 C(6) O(2) 3.535(5) ? . 8_456 C(7) O(5) 3.572(5) ? . 8_556 C(8) O(5) 3.476(5) ? . 8_556 C(14) O(25) 3.419(8) ? . 4_665 C(15) C(15) 3.533(5) ? . 5_767 S(2) H(5) 3.414 ? . 8_556 S(6) H(5) 3.405 ? . 1_655 O(1) H(2) 3.398 ? . 8_456 O(3) H(8) 3.520 ? . 5_767 O(5) H(9) 2.847 ? . 8_456 O(11) H(4) 2.793 ? . 8_556 O(11) H(5) 3.089 ? . 1_655 O(12) H(5) 3.143 ? . 1_655 O(23) H(1) 2.043 ? . 5_666 O(25) H(1) 3.217 ? . 8_556 O(25) H(2) 3.460 ? . . O(25) H(8) 2.993 ? . 4_664 O(26A) H(8) 3.422 ? . 4_664 O(28) H(3) 3.453 ? . 4_664 O(29A) H(2) 2.345 ? . . O(29B) H(1) 3.047 ? . 8_556 O(29B) H(2) 2.010 ? . . C(1) H(9) 3.455 ? . 8_456 C(2) H(9) 2.809 ? . 8_456 C(3) H(2) 3.496 ? . 8_456 C(4) H(2) 3.160 ? . 8_456 C(5) H(2) 3.467 ? . 8_456 C(13) H(5) 3.564 ? . 1_655 C(18) H(4) 3.113 ? . 8_556 H(1) O(23) 2.043 ? . 5_666 H(1) O(25) 3.217 ? . 8_456 H(1) O(29B) 3.047 ? . 8_456 H(1) H(2) 3.563 ? . 8_456 H(2) O(1) 3.398 ? . 8_556 H(2) O(25) 3.460 ? . . H(2) O(29A) 2.345 ? . . H(2) O(29B) 2.010 ? . . H(2) C(3) 3.496 ? . 8_556 H(2) C(4) 3.160 ? . 8_556 H(2) C(5) 3.467 ? . 8_556 H(2) H(1) 3.563 ? . 8_556 H(3) O(28) 3.453 ? . 4_665 H(4) O(11) 2.793 ? . 8_456 H(4) C(18) 3.113 ? . 8_456 H(4) H(5) 3.426 ? . 8_556 H(4) H(9) 2.293 ? . 8_456 H(5) S(2) 3.414 ? . 8_456 H(5) S(6) 3.405 ? . 1_455 H(5) O(11) 3.089 ? . 1_455 H(5) O(12) 3.143 ? . 1_455 H(5) C(13) 3.564 ? . 1_455 H(5) H(4) 3.426 ? . 8_456 H(8) O(3) 3.520 ? . 5_767 H(8) O(25) 2.993 ? . 4_665 H(8) O(26A) 3.422 ? . 4_665 H(9) O(5) 2.847 ? . 8_556 H(9) C(1) 3.455 ? . 8_556 H(9) C(2) 2.809 ? . 8_556 H(9) H(4) 2.293 ? . 8_556 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 830335' ####################################################################### # # 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_General #TrackingRef 'TC6A-SO3CeCIF.cif' _audit_creation_date 2010-06-17 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== data__TC6A-SO3Ce #TrackingRef 'TC6A-SO3CeCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H18 Ce2 O47 S12 ' _chemical_formula_moiety 'C36 H18 Ce2 O47 S12 ' _chemical_formula_weight 1867.47 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 13.9160(8) _cell_length_b 26.5308(13) _cell_length_c 19.3049(11) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 7127.4(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 34621 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 110.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3672.00 _exptl_absorpt_coefficient_mu 1.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.484 _exptl_absorpt_correction_T_max 0.710 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 110.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 61718 _diffrn_reflns_av_R_equivalents 0.085 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Several oxygen atoms of water molecules were disordered. Four water molecules (O27, O28, O29, and O30) were refined with partial occupancy (0.5). One water molecule (O26) indicated disordering at two positions (A and B sites). They were isotropically refined. The parts containing (O26A and O26B) were refined as the disordered water molecules, occupancy of which was fixed at 0.72 and 0.28. ; _reflns_number_total 8257 _reflns_number_gt 5873 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2427 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8257 _refine_ls_number_parameters 447 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1294P)^2^+35.1590P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.77 _refine_diff_density_min -3.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ce Ce -0.249 2.633 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ce(1) Ce 0.72704(4) 0.2500 0.66521(3) 0.03103(18) Uani 1.00 2 d S . . Ce(2) Ce 0.25185(5) 0.2500 0.46877(4) 0.0389(2) Uani 1.00 2 d S . . S(3) S 0.28531(15) 0.51711(8) 0.59900(12) 0.0417(4) Uani 1.00 1 d . . . S(4) S 0.86603(14) 0.34407(7) 0.77340(11) 0.0337(4) Uani 1.00 1 d . . . S(5) S 0.08388(16) 0.34133(8) 0.56469(12) 0.0422(5) Uani 1.00 1 d . . . S(6) S 0.56622(14) 0.38532(7) 0.50007(11) 0.0356(4) Uani 1.00 1 d . . . S(7) S 0.61279(14) 0.49700(8) 0.73804(11) 0.0379(4) Uani 1.00 1 d . . . S(8) S 0.97043(14) 0.50503(7) 0.61560(11) 0.0341(4) Uani 1.00 1 d . . . O(1) O 0.7764(4) 0.5434(2) 0.6556(3) 0.0404(13) Uani 1.00 1 d . . . O(2) O 0.4315(4) 0.5368(2) 0.7018(3) 0.0445(13) Uani 1.00 1 d . . . O(3) O 0.1829(4) 0.54596(19) 0.4691(3) 0.0377(12) Uani 1.00 1 d . . . O(4) O 0.8675(4) 0.3506(2) 0.8473(2) 0.0431(13) Uani 1.00 1 d . . . O(5) O 0.9578(4) 0.3290(2) 0.7441(3) 0.0402(12) Uani 1.00 1 d . . . O(6) O 0.7893(4) 0.30973(19) 0.7526(3) 0.0410(13) Uani 1.00 1 d . . . O(7) O 0.5338(4) 0.3980(2) 0.4315(3) 0.0423(13) Uani 1.00 1 d . . . O(8) O 0.5261(4) 0.3373(2) 0.5245(3) 0.0410(13) Uani 1.00 1 d . . . O(9) O 0.6705(4) 0.3848(2) 0.5070(3) 0.0387(12) Uani 1.00 1 d . . . O(10) O 0.1187(5) 0.3367(2) 0.6343(3) 0.0553(17) Uani 1.00 1 d . . . O(11) O -0.0186(4) 0.3373(2) 0.5565(4) 0.0562(17) Uani 1.00 1 d . . . O(12) O 0.2958(9) 0.2500 0.5952(5) 0.061(2) Uani 1.00 2 d S . . O(13) O 0.3296(5) 0.3337(2) 0.5052(4) 0.0618(18) Uani 1.00 1 d . . . O(14) O 0.4312(10) 0.2500 0.4416(7) 0.092(3) Uani 1.00 2 d S . . O(15) O 0.2699(7) 0.1939(3) 0.3655(5) 0.092(2) Uani 1.00 1 d . . . O(16) O 0.1021(9) 0.2500 0.3905(6) 0.078(3) Uani 1.00 2 d S . . O(17) O 0.1311(5) 0.3072(2) 0.5165(3) 0.0541(16) Uani 1.00 1 d . . . O(18) O 0.9095(6) 0.2500 0.6543(4) 0.0390(18) Uani 1.00 2 d S . . O(19) O 0.7895(4) 0.1769(2) 0.5928(3) 0.0494(15) Uani 1.00 1 d . . . O(20) O 0.6508(7) 0.2500 0.5405(5) 0.050(2) Uani 1.00 2 d S . . O(21) O 0.6238(5) 0.2500 0.7767(4) 0.0310(15) Uani 1.00 2 d S . . O(22) O 0.5953(4) 0.1860(2) 0.6584(3) 0.0435(14) Uani 1.00 1 d . . . O(23) O 0.3762(4) 0.1110(2) 0.3415(3) 0.0459(14) Uani 1.00 1 d . . . O(24) O -0.0593(10) 0.2500 0.4764(7) 0.090(3) Uiso 1.00 2 d S . . O(25) O 0.2690(13) 0.2500 0.0818(10) 0.127(6) Uiso 1.00 2 d S . . O(26A) O 0.5603(11) 0.6149(6) 0.8003(8) 0.104(6) Uiso 0.72 1 d P . . O(26B) O 0.596(2) 0.6497(12) 0.7889(15) 0.077(12) Uiso 0.28 1 d P . . O(27) O 0.3948(12) 0.6348(6) 0.8235(8) 0.069(4) Uiso 0.50 1 d P . . O(28) O 0.3408(19) 0.2500 0.2410(13) 0.081(6) Uiso 0.50 2 d SP . . O(29) O 0.506(2) 0.2500 0.3091(16) 0.105(9) Uiso 0.50 2 d SP . . O(30) O 0.7689(16) 0.1507(8) 0.3789(12) 0.104(6) Uiso 0.50 1 d P . . C(1) C 0.5241(5) 0.4322(2) 0.5581(4) 0.0355(16) Uani 1.00 1 d . . . C(2) C 0.4314(5) 0.4528(2) 0.5501(4) 0.0368(17) Uani 1.00 1 d . . . C(3) C 0.3992(5) 0.4869(2) 0.5986(4) 0.0359(16) Uani 1.00 1 d . . . C(4) C 0.4587(5) 0.5013(2) 0.6543(4) 0.0364(17) Uani 1.00 1 d . . . C(5) C 0.5487(5) 0.4797(2) 0.6625(4) 0.0346(16) Uani 1.00 1 d . . . C(6) C 0.5813(5) 0.4445(2) 0.6145(4) 0.0357(16) Uani 1.00 1 d . . . C(7) C 0.8384(5) 0.4029(2) 0.7359(3) 0.0317(15) Uani 1.00 1 d . . . C(8) C 0.9042(5) 0.4272(2) 0.6942(3) 0.0309(15) Uani 1.00 1 d . . . C(9) C 0.8817(5) 0.4746(2) 0.6665(4) 0.0319(15) Uani 1.00 1 d . . . C(10) C 0.7935(5) 0.4968(2) 0.6810(4) 0.0320(15) Uani 1.00 1 d . . . C(11) C 0.7259(5) 0.4701(3) 0.7206(4) 0.0360(16) Uani 1.00 1 d . . . C(12) C 0.7474(5) 0.4226(2) 0.7477(4) 0.0335(16) Uani 1.00 1 d . . . C(13) C 0.1157(5) 0.4025(2) 0.5371(4) 0.0361(17) Uani 1.00 1 d . . . C(14) C 0.1860(5) 0.4296(2) 0.5706(4) 0.0367(17) Uani 1.00 1 d . . . C(15) C 0.2094(5) 0.4770(2) 0.5497(4) 0.0345(16) Uani 1.00 1 d . . . C(16) C 0.1637(5) 0.4988(2) 0.4919(4) 0.0322(15) Uani 1.00 1 d . . . C(17) C 0.0700(5) 0.4228(2) 0.4794(4) 0.0354(16) Uani 1.00 1 d . . . C(18) C 0.0950(5) 0.4708(2) 0.4557(4) 0.0337(16) Uani 1.00 1 d . . . H(1) H 0.3920 0.4433 0.5121 0.044 Uiso 1.00 1 c R . . H(2) H 0.6423 0.4290 0.6202 0.043 Uiso 1.00 1 c R . . H(3) H 0.9643 0.4119 0.6842 0.037 Uiso 1.00 1 c R . . H(4) H 0.7010 0.4042 0.7735 0.040 Uiso 1.00 1 c R . . H(5) H 0.2186 0.4150 0.6089 0.044 Uiso 1.00 1 c R . . H(6) H 0.0217 0.4040 0.4561 0.042 Uiso 1.00 1 c R . . H(7) H 0.7199 0.5520 0.6655 0.061 Uiso 1.00 1 c R . . H(8) H 0.3725 0.5427 0.6975 0.067 Uiso 1.00 1 c R . . H(9) H 0.2206 0.5603 0.4968 0.057 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ce(1) 0.0196(3) 0.0299(3) 0.0436(3) 0.0000 0.0000(2) 0.0000 Ce(2) 0.0323(3) 0.0354(3) 0.0489(4) 0.0000 0.0010(2) 0.0000 S(3) 0.0311(10) 0.0412(10) 0.0528(13) 0.0077(8) -0.0068(9) 0.0001(8) S(4) 0.0268(9) 0.0295(9) 0.0449(11) -0.0012(6) -0.0020(7) 0.0040(7) S(5) 0.0363(11) 0.0327(9) 0.0576(13) 0.0018(7) 0.0076(9) 0.0113(8) S(6) 0.0274(9) 0.0362(9) 0.0432(11) 0.0009(7) -0.0003(7) 0.0032(7) S(7) 0.0239(9) 0.0448(10) 0.0452(11) 0.0035(7) 0.0041(8) -0.0004(8) S(8) 0.0234(9) 0.0340(9) 0.0450(11) -0.0003(6) 0.0004(7) 0.0062(7) O(1) 0.034(3) 0.034(2) 0.054(3) 0.010(2) 0.009(2) 0.010(2) O(2) 0.030(3) 0.050(3) 0.054(3) 0.007(2) 0.005(2) -0.001(2) O(3) 0.032(3) 0.030(2) 0.051(3) -0.002(2) -0.006(2) 0.005(2) O(4) 0.042(3) 0.045(3) 0.042(3) 0.001(2) -0.004(2) 0.004(2) O(5) 0.029(2) 0.036(2) 0.056(3) 0.001(2) -0.003(2) 0.004(2) O(6) 0.029(2) 0.029(2) 0.065(3) -0.005(2) 0.000(2) -0.000(2) O(7) 0.039(3) 0.050(3) 0.039(3) 0.001(2) -0.006(2) 0.004(2) O(8) 0.037(3) 0.034(2) 0.053(3) -0.003(2) 0.001(2) 0.003(2) O(9) 0.031(2) 0.042(2) 0.043(3) 0.006(2) -0.003(2) 0.004(2) O(10) 0.069(4) 0.047(3) 0.050(3) -0.007(3) -0.001(3) 0.022(2) O(11) 0.033(3) 0.046(3) 0.090(5) -0.006(2) 0.011(3) 0.016(3) O(12) 0.091(8) 0.045(5) 0.048(5) 0.0000 -0.009(5) 0.0000 O(13) 0.057(4) 0.050(3) 0.079(5) -0.022(3) -0.005(3) -0.001(3) O(14) 0.084(5) 0.105(5) 0.087(5) 0.0000 0.001(4) 0.0000 O(15) 0.105(4) 0.087(4) 0.083(4) 0.026(3) -0.013(3) -0.005(3) O(16) 0.067(4) 0.098(5) 0.070(4) 0.0000 -0.003(3) 0.0000 O(17) 0.050(4) 0.035(3) 0.077(4) 0.007(2) 0.015(3) 0.005(2) O(18) 0.031(4) 0.031(3) 0.055(5) 0.0000 0.004(3) 0.0000 O(19) 0.033(3) 0.055(3) 0.061(4) -0.005(2) 0.004(2) -0.021(3) O(20) 0.042(5) 0.060(5) 0.048(5) 0.0000 -0.003(4) 0.0000 O(21) 0.029(3) 0.030(3) 0.034(3) 0.0000 0.002(3) 0.0000 O(22) 0.030(3) 0.052(3) 0.049(3) -0.005(2) 0.003(2) -0.010(2) O(23) 0.036(3) 0.045(3) 0.057(3) -0.005(2) -0.002(2) -0.006(2) C(1) 0.030(4) 0.036(3) 0.041(4) -0.001(3) -0.001(3) 0.009(3) C(2) 0.034(4) 0.030(3) 0.046(4) 0.003(3) -0.004(3) 0.006(3) C(3) 0.024(3) 0.035(3) 0.049(4) 0.001(2) 0.006(3) 0.010(3) C(4) 0.027(4) 0.033(3) 0.050(5) 0.003(3) -0.001(3) 0.004(3) C(5) 0.021(3) 0.039(4) 0.044(4) 0.001(2) 0.004(3) 0.001(3) C(6) 0.028(3) 0.037(3) 0.042(4) 0.003(3) -0.002(3) 0.011(3) C(7) 0.030(3) 0.029(3) 0.036(4) -0.003(2) -0.003(3) 0.002(2) C(8) 0.028(3) 0.032(3) 0.033(3) 0.002(2) -0.001(3) -0.000(2) C(9) 0.023(3) 0.034(3) 0.039(4) -0.003(2) 0.001(3) 0.001(2) C(10) 0.031(4) 0.026(3) 0.039(4) -0.000(2) 0.007(3) 0.004(2) C(11) 0.031(4) 0.041(4) 0.036(4) -0.001(3) 0.001(3) -0.005(3) C(12) 0.024(3) 0.036(3) 0.041(4) -0.003(2) -0.000(3) 0.003(3) C(13) 0.035(4) 0.030(3) 0.044(4) 0.008(3) 0.008(3) 0.007(3) C(14) 0.029(4) 0.034(3) 0.046(4) 0.006(3) 0.001(3) 0.007(3) C(15) 0.022(3) 0.038(4) 0.043(4) 0.005(2) 0.007(3) 0.004(3) C(16) 0.024(3) 0.035(3) 0.037(4) 0.009(2) 0.004(3) 0.004(2) C(17) 0.019(3) 0.035(3) 0.053(4) 0.005(2) 0.002(3) 0.007(3) C(18) 0.022(3) 0.034(3) 0.045(4) 0.005(2) 0.002(3) 0.008(3) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ce(1) O(6) 2.471(5) yes . . Ce(1) O(6) 2.471(5) yes . 3_555 Ce(1) O(18) 2.548(8) yes . . Ce(1) O(19) 2.544(6) yes . . Ce(1) O(19) 2.544(6) yes . 3_555 Ce(1) O(20) 2.631(9) yes . . Ce(1) O(21) 2.588(7) yes . . Ce(1) O(22) 2.502(5) yes . . Ce(1) O(22) 2.502(5) yes . 3_555 Ce(2) O(12) 2.516(9) yes . . Ce(2) O(13) 2.568(6) yes . . Ce(2) O(13) 2.568(6) yes . 3_555 Ce(2) O(14) 2.550(13) yes . . Ce(2) O(15) 2.501(10) yes . . Ce(2) O(15) 2.501(10) yes . 3_555 Ce(2) O(16) 2.574(12) yes . . Ce(2) O(17) 2.445(6) yes . . Ce(2) O(17) 2.445(6) yes . 3_555 S(3) C(3) 1.776(7) yes . . S(3) C(15) 1.776(8) yes . . S(4) O(4) 1.437(5) yes . . S(4) O(5) 1.452(5) yes . . S(4) O(6) 1.460(5) yes . . S(4) C(7) 1.763(7) yes . . S(5) O(10) 1.434(7) yes . . S(5) O(11) 1.439(6) yes . . S(5) O(17) 1.454(7) yes . . S(5) C(13) 1.765(7) yes . . S(6) O(7) 1.438(6) yes . . S(6) O(8) 1.469(5) yes . . S(6) O(9) 1.458(6) yes . . S(6) C(1) 1.773(8) yes . . S(7) C(5) 1.771(8) yes . . S(7) C(11) 1.760(8) yes . . S(8) C(9) 1.773(7) yes . . S(8) C(18) 1.770(8) yes . 5_666 O(1) C(10) 1.350(9) yes . . O(2) C(4) 1.368(9) yes . . O(3) C(16) 1.353(9) yes . . O(26A) O(26B) 1.07(3) yes . . C(1) C(2) 1.409(11) yes . . C(1) C(6) 1.387(11) yes . . C(2) C(3) 1.378(11) yes . . C(3) C(4) 1.410(11) yes . . C(4) C(5) 1.386(11) yes . . C(5) C(6) 1.392(11) yes . . C(7) C(8) 1.380(10) yes . . C(7) C(12) 1.388(10) yes . . C(8) C(9) 1.401(10) yes . . C(9) C(10) 1.389(10) yes . . C(10) C(11) 1.404(11) yes . . C(11) C(12) 1.397(11) yes . . C(13) C(14) 1.376(11) yes . . C(13) C(17) 1.390(11) yes . . C(14) C(15) 1.361(10) yes . . C(15) C(16) 1.408(11) yes . . C(16) C(18) 1.397(10) yes . . C(17) C(18) 1.397(10) yes . . O(1) H(7) 0.840 no . . O(2) H(8) 0.840 no . . O(3) H(9) 0.840 no . . C(2) H(1) 0.950 no . . C(6) H(2) 0.950 no . . C(8) H(3) 0.950 no . . C(12) H(4) 0.950 no . . C(14) H(5) 0.950 no . . C(17) H(6) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(6) Ce(1) O(6) 79.76(18) yes . . 3_555 O(6) Ce(1) O(18) 72.97(18) yes . . . O(6) Ce(1) O(19) 138.09(19) yes . . . O(6) Ce(1) O(19) 76.5(2) yes . . 3_555 O(6) Ce(1) O(20) 140.00(13) yes . . . O(6) Ce(1) O(21) 68.09(17) yes . . . O(6) Ce(1) O(22) 136.70(19) yes . . . O(6) Ce(1) O(22) 81.81(18) yes . . 3_555 O(6) Ce(1) O(18) 72.97(18) yes 3_555 . . O(6) Ce(1) O(19) 76.5(2) yes 3_555 . . O(6) Ce(1) O(19) 138.09(19) yes 3_555 . 3_555 O(6) Ce(1) O(20) 140.00(13) yes 3_555 . . O(6) Ce(1) O(21) 68.09(17) yes 3_555 . . O(6) Ce(1) O(22) 81.81(18) yes 3_555 . . O(6) Ce(1) O(22) 136.70(19) yes 3_555 . 3_555 O(18) Ce(1) O(19) 67.31(17) yes . . . O(18) Ce(1) O(19) 67.31(17) yes . . 3_555 O(18) Ce(1) O(20) 109.0(2) yes . . . O(18) Ce(1) O(21) 128.5(2) yes . . . O(18) Ce(1) O(22) 136.54(14) yes . . . O(18) Ce(1) O(22) 136.54(14) yes . . 3_555 O(19) Ce(1) O(19) 99.4(2) yes . . 3_555 O(19) Ce(1) O(20) 68.61(19) yes . . . O(19) Ce(1) O(21) 130.26(14) yes . . . O(19) Ce(1) O(22) 72.77(19) yes . . . O(19) Ce(1) O(22) 137.64(19) yes . . 3_555 O(19) Ce(1) O(20) 68.61(19) yes 3_555 . . O(19) Ce(1) O(21) 130.26(14) yes 3_555 . . O(19) Ce(1) O(22) 137.64(19) yes 3_555 . . O(19) Ce(1) O(22) 72.77(19) yes 3_555 . 3_555 O(20) Ce(1) O(21) 122.5(2) yes . . . O(20) Ce(1) O(22) 69.91(19) yes . . . O(20) Ce(1) O(22) 69.91(19) yes . . 3_555 O(21) Ce(1) O(22) 68.71(17) yes . . . O(21) Ce(1) O(22) 68.71(17) yes . . 3_555 O(22) Ce(1) O(22) 85.46(19) yes . . 3_555 O(12) Ce(2) O(13) 68.43(19) yes . . . O(12) Ce(2) O(13) 68.43(19) yes . . 3_555 O(12) Ce(2) O(14) 87.8(4) yes . . . O(12) Ce(2) O(15) 138.5(2) yes . . . O(12) Ce(2) O(15) 138.5(2) yes . . 3_555 O(12) Ce(2) O(16) 140.0(3) yes . . . O(12) Ce(2) O(17) 78.5(2) yes . . . O(12) Ce(2) O(17) 78.5(2) yes . . 3_555 O(13) Ce(2) O(13) 119.7(2) yes . . 3_555 O(13) Ce(2) O(14) 69.2(2) yes . . . O(13) Ce(2) O(15) 133.7(2) yes . . . O(13) Ce(2) O(15) 70.2(2) yes . . 3_555 O(13) Ce(2) O(16) 120.10(16) yes . . . O(13) Ce(2) O(17) 69.5(2) yes . . . O(13) Ce(2) O(17) 136.3(2) yes . . 3_555 O(13) Ce(2) O(14) 69.2(2) yes 3_555 . . O(13) Ce(2) O(15) 70.2(2) yes 3_555 . . O(13) Ce(2) O(15) 133.7(2) yes 3_555 . 3_555 O(13) Ce(2) O(16) 120.10(16) yes 3_555 . . O(13) Ce(2) O(17) 136.3(2) yes 3_555 . . O(13) Ce(2) O(17) 69.5(2) yes 3_555 . 3_555 O(14) Ce(2) O(15) 74.8(3) yes . . . O(14) Ce(2) O(15) 74.8(3) yes . . 3_555 O(14) Ce(2) O(16) 132.2(4) yes . . . O(14) Ce(2) O(17) 138.58(18) yes . . . O(14) Ce(2) O(17) 138.58(18) yes . . 3_555 O(15) Ce(2) O(15) 73.1(3) yes . . 3_555 O(15) Ce(2) O(16) 67.3(3) yes . . . O(15) Ce(2) O(17) 137.7(2) yes . . . O(15) Ce(2) O(17) 90.0(2) yes . . 3_555 O(15) Ce(2) O(16) 67.3(3) yes 3_555 . . O(15) Ce(2) O(17) 90.0(2) yes 3_555 . . O(15) Ce(2) O(17) 137.7(2) yes 3_555 . 3_555 O(16) Ce(2) O(17) 70.4(2) yes . . . O(16) Ce(2) O(17) 70.4(2) yes . . 3_555 O(17) Ce(2) O(17) 76.8(2) yes . . 3_555 C(3) S(3) C(15) 105.0(3) yes . . . O(4) S(4) O(5) 114.0(3) yes . . . O(4) S(4) O(6) 111.0(3) yes . . . O(4) S(4) C(7) 107.7(3) yes . . . O(5) S(4) O(6) 111.3(3) yes . . . O(5) S(4) C(7) 106.0(3) yes . . . O(6) S(4) C(7) 106.3(3) yes . . . O(10) S(5) O(11) 115.6(4) yes . . . O(10) S(5) O(17) 113.1(4) yes . . . O(10) S(5) C(13) 106.1(3) yes . . . O(11) S(5) O(17) 109.4(4) yes . . . O(11) S(5) C(13) 106.4(3) yes . . . O(17) S(5) C(13) 105.4(3) yes . . . O(7) S(6) O(8) 112.3(3) yes . . . O(7) S(6) O(9) 113.5(3) yes . . . O(7) S(6) C(1) 108.3(3) yes . . . O(8) S(6) O(9) 109.9(3) yes . . . O(8) S(6) C(1) 106.2(3) yes . . . O(9) S(6) C(1) 106.2(3) yes . . . C(5) S(7) C(11) 100.8(3) yes . . . C(9) S(8) C(18) 103.7(3) yes . . 5_666 Ce(1) O(6) S(4) 147.6(3) yes . . . Ce(2) O(17) S(5) 159.7(4) yes . . . S(6) C(1) C(2) 120.4(6) yes . . . S(6) C(1) C(6) 118.1(5) yes . . . C(2) C(1) C(6) 121.3(7) yes . . . C(1) C(2) C(3) 118.6(7) yes . . . S(3) C(3) C(2) 126.1(6) yes . . . S(3) C(3) C(4) 113.6(5) yes . . . C(2) C(3) C(4) 120.3(7) yes . . . O(2) C(4) C(3) 122.3(7) yes . . . O(2) C(4) C(5) 117.3(7) yes . . . C(3) C(4) C(5) 120.4(7) yes . . . S(7) C(5) C(4) 116.2(6) yes . . . S(7) C(5) C(6) 123.9(6) yes . . . C(4) C(5) C(6) 119.8(7) yes . . . C(1) C(6) C(5) 119.5(7) yes . . . S(4) C(7) C(8) 120.6(5) yes . . . S(4) C(7) C(12) 117.7(5) yes . . . C(8) C(7) C(12) 121.6(6) yes . . . C(7) C(8) C(9) 119.6(6) yes . . . S(8) C(9) C(8) 117.6(5) yes . . . S(8) C(9) C(10) 122.3(5) yes . . . C(8) C(9) C(10) 120.0(6) yes . . . O(1) C(10) C(9) 118.1(6) yes . . . O(1) C(10) C(11) 122.7(6) yes . . . C(9) C(10) C(11) 119.2(6) yes . . . S(7) C(11) C(10) 119.9(6) yes . . . S(7) C(11) C(12) 119.1(6) yes . . . C(10) C(11) C(12) 121.0(7) yes . . . C(7) C(12) C(11) 118.3(7) yes . . . S(5) C(13) C(14) 121.1(6) yes . . . S(5) C(13) C(17) 118.9(5) yes . . . C(14) C(13) C(17) 120.0(7) yes . . . C(13) C(14) C(15) 120.9(7) yes . . . S(3) C(15) C(14) 122.5(6) yes . . . S(3) C(15) C(16) 116.6(5) yes . . . C(14) C(15) C(16) 120.4(7) yes . . . O(3) C(16) C(15) 123.2(6) yes . . . O(3) C(16) C(18) 117.6(6) yes . . . C(15) C(16) C(18) 119.1(6) yes . . . C(13) C(17) C(18) 120.1(7) yes . . . S(8) C(18) C(16) 123.2(5) yes 5_666 . . S(8) C(18) C(17) 117.2(5) yes 5_666 . . C(16) C(18) C(17) 119.4(7) yes . . . C(10) O(1) H(7) 109.5 no . . . C(4) O(2) H(8) 109.5 no . . . C(16) O(3) H(9) 109.5 no . . . C(1) C(2) H(1) 120.7 no . . . C(3) C(2) H(1) 120.7 no . . . C(1) C(6) H(2) 120.2 no . . . C(5) C(6) H(2) 120.2 no . . . C(7) C(8) H(3) 120.2 no . . . C(9) C(8) H(3) 120.2 no . . . C(7) C(12) H(4) 120.8 no . . . C(11) C(12) H(4) 120.8 no . . . C(13) C(14) H(5) 119.6 no . . . C(15) C(14) H(5) 119.5 no . . . C(13) C(17) H(6) 119.9 no . . . C(18) C(17) H(6) 120.0 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(6) Ce(1) O(6) S(4) -101.6(6) ? . . 3_555 3_555 O(6) Ce(1) O(6) S(4) 101.6(6) ? 3_555 . . . O(18) Ce(1) O(6) S(4) 26.4(5) ? . . . . O(19) Ce(1) O(6) S(4) 45.5(7) ? . . . . O(19) Ce(1) O(6) S(4) -43.6(6) ? 3_555 . . . O(20) Ce(1) O(6) S(4) -73.1(7) ? . . . . O(21) Ce(1) O(6) S(4) 172.0(6) ? . . . . O(22) Ce(1) O(6) S(4) 167.9(5) ? . . . . O(22) Ce(1) O(6) S(4) -117.8(6) ? 3_555 . . . O(18) Ce(1) O(6) S(4) -26.4(5) ? . . 3_555 3_555 O(19) Ce(1) O(6) S(4) 43.6(6) ? . . 3_555 3_555 O(19) Ce(1) O(6) S(4) -45.5(7) ? 3_555 . 3_555 3_555 O(20) Ce(1) O(6) S(4) 73.1(7) ? . . 3_555 3_555 O(21) Ce(1) O(6) S(4) -172.0(6) ? . . 3_555 3_555 O(22) Ce(1) O(6) S(4) 117.8(6) ? . . 3_555 3_555 O(22) Ce(1) O(6) S(4) -167.9(5) ? 3_555 . 3_555 3_555 O(12) Ce(2) O(17) S(5) 17.6(11) ? . . . . O(12) Ce(2) O(17) S(5) -17.6(11) ? . . 3_555 3_555 O(13) Ce(2) O(17) S(5) -53.5(11) ? . . . . O(13) Ce(2) O(17) S(5) -58.5(12) ? . . 3_555 3_555 O(13) Ce(2) O(17) S(5) 58.5(12) ? 3_555 . . . O(13) Ce(2) O(17) S(5) 53.5(11) ? 3_555 . 3_555 3_555 O(14) Ce(2) O(17) S(5) -55.6(13) ? . . . . O(14) Ce(2) O(17) S(5) 55.6(13) ? . . 3_555 3_555 O(15) Ce(2) O(17) S(5) 173.4(10) ? . . . . O(15) Ce(2) O(17) S(5) 122.2(11) ? . . 3_555 3_555 O(15) Ce(2) O(17) S(5) -122.2(11) ? 3_555 . . . O(15) Ce(2) O(17) S(5) -173.4(10) ? 3_555 . 3_555 3_555 O(16) Ce(2) O(17) S(5) 172.0(12) ? . . . . O(16) Ce(2) O(17) S(5) -172.0(12) ? . . 3_555 3_555 O(17) Ce(2) O(17) S(5) -98.4(11) ? . . 3_555 3_555 O(17) Ce(2) O(17) S(5) 98.4(11) ? 3_555 . . . C(3) S(3) C(15) C(14) 65.3(7) ? . . . . C(3) S(3) C(15) C(16) -122.8(6) ? . . . . C(15) S(3) C(3) C(2) 23.1(8) ? . . . . C(15) S(3) C(3) C(4) -157.3(6) ? . . . . O(4) S(4) O(6) Ce(1) -156.0(5) ? . . . . O(4) S(4) C(7) C(8) 116.0(6) ? . . . . O(4) S(4) C(7) C(12) -66.5(7) ? . . . . O(5) S(4) O(6) Ce(1) -27.8(7) ? . . . . O(5) S(4) C(7) C(8) -6.4(7) ? . . . . O(5) S(4) C(7) C(12) 171.1(6) ? . . . . O(6) S(4) C(7) C(8) -124.9(6) ? . . . . O(6) S(4) C(7) C(12) 52.5(7) ? . . . . C(7) S(4) O(6) Ce(1) 87.2(6) ? . . . . O(10) S(5) O(17) Ce(2) -19.4(13) ? . . . . O(10) S(5) C(13) C(14) 18.5(8) ? . . . . O(10) S(5) C(13) C(17) -163.0(6) ? . . . . O(11) S(5) O(17) Ce(2) -149.8(10) ? . . . . O(11) S(5) C(13) C(14) 142.2(7) ? . . . . O(11) S(5) C(13) C(17) -39.3(7) ? . . . . O(17) S(5) C(13) C(14) -101.6(7) ? . . . . O(17) S(5) C(13) C(17) 76.8(7) ? . . . . C(13) S(5) O(17) Ce(2) 96.2(11) ? . . . . O(7) S(6) C(1) C(2) 38.9(7) ? . . . . O(7) S(6) C(1) C(6) -146.5(6) ? . . . . O(8) S(6) C(1) C(2) -81.9(7) ? . . . . O(8) S(6) C(1) C(6) 92.7(6) ? . . . . O(9) S(6) C(1) C(2) 161.1(6) ? . . . . O(9) S(6) C(1) C(6) -24.3(7) ? . . . . C(5) S(7) C(11) C(10) 85.0(7) ? . . . . C(5) S(7) C(11) C(12) -96.1(7) ? . . . . C(11) S(7) C(5) C(4) -171.0(6) ? . . . . C(11) S(7) C(5) C(6) 12.4(7) ? . . . . C(9) S(8) C(18) C(16) -45.3(7) ? . . 5_666 5_666 C(9) S(8) C(18) C(17) 140.0(6) ? . . 5_666 5_666 C(18) S(8) C(9) C(8) 136.7(6) ? 5_666 . . . C(18) S(8) C(9) C(10) -45.3(7) ? 5_666 . . . S(6) C(1) C(2) C(3) 176.3(6) ? . . . . S(6) C(1) C(6) C(5) -177.5(5) ? . . . . C(2) C(1) C(6) C(5) -3.0(11) ? . . . . C(6) C(1) C(2) C(3) 1.9(11) ? . . . . C(1) C(2) C(3) S(3) -179.5(6) ? . . . . C(1) C(2) C(3) C(4) 0.9(11) ? . . . . S(3) C(3) C(4) O(2) -2.7(10) ? . . . . S(3) C(3) C(4) C(5) 177.7(6) ? . . . . C(2) C(3) C(4) O(2) 176.9(7) ? . . . . C(2) C(3) C(4) C(5) -2.6(11) ? . . . . O(2) C(4) C(5) S(7) 5.3(9) ? . . . . O(2) C(4) C(5) C(6) -178.0(6) ? . . . . C(3) C(4) C(5) S(7) -175.2(6) ? . . . . C(3) C(4) C(5) C(6) 1.6(11) ? . . . . S(7) C(5) C(6) C(1) 177.7(6) ? . . . . C(4) C(5) C(6) C(1) 1.2(11) ? . . . . S(4) C(7) C(8) C(9) -178.2(5) ? . . . . S(4) C(7) C(12) C(11) 177.5(6) ? . . . . C(8) C(7) C(12) C(11) -5.1(11) ? . . . . C(12) C(7) C(8) C(9) 4.4(11) ? . . . . C(7) C(8) C(9) S(8) 177.9(5) ? . . . . C(7) C(8) C(9) C(10) -0.2(8) ? . . . . S(8) C(9) C(10) O(1) -0.7(10) ? . . . . S(8) C(9) C(10) C(11) 178.8(6) ? . . . . C(8) C(9) C(10) O(1) 177.3(6) ? . . . . C(8) C(9) C(10) C(11) -3.2(11) ? . . . . O(1) C(10) C(11) S(7) 0.8(11) ? . . . . O(1) C(10) C(11) C(12) -178.1(7) ? . . . . C(9) C(10) C(11) S(7) -178.6(6) ? . . . . C(9) C(10) C(11) C(12) 2.5(12) ? . . . . S(7) C(11) C(12) C(7) -177.3(6) ? . . . . C(10) C(11) C(12) C(7) 1.6(12) ? . . . . S(5) C(13) C(14) C(15) -179.2(6) ? . . . . S(5) C(13) C(17) C(18) -178.8(6) ? . . . . C(14) C(13) C(17) C(18) -0.4(9) ? . . . . C(17) C(13) C(14) C(15) 2.4(12) ? . . . . C(13) C(14) C(15) S(3) 169.8(6) ? . . . . C(13) C(14) C(15) C(16) -1.8(12) ? . . . . S(3) C(15) C(16) O(3) 7.0(10) ? . . . . S(3) C(15) C(16) C(18) -172.9(5) ? . . . . C(14) C(15) C(16) O(3) 179.1(7) ? . . . . C(14) C(15) C(16) C(18) -0.9(11) ? . . . . O(3) C(16) C(18) S(8) -2.4(10) ? . . . 5_666 O(3) C(16) C(18) C(17) -177.1(6) ? . . . . C(15) C(16) C(18) S(8) 177.5(5) ? . . . 5_666 C(15) C(16) C(18) C(17) 2.8(11) ? . . . . C(13) C(17) C(18) S(8) -177.2(6) ? . . . 5_666 C(13) C(17) C(18) C(16) -2.2(11) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S(4) O(22) 3.542(6) ? . 6_556 S(5) O(24) 3.570(10) ? . . S(7) S(8) 3.457(2) ? . 8_456 S(7) O(23) 3.395(6) ? . 7_656 S(7) O(26A) 3.430(17) ? . . S(8) S(7) 3.457(2) ? . 8_556 S(8) O(26A) 3.563(17) ? . 8_556 O(1) O(2) 3.502(8) ? . 8_556 O(1) O(23) 2.780(8) ? . 7_656 O(1) O(27) 2.960(17) ? . 8_556 O(2) O(1) 3.502(8) ? . 8_456 O(2) O(23) 3.426(8) ? . 7_656 O(2) O(26A) 3.334(17) ? . . O(2) O(27) 3.541(17) ? . . O(2) C(8) 3.554(9) ? . 8_456 O(2) C(9) 3.109(9) ? . 8_456 O(2) C(10) 3.152(9) ? . 8_456 O(4) O(8) 3.336(8) ? . 8_556 O(4) O(10) 3.500(9) ? . 8_556 O(4) O(12) 3.058(7) ? . 6_556 O(4) O(13) 2.932(9) ? . 8_556 O(4) O(22) 3.317(8) ? . 6_556 O(4) C(1) 3.573(9) ? . 8_556 O(4) C(2) 3.474(9) ? . 8_556 O(5) O(10) 3.092(9) ? . 1_655 O(5) O(21) 3.145(7) ? . 6_556 O(5) O(22) 2.713(8) ? . 6_556 O(6) O(10) 3.303(9) ? . 8_556 O(6) O(12) 3.340(10) ? . 6_556 O(7) O(23) 2.809(8) ? . 3_555 O(8) O(4) 3.336(8) ? . 8_456 O(9) O(30) 2.98(2) ? . 3_555 O(10) O(4) 3.500(9) ? . 8_456 O(10) O(5) 3.092(9) ? . 1_455 O(10) O(6) 3.303(9) ? . 8_456 O(10) O(21) 2.871(7) ? . 6_456 O(11) O(18) 3.152(8) ? . 1_455 O(11) O(19) 2.787(8) ? . 3_455 O(11) O(24) 2.843(10) ? . . O(12) O(4) 3.058(7) ? . 6_456 O(12) O(4) 3.058(7) ? . 8_456 O(12) O(6) 3.340(10) ? . 6_456 O(12) O(6) 3.340(10) ? . 8_456 O(12) O(21) 3.442(13) ? . 6_456 O(13) O(4) 2.932(9) ? . 8_456 O(13) O(23) 3.544(9) ? . 3_555 O(14) O(29) 2.76(3) ? . . O(15) O(23) 2.690(12) ? . . O(15) O(27) 2.893(19) ? . 2_544 O(15) O(28) 2.99(2) ? . . O(16) O(24) 2.791(18) ? . . O(16) O(27) 3.320(16) ? . 2_544 O(16) O(27) 3.320(16) ? . 4_564 O(17) O(24) 3.151(14) ? . . O(18) O(11) 3.152(8) ? . 1_655 O(18) O(11) 3.152(8) ? . 3_655 O(18) O(21) 3.266(10) ? . 6_556 O(18) O(24) 3.462(15) ? . 1_655 O(19) O(11) 2.787(8) ? . 3_655 O(20) O(25) 2.88(2) ? . 6_555 O(21) O(5) 3.145(7) ? . 6_456 O(21) O(5) 3.145(7) ? . 8_456 O(21) O(10) 2.871(7) ? . 6_556 O(21) O(10) 2.871(7) ? . 8_556 O(21) O(12) 3.442(13) ? . 6_556 O(21) O(18) 3.266(10) ? . 6_456 O(22) S(4) 3.542(6) ? . 6_456 O(22) O(4) 3.317(8) ? . 6_456 O(22) O(5) 2.713(8) ? . 6_456 O(23) S(7) 3.395(6) ? . 7_646 O(23) O(1) 2.780(8) ? . 7_646 O(23) O(2) 3.426(8) ? . 7_646 O(23) O(7) 2.809(8) ? . 3_555 O(23) O(13) 3.544(9) ? . 3_555 O(23) O(15) 2.690(12) ? . . O(23) O(26A) 2.878(16) ? . 7_646 O(23) O(26B) 2.75(3) ? . 7_646 O(24) S(5) 3.570(10) ? . . O(24) S(5) 3.570(10) ? . 3_555 O(24) O(11) 2.843(10) ? . . O(24) O(11) 2.843(10) ? . 3_555 O(24) O(16) 2.791(18) ? . . O(24) O(17) 3.151(14) ? . . O(24) O(17) 3.151(14) ? . 3_555 O(24) O(18) 3.462(15) ? . 1_455 O(24) O(25) 2.64(2) ? . 6_455 O(25) O(20) 2.88(2) ? . 6_455 O(25) O(24) 2.64(2) ? . 6_555 O(25) O(28) 3.23(3) ? . . O(25) O(30) 2.74(2) ? . 6_455 O(25) O(30) 2.74(2) ? . 8_455 O(26A) S(7) 3.430(17) ? . . O(26A) S(8) 3.563(17) ? . 8_456 O(26A) O(2) 3.334(17) ? . . O(26A) O(23) 2.878(16) ? . 7_656 O(26A) O(27) 2.40(2) ? . . O(26A) O(30) 2.98(2) ? . 2_655 O(26B) O(23) 2.75(3) ? . 7_656 O(26B) O(27) 2.91(3) ? . . O(26B) O(28) 2.86(3) ? . 5_666 O(26B) O(29) 3.56(3) ? . 5_666 O(26B) O(30) 2.56(3) ? . 2_655 O(27) O(1) 2.960(17) ? . 8_456 O(27) O(2) 3.541(17) ? . . O(27) O(15) 2.893(19) ? . 2_555 O(27) O(16) 3.320(16) ? . 2_555 O(27) O(26A) 2.40(2) ? . . O(27) O(26B) 2.91(3) ? . . O(27) C(17) 3.412(18) ? . 4_565 O(28) O(15) 2.99(2) ? . . O(28) O(15) 2.99(2) ? . 3_555 O(28) O(25) 3.23(3) ? . . O(28) O(26B) 2.86(3) ? . 5_666 O(28) O(26B) 2.86(3) ? . 7_646 O(28) O(29) 2.65(4) ? . . O(29) O(14) 2.76(3) ? . . O(29) O(26B) 3.56(3) ? . 5_666 O(29) O(26B) 3.56(3) ? . 7_646 O(29) O(28) 2.65(4) ? . . O(30) O(9) 2.98(2) ? . 3_555 O(30) O(25) 2.74(2) ? . 6_555 O(30) O(26A) 2.98(2) ? . 2_644 O(30) O(26B) 2.56(3) ? . 2_644 C(1) O(4) 3.573(9) ? . 8_456 C(2) O(4) 3.474(9) ? . 8_456 C(8) O(2) 3.554(9) ? . 8_556 C(9) O(2) 3.109(9) ? . 8_556 C(10) O(2) 3.152(9) ? . 8_556 C(17) O(27) 3.412(18) ? . 4_564 C(18) C(18) 3.509(10) ? . 5_566 S(4) H(5) 3.594 ? . 8_556 S(5) H(3) 3.406 ? . 1_455 S(7) H(3) 3.409 ? . 8_456 O(1) H(8) 3.136 ? . 8_556 O(3) H(6) 3.457 ? . 5_566 O(4) H(5) 2.817 ? . 8_556 O(10) H(3) 3.088 ? . 1_455 O(10) H(4) 2.774 ? . 8_456 O(11) H(3) 3.170 ? . 1_455 O(19) H(9) 3.548 ? . 7_646 O(23) H(7) 2.063 ? . 7_646 O(26A) H(6) 3.256 ? . 4_565 O(27) H(6) 2.995 ? . 4_565 O(27) H(7) 3.284 ? . 8_456 O(27) H(8) 3.461 ? . . O(30) H(9) 3.395 ? . 