# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Pierre Thuery' _publ_contact_author_email thuery@drecam.cea.fr _publ_author_name P.Thuery data_1 _database_code_depnum_ccdc_archive 'CCDC 863485' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H104 N26 Nd2 O78 S8 U4' _chemical_formula_weight 3742.61 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 31.3656(7) _cell_length_b 14.1509(6) _cell_length_c 12.4299(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.607(3) _cell_angle_gamma 90.00 _cell_volume 5439.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 85166 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3580 _exptl_absorpt_coefficient_mu 7.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.606 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps (503 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 85166 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8592 _reflns_number_gt 6467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The solvent water molecules (O24-O27) were given 0.5 occupancy factors in order to retain acceptable displacement parameters. The H atoms bound to O atoms were found on a Fourier-difference map, except for those of the water solvent molecules, and all the others were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some voids in the lattice likely indicate the presence of other, unresolved water solvent molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8592 _refine_ls_number_parameters 403 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.642 _refine_diff_density_min -1.882 _refine_diff_density_rms 0.186 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 U1 U 0.693403(7) 1.0000 0.422185(18) 0.02474(7) Uani 1 2 d S . . U2 U 0.691390(7) 1.0000 0.722366(19) 0.02738(7) Uani 1 2 d S . . Nd Nd 0.583247(12) 0.5000 -0.08852(3) 0.03804(11) Uani 1 2 d S . . S1 S 0.71324(4) 0.76607(9) 0.31268(9) 0.0307(2) Uani 1 1 d . . . S2 S 0.67022(5) 0.67256(10) -0.01979(10) 0.0416(3) Uani 1 1 d . . . O1 O 0.74978(13) 1.0000 0.4226(4) 0.0336(11) Uani 1 2 d S . . O2 O 0.63673(13) 1.0000 0.4188(4) 0.0311(10) Uani 1 2 d S . . O3 O 0.74743(15) 1.0000 0.7776(4) 0.0371(11) Uani 1 2 d S . . O4 O 0.63544(15) 1.0000 0.6732(4) 0.0371(11) Uani 1 2 d S . . O5 O 0.68882(11) 0.8369(2) 0.3651(3) 0.0395(8) Uani 1 1 d . . . O6 O 0.71697(11) 0.6777(3) 0.3711(3) 0.0425(8) Uani 1 1 d . . . O7 O 0.75423(10) 0.8017(3) 0.2906(3) 0.0420(9) Uani 1 1 d . . . O8 O 0.63761(15) 0.6048(3) 0.0015(3) 0.0634(13) Uani 1 1 d . . . O9 O 0.69838(16) 0.6351(3) -0.0895(3) 0.0702(13) Uani 1 1 d . . . O10 O 0.65131(12) 0.7613(3) -0.0580(3) 0.0477(9) Uani 1 1 d . . . O11 O 0.70184(10) 0.9061(2) 0.5782(2) 0.0312(7) Uani 1 1 d . . . H11 H 0.7315 0.8912 0.5932 0.037 Uiso 1 1 d R . . O12 O 0.67927(17) 1.0000 0.2243(4) 0.0452(13) Uani 1 2 d S . . H12A H 0.6960 1.0000 0.1803 0.054 Uiso 1 2 d SR . . H12B H 0.6548 1.0000 0.1978 0.054 Uiso 1 2 d SR . . O13 O 0.68725(12) 0.8322(3) 0.7752(3) 0.0437(9) Uani 1 1 d . . . H13A H 0.6997 0.7831 0.7466 0.052 Uiso 1 1 d R . . H13B H 0.6632 0.8030 0.7923 0.052 Uiso 1 1 d R . . O14 O 0.67417(18) 1.0000 0.9033(4) 0.0506(14) Uani 1 2 d S . . H14A H 0.6870 1.0000 0.9656 0.061 Uiso 1 2 d SR . . H14B H 0.6474 1.0000 0.8972 0.061 Uiso 1 2 d SR . . O15 O 0.59915(10) 0.6060(3) -0.2319(3) 0.0418(9) Uani 1 1 d . . . O16 O 0.59532(12) 0.6248(3) -0.7141(3) 0.0509(10) Uani 1 1 d . . . O17 O 0.50022(12) 0.7342(3) -0.2559(3) 0.0533(10) Uani 1 1 d . . . O18 O 0.53840(17) 0.6329(4) -0.0696(5) 0.0940(14) Uani 1 1 d U . . H18A H 0.5262 0.6849 -0.0953 0.113 Uiso 1 1 d R . . H18B H 0.5412 0.6454 0.0056 0.113 Uiso 1 1 d R . . O19 O 0.5721(2) 0.5000 0.1084(5) 0.0605(15) Uani 1 2 d SU . . H19 H 0.5815 0.5517 0.1555 0.073 Uiso 1 1 d R . . O20 O 0.5146(3) 0.5000 -0.2226(8) 0.119(2) Uani 1 2 d SU . . H20 H 0.4938 0.5516 -0.2416 0.142 Uiso 1 1 d R . . O21 O 0.4960(4) 1.0000 0.1549(13) 0.167(3) Uani 1 2 d SU . . O22 O 0.5363(4) 1.0000 0.2972(12) 0.157(3) Uani 1 2 d SU . . O23 O 0.4680(4) 1.0000 0.2878(11) 0.154(3) Uani 1 2 d SU . . O24 O 0.73776(16) 1.0000 0.0858(5) 0.0525(15) Uani 1 2 d S . . O25 O 0.5956(3) 0.9341(9) 0.9300(9) 0.099(4) Uani 0.50 1 d PU . . O26 O 0.5975(3) 1.0000 0.1431(10) 0.159(4) Uani 1 2 d SU . . O27 O 0.5562(3) 0.7650(9) 0.0901(9) 0.090(3) Uani 0.50 1 d PU . . N1 N 0.64624(12) 0.5854(3) -0.3524(3) 0.0373(10) Uani 1 1 d . . . N2 N 0.60397(12) 0.7125(3) -0.3688(3) 0.0379(10) Uani 1 1 d . . . N3 N 0.60508(13) 0.7220(3) -0.5645(3) 0.0408(10) Uani 1 1 d . . . N4 N 0.63843(13) 0.5857(3) -0.5519(3) 0.0399(10) Uani 1 1 d . . . N5 N 0.53571(14) 0.7931(3) -0.3894(4) 0.0414(10) Uani 1 1 d . . . N6 N 0.53549(14) 0.8010(3) -0.5845(4) 0.0430(11) Uani 1 1 d . . . N7 N 0.4988(4) 1.0000 0.2518(10) 0.094(3) Uani 1 2 d S . . C1 C 0.67970(16) 0.7470(4) 0.1841(4) 0.0408(12) Uani 1 1 d . . . H1A H 0.6542 0.7118 0.1947 0.049 Uiso 1 1 calc R . . H1B H 0.6703 0.8074 0.1516 0.049 Uiso 1 1 calc R . . C2 C 0.70359(18) 0.6931(4) 0.1081(4) 0.0452(13) Uani 1 1 d . . . H2A H 0.7133 0.6330 0.1411 0.054 Uiso 1 1 calc R . . H2B H 0.7289 0.7287 0.0969 0.054 Uiso 1 1 calc R . . C3 C 0.61503(15) 0.6319(4) -0.3110(4) 0.0370(12) Uani 1 1 d . . . C4 C 0.65625(15) 0.6315(4) -0.4503(4) 0.0368(12) Uani 1 1 d . . . H4 H 0.6873 0.6435 -0.4451 0.044 Uiso 1 1 calc R . . C5 C 0.62989(16) 0.7248(4) -0.4553(4) 0.0409(12) Uani 1 1 d . . . H5 H 0.6486 0.7805 -0.4435 0.049 Uiso 1 1 calc R . . C6 C 0.61114(16) 0.6408(4) -0.6187(4) 0.0388(12) Uani 1 1 d . . . C7 C 0.57948(16) 0.7855(4) -0.3292(4) 0.0421(12) Uani 1 1 d . . . H7A H 0.5942 0.8453 -0.3334 0.050 Uiso 1 1 calc R . . H7B H 0.5781 0.7734 -0.2530 0.050 Uiso 1 1 calc R . . C8 C 0.57901(18) 0.7986(4) -0.6134(5) 0.0467(14) Uani 1 1 d . . . H8A H 0.5764 0.7939 -0.6921 0.056 Uiso 1 1 calc R . . H8B H 0.5936 0.8577 -0.5912 0.056 Uiso 1 1 calc R . . C9 C 0.50022(16) 0.7718(4) -0.3448(4) 0.0406(12) Uani 1 1 d . . . C10 C 0.52508(17) 0.8460(4) -0.4902(4) 0.0436(13) Uani 1 1 d . . . H10 H 0.5367 0.9104 -0.4823 0.052 Uiso 1 1 calc R . . C11 C 0.6665(2) 0.5000 -0.3067(5) 0.0394(18) Uani 1 2 d S . . H11A H 0.6665 0.5000 -0.2287 0.047 Uiso 1 2 calc SR . . H11B H 0.6965 0.5000 -0.3175 0.047 Uiso 1 2 calc SR . . C12 C 0.6568(2) 0.5000 -0.5912(6) 0.045(2) Uani 1 2 d S . . H12C H 0.6879 0.5000 -0.5671 0.054 Uiso 1 2 calc SR . . H12D H 0.6515 0.5000 -0.6703 0.054 Uiso 1 2 calc SR . . 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 U1 0.02388(12) 0.02744(14) 0.02327(12) 0.000 0.00498(9) 0.000 U2 0.03039(13) 0.02875(14) 0.02324(12) 0.000 0.00515(9) 0.000 Nd 0.03037(19) 0.0557(3) 0.02977(19) 0.000 0.01017(15) 0.000 S1 0.0345(6) 0.0304(6) 0.0279(6) -0.0061(5) 0.0073(4) -0.0009(5) S2 0.0613(8) 0.0384(7) 0.0244(6) -0.0004(5) 0.0054(6) -0.0045(6) O1 0.023(2) 0.038(3) 0.041(3) 0.000 0.0078(19) 0.000 O2 0.025(2) 0.031(3) 0.037(3) 0.000 0.0044(19) 0.000 O3 0.033(2) 0.038(3) 0.038(3) 0.000 0.000(2) 0.000 O4 0.031(2) 0.039(3) 0.042(3) 0.000 0.005(2) 0.000 O5 0.0414(18) 0.036(2) 0.044(2) -0.0125(17) 0.0155(15) -0.0019(16) O6 0.050(2) 0.034(2) 0.045(2) 0.0051(17) 0.0123(17) 0.0058(16) O7 0.0331(17) 0.047(2) 0.047(2) -0.0121(18) 0.0102(15) -0.0105(16) O8 0.091(3) 0.055(3) 0.039(2) 0.006(2) -0.005(2) -0.033(2) O9 0.095(3) 0.077(3) 0.040(2) -0.006(2) 0.015(2) 0.031(3) O10 0.061(2) 0.039(2) 0.044(2) 0.0070(18) 0.0112(18) 0.0001(18) O11 0.0378(16) 0.0276(18) 0.0283(16) 0.0030(13) 0.0061(13) 0.0026(14) O12 0.044(3) 0.059(4) 0.033(3) 0.000 0.006(2) 0.000 O13 0.055(2) 0.036(2) 0.045(2) 0.0068(17) 0.0221(17) -0.0022(17) O14 0.059(3) 0.064(4) 0.031(3) 0.000 0.015(2) 0.000 O15 0.0378(18) 0.061(3) 0.0279(17) 0.0037(17) 0.0094(14) 0.0031(17) O16 0.051(2) 0.067(3) 0.0303(19) -0.0005(19) -0.0074(16) 0.000(2) O17 0.047(2) 0.068(3) 0.044(2) 0.012(2) 0.0065(18) 0.012(2) O18 0.095(3) 0.111(4) 0.080(3) 0.011(2) 0.028(2) 0.029(2) O19 0.071(3) 0.075(4) 0.040(3) 0.000 0.023(3) 0.000 O20 0.097(4) 0.149(5) 0.107(5) 0.000 0.009(4) 0.000 O21 0.136(5) 0.197(7) 0.167(7) 0.000 0.026(5) 0.000 O22 0.123(5) 0.184(7) 0.163(7) 0.000 0.020(5) 0.000 O23 0.118(5) 0.186(7) 0.163(7) 0.000 0.041(5) 0.000 O24 0.042(3) 0.075(4) 0.042(3) 0.000 0.012(2) 0.000 O25 0.084(6) 0.128(8) 0.086(7) -0.013(6) 0.014(5) 0.017(6) O26 0.096(6) 0.248(9) 0.127(7) 0.000 -0.002(5) 0.000 O27 0.094(6) 0.112(7) 0.070(6) -0.016(6) 0.035(5) -0.021(6) N1 0.0272(19) 0.058(3) 0.026(2) 0.001(2) 0.0047(16) -0.0040(19) N2 0.034(2) 0.052(3) 0.028(2) -0.004(2) 0.0054(17) -0.0085(19) N3 0.038(2) 0.054(3) 0.028(2) 0.002(2) -0.0007(17) -0.010(2) N4 0.034(2) 0.060(3) 0.025(2) 0.000(2) 0.0034(16) -0.007(2) N5 0.045(2) 0.041(3) 0.036(2) 0.002(2) 0.0013(19) -0.0066(19) N6 0.047(2) 0.043(3) 0.038(2) 0.004(2) 0.0030(19) -0.009(2) N7 0.093(8) 0.117(10) 0.071(7) 0.000 0.012(6) 0.000 C1 0.043(3) 0.047(3) 0.032(3) -0.009(2) 0.006(2) -0.005(2) C2 0.054(3) 0.047(3) 0.034(3) -0.010(2) 0.005(2) 0.000(3) C3 0.030(2) 0.051(3) 0.028(2) 0.000(2) -0.0004(19) -0.011(2) C4 0.028(2) 0.058(4) 0.025(2) -0.004(2) 0.0049(18) -0.013(2) C5 0.039(3) 0.053(3) 0.029(2) 0.001(2) 0.001(2) -0.017(2) C6 0.032(2) 0.051(3) 0.032(3) 0.000(2) 0.004(2) -0.009(2) C7 0.049(3) 0.042(3) 0.034(3) -0.008(2) 0.003(2) -0.006(2) C8 0.053(3) 0.049(4) 0.037(3) 0.007(3) 0.006(2) -0.017(3) C9 0.050(3) 0.034(3) 0.038(3) -0.002(2) 0.005(2) 0.005(2) C10 0.060(3) 0.026(3) 0.042(3) 0.002(2) 0.000(3) -0.005(2) C11 0.026(3) 0.069(6) 0.022(3) 0.000 -0.001(3) 0.000 C12 0.034(4) 0.077(6) 0.025(3) 0.000 0.008(3) 0.000 _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 U1 O1 1.767(4) . ? U1 O2 1.771(4) . ? U1 O11 2.330(3) 6_575 ? U1 O11 2.330(3) . ? U1 O5 2.411(3) . ? U1 O5 2.411(3) 6_575 ? U1 O12 2.425(5) . ? U2 O4 1.759(5) . ? U2 O3 1.777(5) . ? U2 O11 2.298(3) . ? U2 O11 2.298(3) 6_575 ? U2 O14 2.399(5) . ? U2 O13 2.473(4) 6_575 ? U2 O13 2.473(4) . ? Nd O18 2.384(5) 6_565 ? Nd O18 2.384(5) . ? Nd O8 2.392(4) . ? Nd O8 2.392(4) 6_565 ? Nd O15 2.444(4) 6_565 ? Nd O15 2.444(4) . ? Nd O20 2.494(9) . ? Nd O19 2.531(6) . ? S1 O6 1.441(4) . ? S1 O7 1.449(3) . ? S1 O5 1.478(3) . ? S1 C1 1.781(5) . ? S2 O10 1.436(4) . ? S2 O9 1.437(4) . ? S2 O8 1.458(4) . ? S2 C2 1.775(5) . ? O11 H11 0.9428 . ? O12 H12A 0.8182 . ? O12 H12B 0.7840 . ? O13 H13A 0.8991 . ? O13 H13B 0.9165 . ? O14 H14A 0.8109 . ? O14 H14B 0.8291 . ? O15 C3 1.229(6) . ? O16 C6 1.228(6) . ? O17 C9 1.227(6) . ? O18 H18A 0.8654 . ? O18 H18B 0.9405 . ? O19 H19 0.9529 . ? O20 H20 0.9795 . ? O21 N7 1.192(14) . ? O22 N7 1.216(14) . ? O23 N7 1.131(14) . ? N1 C3 1.351(6) . ? N1 C11 1.438(5) . ? N1 C4 1.460(6) . ? N2 C3 1.362(7) . ? N2 C7 1.423(7) . ? N2 C5 1.463(6) . ? N3 C6 1.362(7) . ? N3 C8 1.431(7) . ? N3 C5 1.448(6) . ? N4 C6 1.339(7) . ? N4 C4 1.445(6) . ? N4 C12 1.462(6) . ? N5 C9 1.358(7) . ? N5 C10 1.449(7) . ? N5 C7 1.454(6) . ? N6 C9 1.367(6) 2_654 ? N6 C10 1.419(7) . ? N6 C8 1.469(7) . ? C1 C2 1.507(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C5 1.553(8) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N6 1.368(6) 2_654 ? C10 C10 1.551(11) 2_654 ? C10 H10 0.9800 . ? C11 N1 1.438(5) 6_565 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.462(6) 6_565 ? C12 H12C 0.9700 . ? C12 H12D 0.9700 . ? 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 O1 U1 O2 178.8(2) . . ? O1 U1 O11 91.30(15) . 6_575 ? O2 U1 O11 89.65(15) . 6_575 ? O1 U1 O11 91.30(15) . . ? O2 U1 O11 89.65(15) . . ? O11 U1 O11 69.56(16) 6_575 . ? O1 U1 O5 90.65(9) . . ? O2 U1 O5 89.01(9) . . ? O11 U1 O5 141.60(12) 6_575 . ? O11 U1 O5 72.06(12) . . ? O1 U1 O5 90.65(9) . 6_575 ? O2 U1 O5 89.01(9) . 6_575 ? O11 U1 O5 72.06(12) 6_575 6_575 ? O11 U1 O5 141.60(12) . 6_575 ? O5 U1 O5 146.26(18) . 6_575 ? O1 U1 O12 91.0(2) . . ? O2 U1 O12 87.9(2) . . ? O11 U1 O12 145.14(8) 6_575 . ? O11 U1 O12 145.14(8) . . ? O5 U1 O12 73.14(9) . . ? O5 U1 O12 73.14(9) 6_575 . ? O4 U2 O3 177.6(2) . . ? O4 U2 O11 89.61(16) . . ? O3 U2 O11 92.33(16) . . ? O4 U2 O11 89.61(16) . 6_575 ? O3 U2 O11 92.33(16) . 6_575 ? O11 U2 O11 70.67(16) . 6_575 ? O4 U2 O14 87.6(2) . . ? O3 U2 O14 90.0(2) . . ? O11 U2 O14 144.56(8) . . ? O11 U2 O14 144.56(8) 6_575 . ? O4 U2 O13 89.92(10) . 6_575 ? O3 U2 O13 89.41(10) . 6_575 ? O11 U2 O13 141.55(12) . 6_575 ? O11 U2 O13 70.88(12) 6_575 6_575 ? O14 U2 O13 73.80(9) . 6_575 ? O4 U2 O13 89.92(10) . . ? O3 U2 O13 89.41(10) . . ? O11 U2 O13 70.88(12) . . ? O11 U2 O13 141.55(12) 6_575 . ? O14 U2 O13 73.80(9) . . ? O13 U2 O13 147.57(17) 6_575 . ? O18 Nd O18 104.2(3) 6_565 . ? O18 Nd O8 146.03(17) 6_565 . ? O18 Nd O8 81.42(19) . . ? O18 Nd O8 81.42(19) 6_565 6_565 ? O18 Nd O8 146.03(17) . 6_565 ? O8 Nd O8 76.6(2) . 6_565 ? O18 Nd O15 77.48(16) 6_565 6_565 ? O18 Nd O15 138.78(16) . 6_565 ? O8 Nd O15 120.36(14) . 