# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Xintao Wu' _publ_contact_author_email WXT@FJIRSM.AC.CN _publ_section_title ; Synthesis, Crystal Structures, and Luminescent Properties of Eleven New Lanthanide Complexes with Fluorescent Whitener and 1,10-Phenanthroline ; loop_ _publ_author_name 'Xintao Wu' 'Rui-Biao Fu' 'Sheng-min Hu' 'Tianlu Sheng' # Attachment 'B902803J_cif.txt' data_f1 _database_code_depnum_ccdc_archive 'CCDC 679075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H104 Er2 N8 O24 S6' _chemical_formula_weight 2713.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.938 _cell_length_b 15.1750(2) _cell_length_c 17.5546(2) _cell_angle_alpha 81.079(6) _cell_angle_beta 76.752(6) _cell_angle_gamma 69.389(4) _cell_volume 2887.65(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7338 _cell_measurement_theta_min 2.0083 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.4800 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.3000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.631 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9022 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22373 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13049 _reflns_number_gt 11842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+3.7022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13049 _refine_ls_number_parameters 799 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Er1 Er 0.299616(13) -0.001909(11) 0.248817(9) 0.02700(5) Uani 1 1 d . . . S1 S 0.44169(9) -0.20908(7) 0.36466(5) 0.0395(2) Uani 1 1 d . . . S2 S -0.26974(8) -0.24643(6) -0.22122(5) 0.03314(19) Uani 1 1 d . . . S3 S 0.98572(8) -0.19186(7) 0.21247(6) 0.0367(2) Uani 1 1 d . . . O1 O 0.6701(4) -0.0733(4) 0.2940(3) 0.0747(12) Uani 1 1 d . . . H2 H 0.735(7) -0.092(5) 0.257(4) 0.09(2) Uiso 1 1 d . . . H1 H 0.656(11) -0.115(8) 0.303(7) 0.21(6) Uiso 1 1 d . . . O2 O 0.2446(3) -0.1325(2) 0.2434(2) 0.0434(7) Uani 1 1 d . . . H4 H 0.260(5) -0.168(4) 0.274(3) 0.07(2) Uiso 1 1 d . . . H3 H 0.189(5) -0.143(4) 0.223(3) 0.09(2) Uiso 1 1 d . . . O3 O 0.4725(3) 0.0373(2) 0.23896(19) 0.0416(7) Uani 1 1 d . . . H6 H 0.532(4) 0.009(3) 0.253(3) 0.044(13) Uiso 1 1 d . . . H5 H 0.456(5) 0.096(4) 0.237(3) 0.076(18) Uiso 1 1 d . . . O4 O 0.4389(2) -0.12878(17) 0.30434(15) 0.0371(6) Uani 1 1 d . . . O5 O 0.3520(3) -0.2509(2) 0.35911(18) 0.0528(8) Uani 1 1 d . . . O6 O 0.4328(3) -0.1824(3) 0.44165(18) 0.0695(10) Uani 1 1 d . . . O7 O -0.2395(2) -0.15836(16) -0.22838(15) 0.0340(5) Uani 1 1 d . . . O8 O -0.3968(2) -0.2253(2) -0.22476(18) 0.0485(7) Uani 1 1 d . . . O9 O -0.2333(3) -0.30686(19) -0.15359(16) 0.0486(7) Uani 1 1 d . . . O10 O 0.8768(3) -0.1295(2) 0.18482(18) 0.0556(8) Uani 1 1 d . . . O11 O 1.0910(3) -0.1641(2) 0.1735(2) 0.0587(8) Uani 1 1 d . . . O12 O 0.9700(3) -0.2024(2) 0.29633(17) 