# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- Revised_C2DT12227H_ccdc_854826_854828_cif.txt' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Josef Hamacek' ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; 'Soumaila Zebret' ; Department of Physical Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; 'Nathalie Dupont' ; Laboratory of X-ray Crystallography University of Geneva 24, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; C.Besnard ; Laboratory of X-ray Crystallography University of Geneva 24, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; 'Gerald Bernardinelli' ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; _publ_contact_author ; Dr Josef Hamacek Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; _publ_contact_author_email Josef.Hamacek@unige.ch _publ_contact_author_fax '41 22 379 68 30' _publ_contact_author_phone '41 22 379 64 13' _publ_contact_author_name 'Dr Josef Hamacek' # Attachment '- erbe2-com.cif' data_erbe2 _database_code_depnum_ccdc_archive 'CCDC 854826' #TrackingRef '- erbe2-com.cif' #-------------------------------------------------------------------- _audit_creation_date 2008-03-07 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2008-03-07 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 _chemical_formula_moiety 'C16 H13 N3 O6' _chemical_formula_sum 'C16 H13 N3 O6' _chemical_formula_weight 343.3 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 7.1099(4) _cell_length_b 18.8042(11) _cell_length_c 11.6038(7) _cell_angle_alpha 90.00000 _cell_angle_beta 98.278(7) _cell_angle_gamma 90.00000 _cell_volume 1535.22(16) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_meas not_measured _diffrn_ambient_temperature 150 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 26.9 _cell_measurement_temperature 150 _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu .116 _exptl_crystal_description prism _exptl_crystal_size_max .276 _exptl_crystal_size_mid .221 _exptl_crystal_size_min .106 _exptl_crystal_colour colorless _diffrn_measurement_device_type 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_absorpt_correction_T_min .974 _exptl_absorpt_correction_T_max .9893 _diffrn_reflns_number 14'164 _reflns_number_total 3301 _reflns_number_gt 1889 _reflns_threshold_expression 'refl observed if Fo > 2.99 \s(Fo)' _diffrn_reflns_theta_max 26.9 _diffrn_reflns_theta_full 26.9 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .06 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .030 _refine_ls_wR_factor_ref .029 _refine_ls_goodness_of_fit_ref 1.22(2) _refine_ls_number_reflns 1838 _refine_ls_number_parameters 229 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.00015(Fo^2^)] _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .00026 _refine_diff_density_max .573 _refine_diff_density_min -.579 _refine_ls_extinction_method none _refine_ls_abs_structure_details none _computing_data_collection 'EXPOSE (Stoe & Cie, 1999)' _computing_cell_refinement 'CELL (Stoe & Cie, 1999)' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution SIR97 _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal_gx3 _computing_publication_material xtal_CIFIO loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002 H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0 N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type O1 .1747(3) .47581(8) .07686(12) .0381(9) 1.00000 Uani O2 .1265(3) .41214(7) .23296(11) .0357(8) 1.00000 Uani O3 .2002(3) .10557(8) .05466(12) .0433(9) 1.00000 Uani O4 .3902(3) .05663(7) .26690(13) .0429(9) 1.00000 Uani O5 .7464(3) .34468(7) .61838(11) .0344(8) 1.00000 Uani O6 .6338(3) .35422(7) .42824(11) .0324(8) 1.00000 Uani N1 .1794(3) .29086(8) .10682(12) .0234(9) 1.00000 Uani N2 .3360(3) .17290(9) .20967(13) .0253(9) 1.00000 Uani N3 .5444(3) .21736(8) .41005(13) .0225(9) 1.00000 Uani C1 .1196(3) .35152(10) .05333(16) .0241(10) 1.00000 Uani C2 .0363(3) .35545(11) -.06265(16) .0280(11) 1.00000 Uani C3 .0132(3) .29338(12) -.12735(16) .0302(11) 1.00000 Uani C4 .0764(3) .22996(11) -.07454(16) .0291(11) 1.00000 Uani C5 .1585(3) .23132(10) .04199(15) .0247(10) 1.00000 Uani C6 .2310(3) .16320(11) .10063(16) .0278(11) 1.00000 Uani C7 .4100(3) .11982(10) .28605(17) .0284(11) 1.00000 Uani C8 .5131(3) .14721(10) .39983(16) .0241(10) 1.00000 Uani C9 .5668(3) .09887(11) .48893(18) .0310(11) 1.00000 Uani C10 .6482(4) .12395(11) .59637(18) .0321(12) 1.00000 Uani C11 .6784(3) .19631(11) .60986(16) .0292(11) 1.00000 Uani C12 .6296(3) .24065(10) .51421(15) .0232(10) 1.00000 Uani C13 .1453(3) .42013(10) .12167(16) .0257(11) 1.00000 Uani C14 .1438(4) .47782(11) .30042(17) .0443(13) 1.00000 Uani C15 .6763(3) .31852(10) .52735(16) .0241(10) 1.00000 Uani C16 .6753(4) .43009(11) .43786(18) .0423(13) 1.00000 Uani H02 .355(4) .2174(13) .2343(18) .04000 1.00000 Uiso H2 -.00525 .40128 -.09796 .04000 1.00000 Uiso H3 -.04681 .29419 -.20886 .04000 1.00000 Uiso H4 .06397 .18519 -.11819 .04000 1.00000 Uiso H9 .54749 .04768 .47570 .04000 1.00000 Uiso H10 .68367 .09121 .66170 .04000 1.00000 Uiso H11 .73345 .21609 .68550 .04000 1.00000 Uiso H141 .25462 .50369 .28517 .04000 1.00000 Uiso H142 .02710 .50750 .27760 .04000 1.00000 Uiso H143 .15537 .46626 .38297 .04000 1.00000 Uiso H161 .60312 .45180 .49580 .04000 1.00000 Uiso H162 .81417 .43690 .46270 .04000 1.00000 Uiso H163 .63843 .45192 .36259 .04000 1.00000 Uiso 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 O1 .0531(12) .0286(8) .0323(8) -.0067(8) .0052(7) .0053(7) O2 .0617(11) .0218(7) .0231(8) -.0053(7) .0045(7) -.0001(6) O3 .0586(12) .0303(9) .0380(9) -.0025(8) -.0029(8) -.0134(7) O4 .0542(11) .0193(8) .0518(10) .0003(8) -.0037(8) -.0075(7) O5 .0432(10) .0324(8) .0255(8) -.0044(7) -.0026(7) -.0056(6) O6 .0481(10) .0198(7) .0266(8) .0009(7) -.0034(7) -.0014(6) N1 .0224(10) .0250(9) .0228(8) -.0026(8) .0029(7) -.0018(7) N2 .0269(10) .0201(9) .0282(9) -.0013(8) .0019(8) -.0067(7) N3 .0207(10) .0204(9) .0260(9) .0023(7) .0025(7) -.0021(7) C1 .0194(11) .0281(11) .0253(10) -.0047(9) .0046(8) -.0004(8) C2 .0238(12) .0350(12) .0253(10) -.0036(10) .0037(9) .0043(9) C3 .0258(13) .0443(13) .0206(10) -.0071(10) .0032(9) -.0026(9) C4 .0253(12) .0367(12) .0259(11) -.0073(10) .0053(9) -.0076(9) C5 .0203(11) .0293(11) .0252(10) -.0047(9) .0059(9) -.0054(8) C6 .0266(12) .0315(12) .0261(11) -.0046(10) .0069(9) -.0085(9) C7 .0253(12) .0239(12) .0367(11) .0019(9) .0069(9) -.0039(9) C8 .0200(11) .0195(11) .0331(11) .0011(9) .0049(9) -.0012(8) C9 .0280(13) .0221(10) .0435(13) .0014(9) .0069(10) .0051(9) C10 .0269(13) .0329(12) .0355(12) .0012(10) .0011(10) .0131(9) C11 .0225(12) .0349(12) .0289(11) .0013(10) -.0008(9) .0040(9) C12 .0184(11) .0258(11) .0253(10) .0020(9) .0024(8) -.0009(8) C13 .0264(12) .0256(11) .0240(10) -.0009(9) -.0002(8) .0031(9) C14 .078(2) .0266(11) .0274(11) -.0088(12) .0058(12) -.0047(9) C15 .0219(12) .0273(11) .0233(10) .0007(9) .0036(9) -.0024(9) C16 .0688(18) .0193(11) .0362(12) -.0017(11) -.0018(12) -.0006(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance O1 C13 . . 1.201(3) O2 C13 . . 1.326(3) O2 C14 . . 1.458(3) O3 C6 . . 1.214(3) O4 C7 . . 1.213(3) O5 C15 . . 1.206(3) O6 C15 . . 1.328(3) O6 C16 . . 1.458(3) N1 C1 . . 1.338(3) N1 C5 . . 1.345(3) N2 C6 . . 1.385(3) N2 C7 . . 1.387(3) N2 H02 . . .89(3) N3 C8 . . 1.340(3) N3 C12 . . 1.345(3) C1 C2 . . 1.392(3) C1 C13 . . 1.512(3) C2 C3 . . 1.385(3) C3 C4 . . 1.386(3) C4 C5 . . 1.394(3) C5 C6 . . 1.506(3) C7 C8 . . 1.505(3) C8 C9 . . 1.388(3) C9 C10 . . 1.380(3) C10 C11 . . 1.383(3) C11 C12 . . 1.392(3) C12 C15 . . 1.504(3) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle C13 O2 C14 . . . 114.49(15) C15 O6 C16 . . . 114.21(14) C1 N1 C5 . . . 116.62(15) C6 N2 C7 . . . 126.42(16) C6 N2 H02 . . . 117.1(13) C7 N2 H02 . . . 116.4(13) C8 N3 C12 . . . 116.60(15) N1 C1 C2 . . . 123.79(17) N1 C1 C13 . . . 118.55(15) C2 C1 C13 . . . 117.66(17) C1 C2 C3 . . . 118.69(18) C2 C3 C4 . . . 118.69(16) C3 C4 C5 . . . 118.49(17) N1 C5 C4 . . . 123.71(17) N1 C5 C6 . . . 116.89(15) C4 C5 C6 . . . 119.40(17) O3 C6 N2 . . . 123.93(17) O3 C6 C5 . . . 122.18(16) N2 C6 C5 . . . 113.89(16) O4 C7 N2 . . . 124.35(18) O4 C7 C8 . . . 121.64(17) N2 C7 C8 . . . 113.96(16) N3 C8 C7 . . . 117.91(16) N3 C8 C9 . . . 123.65(17) C7 C8 C9 . . . 118.43(16) C8 C9 C10 . . . 118.93(18) C9 C10 C11 . . . 118.47(18) C10 C11 C12 . . . 118.84(17) N3 C12 C11 . . . 123.37(16) N3 C12 C15 . . . 118.18(15) C11 C12 C15 . . . 118.44(16) O1 C13 O2 . . . 124.67(17) O1 C13 C1 . . . 122.17(17) O2 C13 C1 . . . 113.13(16) O5 C15 O6 . . . 124.46(16) O5 C15 C12 . . . 122.90(17) O6 C15 C12 . . . 112.64(15) 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion C14 O2 C13 O1 . . . . .2(3) C14 O2 C13 C1 . . . . -177.93(17) C16 O6 C15 O5 . . . . -1.3(3) C16 O6 C15 C12 . . . . 179.39(18) C5 N1 C1 C2 . . . . 1.1(3) C5 N1 C1 C13 . . . . -178.27(18) C1 N1 C5 C4 . . . . -1.2(3) C1 N1 C5 C6 . . . . 178.15(18) C7 N2 C6 O3 . . . . -4.8(4) C7 N2 C6 C5 . . . . 175.85(19) H02 N2 C6 O3 . . . . 177.0(17) H02 N2 C6 C5 . . . . -2.3(17) C6 N2 C7 O4 . . . . -.7(4) C6 N2 C7 C8 . . . . -178.28(19) H02 N2 C7 O4 . . . . 177.5(17) H02 N2 C7 C8 . . . . -.1(17) C12 N3 C8 C7 . . . . 177.28(18) C12 N3 C8 C9 . . . . -1.4(3) C8 N3 C12 C11 . . . . -2.3(3) C8 N3 C12 C15 . . . . 176.94(18) N1 C1 C2 C3 . . . . -.1(4) C13 C1 C2 C3 . . . . 179.30(19) N1 C1 C13 O1 . . . . 147.4(2) N1 C1 C13 O2 . . . . -34.4(3) C2 C1 C13 O1 . . . . -32.0(3) C2 C1 C13 O2 . . . . 146.19(19) C1 C2 C3 C4 . . . . -.9(4) C2 C3 C4 C5 . . . . .8(4) C3 C4 C5 N1 . . . . .3(4) C3 C4 C5 C6 . . . . -179.04(19) N1 C5 C6 O3 . . . . 171.5(2) N1 C5 C6 N2 . . . . -9.2(3) C4 C5 C6 O3 . . . . -9.2(4) C4 C5 C6 N2 . . . . 170.20(19) O4 C7 C8 N3 . . . . 173.8(2) O4 C7 C8 C9 . . . . -7.4(4) N2 C7 C8 N3 . . . . -8.5(3) N2 C7 C8 C9 . . . . 170.21(19) N3 C8 C9 C10 . . . . 3.6(4) C7 C8 C9 C10 . . . . -175.1(2) C8 C9 C10 C11 . . . . -2.0(4) C9 C10 C11 C12 . . . . -1.4(4) C10 C11 C12 N3 . . . . 3.7(4) C10 C11 C12 C15 . . . . -175.54(19) N3 C12 C15 O5 . . . . 177.32(19) N3 C12 C15 O6 . . . . -3.4(3) C11 C12 C15 O5 . . . . -3.4(4) C11 C12 C15 O6 . . . . 175.91(18) #=END====================================================== data_test1 _database_code_depnum_ccdc_archive 'CCDC 854827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H36 Eu3 F18 N9 O36 S6, 4.65(C2 H3 N) ' _chemical_formula_sum 'C63.30 H49.95 Eu3 F18 N13.65 O36 S6' _chemical_formula_weight 2568.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' '-x+1/2, -y+1/2, z+1' 'x+1/2, y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' '-x+1, -y, z+1' 'x+1/2, y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' '-x+1, -y+1/2, z+1/2' _cell_length_a 55.860(11) _cell_length_b 18.930(6) _cell_length_c 38.762(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 40988(18) _cell_formula_units_Z 16 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 7023 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 29.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 20164 _exptl_absorpt_coefficient_mu 2.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; XDS, Kabsch, W. J. Appl. Cryst. 26, 795-800 (1993) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25011 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 74 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 28.29 _reflns_number_total 25011 _reflns_number_gt 23102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement ; XDS, Kabsch, W. J. Appl. Cryst. 26, 795-800 (1993) ; _computing_data_reduction ; XDS, Kabsch, W. J. Appl. Cryst. 26, 795-800 (1993) ; _computing_structure_solution ; Superflip ,Palatinus L., Chapuis G. (2007): J. Appl. Cryst. 