Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Aime, Silvio' 'Barge, Alessandro' 'Batsanov, Andrei S.' 'Botta, Mauro' 'Delli Castelli, Davide' 'Fedeli, Federico' 'Mortilaro, Antonio' 'Parker, David' 'Puschmann, Horst' _publ_contact_author_name 'Prof D Parker' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email DAVID.PARKER@DURHAM.AC.UK _journal_name_full 'Chemical Communications' _publ_section_title ; Controlling the variation of axial water exchange rates in macrocyclic lanthanide (III) complexes ; #==========================================================END data_7 _database_code_CSD 182447 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Gd N8 O5 3+,3(N O3 1-),5(H2 O)' _chemical_formula_sum 'C48 H76 Gd N11 O19' _chemical_formula_weight 1268.45 _chemical_absolute_configuration ad 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' '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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 23.290(6) _cell_length_b 11.271(3) _cell_length_c 22.244(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.13(1) _cell_angle_gamma 90.00 _cell_volume 5662(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9812 _cell_measurement_theta_min 2.3205 _cell_measurement_theta_max 28.5115 _exptl_crystal_description octahedron _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.6 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2628 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.472 _exptl_absorpt_correction_T_min 0.382 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998), R(int)=0.065 before correction' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 6 sets of \w scans each set at different \f and/or 2\q angles and each scan (5 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'SMART 6000 CCD area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33975 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.51 _reflns_number_total 14382 _reflns_number_gt 14112 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.91 _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. The N(7)O~3~^-^ anion is disordered: O(71), O(72), O(73) occupy 2 sets of positions, A and B, with occupancies 57.8(7)% and 42.2(7)%. H atoms at amido-N, O(1), O(1W), O(2W) and O(5W) atoms - refall, methyl groups - rigid (rotating) bodies with a common refined U for the three H atoms, all other H atoms - 'riding'. ; _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^)+(0.0237P)^2^+5.4307P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(4) _refine_ls_number_reflns 14382 _refine_ls_number_parameters 768 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.5000 0.268594(11) 0.5000 0.01954(4) Uani 1 2 d S . . O1 O 0.5000 0.0600(3) 0.5000 0.0389(6) Uani 1 2 d S . . H01 H 0.4809(15) 0.015(3) 0.5127(16) 0.047(9) Uiso 1 1 d . . . O11 O 0.59670(7) 0.20443(15) 0.54603(7) 0.0307(4) Uani 1 1 d . . . O21 O 0.52691(6) 0.20423(13) 0.40937(6) 0.0243(3) Uani 1 1 d . . . N1 N 0.55896(8) 0.40951(17) 0.58950(8) 0.0241(3) Uani 1 1 d . . . N2 N 0.57401(8) 0.41360(16) 0.46029(8) 0.0228(3) Uani 1 1 d . . . N11 N 0.67839(8) 0.19156(19) 0.62376(8) 0.0282(4) Uani 1 1 d . . . H1N H 0.7013(13) 0.214(3) 0.6584(14) 0.041(8) Uiso 1 1 d . . . N21 N 0.58713(8) 0.18884(18) 0.34470(8) 0.0235(3) Uani 1 1 d . . . H2N H 0.6126(12) 0.220(3) 0.3303(12) 0.030(7) Uiso 1 1 d . . . C1 C 0.59213(10) 0.5044(2) 0.56574(10) 0.0286(4) Uani 1 1 d . . . H011 H 0.6239 0.5348 0.6004 0.037 Uiso 1 1 d R . . H012 H 0.5647 0.5709 0.5503 0.037 Uiso 1 1 d R . . C2 C 0.61940(9) 0.4639(2) 0.51351(10) 0.0275(4) Uani 1 1 d . . . H021 H 0.6394 0.5317 0.4989 0.036 Uiso 1 1 d R . . H022 H 0.6497 0.4025 0.5297 0.036 Uiso 1 1 d R . . C3 C 0.53805(10) 0.5123(2) 0.42447(10) 0.0273(4) Uani 1 1 d . . . H031 H 0.5629 0.5575 0.4023 0.035 Uiso 1 1 d R . . H032 H 0.5258 0.5670 0.4539 0.035 Uiso 1 1 d R . . C4 C 0.48297(9) 0.4677(2) 0.37818(10) 0.0276(4) Uani 1 1 d . . . H041 H 0.4629 0.5349 0.3529 0.036 Uiso 1 1 d R . . H042 H 0.4947 0.4097 0.3500 0.036 Uiso 1 1 d R . . C10 C 0.60038(10) 0.3308(2) 0.63323(10) 0.0274(5) Uani 1 1 d . . . H101 H 0.5788 0.2910 0.6608 0.036 Uiso 1 1 d R . . H102 H 0.6326 0.3788 0.6593 0.036 Uiso 1 1 d R . . C11 C 0.62629(9) 0.2387(2) 0.59821(9) 0.0269(4) Uani 1 1 d . . . C12 C 0.70187(10) 0.0943(2) 0.59215(10) 0.0284(4) Uani 1 1 d . . . H12 H 0.6680 0.0407 0.5734 0.034 Uiso 1 1 d R . . C13 C 0.74605(11) 0.0225(2) 0.63978(11) 0.0351(5) Uani 1 1 d . . . H131 H 0.7777 0.0752 0.6618 0.037(4) Uiso 1 1 d R . . H132 H 0.7630 -0.0399 0.6187 0.037(4) Uiso 1 1 d R . . H133 H 0.7264 -0.0137 0.6695 0.037(4) Uiso 1 1 d R . . C14 C 0.72749(11) 0.1409(2) 0.54102(10) 0.0317(5) Uani 1 1 d . . . C15 C 0.77039(15) 0.2272(4) 0.55231(15) 0.0517(8) Uani 1 1 d . . . H15 H 0.7832 0.2605 0.5926 0.062 Uiso 1 1 d R . . C16 C 0.7949(2) 0.2665(4) 0.5048(2) 0.0710(12) Uani 1 1 d . . . H16 H 0.8239 0.3275 0.5124 0.085 Uiso 1 1 d R . . C17 C 0.77677(17) 0.2178(3) 0.44634(15) 0.0597(9) Uani 1 1 d . . . H17 H 0.7939 0.2445 0.4141 0.072 Uiso 1 1 d R . . C18 C 0.73499(14) 0.1329(4) 0.43485(13) 0.0552(9) Uani 1 1 d . . . H18 H 0.7232 0.0993 0.3945 0.066 Uiso 1 1 d R . . C19 C 0.70941(12) 0.0938(3) 0.48149(12) 0.0443(6) Uani 1 1 d . . . H19 H 0.6796 0.0343 0.4728 0.053 Uiso 1 1 d R . . C20 C 0.60505(10) 0.3473(2) 0.42009(10) 0.0271(5) Uani 1 1 d . . . H201 H 0.6439 0.3199 0.4452 0.035 Uiso 1 1 d R . . H202 H 0.6124 0.4011 0.3876 0.035 Uiso 1 1 d R . . C21 C 0.56952(8) 0.2422(2) 0.38993(8) 0.0226(4) Uani 1 1 d . . . C22 C 0.56117(9) 0.07496(19) 0.32052(10) 0.0247(4) Uani 1 1 d . . . H22 H 0.5588 0.0239 0.3566 0.030 Uiso 1 1 d R . . C23 C 0.60244(10) 0.0144(2) 0.28637(12) 0.0333(5) Uani 1 1 d . . . H231 H 0.6058 0.0636 0.2511 0.040(5) Uiso 1 1 d R . . H232 H 0.5864 -0.0635 0.2714 0.040(5) Uiso 1 1 d R . . H233 H 0.6417 0.0045 0.3146 0.040(5) Uiso 1 1 d R . . C24 C 0.49932(9) 0.08901(19) 0.27967(10) 0.0237(4) Uani 1 1 d . . . C25 C 0.48670(10) 0.17389(19) 0.23340(10) 0.0275(4) Uani 1 1 d . . . H25 H 0.5166 0.2283 0.2291 0.033 Uiso 1 1 d R . . C26 C 0.43039(11) 0.1811(2) 0.19335(10) 0.0326(5) Uani 1 1 d . . . H26 H 0.4220 0.2397 0.1618 0.039 Uiso 1 1 d R . . C27 C 0.38745(11) 0.1021(3) 0.19983(13) 0.0420(6) Uani 1 1 d . . . H27 H 0.3494 0.1050 0.1720 0.050 Uiso 1 1 d R . . C28 C 0.39893(12) 0.0182(3) 0.24635(17) 0.0520(8) Uani 1 1 d . . . H28 H 0.3687 -0.0353 0.2509 0.062 Uiso 1 1 d R . . C29 C 0.45487(11) 0.0121(2) 0.28657(13) 0.0392(6) Uani 1 1 d . . . H29 H 0.4626 -0.0449 0.3190 0.047 Uiso 1 1 d R . . Gd2 Gd 0.5000 0.730731(8) 0.0000 0.01314(3) Uani 1 2 d S . . O2 O 0.5000 0.51933(18) 0.0000 0.0224(4) Uani 1 2 d S . . H02 H 0.4836(16) 0.476(3) 0.0182(17) 0.056(10) Uiso 1 1 d . . . O31 O 0.58987(6) 0.66959(12) 0.06778(6) 0.0192(3) Uani 1 1 d . . . O41 O 0.54623(6) 0.66629(12) -0.07675(6) 0.0196(3) Uani 1 1 d . . . N3 N 0.53851(7) 0.87485(14) 0.09604(7) 0.0173(3) Uani 1 1 d . . . N4 N 0.58554(7) 0.87627(14) -0.01850(7) 0.0180(3) Uani 1 1 d . . . N31 N 0.65863(7) 0.67039(15) 0.15818(7) 0.0191(3) Uani 1 1 d . . . H3N H 0.6716(10) 0.708(2) 0.1906(11) 0.017(6) Uiso 1 1 d . . . N41 N 0.61860(8) 0.65773(15) -0.12728(8) 0.0224(3) Uani 1 1 d . . . H4N H 0.6527(12) 0.691(3) -0.1319(12) 0.035(7) Uiso 1 1 d . . . C5 C 0.57607(9) 0.97119(17) 0.08019(9) 0.0221(4) Uani 1 1 d . . . H51 H 0.5995 1.0072 0.1191 0.029 Uiso 1 1 d R . . H52 H 0.5499 1.0336 0.0569 0.029 Uiso 1 1 d R . . C6 C 0.61795(9) 0.93022(18) 0.04161(9) 0.0211(4) Uani 1 1 d . . . H61 H 0.6415 0.9986 0.0333 0.027 Uiso 1 1 d R . . H62 H 0.6457 0.8709 0.0656 0.027 Uiso 1 1 d R . . C7 C 0.56004(9) 0.97262(17) -0.06235(9) 0.0219(4) Uani 1 1 d . . . H71 H 0.5921 1.0094 -0.0782 0.028 Uiso 1 1 d R . . H72 H 0.5436 1.0345 -0.0397 0.028 Uiso 1 1 d R . . C8 C 0.51175(9) 0.92936(17) -0.11682(9) 0.0208(4) Uani 1 1 d . . . H81 H 0.4969 0.9972 -0.1445 0.027 Uiso 1 1 d R . . H82 H 0.5284 0.8703 -0.1408 0.027 Uiso 1 1 d R . . C30 C 0.57380(8) 0.80088(18) 0.14663(8) 0.0199(3) Uani 1 1 d . . . H301 H 0.5471 0.7607 0.1687 0.026 Uiso 1 1 d R . . H302 H 0.6012 0.8521 0.1768 0.026 Uiso 1 1 d R . . C31 C 0.60892(8) 0.70936(16) 0.12129(9) 0.0164(4) Uani 1 1 d . . . C32 C 0.69273(8) 0.57573(17) 0.13748(9) 0.0203(4) Uani 1 1 d . . . H32 H 0.6644 0.5131 0.1166 0.024 Uiso 1 1 d R . . C33 C 0.73458(11) 0.5210(3) 0.19415(12) 0.0267(5) Uani 1 1 d . . . H331 H 0.7606 0.5826 0.2172 0.033(4) Uiso 1 1 d R . . H332 H 0.7586 0.4597 0.1808 0.033(4) Uiso 1 1 d R . . H333 H 0.7115 0.4853 0.2209 0.033(4) Uiso 1 1 d R . . C34 C 0.72539(8) 0.62320(18) 0.09125(9) 0.0215(4) Uani 1 1 d . . . C35 C 0.75701(8) 0.7290(2) 0.10211(9) 0.0251(4) Uani 1 1 d . . . H35 H 0.7566 0.7746 0.1379 0.030 Uiso 1 1 d R . . C36 C 0.78898(11) 0.7681(3) 0.06037(11) 0.0327(5) Uani 1 1 d . . . H36 H 0.8116 0.8390 0.0687 0.039 Uiso 1 1 d R . . C37 C 0.78783(10) 0.7036(3) 0.00694(12) 0.0364(7) Uani 1 1 d . . . H37 H 0.8089 0.7314 -0.0219 0.044 Uiso 1 1 d R . . C38 C 0.75587(11) 0.5993(2) -0.00436(11) 0.0352(5) Uani 1 1 d . . . H38 H 0.7553 0.5548 -0.0408 0.042 Uiso 1 1 d R . . C39 C 0.72478(10) 0.5588(2) 0.03765(10) 0.0285(4) Uani 1 1 d . . . H39 H 0.7030 0.4868 0.0298 0.034 Uiso 1 1 d R . . C40 C 0.62685(8) 0.80259(18) -0.04381(9) 0.0215(4) Uani 1 1 d . . . H401 H 0.6567 0.7670 -0.0091 0.028 Uiso 1 1 d R . . H402 H 0.6479 0.8533 -0.0678 0.028 Uiso 1 1 d R . . C41 C 0.59433(9) 0.70469(18) -0.08494(9) 0.0188(4) Uani 1 1 d . . . C42 C 0.59092(10) 0.55465(18) -0.16363(10) 0.0249(4) Uani 1 1 d . . . H42 H 0.5837 0.4925 -0.1342 0.030 Uiso 1 1 d R . . C43 C 0.63351(11) 0.5038(2) -0.19947(11) 0.0308(5) Uani 1 1 d . . . H431 H 0.6394 0.5620 -0.2302 0.038(4) Uiso 1 1 d R . . H432 H 0.6167 0.4309 -0.2207 0.038(4) Uiso 1 1 d R . . H433 H 0.6716 0.4859 -0.1707 0.038(4) Uiso 1 1 d R . . C44 C 0.53184(10) 0.58694(18) -0.20697(10) 0.0250(4) Uani 1 1 d . . . C45 C 0.52661(10) 0.6835(2) -0.24667(10) 0.0291(4) Uani 1 1 d . . . H45 H 0.5602 0.7317 -0.2462 0.035 Uiso 1 1 d R . . C46 C 0.47265(11) 0.7102(2) -0.28732(11) 0.0367(6) Uani 1 1 d . . . H46 H 0.4692 0.7762 -0.3146 0.044 Uiso 1 1 d R . . C47 C 0.42331(12) 0.6402(3) -0.28795(12) 0.0426(6) Uani 1 1 d . . . H47 H 0.3862 0.6590 -0.3151 0.051 Uiso 1 1 d R . . C48 C 0.42790(12) 0.5437(3) -0.24921(13) 0.0418(6) Uani 1 1 d . . . H48 H 0.3944 0.4947 -0.2509 0.050 Uiso 1 1 d R . . C49 C 0.48204(11) 0.5174(2) -0.20845(12) 0.0337(5) Uani 1 1 d . . . H49 H 0.4848 0.4523 -0.1808 0.040 Uiso 1 1 d R . . N5 N 0.73491(8) 0.89343(17) 0.26178(9) 0.0261(4) Uani 1 1 d . . . O51 O 0.76680(9) 0.9545(2) 0.30424(10) 0.0372(5) Uani 1 1 d . . . O52 O 0.70767(8) 0.93970(16) 0.21270(8) 0.0358(4) Uani 1 1 d . . . O53 O 0.73050(8) 0.78326(15) 0.27002(8) 0.0382(4) Uani 1 1 d . . . N7 N 0.60127(10) 0.2652(2) 0.10936(10) 0.0390(5) Uani 1 1 d . . . O71A O 0.59288(16) 0.2376(3) 0.05321(14) 0.0397(9) Uiso 0.578(7) 1 d P A 1 O72A O 0.6502(2) 0.2810(4) 0.1418(3) 0.0641(13) Uiso 0.578(7) 1 d P A 1 O73A O 0.5591(2) 0.2591(3) 0.13492(19) 0.0519(11) Uiso 0.578(7) 1 d P A 1 O71B O 0.5608(4) 0.2432(7) 0.0581(3) 0.081(2) Uiso 0.422(7) 1 d P A 2 O72B O 0.6516(3) 0.2878(7) 0.1084(4) 0.078(2) Uiso 0.422(7) 1 d P A 2 O73B O 0.5877(3) 0.2840(7) 0.1560(3) 0.068(2) Uiso 0.422(7) 1 d P A 2 O2W O 0.66340(9) 0.29350(17) 0.27801(10) 0.0356(4) Uani 1 1 d . . . H2W1 H 0.6991(14) 0.271(3) 0.2819(14) 0.040(8) Uiso 1 1 d . . . H2W2 H 0.6486(14) 0.282(3) 0.2484(15) 0.041(10) Uiso 1 1 d . . . O3W O 0.44930(11) 0.34641(18) 0.06070(11) 0.0513(5) Uani 1 1 d . . . H3W1 H 0.4841 0.3202 0.0788 0.077 Uiso 1 1 d R . . H3W2 H 0.4257 0.3372 0.0196 0.077 Uiso 1 1 d R . . N6 N 0.90879(13) 1.2925(2) 0.38209(13) 0.0468(7) Uani 1 1 d . . . O61 O 0.88998(11) 1.2485(3) 0.33979(14) 0.0745(8) Uani 1 1 d . . . O62 O 0.96699(12) 1.2644(2) 0.41152(14) 0.0740(7) Uani 1 1 d . . . O63 O 0.88852(18) 1.3631(4) 0.41077(18) 0.1193(15) Uani 1 1 d . . . O1W O 0.77439(9) 1.19829(18) 0.27928(8) 0.0364(4) Uani 1 1 d . . . H1W1 H 0.8095(18) 1.210(4) 0.2970(18) 0.077(13) Uiso 1 1 d . . . H1W2 H 0.7748(16) 1.122(4) 0.2849(17) 0.062(11) Uiso 1 1 d . . . O4W O 1.06651(13) 1.3963(2) 0.46300(19) 0.0898(10) Uani 1 1 d . . . H4W1 H 1.0348 1.3363 0.4287 0.135 Uiso 1 1 d R . . H4W2 H 1.0824 1.3726 0.5049 0.135 Uiso 1 1 d R . . O5W O 0.77567(9) 1.2371(2) 0.15472(9) 0.0465(5) Uani 1 1 d . . . H5W1 H 0.7320(18) 1.244(4) 0.1377(18) 0.078(12) Uiso 1 1 d . . . H5W2 H 0.7759(15) 1.222(4) 0.1885(16) 0.054(10) Uiso 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 0.01730(7) 0.03107(8) 0.01049(6) 0.000 0.00389(5) 0.000 O1 0.0449(15) 0.0395(15) 0.0397(14) 0.000 0.0242(12) 0.000 O11 0.0238(7) 0.0466(10) 0.0183(6) -0.0107(6) -0.0015(5) 0.0085(6) O21 0.0246(7) 0.0347(9) 0.0153(6) -0.0037(5) 0.0081(5) -0.0055(6) N1 0.0239(8) 0.0322(9) 0.0164(7) -0.0062(6) 0.0055(6) 0.0024(7) N2 0.0207(8) 0.0322(9) 0.0165(7) -0.0068(6) 0.0065(6) -0.0049(7) N11 0.0250(8) 0.0391(9) 0.0172(8) -0.0062(7) -0.0013(7) 0.0058(8) N21 0.0225(8) 0.0301(8) 0.0201(8) -0.0056(7) 0.0093(6) -0.0044(7) C1 0.0269(10) 0.0357(11) 0.0234(10) -0.0126(8) 0.0068(8) -0.0030(8) C2 0.0224(9) 0.0382(12) 0.0219(9) -0.0116(8) 0.0055(8) -0.0060(8) C3 0.0284(10) 0.0327(11) 0.0222(10) 0.0015(8) 0.0087(8) -0.0064(8) C4 0.0262(10) 0.0384(12) 0.0189(9) 0.0073(8) 0.0068(8) -0.0057(8) C10 0.0237(10) 0.0416(13) 0.0153(9) -0.0060(9) 0.0018(8) 0.0057(9) C11 0.0229(9) 0.0399(11) 0.0165(8) -0.0045(9) 0.0021(7) 0.0016(9) C12 0.0280(10) 0.0334(11) 0.0213(9) -0.0033(8) 0.0008(8) 0.0064(8) C13 0.0357(12) 0.0392(13) 0.0269(11) 0.0013(9) 0.0007(9) 0.0091(10) C14 0.0346(11) 0.0348(12) 0.0249(10) 0.0011(9) 0.0057(9) 0.0149(9) C15 0.072(2) 0.0423(15) 0.0498(16) -0.0132(16) 0.0327(15) -0.010(2) C16 0.100(3) 0.047(2) 0.088(3) -0.0039(19) 0.063(2) -0.007(2) C17 0.084(2) 0.055(2) 0.0546(17) 0.0181(15) 0.0437(17) 0.0350(18) C18 0.0528(17) 0.086(2) 0.0286(13) 0.0067(14) 0.0132(12) 0.0294(17) C19 0.0373(13) 0.0669(19) 0.0264(12) -0.0051(11) 0.0034(10) 0.0119(12) C20 0.0226(10) 0.0405(13) 0.0201(10) -0.0092(9) 0.0090(8) -0.0074(9) C21 0.0217(8) 0.0323(10) 0.0142(8) -0.0002(8) 0.0050(7) -0.0011(8) C22 0.0253(10) 0.0275(10) 0.0226(9) -0.0046(8) 0.0085(8) -0.0006(8) C23 0.0272(11) 0.0381(13) 0.0361(13) -0.0133(10) 0.0105(10) 0.0015(9) C24 0.0241(9) 0.0252(10) 0.0230(9) -0.0039(7) 0.0079(8) 0.0013(7) C25 0.0329(11) 0.0261(11) 0.0249(10) -0.0037(8) 0.0098(8) -0.0038(8) C26 0.0396(12) 0.0328(11) 0.0256(10) 0.0029(9) 0.0086(9) 0.0101(10) C27 0.0272(11) 0.0504(15) 0.0441(14) 0.0060(12) 0.0006(10) 0.0094(10) C28 0.0249(12) 0.0578(19) 0.069(2) 0.0231(16) 0.0037(13) -0.0049(12) C29 0.0272(11) 0.0425(14) 0.0485(15) 0.0194(11) 0.0104(10) 0.0007(10) Gd2 0.01543(6) 0.01409(6) 0.01080(6) 0.000 0.00491(5) 0.000 O2 0.0312(11) 0.0178(9) 0.0224(10) 0.000 0.0145(9) 0.000 O31 0.0205(6) 0.0218(7) 0.0146(6) -0.0021(5) 0.0030(5) 0.0017(5) O41 0.0230(7) 0.0211(7) 0.0173(6) -0.0011(5) 0.0103(5) -0.0015(5) N3 0.0206(7) 0.0175(7) 0.0143(7) -0.0014(5) 0.0055(6) 0.0015(6) N4 0.0199(7) 0.0187(7) 0.0163(7) -0.0004(6) 0.0062(6) -0.0018(6) N31 0.0188(7) 0.0239(9) 0.0137(7) -0.0016(6) 0.0025(6) 0.0020(6) N41 0.0254(8) 0.0239(8) 0.0217(8) -0.0032(6) 0.0128(7) -0.0012(6) C5 0.0275(10) 0.0178(8) 0.0214(9) -0.0051(7) 0.0067(8) -0.0036(7) C6 0.0223(9) 0.0216(9) 0.0196(9) -0.0023(7) 0.0056(7) -0.0050(7) C7 0.0250(9) 0.0208(9) 0.0206(9) 0.0045(7) 0.0071(7) -0.0044(7) C8 0.0238(9) 0.0203(9) 0.0188(9) 0.0047(7) 0.0065(7) -0.0041(7) C30 0.0204(8) 0.0257(9) 0.0140(8) -0.0016(7) 0.0051(6) 0.0020(7) C31 0.0175(8) 0.0172(11) 0.0152(8) 0.0010(7) 0.0055(7) -0.0013(6) C32 0.0195(8) 0.0216(9) 0.0191(9) 0.0011(7) 0.0034(7) 0.0028(7) C33 0.0239(11) 0.0295(12) 0.0250(11) 0.0052(10) 0.0026(9) 0.0039(9) C34 0.0183(8) 0.0265(10) 0.0187(9) 0.0002(7) 0.0028(7) 0.0051(7) C35 0.0230(8) 0.0303(9) 0.0221(9) 0.0022(8) 0.0058(7) 0.0015(9) C36 0.0296(11) 0.0372(13) 0.0332(11) 0.0076(10) 0.0114(9) -0.0001(10) C37 0.0254(10) 0.056(2) 0.0312(11) 0.0100(11) 0.0144(9) 0.0097(11) C38 0.0311(11) 0.0508(14) 0.0267(11) -0.0017(10) 0.0130(9) 0.0147(10) C39 0.0271(10) 0.0337(11) 0.0259(10) -0.0034(8) 0.0088(8) 0.0072(8) C40 0.0196(8) 0.0271(9) 0.0200(8) -0.0024(7) 0.0094(7) -0.0022(7) C41 0.0222(9) 0.0197(11) 0.0166(8) 0.0023(7) 0.0089(7) 0.0021(7) C42 0.0338(11) 0.0195(9) 0.0268(10) -0.0037(7) 0.0180(9) -0.0019(8) C43 0.0389(12) 0.0282(11) 0.0315(11) -0.0061(9) 0.0203(10) 0.0016(9) C44 0.0327(11) 0.0237(10) 0.0228(9) -0.0076(7) 0.0152(8) -0.0038(8) C45 0.0355(11) 0.0326(10) 0.0227(9) -0.0058(8) 0.0140(8) -0.0036(9) C46 0.0448(13) 0.0439(16) 0.0233(10) -0.0047(9) 0.0121(9) 0.0057(10) C47 0.0336(12) 0.0613(17) 0.0321(12) -0.0210(12) 0.0064(10) 0.0011(11) C48 0.0369(13) 0.0470(15) 0.0453(15) -0.0234(12) 0.0172(11) -0.0140(11) C49 0.0401(13) 0.0288(11) 0.0385(13) -0.0123(9) 0.0216(11) -0.0089(9) N5 0.0223(8) 0.0303(9) 0.0245(9) -0.0036(7) 0.0035(7) 0.0011(7) O51 0.0335(10) 0.0352(11) 0.0371(10) -0.0090(9) -0.0024(8) -0.0042(8) O52 0.0361(9) 0.0355(9) 0.0308(8) 0.0050(7) -0.0016(7) 0.0041(7) O53 0.0483(10) 0.0282(8) 0.0293(8) 0.0003(7) -0.0075(7) -0.0018(7) N7 0.0402(11) 0.0405(12) 0.0359(11) 0.0029(9) 0.0088(9) 0.0093(9) O2W 0.0342(9) 0.0383(10) 0.0398(10) -0.0003(8) 0.0198(8) 0.0008(8) O3W 0.0645(14) 0.0416(11) 0.0554(13) 0.0011(9) 0.0292(11) -0.0059(9) N6 0.0819(19) 0.0229(11) 0.0572(15) 0.0017(10) 0.0587(15) 0.0023(11) O61 0.0538(14) 0.099(2) 0.0792(18) 0.0203(18) 0.0323(13) 0.0067(16) O62 0.0649(15) 0.0575(16) 0.095(2) -0.0036(14) 0.0110(14) 0.0174(12) O63 0.115(3) 0.145(4) 0.097(2) -0.025(2) 0.023(2) 0.066(3) O1W 0.0409(10) 0.0365(10) 0.0345(9) 0.0009(7) 0.0146(8) 0.0056(8) O4W 0.0732(18) 0.0546(16) 0.160(3) 0.0066(18) 0.063(2) 0.0101(13) O5W 0.0504(11) 0.0628(12) 0.0322(9) 0.0101(9) 0.0218(8) 0.0268(10) _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 O11 2.3490(14) 2_656 ? Gd1 O11 2.3490(14) . ? Gd1 O1 2.351(3) . ? Gd1 O21 2.3665(13) . ? Gd1 O21 2.3665(13) 2_656 ? Gd1 N1 2.6527(17) 2_656 ? Gd1 N1 2.6527(17) . ? Gd1 N2 2.6770(17) 2_656 ? Gd1 N2 2.6770(17) . ? O11 C11 1.257(2) . ? O21 C21 1.251(2) . ? N1 C10 1.485(3) . ? N1 C1 1.490(3) . ? N1 C4 1.498(3) 2_656 ? N2 C20 1.482(3) . ? N2 C2 1.493(3) . ? N2 C3 1.499(3) . ? N11 C11 1.320(3) . ? N11 C12 1.477(3) . ? N21 C21 1.321(3) . ? N21 C22 1.464(3) . ? C1 C2 1.524(3) . ? C3 C4 1.521(3) . ? C4 N1 1.498(3) 2_656 ? C10 C11 1.509(3) . ? C12 C14 1.502(3) . ? C12 C13 1.518(3) . ? C14 C15 1.373(4) . ? C14 C19 1.393(3) . ? C15 C16 1.391(5) . ? C16 C17 1.378(6) . ? C17 C18 1.344(5) . ? C18 C19 1.388(4) . ? C20 C21 1.505(3) . ? C22 C24 1.512(3) . ? C22 C23 1.524(3) . ? C24 C25 1.383(3) . ? C24 C29 1.387(3) . ? C25 C26 1.396(3) . ? C26 C27 1.372(4) . ? C27 C28 1.379(4) . ? C28 C29 1.390(4) . ? Gd2 O41 2.3451(13) 2_655 ? Gd2 O41 2.3451(13) . ? Gd2 O31 2.3639(13) 2_655 ? Gd2 O31 2.3639(13) . ? Gd2 O2 2.383(2) . ? Gd2 N3 2.6591(15) . ? Gd2 N3 2.6591(15) 2_655 ? Gd2 N4 2.6889(16) 2_655 ? Gd2 N4 2.6889(16) . ? O31 C31 1.248(2) . ? O41 C41 1.255(2) . ? N3 C30 1.478(2) . ? N3 C5 1.490(2) . ? N3 C8 1.492(2) 2_655 ? N4 C40 1.482(2) . ? N4 C7 1.483(2) . ? N4 C6 1.495(2) . ? N31 C31 1.320(2) . ? N31 C32 1.470(2) . ? N41 C41 1.322(2) . ? N41 C42 1.471(3) . ? C5 C6 1.520(3) . ? C7 C8 1.518(3) . ? C8 N3 1.492(2) 2_655 ? C30 C31 1.509(3) . ? C32 C34 1.518(3) . ? C32 C33 1.523(3) . ? C34 C35 1.392(3) . ? C34 C39 1.393(3) . ? C35 C36 1.396(3) . ? C36 C37 1.388(4) . ? C37 C38 1.381(4) . ? C38 C39 1.392(3) . ? C40 C41 1.513(3) . ? C42 C44 1.519(3) . ? C42 C43 1.528(3) . ? C44 C45 1.388(3) . ? C44 C49 1.394(3) . ? C45 C46 1.390(3) . ? C46 C47 1.391(4) . ? C47 C48 1.375(4) . ? C48 C49 1.394(4) . ? N5 O52 1.236(2) . ? N5 O51 1.255(3) . ? N5 O53 1.263(3) . ? N7 O73B 1.177(7) . ? N7 O72A 1.204(5) . ? N7 O72B 1.204(8) . ? N7 O73A 1.252(5) . ? N7 O71A 1.255(4) . ? N7 O71B 1.313(8) . ? N6 O61 1.059(4) . ? N6 O63 1.187(4) . ? N6 O62 1.390(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 O11 Gd1 O11 144.14(9) 2_656 . ? O11 Gd1 O1 72.07(4) 2_656 . ? O11 Gd1 O1 72.07(4) . . ? O11 Gd1 O21 87.68(5) 2_656 . ? O11 Gd1 O21 81.48(5) . . ? O1 Gd1 O21 72.15(4) . . ? O11 Gd1 O21 81.48(5) 2_656 2_656 ? O11 Gd1 O21 87.68(5) . 2_656 ? O1 Gd1 O21 72.15(4) . 2_656 ? O21 Gd1 O21 144.29(7) . 2_656 ? O11 Gd1 N1 65.90(5) 2_656 2_656 ? O11 Gd1 N1 140.99(6) . 2_656 ? O1 Gd1 N1 126.78(4) . 2_656 ? O21 Gd1 N1 74.95(5) . 2_656 ? O21 Gd1 N1 128.81(5) 2_656 2_656 ? O11 Gd1 N1 140.99(6) 2_656 . ? O11 Gd1 N1 65.90(5) . . ? O1 Gd1 N1 126.78(4) . . ? O21 Gd1 N1 128.81(5) . . ? O21 Gd1 N1 74.95(5) 2_656 . ? N1 Gd1 N1 106.44(8) 2_656 . ? O11 Gd1 N2 72.89(6) 2_656 2_656 ? O11 Gd1 N2 132.09(5) . 2_656 ? O1 Gd1 N2 127.63(4) . 2_656 ? O21 Gd1 N2 142.57(5) . 2_656 ? O21 Gd1 N2 65.18(5) 2_656 2_656 ? N1 Gd1 N2 67.98(5) 2_656 2_656 ? N1 Gd1 N2 69.13(5) . 2_656 ? O11 Gd1 N2 132.09(5) 2_656 . ? O11 Gd1 N2 72.89(6) . . ? O1 Gd1 N2 127.63(4) . . ? O21 Gd1 N2 65.18(5) . . ? O21 Gd1 N2 142.57(5) 2_656 . ? N1 Gd1 N2 69.13(5) 2_656 . ? N1 Gd1 N2 67.98(5) . . ? N2 Gd1 N2 104.75(8) 2_656 . ? C11 O11 Gd1 123.97(14) . . ? C21 O21 Gd1 125.94(13) . . ? C10 N1 C1 110.56(17) . . ? C10 N1 C4 110.05(16) . 2_656 ? C1 N1 C4 108.11(17) . 2_656 ? C10 N1 Gd1 105.56(13) . . ? C1 N1 Gd1 112.45(12) . . ? C4 N1 Gd1 110.11(12) 2_656 . ? C20 N2 C2 108.33(16) . . ? C20 N2 C3 110.18(17) . . ? C2 N2 C3 109.61(17) . . ? C20 N2 Gd1 109.84(13) . . ? C2 N2 Gd1 110.99(12) . . ? C3 N2 Gd1 107.88(12) . . ? C11 N11 C12 120.14(18) . . ? C21 N21 C22 120.13(18) . . ? N1 C1 C2 113.81(18) . . ? N2 C2 C1 111.85(17) . . ? N2 C3 C4 112.62(18) . . ? N1 C4 C3 111.14(16) 2_656 . ? N1 C10 C11 110.51(16) . . ? O11 C11 N11 120.9(2) . . ? O11 C11 C10 119.33(18) . . ? N11 C11 C10 119.75(18) . . ? N11 C12 C14 111.24(19) . . ? N11 C12 C13 109.27(18) . . ? C14 C12 C13 112.84(19) . . ? C15 C14 C19 118.8(3) . . ? C15 C14 C12 121.0(2) . . ? C19 C14 C12 120.2(2) . . ? C14 C15 C16 120.1(3) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 120.5(3) . . ? C18 C19 C14 120.3(3) . . ? N2 C20 C21 111.69(17) . . ? O21 C21 N21 121.8(2) . . ? O21 C21 C20 120.76(18) . . ? N21 C21 C20 117.30(18) . . ? N21 C22 C24 112.11(17) . . ? N21 C22 C23 108.74(17) . . ? C24 C22 C23 111.81(18) . . ? C25 C24 C29 119.1(2) . . ? C25 C24 C22 121.18(19) . . ? C29 C24 C22 119.7(2) . . ? C24 C25 C26 120.7(2) . . ? C27 C26 C25 119.4(2) . . ? C26 C27 C28 120.7(2) . . ? C27 C28 C29 119.7(3) . . ? C24 C29 C28 120.4(2) . . ? O41 Gd2 O41 143.92(6) 2_655 . ? O41 Gd2 O31 83.20(5) 2_655 2_655 ? O41 Gd2 O31 86.44(5) . 2_655 ? O41 Gd2 O31 86.44(5) 2_655 . ? O41 Gd2 O31 83.20(5) . . ? O31 Gd2 O31 146.10(6) 2_655 . ? O41 Gd2 O2 71.96(3) 2_655 . ? O41 Gd2 O2 71.96(3) . . ? O31 Gd2 O2 73.05(3) 2_655 . ? O31 Gd2 O2 73.05(3) . . ? O41 Gd2 N3 74.28(5) 2_655 . ? O41 Gd2 N3 130.49(5) . . ? O31 Gd2 N3 139.72(5) 2_655 . ? O31 Gd2 N3 66.00(5) . . ? O2 Gd2 N3 127.65(3) . . ? O41 Gd2 N3 130.49(5) 2_655 2_655 ? O41 Gd2 N3 74.28(5) . 2_655 ? O31 Gd2 N3 66.00(5) 2_655 2_655 ? O31 Gd2 N3 139.72(5) . 2_655 ? O2 Gd2 N3 127.65(3) . 2_655 ? N3 Gd2 N3 104.70(7) . 2_655 ? O41 Gd2 N4 65.70(5) 2_655 2_655 ? O41 Gd2 N4 142.13(5) . 2_655 ? O31 Gd2 N4 72.64(5) 2_655 2_655 ? O31 Gd2 N4 130.85(5) . 2_655 ? O2 Gd2 N4 127.59(3) . 2_655 ? N3 Gd2 N4 67.76(5) . 2_655 ? N3 Gd2 N4 68.47(5) 2_655 2_655 ? O41 Gd2 N4 142.13(5) 2_655 . ? O41 Gd2 N4 65.70(5) . . ? O31 Gd2 N4 130.85(5) 2_655 . ? O31 Gd2 N4 72.64(5) . . ? O2 Gd2 N4 127.59(3) . . ? N3 Gd2 N4 68.47(5) . . ? N3 Gd2 N4 67.76(5) 2_655 . ? N4 Gd2 N4 104.81(7) 2_655 . ? C31 O31 Gd2 123.84(12) . . ? C41 O41 Gd2 125.71(12) . . ? C30 N3 C5 109.97(15) . . ? C30 N3 C8 109.20(14) . 2_655 ? C5 N3 C8 108.88(15) . 2_655 ? C30 N3 Gd2 106.43(11) . . ? C5 N3 Gd2 110.95(11) . . ? C8 N3 Gd2 111.36(11) 2_655 . ? C40 N4 C7 110.69(15) . . ? C40 N4 C6 109.57(15) . . ? C7 N4 C6 108.91(15) . . ? C40 N4 Gd2 106.87(11) . . ? C7 N4 Gd2 110.76(11) . . ? C6 N4 Gd2 110.03(11) . . ? C31 N31 C32 120.38(16) . . ? C41 N41 C42 120.10(17) . . ? N3 C5 C6 114.02(15) . . ? N4 C6 C5 112.03(16) . . ? N4 C7 C8 112.91(16) . . ? N3 C8 C7 111.68(15) 2_655 . ? N3 C30 C31 110.65(14) . . ? O31 C31 N31 121.81(17) . . ? O31 C31 C30 120.21(16) . . ? N31 C31 C30 117.94(16) . . ? N31 C32 C34 110.80(16) . . ? N31 C32 C33 108.67(17) . . ? C34 C32 C33 112.22(17) . . ? C35 C34 C39 119.33(19) . . ? C35 C34 C32 121.05(17) . . ? C39 C34 C32 119.61(19) . . ? C34 C35 C36 120.0(2) . . ? C37 C36 C35 120.1(3) . . ? C38 C37 C36 119.9(2) . . ? C37 C38 C39 120.2(2) . . ? C38 C39 C34 120.4(2) . . ? N4 C40 C41 111.28(15) . . ? O41 C41 N41 121.17(18) . . ? O41 C41 C40 119.75(16) . . ? N41 C41 C40 119.01(17) . . ? N41 C42 C44 111.54(17) . . ? N41 C42 C43 109.24(17) . . ? C44 C42 C43 111.19(18) . . ? C45 C44 C49 118.9(2) . . ? C45 C44 C42 121.12(19) . . ? C49 C44 C42 120.0(2) . . ? C44 C45 C46 120.6(2) . . ? C45 C46 C47 119.8(2) . . ? C48 C47 C46 120.3(3) . . ? C47 C48 C49 119.7(2) . . ? C48 C49 C44 120.7(2) . . ? O52 N5 O51 121.0(2) . . ? O52 N5 O53 120.03(18) . . ? O51 N5 O53 118.95(19) . . ? O73B N7 O72A 82.2(4) . . ? O73B N7 O72B 116.8(5) . . ? O72A N7 O72B 36.6(4) . . ? O73B N7 O73A 36.7(4) . . ? O72A N7 O73A 118.0(4) . . ? O72B N7 O73A 153.5(5) . . ? O73B N7 O71A 155.9(5) . . ? O72A N7 O71A 121.8(3) . . ? O72B N7 O71A 87.1(4) . . ? O73A N7 O71A 119.3(3) . . ? O73B N7 O71B 120.6(5) . . ? O72A N7 O71B 157.3(5) . . ? O72B N7 O71B 121.3(5) . . ? O73A N7 O71B 84.6(4) . . ? O71A N7 O71B 35.5(3) . . ? O61 N6 O63 131.2(4) . . ? O61 N6 O62 117.1(3) . . ? O63 N6 O62 111.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.655 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.055 #=============================================END data_8a _database_code_CSD 182448 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Tb N8 O5 3+,3(C F3 O3 S 1-),3(H2 O)' _chemical_formula_sum 'C51 H72 F9 N8 O17 S3 Tb' _chemical_formula_weight 1495.27 _chemical_absolute_configuration ad _chemical_optical_rotation ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.613(3) _cell_length_b 11.728(2) _cell_length_c 19.240(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.94(1) _cell_angle_gamma 90.00 _cell_volume 3226(1) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9172 _cell_measurement_theta_min 4.33 _cell_measurement_theta_max 63.86 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured ' _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 6 sets of \w scans; each set at different \f and/or 2\q angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. Merging of Friedel pairs yields 7385 independent reflections, of which 7056 with I>2\s(I). ; _diffrn_ambient_temperature 120(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 'SMART 6000 CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36411 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.00 _reflns_number_total 14049 _reflns_number_gt 13231 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.902 _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. One triflate ligand is disordered. The O(21), O(22), O(23) atoms were refined in two positions with occupancies 78.1(8)% (A) and 21.9% (B), with the ADP of opposite atoms constrained to equality. Large ADP of the fluorine atoms also indicate a disorder, which we could not rationalise (several models of rotation around the S(2)---C(1S) bond, libration around the S(2) atom or the midpoint of the S(2)---C(2S) bond were tried without success). Methyl groups were refined as rigid bodies, all other H atoms were treated as 'riding', with U(iso) refined for N- and O-bound hydrogens, related to the U(eq) of the carrying atom for the rest. ; _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^)+(0.0466P)^2^+0.6667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.030(6) _refine_ls_number_reflns 14049 _refine_ls_number_parameters 827 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.007 _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 Tb Tb 0.303874(8) 0.699338(16) 0.718605(7) 0.01492(5) Uani 1 1 d . . . O1 O 0.17311(17) 0.6465(2) 0.76517(14) 0.0213(5) Uani 1 1 d . . . O2 O 0.38679(17) 0.6590(2) 0.83311(13) 0.0205(5) Uani 1 1 d . . . O3 O 0.43593(17) 0.6251(2) 0.68240(13) 0.0204(5) Uani 1 1 d . . . O4 O 0.22506(17) 0.6204(2) 0.61173(13) 0.0186(5) Uani 1 1 d . . . O5 O 0.30220(18) 0.4910(2) 0.73347(14) 0.0242(6) Uani 1 1 d . . . H051 H 0.3456 0.4600 0.7581 0.028(12) Uiso 1 1 d R . . H052 H 0.2596 0.4607 0.7467 0.060(19) Uiso 1 1 d R . . N1 N 0.1590(2) 0.8323(2) 0.67467(15) 0.0174(6) Uani 1 1 d . . . N2 N 0.2863(2) 0.8559(3) 0.81528(15) 0.0189(6) Uani 1 1 d . . . N3 N 0.4489(2) 0.8389(3) 0.74452(16) 0.0182(6) Uani 1 1 d . . . N4 N 0.3222(2) 0.8188(3) 0.60420(16) 0.0182(6) Uani 1 1 d . . . N11 N 0.0222(2) 0.6640(3) 0.77232(18) 0.0250(7) Uani 1 1 d . . . H11 H -0.0323 0.6957 0.7546 0.056(14) Uiso 1 1 d R . . N21 N 0.4201(2) 0.6710(3) 0.95208(16) 0.0245(8) Uani 1 1 d . . . H21 H 0.4131 0.7090 0.9901 0.025(10) Uiso 1 1 d R . . N31 N 0.5892(2) 0.6242(3) 0.67983(17) 0.0245(7) Uani 1 1 d . . . H31 H 0.6440 0.6576 0.6927 0.026(12) Uiso 1 1 d R . . N41 N 0.1867(2) 0.6030(3) 0.49268(16) 0.0215(6) Uani 1 1 d . . . H41 H 0.1935 0.6282 0.4510 0.018(10) Uiso 1 1 d R . . C1 C 0.1594(2) 0.9344(3) 0.7219(2) 0.0212(7) Uani 1 1 d . . . H1A H 0.0955 0.9665 0.7139 0.025 Uiso 1 1 d R . . H1B H 0.2010 0.9935 0.7086 0.025 Uiso 1 1 d R . . C2 C 0.1917(2) 0.9079(3) 0.7998(2) 0.0234(8) Uani 1 1 d . . . H2A H 0.1923 0.9790 0.8275 0.028 Uiso 1 1 d R . . H2B H 0.1468 0.8546 0.8147 0.028 Uiso 1 1 d R . . C3 C 0.3562(3) 0.9482(3) 0.8157(2) 0.0230(7) Uani 1 1 d . . . H3A H 0.3611 0.9934 0.8597 0.028 Uiso 1 1 d R . . H3B H 0.3336 0.9996 0.7749 0.028 Uiso 1 1 d R . . C4 C 0.4528(3) 0.9040(3) 0.8111(2) 0.0227(7) Uani 1 1 d . . . H4A H 0.4965 0.9689 0.8128 0.027 Uiso 1 1 d R . . H4B H 0.4766 0.8541 0.8524 0.027 Uiso 1 1 d R . . C5 C 0.4485(3) 0.9224(3) 0.6862(2) 0.0230(8) Uani 1 1 d . . . H5A H 0.5124 0.9534 0.6902 0.028 Uiso 1 1 d R . . H5B H 0.4066 0.9867 0.6918 0.028 Uiso 1 1 d R . . C6 C 0.4163(2) 0.8702(3) 0.61253(19) 0.0206(7) Uani 1 1 d . . . H6A H 0.4149 0.9300 0.5760 0.025 Uiso 1 1 d R . . H6B H 0.4614 0.8110 0.6049 0.025 Uiso 1 1 d R . . C7 C 0.2509(2) 0.9110(3) 0.5904(2) 0.0206(7) Uani 1 1 d . . . H7A H 0.2449 0.9384 0.5410 0.025 Uiso 1 1 d R . . H7B H 0.2727 0.9758 0.6226 0.025 Uiso 1 1 d R . . C8 C 0.1550(2) 0.8730(3) 0.60128(19) 0.0199(7) Uani 1 1 d . . . H8A H 0.1108 0.9378 0.5913 0.024 Uiso 1 1 d R . . H8B H 0.1312 0.8112 0.5673 0.024 Uiso 1 1 d R . . C10 C 0.0757(2) 0.7623(3) 0.67709(19) 0.0198(7) Uani 1 1 d . . . H10A H 0.0598 0.7150 0.6337 0.024 Uiso 1 1 d R . . H10B H 0.0218 0.8128 0.6786 0.024 Uiso 1 1 d R . . C11 C 0.0940(2) 0.6855(4) 0.74207(17) 0.0187(8) Uani 1 1 d . . . C12 C 0.0305(3) 0.5888(4) 0.8346(2) 0.0343(10) Uani 1 1 d . . . H12A H 0.0684 0.5206 0.8271 0.041 Uiso 1 1 calc R . . C13 C -0.0678(3) 0.5492(5) 0.8382(3) 0.0448(12) Uani 1 1 d . . . H13A H -0.0969 0.5120 0.7934 0.067 Uiso 1 1 d R . . H13B H -0.1055 0.6152 0.8461 0.067 Uiso 1 1 d R . . H13C H -0.0644 0.4950 0.8774 0.067 Uiso 1 1 d R . . C14 C 0.0784(3) 0.6477(5) 0.9011(3) 0.0397(12) Uani 1 1 d . . . C15 C 0.0569(4) 0.7575(6) 0.9185(3) 0.0540(15) Uani 1 1 d . . . H15A H 0.0099 0.7982 0.8865 0.065 Uiso 1 1 d R . . C16 C 0.1007(5) 0.8073(8) 0.9803(3) 0.080(2) Uani 1 1 d . . . H16A H 0.0849 0.8825 0.9918 0.097 Uiso 1 1 d R . . C17 C 0.1710(6) 0.7503(11) 1.0274(4) 0.090(3) Uani 1 1 d . . . H17A H 0.2016 0.7852 1.0705 0.108 Uiso 1 1 d R . . C18 C 0.1951(5) 0.6413(9) 1.0121(4) 0.076(2) Uani 1 1 d . . . H18A H 0.2420 0.6012 1.0444 0.091 Uiso 1 1 d R . . C19 C 0.1502(4) 0.5899(6) 0.9492(3) 0.0555(15) Uani 1 1 d . . . H19A H 0.1670 0.5152 0.9375 0.067 Uiso 1 1 d R . . C20 C 0.3031(3) 0.7982(3) 0.8855(2) 0.0234(8) Uani 1 1 d . . . H20A H 0.2436 0.7656 0.8935 0.028 Uiso 1 1 d R . . H20B H 0.3255 0.8546 0.9235 0.028 Uiso 1 1 d R . . C21 C 0.3741(2) 0.7052(5) 0.88879(16) 0.0196(6) Uani 1 1 d . . . C22 C 0.4833(3) 0.5714(3) 0.96001(19) 0.0240(8) Uani 1 1 d . . . H22A H 0.4661 0.5246 0.9158 0.029 Uiso 1 1 calc R . . C23 C 0.4657(3) 0.4993(4) 1.0216(2) 0.0328(9) Uani 1 1 d . . . H23A H 0.3989 0.4812 1.0142 0.049 Uiso 1 1 d R . . H23B H 0.4849 0.5417 1.0661 0.049 Uiso 1 1 d R . . H23C H 0.5017 0.4283 1.0241 0.049 Uiso 1 1 d R . . C29 C 0.6349(4) 0.5661(6) 0.9217(4) 0.078(2) Uani 1 1 d . . . H29A H 0.6063 0.5174 0.8839 0.093 Uiso 1 1 d R . . C24 C 0.5838(3) 0.6082(4) 0.9672(2) 0.0294(8) Uani 1 1 d . . . C25 C 0.6255(3) 0.6830(7) 1.0184(4) 0.073(2) Uani 1 1 d . . . H25A H 0.5902 0.7143 1.0501 0.087 Uiso 1 1 d R . . C26 C 0.7187(4) 0.7129(9) 1.0252(5) 0.096(3) Uani 1 1 d . . . H26A H 0.7462 0.7664 1.0605 0.115 Uiso 1 1 d R . . C27 C 0.7707(4) 0.6677(6) 0.9814(4) 0.076(2) Uani 1 1 d . . . H27A H 0.8349 0.6865 0.9864 0.091 Uiso 1 1 d R . . C28 C 0.7287(5) 0.5930(8) 0.9310(5) 0.106(3) Uani 1 1 d . . . H28A H 0.7642 0.5599 0.9001 0.128 Uiso 1 1 d R . . C30 C 0.5329(2) 0.7649(3) 0.7530(2) 0.0230(8) Uani 1 1 d . . . H30A H 0.5485 0.7355 0.8023 0.028 Uiso 1 1 d R . . H30B H 0.5867 0.8104 0.7447 0.028 Uiso 1 1 d R . . C31 C 0.5164(2) 0.6664(3) 0.70198(19) 0.0192(8) Uani 1 1 d . . . C32 C 0.5806(3) 0.5221(3) 0.6340(2) 0.0250(8) Uani 1 1 d . . . H32A H 0.5426 0.4639 0.6535 0.030 Uiso 1 1 calc R . . C33 C 0.6786(3) 0.4730(4) 0.6374(3) 0.0374(10) Uani 1 1 d . . . H33A H 0.7065 0.4511 0.6863 0.056 Uiso 1 1 d R . . H33B H 0.7180 0.5305 0.6210 0.056 Uiso 1 1 d R . . H33C H 0.6738 0.4057 0.6066 0.056 Uiso 1 1 d R . . C34 C 0.5306(3) 0.5508(3) 0.5586(2) 0.0236(7) Uani 1 1 d . . . C35 C 0.5613(3) 0.6392(3) 0.5198(2) 0.0289(9) Uani 1 1 d . . . H35A H 0.6142 0.6836 0.5407 0.035 Uiso 1 1 d R . . C36 C 0.5140(3) 0.6626(4) 0.4509(2) 0.0345(10) Uani 1 1 d . . . H36A H 0.5348 0.7225 0.4247 0.041 Uiso 1 1 d R . . C37 C 0.4365(3) 0.5994(4) 0.4201(2) 0.0353(10) Uani 1 1 d . . . H37A H 0.4051 0.6154 0.3728 0.042 Uiso 1 1 d R . . C38 C 0.4055(3) 0.5125(4) 0.4568(2) 0.0317(9) Uani 1 1 d . . . H38A H 0.3518 0.4697 0.4353 0.038 Uiso 1 1 d R . . C39 C 0.4529(3) 0.4883(3) 0.5264(2) 0.0265(8) Uani 1 1 d . . . H39A H 0.4314 0.4279 0.5518 0.032 Uiso 1 1 d R . . C40 C 0.3075(2) 0.7380(3) 0.54371(19) 0.0212(7) Uani 1 1 d . . . H40A H 0.3673 0.6995 0.5419 0.025 Uiso 1 1 d R . . H40B H 0.2870 0.7806 0.4987 0.025 Uiso 1 1 d R . . C41 C 0.2348(2) 0.6500(3) 0.55077(18) 0.0182(7) Uani 1 1 d . . . C42 C 0.1209(3) 0.5083(3) 0.4964(2) 0.0232(7) Uani 1 1 d . . . H42A H 0.1511 0.4555 0.5352 0.028 Uiso 1 1 calc R . . C43 C 0.1053(3) 0.4430(4) 0.4266(2) 0.0300(9) Uani 1 1 d . . . H43A H 0.1656 0.4187 0.4169 0.045 Uiso 1 1 d R . . H43B H 0.0734 0.4924 0.3880 0.045 Uiso 1 1 d R . . H43C H 0.0665 0.3759 0.4299 0.045 Uiso 1 1 d R . . C44 C 0.0312(3) 0.5515(3) 0.5140(2) 0.0234(7) Uani 1 1 d . . . C45 C -0.0205(3) 0.6377(3) 0.4730(2) 0.0295(9) Uani 1 1 d . . . H45A H 0.0019 0.6709 0.4347 0.035 Uiso 1 1 d R . . C46 C -0.1041(3) 0.6744(3) 0.4883(3) 0.0382(11) Uani 1 1 d . . . H46A H -0.1391 0.7326 0.4602 0.046 Uiso 1 1 d R . . C47 C -0.1370(3) 0.6267(4) 0.5447(3) 0.0402(11) Uani 1 1 d . . . H47A H -0.1942 0.6525 0.5552 0.048 Uiso 1 1 d R . . C48 C -0.0866(3) 0.5414(4) 0.5854(3) 0.0384(10) Uani 1 1 d . . . H48A H -0.1090 0.5083 0.6238 0.046 Uiso 1 1 d R . . C49 C -0.0026(3) 0.5041(4) 0.5693(2) 0.0297(9) Uani 1 1 d . . . H49A H 0.0320 0.4454 0.5970 0.036 Uiso 1 1 d R . . S1 S 0.50997(8) 0.28471(9) 0.83473(6) 0.0341(2) Uani 1 1 d . . . O11 O 0.4700(2) 0.3927(3) 0.81005(19) 0.0438(8) Uani 1 1 d . . . O12 O 0.5586(2) 0.2836(3) 0.90790(16) 0.0420(8) Uani 1 1 d . . . O13 O 0.4508(3) 0.1883(4) 0.81282(18) 0.0569(9) Uani 1 1 d . . . C1S C 0.6040(5) 0.2665(5) 0.7861(3) 0.0511(14) Uani 1 1 d . . . F11 F 0.6476(3) 0.1688(4) 0.8023(2) 0.0968(16) Uani 1 1 d . . . F12 F 0.5695(3) 0.2686(3) 0.71644(17) 0.0759(12) Uani 1 1 d . . . F13 F 0.6657(3) 0.3503(4) 0.80123(19) 0.0694(10) Uani 1 1 d . . . S2 S 0.07184(9) 0.28389(12) 0.73752(8) 0.0464(3) Uani 1 1 d D . . O21A O -0.0192(4) 0.3274(5) 0.7054(3) 0.0721(18) Uani 0.781(8) 1 d PD A 1 O22A O 0.1352(4) 0.3750(5) 0.7602(4) 0.085(2) Uani 0.781(8) 1 d PD A 1 O23A O 0.1067(3) 0.1992(5) 0.6971(2) 0.0561(13) Uani 0.781(8) 1 d PD A 1 O21B O 0.1642(9) 0.2100(16) 0.7566(8) 0.0721(18) Uani 0.22 1 d PD A 2 O22B O 0.0081(9) 0.2239(14) 0.6869(7) 0.085(2) Uani 0.22 1 d PD A 2 O23B O 0.0896(12) 0.3919(9) 0.7467(9) 0.0561(13) Uani 0.22 1 d PD A 2 C2S C 0.0455(5) 0.2226(6) 0.8166(4) 0.082(3) Uani 1 1 d D A . F21 F -0.0072(6) 0.1353(5) 0.8031(4) 0.163(3) Uani 1 1 d D . . F22 F 0.0330(6) 0.2907(4) 0.8634(3) 0.154(3) Uani 1 1 d D . . F23 F 0.1241(7) 0.1665(6) 0.8490(3) 0.237(6) Uani 1 1 d D . . S3 S 0.79736(7) 0.86745(12) 0.73995(6) 0.0378(3) Uani 1 1 d . . . O31 O 0.7470(3) 0.9498(5) 0.6943(2) 0.0890(19) Uani 1 1 d . . . O32 O 0.7548(3) 0.7567(4) 0.7415(3) 0.0785(15) Uani 1 1 d . . . O33 O 0.8958(2) 0.8588(3) 0.74047(17) 0.0365(7) Uani 1 1 d . . . C3S C 0.7939(3) 0.9221(4) 0.8277(3) 0.0389(10) Uani 1 1 d . . . F31 F 0.8300(3) 1.0251(4) 0.8353(2) 0.0886(14) Uani 1 1 d . . . F32 F 0.8423(3) 0.8625(5) 0.87848(18) 0.0885(15) Uani 1 1 d . . . F33 F 0.70636(18) 0.9323(3) 