Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr M Ephritikhine' _publ_contact_author_address ; Laboratoire de Chimie de coordination Service de Chimie Moleculaire CEA Saclay, Batiment 125 Gif sur Yvette F91191 FRANCE ; _publ_contact_author_phone '33 (1) 69 08 64 36' _publ_contact_author_fax '33 (1) 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_section_title ; Selective complexation of uranium(III) over lanthanide(III) triflates by 2,2':6',2''terpyridine. X-ray crystal structures of [M(OTf)3(terpy)2] and [M(OTf)2(terpy)2(py)][OTf] (M = Nd, Ce, U) and of polynuclear mu-oxo uranium(IV) complexes resulting from hydrolysis ; loop_ _publ_author_name 'M. Ephritikhine' 'Jean-Claude Berthet' 'Charles Madic' 'Yannick Miquel' 'Martine Nierlich' data_1.0.5py _database_code_depnum_ccdc_archive 'CCDC 251214' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H59 Ce2 F18 N15 O18 S6' _chemical_formula_weight 2345.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.465(3) _cell_length_b 15.075(3) _cell_length_c 21.289(4) _cell_angle_alpha 98.38(3) _cell_angle_beta 100.54(3) _cell_angle_gamma 93.18(3) _cell_volume 4499.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 27676 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.252 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.873 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%. A 180\% range in \f was scanned during data collection with 2\%\f steps and 8 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27676 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 24.69 _reflns_number_total 14145 _reflns_number_gt 10206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms. Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. One triflate ion (S3A) was found disordered with two positions for O7A, O9A and F7A, F9A with 0.5 occupations factors ; _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^)+(0.0752P)^2^+34.7053P] 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 14145 _refine_ls_number_parameters 1267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.005 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.320 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.149 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 CeA Ce 0.23903(3) 0.24535(3) 0.47482(2) 0.02066(14) Uani 1 1 d . . . S1A S 0.28514(16) 0.49888(15) 0.51508(11) 0.0288(5) Uani 1 1 d . . . S2A S 0.24012(16) 0.04571(15) 0.56754(11) 0.0263(5) Uani 1 1 d . . . S3A S -0.1801(2) 0.2978(4) 0.23136(17) 0.0945(16) Uani 1 1 d . . . F1A F 0.3967(4) 0.5176(4) 0.6292(3) 0.0465(15) Uani 1 1 d . . . F2A F 0.3811(4) 0.6401(4) 0.5887(3) 0.0464(15) Uani 1 1 d . . . F3A F 0.4674(4) 0.5432(4) 0.5525(3) 0.0476(15) Uani 1 1 d . . . F4A F 0.1899(5) -0.1243(4) 0.5633(3) 0.0547(17) Uani 1 1 d . . . F5A F 0.0796(4) -0.0503(4) 0.5193(3) 0.0547(17) Uani 1 1 d . . . F6A F 0.1936(4) -0.0862(4) 0.4701(3) 0.0459(15) Uani 1 1 d . . . F7A F -0.2431(10) 0.1750(10) 0.2769(8) 0.073(5) Uani 0.50 1 d P . . F8A F -0.1762(5) 0.2777(5) 0.3518(3) 0.072(2) Uani 1 1 d . . . F9A F -0.2314(11) 0.3887(9) 0.3157(6) 0.062(4) Uani 0.50 1 d P . . F10A F -0.3162(5) 0.2736(7) 0.2952(3) 0.092(3) Uani 1 1 d . . . O1A O 0.3077(4) 0.4043(4) 0.5052(3) 0.0297(14) Uani 1 1 d . . . O2A O 0.2846(5) 0.5435(4) 0.4608(3) 0.0429(17) Uani 1 1 d . . . O3A O 0.2074(5) 0.5118(4) 0.5486(3) 0.0394(17) Uani 1 1 d . . . O4A O 0.2087(4) 0.1078(4) 0.5227(3) 0.0291(14) Uani 1 1 d . . . O5A O 0.2104(5) 0.0638(4) 0.6287(3) 0.0359(16) Uani 1 1 d . . . O6A O 0.3356(4) 0.0253(4) 0.5691(3) 0.0391(16) Uani 1 1 d . . . O7A O -0.182(3) 0.1790(13) 0.2205(10) 0.150(14) Uani 0.50 1 d P . . O8A O -0.0901(6) 0.3036(10) 0.2438(5) 0.118(5) Uani 1 1 d . . . O9A O -0.185(2) 0.4111(10) 0.2590(10) 0.107(9) Uani 0.50 1 d P . . O10A O -0.2449(5) 0.2941(6) 0.1785(4) 0.058(2) Uani 1 1 d . . . N2A N 0.1225(5) 0.3515(5) 0.4168(3) 0.0235(16) Uani 1 1 d . . . N3A N 0.0774(5) 0.2690(5) 0.5140(3) 0.0248(16) Uani 1 1 d . . . N4A N 0.4232(5) 0.2353(5) 0.5031(4) 0.0286(17) Uani 1 1 d . . . N5A N 0.3097(5) 0.1043(5) 0.4166(3) 0.0259(16) Uani 1 1 d . . . N6A N 0.1234(5) 0.1306(5) 0.3860(4) 0.0259(17) Uani 1 1 d . . . N1A N 0.2780(5) 0.2990(5) 0.3684(4) 0.0305(18) Uani 1 1 d . . . N7A N 0.2834(5) 0.2913(5) 0.6072(3) 0.0276(17) Uani 1 1 d . . . C1A C 0.3566(7) 0.2753(7) 0.3473(5) 0.037(2) Uani 1 1 d . . . H1AA H 0.3864 0.2272 0.3623 0.045 Uiso 1 1 calc R . . C2A C 0.3948(8) 0.3187(8) 0.3049(5) 0.049(3) Uani 1 1 d . . . H2AB H 0.4491 0.3000 0.2912 0.059 Uiso 1 1 calc R . . C3A C 0.3515(8) 0.3910(8) 0.2824(5) 0.054(3) Uani 1 1 d . . . H3AB H 0.3759 0.4210 0.2530 0.065 Uiso 1 1 calc R . . C4A C 0.2716(7) 0.4176(7) 0.3043(5) 0.043(3) Uani 1 1 d . . . H4AA H 0.2423 0.4670 0.2913 0.051 Uiso 1 1 calc R . . C5A C 0.2363(7) 0.3688(6) 0.3463(4) 0.030(2) Uani 1 1 d . . . C6A C 0.1468(6) 0.3927(6) 0.3684(4) 0.026(2) Uani 1 1 d . . . C7A C 0.0932(7) 0.4558(6) 0.3412(4) 0.031(2) Uani 1 1 d . . . H7AB H 0.1121 0.4839 0.3089 0.038 Uiso 1 1 calc R . . C8A C 0.0109(7) 0.4764(7) 0.3628(5) 0.039(2) Uani 1 1 d . . . H8AB H -0.0271 0.5173 0.3444 0.046 Uiso 1 1 calc R . . C9A C -0.0137(6) 0.4358(6) 0.4117(5) 0.030(2) Uani 1 1 d . . . H9AA H -0.0682 0.4497 0.4271 0.037 Uiso 1 1 calc R . . C10A C 0.0427(6) 0.3739(6) 0.4381(4) 0.026(2) Uani 1 1 d . . . C11A C 0.0176(6) 0.3275(6) 0.4904(4) 0.0247(19) Uani 1 1 d . . . C12A C -0.0650(7) 0.3439(6) 0.5143(5) 0.033(2) Uani 1 1 d . . . H12A H -0.1061 0.3832 0.4968 0.039 Uiso 1 1 calc R . . C13A C -0.0847(7) 0.3015(7) 0.5637(5) 0.035(2) Uani 1 1 d . . . H13A H -0.1383 0.3135 0.5808 0.042 Uiso 1 1 calc R . . C14A C -0.0254(6) 0.2413(6) 0.5880(4) 0.028(2) Uani 1 1 d . . . H14A H -0.0384 0.2107 0.6206 0.034 Uiso 1 1 calc R . . C15A C 0.0551(6) 0.2280(6) 0.5618(4) 0.0245(19) Uani 1 1 d . . . H15A H 0.0961 0.1881 0.5785 0.029 Uiso 1 1 calc R . . C16A C 0.4797(6) 0.3022(6) 0.5435(4) 0.027(2) Uani 1 1 d . . . H16A H 0.4516 0.3511 0.5616 0.033 Uiso 1 1 calc R . . C17A C 0.5757(7) 0.3025(7) 0.5595(5) 0.041(3) Uani 1 1 d . . . H17A H 0.6116 0.3489 0.5889 0.049 Uiso 1 1 calc R . . C18A C 0.6169(7) 0.2328(7) 0.5311(5) 0.042(3) Uani 1 1 d . . . H18A H 0.6823 0.2323 0.5398 0.050 Uiso 1 1 calc R . . C19A C 0.5620(7) 0.1621(7) 0.4892(5) 0.039(2) Uani 1 1 d . . . H19A H 0.5900 0.1141 0.4697 0.046 Uiso 1 1 calc R . . C20A C 0.4652(6) 0.1643(6) 0.4768(4) 0.028(2) Uani 1 1 d . . . C21A C 0.4018(6) 0.0893(6) 0.4342(4) 0.026(2) Uani 1 1 d . . . C22A C 0.4390(6) 0.0081(6) 0.4136(4) 0.029(2) Uani 1 1 d . . . H22A H 0.5022 -0.0006 0.4274 0.034 Uiso 1 1 calc R . . C23A C 0.3791(7) -0.0574(7) 0.3725(5) 0.037(2) Uani 1 1 d . . . H23A H 0.4020 -0.1110 0.3569 0.044 Uiso 1 1 calc R . . C24A C 0.2854(7) -0.0448(7) 0.3541(5) 0.035(2) Uani 1 1 d . . . H24A H 0.2448 -0.0899 0.3264 0.042 Uiso 1 1 calc R . . C25A C 0.2511(6) 0.0370(6) 0.3774(4) 0.027(2) Uani 1 1 d . . . C26A C 0.1503(6) 0.0520(6) 0.3595(4) 0.0244(19) Uani 1 1 d . . . C27A C 0.0862(7) -0.0137(6) 0.3186(5) 0.038(2) Uani 1 1 d . . . H27A H 0.1059 -0.0688 0.3028 0.045 Uiso 1 1 calc R . . C28A C -0.0068(7) 0.0046(7) 0.3021(5) 0.042(3) Uani 1 1 d . . . H28A H -0.0501 -0.0378 0.2741 0.051 Uiso 1 1 calc R . . C29A C -0.0349(6) 0.0847(6) 0.3270(5) 0.033(2) Uani 1 1 d . . . H29A H -0.0974 0.0979 0.3165 0.040 Uiso 1 1 calc R . . C30A C 0.0311(6) 0.1454(6) 0.3679(4) 0.032(2) Uani 1 1 d . . . H30A H 0.0115 0.2002 0.3845 0.038 Uiso 1 1 calc R . . C31A C 0.2423(7) 0.3566(6) 0.6369(4) 0.029(2) Uani 1 1 d . . . H31A H 0.1981 0.3856 0.6117 0.035 Uiso 1 1 calc R . . C32A C 0.2606(7) 0.3846(6) 0.7028(4) 0.034(2) Uani 1 1 d . . . H32A H 0.2284 0.4300 0.7214 0.041 Uiso 1 1 calc R . . C33A C 0.3279(8) 0.3434(7) 0.7405(5) 0.046(3) Uani 1 1 d . . . H33A H 0.3421 0.3604 0.7852 0.055 Uiso 1 1 calc R . . C34A C 0.3738(7) 0.2766(6) 0.7107(5) 0.038(2) Uani 1 1 d . . . H34A H 0.4205 0.2487 0.7349 0.046 Uiso 1 1 calc R . . C35A C 0.3493(7) 0.2519(6) 0.6448(5) 0.035(2) Uani 1 1 d . . . H35A H 0.3796 0.2059 0.6251 0.042 Uiso 1 1 calc R . . C36A C 0.3894(7) 0.5526(7) 0.5754(5) 0.036(2) Uani 1 1 d . . . C37A C 0.1706(7) -0.0588(6) 0.5282(4) 0.030(2) Uani 1 1 d . . . C38A C -0.2276(8) 0.2834(14) 0.2974(7) 0.084(6) Uani 1 1 d . . . CeB Ce 0.25331(3) 0.25371(3) 0.01370(2) 0.02122(14) Uani 1 1 d . . . S1B S -0.01390(16) 0.22279(16) -0.01746(12) 0.0310(5) Uani 1 1 d . . . S2B S 0.46805(16) 0.26020(15) -0.07202(11) 0.0265(5) Uani 1 1 d . . . S3B S 0.17937(19) 0.69741(19) 0.27884(12) 0.0411(6) Uani 1 1 d . . . F1B F -0.1693(4) 0.1366(5) -0.0869(3) 0.065(2) Uani 1 1 d . . . F2B F -0.0466(4) 0.1184(4) -0.1302(3) 0.0507(16) Uani 1 1 d . . . F3B F -0.0641(5) 0.0510(4) -0.0506(3) 0.0551(17) Uani 1 1 d . . . F4B F 0.6408(4) 0.3284(6) -0.0562(3) 0.079(3) Uani 1 1 d . . . F5B F 0.5996(4) 0.3022(5) 0.0314(3) 0.0586(19) Uani 1 1 d . . . F6B F 0.5518(6) 0.4143(5) -0.0117(4) 0.077(2) Uani 1 1 d . . . F7B F 0.2885(9) 0.6099(8) 0.2141(7) 0.155(5) Uani 1 1 d . . . F8B F 0.3247(6) 0.7525(7) 0.2343(4) 0.102(3) Uani 1 1 d . . . F9B F 0.2074(8) 0.6909(7) 0.1610(4) 0.123(4) Uani 1 1 d . . . O1B O 0.0838(4) 0.1988(4) -0.0137(3) 0.0318(15) Uani 1 1 d . . . O2B O -0.0499(5) 0.2218(5) 0.0405(3) 0.0444(18) Uani 1 1 d . . . O3B O -0.0308(5) 0.2990(4) -0.0501(3) 0.0424(17) Uani 1 1 d . . . O4B O 0.3963(4) 0.2791(4) -0.0334(3) 0.0324(15) Uani 1 1 d . . . O5B O 0.4515(5) 0.2942(5) -0.1321(3) 0.0416(17) Uani 1 1 d . . . O6B O 