# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1599 data_global _audit_creation_method SHELXL-97 _publ_contact_author_name ' Colin L. Raston' _publ_contact_author_email ' c.raston@sci.monash.edu.au ' _publ_contact_author_fax ' 61 - 3 - 9905 4597 ' loop_ _publ_author_name _publ_author_address ' Michaele J. Hardie ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; ' Julian A. Johnson ' ; CSIRO Minerals Clayton 3168 Victoria AUSTRALIA ; ' Helen R. Webb ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; ' Colin L. Raston' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; _publ_requested_journal 'Chemical Communications' _chemical_name_systematic ; ? ; _chemical_name_common ;{(tetra-p-sulfonatocalix[4]arene)(18- crown-6)0.5[yttrium hexahydrate]1.333}tetrahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H58.67 O32.33 S4 Y1.33' _chemical_formula_weight 1231.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0226(2) _cell_length_b 28.2424(7) _cell_length_c 15.1695(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.5120(10) _cell_angle_gamma 90.00 _cell_volume 5106.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2549 _exptl_absorpt_coefficient_mu 1.776 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67206 _diffrn_reflns_av_R_equivalents 0.101 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 29.58 _reflns_number_total 13671 _reflns_number_gt 8255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+15.6700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13671 _refine_ls_number_parameters 738 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1547 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2559 _refine_ls_wR_factor_gt 0.2139 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y2 Y -0.4864(3) 0.51735(9) -0.01940(17) 0.0531(6) Uani 0.33 1 d P . . Y1 Y -0.82698(4) 0.519242(18) -0.65353(4) 0.01743(15) Uani 1 1 d . . . S1 S -0.27701(17) 0.61107(6) -0.12096(12) 0.0421(5) Uani 1 1 d . . . S2 S -0.12101(11) 0.62911(5) -0.61450(9) 0.0186(3) Uani 1 1 d . . . S3 S -0.70625(13) 0.61878(5) -0.76366(11) 0.0273(3) Uani 1 1 d . . . S4 S -0.89345(11) 0.61173(5) -0.30738(10) 0.0206(3) Uani 1 1 d . . . C1 C -0.0492(5) 0.0866(2) 0.1048(5) 0.0312(14) Uani 1 1 d . . . H1A H -0.0667 0.1191 0.1181 0.037 Uiso 1 1 calc R . . H1B H 0.0316 0.0828 0.1148 0.037 Uiso 1 1 calc R . . C2 C 0.1022(5) -0.0541(2) -0.1645(5) 0.0319(14) Uani 1 1 d . . . H2A H 0.1828 -0.0536 -0.1476 0.038 Uiso 1 1 calc R . . H2B H 0.0869 -0.0651 -0.2255 0.038 Uiso 1 1 calc R . . C3 C -0.0700(5) 0.1139(2) -0.0432(5) 0.0329(15) Uani 1 1 d . . . H3A H -0.1014 0.1427 -0.0219 0.039 Uiso 1 1 calc R . . H3B H -0.1099 0.1071 -0.1016 0.039 Uiso 1 1 calc R . . C4 C 0.0526(5) 0.1226(2) -0.0523(5) 0.0321(15) Uani 1 1 d . . . H4A H 0.0577 0.1485 -0.0936 0.038 Uiso 1 1 calc R . . H4B H 0.0916 