0.83676(16) 0.0440(7) Uani 1 1 d . . . O1W O 0.2991(2) 0.3523(3) 0.59674(18) 0.0407(7) Uani 1 1 d . . . H1W1 H 0.3008 0.3004 0.6218 0.061 Uiso 1 1 d R . . H2W1 H 0.3002 0.4052 0.6261 0.11(3) Uiso 1 1 d R . . O2W O 0.3003(3) 0.1693(3) 0.69266(19) 0.0417(8) Uani 1 1 d . . . H1W2 H 0.2465 0.1871 0.6963 0.08(2) Uiso 1 1 d R . . H2W2 H 0.3246 0.1893 0.7328 0.09(2) Uiso 1 1 d R . . O3W O -0.1915(3) 0.1847(5) 0.64585(17) 0.0585(12) Uani 1 1 d . . . H1W3 H -0.1332 0.2055 0.6629 0.12(3) Uiso 1 1 d R . . H2W3 H -0.2120 0.1287 0.6695 0.09(3) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb 0.01479(7) 0.01662(7) 0.01295(7) 0.00008(8) 0.00193(4) 0.00081(9) O1 0.0174(11) 0.0272(13) 0.0205(13) 0.0046(11) 0.0066(10) 0.0016(10) O2 0.0223(12) 0.0235(12) 0.0142(12) 0.0009(9) 0.0001(10) 0.0046(9) O3 0.0163(11) 0.0249(13) 0.0197(12) -0.0019(10) 0.0034(10) 0.0016(10) O4 0.0174(11) 0.0222(12) 0.0160(12) -0.0010(10) 0.0029(9) -0.0036(10) O5 0.0253(14) 0.0206(13) 0.0257(13) 0.0035(11) 0.0028(11) 0.0023(11) N1 0.0159(14) 0.0184(14) 0.0170(14) 0.0009(11) 0.0017(11) 0.0041(11) N2 0.0189(14) 0.0220(15) 0.0143(14) -0.0037(11) -0.0003(11) 0.0010(12) N3 0.0161(14) 0.0185(14) 0.0190(15) -0.0024(12) 0.0014(11) 0.0001(11) N4 0.0174(14) 0.0198(14) 0.0171(15) 0.0018(11) 0.0034(12) -0.0012(11) N11 0.0168(14) 0.0307(18) 0.0295(17) 0.0061(12) 0.0093(12) 0.0023(11) N21 0.0263(14) 0.030(2) 0.0158(14) 0.0007(11) 0.0015(11) 0.0040(12) N31 0.0177(14) 0.0297(17) 0.0266(17) -0.0067(13) 0.0057(12) -0.0012(13) N41 0.0218(14) 0.0248(16) 0.0161(15) 0.0002(12) 0.0000(12) -0.0038(13) C1 0.0206(17) 0.0154(16) 0.0271(19) -0.0030(14) 0.0038(15) 0.0054(14) C2 0.0215(18) 0.0240(18) 0.0245(18) -0.0069(15) 0.0042(15) 0.0046(14) C3 0.0227(17) 0.0214(17) 0.0228(18) -0.0041(14) -0.0006(14) -0.0012(14) C4 0.0230(18) 0.0234(18) 0.0198(18) -0.0062(14) 0.0003(14) -0.0048(14) C5 0.0217(17) 0.0219(18) 0.0249(19) -0.0004(15) 0.0035(15) -0.0078(14) C6 0.0180(16) 0.0237(17) 0.0204(17) 0.0009(14) 0.0049(14) -0.0069(14) C7 0.0194(17) 0.0214(17) 0.0197(18) 0.0062(14) 0.0012(14) 0.0021(14) C8 0.0178(16) 0.0220(17) 0.0182(17) 0.0074(14) -0.0001(13) 0.0049(14) C10 0.0157(16) 0.0247(19) 0.0194(17) 0.0008(14) 0.0047(13) 0.0005(14) C11 0.0212(14) 0.016(2) 0.0196(14) 0.0010(15) 0.0063(11) 0.0009(16) C12 0.030(2) 0.039(2) 0.038(2) 0.0167(19) 0.0175(18) 0.0072(18) C13 0.037(2) 0.051(3) 0.053(3) 0.019(2) 0.025(2) 0.002(2) C14 0.032(2) 0.066(3) 0.025(2) 0.018(2) 0.0159(19) 0.007(2) C15 0.047(3) 0.086(4) 0.034(3) -0.010(3) 0.019(2) 0.016(3) C16 0.081(5) 0.124(7) 0.042(3) -0.033(4) 0.027(3) 0.009(4) C17 0.073(5) 0.170(10) 0.027(3) -0.010(4) 0.012(3) -0.012(6) C18 0.060(4) 0.137(7) 0.029(3) 0.034(4) 0.003(3) 0.009(4) C19 0.047(3) 0.080(4) 0.044(3) 0.036(3) 0.018(2) 0.010(3) C20 0.0244(18) 0.027(2) 0.0181(18) -0.0012(14) 0.0040(14) 0.0042(15) C21 0.0189(13) 0.0209(15) 0.0187(14) -0.001(2) 0.0034(11) -0.006(2) C22 0.0300(19) 0.0240(18) 0.0149(17) 0.0022(14) -0.0022(14) 0.0055(15) C23 0.036(2) 0.032(2) 0.028(2) 0.0095(17) 0.0008(17) 0.0033(18) C29 0.064(4) 0.086(5) 0.100(5) -0.053(4) 0.055(4) -0.035(4) C24 0.030(2) 0.028(2) 0.029(2) 0.0016(17) 0.0057(17) 0.0060(17) C25 0.030(2) 0.087(5) 0.095(4) -0.052(4) 0.002(2) -0.001(3) C26 0.037(3) 0.108(7) 0.136(7) -0.074(6) 0.006(3) -0.011(4) C27 0.042(3) 0.089(6) 0.102(5) -0.008(4) 0.029(3) -0.014(3) C28 0.068(5) 0.116(7) 0.157(9) -0.067(7) 0.075(5) -0.032(5) C30 0.0165(16) 0.029(2) 0.0217(19) -0.0045(15) 0.0007(14) 0.0022(15) C31 0.0167(15) 0.0228(19) 0.0177(17) 0.0029(12) 0.0025(13) 0.0020(12) C32 0.0230(18) 0.0252(18) 0.029(2) -0.0006(15) 0.0099(15) 0.0038(15) C33 0.033(2) 0.044(3) 0.038(2) 0.003(2) 0.0127(19) 0.0154(19) C34 0.0261(18) 0.0224(17) 0.0248(19) -0.0054(15) 0.0110(15) 0.0034(15) C35 0.030(2) 0.026(2) 0.033(2) -0.0038(17) 0.0098(17) -0.0023(16) C36 0.047(2) 0.029(2) 0.031(2) 0.0017(16) 0.0146(19) 0.0033(17) C37 0.045(2) 0.038(2) 0.025(2) -0.0024(18) 0.0102(19) 0.014(2) C38 0.028(2) 0.033(2) 0.035(2) -0.0136(18) 0.0097(17) 0.0046(17) C39 0.0275(19) 0.0244(18) 0.030(2) -0.0053(16) 0.0125(16) 0.0011(15) C40 0.0208(17) 0.0261(17) 0.0167(17) -0.0010(13) 0.0041(13) -0.0026(13) C41 0.0197(17) 0.0213(15) 0.0131(16) 0.0012(13) 0.0026(13) 0.0013(14) C42 0.0219(17) 0.0255(18) 0.0197(18) -0.0012(14) -0.0014(14) -0.0040(15) C43 0.026(2) 0.033(2) 0.030(2) -0.0100(17) 0.0025(16) -0.0071(18) C44 0.0229(18) 0.0227(17) 0.0231(19) -0.0045(15) 0.0017(15) -0.0071(14) C45 0.032(2) 0.023(2) 0.032(2) -0.0029(16) 0.0025(17) -0.0035(16) C46 0.032(2) 0.030(3) 0.050(3) -0.0044(18) 0.0031(19) -0.0018(16) C47 0.029(2) 0.034(2) 0.058(3) -0.009(2) 0.012(2) -0.0022(18) C48 0.028(2) 0.038(2) 0.051(3) -0.006(2) 0.014(2) -0.0096(19) C49 0.0273(19) 0.031(2) 0.030(2) 0.0027(17) 0.0032(16) -0.0051(16) S1 0.0443(6) 0.0265(5) 0.0272(5) 0.0022(4) -0.0027(4) 0.0028(4) O11 0.0483(19) 0.0305(16) 0.0445(19) -0.0019(14) -0.0087(15) 0.0104(14) O12 0.0461(18) 0.053(2) 0.0235(15) 0.0113(14) 0.0001(14) -0.0028(16) O13 0.076(2) 0.036(2) 0.0484(18) 0.005(2) -0.0113(16) -0.014(2) C1S 0.070(4) 0.046(3) 0.039(3) 0.004(2) 0.015(3) 0.015(3) F11 0.123(3) 0.081(4) 0.095(3) 0.014(2) 0.041(3) 0.067(3) F12 0.139(4) 0.062(2) 0.0308(17) -0.0099(15) 0.027(2) 0.000(2) F13 0.067(2) 0.094(3) 0.054(2) 0.000(2) 0.0268(18) -0.004(2) S2 0.0480(7) 0.0406(6) 0.0541(8) -0.0106(6) 0.0189(6) -0.0049(6) O21A 0.071(4) 0.081(4) 0.065(4) 0.019(3) 0.014(3) 0.037(3) O22A 0.055(3) 0.070(4) 0.145(6) -0.053(4) 0.058(4) -0.032(3) O23A 0.067(3) 0.039(2) 0.067(3) -0.006(3) 0.023(2) 0.010(3) O21B 0.071(4) 0.081(4) 0.065(4) 0.019(3) 0.014(3) 0.037(3) O22B 0.055(3) 0.070(4) 0.145(6) -0.053(4) 0.058(4) -0.032(3) O23B 0.067(3) 0.039(2) 0.067(3) -0.006(3) 0.023(2) 0.010(3) C2S 0.096(5) 0.085(7) 0.054(4) 0.033(4) -0.012(3) -0.019(4) F21 0.247(8) 0.078(4) 0.197(7) 0.024(4) 0.121(7) -0.052(5) F22 0.332(10) 0.061(3) 0.118(4) 0.038(3) 0.160(6) 0.072(4) F23 0.415(13) 0.145(7) 0.095(4) -0.036(4) -0.081(6) 0.181(8) S3 0.0231(5) 0.0592(7) 0.0311(5) -0.0069(5) 0.0057(4) 0.0096(5) O31 0.083(3) 0.150(5) 0.039(2) 0.030(3) 0.025(2) 0.078(3) O32 0.038(2) 0.096(3) 0.104(4) -0.063(3) 0.021(2) -0.008(2) O33 0.0277(15) 0.0439(18) 0.0414(18) 0.0088(14) 0.0149(13) 0.0090(14) C3S 0.032(2) 0.046(3) 0.040(3) -0.001(2) 0.010(2) 0.009(2) F31 0.070(2) 0.093(3) 0.117(3) -0.063(3) 0.052(2) -0.038(2) F32 0.073(2) 0.152(4) 0.0403(19) 0.019(2) 0.0111(17) 0.056(3) F33 0.0325(13) 0.0543(17) 0.0500(17) -0.0115(14) 0.0199(12) 0.0020(12) O1W 0.055(2) 0.0317(16) 0.0379(18) 0.0019(14) 0.0152(15) -0.0033(15) O2W 0.053(2) 0.0304(19) 0.0400(19) 0.0057(12) 0.0053(15) 0.0027(13) O3W 0.056(2) 0.090(4) 0.0266(15) -0.011(2) 0.0002(14) 0.022(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 Tb O4 2.331(2) . ? Tb O2 2.333(2) . ? Tb O3 2.350(2) . ? Tb O1 2.355(2) . ? Tb O5 2.461(3) . ? Tb N1 2.624(3) . ? Tb N3 2.642(3) . ? Tb N2 2.664(3) . ? Tb N4 2.669(3) . ? O1 C11 1.237(4) . ? O2 C21 1.248(4) . ? O3 C31 1.255(4) . ? O4 C41 1.259(4) . ? N1 C10 1.478(4) . ? N1 C8 1.480(4) . ? N1 C1 1.502(4) . ? N2 C2 1.484(4) . ? N2 C20 1.485(5) . ? N2 C3 1.487(5) . ? N3 C4 1.483(5) . ? N3 C30 1.485(4) . ? N3 C5 1.490(5) . ? N4 C6 1.479(4) . ? N4 C40 1.482(5) . ? N4 C7 1.486(4) . ? N11 C11 1.325(4) . ? N11 C12 1.473(5) . ? N21 C21 1.325(5) . ? N21 C22 1.478(5) . ? N31 C31 1.321(5) . ? N31 C32 1.477(5) . ? N41 C41 1.313(5) . ? N41 C42 1.480(5) . ? C1 C2 1.507(5) . ? C3 C4 1.523(5) . ? C5 C6 1.526(5) . ? C7 C8 1.525(5) . ? C10 C11 1.519(5) . ? C12 C14 1.496(7) . ? C12 C13 1.525(6) . ? C14 C15 1.382(8) . ? C14 C19 1.419(7) . ? C15 C16 1.360(9) . ? C16 C17 1.392(12) . ? C17 C18 1.374(12) . ? C18 C19 1.388(11) . ? C20 C21 1.498(6) . ? C22 C24 1.509(6) . ? C22 C23 1.520(5) . ? C29 C24 1.358(7) . ? C29 C28 1.380(9) . ? C24 C25 1.364(7) . ? C25 C26 1.387(8) . ? C26 C27 1.353(9) . ? C27 C28 1.356(11) . ? C30 C31 1.503(5) . ? C32 C34 1.521(5) . ? C32 C33 1.532(5) . ? C34 C39 1.387(5) . ? C34 C35 1.404(6) . ? C35 C36 1.390(6) . ? C36 C37 1.381(7) . ? C37 C38 1.369(7) . ? C38 C39 1.403(6) . ? C40 C41 1.507(5) . ? C42 C44 1.508(5) . ? C42 C43 1.521(5) . ? C44 C49 1.380(6) . ? C44 C45 1.402(6) . ? C45 C46 1.384(6) . ? C46 C47 1.393(7) . ? C47 C48 1.384(7) . ? C48 C49 1.397(6) . ? S1 O13 1.433(4) . ? S1 O11 1.434(3) . ? S1 O12 1.440(3) . ? S1 C1S 1.827(6) . ? C1S F11 1.316(6) . ? C1S F13 1.326(8) . ? C1S F12 1.332(7) . ? S2 O23B 1.298(10) . ? S2 O22B 1.391(10) . ? S2 O23A 1.419(5) . ? S2 O22A 1.422(5) . ? S2 O21A 1.439(5) . ? S2 O21B 1.581(10) . ? S2 C2S 1.794(7) . ? C2S F22 1.246(8) . ? C2S F21 1.275(8) . ? C2S F23 1.359(8) . ? S3 O31 1.406(4) . ? S3 O33 1.440(3) . ? S3 O32 1.443(5) . ? S3 C3S 1.816(5) . ? C3S F32 1.287(6) . ? C3S F31 1.314(6) . ? C3S F33 1.332(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 O4 Tb O2 144.89(9) . . ? O4 Tb O3 82.97(8) . . ? O2 Tb O3 84.66(9) . . ? O4 Tb O1 86.53(9) . . ? O2 Tb O1 83.75(9) . . ? O3 Tb O1 142.76(10) . . ? O4 Tb O5 72.14(9) . . ? O2 Tb O5 72.81(9) . . ? O3 Tb O5 72.26(9) . . ? O1 Tb O5 70.51(9) . . ? O4 Tb N1 74.53(9) . . ? O2 Tb N1 130.65(9) . . ? O3 Tb N1 141.42(9) . . ? O1 Tb N1 67.34(9) . . ? O5 Tb N1 126.92(9) . . ? O4 Tb N3 130.02(9) . . ? O2 Tb N3 73.01(9) . . ? O3 Tb N3 67.02(9) . . ? O1 Tb N3 140.66(9) . . ? O5 Tb N3 128.31(9) . . ? N1 Tb N3 104.76(10) . . ? O4 Tb N2 142.04(9) . . ? O2 Tb N2 65.58(9) . . ? O3 Tb N2 131.76(9) . . ? O1 Tb N2 73.29(9) . . ? O5 Tb N2 126.76(9) . . ? N1 Tb N2 68.13(9) . . ? N3 Tb N2 68.33(9) . . ? O4 Tb N4 66.19(9) . . ? O2 Tb N4 139.85(9) . . ? O3 Tb N4 73.83(9) . . ? O1 Tb N4 132.79(9) . . ? O5 Tb N4 128.49(9) . . ? N1 Tb N4 68.54(9) . . ? N3 Tb N4 67.49(9) . . ? N2 Tb N4 104.75(9) . . ? C11 O1 Tb 122.5(2) . . ? C21 O2 Tb 125.6(2) . . ? C31 O3 Tb 123.0(2) . . ? C41 O4 Tb 125.6(2) . . ? C10 N1 C8 109.8(3) . . ? C10 N1 C1 108.9(3) . . ? C8 N1 C1 108.3(3) . . ? C10 N1 Tb 106.0(2) . . ? C8 N1 Tb 111.6(2) . . ? C1 N1 Tb 112.1(2) . . ? C2 N2 C20 110.0(3) . . ? C2 N2 C3 108.2(3) . . ? C20 N2 C3 110.1(3) . . ? C2 N2 Tb 111.3(2) . . ? C20 N2 Tb 107.4(2) . . ? C3 N2 Tb 109.9(2) . . ? C4 N3 C30 108.9(3) . . ? C4 N3 C5 107.8(3) . . ? C30 N3 C5 110.0(3) . . ? C4 N3 Tb 111.6(2) . . ? C30 N3 Tb 105.7(2) . . ? C5 N3 Tb 112.8(2) . . ? C6 N4 C40 109.0(3) . . ? C6 N4 C7 109.0(3) . . ? C40 N4 C7 110.1(3) . . ? C6 N4 Tb 111.9(2) . . ? C40 N4 Tb 106.8(2) . . ? C7 N4 Tb 110.0(2) . . ? C11 N11 C12 122.1(3) . . ? C21 N21 C22 121.4(3) . . ? C31 N31 C32 121.5(3) . . ? C41 N41 C42 120.9(3) . . ? N1 C1 C2 113.5(3) . . ? N2 C2 C1 111.8(3) . . ? N2 C3 C4 113.3(3) . . ? N3 C4 C3 110.8(3) . . ? N3 C5 C6 112.8(3) . . ? N4 C6 C5 111.4(3) . . ? N4 C7 C8 113.1(3) . . ? N1 C8 C7 111.6(3) . . ? N1 C10 C11 110.4(3) . . ? O1 C11 N11 122.5(3) . . ? O1 C11 C10 120.5(3) . . ? N11 C11 C10 117.0(3) . . ? N11 C12 C14 111.4(4) . . ? N11 C12 C13 107.4(3) . . ? C14 C12 C13 112.4(4) . . ? C15 C14 C19 117.5(6) . . ? C15 C14 C12 123.2(5) . . ? C19 C14 C12 119.3(5) . . ? C16 C15 C14 121.4(7) . . ? C15 C16 C17 120.9(8) . . ? C18 C17 C16 119.6(8) . . ? C17 C18 C19 119.6(7) . . ? C18 C19 C14 120.9(7) . . ? N2 C20 C21 110.7(3) . . ? O2 C21 N21 121.4(4) . . ? O2 C21 C20 120.3(3) . . ? N21 C21 C20 118.3(3) . . ? N21 C22 C24 111.0(3) . . ? N21 C22 C23 108.5(3) . . ? C24 C22 C23 113.9(3) . . ? C24 C29 C28 119.8(6) . . ? C29 C24 C25 118.5(5) . . ? C29 C24 C22 119.4(4) . . ? C25 C24 C22 122.1(4) . . ? C24 C25 C26 121.0(6) . . ? C27 C26 C25 120.6(7) . . ? C26 C27 C28 118.0(6) . . ? C27 C28 C29 122.1(6) . . ? N3 C30 C31 111.1(3) . . ? O3 C31 N31 121.7(3) . . ? O3 C31 C30 120.4(3) . . ? N31 C31 C30 117.8(3) . . ? N31 C32 C34 110.7(3) . . ? N31 C32 C33 108.5(3) . . ? C34 C32 C33 112.6(3) . . ? C39 C34 C35 118.4(4) . . ? C39 C34 C32 119.8(4) . . ? C35 C34 C32 121.8(4) . . ? C36 C35 C34 120.1(4) . . ? C37 C36 C35 120.4(4) . . ? C38 C37 C36 120.5(4) . . ? C37 C38 C39 119.5(4) . . ? C34 C39 C38 121.1(4) . . ? N4 C40 C41 110.9(3) . . ? O4 C41 N41 122.2(3) . . ? O4 C41 C40 119.4(3) . . ? N41 C41 C40 118.3(3) . . ? N41 C42 C44 111.2(3) . . ? N41 C42 C43 108.4(3) . . ? C44 C42 C43 112.9(3) . . ? C49 C44 C45 119.2(4) . . ? C49 C44 C42 120.2(4) . . ? C45 C44 C42 120.5(4) . . ? C46 C45 C44 120.1(4) . . ? C45 C46 C47 120.1(4) . . ? C48 C47 C46 120.2(4) . . ? C47 C48 C49 119.4(4) . . ? C44 C49 C48 121.0(4) . . ? O13 S1 O11 114.8(2) . . ? O13 S1 O12 115.2(2) . . ? O11 S1 O12 114.6(2) . . ? O13 S1 C1S 103.3(3) . . ? O11 S1 C1S 103.4(2) . . ? O12 S1 C1S 103.2(2) . . ? F11 C1S F13 108.6(5) . . ? F11 C1S F12 108.6(5) . . ? F13 C1S F12 107.8(5) . . ? F11 C1S S1 111.1(5) . . ? F13 C1S S1 110.5(4) . . ? F12 C1S S1 110.2(4) . . ? O23B S2 O22B 132.4(9) . . ? O23B S2 O23A 132.3(8) . . ? O22B S2 O23A 61.8(7) . . ? O23B S2 O22A 29.0(8) . . ? O22B S2 O22A 153.3(8) . . ? O23A S2 O22A 114.2(3) . . ? O23B S2 O21A 81.6(8) . . ? O22B S2 O21A 56.9(7) . . ? O23A S2 O21A 114.7(3) . . ? O22A S2 O21A 110.5(4) . . ? O23B S2 O21B 111.5(9) . . ? O22B S2 O21B 107.5(8) . . ? O23A S2 O21B 50.0(6) . . ? O22A S2 O21B 82.6(8) . . ? O21A S2 O21B 164.2(7) . . ? O23B S2 C2S 110.4(8) . . ? O22B S2 C2S 99.3(7) . . ? O23A S2 C2S 110.3(3) . . ? O22A S2 C2S 106.4(4) . . ? O21A S2 C2S 99.5(3) . . ? O21B S2 C2S 84.6(6) . . ? F22 C2S F21 119.2(8) . . ? F22 C2S F23 102.4(6) . . ? F21 C2S F23 97.0(6) . . ? F22 C2S S2 116.4(5) . . ? F21 C2S S2 112.1(6) . . ? F23 C2S S2 105.9(6) . . ? O31 S3 O33 116.4(3) . . ? O31 S3 O32 117.3(4) . . ? O33 S3 O32 111.8(2) . . ? O31 S3 C3S 103.1(3) . . ? O33 S3 C3S 103.8(2) . . ? O32 S3 C3S 101.7(3) . . ? F32 C3S F31 105.6(5) . . ? F32 C3S F33 109.9(4) . . ? F31 C3S F33 106.1(4) . . ? F32 C3S S3 113.4(4) . . ? F31 C3S S3 109.9(4) . . ? F33 C3S S3 111.4(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H051 O11 0.80 2.04 2.832(4) 170.2 . O5 H052 O22A 0.80 2.14 2.931(5) 168.7 . N11 H11 O33 0.88 2.17 2.922(4) 142.7 1_455 N21 H21 O12 0.88 2.11 2.958(4) 161.6 2_657 N31 H31 O32 0.88 2.06 2.915(5) 164.9 . N41 H41 O3W 0.88 1.97 2.847(5) 172.8 2_556 O1W H1W1 O2W 0.77 2.06 2.828(4) 175.9 . O1W H2W1 O5 0.84 2.29 3.085(4) 158.2 . O2W H1W2 O23A 0.83 2.05 2.869(5) 168.6 . O2W H2W2 O13 0.81 2.14 2.851(5) 145.2 . O3W H1W3 O21A 0.88 2.22 3.043(8) 155.4 . O3W H2W3 O31 0.88 2.26 3.101(9) 158.4 1_445 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.144 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.082 #==============================================END data_8b _database_code_CSD 182449 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Er N8 O5 3+,3(C F3 O3 S 1-),3(H2 O)' _chemical_formula_sum 'C51 H72 Er F9 N8 O17 S3' _chemical_formula_weight 1503.61 _chemical_absolute_configuration ad _chemical_optical_rotation ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.473(1) _cell_length_b 11.845(1) _cell_length_c 19.217(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.35(1) _cell_angle_gamma 90.00 _cell_volume 3218.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 995 _cell_measurement_theta_min 12.09 _cell_measurement_theta_max 22.97 _exptl_crystal_description 'oblique block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1534 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4971 _exptl_absorpt_correction_T_max 0.7827 _exptl_absorpt_process_details 'XPREP (SHELXTL), R(int)=0.068 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 -2.00 0.1350 -1.00 0.00 2.00 0.1350 0.00 0.00 1.00 0.1200 0.00 0.00 -1.00 0.1200 0.00 1.00 1.00 0.1800 0.00 -1.00 2.00 0.1600 0.00 -1.00 -2.00 0.1500 0.00 1.00 -1.00 0.2500 1.00 1.00 -1.00 0.2200 3.00 2.00 1.00 0.2800 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f and/or 2\q angles and each scan (5 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. Merging of Friedel pairs yields 12088 independent reflections. ; _diffrn_ambient_temperature 120(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 'SMART 6000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53154 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 32.50 _reflns_number_total 23033 _reflns_number_gt 21765 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.905 _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. H atoms of water - refall, methyl groups - refined as rigid bodies, other H atoms -'riding'. ; _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^)+(0.0320P)^2^+1.5099P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(3) _refine_ls_number_reflns 23033 _refine_ls_number_parameters 818 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er Er 0.303540(5) 0.700201(8) 0.717991(3) 0.01376(2) Uani 1 1 d . . . O1 O 0.17386(10) 0.64359(13) 0.76242(8) 0.0184(3) Uani 1 1 d . . . O2 O 0.38604(11) 0.65859(14) 0.83095(8) 0.0210(3) Uani 1 1 d . . . O3 O 0.43609(10) 0.62868(13) 0.68458(8) 0.0189(3) Uani 1 1 d . . . O4 O 0.22583(10) 0.62116(13) 0.61267(7) 0.0169(3) Uani 1 1 d . . . O5 O 0.30378(11) 0.49592(14) 0.73092(9) 0.0219(3) Uani 1 1 d . . . H051 H 0.3456 0.4597 0.7582 0.025(7) Uiso 1 1 d R . . H052 H 0.2596 0.4605 0.7468 0.039(9) Uiso 1 1 d R . . N1 N 0.15643(12) 0.82797(14) 0.67284(9) 0.0157(3) Uani 1 1 d . . . N2 N 0.28267(12) 0.85190(15) 0.81403(9) 0.0182(3) Uani 1 1 d . . . N3 N 0.44844(12) 0.83897(15) 0.74663(9) 0.0183(3) Uani 1 1 d . . . N4 N 0.32269(12) 0.81726(15) 0.60525(9) 0.0160(3) Uani 1 1 d . . . N11 N 0.02013(13) 0.65430(17) 0.76803(11) 0.0223(3) Uani 1 1 d . . . H11 H -0.0356 0.6843 0.7504 0.043(9) Uiso 1 1 d R . . N21 N 0.42058(14) 0.67005(16) 0.95026(10) 0.0236(4) Uani 1 1 d . . . H21 H 0.4128 0.7059 0.9887 0.041(8) Uiso 1 1 d R . . N31 N 0.59239(13) 0.62407(18) 0.68665(11) 0.0249(4) Uani 1 1 d . . . H31 H 0.6483 0.6551 0.7018 0.024(7) Uiso 1 1 d R . . N41 N 0.19103(12) 0.59890(16) 0.49397(9) 0.0186(3) Uani 1 1 d . . . H41 H 0.1984 0.6227 0.4521 0.037(9) Uiso 1 1 d R . . C1 C 0.15381(15) 0.92836(18) 0.71928(11) 0.0199(4) Uani 1 1 d . . . H1A H 0.0885 0.9584 0.7102 0.026 Uiso 1 1 d R . . H1B H 0.1952 0.9880 0.7066 0.026 Uiso 1 1 d R . . C2 C 0.18561(15) 0.90088(18) 0.79791(11) 0.0201(4) Uani 1 1 d . . . H2A H 0.1848 0.9705 0.8262 0.026 Uiso 1 1 d R . . H2B H 0.1409 0.8465 0.8118 0.026 Uiso 1 1 d R . . C3 C 0.35181(15) 0.94526(18) 0.81606(12) 0.0208(4) Uani 1 1 d . . . H3A H 0.3555 0.9892 0.8604 0.027 Uiso 1 1 d R . . H3B H 0.3289 0.9965 0.7753 0.027 Uiso 1 1 d R . . C4 C 0.45004(15) 0.90372(19) 0.81298(11) 0.0210(4) Uani 1 1 d . . . H4A H 0.4932 0.9691 0.8151 0.027 Uiso 1 1 d R . . H4B H 0.4745 0.8551 0.8547 0.027 Uiso 1 1 d R . . C5 C 0.44865(15) 0.92209(19) 0.68810(12) 0.0219(4) Uani 1 1 d . . . H5A H 0.5131 0.9536 0.6931 0.028 Uiso 1 1 d R . . H5B H 0.4054 0.9851 0.6927 0.028 Uiso 1 1 d R . . C6 C 0.41795(14) 0.86922(18) 0.61466(11) 0.0193(4) Uani 1 1 d . . . H6A H 0.4169 0.9279 0.5778 0.025 Uiso 1 1 d R . . H6B H 0.4643 0.8108 0.6083 0.025 Uiso 1 1 d R . . C7 C 0.24976(14) 0.90742(18) 0.58990(11) 0.0191(4) Uani 1 1 d . . . H7A H 0.2447 0.9343 0.5405 0.025 Uiso 1 1 d R . . H7B H 0.2703 0.9719 0.6223 0.025 Uiso 1 1 d R . . C8 C 0.15302(14) 0.86823(18) 0.59888(11) 0.0181(3) Uani 1 1 d . . . H8A H 0.1075 0.9314 0.5878 0.024 Uiso 1 1 d R . . H8B H 0.1306 0.8063 0.5649 0.024 Uiso 1 1 d R . . C10 C 0.07333(13) 0.75540(17) 0.67363(11) 0.0172(3) Uani 1 1 d . . . H10A H 0.0595 0.7083 0.6301 0.022 Uiso 1 1 d R . . H10B H 0.0174 0.8033 0.6741 0.022 Uiso 1 1 d R . . C11 C 0.09238(14) 0.68057(15) 0.73853(10) 0.0178(4) Uani 1 1 d . . . C12 C 0.02950(18) 0.5773(2) 0.82901(14) 0.0280(5) Uani 1 1 d . . . H12 H 0.0691 0.5115 0.8207 0.034 Uiso 1 1 d R . . C13 C -0.0684(2) 0.5341(3) 0.83203(17) 0.0394(6) Uani 1 1 d . . . H13A H -0.1098 0.5982 0.8361 0.059 Uiso 1 1 calc R . . H13B H -0.0640 0.4846 0.8735 0.059 Uiso 1 1 calc R . . H13C H -0.0946 0.4917 0.7885 0.059 Uiso 1 1 calc R . . C14 C 0.0779(2) 0.6345(3) 0.89769(15) 0.0348(6) Uani 1 1 d . . . C15 C 0.0511(2) 0.7411(3) 0.91532(17) 0.0452(8) Uani 1 1 d . . . H15 H 0.0026 0.7806 0.8835 0.054 Uiso 1 1 d R . . C16 C 0.0950(3) 0.7905(5) 0.9799(2) 0.0665(12) Uani 1 1 d . . . H16 H 0.0753 0.8628 0.9924 0.080 Uiso 1 1 d R . . C17 C 0.1672(3) 0.7338(5) 1.02614(19) 0.0702(16) Uani 1 1 d . . . H17 H 0.1981 0.7682 1.0695 0.084 Uiso 1 1 d R . . C18 C 0.1940(3) 0.6287(5) 1.00870(19) 0.0644(13) Uani 1 1 d . . . H18 H 0.2429 0.5896 1.0404 0.077 Uiso 1 1 d R . . C19 C 0.1501(2) 0.5785(3) 0.94479(17) 0.0470(8) Uani 1 1 d . . . H19 H 0.1692 0.5055 0.9330 0.056 Uiso 1 1 d R . . C20 C 0.29879(16) 0.79351(19) 0.88351(11) 0.0217(4) Uani 1 1 d . . . H20A H 0.2390 0.7587 0.8900 0.028 Uiso 1 1 d R . . H20B H 0.3195 0.8488 0.9223 0.028 Uiso 1 1 d R . . C21 C 0.37302(12) 0.7037(3) 0.88705(9) 0.0190(3) Uani 1 1 d . . . C22 C 0.48601(16) 0.57396(19) 0.95753(11) 0.0223(4) Uani 1 1 d . . . H22 H 0.4667 0.5254 0.9143 0.027 Uiso 1 1 d R . . C23 C 0.47540(19) 0.5049(2) 1.02192(14) 0.0306(5) Uani 1 1 d . . . H23A H 0.4959 0.5501 1.0652 0.046 Uiso 1 1 calc R . . H23B H 0.5145 0.4368 1.0249 0.046 Uiso 1 1 calc R . . H23C H 0.4090 0.4834 1.0172 0.046 Uiso 1 1 calc R . . C24 C 0.58680(19) 0.6116(2) 0.96144(13) 0.0282(5) Uani 1 1 d . . . C25 C 0.62613(19) 0.7037(5) 0.9977(2) 0.0573(9) Uani 1 1 d . . . H25 H 0.5888 0.7480 1.0224 0.069 Uiso 1 1 d R . . C26 C 0.7195(3) 0.7359(4) 1.0001(3) 0.0649(12) Uani 1 1 d . . . H26 H 0.7441 0.8027 1.0245 0.078 Uiso 1 1 d R . . C27 C 0.7739(3) 0.6727(4) 0.9674(3) 0.0797(16) Uani 1 1 d . . . H27 H 0.8381 0.6927 0.9695 0.096 Uiso 1 1 d R . . C28 C 0.7363(5) 0.5807(6) 0.9311(5) 0.142(4) Uani 1 1 d . . . H28 H 0.7751 0.5342 0.9089 0.171 Uiso 1 1 d R . . C29 C 0.6420(4) 0.5517(5) 0.9262(4) 0.107(3) Uani 1 1 d . . . H29 H 0.6163 0.4888 0.8980 0.128 Uiso 1 1 d R . . C30 C 0.53375(14) 0.7665(2) 0.75683(12) 0.0228(4) Uani 1 1 d . . . H30A H 0.5491 0.7381 0.8064 0.030 Uiso 1 1 d R . . H30B H 0.5881 0.8116 0.7488 0.030 Uiso 1 1 d R . . C31 C 0.51763(15) 0.66842(18) 0.70601(11) 0.0205(4) Uani 1 1 d . . . C32 C 0.58382(16) 0.5238(2) 0.64036(13) 0.0250(4) Uani 1 1 d . . . H32 H 0.5440 0.4667 0.6587 0.030 Uiso 1 1 d R . . C33 C 0.6825(2) 0.4738(3) 0.64611(17) 0.0372(6) Uani 1 1 d . . . H33A H 0.7219 0.5272 0.6264 0.056 Uiso 1 1 calc R . . H33B H 0.6777 0.4029 0.6193 0.056 Uiso 1 1 calc R . . H33C H 0.7113 0.4592 0.6963 0.056 Uiso 1 1 calc R . . C34 C 0.53587(16) 0.55269(18) 0.56417(12) 0.0221(4) Uani 1 1 d . . . C35 C 0.56910(18) 0.6407(2) 0.52722(14) 0.0278(5) Uani 1 1 d . . . H35 H 0.6227 0.6835 0.5497 0.033 Uiso 1 1 d R . . C36 C 0.5234(2) 0.6649(2) 0.45743(15) 0.0336(5) Uani 1 1 d . . . H36 H 0.5458 0.7245 0.4325 0.040 Uiso 1 1 d R . . C37 C 0.4455(2) 0.6029(2) 0.42430(14) 0.0329(5) Uani 1 1 d . . . H37 H 0.4146 0.6203 0.3768 0.040 Uiso 1 1 d R . . C38 C 0.41264(18) 0.5155(2) 0.46000(14) 0.0300(5) Uani 1 1 d . . . H38 H 0.3595 0.4724 0.4370 0.036 Uiso 1 1 d R . . C39 C 0.45796(16) 0.49080(19) 0.53015(13) 0.0249(4) Uani 1 1 d . . . H39 H 0.4351 0.4309 0.5548 0.030 Uiso 1 1 d R . . C40 C 0.31002(14) 0.73690(18) 0.54519(11) 0.0182(3) Uani 1 1 d . . . H40A H 0.3712 0.7001 0.5444 0.024 Uiso 1 1 d R . . H40B H 0.2891 0.7782 0.4998 0.024 Uiso 1 1 d R . . C41 C 0.23760(13) 0.64829(17) 0.55208(10) 0.0156(3) Uani 1 1 d . . . C42 C 0.12659(14) 0.50396(18) 0.49803(11) 0.0194(4) Uani 1 1 d . . . H42 H 0.1580 0.4528 0.5374 0.023 Uiso 1 1 d R . . C43 C 0.11080(17) 0.4380(2) 0.42859(13) 0.0265(4) Uani 1 1 d . . . H43A H 0.0796 0.4865 0.3892 0.040 Uiso 1 1 calc R . . H43B H 0.0708 0.3722 0.4318 0.040 Uiso 1 1 calc R . . H43C H 0.1719 0.4126 0.4200 0.040 Uiso 1 1 calc R . . C44 C 0.03491(14) 0.54542(18) 0.51488(11) 0.0192(4) Uani 1 1 d . . . C45 C -0.01771(17) 0.63107(19) 0.47465(13) 0.0242(4) Uani 1 1 d . . . H45 H 0.0053 0.6655 0.4371 0.029 Uiso 1 1 d R . . C46 C -0.10300(18) 0.6660(2) 0.48909(15) 0.0311(5) Uani 1 1 d . . . H46 H -0.1384 0.7238 0.4611 0.037 Uiso 1 1 d R . . C47 C -0.13664(18) 0.6168(2) 0.54413(16) 0.0338(5) Uani 1 1 d . . . H47 H -0.1950 0.6411 0.5542 0.041 Uiso 1 1 d R . . C48 C -0.08491(18) 0.5313(2) 0.58477(15) 0.0318(5) Uani 1 1 d . . . H48 H -0.1076 0.4975 0.6227 0.038 Uiso 1 1 d R . . C49 C 0.00010(16) 0.4958(2) 0.56966(12) 0.0256(4) Uani 1 1 d . . . H49 H 0.0349 0.4369 0.5970 0.031 Uiso 1 1 d R . . S1 S 0.50154(5) 0.28093(5) 0.83771(3) 0.03093(12) Uani 1 1 d . . . O11 O 0.46383(17) 0.38948(18) 0.81353(13) 0.0462(6) Uani 1 1 d . . . O12 O 0.55408(16) 0.2788(2) 0.91031(11) 0.0412(5) Uani 1 1 d . . . O13 O 0.43766(16) 0.1874(2) 0.81735(12) 0.0485(6) Uani 1 1 d . . . C1S C 0.5931(3) 0.2579(3) 0.7869(2) 0.0500(9) Uani 1 1 d . . . F11 F 0.6327(2) 0.1579(2) 0.80190(19) 0.0889(10) Uani 1 1 d . . . F12 F 0.5544(2) 0.2638(2) 0.71681(12) 0.0745(8) Uani 1 1 d . . . F13 F 0.65968(19) 0.3359(2) 0.80172(14) 0.0674(7) Uani 1 1 d . . . S2 S 0.06941(5) 0.28268(6) 0.73191(4) 0.03313(13) Uani 1 1 d . . . O21 O -0.02850(19) 0.3100(2) 0.70843(15) 0.0565(7) Uani 1 1 d . . . O22 O 0.13032(19) 0.3785(2) 0.74703(16) 0.0535(6) Uani 1 1 d . . . O23 O 0.10313(15) 0.1949(3) 0.69175(11) 0.0464(4) Uani 1 1 d . . . C2S C 0.0754(3) 0.2170(3) 0.81769(19) 0.0574(10) Uani 1 1 d . . . F21 F 0.0214(3) 0.1285(2) 0.81387(19) 0.0931(10) Uani 1 1 d . . . F22 F 0.0512(2) 0.2900(2) 0.86542(13) 0.0742(8) Uani 1 1 d . . . F23 F 0.1639(2) 0.1843(3) 0.84438(14) 0.0952(11) Uani 1 1 d . . . S3 S 0.79964(4) 0.86221(7) 0.74217(4) 0.03355(14) Uani 1 1 d . . . O31 O 0.74026(19) 0.9334(3) 0.69146(13) 0.0661(9) Uani 1 1 d . . . O32 O 0.76230(16) 0.7503(2) 0.75235(14) 0.0524(6) Uani 1 1 d . . . O33 O 0.89834(14) 0.8597(2) 0.73957(12) 0.0399(5) Uani 1 1 d . . . C3S C 0.79806(19) 0.9332(3) 0.82570(16) 0.0366(6) Uani 1 1 d . . . F31 F 0.82606(18) 1.0394(2) 0.82421(16) 0.0684(7) Uani 1 1 d . . . F32 F 0.85461(16) 0.8857(2) 0.88015(11) 0.0622(6) Uani 1 1 d . . . F33 F 0.71065(12) 0.93542(17) 0.83823(10) 0.0411(4) Uani 1 1 d . . . O1W O 0.30462(15) 0.35108(17) 0.59973(11) 0.0347(4) Uani 1 1 d . . . H1W1 H 0.3063 0.2991 0.6248 0.078(16) Uiso 1 1 d R . . H2W1 H 0.3057 0.4039 0.6291 0.088(17) Uiso 1 1 d R . . O2W O 0.29566(15) 0.16414(16) 0.69039(11) 0.0341(4) Uani 1 1 d . . . H1W2 H 0.2419 0.1819 0.6940 0.034(8) Uiso 1 1 d R . . H2W2 H 0.3200 0.1841 0.7305 0.090(17) Uiso 1 1 d R . . O3W O -0.19760(17) 0.1737(2) 0.64563(11) 0.0453(6) Uani 1 1 d . . . H1W3 H -0.1393 0.1945 0.6627 0.092(16) Uiso 1 1 d R . . H2W3 H -0.2180 0.1177 0.6693 0.060(13) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er 0.01466(3) 0.01478(3) 0.01102(3) -0.00002(4) 0.00089(2) 0.00165(4) O1 0.0173(6) 0.0207(7) 0.0178(6) 0.0042(5) 0.0051(5) 0.0030(5) O2 0.0246(7) 0.0236(7) 0.0125(6) 0.0009(5) -0.0008(5) 0.0064(6) O3 0.0169(6) 0.0217(7) 0.0180(7) -0.0015(5) 0.0032(5) 0.0029(5) O4 0.0180(6) 0.0203(7) 0.0115(6) -0.0011(5) 0.0010(5) -0.0021(5) O5 0.0250(7) 0.0180(7) 0.0219(7) 0.0039(5) 0.0030(6) 0.0039(6) N1 0.0157(7) 0.0154(7) 0.0156(7) 0.0012(6) 0.0024(5) 0.0003(6) N2 0.0193(7) 0.0191(8) 0.0147(7) -0.0020(6) 0.0006(6) 0.0014(6) N3 0.0179(7) 0.0192(8) 0.0161(7) -0.0033(6) 0.0002(6) 0.0018(6) N4 0.0143(7) 0.0181(7) 0.0152(7) -0.0003(6) 0.0018(5) -0.0014(6) N11 0.0208(8) 0.0236(8) 0.0245(9) 0.0059(7) 0.0090(7) 0.0031(7) N21 0.0316(9) 0.0233(9) 0.0131(7) -0.0006(6) -0.0015(6) 0.0044(6) N31 0.0176(8) 0.0296(10) 0.0268(9) -0.0063(7) 0.0037(7) 0.0027(7) N41 0.0198(7) 0.0226(8) 0.0128(7) -0.0009(6) 0.0021(6) -0.0040(6) C1 0.0200(9) 0.0185(9) 0.0197(9) -0.0010(7) 0.0011(7) 0.0043(7) C2 0.0205(9) 0.0209(9) 0.0180(9) -0.0029(7) 0.0017(7) 0.0053(7) C3 0.0208(9) 0.0188(9) 0.0203(9) -0.0054(7) -0.0007(7) 0.0003(7) C4 0.0211(9) 0.0215(9) 0.0183(9) -0.0061(7) -0.0007(7) -0.0007(7) C5 0.0214(9) 0.0228(10) 0.0204(9) -0.0024(7) 0.0020(7) -0.0061(7) C6 0.0165(8) 0.0220(9) 0.0192(9) -0.0004(7) 0.0036(7) -0.0045(7) C7 0.0189(8) 0.0182(8) 0.0198(9) 0.0048(7) 0.0035(7) 0.0007(7) C8 0.0181(8) 0.0201(9) 0.0151(8) 0.0041(7) 0.0009(6) 0.0020(7) C10 0.0151(8) 0.0200(9) 0.0158(8) 0.0025(7) 0.0016(6) 0.0008(7) C11 0.0184(7) 0.0184(12) 0.0171(7) 0.0011(6) 0.0051(6) -0.0002(6) C12 0.0290(11) 0.0281(11) 0.0308(12) 0.0106(9) 0.0152(9) 0.0055(9) C13 0.0347(13) 0.0436(16) 0.0458(16) 0.0112(13) 0.0217(12) -0.0020(12) C14 0.0329(13) 0.0486(16) 0.0258(12) 0.0104(11) 0.0124(10) 0.0073(12) C15 0.0463(17) 0.061(2) 0.0300(14) -0.0073(13) 0.0132(12) 0.0127(14) C16 0.073(3) 0.089(3) 0.0401(19) -0.027(2) 0.0179(18) 0.006(2) C17 0.075(3) 0.111(5) 0.0215(14) -0.0025(18) 0.0051(15) -0.004(3) C18 0.059(2) 0.104(4) 0.0271(16) 0.023(2) 0.0020(15) 0.001(2) C19 0.0435(16) 0.062(2) 0.0372(15) 0.0266(15) 0.0120(13) 0.0106(14) C20 0.0272(10) 0.0237(10) 0.0133(8) -0.0009(7) 0.0023(7) 0.0039(8) C21 0.0216(7) 0.0188(7) 0.0148(6) 0.0006(11) -0.0001(5) 0.0016(12) C22 0.0285(10) 0.0201(9) 0.0150(8) 0.0017(7) -0.0028(7) 0.0042(8) C23 0.0333(12) 0.0296(12) 0.0261(11) 0.0107(9) 0.0003(9) 0.0006(9) C24 0.0343(12) 0.0251(11) 0.0255(11) 0.0013(8) 0.0073(9) 0.0028(9) C25 0.0321(12) 0.0587(19) 0.078(2) -0.036(3) 0.0042(13) -0.005(2) C26 0.0385(16) 0.056(2) 0.096(3) -0.021(2) 0.0062(18) -0.0118(14) C27 0.051(2) 0.072(4) 0.130(4) -0.009(3) 0.050(3) -0.0152(19) C28 0.104(4) 0.101(4) 0.269(10) -0.098(6) 0.144(6) -0.054(4) C29 0.090(3) 0.086(3) 0.178(6) -0.084(4) 0.105(4) -0.054(3) C30 0.0156(8) 0.0289(10) 0.0210(9) -0.0062(8) -0.0024(7) 0.0024(7) C31 0.0182(8) 0.0245(9) 0.0182(8) 0.0011(6) 0.0025(7) 0.0044(6) C32 0.0236(10) 0.0237(10) 0.0288(11) 0.0004(8) 0.0084(8) 0.0065(8) C33 0.0316(12) 0.0403(15) 0.0427(15) 0.0042(12) 0.0148(11) 0.0173(11) C34 0.0237(9) 0.0189(9) 0.0262(10) -0.0016(7) 0.0111(8) 0.0036(7) C35 0.0299(11) 0.0229(10) 0.0336(12) -0.0004(9) 0.0133(9) -0.0014(8) C36 0.0439(14) 0.0276(10) 0.0341(13) 0.0036(9) 0.0190(11) 0.0047(10) C37 0.0417(14) 0.0333(13) 0.0253(11) -0.0011(10) 0.0107(10) 0.0133(11) C38 0.0291(11) 0.0294(12) 0.0329(12) -0.0078(9) 0.0096(9) 0.0038(9) C39 0.0254(10) 0.0207(9) 0.0315(11) -0.0034(8) 0.0122(9) 0.0007(8) C40 0.0189(8) 0.0209(8) 0.0144(8) -0.0013(6) 0.0028(6) -0.0023(6) C41 0.0150(8) 0.0179(9) 0.0131(8) -0.0007(6) 0.0009(6) 0.0006(6) C42 0.0194(8) 0.0194(9) 0.0180(9) -0.0032(7) 0.0006(7) -0.0030(7) C43 0.0260(10) 0.0288(11) 0.0238(10) -0.0101(9) 0.0034(8) -0.0048(9) C44 0.0191(8) 0.0192(9) 0.0180(9) -0.0033(7) 0.0009(7) -0.0038(7) C45 0.0264(10) 0.0206(9) 0.0240(10) 0.0002(8) 0.0020(8) -0.0019(8) C46 0.0270(11) 0.0249(10) 0.0394(13) -0.0003(9) 0.0028(10) 0.0022(8) C47 0.0230(10) 0.0351(13) 0.0442(15) -0.0050(11) 0.0089(10) -0.0004(9) C48 0.0260(11) 0.0359(13) 0.0361(13) -0.0016(10) 0.0123(10) -0.0062(10) C49 0.0241(10) 0.0286(11) 0.0238(10) 0.0024(8) 0.0047(8) -0.0020(8) S1 0.0396(3) 0.0239(3) 0.0239(3) 0.0007(2) -0.0052(2) 0.0051(2) O11 0.0542(13) 0.0289(10) 0.0445(12) -0.0046(9) -0.0138(10) 0.0162(9) O12 0.0466(12) 0.0482(12) 0.0232(9) 0.0090(8) -0.0049(8) -0.0085(10) O13 0.0529(11) 0.0381(14) 0.0453(11) 0.0012(11) -0.0103(9) -0.0074(11) C1S 0.076(3) 0.0345(16) 0.0419(18) -0.0029(13) 0.0172(17) 0.0100(16) F11 0.101(2) 0.0585(16) 0.114(3) 0.0033(15) 0.0400(19) 0.0439(15) F12 0.128(2) 0.0677(15) 0.0334(11) -0.0173(10) 0.0289(13) -0.0048(15) F13 0.0726(16) 0.0762(17) 0.0619(15) -0.0034(12) 0.0335(13) -0.0123(13) S2 0.0348(3) 0.0288(3) 0.0362(3) -0.0012(2) 0.0086(3) -0.0008(2) O21 0.0441(13) 0.0625(17) 0.0595(16) 0.0083(13) 0.0031(11) 0.0130(12) O22 0.0548(14) 0.0402(12) 0.0720(17) -0.0158(12) 0.0280(13) -0.0154(11) O23 0.0534(11) 0.0389(10) 0.0479(11) -0.0112(14) 0.0128(8) 0.0032(14) C2S 0.094(3) 0.036(2) 0.0439(16) 0.0075(14) 0.0172(17) 0.0120(18) F21 0.136(3) 0.0466(14) 0.112(3) 0.0196(15) 0.062(2) -0.0127(16) F22 0.140(3) 0.0471(12) 0.0462(12) 0.0039(10) 0.0432(15) 0.0212(14) F23 0.128(2) 0.078(2) 0.0583(14) -0.0067(15) -0.0262(14) 0.052(2) S3 0.0247(3) 0.0511(4) 0.0257(3) 0.0024(3) 0.0074(2) 0.0130(3) O31 0.0560(15) 0.112(2) 0.0323(12) 0.0250(14) 0.0131(11) 0.0490(16) O32 0.0348(11) 0.0579(14) 0.0638(16) -0.0257(12) 0.0092(10) 0.0009(10) O33 0.0290(9) 0.0544(13) 0.0405(11) 0.0104(9) 0.0172(8) 0.0132(9) C3S 0.0286(12) 0.0432(15) 0.0392(15) -0.0020(12) 0.0101(10) 0.0061(11) F31 0.0608(14) 0.0484(13) 0.104(2) -0.0227(13) 0.0349(14) -0.0113(11) F32 0.0516(12) 0.0959(19) 0.0353(10) -0.0048(11) 0.0009(9) 0.0288(12) F33 0.0309(8) 0.0495(10) 0.0470(10) -0.0075(8) 0.0176(7) 0.0056(7) O1W 0.0467(11) 0.0294(9) 0.0311(9) 0.0014(8) 0.0150(8) -0.0015(8) O2W 0.0422(11) 0.0242(8) 0.0341(10) 0.0020(7) 0.0041(8) 0.0009(7) O3W 0.0510(12) 0.0584(18) 0.0246(8) -0.0030(9) 0.0041(8) 0.0117(10) _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 Er O4 2.2944(14) . ? Er O2 2.2961(15) . ? Er O3 2.3103(15) . ? Er O1 2.3209(14) . ? Er O5 2.4324(16) . ? Er N1 2.6050(17) . ? Er N3 2.6286(18) . ? Er N4 2.6363(17) . ? Er N2 2.6390(17) . ? O1 C11 1.250(2) . ? O2 C21 1.253(3) . ? O3 C31 1.255(3) . ? O4 C41 1.254(2) . ? N1 C10 1.481(3) . ? N1 C8 1.490(3) . ? N1 C1 1.492(3) . ? N2 C20 1.477(3) . ? N2 C3 1.486(3) . ? N2 C2 1.490(3) . ? N3 C30 1.482(3) . ? N3 C4 1.484(3) . ? N3 C5 1.495(3) . ? N4 C40 1.477(3) . ? N4 C6 1.485(3) . ? N4 C7 1.486(3) . ? N11 C11 1.329(3) . ? N11 C12 1.468(3) . ? N21 C21 1.323(3) . ? N21 C22 1.468(3) . ? N31 C31 1.326(3) . ? N31 C32 1.473(3) . ? N41 C41 1.312(2) . ? N41 C42 1.474(3) . ? C1 C2 1.518(3) . ? C3 C4 1.518(3) . ? C5 C6 1.521(3) . ? C7 C8 1.520(3) . ? C10 C11 1.507(3) . ? C12 C14 1.515(4) . ? C12 C13 1.520(4) . ? C14 C15 1.384(4) . ? C14 C19 1.394(4) . ? C15 C16 1.396(5) . ? C16 C17 1.392(7) . ? C17 C18 1.366(7) . ? C18 C19 1.390(6) . ? C20 C21 1.503(4) . ? C22 C24 1.512(4) . ? C22 C23 1.518(3) . ? C24 C25 1.352(5) . ? C24 C29 1.353(5) . ? C25 C26 1.396(5) . ? C26 C27 1.337(6) . ? C27 C28 1.345(8) . ? C28 C29 1.392(7) . ? C30 C31 1.503(3) . ? C32 C34 1.519(3) . ? C32 C33 1.529(3) . ? C34 C39 1.386(3) . ? C34 C35 1.403(3) . ? C35 C36 1.393(4) . ? C36 C37 1.381(4) . ? C37 C38 1.381(4) . ? C38 C39 1.398(4) . ? C40 C41 1.509(3) . ? C42 C44 1.513(3) . ? C42 C43 1.521(3) . ? C44 C49 1.391(3) . ? C44 C45 1.398(3) . ? C45 C46 1.385(3) . ? C46 C47 1.384(4) . ? C47 C48 1.395(4) . ? C48 C49 1.388(3) . ? S1 O11 1.435(2) . ? S1 O12 1.439(2) . ? S1 O13 1.443(3) . ? S1 C1S 1.826(4) . ? C1S F11 1.321(4) . ? C1S F13 1.322(5) . ? C1S F12 1.346(5) . ? S2 O22 1.428(2) . ? S2 O21 1.429(3) . ? S2 O23 1.441(3) . ? S2 C2S 1.808(4) . ? C2S F21 1.300(5) . ? C2S F23 1.331(5) . ? C2S F22 1.360(4) . ? S3 O31 1.429(2) . ? S3 O33 1.440(2) . ? S3 O32 1.460(3) . ? S3 C3S 1.816(3) . ? C3S F32 1.309(4) . ? C3S F31 1.325(4) . ? C3S F33 1.338(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 O4 Er O2 143.52(6) . . ? O4 Er O3 83.38(5) . . ? O2 Er O3 83.64(5) . . ? O4 Er O1 85.66(5) . . ? O2 Er O1 83.58(6) . . ? O3 Er O1 141.37(6) . . ? O4 Er O5 70.97(5) . . ? O2 Er O5 72.59(6) . . ? O3 Er O5 71.37(5) . . ? O1 Er O5 70.04(5) . . ? O4 Er N1 74.44(5) . . ? O2 Er N1 131.48(5) . . ? O3 Er N1 142.05(5) . . ? O1 Er N1 67.84(5) . . ? O5 Er N1 126.52(5) . . ? O4 Er N3 131.18(5) . . ? O2 Er N3 72.90(6) . . ? O3 Er N3 67.34(6) . . ? O1 Er N3 140.84(6) . . ? O5 Er N3 128.10(5) . . ? N1 Er N3 105.37(6) . . ? O4 Er N4 66.89(5) . . ? O2 Er N4 139.91(6) . . ? O3 Er N4 74.03(5) . . ? O1 Er N4 133.61(5) . . ? O5 Er N4 127.52(5) . . ? N1 Er N4 69.07(5) . . ? N3 Er N4 67.90(5) . . ? O4 Er N2 141.90(5) . . ? O2 Er N2 66.37(5) . . ? O3 Er N2 132.07(5) . . ? O1 Er N2 73.56(6) . . ? O5 Er N2 127.14(6) . . ? N1 Er N2 68.27(5) . . ? N3 Er N2 68.49(6) . . ? N4 Er N2 105.34(6) . . ? C11 O1 Er 122.51(13) . . ? C21 O2 Er 125.33(15) . . ? C31 O3 Er 123.33(14) . . ? C41 O4 Er 125.18(13) . . ? C10 N1 C8 109.52(15) . . ? C10 N1 C1 109.38(16) . . ? C8 N1 C1 108.40(16) . . ? C10 N1 Er 105.49(11) . . ? C8 N1 Er 111.20(12) . . ? C1 N1 Er 112.79(12) . . ? C20 N2 C3 110.45(17) . . ? C20 N2 C2 109.26(17) . . ? C3 N2 C2 108.38(16) . . ? C20 N2 Er 107.08(12) . . ? C3 N2 Er 110.36(12) . . ? C2 N2 Er 111.32(12) . . ? C30 N3 C4 109.05(16) . . ? C30 N3 C5 110.21(17) . . ? C4 N3 C5 107.69(17) . . ? C30 N3 Er 105.67(13) . . ? C4 N3 Er 111.61(13) . . ? C5 N3 Er 112.59(12) . . ? C40 N4 C6 108.61(16) . . ? C40 N4 C7 110.11(16) . . ? C6 N4 C7 109.14(16) . . ? C40 N4 Er 106.61(12) . . ? C6 N4 Er 112.09(12) . . ? C7 N4 Er 110.25(12) . . ? C11 N11 C12 122.63(19) . . ? C21 N21 C22 121.3(2) . . ? C31 N31 C32 121.37(19) . . ? C41 N41 C42 120.71(17) . . ? N1 C1 C2 112.55(17) . . ? N2 C2 C1 111.24(17) . . ? N2 C3 C4 112.88(17) . . ? N3 C4 C3 111.01(16) . . ? N3 C5 C6 112.32(17) . . ? N4 C6 C5 111.28(17) . . ? N4 C7 C8 112.99(16) . . ? N1 C8 C7 111.26(16) . . ? N1 C10 C11 110.16(15) . . ? O1 C11 N11 121.88(18) . . ? O1 C11 C10 120.10(17) . . ? N11 C11 C10 118.01(17) . . ? N11 C12 C14 111.3(2) . . ? N11 C12 C13 108.2(2) . . ? C14 C12 C13 112.2(2) . . ? C15 C14 C19 119.0(3) . . ? C15 C14 C12 121.3(3) . . ? C19 C14 C12 119.7(3) . . ? C14 C15 C16 120.2(4) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 119.8(4) . . ? C17 C18 C19 120.4(4) . . ? C18 C19 C14 120.5(4) . . ? N2 C20 C21 110.21(17) . . ? O2 C21 N21 121.1(2) . . ? O2 C21 C20 120.03(17) . . ? N21 C21 C20 118.78(19) . . ? N21 C22 C24 111.84(19) . . ? N21 C22 C23 108.6(2) . . ? C24 C22 C23 112.52(19) . . ? C25 C24 C29 116.9(3) . . ? C25 C24 C22 124.0(2) . . ? C29 C24 C22 119.1(3) . . ? C24 C25 C26 122.4(3) . . ? C27 C26 C25 119.7(4) . . ? C26 C27 C28 118.9(4) . . ? C27 C28 C29 121.1(4) . . ? C24 C29 C28 120.9(4) . . ? N3 C30 C31 110.65(16) . . ? O3 C31 N31 121.7(2) . . ? O3 C31 C30 120.48(18) . . ? N31 C31 C30 117.77(19) . . ? N31 C32 C34 111.27(19) . . ? N31 C32 C33 108.2(2) . . ? C34 C32 C33 112.6(2) . . ? C39 C34 C35 119.1(2) . . ? C39 C34 C32 119.6(2) . . ? C35 C34 C32 121.3(2) . . ? C36 C35 C34 119.8(2) . . ? C37 C36 C35 120.5(2) . . ? C36 C37 C38 120.2(3) . . ? C37 C38 C39 119.7(2) . . ? C34 C39 C38 120.7(2) . . ? N4 C40 C41 110.62(16) . . ? O4 C41 N41 121.93(19) . . ? O4 C41 C40 119.64(17) . . ? N41 C41 C40 118.38(17) . . ? N41 C42 C44 110.94(17) . . ? N41 C42 C43 108.88(18) . . ? C44 C42 C43 112.36(17) . . ? C49 C44 C45 118.8(2) . . ? C49 C44 C42 120.1(2) . . ? C45 C44 C42 121.1(2) . . ? C46 C45 C44 120.6(2) . . ? C47 C46 C45 120.1(2) . . ? C46 C47 C48 119.9(2) . . ? C49 C48 C47 119.7(2) . . ? C48 C49 C44 120.7(2) . . ? O11 S1 O12 114.51(14) . . ? O11 S1 O13 115.04(14) . . ? O12 S1 O13 115.14(14) . . ? O11 S1 C1S 103.30(17) . . ? O12 S1 C1S 102.84(17) . . ? O13 S1 C1S 103.66(17) . . ? F11 C1S F13 108.5(4) . . ? F11 C1S F12 109.4(3) . . ? F13 C1S F12 107.9(3) . . ? F11 C1S S1 110.4(3) . . ? F13 C1S S1 111.1(2) . . ? F12 C1S S1 109.5(3) . . ? O22 S2 O21 114.29(18) . . ? O22 S2 O23 114.66(15) . . ? O21 S2 O23 114.90(16) . . ? O22 S2 C2S 104.42(19) . . ? O21 S2 C2S 103.68(19) . . ? O23 S2 C2S 102.84(17) . . ? F21 C2S F23 107.7(3) . . ? F21 C2S F22 108.2(4) . . ? F23 C2S F22 106.9(3) . . ? F21 C2S S2 112.6(3) . . ? F23 C2S S2 109.3(3) . . ? F22 C2S S2 111.9(2) . . ? O31 S3 O33 116.41(15) . . ? O31 S3 O32 116.19(19) . . ? O33 S3 O32 112.59(14) . . ? O31 S3 C3S 102.14(16) . . ? O33 S3 C3S 103.90(14) . . ? O32 S3 C3S 103.10(15) . . ? F32 C3S F31 106.5(3) . . ? F32 C3S F33 108.6(3) . . ? F31 C3S F33 106.9(2) . . ? F32 C3S S3 112.6(2) . . ? F31 C3S S3 111.0(2) . . ? F33 C3S S3 111.1(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H051 O11 0.83 1.99 2.811(3) 168.3 . O5 H052 O22 0.87 2.11 2.944(3) 159.9 . N11 H11 O33 0.88 2.28 2.986(3) 137.4 1_455 N21 H21 O12 0.88 2.08 2.925(3) 159.4 2_657 N31 H31 O32 0.88 2.06 2.924(3) 166.2 . N41 H41 O3W 0.88 1.97 2.846(3) 172.8 2_556 O1W H1W1 O2W 0.78 2.06 2.838(3) 173.9 . O1W H2W1 O5 0.84 2.24 3.052(3) 160.8 . O2W H1W2 O23 0.82 2.01 2.816(3) 168.0 . O2W H2W2 O13 0.81 2.11 2.847(3) 150.2 . O3W H1W3 O21 0.87 2.15 2.965(4) 155.6 . O3W H2W3 O31 0.89 2.33 3.166(4) 157.0 1_445 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.878 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.080 #============================================END data_8c _database_code_CSD 182450 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Lu N8 O5 3+,3(C F3 O3 S 1-),3(H2 O)' _chemical_formula_sum 'C51 H72 F9 Lu N8 O17 S3' _chemical_formula_weight 1511.32 _chemical_absolute_configuration ad _chemical_optical_rotation ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.3873(15) _cell_length_b 11.9307(12) _cell_length_c 19.289(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.69(1) _cell_angle_gamma 90.00 _cell_volume 3230.