# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wang, Ya-Wen' _publ_contact_author_email ywwang@lzu.edu.cn _publ_section_title ; Synthesis, crystal structures, luminescent and magnetic properties of homodinuclear lanthanide complexes with a flexible tripodal carboxylate ligand ; loop_ _publ_author_name 'Ai-Jiang Zhang' 'Ya-Wen Wang' 'Wei Dou' 'Ming Dong' 'Yan-Ling Zhang' 'Yu Tang' 'Wei-Sheng Liu' 'Yu Peng' # Attachment '- complexes.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 795979' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H92 La2 N6 O26 S2' _chemical_formula_weight 2135.74 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.309(2) _cell_length_b 27.404(4) _cell_length_c 16.686(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.115(2) _cell_angle_gamma 90.00 _cell_volume 5875.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2630 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 18.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27336 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.10 _reflns_number_total 10303 _reflns_number_gt 6129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0600P)^2^+0.5532P] 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 10303 _refine_ls_number_parameters 647 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 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 C49B C 0.9646(19) -0.0562(9) 0.8846(18) 0.106(4) Uani 0.447(10) 1 d PU A 2 C48B C 0.9346(17) 0.0328(8) 0.8377(16) 0.089(4) Uani 0.447(10) 1 d PU A 2 N3B N 0.8994(13) -0.0099(6) 0.8710(13) 0.076(3) Uani 0.447(10) 1 d PU A 2 C49A C 1.0022(14) -0.0477(7) 0.9516(14) 0.112(4) Uani 0.553(10) 1 d PU A 1 H49C H 1.0609 -0.0381 0.9966 0.134 Uiso 0.553(10) 1 d PR A 1 H49B H 1.0259 -0.0481 0.9036 0.134 Uiso 0.553(10) 1 d PR A 1 H49A H 0.9619 -0.0681 0.9666 0.134 Uiso 0.553(10) 1 d PR A 1 C48A C 0.9746(14) 0.0389(7) 0.9108(15) 0.112(4) Uani 0.553(10) 1 d PU A 1 H48A H 0.9234 0.0645 0.8979 0.135 Uiso 0.553(10) 1 d PR A 1 H48C H 1.0324 0.0485 0.9549 0.135 Uiso 0.553(10) 1 d PR A 1 H48B H 0.9974 0.0315 0.8619 0.135 Uiso 0.553(10) 1 d PR A 1 N3A N 0.9312(11) -0.0055(5) 0.9279(11) 0.080(3) Uani 0.553(10) 1 d PU A 1 H49E H 1.0302 -0.0422 0.9277 0.096 Uiso 0.447(10) 1 d PR A 2 H49F H 0.9812 -0.0622 0.8367 0.096 Uiso 0.447(10) 1 d PR A 2 H49D H 0.9332 -0.0722 0.9087 0.096 Uiso 0.447(10) 1 d PR A 2 H48D H 0.8839 0.0585 0.8307 0.096 Uiso 0.447(10) 1 d PR A 2 H48E H 0.9979 0.0435 0.8767 0.096 Uiso 0.447(10) 1 d PR A 2 H48F H 0.9489 0.0255 0.7857 0.096 Uiso 0.447(10) 1 d PR A 2 O1 O 0.5921(4) 0.08340(17) 0.8138(3) 0.0589(11) Uani 1 1 d DU A . C47 C 0.5241(7) 0.1004(3) 0.7595(5) 0.0683(17) Uani 1 1 d DU . . H47 H 0.4575 0.1000 0.7674 0.082 Uiso 1 1 calc R . . N2 N 0.5336(7) 0.1194(3) 0.6909(4) 0.0858(19) Uani 1 1 d U . . C45 C 0.4512(8) 0.1430(4) 0.6302(6) 0.127(3) Uani 1 1 d U . . H45C H 0.3884 0.1243 0.6223 0.190 Uiso 1 1 calc R . . H45A H 0.4700 0.1453 0.5786 0.190 Uiso 1 1 calc R . . H45B H 0.4403 0.1751 0.6493 0.190 Uiso 1 1 calc R . . C46 C 0.6410(8) 0.1199(4) 0.6789(6) 0.115(3) Uani 1 1 d U . . H46A H 0.6872 0.1025 0.7236 0.173 Uiso 1 1 calc R . . H46B H 0.6644 0.1530 0.6784 0.173 Uiso 1 1 calc R . . H46C H 0.6405 0.1045 0.6272 0.173 Uiso 1 1 calc R . . O2 O 0.7724(3) 0.02970(17) 0.9133(3) 0.0615(12) Uani 1 1 d DU A . C50 C 0.8287(6) -0.0052(3) 0.9183(6) 0.087(2) Uani 1 1 d DU . . H50A H 0.7946 -0.0296 0.9137 0.104 Uiso 0.50 1 d PR A . H50B H 0.8256 -0.0296 0.9567 0.104 Uiso 0.50 1 d PR . . La1 La 0.60028(3) 0.042484(12) 0.94963(2) 0.03045(12) Uani 1 1 d U . . C1 C -0.2229(5) 0.1837(3) 0.8702(5) 0.070(2) Uani 1 1 d U . . H1A H -0.2735 0.1807 0.9018 0.105 Uiso 1 1 calc R . . H1B H -0.2164 0.1531 0.8440 0.105 Uiso 1 1 calc R . . H1C H -0.2449 0.2084 0.8286 0.105 Uiso 1 1 calc R . . C2 C -0.1183(5) 0.1979(3) 0.9278(4) 0.0523(15) Uani 1 1 d U . . C3 C -0.0687(5) 0.2396(3) 0.9181(5) 0.0609(16) Uani 1 1 d U . . H3 H -0.0993 0.2601 0.8740 0.073 Uiso 1 1 calc R . . C4 C 0.0267(5) 0.2534(3) 0.9716(5) 0.0568(15) Uani 1 1 d U . . H4 H 0.0597 0.2821 0.9629 0.068 Uiso 1 1 calc R . . C5 C 0.0704(5) 0.2232(2) 1.0376(4) 0.0468(13) Uani 1 1 d U . . C6 C 0.0219(5) 0.1807(2) 1.0485(4) 0.0497(14) Uani 1 1 d U . . H6 H 0.0520 0.1601 1.0926 0.060 Uiso 1 1 calc R . . C7 C -0.0719(5) 0.1681(3) 0.9937(4) 0.0535(15) Uani 1 1 d U . . H7 H -0.1043 0.1391 1.0015 0.064 Uiso 1 1 calc R . . C8 C 0.3406(4) 0.1801(2) 1.0854(4) 0.0400(12) Uani 1 1 d U . . C9 C 0.2935(5) 0.1743(2) 0.9932(4) 0.0432(12) Uani 1 1 d U . . H9A H 0.2588 0.2043 0.9705 0.052 Uiso 1 1 calc R . . H9B H 0.3478 0.1675 0.9657 0.052 Uiso 1 1 calc R . . C10 C 0.1806(5) 0.1216(2) 0.8962(4) 0.0376(11) Uani 1 1 d U . . C11 C 0.0918(5) 0.1423(2) 0.8496(4) 0.0445(12) Uani 1 1 d U . . H11 H 0.0588 0.1664 0.8726 0.053 Uiso 1 1 calc R . . C12 C 0.0497(5) 0.1280(2) 0.7676(4) 0.0433(12) Uani 1 1 d U . . C13 C -0.0431(5) 0.1480(3) 0.7159(4) 0.0536(14) Uani 1 1 d U . . H13 H -0.0783 0.1717 0.7378 0.064 Uiso 1 1 calc R . . C14 C -0.0827(6) 0.1338(3) 0.6355(5) 0.0640(17) Uani 1 1 d U . . H14 H -0.1427 0.1484 0.6030 0.077 Uiso 1 1 calc R . . C15 C -0.0329(6) 0.0976(3) 0.6025(5) 0.0690(17) Uani 1 1 d U . . H15 H -0.0606 0.0874 0.5481 0.083 Uiso 1 1 calc R . . C16 C 0.0578(5) 0.0764(3) 0.6498(4) 0.0606(15) Uani 1 1 d U . . H16 H 0.0904 0.0521 0.6271 0.073 Uiso 1 1 calc R . . C17 C 0.1011(5) 0.0918(2) 0.7326(4) 0.0460(13) Uani 1 1 d U . . C18 C 0.1928(5) 0.0710(2) 0.7828(4) 0.0439(12) Uani 1 1 d U . . H18 H 0.2273 0.0472 0.7605 0.053 Uiso 1 1 calc R . . C19 C 0.2322(4) 0.0851(2) 0.8637(4) 0.0366(12) Uani 1 1 d U A . C20 C 0.3275(5) 0.0591(2) 0.9150(4) 0.0379(12) Uani 1 1 d U . . C21 C 0.3821(5) 0.1306(2) 1.1183(4) 0.0443(11) Uani 1 1 d U . . H21A H 0.3254 0.1072 1.1078 0.053 Uiso 1 1 calc R . . H21B H 0.4325 0.1195 1.0895 0.053 Uiso 1 1 calc R . . C22 C 0.5357(5) 0.1223(2) 1.2308(4) 0.0441(11) Uani 1 1 d U . . C23 C 0.5965(5) 0.1522(2) 1.2887(4) 0.0507(12) Uani 1 1 d U . . H23 H 0.5663 0.1784 1.3091 0.061 Uiso 1 1 calc R . . C24 C 0.7038(5) 0.1443(3) 1.3181(4) 0.0549(13) Uani 1 1 d U . . C25 C 0.7692(5) 0.1740(3) 1.3804(4) 0.0617(14) Uani 1 1 d U . . H25 H 0.7405 0.1991 1.4046 0.074 Uiso 1 1 calc R . . C26 C 0.8747(6) 0.1655(3) 1.4049(5) 0.0744(17) Uani 1 1 d U . . H26 H 0.9176 0.1857 1.4439 0.089 Uiso 1 1 calc R . . C27 C 0.9161(6) 0.1277(3) 1.3721(5) 0.0736(17) Uani 1 1 d U . . H27 H 0.9873 0.1220 1.3902 0.088 Uiso 1 1 calc R . . C28 C 0.8558(5) 0.0974(3) 1.3125(5) 0.0635(15) Uani 1 1 d U . . H28 H 0.8866 0.0718 1.2910 0.076 Uiso 1 1 calc R . . C29 C 0.7487(5) 0.1051(3) 1.2846(4) 0.0511(13) Uani 1 1 d U . . C30 C 0.6831(5) 0.0754(2) 1.2252(4) 0.0483(12) Uani 1 1 d U . . H30 H 0.7122 0.0498 1.2023 0.058 Uiso 1 1 calc R . . C31 C 0.5790(5) 0.0824(2) 1.1999(4) 0.0405(11) Uani 1 1 d U A . C32 C 0.5132(5) 0.0452(2) 1.1443(4) 0.0392(11) Uani 1 1 d U . . C33 C 0.4284(4) 0.2183(2) 1.1036(4) 0.0460(12) Uani 1 1 d U . . H33A H 0.4035 0.2491 1.0770 0.055 Uiso 1 1 calc R . . H33B H 0.4539 0.2237 1.1629 0.055 Uiso 1 1 calc R . . C34 C 0.6114(5) 0.2098(2) 1.1092(4) 0.0463(12) Uani 1 1 d U . . C35 C 0.6408(5) 0.2491(2) 1.1619(4) 0.0510(13) Uani 1 1 d U . . H35 H 0.5904 0.2707 1.1699 0.061 Uiso 1 1 calc R . . C36 C 0.7460(5) 0.2568(2) 1.2037(4) 0.0496(12) Uani 1 1 d U . . C37 C 0.7784(5) 0.2960(3) 1.2589(4) 0.0605(15) Uani 1 1 d U . . H37 H 0.7293 0.3180 1.2680 0.073 Uiso 1 1 calc R . . C38 C 0.8794(5) 0.3021(3) 1.2985(5) 0.0618(16) Uani 1 1 d U . . H38 H 0.8987 0.3280 1.3353 0.074 Uiso 1 1 calc R . . C39 C 0.9561(6) 0.2703(3) 1.2856(5) 0.0637(16) Uani 1 1 d U . . H39 H 1.0257 0.2752 1.3130 0.076 Uiso 1 1 calc R . . C40 C 0.9273(5) 0.2316(3) 1.2318(5) 0.0597(14) Uani 1 1 d U . . H40 H 0.9777 0.2103 1.2230 0.072 Uiso 1 1 calc R . . C41 C 0.8219(5) 0.2243(2) 1.1900(4) 0.0489(12) Uani 1 1 d U . . C42 C 0.7891(5) 0.1850(2) 1.1365(4) 0.0476(11) Uani 1 1 d U . . H42 H 0.8391 0.1632 1.1283 0.057 Uiso 1 1 calc R . . C43 C 0.6871(5) 0.1767(2) 1.0955(4) 0.0429(11) Uani 1 1 d U A . C44 C 0.6623(5) 0.1335(2) 1.0387(4) 0.0419(12) Uani 1 1 d U . . N1 N 0.2636(4) 0.19492(19) 1.1314(3) 0.0439(11) Uani 1 1 d U . . H1 H 0.256(5) 0.172(2) 1.171(4) 0.053 Uiso 1 1 d . . . O4 O 0.5763(3) 0.13093(15) 0.9842(3) 0.0526(10) Uani 1 1 d U A . O3 O 0.7295(3) 0.09999(15) 1.0455(3) 0.0481(10) Uani 1 1 d U A . O6 O 0.4412(3) 0.02420(15) 1.1662(3) 0.0449(10) Uani 1 1 d U . . O5 O 0.5358(3) 0.03366(13) 1.0758(2) 0.0374(9) Uani 1 1 d U . . O8 O 0.3135(3) 0.03039(15) 0.9695(3) 0.0447(10) Uani 1 1 d U . . O7 O 0.4118(3) 0.06679(15) 0.8974(3) 0.0458(9) Uani 1 1 d U A . O10 O 0.5096(3) 0.19877(16) 1.0706(3) 0.0515(10) Uani 1 1 d U . . O9 O 0.4304(3) 0.13288(15) 1.2058(3) 0.0473(9) Uani 1 1 d U . . O11 O 0.2203(3) 0.13513(14) 0.9791(3) 0.0418(9) Uani 1 1 d U . . O13 O 0.1580(4) 0.25013(19) 1.1873(3) 0.0725(15) Uani 1 1 d U . . O12 O 0.2327(3) 0.27869(16) 1.0735(3) 0.0644(13) Uani 1 1 d U . . S1 S 0.18615(13) 0.24078(6) 1.11147(12) 0.0515(5) Uani 1 1 d U . . 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 C49B 0.090(7) 0.099(7) 0.131(8) -0.008(8) 0.033(7) 0.008(7) C48B 0.075(7) 0.087(7) 0.115(8) -0.005(7) 0.043(7) 0.002(7) N3B 0.062(5) 0.072(5) 0.111(6) -0.006(5) 0.052(5) 0.002(5) C49A 0.093(7) 0.105(7) 0.131(8) -0.005(7) 0.020(7) 0.009(7) C48A 0.094(7) 0.105(7) 0.139(8) -0.001(8) 0.033(7) -0.006(7) N3A 0.059(5) 0.070(5) 0.118(6) 0.004(5) 0.034(5) 0.000(4) O1 0.068(3) 0.059(2) 0.052(3) 0.011(2) 0.020(2) 0.006(2) C47 0.079(3) 0.068(3) 0.059(3) 0.004(3) 0.020(3) 0.008(3) N2 0.110(5) 0.077(4) 0.066(4) 0.012(3) 0.016(4) 0.017(4) C45 0.154(7) 0.130(7) 0.079(6) 0.019(6) -0.001(6) 0.029(6) C46 0.136(7) 0.125(7) 0.078(6) 0.015(5) 0.017(6) -0.022(6) O2 0.047(2) 0.060(3) 0.088(3) 0.000(2) 0.036(2) 0.008(2) C50 0.069(4) 0.081(4) 0.118(4) -0.004(4) 0.039(4) -0.010(4) La1 0.02836(19) 0.02693(18) 0.0366(2) -0.00047(18) 0.00948(15) -0.00076(18) C1 0.046(4) 0.084(5) 0.070(5) 0.001(4) -0.003(4) -0.007(4) C2 0.036(3) 0.056(3) 0.062(3) -0.001(3) 0.008(3) 0.001(3) C3 0.044(3) 0.063(3) 0.070(3) 0.005(3) 0.005(3) 0.008(3) C4 0.042(3) 0.051(3) 0.075(3) 0.002(3) 0.011(3) 0.003(3) C5 0.032(2) 0.045(3) 0.063(3) -0.009(2) 0.012(2) 0.000(2) C6 0.037(3) 0.051(3) 0.060(3) -0.001(3) 0.011(2) -0.005(2) C7 0.042(3) 0.054(3) 0.063(3) 0.000(3) 0.013(3) -0.009(3) C8 0.031(2) 0.037(2) 0.052(2) -0.008(2) 0.012(2) -0.003(2) C9 0.031(2) 0.041(2) 0.058(2) -0.007(2) 0.012(2) -0.002(2) C10 0.032(2) 0.038(2) 0.044(2) 0.002(2) 0.011(2) -0.004(2) C11 0.035(2) 0.047(2) 0.050(2) -0.002(2) 0.008(2) 0.002(2) C12 0.034(2) 0.046(3) 0.048(3) 0.004(2) 0.007(2) 0.001(2) C13 0.043(3) 0.056(3) 0.056(3) 0.004(3) 0.002(3) 0.005(3) C14 0.048(3) 0.071(3) 0.061(3) 0.007(3) -0.009(3) 0.005(3) C15 0.060(3) 0.072(3) 0.060(3) -0.002(3) -0.011(3) 0.007(3) C16 0.055(3) 0.066(3) 0.051(3) -0.004(3) -0.005(3) 0.009(3) C17 0.039(3) 0.049(3) 0.044(3) 0.001(2) 0.000(2) -0.001(2) C18 0.036(2) 0.044(2) 0.047(2) -0.002(2) 0.005(2) 0.006(2) C19 0.029(2) 0.038(2) 0.041(2) 0.004(2) 0.007(2) -0.002(2) C20 0.033(2) 0.036(2) 0.045(2) -0.004(2) 0.011(2) 0.000(2) C21 0.037(2) 0.045(2) 0.049(2) -0.010(2) 0.006(2) -0.001(2) C22 0.037(2) 0.047(2) 0.047(2) -0.009(2) 0.010(2) -0.001(2) C23 0.042(2) 0.055(2) 0.054(2) -0.016(2) 0.010(2) 0.001(2) C24 0.045(2) 0.058(2) 0.057(2) -0.011(2) 0.004(2) -0.006(2) C25 0.049(3) 0.068(3) 0.062(3) -0.015(3) 0.003(3) -0.005(3) C26 0.059(3) 0.082(3) 0.070(3) -0.019(3) -0.004(3) -0.009(3) C27 0.048(3) 0.084(3) 0.076(3) -0.009(3) -0.007(3) -0.003(3) C28 0.048(3) 0.073(3) 0.065(3) -0.014(3) 0.007(3) 0.002(3) C29 0.038(2) 0.057(3) 0.054(3) -0.008(2) 0.005(2) -0.005(2) C30 0.042(2) 0.050(2) 0.052(2) -0.008(2) 0.009(2) -0.002(2) C31 0.037(2) 0.041(2) 0.044(2) -0.008(2) 0.012(2) -0.001(2) C32 0.037(2) 0.036(2) 0.044(2) -0.001(2) 0.010(2) -0.002(2) C33 0.031(2) 0.048(2) 0.059(2) -0.016(2) 0.011(2) -0.003(2) C34 0.035(2) 0.045(2) 0.059(2) -0.016(2) 0.013(2) -0.006(2) C35 0.037(2) 0.052(3) 0.067(3) -0.022(2) 0.018(2) -0.003(2) C36 0.036(2) 0.052(2) 0.064(3) -0.020(2) 0.017(2) -0.008(2) C37 0.045(3) 0.060(3) 0.076(3) -0.028(3) 0.014(3) -0.009(3) C38 0.048(3) 0.061(3) 0.076(3) -0.033(3) 0.015(3) -0.016(3) C39 0.044(3) 0.066(3) 0.078(3) -0.025(3) 0.011(3) -0.010(3) C40 0.043(3) 0.062(3) 0.073(3) -0.021(3) 0.013(2) -0.005(2) C41 0.037(2) 0.051(2) 0.062(3) -0.019(2) 0.019(2) -0.008(2) C42 0.035(2) 0.048(2) 0.061(2) -0.015(2) 0.017(2) -0.003(2) C43 0.035(2) 0.043(2) 0.053(2) -0.012(2) 0.0163(19) -0.0060(19) C44 0.034(2) 0.040(2) 0.054(3) -0.009(2) 0.014(2) -0.006(2) N1 0.031(2) 0.045(2) 0.056(2) -0.010(2) 0.012(2) -0.003(2) O4 0.047(2) 0.044(2) 0.061(2) -0.0131(19) 0.0040(19) 0.0013(18) O3 0.038(2) 0.042(2) 0.065(2) -0.0106(19) 0.0151(18) -0.0014(18) O6 0.042(2) 0.048(2) 0.049(2) -0.0078(18) 0.0206(18) -0.0091(18) O5 0.0367(18) 0.0330(18) 0.0441(19) -0.0056(16) 0.0132(16) -0.0019(15) O8 0.040(2) 0.045(2) 0.048(2) 0.0123(18) 0.0111(18) 0.0038(17) O7 0.0355(19) 0.0427(19) 0.057(2) 0.0086(18) 0.0072(18) 0.0004(17) O10 0.0322(18) 0.057(2) 0.065(2) -0.0230(18) 0.0115(17) -0.0036(17) O9 0.0379(19) 0.055(2) 0.048(2) -0.0135(18) 0.0082(17) 0.0057(17) O11 0.0337(17) 0.0410(18) 0.0490(19) -0.0027(16) 0.0078(16) -0.0057(16) O13 0.042(3) 0.090(4) 0.087(4) -0.034(3) 0.020(3) 0.010(3) O12 0.043(3) 0.040(2) 0.113(4) -0.007(3) 0.023(3) -0.004(2) S1 0.0341(9) 0.0446(10) 0.0766(13) -0.0206(9) 0.0163(9) -0.0002(8) _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_ _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 -0.008 0.000 0.500 806 210 ' ' 2 -0.003 0.500 1.000 806 211 ' ' _platon_squeeze_details ; ; 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 C49B N3B 1.52(3) . ? C49B H49B 0.8252 . ? C49B H49E 1.0496 . ? C49B H49F 0.8964 . ? C49B H49D 0.7849 . ? C48B N3B 1.43(2) . ? C48B H48B 0.8282 . ? C48B H48D 0.9626 . ? C48B H48E 0.9665 . ? C48B H48F 0.9561 . ? N3B C50 1.382(17) . ? C49A N3A 1.48(2) . ? C49A H49C 0.9684 . ? C49A H49B 0.9338 . ? C49A H49A 0.8562 . ? C49A H49E 0.6298 . ? C49A H49D 1.2088 . ? C48A N3A 1.408(19) . ? C48A H48A 0.9625 . ? C48A H48C 0.9527 . ? C48A H48B 0.9631 . ? C48A H48E 0.7267 . ? N3A C50 1.331(14) . ? O1 C47 1.196(8) . ? O1 La1 2.505(5) . ? C47 N2 1.293(9) . ? C47 H47 0.9300 . ? N2 C45 1.437(10) . ? N2 C46 1.494(11) . ? C45 H45C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? O2 C50 1.205(8) . ? O2 La1 2.543(4) . ? C50 H50A 0.7997 . ? C50 H50B 0.9342 . ? La1 O5 2.485(4) . ? La1 O8 2.513(4) 3_657 ? La1 O7 2.521(4) . ? La1 O4 2.531(4) . ? La1 O3 2.562(4) . ? La1 O6 2.612(4) 3_657 ? La1 O5 2.723(4) 3_657 ? La1 C32 3.045(6) 3_657 ? La1 La1 4.2086(8) 3_657 ? C1 C2 1.521(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.351(9) . ? C2 C7 1.378(9) . ? C3 C4 1.401(9) . ? C3 H3 0.9300 . ? C4 C5 1.378(9) . ? C4 H4 0.9300 . ? C5 C6 1.369(8) . ? C5 S1 1.770(7) . ? C6 C7 1.385(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.488(7) . ? C8 C9 1.510(8) . ? C8 C21 1.512(8) . ? C8 C33 1.541(8) . ? C9 O11 1.426(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.357(8) . ? C10 O11 1.395(7) . ? C10 C19 1.402(8) . ? C11 C12 1.392(8) . ? C11 H11 0.9300 . ? C12 C17 1.413(8) . ? C12 C13 1.419(8) . ? C13 C14 1.365(9) . ? C13 H13 0.9300 . ? C14 C15 1.385(10) . ? C14 H14 0.9300 . ? C15 C16 1.386(9) . ? C15 H15 0.9300 . ? C16 C17 1.415(9) . ? C16 H16 0.9300 . ? C17 C18 1.408(8) . ? C18 C19 1.369(8) . ? C18 H18 0.9300 . ? C19 C20 1.511(8) . ? C20 O7 1.250(7) . ? C20 O8 1.253(7) . ? C21 O9 1.435(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.360(8) . ? C22 O9 1.386(7) . ? C22 C31 1.397(8) . ? C23 C24 1.400(9) . ? C23 H23 0.9300 . ? C24 C29 1.414(9) . ? C24 C25 1.424(9) . ? C25 C26 1.376(10) . ? C25 H25 0.9300 . ? C26 C27 1.354(10) . ? C26 H26 0.9300 . ? C27 C28 1.381(9) . ? C27 H27 0.9300 . ? C28 C29 1.395(9) . ? C28 H28 0.9300 . ? C29 C30 1.399(8) . ? C30 C31 1.353(8) . ? C30 H30 0.9300 . ? C31 C32 1.498(8) . ? C32 O6 1.250(7) . ? C32 O5 1.295(7) . ? C32 La1 3.045(6) 3_657 ? C33 O10 1.437(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O10 1.373(7) . ? C34 C35 1.380(8) . ? C34 C43 1.419(8) . ? C35 C36 1.409(9) . ? C35 H35 0.9300 . ? C36 C37 1.407(8) . ? C36 C41 1.409(8) . ? C37 C38 1.345(9) . ? C37 H37 0.9300 . ? C38 C39 1.401(9) . ? C38 H38 0.9300 . ? C39 C40 1.376(9) . ? C39 H39 0.9300 . ? C40 C41 1.408(9) . ? C40 H40 0.9300 . ? C41 C42 1.394(8) . ? C42 C43 1.370(8) . ? C42 H42 0.9300 . ? C43 C44 1.499(8) . ? C44 O4 1.265(7) . ? C44 O3 1.266(7) . ? N1 S1 1.604(5) . ? N1 H1 0.94(6) . ? O6 La1 2.612(4) 3_657 ? O5 La1 2.723(4) 3_657 ? O8 La1 2.513(4) 3_657 ? O13 S1 1.433(5) . ? O12 S1 1.438(5) . ? 