# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _publ_contact_author ; Dr Marinella Mazzanti LCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; loop_ _publ_author_name _publ_author_address L.Chatelain ; SCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; V.Mougel ; SCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; J.Pecaut ; sCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; M.Mazzanti ; sCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; _publ_section_title ; A stable unsupported cation-cation trimer of pentavalent uranyl exhibiting magnetic communication. ; _publ_contact_author_email marinella.mazzanti@cea.fr _publ_contact_author_name 'Dr Marinella Mazzanti' data_1 _database_code_depnum_ccdc_archive 'CCDC 848286' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H77 N12 O7 U3' _chemical_formula_weight 2152.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.7294(13) _cell_length_b 16.6323(7) _cell_length_c 29.5917(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.954(5) _cell_angle_gamma 90.00 _cell_volume 8232.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1722 _cell_measurement_theta_min 3.3962 _cell_measurement_theta_max 28.8274 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4132 _exptl_absorpt_coefficient_mu 5.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4771 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53639 _diffrn_reflns_av_R_equivalents 0.1477 _diffrn_reflns_av_sigmaI/netI 0.1378 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15282 _reflns_number_gt 9181 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -45.00 51.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - -18.7175 77.0000 -120.0000 96 #__ type_ start__ end____ width___ exp.time_ 2 omega -40.00 -9.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - -18.7175 77.0000 -30.0000 31 #__ type_ start__ end____ width___ exp.time_ 3 omega -9.00 77.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 16.9988 37.0000 120.0000 86 #__ type_ start__ end____ width___ exp.time_ 4 omega 11.00 45.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 16.9988 77.0000 -90.0000 34 #__ type_ start__ end____ width___ exp.time_ 5 omega -12.00 77.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 16.9988 77.0000 120.0000 89 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15282 _refine_ls_number_parameters 1016 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1377 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.14530(3) 0.75343(2) 0.026667(15) 0.02584(15) Uani 1 1 d . . . O1U1 O 0.2591(6) 0.7510(4) 0.0294(3) 0.032(2) Uani 1 1 d . . . O2U1 O 0.0355(6) 0.7534(4) 0.0207(3) 0.033(2) Uani 1 1 d . . . N1 N 0.1280(7) 0.6010(6) 0.0483(4) 0.032(3) Uani 1 1 d . . . N2 N 0.1570(7) 0.6554(6) -0.0377(4) 0.027(3) Uani 1 1 d . . . N3 N 0.1655(7) 0.8370(6) -0.0439(4) 0.027(3) Uani 1 1 d . . . N4 N 0.1253(8) 0.9080(6) 0.0352(4) 0.033(3) Uani 1 1 d . . . C1 C 0.1193(9) 0.5750(7) 0.0891(4) 0.030(4) Uani 1 1 d . . . H1 H 0.1275 0.6115 0.1134 0.036 Uiso 1 1 calc R . . C2 C 0.0983(10) 0.4957(8) 0.0992(5) 0.046(5) Uani 1 1 d . . . H2 H 0.0930 0.4790 0.1297 0.055 Uiso 1 1 calc R . . C3 C 0.0857(10) 0.4423(8) 0.0645(5) 0.043(4) Uani 1 1 d . . . H3 H 0.0724 0.3880 0.0708 0.051 Uiso 1 1 calc R . . C4 C 0.0925(9) 0.4679(7) 0.0202(5) 0.036(4) Uani 1 1 d . . . C5 C 0.0785(10) 0.4170(8) -0.0174(5) 0.042(4) Uani 1 1 d . . . H5 H 0.0645 0.3624 -0.0127 0.051 Uiso 1 1 calc R . . C6 C 0.0850(10) 0.4453(8) -0.0598(5) 0.044(5) Uani 1 1 d . . . H6 H 0.0723 0.4109 -0.0846 0.053 Uiso 1 1 calc R . . C7 C 0.1102(9) 0.5252(6) -0.0684(4) 0.032(4) Uani 1 1 d . . . H7 H 0.1155 0.5435 -0.0986 0.039 Uiso 1 1 calc R . . C8 C 0.1272(9) 0.5764(7) -0.0324(4) 0.027(3) Uani 1 1 d U . . C9 C 0.1156(9) 0.5480(7) 0.0126(4) 0.028(4) Uani 1 1 d . . . C10 C 0.2077(10) 0.6649(8) -0.0704(5) 0.036(4) Uani 1 1 d . . . H10 H 0.2230 0.6171 -0.0855 0.043 Uiso 1 1 calc R . . C11 C 0.2427(9) 0.7358(8) -0.0860(4) 0.033(3) Uani 1 1 d U . . C12 C 0.3121(10) 0.7270(7) -0.1174(4) 0.037(4) Uani 1 1 d . . . C13 C 0.3028(12) 0.6896(8) -0.1598(5) 0.054(5) Uani 1 1 d . . . H13 H 0.2520 0.6710 -0.1700 0.065 Uiso 1 1 calc R . . C14 C 0.3723(12) 0.6801(8) -0.1873(5) 0.046(5) Uani 1 1 d . . . H14 H 0.3679 0.6530 -0.2154 0.056 Uiso 1 1 calc R . . C15 C 0.4452(11) 0.7102(8) -0.1730(5) 0.043(4) Uani 1 1 d . . . C16 C 0.4528(11) 0.7452(8) -0.1318(5) 0.051(5) Uani 1 1 d . . . H16 H 0.5035 0.7652 -0.1221 0.061 Uiso 1 1 calc R . . C17 C 0.3892(9) 0.7523(7) -0.1042(4) 0.029(3) Uani 1 1 d . . . H17 H 0.3971 0.7751 -0.0750 0.034 Uiso 1 1 calc R . . C18 C 0.5199(12) 0.6966(11) -0.2019(5) 0.071(6) Uani 1 1 d . . . H18A H 0.5646 0.7280 -0.1894 0.106 Uiso 1 1 calc R . . H18B H 0.5086 0.7136 -0.2330 0.106 Uiso 1 1 calc R . . H18C H 0.5340 0.6394 -0.2016 0.106 Uiso 1 1 calc R . . C19 C 0.2201(9) 0.8140(7) -0.0743(4) 0.029(4) Uani 1 1 d . . . H19 H 0.2467 0.8562 -0.0896 0.034 Uiso 1 1 calc R . . C20 C 0.1433(9) 0.9181(7) -0.0450(4) 0.029(4) Uani 1 1 d . . . C21 C 0.1394(10) 0.9648(7) -0.0838(4) 0.035(4) Uani 1 1 d . . . H21 H 0.1528 0.9418 -0.1121 0.042 Uiso 1 1 calc R . . C22 C 0.1158(10) 1.0456(7) -0.0816(5) 0.044(5) Uani 1 1 d . . . H22 H 0.1151 1.0767 -0.1086 0.052 Uiso 1 1 calc R . . C23 C 0.0945(9) 1.0800(7) -0.0431(5) 0.032(4) Uani 1 1 d . . . H23 H 0.0778 1.1346 -0.0427 0.039 Uiso 1 1 calc R . . C24 C 0.0969(9) 1.0357(7) -0.0033(4) 0.031(4) Uani 1 1 d . . . C25 C 0.0759(9) 1.0674(8) 0.0397(5) 0.034(4) Uani 1 1 d . . . H25 H 0.0579 1.1214 0.0416 0.041 Uiso 1 1 calc R . . C26 C 0.0808(9) 1.0226(8) 0.0778(4) 0.032(4) Uani 1 1 d . . . H26 H 0.0692 1.0452 0.1065 0.039 Uiso 1 1 calc R . . C27 C 0.1038(9) 0.9408(7) 0.0736(4) 0.032(4) Uani 1 1 d . . . H27 H 0.1037 0.9081 0.0999 0.039 Uiso 1 1 calc R . . C28 C 0.1210(8) 0.9545(6) -0.0032(4) 0.020(3) Uani 1 1 d . . . U2 U 0.38826(3) 0.75244(3) 0.063658(15) 0.02639(15) Uani 1 1 d . . . O1U2 O 0.3276(6) 0.7589(4) 0.1188(3) 0.026(2) Uani 1 1 d . . . O2U2 O 0.4504(6) 0.7507(4) 0.0128(3) 0.033(2) Uani 1 1 d . . . N31 N 0.3761(8) 0.5977(6) 0.0480(4) 0.033(3) Uani 1 1 d . . . N32 N 0.4859(7) 0.6639(5) 0.1073(3) 0.027(3) Uani 1 1 d . . . N33 N 0.4832(7) 0.8432(6) 0.1065(3) 0.025(3) Uani 1 1 d . . . N34 N 0.3790(7) 0.9043(6) 0.0439(3) 0.028(3) Uani 1 1 d . . . C31 C 0.3216(9) 0.5669(7) 0.0205(4) 0.031(4) Uani 1 1 d . . . H31 H 0.2789 0.6002 0.0102 0.037 Uiso 1 1 calc R . . C32 C 0.3241(11) 0.4880(8) 0.0059(5) 0.050(5) Uani 1 1 d . . . H32 H 0.2816 0.4673 -0.0124 0.059 Uiso 1 1 calc R . . C33 C 0.3872(12) 0.4393(9) 0.0175(5) 0.052(5) Uani 1 1 d . . . H33 H 0.3902 0.3859 0.0063 0.062 Uiso 1 1 calc R . . C34 C 0.4474(10) 0.4697(7) 0.0463(5) 0.037(4) Uani 1 1 d . . . C35 C 0.5146(10) 0.4249(8) 0.0602(5) 0.043(4) Uani 1 1 d U . . H35 H 0.5208 0.3711 0.0501 0.052 Uiso 1 1 calc R . . C36 C 0.5716(10) 0.4589(8) 0.0884(5) 0.041(4) Uani 1 1 d . . . H36 H 0.6166 0.4278 0.0976 0.049 Uiso 1 1 calc R . . C37 C 0.5649(10) 0.5373(7) 0.1039(5) 0.038(4) Uani 1 1 d . . . H37 H 0.6055 0.5595 0.1229 0.046 Uiso 1 1 calc R . . C38 C 0.4991(10) 0.5830(8) 0.0916(5) 0.036(4) Uani 1 1 d . . . C39 C 0.4395(10) 0.5500(7) 0.0617(4) 0.029(4) Uani 1 1 d . . . C40 C 0.5101(9) 0.6788(7) 0.1496(4) 0.028(3) Uani 1 1 d . . . H40 H 0.5270 0.6342 0.1674 0.034 Uiso 1 1 calc R . . C41 C 0.5125(9) 0.7542(8) 0.1699(4) 0.031(3) Uani 1 1 d . . . C42 C 0.5206(9) 0.7544(7) 0.2206(4) 0.032(4) Uani 1 1 d . . . C43 C 0.5910(10) 0.7257(8) 0.2435(5) 0.041(4) Uani 1 1 d . . . H43 H 0.6349 0.7070 0.2265 0.050 Uiso 1 1 calc R . . C44 C 0.5955(10) 0.7249(8) 0.2903(5) 0.046(4) Uani 1 1 d . . . H44 H 0.6420 0.7049 0.3053 0.055 Uiso 1 1 calc R . . C45 C 0.5309(10) 0.7539(10) 0.3157(5) 0.050(5) Uani 1 1 d . . . C46 C 0.4635(10) 0.7806(7) 0.2938(4) 0.037(4) Uani 1 1 d . . . H46 H 0.4198 0.7993 0.3109 0.044 Uiso 1 1 calc R . . C47 C 0.4578(9) 0.7808(7) 0.2478(4) 0.033(3) Uani 1 1 d U . . H47 H 0.4099 0.7995 0.2337 0.040 Uiso 1 1 calc R . . C48 C 0.5323(11) 0.7482(9) 0.3677(4) 0.060(5) Uani 1 1 d . . . H48A H 0.4791 0.7609 0.3791 0.089 Uiso 1 1 calc R . . H48B H 0.5714 0.7864 0.3801 0.089 Uiso 1 1 calc R . . H48C H 0.5471 0.6935 0.3768 0.089 Uiso 1 1 calc R . . C49 C 0.5041(9) 0.8281(7) 0.1492(4) 0.027(3) Uani 1 1 d U . . H49 H 0.5146 0.8737 0.1677 0.033 Uiso 1 1 calc R . . C50 C 0.4949(9) 0.9220(7) 0.0911(4) 0.025(3) Uani 1 1 d U . . C51 C 0.5578(9) 0.9711(8) 0.1048(4) 0.035(4) Uani 1 1 d . . . H51 H 0.5973 0.9502 0.1250 0.042 Uiso 1 1 calc R . . C52 C 0.5649(10) 1.0504(8) 0.0898(5) 0.043(4) Uani 1 1 d . . . H52 H 0.6073 1.0831 0.1011 0.052 Uiso 1 1 calc R . . C53 C 0.5112(10) 1.0815(7) 0.0590(4) 0.035(4) Uani 1 1 d . . . H53 H 0.5174 1.1350 0.0482 0.042 Uiso 1 1 calc R . . C54 C 0.4469(10) 1.0340(7) 0.0433(4) 0.033(4) Uani 1 1 d . . . C55 C 0.3883(9) 1.0625(7) 0.0126(4) 0.032(4) Uani 1 1 d . . . H55 H 0.3912 1.1162 0.0019 0.038 Uiso 1 1 calc R . . C56 C 0.3274(10) 1.0141(7) -0.0021(5) 0.037(4) Uani 1 1 d . . . H56 H 0.2877 1.0327 -0.0228 0.045 Uiso 1 1 calc R . . C57 C 0.3264(9) 0.9351(7) 0.0152(4) 0.032(4) Uani 1 1 d . . . H57 H 0.2840 0.9010 0.0052 0.039 Uiso 1 1 calc R . . C58 C 0.4402(10) 0.9549(7) 0.0581(5) 0.032(4) Uani 1 1 d . . . U3 U 0.21232(4) 0.77097(3) 0.162992(16) 0.02719(15) Uani 1 1 d . . . O1U3 O 0.1563(5) 0.7622(4) 0.1066(3) 0.026(2) Uani 1 1 d . . . O2U3 O 0.2605(6) 0.7780(5) 0.2184(3) 0.036(2) Uani 1 1 d . . . N61 N 0.2468(8) 0.6177(6) 0.1723(4) 0.031(3) Uani 1 1 d . . . N62 N 0.1007(8) 0.6854(6) 0.1933(3) 0.028(3) Uani 1 1 d . . . N63 N 0.0985(7) 0.8634(6) 0.1856(3) 0.027(3) Uani 1 1 d U . . N64 N 0.2418(7) 0.9254(6) 0.1592(4) 0.025(3) Uani 1 1 d . . . C61 C 0.3138(10) 0.5856(8) 0.1594(4) 0.032(4) Uani 1 1 d . . . H61 H 0.3486 0.6173 0.1417 0.038 Uiso 1 1 calc R . . C62 C 0.3371(11) 0.5073(9) 0.1702(5) 0.045(5) Uani 1 1 d . . . H62 H 0.3864 0.4861 0.1600 0.054 Uiso 1 1 calc R . . C63 C 0.2867(11) 0.4622(8) 0.1958(5) 