0.4964(6) 0.1708(5) -0.0744(4) 0.056(2) Uani 1 1 d . . . O7B O 0.1422(7) 0.7814(6) 0.2732(7) 0.102(4) Uani 1 1 d . . . O8B O 0.2410(7) 0.7008(12) 0.3372(4) 0.143(6) Uani 1 1 d . . . O9B O 0.1098(6) 0.6242(5) 0.2578(4) 0.063(2) Uani 1 1 d . . . N1B N 0.2016(5) 0.2118(5) 0.1200(3) 0.0262(17) Uani 1 1 d . . . N2B N 0.1584(5) 0.3709(5) 0.0761(3) 0.0245(16) Uani 1 1 d . . . N3B N 0.2342(5) 0.4116(5) -0.0260(4) 0.0274(17) Uani 1 1 d . . . N4B N 0.2508(5) 0.0766(5) -0.0197(4) 0.0282(17) Uani 1 1 d . . . N5B N 0.3940(5) 0.1693(5) 0.0707(3) 0.0230(16) Uani 1 1 d . . . N6B N 0.3832(5) 0.3532(4) 0.1011(4) 0.0276(17) Uani 1 1 d . . . N7B N 0.1975(5) 0.2218(5) -0.1173(3) 0.0286(17) Uani 1 1 d . . . C1B C 0.2174(8) 0.1323(7) 0.1387(5) 0.039(3) Uani 1 1 d . . . H1BA H 0.2595 0.0981 0.1197 0.047 Uiso 1 1 calc R . . C2B C 0.1757(8) 0.0974(7) 0.1840(5) 0.044(3) Uani 1 1 d . . . H2BB H 0.1895 0.0419 0.1958 0.052 Uiso 1 1 calc R . . C3B C 0.1128(7) 0.1482(8) 0.2109(5) 0.044(3) Uani 1 1 d . . . H3BB H 0.0828 0.1266 0.2413 0.053 Uiso 1 1 calc R . . C4B C 0.0938(7) 0.2299(8) 0.1938(5) 0.046(3) Uani 1 1 d . . . H4BA H 0.0511 0.2640 0.2123 0.055 Uiso 1 1 calc R . . C5B C 0.1392(6) 0.2617(6) 0.1479(4) 0.028(2) Uani 1 1 d . . . C6B C 0.1198(6) 0.3492(6) 0.1263(4) 0.028(2) Uani 1 1 d . . . C7B C 0.0646(7) 0.4078(7) 0.1570(5) 0.038(2) Uani 1 1 d . . . H7BB H 0.0407 0.3923 0.1919 0.046 Uiso 1 1 calc R . . C8B C 0.0456(7) 0.4865(7) 0.1367(5) 0.039(2) Uani 1 1 d . . . H8BB H 0.0080 0.5250 0.1570 0.047 Uiso 1 1 calc R . . C9B C 0.0834(7) 0.5095(7) 0.0845(5) 0.037(2) Uani 1 1 d . . . H9BB H 0.0721 0.5639 0.0699 0.045 Uiso 1 1 calc R . . C10B C 0.1385(6) 0.4491(6) 0.0549(4) 0.027(2) Uani 1 1 d . . . C11B C 0.1775(6) 0.4712(6) -0.0011(4) 0.030(2) Uani 1 1 d . . . C12B C 0.1610(7) 0.5515(6) -0.0258(5) 0.033(2) Uani 1 1 d . . . H12B H 0.1246 0.5928 -0.0070 0.040 Uiso 1 1 calc R . . C13B C 0.1988(7) 0.5690(7) -0.0778(5) 0.038(2) Uani 1 1 d . . . H13B H 0.1856 0.6206 -0.0958 0.046 Uiso 1 1 calc R . . C14B C 0.2565(7) 0.5091(6) -0.1031(5) 0.037(2) Uani 1 1 d . . . H14B H 0.2843 0.5201 -0.1377 0.044 Uiso 1 1 calc R . . C15B C 0.2715(6) 0.4332(6) -0.0758(4) 0.031(2) Uani 1 1 d . . . H15B H 0.3106 0.3933 -0.0930 0.037 Uiso 1 1 calc R . . C16B C 0.1778(7) 0.0312(6) -0.0629(5) 0.034(2) Uani 1 1 d . . . H16B H 0.1303 0.0643 -0.0807 0.041 Uiso 1 1 calc R . . C17B C 0.1683(7) -0.0595(7) -0.0824(5) 0.039(2) Uani 1 1 d . . . H17B H 0.1168 -0.0871 -0.1132 0.047 Uiso 1 1 calc R . . C18B C 0.2372(7) -0.1088(7) -0.0550(5) 0.042(3) Uani 1 1 d . . . H18B H 0.2330 -0.1709 -0.0670 0.050 Uiso 1 1 calc R . . C19B C 0.3136(7) -0.0652(7) -0.0092(5) 0.039(2) Uani 1 1 d . . . H19B H 0.3601 -0.0980 0.0103 0.047 Uiso 1 1 calc R . . C20B C 0.3196(6) 0.0299(6) 0.0072(4) 0.028(2) Uani 1 1 d . . . C21B C 0.4007(6) 0.0813(6) 0.0538(4) 0.026(2) Uani 1 1 d . . . C22B C 0.4777(7) 0.0374(7) 0.0773(4) 0.032(2) Uani 1 1 d . . . H22B H 0.4795 -0.0240 0.0641 0.038 Uiso 1 1 calc R . . C23B C 0.5508(7) 0.0857(7) 0.1202(5) 0.038(2) Uani 1 1 d . . . H23B H 0.6031 0.0574 0.1370 0.045 Uiso 1 1 calc R . . C24B C 0.5473(7) 0.1774(6) 0.1388(5) 0.035(2) Uani 1 1 d . . . H24B H 0.5972 0.2115 0.1675 0.042 Uiso 1 1 calc R . . C25B C 0.4669(6) 0.2173(6) 0.1132(4) 0.026(2) Uani 1 1 d . . . C26B C 0.4607(6) 0.3161(6) 0.1318(4) 0.028(2) Uani 1 1 d . . . C27B C 0.5323(7) 0.3669(7) 0.1771(5) 0.038(2) Uani 1 1 d . . . H27B H 0.5819 0.3393 0.1984 0.045 Uiso 1 1 calc R . . C28B C 0.5290(7) 0.4579(7) 0.1900(5) 0.041(2) Uani 1 1 d . . . H28B H 0.5775 0.4928 0.2195 0.049 Uiso 1 1 calc R . . C29B C 0.4543(7) 0.4977(6) 0.1597(4) 0.032(2) Uani 1 1 d . . . H29B H 0.4507 0.5596 0.1674 0.039 Uiso 1 1 calc R . . C30B C 0.3847(7) 0.4414(7) 0.1170(4) 0.035(2) Uani 1 1 d . . . H30B H 0.3333 0.4685 0.0973 0.042 Uiso 1 1 calc R . . C31B C 0.1248(7) 0.2615(7) -0.1455(5) 0.034(2) Uani 1 1 d . . . H31B H 0.0911 0.2965 -0.1195 0.040 Uiso 1 1 calc R . . C32B C 0.0969(7) 0.2530(7) -0.2124(5) 0.042(3) Uani 1 1 d . . . H32B H 0.0473 0.2836 -0.2305 0.050 Uiso 1 1 calc R . . C33B C 0.1436(8) 0.1991(7) -0.2510(5) 0.039(2) Uani 1 1 d . . . H33B H 0.1256 0.1917 -0.2958 0.047 Uiso 1 1 calc R . . C34B C 0.2182(7) 0.1557(7) -0.2225(5) 0.037(2) Uani 1 1 d . . . H34B H 0.2508 0.1183 -0.2478 0.044 Uiso 1 1 calc R . . C35B C 0.2432(7) 0.1688(6) -0.1561(4) 0.032(2) Uani 1 1 d . . . H35B H 0.2937 0.1399 -0.1371 0.039 Uiso 1 1 calc R . . C36B C -0.0775(6) 0.1277(7) -0.0739(5) 0.036(2) Uani 1 1 d . . . C37B C 0.5699(7) 0.3309(8) -0.0240(5) 0.041(3) Uani 1 1 d . . . C38B C 0.2542(11) 0.6891(10) 0.2197(7) 0.070(4) Uani 1 1 d . . . N8 N 0.4952(8) 0.1099(5) 0.2896(4) 0.093(4) Uani 1 1 d G . . C39 C 0.5646(6) 0.0638(9) 0.2986(4) 0.104(6) Uani 1 1 d G . . H39 H 0.6185 0.0896 0.3279 0.125 Uiso 1 1 calc R . . C40 C 0.5654(6) -0.0150(9) 0.2706(5) 0.086(5) Uani 1 1 d G . . H40 H 0.6214 -0.0424 0.2786 0.103 Uiso 1 1 calc R . . C41 C 0.4864(10) -0.0669(5) 0.2267(5) 0.088(6) Uani 1 1 d G . . H41 H 0.4875 -0.1270 0.2093 0.106 Uiso 1 1 calc R . . C42 C 0.3982(6) -0.0111(7) 0.2114(4) 0.076(5) Uani 1 1 d G . . H42 H 0.3423 -0.0316 0.1824 0.091 Uiso 1 1 calc R . . C43 C 0.4189(6) 0.0763(6) 0.2497(4) 0.051(3) Uani 1 1 d G . . H43 H 0.3705 0.1144 0.2452 0.061 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 CeA 0.0195(3) 0.0217(3) 0.0220(3) 0.0056(2) 0.00568(19) 0.0008(2) S1A 0.0282(12) 0.0270(12) 0.0320(13) 0.0072(10) 0.0060(9) 0.0023(10) S2A 0.0254(12) 0.0277(12) 0.0283(12) 0.0069(9) 0.0097(9) 0.0028(10) S3A 0.0343(19) 0.204(5) 0.046(2) 0.038(3) 0.0009(14) -0.013(2) F1A 0.054(4) 0.050(4) 0.034(3) 0.012(3) 0.001(3) -0.001(3) F2A 0.058(4) 0.031(3) 0.046(4) -0.002(3) 0.006(3) -0.001(3) F3A 0.026(3) 0.058(4) 0.057(4) -0.005(3) 0.015(3) -0.008(3) F4A 0.090(5) 0.026(3) 0.052(4) 0.015(3) 0.020(3) -0.003(3) F5A 0.034(4) 0.050(4) 0.075(5) -0.006(3) 0.012(3) -0.010(3) F6A 0.068(4) 0.034(3) 0.039(3) -0.001(3) 0.025(3) -0.004(3) F7A 0.066(10) 0.062(10) 0.080(11) 0.033(8) -0.019(8) -0.027(8) F8A 0.077(5) 0.090(5) 0.042(4) 0.023(4) -0.014(3) -0.003(4) F9A 0.093(11) 0.051(8) 0.051(8) 0.006(6) 0.036(8) 0.029(8) F10A 0.060(5) 0.166(9) 0.049(5) 0.030(5) 0.009(4) -0.024(5) O1A 0.028(3) 0.024(3) 0.036(4) 0.006(3) 0.002(3) 0.004(3) O2A 0.054(5) 0.032(4) 0.042(4) 0.012(3) 0.006(3) -0.005(3) O3A 0.030(4) 0.039(4) 0.054(4) 0.009(3) 0.014(3) 0.015(3) O4A 0.031(4) 0.027(3) 0.036(4) 0.015(3) 0.015(3) 0.002(3) O5A 0.047(4) 0.037(4) 0.026(4) 0.004(3) 0.013(3) 0.002(3) O6A 0.024(4) 0.042(4) 0.053(4) 0.010(3) 0.009(3) 0.013(3) O7A 0.33(4) 0.045(12) 0.049(14) -0.022(10) -0.021(18) 0.093(18) O8A 0.032(5) 0.229(15) 0.080(8) -0.021(8) 0.025(5) -0.010(7) O9A 0.23(3) 0.008(8) 0.071(14) 0.002(8) 0.004(15) -0.018(11) O10A 0.043(5) 0.092(6) 0.042(5) 0.022(4) 0.010(4) -0.009(4) N2A 0.015(4) 0.030(4) 0.025(4) 0.003(3) 0.005(3) 0.002(3) N3A 0.018(4) 0.034(4) 0.023(4) 0.004(3) 0.002(3) 0.006(3) N4A 0.025(4) 0.030(4) 0.035(5) 0.007(3) 0.014(3) 0.005(3) N5A 0.026(4) 0.030(4) 0.024(4) 0.008(3) 0.009(3) 0.004(3) N6A 0.028(4) 0.019(4) 0.037(4) 0.010(3) 0.016(3) 0.007(3) N1A 0.028(4) 0.036(5) 0.032(4) 0.009(4) 0.015(3) 0.000(4) N7A 0.034(4) 0.028(4) 0.019(4) 0.002(3) 0.002(3) -0.007(3) C1A 0.051(7) 0.035(6) 0.035(6) 0.023(5) 0.017(5) 0.012(5) C2A 0.049(7) 0.057(7) 0.053(7) 0.016(6) 0.033(6) 0.020(6) C3A 0.059(8) 0.068(8) 0.053(7) 0.032(6) 0.039(6) 0.016(6) C4A 0.044(6) 0.045(6) 0.051(7) 0.028(5) 0.023(5) 0.015(5) C5A 0.040(6) 0.025(5) 0.025(5) 0.009(4) 0.005(4) 0.001(4) C6A 0.029(5) 0.026(5) 0.022(5) 0.000(4) 0.004(4) 0.000(4) C7A 0.035(6) 0.028(5) 0.030(5) 0.011(4) -0.001(4) -0.001(4) C8A 0.034(6) 0.037(6) 0.045(6) 0.010(5) 0.002(5) 0.009(5) C9A 0.027(5) 0.028(5) 0.042(6) 0.016(4) 0.011(4) 0.011(4) C10A 0.018(5) 0.031(5) 0.029(5) 0.001(4) 0.004(4) 0.000(4) C11A 0.017(4) 0.031(5) 0.023(5) 0.000(4) 0.000(3) 0.002(4) C12A 0.028(5) 0.033(5) 0.037(6) 0.009(4) 0.003(4) 0.007(4) C13A 0.027(5) 0.044(6) 0.040(6) 0.009(5) 0.017(4) 0.004(5) C14A 0.028(5) 0.033(5) 0.028(5) 0.009(4) 0.012(4) -0.006(4) C15A 0.028(5) 0.023(5) 0.024(5) 0.008(4) 0.007(4) -0.007(4) C16A 0.029(5) 0.018(4) 0.034(5) 0.001(4) 0.007(4) -0.002(4) C17A 0.025(5) 0.044(6) 0.050(7) 0.013(5) -0.006(4) -0.008(5) C18A 0.019(5) 0.047(6) 0.062(7) 0.013(5) 0.009(5) 0.006(5) C19A 0.031(6) 0.038(6) 0.051(7) 0.012(5) 0.009(5) 0.012(5) C20A 0.031(5) 0.026(5) 0.034(5) 0.016(4) 0.014(4) 0.010(4) C21A 0.020(5) 0.036(5) 0.027(5) 0.010(4) 0.014(4) 0.009(4) C22A 0.024(5) 0.037(5) 0.030(5) 0.008(4) 0.014(4) 0.009(4) C23A 0.044(6) 0.035(6) 0.037(6) 0.006(4) 0.020(5) 0.012(5) C24A 0.031(6) 0.037(6) 0.036(6) 0.001(4) 0.008(4) 0.005(4) C25A 0.038(5) 0.025(5) 0.020(5) 0.007(4) 0.007(4) -0.001(4) C26A 0.028(5) 0.029(5) 0.020(5) 0.007(4) 0.009(4) 0.002(4) C27A 0.045(6) 0.021(5) 0.042(6) -0.004(4) 0.002(5) -0.001(4) C28A 0.038(6) 0.026(5) 0.056(7) 0.002(5) -0.003(5) -0.011(5) C29A 0.021(5) 0.035(6) 0.042(6) 0.006(4) 0.007(4) -0.009(4) C30A 0.026(5) 0.035(5) 0.035(6) 0.002(4) 0.008(4) 0.003(4) C31A 0.040(6) 0.025(5) 0.024(5) 0.006(4) 0.010(4) -0.004(4) C32A 0.039(6) 0.032(5) 0.031(6) 0.003(4) 0.005(4) -0.005(4) C33A 0.074(8) 0.035(6) 0.021(5) 0.007(5) 0.000(5) -0.021(6) C34A 0.049(6) 0.027(5) 0.036(6) 0.017(5) -0.005(5) -0.004(5) C35A 0.043(6) 0.023(5) 0.035(6) 0.006(4) 0.000(4) -0.004(4) C36A 0.036(6) 0.035(6) 0.036(6) 0.003(4) 0.007(4) -0.005(5) C37A 0.035(6) 0.028(5) 0.033(5) 0.008(4) 0.020(4) -0.002(4) C38A 