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 N3B C49B H49B 107.5 . . ? N3B C49B H49A 100.2 . . ? H49B C49B H49A 87.8 . . ? N3B C49B H49E 97.8 . . ? H49A C49B H49E 69.3 . . ? N3B C49B H49F 106.4 . . ? H49B C49B H49F 86.7 . . ? H49A C49B H49F 153.2 . . ? H49E C49B H49F 108.9 . . ? N3B C49B H49D 100.4 . . ? H49B C49B H49D 123.9 . . ? H49E C49B H49D 108.1 . . ? H49F C49B H49D 130.1 . . ? N3B C48B H48A 97.2 . . ? N3B C48B H48B 99.6 . . ? H48A C48B H48B 87.6 . . ? N3B C48B H48D 110.9 . . ? H48A C48B H48D 54.2 . . ? H48B C48B H48D 132.6 . . ? N3B C48B H48E 107.8 . . ? H48A C48B H48E 63.5 . . ? H48D C48B H48E 108.6 . . ? N3B C48B H48F 110.3 . . ? H48A C48B H48F 152.3 . . ? H48B C48B H48F 91.1 . . ? H48D C48B H48F 110.0 . . ? H48E C48B H48F 109.3 . . ? C50 N3B C48B 119.2(14) . . ? C50 N3B C49B 116.1(16) . . ? C48B N3B C49B 120.6(15) . . ? N3A C49A H49C 109.0 . . ? N3A C49A H49B 96.6 . . ? H49C C49A H49B 106.5 . . ? N3A C49A H49A 100.5 . . ? H49C C49A H49A 113.0 . . ? H49B C49A H49A 128.4 . . ? N3A C49A H49E 94.9 . . ? H49C C49A H49E 86.2 . . ? H49A C49A H49E 149.4 . . ? N3A C49A H49D 86.6 . . ? H49C C49A H49D 160.8 . . ? H49B C49A H49D 82.0 . . ? H49A C49A H49D 51.2 . . ? H49E C49A H49D 104.1 . . ? N3A C48A H48A 111.8 . . ? N3A C48A H48C 111.9 . . ? H48A C48A H48C 110.7 . . ? N3A C48A H48B 103.1 . . ? H48A C48A H48B 109.0 . . ? H48C C48A H48B 110.1 . . ? N3A C48A H48E 126.3 . . ? H48A C48A H48E 96.9 . . ? H48C C48A H48E 97.6 . . ? C50 N3A C48A 115.6(14) . . ? C50 N3A C49A 126.9(13) . . ? C48A N3A C49A 117.5(14) . . ? C47 O1 La1 134.9(5) . . ? O1 C47 N2 126.7(9) . . ? O1 C47 H47 116.6 . . ? N2 C47 H47 116.6 . . ? C47 N2 C45 124.9(9) . . ? C47 N2 C46 116.1(8) . . ? C45 N2 C46 118.8(8) . . ? N2 C45 H45C 109.5 . . ? N2 C45 H45A 109.5 . . ? H45C C45 H45A 109.5 . . ? N2 C45 H45B 109.5 . . ? H45C C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N2 C46 H46A 109.5 . . ? N2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C50 O2 La1 132.5(5) . . ? O2 C50 N3A 127.7(10) . . ? O2 C50 N3B 122.5(11) . . ? O2 C50 H50A 109.2 . . ? N3A C50 H50A 123.0 . . ? N3B C50 H50A 108.8 . . ? O2 C50 H50B 118.5 . . ? N3A C50 H50B 98.1 . . ? N3B C50 H50B 119.0 . . ? H50A C50 H50B 48.9 . . ? O5 La1 O1 150.13(14) . . ? O5 La1 O8 71.22(13) . 3_657 ? O1 La1 O8 138.35(14) . 3_657 ? O5 La1 O7 77.65(13) . . ? O1 La1 O7 76.37(15) . . ? O8 La1 O7 132.01(13) 3_657 . ? O5 La1 O4 78.94(13) . . ? O1 La1 O4 78.40(15) . . ? O8 La1 O4 134.90(14) 3_657 . ? O7 La1 O4 69.66(14) . . ? O5 La1 O2 136.13(15) . . ? O1 La1 O2 71.04(16) . . ? O8 La1 O2 72.84(14) 3_657 . ? O7 La1 O2 146.22(15) . . ? O4 La1 O2 111.18(15) . . ? O5 La1 O3 81.66(13) . . ? O1 La1 O3 98.81(15) . . ? O8 La1 O3 90.88(14) 3_657 . ? O7 La1 O3 119.92(13) . . ? O4 La1 O3 51.16(13) . . ? O2 La1 O3 74.56(14) . . ? O5 La1 O6 120.40(12) . 3_657 ? O1 La1 O6 72.11(14) . 3_657 ? O8 La1 O6 79.63(14) 3_657 3_657 ? O7 La1 O6 85.98(13) . 3_657 ? O4 La1 O6 145.45(14) . 3_657 ? O2 La1 O6 75.92(14) . 3_657 ? O3 La1 O6 150.46(13) . 3_657 ? O5 La1 O5 72.24(14) . 3_657 ? O1 La1 O5 109.36(14) . 3_657 ? O8 La1 O5 70.53(13) 3_657 3_657 ? O7 La1 O5 65.62(12) . 3_657 ? O4 La1 O5 130.64(12) . 3_657 ? O2 La1 O5 117.46(13) . 3_657 ? O3 La1 O5 151.61(13) . 3_657 ? O6 La1 O5 49.06(12) 3_657 3_657 ? O5 La1 C32 97.19(15) . 3_657 ? O1 La1 C32 89.34(16) . 3_657 ? O8 La1 C32 75.24(15) 3_657 3_657 ? O7 La1 C32 73.46(15) . 3_657 ? O4 La1 C32 142.91(15) . 3_657 ? O2 La1 C32 97.18(16) . 3_657 ? O3 La1 C32 165.58(15) . 3_657 ? O6 La1 C32 24.00(13) 3_657 3_657 ? O5 La1 C32 25.15(13) 3_657 3_657 ? O5 La1 La1 38.03(8) . 3_657 ? O1 La1 La1 136.58(11) . 3_657 ? O8 La1 La1 66.07(9) 3_657 3_657 ? O7 La1 La1 66.84(9) . 3_657 ? O4 La1 La1 107.95(10) . 3_657 ? O2 La1 La1 136.38(11) . 3_657 ? O3 La1 La1 118.91(10) . 3_657 ? O6 La1 La1 82.81(9) 3_657 3_657 ? O5 La1 La1 34.21(8) 3_657 3_657 ? C32 La1 La1 59.22(11) 3_657 3_657 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.7(7) . . ? C3 C2 C1 122.4(7) . . ? C7 C2 C1 119.9(7) . . ? C2 C3 C4 122.8(7) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 118.1(7) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C6 C5 C4 120.1(6) . . ? C6 C5 S1 119.6(6) . . ? C4 C5 S1 120.2(5) . . ? C5 C6 C7 119.9(7) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 121.3(7) . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? N1 C8 C9 113.2(5) . . ? N1 C8 C21 107.1(5) . . ? C9 C8 C21 106.9(5) . . ? N1 C8 C33 107.5(5) . . ? C9 C8 C33 111.4(5) . . ? C21 C8 C33 110.6(5) . . ? O11 C9 C8 109.4(5) . . ? O11 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? O11 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C11 C10 O11 120.4(6) . . ? C11 C10 C19 121.2(6) . . ? O11 C10 C19 118.4(5) . . ? C10 C11 C12 120.8(6) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C17 119.3(6) . . ? C11 C12 C13 123.5(6) . . ? C17 C12 C13 117.3(6) . . ? C14 C13 C12 122.7(7) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C13 C14 C15 119.5(7) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.6(7) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 120.3(7) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C12 118.4(6) . . ? C18 C17 C16 121.9(6) . . ? C12 C17 C16 119.6(6) . . ? C19 C18 C17 121.5(6) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C10 118.8(6) . . ? C18 C19 C20 118.4(5) . . ? C10 C19 C20 122.7(6) . . ? O7 C20 O8 126.1(6) . . ? O7 C20 C19 117.3(5) . . ? O8 C20 C19 116.5(5) . . ? O9 C21 C8 110.7(5) . . ? O9 C21 H21A 109.5 . . ? C8 C21 H21A 109.5 . . ? O9 C21 H21B 109.5 . . ? C8 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 O9 117.2(6) . . ? C23 C22 C31 120.5(6) . . ? O9 C22 C31 122.3(6) . . ? C22 C23 C24 121.2(6) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C29 118.5(6) . . ? C23 C24 C25 122.7(7) . . ? C29 C24 C25 118.8(6) . . ? C26 C25 C24 120.1(7) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.0(8) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 122.0(8) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C27 C28 C29 120.0(7) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 122.9(7) . . ? C28 C29 C24 118.9(7) . . ? C30 C29 C24 118.2(6) . . ? C31 C30 C29 122.6(6) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 C31 C22 118.9(6) . . ? C30 C31 C32 118.9(6) . . ? C22 C31 C32 122.1(6) . . ? O6 C32 O5 121.2(6) . . ? O6 C32 C31 120.0(5) . . ? O5 C32 C31 118.7(5) . . ? O6 C32 La1 58.2(3) . 3_657 ? O5 C32 La1 63.4(3) . 3_657 ? C31 C32 La1 170.8(4) . 3_657 ? O10 C33 C8 106.2(5) . . ? O10 C33 H33A 110.5 . . ? C8 C33 H33A 110.5 . . ? O10 C33 H33B 110.5 . . ? C8 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? O10 C34 C35 123.5(6) . . ? O10 C34 C43 116.0(5) . . ? C35 C34 C43 120.4(6) . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C37 C36 C35 122.3(6) . . ? C37 C36 C41 118.6(6) . . ? C35 C36 C41 119.1(6) . . ? C38 C37 C36 120.8(7) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 121.5(7) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C40 C39 C38 119.3(7) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 120.3(7) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 122.2(6) . . ? C42 C41 C36 118.3(6) . . ? C40 C41 C36 119.5(6) . . ? C43 C42 C41 123.5(6) . . ? C43 C42 H42 118.2 . . ? C41 C42 H42 118.2 . . ? C42 C43 C34 117.8(6) . . ? C42 C43 C44 118.3(6) . . ? C34 C43 C44 124.0(6) . . ? O4 C44 O3 120.7(6) . . ? O4 C44 C43 120.5(6) . . ? O3 C44 C43 118.8(6) . . ? C8 N1 S1 126.8(5) . . ? C8 N1 H1 113(4) . . ? S1 N1 H1 119(4) . . ? C44 O4 La1 94.2(4) . . ? C44 O3 La1 92.7(4) . . ? C32 O6 La1 97.8(4) . 3_657 ? C32 O5 La1 159.4(4) . . ? C32 O5 La1 91.5(3) . 3_657 ? La1 O5 La1 107.76(13) . 3_657 ? C20 O8 La1 139.1(4) . 3_657 ? C20 O7 La1 138.4(4) . . ? C34 O10 C33 119.1(5) . . ? C22 O9 C21 116.6(5) . . ? C10 O11 C9 115.5(4) . . ? O13 S1 O12 120.1(3) . . ? O13 S1 N1 105.0(3) . . ? O12 S1 N1 109.3(3) . . ? O13 S1 C5 106.4(3) . . ? O12 S1 C5 106.6(3) . . ? N1 S1 C5 109.1(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.896 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.098 #==END data_2 _database_code_depnum_ccdc_archive 'CCDC 795980' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H92 N6 Nd2 O26 S2' _chemical_formula_weight 2146.40 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3016(5) _cell_length_b 27.1952(12) _cell_length_c 16.6339(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.030(2) _cell_angle_gamma 90.00 _cell_volume 5811.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1976 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 17.83 _exptl_crystal_description BLOCK _exptl_crystal_colour PALE-PURPLE _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31435 _diffrn_reflns_av_R_equivalents 0.1116 _diffrn_reflns_av_sigmaI/netI 0.1780 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10814 _reflns_number_gt 5026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0501P)^2^+0.4162P] 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_number_reflns 10814 _refine_ls_number_parameters 645 _refine_ls_number_restraints 155 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.003 _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 Nd1 Nd 0.40164(3) -0.042209(13) 0.04973(2) 0.03189(11) Uani 1 1 d U . . C1 C -0.2209(6) 0.1838(3) -0.1297(5) 0.074(2) Uani 1 1 d U . . H1A H -0.2545 0.2124 -0.1582 0.111 Uiso 1 1 calc R . . H1B H -0.2647 0.1691 -0.0986 0.111 Uiso 1 1 calc R . . H1C H -0.2087 0.1605 -0.1696 0.111 Uiso 1 1 calc R . . C2 C -0.1198(6) 0.1982(3) -0.0718(5) 0.0555(16) Uani 1 1 d U . . C7 C -0.0722(5) 0.1687(3) -0.0062(4) 0.0483(15) Uani 1 1 d U . . H7 H -0.1044 0.1393 0.0013 0.058 Uiso 1 1 calc R . . C6 C 0.0219(5) 0.1806(3) 0.0497(4) 0.0509(14) Uani 1 1 d U . . H6 H 0.0519 0.1598 0.0937 0.061 Uiso 1 1 calc R . . C5 C 0.0695(5) 0.2239(3) 0.0386(4) 0.0446(13) Uani 1 1 d U . . C4 C 0.0247(6) 0.2537(3) -0.0277(5) 0.0599(16) Uani 1 1 d U . . H4 H 0.0576 0.2827 -0.0358 0.072 Uiso 1 1 calc R . . C3 C -0.0690(6) 0.2407(3) -0.0829(5) 0.0631(18) Uani 1 1 d U . . H3 H -0.0980 0.2611 -0.1278 0.076 Uiso 1 1 calc R . . C8 C 0.3386(5) 0.1804(2) 0.0861(4) 0.0419(13) Uani 1 1 d U . . C9 C 0.2922(5) 0.1744(2) -0.0065(4) 0.0425(12) Uani 1 1 d U . . H9A H 0.2562 0.2043 -0.0295 0.051 Uiso 1 1 calc R . . H9B H 0.3470 0.1683 -0.0340 0.051 Uiso 1 1 calc R . . C10 C 0.1821(5) 0.1200(2) -0.1048(4) 0.0396(12) Uani 1 1 d U . . C11 C 0.0928(5) 0.1418(2) -0.1517(4) 0.0426(13) Uani 1 1 d U . . H11 H 0.0605 0.1666 -0.1290 0.051 Uiso 1 1 calc R . . C12 C 0.0507(5) 0.1263(2) -0.2341(4) 0.0406(13) Uani 1 1 d U . . C13 C -0.0436(5) 0.1470(3) -0.2858(4) 0.0508(15) Uani 1 1 d U . . H13 H -0.0788 0.1711 -0.2643 0.061 Uiso 1 1 calc R . . C14 C -0.0805(6) 0.1322(3) -0.3634(5) 0.0601(17) Uani 1 1 d U . . H14 H -0.1418 0.1459 -0.3957 0.072 Uiso 1 1 calc R . . C15 C -0.0305(6) 0.0971(3) -0.3971(5) 0.0623(17) Uani 1 1 d U . . H15 H -0.0579 0.0873 -0.4520 0.075 Uiso 1 1 calc R . . C16 C 0.0603(6) 0.0761(3) -0.3507(5) 0.0561(16) Uani 1 1 d U . . H16 H 0.0937 0.0521 -0.3741 0.067 Uiso 1 1 calc R . . C17 C 0.1026(5) 0.0910(2) -0.2674(4) 0.0435(14) Uani 1 1 d U . . C18 C 0.1940(5) 0.0705(2) -0.2186(4) 0.0414(13) Uani 1 1 d U . . H18 H 0.2288 0.0470 -0.2419 0.050 Uiso 1 1 calc R . . C19 C 0.2343(5) 0.0838(2) -0.1371(4) 0.0371(13) Uani 1 1 d U . . C20 C 0.3296(5) 0.0578(2) -0.0866(4) 0.0372(13) Uani 1 1 d U . . C33 C 0.4274(5) 0.2180(2) 0.1043(4) 0.0440(12) Uani 1 1 d U . . H33A H 0.4029 0.2493 0.0789 0.053 Uiso 1 1 calc R . . H33B H 0.4535 0.2228 0.1639 0.053 Uiso 1 1 calc R . . C34 C 0.6101(5) 0.2101(3) 0.1085(4) 0.0456(12) Uani 1 1 d U . . C35 C 0.6389(5) 0.2484(3) 0.1619(4) 0.0498(13) Uani 1 1 d U . . H35 H 0.5884 0.2693 0.1724 0.060 Uiso 1 1 calc R . . C36 C 0.7459(5) 0.2569(3) 0.2021(4) 0.0479(13) Uani 1 1 d U . . C37 C 0.7784(5) 0.2962(3) 0.2597(4) 0.0544(15) Uani 1 1 d U . . H37 H 0.7294 0.3182 0.2696 0.065 Uiso 1 1 calc R . . C38 C 0.8792(6) 0.3016(3) 0.2997(5) 0.0594(16) Uani 1 1 d U . . H38 H 0.8993 0.3276 0.3368 0.071 Uiso 1 1 calc R . . C39 C 0.9548(6) 0.2687(3) 0.2866(5) 0.0617(16) Uani 1 1 d U . . H39 H 1.0245 0.2733 0.3142 0.074 Uiso 1 1 calc R . . C40 C 0.9259(6) 0.2302(3) 0.2335(5) 0.0581(15) Uani 1 1 d U . . H40 H 0.9764 0.2084 0.2258 0.070 Uiso 1 1 calc R . . C41 C 0.8207(5) 0.2226(3) 0.1895(4) 0.0490(13) Uani 1 1 d U . . C42 C 0.7871(5) 0.1831(2) 0.1336(4) 0.0477(12) Uani 1 1 d U . . H42 H 0.8364 0.1614 0.1235 0.057 Uiso 1 1 calc R . . C43 C 0.6859(5) 0.1760(2) 0.0946(4) 0.0445(12) Uani 1 1 d U . . C44 C 0.6583(5) 0.1333(3) 0.0376(4) 0.0445(13) Uani 1 1 d U . . C21 C 0.3812(5) 0.1301(2) 0.1204(4) 0.0461(12) Uani 1 1 d U . . H21A H 0.3246 0.1066 0.1105 0.055 Uiso 1 1 calc R . . H21B H 0.4311 0.1189 0.0911 0.055 Uiso 1 1 calc R . . C22 C 0.5345(5) 0.1222(3) 0.2311(4) 0.0457(12) Uani 1 1 d U . . C23 C 0.5968(5) 0.1518(3) 0.2898(4) 0.0514(12) Uani 1 1 d U . . H23 H 0.5675 0.1781 0.3113 0.062 Uiso 1 1 calc R . . C24 C 0.7045(6) 0.1431(3) 0.3184(4) 0.0526(13) Uani 1 1 d U . . C25 C 0.7697(6) 0.1732(3) 0.3797(5) 0.0613(15) Uani 1 1 d U . . H25 H 0.7417 0.1992 0.4032 0.074 Uiso 1 1 calc R . . C26 C 0.8758(6) 0.1635(3) 0.4045(5) 0.0695(17) Uani 1 1 d U . . H26 H 0.9192 0.1836 0.4438 0.083 Uiso 1 1 calc R . . C27 C 0.9174(6) 0.1244(3) 0.3717(5) 0.0704(17) Uani 1 1 d U . . H27 H 0.9883 0.1180 0.3906 0.084 Uiso 1 1 calc R . . C28 C 0.8568(6) 0.0948(3) 0.3117(5) 0.0624(16) Uani 1 1 d U . . H28 H 0.8862 0.0690 0.2890 0.075 Uiso 1 1 calc R . . C29 C 0.7487(5) 0.1042(3) 0.2849(4) 0.0485(13) Uani 1 1 d U . . C30 C 0.6836(5) 0.0739(3) 0.2245(4) 0.0465(12) Uani 1 1 d U . . H30 H 0.7129 0.0479 0.2019 0.056 Uiso 1 1 calc R . . C31 C 0.5789(5) 0.0815(2) 0.1983(4) 