0.042(5) Uani 1 1 d . . . H63 H 0.3007 0.4086 0.2037 0.050 Uiso 1 1 calc R . . C64 C 0.2154(10) 0.4944(8) 0.2101(5) 0.033(4) Uani 1 1 d . . . C65 C 0.1609(11) 0.4510(9) 0.2371(5) 0.042(4) Uani 1 1 d . . . H65 H 0.1735 0.3978 0.2465 0.050 Uiso 1 1 calc R . . C66 C 0.0920(10) 0.4845(8) 0.2493(5) 0.039(4) Uani 1 1 d . . . H66 H 0.0561 0.4547 0.2673 0.047 Uiso 1 1 calc R . . C67 C 0.0716(9) 0.5632(8) 0.2361(5) 0.034(4) Uani 1 1 d . . . H67 H 0.0226 0.5862 0.2454 0.041 Uiso 1 1 calc R . . C68 C 0.1231(10) 0.6073(8) 0.2095(4) 0.032(4) Uani 1 1 d . . . C69 C 0.1954(9) 0.5731(7) 0.1975(4) 0.025(3) Uani 1 1 d . . . C70 C 0.0267(9) 0.6965(7) 0.1808(4) 0.031(4) Uani 1 1 d . . . H70 H -0.0053 0.6498 0.1768 0.037 Uiso 1 1 calc R . . C71 C -0.0110(9) 0.7715(8) 0.1724(4) 0.031(3) Uani 1 1 d . . . C72 C -0.0937(9) 0.7664(7) 0.1505(4) 0.026(3) Uani 1 1 d U . . C73 C -0.1624(11) 0.7902(8) 0.1727(4) 0.041(4) Uani 1 1 d . . . H73 H -0.1585 0.8071 0.2034 0.049 Uiso 1 1 calc R . . C74 C -0.2375(10) 0.7898(8) 0.1507(5) 0.043(4) Uani 1 1 d . . . H74 H -0.2835 0.8075 0.1662 0.052 Uiso 1 1 calc R . . C75 C -0.2445(10) 0.7640(7) 0.1070(4) 0.033(3) Uani 1 1 d U . . C76 C -0.1785(9) 0.7419(6) 0.0843(4) 0.031(4) Uani 1 1 d . . . H76 H -0.1825 0.7249 0.0537 0.037 Uiso 1 1 calc R . . C77 C -0.1058(9) 0.7444(6) 0.1061(5) 0.029(3) Uani 1 1 d . . . H77 H -0.0602 0.7299 0.0892 0.035 Uiso 1 1 calc R . . C78 C -0.3243(10) 0.7628(9) 0.0828(6) 0.057(5) Uani 1 1 d . . . H78A H -0.3193 0.7350 0.0538 0.086 Uiso 1 1 calc R . . H78B H -0.3423 0.8181 0.0775 0.086 Uiso 1 1 calc R . . H78C H -0.3633 0.7347 0.1014 0.086 Uiso 1 1 calc R . . C79 C 0.0230(10) 0.8464(7) 0.1773(4) 0.031(4) Uani 1 1 d . . . H79 H -0.0123 0.8910 0.1743 0.037 Uiso 1 1 calc R . . C80 C 0.1163(10) 0.9455(7) 0.1971(5) 0.033(4) Uani 1 1 d . . . C81 C 0.0665(10) 0.9943(7) 0.2199(4) 0.032(4) Uani 1 1 d . . . H81 H 0.0180 0.9734 0.2314 0.038 Uiso 1 1 calc R . . C82 C 0.0857(11) 1.0754(8) 0.2269(5) 0.043(5) Uani 1 1 d . . . H82 H 0.0486 1.1094 0.2416 0.051 Uiso 1 1 calc R . . C83 C 0.1567(11) 1.1068(8) 0.2129(5) 0.045(5) Uani 1 1 d . . . H83 H 0.1697 1.1611 0.2197 0.054 Uiso 1 1 calc R . . C84 C 0.2114(11) 1.0587(7) 0.1883(5) 0.035(4) Uani 1 1 d . . . C85 C 0.2849(11) 1.0841(8) 0.1724(5) 0.040(4) Uani 1 1 d . . . H85 H 0.3007 1.1382 0.1777 0.048 Uiso 1 1 calc R . . C86 C 0.3347(11) 1.0353(8) 0.1498(5) 0.043(4) Uani 1 1 d . . . H86 H 0.3836 1.0543 0.1379 0.052 Uiso 1 1 calc R . . C87 C 0.3101(10) 0.9528(8) 0.1445(4) 0.035(4) Uani 1 1 d . . . H87 H 0.3449 0.9166 0.1298 0.042 Uiso 1 1 calc R . . C88 C 0.1899(10) 0.9759(7) 0.1808(4) 0.029(4) Uani 1 1 d . . . O91 O 0.7765(8) 0.4917(6) 0.2406(4) 0.064(4) Uani 1 1 d . . . C91 C 0.8310(14) 0.5260(11) 0.2088(6) 0.068(6) Uani 1 1 d . . . H91 H 0.8610 0.5713 0.2233 0.082 Uiso 1 1 calc R . . C92 C 0.7831(13) 0.5574(10) 0.1674(6) 0.075(7) Uani 1 1 d . . . H92A H 0.7565 0.5122 0.1520 0.113 Uiso 1 1 calc R . . H92B H 0.8195 0.5839 0.1465 0.113 Uiso 1 1 calc R . . H92C H 0.7428 0.5960 0.1773 0.113 Uiso 1 1 calc R . . C93 C 0.8885(12) 0.4582(10) 0.1977(6) 0.068(6) Uani 1 1 d . . . H93A H 0.9172 0.4415 0.2253 0.102 Uiso 1 1 calc R . . H93B H 0.9269 0.4769 0.1754 0.102 Uiso 1 1 calc R . . H93C H 0.8585 0.4124 0.1853 0.102 Uiso 1 1 calc R . . C94 C 0.7385(12) 0.5487(11) 0.2683(6) 0.055(5) Uani 1 1 d . . . H94 H 0.7311 0.5996 0.2507 0.066 Uiso 1 1 calc R . . C95 C 0.6555(15) 0.5143(11) 0.2794(7) 0.089(8) Uani 1 1 d . . . H95A H 0.6262 0.5024 0.2512 0.134 Uiso 1 1 calc R . . H95B H 0.6255 0.5539 0.2969 0.134 Uiso 1 1 calc R . . H95C H 0.6619 0.4649 0.2971 0.134 Uiso 1 1 calc R . . C96 C 0.7888(15) 0.5667(14) 0.3104(6) 0.103(8) Uani 1 1 d . . . H96A H 0.7934 0.5181 0.3290 0.155 Uiso 1 1 calc R . . H96B H 0.7632 0.6093 0.3279 0.155 Uiso 1 1 calc R . . H96C H 0.8422 0.5843 0.3016 0.155 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0268(4) 0.0221(3) 0.0286(2) -0.00031(19) 0.0000(2) -0.0010(2) O1U1 0.038(7) 0.021(4) 0.036(4) 0.005(4) -0.009(5) 0.000(4) O2U1 0.018(7) 0.041(5) 0.040(5) -0.001(4) 0.004(5) -0.003(4) N1 0.026(9) 0.035(6) 0.036(7) 0.002(5) 0.012(6) 0.007(5) N2 0.022(9) 0.025(6) 0.035(6) -0.001(5) 0.009(6) 0.005(5) N3 0.018(9) 0.028(6) 0.037(6) 0.006(5) 0.012(6) -0.002(5) N4 0.041(10) 0.033(6) 0.026(6) -0.003(5) -0.001(6) 0.002(6) C1 0.039(11) 0.025(7) 0.025(7) -0.003(5) -0.005(7) 0.008(6) C2 0.058(14) 0.035(8) 0.043(9) 0.016(7) -0.016(9) -0.011(8) C3 0.023(11) 0.031(8) 0.074(11) 0.000(8) -0.011(9) 0.005(7) C4 0.026(11) 0.030(7) 0.051(9) -0.001(7) -0.011(8) 0.007(7) C5 0.034(12) 0.026(7) 0.066(11) -0.010(7) 0.000(9) 0.000(7) C6 0.045(13) 0.036(8) 0.052(10) -0.015(7) -0.009(9) -0.009(7) C7 0.047(12) 0.015(6) 0.034(7) -0.006(5) 0.008(8) 0.004(6) C8 0.027(8) 0.019(5) 0.035(6) -0.011(5) 0.001(6) 0.011(5) C9 0.023(10) 0.030(7) 0.032(7) -0.008(6) -0.004(7) 0.006(6) C10 0.024(11) 0.029(7) 0.053(9) -0.015(7) -0.004(8) 0.006(7) C11 0.030(8) 0.039(6) 0.031(6) 0.005(5) 0.004(6) 0.006(6) C12 0.049(13) 0.026(7) 0.037(7) 0.003(6) -0.003(8) 0.009(7) C13 0.065(16) 0.045(9) 0.051(9) -0.012(8) -0.012(10) -0.004(9) C14 0.051(15) 0.049(9) 0.039(9) -0.012(7) -0.004(9) 0.005(9) C15 0.057(15) 0.036(8) 0.038(8) -0.003(7) 0.015(9) 0.007(8) C16 0.048(14) 0.049(10) 0.056(9) 0.004(8) 0.013(9) -0.018(8) C17 0.018(10) 0.045(8) 0.024(6) -0.004(6) 0.017(6) -0.009(7) C18 0.060(18) 0.097(14) 0.056(11) 0.001(10) 0.029(11) 0.014(12) C19 0.041(11) 0.023(7) 0.022(6) 0.002(5) -0.004(7) -0.008(6) C20 0.031(11) 0.016(6) 0.041(8) 0.008(6) -0.003(8) 0.002(6) C21 0.046(13) 0.026(7) 0.034(8) 0.000(6) 0.011(8) -0.004(7) C22 0.054(14) 0.026(7) 0.051(9) 0.025(7) 0.007(9) 0.004(7) C23 0.027(11) 0.017(6) 0.053(9) 0.007(6) 0.007(8) 0.006(6) C24 0.039(12) 0.021(6) 0.034(8) -0.001(6) -0.004(8) 0.001(6) C25 0.027(11) 0.031(7) 0.045(9) -0.009(6) 0.001(8) 0.014(7) C26 0.024(11) 0.044(8) 0.029(7) -0.020(6) 0.005(7) -0.008(7) C27 0.034(12) 0.035(8) 0.027(7) 0.000(6) 0.006(7) -0.001(7) C28 0.012(9) 0.014(6) 0.032(7) 0.002(5) 0.000(6) -0.004(5) U2 0.0247(4) 0.0238(3) 0.0307(2) -0.0001(2) 0.0024(2) 0.0004(2) O1U2 0.024(7) 0.023(4) 0.031(4) -0.003(3) 0.011(4) 0.002(4) O2U2 0.024(7) 0.038(5) 0.038(5) -0.006(4) 0.008(5) -0.004(4) N31 0.036(10) 0.022(6) 0.041(7) -0.010(5) 0.003(7) -0.005(5) N32 0.021(9) 0.021(5) 0.039(6) 0.000(5) 0.010(6) 0.002(5) N33 0.010(8) 0.034(6) 0.031(6) 0.000(5) 0.004(5) 0.008(5) N34 0.022(9) 0.029(6) 0.032(6) 0.001(5) 0.001(6) -0.013(5) C31 0.018(11) 0.032(7) 0.044(8) -0.005(6) 0.002(8) 0.003(6) C32 0.075(16) 0.037(8) 0.036(8) -0.003(7) -0.009(9) -0.016(9) C33 0.074(17) 0.038(8) 0.043(9) -0.008(7) 0.001(10) -0.004(9) C34 0.040(13) 0.022(7) 0.050(9) -0.003(6) 0.004(9) 0.002(7) C35 0.041(9) 0.039(6) 0.051(7) -0.010(6) 0.011(7) 0.017(6) C36 0.039(13) 0.047(9) 0.037(8) -0.009(7) 0.007(8) 0.017(8) C37 0.039(13) 0.029(7) 0.047(9) -0.006(6) -0.002(9) 0.010(7) C38 0.033(12) 0.030(7) 0.046(9) -0.002(6) 0.007(8) 0.002(7) C39 0.040(12) 0.027(7) 0.022(7) 0.004(5) 0.018(7) 0.003(7) C40 0.019(10) 0.030(7) 0.035(7) -0.003(6) 0.006(7) 0.001(6) C41 0.016(9) 0.049(9) 0.029(6) 0.004(6) 0.004(6) 0.002(7) C42 0.041(11) 0.028(7) 0.028(6) 0.007(6) -0.014(7) -0.012(7) C43 0.031(11) 0.050(8) 0.043(8) 0.004(7) 0.002(8) 0.001(8) C44 0.038(13) 0.049(9) 0.051(9) 0.001(8) -0.015(9) 0.008(8) C45 0.022(11) 0.093(13) 0.034(7) 0.013(8) -0.008(8) 0.003(9) C46 0.041(12) 0.033(7) 0.038(7) 0.007(6) 0.004(8) 0.006(7) C47 0.033(8) 0.033(6) 0.033(6) -0.008(5) -0.006(6) 0.007(6) C48 0.052(14) 0.091(13) 0.034(8) -0.004(8) -0.014(8) 0.016(10) C49 0.020(7) 0.030(6) 0.033(6) 0.001(5) 0.006(6) 0.004(5) C50 0.019(7) 0.027(6) 0.029(6) 0.004(5) 0.003(6) -0.005(5) C51 0.017(11) 0.050(9) 0.038(8) 0.009(7) -0.010(8) 0.008(7) C52 0.039(13) 0.033(8) 0.059(10) 0.000(7) 0.005(9) -0.018(8) C53 0.046(12) 0.020(6) 0.038(8) 0.006(6) -0.003(8) -0.016(7) C54 0.049(13) 0.023(7) 0.028(7) 0.012(5) 0.007(8) -0.009(7) C55 0.033(12) 0.022(7) 0.040(8) 0.003(6) 0.008(8) 0.003(6) C56 0.034(12) 0.026(7) 0.052(9) 0.018(7) 0.007(8) 0.008(7) C57 0.025(11) 0.032(7) 0.041(8) 0.009(6) -0.007(8) -0.002(6) C58 0.025(11) 0.036(8) 0.036(8) 0.004(6) 0.002(7) -0.010(7) U3 0.0274(4) 0.0259(2) 0.0283(2) 0.0004(2) 0.0012(2) -0.0011(2) O1U3 0.017(6) 0.014(4) 0.046(5) -0.001(4) 0.000(4) -0.005(4) O2U3 0.022(7) 0.044(5) 0.043(5) 0.015(4) 0.006(5) -0.005(5) N61 0.029(10) 0.026(6) 0.039(7) 0.004(5) 0.001(6) 0.005(6) N62 0.032(9) 0.025(6) 0.026(6) 0.002(4) 0.010(6) 0.000(5) N63 0.020(7) 0.031(5) 0.029(5) 0.002(4) 0.000(5) 0.008(5) N64 0.016(9) 0.024(6) 0.037(6) -0.004(5) 0.011(6) 0.002(5) C61 0.026(12) 0.041(8) 0.029(7) 0.005(6) 0.006(7) 0.014(7) C62 0.043(13) 0.048(9) 0.045(9) 0.003(7) -0.010(9) 0.008(8) C63 0.045(14) 0.028(8) 0.051(9) 0.002(7) -0.012(9) 0.003(8) C64 0.034(12) 0.029(7) 0.037(8) 0.003(6) -0.008(8) -0.007(7) C65 0.043(14) 0.042(9) 0.040(8) 0.010(7) 0.006(9) 0.002(8) C66 0.032(13) 0.044(9) 0.040(8) 0.014(7) 0.005(8) -0.012(8) C67 0.016(11) 0.041(8) 0.045(8) -0.008(7) 0.006(8) 0.008(7) C68 0.026(11) 0.031(7) 0.039(8) 0.009(6) -0.003(8) -0.014(7) C69 0.018(10) 0.026(7) 0.032(7) 0.014(6) -0.001(7) -0.009(6) C70 0.030(11) 0.029(7) 0.034(7) -0.004(6) 0.010(8) -0.012(7) C71 0.020(10) 0.036(7) 0.038(7) -0.003(6) 0.010(7) 0.000(7) C72 0.016(7) 0.028(6) 0.034(6) 0.009(5) 0.010(6) -0.005(5) C73 0.057(14) 0.042(8) 0.023(7) 0.005(6) -0.004(8) -0.003(8) C74 0.028(12) 0.041(8) 0.061(10) -0.003(7) 0.008(9) 0.006(7) C75 0.027(8) 0.032(6) 0.040(6) -0.002(5) 0.006(6) 0.006(6) C76 0.031(11) 0.023(7) 0.040(7) -0.004(6) -0.002(7) -0.003(6) C77 0.017(9) 0.014(6) 0.056(8) 0.008(6) 0.003(7) -0.008(6) C78 0.041(13) 0.067(11) 0.064(10) 0.002(9) -0.009(10) -0.002(9) C79 0.036(12) 0.029(7) 0.028(7) 0.009(6) 0.012(7) 0.012(7) C80 0.036(12) 0.018(6) 0.044(8) 0.005(6) -0.005(8) 0.003(7) C81 0.033(11) 0.028(7) 0.034(7) -0.010(6) 0.008(7) -0.005(7) C82 0.053(15) 0.027(8) 0.049(9) -0.011(7) 0.009(9) 0.005(8) C83 0.057(15) 0.024(7) 0.055(10) -0.014(7) -0.002(10) 