6_565 ? O8 Nd O15 75.17(13) 6_565 6_565 ? O18 Nd O15 138.78(16) 6_565 . ? O18 Nd O15 77.48(16) . . ? O8 Nd O15 75.17(13) . . ? O8 Nd O15 120.36(14) 6_565 . ? O15 Nd O15 75.76(18) 6_565 . ? O18 Nd O20 66.92(18) 6_565 . ? O18 Nd O20 66.92(18) . . ? O8 Nd O20 141.38(11) . . ? O8 Nd O20 141.38(11) 6_565 . ? O15 Nd O20 76.78(19) 6_565 . ? O15 Nd O20 76.78(19) . . ? O18 Nd O19 74.03(16) 6_565 . ? O18 Nd O19 74.03(16) . . ? O8 Nd O19 75.56(15) . . ? O8 Nd O19 75.56(15) 6_565 . ? O15 Nd O19 141.59(9) 6_565 . ? O15 Nd O19 141.59(9) . . ? O20 Nd O19 113.8(3) . . ? O6 S1 O7 113.4(2) . . ? O6 S1 O5 111.8(2) . . ? O7 S1 O5 112.9(2) . . ? O6 S1 C1 107.9(3) . . ? O7 S1 C1 107.0(2) . . ? O5 S1 C1 103.1(2) . . ? O10 S2 O9 112.6(3) . . ? O10 S2 O8 111.8(3) . . ? O9 S2 O8 112.8(3) . . ? O10 S2 C2 107.6(3) . . ? O9 S2 C2 105.7(3) . . ? O8 S2 C2 105.8(3) . . ? S1 O5 U1 140.3(2) . . ? S2 O8 Nd 142.2(3) . . ? U2 O11 U1 107.95(14) . . ? U2 O11 H11 103.9 . . ? U1 O11 H11 105.2 . . ? U1 O12 H12A 130.5 . . ? U1 O12 H12B 115.3 . . ? H12A O12 H12B 114.2 . . ? U2 O13 H13A 126.3 . . ? U2 O13 H13B 125.2 . . ? H13A O13 H13B 99.9 . . ? U2 O14 H14A 137.9 . . ? U2 O14 H14B 107.3 . . ? H14A O14 H14B 114.8 . . ? C3 O15 Nd 157.7(4) . . ? Nd O18 H18A 150.0 . . ? Nd O18 H18B 106.8 . . ? H18A O18 H18B 99.7 . . ? Nd O19 H19 121.0 . . ? Nd O20 H20 128.7 . . ? C3 N1 C11 124.1(5) . . ? C3 N1 C4 111.7(4) . . ? C11 N1 C4 124.2(5) . . ? C3 N2 C7 121.9(4) . . ? C3 N2 C5 111.3(4) . . ? C7 N2 C5 124.6(5) . . ? C6 N3 C8 123.1(4) . . ? C6 N3 C5 112.9(5) . . ? C8 N3 C5 123.9(5) . . ? C6 N4 C4 113.3(5) . . ? C6 N4 C12 121.5(5) . . ? C4 N4 C12 123.2(5) . . ? C9 N5 C10 112.4(4) . . ? C9 N5 C7 122.7(4) . . ? C10 N5 C7 123.0(4) . . ? C9 N6 C10 113.0(4) 2_654 . ? C9 N6 C8 122.0(5) 2_654 . ? C10 N6 C8 124.3(4) . . ? O23 N7 O21 118.4(15) . . ? O23 N7 O22 129.8(15) . . ? O21 N7 O22 111.9(14) . . ? C2 C1 S1 111.0(4) . . ? C2 C1 H1A 109.4 . . ? S1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? S1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 S2 111.3(4) . . ? C1 C2 H2A 109.4 . . ? S2 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? S2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? O15 C3 N1 125.1(5) . . ? O15 C3 N2 124.8(5) . . ? N1 C3 N2 110.1(4) . . ? N4 C4 N1 115.0(4) . . ? N4 C4 C5 102.7(4) . . ? N1 C4 C5 103.1(4) . . ? N4 C4 H4 111.8 . . ? N1 C4 H4 111.8 . . ? C5 C4 H4 111.8 . . ? N3 C5 N2 114.1(4) . . ? N3 C5 C4 102.4(4) . . ? N2 C5 C4 103.2(4) . . ? N3 C5 H5 112.2 . . ? N2 C5 H5 112.2 . . ? C4 C5 H5 112.2 . . ? O16 C6 N4 127.3(5) . . ? O16 C6 N3 124.5(5) . . ? N4 C6 N3 108.2(4) . . ? N2 C7 N5 113.2(4) . . ? N2 C7 H7A 108.9 . . ? N5 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? N5 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? N3 C8 N6 113.6(4) . . ? N3 C8 H8A 108.8 . . ? N6 C8 H8A 108.8 . . ? N3 C8 H8B 108.8 . . ? N6 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O17 C9 N5 126.0(5) . . ? O17 C9 N6 126.0(5) . 2_654 ? N5 C9 N6 108.0(5) . 2_654 ? N6 C10 N5 115.4(5) . . ? N6 C10 C10 103.7(5) . 2_654 ? N5 C10 C10 102.6(5) . 2_654 ? N6 C10 H10 111.5 . . ? N5 C10 H10 111.5 . . ? C10 C10 H10 111.5 2_654 . ? N1 C11 N1 114.3(5) . 6_565 ? N1 C11 H11A 108.7 . . ? N1 C11 H11A 108.7 6_565 . ? N1 C11 H11B 108.7 . . ? N1 C11 H11B 108.7 6_565 . ? H11A C11 H11B 107.6 . . ? N4 C12 N4 112.2(6) . 6_565 ? N4 C12 H12C 109.2 . . ? N4 C12 H12C 109.2 6_565 . ? N4 C12 H12D 109.2 . . ? N4 C12 H12D 109.2 6_565 . ? H12C C12 H12D 107.9 . . ? 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 O11 H11 O6 0.94 1.88 2.784(5) 161.1 7_666 O12 H12A O24 0.82 1.90 2.717(7) 176.2 . O12 H12B O26 0.78 1.81 2.596(12) 177.2 . O13 H13A O7 0.90 1.99 2.852(5) 159.7 7_666 O13 H13B O10 0.92 2.04 2.712(5) 128.5 1_556 O14 H14A O24 0.81 1.99 2.760(8) 157.3 1_556 O14 H14B O25 0.83 1.97 2.706(13) 146.7 . O18 H18A O17 0.87 2.14 2.815(7) 134.1 . O18 H18B O27 0.94 2.01 2.716(13) 130.9 . O19 H19 O16 0.95 1.91 2.825(6) 160.0 1_556 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 863486' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H86 Dy1.50 N26.50 O66.50 S6 U4' _chemical_formula_weight 3414.60 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 31.1056(12) _cell_length_b 14.1740(3) _cell_length_c 20.8484(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.8479(17) _cell_angle_gamma 90.00 _cell_volume 9171.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 149385 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6474 _exptl_absorpt_coefficient_mu 8.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.600 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (505 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 149385 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 30.51 _reflns_number_total 14501 _reflns_number_gt 10899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The atom Dy2 and the associated nitrate ion were given 0.5 occupancy factors so as to account for the close contact between Dy2 and its image by symmetry and to retain acceptable displacement parameters. One O atom in each of the three nitrate ions is disordered around a symmetry plane, the disorder on the associated N atom being unresolved. Several solvent water molecules were given 0.5 occupancy factors so as to to account for too close contacts and/or to retain acceptable displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to O atoms were found on a Fourier-difference map, except for those of O35, O40 and four solvent water molecules, and all the others were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+31.4742P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14501 _refine_ls_number_parameters 754 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.748 _refine_diff_density_min -2.764 _refine_diff_density_rms 0.185 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 U1 U 0.156713(7) 0.5000 0.245517(11) 0.02210(7) Uani 1 2 d S . . U2 U 0.126285(8) 0.5000 0.067435(12) 0.02987(8) Uani 1 2 d S . . U3 U 0.256500(7) 0.0000 0.156119(12) 0.02391(7) Uani 1 2 d S . . U4 U 0.284873(7) 0.0000 0.334569(12) 0.02265(7) Uani 1 2 d S . . Dy1 Dy 0.090278(10) 0.0000 0.545880(16) 0.03197(10) Uani 1 2 d S . . Dy2 Dy 0.01392(3) 0.0000 0.97681(4) 0.0690(4) Uani 0.50 2 d SP . . S1 S 0.18779(4) 0.26897(10) 0.31492(5) 0.0256(3) Uani 1 1 d . . . S2 S 0.17111(4) 0.17144(11) 0.50893(6) 0.0313(3) Uani 1 1 d . . . S3 S 0.22492(4) 0.23790(11) 0.09505(6) 0.0314(3) Uani 1 1 d . . . O1 O 0.09940(14) 0.5000 0.2480(2) 0.0241(11) Uani 1 2 d S . . O2 O 0.21358(14) 0.5000 0.2454(2) 0.0297(12) Uani 1 2 d S . . O3 O 0.07526(16) 0.5000 0.0995(3) 0.0344(13) Uani 1 2 d S . . O4 O 0.17827(18) 0.5000 0.0360(3) 0.0466(17) Uani 1 2 d S . . O5 O 0.31364(15) 0.0000 0.1542(3) 0.0333(13) Uani 1 2 d S . . O6 O 0.19960(14) 0.0000 0.1579(2) 0.0273(11) Uani 1 2 d S . . O7 O 0.33811(15) 0.0000 0.3077(2) 0.0276(11) Uani 1 2 d S . . O8 O 0.23247(15) 0.0000 0.3642(2) 0.0274(11) Uani 1 2 d S . . O9 O 0.15871(10) 0.3373(3) 0.27977(16) 0.0281(8) Uani 1 1 d . . . O10 O 0.18735(11) 0.1787(3) 0.28216(17) 0.0327(9) Uani 1 1 d . . . O11 O 0.23098(10) 0.3062(3) 0.32971(17) 0.0322(9) Uani 1 1 d . . . O12 O 0.13557(12) 0.1038(3) 0.49409(17) 0.0384(10) Uani 1 1 d . . . O13 O 0.20594(12) 0.1335(3) 0.55099(17) 0.0432(11) Uani 1 1 d . . . O14 O 0.15529(11) 0.2611(3) 0.53153(17) 0.0343(9) Uani 1 1 d . . . O15 O 0.25438(12) 0.1621(3) 0.11775(18) 0.0372(9) Uani 1 1 d . . . O16 O 0.22794(13) 0.3163(4) 0.1390(3) 0.0643(15) Uani 1 1 d . . . O17 O 0.18160(13) 0.2059(3) 0.0803(2) 0.0513(12) Uani 1 1 d . . . O18 O 0.14994(10) 0.4063(3) 0.15338(15) 0.0298(8) Uani 1 1 d . . . H18 H 0.1716 0.3787 0.1457 0.036 Uiso 1 1 d R . . O19 O 0.16064(16) 0.5000 0.3622(2) 0.0322(12) Uani 1 2 d S . . H19A H 0.1851 0.5000 0.3896 0.039 Uiso 1 2 d SR . . H19B H 0.1406 0.5000 0.3852 0.039 Uiso 1 2 d SR . . O20 O 0.11745(13) 0.3326(3) 0.03308(19) 0.0463(11) Uani 1 1 d . . . H20A H 0.1326 0.2813 0.0440 0.056 Uiso 1 1 d R . . H20B H 0.0994 0.3078 0.0002 0.056 Uiso 1 1 d R . . O21 O 0.0960(2) 0.5000 -0.0430(3) 0.065(2) Uani 1 2 d S . . O22 O 0.0443(3) 0.5000 -0.1168(3) 0.069(2) Uani 1 2 d S . . O23 O 0.0386(3) 0.4306(9) -0.0240(5) 0.073(3) Uani 0.50 1 d P . . O24 O 0.26265(10) 0.0948(3) 0.24808(15) 0.0267(8) Uani 1 1 d . . . H24 H 0.2374 0.1143 0.2545 0.032 Uiso 1 1 d R . . O25 O 0.25177(18) 0.0000 0.0397(3) 0.0497(18) Uani 1 2 d S . . H25A H 0.2695 0.0000 0.0020 0.060 Uiso 1 2 d SR . . H25B H 0.2268 0.0000 0.0177 0.060 Uiso 1 2 d SR . . O26 O 0.29310(11) 0.1669(3) 0.36901(16) 0.0304(8) Uani 1 1 d . . . H26A H 0.2731 0.2186 0.3574 0.037 Uiso 1 1 d R . . H26B H 0.3126 0.2021 0.4006 0.037 Uiso 1 1 d R . . O27 O 0.31766(16) 0.0000 0.4424(2) 0.0323(12) Uani 1 2 d S . . H27A H 0.3114 0.0000 0.4862 0.039 Uiso 1 2 d SR . . H27B H 0.3479 0.0000 0.4506 0.039 Uiso 1 2 d SR . . O28 O 0.11842(11) 0.1030(4) 0.62541(16) 0.0423(11) Uani 1 1 d . . . O29 O 0.15089(13) 0.1298(4) 0.90772(18) 0.0609(16) Uani 1 1 d . . . O30 O 0.01939(13) 0.2285(3) 0.6392(2) 0.0462(11) Uani 1 1 d . . . O31 O 0.06424(14) 0.2572(5) 0.9305(2) 0.0665(17) Uani 1 1 d . . . O32 O -0.07405(13) 0.1246(4) 0.65673(18) 0.0463(11) Uani 1 1 d . . . O33 O -0.02913(15) 0.1158(6) 0.9409(2) 0.082(2) Uani 1 1 d . . . O34 O 0.06138(16) 0.0000 0.4367(2) 0.0324(12) Uani 1 2 d S . . H34 H 0.0469 0.0489 0.4238 0.039 Uiso 1 1 d R . . O35 O 0.0370(2) 0.0000 0.6275(4) 0.081(3) Uani 1 2 d S . . O36 O 0.04306(13) 0.1298(4) 0.5319(2) 0.0570(14) Uani 1 1 d . . . H36A H 0.0494 0.1702 0.5609 0.068 Uiso 1 1 d R . . H36B H 0.0507 0.1585 0.4954 0.068 Uiso 1 1 d R . . O37 O 0.0088(5) 0.0000 0.8571(8) 0.081(5) Uani 0.50 2 d SPU . . O38 O 0.0747(7) 0.0000 0.8265(11) 0.111(7) Uani 0.50 2 d SPU . . O39 O 0.0243(6) 0.0453(15) 0.7556(9) 0.067(6) Uani 0.25 1 d PU . . O40 O 0.0663(4) 0.0850(10) 0.9497(5) 0.088(4) Uani 0.50 1 d P . . O41 O 0.4432(2) 0.0000 0.3449(4) 0.074(2) Uani 1 2 d S . . O42 O 0.5118(2) 0.0000 0.3346(3) 0.066(2) Uani 1 2 d S . . O43 O 0.4880(4) 0.0554(11) 0.4220(5) 0.098(5) Uani 0.50 1 d P . . O44 O 0.22898(16) 0.5000 0.4510(2) 0.0380(14) Uani 1 2 d S . . H44 H 0.2459 0.4541 0.4569 0.046 Uiso 1 1 d R . . O45 O 0.1015(3) 0.4450(9) 0.5356(4) 0.072(4) Uani 0.50 1 d P . . O46 O 0.0874(2) 0.4654(8) 0.4152(4) 0.066(5) Uani 0.50 1 d P . . O47 O 0.17233(19) 0.0000 0.0031(3) 0.0551(19) Uani 1 2 d S . . O48 O 0.0598(3) 0.2886(9) 0.4595(5) 0.072(3) Uani 0.50 1 d P . . N1 N 0.0581(3) 0.5000 -0.0615(4) 0.077(3) Uani 1 2 d S . . N2 N 0.17659(13) 0.0841(5) 0.6984(2) 0.0469(15) Uani 1 1 d . . . N3 N 0.13528(16) 0.2127(4) 0.7053(2) 0.0439(14) Uani 1 1 d . . . N4 N 0.15198(16) 0.2265(5) 0.8200(2) 0.0514(16) Uani 1 1 d . . . N5 N 0.18265(14) 0.0851(5) 0.8155(2) 0.0471(15) Uani 1 1 d . . . N6 N 0.06817(18) 0.2900(4) 0.7184(2) 0.0472(13) Uani 1 1 d . . . N7 N -0.00192(18) 0.3008(4) 0.7311(3) 0.0522(15) Uani 1 1 d . . . N8 N 0.01588(17) 0.3002(4) 0.8467(3) 0.0509(15) Uani 1 1 d . . . N9 N 0.08534(18) 0.3109(4) 0.8325(3) 0.0492(14) Uani 1 1 d . . . N10 N -0.06958(17) 0.2227(5) 0.7444(2) 0.0501(15) Uani 1 1 d . . . N11 N -0.10202(14) 0.0860(5) 0.7524(2) 0.0523(17) Uani 1 1 d . . . N12 N -0.08741(14) 0.0862(5) 0.8692(2) 0.0575(19) Uani 1 1 d D . . N13 N -0.05050(16) 0.2159(6) 0.8601(3) 0.062(2) Uani 1 1 d . . . N14 N 0.0371(8) 0.0000 0.8109(11) 0.090(7) Uani 0.50 2 d SPU . . N15 N 0.4807(3) 0.0000 0.3661(5) 0.085(4) Uani 1 2 d S . . C1 C 0.16382(15) 0.2518(4) 0.3897(2) 0.0280(11) Uani 1 1 d . . . H1A H 0.1584 0.3124 0.4091 0.034 Uiso 1 1 calc R . . H1B H 0.1365 0.2194 0.3823 0.034 Uiso 1 1 calc R . . C2 C 0.19391(15) 0.1934(4) 0.4353(2) 0.0297(12) Uani 1 1 d . . . H2A H 0.2209 0.2269 0.4433 0.036 Uiso 1 1 calc R . . H2B H 0.2001 0.1338 0.4149 0.036 Uiso 1 1 calc R . . C3 C 0.2473(3) 0.2804(6) 0.0254(3) 0.071(3) Uani 1 1 d . . . H3A H 0.2295 0.3323 0.0092 0.086 Uiso 1 1 calc R . . H3B H 0.2754 0.3065 0.0384 0.086 Uiso 1 1 calc R . . C4 C 0.14129(16) 0.1301(6) 0.6725(2) 0.0440(18) Uani 1 1 d . . . C5 C 0.19403(16) 0.1316(6) 0.7569(2) 0.051(2) Uani 1 1 d . . . H5 H 0.2252 0.1420 0.7565 0.061 Uiso 1 1 calc R . . C6 C 0.16887(19) 0.2256(6) 0.7566(3) 0.0497(19) Uani 1 1 d . . . H6 H 0.1872 0.2803 0.7493 0.060 Uiso 1 1 calc R . . C7 C 0.16039(17) 0.1466(6) 0.8522(3) 0.051(2) Uani 1 1 d . . . C8 C 0.1061(2) 0.2840(5) 0.6821(3) 0.0513(18) Uani 1 1 d . . . H8A H 0.0973 0.2711 0.6374 0.062 Uiso 1 1 calc R . . H8B H 0.1208 0.3444 0.6839 0.062 Uiso 1 1 calc R . . C9 C 0.1320(2) 0.3072(6) 0.8476(3) 0.059(2) Uani 1 1 d . . . H9A H 0.1450 0.3642 0.8317 0.071 Uiso 1 1 calc R . . H9B H 0.1377 0.3057 0.8939 0.071 Uiso 1 1 calc R . . C10 C 0.0274(2) 0.2684(5) 0.6919(3) 0.0461(16) Uani 1 1 d . . . C11 C 0.0655(3) 0.3497(5) 0.7740(3) 0.059(2) Uani 1 1 d . . . H11 H 0.0760 0.4135 0.7661 0.071 Uiso 1 1 calc R . . C12 C 0.0179(3) 0.3499(5) 0.7856(3) 0.060(2) Uani 1 1 d . . . H12 H 0.0068 0.4144 0.7883 0.071 Uiso 1 1 calc R . . C13 C 0.0561(2) 0.2863(6) 0.8753(3) 0.0488(17) Uani 1 1 d . . . C14 C -0.0484(2) 0.2972(6) 0.7159(3) 0.059(2) Uani 1 1 d . . . H14A H -0.0609 0.3561 0.7293 0.071 Uiso 1 1 calc R . . H14B H -0.0537 0.2925 0.6696 0.071 Uiso 1 1 calc R . . C15 C -0.0230(2) 0.2931(7) 0.8820(3) 0.080(3) Uani 1 1 d . . . H15A H -0.0147 0.2846 0.9274 0.096 Uiso 1 1 calc R . . H15B H -0.0390 0.3517 0.8773 0.096 Uiso 1 1 calc R . . C16 C -0.08063(17) 0.1415(6) 0.7133(3) 0.0477(18) Uani 1 1 d . . . C17 C -0.0849(2) 0.2245(7) 0.8088(3) 0.064(3) Uani 1 1 d . . . H17 H -0.1035 0.2790 0.8153 0.077 Uiso 1 1 calc R . . C18 C -0.10911(18) 0.1316(7) 0.8133(3) 0.064(3) Uani 1 1 d . . . H18A H -0.1398 0.1415 0.8189 0.077 Uiso 1 1 calc R . . C19 C -0.05325(19) 0.1370(7) 0.8938(3) 0.063(2) Uani 1 1 d . . . C20 C -0.1244(3) 0.0000 0.7310(4) 0.063(4) Uani 1 2 d S . . H20C H -0.1529 0.0000 0.7470 0.076 Uiso 1 2 calc SR . . H20D H -0.1277 0.0000 0.6844 0.076 Uiso 1 2 calc SR . . C21 C -0.1021(3) 0.0000 0.8976(4) 0.064(3) Uani 1 2 d SDU . . H21A H -0.0927 0.0000 0.9429 0.076 Uiso 1 2 calc SR . . H21B H -0.1334 0.0000 0.8944 0.076 Uiso 1 2 calc SR . . C22 C 0.1933(2) 0.0000 0.6719(4) 0.048(3) Uani 1 2 d S . . H22A H 0.2244 0.0000 0.6794 0.058 Uiso 1 2 calc SR . . H22B H 0.1866 0.0000 0.6258 0.058 Uiso 1 2 calc SR . . C23 C 0.2029(2) 0.0000 0.8395(4) 0.049(3) Uani 1 2 d S . . H23A H 0.2327 0.0000 0.8283 0.059 Uiso 1 2 calc SR . . H23B H 0.2030 0.0000 0.8860 0.059 Uiso 1 2 calc SR . . 