0.0425(12) Uani 1 1 d U . . C32 C 0.5137(5) 0.0446(3) 0.1422(4) 0.0402(12) Uani 1 1 d U . . C50 C 0.1770(7) 0.0049(3) 0.0788(5) 0.0695(17) Uani 1 1 d U . . H50A H 0.2043 0.0341 0.0642 0.083 Uiso 0.50 1 d PR A . H50B H 0.1993 0.0351 0.1052 0.083 Uiso 0.50 1 d PR . . C46 C 0.3618(7) -0.1191(4) 0.3194(6) 0.100(3) Uani 1 1 d U . . H46A H 0.3175 -0.0983 0.2785 0.150 Uiso 1 1 calc R . . H46B H 0.3653 -0.1067 0.3741 0.150 Uiso 1 1 calc R . . H46C H 0.3341 -0.1519 0.3143 0.150 Uiso 1 1 calc R . . C45 C 0.5487(8) -0.1403(4) 0.3683(6) 0.117(3) Uani 1 1 d U . . H45A H 0.5472 -0.1755 0.3633 0.176 Uiso 1 1 calc R . . H45B H 0.5424 -0.1312 0.4225 0.176 Uiso 1 1 calc R . . H45C H 0.6134 -0.1281 0.3608 0.176 Uiso 1 1 calc R . . C47 C 0.4760(7) -0.0996(3) 0.2363(5) 0.0640(18) Uani 1 1 d U . . H47 H 0.5431 -0.0979 0.2296 0.077 Uiso 1 1 calc R . . C49A C 0.0559(18) 0.0536(8) 0.1251(15) 0.084(4) Uani 0.410(8) 1 d PU A 1 H49A H 0.0813 0.0789 0.1654 0.126 Uiso 0.410(8) 1 d PR A 1 H49C H -0.0137 0.0448 0.1260 0.126 Uiso 0.410(8) 1 d PR A 1 H49B H 0.0559 0.0653 0.0706 0.126 Uiso 0.410(8) 1 d PR A 1 C48A C 0.0792(17) -0.0313(8) 0.1850(15) 0.084(4) Uani 0.410(8) 1 d PU A 1 H48A H 0.1040 -0.0624 0.1706 0.127 Uiso 0.410(8) 1 calc PR A 1 H48B H 0.0045 -0.0309 0.1682 0.127 Uiso 0.410(8) 1 calc PR A 1 H48C H 0.1026 -0.0265 0.2440 0.127 Uiso 0.410(8) 1 calc PR A 1 C49B C 0.0056(11) 0.0502(5) 0.0590(10) 0.087(3) Uani 0.590(8) 1 d PU A 2 H49D H 0.0338 0.0761 0.0975 0.131 Uiso 0.590(8) 1 d PR A 2 H49E H -0.0112 0.0630 0.0033 0.131 Uiso 0.590(8) 1 d PR A 2 H49F H -0.0563 0.0375 0.0710 0.131 Uiso 0.590(8) 1 d PR A 2 C48B C 0.0394(12) -0.0374(6) 0.1186(11) 0.088(3) Uani 0.590(8) 1 d PU A 2 H48D H 0.0944 -0.0612 0.1282 0.131 Uiso 0.590(8) 1 d PR A 2 H48E H -0.0215 -0.0520 0.1295 0.131 Uiso 0.590(8) 1 d PR A 2 H48F H 0.0236 -0.0265 0.0618 0.131 Uiso 0.590(8) 1 d PR A 2 N1 N 0.2630(4) 0.19486(19) 0.1323(3) 0.0446(12) Uani 1 1 d U . . H1 H 0.2598 0.1767 0.1739 0.054 Uiso 1 1 calc R . . N2 N 0.4643(6) -0.1197(3) 0.3063(5) 0.0791(19) Uani 1 1 d U . . N3A N 0.1189(14) 0.0076(7) 0.1431(13) 0.070(3) Uani 0.410(8) 1 d PU A 1 N3B N 0.0763(9) 0.0060(4) 0.0825(9) 0.065(2) Uani 0.590(8) 1 d PU A 2 O2 O 0.2328(4) -0.03046(17) 0.0853(3) 0.0550(12) Uani 1 1 d U A . O1 O 0.4076(4) -0.08365(18) 0.1817(3) 0.0584(13) Uani 1 1 d U . . O5 O 0.5345(3) 0.03388(14) 0.0737(3) 0.0386(9) Uani 1 1 d U . . O6 O 0.4407(3) 0.02256(15) 0.1640(3) 0.0445(10) Uani 1 1 d U . . O3 O 0.5726(3) 0.12883(16) -0.0155(3) 0.0493(11) Uani 1 1 d U . . O4 O 0.7262(3) 0.09827(16) 0.0447(3) 0.0481(11) Uani 1 1 d U . . O8 O 0.3163(3) 0.02923(15) -0.0303(3) 0.0432(10) Uani 1 1 d U . . O7 O 0.4142(3) 0.06577(15) -0.1038(3) 0.0423(10) Uani 1 1 d U . . O10 O 0.5090(3) 0.19903(16) 0.0701(3) 0.0513(10) Uani 1 1 d U . . O9 O 0.4301(3) 0.13231(16) 0.2071(3) 0.0485(10) Uani 1 1 d U . . O11 O 0.2204(3) 0.13377(15) -0.0203(3) 0.0428(9) Uani 1 1 d U . . O13 O 0.1574(4) 0.25089(19) 0.1882(3) 0.0667(15) Uani 1 1 d U . . O12 O 0.2316(4) 0.27942(17) 0.0758(3) 0.0620(14) Uani 1 1 d U . . S1 S 0.18554(14) 0.24127(7) 0.11282(14) 0.0514(5) Uani 1 1 d U . . 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 Nd1 0.02887(18) 0.02842(18) 0.0386(2) -0.0003(2) 0.00910(14) 0.0003(2) C1 0.050(4) 0.091(5) 0.072(5) 0.003(4) -0.001(4) 0.002(4) C2 0.040(3) 0.057(3) 0.063(3) 0.004(3) 0.004(3) 0.002(3) C7 0.037(3) 0.051(3) 0.059(3) 0.000(3) 0.016(3) 0.002(3) C6 0.039(3) 0.053(3) 0.060(3) 0.000(3) 0.011(2) 0.002(2) C5 0.031(2) 0.048(3) 0.057(3) -0.002(2) 0.016(2) -0.001(2) C4 0.046(3) 0.057(3) 0.074(3) 0.004(3) 0.010(3) 0.001(3) C3 0.047(3) 0.065(3) 0.071(3) 0.013(3) 0.001(3) 0.008(3) C8 0.034(2) 0.039(2) 0.052(2) -0.007(2) 0.010(2) -0.001(2) C9 0.034(2) 0.042(2) 0.053(2) -0.008(2) 0.014(2) -0.002(2) C10 0.034(2) 0.038(2) 0.046(2) 0.002(2) 0.010(2) -0.001(2) C11 0.035(2) 0.044(2) 0.049(2) 0.003(2) 0.012(2) 0.002(2) C12 0.034(2) 0.039(3) 0.047(3) 0.001(2) 0.006(2) 0.001(2) C13 0.044(3) 0.050(3) 0.054(3) 0.000(3) 0.006(3) 0.007(3) C14 0.050(3) 0.063(3) 0.059(3) 0.004(3) -0.001(3) 0.003(3) C15 0.054(3) 0.066(3) 0.056(3) -0.003(3) -0.005(3) 0.003(3) C16 0.051(3) 0.056(3) 0.055(3) -0.005(3) 0.002(3) 0.009(3) C17 0.038(3) 0.045(3) 0.045(3) 0.001(2) 0.006(2) 0.000(2) C18 0.036(2) 0.041(2) 0.046(2) -0.002(2) 0.010(2) 0.007(2) C19 0.032(2) 0.036(2) 0.045(2) 0.001(2) 0.012(2) 0.004(2) C20 0.034(2) 0.032(2) 0.047(2) -0.002(2) 0.012(2) 0.001(2) C33 0.031(2) 0.046(2) 0.056(2) -0.012(2) 0.014(2) -0.002(2) C34 0.034(2) 0.046(2) 0.056(2) -0.014(2) 0.010(2) -0.003(2) C35 0.038(2) 0.050(2) 0.061(3) -0.018(2) 0.012(2) -0.005(2) C36 0.036(2) 0.051(2) 0.059(3) -0.018(2) 0.015(2) -0.010(2) C37 0.039(3) 0.057(3) 0.067(3) -0.022(3) 0.013(3) -0.010(3) C38 0.048(3) 0.061(3) 0.071(3) -0.026(3) 0.017(3) -0.010(3) C39 0.045(3) 0.066(3) 0.072(3) -0.023(3) 0.011(3) -0.008(3) C40 0.049(3) 0.060(3) 0.065(3) -0.016(2) 0.013(2) -0.008(2) C41 0.037(2) 0.052(2) 0.059(3) -0.014(2) 0.014(2) -0.009(2) C42 0.037(2) 0.050(2) 0.057(2) -0.013(2) 0.015(2) -0.005(2) C43 0.038(2) 0.045(2) 0.052(2) -0.012(2) 0.014(2) -0.004(2) C44 0.037(2) 0.043(2) 0.054(2) -0.008(2) 0.014(2) -0.003(2) C21 0.039(2) 0.046(2) 0.050(2) -0.011(2) 0.006(2) 0.004(2) C22 0.038(2) 0.046(2) 0.051(2) -0.009(2) 0.009(2) 0.001(2) C23 0.044(2) 0.051(2) 0.056(2) -0.012(2) 0.007(2) 0.002(2) C24 0.046(2) 0.054(2) 0.056(2) -0.012(2) 0.008(2) -0.004(2) C25 0.053(3) 0.061(3) 0.062(3) -0.010(2) 0.002(3) -0.004(3) C26 0.061(3) 0.068(3) 0.071(3) -0.011(3) 0.003(3) -0.007(3) C27 0.057(3) 0.073(3) 0.074(3) -0.011(3) 0.005(3) -0.002(3) C28 0.053(3) 0.066(3) 0.065(3) -0.007(3) 0.009(3) 0.001(3) C29 0.040(2) 0.051(2) 0.053(3) -0.006(2) 0.009(2) -0.003(2) C30 0.041(2) 0.047(2) 0.051(2) -0.007(2) 0.012(2) 0.000(2) C31 0.039(2) 0.040(2) 0.047(2) -0.009(2) 0.010(2) -0.002(2) C32 0.035(2) 0.039(2) 0.046(2) -0.004(2) 0.010(2) 0.002(2) C50 0.064(3) 0.064(3) 0.082(3) -0.001(3) 0.022(3) -0.007(3) C46 0.112(6) 0.097(5) 0.090(5) 0.008(5) 0.024(5) -0.018(5) C45 0.121(6) 0.125(6) 0.093(5) 0.015(5) 0.005(5) 0.020(5) C47 0.065(3) 0.067(3) 0.061(3) -0.001(3) 0.018(3) 0.002(3) C49A 0.087(6) 0.076(6) 0.086(6) 0.001(5) 0.019(5) 0.002(5) C48A 0.080(6) 0.078(6) 0.090(6) 0.009(6) 0.013(5) 0.001(6) C49B 0.076(5) 0.079(5) 0.097(5) -0.001(5) 0.006(5) 0.005(5) C48B 0.081(6) 0.079(6) 0.101(6) 0.006(5) 0.021(5) -0.006(5) N1 0.033(2) 0.047(2) 0.055(2) -0.005(2) 0.012(2) -0.001(2) N2 0.086(4) 0.073(4) 0.070(4) 0.009(3) 0.006(4) 0.010(3) N3A 0.066(5) 0.068(5) 0.081(5) -0.002(4) 0.027(4) -0.002(4) N3B 0.053(4) 0.057(4) 0.086(4) 0.002(4) 0.018(4) 0.000(4) O2 0.045(2) 0.048(2) 0.076(3) 0.004(2) 0.023(2) 0.008(2) O1 0.062(3) 0.057(3) 0.057(3) 0.006(2) 0.015(2) 0.006(2) O5 0.0358(18) 0.036(2) 0.0442(19) -0.0078(17) 0.0106(17) -0.0011(16) O6 0.0397(19) 0.044(2) 0.052(2) -0.0047(17) 0.0159(18) -0.0069(17) O3 0.043(2) 0.044(2) 0.056(2) -0.0104(19) 0.0047(19) -0.0001(18) O4 0.040(2) 0.041(2) 0.060(2) -0.012(2) 0.007(2) -0.0016(19) O8 0.0374(19) 0.042(2) 0.049(2) 0.0051(17) 0.0101(18) 0.0060(17) O7 0.032(2) 0.037(2) 0.056(2) 0.0057(19) 0.0095(19) 0.0014(18) O10 0.0347(19) 0.054(2) 0.064(2) -0.0206(18) 0.0095(18) -0.0015(17) O9 0.041(2) 0.051(2) 0.050(2) -0.0114(18) 0.0040(18) 0.0051(18) O11 0.0333(18) 0.0412(19) 0.0523(19) -0.0022(17) 0.0086(17) -0.0057(16) O13 0.051(3) 0.079(3) 0.077(3) -0.031(3) 0.028(3) 0.002(3) O12 0.043(3) 0.039(3) 0.106(4) -0.006(3) 0.022(3) 0.001(2) S1 0.0341(10) 0.0450(11) 0.0772(14) -0.0177(10) 0.0184(10) -0.0023(9) _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_ _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 -0.008 0.000 0.500 762 293 ' ' 2 -0.003 0.500 1.000 762 294 ' ' _platon_squeeze_details ; ; 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 Nd1 O5 2.428(4) 3_655 ? Nd1 O1 2.451(5) . ? Nd1 O8 2.460(4) . ? Nd1 O7 2.466(4) 3_655 ? Nd1 O3 2.468(4) 3_655 ? Nd1 O2 2.487(5) . ? Nd1 O4 2.510(4) 3_655 ? Nd1 O6 2.545(4) . ? Nd1 O5 2.683(4) . ? Nd1 C44 2.877(7) 3_655 ? C1 C2 1.490(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.370(9) . ? C2 C3 1.377(9) . ? C7 C6 1.391(8) . ? C7 H7 0.9300 . ? C6 C5 1.371(9) . ? C6 H6 0.9300 . ? C5 C4 1.373(9) . ? C5 S1 1.772(7) . ? C4 C3 1.388(9) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C8 N1 1.468(8) . ? C8 C9 1.513(8) . ? C8 C33 1.532(8) . ? C8 C21 1.533(8) . ? C9 O11 1.440(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.375(8) . ? C10 C19 1.389(8) . ? C10 O11 1.416(7) . ? C11 C12 1.405(8) . ? C11 H11 0.9300 . ? C12 C17 1.379(9) . ? C12 C13 1.439(8) . ? C13 C14 1.319(9) . ? C13 H13 0.9300 . ? C14 C15 1.365(9) . ? C14 H14 0.9300 . ? C15 C16 1.377(9) . ? C15 H15 0.9300 . ? C16 C17 1.413(9) . ? C16 H16 0.9300 . ? C17 C18 1.392(8) . ? C18 C19 1.371(8) . ? C18 H18 0.9300 . ? C19 C20 1.504(8) . ? C20 O7 1.250(7) . ? C20 O8 1.264(7) . ? C33 O10 1.445(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.359(8) . ? C34 O10 1.364(7) . ? C34 C43 1.433(8) . ? C35 C36 1.425(9) . ? C35 H35 0.9300 . ? C36 C41 1.417(9) . ? C36 C37 1.426(9) . ? C37 C38 1.341(9) . ? C37 H37 0.9300 . ? C38 C39 1.405(9) . ? C38 H38 0.9300 . ? C39 C40 1.359(9) . ? C39 H39 0.9300 . ? C40 C41 1.416(9) . ? C40 H40 0.9300 . ? C41 C42 1.415(9) . ? C42 C43 1.348(8) . ? C42 H42 0.9300 . ? C43 C44 1.484(9) . ? C44 O3 1.254(7) . ? C44 O4 1.297(7) . ? C44 Nd1 2.877(7) 3_655 ? C21 O9 1.421(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.366(8) . ? C22 O9 1.370(7) . ? C22 C31 1.428(8) . ? C23 C24 1.408(9) . ? C23 H23 0.9300 . ? C24 C29 1.395(9) . ? C24 C25 1.415(9) . ? C25 C26 1.390(10) . ? C25 H25 0.9300 . ? C26 C27 1.374(10) . ? C26 H26 0.9300 . ? C27 C28 1.370(9) . ? C27 H27 0.9300 . ? C28 C29 1.414(9) . ? C28 H28 0.9300 . ? C29 C30 1.410(8) . ? C30 C31 1.364(8) . ? C30 H30 0.9300 . ? C31 C32 1.486(9) . ? C32 O6 1.271(7) . ? C32 O5 1.275(7) . ? C50 O2 1.202(8) . ? C50 N3B 1.356(13) . ? C50 N3A 1.474(19) . ? C50 H50A 0.9337 . ? C50 H50B 0.9436 . ? C46 N2 1.435(10) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C45 N2 1.427(10) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C47 O1 1.187(8) . ? C47 N2 1.332(9) . ? C47 H47 0.9300 . ? C49A N3A 1.49(2) . ? C49A H49A 0.9600 . ? C49A H49C 0.9600 . ? C49A H49B 0.9600 . ? C49A H49D 0.7747 . ? C48A N3A 1.44(2) . ? C48A H48A 0.9600 . ? C48A H48B 0.9600 . ? C48A H48C 0.9600 . ? C49B N3B 1.515(16) . ? C49B H49C 1.2157 . ? C49B H49B 0.7663 . ? C49B H49D 0.9599 . ? C49B H49E 0.9600 . ? C49B H49F 0.9601 . ? C48B N3B 1.465(17) . ? C48B H48D 0.9601 . ? C48B H48E 0.9602 . ? C48B H48F 0.9599 . ? N1 S1 1.608(5) . ? N1 H1 0.8600 . ? N3B H48F 1.1264 . ? O5 Nd1 2.428(4) 3_655 ? O3 Nd1 2.468(4) 3_655 ? O4 Nd1 2.510(4) 3_655 ? O7 Nd1 2.466(4) 3_655 ? O13 S1 1.422(5) . ? O12 S1 1.424(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Nd1 O1 149.70(15) 3_655 . ? O5 Nd1 O8 71.49(14) 3_655 . ? O1 Nd1 O8 138.67(15) . . ? O5 Nd1 O7 78.46(14) 3_655 3_655 ? O1 Nd1 O7 75.85(15) . 3_655 ? O8 Nd1 O7 132.70(14) . 3_655 ? O5 Nd1 O3 78.10(14) 3_655 3_655 ? O1 Nd1 O3 78.10(15) . 3_655 ? O8 Nd1 O3 134.53(15) . 3_655 ? O7 Nd1 O3 69.62(14) 3_655 3_655 ? O5 Nd1 O2 136.45(15) 3_655 . ? O1 Nd1 O2 70.59(16) . . ? O8 Nd1 O2 73.05(15) . . ? O7 Nd1 O2 145.09(15) 3_655 . ? O3 Nd1 O2 111.45(15) 3_655 . ? O5 Nd1 O4 81.74(14) 3_655 3_655 ? O1 Nd1 O4 98.09(16) . 3_655 ? O8 Nd1 O4 89.90(15) . 3_655 ? O7 Nd1 O4 121.23(14) 3_655 3_655 ? O3 Nd1 O4 52.27(14) 3_655 3_655 ? O2 Nd1 O4 73.71(15) . 3_655 ? O5 Nd1 O6 121.25(13) 3_655 . ? O1 Nd1 O6 72.30(15) . . ? O8 Nd1 O6 80.43(14) . . ? O7 Nd1 O6 85.19(14) 3_655 . ? O3 Nd1 O6 145.02(15) 3_655 . ? O2 Nd1 O6 75.86(15) . . ? O4 Nd1 O6 149.56(14) 3_655 . ? O5 Nd1 O5 72.07(15) 3_655 . ? O1 Nd1 O5 110.76(15) . . ? O8 Nd1 O5 70.43(13) . . ? O7 Nd1 O5 65.94(13) 3_655 . ? O3 Nd1 O5 130.15(13) 3_655 . ? O2 Nd1 O5 117.79(14) . . ? O4 Nd1 O5 151.02(14) 3_655 . ? O6 Nd1 O5 49.91(13) . . ? O5 Nd1 C44 76.42(16) 3_655 3_655 ? O1 Nd1 C44 89.83(18) . 3_655 ? O8 Nd1 C44 112.21(18) . 3_655 ? O7 Nd1 C44 94.56(17) 3_655 3_655 ? O3 Nd1 C44 25.70(15) 3_655 3_655 ? O2 Nd1 C44 94.68(17) . 3_655 ? O4 Nd1 C44 26.76(15) 3_655 3_655 ? O6 Nd1 C44 161.67(17) . 3_655 ? O5 Nd1 C44 145.53(16) . 3_655 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 117.3(7) . . ? C7 C2 C1 121.0(7) . . ? C3 C2 C1 121.8(7) . . ? C2 C7 C6 123.0(7) . . ? C2 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C5 C6 C7 118.5(7) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C6 C5 C4 119.7(7) . . ? C6 C5 S1 118.9(6) . . ? C4 C5 S1 121.4(6) . . ? C5 C4 C3 120.6(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C2 C3 C4 120.8(8) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? N1 C8 C9 114.1(5) . . ? N1 C8 C33 108.5(5) . . ? C9 C8 C33 111.3(6) . . ? N1 C8 C21 106.4(6) . . ? C9 C8 C21 107.2(5) . . ? C33 C8 C21 109.2(5) . . ? O11 C9 C8 108.9(5) . . ? O11 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O11 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C19 122.1(7) . . ? C11 C10 O11 118.9(6) . . ? C19 C10 O11 118.9(6) . . ? C10 C11 C12 119.4(7) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C17 C12 C11 119.1(6) . . ? C17 C12 C13 118.8(6) . . ? C11 C12 C13 122.0(6) . . ? C14 C13 C12 120.7(7) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.2(7) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 120.7(8) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 119.9(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C18 119.8(7) . . ? C12 C17 C16 118.7(6) . . ? C18 C17 C16 121.5(7) . . ? C19 C18 C17 121.9(6) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C10 117.6(6) . . ? C18 C19 C20 119.0(6) . . ? C10 C19 C20 123.4(6) . . ? O7 C20 O8 125.7(6) . . ? O7 C20 C19 118.0(6) . . ? O8 C20 C19 116.3(6) . . ? O10 C33 C8 107.7(5) . . ? O10 C33 H33A 110.2 . . ? C8 C33 H33A 110.2 . . ? O10 C33 H33B 110.2 . . ? C8 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C35 C34 O10 123.5(6) . . ? C35 C34 C43 120.7(6) . . ? O10 C34 C43 115.5(6) . . ? C34 C35 C36 120.6(7) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C41 C36 C35 118.6(6) . . ? C41 C36 C37 119.3(6) . . ? C35 C36 C37 121.9(7) . . ? C38 C37 C36 120.4(7) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 121.0(7) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C40 C39 C38 119.9(7) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 121.6(7) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C42 C41 C40 123.5(7) . . ? C42 C41 C36 118.8(6) . . ? C40 C41 C36 117.7(7) . . ? C43 C42 C41 122.1(7) . . ? C43 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C42 C43 C34 119.0(6) . . ? C42 C43 C44 118.1(6) . . ? C34 C43 C44 122.8(6) . . ? O3 C44 O4 118.6(6) . . ? O3 C44 C43 123.7(6) . . ? O4 C44 C43 117.7(6) . . ? O3 C44 Nd1 58.6(3) . 3_655 ? O4 C44 Nd1 60.6(3) . 3_655 ? C43 C44 Nd1 170.6(5) . 