0.0585(8) Uani 1 1 d . . . N1 N 0.0821(3) 0.0370(2) 0.32291(17) 0.0325(6) Uani 1 1 d . . . N2 N 0.2645(3) 0.0482(2) 0.38483(17) 0.0347(7) Uani 1 1 d . . . N3 N 0.4313(3) -0.0675(2) 0.12478(18) 0.0351(7) Uani 1 1 d . . . N4 N 0.1962(3) 0.0449(2) 0.13157(17) 0.0336(6) Uani 1 1 d . . . C1 C -0.0069(3) 0.0236(3) 0.2976(2) 0.0387(8) Uani 1 1 d . . . H1A H 0.0133 -0.0077 0.2523 0.046 Uiso 1 1 calc R . . C2 C -0.1292(4) 0.0538(3) 0.3349(3) 0.0499(10) Uani 1 1 d . . . H2A H -0.1881 0.0429 0.3146 0.060 Uiso 1 1 calc R . . C3 C -0.1606(4) 0.0994(3) 0.4016(3) 0.0491(10) Uani 1 1 d . . . H3A H -0.2417 0.1218 0.4265 0.059 Uiso 1 1 calc R . . C4 C -0.0694(3) 0.1121(3) 0.4323(2) 0.0401(9) Uani 1 1 d . . . C5 C -0.0954(4) 0.1554(3) 0.5048(2) 0.0511(11) Uani 1 1 d . . . H5A H -0.1756 0.1789 0.5310 0.061 Uiso 1 1 calc R . . C6 C -0.0057(4) 0.1620(3) 0.5346(2) 0.0500(10) Uani 1 1 d . . . H6A H -0.0244 0.1908 0.5810 0.060 Uiso 1 1 calc R . . C7 C 0.1192(4) 0.1255(3) 0.4961(2) 0.0392(9) Uani 1 1 d . . . C8 C 0.2159(4) 0.1268(3) 0.5276(2) 0.0489(10) Uani 1 1 d . . . H8A H 0.2005 0.1537 0.5747 0.059 Uiso 1 1 calc R . . C9 C 0.3322(4) 0.0888(3) 0.4896(3) 0.0507(11) Uani 1 1 d . . . H9A H 0.3972 0.0882 0.5107 0.061 Uiso 1 1 calc R . . C10 C 0.3528(4) 0.0503(3) 0.4180(2) 0.0436(9) Uani 1 1 d . . . H10A H 0.4329 0.0249 0.3922 0.052 Uiso 1 1 calc R . . C11 C 0.1472(3) 0.0853(2) 0.4240(2) 0.0311(7) Uani 1 1 d . . . C12 C 0.0511(3) 0.0793(2) 0.3912(2) 0.0326(7) Uani 1 1 d . . . C13 C 0.5497(3) -0.1168(3) 0.1178(2) 0.0424(9) Uani 1 1 d . . . H13A H 0.5885 -0.1196 0.1589 0.051 Uiso 1 1 calc R . . C14 C 0.6176(4) -0.1641(3) 0.0519(3) 0.0515(11) Uani 1 1 d . . . H14A H 0.7006 -0.1960 0.0489 0.062 Uiso 1 1 calc R . . C15 C 0.5629(4) -0.1638(3) -0.0084(3) 0.0523(11) Uani 1 1 d . . . H15A H 0.6071 -0.1973 -0.0518 0.063 Uiso 1 1 calc R . . C16 C 0.4389(4) -0.1122(3) -0.0037(2) 0.0414(9) Uani 1 1 d . . . C17 C 0.3741(5) -0.1059(3) -0.0648(2) 0.0523(11) Uani 1 1 d . . . H17A H 0.4134 -0.1422 -0.1073 0.063 Uiso 1 1 calc R . . C18 C 0.2582(5) -0.0490(3) -0.0623(2) 0.0529(11) Uani 1 1 d . . . H18A H 0.2192 -0.0455 -0.1034 0.064 Uiso 1 1 calc R . . C19 C 0.1940(4) 0.0065(3) 0.0032(2) 0.0410(9) Uani 1 1 d . . . C20 C 0.0772(4) 0.0720(3) 0.0062(2) 0.0482(10) Uani 1 1 d . . . H20A H 0.0357 0.0800 -0.0345 0.058 Uiso 1 1 calc R . . C21 C 0.0243(4) 0.1244(3) 0.0693(3) 0.0499(10) Uani 1 1 d . . . H21A H -0.0527 0.1695 0.0715 0.060 Uiso 1 1 calc R . . C22 C 0.0870(4) 0.1095(3) 0.1308(2) 0.0422(9) Uani 1 1 d . . . H22A H 0.0507 0.1465 0.1731 0.051 Uiso 1 1 calc R . . C23 C 0.2517(3) -0.0045(3) 0.0676(2) 0.0343(8) Uani 1 1 d . . . C24 C 0.3766(3) -0.0641(2) 0.0633(2) 0.0329(8) Uani 1 1 d . . . C25 C 0.5899(3) -0.2930(2) 0.3391(2) 0.0339(8) Uani 1 1 d . . . C26 C 0.6716(4) -0.3016(3) 0.3871(2) 0.0483(10) Uani 1 1 d . . . H26A H 0.6463 -0.2663 0.4305 0.058 Uiso 1 1 calc R . . C27 C 0.7897(4) -0.3621(3) 0.3710(3) 0.0550(12) Uani 1 1 d . . . H27A H 0.8446 -0.3658 0.4024 0.066 Uiso 1 1 calc R . . C28 C 0.8264(4) -0.4168(3) 0.3089(3) 0.0502(11) Uani 1 1 d . . . H28A H 0.9055 -0.4587 0.2986 0.060 Uiso 1 1 calc R . . C29 C 0.7457(4) -0.4093(3) 0.2620(2) 0.0448(10) Uani 1 1 d . . . H29A H 0.7710 -0.4481 0.2209 0.054 Uiso 1 1 calc R . . C30 C 0.6261(3) -0.3454(3) 0.2736(2) 0.0349(8) Uani 1 1 d . . . C31 C 0.5479(4) -0.3373(3) 0.2171(2) 0.0421(9) Uani 1 1 d . . . H31A H 0.4647 -0.3060 0.2315 0.050 Uiso 1 1 calc R . . C32 C 0.5874(4) -0.3713(3) 0.1480(2) 0.0450(10) Uani 1 1 d . . . H32A H 0.6705 -0.4040 0.1357 0.054 Uiso 1 1 calc R . . C33 C 0.5165(4) -0.3640(3) 0.0877(2) 0.0413(9) Uani 1 1 d . . . C34 C 0.5785(4) -0.3920(3) 0.0130(2) 0.0466(10) Uani 1 1 d . . . H34A H 0.6631 -0.4170 0.0034 0.056 Uiso 1 1 calc R . . C35 C 0.5169(4) -0.3834(3) -0.0467(2) 0.0443(9) Uani 1 1 d . . . H35A H 0.5605 -0.4016 -0.0961 0.053 Uiso 1 1 calc R . . C36 C 0.3902(4) -0.3288(3) 0.1003(2) 0.0439(9) Uani 1 1 d . . . H36A H 0.3465 -0.3101 0.1496 0.053 Uiso 1 1 calc R . . C37 C 0.3288(4) -0.3212(3) 0.0406(2) 0.0445(9) Uani 1 1 d . . . H37A H 0.2441 -0.2976 0.0504 0.053 Uiso 1 1 calc R . . C38 C 0.3903(3) -0.3479(3) -0.0338(2) 0.0367(8) Uani 1 1 d . . . C39 C 0.3228(3) -0.3398(3) -0.0971(2) 0.0356(8) Uani 1 1 d . . . C40 C 0.3617(4) -0.3087(3) -0.1739(2) 0.0430(9) Uani 1 1 d . . . H40A H 0.4319 -0.2919 -0.1865 0.052 Uiso 1 1 calc R . . C41 C 0.2180(4) -0.3649(3) -0.0806(2) 0.0442(9) Uani 1 1 d . . . H41A H 0.1900 -0.3856 -0.0295 0.053 Uiso 1 1 calc R . . C42 C 0.2968(4) -0.3022(3) -0.2323(2) 0.0440(9) Uani 1 1 d . . . H42A H 0.3242 -0.2807 -0.2833 0.053 Uiso 1 1 calc R . . C43 C 0.1544(3) -0.3597(3) -0.1392(2) 0.0434(9) Uani 1 1 d . . . H43A H 0.0855 -0.3782 -0.1268 0.052 Uiso 1 1 calc R . . C44 C 0.1920(3) -0.3272(3) -0.2159(2) 0.0371(8) Uani 1 1 d . . . C45 C 0.1256(3) -0.3226(3) -0.2784(2) 0.0388(8) Uani 1 1 d . . . H45A H 0.1659 -0.3186 -0.3302 0.047 Uiso 1 1 calc R . . C46 C 0.0122(3) -0.3236(3) -0.2657(2) 0.0386(8) Uani 1 1 d . . . H46A H -0.0294 -0.3200 -0.2140 0.046 Uiso 1 1 calc R . . C47 C -0.0555(3) -0.3298(3) -0.3236(2) 0.0337(8) Uani 1 1 d . . . C48 C 0.0044(4) -0.3678(3) -0.3949(2) 0.0425(9) Uani 1 1 d . . . H48A H 0.0888 -0.3846 -0.4082 0.051 Uiso 1 1 calc R . . C49 C -0.0589(4) -0.3812(3) -0.4465(2) 0.0507(11) Uani 1 1 d . . . H49A H -0.0170 -0.4066 -0.4939 0.061 Uiso 1 1 calc R . . C50 C -0.1834(4) -0.3570(3) -0.4278(3) 0.0520(11) Uani 1 1 d . . . H50A H -0.2256 -0.3679 -0.4618 0.062 Uiso 1 1 calc R . . C51 C -0.2456(4) -0.3167(3) -0.3591(2) 0.0431(9) Uani 1 1 d . . . H51A H -0.3302 -0.2988 -0.3473 0.052 Uiso 1 1 calc R . . C52 C -0.1831(3) -0.3026(2) -0.3074(2) 0.0321(7) Uani 1 1 d . . . C53 C 1.0165(3) -0.3039(3) 0.1785(2) 