0.1321 0.0050 0.038 Uiso 1 1 calc R . . C5 C 0.0810(5) 0.0757(2) -0.1761(4) 0.0305(14) Uani 1 1 d . . . H5A H 0.1184 0.0995 -0.2077 0.037 Uiso 1 1 calc R . . H5B H 0.0008 0.0783 -0.1940 0.037 Uiso 1 1 calc R . . C6 C 0.1210(6) 0.0275(3) -0.1971(5) 0.0374(16) Uani 1 1 d . . . H6A H 0.1125 0.0229 -0.2610 0.045 Uiso 1 1 calc R . . H6B H 0.1998 0.0241 -0.1743 0.045 Uiso 1 1 calc R . . C7 C -0.3995(5) 0.7368(2) -0.2868(4) 0.0260(13) Uani 1 1 d . . . C8 C -0.4684(5) 0.7173(2) -0.2299(4) 0.0229(12) Uani 1 1 d . A . C9 C -0.4317(6) 0.6774(2) -0.1814(4) 0.0289(14) Uani 1 1 d . . . H9 H -0.4762 0.6639 -0.1425 0.035 Uiso 1 1 calc R A . C10 C -0.3279(6) 0.6576(2) -0.1912(4) 0.0342(16) Uani 1 1 d . A . C11 C -0.2603(5) 0.6774(2) -0.2493(4) 0.0323(15) Uani 1 1 d . . . H11 H -0.1912 0.6637 -0.2550 0.039 Uiso 1 1 calc R A . C12 C -0.2948(5) 0.7173(2) -0.2989(4) 0.0298(14) Uani 1 1 d . A . C13 C -0.2164(5) 0.7395(3) -0.3586(4) 0.0328(15) Uani 1 1 d . . . H13A H -0.2227 0.7737 -0.3551 0.039 Uiso 1 1 calc R A . H13B H -0.1398 0.7311 -0.3358 0.039 Uiso 1 1 calc R . . C14 C -0.3138(5) 0.7500(2) -0.5154(4) 0.0231(12) Uani 1 1 d . . . C15 C -0.2388(5) 0.7250(2) -0.4549(4) 0.0246(13) Uani 1 1 d . A . C16 C -0.1828(4) 0.6869(2) -0.4862(4) 0.0205(11) Uani 1 1 d . . . H16 H -0.1306 0.6700 -0.4477 0.025 Uiso 1 1 calc R A . C17 C -0.2045(4) 0.6738(2) -0.5751(4) 0.0186(11) Uani 1 1 d . A . C18 C -0.2834(5) 0.6977(2) -0.6320(4) 0.0207(12) Uani 1 1 d . . . H18 H -0.2985 0.6881 -0.6909 0.025 Uiso 1 1 calc R A . C19 C -0.3411(5) 0.7361(2) -0.6029(4) 0.0211(12) Uani 1 1 d . A . C20 C -0.4357(5) 0.7588(2) -0.6654(4) 0.0229(12) Uani 1 1 d . . . H20A H -0.4414 0.7921 -0.6509 0.027 Uiso 1 1 calc R A . H20B H -0.4195 0.7565 -0.7263 0.027 Uiso 1 1 calc R . . C21 C -0.6201(5) 0.7504(2) -0.6000(4) 0.0225(12) Uani 1 1 d . . . C22 C -0.5462(5) 0.7340(2) -0.6567(4) 0.0238(12) Uani 1 1 d . A . C23 C -0.5734(5) 0.6931(2) -0.7050(4) 0.0228(12) Uani 1 1 d . . . H23 H -0.5245 0.6816 -0.7427 0.027 Uiso 1 1 calc R A . C24 C -0.6719(5) 0.6692(2) -0.6981(4) 0.0238(12) Uani 1 1 d . A . C25 C -0.7454(5) 0.6859(2) -0.6414(4) 0.0252(13) Uani 1 1 d . . . H25 H -0.8119 0.6696 -0.6374 0.030 Uiso 1 1 calc R A . C26 C -0.7209(5) 0.7264(2) -0.5907(4) 0.0219(12) Uani 1 1 d . A . C27 C -0.8022(4) 0.7440(2) -0.5296(4) 0.0221(12) Uani 1 1 d . . . H27A H -0.8781 0.7363 -0.5557 0.027 Uiso 1 1 calc R A . H27B H -0.7966 0.7782 -0.5253 0.027 Uiso 1 1 calc R . . C28 C -0.7009(4) 0.74241(18) -0.3706(4) 0.0183(11) Uani 1 1 d . . . C29 C -0.7813(4) 0.72296(19) -0.4363(4) 0.0189(11) Uani 1 1 d . A . C30 C -0.8397(4) 0.6834(2) -0.4153(4) 0.0198(11) Uani 1 1 d . . . H30 H -0.8951 0.6706 -0.4571 0.024 Uiso 1 1 calc R A . C31 C -0.8162(4) 0.66227(19) -0.3321(4) 0.0202(11) Uani 1 1 d . A . C32 C -0.7342(4) 0.68087(19) -0.2694(4) 0.0189(11) Uani 1 1 d . . . H32 H -0.7182 0.6663 -0.2142 0.023 Uiso 1 1 calc R A . C33 C -0.6750(4) 0.72151(19) -0.2883(4) 0.0178(11) Uani 1 1 d . A . C34 C -0.5815(5) 0.7395(2) -0.2188(4) 0.0229(12) Uani 1 1 d . . . H34A H -0.6000 0.7322 -0.1599 0.028 Uiso 1 1 calc R A . H34B H -0.5760 0.7736 -0.2236 0.028 Uiso 1 1 calc R . . O1 O 0.0569(3) -0.00715(14) -0.1574(3) 0.0251(9) Uani 1 1 d . . . O2 O 0.1066(3) 0.08236(15) -0.0826(3) 0.0292(10) Uani 1 1 d . . . O3 O -0.0893(3) 0.07647(15) 0.0146(3) 0.0273(9) Uani 1 1 d . . . O4 O -0.2693(4) 0.62768(16) -0.0314(3) 0.0363(11) Uani 1 1 d . A . O5 O -0.3463(6) 0.5723(2) -0.1473(5) 0.0276(15) Uani 0.67 1 d P A 1 O6 O -0.1600(5) 0.6011(2) -0.1424(4) 0.0542(15) Uani 1 1 d . A . O7 O -0.1611(4) 0.62151(16) -0.7077(3) 0.0330(10) Uani 1 1 d . . . O8 O -0.0070(3) 0.64767(14) -0.6007(3) 0.0260(9) Uani 1 1 d . . . O9 O -0.1323(3) 0.58634(14) -0.5618(3) 0.0279(10) Uani 1 1 d . . . O10 O -0.6107(4) 0.60943(18) -0.8092(4) 0.0439(13) Uani 1 1 d . . . O11 O -0.8090(4) 0.62900(16) -0.8218(3) 0.0368(11) Uani 1 1 d . . . O12 O -0.7228(3) 0.58027(14) -0.7021(3) 0.0298(10) Uani 1 1 d . . . O13 O -1.0099(3) 0.62657(15) -0.3104(3) 0.0291(10) Uani 1 1 d . . . O14 O -0.8434(4) 0.59593(16) -0.2198(3) 0.0352(11) Uani 1 1 d . . . O15 O -0.8800(3) 0.57636(14) -0.3761(3) 0.0275(9) Uani 1 1 d . . . O16 O -0.4363(3) 0.77826(15) -0.3274(3) 0.0301(10) Uani 1 1 d . . . H16A H -0.3934 0.7862 -0.3625 0.045 Uiso 1 1 calc R . . O17 O -0.3584(4) 0.79056(16) -0.4826(3) 0.0323(10) Uani 1 1 d . A . H17 H -0.4065 0.7832 -0.4514 0.048 Uiso 1 1 calc R . . O18 O -0.5914(3) 0.79199(15) -0.5565(3) 0.0286(10) Uani 1 1 d . A . H18A H -0.6239 0.7939 -0.5124 0.043 Uiso 1 1 calc R . . O19 O -0.6516(3) 0.78405(13) -0.3920(3) 0.0241(9) Uani 1 1 d . A . H19 H -0.5866 0.7849 -0.3676 0.036 Uiso 1 1 calc R . . O20 O -0.9016(4) 0.48011(15) -0.7826(3) 0.0321(10) Uani 1 1 d . . . O21 O -0.6692(3) 0.48465(15) -0.7076(3) 0.0291(10) Uani 1 1 d . . . O22 O -0.9529(4) 0.57188(15) -0.7424(3) 0.0302(10) Uani 1 1 d . . . O23 O -1.0061(4) 0.50752(15) -0.6093(3) 0.0313(10) Uani 1 1 d . . . O24 O -0.6918(4) 0.50985(15) -0.5291(3) 0.0279(9) Uani 1 1 d . . . O25 O -0.8364(3) 0.43832(14) -0.6106(3) 0.0262(9) Uani 1 1 d . . . O26 O -0.8495(3) 0.58042(14) -0.5523(3) 0.0254(9) Uani 1 1 d . . . O100 O -0.5665(7) 0.1271(2) 0.5752(4) 0.076(2) Uani 1 1 d . . . O101 O -0.1589(16) 0.4490(9) 0.9658(10) 0.080(8) Uani 0.33 1 d P . . O102 O -0.3532(11) 0.3568(8) 0.0169(9) 0.109(7) Uani 0.50 1 d P . . O103 O -0.3252(10) 0.6310(6) 0.1390(7) 0.078(5) Uani 0.50 1 d P . . O104 O -0.9473(12) 0.3885(4) -0.0706(10) 0.077(5) Uani 0.50 1 d P . . O105 O -0.4891(17) 0.6994(8) -0.9119(14) 0.074(6) Uani 0.33 1 d P . . O106 O -0.240(3) 0.5773(8) 0.1304(14) 0.106(10) Uani 0.33 1 d P . . O107 O -1.0315(11) 0.5159(4) -0.9202(8) 0.060(3) Uiso 0.50 1 d P . . O200 O -0.302(2) 0.5163(9) 0.0531(18) 0.097(8) Uani 0.33 1 d P . 