0.018(6) 0.183(19) 0.061(9) 0.049(10) 0.008(6) 0.020(8) CeB 0.0215(3) 0.0214(3) 0.0221(3) 0.0054(2) 0.00657(19) 0.0002(2) S1B 0.0269(13) 0.0303(13) 0.0360(14) 0.0027(10) 0.0093(10) 0.0011(10) S2B 0.0266(12) 0.0276(12) 0.0272(12) 0.0072(9) 0.0084(9) 0.0026(10) S3B 0.0366(15) 0.0497(16) 0.0352(15) 0.0017(12) 0.0051(11) 0.0061(12) F1B 0.037(4) 0.085(5) 0.062(5) -0.007(4) -0.001(3) -0.018(3) F2B 0.049(4) 0.059(4) 0.038(4) -0.006(3) 0.012(3) -0.012(3) F3B 0.070(5) 0.033(3) 0.059(4) 0.007(3) 0.011(3) -0.017(3) F4B 0.033(4) 0.160(8) 0.048(4) 0.032(5) 0.011(3) -0.018(4) F5B 0.044(4) 0.092(5) 0.037(4) 0.024(3) -0.003(3) -0.016(4) F6B 0.087(6) 0.049(4) 0.081(6) 0.008(4) -0.008(4) -0.025(4) F7B 0.162(11) 0.121(9) 0.222(14) 0.008(9) 0.141(11) 0.057(8) F8B 0.091(6) 0.123(8) 0.093(6) -0.011(5) 0.057(5) -0.053(6) F9B 0.174(10) 0.138(9) 0.053(6) 0.018(6) 0.030(6) -0.071(8) O1B 0.018(3) 0.031(4) 0.043(4) 0.005(3) -0.001(3) -0.002(3) O2B 0.041(4) 0.053(5) 0.041(4) 0.000(3) 0.024(3) -0.006(4) O3B 0.039(4) 0.037(4) 0.050(4) 0.005(3) 0.004(3) 0.011(3) O4B 0.026(3) 0.045(4) 0.031(4) 0.011(3) 0.014(3) 0.004(3) O5B 0.044(4) 0.056(5) 0.028(4) 0.015(3) 0.008(3) 0.002(4) O6B 0.072(6) 0.031(4) 0.069(5) 0.008(4) 0.019(4) 0.025(4) O7B 0.061(6) 0.043(5) 0.197(13) -0.018(6) 0.041(7) 0.000(5) O8B 0.050(6) 0.35(2) 0.036(6) 0.046(9) 0.009(4) 0.011(9) O9B 0.083(6) 0.052(5) 0.056(5) 0.002(4) 0.030(4) -0.013(5) N1B 0.024(4) 0.033(4) 0.026(4) 0.012(3) 0.013(3) 0.002(3) N2B 0.027(4) 0.023(4) 0.020(4) -0.003(3) 0.004(3) -0.004(3) N3B 0.029(4) 0.022(4) 0.031(4) 0.003(3) 0.005(3) 0.006(3) N4B 0.032(4) 0.023(4) 0.032(4) 0.006(3) 0.011(3) 0.001(3) N5B 0.027(4) 0.031(4) 0.017(4) 0.010(3) 0.013(3) 0.006(3) N6B 0.036(5) 0.010(4) 0.037(5) -0.002(3) 0.016(3) -0.007(3) N7B 0.028(4) 0.033(4) 0.026(4) 0.008(3) 0.009(3) -0.009(3) C1B 0.054(7) 0.036(6) 0.040(6) 0.021(5) 0.027(5) 0.019(5) C2B 0.049(7) 0.043(6) 0.047(7) 0.022(5) 0.017(5) 0.015(5) C3B 0.043(6) 0.059(7) 0.041(6) 0.024(5) 0.020(5) 0.015(6) C4B 0.037(6) 0.066(8) 0.047(7) 0.023(6) 0.024(5) 0.015(6) C5B 0.027(5) 0.030(5) 0.030(5) 0.009(4) 0.008(4) -0.001(4) C6B 0.027(5) 0.030(5) 0.026(5) -0.001(4) 0.007(4) -0.001(4) C7B 0.038(6) 0.046(6) 0.029(6) -0.002(5) 0.010(4) 0.007(5) C8B 0.033(6) 0.039(6) 0.044(6) -0.003(5) 0.011(4) 0.010(5) C9B 0.040(6) 0.035(6) 0.038(6) 0.005(5) 0.010(4) 0.004(5) C10B 0.022(5) 0.022(5) 0.031(5) -0.003(4) -0.002(4) 0.005(4) C11B 0.030(5) 0.028(5) 0.030(5) 0.008(4) 0.002(4) -0.006(4) C12B 0.032(5) 0.024(5) 0.047(6) 0.008(4) 0.014(4) 0.010(4) C13B 0.039(6) 0.030(5) 0.046(6) 0.017(5) -0.002(5) 0.010(5) C14B 0.045(6) 0.030(5) 0.039(6) 0.018(4) 0.008(5) 0.002(5) C15B 0.027(5) 0.034(5) 0.031(5) 0.005(4) 0.008(4) -0.002(4) C16B 0.033(6) 0.033(5) 0.040(6) 0.008(4) 0.012(4) 0.004(4) C17B 0.038(6) 0.035(6) 0.045(6) -0.002(5) 0.018(5) 0.003(5) C18B 0.038(6) 0.030(6) 0.055(7) -0.009(5) 0.015(5) -0.005(5) C19B 0.044(6) 0.034(6) 0.048(6) 0.012(5) 0.022(5) 0.014(5) C20B 0.025(5) 0.029(5) 0.041(6) 0.014(4) 0.021(4) 0.006(4) C21B 0.034(5) 0.026(5) 0.026(5) 0.010(4) 0.018(4) 0.005(4) C22B 0.034(6) 0.034(5) 0.034(6) 0.009(4) 0.017(4) 0.009(4) C23B 0.039(6) 0.041(6) 0.038(6) 0.017(5) 0.011(5) 0.011(5) C24B 0.033(6) 0.035(6) 0.034(6) 0.010(4) 0.000(4) -0.007(4) C25B 0.033(5) 0.029(5) 0.018(5) 0.009(4) 0.012(4) -0.002(4) C26B 0.023(5) 0.036(5) 0.028(5) 0.011(4) 0.010(4) 0.000(4) C27B 0.028(5) 0.041(6) 0.038(6) 0.005(5) -0.006(4) -0.003(5) C28B 0.033(6) 0.040(6) 0.046(7) 0.000(5) 0.008(5) -0.005(5) C29B 0.038(6) 0.029(5) 0.032(5) 0.003(4) 0.015(4) -0.003(4) C30B 0.032(5) 0.047(6) 0.025(5) 0.006(4) 0.006(4) -0.007(5) C31B 0.028(5) 0.037(6) 0.039(6) 0.018(5) 0.005(4) -0.001(4) C32B 0.040(6) 0.041(6) 0.040(6) 0.012(5) -0.004(5) -0.009(5) C33B 0.051(7) 0.040(6) 0.025(5) 0.007(5) 0.008(5) -0.013(5) C34B 0.038(6) 0.037(6) 0.032(6) -0.003(4) 0.012(4) -0.010(5) C35B 0.029(5) 0.035(5) 0.034(6) 0.004(4) 0.010(4) -0.003(4) C36B 0.021(5) 0.048(6) 0.037(6) 0.005(5) 0.005(4) -0.003(4) C37B 0.035(6) 0.056(7) 0.036(6) 0.020(5) 0.010(4) 0.004(5) C38B 0.094(11) 0.063(9) 0.061(10) 0.006(7) 0.041(8) -0.008(8) N8 0.095(11) 0.114(11) 0.080(9) 0.056(8) 0.010(8) -0.001(9) C39 0.087(14) 0.140(19) 0.104(14) 0.052(14) 0.039(11) 0.012(13) C40 0.084(12) 0.132(15) 0.064(11) 0.040(10) 0.041(9) 0.058(12) C41 0.174(18) 0.049(8) 0.063(10) 0.017(7) 0.071(11) 0.008(10) C42 0.067(9) 0.112(12) 0.044(8) 0.007(8) 0.017(6) -0.040(9) C43 0.043(7) 0.071(8) 0.042(7) 0.014(6) 0.008(5) 0.017(6) _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 CeA O1A 2.489(6) . ? CeA O4A 2.492(6) . ? CeA N6A 2.634(8) . ? CeA N4A 2.640(7) . ? CeA N3A 2.647(7) . ? CeA N2A 2.653(7) . ? CeA N5A 2.653(7) . ? CeA N1A 2.656(7) . ? CeA N7A 2.749(7) . ? S1A O2A 1.418(7) . ? S1A O3A 1.445(7) . ? S1A O1A 1.474(6) . ? S1A C36A 1.852(10) . ? S2A O6A 1.427(6) . ? S2A O5A 1.438(6) . ? S2A O4A 1.464(6) . ? S2A C37A 1.824(9) . ? S3A O8A 1.276(9) . ? S3A O10A 1.319(8) . ? S3A C38A 1.709(13) . ? S3A O9A 1.734(16) . ? S3A O7A 1.770(19) . ? F1A C36A 1.320(11) . ? F2A C36A 1.324(11) . ? F3A C36A 1.316(11) . ? F4A C37A 1.333(10) . ? F5A C37A 1.312(11) . ? F6A C37A 1.352(10) . ? F7A O7A 1.62(3) . ? F7A C38A 1.62(2) . ? F8A C38A 1.274(13) . ? F9A O9A 1.55(3) . ? F9A C38A 1.58(2) . ? F10A C38A 1.273(13) . ? N2A C10A 1.358(11) . ? N2A C6A 1.367(11) . ? N3A C15A 1.343(10) . ? N3A C11A 1.354(11) . ? N4A C16A 1.350(11) . ? N4A C20A 1.360(11) . ? N5A C21A 1.357(11) . ? N5A C25A 1.358(11) . ? N6A C26A 1.344(11) . ? N6A C30A 1.361(11) . ? N1A C5A 1.342(11) . ? N1A C1A 1.345(12) . ? N7A C31A 1.320(12) . ? N7A C35A 1.351(12) . ? C1A C2A 1.366(14) . ? C2A C3A 1.389(15) . ? C3A C4A 1.382(14) . ? C4A C5A 1.385(13) . ? C5A C6A 1.500(13) . ? C6A C7A 1.386(12) . ? C7A C8A 1.388(14) . ? C8A C9A 1.373(13) . ? C9A C10A 1.387(12) . ? C10A C11A 1.484(12) . ? C11A C12A 1.403(13) . ? C12A C13A 1.372(13) . ? C13A C14A 1.375(13) . ? C14A C15A 1.391(12) . ? C16A C17A 1.368(13) . ? C17A C18A 1.356(15) . ? C18A C19A 1.391(14) . ? C19A C20A 1.380(13) . ? C20A C21A 1.491(13) . ? C21A C22A 1.408(12) . ? C22A C23A 1.367(13) . ? C23A C24A 1.372(13) . ? C24A C25A 1.412(13) . ? C25A C26A 1.477(12) . ? C26A C27A 1.396(12) . ? C27A C28A 1.381(14) . ? C28A C29A 1.361(14) . ? C29A C30A 1.368(12) . ? C31A C32A 1.376(13) . ? C32A C33A 1.380(14) . ? C33A C34A 1.377(15) . ? C34A C35A 1.372(14) . ? CeB O1B 2.480(6) . ? CeB O4B 2.493(6) . ? CeB N6B 2.615(7) . ? CeB N2B 2.649(7) . ? CeB N3B 2.652(7) . ? CeB N4B 2.657(7) . ? CeB N1B 2.657(7) . ? CeB N5B 2.659(7) . ? CeB N7B 2.721(7) . ? S1B O2B 1.426(7) . ? S1B O3B 1.437(7) . ? S1B O1B 1.469(6) . ? S1B C36B 1.815(10) . ? S2B O6B 1.426(7) . ? S2B O5B 1.431(7) . ? S2B O4B 1.452(6) . ? S2B C37B 1.819(11) . ? S3B O8B 1.382(9) . ? S3B O9B 1.414(8) . ? S3B O7B 1.415(10) . ? S3B C38B 1.799(13) . ? F1B C36B 1.324(11) . ? F2B C36B 1.345(11) . ? F3B C36B 1.333(12) . ? F4B C37B 1.333(12) . ? F5B C37B 1.323(11) . ? F6B C37B 1.298(13) . ? F7B C38B 1.317(17) . ? F8B C38B 1.319(15) . ? F9B C38B 1.315(17) . ? N1B C1B 1.334(11) . ? N1B C5B 1.370(11) . ? N2B C10B 1.351(11) . ? N2B C6B 1.364(11) . ? N3B C15B 1.347(11) . ? N3B C11B 1.364(12) . ? N4B C20B 1.341(11) . ? N4B C16B 1.345(12) . ? N5B C21B 1.336(11) . ? N5B C25B 1.353(11) . ? N6B C30B 1.321(12) . ? N6B C26B 1.380(12) . ? N7B C31B 1.330(12) . ? N7B C35B 1.350(12) . ? C1B C2B 1.378(13) . ? C2B C3B 1.371(14) . ? C3B C4B 1.364(15) . ? C4B C5B 1.397(13) . ? C5B C6B 1.484(13) . ? C6B C7B 1.394(13) . ? C7B C8B 1.347(14) . ? C8B C9B 1.403(14) . ? C9B C10B 1.401(13) . ? C10B C11B 1.479(13) . ? C11B C12B 1.405(12) . ? C12B C13B 1.373(14) . ? C13B C14B 1.382(14) . ? C14B C15B 1.367(13) . ? C16B C17B 1.362(13) . ? C17B C18B 1.371(15) . ? C18B C19B 1.394(14) . ? C19B C20B 1.420(13) . ? C20B C21B 1.488(13) . ? C21B C22B 1.379(13) . ? C22B C23B 1.361(14) . ? C23B C24B 1.387(14) . ? C24B C25B 1.397(13) . ? C25B C26B 1.497(13) . ? C26B C27B 1.386(12) . ? C27B C28B 1.364(14) . ? C28B C29B 1.369(14) . ? C29B C30B 1.381(13) . ? C31B C32B 1.392(13) . ? C32B C33B 1.363(15) . ? C33B C34B 1.384(15) . ? C34B C35B 1.377(13) . ? N8 C39 1.2535 . ? N8 C43 1.2911 . ? C39 C40 1.2499 . ? C40 C41 1.4446 . ? C41 C42 1.5774 . ? C42 C43 1.4303 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A CeA O4A 141.7(2) . . ? O1A CeA N6A 144.7(2) . . ? O4A CeA N6A 72.2(2) . . ? O1A CeA N4A 75.0(2) . . ? O4A CeA N4A 91.6(2) . . ? N6A CeA N4A 123.9(2) . . ? O1A CeA N3A 97.3(2) . . ? O4A CeA N3A 76.2(2) . . ? N6A CeA N3A 79.4(2) . . ? N4A CeA N3A 149.4(2) . . ? O1A CeA N2A 70.5(2) . . ? O4A CeA N2A 131.6(2) . . ? N6A CeA N2A 77.2(2) . . ? N4A CeA N2A 136.8(2) . . ? N3A CeA N2A 61.8(2) . . ? O1A CeA N5A 129.1(2) . . ? O4A CeA N5A 68.5(2) . . ? N6A CeA N5A 61.9(2) . . ? N4A CeA N5A 62.1(2) . . ? N3A CeA N5A 133.6(2) . . ? N2A CeA N5A 125.9(2) . . ? O1A CeA N1A 72.7(2) . . ? O4A CeA N1A 142.3(2) . . ? N6A CeA N1A 79.9(2) . . ? N4A CeA N1A 83.3(2) . . ? N3A CeA N1A 123.3(2) . . ? N2A CeA N1A 62.3(2) . . ? N5A CeA N1A 76.2(2) . . ? O1A CeA N7A 69.8(2) . . ? O4A CeA N7A 72.2(2) . . ? N6A CeA N7A 139.3(2) . . ? N4A CeA N7A 75.9(2) . . ? N3A CeA N7A 73.6(2) . . ? N2A CeA N7A 114.0(2) . . ? N5A CeA N7A 120.1(2) . . ? N1A CeA N7A 140.6(2) . . ? O2A S1A O3A 116.6(4) . . ? O2A S1A O1A 115.0(4) . . ? O3A S1A O1A 112.5(4) . . ? O2A S1A C36A 104.9(4) . . ? O3A S1A C36A 103.8(4) . . ? O1A S1A C36A 101.7(4) . . ? O6A S2A O5A 117.0(4) . . ? O6A