0.0352(8) Uani 1 1 d . . . C54 C 0.9570(4) -0.3061(3) 0.1204(2) 0.0445(9) Uani 1 1 d . . . H54A H 0.9005 -0.2508 0.1034 0.053 Uiso 1 1 calc R . . C55 C 0.9801(5) -0.3896(4) 0.0869(3) 0.0559(12) Uani 1 1 d . . . H55A H 0.9390 -0.3904 0.0482 0.067 Uiso 1 1 calc R . . C56 C 1.0649(5) -0.4710(3) 0.1121(3) 0.0556(12) Uani 1 1 d . . . H56A H 1.0822 -0.5271 0.0897 0.067 Uiso 1 1 calc R . . C57 C 1.1233(4) -0.4693(3) 0.1699(3) 0.0509(11) Uani 1 1 d . . . H57A H 1.1800 -0.5250 0.1860 0.061 Uiso 1 1 calc R . . C58 C 1.1016(3) -0.3872(3) 0.2060(2) 0.0378(8) Uani 1 1 d . . . C59 C 1.1637(4) -0.3920(3) 0.2709(2) 0.0432(9) Uani 1 1 d . . . H59A H 1.1251 -0.3475 0.3077 0.052 Uiso 1 1 calc R . . C60 C 1.2704(4) -0.4550(3) 0.2808(3) 0.0495(10) Uani 1 1 d . . . H60A H 1.3101 -0.4961 0.2415 0.059 Uiso 1 1 calc R . . C61 C 1.3333(4) -0.4675(3) 0.3464(3) 0.0478(10) Uani 1 1 d . . . C62 C 1.4549(5) -0.5189(5) 0.3381(4) 0.100(2) Uani 1 1 d . . . H62A H 1.4954 -0.5467 0.2914 0.120 Uiso 1 1 calc R . . C63 C 1.5188(5) -0.5304(5) 0.3971(4) 0.107(3) Uani 1 1 d . . . H63A H 1.6017 -0.5644 0.3883 0.129 Uiso 1 1 calc R . . C64 C 1.2793(4) -0.4288(4) 0.4167(3) 0.0591(12) Uani 1 1 d . . . H64A H 1.1971 -0.3927 0.4247 0.071 Uiso 1 1 calc R . . C65 C 1.3436(4) -0.4419(4) 0.4756(3) 0.0618(13) Uani 1 1 d . . . H65A H 1.3029 -0.4144 0.5224 0.074 Uiso 1 1 calc R . . C66 C 1.4654(4) -0.4938(3) 0.4682(3) 0.0467(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.02466(8) 0.02692(8) 0.02789(9) -0.00728(6) -0.00488(6) -0.00456(6) S1 0.0395(5) 0.0367(5) 0.0310(5) -0.0037(4) -0.0048(4) 0.0005(4) S2 0.0313(4) 0.0271(4) 0.0391(5) -0.0076(4) -0.0003(4) -0.0092(4) S3 0.0365(5) 0.0352(5) 0.0375(5) -0.0068(4) -0.0127(4) -0.0055(4) O1 0.0351(18) 0.090(3) 0.090(3) -0.010(3) -0.019(2) -0.004(2) O2 0.0416(16) 0.0328(15) 0.060(2) -0.0026(15) -0.0166(15) -0.0140(13) O3 0.0274(14) 0.0379(16) 0.0588(19) -0.0069(14) -0.0120(13) -0.0064(13) O4 0.0365(13) 0.0302(13) 0.0424(15) -0.0008(11) -0.0131(11) -0.0055(11) O5 0.0400(15) 0.0476(17) 0.0605(19) 0.0073(15) 0.0002(14) -0.0127(14) O6 0.073(2) 0.074(2) 0.0359(17) -0.0197(16) -0.0116(16) 0.0140(19) O7 0.0290(12) 0.0267(12) 0.0457(15) -0.0072(11) -0.0094(11) -0.0053(10) O8 0.0314(13) 0.0453(16) 0.071(2) -0.0168(15) 0.0006(13) -0.0170(13) O9 0.0603(18) 0.0362(15) 0.0361(15) -0.0002(12) 0.0033(13) -0.0086(14) O10 0.0472(17) 0.0513(18) 0.0582(19) -0.0078(15) -0.0226(15) 0.0055(14) O11 0.0539(18) 0.058(2) 0.076(2) -0.0213(17) -0.0065(16) -0.0293(16) O12 0.076(2) 0.0530(18) 0.0361(16) -0.0119(14) -0.0159(15) -0.0018(17) N1 0.0322(15) 0.0308(15) 0.0335(16) -0.0052(12) -0.0045(12) -0.0093(13) N2 0.0320(15) 0.0366(16) 0.0326(16) -0.0076(13) -0.0083(13) -0.0043(13) N3 0.0371(16) 0.0325(16) 0.0327(16) -0.0058(13) -0.0029(13) -0.0089(13) N4 0.0378(16) 0.0328(16) 0.0309(16) -0.0054(12) -0.0091(13) -0.0095(13) C1 