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 U1 0.01702(11) 0.03181(16) 0.01733(11) 0.000 0.00011(8) 0.000 U2 0.02591(13) 0.0443(2) 0.01907(12) 0.000 -0.00073(9) 0.000 U3 0.01944(11) 0.03449(17) 0.01764(12) 0.000 0.00005(8) 0.000 U4 0.02061(11) 0.02962(16) 0.01748(12) 0.000 -0.00052(8) 0.000 Dy1 0.01965(14) 0.0576(3) 0.01829(15) 0.000 -0.00137(11) 0.000 Dy2 0.0316(4) 0.1481(12) 0.0269(4) 0.000 -0.0003(3) 0.000 S1 0.0224(5) 0.0355(8) 0.0186(5) 0.0025(5) -0.0005(4) 0.0025(5) S2 0.0338(6) 0.0428(9) 0.0173(5) 0.0002(6) 0.0009(5) 0.0008(6) S3 0.0389(7) 0.0350(8) 0.0209(6) 0.0013(6) 0.0063(5) 0.0008(6) O1 0.017(2) 0.031(3) 0.024(2) 0.000 -0.0004(17) 0.000 O2 0.016(2) 0.047(4) 0.025(2) 0.000 -0.0033(18) 0.000 O3 0.030(3) 0.038(3) 0.034(3) 0.000 -0.001(2) 0.000 O4 0.036(3) 0.079(5) 0.026(3) 0.000 0.009(2) 0.000 O5 0.023(2) 0.039(3) 0.037(3) 0.000 0.004(2) 0.000 O6 0.021(2) 0.034(3) 0.027(3) 0.000 0.0065(19) 0.000 O7 0.024(2) 0.034(3) 0.024(2) 0.000 -0.0002(19) 0.000 O8 0.027(2) 0.034(3) 0.022(2) 0.000 0.0039(18) 0.000 O9 0.0280(16) 0.034(2) 0.0216(16) 0.0005(16) 0.0001(13) 0.0035(16) O10 0.0339(18) 0.038(2) 0.0259(18) -0.0032(17) -0.0024(14) 0.0045(17) O11 0.0256(16) 0.044(3) 0.0260(18) 0.0049(18) -0.0019(13) -0.0023(17) O12 0.046(2) 0.048(3) 0.0223(17) -0.0051(18) 0.0081(15) -0.011(2) O13 0.045(2) 0.064(3) 0.0205(18) 0.0051(19) -0.0009(15) 0.017(2) O14 0.0331(18) 0.042(3) 0.0276(18) -0.0039(18) -0.0011(14) 0.0051(18) O15 0.0370(19) 0.042(3) 0.032(2) 0.0106(19) -0.0037(15) 0.0007(19) O16 0.034(2) 0.071(4) 0.087(4) -0.039(3) -0.006(2) 0.007(2) O17 0.041(2) 0.044(3) 0.066(3) 0.014(2) -0.022(2) -0.008(2) O18 0.0260(16) 0.042(2) 0.0212(16) -0.0044(16) -0.0002(13) 0.0080(16) O19 0.030(2) 0.047(4) 0.020(2) 0.000 0.0034(19) 0.000 O20 0.049(2) 0.051(3) 0.037(2) -0.008(2) -0.0158(18) 0.016(2) O21 0.060(4) 0.092(6) 0.040(4) 0.000 -0.016(3) 0.000 O22 0.110(6) 0.038(4) 0.051(4) 0.000 -0.053(4) 0.000 O23 0.063(6) 0.100(10) 0.054(6) 0.004(6) -0.008(5) -0.017(6) O24 0.0258(15) 0.032(2) 0.0217(16) -0.0001(16) -0.0004(12) 0.0039(15) O25 0.037(3) 0.089(6) 0.023(3) 0.000 0.005(2) 0.000 O26 0.0293(17) 0.037(2) 0.0243(17) -0.0005(17) -0.0046(13) -0.0008(17) O27 0.032(3) 0.041(4) 0.023(2) 0.000 -0.001(2) 0.000 O28 0.0295(18) 0.080(4) 0.0166(16) -0.002(2) -0.0003(14) -0.009(2) O29 0.046(2) 0.118(5) 0.0194(19) 0.006(3) 0.0048(17) 0.016(3) O30 0.048(2) 0.050(3) 0.039(2) -0.013(2) -0.0076(18) 0.002(2) O31 0.042(2) 0.116(5) 0.039(3) -0.002(3) -0.0135(19) -0.003(3) O32 0.046(2) 0.068(3) 0.0251(19) -0.009(2) 0.0027(16) 0.014(2) O33 0.046(3) 0.160(7) 0.037(2) -0.006(3) -0.025(2) 0.009(3) O34 0.030(3) 0.040(4) 0.026(3) 0.000 -0.004(2) 0.000 O35 0.061(5) 0.121(8) 0.063(5) 0.000 0.020(4) 0.000 O36 0.044(2) 0.083(4) 0.043(2) -0.019(3) -0.0072(19) 0.011(3) O37 0.062(7) 0.110(9) 0.073(8) 0.000 0.015(6) 0.000 O38 0.084(9) 0.131(11) 0.120(10) 0.000 0.019(8) 0.000 O39 0.075(9) 0.081(10) 0.044(8) 0.011(7) 0.001(7) 0.020(7) O40 0.106(9) 0.101(11) 0.056(7) -0.014(7) -0.010(6) 0.058(8) O41 0.042(4) 0.082(6) 0.098(6) 0.000 0.011(4) 0.000 O42 0.051(4) 0.100(7) 0.048(4) 0.000 0.012(3) 0.000 O43 0.086(8) 0.144(15) 0.063(7) -0.022(8) 0.009(6) 0.001(8) O44 0.023(2) 0.059(4) 0.032(3) 0.000 0.000(2) 0.000 O45 0.039(4) 0.132(11) 0.046(5) 0.023(6) 0.004(4) 0.010(5) O46 0.035(4) 0.119(14) 0.044(5) 0.004(5) 0.007(3) -0.004(5) O47 0.041(3) 0.091(6) 0.033(3) 0.000 0.001(3) 0.000 O48 0.089(8) 0.082(9) 0.048(6) 0.034(6) 0.027(5) 0.018(6) N1 0.069(6) 0.116(10) 0.044(5) 0.000 -0.030(5) 0.000 N2 0.023(2) 0.098(5) 0.019(2) -0.001(3) -0.0010(16) -0.007(3) N3 0.042(3) 0.064(4) 0.024(2) 0.008(3) -0.0075(19) -0.027(3) N4 0.037(3) 0.091(5) 0.025(2) -0.001(3) -0.006(2) -0.019(3) N5 0.026(2) 0.096(5) 0.020(2) 0.001(3) -0.0003(17) -0.006(3) N6 0.062(3) 0.042(3) 0.036(3) -0.005(2) -0.009(2) -0.021(3) N7 0.064(3) 0.047(4) 0.043(3) -0.015(3) -0.017(3) 0.028(3) N8 0.048(3) 0.060(4) 0.041(3) -0.018(3) -0.019(2) 0.018(3) N9 0.057(3) 0.049(4) 0.039(3) -0.010(3) -0.015(2) -0.003(3) N10 0.046(3) 0.071(4) 0.032(3) -0.013(3) -0.008(2) 0.028(3) N11 0.027(2) 0.111(6) 0.018(2) -0.012(3) -0.0033(17) 0.005(3) N12 0.028(2) 0.117(6) 0.027(2) -0.017(3) -0.0093(19) 0.019(3) N13 0.032(3) 0.120(6) 0.032(3) -0.023(4) -0.014(2) 0.018(3) N14 0.080(9) 0.111(11) 0.079(10) 0.000 0.002(8) 0.000 N15 0.047(5) 0.149(12) 0.059(6) 0.000 0.009(4) 0.000 C1 0.023(2) 0.040(3) 0.022(2) 0.004(2) 0.0005(17) 0.000(2) C2 0.028(2) 0.041(4) 0.019(2) 0.002(2) -0.0019(18) 0.001(2) C3 0.102(6) 0.069(6) 0.047(4) 0.028(4) 0.032(4) 0.048(5) C4 0.028(2) 0.087(6) 0.018(2) 0.011(3) 0.0010(19) -0.026(3) C5 0.022(2) 0.113(7) 0.019(2) 0.003(3) -0.0018(18) -0.022(3) C6 0.037(3) 0.086(6) 0.026(3) 0.001(3) -0.002(2) -0.032(3) C7 0.026(3) 0.102(6) 0.025(3) 0.000(4) 0.000(2) -0.002(3) C8 0.060(4) 0.057(5) 0.036(3) 0.008(3) -0.005(3) -0.032(4) C9 0.059(4) 0.073(6) 0.043(4) -0.014(4) -0.007(3) -0.027(4) C10 0.057(4) 0.035(4) 0.045(4) 0.002(3) -0.008(3) 0.005(3) C11 0.091(5) 0.036(4) 0.048(4) -0.005(3) -0.017(4) -0.007(4) C12 0.085(5) 0.038(4) 0.051(4) -0.016(3) -0.023(4) 0.018(4) C13 0.049(4) 0.056(5) 0.039(3) -0.017(3) -0.012(3) 0.008(3) C14 0.066(4) 0.073(6) 0.036(3) -0.018(4) -0.023(3) 0.041(4) C15 0.065(5) 0.130(9) 0.043(4) -0.048(5) -0.020(3) 0.052(5) C16 0.028(3) 0.083(6) 0.031(3) -0.008(3) -0.008(2) 0.025(3) C17 0.039(3) 0.119(8) 0.032(3) -0.026(4) -0.011(3) 0.037(4) C18 0.024(3) 0.143(8) 0.025(3) -0.020(4) -0.008(2) 0.021(4) C19 0.032(3) 0.124(8) 0.033(3) -0.016(4) -0.005(2) 0.017(4) C20 0.025(4) 0.144(12) 0.019(4) 0.000 -0.006(3) 0.000 C21 0.041(4) 0.124(8) 0.026(4) 0.000 0.003(3) 0.000 C22 0.022(3) 0.107(9) 0.016(3) 0.000 0.002(3) 0.000 C23 0.021(3) 0.105(9) 0.020(4) 0.000 -0.001(3) 0.000 _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 U1 O2 1.769(4) . ? U1 O1 1.787(4) . ? U1 O18 2.333(3) . ? U1 O18 2.333(3) 6_565 ? U1 O9 2.414(4) 6_565 ? U1 O9 2.414(4) . ? U1 O19 2.428(5) . ? U2 O3 1.763(5) . ? U2 O4 1.785(5) . ? U2 O18 2.311(4) 6_565 ? U2 O18 2.311(4) . ? U2 O21 2.429(6) . ? U2 O20 2.489(5) . ? U2 O20 2.489(5) 6_565 ? U3 O6 1.773(4) . ? U3 O5 1.781(5) . ? U3 O24 2.339(3) . ? U3 O24 2.339(3) 6 ? U3 O25 2.421(5) . ? U3 O15 2.432(4) 6 ? U3 O15 2.432(4) . ? U4 O8 1.781(5) . ? U4 O7 1.784(5) . ? U4 O24 2.317(3) 6 ? U4 O24 2.317(3) . ? U4 O27 2.406(5) . ? U4 O26 2.481(4) . ? U4 O26 2.481(4) 6 ? Dy1 O28 2.334(4) . ? Dy1 O28 2.334(4) 6 ? Dy1 O12 2.350(4) . ? Dy1 O12 2.350(4) 6 ? Dy1 O36 2.360(5) 6 ? Dy1 O36 2.360(5) . ? Dy1 O34 2.390(5) . ? Dy1 O35 2.454(7) . ? Dy2 O40 2.133(15) . ? Dy2 O40 2.133(15) 6 ? Dy2 O33 2.216(6) . ? Dy2 O33 2.216(6) 6 ? Dy2 O33 2.398(6) 2_557 ? Dy2 O33 2.398(6) 5_557 ? Dy2 O37 2.490(17) . ? S1 O10 1.450(4) . ? S1 O11 1.457(4) . ? S1 O9 1.485(4) . ? S1 C1 1.790(5) . ? S2 O13 1.451(4) . ? S2 O14 1.453(4) . ? S2 O12 1.480(4) . ? S2 C2 1.762(5) . ? S3 O17 1.435(4) . ? S3 O16 1.440(5) . ? S3 O15 1.470(4) . ? S3 C3 1.758(7) . ? O18 H18 0.8060 . ? O19 H19A 0.9210 . ? O19 H19B 0.8124 . ? O20 H20A 0.8868 . ? O20 H20B 0.9263 . ? O21 N1 1.216(11) . ? O22 N1 1.202(10) . ? O23 N1 1.417(12) . ? O24 H24 0.8511 . ? O25 H25A 0.9906 . ? O25 H25B 0.8742 . ? O26 H26A 0.9803 . ? O26 H26B 0.9985 . ? O27 H27A 0.9467 . ? O27 H27B 0.9435 . ? O28 C4 1.235(6) . ? O29 C7 1.236(7) . ? O30 C10 1.247(8) . ? O31 C13 1.232(8) . ? O32 C16 1.234(7) . ? O33 C19 1.232(8) . ? O34 H34 0.8601 . ? O36 H36A 0.8466 . ? O36 H36B 0.9081 . ? O37 N14 1.35(3) . ? O38 N14 1.19(3) . ? O39 N14 1.35(2) . ? O41 N15 1.218(11) . ? O42 N15 1.208(10) . ? O43 N15 1.411(14) . ? O44 H44 0.8412 . ? N2 C4 1.358(8) . ? N2 C22 1.426(7) . ? N2 C5 1.466(7) . ? N3 C4 1.374(9) . ? N3 C8 1.421(9) . ? N3 C6 1.456(7) . ? N4 C7 1.333(10) . ? N4 C9 1.440(10) . ? N4 C6 1.455(7) . ? N5 C7 1.378(9) . ? N5 C23 1.435(7) . ? N5 C5 1.453(7) . ? N6 C10 1.383(8) . ? N6 C11 1.442(9) . ? N6 C8 1.447(8) . ? N7 C10 1.345(8) . ? N7 C12 1.437(8) . ? N7 C14 1.459(8) . ? N8 C13 1.364(7) . ? N8 C15 1.460(10) . ? N8 C12 1.460(9) . ? N9 C13 1.361(9) . ? N9 C11 1.439(8) . ? N9 C9 1.466(8) . ? N10 C16 1.354(9) . ? N10 C14 1.398(10) . ? N10 C17 1.454(8) . ? N11 C16 1.341(9) . ? N11 C18 1.454(8) . ? N11 C20 1.458(7) . ? N12 C19 1.355(9) . ? N12 C21 1.445(6) . ? N12 C18 1.456(8) . ? N13 C19 1.327(11) . ? N13 C15 1.445(11) . ? N13 C17 1.465(7) . ? C1 C2 1.530(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.385(15) 7 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.544(11) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.514(11) . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C18 1.525(12) . ? C17 H17 0.9800 . ? C18 H18A 0.9800 . ? C20 N11 1.458(7) 6 ? C20 H20C 0.9700 . ? C20 H20D 0.9700 . ? C21 N12 1.445(6) 6 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N2 1.426(7) 6 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N5 1.434(7) 6 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 U1 O1 178.4(2) . . ? O2 U1 O18 91.95(15) . . ? O1 U1 O18 89.34(15) . . ? O2 U1 O18 91.95(15) . 6_565 ? O1 U1 O18 89.34(15) . 6_565 ? O18 U1 O18 69.39(19) . 6_565 ? O2 U1 O9 89.69(9) . 6_565 ? O1 U1 O9 89.85(9) . 6_565 ? O18 U1 O9 141.86(13) . 6_565 ? O18 U1 O9 72.47(12) 6_565 6_565 ? O2 U1 O9 89.69(9) . . ? O1 U1 O9 89.85(9) . . ? O18 U1 O9 72.47(12) . . ? O18 U1 O9 141.86(13) 6_565 . ? O9 U1 O9 145.66(16) 6_565 . ? O2 U1 O19 91.0(2) . . ? O1 U1 O19 87.39(19) . . ? O18 U1 O19 145.16(10) . . ? O18 U1 O19 145.16(10) 6_565 . ? O9 U1 O19 72.84(8) 6_565 . ? O9 U1 O19 72.84(8) . . ? O3 U2 O4 179.3(2) . . ? O3 U2 O18 87.37(16) . 6_565 ? O4 U2 O18 92.03(17) . 6_565 ? O3 U2 O18 87.37(16) . . ? O4 U2 O18 92.03(17) . . ? O18 U2 O18 70.16(19) 6_565 . ? O3 U2 O21 93.3(2) . . ? O4 U2 O21 87.5(3) . . ? O18 U2 O21 144.92(10) 6_565 . ? O18 U2 O21 144.92(10) . . ? O3 U2 O20 91.38(11) . . ? O4 U2 O20 88.84(11) . . ? O18 U2 O20 142.61(13) 6_565 . ? O18 U2 O20 72.45(13) . . ? O21 U2 O20 72.47(9) . . ? O3 U2 O20 91.38(11) . 6_565 ? O4 U2 O20 88.84(11) . 6_565 ? O18 U2 O20 72.45(13) 6_565 6_565 ? O18 U2 O20 142.61(13) . 6_565 ? O21 U2 O20 72.47(9) . 6_565 ? O20 U2 O20 144.94(18) . 6_565 ? O6 U3 O5 179.9(2) . . ? O6 U3 O24 90.58(15) . . ? O5 U3 O24 89.50(16) . . ? O6 U3 O24 90.58(15) . 6 ? O5 U3 O24 89.50(16) . 6 ? O24 U3 O24 70.16(18) . 6 ? O6 U3 O25 91.5(2) . . ? O5 U3 O25 88.4(2) . . ? O24 U3 O25 144.86(9) . . ? O24 U3 O25 144.86(9) 6 . ? O6 U3 O15 90.10(10) . 6 ? O5 U3 O15 89.87(10) . 6 ? O24 U3 O15 144.23(13) . 6 ? O24 U3 O15 74.07(13) 6 6 ? O25 U3 O15 70.85(9) . 6 ? O6 U3 O15 90.10(10) . . ? O5 U3 O15 89.87(10) . . ? O24 U3 O15 74.07(13) . . ? O24 U3 O15 144.23(13) 6 . ? O25 U3 O15 70.85(9) . . ? O15 U3 O15 141.69(19) 6 . ? O8 U4 O7 178.0(2) . . ? O8 U4 O24 92.16(15) . 6 ? O7 U4 O24 89.43(15) . 6 ? O8 U4 O24 92.16(15) . . ? O7 U4 O24 89.43(15) . . ? O24 U4 O24 70.91(18) 6 . ? O8 U4 O27 90.9(2) . . ? O7 U4 O27 87.1(2) . . ? O24 U4 O27 144.39(9) 6 . ? O24 U4 O27 144.39(9) . . ? O8 U4 O26 88.78(9) . . ? O7 U4 O26 90.63(9) . . ? O24 U4 O26 142.95(12) 6 . ? O24 U4 O26 72.04(12) . . ? O27 U4 O26 72.57(8) . . ? O8 U4 O26 88.78(9) . 6 ? O7 U4 O26 90.63(9) . 6 ? O24 U4 O26 72.04(12) 6 6 ? O24 U4 O26 142.95(12) . 6 ? O27 U4 O26 72.57(8) . 6 ? O26 U4 O26 145.00(16) . 6 ? O28 Dy1 O28 77.4(2) . 6 ? O28 Dy1 O12 74.16(13) . . ? O28 Dy1 O12 120.67(14) 6 . ? O28 Dy1 O12 120.67(14) . 6 ? O28 Dy1 O12 74.16(13) 6 6 ? O12 Dy1 O12 77.6(2) . 6 ? O28 Dy1 O36 140.87(14) . 6 ? O28 Dy1 O36 78.53(15) 6 6 ? O12 Dy1 O36 144.97(14) . 6 ? O12 Dy1 O36 80.92(16) 6 6 ? O28 Dy1 O36 78.53(15) . . ? O28 Dy1 O36 140.87(14) 6 . ? O12 Dy1 O36 80.92(16) . . ? O12 Dy1 O36 144.97(14) 6 . ? O36 Dy1 O36 102.4(2) 6 . ? O28 Dy1 O34 140.84(11) . . ? O28 Dy1 O34 140.84(11) 6 . ? O12 Dy1 O34 76.18(13) . . ? O12 Dy1 O34 76.18(13) 6 . ? O36 Dy1 O34 72.00(12) 6 . ? O36 Dy1 O34 72.00(12) . . ? O28 Dy1 O35 75.29(17) . . ? O28 Dy1 O35 75.29(17) 6 . ? O12 Dy1 O35 140.57(11) . . ? O12 Dy1 O35 140.57(11) 6 . ? O36 Dy1 O35 69.02(16) 6 . ? O36 Dy1 O35 69.02(16) . . ? O34 Dy1 O35 115.6(2) . . ? Dy2 Dy2 O40 137.2(3) 5_557 . ? Dy2 Dy2 O40 137.2(3) 5_557 6 ? O40 Dy2 O40 68.7(6) . 6 ? Dy2 Dy2 O33 80.73(15) 5_557 . ? O40 Dy2 O33 87.0(3) . . ? O40 Dy2 O33 141.6(3) 6 . ? Dy2 Dy2 O33 80.73(15) 5_557 6 ? O40 Dy2 O33 141.6(3) . 6 ? O40 Dy2 O33 87.0(3) 6 6 ? O33 Dy2 O33 95.5(3) . 6 ? Dy2 Dy2 O33 65.78(14) 5_557 2_557 ? O40 Dy2 O33 71.7(3) . 2_557 ? O40 Dy2 O33 117.3(3) 6 2_557 ? O33 Dy2 O33 79.7(3) . 