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 12.08 _cell_measurement_theta_max 23.31 _exptl_crystal_description 'oblique block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5104 _exptl_absorpt_correction_T_max 0.7625 _exptl_absorpt_process_details 'XPREP (SHELXTL), R(int)=0.093 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 -1.00 0.0900 -1.00 0.00 1.00 0.0900 0.00 1.00 1.00 0.1300 0.00 0.00 -1.00 0.1800 0.00 -1.00 1.00 0.2000 0.00 1.00 -1.00 0.1900 0.00 -1.00 -1.00 0.1300 0.00 0.00 1.00 0.2500 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 6 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. Merging of Friedel pairs yields 8174 independent reflections. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47962 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 28.00 _reflns_number_total 15564 _reflns_number_gt 15040 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.904 _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. Methyl groups were refined as rigid bodies, all other H atoms were treated as 'riding' (at idealised distances from the carrying atom), with U(iso) refined for N- and O-bound hydrogens, related to the U(eq) of the carrying atom for the rest. ; _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^)+(0.0147P)^2^+3.9888P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(3) _refine_ls_number_reflns 15564 _refine_ls_number_parameters 817 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu Lu 0.303393(7) 0.701135(10) 0.718146(4) 0.01292(3) Uani 1 1 d . . . O1 O 0.17491(16) 0.64407(16) 0.76138(10) 0.0167(4) Uani 1 1 d . . . O2 O 0.38542(16) 0.65911(17) 0.82978(9) 0.0187(4) Uani 1 1 d . . . O3 O 0.43593(15) 0.63095(17) 0.68676(10) 0.0170(4) Uani 1 1 d . . . O4 O 0.22653(16) 0.62197(16) 0.61413(9) 0.0158(4) Uani 1 1 d . . . O5 O 0.30425(16) 0.49876(17) 0.73044(10) 0.0188(4) Uani 1 1 d . . . H051 H 0.3479 0.4691 0.7611 0.045(13) Uiso 1 1 d R . . H052 H 0.2583 0.4594 0.7365 0.028(11) Uiso 1 1 d R . . N1 N 0.15523(18) 0.82591(19) 0.67194(11) 0.0133(4) Uani 1 1 d . . . N2 N 0.2800(2) 0.85115(19) 0.81315(11) 0.0173(5) Uani 1 1 d . . . N3 N 0.44863(19) 0.8391(2) 0.74839(12) 0.0166(5) Uani 1 1 d . . . N4 N 0.3242(2) 0.81654(19) 0.60677(11) 0.0161(5) Uani 1 1 d . . . N11 N 0.0190(2) 0.6510(2) 0.76565(12) 0.0206(5) Uani 1 1 d . . . H11 H -0.0373 0.6803 0.7477 0.046(13) Uiso 1 1 d R . . N21 N 0.4203(2) 0.6695(2) 0.94921(12) 0.0220(6) Uani 1 1 d . . . H21 H 0.4118 0.7041 0.9877 0.032(9) Uiso 1 1 d R . . N31 N 0.5941(2) 0.6248(2) 0.69031(13) 0.0222(5) Uani 1 1 d . . . H31 H 0.6503 0.6557 0.7060 0.019(9) Uiso 1 1 d R . . N41 N 0.19348(19) 0.5965(2) 0.49562(11) 0.0176(5) Uani 1 1 d . . . H41 H 0.2016 0.6187 0.4538 0.025(10) Uiso 1 1 d R . . C1 C 0.1507(2) 0.9260(2) 0.71766(14) 0.0182(6) Uani 1 1 d . . . H1A H 0.0868 0.9582 0.7096 0.022 Uiso 1 1 d R . . H1B H 0.1923 0.9851 0.7043 0.022 Uiso 1 1 d R . . C2 C 0.1830(2) 0.8982(2) 0.79673(14) 0.0183(6) Uani 1 1 d . . . H2A H 0.1836 0.9693 0.8245 0.022 Uiso 1 1 d R . . H2B H 0.1382 0.8449 0.8116 0.022 Uiso 1 1 d R . . C3 C 0.3497(2) 0.9446(2) 0.81616(14) 0.0198(6) Uani 1 1 d . . . H3A H 0.3547 0.9898 0.8602 0.024 Uiso 1 1 d R . . H3B H 0.3271 0.9960 0.7754 0.024 Uiso 1 1 d R . . C4 C 0.4487(2) 0.9041(2) 0.81470(14) 0.0211(6) Uani 1 1 d . . . H4A H 0.4925 0.9690 0.8164 0.025 Uiso 1 1 d R . . H4B H 0.4726 0.8542 0.8560 0.025 Uiso 1 1 d R . . C5 C 0.4494(2) 0.9220(2) 0.69010(15) 0.0212(6) Uani 1 1 d . . . H5A H 0.5133 0.9530 0.6941 0.025 Uiso 1 1 d R . . H5B H 0.4075 0.9862 0.6957 0.025 Uiso 1 1 d R . . C6 C 0.4193(2) 0.8686(2) 0.61669(14) 0.0180(5) Uani 1 1 d . . . H6A H 0.4179 0.9284 0.5802 0.022 Uiso 1 1 d R . . H6B H 0.4645 0.8094 0.6091 0.022 Uiso 1 1 d R . . C7 C 0.2491(2) 0.9057(2) 0.59019(14) 0.0179(6) Uani 1 1 d . . . H7A H 0.2431 0.9331 0.5408 0.021 Uiso 1 1 d R . . H7B H 0.2709 0.9705 0.6224 0.021 Uiso 1 1 d R . . C8 C 0.1526(2) 0.8660(2) 0.59788(13) 0.0182(6) Uani 1 1 d . . . H8A H 0.1084 0.9308 0.5879 0.022 Uiso 1 1 d R . . H8B H 0.1288 0.8042 0.5639 0.022 Uiso 1 1 d R . . C10 C 0.0721(2) 0.7535(2) 0.67168(13) 0.0168(5) Uani 1 1 d . . . H10A H 0.0563 0.7061 0.6283 0.020 Uiso 1 1 d R . . H10B H 0.0183 0.8040 0.6732 0.020 Uiso 1 1 d R . . C11 C 0.0923(2) 0.67853(19) 0.73700(13) 0.0175(6) Uani 1 1 d . . . C12 C 0.0288(3) 0.5735(3) 0.82652(16) 0.0254(7) Uani 1 1 d . . . H12A H 0.0698 0.5093 0.8183 0.031 Uiso 1 1 calc R . . C13 C -0.0689(3) 0.5275(3) 0.8287(2) 0.0357(8) Uani 1 1 d . . . H13A H -0.0939 0.4847 0.7852 0.054 Uiso 1 1 d R . . H13B H -0.1122 0.5898 0.8321 0.054 Uiso 1 1 d R . . H13C H -0.0639 0.4784 0.8701 0.054 Uiso 1 1 d R . . C14 C 0.0767(3) 0.6301(3) 0.89570(18) 0.0295(7) Uani 1 1 d . . . C15 C 0.0475(3) 0.7350(3) 0.91360(19) 0.0388(10) Uani 1 1 d . . . H15A H -0.0024 0.7729 0.8818 0.047 Uiso 1 1 d R . . C16 C 0.0910(4) 0.7855(5) 0.9784(2) 0.0556(13) Uani 1 1 d . . . H16A H 0.0707 0.8574 0.9903 0.067 Uiso 1 1 d R . . C17 C 0.1635(4) 0.7298(5) 1.0247(2) 0.0611(18) Uani 1 1 d . . . H17A H 0.1927 0.7637 1.0687 0.073 Uiso 1 1 d R . . C18 C 0.1933(4) 0.6267(5) 1.0078(2) 0.0559(14) Uani 1 1 d . . . H18A H 0.2436 0.5898 1.0398 0.067 Uiso 1 1 d R . . C19 C 0.1500(3) 0.5755(4) 0.94347(19) 0.0403(9) Uani 1 1 d . . . H19A H 0.1704 0.5032 0.9322 0.048 Uiso 1 1 d R . . C20 C 0.2966(2) 0.7919(2) 0.88237(13) 0.0205(6) Uani 1 1 d . . . H20A H 0.2372 0.7593 0.8904 0.025 Uiso 1 1 d R . . H20B H 0.3191 0.8483 0.9204 0.025 Uiso 1 1 d R . . C21 C 0.37173(19) 0.7031(4) 0.88593(11) 0.0182(4) Uani 1 1 d . . . C22 C 0.4879(3) 0.5747(2) 0.95637(14) 0.0219(6) Uani 1 1 d . . . H22A H 0.4681 0.5257 0.9136 0.026 Uiso 1 1 calc R . . C23 C 0.4784(3) 0.5067(3) 1.02144(16) 0.0275(7) Uani 1 1 d . . . H23A H 0.4125 0.4810 1.0158 0.041 Uiso 1 1 d R . . H23B H 0.4956 0.5537 1.0640 0.041 Uiso 1 1 d R . . H23C H 0.5211 0.4417 1.0264 0.041 Uiso 1 1 d R . . C29 C 0.6491(6) 0.5470(5) 0.9315(5) 0.103(3) Uani 1 1 d . . . H29A H 0.6256 0.4789 0.9087 0.124 Uiso 1 1 d R . . C24 C 0.5887(3) 0.6130(3) 0.95961(16) 0.0268(7) Uani 1 1 d . . . C25 C 0.6265(3) 0.7108(5) 0.9918(2) 0.0440(9) Uani 1 1 d . . . H25A H 0.5878 0.7582 1.0133 0.053 Uiso 1 1 d R . . C26 C 0.7205(4) 0.7415(4) 0.9936(3) 0.0533(12) Uani 1 1 d . . . H26A H 0.7442 0.8102 1.0153 0.064 Uiso 1 1 d R . . C27 C 0.7775(4) 0.6762(5) 0.9649(4) 0.0727(19) Uani 1 1 d . . . H27A H 0.8408 0.6988 0.9648 0.087 Uiso 1 1 d R . . C28 C 0.7426(6) 0.5757(7) 0.9357(6) 0.133(4) Uani 1 1 d . . . H28A H 0.7834 0.5255 0.9182 0.160 Uiso 1 1 d R . . C30 C 0.5342(2) 0.7678(3) 0.75951(15) 0.0228(6) Uani 1 1 d . . . H30A H 0.5498 0.7384 0.8088 0.027 Uiso 1 1 d R . . H30B H 0.5879 0.8133 0.7512 0.027 Uiso 1 1 d R . . C31 C 0.5171(2) 0.6690(2) 0.70864(14) 0.0206(6) Uani 1 1 d . . . C32 C 0.5853(3) 0.5247(3) 0.64398(16) 0.0257(7) Uani 1 1 d . . . H32A H 0.5443 0.4686 0.6615 0.031 Uiso 1 1 calc R . . C33 C 0.6841(3) 0.4737(4) 0.6504(2) 0.0372(9) Uani 1 1 d . . . H33A H 0.7114 0.4555 0.7002 0.056 Uiso 1 1 d R . . H33B H 0.7253 0.5277 0.6332 0.056 Uiso 1 1 d R . . H33C H 0.6790 0.4052 0.6217 0.056 Uiso 1 1 d R . . C34 C 0.5385(3) 0.5544(3) 0.56744(16) 0.0236(6) Uani 1 1 d . . . C35 C 0.5725(3) 0.6425(3) 0.53164(18) 0.0291(7) Uani 1 1 d . . . H35A H 0.6257 0.6854 0.5552 0.035 Uiso 1 1 d R . . C36 C 0.5280(3) 0.6674(3) 0.46122(19) 0.0340(9) Uani 1 1 d . . . H36A H 0.5516 0.7267 0.4371 0.041 Uiso 1 1 d R . . C37 C 0.4501(3) 0.6064(3) 0.42666(17) 0.0342(9) Uani 1 1 d . . . H37A H 0.4196 0.6244 0.3791 0.041 Uiso 1 1 d R . . C38 C 0.4165(3) 0.5189(3) 0.46133(17) 0.0308(7) Uani 1 1 d . . . H38A H 0.3635 0.4761 0.4373 0.037 Uiso 1 1 d R . . C39 C 0.4604(3) 0.4931(3) 0.53151(17) 0.0266(7) Uani 1 1 d . . . H39A H 0.4367 0.4330 0.5550 0.032 Uiso 1 1 d R . . C40 C 0.3115(2) 0.7365(2) 0.54670(13) 0.0175(6) Uani 1 1 d . . . H40A H 0.3712 0.6979 0.5449 0.021 Uiso 1 1 d R . . H40B H 0.2910 0.7790 0.5017 0.021 Uiso 1 1 d R . . C41 C 0.2391(2) 0.6482(2) 0.55377(14) 0.0159(5) Uani 1 1 d . . . C42 C 0.1292(2) 0.5018(2) 0.50009(14) 0.0186(6) Uani 1 1 d . . . H42A H 0.1611 0.4522 0.5400 0.022 Uiso 1 1 calc R . . C43 C 0.1151(3) 0.4348(3) 0.43135(16) 0.0267(7) Uani 1 1 d . . . H43A H 0.1773 0.4104 0.4238 0.040 Uiso 1 1 d R . . H43B H 0.0836 0.4818 0.3914 0.040 Uiso 1 1 d R . . H43C H 0.0756 0.3689 0.4346 0.040 Uiso 1 1 d R . . C44 C 0.0364(2) 0.5421(2) 0.51594(14) 0.0191(6) Uani 1 1 d . . . C45 C -0.0165(3) 0.6268(3) 0.47516(15) 0.0241(6) Uani 1 1 d . . . H45A H 0.0069 0.6611 0.4379 0.029 Uiso 1 1 d R . . C46 C -0.1031(3) 0.6610(3) 0.48872(17) 0.0269(7) Uani 1 1 d . . . H46A H -0.1389 0.7183 0.4607 0.032 Uiso 1 1 d R . . C47 C -0.1374(3) 0.6111(3) 0.54377(18) 0.0301(7) Uani 1 1 d . . . H47A H -0.1962 0.6349 0.5537 0.036 Uiso 1 1 d R . . C48 C -0.0850(3) 0.5264(3) 0.58407(18) 0.0287(7) Uani 1 1 d . . . H48A H -0.1084 0.4917 0.6212 0.034 Uiso 1 1 d R . . C49 C 0.0008(3) 0.4926(3) 0.57017(15) 0.0249(7) Uani 1 1 d . . . H49A H 0.0362 0.4349 0.5981 0.030 Uiso 1 1 d R . . S1 S 0.50003(7) 0.28019(7) 0.83957(4) 0.02674(17) Uani 1 1 d . . . O11 O 0.4623(2) 0.3888(2) 0.81532(14) 0.0408(7) Uani 1 1 d . . . O12 O 0.5538(2) 0.2779(2) 0.91197(12) 0.0376(6) Uani 1 1 d . . . O13 O 0.4356(2) 0.1874(3) 0.81915(13) 0.0433(7) Uani 1 1 d . . . C1S C 0.5918(4) 0.2567(4) 0.7887(2) 0.0437(11) Uani 1 1 d . . . F11 F 0.6314(3) 0.1578(3) 0.8032(2) 0.0850(13) Uani 1 1 d . . . F12 F 0.5530(3) 0.2621(3) 0.71892(13) 0.0718(10) Uani 1 1 d . . . F13 F 0.6595(3) 0.3345(3) 0.80394(16) 0.0634(8) Uani 1 1 d . . . S2 S 0.06958(7) 0.28118(7) 0.73057(4) 0.02756(17) Uani 1 1 d . . . O21 O -0.0307(2) 0.3058(3) 0.70895(16) 0.0437(7) Uani 1 1 d . . . O22 O 0.1302(2) 0.3779(2) 0.74336(15) 0.0400(7) Uani 1 1 d . . . O23 O 0.1026(2) 0.1926(3) 0.69046(12) 0.0392(6) Uani 1 1 d . . . C2S C 0.0820(4) 0.2178(3) 0.81840(19) 0.0428(11) Uani 1 1 d . . . F21 F 0.0279(3) 0.1283(2) 0.81582(18) 0.0695(9) Uani 1 1 d . . . F22 F 0.0593(3) 0.2906(2) 0.86477(14) 0.0637(9) Uani 1 1 d . . . F23 F 0.1720(2) 0.1866(3) 0.84304(12) 0.0648(9) Uani 1 1 d . . . S3 S 0.80157(7) 0.86312(8) 0.74238(4) 0.03060(18) Uani 1 1 d . . . O31 O 0.7392(2) 0.9315(3) 0.69035(14) 0.0532(9) Uani 1 1 d . . . O32 O 0.7666(2) 0.7523(3) 0.75446(16) 0.0464(7) Uani 1 1 d . . . O33 O 0.9002(2) 0.8633(3) 0.73873(14) 0.0403(7) Uani 1 1 d . . . C3S C 0.8000(3) 0.9384(3) 0.82492(19) 0.0323(8) Uani 1 1 d . . . F31 F 0.8263(2) 1.0449(2) 0.82062(18) 0.0602(8) Uani 1 1 d . . . F32 F 0.8597(2) 0.8935(3) 0.88026(12) 0.0528(7) Uani 1 1 d . . . F33 F 0.71289(18) 0.9384(2) 0.83819(12) 0.0384(5) Uani 1 1 d . . . O1W O 0.3099(2) 0.3515(2) 0.60278(13) 0.0381(6) Uani 1 1 d . . . H1W1 H 0.3034 0.2966 0.6285 0.09(2) Uiso 1 1 d R . . H2W1 H 0.3066 0.4080 0.6281 0.10(2) Uiso 1 1 d R . . O2W O 0.2963(2) 0.1624(2) 0.68946(13) 0.0335(6) Uani 1 1 d . . . H1W2 H 0.2401 0.1716 0.6939 0.040(9) Uiso 1 1 d R . . H2W2 H 0.3345 0.1750 0.7283 0.040(9) Uiso 1 1 d R . . O3W O -0.1984(2) 0.1715(2) 0.64429(12) 0.0391(7) Uani 1 1 d . . . H1W3 H -0.1472 0.1996 0.6669 0.062(14) Uiso 1 1 d R . . H2W3 H -0.2066 0.1222 0.6735 0.067(18) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu 0.01527(5) 0.01296(4) 0.00922(4) -0.00029(5) -0.00016(3) 0.00114(6) O1 0.0154(11) 0.0167(10) 0.0173(9) 0.0019(7) 0.0019(7) 0.0036(8) O2 0.0222(12) 0.0203(8) 0.0112(8) 0.0004(7) -0.0012(7) 0.0044(8) O3 0.0119(11) 0.0215(10) 0.0166(9) 0.0003(7) 0.0008(7) 0.0015(8) O4 0.0199(12) 0.0157(8) 0.0109(8) 0.0000(6) 0.0016(7) -0.0007(8) O5 0.0209(13) 0.0155(9) 0.0183(9) 0.0027(7) 0.0006(8) 0.0007(8) N1 0.0126(13) 0.0163(10) 0.0098(9) -0.0001(8) -0.0004(8) 0.0020(9) N2 0.0229(15) 0.0158(11) 0.0115(10) -0.0013(8) 0.0005(8) 0.0005(10) N3 0.0124(13) 0.0201(11) 0.0158(10) -0.0039(8) 0.0001(8) -0.0015(10) N4 0.0203(14) 0.0151(10) 0.0120(9) 0.0002(8) 0.0013(8) -0.0008(10) N11 0.0201(15) 0.0241(12) 0.0188(11) 0.0044(9) 0.0071(9) 0.0022(11) N21 0.0292(16) 0.0213(12) 0.0124(10) -0.0020(7) -0.0025(9) 0.0040(10) N31 0.0120(14) 0.0282(13) 0.0255(12) -0.0038(10) 0.0022(9) 0.0013(11) N41 0.0190(14) 0.0217(11) 0.0116(10) -0.0017(8) 0.0021(8) -0.0027(10) C1 0.0225(17) 0.0137(12) 0.0168(12) -0.0010(9) 0.0006(10) 0.0051(11) C2 0.0201(16) 0.0177(12) 0.0159(12) -0.0035(9) 0.0013(10) 0.0025(11) C3 0.0239(17) 0.0176(12) 0.0160(12) -0.0043(10) 0.0005(10) -0.0017(12) C4 0.0264(18) 0.0191(13) 0.0146(12) -0.0061(10) -0.0020(10) -0.0016(12) C5 0.0240(18) 0.0198(13) 0.0186(13) 0.0006(10) 0.0022(11) -0.0054(12) C6 0.0148(15) 0.0202(13) 0.0192(12) 0.0012(10) 0.0038(10) -0.0037(11) C7 0.0195(16) 0.0160(12) 0.0171(12) 0.0036(9) 0.0018(10) 0.0027(11) C8 0.0244(17) 0.0174(12) 0.0108(11) 0.0044(9) -0.0008(10) 0.0031(11) C10 0.0185(16) 0.0175(12) 0.0134(11) 0.0005(9) 0.0012(9) 0.0015(11) C11 0.0265(16) 0.0111(16) 0.0146(10) -0.0018(8) 0.0035(9) 0.0001(10) C12 0.030(2) 0.0239(15) 0.0244(14) 0.0079(11) 0.0105(12) 0.0059(13) C13 0.036(2) 0.0344(18) 0.0408(19) 0.0091(15) 0.0187(16) -0.0018(17) C14 0.032(2) 0.0361(18) 0.0225(15) 0.0074(13) 0.0101(13) 0.0015(16) C15 0.044(3) 0.048(2) 0.0251(16) -0.0045(14) 0.0072(15) 0.0110(18) C16 0.067(4) 0.066(3) 0.035(2) -0.016(2) 0.013(2) 0.012(3) C17 0.063(3) 0.094(5) 0.0220(17) -0.005(2) 0.0016(17) -0.004(3) C18 0.056(3) 0.079(4) 0.028(2) 0.023(2) 0.0004(19) 0.002(3) C19 0.042(3) 0.048(2) 0.0309(17) 0.0192(16) 0.0079(15) 0.0080(19) C20 0.0287(18) 0.0203(13) 0.0113(11) 0.0000(10) 0.0015(10) 0.0049(12) C21 0.0207(13) 0.0167(10) 0.0146(9) -0.0006(17) -0.0016(8) -0.002(2) C22 0.0315(19) 0.0175(13) 0.0128(11) 0.0013(9) -0.0039(10) 0.0061(12) C23 0.027(2) 0.0267(16) 0.0268(15) 0.0094(12) 0.0018(12) 0.0007(13) C29 0.102(6) 0.066(4) 0.178(7) -0.071(4) 0.111(6) -0.046(4) C24 0.039(2) 0.0213(15) 0.0203(13) 0.0043(11) 0.0070(12) 0.0025(14) C25 0.030(2) 0.044(2) 0.056(2) -0.020(3) 0.0044(14) -0.003(3) C26 0.042(3) 0.046(2) 0.068(3) -0.007(2) 0.003(2) -0.010(2) C27 0.049(4) 0.062(4) 0.123(5) -0.004(3) 0.053(3) -0.016(3) C28 0.111(7) 0.086(5) 0.248(11) -0.087(6) 0.139(8) -0.046(5) C30 0.0203(17) 0.0249(15) 0.0209(13) -0.0054(11) -0.0005(11) 0.0014(12) C31 0.0239(17) 0.0197(13) 0.0166(12) 0.0020(9) 0.0013(10) 0.0024(11) C32 0.0272(19) 0.0238(14) 0.0264(14) 0.0009(11) 0.0068(12) 0.0076(13) C33 0.033(2) 0.043(2) 0.0373(18) 0.0063(16) 0.0114(16) 0.0186(18) C34 0.0288(19) 0.0182(13) 0.0258(14) -0.0004(11) 0.0102(12) 0.0062(13) C35 0.033(2) 0.0225(16) 0.0343(16) 0.0013(12) 0.0125(14) 0.0021(14) C36 0.046(3) 0.0273(16) 0.0351(17) 0.0066(12) 0.0224(16) 0.0078(15) C37 0.044(2) 0.0372(19) 0.0227(15) 0.0014(13) 0.0104(14) 0.0174(18) C38 0.030(2) 0.0340(17) 0.0291(16) -0.0108(13) 0.0072(13) 0.0056(15) C39 0.033(2) 0.0200(14) 0.0291(15) -0.0030(11) 0.0107(13) 0.0020(13) C40 0.0213(16) 0.0200(12) 0.0107(10) -0.0020(8) 0.0024(9) -0.0020(10) C41 0.0154(16) 0.0191(13) 0.0127(11) 0.0006(9) 0.0018(9) 0.0051(11) C42 0.0201(16) 0.0204(13) 0.0141(11) -0.0017(10) 0.0012(10) -0.0022(12) C43 0.032(2) 0.0272(15) 0.0191(14) -0.0098(11) 0.0022(12) -0.0055(15) C44 0.0235(17) 0.0179(13) 0.0142(11) -0.0044(10) 0.0009(10) -0.0046(12) C45 0.0288(19) 0.0220(13) 0.0192(13) -0.0003(10) 0.0004(11) -0.0025(13) C46 0.0202(18) 0.0259(13) 0.0318(15) 0.0004(11) -0.0001(12) 0.0025(13) C47 0.0195(18) 0.0331(17) 0.0381(17) -0.0076(14) 0.0069(13) -0.0002(14) C48 0.025(2) 0.0339(17) 0.0291(16) 0.0001(13) 0.0097(13) -0.0059(15) C49 0.0293(19) 0.0262(15) 0.0181(13) 0.0007(11) 0.0032(11) -0.0016(13) S1 0.0334(5) 0.0210(3) 0.0211(3) 0.0014(3) -0.0041(3) 0.0034(3) O11 0.0461(19) 0.0260(12) 0.0405(14) -0.0035(10) -0.0115(12) 0.0132(12) O12 0.0441(18) 0.0426(14) 0.0206(11) 0.0091(10) -0.0048(10) -0.0094(13) O13 0.0476(17) 0.0314(17) 0.0432(12) 0.0022(12) -0.0068(10) -0.0078(14) C1S 0.063(3) 0.031(2) 0.038(2) -0.0025(16) 0.016(2) 0.010(2) F11 0.091(3) 0.0550(19) 0.117(3) 0.0008(18) 0.040(2) 0.041(2) F12 0.117(3) 0.0710(19) 0.0318(12) -0.0156(12) 0.0256(15) -0.0051(19) F13 0.064(2) 0.075(2) 0.0596(16) -0.0033(14) 0.0302(15) -0.0141(17) S2 0.0316(5) 0.0229(3) 0.0277(4) -0.0010(3) 0.0054(3) -0.0006(3) O21 0.0322(18) 0.0475(16) 0.0487(16) 0.0068(12) 0.0031(12) 0.0049(13) O22 0.0436(19) 0.0302(13) 0.0495(15) -0.0070(11) 0.0176(13) -0.0077(12) O23 0.0464(16) 0.0336(14) 0.0367(11) -0.0110(14) 0.0070(9) 0.0021(17) C2S 0.067(3) 0.026(3) 0.0361(16) 0.0073(15) 0.0133(16) 0.009(2) F21 0.099(3) 0.0377(14) 0.080(2) 0.0207(14) 0.037(2) -0.0045(16) F22 0.111(3) 0.0472(15) 0.0393(13) 0.0067(11) 0.0305(16) 0.0236(17) F23 0.078(2) 0.058(2) 0.0459(12) 0.0007(14) -0.0135(11) 0.0276(18) S3 0.0261(5) 0.0449(5) 0.0214(3) 0.0033(3) 0.0063(3) 0.0117(4) O31 0.044(2) 0.089(2) 0.0278(13) 0.0169(14) 0.0094(12) 0.0344(19) O32 0.0349(18) 0.0501(16) 0.0522(16) -0.0214(13) 0.0049(13) 0.0008(14) O33 0.0313(17) 0.0563(17) 0.0373(13) 0.0099(12) 0.0163(11) 0.0135(14) C3S 0.027(2) 0.0362(18) 0.0349(17) -0.0010(14) 0.0088(14) 0.0047(15) F31 0.053(2) 0.0391(14) 0.094(2) -0.0148(14) 0.0272(16) -0.0071(13) F32 0.0453(17) 0.0747(18) 0.0333(11) -0.0084(11) -0.0024(10) 0.0219(14) F33 0.0343(14) 0.0444(12) 0.0401(11) -0.0065(9) 0.0162(9) 0.0046(11) O1W 0.053(2) 0.0332(13) 0.0310(12) 0.0004(11) 0.0153(12) 0.0000(13) O2W 0.0381(17) 0.0257(11) 0.0332(12) 0.0001(9) 0.0001(10) -0.0020(11) O3W 0.0444(18) 0.0490(19) 0.0217(10) -0.0027(10) 0.0027(10) 0.0039(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu O2 2.2725(18) . ? Lu O4 2.2727(18) . ? Lu O3 2.283(2) . ? Lu O1 2.292(2) . ? Lu O5 2.426(2) . ? Lu N1 2.592(2) . ? Lu N3 2.623(3) . ? Lu N4 2.623(2) . ? Lu N2 2.636(2) . ? O1 C11 1.248(4) . ? O2 C21 1.257(3) . ? O3 C31 1.238(4) . ? O4 C41 1.256(3) . ? N1 C10 1.475(4) . ? N1 C1 1.495(3) . ? N1 C8 1.499(3) . ? N2 C2 1.472(4) . ? N2 C20 1.483(3) . ? N2 C3 1.492(4) . ? N3 C30 1.473(4) . ? N3 C4 1.495(3) . ? N3 C5 1.499(4) . ? N4 C6 1.477(4) . ? N4 C40 1.482(3) . ? N4 C7 1.499(4) . ? N11 C11 1.334(4) . ? N11 C12 1.477(4) . ? N21 C21 1.328(3) . ? N21 C22 1.478(4) . ? N31 C31 1.342(4) . ? N31 C32 1.480(4) . ? N41 C41 1.321(4) . ? N41 C42 1.475(4) . ? C1 C2 1.530(4) . ? C3 C4 1.510(5) . ? C5 C6 1.526(4) . ? C7 C8 1.505(4) . ? C10 C11 1.520(3) . ? C12 C13 1.518(5) . ? C12 C14 1.520(5) . ? C14 C15 1.388(5) . ? C14 C19 1.400(5) . ? C15 C16 1.405(6) . ? C16 C17 1.385(7) . ? C17 C18 1.366(8) . ? C18 C19 1.401(7) . ? C20 C21 1.504(5) . ? C22 C24 1.509(5) . ? C22 C23 1.526(4) . ? C29 C24 1.369(6) . ? C29 C28 1.374(10) . ? C24 C25 1.376(6) . ? C25 C26 1.393(6) . ? C26 C27 1.336(7) . ? C27 C28 1.372(9) . ? C30 C31 1.519(4) . ? C32 C34 1.524(4) . ? C32 C33 1.525(5) . ? C34 C39 1.390(5) . ? C34 C35 1.404(4) . ? C35 C36 1.400(5) . ? C36 C37 1.378(6) . ? C37 C38 1.383(6) . ? C38 C39 1.397(5) . ? C40 C41 1.509(4) . ? C42 C44 1.512(5) . ? C42 C43 1.524(4) . ? C44 C49 1.393(4) . ? C44 C45 1.399(4) . ? C45 C46 1.388(5) . ? C46 C47 1.399(5) . ? C47 C48 1.391(5) . ? C48 C49 1.381(5) . ? S1 O12 1.440(2) . ? S1 O13 1.442(3) . ? S1 O11 1.443(3) . ? S1 C1S 1.832(5) . ? C1S F11 1.314(5) . ? C1S F13 1.331(6) . ? C1S F12 1.340(5) . ? S2 O22 1.435(3) . ? S2 O21 1.442(3) . ? S2 O23 1.450(3) . ? S2 C2S 1.828(4) . ? C2S F21 1.316(5) . ? C2S F23 1.330(5) . ? C2S F22 1.337(5) . ? S3 O33 1.436(3) . ? S3 O31 1.443(3) . ? S3 O32 1.452(3) . ? S3 C3S 1.832(4) . ? C3S F32 1.327(4) . ? C3S F31 1.333(5) . ? C3S F33 1.333(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 O2 Lu O4 142.70(7) . . ? O2 Lu O3 83.12(7) . . ? O4 Lu O3 83.47(7) . . ? O2 Lu O1 83.23(8) . . ? O4 Lu O1 85.58(7) . . ? O3 Lu O1 140.80(7) . . ? O2 Lu O5 72.38(7) . . ? O4 Lu O5 70.35(7) . . ? O3 Lu O5 70.99(7) . . ? O1 Lu O5 69.88(7) . . ? O2 Lu N1 132.00(7) . . ? O4 Lu N1 74.41(7) . . ? O3 Lu N1 142.30(7) . . ? O1 Lu N1 68.14(7) . . ? O5 Lu N1 126.25(8) . . ? O2 Lu N3 72.86(8) . . ? O4 Lu N3 131.79(7) . . ? O3 Lu N3 67.56(8) . . ? O1 Lu N3 140.55(7) . . ? O5 Lu N3 128.05(8) . . ? N1 Lu N3 105.70(8) . . ? O2 Lu N4 139.72(8) . . ? O4 Lu N4 67.42(7) . . ? O3 Lu N4 73.94(8) . . ? O1 Lu N4 134.42(8) . . ? O5 Lu N4 127.11(7) . . ? N1 Lu N4 69.51(8) . . ? N3 Lu N4 67.93(7) . . ? O2 Lu N2 67.06(7) . . ? O4 Lu N2 141.65(8) . . ? O3 Lu N2 132.48(8) . . ? O1 Lu N2 73.27(8) . . ? O5 Lu N2 127.35(7) . . ? N1 Lu N2 68.16(7) . . ? N3 Lu N2 68.68(8) . . ? N4 Lu N2 105.54(7) . . ? C11 O1 Lu 122.86(17) . . ? C21 O2 Lu 125.2(2) . . ? C31 O3 Lu 123.79(19) . . ? C41 O4 Lu 125.01(19) . . ? C10 N1 C1 109.3(2) . . ? C10 N1 C8 109.5(2) . . ? C1 N1 C8 108.2(2) . . ? C10 N1 Lu 105.63(16) . . ? C1 N1 Lu 113.27(16) . . ? C8 N1 Lu 110.96(17) . . ? C2 N2 C20 109.5(2) . . ? C2 N2 C3 108.7(2) . . ? C20 N2 C3 110.3(2) . . ? C2 N2 Lu 111.67(15) . . ? C20 N2 Lu 106.39(16) . . ? C3 N2 Lu 110.28(17) . . ? C30 N3 C4 109.4(2) . . ? C30 N3 C5 110.3(2) . . ? C4 N3 C5 107.5(2) . . ? C30 N3 Lu 105.59(17) . . ? C4 N3 Lu 111.52(19) . . ? C5 N3 Lu 112.55(17) . . ? C6 N4 C40 108.9(2) . . ? C6 N4 C7 109.4(2) . . ? C40 N4 C7 109.4(2) . . ? C6 N4 Lu 112.56(16) . . ? C40 N4 Lu 106.58(16) . . ? C7 N4 Lu 109.93(16) . . ? C11 N11 C12 122.5(3) . . ? C21 N21 C22 121.3(3) . . ? C31 N31 C32 120.7(3) . . ? C41 N41 C42 120.6(2) . . ? N1 C1 C2 111.8(2) . . ? N2 C2 C1 111.3(2) . . ? N2 C3 C4 113.0(2) . . ? N3 C4 C3 111.0(2) . . ? N3 C5 C6 112.0(2) . . ? N4 C6 C5 111.2(2) . . ? N4 C7 C8 113.1(2) . . ? N1 C8 C7 111.3(2) . . ? N1 C10 C11 109.6(2) . . ? O1 C11 N11 122.5(2) . . ? O1 C11 C10 119.9(3) . . ? N11 C11 C10 117.6(3) . . ? N11 C12 C13 108.7(3) . . ? N11 C12 C14 111.4(3) . . ? C13 C12 C14 112.4(3) . . ? C15 C14 C19 118.8(4) . . ? C15 C14 C12 121.1(4) . . ? C19 C14 C12 120.1(4) . . ? C14 C15 C16 120.5(4) . . ? C17 C16 C15 119.6(5) . . ? C18 C17 C16 120.6(5) . . ? C17 C18 C19 120.2(5) . . ? C14 C19 C18 120.3(4) . . ? N2 C20 C21 110.4(2) . . ? O2 C21 N21 121.0(3) . . ? O2 C21 C20 120.1(2) . . ? N21 C21 C20 118.8(3) . . ? N21 C22 C24 112.3(3) . . ? N21 C22 C23 107.9(3) . . ? C24 C22 C23 112.7(3) . . ? C24 C29 C28 122.1(5) . . ? C29 C24 C25 116.3(4) . . ? C29 C24 C22 119.8(4) . . ? C25 C24 C22 123.8(3) . . ? C24 C25 C26 121.3(4) . . ? C27 C26 C25 121.1(5) . . ? C26 C27 C28 118.5(6) . . ? C27 C28 C29 120.5(6) . . ? N3 C30 C31 110.1(3) . . ? O3 C31 N31 122.6(3) . . ? O3 C31 C30 120.7(3) . . ? N31 C31 C30 116.7(3) . . ? N31 C32 C34 111.0(2) . . ? N31 C32 C33 108.6(3) . . ? C34 C32 C33 112.1(3) . . ? C39 C34 C35 118.7(3) . . ? C39 C34 C32 119.8(3) . . ? C35 C34 C32 121.5(3) . . ? C36 C35 C34 120.1(4) . . ? C37 C36 C35 120.5(3) . . ? C36 C37 C38 119.9(3) . . ? C37 C38 C39 120.2(4) . . ? C34 C39 C38 120.7(3) . . ? N4 C40 C41 110.4(2) . . ? O4 C41 N41 121.7(3) . . ? O4 C41 C40 120.0(2) . . ? N41 C41 C40 118.2(2) . . ? N41 C42 C44 111.2(2) . . ? N41 C42 C43 108.4(2) . . ? C44 C42 C43 112.9(3) . . ? C49 C44 C45 119.0(3) . . ? C49 C44 C42 120.2(3) . . ? C45 C44 C42 120.8(3) . . ? C46 C45 C44 120.4(3) . . ? C45 C46 C47 119.9(3) . . ? C48 C47 C46 119.7(3) . . ? C49 C48 C47 120.1(3) . . ? C48 C49 C44 120.9(3) . . ? O12 S1 O13 115.22(16) . . ? O12 S1 O11 114.52(16) . . ? O13 S1 O11 115.35(18) . . ? O12 S1 C1S 102.7(2) . . ? O13 S1 C1S 103.4(2) . . ? O11 S1 C1S 103.1(2) . . ? F11 C1S F13 108.5(5) . . ? F11 C1S F12 108.8(4) . . ? F13 C1S F12 108.2(4) . . ? F11 C1S S1 110.7(4) . . ? F13 C1S S1 110.7(3) . . ? F12 C1S S1 109.9(4) . . ? O22 S2 O21 114.75(19) . . ? O22 S2 O23 114.78(18) . . ? O21 S2 O23 114.76(17) . . ? O22 S2 C2S 103.95(19) . . ? O21 S2 C2S 103.9(2) . . ? O23 S2 C2S 102.50(19) . . ? F21 C2S F23 107.9(4) . . ? F21 C2S F22 108.8(4) . . ? F23 C2S F22 107.7(4) . . ? F21 C2S S2 111.3(3) . . ? F23 C2S S2 109.7(3) . . ? F22 C2S S2 111.3(3) . . ? O33 S3 O31 115.82(19) . . ? O33 S3 O32 112.94(19) . . ? O31 S3 O32 116.2(2) . . ? O33 S3 C3S 104.05(18) . . ? O31 S3 C3S 101.70(18) . . ? O32 S3 C3S 103.69(17) . . ? F32 C3S F31 107.0(4) . . ? F32 C3S F33 108.3(3) . . ? F31 C3S F33 107.7(3) . . ? F32 C3S S3 111.8(3) . . ? F31 C3S S3 110.8(3) . . ? F33 C3S S3 111.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H051 O11 0.84 1.99 2.817(3) 167.5 . O5 H052 O22 0.84 2.11 2.947(4) 171.9 . N11 H11 O33 0.88 2.35 3.036(4) 134.5 1_455 N21 H20 O12 0.88 2.08 2.923(3) 158.7 2_657 N31 H30 O32 0.88 2.08 2.942(4) 167.4 . N41 H40 O3W 0.88 1.99 2.859(3) 171.2 2_556 O1W H1W1 O2W 0.84 2.00 2.841(4) 176.2 . O1W H2W1 O5 0.84 2.26 3.040(3) 155.2 . O2W H1W2 O23 0.84 1.98 2.814(4) 172.3 . O2W H2W2 O13 0.84 2.02 2.857(4) 172.5 . O3W H1W3 O21 0.84 2.11 2.936(4) 165.9 . O3W H2W3 O31 0.84 2.45 3.185(5) 146.6 1_445 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.650 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.085 #=============================================END data_9a _database_code_CSD 182451 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Ce N8 O5 3+,3(C F3 O3 S 1-),C2 H6 O,1.5(H2 O)' _chemical_formula_sum 'C53 H75 Ce F9 N8 O16.50 S3' _chemical_formula_weight 1495.51 _chemical_absolute_configuration ad _chemical_optical_rotation ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 32.176(8) _cell_length_b 12.754(3) _cell_length_c 33.047(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.46(1) _cell_angle_gamma 90.00 _cell_volume 13537(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7477 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6144 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 6 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 88619 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.54 _reflns_number_total 32385 _reflns_number_gt 27723 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.916 _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. Triflate anion 4 is disordered by libration around the C(4S) atom, separate positions were found only for the sulfur [S(4) 85%, S(4') 15%]. Thiflate anion 5 shows chaotic disorder, rationalised (poorly) as libration around the S(5) centre, i.e. by split (50:50) positions of C(5S), C(5S'), F(52), F(52'), all other atom having very high ADP. Ethanol and water of crystallisation share the same cavity: ethanol molecules O(2S)C(9S)C(10S) and O(3S)C(11S)C(12S) have 50% occupancies, but the O(2S) probably shares the site with a water molecule, it was refined with 75% occupancy, as were water molecules O(2W) and O(3W). The total solvent content (one EtOH and 1.5 water molecule per cation) was estimated from the cavity volume. ; _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^)+(0.0870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.036(12) _refine_ls_number_reflns 32385 _refine_ls_number_parameters 1594 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1889 _refine_ls_goodness_of_fit_ref 1.469 _refine_ls_restrained_S_all 1.469 _refine_ls_shift/su_max 0.239 _refine_ls_shift/su_mean 0.004 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 Ce1A Ce 0.505310(11) 0.37375(3) 0.304991(10) 0.01956(8) Uani 1 1 d . . . O1A O 0.54340(17) 0.2417(4) 0.34577(14) 0.0283(11) Uani 1 1 d . . . O2A O 0.44560(16) 0.3367(4) 0.34650(14) 0.0257(10) Uani 1 1 d . . . O3A O 0.47761(16) 0.5493(4) 0.29979(15) 0.0257(11) Uani 1 1 d . . . O4A O 0.57406(17) 0.4550(4) 0.29660(15) 0.0291(11) Uani 1 1 d . . . O5A O 0.52674(19) 0.4596(4) 0.37067(16) 0.0349(13) Uani 1 1 d . . . H01A H 0.5469 0.4387 0.3859 0.052 Uiso 1 1 d R . . H02A H 0.5263 0.5242 0.3754 0.052 Uiso 1 1 d R . . N1A N 0.54968(19) 0.2290(5) 0.26184(19) 0.0268(13) Uani 1 1 d . . . N2A N 0.46396(19) 0.1874(5) 0.28828(18) 0.0235(12) Uani 1 1 d . . . N3A N 0.43392(18) 0.3967(4) 0.25475(17) 0.0222(12) Uani 1 1 d . . . N4A N 0.51978(17) 0.4400(5) 0.22726(17) 0.0222(12) Uani 1 1 d . . . N11A N 0.5868(2) 0.1077(5) 0.3579(2) 0.0331(14) Uani 1 1 d . . . H11A H 0.6032 0.0597 0.3483 0.040 Uiso 1 1 d R . . N21A N 0.3936(2) 0.2341(5) 0.36786(19) 0.0279(13) Uani 1 1 d . . . H21A H 0.3807 0.1734 0.3656 0.034 Uiso 1 1 d R . . N31A N 0.4304(2) 0.6732(5) 0.2812(2) 0.0293(14) Uani 1 1 d . . . H31A H 0.4059 0.6880 0.2693 0.035 Uiso 1 1 d R . . N41A N 0.62169(19) 0.5389(5) 0.26048(18) 0.0283(13) Uani 1 1 d . . . H41A H 0.6276 0.5650 0.2369 0.034 Uiso 1 1 d R . . C1A C 0.5230(2) 0.1427(6) 0.2465(2) 0.0296(15) Uani 1 1 d . . . H11 H 0.5409 0.0840 0.2385 0.035 Uiso 1 1 d R . . H12 H 0.5067 0.1669 0.2218 0.035 Uiso 1 1 d R . . C2A C 0.4929(2) 0.1014(5) 0.2767(2) 0.0248(14) Uani 1 1 d . . . H21 H 0.5090 0.0757 0.3013 0.030 Uiso 1 1 d R . . H22 H 0.4766 0.0420 0.2648 0.030 Uiso 1 1 d R . . C3A C 0.4303(2) 0.2005(7) 0.2554(2) 0.0306(16) Uani 1 1 d . . . H31 H 0.4424 0.1951 0.2287 0.037 Uiso 1 1 d R . . H32 H 0.4102 0.1422 0.2574 0.037 Uiso 1 1 d R . . C4A C 0.4071(2) 0.3007(7) 0.2573(2) 0.0305(16) Uani 1 1 d . . . H41 H 0.3928 0.3033 0.2830 0.037 Uiso 1 1 d R . . H42 H 0.3854 0.3029 0.2347 0.037 Uiso 1 1 d R . . C5A C 0.4433(2) 0.4121(6) 0.2115(2) 0.0260(15) Uani 1 1 d . . . H51 H 0.4186 0.4432 0.1967 0.031 Uiso 1 1 d R . . H52 H 0.4484 0.3426 0.1994 0.031 Uiso 1 1 d R . . C6A C 0.4809(2) 0.4797(6) 0.20638(19) 0.0241(14) Uani 1 1 d . . . H61 H 0.4852 0.4866 0.1771 0.029 Uiso 1 1 d R . . H62 H 0.4748 0.5505 0.2168 0.029 Uiso 1 1 d R . . C7A C 0.5362(2) 0.3523(6) 0.2037(2) 0.0269(16) Uani 1 1 d . . . H71 H 0.5491 0.3811 0.1797 0.032 Uiso 1 1 d R . . H72 H 0.5126 0.3074 0.1940 0.032 Uiso 1 1 d R . . C8A C 0.5673(2) 0.2811(7) 0.2275(2) 0.0293(16) Uani 1 1 d . . . H81 H 0.5784 0.2280 0.2091 0.035 Uiso 1 1 d R . . H82 H 0.5908 0.3256 0.2378 0.035 Uiso 1 1 d R . . C10A C 0.5840(2) 0.1900(7) 0.2903(2) 0.0310(16) Uani 1 1 d . . . H101 H 0.6079 0.2387 0.2904 0.037 Uiso 1 1 d R . . H102 H 0.5933 0.1208 0.2809 0.037 Uiso 1 1 d R . . C11A C 0.5701(2) 0.1797(6) 0.3334(2) 0.0265(15) Uani 1 1 d . . . C12A C 0.5797(3) 0.1079(7) 0.4013(3) 0.042(2) Uani 1 1 d . . . H12A H 0.5843 0.1808 0.4118 0.051 Uiso 1 1 calc R . . C13A C 0.6111(3) 0.0363(10) 0.4233(3) 0.051(3) Uani 1 1 d . . . H131 H 0.6394 0.0592 0.4180 0.077 Uiso 1 1 calc R . . H132 H 0.6069 -0.0358 0.4137 0.077 Uiso 1 1 calc R . . H133 H 0.6075 0.0391 0.4525 0.077 Uiso 1 1 calc R . . C14A C 0.5362(3) 0.0767(7) 0.4085(2) 0.0363(18) Uani 1 1 d . . . C15A C 0.5189(3) -0.0155(9) 0.3949(3) 0.049(2) Uani 1 1 d . . . H15A H 0.5353 -0.0612 0.3798 0.058 Uiso 1 1 d R . . C16A C 0.4790(4) -0.0449(12) 0.4028(3) 0.069(4) Uani 1 1 d . . . H16A H 0.4672 -0.1088 0.3928 0.082 Uiso 1 1 d R . . C17A C 0.4554(4) 0.0196(17) 0.4249(4) 0.081(5) Uani 1 1 d . . . H17A H 0.4282 0.0000 0.4317 0.097 Uiso 1 1 d R . . C18A C 0.4695(5) 0.112(2) 0.4391(4) 0.103(7) Uani 1 1 d . . . H18A H 0.4526 0.1591 0.4531 0.124 Uiso 1 1 d R . . C19A C 0.5109(4) 0.1399(14) 0.4315(3) 0.074(4) Uani 1 1 d . . . H19A H 0.5226 0.2033 0.4422 0.088 Uiso 1 1 d R . . C20A C 0.4446(2) 0.1550(5) 0.3263(2) 0.0234(14) Uani 1 1 d . . . H201 H 0.4659 0.1205 0.3446 0.028 Uiso 1 1 d R . . H202 H 0.4219 0.1040 0.3200 0.028 Uiso 1 1 d R . . C21A C 0.4276(2) 0.2501(6) 0.3477(2) 0.0252(15) Uani 1 1 d . . . C22A C 0.3772(3) 0.3155(6) 0.3948(2) 0.0324(17) Uani 1 1 d . . . H22A H 0.4010 0.3450 0.4121 0.039 Uiso 1 1 d R . . C23A C 0.3477(3) 0.2623(8) 0.4220(3) 0.050(3) Uani 1 1 d . . . H231 H 0.3622 0.2057 0.4370 0.075 Uiso 1 1 calc R . . H232 H 0.3241 0.2331 0.4055 0.075 Uiso 1 1 calc R . . H233 H 0.3374 0.3135 0.4411 0.075 Uiso 1 1 calc R . . C24A C 0.3574(3) 0.4025(6) 0.3696(2) 0.0312(17) Uani 1 1 d . . . C25A C 0.3252(3) 0.3879(8) 0.3400(3) 0.042(2) Uani 1 1 d . . . H25A H 0.3155 0.3187 0.3346 0.050 Uiso 1 1 d R . . C26A C 0.3066(3) 0.4700(9) 0.3184(3) 0.051(2) Uani 1 1 d . . . H26A H 0.2846 0.4572 0.2986 0.061 Uiso 1 1 d R . . C27A C 0.3196(3) 0.5701(9) 0.3248(3) 0.056(3) Uani 1 1 d . . . H27A H 0.3073 0.6260 0.3094 0.068 Uiso 1 1 d R . . C28A C 0.3515(3) 0.5924(8) 0.3548(3) 0.045(2) Uani 1 1 d . . . H28A H 0.3599 0.6627 0.3602 0.054 Uiso 1 1 d R . . C29A C 0.3710(3) 0.5063(7) 0.3767(3) 0.0371(18) Uani 1 1 d . . . H29A H 0.3935 0.5202 0.3958 0.045 Uiso 1 1 d R . . C30A C 0.4118(2) 0.4890(6) 0.2697(2) 0.0271(15) Uani 1 1 d . . . H301 H 0.3947 0.4683 0.2923 0.032 Uiso 1 1 d R . . H302 H 0.3929 0.5169 0.2475 0.032 Uiso 1 1 d R . . C31A C 0.4429(2) 0.5751(6) 0.2838(2) 0.0240(14) Uani 1 1 d . . . C32A C 0.4567(3) 0.7578(6) 0.2969(2) 0.0353(18) Uani 1 1 d . . . H32A H 0.4696 0.7348 0.3237 0.042 Uiso 1 1 d R . . C33A C 0.4296(3) 0.8543(7) 0.3045(3) 0.043(2) Uani 1 1 d . . . H331 H 0.4083 0.8358 0.3232 0.064 Uiso 1 1 d R . . H332 H 0.4162 0.8782 0.2787 0.064 Uiso 1 1 d R . . H333 H 0.4472 0.9107 0.3163 0.064 Uiso 1 1 d R . . C34A C 0.4916(3) 0.7825(6) 0.2696(3) 0.0350(18) Uani 1 1 d . . . C35A C 0.4829(3) 0.7931(8) 0.2277(3) 0.048(2) Uani 1 1 d . . . H35A H 0.4557 0.7830 0.2156 0.057 Uiso 1 1 d R . . C36A C 0.5177(5) 0.8207(9) 0.2042(3) 0.065(3) Uani 1 1 d . . . H36A H 0.5138 0.8271 0.1756 0.078 Uiso 1 1 d R . . C37A C 0.5574(4) 0.8288(12) 0.2234(6) 0.085(5) Uani 1 1 d . . . H37A H 0.5796 0.8470 0.2070 0.102 Uiso 1 1 d R . . C38A C 0.5638(3) 0.8229(11) 0.2608(5) 0.070(4) Uani 1 1 d . . . H38A H 0.5911 0.8341 0.2726 0.084 Uiso 1 1 d R . . C39A C 0.5329(3) 0.7977(8) 0.2863(4) 0.051(3) Uani 1 1 d . . . H39A H 0.5383 0.7892 0.3146 0.061 Uiso 1 1 d R . . C40A C 0.5503(2) 0.5271(6) 0.2314(2) 0.0270(15) Uani 1 1 d . . . H401 H 0.5361 0.5939 0.2369 0.032 Uiso 1 1 d R . . H402 H 0.5640 0.5349 0.2055 0.032 Uiso 1 1 d R . . C41A C 0.5836(2) 0.5051(6) 0.2648(2) 0.0249(15) Uani 1 1 d . . . C42A C 0.6549(2) 0.5373(6) 0.2939(2) 0.0310(16) Uani 1 1 d . . . H42A H 0.6448 0.5764 0.3176 0.037 Uiso 1 1 calc R . . C43A C 0.6935(3) 0.5929(7) 0.2794(3) 0.044(2) Uani 1 1 d . . . H431 H 0.6862 0.6648 0.2714 0.066 Uiso 1 1 calc R . . H432 H 0.7037 0.5551 0.2562 0.066 Uiso 1 1 calc R . . H433 H 0.7153 0.5942 0.3015 0.066 Uiso 1 1 calc R . . C44A C 0.6653(2) 0.4260(6) 0.3069(2) 0.0268(15) Uani 1 1 d . . . C45A C 0.6814(3) 0.3541(8) 0.2806(3) 0.042(2) Uani 1 1 d . . . H45A H 0.6841 0.3725 0.2530 0.051 Uiso 1 1 d R . . C46A C 0.6929(3) 0.2523(7) 0.2937(3) 0.0390(19) Uani 1 1 d . . . H46A H 0.7056 0.2056 0.2757 0.047 Uiso 1 1 d R . . C47A C 0.6873(3) 0.2228(8) 0.3332(3) 0.041(2) Uani 1 1 d . . . H47A H 0.6946 0.1539 0.3419 0.050 Uiso 1 1 d R . . C48A C 0.6709(3) 0.2933(7) 0.3597(2) 0.0379(19) Uani 1 1 d . . . H48A H 0.6668 0.2735 0.3869 0.046 Uiso 1 1 d R . . C49A C 0.6598(2) 0.3938(6) 0.3471(2) 