3_655 ? O9 C21 C8 111.6(5) . . ? O9 C21 H21A 109.3 . . ? C8 C21 H21A 109.3 . . ? O9 C21 H21B 109.3 . . ? C8 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C23 C22 O9 118.1(6) . . ? C23 C22 C31 119.7(6) . . ? O9 C22 C31 122.2(6) . . ? C22 C23 C24 121.2(7) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C29 C24 C23 119.3(7) . . ? C29 C24 C25 119.0(7) . . ? C23 C24 C25 121.7(7) . . ? C26 C25 C24 119.3(8) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C27 C26 C25 120.8(8) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 121.4(8) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 118.9(8) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C24 C29 C30 119.0(7) . . ? C24 C29 C28 120.6(7) . . ? C30 C29 C28 120.4(7) . . ? C31 C30 C29 121.7(7) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C22 119.1(6) . . ? C30 C31 C32 118.6(6) . . ? C22 C31 C32 122.1(6) . . ? O6 C32 O5 120.4(6) . . ? O6 C32 C31 120.3(6) . . ? O5 C32 C31 119.3(6) . . ? O2 C50 N3B 127.5(9) . . ? O2 C50 N3A 113.8(10) . . ? O2 C50 H50A 115.5 . . ? N3B C50 H50A 116.7 . . ? N3A C50 H50A 117.4 . . ? O2 C50 H50B 122.9 . . ? N3B C50 H50B 98.9 . . ? N3A C50 H50B 77.4 . . ? N2 C46 H46A 109.5 . . ? N2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N2 C45 H45A 109.5 . . ? N2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O1 C47 N2 125.3(9) . . ? O1 C47 H47 117.3 . . ? N2 C47 H47 117.3 . . ? N3A C49A H49A 112.6 . . ? N3A C49A H49C 106.4 . . ? H49A C49A H49C 109.5 . . ? N3A C49A H49B 109.3 . . ? H49A C49A H49B 109.5 . . ? H49C C49A H49B 109.5 . . ? N3A C49A H49D 152.5 . . ? H49A C49A H49D 81.8 . . ? H49C C49A H49D 89.2 . . ? N3A C49A H49F 106.2 . . ? H49A C49A H49F 134.5 . . ? H49B C49A H49F 77.7 . . ? H49D C49A H49F 74.1 . . ? N3A C48A H48D 87.9 . . ? H48B C48A H48D 98.0 . . ? H48C C48A H48D 139.2 . . ? N3A C48A H48E 110.7 . . ? H48A C48A H48E 80.1 . . ? H48C C48A H48E 132.2 . . ? H48D C48A H48E 66.9 . . ? N3B C49B H49C 86.1 . . ? N3B C49B H49B 85.2 . . ? H49C C49B H49B 102.2 . . ? N3B C49B H49D 107.4 . . ? H49C C49B H49D 67.4 . . ? N3B C49B H49E 120.6 . . ? H49C C49B H49E 151.3 . . ? H49B C49B H49E 91.2 . . ? H49D C49B H49E 109.5 . . ? N3B C49B H49F 99.7 . . ? H49C C49B H49F 50.9 . . ? H49B C49B H49F 151.6 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? N3B C48B H48D 106.8 . . ? N3B C48B H48E 143.1 . . ? H48D C48B H48E 109.5 . . ? N3B C48B H48F 50.2 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C8 N1 S1 126.5(5) . . ? C8 N1 H1 116.8 . . ? S1 N1 H1 116.8 . . ? C47 N2 C45 123.0(9) . . ? C47 N2 C46 117.3(8) . . ? C45 N2 C46 119.7(8) . . ? C48A N3A C50 129.9(16) . . ? C48A N3A C49A 117.1(17) . . ? C50 N3A C49A 105.6(15) . . ? C50 N3B C48B 116.1(11) . . ? C50 N3B C49B 124.1(11) . . ? C48B N3B C49B 119.6(12) . . ? C50 N3B H48F 120.8 . . ? C49B N3B H48F 104.4 . . ? C50 O2 Nd1 131.1(5) . . ? C47 O1 Nd1 133.8(6) . . ? C32 O5 Nd1 160.0(4) . 3_655 ? C32 O5 Nd1 91.3(4) . . ? Nd1 O5 Nd1 107.93(15) 3_655 . ? C32 O6 Nd1 97.8(4) . . ? C44 O3 Nd1 95.7(4) . 3_655 ? C44 O4 Nd1 92.6(4) . 3_655 ? C20 O8 Nd1 138.8(4) . . ? C20 O7 Nd1 137.7(4) . 3_655 ? C34 O10 C33 119.1(5) . . ? C22 O9 C21 116.7(5) . . ? C10 O11 C9 114.5(5) . . ? O13 S1 O12 119.2(3) . . ? O13 S1 N1 105.6(3) . . ? O12 S1 N1 109.5(3) . . ? O13 S1 C5 106.4(3) . . ? O12 S1 C5 106.7(3) . . ? N1 S1 C5 109.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.721 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.109 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 795981' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H92 Eu2 N6 O26 S2' _chemical_formula_weight 2161.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2797(10) _cell_length_b 27.072(2) _cell_length_c 16.6564(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.9390(10) _cell_angle_gamma 90.00 _cell_volume 5785.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8025 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50603 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.27 _reflns_number_total 13989 _reflns_number_gt 9295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0562P)^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_number_reflns 13989 _refine_ls_number_parameters 644 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C49A C 0.4873(10) 0.5494(4) 0.4408(10) 0.099(4) Uani 0.578(9) 1 d PDU A 1 H49A H 0.4484 0.5747 0.4592 0.119 Uiso 0.578(9) 1 d PR A 1 H49B H 0.5464 0.5397 0.4842 0.119 Uiso 0.578(9) 1 d PR A 1 H49C H 0.5094 0.5597 0.3932 0.119 Uiso 0.578(9) 1 d PR A 1 C48A C 0.4581(11) 0.4609(4) 0.3919(11) 0.101(3) Uani 0.578(9) 1 d PDU A 1 H48A H 0.4003 0.4376 0.3802 0.122 Uiso 0.578(9) 1 d PR A 1 H48B H 0.5153 0.4466 0.4322 0.122 Uiso 0.578(9) 1 d PR A 1 H48C H 0.4783 0.4666 0.3412 0.122 Uiso 0.578(9) 1 d PR A 1 N3A N 0.4221(7) 0.5052(3) 0.4201(8) 0.070(2) Uani 0.578(9) 1 d PDU A 1 N3B N 0.3871(11) 0.5078(4) 0.3671(10) 0.072(3) Uani 0.422(9) 1 d PDU A 2 C49B C 0.4496(14) 0.5532(6) 0.3771(14) 0.095(4) Uani 0.422(9) 1 d PDU A 2 H48D H 0.4190 0.5784 0.4027 0.115 Uiso 0.422(9) 1 d PR A 2 H49E H 0.5160 0.5444 0.4117 0.115 Uiso 0.422(9) 1 d PR A 2 H49F H 0.4560 0.5644 0.3237 0.115 Uiso 0.422(9) 1 d PR A 2 C48B C 0.4169(14) 0.4661(5) 0.3273(12) 0.082(4) Uani 0.422(9) 1 d PDU A 2 H49D H 0.3654 0.4398 0.3224 0.099 Uiso 0.422(9) 1 d PR A 2 H48E H 0.4824 0.4538 0.3594 0.099 Uiso 0.422(9) 1 d PR A 2 H48F H 0.4224 0.4748 0.2724 0.099 Uiso 0.422(9) 1 d PR A 2 Eu1 Eu 0.097525(15) 0.458060(7) 0.450711(12) 0.02815(7) Uani 1 1 d . . . C1 C -0.7222(4) 0.3166(2) 0.3714(4) 0.0800(19) Uani 1 1 d . . . H1A H -0.7365 0.2967 0.3221 0.120 Uiso 1 1 calc R . . H1B H -0.7203 0.3508 0.3564 0.120 Uiso 1 1 calc R . . H1C H -0.7759 0.3117 0.3996 0.120 Uiso 1 1 calc R . . C2 C -0.6183(4) 0.3020(2) 0.4279(3) 0.0548(13) Uani 1 1 d . . . C3 C -0.5676(4) 0.2590(2) 0.4179(4) 0.0699(16) Uani 1 1 d . . . H3 H -0.5974 0.2385 0.3734 0.084 Uiso 1 1 calc R . . C4 C -0.4743(4) 0.24538(19) 0.4713(4) 0.0611(15) Uani 1 1 d . . . H4 H -0.4417 0.2161 0.4632 0.073 Uiso 1 1 calc R . . C5 C -0.4303(3) 0.27593(16) 0.5371(3) 0.0409(10) Uani 1 1 d . . . C6 C -0.4785(3) 0.31952(17) 0.5483(3) 0.0451(11) Uani 1 1 d . . . H6 H -0.4480 0.3404 0.5922 0.054 Uiso 1 1 calc R . . C7 C -0.5719(4) 0.33191(19) 0.4941(3) 0.0497(12) Uani 1 1 d . . . H7 H -0.6046 0.3612 0.5022 0.060 Uiso 1 1 calc R . . C8 C -0.1605(3) 0.31955(15) 0.5856(3) 0.0369(10) Uani 1 1 d . . . C9 C -0.2069(3) 0.32584(15) 0.4921(3) 0.0395(10) Uani 1 1 d . . . H9A H -0.1519 0.3324 0.4648 0.047 Uiso 1 1 calc R . . H9B H -0.2428 0.2959 0.4687 0.047 Uiso 1 1 calc R . . C10 C -0.3174(3) 0.38043(14) 0.3962(2) 0.0332(9) Uani 1 1 d . . . C11 C -0.4063(3) 0.35937(15) 0.3492(3) 0.0364(10) Uani 1 1 d . . . H11 H -0.4396 0.3351 0.3723 0.044 Uiso 1 1 calc R . . C12 C -0.4487(3) 0.37394(16) 0.2658(3) 0.0369(10) Uani 1 1 d . . . C13 C -0.5410(4) 0.35345(18) 0.2147(3) 0.0520(12) Uani 1 1 d . . . H13 H -0.5762 0.3293 0.2364 0.062 Uiso 1 1 calc R . . C14 C -0.5791(4) 0.3680(2) 0.1357(3) 0.0654(15) Uani 1 1 d . . . H14 H -0.6396 0.3537 0.1033 0.079 Uiso 1 1 calc R . . C15 C -0.5289(4) 0.4042(2) 0.1026(3) 0.0738(17) Uani 1 1 d . . . H15 H -0.5564 0.4145 0.0481 0.089 Uiso 1 1 calc R . . C16 C -0.4388(4) 0.4252(2) 0.1492(3) 0.0622(15) Uani 1 1 d . . . H16 H -0.4056 0.4495 0.1260 0.075 Uiso 1 1 calc R . . C17 C -0.3963(3) 0.41027(16) 0.2317(3) 0.0406(10) Uani 1 1 d . . . C18 C -0.3037(3) 0.43070(16) 0.2815(3) 0.0403(10) Uani 1 1 d . . . H18 H -0.2684 0.4542 0.2585 0.048 Uiso 1 1 calc R . . C19 C -0.2638(3) 0.41722(15) 0.3627(2) 0.0324(9) Uani 1 1 d . . . C20 C -0.1681(3) 0.44306(14) 0.4145(2) 0.0311(9) Uani 1 1 d . . . C33 C -0.0704(3) 0.28148(16) 0.6030(3) 0.0487(12) Uani 1 1 d . . . H33A H -0.0439 0.2763 0.6624 0.058 Uiso 1 1 calc R . . H33B H -0.0948 0.2501 0.5772 0.058 Uiso 1 1 calc R . . C34 C 0.1091(3) 0.29085(16) 0.6076(3) 0.0426(11) Uani 1 1 d . . . C35 C 0.1403(3) 0.25141(17) 0.6607(3) 0.0489(12) Uani 1 1 d . . . H35 H 0.0906 0.2292 0.6691 0.059 Uiso 1 1 calc R . . C36 C 0.2464(4) 0.24416(17) 0.7025(3) 0.0487(12) Uani 1 1 d . . . C37 C 0.2807(4) 0.20500(18) 0.7600(3) 0.0580(15) Uani 1 1 d . . . H37 H 0.2323 0.1826 0.7702 0.070 Uiso 1 1 calc R . . C38 C 0.3812(4) 0.1999(2) 0.7995(4) 0.0648(16) Uani 1 1 d . . . H38 H 0.4016 0.1737 0.8363 0.078 Uiso 1 1 calc R . . C39 C 0.4565(4) 0.2328(2) 0.7869(3) 0.0644(15) Uani 1 1 d . . . H39 H 0.5262 0.2289 0.8154 0.077 Uiso 1 1 calc R . . C40 C 0.4263(4) 0.2711(2) 0.7318(3) 0.0588(14) Uani 1 1 d . . . H40 H 0.4763 0.2928 0.7223 0.071 Uiso 1 1 calc R . . C41 C 0.3215(3) 0.27807(16) 0.6896(3) 0.0424(11) Uani 1 1 d . . . C42 C 0.2866(3) 0.31791(16) 0.6344(3) 0.0414(11) Uani 1 1 d . . . H42 H 0.3358 0.3403 0.6259 0.050 Uiso 1 1 calc R . . C43 C 0.1856(3) 0.32522(15) 0.5934(3) 0.0373(10) Uani 1 1 d . . . C44 C 0.1579(3) 0.36915(15) 0.5366(3) 0.0376(10) Uani 1 1 d . . . C21 C -0.1196(3) 0.36982(16) 0.6180(3) 0.0412(10) Uani 1 1 d . . . H21A H -0.0702 0.3814 0.5882 0.049 Uiso 1 1 calc R . . H21B H -0.1768 0.3932 0.6086 0.049 Uiso 1 1 calc R . . C22 C 0.0360(3) 0.37824(16) 0.7303(3) 0.0376(10) Uani 1 1 d . . . C23 C 0.0976(4) 0.34892(18) 0.7893(3) 0.0487(12) Uani 1 1 d . . . H23 H 0.0682 0.3224 0.8106 0.058 Uiso 1 1 calc R . . C24 C 0.2051(4) 0.35805(18) 0.8184(3) 0.0474(12) Uani 1 1 d . . . C25 C 0.2723(5) 0.3283(2) 0.8808(3) 0.0671(16) Uani 1 1 d . . . H25 H 0.2446 0.3024 0.9050 0.081 Uiso 1 1 calc R . . C26 C 0.3741(5) 0.3374(3) 0.9045(4) 0.083(2) Uani 1 1 d . . . H26 H 0.4166 0.3176 0.9450 0.100 Uiso 1 1 calc R . . C27 C 0.4177(5) 0.3753(3) 0.8705(4) 0.084(2) Uani 1 1 d . . . H27 H 0.4892 0.3806 0.8881 0.101 Uiso 1 1 calc R . . C28 C 0.3576(4) 0.4056(2) 0.8110(3) 0.0664(15) Uani 1 1 d . . . H28 H 0.3880 0.4315 0.7889 0.080 Uiso 1 1 calc R . . C29 C 0.2494(4) 0.39707(18) 0.7836(3) 0.0474(11) Uani 1 1 d . . . C30 C 0.1835(3) 0.42674(16) 0.7221(3) 0.0402(10) Uani 1 1 d . . . H30 H 0.2128 0.4522 0.6982 0.048 Uiso 1 1 calc R . . C31 C 0.0786(3) 0.41924(14) 0.6965(2) 0.0323(9) Uani 1 1 d . . . C32 C 0.0132(3) 0.45600(14) 0.6394(2) 0.0321(9) Uani 1 1 d . . . C45 C -0.0476(7) 0.3595(3) 0.1334(4) 0.134(3) Uani 1 1 d . . . H45B H -0.0388 0.3243 0.1339 0.201 Uiso 1 1 calc R . . H45A H -0.0473 0.3722 0.0797 0.201 Uiso 1 1 calc R . . H45C H -0.1128 0.3674 0.1452 0.201 Uiso 1 1 calc R . . C46 C 0.1390(7) 0.3808(3) 0.1826(4) 0.112(3) Uani 1 1 d . . . H46C H 0.1343 0.3874 0.1251 0.168 Uiso 1 1 calc R . . H46B H 0.1698 0.3489 0.1971 0.168 Uiso 1 1 calc R . . H46A H 0.1813 0.4056 0.2165 0.168 Uiso 1 1 calc R . . C47 C 0.0229(5) 0.3999(2) 0.2643(3) 0.0645(15) Uani 1 1 d . . . H47 H -0.0448 0.4006 0.2703 0.077 Uiso 1 1 calc R . . C50 C 0.3224(5) 0.5050(2) 0.4212(4) 0.0762(18) Uani 1 1 d U . . H50B H 0.2915 0.5358 0.4269 0.091 Uiso 0.50 1 d PR A . H50A H 0.3165 0.5308 0.4579 0.091 Uiso 0.50 1 d PR . . N1 N -0.2373(3) 0.30488(13) 0.6307(2) 0.0397(8) Uani 1 1 d . . . H1 H -0.2415 0.3233 0.6718 0.048 Uiso 1 1 calc R . . N2 N 0.0369(5) 0.38159(17) 0.1960(3) 0.0723(14) Uani 1 1 d . . . O1 O 0.0922(3) 0.41650(12) 0.3218(2) 0.0518(8) Uani 1 1 d . . . O2 O 0.2646(2) 0.46990(12) 0.4148(2) 0.0500(8) Uani 1 1 d . A . O5 O 0.0326(2) 0.46585(9) 0.57082(16) 0.0339(6) Uani 1 1 d . . . O6 O -0.0580(2) 0.47796(11) 0.66186(18) 0.0418(7) Uani 1 1 d . . . O3 O 0.2241(2) 0.40348(11) 0.5435(2) 0.0462(8) Uani 1 1 d . . . O4 O 0.0716(2) 0.37187(11) 0.4843(2) 0.0490(8) Uani 1 1 d . . . O7 O -0.0849(2) 0.43561(10) 0.39631(18) 0.0385(7) Uani 1 1 d . . . O8 O -0.1829(2) 0.47206(11) 0.47006(18) 0.0395(7) Uani 1 1 d . . . O9 O -0.0691(2) 0.36726(12) 0.70574(18) 0.0497(8) Uani 1 1 d . . . O10 O 0.0081(2) 0.30086(13) 0.5694(2) 0.0580(10) Uani 1 1 d . . . O11 O -0.2788(2) 0.36663(10) 0.47938(17) 0.0384(7) Uani 1 1 d . . . O13 O -0.3430(3) 0.24864(14) 0.6874(2) 0.0693(11) Uani 1 1 d . . . O12 O -0.2680(3) 0.21959(11) 0.5733(3) 0.0651(10) Uani 1 1 d . . . S1 S -0.31471(9) 0.25796(4) 0.61137(8) 0.0478(3) 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 C49A 0.085(6) 0.093(6) 0.117(7) 0.004(6) 0.020(5) -0.009(5) C48A 0.088(6) 0.096(6) 0.129(7) -0.008(6) 0.044(5) 0.008(5) N3A 0.058(4) 0.058(4) 0.103(5) -0.004(4) 0.037(4) -0.003(4) N3B 0.075(5) 0.064(5) 0.095(6) 0.003(5) 0.055(5) -0.012(4) C49B 0.094(7) 0.089(6) 0.112(7) 0.000(6) 0.042(6) -0.017(6) C48B 0.082(6) 0.081(6) 0.098(7) -0.012(6) 0.048(5) -0.002(5) Eu1 0.02890(11) 0.02546(10) 0.03044(11) 0.00065(9) 0.00830(8) -0.00016(9) C1 0.042(3) 0.100(5) 0.086(4) -0.010(4) -0.006(3) 0.003(3) C2 0.035(3) 0.067(4) 0.065(3) 0.003(3) 0.016(3) -0.005(2) C3 0.053(4) 0.071(4) 0.082(4) -0.025(3) 0.011(3) -0.016(3) C4 0.044(3) 0.044(3) 0.091(4) -0.013(3) 0.010(3) 0.001(2) C5 0.022(2) 0.038(2) 0.061(3) 0.005(2) 0.009(2) -0.0047(18) C6 0.041(3) 0.044(3) 0.050(3) 0.003(2) 0.012(2) 0.003(2) C7 0.039(3) 0.058(3) 0.054(3) 0.005(2) 0.014(2) 0.008(2) C8 0.030(2) 0.033(2) 0.047(3) 0.0096(19) 0.0078(19) -0.0035(18) C9 0.040(3) 0.031(2) 0.047(3) 0.0020(19) 0.010(2) 0.0014(19) C10 0.036(2) 0.030(2) 0.034(2) -0.0031(17) 0.0087(18) 0.0032(17) C11 0.029(2) 0.034(2) 0.046(3) -0.0002(19) 0.0105(19) -0.0031(17) C12 0.026(2) 0.038(2) 0.042(2) -0.0092(19) 0.0007(18) 0.0003(18) C13 0.035(3) 0.055(3) 0.059(3) -0.006(2) -0.001(2) -0.008(2) C14 0.044(3) 0.072(4) 0.066(4) -0.010(3) -0.012(3) -0.013(3) C15 0.062(4) 0.096(5) 0.044(3) -0.001(3) -0.019(3) -0.011(3) C16 0.062(4) 0.070(4) 0.045(3) 0.008(3) -0.004(3) -0.013(3) C17 0.040(3) 0.039(2) 0.039(2) -0.005(2) 0.003(2) -0.005(2) C18 0.042(3) 0.036(2) 0.042(3) 0.0005(19) 0.009(2) -0.007(2) C19 0.029(2) 0.035(2) 0.032(2) -0.0054(17) 0.0062(18) -0.0015(17) C20 0.035(2) 0.027(2) 0.028(2) 0.0006(16) 0.0037(18) -0.0039(17) C33 0.032(2) 0.043(3) 0.072(3) 0.022(2) 0.016(2) 0.001(2) C34 0.034(2) 0.039(2) 0.056(3) 0.012(2) 0.015(2) 0.008(2) C35 0.032(2) 0.042(3) 0.075(3) 0.023(2) 0.018(2) 0.004(2) C36 0.041(3) 0.045(3) 0.066(3) 0.023(2) 0.024(2) 0.016(2) C37 0.042(3) 0.057(3) 0.081(4) 0.035(3) 0.026(3) 0.012(2) C38 0.053(3) 0.068(4) 0.081(4) 0.040(3) 0.030(3) 0.023(3) C39 0.039(3) 0.081(4) 0.070(4) 0.030(3) 0.009(3) 0.018(3) C40 0.040(3) 0.063(3) 0.072(4) 0.024(3) 0.013(3) 0.007(2) C41 0.034(2) 0.042(3) 0.052(3) 0.017(2) 0.014(2) 0.009(2) C42 0.036(2) 0.043(3) 0.050(3) 0.014(2) 0.020(2) 0.004(2) C43 0.036(2) 0.035(2) 0.044(3) 0.0114(19) 0.015(2) 0.0084(18) C44 0.039(3) 0.032(2) 0.047(3) 0.0061(19) 0.019(2) 0.0072(19) C21 0.034(2) 0.046(3) 0.036(2) 0.012(2) -0.0056(19) -0.006(2) C22 0.033(2) 0.041(2) 0.035(2) 0.0046(19) 0.0024(19) -0.0066(19) C23 0.050(3) 0.048(3) 0.042(3) 0.016(2) 0.000(2) -0.005(2) C24 0.047(3) 0.051(3) 0.040(3) 0.008(2) 0.001(2) 0.007(2) C25 0.064(4) 0.076(4) 0.051(3) 0.018(3) -0.005(3) 0.007(3) C26 0.061(4) 0.099(5) 0.072(4) 0.023(4) -0.013(3) 0.023(4) C27 0.042(3) 0.120(6) 0.077(4) 0.005(4) -0.009(3) 0.015(4) C28 0.040(3) 0.089(4) 0.061(3) 0.008(3) -0.002(3) 0.001(3) C29 0.039(3) 0.055(3) 0.043(3) 0.001(2) 0.001(2) 0.002(2) C30 0.039(3) 0.042(3) 0.040(2) 0.004(2) 0.009(2) -0.001(2) C31 0.032(2) 0.032(2) 0.030(2) 0.0016(17) 0.0044(18) 0.0020(17) C32 0.034(2) 0.027(2) 0.034(2) 0.0020(18) 0.0059(17) -0.0036(18) C45 0.160(8) 0.169(8) 0.063(5) -0.042(5) 0.011(5) -0.057(7) C46 0.157(8) 0.120(6) 0.068(5) -0.007(4) 0.046(5) 0.041(6) C47 0.084(4) 0.060(3) 0.052(3) -0.008(3) 0.023(3) -0.013(3) C50 0.071(4) 0.061(4) 0.113(5) -0.001(3) 0.052(4) 0.009(3) N1 0.034(2) 0.040(2) 0.045(2) 0.0085(17) 0.0094(17) -0.0004(16) N2 0.110(4) 0.064(3) 0.042(3) -0.010(2) 0.019(3) -0.008(3) O1 0.066(2) 0.0463(19) 0.0459(19) -0.0121(16) 