0.0343(19) 0.038(2) 0.046(2) -0.0091(17) -0.0084(17) -0.0107(16) C2 0.038(2) 0.057(3) 0.061(3) -0.005(2) -0.013(2) -0.020(2) C3 0.0292(19) 0.053(3) 0.057(3) -0.005(2) 0.0017(18) -0.0097(18) C4 0.0352(19) 0.041(2) 0.037(2) -0.0038(17) 0.0027(16) -0.0093(17) C5 0.046(2) 0.053(3) 0.039(2) -0.0128(19) 0.0175(19) -0.010(2) C6 0.056(3) 0.054(3) 0.032(2) -0.0151(19) 0.0033(19) -0.011(2) C7 0.050(2) 0.035(2) 0.0263(18) -0.0068(15) -0.0041(16) -0.0063(17) C8 0.064(3) 0.051(2) 0.033(2) -0.0110(18) -0.016(2) -0.013(2) C9 0.056(3) 0.055(3) 0.045(2) -0.013(2) -0.022(2) -0.011(2) C10 0.038(2) 0.046(2) 0.044(2) -0.0122(18) -0.0149(18) -0.0023(18) C11 0.0373(18) 0.0255(16) 0.0265(17) -0.0016(13) -0.0049(14) -0.0064(14) C12 0.0348(18) 0.0280(17) 0.0309(18) -0.0021(14) -0.0021(15) -0.0082(15) C13 0.0363(19) 0.041(2) 0.043(2) -0.0087(17) -0.0011(17) -0.0056(17) C14 0.041(2) 0.049(2) 0.048(3) -0.011(2) 0.0113(19) -0.0042(19) C15 0.064(3) 0.042(2) 0.040(2) -0.0121(19) 0.013(2) -0.015(2) C16 0.059(2) 0.035(2) 0.0295(19) -0.0065(15) 0.0040(17) -0.0204(19) C17 0.078(3) 0.049(3) 0.032(2) -0.0113(18) 0.002(2) -0.028(2) C18 0.083(3) 0.057(3) 0.031(2) -0.0032(19) -0.015(2) -0.035(3) C19 0.060(2) 0.043(2) 0.0291(19) 0.0026(16) -0.0138(18) -0.027(2) C20 0.064(3) 0.052(2) 0.040(2) 0.0076(19) -0.028(2) -0.025(2) C21 0.049(2) 0.047(2) 0.053(3) 0.002(2) -0.025(2) -0.008(2) C22 0.043(2) 0.038(2) 0.044(2) -0.0052(17) -0.0145(18) -0.0071(18) C23 0.045(2) 0.0330(18) 0.0277(18) -0.0045(14) -0.0056(15) -0.0167(16) C24 0.045(2) 0.0272(17) 0.0274(17) -0.0057(14) 0.0008(15) -0.0161(16) C25 0.0380(19) 0.0284(17) 0.0287(18) 0.0002(14) -0.0076(15) -0.0032(15) C26 0.050(2) 0.052(3) 0.039(2) -0.0116(19) -0.0180(19) -0.003(2) C27 0.045(2) 0.067(3) 0.047(3) -0.004(2) -0.021(2) -0.004(2) C28 0.0318(19) 0.059(3) 0.045(2) 0.001(2) -0.0075(18) 0.0003(19) C29 0.044(2) 0.045(2) 0.036(2) -0.0109(17) -0.0088(17) 0.0015(18) C30 0.0372(19) 0.0306(18) 0.0335(19) -0.0024(15) -0.0090(15) -0.0056(15) C31 0.0361(19) 0.046(2) 0.041(2) -0.0117(18) -0.0123(17) -0.0029(17) C32 0.037(2) 0.053(2) 0.043(2) -0.0111(19) -0.0107(18) -0.0076(19) C33 0.042(2) 0.047(2) 0.036(2) -0.0066(17) -0.0082(17) -0.0151(18) C34 0.0304(19) 0.059(3) 0.048(2) -0.014(2) -0.0064(17) -0.0085(19) C35 0.038(2) 0.060(3) 0.035(2) -0.0181(19) -0.0039(17) -0.0120(19) C36 0.039(2) 0.054(3) 0.037(2) -0.0109(18) -0.0025(17) -0.0134(19) C37 0.0328(19) 0.058(3) 0.041(2) -0.0080(19) -0.0041(17) -0.0134(19) C38 0.0350(18) 0.043(2) 0.0329(19) -0.0051(16) -0.0045(15) -0.0136(17) C39 0.0309(17) 0.040(2) 0.036(2) -0.0097(16) -0.0055(15) -0.0095(16) C40 0.036(2) 0.058(3) 0.039(2) -0.0069(19) -0.0025(17) -0.0225(19) C41 0.039(2) 0.059(3) 0.036(2) 0.0021(19) -0.0082(17) -0.0198(19) C42 0.040(2) 0.061(3) 0.032(2) -0.0022(18) -0.0031(16) -0.022(2) C43 0.0318(19) 0.055(2) 0.044(2) 