0.006(8) C84 0.045(13) 0.026(7) 0.034(8) -0.003(6) 0.004(8) -0.006(7) C85 0.046(14) 0.027(7) 0.048(9) 0.000(7) 0.002(9) 0.000(8) C86 0.053(14) 0.027(8) 0.050(9) 0.011(7) 0.008(9) -0.001(8) C87 0.032(13) 0.040(8) 0.032(8) 0.005(6) 0.015(8) 0.006(7) C88 0.027(11) 0.029(7) 0.031(7) 0.001(6) 0.002(7) -0.002(7) O91 0.065(12) 0.055(7) 0.073(8) 0.007(6) 0.022(8) -0.003(7) C91 0.08(2) 0.069(12) 0.051(11) -0.008(9) -0.012(12) -0.015(12) C92 0.10(2) 0.067(12) 0.056(11) -0.010(9) 0.001(12) 0.020(12) C93 0.059(18) 0.070(12) 0.075(13) -0.017(10) 0.014(12) 0.001(11) C94 0.037(15) 0.074(12) 0.056(11) 0.012(9) 0.010(10) 0.023(10) C95 0.11(3) 0.064(13) 0.091(15) -0.001(11) 0.051(15) 0.010(14) C96 0.08(2) 0.17(2) 0.059(13) -0.014(13) -0.001(14) 0.028(17) _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 O2U1 1.842(10) . ? U1 O1U1 1.905(10) . ? U1 O1U3 2.374(8) . ? U1 N2 2.517(10) . ? U1 N3 2.536(10) . ? U1 N4 2.605(10) . ? U1 N1 2.631(10) . ? O1U1 U2 2.371(9) . ? N1 C1 1.293(15) . ? N1 C9 1.389(15) . ? N2 C10 1.306(18) . ? N2 C8 1.415(15) . ? N3 C19 1.347(17) . ? N3 C20 1.400(14) . ? N4 C27 1.314(16) . ? N4 C28 1.377(15) . ? C1 C2 1.398(17) . ? C2 C3 1.370(18) . ? C3 C4 1.38(2) . ? C4 C9 1.406(17) . ? C4 C5 1.414(18) . ? C5 C6 1.35(2) . ? C6 C7 1.419(17) . ? C7 C8 1.390(15) . ? C8 C9 1.431(18) . ? C10 C11 1.399(19) . ? C11 C19 1.399(17) . ? C11 C12 1.51(2) . ? C12 C13 1.405(18) . ? C12 C17 1.407(19) . ? C13 C14 1.44(2) . ? C14 C15 1.38(2) . ? C15 C16 1.355(19) . ? C15 C18 1.54(2) . ? C16 C17 1.36(2) . ? C20 C21 1.387(16) . ? C20 C28 1.431(17) . ? C21 C22 1.402(17) . ? C22 C23 1.331(19) . ? C23 C24 1.388(17) . ? C24 C28 1.409(15) . ? C24 C25 1.428(18) . ? C25 C26 1.352(18) . ? C26 C27 1.421(17) . ? U2 O2U2 1.844(9) . ? U2 O1U2 1.940(8) . ? U2 N33 2.518(10) . ? U2 N32 2.537(10) . ? U2 N34 2.597(10) . ? U2 N31 2.623(9) . ? O1U2 U3 2.356(9) . ? N31 C31 1.317(15) . ? N31 C39 1.380(17) . ? N32 C40 1.333(14) . ? N32 C38 1.441(15) . ? N33 C49 1.330(14) . ? N33 C50 1.401(14) . ? N34 C57 1.316(15) . ? N34 C58 1.385(16) . ? C31 C32 1.383(17) . ? C32 C33 1.37(2) . ? C33 C34 1.40(2) . ? C34 C35 1.40(2) . ? C34 C39 1.417(16) . ? C35 C36 1.38(2) . ? C36 C37 1.386(17) . ? C37 C38 1.382(19) . ? C38 C39 1.430(19) . ? C40 C41 1.391(16) . ? C41 C49 1.381(16) . ? C41 C42 1.503(16) . ? C42 C47 1.40(2) . ? C42 C43 1.430(18) . ? C43 C44 1.388(18) . ? C44 C45 1.41(2) . ? C45 C46 1.366(19) . ? C45 C48 1.540(18) . ? C46 C47 1.363(16) . ? C50 C51 1.386(18) . ? C50 C58 1.437(17) . ? C51 C52 1.398(17) . ? C52 C53 1.370(19) . ? C53 C54 1.407(18) . ? C54 C58 1.392(16) . ? C54 C55 1.408(18) . ? C55 C56 1.362(19) . ? C56 C57 1.411(16) . ? U3 O2U3 1.820(8) . ? U3 O1U3 1.906(8) . ? U3 N62 2.524(12) . ? U3 N63 2.545(11) . ? U3 N64 2.618(10) . ? U3 N61 2.627(10) . ? N61 C61 1.303(17) . ? N61 C69 1.367(17) . ? N62 C70 1.299(17) . ? N62 C68 1.433(15) . ? N63 C79 1.315(17) . ? N63 C80 1.438(15) . ? N64 C87 1.310(18) . ? N64 C88 1.375(17) . ? C61 C62 1.394(18) . ? C62 C63 1.37(2) . ? C63 C64 1.38(2) . ? C64 C69 1.399(17) . ? C64 C65 1.42(2) . ? C65 C66 1.34(2) . ? C66 C67 1.406(18) . ? C67 C68 1.39(2) . ? C68 C69 1.39(2) . ? C70 C71 1.417(18) . ? C71 C79 1.376(17) . ? C71 C72 1.521(18) . ? C72 C77 1.376(17) . ? C72 C73 1.39(2) . ? C73 C74 1.41(2) . ? C74 C75 1.366(18) . ? C75 C76 1.35(2) . ? C75 C78 1.504(19) . ? C76 C77 1.366(18) . ? C80 C81 1.35(2) . ? C80 C88 1.42(2) . ? C81 C82 1.402(17) . ? C82 C83 1.37(2) . ? C83 C84 1.42(2) . ? C84 C85 1.39(2) . ? C84 C88 1.439(17) . ? C85 C86 1.35(2) . ? C86 C87 1.440(18) . ? O91 C94 1.412(19) . ? O91 C91 1.44(2) . ? C91 C93 1.52(2) . ? C91 C92 1.54(2) . ? C94 C96 1.52(2) . ? C94 C95 1.54(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2U1 U1 O1U1 176.7(4) . . ? O2U1 U1 O1U3 99.0(3) . . ? O1U1 U1 O1U3 84.2(3) . . ? O2U1 U1 N2 91.0(4) . . ? O1U1 U1 N2 85.9(4) . . ? O1U3 U1 N2 142.0(3) . . ? O2U1 U1 N3 93.9(4) . . ? O1U1 U1 N3 84.2(4) . . ? O1U3 U1 N3 141.0(3) . . ? N2 U1 N3 73.7(3) . . ? O2U1 U1 N4 83.1(4) . . ? O1U1 U1 N4 98.4(3) . . ? O1U3 U1 N4 81.4(3) . . ? N2 U1 N4 136.4(3) . . ? N3 U1 N4 63.8(3) . . ? O2U1 U1 N1 84.8(4) . . ? O1U1 U1 N1 94.8(3) . . ? O1U3 U1 N1 79.9(3) . . ? N2 U1 N1 64.5(3) . . ? N3 U1 N1 138.2(3) . . ? N4 U1 N1 155.8(4) . . ? U1 O1U1 U2 157.1(5) . . ? C1 N1 C9 118.6(11) . . ? C1 N1 U1 124.3(8) . . ? C9 N1 U1 116.3(8) . . ? C10 N2 C8 115.4(11) . . ? C10 N2 U1 122.8(9) . . ? C8 N2 U1 119.1(8) . . ? C19 N3 C20 116.2(11) . . ? C19 N3 U1 119.7(8) . . ? C20 N3 U1 120.5(8) . . ? C27 N4 C28 117.9(11) . . ? C27 N4 U1 122.1(8) . . ? C28 N4 U1 118.6(8) . . ? N1 C1 C2 123.2(12) . . ? C3 C2 C1 119.1(13) . . ? C2 C3 C4 119.7(13) . . ? C3 C4 C9 118.0(12) . . ? C3 C4 C5 123.1(13) . . ? C9 C4 C5 118.9(13) . . ? C6 C5 C4 120.7(13) . . ? C5 C6 C7 121.5(12) . . ? C8 C7 C6 119.7(12) . . ? C7 C8 N2 123.6(12) . . ? C7 C8 C9 118.8(11) . . ? N2 C8 C9 117.6(10) . . ? N1 C9 C4 121.2(12) . . ? N1 C9 C8 118.5(11) . . ? C4 C9 C8 120.3(11) . . ? N2 C10 C11 128.8(13) . . ? C19 C11 C10 125.8(14) . . ? C19 C11 C12 117.3(12) . . ? C10 C11 C12 116.9(12) . . ? C13 C12 C17 117.8(15) . . ? C13 C12 C11 121.2(15) . . ? C17 C12 C11 120.8(12) . . ? C12 C13 C14 118.4(16) . . ? C15 C14 C13 120.4(14) . . ? C16 C15 C14 120.1(17) . . ? C16 C15 C18 119.8(16) . . ? C14 C15 C18 119.8(15) . . ? C15 C16 C17 121.1(16) . . ? C16 C17 C12 122.1(13) . . ? N3 C19 C11 128.2(12) . . ? C21 C20 N3 124.5(12) . . ? C21 C20 C28 118.0(11) . . ? N3 C20 C28 117.4(10) . . ? C20 C21 C22 120.5(12) . . ? C23 C22 C21 122.1(12) . . ? C22 C23 C24 119.6(11) . . ? C23 C24 C28 121.0(12) . . ? C23 C24 C25 123.7(12) . . ? C28 C24 C25 115.2(11) . . ? C26 C25 C24 121.9(12) . . ? C25 C26 C27 117.8(12) . . ? N4 C27 C26 123.6(12) . . ? N4 C28 C24 123.5(11) . . ? N4 C28 C20 117.7(10) . . ? C24 C28 C20 118.8(10) . . ? O2U2 U2 O1U2 176.4(3) . . ? O2U2 U2 O1U1 100.0(4) . . ? O1U2 U2 O1U1 82.8(3) . . ? O2U2 U2 N33 93.5(4) . . ? O1U2 U2 N33 83.0(3) . . ? O1U1 U2 N33 141.6(3) . . ? O2U2 U2 N32 92.2(4) . . ? O1U2 U2 N32 86.9(3) . . ? O1U1 U2 N32 141.8(3) . . ? N33 U2 N32 72.4(3) . . ? O2U2 U2 N34 82.1(3) . . ? O1U2 U2 N34 96.1(3) . . ? O1U1 U2 N34 82.1(3) . . ? N33 U2 N34 64.2(3) . . ? N32 U2 N34 135.6(3) . . ? O2U2 U2 N31 83.3(3) . . ? O1U2 U2 N31 99.4(3) . . ? O1U1 U2 N31 81.2(3) . . ? N33 U2 N31 136.4(3) . . ? N32 U2 N31 64.4(3) . . ? N34 U2 N31 155.6(3) . . ? U2 O1U2 U3 156.4(4) . . ? C31 N31 C39 118.7(11) . . ? C31 N31 U2 122.8(9) . . ? C39 N31 U2 117.1(8) . . ? C40 N32 C38 115.6(10) . . ? C40 N32 U2 123.5(8) . . ? C38 N32 U2 118.6(8) . . ? C49 N33 C50 116.6(10) . . ? C49 N33 U2 121.2(8) . . ? C50 N33 U2 119.2(7) . . ? C57 N34 C58 116.3(11) . . ? C57 N34 U2 124.1(8) . . ? C58 N34 U2 118.7(8) . . ? N31 C31 C32 122.5(13) . . ? C33 C32 C31 120.7(14) . . ? C32 C33 C34 118.8(14) . . ? C35 C34 C33 123.3(13) . . ? C35 C34 C39 119.0(14) . . ? C33 C34 C39 117.7(14) . . ? C36 C35 C34 120.1(13) . . ? C35 C36 C37 121.8(15) . . ? C38 C37 C36 120.0(14) . . ? C37 C38 C39 119.6(12) . . ? C37 C38 N32 123.6(13) . . ? C39 C38 N32 116.7(13) . . ? N31 C39 C34 121.5(13) . . ? N31 C39 C38 119.0(11) . . ? C34 C39 C38 119.5(13) . . ? N32 C40 C41 125.5(11) . . ? C49 C41 C40 127.4(12) . . ? C49 C41 C42 116.6(11) . . ? C40 C41 C42 115.8(11) . . ? C47 C42 C43 116.9(12) . . ? C47 C42 C41 121.1(12) . . ? C43 C42 C41 122.0(14) . . ? C44 C43 C42 120.4(15) . . ? C43 C44 C45 120.0(13) . . ? C46 C45 C44 119.5(13) . . ? C46 C45 C48 119.5(16) . . ? C44 C45 C48 120.8(13) . . ? C47 C46 C45 121.2(15) . . ? C46 C47 C42 122.0(13) . . ? N33 C49 C41 127.9(12) . . ? C51 C50 N33 124.5(11) . . ? C51 C50 C58 116.5(11) . . ? N33 C50 C58 119.0(11) . . ? C50 C51 C52 122.1(12) . . ? C53 C52 C51 120.6(13) . . ? C52 C53 C54 119.8(12) . . ? C58 C54 C55 117.5(13) . . ? C58 C54 C53 119.5(13) . . ? C55 C54 C53 123.0(11) . . ? C56 C55 C54 121.0(12) . . ? C55 C56 C57 116.6(13) . . ? N34 C57 C56 125.7(13) . . ? N34 C58 C54 122.8(12) . . ? N34 C58 C50 115.8(11) . . ? C54 C58 C50 121.4(12) . . ? O2U3 U3 O1U3 176.7(4) . . ? O2U3 U3 O1U2 98.7(4) . . ? O1U3 U3 O1U2 84.5(3) . . ? O2U3 U3 N62 92.0(4) . . ? O1U3 U3 N62 84.9(3) . . ? O1U2 U3 N62 140.0(3) . . ? O2U3 U3 N63 92.6(4) . . ? O1U3 U3 N63 85.3(3) . . ? O1U2 U3 N63 145.1(3) . . ? N62 U3 N63 71.7(3) . . ? O2U3 U3 N64 83.9(3) . . ? O1U3 U3 N64 97.4(3) . . ? O1U2 U3 N64 84.4(3) . . ? N62 U3 N64 135.2(4) . . ? N63 U3 N64 64.0(4) . . ? O2U3 U3 N61 82.8(3) . . ? O1U3 U3 N61 97.0(3) . . ? O1U2 U3 N61 78.2(3) . . ? N62 U3 N61 65.1(4) . . ? N63 U3 N61 136.3(4) . . ? N64 U3 N61 156.2(4) . . ? U3 O1U3 U1 154.9(5) . . ? C61 N61 C69 119.2(12) . . ? C61 N61 U3 123.8(10) . . ? C69 N61 U3 116.4(9) . . ? C70 N62 C68 117.8(11) . . ? C70 N62 U3 121.7(8) . . ? C68 N62 U3 116.1(9) . . ? C79 N63 C80 116.3(11) . . ? C79 N63 U3 122.8(8) . . ? C80 N63 U3 118.9(9) . . ? C87 N64 C88 120.1(11) . . ? C87 N64 U3 121.4(9) . . ? C88 N64 U3 117.3(9) . . ? N61 C61 C62 123.7(15) . . ? C63 C62 C61 117.8(16) . . ? C62 C63 C64 120.0(14) . . ? C63 C64 C69 119.0(14) . . ? C63 C64 C65 122.7(13) . . ? C69 C64 C65 118.3(15) . . ? C66 C65 C64 120.2(14) . . ? C65 C66 C67 121.4(15) . . ? C68 C67 C66 120.0(15) . . ? C67 C68 C69 118.7(12) . . ? C67 C68 N62 120.6(14) . . ? C69 C68 N62 120.6(12) . . ? N61 C69 C68 118.4(11) . . ? N61 C69 C64 120.2(14) . . ? C68 C69 C64 121.3(13) . . ? N62 C70 C71 126.5(12) . . ? C79 C71 C70 126.6(13) . . ? C79 C71 C72 117.8(12) . . ? C70 C71 C72 115.1(11) . . ? C77 C72 C73 114.7(13) . . ? C77 C72 C71 122.8(14) . . ? C73 C72 C71 122.3(12) . . ? C72 C73 C74 121.2(13) . . ? C75 C74 C73 120.2(16) . . ? C76 C75 C74 119.8(14) . . ? C76 C75 C78 119.1(13) . . ? C74 C75 C78 121.0(15) . . ? C75 C76 C77 119.0(13) . . ? C76 C77 C72 125.1(15) . . ? N63 C79 C71 127.4(13) . . ? C81 C80 C88 120.0(12) . . ? C81 C80 N63 124.2(15) . . ? C88 C80 N63 115.7(13) . . ? C80 C81 C82 120.6(15) . . ? C83 C82 C81 121.4(15) . . ? C82 C83 C84 120.6(13) . . ? C85 C84 C83 125.6(13) . . ? C85 C84 C88 117.3(14) . . ? C83 C84 C88 117.0(15) . . ? C86 C85 C84 122.8(14) . . ? C85 C86 C87 116.6(16) . . ? N64 C87 C86 123.1(14) . . ? N64 C88 C80 119.8(11) . . ? N64 C88 C84 119.9(14) . . ? C80 C88 C84 120.2(13) . . ? C94 O91 C91 114.2(13) . . ? O91 C91 C93 104.9(15) . . ? O91 C91 C92 109.1(17) . . ? C93 C91 C92 113.7(15) . . ? O91 C94 C96 111.1(15) . . ? O91 C94 C95 106.9(15) . . ? C96 C94 C95 112.7(17) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 3.454 _refine_diff_density_min -1.579 _refine_diff_density_rms 0.231 data_2 _database_code_depnum_ccdc_archive 'CCDC 848287' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H23 Cl3 N4 O2 U' _chemical_formula_weight 803.