40, 786 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Among the 6 triflate molecules, two are disordered. One was refine with two components, sharing an oxygen atom (O135), using restrains on the distances and anisotropic displacement parameters. The occupancies of each group were refined, their sum being constrained to one. The second one (containing S991 and S201) was refined using two components that were regularized and refined as rigid body. For this position, the description of the disorder is not optimal, as shown by the small density peaks still present in the last difference Fourier map and the strong restrains and constrains (eadp on F and O atoms) that had to be applied to the displacement parameters in order to get the refinement to converge. The occupancies were first refined with fixed displacement parameters and then blocked to the value they converged to. The occupancy of the acetonitrile solvent molecules were first refine with isotropic displacement parameters fixed to 0.05. Then, the occupancies were fixed and the anisotropic displacement parameters were refined. Restrains were applied on distances and anisotropic displacement parameters (similarity restrains). Not all the solvent molecules have been found, there are still small voids in the structure and some remaining density can be attributed to acetonitrile molecule with very weak occupancies. These were not included in the final model as they did not improve the quality of the fit significantly and their geometry tended to be unstable. 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^)+(0.0792P)^2^+141.9634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.046(8) _refine_ls_number_reflns 25011 _refine_ls_number_parameters 1397 _refine_ls_number_restraints 520 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.395951(4) 0.501560(13) 0.573172(7) 0.02419(5) Uani 1 1 d . H . C14C C 0.35479(9) 0.6091(3) 0.61250(14) 0.0282(10) Uani 1 1 d . J . O15C O 0.37337(7) 0.5997(2) 0.59624(10) 0.0290(7) Uani 1 1 d . . . N13C N 0.33910(8) 0.5601(2) 0.62442(12) 0.0289(8) Uani 1 1 d . J . Eu2 Eu 0.297547(4) 0.593455(14) 0.644798(7) 0.03016(6) Uani 1 1 d . . . O4C O 0.27311(8) 0.5280(2) 0.68858(12) 0.0393(9) Uani 1 1 d D J . C3C C 0.27967(11) 0.4717(3) 0.70054(17) 0.0390(13) Uani 1 1 d . . . O2C O 0.26897(9) 0.4389(3) 0.72583(13) 0.0479(12) Uani 1 1 d . J . C1C C 0.24810(14) 0.4735(5) 0.7400(2) 0.0562(19) Uani 1 1 d . . . H1CA H 0.2522 0.5214 0.7457 0.084 Uiso 1 1 d R J . H1CB H 0.2429 0.4493 0.7604 0.084 Uiso 1 1 d R . . H1CC H 0.2354 0.4734 0.7233 0.084 Uiso 1 1 d R . . C5C C 0.30176(10) 0.4355(3) 0.68824(17) 0.0371(12) Uani 1 1 d . J . N10C N 0.31345(8) 0.4733(3) 0.66381(13) 0.0324(9) Uani 1 1 d . J . C9C C 0.33328(9) 0.4459(3) 0.65012(16) 0.0326(11) Uani 1 1 d . . . C11C C 0.34626(9) 0.4919(3) 0.62461(14) 0.0285(10) Uani 1 1 d . J . O12C O 0.36243(7) 0.4637(2) 0.60727(10) 0.0298(7) Uani 1 1 d . . . C8C C 0.34259(10) 0.3815(3) 0.66032(19) 0.0406(13) Uani 1 1 d . J . H8C H 0.3568 0.3643 0.6504 0.049 Uiso 1 1 calc R . . C7C C 0.33060(12) 0.3426(3) 0.68540(18) 0.0421(14) Uani 1 1 d . . . H7C H 0.3366 0.2987 0.6928 0.050 Uiso 1 1 calc R J . C6C C 0.30965(11) 0.3699(3) 0.69933(18) 0.0418(14) Uani 1 1 d . J . H6C H 0.3010 0.3443 0.7160 0.050 Uiso 1 1 calc R . . O23C O 0.28434(8) 0.7110(3) 0.66523(13) 0.0422(10) Uani 1 1 d . J . C22C C 0.29787(11) 0.7610(4) 0.66703(17) 0.0407(13) Uani 1 1 d . . . O24C O 0.29379(9) 0.8211(3) 0.68221(17) 0.0618(16) Uani 1 1 d . J . C25C C 0.27068(14) 0.8256(6) 0.7003(3) 0.067(3) Uani 1 1 d . . . H25A H 0.2579 0.8128 0.6849 0.101 Uiso 1 1 d R J . H25B H 0.2683 0.8732 0.7082 0.101 Uiso 1 1 d R . . H25C H 0.2707 0.7941 0.7197 0.101 Uiso 1 1 d R . . C20C C 0.32210(10) 0.7577(3) 0.64897(16) 0.0355(11) Uani 1 1 d . J . N21C N 0.32770(8) 0.6932(3) 0.63848(12) 0.0309(9) Uani 1 1 d . J . C16C C 0.34870(10) 0.6837(3) 0.62271(15) 0.0316(10) Uani 1 1 d . . . C17C C 0.36473(11) 0.7383(3) 0.61708(17) 0.0366(12) Uani 1 1 d . J . H17C H 0.3793 0.7303 0.6057 0.044 Uiso 1 1 calc R . . C18C C 0.35854(13) 0.8054(4) 0.6288(2) 0.0515(18) Uani 1 1 d . . . H18C H 0.3692 0.8434 0.6256 0.062 Uiso 1 1 calc R J . C19C C 0.33690(11) 0.8163(3) 0.6449(2) 0.0479(16) Uani 1 1 d . J . H19C H 0.3323 0.8613 0.6528 0.058 Uiso 1 1 calc R . . O12B O 0.29578(7) 0.6446(2) 0.58889(10) 0.0322(8) Uani 1 1 d . J . C11B C 0.29340(9) 0.6249(3) 0.55830(14) 0.0269(9) Uani 1 1 d . . . N13B N 0.29355(8) 0.5581(2) 0.54578(13) 0.0303(9) Uani 1 1 d . J . Eu3 Eu 0.301575(4) 0.535552(13) 0.481901(7) 0.02616(6) Uani 1 1 d . . . O23B O 0.29002(8) 0.4294(2) 0.44929(13) 0.0399(9) Uani 1 1 d . J . C22B C 0.28140(10) 0.3761(3) 0.4641(2) 0.0432(15) Uani 1 1 d . . . O24B O 0.27403(10) 0.3200(3) 0.44698(18) 0.0589(14) Uani 1 1 d . J . C25B C 0.27589(18) 0.3222(5) 0.4096(3) 0.073(3) Uani 1 1 d . . . H25D H 0.2666 0.3610 0.4010 0.109 Uiso 1 1 d R J . H25E H 0.2699 0.2788 0.4000 0.109 Uiso 1 1 d R . . H25F H 0.2923 0.3282 0.4031 0.109 Uiso 1 1 d R . . C20B C 0.27963(11) 0.3723(3) 0.5010(2) 0.0440(15) Uani 1 1 d . J . N21B N 0.28422(8) 0.4325(3) 0.51752(15) 0.0346(10) Uani 1 1 d . J . C16B C 0.28428(10) 0.4347(3) 0.55197(17) 0.0367(12) Uani 1 1 d . . . C14B C 0.29007(9) 0.5041(3) 0.56850(17) 0.0344(12) Uani 1 1 d . J . O15B O 0.29072(7) 0.5065(2) 0.60082(12) 0.0362(9) Uani 1 1 d . J . C17B C 0.27928(13) 0.3753(4) 0.5722(3) 0.0546(18) Uani 1 1 d . J . H17B H 0.2788 0.3781 0.5964 0.066 Uiso 1 1 calc R . . C18B C 0.27491(16) 0.3113(4) 0.5548(3) 0.063(2) Uani 1 1 d . . . H18B H 0.2721 0.2696 0.5674 0.076 Uiso 1 1 calc R J . C19B C 0.27469(14) 0.3099(4) 0.5195(2) 0.0534(18) Uani 1 1 d . J . H19B H 0.2713 0.2677 0.5076 0.064 Uiso 1 1 calc R . . O68 O 0.25871(7) 0.5433(2) 0.47534(11) 0.0339(8) Uani 1 1 d . J . S69 S 0.23637(2) 0.51121(8) 0.46348(4) 0.0343(3) Uani 1 1 d . . . O70 O 0.21523(7) 0.5451(2) 0.47632(12) 0.0397(9) Uani 1 1 d . J . O71 O 0.23637(8) 0.4362(3) 0.46391(14) 0.0457(10) Uani 1 1 d . J . C72 C 0.23702(11) 0.5328(3) 0.41747(18) 0.0403(13) Uani 1 1 d . J . F73 F 0.25586(8) 0.5049(3) 0.40202(12) 0.0535(10) Uani 1 1 d . . . F74 F 0.21748(8) 0.5097(2) 0.40140(12) 0.0538(11) Uani 1 1 d . . . F75 F 0.23818(7) 0.6032(2) 0.41306(11) 0.0436(8) Uani 1 1 d . . . O4B O 0.29252(7) 0.6201(2) 0.43360(10) 0.0314(8) Uani 1 1 d . J . C3B C 0.28650(9) 0.6810(3) 0.43909(15) 0.0291(10) Uani 1 1 d . . . O2B O 0.27987(7) 0.7274(2) 0.41580(10) 0.0318(8) Uani 1 1 d . J . C1B C 0.28242(12) 0.7063(4) 0.37994(16) 0.0398(13) Uani 1 1 d . . . H1BA H 0.2985 0.6901 0.3759 0.060 Uiso 1 1 d R J . H1BB H 0.2791 0.7456 0.3651 0.060 Uiso 1 1 d R . . H1BC H 0.2713 0.6688 0.3753 0.060 Uiso 1 1 d R . . C5B C 0.28506(9) 0.7100(3) 0.47500(14) 0.0273(10) Uani 1 1 d . J . N10B N 0.28992(8) 0.6611(2) 0.49924(12) 0.0266(8) Uani 1 1 d . J . C9B C 0.28894(9) 0.6812(3) 0.53196(13) 0.0268(9) Uani 1 1 d . J . C8B C 0.28288(11) 0.7496(3) 0.54249(15) 0.0326(11) Uani 1 1 d . . . H8B H 0.2821 0.7614 0.5660 0.039 Uiso 1 1 calc R J . C7B C 0.27813(11) 0.7993(3) 0.51741(16) 0.0345(11) Uani 1 1 d . J . H7B H 0.2742 0.8459 0.5236 0.041 Uiso 1 1 calc R . . C6B C 0.27914(9) 0.7801(3) 0.48305(17) 0.0331(10) Uani 1 1 d . . . H6B H 0.2759 0.8131 0.4655 0.040 Uiso 1 1 calc R J . O12A O 0.33742(6) 0.59029(19) 0.50134(11) 0.0294(7) Uani 1 1 d . J . C11A C 0.35672(9) 0.5724(3) 0.51477(13) 0.0273(9) Uani 1 1 d . . . N13A N 0.36235(8) 0.5095(2) 0.52987(13) 0.0304(9) Uani 1 1 d . H . C14A C 0.34878(9) 0.4526(3) 0.52132(14) 0.0273(9) Uani 1 1 d . . . O15A O 0.32986(7) 0.4515(2) 0.50419(11) 0.0316(8) Uani 1 1 d . J . C16A C 0.35878(9) 0.3828(3) 0.53325(16) 0.0310(10) Uani 1 1 d . J . N21A N 0.37907(8) 0.3850(2) 0.55083(12) 0.0282(8) Uani 1 1 d . . . C20A C 0.38905(10) 0.3237(3) 0.56071(15) 0.0308(10) Uani 1 1 d . J . C19A C 0.37920(12) 0.2590(3) 0.5533(2) 0.0448(15) Uani 1 1 d . . . H19A H 0.3869 0.2171 0.5600 0.054 Uiso 1 1 calc R J . C18A C 0.35754(14) 0.2570(3) 0.5356(2) 0.0529(19) Uani 1 1 d . J . H18A H 0.3500 0.2136 0.5309 0.063 Uiso 1 1 calc R . . C17A C 0.34716(12) 0.3198(3) 0.5250(2) 0.0419(14) Uani 1 1 d . . . H17A H 0.3327 0.3199 0.5127 0.050 Uiso 1 1 calc R J . C22A C 0.41212(10) 0.3340(3) 0.58016(15) 0.0318(11) Uani 1 1 d . . . O23A O 0.41807(7) 0.3921(2) 0.58987(11) 0.0337(8) Uani 1 1 d . H . O24A O 0.42456(7) 0.2763(2) 0.58393(11) 0.0340(8) Uani 1 1 d . J . C25A C 0.44720(11) 0.2838(3) 0.60217(19) 0.0409(14) Uani 1 1 d . . . H25G H 0.4566 0.3203 0.5916 0.061 Uiso 1 1 d R J . H25H H 0.4558 0.2400 0.6014 0.061 Uiso 1 1 d R . . H25I H 0.4440 0.2962 0.6258 0.061 Uiso 1 1 d R . . C9A C 0.37704(9) 0.6243(3) 0.51387(14) 0.0289(10) Uani 1 1 d . J . N10A N 0.39623(7) 0.6080(2) 0.53329(11) 0.0259(8) Uani 1 1 d . . . C5A C 0.41478(10) 0.6529(3) 0.53364(15) 0.0336(11) Uani 1 1 d . J . C3A C 0.43459(10) 0.6289(3) 0.55613(14) 0.0342(11) Uani 1 1 d . . . O4A O 0.43271(7) 0.5782(2) 0.57519(11) 0.0321(8) Uani 1 1 d . H . O2A O 0.45370(8) 0.6696(3) 0.55499(12) 0.0442(11) Uani 1 1 d . J . C1A C 0.47350(13) 0.6493(6) 0.5766(2) 0.063(2) Uani 1 1 d . . . H1AA H 0.4680 0.6450 0.5999 0.095 Uiso 1 1 d R J . H1AB H 0.4857 0.6850 0.5754 0.095 Uiso 1 1 d R . . H1AC H 0.4800 0.6049 0.5691 0.095 Uiso 1 1 d R . . C6A C 0.41485(11) 0.7150(3) 0.51455(17) 0.0390(13) Uani 1 1 d . . . H6A H 0.4277 0.7461 0.5162 0.047 Uiso 1 1 d R J . C7A C 0.39492(11) 0.7319(3) 0.4943(2) 0.0447(16) Uani 1 1 d . J . H7A H 0.3952 0.7716 0.4802 0.054 Uiso 1 1 d R . . C8A C 0.37552(10) 0.6860(3) 0.49415(16) 0.0362(12) Uani 1 1 d . . . H8A H 0.3617 0.6962 0.4812 0.043 Uiso 1 1 calc R J . O111 O 0.32954(7) 0.5199(2) 0.43489(12) 0.0350(8) Uani 1 1 d . J . S112 S 0.35297(3) 0.49608(8) 0.42321(4) 0.0357(3) Uani 1 1 d . . . O113 O 0.36082(8) 0.5308(3) 0.39246(13) 0.0421(10) Uani 1 1 d . J . O114 O 0.37056(8) 0.4884(3) 0.45014(13) 0.0479(11) Uani 1 1 d . J . C115 C 0.34633(14) 0.4058(4) 0.4092(2) 0.0510(16) Uani 1 1 d . J . F116 F 0.36579(10) 0.3765(3) 0.39506(19) 0.0791(17) Uani 1 1 d . . . F117 F 0.33983(9) 0.3648(2) 0.43515(15) 0.0615(12) Uani 1 1 d . . . F118 F 0.32959(10) 0.4049(3) 0.38519(14) 0.0664(13) Uani 1 1 d . . . O119 O 0.25571(7) 0.6030(3) 0.63142(13) 0.0434(10) Uani 1 1 d . J . S120 S 0.23514(3) 0.59016(10) 0.60828(5) 0.0464(4) Uani 1 1 d . . . O121 O 0.24166(9) 0.5653(3) 0.57439(15) 0.0567(13) Uani 1 1 d . J . O122 O 0.21717(9) 0.6440(4) 0.60950(17) 0.0656(17) Uani 1 1 d . J . C123 C 0.22101(15) 0.5142(6) 0.6289(3) 0.065(2) Uani 1 1 d . J . F124 F 0.21471(9) 0.5276(3) 0.66149(14) 0.0713(15) Uani 1 1 d . . . F125 F 0.20128(11) 0.4955(4) 0.61182(18) 0.096(2) Uani 1 1 d . . . F126 F 0.23570(11) 0.4586(3) 0.62951(19) 0.0803(17) Uani 1 1 d . . . O127 O 0.40966(7) 0.5132(2) 0.63133(10) 0.0326(8) Uani 1 1 d . . . S128 S 0.40434(2) 0.52645(9) 0.66747(3) 0.0337(3) Uani 1 1 d . J . O129 O 0.37949(8) 0.5365(3) 0.67457(12) 0.0459(11) Uani 1 1 d . . . O130 O 0.41744(8) 0.4813(3) 0.69048(12) 0.0457(11) Uani 1 1 d . . . C131 C 0.41756(13) 0.6126(4) 0.67383(19) 0.0475(15) Uani 1 1 d . . . F132 F 0.44090(7) 0.6128(2) 0.66558(13) 0.0532(10) Uani 1 1 d . J . F133 F 0.40691(10) 0.6614(3) 0.65532(17) 0.0737(16) Uani 1 1 d . J . F134 F 0.41609(11) 0.6303(4) 0.70716(15) 0.0835(19) Uani 1 1 d . J . O135 O 0.42109(7) 0.4710(3) 0.52453(12) 0.0409(9) Uani 1 1 d DU . . N150 N 0.1658(2) 0.4222(8) 0.5499(4) 0.129(4) Uani 1 1 d DU A 2 C151 C 0.1868(2) 0.4138(8) 0.5448(4) 0.109(5) Uani 1 1 d DU A 2 C152 C 0.21386(18) 0.4098(7) 0.5425(3) 0.083(3) Uani 1 1 d DU A 2 H15D H 0.2207 0.4556 0.5463 0.125 Uiso 1 1 d R A 2 H15E H 0.2179 0.3937 0.5198 0.125 Uiso 1 1 d R A 2 H15F H 0.2200 0.3772 0.5593 0.125 Uiso 1 1 d R A 2 N165 N 0.3410(2) 0.7644(9) 0.5440(4) 0.111(6) Uani 0.80 1 d PDU B 6 