0.0288(17) Uani 1 1 d . . . H49A H 0.6485 0.4423 0.3653 0.035 Uiso 1 1 d R . . Ce1B Ce 0.192024(12) 0.62667(3) 0.494038(11) 0.02737(10) Uani 1 1 d . . . O1B O 0.18536(18) 0.7230(5) 0.55678(17) 0.0357(13) Uani 1 1 d . . . O2B O 0.14250(18) 0.5010(5) 0.51873(17) 0.0367(14) Uani 1 1 d . . . O3B O 0.16227(18) 0.5773(4) 0.42753(15) 0.0310(12) Uani 1 1 d . . . O4B O 0.20602(19) 0.7954(5) 0.46525(17) 0.0365(13) Uani 1 1 d . . . O5B O 0.1226(2) 0.7125(6) 0.4854(2) 0.0499(17) Uani 1 1 d . . . H01B H 0.1069 0.7059 0.4690 0.075 Uiso 1 1 d R . . H02B H 0.1188 0.7641 0.4882 0.075 Uiso 1 1 d R . . N1B N 0.2658(2) 0.6993(7) 0.5317(3) 0.049(2) Uani 1 1 d . . . N2B N 0.2223(2) 0.4982(6) 0.5551(2) 0.0395(17) Uani 1 1 d . . . N3B N 0.2155(2) 0.4323(6) 0.4670(2) 0.0314(14) Uani 1 1 d . . . N4B N 0.2580(2) 0.6340(7) 0.4437(2) 0.0402(17) Uani 1 1 d . . . N11B N 0.2060(2) 0.8289(6) 0.6077(2) 0.0395(17) Uani 1 1 d . . . H11B H 0.2258 0.8695 0.6185 0.047 Uiso 1 1 d R . . N21B N 0.1183(3) 0.3909(8) 0.5649(2) 0.057(2) Uani 1 1 d . . . H21B H 0.1227 0.3569 0.5879 0.068 Uiso 1 1 d R . . N31B N 0.1467(2) 0.4632(6) 0.3772(2) 0.0359(16) Uani 1 1 d . . . H31B H 0.1515 0.4020 0.3661 0.043 Uiso 1 1 d R . . N41B N 0.2336(3) 0.9086(6) 0.4229(2) 0.0388(17) Uani 1 1 d . . . H41B H 0.2505 0.9200 0.4034 0.047 Uiso 1 1 d R . . C1B C 0.2851(3) 0.6165(9) 0.5603(3) 0.057(3) Uani 1 1 d . . . H1BB H 0.3044 0.6520 0.5802 0.069 Uiso 1 1 d R . . H1BC H 0.3016 0.5670 0.5446 0.069 Uiso 1 1 d R . . C2B C 0.2538(4) 0.5568(10) 0.5825(3) 0.060(3) Uani 1 1 d . . . H2BA H 0.2687 0.5057 0.6006 0.072 Uiso 1 1 d R . . H2BB H 0.2386 0.6055 0.5996 0.072 Uiso 1 1 d R . . C3B C 0.2406(3) 0.4029(7) 0.5402(3) 0.042(2) Uani 1 1 d . . . H3BA H 0.2411 0.3504 0.5623 0.050 Uiso 1 1 d R . . H3BB H 0.2699 0.4176 0.5344 0.050 Uiso 1 1 d R . . C4B C 0.2190(3) 0.3555(8) 0.5030(3) 0.044(2) Uani 1 1 d . . . H4BA H 0.2349 0.2932 0.4950 0.053 Uiso 1 1 d R . . H4BB H 0.1908 0.3321 0.5092 0.053 Uiso 1 1 d R . . C5B C 0.2553(3) 0.4372(8) 0.4482(3) 0.045(2) Uani 1 1 d . . . H5BA H 0.2584 0.3733 0.4317 0.054 Uiso 1 1 d R . . H5BB H 0.2782 0.4380 0.4696 0.054 Uiso 1 1 d R . . C6B C 0.2588(3) 0.5326(8) 0.4216(3) 0.048(2) Uani 1 1 d . . . H6BA H 0.2854 0.5283 0.4082 0.058 Uiso 1 1 d R . . H6BB H 0.2360 0.5315 0.4001 0.058 Uiso 1 1 d R . . C7B C 0.2984(3) 0.6462(10) 0.4679(4) 0.059(3) Uani 1 1 d . . . H7BA H 0.3198 0.6698 0.4497 0.071 Uiso 1 1 d R . . H7BB H 0.3075 0.5778 0.4795 0.071 Uiso 1 1 d R . . C8B C 0.2962(3) 0.7259(10) 0.5028(3) 0.057(3) Uani 1 1 d . . . H8BA H 0.3242 0.7337 0.5167 0.069 Uiso 1 1 d R . . H8BB H 0.2882 0.7948 0.4910 0.069 Uiso 1 1 d R . . C10B C 0.2545(3) 0.7925(8) 0.5548(3) 0.044(2) Uani 1 1 d . . . H10D H 0.2761 0.8076 0.5767 0.053 Uiso 1 1 d R . . H10E H 0.2529 0.8534 0.5362 0.053 Uiso 1 1 d R . . C11B C 0.2126(3) 0.7776(6) 0.5738(2) 0.0346(18) Uani 1 1 d . . . C12B C 0.1661(3) 0.8175(8) 0.6281(3) 0.041(2) Uani 1 1 d . . . H12B H 0.1427 0.8291 0.6073 0.050 Uiso 1 1 d R . . C13B C 0.1648(4) 0.9047(8) 0.6587(3) 0.052(3) Uani 1 1 d . . . H13D H 0.1387 0.9011 0.6725 0.078 Uiso 1 1 d R . . H13E H 0.1666 0.9724 0.6449 0.078 Uiso 1 1 d R . . H13F H 0.1884 0.8973 0.6787 0.078 Uiso 1 1 d R . . C14B C 0.1607(4) 0.7142(8) 0.6460(3) 0.051(2) Uani 1 1 d . . . C15B C 0.1950(4) 0.6703(9) 0.6702(3) 0.053(3) Uani 1 1 d . . . H15B H 0.2210 0.7055 0.6738 0.063 Uiso 1 1 d R . . C16B C 0.1906(4) 0.5770(10) 0.6890(3) 0.062(3) Uani 1 1 d . . . H16B H 0.2125 0.5469 0.7058 0.074 Uiso 1 1 d R . . C17B C 0.1532(6) 0.5268(12) 0.6840(4) 0.084(5) Uani 1 1 d . . . H17B H 0.1505 0.4609 0.6970 0.101 Uiso 1 1 d R . . C18B C 0.1194(4) 0.5640(11) 0.6602(4) 0.067(3) Uani 1 1 d . . . H18B H 0.0936 0.5274 0.6571 0.080 Uiso 1 1 d R . . C19B C 0.1239(4) 0.6589(10) 0.6407(3) 0.058(3) Uani 1 1 d . . . H19B H 0.1019 0.6857 0.6232 0.069 Uiso 1 1 d R . . C20B C 0.1863(3) 0.4738(8) 0.5795(3) 0.049(2) Uani 1 1 d . . . H20D H 0.1812 0.5321 0.5983 0.058 Uiso 1 1 d R . . H20E H 0.1927 0.4101 0.5959 0.058 Uiso 1 1 d R . . C21B C 0.1473(3) 0.4534(8) 0.5518(3) 0.047(2) Uani 1 1 d . . . C22B C 0.0779(3) 0.3775(11) 0.5418(3) 0.059(3) Uani 1 1 d . . . H22B H 0.0654 0.4478 0.5352 0.071 Uiso 1 1 d R . . C23B C 0.0498(4) 0.3138(13) 0.5690(4) 0.077(4) Uani 1 1 d . . . H23D H 0.0459 0.3529 0.5940 0.116 Uiso 1 1 d R . . H23E H 0.0628 0.2460 0.5757 0.116 Uiso 1 1 d R . . H23F H 0.0227 0.3022 0.5545 0.116 Uiso 1 1 d R . . C24B C 0.0844(3) 0.3160(11) 0.5028(3) 0.060(3) Uani 1 1 d . . . C25B C 0.1051(3) 0.2252(12) 0.5028(4) 0.067(4) Uani 1 1 d . . . H25B H 0.1154 0.1962 0.5280 0.080 Uiso 1 1 d R . . C26B C 0.1110(4) 0.1691(14) 0.4665(5) 0.084(4) Uani 1 1 d . . . H26B H 0.1249 0.1034 0.4668 0.101 Uiso 1 1 d R . . C27B C 0.0959(4) 0.2102(14) 0.4323(5) 0.075(4) Uani 1 1 d . . . H27B H 0.0990 0.1738 0.4076 0.090 Uiso 1 1 d R . . C28B C 0.0726(4) 0.3079(16) 0.4303(5) 0.093(6) Uani 1 1 d . . . H28B H 0.0618 0.3359 0.4052 0.112 Uiso 1 1 d R . . C29B C 0.0690(3) 0.3615(14) 0.4666(4) 0.078(4) Uani 1 1 d . . . H29B H 0.0557 0.4281 0.4664 0.093 Uiso 1 1 d R . . C30B C 0.1813(3) 0.3970(6) 0.4376(2) 0.0345(18) Uani 1 1 d . . . H30D H 0.1590 0.3646 0.4528 0.041 Uiso 1 1 d R . . H30E H 0.1920 0.3428 0.4195 0.041 Uiso 1 1 d R . . C31B C 0.1629(3) 0.4851(7) 0.4128(2) 0.0328(17) Uani 1 1 d . . . C32B C 0.1213(3) 0.5428(7) 0.3539(2) 0.0366(19) Uani 1 1 d . . . H32B H 0.1016 0.5747 0.3727 0.044 Uiso 1 1 d R . . C33B C 0.0952(3) 0.4871(6) 0.3197(3) 0.044(2) Uani 1 1 d . . . H33D H 0.0784 0.4318 0.3313 0.066 Uiso 1 1 d R . . H33E H 0.1138 0.4560 0.3006 0.066 Uiso 1 1 d R . . H33F H 0.0768 0.5379 0.3054 0.066 Uiso 1 1 d R . . C34B C 0.1489(3) 0.6319(7) 0.3379(2) 0.0392(18) Uani 1 1 d . . . C35B C 0.1802(4) 0.6079(12) 0.3113(3) 0.072(4) Uani 1 1 d . . . H35B H 0.1847 0.5380 0.3026 0.086 Uiso 1 1 d R . . C36B C 0.2043(4) 0.6903(16) 0.2992(4) 0.084(5) Uani 1 1 d . . . H36B H 0.2265 0.6770 0.2822 0.100 Uiso 1 1 d R . . C37B C 0.1940(5) 0.7978(15) 0.3122(5) 0.097(7) Uani 1 1 d . . . H37B H 0.2087 0.8551 0.3014 0.116 Uiso 1 1 d R . . C38B C 0.1676(5) 0.8150(10) 0.3360(4) 0.072(4) Uani 1 1 d . . . H38B H 0.1643 0.8848 0.3453 0.086 Uiso 1 1 d R . . C39B C 0.1429(4) 0.7347(8) 0.3508(3) 0.053(3) Uani 1 1 d . . . H39B H 0.1223 0.7510 0.3692 0.064 Uiso 1 1 d R . . C40B C 0.2495(3) 0.7216(8) 0.4155(3) 0.046(2) Uani 1 1 d . . . H40D H 0.2303 0.6969 0.3929 0.056 Uiso 1 1 d R . . H40E H 0.2756 0.7446 0.4038 0.056 Uiso 1 1 d R . . C41B C 0.2297(3) 0.8130(6) 0.4366(2) 0.0326(17) Uani 1 1 d . . . C42B C 0.2105(3) 0.9989(7) 0.4391(2) 0.0371(19) Uani 1 1 d . . . H42B H 0.1819 0.9735 0.4443 0.044 Uiso 1 1 calc R . . C43B C 0.2058(3) 1.0830(7) 0.4073(2) 0.042(2) Uani 1 1 d . . . H43D H 0.1925 1.0532 0.3824 0.063 Uiso 1 1 d R . . H43E H 0.2333 1.1106 0.4017 0.063 Uiso 1 1 d R . . H43F H 0.1885 1.1399 0.4170 0.063 Uiso 1 1 d R . . C44B C 0.2306(3) 1.0347(7) 0.4793(2) 0.0352(18) Uani 1 1 d . . . C45B C 0.2721(3) 1.0730(7) 0.4813(2) 0.0325(17) Uani 1 1 d . . . H45B H 0.2879 1.0688 0.4580 0.039 Uiso 1 1 d R . . C46B C 0.2910(3) 1.1134(10) 0.5165(3) 0.054(3) Uani 1 1 d . . . H46B H 0.3186 1.1403 0.5172 0.064 Uiso 1 1 d R . . C47B C 0.2682(3) 1.1148(8) 0.5518(3) 0.049(2) Uani 1 1 d . . . H47B H 0.2806 1.1407 0.5766 0.058 Uiso 1 1 d R . . C48B C 0.2275(3) 1.0772(8) 0.5502(3) 0.046(2) Uani 1 1 d . . . H48B H 0.2120 1.0788 0.5738 0.056 Uiso 1 1 d R . . C49B C 0.2079(3) 1.0401(7) 0.5144(2) 0.0345(17) Uani 1 1 d . . . H49B H 0.1800 1.0155 0.5138 0.041 Uiso 1 1 d R . . S1 S 0.15376(7) 0.20239(17) 0.31021(6) 0.0370(5) Uani 1 1 d . . . O11 O 0.1515(3) 0.0910(5) 0.3117(2) 0.060(2) Uani 1 1 d . . . O12 O 0.1296(2) 0.2501(5) 0.2774(2) 0.0510(17) Uani 1 1 d . . . O13 O 0.1517(2) 0.2533(5) 0.3487(2) 0.0522(17) Uani 1 1 d . . . C1S C 0.2082(4) 0.2286(14) 0.2975(4) 0.075(4) Uani 1 1 d . . . F11 F 0.2150(3) 0.1889(13) 0.2636(3) 0.150(6) Uani 1 1 d . . . F12 F 0.2341(2) 0.1932(8) 0.3261(2) 0.087(3) Uani 1 1 d . . . F13 F 0.2118(3) 0.3362(10) 0.2957(3) 0.114(4) Uani 1 1 d . . . S2 S 0.31586(8) 0.89654(18) 0.66035(7) 0.0443(5) Uani 1 1 d . . . O21 O 0.2829(2) 0.9449(5) 0.63660(19) 0.0505(17) Uani 1 1 d . . . O22 O 0.3217(2) 0.7850(7) 0.6517(2) 0.0562(19) Uani 1 1 d . . . O23 O 0.3534(3) 0.9539(8) 0.6646(3) 0.080(3) Uani 1 1 d . . . C2S C 0.2987(3) 0.8973(7) 0.7101(3) 0.045(2) Uani 1 1 d . . . F21 F 0.3269(2) 0.8651(6) 0.73805(18) 0.0664(17) Uani 1 1 d . . . F22 F 0.26329(19) 0.8393(5) 0.71384(18) 0.0574(15) Uani 1 1 d . . . F23 F 0.2864(3) 0.9960(5) 0.7215(2) 0.079(2) Uani 1 1 d . . . S3 S 0.14314(8) 0.19888(19) 0.64978(6) 0.0412(5) Uani 1 1 d . . . O31 O 0.12870(19) 0.1429(5) 0.68349(17) 0.0406(14) Uani 1 1 d . . . O32 O 0.1280(2) 0.3051(6) 0.64532(19) 0.0507(17) Uani 1 1 d . . . O33 O 0.1433(2) 0.1436(7) 0.6121(2) 0.0594(19) Uani 1 1 d . . . C3S C 0.1987(3) 0.2135(8) 0.6634(3) 0.048(2) Uani 1 1 d . . . F31 F 0.21700(18) 0.1228(6) 0.6712(2) 0.0666(17) Uani 1 1 d . . . F32 F 0.2182(2) 0.2594(6) 0.6337(2) 0.0694(19) Uani 1 1 d . . . F33 F 0.2056(2) 0.2712(7) 0.6957(2) 0.076(2) Uani 1 1 d . . . S4 S 0.61553(8) 0.4402(3) 0.45585(8) 0.0464(7) Uani 0.85 1 d P A 1 S4' S 0.6154(7) 0.4632(19) 0.4921(6) 0.066(5) Uiso 0.15 1 d P A 2 O41 O 0.5961(2) 0.3876(9) 0.4232(2) 0.071(2) Uani 1 1 d . . . O42 O 0.6528(2) 0.3979(9) 0.4735(3) 0.089(3) Uani 1 1 d . . . O43 O 0.6165(3) 0.5532(8) 0.4498(4) 0.096(3) Uani 1 1 d . . . C4S C 0.5788(5) 0.4257(15) 0.4942(4) 0.084(5) Uani 1 1 d . . . F41 F 0.5747(3) 0.3266(9) 0.5061(3) 0.112(4) Uani 1 1 d . A . F42 F 0.5425(3) 0.4620(12) 0.4821(3) 0.140(5) Uani 1 1 d . A . F43 F 0.5919(5) 0.4804(9) 0.5278(3) 0.135(5) Uani 1 1 d . A . S5 S 0.02645(18) 0.7037(4) 0.39188(15) 0.1016(14) Uani 1 1 d . . . O51 O 0.0337(4) 0.6965(9) 0.3491(3) 0.098(4) Uani 1 1 d . B . O52 O 0.0604(5) 0.6883(17) 0.4200(4) 0.165(8) Uani 1 1 d . B . O53 O -0.0052(8) 0.770(2) 0.3990(8) 0.212(9) Uiso 1 1 d . B . C5S C 0.0024(16) 0.599(5) 0.3766(15) 0.132(15) Uiso 0.50 1 d P B 1 C5S' C 0.0136(6) 0.6417(19) 0.4084(6) 0.050(5) Uiso 0.50 1 d P B 2 F51 F 0.0232(5) 0.5133(14) 0.3942(5) 0.190(7) Uani 1 1 d . . . F52 F -0.0282(13) 0.560(3) 0.3618(12) 0.197(14) Uiso 0.50 1 d P B 1 F52' F -0.0031(8) 0.571(2) 0.4430(8) 0.139(8) Uiso 0.50 1 d P B 2 F53 F -0.0309(11) 0.570(3) 0.4099(11) 0.329(15) Uiso 1 1 d . . . S6 S 0.32788(8) 0.9702(2) 0.35543(8) 0.0533(6) Uani 1 1 d . . . O61 O 0.3685(2) 1.0135(6) 0.3632(2) 0.0533(17) Uani 1 1 d . . . O62 O 0.2944(3) 1.0099(9) 0.3762(3) 0.095(3) Uani 1 1 d . . . O63 O 0.3258(5) 0.8557(9) 0.3545(4) 0.115(4) Uani 1 1 d . . . C6S C 0.3149(3) 1.0009(11) 0.3023(4) 0.060(3) Uani 1 1 d . . . F61 F 0.3170(3) 1.1084(8) 0.2979(3) 0.097(3) Uani 1 1 d . . . F62 F 0.3416(3) 0.9669(10) 0.2775(2) 0.108(4) Uani 1 1 d . . . F63 F 0.2772(2) 0.9792(8) 0.2890(3) 0.090(2) Uani 1 1 d . . . O1S O 0.5247(4) 0.6680(9) 0.3865(3) 0.099(3) Uani 1 1 d . . . H01S H 0.5488 0.6941 0.3849 0.149 Uiso 1 1 d R . . C7S C 0.5128(6) 0.6829(18) 0.4259(6) 0.111(6) Uiso 1 1 d . . . H7S1 H 0.5125 0.7579 0.4336 0.144 Uiso 1 1 d R . . H7S2 H 0.5314 0.6445 0.4457 0.144 Uiso 1 1 d R . . C8S C 0.4709(8) 0.638(2) 0.4257(7) 0.149(8) Uiso 1 1 d . . . H8S1 H 0.4596 0.6439 0.4525 0.223 Uiso 1 1 d R . . H8S2 H 0.4718 0.5634 0.4180 0.223 Uiso 1 1 d R . . H8S3 H 0.4530 0.6759 0.4057 0.223 Uiso 1 1 d R . . O2S O 0.1074(6) 0.9180(16) 0.4969(6) 0.123(6) Uiso 0.75 1 d P . . H02S H 0.0968 0.9269 0.5196 0.185 Uiso 0.75 1 d PR . . C9S C 0.0721(13) 0.937(4) 0.4620(12) 0.111(12) Uiso 0.50 1 d P . . H9S1 H 0.0499 0.8849 0.4657 0.145 Uiso 0.50 1 d PR . . H9S2 H 0.0599 1.0069 0.4671 0.145 Uiso 0.50 1 d PR . . C10S C 0.0850(13) 0.934(3) 0.4229(11) 0.110(12) Uiso 0.50 1 d P . . H10A H 0.0595 0.9478 0.4060 0.166 Uiso 0.50 1 d PR . . H10B H 0.0958 0.8646 0.4164 0.166 Uiso 0.50 1 d PR . . H10C H 0.1059 0.9875 0.4178 0.166 Uiso 0.50 1 d PR . . O3S O 0.0265(10) 0.982(3) 0.6062(9) 0.128(9) Uiso 0.50 1 d P . . C11S C 0.024(3) 1.060(8) 0.591(2) 0.24(4) Uiso 0.50 1 d P . . H11C H 0.0381 1.1285 0.5973 0.315 Uiso 0.50 1 d PR . . H11D H -0.0034 1.0609 0.6030 0.315 Uiso 0.50 1 d PR . . C12S C -0.0014(11) 1.048(3) 0.5454(9) 0.090(9) Uiso 0.50 1 d P . . H12C H -0.0182 1.1041 0.5321 0.135 Uiso 0.50 1 d PR . . H12D H -0.0149 0.9806 0.5402 0.135 Uiso 0.50 1 d PR . . H12E H 0.0263 1.0478 0.5346 0.135 Uiso 0.50 1 d PR . . O1W O 0.6074(5) 0.7306(16) 0.3927(6) 0.161(6) Uiso 1 1 d . . . H2W1 H 0.6181 0.6918 0.4114 0.242 Uiso 1 1 d R . . H1W1 H 0.6208 0.7221 0.3715 0.242 Uiso 1 1 d R . . O2W O 0.0956(8) 0.986(2) 0.5751(8) 0.165(9) Uiso 0.75 1 d P . . O3W C 0.4145(12) -0.184(3) 0.4964(11) 0.159(13) Uiso 0.75 1 d P . . 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 Ce1A 0.02268(17) 0.01530(16) 0.02092(15) 0.00191(14) 0.00310(12) 0.00505(16) O1A 0.038(3) 0.021(3) 0.026(2) 0.0036(18) 0.003(2) 0.015(2) O2A 0.028(3) 0.022(3) 0.028(2) -0.0007(18) 0.009(2) 0.008(2) O3A 0.027(3) 0.018(3) 0.031(3) -0.0014(19) 0.001(2) 0.008(2) O4A 0.031(3) 0.026(3) 0.031(3) 0.010(2) 0.004(2) 0.000(2) O5A 0.051(3) 0.020(3) 0.033(3) -0.003(2) -0.006(2) 0.010(3) N1A 0.026(3) 0.017(3) 0.039(3) 0.002(2) 0.010(2) 0.012(3) N2A 0.021(3) 0.018(3) 0.032(3) -0.003(2) 0.009(2) -0.003(2) N3A 0.022(3) 0.019(3) 0.027(3) 0.0021(19) 0.008(2) 0.001(2) N4A 0.017(3) 0.025(3) 0.025(3) 0.004(2) 0.004(2) 0.000(2) N11A 0.034(3) 0.022(4) 0.043(3) 0.003(3) 0.008(3) 0.010(3) N21A 0.027(3) 0.025(3) 0.032(3) -0.003(2) 0.010(3) 0.000(3) N31A 0.032(3) 0.018(3) 0.039(3) 0.005(2) 0.008(3) 0.010(3) N41A 0.026(3) 0.032(4) 0.026(3) 0.013(2) 0.003(2) -0.003(3) C1A 0.032(4) 0.014(4) 0.044(4) -0.004(3) 0.010(3) -0.005(3) C2A 0.030(4) 0.014(3) 0.031(3) -0.006(2) 0.009(3) -0.003(3) C3A 0.033(4) 0.027(4) 0.032(4) -0.002(3) 0.004(3) -0.003(3) C4A 0.030(4) 0.039(5) 0.022(3) 0.003(3) 0.003(3) -0.007(3) C5A 0.023(3) 0.029(4) 0.026(3) 0.002(3) -0.002(3) 0.003(3) C6A 0.028(3) 0.027(4) 0.017(3) 0.006(2) 0.003(3) 0.004(3) C7A 0.035(4) 0.026(4) 0.022(3) 0.001(2) 0.012(3) 0.005(3) C8A 0.026(4) 0.034(5) 0.028(4) 0.002(3) 0.004(3) 0.017(3) C10A 0.021(3) 0.037(5) 0.035(4) 0.003(3) 0.006(3) 0.012(3) C11A 0.024(3) 0.025(4) 0.030(3) 0.005(3) -0.001(3) 0.004(3) C12A 0.048(5) 0.032(5) 0.045(4) 0.002(3) -0.015(4) 0.008(4) C13A 0.024(4) 0.066(7) 0.064(6) 0.024(5) -0.006(4) 0.006(4) C14A 0.050(5) 0.034(5) 0.025(4) 0.005(3) 0.003(3) 0.013(4) C15A 0.053(6) 0.046(6) 0.047(5) 0.020(4) 0.007(4) 0.000(5) C16A 0.067(7) 0.084(9) 0.054(6) 0.045(6) -0.004(6) -0.017(7) C17A 0.049(7) 0.130(15) 0.067(8) 0.050(9) 0.021(6) 0.011(9) C18A 0.072(9) 0.18(2) 0.065(8) 0.048(11) 0.036(7) 0.058(13) C19A 0.073(8) 0.101(11) 0.047(5) 0.010(6) 0.008(5) 0.034(8) C20A 0.033(4) 0.013(3) 0.026(3) 0.003(2) 0.012(3) 0.001(3) C21A 0.028(4) 0.027(4) 0.021(3) 0.001(3) 0.007(3) 0.007(3) C22A 0.049(5) 0.020(4) 0.030(4) 0.000(3) 0.021(3) 0.008(3) C23A 0.062(6) 0.039(6) 0.051(5) 0.014(4) 0.031(5) 0.016(5) C24A 0.038(4) 0.027(4) 0.031(4) 0.007(3) 0.015(3) 0.007(3) C25A 0.035(4) 0.030(5) 0.062(5) 0.000(4) 0.020(4) -0.004(4) C26A 0.033(5) 0.059(7) 0.061(6) 0.004(5) -0.001(4) 0.011(5) C27A 0.058(6) 0.054(7) 0.061(6) 0.021(5) 0.034(5) 0.017(5) C28A 0.057(6) 0.032(5) 0.049(5) 0.018(4) 0.025(4) 0.017(4) C29A 0.037(4) 0.038(5) 0.038(4) -0.003(3) 0.014(3) 0.002(4) C30A 0.023(3) 0.032(4) 0.026(3) 0.004(3) 0.001(3) 0.004(3) C31A 0.024(3) 0.027(4) 0.022(3) 0.003(3) 0.007(3) 0.007(3) C32A 0.047(5) 0.021(4) 0.038(4) 0.007(3) 0.007(3) 0.012(4) C33A 0.054(5) 0.025(5) 0.051(5) 0.002(3) 0.017(4) 0.006(4) C34A 0.036(4) 0.013(4) 0.057(5) 0.004(3) 0.015(4) 0.011(3) C35A 0.054(6) 0.036(5) 0.057(5) 0.021(4) 0.032(5) 0.021(4) C36A 0.104(10) 0.042(6) 0.054(6) 0.009(5) 0.041(6) 0.014(6) C37A 0.062(8) 0.066(9) 0.132(14) -0.020(9) 0.054(9) -0.014(7) C38A 0.033(5) 0.064(8) 0.116(11) -0.026(7) 0.028(6) -0.006(5) C39A 0.033(5) 0.033(5) 0.089(7) -0.026(5) 0.017(5) 0.003(4) C40A 0.032(4) 0.018(4) 0.032(4) 0.003(3) 0.004(3) 0.007(3) C41A 0.032(4) 0.016(4) 0.026(3) -0.004(3) 0.003(3) -0.003(3) C42A 0.030(4) 0.026(4) 0.036(4) 0.002(3) -0.008(3) 0.002(3) C43A 0.038(4) 0.030(5) 0.062(5) 0.016(4) -0.015(4) -0.011(4) C44A 0.019(3) 0.030(4) 0.031(4) 0.009(3) -0.002(3) -0.001(3) C45A 0.044(5) 0.049(7) 0.034(4) 0.008(4) 0.006(3) -0.005(4) C46A 0.037(4) 0.030(5) 0.051(5) -0.006(3) 0.009(4) 0.009(4) C47A 0.028(4) 0.035(5) 0.061(5) 0.019(4) 0.002(4) 0.008(4) C48A 0.045(5) 0.040(5) 0.030(4) 0.009(3) 0.005(3) 0.018(4) C49A 0.028(3) 0.031(5) 0.027(3) 0.003(3) -0.002(3) 0.006(3) Ce1B 0.0291(2) 0.0303(2) 0.02304(18) -0.00328(16) 0.00426(14) 0.00569(18) O1B 0.038(3) 0.035(3) 0.033(3) -0.005(2) 0.001(2) 0.013(3) O2B 0.035(3) 0.041(4) 0.035(3) 0.017(2) 0.012(2) 0.012(3) O3B 0.047(3) 0.019(3) 0.026(2) 0.0025(19) 0.001(2) 0.001(2) O4B 0.049(3) 0.026(3) 0.037(3) -0.009(2) 0.021(3) -0.006(3) O5B 0.054(4) 0.042(4) 0.052(4) 0.002(3) -0.008(3) 0.018(3) N1B 0.037(4) 0.054(5) 0.055(5) -0.031(4) 0.000(3) 0.005(4) N2B 0.043(4) 0.042(4) 0.032(3) -0.003(3) -0.006(3) 0.020(3) N3B 0.023(3) 0.031(4) 0.040(4) -0.007(3) -0.001(3) 0.005(3) N4B 0.036(3) 0.043(4) 0.044(4) -0.021(3) 0.022(3) -0.004(4) N11B 0.046(4) 0.041(4) 0.031(3) -0.011(3) 0.003(3) -0.003(3) N21B 0.060(5) 0.066(7) 0.047(4) 0.031(4) 0.019(4) 0.015(5) N31B 0.053(4) 0.021(3) 0.034(3) -0.003(3) 0.004(3) -0.007(3) N41B 0.058(5) 0.031(4) 0.029(3) -0.012(3) 0.009(3) -0.009(3) C1B 0.052(6) 0.041(6) 0.077(7) -0.026(5) -0.012(5) 0.023(5) C2B 0.069(7) 0.055(7) 0.052(6) -0.005(5) -0.021(5) 0.020(6) C3B 0.044(5) 0.036(5) 0.042(4) -0.002(3) -0.011(4) 0.011(4) C4B 0.038(4) 0.044(6) 0.049(5) 0.001(4) -0.002(3) 0.022(4) C5B 0.036(5) 0.054(6) 0.046(5) -0.020(4) 0.005(4) 0.011(4) C6B 0.052(5) 0.052(6) 0.043(5) -0.025(4) 0.025(4) -0.006(5) C7B 0.038(5) 0.058(7) 0.081(7) -0.042(6) 0.013(5) 0.001(5) C8B 0.048(6) 0.065(8) 0.059(6) -0.036(5) 0.010(5) -0.015(5) C10B 0.045(5) 0.043(5) 0.044(5) -0.023(4) 0.002(4) 0.001(4) C11B 0.047(5) 0.023(4) 0.033(4) 0.001(3) -0.004(3) 0.006(4) C12B 0.037(5) 0.042(5) 0.045(5) -0.005(4) 0.001(4) 0.013(4) C13B 0.070(7) 0.042(6) 0.044(5) -0.003(4) 0.013(5) 0.013(5) C14B 0.084(7) 0.035(5) 0.033(4) -0.012(3) 0.006(4) 0.008(5) C15B 0.070(7) 0.056(6) 0.033(4) 0.002(4) 0.003(4) 0.000(5) C16B 0.083(8) 0.064(8) 0.037(5) 0.011(5) -0.014(5) -0.009(6) C17B 0.141(14) 0.068(9) 0.043(6) -0.004(6) 0.004(7) 0.018(10) C18B 0.061(7) 0.066(9) 0.074(8) -0.027(6) 0.016(6) -0.017(6) C19B 0.070(7) 0.057(7) 0.046(5) -0.015(5) 0.006(5) -0.005(6) C20B 0.057(6) 0.041(6) 0.049(5) 0.018(4) 0.012(4) 0.028(5) C21B 0.049(5) 0.048(6) 0.044(5) 0.009(4) 0.013(4) 0.026(5) C22B 0.039(4) 0.075(8) 0.066(6) 0.038(6) 0.018(4) 0.015(6) C23B 0.052(6) 0.110(12) 0.075(8) 0.022(7) 0.038(6) 0.007(7) C24B 0.025(4) 0.090(9) 0.068(7) 0.037(6) 0.019(4) 0.010(5) C25B 0.039(6) 0.084(10) 0.078(8) 0.030(7) 0.004(5) 0.008(6) C26B 0.069(8) 0.099(12) 0.088(10) 0.010(8) 0.035(7) 0.009(8) C27B 0.046(6) 0.099(12) 0.082(9) 0.010(8) 0.015(6) -0.008(7) C28B 0.054(7) 0.150(17) 0.074(9) 0.037(9) -0.011(6) -0.051(9) C29B 0.036(5) 0.095(11) 0.101(10) 0.032(9) -0.001(6) -0.012(7) C30B 0.044(4) 0.024(5) 0.035(4) -0.004(3) -0.003(3) -0.002(3) C31B 0.039(4) 0.031(5) 0.028(4) 0.005(3) 0.008(3) -0.009(4) C32B 0.056(5) 0.027(4) 0.026(4) -0.003(3) -0.006(3) -0.010(4) C33B 0.077(7) 0.011(4) 0.041(4) 0.001(3) -0.019(4) -0.007(4) C34B 0.056(5) 0.026(4) 0.035(4) -0.001(3) -0.005(3) -0.010(4) C35B 0.087(8) 0.087(10) 0.041(5) 0.018(6) 0.004(5) -0.028(8) C36B 0.068(8) 0.138(16) 0.046(6) 0.018(7) 0.016(6) -0.014(9) C37B 0.100(11) 0.106(13) 0.080(9) 0.074(10) -0.039(9) -0.060(10) C38B 0.097(10) 0.053(7) 0.061(7) 0.029(6) -0.041(7) -0.042(7) C39B 0.080(8) 0.035(5) 0.042(5) 0.005(4) -0.015(5) -0.017(5) C40B 0.058(6) 0.032(5) 0.052(5) -0.019(4) 0.031(5) -0.002(4) C41B 0.039(4) 0.022(4) 0.037(4) -0.010(3) 0.006(3) -0.006(3) C42B 0.046(5) 0.036(5) 0.030(4) -0.001(3) 0.005(3) -0.012(4) C43B 0.066(6) 0.034(5) 0.026(4) 0.005(3) -0.004(4) -0.010(4) C44B 0.049(5) 0.030(4) 0.028(4) 0.004(3) 0.006(3) -0.002(4) C45B 0.034(4) 0.029(4) 0.035(4) -0.001(3) 0.004(3) 0.005(3) C46B 0.045(5) 0.060(7) 0.054(5) -0.013(5) -0.007(4) 0.015(5) C47B 0.075(7) 0.027(5) 0.041(4) 0.006(4) -0.016(4) 0.002(5) C48B 0.065(6) 0.043(5) 0.033(4) 0.002(3) 0.007(4) 0.018(5) C49B 0.037(4) 0.031(4) 0.037(4) -0.004(3) 0.015(3) -0.002(4) S1 0.0425(11) 0.0283(11) 0.0393(10) -0.0057(8) -0.0051(8) -0.0065(9) O11 0.084(5) 0.026(4) 0.066(4) -0.008(3) -0.021(4) -0.013(3) O12 0.048(4) 0.037(4) 0.065(4) 0.004(3) -0.022(3) -0.012(3) O13 0.077(5) 0.028(4) 0.050(4) 0.001(3) -0.001(3) 0.006(3) C1S 0.064(7) 0.111(13) 0.049(6) 0.015(7) 0.007(5) 0.020(8) F11 0.109(7) 0.287(17) 0.056(5) 0.003(7) 0.032(5) 0.076(9) F12 0.042(3) 0.150(8) 0.070(4) 0.038(5) 0.003(3) 0.022(4) F13 0.073(5) 0.166(11) 0.102(6) 0.078(7) -0.011(4) -0.051(6) S2 0.0497(12) 0.0331(14) 0.0507(12) -0.0087(9) 0.0085(10) -0.0136(10) O21 0.079(5) 0.033(4) 0.039(3) -0.004(3) 0.001(3) -0.005(3) O22 0.049(4) 0.060(5) 0.060(4) -0.019(4) 0.010(3) -0.002(4) O23 0.061(5) 0.063(6) 0.117(7) 0.000(5) 0.011(5) -0.027(5) C2S 0.066(6) 0.030(5) 0.038(4) -0.011(3) -0.002(4) -0.004(4) F21 0.075(4) 0.067(4) 0.054(3) -0.012(3) -0.017(3) -0.007(4) F22 0.058(3) 0.058(4) 0.057(3) -0.002(3) 0.010(3) -0.001(3) F23 0.129(7) 0.045(4) 0.062(4) -0.015(3) 0.000(4) 0.024(4) S3 0.0475(12) 0.0409(13) 0.0364(10) 0.0115(8) 0.0131(9) 0.0140(10) O31 0.043(3) 0.040(4) 0.041(3) 0.016(3) 0.013(2) 0.008(3) O32 0.065(4) 0.046(4) 0.043(3) 0.014(3) 0.016(3) 0.024(3) O33 0.071(5) 0.059(5) 0.048(4) -0.005(3) 0.000(3) 0.015(4) C3S 0.046(5) 0.036(5) 0.062(6) 0.017(4) 0.001(4) -0.006(4) F31 0.051(3) 0.051(4) 0.096(4) 0.033(4) -0.012(3) 0.000(3) F32 0.057(4) 0.061(4) 0.093(5) 0.033(4) 0.021(3) 0.007(3) F33 0.078(5) 0.079(5) 0.068(4) -0.022(4) -0.015(4) 0.003(4) S4 0.0340(13) 0.062(2) 0.0422(14) 0.0025(12) -0.0070(10) -0.0022(13) O41 0.067(5) 0.097(7) 0.048(4) 0.002(4) -0.009(3) 0.021(5) O42 0.041(4) 0.098(9) 0.125(8) 0.041(6) -0.004(4) -0.004(5) O43 0.095(7) 0.059(6) 0.133(9) 0.036(6) -0.004(6) -0.027(6) C4S 0.086(10) 0.116(13) 0.052(7) 0.023(7) 0.012(7) 0.013(9) F41 0.103(7) 0.122(8) 0.106(7) 0.050(6) -0.019(5) -0.039(6) F42 0.080(6) 0.224(14) 0.120(8) 0.077(9) 0.045(6) 0.054(7) F43 0.238(14) 0.109(8) 0.059(5) -0.015(5) 0.006(6) 0.058(9) S5 0.117(4) 0.093(3) 0.096(3) 0.008(2) 0.018(3) 0.031(3) O51 0.136(9) 0.097(8) 0.064(5) 0.028(5) 0.022(6) 0.043(7) O52 0.136(11) 0.28(2) 0.078(7) -0.081(11) -0.023(8) 0.011(12) F51 0.182(14) 0.171(15) 0.221(16) 0.080(13) 0.035(12) -0.077(12) S6 0.0475(14) 0.0608(18) 0.0542(14) 0.0036(12) 0.0243(11) -0.0080(12) O61 0.043(4) 0.055(5) 0.063(4) -0.007(3) 0.013(3) -0.008(3) O62 0.097(7) 0.089(8) 0.107(7) 0.015(6) 0.064(6) 0.016(6) O63 0.165(11) 0.057(8) 0.127(9) 0.008(6) 0.035(8) -0.013(7) C6S 0.043(6) 0.078(9) 0.060(6) -0.008(6) 0.009(5) -0.005(6) F61 0.118(7) 0.077(6) 0.095(5) 0.028(5) 0.007(5) 0.012(5) F62 0.077(5) 0.180(11) 0.067(5) -0.015(5) 0.003(4) 0.059(6) F63 0.063(4) 0.093(7) 0.111(6) -0.004(5) -0.012(4) 0.003(4) O1S 0.134(9) 0.082(8) 0.079(6) -0.019(5) -0.006(6) 0.019(7) _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 Ce1A O3A 2.413(5) . ? Ce1A O1A 2.441(5) . ? Ce1A O2A 2.473(5) . ? Ce1A O4A 2.474(5) . ? Ce1A O5A 2.491(5) . ? Ce1A N2A 2.763(6) . ? Ce1A N3A 2.767(6) . ? Ce1A N4A 2.770(6) . ? Ce1A N1A 2.779(6) . ? O1A C11A 1.254(9) . ? O2A C21A 1.249(9) . ? O3A C31A 1.249(9) . ? O4A C41A 1.282(9) . ? N1A C8A 1.460(10) . ? N1A C1A 1.468(10) . ? N1A C10A 1.492(9) . ? N2A C20A 1.494(8) . ? N2A C3A 1.498(10) . ? N2A C2A 1.504(9) . ? N3A C30A 1.477(9) . ? N3A C5A 1.491(9) . ? N3A C4A 1.503(10) . ? N4A C7A 1.478(9) . ? N4A C40A 1.484(10) . ? N4A C6A 1.481(9) . ? N11A C11A 1.316(9) . ? N11A C12A 1.467(11) . ? N21A C21A 1.330(9) . ? N21A C22A 1.485(9) . ? N31A C31A 1.317(9) . ? N31A C32A 1.449(11) . ? N41A C41A 1.314(10) . ? N41A C42A 1.490(9) . ? C1A C2A 1.526(10) . ? C3A C4A 1.483(12) . ? C5A C6A 1.504(11) . ? C7A C8A 1.532(10) . ? C10A C11A 1.523(10) . ? C12A C14A 1.489(13) . ? C12A C13A 1.516(12) . ? C14A C15A 1.366(14) . ? C14A C19A 1.402(15) . ? C15A C16A 1.377(16) . ? C16A C17A 1.36(2) . ? C17A C18A 1.33(3) . ? C18A C19A 1.42(2) . ? C20A C21A 1.522(10) . ? C22A C24A 1.507(11) . ? C22A C23A 1.509(12) . ? C24A C25A 1.393(13) . ? C24A C29A 1.409(12) . ? C25A C26A 1.383(14) . ? C26A C27A 1.355(17) . ? C27A C28A 1.411(16) . ? C28A C29A 1.438(12) . ? C30A C31A 1.540(11) . ? C32A C34A 1.516(12) . ? C32A C33A 1.538(11) . ? C34A C35A 1.403(13) . ? C34A C39A 1.421(13) . ? C35A C36A 1.442(15) . ? C36A C37A 1.40(2) . ? C37A C38A 1.24(2) . ? C38A C39A 1.376(16) . ? C40A C41A 1.519(10) . ? C42A C44A 1.515(11) . ? C42A C43A 1.529(12) . ? C44A C45A 1.383(12) . ? C44A C49A 1.413(10) . ? C45A C46A 1.412(13) . ? C46A C47A 1.380(13) . ? C47A C48A 1.382(13) . ? C48A C49A 1.388(11) . ? Ce1B O4B 2.407(6) . ? Ce1B O3B 2.427(5) . ? Ce1B O1B 2.431(6) . ? Ce1B O2B 2.435(6) . ? Ce1B O5B 2.489(6) . ? Ce1B N2B 2.734(7) . ? Ce1B N3B 2.756(7) . ? Ce1B N1B 2.770(8) . ? Ce1B N4B 2.776(6) . ? O1B C11B 1.229(10) . ? O2B C21B 1.253(10) . ? O3B C31B 1.273(10) . ? O4B C41B 1.269(10) . ? N1B C8B 1.449(14) . ? N1B C10B 1.471(11) . ? N1B C1B 1.525(15) . ? N2B C3B 1.451(11) . ? N2B C20B 1.483(13) . ? N2B C2B 1.513(13) . ? N3B C5B 1.458(11) . ? N3B C30B 1.492(10) . ? N3B C4B 1.539(11) . ? N4B C40B 1.471(14) . ? N4B C7B 1.493(12) . ? N4B C6B 1.487(11) . ? N11B C11B 1.326(10) . ? N11B C12B 1.492(12) . ? N21B C21B 1.318(14) . ? N21B C22B 1.478(14) . ? N31B C31B 1.289(10) . ? N31B C32B 1.488(11) . ? N41B C41B 1.310(11) . ? N41B C42B 1.488(12) . ? C1B C2B 1.490(18) . ? C3B C4B 1.501(12) . ? C5B C6B 1.508(15) . ? C7B C8B 1.541(12) . ? C10B C11B 1.532(13) . ? C12B C14B 1.459(14) . ? C12B C13B 1.506(13) . ? C14B C19B 1.379(16) . ? C14B C15B 1.439(16) . ? C15B C16B 1.354(16) . ? C16B C17B 1.37(2) . ? C17B C18B 1.39(2) . ? C18B C19B 1.383(18) . ? C20B C21B 1.531(15) . ? C22B C24B 1.533(19) . ? C22B C23B 1.545(15) . ? C24B C25B 1.336(18) . ? C24B C29B 1.395(16) . ? C25B C26B 1.42(2) . ? C26B C27B 1.31(2) . ? C27B C28B 1.45(2) . ? C28B C29B 1.39(2) . ? C30B C31B 1.491(11) . ? C32B C33B 1.541(11) . ? C32B C34B 1.554(12) . ? C34B C39B 1.396(14) . ? C34B C35B 1.410(16) . ? C35B C36B 1.38(2) . ? C36B C37B 1.48(3) . ? C37B C38B 1.21(2) . ? C38B C39B 1.403(16) . ? C40B C41B 1.519(11) . ? C42B C43B 1.503(12) . ? C42B C44B 1.514(11) . ? C44B C49B 1.409(11) . ? C44B C45B 1.419(12) . ? C45B C46B 1.379(12) . ? C46B C47B 1.417(15) . ? C47B C48B 1.393(15) . ? C48B C49B 1.386(13) . ? S1 O11 1.423(7) . ? S1 O12 1.431(7) . ? S1 O13 1.432(7) . ? S1 C1S 1.856(14) . ? C1S F11 1.262(16) . ? C1S F12 1.301(13) . ? C1S F13 1.379(19) . ? S2 O23 1.412(9) . ? S2 O21 1.422(8) . ? S2 O22 1.465(8) . ? S2 C2S 1.767(10) . ? C2S F21 1.318(11) . ? C2S F22 1.370(12) . ? C2S F23 1.378(11) . ? S3 O31 1.424(6) . ? S3 O33 1.431(7) . ? S3 O32 1.444(7) . ? S3 C3S 1.825(10) . ? C3S F33 1.305(13) . ? C3S F31 1.317(12) . ? C3S F32 1.333(11) . ? S4 O41 1.388(9) . ? S4 O42 1.409(9) . ? S4 O43 1.455(11) . ? S4 C4S 1.794(15) . ? S4' C4S 1.28(3) . ? S4' F43 1.46(2) . ? S4' O42 1.61(3) . ? S4' O43 1.81(2) . ? C4S F42 1.297(17) . ? C4S F43 1.357(19) . ? C4S F41 1.332(19) . ? S5 C5S' 1.06(2) . ? S5 O53 1.35(3) . ? S5 O52 1.404(15) . ? S5 O51 1.450(11) . ? S5 C5S 1.61(6) . ? O51 C5S 1.87(6) . ? O52 C5S' 1.64(3) . ? O53 C5S' 1.76(4) . ? C5S F52 1.18(5) . ? C5S F51 1.39(5) . ? C5S F53 1.62(6) . ? C5S' F52' 1.57(4) . ? C5S' F53 1.70(4) . ? C5S' F51 1.74(3) . ? F52 F53 1.60(4) . ? F52' F53 1.37(4) . ? S6 O62 1.406(9) . ? S6 O61 1.429(8) . ? S6 O63 1.462(12) . ? S6 C6S 1.823(12) . ? C6S F62 1.296(13) . ? C6S F63 1.296(13) . ? C6S F61 1.380(16) . ? O1S C7S 1.39(2) . ? C7S C8S 1.47(3) . ? O2S C9S 1.59(4) . ? C9S C10S 1.38(5) . ? O3S C11S 1.12(9) . ? C11S C12S 1.69(9) . ? 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 O3A Ce1A O1A 148.33(17) . . ? O3A Ce1A O2A 85.45(17) . . ? O1A Ce1A O2A 86.73(17) . . ? O3A Ce1A O4A 86.11(18) . . ? O1A Ce1A O4A 85.90(18) . . ? O2A Ce1A O4A 150.72(17) . . ? O3A Ce1A O5A 74.69(17) . . ? O1A Ce1A O5A 73.66(18) . . ? O2A Ce1A O5A 77.52(19) . . ? O4A Ce1A O5A 73.21(19) . . ? O3A Ce1A N2A 127.79(18) . . ? O1A Ce1A N2A 74.71(19) . . ? O2A Ce1A N2A 64.27(17) . . ? O4A Ce1A N2A 139.56(18) . . ? O5A Ce1A N2A 131.05(19) . . ? O3A Ce1A N3A 64.50(17) . . ? O1A Ce1A N3A 140.82(18) . . ? O2A Ce1A N3A 73.05(16) . . ? O4A Ce1A N3A 127.16(16) . . ? O5A Ce1A N3A 130.73(18) . . ? N2A Ce1A N3A 66.35(18) . . ? O3A Ce1A N4A 74.50(18) . . ? O1A Ce1A N4A 128.01(17) . . ? O2A Ce1A N4A 138.80(16) . . ? O4A Ce1A N4A 64.33(16) . . ? O5A Ce1A N4A 128.38(19) . . ? N2A Ce1A N4A 100.54(18) . . ? N3A Ce1A N4A 65.88(16) . . ? O3A Ce1A N1A 141.16(18) . . ? O1A Ce1A N1A 64.44(17) . . ? O2A Ce1A N1A 126.74(18) . . ? O4A Ce1A N1A 74.36(19) . . ? O5A Ce1A N1A 127.97(19) . . ? N2A Ce1A N1A 65.30(18) . . ? N3A Ce1A N1A 101.29(18) . . ? N4A Ce1A N1A 66.83(18) . . ? C11A O1A Ce1A 125.9(4) . . ? C21A O2A Ce1A 124.3(4) . . ? C31A O3A Ce1A 126.2(5) . . ? C41A O4A Ce1A 124.2(5) . . ? C8A N1A C1A 108.6(6) . . ? C8A N1A C10A 109.6(6) . . ? C1A N1A C10A 111.3(6) . . ? C8A N1A Ce1A 109.5(4) . . ? C1A N1A Ce1A 111.6(4) . . ? C10A N1A Ce1A 106.3(4) . . ? C20A N2A C3A 108.7(6) . . ? C20A N2A C2A 108.0(5) . . ? C3A N2A C2A 109.3(6) . . ? C20A N2A Ce1A 106.9(4) . . ? C3A N2A Ce1A 111.6(4) . . ? C2A N2A Ce1A 112.3(4) . . ? C30A N3A C5A 110.2(5) . . ? C30A N3A C4A 109.9(5) . . ? C5A N3A C4A 108.0(5) . . ? C30A N3A Ce1A 106.5(4) . . ? C5A N3A Ce1A 112.4(4) . . ? C4A N3A Ce1A 109.9(4) . . ? C7A N4A C40A 111.0(5) . . ? C7A N4A C6A 109.4(5) . . ? C40A N4A C6A 108.9(6) . . ? C7A N4A Ce1A 110.0(4) . . ? C40A N4A Ce1A 106.9(4) . . ? C6A N4A Ce1A 110.6(4) . . ? C11A N11A C12A 121.2(7) . . ? C21A N21A C22A 121.7(7) . . ? C31A N31A C32A 120.9(7) . . ? C41A N41A C42A 123.1(6) . . ? N1A C1A C2A 114.4(6) . . ? N2A C2A C1A 110.0(6) . . ? C4A C3A N2A 114.2(6) . . ? C3A C4A N3A 114.0(6) . . ? N3A C5A C6A 113.2(6) . . ? N4A C6A C5A 114.5(6) . . ? N4A C7A C8A 115.0(6) . . ? N1A C8A C7A 113.3(6) . . ? N1A C10A C11A 111.9(6) . . ? O1A C11A N11A 120.2(7) . . ? O1A C11A C10A 119.6(6) . . ? N11A C11A C10A 120.2(7) . . ? N11A C12A C14A 111.0(7) . . ? N11A C12A C13A 109.2(8) . . ? C14A C12A C13A 111.7(8) . . ? C15A C14A C19A 115.9(11) . . ? C15A C14A C12A 123.1(8) . . ? C19A C14A C12A 121.0(10) . . ? C14A C15A C16A 122.5(12) . . ? C15A C16A C17A 119.5(14) . . ? C18A C17A C16A 122.3(13) . . ? C17A C18A C19A 117.6(16) . . ? C14A C19A C18A 122.2(17) . . ? N2A C20A C21A 110.5(5) . . ? O2A C21A N21A 123.2(7) . . ? O2A C21A C20A 120.7(6) . . ? N21A C21A C20A 116.0(7) . . ? N21A C22A C24A 109.8(6) . . ? N21A C22A C23A 107.6(7) . . ? C24A C22A C23A 113.4(7) . . ? C25A C24A C29A 116.9(8) . . ? C25A C24A C22A 124.2(8) . . ? C29A C24A C22A 118.9(8) . . ? C26A C25A C24A 122.8(9) . . ? C27A C26A C25A 120.9(10) . . ? C26A C27A C28A 120.3(10) . . ? C27A C28A C29A 118.3(10) . . ? C24A C29A C28A 120.8(9) . . ? N3A C30A C31A 110.6(6) . . ? O3A C31A N31A 122.7(7) . . ? O3A C31A C30A 119.3(7) . . ? N31A C31A C30A 117.7(6) . . ? N31A C32A C34A 112.3(7) . . ? N31A C32A C33A 109.3(7) . . ? C34A C32A C33A 112.3(7) . . ? C35A C34A C39A 119.7(9) . . ? C35A C34A C32A 119.8(8) . . ? C39A C34A C32A 120.5(8) . . ? C34A C35A C36A 116.1(10) . . ? C37A C36A C35A 119.5(11) . . ? C38A C37A C36A 122.5(12) . . ? C37A C38A C39A 122.7(13) . . ? C38A C39A C34A 119.2(12) . . ? N4A C40A C41A 111.3(6) . . ? O4A C41A N41A 121.6(7) . . ? O4A C41A C40A 119.6(7) . . ? N41A C41A C40A 118.7(6) . . ? N41A C42A C44A 111.0(6) . . ? N41A C42A C43A 108.8(6) . . ? C44A C42A C43A 110.7(7) . . ? C45A C44A C49A 118.1(7) . . ? C45A C44A C42A 121.9(7) . . ? C49A C44A C42A 120.0(7) . . ? C44A C45A C46A 121.3(8) . . ? C47A C46A C45A 119.5(8) . . ? C48A C47A C46A 120.0(8) . . ? C47A C48A C49A 120.8(7) . . ? C48A C49A C44A 120.4(7) . . ? O4B Ce1B O3B 86.97(19) . . ? O4B Ce1B O1B 85.03(19) . . ? O3B Ce1B O1B 148.59(19) . . ? O4B Ce1B O2B 149.6(2) . . ? O3B Ce1B O2B 84.39(19) . . ? O1B Ce1B O2B 87.4(2) . . ? O4B Ce1B O5B 75.5(2) . . ? O3B Ce1B O5B 73.0(2) . . ? O1B Ce1B O5B 75.6(2) . . ? O2B Ce1B O5B 74.2(2) . . ? O4B Ce1B N2B 139.6(2) . . ? O3B Ce1B N2B 128.1(2) . . ? O1B Ce1B N2B 73.7(2) . . ? O2B Ce1B N2B 64.5(2) . . ? O5B Ce1B N2B 128.8(2) . . ? O4B Ce1B N3B 127.95(18) . . ? O3B Ce1B N3B 64.75(19) . . ? O1B Ce1B N3B 140.5(2) . . ? O2B Ce1B N3B 73.4(2) . . ? O5B Ce1B N3B 128.3(2) . . ? N2B Ce1B N3B 66.9(2) . . ? O4B Ce1B N1B 72.7(3) . . ? O3B Ce1B N1B 140.7(2) . . ? O1B Ce1B N1B 64.2(2) . . ? O2B Ce1B N1B 129.0(2) . . ? O5B Ce1B N1B 130.0(2) . . ? N2B Ce1B N1B 67.1(3) . . ? N3B Ce1B N1B 101.7(2) . . ? O4B Ce1B N4B 64.2(2) . . ? O3B Ce1B N4B 75.0(2) . . ? O1B Ce1B N4B 127.1(2) . . ? O2B Ce1B N4B 139.7(2) . . ? O5B Ce1B N4B 129.0(2) . . ? N2B Ce1B N4B 102.2(2) . . ? N3B Ce1B N4B 66.6(2) . . ? N1B Ce1B N4B 66.0(2) . . ? C11B O1B Ce1B 125.4(5) . . ? C21B O2B Ce1B 124.3(7) . . ? C31B O3B Ce1B 124.8(5) . . ? C41B O4B Ce1B 126.0(5) . . ? C8B N1B C10B 110.6(9) . . ? C8B N1B C1B 107.6(8) . . ? C10B N1B C1B 109.9(8) . . ? C8B N1B Ce1B 112.2(6) . . ? C10B N1B Ce1B 105.8(5) . . ? C1B N1B Ce1B 110.7(6) . . ? C3B N2B C20B 110.8(8) . . ? C3B N2B C2B 110.3(7) . . ? C20B N2B C2B 107.2(8) . . ? C3B N2B Ce1B 112.6(5) . . ? C20B N2B Ce1B 105.8(5) . . ? C2B N2B Ce1B 109.9(6) . . ? C5B N3B C30B 111.5(7) . . ? C5B N3B C4B 109.4(7) . . ? C30B N3B C4B 109.2(7) . . ? C5B N3B Ce1B 111.3(5) . . ? C30B N3B Ce1B 106.1(4) . . ? C4B N3B Ce1B 109.3(5) . . ? C40B N4B C7B 112.6(9) . . ? C40B N4B C6B 110.9(7) . . ? C7B N4B C6B 108.3(8) . . ? C40B N4B Ce1B 106.6(5) . . ? C7B N4B Ce1B 110.8(5) . . ? C6B N4B Ce1B 107.5(5) . . ? C11B N11B C12B 121.3(8) . . ? C21B N21B C22B 121.3(8) . . ? C31B N31B C32B 120.3(7) . . ? C41B N41B C42B 122.3(7) . . ? C2B C1B N1B 113.4(8) . . ? C1B C2B N2B 114.0(9) . . ? N2B C3B C4B 116.0(7) . . ? C3B C4B N3B 112.7(8) . . ? N3B C5B C6B 112.5(8) . . ? N4B C6B C5B 114.3(7) . . ? N4B C7B C8B 113.1(8) . . ? N1B C8B C7B 113.6(9) . . ? N1B C10B C11B 111.3(8) . . ? O1B C11B N11B 121.3(8) . . ? O1B C11B C10B 120.2(7) . . ? N11B C11B C10B 118.4(8) . . ? C14B C12B N11B 113.5(8) . . ? C14B C12B C13B 112.8(8) . . ? N11B C12B C13B 106.9(8) . . ? C19B C14B C15B 119.8(10) . . ? C19B C14B C12B 122.2(10) . . ? C15B C14B C12B 118.0(10) . . ? C16B C15B C14B 119.9(11) . . ? C15B C16B C17B 118.1(12) . . ? C16B C17B C18B 124.4(14) . . ? C17B C18B C19B 117.5(13) . . ? C14B C19B C18B 120.1(12) . . ? N2B C20B C21B 110.5(7) . . ? O2B C21B N21B 121.8(10) . . ? O2B C21B C20B 119.5(10) . . ? N21B C21B C20B 118.6(8) . . ? N21B C22B C24B 109.4(8) . . ? N21B C22B C23B 106.8(8) . . ? C24B C22B C23B 109.5(12) . . ? C25B C24B C29B 120.8(14) . . ? C25B C24B C22B 122.5(10) . . ? C29B C24B C22B 116.7(12) . . ? C24B C25B C26B 121.8(12) . . ? C27B C26B C25B 117.8(15) . . ? C26B C27B C28B 122.9(15) . . ? C29B C28B C27B 117.0(13) . . ? C28B C29B C24B 119.4(16) . . ? N3B C30B C31B 112.5(7) . . ? O3B C31B N31B 122.2(7) . . ? O3B C31B C30B 120.1(7) . . ? N31B C31B C30B 117.6(8) . . ? N31B C32B C33B 108.9(7) . . ? N31B C32B C34B 111.5(7) . . ? C33B C32B C34B 112.6(7) . . ? C39B C34B C35B 120.7(10) . . ? C39B C34B C32B 119.4(9) . . ? C35B C34B C32B 119.9(9) . . ? C36B C35B C34B 116.8(14) . . ? C35B C36B C37B 118.8(13) . . ? C38B C37B C36B 122.3(12) . . ? C37B C38B C39B 121.8(15) . . ? C34B C39B C38B 119.3(12) . . ? N4B C40B C41B 111.0(7) . . ? O4B C41B N41B 119.8(8) . . ? O4B C41B C40B 119.6(8) . . ? N41B C41B C40B 120.2(7) . . ? N41B C42B C43B 109.4(7) . . ? N41B C42B C44B 110.6(7) . . ? C43B C42B C44B 114.7(7) . . ? C49B C44B C45B 118.5(7) . . ? C49B C44B C42B 121.5(8) . . ? C45B C44B C42B 119.7(7) . . ? C46B C45B C44B 122.3(8) . . ? C45B C46B C47B 118.2(9) . . ? C48B C47B C46B 119.9(9) . . ? C49B C48B C47B 121.8(8) . . ? C48B C49B C44B 119.1(8) . . ? O11 S1 O12 115.2(4) . . ? O11 S1 O13 114.6(5) . . ? O12 S1 O13 115.3(4) . . ? O11 S1 C1S 103.8(7) . . ? O12 S1 C1S 103.2(5) . . ? O13 S1 C1S 102.3(6) . . ? F11 C1S F12 111.5(12) . . ? F11 C1S F13 109.9(13) . . ? F12 C1S F13 108.9(13) . . ? F11 C1S S1 110.2(12) . . ? F12 C1S S1 110.2(9) . . ? F13 C1S S1 105.8(9) . . ? O23 S2 O21 115.8(5) . . ? O23 S2 O22 113.8(6) . . ? O21 S2 O22 114.4(4) . . ? O23 S2 C2S 102.6(6) . . ? O21 S2 C2S 104.3(5) . . ? O22 S2 C2S 103.8(4) . . ? F21 C2S F22 108.0(8) . . ? F21 C2S F23 106.9(7) . . ? F22 C2S F23 102.4(8) . . ? F21 C2S S2 114.2(7) . . ? F22 C2S S2 112.9(6) . . ? F23 C2S S2 111.7(7) . . ? O31 S3 O33 116.9(5) . . ? O31 S3 O32 115.2(4) . . ? O33 S3 O32 113.1(4) . . ? O31 S3 C3S 102.7(4) . . ? O33 S3 C3S 102.0(5) . . ? O32 S3 C3S 104.4(5) . . ? F33 C3S F31 106.4(9) . . ? F33 C3S F32 106.8(9) . . ? F31 C3S F32 107.7(9) . . ? F33 C3S S3 112.1(8) . . ? F31 C3S S3 112.2(7) . . ? F32 C3S S3 111.3(7) . . ? O41 S4 O42 118.1(7) . . ? O41 S4 O43 112.6(6) . . ? O42 S4 O43 114.3(6) . . ? O41 S4 C4S 102.4(7) . . ? O42 S4 C4S 104.3(6) . . ? O43 S4 C4S 102.7(8) . . ? C4S S4' F43 59.1(13) . . ? C4S S4' O42 122.6(19) . . ? F43 S4' O42 145.1(17) . . ? C4S S4' O43 110.0(16) . . ? F43 S4' O43 124.5(16) . . ? O42 S4' O43 89.0(12) . . ? S4 O42 S4' 47.6(8) . . ? S4 O43 S4' 42.6(8) . . ? S4' C4S