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2599(4) _cell_length_b 12.1368(9) _cell_length_c 16.1046(8) _cell_angle_alpha 99.775(5) _cell_angle_beta 90.893(4) _cell_angle_gamma 95.133(5) _cell_volume 1392.11(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3572 _cell_measurement_theta_min 3.3152 _cell_measurement_theta_max 32.4185 _exptl_crystal_description needle _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 0 0.0148 0.0002 1.0003 0.0011 -0.0015 0.0014 0.0596 0 -1 0 0.0148 -0.0002 -1.0003 -0.0011 0.0015 -0.0014 -0.0596 0 0 -1 0.0232 0.0000 0.0004 -1.0010 -0.0154 0.0410 -0.0090 1 0 0 0.0968 1.0004 -0.0003 -0.0011 0.0917 0.0336 0.0106 -1 0 0 0.0968 -1.0004 0.0003 0.0011 -0.0917 -0.0336 -0.0106 0 0 1 0.0232 -0.0000 -0.0004 1.0010 0.0154 -0.0410 0.0090 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 6.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3755 _exptl_absorpt_correction_T_max 0.8369 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12801 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6907 _reflns_number_gt 5629 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 34.00 96.00 1.0000 140.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 2 omega 3.00 39.00 1.0000 140.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 77.0000 90.0000 36 #__ type_ start__ end____ width___ exp.time_ 3 omega -76.00 15.00 1.0000 140.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 111.0000 157.0000 91 #__ type_ start__ end____ width___ exp.time_ 4 omega -70.00 -12.00 1.0000 140.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 111.0000 -63.0000 58 #__ type_ start__ end____ width___ exp.time_ 5 omega -53.00 44.00 1.0000 140.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 37.0000 150.0000 97 #__ type_ start__ end____ width___ exp.time_ 6 omega -93.00 -1.00 1.0000 140.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -37.0000 -30.0000 92 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6907 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C61 C 0.118(4) 0.454(2) 0.838(2) 0.152(16) Uani 1 1 d . . . H61A H 0.0559 0.4816 0.7919 0.182 Uiso 1 1 calc R . . H61B H 0.0413 0.3872 0.8508 0.182 Uiso 1 1 calc R . . Cl61 Cl 0.3401(12) 0.4153(7) 0.8072(4) 0.114(2) Uani 1 1 d . . . U1 U 0.67091(5) 0.99686(3) 0.74618(2) 0.02206(15) Uani 1 1 d . . . O1U O 0.9091(12) 0.9712(7) 0.7485(5) 0.0284(17) Uani 1 1 d . . . O2U O 0.4352(12) 1.0194(8) 0.7459(5) 0.040(2) Uani 1 1 d . . . Cl1 Cl 0.7677(7) 1.2194(3) 0.7777(2) 0.0589(11) Uani 1 1 d . . . N1 N 0.7078(13) 1.0279(9) 0.9105(6) 0.030(2) Uani 1 1 d . . . N2 N 0.5743(14) 0.8329(8) 0.8125(6) 0.029(2) Uani 1 1 d . . . N3 N 0.6018(13) 0.8325(7) 0.6317(6) 0.0255(18) Uani 1 1 d . . . N4 N 0.7183(13) 1.0368(8) 0.5927(6) 0.0278(19) Uani 1 1 d . . . C1 C 0.7661(17) 1.1237(12) 0.9587(8) 0.041(3) Uani 1 1 d . . . H1 H 0.7710 1.1899 0.9344 0.049 Uiso 1 1 calc R . . C2 C 0.8215(18) 1.1344(14) 1.0436(7) 0.045(3) Uani 1 1 d . . . H2 H 0.8652 1.2056 1.0752 0.053 Uiso 1 1 calc R . . C3 C 0.8114(17) 1.0401(15) 1.0803(9) 0.050(4) Uani 1 1 d . . . H3 H 0.8453 1.0453 1.1382 0.060 Uiso 1 1 calc R . . C4 C 0.7497(17) 0.9343(13) 1.0306(8) 0.041(3) Uani 1 1 d . . . C5 C 0.739(2) 0.8342(14) 1.0640(9) 0.053(4) Uani 1 1 d . . . H5 H 0.7676 0.8359 1.1219 0.063 Uiso 1 1 calc R . . C6 C 0.686(2) 0.7341(13) 1.0123(9) 0.055(4) Uani 1 1 d . . . H6 H 0.6859 0.6659 1.0339 0.066 Uiso 1 1 calc R . . C7 C 0.633(2) 0.7313(13) 0.9276(9) 0.046(3) Uani 1 1 d . . . H7 H 0.5926 0.6618 0.8927 0.055 Uiso 1 1 calc R . . C8 C 0.6386(18) 0.8299(11) 0.8955(8) 0.036(3) Uani 1 1 d . . . C9 C 0.7020(17) 0.9320(10) 0.9468(7) 0.032(2) Uani 1 1 d . . . C10 C 0.4304(16) 0.7599(9) 0.7843(8) 0.029(2) Uani 1 1 d . . . H10 H 0.3664 0.7244 0.8250 0.035 Uiso 1 1 calc R . . C11 C 0.3632(15) 0.7298(9) 0.7005(7) 0.029(2) Uani 1 1 d . . . C12 C 0.4610(16) 0.7577(8) 0.6320(7) 0.027(2) Uani 1 1 d . . . H12 H 0.4195 0.7169 0.5784 0.032 Uiso 1 1 calc R . . C13 C 0.6806(14) 0.8368(9) 0.5523(7) 0.026(2) Uani 1 1 d . . . C14 C 0.6995(16) 0.7422(9) 0.4928(7) 0.029(2) Uani 1 1 d . . . H14 H 0.6763 0.6699 0.5077 0.035 Uiso 1 1 calc R . . C15 C 0.7524(16) 0.7517(11) 0.4105(8) 0.036(3) Uani 1 1 d . . . H15 H 0.7621 0.6855 0.3704 0.044 Uiso 1 1 calc R . . C16 C 0.7904(16) 0.8544(10) 0.3871(7) 0.030(2) Uani 1 1 d . . . H16 H 0.8242 0.8599 0.3310 0.036 Uiso 1 1 calc R . . C17 C 0.7783(14) 0.9526(9) 0.4479(7) 0.027(2) Uani 1 1 d . . . C18 C 0.8225(16) 1.0607(10) 0.4305(8) 0.032(2) Uani 1 1 d . . . H18 H 0.8573 1.0702 0.3753 0.039 Uiso 1 1 calc R . . C19 C 0.8161(16) 1.1523(11) 0.4917(8) 0.033(2) Uani 1 1 d . . . H19 H 0.8474 1.2257 0.4800 0.040 Uiso 1 1 calc R . . C20 C 0.7626(16) 1.1365(9) 0.5722(8) 0.032(2) Uani 1 1 d . . . H20 H 0.7578 1.2010 0.6144 0.038 Uiso 1 1 calc R . . C21 C 0.7282(14) 0.9445(9) 0.5310(7) 0.027(2) Uani 1 1 d . . . C22 C 0.1827(15) 0.6576(10) 0.6830(7) 0.029(2) Uani 1 1 d . . . C23 C 0.0242(16) 0.6886(10) 0.7251(8) 0.035(3) Uani 1 1 d . . . H23 H 0.0314 0.7554 0.7660 0.042 Uiso 1 1 calc R . . C24 C -0.1425(18) 0.6246(11) 0.7087(9) 0.039(3) Uani 1 1 d . . . H24 H -0.2483 0.6484 0.7381 0.047 Uiso 1 1 calc R . . C25 C -0.1595(18) 0.5279(11) 0.6513(9) 0.040(3) Uani 1 1 d . . . C26 C -0.0075(18) 0.4972(11) 0.6046(10) 0.044(3) Uani 1 1 d . . . H26 H -0.0187 0.4333 0.5611 0.053 Uiso 1 1 calc R . . C27 C 0.1631(17) 0.5617(10) 0.6226(9) 0.037(3) Uani 1 1 d . . . H27 H 0.2683 0.5386 0.5924 0.045 Uiso 1 1 calc R . . C28 C -0.3442(19) 0.4554(13) 0.6328(12) 0.056(4) Uani 1 1 d . . . H28A H -0.3390 0.3862 0.6561 0.083 Uiso 1 1 calc R . . H28B H -0.3676 0.4366 0.5717 0.083 Uiso 1 1 calc R . . H28C H -0.4442 0.4971 0.6588 0.083 Uiso 1 1 calc R . . Cl62 Cl 0.1394(18) 0.5542(7) 0.9245(7) 0.170(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C61 0.11(2) 0.076(15) 0.28(4) 0.10(2) -0.09(3) -0.022(15) Cl61 0.140(6) 0.149(6) 0.059(3) 0.036(4) 0.012(4) 0.022(5) U1 0.0184(2) 0.0271(2) 0.0200(2) 0.00239(13) -0.00207(13) 0.00221(13) O1U 0.038(4) 0.038(4) 0.016(4) 0.015(3) 0.010(3) 0.013(3) O2U 0.027(4) 0.060(6) 0.031(5) 0.004(4) -0.005(3) 0.011(4) Cl1 0.096(3) 0.0364(16) 0.0387(19) 0.0009(14) -0.0004(19) -0.0130(18) N1 0.020(4) 0.048(6) 0.019(4) 0.003(4) 0.001(4) -0.002(4) N2 0.034(5) 0.029(5) 0.020(4) -0.003(3) -0.001(4) 0.006(4) N3 0.026(5) 0.029(4) 0.024(4) 0.008(3) -0.001(4) 0.003(4) N4 0.023(5) 0.034(5) 0.028(5) 0.009(4) -0.001(4) 0.005(4) C1 0.026(6) 0.057(8) 0.034(7) -0.005(6) 0.005(5) 0.001(5) C2 0.036(7) 0.078(10) 0.013(5) -0.010(6) 0.002(5) 0.000(6) C3 0.019(6) 0.103(12) 0.026(6) 0.007(7) 0.005(5) 0.007(7) C4 0.022(6) 0.070(9) 0.032(7) 0.008(6) 0.008(5) 0.007(6) C5 0.053(9) 0.082(11) 0.025(7) 0.011(7) 0.000(6) 0.012(8) C6 0.076(11) 0.064(9) 0.037(8) 0.027(7) -0.005(7) 0.031(8) C7 0.048(8) 0.059(8) 0.033(7) 0.010(6) -0.004(6) 0.014(7) C8 0.034(6) 0.050(7) 0.029(6) 0.010(5) 0.006(5) 0.019(5) C9 0.030(6) 0.042(6) 0.023(6) 0.000(5) 0.004(5) 0.006(5) C10 0.029(6) 0.027(5) 0.034(6) 0.009(4) 0.005(5) 0.005(4) C11 0.021(5) 0.031(5) 0.033(6) 0.003(4) -0.001(4) 0.004(4) C12 0.032(6) 0.020(5) 0.029(6) 0.003(4) -0.004(4) 0.005(4) C13 0.015(5) 0.031(5) 0.029(6) 0.000(4) -0.008(4) 0.002(4) C14 0.029(6) 0.031(5) 0.026(6) 0.000(4) -0.004(4) 0.004(4) C15 0.027(6) 0.040(6) 0.037(7) -0.010(5) 0.002(5) 0.001(5) C16 0.026(5) 0.042(6) 0.021(5) 0.002(4) -0.005(4) 0.004(5) C17 0.017(5) 0.032(5) 0.033(6) 0.005(4) -0.011(4) 0.005(4) C18 0.025(5) 0.041(6) 0.035(6) 0.014(5) -0.004(5) 0.009(5) C19 0.025(6) 0.044(6) 0.032(6) 0.013(5) -0.004(5) 0.006(5) C20 0.024(5) 0.027(5) 0.043(7) 0.004(5) -0.010(5) -0.001(4) C21 0.016(5) 0.039(6) 0.029(6) 0.012(5) -0.009(4) 0.008(4) C22 0.022(5) 0.041(6) 0.023(5) -0.001(4) 0.000(4) 0.007(4) C23 0.026(6) 0.037(6) 0.043(7) 0.006(5) 0.000(5) 0.007(5) C24 0.028(6) 0.039(6) 0.051(8) 0.007(6) -0.001(6) 0.006(5) C25 0.032(6) 0.036(6) 0.055(8) 0.008(6) -0.002(6) 0.012(5) C26 0.033(7) 0.031(6) 0.066(10) 0.002(6) -0.010(6) 0.001(5) C27 0.024(6) 0.031(6) 0.054(8) 0.000(5) 0.001(5) 0.004(5) C28 0.026(7) 0.050(8) 0.086(12) 0.002(8) 0.004(7) -0.003(6) Cl62 0.242(12) 0.120(6) 0.168(9) 0.057(6) 0.107(9) 0.049(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C61 Cl62 1.68(4) . ? C61 Cl61 1.77(3) . ? U1 O2U 1.757(9) . ? U1 O1U 1.785(8) . ? U1 N2 2.467(10) . ? U1 N3 2.485(9) . ? U1 N1 2.614(9) . ? U1 N4 2.620(10) . ? U1 Cl1 2.689(3) . ? N1 C1 1.315(16) . ? N1 C9 1.387(16) . ? N2 C10 1.328(14) . ? N2 C8 1.417(15) . ? N3 C12 1.305(14) . ? N3 C13 1.416(14) . ? N4 C20 1.321(15) . ? N4 C21 1.373(14) . ? C1 C2 1.401(18) . ? C2 C3 1.37(2) . ? C3 C4 1.42(2) . ? C4 C9 1.383(18) . ? C4 C5 1.41(2) . ? C5 C6 1.37(2) . ? C6 C7 1.406(19) . ? C7 C8 1.379(19) . ? C8 C9 1.403(17) . ? C10 C11 1.404(16) . ? C11 C12 1.395(16) . ? C11 C22 1.505(15) . ? C13 C14 1.383(14) . ? C13 C21 1.422(16) . ? C14 C15 1.405(17) . ? C15 C16 1.370(18) . ? C16 C17 1.419(15) . ? C17 C18 1.399(16) . ? C17 C21 1.409(16) . ? C18 C19 1.360(17) . ? C19 C20 1.398(18) . ? C22 C27 1.379(16) . ? C22 C23 1.393(16) . ? C23 C24 1.375(17) . ? C24 C25 1.359(18) . ? C25 C26 1.388(19) . ? C25 C28 1.533(19) . ? C26 C27 1.403(17) . ? 