7_646 C(7) H(5) 3.443 ? . 8_556 C(9) H(8) 3.191 ? . 8_556 C(10) H(8) 2.864 ? . 8_556 C(11) H(8) 3.222 ? . 8_556 C(12) H(5) 2.804 ? . 8_556 C(13) H(3) 3.545 ? . 1_455 C(14) H(4) 3.091 ? . 8_456 H(3) S(5) 3.406 ? . 1_655 H(3) S(7) 3.409 ? . 8_556 H(3) O(10) 3.088 ? . 1_655 H(3) O(11) 3.170 ? . 1_655 H(3) C(13) 3.545 ? . 1_655 H(3) H(4) 3.400 ? . 8_556 H(4) O(10) 2.774 ? . 8_556 H(4) C(14) 3.091 ? . 8_556 H(4) H(3) 3.400 ? . 8_456 H(4) H(5) 2.301 ? . 8_556 H(5) S(4) 3.594 ? . 8_456 H(5) O(4) 2.817 ? . 8_456 H(5) C(7) 3.443 ? . 8_456 H(5) C(12) 2.804 ? . 8_456 H(5) H(4) 2.301 ? . 8_456 H(6) O(3) 3.457 ? . 5_566 H(6) O(26A) 3.256 ? . 4_564 H(6) O(27) 2.995 ? . 4_564 H(7) O(23) 2.063 ? . 7_656 H(7) O(27) 3.284 ? . 8_556 H(7) H(8) 3.401 ? . 8_556 H(8) O(1) 3.136 ? . 8_456 H(8) O(27) 3.461 ? . . H(8) C(9) 3.191 ? . 8_456 H(8) C(10) 2.864 ? . 8_456 H(8) C(11) 3.222 ? . 8_456 H(8) H(7) 3.401 ? . 8_456 H(9) O(19) 3.548 ? . 7_656 H(9) O(30) 3.395 ? . 7_656 _database_code_depnum_ccdc_archive 'CCDC 894435' ####################################################################### # # 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_General #TrackingRef 'TC6A-SO3CeCIF.cif' _audit_creation_date 2010-06-17 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'TC6A-SO3EuCIF.cif' #============================================================================== data_TC6A-SO3Eu #TrackingRef 'TC6A-SO3EuCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H74 Eu2 O56 S12' _chemical_formula_moiety 'C36 H74 Eu2 O56 S12' _chemical_formula_weight 2091.59 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.5737(6) _cell_length_b 12.2953(5) _cell_length_c 20.6509(8) _cell_angle_alpha 90.0000 _cell_angle_beta 110.6210(11) _cell_angle_gamma 90.0000 _cell_volume 3700.9(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 28960 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.45 _cell_measurement_temperature 100.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112.00 _exptl_absorpt_coefficient_mu 2.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.458 _exptl_absorpt_correction_T_max 0.653 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 35005 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Two water molecules (O27 and O28) indicated disordering at two positions (A and B sites). They were isotropically refined. The parts containing (O27A and O27B) were refined as the disordered water molecules, occupancy of which was fixed at 0.80 and 0.20. The parts containing (O28A and O28B) were refined as the disordered water molecules, occupancy of which was fixed at 0.80 and 0.20. ; _reflns_number_total 8422 _reflns_number_gt 7687 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0680 _refine_ls_number_restraints 5 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8422 _refine_ls_number_parameters 588 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0326P)^2^+6.1319P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.840 _refine_diff_density_min -1.250 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Eu Eu -0.158 3.668 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.332534(9) 0.263622(10) 0.852303(6) 0.01158(5) Uani 1.0 4 d . . . S1 S 0.78446(4) 0.41362(5) 0.75928(3) 0.01079(12) Uani 1.0 4 d . . . S2 S 0.61963(4) 0.06057(5) 0.59619(3) 0.01054(12) Uani 1.0 4 d . . . S3 S 0.51459(4) 0.33970(5) 0.37057(3) 0.01147(12) Uani 1.0 4 d . . . S4 S 0.97797(4) 0.16445(5) 0.64107(3) 0.01385(13) Uani 1.0 4 d . . . S5 S 0.58325(4) -0.08670(5) 0.33834(3) 0.01164(12) Uani 1.0 4 d . . . S6 S 0.17834(4) 0.23481(5) 0.39320(3) 0.01467(13) Uani 1.0 4 d . . . O1 O 0.62981(13) 0.26768(14) 0.68089(10) 0.0144(4) Uani 1.0 4 d . . . O2 O 0.55323(14) 0.26862(14) 0.52242(9) 0.0152(4) Uani 1.0 4 d . . . O3 O 0.41302(12) 0.50926(14) 0.28850(9) 0.0143(4) Uani 1.0 4 d . . . O4 O 0.98568(14) 0.24608(17) 0.59170(10) 0.0219(5) Uani 1.0 4 d . . . O5 O 0.96981(14) 0.05385(17) 0.61308(11) 0.0238(5) Uani 1.0 4 d . . . O6 O 1.05192(13) 0.17476(16) 0.70783(10) 0.0186(4) Uani 1.0 4 d . . . O7 O 0.68148(13) -0.09401(16) 0.34738(10) 0.0175(4) Uani 1.0 4 d . . . O8 O 0.52760(13) -0.05398(16) 0.26816(9) 0.0183(4) Uani 1.0 4 d . . . O9 O 0.55045(14) -0.18369(15) 0.36222(10) 0.0180(4) Uani 1.0 4 d . . . O10 O 0.11042(14) 0.18557(17) 0.33283(11) 0.0228(5) Uani 1.0 4 d . . . O11 O 0.13580(14) 0.30679(17) 0.43055(10) 0.0209(4) Uani 1.0 4 d . . . O12 O 0.24016(14) 0.15684(17) 0.43998(11) 0.0239(5) Uani 1.0 4 d . . . O13 O 0.41713(15) 0.10565(17) 0.83914(11) 0.0177(4) Uani 1.0 4 d . . . O14 O 0.42472(15) 0.31572(17) 0.78792(11) 0.0171(4) Uani 1.0 4 d . . . O15 O 0.46994(16) 0.2465(2) 0.95270(11) 0.0269(5) Uani 1.0 4 d . . . O16 O 0.24148(14) 0.18313(17) 0.74272(10) 0.0180(4) Uani 1.0 4 d . . . O17 O 0.37281(16) 0.45345(18) 0.88076(12) 0.0238(5) Uani 1.0 4 d . . . O18 O 0.20727(15) 0.37983(18) 0.78884(11) 0.0218(5) Uani 1.0 4 d . . . O19 O 0.28115(14) 0.31542(18) 0.94550(10) 0.0187(4) Uani 1.0 4 d . . . O20 O 0.25939(16) 0.11110(18) 0.88212(12) 0.0230(5) Uani 1.0 4 d . . . O21 O 0.33983(16) 0.51958(18) 0.99367(11) 0.0210(5) Uani 1.0 4 d . . . O22 O 0.38342(14) 0.49036(17) 0.70328(11) 0.0195(4) Uani 1.0 4 d . . . O23 O 0.13020(16) 0.39209(17) 0.64658(11) 0.0222(5) Uani 1.0 4 d . . . O24 O 0.4037(2) 0.39524(19) 0.58668(13) 0.0319(6) Uani 1.0 4 d . . . O25 O 0.23692(17) 0.2979(2) 0.57679(13) 0.0281(5) Uani 1.0 4 d . . . O26 O 0.3906(2) 0.52556(19) 0.47950(12) 0.0366(7) Uani 1.0 4 d . . . O27A O 0.2468(3) 0.6353(3) 0.48961(15) 0.0257(7) Uiso 0.8000 4 d . . . O27B O 0.2111(9) 0.6210(9) 0.4795(6) 0.022(3) Uiso 0.2000 4 d . . . O28A O 0.0968(4) 0.5302(4) 0.4164(3) 0.0687(12) Uiso 0.8000 4 d . . . O28B O 0.0806(12) 0.5164(14) 0.4534(9) 0.058(4) Uiso 0.2000 4 d . . . C1 C 0.87395(17) 0.1911(2) 0.65417(12) 0.0120(5) Uani 1.0 4 d . . . C2 C 0.86720(18) 0.2831(2) 0.69168(12) 0.0123(5) Uani 1.0 4 d . . . C3 C 0.78548(18) 0.3064(2) 0.70131(12) 0.0116(5) Uani 1.0 4 d . . . C4 C 0.70803(18) 0.24004(19) 0.67120(12) 0.0112(5) Uani 1.0 4 d . . . C5 C 0.71587(17) 0.1479(2) 0.63304(12) 0.0110(5) Uani 1.0 4 d . . . C6 C 0.79917(17) 0.1224(2) 0.62637(12) 0.0121(5) Uani 1.0 4 d . . . C7 C 0.57583(17) 0.0212(2) 0.39283(12) 0.0111(5) Uani 1.0 4 d . . . C8 C 0.59917(16) 0.0034(2) 0.46365(12) 0.0110(5) Uani 1.0 4 d . . . C9 C 0.59230(17) 0.0875(2) 0.50645(12) 0.0105(5) Uani 1.0 4 d . . . C10 C 0.56135(17) 0.1913(2) 0.47868(12) 0.0106(5) Uani 1.0 4 d . . . C11 C 0.53962(16) 0.20800(19) 0.40709(12) 0.0102(5) Uani 1.0 4 d . . . C12 C 0.54736(16) 0.1230(2) 0.36510(12) 0.0114(5) Uani 1.0 4 d . . . C13 C 0.24864(17) 0.3189(2) 0.36265(12) 0.0118(5) Uani 1.0 4 d . . . C14 C 0.34144(17) 0.2937(2) 0.37888(12) 0.0109(5) Uani 1.0 4 d . . . C15 C 0.39555(17) 0.35882(19) 0.35355(12) 0.0099(5) Uani 1.0 4 d . . . C16 C 0.35677(17) 0.45032(19) 0.31199(12) 0.0100(5) Uani 1.0 4 d . . . C17 C 0.26415(17) 0.47496(19) 0.29702(12) 0.0105(5) Uani 1.0 4 d . . . C18 C 0.20955(17) 0.4088(2) 0.32178(12) 0.0116(5) Uani 1.0 4 d . . . H1 H 0.9175 0.3288 0.7102 0.0147 Uiso 1.0 4 calc R . . H2 H 0.8049 0.0594 0.6033 0.0145 Uiso 1.0 4 calc R . . H3 H 0.6194 -0.0648 0.4822 0.0132 Uiso 1.0 4 calc R . . H4 H 0.5333 0.1347 0.3180 0.0137 Uiso 1.0 4 calc R . . H5 H 0.3668 0.2338 0.4064 0.0130 Uiso 1.0 4 calc R . . H6 H 0.1477 0.4245 0.3111 0.0139 Uiso 1.0 4 calc R . . H7 H 0.5890 0.2252 0.6598 0.0173 Uiso 1.0 4 calc R . . H8 H 0.5615 0.3287 0.5083 0.0182 Uiso 1.0 4 calc R . . H9 H 0.3856 0.5630 0.2679 0.0172 Uiso 1.0 4 calc R . . H10 H 0.4331 0.0988 0.8080 0.0278 Uiso 1.0 4 calc R . . H11 H 0.4032 0.0527 0.8483 0.0285 Uiso 1.0 4 calc R . . H12 H 0.4080 0.3674 0.7647 0.0243 Uiso 1.0 4 calc R . . H13 H 0.4765 0.3121 0.8012 0.0213 Uiso 1.0 4 calc R . . H14 H 0.5173 0.2303 0.9514 0.0169 Uiso 1.0 4 calc R . . H15 H 0.4743 0.2544 0.9923 0.0453 Uiso 1.0 4 calc R . . H16 H 0.2643 0.1586 0.7193 0.0199 Uiso 1.0 4 calc R . . H17 H 0.1868 0.1768 0.7277 0.0297 Uiso 1.0 4 calc R . . H18 H 0.4258 0.4665 0.8801 0.0269 Uiso 1.0 4 calc R . . H19 H 0.3635 0.4844 0.9102 0.0405 Uiso 1.0 4 calc R . . H20 H 0.2105 0.4356 0.8060 0.0412 Uiso 1.0 4 calc R . . H21 H 0.1835 0.3784 0.7475 0.0415 Uiso 1.0 4 calc R . . H22 H 0.2887 0.3695 0.9615 0.0249 Uiso 1.0 4 calc R . . H23 H 0.2686 0.2700 0.9725 0.0340 Uiso 1.0 4 calc R . . H24 H 0.2219 0.0741 0.8533 0.0313 Uiso 1.0 4 calc R . . H25 H 0.2559 0.1070 0.9175 0.0550 Uiso 1.0 4 calc R . . H26 H 0.3125 0.5609 1.0024 0.0429 Uiso 1.0 4 calc R . . H27 H 0.3901 0.5063 1.0298 0.0679 Uiso 1.0 4 calc R . . H28 H 0.4153 0.5374 0.7262 0.0573 Uiso 1.0 4 calc R . . H29 H 0.4054 0.4659 0.6776 0.0291 Uiso 1.0 4 calc R . . H30 H 0.1676 0.3715 0.6249 0.0564 Uiso 1.0 4 calc R . . H31 H 0.0877 0.3434 0.6330 0.0574 Uiso 1.0 4 calc R . . H32 H 0.3492 0.3635 0.5810 0.0476 Uiso 1.0 4 calc R . . H33 H 0.4474 0.3584 0.6042 0.0590 Uiso 1.0 4 calc R . . H34 H 0.2526 0.2372 0.5893 0.0595 Uiso 1.0 4 calc R . . H35 H 0.2086 0.2995 0.5344 0.0560 Uiso 1.0 4 calc R . . H36 H 0.4008 0.4838 0.5088 0.0365 Uiso 1.0 4 calc R . . H37 H 0.3887 0.4891 0.4468 0.0504 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Eu1 0.01130(7) 0.01334(7) 0.01004(7) -0.00157(5) 0.00370(5) -0.00210(4) S1 0.0128(3) 0.0098(3) 0.0074(3) 0.0015(3) 0.0008(3) 0.0001(2) S2 0.0118(3) 0.0112(3) 0.0074(3) -0.0011(3) 0.0019(3) 0.0003(2) S3 0.0096(3) 0.0111(3) 0.0133(3) 0.0017(3) 0.0036(3) 0.0033(2) S4 0.0098(3) 0.0180(3) 0.0131(3) 0.0007(3) 0.0033(3) -0.0017(3) S5 0.0127(3) 0.0119(3) 0.0102(3) -0.0003(3) 0.0039(3) -0.0028(2) S6 0.0111(3) 0.0155(3) 0.0177(3) 0.0007(3) 0.0055(3) 0.0061(3) O1 0.0113(9) 0.0158(9) 0.0154(9) -0.0009(7) 0.0037(8) -0.0043(7) O2 0.0238(11) 0.0107(9) 0.0115(9) 0.0020(8) 0.0068(8) -0.0004(7) O3 0.0122(9) 0.0135(9) 0.0176(9) 0.0019(7) 0.0057(8) 0.0065(7) O4 0.0179(10) 0.0330(12) 0.0149(10) -0.0043(9) 0.0059(9) 0.0014(8) O5 0.0148(10) 0.0239(11) 0.0328(12) 0.0010(9) 0.0086(9) -0.0112(9) O6 0.0097(9) 0.0282(11) 0.0146(9) 0.0002(8) 0.0001(8) 0.0002(8) O7 0.0125(9) 0.0224(10) 0.0180(10) -0.0006(8) 0.0059(8) -0.0062(8) O8 0.0200(10) 0.0224(10) 0.0094(9) 0.0031(8) 0.0012(8) -0.0028(8) O9 0.0215(10) 0.0130(9) 0.0213(10) -0.0013(8) 0.0095(9) -0.0022(8) O10 0.0177(10) 0.0234(11) 0.0266(11) -0.0071(9) 0.0070(9) -0.0017(9) O11 0.0187(10) 0.0246(11) 0.0231(10) 0.0007(9) 0.0118(9) 0.0039(9) O12 0.0162(10) 0.0255(11) 0.0310(12) 0.0043(9) 0.0097(9) 0.0175(9) O13 0.0231(11) 0.0150(10) 0.0171(10) 0.0021(9) 0.0096(9) 0.0001(8) O14 0.0146(11) 0.0203(11) 0.0178(10) 0.0030(9) 0.0073(9) 0.0057(8) O15 0.0135(11) 0.0514(15) 0.0139(11) 0.0055(10) 0.0024(9) -0.0104(10) O16 0.0099(10) 0.0274(11) 0.0157(10) 0.0008(9) 0.0033(9) -0.0082(8) O17 0.0260(12) 0.0234(11) 0.0280(12) -0.0101(10) 0.0171(10) -0.0102(9) O18 0.0270(12) 0.0196(11) 0.0157(11) 0.0048(9) 0.0036(9) -0.0044(9) O19 0.0224(11) 0.0173(11) 0.0191(10) -0.0024(9) 0.0109(9) -0.0037(9) O20 0.0292(12) 0.0245(11) 0.0163(11) -0.0121(10) 0.0092(10) -0.0048(9) O21 0.0230(12) 0.0219(11) 0.0186(10) 0.0049(9) 0.0079(10) -0.0040(9) O22 0.0196(11) 0.0195(10) 0.0193(10) 0.0003(9) 0.0069(9) 0.0025(8) O23 0.0263(12) 0.0189(10) 0.0220(11) -0.0014(9) 0.0092(10) -0.0006(8) O24 0.0395(15) 0.0199(11) 0.0363(14) 0.0027(11) 0.0132(12) 0.0034(10) O25 0.0318(13) 0.0305(13) 0.0210(12) 0.0040(11) 0.0081(10) 0.0006(10) O26 0.075(2) 0.0205(12) 0.0193(12) -0.0108(12) 0.0227(13) -0.0074(10) C1 0.0091(12) 0.0156(12) 0.0105(11) 0.0023(10) 0.0026(10) 0.0014(9) C2 0.0114(12) 0.0132(12) 0.0100(11) -0.0007(10) 0.0010(10) 0.0009(9) C3 0.0142(12) 0.0109(11) 0.0072(11) 0.0025(10) 0.0004(10) 0.0008(9) C4 0.0122(12) 0.0120(12) 0.0078(11) 0.0019(10) 0.0014(10) 0.0024(9) C5 0.0115(12) 0.0121(11) 0.0069(11) -0.0010(10) 0.0002(10) 0.0016(9) C6 0.0149(13) 0.0122(11) 0.0076(11) 0.0034(10) 0.0019(10) 0.0009(9) C7 0.0096(12) 0.0121(11) 0.0114(11) -0.0002(10) 0.0034(10) -0.0026(9) C8 0.0089(12) 0.0116(11) 0.0118(12) 0.0001(9) 0.0027(10) 0.0018(9) C9 0.0090(11) 0.0129(12) 0.0083(11) -0.0005(9) 0.0014(9) 0.0006(9) C10 0.0090(11) 0.0105(11) 0.0114(11) -0.0020(9) 0.0026(10) -0.0022(9) C11 0.0080(11) 0.0102(11) 0.0113(11) 0.0002(9) 0.0023(10) 0.0026(9) C12 0.0089(11) 0.0156(12) 0.0088(11) -0.0003(10) 0.0020(9) 0.0013(9) C13 0.0113(12) 0.0142(12) 0.0098(11) -0.0014(10) 0.0036(10) -0.0005(9) C14 0.0120(12) 0.0112(11) 0.0079(11) 0.0010(10) 0.0016(10) 0.0002(9) C15 0.0099(12) 0.0094(11) 0.0096(11) 0.0022(9) 0.0022(9) -0.0014(9) C16 0.0126(12) 0.0086(11) 0.0084(11) -0.0030(9) 0.0033(10) -0.0019(9) C17 0.0127(12) 0.0093(11) 0.0076(11) 0.0000(9) 0.0012(10) -0.0004(9) C18 0.0095(12) 0.0136(12) 0.0109(11) -0.0002(10) 0.0026(10) -0.0018(9) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Eu1 O13 2.415(3) yes . . Eu1 O14 2.363(3) yes . . Eu1 O15 2.408(2) yes . . Eu1 O16 2.4189(19) yes . . Eu1 O17 2.434(3) yes . . Eu1 O18 2.401(2) yes . . Eu1 O19 2.416(3) yes . . Eu1 O20 2.385(3) yes . . S1 C3 1.785(3) yes . . S1 C17 1.784(3) yes . 3_666 S2 C5 1.782(3) yes . . S2 C9 1.780(3) yes . . S3 C11 1.771(3) yes . . S3 C15 1.777(3) yes . . S4 O4 1.465(3) yes . . S4 O5 1.466(3) yes . . S4 O6 1.4576(18) yes . . S4 C1 1.764(3) yes . . S5 O7 1.477(3) yes . . S5 O8 1.4590(18) yes . . S5 O9 1.450(3) yes . . S5 C7 1.770(3) yes . . S6 O10 1.453(2) yes . . S6 O11 1.475(3) yes . . S6 O12 1.457(2) yes . . S6 C13 1.776(3) yes . . O1 C4 1.346(4) yes . . O2 C10 1.348(4) yes . . O3 C16 1.352(4) yes . . C1 C2 1.396(4) yes . . C1 C6 1.389(4) yes . . C2 C3 1.385(5) yes . . C3 C4 1.406(4) yes . . C4 C5 1.409(4) yes . . C5 C6 1.388(4) yes . . C7 C8 1.394(4) yes . . C7 C12 1.383(4) yes . . C8 C9 1.388(4) yes . . C9 C10 1.413(4) yes . . C10 C11 1.411(4) yes . . C11 C12 1.390(4) yes . . C13 C14 1.399(4) yes . . C13 C18 1.393(4) yes . . C14 C15 1.391(4) yes . . C15 C16 1.415(4) yes . . C16 C17 1.398(4) yes . . C17 C18 1.398(4) yes . . O1 H7 0.820 no . . O2 H8 0.820 no . . O3 H9 0.820 no . . O13 H10 0.771 no . . O13 H11 0.732 no . . O14 H12 0.783 no . . O14 H13 0.756 no . . O15 H14 0.773 no . . O15 H15 0.803 no . . O16 H16 0.756 no . . O16 H17 0.800 no . . O17 H18 0.845 no . . O17 H19 0.772 no . . O18 H20 0.765 no . . O18 H21 0.803 no . . O19 H22 0.733 no . . O19 H23 0.858 no . . O20 H24 0.811 no . . O20 H25 0.754 no . . O21 H26 0.725 no . . O21 H27 0.885 no . . O22 H28 0.800 no . . O22 H29 0.786 no . . O23 H30 0.887 no . . O23 H31 0.863 no . . O24 H32 0.904 no . . O24 H33 0.792 no . . O25 H34 0.799 no . . O25 H35 0.831 no . . O26 H36 0.765 no . . O26 H37 0.802 no . . C2 H1 0.930 no . . C6 H2 0.930 no . . C8 H3 0.930 no . . C12 H4 0.930 no . . C14 H5 0.930 no . . C18 H6 0.930 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O13 Eu1 O14 72.01(8) yes . . . O13 Eu1 O15 70.85(8) yes . . . O13 Eu1 O16 74.28(7) yes . . . O13 Eu1 O17 133.93(8) yes . . . O13 Eu1 O18 141.97(8) yes . . . O13 Eu1 O19 130.43(8) yes . . . O13 Eu1 O20 74.09(9) yes . . . O14 Eu1 O15 88.64(8) yes . . . O14 Eu1 O16 81.76(8) yes . . . O14 Eu1 O17 73.74(9) yes . . . O14 Eu1 O18 93.98(8) yes . . . O14 Eu1 O19 144.51(8) yes . . . O14 Eu1 O20 142.99(9) yes . . . O15 Eu1 O16 145.11(8) yes . . . O15 Eu1 O17 78.50(8) yes . . . O15 Eu1 O18 145.79(8) yes . . . O15 Eu1 O19 77.31(8) yes . . . O15 Eu1 O20 93.98(8) yes . . . O16 Eu1 O17 129.38(7) yes . . . O16 Eu1 O18 68.71(7) yes . . . O16 Eu1 O19 127.14(8) yes . . . O16 Eu1 O20 75.16(8) yes . . . O17 Eu1 O18 69.63(7) yes . . . O17 Eu1 O19 71.60(9) yes . . . O17 Eu1 O20 142.89(10) yes . . . O18 Eu1 O19 81.05(8) yes . . . O18 Eu1 O20 103.81(8) yes . . . O19 Eu1 O20 71.29(9) yes . . . C3 S1 C17 103.43(12) yes . . 3_666 C5 S2 C9 100.91(12) yes . . . C11 S3 C15 105.25(12) yes . . . O4 S4 O5 112.22(14) yes . . . O4 S4 O6 111.56(12) yes . . . O4 S4 C1 106.52(13) yes . . . O5 S4 O6 112.56(12) yes . . . O5 S4 C1 106.00(13) yes . . . O6 S4 C1 107.52(13) yes . . . O7 S5 O8 111.64(13) yes . . . O7 S5 O9 112.34(12) yes . . . O7 S5 C7 105.18(12) yes . . . O8 S5 O9 114.04(11) yes . . . O8 S5 C7 106.01(12) yes . . . O9 S5 C7 106.90(14) yes . . . O10 S6 O11 111.92(13) yes . . . O10 S6 O12 113.96(12) yes . . . O10 S6 C13 106.95(13) yes . . . O11 S6 O12 111.19(13) yes . . . O11 S6 C13 106.43(13) yes . . . O12 S6 C13 105.82(13) yes . . . S4 C1 C2 119.2(2) yes . . . S4 C1 C6 120.4(2) yes . . . C2 C1 C6 120.4(3) yes . . . C1 C2 C3 120.0(3) yes . . . S1 C3 C2 118.32(18) yes . . . S1 C3 C4 121.1(3) yes . . . C2 C3 C4 120.3(3) yes . . . O1 C4 C3 117.9(3) yes . . . O1 C4 C5 123.2(3) yes . . . C3 C4 C5 118.9(3) yes . . . S2 C5 C4 119.8(3) yes . . . S2 C5 C6 119.75(19) yes . . . C4 C5 C6 120.4(3) yes . . . C1 C6 C5 119.9(3) yes . . . S5 C7 C8 119.85(19) yes . . . S5 C7 C12 119.91(19) yes . . . C8 C7 C12 120.2(3) yes . . . C7 C8 C9 120.1(3) yes . . . S2 C9 C8 118.73(18) yes . . . S2 C9 C10 120.8(2) yes . . . C8 C9 C10 120.4(3) yes . . . O2 C10 C9 117.7(3) yes . . . O2 C10 C11 123.7(3) yes . . . C9 C10 C11 118.6(3) yes . . . S3 C11 C10 120.99(19) yes . . . S3 C11 C12 118.44(19) yes . . . C10 C11 C12 120.2(3) yes . . . C7 C12 C11 120.5(3) yes . . . S6 C13 C14 120.00(19) yes . . . S6 C13 C18 119.0(2) yes . . . C14 C13 C18 121.0(3) yes . . . C13 C14 C15 119.6(3) yes . . . S3 C15 C14 125.28(18) yes . . . S3 C15 C16 114.7(2) yes . . . C14 C15 C16 120.0(3) yes . . . O3 C16 C15 116.9(3) yes . . . O3 C16 C17 123.6(2) yes . . . C15 C16 C17 119.6(3) yes . . . S1 C17 C16 118.6(2) yes 3_666 . . S1 C17 C18 120.83(19) yes 3_666 . . C16 C17 C18 120.4(3) yes . . . C13 C18 C17 119.4(3) yes . . . C4 O1 H7 109.472 no . . . C10 O2 H8 109.483 no . . . C16 O3 H9 109.465 no . . . Eu1 O13 H10 122.013 no . . . Eu1 O13 H11 117.614 no . . . H10 O13 H11 109.315 no . . . Eu1 O14 H12 115.248 no . . . Eu1 O14 H13 124.212 no . . . H12 O14 H13 110.605 no . . . Eu1 O15 H14 124.150 no . . . Eu1 O15 H15 126.684 no . . . H14 O15 H15 109.139 no . . . Eu1 O16 H16 120.595 no . . . Eu1 O16 H17 126.534 no . . . H16 O16 H17 112.829 no . . . Eu1 O17 H18 110.364 no . . . Eu1 O17 H19 124.020 no . . . H18 O17 H19 111.851 no . . . Eu1 O18 H20 111.855 no . . . Eu1 O18 H21 123.263 no . . . H20 O18 H21 116.307 no . . . Eu1 O19 H22 123.603 no . . . Eu1 O19 H23 124.079 no . . . H22 O19 H23 109.477 no . . . Eu1 O20 H24 122.569 no . . . Eu1 O20 H25 120.459 no . . . H24 O20 H25 113.237 no . . . H26 O21 H27 110.000 no . . . H28 O22 H29 110.411 no . . . H30 O23 H31 101.709 no . . . H32 O24 H33 115.501 no . . . H34 O25 H35 110.500 no . . . H36 O26 H37 103.000 no . . . C1 C2 H1 120.018 no . . . C3 C2 H1 120.023 no . . . C1 C6 H2 120.039 no . . . C5 C6 H2 120.062 no . . . C7 C8 H3 119.971 no . . . C9 C8 H3 119.979 no . . . C7 C12 H4 119.749 no . . . C11 C12 H4 119.745 no . . . C13 C14 H5 120.205 no . . . C15 C14 H5 120.195 no . . . C13 C18 H6 120.299 no . . . C17 C18 H6 120.298 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C3 S1 C17 C16 100.31(19) no . . 3_666 3_666 C3 S1 C17 C18 -84.20(19) no . . 3_666 3_666 C17 S1 C3 C2 100.44(18) no 3_666 . . . C17 S1 C3 C4 -85.60(19) no 3_666 . . . C5 S2 C9 C8 116.76(19) no . . . . C5 S2 C9 C10 -65.3(2) no . . . . C9 S2 C5 C4 110.80(18) no . . . . C9 S2 C5 C6 -71.82(19) no . . . . C11 S3 C15 C14 13.2(3) no . . . . C11 S3 C15 C16 -168.34(15) no . . . . C15 S3 C11 C10 -85.81(19) no . . . . C15 S3 C11 C12 101.18(19) no . . . . O4 S4 C1 C2 -71.37(18) no . . . . O4 S4 C1 C6 107.40(18) no . . . . O5 S4 C1 C2 168.94(16) no . . . . O5 S4 C1 C6 -12.3(2) no . . . . O6 S4 C1 C2 48.3(2) no . . . . O6 S4 C1 C6 -132.89(17) no . . . . O7 S5 C7 C8 -79.8(2) no . . . . O7 S5 C7 C12 99.88(19) no . . . . O8 S5 C7 C8 161.82(18) no . . . . O8 S5 C7 C12 -18.5(3) no . . . . O9 S5 C7 C8 39.8(2) no . . . . O9 S5 C7 C12 -140.51(18) no . . . . O10 S6 C13 C14 -114.69(18) no . . . . O10 S6 C13 C18 64.4(2) no . . . . O11 S6 C13 C14 125.53(17) no . . . . O11 S6 C13 C18 -55.38(19) no . . . . O12 S6 C13 C14 7.2(2) no . . . . O12 S6 C13 C18 -173.75(17) no . . . . S4 C1 C2 C3 178.75(15) no . . . . S4 C1 C6 C5 -175.72(15) no . . . . C2 C1 C6 C5 3.0(4) no . . . . C6 C1 C2 C3 -0.0(4) no . . . . C1 C2 C3 S1 171.50(19) no . . . . C1 C2 C3 C4 -2.5(4) no . . . . S1 C3 C4 O1 7.6(3) no . . . . S1 C3 C4 C5 -171.85(15) no . . . . C2 C3 C4 O1 -178.5(2) no . . . . C2 C3 C4 C5 2.0(4) no . . . . O1 C4 C5 S2 -1.1(4) no . . . . O1 C4 C5 C6 -178.4(2) no . . . . C3 C4 C5 S2 178.41(18) no . . . . C3 C4 C5 C6 1.0(4) no . . . . S2 C5 C6 C1 179.09(15) no . . . . C4 C5 C6 C1 -3.5(4) no . . . . S5 C7 C8 C9 -179.15(16) no . . . . S5 C7 C12 C11 178.82(16) no . . . . C8 C7 C12 C11 -1.5(4) no . . . . C12 C7 C8 C9 1.2(4) no . . . . C7 C8 C9 S2 178.3(2) no . . . . C7 C8 C9 C10 0.3(4) no . . . . S2 C9 C10 O2 -0.1(4) no . . . . S2 C9 C10 C11 -179.28(16) no . . . . C8 C9 C10 O2 177.9(3) no . . . . C8 C9 C10 C11 -1.3(4) no . . . . O2 C10 C11 S3 9.0(4) no . . . . O2 C10 C11 C12 -178.1(3) no . . . . C9 C10 C11 S3 -171.9(2) no . . . . C9 C10 C11 C12 1.0(4) no . . . . S3 C11 C12 C7 173.46(16) no . . . . C10 C11 C12 C7 0.4(4) no . . . . S6 C13 C14 C15 178.70(15) no . . . . S6 C13 C18 C17 -179.48(15) no . . . . C14 C13 C18 C17 -0.4(4) no . . . . C18 C13 C14 C15 -0.4(4) no . . . . C13 C14 C15 S3 178.74(19) no . . . . C13 C14 C15 C16 0.4(4) no . . . . S3 C15 C16 O3 2.2(3) no . . . . S3 C15 C16 C17 -178.14(15) no . . . . C14 C15 C16 O3 -179.3(2) no . . . . C14 C15 C16 C17 0.4(4) no . . . . O3 C16 C17 S1 3.0(4) no . . . 3_666 O3 C16 C17 C18 178.47(19) no . . . . C15 C16 C17 S1 -176.67(18) no . . . 3_666 C15 C16 C17 C18 -1.2(4) no . . . . S1 C17 C18 C13 176.57(15) no 3_666 . . . C16 C17 C18 C13 1.2(4) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 O1 2.9824(18) no . . S1 O3 3.0321(19) no . 3_666 S2 O1 3.062(2) no . . S2 O2 2.9705(18) no . . S3 O2 3.103(2) no . . S3 O3 2.7987(18) no . . O1 O2 3.063(3) no . . O1 O3 2.943(3) no . 3_666 O1 C16 3.474(3) no . 3_666 O1 C17 3.524(3) no . 3_666 O2 C4 3.187(3) no . . O2 C5 3.124(3) no . . O2 C14 3.588(3) no . . O4 C2 3.249(4) no . . O4 C6 3.568(4) no . . O5 C6 2.892(4) no . . O6 C2 3.080(4) no . . O7 C8 3.318(4) no . . O7 C12 3.487(4) no . . O8 C12 2.899(4) no . . O9 C8 3.023(3) no . . O10 C18 3.196(4) no . . O11 C18 3.123(4) no . . O12 C14 2.883(4) no . . C1 C4 2.793(5) no . . C2 C5 2.788(4) no . . C3 C6 2.791(4) no . . C3 C18 3.540(4) no . 3_666 C4 C17 3.563(4) no . 3_666 C5 C10 3.291(3) no . . C6 C9 3.328(3) no . . C7 C10 2.801(4) no . . C8 C11 2.791(4) no . . C9 C12 2.786(4) no . . C10 C14 3.548(4) no . . C10 C15 3.590(3) no . . C11 C14 3.116(4) no . . C13 C16 2.789(4) no . . C14 C17 2.800(4) no . . C15 C18 2.804(4) no . . S1 S2 3.3561(8) no . 2_656 S1 C14 3.441(3) no . 4_555 S2 S1 3.3561(8) no . 2_646 S2 O9 3.413(3) no . 3_656 S2 C7 3.289(3) no . 3_656 S2 C8 3.285(3) no . 3_656 S3 O22 3.305(3) no . 3_666 S3 O24 3.497(3) no . 3_666 S3 O26 3.360(3) no . 3_666 S5 O18 3.555(3) no . 4_554 O1 O9 2.825(3) no . 3_656 O1 O10 3.307(4) no . 4_555 O1 C18 3.488(3) no . 4_555 O2 O9 3.476(4) no . 3_656 O2 O24 3.433(4) no . . O2 O26 2.682(3) no . 3_666 O2 O27A 3.421(5) no . 3_666 O3 O10 3.235(3) no . 2_555 O3 O22 3.114(3) no . 3_666 O3 O24 3.315(3) no . 3_666 O3 C1 3.598(3) no . 4_454 O3 C6 3.577(3) no . 4_454 O4 O15 2.795(4) no . 4_554 O4 O23 2.789(3) no . 1_655 O4 O27B 3.324(12) no . 3_666 O4 O28A 3.015(6) no . 3_666 O4 O28B 3.128(17) no . 3_666 O5 O10 3.530(4) no . 3_656 O5 O17 2.707(4) no . 2_646 O5 O21 2.735(3) no . 4_554 O6 O16 2.783(3) no . 1_655 O6 O18 3.487(3) no . 1_655 O6 O22 2.867(3) no . 2_646 O6 O23 3.363(4) no . 1_655 O7 O16 2.770(4) no . 3_656 O7 O17 3.301(3) no . 4_554 O7 O18 2.983(3) no . 4_554 O7 O21 3.286(3) no . 4_554 O7 O25 2.992(3) no . 3_656 O8 O13 2.720(4) no . 3_656 O8 O14 3.585(3) no . 3_656 O8 O18 3.429(3) no . 4_554 O8 C18 3.531(3) no . 2_545 O9 S2 3.413(3) no . 3_656 O9 O1 2.825(3) no . 3_656 O9 O2 3.476(4) no . 3_656 O9 O24 2.803(3) no . 3_656 O9 O25 3.404(4) no . 3_656 O10 O1 3.307(4) no . 4_454 O10 O3 3.235(3) no . 2_545 O10 O5 3.530(4) no . 3_656 O10 O14 2.708(3) no . 4_454 O11 O13 3.434(3) no . 4_454 O11 O15 2.854(4) no . 4_454 O11 O25 2.874(3) no . . O11 O28A 2.807(6) no . . O11 O28B 2.808(18) no . . O12 O21 2.735(4) no . 2_546 O12 O25 3.331(4) no . . O12 C8 3.255(3) no . 3_656 O13 O8 2.720(4) no . 3_656 O13 O11 3.434(3) no . 4_555 O13 O23 2.771(3) no . 2_546 O13 O28A 3.165(5) no . 4_555 O13 O28B 3.173(16) no . 4_555 O14 O8 3.585(3) no . 3_656 O14 O10 2.708(3) no . 4_555 O14 O22 2.700(3) no . . O15 O4 2.795(4) no . 4_455 O15 O11 2.854(4) no . 4_555 O16 O6 2.783(3) no . 1_455 O16 O7 2.770(4) no . 3_656 O16 O22 3.489(4) no . 2_546 O16 O23 3.335(3) no . . O17 O5 2.707(4) no . 2_656 O17 O7 3.301(3) no . 4_455 O17 O21 2.684(4) no . . O18 S5 3.555(3) no . 4_455 O18 O6 3.487(3) no . 1_455 O18 O7 2.983(3) no . 4_455 O18 O8 3.429(3) no . 4_455 O18 O23 2.759(3) no . . O18 C12 3.383(4) no . 4_455 O19 O21 2.736(3) no . . O19 O27A 2.702(4) no . 2_546 O19 O27B 2.828(12) no . 2_546 O19 C11 3.572(4) no . 4_455 O19 C12 3.511(3) no . 4_455 O20 O22 2.738(3) no . 2_546 O20 O23 3.358(4) no . 2_546 O20 O27A 2.701(5) no . 2_546 O20 O27B 2.733(13) no . 2_546 O21 O5 2.735(3) no . 4_455 O21 O7 3.286(3) no . 4_455 O21 O12 2.735(4) no . 2_556 O21 O17 2.684(4) no . . O21 O19 2.736(3) no . . O21 C6 3.490(4) no . 4_455 O21 C8 3.588(4) no . 4_455 O22 S3 3.305(3) no . 3_666 O22 O3 3.114(3) no . 3_666 O22 O6 2.867(3) no . 2_656 O22 O14 2.700(3) no . . O22 O16 3.489(4) no . 2_556 O22 O20 2.738(3) no . 2_556 O22 O24 2.793(4) no . . O23 O4 2.789(3) no . 1_455 O23 O6 3.363(4) no . 1_455 O23 O13 2.771(3) no . 2_556 O23 O16 3.335(3) no . . O23 O18 2.759(3) no . . O23 O20 3.358(4) no . 2_556 O23 O25 2.805(4) no . . O23 O28A 3.444(6) no . 3_566 O23 O28B 3.396(16) no . 3_566 O24 S3 3.497(3) no . 3_666 O24 O2 3.433(4) no . . O24 O3 3.315(3) no . 3_666 O24 O9 2.803(3) no . 3_656 O24 O22 2.793(4) no . . O24 O25 2.801(5) no . . O24 O26 2.682(4) no . . O25 O7 2.992(3) no . 3_656 O25 O9 3.404(4) no . 3_656 O25 O11 2.874(3) no . . O25 O12 3.331(4) no . . O25 O23 2.805(4) no . . O25 O24 2.801(5) no . . O26 S3 3.360(3) no . 3_666 O26 O2 2.682(3) no . 3_666 O26 O24 2.682(4) no . . O26 O26 3.270(5) no . 3_666 O26 O27A 2.685(5) no . . O26 O27B 3.032(15) no . . O26 C14 3.451(4) no . . O26 C15 3.334(4) no . . O26 C16 3.437(4) no . . O27A O2 3.421(5) no . 3_666 O27A O19 2.702(4) no . 2_556 O27A O20 2.701(5) no . 2_556 O27A O26 2.685(5) no . . O27A O28A 2.632(6) no . . O27A C10 3.539(5) no . 3_666 O27B O4 3.324(12) no . 3_666 O27B O19 2.828(12) no . 2_556 O27B O20 2.733(13) no . 2_556 O27B O26 3.032(15) no . . O27B O28B 2.30(3) no . . O27B C1 3.484(11) no . 3_666 O27B C2 3.512(12) no . 3_666 O28A O4 3.015(6) no . 3_666 O28A O11 2.807(6) no . . O28A O13 3.165(5) no . 4_454 O28A O23 3.444(6) no . 3_566 O28A O27A 2.632(6) no . . O28A C2 3.383(6) no . 3_666 O28A C18 3.398(7) no . . O28B O4 3.128(17) no . 3_666 O28B O11 2.808(18) no . . O28B O13 3.173(16) no . 4_454 O28B O23 3.396(16) no . 3_566 O28B O27B 2.30(3) no . . C1 O3 3.598(3) no . 4_555 C1 O27B 3.484(11) no . 3_666 C2 O27B 3.512(12) no . 3_666 C2 O28A 3.383(6) no . 3_666 C4 C17 3.592(4) no . 4_555 C5 C17 3.539(4) no . 4_555 C6 O3 3.577(3) no . 4_555 C6 O21 3.490(4) no . 4_554 C7 S2 3.289(3) no . 3_656 C8 S2 3.285(3) no . 3_656 C8 O12 3.255(3) no . 3_656 C8 O21 3.588(4) no . 4_554 C8 C9 3.438(4) no . 3_656 C9 C8 3.438(4) no . 3_656 C9 C9 3.525(4) no . 3_656 C10 O27A 3.539(5) no . 3_666 C11 O19 3.572(4) no . 4_554 C12 O18 3.383(4) no . 4_554 C12 O19 3.511(3) no . 4_554 C14 S1 3.441(3) no . 4_454 C14 O26 3.451(4) no . . C15 O26 3.334(4) no . . C16 O26 3.437(4) no . . C17 C4 3.592(4) no . 4_454 C17 C5 3.539(4) no . 4_454 C18 O1 3.488(3) no . 4_454 C18 O8 3.531(3) no . 2_555 C18 O28A 3.398(7) no . . S1 H1 2.8090 no . . S1 H6 2.8755 no . 3_666 S1 H9 2.5226 no . 3_666 S2 H2 2.8369 no . . S2 H3 2.8122 no . . S2 H7 2.5476 no . . S3 H4 2.7998 no . . S3 H5 2.9566 no . . S3 H8 2.6798 no . . S4 H1 2.8199 no . . S4 H2 2.8394 no . . S5 H3 2.8355 no . . S5 H4 2.8218 no . . S6 H5 2.8506 no . . S6 H6 2.8243 no . . O1 H8 3.4238 no . . O1 H9 2.3849 no . 3_666 O2 H5 3.0743 no . . O2 H7 2.7442 no . . O3 H7 3.4390 no . 