2 O201 O -0.600(3) 0.4666(8) -0.1098(14) 0.094(8) Uani 0.33 1 d P . 2 O202 O -0.4721(18) 0.5703(9) 0.0949(13) 0.075(6) Uani 0.33 1 d P . 2 O203 O -0.623(2) 0.5689(7) -0.0874(12) 0.075(7) Uani 0.33 1 d P . 2 O204 O -0.4760(15) 0.4452(5) 0.0538(12) 0.044(4) Uani 0.33 1 d P . 2 O205 O -0.6416(18) 0.5109(8) 0.0611(13) 0.049(5) Uani 0.33 1 d P . 2 O206 O -0.405(2) 0.5778(7) -0.0998(19) 0.091(9) Uani 0.33 1 d P . 2 O207 O -0.375(3) 0.4757(8) -0.1050(19) 0.078(9) Uani 0.33 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y2 0.0788(18) 0.0391(14) 0.0418(14) -0.0067(11) 0.0100(12) -0.0041(13) Y1 0.0142(3) 0.0117(2) 0.0257(3) -0.0032(2) 0.0001(2) 0.00006(19) S1 0.0637(12) 0.0245(8) 0.0332(10) -0.0127(7) -0.0120(8) 0.0198(8) S2 0.0174(6) 0.0168(6) 0.0215(7) -0.0028(5) 0.0022(5) -0.0013(5) S3 0.0308(8) 0.0153(7) 0.0371(9) 0.0041(6) 0.0098(7) 0.0012(6) S4 0.0194(6) 0.0159(6) 0.0271(8) -0.0008(5) 0.0057(6) -0.0050(5) C1 0.032(3) 0.017(3) 0.042(4) -0.004(3) -0.002(3) 0.000(2) C2 0.030(3) 0.026(3) 0.039(4) -0.004(3) 0.003(3) 0.011(3) C3 0.028(3) 0.022(3) 0.048(4) 0.012(3) 0.001(3) 0.004(2) C4 0.031(3) 0.019(3) 0.045(4) 0.007(3) 0.000(3) -0.008(2) C5 0.031(3) 0.023(3) 0.035(4) 0.012(3) -0.004(3) -0.010(3) C6 0.028(3) 0.047(4) 0.038(4) 0.006(3) 0.010(3) -0.010(3) C7 0.023(3) 0.025(3) 0.027(3) -0.007(3) -0.006(2) 0.004(2) C8 0.025(3) 0.019(3) 0.023(3) -0.008(2) -0.003(2) 0.004(2) C9 0.041(3) 0.021(3) 0.024(3) -0.009(2) -0.001(3) 0.003(3) C10 0.048(4) 0.026(3) 0.024(3) -0.015(3) -0.014(3) 0.015(3) C11 0.030(3) 0.037(4) 0.028(3) -0.018(3) -0.003(3) 0.012(3) C12 0.025(3) 0.040(4) 0.023(3) -0.015(3) -0.005(2) 0.004(3) C13 0.019(3) 0.044(4) 0.033(4) -0.015(3) -0.004(3) 0.005(3) C14 0.018(3) 0.018(3) 0.035(3) -0.004(2) 0.008(2) -0.003(2) C15 0.019(3) 0.026(3) 0.030(3) -0.007(3) 0.005(2) -0.004(2) C16 0.014(2) 0.025(3) 0.022(3) 0.001(2) 0.001(2) 0.000(2) C17 0.016(2) 0.018(3) 0.022(3) 0.000(2) 0.006(2) -0.002(2) C18 0.021(3) 0.019(3) 0.023(3) 0.002(2) 0.007(2) -0.002(2) C19 0.019(3) 0.019(3) 0.025(3) 0.005(2) 0.007(2) -0.001(2) C20 0.025(3) 0.018(3) 0.026(3) 0.010(2) 0.007(2) 0.004(2) C21 0.019(3) 0.020(3) 0.027(3) 0.008(2) -0.003(2) 0.004(2) C22 0.023(3) 0.019(3) 0.028(3) 0.012(2) -0.002(2) 0.004(2) C23 0.020(3) 0.016(3) 0.031(3) 0.009(2) 0.003(2) 0.006(2) C24 0.027(3) 0.017(3) 0.028(3) 0.006(2) 0.005(2) 0.002(2) C25 0.023(3) 0.015(3) 0.037(4) 0.008(2) 0.001(3) -0.001(2) C26 0.021(3) 0.017(3) 0.027(3) 0.009(2) 0.002(2) 0.004(2) C27 0.016(3) 0.020(3) 0.030(3) 0.005(2) 0.000(2) 0.003(2) C28 0.018(2) 0.010(2) 0.027(3) 0.000(2) 0.006(2) 0.0004(19) C29 0.014(2) 0.011(2) 0.031(3) 0.002(2) 0.004(2) 0.0053(19) C30 0.014(2) 0.019(3) 0.025(3) 0.000(2) -0.002(2) 0.001(2) C31 0.018(3) 0.015(3) 0.028(3) 0.000(2) 0.004(2) 0.001(2) C32 