0.0009(19) -0.0067(17) -0.0174(18) C44 0.0313(18) 0.040(2) 0.040(2) -0.0085(16) -0.0095(16) -0.0079(16) C45 0.0365(19) 0.047(2) 0.035(2) -0.0054(17) -0.0087(16) -0.0132(17) C46 0.0334(18) 0.044(2) 0.035(2) -0.0110(17) -0.0060(16) -0.0050(17) C47 0.0362(18) 0.0310(18) 0.0333(19) -0.0040(15) -0.0103(15) -0.0072(15) C48 0.038(2) 0.048(2) 0.037(2) -0.0086(18) -0.0043(17) -0.0089(18) C49 0.064(3) 0.053(3) 0.034(2) -0.0127(19) -0.008(2) -0.017(2) C50 0.062(3) 0.061(3) 0.045(2) -0.012(2) -0.022(2) -0.024(2) C51 0.043(2) 0.044(2) 0.048(2) -0.0072(18) -0.0154(19) -0.0160(18) C52 0.0333(17) 0.0256(16) 0.0361(19) -0.0057(14) -0.0056(15) -0.0075(14) C53 0.0350(18) 0.040(2) 0.0318(19) -0.0056(16) -0.0041(15) -0.0143(16) C54 0.048(2) 0.050(2) 0.041(2) -0.0049(18) -0.0121(18) -0.021(2) C55 0.069(3) 0.075(3) 0.040(2) -0.015(2) -0.008(2) -0.041(3) C56 0.069(3) 0.050(3) 0.056(3) -0.019(2) 0.001(2) -0.032(2) C57 0.057(3) 0.035(2) 0.058(3) -0.0067(19) -0.004(2) -0.014(2) C58 0.040(2) 0.0336(19) 0.037(2) -0.0029(16) -0.0029(16) -0.0120(16) C59 0.047(2) 0.035(2) 0.045(2) -0.0017(17) -0.0106(18) -0.0093(18) C60 0.047(2) 0.042(2) 0.051(3) -0.0008(19) -0.012(2) -0.0050(19) C61 0.042(2) 0.035(2) 0.061(3) 0.0030(19) -0.013(2) -0.0054(18) C62 0.063(3) 0.120(5) 0.087(4) -0.054(4) -0.037(3) 0.039(4) C63 0.055(3) 0.136(6) 0.097(5) -0.056(4) -0.040(3) 0.045(4) C64 0.034(2) 0.080(3) 0.056(3) -0.006(3) -0.008(2) -0.009(2) C65 0.037(2) 0.089(4) 0.049(3) -0.007(3) -0.006(2) -0.008(2) C66 0.042(2) 0.038(2) 0.053(3) 0.0054(19) -0.0128(19) -0.0064(18) _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 Er1 O7 2.275(2) 2 ? Er1 O3 2.306(3) . ? Er1 O4 2.308(2) . ? Er1 O2 2.318(3) . ? Er1 N3 2.491(3) . ? Er1 N2 2.517(3) . ? Er1 N4 2.522(3) . ? Er1 N1 2.529(3) . ? S1 O6 1.440(3) . ? S1 O5 1.450(3) . ? S1 O4 1.481(3) . ? S1 C25 1.783(4) . ? S2 O9 1.434(3) . ? S2 O8 1.450(3) . ? S2 O7 1.483(2) . ? S2 C52 1.774(4) . ? S3 O12 1.432(3) . ? S3 O10 1.450(3) . ? S3 O11 1.453(3) . ? S3 C53 1.777(4) . ? O7 Er1 2.275(2) 2 ? N1 C1 1.327(4) . ? N1 C12 1.362(4) . ? N2 C10 1.327(5) . ? N2 C11 1.369(4) . ? N3 C13 1.333(5) . ? N3 C24 1.369(5) . ? N4 C22 1.328(5) . ? N4 C23 1.354(5) . ? C1 C2 1.398(5) . ? C2 C3 1.362(6) . ? C3 C4 1.400(6) . ? C4 C12 1.404(5) . ? C4 C5 1.443(6) . ? C5 C6 1.333(6) . ? C6 C7 1.434(6) . ? C7 C8 1.397(6) . ? C7 C11 1.412(5) . ? C8 C9 1.355(6) . ? C9 C10 1.403(5) . ? C11 C12 1.430(5) . ? C13 C14 1.389(6) . ? C14 C15 1.365(6) . ? C15 C16 1.399(6) . ? C16 C24 1.397(5) . ? C16 C17 1.434(6) . ? C17 C18 1.344(7) . ? C18 C19 1.436(6) . ? C19 C20 1.395(6) . ? C19 C23 1.413(5) . ? C20 C21 1.362(6) . ? C21 C22 1.397(5) . ? C23 C24 1.438(5) . ? C25 C26 1.391(5) . ? C25 C30 1.397(5) . ? C26 C27 1.377(6) . ? C27 C28 1.370(6) . ? C28 C29 1.370(6) . ? C29 C30 1.405(5) . ? C30 C31 1.476(5) . ? C31 C32 1.311(5) . ? C32 