3_666 O4 H1 3.1586 no . . O5 H2 2.5052 no . . O6 H1 2.8356 no . . O7 H3 3.2736 no . . O7 H4 3.5520 no . . O8 H4 2.5269 no . . O9 H3 2.7489 no . . O10 H6 3.0587 no . . O11 H6 2.9223 no . . O12 H5 2.4956 no . . O13 H12 3.5476 no . . O13 H13 2.9025 no . . O13 H14 2.7581 no . . O13 H15 3.4875 no . . O13 H16 2.8401 no . . O13 H24 3.1797 no . . O13 H25 3.4336 no . . O14 H10 2.6947 no . . O14 H11 3.5244 no . . O14 H14 3.3389 no . . O14 H16 3.0805 no . . O14 H18 2.6533 no . . O15 H10 3.3678 no . . O15 H11 3.1352 no . . O15 H13 3.2677 no . . O15 H18 3.0510 no . . O15 H19 3.3244 no . . O15 H22 3.2633 no . . O15 H23 3.3136 no . . O15 H25 3.5883 no . . O16 H10 2.9943 no . . O16 H11 3.1309 no . . O16 H12 3.3518 no . . O16 H20 3.4670 no . . O16 H21 2.5783 no . . O16 H24 2.7566 no . . O17 H12 2.8432 no . . O17 H13 3.1936 no . . O17 H14 3.5221 no . . O17 H15 3.3511 no . . O17 H20 2.4641 no . . O17 H21 3.3768 no . . O17 H22 2.6654 no . . O18 H12 3.3373 no . . O18 H16 3.3389 no . . O18 H17 2.7649 no . . O18 H18 3.4281 no . . O18 H19 3.0918 no . . O18 H22 3.3402 no . . O19 H15 2.9148 no . . O19 H18 3.5338 no . . O19 H19 2.6756 no . . O19 H20 3.0762 no . . O19 H24 3.4700 no . . O19 H25 2.6254 no . . O20 H10 3.5496 no . . O20 H11 2.6688 no . . O20 H16 3.4401 no . . O20 H17 3.0917 no . . O20 H22 3.5299 no . . O20 H23 2.6703 no . . C2 H2 3.2547 no . . C3 H6 3.5048 no . 3_666 C3 H7 3.0412 no . . C3 H9 3.3578 no . 3_666 C4 H1 3.2609 no . . C4 H2 3.2660 no . . C4 H8 3.5072 no . . C4 H9 3.2958 no . 3_666 C5 H7 2.4253 no . . C6 H1 3.2537 no . . C8 H2 3.5422 no . . C8 H4 3.2454 no . . C9 H2 3.2277 no . . C9 H8 3.0062 no . . C10 H3 3.2697 no . . C10 H4 3.2658 no . . C10 H5 2.9143 no . . C11 H5 2.7050 no . . C11 H8 2.4871 no . . C12 H3 3.2449 no . . C12 H5 3.4897 no . . C14 H6 3.2679 no . . C14 H8 3.5529 no . . C15 H8 3.3489 no . . C15 H9 3.0436 no . . C16 H5 3.2715 no . . C16 H6 3.2652 no . . C17 H9 2.4314 no . . C18 H5 3.2664 no . . H1 H6 3.1794 no . 3_666 H2 H3 3.4414 no . . H5 H8 3.2385 no . . H7 H8 3.2623 no . . H7 H9 2.9585 no . 3_666 H10 H12 3.4074 no . . H10 H13 2.7239 no . . H10 H14 3.2186 no . . H10 H16 2.7238 no . . H11 H14 3.1294 no . . H11 H16 3.0684 no . . H11 H24 2.8743 no . . H11 H25 3.1725 no . . H12 H16 3.3169 no . . H12 H18 2.6025 no . . H12 H20 3.5679 no . . H12 H21 3.3889 no . . H13 H14 3.1063 no . . H13 H18 2.7914 no . . H14 H18 3.3393 no . . H15 H18 3.3918 no . . H15 H19 3.4340 no . . H15 H22 3.0765 no . . H15 H23 3.0883 no . . H16 H21 3.1202 no . . H16 H24 3.2350 no . . H17 H20 3.5295 no . . H17 H21 2.5152 no . . H17 H24 2.7612 no . . H18 H20 3.1800 no . . H18 H22 3.3669 no . . H19 H20 2.6565 no . . H19 H22 2.3142 no . . H19 H23 3.4828 no . . H20 H22 3.1158 no . . H22 H25 3.3421 no . . H23 H24 3.3352 no . . H23 H25 2.2769 no . . S1 H5 3.3790 no . 4_555 S2 H3 3.4975 no . 3_656 S3 H24 3.5329 no . 4_554 S3 H25 3.5949 no . 4_554 S3 H28 3.0004 no . 3_666 S3 H29 3.0209 no . 3_666 S3 H36 3.2159 no . 3_666 S3 H37 3.4459 no . . S4 H15 3.2108 no . 4_554 S4 H17 3.1154 no . 1_655 S4 H18 2.9707 no . 2_646 S4 H27 3.0579 no . 4_554 S4 H28 3.0834 no . 2_646 S4 H31 2.8262 no . 1_655 S5 H7 3.1885 no . 3_656 S5 H10 2.9465 no . 3_656 S5 H16 3.1348 no . 3_656 S5 H20 2.9595 no . 4_554 S5 H34 3.0830 no . 3_656 S6 H13 3.1009 no . 4_454 S6 H14 3.1690 no . 4_454 S6 H26 3.0046 no . 2_546 S6 H27 3.5707 no . 2_546 S6 H35 2.8959 no . . O1 H6 3.5162 no . 4_555 O1 H33 2.9414 no . . O2 H33 2.9571 no . . O2 H36 3.4993 no . . O2 H36 3.2428 no . 3_666 O2 H37 3.1131 no . 3_666 O3 H28 2.8529 no . 3_666 O3 H29 2.6808 no . 3_666 O3 H33 2.9815 no . 3_666 O3 H37 3.4307 no . . O4 H14 3.1189 no . 4_554 O4 H15 1.9965 no . 4_554 O4 H17 3.4974 no . 1_655 O4 H22 3.5842 no . 4_554 O4 H23 3.4156 no . 4_554 O4 H27 3.4848 no . 4_554 O4 H30 3.0831 no . 1_655 O4 H31 1.9308 no . 1_655 O5 H12 3.4439 no . 2_646 O5 H13 3.4096 no . 2_646 O5 H15 3.4500 no . 4_554 O5 H18 1.9122 no . 2_646 O5 H19 2.9275 no . 2_646 O5 H22 3.5245 no . 4_554 O5 H26 3.0452 no . 4_554 O5 H27 1.8828 no . 4_554 O5 H28 3.1744 no . 2_646 O6 H4 3.3485 no . 4_555 O6 H16 3.2376 no . 1_655 O6 H17 1.9941 no . 1_655 O6 H18 3.2283 no . 2_646 O6 H21 3.1553 no . 1_655 O6 H24 3.4589 no . 1_655 O6 H28 2.1164 no . 2_646 O6 H29 3.3954 no . 2_646 O6 H31 2.7571 no . 1_655 O7 H10 3.0750 no . 3_656 O7 H16 2.0147 no . 3_656 O7 H17 3.1442 no . 3_656 O7 H19 2.9910 no . 4_554 O7 H20 2.2362 no . 4_554 O7 H21 3.3668 no . 4_554 O7 H26 3.1582 no . 4_554 O7 H34 2.2180 no . 3_656 O7 H35 3.5114 no . 3_656 O8 H1 3.2548 no . 4_454 O8 H6 2.6555 no . 2_545 O8 H7 3.4413 no . 3_656 O8 H10 1.9577 no . 3_656 O8 H11 2.9615 no . 3_656 O8 H13 3.4731 no . 3_656 O8 H16 3.4111 no . 3_656 O8 H20 3.0456 no . 4_554 O8 H21 3.3874 no . 4_554 O9 H7 2.1180 no . 3_656 O9 H32 2.7233 no . 3_656 O9 H33 2.2540 no . 3_656 O9 H34 2.9468 no . 3_656 O10 H2 3.3648 no . 3_656 O10 H9 2.5868 no . 2_545 O10 H12 3.0363 no . 4_454 O10 H13 1.9536 no . 4_454 O10 H14 3.4161 no . 4_454 O10 H26 3.5349 no . 2_546 O10 H27 3.5948 no . 2_546 O11 H10 3.4763 no . 4_454 O11 H13 3.2802 no . 4_454 O11 H14 2.0880 no . 4_454 O11 H15 3.2835 no . 4_454 O11 H26 3.3049 no . 2_546 O11 H34 3.2536 no . . O11 H35 2.0442 no . . O12 H2 2.8134 no . 3_656 O12 H3 2.4845 no . 3_656 O12 H26 2.0421 no . 2_546 O12 H27 2.9699 no . 2_546 O12 H34 3.1783 no . . O12 H35 2.7914 no . . O13 H21 3.3900 no . 2_546 O13 H30 3.3572 no . 2_546 O13 H31 3.2810 no . 2_546 O14 H28 2.9910 no . . O14 H29 2.8656 no . . O15 H35 3.5446 no . 4_555 O16 H20 3.3706 no . 2_546 O16 H28 3.2695 no . 2_546 O16 H30 3.2611 no . . O16 H31 3.3060 no . . O16 H34 3.3009 no . . O17 H16 3.4760 no . 2_556 O17 H17 3.4576 no . 2_556 O17 H26 3.2549 no . . O17 H27 3.0629 no . . O17 H27 3.5339 no . 3_667 O18 H4 2.9809 no . 4_455 O18 H10 3.5992 no . 2_556 O18 H11 3.4734 no . 2_556 O18 H16 3.4677 no . 2_556 O18 H30 3.2217 no . . O18 H31 3.1311 no . . O19 H2 3.5041 no . 4_455 O19 H26 3.2129 no . . O19 H27 3.0558 no . . O20 H28 2.9899 no . 2_546 O20 H29 3.0104 no . 2_546 O20 H30 3.1796 no . 2_546 O21 H2 2.6892 no . 4_455 O21 H3 3.4033 no . 4_455 O21 H18 3.1507 no . . O21 H19 1.9356 no . . O21 H22 2.0273 no . . O21 H23 3.2393 no . . O21 H34 3.2294 no . 2_556 O21 H35 3.5270 no . 2_556 O22 H9 3.4955 no . 3_666 O22 H12 1.9236 no . . O22 H13 2.9880 no . . O22 H17 3.0952 no . 2_556 O22 H18 3.4874 no . . O22 H24 1.9405 no . 2_556 O22 H25 3.0291 no . 2_556 O22 H30 3.4960 no . . O22 H32 2.8537 no . . O22 H33 3.0414 no . . O23 H10 2.9941 no . 2_556 O23 H11 2.0540 no . 2_556 O23 H16 3.5564 no . . O23 H17 3.0907 no . . O23 H20 3.1283 no . . O23 H21 1.9597 no . . O23 H24 3.2112 no . 2_556 O23 H34 3.2008 no . . O23 H35 3.1858 no . . O24 H7 3.4512 no . . O24 H8 3.4830 no . . O24 H24 3.4497 no . 2_556 O24 H25 3.5793 no . 2_556 O24 H28 3.3196 no . . O24 H29 2.0598 no . . O24 H34 3.0669 no . . O24 H35 3.0774 no . . O24 H36 1.9307 no . . O24 H37 3.0415 no . . O25 H14 3.5056 no . 4_454 O25 H16 3.3004 no . . O25 H26 3.2973 no . 2_546 O25 H29 3.4110 no . . O25 H30 1.9306 no . . O25 H31 2.9938 no . . O25 H32 1.8988 no . . O25 H33 3.2116 no . . O26 H8 3.4905 no . . O26 H8 1.9237 no . 3_666 O26 H32 3.1199 no . . O26 H33 3.1674 no . . O26 H36 3.1736 no . 3_666 O26 H37 3.2370 no . 3_666 O27A H8 3.0040 no . 3_666 O27A H22 3.1633 no . 2_556 O27A H23 1.8841 no . 2_556 O27A H24 3.1951 no . 2_556 O27A H25 1.9637 no . 2_556 O27A H36 2.9510 no . . O27A H37 3.2047 no . . O27B H8 3.5157 no . 3_666 O27B H15 3.5426 no . 2_556 O27B H22 3.2882 no . 2_556 O27B H23 2.0548 no . 2_556 O27B H24 3.2868 no . 2_556 O27B H25 2.0117 no . 2_556 O27B H36 3.2678 no . . O27B H37 3.4709 no . . O28A H1 3.0782 no . 3_666 O28A H6 2.8738 no . . O28A H10 3.1625 no . 4_454 O28A H11 3.0193 no . 4_454 O28A H14 3.5982 no . 4_454 O28A H25 3.5188 no . 2_556 O28A H31 3.1052 no . 3_566 O28B H10 3.3817 no . 4_454 O28B H11 2.9735 no . 4_454 O28B H14 3.1852 no . 4_454 O28B H15 3.3514 no . 2_556 O28B H25 3.1705 no . 2_556 O28B H31 3.1200 no . 3_566 O28B H35 3.3961 no . . C1 H23 3.5590 no . 4_554 C2 H4 3.1245 no . 4_555 C6 H9 3.5746 no . 4_555 C6 H22 3.3516 no . 4_554 C6 H23 3.3188 no . 4_554 C6 H26 3.4717 no . 4_554 C6 H27 3.2370 no . 4_554 C7 H20 3.2478 no . 4_554 C7 H22 3.3905 no . 4_554 C8 H22 3.3537 no . 4_554 C8 H26 3.2301 no . 4_554 C9 H3 3.3973 no . 3_656 C9 H22 3.5347 no . 4_554 C9 H23 3.5300 no . 4_554 C10 H3 3.5486 no . 3_656 C10 H23 3.3099 no . 4_554 C11 H23 3.3502 no . 4_554 C12 H1 3.1808 no . 4_454 C12 H20 3.2638 no . 4_554 C12 H22 3.5816 no . 4_554 C13 H37 3.0799 no . . C14 H36 3.4301 no . . C14 H37 2.7485 no . . C15 H36 3.5294 no . . C15 H37 2.5364 no . . C16 H37 2.6934 no . . C17 H37 3.0228 no . . C18 H37 3.2177 no . . H1 O8 3.2548 no . 4_555 H1 O28A 3.0782 no . 3_666 H1 C12 3.1808 no . 4_555 H1 H4 2.3623 no . 4_555 H1 H31 3.5453 no . 1_655 H2 O10 3.3648 no . 3_656 H2 O12 2.8134 no . 3_656 H2 O19 3.5041 no . 4_554 H2 O21 2.6892 no . 4_554 H2 H9 3.5193 no . 4_555 H2 H22 2.9803 no . 4_554 H2 H23 3.3086 no . 4_554 H2 H26 2.5921 no . 4_554 H2 H27 2.4774 no . 4_554 H3 S2 3.4975 no . 3_656 H3 O12 2.4845 no . 3_656 H3 O21 3.4033 no . 4_554 H3 C9 3.3973 no . 3_656 H3 C10 3.5486 no . 3_656 H3 H5 3.0497 no . 3_656 H3 H26 2.8885 no . 4_554 H3 H34 3.5676 no . 3_656 H4 O6 3.3485 no . 4_454 H4 O18 2.9809 no . 4_554 H4 C2 3.1245 no . 4_454 H4 H1 2.3623 no . 4_454 H4 H20 2.9851 no . 4_554 H4 H21 3.1659 no . 4_554 H5 S1 3.3790 no . 4_454 H5 H3 3.0497 no . 3_656 H5 H37 3.2354 no . . H6 O1 3.5162 no . 4_454 H6 O8 2.6555 no . 2_555 H6 O28A 2.8738 no . . H6 H7 3.4601 no . 4_454 H6 H10 3.3321 no . 4_454 H7 S5 3.1885 no . 3_656 H7 O8 3.4413 no . 3_656 H7 O9 2.1180 no . 3_656 H7 O24 3.4512 no . . H7 H6 3.4601 no . 4_555 H7 H33 2.6604 no . . H8 O24 3.4830 no . . H8 O26 3.4905 no . . H8 O26 1.9237 no . 3_666 H8 O27A 3.0040 no . 3_666 H8 O27B 3.5157 no . 3_666 H8 H33 3.1122 no . . H8 H36 3.1496 no . . H8 H36 2.4354 no . 3_666 H8 H37 3.2155 no . . H8 H37 2.4443 no . 3_666 H9 O10 2.5868 no . 2_555 H9 O22 3.4955 no . 3_666 H9 C6 3.5746 no . 4_454 H9 H2 3.5193 no . 4_454 H9 H13 3.3409 no . 3_666 H9 H28 3.2996 no . 3_666 H9 H29 3.0677 no . 3_666 H9 H33 3.1363 no . 3_666 H10 S5 2.9465 no . 3_656 H10 O7 3.0750 no . 3_656 H10 O8 1.9577 no . 3_656 H10 O11 3.4763 no . 4_555 H10 O18 3.5992 no . 2_546 H10 O23 2.9941 no . 2_546 H10 O28A 3.1625 no . 4_555 H10 O28B 3.3817 no . 4_555 H10 H6 3.3321 no . 4_555 H10 H20 3.2965 no . 2_546 H10 H21 3.2401 no . 2_546 H10 H31 3.4251 no . 2_546 H11 O8 2.9615 no . 3_656 H11 O18 3.4734 no . 2_546 H11 O23 2.0540 no . 2_546 H11 O28A 3.0193 no . 4_555 H11 O28B 2.9735 no . 4_555 H11 H20 3.3741 no . 2_546 H11 H21 2.9066 no . 2_546 H11 H30 2.6294 no . 2_546 H11 H31 2.5985 no . 2_546 H12 O5 3.4439 no . 2_656 H12 O10 3.0363 no . 4_555 H12 O22 1.9236 no . . H12 H28 2.2539 no . . H12 H29 2.1583 no . . H12 H32 3.5762 no . . H12 H33 3.5801 no . . H13 S6 3.1009 no . 4_555 H13 O5 3.4096 no . 2_656 H13 O8 3.4731 no . 3_656 H13 O10 1.9536 no . 4_555 H13 O11 3.2802 no . 4_555 H13 O22 2.9880 no . . H13 H9 3.3409 no . 3_666 H13 H28 3.1530 no . . H13 H29 3.0543 no . . H14 S6 3.1690 no . 4_555 H14 O4 3.1189 no . 4_455 H14 O10 3.4161 no . 4_555 H14 O11 2.0880 no . 4_555 H14 O25 3.5056 no . 4_555 H14 O28A 3.5982 no . 4_555 H14 O28B 3.1852 no . 4_555 H14 H26 3.5703 no . 3_667 H14 H27 3.5103 no . 3_667 H14 H35 2.8903 no . 4_555 H15 S4 3.2108 no . 4_455 H15 O4 1.9965 no . 4_455 H15 O5 3.4500 no . 4_455 H15 O11 3.2835 no . 4_555 H15 O27B 3.5426 no . 2_546 H15 O28B 3.3514 no . 2_546 H15 H27 3.5534 no . . H15 H31 3.0644 no . 4_555 H15 H35 3.5040 no . 4_555 H16 S5 3.1348 no . 3_656 H16 O6 3.2376 no . 1_455 H16 O7 2.0147 no . 3_656 H16 O8 3.4111 no . 3_656 H16 O17 3.4760 no . 2_546 H16 O18 3.4677 no . 2_546 H16 O23 3.5564 no . . H16 O25 3.3004 no . . H16 H19 3.4561 no . 2_546 H16 H20 2.8438 no . 2_546 H16 H21 3.5513 no . 2_546 H16 H30 3.2940 no . . H16 H31 3.5283 no . . H16 H34 2.7981 no . . H17 S4 3.1154 no . 1_455 H17 O4 3.4974 no . 1_455 H17 O6 1.9941 no . 1_455 H17 O7 3.1442 no . 3_656 H17 O17 3.4576 no . 2_546 H17 O22 3.0952 no . 2_546 H17 O23 3.0907 no . . H17 H18 3.4599 no . 2_546 H17 H19 3.5692 no . 2_546 H17 H20 3.5517 no . 2_546 H17 H28 2.7278 no . 2_546 H17 H30 3.1432 no . . H17 H31 2.8772 no . . H17 H34 3.4397 no . . H18 S4 2.9707 no . 2_656 H18 O5 1.9122 no . 2_656 H18 O6 3.2283 no . 2_656 H18 O21 3.1507 no . . H18 O22 3.4874 no . . H18 H17 3.4599 no . 2_556 H18 H27 3.3629 no . . H18 H27 2.8352 no . 3_667 H18 H28 3.2449 no . . H19 O5 2.9275 no . 2_656 H19 O7 2.9910 no . 4_455 H19 O21 1.9356 no . . H19 H16 3.4561 no . 2_556 H19 H17 3.5692 no . 2_556 H19 H26 2.4915 no . . H19 H27 2.3720 no . . H19 H27 3.5946 no . 3_667 H19 H34 3.5976 no . 2_556 H20 S5 2.9595 no . 4_455 H20 O7 2.2361 no . 4_455 H20 O8 3.0456 no . 4_455 H20 O16 3.3706 no . 2_556 H20 O23 3.1283 no . . H20 C7 3.2478 no . 4_455 H20 C12 3.2638 no . 4_455 H20 H4 2.9851 no . 4_455 H20 H10 3.2965 no . 2_556 H20 H11 3.3741 no . 2_556 H20 H16 2.8438 no . 2_556 H20 H17 3.5517 no . 2_556 H20 H31 3.5905 no . . H21 O6 3.1553 no . 1_455 H21 O7 3.3668 no . 4_455 H21 O8 3.3874 no . 4_455 H21 O13 3.3900 no . 2_556 H21 O23 1.9597 no . . H21 H4 3.1659 no . 4_455 H21 H10 3.2401 no . 2_556 H21 H11 2.9066 no . 2_556 H21 H16 3.5513 no . 2_556 H21 H30 2.4560 no . . H21 H31 2.3484 no . . H22 O4 3.5842 no . 4_455 H22 O5 3.5245 no . 4_455 H22 O21 2.0273 no . . H22 O27A 3.1633 no . 2_546 H22 O27B 3.2882 no . 2_546 H22 C6 3.3516 no . 4_455 H22 C7 3.3905 no . 4_455 H22 C8 3.3537 no . 4_455 H22 C9 3.5347 no . 4_455 H22 C12 3.5816 no . 4_455 H22 H2 2.9803 no . 4_455 H22 H26 2.4837 no . . H22 H27 2.3969 no . . H23 O4 3.4156 no . 4_455 H23 O21 3.2393 no . . H23 O27A 1.8841 no . 2_546 H23 O27B 2.0548 no . 2_546 H23 C1 3.5590 no . 4_455 H23 C6 3.3188 no . 4_455 H23 C9 3.5300 no . 4_455 H23 C10 3.3099 no . 4_455 H23 C11 3.3502 no . 4_455 H23 H2 3.3086 no . 4_455 H23 H27 3.4414 no . . H24 S3 3.5329 no . 4_455 H24 O6 3.4589 no . 1_455 H24 O22 1.9405 no . 2_546 H24 O23 3.2112 no . 2_546 H24 O24 3.4497 no . 2_546 H24 O27A 3.1951 no . 2_546 H24 O27B 3.2868 no . 2_546 H24 H28 2.2347 no . 2_546 H24 H29 2.2833 no . 2_546 H24 H30 2.9709 no . 2_546 H24 H32 3.2898 no . 2_546 H25 S3 3.5949 no . 4_455 H25 O22 3.0291 no . 2_546 H25 O24 3.5793 no . 2_546 H25 O27A 1.9637 no . 2_546 H25 O27B 2.0117 no . 2_546 H25 O28A 3.5188 no . 2_546 H25 O28B 3.1705 no . 2_546 H25 H28 3.3279 no . 2_546 H25 H29 3.1144 no . 2_546 H25 H30 3.3633 no . 2_546 H25 H32 3.4172 no . 2_546 H26 S6 3.0046 no . 2_556 H26 O5 3.0452 no . 4_455 H26 O7 3.1582 no . 4_455 H26 O10 3.5349 no . 2_556 H26 O11 3.3049 no . 2_556 H26 O12 2.0421 no . 2_556 H26 O17 3.2549 no . . H26 O19 3.2129 no . . H26 O25 3.2973 no . 2_556 H26 C6 3.4717 no . 4_455 H26 C8 3.2301 no . 4_455 H26 H2 2.5921 no . 4_455 H26 H3 2.8885 no . 4_455 H26 H14 3.5703 no . 3_667 H26 H19 2.4915 no . . H26 H22 2.4837 no . . H26 H34 2.8211 no . 2_556 H26 H35 3.0188 no . 2_556 H27 S4 3.0579 no . 4_455 H27 S6 3.5707 no . 2_556 H27 O4 3.4848 no . 4_455 H27 O5 1.8828 no . 4_455 H27 O10 3.5948 no . 2_556 H27 O12 2.9699 no . 2_556 H27 O17 3.0629 no . . H27 O17 3.5339 no . 3_667 H27 O19 3.0558 no . . H27 C6 3.2370 no . 4_455 H27 H2 2.4774 no . 4_455 H27 H14 3.5103 no . 3_667 H27 H15 3.5534 no . . H27 H18 3.3629 no . . H27 H18 2.8352 no . 3_667 H27 H19 2.3720 no . . H27 H19 3.5946 no . 3_667 H27 H22 2.3969 no . . H27 H23 3.4414 no . . H28 S3 3.0004 no . 3_666 H28 S4 3.0834 no . 2_656 H28 O3 2.8529 no . 3_666 H28 O5 3.1744 no . 2_656 H28 O6 2.1164 no . 2_656 H28 O14 2.9910 no . . H28 O16 3.2695 no . 2_556 H28 O20 2.9899 no . 2_556 H28 O24 3.3196 no . . H28 H9 3.2996 no . 3_666 H28 H12 2.2539 no . . H28 H13 3.1530 no . . H28 H17 2.7278 no . 2_556 H28 H18 3.2449 no . . H28 H24 2.2347 no . 2_556 H28 H25 3.3279 no . 2_556 H28 H32 3.5278 no . . H28 H33 3.5112 no . . H29 S3 3.0209 no . 3_666 H29 O3 2.6808 no . 3_666 H29 O6 3.3954 no . 2_656 H29 O14 2.8656 no . . H29 O20 3.0104 no . 2_556 H29 O24 2.0598 no . . H29 O25 3.4110 no . . H29 H9 3.0677 no . 3_666 H29 H12 2.1583 no . . H29 H13 3.0543 no . . H29 H24 2.2833 no . 2_556 H29 H25 3.1144 no . 2_556 H29 H32 2.2579 no . . H29 H33 2.2740 no . . H29 H36 3.4685 no . . H30 O4 3.0831 no . 1_455 H30 O13 3.3572 no . 2_556 H30 O16 3.2611 no . . H30 O18 3.2217 no . . H30 O20 3.1796 no . 2_556 H30 O22 3.4960 no . . H30 O25 1.9306 no . . H30 H11 2.6294 no . 2_556 H30 H16 3.2940 no . . H30 H17 3.1432 no . . H30 H21 2.4560 no . . H30 H24 2.9709 no . 2_556 H30 H25 3.3633 no . 2_556 H30 H32 3.2607 no . . H30 H34 2.3882 no . . H30 H35 2.3513 no . . H31 S4 2.8262 no . 1_455 H31 O4 1.9308 no . 1_455 H31 O6 2.7571 no . 1_455 H31 O13 3.2810 no . 2_556 H31 O16 3.3060 no . . H31 O18 3.1311 no . . H31 O25 2.9938 no . . H31 O28A 3.1052 no . 3_566 H31 O28B 3.1200 no . 3_566 H31 H1 3.5453 no . 1_455 H31 H10 3.4251 no . 2_556 H31 H11 2.5985 no . 2_556 H31 H15 3.0644 no . 4_454 H31 H16 3.5283 no . . H31 H17 2.8772 no . . H31 H20 3.5905 no . . H31 H21 2.3484 no . . H31 H34 3.2781 no . . H31 H35 3.2694 no . . H32 O9 2.7233 no . 3_656 H32 O22 2.8537 no . . H32 O25 1.8988 no . . H32 O26 3.1199 no . . H32 H12 3.5762 no . . H32 H24 3.2898 no . 2_556 H32 H25 3.4172 no . 2_556 H32 H28 3.5278 no . . H32 H29 2.2579 no . . H32 H30 3.2607 no . . H32 H34 2.2101 no . . H32 H35 2.2030 no . . H32 H36 2.4305 no . . H32 H37 3.4120 no . . H33 O1 2.9414 no . . H33 O2 2.9571 no . . H33 O3 2.9815 no . 3_666 H33 O9 2.2540 no . 3_656 H33 O22 3.0414 no . . H33 O25 3.2116 no . . H33 O26 3.1674 no . . H33 H7 2.6604 no . . H33 H8 3.1122 no . . H33 H9 3.1363 no . 3_666 H33 H12 3.5801 no . . H33 H28 3.5112 no . . H33 H29 2.2740 no . . H33 H34 3.2966 no . . H33 H35 3.5581 no . . H33 H36 2.4046 no . . H33 H37 3.4473 no . . H34 S5 3.0830 no . 3_656 H34 O7 2.2180 no . 3_656 H34 O9 2.9468 no . 3_656 H34 O11 3.2536 no . . H34 O12 3.1783 no . . H34 O16 3.3009 no . . H34 O21 3.2294 no . 2_546 H34 O23 3.2008 no . . H34 O24 3.0669 no . . H34 H3 3.5676 no . 3_656 H34 H16 2.7981 no . . H34 H17 3.4397 no . . H34 H19 3.5976 no . 2_546 H34 H26 2.8211 no . 2_546 H34 H30 2.3882 no . . H34 H31 3.2781 no . . H34 H32 2.2101 no . . H34 H33 3.2966 no . . H35 S6 2.8959 no . . H35 O7 3.5114 no . 3_656 H35 O11 2.0442 no . . H35 O12 2.7914 no . . H35 O15 3.5446 no . 4_454 H35 O21 3.5270 no . 2_546 H35 O23 3.1858 no . . H35 O24 3.0774 no . . H35 O28B 3.3961 no . . H35 H14 2.8903 no . 4_454 H35 H15 3.5040 no . 4_454 H35 H26 3.0188 no . 2_546 H35 H30 2.3513 no . . H35 H31 3.2694 no . . H35 H32 2.2030 no . . H35 H33 3.5581 no . . H36 S3 3.2159 no . 3_666 H36 O2 3.4993 no . . H36 O2 3.2428 no . 3_666 H36 O24 1.9307 no . . H36 O26 3.1736 no . 3_666 H36 O27A 2.9510 no . . H36 O27B 3.2678 no . . H36 C14 3.4301 no . . H36 C15 3.5294 no . . H36 H8 3.1496 no . . H36 H8 2.4354 no . 3_666 H36 H29 3.4685 no . . H36 H32 2.4305 no . . H36 H33 2.4046 no . . H36 H36 3.2595 no . 3_666 H36 H37 3.0957 no . 3_666 H37 S3 3.4459 no . . H37 O2 3.1131 no . 3_666 H37 O3 3.4307 no . . H37 O24 3.0415 no . . H37 O26 3.2370 no . 3_666 H37 O27A 3.2047 no . . H37 O27B 3.4709 no . . H37 C13 3.0799 no . . H37 C14 2.7485 no . . H37 C15 2.5364 no . . H37 C16 2.6934 no . . H37 C17 3.0228 no . . H37 C18 3.2177 no . . H37 H5 3.2354 no . . H37 H8 3.2155 no . . H37 H8 2.4443 no . 3_666 H37 H32 3.4120 no . . H37 H33 3.4473 no . . H37 H36 3.0957 no . 3_666 H37 H37 3.3987 no . 3_666 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H7 S2 . . . 3.062(2) 0.820 2.548 121.9 no O1 H7 O9 . . 3_656 2.825(3) 0.820 2.118 144.3 no O2 H8 S3 . . . 3.103(2) 0.820 2.680 113.8 no O2 H8 O26 . . 3_666 2.682(3) 0.820 1.924 153.4 no O3 H9 S1 . . 3_666 3.0321(19) 0.820 2.523 121.4 no O3 H9 O1 . . 3_666 2.943(3) 0.820 2.385 126.1 no O13 H10 O8 . . 3_656 2.720(4) 0.771 1.958 169.9 no O13 H11 O23 . . 2_546 2.771(3) 0.732 2.054 166.4 no O14 H12 O22 . . . 2.700(3) 0.783 1.924 170.8 no O14 H13 O10 . . 4_555 2.708(3) 0.756 1.954 175.5 no O15 H14 O11 . . 4_555 2.854(4) 0.773 2.088 170.5 no O15 H15 O4 . . 4_455 2.795(4) 0.803 1.997 172.9 no O16 H16 O7 . . 3_656 2.770(4) 0.756 2.015 176.9 no O16 H17 O6 . . 1_455 2.783(3) 0.800 1.994 168.7 no O17 H18 O5 . . 2_656 2.707(4) 0.845 1.912 156.2 no O17 H19 O21 . . . 2.684(4) 0.772 1.936 163.3 no O18 H20 O7 . . 4_455 2.983(3) 0.765 2.236 165.5 no O18 H21 O23 . . . 2.759(3) 0.803 1.960 173.4 no O19 H22 O21 . . . 2.736(3) 0.733 2.027 162.8 no O19 H23 O27A . . 2_546 2.702(4) 0.858 1.884 159.0 no O19 H23 O27B . . 2_546 2.828(12) 0.858 2.055 149.6 no O20 H24 O22 . . 2_546 2.738(3) 0.811 1.941 167.8 no O20 H25 O27A . . 2_546 2.701(5) 0.754 1.964 165.8 no O20 H25 O27B . . 2_546 2.733(13) 0.754 2.012 160.2 no O21 H26 O12 . . 2_556 2.735(4) 0.725 2.042 160.2 no O21 H27 O5 . . 4_455 2.735(3) 0.885 1.883 160.8 no O22 H28 O6 . . 2_656 2.867(3) 0.800 2.116 156.4 no O22 H29 O24 . . . 2.793(4) 0.786 2.060 155.3 no O23 H30 O25 . . . 2.805(4) 0.887 1.931 168.2 no O23 H31 O4 . . 1_455 2.789(3) 0.863 1.931 172.4 no O24 H32 O25 . . . 2.801(5) 0.904 1.899 175.5 no O24 H33 O9 . . 3_656 2.803(3) 0.792 2.254 127.1 no O25 H34 O7 . . 3_656 2.992(3) 0.799 2.218 163.1 no O25 H35 O11 . . . 2.874(3) 0.831 2.044 178.1 no O26 H36 O24 . . . 2.682(4) 0.765 1.931 166.8 no _database_code_depnum_ccdc_archive 'CCDC 894436' ####################################################################### # # 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_General #TrackingRef 'TC6A-SO3CeCIF.cif' _audit_creation_date 2010-06-17 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'TC6A-SO3LuCIF.cif' #============================================================================== data_TC6A-SO3Lu #TrackingRef 'TC6A-SO3LuCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H18 Lu2 O56 S12' _chemical_formula_moiety 'C36 H18 Lu2 O56 S12' _chemical_formula_weight 2081.16 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 14.9888(7) _cell_length_b 12.4793(6) _cell_length_c 20.4181(10) _cell_angle_alpha 90.0000 _cell_angle_beta 109.1894(15) _cell_angle_gamma 90.0000 _cell_volume 3607.0(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 24748 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 25.32 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032.00 _exptl_absorpt_coefficient_mu 3.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.529 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 27212 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_theta_max 25.32 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Rasidual electron density was located around 1 angstrom from lutetium metal center. ; _reflns_number_total 6549 _reflns_number_gt 6043 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1256 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6549 _refine_ls_number_parameters 478 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0003P)^2^+70.6376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_diff_density_max 4.930 _refine_diff_density_min -2.610 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Lu Lu -0.472 5.858 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Lu1 Lu 0.14822(2) 0.72319(3) 0.646958(16) 0.01428(11) Uani 1.0 4 d . . . S1 S 0.52339(13) 1.16243(15) 0.36633(10) 0.0149(4) Uani 1.0 4 d . . . S2 S 0.21621(13) 0.91771(15) 0.24171(9) 0.0138(4) Uani 1.0 4 d . . . S3 S 0.36850(14) 0.56614(15) 0.40448(9) 0.0151(4) Uani 1.0 4 d . . . S4 S 0.17598(14) 1.26342(16) 0.39476(10) 0.0182(4) Uani 1.0 4 d . . . S5 S -0.00428(14) 0.68197(16) 0.35133(10) 0.0170(4) Uani 1.0 4 d . . . S6 S 0.41105(14) 0.41740(16) 0.66371(10) 0.0161(4) Uani 1.0 4 d . . . O1 O 0.4182(4) 0.9907(5) 0.2878(3) 0.0180(12) Uani 1.0 4 d . . . O2 O 0.3694(4) 0.7673(5) 0.3224(3) 0.0169(12) Uani 1.0 4 d . . . O3 O 0.4370(4) 0.7714(5) 0.4796(3) 0.0192(12) Uani 1.0 4 d . . . O4 O 0.2377(5) 1.3172(6) 0.4566(4) 0.0301(15) Uani 1.0 4 d . . . O5 O 0.1258(5) 1.3379(5) 0.3402(4) 0.0272(14) Uani 1.0 4 d . . . O6 O 0.1126(5) 1.1891(5) 0.4123(4) 0.0254(14) Uani 1.0 4 d . . . O7 O 0.0077(4) 0.6690(5) 0.4244(3) 0.0236(13) Uani 1.0 4 d . . . O8 O -0.0622(4) 0.7740(5) 0.3199(4) 0.0266(14) Uani 1.0 4 d . . . O9 O -0.0386(5) 0.5826(5) 0.3129(3) 0.0238(14) Uani 1.0 4 d . . . O10 O 0.3099(4) 0.4076(5) 0.6561(3) 0.0175(12) Uani 1.0 4 d . . . O11 O 0.4442(4) 0.3198(5) 0.6403(3) 0.0224(13) Uani 1.0 4 d . . . O12 O 0.4684(4) 0.4496(5) 0.7338(3) 0.0231(13) Uani 1.0 4 d . . . O13 O 0.2485(4) 0.7748(5) 0.7552(3) 0.0235(13) Uani 1.0 4 d . . . O14 O 0.2320(5) 0.5778(5) 0.7026(3) 0.0249(14) Uani 1.0 4 d . . . O15 O 0.1950(4) 0.6383(5) 0.5604(3) 0.0233(13) Uani 1.0 4 d . . . O16 O 0.2555(4) 0.8256(5) 0.6218(3) 0.0238(13) Uani 1.0 4 d . . . O17 O 0.0383(4) 0.7850(5) 0.5417(3) 0.0244(14) Uani 1.0 4 d . . . O18 O 0.1021(4) 0.8932(5) 0.6653(3) 0.0198(12) Uani 1.0 4 d . . . O19 O 0.0596(5) 0.6973(5) 0.7209(3) 0.0213(13) Uani 1.0 4 d . . . O20 O 0.0427(4) 0.5846(5) 0.6054(3) 0.0225(13) Uani 1.0 4 d . . . O21 O 0.3823(5) 0.9797(5) 0.4853(4) 0.0326(16) Uani 1.0 4 d . . . O22 O 0.4199(6) 1.1004(6) 0.6048(4) 0.0367(17) Uani 1.0 4 d . . . O23 O 0.3330(5) 0.9994(5) 0.6949(3) 0.0261(14) Uani 1.0 4 d . . . O24 O 0.1167(5) 0.4388(5) 0.5100(3) 0.0258(14) Uani 1.0 4 d . . . O25 O 0.2351(5) 0.8356(6) 0.4886(3) 0.0278(14) Uani 1.0 4 d . . . O26 O 0.0852(5) 0.9701(6) 0.4408(4) 0.0350(16) Uani 1.0 4 d . . . O27 O -0.1057(6) 0.9512(6) 0.4242(4) 0.0391(17) Uani 1.0 4 d . . . O28 O -0.2287(6) 0.7869(7) 0.4196(4) 0.0433(19) Uani 1.0 4 d . . . C1 C 0.2493(6) 1.1825(6) 0.3625(4) 0.0141(16) Uani 1.0 4 d . . . C2 C 0.2089(6) 1.0948(6) 0.3220(4) 0.0148(16) Uani 1.0 4 d . . . C3 C 0.2649(6) 1.0283(6) 0.2973(4) 0.0145(16) Uani 1.0 4 d . . . C4 C 0.3611(6) 1.0519(6) 0.3113(4) 0.0125(15) Uani 1.0 4 d . . . C5 C 0.4004(5) 1.1432(7) 0.3517(4) 0.0136(16) Uani 1.0 4 d . . . C6 C 0.3442(6) 1.2071(7) 0.3773(4) 0.0145(16) Uani 1.0 4 d . . . C7 C 0.1093(6) 0.7053(7) 0.3450(4) 0.0149(16) Uani 1.0 4 d . . . C8 C 0.1838(6) 0.6351(7) 0.3732(4) 0.0162(17) Uani 1.0 4 d . . . C9 C 0.2710(6) 0.6555(7) 0.3680(4) 0.0153(16) Uani 1.0 4 d . . . C10 C 0.2853(6) 0.7456(7) 0.3306(4) 0.0149(16) Uani 1.0 4 d . . . C11 C 0.2100(6) 0.8137(6) 0.3003(4) 0.0153(16) Uani 1.0 4 d . . . C12 C 0.1226(6) 0.7958(6) 0.3086(4) 0.0144(16) Uani 1.0 4 d . . . C13 C 0.4193(6) 0.5231(6) 0.6088(4) 0.0135(16) Uani 1.0 4 d . . . C14 C 0.4463(6) 0.6233(7) 0.6371(4) 0.0160(16) Uani 1.0 4 d . . . C15 C 0.4526(5) 0.7087(6) 0.5953(4) 0.0132(16) Uani 1.0 4 d . . . C16 C 0.4296(5) 0.6940(6) 0.5236(4) 0.0131(16) Uani 1.0 4 d . . . C17 C 0.3990(6) 0.5918(6) 0.4949(4) 0.0128(15) Uani 1.0 4 d . . . C18 C 0.3944(6) 0.5073(6) 0.5376(4) 0.0138(16) Uani 1.0 4 d . . . H1 H 0.1434 1.0802 0.3112 0.0178 Uiso 1.0 4 calc R . . H2 H 0.3705 1.2678 0.4050 0.0174 Uiso 1.0 4 calc R . . H3 H 0.1743 0.5722 0.3964 0.0194 Uiso 1.0 4 calc R . . H4 H 0.0721 0.8447 0.2897 0.0173 Uiso 1.0 4 calc R . . H5 H 0.4607 0.6339 0.6856 0.0191 Uiso 1.0 4 calc R . . H6 H 0.3743 0.4386 0.5183 0.0165 Uiso 1.0 4 calc R . . H7 H 0.3890 0.9354 0.2689 0.0216 Uiso 1.0 4 calc R . . H8 H 0.4058 0.7146 0.3358 0.0203 Uiso 1.0 4 calc R . . H9 H 0.4476 0.8305 0.5005 0.0230 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Lu1 0.01579(18) 0.01515(18) 0.00949(16) 0.00150(14) 0.00089(12) -0.00071(13) S1 0.0130(9) 0.0138(9) 0.0151(9) -0.0015(8) 0.0007(8) -0.0034(8) S2 0.0161(9) 0.0125(9) 0.0090(9) -0.0020(8) -0.0009(7) 0.0008(7) S3 0.0187(10) 0.0148(9) 0.0084(9) 0.0019(8) 0.0001(8) -0.0004(7) S4 0.0169(10) 0.0170(10) 0.0204(10) -0.0014(8) 0.0060(8) -0.0048(8) S5 0.0163(10) 0.0181(10) 0.0148(9) -0.0045(8) 0.0026(8) -0.0003(8) S6 0.0176(10) 0.0152(10) 0.0135(9) 0.0016(8) 0.0023(8) 0.0051(8) O1 0.017(3) 0.015(3) 0.019(3) -0.004(3) 0.002(3) -0.006(3) O2 0.013(3) 0.017(3) 0.017(3) 0.001(3) 0.000(3) 0.005(3) O3 0.028(4) 0.014(3) 0.013(3) -0.005(3) 0.004(3) -0.000(3) O4 0.021(4) 0.034(4) 0.036(4) -0.003(3) 0.010(3) -0.022(3) O5 0.025(4) 0.024(4) 0.035(4) 0.007(3) 0.014(3) 0.008(3) O6 0.025(4) 0.022(3) 0.035(4) 0.003(3) 0.018(3) -0.002(3) O7 0.023(3) 0.030(4) 0.017(3) -0.003(3) 0.006(3) -0.003(3) O8 0.013(3) 0.027(4) 0.036(4) 0.003(3) 0.003(3) 0.004(3) O9 0.025(4) 0.026(4) 0.019(3) -0.010(3) 0.003(3) 0.001(3) O10 0.018(3) 0.015(3) 0.018(3) 0.001(3) 0.004(3) 0.003(3) O11 0.023(3) 0.014(3) 0.029(4) 0.003(3) 0.008(3) 0.004(3) O12 0.023(3) 0.029(4) 0.013(3) -0.003(3) -0.001(3) 0.006(3) O13 0.017(3) 0.032(4) 0.018(3) 0.003(3) 0.001(3) -0.006(3) O14 0.028(4) 0.024(4) 0.019(3) 0.006(3) 0.002(3) 0.002(3) O15 0.023(3) 0.028(4) 0.017(3) 0.003(3) 0.004(3) -0.002(3) O16 0.021(3) 0.032(4) 0.020(3) -0.002(3) 0.009(3) -0.002(3) O17 0.024(3) 0.029(4) 0.010(3) 0.011(3) -0.010(3) 0.000(3) O18 0.025(3) 0.015(3) 0.017(3) 0.004(3) 0.004(3) 0.000(3) O19 0.028(4) 0.019(3) 0.018(3) -0.001(3) 0.008(3) 0.001(3) O20 0.024(3) 0.019(3) 0.023(3) -0.005(3) 0.006(3) -0.004(3) O21 0.047(5) 0.023(4) 0.026(4) -0.001(3) 0.009(3) 0.006(3) O22 0.048(5) 0.023(4) 0.039(4) 0.003(4) 0.015(4) -0.001(3) O23 0.035(4) 0.018(3) 0.023(3) -0.002(3) 0.008(3) -0.005(3) O24 0.028(4) 0.027(4) 0.017(3) 0.005(3) -0.000(3) -0.003(3) O25 0.028(4) 0.036(4) 0.017(3) 0.001(3) 0.004(3) -0.001(3) O26 0.033(4) 0.027(4) 0.042(4) 0.006(3) 0.009(4) 0.007(3) O27 0.044(5) 0.035(4) 0.034(4) -0.003(4) 0.006(4) 0.010(4) O28 0.052(5) 0.044(5) 0.029(4) -0.016(4) 0.006(4) -0.007(4) C1 0.017(4) 0.013(4) 0.010(4) 0.002(4) 0.001(3) 0.002(3) C2 0.016(4) 0.013(4) 0.013(4) -0.003(4) 0.001(3) 0.000(3) C3 0.019(4) 0.012(4) 0.009(4) -0.003(4) 0.000(3) 0.003(3) C4 0.014(4) 0.011(4) 0.013(4) 0.004(3) 0.005(3) 0.001(3) C5 0.010(4) 0.018(4) 0.009(4) -0.001(3) -0.003(3) 0.004(3) C6 0.017(4) 0.014(4) 0.008(4) 0.003(4) -0.001(3) -0.000(3) C7 0.013(4) 0.018(4) 0.011(4) -0.001(4) -0.000(3) -0.002(3) C8 0.023(5) 0.015(4) 0.007(4) -0.006(4) 0.000(3) -0.001(3) C9 0.020(4) 0.016(4) 0.004(4) -0.002(4) -0.003(3) -0.002(3) C10 0.015(4) 0.017(4) 0.010(4) -0.005(4) 0.001(3) -0.004(3) C11 0.023(5) 0.012(4) 0.008(4) -0.005(4) 0.001(3) 0.000(3) C12 0.014(4) 0.013(4) 0.011(4) -0.005(3) -0.003(3) 0.001(3) C13 0.012(4) 0.012(4) 0.012(4) -0.001(3) -0.001(3) 0.005(3) C14 0.016(4) 0.018(4) 0.011(4) 0.002(4) -0.000(3) -0.000(3) C15 0.010(4) 0.012(4) 0.014(4) -0.000(3) -0.001(3) -0.002(3) C16 0.011(4) 0.012(4) 0.014(4) 0.001(3) 0.000(3) 0.001(3) C17 0.015(4) 0.014(4) 0.007(4) -0.002(3) -0.001(3) -0.001(3) C18 0.013(4) 0.011(4) 0.015(4) 0.003(3) 0.001(3) -0.001(3) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Lu1 O13 2.319(6) yes . . Lu1 O14 2.285(6) yes . . Lu1 O15 2.358(7) yes . . Lu1 O16 2.242(7) yes . . Lu1 O17 2.366(5) yes . . Lu1 O18 2.300(6) yes . . Lu1 O19 2.337(7) yes . . Lu1 O20 2.309(6) yes . . S1 C5 1.784(8) yes . . S1 C15 1.773(8) yes . 