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 Cl62 C61 Cl61 109.7(16) . . ? O2U U1 O1U 178.4(4) . . ? O2U U1 N2 85.5(4) . . ? O1U U1 N2 92.9(3) . . ? O2U U1 N3 89.2(4) . . ? O1U U1 N3 90.7(3) . . ? N2 U1 N3 72.3(3) . . ? O2U U1 N1 94.6(4) . . ? O1U U1 N1 84.3(3) . . ? N2 U1 N1 64.2(3) . . ? N3 U1 N1 135.8(3) . . ? O2U U1 N4 94.1(4) . . ? O1U U1 N4 87.3(3) . . ? N2 U1 N4 136.8(3) . . ? N3 U1 N4 64.5(3) . . ? N1 U1 N4 158.0(3) . . ? O2U U1 Cl1 90.9(3) . . ? O1U U1 Cl1 90.1(3) . . ? N2 U1 Cl1 143.8(2) . . ? N3 U1 Cl1 143.7(2) . . ? N1 U1 Cl1 80.3(2) . . ? N4 U1 Cl1 79.4(2) . . ? C1 N1 C9 117.2(11) . . ? C1 N1 U1 125.0(9) . . ? C9 N1 U1 116.4(7) . . ? C10 N2 C8 115.3(11) . . ? C10 N2 U1 123.1(8) . . ? C8 N2 U1 119.4(8) . . ? C12 N3 C13 115.8(9) . . ? C12 N3 U1 123.3(7) . . ? C13 N3 U1 118.2(6) . . ? C20 N4 C21 117.3(10) . . ? C20 N4 U1 125.6(8) . . ? C21 N4 U1 116.2(7) . . ? N1 C1 C2 124.3(15) . . ? C3 C2 C1 118.7(13) . . ? C2 C3 C4 119.2(13) . . ? C9 C4 C5 120.1(13) . . ? C9 C4 C3 117.8(14) . . ? C5 C4 C3 122.1(13) . . ? C6 C5 C4 119.6(13) . . ? C5 C6 C7 120.6(14) . . ? C8 C7 C6 119.7(14) . . ? C7 C8 C9 119.9(12) . . ? C7 C8 N2 122.1(12) . . ? C9 C8 N2 118.0(11) . . ? C4 C9 N1 122.8(11) . . ? C4 C9 C8 120.0(13) . . ? N1 C9 C8 117.2(11) . . ? N2 C10 C11 126.8(11) . . ? C12 C11 C10 123.2(11) . . ? C12 C11 C22 118.1(10) . . ? C10 C11 C22 118.6(11) . . ? N3 C12 C11 128.7(10) . . ? C14 C13 N3 123.2(10) . . ? C14 C13 C21 119.0(11) . . ? N3 C13 C21 117.6(9) . . ? C13 C14 C15 120.9(11) . . ? C16 C15 C14 121.3(10) . . ? C15 C16 C17 118.8(11) . . ? C18 C17 C21 116.7(10) . . ? C18 C17 C16 122.6(11) . . ? C21 C17 C16 120.6(11) . . ? C19 C18 C17 120.6(12) . . ? C18 C19 C20 118.7(11) . . ? N4 C20 C19 123.7(11) . . ? N4 C21 C17 122.9(10) . . ? N4 C21 C13 117.8(10) . . ? C17 C21 C13 119.2(10) . . ? C27 C22 C23 116.9(11) . . ? C27 C22 C11 122.4(10) . . ? C23 C22 C11 120.7(10) . . ? C24 C23 C22 121.3(12) . . ? C25 C24 C23 121.6(12) . . ? C24 C25 C26 119.0(13) . . ? C24 C25 C28 122.0(12) . . ? C26 C25 C28 118.9(12) . . ? C25 C26 C27 119.2(12) . . ? C22 C27 C26 122.0(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 13.239 _refine_diff_density_min -2.787 _refine_diff_density_rms 0.392 data_3 _database_code_depnum_ccdc_archive 'CCDC 848288' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57.50 H44.25 N8.75 O5 U2' _chemical_formula_weight 1413.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.1234(13) _cell_length_b 27.3660(13) _cell_length_c 28.2322(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.531(4) _cell_angle_gamma 90.00 _cell_volume 20954.7(19) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5782 _cell_measurement_theta_min 3.3157 _cell_measurement_theta_max 32.2618 _exptl_crystal_description Plate _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10792 _exptl_absorpt_coefficient_mu 6.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2743 _exptl_absorpt_correction_T_max 0.8908 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42381 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 24.71 _reflns_number_total 17778 _reflns_number_gt 11780 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 60.00 101.00 1.0000 160.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 -120.0000 41 #__ type_ start__ end____ width___ exp.time_ 2 omega -48.00 93.00 1.0000 160.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 0.0000 30.0000 141 #__ type_ start__ end____ width___ exp.time_ 3 omega 61.00 101.00 1.0000 160.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 -30.0000 40 #__ type_ start__ end____ width___ exp.time_ 4 omega 1.00 44.00 1.0000 160.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 0.0000 120.0000 43 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+853.3683P] 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 17778 _refine_ls_number_parameters 1321 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.19235(2) 0.39425(2) 0.56693(2) 0.03064(16) Uani 1 1 d . . . O1U1 O 0.2543(4) 0.3879(4) 0.5460(4) 0.035(3) Uani 1 1 d . . . O2U1 O 0.1320(4) 0.3992(4) 0.5916(4) 0.040(3) Uani 1 1 d . . . U2 U 0.14385(2) 0.45029(2) 0.42875(2) 0.03339(17) Uani 1 1 d . . . O1U2 O 0.1506(4) 0.3917(4) 0.4004(4) 0.041(3) Uani 1 1 d . . . O2U2 O 0.1352(4) 0.5125(4) 0.4500(4) 0.038(3) Uani 1 1 d . . . O1 O 0.1664(5) 0.4214(5) 0.4983(4) 0.060(4) Uani 1 1 d U . . N1 N 0.1790(5) 0.3072(5) 0.5279(5) 0.035(3) Uani 1 1 d . . . N2 N 0.1996(5) 0.3203(5) 0.6217(5) 0.033(3) Uani 1 1 d . . . N3 N 0.2250(5) 0.4184(5) 0.6451(5) 0.038(3) Uani 1 1 d . . . N4 N 0.2178(5) 0.4888(6) 0.5784(5) 0.040(4) Uani 1 1 d . . . C1 C 0.1659(6) 0.3007(6) 0.4829(6) 0.034(4) Uani 1 1 d . . . H1 H 0.1541 0.3281 0.4655 0.040 Uiso 1 1 calc R . . C2 C 0.1684(6) 0.2550(6) 0.4594(6) 0.037(4) Uani 1 1 d . . . H2 H 0.1564 0.2512 0.4279 0.045 Uiso 1 1 calc R . . C3 C 0.1882(6) 0.2171(6) 0.4831(6) 0.038(4) Uani 1 1 d . . . H3 H 0.1921 0.1867 0.4675 0.045 Uiso 1 1 calc R . . C4 C 0.2036(6) 0.2217(6) 0.5312(7) 0.042(5) Uani 1 1 d . . . C5 C 0.2240(6) 0.1838(6) 0.5568(7) 0.042(4) Uani 1 1 d . . . H5 H 0.2289 0.1529 0.5422 0.050 Uiso 1 1 calc R . . C6 C 0.2376(6) 0.1903(6) 0.6039(7) 0.042(4) Uani 1 1 d . . . H6 H 0.2516 0.1640 0.6213 0.050 Uiso 1 1 calc R . . C7 C 0.2306(6) 0.2363(6) 0.6264(7) 0.042(4) Uani 1 1 d . . . H7 H 0.2400 0.2407 0.6586 0.050 Uiso 1 1 calc R . . C8 C 0.2101(6) 0.2745(6) 0.6011(6) 0.037(4) Uani 1 1 d . . . C9 C 0.1985(5) 0.2675(5) 0.5529(6) 0.028(4) Uani 1 1 d . . . C10 C 0.1845(6) 0.3211(6) 0.6666(6) 0.037(4) Uani 1 1 d . . . H10 H 0.1753 0.2907 0.6801 0.045 Uiso 1 1 calc R . . C11 C 0.1809(6) 0.3624(6) 0.6960(6) 0.036(4) Uani 1 1 d . . . C12 C 0.2064(6) 0.4063(6) 0.6859(6) 0.037(4) Uani 1 1 d . . . H12 H 0.2103 0.4289 0.7112 0.045 Uiso 1 1 calc R . . C13 C 0.2586(6) 0.4607(6) 0.6485(6) 0.039(4) Uani 1 1 d . . . C14 C 0.2936(7) 0.4651(6) 0.6837(6) 0.045(5) Uani 1 1 d . . . H14 H 0.2972 0.4409 0.7077 0.054 Uiso 1 1 calc R . . C15 C 0.3245(7) 0.5078(6) 0.6829(7) 0.050(5) Uani 1 1 d . . . H15 H 0.3488 0.5118 0.7070 0.060 Uiso 1 1 calc R . . C16 C 0.3202(7) 0.5427(6) 0.6489(7) 0.051(5) Uani 1 1 d . . . H16 H 0.3417 0.5701 0.6485 0.061 Uiso 1 1 calc R . . C17 C 0.2831(8) 0.5373(6) 0.6141(7) 0.051(5) Uani 1 1 d . . . C18 C 0.2728(7) 0.5738(6) 0.5783(8) 0.057(6) Uani 1 1 d . . . H18 H 0.2927 0.6024 0.5766 0.068 Uiso 1 1 calc R . . C19 C 0.2354(7) 0.5676(7) 0.5476(7) 0.052(5) Uani 1 1 d . . . H19 H 0.2258 0.5927 0.5262 0.062 Uiso 1 1 calc R . . C20 C 0.2103(5) 0.5216(5) 0.5486(6) 0.031(4) Uani 1 1 d U . . H20 H 0.1862 0.5156 0.5247 0.037 Uiso 1 1 calc R . . C21 C 0.2528(6) 0.4955(6) 0.6127(6) 0.038(4) Uani 1 1 d . . . C22 C 0.1568(6) 0.3598(6) 0.7434(6) 0.039(4) Uani 1 1 d . . . C23 C 0.1222(6) 0.3962(6) 0.7567(7) 0.043(4) Uani 1 1 d . . . H23 H 0.1103 0.4183 0.7333 0.052 Uiso 1 1 calc R . . C24 C 0.1056(7) 0.4003(6) 0.8015(7) 0.049(5) Uani 1 1 d . . . H24 H 0.0830 0.4256 0.8088 0.058 Uiso 1 1 calc R . . C25 C 0.1208(7) 0.3685(7) 0.8370(7) 0.048(5) Uani 1 1 d . . . C26 C 0.1529(7) 0.3305(6) 0.8241(7) 0.048(5) Uani 1 1 d . . . H26 H 0.1628 0.3070 0.8471 0.058 Uiso 1 1 calc R . . C27 C 0.1702(6) 0.3270(6) 0.7779(6) 0.040(4) Uani 1 1 d . . . H27 H 0.1919 0.3011 0.7701 0.048 Uiso 1 1 calc R . . C28 C 0.1038(8) 0.3744(7) 0.8881(7) 0.063(6) Uani 1 1 d . . . H28A H 0.1250 0.3981 0.9044 0.094 Uiso 1 1 calc R . . H28B H 0.1059 0.3428 0.9043 0.094 Uiso 1 1 calc R . . H28C H 0.0696 0.3860 0.8883 0.094 Uiso 1 1 calc R . . N31 N 0.2347(4) 0.4787(5) 0.4265(5) 0.038(4) Uani 1 1 d . . . N32 N 0.1715(4) 0.4861(5) 0.3522(5) 0.034(3) Uani 1 1 d . . . N33 N 0.0715(5) 0.4604(5) 0.3731(5) 0.039(3) Uani 1 1 d . . . N34 N 0.0571(5) 0.4349(5) 0.4645(5) 0.041(4) Uani 1 1 d . . . C31 C 0.2671(6) 0.4721(6) 0.4625(7) 0.042(4) Uani 1 1 d . . . H31 H 0.2613 0.4465 0.4844 0.051 Uiso 1 1 calc R . . C32 C 0.3093(6) 0.5015(7) 0.4690(6) 0.043(4) Uani 1 1 d . . . H32 H 0.3307 0.4968 0.4955 0.051 Uiso 1 1 calc R . . C33 C 0.3185(6) 0.5369(6) 0.4362(6) 0.041(4) Uani 1 1 d . . . H33 H 0.3468 0.5570 0.4403 0.050 Uiso 1 1 calc R . . C34 C 0.2885(6) 0.5445(6) 0.3975(6) 0.040(4) Uani 1 1 d . . . C35 C 0.2958(6) 0.5793(6) 0.3618(6) 0.042(4) Uani 1 1 d . . . H35 H 0.3234 0.6007 0.3640 0.050 Uiso 1 1 calc R . . C36 C 0.2653(7) 0.5832(7) 0.3248(7) 0.047(5) Uani 1 1 d . . . H36 H 0.2719 0.6064 0.3006 0.057 Uiso 1 1 calc R . . C37 C 0.2237(7) 0.5536(7) 0.3212(6) 0.047(5) Uani 1 1 d . . . H37 H 0.2014 0.5586 0.2955 0.057 Uiso 1 1 calc R . . C38 C 0.2136(6) 0.5177(6) 0.3532(6) 0.040(4) Uani 1 1 d . . . C39 C 0.2456(6) 0.5137(5) 0.3934(6) 0.032(4) Uani 1 1 d . . . C40 C 0.1584(6) 0.4716(6) 0.3092(7) 0.042(4) Uani 1 1 d . . . H40 H 0.1816 0.4766 0.2846 0.051 Uiso 1 1 calc R . . C41 C 0.1136(6) 0.4495(6) 0.2968(6) 0.035(4) Uani 1 1 d . . . C42 C 0.0726(6) 0.4501(6) 0.3274(7) 0.045(5) Uani 1 1 d . . . H42 H 0.0418 0.4421 0.3133 0.054 Uiso 1 1 calc R . . C43 C 0.0246(6) 0.4706(6) 0.3933(7) 0.042(5) Uani 1 1 d . . . C44 C -0.0134(6) 0.4938(7) 0.3689(7) 0.050(5) Uani 1 1 d . . . H44 H -0.0080 0.5069 0.3382 0.060 Uiso 1 1 calc R . . C45 C -0.0599(7) 0.4978(7) 0.3904(9) 0.065(7) Uani 1 1 d . . . H45 H -0.0865 0.5121 0.3731 0.078 Uiso 1 1 calc R . . C46 C -0.0677(9) 0.4814(8) 0.4355(8) 0.069(7) Uani 1 1 d . . . H46 H -0.0992 0.4857 0.4494 0.083 Uiso 1 1 calc R . . C47 C -0.0286(6) 0.4575(6) 0.4629(8) 0.050(6) Uani 1 1 d . . . C48 C -0.0345(7) 0.4391(6) 0.5084(7) 0.049(5) Uani 1 1 d . . . H48 H -0.0657 0.4400 0.5234 0.059 Uiso 1 1 calc R . . C49 C 0.0050(7) 0.4202(6) 0.5305(8) 0.052(5) Uani 1 1 d . . . H49 H 0.0023 0.4074 0.5617 0.062 Uiso 1 1 calc R . . C50 C 0.0500(6) 0.4196(6) 0.5071(7) 0.043(4) Uani 1 1 d . . . H50 H 0.0777 0.4069 0.5239 0.051 Uiso 1 1 calc R . . C51 C 0.0175(6) 0.4543(6) 0.4410(7) 0.042(4) Uani 1 1 d . . . C52 C 0.1075(7) 0.4266(7) 0.2490(6) 0.042(4) Uani 1 1 d . . . C53 C 0.1346(7) 0.4421(7) 0.2110(7) 0.058(5) Uani 1 1 d . . . H53 H 0.1564 0.4691 0.2145 0.070 Uiso 1 1 calc R . . C54 C 0.1302(7) 0.4185(8) 0.1671(7) 