C166 C 0.3364(3) 0.8262(8) 0.5437(3) 0.105(6) Uani 0.80 1 d PDU B 6 C167 C 0.3276(3) 0.9019(7) 0.5439(4) 0.089(4) Uani 0.80 1 d PDU B 6 H16A H 0.3122 0.9022 0.5329 0.134 Uiso 0.80 1 d PR B 6 H16B H 0.3385 0.9315 0.5313 0.134 Uiso 0.80 1 d PR B 6 H16C H 0.3260 0.9194 0.5671 0.134 Uiso 0.80 1 d PR B 6 N153 N 0.2897(2) 0.2040(14) 0.6136(4) 0.149(9) Uani 0.79 1 d PDU C 7 C154 C 0.30955(17) 0.1943(9) 0.6228(3) 0.075(4) Uani 0.79 1 d PDU C 7 C155 C 0.3344(2) 0.1744(8) 0.6330(4) 0.080(4) Uani 0.79 1 d PDU C 7 H15A H 0.3340 0.1522 0.6553 0.119 Uiso 0.79 1 d PR C 7 H15B H 0.3445 0.2155 0.6340 0.119 Uiso 0.79 1 d PR C 7 H15C H 0.3407 0.1419 0.6163 0.119 Uiso 0.79 1 d PR C 7 N156 N 0.3146(2) 0.2099(8) 0.4806(4) 0.060(4) Uani 0.47 1 d PDU D 8 C157 C 0.3159(3) 0.1767(9) 0.4552(4) 0.057(4) Uani 0.47 1 d PDU D 8 C158 C 0.3153(4) 0.1207(14) 0.4269(6) 0.093(7) Uani 0.47 1 d PDU D 8 H15G H 0.3005 0.1302 0.4154 0.139 Uiso 0.47 1 d PR D 8 H15H H 0.3159 0.0719 0.4336 0.139 Uiso 0.47 1 d PR D 8 H15I H 0.3284 0.1309 0.4117 0.139 Uiso 0.47 1 d PR D 8 C162 C 0.3904(4) 0.7811(11) 0.7232(6) 0.069(6) Uani 0.41 1 d PDU E 10 H16D H 0.4032 0.7627 0.7095 0.103 Uiso 0.41 1 d PR E 10 H16E H 0.3951 0.7821 0.7470 0.103 Uiso 0.41 1 d PR E 10 H16F H 0.3866 0.8282 0.7158 0.103 Uiso 0.41 1 d PR E 10 N310 N 0.3546(3) 0.6896(11) 0.7148(5) 0.066(5) Uani 0.41 1 d PDU E 10 C311 C 0.3698(3) 0.7309(10) 0.7202(5) 0.079(7) Uani 0.41 1 d PDU E 10 C202 C 0.3995(5) 0.137(2) 0.4974(11) 0.087(9) Uani 0.30 1 d PDU F 5 H20A H 0.3904 0.0973 0.4895 0.131 Uiso 0.30 1 d PR F 5 H20B H 0.4098 0.1538 0.4791 0.131 Uiso 0.30 1 d PR F 5 H20C H 0.3888 0.1746 0.5042 0.131 Uiso 0.30 1 d PR F 5 C201 C 0.4259(6) 0.146(3) 0.5084(11) 0.107(11) Uani 0.30 1 d PDU F 5 N200 N 0.4438(4) 0.1408(13) 0.5258(6) 0.063(6) Uani 0.30 1 d PDU F 5 C305 C 0.3983(4) 0.2932(9) 0.4566(5) 0.053(5) Uani 0.38 1 d PDU G 4 H30A H 0.4098 0.3177 0.4427 0.080 Uiso 0.38 1 d PR G 4 H30B H 0.4063 0.2707 0.4756 0.080 Uiso 0.38 1 d PR G 4 H30C H 0.3867 0.3262 0.4653 0.080 Uiso 0.38 1 d PR G 4 C306 C 0.3847(3) 0.2391(9) 0.4354(6) 0.055(5) Uani 0.38 1 d PDU G 4 N307 N 0.3748(6) 0.2026(13) 0.4150(9) 0.129(14) Uani 0.38 1 d PDU G 4 S136 S 0.43714(3) 0.42895(9) 0.50466(5) 0.0315(4) Uani 0.798(5) 1 d PDU H 40 O138 O 0.43678(11) 0.3560(3) 0.51494(15) 0.0409(12) Uani 0.798(5) 1 d PDU H 40 C140 C 0.46594(14) 0.4613(4) 0.5191(2) 0.0416(15) Uani 0.798(5) 1 d PDU H 40 F142 F 0.46936(10) 0.4491(4) 0.55295(15) 0.0593(15) Uani 0.798(5) 1 d PDU H 40 F143 F 0.46792(10) 0.5319(3) 0.51439(14) 0.0445(12) Uani 0.798(5) 1 d PDU H 40 F147 F 0.48381(10) 0.4318(3) 0.50229(19) 0.0644(16) Uani 0.798(5) 1 d PDU H 40 O149 O 0.43746(13) 0.4434(4) 0.46829(16) 0.0435(14) Uani 0.798(5) 1 d PDU H 40 S8 S 0.44838(13) 0.4481(4) 0.5185(2) 0.0390(18) Uani 0.202(5) 1 d PDU H 41 C22 C 0.4453(4) 0.3949(12) 0.4803(5) 0.049(4) Uani 0.202(5) 1 d PDU H 41 F28 F 0.4675(4) 0.3869(16) 0.4650(8) 0.082(7) Uani 0.202(5) 1 d PDU H 41 O1 O 0.4597(4) 0.5113(13) 0.5055(8) 0.050(5) Uani 0.202(5) 1 d PDU H 41 F39 F 0.4302(5) 0.4262(15) 0.4576(6) 0.060(5) Uani 0.202(5) 1 d PDU H 41 F9 F 0.4394(5) 0.3261(12) 0.4840(7) 0.070(5) Uani 0.202(5) 1 d PDU H 41 O12 O 0.4618(5) 0.4042(14) 0.5411(7) 0.055(5) Uani 0.202(5) 1 d PDU H 41 C1 C 0.2455(3) 0.2121(4) 0.6686(4) 0.118(6) Uani 1 1 d DU . 11 H1A H 0.2432 0.1968 0.6916 0.178 Uiso 0.50 1 d PR . 11 H1B H 0.2576 0.1825 0.6581 0.178 Uiso 0.50 1 d PR . 11 H1C H 0.2314 0.2086 0.6559 0.178 Uiso 0.50 1 d PR . 11 N6 N 0.2371(4) 0.1561(9) 0.6589(6) 0.105(7) Uani 0.50 1 d PDU I 11 O999 O 0.31575(8) 0.6143(2) 0.70285(10) 0.0662(11) Uani 0.80 1 d PGU J 50 S991 S 0.32081(5) 0.66159(12) 0.73234(6) 0.0665(7) Uani 0.80 1 d PGU J 50 O997 O 0.32084(8) 0.7360(2) 0.72392(12) 0.0662(11) Uani 0.80 1 d PGU J 50 O996 O 0.33969(7) 0.6378(2) 0.75475(10) 0.0662(11) Uani 0.80 1 d PGU J 50 C998 C 0.29360(6) 0.6491(2) 0.75865(10) 0.0865(19) Uani 0.80 1 d PGU J 50 F995 F 0.29416(10) 0.6896(3) 0.78739(13) 0.0931(13) Uani 0.80 1 d PGU J 50 F997 F 0.29101(9) 0.5819(3) 0.76876(15) 0.0931(13) Uani 0.80 1 d PGU J 50 F996 F 0.27379(9) 0.6669(3) 0.74037(14) 0.0931(13) Uani 0.80 1 d PGU J 50 S201 S 0.3005(2) 0.6286(7) 0.7261(3) 0.0844(17) Uani 0.20 1 d PGU J 51 O200 O 0.2924(4) 0.6919(9) 0.7182(5) 0.090(2) Uani 0.20 1 d PGDU J 51 O202 O 0.3227(3) 0.6183(11) 0.7186(5) 0.090(2) Uani 0.20 1 d PGU J 51 O203 O 0.2861(4) 0.5779(10) 0.7190(5) 0.090(2) Uani 0.20 1 d PGU J 51 C204 C 0.3000(3) 0.6316(7) 0.7684(3) 0.085(2) Uani 0.20 1 d PGU J 51 F205 F 0.3073(4) 0.5775(10) 0.7809(5) 0.076(2) Uani 0.20 1 d PGU J 51 F207 F 0.2802(3) 0.6409(12) 0.7792(5) 0.076(2) Uani 0.20 1 d PGU J 51 F206 F 0.3123(4) 0.6795(10) 0.7789(5) 0.076(2) Uani 0.20 1 d PGU J 51 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01537(9) 0.02979(10) 0.02741(10) 0.00259(8) -0.00118(8) -0.00080(8) C14C 0.019(2) 0.037(3) 0.029(2) 0.007(2) -0.0023(17) 0.0000(18) O15C 0.0221(16) 0.0343(18) 0.0306(18) 0.0041(15) 0.0000(13) 0.0012(13) N13C 0.023(2) 0.033(2) 0.031(2) 0.0050(17) -0.0028(16) 0.0012(16) Eu2 0.01945(11) 0.03764(13) 0.03338(12) 0.00766(10) 0.00288(9) 0.00165(9) O4C 0.030(2) 0.048(2) 0.040(2) 0.0118(18) 0.0108(17) 0.0044(17) C3C 0.029(3) 0.043(3) 0.045(3) 0.012(3) 0.007(2) -0.002(2) O2C 0.043(2) 0.050(2) 0.051(3) 0.018(2) 0.021(2) 0.0070(19) C1C 0.049(4) 0.062(4) 0.058(4) 0.009(4) 0.028(3) 0.001(3) C5C 0.026(3) 0.040(3) 0.046(3) 0.009(2) 0.006(2) -0.003(2) N10C 0.0207(19) 0.036(2) 0.040(2) 0.0117(19) 0.0052(18) 0.0015(17) C9C 0.024(2) 0.031(2) 0.043(3) 0.006(2) 0.000(2) -0.0006(19) C11C 0.019(2) 0.035(2) 0.031(2) 0.003(2) -0.0034(18) -0.0029(18) O12C 0.0202(16) 0.0309(17) 0.038(2) 0.0060(15) 0.0030(14) -0.0008(13) C8C 0.025(3) 0.034(3) 0.063(4) 0.011(3) 0.008(2) 0.003(2) C7C 0.044(3) 0.030(3) 0.052(4) 0.013(3) 0.011(3) 0.006(2) C6C 0.029(3) 0.043(3) 0.053(4) 0.018(3) 0.004(2) -0.007(2) O23C 0.028(2) 0.052(3) 0.047(2) -0.010(2) 0.0041(18) 0.0044(17) C22C 0.029(3) 0.052(3) 0.041(3) -0.012(3) -0.005(2) 0.007(2) O24C 0.033(2) 0.078(4) 0.075(4) -0.043(3) 0.005(2) -0.002(2) C25C 0.034(3) 0.090(6) 0.077(6) -0.043(5) -0.003(3) 0.019(4) C20C 0.027(3) 0.040(3) 0.040(3) -0.010(2) -0.002(2) -0.003(2) N21C 0.0224(19) 0.037(2) 0.033(2) -0.0047(18) -0.0044(16) 0.0002(16) C16C 0.023(2) 0.035(3) 0.036(3) 0.002(2) -0.006(2) -0.002(2) C17C 0.028(3) 0.033(3) 0.049(3) 0.000(2) 0.004(2) 0.000(2) C18C 0.036(3) 0.033(3) 0.085(5) -0.013(3) 0.005(3) -0.005(2) C19C 0.031(3) 0.036(3) 0.077(5) -0.019(3) -0.006(3) 0.000(2) O12B 0.0318(19) 0.0363(19) 0.0284(18) 0.0077(15) -0.0043(15) -0.0059(15) C11B 0.019(2) 0.033(2) 0.029(2) 0.0016(19) -0.0031(17) -0.0053(17) N13B 0.0163(18) 0.0267(19) 0.048(3) 0.0074(19) -0.0025(17) -0.0034(15) Eu3 0.01792(10) 0.02600(10) 0.03455(12) 0.00090(9) -0.00602(9) -0.00386(8) O23B 0.0268(19) 0.039(2) 0.054(3) -0.0099(19) -0.0053(18) -0.0048(16) C22B 0.022(2) 0.030(3) 0.078(5) -0.011(3) -0.012(3) -0.005(2) O24B 0.044(3) 0.041(3) 0.092(4) -0.016(3) -0.011(3) -0.010(2) C25B 0.061(5) 0.061(5) 0.095(7) -0.047(5) -0.010(5) -0.014(4) C20B 0.029(3) 0.028(3) 0.075(5) 0.006(3) -0.007(3) -0.010(2) N21B 0.0188(19) 0.032(2) 0.053(3) 0.008(2) -0.0054(18) -0.0038(16) C16B 0.023(2) 0.034(3) 0.054(3) 0.011(3) -0.005(2) -0.0064(19) C14B 0.019(2) 0.033(2) 0.051(4) 0.011(2) -0.005(2) -0.0035(18) O15B 0.0224(18) 0.038(2) 0.048(2) 0.0140(18) 0.0038(16) -0.0034(14) C17B 0.047(4) 0.036(3) 0.081(5) 0.020(3) -0.010(4) -0.013(3) C18B 0.058(5) 0.036(3) 0.095(7) 0.019(4) -0.006(4) -0.019(3) C19B 0.047(4) 0.030(3) 0.083(6) 0.007(3) -0.008(4) -0.012(3) O68 0.0227(17) 0.0352(18) 0.044(2) 0.0024(16) -0.0071(15) -0.0065(14) S69 0.0204(6) 0.0380(6) 0.0444(7) 0.0006(6) -0.0051(5) -0.0056(5) O70 0.0244(18) 0.049(2) 0.046(2) 0.0021(19) -0.0012(16) -0.0025(16) O71 0.032(2) 0.042(2) 0.063(3) 0.004(2) -0.006(2) -0.0069(18) C72 0.033(3) 0.046(3) 0.042(3) -0.004(3) -0.001(2) 0.002(2) F73 0.043(2) 0.067(3) 0.051(2) -0.007(2) 0.0022(18) 0.0089(19) F74 0.045(2) 0.062(3) 0.054(2) -0.006(2) -0.0244(19) -0.0094(18) F75 0.0328(18) 0.050(2) 0.048(2) 0.0089(17) -0.0092(15) -0.0038(15) O4B 0.0255(17) 0.0365(19) 0.0321(19) -0.0011(15) -0.0054(14) 0.0001(14) C3B 0.018(2) 0.032(2) 0.037(3) 0.004(2) -0.0011(18) -0.0006(17) O2B 0.0297(18) 0.0381(19) 0.0275(18) 0.0092(15) -0.0021(14) -0.0004(15) C1B 0.035(3) 0.054(4) 0.030(3) 0.006(2) -0.004(2) 0.003(2) C5B 0.0175(19) 0.031(2) 0.034(3) 0.0073(19) -0.0008(17) -0.0035(16) N10B 0.0188(18) 0.0282(19) 0.033(2) 0.0008(17) -0.0037(15) -0.0031(14) C9B 0.021(2) 0.030(2) 0.029(2) 0.0056(19) -0.0014(17) -0.0045(17) C8B 0.033(3) 0.033(3) 0.031(3) 0.002(2) 0.001(2) 0.001(2) C7B 0.033(3) 0.029(2) 0.042(3) 0.002(2) 0.004(2) 0.001(2) C6B 0.028(2) 0.030(2) 0.042(3) 0.007(2) 0.002(2) -0.0005(18) O12A 0.0200(16) 0.0296(17) 0.038(2) 0.0040(15) -0.0094(14) -0.0039(13) C11A 0.021(2) 0.033(2) 0.028(2) 0.0043(19) 0.0006(17) -0.0045(18) N13A 0.023(2) 0.028(2) 0.040(2) 0.0038(18) -0.0004(18) -0.0035(16) C14A 0.019(2) 0.029(2) 0.034(2) 0.0042(19) -0.0009(18) -0.0038(17) O15A 0.0214(17) 0.0314(18) 0.042(2) 0.0030(16) -0.0078(15) -0.0063(13) C16A 0.023(2) 0.027(2) 0.043(3) 0.000(2) -0.001(2) -0.0013(18) N21A 0.0191(19) 0.030(2) 0.035(2) 0.0032(17) 0.0005(16) -0.0001(15) C20A 0.027(2) 0.029(2) 0.036(3) 0.007(2) -0.006(2) 0.0001(18) C19A 0.037(3) 0.030(3) 0.067(4) 0.008(3) -0.012(3) -0.001(2) C18A 0.045(4) 0.032(3) 0.082(5) 0.004(3) -0.020(4) -0.008(3) C17A 0.032(3) 0.031(3) 0.062(4) 0.004(3) -0.011(3) -0.003(2) C22A 0.029(3) 0.030(2) 0.036(3) 0.006(2) 0.001(2) 0.0053(19) O23A 0.0274(19) 0.040(2) 0.0342(19) -0.0020(16) -0.0085(15) 0.0041(15) O24A 0.0274(19) 0.0343(19) 0.040(2) 0.0026(16) -0.0065(15) 0.0078(15) C25A 0.032(3) 0.040(3) 0.051(4) -0.003(3) -0.013(2) 0.010(2) C9A 0.025(2) 0.032(2) 0.029(2) 0.0030(19) -0.0021(18) -0.0053(18) N10A 0.0190(18) 0.034(2) 0.0244(19) -0.0008(16) -0.0006(14) -0.0048(15) C5A 0.024(2) 0.046(3) 0.031(2) 0.003(2) -0.0041(19) -0.013(2) C3A 0.023(2) 0.050(3) 0.029(2) 0.005(2) -0.0029(19) -0.009(2) O4A 0.0216(16) 0.042(2) 0.0322(18) 0.0031(16) -0.0010(14) -0.0030(14) O2A 0.029(2) 0.066(3) 0.038(2) 0.014(2) -0.0121(17) -0.023(2) C1A 0.029(3) 0.111(7) 0.050(4) 0.022(4) -0.020(3) -0.030(4) C6A 0.032(3) 0.042(3) 0.043(3) 0.013(2) -0.014(2) -0.017(2) C7A 0.032(3) 0.041(3) 0.061(4) 0.022(3) -0.015(3) -0.019(2) C8A 0.028(3) 0.037(3) 0.044(3) 0.013(2) -0.009(2) -0.014(2) O111 0.0234(18) 0.038(2) 0.043(2) 0.0004(17) -0.0033(15) 0.0005(15) S112 0.0256(6) 0.0409(7) 0.0406(7) 0.0003(6) -0.0005(5) -0.0010(5) O113 0.032(2) 0.051(2) 0.044(2) -0.003(2) 0.0027(18) -0.0080(18) O114 0.028(2) 0.068(3) 0.048(3) 0.012(2) -0.0035(18) -0.003(2) C115 0.043(4) 0.045(3) 0.064(4) -0.001(3) 0.014(3) 0.000(3) F116 0.070(3) 0.054(3) 0.113(5) -0.023(3) 0.038(3) 0.009(2) F117 0.060(3) 0.044(2) 0.081(3) 0.014(2) 0.011(2) 0.0025(19) F118 0.077(3) 0.052(3) 0.070(3) -0.015(2) -0.006(3) -0.019(2) O119 0.0220(18) 0.055(3) 0.053(3) 0.012(2) -0.0021(17) 0.0003(17) S120 0.0192(6) 0.0662(10) 0.0539(9) 0.0239(8) -0.0003(6) -0.0031(6) O121 0.034(2) 0.082(4) 0.055(3) 0.016(3) -0.007(2) -0.006(2) O122 0.030(2) 0.095(4) 0.072(4) 0.041(3) 0.009(2) 0.017(3) C123 0.038(4) 0.086(6) 0.070(5) 0.022(5) -0.004(4) -0.023(4) F124 0.050(3) 0.101(4) 0.062(3) 0.032(3) 0.006(2) -0.021(3) F125 0.055(3) 0.142(6) 0.091(4) 0.032(4) -0.019(3) -0.056(4) F126 0.074(4) 0.056(3) 0.111(5) 0.021(3) 0.001(3) -0.012(3) O127 0.0205(16) 0.048(2) 0.0295(18) -0.0017(16) -0.0013(14) 0.0015(15) S128 0.0192(5) 0.0551(8) 0.0268(6) 0.0036(5) -0.0005(4) 0.0052(5) O129 0.0218(19) 0.083(3) 0.033(2) 0.002(2) 0.0012(15) 0.010(2) O130 0.0247(19) 0.080(3) 0.033(2) 0.015(2) 0.0010(16) 0.006(2) C131 0.038(3) 0.058(4) 0.047(4) -0.011(3) -0.009(3) 0.007(3) F132 0.0313(19) 0.061(2) 