S2A O4A 113.4(4) . . ? O5A S2A O4A 114.4(4) . . ? O6A S2A C37A 104.2(4) . . ? O5A S2A C37A 103.3(4) . . ? O4A S2A C37A 102.0(4) . . ? O8A S3A O10A 134.7(7) . . ? O8A S3A C38A 112.5(7) . . ? O10A S3A C38A 112.6(5) . . ? O8A S3A O9A 93.1(12) . . ? O10A S3A O9A 95.8(9) . . ? C38A S3A O9A 83.6(10) . . ? O8A S3A O7A 89.9(13) . . ? O10A S3A O7A 91.1(9) . . ? C38A S3A O7A 83.3(12) . . ? O9A S3A O7A 166.8(12) . . ? O7A F7A C38A 91.1(11) . . ? O9A F9A C38A 94.1(10) . . ? S1A O1A CeA 144.5(4) . . ? S2A O4A CeA 150.1(4) . . ? F7A O7A S3A 90.9(11) . . ? F9A O9A S3A 91.2(9) . . ? C10A N2A C6A 117.8(7) . . ? C10A N2A CeA 121.7(6) . . ? C6A N2A CeA 120.1(5) . . ? C15A N3A C11A 117.4(7) . . ? C15A N3A CeA 120.7(6) . . ? C11A N3A CeA 121.7(6) . . ? C16A N4A C20A 117.4(8) . . ? C16A N4A CeA 120.7(6) . . ? C20A N4A CeA 121.8(6) . . ? C21A N5A C25A 117.8(8) . . ? C21A N5A CeA 121.0(6) . . ? C25A N5A CeA 120.1(6) . . ? C26A N6A C30A 116.5(8) . . ? C26A N6A CeA 122.2(6) . . ? C30A N6A CeA 121.1(6) . . ? C5A N1A C1A 117.6(8) . . ? C5A N1A CeA 119.8(6) . . ? C1A N1A CeA 119.9(6) . . ? C31A N7A C35A 116.6(8) . . ? C31A N7A CeA 120.4(6) . . ? C35A N7A CeA 123.0(6) . . ? N1A C1A C2A 123.0(9) . . ? C1A C2A C3A 119.1(10) . . ? C4A C3A C2A 119.0(9) . . ? C3A C4A C5A 118.3(9) . . ? N1A C5A C4A 123.1(9) . . ? N1A C5A C6A 117.2(8) . . ? C4A C5A C6A 119.7(8) . . ? N2A C6A C7A 122.3(8) . . ? N2A C6A C5A 117.2(7) . . ? C7A C6A C5A 120.5(8) . . ? C6A C7A C8A 118.9(9) . . ? C9A C8A C7A 119.3(9) . . ? C8A C9A C10A 119.9(9) . . ? N2A C10A C9A 121.8(8) . . ? N2A C10A C11A 116.7(8) . . ? C9A C10A C11A 121.5(8) . . ? N3A C11A C12A 121.4(8) . . ? N3A C11A C10A 117.6(7) . . ? C12A C11A C10A 121.0(8) . . ? C13A C12A C11A 119.4(9) . . ? C12A C13A C14A 120.0(9) . . ? C13A C14A C15A 117.4(8) . . ? N3A C15A C14A 124.3(8) . . ? N4A C16A C17A 124.0(9) . . ? C18A C17A C16A 117.9(10) . . ? C17A C18A C19A 120.3(9) . . ? C20A C19A C18A 118.9(9) . . ? N4A C20A C19A 121.3(9) . . ? N4A C20A C21A 116.9(8) . . ? C19A C20A C21A 121.8(8) . . ? N5A C21A C22A 123.3(8) . . ? N5A C21A C20A 117.0(8) . . ? C22A C21A C20A 119.7(8) . . ? C23A C22A C21A 117.7(8) . . ? C22A C23A C24A 120.6(9) . . ? C23A C24A C25A 119.5(9) . . ? N5A C25A C24A 121.1(8) . . ? N5A C25A C26A 118.0(8) . . ? C24A C25A C26A 120.9(8) . . ? N6A C26A C27A 122.1(8) . . ? N6A C26A C25A 116.7(8) . . ? C27A C26A C25A 121.2(8) . . ? C28A C27A C26A 118.9(9) . . ? C29A C28A C27A 119.8(9) . . ? C28A C29A C30A 118.3(9) . . ? N6A C30A C29A 124.2(9) . . ? N7A C31A C32A 124.4(9) . . ? C31A C32A C33A 118.1(10) . . ? C34A C33A C32A 118.8(10) . . ? C35A C34A C33A 118.8(9) . . ? N7A C35A C34A 123.1(10) . . ? F3A C36A F1A 109.2(8) . . ? F3A C36A F2A 107.2(8) . . ? F1A C36A F2A 109.2(8) . . ? F3A C36A S1A 111.1(7) . . ? F1A C36A S1A 110.7(7) . . ? F2A C36A S1A 109.4(7) . . ? F5A C37A F4A 108.7(7) . . ? F5A C37A F6A 108.4(8) . . ? F4A C37A F6A 106.6(7) . . ? F5A C37A S2A 112.3(6) . . ? F4A C37A S2A 110.5(7) . . ? F6A C37A S2A 110.1(6) . . ? F10A C38A F8A 115.3(11) . . ? F10A C38A F9A 88.9(12) . . ? F8A C38A F9A 92.7(13) . . ? F10A C38A F7A 81.5(12) . . ? F8A C38A F7A 92.5(12) . . ? F9A C38A F7A 170.3(11) . . ? F10A C38A S3A 122.7(9) . . ? F8A C38A S3A 121.9(9) . . ? F9A C38A S3A 91.0(10) . . ? F7A C38A S3A 93.2(11) . . ? O1B CeB O4B 143.6(2) . . ? O1B CeB N6B 144.1(2) . . ? O4B CeB N6B 70.9(2) . . ? O1B CeB N2B 71.7(2) . . ? O4B CeB N2B 129.9(2) . . ? N6B CeB N2B 75.7(2) . . ? O1B CeB N3B 96.9(2) . . ? O4B CeB N3B 76.1(2) . . ? N6B CeB N3B 80.2(2) . . ? N2B CeB N3B 62.2(2) . . ? O1B CeB N4B 74.9(2) . . ? O4B CeB N4B 91.4(2) . . ? N6B CeB N4B 124.9(2) . . ? N2B CeB N4B 138.6(2) . . ? N3B CeB N4B 146.9(2) . . ? O1B CeB N1B 71.7(2) . . ? O4B CeB N1B 141.5(2) . . ? N6B CeB N1B 80.6(2) . . ? N2B CeB N1B 62.7(2) . . ? N3B CeB N1B 124.4(2) . . ? N4B CeB N1B 84.1(2) . . ? O1B CeB N5B 126.5(2) . . ? O4B CeB N5B 70.0(2) . . ? N6B CeB N5B 63.5(2) . . ? N2B CeB N5B 124.4(2) . . ? N3B CeB N5B 136.4(2) . . ? N4B CeB N5B 61.5(2) . . ? N1B CeB N5B 74.4(2) . . ? O1B CeB N7B 71.1(2) . . ? O4B CeB N7B 72.8(2) . . ? N6B CeB N7B 138.6(2) . . ? N2B CeB N7B 115.4(2) . . ? N3B CeB N7B 72.4(2) . . ? N4B CeB N7B 74.6(2) . . ? N1B CeB N7B 140.7(2) . . ? N5B CeB N7B 120.2(2) . . ? O2B S1B O3B 117.1(4) . . ? O2B S1B O1B 115.0(4) . . ? O3B S1B O1B 111.7(4) . . ? O2B S1B C36B 105.1(4) . . ? O3B S1B C36B 104.7(4) . . ? O1B S1B C36B 101.0(4) . . ? O6B S2B O5B 116.4(5) . . ? O6B S2B O4B 114.0(5) . . ? O5B S2B O4B 113.8(4) . . ? O6B S2B C37B 104.6(5) . . ? O5B S2B C37B 104.0(4) . . ? O4B S2B C37B 101.9(4) . . ? O8B S3B O9B 119.0(8) . . ? O8B S3B O7B 111.3(9) . . ? O9B S3B O7B 112.5(6) . . ? O8B S3B C38B 104.2(7) . . ? O9B S3B C38B 105.6(6) . . ? O7B S3B C38B 102.2(7) . . ? S1B O1B CeB 146.3(4) . . ? S2B O4B CeB 158.9(4) . . ? C1B N1B C5B 117.3(7) . . ? C1B N1B CeB 121.2(6) . . ? C5B N1B CeB 119.7(5) . . ? C10B N2B C6B 118.2(7) . . ? C10B N2B CeB 120.9(5) . . ? C6B N2B CeB 120.5(6) . . ? C15B N3B C11B 116.6(8) . . ? C15B N3B CeB 122.0(6) . . ? C11B N3B CeB 121.0(6) . . ? C20B N4B C16B 118.4(8) . . ? C20B N4B CeB 121.6(6) . . ? C16B N4B CeB 120.0(6) . . ? C21B N5B C25B 117.8(8) . . ? C21B N5B CeB 122.1(6) . . ? C25B N5B CeB 119.8(5) . . ? C30B N6B C26B 114.4(8) . . ? C30B N6B CeB 124.7(6) . . ? C26B N6B CeB 120.8(5) . . ? C31B N7B C35B 117.6(8) . . ? C31B N7B CeB 120.0(6) . . ? C35B N7B CeB 122.3(6) . . ? N1B C1B C2B 124.7(9) . . ? C3B C2B C1B 117.0(10) . . ? C4B C3B C2B 121.1(10) . . ? C3B C4B C5B 119.0(10) . . ? N1B C5B C4B 120.9(9) . . ? N1B C5B C6B 117.6(7) . . ? C4B C5B C6B 121.4(9) . . ? N2B C6B C7B 121.2(9) . . ? N2B C6B C5B 117.9(8) . . ? C7B C6B C5B 120.9(8) . . ? C8B C7B C6B 121.0(9) . . ? C7B C8B C9B 118.8(9) . . ? C10B C9B C8B 118.7(9) . . ? N2B C10B C9B 122.0(9) . . ? N2B C10B C11B 118.3(8) . . ? C9B C10B C11B 119.6(8) . . ? N3B C11B C12B 121.1(8) . . ? N3B C11B C10B 116.9(8) . . ? C12B C11B C10B 121.9(8) . . ? C13B C12B C11B 119.7(9) . . ? C12B C13B C14B 119.3(9) . . ? C15B C14B C13B 117.9(9) . . ? N3B C15B C14B 125.2(9) . . ? N4B C16B C17B 125.0(10) . . ? C16B C17B C18B 117.7(10) . . ? C17B C18B C19B 119.7(9) . . ? C18B C19B C20B 119.1(10) . . ? N4B C20B C19B 120.1(9) . . ? N4B C20B C21B 117.7(8) . . ? C19B C20B C21B 122.2(8) . . ? N5B C21B C22B 123.6(9) . . ? N5B C21B C20B 116.8(8) . . ? C22B C21B C20B 119.6(8) . . ? C23B C22B C21B 118.5(9) . . ? C22B C23B C24B 120.0(9) . . ? C23B C24B C25B 118.3(9) . . ? N5B C25B C24B 121.8(8) . . ? N5B C25B C26B 118.2(8) . . ? C24B C25B C26B 120.0(8) . . ? N6B C26B C27B 122.6(9) . . ? N6B C26B C25B 117.5(8) . . ? C27B C26B C25B 119.9(8) . . ? C28B C27B C26B 119.2(9) . . ? C27B C28B C29B 120.0(10) . . ? C28B C29B C30B 116.7(9) . . ? N6B C30B C29B 127.0(10) . . ? N7B C31B C32B 122.8(10) . . ? C33B C32B C31B 119.0(10) . . ? C32B C33B C34B 119.1(9) . . ? C35B C34B C33B 118.8(9) . . ? N7B C35B C34B 122.7(9) . . ? F1B C36B F3B 108.5(8) . . ? F1B C36B F2B 107.8(8) . . ? F3B C36B F2B 106.4(8) . . ? F1B C36B S1B 111.8(7) . . ? F3B C36B S1B 111.0(6) . . ? F2B C36B S1B 111.1(6) . . ? F6B C37B F5B 108.6(9) . . ? F6B C37B F4B 107.7(9) . . ? F5B C37B F4B 107.4(8) . . ? F6B C37B S2B 112.0(7) . . ? F5B C37B S2B 111.2(7) . . ? F4B C37B S2B 109.7(8) . . ? F9B C38B F7B 102.8(12) . . ? F9B C38B F8B 109.3(11) . . ? F7B C38B F8B 109.0(14) . . ? F9B C38B S3B 112.5(12) . . ? F7B C38B S3B 110.5(10) . . ? F8B C38B S3B 112.2(9) . . ? C39 N8 C43 120.1 . . ? C40 C39 N8 123.7 . . ? C39 C40 C41 125.4 . . ? C40 C41 C42 113.0 . . ? C43 C42 C41 108.4 . . ? N8 C43 C42 129.2 . . ? #===END data_2.0.5py _database_code_depnum_ccdc_archive 'CCDC 251215' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H59 F18 N15 Nd2 O18 S6' _chemical_formula_weight 2353.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 14.441(3) _cell_length_b 15.030(3) _cell_length_c 21.304(4) _cell_angle_alpha 98.51(3) _cell_angle_beta 100.52(3) _cell_angle_gamma 93.23(3) _cell_volume 4479.5(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 27546 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.400 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 8 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27546 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 24.69 _reflns_number_total 13981 _reflns_number_gt 10651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. One triflate ion (S3A) was found disordered with two positions for O7A, O9A and F7A, F9A with 0.5 occupations factors ; _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^+27.6408P] 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 13981 _refine_ls_number_parameters 1267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.832 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.129 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 NdA Nd 0.23974(3) 0.24543(3) 0.474987(17) 0.01913(11) Uani 1 1 d . . . S1A S 0.28419(13) 0.49871(13) 0.51505(9) 0.0265(4) Uani 1 1 d . . . S2A S 0.24078(13) 0.04573(13) 0.56672(9) 0.0243(4) Uani 1 1 d . . . S3A S -0.18104(19) 0.2979(3) 0.23090(14) 0.0946(14) Uani 1 1 d . . . F1A F 0.3955(3) 0.5194(3) 0.6293(2) 0.0417(12) Uani 1 1 d . . . F2A F 0.3797(4) 0.6415(3) 0.5879(2) 0.0447(12) Uani 1 1 d . . . F3A F 0.4663(3) 0.5427(3) 0.5523(2) 0.0423(12) Uani 1 1 d . . . F4A F 0.1894(4) -0.1244(3) 0.5622(2) 0.0515(14) Uani 1 1 d . . . F5A F 0.0790(3) -0.0494(4) 0.5186(3) 0.0530(14) Uani 1 1 d . . . F6A F 0.1924(4) -0.0866(3) 0.4694(2) 0.0446(12) Uani 1 1 d . . . F7A F -0.2446(10) 0.1736(9) 0.2737(7) 0.081(4) Uani 0.50 1 d P . . F8A F -0.1760(4) 0.2788(4) 0.3514(3) 0.0697(18) Uani 1 1 d . . . F9A F -0.2291(10) 0.3910(8) 0.3144(6) 0.069(4) Uani 0.50 1 d P . . F10A F -0.3168(5) 0.2762(6) 0.2952(3) 0.091(3) Uani 1 1 d . . . O1A O 0.3062(4) 0.4043(3) 0.5060(2) 0.0259(11) Uani 1 1 d . . . O2A O 0.2837(4) 0.5413(4) 0.4597(3) 0.0408(15) Uani 1 1 d . . . O3A O 0.2062(4) 0.5126(4) 0.5481(3) 0.0364(13) Uani 1 1 d . . . O4A O 0.2098(4) 0.1094(3) 0.5223(2) 0.0258(11) Uani 1 1 d . . . O5A O 0.2113(4) 0.0653(4) 0.6279(2) 0.0320(12) Uani 1 1 d . . . O6A O 0.3367(4) 0.0255(4) 0.5678(3) 0.0389(14) Uani 1 1 d . . . O7A O -0.182(2) 0.1788(11) 0.2204(8) 0.156(13) Uani 0.50 1 d P . . O8A O -0.0902(5) 0.3023(9) 0.2422(4) 0.115(4) Uani 1 1 d . . . O9A O -0.1854(14) 0.4124(8) 0.2599(8) 0.081(6) Uani 0.50 1 d P . . O10A O -0.2470(4) 0.2952(5) 0.1777(3) 0.0540(18) Uani 1 1 d . . . N2A N 0.1252(4) 0.3499(4) 0.4172(3) 0.0208(13) Uani 1 1 d . . . N3A N 0.0806(4) 0.2687(4) 0.5153(3) 0.0240(13) Uani 1 1 d . . . N4A N 0.4227(4) 0.2376(4) 0.5039(3) 0.0257(14) Uani 1 1 d . . . N5A N 0.3101(4) 0.1056(4) 0.4178(3) 0.0231(13) Uani 1 1 d . . . N6A N 0.1239(4) 0.1330(4) 0.3865(3) 0.0240(13) Uani 1 1 d . . . N1A N 0.2817(4) 0.2981(4) 0.3708(3) 0.0265(14) Uani 1 1 d . . . N7A N 0.2852(4) 0.2900(4) 0.6058(3) 0.0243(14) Uani 1 1 d . . . C1A C 0.3604(6) 0.2747(6) 0.3493(4) 0.0328(19) Uani 1 1 d . . . H1AA H 0.3907 0.2273 0.3649 0.039 Uiso 1 1 calc R . . C2A C 0.3985(6) 0.3164(6) 0.3057(4) 0.040(2) Uani 1 1 d . . . H2AB H 0.4526 0.2974 0.2918 0.048 Uiso 1 1 calc R . . C3A C 0.3541(7) 0.3875(7) 0.2832(4) 0.047(2) Uani 1 1 d . . . H3AB H 0.3790 0.4181 0.2543 0.057 Uiso 1 1 calc R . . C4A C 0.2734(6) 0.4132(6) 0.3033(4) 0.040(2) Uani 1 1 d . . . H4AA H 0.2425 0.4606 0.2880 0.048 Uiso 1 1 calc R . . C5A C 0.2386(6) 0.3667(5) 0.3470(3) 0.0281(17) Uani 1 1 d . . . C6A C 0.1489(5) 0.3909(5) 0.3695(3) 0.0246(16) Uani 1 1 d . . . C7A C 0.0950(5) 0.4538(5) 0.3412(4) 0.0298(18) Uani 1 1 d . . . H7AB H 0.1136 0.4813 0.3087 0.036 Uiso 1 1 calc R . . C8A C 0.0133(6) 0.4737(5) 0.3630(4) 0.0320(18) Uani 1 1 d . . . H8AB H -0.0248 0.5146 0.3446 0.038 Uiso 1 1 calc R . . C9A C -0.0122(6) 0.4334(5) 0.4120(4) 0.0319(18) Uani 1 1 d . . . H9AA H -0.0672 0.4470 0.4270 0.038 Uiso 1 1 calc R . . C10A C 0.0455(5) 0.3721(5) 0.4391(3) 0.0215(15) Uani 1 1 d . . . C11A C 0.0203(5) 0.3271(5) 0.4919(3) 0.0219(15) Uani 1 1 d . . . C12A C -0.0621(5) 0.3437(5) 0.5150(4) 0.0287(17) Uani 1 1 d . . . H12A H -0.1030 0.3829 0.4971 0.034 Uiso 1 1 calc R . . C13A C -0.0825(5) 0.3012(5) 0.5650(4) 0.0317(18) Uani 1 1 d . . . H13A H -0.1367 0.3126 0.5816 0.038 Uiso 1 1 calc R . . C14A C -0.0221(5) 0.2422(5) 0.5895(4) 0.0291(18) Uani 1 1 d . . . H14A H -0.0342 0.2135 0.6233 0.035 Uiso 1 1 calc R . . C15A C 0.0576(5) 0.2259(5) 0.5630(3) 0.0221(16) Uani 1 1 d . . . H15A H 0.0970 0.1839 0.5786 0.026 Uiso 1 1 calc R . . C16A C 0.4782(5) 0.3056(5) 0.5443(4) 0.0311(18) Uani 1 1 d . . . H16A H 0.4493 0.3547 0.5616 0.037 Uiso 1 1 calc R . . C17A C 0.5750(6) 0.3066(6) 0.5614(4) 0.0341(19) Uani 1 1 d . . . H17A H 0.6104 0.3537 0.5908 0.041 Uiso 1 1 calc R . . C18A C 0.6174(6) 0.2360(6) 0.5336(4) 0.038(2) Uani 1 1 d . . . H18A H 0.6828 0.2356 0.5428 0.046 Uiso 1 1 calc R . . C19A C 0.5626(6) 0.1649(6) 0.4917(4) 0.0346(19) Uani 1 1 d . . . H19A H 0.5910 0.1164 0.4729 0.042 Uiso 1 1 calc R . . C20A C 0.4650(5) 0.1670(5) 0.4783(4) 0.0260(17) Uani 1 1 d . . . C21A C 0.4023(5) 0.0921(5) 0.4355(3) 0.0249(16) Uani 1 1 d . . . C22A C 0.4390(6) 0.0117(5) 0.4144(4) 0.0314(18) Uani 1 1 d . . . H22A H 0.5026 0.0040 0.4277 0.038 Uiso 1 1 calc R . . C23A C 0.3799(6) -0.0564(6) 0.3736(4) 0.0351(19) Uani 1 1 d . . . H23A H 0.4030 -0.1106 0.3589 0.042 Uiso 1 1 calc R . . C24A C 0.2866(6) -0.0428(6) 0.3551(4) 0.0347(19) Uani 1 1 d . . . H24A H 0.2458 -0.0878 0.3272 0.042 Uiso 1 1 calc R . . C25A C 0.2527(5) 0.0375(5) 0.3778(3) 0.0211(15) Uani 1 1 d . . . C26A C 0.1510(6) 0.0532(5) 0.3603(3) 0.0268(17) Uani 1 1 d . . . C27A C 0.0859(6) -0.0118(5) 0.3186(4) 0.037(2) Uani 1 1 d . . . H27A H 0.1056 -0.0667 0.3019 0.044 Uiso 1 1 calc R . . C28A C -0.0064(6) 0.0053(6) 0.3024(4) 0.044(2) Uani 1 1 d . . . H28A H -0.0492 -0.0373 0.2739 0.052 Uiso 1 1 calc R . . C29A C -0.0363(5) 0.0852(5) 0.3281(4) 0.0307(18) Uani 1 1 d . . . H29A H -0.0991 0.0977 0.3183 0.037 Uiso 1 1 calc R . . C30A C 0.0308(5) 0.1459(5) 0.3689(4) 0.0285(17) Uani 1 1 d . . . H30A H 0.0109 0.2005 0.3860 0.034 Uiso 1 1 calc R . . C31A C 0.2437(6) 0.3554(5) 0.6361(4) 0.0305(18) Uani 1 1 d . . . H31A H 0.1994 0.3849 0.6111 0.037 Uiso 1 1 calc R . . C32A C 0.2624(6) 0.3829(5) 0.7029(4) 0.0334(19) Uani 1 1 d . . . H32A H 0.2306 0.4285 0.7219 0.040 Uiso 1 1 calc R . . C33A C 0.3280(7) 0.3414(5) 0.7397(4) 0.039(2) Uani 1 1 d . . . H33A H 0.3420 0.3581 0.7844 0.047 Uiso 1 1 calc R . . C34A C 0.3734(6) 0.2747(6) 0.7101(4) 0.037(2) Uani 1 1 d . . . H34A H 0.4191 0.2459 0.7344 0.045 Uiso 1 1 calc R . . C35A C 0.3507(6) 0.2505(5) 0.6435(4) 0.0332(19) Uani 1 1 d . . . H35A H 0.3819 0.2049 0.6240 0.040 Uiso 1 1 calc R . . C36A C 0.3874(6) 0.5543(6) 0.5743(4) 0.0339(19) Uani 1 1 d . . . C37A C 0.1710(6) -0.0584(5) 0.5274(4) 0.0315(18) Uani 1 1 d . . . C38A C -0.2284(7) 0.2847(12) 0.2966(5) 0.088(5) Uani 1 1 d . . . NdB Nd 0.25280(3) 0.25364(3) 0.013976(17) 0.01958(11) Uani 1 1 d . . . S1B S -0.01323(13) 0.22433(13) -0.01638(9) 0.0285(4) Uani 1 1 d . . . S2B S 0.46713(13) 0.25849(13) -0.07081(9) 0.0247(4) Uani 1 1 d . . . S3B S 0.17865(16) 0.69582(16) 0.27853(10) 0.0402(5) Uani 1 1 d . . . F1B F -0.1700(3) 0.1370(4) -0.0848(3) 0.0580(15) Uani 1 1 d . . . F2B F -0.0497(4) 0.1201(3) -0.1297(2) 0.0475(13) Uani 1 1 d . . . F3B F -0.0641(4) 0.0514(3) -0.0504(2) 0.0518(14) Uani 1 1 d . . . F4B F 0.6397(4) 0.3287(5) -0.0556(3) 0.073(2) Uani 1 1 d . . . F5B F 0.5999(3) 0.3017(4) 0.0329(2) 0.0550(15) Uani 1 1 d . . . F6B F 0.5504(5) 0.4136(4) -0.0113(3) 0.075(2) Uani 1 1 d . . . F7B F 0.2850(8) 0.6093(7) 0.2114(6) 0.155(5) Uani 1 1 d . . . F8B F 0.3247(6) 0.7499(6) 0.2354(4) 0.108(3) Uani 1 1 d . . . F9B F 0.2046(7) 0.6918(7) 0.1610(3) 0.129(4) Uani 1 1 d . . . O1B O 0.0844(3) 0.2005(3) -0.0133(2) 0.0283(12) Uani 1 1 d . . . O2B O -0.0484(4) 0.2219(4) 0.0421(3) 0.0431(15) Uani 1 1 d . . . O3B O -0.0321(4) 0.3002(4) -0.0487(3) 0.0413(14) Uani 1 1 d . . . O4B O 0.3947(3) 0.2775(4) -0.0323(2) 0.0296(12) Uani 1 1 d . . . O5B O 0.4500(4) 0.2918(4) -0.1311(2) 0.0353(13) Uani 1 1 d . . . O6B O 0.4946(5) 0.1688(4) -0.0723(3) 0.0488(16) Uani 1 1 d . . . O7B O 0.1415(6) 0.7805(5) 0.2763(6) 0.118(4) Uani 1 1 d . . . O8B O 0.2402(6) 0.6949(11) 0.3364(4) 0.158(6) Uani 1 1 d . . . O9B O 0.1075(6) 0.6228(5) 0.2570(3) 0.065(2) Uani 1 1 d . . . N1B N 0.2008(4) 0.2111(4) 0.1180(3) 0.0259(14) Uani 1 1 d . . . N2B N 0.1590(4) 0.3702(4) 0.0757(3) 0.0221(13) Uani 1 1 d . . . N3B N 0.2351(4) 0.4091(4) -0.0266(3) 0.0244(14) Uani 1 1 d . . . N4B N 0.2472(4) 0.0788(4) -0.0205(3) 0.0279(14) Uani 1 1 d . . . N5B N 0.3910(4) 0.1703(4) 0.0701(3) 0.0230(13) Uani 1 1 d . . . N6B N 0.3811(4) 0.3542(4) 0.1011(3) 0.0242(14) Uani 1 1 d . . . N7B N 0.1983(4) 0.2216(4) -0.1153(3) 0.0271(14) Uani 1 1 d . . . C1B C 0.2161(6) 0.1304(6) 0.1377(4) 0.0348(19) Uani 1 1 d . . . H1BA H 0.2577 0.0956 0.1185 0.042 Uiso 1 1 calc R . . C2B C 0.1764(6) 0.0960(6) 0.1827(4) 0.040(2) Uani 1 1 d . . . H2BB H 0.1896 0.0397 0.1935 0.048 Uiso 1 1 calc R . . C3B C 0.1152(7) 0.1479(7) 0.2118(4) 0.047(2) Uani 1 1 d . . . H3BB H 0.0861 0.1271 0.2430 0.056 Uiso 1 1 calc R . . C4B C 0.0977(6) 0.2301(6) 0.1942(4) 0.037(2) Uani 1 1 d . . . H4BA H 0.0563 0.2653 0.2133 0.045 Uiso 1 1 calc R . . C5B C 0.1418(5) 0.2612(5) 0.1480(3) 0.0256(16) Uani 1 1 d . . . C6B C 0.1217(5) 0.3484(5) 0.1257(3) 0.0241(16) Uani 1 1 d . . . C7B C 0.0656(6) 0.4055(6) 0.1561(4) 0.0343(19) Uani 1 1 d . . . H7BB H 0.0410 0.3893 0.1906 0.041 Uiso 1 1 calc R . . C8B C 0.0462(6) 0.4862(6) 0.1352(4) 0.037(2) Uani 1 1 d . . . H8BB H 0.0088 0.5250 0.1555 0.045 Uiso 1 1 calc R . . C9B C 0.0829(5) 0.5081(5) 0.0839(4) 0.0319(18) Uani 1 1 d . . . H9BB H 0.0706 0.5620 0.0688 0.038 Uiso 1 1 calc R . . C10B C 0.1388(5) 0.4485(5) 0.0546(3) 0.0272(17) Uani 1 1 d . . . C11B C 0.1794(5) 0.4694(5) -0.0011(4) 0.0265(17) Uani 1 1 d . . . C12B C 0.1616(6) 0.5490(5) -0.0268(4) 0.0335(19) Uani 1 1 d . . . H12B H 0.1240 0.5899 -0.0088 0.040 Uiso 1 1 calc R . . C13B C 0.2001(6) 0.5660(5) -0.0789(4) 0.038(2) Uani 1 1 d . . . H13B H 0.1875 0.6178 -0.0969 0.046 Uiso 1 1 calc R . . C14B C 0.2572(6) 0.5058(5) -0.1040(4) 0.0310(18) Uani 1 1 d . . . H14B H 0.2845 0.5163 -0.1388 0.037 Uiso 1 1 calc R . . C15B C 0.2731(5) 0.4298(5) -0.0765(3) 0.0269(17) Uani 1 1 d . . . H15B H 0.3125 0.3898 -0.0934 0.032 Uiso 1 1 calc R . . C16B C 0.1743(6) 0.0335(5) -0.0637(4) 0.0308(18) Uani 1 1 d . . . H16B H 0.1266 0.0668 -0.0813 0.037 Uiso 1 1 calc R . . C17B C 0.1648(6) -0.0586(6) -0.0841(4) 0.038(2) Uani 1 1 d . . . H17B H 0.1131 -0.0868 -0.1147 0.045 Uiso 1 1 calc R . . C18B C 0.2368(6) -0.1075(6) -0.0565(4) 0.041(2) Uani 1 1 d . . . H18B H 0.2336 -0.1698 -0.0683 0.049 Uiso 1 1 calc R . . C19B C 0.3121(6) -0.0630(5) -0.0121(4) 0.0334(19) Uani 1 1 d . . . H19B H 0.3601 -0.0952 0.0064 0.040 Uiso 1 1 calc R . . C20B C 0.3167(5) 0.0307(5) 0.0053(4) 