3_676 S2 C3 1.783(8) yes . . S2 C11 1.788(9) yes . . S3 C9 1.794(8) yes . . S3 C17 1.780(8) yes . . S4 O4 1.460(7) yes . . S4 O5 1.456(7) yes . . S4 O6 1.455(7) yes . . S4 C1 1.771(9) yes . . S5 O7 1.452(7) yes . . S5 O8 1.456(7) yes . . S5 O9 1.467(7) yes . . S5 C7 1.772(9) yes . . S6 O10 1.478(7) yes . . S6 O11 1.454(7) yes . . S6 O12 1.462(6) yes . . S6 C13 1.763(9) yes . . O1 C4 1.349(11) yes . . O2 C10 1.354(11) yes . . O3 C16 1.348(10) yes . . C1 C2 1.386(11) yes . . C1 C6 1.389(12) yes . . C2 C3 1.388(13) yes . . C3 C4 1.406(12) yes . . C4 C5 1.415(11) yes . . C5 C6 1.382(12) yes . . C7 C8 1.387(11) yes . . C7 C12 1.402(12) yes . . C8 C9 1.370(13) yes . . C9 C10 1.414(12) yes . . C10 C11 1.386(11) yes . . C11 C12 1.395(13) yes . . C13 C14 1.382(11) yes . . C13 C18 1.390(11) yes . . C14 C15 1.387(12) yes . . C15 C16 1.402(11) yes . . C16 C17 1.416(11) yes . . C17 C18 1.384(12) yes . . O1 H7 0.840 no . . O2 H8 0.840 no . . O3 H9 0.840 no . . C2 H1 0.950 no . . C6 H2 0.950 no . . C8 H3 0.950 no . . C12 H4 0.950 no . . C14 H5 0.950 no . . C18 H6 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O13 Lu1 O14 70.6(2) yes . . . O13 Lu1 O15 125.5(2) yes . . . O13 Lu1 O16 76.8(3) yes . . . O13 Lu1 O17 144.6(3) yes . . . O13 Lu1 O18 74.0(2) yes . . . O13 Lu1 O19 75.6(3) yes . . . O13 Lu1 O20 135.2(3) yes . . . O14 Lu1 O15 76.5(3) yes . . . O14 Lu1 O16 104.4(3) yes . . . O14 Lu1 O17 144.6(2) yes . . . O14 Lu1 O18 142.8(2) yes . . . O14 Lu1 O19 84.6(3) yes . . . O14 Lu1 O20 77.7(2) yes . . . O15 Lu1 O16 70.8(3) yes . . . O15 Lu1 O17 75.9(2) yes . . . O15 Lu1 O18 135.8(3) yes . . . O15 Lu1 O19 142.6(2) yes . . . O15 Lu1 O20 74.0(3) yes . . . O16 Lu1 O17 86.8(2) yes . . . O16 Lu1 O18 77.8(3) yes . . . O16 Lu1 O19 146.0(2) yes . . . O16 Lu1 O20 143.0(3) yes . . . O17 Lu1 O18 72.0(2) yes . . . O17 Lu1 O19 104.9(2) yes . . . O17 Lu1 O20 73.9(2) yes . . . O18 Lu1 O19 75.9(3) yes . . . O18 Lu1 O20 123.0(2) yes . . . O19 Lu1 O20 70.6(3) yes . . . C5 S1 C15 104.2(4) yes . . 3_676 C3 S2 C11 103.7(4) yes . . . C9 S3 C17 102.4(4) yes . . . O4 S4 O5 112.9(4) yes . . . O4 S4 O6 111.1(4) yes . . . O4 S4 C1 106.8(4) yes . . . O5 S4 O6 112.4(4) yes . . . O5 S4 C1 107.9(4) yes . . . O6 S4 C1 105.3(4) yes . . . O7 S5 O8 113.3(4) yes . . . O7 S5 O9 111.0(4) yes . . . O7 S5 C7 107.2(4) yes . . . O8 S5 O9 112.2(4) yes . . . O8 S5 C7 106.6(4) yes . . . O9 S5 C7 106.0(4) yes . . . O10 S6 O11 110.2(4) yes . . . O10 S6 O12 112.3(4) yes . . . O10 S6 C13 106.2(4) yes . . . O11 S6 O12 113.4(4) yes . . . O11 S6 C13 108.3(4) yes . . . O12 S6 C13 106.0(4) yes . . . S4 C1 C2 118.0(7) yes . . . S4 C1 C6 120.7(6) yes . . . C2 C1 C6 121.3(8) yes . . . C1 C2 C3 119.4(8) yes . . . S2 C3 C2 121.6(6) yes . . . S2 C3 C4 118.1(7) yes . . . C2 C3 C4 120.2(7) yes . . . O1 C4 C3 122.5(7) yes . . . O1 C4 C5 118.1(7) yes . . . C3 C4 C5 119.4(8) yes . . . S1 C5 C4 114.6(7) yes . . . S1 C5 C6 125.7(6) yes . . . C4 C5 C6 119.7(7) yes . . . C1 C6 C5 119.9(7) yes . . . S5 C7 C8 121.9(7) yes . . . S5 C7 C12 118.5(6) yes . . . C8 C7 C12 119.6(8) yes . . . C7 C8 C9 120.6(8) yes . . . S3 C9 C8 121.3(6) yes . . . S3 C9 C10 118.1(7) yes . . . C8 C9 C10 120.5(7) yes . . . O2 C10 C9 122.6(7) yes . . . O2 C10 C11 118.4(8) yes . . . C9 C10 C11 119.0(8) yes . . . S2 C11 C10 122.1(7) yes . . . S2 C11 C12 117.1(6) yes . . . C10 C11 C12 120.4(8) yes . . . C7 C12 C11 119.8(7) yes . . . S6 C13 C14 118.9(6) yes . . . S6 C13 C18 120.5(6) yes . . . C14 C13 C18 120.5(8) yes . . . C13 C14 C15 120.4(8) yes . . . S1 C15 C14 118.0(6) yes 3_676 . . S1 C15 C16 121.6(6) yes 3_676 . . C14 C15 C16 120.0(7) yes . . . O3 C16 C15 123.9(7) yes . . . O3 C16 C17 117.1(7) yes . . . C15 C16 C17 119.0(7) yes . . . S3 C17 C16 122.0(6) yes . . . S3 C17 C18 117.8(6) yes . . . C16 C17 C18 120.2(7) yes . . . C13 C18 C17 119.9(7) yes . . . C4 O1 H7 109.470 no . . . C10 O2 H8 109.472 no . . . C16 O3 H9 109.467 no . . . C1 C2 H1 120.293 no . . . C3 C2 H1 120.275 no . . . C1 C6 H2 120.024 no . . . C5 C6 H2 120.042 no . . . C7 C8 H3 119.703 no . . . C9 C8 H3 119.690 no . . . C7 C12 H4 120.075 no . . . C11 C12 H4 120.080 no . . . C13 C14 H5 119.774 no . . . C15 C14 H5 119.779 no . . . C13 C18 H6 120.069 no . . . C17 C18 H6 120.067 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C5 S1 C15 C14 -100.8(6) no . . 3_676 3_676 C5 S1 C15 C16 86.5(6) no . . 3_676 3_676 C15 S1 C5 C4 170.7(5) no 3_676 . . . C15 S1 C5 C6 -10.9(7) no 3_676 . . . C3 S2 C11 C10 -87.4(6) no . . . . C3 S2 C11 C12 99.5(6) no . . . . C11 S2 C3 C2 -82.8(6) no . . . . C11 S2 C3 C4 102.1(6) no . . . . C9 S3 C17 C16 -61.7(7) no . . . . C9 S3 C17 C18 120.1(6) no . . . . C17 S3 C9 C8 -73.8(6) no . . . . C17 S3 C9 C10 109.2(6) no . . . . O4 S4 C1 C2 155.9(5) no . . . . O4 S4 C1 C6 -24.4(7) no . . . . O5 S4 C1 C2 -82.4(6) no . . . . O5 S4 C1 C6 97.3(6) no . . . . O6 S4 C1 C2 37.8(6) no . . . . O6 S4 C1 C6 -142.5(6) no . . . . O7 S5 C7 C8 55.2(7) no . . . . O7 S5 C7 C12 -126.8(6) no . . . . O8 S5 C7 C8 176.8(6) no . . . . O8 S5 C7 C12 -5.1(7) no . . . . O9 S5 C7 C8 -63.5(6) no . . . . O9 S5 C7 C12 114.6(6) no . . . . O10 S6 C13 C14 99.1(6) no . . . . O10 S6 C13 C18 -77.6(7) no . . . . O11 S6 C13 C14 -142.5(5) no . . . . O11 S6 C13 C18 40.8(7) no . . . . O12 S6 C13 C14 -20.5(7) no . . . . O12 S6 C13 C18 162.8(6) no . . . . S4 C1 C2 C3 -178.5(5) no . . . . S4 C1 C6 C5 -180.0(5) no . . . . C2 C1 C6 C5 -0.3(11) no . . . . C6 C1 C2 C3 1.8(11) no . . . . C1 C2 C3 S2 -177.1(6) no . . . . C1 C2 C3 C4 -2.1(11) no . . . . S2 C3 C4 O1 -4.0(10) no . . . . S2 C3 C4 C5 176.1(5) no . . . . C2 C3 C4 O1 -179.2(7) no . . . . C2 C3 C4 C5 0.9(11) no . . . . O1 C4 C5 S1 -0.7(9) no . . . . O1 C4 C5 C6 -179.3(6) no . . . . C3 C4 C5 S1 179.3(6) no . . . . C3 C4 C5 C6 0.7(11) no . . . . S1 C5 C6 C1 -179.4(5) no . . . . C4 C5 C6 C1 -1.0(11) no . . . . S5 C7 C8 C9 -179.5(5) no . . . . S5 C7 C12 C11 -177.3(5) no . . . . C8 C7 C12 C11 0.8(11) no . . . . C12 C7 C8 C9 2.4(11) no . . . . C7 C8 C9 S3 179.7(6) no . . . . C7 C8 C9 C10 -3.4(11) no . . . . S3 C9 C10 O2 -1.0(10) no . . . . S3 C9 C10 C11 178.1(5) no . . . . C8 C9 C10 O2 -178.1(7) no . . . . C8 C9 C10 C11 1.0(11) no . . . . O2 C10 C11 S2 8.5(10) no . . . . O2 C10 C11 C12 -178.6(6) no . . . . C9 C10 C11 S2 -170.6(6) no . . . . C9 C10 C11 C12 2.2(11) no . . . . S2 C11 C12 C7 170.0(5) no . . . . C10 C11 C12 C7 -3.2(11) no . . . . S6 C13 C14 C15 -179.3(5) no . . . . S6 C13 C18 C17 178.3(5) no . . . . C14 C13 C18 C17 1.7(12) no . . . . C18 C13 C14 C15 -2.6(12) no . . . . C13 C14 C15 S1 174.1(7) no . . . 3_676 C13 C14 C15 C16 1.3(12) no . . . . S1 C15 C16 O3 9.9(11) no 3_676 . . . S1 C15 C16 C17 -171.7(5) no 3_676 . . . C14 C15 C16 O3 -177.5(7) no . . . . C14 C15 C16 C17 0.9(11) no . . . . O3 C16 C17 S3 -1.5(11) no . . . . O3 C16 C17 C18 176.7(6) no . . . . C15 C16 C17 S3 -180.0(6) no . . . . C15 C16 C17 C18 -1.8(11) no . . . . S3 C17 C18 C13 178.8(5) no . . . . C16 C17 C18 C13 0.5(12) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 O1 2.826(6) no . . S1 O3 3.115(6) no . 3_676 S2 O1 3.002(6) no . . S2 O2 3.004(6) no . . S3 O2 3.021(6) no . . S3 O3 2.989(6) no . . O1 O2 3.023(8) no . . O2 O3 3.033(8) no . . O2 C3 3.577(10) no . . O2 C4 3.558(10) no . . O3 C9 3.122(9) no . . O3 C10 3.160(8) no . . O4 C6 2.959(12) no . . O5 C2 3.346(11) no . . O5 C6 3.511(10) no . . O6 C2 2.936(12) no . . O7 C8 3.171(12) no . . O8 C12 2.866(11) no . . O9 C8 3.218(10) no . . O10 C14 3.478(11) no . . O10 C18 3.319(11) no . . O11 C18 3.066(10) no . . O12 C14 2.876(10) no . . C1 C4 2.776(12) no . . C2 C5 2.799(11) no . . C2 C11 3.536(11) no . . C3 C6 2.790(11) no . . C3 C10 3.587(11) no . . C5 C16 3.583(10) no . 3_676 C6 C15 3.094(11) no . 3_676 C6 C16 3.550(10) no . 3_676 C7 C10 2.795(13) no . . C8 C11 2.780(12) no . . C8 C17 3.406(10) no . . C9 C12 2.777(11) no . . C9 C16 3.319(9) no . . C13 C16 2.788(11) no . . C14 C17 2.781(11) no . . C15 C18 2.791(11) no . . S1 O16 3.246(7) no . 3_676 S1 O21 3.392(7) no . 3_676 S1 O22 3.391(7) no . 3_676 S1 O23 3.470(8) no . 3_676 S2 S3 3.385(3) no . 2_555 S2 O5 3.465(8) no . 2_545 S2 C6 3.491(8) no . 2_545 S3 S2 3.385(3) no . 2_545 S3 O11 3.526(7) no . 3_666 S3 C13 3.463(9) no . 3_666 S3 C18 3.479(8) no . 3_666 S4 O19 3.578(6) no . 3_576 S4 O24 3.534(7) no . 1_565 S5 O20 3.538(7) no . 3_566 S6 O18 3.574(7) no . 2_546 S6 O19 3.551(6) no . 2_546 O1 O5 3.126(9) no . 2_545 O1 O9 3.352(10) no . 2_555 O1 O22 2.914(8) no . 3_676 O2 O5 3.458(10) no . 2_545 O2 O11 2.858(8) no . 3_666 O2 O22 3.438(9) no . 3_676 O2 C2 3.525(9) no . 2_545 O3 O21 2.740(9) no . . O3 O22 3.543(11) no . 3_676 O3 O25 3.193(10) no . . O4 O24 2.844(10) no . 1_565 O4 O28 2.885(11) no . 3_576 O4 C18 3.365(10) no . 1_565 O5 S2 3.465(8) no . 2_555 O5 O1 3.126(9) no . 2_555 O5 O2 3.458(10) no . 2_555 O5 O19 2.681(9) no . 3_576 O5 O20 3.223(10) no . 3_576 O6 O17 2.737(10) no . 3_576 O6 O18 3.251(8) no . 3_576 O6 O19 3.384(8) no . 3_576 O6 O26 2.851(10) no . . O6 O28 3.311(9) no . 3_576 O7 O15 3.258(7) no . . O7 O17 2.706(9) no . . O7 O20 3.264(9) no . 3_566 O7 O24 3.478(9) no . . O7 O24 2.953(10) no . 3_566 O8 O13 2.775(8) no . 4_464 O8 O27 3.281(11) no . . O9 O1 3.352(10) no . 2_545 O9 O13 3.502(9) no . 4_464 O9 O14 3.451(9) no . 3_566 O9 O19 3.555(9) no . 3_566 O9 O20 2.686(9) no . 3_566 O9 O23 2.741(8) no . 4_464 O10 O13 2.799(10) no . 2_546 O10 O14 2.739(9) no . . O10 O15 3.585(8) no . . O10 O18 3.451(8) no . 2_546 O10 O24 3.429(7) no . . O10 O28 2.920(9) no . 3_566 O11 S3 3.526(7) no . 3_666 O11 O2 2.858(8) no . 3_666 O11 O19 3.237(9) no . 2_546 O11 O22 2.825(9) no . 1_545 O11 O28 3.333(10) no . 3_566 O12 O18 2.700(10) no . 2_546 O12 O19 3.348(9) no . 2_546 O12 C2 3.503(10) no . 4_565 O13 O8 2.775(8) no . 4_565 O13 O9 3.502(9) no . 4_565 O13 O10 2.799(10) no . 2_556 O13 O23 3.465(10) no . . O13 O28 3.350(10) no . 4_565 O14 O9 3.451(9) no . 3_566 O14 O10 2.739(9) no . . O14 O23 2.762(10) no . 2_546 O15 O7 3.258(7) no . . O15 O10 3.585(8) no . . O15 O24 2.800(9) no . . O15 O25 3.025(10) no . . O15 C13 3.487(10) no . . O15 C14 3.577(10) no . . O15 C18 3.568(11) no . . O16 S1 3.246(7) no . 3_676 O16 O23 2.672(9) no . . O16 O25 2.638(9) no . . O16 O27 3.507(10) no . 3_576 O16 C15 3.492(11) no . . O17 O6 2.737(10) no . 3_576 O17 O7 2.706(9) no . . O17 O24 3.564(9) no . 3_566 O17 O25 3.519(10) no . . O17 O26 3.321(10) no . . O17 O27 3.363(9) no . . O17 O27 3.447(10) no . 3_576 O18 S6 3.574(7) no . 2_556 O18 O6 3.251(8) no . 3_576 O18 O10 3.451(8) no . 2_556 O18 O12 2.700(10) no . 2_556 O18 O23 3.567(9) no . . O18 O26 3.389(8) no . 3_576 O18 O27 2.679(10) no . 3_576 O19 S4 3.578(6) no . 3_576 O19 S6 3.551(6) no . 2_556 O19 O5 2.681(9) no . 3_576 O19 O6 3.384(8) no . 3_576 O19 O9 3.555(9) no . 3_566 O19 O11 3.237(9) no . 2_556 O19 O12 3.348(9) no . 2_556 O19 O23 3.136(8) no . 2_546 O20 S5 3.538(7) no . 3_566 O20 O5 3.223(10) no . 3_576 O20 O7 3.264(9) no . 3_566 O20 O9 2.686(9) no . 3_566 O20 O24 3.123(10) no . . O20 O24 2.764(8) no . 3_566 O21 S1 3.392(7) no . 3_676 O21 O3 2.740(9) no . . O21 O21 3.417(11) no . 3_676 O21 O22 2.762(10) no . . O21 O25 2.865(10) no . . O21 C4 3.576(11) no . . O21 C5 3.488(11) no . . O21 C6 3.523(10) no . . O22 S1 3.391(7) no . 3_676 O22 O1 2.914(8) no . 3_676 O22 O2 3.438(9) no . 3_676 O22 O3 3.543(11) no . 3_676 O22 O11 2.825(9) no . 1_565 O22 O21 2.762(10) no . . O22 O23 2.872(11) no . . O22 O28 3.083(11) no . 3_576 O23 S1 3.470(8) no . 3_676 O23 O9 2.741(8) no . 4_565 O23 O13 3.465(10) no . . O23 O14 2.762(10) no . 2_556 O23 O16 2.672(9) no . . O23 O18 3.567(9) no . . O23 O19 3.136(8) no . 2_556 O23 O22 2.872(11) no . . O23 O27 3.529(9) no . 3_576 O23 O28 3.552(10) no . 3_576 O24 S4 3.534(7) no . 1_545 O24 O4 2.844(10) no . 1_545 O24 O7 3.478(9) no . . O24 O7 2.953(10) no . 3_566 O24 O10 3.429(7) no . . O24 O15 2.800(9) no . . O24 O17 3.564(9) no . 3_566 O24 O20 3.123(10) no . . O24 O20 2.764(8) no . 3_566 O24 O28 3.352(10) no . 3_566 O25 O3 3.193(10) no . . O25 O15 3.025(10) no . . O25 O16 2.638(9) no . . O25 O17 3.519(10) no . . O25 O21 2.865(10) no . . O25 O26 2.716(9) no . . O25 C7 3.340(9) no . . O25 C8 3.348(10) no . . O25 C9 3.503(11) no . . O25 C12 3.537(9) no . . O25 C16 3.281(10) no . . O26 O6 2.851(10) no . . O26 O17 3.321(10) no . . O26 O18 3.389(8) no . 3_576 O26 O25 2.716(9) no . . O26 O27 2.779(11) no . . O26 O27 2.846(11) no . 3_576 O27 O8 3.281(11) no . . O27 O16 3.507(10) no . 3_576 O27 O17 3.363(9) no . . O27 O17 3.447(10) no . 3_576 O27 O18 2.679(10) no . 3_576 O27 O23 3.529(9) no . 3_576 O27 O26 2.779(11) no . . O27 O26 2.846(11) no . 3_576 O27 O28 2.738(11) no . . O28 O4 2.885(11) no . 3_576 O28 O6 3.311(9) no . 3_576 O28 O10 2.920(9) no . 3_566 O28 O11 3.333(10) no . 3_566 O28 O13 3.350(10) no . 4_464 O28 O22 3.083(11) no . 3_576 O28 O23 3.552(10) no . 3_576 O28 O24 3.352(10) no . 3_566 O28 O27 2.738(11) no . . C2 O2 3.525(9) no . 2_555 C2 O12 3.503(10) no . 4_464 C4 O21 3.576(11) no . . C5 O21 3.488(11) no . . C6 S2 3.491(8) no . 2_555 C6 O21 3.523(10) no . . C7 O25 3.340(9) no . . C8 O25 3.348(10) no . . C9 O25 3.503(11) no . . C12 O25 3.537(9) no . . C13 S3 3.463(9) no . 3_666 C13 O15 3.487(10) no . . C14 O15 3.577(10) no . . C15 O16 3.492(11) no . . C16 O25 3.281(10) no . . C17 C18 3.594(12) no . 3_666 C18 S3 3.479(8) no . 3_666 C18 O4 3.365(10) no . 1_545 C18 O15 3.568(11) no . . C18 C17 3.594(12) no . 3_666 S1 H2 2.9653 no . . S1 H5 2.7946 no . 3_676 S1 H9 2.6102 no . 3_676 S2 H1 2.8876 no . . S2 H4 2.8011 no . . S2 H7 2.4739 no . . S3 H3 2.8618 no . . S3 H6 2.7947 no . . S3 H8 2.4956 no . . S4 H1 2.7975 no . . S4 H2 2.8542 no . . S5 H3 2.8752 no . . S5 H4 2.8226 no . . S6 H5 2.7985 no . . S6 H6 2.8479 no . . O2 H7 2.4269 no . . O2 H9 3.5241 no . . O3 H2 3.1063 no . 3_676 O3 H8 2.9053 no . . O4 H2 2.6132 no . . O5 H1 3.2952 no . . O5 H2 3.5748 no . . O6 H1 2.6358 no . . O7 H3 2.9940 no . . O8 H4 2.4548 no . . O9 H3 3.0867 no . . O10 H5 3.5422 no . . O10 H6 3.2833 no . . O11 H6 2.7899 no . . O12 H5 2.4883 no . . C2 H2 3.2718 no . . C3 H7 2.4183 no . . C4 H1 3.2812 no . . C4 H2 3.2795 no . . C5 H7 3.0690 no . . C5 H9 3.1445 no . 3_676 C6 H1 3.2737 no . . C6 H9 3.3265 no . 3_676 C8 H4 3.2682 no . . C9 H8 2.4355 no . . C10 H3 3.2735 no . . C10 H4 3.2684 no . . C10 H7 3.3027 no . . C11 H1 3.5006 no . . C11 H7 3.3233 no . . C11 H8 3.0438 no . . C12 H1 3.5627 no . . C12 H3 3.2677 no . . C14 H2 3.4172 no . 3_676 C14 H6 3.2622 no . . C15 H2 2.6703 no . 3_676 C15 H9 2.4432 no . . C16 H2 2.9081 no . 3_676 C16 H5 3.2722 no . . C16 H6 3.2863 no . . C17 H3 3.3160 no . . C17 H9 3.0589 no . . C18 H5 3.2614 no . . H1 H4 3.1085 no . . H2 H9 3.0337 no . 3_676 H7 H8 3.0485 no . . H8 H9 3.5222 no . . S2 H2 3.4060 no . 2_545 S6 H8 3.1994 no . 3_666 O2 H1 3.5473 no . 2_545 O4 H3 3.4315 no . 1_565 O4 H6 2.5260 no . 1_565 O5 H3 3.1385 no . 1_565 O5 H7 2.4835 no . 2_555 O8 H5 3.0940 no . 4_464 O11 H8 2.1818 no . 3_666 O12 H1 2.6057 no . 4_565 O12 H4 3.0228 no . 4_565 O12 H8 3.3963 no . 3_666 O15 H3 3.3617 no . . O19 H7 3.4484 no . 4_465 O21 H9 2.0796 no . . O21 H9 3.4219 no . 3_676 O22 H7 3.1940 no . 3_676 O22 H8 3.3977 no . 3_676 O22 H9 3.4803 no . 3_676 O24 H3 3.1961 no . . O25 H9 3.1146 no . . O26 H1 3.3413 no . . O26 H4 3.4065 no . . C2 H8 3.4537 no . 2_555 C12 H5 2.9941 no . 4_464 C14 H4 3.0916 no . 4_565 C17 H6 3.5168 no . 3_666 H1 O2 3.5473 no . 2_555 H1 O12 2.6057 no . 4_464 H1 O26 3.3413 no . . H1 H8 3.3034 no . 2_555 H2 S2 3.4060 no . 2_555 H2 H6 3.1332 no . 1_565 H3 O4 3.4315 no . 1_545 H3 O5 3.1385 no . 1_545 H3 O15 3.3617 no . . H3 O24 3.1961 no . . H4 O12 3.0228 no . 4_464 H4 O26 3.4065 no . . H4 C14 3.0916 no . 4_464 H4 H5 2.2466 no . 4_464 H5 O8 3.0940 no . 4_565 H5 C12 2.9941 no . 4_565 H5 H4 2.2466 no . 4_565 H6 O4 2.5260 no . 1_545 H6 C17 3.5168 no . 3_666 H6 H2 3.1332 no . 1_545 H7 O5 2.4835 no . 2_545 H7 O19 3.4484 no . 4_564 H7 O22 3.1940 no . 3_676 H8 S6 3.1994 no . 3_666 H8 O11 2.1818 no . 3_666 H8 O12 3.3963 no . 3_666 H8 O22 3.3977 no . 3_676 H8 C2 3.4537 no . 2_545 H8 H1 3.3034 no . 2_545 H9 O21 2.0796 no . . H9 O21 3.4219 no . 3_676 H9 O22 3.4803 no . 3_676 H9 O25 3.1146 no . . #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H7 S2 . . . 3.002(6) 0.840 2.474 121.7 no O1 H7 O2 . . . 3.023(8) 0.840 2.427 128.6 no O2 H8 S3 . . . 3.021(6) 0.840 2.496 121.6 no O2 H8 O11 . . 3_666 2.858(8) 0.840 2.182 137.5 no O3 H9 S1 . . 3_676 3.115(6) 0.840 2.610 119.8 no O3 H9 O21 . . . 2.740(9) 0.840 2.080 135.1 no _database_code_depnum_ccdc_archive 'CCDC 894437' ####################################################################### # # 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_General #TrackingRef 'TC6A-SO3CeCIF.cif' _audit_creation_date 2010-06-17 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'TC6A-SO3TbCIF.cif' #============================================================================== data_TC6A-SO3Tb #TrackingRef 'TC6A-SO3TbCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H78 O56 S12 Tb2' _chemical_formula_moiety 'C36 H78 O56 S12 Tb2' _chemical_formula_weight 2109.55 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.5538(4) _cell_length_b 12.2885(4) _cell_length_c 20.6249(6) _cell_angle_alpha 90.0000 _cell_angle_beta 110.5668(9) _cell_angle_gamma 90.0000 _cell_volume 3690.82(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 30612 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.45 _cell_measurement_temperature 100.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128.00 _exptl_absorpt_coefficient_mu 2.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.490 _exptl_absorpt_correction_T_max 0.556 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 35225 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). The water molecule (O28) indicated disordering at two positions (A and B sites) and was isotropically refined. The parts containing (O28A and O28B) were refined as the disordered water molecules, occupancy of which was fixed at 0.80 and 0.20. ; _reflns_number_total 8400 _reflns_number_gt 7817 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0543 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8400 _refine_ls_number_parameters 570 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0179P)^2^+7.0514P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.620 _refine_diff_density_min -1.010 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Tb Tb -0.172 4.154 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.167734(7) 0.736330(8) 0.647958(5) 0.00955(4) Uani 1.0 4 d . . . S1 S 0.48543(4) 0.83953(4) 0.62945(3) 0.00991(11) Uani 1.0 4 d . . . S2 S 0.38040(4) 0.56032(4) 0.40370(3) 0.00880(10) Uani 1.0 4 d . . . S3 S 0.21540(4) 0.91362(4) 0.24068(3) 0.00927(10) Uani 1.0 4 d . . . S4 S 0.41625(4) 0.41326(4) 0.66176(3) 0.01005(11) Uani 1.0 4 d . . . S5 S 0.02151(4) 0.66398(5) 0.35896(3) 0.01196(11) Uani 1.0 4 d . . . S6 S 0.17735(4) 1.26540(5) 0.39286(3) 0.01260(11) Uani 1.0 4 d . . . O1 O 0.44699(12) 0.76842(13) 0.47736(9) 0.0134(4) Uani 1.0 4 d . . . O2 O 0.37046(11) 0.76761(13) 0.31914(9) 0.0125(4) Uani 1.0 4 d . . . O3 O 0.41313(11) 0.99080(13) 0.28849(9) 0.0127(4) Uani 1.0 4 d . . . O4 O 0.31786(11) 0.40602(14) 0.65268(9) 0.0151(4) Uani 1.0 4 d . . . O5 O 0.47174(12) 0.44571(14) 0.73192(9) 0.0169(4) Uani 1.0 4 d . . . O6 O 0.44886(12) 0.31608(13) 0.63765(9) 0.0167(4) Uani 1.0 4 d . . . O7 O 0.01360(13) 0.74537(15) 0.40857(9) 0.0200(4) Uani 1.0 4 d . . . O8 O 0.02964(12) 0.55325(15) 0.38659(10) 0.0216(4) Uani 1.0 4 d . . . O9 O -0.05244(11) 0.67483(15) 0.29215(9) 0.0163(4) Uani 1.0 4 d . . . O10 O 0.13496(12) 1.19372(15) 0.43051(9) 0.0179(4) Uani 1.0 4 d . . . O11 O 0.10931(12) 1.31402(15) 0.33241(10) 0.0197(4) Uani 1.0 4 d . . . O12 O 0.23896(12) 1.34380(15) 0.43943(10) 0.0208(4) Uani 1.0 4 d . . . O13 O 0.24066(14) 0.88667(16) 0.61870(10) 0.0201(4) Uani 1.0 4 d . . . O14 O 0.08390(13) 0.89295(15) 0.66093(10) 0.0153(4) Uani 1.0 4 d . . . O15 O 0.25767(13) 0.81585(16) 0.75652(9) 0.0162(4) Uani 1.0 4 d . . . O16 O 0.07706(13) 0.68525(15) 0.71235(10) 0.0148(4) Uani 1.0 4 d . . . O17 O 0.29179(13) 0.62113(15) 0.71046(10) 0.0191(4) Uani 1.0 4 d . . . O18 O 0.12679(14) 0.54891(16) 0.61969(11) 0.0216(4) Uani 1.0 4 d . . . O19 O 0.21889(13) 0.68409(16) 0.55597(10) 0.0164(4) Uani 1.0 4 d . . . O20 O 0.03236(14) 0.75406(19) 0.54815(11) 0.0256(5) Uani 1.0 4 d . . . O21 O 0.2428(2) 0.86497(19) 0.48965(12) 0.0339(5) Uani 1.0 4 d . . . O22 O 0.15961(14) 0.48081(16) 0.50691(10) 0.0196(4) Uani 1.0 4 d . . . O23 O 0.11751(13) 0.50960(16) 0.79696(10) 0.0173(4) Uani 1.0 4 d . . . O24 O 0.36939(14) 0.60756(15) 0.85294(10) 0.0192(4) Uani 1.0 4 d . . . O25 O 0.26323(15) 0.70196(18) 0.92327(11) 0.0256(5) Uani 1.0 4 d . . . O26 O 0.09688(17) 0.60459(16) 0.91352(12) 0.0287(5) Uani 1.0 4 d . . . O27 O 0.10918(18) 0.47426(17) 1.02051(11) 0.0307(5) Uani 1.0 4 d . . . O28A O 0.0956(3) 0.9698(3) 0.4165(2) 0.0568(10) Uiso 0.8000 4 d . . . O28B O 0.0813(9) 0.9838(11) 0.4526(7) 0.042(3) Uiso 0.2000 4 d . . . C1 C 0.42418(15) 0.52125(18) 0.60744(11) 0.0095(4) Uani 1.0 4 d . . . C2 C 0.40040(15) 0.50305(17) 0.53621(11) 0.0088(4) Uani 1.0 4 d . . . C3 C 0.40745(15) 0.58743(18) 0.49326(11) 0.0088(4) Uani 1.0 4 d . . . C4 C 0.43908(15) 0.69092(17) 0.52155(11) 0.0085(4) Uani 1.0 4 d . . . C5 C 0.46052(15) 0.70763(18) 0.59280(12) 0.0090(4) Uani 1.0 4 d . . . C6 C 0.45243(14) 0.62282(18) 0.63501(11) 0.0097(5) Uani 1.0 4 d . . . C7 C 0.12547(15) 0.69107(19) 0.34596(12) 0.0107(5) Uani 1.0 4 d . . . C8 C 0.13237(15) 0.78281(18) 0.30852(11) 0.0100(5) Uani 1.0 4 d . . . C9 C 0.21432(15) 0.80661(18) 0.29881(11) 0.0097(5) Uani 1.0 4 d . . . C10 C 0.29219(15) 0.74007(18) 0.32906(12) 0.0101(5) Uani 1.0 4 d . . . C11 C 0.28407(15) 0.64771(18) 0.36671(11) 0.0091(4) Uani 1.0 4 d . . . C12 C 0.20076(15) 0.62214(18) 0.37397(11) 0.0103(5) Uani 1.0 4 d . . . C13 C 0.24793(15) 1.18142(18) 0.36235(12) 0.0104(5) Uani 1.0 4 d . . . C14 C 0.34090(15) 1.20640(18) 0.37863(11) 0.0089(4) Uani 1.0 4 d . . . C15 C 0.39532(15) 1.14157(17) 0.35338(11) 0.0083(4) Uani 1.0 4 d . . . C16 C 0.35665(15) 1.05001(17) 0.31180(11) 0.0087(4) Uani 1.0 4 d . . . C17 C 0.26382(15) 1.02529(17) 0.29717(11) 0.0085(4) Uani 1.0 4 d . . . C18 C 0.20905(15) 1.09165(18) 0.32175(11) 0.0103(5) Uani 1.0 4 d . . . H1 H 0.3795 0.4334 0.5173 0.0106 Uiso 1.0 4 calc R . . H2 H 0.4665 0.6350 0.6831 0.0116 Uiso 1.0 4 calc R . . H3 H 0.0808 0.8294 0.2895 0.0120 Uiso 1.0 4 calc R . . H4 H 0.1952 0.5580 0.3979 0.0124 Uiso 1.0 4 calc R . . H5 H 0.3668 1.2676 0.4069 0.0107 Uiso 1.0 4 calc R . . H6 H 0.1458 1.0755 0.3108 0.0123 Uiso 1.0 4 calc R . . H7 H 0.4488 0.8301 0.4954 0.0160 Uiso 1.0 4 calc R . . H8 H 0.4131 0.7265 0.3427 0.0150 Uiso 1.0 4 calc R . . H9 H 0.3848 0.9362 0.2669 0.0152 Uiso 1.0 4 calc R . . H10 H 0.2770 0.9262 0.6455 0.0241 Uiso 1.0 4 calc R . . H11 H 0.2435 0.8890 0.5843 0.0241 Uiso 1.0 4 calc R . . H12 H 0.0684 0.8999 0.6908 0.0183 Uiso 1.0 4 calc R . . H13 H 0.1001 0.9515 0.6543 0.0183 Uiso 1.0 4 calc R . . H14 H 0.2375 0.8410 0.7817 0.0194 Uiso 1.0 4 calc R . . H15 H 0.3066 0.8210 0.7684 0.0194 Uiso 1.0 4 calc R . . H16 H 0.0231 0.6892 0.6990 0.0178 Uiso 1.0 4 calc R . . H17 H 0.0896 0.6377 0.7341 0.0178 Uiso 1.0 4 calc R . . H18 H 0.3156 0.6175 0.7519 0.0230 Uiso 1.0 4 calc R . . H19 H 0.2900 0.5623 0.6942 0.0230 Uiso 1.0 4 calc R . . H20 H 0.1335 0.5190 0.5871 0.0259 Uiso 1.0 4 calc R . . H21 H 0.0747 0.5302 0.6221 0.0259 Uiso 1.0 4 calc R . . H22 H 0.2117 0.6318 0.5393 0.0197 Uiso 1.0 4 calc R . . H23 H 0.2323 0.7271 0.5320 0.0197 Uiso 1.0 4 calc R . . H24 H 0.0281 0.7459 0.5127 0.0307 Uiso 1.0 4 calc R . . H25 H -0.0183 0.7760 0.5489 0.0307 Uiso 1.0 4 calc R . . H26 H 0.1946 0.8955 0.4722 0.0407 Uiso 1.0 4 calc R . . H27 H 0.2840 0.8981 0.4784 0.0407 Uiso 1.0 4 calc R . . H28 H 0.1870 0.4378 0.4961 0.0235 Uiso 1.0 4 calc R . . H29 H 0.1165 0.4954 0.4751 0.0235 Uiso 1.0 4 calc R . . H30 H 0.0876 0.4661 0.7750 0.0208 Uiso 1.0 4 calc R . . H31 H 0.0977 0.5323 0.8225 0.0208 Uiso 1.0 4 calc R . . H32 H 0.3345 0.6248 0.8744 0.0230 Uiso 1.0 4 calc R . . H33 H 0.4172 0.6545 0.8669 0.0230 Uiso 1.0 4 calc R . . H34 H 0.2418 0.7597 0.9068 0.0307 Uiso 1.0 4 calc R . . H35 H 0.2914 0.7047 0.9636 0.0307 Uiso 1.0 4 calc R . . H36 H 0.0548 0.6353 0.8952 0.0344 Uiso 1.0 4 calc R . . H37 H 0.1522 0.6355 0.9188 0.0344 Uiso 1.0 4 calc R . . H38 H 0.0997 0.5182 0.9896 0.0368 Uiso 1.0 4 calc R . . H39 H 0.1145 0.5076 1.0523 0.0368 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tb1 0.00949(6) 0.01012(6) 0.00945(6) -0.00145(4) 0.00382(4) -0.00189(4) S1 0.0081(3) 0.0085(3) 0.0133(3) -0.00137(19) 0.0040(2) -0.0030(2) S2 0.0102(3) 0.0086(3) 0.0070(3) 0.00156(19) 0.0022(2) 0.00014(19) S3 0.0114(3) 0.0074(3) 0.0073(3) -0.00084(19) 0.0011(2) 0.00072(19) S4 0.0107(3) 0.0095(3) 0.0106(3) 0.0004(2) 0.0046(2) 0.0030(2) S5 0.0086(3) 0.0149(3) 0.0124(3) -0.0007(2) 0.0037(2) 0.0011(2) S6 0.0097(3) 0.0122(3) 0.0168(3) -0.0001(2) 0.0057(3) -0.0050(2) O1 0.0213(9) 0.0077(8) 0.0118(8) -0.0025(7) 0.0066(7) 0.0003(6) O2 0.0092(8) 0.0124(8) 0.0154(9) 0.0008(6) 0.0037(7) 0.0040(7) O3 0.0104(8) 0.0100(8) 0.0178(9) -0.0022(6) 0.0052(7) -0.0076(7) O4 0.0102(8) 0.0189(9) 0.0167(9) -0.0004(7) 0.0052(7) 0.0056(7) O5 0.0169(9) 0.0199(9) 0.0117(8) -0.0020(7) 0.0021(7) 0.0046(7) O6 0.0207(9) 0.0103(8) 0.0217(9) 0.0013(7) 0.0105(8) 0.0015(7) O7 0.0182(9) 0.0277(10) 0.0150(9) 0.0027(8) 0.0067(8) -0.0031(8) O8 0.0131(9) 0.0197(9) 0.0320(11) 0.0002(7) 0.0081(8) 0.0110(8) O9 0.0088(8) 0.0231(9) 0.0145(9) -0.0001(7) 0.0009(7) -0.0000(7) O10 0.0164(9) 0.0200(9) 0.0208(9) -0.0007(7) 0.0110(8) -0.0018(8) O11 0.0154(9) 0.0197(9) 0.0235(10) 0.0063(7) 0.0061(8) 0.0017(8) O12 0.0151(9) 0.0203(9) 0.0290(10) -0.0033(7) 0.0103(8) -0.0133(8) O13 0.0257(10) 0.0219(10) 0.0148(9) -0.0121(8) 0.0098(9) -0.0056(8) O14 0.0203(9) 0.0121(9) 0.0157(9) 0.0003(7) 0.0092(8) -0.0028(7) O15 0.0093(8) 0.0247(10) 0.0145(9) 0.0006(8) 0.0039(7) -0.0064(8) O16 0.0134(9) 0.0160(9) 0.0170(9) 0.0022(7) 0.0078(8) 0.0042(7) O17 0.0246(10) 0.0156(9) 0.0136(9) 0.0049(8) 0.0022(8) -0.0020(8) O18 0.0249(10) 0.0205(10) 0.0262(11) -0.0116(8) 0.0175(9) -0.0126(8) O19 0.0216(10) 0.0142(9) 0.0174(9) -0.0022(8) 0.0118(8) -0.0039(8) O20 0.0132(9) 0.0485(13) 0.0130(9) 0.0073(9) 0.0021(8) -0.0088(9) O21 0.0532(15) 0.0278(12) 0.0268(12) -0.0050(11) 0.0218(12) 0.0017(9) O22 0.0210(10) 0.0199(10) 0.0190(10) 0.0044(8) 0.0083(8) -0.0047(8) O23 0.0171(9) 0.0162(9) 0.0186(10) -0.0003(7) 0.0063(8) 0.0023(8) O24 0.0237(10) 0.0149(9) 0.0204(10) -0.0006(8) 0.0096(8) 0.0004(7) O25 0.0289(11) 0.0270(11) 0.0201(10) 0.0043(9) 0.0077(9) 0.0012(9) O26 0.0361(13) 0.0167(10) 0.0328(12) 0.0037(9) 0.0115(11) 0.0069(9) O27 0.0616(16) 0.0160(10) 0.0180(10) -0.0088(10) 0.0183(11) -0.0071(8) C1 0.0084(10) 0.0100(10) 0.0103(11) 0.0018(8) 0.0036(9) 0.0044(8) C2 0.0081(10) 0.0081(10) 0.0095(10) -0.0002(8) 0.0022(9) -0.0012(8) C3 0.0073(10) 0.0107(10) 0.0074(10) 0.0014(8) 0.0013(8) 0.0001(8) C4 0.0083(10) 0.0080(10) 0.0084(10) 0.0007(8) 0.0021(9) 0.0010(8) C5 0.0071(10) 0.0083(10) 0.0112(11) 0.0006(8) 0.0026(9) 0.0004(8) C6 0.0067(10) 0.0131(11) 0.0088(10) -0.0004(8) 0.0022(9) 0.0002(9) C7 0.0086(10) 0.0127(11) 0.0101(10) -0.0038(9) 0.0024(9) -0.0041(9) C8 0.0098(10) 0.0103(10) 0.0071(10) 0.0001(8) -0.0005(9) -0.0016(8) C9 0.0121(11) 0.0074(10) 0.0076(10) -0.0006(8) 0.0012(9) 0.0015(8) C10 0.0102(11) 0.0104(10) 0.0090(10) -0.0021(8) 0.0026(9) -0.0026(8) C11 0.0104(10) 0.0090(10) 0.0060(10) 0.0009(8) 0.0006(8) -0.0005(8) C12 0.0131(11) 0.0099(10) 0.0069(10) -0.0019(9) 0.0022(9) -0.0018(8) C13 0.0114(11) 0.0102(10) 0.0109(11) 0.0022(9) 0.0055(9) 0.0013(9) C14 0.0107(11) 0.0075(10) 0.0077(10) -0.0008(8) 0.0021(9) 0.0012(8) C15 0.0095(10) 0.0074(10) 0.0077(10) -0.0000(8) 0.0025(8) 0.0030(8) C16 0.0104(10) 0.0083(10) 0.0079(10) 0.0017(8) 0.0040(9) 0.0026(8) C17 0.0110(10) 0.0061(10) 0.0062(10) -0.0005(8) 0.0004(8) 0.0015(8) C18 0.0092(10) 0.0109(10) 0.0105(11) -0.0004(8) 0.0032(9) 0.0017(9) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tb1 O13 2.355(3) yes . . Tb1 O14 2.392(2) yes . . Tb1 O15 2.3926(17) yes . . Tb1 O16 2.337(3) yes . . Tb1 O17 2.3751(18) yes . . Tb1 O18 2.406(2) yes . . Tb1 O19 2.389(3) yes . . Tb1 O20 2.3818(18) yes . . S1 C5 1.773(3) yes . . S1 C15 1.777(3) yes . 