C33 1.469(5) . ? C33 C36 1.387(5) . ? C33 C34 1.397(6) . ? C34 C35 1.378(5) . ? C35 C38 1.391(5) . ? C36 C37 1.382(5) . ? C37 C38 1.386(5) . ? C38 C39 1.483(5) . ? C39 C40 1.387(5) . ? C39 C41 1.389(5) . ? C40 C42 1.393(5) . ? C41 C43 1.389(5) . ? C42 C44 1.389(5) . ? C43 C44 1.389(5) . ? C44 C45 1.474(5) . ? C45 C46 1.325(5) . ? C46 C47 1.467(5) . ? C47 C48 1.391(5) . ? C47 C52 1.403(5) . ? C48 C49 1.382(6) . ? C49 C50 1.372(6) . ? C50 C51 1.371(6) . ? C51 C52 1.382(5) . ? C53 C54 1.379(5) . ? C53 C58 1.413(5) . ? C54 C55 1.392(6) . ? C55 C56 1.379(7) . ? C56 C57 1.365(6) . ? C57 C58 1.401(6) . ? C58 C59 1.475(5) . ? C59 C60 1.326(5) . ? C60 C61 1.468(6) . ? C61 C64 1.370(6) . ? C61 C62 1.370(6) . ? C62 C63 1.378(7) . ? C63 C66 1.369(7) . ? C64 C65 1.375(6) . ? C65 C66 1.376(6) . ? C66 C66 1.486(8) 2_846 ? 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 O7 Er1 O3 74.45(10) 2 . ? O7 Er1 O4 141.97(9) 2 . ? O3 Er1 O4 72.46(10) . . ? O7 Er1 O2 143.39(10) 2 . ? O3 Er1 O2 139.63(11) . . ? O4 Er1 O2 74.13(10) . . ? O7 Er1 N3 107.54(10) 2 . ? O3 Er1 N3 76.22(10) . . ? O4 Er1 N3 82.19(10) . . ? O2 Er1 N3 77.40(11) . . ? O7 Er1 N2 77.46(9) 2 . ? O3 Er1 N2 80.23(10) . . ? O4 Er1 N2 78.96(9) . . ? O2 Er1 N2 114.70(12) . . ? N3 Er1 N2 153.36(10) . . ? O7 Er1 N4 72.35(9) 2 . ? O3 Er1 N4 117.08(11) . . ? O4 Er1 N4 140.83(9) . . ? O2 Er1 N4 77.61(11) . . ? N3 Er1 N4 65.44(10) . . ? N2 Er1 N4 138.43(10) . . ? O7 Er1 N1 80.84(9) 2 . ? O3 Er1 N1 140.95(10) . . ? O4 Er1 N1 114.97(9) . . ? O2 Er1 N1 74.77(10) . . ? N3 Er1 N1 141.07(10) . . ? N2 Er1 N1 65.02(9) . . ? N4 Er1 N1 82.30(10) . . ? O6 S1 O5 114.7(2) . . ? O6 S1 O4 111.45(19) . . ? O5 S1 O4 110.16(16) . . ? O6 S1 C25 106.91(18) . . ? O5 S1 C25 108.55(18) . . ? O4 S1 C25 104.52(16) . . ? O9 S2 O8 113.82(18) . . ? O9 S2 O7 111.52(17) . . ? O8 S2 O7 110.81(15) . . ? O9 S2 C52 109.30(17) . . ? O8 S2 C52 106.54(17) . . ? O7 S2 C52 104.28(16) . . ? O12 S3 O10 112.71(19) . . ? O12 S3 O11 113.9(2) . . ? O10 S3 O11 110.7(2) . . ? O12 S3 C53 108.51(18) . . ? O10 S3 C53 106.22(18) . . ? O11 S3 C53 104.13(18) . . ? S1 O4 Er1 139.70(16) . . ? S2 O7 Er1 148.52(14) . 2 ? C1 N1 C12 116.9(3) . . ? C1 N1 Er1 124.3(2) . . ? C12 N1 Er1 118.6(2) . . ? C10 N2 C11 117.3(3) . . ? C10 N2 Er1 123.6(3) . . ? C11 N2 Er1 118.7(2) . . ? C13 N3 C24 117.4(3) . . ? C13 N3 Er1 123.7(3) . . ? C24 N3 Er1 118.3(2) . . ? C22 N4 C23 118.1(3) . . ? C22 N4 Er1 124.3(3) . . ? C23 N4 Er1 117.4(2) . . ? N1 C1 C2 124.0(4) . . ? C3 C2 C1 118.9(4) . . ? C2 C3 C4 119.3(4) . . ? C3 C4 C12 118.0(4) . . ? C3 C4 C5 122.2(4) . . ? C12 C4 C5 119.7(4) . . ? C6 C5 C4 120.8(4) . . ? C5 C6 C7 121.2(4) . . ? C8 C7 C11 117.9(4) . . ? C8 C7 C6 122.7(4) . . ? C11 C7 C6 119.4(4) . . ? C9 C8 C7 120.0(4) . . ? C8 C9 C10 118.8(4) . . ? N2 C10 C9 123.8(4) . . ? N2 C11 C7 122.2(3) . . ? N2 C11 C12 