0.0193(18) -0.0016(17) O2 0.0427(19) 0.050(2) 0.063(2) -0.0005(16) 0.0238(17) -0.0075(15) O5 0.0373(16) 0.0334(16) 0.0323(15) 0.0059(12) 0.0111(13) -0.0004(12) O6 0.0494(19) 0.0410(17) 0.0387(17) 0.0083(14) 0.0179(15) 0.0133(15) O3 0.0350(17) 0.0407(18) 0.064(2) 0.0185(15) 0.0146(15) 0.0024(14) O4 0.0459(19) 0.0382(17) 0.055(2) 0.0124(15) -0.0007(16) -0.0046(15) O7 0.0279(16) 0.0364(16) 0.0497(18) -0.0089(14) 0.0073(14) -0.0006(13) O8 0.0356(17) 0.0442(17) 0.0403(17) -0.0099(13) 0.0127(14) -0.0090(13) O9 0.0416(18) 0.061(2) 0.0421(18) 0.0173(16) 0.0019(14) -0.0155(16) O10 0.0268(17) 0.069(2) 0.079(2) 0.0389(19) 0.0154(17) 0.0069(16) O11 0.0377(17) 0.0386(16) 0.0363(16) 0.0027(13) 0.0052(13) 0.0068(13) O13 0.050(2) 0.086(3) 0.077(3) 0.039(2) 0.0259(19) 0.0027(19) O12 0.044(2) 0.0345(18) 0.122(3) 0.0082(19) 0.030(2) 0.0057(15) S1 0.0327(6) 0.0399(6) 0.0729(8) 0.0199(6) 0.0174(6) 0.0017(5) _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_ _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 -0.008 0.000 0.500 745 111 ' ' 2 -0.004 0.500 1.000 745 111 ' ' _platon_squeeze_details ; ; 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 C49A N3A 1.465(11) . ? C49A H49A 0.9556 . ? C49A H49B 0.9561 . ? C49A H49C 0.9561 . ? C49A H48D 1.2435 . ? C49A H49E 0.7024 . ? C48A N3A 1.415(11) . ? C48A H48A 0.9732 . ? C48A H48B 0.9573 . ? C48A H48C 0.9615 . ? C48A H48E 0.7239 . ? N3A C50 1.328(10) . ? N3B C50 1.398(13) . ? N3B C48B 1.417(13) . ? N3B C49B 1.466(14) . ? C49B H49C 0.7912 . ? C49B H48D 0.9503 . ? C49B H49E 0.9512 . ? C49B H49F 0.9647 . ? C48B H48A 1.2324 . ? C48B H48C 0.7883 . ? C48B H49D 0.9753 . ? C48B H48E 0.9556 . ? C48B H48F 0.9659 . ? Eu1 O5 2.384(3) . ? Eu1 O1 2.409(3) . ? Eu1 O8 2.415(3) 3_566 ? Eu1 O7 2.435(3) . ? Eu1 O4 2.444(3) . ? Eu1 O3 2.462(3) . ? Eu1 O2 2.464(3) . ? Eu1 O6 2.507(3) 3_566 ? Eu1 O5 2.653(3) 3_566 ? Eu1 C44 2.809(4) . ? Eu1 C32 2.948(4) 3_566 ? Eu1 Eu1 4.0932(4) 3_566 ? C1 C2 1.509(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(7) . ? C2 C7 1.378(7) . ? C3 C4 1.377(7) . ? C3 H3 0.9300 . ? C4 C5 1.377(7) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 S1 1.773(4) . ? C6 C7 1.375(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.469(5) . ? C8 C21 1.512(6) . ? C8 C9 1.531(6) . ? C8 C33 1.548(6) . ? C9 O11 1.440(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.362(5) . ? C10 O11 1.398(5) . ? C10 C19 1.420(5) . ? C11 C12 1.414(6) . ? C11 H11 0.9300 . ? C12 C17 1.407(6) . ? C12 C13 1.413(6) . ? C13 C14 1.341(7) . ? C13 H13 0.9300 . ? C14 C15 1.379(8) . ? C14 H14 0.9300 . ? C15 C16 1.369(7) . ? C15 H15 0.9300 . ? C16 C17 1.403(6) . ? C16 H16 0.9300 . ? C17 C18 1.407(6) . ? C18 C19 1.368(6) . ? C18 H18 0.9300 . ? C19 C20 1.511(5) . ? C20 O7 1.235(5) . ? C20 O8 1.266(5) . ? C33 O10 1.406(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O10 1.355(5) . ? C34 C35 1.380(6) . ? C34 C43 1.442(6) . ? C35 C36 1.416(6) . ? C35 H35 0.9300 . ? C36 C41 1.412(6) . ? C36 C37 1.422(6) . ? C37 C38 1.335(7) . ? C37 H37 0.9300 . ? C38 C39 1.396(7) . ? C38 H38 0.9300 . ? C39 C40 1.375(7) . ? C39 H39 0.9300 . ? C40 C41 1.400(6) . ? C40 H40 0.9300 . ? C41 C42 1.416(6) . ? C42 C43 1.353(6) . ? C42 H42 0.9300 . ? C43 C44 1.505(6) . ? C44 O4 1.251(5) . ? C44 O3 1.264(5) . ? C21 O9 1.444(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.360(6) . ? C22 O9 1.382(5) . ? C22 C31 1.426(5) . ? C23 C24 1.406(6) . ? C23 H23 0.9300 . ? C24 C29 1.405(6) . ? C24 C25 1.432(6) . ? C25 C26 1.330(8) . ? C25 H25 0.9300 . ? C26 C27 1.372(9) . ? C26 H26 0.9300 . ? C27 C28 1.373(8) . ? C27 H27 0.9300 . ? C28 C29 1.411(7) . ? C28 H28 0.9300 . ? C29 C30 1.414(6) . ? C30 C31 1.362(6) . ? C30 H30 0.9300 . ? C31 C32 1.491(5) . ? C32 O6 1.253(5) . ? C32 O5 1.263(4) . ? C32 Eu1 2.948(4) 3_566 ? C45 N2 1.449(8) . ? C45 H45B 0.9600 . ? C45 H45A 0.9600 . ? C45 H45C 0.9600 . ? C46 N2 1.430(8) . ? C46 H46C 0.9600 . ? C46 H46B 0.9600 . ? C46 H46A 0.9600 . ? C47 O1 1.228(6) . ? C47 N2 1.299(6) . ? C47 H47 0.9300 . ? C50 O2 1.208(6) . ? C50 H50B 0.9444 . ? C50 H50A 0.9444 . ? N1 S1 1.613(4) . ? N1 H1 0.8600 . ? O5 Eu1 2.653(3) 3_566 ? O6 Eu1 2.507(3) 3_566 ? O8 Eu1 2.415(3) 3_566 ? O13 S1 1.434(3) . ? O12 S1 1.438(3) . ? 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 N3A C49A H49A 109.1 . . ? N3A C49A H49B 106.0 . . ? H49A C49A H49B 111.1 . . ? N3A C49A H49C 109.5 . . ? H49A C49A H49C 111.2 . . ? H49B C49A H49C 109.8 . . ? N3A C49A H48D 95.0 . . ? H49A C49A H48D 47.6 . . ? H49B C49A H48D 155.1 . . ? H49C C49A H48D 74.4 . . ? N3A C49A H49E 94.3 . . ? H49A C49A H49E 142.4 . . ? H49B C49A H49E 89.0 . . ? H48D C49A H49E 102.9 . . ? N3A C48A H48A 107.4 . . ? N3A C48A H48B 112.6 . . ? H48A C48A H48B 108.7 . . ? N3A C48A H48C 110.5 . . ? H48A C48A H48C 108.3 . . ? H48B C48A H48C 109.3 . . ? N3A C48A H49D 106.7 . . ? H48B C48A H49D 134.7 . . ? H48C C48A H49D 75.8 . . ? N3A C48A H48E 136.6 . . ? H48A C48A H48E 99.2 . . ? H48B C48A H48E 89.4 . . ? H49D C48A H48E 76.6 . . ? C50 N3A C48A 115.1(9) . . ? C50 N3A C49A 122.1(9) . . ? C48A N3A C49A 122.7(10) . . ? C50 N3B C48B 123.3(11) . . ? C50 N3B C49B 113.4(11) . . ? C48B N3B C49B 120.2(13) . . ? N3B C49B H49A 107.1 . . ? N3B C49B H49C 135.8 . . ? H49A C49B H49C 81.3 . . ? N3B C49B H48D 111.0 . . ? H49C C49B H48D 101.2 . . ? N3B C49B H49E 105.6 . . ? H49A C49B H49E 76.6 . . ? H48D C49B H49E 110.1 . . ? N3B C49B H49F 110.0 . . ? H49A C49B H49F 138.3 . . ? H49C C49B H49F 85.4 . . ? H48D C49B H49F 109.6 . . ? H49E C49B H49F 110.4 . . ? N3B C48B H48A 92.4 . . ? N3B C48B H48C 103.9 . . ? H48A C48B H48C 99.4 . . ? N3B C48B H49D 110.3 . . ? H48A C48B H49D 49.7 . . ? H48C C48B H49D 133.4 . . ? N3B C48B H48E 109.9 . . ? H48A C48B H48E 71.8 . . ? H49D C48B H48E 108.1 . . ? N3B C48B H48F 110.2 . . ? H48A C48B H48F 154.3 . . ? H48C C48B H48F 87.0 . . ? H49D C48B H48F 108.7 . . ? H48E C48B H48F 109.5 . . ? O5 Eu1 O1 148.83(10) . . ? O5 Eu1 O8 72.09(9) . 3_566 ? O1 Eu1 O8 139.00(10) . 3_566 ? O5 Eu1 O7 78.09(9) . . ? O1 Eu1 O7 75.76(11) . . ? O8 Eu1 O7 132.88(9) 3_566 . ? O5 Eu1 O4 77.86(10) . . ? O1 Eu1 O4 77.56(11) . . ? O8 Eu1 O4 134.16(10) 3_566 . ? O7 Eu1 O4 70.21(10) . . ? O5 Eu1 O3 82.09(10) . . ? O1 Eu1 O3 97.93(11) . . ? O8 Eu1 O3 88.77(11) 3_566 . ? O7 Eu1 O3 122.47(10) . . ? O4 Eu1 O3 52.92(10) . . ? O5 Eu1 O2 137.39(10) . . ? O1 Eu1 O2 70.47(11) . . ? O8 Eu1 O2 72.88(10) 3_566 . ? O7 Eu1 O2 144.52(11) . . ? O4 Eu1 O2 111.63(11) . . ? O3 Eu1 O2 73.66(10) . . ? O5 Eu1 O6 121.03(9) . 3_566 ? O1 Eu1 O6 72.75(10) . 3_566 ? O8 Eu1 O6 81.13(10) 3_566 3_566 ? O7 Eu1 O6 84.14(10) . 3_566 ? O4 Eu1 O6 144.69(10) . 3_566 ? O3 Eu1 O6 149.52(10) . 3_566 ? O2 Eu1 O6 75.89(10) . 3_566 ? O5 Eu1 O5 71.38(9) . 3_566 ? O1 Eu1 O5 111.94(10) . 3_566 ? O8 Eu1 O5 70.31(9) 3_566 3_566 ? O7 Eu1 O5 65.96(9) . 3_566 ? O4 Eu1 O5 130.31(9) . 3_566 ? O3 Eu1 O5 150.05(9) . 3_566 ? O2 Eu1 O5 117.52(9) . 3_566 ? O6 Eu1 O5 50.13(8) 3_566 3_566 ? O5 Eu1 C44 76.46(10) . . ? O1 Eu1 C44 89.59(12) . . ? O8 Eu1 C44 111.14(12) 3_566 . ? O7 Eu1 C44 95.84(12) . . ? O4 Eu1 C44 26.39(11) . . ? O3 Eu1 C44 26.72(11) . . ? O2 Eu1 C44 94.50(11) . . ? O6 Eu1 C44 161.83(11) 3_566 . ? O5 Eu1 C44 145.55(10) 3_566 . ? O5 Eu1 C32 96.70(10) . 3_566 ? O1 Eu1 C32 91.06(11) . 3_566 ? O8 Eu1 C32 76.25(11) 3_566 3_566 ? O7 Eu1 C32 71.92(10) . 3_566 ? O4 Eu1 C32 142.06(11) . 3_566 ? O3 Eu1 C32 164.52(11) . 3_566 ? O2 Eu1 C32 97.81(11) . 3_566 ? O6 Eu1 C32 24.92(10) 3_566 3_566 ? O5 Eu1 C32 25.36(9) 3_566 3_566 ? C44 Eu1 C32 167.16(12) . 3_566 ? O5 Eu1 Eu1 37.89(6) . 3_566 ? O1 Eu1 Eu1 137.76(8) . 3_566 ? O8 Eu1 Eu1 66.59(7) 3_566 3_566 ? O7 Eu1 Eu1 67.41(6) . 3_566 ? O4 Eu1 Eu1 107.26(8) . 3_566 ? O3 Eu1 Eu1 118.77(7) . 3_566 ? O2 Eu1 Eu1 136.72(8) . 3_566 ? O6 Eu1 Eu1 83.38(7) 3_566 3_566 ? O5 Eu1 Eu1 33.49(6) 3_566 3_566 ? C44 Eu1 Eu1 113.46(8) . 3_566 ? C32 Eu1 Eu1 58.82(8) 3_566 3_566 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.5(5) . . ? C3 C2 C1 122.9(5) . . ? C7 C2 C1 119.5(5) . . ? C2 C3 C4 122.4(5) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 118.7(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 S1 120.2(4) . . ? C6 C5 S1 119.3(4) . . ? C7 C6 C5 119.5(5) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C2 121.6(5) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? N1 C8 C21 107.1(4) . . ? N1 C8 C9 113.6(3) . . ? C21 C8 C9 106.0(3) . . ? N1 C8 C33 109.2(3) . . ? C21 C8 C33 110.1(4) . . ? C9 C8 C33 110.7(4) . . ? O11 C9 C8 108.2(3) . . ? O11 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? O11 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C11 C10 O11 120.0(4) . . ? C11 C10 C19 121.0(4) . . ? O11 C10 C19 119.0(4) . . ? C10 C11 C12 121.0(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C17 C12 C13 118.3(4) . . ? C17 C12 C11 118.6(4) . . ? C13 C12 C11 123.1(4) . . ? C14 C13 C12 121.6(5) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.6(5) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 118.7(4) . . ? C16 C17 C18 122.3(4) . . ? C12 C17 C18 119.0(4) . . ? C19 C18 C17 122.4(4) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C10 118.0(4) . . ? C18 C19 C20 119.7(4) . . ? C10 C19 C20 122.2(4) . . ? O7 C20 O8 126.7(4) . . ? O7 C20 C19 117.2(3) . . ? O8 C20 C19 116.0(4) . . ? O10 C33 C8 107.1(3) . . ? O10 C33 H33A 110.3 . . ? C8 C33 H33A 110.3 . . ? O10 C33 H33B 110.3 . . ? C8 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? O10 C34 C35 123.5(4) . . ? O10 C34 C43 116.6(4) . . ? C35 C34 C43 119.8(4) . . ? C34 C35 C36 121.2(4) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C41 C36 C35 119.2(4) . . ? C41 C36 C37 118.1(4) . . ? C35 C36 C37 122.7(4) . . ? C38 C37 C36 121.0(5) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 121.6(5) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C40 C39 C38 119.0(5) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C41 121.1(5) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C36 119.1(4) . . ? C40 C41 C42 123.0(4) . . ? C36 C41 C42 117.9(4) . . ? C43 C42 C41 123.8(4) . . ? C43 C42 H42 118.1 . . ? C41 C42 H42 118.1 . . ? C42 C43 C34 118.1(4) . . ? C42 C43 C44 118.9(4) . . ? C34 C43 C44 123.0(4) . . ? O4 C44 O3 120.8(4) . . ? O4 C44 C43 121.1(4) . . ? O3 C44 C43 118.2(4) . . ? O4 C44 Eu1 60.3(2) . . ? O3 C44 Eu1 61.1(2) . . ? C43 C44 Eu1 171.3(3) . . ? O9 C21 C8 110.4(3) . . ? O9 C21 H21A 109.6 . . ? C8 C21 H21A 109.6 . . ? O9 C21 H21B 109.6 . . ? C8 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 O9 117.5(4) . . ? C23 C22 C31 120.9(4) . . ? O9 C22 C31 121.6(4) . . ? C22 C23 C24 121.0(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C29 C24 C23 119.1(4) . . ? C29 C24 C25 118.3(5) . . ? C23 C24 C25 122.7(5) . . ? C26 C25 C24 120.5(6) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 121.4(6) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C28 121.2(6) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 119.3(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C24 C29 C28 119.4(5) . . ? C24 C29 C30 118.6(4) . . ? C28 C29 C30 122.0(5) . . ? C31 C30 C29 122.2(4) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C22 118.1(4) . . ? C30 C31 C32 118.7(4) . . ? C22 C31 C32 123.0(4) . . ? O6 C32 O5 121.0(4) . . ? O6 C32 C31 119.1(3) . . ? O5 C32 C31 119.8(4) . . ? O6 C32 Eu1 57.4(2) . 3_566 ? O5 C32 Eu1 64.1(2) . 3_566 ? C31 C32 Eu1 169.6(3) . 3_566 ? N2 C45 H45B 109.5 . . ? N2 C45 H45A 109.5 . . ? H45B C45 H45A 109.5 . . ? N2 C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? N2 C46 H46C 109.5 . . ? N2 C46 H46B 109.5 . . ? H46C C46 H46B 109.5 . . ? N2 C46 H46A 109.5 . . ? H46C C46 H46A 109.5 . . ? H46B C46 H46A 109.5 . . ? O1 C47 N2 125.1(6) . . ? O1 C47 H47 117.4 . . ? N2 C47 H47 117.4 . . ? O2 C50 N3A 127.9(6) . . ? O2 C50 N3B 117.9(7) . . ? O2 C50 H50B 114.8 . . ? N3A C50 H50B 117.3 . . ? N3B C50 H50B 111.8 . . ? O2 C50 H50A 118.7 . . ? N3A C50 H50A 104.8 . . ? N3B C50 H50A 122.9 . . ? C8 N1 S1 127.0(3) . . ? C8 N1 H1 116.5 . . ? S1 N1 H1 116.5 . . ? C47 N2 C46 119.9(6) . . ? C47 N2 C45 121.9(6) . . ? C46 N2 C45 118.1(6) . . ? C47 O1 Eu1 135.2(4) . . ? C50 O2 Eu1 132.2(3) . . ? C32 O5 Eu1 160.6(3) . . ? C32 O5 Eu1 90.5(2) . 3_566 ? Eu1 O5 Eu1 108.62(9) . 3_566 ? C32 O6 Eu1 97.6(2) . 3_566 ? C44 O3 Eu1 92.2(3) . . ? C44 O4 Eu1 93.3(3) . . ? C20 O7 Eu1 137.3(3) . . ? C20 O8 Eu1 138.2(3) . 3_566 ? C22 O9 C21 117.3(3) . . ? C34 O10 C33 119.0(3) . . ? C10 O11 C9 114.2(3) . . ? O13 S1 O12 120.3(2) . . ? O13 S1 N1 105.1(2) . . ? O12 S1 N1 109.36(19) . . ? O13 S1 C5 106.7(2) . . ? O12 S1 C5 106.5(2) . . ? N1 S1 C5 108.41(19) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.755 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.091 #==END data_4 _database_code_depnum_ccdc_archive 'CCDC 795982' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H92 Gd2 N6 O26 S2' _chemical_formula_weight 2172.42 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2855(3) _cell_length_b 27.0074(6) _cell_length_c 16.6357(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.9790(10) _cell_angle_gamma 90.00 _cell_volume 5766.