0.0255(16) Uani 1 1 d . . . C21B C 0.3975(5) 0.0818(5) 0.0521(3) 0.0256(17) Uani 1 1 d . . . C22B C 0.4747(6) 0.0390(5) 0.0767(4) 0.0300(18) Uani 1 1 d . . . H22B H 0.4765 -0.0226 0.0633 0.036 Uiso 1 1 calc R . . C23B C 0.5495(6) 0.0865(6) 0.1212(4) 0.038(2) Uani 1 1 d . . . H23B H 0.6012 0.0575 0.1383 0.045 Uiso 1 1 calc R . . C24B C 0.5452(6) 0.1777(6) 0.1395(4) 0.0345(19) Uani 1 1 d . . . H24B H 0.5947 0.2117 0.1689 0.041 Uiso 1 1 calc R . . C25B C 0.4651(5) 0.2187(5) 0.1132(3) 0.0237(16) Uani 1 1 d . . . C26B C 0.4595(5) 0.3175(5) 0.1320(3) 0.0237(16) Uani 1 1 d . . . C27B C 0.5313(6) 0.3691(6) 0.1758(4) 0.036(2) Uani 1 1 d . . . H27B H 0.5824 0.3419 0.1958 0.044 Uiso 1 1 calc R . . C28B C 0.5276(6) 0.4608(6) 0.1900(4) 0.040(2) Uani 1 1 d . . . H28B H 0.5757 0.4961 0.2199 0.048 Uiso 1 1 calc R . . C29B C 0.4517(5) 0.4998(5) 0.1593(4) 0.0294(18) Uani 1 1 d . . . H29B H 0.4477 0.5618 0.1671 0.035 Uiso 1 1 calc R . . C30B C 0.3814(6) 0.4430(6) 0.1165(4) 0.0311(18) Uani 1 1 d . . . H30B H 0.3298 0.4697 0.0967 0.037 Uiso 1 1 calc R . . C31B C 0.1253(6) 0.2611(6) -0.1443(4) 0.0326(19) Uani 1 1 d . . . H31B H 0.0913 0.2961 -0.1184 0.039 Uiso 1 1 calc R . . C32B C 0.0977(6) 0.2527(6) -0.2106(4) 0.035(2) Uani 1 1 d . . . H32B H 0.0476 0.2829 -0.2287 0.042 Uiso 1 1 calc R . . C33B C 0.1460(6) 0.1988(6) -0.2494(4) 0.041(2) Uani 1 1 d . . . H33B H 0.1293 0.1924 -0.2942 0.049 Uiso 1 1 calc R . . C34B C 0.2189(6) 0.1547(6) -0.2210(4) 0.036(2) Uani 1 1 d . . . H34B H 0.2512 0.1165 -0.2462 0.044 Uiso 1 1 calc R . . C35B C 0.2435(5) 0.1679(5) -0.1542(4) 0.0292(18) Uani 1 1 d . . . H35B H 0.2936 0.1385 -0.1352 0.035 Uiso 1 1 calc R . . C36B C -0.0786(6) 0.1294(6) -0.0729(4) 0.037(2) Uani 1 1 d . . . C37B C 0.5696(6) 0.3306(7) -0.0232(4) 0.040(2) Uani 1 1 d . . . C38B C 0.2516(9) 0.6895(9) 0.2185(6) 0.067(3) Uani 1 1 d . . . N8 N 0.4945(6) 0.1095(4) 0.2904(3) 0.087(3) Uani 1 1 d G . . C39 C 0.5648(5) 0.0647(7) 0.3002(4) 0.092(4) Uani 1 1 d G . . H39 H 0.6181 0.0917 0.3297 0.110 Uiso 1 1 calc R . . C40 C 0.5672(5) -0.0140(7) 0.2727(4) 0.080(4) Uani 1 1 d G . . H40 H 0.6239 -0.0405 0.2813 0.096 Uiso 1 1 calc R . . C41 C 0.4894(8) -0.0675(4) 0.2288(4) 0.085(5) Uani 1 1 d G . . H41 H 0.4916 -0.1278 0.2117 0.102 Uiso 1 1 calc R . . C42 C 0.4001(5) -0.0134(5) 0.2125(3) 0.079(4) Uani 1 1 d G . . H42 H 0.3447 -0.0351 0.1832 0.094 Uiso 1 1 calc R . . C43 C 0.4190(5) 0.0745(5) 0.2503(3) 0.051(3) Uani 1 1 d G . . H43 H 0.3698 0.1118 0.2452 0.061 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 NdA 0.0185(2) 0.0210(2) 0.0180(2) 0.00392(15) 0.00294(15) 0.00263(17) S1A 0.0260(10) 0.0238(10) 0.0285(10) 0.0047(8) 0.0014(8) 0.0024(8) S2A 0.0260(10) 0.0250(10) 0.0230(9) 0.0056(7) 0.0051(7) 0.0040(8) S3A 0.0347(15) 0.208(5) 0.0413(16) 0.039(2) -0.0017(12) -0.011(2) F1A 0.047(3) 0.049(3) 0.027(2) 0.011(2) 0.001(2) -0.001(3) F2A 0.056(3) 0.030(3) 0.044(3) 0.001(2) 0.003(2) 0.000(2) F3A 0.027(2) 0.050(3) 0.045(3) -0.006(2) 0.010(2) -0.007(2) F4A 0.082(4) 0.028(3) 0.047(3) 0.016(2) 0.014(3) -0.003(3) F5A 0.033(3) 0.050(3) 0.070(4) -0.001(3) 0.007(3) -0.010(3) F6A 0.067(3) 0.031(3) 0.036(3) -0.001(2) 0.018(2) -0.002(3) F7A 0.086(10) 0.057(8) 0.092(11) 0.030(7) -0.011(8) -0.020(8) F8A 0.077(4) 0.087(4) 0.038(3) 0.020(3) -0.015(3) -0.003(4) F9A 0.104(10) 0.050(7) 0.063(8) 0.004(6) 0.041(7) 0.035(7) F10A 0.059(4) 0.170(8) 0.042(3) 0.020(4) 0.011(3) -0.025(5) O1A 0.031(3) 0.021(3) 0.025(3) 0.003(2) 0.000(2) 0.005(2) O2A 0.056(4) 0.032(3) 0.032(3) 0.014(2) -0.002(3) -0.004(3) O3A 0.025(3) 0.037(3) 0.049(4) 0.007(3) 0.010(3) 0.015(3) O4A 0.035(3) 0.022(3) 0.024(3) 0.009(2) 0.010(2) 0.007(2) O5A 0.042(3) 0.034(3) 0.023(3) 0.005(2) 0.014(2) 0.005(3) O6A 0.024(3) 0.039(3) 0.055(4) 0.009(3) 0.009(3) 0.011(3) O7A 0.35(4) 0.045(10) 0.053(11) -0.027(8) -0.025(16) 0.109(16) O8A 0.029(4) 0.234(13) 0.072(6) -0.011(7) 0.019(4) -0.005(6) O9A 0.145(16) 0.010(6) 0.072(11) -0.002(6) -0.008(10) -0.012(8) O10A 0.044(4) 0.085(5) 0.037(4) 0.020(3) 0.012(3) 0.000(4) N2A 0.021(3) 0.022(3) 0.018(3) 0.002(2) 0.002(2) 0.004(3) N3A 0.018(3) 0.028(3) 0.025(3) 0.005(3) 0.002(2) 0.001(3) N4A 0.022(3) 0.027(3) 0.030(3) 0.007(3) 0.005(3) 0.006(3) N5A 0.027(3) 0.023(3) 0.023(3) 0.010(3) 0.009(3) 0.005(3) N6A 0.022(3) 0.022(3) 0.030(3) 0.007(3) 0.007(3) 0.009(3) N1A 0.030(3) 0.028(3) 0.023(3) 0.004(3) 0.008(3) 0.006(3) N7A 0.026(3) 0.025(3) 0.021(3) 0.003(3) 0.004(3) -0.001(3) C1A 0.039(5) 0.036(5) 0.030(4) 0.016(4) 0.014(4) 0.009(4) C2A 0.037(5) 0.049(5) 0.042(5) 0.012(4) 0.020(4) 0.013(4) C3A 0.052(6) 0.058(6) 0.045(5) 0.028(5) 0.026(5) 0.010(5) C4A 0.044(5) 0.044(5) 0.042(5) 0.027(4) 0.014(4) 0.011(4) C5A 0.036(4) 0.026(4) 0.024(4) 0.008(3) 0.008(3) -0.001(4) C6A 0.024(4) 0.024(4) 0.022(4) -0.001(3) 0.000(3) 0.002(3) C7A 0.035(4) 0.028(4) 0.024(4) 0.011(3) -0.006(3) 0.005(4) C8A 0.028(4) 0.027(4) 0.041(5) 0.010(4) 0.002(4) 0.006(4) C9A 0.025(4) 0.032(4) 0.041(5) 0.010(4) 0.006(3) 0.010(4) C10A 0.020(4) 0.020(4) 0.023(4) -0.001(3) 0.002(3) 0.005(3) C11A 0.016(4) 0.016(4) 0.033(4) 0.003(3) 0.004(3) 0.004(3) C12A 0.023(4) 0.032(4) 0.031(4) 0.003(3) 0.005(3) 0.005(4) C13A 0.025(4) 0.038(5) 0.036(5) 0.007(4) 0.013(3) 0.010(4) C14A 0.026(4) 0.035(4) 0.026(4) 0.006(3) 0.007(3) -0.004(4) C15A 0.025(4) 0.025(4) 0.017(3) 0.004(3) 0.005(3) 0.001(3) C16A 0.024(4) 0.021(4) 0.046(5) 0.006(3) 0.000(4) 0.002(4) C17A 0.026(4) 0.036(5) 0.039(5) 0.012(4) 0.000(4) -0.002(4) C18A 0.020(4) 0.042(5) 0.052(5) 0.007(4) 0.005(4) 0.006(4) C19A 0.027(4) 0.034(5) 0.046(5) 0.013(4) 0.008(4) 0.013(4) C20A 0.023(4) 0.025(4) 0.033(4) 0.009(3) 0.008(3) 0.003(3) C21A 0.030(4) 0.025(4) 0.022(4) 0.005(3) 0.007(3) 0.011(3) C22A 0.026(4) 0.036(5) 0.033(4) 0.006(4) 0.006(3) 0.013(4) C23A 0.036(5) 0.031(5) 0.044(5) 0.007(4) 0.017(4) 0.020(4) C24A 0.037(5) 0.032(4) 0.034(4) -0.004(4) 0.011(4) 0.011(4) C25A 0.028(4) 0.020(4) 0.018(3) 0.006(3) 0.008(3) 0.004(3) C26A 0.036(4) 0.028(4) 0.018(4) 0.008(3) 0.008(3) -0.001(4) C27A 0.042(5) 0.019(4) 0.042(5) -0.009(3) 0.000(4) -0.001(4) C28A 0.035(5) 0.034(5) 0.053(6) 0.005(4) -0.009(4) -0.009(4) C29A 0.020(4) 0.033(5) 0.036(4) 0.005(4) -0.001(3) 0.001(4) C30A 0.021(4) 0.033(4) 0.031(4) 0.002(3) 0.003(3) 0.008(4) C31A 0.039(5) 0.028(4) 0.024(4) 0.009(3) 0.003(3) -0.007(4) C32A 0.045(5) 0.029(4) 0.026(4) 0.002(3) 0.009(4) 0.002(4) C33A 0.065(6) 0.028(4) 0.019(4) 0.004(3) -0.003(4) -0.010(5) C34A 0.041(5) 0.034(5) 0.028(4) 0.007(4) -0.014(4) -0.010(4) C35A 0.040(5) 0.025(4) 0.032(4) 0.007(3) -0.002(4) 0.001(4) C36A 0.037(5) 0.033(5) 0.032(4) 0.000(4) 0.011(4) 0.002(4) C37A 0.044(5) 0.027(4) 0.025(4) 0.008(3) 0.010(4) 0.002(4) C38A 0.035(6) 0.197(17) 0.046(7) 0.056(9) 0.004(5) 0.036(8) NdB 0.0216(2) 0.0197(2) 0.0178(2) 0.00356(15) 0.00418(15) 0.00261(17) S1B 0.0234(10) 0.0283(10) 0.0324(10) 0.0005(8) 0.0058(8) 0.0001(9) S2B 0.0256(10) 0.0260(10) 0.0241(9) 0.0064(7) 0.0065(7) 0.0046(8) S3B 0.0349(12) 0.0507(14) 0.0316(11) 0.0000(10) 0.0021(9) 0.0074(11) F1B 0.032(3) 0.080(4) 0.052(3) -0.006(3) 0.000(2) -0.009(3) F2B 0.052(3) 0.053(3) 0.033(3) -0.003(2) 0.007(2) -0.008(3) F3B 0.065(4) 0.035(3) 0.051(3) 0.004(2) 0.007(3) -0.012(3) F4B 0.031(3) 0.146(6) 0.046(3) 0.029(4) 0.011(2) -0.018(4) F5B 0.040(3) 0.087(4) 0.036(3) 0.025(3) -0.005(2) -0.011(3) F6B 0.085(5) 0.040(3) 0.085(5) 0.001(3) -0.010(4) -0.019(3) F7B 0.153(9) 0.117(8) 0.225(12) -0.001(8) 0.128(9) 0.053(7) F8B 0.097(6) 0.132(7) 0.090(6) -0.017(5) 0.053(5) -0.051(6) F9B 0.182(9) 0.153(8) 0.046(4) 0.026(5) 0.019(5) -0.065(7) O1B 0.019(3) 0.032(3) 0.034(3) 0.005(2) 0.005(2) 0.003(2) O2B 0.038(3) 0.055(4) 0.036(3) -0.004(3) 0.018(3) -0.007(3) O3B 0.039(3) 0.034(3) 0.052(4) 0.010(3) 0.005(3) 0.011(3) O4B 0.024(3) 0.042(3) 0.027(3) 0.013(2) 0.009(2) 0.003(3) O5B 0.036(3) 0.051(4) 0.023(3) 0.017(3) 0.006(2) 0.006(3) O6B 0.066(4) 0.025(3) 0.059(4) 0.007(3) 0.016(3) 0.023(3) O7B 0.072(6) 0.037(4) 0.234(13) -0.034(6) 0.045(7) 0.005(4) O8B 0.051(5) 0.38(2) 0.048(5) 0.062(8) -0.001(4) 0.010(8) O9B 0.084(5) 0.049(4) 0.060(5) 0.002(3) 0.022(4) -0.010(4) N1B 0.026(3) 0.026(3) 0.026(3) 0.006(3) 0.005(3) -0.001(3) N2B 0.024(3) 0.022(3) 0.017(3) -0.002(2) 0.002(2) -0.002(3) N3B 0.027(3) 0.019(3) 0.027(3) 0.005(3) 0.004(3) 0.002(3) N4B 0.032(4) 0.016(3) 0.039(4) 0.007(3) 0.013(3) 0.003(3) N5B 0.029(3) 0.021(3) 0.022(3) 0.008(2) 0.008(3) 0.003(3) N6B 0.029(3) 0.019(3) 0.025(3) 0.001(3) 0.011(3) 0.001(3) N7B 0.026(3) 0.030(4) 0.026(3) 0.008(3) 0.007(3) -0.002(3) C1B 0.042(5) 0.035(5) 0.032(4) 0.009(4) 0.014(4) 0.013(4) C2B 0.043(5) 0.049(5) 0.041(5) 0.019(4) 0.023(4) 0.017(5) C3B 0.051(6) 0.063(6) 0.035(5) 0.025(5) 0.018(4) 0.015(5) C4B 0.040(5) 0.050(5) 0.025(4) 0.008(4) 0.011(4) 0.011(4) C5B 0.020(4) 0.030(4) 0.027(4) 0.003(3) 0.006(3) 0.004(3) C6B 0.024(4) 0.025(4) 0.023(4) 0.002(3) 0.003(3) 0.001(3) C7B 0.033(5) 0.043(5) 0.027(4) 0.004(4) 0.008(3) 0.004(4) C8B 0.040(5) 0.034(5) 0.036(5) -0.008(4) 0.012(4) 0.015(4) C9B 0.029(4) 0.023(4) 0.039(5) -0.003(3) 0.003(4) 0.006(4) C10B 0.031(4) 0.023(4) 0.025(4) 0.002(3) 0.000(3) 0.001(4) C11B 0.026(4) 0.021(4) 0.030(4) 0.006(3) 0.000(3) -0.001(3) C12B 0.032(4) 0.027(4) 0.042(5) 0.009(4) 0.003(4) 0.005(4) C13B 0.038(5) 0.025(4) 0.053(6) 0.018(4) 0.002(4) 0.008(4) C14B 0.032(4) 0.032(4) 0.030(4) 0.016(3) 0.002(3) 0.002(4) C15B 0.025(4) 0.029(4) 0.026(4) 0.005(3) 0.003(3) -0.004(4) C16B 0.031(4) 0.031(4) 0.029(4) 0.000(3) 0.006(3) -0.001(4) C17B 