118.1(3) . . ? C7 C11 C12 119.6(3) . . ? N1 C12 C4 122.8(3) . . ? N1 C12 C11 117.9(3) . . ? C4 C12 C11 119.2(3) . . ? N3 C13 C14 122.8(4) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 118.7(4) . . ? C24 C16 C15 118.2(4) . . ? C24 C16 C17 119.0(4) . . ? C15 C16 C17 122.8(4) . . ? C18 C17 C16 121.8(4) . . ? C17 C18 C19 120.6(4) . . ? C20 C19 C23 118.0(4) . . ? C20 C19 C18 123.0(4) . . ? C23 C19 C18 119.0(4) . . ? C21 C20 C19 119.4(4) . . ? C20 C21 C22 119.3(4) . . ? N4 C22 C21 123.0(4) . . ? N4 C23 C19 122.1(4) . . ? N4 C23 C24 118.1(3) . . ? C19 C23 C24 119.6(3) . . ? N3 C24 C16 122.6(4) . . ? N3 C24 C23 117.6(3) . . ? C16 C24 C23 119.7(3) . . ? C26 C25 C30 120.6(3) . . ? C26 C25 S1 115.8(3) . . ? C30 C25 S1 123.5(3) . . ? C27 C26 C25 120.5(4) . . ? C28 C27 C26 120.1(4) . . ? C27 C28 C29 119.6(4) . . ? C28 C29 C30 122.5(4) . . ? C25 C30 C29 116.6(3) . . ? C25 C30 C31 124.5(3) . . ? C29 C30 C31 118.9(3) . . ? C32 C31 C30 124.6(4) . . ? C31 C32 C33 127.9(4) . . ? C36 C33 C34 117.7(4) . . ? C36 C33 C32 123.4(4) . . ? C34 C33 C32 118.9(4) . . ? C35 C34 C33 121.4(4) . . ? C34 C35 C38 120.7(4) . . ? C37 C36 C33 120.7(4) . . ? C36 C37 C38 121.6(4) . . ? C37 C38 C35 117.9(3) . . ? C37 C38 C39 120.9(3) . . ? C35 C38 C39 121.2(3) . . ? C40 C39 C41 118.0(3) . . ? C40 C39 C38 122.1(3) . . ? C41 C39 C38 120.0(3) . . ? C39 C40 C42 120.8(3) . . ? C43 C41 C39 121.1(4) . . ? C44 C42 C40 121.2(4) . . ? C41 C43 C44 121.1(4) . . ? C42 C44 C43 117.7(3) . . ? C42 C44 C45 121.0(4) . . ? C43 C44 C45 121.3(3) . . ? C46 C45 C44 124.4(4) . . ? C45 C46 C47 127.8(4) . . ? C48 C47 C52 117.2(3) . . ? C48 C47 C46 121.4(3) . . ? C52 C47 C46 121.4(3) . . ? C49 C48 C47 121.4(4) . . ? C50 C49 C48 120.1(4) . . ? C51 C50 C49 120.0(4) . . ? C50 C51 C52 120.2(4) . . ? C51 C52 C47 121.0(3) . . ? C51 C52 S2 117.8(3) . . ? C47 C52 S2 121.2(3) . . ? C54 C53 C58 120.4(4) . . ? C54 C53 S3 116.9(3) . . ? C58 C53 S3 122.6(3) . . ? C53 C54 C55 121.1(4) . . ? C56 C55 C54 119.0(4) . . ? C57 C56 C55 120.0(4) . . ? C56 C57 C58 122.9(4) . . ? C57 C58 C53 116.5(4) . . ? C57 C58 C59 119.7(4) . . ? C53 C58 C59 123.8(3) . . ? C60 C59 C58 124.9(4) . . ? C59 C60 C61 127.7(4) . . ? C64 C61 C62 116.1(4) . . ? C64 C61 C60 124.4(4) . . ? C62 C61 C60 119.5(5) . . ? C61 C62 C63 121.7(5) . . ? C66 C63 C62 122.8(5) . . ? C61 C64 C65 121.7(4) . . ? C64 C65 C66 122.7(5) . . ? C63 C66 C65 114.9(4) . . ? C63 C66 C66 122.7(5) . 2_846 ? C65 C66 C66 122.4(5) . 2_846 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H4 O5 0.70(5) 2.06(6) 2.727(5) 160(6) . O2 H3 O11 0.89(6) 1.75(6) 2.633(4) 173(6) 1_455 O3 H6 O1 0.76(5) 1.90(5) 2.658(5) 172(5) . O3 H5 O8 0.83(6) 1.84(6) 2.661(4) 169(5) 2 O1 H2 O10 0.88(7) 1.83(7) 2.711(6) 176(6) . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.251 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.090