0.022(3) 0.015(3) 0.021(3) 0.000(2) 0.005(2) 0.001(2) C33 0.014(2) 0.014(2) 0.026(3) -0.008(2) 0.001(2) 0.0004(19) C34 0.024(3) 0.016(3) 0.029(3) -0.007(2) 0.003(2) -0.001(2) O1 0.0186(19) 0.016(2) 0.041(3) 0.0068(18) 0.0044(18) 0.0001(15) O2 0.024(2) 0.024(2) 0.039(3) 0.0043(19) 0.0015(19) 0.0000(17) O3 0.025(2) 0.020(2) 0.035(3) 0.0010(18) -0.0023(18) -0.0054(16) O4 0.058(3) 0.027(2) 0.024(2) -0.0011(19) 0.009(2) 0.007(2) O5 0.036(4) 0.015(3) 0.034(4) -0.004(3) 0.011(3) -0.004(3) O6 0.061(4) 0.041(3) 0.060(4) -0.010(3) 0.006(3) 0.018(3) O7 0.042(3) 0.035(3) 0.021(2) -0.0097(19) -0.0007(19) 0.007(2) O8 0.0179(19) 0.020(2) 0.041(3) -0.0032(18) 0.0052(18) -0.0024(16) O9 0.027(2) 0.017(2) 0.041(3) 0.0019(18) 0.0112(19) 0.0019(16) O10 0.044(3) 0.032(3) 0.062(3) -0.007(2) 0.031(3) -0.006(2) O11 0.047(3) 0.024(2) 0.036(3) 0.003(2) -0.006(2) 0.005(2) O12 0.027(2) 0.017(2) 0.046(3) 0.0070(19) 0.005(2) 0.0005(17) O13 0.021(2) 0.023(2) 0.045(3) -0.0061(19) 0.0124(19) -0.0028(17) O14 0.044(3) 0.029(2) 0.031(3) 0.009(2) 0.000(2) -0.016(2) O15 0.029(2) 0.016(2) 0.040(3) -0.0032(18) 0.0133(19) -0.0036(17) O16 0.025(2) 0.024(2) 0.043(3) 0.0020(19) 0.0093(19) -0.0005(18) O17 0.031(2) 0.027(2) 0.040(3) -0.011(2) 0.009(2) 0.0047(19) O18 0.026(2) 0.020(2) 0.041(3) 0.0016(19) 0.0065(19) -0.0022(17) O19 0.025(2) 0.0118(19) 0.035(2) 0.0008(17) 0.0009(18) -0.0060(16) O20 0.033(2) 0.027(2) 0.034(3) -0.0111(19) -0.0039(19) 0.0078(19) O21 0.020(2) 0.026(2) 0.041(3) -0.0081(19) 0.0059(19) 0.0017(17) O22 0.029(2) 0.025(2) 0.035(3) -0.0043(19) -0.0022(19) 0.0082(18) O23 0.025(2) 0.022(2) 0.049(3) -0.010(2) 0.016(2) -0.0034(17) O24 0.028(2) 0.021(2) 0.032(2) -0.0047(18) -0.0054(18) 0.0039(17) O25 0.024(2) 0.016(2) 0.037(3) 0.0013(18) 0.0009(18) -0.0020(16) O26 0.026(2) 0.015(2) 0.035(2) -0.0073(17) 0.0023(18) 0.0033(16) O100 0.122(6) 0.050(4) 0.062(4) 0.005(3) 0.034(4) -0.002(4) O101 0.069(12) 0.15(2) 0.019(8) 0.026(10) 0.016(8) 0.075(14) O102 0.056(8) 0.21(2) 0.063(9) -0.065(11) 0.023(7) 0.014(10) O103 0.054(7) 0.150(15) 0.027(6) 0.006(7) -0.004(5) -0.006(8) O104 0.084(9) 0.037(7) 0.092(10) 0.024(7) -0.051(8) -0.006(6) O105 0.077(13) 0.082(15) 0.073(13) 0.003(11) 0.043(11) -0.019(11) O106 0.19(3) 0.078(17) 0.043(12) -0.004(11) 0.001(14) 0.071(18) O200 0.11(2) 0.088(19) 0.091(18) -0.013(14) 0.005(15) -0.012(15) O201 0.17(3) 0.064(14) 0.048(12) -0.037(11) -0.010(14) 0.021(16) O202 0.081(14) 0.091(17) 0.059(12) -0.037(11) 0.027(11) -0.009(12) O203 0.14(2) 0.054(12) 0.031(10) -0.011(9) 0.017(11) -0.011(13) O204 0.052(10) 0.026(8) 0.063(11) -0.007(8) 0.035(9) 0.000(7) O205 0.068(12) 0.048(13) 0.031(10) 0.016(9) 0.002(10) 0.012(10) O206 0.099(18) 0.035(11) 0.12(2) 0.035(13) -0.053(16) -0.039(12) O207 0.13(2) 0.039(12) 0.082(19) -0.017(12) 0.051(18) -0.018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y2 