0.058(5) Uani 1 1 d . . . H54 H 0.1505 0.4288 0.1418 0.069 Uiso 1 1 calc R . . C55 C 0.0971(8) 0.3802(7) 0.1595(8) 0.056(5) Uani 1 1 d . . . C56 C 0.0704(9) 0.3660(9) 0.1971(8) 0.071(7) Uani 1 1 d . . . H56 H 0.0474 0.3401 0.1932 0.085 Uiso 1 1 calc R . . C57 C 0.0751(7) 0.3882(8) 0.2418(7) 0.055(5) Uani 1 1 d . . . H57 H 0.0559 0.3767 0.2674 0.066 Uiso 1 1 calc R . . C58 C 0.0935(9) 0.3561(8) 0.1105(8) 0.078(7) Uani 1 1 d . . . H58A H 0.0840 0.3217 0.1141 0.117 Uiso 1 1 calc R . . H58B H 0.1256 0.3580 0.0949 0.117 Uiso 1 1 calc R . . H58C H 0.0687 0.3731 0.0913 0.117 Uiso 1 1 calc R . . U3 U 0.60576(2) 0.30444(2) 0.42551(2) 0.03166(16) Uani 1 1 d . . . O1U3 O 0.6118(4) 0.2426(4) 0.4473(4) 0.035(3) Uani 1 1 d . . . O2U3 O 0.6011(4) 0.3648(4) 0.3988(4) 0.040(3) Uani 1 1 d . . . U4 U 0.55389(2) 0.35515(2) 0.56351(2) 0.03038(16) Uani 1 1 d . . . O1U4 O 0.4912(4) 0.3643(4) 0.5453(4) 0.043(3) Uani 1 1 d . . . O2U4 O 0.6139(4) 0.3470(4) 0.5889(4) 0.043(3) Uani 1 1 d . . . O2 O 0.5803(5) 0.3326(4) 0.4929(4) 0.056(3) Uani 1 1 d U . . N61 N 0.6944(5) 0.3183(4) 0.4665(5) 0.040(4) Uani 1 1 d . . . N62 N 0.6800(5) 0.2933(5) 0.3725(5) 0.037(3) Uani 1 1 d . . . N63 N 0.5795(5) 0.2696(5) 0.3470(5) 0.042(4) Uani 1 1 d . . . N64 N 0.5126(5) 0.2804(5) 0.4155(5) 0.037(3) Uani 1 1 d . . . C61 C 0.7020(6) 0.3327(6) 0.5101(6) 0.038(4) Uani 1 1 d . . . H61 H 0.6747 0.3455 0.5269 0.045 Uiso 1 1 calc R . . C62 C 0.7464(7) 0.3306(6) 0.5332(7) 0.046(5) Uani 1 1 d . . . H62 H 0.7497 0.3431 0.5645 0.055 Uiso 1 1 calc R . . C63 C 0.7856(7) 0.3107(6) 0.5111(7) 0.047(5) Uani 1 1 d . . . H63 H 0.8164 0.3084 0.5271 0.057 Uiso 1 1 calc R . . C64 C 0.7808(7) 0.2933(6) 0.4645(7) 0.045(5) Uani 1 1 d . . . C65 C 0.8196(10) 0.2694(7) 0.4383(7) 0.075(8) Uani 1 1 d . . . H65 H 0.8511 0.2642 0.4524 0.090 Uiso 1 1 calc R . . C66 C 0.8103(6) 0.2546(7) 0.3937(9) 0.062(7) Uani 1 1 d . . . H66 H 0.8362 0.2392 0.3769 0.074 Uiso 1 1 calc R . . C67 C 0.7648(7) 0.2605(7) 0.3706(7) 0.048(5) Uani 1 1 d . . . H67 H 0.7604 0.2489 0.3391 0.058 Uiso 1 1 calc R . . C68 C 0.7262(6) 0.2833(6) 0.3937(7) 0.041(4) Uani 1 1 d . . . C69 C 0.7333(6) 0.2979(5) 0.4424(6) 0.037(4) Uani 1 1 d . . . C70 C 0.6793(6) 0.3059(5) 0.3274(6) 0.034(4) Uani 1 1 d . . . H70 H 0.7105 0.3145 0.3147 0.041 Uiso 1 1 calc R . . C71 C 0.6391(6) 0.3085(6) 0.2951(6) 0.037(4) Uani 1 1 d . . . C72 C 0.5952(6) 0.2844(5) 0.3052(7) 0.041(4) Uani 1 1 d . . . H72 H 0.5741 0.2778 0.2789 0.050 Uiso 1 1 calc R . . C73 C 0.5376(6) 0.2385(6) 0.3456(6) 0.040(4) Uani 1 1 d . . . C74 C 0.5296(6) 0.2021(6) 0.3112(6) 0.042(4) Uani 1 1 d . . . H74 H 0.5529 0.1969 0.2867 0.051 Uiso 1 1 calc R . . C75 C 0.4864(7) 0.1732(7) 0.3136(7) 0.050(5) Uani 1 1 d . . . H75 H 0.4810 0.1487 0.2903 0.060 Uiso 1 1 calc R . . C76 C 0.4528(7) 0.1791(7) 0.3478(7) 0.052(5) Uani 1 1 d . . . H76 H 0.4245 0.1587 0.3484 0.063 Uiso 1 1 calc R . . C77 C 0.4591(7) 0.2149(6) 0.3825(7) 0.048(5) Uani 1 1 d . . . C78 C 0.4257(6) 0.2263(7) 0.4184(7) 0.052(5) Uani 1 1 d . . . H78 H 0.3970 0.2067 0.4216 0.063 Uiso 1 1 calc R . . C79 C 0.4326(6) 0.2639(7) 0.4485(7) 0.049(5) Uani 1 1 d U . . H79 H 0.4084 0.2730 0.4710 0.058 Uiso 1 1 calc R . . C80 C 0.4794(5) 0.2901(5) 0.4447(5) 0.023(3) Uani 1 1 d U . . H80 H 0.4851 0.3165 0.4659 0.027 Uiso 1 1 calc R . . C81 C 0.5021(6) 0.2453(7) 0.3805(6) 0.038(4) Uani 1 1 d . . . C82 C 0.6453(6) 0.3325(5) 0.2480(6) 0.038(4) Uani 1 1 d . . . C83 C 0.6714(7) 0.3772(7) 0.2442(7) 0.056(5) Uani 1 1 d . . . H83 H 0.6877 0.3905 0.2713 0.068 Uiso 1 1 calc R . . C84 C 0.6734(8) 0.4016(8) 0.2015(7) 0.064(6) Uani 1 1 d . . . H84 H 0.6915 0.4313 0.2003 0.076 Uiso 1 1 calc R . . C85 C 0.6513(8) 0.3858(7) 0.1611(7) 0.055(5) Uani 1 1 d . . . C86 C 0.6265(6) 0.3397(7) 0.1642(6) 0.044(4) Uani 1 1 d . . . H86 H 0.6117 0.3260 0.1367 0.053 Uiso 1 1 calc R . . C87 C 0.6237(7) 0.3149(6) 0.2069(6) 0.047(5) Uani 1 1 d . . . H87 H 0.6064 0.2848 0.2080 0.056 Uiso 1 1 calc R . . C88 C 0.6532(8) 0.4140(8) 0.1151(8) 0.070(7) Uani 1 1 d . . . H88A H 0.6285 0.4402 0.1156 0.105 Uiso 1 1 calc R . . H88B H 0.6461 0.3919 0.0886 0.105 Uiso 1 1 calc R . . H88C H 0.6861 0.4281 0.1113 0.105 Uiso 1 1 calc R . . N91 N 0.5263(4) 0.2631(6) 0.5695(5) 0.040(4) Uani 1 1 d . . . N92 N 0.5241(5) 0.3278(5) 0.6412(5) 0.034(3) Uani 1 1 d . . . N93 N 0.5516(5) 0.4267(5) 0.6194(5) 0.037(3) Uani 1 1 d . . . N94 N 0.5682(5) 0.4413(5) 0.5261(5) 0.038(3) Uani 1 1 d . . . C91 C 0.5282(6) 0.2327(6) 0.5339(6) 0.039(4) Uani 1 1 d . . . H91 H 0.5507 0.2399 0.5092 0.047 Uiso 1 1 calc R . . C92 C 0.4995(7) 0.1900(6) 0.5292(6) 0.043(4) Uani 1 1 d . . . H92 H 0.5042 0.1678 0.5038 0.051 Uiso 1 1 calc R . . C93 C 0.4651(7) 0.1822(6) 0.5626(7) 0.045(5) Uani 1 1 d . . . H93 H 0.4436 0.1550 0.5593 0.054 Uiso 1 1 calc R . . C94 C 0.4602(6) 0.2135(6) 0.6026(7) 0.041(4) Uani 1 1 d . . . C95 C 0.4266(6) 0.2059(7) 0.6404(7) 0.046(5) Uani 1 1 d . . . H95 H 0.4054 0.1783 0.6406 0.056 Uiso 1 1 calc R . . C96 C 0.4259(7) 0.2397(7) 0.6767(7) 0.051(5) Uani 1 1 d . . . H96 H 0.4032 0.2350 0.7018 0.062 Uiso 1 1 calc R . . C97 C 0.4566(6) 0.2800(7) 0.6783(7) 0.044(4) Uani 1 1 d . . . H97 H 0.4552 0.3022 0.7041 0.052 Uiso 1 1 calc R . . C98 C 0.4897(5) 0.2876(6) 0.6415(6) 0.035(4) Uani 1 1 d . . . C99 C 0.4917(6) 0.2541(6) 0.6033(6) 0.038(4) Uani 1 1 d . . . C100 C 0.5425(6) 0.3406(6) 0.6822(6) 0.037(4) Uani 1 1 d . . . H100 H 0.5380 0.3180 0.7073 0.045 Uiso 1 1 calc R . . C101 C 0.5678(6) 0.3833(6) 0.6938(6) 0.034(4) Uani 1 1 d . . . C102 C 0.5661(6) 0.4254(6) 0.6647(6) 0.034(4) Uani 1 1 d . . . H102 H 0.5761 0.4554 0.6786 0.040 Uiso 1 1 calc R . . C103 C 0.5435(5) 0.4741(6) 0.6004(6) 0.033(4) Uani 1 1 d . . . C104 C 0.5263(7) 0.5138(6) 0.6263(7) 0.051(5) Uani 1 1 d . . . H104 H 0.5185 0.5097 0.6588 0.061 Uiso 1 1 calc R . . C105 C 0.5202(8) 0.5604(7) 0.6049(7) 0.057(5) Uani 1 1 d . . . H105 H 0.5063 0.5867 0.6224 0.068 Uiso 1 1 calc R . . C106 C 0.5343(6) 0.5672(6) 0.5594(7) 0.044(5) Uani 1 1 d . . . H106 H 0.5337 0.5992 0.5463 0.053 Uiso 1 1 calc R . . C107 C 0.5499(6) 0.5275(6) 0.5312(7) 0.039(4) Uani 1 1 d . . . C108 C 0.5637(6) 0.5325(6) 0.4822(7) 0.044(5) Uani 1 1 d . . . H108 H 0.5624 0.5637 0.4674 0.052 Uiso 1 1 calc R . . C109 C 0.5786(6) 0.4931(6) 0.4573(7) 0.040(4) Uani 1 1 d . . . H109 H 0.5883 0.4959 0.4251 0.049 Uiso 1 1 calc R . . C110 C 0.5792(6) 0.4474(6) 0.4809(6) 0.040(4) Uani 1 1 d . . . H110 H 0.5880 0.4194 0.4631 0.048 Uiso 1 1 calc R . . C111 C 0.5526(6) 0.4812(6) 0.5510(6) 0.036(4) Uani 1 1 d . . . C112 C 0.5895(6) 0.3862(6) 0.7431(6) 0.039(4) Uani 1 1 d . . . C113 C 0.6286(6) 0.3557(6) 0.7565(7) 0.045(4) Uani 1 1 d . . . H113 H 0.6445 0.3365 0.7331 0.054 Uiso 1 1 calc R . . C114 C 0.6447(7) 0.3531(7) 0.8034(7) 0.051(5) Uani 1 1 d . . . H114 H 0.6714 0.3321 0.8114 0.061 Uiso 1 1 calc R . . C115 C 0.6224(7) 0.3804(7) 0.8389(7) 0.053(5) Uani 1 1 d . . . C116 C 0.5848(7) 0.4118(7) 0.8240(7) 0.053(5) Uani 1 1 d . . . H116 H 0.5695 0.4318 0.8470 0.063 Uiso 1 1 calc R . . C117 C 0.5682(7) 0.4155(7) 0.7768(7) 0.052(5) Uani 1 1 d . . . H117 H 0.5428 0.4378 0.7684 0.063 Uiso 1 1 calc R . . C118 C 0.6383(8) 0.3749(9) 0.8889(7) 0.073(7) Uani 1 1 d . . . H11A H 0.6422 0.4073 0.9032 0.110 Uiso 1 1 calc R . . H11B H 0.6699 0.3575 0.8902 0.110 Uiso 1 1 calc R . . H11C H 0.6134 0.3563 0.9062 0.110 Uiso 1 1 calc R . . N121 N 0.2892(8) 0.2499(9) 0.7478(8) 0.090(7) Uani 1 1 d . . . C121 C 0.2954(8) 0.2107(10) 0.7389(9) 0.069(7) Uani 1 1 d . . . C122 C 0.3054(9) 0.1603(10) 0.7256(12) 0.111(11) Uani 1 1 d . . . H12A H 0.2742 0.1428 0.7212 0.167 Uiso 1 1 calc R . . H12B H 0.3248 0.1445 0.7508 0.167 Uiso 1 1 calc R . . H12C H 0.3240 0.1597 0.6960 0.167 Uiso 1 1 calc R . . N122 N 0.5000 0.4706(16) 0.2500 0.24(4) Uani 1 2 d S . . C123 C 0.5000 0.435(3) 0.2500 0.21(4) Uani 1 2 d SU . . C124 C 0.5000 0.372(3) 0.2500 0.31(5) Uani 1 2 d SU . . H12D H 0.5174 0.3599 0.2783 0.470 Uiso 0.50 1 calc PR . . H12E H 0.5166 0.3599 0.2216 0.470 Uiso 0.50 1 calc PR . . H12F H 0.4659 0.3599 0.2501 0.470 Uiso 0.50 1 calc PR . . 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 0.0306(3) 0.0253(3) 0.0362(4) -0.0007(3) 0.0030(3) -0.0007(2) O1U1 0.041(7) 0.031(6) 0.032(6) -0.008(5) 0.007(5) 0.010(5) O2U1 0.051(7) 0.038(6) 0.030(6) -0.003(5) 0.012(5) 0.001(5) U2 0.0245(3) 0.0295(3) 0.0462(4) -0.0038(3) 0.0034(3) -0.0019(2) O1U2 0.026(6) 0.048(7) 0.050(8) -0.007(6) -0.003(5) -0.001(5) O2U2 0.035(7) 0.034(6) 0.045(7) 0.001(6) 0.005(5) -0.005(5) O1 0.054(5) 0.083(5) 0.043(5) 0.018(4) 0.005(4) 0.003(4) N1 0.028(7) 0.031(7) 0.044(9) 0.000(7) -0.002(6) -0.007(6) N2 0.036(8) 0.033(7) 0.028(8) 0.004(6) -0.002(6) 0.004(6) N3 0.054(9) 0.035(8) 0.026(8) -0.004(7) 0.010(7) -0.010(6) N4 0.026(8) 0.070(10) 0.024(8) -0.004(8) 0.014(6) 0.008(7) C1 0.036(9) 0.029(9) 0.036(10) -0.002(8) 0.001(8) -0.007(7) C2 0.024(9) 0.043(10) 0.045(11) -0.018(9) -0.004(8) 0.005(7) C3 0.026(9) 0.035(9) 0.052(12) -0.009(9) 0.005(8) 0.002(7) C4 0.042(10) 0.026(9) 0.057(13) 0.017(9) 0.013(9) 0.007(7) C5 0.043(11) 0.030(9) 0.052(12) 0.005(9) 0.012(9) 0.009(7) C6 0.042(10) 0.028(9) 0.057(13) 0.002(9) 0.012(9) 0.015(7) C7 0.051(11) 0.030(9) 0.045(11) 0.008(9) 0.007(9) 0.006(8) C8 0.030(9) 0.032(9) 0.048(11) -0.004(9) 0.010(8) -0.004(7) C9 0.029(9) 0.021(8) 0.032(9) -0.001(7) 0.003(7) -0.006(6) C10 0.029(9) 0.032(9) 0.050(11) -0.004(9) 0.001(8) 0.006(7) C11 0.042(10) 0.028(9) 0.039(10) 0.004(8) 0.001(8) -0.011(7) C12 0.044(10) 0.026(9) 0.041(11) -0.006(8) -0.002(8) -0.002(7) C13 0.048(11) 0.036(9) 0.033(10) -0.019(9) 0.006(8) -0.002(8) C14 0.062(13) 0.047(11) 0.026(10) -0.004(9) -0.001(9) -0.002(9) C15 0.069(14) 0.033(10) 0.049(12) -0.010(10) 0.001(10) -0.016(9) C16 0.060(13) 0.035(10) 0.059(13) -0.008(10) 0.016(10) -0.015(9) C17 0.068(14) 0.034(10) 0.051(13) 0.003(10) 0.002(10) 0.002(9) C18 0.048(12) 0.027(9) 0.097(18) -0.006(11) 0.029(12) -0.018(8) C19 0.043(12) 0.049(11) 0.064(14) 0.018(10) 0.006(10) 0.021(9) C20 