0.067(3) -0.002(2) -0.0047(18) -0.0043(17) F133 0.060(3) 0.052(2) 0.109(5) -0.006(3) -0.036(3) 0.014(2) F134 0.065(3) 0.121(5) 0.064(3) -0.049(3) -0.017(3) 0.017(3) O135 0.0255(19) 0.055(2) 0.042(2) -0.0072(19) 0.0032(16) -0.0050(17) N150 0.103(7) 0.131(8) 0.151(8) -0.001(7) -0.033(7) -0.012(6) C151 0.117(11) 0.098(9) 0.111(10) 0.013(8) -0.018(9) -0.041(8) C152 0.077(7) 0.089(7) 0.084(7) 0.009(6) 0.000(5) -0.028(6) N165 0.060(7) 0.188(17) 0.084(9) -0.034(10) -0.018(6) 0.036(9) C166 0.078(10) 0.19(2) 0.044(6) -0.016(9) -0.014(6) 0.020(11) C167 0.084(10) 0.110(11) 0.072(8) -0.016(8) 0.007(7) -0.031(9) N153 0.077(9) 0.30(3) 0.067(8) 0.077(12) 0.015(7) 0.047(13) C154 0.053(6) 0.122(11) 0.052(6) 0.010(6) 0.007(5) -0.002(7) C155 0.073(8) 0.089(9) 0.077(8) -0.023(7) -0.013(6) 0.011(7) N156 0.037(6) 0.063(8) 0.082(10) -0.003(8) -0.015(7) -0.012(5) C157 0.041(7) 0.074(10) 0.055(9) 0.020(8) 0.000(7) 0.002(7) C158 0.048(10) 0.134(17) 0.097(15) -0.041(14) 0.001(10) -0.028(11) C162 0.095(16) 0.057(11) 0.054(11) -0.016(9) -0.017(10) 0.015(10) N310 0.037(8) 0.092(13) 0.069(11) -0.021(10) -0.013(7) -0.004(8) C311 0.106(16) 0.099(15) 0.033(8) 0.010(9) -0.005(9) 0.069(13) C202 0.098(13) 0.067(11) 0.096(13) 0.003(9) 0.003(9) 0.007(9) C201 0.110(12) 0.105(12) 0.107(12) -0.002(5) 0.001(5) 0.002(5) N200 0.052(12) 0.066(12) 0.069(14) -0.041(11) 0.028(10) -0.011(10) C305 0.076(14) 0.046(9) 0.039(9) 0.007(7) -0.014(9) -0.017(9) C306 0.050(10) 0.044(9) 0.070(12) -0.026(9) -0.020(9) 0.023(8) N307 0.16(3) 0.087(16) 0.14(2) -0.065(17) -0.06(2) 0.088(19) S136 0.0263(8) 0.0377(8) 0.0306(8) 0.0021(7) 0.0026(7) 0.0052(6) O138 0.044(3) 0.035(2) 0.044(3) -0.001(2) 0.006(2) 0.008(2) C140 0.035(3) 0.043(3) 0.046(4) 0.009(3) 0.002(3) 0.006(3) F142 0.042(3) 0.079(4) 0.056(3) 0.018(3) -0.021(2) -0.001(3) F143 0.036(3) 0.049(3) 0.048(3) 0.005(2) 0.000(2) -0.003(2) F147 0.031(3) 0.070(4) 0.092(4) -0.003(3) 0.017(3) 0.014(2) O149 0.046(3) 0.059(4) 0.026(3) -0.003(3) -0.006(2) 0.014(3) S8 0.027(3) 0.052(3) 0.038(3) 0.004(3) 0.006(3) 0.012(3) C22 0.048(7) 0.058(7) 0.043(7) -0.002(7) 0.006(6) 0.013(6) F28 0.072(13) 0.091(14) 0.082(14) -0.013(12) 0.032(12) 0.033(12) O1 0.040(9) 0.058(10) 0.051(9) 0.023(9) -0.007(8) 0.002(8) F39 0.070(12) 0.077(11) 0.034(10) -0.009(9) -0.005(9) 0.033(10) F9 0.068(11) 0.074(10) 0.066(10) 0.008(10) 0.011(10) 0.006(9) O12 0.053(7) 0.057(7) 0.055(7) 0.015(7) -0.003(7) 0.008(7) C1 0.145(14) 0.085(8) 0.125(12) 0.020(8) 0.069(11) -0.008(8) N6 0.085(14) 0.14(2) 0.090(14) 0.019(14) 0.011(11) -0.033(13) O999 0.077(3) 0.066(2) 0.055(2) 0.0029(19) -0.008(2) 0.006(2) S991 0.0796(17) 0.0622(14) 0.0579(14) -0.0016(12) -0.0072(13) 0.0149(12) O997 0.077(3) 0.066(2) 0.055(2) 0.0029(19) -0.008(2) 0.006(2) O996 0.077(3) 0.066(2) 0.055(2) 0.0029(19) -0.008(2) 0.006(2) C998 0.082(3) 0.085(3) 0.093(4) 0.001(3) -0.015(3) 0.025(3) F995 0.083(3) 0.094(3) 0.102(3) 0.003(2) -0.006(2) 0.026(2) F997 0.083(3) 0.094(3) 0.102(3) 0.003(2) -0.006(2) 0.026(2) F996 0.083(3) 0.094(3) 0.102(3) 0.003(2) -0.006(2) 0.026(2) S201 0.084(3) 0.081(3) 0.088(3) 0.004(3) -0.010(3) 0.018(3) O200 0.091(4) 0.085(4) 0.095(4) -0.001(4) -0.004(4) 0.018(4) O202 0.091(4) 0.085(4) 0.095(4) -0.001(4) -0.004(4) 0.018(4) O203 0.091(4) 0.085(4) 0.095(4) -0.001(4) -0.004(4) 0.018(4) C204 0.081(4) 0.084(4) 0.090(4) 0.003(4) -0.011(4) 0.021(4) F205 0.070(3) 0.079(3) 0.080(3) 0.005(3) -0.009(3) 0.021(3) F207 0.070(3) 0.079(3) 0.080(3) 0.005(3) -0.009(3) 0.021(3) F206 0.070(3) 0.079(3) 0.080(3) 0.005(3) -0.009(3) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O127 2.391(4) . ? Eu1 O12C 2.401(4) . ? Eu1 O15C 2.418(4) . ? Eu1 O135 2.421(4) . ? Eu1 O23A 2.498(4) . ? Eu1 O4A 2.516(4) . ? Eu1 N13A 2.523(5) . ? Eu1 N10A 2.539(4) . ? Eu1 N21A 2.551(5) . ? C14C O15C 1.227(6) . ? C14C N13C 1.358(7) . ? C14C C16C 1.504(8) . ? N13C C11C 1.351(7) . ? N13C Eu2 2.532(5) . ? Eu2 O12B 2.376(4) . ? Eu2 O15B 2.401(5) . ? Eu2 O119 2.401(4) . ? Eu2 O23C 2.475(5) . ? Eu2 O999 2.501(4) . ? Eu2 O4C 2.506(4) . ? Eu2 N21C 2.542(5) . ? Eu2 N10C 2.551(5) . ? Eu2 O203 2.959(19) . ? Eu2 S201 3.224(13) . ? O4C C3C 1.220(8) . ? O4C O203 1.675(18) . ? C3C O2C 1.305(7) . ? C3C C5C 1.489(8) . ? O2C C1C 1.446(8) . ? C5C N10C 1.354(7) . ? C5C C6C 1.387(9) . ? N10C C9C 1.333(7) . ? C9C C8C 1.383(8) . ? C9C C11C 1.504(7) . ? C11C O12C 1.246(7) . ? C8C C7C 1.391(9) . ? C7C C6C 1.388(9) . ? O23C C22C 1.213(8) . ? C22C O24C 1.301(8) . ? C22C C20C 1.525(9) . ? O24C C25C 1.471(10) . ? C20C N21C 1.325(7) . ? C20C C19C 1.392(9) . ? N21C C16C 1.335(7) . ? C16C C17C 1.385(8) . ? C17C C18C 1.394(9) . ? C18C C19C 1.376(10) . ? O12B C11B 1.250(6) . ? C11B N13B 1.355(7) . ? C11B C9B 1.497(7) . ? N13B C14B 1.363(7) . ? N13B Eu3 2.552(5) . ? Eu3 O12A 2.377(4) . ? Eu3 O15A 2.403(4) . ? Eu3 O68 2.412(4) . ? Eu3 O111 2.418(4) . ? Eu3 O23B 2.461(4) . ? Eu3 O4B 2.514(4) . ? Eu3 N10B 2.554(4) . ? Eu3 N21B 2.579(5) . ? O23B C22B 1.256(8) . ? C22B O24B 1.317(8) . ? C22B C20B 1.437(11) . ? O24B C25B 1.453(13) . ? C20B N21B 1.333(8) . ? C20B C19B 1.408(9) . ? N21B C16B 1.336(9) . ? C16B C17B 1.398(9) . ? C16B C14B 1.496(9) . ? C14B O15B 1.254(8) . ? C17B C18B 1.409(12) . ? C18B C19B 1.370(14) . ? O68 S69 1.462(4) . ? S69 O71 1.420(5) . ? S69 O70 1.433(5) . ? S69 C72 1.830(7) . ? C72 F73 1.321(8) . ? C72 F74 1.331(7) . ? C72 F75 1.346(8) . ? O4B C3B 1.219(7) . ? C3B O2B 1.313(6) . ? C3B C5B 1.499(8) . ? O2B C1B 1.453(7) . ? C5B N10B 1.346(7) . ? C5B C6B 1.404(7) . ? N10B C9B 1.325(7) . ? C9B C8B 1.399(8) . ? C8B C7B 1.378(8) . ? C7B C6B 1.382(9) . ? O12A C11A 1.244(6) . ? C11A N13A 1.362(7) . ? C11A C9A 1.503(7) . ? N13A C14A 1.358(7) . ? C14A O15A 1.248(6) . ? C14A C16A 1.507(7) . ? C16A N21A 1.323(7) . ? C16A C17A 1.395(8) . ? N21A C20A 1.344(7) . ? C20A C19A 1.372(8) . ? C20A C22A 1.506(8) . ? C19A C18A 1.391(9) . ? C18A C17A 1.384(9) . ? C22A O23A 1.209(7) . ? C22A O24A 1.303(6) . ? O24A C25A 1.456(7) . ? C9A N10A 1.346(7) . ? C9A C8A 1.398(7) . ? N10A C5A 1.340(6) . ? C5A C6A 1.389(8) . ? C5A C3A 1.480(8) . ? C3A O4A 1.216(7) . ? C3A O2A 1.317(6) . ? O2A C1A 1.439(8) . ? C6A C7A 1.400(8) . ? C7A C8A 1.389(7) . ? O111 S112 1.456(4) . ? S112 O113 1.430(5) . ? S112 O114 1.441(5) . ? S112 C115 1.831(8) . ? C115 F118 1.319(10) . ? C115 F117 1.323(9) . ? C115 F116 1.338(9) . ? O119 S120 1.478(5) . ? S120 O122 1.431(6) . ? S120 O121 1.442(7) . ? S120 C123 1.824(9) . ? C123 F125 1.333(10) . ? C123 F124 1.336(12) . ? C123 F126 1.336(12) . ? O127 S128 1.454(4) . ? S128 O129 1.428(4) . ? S128 O130 1.436(5) . ? S128 C131 1.807(8) . ? C131 F133 1.313(9) . ? C131 F134 1.337(9) . ? C131 F132 1.343(8) . ? O135 S136 1.426(5) . ? O135 S8 1.602(8) . ? N150 C151 1.203(9) . ? C151 C152 1.514(9) . ? N165 C166 1.197(9) . ? C166 C167 1.515(10) . ? N153 C154 1.178(9) . ? C154 C155 1.493(9) . ? N156 C157 1.172(9) . ? C157 C158 1.524(10) . ? C162 C311 1.495(10) . ? N310 C311 1.174(10) . ? C202 C201 1.541(10) . ? C201 N200 1.212(10) . ? C305 C306 1.518(10) . ? C306 N307 1.187(10) . ? S136 O149 1.436(6) . ? S136 O138 1.437(5) . ? S136 C140 1.810(8) . ? C140 F147 1.317(9) . ? C140 F142 1.346(9) . ? C140 F143 1.352(9) . ? S8 O12 1.421(16) . ? S8 O1 1.443(17) . ? S8 C22 1.799(17) . ? C22 F9 1.352(18) . ? C22 F39 1.358(18) . ? C22 F28 1.384(18) . ? C1 N6 1.217(10) . ? C1 C1 1.522(10) 8_554 ? O999 S991 1.479(3) . ? S991 O996 1.439(3) . ? S991 O997 1.445(3) . ? S991 C998 1.846(3) . ? C998 F997 1.340(2) . ? C998 F995 1.353(2) . ? C998 F996 1.356(2) . ? S201 O203 1.281(10) . ? S201 O202 1.288(10) . ? S201 O200 1.318(11) . ? S201 C204 1.644(13) . ? C204 F207 1.194(10) . ? C204 F205 1.205(10) . ? C204 F206 1.209(10) . ? 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 O127 Eu1 O12C 76.00(13) . . ? O127 Eu1 O15C 75.39(13) . . ? O12C Eu1 O15C 67.61(13) . . ? O127 Eu1 O135 124.79(14) . . ? O12C Eu1 O135 144.07(14) . . ? O15C Eu1 O135 140.73(15) . . ? O127 Eu1 O23A 70.94(14) . . ? O12C Eu1 O23A 89.74(13) . . ? O15C Eu1 O23A 143.13(13) . . ? O135 Eu1 O23A 73.56(15) . . ? O127 Eu1 O4A 69.90(14) . . ? O12C Eu1 O4A 142.33(14) . . ? O15C Eu1 O4A 88.34(13) . . ? O135 Eu1 O4A 71.84(14) . . ? O23A Eu1 O4A 93.82(13) . . ? O127 Eu1 N13A 149.33(15) . . ? O12C Eu1 N13A 78.69(14) . . ? O15C Eu1 N13A 79.15(14) . . ? O135 Eu1 N13A 85.86(16) . . ? O23A Eu1 N13A 126.17(14) . . ? O4A Eu1 N13A 126.41(14) . . ? O127 Eu1 N10A 119.94(14) . . ? O12C Eu1 N10A 125.22(13) . . ? O15C Eu1 N10A 67.57(13) . . ? O135 Eu1 N10A 73.23(15) . . ? O23A Eu1 N10A 144.37(14) . . ? O4A Eu1 N10A 63.66(13) . . ? N13A Eu1 N10A 63.39(14) . . ? O127 Eu1 N21A 121.19(15) . . ? O12C Eu1 N21A 68.93(14) . . ? O15C Eu1 N21A 126.69(13) . . ? O135 Eu1 N21A 75.15(15) . . ? O23A Eu1 N21A 63.47(14) . . ? O4A Eu1 N21A 144.21(14) . . ? N13A Eu1 N21A 63.31(15) . . ? N10A Eu1 N21A 118.80(14) . . ? O15C C14C N13C 128.4(5) . . ? O15C C14C C16C 117.6(5) . . ? N13C C14C C16C 113.9(5) . . ? C14C O15C Eu1 138.0(4) . . ? C11C N13C C14C 117.6(5) . . ? C11C N13C Eu2 120.5(3) . . ? C14C N13C Eu2 121.8(3) . . ? O12B Eu2 O15B 68.00(14) . . ? O12B Eu2 O119 74.45(15) . . ? O15B Eu2 O119 75.13(16) . . ? O12B Eu2 O23C 84.99(16) . . ? O15B Eu2 O23C 142.82(15) . . ? O119 Eu2 O23C 73.23(17) . . ? O12B Eu2 O999 140.66(14) . . ? O15B Eu2 O999 144.28(14) . . ? O119 Eu2 O999 125.33(16) . . ? O23C Eu2 O999 72.02(15) . . ? O12B Eu2 O4C 142.82(14) . . ? O15B Eu2 O4C 93.19(15) . . ? O119 Eu2 O4C 69.68(15) . . ? O23C Eu2 O4C 93.74(16) . . ? O999 Eu2 O4C 71.93(15) . . ? O12B Eu2 N13C 81.68(14) . . ? O15B Eu2 N13C 75.69(14) . . ? O119 Eu2 N13C 147.54(17) . . ? O23C Eu2 N13C 126.69(15) . . ? O999 Eu2 N13C 86.99(14) . . ? O4C Eu2 N13C 125.99(14) . . ? O12B Eu2 N21C 68.70(14) . . ? O15B Eu2 N21C 123.11(14) . . ? O119 Eu2 N21C 124.66(16) . . ? O23C Eu2 N21C 63.93(15) . . ? O999 Eu2 N21C 72.55(15) . . ? O4C Eu2 N21C 142.50(16) . . ? N13C Eu2 N21C 63.11(15) . . ? O12B Eu2 N10C 129.92(16) . . ? O15B Eu2 N10C 69.44(16) . . ? O119 Eu2 N10C 117.91(16) . . ? O23C Eu2 N10C 144.42(17) . . ? O999 Eu2 N10C 74.88(16) . . ? O4C Eu2 N10C 63.47(14) . . ? N13C Eu2 N10C 63.16(15) . . ? N21C Eu2 N10C 117.36(15) . . ? O12B Eu2 O203 156.6(4) . . ? O15B Eu2 O203 126.0(4) . . ? O119 Eu2 O203 90.4(4) . . ? O23C Eu2 O203 73.4(4) . . ? O999 Eu2 O203 39.6(4) . . ? O4C Eu2 O203 34.5(4) . . ? N13C Eu2 O203 118.4(4) . . ? N21C Eu2 O203 108.1(4) . . ? N10C Eu2 O203 72.9(4) . . ? O12B Eu2 S201 144.0(2) . . ? O15B Eu2 S201 147.5(3) . . ? O119 Eu2 S201 104.2(3) . . ? O23C Eu2 S201 61.1(2) . . ? O999 Eu2 S201 21.1(3) . . ? O4C Eu2 S201 57.9(3) . . ? N13C Eu2 S201 108.0(3) . . ? N21C Eu2 S201 84.7(3) . . ? N10C Eu2 S201 83.3(2) . . ? O203 Eu2 S201 23.4(3) . . ? C3C O4C O203 95.5(8) . . ? C3C O4C Eu2 121.7(4) . . ? O203 O4C Eu2 87.8(7) . . ? O4C C3C O2C 124.3(6) . . ? O4C C3C C5C 121.9(5) . . ? O2C C3C C5C 113.7(5) . . ? C3C O2C C1C 116.1(5) . . ? N10C C5C C6C 122.4(5) . . ? N10C C5C C3C 112.4(5) . . ? C6C C5C C3C 125.2(5) . . ? C9C N10C C5C 118.3(5) . . ? C9C N10C Eu2 121.4(4) . . ? C5C N10C Eu2 120.3(4) . . ? N10C C9C C8C 122.8(5) . . ? N10C C9C C11C 115.9(5) . . ? C8C C9C C11C 121.1(5) . . ? O12C C11C N13C 128.4(5) . . ? O12C C11C C9C 117.1(5) . . ? N13C C11C C9C 114.4(5) . . ? C11C O12C Eu1 137.2(3) . . ? C9C C8C C7C 119.0(6) . . ? C6C C7C C8C 118.7(5) . . ? C5C C6C C7C 118.7(5) . . ? C22C O23C Eu2 122.3(4) . . ? O23C C22C O24C 126.8(6) . . ? O23C C22C C20C 119.7(5) . . ? O24C C22C C20C 113.5(6) . . ? C22C O24C C25C 114.9(6) . . ? N21C C20C C19C 124.0(6) . . ? N21C C20C C22C 112.8(5) . . ? C19C C20C C22C 123.2(6) . . ? C20C N21C C16C 118.2(5) . . ? C20C N21C Eu2 119.9(4) . . ? C16C N21C Eu2 121.7(4) . . ? N21C C16C C17C 122.6(5) . . ? N21C C16C C14C 116.5(5) . . ? C17C C16C C14C 