2_557 ? O33 Dy2 O33 146.51(10) 6 2_557 ? Dy2 Dy2 O33 65.78(14) 5_557 5_557 ? O40 Dy2 O33 117.3(3) . 5_557 ? O40 Dy2 O33 71.7(3) 6 5_557 ? O33 Dy2 O33 146.51(10) . 5_557 ? O33 Dy2 O33 79.7(3) 6 5_557 ? O33 Dy2 O33 86.3(3) 2_557 5_557 ? Dy2 Dy2 O37 136.2(4) 5_557 . ? O40 Dy2 O37 74.5(4) . . ? O40 Dy2 O37 74.5(4) 6 . ? O33 Dy2 O37 70.4(3) . . ? O33 Dy2 O37 70.4(3) 6 . ? O33 Dy2 O37 135.51(17) 2_557 . ? O33 Dy2 O37 135.51(17) 5_557 . ? O10 S1 O11 113.5(2) . . ? O10 S1 O9 110.9(2) . . ? O11 S1 O9 113.0(2) . . ? O10 S1 C1 107.4(3) . . ? O11 S1 C1 107.3(2) . . ? O9 S1 C1 104.1(2) . . ? O13 S2 O14 112.6(2) . . ? O13 S2 O12 113.8(3) . . ? O14 S2 O12 111.7(2) . . ? O13 S2 C2 105.3(2) . . ? O14 S2 C2 107.0(3) . . ? O12 S2 C2 105.7(2) . . ? O17 S3 O16 113.6(3) . . ? O17 S3 O15 113.2(3) . . ? O16 S3 O15 110.3(3) . . ? O17 S3 C3 110.5(4) . . ? O16 S3 C3 104.4(4) . . ? O15 S3 C3 104.1(3) . . ? S1 O9 U1 140.5(2) . . ? S2 O12 Dy1 140.5(2) . . ? S3 O15 U3 143.0(2) . . ? U2 O18 U1 108.53(17) . . ? U2 O18 H18 110.6 . . ? U1 O18 H18 114.2 . . ? U1 O19 H19A 127.3 . . ? U1 O19 H19B 127.1 . . ? H19A O19 H19B 105.7 . . ? U2 O20 H20A 131.3 . . ? U2 O20 H20B 128.6 . . ? H20A O20 H20B 99.5 . . ? N1 O21 U2 127.4(7) . . ? U4 O24 U3 107.96(15) . . ? U4 O24 H24 107.2 . . ? U3 O24 H24 106.9 . . ? U3 O25 H25A 142.7 . . ? U3 O25 H25B 121.2 . . ? H25A O25 H25B 96.1 . . ? U4 O26 H26A 126.1 . . ? U4 O26 H26B 135.6 . . ? H26A O26 H26B 97.9 . . ? U4 O27 H27A 143.2 . . ? U4 O27 H27B 121.6 . . ? H27A O27 H27B 95.2 . . ? C4 O28 Dy1 158.2(5) . . ? C19 O33 Dy2 140.5(6) . . ? C19 O33 Dy2 144.8(7) . 5_557 ? Dy1 O34 H34 117.0 . . ? Dy1 O36 H36A 109.0 . . ? Dy1 O36 H36B 104.9 . . ? H36A O36 H36B 103.5 . . ? N14 O37 Dy2 135.8(15) . . ? O22 N1 O21 125.5(11) . . ? O22 N1 O23 113.0(7) . . ? O21 N1 O23 105.4(7) . . ? C4 N2 C22 123.6(5) . . ? C4 N2 C5 110.7(6) . . ? C22 N2 C5 125.6(6) . . ? C4 N3 C8 122.8(5) . . ? C4 N3 C6 111.0(6) . . ? C8 N3 C6 124.8(6) . . ? C7 N4 C9 123.3(6) . . ? C7 N4 C6 112.4(6) . . ? C9 N4 C6 124.1(7) . . ? C7 N5 C23 124.3(5) . . ? C7 N5 C5 109.9(6) . . ? C23 N5 C5 123.3(6) . . ? C10 N6 C11 110.4(6) . . ? C10 N6 C8 122.4(5) . . ? C11 N6 C8 123.3(6) . . ? C10 N7 C12 111.9(6) . . ? C10 N7 C14 124.0(5) . . ? C12 N7 C14 123.7(6) . . ? C13 N8 C15 122.3(6) . . ? C13 N8 C12 111.0(6) . . ? C15 N8 C12 124.0(6) . . ? C13 N9 C11 112.7(6) . . ? C13 N9 C9 123.1(6) . . ? C11 N9 C9 123.9(6) . . ? C16 N10 C14 123.4(6) . . ? C16 N10 C17 111.6(7) . . ? C14 N10 C17 124.9(7) . . ? C16 N11 C18 112.4(7) . . ? C16 N11 C20 123.4(5) . . ? C18 N11 C20 122.7(6) . . ? C19 N12 C21 123.8(7) . . ? C19 N12 C18 112.2(7) . . ? C21 N12 C18 123.9(6) . . ? C19 N13 C15 121.9(6) . . ? C19 N13 C17 112.8(7) . . ? C15 N13 C17 123.8(8) . . ? O38 N14 O37 119(2) . . ? O38 N14 O39 117(2) . . ? O37 N14 O39 116.2(19) . . ? O42 N15 O41 125.8(10) . . ? O42 N15 O43 111.1(8) . . ? O41 N15 O43 113.4(8) . . ? C2 C1 S1 109.9(3) . . ? C2 C1 H1A 109.7 . . ? S1 C1 H1A 109.7 . . ? C2 C1 H1B 109.7 . . ? S1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 C2 S2 111.8(3) . . ? C1 C2 H2A 109.3 . . ? S2 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? S2 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C3 C3 S3 119.6(9) 7 . ? C3 C3 H3A 107.4 7 . ? S3 C3 H3A 107.4 . . ? C3 C3 H3B 107.4 7 . ? S3 C3 H3B 107.4 . . ? H3A C3 H3B 107.0 . . ? O28 C4 N2 125.0(7) . . ? O28 C4 N3 124.8(6) . . ? N2 C4 N3 110.2(5) . . ? N5 C5 N2 113.2(6) . . ? N5 C5 C6 104.1(5) . . ? N2 C5 C6 103.5(5) . . ? N5 C5 H5 111.8 . . ? N2 C5 H5 111.8 . . ? C6 C5 H5 111.8 . . ? N4 C6 N3 112.6(5) . . ? N4 C6 C5 102.5(6) . . ? N3 C6 C5 103.5(6) . . ? N4 C6 H6 112.5 . . ? N3 C6 H6 112.5 . . ? C5 C6 H6 112.5 . . ? O29 C7 N4 125.8(7) . . ? O29 C7 N5 124.0(8) . . ? N4 C7 N5 110.2(5) . . ? N3 C8 N6 112.8(5) . . ? N3 C8 H8A 109.0 . . ? N6 C8 H8A 109.0 . . ? N3 C8 H8B 109.0 . . ? N6 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N4 C9 N9 112.9(5) . . ? N4 C9 H9A 109.0 . . ? N9 C9 H9A 109.0 . . ? N4 C9 H9B 109.0 . . ? N9 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? O30 C10 N7 125.9(6) . . ? O30 C10 N6 125.2(6) . . ? N7 C10 N6 108.9(6) . . ? N9 C11 N6 114.4(6) . . ? N9 C11 C12 103.5(6) . . ? N6 C11 C12 103.9(5) . . ? N9 C11 H11 111.5 . . ? N6 C11 H11 111.5 . . ? C12 C11 H11 111.5 . . ? N7 C12 N8 114.5(7) . . ? N7 C12 C11 104.2(6) . . ? N8 C12 C11 103.8(5) . . ? N7 C12 H12 111.3 . . ? N8 C12 H12 111.3 . . ? C11 C12 H12 111.3 . . ? O31 C13 N9 126.4(6) . . ? O31 C13 N8 125.6(7) . . ? N9 C13 N8 108.0(6) . . ? N10 C14 N7 115.1(6) . . ? N10 C14 H14A 108.5 . . ? N7 C14 H14A 108.5 . . ? N10 C14 H14B 108.5 . . ? N7 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N13 C15 N8 112.7(6) . . ? N13 C15 H15A 109.1 . . ? N8 C15 H15A 109.1 . . ? N13 C15 H15B 109.1 . . ? N8 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? O32 C16 N11 126.0(7) . . ? O32 C16 N10 124.7(7) . . ? N11 C16 N10 109.2(5) . . ? N10 C17 N13 113.9(5) . . ? N10 C17 C18 103.7(6) . . ? N13 C17 C18 102.8(7) . . ? N10 C17 H17 111.9 . . ? N13 C17 H17 111.9 . . ? C18 C17 H17 111.9 . . ? N11 C18 N12 114.4(6) . . ? N11 C18 C17 103.0(6) . . ? N12 C18 C17 103.1(5) . . ? N11 C18 H18A 111.9 . . ? N12 C18 H18A 111.9 . . ? C17 C18 H18A 111.9 . . ? O33 C19 N13 124.8(8) . . ? O33 C19 N12 126.3(9) . . ? N13 C19 N12 108.9(6) . . ? N11 C20 N11 113.5(7) 6 . ? N11 C20 H20C 108.9 6 . ? N11 C20 H20C 108.9 . . ? N11 C20 H20D 108.9 6 . ? N11 C20 H20D 108.9 . . ? H20C C20 H20D 107.7 . . ? N12 C21 N12 115.4(7) 6 . ? N12 C21 H21A 108.4 6 . ? N12 C21 H21A 108.4 . . ? N12 C21 H21B 108.4 6 . ? N12 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? N2 C22 N2 113.4(6) . 6 ? N2 C22 H22A 108.9 . . ? N2 C22 H22A 108.9 6 . ? N2 C22 H22B 108.9 . . ? N2 C22 H22B 108.9 6 . ? H22A C22 H22B 107.7 . . ? N5 C23 N5 114.5(6) 6 . ? N5 C23 H23A 108.6 6 . ? N5 C23 H23A 108.6 . . ? N5 C23 H23B 108.6 6 . ? N5 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? 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 O18 H18 O16 0.81 1.97 2.775(5) 172.0 . O19 H19A O44 0.92 1.81 2.723(7) 173.3 . O19 H19B O46 0.81 1.87 2.643(9) 158.1 . O20 H20A O17 0.89 1.97 2.813(6) 157.9 . O20 H20B O31 0.93 1.90 2.825(6) 177.7 1_554 O24 H24 O10 0.85 1.93 2.762(5) 166.8 . O25 H25A O4 0.99 1.85 2.773(7) 152.9 7 O25 H25B O47 0.87 1.70 2.537(8) 158.7 . O26 H26A O11 0.98 1.87 2.845(5) 173.1 . O26 H26B O14 1.00 1.76 2.733(5) 165.3 7_556 O27 H27A O44 0.95 1.87 2.734(7) 149.8 7_556 O27 H27B O45 0.94 1.76 2.643(10) 153.8 7_556 O34 H34 O32 0.86 2.21 2.679(6) 114.3 2_556 O36 H36A O30 0.85 2.10 2.780(6) 136.6 . O36 H36B O48 0.91 2.02 2.778(12) 140.5 . O44 H44 O13 0.84 1.96 2.773(5) 162.2 7_556 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 863487' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H86 Er1.50 N26.50 O66.50 S6 U4' _chemical_formula_weight 3421.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 31.0881(9) _cell_length_b 14.1832(3) _cell_length_c 20.8347(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.8691(15) _cell_angle_gamma 90.00 _cell_volume 9165.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 183651 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6486 _exptl_absorpt_coefficient_mu 8.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.372 _exptl_absorpt_correction_T_max 0.545 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (513 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 183651 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 30.51 _reflns_number_total 14484 _reflns_number_gt 11056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The atom Er2 and the associated nitrate ion were given 0.5 occupancy factors so as to account for the close contact between Er2 and its image by symmetry and to retain acceptable displacement parameters. One O atom in each of the three nitrate ions is disordered around a symmetry plane, the disorder on the associated N atom being unresolved. Several solvent water molecules were given 0.5 occupancy factors so as to to account for too close contacts and/or to retain acceptable displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to O atoms were found on a Fourier-difference map, except for those of O35, O40 and four solvent water molecules, and all the others were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+41.4195P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14484 _refine_ls_number_parameters 754 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.737 _refine_diff_density_min -4.456 _refine_diff_density_rms 0.184 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 U1 U 0.156473(7) 0.5000 0.245690(10) 0.02091(6) Uani 1 2 d S . . U2 U 0.126088(8) 0.5000 0.067480(11) 0.02848(7) Uani 1 2 d S . . U3 U 0.256466(8) 0.0000 0.156145(10) 0.02209(6) Uani 1 2 d S . . U4 U 0.284640(8) 0.0000 0.334814(10) 0.02084(6) Uani 1 2 d S . . Er1 Er 0.090090(10) 0.0000 0.546588(13) 0.02868(8) Uani 1 2 d S . . Er2 Er 0.01423(2) 0.0000 0.97679(3) 0.0648(3) Uani 0.50 2 d SP . . S1 S 0.18751(4) 0.26916(9) 0.31533(5) 0.0240(2) Uani 1 1 d . . . S2 S 0.17053(4) 0.17083(10) 0.50931(5) 0.0289(3) Uani 1 1 d . . . S3 S 0.22485(4) 0.23791(9) 0.09507(5) 0.0286(3) Uani 1 1 d . . . O1 O 0.09948(14) 0.5000 0.2485(2) 0.0220(9) Uani 1 2 d S . . O2 O 0.21352(15) 0.5000 0.2455(2) 0.0295(11) Uani 1 2 d S . . O3 O 0.07492(16) 0.5000 0.0992(2) 0.0336(12) Uani 1 2 d S . . O4 O 0.17810(18) 0.5000 0.0367(2) 0.0447(15) Uani 1 2 d S . . O5 O 0.31354(15) 0.0000 0.1537(2) 0.0300(11) Uani 1 2 d S . . O6 O 0.19966(15) 0.0000 0.1580(2) 0.0255(10) Uani 1 2 d S . . O7 O 0.33770(15) 0.0000 0.3082(2) 0.0266(10) Uani 1 2 d S . . O8 O 0.23240(15) 0.0000 0.3640(2) 0.0262(10) Uani 1 2 d S . . O9 O 0.15861(11) 0.3372(3) 0.28031(15) 0.0279(7) Uani 1 1 d . . . O10 O 0.18710(11) 0.1790(3) 0.28260(15) 0.0303(8) Uani 1 1 d . . . O11 O 0.23069(11) 0.3061(3) 0.33062(16) 0.0304(8) Uani 1 1 d . . . O12 O 0.13511(12) 0.1030(3) 0.49481(15) 0.0341(8) Uani 1 1 d . . . O13 O 0.20551(12) 0.1329(3) 0.55121(16) 0.0402(10) Uani 1 1 d . . . O14 O 0.15484(12) 0.2612(3) 0.53196(16) 0.0331(8) Uani 1 1 d . . . O15 O 0.25439(12) 0.1623(3) 0.11790(16) 0.0358(9) Uani 1 1 d . . . O16 O 0.22801(14) 0.3159(4) 0.1393(2) 0.0619(15) Uani 1 1 d . . . O17 O 0.18159(14) 0.2062(3) 0.0799(2) 0.0515(12) Uani 1 1 d . . . O18 O 0.14964(11) 0.4064(3) 0.15323(14) 0.0295(8) Uani 1 1 d . . . H18 H 0.1713 0.3788 0.1455 0.035 Uiso 1 1 d R . . O19 O 0.16074(16) 0.5000 0.3624(2) 0.0287(11) Uani 1 2 d S . . H19A H 0.1852 0.5000 0.3898 0.034 Uiso 1 2 d SR . . H19B H 0.1407 0.5000 0.3854 0.034 Uiso 1 2 d SR . . O20 O 0.11732(13) 0.3322(3) 0.03341(17) 0.0412(10) Uani 1 1 d . . . H20A H 0.1325 0.2810 0.0443 0.049 Uiso 1 1 d R . . H20B H 0.0993 0.3075 0.0005 0.049 Uiso 1 1 d R . . O21 O 0.0959(2) 0.5000 -0.0424(3) 0.0579(19) Uani 1 2 d S . . O22 O 0.0438(2) 0.5000 -0.1162(3) 0.0559(19) Uani 1 2 d S . . O23 O 0.0380(3) 0.4302(8) -0.0246(4) 0.058(3) Uani 0.50 1 d P . . O24 O 0.26288(10) 0.0947(2) 0.24808(14) 0.0243(7) Uani 1 1 d . . . H24 H 0.2376 0.1142 0.2545 0.029 Uiso 1 1 d R . . O25 O 0.25182(18) 0.0000 0.0401(2) 0.0439(15) Uani 1 2 d S . . H25A H 0.2696 0.0000 0.0024 0.053 Uiso 1 2 d SR . . H25B H 0.2269 0.0000 0.0181 0.053 Uiso 1 2 d SR . . O26 O 0.29248(11) 0.1670(3) 0.36972(15) 0.0285(7) Uani 1 1 d . . . H26A H 0.2725 0.2187 0.3581 0.034 Uiso 1 1 d R . . H26B H 0.3120 0.2023 0.4013 0.034 Uiso 1 1 d R . . O27 O 0.31740(17) 0.0000 0.4425(2) 0.0332(12) Uani 1 2 d S . . H27A H 0.3112 0.0000 0.4863 0.040 Uiso 1 2 d SR . . H27B H 0.3476 0.0000 0.4507 0.040 Uiso 1 2 d SR . . O28 O 0.11822(12) 0.1031(3) 0.62498(15) 0.0416(10) Uani 1 1 d . . . O29 O 0.15116(14) 0.1309(4) 0.90737(18) 0.0645(16) Uani 1 1 d . . . O30 O 0.01966(14) 0.2281(3) 0.63880(19) 0.0447(10) Uani 1 1 d . . . O31 O 0.06439(15) 0.2582(5) 0.9303(2) 0.0666(16) Uani 1 1 d . . . O32 O -0.07385(14) 0.1239(3) 0.65647(17) 0.0453(11) Uani 1 1 d . . . O33 O -0.02880(16) 0.1164(5) 0.9407(2) 0.0826(19) Uani 1 1 d U . . O34 O 0.06200(16) 0.0000 0.4387(2) 0.0284(11) Uani 1 2 d S . . H34 H 0.0475 0.0489 0.4258 0.034 Uiso 1 1 d R . . O35 O 0.0384(2) 0.0000 0.6284(3) 0.062(2) Uani 1 2 d S . . O36 O 0.04359(13) 0.1297(3) 0.53206(18) 0.0443(10) Uani 1 1 d . . . H36A H 0.0499 0.1700 0.5611 0.053 Uiso 1 1 d R . . H36B H 0.0513 0.1584 0.4956 0.053 Uiso 1 1 d R . . O37 O 0.0101(4) 0.0000 0.8583(5) 0.058(4) Uani 0.50 2 d SP . . O38 O 0.0753(5) 0.0000 0.8278(8) 0.093(6) Uani 0.50 2 d SP . . O39 O 0.0256(6) 0.0463(13) 0.7570(7) 0.054(5) Uani 0.25 1 d PU . . O40 O 0.0679(4) 0.0881(8) 0.9523(4) 0.067(3) Uani 0.50 1 d PU . . O41 O 0.4444(2) 0.0000 0.3470(4) 0.075(2) Uani 1 2 d S . . O42 O 0.5120(2) 0.0000 0.3344(3) 0.068(2) Uani 1 2 d S . . O43 O 0.4874(4) 0.0556(11) 0.4207(5) 0.091(4) Uani 0.50 1 d P . . O44 O 0.22905(17) 0.5000 0.4512(2) 0.0372(13) Uani 1 2 d S . . H44 H 0.2460 0.4541 0.4571 0.045 Uiso 1 1 d R . . O45 O 0.1018(3) 0.4480(8) 0.5359(4) 0.065(3) Uani 0.50 1 d P . . O46 O 0.0874(3) 0.4645(7) 0.4149(4) 0.059(3) Uani 0.50 1 d P . . O47 O 0.17211(19) 0.0000 0.0030(3) 0.0469(16) Uani 1 2 d S . . O48 O 0.0606(3) 0.2889(7) 0.4609(4) 0.062(3) Uani 0.50 1 d P . . N1 N 0.0577(3) 0.5000 -0.0610(4) 