0.021(6) 0.023(6) 0.048(8) -0.011(6) 0.004(6) -0.009(5) C21 0.048(11) 0.030(9) 0.035(10) 0.010(8) -0.001(8) 0.011(7) C22 0.029(9) 0.033(9) 0.053(12) -0.003(9) 0.001(8) -0.016(7) C23 0.044(11) 0.041(10) 0.045(11) 0.000(9) 0.003(9) 0.000(8) C24 0.048(11) 0.033(10) 0.065(14) 0.009(10) 0.011(10) -0.005(8) C25 0.046(11) 0.051(11) 0.049(12) -0.004(10) 0.023(9) -0.010(9) C26 0.049(12) 0.039(10) 0.057(13) 0.000(10) 0.001(10) -0.012(8) C27 0.051(11) 0.036(9) 0.034(10) 0.010(8) 0.005(8) 0.009(8) C28 0.082(16) 0.050(12) 0.057(14) 0.001(11) 0.022(12) 0.009(11) N31 0.013(7) 0.045(8) 0.057(10) -0.001(8) 0.005(6) 0.014(6) N32 0.014(6) 0.044(8) 0.043(9) 0.002(7) 0.000(6) -0.004(5) N33 0.041(9) 0.041(8) 0.036(9) -0.003(7) 0.008(7) 0.004(6) N34 0.040(9) 0.041(8) 0.043(9) -0.006(7) 0.011(7) -0.010(6) C31 0.036(10) 0.040(10) 0.051(12) 0.017(9) -0.005(9) 0.004(8) C32 0.032(10) 0.060(12) 0.036(10) -0.011(10) -0.003(8) 0.006(8) C33 0.030(10) 0.053(11) 0.040(11) -0.013(9) -0.004(8) -0.015(8) C34 0.046(11) 0.045(10) 0.029(10) -0.006(9) 0.008(8) 0.001(8) C35 0.035(10) 0.050(11) 0.039(11) -0.006(9) -0.005(8) -0.021(8) C36 0.045(11) 0.055(11) 0.043(11) 0.016(10) 0.008(9) -0.012(9) C37 0.053(12) 0.055(12) 0.033(10) 0.001(10) -0.010(9) -0.001(9) C38 0.045(11) 0.027(9) 0.048(12) 0.002(9) 0.003(9) 0.004(7) C39 0.038(10) 0.028(8) 0.029(9) 0.007(8) 0.008(7) 0.002(7) C40 0.036(10) 0.048(11) 0.042(11) -0.003(9) -0.007(8) 0.011(8) C41 0.036(10) 0.036(9) 0.033(10) 0.006(8) -0.001(8) -0.003(7) C42 0.039(10) 0.029(9) 0.066(14) -0.001(10) -0.012(9) -0.010(7) C43 0.033(10) 0.031(9) 0.063(13) -0.015(9) -0.003(9) 0.000(7) C44 0.038(11) 0.053(11) 0.059(13) -0.020(10) -0.012(9) 0.008(9) C45 0.035(11) 0.067(14) 0.093(18) -0.050(14) -0.017(11) 0.025(10) C46 0.077(17) 0.069(14) 0.062(15) -0.036(13) 0.028(13) -0.039(12) C47 0.014(8) 0.044(10) 0.093(17) -0.039(11) -0.010(9) 0.008(7) C48 0.044(12) 0.041(10) 0.064(14) -0.032(10) 0.025(10) -0.022(9) C49 0.032(11) 0.041(10) 0.082(16) -0.012(10) 0.005(10) 0.002(8) C50 0.035(10) 0.042(10) 0.051(12) -0.016(9) -0.005(9) -0.005(8) C51 0.040(10) 0.024(8) 0.062(13) 0.004(9) -0.013(9) 0.003(7) C52 0.049(11) 0.053(11) 0.025(10) -0.003(9) -0.012(8) 0.003(9) C53 0.052(13) 0.061(13) 0.061(14) -0.004(12) -0.025(11) -0.003(10) C54 0.041(12) 0.084(15) 0.047(13) 0.010(12) -0.003(9) 0.014(10) C55 0.067(14) 0.050(12) 0.052(13) -0.013(11) -0.025(11) 0.017(10) C56 0.067(16) 0.095(18) 0.051(14) -0.017(14) -0.020(12) 0.013(13) C57 0.040(11) 0.074(14) 0.051(13) -0.010(11) -0.005(9) 0.005(10) C58 0.092(18) 0.080(16) 0.061(15) -0.023(13) -0.024(13) 0.018(14) U3 0.0284(3) 0.0283(3) 0.0384(4) -0.0004(3) 0.0037(3) -0.0017(2) O1U3 0.033(6) 0.040(6) 0.033(6) 0.001(5) -0.006(5) 0.005(5) O2U3 0.042(7) 0.036(6) 0.040(7) 0.005(6) 0.003(6) 0.003(5) U4 0.0270(3) 0.0253(3) 0.0388(4) 0.0013(3) -0.0011(3) -0.0011(2) O1U4 0.028(6) 0.040(7) 0.062(8) 0.004(6) 0.003(6) 0.000(5) O2U4 0.033(7) 0.028(6) 0.067(9) 0.006(6) -0.008(6) -0.005(5) O2 0.094(8) 0.048(6) 0.025(6) 0.006(5) 0.016(6) 0.017(6) N61 0.035(8) 0.025(7) 0.059(11) -0.004(7) 0.003(7) -0.002(6) N62 0.049(9) 0.030(7) 0.032(8) -0.009(7) 0.010(7) -0.007(6) N63 0.035(8) 0.058(9) 0.033(8) 0.001(7) 0.004(7) -0.005(7) N64 0.034(8) 0.041(8) 0.035(8) 0.007(7) 0.010(6) 0.010(6) C61 0.037(10) 0.047(10) 0.030(10) 0.006(9) 0.001(8) -0.008(8) C62 0.048(12) 0.038(10) 0.052(12) -0.004(9) -0.008(10) -0.015(8) C63 0.045(11) 0.047(11) 0.050(12) 0.026(10) -0.011(9) -0.010(9) C64 0.037(10) 0.042(10) 0.055(13) 0.019(10) 0.017(9) 0.004(8) C65 0.13(2) 0.058(14) 0.033(12) 0.025(11) -0.029(13) -0.053(14) C66 0.018(9) 0.045(11) 0.12(2) 0.026(13) 0.005(11) 0.006(8) C67 0.053(12) 0.054(11) 0.037(11) 0.017(9) 0.005(9) -0.002(9) C68 0.032(10) 0.033(9) 0.057(12) 0.027(9) 0.009(9) -0.006(7) C69 0.041(10) 0.020(8) 0.050(12) -0.002(8) 0.003(8) -0.006(7) C70 0.040(10) 0.021(8) 0.041(11) -0.009(8) 0.014(8) -0.007(7) C71 0.048(11) 0.030(9) 0.033(10) 0.005(8) 0.006(8) -0.002(8) C72 0.038(10) 0.027(9) 0.060(13) -0.006(9) 0.001(9) 0.001(7) C73 0.031(10) 0.045(10) 0.044(11) -0.002(9) -0.001(8) -0.004(7) C74 0.042(10) 0.051(11) 0.034(10) 0.004(9) -0.004(8) 0.008(8) C75 0.045(12) 0.051(11) 0.054(13) -0.013(10) -0.002(10) -0.018(9) C76 0.031(10) 0.061(12) 0.065(14) -0.009(11) -0.011(9) -0.018(9) C77 0.044(11) 0.040(10) 0.060(13) 0.012(10) -0.007(10) 0.000(8) C78 0.018(9) 0.075(14) 0.064(14) 0.025(12) 0.000(9) -0.015(8) C79 0.031(7) 0.060(8) 0.055(9) -0.005(7) -0.003(7) 0.019(7) C80 0.015(5) 0.021(5) 0.031(5) -0.003(4) -0.007(4) 0.004(4) C81 0.027(9) 0.058(11) 0.027(9) 0.006(9) -0.007(7) 0.012(8) C82 0.040(10) 0.023(8) 0.051(11) -0.014(8) 0.017(9) -0.009(7) C83 0.059(13) 0.059(12) 0.051(13) -0.003(11) 0.002(10) -0.014(10) C84 0.095(18) 0.057(13) 0.038(12) 0.003(11) -0.002(11) -0.029(12) C85 0.060(13) 0.052(12) 0.053(13) 0.007(11) 0.013(10) 0.010(10) C86 0.038(10) 0.058(12) 0.037(11) 0.000(9) 0.000(8) -0.002(8) C87 0.064(13) 0.043(11) 0.034(11) 0.000(9) 0.019(9) -0.010(9) C88 0.056(14) 0.087(16) 0.067(15) 0.039(13) 0.005(11) 0.003(11) N91 0.016(7) 0.079(11) 0.025(8) 0.005(8) -0.004(6) -0.011(7) N92 0.031(8) 0.035(7) 0.035(8) -0.010(7) -0.007(6) 0.009(6) N93 0.045(9) 0.029(7) 0.038(9) -0.003(7) -0.006(7) -0.003(6) N94 0.033(8) 0.033(8) 0.047(9) -0.004(7) -0.003(7) 0.000(6) C91 0.036(10) 0.039(10) 0.044(11) 0.007(9) 0.005(8) -0.003(7) C92 0.054(12) 0.033(9) 0.041(11) -0.005(9) 0.008(9) 0.002(8) C93 0.050(11) 0.029(9) 0.057(12) -0.007(9) 0.003(9) -0.022(8) C94 0.036(10) 0.029(9) 0.058(12) -0.001(9) -0.004(9) -0.001(7) C95 0.032(10) 0.051(11) 0.055(12) 0.003(10) 0.000(9) -0.016(8) C96 0.040(11) 0.053(12) 0.061(13) -0.012(11) 0.010(9) -0.010(9) C97 0.020(9) 0.058(11) 0.052(12) -0.003(10) 0.003(8) -0.006(8) C98 0.015(8) 0.037(9) 0.051(11) 0.003(9) -0.007(7) -0.004(6) C99 0.038(10) 0.031(9) 0.045(11) -0.002(9) -0.006(8) 0.014(7) C100 0.031(9) 0.043(10) 0.037(10) 0.001(9) -0.005(8) 0.003(7) C101 0.032(9) 0.041(10) 0.028(9) -0.001(8) -0.003(7) -0.009(7) C102 0.030(9) 0.031(9) 0.040(10) 0.002(8) -0.006(8) 0.000(7) C103 0.024(9) 0.036(9) 0.037(10) 0.009(8) -0.015(7) 0.007(7) C104 0.059(13) 0.041(11) 0.052(12) -0.007(10) 0.003(10) 0.014(9) C105 0.075(15) 0.042(11) 0.053(13) -0.009(10) -0.005(11) 0.023(10) C106 0.029(10) 0.034(9) 0.070(14) -0.005(10) -0.011(9) 0.004(7) C107 0.025(9) 0.036(9) 0.057(12) -0.001(9) -0.010(8) 0.003(7) C108 0.042(11) 0.032(9) 0.057(13) 0.005(9) -0.015(9) -0.003(8) C109 0.022(9) 0.037(9) 0.063(12) 0.019(9) 0.008(8) 0.006(7) C110 0.042(10) 0.036(10) 0.042(11) -0.001(9) -0.008(8) -0.006(8) C111 0.027(9) 0.028(9) 0.054(12) 0.002(9) -0.013(8) -0.001(7) C112 0.042(10) 0.038(10) 0.036(10) -0.004(8) -0.004(8) -0.028(8) C113 0.030(10) 0.047(10) 0.058(13) 0.002(10) 0.000(9) 0.003(8) C114 0.041(11) 0.050(11) 0.062(14) 0.017(11) -0.015(10) -0.012(9) C115 0.048(12) 0.061(13) 0.049(12) 0.011(11) -0.003(10) -0.019(10) C116 0.053(13) 0.048(11) 0.056(13) -0.006(10) 0.000(10) -0.003(9) C117 0.054(12) 0.043(11) 0.061(14) -0.012(10) -0.010(10) 0.006(9) C118 0.070(16) 0.104(18) 0.046(13) 0.000(13) -0.020(11) -0.013(13) N121 0.092(17) 0.105(18) 0.072(15) 0.008(15) -0.007(12) 0.010(14) C121 0.050(14) 0.081(17) 0.074(17) 0.009(16) 0.016(12) -0.015(13) C122 0.055(16) 0.10(2) 0.18(3) 0.01(2) -0.003(18) 0.020(15) N122 0.54(12) 0.08(3) 0.09(3) 0.000 0.11(5) 0.000 C123 0.21(4) 0.21(4) 0.21(4) 0.000 0.007(10) 0.000 C124 0.31(5) 0.31(5) 0.32(5) 0.000 0.02(2) 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 O2U1 1.789(11) . ? U1 O1U1 1.795(10) . ? U1 O1 2.186(13) . ? U1 N3 2.460(14) . ? U1 N2 2.554(12) . ? U1 N1 2.649(13) . ? U1 N4 2.696(15) . ? U2 O1U2 1.803(11) . ? U2 O2U2 1.822(10) . ? U2 O1 2.198(13) . ? U2 N32 2.494(13) . ? U2 N33 2.517(15) . ? U2 N31 2.585(13) . ? U2 N34 2.604(13) . ? N1 C1 1.33(2) . ? N1 C9 1.398(19) . ? N2 C10 1.34(2) . ? N2 C8 1.410(19) . ? N3 C12 1.31(2) . ? N3 C13 1.48(2) . ? N4 C20 1.25(2) . ? N4 C21 1.36(2) . ? C1 C2 1.42(2) . ? C2 C3 1.34(2) . ? C3 C4 1.42(2) . ? C4 C5 1.38(2) . ? C4 C9 1.40(2) . ? C5 C6 1.39(2) . ? C6 C7 1.42(2) . ? C7 C8 1.38(2) . ? C8 C9 1.41(2) . ? C10 C11 1.41(2) . ? C11 C12 1.41(2) . ? C11 C22 1.50(2) . ? C13 C14 1.37(2) . ? C13 C21 1.40(2) . ? C14 C15 1.44(2) . ? C15 C16 1.36(3) . ? C16 C17 1.41(3) . ? C17 C21 1.41(2) . ? C17 C18 1.45(3) . ? C18 C19 1.34(3) . ? C19 C20 1.43(2) . ? C22 C27 1.37(2) . ? C22 C23 1.42(2) . ? C23 C24 1.35(2) . ? C24 C25 1.39(3) . ? C25 C26 1.41(2) . ? C25 C28 1.53(2) . ? C26 C27 1.39(2) . ? N31 C31 1.35(2) . ? N31 C39 1.37(2) . ? N32 C40 1.32(2) . ? N32 C38 1.43(2) . ? N33 C42 1.32(2) . ? N33 C43 1.43(2) . ? N34 C50 1.29(2) . ? N34 C51 1.36(2) . ? C31 C32 1.41(2) . ? C32 C33 1.36(2) . ? C33 C34 1.37(2) . ? C34 C35 1.40(2) . ? C34 C39 1.44(2) . ? C35 C36 1.33(2) . ? C36 C37 1.39(2) . ? C37 C38 1.36(2) . ? C38 C39 1.43(2) . ? C40 C41 1.40(2) . ? C41 C42 1.42(2) . ? C41 C52 1.49(2) . ? C43 C44 1.39(2) . ? C43 C51 1.43(3) . ? C44 C45 1.41(3) . ? C45 C46 1.37(3) . ? C46 C47 1.46(3) . ? C47 C48 1.39(3) . ? C47 C51 1.41(2) . ? C48 C49 1.34(3) . ? C49 C50 1.39(2) . ? C52 C53 1.37(3) . ? C52 C57 1.38(3) . ? C53 C54 1.40(3) . ? C54 C55 1.40(3) . ? C55 C56 1.35(3) . ? C55 C58 1.53(3) . ? C56 C57 1.41(3) . ? U3 O1U3 1.807(10) . ? U3 O2U3 1.821(10) . ? U3 O2 2.171(11) . ? U3 N63 2.511(14) . ? U3 N62 2.539(13) . ? U3 N64 2.623(14) . ? U3 N61 2.684(14) . ? U4 O2U4 1.787(11) . ? U4 O1U4 1.790(11) . ? U4 O2 2.213(11) . ? U4 N92 2.461(14) . ? U4 N93 2.517(13) . ? U4 N94 2.614(13) . ? U4 N91 2.634(15) . ? N61 C61 1.31(2) . ? N61 C69 1.38(2) . ? N62 C70 1.32(2) . ? N62 C68 1.41(2) . ? N63 C72 1.32(2) . ? N63 C73 1.42(2) . ? N64 C80 1.254(18) . ? N64 C81 1.41(2) . ? C61 C62 1.36(2) . ? C62 C63 1.35(2) . ? C63 C64 1.40(3) . ? C64 C69 1.43(2) . ? C64 C65 1.45(3) . ? C65 C66 1.34(3) . ? C66 C67 1.40(3) . ? C67 C68 1.39(2) . ? C68 C69 1.45(2) . ? C70 C71 1.42(2) . ? C71 C72 1.39(2) . ? C71 C82 1.49(2) . ? C73 C81 1.40(2) . ? C73 C74 1.41(2) . ? C74 