Y2 1.210(5) 3_465 ? Y2 O204 1.238(17) 3_465 ? Y2 O205 1.91(2) 3_465 ? Y2 O201 2.14(2) 3_465 ? Y2 O202 2.279(19) . ? Y2 O201 2.30(2) . ? Y2 O207 2.31(2) . ? Y2 O204 2.315(17) . ? Y2 O203 2.33(3) . ? Y2 O200 2.34(3) . ? Y2 O205 2.37(2) . ? Y2 O206 2.38(2) . ? Y1 O12 2.308(4) . ? Y1 O20 2.324(4) . ? Y1 O24 2.340(4) . ? Y1 O26 2.350(4) . ? Y1 O23 2.361(4) . ? Y1 O21 2.373(4) . ? Y1 O25 2.383(4) . ? Y1 O22 2.405(4) . ? S1 O5 1.401(7) . ? S1 O4 1.429(5) . ? S1 O6 1.511(6) . ? S1 C10 1.751(7) . ? S1 O206 1.87(2) . ? S2 O7 1.448(4) . ? S2 O8 1.457(4) . ? S2 O9 1.464(4) . ? S2 C17 1.765(5) . ? S3 O10 1.440(5) . ? S3 O11 1.450(5) . ? S3 O12 1.464(4) . ? S3 C24 1.754(6) . ? S4 O14 1.455(5) . ? S4 O13 1.457(4) . ? S4 O15 1.468(4) . ? S4 C31 1.770(6) . ? C1 O3 1.419(8) . ? C1 C2 1.490(9) 3 ? C2 O1 1.443(7) . ? C2 C1 1.490(10) 3 ? C3 O3 1.411(7) . ? C3 C4 1.518(9) . ? C4 O2 1.415(8) . ? C5 O2 1.424(8) . ? C5 C6 1.493(10) . ? C6 O1 1.426(7) . ? C7 O16 1.368(7) . ? C7 C8 1.387(9) . ? C7 C12 1.409(8) . ? C8 C9 1.386(9) . ? C8 C34 1.526(8) . ? C9 C10 1.392(9) . ? C10 C11 1.392(10) . ? C11 C12 1.388(10) . ? C12 C13 1.525(10) . ? C13 C15 1.509(9) . ? C14 C19 1.381(8) . ? C14 O17 1.386(7) . ? C14 C15 1.392(9) . ? C15 C16 1.386(8) . ? C16 C17 1.389(8) . ? C17 C18 1.373(8) . ? C18 C19 1.389(8) . ? C19 C20 1.525(8) . ? C20 C22 1.524(8) . ? C21 O18 1.369(7) . ? C21 C22 1.394(9) . ? C21 C26 1.411(8) . ? C22 C23 1.383(9) . ? C23 C24 1.380(8) . ? C24 C25 1.394(8) . ? C25 C26 1.389(8) . ? C26 C27 1.517(8) . ? C27 C29 1.526(8) . ? C28 O19 1.375(6) . ? C28 C33 1.378(8) . ? C28 C29 1.407(8) . ? C29 C30 1.379(8) . ? C30 C31 1.391(8) . ? C31 C32 1.381(8) . ? C32 C33 1.400(7) . ? C33 C34 1.525(8) . ? O200 O201 1.62(4) 3_465 ? O200 Y2 2.70(3) 3_465 ? O201 O202 1.36(3) 3_465 ? O201 O200 1.62(4) 3_465 ? O201 Y2 2.14(2) 3_465 ? O202 O201 1.36(3) 3_465 ? O202 Y2 2.75(2) 3_465 ? O203 O204 1.29(3) 3_465 ? O204 Y2 1.238(17) 3_465 ? O204 O203 1.29(3) 3_465 ? O204 O206 1.80(3) 3_465 ? O205 O207 0.77(2) 3_465 ? O205 Y2 1.91(2) 3_465 ? O206 O204 1.80(3) 3_465 ? O207 O205 0.77(2) 3_465 ? O207 Y2 2.68(2) 3_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Y2 Y2 O204 142.1(8) 3_465 3_465 ? Y2 Y2 O205 96.0(7) 3_465 3_465 ? O204 Y2 O205 118.8(9) 3_465 3_465 ? Y2 Y2 O201 81.7(8) 3_465 3_465 ? O204 Y2 O201 108.2(10) 3_465 3_465 ? O205 Y2 O201 94.4(10) 3_465 3_465 ? Y2 Y2 O202 99.2(7) 3_465 . ? O204 Y2 O202 75.4(10) 3_465 . ? O205 Y2 O202 122.8(9) 3_465 . ? O201 Y2 O202 35.5(8) 3_465 . ? Y2 Y2 O201 67.0(7) 3_465 . ? O204 Y2 O201 97.1(11) 3_465 . ? O205 Y2 O201 89.1(10) 3_465 . ? O201 Y2 O201 148.7(3) 3_465 . ? O202 Y2 O201 147.2(9) . . ? Y2 Y2 O207 94.3(7) 3_465 . ? O204 Y2 O207 113.9(10) 3_465 . ? O205 Y2 O207 18.2(9) 3_465 . ? O201 Y2 O207 112.1(11) 3_465 . ? O202 Y2 O207 140.5(10) . . ? O201 Y2 O207 71.9(10) . . ? Y2 