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3464 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 19.18 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30356 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10144 _reflns_number_gt 6474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0329P)^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_number_reflns 10144 _refine_ls_number_parameters 643 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.596835(8) 0.041992(4) 0.950597(6) 0.03180(3) Uani 1 1 d . . . C1 C -0.2208(2) 0.18406(12) 0.87070(17) 0.0875(12) Uani 1 1 d . . . H1A H -0.2759 0.1938 0.8950 0.131 Uiso 1 1 calc R . . H1B H -0.2232 0.1489 0.8622 0.131 Uiso 1 1 calc R . . H1C H -0.2292 0.2005 0.8182 0.131 Uiso 1 1 calc R . . C2 C -0.11853(18) 0.19798(10) 0.92757(15) 0.0583(9) Uani 1 1 d . . . C3 C -0.06817(19) 0.24075(10) 0.91796(17) 0.0742(10) Uani 1 1 d . . . H3 H -0.0982 0.2615 0.8737 0.089 Uiso 1 1 calc R . . C4 C 0.02642(19) 0.25450(9) 0.97194(16) 0.0670(9) Uani 1 1 d . . . H4 H 0.0587 0.2839 0.9636 0.080 Uiso 1 1 calc R . . C5 C 0.07137(15) 0.22420(8) 1.03750(13) 0.0422(7) Uani 1 1 d . . . C6 C 0.02162(16) 0.18102(8) 1.04826(13) 0.0481(8) Uani 1 1 d . . . H6 H 0.0513 0.1603 1.0927 0.058 Uiso 1 1 calc R . . C7 C -0.07199(17) 0.16811(9) 0.99369(14) 0.0535(8) Uani 1 1 d . . . H7 H -0.1042 0.1386 1.0018 0.064 Uiso 1 1 calc R . . C8 C 0.33854(16) 0.18056(8) 1.08561(13) 0.0401(7) Uani 1 1 d . . . C9 C 0.29208(16) 0.17397(8) 0.99253(13) 0.0429(7) Uani 1 1 d . . . H9A H 0.2554 0.2038 0.9692 0.052 Uiso 1 1 calc R . . H9B H 0.3471 0.1679 0.9652 0.052 Uiso 1 1 calc R . . C10 C 0.18305(15) 0.11913(8) 0.89624(12) 0.0347(6) Uani 1 1 d . . . C11 C 0.09434(16) 0.14037(8) 0.84965(13) 0.0409(7) Uani 1 1 d . . . H11 H 0.0612 0.1647 0.8730 0.049 Uiso 1 1 calc R . . C12 C 0.05186(15) 0.12587(8) 0.76621(13) 0.0420(7) Uani 1 1 d . . . C13 C -0.04067(17) 0.14677(9) 0.71617(14) 0.0542(8) Uani 1 1 d . . . H13 H -0.0758 0.1711 0.7378 0.065 Uiso 1 1 calc R . . C14 C -0.0788(2) 0.13095(10) 0.63519(15) 0.0690(10) Uani 1 1 d . . . H14 H -0.1398 0.1448 0.6023 0.083 Uiso 1 1 calc R . . C15 C -0.0277(2) 0.09494(11) 0.60251(16) 0.0761(11) Uani 1 1 d . . . H15 H -0.0552 0.0844 0.5480 0.091 Uiso 1 1 calc R . . C16 C 0.0621(2) 0.07462(10) 0.64841(14) 0.0704(10) Uani 1 1 d . . . H16 H 0.0964 0.0509 0.6248 0.084 Uiso 1 1 calc R . . C17 C 0.10384(16) 0.08918(8) 0.73156(13) 0.0417(7) Uani 1 1 d . . . C18 C 0.19593(17) 0.06862(8) 0.78197(12) 0.0429(7) Uani 1 1 d . . . H18 H 0.2309 0.0448 0.7592 0.051 Uiso 1 1 calc R . . C19 C 0.23604(15) 0.08228(8) 0.86300(12) 0.0364(7) Uani 1 1 d . . . C20 C 0.33106(15) 0.05637(7) 0.91481(12) 0.0349(7) Uani 1 1 d . . . C21 C 0.38104(17) 0.12995(8) 1.11892(12) 0.0466(7) Uani 1 1 d . . . H21A H 0.3243 0.1063 1.1097 0.056 Uiso 1 1 calc R . . H21B H 0.4303 0.1185 1.0889 0.056 Uiso 1 1 calc R . . C22 C 0.53646(16) 0.12150(8) 1.23005(12) 0.0409(7) Uani 1 1 d . . . C23 C 0.59826(18) 0.15054(9) 1.28858(13) 0.0532(8) Uani 1 1 d . . . H23 H 0.5686 0.1771 1.3097 0.064 Uiso 1 1 calc R . . C24 C 0.70463(18) 0.14218(9) 1.31841(13) 0.0512(8) Uani 1 1 d . . . C25 C 0.7719(2) 0.17195(10) 1.37953(15) 0.0724(10) Uani 1 1 d . . . H25 H 0.7443 0.1982 1.4032 0.087 Uiso 1 1 calc R . . C26 C 0.8751(2) 0.16293(12) 1.40393(16) 0.0889(12) Uani 1 1 d . . . H26 H 0.9175 0.1829 1.4444 0.107 Uiso 1 1 calc R . . C27 C 0.9191(2) 0.12437(13) 1.36964(16) 0.0904(12) Uani 1 1 d . . . H27 H 0.9905 0.1188 1.3868 0.108 Uiso 1 1 calc R . . C28 C 0.85729(19) 0.09462(11) 1.31056(15) 0.0718(10) Uani 1 1 d . . . H28 H 0.8870 0.0686 1.2881 0.086 Uiso 1 1 calc R . . C29 C 0.74939(18) 0.10285(9) 1.28344(13) 0.0504(8) Uani 1 1 d . . . C30 C 0.68368(16) 0.07335(8) 1.22231(13) 0.0431(7) Uani 1 1 d . . . H30 H 0.7126 0.0475 1.1988 0.052 Uiso 1 1 calc R . . C31 C 0.57831(16) 0.08131(8) 1.19600(12) 0.0353(7) Uani 1 1 d . . . C32 C 0.51352(15) 0.04387(7) 1.14002(11) 0.0324(6) Uani 1 1 d . . . C33 C 0.42722(15) 0.21874(8) 1.10219(14) 0.0486(7) Uani 1 1 d . . . H33A H 0.4022 0.2500 1.0756 0.058 Uiso 1 1 calc R . . H33B H 0.4535 0.2244 1.1615 0.058 Uiso 1 1 calc R . . C34 C 0.60982(16) 0.20902(8) 1.10781(14) 0.0449(7) Uani 1 1 d . . . C35 C 0.64082(17) 0.24836(9) 1.15959(14) 0.0555(8) Uani 1 1 d . . . H35 H 0.5912 0.2709 1.1671 0.067 Uiso 1 1 calc R . . C36 C 0.74585(17) 0.25568(9) 1.20191(14) 0.0495(7) Uani 1 1 d . . . C37 C 0.78070(18) 0.29443(9) 1.25915(14) 0.0639(9) Uani 1 1 d . . . H37 H 0.7325 0.3171 1.2690 0.077 Uiso 1 1 calc R . . C38 C 0.88156(19) 0.29949(10) 1.29990(15) 0.0696(9) Uani 1 1 d . . . H38 H 0.9018 0.3250 1.3381 0.083 Uiso 1 1 calc R . . C39 C 0.95579(19) 0.26701(10) 1.28552(15) 0.0701(10) Uani 1 1 d . . . H39 H 1.0257 0.2716 1.3126 0.084 Uiso 1 1 calc R . . C40 C 0.92684(18) 0.22849(10) 1.23197(15) 0.0649(9) Uani 1 1 d . . . H40 H 0.9768 0.2064 1.2235 0.078 Uiso 1 1 calc R . . C41 C 0.82148(17) 0.22193(9) 1.18932(13) 0.0468(7) Uani 1 1 d . . . C42 C 0.78603(16) 0.18196(8) 1.13428(12) 0.0431(7) Uani 1 1 d . . . H42 H 0.8350 0.1594 1.1257 0.052 Uiso 1 1 calc R . . C43 C 0.68502(15) 0.17471(8) 1.09341(12) 0.0398(7) Uani 1 1 d . . . C44 C 0.65796(16) 0.13063(8) 1.03614(12) 0.0389(7) Uani 1 1 d . . . C45 C 0.4518(3) 0.13961(14) 0.63235(17) 0.1441(18) Uani 1 1 d . . . H45A H 0.4539 0.1270 0.5789 0.216 Uiso 1 1 calc R . . H45B H 0.4597 0.1750 0.6329 0.216 Uiso 1 1 calc R . . H45C H 0.3862 0.1313 0.6431 0.216 Uiso 1 1 calc R . . C46 C 0.6374(2) 0.11878(13) 0.68123(17) 0.1180(14) Uani 1 1 d . . . H46A H 0.6722 0.0880 0.6993 0.142 Uiso 1 1 d R . . H46B H 0.6770 0.1456 0.7117 0.142 Uiso 1 1 d R . . H46C H 0.6311 0.1232 0.6229 0.142 Uiso 1 1 d R . . C47 C 0.5225(2) 0.09969(10) 0.76476(15) 0.0706(10) Uani 1 1 d . . . H47 H 0.4548 0.0988 0.7707 0.085 Uiso 1 1 calc R . . C48A C 0.9547(4) 0.03895(17) 0.8808(3) 0.0998(15) Uani 0.595(2) 1 d PDU A 1 H48A H 0.9025 0.0640 0.8782 0.120 Uiso 0.595(2) 1 d PR A 1 H48B H 0.9635 0.0310 0.8282 0.120 Uiso 0.595(2) 1 d PR A 1 H48C H 1.0195 0.0500 0.9182 0.120 Uiso 0.595(2) 1 d PR A 1 C48B C 0.9042(6) 0.0321(2) 0.8125(4) 0.103(2) Uani 0.405(2) 1 d PDU A 2 H48D H 0.8576 0.0586 0.8228 0.123 Uiso 0.405(2) 1 d PR A 2 H48E H 0.9736 0.0406 0.8428 0.123 Uiso 0.405(2) 1 d PR A 2 H48F H 0.9006 0.0236 0.7628 0.123 Uiso 0.405(2) 1 d PR A 2 C49A C 0.9854(4) -0.04979(18) 0.9290(3) 0.1076(17) Uani 0.595(2) 1 d PDU A 1 H49A H 0.9490 -0.0687 0.9554 0.129 Uiso 0.595(2) 1 d PR A 1 H49B H 1.0050 -0.0587 0.8854 0.129 Uiso 0.595(2) 1 d PR A 1 H49C H 1.0510 -0.0387 0.9754 0.129 Uiso 0.595(2) 1 d PR A 1 C49B C 0.9324(6) -0.0553(3) 0.8557(5) 0.116(2) Uani 0.405(2) 1 d PDU A 2 H49D H 0.8859 -0.0804 0.8511 0.139 Uiso 0.405(2) 1 d PR A 2 H49E H 0.9789 -0.0504 0.9111 0.139 Uiso 0.405(2) 1 d PR A 2 H49F H 0.9719 -0.0504 0.8211 0.139 Uiso 0.405(2) 1 d PR A 2 N3A N 0.9182(3) -0.00505(13) 0.9155(2) 0.0713(11) Uani 0.595(2) 1 d PDU A 1 N3B N 0.8791(4) -0.0080(2) 0.8594(4) 0.0832(15) Uani 0.405(2) 1 d PDU A 2 C50 C 0.8179(2) -0.00527(11) 0.92001(18) 0.0871(11) Uani 1 1 d . . . H50A H 0.7883 -0.0278 0.9380 0.105 Uiso 0.50 1 d PR A . H50B H 0.8193 -0.0278 0.9680 0.105 Uiso 0.50 1 d PR . . N1 N 0.26293(12) 0.19585(6) 1.13075(10) 0.0417(6) Uani 1 1 d . . . H1 H 0.2598 0.1778 1.1726 0.050 Uiso 1 1 calc R . . N2 N 0.53544(19) 0.11802(8) 0.69584(12) 0.0769(9) Uani 1 1 d . . . O1 O 0.59100(12) 0.08363(6) 0.82218(9) 0.0534(5) Uani 1 1 d . . . O2 O 0.76213(11) 0.03045(6) 0.91469(10) 0.0552(5) Uani 1 1 d . A . O3 O 0.72312(11) 0.09621(5) 1.04280(9) 0.0492(5) Uani 1 1 d . . . O4 O 0.57058(12) 0.12807(6) 0.98351(9) 0.0526(5) Uani 1 1 d . . . O5 O 0.53268(10) 0.03437(5) 1.07018(8) 0.0371(4) Uani 1 1 d . . . O6 O 0.44204(11) 0.02149(5) 1.16181(8) 0.0459(5) Uani 1 1 d . . . O7 O 0.41539(10) 0.06380(5) 0.89560(8) 0.0416(5) Uani 1 1 d . . . O8 O 0.31698(10) 0.02745(5) 0.97020(8) 0.0417(5) Uani 1 1 d . . . O9 O 0.43155(11) 0.13242(6) 1.20585(8) 0.0517(5) Uani 1 1 d . . . O10 O 0.50800(11) 0.19923(6) 1.06865(10) 0.0624(6) Uani 1 1 d . . . O11 O 0.22164(10) 0.13301(5) 0.97930(8) 0.0407(5) Uani 1 1 d . . . O12 O 0.23139(12) 0.28038(6) 1.07373(11) 0.0702(6) Uani 1 1 d . . . O13 O 0.15743(12) 0.25152(7) 1.18720(10) 0.0711(6) Uani 1 1 d . . . S1 S 0.18560(5) 0.24193(2) 1.11190(4) 0.0527(2) 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 Gd1 0.03328(5) 0.02765(5) 0.03515(5) -0.00038(6) 0.01009(4) 0.00038(6) C1 0.0523(17) 0.113(3) 0.086(2) 0.0121(19) -0.0026(16) -0.0062(18) C2 0.0360(13) 0.0707(18) 0.0688(16) -0.0009(14) 0.0145(12) 0.0003(13) C3 0.0438(15) 0.077(2) 0.092(2) 0.0222(16) 0.0002(15) 0.0113(15) C4 0.0528(15) 0.0480(16) 0.1028(19) 0.0165(14) 0.0246(14) 0.0000(13) C5 0.0300(11) 0.0444(13) 0.0569(13) -0.0050(11) 0.0198(10) 0.0043(10) C6 0.0459(13) 0.0479(15) 0.0533(14) 0.0007(12) 0.0179(11) 0.0042(12) C7 0.0427(13) 0.0546(15) 0.0645(15) -0.0078(13) 0.0163(12) -0.0079(12) C8 0.0339(12) 0.0378(13) 0.0481(13) -0.0089(11) 0.0097(10) -0.0022(10) C9 0.0340(12) 0.0355(13) 0.0613(14) -0.0057(11) 0.0161(11) -0.0016(10) C10 0.0269(11) 0.0371(12) 0.0392(12) 0.0023(10) 0.0070(9) -0.0032(10) C11 0.0320(11) 0.0358(13) 0.0550(13) 0.0024(11) 0.0116(10) -0.0018(10) C12 0.0263(11) 0.0409(13) 0.0551(14) 0.0095(11) 0.0040(10) 0.0023(10) C13 0.0392(13) 0.0499(15) 0.0686(16) 0.0100(13) 0.0052(12) 0.0067(12) C14 0.0516(16) 0.0775(19) 0.0634(17) 0.0159(15) -0.0112(14) 0.0101(15) C15 0.0727(19) 0.088(2) 0.0529(16) -0.0019(15) -0.0110(15) 0.0241(17) C16 0.0778(19) 0.0722(19) 0.0513(16) -0.0071(14) -0.0009(14) 0.0194(16) C17 0.0388(12) 0.0412(13) 0.0412(13) 0.0021(11) 0.0036(11) -0.0009(11) C18 0.0481(13) 0.0367(12) 0.0399(13) -0.0001(10) 0.0043(11) 0.0156(11) C19 0.0313(11) 0.0389(13) 0.0399(12) 0.0083(10) 0.0111(10) 0.0006(10) C20 0.0336(11) 0.0344(13) 0.0368(12) 0.0004(9) 0.0092(9) 0.0031(9) C21 0.0431(13) 0.0532(14) 0.0396(13) -0.0126(11) 0.0037(11) 0.0057(12) C22 0.0379(12) 0.0436(13) 0.0392(12) -0.0097(11) 0.0062(10) 0.0017(11) C23 0.0553(15) 0.0485(15) 0.0509(14) -0.0170(12) 0.0048(12) 0.0066(13) C24 0.0511(15) 0.0526(15) 0.0419(13) -0.0054(12) -0.0027(12) -0.0038(13) C25 0.0666(18) 0.0765(19) 0.0614(17) -0.0182(15) -0.0065(15) -0.0137(16) C26 0.0670(19) 0.122(3) 0.0640(18) -0.0173(18) -0.0087(16) -0.0257(19) C27 0.0430(16) 0.137(3) 0.079(2) -0.011(2) -0.0070(15) -0.0138(19) C28 0.0457(15) 0.095(2) 0.0664(17) -0.0062(16) -0.0002(14) 0.0063(16) C29 0.0465(14) 0.0562(16) 0.0428(13) 0.0007(12) 0.0010(12) -0.0047(12) C30 0.0481(13) 0.0362(13) 0.0458(13) 0.0002(11) 0.0136(11) 0.0059(11) C31 0.0391(12) 0.0347(12) 0.0320(11) -0.0021(10) 0.0087(10) -0.0025(10) C32 0.0384(11) 0.0244(10) 0.0331(10) -0.0034(10) 0.0069(9) 0.0083(10) C33 0.0332(12) 0.0475(14) 0.0653(14) -0.0249(12) 0.0130(11) -0.0028(11) C34 0.0298(11) 0.0400(13) 0.0670(14) -0.0115(12) 0.0161(11) -0.0099(10) C35 0.0407(13) 0.0457(14) 0.0849(16) -0.0237(13) 0.0247(12) -0.0044(11) C36 0.0383(12) 0.0498(14) 0.0653(14) -0.0203(12) 0.0221(11) -0.0133(11) C37 0.0479(14) 0.0639(17) 0.0872(17) -0.0333(14) 0.0306(13) -0.0115(13) C38 0.0550(15) 0.0756(18) 0.0825(17) -0.0417(14) 0.0256(13) -0.0159(14) C39 0.0399(14) 0.0854(19) 0.0842(18) -0.0359(15) 0.0145(13) -0.0190(14) C40 0.0402(13) 0.0676(17) 0.0899(18) -0.0324(14) 0.0221(13) -0.0108(13) C41 0.0403(12) 0.0458(14) 0.0590(14) -0.0142(11) 0.0211(11) -0.0089(11) C42 0.0370(11) 0.0457(14) 0.0541(13) -0.0137(11) 0.0255(10) -0.0078(11) C43 0.0322(11) 0.0434(13) 0.0489(12) -0.0140(10) 0.0198(10) -0.0114(10) C44 0.0458(12) 0.0337(12) 0.0438(12) -0.0007(10) 0.0234(10) -0.0091(10) C45 0.197(4) 0.166(3) 0.0566(19) 0.049(2) 0.009(2) 0.057(3) C46 0.155(3) 0.127(3) 0.076(2) 0.010(2) 0.037(2) -0.055(2) C47 0.0859(19) 0.0697(19) 0.0608(16) 0.0111(14) 0.0272(14) 0.0105(16) C48A 0.083(2) 0.091(3) 0.139(3) 0.010(2) 0.054(2) -0.010(2) C48B 0.097(3) 0.097(3) 0.121(3) 0.016(3) 0.040(3) 0.002(3) C49A 0.089(3) 0.092(3) 0.137(3) -0.006(3) 0.019(2) 0.014(2) C49B 0.112(3) 0.104(3) 0.134(3) -0.003(3) 0.037(3) 0.009(3) N3A 0.0568(17) 0.0557(19) 0.111(2) 0.0089(17) 0.0385(16) 0.0033(16) N3B 0.079(2) 0.073(3) 0.112(3) -0.002(2) 0.051(2) 0.005(2) C50 0.0862(17) 0.069(2) 0.127(2) -0.0013(17) 0.0651(15) -0.0187(16) N1 0.0360(10) 0.0407(11) 0.0499(11) -0.0068(9) 0.0138(8) 0.0011(9) N2 0.1178(18) 0.0716(16) 0.0429(12) 0.0172(11) 0.0236(12) 0.0070(15) O1 0.0698(10) 0.0475(10) 0.0452(9) 0.0125(8) 0.0192(8) 0.0023(9) O2 0.0447(8) 0.0497(11) 0.0754(10) 0.0013(8) 0.0230(8) 0.0092(8) O3 0.0403(8) 0.0389(9) 0.0690(10) -0.0186(8) 0.0150(8) -0.0001(7) O4 0.0489(9) 0.0428(9) 0.0590(10) -0.0090(8) 0.0013(8) 0.0017(8) O5 0.0424(8) 0.0317(8) 0.0382(7) -0.0058(6) 0.0125(6) 0.0027(7) O6 0.0509(9) 0.0413(9) 0.0498(9) -0.0041(7) 0.0211(7) -0.0136(7) O7 0.0332(8) 0.0370(8) 0.0521(9) 0.0086(7) 0.0064(7) -0.0008(7) O8 0.0396(8) 0.0415(9) 0.0454(8) 0.0124(7) 0.0135(7) 0.0095(7) O9 0.0427(9) 0.0653(10) 0.0431(9) -0.0155(8) 0.0036(7) 0.0140(8) O10 0.0341(8) 0.0725(11) 0.0839(11) -0.0393(9) 0.0210(8) -0.0066(8) O11 0.0389(8) 0.0424(9) 0.0384(8) -0.0041(7) 0.0056(7) -0.0055(7) O12 0.0521(9) 0.0379(10) 0.1268(14) -0.0096(10) 0.0341(9) -0.0063(8) O13 0.0484(9) 0.0935(13) 0.0745(10) -0.0449(9) 0.0213(8) 0.0020(9) S1 0.0374(3) 0.0435(4) 0.0791(4) -0.0200(3) 0.0183(3) -0.0009(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 Gd1 O5 2.3670(14) . ? Gd1 O1 2.3977(15) . ? Gd1 O8 2.4052(13) 3_657 ? Gd1 O7 2.4197(13) . ? Gd1 O4 2.4341(15) . ? Gd1 O2 2.4402(16) . ? Gd1 O3 2.4456(14) . ? Gd1 O6 2.4907(14) 3_657 ? Gd1 O5 2.6506(13) 3_657 ? Gd1 C44 2.796(2) . ? Gd1 C32 2.9422(19) 3_657 ? C1 C2 1.489(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.365(4) . ? C2 C7 1.375(3) . ? C3 C4 1.393(3) . ? C3 H3 0.9300 . ? C4 C5 1.371(3) . ? C4 H4 0.9300 . ? C5 C6 1.375(3) . ? C5 S1 1.759(2) . ? C6 C7 1.382(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.461(3) . ? C8 C9 1.522(3) . ? C8 C21 1.527(3) . ? C8 C33 1.536(3) . ? C9 O11 1.429(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.359(3) . ? C10 O11 1.395(2) . ? C10 C19 1.412(3) . ? C11 C12 1.412(3) . ? C11 H11 0.9300 . ? C12 C13 1.412(3) . ? C12 C17 1.413(3) . ? C13 C14 1.379(3) . ? C13 H13 0.9300 . ? C14 C15 1.376(4) . ? C14 H14 0.9300 . ? C15 C16 1.355(3) . ? C15 H15 0.9300 . ? C16 C17 1.407(3) . ? C16 H16 0.9300 . ? C17 C18 1.406(3) . ? C18 C19 1.366(3) . ? C18 H18 0.9300 . ? C19 C20 1.505(3) . ? C20 O7 1.258(3) . ? C20 O8 1.258(2) . ? C21 O9 1.430(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.350(3) . ? C22 O9 1.379(2) . ? C22 C31 1.404(3) . ? C23 C24 1.390(3) . ? C23 H23 0.9300 . ? C24 C29 1.414(3) . ? C24 C25 1.417(3) . ? C25 C26 1.348(4) . ? C25 H25 0.9300 . ? C26 C27 1.387(4) . ? C26 H26 0.9300 . ? C27 C28 1.367(4) . ? C27 H27 0.9300 . ? C28 C29 1.405(3) . ? C28 H28 0.9300 . ? C29 C30 1.404(3) . ? C30 C31 1.371(3) . ? C30 H30 0.9300 . ? C31 C32 1.489(3) . ? C32 O6 1.255(3) . ? C32 O5 1.278(2) . ? C32 Gd1 2.9422(19) 3_657 ? C33 O10 1.432(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.363(3) . ? C34 O10 1.367(2) . ? C34 C43 1.428(3) . ? C35 C36 1.405(3) . ? C35 H35 0.9300 . ? C36 C37 1.410(3) . ? C36 C41 1.412(3) . ? C37 C38 1.343(3) . ? C37 H37 0.9300 . ? C38 C39 1.386(4) . ? C38 H38 0.9300 . ? C39 C40 1.359(3) . ? C39 H39 0.9300 . ? C40 C41 1.407(3) . ? C40 H40 0.9300 . ? C41 C42 1.415(3) . ? C42 C43 1.353(3) . ? C42 H42 0.9300 . ? C43 C44 1.509(3) . ? C44 O3 1.256(2) . ? C44 O4 1.262(2) . ? C45 N2 1.443(4) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 N2 1.437(4) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 O1 1.216(3) . ? C47 N2 1.300(3) . ? C47 H47 0.9300 . ? C48A N3A 1.458(6) . ? C48A H48A 0.9617 . ? C48A H48B 0.9370 . ? C48A H48C 0.9695 . ? C48B N3B 1.425(8) . ? C48B H48D 0.9890 . ? C48B H48E 0.9571 . ? C48B H48F 0.8472 . ? C49A N3A 1.484(6) . ? C49A H49A 0.8924 . ? C49A H49B 0.8672 . ? C49A H49C 1.0476 . ? C49B N3B 1.470(8) . ? C49B H49D 0.9060 . ? C49B H49E 0.9766 . ? C49B H49F 0.8838 . ? N3A C50 1.354(4) . ? N3B C50 1.451(7) . ? C50 O2 1.206(3) . ? C50 H50A 0.8220 . ? C50 H50B 1.0006 . ? N1 S1 1.5926(17) . ? N1 H1 0.8600 . ? O5 Gd1 2.6506(13) 3_657 ? O6 Gd1 2.4907(14) 3_657 ? O8 Gd1 2.4052(13) 3_657 ? O12 S1 1.4322(18) . ? O13 S1 1.4208(18) . ? 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 -0.008 0.000 0.500 739 236 ' ' 2 -0.003 0.500 1.000 739 236 ' ' _platon_squeeze_details ; ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Gd1 O1 148.63(5) . . ? O5 Gd1 O8 72.28(5) . 3_657 ? O1 Gd1 O8 139.03(5) . 3_657 ? O5 Gd1 O7 78.40(5) . . ? O1 Gd1 O7 75.48(5) . . ? O8 Gd1 O7 133.12(5) 3_657 . ? O5 Gd1 O4 77.90(5) . . ? O1 Gd1 O4 77.23(5) . . ? O8 Gd1 O4 134.20(5) 3_657 . ? O7 Gd1 O4 70.48(5) . . ? O5 Gd1 O2 137.47(5) . . ? O1 Gd1 O2 70.47(5) . . ? O8 Gd1 O2 72.75(5) 3_657 . ? O7 Gd1 O2 144.11(5) . . ? O4 Gd1 O2 111.56(5) . . ? O5 Gd1 O3 82.11(5) . . ? O1 Gd1 O3 97.87(5) . . ? O8 Gd1 O3 88.34(5) 3_657 . ? O7 Gd1 O3 123.12(5) . . ? O4 Gd1 O3 53.28(5) . . ? O2 Gd1 O3 73.45(5) . . ? O5 Gd1 O6 121.42(5) . 3_657 ? O1 Gd1 O6 72.62(5) . 3_657 ? O8 Gd1 O6 81.46(5) 3_657 3_657 ? O7 Gd1 O6 83.72(5) . 3_657 ? O4 Gd1 O6 144.33(5) . 3_657 ? O2 Gd1 O6 75.72(5) . 3_657 ? O3 Gd1 O6 149.15(5) . 3_657 ? O5 Gd1 O5 71.29(5) . 3_657 ? O1 Gd1 O5 112.23(4) . 