C75 1.42(2) . ? C75 C76 1.34(2) . ? C76 C77 1.39(3) . ? C77 C78 1.40(3) . ? C77 C81 1.43(2) . ? C78 C79 1.35(3) . ? C79 C80 1.46(2) . ? C82 C87 1.38(2) . ? C82 C83 1.42(2) . ? C83 C84 1.38(3) . ? C84 C85 1.35(3) . ? C85 C86 1.43(2) . ? C85 C88 1.51(3) . ? C86 C87 1.39(2) . ? N91 C91 1.31(2) . ? N91 C99 1.37(2) . ? N92 C100 1.30(2) . ? N92 C98 1.442(19) . ? N93 C102 1.33(2) . ? N93 C103 1.419(19) . ? N94 C110 1.32(2) . ? N94 C111 1.37(2) . ? C91 C92 1.41(2) . ? C92 C93 1.35(2) . ? C93 C94 1.43(2) . ? C94 C99 1.40(2) . ? C94 C95 1.42(2) . ? C95 C96 1.38(2) . ? C96 C97 1.38(2) . ? C97 C98 1.40(2) . ? C98 C99 1.42(2) . ? C100 C101 1.39(2) . ? C101 C102 1.42(2) . ? C101 C112 1.51(2) . ? C103 C104 1.40(2) . ? C103 C111 1.43(2) . ? C104 C105 1.42(2) . ? C105 C106 1.36(3) . ? C106 C107 1.42(2) . ? C107 C111 1.39(2) . ? C107 C108 1.44(2) . ? C108 C109 1.35(2) . ? C109 C110 1.42(2) . ? C112 C117 1.37(2) . ? C112 C113 1.40(2) . ? C113 C114 1.39(2) . ? C114 C115 1.39(3) . ? C115 C116 1.40(3) . ? C115 C118 1.48(3) . ? C116 C117 1.40(3) . ? N121 C121 1.12(3) . ? C121 C122 1.45(3) . ? N122 C123 0.97(9) . ? C123 C124 1.73(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2U1 U1 O1U1 176.2(5) . . ? O2U1 U1 O1 91.7(5) . . ? O1U1 U1 O1 92.1(5) . . ? O2U1 U1 N3 87.4(5) . . ? O1U1 U1 N3 89.5(5) . . ? O1 U1 N3 144.5(5) . . ? O2U1 U1 N2 83.7(5) . . ? O1U1 U1 N2 93.1(4) . . ? O1 U1 N2 145.9(5) . . ? N3 U1 N2 69.2(4) . . ? O2U1 U1 N1 96.2(4) . . ? O1U1 U1 N1 84.3(4) . . ? O1 U1 N1 83.9(5) . . ? N3 U1 N1 131.4(4) . . ? N2 U1 N1 63.2(4) . . ? O2U1 U1 N4 96.6(4) . . ? O1U1 U1 N4 83.9(4) . . ? O1 U1 N4 82.0(5) . . ? N3 U1 N4 62.9(4) . . ? N2 U1 N4 132.0(4) . . ? N1 U1 N4 161.2(4) . . ? O1U2 U2 O2U2 172.8(5) . . ? O1U2 U2 O1 92.7(5) . . ? O2U2 U2 O1 94.5(5) . . ? O1U2 U2 N32 86.1(5) . . ? O2U2 U2 N32 87.6(5) . . ? O1 U2 N32 146.3(4) . . ? O1U2 U2 N33 84.4(5) . . ? O2U2 U2 N33 90.0(5) . . ? O1 U2 N33 143.6(5) . . ? N32 U2 N33 69.8(4) . . ? O1U2 U2 N31 99.0(4) . . ? O2U2 U2 N31 81.5(4) . . ? O1 U2 N31 82.7(5) . . ? N32 U2 N31 64.3(4) . . ? N33 U2 N31 133.6(4) . . ? O1U2 U2 N34 97.1(4) . . ? O2U2 U2 N34 84.5(4) . . ? O1 U2 N34 80.8(5) . . ? N32 U2 N34 132.8(4) . . ? N33 U2 N34 63.7(5) . . ? N31 U2 N34 157.4(5) . . ? U1 O1 U2 177.2(7) . . ? C1 N1 C9 118.4(14) . . ? C1 N1 U1 123.7(10) . . ? C9 N1 U1 116.0(10) . . ? C10 N2 C8 118.1(13) . . ? C10 N2 U1 122.6(10) . . ? C8 N2 U1 117.9(10) . . ? C12 N3 C13 112.7(13) . . ? C12 N3 U1 125.8(11) . . ? C13 N3 U1 119.1(10) . . ? C20 N4 C21 119.4(15) . . ? C20 N4 U1 124.8(11) . . ? C21 N4 U1 112.9(11) . . ? N1 C1 C2 123.6(16) . . ? C3 C2 C1 117.9(16) . . ? C2 C3 C4 121.3(16) . . ? C5 C4 C9 119.0(18) . . ? C5 C4 C3 123.2(16) . . ? C9 C4 C3 117.9(15) . . ? C4 C5 C6 120.4(16) . . ? C5 C6 C7 120.5(16) . . ? C8 C7 C6 119.6(17) . . ? C7 C8 C9 118.8(15) . . ? C7 C8 N2 122.7(16) . . ? C9 C8 N2 118.5(15) . . ? N1 C9 C4 120.8(15) . . ? N1 C9 C8 117.6(13) . . ? C4 C9 C8 121.6(15) . . ? N2 C10 C11 126.7(16) . . ? C10 C11 C12 121.7(15) . . ? C10 C11 C22 121.6(14) . . ? C12 C11 C22 116.0(14) . . ? N3 C12 C11 125.9(16) . . ? C14 C13 C21 122.5(16) . . ? C14 C13 N3 122.6(16) . . ? C21 C13 N3 114.9(15) . . ? C13 C14 C15 117.3(17) . . ? C16 C15 C14 122.3(19) . . ? C15 C16 C17 118.5(17) . . ? C16 C17 C21 121.2(17) . . ? C16 C17 C18 123.1(17) . . ? C21 C17 C18 115.7(18) . . ? C19 C18 C17 120.2(16) . . ? C18 C19 C20 117.1(17) . . ? N4 C20 C19 125.0(17) . . ? N4 C21 C13 119.8(16) . . ? N4 C21 C17 122.1(16) . . ? C13 C21 C17 118.1(17) . . ? C27 C22 C23 116.3(16) . . ? C27 C22 C11 123.5(15) . . ? C23 C22 C11 119.8(16) . . ? C24 C23 C22 122.1(18) . . ? C23 C24 C25 121.8(17) . . ? C24 C25 C26 117.2(17) . . ? C24 C25 C28 121.9(17) . . ? C26 C25 C28 121.0(18) . . ? C27 C26 C25 120.5(18) . . ? C22 C27 C26 122.1(16) . . ? C31 N31 C39 117.5(14) . . ? C31 N31 U2 123.9(11) . . ? C39 N31 U2 116.0(10) . . ? C40 N32 C38 114.0(14) . . ? C40 N32 U2 126.7(11) . . ? C38 N32 U2 117.8(11) . . ? C42 N33 C43 117.4(15) . . ? C42 N33 U2 124.1(11) . . ? C43 N33 U2 117.8(11) . . ? C50 N34 C51 117.2(16) . . ? C50 N34 U2 123.8(12) . . ? C51 N34 U2 117.3(11) . . ? N31 C31 C32 123.1(16) . . ? C33 C32 C31 118.0(16) . . ? C32 C33 C34 122.5(16) . . ? C33 C34 C35 126.0(17) . . ? C33 C34 C39 116.6(15) . . ? C35 C34 C39 117.4(16) . . ? C36 C35 C34 121.8(16) . . ? C35 C36 C37 120.6(17) . . ? C38 C37 C36 122.5(18) . . ? C37 C38 C39 117.3(16) . . ? C37 C38 N32 125.8(17) . . ? C39 C38 N32 116.6(14) . . ? N31 C39 C38 117.5(14) . . ? N31 C39 C34 122.3(15) . . ? C38 C39 C34 120.2(14) . . ? N32 C40 C41 125.8(17) . . ? C40 C41 C42 121.7(16) . . ? C40 C41 C52 119.8(15) . . ? C42 C41 C52 118.5(15) . . ? N33 C42 C41 128.8(16) . . ? C44 C43 N33 123.5(18) . . ? C44 C43 C51 120.2(17) . . ? N33 C43 C51 116.3(15) . . ? C43 C44 C45 119(2) . . ? C46 C45 C44 121(2) . . ? C45 C46 C47 122(2) . . ? C48 C47 C51 119.7(17) . . ? C48 C47 C46 124.2(18) . . ? C51 C47 C46 116(2) . . ? C49 C48 C47 118.2(17) . . ? C48 C49 C50 119(2) . . ? N34 C50 C49 125.2(18) . . ? N34 C51 C47 120.6(18) . . ? N34 C51 C43 117.8(16) . . ? C47 C51 C43 121.5(17) . . ? C53 C52 C57 117.6(17) . . ? C53 C52 C41 121.3(17) . . ? C57 C52 C41 121.0(17) . . ? C52 C53 C54 120.5(19) . . ? C55 C54 C53 122(2) . . ? C56 C55 C54 116(2) . . ? C56 C55 C58 124(2) . . ? C54 C55 C58 120(2) . . ? C55 C56 C57 123(2) . . ? C52 C57 C56 121(2) . . ? O1U3 U3 O2U3 175.2(5) . . ? O1U3 U3 O2 93.7(5) . . ? O2U3 U3 O2 91.1(5) . . ? O1U3 U3 N63 88.2(5) . . ? O2U3 U3 N63 87.7(5) . . ? O2 U3 N63 144.9(5) . . ? O1U3 U3 N62 91.0(4) . . ? O2U3 U3 N62 85.2(5) . . ? O2 U3 N62 145.0(5) . . ? N63 U3 N62 69.8(4) . . ? O1U3 U3 N64 83.5(4) . . ? O2U3 U3 N64 96.9(5) . . ? O2 U3 N64 82.5(5) . . ? N63 U3 N64 62.9(4) . . ? N62 U3 N64 132.5(4) . . ? O1U3 U3 N61 84.7(4) . . ? O2U3 U3 N61 96.2(5) . . ? O2 U3 N61 82.1(5) . . ? N63 U3 N61 132.9(4) . . ? N62 U3 N61 63.8(5) . . ? N64 U3 N61 159.9(4) . . ? O2U4 U4 O1U4 173.0(6) . . ? O2U4 U4 O2 91.5(5) . . ? O1U4 U4 O2 95.5(5) . . ? O2U4 U4 N92 84.8(5) . . ? O1U4 U4 N92 88.8(5) . . ? O2 U4 N92 146.1(4) . . ? O2U4 U4 N93 82.7(5) . . ? O1U4 U4 N93 92.5(5) . . ? O2 U4 N93 142.4(5) . . ? N92 U4 N93 70.6(4) . . ? O2U4 U4 N94 97.8(4) . . ? O1U4 U4 N94 84.4(4) . . ? O2 U4 N94 80.6(4) . . ? N92 U4 N94 133.3(4) . . ? N93 U4 N94 63.7(4) . . ? O2U4 U4 N91 96.5(4) . . ? O1U4 U4 N91 83.2(4) . . ? O2 U4 N91 83.5(4) . . ? N92 U4 N91 63.6(4) . . ? N93 U4 N91 134.0(4) . . ? N94 U4 N91 158.8(4) . . ? U3 O2 U4 175.3(6) . . ? C61 N61 C69 118.0(15) . . ? C61 N61 U3 125.6(11) . . ? C69 N61 U3 114.7(11) . . ? C70 N62 C68 117.7(14) . . ? C70 N62 U3 122.3(11) . . ? C68 N62 U3 118.7(11) . . ? C72 N63 C73 115.1(15) . . ? C72 N63 U3 125.4(11) . . ? C73 N63 U3 118.2(10) . . ? C80 N64 C81 117.6(14) . . ? C80 N64 U3 125.0(11) . . ? C81 N64 U3 115.9(9) . . ? N61 C61 C62 124.8(17) . . ? C63 C62 C61 119.2(19) . . ? C62 C63 C64 120.3(17) . . ? C63 C64 C69 116.9(16) . . ? C63 C64 C65 124.8(18) . . ? C69 C64 C65 118.3(19) . . ? C66 C65 C64 119(2) . . ? C65 C66 C67 124(2) . . ? C68 C67 C66 120(2) . . ? C67 C68 N62 124.0(18) . . ? C67 C68 C69 118.5(17) . . ? N62 C68 C69 117.5(15) . . ? N61 C69 C64 120.9(17) . . ? N61 C69 C68 118.9(16) . . ? C64 C69 C68 120.1(16) . . ? N62 C70 C71 129.6(15) . . ? C72 C71 C70 119.9(15) . . ? C72 C71 C82 119.6(16) . . ? C70 C71 C82 120.1(15) . . ? N63 C72 C71 127.7(18) . . ? C81 C73 C74 118.6(16) . . ? C81 C73 N63 117.3(16) . . ? C74 C73 N63 124.2(15) . . ? C73 C74 C75 118.9(16) . . ? C76 C75 C74 122.3(17) . . ? C75 C76 C77 120.7(17) . . ? C76 C77 C78 126.1(18) . . ? C76 C77 C81 118.3(17) . . ? C78 C77 C81 115.5(17) . . ? C79 C78 C77 122.6(17) . . ? C78 C79 C80 116.3(16) . . ? N64 C80 C79 125.0(15) . . ? C73 C81 N64 116.7(15) . . ? C73 C81 C77 121.1(17) . . ? N64 C81 C77 122.0(15) . . ? C87 C82 C83 116.3(17) . . ? C87 C82 C71 123.0(14) . . ? C83 C82 C71 120.5(16) . . ? C84 C83 C82 120.4(19) . . ? C85 C84 C83 124.1(19) . . ? C84 C85 C86 115.7(18) . . ? C84 C85 C88 122.8(19) . . ? C86 C85 C88 121.5(19) . . ? C87 C86 C85 120.9(17) . . ? C82 C87 C86 122.4(16) . . ? C91 N91 C99 117.1(14) . . ? C91 N91 U4 123.1(11) . . ? C99 N91 U4 114.4(11) . . ? C100 N92 C98 116.2(14) . . ? C100 N92 U4 125.7(11) . . ? C98 N92 U4 117.0(10) . . ? C102 N93 C103 115.5(13) . . ? C102 N93 U4 124.8(10) . . ? C103 N93 U4 118.5(10) . . ? C110 N94 C111 117.9(15) . . ? C110 N94 U4 122.6(11) . . ? C111 N94 U4 117.7(11) . . ? N91 C91 C92 124.9(16) . . ? C93 C92 C91 116.9(16) . . ? C92 C93 C94 121.9(15) . . ? C99 C94 C95 119.9(16) . . ? C99 C94 C93 115.2(16) . . ? C95 C94 C93 124.8(15) . . ? C96 C95 C94 118.2(16) . . ? C95 C96 C97 123.0(18) . . ? C96 C97 C98 119.2(17) . . ? C97 C98 C99 119.9(15) . . ? C97 C98 N92 122.6(15) . . ? C99 C98 N92 117.4(14) . . ? N91 C99 C94 123.7(16) . . ? N91 C99 C98 116.5(15) . . ? C94 C99 C98 119.8(16) . . ? N92 C100 C101 128.1(16) . . ? C100 C101 C102 122.1(15) . . ? C100 C101 C112 116.6(14) . . ? C102 C101 C112 120.3(14) . . ? N93 C102 C101 125.9(15) . . ? C104 C103 N93 124.4(16) . . ? C104 C103 C111 117.8(15) . . ? N93 C103 C111 117.8(14) . . ? C103 C104 C105 121.1(18) . . ? C106 C105 C104 119.5(17) . . ? C105 C106 C107 121.0(17) . . ? C111 C107 C106 119.4(18) . . ? C111 C107 C108 117.5(16) . . ? C106 C107 C108 123.1(16) . . ? C109 C108 C107 120.2(16) . . ? C108 C109 C110 117.5(17) . . ? N94 C110 C109 124.3(17) . . ? N94 C111 C107 122.5(17) . . ? N94 C111 C103 116.7(14) . . ? C107 C111 C103 120.6(16) . . ? C117 C112 C113 118.8(17) . . ? C117 C112 C101 120.5(17) . . ? C113 C112 C101 120.4(16) . . ? C114 C113 C112 121.2(18) . . ? C115 C114 C113 121.6(18) . . ? C114 C115 C116 115.7(19) . . ? C114 C115 C118 121(2) . . ? C116 C115 C118 124(2) . . ? C115 C116 C117 123.8(19) . . ? C112 C117 C116 118.8(18) . . ? N121 C121 C122 177(3) . . ? N122 C123 C124 180.000(19) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.369 _refine_diff_density_min -1.593 _refine_diff_density_rms 0.223