Y2 O204 19.2(5) 3_465 . ? O204 Y2 O204 161.3(4) 3_465 . ? O205 Y2 O204 78.3(7) 3_465 . ? O201 Y2 O204 76.0(8) 3_465 . ? O202 Y2 O204 102.6(8) . . ? O201 Y2 O204 74.3(8) . . ? O207 Y2 O204 79.8(7) . . ? Y2 Y2 O203 120.1(6) 3_465 . ? O204 Y2 O203 23.5(9) 3_465 . ? O205 Y2 O203 131.6(7) 3_465 . ? O201 Y2 O203 120.1(8) 3_465 . ? O202 Y2 O203 84.6(8) . . ? O201 Y2 O203 78.3(8) . . ? O207 Y2 O203 119.7(9) . . ? O204 Y2 O203 138.8(7) . . ? Y2 Y2 O200 93.5(7) 3_465 . ? O204 Y2 O200 118.7(10) 3_465 . ? O205 Y2 O200 53.0(9) 3_465 . ? O201 Y2 O200 42.0(10) 3_465 . ? O202 Y2 O200 71.2(9) . . ? O201 Y2 O200 136.3(9) . . ? O207 Y2 O200 71.1(10) . . ? O204 Y2 O200 77.0(8) . . ? O203 Y2 O200 141.6(8) . . ? Y2 Y2 O205 53.5(5) 3_465 . ? O204 Y2 O205 90.8(8) 3_465 . ? O205 Y2 O205 149.4(4) 3_465 . ? O201 Y2 O205 82.2(10) 3_465 . ? O202 Y2 O205 69.2(8) . . ? O201 Y2 O205 79.2(9) . . ? O207 Y2 O205 143.7(9) . . ? O204 Y2 O205 71.4(6) . . ? O203 Y2 O205 73.7(7) . . ? O200 Y2 O205 121.2(8) . . ? Y2 Y2 O206 170.1(8) 3_465 . ? O204 Y2 O206 47.5(10) 3_465 . ? O205 Y2 O206 74.1(10) 3_465 . ? O201 Y2 O206 97.8(10) 3_465 . ? O202 Y2 O206 85.7(9) . . ? O201 Y2 O206 113.1(9) . . ? O207 Y2 O206 76.6(10) . . ? O204 Y2 O206 151.2(8) . . ? O203 Y2 O206 68.8(8) . . ? O200 Y2 O206 79.8(8) . . ? O205 Y2 O206 136.4(9) . . ? O12 Y1 O20 104.59(17) . . ? O12 Y1 O24 89.62(16) . . ? O20 Y1 O24 140.97(15) . . ? O12 Y1 O26 76.90(15) . . ? O20 Y1 O26 146.63(15) . . ? O24 Y1 O26 71.56(14) . . ? O12 Y1 O23 138.49(15) . . ? O20 Y1 O23 84.67(16) . . ? O24 Y1 O23 108.56(16) . . ? O26 Y1 O23 74.34(14) . . ? O12 Y1 O21 72.86(15) . . ? O20 Y1 O21 75.56(15) . . ? O24 Y1 O21 74.33(15) . . ? O26 Y1 O21 133.96(14) . . ? O23 Y1 O21 147.18(15) . . ? O12 Y1 O25 148.31(14) . . ? O20 Y1 O25 75.38(16) . . ? O24 Y1 O25 73.95(15) . . ? O26 Y1 O25 120.84(15) . . ? O23 Y1 O25 73.15(15) . . ? O21 Y1 O25 76.62(15) . . ? O12 Y1 O22 71.78(15) . . ? O20 Y1 O22 71.12(15) . . ? O24 Y1 O22 147.38(15) . . ? O26 Y1 O22 78.11(15) . . ? O23 Y1 O22 73.48(16) . . ? O21 Y1 O22 122.23(16) . . ? O25 Y1 O22 134.19(15) . . ? O5 S1 O4 119.3(4) . . ? O5 S1 O6 109.2(4) . . ? O4 S1 O6 108.6(3) . . ? O5 S1 C10 105.4(4) . . ? O4 S1 C10 107.8(3) . . ? O6 S1 C10 105.7(4) . . ? O5 S1 O206 35.2(9) . . ? O4 S1 O206 87.4(9) . . ? O6 S1 O206 138.9(9) . . ? C10 S1 O206 104.6(7) . . ? O7 S2 O8 112.3(3) . . ? O7 S2 O9 111.6(3) . . ? O8 S2 O9 111.8(3) . . ? O7 S2 C17 107.7(3) . . ? O8 S2 C17 105.1(2) . . ? O9 S2 C17 107.9(2) . . ? O10 S3 O11 114.5(3) . . ? O10 S3 O12 110.7(3) . . ? O11 S3 O12 111.1(3) . . ? O10 S3 C24 106.1(3) . . ? O11 S3 C24 107.6(3) . . ? O12 S3 C24 106.4(3) . . ? O14 S4 O13 113.5(3) . . ? O14 S4 O15 111.6(3) . . ? O13 S4 O15 111.6(3) . . ? O14 S4 C31 105.9(3) . . ? O13 S4 C31 106.9(3) . . ? O15 S4 C31 106.8(3) . . ? O3 C1 C2 110.1(5) . 3 ? O1 C2 C1 109.0(5) . 