0.073(3) Uani 1 2 d S . . N2 N 0.17668(14) 0.0848(5) 0.69764(19) 0.0496(15) Uani 1 1 d . . . N3 N 0.13550(16) 0.2121(4) 0.7041(2) 0.0449(14) Uani 1 1 d . . . N4 N 0.15209(16) 0.2277(5) 0.8192(2) 0.0520(15) Uani 1 1 d . . . N5 N 0.18297(14) 0.0850(5) 0.81526(19) 0.0461(14) Uani 1 1 d . . . N6 N 0.06798(19) 0.2904(4) 0.7175(2) 0.0465(13) Uani 1 1 d . . . N7 N -0.00164(19) 0.3006(4) 0.7305(2) 0.0522(15) Uani 1 1 d . . . N8 N 0.01617(18) 0.2996(4) 0.8464(2) 0.0522(15) Uani 1 1 d . . . N9 N 0.08562(19) 0.3109(4) 0.8325(2) 0.0469(13) Uani 1 1 d . . . N10 N -0.06958(18) 0.2222(5) 0.7442(2) 0.0533(16) Uani 1 1 d . . . N11 N -0.10197(15) 0.0852(5) 0.7525(2) 0.0561(17) Uani 1 1 d . . . N12 N -0.08726(16) 0.0855(5) 0.8695(2) 0.069(2) Uani 1 1 d D . . N13 N -0.05035(17) 0.2156(6) 0.8600(3) 0.073(2) Uani 1 1 d . . . N14 N 0.0372(5) 0.0000 0.8135(6) 0.062(5) Uani 0.50 2 d SP . . N15 N 0.4814(3) 0.0000 0.3663(4) 0.083(4) Uani 1 2 d S . . C1 C 0.16325(15) 0.2520(4) 0.3898(2) 0.0266(10) Uani 1 1 d . . . H1A H 0.1581 0.3126 0.4095 0.032 Uiso 1 1 calc R . . H1B H 0.1358 0.2203 0.3821 0.032 Uiso 1 1 calc R . . C2 C 0.19323(15) 0.1925(4) 0.4351(2) 0.0284(11) Uani 1 1 d . . . H2A H 0.2205 0.2251 0.4430 0.034 Uiso 1 1 calc R . . H2B H 0.1989 0.1328 0.4145 0.034 Uiso 1 1 calc R . . C3 C 0.2479(3) 0.2830(5) 0.0259(3) 0.0560(19) Uani 1 1 d . . . H3A H 0.2305 0.3356 0.0096 0.067 Uiso 1 1 calc R . . H3B H 0.2764 0.3073 0.0388 0.067 Uiso 1 1 calc R . . C4 C 0.14142(17) 0.1306(5) 0.6713(2) 0.0406(15) Uani 1 1 d . . . C5 C 0.19434(18) 0.1314(6) 0.7562(2) 0.052(2) Uani 1 1 d . . . H5 H 0.2255 0.1419 0.7556 0.063 Uiso 1 1 calc R . . C6 C 0.1689(2) 0.2252(6) 0.7569(3) 0.054(2) Uani 1 1 d . . . H6 H 0.1874 0.2797 0.7496 0.064 Uiso 1 1 calc R . . C7 C 0.16099(18) 0.1465(6) 0.8518(3) 0.053(2) Uani 1 1 d . . . C8 C 0.1061(2) 0.2846(5) 0.6808(3) 0.0526(18) Uani 1 1 d . . . H8A H 0.0972 0.2722 0.6361 0.063 Uiso 1 1 calc R . . H8B H 0.1208 0.3449 0.6829 0.063 Uiso 1 1 calc R . . C9 C 0.1316(2) 0.3077(6) 0.8471(3) 0.0577(19) Uani 1 1 d . . . H9A H 0.1443 0.3650 0.8314 0.069 Uiso 1 1 calc R . . H9B H 0.1374 0.3060 0.8934 0.069 Uiso 1 1 calc R . . C10 C 0.0278(2) 0.2679(4) 0.6907(3) 0.0407(14) Uani 1 1 d . . . C11 C 0.0660(3) 0.3497(4) 0.7739(3) 0.057(2) Uani 1 1 d . . . H11 H 0.0765 0.4135 0.7660 0.069 Uiso 1 1 calc R . . C12 C 0.0176(3) 0.3497(4) 0.7856(3) 0.057(2) Uani 1 1 d . . . H12 H 0.0063 0.4139 0.7885 0.068 Uiso 1 1 calc R . . C13 C 0.0567(2) 0.2870(5) 0.8748(3) 0.0465(16) Uani 1 1 d . . . C14 C -0.0482(2) 0.2971(6) 0.7149(3) 0.062(2) Uani 1 1 d . . . H14A H -0.0607 0.3562 0.7279 0.075 Uiso 1 1 calc R . . H14B H -0.0534 0.2917 0.6686 0.075 Uiso 1 1 calc R . . C15 C -0.0223(2) 0.2944(7) 0.8815(3) 0.083(3) Uani 1 1 d . . . H15A H -0.0382 0.3530 0.8758 0.099 Uiso 1 1 calc R . . H15B H -0.0141 0.2872 0.9269 0.099 Uiso 1 1 calc R . . C16 C -0.08067(18) 0.1402(6) 0.7128(3) 0.0474(17) Uani 1 1 d . . . C17 C -0.0845(2) 0.2248(7) 0.8089(3) 0.071(3) Uani 1 1 d . . . H17 H -0.1030 0.2795 0.8154 0.085 Uiso 1 1 calc R . . C18 C -0.1090(2) 0.1320(7) 0.8133(3) 0.071(3) Uani 1 1 d . . . H18A H -0.1397 0.1422 0.8187 0.086 Uiso 1 1 calc R . . C19 C -0.0530(2) 0.1377(9) 0.8933(3) 0.078(3) Uani 1 1 d . . . C20 C -0.1243(3) 0.0000 0.7310(4) 0.057(3) Uani 1 2 d S . . H20C H -0.1529 0.0000 0.7470 0.069 Uiso 1 2 calc SR . . H20D H -0.1277 0.0000 0.6844 0.069 Uiso 1 2 calc SR . . C21 C -0.1021(4) 0.0000 0.8982(4) 0.072(3) Uani 1 2 d SDU . . H21A H -0.0925 0.0000 0.9435 0.086 Uiso 1 2 calc SR . . H21B H -0.1333 0.0000 0.8952 0.086 Uiso 1 2 calc SR . . C22 C 0.1938(2) 0.0000 0.6718(3) 0.049(3) Uani 1 2 d S . . H22A H 0.2248 0.0000 0.6803 0.059 Uiso 1 2 calc SR . . H22B H 0.1878 0.0000 0.6256 0.059 Uiso 1 2 calc SR . . C23 C 0.2031(2) 0.0000 0.8397(3) 0.052(3) Uani 1 2 d S . . H23A H 0.2027 0.0000 0.8862 0.062 Uiso 1 2 calc SR . . H23B H 0.2330 0.0000 0.8291 0.062 Uiso 1 2 calc SR . . 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 U1 0.01718(11) 0.02923(14) 0.01620(10) 0.000 0.00022(8) 0.000 U2 0.02346(13) 0.04434(17) 0.01734(11) 0.000 -0.00084(9) 0.000 U3 0.01917(11) 0.03071(14) 0.01622(10) 0.000 -0.00005(8) 0.000 U4 0.02013(11) 0.02592(13) 0.01623(10) 0.000 -0.00059(8) 0.000 Er1 0.01880(14) 0.0507(2) 0.01627(12) 0.000 -0.00085(10) 0.000 Er2 0.0186(3) 0.1598(11) 0.0157(3) 0.000 -0.0013(2) 0.000 S1 0.0214(5) 0.0314(6) 0.0188(5) 0.0014(4) -0.0012(4) 0.0031(5) S2 0.0266(6) 0.0431(8) 0.0169(5) -0.0001(5) -0.0001(4) 0.0009(5) S3 0.0356(6) 0.0293(7) 0.0214(5) 0.0006(5) 0.0048(4) 0.0000(5) O1 0.019(2) 0.023(2) 0.025(2) 0.000 0.0021(17) 0.000 O2 0.019(2) 0.045(3) 0.025(2) 0.000 0.0025(18) 0.000 O3 0.023(2) 0.047(3) 0.030(3) 0.000 0.000(2) 0.000 O4 0.031(3) 0.077(5) 0.027(3) 0.000 0.007(2) 0.000 O5 0.018(2) 0.042(3) 0.029(2) 0.000 0.0015(19) 0.000 O6 0.023(2) 0.031(3) 0.022(2) 0.000 -0.0008(17) 0.000 O7 0.022(2) 0.034(3) 0.024(2) 0.000 0.0020(18) 0.000 O8 0.026(2) 0.030(3) 0.024(2) 0.000 0.0046(18) 0.000 O9 0.0256(17) 0.034(2) 0.0236(15) 0.0017(14) -0.0038(13) 0.0045(15) O10 0.0318(18) 0.035(2) 0.0238(16) 0.0002(14) -0.0019(13) 0.0080(16) O11 0.0233(17) 0.041(2) 0.0265(16) 0.0046(15) -0.0021(13) -0.0029(16) O12 0.036(2) 0.045(2) 0.0219(16) -0.0001(15) 0.0052(14) -0.0068(18) O13 0.032(2) 0.067(3) 0.0210(16) 0.0057(17) -0.0024(14) 0.010(2) O14 0.0315(19) 0.043(2) 0.0243(16) -0.0073(15) -0.0016(14) 0.0019(17) O15 0.037(2) 0.042(2) 0.0280(17) 0.0113(16) -0.0041(15) -0.0005(18) O16 0.038(2) 0.062(3) 0.083(3) -0.044(3) -0.010(2) 0.015(2) O17 0.043(2) 0.041(3) 0.066(3) 0.018(2) -0.023(2) -0.006(2) O18 0.0261(17) 0.042(2) 0.0202(15) -0.0040(14) 0.0003(12) 0.0096(16) O19 0.029(3) 0.041(3) 0.017(2) 0.000 0.0008(18) 0.000 O20 0.044(2) 0.048(3) 0.0298(18) -0.0078(17) -0.0134(16) 0.012(2) O21 0.050(4) 0.096(6) 0.025(3) 0.000 -0.014(3) 0.000 O22 0.083(5) 0.038(4) 0.040(3) 0.000 -0.038(3) 0.000 O23 0.053(6) 0.072(7) 0.047(5) -0.001(5) -0.007(4) -0.019(5) O24 0.0252(16) 0.0294(19) 0.0179(14) 0.0007(13) -0.0021(12) 0.0049(14) O25 0.035(3) 0.082(5) 0.015(2) 0.000 0.002(2) 0.000 O26 0.0287(18) 0.0302(19) 0.0258(16) -0.0028(14) -0.0042(13) -0.0008(15) O27 0.035(3) 0.047(3) 0.018(2) 0.000 -0.0043(19) 0.000 O28 0.0287(19) 0.080(3) 0.0157(15) -0.0018(17) -0.0020(13) -0.011(2) O29 0.044(3) 0.130(5) 0.0197(17) 0.008(2) 0.0048(16) 0.023(3) O30 0.048(2) 0.046(3) 0.039(2) -0.0159(19) -0.0083(18) 0.003(2) O31 0.039(2) 0.123(5) 0.036(2) -0.003(3) -0.0161(19) 0.002(3) O32 0.047(2) 0.063(3) 0.0252(17) -0.0104(18) 0.0000(16) 0.018(2) O33 0.044(3) 0.166(6) 0.034(2) 0.001(3) -0.0185(19) 0.004(3) O34 0.030(3) 0.034(3) 0.021(2) 0.000 -0.0024(18) 0.000 O35 0.039(4) 0.104(6) 0.045(4) 0.000 0.019(3) 0.000 O36 0.040(2) 0.060(3) 0.0320(19) -0.0115(19) -0.0011(16) 0.006(2) O37 0.033(6) 0.115(13) 0.026(5) 0.000 0.001(5) 0.000 O38 0.029(7) 0.17(2) 0.081(11) 0.000 0.023(7) 0.000 O39 0.060(8) 0.072(9) 0.029(6) 0.001(6) -0.004(6) 0.019(7) O40 0.081(6) 0.078(6) 0.041(4) -0.015(4) -0.013(4) 0.051(5) O41 0.044(4) 0.083(6) 0.096(6) 0.000 -0.005(4) 0.000 O42 0.050(4) 0.111(7) 0.044(4) 0.000 0.010(3) 0.000 O43 0.080(8) 0.139(13) 0.056(6) -0.014(7) 0.010(6) 0.010(7) O44 0.031(3) 0.053(4) 0.027(2) 0.000 0.001(2) 0.000 O45 0.035(5) 0.107(9) 0.053(5) 0.017(5) 0.004(4) -0.002(5) O46 0.039(4) 0.098(10) 0.040(4) -0.005(4) 0.007(3) -0.003(4) O47 0.034(3) 0.076(5) 0.030(3) 0.000 0.000(2) 0.000 O48 0.068(7) 0.064(7) 0.056(6) 0.031(5) 0.026(5) 0.019(5) N1 0.058(6) 0.122(9) 0.036(4) 0.000 -0.026(4) 0.000 N2 0.024(2) 0.109(5) 0.0161(18) -0.002(2) 0.0007(16) -0.011(3) N3 0.044(3) 0.065(4) 0.025(2) 0.007(2) -0.0063(19) -0.032(3) N4 0.033(3) 0.097(5) 0.025(2) 0.000(3) -0.0057(19) -0.014(3) N5 0.024(2) 0.096(5) 0.0176(18) 0.000(2) -0.0008(16) -0.009(3) N6 0.065(4) 0.037(3) 0.036(2) -0.005(2) -0.010(2) -0.021(3) N7 0.065(4) 0.044(3) 0.043(3) -0.018(2) -0.024(3) 0.028(3) N8 0.052(3) 0.060(4) 0.041(3) -0.019(3) -0.020(2) 0.020(3) N9 0.059(3) 0.034(3) 0.045(3) -0.008(2) -0.017(2) -0.004(2) N10 0.047(3) 0.081(5) 0.030(2) -0.019(3) -0.012(2) 0.037(3) N11 0.025(2) 0.122(6) 0.021(2) -0.019(3) -0.0062(17) 0.005(3) N12 0.031(3) 0.151(7) 0.025(2) -0.027(3) -0.0113(19) 0.023(4) N13 0.027(3) 0.161(8) 0.030(3) -0.033(4) -0.013(2) 0.024(4) N14 0.048(9) 0.121(17) 0.017(6) 0.000 0.005(6) 0.000 N15 0.043(5) 0.166(12) 0.040(5) 0.000 0.009(4) 0.000 C1 0.020(2) 0.039(3) 0.022(2) 0.0013(19) -0.0008(16) 0.000(2) C2 0.024(2) 0.042(3) 0.019(2) 0.0029(19) 0.0002(17) -0.002(2) C3 0.074(5) 0.058(5) 0.038(3) 0.018(3) 0.017(3) 0.023(4) C4 0.024(2) 0.078(5) 0.020(2) 0.004(3) 0.0035(18) -0.020(3) C5 0.022(2) 0.117(6) 0.017(2) 0.001(3) 0.0006(18) -0.022(3) C6 0.038(3) 0.097(6) 0.025(3) -0.003(3) -0.001(2) -0.039(4) C7 0.022(3) 0.110(6) 0.025(2) -0.001(3) -0.004(2) -0.002(3) C8 0.064(4) 0.052(4) 0.039(3) 0.012(3) -0.012(3) -0.032(4) C9 0.060(4) 0.070(5) 0.041(3) -0.016(3) -0.008(3) -0.027(4) C10 0.057(4) 0.022(3) 0.041(3) -0.002(2) -0.011(3) 0.005(3) C11 0.099(6) 0.021(3) 0.048(4) -0.009(3) -0.020(4) -0.012(3) C12 0.088(5) 0.027(3) 0.051(4) -0.017(3) -0.029(3) 0.026(3) C13 0.049(4) 0.048(4) 0.040(3) -0.019(3) -0.011(3) 0.005(3) C14 0.073(5) 0.068(5) 0.043(3) -0.017(3) -0.026(3) 0.050(4) C15 0.053(4) 0.144(9) 0.047(4) -0.055(5) -0.021(3) 0.050(5) C16 0.029(3) 0.085(5) 0.027(2) -0.012(3) -0.007(2) 0.026(3) C17 0.032(3) 0.142(8) 0.035(3) -0.036(4) -0.015(3) 0.043(4) C18 0.026(3) 0.161(9) 0.025(3) -0.030(4) -0.008(2) 0.027(4) C19 0.029(3) 0.180(10) 0.023(3) -0.020(5) -0.008(2) 0.019(5) C20 0.019(4) 0.132(10) 0.020(3) 0.000 -0.008(3) 0.000 C21 0.055(5) 0.135(8) 0.025(4) 0.000 0.002(4) 0.000 C22 0.015(3) 0.115(9) 0.018(3) 0.000 0.002(2) 0.000 C23 0.021(4) 0.119(9) 0.015(3) 0.000 0.000(3) 0.000 _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 U1 O2 1.774(5) . ? U1 O1 1.777(4) . ? U1 O18 2.337(3) . ? U1 O18 2.337(3) 6_565 ? U1 O9 2.418(4) 6_565 ? U1 O9 2.418(4) . ? U1 O19 2.426(4) . ? U2 O3 1.763(5) . ? U2 O4 1.779(5) . ? U2 O18 2.305(3) 6_565 ? U2 O18 2.305(3) . ? U2 O21 2.415(5) . ? U2 O20 2.493(4) . ? U2 O20 2.493(4) 6_565 ? U3 O6 1.769(5) . ? U3 O5 1.778(5) . ? U3 O24 2.337(3) . ? U3 O24 2.337(3) 6 ? U3 O25 2.412(5) . ? U3 O15 2.436(4) 6 ? U3 O15 2.436(4) . ? U4 O8 1.772(5) . ? U4 O7 1.775(5) . ? U4 O24 2.316(3) 6 ? U4 O24 2.316(3) . ? U4 O27 2.400(4) . ? U4 O26 2.485(4) . ? U4 O26 2.485(4) 6 ? Er1 O28 2.319(4) . ? Er1 O28 2.319(4) 6 ? Er1 O12 2.337(4) . ? Er1 O12 2.337(4) 6 ? Er1 O36 2.346(4) 6 ? Er1 O36 2.346(4) . ? Er1 O34 2.356(4) . ? Er1 O35 2.421(6) . ? Er2 O40 2.172(13) . ? Er2 O40 2.172(13) 6 ? Er2 O33 2.224(6) 6 ? Er2 O33 2.224(6) . ? Er2 O33 2.404(6) 2_557 ? Er2 O33 2.404(6) 5_557 ? Er2 O37 2.463(11) . ? S1 O10 1.449(4) . ? S1 O11 1.456(4) . ? S1 O9 1.478(3) . ? S1 C1 1.787(5) . ? S2 O13 1.451(4) . ? S2 O14 1.461(4) . ? S2 O12 1.478(4) . ? S2 C2 1.770(5) . ? S3 O17 1.433(4) . ? S3 O16 1.438(4) . ? S3 O15 1.470(4) . ? S3 C3 1.773(6) . ? O18 H18 0.8058 . ? O19 H19A 0.9203 . ? O19 H19B 0.8121 . ? O20 H20A 0.8870 . ? O20 H20B 0.9257 . ? O21 N1 1.224(10) . ? O22 N1 1.201(9) . ? O23 N1 1.410(11) . ? O24 H24 0.8508 . ? O25 H25A 0.9901 . ? O25 H25B 0.8736 . ? O26 H26A 0.9802 . ? O26 H26B 0.9982 . ? O27 H27A 0.9462 . ? O27 H27B 0.9429 . ? O28 C4 1.228(6) . ? O29 C7 1.238(7) . ? O30 C10 1.230(7) . ? O31 C13 1.234(8) . ? O32 C16 1.229(6) . ? O33 C19 1.238(8) . ? O33 Er2 2.405(6) 5_557 ? O34 H34 0.8602 . ? O36 H36A 0.8465 . ? O36 H36B 0.9078 . ? O37 N14 1.300(18) . ? O38 N14 1.20(2) . ? O39 N14 1.375(19) . ? O41 N15 1.195(11) . ? O42 N15 1.196(11) . ? O43 N15 1.382(13) . ? O44 H44 0.8413 . ? N2 C4 1.358(8) . ? N2 C22 1.434(7) . ? N2 C5 1.462(7) . ? N3 C4 1.361(9) . ? N3 C8 1.439(9) . ? N3 C6 1.473(7) . ? N4 C7 1.355(10) . ? N4 C6 1.434(7) . ? N4 C9 1.442(10) . ? N5 C7 1.370(9) . ? N5 C23 1.436(7) . ? N5 C5 1.459(7) . ? N6 C10 1.370(8) . ? N6 C11 1.449(8) . ? N6 C8 1.454(9) . ? N7 C10 1.358(8) . ? N7 C12 1.438(7) . ? N7 C14 1.462(9) . ? N8 C13 1.366(8) . ? N8 C15 1.446(10) . ? N8 C12 1.456(9) . ? N9 C13 1.344(9) . ? N9 C11 1.438(8) . ? N9 C9 1.442(9) . ? N10 C16 1.368(9) . ? N10 C14 1.413(10) . ? N10 C17 1.454(8) . ? N11 C16 1.344(9) . ? N11 C20 1.450(7) . ? N11 C18 1.458(7) . ? N12 C19 1.362(10) . ? N12 C21 1.441(7) . ? N12 C18 1.469(8) . ? N13 C19 1.310(13) . ? N13 C17 1.458(7) . ? N13 C15 1.469(12) . ? C1 C2 1.534(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.440(13) 7 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.547(11) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.539(11) . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C18 1.527(13) . ? C17 H17 0.9800 . ? C18 H18A 0.9800 . ? C20 N11 1.450(7) 6 ? C20 H20C 0.9700 . ? C20 H20D 0.9700 . ? C21 N12 1.441(7) 6 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N2 1.434(7) 6 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N5 1.436(7) 6 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 U1 O1 178.2(2) . . ? O2 U1 O18 91.94(15) . . ? O1 U1 O18 89.54(14) . . ? O2 U1 O18 91.94(15) . 6_565 ? O1 U1 O18 89.54(14) . 6_565 ? O18 U1 O18 69.19(18) . 6_565 ? O2 U1 O9 89.61(9) . 6_565 ? O1 U1 O9 89.85(9) . 6_565 ? O18 U1 O9 141.91(12) . 