120.8(5) . . ? C16C C17C C18C 118.0(6) . . ? C19C C18C C17C 120.2(6) . . ? C18C C19C C20C 117.0(6) . . ? C11B O12B Eu2 138.4(4) . . ? O12B C11B N13B 128.2(5) . . ? O12B C11B C9B 116.9(5) . . ? N13B C11B C9B 114.9(5) . . ? C11B N13B C14B 117.9(5) . . ? C11B N13B Eu3 120.3(3) . . ? C14B N13B Eu3 121.8(4) . . ? O12A Eu3 O15A 67.71(12) . . ? O12A Eu3 O68 147.47(14) . . ? O15A Eu3 O68 136.95(13) . . ? O12A Eu3 O111 75.41(14) . . ? O15A Eu3 O111 76.40(14) . . ? O68 Eu3 O111 124.69(14) . . ? O12A Eu3 O23B 137.72(14) . . ? O15A Eu3 O23B 79.41(14) . . ? O68 Eu3 O23B 74.63(14) . . ? O111 Eu3 O23B 71.47(15) . . ? O12A Eu3 O4B 97.35(13) . . ? O15A Eu3 O4B 145.22(14) . . ? O68 Eu3 O4B 71.53(13) . . ? O111 Eu3 O4B 69.33(14) . . ? O23B Eu3 O4B 94.86(15) . . ? O12A Eu3 N13B 76.56(14) . . ? O15A Eu3 N13B 82.95(14) . . ? O68 Eu3 N13B 85.29(14) . . ? O111 Eu3 N13B 149.87(14) . . ? O23B Eu3 N13B 126.07(15) . . ? O4B Eu3 N13B 125.51(13) . . ? O12A Eu3 N10B 74.09(13) . . ? O15A Eu3 N10B 133.56(14) . . ? O68 Eu3 N10B 73.63(13) . . ? O111 Eu3 N10B 118.50(14) . . ? O23B Eu3 N10B 145.93(14) . . ? O4B Eu3 N10B 63.42(14) . . ? N13B Eu3 N10B 62.90(14) . . ? O12A Eu3 N21B 118.46(14) . . ? O15A Eu3 N21B 63.50(14) . . ? O68 Eu3 N21B 74.29(14) . . ? O111 Eu3 N21B 123.60(16) . . ? O23B Eu3 N21B 63.81(17) . . ? O4B Eu3 N21B 143.56(14) . . ? N13B Eu3 N21B 62.67(16) . . ? N10B Eu3 N21B 117.84(16) . . ? C22B O23B Eu3 121.5(5) . . ? O23B C22B O24B 122.5(8) . . ? O23B C22B C20B 121.4(6) . . ? O24B C22B C20B 116.0(7) . . ? C22B O24B C25B 117.1(7) . . ? N21B C20B C19B 120.7(8) . . ? N21B C20B C22B 115.0(6) . . ? C19B C20B C22B 124.2(7) . . ? C20B N21B C16B 120.5(6) . . ? C20B N21B Eu3 117.5(5) . . ? C16B N21B Eu3 120.7(4) . . ? N21B C16B C17B 122.3(6) . . ? N21B C16B C14B 117.1(5) . . ? C17B C16B C14B 120.6(7) . . ? O15B C14B N13B 127.9(6) . . ? O15B C14B C16B 117.8(5) . . ? N13B C14B C16B 114.3(6) . . ? C14B O15B Eu2 137.6(4) . . ? C16B C17B C18B 117.3(9) . . ? C19B C18B C17B 119.7(7) . . ? C18B C19B C20B 119.4(7) . . ? S69 O68 Eu3 148.8(3) . . ? O71 S69 O70 116.3(3) . . ? O71 S69 O68 114.3(3) . . ? O70 S69 O68 114.1(3) . . ? O71 S69 C72 103.6(3) . . ? O70 S69 C72 104.8(3) . . ? O68 S69 C72 101.4(3) . . ? F73 C72 F74 108.1(6) . . ? F73 C72 F75 107.4(5) . . ? F74 C72 F75 107.8(5) . . ? F73 C72 S69 111.6(5) . . ? F74 C72 S69 111.5(5) . . ? F75 C72 S69 110.2(4) . . ? C3B O4B Eu3 121.8(4) . . ? O4B C3B O2B 126.2(5) . . ? O4B C3B C5B 121.5(5) . . ? O2B C3B C5B 112.2(5) . . ? C3B O2B C1B 116.5(5) . . ? N10B C5B C6B 122.9(5) . . ? N10B C5B C3B 112.7(5) . . ? C6B C5B C3B 124.4(5) . . ? C9B N10B C5B 117.5(5) . . ? C9B N10B Eu3 122.0(3) . . ? C5B N10B Eu3 120.5(4) . . ? N10B C9B C8B 123.7(5) . . ? N10B C9B C11B 116.2(5) . . ? C8B C9B C11B 120.0(5) . . ? C7B C8B C9B 118.2(5) . . ? C8B C7B C6B 119.5(5) . . ? C7B C6B C5B 118.2(5) . . ? C11A O12A Eu3 138.0(3) . . ? O12A C11A N13A 128.2(5) . . ? O12A C11A C9A 117.8(5) . . ? N13A C11A C9A 114.0(4) . . ? C14A N13A C11A 117.3(5) . . ? C14A N13A Eu1 122.0(3) . . ? C11A N13A Eu1 120.7(3) . . ? O15A C14A N13A 128.0(5) . . ? O15A C14A C16A 117.5(4) . . ? N13A C14A C16A 114.4(4) . . ? C14A O15A Eu3 137.5(3) . . ? N21A C16A C17A 122.9(5) . . ? N21A C16A C14A 116.6(5) . . ? C17A C16A C14A 120.5(5) . . ? C16A N21A C20A 118.4(5) . . ? C16A N21A Eu1 121.2(3) . . ? C20A N21A Eu1 119.8(4) . . ? N21A C20A C19A 123.0(5) . . ? N21A C20A C22A 112.7(5) . . ? C19A C20A C22A 124.4(5) . . ? C20A C19A C18A 118.5(6) . . ? C17A C18A C19A 119.1(6) . . ? C18A C17A C16A 118.2(6) . . ? O23A C22A O24A 125.5(5) . . ? O23A C22A C20A 120.6(5) . . ? O24A C22A C20A 113.8(5) . . ? C22A O23A Eu1 122.5(4) . . ? C22A O24A C25A 115.8(5) . . ? N10A C9A C8A 123.1(5) . . ? N10A C9A C11A 116.0(4) . . ? C8A C9A C11A 120.9(5) . . ? C5A N10A C9A 118.4(5) . . ? C5A N10A Eu1 120.1(4) . . ? C9A N10A Eu1 121.2(3) . . ? N10A C5A C6A 122.3(5) . . ? N10A C5A C3A 112.9(5) . . ? C6A C5A C3A 124.8(5) . . ? O4A C3A O2A 123.5(5) . . ? O4A C3A C5A 122.3(5) . . ? O2A C3A C5A 114.0(5) . . ? C3A O4A Eu1 120.5(3) . . ? C3A O2A C1A 116.6(5) . . ? C5A C6A C7A 119.4(5) . . ? C8A C7A C6A 118.6(5) . . ? C7A C8A C9A 118.2(5) . . ? S112 O111 Eu3 148.5(3) . . ? O113 S112 O114 116.2(3) . . ? O113 S112 O111 113.1(3) . . ? O114 S112 O111 114.8(3) . . ? O113 S112 C115 104.1(3) . . ? O114 S112 C115 105.1(4) . . ? O111 S112 C115 101.5(3) . . ? F118 C115 F117 109.5(6) . . ? F118 C115 F116 106.4(7) . . ? F117 C115 F116 106.9(7) . . ? F118 C115 S112 111.5(5) . . ? F117 C115 S112 112.2(6) . . ? F116 C115 S112 110.1(5) . . ? S120 O119 Eu2 151.1(3) . . ? O122 S120 O121 116.1(4) . . ? O122 S120 O119 114.1(4) . . ? O121 S120 O119 114.2(3) . . ? O122 S120 C123 104.1(4) . . ? O121 S120 C123 104.6(4) . . ? O119 S120 C123 101.5(3) . . ? F125 C123 F124 107.6(7) . . ? F125 C123 F126 107.9(9) . . ? F124 C123 F126 107.1(8) . . ? F125 C123 S120 110.5(6) . . ? F124 C123 S120 112.3(7) . . ? F126 C123 S120 111.3(6) . . ? S128 O127 Eu1 149.2(2) . . ? O129 S128 O130 117.1(3) . . ? O129 S128 O127 114.0(3) . . ? O130 S128 O127 113.0(3) . . ? O129 S128 C131 104.5(3) . . ? O130 S128 C131 104.1(3) . . ? O127 S128 C131 101.8(3) . . ? F133 C131 F134 108.9(7) . . ? F133 C131 F132 107.9(7) . . ? F134 C131 F132 106.8(6) . . ? F133 C131 S128 112.1(5) . . ? F134 C131 S128 109.4(6) . . ? F132 C131 S128 111.5(5) . . ? S136 O135 S8 34.0(3) . . ? S136 O135 Eu1 156.8(3) . . ? S8 O135 Eu1 136.9(4) . . ? N150 C151 C152 172.2(17) . . ? N165 C166 C167 173.4(19) . . ? N153 C154 C155 174(2) . . ? N156 C157 C158 168(2) . . ? N310 C311 C162 173(2) . . ? N200 C201 C202 159(4) . . ? N307 C306 C305 171(3) . . ? O135 S136 O149 115.6(4) . . ? O135 S136 O138 112.2(3) . . ? O149 S136 O138 117.1(4) . . ? O135 S136 C140 101.7(3) . . ? O149 S136 C140 103.2(4) . . ? O138 S136 C140 104.6(4) . . ? F147 C140 F142 107.5(7) . . ? F147 C140 F143 106.9(7) . . ? F142 C140 F143 106.8(7) . . ? F147 C140 S136 112.1(6) . . ? F142 C140 S136 111.7(5) . . ? F143 C140 S136 111.4(5) . . ? O12 S8 O1 117.9(17) . . ? O12 S8 O135 124.7(13) . . ? O1 S8 O135 104.2(12) . . ? O12 S8 C22 103.2(16) . . ? O1 S8 C22 102.7(17) . . ? O135 S8 C22 100.5(9) . . ? F9 C22 F39 110(2) . . ? F9 C22 F28 99(2) . . ? F39 C22 F28 109(2) . . ? F9 C22 S8 118(2) . . ? F39 C22 S8 110.4(17) . . ? F28 C22 S8 109.2(18) . . ? N6 C1 C1 161.5(16) . 8_554 ? S991 O999 Eu2 150.3(2) . . ? O996 S991 O997 116.2 . . ? O996 S991 O999 114.6 . . ? O997 S991 O999 114.5 . . ? O996 S991 C998 103.3 . . ? O997 S991 C998 104.5 . . ? O999 S991 C998 101.1 . . ? F997 C998 F995 107.5 . . ? F997 C998 F996 107.5 . . ? F995 C998 F996 108.0 . . ? F997 C998 S991 111.8 . . ? F995 C998 S991 111.3 . . ? F996 C998 S991 110.6 . . ? O203 S201 O202 116.2 . . ? O203 S201 O200 114.7 . . ? O202 S201 O200 114.6 . . ? O203 S201 C204 103.3 . . ? O202 S201 C204 104.4 . . ? O200 S201 C204 101.1 . . ? O203 S201 Eu2 66.6(7) . . ? O202 S201 Eu2 78.3(7) . . ? O200 S201 Eu2 86.8(6) . . ? C204 S201 Eu2 169.3(7) . . ? S201 O203 O4C 147.7(12) . . ? S201 O203 Eu2 90.0(8) . . ? O4C O203 Eu2 57.8(6) . . ? F207 C204 F205 107.5 . . ? F207 C204 F206 107.4 . . ? F205 C204 F206 107.9 . . ? F207 C204 S201 111.8 . . ? F205 C204 S201 111.4 . . ? F206 C204 S201 110.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.350 _refine_diff_density_min -1.553 _refine_diff_density_rms 0.156 # Attachment '- Tb1-comp.cif' data_Tb1-comp _database_code_depnum_ccdc_archive 'CCDC 854828' #TrackingRef '- Tb1-comp.cif' # start Validation Reply Form _vrf_PLAT029_tb ; PROBLEM: diffraction theta full too low RESPONSE: The set-up used was not optimal for such a large unit-cell. Due to the fixed detector ( no theta arm), in order to reach a certain resolution, the distance had to be kept short (110 mm) resulting in spots close to each other that the integration software rejected as overlapped, creating imcomplete data. ; _vrf_PLAT601_tb ; PROBLEM: _large void RESPONSE: the squeeze/bypass procedure was used (see _refine_special_details ) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H36 F18 N9 O36 S6 Tb3, 6(C2 H3 N)' _chemical_formula_sum 'C66 H54 F18 N15 O36 S6 Tb3' _chemical_formula_weight 2644.3389 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' '-x+1/2, -y+1/2, z+1' 'x+1/2, y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' '-x+1, -y, z+1' 'x+1/2, y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' '-x+1, -y+1/2, z+1/2' _cell_length_a 55.75(2) _cell_length_b 18.937(15) _cell_length_c 38.852(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 41018(38) _cell_formula_units_Z 16 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 20731.79 _exptl_absorpt_coefficient_mu 2.281 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4498 _exptl_absorpt_correction_T_max 0.6631 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 55 _diffrn_source_current 35 _diffrn_source_power 1.93 _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_reflns_number 60755 _diffrn_reflns_av_R_equivalents 0.1072 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 73 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.93 _reflns_number_total 23410 _reflns_number_gt 17382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS' _computing_cell_refinement 'STOE IPDS' _computing_data_reduction ' STOE IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; One triflate molecule is disordered. It was refined using two component as rigid boby. This model does not completely describe the disorder. Two acetonitrile solvent molecules are included in the model. Their occupancies were refined. The contribution of the other solvent molecules was taken care using the squeeze procedure. The SQUEEZE/BYPASS method was used within Platon(Sluis and Spek, Acta Cryst. (1990). A46, 194-201 ). A void of 11286 A3 (27 percent of the unit.-cell) was located in the unit-cell containing 1378 electrons. These were attributed to about 62 molecules of CH*CN (about 4 per formula) that were added to the 1.92 one included in the model to give a final content rounded to 6 molecules of CH*CN per unit. The values of F00, molecular weight, density and absorption coefficient were corrected according to this new formula. 