3_657 ? O8 Gd1 O5 70.47(4) 3_657 3_657 ? O7 Gd1 O5 65.82(4) . 3_657 ? O4 Gd1 O5 130.28(5) . 3_657 ? O2 Gd1 O5 117.62(5) . 3_657 ? O3 Gd1 O5 149.83(5) . 3_657 ? O6 Gd1 O5 50.57(5) 3_657 3_657 ? O5 Gd1 C44 76.52(5) . . ? O1 Gd1 C44 89.44(6) . . ? O8 Gd1 C44 110.75(5) 3_657 . ? O7 Gd1 C44 96.54(5) . . ? O4 Gd1 C44 26.81(5) . . ? O2 Gd1 C44 94.16(6) . . ? O3 Gd1 C44 26.66(5) . . ? O6 Gd1 C44 161.45(6) 3_657 . ? O5 Gd1 C44 145.67(5) 3_657 . ? O5 Gd1 C32 97.01(5) . 3_657 ? O1 Gd1 C32 90.92(5) . 3_657 ? O8 Gd1 C32 76.69(5) 3_657 3_657 ? O7 Gd1 C32 71.47(5) . 3_657 ? O4 Gd1 C32 141.87(5) . 3_657 ? O2 Gd1 C32 97.74(5) . 3_657 ? O3 Gd1 C32 164.46(5) . 3_657 ? O6 Gd1 C32 24.99(5) 3_657 3_657 ? O5 Gd1 C32 25.75(5) 3_657 3_657 ? C44 Gd1 C32 167.49(6) . 3_657 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.2(2) . . ? C3 C2 C1 122.2(2) . . ? C7 C2 C1 120.5(2) . . ? C2 C3 C4 122.5(2) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.00(19) . . ? C4 C5 S1 121.10(18) . . ? C6 C5 S1 119.72(16) . . ? C5 C6 C7 120.7(2) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 121.3(2) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N1 C8 C9 113.84(16) . . ? N1 C8 C21 107.79(18) . . ? C9 C8 C21 106.21(17) . . ? N1 C8 C33 108.39(17) . . ? C9 C8 C33 110.59(18) . . ? C21 C8 C33 109.95(17) . . ? O11 C9 C8 108.94(17) . . ? O11 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O11 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 O11 119.61(19) . . ? C11 C10 C19 121.39(18) . . ? O11 C10 C19 118.98(16) . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 122.3(2) . . ? C13 C12 C17 118.86(19) . . ? C11 C12 C17 118.82(18) . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 121.1(2) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 122.5(2) . . ? C18 C17 C12 118.38(18) . . ? C16 C17 C12 119.2(2) . . ? C19 C18 C17 122.6(2) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C18 C19 C10 118.04(18) . . ? C18 C19 C20 119.68(19) . . ? C10 C19 C20 122.21(17) . . ? O7 C20 O8 126.57(18) . . ? O7 C20 C19 116.79(18) . . ? O8 C20 C19 116.53(18) . . ? O9 C21 C8 110.98(17) . . ? O9 C21 H21A 109.4 . . ? C8 C21 H21A 109.4 . . ? O9 C21 H21B 109.4 . . ? C8 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C23 C22 O9 117.8(2) . . ? C23 C22 C31 120.6(2) . . ? O9 C22 C31 121.55(17) . . ? C22 C23 C24 122.4(2) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C23 C24 C29 118.2(2) . . ? C23 C24 C25 124.0(2) . . ? C29 C24 C25 117.8(2) . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 121.0(3) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.7(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 122.3(2) . . ? C30 C29 C24 118.4(2) . . ? C28 C29 C24 119.3(2) . . ? C31 C30 C29 122.3(2) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 C22 118.06(18) . . ? C30 C31 C32 118.08(19) . . ? C22 C31 C32 123.53(18) . . ? O6 C32 O5 120.60(17) . . ? O6 C32 C31 120.30(18) . . ? O5 C32 C31 119.09(18) . . ? O6 C32 Gd1 56.95(10) . 3_657 ? O5 C32 Gd1 64.28(10) . 3_657 ? C31 C32 Gd1 170.69(13) . 3_657 ? O10 C33 C8 107.48(17) . . ? O10 C33 H33A 110.2 . . ? C8 C33 H33A 110.2 . . ? O10 C33 H33B 110.2 . . ? C8 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C35 C34 O10 123.5(2) . . ? C35 C34 C43 120.12(19) . . ? O10 C34 C43 116.35(18) . . ? C34 C35 C36 121.7(2) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C37 123.6(2) . . ? C35 C36 C41 119.2(2) . . ? C37 C36 C41 117.21(19) . . ? C38 C37 C36 121.8(2) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C39 120.7(2) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 120.3(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.2(2) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C36 119.8(2) . . ? C40 C41 C42 122.9(2) . . ? C36 C41 C42 117.25(19) . . ? C43 C42 C41 123.8(2) . . ? C43 C42 H42 118.1 . . ? C41 C42 H42 118.1 . . ? C42 C43 C34 117.91(19) . . ? C42 C43 C44 118.36(19) . . ? C34 C43 C44 123.72(17) . . ? O3 C44 O4 120.68(19) . . ? O3 C44 C43 118.83(17) . . ? O4 C44 C43 120.49(19) . . ? O3 C44 Gd1 60.92(10) . . ? O4 C44 Gd1 60.41(11) . . ? C43 C44 Gd1 170.84(15) . . ? N2 C45 H45A 109.5 . . ? N2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N2 C46 H46A 109.5 . . ? N2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O1 C47 N2 125.8(3) . . ? O1 C47 H47 117.1 . . ? N2 C47 H47 117.1 . . ? N3A C48A H48A 106.3 . . ? N3A C48A H48B 108.5 . . ? H48A C48A H48B 112.5 . . ? N3A C48A H48C 109.1 . . ? H48A C48A H48C 108.8 . . ? H48B C48A H48C 111.5 . . ? N3A C48A H48D 103.0 . . ? H48B C48A H48D 76.9 . . ? H48C C48A H48D 141.3 . . ? N3A C48A H48E 127.4 . . ? H48A C48A H48E 108.7 . . ? H48C C48A H48E 95.1 . . ? H48D C48A H48E 81.6 . . ? N3B C48B H48A 89.2 . . ? N3B C48B H48B 98.6 . . ? H48A C48B H48B 88.9 . . ? N3B C48B H48D 102.0 . . ? H48B C48B H48D 127.3 . . ? N3B C48B H48E 102.9 . . ? H48A C48B H48E 69.5 . . ? H48D C48B H48E 107.3 . . ? N3B C48B H48F 111.4 . . ? H48A C48B H48F 157.4 . . ? H48B C48B H48F 96.7 . . ? H48D C48B H48F 119.1 . . ? H48E C48B H48F 112.5 . . ? N3A C49A H49A 99.3 . . ? N3A C49A H49B 113.5 . . ? H49A C49A H49B 124.7 . . ? N3A C49A H49C 103.5 . . ? H49A C49A H49C 104.8 . . ? H49B C49A H49C 108.8 . . ? N3A C49A H49E 83.2 . . ? H49A C49A H49E 115.1 . . ? H49C C49A H49E 138.1 . . ? N3B C49B H49B 119.3 . . ? N3B C49B H49D 109.1 . . ? H49B C49B H49D 122.7 . . ? N3B C49B H49E 92.0 . . ? H49D C49B H49E 115.7 . . ? N3B C49B H49F 105.7 . . ? H49B C49B H49F 70.5 . . ? H49D C49B H49F 124.4 . . ? H49E C49B H49F 104.9 . . ? C50 N3A C48A 117.3(3) . . ? C50 N3A C49A 123.4(4) . . ? C48A N3A C49A 118.4(4) . . ? C50 N3A H49E 123.8 . . ? C48A N3A H49E 114.4 . . ? C48B N3B C50 126.5(5) . . ? C48B N3B C49B 117.0(6) . . ? C50 N3B C49B 115.9(5) . . ? O2 C50 N3A 126.0(3) . . ? O2 C50 N3B 115.7(3) . . ? O2 C50 H50A 106.0 . . ? N3A C50 H50A 126.4 . . ? N3B C50 H50A 128.5 . . ? O2 C50 H50B 115.4 . . ? N3A C50 H50B 103.4 . . ? N3B C50 H50B 128.7 . . ? C8 N1 S1 127.89(15) . . ? C8 N1 H1 116.1 . . ? S1 N1 H1 116.1 . . ? C47 N2 C46 120.0(2) . . ? C47 N2 C45 123.1(3) . . ? C46 N2 C45 116.8(2) . . ? C47 O1 Gd1 135.42(18) . . ? C50 O2 Gd1 131.24(18) . . ? C44 O3 Gd1 92.43(11) . . ? C44 O4 Gd1 92.79(13) . . ? C32 O5 Gd1 161.12(13) . . ? C32 O5 Gd1 89.97(11) . 3_657 ? Gd1 O5 Gd1 108.71(5) . 3_657 ? C32 O6 Gd1 98.06(12) . 3_657 ? C20 O7 Gd1 136.95(12) . . ? C20 O8 Gd1 138.19(13) . 3_657 ? C22 O9 C21 117.39(17) . . ? C34 O10 C33 119.49(17) . . ? C10 O11 C9 114.77(16) . . ? O13 S1 O12 119.84(11) . . ? O13 S1 N1 105.81(10) . . ? O12 S1 N1 109.12(10) . . ? O13 S1 C5 107.10(10) . . ? O12 S1 C5 105.88(10) . . ? N1 S1 C5 108.73(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.625 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.079 #==END data_6 _database_code_depnum_ccdc_archive 'CCDC 795983' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H92 Dy2 N6 O26 S2' _chemical_formula_weight 2182.92 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2837(5) _cell_length_b 26.9105(10) _cell_length_c 16.6066(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.917(2) _cell_angle_gamma 90.00 _cell_volume 5736.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2427 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 18.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31318 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1394 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10656 _reflns_number_gt 5702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0403P)^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_number_reflns 10656 _refine_ls_number_parameters 644 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2207(6) 0.1837(3) -0.1280(5) 0.082(3) Uani 1 1 d . . . H1A H -0.2229 0.1483 -0.1353 0.123 Uiso 1 1 calc R . . H1B H -0.2287 0.1996 -0.1810 0.123 Uiso 1 1 calc R . . H1C H -0.2762 0.1938 -0.1043 0.123 Uiso 1 1 calc R . . C2 C -0.1177(5) 0.1983(3) -0.0704(5) 0.0514(19) Uani 1 1 d . . . C3 C -0.0670(6) 0.2418(3) -0.0818(5) 0.071(2) Uani 1 1 d . . . H3 H -0.0963 0.2624 -0.1266 0.086 Uiso 1 1 calc R . . C4 C 0.0268(5) 0.2548(3) -0.0270(5) 0.058(2) Uani 1 1 d . . . H4 H 0.0598 0.2843 -0.0344 0.070 Uiso 1 1 calc R . . C5 C 0.0708(4) 0.2237(2) 0.0386(4) 0.0384(16) Uani 1 1 d . . . C6 C 0.0218(5) 0.1809(2) 0.0488(4) 0.0442(17) Uani 1 1 d . . . H6 H 0.0514 0.1600 0.0933 0.053 Uiso 1 1 calc R . . C7 C -0.0710(5) 0.1679(3) -0.0059(4) 0.0492(18) Uani 1 1 d . . . H7 H -0.1025 0.1379 0.0013 0.059 Uiso 1 1 calc R . . C8 C 0.3388(5) 0.1806(2) 0.0868(4) 0.0386(16) Uani 1 1 d . . . C9 C 0.2927(5) 0.1743(2) -0.0071(4) 0.0389(16) Uani 1 1 d . . . H9A H 0.2560 0.2042 -0.0306 0.047 Uiso 1 1 calc R . . H9B H 0.3478 0.1681 -0.0345 0.047 Uiso 1 1 calc R . . C10 C 0.1840(5) 0.1190(2) -0.1031(4) 0.0345(15) Uani 1 1 d . . . C11 C 0.0948(5) 0.1398(2) -0.1506(4) 0.0426(17) Uani 1 1 d . . . H11 H 0.0614 0.1641 -0.1272 0.051 Uiso 1 1 calc R . . C12 C 0.0518(5) 0.1256(2) -0.2335(4) 0.0349(15) Uani 1 1 d . . . C13 C -0.0400(5) 0.1459(3) -0.2841(4) 0.0515(19) Uani 1 1 d . . . H13 H -0.0759 0.1700 -0.2624 0.062 Uiso 1 1 calc R . . C14 C -0.0774(6) 0.1309(3) -0.3645(5) 0.067(2) Uani 1 1 d . . . H14 H -0.1377 0.1452 -0.3975 0.080 Uiso 1 1 calc R . . C15 C -0.0269(6) 0.0949(3) -0.3974(5) 0.074(3) Uani 1 1 d . . . H15 H -0.0551 0.0838 -0.4515 0.089 Uiso 1 1 calc R . . C16 C 0.0648(6) 0.0750(3) -0.3512(4) 0.060(2) Uani 1 1 d . . . H16 H 0.1005 0.0519 -0.3751 0.072 Uiso 1 1 calc R . . C17 C 0.1047(5) 0.0894(2) -0.2681(4) 0.0388(16) Uani 1 1 d . . . C18 C 0.1979(5) 0.0688(2) -0.2178(4) 0.0414(16) Uani 1 1 d . . . H18 H 0.2335 0.0454 -0.2410 0.050 Uiso 1 1 calc R . . C19 C 0.2374(4) 0.0821(2) -0.1365(4) 0.0335(15) Uani 1 1 d . . . C20 C 0.3334(5) 0.0559(2) -0.0848(4) 0.0325(15) Uani 1 1 d . . . C21 C 0.3812(5) 0.1291(2) 0.1205(3) 0.0420(17) Uani 1 1 d . . . H21A H 0.3243 0.1054 0.1112 0.050 Uiso 1 1 calc R . . H21B H 0.4308 0.1175 0.0908 0.050 Uiso 1 1 calc R . . C22 C 0.5354(5) 0.1209(2) 0.2317(4) 0.0413(17) Uani 1 1 d . . . C23 C 0.5969(5) 0.1500(2) 0.2910(4) 0.0488(19) Uani 1 1 d . . . H23 H 0.5673 0.1760 0.3139 0.059 Uiso 1 1 calc R . . C24 C 0.7052(5) 0.1414(2) 0.3185(4) 0.0459(18) Uani 1 1 d . . . C25 C 0.7705(6) 0.1710(3) 0.3823(4) 0.066(2) Uani 1 1 d . . . H25 H 0.7420 0.1960 0.4082 0.079 Uiso 1 1 calc R . . C26 C 0.8743(7) 0.1623(4) 0.4048(5) 0.085(3) Uani 1 1 d . . . H26 H 0.9172 0.1827 0.4444 0.102 Uiso 1 1 calc R . . C27 C 0.9188(6) 0.1234(4) 0.3699(5) 0.082(3) Uani 1 1 d . . . H27 H 0.9902 0.1178 0.3871 0.098 Uiso 1 1 calc R . . C28 C 0.8580(6) 0.0937(3) 0.3113(5) 0.072(2) Uani 1 1 d . . . H28 H 0.8880 0.0678 0.2886 0.086 Uiso 1 1 calc R . . C29 C 0.7506(5) 0.1018(2) 0.2845(4) 0.0448(17) Uani 1 1 d . . . C30 C 0.6832(5) 0.0727(2) 0.2220(4) 0.0404(16) Uani 1 1 d . . . H30 H 0.7116 0.0472 0.1970 0.048 Uiso 1 1 calc R . . C31 C 0.5777(5) 0.0807(2) 0.1971(3) 0.0321(15) Uani 1 1 d . . . C32 C 0.5137(4) 0.0438(2) 0.1384(3) 0.0298(13) Uani 1 1 d . . . C33 C 0.4283(4) 0.2185(2) 0.1039(4) 0.0453(18) Uani 1 1 d . . . H33A H 0.4038 0.2501 0.0784 0.054 Uiso 1 1 calc R . . H33B H 0.4551 0.2235 0.1635 0.054 Uiso 1 1 calc R . . C34 C 0.6099(5) 0.2093(2) 0.1073(4) 0.0410(16) Uani 1 1 d . . . C35 C 0.6398(5) 0.2481(2) 0.1603(4) 0.0484(19) Uani 1 1 d . . . H35 H 0.5900 0.2704 0.1689 0.058 Uiso 1 1 calc R . . C36 C 0.7459(5) 0.2552(2) 0.2028(4) 0.0459(18) Uani 1 1 d . . . C37 C 0.7809(5) 0.2946(3) 0.2610(4) 0.057(2) Uani 1 1 d . . . H37 H 0.7330 0.3173 0.2715 0.068 Uiso 1 1 calc R . . C38 C 0.8820(5) 0.2994(3) 0.3006(4) 0.064(2) Uani 1 1 d . . . H38 H 0.9027 0.3251 0.3386 0.077 Uiso 1 1 calc R . . C39 C 0.9577(6) 0.2662(3) 0.2861(5) 0.067(2) Uani 1 1 d . . . H39 H 1.0278 0.2706 0.3129 0.080 Uiso 1 1 calc R . . C40 C 0.9265(5) 0.2278(3) 0.2324(4) 0.060(2) Uani 1 1 d . . . H40 H 0.9758 0.2054 0.2236 0.072 Uiso 1 1 calc R . . C41 C 0.8198(5) 0.2211(2) 0.1893(4) 0.0417(17) Uani 1 1 d . . . C42 C 0.7847(5) 0.1817(2) 0.1338(4) 0.0424(17) Uani 1 1 d . . . H42 H 0.8338 0.1592 0.1246 0.051 Uiso 1 1 calc R . . C43 C 0.6839(5) 0.1745(2) 0.0930(4) 0.0326(15) Uani 1 1 d . . . C44 C 0.6567(5) 0.1304(2) 0.0374(4) 0.0363(16) Uani 1 1 d . . . C45 C 0.5483(8) -0.1395(4) 0.3661(5) 0.122(4) Uani 1 1 d . . . H45A H 0.5431 -0.1750 0.3630 0.183 Uiso 1 1 calc R . . H45B H 0.5440 -0.1286 0.4202 0.183 Uiso 1 1 calc R . . H45C H 0.6136 -0.1292 0.3569 0.183 Uiso 1 1 calc R . . C46 C 0.3611(8) -0.1179(3) 0.3152(5) 0.106(4) Uani 1 1 d . . . H46A H 0.3194 -0.0932 0.2800 0.159 Uiso 1 1 calc R . . H46B H 0.3646 -0.1104 0.3724 0.159 Uiso 1 1 calc R . . H46C H 0.3302 -0.1500 0.3014 0.159 Uiso 1 1 calc R . . C47 C 0.4769(7) -0.0992(3) 0.2337(5) 0.062(2) Uani 1 1 d . . . H47 H 0.5448 -0.0976 0.2283 0.074 Uiso 1 1 calc R . . C48A C 0.0919(15) -0.0327(6) 0.1775(12) 0.090(4) Uani 0.489(11) 1 d PDU A 1 H48A H 0.0263 -0.0366 0.1467 0.108 Uiso 0.489(11) 1 d PR A 1 H48B H 0.1453 -0.0566 0.1797 0.108 Uiso 0.489(11) 1 d PR A 1 H48C H 0.0883 -0.0166 0.2327 0.108 Uiso 0.489(11) 1 d PR A 1 C48B C 0.0451(12) -0.0404(6) 0.1150(13) 0.088(4) Uani 0.511(11) 1 d PDU A 2 H48D H 0.0283 -0.0299 0.1652 0.105 Uiso 0.511(11) 1 d PR A 2 H48E H -0.0127 -0.0499 0.0772 0.105 Uiso 0.511(11) 1 d PR A 2 H48F H 0.1003 -0.0599 0.1262 0.105 Uiso 0.511(11) 1 d PR A 2 C49A C 0.0538(14) 0.0527(6) 0.1265(14) 0.097(5) Uani 0.489(11) 1 d PDU A 1 H49A H 0.0801 0.0774 0.0970 0.117 Uiso 0.489(11) 1 d PR A 1 H49B H -0.0089 0.0424 0.0930 0.117 Uiso 0.489(11) 1 d PR A 1 H49C H 0.0481 0.0644 0.1790 0.117 Uiso 0.489(11) 1 d PR A 1 C49B C 0.0185(11) 0.0483(6) 0.0593(13) 0.094(4) Uani 0.511(11) 1 d PDU A 2 H49D H 0.0564 0.0716 0.0353 0.113 Uiso 0.511(11) 1 d PR A 2 H49E H 0.0024 0.0626 0.1063 0.113 Uiso 0.511(11) 1 d PR A 2 H49F H -0.0376 0.0386 0.0183 0.113 Uiso 0.511(11) 1 d PR A 2 N3A N 0.1134(12) 0.0077(5) 0.1302(11) 0.075(4) Uani 0.489(11) 1 d PDU A 1 N3B N 0.0801(10) 0.0040(5) 0.0800(11) 0.070(3) Uani 0.511(11) 1 d PDU A 2 C50 C 0.1820(6) 0.0046(3) 0.0798(5) 0.077(3) Uani 1 1 d D . . H50A H 0.1856 0.0305 0.0405 0.092 Uiso 0.50 1 d PR A . H50B H 0.2106 0.0355 0.0725 0.092 Uiso 0.50 1 d PR . . Dy1 Dy 0.40354(2) -0.041979(10) 0.049035(18) 0.03036(9) Uani 1 1 d . . . N1 N 0.2632(3) 0.19543(17) 0.1320(3) 0.0385(13) Uani 1 1 d . . . H1 H 0.2598 0.1771 0.1737 0.046 Uiso 1 1 calc R . . N2 N 0.4639(6) -0.1178(2) 0.3031(4) 0.0677(19) Uani 1 1 d . . . O1 O 0.4084(3) -0.08379(16) 0.1758(3) 0.0496(12) Uani 1 1 d . A . O2 O 0.2384(3) -0.03043(16) 0.0846(3) 0.0511(13) Uani 1 1 d . A . O3 O 0.7219(3) 0.09531(16) 0.0426(3) 0.0462(12) Uani 1 1 d . . . O4 O 0.5699(3) 0.12769(15) -0.0156(3) 0.0508(12) Uani 1 1 d . . . O5 O 0.5326(3) 0.03479(13) 0.0688(2) 0.0336(10) Uani 1 1 d . . . O6 O 0.4425(3) 0.02075(15) 0.1603(3) 0.0443(11) Uani 1 1 d . A . O7 O 0.4173(3) 0.06340(14) -0.1044(2) 0.0372(10) Uani 1 1 d . . . O8 O 0.3194(3) 0.02728(14) -0.0289(2) 0.0386(11) Uani 1 1 d . A . O9 O 0.4306(3) 0.13189(17) 0.2072(2) 0.0512(12) Uani 1 1 d . . . O10 O 0.5082(3) 0.19920(17) 0.0694(3) 0.0569(14) Uani 1 1 d . . . O11 O 0.2222(3) 0.13297(14) -0.0194(2) 0.0375(10) Uani 1 1 d . . . O12 O 0.2324(3) 0.28081(16) 0.0751(3) 0.0672(15) Uani 1 1 d . . . O13 O 0.1574(3) 0.25179(18) 