6_565 ? O18 U1 O9 72.72(12) 6_565 6_565 ? O2 U1 O9 89.61(9) . . ? O1 U1 O9 89.85(9) . . ? O18 U1 O9 72.72(12) . . ? O18 U1 O9 141.91(12) 6_565 . ? O9 U1 O9 145.36(15) 6_565 . ? O2 U1 O19 90.85(19) . . ? O1 U1 O19 87.35(18) . . ? O18 U1 O19 145.27(9) . . ? O18 U1 O19 145.27(9) 6_565 . ? O9 U1 O19 72.70(8) 6_565 . ? O9 U1 O19 72.70(8) . . ? O3 U2 O4 179.1(2) . . ? O3 U2 O18 87.52(16) . 6_565 ? O4 U2 O18 91.74(16) . 6_565 ? O3 U2 O18 87.52(16) . . ? O4 U2 O18 91.74(16) . . ? O18 U2 O18 70.30(18) 6_565 . ? O3 U2 O21 93.0(2) . . ? O4 U2 O21 87.9(2) . . ? O18 U2 O21 144.85(9) 6_565 . ? O18 U2 O21 144.85(9) . . ? O3 U2 O20 91.30(11) . . ? O4 U2 O20 88.97(11) . . ? O18 U2 O20 142.49(12) 6_565 . ? O18 U2 O20 72.19(12) . . ? O21 U2 O20 72.66(8) . . ? O3 U2 O20 91.30(11) . 6_565 ? O4 U2 O20 88.97(11) . 6_565 ? O18 U2 O20 72.19(12) 6_565 6_565 ? O18 U2 O20 142.49(12) . 6_565 ? O21 U2 O20 72.66(8) . 6_565 ? O20 U2 O20 145.31(16) . 6_565 ? O6 U3 O5 179.7(2) . . ? O6 U3 O24 90.67(14) . . ? O5 U3 O24 89.60(15) . . ? O6 U3 O24 90.67(14) . 6 ? O5 U3 O24 89.60(15) . 6 ? O24 U3 O24 70.17(16) . 6 ? O6 U3 O25 91.7(2) . . ? O5 U3 O25 87.9(2) . . ? O24 U3 O25 144.84(8) . . ? O24 U3 O25 144.84(8) 6 . ? O6 U3 O15 90.17(10) . 6 ? O5 U3 O15 89.73(10) . 6 ? O24 U3 O15 144.13(12) . 6 ? O24 U3 O15 73.96(12) 6 6 ? O25 U3 O15 70.95(9) . 6 ? O6 U3 O15 90.17(10) . . ? O5 U3 O15 89.73(10) . . ? O24 U3 O15 73.96(12) . . ? O24 U3 O15 144.13(12) 6 . ? O25 U3 O15 70.95(9) . . ? O15 U3 O15 141.89(17) 6 . ? O8 U4 O7 178.1(2) . . ? O8 U4 O24 92.37(15) . 6 ? O7 U4 O24 89.14(14) . 6 ? O8 U4 O24 92.37(15) . . ? O7 U4 O24 89.14(14) . . ? O24 U4 O24 70.91(17) 6 . ? O8 U4 O27 91.2(2) . . ? O7 U4 O27 87.0(2) . . ? O24 U4 O27 144.34(8) 6 . ? O24 U4 O27 144.34(8) . . ? O8 U4 O26 88.49(9) . . ? O7 U4 O26 90.95(9) . . ? O24 U4 O26 143.03(11) 6 . ? O24 U4 O26 72.13(11) . . ? O27 U4 O26 72.51(8) . . ? O8 U4 O26 88.49(9) . 6 ? O7 U4 O26 90.95(9) . 6 ? O24 U4 O26 72.13(11) 6 6 ? O24 U4 O26 143.03(11) . 6 ? O27 U4 O26 72.51(8) . 6 ? O26 U4 O26 144.81(15) . 6 ? O28 Er1 O28 78.2(2) . 6 ? O28 Er1 O12 73.84(12) . . ? O28 Er1 O12 120.69(14) 6 . ? O28 Er1 O12 120.69(14) . 6 ? O28 Er1 O12 73.84(12) 6 6 ? O12 Er1 O12 77.39(19) . 6 ? O28 Er1 O36 141.72(13) . 6 ? O28 Er1 O36 78.24(14) 6 6 ? O12 Er1 O36 144.44(13) . 6 ? O12 Er1 O36 80.41(15) 6 6 ? O28 Er1 O36 78.24(14) . . ? O28 Er1 O36 141.72(13) 6 . ? O12 Er1 O36 80.41(15) . . ? O12 Er1 O36 144.44(13) 6 . ? O36 Er1 O36 103.2(2) 6 . ? O28 Er1 O34 140.33(11) . . ? O28 Er1 O34 140.33(11) 6 . ? O12 Er1 O34 75.79(12) . . ? O12 Er1 O34 75.79(12) 6 . ? O36 Er1 O34 72.02(11) 6 . ? O36 Er1 O34 72.02(11) . . ? O28 Er1 O35 74.97(15) . . ? O28 Er1 O35 74.97(15) 6 . ? O12 Er1 O35 140.53(10) . . ? O12 Er1 O35 140.53(10) 6 . ? O36 Er1 O35 70.02(14) 6 . ? O36 Er1 O35 70.02(14) . . ? O34 Er1 O35 116.8(2) . . ? Er2 Er2 O40 135.8(2) 5_557 . ? Er2 Er2 O40 135.8(2) 5_557 6 ? O40 Er2 O40 70.2(5) . 6 ? Er2 Er2 O33 80.46(14) 5_557 6 ? O40 Er2 O33 143.3(3) . 6 ? O40 Er2 O33 87.0(3) 6 6 ? Er2 Er2 O33 80.46(14) 5_557 . ? O40 Er2 O33 87.0(3) . . ? O40 Er2 O33 143.3(3) 6 . ? O33 Er2 O33 95.9(3) 6 . ? Er2 Er2 O33 65.79(14) 5_557 2_557 ? O40 Er2 O33 70.3(3) . 2_557 ? O40 Er2 O33 116.9(3) 6 2_557 ? O33 Er2 O33 146.25(10) 6 2_557 ? O33 Er2 O33 79.2(3) . 2_557 ? Er2 Er2 O33 65.79(14) 5_557 5_557 ? O40 Er2 O33 116.9(3) . 5_557 ? O40 Er2 O33 70.3(3) 6 5_557 ? O33 Er2 O33 79.2(3) 6 5_557 ? O33 Er2 O33 146.25(10) . 5_557 ? O33 Er2 O33 86.7(3) 2_557 5_557 ? Er2 Er2 O37 136.3(3) 5_557 . ? O40 Er2 O37 75.8(3) . . ? O40 Er2 O37 75.8(3) 6 . ? O33 Er2 O37 70.8(2) 6 . ? O33 Er2 O37 70.8(2) . . ? O33 Er2 O37 135.33(16) 2_557 . ? O33 Er2 O37 135.33(16) 5_557 . ? O10 S1 O11 113.5(2) . . ? O10 S1 O9 111.0(2) . . ? O11 S1 O9 113.2(2) . . ? O10 S1 C1 107.3(2) . . ? O11 S1 C1 107.2(2) . . ? O9 S1 C1 103.8(2) . . ? O13 S2 O14 112.6(2) . . ? O13 S2 O12 113.5(3) . . ? O14 S2 O12 112.1(2) . . ? O13 S2 C2 105.3(2) . . ? O14 S2 C2 106.9(2) . . ? O12 S2 C2 105.7(2) . . ? O17 S3 O16 113.9(3) . . ? O17 S3 O15 113.5(2) . . ? O16 S3 O15 109.8(3) . . ? O17 S3 C3 111.0(3) . . ? O16 S3 C3 103.3(4) . . ? O15 S3 C3 104.3(3) . . ? S1 O9 U1 140.8(2) . . ? S2 O12 Er1 140.7(2) . . ? S3 O15 U3 142.9(2) . . ? U2 O18 U1 108.57(15) . . ? U2 O18 H18 110.6 . . ? U1 O18 H18 114.2 . . ? U1 O19 H19A 127.5 . . ? U1 O19 H19B 126.8 . . ? H19A O19 H19B 105.7 . . ? U2 O20 H20A 131.5 . . ? U2 O20 H20B 128.5 . . ? H20A O20 H20B 99.5 . . ? N1 O21 U2 127.4(6) . . ? U4 O24 U3 108.09(14) . . ? U4 O24 H24 106.8 . . ? U3 O24 H24 106.7 . . ? U3 O25 H25A 142.8 . . ? U3 O25 H25B 121.1 . . ? H25A O25 H25B 96.1 . . ? U4 O26 H26A 126.3 . . ? U4 O26 H26B 135.5 . . ? H26A O26 H26B 97.8 . . ? U4 O27 H27A 143.2 . . ? U4 O27 H27B 121.6 . . ? H27A O27 H27B 95.2 . . ? C4 O28 Er1 157.9(5) . . ? C19 O33 Er2 140.4(7) . . ? Er1 O34 H34 116.8 . . ? Er1 O36 H36A 109.0 . . ? Er1 O36 H36B 105.4 . . ? H36A O36 H36B 103.4 . . ? N14 O37 Er2 136.6(10) . . ? O22 N1 O21 125.6(10) . . ? O22 N1 O23 111.9(6) . . ? O21 N1 O23 106.0(6) . . ? C4 N2 C22 124.0(5) . . ? C4 N2 C5 111.6(6) . . ? C22 N2 C5 124.4(6) . . ? C4 N3 C8 122.9(5) . . ? C4 N3 C6 111.6(6) . . ? C8 N3 C6 124.2(6) . . ? C7 N4 C6 111.0(6) . . ? C7 N4 C9 123.2(5) . . ? C6 N4 C9 125.6(7) . . ? C7 N5 C23 124.0(5) . . ? C7 N5 C5 109.9(6) . . ? C23 N5 C5 123.6(6) . . ? C10 N6 C11 112.2(6) . . ? C10 N6 C8 121.6(5) . . ? C11 N6 C8 122.6(5) . . ? C10 N7 C12 113.0(6) . . ? C10 N7 C14 123.5(5) . . ? C12 N7 C14 123.1(6) . . ? C13 N8 C15 123.0(6) . . ? C13 N8 C12 111.0(6) . . ? C15 N8 C12 122.7(6) . . ? C13 N9 C11 112.8(6) . . ? C13 N9 C9 123.6(5) . . ? C11 N9 C9 123.2(6) . . ? C16 N10 C14 122.9(5) . . ? C16 N10 C17 112.3(7) . . ? C14 N10 C17 124.8(7) . . ? C16 N11 C20 122.6(5) . . ? C16 N11 C18 112.3(7) . . ? C20 N11 C18 123.4(6) . . ? C19 N12 C21 124.7(7) . . ? C19 N12 C18 110.6(7) . . ? C21 N12 C18 124.5(7) . . ? C19 N13 C17 113.2(7) . . ? C19 N13 C15 122.6(6) . . ? C17 N13 C15 122.8(8) . . ? O38 N14 O37 120.0(14) . . ? O38 N14 O39 114.2(15) . . ? O37 N14 O39 118.0(14) . . ? O41 N15 O42 126.6(10) . . ? O41 N15 O43 110.4(8) . . ? O42 N15 O43 112.8(8) . . ? C2 C1 S1 109.5(3) . . ? C2 C1 H1A 109.8 . . ? S1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? S1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C1 C2 S2 111.8(3) . . ? C1 C2 H2A 109.3 . . ? S2 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? S2 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C3 C3 S3 115.9(7) 7 . ? C3 C3 H3A 108.3 7 . ? S3 C3 H3A 108.3 . . ? C3 C3 H3B 108.3 7 . ? S3 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? O28 C4 N2 125.5(7) . . ? O28 C4 N3 124.8(6) . . ? N2 C4 N3 109.6(5) . . ? N5 C5 N2 113.6(6) . . ? N5 C5 C6 103.1(5) . . ? N2 C5 C6 103.5(5) . . ? N5 C5 H5 112.0 . . ? N2 C5 H5 112.0 . . ? C6 C5 H5 112.0 . . ? N4 C6 N3 113.4(5) . . ? N4 C6 C5 104.3(6) . . ? N3 C6 C5 102.7(5) . . ? N4 C6 H6 111.9 . . ? N3 C6 H6 111.9 . . ? C5 C6 H6 111.9 . . ? O29 C7 N4 124.5(7) . . ? O29 C7 N5 124.7(8) . . ? N4 C7 N5 110.8(5) . . ? N3 C8 N6 112.7(5) . . ? N3 C8 H8A 109.1 . . ? N6 C8 H8A 109.1 . . ? N3 C8 H8B 109.1 . . ? N6 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N4 C9 N9 113.5(5) . . ? N4 C9 H9A 108.9 . . ? N9 C9 H9A 108.9 . . ? N4 C9 H9B 108.9 . . ? N9 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? O30 C10 N7 125.8(6) . . ? O30 C10 N6 126.4(6) . . ? N7 C10 N6 107.8(5) . . ? N9 C11 N6 115.4(6) . . ? N9 C11 C12 103.2(6) . . ? N6 C11 C12 102.9(5) . . ? N9 C11 H11 111.6 . . ? N6 C11 H11 111.6 . . ? C12 C11 H11 111.6 . . ? N7 C12 N8 115.0(6) . . ? N7 C12 C11 103.5(5) . . ? N8 C12 C11 103.0(5) . . ? N7 C12 H12 111.6 . . ? N8 C12 H12 111.6 . . ? C11 C12 H12 111.6 . . ? O31 C13 N9 126.8(6) . . ? O31 C13 N8 124.4(7) . . ? N9 C13 N8 108.8(6) . . ? N10 C14 N7 114.6(5) . . ? N10 C14 H14A 108.6 . . ? N7 C14 H14A 108.6 . . ? N10 C14 H14B 108.6 . . ? N7 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N8 C15 N13 112.3(5) . . ? N8 C15 H15A 109.1 . . ? N13 C15 H15A 109.1 . . ? N8 C15 H15B 109.1 . . ? N13 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? O32 C16 N11 127.1(7) . . ? O32 C16 N10 124.3(7) . . ? N11 C16 N10 108.5(5) . . ? N10 C17 N13 114.4(5) . . ? N10 C17 C18 103.0(6) . . ? N13 C17 C18 102.7(7) . . ? N10 C17 H17 112.0 . . ? N13 C17 H17 112.0 . . ? C18 C17 H17 112.0 . . ? N11 C18 N12 113.6(6) . . ? N11 C18 C17 103.6(6) . . ? N12 C18 C17 103.3(5) . . ? N11 C18 H18A 111.9 . . ? N12 C18 H18A 111.9 . . ? C17 C18 H18A 111.9 . . ? O33 C19 N13 124.8(9) . . ? O33 C19 N12 125.2(10) . . ? N13 C19 N12 110.0(6) . . ? N11 C20 N11 112.9(6) 6 . ? N11 C20 H20C 109.0 6 . ? N11 C20 H20C 109.0 . . ? N11 C20 H20D 109.0 6 . ? N11 C20 H20D 109.0 . . ? H20C C20 H20D 107.8 . . ? N12 C21 N12 114.6(8) 6 . ? N12 C21 H21A 108.6 6 . ? N12 C21 H21A 108.6 . . ? N12 C21 H21B 108.6 6 . ? N12 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? N2 C22 N2 114.0(6) . 6 ? N2 C22 H22A 108.8 . . ? N2 C22 H22A 108.8 6 . ? N2 C22 H22B 108.8 . . ? N2 C22 H22B 108.8 6 . ? H22A C22 H22B 107.6 . . ? N5 C23 N5 114.2(6) . 6 ? N5 C23 H23A 108.7 . . ? N5 C23 H23A 108.7 6 . ? N5 C23 H23B 108.7 . . ? N5 C23 H23B 108.7 6 . ? H23A C23 H23B 107.6 . . ? 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 O18 H18 O16 0.81 1.99 2.787(5) 171.8 . O19 H19A O44 0.92 1.81 2.721(7) 173.2 . O19 H19B O46 0.81 1.87 2.642(10) 157.7 . O20 H20A O17 0.89 1.96 2.805(6) 157.7 . O20 H20B O31 0.93 1.89 2.820(6) 177.2 1_554 O24 H24 O10 0.85 1.94 2.779(5) 166.8 . O25 H25A O4 0.99 1.87 2.789(7) 153.5 7 O25 H25B O47 0.87 1.71 2.546(8) 159.0 . O26 H26A O11 0.98 1.86 2.834(5) 173.3 . O26 H26B O14 1.00 1.75 2.731(5) 165.8 7_556 O27 H27A O44 0.95 1.86 2.724(7) 149.8 7_556 O27 H27B O45 0.94 1.74 2.626(10) 154.9 7_556 O34 H34 O32 0.86 2.22 2.694(5) 114.6 2_556 O36 H36A O30 0.85 2.10 2.770(5) 136.3 . O36 H36B O48 0.91 2.01 2.771(10) 139.9 . O44 H44 O13 0.84 1.96 2.776(6) 161.8 7_556 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 863488' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H86 N26.50 O66.50 S6 U4 Yb1.50' _chemical_formula_weight 3430.41 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 31.1082(12) _cell_length_b 14.1633(4) _cell_length_c 20.7953(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.892(2) _cell_angle_gamma 90.00 _cell_volume 9141.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 151336 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 30.51 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6498 _exptl_absorpt_coefficient_mu 8.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.213 _exptl_absorpt_correction_T_max 0.413 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (581 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 151336 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 30.51 _reflns_number_total 14444 _reflns_number_gt 10414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The atom Yb2 and the associated nitrate ion were given 0.5 occupancy factors so as to account for the close contact between Yb2 and its image by symmetry and to retain acceptable displacement parameters. One O atom in each of the three nitrate ions is disordered around a symmetry plane, the disorder on the associated N atom being unresolved. Several solvent water molecules were given 0.5 occupancy factors so as to to account for too close contacts and/or to retain acceptable displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to O atoms were found on a Fourier-difference map, except for those of O35, O40 and four solvent water molecules, and all the others were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+19.1278P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14444 _refine_ls_number_parameters 754 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.271 _refine_diff_density_min -2.796 _refine_diff_density_rms 0.199 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 U1 U 0.156500(9) 0.5000 0.245825(11) 0.02187(7) Uani 1 2 d S . . U2 U 0.126257(10) 0.5000 0.067339(12) 0.02926(8) Uani 1 2 d S . . U3 U 0.256460(9) 0.0000 0.156165(12) 0.02344(7) Uani 1 2 d S . . U4 U 0.284697(9) 0.0000 0.335030(12) 0.02264(7) Uani 1 2 d S . . Yb1 Yb 0.090510(12) 0.0000 0.546551(15) 0.03086(9) Uani 1 2 d S . . Yb2 Yb 0.01440(3) 0.0000 0.97641(4) 0.0650(3) Uani 0.50 2 d SP . . S1 S 0.18745(5) 0.26888(10) 0.31531(6) 0.0262(3) Uani 1 1 d . . . S2 S 0.17042(5) 0.17003(11) 0.50964(6) 0.0307(3) Uani 1 1 d . . . S3 S 0.22506(5) 0.23816(11) 0.09523(6) 0.0304(3) Uani 1 1 d . . . O1 O 0.09950(16) 0.5000 0.2484(2) 0.0226(11) Uani 1 2 d S . . O2 O 0.21335(17) 0.5000 0.2460(2) 0.0256(11) Uani 1 2 d S . . O3 O 0.07552(18) 0.5000 0.0992(3) 0.0322(13) Uani 1 2 d S . . O4 O 0.1780(2) 0.5000 0.0357(3) 0.0462(17) Uani 1 2 d S . . O5 O 0.31416(18) 0.0000 0.1544(2) 0.0299(12) Uani 1 2 d S . . O6 O 0.19983(18) 0.0000 0.1573(2) 0.0253(12) Uani 1 2 d S . . O7 O 0.33773(18) 0.0000 0.3083(2) 0.0270(12) Uani 1 2 d S . . O8 O 0.23260(18) 0.0000 0.3647(2) 0.0271(12) Uani 1 2 d S . . O9 O 0.15833(13) 0.3371(3) 0.28045(16) 0.0288(9) Uani 1 1 d . . . O10 O 0.18695(13) 0.1784(3) 0.28232(17) 0.0313(9) Uani 1 1 d . . . O11 O 0.23033(13) 0.3062(3) 0.33066(18) 0.0322(9) Uani 1 1 d . . . O12 O 0.13527(15) 0.1011(3) 0.49531(17) 0.0383(10) Uani 1 1 d . . . O13 O 0.20568(15) 0.1328(3) 0.55128(17) 0.0420(11) Uani 1 1 d . . . O14 O 0.15446(14) 0.2599(3) 0.53214(17) 0.0344(10) Uani 1 1 d . . . O15 O 0.25445(14) 0.1623(3) 0.11774(17) 0.0353(10) Uani 1 1 d . . . O16 O 0.22787(16) 0.3158(4) 0.1396(3) 0.0613(15) Uani 1 1 d . . . O17 O 0.18239(16) 0.2061(3) 0.0797(2) 0.0510(13) Uani 1 1 d . . . O18 O 0.14994(13) 0.4069(3) 0.15332(15) 0.0289(9) Uani 1 1 d . . . H18 H 0.1716 0.3793 0.1456 0.035 Uiso 1 1 d R . . O19 O 0.16034(19) 0.5000 0.3622(2) 0.0302(13) Uani 1 2 d S . . H19A H 0.1848 0.5000 0.3896 0.036 Uiso 1 2 d SR . . H19B H 0.1403 0.5000 0.3852 0.036 Uiso 1 2 d SR . . O20 O 0.11770(15) 0.3328(3) 0.03283(19) 0.0455(12) Uani 1 1 d . . . H20A H 0.1328 0.2816 0.0437 0.055 Uiso 1 1 d R . . H20B H 0.0996 0.3081 -0.0001 0.055 Uiso 1 1 d R . . O21 O 0.0963(3) 0.5000 -0.0420(3) 0.062(2) Uani 1 2 d S . . O22 O 0.0439(3) 0.5000 -0.1166(3) 0.065(2) Uani 1 2 d S . . O23 O 0.0385(4) 0.4297(8) -0.0240(5) 0.066(3) Uani 0.50 1 d P . . O24 O 0.26294(12) 0.0941(3) 0.24797(15) 0.0269(8) Uani 1 1 d . . . H24 H 0.2377 0.1136 0.2544 0.032 Uiso 1 1 d R . . O25 O 0.2519(2) 0.0000 0.0399(3) 0.0439(17) Uani 1 2 d S . . H25A H 0.2696 0.0000 0.0022 0.053 Uiso 1 2 d SR . . H25B H 0.2270 0.0000 0.0179 0.053 Uiso 1 2 d SR . . O26 O 0.29268(13) 0.1672(3) 0.36996(17) 0.0302(9) Uani 1 1 d . . . H26A H 0.2727 0.2188 0.3583 0.036 Uiso 1 1 d R . . H26B H 0.3122 0.2024 0.4015 0.036 Uiso 1 1 d R . . O27 O 0.31728(19) 0.0000 0.4427(2) 0.0333(14) Uani 1 2 d S . . H27A H 0.3110 0.0000 0.4865 0.040 Uiso 1 2 d SR . . H27B H 0.3475 0.0000 0.4509 0.040 Uiso 1 2 d SR . . O28 O 0.11765(13) 0.1014(4) 0.62500(16) 0.0410(11) Uani 1 1 d . . . O29 O 0.15089(16) 0.1305(5) 0.90739(19) 0.0620(16) Uani 1 1 d . . . O30 O 0.01920(16) 0.2278(3) 0.6388(2) 0.0466(12) Uani 1 1 d . . . O31 O 0.06434(18) 0.2573(5) 0.9302(2) 0.0722(19) Uani 1 1 d . . . O32 O -0.07401(16) 0.1243(4) 0.65710(18) 0.0497(13) Uani 1 1 d . . . O33 O -0.02843(18) 0.1149(6) 0.9412(2) 0.087(2) Uani 1 1 d . . . O34 O 0.06299(19) 0.0000 0.4395(2) 0.0331(13) Uani 1 2 d S . . H34 H 0.0485 0.0489 0.4265 0.040 Uiso 1 1 d R . . O35 O 0.0387(3) 0.0000 0.6271(4) 0.071(2) Uani 1 2 d S . . O36 O 0.04427(16) 0.1270(4) 0.5328(2) 0.0537(13) Uani 1 1 d . . . H36A H 0.0506 0.1674 0.5618 0.064 Uiso 1 1 d R . . H36B H 0.0520 0.1557 0.4963 0.064 Uiso 1 1 d R . . O37 O 0.0088(5) 0.0000 0.8574(7) 0.073(5) Uani 0.50 2 d SP . . O38 O 0.0746(7) 0.0000 0.8237(9) 0.083(5) Uani 0.50 2 d SPU . . O39 O 0.0263(8) 0.0462(16) 0.7555(10) 0.071(5) Uani 0.25 1 d PU . . O40 O 0.0664(4) 0.0841(9) 0.9494(5) 0.083(4) Uani 0.50 1 d P . . O41 O 0.4437(3) 0.0000 0.3471(5) 0.087(3) Uani 1 2 d S . . O42 O 0.5121(3) 0.0000 0.3351(3) 0.069(2) Uani 1 2 d S . . O43 O 0.4887(4) 0.0551(11) 0.4225(6) 0.097(5) Uani 0.50 1 d P . . O44 O 0.22898(19) 0.5000 0.4514(3) 0.0354(14) Uani 1 2 d S . . H44 H 0.2459 0.4541 0.4573 0.042 Uiso 1 1 d R . . O45 O 0.1025(3) 0.4451(8) 0.5351(4) 0.064(3) Uani 0.50 1 d P . . O46 O 0.0874(3) 0.4630(7) 0.4153(4) 0.058(3) Uani 0.50 1 d P . . O47 O 0.1726(2) 0.0000 0.0024(3) 0.054(2) Uani 1 2 d S . . O48 O 0.0587(4) 0.2851(8) 0.4588(5) 0.064(3) Uani 0.50 1 d P . . N1 N 0.0578(4) 0.5000 -0.0606(5) 0.082(4) Uani 1 2 d S . . N2 N 0.17673(16) 0.0845(5) 0.6975(2) 0.0428(14) Uani 1 1 d . . . N3 N 0.13518(19) 0.2125(4) 0.7046(2) 0.0417(14) Uani 1 1 d . . . N4 N 0.15214(18) 0.2278(5) 0.8188(2) 0.0467(15) Uani 1 1 d . . . N5 N 0.18291(17) 0.0861(5) 0.8147(2) 0.0445(15) Uani 1 1 d . . . N6 N 0.0681(2) 0.2901(4) 0.7179(3) 0.0473(15) Uani 1 1 d . . . N7 N -0.0021(2) 0.3002(4) 0.7311(3) 0.0534(17) Uani 1 1 d . . . N8 N 0.0162(2) 0.3002(5) 0.8467(3) 0.0518(16) Uani 1 1 d . . . N9 N 0.0855(2) 0.3112(4) 0.8318(3) 0.0498(16) Uani 1 1 d . . . N10 N -0.0696(2) 0.2214(5) 0.7450(3) 0.0500(16) Uani 1 1 d . . . N11 N -0.10233(17) 0.0846(5) 0.7536(2) 0.0533(18) Uani 1 1 d . . . N12 N -0.08747(19) 0.0853(6) 0.8700(2) 0.063(2) Uani 1 1 d . . . N13 N -0.05025(19) 0.2144(6) 0.8612(3) 0.061(2) Uani 1 1 d . . . N14 N 0.0360(8) 0.0000 0.8116(10) 0.073(6) Uani 0.50 2 d SPU . . N15 N 0.4814(4) 0.0000 0.3672(5) 0.089(4) Uani 1 2 d S . . C1 C 0.16287(18) 0.2507(4) 0.3904(2) 0.0284(12) Uani 1 1 d . . . H1A H 0.1575 0.3111 0.4102 0.034 Uiso 1 1 calc R . . H1B H 0.1355 0.2185 0.3824 0.034 Uiso 1 1 calc R . . C2 C 0.19276(19) 0.1914(5) 0.4357(2) 0.0315(13) Uani 1 1 d . . . H2A H 0.2200 0.2241 0.4436 0.038 Uiso 1 1 calc R . . H2B H 0.1984 0.1316 0.4152 0.038 Uiso 1 1 calc R . . C3 C 0.2472(3) 0.2819(6) 0.0244(3) 0.064(3) Uani 1 1 d . . . H3A H 0.2288 0.3323 0.0072 0.077 Uiso 1 1 calc R . . H3B H 0.2751 0.3097 0.0369 0.077 Uiso 1 1 calc R . . C4 C 0.1415(2) 0.1293(5) 0.6715(2) 0.0385(16) Uani 1 1 d . . . C5 C 0.1943(2) 0.1328(6) 0.7561(3) 0.0469(19) Uani 1 1 d . . . H5 H 0.2254 0.1437 0.7556 0.056 Uiso 1 1 calc R . . C6 C 0.1686(2) 0.2260(6) 0.7562(3) 0.050(2) Uani 1 1 d . . . H6 H 0.1867 0.2809 0.7486 0.060 Uiso 1 1 calc R . . C7 C 0.1606(2) 0.1474(7) 0.8519(3) 0.052(2) Uani 1 1 d . . . C8 C 0.1061(2) 0.2837(5) 0.6812(3) 0.0483(19) Uani 1 1 d . . . H8A H 0.0971 0.2705 0.6365 0.058 Uiso 1 1 calc R . . H8B H 0.1208 0.3441 0.6828 0.058 Uiso 1 1 calc R . . C9 C 0.1318(3) 0.3077(6) 0.8462(4) 0.060(2) Uani 1 1 d . . . H9A H 0.1445 0.3649 0.8302 0.072 Uiso 1 1 calc R . . H9B H 0.1376 0.3063 0.8926 0.072 Uiso 1 1 calc R . . C10 C 0.0280(3) 0.2682(5) 0.6913(3) 0.0450(17) Uani 1 1 d . . . C11 C 0.0656(3) 0.3490(5) 0.7736(3) 0.060(2) Uani 1 1 d . . . H11 H 0.0759 0.4130 0.7656 0.072 Uiso 1 1 calc R . . C12 C 0.0176(3) 0.3491(6) 0.7856(3) 0.057(2) Uani 1 1 d . . . H12 H 0.0064 0.4136 0.7883 0.069 Uiso 1 1 calc R . . C13 C 0.0568(2) 0.2862(6) 0.8744(3) 0.052(2) Uani 1 1 d . . . C14 C -0.0481(3) 0.2970(7) 0.7158(3) 0.061(3) Uani 1 1 d . . . H14A H -0.0606 0.3560 0.7290 0.074 Uiso 1 1 calc R . . H14B H -0.0533 0.2920 0.6694 0.074 Uiso 1 1 calc R . . C15 C -0.0223(3) 0.2926(7) 0.8825(4) 0.078(3) Uani 1 1 d . . . H15A H -0.0384 0.3511 0.8779 0.094 Uiso 1 1 calc R . . H15B H -0.0137 0.2844 0.9279 0.094 Uiso 1 1 calc R . . C16 C -0.0804(2) 0.1411(6) 0.7138(3) 0.0463(18) Uani 1 1 d . . . C17 C -0.0845(2) 0.2244(7) 0.8093(3) 0.066(3) Uani 1 1 d . . . H17 H -0.1028 0.2794 0.8157 0.079 Uiso 1 1 calc R . . C18 C -0.1091(2) 0.1317(7) 0.8141(3) 0.062(3) Uani 1 1 d . . . H18A H -0.1398 0.1423 0.8197 0.075 Uiso 1 1 calc R . . C19 C -0.0531(2) 0.1358(8) 0.8945(3) 0.066(3) Uani 1 1 d . . . C20 C -0.1242(3) 0.0000 0.7316(4) 0.054(3) Uani 1 2 d S . . H20C H -0.1531 0.0000 0.7467 0.065 Uiso 1 2 calc SR . . H20D H -0.1269 0.0000 0.6849 0.065 Uiso 1 2 calc SR . . C21 C -0.1021(4) 0.0000 0.8980(5) 0.081(5) Uani 1 2 d S . . H21A H -0.0929 0.0000 0.9435 0.097 Uiso 1 2 calc SR . . H21B H -0.1334 0.0000 0.8946 0.097 Uiso 1 2 calc SR . . C22 C 0.1935(3) 0.0000 0.6707(4) 0.052(3) Uani 1 2 d S . . H22A H 0.2246 0.0000 0.6780 0.062 Uiso 1 2 calc SR . . H22B H 0.1866 0.0000 0.6245 0.062 Uiso 1 2 calc SR . . C23 C 0.2031(3) 0.0000 0.8389(4) 0.049(3) Uani 1 2 d S . . H23A H 0.2030 0.0000 0.8855 0.059 Uiso 1 2 calc SR . . H23B H 0.2329 0.0000 0.8280 0.059 Uiso 1 2 calc SR . . 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 U1 0.02025(14) 0.02752(16) 0.01769(11) 0.000 0.00011(9) 0.000 U2 0.02838(17) 0.03997(19) 0.01905(12) 0.000 -0.00117(10) 0.000 U3 0.02255(15) 0.02982(16) 0.01771(11) 0.000 -0.00027(10) 0.000 U4 0.02421(15) 0.02557(15) 0.01782(11) 0.000 -0.00091(10) 0.000 Yb1 0.02311(18) 0.0493(2) 0.01968(14) 0.000 -0.00196(12) 0.000 Yb2 0.0288(5) 0.1421(11) 0.0237(3) 0.000 -0.0020(3) 0.000 S1 0.0256(7) 0.0317(8) 0.0210(5) 0.0029(5) -0.0009(5) 0.0016(6) S2 0.0353(8) 0.0375(8) 0.0190(5) -0.0009(6) -0.0006(5) 0.0000(7) S3 0.0398(9) 0.0292(8) 0.0227(6) 0.0010(5) 0.0047(5) 0.0022(7) O1 0.017(3) 0.027(3) 0.023(2) 0.000 -0.0014(19) 0.000 O2 0.018(3) 0.032(3) 0.027(2) 0.000 0.003(2) 0.000 O3 0.026(3) 0.036(3) 0.034(3) 0.000 -0.001(2) 0.000 O4 0.046(4) 0.066(5) 0.027(3) 0.000 0.007(3) 0.000 O5 0.021(3) 0.035(3) 0.034(3) 0.000 0.003(2) 0.000 O6 0.028(3) 0.027(3) 0.020(2) 0.000 -0.002(2) 0.000 O7 0.028(3) 0.028(3) 0.026(2) 0.000 0.004(2) 0.000 O8 0.031(3) 0.024(3) 0.027(2) 0.000 0.004(2) 0.000 O9 0.028(2) 0.032(2) 0.0259(17) 0.0031(16) -0.0032(15) 0.0035(18) O10 0.033(2) 0.029(2) 0.0313(19) -0.0003(16) 0.0008(16) 0.0050(18) O11 0.025(2) 0.038(2) 0.0325(19) 0.0059(18) -0.0020(16) -0.0048(19) O12 0.053(3) 0.041(3) 0.0222(17) -0.0021(17) 0.0082(17) -0.010(2) O13 0.046(3) 0.057(3) 0.0225(18) 0.0068(19) -0.0019(17) 0.013(2) O14 0.036(2) 0.040(3) 0.0267(18) -0.0042(18) -0.0033(16) 0.001(2) O15 0.037(2) 0.043(3) 0.0255(18) 0.0106(18) -0.0011(16) -0.001(2) O16 0.035(3) 0.064(4) 0.084(4) -0.040(3) -0.006(3) 0.011(3) O17 0.040(3) 0.044(3) 0.066(3) 0.011(2) -0.019(2) -0.005(2) O18 0.028(2) 0.035(2) 0.0226(16) -0.0049(16) -0.0014(14) 0.0086(18) O19 0.032(3) 0.038(3) 0.021(2) 0.000 0.004(2) 0.000 O20 0.048(3) 0.052(3) 0.034(2) -0.009(2) -0.017(2) 0.015(2) O21 0.060(5) 0.087(6) 0.036(3) 0.000 -0.008(3) 0.000 O22 0.101(7) 0.032(4) 0.054(4) 0.000 -0.045(4) 0.000 O23 0.065(8) 0.080(9) 0.051(6) 0.002(6) -0.011(5) -0.024(7) O24 0.025(2) 0.034(2) 0.0207(15) 0.0016(15) -0.0022(14) 0.0013(18) O25 0.035(4) 0.076(5) 0.021(2) 0.000 0.003(2) 0.000 O26 0.030(2) 0.033(2) 0.0266(17) -0.0046(17) -0.0052(15) 0.0030(19) O27 0.032(3) 0.044(4) 0.023(2) 0.000 -0.006(2) 0.000 O28 0.034(2) 0.073(3) 0.0155(16) -0.0005(19) 0.0002(15) -0.003(2) O29 0.044(3) 0.121(5) 0.0217(19) 0.007(3) 0.0042(18) 0.023(3) O30 0.049(3) 0.050(3) 0.040(2) -0.013(2) -0.007(2) 0.005(2) O31 0.047(3) 0.127(6) 0.040(3) -0.006(3) -0.016(2) -0.005(4) O32 0.062(3) 0.063(3) 0.0238(19) -0.010(2) -0.002(2) 0.013(3) O33 0.054(4) 0.169(7) 0.035(2) -0.001(3) -0.024(2) 0.010(4) O34 0.038(4) 0.034(3) 0.026(3) 0.000 -0.002(2) 0.000 O35 0.065(6) 0.094(7) 0.057(5) 0.000 0.025(4) 0.000 O36 0.052(3) 0.071(4) 0.037(2) -0.012(2) -0.001(2) 0.011(3) O37 0.034(9) 0.133(16) 0.053(8) 0.000 0.015(7) 0.000 O38 0.078(7) 0.095(7) 0.076(6) 0.000 0.010(6) 0.000 O39 0.078(7) 0.079(8) 0.056(7) 0.005(6) 0.000(6) 0.010(6) O40 0.097(10) 0.101(10) 0.048(6) -0.014(6) -0.012(6) 0.065(8) O41 0.042(5) 0.110(8) 0.107(7) 0.000 -0.007(5) 0.000 O42 0.054(5) 0.104(7) 0.050(4) 0.000 0.010(4) 0.000 O43 0.067(9) 0.154(15) 0.073(7) -0.018(8) 0.014(7) 0.021(8) O44 0.027(3) 0.043(4) 0.035(3) 0.000 -0.003(2) 0.000 O45 0.040(6) 0.110(9) 0.042(5) 0.014(5) 0.005(4) 0.006(6) O46 0.036(5) 0.089(10) 0.049(5) -0.003(5) 0.008(4) -0.010(5) O47 0.039(4) 0.092(6) 0.029(3) 0.000 -0.003(3) 0.000 O48 0.078(8) 0.067(8) 0.051(6) 0.029(5) 0.025(6) 0.027(6) N1 0.066(8) 0.128(11) 0.048(5) 0.000 -0.017(5) 0.000 N2 0.029(3) 0.083(4) 0.0160(19) 0.001(2) -0.0005(18) -0.006(3) N3 0.047(3) 0.050(4) 0.027(2) 0.004(2) -0.005(2) -0.021(3) N4 0.032(3) 0.077(5) 0.030(2) -0.003(3) -0.005(2) -0.013(3) N5 0.027(3) 0.084(5) 0.022(2) -0.002(3) -0.0006(19) -0.008(3) N6 0.060(4) 0.042(3) 0.039(3) -0.006(3) -0.009(3) -0.013(3) N7 0.066(4) 0.052(4) 0.039(3) -0.015(3) -0.016(3) 0.026(3) N8 0.049(4) 0.058(4) 0.046(3) -0.020(3) -0.014(3) 0.013(3) N9 0.055(4) 0.045(4) 0.047(3) -0.008(3) -0.017(3) -0.005(3) N10 0.050(4) 0.065(4) 0.033(3) -0.015(3) -0.010(2) 0.029(3) N11 0.028(3) 0.106(5) 0.025(2) -0.017(3) -0.005(2) 0.000(3) N12 0.034(3) 0.130(7) 0.025(2) -0.021(3) -0.008(2) 0.017(4) N13 0.034(3) 0.114(6) 0.033(3) -0.022(4) -0.015(2) 0.010(4) N14 0.071(9) 0.089(9) 0.060(8) 0.000 0.006(7) 0.000 N15 0.065(8) 0.154(13) 0.050(6) 0.000 0.018(6) 0.000 C1 0.024(3) 0.036(3) 0.024(2) 0.005(2) -0.002(2) 0.003(3) C2 0.031(3) 0.040(4) 0.023(2) 0.005(2) 0.000(2) 0.000(3) C3 0.091(7) 0.060(5) 0.045(4) 0.025(4) 0.025(4) 0.036(5) C4 0.028(3) 0.069(5) 0.018(2) 0.011(3) 0.003(2) -0.018(3) C5 0.027(3) 0.092(6) 0.022(2) 0.001(3) 0.004(2) -0.021(4) C6 0.036(4) 0.086(6) 0.027(3) -0.005(3) 0.001(3) -0.031(4) C7 0.030(3) 0.100(7) 0.026(3) -0.009(4) -0.006(2) 0.004(4) C8 0.065(5) 0.041(4) 0.037(3) 0.011(3) -0.008(3) -0.024(4) C9 0.054(5) 0.073(6) 0.050(4) -0.018(4) -0.009(4) -0.022(4) C10 0.061(5) 0.027(3) 0.046(3) -0.002(3) -0.002(3) 0.013(3) C11 0.100(7) 0.027(4) 0.050(4) -0.010(3) -0.018(4) -0.008(4) C12 0.076(6) 0.040(4) 0.052(4) -0.014(3) -0.022(4) 0.021(4) C13 0.043(4) 0.064(5) 0.045(4) -0.021(4) -0.013(3) 0.001(4) C14 0.070(6) 0.071(6) 0.040(3) -0.017(4) -0.026(4) 0.041(5) C15 0.061(5) 0.124(8) 0.047(4) -0.050(5) -0.014(4) 0.045(6) C16 0.033(4) 0.071(5) 0.034(3) -0.010(3) -0.008(3) 0.025(4) C17 0.035(4) 0.125(8) 0.036(3) -0.029(4) -0.013(3) 0.037(5) C18 0.025(3) 0.134(8) 0.027(3) -0.016(4) -0.012(2) 0.021(4) C19 0.033(4) 0.136(9) 0.028(3) -0.016(4) -0.006(3) 0.020(5) C20 0.027(5) 0.121(10) 0.014(3) 0.000 -0.006(3) 0.000 C21 0.043(7) 0.178(16) 0.022(4) 0.000 0.003(4) 0.000 C22 0.018(4) 0.118(10) 0.020(4) 0.000 0.008(3) 0.000 C23 0.023(5) 0.106(9) 0.019(3) 0.000 0.005(3) 0.000 _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 U1 O2 1.768(5) . ? U1 O1 1.777(5) . ? U1 O18 2.330(3) . ? U1 O18 2.330(3) 6_565 ? U1 O19 2.414(5) . ? U1 O9 2.417(4) 6_565 ? U1 O9 2.417(4) . ? U2 O3 1.752(6) . ? U2 O4 1.780(7) . ? U2 O18 2.302(4) 6_565 ? U2 O18 2.302(4) . ? U2 O21 