3_676 S2 C3 1.776(3) yes . . S2 C11 1.782(3) yes . . S3 C9 1.784(3) yes . . S3 C17 1.786(2) yes . . S4 O4 1.4777(19) yes . . S4 O5 1.4561(17) yes . . S4 O6 1.4518(19) yes . . S4 C1 1.769(3) yes . . S5 O7 1.467(2) yes . . S5 O8 1.463(2) yes . . S5 O9 1.4581(16) yes . . S5 C7 1.761(3) yes . . S6 O10 1.474(3) yes . . S6 O11 1.4506(18) yes . . S6 O12 1.4568(18) yes . . S6 C13 1.775(3) yes . . O1 C4 1.353(3) yes . . O2 C10 1.347(4) yes . . O3 C16 1.352(4) yes . . C1 C2 1.401(4) yes . . C1 C6 1.378(3) yes . . C2 C3 1.393(4) yes . . C3 C4 1.414(3) yes . . C4 C5 1.403(4) yes . . C5 C6 1.392(4) yes . . C7 C8 1.392(4) yes . . C7 C12 1.395(3) yes . . C8 C9 1.389(4) yes . . C9 C10 1.412(3) yes . . C10 C11 1.406(4) yes . . C11 C12 1.392(4) yes . . C13 C14 1.399(4) yes . . C13 C18 1.389(3) yes . . C14 C15 1.390(4) yes . . C15 C16 1.414(3) yes . . C16 C17 1.401(4) yes . . C17 C18 1.397(4) yes . . O1 H7 0.840 no . . O2 H8 0.840 no . . O3 H9 0.840 no . . O13 H10 0.801 no . . O13 H11 0.727 no . . O14 H12 0.741 no . . O14 H13 0.790 no . . O15 H14 0.761 no . . O15 H15 0.715 no . . O16 H16 0.788 no . . O16 H17 0.721 no . . O17 H18 0.804 no . . O17 H19 0.793 no . . O18 H20 0.805 no . . O18 H21 0.860 no . . O19 H22 0.719 no . . O19 H23 0.800 no . . O20 H24 0.718 no . . O20 H25 0.838 no . . O21 H26 0.802 no . . O21 H27 0.857 no . . O22 H28 0.760 no . . O22 H29 0.776 no . . O23 H30 0.748 no . . O23 H31 0.751 no . . O24 H32 0.839 no . . O24 H33 0.905 no . . O25 H34 0.807 no . . O25 H35 0.793 no . . O26 H36 0.735 no . . O26 H37 0.912 no . . O27 H38 0.809 no . . O27 H39 0.753 no . . C2 H1 0.950 no . . C6 H2 0.950 no . . C8 H3 0.950 no . . C12 H4 0.950 no . . C14 H5 0.950 no . . C18 H6 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O13 Tb1 O14 74.21(8) yes . . . O13 Tb1 O15 75.14(7) yes . . . O13 Tb1 O16 142.89(8) yes . . . O13 Tb1 O17 103.54(7) yes . . . O13 Tb1 O18 143.06(9) yes . . . O13 Tb1 O19 71.48(8) yes . . . O13 Tb1 O20 93.78(8) yes . . . O14 Tb1 O15 74.29(7) yes . . . O14 Tb1 O16 72.00(7) yes . . . O14 Tb1 O17 142.16(7) yes . . . O14 Tb1 O18 133.56(7) yes . . . O14 Tb1 O19 130.69(7) yes . . . O14 Tb1 O20 70.85(7) yes . . . O15 Tb1 O16 81.32(7) yes . . . O15 Tb1 O17 68.84(7) yes . . . O15 Tb1 O18 129.47(7) yes . . . O15 Tb1 O19 127.21(7) yes . . . O15 Tb1 O20 145.10(8) yes . . . O16 Tb1 O17 93.95(7) yes . . . O16 Tb1 O18 73.71(8) yes . . . O16 Tb1 O19 144.59(7) yes . . . O16 Tb1 O20 89.37(8) yes . . . O17 Tb1 O18 69.90(7) yes . . . O17 Tb1 O19 80.63(7) yes . . . O17 Tb1 O20 145.75(8) yes . . . O18 Tb1 O19 71.57(8) yes . . . O18 Tb1 O20 78.45(7) yes . . . O19 Tb1 O20 77.18(8) yes . . . C5 S1 C15 105.12(11) yes . . 3_676 C3 S2 C11 100.87(11) yes . . . C9 S3 C17 103.26(11) yes . . . O4 S4 O5 111.61(12) yes . . . O4 S4 O6 112.21(11) yes . . . O4 S4 C1 105.33(11) yes . . . O5 S4 O6 114.15(10) yes . . . O5 S4 C1 105.97(10) yes . . . O6 S4 C1 106.84(12) yes . . . O7 S5 O8 112.29(12) yes . . . O7 S5 O9 111.43(11) yes . . . O7 S5 C7 106.49(12) yes . . . O8 S5 O9 112.62(11) yes . . . O8 S5 C7 106.06(12) yes . . . O9 S5 C7 107.49(12) yes . . . O10 S6 O11 111.87(11) yes . . . O10 S6 O12 111.11(12) yes . . . O10 S6 C13 106.62(12) yes . . . O11 S6 O12 113.99(11) yes . . . O11 S6 C13 106.86(12) yes . . . O12 S6 C13 105.83(11) yes . . . S4 C1 C2 119.53(17) yes . . . S4 C1 C6 120.09(18) yes . . . C2 C1 C6 120.4(3) yes . . . C1 C2 C3 119.8(2) yes . . . S2 C3 C2 118.62(17) yes . . . S2 C3 C4 121.27(18) yes . . . C2 C3 C4 120.1(2) yes . . . O1 C4 C3 117.1(2) yes . . . O1 C4 C5 123.92(19) yes . . . C3 C4 C5 119.0(2) yes . . . S1 C5 C4 121.09(18) yes . . . S1 C5 C6 118.18(19) yes . . . C4 C5 C6 120.3(2) yes . . . C1 C6 C5 120.4(2) yes . . . S5 C7 C8 119.44(18) yes . . . S5 C7 C12 120.3(2) yes . . . C8 C7 C12 120.3(3) yes . . . C7 C8 C9 120.3(2) yes . . . S3 C9 C8 118.55(16) yes . . . S3 C9 C10 121.0(2) yes . . . C8 C9 C10 120.2(3) yes . . . O2 C10 C9 117.9(2) yes . . . O2 C10 C11 123.2(2) yes . . . C9 C10 C11 118.8(3) yes . . . S2 C11 C10 119.85(19) yes . . . S2 C11 C12 119.50(17) yes . . . C10 C11 C12 120.6(2) yes . . . C7 C12 C11 119.7(3) yes . . . S6 C13 C14 120.21(17) yes . . . S6 C13 C18 118.89(18) yes . . . C14 C13 C18 120.9(3) yes . . . C13 C14 C15 119.9(2) yes . . . S1 C15 C14 125.50(16) yes 3_676 . . S1 C15 C16 114.61(19) yes 3_676 . . C14 C15 C16 119.9(2) yes . . . O3 C16 C15 116.9(2) yes . . . O3 C16 C17 123.77(19) yes . . . C15 C16 C17 119.3(3) yes . . . S3 C17 C16 118.27(19) yes . . . S3 C17 C18 120.93(17) yes . . . C16 C17 C18 120.61(19) yes . . . C13 C18 C17 119.4(2) yes . . . C4 O1 H7 109.472 no . . . C10 O2 H8 109.469 no . . . C16 O3 H9 109.475 no . . . Tb1 O13 H10 125.785 no . . . Tb1 O13 H11 118.806 no . . . H10 O13 H11 112.332 no . . . Tb1 O14 H12 122.385 no . . . Tb1 O14 H13 119.616 no . . . H12 O14 H13 104.723 no . . . Tb1 O15 H14 124.005 no . . . Tb1 O15 H15 123.940 no . . . H14 O15 H15 111.999 no . . . Tb1 O16 H16 124.561 no . . . Tb1 O16 H17 119.110 no . . . H16 O16 H17 106.817 no . . . Tb1 O17 H18 126.379 no . . . Tb1 O17 H19 114.350 no . . . H18 O17 H19 109.496 no . . . Tb1 O18 H20 122.588 no . . . Tb1 O18 H21 114.568 no . . . H20 O18 H21 109.131 no . . . Tb1 O19 H22 125.469 no . . . Tb1 O19 H23 122.989 no . . . H22 O19 H23 109.096 no . . . Tb1 O20 H24 127.227 no . . . Tb1 O20 H25 124.358 no . . . H24 O20 H25 108.268 no . . . H26 O21 H27 109.157 no . . . H28 O22 H29 108.694 no . . . H30 O23 H31 111.541 no . . . H32 O24 H33 106.471 no . . . H34 O25 H35 113.558 no . . . H36 O26 H37 118.692 no . . . H38 O27 H39 104.968 no . . . C1 C2 H1 120.094 no . . . C3 C2 H1 120.090 no . . . C1 C6 H2 119.802 no . . . C5 C6 H2 119.802 no . . . C7 C8 H3 119.876 no . . . C9 C8 H3 119.856 no . . . C7 C12 H4 120.137 no . . . C11 C12 H4 120.120 no . . . C13 C14 H5 120.056 no . . . C15 C14 H5 120.044 no . . . C13 C18 H6 120.309 no . . . C17 C18 H6 120.301 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C5 S1 C15 C14 13.3(2) no . . 3_676 3_676 C5 S1 C15 C16 -168.42(14) no . . 3_676 3_676 C15 S1 C5 C4 -85.87(18) no 3_676 . . . C15 S1 C5 C6 101.35(17) no 3_676 . . . C3 S2 C11 C10 110.25(17) no . . . . C3 S2 C11 C12 -71.37(17) no . . . . C11 S2 C3 C2 116.77(17) no . . . . C11 S2 C3 C4 -65.74(19) no . . . . C9 S3 C17 C16 100.68(17) no . . . . C9 S3 C17 C18 -84.34(17) no . . . . C17 S3 C9 C8 100.52(16) no . . . . C17 S3 C9 C10 -85.81(17) no . . . . O4 S4 C1 C2 -79.49(19) no . . . . O4 S4 C1 C6 99.67(17) no . . . . O5 S4 C1 C2 162.10(16) no . . . . O5 S4 C1 C6 -18.7(2) no . . . . O6 S4 C1 C2 40.01(19) no . . . . O6 S4 C1 C6 -140.83(16) no . . . . O7 S5 C7 C8 -71.64(18) no . . . . O7 S5 C7 C12 107.28(17) no . . . . O8 S5 C7 C8 168.57(16) no . . . . O8 S5 C7 C12 -12.5(2) no . . . . O9 S5 C7 C8 47.88(19) no . . . . O9 S5 C7 C12 -133.21(16) no . . . . O10 S6 C13 C14 -125.14(16) no . . . . O10 S6 C13 C18 55.45(18) no . . . . O11 S6 C13 C14 115.07(17) no . . . . O11 S6 C13 C18 -64.34(19) no . . . . O12 S6 C13 C14 -6.8(2) no . . . . O12 S6 C13 C18 173.83(16) no . . . . S4 C1 C2 C3 -179.30(15) no . . . . S4 C1 C6 C5 178.76(14) no . . . . C2 C1 C6 C5 -2.1(4) no . . . . C6 C1 C2 C3 1.5(4) no . . . . C1 C2 C3 S2 177.93(18) no . . . . C1 C2 C3 C4 0.4(4) no . . . . S2 C3 C4 O1 0.6(3) no . . . . S2 C3 C4 C5 -179.25(14) no . . . . C2 C3 C4 O1 178.0(2) no . . . . C2 C3 C4 C5 -1.8(4) no . . . . O1 C4 C5 S1 8.8(4) no . . . . O1 C4 C5 C6 -178.55(19) no . . . . C3 C4 C5 S1 -171.35(18) no . . . . C3 C4 C5 C6 1.3(4) no . . . . S1 C5 C6 C1 173.49(14) no . . . . C4 C5 C6 C1 0.7(4) no . . . . S5 C7 C8 C9 178.82(14) no . . . . S5 C7 C12 C11 -176.36(14) no . . . . C8 C7 C12 C11 2.5(4) no . . . . C12 C7 C8 C9 -0.1(4) no . . . . C7 C8 C9 S3 171.37(18) no . . . . C7 C8 C9 C10 -2.4(3) no . . . . S3 C9 C10 O2 7.6(3) no . . . . S3 C9 C10 C11 -171.24(14) no . . . . C8 C9 C10 O2 -178.86(19) no . . . . C8 C9 C10 C11 2.3(4) no . . . . O2 C10 C11 S2 -0.3(4) no . . . . O2 C10 C11 C12 -178.62(18) no . . . . C9 C10 C11 S2 178.47(17) no . . . . C9 C10 C11 C12 0.1(4) no . . . . S2 C11 C12 C7 179.10(14) no . . . . C10 C11 C12 C7 -2.5(4) no . . . . S6 C13 C14 C15 -178.67(14) no . . . . S6 C13 C18 C17 179.69(14) no . . . . C14 C13 C18 C17 0.3(4) no . . . . C18 C13 C14 C15 0.7(4) no . . . . C13 C14 C15 S1 -178.69(18) no . . . 3_676 C13 C14 C15 C16 -0.5(3) no . . . . S1 C15 C16 O3 -2.1(3) no 3_676 . . . S1 C15 C16 C17 177.72(13) no 3_676 . . . C14 C15 C16 O3 179.54(18) no . . . . C14 C15 C16 C17 -0.6(3) no . . . . O3 C16 C17 S3 -3.5(3) no . . . . O3 C16 C17 C18 -178.53(18) no . . . . C15 C16 C17 S3 176.64(17) no . . . . C15 C16 C17 C18 1.6(3) no . . . . S3 C17 C18 C13 -176.34(14) no . . . . C16 C17 C18 C13 -1.5(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 O1 3.105(2) no . . S1 O3 2.7973(17) no . 3_676 S2 O1 2.9690(17) no . . S2 O2 3.0602(18) no . . S3 O2 2.9854(16) no . . S3 O3 3.0331(18) no . . O1 O2 3.056(3) no . . O1 C10 3.178(3) no . . O1 C11 3.125(3) no . . O1 C14 3.594(3) no . 3_676 O2 O3 2.942(3) no . . O2 C16 3.477(3) no . . O2 C17 3.529(3) no . . O4 C2 3.318(4) no . . O4 C6 3.485(3) no . . O5 C6 2.898(3) no . . O6 C2 3.019(3) no . . O7 C8 3.250(4) no . . O7 C12 3.569(4) no . . O8 C12 2.891(4) no . . O9 C8 3.075(3) no . . O10 C18 3.122(4) no . . O11 C18 3.188(3) no . . O12 C14 2.887(4) no . . C1 C4 2.798(4) no . . C2 C5 2.791(3) no . . C3 C6 2.791(4) no . . C3 C12 3.319(3) no . . C4 C11 3.299(3) no . . C4 C14 3.548(3) no . 3_676 C4 C15 3.586(3) no . 3_676 C5 C14 3.118(4) no . 3_676 C7 C10 2.801(4) no . . C8 C11 2.788(3) no . . C9 C12 2.796(4) no . . C9 C18 3.539(4) no . . C10 C17 3.565(3) no . . C13 C16 2.792(4) no . . C14 C17 2.792(3) no . . C15 C18 2.805(4) no . . S1 O23 3.308(3) no . 2_556 S1 O26 3.498(2) no . 2_556 S1 O27 3.358(3) no . 2_556 S2 S3 3.3496(8) no . 2_545 S2 O6 3.417(3) no . 3_666 S2 C1 3.284(3) no . 3_666 S2 C2 3.286(3) no . 3_666 S3 S2 3.3496(8) no . 2_555 S3 C14 3.434(3) no . 2_545 S4 O17 3.556(3) no . . O1 O6 3.468(3) no . 3_666 O1 O21 3.482(4) no . . O1 O26 3.429(4) no . 4_564 O1 O27 2.681(3) no . 2_556 O2 O6 2.827(3) no . 3_666 O2 O11 3.299(3) no . 2_545 O2 C18 3.482(3) no . 2_545 O3 O11 3.232(3) no . 2_545 O3 O23 3.122(3) no . 4_564 O3 O26 3.319(3) no . 4_564 O3 C7 3.597(3) no . 2_555 O3 C12 3.578(3) no . 2_555 O4 O15 2.768(3) no . 2_546 O4 O17 2.985(3) no . . O4 O18 3.310(3) no . . O4 O22 3.278(3) no . . O4 O25 2.991(3) no . 2_546 O5 O14 2.720(4) no . 2_546 O5 O16 3.571(3) no . 2_546 O5 O17 3.436(3) no . . O5 C18 3.530(3) no . 4_565 O6 S2 3.417(3) no . 3_666 O6 O1 3.468(3) no . 3_666 O6 O2 2.827(3) no . 3_666 O6 O25 3.393(3) no . 2_546 O6 O26 2.801(3) no . 2_546 O7 O20 2.792(3) no . . O7 O24 2.794(3) no . 4_464 O7 O28A 3.019(5) no . . O7 O28B 3.138(13) no . . O8 O11 3.521(3) no . 1_545 O8 O18 2.700(3) no . 3_566 O8 O22 2.741(3) no . . O9 O15 2.784(3) no . 4_464 O9 O17 3.482(3) no . 4_464 O9 O23 2.869(3) no . 3_566 O9 O24 3.357(3) no . 4_464 O10 O14 3.430(3) no . 3_576 O10 O20 2.861(4) no . 3_576 O10 O25 2.874(3) no . 2_556 O10 O28A 2.812(5) no . . O10 O28B 2.797(14) no . . O11 O2 3.299(3) no . 2_555 O11 O3 3.232(3) no . 2_555 O11 O8 3.521(3) no . 1_565 O11 O16 2.716(3) no . 3_576 O12 O22 2.739(4) no . 1_565 O12 O25 3.336(4) no . 2_556 O12 C2 3.255(3) no . 1_565 O13 O21 2.687(4) no . . O13 O23 2.735(3) no . 2_556 O13 O24 3.368(3) no . 2_556 O14 O5 2.720(4) no . 2_556 O14 O10 3.430(3) no . 3_576 O14 O24 2.777(3) no . 2_556 O14 O28A 3.171(4) no . 3_576 O14 O28B 3.187(12) no . 3_576 O15 O4 2.768(3) no . 2_556 O15 O9 2.784(3) no . 4_565 O15 O23 3.487(3) no . 2_556 O15 O24 3.331(3) no . . O16 O5 3.571(3) no . 2_556 O16 O11 2.716(3) no . 3_576 O16 O23 2.707(3) no . . O17 S4 3.556(3) no . . O17 O4 2.985(3) no . . O17 O5 3.436(3) no . . O17 O9 3.482(3) no . 4_565 O17 O24 2.762(3) no . . O17 C6 3.376(4) no . . O18 O4 3.310(3) no . . O18 O8 2.700(3) no . 3_566 O18 O22 2.684(4) no . . O19 O21 2.703(4) no . . O19 O22 2.731(3) no . . O19 C1 3.598(3) no . . O19 C5 3.575(3) no . . O19 C6 3.501(3) no . . O20 O7 2.792(3) no . . O20 O10 2.861(4) no . 3_576 O21 O1 3.482(4) no . . O21 O13 2.687(4) no . . O21 O19 2.703(4) no . . O21 O27 2.737(5) no . 2_556 O21 O28A 2.598(5) no . . O21 O28B 2.770(14) no . . O21 C4 3.594(4) no . . O21 C7 3.589(4) no . . O22 O4 3.278(3) no . . O22 O8 2.741(3) no . . O22 O12 2.739(4) no . 1_545 O22 O18 2.684(4) no . . O22 O19 2.731(3) no . . O22 C2 3.588(4) no . . O22 C12 3.490(4) no . . O23 S1 3.308(3) no . 2_546 O23 O3 3.122(3) no . 4_465 O23 O9 2.869(3) no . 3_566 O23 O13 2.735(3) no . 2_546 O23 O15 3.487(3) no . 2_546 O23 O16 2.707(3) no . . O23 O26 2.790(4) no . . O24 O7 2.794(3) no . 4_565 O24 O9 3.357(3) no . 4_565 O24 O13 3.368(3) no . 2_546 O24 O14 2.777(3) no . 2_546 O24 O15 3.331(3) no . . O24 O17 2.762(3) no . . O24 O25 2.803(4) no . . O24 O28A 3.429(5) no . 4_565 O24 O28B 3.405(12) no . 4_565 O25 O4 2.991(3) no . 2_556 O25 O6 3.393(3) no . 2_556 O25 O10 2.874(3) no . 2_546 O25 O12 3.336(4) no . 2_546 O25 O24 2.803(4) no . . O25 O26 2.793(4) no . . O26 S1 3.498(2) no . 2_546 O26 O1 3.429(4) no . 4_465 O26 O3 3.319(3) no . 4_465 O26 O6 2.801(3) no . 2_556 O26 O23 2.790(4) no . . O26 O25 2.793(4) no . . O26 O27 2.678(4) no . . O27 S1 3.358(3) no . 2_546 O27 O1 2.681(3) no . 2_546 O27 O21 2.737(5) no . 2_546 O27 O26 2.678(4) no . . O27 O27 3.261(4) no . 3_567 O27 C14 3.454(3) no . 2_546 O27 C15 3.335(4) no . 2_546 O27 C16 3.438(4) no . 2_546 O28A O7 3.019(5) no . . O28A O10 2.812(5) no . . O28A O14 3.171(4) no . 3_576 O28A O21 2.598(5) no . . O28A O24 3.429(5) no . 4_464 O28A C8 3.386(5) no . . O28A C18 3.406(6) no . . O28B O7 3.138(13) no . . O28B O10 2.797(14) no . . O28B O14 3.187(12) no . 3_576 O28B O21 2.770(14) no . . O28B O24 3.405(12) no . 4_464 C1 S2 3.284(3) no . 3_666 C1 O19 3.598(3) no . . C2 S2 3.286(3) no . 3_666 C2 O12 3.255(3) no . 1_545 C2 O22 3.588(4) no . . C2 C3 3.437(4) no . 3_666 C3 C2 3.437(4) no . 3_666 C3 C3 3.524(4) no . 3_666 C4 O21 3.594(4) no . . C5 O19 3.575(3) no . . C6 O17 3.376(4) no . . C6 O19 3.501(3) no . . C7 O3 3.597(3) no . 2_545 C7 O21 3.589(4) no . . C8 O28A 3.386(5) no . . C10 C17 3.593(3) no . 2_545 C10 C18 3.600(4) no . 2_545 C11 C17 3.532(4) no . 2_545 C12 O3 3.578(3) no . 2_545 C12 O22 3.490(4) no . . C14 S3 3.434(3) no . 2_555 C14 O27 3.454(3) no . 2_556 C15 O27 3.335(4) no . 2_556 C16 O27 3.438(4) no . 2_556 C17 C10 3.593(3) no . 2_555 C17 C11 3.532(4) no . 2_555 C18 O2 3.482(3) no . 2_555 C18 O5 3.530(3) no . 4_464 C18 O28A 3.406(6) no . . C18 C10 3.600(4) no . 2_555 S1 H2 2.8030 no . . S1 H5 2.9643 no . 3_676 S1 H7 2.6222 no . . S2 H1 2.8183 no . . S2 H4 2.8413 no . . S2 H8 2.5416 no . . S3 H3 2.8195 no . . S3 H6 2.8846 no . . S3 H9 2.5120 no . . S4 H1 2.8414 no . . S4 H2 2.8265 no . . S5 H3 2.8214 no . . S5 H4 2.8483 no . . S6 H5 2.8581 no . . S6 H6 2.8227 no . . O1 H5 3.0699 no . 3_676 O1 H8 2.6885 no . . O2 H7 3.4896 no . . O2 H9 2.3814 no . . O3 H8 3.4353 no . . O4 H1 3.2735 no . . O4 H2 3.5548 no . . O5 H2 2.5247 no . . O6 H1 2.7429 no . . O7 H3 3.1609 no . . O8 H4 2.5030 no . . O9 H3 2.8256 no . . O10 H6 2.9202 no . . O11 H6 3.0478 no . . O12 H5 2.4938 no . . O13 H12 3.4945 no . . O13 H13 2.6613 no . . O13 H14 3.4264 no . . O13 H15 3.0022 no . . O13 H22 3.4898 no . . O13 H23 2.6253 no . . O14 H10 3.1550 no . . O14 H11 3.3798 no . . O14 H14 2.8528 no . . O14 H15 3.5070 no . . O14 H16 2.8812 no . . O14 H17 3.4691 no . . O14 H24 3.3912 no . . O14 H25 2.7109 no . . O15 H10 2.7660 no . . O15 H11 3.5950 no . . O15 H12 2.9610 no . . O15 H13 3.0978 no . . O15 H17 3.3156 no . . O15 H18 2.6125 no . . O15 H19 3.4739 no . . O16 H12 2.6710 no . . O16 H13 3.5448 no . . O16 H14 3.0706 no . . O16 H21 2.6542 no . . O16 H25 3.3601 no . . O17 H14 3.3240 no . . O17 H15 2.7052 no . . O17 H17 3.3538 no . . O17 H20 3.1166 no . . O17 H21 3.4121 no . . O17 H22 3.3077 no . . O18 H16 3.1794 no . . O18 H17 2.8380 no . . O18 H18 3.3374 no . . O18 H19 2.4684 no . . O18 H22 2.6582 no . . O18 H23 3.5836 no . . O18 H24 3.2720 no . . O18 H25 3.5625 no . . O19 H10 3.4508 no . . O19 H11 2.5833 no . . O19 H19 3.0609 no . . O19 H20 2.6249 no . . O19 H21 3.5514 no . . O19 H24 2.8843 no . . O20 H11 3.5179 no . . O20 H12 3.3199 no . . O20 H13 3.1893 no . . O20 H16 3.2644 no . . O20 H20 3.2513 no . . O20 H21 3.1017 no . . O20 H22 3.2291 no . . O20 H23 3.2581 no . . C2 H2 3.2680 no . . C2 H4 3.5194 no . . C3 H4 3.2153 no . . C3 H7 3.0474 no . . C3 H8 3.5722 no . . C4 H1 3.2903 no . . C4 H2 3.2803 no . . C4 H5 2.9022 no . 3_676 C4 H8 3.5934 no . . C5 H5 2.7007 no . 3_676 C5 H7 2.4649 no . . C6 H1 3.2665 no . . C6 H5 3.4890 no . 3_676 C8 H4 3.2739 no . . C9 H6 3.5073 no . . C9 H8 3.0633 no . . C9 H9 3.3505 no . . C10 H3 3.2852 no . . C10 H4 3.2868 no . . C10 H9 3.2901 no . . C11 H8 2.4308 no . . C12 H3 3.2733 no . . C14 H6 3.2819 no . . C14 H7 3.4172 no . 3_676 C15 H7 3.2269 no . 3_676 C15 H9 3.0620 no . . C16 H5 3.2867 no . . C16 H6 3.2874 no . . C17 H9 2.4405 no . . C18 H5 3.2789 no . . H1 H4 3.4161 no . . H3 H6 3.1705 no . . H5 H7 3.1086 no . 3_676 H7 H8 3.2585 no . . H8 H9 2.9660 no . . H10 H13 2.8366 no . . H10 H14 3.2519 no . . H10 H15 2.7361 no . . H10 H23 3.2871 no . . H11 H13 3.1491 no . . H11 H22 3.2832 no . . H11 H23 2.2402 no . . H12 H14 2.7371 no . . H12 H16 2.7045 no . . H12 H17 3.3300 no . . H12 H25 3.1505 no . . H13 H14 3.0604 no . . H13 H25 3.1554 no . . H14 H17 3.3034 no . . H14 H18 3.1511 no . . H15 H18 2.5344 no . . H15 H19 3.4979 no . . H16 H21 2.8062 no . . H16 H25 3.1203 no . . H17 H18 3.4127 no . . H17 H21 2.5994 no . . H19 H20 2.7044 no . . H19 H21 3.1751 no . . H19 H22 3.1110 no . . H20 H22 2.2828 no . . H20 H23 3.3789 no . . H20 H24 3.3233 no . . H21 H22 3.4009 no . . H21 H24 3.3902 no . . H21 H25 3.4576 no . . H22 H24 3.0528 no . . H23 H24 3.0672 no . . S1 H10 3.5375 no . . S1 H11 3.5958 no . . S1 H30 3.0268 no . 2_556 S1 H31 3.0270 no . 2_556 S1 H38 3.2124 no . 2_556 S1 H39 3.5116 no . 4_564 S2 H1 3.5113 no . 3_666 S3 H5 3.3743 no . 2_545 S4 H8 3.1894 no . 3_666 S4 H12 2.9707 no . 2_546 S4 H14 3.1338 no . 2_546 S4 H19 2.9287 no . . S4 H34 3.0264 no . 2_546 S5 H15 3.2110 no . 4_464 S5 H21 2.9154 no . 3_566 S5 H24 3.2940 no . . S5 H29 3.1191 no . . S5 H30 3.1267 no . 3_566 S5 H33 2.7965 no . 4_464 S6 H16 3.0777 no . 3_576 S6 H25 3.1480 no . 3_576 S6 H28 2.9703 no . 1_565 S6 H29 3.5900 no . 1_565 S6 H35 2.9233 no . 2_556 O1 H27 3.0006 no . . O1 H36 3.0124 no . 4_564 O1 H38 3.2807 no . 2_556 O1 H38 3.4874 no . 4_564 O1 H39 3.0846 no . 2_556 O2 H6 3.5131 no . 2_545 O2 H36 2.9910 no . 4_564 O3 H30 2.8723 no . 4_564 O3 H31 2.7194 no . 4_564 O3 H36 2.9494 no . 4_564 O3 H39 3.4632 no . 2_556 O4 H12 3.0898 no . 2_546 O4 H14 2.0066 no . 2_546 O4 H15 3.1147 no . 2_546 O4 H18 3.3146 no . . O4 H19 2.2065 no . . O4 H20 3.0430 no . . O4 H28 3.1782 no . . O4 H34 2.1902 no . 2_546 O4 H35 3.4494 no . 2_546 O5 H3 3.2426 no . 4_565 O5 H6 2.6360 no . 4_565 O5 H8 3.4626 no . 3_666 O5 H12 1.9871 no . 2_546 O5 H13 2.9324 no . 2_546 O5 H14 3.4174 no . 2_546 O5 H16 3.4476 no . 2_546 O5 H18 3.3503 no . . O5 H19 3.0168 no . . O6 H8 2.1059 no . 3_666 O6 H16 3.5960 no . 2_546 O6 H34 2.8643 no . 2_546 O6 H36 2.3171 no . 2_546 O6 H37 2.7322 no . 2_546 O7 H15 3.5845 no . 4_464 O7 H22 3.5879 no . . O7 H23 3.4665 no . . O7 H24 2.0792 no . . O7 H25 3.1265 no . . O7 H26 3.2328 no . . O7 H29 3.5129 no . . O7 H32 3.0702 no . 4_464 O7 H33 1.8959 no . 4_464 O8 H16 3.4138 no . 3_566 O8 H17 3.4494 no . 3_566 O8 H20 2.9133 no . 3_566 O8 H21 1.8750 no . 3_566 O8 H22 3.5498 no . . O8 H24 3.5234 no . . O8 H28 3.0373 no . . O8 H29 1.9829 no . . O8 H30 3.1972 no . 3_566 O9 H2 3.3267 no . 4_464 O9 H10 3.4768 no . 4_464 O9 H14 3.2045 no . 4_464 O9 H15 2.0726 no . 4_464 O9 H18 3.1970 no . 4_464 O9 H21 3.1666 no . 3_566 O9 H30 2.1644 no . 3_566 O9 H31 3.3751 no . 3_566 O9 H33 2.7404 no . 4_464 O10 H12 3.4681 no . 3_576 O10 H16 3.2615 no . 3_576 O10 H24 3.2314 no . 3_576 O10 H25 2.0382 no . 3_576 O10 H28 3.2733 no . 1_565 O10 H34 3.3281 no . 2_556 O10 H35 2.0836 no . 2_556 O11 H4 3.3659 no . 1_565 O11 H9 2.5664 no . 2_555 O11 H16 1.9301 no . 3_576 O11 H17 2.9706 no . 3_576 O11 H25 3.4136 no . 3_576 O11 H28 3.5086 no . 1_565 O12 H1 2.4703 no . 1_565 O12 H4 2.7778 no . 1_565 O12 H28 2.0045 no . 1_565 O12 H29 2.9367 no . 1_565 O12 H34 3.2486 no . 2_556 O12 H35 2.7944 no . 2_556 O13 H26 2.8515 no . . O13 H27 3.1958 no . . O13 H30 2.9629 no . 2_556 O13 H31 2.9755 no . 2_556 O13 H32 3.1727 no . 2_556 O14 H18 3.3639 no . 2_556 O14 H32 3.3029 no . 2_556 O14 H33 3.2639 no . 2_556 O15 H19 3.3602 no . 2_556 O15 H30 3.2748 no . 2_556 O15 H32 3.2872 no . . O15 H33 3.3621 no . . O15 H34 3.2674 no . . O16 H30 2.9670 no . . O16 H31 2.8783 no . . O17 H2 2.9672 no . . O17 H13 3.4138 no . 2_546 O17 H14 3.4831 no . 2_546 O17 H32 3.2084 no . . O17 H33 3.1565 no . . O18 H14 3.4786 no . 2_546 O18 H15 3.5449 no . 2_546 O18 H28 3.3036 no . . O18 H29 3.0023 no . . O19 H4 3.5103 no . . O19 H26 3.0685 no . . O19 H27 3.4111 no . . O19 H28 3.2401 no . . O19 H29 2.9715 no . . O20 H35 3.5709 no . 4_464 O21 H7 3.1941 no . . O21 H10 3.1600 no . . O21 H11 1.9705 no . . O21 H22 3.1375 no . . O21 H23 1.9389 no . . O21 H38 2.9987 no . 2_556 O21 H39 3.1781 no . 2_556 O22 H1 3.4019 no . . O22 H4 2.6712 no . . O22 H20 1.8951 no . . O22 H21 3.1564 no . . O22 H22 2.0402 no . . O22 H23 3.2089 no . . O22 H34 3.3143 no . 2_546 O22 H35 3.4840 no . 2_546 O23 H9 3.5147 no . 4_465 O23 H10 1.9451 no . 2_546 O23 H11 3.0239 no . 2_546 O23 H15 3.1150 no . 2_546 O23 H16 3.0040 no . . O23 H17 1.9872 no . . O23 H21 3.4386 no . . O23 H32 3.4862 no . . O23 H36 2.9727 no . . O23 H37 2.8370 no . . O24 H10 3.1937 no . 2_546 O24 H12 2.9784 no . 2_546 O24 H13 1.9940 no . 2_546 O24 H14 3.5328 no . . O24 H15 3.1103 no . . O24 H18 1.9587 no . . O24 H19 3.1174 no . . O24 H34 3.1960 no . . O24 H35 3.1703 no . . O25 H14 3.2835 no . . O25 H25 3.4861 no . 4_565 O25 H28 3.2950 no . 2_556 O25 H31 3.3973 no . . O25 H32 1.9821 no . . O25 H33 3.0633 no . . O25 H36 3.1930 no . . O25 H37 1.8826 no . . O26 H7 3.3958 no . 4_465 O26 H8 3.4175 no . 4_465 O26 H10 3.4379 no . 2_546 O26 H27 3.4548 no . 2_546 O26 H30 3.2843 no . . O26 H31 2.0815 no . . O26 H34 2.9925 no . . O26 H35 3.0885 no . . O26 H38 1.8820 no . . O26 H39 3.0239 no . . O27 H7 1.9630 no . 2_546 O27 H7 3.3708 no . 4_465 O27 H26 3.1555 no . 2_546 O27 H27 1.9002 no . 2_546 O27 H36 3.1262 no . . O27 H37 3.1244 no . . O27 H38 3.1836 no . 3_567 O27 H39 3.2769 no . 3_567 O28A H3 3.0778 no . . O28A H6 2.8725 no . . O28A H11 3.5578 no . . O28A H12 3.1626 no . 3_576 O28A H13 3.0352 no . 3_576 O28A H25 3.5095 no . 3_576 O28A H26 1.8109 no . . O28A H27 2.8926 no . . O28A H33 3.0139 no . 4_464 O28B H6 3.5907 no . . O28B H11 3.2070 no . . O28B H12 3.3722 no . 3_576 O28B H13 3.0148 no . 3_576 O28B H24 3.3895 no . . O28B H25 3.1072 no . 3_576 O28B H26 1.9857 no . . O28B H27 3.1866 no . . O28B H33 3.0594 no . 4_464 O28B H35 3.4446 no . 2_556 C1 H19 3.2292 no . . C1 H22 3.3884 no . . C2 H22 3.3548 no . . C2 H28 3.2267 no . . C3 H1 3.4052 no . 3_666 C3 H22 3.5361 no . . C3 H23 3.5413 no . . C4 H1 3.5382 no . 3_666 C4 H23 3.3286 no . . C4 H27 3.4030 no . . C5 H23 3.3325 no . . C6 H3 3.1651 no . 4_565 C6 H19 3.2533 no . . C6 H22 3.5692 no . . C6 H23 3.5736 no . . C7 H26 3.5042 no . . C8 H2 3.1110 no . 4_464 C8 H26 3.4580 no . . C12 H9 3.5659 no . 2_545 C12 H22 3.3562 no . . C12 H23 3.3777 no . . C12 H28 3.4502 no . . C12 H29 3.2278 no . . C13 H39 3.0973 no . 2_556 C14 H38 3.4385 no . 2_556 C14 H39 2.7899 no . 2_556 C15 H38 3.5520 no . 2_556 C15 H39 2.5930 no . 2_556 C16 H39 2.7277 no . 2_556 C17 H39 3.0224 no . 2_556 C18 H39 3.2149 no . 2_556 H1 S2 3.5113 no . 3_666 H1 O12 2.4703 no . 1_545 H1 O22 3.4019 no . . H1 C3 3.4052 no . 3_666 H1 C4 3.5382 no . 3_666 H1 H5 3.0089 no . 1_545 H1 H28 2.8706 no . . H1 H34 3.5563 no . 2_546 H2 O9 3.3267 no . 4_565 H2 O17 2.9672 no . . H2 C8 3.1110 no . 4_565 H2 H3 2.3300 no . 4_565 H2 H18 3.1465 no . . H2 H19 2.9695 no . . H3 O5 3.2426 no . 4_464 H3 O28A 3.0778 no . . H3 C6 3.1651 no . 4_464 H3 H2 2.3300 no . 4_464 H3 H33 3.4521 no . 4_464 H4 O11 3.3659 no . 1_545 H4 O12 2.7778 no . 1_545 H4 O19 3.5103 no . . H4 O22 2.6712 no . . H4 H9 3.5166 no . 2_545 H4 H22 2.9779 no . . H4 H23 3.3443 no . . H4 H28 2.5464 no . . H4 H29 2.4489 no . . H5 S3 3.3743 no . 2_555 H5 H1 3.0089 no . 1_565 H5 H39 3.2906 no . 2_556 H6 O2 3.5131 no . 2_555 H6 O5 2.6360 no . 4_464 H6 O28A 2.8725 no . . H6 O28B 3.5907 no . . H6 H8 3.5023 no . 2_555 H6 H12 3.3341 no . 3_576 H7 O21 3.1941 no . . H7 O26 3.3958 no . 4_564 H7 O27 1.9630 no . 2_556 H7 O27 3.3708 no . 4_564 H7 H27 2.6003 no . . H7 H36 3.0915 no . 4_564 H7 H38 2.4851 no . 2_556 H7 H38 3.0327 no . 4_564 H7 H39 2.4528 no . 2_556 H7 H39 3.1421 no . 4_564 H8 S4 3.1894 no . 3_666 H8 O5 3.4626 no . 3_666 H8 O6 2.1059 no . 3_666 H8 O26 3.4175 no . 4_564 H8 H6 3.5023 no . 2_545 H8 H36 2.6902 no . 4_564 H9 O11 2.5664 no . 2_545 H9 O23 3.5147 no . 4_564 H9 C12 3.5659 no . 2_555 H9 H4 3.5166 no . 2_555 H9 H16 3.3277 no . 4_564 H9 H17 3.5970 no . 4_564 H9 H30 3.3238 no . 4_564 H9 H31 3.1240 no . 4_564 H9 H36 3.1397 no . 4_564 H10 S1 3.5375 no . . H10 O9 3.4768 no . 4_565 H10 O21 3.1600 no . . H10 O23 1.9451 no . 2_556 H10 O24 3.1937 no . 2_556 H10 O26 3.4379 no . 2_556 H10 H26 3.3682 no . . H10 H27 3.5034 no . . H10 H30 2.2220 no . 2_556 H10 H31 2.2435 no . 2_556 H10 H32 2.9373 no . 2_556 H10 H37 3.2585 no . 2_556 H11 S1 3.5958 no . . H11 O21 1.9705 no . . H11 O23 3.0239 no . 2_556 H11 O28A 3.5578 no . . H11 O28B 3.2070 no . . H11 H26 2.1665 no . . H11 H27 2.4782 no . . H11 H30 3.2951 no . 2_556 H11 H31 3.0917 no . 2_556 H11 H32 3.3644 no . 2_556 H11 H37 3.4467 no . 2_556 H12 S4 2.9707 no . 2_556 H12 O4 3.0898 no . 2_556 H12 O5 1.9871 no . 2_556 H12 O10 3.4681 no . 3_576 H12 O24 2.9784 no . 2_556 H12 O28A 3.1626 no . 3_576 H12 O28B 3.3722 no . 3_576 H12 H6 3.3341 no . 