F42 131.8(19) . . ? S4' C4S F43 67.1(15) . . ? F42 C4S F43 107.3(15) . . ? S4' C4S F41 118.7(18) . . ? F42 C4S F41 108.9(16) . . ? F43 C4S F41 106.1(11) . . ? S4' C4S S4 43.4(11) . . ? F42 C4S S4 111.4(9) . . ? F43 C4S S4 109.9(13) . . ? F41 C4S S4 112.8(12) . . ? C4S F43 S4' 53.8(11) . . ? C5S' S5 O53 93.1(17) . . ? C5S' S5 O52 82.3(14) . . ? O53 S5 O52 122.4(13) . . ? C5S' S5 O51 123.1(14) . . ? O53 S5 O51 112.0(12) . . ? O52 S5 O51 118.2(8) . . ? C5S' S5 C5S 49(2) . . ? O53 S5 C5S 103(2) . . ? O52 S5 C5S 116(2) . . ? O51 S5 C5S 75.2(19) . . ? S5 O51 C5S 56.3(17) . . ? S5 O52 C5S' 39.8(9) . . ? S5 O53 C5S' 36.9(10) . . ? F52 C5S F51 102(5) . . ? F52 C5S S5 149(5) . . ? F51 C5S S5 108(3) . . ? F52 C5S O51 123(4) . . ? F51 C5S O51 118(3) . . ? S5 C5S O51 48.6(16) . . ? F52 C5S F53 68(3) . . ? F51 C5S F53 82(3) . . ? S5 C5S F53 108(3) . . ? O51 C5S F53 151(4) . . ? S5 C5S' F52' 164(2) . . ? S5 C5S' O52 58.0(13) . . ? F52' C5S' O52 112.7(17) . . ? S5 C5S' F53 140(2) . . ? F52' C5S' F53 49.3(15) . . ? O52 C5S' F53 162(2) . . ? S5 C5S' F51 118.9(17) . . ? F52' C5S' F51 74.5(16) . . ? O52 C5S' F51 103.3(14) . . ? F53 C5S' F51 70.5(16) . . ? S5 C5S' O53 50.0(13) . . ? F52' C5S' O53 121.9(18) . . ? O52 C5S' O53 90.4(16) . . ? F53 C5S' O53 102.8(18) . . ? F51 C5S' O53 152.9(16) . . ? C5S F51 C5S' 44(2) . . ? C5S F52 F53 69(3) . . ? F53 F52' C5S' 70(2) . . ? F52' F53 F52 136(3) . . ? F52' F53 C5S' 60(2) . . ? F52 F53 C5S' 85(2) . . ? F52' F53 C5S 96(3) . . ? F52 F53 C5S 43(2) . . ? C5S' F53 C5S 43(2) . . ? O62 S6 O61 119.5(6) . . ? O62 S6 O63 109.5(7) . . ? O61 S6 O63 115.5(7) . . ? O62 S6 C6S 104.8(6) . . ? O61 S6 C6S 104.2(5) . . ? O63 S6 C6S 100.7(7) . . ? F62 C6S F63 110.9(10) . . ? F62 C6S F61 103.2(11) . . ? F63 C6S F61 103.1(11) . . ? F62 C6S S6 114.5(9) . . ? F63 C6S S6 115.8(9) . . ? F61 C6S S6 107.7(8) . . ? O1S C7S C8S 104.2(18) . . ? C10S C9S O2S 116(3) . . ? O3S C11S C12S 109(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11A H11A O23 0.88 2.00 2.876(11) 170.1 2_646 N21A H21A O61 0.88 2.08 2.929(10) 162.6 1_545 N31A H31A O12 0.88 2.02 2.826(9) 150.9 4 N41A H41A O31 0.88 2.03 2.891(8) 166.9 3_554 O5A H01A O41 0.84 2.05 2.892(9) 179.9 . O5A H02A O1S 0.84 1.87 2.711(12) 179.2 . N11B H11B O21 0.88 2.13 2.989(11) 166.5 . N21B H21B O32 0.88 2.01 2.874(10) 168.7 . N31B H31B O13 0.88 1.98 2.847(10) 166.8 . N41B H41B O62 0.88 2.07 2.871(12) 151.5 . O5B H01B O52 0.72 2.15 2.872(14) 179.3 . O5B H02B O2S 0.68 2.02 2.70(2) 179.9 . O1S H01S O1W 0.85 1.94 2.77(2) 165.8 . O1W H1W1 O22 0.85 2.20 2.872(19) 136.1 2_656 O1W H2W1 O43 0.85 2.18 2.95(2) 151.1 . O2S H02S O2W 0.85 1.98 2.77(3) 153.8 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.502 _refine_diff_density_min -3.119 _refine_diff_density_rms 0.162 #=============================================END data_9b _database_code_CSD 182452 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 N8 O5 Pr 3+,3(C F3 O3 S 1-),C2 H6 O,H2 O' _chemical_formula_sum 'C53 H74 F9 N8 O16 Pr S3' _chemical_formula_weight 1487.29 _chemical_absolute_configuration ad _chemical_optical_rotation ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 32.148(9) _cell_length_b 12.713(4) _cell_length_c 32.952(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.70(1) _cell_angle_gamma 90.00 _cell_volume 13439(11) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6112 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8290 _exptl_absorpt_correction_T_max 0.9099 _exptl_absorpt_process_details 'XPREP (SHELXTL), R(int)=0.080 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 -1.00 0.0800 -1.00 0.00 1.00 0.0800 0.00 2.00 3.00 0.0600 0.00 -3.00 -2.00 0.0600 1.00 0.00 1.00 0.1100 -1.00 0.00 -1.00 0.1100 0.00 0.00 1.00 0.1000 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. Merging Friedel equivalents yields 17762 unique reflections. ; _diffrn_ambient_temperature 120(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 'SMART 6000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 86128 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.50 _reflns_number_total 34025 _reflns_number_gt 22804 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.806 _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. Triflate ligand containing S(5) displays chaotic disorder, for which no satisfactory model was found. Positions O(1S)C(7S)C(8S) and O(2S)C(9S)C(10S)are shared between water and ethanol (assumed occupancies 50% and 50% for the former, 30% and 50% in the latter), ethanol O(3S)C(11S)C(12S) was refined with 50% occupancy, water O(2W) - 70% occupancy. The total amount of the crystallisation solvent was estimated from the sizes of the cavities. ; _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^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.029(9) _refine_ls_number_reflns 34025 _refine_ls_number_parameters 1605 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.009 _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 Pr1A Pr 0.505226(9) 0.37322(2) 0.303745(8) 0.02669(7) Uani 1 1 d . . . O1A O 0.54317(12) 0.2438(3) 0.34423(12) 0.0333(9) Uani 1 1 d . . . O2A O 0.44589(12) 0.3380(3) 0.34613(11) 0.0284(8) Uani 1 1 d . . . O3A O 0.47802(12) 0.5500(3) 0.29888(13) 0.0329(9) Uani 1 1 d . . . O4A O 0.57299(13) 0.4548(3) 0.29570(12) 0.0339(9) Uani 1 1 d . . . O5A O 0.52660(14) 0.4566(4) 0.36928(12) 0.0404(10) Uani 1 1 d . . . H01A H 0.5468 0.4352 0.3851 0.061 Uiso 1 1 d R . . H02A H 0.5259 0.5224 0.3737 0.061 Uiso 1 1 d R . . N1A N 0.54984(15) 0.2292(4) 0.26104(15) 0.0320(11) Uani 1 1 d . . . N2A N 0.46361(16) 0.1870(4) 0.28815(14) 0.0297(11) Uani 1 1 d . . . N3A N 0.43366(14) 0.3957(3) 0.25446(14) 0.0286(11) Uani 1 1 d . . . N4A N 0.51911(15) 0.4410(4) 0.22679(14) 0.0300(11) Uani 1 1 d . . . N11A N 0.58688(15) 0.1099(4) 0.35719(15) 0.0383(12) Uani 1 1 d . . . H11A H 0.6033 0.0620 0.3474 0.046 Uiso 1 1 d R . . N21A N 0.39510(15) 0.2350(4) 0.36785(15) 0.0320(11) Uani 1 1 d . . . H21A H 0.3819 0.1743 0.3656 0.038 Uiso 1 1 d R . . N31A N 0.43069(15) 0.6723(4) 0.28082(15) 0.0322(11) Uani 1 1 d . . . H31A H 0.4060 0.6874 0.2693 0.039 Uiso 1 1 d R . . N41A N 0.62129(15) 0.5398(4) 0.25997(15) 0.0330(11) Uani 1 1 d . . . H41A H 0.6273 0.5666 0.2364 0.040 Uiso 1 1 d R . . C1A C 0.52309(18) 0.1402(5) 0.24604(18) 0.0361(13) Uani 1 1 d . . . H11 H 0.5411 0.0810 0.2385 0.043 Uiso 1 1 d R . . H12 H 0.5068 0.1632 0.2211 0.043 Uiso 1 1 d R . . C2A C 0.49328(19) 0.1009(4) 0.27648(18) 0.0335(13) Uani 1 1 d . . . H21 H 0.5094 0.0748 0.3011 0.040 Uiso 1 1 d R . . H22 H 0.4769 0.0413 0.2645 0.040 Uiso 1 1 d R . . C3A C 0.42980(18) 0.2002(5) 0.25526(19) 0.0330(13) Uani 1 1 d . . . H31 H 0.4421 0.1960 0.2285 0.040 Uiso 1 1 d R . . H32 H 0.4098 0.1412 0.2569 0.040 Uiso 1 1 d R . . C4A C 0.40687(18) 0.3006(5) 0.25708(18) 0.0310(12) Uani 1 1 d . . . H41 H 0.3932 0.3030 0.2831 0.037 Uiso 1 1 d R . . H42 H 0.3847 0.3028 0.2348 0.037 Uiso 1 1 d R . . C5A C 0.44284(19) 0.4104(5) 0.21132(18) 0.0359(14) Uani 1 1 d . . . H51 H 0.4179 0.4406 0.1963 0.043 Uiso 1 1 d R . . H52 H 0.4482 0.3405 0.1994 0.043 Uiso 1 1 d R . . C6A C 0.48011(19) 0.4823(5) 0.20551(18) 0.0346(13) Uani 1 1 d . . . H61 H 0.4844 0.4880 0.1761 0.042 Uiso 1 1 d R . . H62 H 0.4741 0.5537 0.2157 0.042 Uiso 1 1 d R . . C7A C 0.53603(18) 0.3525(5) 0.20245(18) 0.0356(14) Uani 1 1 d . . . H71 H 0.5490 0.3823 0.1785 0.043 Uiso 1 1 d R . . H72 H 0.5124 0.3077 0.1922 0.043 Uiso 1 1 d R . . C8A C 0.56786(19) 0.2823(5) 0.22642(18) 0.0334(13) Uani 1 1 d . . . H81 H 0.5784 0.2284 0.2080 0.040 Uiso 1 1 d R . . H82 H 0.5918 0.3264 0.2365 0.040 Uiso 1 1 d R . . C10A C 0.5838(2) 0.1892(5) 0.29034(18) 0.0387(14) Uani 1 1 d . . . H101 H 0.6079 0.2378 0.2905 0.046 Uiso 1 1 d R . . H102 H 0.5931 0.1194 0.2811 0.046 Uiso 1 1 d R . . C11A C 0.56967(19) 0.1801(5) 0.33277(19) 0.0347(13) Uani 1 1 d . . . C12A C 0.5800(2) 0.1085(5) 0.40081(19) 0.0426(15) Uani 1 1 d . . . H12A H 0.5845 0.1815 0.4116 0.051 Uiso 1 1 d R . . C13A C 0.6125(2) 0.0379(7) 0.4231(2) 0.060(2) Uani 1 1 d . . . H131 H 0.6408 0.0651 0.4202 0.090 Uiso 1 1 d R . . H132 H 0.6104 -0.0335 0.4117 0.090 Uiso 1 1 d R . . H133 H 0.6073 0.0351 0.4522 0.090 Uiso 1 1 d R . . C14A C 0.5356(2) 0.0755(5) 0.4083(2) 0.0429(16) Uani 1 1 d . . . C15A C 0.5189(3) -0.0177(6) 0.3942(2) 0.0518(18) Uani 1 1 d . . . H15A H 0.5352 -0.0633 0.3788 0.062 Uiso 1 1 d R . . C16A C 0.4789(3) -0.0467(8) 0.4028(3) 0.069(3) Uani 1 1 d . . . H16A H 0.4675 -0.1117 0.3930 0.083 Uiso 1 1 d R . . C17 C 0.4555(3) 0.0189(11) 0.4248(3) 0.082(3) Uani 1 1 d . . . H17A H 0.4279 -0.0004 0.4305 0.098 Uiso 1 1 d R . . C18A C 0.4705(3) 0.1095(10) 0.4386(3) 0.082(3) Uani 1 1 d . . . H18A H 0.4540 0.1544 0.4541 0.099 Uiso 1 1 d R . . C19A C 0.5116(3) 0.1412(7) 0.4311(2) 0.062(2) Uani 1 1 d . . . H19A H 0.5224 0.2070 0.4405 0.074 Uiso 1 1 d R . . C20A C 0.44585(19) 0.1556(4) 0.32632(18) 0.0331(13) Uani 1 1 d . . . H201 H 0.4676 0.1220 0.3446 0.040 Uiso 1 1 d R . . H202 H 0.4233 0.1035 0.3204 0.040 Uiso 1 1 d R . . C21A C 0.42860(17) 0.2507(4) 0.34719(17) 0.0285(12) Uani 1 1 d . . . C22A C 0.3795(2) 0.3174(5) 0.39490(18) 0.0360(14) Uani 1 1 d . . . H22A H 0.4035 0.3471 0.4120 0.043 Uiso 1 1 d R . . C23A C 0.3498(2) 0.2646(6) 0.4229(2) 0.0504(19) Uani 1 1 d . . . H231 H 0.3640 0.2084 0.4392 0.076 Uiso 1 1 d R . . H232 H 0.3262 0.2333 0.4065 0.076 Uiso 1 1 d R . . H233 H 0.3391 0.3174 0.4415 0.076 Uiso 1 1 d R . . C24A C 0.35900(19) 0.4052(5) 0.37008(18) 0.0355(14) Uani 1 1 d . . . C25A C 0.32622(19) 0.3868(6) 0.3406(2) 0.0472(16) Uani 1 1 d . . . H25A H 0.3166 0.3169 0.3356 0.057 Uiso 1 1 d R . . C26A C 0.3070(2) 0.4710(7) 0.3184(2) 0.0556(19) Uani 1 1 d . . . H26A H 0.2853 0.4577 0.2981 0.067 Uiso 1 1 d R . . C27A C 0.3201(2) 0.5729(6) 0.3265(2) 0.054(2) Uani 1 1 d . . . H27A H 0.3065 0.6297 0.3124 0.065 Uiso 1 1 d R . . C28A C 0.3524(2) 0.5921(5) 0.3547(2) 0.0450(17) Uani 1 1 d . . . H28A H 0.3620 0.6621 0.3593 0.054 Uiso 1 1 d R . . C29A C 0.3720(2) 0.5097(5) 0.37650(19) 0.0410(15) Uani 1 1 d . . . H29A H 0.3943 0.5240 0.3960 0.049 Uiso 1 1 d R . . C30A C 0.41243(18) 0.4894(5) 0.26905(17) 0.0311(13) Uani 1 1 d . . . H301 H 0.3955 0.4690 0.2918 0.037 Uiso 1 1 d R . . H302 H 0.3933 0.5174 0.2469 0.037 Uiso 1 1 d R . . C31A C 0.44272(19) 0.5745(5) 0.28328(18) 0.0310(13) Uani 1 1 d . . . C32A C 0.4576(2) 0.7581(5) 0.2969(2) 0.0378(14) Uani 1 1 d . . . H32A H 0.4712 0.7348 0.3235 0.045 Uiso 1 1 d R . . C33A C 0.4305(2) 0.8538(5) 0.3045(2) 0.0433(16) Uani 1 1 d . . . H331 H 0.4086 0.8346 0.3226 0.065 Uiso 1 1 d R . . H332 H 0.4176 0.8801 0.2787 0.065 Uiso 1 1 d R . . H333 H 0.4481 0.9092 0.3173 0.065 Uiso 1 1 d R . . C34A C 0.4917(2) 0.7839(5) 0.2684(2) 0.0410(15) Uani 1 1 d . . . C35A C 0.4824(2) 0.7936(6) 0.2264(2) 0.0519(19) Uani 1 1 d . . . H35A H 0.4547 0.7847 0.2150 0.062 Uiso 1 1 d R . . C36A C 0.5153(4) 0.8180(7) 0.2022(3) 0.080(3) Uani 1 1 d . . . H36A H 0.5099 0.8235 0.1736 0.097 Uiso 1 1 d R . . C37A C 0.5552(3) 0.8327(7) 0.2197(5) 0.091(4) Uani 1 1 d . . . H37A H 0.5767 0.8507 0.2025 0.109 Uiso 1 1 d R . . C38A C 0.5645(3) 0.8229(8) 0.2601(4) 0.079(3) Uani 1 1 d . . . H38A H 0.5923 0.8337 0.2709 0.095 Uiso 1 1 d R . . C39A C 0.5319(2) 0.7978(6) 0.2854(3) 0.061(2) Uani 1 1 d . . . H39A H 0.5378 0.7903 0.3138 0.074 Uiso 1 1 d R . . C40A C 0.54992(18) 0.5278(5) 0.23111(18) 0.0341(13) Uani 1 1 d . . . H401 H 0.5356 0.5942 0.2375 0.041 Uiso 1 1 d R . . H402 H 0.5630 0.5375 0.2049 0.041 Uiso 1 1 d R . . C41A C 0.58343(19) 0.5045(5) 0.26407(18) 0.0297(13) Uani 1 1 d . . . C42A C 0.65466(19) 0.5371(5) 0.29369(19) 0.0348(13) Uani 1 1 d . . . H42A H 0.6444 0.5757 0.3175 0.042 Uiso 1 1 d R . . C43A C 0.6920(2) 0.5945(5) 0.2794(2) 0.0471(17) Uani 1 1 d . . . H431 H 0.6850 0.6681 0.2702 0.071 Uiso 1 1 d R . . H432 H 0.7042 0.5582 0.2557 0.071 Uiso 1 1 d R . . H433 H 0.7149 0.6002 0.3017 0.071 Uiso 1 1 d R . . C44A C 0.66506(18) 0.4244(5) 0.30697(18) 0.0352(13) Uani 1 1 d . . . C45A C 0.68189(19) 0.3535(5) 0.28104(19) 0.0406(16) Uani 1 1 d . . . H45A H 0.6856 0.3739 0.2538 0.049 Uiso 1 1 d R . . C46A C 0.6932(2) 0.2537(5) 0.2935(2) 0.0478(17) Uani 1 1 d . . . H46A H 0.7047 0.2058 0.2751 0.057 Uiso 1 1 d R . . C47A C 0.6881(2) 0.2235(6) 0.3338(2) 0.0472(17) Uani 1 1 d . . . H47A H 0.6967 0.1556 0.3432 0.057 Uiso 1 1 d R . . C48A C 0.6704(2) 0.2931(5) 0.3599(2) 0.0442(16) Uani 1 1 d . . . H48A H 0.6657 0.2726 0.3870 0.053 Uiso 1 1 d R . . C49 C 0.65898(18) 0.3947(5) 0.34654(18) 0.0395(16) Uani 1 1 d . . . H49A H 0.6472 0.4431 0.3646 0.047 Uiso 1 1 d R . . Pr1B Pr 0.194121(10) 0.62679(3) 0.494138(9) 0.03469(9) Uani 1 1 d . . . O1B O 0.18643(15) 0.7232(4) 0.55627(13) 0.0483(12) Uani 1 1 d . . . O2B O 0.14452(14) 0.5032(4) 0.51802(14) 0.0473(12) Uani 1 1 d . . . O3B O 0.16482(13) 0.5773(3) 0.42790(12) 0.0356(10) Uani 1 1 d . . . O4B O 0.20802(14) 0.7942(3) 0.46500(14) 0.0423(11) Uani 1 1 d . . . O5B O 0.12508(14) 0.7136(4) 0.48512(14) 0.0494(12) Uani 1 1 d . . . H01B H 0.1067 0.7044 0.4657 0.074 Uiso 1 1 d R . . H02B H 0.1191 0.7773 0.4900 0.074 Uiso 1 1 d R . . N1B N 0.26659(19) 0.6978(5) 0.53184(17) 0.0517(16) Uani 1 1 d . . . N2B N 0.22389(19) 0.4999(5) 0.55581(17) 0.0495(15) Uani 1 1 d . . . N3B N 0.21636(16) 0.4324(4) 0.46781(16) 0.0374(12) Uani 1 1 d . . . N4B N 0.25936(16) 0.6337(5) 0.44401(15) 0.0410(12) Uani 1 1 d . . . N11B N 0.2071(2) 0.8284(5) 0.60776(17) 0.0536(16) Uani 1 1 d . . . H10B H 0.2270 0.8683 0.6191 0.064 Uiso 1 1 d R . . N21B N 0.1189(2) 0.3939(6) 0.5647(2) 0.075(2) Uani 1 1 d . . . H20B H 0.1227 0.3617 0.5882 0.090 Uiso 1 1 d R . . N31B N 0.14797(17) 0.4644(4) 0.37705(16) 0.0416(13) Uani 1 1 d . . . H30B H 0.1516 0.4019 0.3663 0.050 Uiso 1 1 d R . . N41B N 0.23466(18) 0.9101(4) 0.42222(16) 0.0421(13) Uani 1 1 d . . . H40B H 0.2519 0.9221 0.4030 0.050 Uiso 1 1 d R . . C1B C 0.2856(2) 0.6155(6) 0.5604(2) 0.060(2) Uani 1 1 d . . . H13 H 0.3055 0.6512 0.5800 0.072 Uiso 1 1 d R . . H14 H 0.3017 0.5651 0.5446 0.072 Uiso 1 1 d R . . C2B C 0.2551(3) 0.5585(6) 0.5829(2) 0.058(2) Uani 1 1 d . . . H23 H 0.2701 0.5077 0.6014 0.069 Uiso 1 1 d R . . H24 H 0.2400 0.6084 0.5998 0.069 Uiso 1 1 d R . . C3B C 0.2423(2) 0.4038(6) 0.5406(2) 0.054(2) Uani 1 1 d . . . H33 H 0.2436 0.3507 0.5627 0.065 Uiso 1 1 d R . . H34 H 0.2714 0.4197 0.5343 0.065 Uiso 1 1 d R . . C4B C 0.2197(2) 0.3557(5) 0.50311(19) 0.0456(17) Uani 1 1 d . . . H43 H 0.2351 0.2925 0.4949 0.055 Uiso 1 1 d R . . H44 H 0.1914 0.3331 0.5099 0.055 Uiso 1 1 d R . . C5B C 0.2577(2) 0.4377(5) 0.4488(2) 0.0438(16) Uani 1 1 d . . . H53 H 0.2612 0.3726 0.4328 0.053 Uiso 1 1 d R . . H54 H 0.2805 0.4403 0.4704 0.053 Uiso 1 1 d R . . C6B C 0.2607(2) 0.5316(5) 0.4213(2) 0.0422(16) Uani 1 1 d . . . H63 H 0.2874 0.5276 0.4078 0.051 Uiso 1 1 d R . . H64 H 0.2377 0.5299 0.3999 0.051 Uiso 1 1 d R . . C7B C 0.3003(2) 0.6490(6) 0.4681(2) 0.056(2) Uani 1 1 d . . . H73 H 0.3215 0.6729 0.4497 0.067 Uiso 1 1 d R . . H74 H 0.3096 0.5805 0.4797 0.067 Uiso 1 1 d R . . C8B C 0.2977(2) 0.7279(7) 0.5021(2) 0.057(2) Uani 1 1 d . . . H83 H 0.3255 0.7348 0.5167 0.069 Uiso 1 1 d R . . H84 H 0.2900 0.7975 0.4904 0.069 Uiso 1 1 d R . . C10B C 0.2554(2) 0.7923(6) 0.5547(2) 0.056(2) Uani 1 1 d . . . H103 H 0.2773 0.8068 0.5765 0.067 Uiso 1 1 d R . . H104 H 0.2537 0.8537 0.5362 0.067 Uiso 1 1 d R . . C11B C 0.2137(2) 0.7782(5) 0.5730(2) 0.0466(17) Uani 1 1 d . . . C12B C 0.1671(3) 0.8188(7) 0.6279(2) 0.059(2) Uani 1 1 d . . . H12B H 0.1440 0.8307 0.6066 0.070 Uiso 1 1 d R . . C13B C 0.1650(3) 0.9079(7) 0.6588(3) 0.074(3) Uani 1 1 d . . . H134 H 0.1397 0.8987 0.6737 0.111 Uiso 1 1 d R . . H135 H 0.1641 0.9775 0.6456 0.111 Uiso 1 1 d R . . H136 H 0.1897 0.9040 0.6780 0.111 Uiso 1 1 d R . . C14B C 0.1606(3) 0.7134(6) 0.6453(2) 0.061(2) Uani 1 1 d . . . C15B C 0.1950(3) 0.6702(7) 0.6709(2) 0.062(2) Uani 1 1 d . . . H15B H 0.2207 0.7070 0.6752 0.075 Uiso 1 1 d R . . C16B C 0.1904(4) 0.5783(9) 0.6893(3) 0.084(3) Uani 1 1 d . . . H16B H 0.2122 0.5474 0.7061 0.101 Uiso 1 1 d R . . C17B C 0.1531(4) 0.5262(10) 0.6828(3) 0.097(4) Uani 1 1 d . . . H17B H 0.1500 0.4594 0.6952 0.117 Uiso 1 1 d R . . C18B C 0.1185(3) 0.5669(9) 0.6582(4) 0.089(3) Uani 1 1 d . . . H18B H 0.0926 0.5304 0.6550 0.106 Uiso 1 1 d R . . C19B C 0.1238(3) 0.6582(8) 0.6402(3) 0.072(3) Uani 1 1 d . . . H19B H 0.1016 0.6865 0.6231 0.087 Uiso 1 1 d R . . C20B C 0.1875(2) 0.4760(7) 0.5798(2) 0.0539(19) Uani 1 1 d . . . H203 H 0.1937 0.4117 0.5961 0.065 Uiso 1 1 d R . . H204 H 0.1822 0.5342 0.5988 0.065 Uiso 1 1 d R . . C21B C 0.1485(2) 0.4561(6) 0.5518(2) 0.0502(18) Uani 1 1 d . . . C22B C 0.0794(2) 0.3812(8) 0.5401(3) 0.069(2) Uani 1 1 d . . . H22B H 0.0673 0.4520 0.5331 0.083 Uiso 1 1 d R . . C23B C 0.0495(3) 0.3178(10) 0.5675(3) 0.101(4) Uani 1 1 d . . . H234 H 0.0486 0.3492 0.5953 0.151 Uiso 1 1 d R . . H235 H 0.0582 0.2431 0.5709 0.151 Uiso 1 1 d R . . H236 H 0.0203 0.3196 0.5548 0.151 Uiso 1 1 d R . . C24B C 0.0855(2) 0.3206(8) 0.5027(3) 0.072(3) Uani 1 1 d . . . C25B C 0.1057(3) 0.2234(8) 0.5027(3) 0.073(3) Uani 1 1 d . . . H25B H 0.1159 0.1932 0.5278 0.087 Uiso 1 1 d R . . C26B C 0.1112(3) 0.1702(9) 0.4679(4) 0.084(3) Uani 1 1 d . . . H26B H 0.1257 0.1049 0.4684 0.100 Uiso 1 1 d R . . C27B C 0.0960(3) 0.2093(11) 0.4328(4) 0.095(3) Uani 1 1 d . . . H27B H 0.0991 0.1712 0.4084 0.114 Uiso 1 1 d R . . C28B C 0.0754(3) 0.3076(12) 0.4293(4) 0.105(5) Uani 1 1 d . . . H28B H 0.0649 0.3351 0.4038 0.126 Uiso 1 1 d R . . C29B C 0.0708(2) 0.3613(10) 0.4655(3) 0.084(3) Uani 1 1 d . . . H29B H 0.0573 0.4279 0.4646 0.101 Uiso 1 1 d R . . C30B C 0.1833(2) 0.3966(5) 0.43845(19) 0.0412(16) Uani 1 1 d . . . H303 H 0.1610 0.3629 0.4533 0.049 Uiso 1 1 d R . . H304 H 0.1948 0.3428 0.4205 0.049 Uiso 1 1 d R . . C31B C 0.16455(18) 0.4855(5) 0.41297(18) 0.0340(13) Uani 1 1 d . . . C32B C 0.1227(2) 0.5443(5) 0.35354(18) 0.0361(14) Uani 1 1 d . . . H32B H 0.1032 0.5765 0.3725 0.043 Uiso 1 1 d R . . C33B C 0.0962(2) 0.4877(6) 0.3199(2) 0.0517(19) Uani 1 1 d . . . H334 H 0.0800 0.4324 0.3324 0.078 Uiso 1 1 d R . . H335 H 0.1143 0.4560 0.3004 0.078 Uiso 1 1 d R . . H336 H 0.0772 0.5376 0.3056 0.078 Uiso 1 1 d R . . C34B C 0.1496(2) 0.6321(5) 0.33828(18) 0.0416(15) Uani 1 1 d . . . C35B C 0.1802(3) 0.6106(7) 0.3118(2) 0.064(2) Uani 1 1 d . . . H35B H 0.1843 0.5406 0.3027 0.077 Uiso 1 1 d R . . C36B C 0.2041(3) 0.6922(12) 0.2987(3) 0.096(4) Uani 1 1 d . . . H36B H 0.2257 0.6780 0.2812 0.115 Uiso 1 1 d R . . C37B C 0.1946(4) 0.7986(12) 0.3124(4) 0.107(6) Uani 1 1 d . . . H37B H 0.2107 0.8552 0.3029 0.129 Uiso 1 1 d R . . C38B C 0.1680(4) 0.8177(8) 0.3365(3) 0.092(4) Uani 1 1 d . . . H38B H 0.1631 0.8880 0.3448 0.110 Uiso 1 1 d R . . C39B C 0.1443(3) 0.7337(6) 0.3505(2) 0.060(2) Uani 1 1 d . . . H39B H 0.1241 0.7491 0.3695 0.072 Uiso 1 1 d R . . C40B C 0.2507(2) 0.7202(5) 0.4159(2) 0.0437(17) Uani 1 1 d . . . H403 H 0.2316 0.6952 0.3931 0.052 Uiso 1 1 d R . . H404 H 0.2769 0.7433 0.4045 0.052 Uiso 1 1 d R . . C41B C 0.2312(2) 0.8124(6) 0.43617(19) 0.0392(16) Uani 1 1 d . . . C42B C 0.2114(2) 0.9973(5) 0.43861(19) 0.0387(15) Uani 1 1 d . . . H42B H 0.1830 0.9711 0.4440 0.046 Uiso 1 1 d R . . C43B C 0.2060(2) 1.0823(6) 0.4067(2) 0.0506(18) Uani 1 1 d . . . H434 H 0.1951 1.0529 0.3800 0.076 Uiso 1 1 d R . . H435 H 0.2335 1.1179 0.4026 0.076 Uiso 1 1 d R . . H436 H 0.1862 1.1399 0.4139 0.076 Uiso 1 1 d R . . C44B C 0.2320(2) 1.0374(5) 0.47859(19) 0.0384(14) Uani 1 1 d . . . C45B C 0.2731(2) 1.0746(5) 0.4811(2) 0.0409(15) Uani 1 1 d . . . H45B H 0.2890 1.0718 0.4578 0.049 Uiso 1 1 d R . . C46B C 0.2907(2) 1.1145(6) 0.5168(2) 0.0508(17) Uani 1 1 d . . . H46B H 0.3184 1.1411 0.5179 0.061 Uiso 1 1 d R . . C47B C 0.2683(2) 1.1147(6) 0.5516(2) 0.0503(18) Uani 1 1 d . . . H47B H 0.2808 1.1412 0.5765 0.060 Uiso 1 1 d R . . C48B C 0.2283(2) 1.0793(5) 0.5495(2) 0.0486(17) Uani 1 1 d . . . H48B H 0.2130 1.0811 0.5732 0.058 Uiso 1 1 d R . . C49B C 0.2098(2) 1.0413(5) 0.5136(2) 0.0460(16) Uani 1 1 d . . . H49B H 0.1820 1.0162 0.5129 0.055 Uiso 1 1 d R . . S1 S 0.15414(5) 0.20249(13) 0.30999(5) 0.0418(4) Uani 1 1 d . . . O11 O 0.1518(2) 0.0902(4) 0.31138(16) 0.0662(16) Uani 1 1 d . . . O12 O 0.12996(16) 0.2514(4) 0.27697(16) 0.0563(13) Uani 1 1 d . . . O13 O 0.15223(16) 0.2541(4) 0.34811(15) 0.0508(12) Uani 1 1 d . . . C1S C 0.2081(3) 0.2332(9) 0.2973(2) 0.067(2) Uani 1 1 d . . . F11 F 0.2160(2) 0.1887(8) 0.26322(18) 0.151(4) Uani 1 1 d . . . F12 F 0.23485(14) 0.1930(5) 0.32609(16) 0.0906(18) Uani 1 1 d . . . F13 F 0.21242(17) 0.3367(6) 0.2954(2) 0.116(3) Uani 1 1 d . . . S2 S 0.31623(6) 0.89792(15) 0.66122(6) 0.0551(5) Uani 1 1 d . . . O21 O 0.2837(2) 0.9471(4) 0.63628(16) 0.0664(16) Uani 1 1 d . . . O22 O 0.32144(18) 0.7845(5) 0.65219(17) 0.0650(15) Uani 1 1 d . . . O23 O 0.35333(19) 0.9582(5) 0.6665(2) 0.0855(19) Uani 1 1 d . . . C2S C 0.2981(3) 0.8983(6) 0.7108(2) 0.0523(19) Uani 1 1 d . . . F21 F 0.32609(14) 0.8677(5) 0.73871(13) 0.0717(12) Uani 1 1 d . . . F22 F 0.26305(15) 0.8397(4) 0.71429(14) 0.0709(13) Uani 1 1 d . . . F23 F 0.28546(19) 0.9973(4) 0.72152(15) 0.0849(16) Uani 1 1 d . . . S3 S 0.14267(7) 0.20011(15) 0.64922(6) 0.0544(5) Uani 1 1 d . . . O31 O 0.12874(14) 0.1450(4) 0.68336(14) 0.0499(12) Uani 1 1 d . . . O32 O 0.12726(18) 0.3040(4) 0.64467(16) 0.0673(16) Uani 1 1 d . . . O33 O 0.14451(18) 0.1470(5) 0.61201(15) 0.0673(15) Uani 1 1 d . . . C3S C 0.1989(3) 0.2153(6) 0.6635(3) 0.062(2) Uani 1 1 d . . . F31 F 0.21733(14) 0.1232(4) 0.67116(15) 0.0735(13) Uani 1 1 d . . . F32 F 0.21892(16) 0.2607(4) 0.63404(17) 0.0838(16) Uani 1 1 d . . . F33 F 0.20596(18) 0.2736(5) 0.69633(17) 0.0909(17) Uani 1 1 d . . . S4 S 0.61420(7) 0.4384(2) 0.45629(6) 0.0640(6) Uani 1 1 d . . . O41 O 0.59524(17) 0.3851(5) 0.42260(14) 0.0690(15) Uani 1 1 d . . . O42 O 0.65154(18) 0.3997(6) 0.4741(2) 0.090(2) Uani 1 1 d . . . O43 O 0.6156(2) 0.5537(6) 0.4503(3) 0.106(3) Uani 1 1 d . . . C4S C 0.5791(4) 0.4271(9) 0.4944(3) 0.082(3) Uani 1 1 d . . . F41 F 0.5734(2) 0.3236(6) 0.5043(2) 0.114(2) Uani 1 1 d . . . F42 F 0.54157(18) 0.4638(6) 0.4824(2) 0.118(3) Uani 1 1 d . . . F43 F 0.5912(3) 0.4805(6) 0.52792(18) 0.137(3) Uani 1 1 d . . . S5 S 0.02811(12) 0.7054(3) 0.39364(11) 0.1159(12) Uani 1 1 d . . . O51 O 0.0335(3) 0.6982(6) 0.3506(2) 0.104(3) Uani 1 1 d . . . O52 O 0.0634(3) 0.6817(11) 0.4206(2) 0.174(6) Uani 1 1 d . . . O53 O -0.0061(8) 0.7751(16) 0.3983(5) 0.366(16) Uani 1 1 d . . . C5S C 0.0056(6) 0.6146(18) 0.3714(6) 0.079(5) Uiso 0.50 1 d P . . C5S' C 0.0008(8) 0.5949(19) 0.4046(8) 0.089(6) Uiso 0.50 1 d P . . F51 F 0.0225(4) 0.5138(10) 0.3932(4) 0.202(5) Uani 1 1 d . . . F52 F -0.0081(5) 0.5816(16) 0.4411(6) 0.349(12) Uani 1 1 d . . . F53 F -0.0331(5) 0.5848(13) 0.3841(12) 0.59(3) Uani 1 1 d . . . S6 S 0.32866(6) 0.97066(17) 0.35566(6) 0.0565(5) Uani 1 1 d . . . O61 O 0.36873(15) 1.0140(4) 0.36282(17) 0.0557(13) Uani 1 1 d . . . O62 O 0.2962(2) 1.0153(6) 0.3771(2) 0.095(2) Uani 1 1 d . . . O63 O 0.3269(3) 0.8601(6) 0.3556(3) 0.128(3) Uani 1 1 d . . . C6S C 0.3151(3) 1.0032(9) 0.3031(3) 0.073(3) Uani 1 1 d . . . F61 F 0.31862(19) 1.1114(5) 0.29806(18) 0.0991(18) Uani 1 1 d . . . F62 F 0.34155(19) 0.9634(7) 0.27863(17) 0.120(3) Uani 1 1 d . . . F63 F 0.27753(17) 0.9795(5) 0.28962(18) 0.0901(17) Uani 1 1 d . . . O1S O 0.5241(4) 0.6680(7) 0.3846(3) 0.142(4) Uani 1 1 d . . . C7S C 0.5110(6) 0.6771(16) 0.4243(6) 0.169(7) Uiso 1 1 d . . . C8S C 0.4678(7) 0.633(2) 0.4191(6) 0.197(8) Uiso 1 1 d . . . O2S O 0.1059(4) 0.9127(11) 0.4996(4) 0.161(5) Uiso 0.80 1 d P . . C9S C 0.0612(10) 0.942(3) 0.4642(10) 0.140(11) Uiso 0.50 1 d P . . C10S C 0.0811(12) 0.937(3) 0.4180(12) 0.174(14) Uiso 0.50 1 d P . . O3S O 0.0257(7) 0.9865(18) 0.6042(6) 0.141(7) Uiso 0.50 1 d P . . C11S C 0.0052(8) 1.063(2) 0.5912(8) 0.108(8) Uiso 0.50 1 d P . . C12S C 0.0016(9) 1.051(2) 0.5425(9) 0.121(9) Uiso 0.50 1 d P . . O1W O 0.6059(4) 0.7302(10) 0.3917(4) 0.174(4) Uiso 1 1 d . . . O2W O 0.0955(6) 0.9886(17) 0.5720(6) 0.202(8) Uiso 0.70 1 d P . . 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 Pr1A 0.02911(15) 0.02405(14) 0.02707(14) 0.00198(13) 0.00303(11) 0.00276(14) O1A 0.037(2) 0.028(2) 0.035(2) 0.0001(17) 0.0004(18) 0.0084(18) O2A 0.032(2) 0.0251(19) 0.028(2) 0.0009(15) 0.0041(17) 0.0011(15) O3A 0.032(2) 0.023(2) 0.043(2) -0.0021(17) -0.0022(19) 0.0026(17) O4A 0.037(2) 0.031(2) 0.034(2) 0.0088(18) 0.0055(18) 0.0031(18) O5A 0.046(3) 0.041(3) 0.033(2) -0.0082(19) -0.004(2) 0.007(2) N1A 0.029(3) 0.032(3) 0.035(3) 0.005(2) -0.001(2) 0.005(2) N2A 0.038(3) 0.027(3) 0.025(2) 0.0021(19) 0.013(2) 0.002(2) N3A 0.029(2) 0.027(3) 0.030(2) 0.0020(18) 0.005(2) -0.0009(18) N4A 0.029(3) 0.029(3) 0.032(3) 0.004(2) 0.002(2) -0.001(2) N11A 0.040(3) 0.035(3) 0.040(3) 0.009(2) 0.002(2) 0.012(2) N21A 0.030(3) 0.029(3) 0.038(3) 0.002(2) 0.012(2) 0.002(2) N31A 0.029(3) 0.030(3) 0.037(3) -0.001(2) 0.002(2) 0.006(2) N41A 0.033(3) 0.031(3) 0.034(3) 0.007(2) 0.003(2) -0.001(2) C1A 0.040(3) 0.028(3) 0.041(3) 0.001(3) 0.010(3) 0.010(3) C2A 0.042(3) 0.025(3) 0.035(3) -0.005(2) 0.012(3) 0.002(2) C3A 0.028(3) 0.035(3) 0.037(3) 0.001(3) 0.005(3) -0.005(2) C4A 0.027(3) 0.036(3) 0.029(3) 0.001(2) 0.000(2) -0.003(2) C5A 0.033(3) 0.043(3) 0.032(3) 0.001(3) 0.006(3) 0.001(3) C6A 0.035(3) 0.041(3) 0.028(3) 0.008(3) 0.004(3) 0.001(3) C7A 0.031(3) 0.037(4) 0.039(3) 0.001(3) 0.004(3) 0.002(2) C8A 0.032(3) 0.035(3) 0.035(3) 0.003(3) 0.013(3) 0.007(3) C10A 0.040(4) 0.036(3) 0.041(4) 0.004(3) 0.005(3) 0.009(3) C11A 0.031(3) 0.034(3) 0.039(3) 0.005(3) 0.001(3) 0.001(3) C12A 0.047(4) 0.037(4) 0.043(3) 0.002(3) -0.010(3) -0.001(3) C13A 0.046(4) 0.070(5) 0.061(5) 0.023(4) -0.013(4) 0.007(4) C14A 0.047(4) 0.045(4) 0.036(3) 0.015(3) 0.003(3) 0.008(3) C15A 0.071(5) 0.038(4) 0.046(4) 0.009(3) 0.002(4) -0.001(4) C16A 0.050(5) 0.075(6) 0.081(6) 0.033(5) -0.012(5) -0.013(4) C17 0.049(5) 0.130(10) 0.066(6) 0.039(6) -0.001(5) -0.014(6) C18A 0.064(6) 0.127(10) 0.059(5) 0.025(6) 0.026(5) 0.035(7) C19A 0.070(5) 0.070(6) 0.046(4) 0.000(4) 0.002(4) 0.019(5) C20A 0.031(3) 0.029(3) 0.040(3) 0.004(2) 0.011(3) -0.001(2) C21A 0.027(3) 0.030(3) 0.028(3) 0.001(2) 0.001(2) 0.004(2) C22A 0.042(4) 0.033(3) 0.034(3) -0.004(3) 0.013(3) 0.003(3) C23A 0.050(4) 0.051(4) 0.053(4) 0.021(3) 0.025(4) 0.012(3) C24A 0.039(3) 0.037(3) 0.032(3) 0.002(2) 0.017(3) 0.004(3) C25A 0.035(3) 0.047(4) 0.061(4) 0.002(4) 0.010(3) -0.001(3) C26A 0.040(4) 0.069(5) 0.057(5) 0.008(4) 0.001(3) 0.007(4) C27A 0.060(5) 0.049(4) 0.057(5) 0.022(4) 0.017(4) 0.022(4) C28A 0.052(4) 0.030(3) 0.056(4) 0.005(3) 0.025(4) 0.010(3) C29A 0.049(4) 0.040(4) 0.035(3) 0.000(3) 0.016(3) 0.000(3) C30A 0.030(3) 0.037(3) 0.026(3) 0.000(2) 0.003(2) 0.005(2) C31A 0.038(3) 0.026(3) 0.030(3) 0.005(2) 0.010(3) 0.003(3) C32A 0.044(4) 0.024(3) 0.045(4) 0.007(3) 0.008(3) 0.004(3) C33A 0.047(4) 0.038(4) 0.046(4) -0.001(3) 0.009(3) 0.007(3) C34A 0.040(4) 0.025(3) 0.060(4) 0.002(3) 0.014(3) 0.005(3) C35A 0.056(4) 0.047(4) 0.056(5) 0.020(3) 0.026(4) 0.016(3) C36A 0.110(8) 0.053(5) 0.083(7) 0.022(5) 0.046(6) 0.007(5) C37A 0.057(6) 0.052(5) 0.172(12) 0.008(6) 0.067(7) 0.001(4) C38A 0.052(5) 0.067(6) 0.120(9) -0.010(6) 0.014(6) -0.007(4) C39A 0.044(4) 0.049(4) 0.090(6) -0.007(4) 0.000(4) -0.014(4) C40A 0.030(3) 0.038(3) 0.034(3) 0.014(3) 0.007(3) 0.008(3) C41A 0.033(3) 0.026(3) 0.031(3) 0.002(2) 0.002(3) 0.001(2) C42A 0.037(3) 0.031(3) 0.036(3) -0.003(3) -0.001(3) 0.001(3) C43A 0.038(4) 0.045(4) 0.057(4) 0.010(3) -0.005(3) -0.007(3) C44A 0.027(3) 0.042(3) 0.036(3) 0.009(3) -0.002(3) 0.007(3) C45A 0.039(3) 0.051(5) 0.031(3) 0.003(3) -0.004(3) 0.007(3) C46A 0.042(4) 0.041(4) 0.061(5) -0.004(3) 0.004(3) 0.011(3) C47A 0.042(4) 0.050(4) 0.049(4) 0.014(3) 0.009(3) 0.014(3) C48A 0.048(4) 0.049(4) 0.036(3) 0.014(3) 0.005(3) 0.005(3) C49 0.028(3) 0.055(5) 0.035(3) 0.004(3) 0.001(2) 0.000(3) Pr1B 0.03793(18) 0.03890(19) 0.02743(16) 0.00098(15) 0.00372(13) 0.00827(15) O1B 0.052(3) 0.060(3) 0.032(2) -0.007(2) 0.002(2) 0.017(3) O2B 0.040(3) 0.053(3) 0.049(3) 0.024(2) 0.008(2) 0.012(2) O3B 0.045(3) 0.035(2) 0.027(2) 0.0013(17) 0.0013(19) 0.0053(19) O4B 0.052(3) 0.034(2) 0.042(3) -0.0011(19) 0.015(2) -0.004(2) O5B 0.050(3) 0.046(3) 0.052(3) 0.004(2) -0.005(2) 0.018(2) N1B 0.053(4) 0.062(4) 0.039(3) -0.016(3) -0.006(3) 0.018(3) N2B 0.053(4) 0.059(4) 0.035(3) 0.006(3) -0.004(3) 0.028(3) N3B 0.036(3) 0.039(3) 0.038(3) 0.003(2) 0.006(2) 0.002(2) N4B 0.042(3) 0.046(3) 0.036(3) -0.014(3) 0.011(2) 0.000(3) N11B 0.066(4) 0.058(4) 0.036(3) -0.009(3) -0.003(3) 0.019(3) N21B 0.059(4) 0.099(6) 0.069(4) 0.050(4) 0.032(3) 0.032(4) N31B 0.053(3) 0.034(3) 0.038(3) 0.002(2) -0.002(3) -0.004(2) N41B 0.048(3) 0.043(3) 0.037(3) -0.006(2) 0.013(3) -0.013(2) C1B 0.063(5) 0.048(4) 0.066(5) -0.019(4) -0.020(4) 0.022(4) C2B 0.071(5) 0.060(5) 0.039(4) -0.003(4) -0.012(4) 0.032(4) C3B 0.056(4) 0.060(5) 0.046(4) 0.007(3) -0.009(3) 0.021(4) C4B 0.048(4) 0.047(4) 0.042(3) 0.005(3) 0.002(3) 0.018(3) C5B 0.042(4) 0.051(4) 0.040(4) -0.010(3) 0.011(3) 0.011(3) C6B 0.043(4) 0.041(4) 0.046(4) -0.017(3) 0.020(3) -0.005(3) C7B 0.043(4) 0.063(5) 0.063(5) -0.018(4) 0.011(4) -0.001(3) C8B 0.044(4) 0.064(5) 0.064(5) -0.029(4) 0.000(4) -0.004(4) C10B 0.070(5) 0.049(4) 0.045(4) -0.017(3) -0.015(4) 0.014(4) C11B 0.063(5) 0.038(4) 0.039(4) -0.002(3) 0.004(4) 0.022(3) C12B 0.065(5) 0.074(5) 0.038(4) -0.008(4) 0.008(4) 0.016(4) C13B 0.095(7) 0.079(7) 0.050(5) -0.003(4) 0.017(5) 0.022(5) C14B 0.095(7) 0.055(5) 0.037(4) 0.002(3) 0.022(4) 0.019(4) C15B 0.073(6) 0.063(5) 0.050(5) 0.008(4) -0.002(4) 0.017(4) C16B 0.095(8) 0.086(7) 0.069(6) 0.017(5) -0.009(6) 0.004(6) C17B 0.141(11) 0.103(9) 0.053(6) 0.020(6) 0.039(7) 0.041(8) C18B 0.076(7) 0.080(7) 0.114(9) -0.005(7) 0.032(7) 0.000(6) C19B 0.062(5) 0.083(7) 0.074(6) -0.014(5) 0.028(5) 0.001(5) C20B 0.061(5) 0.067(5) 0.035(4) 0.016(3) 0.008(3) 0.017(4) C21B 0.054(4) 0.055(4) 0.043(4) 0.018(3) 0.013(3) 0.024(4) C22B 0.042(4) 0.085(6) 0.084(6) 0.040(6) 0.023(4) 0.021(5) C23B 0.064(6) 0.140(10) 0.104(8) 0.016(7) 0.050(6) -0.002(6) C24B 0.028(4) 0.102(7) 0.088(7) 0.046(6) 0.013(4) -0.004(4) C25B 0.050(5) 0.081(7) 0.089(7) 0.027(6) 0.021(5) 0.007(5) C26B 0.052(5) 0.102(8) 0.098(8) 0.031(7) 0.013(6) 0.009(5) C27B 0.060(6) 0.116(10) 0.112(10) -0.004(8) 0.025(6) -0.007(6) C28B 0.059(6) 0.166(13) 0.089(8) 0.049(8) -0.008(6) -0.048(7) C29B 0.032(4) 0.121(9) 0.100(7) 0.012(8) 0.006(4) -0.010(5) C30B 0.051(4) 0.039(4) 0.035(3) 0.002(3) 0.009(3) -0.002(3) C31B 0.032(3) 0.035(3) 0.034(3) -0.003(3) 0.000(3) -0.003(3) C32B 0.045(4) 0.031(3) 0.031(3) 0.003(2) -0.009(3) -0.007(3) C33B 0.071(5) 0.038(4) 0.044(4) 0.004(3) -0.014(4) -0.017(3) C34B 0.052(4) 0.034(3) 0.038(3) 0.003(3) -0.013(3) -0.014(3) C35B 0.071(5) 0.069(6) 0.052(4) 0.013(4) 0.005(4) -0.015(5) C36B 0.071(7) 0.151(12) 0.066(6) 0.020(7) 0.011(5) -0.040(7) C37B 0.097(9) 0.134(12) 0.083(8) 0.076(9) -0.048(7) -0.064(9) C38B 0.133(10) 0.058(6) 0.076(7) 0.032(5) -0.060(7) -0.051(6) C39B 0.083(6) 0.042(4) 0.051(4) 0.001(3) -0.023(4) -0.020(4) C40B 0.052(4) 0.040(4) 0.041(4) -0.011(3) 0.017(3) -0.009(3) C41B 0.035(4) 0.050(4) 0.033(3) -0.011(3) 0.007(3) -0.007(3) C42B 0.039(4) 0.040(4) 0.038(3) -0.002(3) 0.006(3) -0.006(3) C43B 0.058(5) 0.043(4) 0.049(4) 0.004(3) -0.008(4) -0.003(3) C44B 0.046(4) 0.031(3) 0.038(3) 0.002(3) 0.005(3) 0.000(3) C45B 0.042(4) 0.038(4) 0.042(4) 0.003(3) 0.000(3) 0.006(3) C46B 0.046(4) 0.054(4) 0.051(4) -0.002(4) -0.006(3) 0.001(4) C47B 0.067(5) 0.038(4) 0.044(4) -0.007(3) -0.014(4) 0.006(4) C48B 0.069(5) 0.040(4) 0.038(4) -0.005(3) 0.012(4) 0.008(3) C49B 0.046(4) 0.048(4) 0.045(4) -0.003(3) 0.011(3) 0.001(3) S1 0.0454(10) 0.0349(8) 0.0436(9) -0.0058(7) -0.0078(8) -0.0050(7) O11 0.099(4) 0.032(3) 0.062(3) -0.004(2) -0.032(3) -0.008(3) O12 0.063(3) 0.040(3) 0.063(3) 0.000(2) -0.020(3) -0.006(2) O13 0.064(3) 0.033(2) 0.055(3) -0.003(2) -0.003(2) 0.007(2) C1S 0.051(5) 0.106(8) 0.046(5) 0.012(5) 0.005(4) 0.017(5) F11 0.117(5) 0.287(11) 0.054(3) 0.004(5) 0.034(4) 0.064(6) F12 0.043(3) 0.153(5) 0.076(3) 0.029(3) 0.006(2) 0.017(3) F13 0.068(3) 0.159(7) 0.118(5) 0.076(5) -0.014(3) -0.041(4) S2 0.0598(12) 0.0486(12) 0.0585(11) -0.0040(8) 0.0162(9) -0.0122(9) O21 0.107(5) 0.046(3) 0.046(3) 0.000(2) 0.003(3) 0.001(3) O22 0.072(4) 0.064(4) 0.061(3) -0.011(3) 0.020(3) -0.003(3) O23 0.065(4) 0.073(4) 0.120(5) 0.005(4) 0.015(4) -0.020(3) C2S 0.066(5) 0.048(5) 0.041(4) 0.003(3) -0.010(4) -0.007(3) F21 0.079(3) 0.075(3) 0.058(3) -0.003(3) -0.016(2) -0.003(3) F22 0.068(3) 0.081(4) 0.065(3) 0.000(2) 0.016(2) 0.000(2) F23 0.138(5) 0.060(3) 0.057(3) -0.014(2) 0.003(3) 0.014(3) S3 0.0675(12) 0.0516(11) 0.0462(10) 0.0172(8) 0.0202(9) 0.0204(9) O31 0.049(3) 0.056(3) 0.047(3) 0.021(2) 0.016(2) 0.010(2) O32 0.083(4) 0.064(4) 0.058(3) 0.026(3) 0.029(3) 0.032(3) O33 0.089(4) 0.071(4) 0.042(3) 0.003(3) 0.006(3) 0.015(3) C3S 0.075(6) 0.046(5) 0.066(5) 0.015(4) 0.000(4) -0.001(4) F31 0.060(3) 0.062(3) 0.097(3) 0.021(3) -0.001(2) 0.008(3) F32 0.070(3) 0.084(4) 0.100(4) 0.035(3) 0.026(3) 0.005(3) F33 0.091(4) 0.094(4) 0.085(4) -0.027(3) -0.013(3) 0.006(3) S4 0.0482(11) 0.0886(16) 0.0541(12) -0.0064(11) -0.0052(9) -0.0013(11) O41 0.069(3) 0.092(4) 0.044(3) -0.010(3) -0.007(2) 0.014(4) O42 0.052(3) 0.121(6) 0.093(4) 0.033(4) -0.013(3) -0.001(4) O43 0.100(5) 0.067(4) 0.147(7) 0.028(4) -0.029(5) -0.030(4) C4S 0.101(8) 0.079(7) 0.064(6) 0.013(5) -0.008(5) 0.026(6) F41 0.106(5) 0.112(5) 0.120(5) 0.052(4) -0.014(4) -0.020(4) F42 0.074(4) 0.179(7) 0.107(5) 0.047(5) 0.042(3) 0.052(4) F43 0.233(9) 0.127(6) 0.053(3) -0.007(4) 0.013(4) 0.052(6) S5 0.113(3) 0.129(3) 0.105(3) 0.009(2) 0.001(2) 0.044(2) O51 0.139(7) 0.108(6) 0.067(4) 0.024(4) 0.006(4) 0.044(5) O52 0.138(8) 0.296(15) 0.081(5) -0.077(7) -0.048(6) 0.077(9) O53 0.56(3) 0.37(2) 0.188(14) 0.124(15) 0.173(18) 0.36(3) F51 0.205(11) 0.193(11) 0.213(11) 0.057(9) 0.054(9) -0.050(9) F52 0.256(16) 0.45(3) 0.36(2) 0.23(2) 0.139(16) -0.007(17) F53 0.170(12) 0.227(17) 1.34(8) 0.22(3) -0.31(3) -0.108(12) S6 0.0512(11) 0.0606(12) 0.0601(12) 0.0015(10) 0.0214(10) -0.0078(9) O61 0.043(3) 0.050(3) 0.075(4) -0.002(3) 0.005(3) -0.009(2) O62 0.092(5) 0.101(5) 0.095(5) 0.003(4) 0.039(4) 0.014(4) O63 0.153(7) 0.060(5) 0.176(8) 0.024(5) 0.054(6) -0.024(5) C6S 0.056(5) 0.097(8) 0.064(6) -0.014(5) -0.001(5) 0.002(5) F61 0.120(5) 0.079(4) 0.097(4) 0.027(3) 0.002(3) -0.005(4) F62 0.085(4) 0.214(8) 0.061(3) -0.032(4) -0.001(3) 0.064(5) F63 0.065(3) 0.098(4) 0.104(4) -0.017(3) -0.014(3) -0.006(3) O1S 0.213(10) 0.123(7) 0.088(6) -0.026(5) -0.022(6) 0.051(7) _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 Pr1A O1A 2.401(4) . ? Pr1A O3A 2.414(4) . ? Pr1A O4A 2.443(4) . ? Pr1A O5A 2.463(4) . ? Pr1A O2A 2.477(4) . ? Pr1A N4A 2.742(5) . ? Pr1A N3A 2.744(5) . ? Pr1A N2A 2.751(5) . ? Pr1A N1A 2.766(5) . ? O1A C11A 1.251(7) . ? O2A C21A 1.242(7) . ? O3A C31A 1.255(7) . ? O4A C41A 1.282(7) . ? N1A C8A 1.476(7) . ? N1A C1A 1.486(8) . ? N1A C10A 1.498(8) . ? N2A C20A 1.470(7) . ? N2A C3A 1.494(8) . ? N2A C2A 1.518(7) . ? N3A C30A 1.469(7) . ? N3A C5A 1.482(7) . ? N3A C4A 1.490(7) . ? N4A C40A 1.483(8) . ? N4A C6A 1.492(7) . ? N4A C7A 1.505(7) . ? N11A C11A 1.301(7) . ? N11A C12A 1.468(8) . ? N21A C21A 1.326(7) . ? N21A C22A 1.485(7) . ? N31A C31A 1.302(7) . ? N31A C32A 1.469(8) . ? N41A C41A 1.312(7) . ? N41A C42A 1.494(8) . ? C1A C2A 1.516(8) . ? C3A C4A 1.477(8) . ? C5A C6A 1.529(8) . ? C7A C8A 1.537(8) . ? C10A C11A 1.502(9) . ? C12A C14A 1.524(9) . ? C12A C13A 1.529(9) . ? C14A C15A 1.370(10) . ? C14A C19A 1.390(10) . ? C15A C16A 1.385(11) . ? C16A C17 1.365(15) . ? C17 C18A 1.317(15) . ? C18A C19A 1.417(13) . ? C20A C21A 1.515(8) . ? C22A C24A 1.509(9) . ? C22A C23A 1.525(8) . ? C24A C29A 1.403(9) . ? C24A C25A 1.407(9) . ? C25A C26A 1.415(10) . ? C26A C27A 1.383(11) . ? C27A C28A 1.369(11) . ? C28A C29A 1.397(9) . ? C30A C31A 1.510(9) . ? C32A C34A 1.523(9) . ? C32A C33A 1.527(8) . ? C34A C39A 1.386(10) . ? C34A C35A 1.405(10) . ? C35A C36A 1.397(11) . ? C36A C37A 1.385(15) . ? C37A C38A 1.350(15) . ? C38A C39A 1.416(12) . ? C40A C41A 1.509(8) . ? C42A C43A 1.505(9) . ? C42A C44A 1.529(8) . ? C44A C45A 1.377(9) . ? C44A C49 1.383(8) . ? C45A C46A 1.374(9) . ? C46A C47A 1.403(10) . ? C47A C48A 1.381(10) . ? C48A C49 1.406(9) . ? Pr1B O4B 2.389(4) . ? Pr1B O3B 2.405(4) . ? Pr1B O2B 2.407(5) . ? Pr1B O1B 2.413(5) . ? Pr1B O5B 2.480(4) . ? Pr1B N2B 2.720(5) . ? Pr1B N1B 2.722(6) . ? Pr1B N3B 2.729(5) . ? Pr1B N4B 2.754(5) . ? O1B C11B 1.224(9) . ? O2B C21B 1.263(8) . ? O3B C31B 1.266(7) . ? O4B C41B 1.265(7) . ? N1B C10B 1.476(9) . ? N1B C8B 1.493(10) . ? N1B C1B 1.510(10) . ? N2B C3B 1.460(9) . ? N2B C20B 1.485(9) . ? N2B C2B 1.497(10) . ? N3B C30B 1.463(8) . ? N3B C5B 1.508(8) . ? N3B C4B 1.517(8) . ? N4B C40B 1.454(9) . ? N4B C6B 1.500(8) . ? N4B C7B 1.504(9) . ? N11B C11B 1.339(8) . ? N11B C12B 1.489(10) . ? N21B C21B 1.327(10) . ? N21B C22B 1.471(11) . ? N31B C31B 1.295(8) . ? N31B C32B 1.486(8) . ? N41B C41B 1.332(8) . ? N41B C42B 1.460(8) . ? C1B C2B 1.460(12) . ? C3B C4B 1.523(9) . ? C5B C6B 1.504(10) . ? C7B C8B 1.512(10) . ? C10B C11B 1.517(11) . ? C12B