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^)+(0.1303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(1) _refine_ls_number_reflns 23410 _refine_ls_number_parameters 1217 _refine_ls_number_restraints 317 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb -0.604581(7) -0.49982(3) -1.425477(13) 0.03722(11) Uani 1 1 d . C . O1C O -0.62588(12) -0.4010(4) -1.40303(19) 0.0364(15) Uani 1 1 d . . . C4C C -0.64524(16) -0.3924(7) -1.3863(3) 0.040(2) Uani 1 1 d . D . N2C N -0.66125(16) -0.4414(6) -1.3748(3) 0.044(2) Uani 1 1 d . D . Tb5 Tb -0.702147(8) -0.40714(3) -1.354378(14) 0.04343(13) Uani 1 1 d . . . O23C O -0.72643(12) -0.4710(5) -1.3121(2) 0.0488(19) Uani 1 1 d . D . C22C C -0.71976(18) -0.5260(7) -1.2984(3) 0.047(3) Uani 1 1 d . . . O24C O -0.73156(16) -0.5584(6) -1.2737(3) 0.061(2) Uani 1 1 d . D . C25C C -0.7525(3) -0.5193(11) -1.2600(5) 0.082(5) Uani 1 1 d . . . H25A H -0.7657 -0.5517 -1.2564 0.123 Uiso 1 1 calc R D . H25B H -0.7572 -0.4831 -1.2763 0.123 Uiso 1 1 calc R . . H25C H -0.7482 -0.4974 -1.2382 0.123 Uiso 1 1 calc R . . C18C C -0.69836(18) -0.5638(8) -1.3113(3) 0.046(3) Uani 1 1 d . D . N17C N -0.68713(15) -0.5276(6) -1.3356(3) 0.045(2) Uani 1 1 d . D . C16C C -0.66669(17) -0.5538(7) -1.3496(3) 0.044(2) Uani 1 1 d . . . C15C C -0.65410(19) -0.5102(8) -1.3746(3) 0.048(3) Uani 1 1 d . D . O3C O -0.63745(12) -0.5393(4) -1.3917(2) 0.0383(15) Uani 1 1 d . . . C21C C -0.6575(2) -0.6176(8) -1.3386(4) 0.060(4) Uani 1 1 d . D . H21 H -0.6429 -0.6346 -1.3476 0.072 Uiso 1 1 calc R . . C20C C -0.6699(2) -0.6563(7) -1.3144(4) 0.053(3) Uani 1 1 d . . . H20 H -0.6643 -0.7006 -1.3070 0.064 Uiso 1 1 calc R D . C19C C -0.6911(2) -0.6274(7) -1.3011(3) 0.049(3) Uani 1 1 d . D . H19 H -0.7002 -0.6529 -1.2850 0.059 Uiso 1 1 calc R . . O14C O -0.71558(13) -0.2898(5) -1.3347(2) 0.052(2) Uani 1 1 d . D . C11C C -0.70240(18) -0.2443(8) -1.3335(4) 0.054(3) Uani 1 1 d . . . O12C O -0.70661(15) -0.1780(6) -1.3185(3) 0.062(3) Uani 1 1 d . D . C13C C -0.7295(3) -0.1724(11) -1.2995(4) 0.071(4) Uani 1 1 d . . . H13A H -0.7300 -0.2079 -1.2815 0.107 Uiso 1 1 calc R D . H13B H -0.7428 -0.1799 -1.3152 0.107 Uiso 1 1 calc R . . H13C H -0.7308 -0.1259 -1.2892 0.107 Uiso 1 1 calc R . . C7C C -0.67828(18) -0.2425(7) -1.3516(3) 0.046(3) Uani 1 1 d . D . N6C N -0.67296(15) -0.3102(7) -1.3613(2) 0.050(3) Uani 1 1 d . D . C5C C -0.65135(17) -0.3173(7) -1.3775(3) 0.044(3) Uani 1 1 d . . . C10C C -0.63514(18) -0.2631(6) -1.3822(4) 0.050(3) Uani 1 1 d . D . H10 H -0.6203 -0.2713 -1.3931 0.060 Uiso 1 1 calc R . . C9C C -0.6412(2) -0.1971(7) -1.3708(3) 0.050(3) Uani 1 1 d . . . H9C H -0.6302 -0.1597 -1.3733 0.060 Uiso 1 1 calc R D . C8C C -0.66321(19) -0.1851(7) -1.3554(4) 0.052(3) Uani 1 1 d . D . H8C H -0.6677 -0.1398 -1.3479 0.062 Uiso 1 1 calc R . . O1B O -0.70381(14) -0.3573(5) -1.40888(19) 0.0456(19) Uani 1 1 d . D . C4B C -0.70643(16) -0.3758(6) -1.4409(3) 0.036(2) Uani 1 1 d . . . N2B N -0.70605(15) -0.4429(5) -1.4528(2) 0.0382(18) Uani 1 1 d . D . Tb55 Tb -0.698563(8) -0.46513(3) -1.515605(14) 0.03982(12) Uani 1 1 d . . . O23B O -0.70975(13) -0.5677(4) -1.5489(2) 0.0473(19) Uani 1 1 d . D . C22B C -0.7181(2) -0.6225(8) -1.5355(4) 0.060(4) Uani 1 1 d . . . O24B O -0.72650(19) -0.6788(5) -1.5529(3) 0.064(3) Uani 1 1 d . D . C25B C -0.7252(3) -0.6762(10) -1.5898(5) 0.083(5) Uani 1 1 d . . . H25D H -0.7086 -0.6755 -1.5969 0.124 Uiso 1 1 calc R D . H25E H -0.7332 -0.6339 -1.5980 0.124 Uiso 1 1 calc R . . H25F H -0.7331 -0.7175 -1.5994 0.124 Uiso 1 1 calc R . . C18B C -0.7202(2) -0.6281(6) -1.4976(4) 0.052(3) Uani 1 1 d . D . N17B N -0.71588(15) -0.5657(5) -1.4811(3) 0.047(2) Uani 1 1 d . D . C16B C -0.71573(19) -0.5636(7) -1.4466(3) 0.048(3) Uani 1 1 d . . . C15B C -0.70961(18) -0.4964(7) -1.4294(4) 0.050(3) Uani 1 1 d . D . O3B O -0.70928(14) -0.4942(5) -1.3976(2) 0.051(2) Uani 1 1 d . D . C21B C -0.7212(2) -0.6231(7) -1.4278(5) 0.063(4) Uani 1 1 d . D . H21A H -0.7225 -0.6205 -1.4038 0.076 Uiso 1 1 calc R . . C20B C -0.7250(3) -0.6885(9) -1.4451(5) 0.070(4) Uani 1 1 d . . . H20A H -0.7274 -0.7306 -1.4327 0.084 Uiso 1 1 calc R D . C19B C -0.7250(2) -0.6876(8) -1.4792(4) 0.061(3) Uani 1 1 d . D . H19A H -0.7283 -0.7296 -1.4911 0.073 Uiso 1 1 calc R . . O2F O -0.74065(12) -0.4574(4) -1.52208(19) 0.0416(17) Uani 1 1 d . D . S1F S -0.76366(4) -0.48800(16) -1.53426(8) 0.0445(6) Uani 1 1 d . . . O4F O -0.78449(13) -0.4521(5) -1.5219(2) 0.049(2) Uani 1 1 d . D . O3F O -0.76403(16) -0.5657(5) -1.5333(3) 0.059(2) Uani 1 1 d . D . C5F C -0.76340(18) -0.4678(8) -1.5807(4) 0.053(3) Uani 1 1 d . D . F6F F -0.74417(14) -0.4941(5) -1.5962(2) 0.065(2) Uani 1 1 d . . . F8F F -0.78319(13) -0.4874(5) -1.59573(19) 0.061(2) Uani 1 1 d . . . F7F F -0.76206(12) -0.3949(4) -1.5845(2) 0.0539(17) Uani 1 1 d . . . O14B O -0.70790(13) -0.3835(5) -1.56393(19) 0.0455(19) Uani 1 1 d . D . C11B C -0.71380(16) -0.3213(6) -1.5585(3) 0.041(2) Uani 1 1 d . . . O12B O -0.71987(13) -0.2760(4) -1.5832(2) 0.0443(17) Uani 1 1 d . D . C13B C -0.7178(2) -0.2961(8) -1.6182(4) 0.053(3) Uani 1 1 d . . . H13D H -0.7015 -0.3121 -1.6227 0.080 Uiso 1 1 calc R D . H13E H -0.7214 -0.2559 -1.6328 0.080 Uiso 1 1 calc R . . H13F H -0.7289 -0.3341 -1.6231 0.080 Uiso 1 1 calc R . . C7B C -0.71493(17) -0.2920(7) -1.5228(3) 0.045(3) Uani 1 1 d . D . N6B N -0.70972(15) -0.3414(5) -1.4993(2) 0.041(2) Uani 1 1 d . D . C5B C -0.71094(16) -0.3193(7) -1.4663(3) 0.041(2) Uani 1 1 d . D . C10B C -0.7164(2) -0.2528(6) -1.4562(3) 0.044(2) Uani 1 1 d . . . H10A H -0.7169 -0.2405 -1.4328 0.052 Uiso 1 1 calc R D . C9B C -0.7214(2) -0.2030(6) -1.4821(3) 0.045(2) Uani 1 1 d . D . H9B H -0.7247 -0.1559 -1.4761 0.054 Uiso 1 1 calc R . . C8B C -0.72128(18) -0.2234(7) -1.5164(4) 0.049(3) Uani 1 1 d . . . H8B H -0.7253 -0.1920 -1.5342 0.058 Uiso 1 1 calc R D . O1A O -0.66267(11) -0.4107(4) -1.4974(2) 0.0384(16) Uani 1 1 d . D . C4A C -0.64319(18) -0.4290(6) -1.4843(3) 0.038(2) Uani 1 1 d . . . N2A N -0.63821(14) -0.4912(5) -1.4673(3) 0.0403(19) Uani 1 1 d . C . C15A C -0.65149(17) -0.5475(6) -1.4765(3) 0.039(2) Uani 1 1 d . . . O3A O -0.67061(12) -0.5486(4) -1.4943(2) 0.0439(18) Uani 1 1 d . D . C16A C -0.64191(17) -0.6175(7) -1.4642(3) 0.042(2) Uani 1 1 d . D . N17A N -0.62127(15) -0.6130(6) -1.4478(2) 0.042(2) Uani 1 1 d . . . C18A C -0.61144(18) -0.6762(7) -1.4364(4) 0.050(3) Uani 1 1 d . D . C19A C -0.6210(2) -0.7418(7) -1.4448(3) 0.051(3) Uani 1 1 d . . . H19B H -0.6127 -0.7838 -1.4397 0.062 Uiso 1 1 calc R D . C20A C -0.6436(3) -0.7434(8) -1.4611(4) 0.065(4) Uani 1 1 d . D . H20B H -0.6521 -0.7858 -1.4636 0.078 Uiso 1 1 calc R . . C21A C -0.6528(2) -0.6791(9) -1.4736(4) 0.056(3) Uani 1 1 d . . . H21B H -0.6663 -0.6785 -1.4882 0.067 Uiso 1 1 calc R D . C22A C -0.58837(19) -0.6667(8) -1.4185(3) 0.047(3) Uani 1 1 d . . . O23A O -0.58194(13) -0.6069(5) -1.4089(2) 0.0469(19) Uani 1 1 d . C . O24A O -0.57591(13) -0.7236(5) -1.4152(2) 0.0448(18) Uani 1 1 d . D . C25A C -0.5535(2) -0.7165(9) -1.3954(4) 0.063(4) Uani 1 1 d . . . H25G H -0.5571 -0.7018 -1.3721 0.094 Uiso 1 1 calc R D . H25H H -0.5433 -0.6815 -1.4063 0.094 Uiso 1 1 calc R . . H25I H -0.5452 -0.7616 -1.3949 0.094 Uiso 1 1 calc R . . C5A C -0.62325(16) -0.3779(8) -1.4843(3) 0.048(3) Uani 1 1 d . D . N6A N -0.60409(13) -0.3958(6) -1.4645(2) 0.044(2) Uani 1 1 d . . . C7A C -0.5854(2) -0.3507(7) -1.4653(3) 0.048(3) Uani 1 1 d . D . C11A C -0.56603(17) -0.3751(9) -1.4425(3) 0.054(3) Uani 1 1 d . . . O14A O -0.56766(13) -0.4255(5) -1.4237(2) 0.0452(17) Uani 1 1 d . C . O12A O -0.54626(13) -0.3342(5) -1.4437(2) 0.054(2) Uani 1 1 d . D . C13A C -0.5274(2) -0.3514(9) -1.4212(4) 0.066(4) Uani 1 1 d . . . H13G H -0.5340 -0.3683 -1.3996 0.099 Uiso 1 1 calc R D . H13H H -0.5177 -0.3099 -1.4170 0.099 Uiso 1 1 calc R . . H13I H -0.5176 -0.3881 -1.4314 0.099 Uiso 1 1 calc R . . C8A C -0.5848(2) -0.2880(7) -1.4848(3) 0.051(3) Uani 1 1 d . . . H8A H -0.5712 -0.2586 -1.4841 0.061 Uiso 1 1 calc R D . C9A C -0.60458(19) -0.2697(7) -1.5053(4) 0.055(3) Uani 1 1 d . D . H9A H -0.6047 -0.2279 -1.5184 0.065 Uiso 1 1 calc R . . C10A C -0.6243(2) -0.3164(6) -1.5055(3) 0.047(3) Uani 1 1 d . . . H10B H -0.6378 -0.3073 -1.5193 0.056 Uiso 1 1 calc R D . O4D O -0.67071(12) -0.4805(5) -1.5626(2) 0.0466(19) Uani 1 1 d . D . S1D S -0.64720(5) -0.50337(18) -1.57426(8) 0.0466(6) Uani 1 1 d . . . O2D O -0.63993(15) -0.4670(5) -1.6046(2) 0.055(2) Uani 1 1 d . D . O3D O -0.62970(16) -0.5103(6) -1.5475(2) 0.061(3) Uani 1 1 d . D . C5D C -0.6529(2) -0.5930(8) -1.5882(4) 0.058(3) Uani 1 1 d . D . F6D F -0.63372(18) -0.6215(6) -1.6034(3) 0.094(4) Uani 1 1 d . . . F8D F -0.66038(16) -0.6364(5) -1.5633(3) 0.075(2) Uani 1 1 d . . . F7D F -0.6707(2) -0.5950(5) -1.6121(2) 0.078(3) Uani 1 1 d . . . O0AA O -0.74369(13) -0.3987(5) -1.3676(2) 0.052(2) Uani 1 1 d . D . S0AA S -0.76447(5) -0.4099(2) -1.39096(9) 0.0571(8) Uani 1 1 d . . . O4G O -0.75817(15) -0.4328(7) -1.4242(3) 0.068(3) Uani 1 1 d . D . O3G O -0.78184(18) -0.3559(8) -1.3896(3) 0.080(4) Uani 1 1 d . D . C5G C -0.7790(2) -0.4842(14) -1.3698(5) 0.087(6) Uani 1 1 d . D . F6G F -0.78558(16) -0.4715(6) -1.3378(2) 0.079(3) Uani 1 1 d . . . F8G F -0.7992(2) -0.5038(8) -1.3870(3) 0.109(5) Uani 1 1 d . . . F7G F -0.7652(2) -0.5411(7) -1.3705(3) 0.094(3) Uani 1 1 d . . . O2H O -0.59093(12) -0.4871(5) -1.3683(2) 0.0427(17) Uani 1 1 d . . . S1H S -0.59599(4) -0.47574(19) -1.33201(7) 0.0453(6) Uani 1 1 d . D . O3H O -0.62081(13) -0.4653(6) -1.3246(2) 0.052(2) Uani 1 1 d . . . O4H O -0.58308(14) -0.5211(6) -1.3092(2) 0.052(2) Uani 1 1 d . . . C5H C -0.5824(2) -0.3899(7) -1.3261(4) 0.051(3) Uani 1 1 d . . . F7H F -0.55940(13) -0.3906(4) -1.3335(2) 0.062(2) Uani 1 1 d . D . F6H F -0.59263(18) -0.3408(4) -1.3450(3) 0.092(4) Uani 1 1 d . D . F8H F -0.58389(19) -0.3710(8) -1.2932(3) 0.104(4) Uani 1 1 d . D . N150 N -0.8340(4) -0.5774(11) -1.4478(8) 0.118(9) Uani 0.92(3) 1 d P A 30 C151 C -0.8132(6) -0.5904(11) -1.4531(5) 0.087(7) Uani 0.92(3) 1 d P A 30 C152 C -0.7872(3) -0.5911(10) -1.4544(5) 0.070(5) Uani 0.92(3) 1 d P A 30 H15A H -0.7820 -0.5867 -1.4782 0.105 Uiso 0.92(3) 1 calc PR A 30 H15B H -0.7813 -0.6352 -1.4449 0.105 Uiso 0.92(3) 1 calc PR A 30 H15C H -0.7809 -0.5519 -1.4411 0.105 Uiso 0.92(3) 1 calc PR A 30 N1 N -0.6625(6) -0.2498(15) -1.4541(9) 0.042(11) Uiso 0.28(4) 1 d PDU B 2 C1 C -0.6647(6) -0.1872(16) -1.4567(8) 0.028(9) Uiso 0.28(4) 1 d PDU B 2 C0AA C -0.6687(9) -0.108(2) -1.4552(13) 0.051(12) Uiso 0.28(4) 1 d PDU B 2 H0AA H -0.6696 -0.0897 -1.4784 0.076 Uiso 0.28(4) 1 calc PR B 2 H0AB H -0.6556 -0.0863 -1.4431 0.076 Uiso 0.28(4) 1 calc PR B 2 H0AC H -0.6837 -0.0988 -1.4433 0.076 Uiso 0.28(4) 1 calc PR B 2 O1LM O -0.58016(13) -0.5292(5) -1.4747(2) 0.0451(17) Uani 1 1 d . . . S1L S -0.56360(5) -0.57322(19) -1.49378(8) 0.0506(7) Uani 1 1 d . C 21 O2L O -0.56389(18) -0.6461(5) -1.4833(3) 0.063(2) Uani 1 1 d . C 21 O4L O -0.5639(2) -0.5581(6) -1.5302(3) 0.068(3) Uani 1 1 d . C 21 C5L C -0.5341(2) -0.5392(7) -1.4786(3) 0.049(3) Uani 1 1 d . C 21 F6L F -0.53016(16) -0.5549(7) -1.4459(3) 0.085(3) Uani 1 1 d . C 21 F7L F -0.51694(15) -0.5690(7) -1.4973(3) 0.091(3) Uani 1 1 d . C 21 F8L F -0.53266(15) -0.4741(5) -1.4841(2) 0.067(2) Uani 1 1 d . C 21 OQA O -0.68320(15) -0.3692(4) -1.29934(15) 0.077(4) Uani 0.632(9) 1 d PGU D 23 S1Q S -0.67892(10) -0.3413(3) -1.26736(13) 0.0733(18) Uani 0.632(9) 1 d PGU D 23 O3Q O -0.67852(17) -0.2674(3) -1.27703(19) 0.125(7) Uani 0.632(9) 1 d PGU D 23 O4Q O -0.65993(11) -0.3622(6) -1.24378(18) 0.095(6) Uani 0.632(9) 1 d PGU D 23 C5Q C -0.70566(12) -0.3503(5) -1.24048(17) 0.091(4) Uani 0.632(9) 1 d PGU D 23 F6Q F -0.72524(10) -0.3374(7) -1.2587(2) 0.112(5) Uani 0.632(9) 1 d PGU D 23 F8Q F -0.7052(2) -0.3061(6) -1.21351(19) 0.108(5) Uani 0.632(9) 1 d PGU D 23 F7Q F -0.70772(16) -0.4151(5) -1.2279(2) 0.102(5) Uani 0.632(9) 1 d PGU D 23 N0AA N -0.6556(4) -0.2220(16) -1.4580(3) 0.137(12) Uiso 0.72(4) 1 d PGDU B 1 C2AA C -0.6611(4) -0.1620(16) -1.4568(4) 0.120(12) Uiso 0.72(4) 1 d PGDU B 1 C1AA C -0.6722(5) -0.0912(15) -1.4527(5) 0.148(19) Uiso 0.72(4) 1 d PGDU B 1 H1AA H -0.6752 -0.0710 -1.4752 0.222 Uiso 0.72(4) 1 calc PR B 1 H1AB H -0.6613 -0.0608 -1.4400 0.222 Uiso 0.72(4) 1 calc PR B 1 H1AC H -0.6871 -0.0956 -1.4401 0.222 Uiso 0.72(4) 1 calc PR B 1 O1AA O -0.6844(3) -0.3957(10) -1.2945(4) 0.043(4) Uani 0.368(9) 1 d PGU D 25 S1AA S -0.7006(2) -0.3626(7) -1.2778(3) 0.116(4) Uani 0.368(9) 1 d PGU D 25 F0AA F -0.7189(2) -0.3684(9) -1.2199(3) 0.048(4) Uani 0.368(9) 1 d PGU D 25 F1AA F -0.6843(3) -0.3989(14) -1.2217(4) 0.129(10) Uani 0.368(9) 1 d PGU D 25 F2AA F -0.7108(4) -0.4632(7) -1.2403(5) 0.148(12) Uani 0.368(9) 1 d PGU D 25 O2AA O -0.6943(4) -0.2943(7) -1.2698(5) 0.122(9) Uani 0.368(9) 1 d PGU D 25 O3AA O -0.7229(3) -0.3658(14) -1.2918(4) 0.142(10) Uani 0.368(9) 1 d PGU D 25 C3AA C -0.7036(2) -0.4002(7) -1.2379(3) 0.100(8) Uani 0.368(9) 1 d PGU D 25 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02549(17) 0.0456(3) 0.0406(2) 0.0013(2) -0.00095(17) -0.00036(18) O1C 0.031(3) 0.034(4) 0.045(4) 0.012(3) 0.002(3) 0.001(3) C4C 0.030(4) 0.059(7) 0.032(5) -0.006(5) 0.001(3) -0.003(4) N2C 0.038(4) 0.046(6) 0.049(5) 0.018(4) -0.008(4) 0.001(4) Tb5 0.02981(19) 0.0535(3) 