2.398(7) . ? U2 O20 2.483(5) . ? U2 O20 2.483(5) 6_565 ? U3 O6 1.763(6) . ? U3 O5 1.798(5) . ? U3 O24 2.326(3) . ? U3 O24 2.326(3) 6 ? U3 O25 2.412(5) . ? U3 O15 2.433(4) 6 ? U3 O15 2.433(4) . ? U4 O8 1.773(6) . ? U4 O7 1.777(5) . ? U4 O24 2.312(3) 6 ? U4 O24 2.312(3) . ? U4 O27 2.394(5) . ? U4 O26 2.485(4) . ? U4 O26 2.485(4) 6 ? Yb1 O28 2.292(4) . ? Yb1 O28 2.292(4) 6 ? Yb1 O12 2.308(4) . ? Yb1 O12 2.308(4) 6 ? Yb1 O36 2.309(5) 6 ? Yb1 O36 2.309(5) . ? Yb1 O34 2.331(5) . ? Yb1 O35 2.402(7) . ? Yb2 O40 2.115(15) . ? Yb2 O40 2.115(15) 6 ? Yb2 O33 2.197(7) 6 ? Yb2 O33 2.197(7) . ? Yb2 O33 2.381(7) 2_557 ? Yb2 O33 2.381(7) 5_557 ? Yb2 O37 2.469(14) . ? S1 O11 1.450(4) . ? S1 O10 1.453(4) . ? S1 O9 1.480(4) . ? S1 C1 1.803(5) . ? S2 O13 1.450(4) . ? S2 O14 1.455(4) . ? S2 O12 1.481(5) . ? S2 C2 1.755(5) . ? S3 O17 1.419(5) . ? S3 O16 1.434(5) . ? S3 O15 1.467(4) . ? S3 C3 1.779(7) . ? O18 H18 0.8057 . ? O19 H19A 0.9199 . ? O19 H19B 0.8120 . ? O20 H20A 0.8860 . ? O20 H20B 0.9247 . ? O21 N1 1.232(12) . ? O22 N1 1.213(11) . ? O23 N1 1.412(12) . ? O24 H24 0.8513 . ? O25 H25A 0.9894 . ? O25 H25B 0.8732 . ? O26 H26A 0.9795 . ? O26 H26B 0.9972 . ? O27 H27A 0.9446 . ? O27 H27B 0.9434 . ? O28 C4 1.243(7) . ? O29 C7 1.236(7) . ? O30 C10 1.245(7) . ? O31 C13 1.239(9) . ? O32 C16 1.233(7) . ? O33 C19 1.231(8) . ? O34 H34 0.8593 . ? O36 H36A 0.8451 . ? O36 H36B 0.9064 . ? O37 N14 1.32(2) . ? O38 N14 1.21(3) . ? O39 O39 1.31(4) 6 ? O39 N14 1.35(2) . ? O41 N15 1.219(13) . ? O42 N15 1.202(12) . ? O43 N15 1.394(14) . ? O43 O43 1.56(3) 6 ? O44 H44 0.8408 . ? N1 O23 1.412(12) 6_565 ? N2 C4 1.347(8) . ? N2 C22 1.433(7) . ? N2 C5 1.469(7) . ? N3 C4 1.385(9) . ? N3 C8 1.420(9) . ? N3 C6 1.454(7) . ? N4 C7 1.348(10) . ? N4 C6 1.432(8) . ? N4 C9 1.433(10) . ? N5 C7 1.382(9) . ? N5 C23 1.446(7) . ? N5 C5 1.451(7) . ? N6 C10 1.368(9) . ? N6 C11 1.434(9) . ? N6 C8 1.451(9) . ? N7 C10 1.367(9) . ? N7 C12 1.430(8) . ? N7 C14 1.446(10) . ? N8 C13 1.364(9) . ? N8 C12 1.450(9) . ? N8 C15 1.457(10) . ? N9 C13 1.348(10) . ? N9 C11 1.428(9) . ? N9 C9 1.450(9) . ? N10 C16 1.341(9) . ? N10 C14 1.420(11) . ? N10 C17 1.445(8) . ? N11 C16 1.366(9) . ? N11 C20 1.438(8) . ? N11 C18 1.452(8) . ? N12 C19 1.357(10) . ? N12 C21 1.430(9) . ? N12 C18 1.460(9) . ? N13 C19 1.317(12) . ? N13 C15 1.459(12) . ? N13 C17 1.472(8) . ? N14 O39 1.35(2) 6 ? N15 O43 1.394(14) 6 ? C1 C2 1.530(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.380(14) 7 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.542(11) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.530(12) . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C18 1.527(13) . ? C17 H17 0.9800 . ? C18 H18A 0.9800 . ? C20 N11 1.438(8) 6 ? C20 H20C 0.9700 . ? C20 H20D 0.9700 . ? C21 N12 1.429(9) 6 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N2 1.433(7) 6 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N5 1.446(7) 6 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 U1 O1 178.2(2) . . ? O2 U1 O18 91.91(16) . . ? O1 U1 O18 89.60(16) . . ? O2 U1 O18 91.91(16) . 6_565 ? O1 U1 O18 89.60(16) . 6_565 ? O18 U1 O18 68.95(19) . 6_565 ? O2 U1 O19 90.9(2) . . ? O1 U1 O19 87.2(2) . . ? O18 U1 O19 145.39(10) . . ? O18 U1 O19 145.39(10) 6_565 . ? O2 U1 O9 89.77(10) . 6_565 ? O1 U1 O9 89.68(10) . 6_565 ? O18 U1 O9 141.76(13) . 6_565 ? O18 U1 O9 72.82(13) 6_565 6_565 ? O19 U1 O9 72.71(8) . 6_565 ? O2 U1 O9 89.77(10) . . ? O1 U1 O9 89.68(10) . . ? O18 U1 O9 72.82(13) . . ? O18 U1 O9 141.76(13) 6_565 . ? O19 U1 O9 72.71(8) . . ? O9 U1 O9 145.40(17) 6_565 . ? O3 U2 O4 179.5(3) . . ? O3 U2 O18 87.45(17) . 6_565 ? O4 U2 O18 92.13(18) . 6_565 ? O3 U2 O18 87.45(17) . . ? O4 U2 O18 92.13(18) . . ? O18 U2 O18 69.89(19) 6_565 . ? O3 U2 O21 93.2(3) . . ? O4 U2 O21 87.3(3) . . ? O18 U2 O21 145.05(10) 6_565 . ? O18 U2 O21 145.05(10) . . ? O3 U2 O20 91.58(12) . . ? O4 U2 O20 88.57(12) . . ? O18 U2 O20 142.46(13) 6_565 . ? O18 U2 O20 72.58(13) . . ? O21 U2 O20 72.48(9) . . ? O3 U2 O20 91.58(12) . 6_565 ? O4 U2 O20 88.57(12) . 6_565 ? O18 U2 O20 72.58(13) 6_565 6_565 ? O18 U2 O20 142.46(13) . 6_565 ? O21 U2 O20 72.48(9) . 6_565 ? O20 U2 O20 144.93(18) . 6_565 ? O6 U3 O5 179.6(2) . . ? O6 U3 O24 91.14(15) . . ? O5 U3 O24 89.18(16) . . ? O6 U3 O24 91.14(15) . 6 ? O5 U3 O24 89.18(16) . 6 ? O24 U3 O24 69.93(18) . 6 ? O6 U3 O25 91.3(2) . . ? O5 U3 O25 88.3(2) . . ? O24 U3 O25 144.95(9) . . ? O24 U3 O25 144.95(9) 6 . ? O6 U3 O15 90.06(11) . 6 ? O5 U3 O15 89.81(11) . 6 ? O24 U3 O15 144.08(13) . 6 ? O24 U3 O15 74.16(13) 6 6 ? O25 U3 O15 70.88(9) . 6 ? O6 U3 O15 90.06(11) . . ? O5 U3 O15 89.81(11) . . ? O24 U3 O15 74.16(13) . . ? O24 U3 O15 144.08(13) 6 . ? O25 U3 O15 70.88(9) . . ? O15 U3 O15 141.75(18) 6 . ? O8 U4 O7 177.9(2) . . ? O8 U4 O24 92.68(16) . 6 ? O7 U4 O24 89.04(16) . 6 ? O8 U4 O24 92.68(16) . . ? O7 U4 O24 89.04(16) . . ? O24 U4 O24 70.40(19) 6 . ? O8 U4 O27 90.8(2) . . ? O7 U4 O27 87.1(2) . . ? O24 U4 O27 144.60(10) 6 . ? O24 U4 O27 144.60(10) . . ? O8 U4 O26 88.50(10) . . ? O7 U4 O26 90.86(10) . . ? O24 U4 O26 142.80(12) 6 . ? O24 U4 O26 72.40(12) . . ? O27 U4 O26 72.48(8) . . ? O8 U4 O26 88.50(10) . 6 ? O7 U4 O26 90.86(10) . 6 ? O24 U4 O26 72.40(12) 6 6 ? O24 U4 O26 142.80(12) . 6 ? O27 U4 O26 72.48(8) . 6 ? O26 U4 O26 144.79(16) . 6 ? O28 Yb1 O28 77.7(2) . 6 ? O28 Yb1 O12 74.64(14) . . ? O28 Yb1 O12 120.86(16) 6 . ? O28 Yb1 O12 120.86(16) . 6 ? O28 Yb1 O12 74.64(14) 6 6 ? O12 Yb1 O12 76.7(2) . 6 ? O28 Yb1 O36 140.63(15) . 6 ? O28 Yb1 O36 78.24(16) 6 6 ? O12 Yb1 O36 144.73(14) . 6 ? O12 Yb1 O36 81.36(18) 6 6 ? O28 Yb1 O36 78.24(16) . . ? O28 Yb1 O36 140.63(15) 6 . ? O12 Yb1 O36 81.36(18) . . ? O12 Yb1 O36 144.73(14) 6 . ? O36 Yb1 O36 102.4(3) 6 . ? O28 Yb1 O34 140.70(11) . . ? O28 Yb1 O34 140.70(11) 6 . ? O12 Yb1 O34 75.69(15) . . ? O12 Yb1 O34 75.69(15) 6 . ? O36 Yb1 O34 72.31(13) 6 . ? O36 Yb1 O34 72.31(13) . . ? O28 Yb1 O35 74.66(19) . . ? O28 Yb1 O35 74.66(19) 6 . ? O12 Yb1 O35 140.93(11) . . ? O12 Yb1 O35 140.93(11) 6 . ? O36 Yb1 O35 69.20(17) 6 . ? O36 Yb1 O35 69.20(17) . . ? O34 Yb1 O35 116.5(3) . . ? O40 Yb2 O33 141.8(3) . 6 ? O40 Yb2 O33 87.2(3) 6 6 ? O40 Yb2 O33 87.2(3) . . ? O40 Yb2 O33 141.8(3) 6 . ? O33 Yb2 O33 95.6(4) 6 . ? O40 Yb2 O33 72.6(3) . 2_557 ? O40 Yb2 O33 118.0(3) 6 2_557 ? O33 Yb2 O33 145.40(11) 6 2_557 ? O33 Yb2 O33 79.1(3) . 2_557 ? O40 Yb2 O33 118.0(3) . 5_557 ? O40 Yb2 O33 72.6(3) 6 5_557 ? O33 Yb2 O33 79.1(3) 6 5_557 ? O33 Yb2 O33 145.39(11) . 5_557 ? O33 Yb2 O33 86.2(3) 2_557 5_557 ? O40 Yb2 O37 74.7(4) . . ? O40 Yb2 O37 74.7(4) 6 . ? O33 Yb2 O37 70.5(3) 6 . ? O33 Yb2 O37 70.5(3) . . ? O33 Yb2 O37 135.88(18) 2_557 . ? O33 Yb2 O37 135.88(18) 5_557 . ? O11 S1 O10 113.9(3) . . ? O11 S1 O9 113.1(2) . . ? O10 S1 O9 111.0(2) . . ? O11 S1 C1 107.4(2) . . ? O10 S1 C1 106.9(3) . . ? O9 S1 C1 103.6(2) . . ? O13 S2 O14 112.8(2) . . ? O13 S2 O12 113.5(3) . . ? O14 S2 O12 112.2(3) . . ? O13 S2 C2 104.9(3) . . ? O14 S2 C2 107.1(3) . . ? O12 S2 C2 105.6(3) . . ? O17 S3 O16 114.0(3) . . ? O17 S3 O15 113.0(3) . . ? O16 S3 O15 110.3(3) . . ? O17 S3 C3 109.4(4) . . ? O16 S3 C3 104.8(4) . . ? O15 S3 C3 104.5(3) . . ? S1 O9 U1 140.4(2) . . ? S2 O12 Yb1 140.9(2) . . ? S3 O15 U3 143.0(3) . . ? U2 O18 U1 108.82(16) . . ? U2 O18 H18 110.6 . . ? U1 O18 H18 114.3 . . ? U1 O19 H19A 127.1 . . ? U1 O19 H19B 127.1 . . ? H19A O19 H19B 105.8 . . ? U2 O20 H20A 131.5 . . ? U2 O20 H20B 128.5 . . ? H20A O20 H20B 99.5 . . ? N1 O21 U2 127.2(7) . . ? U4 O24 U3 108.47(16) . . ? U4 O24 H24 106.7 . . ? U3 O24 H24 106.6 . . ? U3 O25 H25A 142.8 . . ? U3 O25 H25B 121.0 . . ? H25A O25 H25B 96.2 . . ? U4 O26 H26A 126.2 . . ? U4 O26 H26B 135.5 . . ? H26A O26 H26B 97.9 . . ? U4 O27 H27A 143.2 . . ? U4 O27 H27B 121.5 . . ? H27A O27 H27B 95.3 . . ? C4 O28 Yb1 157.6(5) . . ? C19 O33 Yb2 140.5(7) . . ? C19 O33 Yb2 143.6(7) . 5_557 ? Yb1 O34 H34 116.7 . . ? Yb1 O36 H36A 109.0 . . ? Yb1 O36 H36B 104.8 . . ? H36A O36 H36B 103.4 . . ? N14 O37 Yb2 136.1(14) . . ? O39 O39 N14 61.1(10) 6 . ? N15 O43 O43 56.0(7) . 6 ? O22 N1 O21 125.2(12) . . ? O22 N1 O23 112.3(8) . 6_565 ? O21 N1 O23 105.7(7) . 6_565 ? O22 N1 O23 112.3(8) . . ? O21 N1 O23 105.7(7) . . ? O23 N1 O23 89.6(12) 6_565 . ? C4 N2 C22 122.9(6) . . ? C4 N2 C5 111.1(6) . . ? C22 N2 C5 125.9(6) . . ? C4 N3 C8 122.9(5) . . ? C4 N3 C6 111.1(6) . . ? C8 N3 C6 124.5(6) . . ? C7 N4 C6 112.3(7) . . ? C7 N4 C9 122.7(6) . . ? C6 N4 C9 124.8(7) . . ? C7 N5 C23 123.8(6) . . ? C7 N5 C5 110.1(6) . . ? C23 N5 C5 123.5(6) . . ? C10 N6 C11 111.1(7) . . ? C10 N6 C8 121.7(5) . . ? C11 N6 C8 123.6(6) . . ? C10 N7 C12 111.6(7) . . ? C10 N7 C14 124.3(6) . . ? C12 N7 C14 123.6(6) . . ? C13 N8 C12 111.0(7) . . ? C13 N8 C15 122.8(6) . . ? C12 N8 C15 123.8(7) . . ? C13 N9 C11 112.7(7) . . ? C13 N9 C9 123.4(6) . . ? C11 N9 C9 123.8(7) . . ? C16 N10 C14 122.8(6) . . ? C16 N10 C17 112.8(8) . . ? C14 N10 C17 124.3(7) . . ? C16 N11 C20 122.7(6) . . ? C16 N11 C18 111.3(7) . . ? C20 N11 C18 124.4(7) . . ? C19 N12 C21 123.9(7) . . ? C19 N12 C18 111.9(8) . . ? C21 N12 C18 124.2(7) . . ? C19 N13 C15 122.8(6) . . ? C19 N13 C17 113.4(7) . . ? C15 N13 C17 122.5(8) . . ? O38 N14 O37 122(2) . . ? O38 N14 O39 110(2) . . ? O37 N14 O39 120(2) . . ? O38 N14 O39 110(2) . 6 ? O37 N14 O39 120(2) . 6 ? O39 N14 O39 58(2) . 6 ? O42 N15 O41 126.3(11) . . ? O42 N15 O43 111.5(10) . 6 ? O41 N15 O43 112.4(10) . 6 ? O42 N15 O43 111.5(10) . . ? O41 N15 O43 112.4(10) . . ? O43 N15 O43 68.1(14) 6 . ? C2 C1 S1 109.7(4) . . ? C2 C1 H1A 109.7 . . ? S1 C1 H1A 109.7 . . ? C2 C1 H1B 109.7 . . ? S1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 C2 S2 112.0(4) . . ? C1 C2 H2A 109.2 . . ? S2 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? S2 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C3 C3 S3 117.1(8) 7 . ? C3 C3 H3A 108.0 7 . ? S3 C3 H3A 108.0 . . ? C3 C3 H3B 108.0 7 . ? S3 C3 H3B 108.0 . . ? H3A C3 H3B 107.3 . . ? O28 C4 N2 126.1(7) . . ? O28 C4 N3 124.0(6) . . ? N2 C4 N3 109.9(5) . . ? N5 C5 N2 112.6(6) . . ? N5 C5 C6 103.5(5) . . ? N2 C5 C6 103.6(5) . . ? N5 C5 H5 112.1 . . ? N2 C5 H5 112.1 . . ? C6 C5 H5 112.1 . . ? N4 C6 N3 113.0(5) . . ? N4 C6 C5 103.6(6) . . ? N3 C6 C5 103.4(6) . . ? N4 C6 H6 112.1 . . ? N3 C6 H6 112.1 . . ? C5 C6 H6 112.1 . . ? O29 C7 N4 126.1(7) . . ? O29 C7 N5 124.4(8) . . ? N4 C7 N5 109.4(6) . . ? N3 C8 N6 112.8(5) . . ? N3 C8 H8A 109.0 . . ? N6 C8 H8A 109.0 . . ? N3 C8 H8B 109.0 . . ? N6 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N4 C9 N9 113.9(6) . . ? N4 C9 H9A 108.8 . . ? N9 C9 H9A 108.8 . . ? N4 C9 H9B 108.8 . . ? N9 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? O30 C10 N7 124.4(7) . . ? O30 C10 N6 126.8(7) . . ? N7 C10 N6 108.8(6) . . ? N9 C11 N6 114.9(6) . . ? N9 C11 C12 103.6(7) . . ? N6 C11 C12 104.0(6) . . ? N9 C11 H11 111.3 . . ? N6 C11 H11 111.3 . . ? C12 C11 H11 111.3 . . ? N7 C12 N8 115.3(7) . . ? N7 C12 C11 103.8(6) . . ? N8 C12 C11 103.2(6) . . ? N7 C12 H12 111.3 . . ? N8 C12 H12 111.3 . . ? C11 C12 H12 111.3 . . ? O31 C13 N9 127.6(7) . . ? O31 C13 N8 123.7(8) . . ? N9 C13 N8 108.7(7) . . ? N10 C14 N7 114.7(6) . . ? N10 C14 H14A 108.6 . . ? N7 C14 H14A 108.6 . . ? N10 C14 H14B 108.6 . . ? N7 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N8 C15 N13 113.3(6) . . ? N8 C15 H15A 108.9 . . ? N13 C15 H15A 108.9 . . ? N8 C15 H15B 108.9 . . ? N13 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? O32 C16 N10 125.1(8) . . ? O32 C16 N11 125.9(7) . . ? N10 C16 N11 108.8(6) . . ? N10 C17 N13 114.5(6) . . ? N10 C17 C18 103.3(6) . . ? N13 C17 C18 102.2(7) . . ? N10 C17 H17 112.0 . . ? N13 C17 H17 112.0 . . ? C18 C17 H17 112.0 . . ? N11 C18 N12 113.4(7) . . ? N11 C18 C17 103.6(6) . . ? N12 C18 C17 103.4(6) . . ? N11 C18 H18A 112.0 . . ? N12 C18 H18A 112.0 . . ? C17 C18 H18A 112.0 . . ? O33 C19 N13 123.9(9) . . ? O33 C19 N12 127.0(10) . . ? N13 C19 N12 109.0(6) . . ? N11 C20 N11 112.9(7) 6 . ? N11 C20 H20C 109.0 6 . ? N11 C20 H20C 109.0 . . ? N11 C20 H20D 109.0 6 . ? N11 C20 H20D 109.0 . . ? H20C C20 H20D 107.8 . . ? N12 C21 N12 115.4(9) 6 . ? N12 C21 H21A 108.4 6 . ? N12 C21 H21A 108.4 . . ? N12 C21 H21B 108.4 6 . ? N12 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? N2 C22 N2 113.3(7) . 6 ? N2 C22 H22A 108.9 . . ? N2 C22 H22A 108.9 6 . ? N2 C22 H22B 108.9 . . ? N2 C22 H22B 108.9 6 . ? H22A C22 H22B 107.7 . . ? N5 C23 N5 115.0(7) . 6 ? N5 C23 H23A 108.5 . . ? N5 C23 H23A 108.5 6 . ? N5 C23 H23B 108.5 . . ? N5 C23 H23B 108.5 6 . ? H23A C23 H23B 107.5 . . ? 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 O18 H18 O16 0.81 1.98 2.778(6) 171.8 . O19 H19A O44 0.92 1.82 2.731(8) 173.3 . O19 H19B O46 0.81 1.87 2.641(11) 157.5 . O20 H20A O17 0.89 1.98 2.821(6) 157.7 . O20 H20B O31 0.92 1.90 2.823(6) 177.8 1_554 O24 H24 O10 0.85 1.95 2.785(6) 167.0 . O25 H25A O4 0.99 1.86 2.774(9) 152.8 7 O25 H25B O47 0.87 1.70 2.536(9) 159.4 . O26 H26A O11 0.98 1.87 2.844(6) 172.9 . O26 H26B O14 1.00 1.75 2.731(5) 166.4 7_556 O27 H27A O44 0.94 1.85 2.712(8) 149.8 7_556 O27 H27B O45 0.94 1.75 2.625(12) 153.6 7_556 O34 H34 O32 0.86 2.23 2.709(6) 115.0 2_556 O36 H36A O30 0.85 2.11 2.782(6) 135.9 . O36 H36B O48 0.91 2.01 2.771(11) 140.8 . O44 H44 O13 0.84 1.96 2.773(6) 161.7 7_556