C14B 1.478(12) . ? C12B C13B 1.527(11) . ? C14B C19B 1.378(12) . ? C14B C15B 1.454(12) . ? C15B C16B 1.329(13) . ? C16B C17B 1.375(16) . ? C17B C18B 1.430(16) . ? C18B C19B 1.319(14) . ? C20B C21B 1.528(11) . ? C22B C24B 1.478(14) . ? C22B C23B 1.582(12) . ? C24B C29B 1.384(13) . ? C24B C25B 1.395(13) . ? C25B C26B 1.354(14) . ? C26B C27B 1.322(15) . ? C27B C28B 1.415(17) . ? C28B C29B 1.393(16) . ? C30B C31B 1.510(8) . ? C32B C34B 1.517(9) . ? C32B C33B 1.532(8) . ? C34B C39B 1.366(10) . ? C34B C35B 1.385(10) . ? C35B C36B 1.376(13) . ? C36B C37B 1.463(19) . ? C37B C38B 1.228(17) . ? C38B C39B 1.406(12) . ? C40B C41B 1.505(9) . ? C42B C43B 1.510(9) . ? C42B C44B 1.524(9) . ? C44B C49B 1.396(9) . ? C44B C45B 1.401(9) . ? C45B C46B 1.368(9) . ? C46B C47B 1.393(10) . ? C47B C48B 1.360(10) . ? C48B C49B 1.375(10) . ? S1 O13 1.422(5) . ? S1 O11 1.431(5) . ? S1 O12 1.437(5) . ? S1 C1S 1.851(9) . ? C1S F11 1.298(11) . ? C1S F13 1.325(12) . ? C1S F12 1.341(9) . ? S2 O23 1.419(6) . ? S2 O21 1.432(6) . ? S2 O22 1.484(6) . ? S2 C2S 1.769(8) . ? C2S F21 1.305(8) . ? C2S F22 1.362(9) . ? C2S F23 1.375(9) . ? S3 O33 1.404(5) . ? S3 O32 1.415(6) . ? S3 O31 1.422(5) . ? S3 C3S 1.850(9) . ? C3S F33 1.320(10) . ? C3S F31 1.328(9) . ? C3S F32 1.329(9) . ? S4 O42 1.392(6) . ? S4 O41 1.405(6) . ? S4 O43 1.481(7) . ? S4 C4S 1.745(11) . ? C4S F42 1.331(11) . ? C4S F43 1.333(12) . ? C4S F41 1.372(11) . ? S5 O52 1.428(9) . ? S5 O53 1.428(14) . ? S5 O51 1.442(8) . ? S5 C5S 1.53(2) . ? S5 C5S' 1.71(3) . ? O51 C5S 1.58(2) . ? C5S C5S' 1.14(3) . ? C5S F53 1.39(3) . ? C5S F51 1.55(2) . ? C5S' F53 1.25(3) . ? C5S' F52 1.27(3) . ? C5S' F51 1.31(2) . ? S6 O61 1.407(5) . ? S6 O63 1.407(8) . ? S6 O62 1.417(6) . ? S6 C6S 1.806(10) . ? C6S F63 1.296(10) . ? C6S F62 1.311(10) . ? C6S F61 1.392(12) . ? O1S C7S 1.405(19) . ? C7S C8S 1.50(3) . ? O2S C9S 1.83(3) . ? C9S C10S 1.69(5) . ? O3S C11S 1.24(3) . ? C11S C12S 1.61(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 O1A Pr1A O3A 147.58(14) . . ? O1A Pr1A O4A 85.80(14) . . ? O3A Pr1A O4A 85.36(13) . . ? O1A Pr1A O5A 72.83(14) . . ? O3A Pr1A O5A 74.75(14) . . ? O4A Pr1A O5A 73.27(14) . . ? O1A Pr1A O2A 86.84(13) . . ? O3A Pr1A O2A 85.23(13) . . ? O4A Pr1A O2A 149.62(13) . . ? O5A Pr1A O2A 76.39(14) . . ? O1A Pr1A N4A 128.47(14) . . ? O3A Pr1A N4A 74.07(14) . . ? O4A Pr1A N4A 64.31(14) . . ? O5A Pr1A N4A 128.51(15) . . ? O2A Pr1A N4A 139.08(13) . . ? O1A Pr1A N3A 140.95(13) . . ? O3A Pr1A N3A 65.00(13) . . ? O4A Pr1A N3A 127.67(13) . . ? O5A Pr1A N3A 130.53(14) . . ? O2A Pr1A N3A 72.88(13) . . ? N4A Pr1A N3A 66.44(14) . . ? O1A Pr1A N2A 74.79(14) . . ? O3A Pr1A N2A 128.25(14) . . ? O4A Pr1A N2A 140.49(14) . . ? O5A Pr1A N2A 129.70(14) . . ? O2A Pr1A N2A 64.33(13) . . ? N4A Pr1A N2A 101.77(14) . . ? N3A Pr1A N2A 66.42(14) . . ? O1A Pr1A N1A 64.37(13) . . ? O3A Pr1A N1A 141.28(14) . . ? O4A Pr1A N1A 74.36(14) . . ? O5A Pr1A N1A 127.33(14) . . ? O2A Pr1A N1A 127.66(13) . . ? N4A Pr1A N1A 67.48(14) . . ? N3A Pr1A N1A 102.14(14) . . ? N2A Pr1A N1A 66.26(14) . . ? C11A O1A Pr1A 127.4(4) . . ? C21A O2A Pr1A 122.7(3) . . ? C31A O3A Pr1A 124.9(4) . . ? C41A O4A Pr1A 125.4(4) . . ? C8A N1A C1A 109.8(5) . . ? C8A N1A C10A 110.4(5) . . ? C1A N1A C10A 109.7(5) . . ? C8A N1A Pr1A 109.4(3) . . ? C1A N1A Pr1A 111.4(3) . . ? C10A N1A Pr1A 106.1(3) . . ? C20A N2A C3A 110.3(5) . . ? C20A N2A C2A 107.8(4) . . ? C3A N2A C2A 109.7(4) . . ? C20A N2A Pr1A 106.6(3) . . ? C3A N2A Pr1A 111.2(3) . . ? C2A N2A Pr1A 111.2(3) . . ? C30A N3A C5A 109.7(4) . . ? C30A N3A C4A 110.9(4) . . ? C5A N3A C4A 108.0(4) . . ? C30A N3A Pr1A 106.3(3) . . ? C5A N3A Pr1A 111.7(3) . . ? C4A N3A Pr1A 110.3(3) . . ? C40A N4A C6A 108.6(4) . . ? C40A N4A C7A 110.2(4) . . ? C6A N4A C7A 109.5(4) . . ? C40A N4A Pr1A 107.0(3) . . ? C6A N4A Pr1A 111.3(3) . . ? C7A N4A Pr1A 110.1(3) . . ? C11A N11A C12A 122.0(5) . . ? C21A N21A C22A 121.3(5) . . ? C31A N31A C32A 121.4(5) . . ? C41A N41A C42A 122.8(5) . . ? N1A C1A C2A 114.1(5) . . ? C1A C2A N2A 111.4(4) . . ? C4A C3A N2A 114.2(5) . . ? C3A C4A N3A 114.0(5) . . ? N3A C5A C6A 113.7(5) . . ? N4A C6A C5A 111.9(5) . . ? N4A C7A C8A 114.3(5) . . ? N1A C8A C7A 112.4(5) . . ? N1A C10A C11A 112.1(5) . . ? O1A C11A N11A 121.9(6) . . ? O1A C11A C10A 118.9(5) . . ? N11A C11A C10A 119.2(5) . . ? N11A C12A C14A 111.3(5) . . ? N11A C12A C13A 109.7(6) . . ? C14A C12A C13A 112.3(6) . . ? C15A C14A C19A 118.9(7) . . ? C15A C14A C12A 122.3(6) . . ? C19A C14A C12A 118.8(7) . . ? C14A C15A C16A 120.7(8) . . ? C17 C16A C15A 119.8(9) . . ? C18A C17 C16A 121.0(9) . . ? C17 C18A C19A 120.9(10) . . ? C14A C19A C18A 118.7(9) . . ? N2A C20A C21A 110.2(4) . . ? O2A C21A N21A 121.9(5) . . ? O2A C21A C20A 121.5(5) . . ? N21A C21A C20A 116.5(5) . . ? N21A C22A C24A 110.5(5) . . ? N21A C22A C23A 107.6(5) . . ? C24A C22A C23A 112.7(5) . . ? C29A C24A C25A 117.6(6) . . ? C29A C24A C22A 120.2(6) . . ? C25A C24A C22A 122.2(6) . . ? C24A C25A C26A 120.9(7) . . ? C27A C26A C25A 119.5(7) . . ? C28A C27A C26A 120.4(6) . . ? C27A C28A C29A 120.8(7) . . ? C28A C29A C24A 120.9(7) . . ? N3A C30A C31A 112.3(5) . . ? O3A C31A N31A 121.3(6) . . ? O3A C31A C30A 119.8(5) . . ? N31A C31A C30A 118.8(5) . . ? N31A C32A C34A 111.7(5) . . ? N31A C32A C33A 108.8(5) . . ? C34A C32A C33A 111.7(5) . . ? C39A C34A C35A 121.3(7) . . ? C39A C34A C32A 118.1(7) . . ? C35A C34A C32A 120.7(6) . . ? C36A C35A C34A 117.5(8) . . ? C37A C36A C35A 120.4(10) . . ? C38A C37A C36A 122.6(9) . . ? C37A C38A C39A 118.3(9) . . ? C34A C39A C38A 119.9(9) . . ? N4A C40A C41A 111.4(5) . . ? O4A C41A N41A 123.1(5) . . ? O4A C41A C40A 118.0(5) . . ? N41A C41A C40A 118.8(5) . . ? N41A C42A C43A 107.7(5) . . ? N41A C42A C44A 111.6(5) . . ? C43A C42A C44A 112.4(5) . . ? C45A C44A C49 119.5(6) . . ? C45A C44A C42A 121.6(5) . . ? C49 C44A C42A 118.9(6) . . ? C46A C45A C44A 121.7(6) . . ? C45A C46A C47A 119.4(7) . . ? C48A C47A C46A 119.4(6) . . ? C47A C48A C49 120.2(6) . . ? C44A C49 C48A 119.7(6) . . ? O4B Pr1B O3B 86.61(15) . . ? O4B Pr1B O2B 149.11(15) . . ? O3B Pr1B O2B 84.08(16) . . ? O4B Pr1B O1B 85.44(16) . . ? O3B Pr1B O1B 147.96(15) . . ? O2B Pr1B O1B 87.01(18) . . ? O4B Pr1B O5B 75.19(16) . . ? O3B Pr1B O5B 73.29(15) . . ? O2B Pr1B O5B 73.92(16) . . ? O1B Pr1B O5B 74.67(16) . . ? O4B Pr1B N2B 139.71(18) . . ? O3B Pr1B N2B 128.41(17) . . ? O2B Pr1B N2B 64.98(18) . . ? O1B Pr1B N2B 73.59(17) . . ? O5B Pr1B N2B 128.51(17) . . ? O4B Pr1B N1B 73.22(18) . . ? O3B Pr1B N1B 140.76(16) . . ? O2B Pr1B N1B 129.25(18) . . ? O1B Pr1B N1B 64.91(17) . . ? O5B Pr1B N1B 129.81(17) . . ? N2B Pr1B N1B 66.8(2) . . ? O4B Pr1B N3B 128.26(14) . . ? O3B Pr1B N3B 64.52(15) . . ? O2B Pr1B N3B 72.87(16) . . ? O1B Pr1B N3B 140.62(16) . . ? O5B Pr1B N3B 128.00(16) . . ? N2B Pr1B N3B 67.28(17) . . ? N1B Pr1B N3B 102.19(17) . . ? O4B Pr1B N4B 63.97(17) . . ? O3B Pr1B N4B 74.50(15) . . ? O2B Pr1B N4B 139.74(17) . . ? O1B Pr1B N4B 128.08(17) . . ? O5B Pr1B N4B 128.65(16) . . ? N2B Pr1B N4B 102.84(17) . . ? N1B Pr1B N4B 66.46(16) . . ? N3B Pr1B N4B 67.22(16) . . ? C11B O1B Pr1B 124.3(4) . . ? C21B O2B Pr1B 124.4(5) . . ? C31B O3B Pr1B 125.9(4) . . ? C41B O4B Pr1B 126.8(4) . . ? C10B N1B C8B 108.7(6) . . ? C10B N1B C1B 110.4(5) . . ? C8B N1B C1B 108.9(6) . . ? C10B N1B Pr1B 105.9(4) . . ? C8B N1B Pr1B 112.0(4) . . ? C1B N1B Pr1B 110.8(5) . . ? C3B N2B C20B 111.2(6) . . ? C3B N2B C2B 110.4(5) . . ? C20B N2B C2B 107.8(6) . . ? C3B N2B Pr1B 111.8(4) . . ? C20B N2B Pr1B 105.6(4) . . ? C2B N2B Pr1B 109.9(4) . . ? C30B N3B C5B 111.2(5) . . ? C30B N3B C4B 108.6(5) . . ? C5B N3B C4B 109.1(5) . . ? C30B N3B Pr1B 107.4(4) . . ? C5B N3B Pr1B 110.4(4) . . ? C4B N3B Pr1B 110.2(4) . . ? C40B N4B C6B 110.4(5) . . ? C40B N4B C7B 111.3(6) . . ? C6B N4B C7B 108.8(5) . . ? C40B N4B Pr1B 106.5(4) . . ? C6B N4B Pr1B 108.7(4) . . ? C7B N4B Pr1B 111.2(4) . . ? C11B N11B C12B 122.0(7) . . ? C21B N21B C22B 120.1(6) . . ? C31B N31B C32B 120.9(5) . . ? C41B N41B C42B 121.6(5) . . ? C2B C1B N1B 113.6(6) . . ? C1B C2B N2B 113.0(6) . . ? N2B C3B C4B 115.5(5) . . ? N3B C4B C3B 111.8(6) . . ? C6B C5B N3B 112.3(5) . . ? N4B C6B C5B 112.4(5) . . ? N4B C7B C8B 112.9(6) . . ? N1B C8B C7B 112.8(6) . . ? N1B C10B C11B 111.0(6) . . ? O1B C11B N11B 120.7(7) . . ? O1B C11B C10B 120.9(6) . . ? N11B C11B C10B 118.4(7) . . ? C14B C12B N11B 113.4(7) . . ? C14B C12B C13B 113.6(6) . . ? N11B C12B C13B 108.2(7) . . ? C19B C14B C15B 119.6(8) . . ? C19B C14B C12B 123.9(8) . . ? C15B C14B C12B 116.4(8) . . ? C16B C15B C14B 119.5(10) . . ? C15B C16B C17B 118.3(10) . . ? C16B C17B C18B 123.6(11) . . ? C19B C18B C17B 117.0(11) . . ? C18B C19B C14B 121.9(10) . . ? N2B C20B C21B 110.8(5) . . ? O2B C21B N21B 121.9(7) . . ? O2B C21B C20B 119.2(7) . . ? N21B C21B C20B 118.8(6) . . ? N21B C22B C24B 111.0(6) . . ? N21B C22B C23B 106.1(7) . . ? C24B C22B C23B 109.3(9) . . ? C29B C24B C25B 117.7(11) . . ? C29B C24B C22B 119.1(9) . . ? C25B C24B C22B 123.2(9) . . ? C26B C25B C24B 121.9(10) . . ? C27B C26B C25B 119.4(11) . . ? C26B C27B C28B 123.3(12) . . ? C29B C28B C27B 115.9(11) . . ? C24B C29B C28B 121.7(12) . . ? N3B C30B C31B 112.4(5) . . ? O3B C31B N31B 122.6(6) . . ? O3B C31B C30B 118.8(5) . . ? N31B C31B C30B 118.6(6) . . ? N31B C32B C34B 111.9(5) . . ? N31B C32B C33B 108.4(5) . . ? C34B C32B C33B 114.0(5) . . ? C39B C34B C35B 118.7(7) . . ? C39B C34B C32B 120.9(7) . . ? C35B C34B C32B 120.4(7) . . ? C36B C35B C34B 118.8(10) . . ? C35B C36B C37B 118.0(10) . . ? C38B C37B C36B 123.3(10) . . ? C37B C38B C39B 118.4(12) . . ? C34B C39B C38B 122.7(10) . . ? N4B C40B C41B 112.0(5) . . ? O4B C41B N41B 119.7(6) . . ? O4B C41B C40B 118.2(6) . . ? N41B C41B C40B 121.8(6) . . ? N41B C42B C43B 109.0(5) . . ? N41B C42B C44B 111.7(5) . . ? C43B C42B C44B 112.8(5) . . ? C49B C44B C45B 118.0(6) . . ? C49B C44B C42B 120.7(6) . . ? C45B C44B C42B 121.3(6) . . ? C46B C45B C44B 120.8(7) . . ? C45B C46B C47B 120.1(7) . . ? C48B C47B C46B 119.7(6) . . ? C47B C48B C49B 121.0(7) . . ? C48B C49B C44B 120.5(7) . . ? O13 S1 O11 115.2(3) . . ? O13 S1 O12 114.7(3) . . ? O11 S1 O12 115.4(3) . . ? O13 S1 C1S 101.4(4) . . ? O11 S1 C1S 105.7(4) . . ? O12 S1 C1S 101.9(4) . . ? F11 C1S F13 111.5(9) . . ? F11 C1S F12 107.0(8) . . ? F13 C1S F12 110.3(8) . . ? F11 C1S S1 110.1(7) . . ? F13 C1S S1 108.9(6) . . ? F12 C1S S1 109.1(6) . . ? O23 S2 O21 114.3(4) . . ? O23 S2 O22 116.4(4) . . ? O21 S2 O22 113.4(3) . . ? O23 S2 C2S 102.1(4) . . ? O21 S2 C2S 104.8(4) . . ? O22 S2 C2S 103.7(3) . . ? F21 C2S F22 108.3(6) . . ? F21 C2S F23 107.0(6) . . ? F22 C2S F23 102.7(6) . . ? F21 C2S S2 113.4(6) . . ? F22 C2S S2 113.7(5) . . ? F23 C2S S2 111.1(5) . . ? O33 S3 O32 113.0(3) . . ? O33 S3 O31 119.1(4) . . ? O32 S3 O31 114.7(3) . . ? O33 S3 C3S 100.1(4) . . ? O32 S3 C3S 105.0(4) . . ? O31 S3 C3S 101.7(3) . . ? F33 C3S F31 106.7(7) . . ? F33 C3S F32 106.8(7) . . ? F31 C3S F32 107.0(7) . . ? F33 C3S S3 112.3(6) . . ? F31 C3S S3 111.9(6) . . ? F32 C3S S3 111.8(6) . . ? O42 S4 O41 118.7(4) . . ? O42 S4 O43 111.9(4) . . ? O41 S4 O43 112.8(4) . . ? O42 S4 C4S 104.3(4) . . ? O41 S4 C4S 105.1(5) . . ? O43 S4 C4S 101.7(5) . . ? F42 C4S F43 106.0(9) . . ? F42 C4S F41 105.8(10) . . ? F43 C4S F41 109.0(8) . . ? F42 C4S S4 112.0(7) . . ? F43 C4S S4 112.9(9) . . ? F41 C4S S4 110.8(7) . . ? O52 S5 O53 130.6(10) . . ? O52 S5 O51 117.2(6) . . ? O53 S5 O51 106.8(7) . . ? O52 S5 C5S 118.2(10) . . ? O53 S5 C5S 100.1(14) . . ? O51 S5 C5S 64.0(9) . . ? O52 S5 C5S' 95.3(10) . . ? O53 S5 C5S' 94.4(13) . . ? O51 S5 C5S' 104.5(10) . . ? C5S S5 C5S' 40.9(10) . . ? S5 O51 C5S 60.6(8) . . ? C5S' C5S F53 58(2) . . ? C5S' C5S S5 78.1(18) . . ? F53 C5S S5 118(2) . . ? C5S' C5S F51 55.9(15) . . ? F53 C5S F51 85.9(15) . . ? S5 C5S F51 105.1(13) . . ? C5S' C5S O51 133(2) . . ? F53 C5S O51 149.4(18) . . ? S5 C5S O51 55.4(8) . . ? F51 C5S O51 124.5(14) . . ? C5S C5S' F53 71(2) . . ? C5S C5S' F52 173(3) . . ? F53 C5S' F52 105(3) . . ? C5S C5S' F51 78(2) . . ? F53 C5S' F51 103(2) . . ? F52 C5S' F51 109(2) . . ? C5S C5S' S5 61.0(16) . . ? F53 C5S' S5 114(2) . . ? F52 C5S' S5 117(2) . . ? F51 C5S' S5 107.2(17) . . ? C5S' F51 C5S 46.1(13) . . ? C5S' F53 C5S 50.9(14) . . ? O61 S6 O63 115.3(5) . . ? O61 S6 O62 117.1(4) . . ? O63 S6 O62 111.8(5) . . ? O61 S6 C6S 103.4(4) . . ? O63 S6 C6S 102.7(5) . . ? O62 S6 C6S 104.3(4) . . ? F63 C6S F62 109.0(8) . . ? F63 C6S F61 105.6(8) . . ? F62 C6S F61 104.4(8) . . ? F63 C6S S6 115.9(7) . . ? F62 C6S S6 112.1(7) . . ? F61 C6S S6 109.0(6) . . ? O1S C7S C8S 101.2(16) . . ? C10S C9S O2S 104(2) . . ? O3S C11S C12S 106(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11A H11A O23 0.88 1.99 2.866(8) 170.6 2_646 N21A H21A O61 0.88 2.08 2.936(7) 163.0 1_545 N31A H31A O12 0.88 2.02 2.822(7) 150.4 4 N41A H41A O31 0.88 2.02 2.880(6) 167.0 3_554 O5A H01A O41 0.85 2.03 2.878(7) 179.5 . O5A H02A O1S 0.85 1.89 2.737(10) 178.9 . N11B H11B O21 0.88 2.12 2.986(9) 166.4 . N21B H21B O32 0.88 2.00 2.871(8) 172.6 . N31B H31B O13 0.88 1.97 2.845(7) 170.2 . N41B H41B O62 0.88 2.08 2.878(9) 150.9 . O5B H01B O52 0.85 1.99 2.840(9) 179.4 . O5B H02B O2S 0.85 1.81 2.656(15) 179.1 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.359 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.112 #==============================================END data_9c _database_code_CSD 182453 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Gd N8 O5 3+,3(C F3 O3 S 1-),C2 H6 O,H2 O' _chemical_formula_sum 'C53 H74 F9 Gd N8 O16 S3' _chemical_formula_weight 1503.63 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' 'F' 'F' 0.0171 0.0103 '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 I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 32.018(11) _cell_length_b 12.654(5) _cell_length_c 32.715(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.63(2) _cell_angle_gamma 90.00 _cell_volume 13228(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6830 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 23.12 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6152 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8093 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details 'SADABS V2.03 (Bruker,2001), R(int)=0.108 before correction' _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f and/or 2\q angles and each scan (30 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'SMART 6000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 80020 _diffrn_reflns_av_R_equivalents 0.0951 _diffrn_reflns_av_sigmaI/netI 0.1459 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 30361 _reflns_number_gt 21541 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. The triflate ligand containing S(5) is chaotically disordered. O(2S) probably belongs to a disordered ethanol molecule, no stable refinement of the carbon atoms was possible. ; _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^)+(0.0908P)^2^+7.5371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(11) _refine_ls_number_reflns 30361 _refine_ls_number_parameters 1579 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.2105 _refine_ls_wR_factor_gt 0.1908 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.013 _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 Gd1A Gd 0.504226(13) 0.37312(3) 0.301258(13) 0.02237(11) Uani 1 1 d . . . O1A O 0.5414(2) 0.2499(5) 0.3430(2) 0.0287(15) Uani 1 1 d . . . O2A O 0.44741(19) 0.3423(5) 0.3441(2) 0.0243(15) Uani 1 1 d . . . O3A O 0.4787(2) 0.5470(5) 0.2982(2) 0.0289(15) Uani 1 1 d . . . O4A O 0.5711(2) 0.4530(5) 0.2946(2) 0.0271(15) Uani 1 1 d . . . O5A O 0.5245(2) 0.4553(5) 0.3659(2) 0.0289(15) Uani 1 1 d . . . H01A H 0.5447 0.4344 0.3811 0.043 Uiso 1 1 d R . . H02A H 0.5241 0.5200 0.3706 0.043 Uiso 1 1 d R . . N1A N 0.5491(3) 0.2333(6) 0.2600(2) 0.0276(18) Uani 1 1 d . . . N2A N 0.4645(3) 0.1882(6) 0.2873(2) 0.0251(18) Uani 1 1 d . . . N3A N 0.4330(2) 0.3939(6) 0.2543(2) 0.0258(18) Uani 1 1 d . . . N4A N 0.5173(3) 0.4431(6) 0.2255(3) 0.0263(18) Uani 1 1 d . . . N11A N 0.5869(3) 0.1176(8) 0.3569(2) 0.0352(19) Uani 1 1 d . . . H11A H 0.6034 0.0696 0.3473 0.042 Uiso 1 1 d R . . N21A N 0.3972(2) 0.2382(7) 0.3690(2) 0.0267(18) Uani 1 1 d . . . H21A H 0.3842 0.1775 0.3668 0.032 Uiso 1 1 d R . . N31A N 0.4314(2) 0.6708(6) 0.2825(3) 0.0261(18) Uani 1 1 d . . . H31A H 0.4069 0.6856 0.2705 0.031 Uiso 1 1 d R . . N41A N 0.6186(3) 0.5458(6) 0.2605(2) 0.0288(18) Uani 1 1 d . . . H41A H 0.6245 0.5719 0.2369 0.035 Uiso 1 1 d R . . C1A C 0.5240(3) 0.1441(7) 0.2451(3) 0.030(2) Uani 1 1 d . . . H11 H 0.5419 0.0854 0.2371 0.036 Uiso 1 1 d R . . H12 H 0.5077 0.1683 0.2204 0.036 Uiso 1 1 d R . . C2A C 0.4935(3) 0.1033(7) 0.2753(3) 0.027(2) Uani 1 1 d . . . H21 H 0.5095 0.0776 0.2999 0.032 Uiso 1 1 d R . . H22 H 0.4772 0.0439 0.2634 0.032 Uiso 1 1 d R . . C3A C 0.4307(3) 0.1976(8) 0.2553(3) 0.032(2) Uani 1 1 d . . . H31 H 0.4428 0.1921 0.2286 0.039 Uiso 1 1 d R . . H32 H 0.4106 0.1392 0.2574 0.039 Uiso 1 1 d R . . C4A C 0.4063(3) 0.3011(8) 0.2569(3) 0.029(2) Uani 1 1 d . . . H41 H 0.3921 0.3036 0.2827 0.034 Uiso 1 1 d R . . H42 H 0.3846 0.3032 0.2344 0.034 Uiso 1 1 d R . . C5A C 0.4416(3) 0.4098(9) 0.2103(3) 0.031(2) Uani 1 1 d . . . H51 H 0.4170 0.4408 0.1954 0.038 Uiso 1 1 d R . . H52 H 0.4468 0.3403 0.1982 0.038 Uiso 1 1 d R . . C6A C 0.4790(3) 0.4835(8) 0.2047(3) 0.031(2) Uani 1 1 d . . . H61 H 0.4833 0.4904 0.1754 0.037 Uiso 1 1 d R . . H62 H 0.4730 0.5542 0.2151 0.037 Uiso 1 1 d R . . C7A C 0.5350(3) 0.3546(9) 0.2011(3) 0.032(2) Uani 1 1 d . . . H71 H 0.5479 0.3834 0.1770 0.038 Uiso 1 1 d R . . H72 H 0.5113 0.3098 0.1913 0.038 Uiso 1 1 d R . . C8A C 0.5672(3) 0.2877(8) 0.2239(3) 0.025(2) Uani 1 1 d . . . H81 H 0.5783 0.2346 0.2055 0.030 Uiso 1 1 d R . . H82 H 0.5907 0.3322 0.2342 0.030 Uiso 1 1 d R . . C10A C 0.5837(4) 0.1980(9) 0.2898(3) 0.037(3) Uani 1 1 d . . . H101 H 0.6076 0.2467 0.2899 0.045 Uiso 1 1 d R . . H102 H 0.5931 0.1288 0.2804 0.045 Uiso 1 1 d R . . C11A C 0.5684(3) 0.1893(8) 0.3322(3) 0.028(2) Uani 1 1 d . . . C12A C 0.5792(3) 0.1194(10) 0.4015(3) 0.035(2) Uani 1 1 d . . . H12A H 0.5826 0.1935 0.4118 0.042 Uiso 1 1 calc R . . C13A C 0.6138(4) 0.0496(13) 0.4234(4) 0.064(4) Uani 1 1 d . . . H131 H 0.6414 0.0762 0.4170 0.096 Uiso 1 1 calc R . . H132 H 0.6107 -0.0235 0.4138 0.096 Uiso 1 1 calc R . . H133 H 0.6112 0.0521 0.4530 0.096 Uiso 1 1 calc R . . C14A C 0.5356(3) 0.0817(9) 0.4092(3) 0.037(3) Uani 1 1 d . . . C15A C 0.5210(5) -0.0151(10) 0.3953(4) 0.052(3) Uani 1 1 d . . . H15A H 0.5375 -0.0607 0.3802 0.062 Uiso 1 1 d R . . C16A C 0.4806(5) -0.0462(12) 0.4047(5) 0.067(5) Uani 1 1 d . . . H16A H 0.4688 -0.1101 0.3947 0.080 Uiso 1 1 d R . . C17A C 0.4554(5) 0.0201(16) 0.4272(5) 0.068(4) Uani 1 1 d . . . H17A H 0.4282 0.0005 0.4340 0.081 Uiso 1 1 d R . . C18A C 0.4698(5) 0.1159(18) 0.4397(4) 0.074(5) Uani 1 1 d . . . H18A H 0.4530 0.1631 0.4538 0.088 Uiso 1 1 d R . . C19A C 0.5101(4) 0.1468(11) 0.4317(4) 0.048(3) Uani 1 1 d . . . H19A H 0.5218 0.2101 0.4424 0.057 Uiso 1 1 d R . . C20A C 0.4469(3) 0.1579(7) 0.3272(3) 0.024(2) Uani 1 1 d . . . H201 H 0.4682 0.1234 0.3454 0.029 Uiso 1 1 d R . . H202 H 0.4242 0.1069 0.3209 0.029 Uiso 1 1 d R . . C21A C 0.4300(3) 0.2529(8) 0.3468(3) 0.025(2) Uani 1 1 d . . . C22A C 0.3819(3) 0.3223(8) 0.3958(3) 0.028(2) Uani 1 1 d . . . H22A H 0.4057 0.3518 0.4131 0.033 Uiso 1 1 d R . . C23A C 0.3512(4) 0.2682(9) 0.4246(4) 0.042(3) Uani 1 1 d . . . H231 H 0.3657 0.2110 0.4399 0.063 Uiso 1 1 calc R . . H232 H 0.3272 0.2391 0.4081 0.063 Uiso 1 1 calc R . . H233 H 0.3412 0.3205 0.4438 0.063 Uiso 1 1 calc R . . C24A C 0.3605(3) 0.4100(8) 0.3708(3) 0.028(2) Uani 1 1 d . . . C25A C 0.3273(3) 0.3889(10) 0.3415(4) 0.040(3) Uani 1 1 d . . . H25A H 0.3176 0.3197 0.3361 0.048 Uiso 1 1 d R . . C26A C 0.3086(4) 0.4703(12) 0.3188(4) 0.054(3) Uani 1 1 d . . . H26A H 0.2866 0.4575 0.2989 0.065 Uiso 1 1 d R . . C27A C 0.3219(4) 0.5743(11) 0.3264(4) 0.052(3) Uani 1 1 d . . . H27A H 0.3095 0.6303 0.3110 0.062 Uiso 1 1 d R . . C28A C 0.3530(4) 0.5963(9) 0.3554(4) 0.046(3) Uani 1 1 d . . . H28A H 0.3613 0.6666 0.3609 0.055 Uiso 1 1 d R . . C29A C 0.3736(4) 0.5134(9) 0.3766(3) 0.034(2) Uani 1 1 d . . . H29A H 0.3962 0.5272 0.3958 0.041 Uiso 1 1 d R . . C30A C 0.4118(3) 0.4870(8) 0.2698(3) 0.030(2) Uani 1 1 d . . . H301 H 0.3947 0.4663 0.2924 0.036 Uiso 1 1 d R . . H302 H 0.3929 0.5149 0.2476 0.036 Uiso 1 1 d R . . C31A C 0.4430(3) 0.5741(8) 0.2837(3) 0.026(2) Uani 1 1 d . . . C32A C 0.4581(3) 0.7566(8) 0.2976(3) 0.034(2) Uani 1 1 d . . . H32A H 0.4710 0.7336 0.3244 0.041 Uiso 1 1 d R . . C33A C 0.4314(4) 0.8530(8) 0.3065(3) 0.038(3) Uani 1 1 d . . . H331 H 0.4101 0.8344 0.3252 0.056 Uiso 1 1 d R . . H332 H 0.4180 0.8768 0.2807 0.056 Uiso 1 1 d R . . H333 H 0.4490 0.9093 0.3183 0.056 Uiso 1 1 d R . . C34A C 0.4919(3) 0.7854(8) 0.2686(4) 0.038(3) Uani 1 1 d . . . C35A C 0.4823(4) 0.7970(9) 0.2278(4) 0.043(3) Uani 1 1 d . . . H35A H 0.4551 0.7869 0.2157 0.051 Uiso 1 1 d R . . C36A C 0.5151(6) 0.8194(12) 0.2031(5) 0.073(5) Uani 1 1 d . . . H36A H 0.5112 0.8258 0.1745 0.088 Uiso 1 1 d R . . C37A C 0.5538(5) 0.8387(11) 0.2187(7) 0.080(6) Uani 1 1 d . . . H37A H 0.5760 0.8569 0.2024 0.097 Uiso 1 1 d R . . C38A C 0.5638(5) 0.8293(12) 0.2599(6) 0.068(4) Uani 1 1 d . . . H38A H 0.5912 0.8404 0.2717 0.082 Uiso 1 1 d R . . C39A C 0.5335(4) 0.7984(9) 0.2844(5) 0.048(3) Uani 1 1 d . . . H39A H 0.5389 0.7899 0.3128 0.058 Uiso 1 1 d R . . C40A C 0.5481(3) 0.5297(9) 0.2299(3) 0.035(2) Uani 1 1 d . . . H401 H 0.5339 0.5966 0.2355 0.042 Uiso 1 1 d R . . H402 H 0.5617 0.5376 0.2040 0.042 Uiso 1 1 d R . . C41A C 0.5814(3) 0.5076(8) 0.2642(3) 0.029(2) Uani 1 1 d . . . C42A C 0.6520(3) 0.5415(8) 0.2945(3) 0.033(2) Uani 1 1 d . . . H42A H 0.6416 0.5786 0.3188 0.040 Uiso 1 1 calc R . . C43A C 0.6892(4) 0.6044(9) 0.2795(4) 0.050(3) Uani 1 1 d . . . H431 H 0.6800 0.6760 0.2719 0.075 Uiso 1 1 calc R . . H432 H 0.6999 0.5690 0.2557 0.075 Uiso 1 1 calc R . . H433 H 0.7114 0.6083 0.3015 0.075 Uiso 1 1 calc R . . C44A C 0.6641(3) 0.4301(9) 0.3069(3) 0.031(2) Uani 1 1 d . . . C45A C 0.6805(3) 0.3616(12) 0.2802(3) 0.043(3) Uani 1 1 d . . . H45A H 0.6832 0.3799 0.2526 0.052 Uiso 1 1 d R . . C46A C 0.6936(4) 0.2599(9) 0.2925(4) 0.041(3) Uani 1 1 d . . . H46A H 0.7063 0.2132 0.2745 0.049 Uiso 1 1 d R . . C47A C 0.6894(3) 0.2289(9) 0.3331(4) 0.040(3) Uani 1 1 d . . . H47A H 0.6966 0.1599 0.3418 0.048 Uiso 1 1 d R . . C48A C 0.6702(4) 0.2978(9) 0.3599(3) 0.040(3) Uani 1 1 d . . . H48A H 0.6660 0.2781 0.3871 0.048 Uiso 1 1 d R . . C49A C 0.6588(3) 0.3991(8) 0.3463(3) 0.033(2) Uani 1 1 d . . . H49A H 0.6475 0.4476 0.3645 0.040 Uiso 1 1 d R . . Gd1B Gd 0.196435(14) 0.62550(4) 0.493765(13) 0.02637(12) Uani 1 1 d . . . O1B O 0.1873(2) 0.7210(6) 0.5540(2) 0.0338(17) Uani 1 1 d . . . O2B O 0.1464(2) 0.5066(6) 0.5164(2) 0.0341(17) Uani 1 1 d . . . O3B O 0.1668(2) 0.5809(6) 0.4286(2) 0.0367(18) Uani 1 1 d . . . O4B O 0.2071(2) 0.7914(5) 0.4650(2) 0.0305(16) Uani 1 1 d . . . O5B O 0.1284(2) 0.7091(6) 0.4860(2) 0.0391(18) Uani 1 1 d . . . H01B H 0.1127 0.7025 0.4696 0.059 Uiso 1 1 d R . . H02B H 0.1246 0.7607 0.4889 0.059 Uiso 1 1 d R . . N1B N 0.2676(3) 0.7026(7) 0.5295(3) 0.033(2) Uani 1 1 d . . . N2B N 0.2248(3) 0.5051(8) 0.5559(3) 0.037(2) Uani 1 1 d . . . N3B N 0.2172(3) 0.4335(7) 0.4680(2) 0.0304(19) Uani 1 1 d . . . N4B N 0.2596(2) 0.6327(7) 0.4428(2) 0.0295(17) Uani 1 1 d . . . N11B N 0.2069(3) 0.8305(8) 0.6053(3) 0.039(2) Uani 1 1 d . . . H11B H 0.2268 0.8712 0.6161 0.046 Uiso 1 1 d R . . N21B N 0.1194(3) 0.4026(9) 0.5641(3) 0.056(3) Uani 1 1 d . . . H21B H 0.1237 0.3686 0.5872 0.067 Uiso 1 1 d R . . N31B N 0.1477(3) 0.4675(8) 0.3780(3) 0.041(2) Uani 1 1 d . . . H31B H 0.1525 0.4063 0.3669 0.049 Uiso 1 1 d R . . N41B N 0.2332(3) 0.9075(7) 0.4218(3) 0.035(2) Uani 1 1 d . . . H41B H 0.2501 0.9188 0.4023 0.042 Uiso 1 1 d R . . C1B C 0.2871(4) 0.6206(11) 0.5592(3) 0.044(3) Uani 1 1 d . . . H1BB H 0.3064 0.6561 0.5792 0.053 Uiso 1 1 d R . . H1BC H 0.3036 0.5712 0.5436 0.053 Uiso 1 1 d R . . C2B C 0.2575(4) 0.5630(10) 0.5829(3) 0.044(3) Uani 1 1 d . . . H2BA H 0.2724 0.5118 0.6010 0.053 Uiso 1 1 d R . . H2BB H 0.2423 0.6116 0.6001 0.053 Uiso 1 1 d R . . C3B C 0.2448(4) 0.4061(9) 0.5414(3) 0.042(3) Uani 1 1 d . . . H3BA H 0.2453 0.3536 0.5635 0.050 Uiso 1 1 d R . . H3BB H 0.2741 0.4208 0.5357 0.050 Uiso 1 1 d R . . C4B C 0.2212(4) 0.3564(9) 0.5039(3) 0.037(3) Uani 1 1 d . . . H4BA H 0.2371 0.2941 0.4958 0.044 Uiso 1 1 d R . . H4BB H 0.1930 0.3330 0.5101 0.044 Uiso 1 1 d R . . C5B C 0.2580(4) 0.4361(9) 0.4484(3) 0.036(3) Uani 1 1 d . . . H5BA H 0.2611 0.3722 0.4319 0.044 Uiso 1 1 d R . . H5BB H 0.2809 0.4369 0.4698 0.044 Uiso 1 1 d R . . C6B C 0.2622(3) 0.5296(8) 0.4206(3) 0.032(2) Uani 1 1 d . . . H6BA H 0.2888 0.5253 0.4072 0.039 Uiso 1 1 d R . . H6BB H 0.2394 0.5285 0.3991 0.039 Uiso 1 1 d R . . C7B C 0.3002(3) 0.6497(9) 0.4663(3) 0.040(3) Uani 1 1 d . . . H7BA H 0.3216 0.6733 0.4480 0.047 Uiso 1 1 d R . . H7BB H 0.3092 0.5813 0.4779 0.047 Uiso 1 1 d R . . C8B C 0.2977(3) 0.7303(10) 0.4997(3) 0.035(3) Uani 1 1 d . . . H8BA H 0.3257 0.7381 0.5136 0.042 Uiso 1 1 d R . . H8BB H 0.2897 0.7992 0.4879 0.042 Uiso 1 1 d R . . C10B C 0.2557(4) 0.7958(9) 0.5526(4) 0.040(3) Uani 1 1 d . . . H10D H 0.2772 0.8108 0.5744 0.047 Uiso 1 1 d R . . H10E H 0.2540 0.8567 0.5340 0.047 Uiso 1 1 d R . . C11B C 0.2134(4) 0.7816(9) 0.5713(3) 0.036(3) Uani 1 1 d . . . C12B C 0.1660(4) 0.8216(10) 0.6245(4) 0.047(3) Uani 1 1 d . . . H12B H 0.1426 0.8332 0.6037 0.057 Uiso 1 1 d R . . C13B C 0.1632(5) 0.9113(10) 0.6557(4) 0.053(3) Uani 1 1 d . . . H13D H 0.1371 0.9077 0.6695 0.080 Uiso 1 1 d R . . H13E H 0.1650 0.9790 0.6419 0.080 Uiso 1 1 d R . . H13F H 0.1868 0.9038 0.6757 0.080 Uiso 1 1 d R . . C14B C 0.1606(4) 0.7160(10) 0.6433(3) 0.046(3) Uani 1 1 d . . . C15B C 0.1955(5) 0.6736(12) 0.6692(4) 0.058(4) Uani 1 1 d . . . H15B H 0.2215 0.7088 0.6728 0.070 Uiso 1 1 d R . . C16B C 0.1893(8) 0.5809(15) 0.6881(5) 0.090(7) Uani 1 1 d . . . H16B H 0.2112 0.5508 0.7048 0.108 Uiso 1 1 d R . . C17B C 0.1506(7) 0.5261(16) 0.6813(5) 0.083(6) Uani 1 1 d . . . H17B H 0.1479 0.4602 0.6943 0.099 Uiso 1 1 d R . . C18B C 0.1181(6) 0.5678(14) 0.6575(6) 0.072(5) Uani 1 1 d . . . H18B H 0.0924 0.5312 0.6544 0.087 Uiso 1 1 d R . . C19B C 0.1246(5) 0.6594(12) 0.6384(5) 0.067(4) Uani 1 1 d . . . H19B H 0.1026 0.6862 0.6209 0.081 Uiso 1 1 d R . . C20B C 0.1882(4) 0.4796(10) 0.5800(4) 0.042(3) Uani 1 1 d . . . H20D H 0.1830 0.5380 0.5988 0.051 Uiso 1 1 d R . . H20E H 0.1945 0.4159 0.5963 0.051 Uiso 1 1 d R . . C21B C 0.1498(4) 0.4646(10) 0.5514(4) 0.044(3) Uani 1 1 d . . . C22B C 0.0795(3) 0.3864(12) 0.5396(4) 0.054(4) Uani 1 1 d . . . H22B H 0.0671 0.4567 0.5330 0.064 Uiso 1 1 d R . . C23B C 0.0476(5) 0.3354(16) 0.5656(6) 0.091(6) Uani 1 1 d . . . H23D H 0.0437 0.3746 0.5906 0.137 Uiso 1 1 d R . . H23E H 0.0606 0.2677 0.5723 0.137 Uiso 1 1 d R . . H23F H 0.0205 0.3239 0.5511 0.137 Uiso 1 1 d R . . C24B C 0.0856(3) 0.3246(12) 0.5010(4) 0.052(3) Uani 1 1 d . . . C25B C 0.1043(4) 0.2289(13) 0.5022(5) 0.061(4) Uani 1 1 d . . . H25B H 0.1146 0.2000 0.5273 0.073 Uiso 1 1 d R . . C26B C 0.1095(5) 0.1765(15) 0.4676(6) 0.076(5) Uani 1 1 d . . . H26B H 0.1235 0.1108 0.4680 0.091 Uiso 1 1 d R . . C27B C 0.0924(5) 0.2175(19) 0.4313(6) 0.087(6) Uani 1 1 d . . . H27B H 0.0955 0.1810 0.4066 0.105 Uiso 1 1 d R . . C28B C 0.0734(4) 0.3122(16) 0.4268(6) 0.076(5) Uani 1 1 d . . . H28B H 0.0626 0.3402 0.4017 0.092 Uiso 1 1 d R . . C29B C 0.0712(4) 0.3630(17) 0.4639(5) 0.076(5) Uani 1 1 d . . . H29B H 0.0580 0.4296 0.4638 0.091 Uiso 1 1 d R . . C30B C 0.1833(3) 0.3995(8) 0.4392(3) 0.029(2) Uani 1 1 d . . . H30D H 0.1610 0.3671 0.4545 0.035 Uiso 1 1 d R . . H30E H 0.1940 0.3453 0.4211 0.035 Uiso 1 1 d R . . C31B C 0.1661(3) 0.4894(9) 0.4137(3) 0.035(2) Uani 1 1 d . . . C32B C 0.1214(4) 0.5474(9) 0.3548(3) 0.036(3) Uani 1 1 d . . . H32B H 0.1017 0.5793 0.3735 0.043 Uiso 1 1 d R . . C33B C 0.0960(4) 0.4891(10) 0.3212(4) 0.046(3) Uani 1 1 d . . . H33D H 0.0792 0.4338 0.3328 0.069 Uiso 1 1 d R . . H33E H 0.1146 0.4580 0.3020 0.069 Uiso 1 1 d R . . H33F H 0.0775 0.5399 0.3069 0.069 Uiso 1 1 d R . . C34B C 0.1499(3) 0.6318(9) 0.3389(3) 0.036(2) Uani 1 1 d . . . C35B C 0.1798(4) 0.6148(12) 0.3120(4) 0.050(3) Uani 1 1 d . . . H35B H 0.1842 0.5449 0.3033 0.060 Uiso 1 1 d R . . C36B C 0.2030(6) 0.703(2) 0.2984(5) 0.106(9) Uani 1 1 d . . . H36B H 0.2252 0.6891 0.2814 0.127 Uiso 1 1 d R . . C37B C 0.1978(7) 0.7984(17) 0.3116(6) 0.091(8) Uani 1 1 d . . . H37B H 0.2125 0.8556 0.3009 0.109 Uiso 1 1 d R . . C38B C 0.1673(6) 0.8207(11) 0.3365(5) 0.068(5) Uani 1 1 d . . . H38B H 0.1640 0.8905 0.3458 0.081 Uiso 1 1 d R . . C39B C 0.1449(4) 0.7376(10) 0.3502(4) 0.053(4) Uani 1 1 d . . . H39B H 0.1243 0.7540 0.3687 0.064 Uiso 1 1 d R . . C40B C 0.2500(4) 0.7191(9) 0.4142(3) 0.033(2) Uani 1 1 d . . . H40D H 0.2308 0.6944 0.3916 0.039 Uiso 1 1 d R . . H40E H 0.2761 0.7421 0.4025 0.039 Uiso 1 1 d R . . C41B C 0.2300(3) 0.8092(9) 0.4360(3) 0.034(3) Uani 1 1 d . . . C42B C 0.2104(3) 0.9964(9) 0.4390(3) 0.034(2) Uani 1 1 d . . . H42B H 0.1820 0.9697 0.4448 0.040 Uiso 1 1 calc R . . C43B C 0.2042(4) 1.0810(9) 0.4054(3) 0.038(3) Uani 1 1 d . . . H43D H 0.1909 1.0512 0.3805 0.057 Uiso 1 1 d R . . H43E H 0.2316 1.1086 0.3998 0.057 Uiso 1 1 d R . . H43F H 0.1868 1.1379 0.4151 0.057 Uiso 1 1 d R . . C44B C 0.2300(3) 1.0367(8) 0.4784(3) 0.033(2) Uani 1 1 d . . . C45B C 0.2717(3) 1.0718(9) 0.4807(3) 0.035(2) Uani 1 1 d . . . H45B H 0.2874 1.0676 0.4574 0.042 Uiso 1 1 d R . . C46B C 0.2881(4) 1.1121(11) 0.5159(3) 0.044(3) Uani 1 1 d . . . H46B H 0.3156 1.1390 0.5166 0.053 Uiso 1 1 d R . . C47B C 0.2680(4) 1.1155(9) 0.5511(3) 0.045(3) Uani 1 1 d . . . H47B H 0.2804 1.1414 0.5759 0.054 Uiso 1 1 d R . . C48B C 0.2269(4) 1.0820(9) 0.5491(3) 0.038(3) Uani 1 1 d . . . H48B H 0.2114 1.0836 0.5727 0.046 Uiso 1 1 d R . . C49B C 0.2089(4) 1.0421(8) 0.5141(3) 0.036(2) Uani 1 1 d . . . H49B H 0.1810 1.0175 0.5134 0.043 Uiso 1 1 d R . . S1 S 0.15358(9) 0.2061(2) 0.30916(9) 0.0358(6) Uani 1 1 d . . . O11 O 0.1513(3) 0.0938(6) 0.3106(3) 0.060(3) Uani 1 1 d . . . O12 O 0.1302(3) 0.2542(6) 0.2756(3) 0.048(2) Uani 1 1 d . . . O13 O 0.1505(2) 0.2555(6) 0.3476(2) 0.0418(19) Uani 1 1 d . . . C1S C 0.2073(5) 0.2351(14) 0.2973(4) 0.060(4) Uani 1 1 d . . . F11 F 0.2162(4) 0.1960(13) 0.2632(3) 0.129(5) Uani 1 1 d . . . F12 F 0.2343(2) 0.1988(8) 0.3262(3) 0.079(3) Uani 1 1 d . . . F13 F 0.2115(3) 0.3403(10) 0.2962(4) 0.112(5) Uani 1 1 d . . . S2 S 0.31537(10) 0.9046(2) 0.65943(10) 0.0440(7) Uani 1 1 d . . . O21 O 0.2821(3) 0.9525(7) 0.6349(3) 0.053(2) Uani 1 1 d . . . O22 O 0.3216(3) 0.7925(7) 0.6502(3) 0.054(2) Uani 1 1 d . . . O23 O 0.3529(3) 0.9654(8) 0.6651(4) 0.072(3) Uani 1 1 d . . . C2S C 0.2976(4) 0.9059(9) 0.7101(3) 0.041(3) Uani 1 1 d . . . F21 F 0.3258(2) 0.8764(7) 0.7374(2) 0.0575(18) Uani 1 1 d . . . F22 F 0.2630(2) 0.8418(6) 0.7128(2) 0.061(2) Uani 1 1 d . . . F23 F 0.2841(3) 1.0034(6) 0.7200(2) 0.069(2) Uani 1 1 d . . . S3 S 0.14119(11) 0.2036(2) 0.64823(9) 0.0458(8) Uani 1 1 d . . . O31 O 0.1263(3) 0.1482(7) 0.6824(2) 0.047(2) Uani 1 1 d . . . O32 O 0.1263(3) 0.3104(7) 0.6444(3) 0.052(2) Uani 1 1 d . . . O33 O 0.1414(3) 0.1500(8) 0.6105(3) 0.059(2) Uani 1 1 d . . . C3S C 0.1972(4) 0.2168(10) 0.6626(4) 0.051(3) Uani 1 1 d . . . F31 F 0.2149(2) 0.1253(7) 0.6705(3) 0.064(2) Uani 1 1 d . . . F32 F 0.2163(3) 0.2620(6) 0.6320(3) 0.070(3) Uani 1 1 d . . . F33 F 0.2047(3) 0.2748(8) 0.6960(3) 0.078(3) Uani 1 1 d . . . S4 S 0.61211(11) 0.4453(3) 0.45470(11) 0.0588(9) Uani 1 1 d . . . O41 O 0.5927(3) 0.3917(8) 0.4214(2) 0.057(2) Uani 1 1 d . . . O42 O 0.6498(3) 0.3985(10) 0.4730(3) 0.078(3) Uani 1 1 d . . . O43 O 0.6137(4) 0.5631(9) 0.4494(4) 0.091(4) Uani 1 1 d . . . C4S C 0.5764(7) 0.4290(16) 0.4928(5) 0.080(5) Uani 1 1 d . . . F41 F 0.5709(4) 0.3290(9) 0.5029(3) 0.098(4) Uani 1 1 d . . . F42 F 0.5396(4) 0.4700(13) 0.4803(4) 0.144(6) Uani 1 1 d . . . F43 F 0.5902(6) 0.4875(11) 0.5266(3) 0.152(7) Uani 1 1 d . . . S5 S 0.0287(2) 0.7081(7) 0.3967(2) 0.107(2) Uani 0.85 1 d PD . . O51 O 0.0332(5) 0.7015(14) 0.3530(4) 0.121(6) Uani 1 1 d . . . O52 O 0.0623(4) 0.6747(16) 0.4232(4) 0.132(7) Uani 1 1 d . . . O53 O 0.0008(12) 0.785(3) 0.4056(11) 0.142(13) Uiso 0.50 1 d P . . C5S C -0.0041(12) 0.593(4) 0.3997(7) 0.122(16) Uiso 0.50 1 d PD . . F51 F 0.0185(8) 0.5161(17) 0.3943(7) 0.248(11) Uiso 1 1 d D . . F52 F -0.0186(9) 0.594(2) 0.4334(9) 0.161(12) Uiso 0.50 1 d PD . . F53 F -0.0317(9) 0.600(3) 0.3718(11) 0.21(2) Uiso 0.35 1 d PD . . S6 S 0.32897(10) 0.9756(3) 0.35791(10) 0.0497(8) Uani 1 1 d . . . O61 O 0.3697(2) 1.0181(6) 0.3649(3) 0.045(2) Uani 1 1 d . . . O62 O 0.2963(4) 1.0200(12) 0.3785(3) 0.095(4) Uani 1 1 d . . . O63 O 0.3272(4) 0.8624(11) 0.3573(5) 0.113(5) Uani 1 1 d . . . C6S C 0.3174(4) 1.0098(14) 0.3041(5) 0.063(4) Uani 1 1 d . . . F61 F 0.3204(3) 1.1126(8) 0.2990(3) 0.086(3) Uani 1 1 d . . . F62 F 0.3434(3) 0.9652(11) 0.2805(3) 0.107(4) Uani 1 1 d . . . F63 F 0.2776(3) 0.9822(9) 0.2919(3) 0.085(3) Uani 1 1 d . . . O1S O 0.5226(5) 0.6702(9) 0.3836(4) 0.092(4) Uani 1 1 d . . . C7S C 0.5121(11) 0.681(3) 0.4275(11) 0.102(10) Uiso 0.65 1 d P . . C7S' C 0.485(3) 0.613(7) 0.394(2) 0.13(2) Uiso 0.35 1 d P . . C8S C 0.4678(8) 0.6544(18) 0.4315(11) 0.149(13) Uani 1 1 d . . . O2S O 0.1075(9) 0.903(2) 0.4975(9) 0.179(11) Uiso 0.75 1 d P . . O3S O -0.0227(12) 0.996(3) 0.3955(12) 0.146(13) Uiso 0.50 1 d P . . C11S C 0.0014(15) 1.078(4) 0.4108(15) 0.112(15) Uiso 0.50 1 d P . . C12S C 0.0017(19) 1.060(5) 0.4613(18) 0.15(2) Uiso 0.50 1 d P . . O1W O 0.6060(5) 0.7314(16) 0.3906(6) 0.145(7) Uani 1 1 d . . . O2W O 0.0944(10) 0.984(3) 0.5671(10) 0.125(10) Uiso 0.50 1 d P . . 