0.039(5) 0.041(5) 0.032(5) -0.003(4) 0.014(4) 0.000(4) C18B 0.042(5) 0.028(5) 0.056(6) 0.005(4) 0.017(4) 0.000(4) C19B 0.030(4) 0.025(4) 0.047(5) 0.007(4) 0.011(4) 0.003(4) C20B 0.023(4) 0.026(4) 0.033(4) 0.011(3) 0.013(3) 0.003(3) C21B 0.036(4) 0.031(4) 0.015(3) 0.012(3) 0.010(3) 0.011(4) C22B 0.040(5) 0.028(4) 0.026(4) 0.007(3) 0.014(3) 0.010(4) C23B 0.040(5) 0.047(5) 0.029(4) 0.015(4) 0.003(4) 0.013(4) C24B 0.031(4) 0.042(5) 0.028(4) 0.007(4) -0.003(3) 0.009(4) C25B 0.025(4) 0.024(4) 0.023(4) 0.006(3) 0.005(3) 0.001(3) C26B 0.022(4) 0.030(4) 0.020(4) 0.006(3) 0.005(3) 0.001(3) C27B 0.026(4) 0.041(5) 0.040(5) 0.011(4) 0.000(4) 0.002(4) C28B 0.036(5) 0.044(5) 0.038(5) -0.002(4) 0.005(4) 0.004(4) C29B 0.033(4) 0.025(4) 0.027(4) -0.004(3) 0.010(3) -0.007(4) C30B 0.027(4) 0.041(5) 0.023(4) 0.002(3) 0.005(3) -0.006(4) C31B 0.029(4) 0.036(5) 0.032(4) 0.004(4) 0.006(3) -0.001(4) C32B 0.028(4) 0.039(5) 0.035(5) 0.013(4) -0.005(4) -0.007(4) C33B 0.045(5) 0.049(5) 0.026(4) 0.006(4) 0.007(4) -0.013(5) C34B 0.038(5) 0.035(5) 0.035(5) -0.002(4) 0.015(4) -0.005(4) C35B 0.026(4) 0.028(4) 0.034(4) 0.005(3) 0.007(3) -0.003(4) C36B 0.028(5) 0.046(5) 0.036(5) 0.002(4) 0.007(4) 0.000(4) C37B 0.033(5) 0.061(6) 0.028(4) 0.017(4) 0.002(4) -0.004(5) C38B 0.070(8) 0.071(8) 0.064(8) 0.008(6) 0.025(6) 0.003(7) N8 0.086(8) 0.109(9) 0.066(7) 0.038(6) 0.004(6) -0.006(7) C39 0.080(10) 0.117(13) 0.094(11) 0.038(10) 0.036(8) 0.021(10) C40 0.072(9) 0.122(12) 0.068(8) 0.044(8) 0.030(7) 0.053(9) C41 0.170(15) 0.043(6) 0.057(7) 0.016(6) 0.050(9) 0.026(8) C42 0.090(9) 0.102(10) 0.040(6) 0.014(6) 0.017(6) -0.045(8) C43 0.041(5) 0.072(7) 0.043(6) 0.016(5) 0.006(4) 0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag NdA O4A 2.460(5) . ? NdA O1A 2.471(5) . ? NdA N6A 2.607(6) . ? NdA N2A 2.614(6) . ? NdA N4A 2.615(6) . ? NdA N3A 2.620(6) . ? NdA N5A 2.622(6) . ? NdA N1A 2.623(6) . ? NdA N7A 2.717(6) . ? S1A O2A 1.423(6) . ? S1A O3A 1.442(6) . ? S1A O1A 1.464(5) . ? S1A C36A 1.836(8) . ? S2A O6A 1.432(6) . ? S2A O5A 1.439(5) . ? S2A O4A 1.475(5) . ? S2A C37A 1.814(8) . ? S3A O8A 1.286(8) . ? S3A O10A 1.333(7) . ? S3A C38A 1.699(11) . ? S3A O9A 1.748(13) . ? S3A O7A 1.770(16) . ? F1A C36A 1.341(9) . ? F2A C36A 1.315(9) . ? F3A C36A 1.320(9) . ? F4A C37A 1.334(9) . ? F5A C37A 1.324(10) . ? F6A C37A 1.342(9) . ? F7A O7A 1.58(3) . ? F7A C38A 1.66(2) . ? F8A C38A 1.287(11) . ? F9A O9A 1.48(2) . ? F9A C38A 1.59(2) . ? F10A C38A 1.271(12) . ? N2A C6A 1.349(9) . ? N2A C10A 1.359(9) . ? N3A C11A 1.355(9) . ? N3A C15A 1.360(9) . ? N4A C20A 1.349(9) . ? N4A C16A 1.349(9) . ? N5A C21A 1.351(9) . ? N5A C25A 1.360(9) . ? N6A C26A 1.355(10) . ? N6A C30A 1.361(9) . ? N1A C1A 1.346(10) . ? N1A C5A 1.349(10) . ? N7A C31A 1.327(10) . ? N7A C35A 1.349(10) . ? C1A C2A 1.369(11) . ? C2A C3A 1.378(12) . ? C3A C4A 1.369(12) . ? C4A C5A 1.389(10) . ? C5A C6A 1.506(11) . ? C6A C7A 1.394(10) . ? C7A C8A 1.377(11) . ? C8A C9A 1.377(11) . ? C9A C10A 1.394(10) . ? C10A C11A 1.483(10) . ? C11A C12A 1.390(10) . ? C12A C13A 1.387(11) . ? C13A C14A 1.372(11) . ? C14A C15A 1.390(10) . ? C16A C17A 1.378(11) . ? C17A C18A 1.368(12) . ? C18A C19A 1.389(11) . ? C19A C20A 1.389(11) . ? C20A C21A 1.483(10) . ? C21A C22A 1.393(10) . ? C22A C23A 1.377(11) . ? C23A C24A 1.369(11) . ? C24A C25A 1.382(10) . ? C25A C26A 1.489(10) . ? C26A C27A 1.401(10) . ? C27A C28A 1.363(12) . ? C28A C29A 1.370(12) . ? C29A C30A 1.373(10) . ? C31A C32A 1.395(10) . ? C32A C33A 1.357(12) . ? C33A C34A 1.367(12) . ? C34A C35A 1.383(11) . ? NdB O1B 2.453(5) . ? NdB O4B 2.461(5) . ? NdB N6B 2.600(6) . ? NdB N4B 2.614(6) . ? NdB N5B 2.614(6) . ? NdB N3B 2.618(6) . ? NdB N1B 2.619(6) . ? NdB N2B 2.621(6) . ? NdB N7B 2.686(6) . ? S1B O3B 1.431(6) . ? S1B O2B 1.433(6) . ? S1B O1B 1.467(5) . ? S1B C36B 1.817(9) . ? S2B O6B 1.424(6) . ? S2B O5B 1.431(5) . ? S2B O4B 1.459(5) . ? S2B C37B 1.828(9) . ? S3B O8B 1.384(8) . ? S3B O7B 1.412(9) . ? S3B O9B 1.421(7) . ? S3B C38B 1.795(12) . ? F1B C36B 1.313(9) . ? F2B C36B 1.341(9) . ? F3B C36B 1.343(10) . ? F4B C37B 1.325(10) . ? F5B C37B 1.337(9) . ? F6B C37B 1.292(11) . ? F7B C38B 1.322(14) . ? F8B C38B 1.313(13) . ? F9B C38B 1.295(14) . ? N1B C5B 1.352(9) . ? N1B C1B 1.358(10) . ? N2B C10B 1.350(9) . ? N2B C6B 1.350(9) . ? N3B C15B 1.350(9) . ? N3B C11B 1.365(10) . ? N4B C16B 1.340(10) . ? N4B C20B 1.353(9) . ? N5B C21B 1.342(9) . ? N5B C25B 1.369(9) . ? N6B C30B 1.326(10) . ? N6B C26B 1.387(9) . ? N7B C31B 1.336(10) . ? N7B C35B 1.351(10) . ? C1B C2B 1.352(11) . ? C2B C3B 1.382(12) . ? C3B C4B 1.366(12) . ? C4B C5B 1.388(11) . ? C5B C6B 1.485(10) . ? C6B C7B 1.384(11) . ? C7B C8B 1.379(12) . ? C8B C9B 1.373(12) . ? C9B C10B 1.394(11) . ? C10B C11B 1.480(11) . ? C11B C12B 1.405(10) . ? C12B C13B 1.377(12) . ? C13B C14B 1.374(12) . ? C14B C15B 1.370(10) . ? C16B C17B 1.380(11) . ? C17B C18B 1.399(12) . ? C18B C19B 1.371(12) . ? C19B C20B 1.397(11) . ? C20B C21B 1.480(11) . ? C21B C22B 1.378(10) . ? C22B C23B 1.383(11) . ? C23B C24B 1.377(12) . ? C24B C25B 1.407(10) . ? C25B C26B 1.490(10) . ? C26B C27B 1.374(10) . ? C27B C28B 1.373(12) . ? C28B C29B 1.376(11) . ? C29B C30B 1.387(10) . ? C31B C32B 1.380(11) . ? C32B C33B 1.380(12) . ? C33B C34B 1.370(12) . ? C34B C35B 1.384(11) . ? N8 C39 1.2517 . ? N8 C43 1.2885 . ? C39 C40 1.2458 . ? C40 C41 1.4410 . ? C41 C42 1.5754 . ? C42 C43 1.4254 . ? 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 O4A NdA O1A 141.34(16) . . ? O4A NdA N6A 72.88(18) . . ? O1A NdA N6A 143.93(17) . . ? O4A NdA N2A 131.80(18) . . ? O1A NdA N2A 70.23(17) . . ? N6A NdA N2A 76.35(18) . . ? O4A NdA N4A 91.90(18) . . ? O1A NdA N4A 74.94(18) . . ? N6A NdA N4A 125.13(19) . . ? N2A NdA N4A 136.29(18) . . ? O4A NdA N3A 75.75(18) . . ? O1A NdA N3A 96.44(18) . . ? N6A NdA N3A 79.60(18) . . ? N2A NdA N3A 62.77(18) . . ? N4A NdA N3A 148.26(18) . . ? O4A NdA N5A 68.55(17) . . ? O1A NdA N5A 129.79(18) . . ? N6A NdA N5A 62.69(18) . . ? N2A NdA N5A 125.76(18) . . ? N4A NdA N5A 62.67(19) . . ? N3A NdA N5A 133.76(19) . . ? O4A NdA N1A 142.28(18) . . ? O1A NdA N1A 72.89(18) . . ? N6A NdA N1A 80.22(19) . . ? N2A NdA N1A 62.96(19) . . ? N4A NdA N1A 82.28(19) . . ? N3A NdA N1A 125.04(19) . . ? N5A NdA N1A 75.82(18) . . ? O4A NdA N7A 71.78(17) . . ? O1A NdA N7A 69.73(17) . . ? N6A NdA N7A 139.65(18) . . ? N2A NdA N7A 114.97(18) . . ? N4A NdA N7A 74.95(19) . . ? N3A NdA N7A 73.42(18) . . ? N5A NdA N7A 119.28(18) . . ? N1A NdA N7A 140.04(19) . . ? O2A S1A O3A 116.7(4) . . ? O2A S1A O1A 114.3(3) . . ? O3A S1A O1A 112.6(3) . . ? O2A S1A C36A 104.8(4) . . ? O3A S1A C36A 104.0(4) . . ? O1A S1A C36A 102.5(3) . . ? O6A S2A O5A 117.5(3) . . ? O6A S2A O4A 112.8(3) . . ? O5A S2A O4A 113.4(3) . . ? O6A S2A C37A 104.5(4) . . ? O5A S2A C37A 104.0(3) . . ? O4A S2A C37A 102.6(3) . . ? O8A S3A O10A 134.0(5) . . ? O8A S3A C38A 113.4(6) . . ? O10A S3A C38A 112.4(5) . . ? O8A S3A O9A 94.1(9) . . ? O10A S3A O9A 95.7(7) . . ? C38A S3A O9A 82.5(9) . . ? O8A S3A O7A 88.4(12) . . ? O10A S3A O7A 92.4(8) . . ? C38A S3A O7A 83.8(11) . . ? O9A S3A O7A 166.0(10) . . ? O7A F7A C38A 91.2(9) . . ? O9A F9A C38A 95.4(8) . . ? S1A O1A NdA 145.3(3) . . ? S2A O4A NdA 150.8(3) . . ? F7A O7A S3A 91.5(10) . . ? F9A O9A S3A 91.8(8) . . ? C6A N2A C10A 118.1(6) . . ? C6A N2A NdA 120.7(5) . . ? C10A N2A NdA 120.9(4) . . ? C11A N3A C15A 117.4(6) . . ? C11A N3A NdA 121.4(5) . . ? C15A N3A NdA 121.1(5) . . ? C20A N4A C16A 117.8(6) . . ? C20A N4A NdA 121.6(5) . . ? C16A N4A NdA 120.6(5) . . ? C21A N5A C25A 117.7(6) . . ? C21A N5A NdA 120.5(5) . . ? C25A N5A NdA 120.9(4) . . ? C26A N6A C30A 116.0(6) . . ? C26A N6A NdA 121.3(5) . . ? C30A N6A NdA 122.4(5) . . ? C1A N1A C5A 116.8(6) . . ? C1A N1A NdA 121.4(5) . . ? C5A N1A NdA 119.8(5) . . ? C31A N7A C35A 116.2(6) . . ? C31A N7A NdA 120.0(5) . . ? C35A N7A NdA 123.8(5) . . ? N1A C1A C2A 124.1(8) . . ? C1A C2A C3A 117.9(8) . . ? C4A C3A C2A 120.1(8) . . ? C3A C4A C5A 118.5(8) . . ? N1A C5A C4A 122.6(7) . . ? N1A C5A C6A 116.8(6) . . ? C4A C5A C6A 120.6(7) . . ? N2A C6A C7A 123.2(7) . . ? N2A C6A C5A 117.2(6) . . ? C7A C6A C5A 119.7(7) . . ? C8A C7A C6A 117.8(7) . . ? C9A C8A C7A 120.2(7) . . ? C8A C9A C10A 119.2(7) . . ? N2A C10A C9A 121.5(7) . . ? N2A C10A C11A 117.7(6) . . ? C9A C10A C11A 120.8(6) . . ? N3A C11A C12A 122.2(7) . . ? N3A C11A C10A 116.8(6) . . ? C12A C11A C10A 121.0(6) . . ? C13A C12A C11A 119.3(7) . . ? C14A C13A C12A 119.3(7) . . ? C13A C14A C15A 118.9(7) . . ? N3A C15A C14A 122.9(7) . . ? N4A C16A C17A 124.0(8) . . ? C18A C17A C16A 117.6(8) . . ? C17A C18A C19A 120.0(7) . . ? C18A C19A C20A 119.1(8) . . ? N4A C20A C19A 121.4(7) . . ? N4A C20A C21A 116.8(6) . . ? C19A C20A C21A 121.9(7) . . ? N5A C21A C22A 122.2(7) . . ? N5A C21A C20A 117.6(6) . . ? C22A C21A C20A 120.2(7) . . ? C23A C22A C21A 119.3(7) . . ? C24A C23A C22A 118.7(7) . . ? C23A C24A C25A 120.2(8) . . ? N5A C25A C24A 121.9(7) . . ? N5A C25A C26A 116.6(6) . . ? C24A C25A C26A 121.6(7) . . ? N6A C26A C27A 121.2(7) . . ? N6A C26A C25A 117.3(6) . . ? C27A C26A C25A 121.4(7) . . ? C28A C27A C26A 120.1(8) . . ? C27A C28A C29A 120.2(8) . . ? C28A C29A C30A 117.0(7) . . ? N6A C30A C29A 125.5(7) . . ? N7A C31A C32A 124.1(7) . . ? C33A C32A C31A 118.4(8) . . ? C32A C33A C34A 119.1(7) . . ? C33A C34A C35A 119.3(8) . . ? N7A C35A C34A 122.9(8) . . ? F2A C36A F3A 108.4(7) . . ? F2A C36A F1A 108.5(6) . . ? F3A C36A F1A 107.3(7) . . ? F2A