0.1884(3) 0.0667(15) Uani 1 1 d . . . S1 S 0.18571(13) 0.24217(7) 0.11301(12) 0.0491(5) 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 C1 0.054(5) 0.099(7) 0.078(6) 0.011(5) -0.009(5) -0.008(5) C2 0.036(4) 0.058(5) 0.060(5) -0.006(4) 0.011(4) 0.002(4) C3 0.047(5) 0.071(6) 0.085(6) 0.031(5) -0.002(4) 0.017(5) C4 0.032(4) 0.051(5) 0.089(6) 0.015(4) 0.013(4) 0.003(4) C5 0.027(4) 0.037(4) 0.053(4) -0.004(3) 0.014(3) 0.005(3) C6 0.037(4) 0.037(4) 0.056(5) 0.001(3) 0.007(4) -0.003(3) C7 0.050(5) 0.053(5) 0.045(4) -0.002(4) 0.011(4) -0.010(4) C8 0.030(4) 0.034(4) 0.052(4) -0.013(3) 0.010(3) -0.003(3) C9 0.038(4) 0.031(4) 0.050(4) -0.008(3) 0.016(3) -0.004(3) C10 0.035(4) 0.029(4) 0.041(4) 0.000(3) 0.012(3) -0.005(3) C11 0.025(4) 0.045(4) 0.057(5) 0.000(4) 0.007(3) 0.002(3) C12 0.031(4) 0.031(4) 0.040(4) 0.005(3) 0.005(3) -0.001(3) C13 0.045(4) 0.056(5) 0.051(5) 0.009(4) 0.007(4) 0.013(4) C14 0.045(5) 0.089(6) 0.056(5) 0.015(5) -0.008(4) 0.009(5) C15 0.063(6) 0.093(7) 0.047(5) -0.011(5) -0.020(4) 0.017(5) C16 0.064(5) 0.072(5) 0.038(4) -0.012(4) 0.002(4) 0.019(4) C17 0.034(4) 0.045(4) 0.034(4) 0.001(3) 0.002(3) 0.000(3) C18 0.048(4) 0.036(4) 0.038(4) -0.003(3) 0.007(3) 0.009(3) C19 0.033(4) 0.031(4) 0.035(4) 0.003(3) 0.007(3) 0.003(3) C20 0.034(4) 0.030(4) 0.030(4) -0.004(3) 0.001(3) 0.009(3) C21 0.040(4) 0.043(4) 0.035(4) -0.012(3) -0.004(3) 0.012(3) C22 0.039(4) 0.046(4) 0.034(4) -0.012(3) 0.000(3) 0.002(3) C23 0.045(4) 0.046(4) 0.050(4) -0.024(4) 0.003(4) 0.005(4) C24 0.049(5) 0.043(4) 0.040(4) -0.010(3) 0.002(3) -0.008(4) C25 0.055(5) 0.071(6) 0.061(5) -0.021(4) -0.004(4) -0.011(4) C26 0.071(7) 0.102(8) 0.068(6) -0.030(6) -0.007(5) -0.028(6) C27 0.040(5) 0.125(8) 0.065(6) -0.011(6) -0.017(4) -0.011(5) C28 0.040(5) 0.102(7) 0.066(6) -0.003(5) 0.001(4) 0.000(5) C29 0.038(4) 0.053(5) 0.038(4) -0.010(3) -0.001(3) -0.003(4) C30 0.038(4) 0.040(4) 0.042(4) -0.004(3) 0.008(3) 0.008(3) C31 0.037(4) 0.036(4) 0.021(3) -0.001(3) 0.004(3) -0.002(3) C32 0.029(3) 0.022(3) 0.035(4) 0.007(3) 0.001(3) 0.011(3) C33 0.024(4) 0.051(4) 0.060(5) -0.020(4) 0.010(3) -0.005(3) C34 0.032(4) 0.041(4) 0.056(5) -0.010(3) 0.023(3) 0.000(3) C35 0.025(4) 0.048(4) 0.073(5) -0.027(4) 0.015(4) -0.010(3) C36 0.038(4) 0.039(4) 0.065(5) -0.017(4) 0.022(4) -0.008(3) C37 0.036(5) 0.053(5) 0.083(6) -0.029(4) 0.020(4) -0.008(4) C38 0.040(5) 0.079(6) 0.074(6) -0.045(5) 0.015(4) -0.027(4) C39 0.037(5) 0.087(6) 0.073(6) -0.037(5) 0.008(4) -0.017(4) C40 0.044(5) 0.070(5) 0.071(5) -0.034(4) 0.024(4) -0.005(4) C41 0.035(4) 0.040(4) 0.053(4) -0.015(3) 0.016(3) -0.014(3) C42 0.036(4) 0.044(4) 0.052(4) -0.012(3) 0.020(3) -0.004(3) C43 0.035(4) 0.029(3) 0.037(4) -0.008(3) 0.016(3) -0.010(3) C44 0.035(4) 0.036(4) 0.044(4) -0.001(3) 0.021(3) -0.006(3) C45 0.149(10) 0.147(10) 0.058(6) 0.050(6) 0.006(6) 0.051(8) C46 0.152(10) 0.103(8) 0.069(7) 0.007(6) 0.037(7) -0.045(8) C47 0.080(6) 0.064(5) 0.044(5) 0.013(4) 0.023(5) 0.006(5) C48A 0.088(7) 0.081(7) 0.105(7) 0.013(6) 0.034(6) 0.000(6) C48B 0.075(6) 0.081(6) 0.112(7) 0.010(6) 0.036(6) -0.006(6) C49A 0.099(7) 0.084(7) 0.112(7) 0.005(6) 0.034(6) 0.013(6) C49B 0.087(7) 0.081(7) 0.110(7) -0.006(6) 0.017(6) 0.007(6) N3A 0.069(6) 0.067(5) 0.100(7) -0.001(6) 0.041(5) 0.005(5) N3B 0.060(6) 0.062(5) 0.097(7) 0.002(5) 0.035(5) 0.005(5) C50 0.073(6) 0.044(5) 0.126(8) -0.024(5) 0.049(6) -0.023(5) Dy1 0.03153(15) 0.02699(14) 0.03170(16) -0.00078(17) 0.00658(11) 0.00092(17) N1 0.029(3) 0.040(3) 0.045(3) -0.006(3) 0.008(3) 0.006(2) N2 0.091(6) 0.067(5) 0.046(4) 0.011(4) 0.020(4) 0.004(4) O1 0.057(3) 0.051(3) 0.043(3) 0.014(2) 0.017(3) 0.008(3) O2 0.048(3) 0.047(3) 0.064(3) -0.003(2) 0.024(2) 0.006(2) O3 0.040(3) 0.042(3) 0.058(3) -0.019(2) 0.014(2) -0.001(2) O4 0.050(3) 0.038(3) 0.056(3) -0.022(2) -0.001(2) 0.001(2) O5 0.045(3) 0.024(2) 0.036(2) -0.002(2) 0.017(2) 0.005(2) O6 0.042(3) 0.043(3) 0.050(3) -0.003(2) 0.016(2) -0.012(2) O7 0.032(2) 0.028(2) 0.052(3) 0.003(2) 0.009(2) 0.002(2) O8 0.035(3) 0.039(3) 0.040(3) 0.012(2) 0.008(2) 0.010(2) O9 0.040(3) 0.068(3) 0.039(3) -0.015(2) -0.001(2) 0.018(2) O10 0.028(3) 0.070(3) 0.073(3) -0.037(3) 0.014(2) -0.006(2) O11 0.040(3) 0.035(2) 0.035(3) -0.007(2) 0.005(2) -0.002(2) O12 0.044(3) 0.037(3) 0.122(5) -0.011(3) 0.024(3) 0.001(2) O13 0.053(3) 0.081(4) 0.071(4) -0.043(3) 0.024(3) -0.002(3) S1 0.0332(10) 0.0418(11) 0.0725(14) -0.0171(10) 0.0140(9) -0.0026(9) _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_ _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 -0.005 0.000 0.500 713 263 ' ' 2 -0.003 0.500 1.000 713 264 ' ' _platon_squeeze_details ; ; 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 C1 C2 1.506(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.365(9) . ? C2 C3 1.386(9) . ? C3 C4 1.386(9) . ? C3 H3 0.9300 . ? C4 C5 1.380(8) . ? C4 H4 0.9300 . ? C5 C6 1.356(8) . ? C5 S1 1.770(6) . ? C6 C7 1.375(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.457(7) . ? C8 C9 1.532(8) . ? C8 C33 1.536(8) . ? C8 C21 1.545(8) . ? C9 O11 1.434(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.363(8) . ? C10 O11 1.402(6) . ? C10 C19 1.414(8) . ? C11 C12 1.401(8) . ? C11 H11 0.9300 . ? C12 C13 1.402(8) . ? C12 C17 1.407(8) . ? C13 C14 1.362(9) . ? C13 H13 0.9300 . ? C14 C15 1.368(10) . ? C14 H14 0.9300 . ? C15 C16 1.369(9) . ? C15 H15 0.9300 . ? C16 C17 1.400(8) . ? C16 H16 0.9300 . ? C17 C18 1.416(8) . ? C18 C19 1.363(7) . ? C18 H18 0.9300 . ? C19 C20 1.516(7) . ? C20 O8 1.255(6) . ? C20 O7 1.256(7) . ? C21 O9 1.422(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.356(8) . ? C22 O9 1.378(7) . ? C22 C31 1.408(8) . ? C23 C24 1.411(8) . ? C23 H23 0.9300 . ? C24 C29 1.413(8) . ? C24 C25 1.426(8) . ? C25 C26 1.353(10) . ? C25 H25 0.9300 . ? C26 C27 1.400(10) . ? C26 H26 0.9300 . ? C27 C28 1.353(10) . ? C27 H27 0.9300 . ? C28 C29 1.398(9) . ? C28 H28 0.9300 . ? C29 C30 1.419(8) . ? C30 C31 1.372(7) . ? C30 H30 0.9300 . ? C31 C32 1.494(7) . ? C32 O6 1.261(6) . ? C32 O5 1.268(6) . ? C33 O10 1.427(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.358(8) . ? C34 O10 1.363(7) . ? C34 C43 1.422(8) . ? C35 C36 1.416(8) . ? C35 H35 0.9300 . ? C36 C41 1.402(8) . ? C36 C37 1.432(8) . ? C37 C38 1.340(8) . ? C37 H37 0.9300 . ? C38 C39 1.411(9) . ? C38 H38 0.9300 . ? C39 C40 1.358(9) . ? C39 H39 0.9300 . ? C40 C41 1.425(9) . ? C40 H40 0.9300 . ? C41 C42 1.404(8) . ? C42 C43 1.350(8) . ? C42 H42 0.9300 . ? C43 C44 1.490(8) . ? C44 O4 1.259(7) . ? C44 O3 1.268(7) . ? C44 Dy1 2.787(6) 3_655 ? C45 N2 1.446(9) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 N2 1.431(10) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 O1 1.214(8) . ? C47 N2 1.307(8) . ? C47 H47 0.9300 . ? C48A N3A 1.412(13) . ? C48A H48A 0.8957 . ? C48A H48B 0.9520 . ? C48A H48C 1.0256 . ? C48B N3B 1.457(13) . ? C48B H48D 0.9592 . ? C48B H48E 0.8947 . ? C48B H48F 0.8816 . ? C49A N3A 1.439(14) . ? C49A H49A 0.9437 . ? C49A H49B 0.9171 . ? C49A H49C 0.9486 . ? C49B N3B 1.435(13) . ? C49B H49D 0.9531 . ? C49B H49E 0.9430 . ? C49B H49F 0.9091 . ? N3A C50 1.391(12) . ? N3B C50 1.355(12) . ? C50 O2 1.193(8) . ? C50 H50A 0.9652 . ? C50 H50B 0.9360 . ? Dy1 O5 2.332(4) 3_655 ? Dy1 O1 2.374(4) . ? Dy1 O8 2.378(4) . ? Dy1 O7 2.391(4) 3_655 ? Dy1 O3 2.418(4) 3_655 ? Dy1 O4 2.419(4) 3_655 ? Dy1 O2 2.434(4) . ? Dy1 O6 2.458(4) . ? Dy1 O5 2.651(4) . ? Dy1 C44 2.787(6) 3_655 ? N1 S1 1.605(5) . ? N1 H1 0.8600 . ? O3 Dy1 2.418(4) 3_655 ? O4 Dy1 2.419(4) 3_655 ? O5 Dy1 2.332(4) 3_655 ? O7 Dy1 2.391(4) 3_655 ? O12 S1 1.436(5) . ? O13 S1 1.420(4) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 118.4(7) . . ? C7 C2 C1 119.7(7) . . ? C3 C2 C1 121.9(7) . . ? C4 C3 C2 120.7(7) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.4(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 119.7(6) . . ? C6 C5 S1 120.5(5) . . ? C4 C5 S1 119.6(5) . . ? C5 C6 C7 120.8(7) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C2 C7 C6 121.0(7) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N1 C8 C9 114.1(5) . . ? N1 C8 C33 109.0(5) . . ? C9 C8 C33 110.5(5) . . ? N1 C8 C21 107.1(5) . . ? C9 C8 C21 106.4(5) . . ? C33 C8 C21 109.6(5) . . ? O11 C9 C8 107.8(5) . . ? O11 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? O11 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.5 . . ? C11 C10 O11 120.2(5) . . ? C11 C10 C19 120.7(6) . . ? O11 C10 C19 119.1(5) . . ? C10 C11 C12 122.1(6) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C13 123.6(6) . . ? C11 C12 C17 118.0(6) . . ? C13 C12 C17 118.3(6) . . ? C14 C13 C12 120.8(7) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.6(7) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 120.6(7) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 120.0(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 119.4(6) . . ? C16 C17 C18 121.7(6) . . ? C12 C17 C18 118.8(6) . . ? C19 C18 C17 122.5(6) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C10 117.9(6) . . ? C18 C19 C20 119.5(5) . . ? C10 C19 C20 122.5(5) . . ? O8 C20 O7 126.9(5) . . ? O8 C20 C19 116.2(6) . . ? O7 C20 C19 116.8(6) . . ? O9 C21 C8 110.5(5) . . ? O9 C21 H21A 109.6 . . ? C8 C21 H21A 109.6 . . ? O9 C21 H21B 109.6 . . ? C8 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 O9 117.6(6) . . ? C23 C22 C31 120.7(6) . . ? O9 C22 C31 121.6(5) . . ? C22 C23 C24 120.9(6) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C29 119.9(6) . . ? C23 C24 C25 121.6(6) . . ? C29 C24 C25 118.4(6) . . ? C26 C25 C24 119.4(8) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 121.6(8) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 120.1(8) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.6(8) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C24 119.8(6) . . ? C28 C29 C30 123.2(7) . . ? C24 C29 C30 117.0(6) . . ? C31 C30 C29 122.5(6) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 C31 C22 118.8(6) . . ? C30 C31 C32 117.3(5) . . ? C22 C31 C32 123.8(5) . . ? O6 C32 O5 120.6(6) . . ? O6 C32 C31 118.8(5) . . ? O5 C32 C31 120.6(5) . . ? O10 C33 C8 107.7(5) . . ? O10 C33 H33A 110.2 . . ? C8 C33 H33A 110.2 . . ? O10 C33 H33B 110.2 . . ? C8 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C35 C34 O10 122.9(6) . . ? C35 C34 C43 121.0(6) . . ? O10 C34 C43 115.9(5) . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C41 C36 C35 118.8(6) . . ? C41 C36 C37 118.2(6) . . ? C35 C36 C37 123.0(6) . . ? C38 C37 C36 120.8(7) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 121.6(7) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C40 C39 C38 118.9(7) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C39 C40 C41 121.4(7) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C36 C41 C42 118.1(6) . . ? C36 C41 C40 119.0(6) . . ? C42 C41 C40 122.9(6) . . ? C43 C42 C41 123.9(6) . . ? C43 C42 H42 118.1 . . ? C41 C42 H42 118.1 . . ? C42 C43 C34 117.4(6) . . ? C42 C43 C44 118.5(6) . . ? C34 C43 C44 124.1(6) . . ? O4 C44 O3 119.5(6) . . ? O4 C44 C43 120.7(6) . . ? O3 C44 C43 119.8(6) . . ? O4 C44 Dy1 60.1(3) . 3_655 ? O3 C44 Dy1 60.1(3) . 3_655 ? C43 C44 Dy1 172.2(4) . 3_655 ? N2 C45 H45A 109.5 . . ? N2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N2 C46 H46A 109.5 . . ? N2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O1 C47 N2 125.9(8) . . ? O1 C47 H47 117.1 . . ? N2 C47 H47 117.1 . . ? N3A C48A H48A 94.6 . . ? N3A C48A H48B 106.7 . . ? H48A C48A H48B 123.2 . . ? N3A C48A H48C 103.6 . . ? H48A C48A H48C 107.3 . . ? H48B C48A H48C 117.2 . . ? N3A C48A H48D 97.7 . . ? H48B C48A H48D 141.4 . . ? H48C C48A H48D 84.4 . . ? N3A C48A H48F 90.3 . . ? H48A C48A H48F 76.6 . . ? H48B C48A H48F 52.0 . . ? H48C C48A H48F 165.0 . . ? H48D C48A H48F 99.4 . . ? N3B C48B H48A 115.1 . . ? N3B C48B H48B 101.7 . . ? H48A C48B H48B 85.6 . . ? N3B C48B H48D 105.9 . . ? H48B C48B H48D 80.2 . . ? N3B C48B H48E 105.0 . . ? H48A C48B H48E 100.1 . . ? H48B C48B H48E 147.0 . . ? H48D C48B H48E 110.2 . . ? N3B C48B H48F 103.8 . . ? H48A C48B H48F 113.4 . . ? H48D C48B H48F 111.1 . . ? H48E C48B H48F 119.7 . . ? N3A C49A H49A 110.0 . . ? N3A C49A H49B 100.1 . . ? H49A C49A H49B 107.4 . . ? N3A C49A H49C 114.3 . . ? H49A C49A H49C 111.8 . . ? H49B C49A H49C 112.5 . . ? N3A C49A H49E 140.0 . . ? H49A C49A H49E 86.2 . . ? H49C C49A H49E 90.9 . . ? N3B C49B H49A 98.5 . . ? N3B C49B H49B 90.1 . . ? H49A C49B H49B 98.3 . . ? N3B C49B H49D 108.5 . . ? H49A C49B H49D 54.6 . . ? H49B C49B H49D 148.3 . . ? N3B C49B H49E 112.2 . . ? H49A C49B H49E 64.3 . . ? H49D C49B H49E 109.5 . . ? N3B C49B H49F 104.4 . . ? H49A C49B H49F 154.8 . . ? H49B C49B H49F 92.1 . . ? H49D C49B H49F 107.1 . . ? H49E C49B H49F 114.8 . . ? C50 N3A C48A 123.1(12) . . ? C50 N3A C49A 117.6(12) . . ? C48A N3A C49A 119.0(14) . . ? C50 N3B C49B 119.9(11) . . ? C50 N3B C48B 115.5(11) . . ? C49B N3B C48B 123.8(13) . . ? O2 C50 N3B 127.0(8) . . ? O2 C50 N3A 120.3(9) . . ? O2 C50 H50A 118.6 . . ? N3B C50 H50A 103.4 . . ? N3A C50 H50A 121.1 . . ? O2 C50 H50B 116.3 . . ? N3B C50 H50B 116.6 . . ? N3A C50 H50B 112.0 . . ? O5 Dy1 O1 148.29(14) 3_655 . ? O5 Dy1 O8 72.52(13) 3_655 . ? O1 Dy1 O8 139.14(14) . . ? O5 Dy1 O7 78.58(13) 3_655 3_655 ? O1 Dy1 O7 75.35(14) . 3_655 ? O8 Dy1 O7 132.88(13) . 3_655 ? O5 Dy1 O3 82.04(13) 3_655 3_655 ? O1 Dy1 O3 97.71(15) . 3_655 ? O8 Dy1 O3 88.34(15) . 3_655 ? O7 Dy1 O3 123.75(14) 3_655 3_655 ? O5 Dy1 O4 77.33(14) 3_655 3_655 ? O1 Dy1 O4 77.25(15) . 3_655 ? O8 Dy1 O4 134.28(14) . 3_655 ? O7 Dy1 O4 70.67(14) 3_655 3_655 ? O3 Dy1 O4 53.65(14) 3_655 3_655 ? O5 Dy1 O2 137.58(14) 3_655 . ? O1 Dy1 O2 70.46(15) . . ? O8 Dy1 O2 72.87(14) . . ? O7 Dy1 O2 143.84(15) 3_655 . ? O3 Dy1 O2 73.19(14) 3_655 . ? O4 Dy1 O2 111.78(15) 3_655 . ? O5 Dy1 O6 121.49(13) 3_655 . ? O1 Dy1 O6 72.91(15) . . ? O8 Dy1 O6 81.36(14) . . ? O7 Dy1 O6 83.11(13) 3_655 . ? O3 Dy1 O6 149.16(14) 3_655 . ? O4 Dy1 O6 144.33(14) 3_655 . ? O2 Dy1 O6 76.01(14) . . ? O5 Dy1 O5 71.08(14) 3_655 . ? O1 Dy1 O5 113.00(14) . . ? O8 Dy1 O5 69.82(13) . . ? O7 Dy1 O5 65.93(12) 3_655 . ? O3 Dy1 O5 149.25(13) 3_655 . ? O4 Dy1 O5 130.06(13) 3_655 . ? O2 Dy1 O5 117.72(13) . . ? O6 Dy1 O5 50.76(12) . . ? O5 Dy1 C44 75.92(15) 3_655 3_655 ? O1 Dy1 C44 89.48(16) . 3_655 ? O8 Dy1 C44 110.86(17) . 3_655 ? O7 Dy1 C44 96.76(17) 3_655 3_655 ? O3 Dy1 C44 27.04(15) 3_655 3_655 ? O4 Dy1 C44 26.82(15) 3_655 3_655 ? O2 Dy1 C44 94.41(16) . 3_655 ? O6 Dy1 C44 161.89(16) . 3_655 ? O5 Dy1 C44 145.05(14) . 3_655 ? C8 N1 S1 127.3(4) . . ? C8 N1 H1 116.3 . . ? S1 N1 H1 116.3 . . ? C47 N2 C46 118.2(7) . . ? C47 N2 C45 122.6(8) . . ? C46 N2 C45 119.2(7) . . ? C47 O1 Dy1 135.1(5) . . ? C50 O2 Dy1 132.4(5) . . ? C44 O3 Dy1 92.9(4) . 3_655 ? C44 O4 Dy1 93.1(4) . 3_655 ? C32 O5 Dy1 161.7(4) . 3_655 ? C32 O5 Dy1 89.3(3) . . ? Dy1 O5 Dy1 108.92(14) 3_655 . ? C32 O6 Dy1 98.6(4) . . ? C20 O7 Dy1 136.3(4) . 3_655 ? C20 O8 Dy1 138.1(4) . . ? C22 O9 C21 117.1(5) . . ? C34 O10 C33 119.6(5) . . ? C10 O11 C9 113.9(4) . . ? O13 S1 O12 119.8(3) . . ? O13 S1 N1 105.8(3) . . ? O12 S1 N1 109.0(3) . . ? O13 S1 C5 106.9(3) . . ? O12 S1 C5 106.8(3) . . ? N1 S1 C5 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.067 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.108 #==END