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 Gd1A 0.0219(2) 0.0208(2) 0.0245(2) 0.0014(2) 0.00240(16) 0.0011(2) O1A 0.033(4) 0.026(4) 0.027(4) 0.003(3) 0.002(3) 0.002(3) O2A 0.019(3) 0.020(3) 0.034(4) -0.003(3) 0.008(3) -0.001(2) O3A 0.022(4) 0.019(3) 0.045(4) -0.001(3) 0.004(3) -0.001(3) O4A 0.021(3) 0.031(4) 0.029(4) 0.008(3) -0.001(3) 0.000(3) O5A 0.030(4) 0.017(3) 0.038(4) -0.005(3) -0.006(3) -0.003(3) N1A 0.031(5) 0.025(4) 0.027(4) 0.001(3) 0.003(3) -0.004(4) N2A 0.031(5) 0.015(4) 0.029(4) -0.003(3) 0.002(4) 0.004(3) N3A 0.014(4) 0.033(5) 0.030(4) 0.000(3) 0.005(3) -0.003(3) N4A 0.027(4) 0.020(4) 0.032(5) 0.005(3) 0.003(3) -0.003(3) N11A 0.039(5) 0.032(5) 0.035(4) 0.010(4) 0.011(4) 0.005(4) N21A 0.019(4) 0.028(4) 0.034(5) 0.001(4) 0.011(3) 0.000(3) N31A 0.019(4) 0.022(4) 0.037(5) -0.002(3) 0.000(3) 0.003(3) N41A 0.035(5) 0.027(4) 0.025(4) 0.008(3) 0.006(3) -0.002(4) C1A 0.027(5) 0.021(5) 0.044(6) -0.002(4) 0.008(4) 0.010(4) C2A 0.036(5) 0.012(5) 0.034(5) -0.008(4) 0.010(4) -0.003(4) C3A 0.041(6) 0.033(6) 0.023(5) -0.003(4) 0.003(4) 0.000(5) C4A 0.023(5) 0.038(6) 0.025(5) -0.003(4) 0.004(4) 0.002(4) C5A 0.035(6) 0.036(6) 0.023(5) 0.002(4) 0.001(4) 0.005(4) C6A 0.032(5) 0.033(6) 0.027(5) 0.001(4) 0.002(4) 0.011(5) C7A 0.031(5) 0.041(7) 0.024(5) 0.003(4) 0.005(4) -0.001(5) C8A 0.020(5) 0.024(5) 0.031(5) 0.003(4) 0.007(4) 0.000(4) C10A 0.041(6) 0.034(6) 0.037(6) 0.007(5) 0.003(5) 0.016(5) C11A 0.021(5) 0.024(5) 0.038(6) 0.002(4) 0.000(4) 0.008(4) C12A 0.023(5) 0.044(6) 0.037(5) 0.012(6) 0.001(4) 0.000(5) C13A 0.042(8) 0.090(11) 0.057(9) 0.035(8) -0.012(6) 0.015(7) C14A 0.033(6) 0.044(6) 0.034(6) 0.018(5) -0.002(5) 0.001(5) C15A 0.069(9) 0.032(6) 0.051(8) 0.007(6) -0.007(7) 0.006(6) C16A 0.054(9) 0.051(8) 0.093(12) 0.026(8) -0.026(8) -0.021(7) C17A 0.043(8) 0.104(14) 0.055(9) 0.027(9) -0.003(7) -0.002(9) C18A 0.064(9) 0.108(14) 0.050(8) 0.032(10) 0.010(7) 0.014(11) C19A 0.038(6) 0.055(8) 0.051(7) 0.006(6) 0.008(5) 0.005(6) C20A 0.027(5) 0.021(5) 0.025(5) 0.006(4) 0.007(4) 0.001(4) C21A 0.021(5) 0.026(5) 0.026(5) 0.002(4) 0.000(4) -0.004(4) C22A 0.025(5) 0.026(5) 0.032(5) -0.001(4) 0.006(4) -0.001(4) C23A 0.037(6) 0.043(7) 0.049(7) 0.012(6) 0.021(5) 0.013(5) C24A 0.028(5) 0.029(5) 0.028(5) 0.005(4) 0.013(4) 0.009(4) C25A 0.033(6) 0.034(7) 0.054(7) 0.004(5) 0.009(5) 0.008(5) C26A 0.031(6) 0.074(10) 0.056(8) 0.008(7) 0.004(6) 0.013(6) C27A 0.065(9) 0.049(8) 0.044(7) 0.020(6) 0.022(7) 0.019(7) C28A 0.060(8) 0.031(7) 0.048(7) 0.003(5) 0.021(6) 0.003(5) C29A 0.039(6) 0.036(6) 0.028(5) -0.001(4) 0.013(4) -0.002(5) C30A 0.015(5) 0.033(6) 0.042(6) 0.000(5) 0.003(4) 0.004(4) C31A 0.024(5) 0.025(5) 0.029(5) 0.006(4) 0.005(4) 0.004(4) C32A 0.039(6) 0.023(5) 0.042(6) 0.002(5) 0.009(5) -0.005(4) C33A 0.046(6) 0.029(6) 0.039(6) -0.003(5) 0.015(5) 0.001(5) C34A 0.027(5) 0.023(5) 0.064(8) 0.009(5) 0.009(5) 0.001(4) C35A 0.035(6) 0.034(6) 0.061(8) 0.014(6) 0.018(6) 0.014(5) C36A 0.103(14) 0.045(8) 0.076(11) 0.024(8) 0.042(10) -0.008(9) C37A 0.057(10) 0.039(8) 0.152(18) 0.028(9) 0.066(12) 0.002(7) C38A 0.039(8) 0.050(8) 0.117(15) 0.000(9) 0.018(9) 0.000(6) C39A 0.041(7) 0.032(6) 0.072(9) -0.002(6) 0.005(6) -0.012(5) C40A 0.035(6) 0.031(6) 0.040(6) 0.010(5) 0.015(5) -0.001(5) C41A 0.024(5) 0.027(5) 0.034(6) 0.002(4) 0.003(4) 0.007(4) C42A 0.028(5) 0.024(5) 0.048(6) -0.004(5) 0.006(5) -0.008(4) C43A 0.044(7) 0.038(7) 0.065(8) 0.010(6) -0.015(6) -0.019(5) C44A 0.020(5) 0.039(6) 0.035(6) 0.013(5) -0.001(4) 0.003(4) C45A 0.030(5) 0.061(8) 0.038(6) 0.000(6) -0.005(4) 0.006(6) C46A 0.030(6) 0.036(6) 0.058(8) 0.001(6) 0.006(5) 0.004(5) C47A 0.033(6) 0.037(6) 0.051(7) 0.008(5) 0.006(5) 0.008(5) C48A 0.042(7) 0.044(7) 0.033(6) 0.007(5) -0.002(5) 0.004(5) C49A 0.030(5) 0.038(7) 0.031(5) -0.005(4) -0.007(4) 0.000(4) Gd1B 0.0268(2) 0.0301(3) 0.0223(2) 0.0023(2) 0.00254(17) 0.0060(2) O1B 0.040(4) 0.041(4) 0.021(3) 0.000(3) 0.008(3) -0.001(4) O2B 0.033(4) 0.035(4) 0.035(4) 0.019(3) 0.005(3) 0.003(3) O3B 0.047(5) 0.039(4) 0.024(4) -0.003(3) -0.003(3) 0.029(4) O4B 0.040(4) 0.024(4) 0.028(4) -0.003(3) 0.007(3) -0.003(3) O5B 0.038(4) 0.036(4) 0.043(4) 0.002(3) -0.008(3) 0.013(3) N1B 0.030(5) 0.042(5) 0.027(4) -0.007(4) -0.001(4) 0.009(4) N2B 0.041(5) 0.042(5) 0.027(5) 0.001(4) -0.005(4) 0.004(4) N3B 0.034(5) 0.034(5) 0.023(4) 0.001(4) 0.001(4) 0.006(4) N4B 0.027(4) 0.033(4) 0.029(4) -0.009(4) 0.004(3) 0.005(4) N11B 0.040(5) 0.047(5) 0.028(5) -0.002(4) -0.002(4) 0.009(4) N21B 0.049(6) 0.070(8) 0.051(6) 0.025(5) 0.022(5) 0.012(5) N31B 0.062(7) 0.031(5) 0.029(5) 0.004(4) -0.006(4) 0.000(5) N41B 0.046(5) 0.036(5) 0.024(4) -0.001(4) 0.011(4) -0.010(4) C1B 0.050(7) 0.040(6) 0.041(6) 0.002(6) -0.009(5) 0.020(6) C2B 0.054(8) 0.048(7) 0.028(6) 0.005(5) -0.009(5) 0.027(6) C3B 0.047(7) 0.049(7) 0.028(5) 0.010(5) -0.002(5) 0.013(5) C4B 0.043(6) 0.033(7) 0.034(5) 0.009(5) -0.002(4) 0.011(5) C5B 0.042(6) 0.035(6) 0.032(6) -0.008(5) 0.004(5) 0.013(5) C6B 0.033(6) 0.035(6) 0.030(5) -0.005(4) 0.012(4) -0.001(5) C7B 0.037(6) 0.044(7) 0.039(6) -0.016(5) 0.009(5) -0.003(5) C8B 0.012(5) 0.051(7) 0.041(6) -0.012(5) -0.005(4) -0.010(4) C10B 0.042(7) 0.038(6) 0.038(6) -0.004(5) -0.006(5) 0.010(5) C11B 0.046(7) 0.030(6) 0.034(6) 0.004(5) 0.006(5) 0.001(5) C12B 0.060(8) 0.054(7) 0.029(6) 0.000(5) 0.011(5) 0.011(6) C13B 0.075(9) 0.046(7) 0.041(7) 0.012(6) 0.020(6) 0.012(6) C14B 0.073(9) 0.038(7) 0.028(6) -0.001(5) 0.009(6) 0.012(6) C15B 0.062(9) 0.071(9) 0.042(7) 0.009(7) 0.001(6) 0.005(7) C16B 0.16(2) 0.073(11) 0.036(8) 0.008(8) 0.011(10) 0.044(13) C17B 0.124(17) 0.080(13) 0.049(10) 0.008(9) 0.034(11) -0.020(13) C18B 0.077(12) 0.066(10) 0.080(12) -0.007(9) 0.047(10) -0.004(9) C19B 0.062(10) 0.067(10) 0.075(11) -0.003(8) 0.029(8) 0.004(8) C20B 0.045(7) 0.045(7) 0.037(6) 0.011(5) 0.000(5) 0.004(6) C21B 0.042(7) 0.052(7) 0.040(7) 0.014(6) 0.009(5) 0.017(6) C22B 0.022(5) 0.067(9) 0.072(8) 0.034(8) 0.010(5) 0.005(6) C23B 0.044(9) 0.124(17) 0.110(14) -0.005(12) 0.039(9) -0.021(9) C24B 0.016(5) 0.076(9) 0.065(9) 0.018(7) 0.013(5) -0.005(6) C25B 0.050(8) 0.081(11) 0.055(9) 0.005(8) 0.024(7) -0.010(8) C26B 0.043(8) 0.094(13) 0.093(13) 0.014(10) 0.017(8) 0.004(8) C27B 0.056(10) 0.132(18) 0.075(12) 0.009(12) 0.016(9) -0.017(11) C28B 0.028(7) 0.110(15) 0.090(13) 0.043(11) -0.008(7) -0.025(8) C29B 0.033(7) 0.114(14) 0.081(11) 0.021(12) 0.005(7) -0.031(9) C30B 0.037(6) 0.027(6) 0.023(5) 0.007(4) -0.001(4) 0.000(4) C31B 0.041(6) 0.031(6) 0.033(6) 0.007(5) 0.006(5) 0.003(5) C32B 0.042(6) 0.038(6) 0.026(5) 0.005(5) -0.015(5) -0.007(5) C33B 0.050(7) 0.046(7) 0.039(7) 0.007(6) -0.007(5) -0.015(6) C34B 0.054(7) 0.027(5) 0.026(5) 0.004(5) -0.011(4) -0.012(5) C35B 0.049(7) 0.051(8) 0.051(7) 0.003(7) 0.007(6) -0.008(7) C36B 0.076(13) 0.19(3) 0.043(9) 0.035(13) -0.017(8) -0.063(15) C37B 0.103(16) 0.082(13) 0.078(13) 0.051(11) -0.064(12) -0.061(13) C38B 0.089(12) 0.033(7) 0.073(11) 0.020(7) -0.056(9) -0.017(8) C39B 0.054(8) 0.043(7) 0.057(8) 0.002(6) -0.039(7) -0.005(6) C40B 0.032(6) 0.034(6) 0.034(6) 0.001(5) 0.004(5) 0.002(5) C41B 0.029(6) 0.048(7) 0.025(5) -0.006(5) 0.009(4) -0.010(5) C42B 0.032(6) 0.036(6) 0.033(6) -0.002(5) 0.004(4) -0.006(5) C43B 0.034(6) 0.041(6) 0.038(6) 0.007(5) 0.002(5) 0.008(5) C44B 0.037(6) 0.022(5) 0.039(6) 0.003(4) 0.001(5) -0.007(4) C45B 0.034(6) 0.032(6) 0.039(6) -0.001(5) 0.001(5) 0.011(5) C46B 0.034(6) 0.060(8) 0.038(6) -0.003(6) -0.014(5) 0.006(6) C47B 0.079(9) 0.025(6) 0.028(5) -0.006(5) -0.015(5) -0.001(7) C48B 0.039(6) 0.042(6) 0.034(6) -0.005(5) 0.010(5) 0.012(5) C49B 0.037(6) 0.027(5) 0.044(6) -0.001(5) 0.005(5) 0.001(5) S1 0.0389(15) 0.0306(14) 0.0362(15) -0.0003(11) -0.0102(12) -0.0053(12) O11 0.090(7) 0.023(4) 0.063(6) 0.001(4) -0.035(5) -0.004(4) O12 0.048(5) 0.040(5) 0.055(5) 0.008(4) -0.018(4) -0.007(4) O13 0.044(5) 0.033(4) 0.047(5) 0.006(4) -0.002(4) 0.004(4) C1S 0.055(9) 0.079(11) 0.047(8) 0.015(7) 0.003(7) -0.004(8) F11 0.103(9) 0.229(16) 0.058(6) -0.008(8) 0.033(6) 0.041(9) F12 0.040(4) 0.113(8) 0.084(6) 0.030(6) 0.002(4) 0.015(5) F13 0.050(5) 0.151(12) 0.132(9) 0.075(8) -0.013(5) -0.033(6) S2 0.0444(17) 0.0425(17) 0.0465(17) -0.0049(13) 0.0131(13) -0.0086(13) O21 0.071(6) 0.050(5) 0.037(5) 0.003(4) -0.001(4) -0.004(5) O22 0.060(6) 0.058(6) 0.045(5) -0.011(4) 0.009(4) 0.001(5) O23 0.054(6) 0.059(6) 0.105(9) -0.002(6) 0.021(6) -0.020(5) C2S 0.066(8) 0.030(6) 0.026(5) 0.000(4) 0.001(5) -0.010(5) F21 0.063(4) 0.055(4) 0.053(4) -0.005(4) -0.010(3) 0.009(4) F22 0.059(5) 0.064(5) 0.061(5) 0.003(4) 0.012(4) 0.002(4) F23 0.110(7) 0.045(4) 0.051(5) -0.006(4) 0.008(5) 0.008(4) S3 0.0565(19) 0.0432(17) 0.0398(16) 0.0133(14) 0.0187(14) 0.0164(14) O31 0.047(5) 0.050(5) 0.046(5) 0.023(4) 0.019(4) 0.007(4) O32 0.055(5) 0.054(5) 0.051(5) 0.018(4) 0.029(4) 0.025(4) O33 0.062(6) 0.064(6) 0.050(5) 0.008(5) 0.006(4) 0.007(5) C3S 0.054(8) 0.032(6) 0.069(9) 0.012(6) 0.004(7) 0.017(6) F31 0.058(4) 0.051(4) 0.082(5) 0.008(5) -0.001(4) 0.007(4) F32 0.062(5) 0.057(5) 0.096(6) 0.038(5) 0.036(5) 0.020(4) F33 0.075(6) 0.076(6) 0.082(6) -0.027(5) -0.003(5) -0.005(5) S4 0.0434(19) 0.084(3) 0.0476(19) -0.0031(18) -0.0048(15) -0.0061(18) O41 0.061(5) 0.078(7) 0.031(4) -0.008(4) -0.011(4) 0.014(5) O42 0.037(5) 0.121(10) 0.074(6) 0.027(7) -0.015(4) -0.010(6) O43 0.068(7) 0.071(7) 0.129(11) 0.042(7) -0.021(7) -0.027(6) C4S 0.122(17) 0.081(12) 0.038(8) 0.003(8) 0.014(9) 0.002(11) F41 0.101(8) 0.108(8) 0.083(7) 0.044(6) -0.004(6) -0.035(6) F42 0.071(7) 0.220(16) 0.149(11) 0.067(11) 0.071(7) 0.064(9) F43 0.30(2) 0.109(10) 0.048(6) -0.004(6) 0.036(9) 0.053(12) S5 0.073(4) 0.149(6) 0.097(5) 0.000(4) -0.002(3) 0.054(4) O51 0.134(13) 0.140(13) 0.087(10) 0.024(9) -0.015(9) 0.060(11) O52 0.069(8) 0.26(2) 0.064(7) -0.061(10) -0.019(6) 0.054(10) S6 0.0370(16) 0.061(2) 0.0525(19) 0.0045(16) 0.0128(14) -0.0102(15) O61 0.036(4) 0.043(5) 0.056(5) -0.004(4) 0.008(4) -0.009(4) O62 0.071(7) 0.161(13) 0.054(6) -0.002(7) 0.022(5) 0.026(8) O63 0.117(11) 0.065(8) 0.159(13) 0.029(9) 0.019(9) -0.038(8) C6S 0.035(7) 0.097(13) 0.058(9) -0.017(9) 0.002(6) 0.003(8) F61 0.102(7) 0.072(6) 0.083(6) 0.032(5) -0.008(5) -0.012(6) F62 0.085(7) 0.177(12) 0.057(6) -0.033(7) 0.003(5) 0.061(7) F63 0.062(6) 0.102(8) 0.090(7) 0.000(6) -0.016(5) -0.019(5) O1S 0.124(11) 0.056(7) 0.092(9) -0.003(6) -0.034(8) 0.004(7) C8S 0.105(18) 0.078(15) 0.28(4) 0.044(18) 0.10(2) 0.003(12) O1W 0.086(11) 0.171(17) 0.179(18) 0.064(14) 0.010(11) 0.006(11) _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 Gd1A O1A 2.347(7) . ? Gd1A O3A 2.348(7) . ? Gd1A O4A 2.389(6) . ? Gd1A O2A 2.398(6) . ? Gd1A O5A 2.408(7) . ? Gd1A N3A 2.681(8) . ? Gd1A N2A 2.688(8) . ? Gd1A N4A 2.688(8) . ? Gd1A N1A 2.694(8) . ? O1A C11A 1.224(11) . ? O2A C21A 1.267(11) . ? O3A C31A 1.257(12) . ? O4A C41A 1.273(12) . ? N1A C1A 1.452(13) . ? N1A C10A 1.497(13) . ? N1A C8A 1.512(12) . ? N2A C3A 1.463(13) . ? N2A C2A 1.489(11) . ? N2A C20A 1.503(12) . ? N3A C4A 1.458(13) . ? N3A C30A 1.467(13) . ? N3A C5A 1.497(12) . ? N4A C6A 1.458(13) . ? N4A C40A 1.476(13) . ? N4A C7A 1.506(13) . ? N11A C11A 1.328(13) . ? N11A C12A 1.498(13) . ? N21A C21A 1.327(12) . ? N21A C22A 1.481(12) . ? N31A C31A 1.278(12) . ? N31A C32A 1.450(13) . ? N41A C41A 1.297(13) . ? N41A C42A 1.495(14) . ? C1A C2A 1.524(13) . ? C3A C4A 1.528(14) . ? C5A C6A 1.538(15) . ? C7A C8A 1.498(14) . ? C10A C11A 1.503(15) . ? C12A C14A 1.513(14) . ? C12A C13A 1.555(15) . ? C14A C15A 1.377(17) . ? C14A C19A 1.400(17) . ? C15A C16A 1.41(2) . ? C16A C17A 1.41(2) . ? C17A C18A 1.35(3) . ? C18A C19A 1.39(2) . ? C20A C21A 1.481(13) . ? C22A C24A 1.517(14) . ? C22A C23A 1.562(14) . ? C24A C29A 1.384(15) . ? C24A C25A 1.410(15) . ? C25A C26A 1.384(17) . ? C26A C27A 1.40(2) . ? C27A C28A 1.358(19) . ? C28A C29A 1.402(17) . ? C30A C31A 1.538(14) . ? C32A C33A 1.527(14) . ? C32A C34A 1.527(15) . ? C34A C35A 1.360(18) . ? C34A C39A 1.409(17) . ? C35A C36A 1.394(18) . ? C36A C37A 1.33(3) . ? C37A C38A 1.37(2) . ? C38A C39A 1.354(19) . ? C40A C41A 1.523(15) . ? C42A C44A 1.511(15) . ? C42A C43A 1.537(15) . ? C44A C45A 1.360(16) . ? C44A C49A 1.367(14) . ? C45A C46A 1.404(18) . ? C46A C47A 1.402(17) . ? C47A C48A 1.406(16) . ? C48A C49A 1.397(16) . ? Gd1B O4B 2.335(7) . ? Gd1B O3B 2.345(7) . ? Gd1B O1B 2.347(7) . ? Gd1B O2B 2.352(7) . ? Gd1B O5B 2.421(7) . ? Gd1B N2B 2.653(9) . ? Gd1B N3B 2.669(9) . ? Gd1B N1B 2.679(9) . ? Gd1B N4B 2.701(8) . ? O1B C11B 1.244(13) . ? O2B C21B 1.260(13) . ? O3B C31B 1.256(13) . ? O4B C41B 1.257(12) . ? N1B C8B 1.458(13) . ? N1B C10B 1.464(14) . ? N1B C1B 1.526(14) . ? N2B C3B 1.497(15) . ? N2B C20B 1.489(15) . ? N2B C2B 1.516(15) . ? N3B C30B 1.457(13) . ? N3B C5B 1.491(14) . ? N3B C4B 1.524(13) . ? N4B C40B 1.460(14) . ? N4B C7B 1.483(13) . ? N4B C6B 1.500(13) . ? N11B C11B 1.302(14) . ? N11B C12B 1.492(15) . ? N21B C21B 1.339(16) . ? N21B C22B 1.477(16) . ? N31B C31B 1.304(14) . ? N31B C32B 1.494(14) . ? N41B C41B 1.334(14) . ? N41B C42B 1.473(14) . ? C1B C2B 1.459(18) . ? C3B C4B 1.536(15) . ? C5B C6B 1.503(15) . ? C7B C8B 1.501(14) . ? C10B C11B 1.531(16) . ? C12B C14B 1.486(18) . ? C12B C13B 1.533(17) . ? C14B C19B 1.36(2) . ? C14B C15B 1.462(19) . ? C15B C16B 1.35(2) . ? C16B C17B 1.43(3) . ? C17B C18B 1.37(3) . ? C18B C19B 1.34(2) . ? C20B C21B 1.508(17) . ? C22B C24B 1.51(2) . ? C22B C23B 1.515(18) . ? C24B C25B 1.35(2) . ? C24B C29B 1.36(2) . ? C25B C26B 1.33(2) . ? C26B C27B 1.38(2) . ? C27B C28B 1.35(3) . ? C28B C29B 1.38(2) . ? C30B C31B 1.495(14) . ? C32B C33B 1.517(15) . ? C32B C34B 1.518(15) . ? C34B C35B 1.358(16) . ? C34B C39B 1.401(17) . ? C35B C36B 1.42(2) . ? C36B C37B 1.30(3) . ? C37B C38B 1.34(3) . ? C38B C39B 1.36(2) . ? C40B C41B 1.508(15) . ? C42B C44B 1.486(15) . ? C42B C43B 1.539(15) . ? C44B C49B 1.387(15) . ? C44B C45B 1.403(15) . ? C45B C46B 1.336(15) . ? C46B C47B 1.356(16) . ? C47B C48B 1.381(17) . ? C48B C49B 1.347(16) . ? S1 O13 1.413(9) . ? S1 O11 1.423(8) . ? S1 O12 1.426(8) . ? S1 C1S 1.823(15) . ? C1S F11 1.269(18) . ? C1S F12 1.324(16) . ? C1S F13 1.340(19) . ? S2 O23 1.429(10) . ? S2 O21 1.429(10) . ? S2 O22 1.466(10) . ? S2 C2S 1.786(12) . ? C2S F21 1.285(14) . ? C2S F23 1.352(14) . ? C2S F22 1.380(14) . ? S3 O33 1.408(10) . ? S3 O31 1.427(8) . ? S3 O32 1.436(9) . ? S3 C3S 1.834(14) . ? C3S F31 1.308(14) . ? C3S F33 1.325(16) . ? C3S F32 1.334(15) . ? S4 O41 1.396(9) . ? S4 O42 1.439(10) . ? S4 O43 1.501(12) . ? S4 C4S 1.755(18) . ? C4S F41 1.322(19) . ? C4S F42 1.33(2) . ? C4S F43 1.38(2) . ? S5 O53 1.36(4) . ? S5 O52 1.403(13) . ? S5 O51 1.448(15) . ? S5 C5S 1.80(5) . ? C5S F52 1.22(3) . ? C5S F51 1.23(3) . ? C5S F53 1.23(3) . ? S6 O62 1.398(11) . ? S6 O61 1.417(8) . ? S6 O63 1.435(14) . ? S6 C6S 1.829(16) . ? C6S F62 1.299(16) . ? C6S F61 1.316(19) . ? C6S F63 1.356(16) . ? O1S C7S 1.50(4) . ? O1S C7S' 1.46(8) . ? C7S C8S 1.47(4) . ? C7S C7S' 1.60(8) . ? C7S' C8S 1.48(8) . ? O3S C11S 1.36(6) . ? C11S C12S 1.67(7) . ? 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 O1A Gd1A O3A 144.1(2) . . ? O1A Gd1A O4A 84.8(2) . . ? O3A Gd1A O4A 84.9(2) . . ? O1A Gd1A O2A 85.8(2) . . ? O3A Gd1A O2A 84.4(2) . . ? O4A Gd1A O2A 147.0(2) . . ? O1A Gd1A O5A 71.2(2) . . ? O3A Gd1A O5A 73.0(2) . . ? O4A Gd1A O5A 72.7(2) . . ? O2A Gd1A O5A 74.3(2) . . ? O1A Gd1A N3A 141.3(2) . . ? O3A Gd1A N3A 66.6(2) . . ? O4A Gd1A N3A 129.9(2) . . ? O2A Gd1A N3A 72.6(2) . . ? O5A Gd1A N3A 129.3(2) . . ? O1A Gd1A N2A 74.8(2) . . ? O3A Gd1A N2A 130.5(2) . . ? O4A Gd1A N2A 140.3(2) . . ? O2A Gd1A N2A 65.7(2) . . ? O5A Gd1A N2A 128.5(2) . . ? N3A Gd1A N2A 67.2(2) . . ? O1A Gd1A N4A 130.7(2) . . ? O3A Gd1A N4A 74.1(2) . . ? O4A Gd1A N4A 65.4(2) . . ? O2A Gd1A N4A 139.5(2) . . ? O5A Gd1A N4A 128.1(2) . . ? N3A Gd1A N4A 67.4(2) . . ? N2A Gd1A N4A 103.3(2) . . ? O1A Gd1A N1A 65.7(2) . . ? O3A Gd1A N1A 142.1(2) . . ? O4A Gd1A N1A 73.9(2) . . ? O2A Gd1A N1A 129.4(2) . . ? O5A Gd1A N1A 126.9(2) . . ? N3A Gd1A N1A 103.8(2) . . ? N2A Gd1A N1A 66.8(2) . . ? N4A Gd1A N1A 68.6(2) . . ? C11A O1A Gd1A 126.1(6) . . ? C21A O2A Gd1A 122.7(6) . . ? C31A O3A Gd1A 125.3(6) . . ? C41A O4A Gd1A 125.4(6) . . ? C1A N1A C10A 111.0(8) . . ? C1A N1A C8A 108.8(8) . . ? C10A N1A C8A 109.9(8) . . ? C1A N1A Gd1A 112.2(6) . . ? C10A N1A Gd1A 105.4(6) . . ? C8A N1A Gd1A 109.6(6) . . ? C3A N2A C2A 108.3(8) . . ? C3A N2A C20A 109.9(8) . . ? C2A N2A C20A 108.7(7) . . ? C3A N2A Gd1A 111.8(6) . . ? C2A N2A Gd1A 112.1(6) . . ? C20A N2A Gd1A 106.0(5) . . ? C4A N3A C30A 109.9(7) . . ? C4A N3A C5A 108.1(8) . . ? C30A N3A C5A 110.0(8) . . ? C4A N3A Gd1A 111.6(6) . . ? C30A N3A Gd1A 106.1(6) . . ? C5A N3A Gd1A 111.2(5) . . ? C6A N4A C40A 108.8(8) . . ? C6A N4A C7A 110.2(8) . . ? C40A N4A C7A 109.5(8) . . ? C6A N4A Gd1A 111.8(6) . . ? C40A N4A Gd1A 107.3(6) . . ? C7A N4A Gd1A 109.2(5) . . ? C11A N11A C12A 119.1(9) . . ? C21A N21A C22A 121.7(8) . . ? C31A N31A C32A 122.8(9) . . ? C41A N41A C42A 122.3(8) . . ? N1A C1A C2A 114.1(8) . . ? N2A C2A C1A 111.3(7) . . ? N2A C3A C4A 113.6(8) . . ? N3A C4A C3A 112.7(8) . . ? N3A C5A C6A 112.9(8) . . ? N4A C6A C5A 111.7(8) . . ? C8A C7A N4A 115.2(8) . . ? C7A C8A N1A 111.1(8) . . ? N1A C10A C11A 110.6(9) . . ? O1A C11A N11A 123.3(10) . . ? O1A C11A C10A 119.8(9) . . ? N11A C11A C10A 116.8(8) . . ? N11A C12A C14A 111.7(9) . . ? N11A C12A C13A 106.5(9) . . ? C14A C12A C13A 112.6(10) . . ? C15A C14A C19A 120.1(12) . . ? C15A C14A C12A 121.5(12) . . ? C19A C14A C12A 118.5(11) . . ? C14A C15A C16A 118.3(14) . . ? C17A C16A C15A 121.0(14) . . ? C18A C17A C16A 119.8(15) . . ? C17A C18A C19A 120.0(17) . . ? C14A C19A C18A 120.9(15) . . ? C21A C20A N2A 109.7(7) . . ? O2A C21A N21A 122.1(9) . . ? O2A C21A C20A 121.3(8) . . ? N21A C21A C20A 116.6(8) . . ? N21A C22A C24A 111.2(8) . . ? N21A C22A C23A 106.6(8) . . ? C24A C22A C23A 111.4(8) . . ? C29A C24A C25A 118.8(10) . . ? C29A C24A C22A 119.6(10) . . ? C25A C24A C22A 121.6(9) . . ? C26A C25A C24A 120.4(12) . . ? C25A C26A C27A 119.2(13) . . ? C28A C27A C26A 121.2(12) . . ? C27A C28A C29A 119.6(11) . . ? C24A C29A C28A 120.6(11) . . ? N3A C30A C31A 111.8(7) . . ? O3A C31A N31A 121.9(9) . . ? O3A C31A C30A 118.4(8) . . ? N31A C31A C30A 119.6(9) . . ? N31A C32A C33A 109.8(9) . . ? N31A C32A C34A 113.1(9) . . ? C33A C32A C34A 110.7(8) . . ? C35A C34A C39A 119.8(11) . . ? C35A C34A C32A 120.8(10) . . ? C39A C34A C32A 119.4(11) . . ? C34A C35A C36A 117.3(13) . . ? C37A C36A C35A 122.2(17) . . ? C36A C37A C38A 121.0(13) . . ? C39A C38A C37A 118.3(15) . . ? C38A C39A C34A 121.0(14) . . ? N4A C40A C41A 111.6(8) . . ? O4A C41A N41A 124.1(10) . . ? O4A C41A C40A 118.0(9) . . ? N41A C41A C40A 117.8(9) . . ? N41A C42A C44A 113.1(8) . . ? N41A C42A C43A 106.1(9) . . ? C44A C42A C43A 112.2(9) . . ? C45A C44A C49A 119.9(10) . . ? C45A C44A C42A 121.6(10) . . ? C49A C44A C42A 118.5(10) . . ? C44A C45A C46A 121.4(11) . . ? C47A C46A C45A 118.9(11) . . ? C46A C47A C48A 119.3(10) . . ? C49A C48A C47A 119.0(10) . . ? C44A C49A C48A 121.3(10) . . ? O4B Gd1B O3B 84.9(3) . . ? O4B Gd1B O1B 84.5(2) . . ? O3B Gd1B O1B 145.3(2) . . ? O4B Gd1B O2B 145.3(2) . . ? O3B Gd1B O2B 83.6(3) . . ? O1B Gd1B O2B 86.6(3) . . ? O4B Gd1B O5B 73.6(3) . . ? O3B Gd1B O5B 72.6(2) . . ? O1B Gd1B O5B 72.8(3) . . ? O2B Gd1B O5B 71.7(3) . . ? O4B Gd1B N2B 140.7(3) . . ? O3B Gd1B N2B 131.0(3) . . ? O1B Gd1B N2B 73.0(3) . . ? O2B Gd1B N2B 66.3(3) . . ? O5B Gd1B N2B 126.4(3) . . ? O4B Gd1B N3B 130.2(2) . . ? O3B Gd1B N3B 65.7(2) . . ? O1B Gd1B N3B 141.3(3) . . ? O2B Gd1B N3B 72.9(3) . . ? O5B Gd1B N3B 127.2(3) . . ? N2B Gd1B N3B 68.8(3) . . ? O4B Gd1B N1B 73.0(3) . . ? O3B Gd1B N1B 140.2(3) . . ? O1B Gd1B N1B 66.0(3) . . ? O2B Gd1B N1B 132.3(3) . . ? O5B Gd1B N1B 128.5(3) . . ? N2B Gd1B N1B 68.6(3) . . ? N3B Gd1B N1B 104.3(3) . . ? O4B Gd1B N4B 65.6(3) . . ? O3B Gd1B N4B 73.9(3) . . ? O1B Gd1B N4B 129.7(3) . . ? O2B Gd1B N4B 140.1(3) . . ? O5B Gd1B N4B 128.6(3) . . ? N2B Gd1B N4B 105.0(3) . . ? N3B Gd1B N4B 68.0(3) . . ? N1B Gd1B N4B 66.9(2) . . ? C11B O1B Gd1B 125.6(7) . . ? C21B O2B Gd1B 122.2(8) . . ? C31B O3B Gd1B 124.8(7) . . ? C41B O4B Gd1B 124.9(7) . . ? C8B N1B C10B 110.9(9) . . ? C8B N1B C1B 109.2(8) . . ? C10B N1B C1B 109.2(8) . . ? C8B N1B Gd1B 112.1(6) . . ? C10B N1B Gd1B 106.0(6) . . ? C1B N1B Gd1B 109.4(7) . . ? C3B N2B C20B 110.7(9) . . ? C3B N2B C2B 107.1(9) . . ? C20B N2B C2B 109.4(9) . . ? C3B N2B Gd1B 111.9(6) . . ? C20B N2B Gd1B 106.7(6) . . ? C2B N2B Gd1B 111.1(7) . . ? C30B N3B C5B 111.4(8) . . ? C30B N3B C4B 109.4(8) . . ? C5B N3B C4B 108.1(8) . . ? C30B N3B Gd1B 106.4(6) . . ? C5B N3B Gd1B 111.0(6) . . ? C4B N3B Gd1B 110.5(6) . . ? C40B N4B C7B 111.4(9) . . ? C40B N4B C6B 110.9(7) . . ? C7B N4B C6B 107.6(8) . . ? C40B N4B Gd1B 106.6(6) . . ? C7B N4B Gd1B 110.6(6) . . ? C6B N4B Gd1B 109.7(6) . . ? C11B N11B C12B 121.0(10) . . ? C21B N21B C22B 122.2(10) . . ? C31B N31B C32B 121.4(10) . . ? C41B N41B C42B 122.0(9) . . ? C2B C1B N1B 115.2(9) . . ? C1B C2B N2B 112.2(9) . . ? N2B C3B C4B 113.3(9) . . ? N3B C4B C3B 111.5(9) . . ? N3B C5B C6B 113.1(9) . . ? N4B C6B C5B 112.4(8) . . ? N4B C7B C8B 113.0(9) . . ? N1B C8B C7B 113.0(9) . . ? N1B C10B C11B 112.2(9) . . ? O1B C11B N11B 122.9(11) . . ? O1B C11B C10B 118.5(10) . . ? N11B C11B C10B 118.6(10) . . ? N11B C12B C14B 111.9(10) . . ? N11B C12B C13B 108.3(11) . . ? C14B C12B C13B 112.1(9) . . ? C19B C14B C15B 119.3(13) . . ? C19B C14B C12B 123.1(13) . . ? C15B C14B C12B 117.6(13) . . ? C16B C15B C14B 117.1(17) . . ? C15B C16B C17B 120.3(18) . . ? C18B C17B C16B 121.6(17) . . ? C19B C18B C17B 117.8(18) . . ? C18B C19B C14B 123.7(17) . . ? N2B C20B C21B 109.6(9) . . ? O2B C21B N21B 120.4(12) . . ? O2B C21B C20B 122.1(11) . . ? N21B C21B C20B 117.5(10) . . ? N21B C22B C24B 111.9(10) . . ? N21B C22B C23B 110.2(11) . . ? C24B C22B C23B 112.1(13) . . ? C25B C24B C29B 118.2(16) . . ? C25B C24B C22B 121.3(13) . . ? C29B C24B C22B 120.5(15) . . ? C26B C25B C24B 120.0(16) . . ? C25B C26B C27B 118.8(18) . . ? C28B C27B C26B 126(2) . . ? C27B C28B C29B 111.3(17) . . ? C24B C29B C28B 126(2) . . ? N3B C30B C31B 111.6(8) . . ? O3B C31B N31B 122.6(10) . . ? O3B C31B C30B 119.2(10) . . ? N31B C31B C30B 117.9(10) . . ? N31B C32B C33B 107.4(9) . . ? N31B C32B C34B 108.5(9) . . ? C33B C32B C34B 113.7(9) . . ? C35B C34B C39B 114.8(12) . . ? C35B C34B C32B 125.0(11) . . ? C39B C34B C32B 120.1(12) . . ? C34B C35B C36B 118.9(16) . . ? C37B C36B C35B 123(2) . . ? C36B C37B C38B 120.8(17) . . ? C37B C38B C39B 117.1(16) . . ? C38B C39B C34B 125.4(16) . . ? N4B C40B C41B 109.9(9) . . ? O4B C41B N41B 119.3(10) . . ? O4B C41B C40B 120.5(10) . . ? N41B C41B C40B 119.8(9) . . ? N41B C42B C44B 113.7(9) . . ? N41B C42B C43B 107.6(8) . . ? C44B C42B C43B 114.1(9) . . ? C49B C44B C45B 116.8(10) . . ? C49B C44B C42B 123.0(10) . . ? C45B C44B C42B 120.2(10) . . ? C46B C45B C44B 119.2(11) . . ? C45B C46B C47B 124.2(12) . . ? C46B C47B C48B 116.9(10) . . ? C49B C48B C47B 120.6(10) . . ? C48B C49B C44B 122.0(11) . . ? O13 S1 O11 114.0(6) . . ? O13 S1 O12 115.6(5) . . ? O11 S1 O12 115.2(5) . . ? O13 S1 C1S 102.6(6) . . ? O11 S1 C1S 105.0(7) . . ? O12 S1 C1S 102.0(6) . . ? F11 C1S F12 108.6(14) . . ? F11 C1S F13 109.6(14) . . ? F12 C1S F13 107.4(13) . . ? F11 C1S S1 112.1(12) . . ? F12 C1S S1 111.2(10) . . ? F13 C1S S1 107.8(11) . . ? O23 S2 O21 115.8(6) . . ? O23 S2 O22 115.0(6) . . ? O21 S2 O22 113.7(6) . . ? O23 S2 C2S 100.9(6) . . ? O21 S2 C2S 104.3(6) . . ? O22 S2 C2S 104.8(5) . . ? F21 C2S F23 108.6(9) . . ? F21 C2S F22 108.5(9) . . ? F23 C2S F22 104.6(10) . . ? F21 C2S S2 113.1(9) . . ? F23 C2S S2 110.8(8) . . ? F22 C2S S2 111.0(8) . . ? O33 S3 O31 118.1(6) . . ? O33 S3 O32 113.4(6) . . ? O31 S3 O32 113.9(5) . . ? O33 S3 C3S 102.1(6) . . ? O31 S3 C3S 102.4(6) . . ? O32 S3 C3S 104.5(6) . . ? F31 C3S F33 106.0(11) . . ? F31 C3S F32 108.4(11) . . ? F33 C3S F32 108.2(12) . . ? F31 C3S S3 112.0(9) . . ? F33 C3S S3 112.6(9) . . ? F32 C3S S3 109.4(9) . . ? O41 S4 O42 116.4(7) . . ? O41 S4 O43 114.2(7) . . ? O42 S4 O43 115.0(7) . . ? O41 S4 C4S 102.7(8) . . ? O42 S4 C4S 102.9(8) . . ? O43 S4 C4S 103.1(9) . . ? F41 C4S F42 108.7(19) . . ? F41 C4S F43 110.8(14) . . ? F42 C4S F43 105.6(16) . . ? F41 C4S S4 113.2(13) . . ? F42 C4S S4 109.9(11) . . ? F43 C4S S4 108.5(15) . . ? O53 S5 O52 124.7(18) . . ? O53 S5 O51 111.2(18) . . ? O52 S5 O51 118.1(8) . . ? O53 S5 C5S 99.8(18) . . ? O52 S5 C5S 98.7(12) . . ? O51 S5 C5S 95.9(11) . . ? F52 C5S F51 113(3) . . ? F52 C5S F53 112(3) . . ? F51 C5S F53 110(3) . . ? F52 C5S S5 108(3) . . ? F51 C5S S5 106(3) . . ? F53 C5S S5 108(3) . . ? O62 S6 O61 118.7(7) . . ? O62 S6 O63 112.2(9) . . ? O61 S6 O63 114.6(7) . . ? O62 S6 C6S 104.9(7) . . ? O61 S6 C6S 101.2(6) . . ? O63 S6 C6S 102.6(9) . . ? F62 C6S F61 107.6(14) . . ? F62 C6S F63 109.8(13) . . ? F61 C6S F63 107.0(13) . . ? F62 C6S S6 111.8(11) . . ? F61 C6S S6 110.0(10) . . ? F63 C6S S6 110.5(11) . . ? C7S O1S C7S' 65(3) . . ? C8S C7S O1S 110(3) . . ? C8S C7S C7S' 57(3) . . ? O1S C7S C7S' 56(3) . . ? C8S C7S' O1S 112(6) . . ? C8S C7S' C7S 57(3) . . ? O1S C7S' C7S 59(3) . . ? C7S' C8S C7S 66(3) . . ? O3S C11S C12S 103(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11A H11A O23 0.87 1.98 2.848(13) 169.4 2_646 N21A H21A O61 0.87 2.07 2.920(12) 164.5 1_545 N31A H31A O12 0.87 2.05 2.853(11) 151.6 4 N41A H41A O31 0.87 2.03 2.889(11) 167.8 3_554 O5A H01A O41 0.83 2.03 2.865(11) 175.7 . O5A H02A O1S 0.83 1.95 2.782(13) 178.1 . N11B H11B O21 0.87 2.11 2.968(14) 169.0 . N21B H21B O32 0.87 2.01 2.869(13) 169.3 . N31B H31B O13 0.87 2.01 2.865(13) 166.0 . N41B H41B O62 0.87 2.14 2.912(15) 146.9 . O5B H01B O52 0.71 2.17 2.887(14) 175.4 . O5B H02B O2S 0.67 1.91 2.58(3) 173.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.914 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.169 #===============================================END data_9d _database_code_CSD 182454 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 Er N8 O5 3+,3(C F3 O3 S 1-),C2 H6 O,2(H2 O)' _chemical_formula_sum 'C53 H76 Er F9 N8 O17 S3' _chemical_formula_weight 1531.66 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 32.134(8) _cell_length_b 12.697(4) _cell_length_c 32.738(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.54(1) _cell_angle_gamma 90.00 _cell_volume 13332(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8628 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.62 _exptl_crystal_description 'plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6264 _exptl_absorpt_coefficient_mu 1.448 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5242 _exptl_absorpt_correction_T_max 0.9042 _exptl_absorpt_process_details 'XPREP (SHELXTL), R(int)=0.070 before correction' _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (15 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 81447 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.62 _reflns_number_total 33972 _reflns_number_gt 30161 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. Triflate anion containing S(4) is disordered between 2 positions with occupancies 78.5(5)% (unprimed) and 21.5(5)% primed. Triflate anion containing S(6) is disordered between 2 positions with occupancies 76.0(8)% (unprimed) and 24.0(8)% primed, for C(6S), F(61), F(63), O(61) the positions were not resolved. Triflate anion containing S(5) has the CF~3~ disordered equally between two positions (differing by libration around the S(5) atom), individual positions of oxygen atoms were resolved only for O(53). Ethanol and water of crystallisation show complicated disorder and non-stoichemetric occupancies. ; _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^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(4) _refine_ls_number_reflns 33972 _refine_ls_number_parameters 1655 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.240 _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 Er1A Er 0.503709(5) 0.374112(14) 0.299233(5) 0.01794(4) Uani 1 1 d . . . O1A O 0.53977(9) 0.2552(2) 0.34123(10) 0.0235(6) Uani 1 1 d . . . O2A O 0.44890(9) 0.3441(2) 0.34212(10) 0.0209(6) Uani 1 1 d . . . O3A O 0.47907(9) 0.5442(2) 0.29645(10) 0.0221(6) Uani 1 1 d . . . O4A O 0.56945(9) 0.4542(2) 0.29352(10) 0.0225(6) Uani 1 1 d . . . O5A O 0.52283(10) 0.4558(3) 0.36286(10) 0.0277(7) Uani 1 1 d . . . H01A H 0.5430 0.4350 0.3781 0.042 Uiso 1 1 d R . . H02A H 0.5224 0.5205 0.3676 0.042 Uiso 1 1 d R . . N1A N 0.54929(11) 0.2378(3) 0.25818(12) 0.0223(7) Uani 1 1 d . . . N2A N 0.46558(11) 0.1891(3) 0.28646(12) 0.0207(7) Uani 1 1 d . . . N3A N 0.43308(11) 0.3937(3) 0.25349(11) 0.0209(8) Uani 1 1 d . . . N4A N 0.51636(11) 0.4429(3) 0.22388(11) 0.0204(7) Uani 1 1 d . . . N11A N 0.58714(12) 0.1284(4) 0.35703(12) 0.0339(9) Uani 1 1 d . . . H11A H 0.6036 0.0804 0.3474 0.041 Uiso 1 1 d R . . N21A N 0.39943(11) 0.2413(3) 0.36942(12) 0.0238(8) Uani 1 1 d . . . H21A H 0.3865 0.1806 0.3672 0.029 Uiso 1 1 d R . . N31A N 0.43140(11) 0.6708(3) 0.28190(12) 0.0207(7) Uani 1 1 d . . . H31A H 0.4069 0.6856 0.2700 0.025 Uiso 1 1 d R . . N41A N 0.61687(11) 0.5485(3) 0.25999(12) 0.0247(8) Uani 1 1 d . . . H41A H 0.6227 0.5746 0.2364 0.030 Uiso 1 1 d R . . C1A C 0.52416(14) 0.1451(3) 0.24328(14) 0.0257(9) Uani 1 1 d . . . H11 H 0.5421 0.0864 0.2353 0.031 Uiso 1 1 d R . . H12 H 0.5079 0.1693 0.2186 0.031 Uiso 1 1 d R . . C2A C 0.49486(14) 0.1047(3) 0.27491(14) 0.0236(9) Uani 1 1 d . . . H21 H 0.5109 0.0791 0.2995 0.028 Uiso 1 1 d R . . H22 H 0.4785 0.0453 0.2630 0.028 Uiso 1 1 d R . . C3A C 0.43050(14) 0.1986(3) 0.25429(14) 0.0244(9) Uani 1 1 d . . . H31 H 0.4427 0.1931 0.2276 0.029 Uiso 1 1 d R . . H32 H 0.4104 0.1403 0.2563 0.029 Uiso 1 1 d R . . C4A C 0.40574(13) 0.2994(3) 0.25668(14) 0.0207(8) Uani 1 1 d . . . H41 H 0.3915 0.3019 0.2824 0.025 Uiso 1 1 d R . . H42 H 0.3840 0.3015 0.2341 0.025 Uiso 1 1 d R . . C5A C 0.44072(14) 0.4094(4) 0.20891(14) 0.0246(9) Uani 1 1 d . . . H51 H 0.4161 0.4405 0.1941 0.030 Uiso 1 1 d R . . H52 H 0.4458 0.3400 0.1968 0.030 Uiso 1 1 d R . . C6A C 0.47719(13) 0.4833(4) 0.20270(14) 0.0239(9) Uani 1 1 d . . . H61 H 0.4815 0.4901 0.1734 0.029 Uiso 1 1 d R . . H62 H 0.4711 0.5540 0.2132 0.029 Uiso 1 1 d R . . C7A C 0.53455(14) 0.3574(4) 0.19875(13) 0.0249(9) Uani 1 1 d . . . H71 H 0.5475 0.3861 0.1747 0.030 Uiso 1 1 d R . . H72 H 0.5109 0.3125 0.1890 0.030 Uiso 1 1 d R . . C8A C 0.56703(14) 0.2893(4) 0.22240(14) 0.0244(9) Uani 1 1 d . . . H81 H 0.5781 0.2363 0.2040 0.029 Uiso 1 1 d R . . H82 H 0.5905 0.3338 0.2327 0.029 Uiso 1 1 d R . . C10A C 0.58357(14) 0.2022(4) 0.28805(14) 0.0261(9) Uani 1 1 d . . . H101 H 0.6075 0.2509 0.2881 0.031 Uiso 1 1 d R . . H102 H 0.5930 0.1329 0.2786 0.031 Uiso 1 1 d R . . C11A C 0.56823(14) 0.1955(4) 0.33095(15) 0.0258(9) Uani 1 1 d . . . C12A C 0.57873(14) 0.1304(6) 0.40060(15) 0.0376(11) Uani 1 1 d . . . H12A H 0.5806 0.2049 0.4104 0.045 Uiso 1 1 calc R . . C13A C 0.6129(2) 0.0651(9) 0.4246(2) 0.084(3) Uani 1 1 d . . . H131 H 0.6405 0.0914 0.4183 0.125 Uiso 1 1 calc R . . H132 H 0.6103 -0.0091 0.4166 0.125 Uiso 1 1 calc R . . H133 H 0.6095 0.0718 0.4540 0.125 Uiso 1 1 calc R . . C14A C 0.53542(15) 0.0878(4) 0.40834(15) 0.0293(10) Uani 1 1 d . . . C15A C 0.5225(2) -0.0120(5) 0.3953(2) 0.0477(15) Uani 1 1 d . . . H15A H 0.5390 -0.0576 0.3802 0.057 Uiso 1 1 d R . . C16A C 0.4829(3) -0.0498(6) 0.4039(2) 0.071(3) Uani 1 1 d . . . H16A H 0.4711 -0.1138 0.3939 0.085 Uiso 1 1 d R . . C17A C 0.4571(2) 0.0160(9) 0.4264(3) 0.078(3) Uani 1 1 d . . . H17A H 0.4298 -0.0036 0.4331 0.094 Uiso 1 1 d R . . C18A C 0.4700(2) 0.1107(8) 0.4397(2) 0.065(2) Uani 1 1 d . . . H18A H 0.4532 0.1580 0.4537 0.078 Uiso 1 1 d R . . C19A C 0.50888(18) 0.1479(5) 0.43035(18) 0.0447(14) Uani 1 1 d . . . H19A H 0.5206 0.2112 0.4410 0.054 Uiso 1 1 d R . . C20A C 0.44849(13) 0.1598(3) 0.32620(14) 0.0221(8) Uani 1 1 d . . . H201 H 0.4698 0.1253 0.3445 0.026 Uiso 1 1 d R . . H202 H 0.4258 0.1088 0.3199 0.026 Uiso 1 1 d R . . C21A C 0.43167(12) 0.2565(3) 0.34651(13) 0.0188(8) Uani 1 1 d . . . C22A C 0.38385(15) 0.3262(4) 0.39582(14) 0.0271(9) Uani 1 1 d . . . H22A H 0.4076 0.3558 0.4131 0.032 Uiso 1 1 d R . . C23A C 0.35435(19) 0.2750(5) 0.42577(18) 0.0424(14) Uani 1 1 d . . . H231 H 0.3691 0.2182 0.4409 0.064 Uiso 1 1 calc R . . H232 H 0.3299 0.2462 0.4103 0.064 Uiso 1 1 calc R . . H233 H 0.3454 0.3282 0.4451 0.064 Uiso 1 1 calc R . . C24A C 0.36152(14) 0.4128(4) 0.37058(15) 0.0264(9) Uani 1 1 d . . . C25A C 0.32918(15) 0.3898(4) 0.34172(16) 0.0328(11) Uani 1 1 d . . . H25A H 0.3195 0.3205 0.3363 0.039 Uiso 1 1 d R . . C26A C 0.30884(19) 0.4718(5) 0.31925(19) 0.0444(14) Uani 1 1 d . . . H26A H 0.2869 0.4590 0.2994 0.053 Uiso 1 1 d R . . C27A C 0.3213(2) 0.5749(5) 0.3257(2) 0.0456(15) Uani 1 1 d . . . H27A H 0.3089 0.6309 0.3103 0.055 Uiso 1 1 d R . . C28A C 0.35357(19) 0.5978(4) 0.35419(19) 0.0408(14) Uani 1 1 d . . . H28A H 0.3620 0.6681 0.3597 0.049 Uiso 1 1 d R . . C29A C 0.37387(17) 0.5175(4) 0.37638(16) 0.0333(11) Uani 1 1 d . . . H29A H 0.3964 0.5314 0.3955 0.040 Uiso 1 1 d R . . C30A C 0.41211(13) 0.4883(3) 0.26947(14) 0.0219(9) Uani 1 1 d . . . H301 H 0.3950 0.4676 0.2921 0.026 Uiso 1 1 d R . . H302 H 0.3932 0.5162 0.2473 0.026 Uiso 1 1 d R . . C31A C 0.44358(13) 0.5711(4) 0.28303(14) 0.0214(9) Uani 1 1 d . . . C32A C 0.45847(13) 0.7559(3) 0.29801(15) 0.0234(9) Uani 1 1 d . . . H32A H 0.4714 0.7328 0.3248 0.028 Uiso 1 1 d R . . C33A C 0.43132(15) 0.8523(3) 0.30680(17) 0.0303(10) Uani 1 1 d . . . H331 H 0.4100 0.8337 0.3255 0.045 Uiso 1 1 d R . . H332 H 0.4179 0.8761 0.2810 0.045 Uiso 1 1 d R . . H333 H 0.4488 0.9086 0.3186 0.045 Uiso 1 1 d R . . C34A C 0.49216(15) 0.7845(3) 0.26877(17) 0.0290(10) Uani 1 1 d . . . C35A C 0.48166(18) 0.7969(4) 0.2275(2) 0.0398(13) Uani 1 1 d . . . H35A H 0.4544 0.7868 0.2154 0.048 Uiso 1 1 d R . . C36A C 0.5128(2) 0.8252(5) 0.2009(2) 0.0520(17) Uani 1 1 d . . . H36A H 0.5089 0.8316 0.1722 0.062 Uiso 1 1 d R . . C37A C 0.5537(2) 0.8406(5) 0.2166(3) 0.064(2) Uani 1 1 d . . . H37A H 0.5758 0.8588 0.2002 0.077 Uiso 1 1 d R . . C38A C 0.5638(2) 0.8275(5) 0.2577(3) 0.0584(19) Uani 1 1 d . . . H38A H 0.5911 0.8386 0.2695 0.070 Uiso 1 1 d R . . C39A C 0.53322(16) 0.8006(4) 0.2839(2) 0.0406(13) Uani 1 1 d . . . H39A H 0.5386 0.7921 0.3123 0.049 Uiso 1 1 d R . . C40A C 0.54642(14) 0.5315(4) 0.22869(15) 0.0258(9) Uani 1 1 d . . . H401 H 0.5322 0.5984 0.2342 0.031 Uiso 1 1 d R . . H402 H 0.5601 0.5393 0.2028 0.031 Uiso 1 1 d R . . C41A C 0.57885(13) 0.5065(3) 0.26326(14) 0.0218(9) Uani 1 1 d . . . C42A C 0.64996(15) 0.5470(4) 0.29405(16) 0.0283(10) Uani 1 1 d . . . H42A H 0.6388 0.5827 0.3183 0.034 Uiso 1 1 calc R . . C43A C 0.68684(16) 0.6108(4) 0.28037(19) 0.0424(13) Uani 1 1 d . . . H431 H 0.6775 0.6820 0.2728 0.064 Uiso 1 1 calc R . . H432 H 0.6983 0.5765 0.2567 0.064 Uiso 1 1 calc R . . H433 H 0.7084 0.6148 0.3028 0.064 Uiso 1 1 calc R . . C44A C 0.66261(14) 0.4350(4) 0.30635(15) 0.0254(9) Uani 1 1 d . . . C45A C 0.68052(14) 0.3666(5) 0.27875(15) 0.0310(10) Uani 1 1 d . . . H45A H 0.6832 0.3849 0.2512 0.037 Uiso 1 1 d R . . C46A C 0.69406(17) 0.2670(4) 0.29217(18) 0.0358(12) Uani 1 1 d . . . H46A H 0.7067 0.2203 0.2742 0.043 Uiso 1 1 d R . . C47A C 0.68949(16) 0.2351(4) 0.33192(18) 0.0365(12) Uani 1 1 d . . . H47A H 0.6967 0.1662 0.3406 0.044 Uiso 1 1 d R . . C48A C 0.67128(17) 0.3013(4) 0.35890(17) 0.0363(11) Uani 1 1 d . . . H48A H 0.6672 0.2815 0.3861 0.044 Uiso 1 1 d R . . C49A C 0.65835(15) 0.4014(4) 0.34629(16) 0.0321(11) Uani 1 1 d . . . H49A H 0.6471 0.4499 0.3645 0.039 Uiso 1 1 d R . . Er1B Er 0.198627(5) 0.623798(15) 0.493309(5) 0.02025(4) Uani 1 1 d . . . O1B O 0.18856(10) 0.7187(3) 0.55234(10) 0.0268(7) Uani 1 1 d . . . O2B O 0.14886(10) 0.5080(3) 0.51500(11) 0.0304(7) Uani 1 1 d . . . O3B O 0.16837(10) 0.5802(2) 0.42955(10) 0.0252(7) Uani 1 1 d . . . O4B O 0.20837(10) 0.7876(3) 0.46538(10) 0.0241(7) Uani 1 1 d . . . O5B O 0.13197(10) 0.7058(3) 0.48611(11) 0.0289(7) Uani 1 1 d . . . H01B H 0.1136 0.6981 0.4669 0.043 Uiso 1 1 d R . . H02B H 0.1272 0.7701 0.4897 0.043 Uiso 1 1 d R . . N1B N 0.26887(12) 0.7010(3) 0.52882(12) 0.0262(8) Uani 1 1 d . . . N2B N 0.22647(13) 0.5056(3) 0.55539(12) 0.0265(8) Uani 1 1 d . . . N3B N 0.21864(12) 0.4321(3) 0.46881(12) 0.0238(8) Uani 1 1 d . . . N4B N 0.26061(11) 0.6292(4) 0.44287(11) 0.0252(7) Uani 1 1 d . . . N11B N 0.20704(14) 0.8334(3) 0.60312(12) 0.0307(9) Uani 1 1 d . . . H11B H 0.2269 0.8740 0.6139 0.037 Uiso 1 1 d R . . N21B N 0.11962(14) 0.4100(4) 0.56312(15) 0.0396(11) Uani 1 1 d . . . H21B H 0.1239 0.3761 0.5862 0.048 Uiso 1 1 d R . . N31B N 0.14780(13) 0.4680(3) 0.37877(12) 0.0284(8) Uani 1 1 d . . . H31B H 0.1526 0.4068 0.3677 0.034 Uiso 1 1 d R . . N41B N 0.23299(12) 0.9050(3) 0.42115(12) 0.0260(8) Uani 1 1 d . . . H41B H 0.2499 0.9163 0.4016 0.031 Uiso 1 1 d R . . C1B C 0.28869(14) 0.6223(5) 0.55827(14) 0.0310(9) Uani 1 1 d . . . H1BB H 0.3081 0.6578 0.5783 0.037 Uiso 1 1 d R . . H1BC H 0.3052 0.5729 0.5426 0.037 Uiso 1 1 d R . . C2B C 0.25809(16) 0.5639(4) 0.58240(15) 0.0303(10) Uani 1 1 d . . . H2BA H 0.2730 0.5128 0.6005 0.036 Uiso 1 1 d R . . H2BB H 0.2429 0.6126 0.5996 0.036 Uiso 1 1 d R . . C3B C 0.24616(15) 0.4070(4) 0.54100(15) 0.0287(10) Uani 1 1 d . . . H3BA H 0.2467 0.3545 0.5631 0.034 Uiso 1 1 d R . . H3BB H 0.2754 0.4216 0.5352 0.034 Uiso 1 1 d R . . C4B C 0.22239(15) 0.3568(4) 0.50423(14) 0.0285(10) Uani 1 1 d . . . H4BA H 0.2383 0.2945 0.4962 0.034 Uiso 1 1 d R . . H4BB H 0.1942 0.3334 0.5105 0.034 Uiso 1 1 d R . . C5B C 0.25930(15) 0.4335(4) 0.44811(15) 0.0273(10) Uani 1 1 d . . . H5BA H 0.2625 0.3695 0.4316 0.033 Uiso 1 1 d R . . H5BB H 0.2822 0.4343 0.4695 0.033 Uiso 1 1 d R . . C6B C 0.26284(16) 0.5279(4) 0.41959(15) 0.0275(10) Uani 1 1 d . . . H6BA H 0.2895 0.5236 0.4062 0.033 Uiso 1 1 d R . . H6BB H 0.2400 0.5268 0.3981 0.033 Uiso 1 1 d R . . C7B C 0.30152(14) 0.6493(4) 0.46544(15) 0.0322(11) Uani 1 1 d . . . H7BA H 0.3229 0.6729 0.4472 0.039 Uiso 1 1 d R . . H7BB H 0.3106 0.5809 0.4770 0.039 Uiso 1 1 d R . . C8B C 0.29934(14) 0.7307(5) 0.49849(16) 0.0332(11) Uani 1 1 d . . . H8BA H 0.3273 0.7385 0.5123 0.040 Uiso 1 1 d R . . H8BB H 0.2913 0.7996 0.4866 0.040 Uiso 1 1 d R . . C10B C 0.25656(15) 0.7966(4) 0.55122(14) 0.0276(10) Uani 1 1 d . . . H10D H 0.2781 0.8116 0.5731 0.033 Uiso 1 1 d R . . H10E H 0.2549 0.8575 0.5326 0.033 Uiso 1 1 d R . . C11B C 0.21481(16) 0.7800(4) 0.56903(15) 0.0290(10) Uani 1 1 d . . . C12B C 0.16635(17) 0.8252(4) 0.62208(16) 0.0338(11) Uani 1 1 d . . . H12B H 0.1429 0.8368 0.6012 0.041 Uiso 1 1 d R . . C13B C 0.1631(2) 0.9147(4) 0.65212(19) 0.0442(14) Uani 1 1 d . . . H13D H 0.1370 0.9111 0.6659 0.066 Uiso 1 1 d R . . H13E H 0.1649 0.9824 0.6383 0.066 Uiso 1 1 d R . . H13F H 0.1867 0.9072 0.6721 0.066 Uiso 1 1 d R . . C14B C 0.16135(19) 0.7184(4) 0.64196(16) 0.0368(12) Uani 1 1 d . . . C15B C 0.1937(2) 0.6771(5) 0.66789(17) 0.0464(15) Uani 1 1 d . . . H15B H 0.2197 0.7123 0.6715 0.056 Uiso 1 1 d R . . C16B C 0.1878(3) 0.5819(6) 0.6881(2) 0.064(2) Uani 1 1 d . . . H16B H 0.2097 0.5518 0.7049 0.077 Uiso 1 1 d R . . C17B C 0.1490(3) 0.5299(6) 0.6827(2) 0.064(2) Uani 1 1 d . . . H17B H 0.1463 0.4641 0.6957 0.077 Uiso 1 1 d R . . C18B C 0.1185(3) 0.5682(6) 0.6568(2) 0.061(2) Uani 1 1 d . . . H18B H 0.0928 0.5316 0.6538 0.073 Uiso 1 1 d R . . C19B C 0.1246(2) 0.6629(5) 0.6362(2) 0.0463(14) Uani 1 1 d . . . H19B H 0.1026 0.6897 0.6187 0.056 Uiso 1 1 d R . . C20B C 0.18956(16) 0.4818(4) 0.57873(14) 0.0304(10) Uani 1 1 d . . . H20D H 0.1844 0.5401 0.5975 0.036 Uiso 1 1 d R . . H20E H 0.1959 0.4181 0.5951 0.036 Uiso 1 1 d R . . C21B C 0.15069(15) 0.4657(4) 0.55037(16) 0.0305(10) Uani 1 1 d . . . C22B C 0.08011(16) 0.3986(5) 0.5385(2) 0.0460(15) Uani 1 1 d . . . H22B H 0.0677 0.4689 0.5319 0.055 Uiso 1 1 d R . . C23B C 0.0479(2) 0.3485(7) 0.5654(3) 0.069(2) Uani 1 1 d . . . H23D H 0.0440 0.3877 0.5904 0.103 Uiso 1 1 d R . . H23E H 0.0609 0.2808 0.5721 0.103 Uiso 1 1 d R . . H23F H 0.0208 0.3370 0.5509 0.103 Uiso 1 1 d R . . C24B C 0.08549(18) 0.3346(5) 0.5001(2) 0.0451(14) Uani 1 1 d . . . C25B C 0.10423(19) 0.2352(6) 0.5026(2) 0.0512(16) Uani 1 1 d . . . H25B H 0.1146 0.2062 0.5277 0.061 Uiso 1 1 d R . . C26B C 0.1082(2) 0.1777(6) 0.4667(2) 0.0579(18) Uani 1 1 d . . . H26B H 0.1221 0.1120 0.4671 0.070 Uiso 1 1 d R . . C27B C 0.0933(2) 0.2161(7) 0.4296(2) 0.064(2) Uani 1 1 d . . . H27B H 0.0964 0.1797 0.4049 0.077 Uiso 1 1 d R . . C28B C 0.0745(2) 0.3125(8) 0.4274(2) 0.069(2) Uani 1 1 