3_576 H12 H18 3.2095 no . 2_556 H12 H19 3.2851 no . 2_556 H12 H33 3.3819 no . 2_556 H13 O5 2.9324 no . 2_556 H13 O17 3.4138 no . 2_556 H13 O24 1.9940 no . 2_556 H13 O28A 3.0352 no . 3_576 H13 O28B 3.0148 no . 3_576 H13 H18 2.8000 no . 2_556 H13 H19 3.2846 no . 2_556 H13 H32 2.5190 no . 2_556 H13 H33 2.5309 no . 2_556 H14 S4 3.1338 no . 2_556 H14 O4 2.0066 no . 2_556 H14 O5 3.4174 no . 2_556 H14 O9 3.2045 no . 4_565 H14 O17 3.4831 no . 2_556 H14 O18 3.4786 no . 2_556 H14 O24 3.5328 no . . H14 O25 3.2835 no . . H14 H18 3.5068 no . 2_556 H14 H19 2.8242 no . 2_556 H14 H20 3.5102 no . 2_556 H14 H32 3.3107 no . . H14 H33 3.5645 no . . H14 H34 2.7442 no . . H15 S5 3.2110 no . 4_565 H15 O4 3.1147 no . 2_556 H15 O7 3.5845 no . 4_565 H15 O9 2.0726 no . 4_565 H15 O18 3.5449 no . 2_556 H15 O23 3.1150 no . 2_556 H15 O24 3.1103 no . . H15 H19 3.5311 no . 2_556 H15 H21 3.4914 no . 2_556 H15 H30 2.7799 no . 2_556 H15 H32 3.1793 no . . H15 H33 2.9692 no . . H15 H34 3.4270 no . . H16 S6 3.0777 no . 3_576 H16 O5 3.4476 no . 2_556 H16 O6 3.5960 no . 2_556 H16 O8 3.4138 no . 3_566 H16 O10 3.2615 no . 3_576 H16 O11 1.9301 no . 3_576 H16 O23 3.0040 no . . H16 H9 3.3277 no . 4_465 H16 H30 3.1429 no . . H16 H31 3.0776 no . . H17 O8 3.4494 no . 3_566 H17 O11 2.9706 no . 3_576 H17 O23 1.9872 no . . H17 H9 3.5970 no . 4_465 H17 H30 2.2752 no . . H17 H31 2.2029 no . . H17 H36 3.5496 no . . H17 H37 3.5848 no . . H18 O4 3.3146 no . . H18 O5 3.3503 no . . H18 O9 3.1970 no . 4_565 H18 O14 3.3639 no . 2_546 H18 O24 1.9587 no . . H18 H2 3.1465 no . . H18 H12 3.2095 no . 2_546 H18 H13 2.8000 no . 2_546 H18 H14 3.5068 no . 2_546 H18 H32 2.4408 no . . H18 H33 2.3879 no . . H19 S4 2.9287 no . . H19 O4 2.2065 no . . H19 O5 3.0168 no . . H19 O15 3.3602 no . 2_546 H19 O24 3.1174 no . . H19 C1 3.2292 no . . H19 C6 3.2533 no . . H19 H2 2.9695 no . . H19 H12 3.2851 no . 2_546 H19 H13 3.2846 no . 2_546 H19 H14 2.8242 no . 2_546 H19 H15 3.5311 no . 2_546 H19 H33 3.5971 no . . H20 O4 3.0430 no . . H20 O8 2.9133 no . 3_566 H20 O22 1.8951 no . . H20 H14 3.5102 no . 2_546 H20 H28 2.5111 no . . H20 H29 2.2487 no . . H21 S5 2.9154 no . 3_566 H21 O8 1.8750 no . 3_566 H21 O9 3.1666 no . 3_566 H21 O22 3.1564 no . . H21 O23 3.4386 no . . H21 H15 3.4914 no . 2_546 H21 H29 3.3440 no . . H21 H29 2.9626 no . 3_566 H21 H30 3.1880 no . . H22 O7 3.5879 no . . H22 O8 3.5498 no . . H22 O21 3.1375 no . . H22 O22 2.0402 no . . H22 C1 3.3884 no . . H22 C2 3.3548 no . . H22 C3 3.5361 no . . H22 C6 3.5692 no . . H22 C12 3.3562 no . . H22 H4 2.9779 no . . H22 H26 3.4969 no . . H22 H28 2.5260 no . . H22 H29 2.3186 no . . H23 O7 3.4665 no . . H23 O21 1.9389 no . . H23 O22 3.2089 no . . H23 C3 3.5413 no . . H23 C4 3.3286 no . . H23 C5 3.3325 no . . H23 C6 3.5736 no . . H23 C12 3.3777 no . . H23 H4 3.3443 no . . H23 H26 2.3741 no . . H23 H27 2.6280 no . . H23 H29 3.3538 no . . H24 S5 3.2940 no . . H24 O7 2.0792 no . . H24 O8 3.5234 no . . H24 O10 3.2314 no . 3_576 H24 O28B 3.3895 no . . H24 H26 3.5066 no . . H24 H29 3.5664 no . . H24 H33 3.1416 no . 4_464 H24 H35 3.5111 no . 4_464 H25 S6 3.1480 no . 3_576 H25 O7 3.1265 no . . H25 O10 2.0382 no . 3_576 H25 O11 3.4136 no . 3_576 H25 O25 3.4861 no . 4_464 H25 O28A 3.5095 no . 3_576 H25 O28B 3.1072 no . 3_576 H25 H28 3.5974 no . 3_566 H25 H35 2.8735 no . 4_464 H26 O7 3.2328 no . . H26 O13 2.8515 no . . H26 O19 3.0685 no . . H26 O27 3.1555 no . 2_556 H26 O28A 1.8109 no . . H26 O28B 1.9857 no . . H26 C7 3.5042 no . . H26 C8 3.4580 no . . H26 H10 3.3682 no . . H26 H11 2.1665 no . . H26 H22 3.4969 no . . H26 H23 2.3741 no . . H26 H24 3.5066 no . . H26 H38 3.3707 no . 2_556 H26 H39 3.4689 no . 2_556 H27 O1 3.0006 no . . H27 O13 3.1958 no . . H27 O19 3.4111 no . . H27 O26 3.4548 no . 2_556 H27 O27 1.9002 no . 2_556 H27 O28A 2.8926 no . . H27 O28B 3.1866 no . . H27 C4 3.4030 no . . H27 H7 2.6003 no . . H27 H10 3.5034 no . . H27 H11 2.4782 no . . H27 H23 2.6280 no . . H27 H37 3.5370 no . 2_556 H27 H38 2.2460 no . 2_556 H27 H39 2.3259 no . 2_556 H28 S6 2.9703 no . 1_545 H28 O4 3.1782 no . . H28 O8 3.0373 no . . H28 O10 3.2733 no . 1_545 H28 O11 3.5086 no . 1_545 H28 O12 2.0045 no . 1_545 H28 O18 3.3036 no . . H28 O19 3.2401 no . . H28 O25 3.2950 no . 2_546 H28 C2 3.2267 no . . H28 C12 3.4502 no . . H28 H1 2.8706 no . . H28 H4 2.5464 no . . H28 H20 2.5111 no . . H28 H22 2.5260 no . . H28 H25 3.5974 no . 3_566 H28 H34 2.9098 no . 2_546 H28 H35 2.9686 no . 2_546 H29 S5 3.1191 no . . H29 S6 3.5900 no . 1_545 H29 O7 3.5129 no . . H29 O8 1.9829 no . . H29 O12 2.9367 no . 1_545 H29 O18 3.0023 no . . H29 O19 2.9715 no . . H29 C12 3.2278 no . . H29 H4 2.4489 no . . H29 H20 2.2487 no . . H29 H21 3.3440 no . . H29 H21 2.9626 no . 3_566 H29 H22 2.3186 no . . H29 H23 3.3538 no . . H29 H24 3.5664 no . . H30 S1 3.0268 no . 2_546 H30 S5 3.1267 no . 3_566 H30 O3 2.8723 no . 4_465 H30 O8 3.1972 no . 3_566 H30 O9 2.1644 no . 3_566 H30 O13 2.9629 no . 2_546 H30 O15 3.2748 no . 2_546 H30 O16 2.9670 no . . H30 O26 3.2843 no . . H30 H9 3.3238 no . 4_465 H30 H10 2.2220 no . 2_546 H30 H11 3.2951 no . 2_546 H30 H15 2.7799 no . 2_546 H30 H16 3.1429 no . . H30 H17 2.2752 no . . H30 H21 3.1880 no . . H30 H36 3.4092 no . . H30 H37 3.4706 no . . H31 S1 3.0270 no . 2_546 H31 O3 2.7194 no . 4_465 H31 O9 3.3751 no . 3_566 H31 O13 2.9755 no . 2_546 H31 O16 2.8783 no . . H31 O25 3.3973 no . . H31 O26 2.0815 no . . H31 H9 3.1240 no . 4_465 H31 H10 2.2435 no . 2_546 H31 H11 3.0917 no . 2_546 H31 H16 3.0776 no . . H31 H17 2.2029 no . . H31 H36 2.2371 no . . H31 H37 2.2569 no . . H31 H38 3.4401 no . . H32 O7 3.0702 no . 4_565 H32 O13 3.1727 no . 2_546 H32 O14 3.3029 no . 2_546 H32 O15 3.2872 no . . H32 O17 3.2084 no . . H32 O23 3.4862 no . . H32 O25 1.9821 no . . H32 H10 2.9373 no . 2_546 H32 H11 3.3644 no . 2_546 H32 H13 2.5190 no . 2_546 H32 H14 3.3107 no . . H32 H15 3.1793 no . . H32 H18 2.4408 no . . H32 H34 2.4390 no . . H32 H35 2.3803 no . . H32 H37 3.2736 no . . H33 S5 2.7965 no . 4_565 H33 O7 1.8959 no . 4_565 H33 O9 2.7404 no . 4_565 H33 O14 3.2639 no . 2_546 H33 O15 3.3621 no . . H33 O17 3.1565 no . . H33 O25 3.0633 no . . H33 O28A 3.0139 no . 4_565 H33 O28B 3.0594 no . 4_565 H33 H3 3.4521 no . 4_565 H33 H12 3.3819 no . 2_546 H33 H13 2.5309 no . 2_546 H33 H14 3.5645 no . . H33 H15 2.9692 no . . H33 H18 2.3879 no . . H33 H19 3.5971 no . . H33 H24 3.1416 no . 4_565 H33 H34 3.3715 no . . H33 H35 3.3059 no . . H34 S4 3.0264 no . 2_556 H34 O4 2.1902 no . 2_556 H34 O6 2.8643 no . 2_556 H34 O10 3.3281 no . 2_546 H34 O12 3.2486 no . 2_546 H34 O15 3.2674 no . . H34 O22 3.3143 no . 2_556 H34 O24 3.1960 no . . H34 O26 2.9925 no . . H34 H1 3.5563 no . 2_556 H34 H14 2.7442 no . . H34 H15 3.4270 no . . H34 H28 2.9098 no . 2_556 H34 H32 2.4390 no . . H34 H33 3.3715 no . . H34 H36 3.2195 no . . H34 H37 2.1390 no . . H35 S6 2.9233 no . 2_546 H35 O4 3.4494 no . 2_556 H35 O10 2.0836 no . 2_546 H35 O12 2.7944 no . 2_546 H35 O20 3.5709 no . 4_565 H35 O22 3.4840 no . 2_556 H35 O24 3.1703 no . . H35 O26 3.0885 no . . H35 O28B 3.4446 no . 2_546 H35 H24 3.5111 no . 4_565 H35 H25 2.8735 no . 4_565 H35 H28 2.9686 no . 2_556 H35 H32 2.3803 no . . H35 H33 3.3059 no . . H35 H36 3.5510 no . . H35 H37 2.2038 no . . H36 O1 3.0124 no . 4_465 H36 O2 2.9910 no . 4_465 H36 O3 2.9494 no . 4_465 H36 O6 2.3171 no . 2_556 H36 O23 2.9727 no . . H36 O25 3.1930 no . . H36 O27 3.1262 no . . H36 H7 3.0915 no . 4_465 H36 H8 2.6902 no . 4_465 H36 H9 3.1397 no . 4_465 H36 H17 3.5496 no . . H36 H30 3.4092 no . . H36 H31 2.2371 no . . H36 H34 3.2195 no . . H36 H35 3.5510 no . . H36 H38 2.3220 no . . H36 H39 3.4224 no . . H37 O6 2.7322 no . 2_556 H37 O23 2.8370 no . . H37 O25 1.8826 no . . H37 O27 3.1244 no . . H37 H10 3.2585 no . 2_546 H37 H11 3.4467 no . 2_546 H37 H17 3.5848 no . . H37 H27 3.5370 no . 2_546 H37 H30 3.4706 no . . H37 H31 2.2569 no . . H37 H32 3.2736 no . . H37 H34 2.1390 no . . H37 H35 2.2038 no . . H37 H38 2.3904 no . . H37 H39 3.3968 no . . H38 S1 3.2124 no . 2_546 H38 O1 3.2807 no . 2_546 H38 O1 3.4874 no . 4_465 H38 O21 2.9987 no . 2_546 H38 O26 1.8820 no . . H38 O27 3.1836 no . 3_567 H38 C14 3.4385 no . 2_546 H38 C15 3.5520 no . 2_546 H38 H7 2.4851 no . 2_546 H38 H7 3.0327 no . 4_465 H38 H26 3.3707 no . 2_546 H38 H27 2.2460 no . 2_546 H38 H31 3.4401 no . . H38 H36 2.3220 no . . H38 H37 2.3904 no . . H38 H38 3.3085 no . 3_567 H38 H39 3.1506 no . 3_567 H39 S1 3.5116 no . 4_465 H39 O1 3.0846 no . 2_546 H39 O3 3.4632 no . 2_546 H39 O21 3.1781 no . 2_546 H39 O26 3.0239 no . . H39 O27 3.2769 no . 3_567 H39 C13 3.0973 no . 2_546 H39 C14 2.7899 no . 2_546 H39 C15 2.5930 no . 2_546 H39 C16 2.7277 no . 2_546 H39 C17 3.0224 no . 2_546 H39 C18 3.2149 no . 2_546 H39 H5 3.2906 no . 2_546 H39 H7 2.4528 no . 2_546 H39 H7 3.1421 no . 4_465 H39 H26 3.4689 no . 2_546 H39 H27 2.3259 no . 2_546 H39 H36 3.4224 no . . H39 H37 3.3968 no . . H39 H38 3.1506 no . 3_567 H39 H39 3.4610 no . 3_567 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H7 S1 . . . 3.105(2) 0.840 2.622 117.9 no O1 H7 O27 . . 2_556 2.681(3) 0.840 1.963 142.9 no O2 H8 S2 . . . 3.0602(18) 0.840 2.542 121.0 no O2 H8 O6 . . 3_666 2.827(3) 0.840 2.106 143.6 no O3 H9 S3 . . . 3.0331(18) 0.840 2.512 121.2 no O3 H9 O2 . . . 2.942(3) 0.840 2.381 124.7 no O13 H10 O23 . . 2_556 2.735(3) 0.801 1.945 168.5 no O13 H11 O21 . . . 2.687(4) 0.727 1.970 168.5 no O14 H12 O5 . . 2_556 2.720(4) 0.741 1.987 170.2 no O14 H13 O24 . . 2_556 2.777(3) 0.790 1.994 171.1 no O15 H14 O4 . . 2_556 2.768(3) 0.761 2.007 179.0 no O15 H15 O9 . . 4_565 2.784(3) 0.715 2.073 173.0 no O16 H16 O11 . . 3_576 2.716(3) 0.788 1.930 175.2 no O16 H17 O23 . . . 2.707(3) 0.721 1.987 176.0 no O17 H18 O24 . . . 2.762(3) 0.804 1.959 178.0 no O17 H19 O4 . . . 2.985(3) 0.793 2.207 167.1 no O18 H20 O22 . . . 2.684(4) 0.805 1.895 166.6 no O18 H21 O8 . . 3_566 2.700(3) 0.860 1.875 160.4 no O19 H22 O22 . . . 2.731(3) 0.719 2.040 161.2 no O19 H23 O21 . . . 2.703(4) 0.800 1.939 159.7 no O20 H24 O7 . . . 2.792(3) 0.718 2.079 172.1 no O20 H25 O10 . . 3_576 2.861(4) 0.838 2.038 167.1 no O21 H26 O28A . . . 2.598(5) 0.802 1.811 166.6 no O21 H26 O28B . . . 2.770(14) 0.802 1.986 165.9 no O21 H27 O27 . . 2_556 2.737(5) 0.857 1.900 164.8 no O22 H28 O12 . . 1_545 2.739(4) 0.760 2.005 162.6 no O22 H29 O8 . . . 2.741(3) 0.776 1.983 165.3 no O23 H30 O9 . . 3_566 2.869(3) 0.748 2.164 157.3 no O23 H31 O26 . . . 2.790(4) 0.751 2.081 157.6 no O24 H32 O25 . . . 2.803(4) 0.839 1.982 165.9 no O24 H33 O7 . . 4_565 2.794(3) 0.905 1.896 171.4 no O25 H34 O4 . . 2_556 2.991(3) 0.807 2.190 171.6 no O25 H35 O10 . . 2_546 2.874(3) 0.793 2.084 173.9 no O26 H36 O6 . . 2_556 2.801(3) 0.735 2.317 124.7 no O26 H37 O25 . . . 2.793(4) 0.912 1.883 176.1 no O27 H38 O26 . . . 2.678(4) 0.809 1.882 168.1 no _database_code_depnum_ccdc_archive 'CCDC 894438' ####################################################################### # # 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_General #TrackingRef 'TC6A-SO3CeCIF.cif' _audit_creation_date 2010-06-17 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'TC6A-SO3TmCIF.cif' #============================================================================== data_TC6A-SO3Tm #TrackingRef 'TC6A-SO3TmCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H78 Tm2 O56 S12 ' _chemical_formula_moiety 'C36 H78 Tm2 O56 S12 ' _chemical_formula_weight 2129.57 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.4846(7) _cell_length_b 12.3023(5) _cell_length_c 20.5851(8) _cell_angle_alpha 90.0000 _cell_angle_beta 110.4513(12) _cell_angle_gamma 90.0000 _cell_volume 3674.2(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 29186 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.45 _cell_measurement_temperature 100.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144.00 _exptl_absorpt_coefficient_mu 2.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.566 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 35142 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). The water molecule (O28) indicated disordering at two positions (A and B sites) and was isotropically refined. The parts containing (O28A and O28B) were refined as the disordered water molecules, occupancy of which was fixed at 0.57 and 0.43. Rasidual electron density was located around 1 angstrom from thulium metal center. ; _reflns_number_total 8355 _reflns_number_gt 7857 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0619 _refine_ls_number_restraints 9 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8355 _refine_ls_number_parameters 598 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0135P)^2^+14.3059P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.670 _refine_diff_density_min -0.800 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Tm Tm -0.314 5.248 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Tm1 Tm 0.16751(3) 0.23629(4) 0.64819(2) 0.01061(16) Uani 1.0 4 d . . . S1 S 0.38054(19) 0.0604(2) 0.40351(13) 0.0103(5) Uani 1.0 4 d . . . S2 S 0.21513(18) 0.4137(2) 0.24047(13) 0.0099(5) Uani 1.0 4 d . . . S3 S 0.51481(18) 0.6606(2) 0.37038(14) 0.0107(5) Uani 1.0 4 d . . . S4 S 0.41514(19) -0.0868(2) 0.66173(14) 0.0113(6) Uani 1.0 4 d . . . S5 S 0.02051(19) 0.1643(3) 0.35902(14) 0.0136(6) Uani 1.0 4 d . . . S6 S 0.17570(19) 0.7654(3) 0.39250(15) 0.0132(6) Uani 1.0 4 d . . . O1 O 0.4472(6) 0.2682(7) 0.4778(5) 0.0145(16) Uani 1.0 4 d . . . O2 O 0.3709(6) 0.2677(7) 0.3189(4) 0.0132(16) Uani 1.0 4 d . . . O3 O 0.4135(6) 0.4911(7) 0.2886(5) 0.0140(16) Uani 1.0 4 d . . . O4 O 0.4710(6) -0.0542(7) 0.7323(5) 0.0183(18) Uani 1.0 4 d . . . O5 O 0.4477(6) -0.1840(7) 0.6375(5) 0.0185(18) Uani 1.0 4 d . . . O6 O 0.3165(6) -0.0936(7) 0.6529(5) 0.0170(17) Uani 1.0 4 d . . . O7 O 0.0128(7) 0.2443(8) 0.4091(5) 0.024(2) Uani 1.0 4 d . . . O8 O 0.0290(7) 0.0529(8) 0.3863(5) 0.024(2) Uani 1.0 4 d . . . O9 O -0.0532(6) 0.1749(8) 0.2925(5) 0.0195(18) Uani 1.0 4 d . . . O10 O 0.1336(6) 0.6935(8) 0.4306(5) 0.0192(18) Uani 1.0 4 d . . . O11 O 0.1070(6) 0.8133(8) 0.3317(5) 0.0211(19) Uani 1.0 4 d . . . O12 O 0.2373(6) 0.8440(8) 0.4391(5) 0.0208(19) Uani 1.0 4 d . . . O13 O 0.0365(7) 0.2575(10) 0.5498(5) 0.028(3) Uani 1.0 4 d . . . O14 O 0.2399(7) 0.3832(8) 0.6197(6) 0.022(2) Uani 1.0 4 d . . . O15 O 0.0850(7) 0.3902(8) 0.6612(5) 0.0159(17) Uani 1.0 4 d . . . O16 O 0.2566(7) 0.3131(9) 0.7545(5) 0.0173(19) Uani 1.0 4 d . . . O17 O 0.0800(7) 0.1860(8) 0.7127(5) 0.0158(17) Uani 1.0 4 d . . . O18 O 0.2894(7) 0.1228(8) 0.7087(6) 0.022(2) Uani 1.0 4 d . . . O19 O 0.1253(8) 0.0530(8) 0.6195(6) 0.026(3) Uani 1.0 4 d . . . O20 O 0.2190(6) 0.1843(8) 0.5583(5) 0.0165(17) Uani 1.0 4 d . . . O21 O 0.1582(8) -0.0182(8) 0.5069(5) 0.0209(19) Uani 1.0 4 d . . . O22 O 0.3806(7) 0.5094(8) 0.7032(5) 0.0185(18) Uani 1.0 4 d . . . O23 O 0.1316(7) 0.6064(8) 0.6481(5) 0.0223(19) Uani 1.0 4 d . . . O24 O 0.2359(8) 0.7025(9) 0.5765(6) 0.027(2) Uani 1.0 4 d . . . O25 O 0.4031(9) 0.6044(9) 0.5868(6) 0.032(3) Uani 1.0 4 d . . . O26 O 0.3903(9) 0.4740(8) 0.4799(6) 0.032(3) Uani 1.0 4 d . . . O27 O 0.2421(10) 0.3638(10) 0.4908(6) 0.034(3) Uani 1.0 4 d . . . O28A O 0.0956(15) 0.4685(18) 0.4152(14) 0.039(9) Uiso 0.57(7) 4 d . . . O28B O 0.082(4) 0.479(4) 0.448(4) 0.079(17) Uiso 0.43(7) 4 d . . . C1 C 0.4233(8) 0.0212(9) 0.6073(6) 0.010(2) Uani 1.0 4 d . . . C2 C 0.4000(8) 0.0035(9) 0.5367(6) 0.011(2) Uani 1.0 4 d . . . C3 C 0.4076(8) 0.0877(9) 0.4936(6) 0.009(2) Uani 1.0 4 d . . . C4 C 0.4385(8) 0.1910(9) 0.5213(6) 0.010(2) Uani 1.0 4 d . . . C5 C 0.4602(8) 0.2076(9) 0.5927(6) 0.010(2) Uani 1.0 4 d . . . C6 C 0.4517(8) 0.1228(9) 0.6349(6) 0.010(2) Uani 1.0 4 d . . . C7 C 0.1252(8) 0.1911(10) 0.3461(6) 0.013(3) Uani 1.0 4 d . . . C8 C 0.1319(8) 0.2834(9) 0.3088(6) 0.010(2) Uani 1.0 4 d . . . C9 C 0.2142(8) 0.3070(9) 0.2990(6) 0.010(2) Uani 1.0 4 d . . . C10 C 0.2922(8) 0.2401(9) 0.3287(6) 0.011(2) Uani 1.0 4 d . . . C11 C 0.2838(8) 0.1477(9) 0.3668(6) 0.010(2) Uani 1.0 4 d . . . C12 C 0.2004(8) 0.1225(9) 0.3737(6) 0.011(2) Uani 1.0 4 d . . . C13 C 0.2473(8) 0.6813(9) 0.3626(6) 0.010(2) Uani 1.0 4 d . . . C14 C 0.3404(8) 0.7068(9) 0.3786(6) 0.010(2) Uani 1.0 4 d . . . C15 C 0.3953(8) 0.6416(9) 0.3538(6) 0.010(2) Uani 1.0 4 d . . . C16 C 0.3566(8) 0.5499(9) 0.3120(6) 0.009(2) Uani 1.0 4 d . . . C17 C 0.2634(8) 0.5255(9) 0.2972(6) 0.009(2) Uani 1.0 4 d . . . C18 C 0.2078(8) 0.5916(9) 0.3210(6) 0.011(2) Uani 1.0 4 d . . . H1 H 0.3787 -0.0660 0.5177 0.0128 Uiso 1.0 4 calc R . . H2 H 0.4657 0.1351 0.6830 0.0122 Uiso 1.0 4 calc R . . H3 H 0.0803 0.3300 0.2901 0.0124 Uiso 1.0 4 calc R . . H4 H 0.1945 0.0582 0.3974 0.0134 Uiso 1.0 4 calc R . . H5 H 0.3660 0.7685 0.4064 0.0118 Uiso 1.0 4 calc R . . H6 H 0.1440 0.5761 0.3092 0.0128 Uiso 1.0 4 calc R . . H7 H 0.4426 0.3299 0.4938 0.0174 Uiso 1.0 4 calc R . . H8 H 0.4119 0.2219 0.3384 0.0158 Uiso 1.0 4 calc R . . H9 H 0.3847 0.4377 0.2658 0.0168 Uiso 1.0 4 calc R . . H10 H 0.0289 0.2452 0.5077 0.0241 Uiso 1.0 4 calc R . . H11 H -0.0096 0.2969 0.5492 0.0715 Uiso 1.0 4 calc R . . H12 H 0.2729 0.4224 0.6443 0.0292 Uiso 1.0 4 calc R . . H13 H 0.2415 0.3869 0.5820 0.0621 Uiso 1.0 4 calc R . . H14 H 0.0662 0.4000 0.6905 0.0133 Uiso 1.0 4 calc R . . H15 H 0.1055 0.4454 0.6584 0.0435 Uiso 1.0 4 calc R . . H16 H 0.3124 0.3157 0.7674 0.0208 Uiso 1.0 4 calc R . . H17 H 0.2377 0.3361 0.7704 0.0064 Uiso 1.0 4 calc R . . H18 H 0.0248 0.1927 0.6978 0.0238 Uiso 1.0 4 calc R . . H19 H 0.0935 0.1368 0.7374 0.0287 Uiso 1.0 4 calc R . . H20 H 0.2856 0.0591 0.6915 0.0274 Uiso 1.0 4 calc R . . H21 H 0.3055 0.1139 0.7469 0.0212 Uiso 1.0 4 calc R . . H22 H 0.0718 0.0397 0.6194 0.0214 Uiso 1.0 4 calc R . . H23 H 0.1342 0.0215 0.5852 0.0374 Uiso 1.0 4 calc R . . H24 H 0.2080 0.1228 0.5449 0.0242 Uiso 1.0 4 calc R . . H25 H 0.2304 0.2270 0.5270 0.0386 Uiso 1.0 4 calc R . . H26 H 0.1902 -0.0671 0.4989 0.0238 Uiso 1.0 4 calc R . . H27 H 0.1090 -0.0101 0.4759 0.1074 Uiso 1.0 4 calc R . . H28 H 0.4034 0.5377 0.6782 0.0254 Uiso 1.0 4 calc R . . H29 H 0.4114 0.4648 0.7309 0.0538 Uiso 1.0 4 calc R . . H30 H 0.1688 0.6236 0.6236 0.0342 Uiso 1.0 4 calc R . . H31 H 0.0875 0.6580 0.6338 0.0347 Uiso 1.0 4 calc R . . H32 H 0.2092 0.7017 0.5338 0.0542 Uiso 1.0 4 calc R . . H33 H 0.2652 0.7572 0.5930 0.1869 Uiso 1.0 4 calc R . . H34 H 0.3528 0.6350 0.5804 0.0667 Uiso 1.0 4 calc R . . H35 H 0.4456 0.6464 0.6049 0.0406 Uiso 1.0 4 calc R . . H36 H 0.3935 0.5217 0.5075 0.0647 Uiso 1.0 4 calc R . . H37 H 0.3869 0.5034 0.4452 0.0376 Uiso 1.0 4 calc R . . H38 H 0.1959 0.3915 0.4705 0.0108 Uiso 1.0 4 calc R . . H39 H 0.2770 0.4068 0.4815 0.1137 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tm1 0.0103(3) 0.0115(3) 0.0103(3) -0.00158(18) 0.00387(17) -0.00207(18) S1 0.0117(13) 0.0100(12) 0.0082(12) 0.0013(10) 0.0022(10) -0.0003(10) S2 0.0119(13) 0.0083(12) 0.0074(12) -0.0011(10) 0.0007(10) 0.0003(9) S3 0.0090(12) 0.0096(12) 0.0132(12) -0.0012(10) 0.0036(10) -0.0032(10) S4 0.0123(13) 0.0101(12) 0.0117(12) 0.0005(10) 0.0046(10) 0.0031(10) S5 0.0103(13) 0.0162(13) 0.0144(13) -0.0011(10) 0.0044(11) 0.0015(11) S6 0.0103(13) 0.0128(13) 0.0171(13) 0.0000(10) 0.0055(11) -0.0045(11) O1 0.022(5) 0.008(4) 0.015(4) -0.002(4) 0.008(4) 0.001(3) O2 0.012(4) 0.013(4) 0.014(4) 0.001(3) 0.004(3) 0.004(3) O3 0.013(4) 0.011(4) 0.019(4) -0.002(3) 0.006(4) -0.006(4) O4 0.018(5) 0.021(5) 0.012(4) -0.002(4) 0.001(4) 0.004(4) O5 0.022(5) 0.012(4) 0.023(5) 0.000(4) 0.010(4) 0.002(4) O6 0.012(4) 0.019(5) 0.020(5) -0.001(4) 0.006(4) 0.006(4) O7 0.019(5) 0.032(5) 0.021(5) 0.003(4) 0.009(4) -0.002(4) O8 0.015(5) 0.023(5) 0.034(6) -0.000(4) 0.008(4) 0.011(4) O9 0.010(4) 0.027(5) 0.020(5) -0.001(4) 0.003(4) -0.001(4) O10 0.017(5) 0.022(5) 0.022(5) -0.001(4) 0.011(4) -0.003(4) O11 0.015(5) 0.022(5) 0.027(5) 0.007(4) 0.007(4) 0.001(4) O12 0.015(5) 0.022(5) 0.026(5) -0.003(4) 0.007(4) -0.014(4) O13 0.014(5) 0.052(7) 0.015(5) 0.009(5) 0.002(4) -0.014(5) O14 0.027(6) 0.025(5) 0.014(5) -0.013(4) 0.008(4) -0.007(4) O15 0.019(5) 0.013(5) 0.017(5) 0.000(4) 0.008(4) -0.001(4) O16 0.010(5) 0.028(5) 0.014(5) 0.002(4) 0.004(4) -0.009(4) O17 0.012(5) 0.017(5) 0.019(5) 0.003(4) 0.006(4) 0.006(4) O18 0.028(6) 0.019(5) 0.017(5) 0.007(4) 0.005(4) -0.002(4) O19 0.030(6) 0.025(5) 0.032(6) -0.015(5) 0.022(5) -0.014(5) O20 0.020(5) 0.016(5) 0.016(4) -0.002(4) 0.009(4) -0.004(4) O21 0.025(5) 0.020(5) 0.019(5) 0.003(4) 0.009(4) -0.006(4) O22 0.019(5) 0.018(5) 0.019(5) -0.000(4) 0.007(4) -0.003(4) O23 0.026(5) 0.017(5) 0.026(5) 0.001(4) 0.011(5) 0.002(4) O24 0.030(6) 0.030(6) 0.020(5) -0.004(5) 0.009(5) 0.001(5) O25 0.040(7) 0.017(5) 0.040(7) -0.003(5) 0.015(6) -0.005(5) O26 0.061(8) 0.017(5) 0.022(6) 0.008(5) 0.021(6) 0.009(5) O27 0.051(8) 0.030(6) 0.022(5) -0.002(6) 0.016(6) 0.004(5) C1 0.009(5) 0.011(5) 0.012(5) 0.001(4) 0.004(4) 0.005(4) C2 0.008(5) 0.008(5) 0.015(5) -0.000(4) 0.003(4) -0.000(4) C3 0.009(5) 0.011(5) 0.006(5) 0.001(4) 0.001(4) 0.000(4) C4 0.009(5) 0.010(5) 0.012(5) 0.001(4) 0.003(4) 0.001(4) C5 0.007(5) 0.009(5) 0.013(5) 0.000(4) 0.001(4) -0.002(4) C6 0.007(5) 0.013(5) 0.009(5) -0.000(4) 0.002(4) -0.001(4) C7 0.010(6) 0.015(6) 0.014(5) -0.005(5) 0.005(5) -0.003(5) C8 0.011(5) 0.011(5) 0.006(5) -0.000(4) -0.001(4) -0.002(4) C9 0.012(6) 0.008(5) 0.007(5) -0.002(4) 0.001(4) -0.001(4) C10 0.012(6) 0.010(5) 0.009(5) -0.002(4) 0.003(4) -0.004(4) C11 0.012(6) 0.010(5) 0.006(5) 0.000(4) 0.000(4) -0.002(4) C12 0.014(6) 0.012(5) 0.006(5) -0.003(4) 0.002(4) -0.000(4) C13 0.011(5) 0.010(5) 0.010(5) 0.002(4) 0.004(4) 0.000(4) C14 0.012(6) 0.009(5) 0.007(5) -0.000(4) 0.002(4) -0.000(4) C15 0.009(5) 0.008(5) 0.011(5) -0.000(4) 0.002(4) 0.003(4) C16 0.012(6) 0.009(5) 0.006(5) 0.002(4) 0.001(4) 0.002(4) C17 0.011(5) 0.008(5) 0.007(5) -0.001(4) 0.001(4) -0.000(4) C18 0.010(5) 0.011(5) 0.010(5) 0.001(4) 0.003(4) 0.001(4) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tm1 O13 2.327(9) yes . . Tm1 O14 2.308(11) yes . . Tm1 O15 2.352(10) yes . . Tm1 O16 2.341(9) yes . . Tm1 O17 2.289(12) yes . . Tm1 O18 2.329(10) yes . . Tm1 O19 2.365(10) yes . . Tm1 O20 2.345(11) yes . . S1 C3 1.784(11) yes . . S1 C11 1.782(11) yes . . S2 C9 1.785(12) yes . . S2 C17 1.790(11) yes . . S3 C5 1.774(11) yes . 3_666 S3 C15 1.775(12) yes . . S4 O4 1.464(8) yes . . S4 O5 1.452(10) yes . . S4 O6 1.476(10) yes . . S4 C1 1.771(12) yes . . S5 O7 1.460(11) yes . . S5 O8 1.470(10) yes . . S5 O9 1.450(8) yes . . S5 C7 1.764(14) yes . . S6 O10 1.476(11) yes . . S6 O11 1.454(9) yes . . S6 O12 1.458(9) yes . . S6 C13 1.776(13) yes . . O1 C4 1.345(15) yes . . O2 C10 1.345(16) yes . . O3 C16 1.352(16) yes . . C1 C2 1.387(16) yes . . C1 C6 1.380(15) yes . . C2 C3 1.396(17) yes . . C3 C4 1.407(15) yes . . C4 C5 1.405(17) yes . . C5 C6 1.392(17) yes . . C7 C8 1.394(17) yes . . C7 C12 1.388(16) yes . . C8 C9 1.388(18) yes . . C9 C10 1.412(15) yes . . C10 C11 1.413(16) yes . . C11 C12 1.384(18) yes . . C13 C14 1.397(16) yes . . C13 C18 1.400(15) yes . . C14 C15 1.391(18) yes . . C15 C16 1.418(15) yes . . C16 C17 1.399(16) yes . . C17 C18 1.393(18) yes . . O1 H7 0.840 no . . O2 H8 0.840 no . . O3 H9 0.840 no . . O13 H10 0.845 no . . O13 H11 0.860 no . . O14 H12 0.755 no . . O14 H13 0.786 no . . O15 H14 0.764 no . . O15 H15 0.760 no . . O16 H16 0.810 no . . O16 H17 0.582 no . . O17 H18 0.804 no . . O17 H19 0.771 no . . O18 H20 0.853 no . . O18 H21 0.744 no . . O19 H22 0.844 no . . O19 H23 0.857 no . . O20 H24 0.803 no . . O20 H25 0.895 no . . O21 H26 0.832 no . . O21 H27 0.811 no . . O22 H28 0.799 no . . O22 H29 0.814 no . . O23 H30 0.913 no . . O23 H31 0.902 no . . O24 H32 0.831 no . . O24 H33 0.817 no . . O25 H34 0.834 no . . O25 H35 0.818 no . . O26 H36 0.807 no . . O26 H37 0.785 no . . O27 H38 0.771 no . . O27 H39 0.825 no . . C2 H1 0.950 no . . C6 H2 0.950 no . . C8 H3 0.950 no . . C12 H4 0.950 no . . C14 H5 0.950 no . . C18 H6 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O13 Tm1 O14 92.5(4) yes . . . O13 Tm1 O15 70.5(4) yes . . . O13 Tm1 O16 145.0(4) yes . . . O13 Tm1 O17 91.3(4) yes . . . O13 Tm1 O18 146.1(4) yes . . . O13 Tm1 O19 79.0(4) yes . . . O13 Tm1 O20 77.1(4) yes . . . O14 Tm1 O15 74.3(4) yes . . . O14 Tm1 O16 75.0(4) yes . . . O14 Tm1 O17 142.9(4) yes . . . O14 Tm1 O18 103.3(4) yes . . . O14 Tm1 O19 143.1(5) yes . . . O14 Tm1 O20 71.6(4) yes . . . O15 Tm1 O16 74.6(4) yes . . . O15 Tm1 O17 72.3(4) yes . . . O15 Tm1 O18 142.5(4) yes . . . O15 Tm1 O19 133.0(4) yes . . . O15 Tm1 O20 131.1(4) yes . . . O16 Tm1 O17 80.9(4) yes . . . O16 Tm1 O18 68.8(4) yes . . . O16 Tm1 O19 129.8(4) yes . . . O16 Tm1 O20 126.6(4) yes . . . O17 Tm1 O18 93.5(4) yes . . . O17 Tm1 O19 73.7(4) yes . . . O17 Tm1 O20 144.9(4) yes . . . O18 Tm1 O19 70.3(4) yes . . . O18 Tm1 O20 79.8(4) yes . . . O19 Tm1 O20 71.5(4) yes . . . C3 S1 C11 100.6(6) yes . . . C9 S2 C17 102.9(5) yes . . . C5 S3 C15 105.1(6) yes 3_666 . . O4 S4 O5 114.2(5) yes . . . O4 S4 O6 111.4(6) yes . . . O4 S4 C1 105.9(5) yes . . . O5 S4 O6 112.4(6) yes . . . O5 S4 C1 106.9(6) yes . . . O6 S4 C1 105.3(5) yes . . . O7 S5 O8 112.1(7) yes . . . O7 S5 O9 112.0(6) yes . . . O7 S5 C7 106.7(6) yes . . . O8 S5 O9 112.4(6) yes . . . O8 S5 C7 105.5(6) yes . . . O9 S5 C7 107.6(6) yes . . . O10 S6 O11 112.0(6) yes . . . O10 S6 O12 110.9(6) yes . . . O10 S6 C13 106.3(6) yes . . . O11 S6 O12 114.2(6) yes . . . O11 S6 C13 107.2(6) yes . . . O12 S6 C13 105.7(6) yes . . . S4 C1 C2 119.6(8) yes . . . S4 C1 C6 120.2(9) yes . . . C2 C1 C6 120.1(11) yes . . . C1 C2 C3 120.1(10) yes . . . S1 C3 C2 118.7(8) yes . . . S1 C3 C4 120.9(9) yes . . . C2 C3 C4 120.3(10) yes . . . O1 C4 C3 117.9(10) yes . . . O1 C4 C5 123.5(10) yes . . . C3 C4 C5 118.6(11) yes . . . S3 C5 C4 121.2(9) yes 3_666 . . S3 C5 C6 118.2(9) yes 3_666 . . C4 C5 C6 120.2(10) yes . . . C1 C6 C5 120.6(11) yes . . . S5 C7 C8 119.0(9) yes . . . S5 C7 C12 120.5(10) yes . . . C8 C7 C12 120.5(12) yes . . . C7 C8 C9 119.9(10) yes . . . S2 C9 C8 118.4(8) yes . . . S2 C9 C10 120.9(10) yes . . . C8 C9 C10 120.3(11) yes . . . O2 C10 C9 118.1(10) yes . . . O2 C10 C11 123.4(10) yes . . . C9 C10 C11 118.6(11) yes . . . S1 C11 C10 119.6(10) yes . . . S1 C11 C12 119.9(9) yes . . . C10 C11 C12 120.5(10) yes . . . C7 C12 C11 120.1(11) yes . . . S6 C13 C14 120.4(9) yes . . . S6 C13 C18 118.6(9) yes . . . C14 C13 C18 121.1(12) yes . . . C13 C14 C15 119.8(10) yes . . . S3 C15 C14 125.7(8) yes . . . S3 C15 C16 114.4(9) yes . . . C14 C15 C16 119.9(11) yes . . . O3 C16 C15 116.8(10) yes . . . O3 C16 C17 123.9(10) yes . . . C15 C16 C17 119.3(11) yes . . . S2 C17 C16 118.1(9) yes . . . S2 C17 C18 120.6(8) yes . . . C16 C17 C18 121.0(10) yes . . . C13 C18 C17 118.9(11) yes . . . C4 O1 H7 109.480 no . . . C10 O2 H8 109.478 no . . . C16 O3 H9 109.477 no . . . Tm1 O13 H10 129.735 no . . . Tm1 O13 H11 122.772 no . . . H10 O13 H11 105.619 no . . . Tm1 O14 H12 127.303 no . . . Tm1 O14 H13 118.779 no . . . H12 O14 H13 112.151 no . . . Tm1 O15 H14 126.038 no . . . Tm1 O15 H15 116.902 no . . . H14 O15 H15 101.766 no . . . Tm1 O16 H16 122.225 no . . . Tm1 O16 H17 118.120 no . . . H16 O16 H17 119.158 no . . . Tm1 O17 H18 121.104 no . . . Tm1 O17 H19 121.006 no . . . H18 O17 H19 109.759 no . . . Tm1 O18 H20 113.665 no . . . Tm1 O18 H21 124.216 no . . . H20 O18 H21 104.683 no . . . Tm1 O19 H22 111.741 no . . . Tm1 O19 H23 121.805 no . . . H22 O19 H23 110.539 no . . . Tm1 O20 H24 115.907 no . . . Tm1 O20 H25 127.907 no . . . H24 O20 H25 112.260 no . . . H26 O21 H27 113.105 no . . . H28 O22 H29 117.434 no . . . H30 O23 H31 101.898 no . . . H32 O24 H33 116.630 no . . . H34 O25 H35 110.184 no . . . H36 O26 H37 105.844 no . . . H38 O27 H39 98.610 no . . . C1 C2 H1 119.956 no . . . C3 C2 H1 119.968 no . . . C1 C6 H2 119.699 no . . . C5 C6 H2 119.693 no . . . C7 C8 H3 120.040 no . . . C9 C8 H3 120.033 no . . . C7 C12 H4 119.966 no . . . C11 C12 H4 119.967 no . . . C13 C14 H5 120.084 no . . . C15 C14 H5 120.097 no . . . C13 C18 H6 120.542 no . . . C17 C18 H6 120.543 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C3 S1 C11 C10 110.7(8) no . . . . C3 S1 C11 C12 -71.6(8) no . . . . C11 S1 C3 C2 116.4(8) no . . . . C11 S1 C3 C4 -65.4(9) no . . . . C9 S2 C17 C16 100.4(8) no . . . . C9 S2 C17 C18 -84.9(8) no . . . . C17 S2 C9 C8 100.5(8) no . . . . C17 S2 C9 C10 -86.8(9) no . . . . C5 S3 C15 C14 -12.5(10) no 3_666 . . . C5 S3 C15 C16 168.5(7) no 3_666 . . . C15 S3 C5 C4 85.7(9) no . . 