0.0470(3) 0.0043(2) 0.00346(18) 0.0016(2) O23C 0.029(3) 0.063(6) 0.055(5) -0.004(4) 0.009(3) 0.002(3) C22C 0.031(4) 0.051(7) 0.058(7) 0.006(6) -0.001(4) 0.004(4) O24C 0.050(4) 0.064(6) 0.069(6) 0.008(5) 0.018(4) -0.001(4) C25C 0.052(7) 0.098(13) 0.097(13) 0.014(11) 0.036(8) 0.024(8) C18C 0.036(4) 0.067(8) 0.034(5) 0.006(5) 0.005(4) -0.016(5) N17C 0.035(4) 0.054(6) 0.045(5) 0.017(4) 0.003(3) -0.009(4) C16C 0.030(4) 0.049(6) 0.053(6) 0.003(5) 0.011(4) 0.009(4) C15C 0.034(5) 0.082(9) 0.027(5) 0.001(5) -0.001(3) -0.002(5) O3C 0.030(3) 0.033(4) 0.052(4) 0.011(3) 0.006(3) 0.002(3) C21C 0.036(5) 0.063(9) 0.082(9) 0.025(7) 0.008(5) 0.017(5) C20C 0.046(5) 0.035(6) 0.079(9) 0.006(6) 0.006(5) 0.000(5) C19C 0.048(5) 0.043(6) 0.057(7) 0.018(5) -0.006(5) -0.023(5) O14C 0.030(3) 0.061(6) 0.066(5) -0.015(5) 0.003(3) 0.001(3) C11C 0.027(4) 0.064(8) 0.070(8) -0.029(7) 0.002(4) 0.010(5) O12C 0.040(4) 0.080(7) 0.067(6) -0.035(5) 0.005(4) 0.008(4) C13C 0.052(7) 0.107(14) 0.054(7) -0.009(8) 0.004(6) 0.016(8) C7C 0.029(4) 0.073(8) 0.035(5) 0.006(5) -0.001(4) -0.012(5) N6C 0.033(4) 0.075(7) 0.043(5) -0.010(5) 0.003(3) 0.017(4) C5C 0.030(4) 0.055(7) 0.047(6) 0.009(5) -0.001(4) 0.016(4) C10C 0.029(4) 0.034(6) 0.087(9) 0.000(6) 0.008(5) 0.001(4) C9C 0.052(6) 0.036(6) 0.060(7) -0.008(5) -0.009(5) 0.002(5) C8C 0.040(5) 0.044(6) 0.071(8) 0.009(6) 0.000(5) 0.000(5) O1B 0.048(4) 0.053(5) 0.036(4) 0.030(4) 0.002(3) -0.003(3) C4B 0.031(4) 0.041(6) 0.036(5) 0.012(4) -0.003(3) -0.002(4) N2B 0.040(4) 0.024(4) 0.050(5) -0.001(4) -0.003(3) -0.009(3) Tb55 0.02837(18) 0.0428(3) 0.0483(3) 0.0012(2) -0.00523(18) -0.00402(18) O23B 0.037(3) 0.033(4) 0.072(5) 0.002(4) -0.004(3) -0.010(3) C22B 0.044(6) 0.051(8) 0.085(10) -0.021(7) -0.017(6) 0.003(5) O24B 0.067(5) 0.032(5) 0.094(8) -0.009(5) -0.019(5) -0.012(4) C25B 0.077(10) 0.067(11) 0.105(14) -0.020(10) -0.022(9) -0.029(8) C18B 0.042(5) 0.027(5) 0.087(9) 0.005(6) -0.008(5) -0.005(4) N17B 0.031(4) 0.043(5) 0.066(6) 0.011(5) -0.019(4) -0.004(4) C16B 0.037(5) 0.056(7) 0.052(6) 0.000(6) -0.010(4) -0.002(5) C15B 0.035(4) 0.039(6) 0.076(9) 0.018(6) -0.007(5) -0.015(4) O3B 0.041(4) 0.062(6) 0.049(5) 0.011(4) 0.006(3) -0.007(4) C21B 0.057(7) 0.045(7) 0.087(10) 0.022(7) -0.006(7) -0.025(6) C20B 0.061(8) 0.059(9) 0.090(11) 0.022(8) -0.001(7) -0.021(7) C19B 0.049(6) 0.052(8) 0.082(10) 0.005(7) -0.002(6) -0.008(6) O2F 0.038(3) 0.045(4) 0.042(4) 0.012(3) -0.019(3) -0.001(3) S1F 0.0291(10) 0.0459(16) 0.0586(16) 0.0006(13) -0.0079(10) -0.0056(10) O4F 0.039(3) 0.066(6) 0.042(4) 0.009(4) -0.006(3) 0.001(3) O3F 0.048(4) 0.041(5) 0.087(7) 0.000(5) -0.008(4) -0.009(4) C5F 0.029(4) 0.067(8) 0.064(7) 0.001(7) -0.006(4) 0.004(5) F6F 0.050(4) 0.083(6) 0.063(5) -0.005(4) 0.000(3) 0.013(4) F8F 0.054(4) 0.076(6) 0.051(4) -0.012(4) -0.026(3) -0.013(4) F7F 0.046(3) 0.060(5) 0.056(4) 0.007(4) -0.014(3) -0.001(3) O14B 0.037(3) 0.067(6) 0.032(3) -0.006(4) 0.005(3) -0.002(3) C11B 0.024(4) 0.045(6) 0.054(6) 0.016(5) -0.002(4) 0.000(4) O12B 0.045(4) 0.040(4) 0.049(4) 0.017(4) -0.009(3) -0.003(3) C13B 0.046(6) 0.054(8) 0.060(7) -0.002(6) 0.003(5) 0.012(5) C7B 0.028(4) 0.052(7) 0.055(7) 0.004(5) 0.002(4) -0.006(4) N6B 0.035(4) 0.053(6) 0.034(4) 0.000(4) 0.002(3) -0.015(4) C5B 0.026(4) 0.050(6) 0.047(6) 0.014(5) -0.001(4) -0.006(4) C10B 0.044(5) 0.043(6) 0.045(6) -0.003(5) -0.005(4) -0.011(4) C9B 0.048(5) 0.025(5) 0.061(7) 0.010(5) 0.003(5) 0.005(4) C8B 0.036(4) 0.053(7) 0.057(6) -0.001(6) 0.005(5) 0.012(4) O1A 0.025(3) 0.042(4) 0.048(4) -0.009(3) -0.014(3) 0.000(3) C4A 0.045(5) 0.031(5) 0.038(5) -0.009(4) 0.007(4) 0.004(4) N2A 0.028(3) 0.041(5) 0.052(5) 0.002(4) -0.002(3) -0.005(3) C15A 0.032(4) 0.044(6) 0.040(5) 0.007(4) 0.010(4) 0.002(4) O3A 0.027(3) 0.049(5) 0.056(4) 0.013(4) -0.016(3) -0.006(3) C16A 0.031(4) 0.045(6) 0.050(6) 0.015(5) -0.006(4) -0.001(4) N17A 0.033(4) 0.054(6) 0.039(4) -0.003(4) -0.004(3) -0.002(4) C18A 0.028(4) 0.058(7) 0.064(7) -0.003(6) -0.005(4) 0.003(4) C19A 0.064(7) 0.042(7) 0.048(6) 0.001(5) -0.013(5) 0.007(5) C20A 0.066(8) 0.052(8) 0.078(9) 0.006(7) -0.034(7) -0.026(6) C21A 0.040(5) 0.073(9) 0.055(7) 0.002(7) -0.009(5) -0.001(5) C22A 0.038(5) 0.072(8) 0.032(5) 0.005(5) 0.008(4) -0.002(5) O23A 0.036(3) 0.060(5) 0.044(4) 0.001(4) -0.008(3) 0.000(3) O24A 0.035(3) 0.042(4) 0.058(5) 0.000(4) -0.004(3) 0.003(3) C25A 0.037(5) 0.083(11) 0.068(8) 0.016(8) -0.018(5) 0.009(6) C5A 0.025(4) 0.089(10) 0.031(5) -0.012(5) -0.010(3) -0.006(5) N6A 0.025(3) 0.070(7) 0.036(4) -0.011(4) 0.000(3) 0.004(4) C7A 0.049(5) 0.058(7) 0.037(5) 0.016(5) -0.019(4) -0.023(5) C11A 0.028(4) 0.097(11) 0.035(5) 0.008(6) 0.007(4) -0.002(5) O14A 0.040(3) 0.056(5) 0.040(4) 0.005(4) -0.001(3) 0.002(3) O12A 0.037(4) 0.066(6) 0.058(5) 0.014(4) -0.008(3) -0.021(4) C13A 0.036(5) 0.090(11) 0.072(9) -0.003(8) -0.013(5) -0.028(6) C8A 0.053(6) 0.054(7) 0.047(6) 0.004(5) -0.013(5) -0.015(5) C9A 0.034(5) 0.041(6) 0.089(10) 0.015(6) -0.005(5) -0.013(4) C10A 0.044(5) 0.030(5) 0.068(8) 0.008(5) 0.004(5) -0.007(4) O4D 0.026(3) 0.063(5) 0.051(4) 0.017(4) -0.005(3) -0.001(3) S1D 0.0355(11) 0.0557(17) 0.0487(15) 0.0014(13) 0.0033(10) -0.0011(11) O2D 0.047(4) 0.064(6) 0.053(5) 0.001(5) 0.010(4) -0.005(4) O3D 0.044(4) 0.091(8) 0.048(5) -0.014(5) 0.002(3) -0.003(4) C5D 0.054(6) 0.053(8) 0.069(8) 0.005(7) 0.013(6) 0.010(6) F6D 0.077(6) 0.068(6) 0.138(9) -0.038(7) 0.044(6) -0.012(5) F8D 0.065(5) 0.068(6) 0.091(6) 0.011(5) 0.004(4) 0.000(4) F7D 0.122(8) 0.048(5) 0.063(5) -0.009(4) -0.010(5) -0.014(5) O0AA 0.032(3) 0.063(6) 0.061(5) 0.000(4) 0.000(3) -0.004(4) S0AA 0.0288(10) 0.083(2) 0.0596(18) 0.0175(17) -0.0026(11) -0.0028(13) O4G 0.042(4) 0.109(9) 0.053(5) 0.034(6) -0.006(4) -0.008(5) O3G 0.052(5) 0.125(11) 0.063(6) 0.035(7) 0.006(4) 0.019(6) C5G 0.036(6) 0.15(2) 0.070(10) 0.012(11) -0.018(6) -0.013(9) F6G 0.068(5) 0.117(8) 0.052(5) 0.018(5) 0.005(4) -0.028(5) F8G 0.081(7) 0.166(13) 0.079(7) 0.004(7) -0.010(5) -0.072(8) F7G 0.088(7) 0.093(9) 0.101(8) 0.011(7) 0.000(6) -0.029(6) O2H 0.032(3) 0.052(5) 0.044(4) -0.003(3) -0.001(3) -0.015(3) S1H 0.0304(10) 0.0668(19) 0.0387(13) 0.0004(13) 0.0001(9) 0.0057(11) O3H 0.032(3) 0.088(7) 0.036(4) -0.003(4) 0.003(3) 0.009(4) O4H 0.038(4) 0.070(6) 0.048(4) 0.019(4) 0.000(3) 0.008(4) C5H 0.038(5) 0.041(6) 0.075(8) -0.001(6) -0.015(5) 0.009(4) F7H 0.047(3) 0.047(4) 0.093(6) -0.011(4) 0.005(4) -0.009(3) F6H 0.080(6) 0.037(4) 0.160(11) 0.006(5) -0.058(7) 0.005(4) F8H 0.071(6) 0.175(13) 0.066(6) -0.036(7) -0.012(5) 0.024(7) N150 0.100(14) 0.073(13) 0.18(3) -0.018(14) -0.025(14) -0.045(11) C151 0.14(2) 0.052(11) 0.070(12) 0.014(9) -0.003(12) -0.009(12) C152 0.086(11) 0.060(11) 0.063(10) 0.015(8) 0.008(8) 0.011(8) O1LM 0.040(4) 0.046(5) 0.049(4) -0.003(4) 0.009(3) -0.001(3) S1L 0.0436(13) 0.0608(19) 0.0473(15) 0.0000(14) 0.0039(11) 0.0121(13) O2L 0.065(5) 0.049(6) 0.076(6) 0.015(5) 0.002(5) 0.009(4) O4L 0.074(6) 0.074(7) 0.056(5) -0.010(5) 0.006(5) 0.022(5) C5L 0.038(5) 0.051(7) 0.057(7) 0.001(6) 0.003(4) 0.004(5) F6L 0.060(5) 0.117(9) 0.078(6) 0.029(6) -0.019(4) -0.016(5) F7L 0.049(4) 0.107(9) 0.116(8) -0.005(7) 0.015(5) 0.010(5) F8L 0.063(4) 0.058(5) 0.081(6) 0.004(4) 0.009(4) -0.010(4) OQA 0.071(8) 0.104(10) 0.056(6) 0.014(7) -0.008(6) -0.001(8) S1Q 0.084(4) 0.079(4) 0.057(3) 0.003(3) -0.010(3) 0.018(3) O3Q 0.19(2) 0.090(9) 0.092(14) 0.034(9) 0.015(14) -0.029(13) O4Q 0.100(9) 0.125(15) 0.061(9) -0.034(10) -0.032(8) 0.018(12) C5Q 0.093(7) 0.095(10) 0.086(9) 0.005(8) 0.001(6) -0.003(9) F6Q 0.097(7) 0.129(13) 0.109(11) -0.007(10) -0.019(8) 0.052(9) F8Q 0.147(14) 0.101(11) 0.077(9) -0.002(8) 0.011(8) -0.007(12) F7Q 0.077(9) 0.077(9) 0.154(14) 0.015(8) -0.005(9) 0.002(8) O1AA 0.040(7) 0.039(9) 0.051(9) 0.011(8) 0.009(7) -0.002(7) S1AA 0.104(7) 0.114(8) 0.131(8) -0.002(8) 0.006(7) -0.009(7) F0AA 0.033(7) 0.053(9) 0.059(9) -0.041(8) 0.006(6) 0.004(7) F1AA 0.121(18) 0.116(19) 0.15(2) -0.001(18) -0.007(18) -0.015(17) F2AA 0.14(2) 0.15(2) 0.15(2) -0.02(2) -0.04(2) 0.01(2) O2AA 0.151(19) 0.114(18) 0.101(17) 0.005(17) -0.008(17) -0.008(18) O3AA 0.126(17) 0.146(18) 0.155(18) -0.003(17) -0.019(17) 0.012(17) C3AA 0.095(14) 0.099(16) 0.106(15) 0.013(15) -0.005(14) 0.008(15) _geom_special_details ; The acetonitrile solvent molecules are disordered. Only two sites were kept in the final model, the rest of the solvent was taken care using the SQUEEZE/BYPASS method was used within Platon(Sluis and Spek, Acta Cryst. (1990). A46, 194-201 ). A void of 11286 A3 (27 percent of the unit.-cell) was located in the unit-cell containing 1378 electrons. These were attributed to about 62 molecules of CH*CN (about 4 per formula) that were added to the 1.92 one included in the model to give a final content rounded to 6 molecules of CH*CN per unit. The values of F00, molecular weight, density and absorption coefficient were corrected according to this new formula. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O2H 2.362(8) . ? Tb1 O3C 2.375(7) . ? Tb1 O1C 2.382(8) . ? Tb1 O1LM 2.414(8) . ? Tb1 O23A 2.474(9) . ? Tb1 N6A 2.485(11) . ? Tb1 N2A 2.487(9) . ? Tb1 N17A 2.492(10) . ? Tb1 O14A 2.495(8) . ? O1C C4C 1.270(12) . ? C4C N2C 1.363(15) . ? C4C C5C 1.501(17) . ? N2C C15C 1.364(17) . ? N2C Tb5 2.500(10) . ? Tb5 O1B 2.321(7) . ? Tb5 O0AA 2.378(8) . ? Tb5 O3B 2.387(10) . ? Tb5 O23C 2.447(8) . ? Tb5 O14C 2.465(9) . ? Tb5 N6C 2.467(12) . ? Tb5 OQA 2.491(6) . ? Tb5 O1AA 2.536(17) . ? Tb5 N17C 2.537(11) . ? Tb5 O3AA 2.803(17) . ? Tb5 S1AA 3.094(13) . ? O23C C22C 1.227(15) . ? C22C O24C 1.318(15) . ? C22C C18C 1.479(16) . ? O24C C25C 1.481(16) . ? C18C N17C 1.324(13) . ? C18C C19C 1.330(18) . ? N17C C16C 1.357(13) . ? C16C C21C 1.381(17) . ? C16C C15C 1.456(16) . ? C15C O3C 1.267(14) . ? C21C C20C 1.379(19) . ? C20C C19C 1.399(18) . ? O14C C11C 1.133(16) . ? C11C O12C 1.404(16) . ? C11C C7C 1.519(14) . ? O12C C13C 1.481(16) . ? C7C N6C 1.370(17) . ? C7C C8C 1.381(17) . ? N6C C5C 1.365(13) . ? C5C C10C 1.381(17) . ? C10C C9C 1.368(16) . ? C9C C8C 1.385(17) . ? O1B C4B 1.301(13) . ? C4B N2B 1.351(14) . ? C4B C5B 1.478(14) . ? N2B C15B 1.374(15) . ? N2B Tb55 2.511(10) . ? Tb55 O1A 2.360(6) . ? Tb55 O2F 2.365(7) . ? Tb55 O3A 2.368(7) . ? Tb55 O4D 2.413(8) . ? Tb55 O23B 2.415(9) . ? Tb55 O14B 2.487(9) . ? Tb55 N6B 2.505(11) . ? Tb55 N17B 2.521(10) . ? O23B C22B 1.252(18) . ? C22B O24B 1.346(16) . ? C22B C18B 1.48(2) . ? O24B C25B 1.44(2) . ? C18B C19B 1.359(19) . ? C18B N17B 1.365(16) . ? N17B C16B 1.341(17) . ? C16B C21B 1.377(18) . ? C16B C15B 1.478(19) . ? C15B O3B 1.238(17) . ? C21B C20B 1.42(2) . ? C20B C19B 1.33(2) . ? O2F S1F 1.485(7) . ? S1F O4F 1.429(9) . ? S1F O3F 1.473(10) . ? S1F C5F 1.845(14) . ? C5F F8F 1.302(13) . ? C5F F6F 1.326(14) . ? C5F F7F 1.391(16) . ? O14B C11B 1.241(15) . ? C11B O12B 1.329(13) . ? C11B C7B 1.497(18) . ? O12B C13B 1.419(16) . ? C7B N6B 1.338(16) . ? C7B C8B 1.369(18) . ? N6B C5B 1.351(15) . ? C5B C10B 1.354(17) . ? C10B C9B 1.406(17) . ? C9B C8B 1.390(19) . ? O1A C4A 1.248(12) . ? C4A N2A 1.379(15) . ? C4A C5A 1.474(16) . ? N2A C15A 1.346(15) . ? C15A O3A 1.272(12) . ? C15A C16A 1.506(15) . ? C16A N17A 1.318(13) . ? C16A C21A 1.365(19) . ? N17A C18A 1.389(16) . ? C18A C19A 1.390(18) . ? C18A C22A 1.473(15) . ? C19A C20A 1.410(17) . ? C20A C21A 1.41(2) . ? C22A O23A 1.246(16) . ? C22A O24A 1.289(16) . ? O24A C25A 1.474(13) . ? C5A N6A 1.360(12) . ? C5A C10A 1.428(18) . ? N6A C7A 1.349(14) . ? C7A C8A 1.409(17) . ? C7A C11A 1.472(15) . ? C11A O14A 1.202(16) . ? C11A O12A 1.349(14) . ? O12A C13A 1.405(15) . ? C8A C9A 1.404(17) . ? C9A C10A 1.412(14) . ? O4D S1D 1.453(8) . ? S1D O2D 1.424(10) . ? S1D O3D 1.432(10) . ? S1D C5D 1.811(16) . ? C5D F8D 1.335(17) . ? C5D F6D 1.336(16) . ? C5D F7D 1.359(18) . ? O0AA S0AA 1.487(9) . ? S0AA O4G 1.406(12) . ? S0AA O3G 1.410(12) . ? S0AA C5G 1.82(2) . ? C5G F6G 1.32(2) . ? C5G F7G 1.33(2) . ? C5G F8G 1.360(16) . ? O2H S1H 1.452(8) . ? S1H O3H 1.427(7) . ? S1H O4H 1.429(9) . ? S1H C5H 1.809(14) . ? C5H F7H 1.313(14) . ? C5H F6H 1.314(15) . ? C5H F8H 1.332(17) . ? N150 C151 1.20(3) . ? C151 C152 1.45(4) . ? N1 C1 1.196(19) . ? C1 C0AA 1.51(4) . ? O1LM S1L 1.447(8) . ? S1L O2L 1.438(11) . ? S1L O4L 1.444(11) . ? S1L C5L 1.862(13) . ? C5L F8L 1.255(16) . ? C5L F6L 1.323(16) . ? C5L F7L 1.327(15) . ? OQA S1Q 1.3707 . ? S1Q O3Q 1.4488 . ? S1Q O4Q 1.4551 . ? S1Q C5Q 1.8281 . ? C5Q F6Q 1.3238 . ? C5Q F7Q 1.3256 . ? C5Q F8Q 1.3408 . ? N0AA C2AA 1.1782 . ? C2AA C1AA 1.4828 . ? O1AA S1AA 1.2789 . ? S1AA O3AA 1.3548 . ? S1AA O2AA 1.3756 . ? S1AA C3AA 1.7145 . ? F0AA C3AA 1.2577 . ? F1AA C3AA 1.2467 . ? F2AA C3AA 1.2618 . ? 