3 ? O3 C3 C4 114.8(5) . . ? O2 C4 C3 113.1(5) . . ? O2 C5 C6 107.4(5) . . ? O1 C6 C5 109.2(5) . . ? O16 C7 C8 115.8(5) . . ? O16 C7 C12 121.3(6) . . ? C8 C7 C12 122.8(6) . . ? C9 C8 C7 118.6(5) . . ? C9 C8 C34 120.1(6) . . ? C7 C8 C34 121.3(5) . . ? C8 C9 C10 119.9(6) . . ? C11 C10 C9 120.8(6) . . ? C11 C10 S1 120.0(5) . . ? C9 C10 S1 118.9(6) . . ? C12 C11 C10 120.7(6) . . ? C11 C12 C7 117.2(6) . . ? C11 C12 C13 119.5(6) . . ? C7 C12 C13 123.2(6) . . ? C15 C13 C12 114.7(5) . . ? C19 C14 O17 121.7(5) . . ? C19 C14 C15 122.8(5) . . ? O17 C14 C15 115.5(5) . . ? C16 C15 C14 118.0(5) . . ? C16 C15 C13 120.7(6) . . ? C14 C15 C13 121.2(5) . . ? C15 C16 C17 120.0(5) . . ? C18 C17 C16 120.4(5) . . ? C18 C17 S2 121.1(4) . . ? C16 C17 S2 118.3(4) . . ? C17 C18 C19 121.1(5) . . ? C14 C19 C18 117.5(5) . . ? C14 C19 C20 122.8(5) . . ? C18 C19 C20 119.6(5) . . ? C22 C20 C19 109.8(4) . . ? O18 C21 C22 116.2(5) . . ? O18 C21 C26 122.0(5) . . ? C22 C21 C26 121.8(6) . . ? C23 C22 C21 118.6(5) . . ? C23 C22 C20 119.1(5) . . ? C21 C22 C20 122.3(5) . . ? C24 C23 C22 121.0(6) . . ? C23 C24 C25 120.0(6) . . ? C23 C24 S3 119.7(5) . . ? C25 C24 S3 120.2(5) . . ? C26 C25 C24 121.0(5) . . ? C25 C26 C21 117.6(5) . . ? C25 C26 C27 120.1(5) . . ? C21 C26 C27 122.3(5) . . ? C26 C27 C29 113.4(4) . . ? O19 C28 C33 121.8(5) . . ? O19 C28 C29 116.3(5) . . ? C33 C28 C29 121.8(5) . . ? C30 C29 C28 118.4(5) . . ? C30 C29 C27 120.2(5) . . ? C28 C29 C27 121.3(5) . . ? C29 C30 C31 120.5(5) . . ? C32 C31 C30 120.3(5) . . ? C32 C31 S4 120.6(4) . . ? C30 C31 S4 119.2(4) . . ? C31 C32 C33 120.5(5) . . ? C28 C33 C32 118.4(5) . . ? C28 C33 C34 122.8(5) . . ? C32 C33 C34 118.6(5) . . ? C33 C34 C8 112.0(5) . . ? C6 O1 C2 111.6(5) . . ? C4 O2 C5 112.4(5) . . ? C3 O3 C1 112.7(5) . . ? S3 O12 Y1 152.1(3) . . ? O201 O200 Y2 62.5(12) 3_465 . ? O201 O200 Y2 58.3(12) 3_465 3_465 ? Y2 O200 Y2 26.6(3) . 3_465 ? O202 O201 O200 129(2) 3_465 3_465 ? O202 O201 Y2 77.7(14) 3_465 3_465 ? O200 O201 Y2 75.5(12) 3_465 3_465 ? O202 O201 Y2 93.6(16) 3_465 . ? O200 O201 Y2 85.0(12) 3_465 . ? Y2 O201 Y2 31.3(3) 3_465 . ? O201 O202 Y2 66.7(11) 3_465 . ? O201 O202 Y2 56.8(13) 3_465 3_465 ? Y2 O202 Y2 25.8(3) . 3_465 ? O204 O203 Y2 22.4(8) 3_465 . ? Y2 O204 O203 134.1(16) 3_465 3_465 ? Y2 O204 O206 101.9(12) 3_465 3_465 ? O203 O204 O206 118.3(16) 3_465 3_465 ? Y2 O204 Y2 18.7(4) 3_465 . ? O203 O204 Y2 116.7(13) 3_465 . ? O206 O204 Y2 120.6(11) 3_465 . ? O207 O205 Y2 111(3) 3_465 3_465 ? O207 O205 Y2 106(3) 3_465 . ? Y2 O205 Y2 30.6(4) 3_465 . ? O204 O206 S1 165.2(19) 3_465 . ? O204 O206 Y2 30.6(7) 3_465 . ? S1 O206 Y2 148.5(11) . . ? O205 O207 Y2 51(3) 3_465 . ? O205 O207 Y2 58(3) 3_465 3_465 ? Y2 O207 Y2 26.7(3) . 3_465 ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 2.255 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.224