3_666 3_666 C15 S3 C5 C6 -101.8(9) no . . 3_666 3_666 O4 S4 C1 C2 162.0(8) no . . . . O4 S4 C1 C6 -18.7(10) no . . . . O5 S4 C1 C2 39.8(9) no . . . . O5 S4 C1 C6 -140.9(8) no . . . . O6 S4 C1 C2 -79.9(9) no . . . . O6 S4 C1 C6 99.4(9) no . . . . O7 S5 C7 C8 -72.0(9) no . . . . O7 S5 C7 C12 106.7(9) no . . . . O8 S5 C7 C8 168.6(8) no . . . . O8 S5 C7 C12 -12.7(10) no . . . . O9 S5 C7 C8 48.4(10) no . . . . O9 S5 C7 C12 -132.9(8) no . . . . O10 S6 C13 C14 -125.2(8) no . . . . O10 S6 C13 C18 56.9(9) no . . . . O11 S6 C13 C14 114.9(8) no . . . . O11 S6 C13 C18 -63.0(9) no . . . . O12 S6 C13 C14 -7.3(10) no . . . . O12 S6 C13 C18 174.8(8) no . . . . S4 C1 C2 C3 -179.0(7) no . . . . S4 C1 C6 C5 178.6(7) no . . . . C2 C1 C6 C5 -2.1(17) no . . . . C6 C1 C2 C3 1.7(17) no . . . . C1 C2 C3 S1 177.9(9) no . . . . C1 C2 C3 C4 -0.3(16) no . . . . S1 C3 C4 O1 -0.1(14) no . . . . S1 C3 C4 C5 -179.0(7) no . . . . C2 C3 C4 O1 178.0(10) no . . . . C2 C3 C4 C5 -0.9(16) no . . . . O1 C4 C5 S3 9.4(16) no . . . 3_666 O1 C4 C5 C6 -178.3(10) no . . . . C3 C4 C5 S3 -171.8(9) no . . . 3_666 C3 C4 C5 C6 0.6(16) no . . . . S3 C5 C6 C1 173.5(7) no 3_666 . . . C4 C5 C6 C1 0.9(17) no . . . . S5 C7 C8 C9 178.8(7) no . . . . S5 C7 C12 C11 -176.1(7) no . . . . C8 C7 C12 C11 2.6(16) no . . . . C12 C7 C8 C9 0.1(16) no . . . . C7 C8 C9 S2 170.7(9) no . . . . C7 C8 C9 C10 -2.1(15) no . . . . S2 C9 C10 O2 8.7(13) no . . . . S2 C9 C10 C11 -171.3(7) no . . . . C8 C9 C10 O2 -178.6(9) no . . . . C8 C9 C10 C11 1.4(15) no . . . . O2 C10 C11 S1 -1.0(15) no . . . . O2 C10 C11 C12 -178.7(9) no . . . . C9 C10 C11 S1 178.9(8) no . . . . C9 C10 C11 C12 1.3(15) no . . . . S1 C11 C12 C7 179.1(7) no . . . . C10 C11 C12 C7 -3.3(15) no . . . . S6 C13 C14 C15 -178.7(7) no . . . . S6 C13 C18 C17 179.8(7) no . . . . C14 C13 C18 C17 1.9(16) no . . . . C18 C13 C14 C15 -0.8(16) no . . . . C13 C14 C15 S3 -178.7(9) no . . . . C13 C14 C15 C16 0.2(15) no . . . . S3 C15 C16 O3 -2.0(12) no . . . . S3 C15 C16 C17 178.3(7) no . . . . C14 C15 C16 O3 178.9(9) no . . . . C14 C15 C16 C17 -0.8(15) no . . . . O3 C16 C17 S2 -3.1(15) no . . . . O3 C16 C17 C18 -177.8(9) no . . . . C15 C16 C17 S2 176.6(8) no . . . . C15 C16 C17 C18 1.9(15) no . . . . S2 C17 C18 C13 -177.0(7) no . . . . C16 C17 C18 C13 -2.5(16) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 O1 2.972(8) no . . S1 O2 3.062(9) no . . S2 O2 2.987(8) no . . S2 O3 3.032(9) no . . S3 O1 3.098(9) no . 3_666 S3 O3 2.792(8) no . . O1 O2 3.064(12) no . . O1 C10 3.187(12) no . . O1 C11 3.127(12) no . . O1 C14 3.585(12) no . 3_666 O2 O3 2.944(12) no . . O2 C16 3.478(13) no . . O2 C17 3.536(14) no . . O4 C6 2.905(15) no . . O5 C2 3.017(14) no . . O6 C2 3.313(17) no . . O6 C6 3.486(15) no . . O7 C8 3.250(18) no . . O7 C12 3.563(17) no . . O8 C12 2.885(17) no . . O9 C8 3.073(15) no . . O10 C18 3.128(17) no . . O11 C18 3.188(15) no . . O12 C14 2.887(16) no . . C1 C4 2.802(17) no . . C2 C5 2.784(15) no . . C3 C6 2.779(16) no . . C3 C12 3.322(14) no . . C4 C11 3.288(14) no . . C4 C14 3.552(14) no . 3_666 C4 C15 3.585(14) no . 3_666 C5 C14 3.118(16) no . 3_666 C7 C10 2.798(18) no . . C8 C11 2.790(15) no . . C9 C12 2.791(16) no . . C9 C18 3.536(15) no . . C10 C17 3.570(15) no . . C13 C16 2.791(18) no . . C14 C17 2.794(15) no . . C15 C18 2.810(16) no . . S1 S2 3.342(4) no . 2_545 S1 O5 3.416(11) no . 3_656 S1 C1 3.280(13) no . 3_656 S1 C2 3.281(11) no . 3_656 S2 S1 3.342(4) no . 2_555 S2 C14 3.429(11) no . 2_545 S3 O22 3.318(11) no . 3_666 S3 O25 3.498(11) no . 3_666 S3 O26 3.353(11) no . 3_666 S4 O18 3.562(12) no . . O1 O5 3.471(15) no . 3_656 O1 O25 3.427(18) no . 3_666 O1 O26 2.685(14) no . . O1 O27 3.483(19) no . . O2 O5 2.828(12) no . 3_656 O2 O11 3.286(14) no . 2_545 O2 C18 3.468(13) no . 2_545 O3 O11 3.237(13) no . 2_545 O3 O22 3.134(14) no . 3_666 O3 O25 3.307(13) no . 3_666 O3 C7 3.597(15) no . 2_555 O3 C12 3.574(13) no . 2_555 O4 O15 2.711(15) no . 2_546 O4 O17 3.570(14) no . 2_546 O4 O18 3.454(14) no . . O4 C18 3.508(14) no . 4_555 O5 S1 3.416(11) no . 3_656 O5 O1 3.471(15) no . 3_656 O5 O2 2.828(12) no . 3_656 O5 O24 3.378(14) no . 1_545 O5 O25 2.801(14) no . 1_545 O6 O15 3.595(13) no . 2_546 O6 O16 2.781(16) no . 2_546 O6 O18 2.986(14) no . . O6 O19 3.326(14) no . . O6 O21 3.279(12) no . . O6 O24 2.993(13) no . 1_545 O7 O13 2.793(15) no . . O7 O23 2.814(13) no . 3_566 O7 O28A 3.03(3) no . . O7 O28B 3.09(5) no . . O8 O11 3.515(14) no . 1_545 O8 O19 2.688(16) no . 3_556 O8 O21 2.731(12) no . . O9 O16 2.773(13) no . 4_454 O9 O18 3.488(13) no . 4_454 O9 O22 2.874(13) no . 4_454 O9 O23 3.352(15) no . 3_566 O10 O13 2.866(15) no . 3_566 O10 O15 3.408(12) no . 3_566 O10 O24 2.867(13) no . . O10 O28A 2.82(3) no . . O10 O28B 2.81(5) no . . O11 O2 3.286(14) no . 2_555 O11 O3 3.237(13) no . 2_555 O11 O8 3.515(14) no . 1_565 O11 O17 2.714(13) no . 3_566 O12 O21 2.742(16) no . 1_565 O12 O24 3.329(15) no . . O12 C2 3.270(13) no . 1_565 O13 O7 2.793(15) no . . O13 O10 2.866(15) no . 3_566 O14 O22 2.738(13) no . . O14 O23 3.373(15) no . . O14 O27 2.678(18) no . . O15 O4 2.711(15) no . 2_556 O15 O6 3.595(13) no . 2_556 O15 O10 3.408(12) no . 3_566 O15 O23 2.793(14) no . . O15 O28A 3.20(3) no . 3_566 O15 O28B 3.20(5) no . 3_566 O16 O6 2.781(16) no . 2_556 O16 O9 2.773(13) no . 4_555 O16 O22 3.472(15) no . . O16 O23 3.326(13) no . 2_546 O17 O4 3.570(14) no . 2_556 O17 O11 2.714(13) no . 3_566 O17 O22 2.711(13) no . 2_546 O18 S4 3.562(12) no . . O18 O4 3.454(14) no . . O18 O6 2.986(14) no . . O18 O9 3.488(13) no . 4_555 O18 O23 2.775(14) no . 2_546 O18 C6 3.361(18) no . . O19 O6 3.326(14) no . . O19 O8 2.688(16) no . 3_556 O19 O21 2.687(17) no . . O20 O21 2.741(13) no . . O20 O27 2.698(16) no . . O20 C1 3.580(14) no . . O20 C5 3.561(15) no . . O20 C6 3.475(14) no . . O21 O6 3.279(12) no . . O21 O8 2.731(12) no . . O21 O12 2.742(16) no . 1_545 O21 O19 2.687(17) no . . O21 O20 2.741(13) no . . O21 C2 3.585(16) no . . O21 C12 3.492(17) no . . O22 S3 3.318(11) no . 3_666 O22 O3 3.134(14) no . 3_666 O22 O9 2.874(13) no . 4_555 O22 O14 2.738(13) no . . O22 O16 3.472(15) no . . O22 O17 2.711(13) no . 2_556 O22 O25 2.795(17) no . . O23 O7 2.814(13) no . 3_566 O23 O9 3.352(15) no . 3_566 O23 O14 3.373(15) no . . O23 O15 2.793(14) no . . O23 O16 3.326(13) no . 2_556 O23 O18 2.775(14) no . 2_556 O23 O24 2.800(18) no . . O23 O28A 3.42(3) no . 3_566 O23 O28B 3.37(5) no . 3_566 O24 O5 3.378(14) no . 1_565 O24 O6 2.993(13) no . 1_565 O24 O10 2.867(13) no . . O24 O12 3.329(15) no . . O24 O23 2.800(18) no . . O24 O25 2.797(18) no . . O25 S3 3.498(11) no . 3_666 O25 O1 3.427(18) no . 3_666 O25 O3 3.307(13) no . 3_666 O25 O5 2.801(14) no . 1_565 O25 O22 2.795(17) no . . O25 O24 2.797(18) no . . O25 O26 2.674(17) no . . O26 S3 3.353(11) no . 3_666 O26 O1 2.685(14) no . . O26 O25 2.674(17) no . . O26 O26 3.265(19) no . 3_666 O26 O27 2.74(2) no . . O26 C4 3.600(15) no . . O26 C14 3.467(15) no . . O26 C15 3.338(17) no . . O26 C16 3.438(16) no . . O27 O1 3.483(19) no . . O27 O14 2.678(18) no . . O27 O20 2.698(16) no . . O27 O26 2.74(2) no . . O27 O28A 2.60(3) no . . O27 O28B 2.73(5) no . . O27 C4 3.581(18) no . . O27 C7 3.591(15) no . . O28A O7 3.03(3) no . . O28A O10 2.82(3) no . . O28A O15 3.20(3) no . 3_566 O28A O23 3.42(3) no . 3_566 O28A O27 2.60(3) no . . O28A C8 3.34(3) no . . O28A C18 3.38(4) no . . O28B O7 3.09(5) no . . O28B O10 2.81(5) no . . O28B O15 3.20(5) no . 3_566 O28B O23 3.37(5) no . 3_566 O28B O27 2.73(5) no . . C1 S1 3.280(13) no . 3_656 C1 O20 3.580(14) no . . C2 S1 3.281(11) no . 3_656 C2 O12 3.270(13) no . 1_545 C2 O21 3.585(16) no . . C2 C3 3.440(18) no . 3_656 C3 C2 3.440(18) no . 3_656 C3 C3 3.520(16) no . 3_656 C4 O26 3.600(15) no . . C4 O27 3.581(18) no . . C5 O20 3.561(15) no . . C6 O18 3.361(18) no . . C6 O20 3.475(14) no . . C7 O3 3.597(15) no . 2_545 C7 O27 3.591(15) no . . C8 O28A 3.34(3) no . . C10 C17 3.586(15) no . 2_545 C10 C18 3.581(17) no . 2_545 C11 C17 3.531(16) no . 2_545 C12 O3 3.574(13) no . 2_545 C12 O21 3.492(17) no . . C14 S2 3.429(11) no . 2_555 C14 O26 3.467(15) no . . C15 O26 3.338(17) no . . C16 O26 3.438(16) no . . C17 C10 3.586(15) no . 2_555 C17 C11 3.531(16) no . 2_555 C18 O2 3.468(13) no . 2_555 C18 O4 3.508(14) no . 4_454 C18 O28A 3.38(4) no . . C18 C10 3.581(17) no . 2_555 S1 H1 2.8278 no . . S1 H4 2.8392 no . . S1 H8 2.5362 no . . S2 H3 2.8207 no . . S2 H6 2.8804 no . . S2 H9 2.5089 no . . S3 H2 2.8016 no . 3_666 S3 H5 2.9685 no . . S3 H7 2.6409 no . 3_666 S4 H1 2.8287 no . . S4 H2 2.8313 no . . S5 H3 2.8181 no . . S5 H4 2.8458 no . . S6 H5 2.8601 no . . S6 H6 2.8307 no . . O1 H5 3.0707 no . 3_666 O1 H8 2.7852 no . . O2 H7 3.4618 no . . O2 H9 2.4042 no . . O3 H8 3.4698 no . . O4 H2 2.5294 no . . O5 H1 2.7364 no . . O6 H1 3.2651 no . . O6 H2 3.5538 no . . O7 H3 3.1617 no . . O8 H4 2.4925 no . . O9 H3 2.8262 no . . O10 H6 2.9384 no . . O11 H6 3.0404 no . . O12 H5 2.4954 no . . O13 H13 3.4027 no . . O13 H14 3.2779 no . . O13 H15 3.1334 no . . O13 H18 3.2161 no . . O13 H22 2.9976 no . . O13 H23 3.2373 no . . O13 H24 3.1614 no . . O13 H25 3.2175 no . . O14 H14 3.4839 no . . O14 H15 2.5906 no . . O14 H16 2.9671 no . . O14 H17 3.1665 no . . O14 H24 3.5140 no . . O14 H25 2.6758 no . . O15 H10 3.4643 no . . O15 H11 2.5335 no . . O15 H12 3.0753 no . . O15 H13 3.3611 no . . O15 H16 3.5549 no . . O15 H17 2.7144 no . . O15 H18 2.7979 no . . O15 H19 3.4708 no . . O16 H12 2.7239 no . . O16 H13 3.5927 no . . O16 H14 2.9763 no . . O16 H15 2.9673 no . . O16 H19 3.2542 no . . O16 H20 3.4723 no . . O16 H21 2.5864 no . . O17 H11 3.4416 no . . O17 H14 2.6668 no . . O17 H15 3.4486 no . . O17 H17 2.9582 no . . O17 H21 3.4295 no . . O17 H22 2.6027 no . . O18 H16 2.6298 no . . O18 H17 3.1381 no . . O18 H19 3.2918 no . . O18 H22 3.3838 no . . O18 H23 3.0862 no . . O18 H24 3.1604 no . . O19 H10 3.2736 no . . O19 H18 3.1190 no . . O19 H19 2.8336 no . . O19 H20 2.4058 no . . O19 H21 3.1792 no . . O19 H24 2.4712 no . . O20 H10 2.8585 no . . O20 H12 3.3736 no . . O20 H13 2.5398 no . . O20 H20 2.9965 no . . O20 H22 3.4569 no . . O20 H23 2.5604 no . . C2 H2 3.2529 no . . C2 H4 3.5252 no . . C3 H4 3.2204 no . . C3 H7 3.0284 no . . C4 H1 3.2885 no . . C4 H2 3.2803 no . . C4 H5 2.9109 no . 3_666 C5 H5 2.7011 no . 3_666 C5 H7 2.4686 no . . C6 H1 3.2535 no . . C6 H5 3.4858 no . 3_666 C8 H4 3.2714 no . . C9 H6 3.5130 no . . C9 H8 3.0650 no . . C9 H9 3.3587 no . . C10 H3 3.2876 no . . C10 H4 3.2853 no . . C10 H7 3.5598 no . . C10 H9 3.3062 no . . C11 H8 2.4330 no . . C12 H3 3.2713 no . . C14 H6 3.2915 no . . C14 H7 3.4957 no . 3_666 C15 H7 3.2804 no . 3_666 C15 H9 3.0642 no . . C16 H5 3.2908 no . . C16 H6 3.2873 no . . C17 H9 2.4408 no . . C18 H5 3.2894 no . . H1 H4 3.4169 no . . H3 H6 3.1662 no . . H5 H7 3.1943 no . 3_666 H7 H8 3.3412 no . . H8 H9 3.0038 no . . H10 H13 3.5634 no . . H10 H22 3.3246 no . . H10 H23 3.3113 no . . H10 H24 3.0113 no . . H10 H25 3.0127 no . . H11 H14 3.0090 no . . H11 H15 2.9606 no . . H11 H18 3.1848 no . . H11 H22 3.5234 no . . H12 H15 2.7229 no . . H12 H16 2.7265 no . . H12 H17 3.0248 no . . H12 H25 3.3067 no . . H13 H15 3.1214 no . . H13 H24 3.3367 no . . H13 H25 2.2459 no . . H14 H17 2.7059 no . . H14 H18 2.6461 no . . H14 H19 3.3624 no . . H15 H16 3.5808 no . . H15 H17 2.8309 no . . H15 H18 3.5481 no . . H16 H20 3.4815 no . . H16 H21 2.5140 no . . H17 H18 3.5724 no . . H17 H19 3.2242 no . . H17 H21 3.0269 no . . H18 H22 2.7380 no . . H19 H20 3.5518 no . . H19 H21 3.2326 no . . H19 H22 2.6199 no . . H20 H22 3.1272 no . . H20 H23 2.6285 no . . H20 H24 2.9366 no . . H22 H24 3.1787 no . . H23 H24 2.0517 no . . H23 H25 3.3610 no . . S1 H1 3.5075 no . 3_656 S2 H5 3.3558 no . 2_545 S3 H12 3.5546 no . 3_666 S3 H13 3.5996 no . 3_666 S3 H28 3.0721 no . 3_666 S3 H29 3.1138 no . 3_666 S3 H36 3.2971 no . 3_666 S3 H37 3.4884 no . . S4 H8 3.1519 no . 3_656 S4 H14 2.9581 no . 2_546 S4 H17 3.2808 no . 2_546 S4 H20 2.9130 no . . S4 H33 2.9624 no . 1_545 S4 H35 3.5702 no . 1_545 S5 H10 3.1785 no . . S5 H16 3.1236 no . 4_454 S5 H22 2.9972 no . 3_556 S5 H27 3.1579 no . . S5 H29 3.0373 no . 4_454 S5 H31 2.7881 no . 3_566 S6 H11 3.2855 no . 3_566 S6 H18 3.0546 no . 3_566 S6 H26 2.9580 no . 1_565 S6 H27 3.5895 no . 1_565 S6 H32 2.8785 no . . O1 H35 2.9524 no . 3_666 O1 H36 3.3384 no . . O1 H36 3.5110 no . 3_666 O1 H37 3.0424 no . . O1 H39 3.1632 no . . O2 H6 3.4849 no . 2_545 O2 H35 2.9213 no . 3_666 O3 H28 2.6978 no . 3_666 O3 H29 2.9275 no . 3_666 O3 H35 3.0147 no . 3_666 O3 H37 3.3922 no . . O4 H3 3.2364 no . 4_555 O4 H6 2.6058 no . 4_555 O4 H8 3.3915 no . 3_656 O4 H14 1.9534 no . 2_546 O4 H15 2.8852 no . 2_546 O4 H17 3.4849 no . 2_546 O4 H18 3.4211 no . 2_546 O4 H20 3.0352 no . . O4 H21 3.3871 no . . O5 H8 2.1051 no . 3_656 O5 H33 2.7456 no . 1_545 O5 H34 2.7007 no . 1_545 O5 H35 2.1881 no . 1_545 O6 H14 3.0996 no . 2_546 O6 H16 3.1951 no . 2_546 O6 H17 2.2075 no . 2_546 O6 H20 2.1576 no . . O6 H21 3.2425 no . . O6 H23 3.0268 no . . O6 H24 3.4978 no . . O6 H26 3.1069 no . . O6 H32 3.5032 no . 1_545 O6 H33 2.1994 no . 1_545 O7 H10 1.9569 no . . O7 H11 3.0914 no . . O7 H16 3.5158 no . 4_454 O7 H25 3.4013 no . . O7 H27 3.5321 no . . O7 H30 3.1102 no . 3_566 O7 H31 1.9185 no . 3_566 O7 H38 3.2263 no . . O8 H10 3.4420 no . . O8 H18 3.4376 no . 3_556 O8 H19 3.4864 no . 3_556 O8 H22 1.9033 no . 3_556 O8 H23 2.9335 no . 3_556 O8 H24 3.5714 no . . O8 H26 3.1193 no . . O8 H27 1.9853 no . . O8 H29 3.0882 no . 4_454 O9 H2 3.3302 no . 4_454 O9 H12 3.5000 no . 4_454 O9 H16 1.9641 no . 4_454 O9 H17 3.1107 no . 4_454 O9 H21 3.3132 no . 4_454 O9 H22 3.2717 no . 3_556 O9 H28 3.4250 no . 4_454 O9 H29 2.0936 no . 4_454 O9 H31 2.7146 no . 3_566 O10 H10 3.2777 no . 3_566 O10 H11 2.1050 no . 3_566 O10 H14 3.4226 no . 3_566 O10 H18 3.2307 no . 3_566 O10 H26 3.2494 no . 1_565 O10 H32 2.0381 no . . O10 H33 3.3444 no . . O11 H4 3.3854 no . 1_565 O11 H8 3.5918 no . 2_555 O11 H9 2.5634 no . 2_555 O11 H11 3.5630 no . 3_566 O11 H18 1.9168 no . 3_566 O11 H19 2.9916 no . 3_566 O11 H26 3.5445 no . 1_565 O12 H1 2.4831 no . 1_565 O12 H4 2.7785 no . 1_565 O12 H26 1.9674 no . 1_565 O12 H27 2.9652 no . 1_565 O12 H32 2.7658 no . . O12 H33 3.2268 no . . O14 H28 3.0563 no . . O14 H29 3.0079 no . . O14 H30 3.1670 no . . O14 H38 2.9068 no . . O14 H39 3.1067 no . . O15 H21 3.4333 no . 2_556 O15 H30 3.3514 no . . O15 H31 3.3452 no . . O16 H20 3.3654 no . 2_556 O16 H29 3.2061 no . . O16 H30 3.3220 no . 2_546 O16 H31 3.2976 no . 2_546 O16 H33 3.3435 no . 2_546 O17 H28 2.8357 no . 2_546 O17 H29 2.9436 no . 2_546 O18 H2 2.9591 no . . O18 H15 3.4321 no . 2_546 O18 H17 3.5957 no . 2_546 O18 H30 3.2811 no . 2_546 O18 H31 3.1636 no . 2_546 O19 H26 3.3315 no . . O19 H27 2.9796 no . . O19 H27 3.5106 no . 3_556 O19 H29 3.4945 no . 2_546 O20 H4 3.5557 no . . O20 H26 3.2988 no . . O20 H27 3.0789 no . . O20 H38 3.0715 no . . O20 H39 3.4332 no . . O21 H1 3.3949 no . . O21 H4 2.6774 no . . O21 H22 3.1347 no . . O21 H23 1.8420 no . . O21 H24 1.9472 no . . O21 H25 3.1931 no . . O21 H32 3.5358 no . 1_545 O21 H33 3.3870 no . 1_545 O22 H9 3.5244 no . 3_666 O22 H12 1.9953 no . . O22 H13 3.0623 no . . O22 H16 3.0853 no . . O22 H18 3.0485 no . 2_556 O22 H19 1.9416 no . 2_556 O22 H22 3.4834 no . 2_556 O22 H30 3.4146 no . . O22 H34 2.8637 no . . O22 H35 3.0622 no . . O23 H12 3.1681 no . . O23 H14 2.9752 no . . O23 H15 2.0471 no . . O23 H16 3.0585 no . 2_556 O23 H17 3.5392 no . 2_556 O23 H20 3.1503 no . 2_556 O23 H21 2.0395 no . 2_556 O23 H32 3.2152 no . . O23 H33 3.2642 no . . O24 H11 3.5547 no . 3_566 O24 H17 3.4502 no . 2_556 O24 H26 3.2095 no . 1_565 O24 H28 3.3805 no . . O24 H30 1.9145 no . . O24 H31 2.9760 no . . O24 H34 1.9678 no . . O24 H35 3.1692 no . . O25 H7 3.4473 no . 3_666 O25 H8 3.4730 no . 3_666 O25 H12 3.4846 no . . O25 H28 2.0508 no . . O25 H29 3.3901 no . . O25 H32 3.0577 no . . O25 H33 2.8809 no . . O25 H36 1.8835 no . . O25 H37 3.0959 no . . O25 H39 3.3846 no . . O26 H7 1.9283 no . . O26 H7 3.4390 no . 3_666 O26 H34 3.0636 no . . O26 H35 3.2120 no . . O26 H36 3.2655 no . 3_666 O26 H37 3.2615 no . 3_666 O26 H38 3.1191 no . . O26 H39 1.9510 no . . O27 H7 3.1113 no . . O27 H12 3.1123 no . . O27 H13 1.9035 no . . O27 H24 3.2748 no . . O27 H25 1.8744 no . . O27 H36 2.9706 no . . O27 H37 3.2133 no . . O28A H3 3.0276 no . . O28A H6 2.8673 no . . O28A H11 3.3646 no . 3_566 O28A H13 3.5325 no . . O28A H14 3.1339 no . 3_566 O28A H15 3.1331 no . 3_566 O28A H31 3.0797 no . 3_566 O28A H38 1.8352 no . . O28A H39 2.7648 no . . O28B H6 3.5217 no . . O28B H10 3.3446 no . . O28B H11 2.9812 no . 3_566 O28B H13 3.2074 no . . O28B H14 3.3141 no . 3_566 O28B H15 3.0977 no . 3_566 O28B H31 3.0736 no . 3_566 O28B H32 3.4776 no . . O28B H38 1.9840 no . . O28B H39 2.9929 no . . C1 H20 3.2167 no . . C1 H24 3.3658 no . . C2 H24 3.3709 no . . C2 H26 3.1852 no . . C3 H1 3.4080 no . 3_656 C3 H25 3.5014 no . . C4 H1 3.5500 no . 3_656 C4 H25 3.2964 no . . C4 H39 3.5422 no . . C5 H25 3.3447 no . . C6 H3 3.1724 no . 4_555 C6 H20 3.2693 no . . C6 H24 3.5755 no . . C7 H25 3.5329 no . . C7 H38 3.4461 no . . C8 H2 3.1114 no . 4_454 C8 H38 3.3946 no . . C12 H9 3.5361 no . 2_545 C12 H24 3.4854 no . . C12 H25 3.2867 no . . C12 H26 3.5201 no . . C12 H27 3.3430 no . . C13 H37 3.1273 no . . C14 H36 3.3728 no . . C14 H37 2.8223 no . . C15 H36 3.5014 no . . C15 H37 2.5736 no . . C16 H37 2.6764 no . . C17 H37 2.9900 no . . C18 H8 3.5390 no . 2_555 C18 H37 3.2325 no . . H1 S1 3.5075 no . 3_656 H1 O12 2.4831 no . 1_545 H1 O21 3.3949 no . . H1 C3 3.4080 no . 3_656 H1 C4 3.5500 no . 3_656 H1 H5 3.0195 no . 1_545 H1 H26 2.8084 no . . H1 H33 3.4818 no . 1_545 H2 O9 3.3302 no . 4_555 H2 O18 2.9591 no . . H2 C8 3.1114 no . 4_555 H2 H3 2.3363 no . 4_555 H2 H20 3.0031 no . . H2 H21 3.1969 no . . H3 O4 3.2364 no . 4_454 H3 O28A 3.0276 no . . H3 C6 3.1724 no . 4_454 H3 H2 2.3363 no . 4_454 H3 H31 3.4744 no . 3_566 H3 H38 3.5944 no . . H4 O11 3.3854 no . 1_545 H4 O12 2.7785 no . 1_545 H4 O20 3.5557 no . . H4 O21 2.6774 no . . H4 H9 3.4790 no . 2_545 H4 H24 3.0751 no . . H4 H25 3.2718 no . . H4 H26 2.6162 no . . H4 H27 2.5634 no . . H5 S2 3.3558 no . 2_555 H5 H1 3.0195 no . 1_565 H5 H37 3.3454 no . . H6 O2 3.4849 no . 2_555 H6 O4 2.6058 no . 4_454 H6 O28A 2.8673 no . . H6 O28B 3.5217 no . . H6 H8 3.3706 no . 2_555 H6 H14 3.2704 no . 3_566 H7 O25 3.4473 no . 3_666 H7 O26 1.9283 no . . H7 O26 3.4390 no . 3_666 H7 O27 3.1113 no . . H7 H35 3.1080 no . 3_666 H7 H36 2.5253 no . . H7 H36 3.1337 no . 3_666 H7 H37 2.3880 no . . H7 H37 3.2300 no . 3_666 H7 H39 2.6622 no . . H8 S4 3.1519 no . 3_656 H8 O4 3.3915 no . 3_656 H8 O5 2.1051 no . 3_656 H8 O11 3.5918 no . 2_545 H8 O25 3.4730 no . 3_666 H8 C18 3.5390 no . 2_545 H8 H6 3.3706 no . 2_545 H8 H35 2.6551 no . 3_666 H9 O11 2.5634 no . 2_545 H9 O22 3.5244 no . 3_666 H9 C12 3.5361 no . 2_555 H9 H4 3.4790 no . 2_555 H9 H18 3.3710 no . 4_554 H9 H19 3.5998 no . 4_554 H9 H28 3.0895 no . 3_666 H9 H29 3.3561 no . 3_666 H9 H35 3.1903 no . 3_666 H10 S5 3.1785 no . . H10 O7 1.9569 no . . H10 O8 3.4420 no . . H10 O10 3.2777 no . 3_566 H10 O28B 3.3446 no . . H10 H27 3.5220 no . . H10 H31 3.0798 no . 3_566 H10 H32 3.5418 no . 3_566 H10 H38 3.4494 no . . H11 S6 3.2855 no . 3_566 H11 O7 3.0914 no . . H11 O10 2.1050 no . 3_566 H11 O11 3.5630 no . 3_566 H11 O24 3.5547 no . 3_566 H11 O28A 3.3646 no . 3_566 H11 O28B 2.9812 no . 3_566 H11 H31 3.5753 no . 3_566 H11 H32 2.9632 no . 3_566 H12 S3 3.5546 no . 3_666 H12 O9 3.5000 no . 4_555 H12 O22 1.9953 no . . H12 O23 3.1681 no . . H12 O25 3.4846 no . . H12 O27 3.1123 no . . H12 H28 2.3651 no . . H12 H29 2.3179 no . . H12 H30 2.9031 no . . H12 H34 3.3522 no . . H12 H38 3.3749 no . . H12 H39 3.3793 no . . H13 S3 3.5996 no . 3_666 H13 O22 3.0623 no . . H13 O27 1.9035 no . . H13 O28A 3.5325 no . . H13 O28B 3.2074 no . . H13 H28 3.1899 no . . H13 H29 3.4048 no . . H13 H30 3.3404 no . . H13 H34 3.5112 no . . H13 H38 2.1542 no . . H13 H39 2.3319 no . . H14 S4 2.9581 no . 2_556 H14 O4 1.9534 no . 2_556 H14 O6 3.0996 no . 2_556 H14 O10 3.4226 no . 3_566 H14 O23 2.9752 no . . H14 O28A 3.1339 no . 3_566 H14 O28B 3.3141 no . 3_566 H14 H6 3.2704 no . 3_566 H14 H20 3.3334 no . 2_556 H14 H21 3.2786 no . 2_556 H14 H31 3.4378 no . . H15 O4 2.8852 no . 2_556 H15 O18 3.4321 no . 2_556 H15 O23 2.0471 no . . H15 O28A 3.1331 no . 3_566 H15 O28B 3.0977 no . 3_566 H15 H20 3.2725 no . 2_556 H15 H21 2.8500 no . 2_556 H15 H30 2.6024 no . . H15 H31 2.6601 no . . H16 S5 3.1236 no . 4_555 H16 O6 3.1951 no . 2_556 H16 O7 3.5158 no . 4_555 H16 O9 1.9641 no . 4_555 H16 O22 3.0853 no . . H16 O23 3.0585 no . 2_546 H16 H20 3.5894 no . 2_556 H16 H29 2.6622 no . . H16 H30 3.2006 no . 2_546 H16 H31 2.8462 no . 2_546 H16 H33 3.5547 no . 2_546 H17 S4 3.2808 no . 2_556 H17 O4 3.4849 no . 2_556 H17 O6 2.2075 no . 2_556 H17 O9 3.1107 no . 4_555 H17 O18 3.5957 no . 2_556 H17 O23 3.5392 no . 2_546 H17 O24 3.4502 no . 2_546 H17 H20 2.9112 no . 2_556 H17 H21 3.4772 no . 2_556 H17 H29 3.4548 no . . H17 H30 3.3885 no . 2_546 H17 H31 3.5052 no . 2_546 H17 H33 2.9903 no . 2_546 H18 S6 3.0546 no . 3_566 H18 O4 3.4211 no . 2_556 H18 O8 3.4376 no . 3_556 H18 O10 3.2307 no . 3_566 H18 O11 1.9168 no . 3_566 H18 O22 3.0485 no . 2_546 H18 H9 3.3710 no . 4_455 H18 H28 3.0670 no . 2_546 H18 H29 3.1584 no . 2_546 H19 O8 3.4864 no . 3_556 H19 O11 2.9916 no . 3_566 H19 O22 1.9416 no . 2_546 H19 H9 3.5998 no . 4_455 H19 H28 2.1107 no . 2_546 H19 H29 2.2235 no . 2_546 H19 H34 3.5477 no . 2_546 H19 H35 3.5076 no . 2_546 H20 S4 2.9130 no . . H20 O4 3.0352 no . . H20 O6 2.1576 no . . H20 O16 3.3654 no . 2_546 H20 O23 3.1503 no . 2_546 H20 C1 3.2167 no . . H20 C6 3.2693 no . . H20 H2 3.0031 no . . H20 H14 3.3334 no . 2_546 H20 H15 3.2725 no . 2_546 H20 H16 3.5894 no . 2_546 H20 H17 2.9112 no . 2_546 H21 O4 3.3871 no . . H21 O6 3.2425 no . . H21 O9 3.3132 no . 4_555 H21 O15 3.4333 no . 2_546 H21 O23 2.0395 no . 2_546 H21 H2 3.1969 no . . H21 H14 3.2786 no . 2_546 H21 H15 2.8500 no . 2_546 H21 H17 3.4772 no . 2_546 H21 H30 2.5570 no . 2_546 H21 H31 2.4959 no . 2_546 H22 S5 2.9972 no . 3_556 H22 O8 1.9033 no . 3_556 H22 O9 3.2717 no . 3_556 H22 O21 3.1347 no . . H22 O22 3.4834 no . 2_546 H22 H27 3.2590 no . . H22 H27 2.8262 no . 3_556 H22 H29 3.1390 no . 2_546 H23 O6 3.0268 no . . H23 O8 2.9335 no . 3_556 H23 O21 1.8420 no . . H23 H26 2.4846 no . . H23 H27 2.1795 no . . H23 H27 3.5323 no . 3_556 H24 O6 3.4978 no . . H24 O8 3.5714 no . . H24 O21 1.9472 no . . H24 O27 3.2748 no . . H24 C1 3.3658 no . . H24 C2 3.3709 no . . H24 C6 3.5755 no . . H24 C12 3.4854 no . . H24 H4 3.0751 no . . H24 H26 2.4996 no . . H24 H27 2.3492 no . . H25 O7 3.4013 no . . H25 O21 3.1931 no . . H25 O27 1.8744 no . . H25 C3 3.5014 no . . H25 C4 3.2964 no . . H25 C5 3.3447 no . . H25 C7 3.5329 no . . H25 C12 3.2867 no . . H25 H4 3.2718 no . . H25 H27 3.4303 no . . H25 H38 2.3011 no . . H25 H39 2.6005 no . . H26 S6 2.9580 no . 1_545 H26 O6 3.1069 no . . H26 O8 3.1193 no . . H26 O10 3.2494 no . 1_545 H26 O11 3.5445 no . 1_545 H26 O12 1.9674 no . 1_545 H26 O19 3.3315 no . . H26 O20 3.2988 no . . H26 O24 3.2095 no . 1_545 H26 C2 3.1852 no . . H26 C12 3.5201 no . . H26 H1 2.8084 no . . H26 H4 2.6162 no . . H26 H23 2.4846 no . . H26 H24 2.4996 no . . H26 H32 2.9234 no . 1_545 H26 H33 2.8645 no . 1_545 H27 S5 3.1579 no . . H27 S6 3.5895 no . 1_545 H27 O7 3.5321 no . . H27 O8 1.9853 no . . H27 O12 2.9652 no . 1_545 H27 O19 2.9796 no . . H27 O19 3.5106 no . 3_556 H27 O20 3.0789 no . . H27 C12 3.3430 no . . H27 H4 2.5634 no . . H27 H10 3.5220 no . . H27 H22 3.2590 no . . H27 H22 2.8262 no . 3_556 H27 H23 2.1795 no . . H27 H23 3.5323 no . 3_556 H27 H24 2.3492 no . . H27 H25 3.4303 no . . H28 S3 3.0721 no . 3_666 H28 O3 2.6978 no . 3_666 H28 O9 3.4250 no . 4_555 H28 O14 3.0563 no . . H28 O17 2.8357 no . 2_556 H28 O24 3.3805 no . . H28 O25 2.0508 no . . H28 H9 3.0895 no . 3_666 H28 H12 2.3651 no . . H28 H13 3.1899 no . . H28 H18 3.0670 no . 2_556 H28 H19 2.1107 no . 2_556 H28 H30 3.5681 no . . H28 H33 3.5105 no . . H28 H34 2.2355 no . . H28 H35 2.2771 no . . H28 H36 3.4675 no . . H29 S3 3.1138 no . 3_666 H29 S5 3.0373 no . 4_555 H29 O3 2.9275 no . 3_666 H29 O8 3.0882 no . 4_555 H29 O9 2.0936 no . 4_555 H29 O14 3.0079 no . . H29 O16 3.2061 no . . H29 O17 2.9436 no . 2_556 H29 O19 3.4945 no . 2_556 H29 O25 3.3901 no . . H29 H9 3.3561 no . 3_666 H29 H12 2.3179 no . . H29 H13 3.4048 no . . H29 H16 2.6622 no . . H29 H17 3.4548 no . . H29 H18 3.1584 no . 2_556 H29 H19 2.2235 no . 2_556 H29 H22 3.1390 no . 2_556 H29 H34 3.5828 no . . H30 O7 3.1102 no . 3_566 H30 O14 3.1670 no . . H30 O15 3.3514 no . . H30 O16 3.3220 no . 2_556 H30 O18 3.2811 no . 2_556 H30 O22 3.4146 no . . H30 O24 1.9145 no . . H30 H12 2.9031 no . . H30 H13 3.3404 no . . H30 H15 2.6024 no . . H30 H16 3.2006 no . 2_556 H30 H17 3.3885 no . 2_556 H30 H21 2.5570 no . 2_556 H30 H28 3.5681 no . . H30 H32 2.3547 no . . H30 H33 2.4468 no . . H30 H34 3.2718 no . . H31 S5 2.7881 no . 3_566 H31 O7 1.9185 no . 3_566 H31 O9 2.7146 no . 3_566 H31 O15 3.3452 no . . H31 O16 3.2976 no . 2_556 H31 O18 3.1636 no . 2_556 H31 O24 2.9760 no . . H31 O28A 3.0797 no . 3_566 H31 O28B 3.0736 no . 3_566 H31 H3 3.4744 no . 3_566 H31 H10 3.0798 no . 3_566 H31 H11 3.5753 no . 3_566 H31 H14 3.4378 no . . H31 H15 2.6601 no . . H31 H16 2.8462 no . 2_556 H31 H17 3.5052 no . 2_556 H31 H21 2.4959 no . 2_556 H31 H32 3.2843 no . . H31 H33 3.3734 no . . H32 S6 2.8785 no . . H32 O6 3.5032 no . 1_565 H32 O10 2.0381 no . . H32 O12 2.7658 no . . H32 O21 3.5358 no . 1_565 H32 O23 3.2152 no . . H32 O25 3.0577 no . . H32 O28B 3.4776 no . . H32 H10 3.5418 no . 3_566 H32 H11 2.9632 no . 3_566 H32 H26 2.9234 no . 1_565 H32 H30 2.3547 no . . H32 H31 3.2843 no . . H32 H34 2.2464 no . . H32 H35 3.5022 no . . H33 S4 2.9624 no . 1_565 H33 O5 2.7456 no . 1_565 H33 O6 2.1994 no . 1_565 H33 O10 3.3444 no . . H33 O12 3.2268 no . . H33 O16 3.3435 no . 2_556 H33 O21 3.3870 no . 1_565 H33 O23 3.2642 no . . H33 O25 2.8809 no . . H33 H1 3.4818 no . 1_565 H33 H16 3.5547 no . 2_556 H33 H17 2.9903 no . 2_556 H33 H26 2.8645 no . 1_565 H33 H28 3.5105 no . . H33 H30 2.4468 no . . H33 H31 3.3734 no . . H33 H34 2.1001 no . . H33 H35 3.0403 no . . H34 O5 2.7007 no . 1_565 H34 O22 2.8637 no . . H34 O24 1.9678 no . . H34 O26 3.0636 no . . H34 H12 3.3522 no . . H34 H13 3.5112 no . . H34 H19 3.5477 no . 2_556 H34 H28 2.2355 no . . H34 H29 3.5828 no . . H34 H30 3.2718 no . . H34 H32 2.2464 no . . H34 H33 2.1001 no . . H34 H36 2.2916 no . . H34 H37 3.4159 no . . H34 H39 3.4249 no . . H35 S4 3.5702 no . 1_565 H35 O1 2.9524 no . 3_666 H35 O2 2.9213 no . 3_666 H35 O3 3.0147 no . 3_666 H35 O5 2.1881 no . 1_565 H35 O22 3.0622 no . . H35 O24 3.1692 no . . H35 O26 3.2120 no . . H35 H7 3.1080 no . 3_666 H35 H8 2.6551 no . 3_666 H35 H9 3.1903 no . 3_666 H35 H19 3.5076 no . 2_556 H35 H28 2.2771 no . . H35 H32 3.5022 no . . H35 H33 3.0403 no . . H35 H36 2.4271 no . . H35 H37 3.5544 no . . H36 S3 3.2971 no . 3_666 H36 O1 3.3384 no . . H36 O1 3.5110 no . 3_666 H36 O25 1.8835 no . . H36 O26 3.2655 no . 3_666 H36 O27 2.9706 no . . H36 C14 3.3728 no . . H36 C15 3.5014 no . . H36 H7 2.5253 no . . H36 H7 3.1337 no . 3_666 H36 H28 3.4675 no . . H36 H34 2.2916 no . . H36 H35 2.4271 no . . H36 H36 3.4594 no . 3_666 H36 H37 3.2080 no . 3_666 H36 H38 3.2992 no . . H36 H39 2.2058 no . . H37 S3 3.4884 no . . H37 O1 3.0424 no . . H37 O3 3.3922 no . . H37 O25 3.0959 no . . H37 O26 3.2615 no . 3_666 H37 O27 3.2133 no . . H37 C13 3.1273 no . . H37 C14 2.8223 no . . H37 C15 2.5736 no . . H37 C16 2.6764 no . . H37 C17 2.9900 no . . H37 C18 3.2325 no . . H37 H5 3.3454 no . . H37 H7 2.3880 no . . H37 H7 3.2300 no . 3_666 H37 H34 3.4159 no . . H37 H35 3.5544 no . . H37 H36 3.2080 no . 3_666 H37 H37 3.4415 no . 