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 O2H Tb1 O3C 76.2(3) . . ? O2H Tb1 O1C 74.7(3) . . ? O3C Tb1 O1C 70.2(2) . . ? O2H Tb1 O1LM 126.0(3) . . ? O3C Tb1 O1LM 143.2(3) . . ? O1C Tb1 O1LM 138.8(3) . . ? O2H Tb1 O23A 71.0(3) . . ? O3C Tb1 O23A 89.5(3) . . ? O1C Tb1 O23A 143.5(3) . . ? O1LM Tb1 O23A 74.3(3) . . ? O2H Tb1 N6A 119.3(3) . . ? O3C Tb1 N6A 126.5(2) . . ? O1C Tb1 N6A 66.8(3) . . ? O1LM Tb1 N6A 72.1(3) . . ? O23A Tb1 N6A 143.4(3) . . ? O2H Tb1 N2A 148.4(3) . . ? O3C Tb1 N2A 78.5(3) . . ? O1C Tb1 N2A 79.2(3) . . ? O1LM Tb1 N2A 85.5(3) . . ? O23A Tb1 N2A 127.5(3) . . ? N6A Tb1 N2A 63.8(3) . . ? O2H Tb1 N17A 122.4(3) . . ? O3C Tb1 N17A 68.5(3) . . ? O1C Tb1 N17A 128.1(3) . . ? O1LM Tb1 N17A 74.7(3) . . ? O23A Tb1 N17A 64.9(3) . . ? N6A Tb1 N17A 118.3(3) . . ? N2A Tb1 N17A 63.1(3) . . ? O2H Tb1 O14A 69.6(3) . . ? O3C Tb1 O14A 143.1(3) . . ? O1C Tb1 O14A 87.6(3) . . ? O1LM Tb1 O14A 71.7(3) . . ? O23A Tb1 O14A 92.0(3) . . ? N6A Tb1 O14A 63.9(3) . . ? N2A Tb1 O14A 127.1(3) . . ? N17A Tb1 O14A 143.4(3) . . ? C4C O1C Tb1 135.4(8) . . ? O1C C4C N2C 129.5(12) . . ? O1C C4C C5C 115.6(10) . . ? N2C C4C C5C 114.9(9) . . ? C4C N2C C15C 117.5(10) . . ? C4C N2C Tb5 121.7(8) . . ? C15C N2C Tb5 120.8(7) . . ? O1B Tb5 O0AA 74.7(3) . . ? O1B Tb5 O3B 68.4(3) . . ? O0AA Tb5 O3B 74.5(3) . . ? O1B Tb5 O23C 142.3(3) . . ? O0AA Tb5 O23C 68.9(3) . . ? O3B Tb5 O23C 92.2(3) . . ? O1B Tb5 O14C 84.5(3) . . ? O0AA Tb5 O14C 73.2(3) . . ? O3B Tb5 O14C 142.1(3) . . ? O23C Tb5 O14C 94.0(3) . . ? O1B Tb5 N6C 67.9(3) . . ? O0AA Tb5 N6C 124.7(3) . . ? O3B Tb5 N6C 123.2(3) . . ? O23C Tb5 N6C 143.6(3) . . ? O14C Tb5 N6C 64.1(3) . . ? O1B Tb5 OQA 133.1(3) . . ? O0AA Tb5 OQA 125.4(3) . . ? O3B Tb5 OQA 150.9(3) . . ? O23C Tb5 OQA 78.5(3) . . ? O14C Tb5 OQA 66.6(3) . . ? N6C Tb5 OQA 66.4(3) . . ? O1B Tb5 N2C 81.5(3) . . ? O0AA Tb5 N2C 146.8(3) . . ? O3B Tb5 N2C 75.5(3) . . ? O23C Tb5 N2C 126.1(3) . . ? O14C Tb5 N2C 127.5(3) . . ? N6C Tb5 N2C 63.7(3) . . ? OQA Tb5 N2C 87.8(3) . . ? O1B Tb5 O1AA 144.8(5) . . ? O0AA Tb5 O1AA 124.9(4) . . ? O3B Tb5 O1AA 140.3(5) . . ? O23C Tb5 O1AA 69.1(4) . . ? O14C Tb5 O1AA 76.0(4) . . ? N6C Tb5 O1AA 77.2(5) . . ? OQA Tb5 O1AA 12.3(4) . . ? N2C Tb5 O1AA 87.6(4) . . ? O1B Tb5 N17C 129.9(3) . . ? O0AA Tb5 N17C 116.4(3) . . ? O3B Tb5 N17C 68.7(3) . . ? O23C Tb5 N17C 63.0(3) . . ? O14C Tb5 N17C 145.2(3) . . ? N6C Tb5 N17C 118.8(3) . . ? OQA Tb5 N17C 82.7(3) . . ? N2C Tb5 N17C 63.7(3) . . ? O1AA Tb5 N17C 71.6(5) . . ? O1B Tb5 O3AA 131.4(5) . . ? O0AA Tb5 O3AA 76.5(3) . . ? O3B Tb5 O3AA 137.3(5) . . ? O23C Tb5 O3AA 47.8(6) . . ? O14C Tb5 O3AA 49.8(6) . . ? N6C Tb5 O3AA 99.1(5) . . ? OQA Tb5 O3AA 49.4(4) . . ? N2C Tb5 O3AA 136.4(3) . . ? O1AA Tb5 O3AA 48.8(2) . . ? N17C Tb5 O3AA 97.9(5) . . ? O1B Tb5 S1AA 140.1(3) . . ? O0AA Tb5 S1AA 102.5(3) . . ? O3B Tb5 S1AA 150.4(3) . . ? O23C Tb5 S1AA 60.3(3) . . ? O14C Tb5 S1AA 57.6(3) . . ? N6C Tb5 S1AA 83.3(3) . . ? OQA Tb5 S1AA 23.7(3) . . ? N2C Tb5 S1AA 110.6(3) . . ? O1AA Tb5 S1AA 23.71(14) . . ? N17C Tb5 S1AA 87.7(3) . . ? O3AA Tb5 S1AA 25.97(12) . . ? C22C O23C Tb5 122.9(7) . . ? O23C C22C O24C 124.1(10) . . ? O23C C22C C18C 120.6(11) . . ? O24C C22C C18C 115.1(11) . . ? C22C O24C C25C 115.0(12) . . ? N17C C18C C19C 122.5(11) . . ? N17C C18C C22C 111.8(12) . . ? C19C C18C C22C 125.7(11) . . ? C18C N17C C16C 119.5(11) . . ? C18C N17C Tb5 121.0(8) . . ? C16C N17C Tb5 119.4(7) . . ? N17C C16C C21C 120.5(11) . . ? N17C C16C C15C 117.7(11) . . ? C21C C16C C15C 121.6(10) . . ? O3C C15C N2C 128.8(11) . . ? O3C C15C C16C 117.1(12) . . ? N2C C15C C16C 113.9(10) . . ? C15C O3C Tb1 135.8(8) . . ? C20C C21C C16C 119.3(11) . . ? C21C C20C C19C 117.9(12) . . ? C18C C19C C20C 120.1(11) . . ? C11C O14C Tb5 120.1(7) . . ? O14C C11C O12C 126.1(10) . . ? O14C C11C C7C 124.9(11) . . ? O12C C11C C7C 108.6(11) . . ? C11C O12C C13C 114.5(12) . . ? N6C C7C C8C 125.2(10) . . ? N6C C7C C11C 107.3(10) . . ? C8C C7C C11C 127.3(12) . . ? C5C N6C C7C 114.2(11) . . ? C5C N6C Tb5 124.0(9) . . ? C7C N6C Tb5 121.6(6) . . ? N6C C5C C10C 124.5(12) . . ? N6C C5C C4C 113.5(11) . . ? C10C C5C C4C 121.6(9) . . ? C9C C10C C5C 118.3(11) . . ? C10C C9C C8C 120.6(12) . . ? C7C C8C C9C 117.1(12) . . ? C4B O1B Tb5 140.1(8) . . ? O1B C4B N2B 125.4(9) . . ? O1B C4B C5B 117.5(10) . . ? N2B C4B C5B 117.0(10) . . ? C4B N2B C15B 117.6(10) . . ? C4B N2B Tb55 119.5(7) . . ? C15B N2B Tb55 122.8(8) . . ? O1A Tb55 O2F 147.8(3) . . ? O1A Tb55 O3A 68.2(3) . . ? O2F Tb55 O3A 137.0(3) . . ? O1A Tb55 O4D 74.6(3) . . ? O2F Tb55 O4D 124.4(3) . . ? O3A Tb55 O4D 76.1(3) . . ? O1A Tb55 O23B 137.0(3) . . ? O2F Tb55 O23B 74.7(3) . . ? O3A Tb55 O23B 79.7(3) . . ? O4D Tb55 O23B 70.4(3) . . ? O1A Tb55 O14B 97.7(3) . . ? O2F Tb55 O14B 70.9(2) . . ? O3A Tb55 O14B 144.7(3) . . ? O4D Tb55 O14B 68.8(3) . . ? O23B Tb55 O14B 92.3(3) . . ? O1A Tb55 N6B 74.1(3) . . ? O2F Tb55 N6B 73.9(3) . . ? O3A Tb55 N6B 134.4(3) . . ? O4D Tb55 N6B 117.6(3) . . ? O23B Tb55 N6B 145.4(3) . . ? O14B Tb55 N6B 63.7(3) . . ? O1A Tb55 N2B 77.0(3) . . ? O2F Tb55 N2B 85.9(3) . . ? O3A Tb55 N2B 83.2(3) . . ? O4D Tb55 N2B 149.5(3) . . ? O23B Tb55 N2B 127.8(3) . . ? O14B Tb55 N2B 126.5(3) . . ? N6B Tb55 N2B 63.7(3) . . ? O1A Tb55 N17B 119.7(3) . . ? O2F Tb55 N17B 74.0(3) . . ? O3A Tb55 N17B 64.1(3) . . ? O4D Tb55 N17B 123.8(3) . . ? O23B Tb55 N17B 65.1(3) . . ? O14B Tb55 N17B 142.2(3) . . ? N6B Tb55 N17B 118.5(3) . . ? N2B Tb55 N17B 63.1(3) . . ? C22B O23B Tb55 122.6(9) . . ? O23B C22B O24B 125.2(15) . . ? O23B C22B C18B 120.3(12) . . ? O24B C22B C18B 114.5(14) . . ? C22B O24B C25B 117.2(13) . . ? C19B C18B N17B 120.3(14) . . ? C19B C18B C22B 126.7(14) . . ? N17B C18B C22B 112.9(11) . . ? C16B N17B C18B 119.7(11) . . ? C16B N17B Tb55 120.4(8) . . ? C18B N17B Tb55 118.3(9) . . ? N17B C16B C21B 120.3(13) . . ? N17B C16B C15B 118.6(12) . . ? C21B C16B C15B 121.1(13) . . ? O3B C15B N2B 129.3(12) . . ? O3B C15B C16B 118.9(11) . . ? N2B C15B C16B 111.7(12) . . ? C15B O3B Tb5 136.8(8) . . ? C16B C21B C20B 119.7(16) . . ? C19B C20B C21B 117.3(15) . . ? C20B C19B C18B 122.5(16) . . ? S1F O2F Tb55 150.1(5) . . ? O4F S1F O3F 117.1(6) . . ? O4F S1F O2F 114.1(5) . . ? O3F S1F O2F 113.2(5) . . ? O4F S1F C5F 103.7(5) . . ? O3F S1F C5F 103.5(7) . . ? O2F S1F C5F 102.9(5) . . ? F8F C5F F6F 112.0(12) . . ? F8F C5F F7F 106.3(10) . . ? F6F C5F F7F 106.3(11) . . ? F8F C5F S1F 111.8(9) . . ? F6F C5F S1F 111.8(9) . . ? F7F C5F S1F 108.0(9) . . ? C11B O14B Tb55 121.2(7) . . ? O14B C11B O12B 124.0(11) . . ? O14B C11B C7B 121.4(10) . . ? O12B C11B C7B 114.7(10) . . ? C11B O12B C13B 119.8(10) . . ? N6B C7B C8B 126.7(12) . . ? N6B C7B C11B 111.3(10) . . ? C8B C7B C11B 122.0(11) . . ? C7B N6B C5B 114.8(11) . . ? C7B N6B Tb55 122.4(8) . . ? C5B N6B Tb55 122.8(8) . . ? N6B C5B C10B 125.1(11) . . ? N6B C5B C4B 113.7(11) . . ? C10B C5B C4B 121.2(11) . . ? C5B C10B C9B 117.5(11) . . ? C8B C9B C10B 120.0(11) . . ? C7B C8B C9B 116.0(12) . . ? C4A O1A Tb55 137.7(7) . . ? O1A C4A N2A 127.4(10) . . ? O1A C4A C5A 118.3(10) . . ? N2A C4A C5A 114.2(10) . . ? C15A N2A C4A 116.1(9) . . ? C15A N2A Tb1 122.4(7) . . ? C4A N2A Tb1 121.4(7) . . ? O3A C15A N2A 128.1(10) . . ? O3A C15A C16A 117.2(10) . . ? N2A C15A C16A 114.7(9) . . ? C15A O3A Tb55 137.0(8) . . ? N17A C16A C21A 125.1(11) . . ? N17A C16A C15A 113.9(10) . . ? C21A C16A C15A 120.5(10) . . ? C16A N17A C18A 116.2(10) . . ? C16A N17A Tb1 123.4(8) . . ? C18A N17A Tb1 118.9(7) . . ? N17A C18A C19A 123.0(10) . . ? N17A C18A C22A 112.9(11) . . ? C19A C18A C22A 123.7(12) . . ? C18A C19A C20A 117.8(12) . . ? C21A C20A C19A 117.7(12) . . ? C16A C21A C20A 118.8(11) . . ? O23A C22A O24A 125.1(10) . . ? O23A C22A C18A 120.2(12) . . ? O24A C22A C18A 114.7(12) . . ? C22A O23A Tb1 121.4(7) . . ? C22A O24A C25A 115.8(11) . . ? N6A C5A C10A 124.3(11) . . ? N6A C5A C4A 115.4(12) . . ? C10A C5A C4A 120.3(9) . . ? C7A N6A C5A 115.8(11) . . ? C7A N6A Tb1 121.7(7) . . ? C5A N6A Tb1 122.3(8) . . ? N6A C7A C8A 124.4(10) . . ? N6A C7A C11A 110.7(10) . . ? C8A C7A C11A 124.9(10) . . ? O14A C11A O12A 122.7(10) . . ? O14A C11A C7A 124.0(11) . . ? O12A C11A C7A 113.3(11) . . ? C11A O14A Tb1 119.6(7) . . ? C11A O12A C13A 117.0(10) . . ? C9A C8A C7A 119.7(10) . . ? C8A C9A C10A 117.4(12) . . ? C9A C10A C5A 118.4(11) . . ? S1D O4D Tb55 148.5(5) . . ? O2D S1D O3D 116.9(6) . . ? O2D S1D O4D 111.8(5) . . ? O3D S1D O4D 114.5(5) . . ? O2D S1D C5D 104.8(6) . . ? O3D S1D C5D 104.6(7) . . ? O4D S1D C5D 102.4(6) . . ? F8D C5D F6D 108.8(12) . . ? F8D C5D F7D 104.5(11) . . ? F6D C5D F7D 105.8(13) . . ? F8D C5D S1D 114.5(11) . . ? F6D C5D S1D 111.6(10) . . ? F7D C5D S1D 111.1(10) . . ? S0AA O0AA Tb5 151.8(6) . . ? O4G S0AA O3G 115.4(6) . . ? O4G S0AA O0AA 114.2(5) . . ? O3G S0AA O0AA 114.1(7) . . ? O4G S0AA C5G 106.8(9) . . ? O3G S0AA C5G 103.7(8) . . ? O0AA S0AA C5G 100.5(6) . . ? F6G C5G F7G 109.3(16) . . ? F6G C5G F8G 106.6(13) . . ? F7G C5G F8G 104.2(19) . . ? F6G C5G S0AA 114.1(17) . . ? F7G C5G S0AA 111.1(11) . . ? F8G C5G S0AA 110.9(13) . . ? S1H O2H Tb1 149.9(4) . . ? O3H S1H O4H 116.6(5) . . ? O3H S1H O2H 113.8(5) . . ? O4H S1H O2H 114.5(5) . . ? O3H S1H C5H 104.9(6) . . ? O4H S1H C5H 104.5(6) . . ? O2H S1H C5H 100.0(6) . . ? F7H C5H F6H 108.1(12) . . ? F7H C5H F8H 105.9(10) . . ? F6H C5H F8H 108.5(12) . . ? F7H C5H S1H 111.9(9) . . ? F6H C5H S1H 112.5(8) . . ? F8H C5H S1H 109.7(11) . . ? N150 C151 C152 166(2) . . ? N1 C1 C0AA 172(4) . . ? S1L O1LM Tb1 153.9(6) . . ? O2L S1L O4L 117.9(7) . . ? O2L S1L O1LM 113.6(6) . . ? O4L S1L O1LM 112.2(6) . . ? O2L S1L C5L 104.6(6) . . ? O4L S1L C5L 104.6(7) . . ? O1LM S1L C5L 101.7(6) . . ? F8L C5L F6L 112.0(13) . . ? F8L C5L F7L 106.2(11) . . ? F6L C5L F7L 108.0(11) . . ? F8L C5L S1L 110.0(9) . . ? F6L C5L S1L 111.9(9) . . ? F7L C5L S1L 108.5(10) . . ? S1Q OQA Tb5 164.4(4) . . ? OQA S1Q O3Q 98.0 . . ? OQA S1Q O4Q 126.3 . . ? O3Q S1Q O4Q 114.5 . . ? OQA S1Q C5Q 109.9 . . ? O3Q S1Q C5Q 104.5 . . ? O4Q S1Q C5Q 102.0 . . ? F6Q C5Q F7Q 107.2 . . ? F6Q C5Q F8Q 108.5 . . ? F7Q C5Q F8Q 107.0 . . ? F6Q C5Q S1Q 110.5 . . ? F7Q C5Q S1Q 111.5 . . ? F8Q C5Q S1Q 111.9 . . ? N0AA C2AA C1AA 169.71(6) . . ? S1AA O1AA Tb5 103.4(7) . . ? O1AA S1AA O3AA 114.9 . . ? O1AA S1AA O2AA 113.1 . . ? O3AA S1AA O2AA 111.6 . . ? O1AA S1AA C3AA 109.0 . . ? O3AA S1AA C3AA 104.8 . . ? O2AA S1AA C3AA 102.2 . . ? O1AA S1AA Tb5 52.9(6) . . ? O3AA S1AA Tb5 65.0(6) . . ? O2AA S1AA Tb5 118.7(7) . . ? C3AA S1AA Tb5 139.0(7) . . ? S1AA O3AA Tb5 89.1(6) . . ? F1AA C3AA F0AA 107.3 . . ? F1AA C3AA F2AA 109.2 . . ? F0AA C3AA F2AA 106.1 . . ? F1AA C3AA S1AA 111.4 . . ? F0AA C3AA S1AA 111.7 . . ? F2AA C3AA S1AA 110.9 . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.379 _refine_diff_density_min -3.751 _refine_diff_density_rms 0.184 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.044 0.937 0.018 10775 1378 ' ' _platon_squeeze_details ; ;