d . . . H28B H 0.0637 0.3406 0.4023 0.082 Uiso 1 1 d R . . C29B C 0.07064(17) 0.3740(7) 0.4618(2) 0.0549(16) Uani 1 1 d . . . H29B H 0.0574 0.4406 0.4616 0.066 Uiso 1 1 d R . . C30B C 0.18462(15) 0.3969(3) 0.43925(14) 0.0270(10) Uani 1 1 d . . . H30D H 0.1624 0.3645 0.4545 0.032 Uiso 1 1 d R . . H30E H 0.1954 0.3427 0.4211 0.032 Uiso 1 1 d R . . C31B C 0.16683(14) 0.4889(4) 0.41450(14) 0.0244(9) Uani 1 1 d . . . C32B C 0.12245(15) 0.5495(4) 0.35613(14) 0.0271(9) Uani 1 1 d . . . H32B H 0.1027 0.5814 0.3749 0.032 Uiso 1 1 d R . . C33B C 0.0947(2) 0.4928(5) 0.32317(18) 0.0440(14) Uani 1 1 d . . . H33D H 0.0780 0.4375 0.3348 0.066 Uiso 1 1 d R . . H33E H 0.1133 0.4617 0.3041 0.066 Uiso 1 1 d R . . H33F H 0.0763 0.5437 0.3089 0.066 Uiso 1 1 d R . . C34B C 0.14966(15) 0.6354(4) 0.33953(14) 0.0306(10) Uani 1 1 d . . . C35B C 0.1798(2) 0.6116(6) 0.31192(17) 0.0504(15) Uani 1 1 d . . . H35B H 0.1843 0.5417 0.3032 0.061 Uiso 1 1 d R . . C36B C 0.2030(3) 0.6972(10) 0.2982(3) 0.084(3) Uani 1 1 d . . . H36B H 0.2252 0.6838 0.2812 0.101 Uiso 1 1 d R . . C37B C 0.1990(3) 0.7953(9) 0.3092(3) 0.095(4) Uani 1 1 d . . . H37B H 0.2137 0.8526 0.2985 0.114 Uiso 1 1 d R . . C38B C 0.1692(3) 0.8192(5) 0.3355(3) 0.067(2) Uani 1 1 d . . . H38B H 0.1659 0.8890 0.3448 0.080 Uiso 1 1 d R . . C39B C 0.1445(2) 0.7391(4) 0.35101(19) 0.0433(14) Uani 1 1 d . . . H39B H 0.1239 0.7554 0.3694 0.052 Uiso 1 1 d R . . C40B C 0.25058(15) 0.7187(4) 0.41345(15) 0.0273(10) Uani 1 1 d . . . H40D H 0.2314 0.6940 0.3909 0.033 Uiso 1 1 d R . . H40E H 0.2767 0.7417 0.4018 0.033 Uiso 1 1 d R . . C41B C 0.22994(14) 0.8074(4) 0.43515(14) 0.0240(9) Uani 1 1 d . . . C42B C 0.20847(14) 0.9923(4) 0.43867(15) 0.0252(9) Uani 1 1 d . . . H42B H 0.1804 0.9643 0.4448 0.030 Uiso 1 1 calc R . . C43B C 0.20243(17) 1.0786(4) 0.40663(16) 0.0343(11) Uani 1 1 d . . . H43D H 0.1891 1.0488 0.3818 0.051 Uiso 1 1 d R . . H43E H 0.2299 1.1062 0.4010 0.051 Uiso 1 1 d R . . H43F H 0.1851 1.1355 0.4163 0.051 Uiso 1 1 d R . . C44B C 0.22976(15) 1.0335(4) 0.47800(14) 0.0256(9) Uani 1 1 d . . . C45B C 0.27086(15) 1.0703(4) 0.47946(16) 0.0289(10) Uani 1 1 d . . . H45B H 0.2866 1.0662 0.4561 0.035 Uiso 1 1 d R . . C46B C 0.28934(16) 1.1123(5) 0.51564(16) 0.0375(11) Uani 1 1 d . . . H46B H 0.3169 1.1391 0.5164 0.045 Uiso 1 1 d R . . C47B C 0.26728(18) 1.1166(5) 0.55125(15) 0.0384(12) Uani 1 1 d . . . H47B H 0.2797 1.1425 0.5761 0.046 Uiso 1 1 d R . . C48B C 0.22652(18) 1.0823(4) 0.54961(16) 0.0354(12) Uani 1 1 d . . . H48B H 0.2111 1.0839 0.5732 0.042 Uiso 1 1 d R . . C49B C 0.20800(16) 1.0408(4) 0.51369(15) 0.0309(10) Uani 1 1 d . . . H49B H 0.1801 1.0162 0.5131 0.037 Uiso 1 1 d R . . S1 S 0.15352(4) 0.20720(10) 0.30878(4) 0.0298(2) Uani 1 1 d . . . O11 O 0.15188(18) 0.0948(3) 0.30975(15) 0.0616(14) Uani 1 1 d . . . O12 O 0.12986(13) 0.2570(3) 0.27503(13) 0.0452(10) Uani 1 1 d . . . O13 O 0.14949(13) 0.2570(3) 0.34786(12) 0.0391(9) Uani 1 1 d . . . C1S C 0.2071(2) 0.2401(7) 0.2984(2) 0.0570(19) Uani 1 1 d . . . F11 F 0.21674(19) 0.2005(8) 0.26346(16) 0.138(3) Uani 1 1 d . . . F12 F 0.23393(12) 0.2007(5) 0.32691(14) 0.0795(15) Uani 1 1 d . . . F13 F 0.21209(13) 0.3448(5) 0.29684(18) 0.098(2) Uani 1 1 d . . . S2 S 0.31497(4) 0.91186(11) 0.65765(4) 0.0360(3) Uani 1 1 d . . . O21 O 0.28098(14) 0.9583(3) 0.63318(12) 0.0429(9) Uani 1 1 d . . . O22 O 0.32227(14) 0.8019(4) 0.64934(14) 0.0508(11) Uani 1 1 d . . . O23 O 0.35185(15) 0.9750(4) 0.66366(18) 0.0663(14) Uani 1 1 d . . . C2S C 0.29602(18) 0.9114(4) 0.70865(17) 0.0364(12) Uani 1 1 d . . . F21 F 0.32568(11) 0.8809(3) 0.73679(11) 0.0537(9) Uani 1 1 d . . . F22 F 0.26332(10) 0.8469(3) 0.71168(11) 0.0482(9) Uani 1 1 d . . . F23 F 0.28317(14) 1.0079(3) 0.71920(11) 0.0575(10) Uani 1 1 d . . . S3 S 0.14023(4) 0.20685(10) 0.64696(4) 0.0336(3) Uani 1 1 d . . . O31 O 0.12425(12) 0.1494(3) 0.68043(12) 0.0380(9) Uani 1 1 d . . . O32 O 0.12613(13) 0.3155(3) 0.64336(12) 0.0408(9) Uani 1 1 d . . . O33 O 0.14053(13) 0.1528(3) 0.60824(13) 0.0445(10) Uani 1 1 d . . . C3S C 0.19574(17) 0.2188(4) 0.66208(19) 0.0385(12) Uani 1 1 d . . . F31 F 0.21389(10) 0.1271(3) 0.67040(12) 0.0517(8) Uani 1 1 d . . . F32 F 0.21674(11) 0.2640(3) 0.63237(13) 0.0551(10) Uani 1 1 d . . . F33 F 0.20222(13) 0.2798(4) 0.69517(13) 0.0654(11) Uani 1 1 d . . . S4 S 0.61072(5) 0.45337(16) 0.45337(5) 0.0350(5) Uani 0.785(5) 1 d P A 1 O41 O 0.59208(14) 0.3970(4) 0.41957(12) 0.0540(12) Uani 1 1 d . . . O42 O 0.64831(13) 0.4045(5) 0.47256(17) 0.0710(16) Uani 1 1 d . . . O43 O 0.6120(3) 0.5680(8) 0.4475(3) 0.060(2) Uani 0.785(5) 1 d P A 1 C4S C 0.5721(4) 0.4347(8) 0.4912(3) 0.063(3) Uani 0.785(5) 1 d P A 1 F41 F 0.5679(2) 0.3353(6) 0.5015(2) 0.075(2) Uani 0.785(5) 1 d P A 1 F42 F 0.5350(2) 0.4669(7) 0.4765(3) 0.114(3) Uani 0.785(5) 1 d P A 1 F43 F 0.5826(4) 0.4849(6) 0.52542(18) 0.129(4) Uani 0.785(5) 1 d P A 1 S4' S 0.6056(2) 0.3930(6) 0.4656(2) 0.0373(19) Uiso 0.215(5) 1 d P A 2 O43' O 0.5813(11) 0.316(3) 0.4907(11) 0.066(9) Uiso 0.215(5) 1 d P A 2 C4S' C 0.5916(10) 0.526(3) 0.4814(10) 0.050(7) Uiso 0.215(5) 1 d P A 2 F41' F 0.6106(12) 0.593(3) 0.4602(11) 0.074(12) Uiso 0.215(5) 1 d P A 2 F42' F 0.5514(6) 0.5436(16) 0.4795(6) 0.053(5) Uiso 0.215(5) 1 d P A 2 F43' F 0.6059(6) 0.5314(18) 0.5218(7) 0.060(5) Uiso 0.215(5) 1 d P A 2 S5 S 0.03161(9) 0.7175(3) 0.40233(13) 0.1195(13) Uani 1 1 d . . . O51 O 0.0346(3) 0.7075(9) 0.3568(3) 0.156(4) Uani 1 1 d . B . O52 O 0.06284(17) 0.6638(6) 0.42705(18) 0.090(2) Uani 1 1 d . B . O53 O 0.0409(5) 0.8350(13) 0.4125(5) 0.107(5) Uiso 0.50 1 d P B 1 C5S C -0.0027(6) 0.5895(17) 0.3948(5) 0.099(7) Uiso 0.50 1 d PD B 1 F51 F 0.0175(5) 0.5046(13) 0.3897(5) 0.136(5) Uiso 0.50 1 d PD B 1 F52 F -0.0304(7) 0.599(2) 0.3663(6) 0.234(11) Uiso 0.50 1 d PD B 1 F53 F -0.0207(6) 0.5870(15) 0.4268(6) 0.159(7) Uiso 0.50 1 d PD B 1 O53' O -0.0034(7) 0.7839(18) 0.4050(7) 0.149(7) Uiso 0.50 1 d P B 2 C5S' C -0.0106(7) 0.7124(16) 0.4376(7) 0.101(7) Uiso 0.50 1 d PD B 2 F51' F -0.0241(7) 0.6310(16) 0.4494(7) 0.196(9) Uiso 0.50 1 d PD B 2 F52' F -0.0040(6) 0.7464(15) 0.4727(5) 0.168(7) Uiso 0.50 1 d PD . 2 F53' F -0.0433(6) 0.7610(15) 0.4315(6) 0.178(7) Uiso 0.50 1 d PD B 2 S6 S 0.33008(6) 0.9731(2) 0.35862(7) 0.0310(5) Uani 0.760(8) 1 d P C 1 O61 O 0.37069(11) 1.0215(3) 0.36628(13) 0.0410(9) Uani 1 1 d . . . O62 O 0.29646(17) 1.0198(5) 0.37961(18) 0.0493(17) Uani 0.760(8) 1 d P C 1 O63 O 0.3300(2) 0.8618(5) 0.3580(2) 0.068(2) Uani 0.760(8) 1 d P C 1 S6' S 0.3270(2) 1.0128(8) 0.3621(2) 0.0297(18) Uiso 0.240(8) 1 d P C 2 O62' O 0.3093(6) 0.9198(16) 0.3786(6) 0.053(5) Uiso 0.240(8) 1 d P C 2 O63' O 0.3050(5) 1.1049(15) 0.3741(5) 0.048(5) Uiso 0.240(8) 1 d P C 2 F62' F 0.3323(7) 0.9037(19) 0.2934(7) 0.081(7) Uiso 0.240(8) 1 d P C 2 C6S C 0.31693(18) 1.0091(6) 0.30506(19) 0.0493(16) Uani 1 1 d . . . F61 F 0.32013(16) 1.1139(4) 0.29918(14) 0.0822(13) Uani 1 1 d . C . F62 F 0.34404(17) 0.9717(6) 0.28030(15) 0.0636(19) Uani 0.760(8) 1 d P C 1 F63 F 0.27869(14) 0.9852(4) 0.29245(15) 0.0791(14) Uani 1 1 d . C . O1S O 0.52301(19) 0.6702(4) 0.38200(16) 0.0668(14) Uani 1 1 d . . . H01S H 0.5472 0.6963 0.3805 0.100 Uiso 1 1 d R . . C7S C 0.5132(6) 0.6838(15) 0.4224(6) 0.109(6) Uiso 0.67 1 d P . . C8S C 0.4683(4) 0.6644(10) 0.4299(4) 0.065(3) Uiso 0.67 1 d P . . C8S' C 0.5327(8) 0.726(2) 0.4719(8) 0.074(7) Uiso 0.33 1 d P . . O2S O 0.1075(3) 0.9085(6) 0.4898(3) 0.115(3) Uiso 1 1 d . D . H02S H 0.1001 0.8899 0.5152 0.172 Uiso 1 1 d R . . C9S C 0.0745(9) 0.921(2) 0.4619(7) 0.120(8) Uiso 0.50 1 d PD . . C10S C 0.0890(9) 0.932(2) 0.4187(8) 0.058(7) Uiso 0.25 1 d PD D 2 O3S O 0.0220(5) 0.9961(13) 0.6002(5) 0.097(4) Uiso 0.50 1 d P . . C11S C 0.0092(9) 1.077(2) 0.5875(8) 0.120(8) Uiso 0.50 1 d P . . H11C H 0.0231 1.1445 0.5934 0.156 Uiso 0.50 1 d PR . . H11D H -0.0185 1.0769 0.5992 0.156 Uiso 0.50 1 d PR . . C12S C 0.0001(8) 1.090(2) 0.5410(7) 0.112(8) Uiso 0.50 1 d P . . H12C H -0.0167 1.1459 0.5277 0.168 Uiso 0.50 1 d PR . . H12D H -0.0134 1.0223 0.5359 0.168 Uiso 0.50 1 d PR . . H12E H 0.0278 1.0896 0.5302 0.168 Uiso 0.50 1 d PR . . O1W O 0.6040(3) 0.7254(8) 0.3853(3) 0.144(3) Uiso 1 1 d . . . H1W1 H 0.6257 0.7476 0.3751 0.215 Uiso 1 1 d R . . H2W1 H 0.6147 0.6865 0.4041 0.215 Uiso 1 1 d R . . O2W O 0.0936(4) 0.9850(10) 0.5686(4) 0.074(3) Uiso 0.50 1 d P . . O3W O 0.4206(6) -0.1582(15) 0.5108(6) 0.132(6) Uiso 0.50 1 d P . . O4W O 0.4706(6) 0.4563(16) 0.4295(6) 0.108(6) Uiso 0.40 1 d P . . O5W O 0.3888(8) 0.787(2) 0.4368(8) 0.080(7) Uiso 0.25 1 d P . . O6W O 0.5000 0.774(3) 0.5000 0.086(9) Uiso 0.30 2 d SP . . O7W O 0.5000 0.344(2) 0.5000 0.047(7) Uiso 0.20 2 d SP E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1A 0.01665(8) 0.01793(8) 0.01926(8) 0.00041(8) 0.00119(6) 0.00147(7) O1A 0.0215(14) 0.0255(16) 0.0234(15) 0.0008(13) -0.0009(12) 0.0039(12) O2A 0.0188(13) 0.0174(14) 0.0263(15) -0.0001(11) 0.0011(12) -0.0005(10) O3A 0.0206(14) 0.0175(14) 0.0278(16) -0.0008(12) -0.0029(12) 0.0014(11) O4A 0.0205(14) 0.0225(15) 0.0247(16) 0.0070(13) 0.0033(12) -0.0012(12) O5A 0.0294(17) 0.0287(17) 0.0243(16) -0.0058(14) -0.0041(13) 0.0015(13) N1A 0.0227(18) 0.0211(18) 0.0233(19) 0.0006(15) 0.0043(15) 0.0027(14) N2A 0.0213(17) 0.0168(17) 0.0241(18) -0.0041(14) 0.0032(15) 0.0003(13) N3A 0.0218(16) 0.020(2) 0.0205(17) 0.0013(14) 0.0006(13) 0.0008(13) N4A 0.0183(16) 0.0248(18) 0.0183(17) 0.0059(14) 0.0022(14) 0.0001(14) N11A 0.0285(18) 0.039(2) 0.035(2) 0.013(2) 0.0027(16) 0.010(2) N21A 0.0218(18) 0.0260(19) 0.0249(18) 0.0019(15) 0.0105(15) 0.0022(14) N31A 0.0135(15) 0.0214(17) 0.0273(19) -0.0019(15) 0.0008(14) -0.0006(13) N41A 0.0196(17) 0.0261(19) 0.029(2) 0.0064(16) 0.0032(15) -0.0007(14) C1A 0.030(2) 0.019(2) 0.030(2) -0.0018(17) 0.0115(18) 0.0019(16) C2A 0.029(2) 0.010(2) 0.033(2) -0.0012(16) 0.0094(18) 0.0020(15) C3A 0.028(2) 0.019(2) 0.026(2) -0.0038(18) -0.0004(18) -0.0030(17) C4A 0.0193(19) 0.022(2) 0.021(2) -0.0023(17) -0.0012(16) -0.0036(16) C5A 0.025(2) 0.027(2) 0.021(2) 0.0007(17) -0.0016(17) -0.0012(17) C6A 0.023(2) 0.027(2) 0.021(2) 0.0049(18) -0.0017(17) 0.0034(17) C7A 0.029(2) 0.027(3) 0.0192(19) 0.0006(17) 0.0060(16) 0.0048(18) C8A 0.026(2) 0.027(2) 0.021(2) 0.0004(18) 0.0039(17) 0.0029(17) C10A 0.021(2) 0.030(2) 0.029(2) 0.0020(19) 0.0065(18) 0.0054(17) C11A 0.020(2) 0.030(2) 0.028(2) 0.0067(19) 0.0035(17) 0.0022(17) C12A 0.026(2) 0.057(3) 0.030(2) 0.006(3) -0.0013(18) -0.002(3) C13A 0.028(3) 0.171(9) 0.051(4) 0.058(5) 0.000(3) 0.012(4) C14A 0.026(2) 0.034(2) 0.028(2) 0.0108(19) -0.0029(19) 0.0003(18) C15A 0.064(4) 0.030(3) 0.048(3) 0.008(3) -0.010(3) -0.001(3) C16A 0.089(6) 0.053(4) 0.066(5) 0.026(4) -0.037(5) -0.037(4) C17A 0.038(4) 0.119(8) 0.075(6) 0.056(6) -0.010(4) -0.014(4) C18A 0.037(3) 0.103(7) 0.056(4) 0.022(5) 0.011(3) 0.004(4) C19A 0.040(3) 0.056(4) 0.038(3) 0.003(3) 0.001(2) 0.006(3) C20A 0.0210(19) 0.0195(19) 0.027(2) 0.0042(16) 0.0084(17) 0.0016(15) C21A 0.0160(18) 0.020(2) 0.0197(19) 0.0004(16) -0.0004(15) 0.0033(15) C22A 0.030(2) 0.028(2) 0.024(2) 0.0010(18) 0.0086(18) 0.0039(18) C23A 0.050(3) 0.041(3) 0.040(3) 0.015(3) 0.028(3) 0.016(3) C24A 0.026(2) 0.025(2) 0.030(2) 0.0002(18) 0.0139(19) 0.0070(17) C25A 0.030(2) 0.028(3) 0.041(3) 0.007(2) 0.004(2) 0.0065(19) C26A 0.037(3) 0.055(4) 0.041(3) 0.012(3) 0.003(2) 0.013(3) C27A 0.053(4) 0.039(3) 0.048(3) 0.020(3) 0.027(3) 0.020(3) C28A 0.049(3) 0.024(3) 0.052(3) 0.003(2) 0.026(3) 0.003(2) C29A 0.038(3) 0.029(2) 0.034(3) 0.001(2) 0.012(2) 0.003(2) C30A 0.0170(18) 0.020(2) 0.028(2) 0.0020(17) -0.0004(16) 0.0018(15) C31A 0.019(2) 0.022(2) 0.023(2) 0.0038(17) 0.0030(17) 0.0017(16) C32A 0.020(2) 0.018(2) 0.033(2) -0.0012(18) 0.0027(17) -0.0017(15) C33A 0.030(2) 0.019(2) 0.042(3) -0.0058(19) 0.010(2) 0.0006(16) C34A 0.028(2) 0.015(2) 0.045(3) 0.0047(19) 0.012(2) 0.0024(17) C35A 0.036(3) 0.031(3) 0.054(4) 0.014(3) 0.011(3) 0.009(2) C36A 0.069(4) 0.036(3) 0.054(4) 0.012(3) 0.029(3) 0.003(3) C37A 0.051(4) 0.040(3) 0.106(7) 0.007(4) 0.051(4) 0.000(3) C38A 0.040(3) 0.042(3) 0.094(6) -0.004(4) 0.020(4) -0.006(3) C39A 0.027(2) 0.027(3) 0.068(4) -0.003(3) 0.005(3) 0.000(2) C40A 0.027(2) 0.020(2) 0.031(2) 0.0067(18) -0.0003(19) 0.0028(17) C41A 0.020(2) 0.019(2) 0.027(2) 0.0018(17) 0.0002(17) 0.0015(16) C42A 0.027(2) 0.024(2) 0.033(2) -0.0020(19) -0.0062(19) -0.0009(18) C43A 0.036(3) 0.030(3) 0.060(3) 0.009(3) -0.010(2) -0.007(2) C44A 0.022(2) 0.027(2) 0.027(2) -0.0006(18) -0.0038(17) 0.0005(17) C45A 0.027(2) 0.031(2) 0.035(2) -0.002(2) -0.0013(18) 0.001(2) C46A 0.034(3) 0.028(3) 0.046(3) -0.003(2) 0.008(2) 0.007(2) C47A 0.028(2) 0.035(3) 0.046(3) 0.003(2) -0.004(2) 0.000(2) C48A 0.036(3) 0.039(3) 0.033(3) 0.006(2) -0.003(2) 0.001(2) C49A 0.029(2) 0.035(3) 0.032(2) 0.000(2) 0.002(2) 0.0009(19) Er1B 0.02036(8) 0.02251(9) 0.01794(8) 0.00136(8) 0.00163(6) 0.00318(7) O1B 0.0290(16) 0.0322(18) 0.0192(15) -0.0035(13) 0.0015(13) 0.0035(13) O2B 0.0283(17) 0.0310(18) 0.0320(18) 0.0136(15) 0.0020(14) 0.0025(14) O3B 0.0307(17) 0.0219(15) 0.0225(15) 0.0010(13) -0.0019(13) 0.0028(12) O4B 0.0260(16) 0.0244(16) 0.0224(16) -0.0006(13) 0.0045(13) 0.0026(13) O5B 0.0222(15) 0.0256(16) 0.0388(19) 0.0003(15) 0.0008(14) 0.0049(12) N1B 0.0251(19) 0.033(2) 0.0208(18) -0.0046(16) -0.0003(15) 0.0030(16) N2B 0.030(2) 0.026(2) 0.0228(19) 0.0018(16) 0.0018(16) 0.0040(16) N3B 0.0253(18) 0.025(2) 0.0208(18) -0.0007(15) 0.0003(15) 0.0049(15) N4B 0.0252(17) 0.0273(18) 0.0234(17) -0.0050(18) 0.0030(13) 0.0009(17) N11B 0.041(2) 0.029(2) 0.0223(19) -0.0024(16) 0.0082(17) 0.0007(17) N21B 0.038(2) 0.044(3) 0.038(2) 0.014(2) 0.012(2) 0.0036(19) N31B 0.041(2) 0.0176(18) 0.025(2) 0.0012(15) -0.0054(17) 0.0004(16) N41B 0.031(2) 0.027(2) 0.0208(18) -0.0012(15) 0.0085(15) -0.0026(15) C1B 0.029(2) 0.036(2) 0.027(2) -0.005(2) -0.0067(17) 0.007(2) C2B 0.040(3) 0.030(3) 0.020(2) 0.0029(19) -0.005(2) 0.007(2) C3B 0.029(2) 0.032(2) 0.025(2) 0.0033(19) 0.0008(19) 0.0095(18) C4B 0.032(2) 0.024(3) 0.029(2) 0.0057(19) -0.0041(18) 0.0095(18) C5B 0.028(2) 0.028(2) 0.027(2) -0.0016(19) 0.0063(18) 0.0084(18) C6B 0.032(2) 0.026(2) 0.025(2) -0.0064(19) 0.0072(19) -0.0002(18) C7B 0.022(2) 0.044(3) 0.032(2) -0.005(2) 0.0070(18) 0.0034(18) C8B 0.020(2) 0.043(3) 0.036(3) -0.005(2) -0.002(2) -0.0018(19) C10B 0.034(2) 0.029(2) 0.020(2) -0.0047(18) 0.0004(18) 0.0025(19) C11B 0.039(3) 0.025(2) 0.023(2) 0.0022(19) 0.003(2) 0.006(2) C12B 0.040(3) 0.035(3) 0.027(2) 0.001(2) 0.004(2) 0.000(2) C13B 0.064(4) 0.031(3) 0.040(3) -0.001(2) 0.022(3) 0.006(3) C14B 0.056(3) 0.031(3) 0.025(2) -0.003(2) 0.015(2) 0.002(2) C15B 0.076(4) 0.034(3) 0.028(3) -0.001(2) -0.004(3) 0.000(3) C16B 0.112(7) 0.045(4) 0.035(3) 0.005(3) 0.004(4) 0.010(4) C17B 0.121(7) 0.045(4) 0.028(3) 0.004(3) 0.011(4) -0.015(4) C18B 0.080(5) 0.049(4) 0.060(4) -0.005(3) 0.042(4) -0.018(4) C19B 0.049(3) 0.042(3) 0.050(4) -0.005(3) 0.018(3) -0.001(3) C20B 0.040(3) 0.030(2) 0.021(2) 0.0026(19) 0.004(2) 0.006(2) C21B 0.029(2) 0.031(3) 0.033(3) 0.008(2) 0.012(2) 0.0064(19) C22B 0.025(2) 0.054(4) 0.059(4) 0.017(3) 0.009(2) 0.004(2) C23B 0.051(4) 0.076(6) 0.083(5) 0.007(4) 0.031(4) -0.011(3) C24B 0.033(3) 0.056(4) 0.047(3) 0.015(3) 0.007(3) 0.003(2) C25B 0.036(3) 0.062(4) 0.056(4) 0.014(3) 0.008(3) 0.001(3) C26B 0.049(4) 0.067(5) 0.059(4) 0.002(4) 0.012(3) 0.007(3) C27B 0.055(4) 0.084(6) 0.054(4) 0.000(4) -0.002(3) -0.009(4) C28B 0.039(3) 0.115(7) 0.050(4) 0.024(4) -0.011(3) -0.023(4) C29B 0.030(2) 0.071(4) 0.062(4) 0.023(4) -0.005(3) -0.001(3) C30B 0.035(2) 0.021(2) 0.024(2) 0.0025(17) -0.0050(18) 0.0019(17) C31B 0.025(2) 0.024(2) 0.024(2) 0.0049(18) 0.0010(17) -0.0023(17) C32B 0.032(2) 0.025(2) 0.023(2) 0.0060(19) -0.0052(19) -0.0020(19) C33B 0.054(3) 0.033(3) 0.041(3) 0.013(2) -0.022(3) -0.013(3) C34B 0.034(2) 0.028(2) 0.028(2) 0.010(2) -0.0080(18) -0.005(2) C35B 0.056(3) 0.065(4) 0.031(3) 0.005(3) 0.005(2) -0.014(3) C36B 0.068(5) 0.132(9) 0.050(4) 0.030(5) -0.004(4) -0.049(6) C37B 0.093(7) 0.105(8) 0.079(6) 0.055(6) -0.062(6) -0.071(6) C38B 0.095(6) 0.036(3) 0.063(5) 0.020(3) -0.051(5) -0.028(4) C39B 0.052(3) 0.028(3) 0.045(3) 0.001(2) -0.026(3) -0.006(2) C40B 0.030(2) 0.029(2) 0.025(2) -0.0024(19) 0.0096(19) -0.0028(19) C41B 0.024(2) 0.028(2) 0.019(2) -0.0023(18) 0.0017(17) -0.0054(18) C42B 0.022(2) 0.026(2) 0.028(2) 0.0018(19) 0.0030(18) 0.0003(17) C43B 0.040(3) 0.030(2) 0.031(3) 0.007(2) -0.007(2) -0.002(2) C44B 0.030(2) 0.022(2) 0.025(2) 0.0042(18) 0.0006(18) 0.0055(17) C45B 0.026(2) 0.029(2) 0.031(2) -0.001(2) -0.0035(19) 0.0034(18) C46B 0.030(2) 0.043(3) 0.039(3) 0.003(3) -0.007(2) 0.009(2) C47B 0.058(3) 0.030(2) 0.026(2) 0.003(2) -0.013(2) 0.011(3) C48B 0.053(3) 0.030(2) 0.024(2) 0.002(2) 0.007(2) 0.013(2) C49B 0.036(3) 0.030(2) 0.028(2) 0.000(2) 0.007(2) 0.006(2) S1 0.0328(6) 0.0249(6) 0.0306(6) -0.0012(5) -0.0080(5) -0.0015(5) O11 0.099(4) 0.025(2) 0.056(3) -0.0044(19) -0.035(3) -0.002(2) O12 0.044(2) 0.041(2) 0.047(2) 0.0069(19) -0.0224(19) -0.0038(17) O13 0.052(2) 0.0296(19) 0.036(2) -0.0030(16) 0.0092(18) 0.0062(16) C1S 0.035(3) 0.094(6) 0.042(3) 0.018(4) 0.004(3) 0.008(3) F11 0.086(4) 0.276(10) 0.055(3) -0.013(4) 0.026(3) 0.059(5) F12 0.0329(19) 0.137(4) 0.069(3) 0.035(3) -0.0016(19) 0.016(2) F13 0.047(2) 0.118(5) 0.127(4) 0.069(4) -0.009(3) -0.029(3) S2 0.0372(7) 0.0346(6) 0.0369(7) -0.0088(5) 0.0081(6) -0.0084(5) O21 0.063(3) 0.037(2) 0.0283(19) 0.0013(17) -0.0002(18) -0.0039(19) O22 0.057(3) 0.048(3) 0.048(3) -0.018(2) 0.007(2) 0.004(2) O23 0.051(3) 0.063(3) 0.086(4) -0.011(3) 0.015(3) -0.027(2) C2S 0.045(3) 0.029(2) 0.034(3) -0.003(2) -0.005(2) 0.004(2) F21 0.061(2) 0.052(2) 0.0449(18) -0.004(2) -0.0170(16) 0.004(2) F22 0.0431(18) 0.055(2) 0.0473(19) 0.0021(16) 0.0089(15) -0.0037(15) F23 0.093(3) 0.0365(19) 0.043(2) -0.0099(16) 0.004(2) 0.0175(19) S3 0.0389(7) 0.0291(6) 0.0341(6) 0.0081(5) 0.0122(5) 0.0069(5) O31 0.0363(19) 0.037(2) 0.042(2) 0.0133(16) 0.0140(16) 0.0021(15) O32 0.048(2) 0.035(2) 0.041(2) 0.0109(17) 0.0202(18) 0.0119(17) O33 0.049(2) 0.045(2) 0.040(2) 0.0008(17) 0.0045(18) 0.0106(17) C3S 0.035(3) 0.035(3) 0.046(3) 0.004(2) 0.008(2) -0.003(2) F31 0.0403(16) 0.0383(17) 0.076(2) 0.020(2) -0.0014(16) 0.0041(16) F32 0.0410(19) 0.057(2) 0.069(2) 0.024(2) 0.0180(18) 0.0029(16) F33 0.061(2) 0.072(3) 0.062(3) -0.022(2) -0.002(2) -0.003(2) S4 0.0265(8) 0.0477(12) 0.0301(9) 0.0092(8) -0.0041(6) -0.0077(7) O41 0.057(3) 0.069(3) 0.034(2) -0.016(2) -0.0122(19) 0.009(2) O42 0.031(2) 0.100(4) 0.080(3) 0.037(3) -0.013(2) -0.011(2) O43 0.051(4) 0.061(5) 0.066(6) 0.020(5) -0.006(4) -0.022(4) C4S 0.102(8) 0.051(5) 0.039(5) 0.008(4) 0.038(5) -0.002(5) F41 0.079(5) 0.074(5) 0.074(4) 0.024(3) 0.025(4) -0.017(3) F42 0.068(4) 0.130(7) 0.153(7) 0.054(6) 0.078(5) 0.040(4) F43 0.287(12) 0.074(5) 0.032(3) -0.014(3) 0.049(5) -0.024(6) S5 0.0759(16) 0.118(2) 0.167(3) 0.060(2) 0.0279(19) 0.0484(16) O51 0.191(10) 0.178(9) 0.092(6) 0.033(6) -0.038(6) 0.087(8) O52 0.052(3) 0.148(7) 0.069(4) -0.027(4) -0.010(3) 0.028(3) S6 0.0278(9) 0.0231(12) 0.0436(11) 0.0028(8) 0.0135(7) -0.0028(7) O61 0.0286(18) 0.038(2) 0.057(2) 0.0030(19) 0.0015(17) -0.0092(15) O62 0.039(3) 0.064(4) 0.047(3) 0.001(3) 0.023(3) 0.006(3) O63 0.071(4) 0.037(4) 0.095(5) 0.010(4) 0.007(4) -0.011(3) C6S 0.031(3) 0.077(5) 0.040(3) -0.014(3) 0.006(2) 0.000(3) F61 0.102(3) 0.065(3) 0.078(3) 0.027(3) -0.008(3) -0.007(3) F62 0.058(3) 0.098(5) 0.035(3) -0.005(3) 0.007(2) 0.027(3) F63 0.055(2) 0.098(4) 0.081(3) -0.007(3) -0.020(2) -0.009(2) O1S 0.091(4) 0.049(3) 0.057(3) -0.003(2) -0.026(3) 0.000(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 Er1A O3A 2.300(3) . ? Er1A O1A 2.305(3) . ? Er1A O2A 2.350(3) . ? Er1A O4A 2.362(3) . ? Er1A O5A 2.374(3) . ? Er1A N3A 2.652(4) . ? Er1A N4A 2.672(4) . ? Er1A N2A 2.670(4) . ? Er1A N1A 2.681(4) . ? O1A C11A 1.250(5) . ? O2A C21A 1.255(5) . ? O3A C31A 1.244(5) . ? O4A C41A 1.245(5) . ? N1A C8A 1.486(6) . ? N1A C1A 1.492(6) . ? N1A C10A 1.497(6) . ? N2A C2A 1.490(5) . ? N2A C20A 1.490(6) . ? N2A C3A 1.499(6) . ? N3A C30A 1.488(5) . ? N3A C4A 1.493(5) . ? N3A C5A 1.508(6) . ? N4A C40A 1.485(6) . ? N4A C6A 1.490(5) . ? N4A C7A 1.502(6) . ? N11A C11A 1.327(6) . ? N11A C12A 1.468(6) . ? N21A C21A 1.330(5) . ? N21A C22A 1.488(6) . ? N31A C31A 1.325(5) . ? N31A C32A 1.464(6) . ? N41A C41A 1.344(6) . ? N41A C42A 1.493(6) . ? C1A C2A 1.531(6) . ? C3A C4A 1.511(6) . ? C5A C6A 1.524(6) . ? C7A C8A 1.528(6) . ? C10A C11A 1.519(6) . ? C12A C14A 1.529(7) . ? C12A C13A 1.549(8) . ? C14A C19A 1.380(8) . ? C14A C15A 1.392(8) . ? C15A C16A 1.403(11) . ? C16A C17A 1.417(13) . ? C17A C18A 1.337(14) . ? C18A C19A 1.386(9) . ? C20A C21A 1.512(6) . ? C22A C24A 1.527(7) . ? C22A C23A 1.548(7) . ? C24A C25A 1.392(7) . ? C24A C29A 1.397(7) . ? C25A C26A 1.413(7) . ? C26A C27A 1.381(9) . ? C27A C28A 1.383(9) . ? C28A C29A 1.391(8) . ? C30A C31A 1.507(6) . ? C32A C34A 1.533(6) . ? C32A C33A 1.541(6) . ? C34A C35A 1.382(8) . ? C34A C39A 1.395(7) . ? C35A C36A 1.414(8) . ? C36A C37A 1.394(11) . ? C37A C38A 1.375(12) . ? C38A C39A 1.386(9) . ? C40A C41A 1.524(6) . ? C42A C43A 1.525(7) . ? C42A C44A 1.527(6) . ? C44A C49A 1.390(7) . ? C44A C45A 1.402(7) . ? C45A C46A 1.399(8) . ? C46A C47A 1.379(8) . ? C47A C48A 1.375(8) . ? C48A C49A 1.392(7) . ? Er1B O4B 2.301(3) . ? Er1B O3B 2.315(3) . ? Er1B O2B 2.316(3) . ? Er1B O1B 2.317(3) . ? Er1B O5B 2.380(3) . ? Er1B N2B 2.638(4) . ? Er1B N3B 2.654(4) . ? Er1B N1B 2.661(4) . ? Er1B N4B 2.665(4) . ? O1B C11B 1.248(6) . ? O2B C21B 1.275(6) . ? O3B C31B 1.259(6) . ? O4B C41B 1.268(5) . ? N1B C8B 1.486(6) . ? N1B C10B 1.485(6) . ? N1B C1B 1.502(6) . ? N2B C20B 1.481(6) . ? N2B C3B 1.493(6) . ? N2B C2B 1.500(6) . ? N3B C30B 1.484(6) . ? N3B C4B 1.502(6) . ? N3B C5B 1.509(6) . ? N4B C7B 1.490(6) . ? N4B C6B 1.499(6) . ? N4B C40B 1.512(7) . ? N11B C11B 1.342(6) . ? N11B C12B 1.485(7) . ? N21B C21B 1.312(7) . ? N21B C22B 1.468(7) . ? N31B C31B 1.313(6) . ? N31B C32B 1.486(6) . ? N41B C41B 1.326(6) . ? N41B C42B 1.495(6) . ? C1B C2B 1.496(7) . ? C3B C4B 1.525(7) . ? C5B C6B 1.528(7) . ? C7B C8B 1.501(7) . ? C10B C11B 1.510(7) . ? C12B C13B 1.511(8) . ? C12B C14B 1.516(8) . ? C14B C19B 1.378(9) . ? C14B C15B 1.403(9) . ? C15B C16B 1.397(9) . ? C16B C17B 1.414(12) . ? C17B C18B 1.345(12) . ? C18B C19B 1.398(9) . ? C20B C21B 1.524(7) . ? C22B C24B 1.516(9) . ? C22B C23B 1.538(8) . ? C24B C25B 1.399(9) . ? C24B C29B 1.406(9) . ? C25B C26B 1.395(10) . ? C26B C27B 1.367(11) . ? C27B C28B 1.366(12) . ? C28B C29B 1.380(12) . ? C30B C31B 1.514(6) . ? C32B C34B 1.519(7) . ? C32B C33B 1.536(7) . ? C34B C39B 1.382(8) . ? C34B C35B 1.399(8) . ? C35B C36B 1.407(11) . ? C36B C37B 1.305(16) . ? C37B C38B 1.359(14) . ? C38B C39B 1.405(10) . ? C40B C41B 1.507(7) . ? C42B C44B 1.514(7) . ? C42B C43B 1.522(7) . ? C44B C45B 1.399(7) . ? C44B C49B 1.401(7) . ? C45B C46B 1.397(7) . ? C46B C47B 1.402(8) . ? C47B C48B 1.378(8) . ? C48B C49B 1.389(7) . ? S1 O11 1.428(4) . ? S1 O13 1.440(4) . ? S1 O12 1.447(4) . ? S1 C1S 1.823(7) . ? C1S F11 1.305(9) . ? C1S F12 1.329(7) . ? C1S F13 1.340(10) . ? S2 O23 1.434(5) . ? S2 O21 1.440(4) . ? S2 O22 1.445(5) . ? S2 C2S 1.812(6) . ? C2S F22 1.340(7) . ? C2S F21 1.341(6) . ? C2S F23 1.346(6) . ? S3 O31 1.438(4) . ? S3 O33 1.442(4) . ? S3 O32 1.454(4) . ? S3 C3S 1.828(6) . ? C3S F31 1.322(7) . ? C3S F33 1.338(7) . ? C3S F32 1.346(6) . ? S4 O41 1.419(4) . ? S4 O42 1.465(5) . ? S4 O43 1.468(10) . ? S4 C4S 1.823(9) . ? O41 S4' 1.544(8) . ? O42 S4' 1.386(7) . ? C4S F43 1.314(12) . ? C4S F41 1.315(11) . ? C4S F42 1.322(13) . ? S4' O43' 1.53(4) . ? S4' C4S' 1.84(3) . ? C4S' F41' 1.27(5) . ? C4S' F42' 1.31(4) . ? C4S' F43' 1.37(4) . ? S5 O53' 1.41(2) . ? S5 O52 1.424(6) . ? S5 O51 1.504(9) . ? S5 O53 1.554(16) . ? S5 C5S' 1.84(3) . ? S5 C5S 1.97(2) . ? C5S F53 1.229(17) . ? C5S F52 1.254(17) . ? C5S F51 1.274(17) . ? O53' C5S' 1.43(3) . ? O53' F53' 1.62(3) . ? C5S' F51' 1.194(18) . ? C5S' F53' 1.224(18) . ? C5S' F52' 1.233(18) . ? F51' F52' 1.76(2) . ? F52' F52' 1.79(3) 2_556 ? S6 O63 1.412(7) . ? S6 O62 1.443(6) . ? S6 O61 1.451(4) . ? S6 C6S 1.836(7) . ? O61 S6' 1.406(8) . ? S6' O63' 1.44(2) . ? S6' O62' 1.43(2) . ? S6' C6S 1.875(9) . ? F62' C6S 1.48(2) . ? C6S F63 1.307(7) . ? C6S F62 1.315(7) . ? C6S F61 1.349(9) . ? O1S C7S 1.388(19) . ? C7S C8S 1.50(2) . ? C7S C8S' 1.78(3) . ? C8S' O6W 1.56(3) . ? O2S C9S 1.37(3) . ? C9S C10S 1.524(18) . ? O3S C11S 1.17(3) . ? C11S C12S 1.54(3) . ? O6W C8S' 1.56(3) 2_656 ? 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 O3A Er1A O1A 142.89(11) . . ? O3A Er1A O2A 84.67(11) . . ? O1A Er1A O2A 84.56(11) . . ? O3A Er1A O4A 84.26(11) . . ? O1A Er1A O4A 84.84(11) . . ? O2A Er1A O4A 145.48(11) . . ? O3A Er1A O5A 72.20(12) . . ? O1A Er1A O5A 70.69(12) . . ? O2A Er1A O5A 73.12(11) . . ? O4A Er1A O5A 72.37(11) . . ? O3A Er1A N3A 66.99(11) . . ? O1A Er1A N3A 141.18(11) . . ? O2A Er1A N3A 72.89(11) . . ? O4A Er1A N3A 130.77(11) . . ? O5A Er1A N3A 128.36(11) . . ? O3A Er1A N4A 74.22(11) . . ? O1A Er1A N4A 131.70(11) . . ? O2A Er1A N4A 140.08(10) . . ? O4A Er1A N4A 66.32(11) . . ? O5A Er1A N4A 128.43(12) . . ? N3A Er1A N4A 67.77(11) . . ? O3A Er1A N2A 131.78(11) . . ? O1A Er1A N2A 74.11(11) . . ? O2A Er1A N2A 66.26(11) . . ? O4A Er1A N2A 140.37(11) . . ? O5A Er1A N2A 127.82(12) . . ? N3A Er1A N2A 68.03(11) . . ? N4A Er1A N2A 103.74(12) . . ? O3A Er1A N1A 141.58(11) . . ? O1A Er1A N1A 66.82(11) . . ? O2A Er1A N1A 130.35(11) . . ? O4A Er1A N1A 73.70(11) . . ? O5A Er1A N1A 127.02(11) . . ? N3A Er1A N1A 104.62(11) . . ? N4A Er1A N1A 68.24(11) . . ? N2A Er1A N1A 67.25(11) . . ? C11A O1A Er1A 125.8(3) . . ? C21A O2A Er1A 124.4(3) . . ? C31A O3A Er1A 125.2(3) . . ? C41A O4A Er1A 123.7(3) . . ? C8A N1A C1A 108.4(3) . . ? C8A N1A C10A 110.2(3) . . ? C1A N1A C10A 109.7(4) . . ? C8A N1A Er1A 111.0(3) . . ? C1A N1A Er1A 111.8(2) . . ? C10A N1A Er1A 105.7(3) . . ? C2A N2A C20A 108.3(3) . . ? C2A N2A C3A 109.8(3) . . ? C20A N2A C3A 109.4(3) . . ? C2A N2A Er1A 112.4(3) . . ? C20A N2A Er1A 105.9(2) . . ? C3A N2A Er1A 110.9(2) . . ? C30A N3A C4A 110.0(3) . . ? C30A N3A C5A 109.7(3) . . ? C4A N3A C5A 107.8(3) . . ? C30A N3A Er1A 105.5(2) . . ? C4A N3A Er1A 111.8(2) . . ? C5A N3A Er1A 112.0(2) . . ? C40A N4A C6A 108.3(3) . . ? C40A N4A C7A 109.4(3) . . ? C6A N4A C7A 109.9(3) . . ? C40A N4A Er1A 106.5(3) . . ? C6A N4A Er1A 111.7(2) . . ? C7A N4A Er1A 110.9(2) . . ? C11A N11A C12A 120.6(5) . . ? C21A N21A C22A 121.6(4) . . ? C31A N31A C32A 121.8(4) . . ? C41A N41A C42A 123.0(4) . . ? N1A C1A C2A 112.7(4) . . ? N2A C2A C1A 110.8(3) . . ? N2A C3A C4A 114.0(3) . . ? N3A C4A C3A 111.2(3) . . ? N3A C5A C6A 112.5(4) . . ? N4A C6A C5A 111.1(4) . . ? N4A C7A C8A 114.1(3) . . ? N1A C8A C7A 111.4(4) . . ? N1A C10A C11A 110.7(3) . . ? O1A C11A N11A 122.0(4) . . ? O1A C11A C10A 120.0(4) . . ? N11A C11A C10A 117.9(4) . . ? N11A C12A C14A 112.3(4) . . ? N11A C12A C13A 108.4(5) . . ? C14A C12A C13A 110.6(5) . . ? C19A C14A C15A 118.7(5) . . ? C19A C14A C12A 119.3(5) . . ? C15A C14A C12A 121.9(5) . . ? C14A C15A C16A 120.5(7) . . ? C15A C16A C17A 118.0(7) . . ? C18A C17A C16A 121.2(7) . . ? C17A C18A C19A 120.1(8) . . ? C14A C19A C18A 121.4(7) . . ? N2A C20A C21A 110.0(3) . . ? O2A C21A N21A 123.9(4) . . ? O2A C21A C20A 119.8(4) . . ? N21A C21A C20A 116.3(4) . . ? N21A C22A C24A 111.8(4) . . ? N21A C22A C23A 107.7(4) . . ? C24A C22A C23A 111.1(4) . . ? C25A C24A C29A 119.1(5) . . ? C25A C24A C22A 121.5(4) . . ? C29A C24A C22A 119.4(5) . . ? C24A C25A C26A 120.0(5) . . ? C27A C26A C25A 120.0(6) . . ? C26A C27A C28A 120.0(5) . . ? C27A C28A C29A 120.4(5) . . ? C28A C29A C24A 120.4(5) . . ? N3A C30A C31A 110.9(3) . . ? O3A C31A N31A 122.3(4) . . ? O3A C31A C30A 119.8(4) . . ? N31A C31A C30A 117.9(4) . . ? N31A C32A C34A 112.1(4) . . ? N31A C32A C33A 108.8(4) . . ? C34A C32A C33A 111.0(4) . . ? C35A C34A C39A 119.9(5) . . ? C35A C34A C32A 119.9(5) . . ? C39A C34A C32A 120.2(5) . . ? C34A C35A C36A 119.5(6) . . ? C37A C36A C35A 119.6(7) . . ? C38A C37A C36A 120.4(6) . . ? C37A C38A C39A 120.0(7) . . ? C38A C39A C34A 120.5(7) . . ? N4A C40A C41A 109.4(4) . . ? O4A C41A N41A 122.8(4) . . ? O4A C41A C40A 120.9(4) . . ? N41A C41A C40A 116.2(4) . . ? N41A C42A C43A 107.7(4) . . ? N41A C42A C44A 112.0(4) . . ? C43A C42A C44A 111.9(4) . . ? C49A C44A C45A 119.0(5) . . ? C49A C44A C42A 119.6(4) . . ? C45A C44A C42A 121.3(4) . . ? C46A C45A C44A 119.3(5) . . ? C47A C46A C45A 120.8(5) . . ? C48A C47A C46A 120.1(5) . . ? C47A C48A C49A 119.9(5) . . ? C44A C49A C48A 120.9(5) . . ? O4B Er1B O3B 85.27(11) . . ? O4B Er1B O2B 144.01(11) . . ? O3B Er1B O2B 82.26(12) . . ? O4B Er1B O1B 83.73(12) . . ? O3B Er1B O1B 143.50(11) . . ? O2B Er1B O1B 86.55(13) . . ? O4B Er1B O5B 73.08(11) . . ? O3B Er1B O5B 71.93(12) . . ? O2B Er1B O5B 70.96(12) . . ? O1B Er1B O5B 71.57(12) . . ? O4B Er1B N2B 140.55(12) . . ? O3B Er1B N2B 131.50(12) . . ? O2B Er1B N2B 67.08(12) . . ? O1B Er1B N2B 73.22(12) . . ? O5B Er1B N2B 125.84(12) . . ? O4B Er1B N3B 131.86(11) . . ? O3B Er1B N3B 66.70(11) . . ? O2B Er1B N3B 72.26(12) . . ? O1B Er1B N3B 141.07(12) . . ? O5B Er1B N3B 127.20(12) . . ? N2B Er1B N3B 68.55(12) . . ? O4B Er1B N1B 73.04(12) . . ? O3B Er1B N1B 141.23(12) . . ? O2B Er1B N1B 133.07(12) . . ? O1B Er1B N1B 66.58(12) . . ? O5B Er1B N1B 128.02(12) . . ? N2B Er1B N1B 68.57(13) . . ? N3B Er1B N1B 104.76(12) . . ? O4B Er1B N4B 66.76(12) . . ? O3B Er1B N4B 74.68(11) . . ? O2B Er1B N4B 139.72(13) . . ? O1B Er1B N4B 130.65(12) . . ? O5B Er1B N4B 129.03(12) . . ? N2B Er1B N4B 105.13(12) . . ? N3B Er1B N4B 68.42(13) . . ? N1B Er1B N4B 67.36(12) . . ? C11B O1B Er1B 124.3(3) . . ? C21B O2B Er1B 123.5(3) . . ? C31B O3B Er1B 125.2(3) . . ? C41B O4B Er1B 125.8(3) . . ? C8B N1B C10B 109.2(4) . . ? C8B N1B C1B 109.1(4) . . ? C10B N1B C1B 110.0(4) . . ? C8B N1B Er1B 112.2(3) . . ? C10B N1B Er1B 105.8(3) . . ? C1B N1B Er1B 110.5(3) . . ? C20B N2B C3B 111.1(4) . . ? C20B N2B C2B 109.4(4) . . ? C3B N2B C2B 108.4(4) . . ? C20B N2B Er1B 105.6(3) . . ? C3B N2B Er1B 111.4(3) . . ? C2B N2B Er1B 111.0(3) . . ? C30B N3B C4B 109.4(4) . . ? C30B N3B C5B 109.5(4) . . ? C4B N3B C5B 108.9(3) . . ? C30B N3B Er1B 106.9(3) . . ? C4B N3B Er1B 111.1(3) . . ? C5B N3B Er1B 111.0(3) . . ? C7B N4B C6B 109.3(4) . . ? C7B N4B C40B 109.5(4) . . ? C6B N4B C40B 109.7(3) . . ? C7B N4B Er1B 111.6(3) . . ? C6B N4B Er1B 110.7(3) . . ? C40B N4B Er1B 106.0(3) . . ? C11B N11B C12B 121.7(4) . . ? C21B N21B C22B 121.8(5) . . ? C31B N31B C32B 121.0(4) . . ? C41B N41B C42B 120.5(4) . . ? C2B C1B N1B 113.7(4) . . ? N2B C2B C1B 112.1(4) . . ? N2B C3B C4B 113.5(4) . . ? N3B C4B C3B 110.8(4) . . ? N3B C5B C6B 112.5(4) . . ? N4B C6B C5B 110.8(4) . . ? N4B C7B C8B 113.3(4) . . ? N1B C8B C7B 111.6(4) . . ? N1B C10B C11B 110.3(4) . . ? O1B C11B N11B 121.6(5) . . ? O1B C11B C10B 120.7(4) . . ? N11B C11B C10B 117.8(4) . . ? N11B C12B C13B 108.5(5) . . ? N11B C12B C14B 111.2(4) . . ? C13B C12B C14B 112.3(4) . . ? C19B C14B C15B 119.2(6) . . ? C19B C14B C12B 120.8(6) . . ? C15B C14B C12B 120.0(5) . . ? C16B C15B C14B 119.6(7) . . ? C15B C16B C17B 119.2(7) . . ? C18B C17B C16B 120.9(7) . . ? C17B C18B C19B 119.7(7) . . ? C14B C19B C18B 121.2(7) . . ? N2B C20B C21B 111.5(4) . . ? O2B C21B N21B 121.5(5) . . ? O2B C21B C20B 119.1(4) . . ? N21B C21B C20B 119.3(5) . . ? N21B C22B C24B 111.7(5) . . ? N21B C22B C23B 108.4(5) . . ? C24B C22B C23B 111.6(6) . . ? C25B C24B C29B 119.6(7) . . ? C25B C24B C22B 120.4(6) . . ? C29B C24B C22B 120.0(6) . . ? C24B C25B C26B 119.0(7) . . ? C27B C26B C25B 121.1(7) . . ? C28B C27B C26B 119.7(8) . . ? C27B C28B C29B 121.7(7) . . ? C28B C29B C24B 118.9(7) . . ? N3B C30B C31B 110.8(4) . . ? O3B C31B N31B 122.6(4) . . ? O3B C31B C30B 119.8(4) . . ? N31B C31B C30B 117.4(4) . . ? N31B C32B C34B 111.6(4) . . ? N31B C32B C33B 107.4(4) . . ? C34B C32B C33B 114.0(4) . . ? C39B C34B C35B 118.8(6) . . ? C39B C34B C32B 120.3(5) . . ? C35B C34B C32B 120.9(5) . . ? C36B C35B C34B 116.2(8) . . ? C37B C36B C35B 125.8(10) . . ? C36B C37B C38B 118.2(8) . . ? C37B C38B C39B 120.2(8) . . ? C34B C39B C38B 120.7(7) . . ? N4B C40B C41B 110.1(4) . . ? O4B C41B N41B 120.7(4) . . ? O4B C41B C40B 119.8(4) . . ? N41B C41B C40B 119.4(4) . . ? N41B C42B C44B 111.2(4) . . ? N41B C42B C43B 108.5(4) . . ? C44B C42B C43B 111.7(4) . . ? C45B C44B C49B 117.9(5) . . ? C45B C44B C42B 121.4(4) . . ? C49B C44B C42B 120.6(4) . . ? C44B C45B C46B 120.5(5) . . ? C45B C46B C47B 120.6(5) . . ? C48B C47B C46B 118.9(5) . . ? C47B C48B C49B 120.6(5) . . ? C48B C49B C44B 121.4(5) . . ? O11 S1 O13 114.4(3) . . ? O11 S1 O12 115.8(3) . . ? O13 S1 O12 114.5(2) . . ? O11 S1 C1S 105.6(4) . . ? O13 S1 C1S 101.7(3) . . ? O12 S1 C1S 102.4(3) . . ? F11 C1S F12 107.0(6) . . ? F11 C1S F13 108.2(7) . . ? F12 C1S F13 109.0(7) . . ? F11 C1S S1 110.7(6) . . ? F12 C1S S1 111.3(5) . . ? F13 C1S S1 110.5(5) . . ? O23 S2 O21 116.1(3) . . ? O23 S2 O22 115.1(3) . . ? O21 S2 O22 114.7(3) . . ? O23 S2 C2S 101.4(3) . . ? O21 S2 C2S 103.1(2) . . ? O22 S2 C2S 103.8(3) . . ? F22 C2S F21 107.5(5) . . ? F22 C2S F23 106.4(5) . . ? F21 C2S F23 107.6(4) . . ? F22 C2S S2 112.3(4) . . ? F21 C2S S2 111.6(4) . . ? F23 C2S S2 111.0(4) . . ? O31 S3 O33 116.8(3) . . ? O31 S3 O32 114.8(2) . . ? O33 S3 O32 113.5(2) . . ? O31 S3 C3S 102.9(3) . . ? O33 S3 C3S 102.6(3) . . ? O32 S3 C3S 103.7(3) . . ? F31 C3S F33 107.4(5) . . ? F31 C3S F32 106.9(5) . . ? F33 C3S F32 106.1(5) . . ? F31 C3S S3 113.2(4) . . ? F33 C3S S3 111.6(4) . . ? F32 C3S S3 111.3(4) . . ? O41 S4 O42 114.7(3) . . ? O41 S4 O43 114.4(5) . . ? O42 S4 O43 116.5(4) . . ? O41 S4 C4S 101.1(4) . . ? O42 S4 C4S 103.4(4) . . ? O43 S4 C4S 104.1(5) . . ? S4 O41 S4' 34.5(3) . . ? S4' O42 S4 36.1(3) . . ? F43 C4S F41 105.9(8) . . ? F43 C4S F42 109.9(10) . . ? F41 C4S F42 106.6(10) . . ? F43 C4S S4 111.4(8) . . ? F41 C4S S4 112.5(7) . . ? F42 C4S S4 110.4(6) . . ? O42 S4' O43' 121.0(14) . . ? O42 S4' O41 111.9(5) . . ? O43' S4' O41 115.1(14) . . ? O42 S4' C4S' 96.5(11) . . ? O43' S4' C4S' 107.6(16) . . ? O41 S4' C4S' 100.7(11) . . ? F41' C4S' F42' 112(3) . . ? F41' C4S' F43' 111(3) . . ? F42' C4S' F43' 108(3) . . ? F41' C4S' S4' 109(3) . . ? F42' C4S' S4' 113(2) . . ? F43' C4S' S4' 104(2) . . ? O53' S5 O52 141.9(10) . . ? O53' S5 O51 102.2(10) . . ? O52 S5 O51 115.9(4) . . ? O53' S5 O53 63.7(10) . . ? O52 S5 O53 102.6(7) . . ? O51 S5 O53 105.7(8) . . ? O53' S5 C5S' 50.2(11) . . ? O52 S5 C5S' 98.5(7) . . ? O51 S5 C5S' 135.7(8) . . ? O53 S5 C5S' 92.2(9) . . ? O53' S5 C5S 93.3(11) . . ? O52 S5 C5S 92.7(6) . . ? O51 S5 C5S 82.9(8) . . ? O53 S5 C5S 156.5(8) . . ? C5S' S5 C5S 67.7(8) . . ? F53 C5S F52 106.7(17) . . ? F53 C5S F51 111.0(17) . . ? F52 C5S F51 109.2(17) . . ? F53 C5S S5 101.7(17) . . ? F52 C5S S5 112(2) . . ? F51 C5S S5 115.4(16) . . ? S5 O53' C5S' 80.4(16) . . ? S5 O53' F53' 125.8(17) . . ? C5S' O53' F53' 46.8(10) . . ? F51' C5S' F53' 99(2) . . ? F51' C5S' F52' 92.6(19) . . ? F53' C5S' F52' 94.2(19) . . ? F51' C5S' O53' 150(2) . . ? F53' C5S' O53' 74.6(17) . . ? F52' C5S' O53' 116.6(19) . . ? F51' C5S' S5 122(2) . . ? F53' C5S' S5 122.7(19) . . ? F52' C5S' S5 118.9(19) . . ? O53' C5S' S5 49.4(12) . . ? C5S' F51' F52' 44.5(11) . . ? C5S' F52' F52' 159.4(12) . 2_556 ? C5S' F52' F51' 42.8(10) . . ? F52' F52' F51' 117.4(12) 2_556 . ? C5S' F53' O53' 58.5(16) . . ? O63 S6 O62 114.7(4) . . ? O63 S6 O61 115.3(4) . . ? O62 S6 O61 115.8(4) . . ? O63 S6 C6S 103.6(4) . . ? O62 S6 C6S 102.6(3) . . ? O61 S6 C6S 102.2(3) . . ? S6' O61 S6 21.2(3) . . ? O61 S6' O63' 114.6(9) . . ? O61 S6' O62' 116.5(10) . . ? O63' S6' O62' 110.7(12) . . ? O61 S6' C6S 102.1(5) . . ? O63' S6' C6S 103.6(9) . . ? O62' S6' C6S 107.8(10) . . ? F63 C6S F62 111.6(6) . . ? F63 C6S F61 105.2(6) . . ? F62 C6S F61 102.1(6) . . ? F63 C6S F62' 91.8(10) . . ? F62 C6S F62' 43.3(9) . . ? F61 C6S F62' 145.3(11) . . ? F63 C6S S6 113.6(5) . . ? F62 C6S S6 112.1(5) . . ? F61 C6S S6 111.5(5) . . ? F62' C6S S6 87.7(10) . . ? F63 C6S S6' 114.9(5) . . ? F62 C6S S6' 122.8(5) . . ? F61 C6S S6' 96.1(5) . . ? F62' C6S S6' 103.8(10) . . ? S6 C6S S6' 16.3(2) . . ? O1S C7S C8S 114.5(15) . . ? O1S C7S C8S' 144.5(16) . . ? C8S C7S C8S' 100.8(15) . . ? O6W C8S' C7S 116.2(17) . . ? O2S C9S C10S 111(2) . . ? O3S C11S C12S 119(3) . . ? C8S' O6W C8S' 134(3) . 2_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11A H11A O23 0.88 2.01 2.874(6) 168.2 2_646 N21A H21A O61 0.88 2.08 2.939(6) 165.5 1_545 N31A H31A O12 0.88 2.04 2.845(5) 151.5 4 N41A H41A O31 0.87 2.07 2.925(5) 168.0 3_554 O5A H01A O41 0.84 2.07 2.906(5) 174.1 . O5A H02A O1S 0.84 1.96 2.794(6) 176.5 . N11B H11B O21 0.88 2.11 2.974(6) 170.4 . N21B H21B O32 0.87 2.02 2.884(6) 169.6 . N31B H31B O13 0.88 2.01 2.866(5) 165.4 . N41B H41B O62 0.88 2.15 2.912(7) 145.3 . O5B H01B O52 0.84 2.07 2.903(7) 169.9 . O5B H02B O2S 0.84 1.87 2.697(9) 168.3 . O1S H01S O1W 0.85 1.86 2.691(11) 165.9 . O1W H1W1 O22 0.84 2.02 2.859(11) 179.7 2_656 O1W H2W1 O43 0.84 2.08 2.855(13) 152.9 . O2S H02S O2W 0.91 2.14 2.816(15) 129.9 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.930 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.102 #==============================================END