3_666 H37 H38 3.4630 no . . H37 H39 2.3993 no . . H38 O7 3.2263 no . . H38 O14 2.9068 no . . H38 O20 3.0715 no . . H38 O26 3.1191 no . . H38 O28A 1.8352 no . . H38 O28B 1.9840 no . . H38 C7 3.4461 no . . H38 C8 3.3946 no . . H38 H3 3.5944 no . . H38 H10 3.4494 no . . H38 H12 3.3749 no . . H38 H13 2.1542 no . . H38 H25 2.3011 no . . H38 H36 3.2992 no . . H38 H37 3.4630 no . . H39 O1 3.1632 no . . H39 O14 3.1067 no . . H39 O20 3.4332 no . . H39 O25 3.3846 no . . H39 O26 1.9510 no . . H39 O28A 2.7648 no . . H39 O28B 2.9929 no . . H39 C4 3.5422 no . . H39 H7 2.6622 no . . H39 H12 3.3793 no . . H39 H13 2.3319 no . . H39 H25 2.6005 no . . H39 H34 3.4249 no . . H39 H36 2.2058 no . . H39 H37 2.3993 no . . #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H7 S3 . . 3_666 3.098(9) 0.840 2.641 115.6 no O1 H7 O26 . . . 2.685(14) 0.840 1.928 149.3 no O2 H8 S1 . . . 3.062(9) 0.840 2.536 121.7 no O2 H8 O5 . . 3_656 2.828(12) 0.840 2.105 144.0 no O3 H9 S2 . . . 3.032(9) 0.840 2.509 121.4 no O3 H9 O2 . . . 2.944(12) 0.840 2.404 122.7 no O13 H10 O7 . . . 2.793(15) 0.845 1.957 170.0 no O13 H11 O10 . . 3_566 2.866(15) 0.860 2.105 147.2 no O14 H12 O22 . . . 2.738(13) 0.755 1.995 167.6 no O14 H13 O27 . . . 2.678(18) 0.786 1.903 168.0 no O15 H14 O4 . . 2_556 2.711(15) 0.764 1.953 171.1 no O15 H15 O23 . . . 2.793(14) 0.760 2.047 167.1 no O16 H16 O9 . . 4_555 2.773(13) 0.810 1.964 176.3 no O16 H17 O6 . . 2_556 2.781(16) 0.582 2.207 169.3 no O17 H18 O11 . . 3_566 2.714(13) 0.804 1.917 171.2 no O17 H19 O22 . . 2_546 2.711(13) 0.771 1.942 176.3 no O18 H20 O6 . . . 2.986(14) 0.853 2.158 163.7 no O18 H21 O23 . . 2_546 2.775(14) 0.744 2.040 170.0 no O19 H22 O8 . . 3_556 2.688(16) 0.844 1.903 154.1 no O19 H23 O21 . . . 2.687(17) 0.857 1.842 168.4 no O20 H24 O21 . . . 2.741(13) 0.803 1.947 169.6 no O20 H25 O27 . . . 2.698(16) 0.895 1.874 152.1 no O21 H26 O12 . . 1_545 2.742(16) 0.832 1.967 154.6 no O21 H27 O8 . . . 2.731(12) 0.811 1.985 152.6 no O22 H28 O25 . . . 2.795(17) 0.799 2.051 154.9 no O22 H29 O9 . . 4_555 2.874(13) 0.814 2.094 160.5 no O23 H30 O24 . . . 2.800(18) 0.913 1.914 163.0 no O23 H31 O7 . . 3_566 2.814(13) 0.902 1.918 171.6 no O24 H32 O10 . . . 2.867(13) 0.831 2.038 174.7 no O24 H33 O6 . . 1_565 2.993(13) 0.817 2.199 163.8 no O25 H34 O24 . . . 2.797(18) 0.834 1.968 173.3 no O25 H35 O5 . . 1_565 2.801(14) 0.818 2.188 131.8 no O26 H36 O25 . . . 2.674(17) 0.807 1.884 166.0 no O27 H38 O28A . . . 2.60(3) 0.771 1.835 171.3 no O27 H38 O28B . . . 2.73(5) 0.771 1.984 162.1 no O27 H39 O26 . . . 2.74(2) 0.825 1.951 160.3 no _database_code_depnum_ccdc_archive 'CCDC 894439' ####################################################################### # # 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_General #TrackingRef 'TC6A-SO3CeCIF.cif' _audit_creation_date 2010-06-17 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'TC6A-SO3YbCIF.cif' #============================================================================== data_TC6A-SO3Yb #TrackingRef 'TC6A-SO3YbCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H18 Yb2 O56 S12 ' _chemical_formula_moiety 'C36 H18 Yb2 O56 S12 ' _chemical_formula_weight 2077.30 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.4625(5) _cell_length_b 12.2942(4) _cell_length_c 20.5701(6) _cell_angle_alpha 90.0000 _cell_angle_beta 110.4422(8) _cell_angle_gamma 90.0000 _cell_volume 3664.08(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 24131 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.47 _cell_measurement_temperature 100.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028.00 _exptl_absorpt_coefficient_mu 2.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.741 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 33947 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). The disordered water molecule (O27) was isotropically refined. The water molecule indicated disordering at two positions (A and B sites). The parts containing (O27A and O27B) were refined as the disordered water molecules, occupancy of which was fixed at 0.54 and 0.46. Rasidual electron density was located around 1 angstrom from ytterbium metal center. ; _reflns_number_total 8308 _reflns_number_gt 6662 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1150 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8308 _refine_ls_number_parameters 478 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0255P)^2^+41.7697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 3.080 _refine_diff_density_min -1.810 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Yb Yb -0.385 5.549 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.832379(18) 0.23534(2) 0.351465(13) 0.01355(8) Uani 1.0 4 d . . . S1 S 0.51488(10) 0.33951(12) 0.37018(7) 0.0128(3) Uani 1.0 4 d . . . S2 S 0.61973(11) 0.06043(12) 0.59639(7) 0.0136(3) Uani 1.0 4 d . . . S3 S 0.78519(10) 0.41333(12) 0.75964(7) 0.0120(3) Uani 1.0 4 d . . . S4 S 0.58462(11) -0.08684(12) 0.33785(7) 0.0139(3) Uani 1.0 4 d . . . S5 S 0.97987(11) 0.16452(13) 0.64059(8) 0.0170(4) Uani 1.0 4 d . . . S6 S 0.82458(10) 0.76570(13) 0.60768(8) 0.0146(3) Uani 1.0 4 d . . . O1 O 0.5532(3) 0.2680(4) 0.5223(2) 0.0162(9) Uani 1.0 4 d . . . O2 O 0.6297(3) 0.2676(4) 0.6811(2) 0.0149(9) Uani 1.0 4 d . . . O3 O 0.5865(3) 0.4909(4) 0.7116(2) 0.0150(9) Uani 1.0 4 d . . . O4 O 0.6840(3) -0.0939(4) 0.3472(3) 0.0185(10) Uani 1.0 4 d . . . O5 O 0.5290(3) -0.0536(4) 0.2673(3) 0.0203(10) Uani 1.0 4 d . . . O6 O 0.5514(4) -0.1840(4) 0.3615(3) 0.0202(10) Uani 1.0 4 d . . . O7 O 0.9876(4) 0.2435(5) 0.5905(3) 0.0283(12) Uani 1.0 4 d . . . O8 O 0.9705(4) 0.0531(5) 0.6128(3) 0.0298(12) Uani 1.0 4 d . . . O9 O 1.0531(4) 0.1741(5) 0.7069(3) 0.0261(11) Uani 1.0 4 d . . . O10 O 0.8677(4) 0.6947(4) 0.5702(3) 0.0225(11) Uani 1.0 4 d . . . O11 O 0.8933(3) 0.8143(4) 0.6682(3) 0.0211(10) Uani 1.0 4 d . . . O12 O 0.7631(4) 0.8443(4) 0.5613(3) 0.0250(11) Uani 1.0 4 d . . . O13 O 0.8745(4) 0.0522(4) 0.3797(3) 0.0297(12) Uani 1.0 4 d . . . O14 O 0.9200(3) 0.1858(4) 0.2870(3) 0.0175(10) Uani 1.0 4 d . . . O15 O 0.7101(4) 0.1226(4) 0.2911(3) 0.0244(11) Uani 1.0 4 d . . . O16 O 0.7819(4) 0.1830(4) 0.4418(3) 0.0216(10) Uani 1.0 4 d . . . O17 O 0.7436(3) 0.3128(4) 0.2442(3) 0.0204(10) Uani 1.0 4 d . . . O18 O 0.9141(3) 0.3913(4) 0.3387(2) 0.0177(10) Uani 1.0 4 d . . . O19 O 0.9627(4) 0.2573(5) 0.4502(3) 0.0288(12) Uani 1.0 4 d . . . O20 O 0.7588(4) 0.3806(4) 0.3795(3) 0.0249(11) Uani 1.0 4 d . . . O21 O 0.8810(4) 0.0091(4) 0.2036(3) 0.0225(11) Uani 1.0 4 d . . . O22 O 0.8686(4) 0.6072(4) 0.3522(3) 0.0269(11) Uani 1.0 4 d . . . O23 O 0.7586(4) 0.3628(5) 0.5093(3) 0.0344(13) Uani 1.0 4 d . . . O24 O 0.6097(4) 0.4749(4) 0.5199(3) 0.0310(13) Uani 1.0 4 d . . . O25 O 0.5967(4) 0.6051(4) 0.4121(3) 0.0332(13) Uani 1.0 4 d . . . O26 O 0.7639(4) 0.7036(5) 0.4237(3) 0.0291(12) Uani 1.0 4 d . . . O27A O 0.9049(8) 0.4691(9) 0.5840(8) 0.034(5) Uiso 0.54(4) 4 d . . . O27B O 0.9191(14) 0.4782(17) 0.5526(15) 0.077(8) Uiso 0.46(4) 4 d . . . O28 O 0.8423(4) -0.0191(4) 0.4927(3) 0.0267(11) Uani 1.0 4 d . . . C1 C 0.5771(4) 0.0211(5) 0.3926(3) 0.0123(12) Uani 1.0 4 d . . . C2 C 0.5997(4) 0.0031(5) 0.4636(3) 0.0128(12) Uani 1.0 4 d . . . C3 C 0.5926(4) 0.0877(5) 0.5063(3) 0.0123(12) Uani 1.0 4 d . . . C4 C 0.5617(4) 0.1911(5) 0.4784(3) 0.0117(12) Uani 1.0 4 d . . . C5 C 0.5402(4) 0.2074(5) 0.4071(3) 0.0132(12) Uani 1.0 4 d . . . C6 C 0.5481(4) 0.1227(5) 0.3645(3) 0.0120(12) Uani 1.0 4 d . . . C7 C 0.8756(4) 0.1908(5) 0.6534(3) 0.0122(12) Uani 1.0 4 d . . . C8 C 0.8688(4) 0.2834(5) 0.6910(3) 0.0126(12) Uani 1.0 4 d . . . C9 C 0.7864(5) 0.3071(5) 0.7009(3) 0.0114(12) Uani 1.0 4 d . . . C10 C 0.7081(4) 0.2396(5) 0.6709(3) 0.0107(12) Uani 1.0 4 d . . . C11 C 0.7158(5) 0.1486(5) 0.6325(3) 0.0143(13) Uani 1.0 4 d . . . C12 C 0.8000(5) 0.1234(5) 0.6255(3) 0.0140(13) Uani 1.0 4 d . . . C13 C 0.7531(5) 0.6815(5) 0.6377(3) 0.0131(12) Uani 1.0 4 d . . . C14 C 0.6593(5) 0.7068(5) 0.6215(3) 0.0136(13) Uani 1.0 4 d . . . C15 C 0.6048(4) 0.6418(5) 0.6468(3) 0.0118(12) Uani 1.0 4 d . . . C16 C 0.6440(5) 0.5499(5) 0.6882(3) 0.0117(12) Uani 1.0 4 d . . . C17 C 0.7370(4) 0.5246(5) 0.7029(3) 0.0092(11) Uani 1.0 4 d . . . C18 C 0.7927(5) 0.5920(5) 0.6794(3) 0.0133(12) Uani 1.0 4 d . . . H1 H 0.5613 0.3296 0.5078 0.0194 Uiso 1.0 4 calc R . . H2 H 0.6199 -0.0668 0.4826 0.0153 Uiso 1.0 4 calc R . . H3 H 0.6160 0.4395 0.7364 0.0180 Uiso 1.0 4 calc R . . H4 H 0.5865 0.2272 0.6571 0.0179 Uiso 1.0 4 calc R . . H6 H 0.5335 0.1346 0.3162 0.0144 Uiso 1.0 4 calc R . . H8 H 0.9206 0.3300 0.7097 0.0151 Uiso 1.0 4 calc R . . H12 H 0.8055 0.0594 0.6013 0.0167 Uiso 1.0 4 calc R . . H14 H 0.6333 0.7681 0.5933 0.0164 Uiso 1.0 4 calc R . . H18 H 0.8567 0.5772 0.6916 0.0160 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Yb1 0.01660(14) 0.01238(14) 0.01154(13) 0.00032(10) 0.00475(10) 0.00167(10) S1 0.0142(7) 0.0084(7) 0.0150(7) 0.0009(6) 0.0042(6) 0.0031(6) S2 0.0195(8) 0.0105(8) 0.0087(7) -0.0023(6) 0.0025(6) 0.0007(5) S3 0.0170(8) 0.0071(7) 0.0091(7) 0.0013(6) 0.0010(6) -0.0003(5) S4 0.0185(8) 0.0118(8) 0.0116(7) 0.0002(6) 0.0054(6) -0.0026(6) S5 0.0174(8) 0.0178(9) 0.0166(8) 0.0028(6) 0.0069(7) -0.0004(6) S6 0.0148(7) 0.0124(8) 0.0174(7) -0.0007(6) 0.0065(6) 0.0037(6) O1 0.027(3) 0.007(2) 0.016(2) 0.0012(18) 0.0097(19) -0.0029(16) O2 0.017(3) 0.013(3) 0.014(2) -0.0025(18) 0.0045(18) -0.0036(16) O3 0.016(3) 0.013(3) 0.015(2) 0.0023(17) 0.0036(18) 0.0062(17) O4 0.019(3) 0.017(3) 0.020(3) -0.0007(19) 0.0066(19) -0.0053(18) O5 0.023(3) 0.021(3) 0.013(3) 0.005(2) 0.0023(19) -0.0045(18) O6 0.028(3) 0.012(3) 0.024(3) -0.0017(19) 0.012(2) -0.0008(18) O7 0.027(3) 0.038(4) 0.022(3) 0.002(3) 0.011(3) 0.004(3) O8 0.019(3) 0.029(3) 0.040(3) 0.006(3) 0.008(3) -0.011(3) O9 0.018(3) 0.035(3) 0.022(3) -0.000(3) 0.004(2) 0.001(2) O10 0.024(3) 0.020(3) 0.028(3) 0.001(2) 0.015(3) 0.0024(19) O11 0.017(3) 0.023(3) 0.023(3) -0.009(2) 0.007(2) -0.0038(19) O12 0.024(3) 0.021(3) 0.029(3) 0.002(2) 0.008(3) 0.014(2) O13 0.039(3) 0.020(3) 0.034(3) 0.010(3) 0.017(3) 0.010(2) O14 0.020(3) 0.015(3) 0.017(3) 0.0005(18) 0.0060(19) -0.0044(17) O15 0.030(3) 0.022(3) 0.021(3) -0.008(2) 0.008(2) -0.0024(19) O16 0.024(3) 0.025(3) 0.016(3) -0.003(2) 0.007(2) 0.0049(18) O17 0.016(3) 0.023(3) 0.018(3) 0.0025(19) 0.0013(19) 0.0073(19) O18 0.021(3) 0.017(3) 0.015(2) -0.0031(19) 0.0055(19) 0.0017(17) O19 0.015(3) 0.046(4) 0.023(3) -0.011(3) 0.003(2) 0.009(3) O20 0.031(3) 0.026(3) 0.021(3) 0.010(3) 0.013(3) 0.006(2) O21 0.026(3) 0.016(3) 0.023(3) -0.002(2) 0.005(2) -0.0056(19) O22 0.036(3) 0.017(3) 0.030(3) 0.003(3) 0.014(3) 0.001(2) O23 0.053(4) 0.031(3) 0.023(3) 0.004(3) 0.018(3) -0.001(3) O24 0.060(4) 0.012(3) 0.023(3) -0.007(3) 0.018(3) -0.0074(19) O25 0.050(4) 0.013(3) 0.038(3) 0.004(3) 0.017(3) 0.007(2) O26 0.036(3) 0.029(3) 0.025(3) 0.006(3) 0.014(3) 0.001(2) O28 0.033(3) 0.026(3) 0.024(3) -0.001(3) 0.014(3) 0.006(2) C1 0.013(3) 0.012(3) 0.009(3) -0.002(3) -0.001(3) -0.003(3) C2 0.017(3) 0.007(3) 0.014(3) 0.001(3) 0.004(3) 0.001(3) C3 0.015(3) 0.012(3) 0.009(3) -0.002(3) 0.003(3) 0.000(2) C4 0.015(3) 0.006(3) 0.012(3) 0.001(3) 0.003(3) -0.002(2) C5 0.012(3) 0.014(4) 0.012(3) 0.000(3) 0.002(3) -0.001(3) C6 0.014(3) 0.009(3) 0.012(3) 0.000(3) 0.004(3) 0.001(3) C7 0.016(3) 0.014(3) 0.009(3) 0.003(3) 0.007(3) 0.003(3) C8 0.016(3) 0.010(3) 0.009(3) -0.002(3) 0.001(3) 0.002(2) C9 0.021(3) 0.006(3) 0.006(3) 0.005(3) 0.003(3) 0.002(2) C10 0.019(3) 0.007(3) 0.007(3) 0.005(3) 0.004(3) 0.004(2) C11 0.021(4) 0.010(3) 0.010(3) 0.000(3) 0.003(3) 0.001(3) C12 0.025(4) 0.005(3) 0.010(3) 0.003(3) 0.002(3) 0.000(2) C13 0.022(4) 0.003(3) 0.013(3) -0.002(3) 0.004(3) -0.002(2) C14 0.020(3) 0.007(3) 0.010(3) -0.002(3) -0.000(3) 0.000(2) C15 0.011(3) 0.013(3) 0.009(3) -0.001(3) 0.001(3) -0.005(3) C16 0.019(3) 0.010(3) 0.006(3) 0.000(3) 0.005(3) -0.000(2) C17 0.012(3) 0.007(3) 0.008(3) 0.001(3) 0.002(3) -0.002(2) C18 0.014(3) 0.013(3) 0.011(3) 0.001(3) 0.002(3) -0.002(3) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Yb1 O13 2.359(5) yes . . Yb1 O14 2.286(6) yes . . Yb1 O15 2.323(5) yes . . Yb1 O16 2.343(6) yes . . Yb1 O17 2.354(5) yes . . Yb1 O18 2.361(5) yes . . Yb1 O19 2.324(4) yes . . Yb1 O20 2.297(6) yes . . S1 C5 1.778(6) yes . . S1 C15 1.775(7) yes . 3_666 S2 C3 1.783(6) yes . . S2 C11 1.779(6) yes . . S3 C9 1.784(6) yes . . S3 C17 1.784(6) yes . . S4 O4 1.483(5) yes . . S4 O5 1.464(5) yes . . S4 O6 1.450(5) yes . . S4 C1 1.771(7) yes . . S5 O7 1.450(6) yes . . S5 O8 1.472(6) yes . . S5 O9 1.442(5) yes . . S5 C7 1.753(7) yes . . S6 O10 1.469(6) yes . . S6 O11 1.454(5) yes . . S6 O12 1.454(5) yes . . S6 C13 1.775(7) yes . . O1 C4 1.345(8) yes . . O2 C10 1.345(9) yes . . O3 C16 1.358(9) yes . . C1 C2 1.394(9) yes . . C1 C6 1.383(9) yes . . C2 C3 1.392(9) yes . . C3 C4 1.408(9) yes . . C4 C5 1.400(9) yes . . C5 C6 1.393(9) yes . . C7 C8 1.399(9) yes . . C7 C12 1.384(9) yes . . C8 C9 1.390(10) yes . . C9 C10 1.418(8) yes . . C10 C11 1.399(9) yes . . C11 C12 1.393(10) yes . . C13 C14 1.404(9) yes . . C13 C18 1.398(8) yes . . C14 C15 1.388(10) yes . . C15 C16 1.417(8) yes . . C16 C17 1.398(9) yes . . C17 C18 1.397(10) yes . . O1 H1 0.840 no . . O2 H4 0.840 no . . O3 H3 0.840 no . . C2 H2 0.950 no . . C6 H6 0.950 no . . C8 H8 0.950 no . . C12 H12 0.950 no . . C14 H14 0.950 no . . C18 H18 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O13 Yb1 O14 73.75(19) yes . . . O13 Yb1 O15 70.46(17) yes . . . O13 Yb1 O16 71.5(2) yes . . . O13 Yb1 O17 129.58(17) yes . . . O13 Yb1 O18 133.63(18) yes . . . O13 Yb1 O19 79.36(18) yes . . . O13 Yb1 O20 143.0(2) yes . . . O14 Yb1 O15 93.89(18) yes . . . O14 Yb1 O16 144.74(16) yes . . . O14 Yb1 O17 80.45(17) yes . . . O14 Yb1 O18 72.70(17) yes . . . O14 Yb1 O19 91.68(17) yes . . . O14 Yb1 O20 143.04(18) yes . . . O15 Yb1 O16 79.95(17) yes . . . O15 Yb1 O17 68.95(16) yes . . . O15 Yb1 O18 142.39(15) yes . . . O15 Yb1 O19 146.30(18) yes . . . O15 Yb1 O20 102.47(18) yes . . . O16 Yb1 O17 127.39(17) yes . . . O16 Yb1 O18 130.63(16) yes . . . O16 Yb1 O19 76.48(18) yes . . . O16 Yb1 O20 71.53(18) yes . . . O17 Yb1 O18 74.15(15) yes . . . O17 Yb1 O19 144.68(18) yes . . . O17 Yb1 O20 75.08(17) yes . . . O18 Yb1 O19 70.64(17) yes . . . O18 Yb1 O20 74.21(19) yes . . . O19 Yb1 O20 92.55(18) yes . . . C5 S1 C15 105.2(3) yes . . 3_666 C3 S2 C11 100.3(3) yes . . . C9 S3 C17 102.7(3) yes . . . O4 S4 O5 111.6(3) yes . . . O4 S4 O6 112.3(3) yes . . . O4 S4 C1 104.9(3) yes . . . O5 S4 O6 114.1(3) yes . . . O5 S4 C1 106.0(3) yes . . . O6 S4 C1 107.1(3) yes . . . O7 S5 O8 111.6(4) yes . . . O7 S5 O9 112.7(3) yes . . . O7 S5 C7 107.0(3) yes . . . O8 S5 O9 112.4(3) yes . . . O8 S5 C7 105.0(3) yes . . . O9 S5 C7 107.6(3) yes . . . O10 S6 O11 111.3(3) yes . . . O10 S6 O12 111.3(3) yes . . . O10 S6 C13 106.8(3) yes . . . O11 S6 O12 113.8(3) yes . . . O11 S6 C13 107.4(3) yes . . . O12 S6 C13 105.8(3) yes . . . S4 C1 C2 119.9(5) yes . . . S4 C1 C6 119.6(5) yes . . . C2 C1 C6 120.5(6) yes . . . C1 C2 C3 119.7(6) yes . . . S2 C3 C2 118.3(5) yes . . . S2 C3 C4 121.1(5) yes . . . C2 C3 C4 120.5(6) yes . . . O1 C4 C3 117.3(6) yes . . . O1 C4 C5 124.1(6) yes . . . C3 C4 C5 118.6(6) yes . . . S1 C5 C4 120.9(5) yes . . . S1 C5 C6 118.0(5) yes . . . C4 C5 C6 120.7(6) yes . . . C1 C6 C5 119.9(6) yes . . . S5 C7 C8 118.9(5) yes . . . S5 C7 C12 121.0(5) yes . . . C8 C7 C12 120.1(7) yes . . . C7 C8 C9 120.0(6) yes . . . S3 C9 C8 118.7(5) yes . . . S3 C9 C10 120.9(6) yes . . . C8 C9 C10 120.0(6) yes . . . O2 C10 C9 117.5(6) yes . . . O2 C10 C11 123.5(6) yes . . . C9 C10 C11 119.0(6) yes . . . S2 C11 C10 120.0(6) yes . . . S2 C11 C12 119.7(5) yes . . . C10 C11 C12 120.2(6) yes . . . C7 C12 C11 120.5(6) yes . . . S6 C13 C14 120.3(5) yes . . . S6 C13 C18 118.7(5) yes . . . C14 C13 C18 121.0(7) yes . . . C13 C14 C15 119.6(6) yes . . . S1 C15 C14 125.4(5) yes 3_666 . . S1 C15 C16 114.8(5) yes 3_666 . . C14 C15 C16 119.8(6) yes . . . O3 C16 C15 116.3(6) yes . . . O3 C16 C17 123.8(5) yes . . . C15 C16 C17 119.9(6) yes . . . S3 C17 C16 118.3(5) yes . . . S3 C17 C18 121.0(5) yes . . . C16 C17 C18 120.4(6) yes . . . C13 C18 C17 119.2(6) yes . . . C4 O1 H1 109.473 no . . . C10 O2 H4 109.476 no . . . C16 O3 H3 109.471 no . . . C1 C2 H2 120.132 no . . . C3 C2 H2 120.133 no . . . C1 C6 H6 120.034 no . . . C5 C6 H6 120.035 no . . . C7 C8 H8 119.981 no . . . C9 C8 H8 119.989 no . . . C7 C12 H12 119.769 no . . . C11 C12 H12 119.766 no . . . C13 C14 H14 120.179 no . . . C15 C14 H14 120.188 no . . . C13 C18 H18 120.387 no . . . C17 C18 H18 120.383 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C5 S1 C15 C14 13.2(6) no . . 3_666 3_666 C5 S1 C15 C16 -168.7(4) no . . 3_666 3_666 C15 S1 C5 C4 -85.8(5) no 3_666 . . . C15 S1 C5 C6 101.1(5) no 3_666 . . . C3 S2 C11 C10 111.4(5) no . . . . C3 S2 C11 C12 -71.9(5) no . . . . C11 S2 C3 C2 117.2(5) no . . . . C11 S2 C3 C4 -65.0(5) no . . . . C9 S3 C17 C16 101.1(5) no . . . . C9 S3 C17 C18 -85.4(5) no . . . . C17 S3 C9 C8 100.3(4) no . . . . C17 S3 C9 C10 -86.8(5) no . . . . O4 S4 C1 C2 -80.2(5) no . . . . O4 S4 C1 C6 100.3(5) no . . . . O5 S4 C1 C2 161.6(5) no . . . . O5 S4 C1 C6 -17.9(6) no . . . . O6 S4 C1 C2 39.4(5) no . . . . O6 S4 C1 C6 -140.1(5) no . . . . O7 S5 C7 C8 -72.5(5) no . . . . O7 S5 C7 C12 105.8(5) no . . . . O8 S5 C7 C8 168.8(4) no . . . . O8 S5 C7 C12 -13.0(5) no . . . . O9 S5 C7 C8 48.8(5) no . . . . O9 S5 C7 C12 -132.9(4) no . . . . O10 S6 C13 C14 -125.6(4) no . . . . O10 S6 C13 C18 56.3(5) no . . . . O11 S6 C13 C14 114.9(4) no . . . . O11 S6 C13 C18 -63.2(5) no . . . . O12 S6 C13 C14 -6.9(5) no . . . . O12 S6 C13 C18 174.9(4) no . . . . S4 C1 C2 C3 -179.2(4) no . . . . S4 C1 C6 C5 178.7(4) no . . . . C2 C1 C6 C5 -0.8(9) no . . . . C6 C1 C2 C3 0.3(9) no . . . . C1 C2 C3 S2 178.6(5) no . . . . C1 C2 C3 C4 0.8(9) no . . . . S2 C3 C4 O1 -0.2(8) no . . . . S2 C3 C4 C5 -179.1(4) no . . . . C2 C3 C4 O1 177.6(6) no . . . . C2 C3 C4 C5 -1.3(9) no . . . . O1 C4 C5 S1 9.2(9) no . . . . O1 C4 C5 C6 -178.0(5) no . . . . C3 C4 C5 S1 -172.0(5) no . . . . C3 C4 C5 C6 0.8(9) no . . . . S1 C5 C6 C1 173.2(4) no . . . . C4 C5 C6 C1 0.2(9) no . . . . S5 C7 C8 C9 178.9(4) no . . . . S5 C7 C12 C11 -176.2(4) no . . . . C8 C7 C12 C11 2.0(8) no . . . . C12 C7 C8 C9 0.7(8) no . . . . C7 C8 C9 S3 170.7(5) no . . . . C7 C8 C9 C10 -2.3(8) no . . . . S3 C9 C10 O2 8.5(7) no . . . . S3 C9 C10 C11 -171.6(4) no . . . . C8 C9 C10 O2 -178.7(5) no . . . . C8 C9 C10 C11 1.1(8) no . . . . O2 C10 C11 S2 -1.9(8) no . . . . O2 C10 C11 C12 -178.6(5) no . . . . C9 C10 C11 S2 178.2(5) no . . . . C9 C10 C11 C12 1.6(8) no . . . . S2 C11 C12 C7 -179.8(4) no . . . . C10 C11 C12 C7 -3.2(9) no . . . . S6 C13 C14 C15 -178.4(4) no . . . . S6 C13 C18 C17 -179.5(4) no . . . . C14 C13 C18 C17 2.4(9) no . . . . C18 C13 C14 C15 -0.3(9) no . . . . C13 C14 C15 S1 -178.6(5) no . . . 3_666 C13 C14 C15 C16 -0.6(8) no . . . . S1 C15 C16 O3 -2.4(7) no 3_666 . . . S1 C15 C16 C17 177.7(4) no 3_666 . . . C14 C15 C16 O3 179.4(5) no . . . . C14 C15 C16 C17 -0.6(8) no . . . . O3 C16 C17 S3 -3.8(8) no . . . . O3 C16 C17 C18 -177.3(5) no . . . . C15 C16 C17 S3 176.2(5) no . . . . C15 C16 C17 C18 2.7(8) no . . . . S3 C17 C18 C13 -176.9(4) no . . . . C16 C17 C18 C13 -3.6(8) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 O1 3.102(5) no . . S1 O3 2.791(5) no . 3_666 S2 O1 2.966(5) no . . S2 O2 3.059(5) no . . S3 O2 2.981(5) no . . S3 O3 3.033(5) no . . O1 O2 3.060(6) no . . O1 C10 3.176(6) no . . O1 C11 3.104(7) no . . O1 C14 3.585(7) no . 3_666 O2 O3 2.945(7) no . . O2 C16 3.478(8) no . . O2 C17 3.524(7) no . . O4 C2 3.320(9) no . . O4 C6 3.487(8) no . . O5 C6 2.893(8) no . . O6 C2 3.026(8) no . . O7 C8 3.247(10) no . . O7 C12 3.546(9) no . . O8 C12 2.872(9) no . . O9 C8 3.063(9) no . . O10 C18 3.131(9) no . . O11 C18 3.193(8) no . . O12 C14 2.889(9) no . . C1 C4 2.798(9) no . . C2 C5 2.785(9) no . . C3 C6 2.786(9) no . . C3 C12 3.315(8) no . . C4 C11 3.276(8) no . . C4 C14 3.545(8) no . 3_666 C4 C15 3.584(8) no . 3_666 C5 C14 3.116(9) no . 3_666 C7 C10 2.800(10) no . . C8 C11 2.793(9) no . . C9 C12 2.789(9) no . . C9 C18 3.537(9) no . . C10 C17 3.564(8) no . . C13 C16 2.787(10) no . . C14 C17 2.803(8) no . . C15 C18 2.810(9) no . . S1 O21 3.309(6) no . 2_655 S1 O24 3.354(5) no . . S1 O25 3.499(6) no . . S2 S3 3.3408(19) no . 2_646 S2 O6 3.415(6) no . 3_656 S2 C1 3.286(7) no . 3_656 S2 C2 3.274(7) no . 3_656 S3 S2 3.3408(19) no . 2_656 S3 C14 3.420(6) no . 2_646 S4 O15 3.553(6) no . . O1 O6 3.478(8) no . 3_656 O1 O23 3.479(9) no . . O1 O24 2.696(7) no . . O1 O25 3.438(9) no . 3_666 O2 O6 2.820(7) no . 3_656 O2 O11 3.292(7) no . 2_646 O2 C18 3.455(7) no . 2_646 O3 O11 3.223(7) no . 2_646 O3 O21 3.124(7) no . 4_455 O3 O25 3.295(6) no . 3_666 O3 C7 3.600(8) no . 2_656 O3 C12 3.585(7) no . 2_656 O4 O13 3.313(7) no . . O4 O15 2.985(7) no . . O4 O17 2.753(8) no . 2_645 O4 O18 3.592(6) no . 2_645 O4 O26 2.973(7) no . 1_545 O4 O28 3.267(6) no . . O5 O14 3.571(7) no . 2_645 O5 O15 3.437(7) no . . O5 O18 2.706(8) no . 2_645 O5 C18 3.497(8) no . 4_454 O6 S2 3.415(6) no . 3_656 O6 O1 3.478(8) no . 3_656 O6 O2 2.820(7) no . 3_656 O6 O25 2.790(7) no . 1_545 O6 O26 3.377(7) no . 1_545 O7 O19 2.780(8) no . . O7 O22 2.806(7) no . 3_766 O7 O27A 3.039(13) no . . O7 O27B 3.08(2) no . . O8 O11 3.506(8) no . 1_545 O8 O13 2.681(8) no . 3_756 O8 O28 2.721(7) no . . O9 O15 3.493(7) no . 4_555 O9 O17 2.776(7) no . 4_555 O9 O21 2.862(7) no . 3_756 O9 O22 3.347(8) no . 3_766 O10 O18 3.405(6) no . 3_766 O10 O19 2.858(8) no . 3_766 O10 O26 2.879(7) no . . O10 O27A 2.827(12) no . . O10 O27B 2.84(3) no . . O11 O2 3.292(7) no . 2_656 O11 O3 3.223(7) no . 2_656 O11 O8 3.506(8) no . 1_565 O11 O14 2.705(7) no . 3_766 O12 O26 3.321(8) no . . O12 O28 2.743(8) no . 1_565 O12 C2 3.269(7) no . 1_565 O13 O4 3.313(7) no . . O13 O8 2.681(8) no . 3_756 O13 O28 2.688(9) no . . O14 O5 3.571(7) no . 2_655 O14 O11 2.705(7) no . 3_766 O14 O21 2.702(7) no . . O15 S4 3.553(6) no . . O15 O4 2.985(7) no . . O15 O5 3.437(7) no . . O15 O9 3.493(7) no . 4_454 O15 O22 2.775(7) no . 2_645 O15 C6 3.346(10) no . . O16 O23 2.701(8) no . . O16 O28 2.731(7) no . . O16 C1 3.574(8) no . . O16 C5 3.564(8) no . . O16 C6 3.483(8) no . . O17 O4 2.753(8) no . 2_655 O17 O9 2.776(7) no . 4_454 O17 O21 3.483(8) no . 2_655 O17 O22 3.306(7) no . 2_645 O18 O4 3.592(6) no . 2_655 O18 O5 2.706(8) no . 2_655 O18 O10 3.405(6) no . 3_766 O18 O22 2.785(7) no . . O18 O27A 3.194(12) no . 3_766 O18 O27B 3.19(2) no . 3_766 O19 O7 2.780(8) no . . O19 O10 2.858(8) no . 3_766 O20 O21 2.740(7) no . 2_655 O20 O22 3.409(8) no . . O20 O23 2.681(8) no . . O21 S1 3.309(6) no . 2_645 O21 O3 3.124(7) no . 4_554 O21 O9 2.862(7) no . 3_756 O21 O14 2.702(7) no . . O21 O17 3.483(8) no . 2_645 O21 O20 2.740(7) no . 2_645 O21 O25 2.782(8) no . 2_645 O22 O7 2.806(7) no . 3_766 O22 O9 3.347(8) no . 3_766 O22 O15 2.775(7) no . 2_655 O22 O17 3.306(7) no . 2_655 O22 O18 2.785(7) no . . O22 O20 3.409(8) no . . O22 O26 2.802(9) no . . O22 O27A 3.415(12) no . 3_766 O22 O27B 3.35(2) no . 3_766 O23 O1 3.479(9) no . . O23 O16 2.701(8) no . . O23 O20 2.681(8) no . . O23 O24 2.755(9) no . . O23 O27A 2.600(12) no . . O23 O27B 2.72(2) no . . O23 C4 3.574(9) no . . O23 C7 3.575(8) no . . O24 S1 3.354(5) no . . O24 O1 2.696(7) no . . O24 O23 2.755(9) no . . O24 O24 3.260(9) no . 3_666 O24 O25 2.685(8) no . . O24 C14 3.459(8) no . . O24 C15 3.342(8) no . . O24 C16 3.442(8) no . . O25 S1 3.499(6) no . . O25 O1 3.438(9) no . 3_666 O25 O3 3.295(6) no . 3_666 O25 O6 2.790(7) no . 1_565 O25 O21 2.782(8) no . 2_655 O25 O24 2.685(8) no . . O25 O26 2.788(9) no . . O26 O4 2.973(7) no . 1_565 O26 O6 3.377(7) no . 1_565 O26 O10 2.879(7) no . . O26 O12 3.321(8) no . . O26 O22 2.802(9) no . . O26 O25 2.788(9) no . . O27A O7 3.039(13) no . . O27A O10 2.827(12) no . . O27A O18 3.194(12) no . 3_766 O27A O22 3.415(12) no . 3_766 O27A O23 2.600(12) no . . O27A C8 3.351(15) no . . O27A C18 3.394(17) no . . O27B O7 3.08(2) no . . O27B O10 2.84(3) no . . O27B O18 3.19(2) no . 3_766 O27B O22 3.35(2) no . 3_766 O27B O23 2.72(2) no . . O28 O4 3.267(6) no . . O28 O8 2.721(7) no . . O28 O12 2.743(8) no . 1_545 O28 O13 2.688(9) no . . O28 O16 2.731(7) no . . O28 C2 3.596(9) no . . O28 C12 3.494(9) no . . C1 S2 3.286(7) no . 3_656 C1 O16 3.574(8) no . . C2 S2 3.274(7) no . 3_656 C2 O12 3.269(7) no . 1_545 C2 O28 3.596(9) no . . C2 C3 3.430(10) no . 3_656 C3 C2 3.430(10) no . 3_656 C3 C3 3.522(9) no . 3_656 C4 O23 3.574(9) no . . C5 O16 3.564(8) no . . C6 O15 3.346(10) no . . C6 O16 3.483(8) no . . C7 O3 3.600(8) no . 2_646 C7 O23 3.575(8) no . . C8 O27A 3.351(15) no . . C10 C17 3.592(8) no . 2_646 C10 C18 3.578(9) no . 2_646 C11 C17 3.548(8) no . 2_646 C12 O3 3.585(7) no . 2_646 C12 O28 3.494(9) no . . C14 S3 3.420(6) no . 2_656 C14 O24 3.459(8) no . . C15 O24 3.342(8) no . . C16 O24 3.442(8) no . . C17 C10 3.592(8) no . 2_656 C17 C11 3.548(8) no . 2_656 C18 O2 3.455(7) no . 2_656 C18 O5 3.497(8) no . 4_555 C18 O27A 3.394(17) no . . C18 C10 3.578(9) no . 2_656 S1 H1 2.6695 no . . S1 H6 2.8076 no . . S1 H14 2.9610 no . 3_666 S2 H2 2.8156 no . . S2 H4 2.5452 no . . S2 H12 2.8382 no . . S3 H3 2.5097 no . . S3 H8 2.8263 no . . S3 H18 2.8844 no . . S4 H2 2.8444 no . . S4 H6 2.8266 no . . S5 H8 2.8130 no . . S5 H12 2.8414 no . . S6 H14 2.8678 no . . S6 H18 2.8283 no . . O1 H4 2.6848 no . . O1 H14 3.0626 no . 3_666 O2 H1 3.4306 no . . O2 H3 2.4443 no . . O3 H4 3.4301 no . . O4 H2 3.2829 no . . O4 H6 3.5611 no . . O5 H6 2.5143 no . . O6 H2 2.7501 no . . O7 H8 3.1614 no . . O8 H12 2.4804 no . . O9 H8 2.8216 no . . O10 H18 2.9405 no . . O11 H18 3.0398 no . . O12 H14 2.5018 no . . C2 H6 3.2678 no . . C2 H12 3.5119 no . . C3 H1 3.0151 no . . C3 H4 3.5749 no . . C3 H12 3.2062 no . . C4 H2 3.2887 no . . C4 H4 3.5888 no . . C4 H6 3.2833 no . . C4 H14 2.8999 no . 3_666 C5 H1 2.4876 no . . C5 H14 2.6970 no . 3_666 C6 H2 3.2669 no . . C6 H14 3.4817 no . 3_666 C8 H12 3.2685 no . . C9 H3 3.3861 no . . C9 H4 3.0635 no . . C9 H18 3.5198 no . . C10 H1 3.5090 no . . C10 H3 3.3496 no . . C10 H8 3.2910 no . . C10 H12 3.2758 no . . C11 H4 2.4285 no . . C12 H8 3.2679 no . . C14 H1 3.5460 no . 3_666 C14 H18 3.2954 no . . C15 H1 3.3366 no . 3_666 C15 H3 3.0635 no . . C16 H14 3.2879 no . . C16 H18 3.2826 no . . C17 H3 2.4430 no . . C18 H14 3.2934 no . . H1 H4 3.2148 no . . H1 H14 3.2332 no . 3_666 H2 H12 3.4213 no . . H3 H4 3.0265 no . . H8 H18 3.1761 no . . S2 H2 3.4888 no . 3_656 S3 H14 3.3566 no . 2_646 S4 H4 3.1908 no . 3_656 O2 H18 3.4646 no . 2_646 O5 H4 3.4790 no . 3_656 O5 H8 3.2211 no . 4_454 O5 H18 2.5900 no . 4_454 O6 H4 2.0991 no . 3_656 O9 H6 3.3400 no . 4_555 O11 H3 2.5378 no . 2_656 O11 H12 3.3933 no . 1_565 O12 H2 2.4933 no . 1_565 O12 H12 2.7788 no . 1_565 O15 H6 2.9547 no . . O16 H12 3.5180 no . . O21 H3 3.5142 no . 4_554 O23 H1 3.0664 no . . O24 H1 1.9188 no . . O24 H1 3.4704 no . 3_666 O25 H1 3.4850 no . 3_666 O25 H4 3.3890 no . 3_666 O27A H8 3.0386 no . . O27A H18 2.8931 no . . O27B H18 3.5379 no . . O28 H2 3.4224 no . . O28 H12 2.6716 no . . C3 H2 3.3826 no . 3_656 C4 H2 3.5273 no . 3_656 C6 H8 3.1593 no . 4_454 C8 H6 3.0913 no . 4_555 C12 H3 3.5055 no . 2_646 H1 O23 3.0664 no . . H1 O24 1.9188 no . . H1 O24 3.4704 no . 3_666 H1 O25 3.4850 no . 3_666 H2 S2 3.4888 no . 3_656 H2 O12 2.4933 no . 1_545 H2 O28 3.4224 no . . H2 C3 3.3826 no . 3_656 H2 C4 3.5273 no . 3_656 H2 H14 3.0032 no . 1_545 H3 O11 2.5378 no . 2_646 H3 O21 3.5142 no . 4_455 H3 C12 3.5055 no . 2_656 H3 H12 3.4581 no . 2_656 H4 S4 3.1908 no . 3_656 H4 O5 3.4790 no . 3_656 H4 O6 2.0991 no . 3_656 H4 O25 3.3890 no . 3_666 H4 H18 3.4572 no . 2_646 H6 O9 3.3400 no . 4_454 H6 O15 2.9547 no . . H6 C8 3.0913 no . 4_454 H6 H8 2.3168 no . 4_454 H8 O5 3.2211 no . 4_555 H8 O27A 3.0386 no . . H8 C6 3.1593 no . 4_555 H8 H6 2.3168 no . 4_555 H12 O11 3.3933 no . 1_545 H12 O12 2.7788 no . 1_545 H12 O16 3.5180 no . . H12 O28 2.6716 no . . H12 H3 3.4581 no . 2_646 H14 S3 3.3566 no . 2_656 H14 H2 3.0032 no . 1_565 H18 O2 3.4646 no . 2_656 H18 O5 2.5900 no . 4_555 H18 O27A 2.8931 no . . H18 O27B 3.5379 no . . H18 H4 3.4572 no . 2_656 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 S1 . . . 3.102(5) 0.840 2.670 113.6 no O1 H1 O24 . . . 2.696(7) 0.840 1.919 153.4 no O2 H4 S2 . . . 3.059(5) 0.840 2.545 120.6 no O2 H4 O6 . . 3_656 2.820(7) 0.840 2.099 143.7 no O3 H3 S3 . . . 3.033(5) 0.840 2.510 121.4 no O3 H3 O2 . . . 2.945(7) 0.840 2.444 119.0 no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 894440'