C36A S1A 110.8(6) . . ? F3A C36A S1A 111.2(5) . . ? F1A C36A S1A 110.5(6) . . ? F5A C37A F4A 108.4(7) . . ? F5A C37A F6A 107.9(6) . . ? F4A C37A F6A 106.4(6) . . ? F5A C37A S2A 112.3(6) . . ? F4A C37A S2A 110.7(5) . . ? F6A C37A S2A 111.0(5) . . ? F10A C38A F8A 115.1(9) . . ? F10A C38A F9A 89.6(11) . . ? F8A C38A F9A 92.7(11) . . ? F10A C38A F7A 82.5(11) . . ? F8A C38A F7A 93.5(10) . . ? F9A C38A F7A 171.5(10) . . ? F10A C38A S3A 123.3(7) . . ? F8A C38A S3A 121.6(8) . . ? F9A C38A S3A 90.2(9) . . ? F7A C38A S3A 91.5(9) . . ? O1B NdB O4B 143.64(17) . . ? O1B NdB N6B 143.55(18) . . ? O4B NdB N6B 71.25(18) . . ? O1B NdB N4B 74.50(19) . . ? O4B NdB N4B 91.47(19) . . ? N6B NdB N4B 126.5(2) . . ? O1B NdB N5B 126.92(17) . . ? O4B NdB N5B 69.69(17) . . ? N6B NdB N5B 63.99(19) . . ? N4B NdB N5B 62.49(19) . . ? O1B NdB N3B 96.69(18) . . ? O4B NdB N3B 75.94(18) . . ? N6B NdB N3B 80.19(19) . . ? N4B NdB N3B 145.50(19) . . ? N5B NdB N3B 136.35(18) . . ? O1B NdB N1B 71.46(18) . . ? O4B NdB N1B 141.43(18) . . ? N6B NdB N1B 80.94(18) . . ? N4B NdB N1B 83.93(19) . . ? N5B NdB N1B 74.35(18) . . ? N3B NdB N1B 125.58(19) . . ? O1B NdB N2B 71.34(17) . . ? O4B NdB N2B 130.26(18) . . ? N6B NdB N2B 75.13(18) . . ? N4B NdB N2B 138.24(19) . . ? N5B NdB N2B 124.39(18) . . ? N3B NdB N2B 62.93(18) . . ? N1B NdB N2B 62.99(19) . . ? O1B NdB N7B 71.21(18) . . ? O4B NdB N7B 72.69(18) . . ? N6B NdB N7B 138.56(18) . . ? N4B NdB N7B 73.8(2) . . ? N5B NdB N7B 120.00(19) . . ? N3B NdB N7B 71.83(19) . . ? N1B NdB N7B 140.38(18) . . ? N2B NdB N7B 115.61(19) . . ? O3B S1B O2B 117.4(4) . . ? O3B S1B O1B 112.5(3) . . ? O2B S1B O1B 114.6(3) . . ? O3B S1B C36B 103.9(4) . . ? O2B S1B C36B 104.5(4) . . ? O1B S1B C36B 101.5(3) . . ? O6B S2B O5B 116.9(4) . . ? O6B S2B O4B 113.1(4) . . ? O5B S2B O4B 113.5(3) . . ? O6B S2B C37B 105.0(4) . . ? O5B S2B C37B 103.9(4) . . ? O4B S2B C37B 102.3(4) . . ? O8B S3B O7B 111.6(9) . . ? O8B S3B O9B 117.3(7) . . ? O7B S3B O9B 112.2(5) . . ? O8B S3B C38B 105.2(6) . . ? O7B S3B C38B 103.2(7) . . ? O9B S3B C38B 105.9(5) . . ? S1B O1B NdB 146.8(3) . . ? S2B O4B NdB 159.3(3) . . ? C5B N1B C1B 115.6(6) . . ? C5B N1B NdB 121.0(5) . . ? C1B N1B NdB 122.3(5) . . ? C10B N2B C6B 118.6(6) . . ? C10B N2B NdB 121.2(5) . . ? C6B N2B NdB 120.0(5) . . ? C15B N3B C11B 117.3(6) . . ? C15B N3B NdB 122.2(5) . . ? C11B N3B NdB 120.3(4) . . ? C16B N4B C20B 117.7(6) . . ? C16B N4B NdB 121.0(5) . . ? C20B N4B NdB 121.3(5) . . ? C21B N5B C25B 118.0(6) . . ? C21B N5B NdB 121.5(5) . . ? C25B N5B NdB 120.0(4) . . ? C30B N6B C26B 114.8(6) . . ? C30B N6B NdB 124.3(5) . . ? C26B N6B NdB 120.8(4) . . ? C31B N7B C35B 116.8(7) . . ? C31B N7B NdB 120.5(5) . . ? C35B N7B NdB 122.7(5) . . ? C2B C1B N1B 126.0(8) . . ? C1B C2B C3B 117.1(8) . . ? C4B C3B C2B 119.4(8) . . ? C3B C4B C5B 120.1(8) . . ? N1B C5B C4B 121.7(7) . . ? N1B C5B C6B 116.4(6) . . ? C4B C5B C6B 121.7(7) . . ? N2B C6B C7B 121.4(7) . . ? N2B C6B C5B 118.7(6) . . ? C7B C6B C5B 119.8(7) . . ? C8B C7B C6B 120.1(7) . . ? C9B C8B C7B 118.8(7) . . ? C8B C9B C10B 119.3(7) . . ? N2B C10B C9B 121.9(7) . . ? N2B C10B C11B 117.2(7) . . ? C9B C10B C11B 120.9(7) . . ? N3B C11B C12B 120.8(7) . . ? N3B C11B C10B 117.9(6) . . ? C12B C11B C10B 121.3(7) . . ? C13B C12B C11B 119.7(8) . . ? C14B C13B C12B 119.4(7) . . ? C15B C14B C13B 118.5(7) . . ? N3B C15B C14B 124.3(8) . . ? N4B C16B C17B 125.0(8) . . ? C16B C17B C18B 116.6(8) . . ? C19B C18B C17B 119.7(8) . . ? C18B C19B C20B 120.0(8) . . ? N4B C20B C19B 121.0(7) . . ? N4B C20B C21B 117.1(6) . . ? C19B C20B C21B 121.8(7) . . ? N5B C21B C22B 122.1(7) . . ? N5B C21B C20B 117.1(6) . . ? C22B C21B C20B 120.8(7) . . ? C21B C22B C23B 120.7(7) . . ? C24B C23B C22B 118.3(8) . . ? C23B C24B C25B 119.2(7) . . ? N5B C25B C24B 121.8(7) . . ? N5B C25B C26B 118.3(6) . . ? C24B C25B C26B 120.0(7) . . ? C27B C26B N6B 122.5(7) . . ? C27B C26B C25B 120.7(7) . . ? N6B C26B C25B 116.7(6) . . ? C28B C27B C26B 120.1(8) . . ? C27B C28B C29B 118.9(8) . . ? C28B C29B C30B 117.5(8) . . ? N6B C30B C29B 126.0(8) . . ? N7B C31B C32B 123.5(8) . . ? C31B C32B C33B 118.7(8) . . ? C34B C33B C32B 119.0(8) . . ? C33B C34B C35B 118.9(8) . . ? N7B C35B C34B 123.1(7) . . ? F1B C36B F2B 107.5(7) . . ? F1B C36B F3B 108.1(7) . . ? F2B C36B F3B 105.8(7) . . ? F1B C36B S1B 112.6(6) . . ? F2B C36B S1B 111.5(6) . . ? F3B C36B S1B 111.0(6) . . ? F6B C37B F4B 107.6(8) . . ? F6B C37B F5B 109.0(8) . . ? F4B C37B F5B 108.1(7) . . ? F6B C37B S2B 111.5(6) . . ? F4B C37B S2B 109.8(6) . . ? F5B C37B S2B 110.8(6) . . ? F9B C38B F8B 112.5(10) . . ? F9B C38B F7B 102.2(11) . . ? F8B C38B F7B 107.1(11) . . ? F9B C38B S3B 113.1(9) . . ? F8B C38B S3B 111.7(8) . . ? F7B C38B S3B 109.7(9) . . ? C39 N8 C43 120.2 . . ? C40 C39 N8 123.7 . . ? C39 C40 C41 125.4 . . ? C40 C41 C42 113.1 . . ? C43 C42 C41 108.3 . . ? N8 C43 C42 129.1 . . ? #===END data_3.0.5py _database_code_depnum_ccdc_archive 'CCDC 251216' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H59 F18 N15 O18 S6 U2' _chemical_formula_weight 2540.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 14.487(3) _cell_length_b 14.997(3) _cell_length_c 21.269(4) _cell_angle_alpha 98.67(3) _cell_angle_beta 100.48(3) _cell_angle_gamma 93.26(3) _cell_volume 4474.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 27774 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 3.869 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.610 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 8 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27774 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 24.75 _reflns_number_total 14085 _reflns_number_gt 9575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms. Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0634P)^2^+8.9391P] 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 14085 _refine_ls_number_parameters 1249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.034 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.847 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.141 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 U1A U 0.239920(10) 0.245968(9) 0.475424(7) 0.03501(4) Uani 1 1 d . . . S1A S 0.28412(8) 0.50134(7) 0.51583(5) 0.0442(3) Uani 1 1 d . . . S2A S 0.23931(7) 0.04368(7) 0.56655(5) 0.0396(3) Uani 1 1 d . . . S3A S -0.18274(11) 0.30756(14) 0.23174(7) 0.0978(6) Uani 1 1 d . . . O1A O 0.30821(19) 0.40662(17) 0.50540(13) 0.0422(8) Uani 1 1 d . . . O2A O 0.2824(2) 0.54642(19) 0.46075(14) 0.0605(10) Uani 1 1 d . . . O3A O 0.2077(2) 0.51444(19) 0.54978(16) 0.0576(10) Uani 1 1 d . . . O4A O 0.20768(19) 0.10723(16) 0.52266(13) 0.0422(8) Uani 1 1 d . . . O5A O 0.2084(2) 0.06300(18) 0.62822(13) 0.0514(9) Uani 1 1 d . . . O6A O 0.3354(2) 0.02473(19) 0.56781(15) 0.0534(10) Uani 1 1 d . . . N2A N 0.1257(2) 0.35003(19) 0.41692(15) 0.0360(9) Uani 1 1 d . . . N3A N 0.0800(2) 0.2702(2) 0.51548(15) 0.0408(10) Uani 1 1 d . . . N4A N 0.4217(2) 0.2386(2) 0.50463(15) 0.0398(10) Uani 1 1 d . . . N5A N 0.3106(2) 0.10566(19) 0.41812(15) 0.0365(9) Uani 1 1 d . . . N6A N 0.1235(2) 0.1314(2) 0.38547(14) 0.0382(9) Uani 1 1 d . . . N1A N 0.2807(2) 0.2993(2) 0.37121(15) 0.0416(10) Uani 1 1 d . . . N7A N 0.2838(2) 0.2890(2) 0.60562(16) 0.0456(10) Uani 1 1 d . . . C1A C 0.3608(3) 0.2756(3) 0.3493(2) 0.0563(15) Uani 1 1 d . . . H1AA H 0.3912 0.2283 0.3652 0.068 Uiso 1 1 calc R . . C2A C 0.3996(4) 0.3178(3) 0.3049(2) 0.0602(15) Uani 1 1 d . . . H2AB H 0.4534 0.2994 0.2905 0.072 Uiso 1 1 calc R . . C3A C 0.3533(4) 0.3882(3) 0.2837(3) 0.0760(17) Uani 1 1 d . . . H3AB H 0.3763 0.4184 0.2539 0.091 Uiso 1 1 calc R . . C4A C 0.2755(4) 0.4149(3) 0.3049(2) 0.0570(15) Uani 1 1 d . . . H4AA H 0.2469 0.4645 0.2913 0.068 Uiso 1 1 calc R . . C5A C 0.2391(3) 0.3683(3) 0.34642(18) 0.0439(12) Uani 1 1 d . . . C6A C 0.1498(3) 0.3898(3) 0.36880(19) 0.0419(12) Uani 1 1 d . . . C7A C 0.0940(3) 0.4524(3) 0.34107(18) 0.0436(12) Uani 1 1 d . . . H7AB H 0.1128 0.4805 0.3088 0.052 Uiso 1 1 calc R . . C8A C 0.0129(3) 0.4722(3) 0.3611(2) 0.0516(14) Uani 1 1 d . . . H8AB H -0.0256 0.5116 0.3412 0.062 Uiso 1 1 calc R . . C9A C -0.0125(3) 0.4337(3) 0.4112(2) 0.0498(13) Uani 1 1 d . . . H9AA H -0.0668 0.4487 0.4265 0.060 Uiso 1 1 calc R . . C10A C 0.0448(3) 0.3715(2) 0.43885(19) 0.0419(12) Uani 1 1 d . . . C11A C 0.0197(3) 0.3272(3) 0.49049(19) 0.0437(13) Uani 1 1 d . . . C12A C -0.0615(3) 0.3443(3) 0.5150(2) 0.0480(13) Uani 1 1 d . . . H12A H -0.1024 0.3836 0.4972 0.058 Uiso 1 1 calc R . . C13A C -0.0819(3) 0.3033(3) 0.56538(19) 0.0435(12) Uani 1 1 d . . . H13A H -0.1356 0.3153 0.5823 0.052 Uiso 1 1 calc R . . C14A C -0.0207(3) 0.2442(3) 0.59003(19) 0.0456(12) Uani 1 1 d . . . H14A H -0.0329 0.2149 0.6236 0.055 Uiso 1 1 calc R . . C15A C 0.0569(3) 0.2295(3) 0.56468(18) 0.0428(12) Uani 1 1 d . . . H15A H 0.0973 0.1893 0.5816 0.051 Uiso 1 1 calc R . . C16A C 0.4768(3) 0.3059(3) 0.5450(2) 0.0493(13) Uani 1 1 d . . . H16A H 0.4480 0.3556 0.5617 0.059 Uiso 1 1 calc R . . C17A C 0.5742(3) 0.3070(3) 0.5639(2) 0.0487(13) Uani 1 1 d . . . H17A H 0.6087 0.3531 0.5949 0.058 Uiso 1 1 calc R . . C18A C 0.6170(3) 0.2374(3) 0.5352(2) 0.0556(15) Uani 1 1 d . . . H18A H 0.6824 0.2386 0.5437 0.067 Uiso 1 1 calc R . . C19A C 0.5638(3) 0.1647(3) 0.4931(2) 0.0561(15) Uani 1 1 d . . . H19A H 0.5928 0.1161 0.4750 0.067 Uiso 1 1 calc R . . C20A C 0.4660(3) 0.1664(2) 0.4789(2) 0.0439(12) Uani 1 1 d . . . C21A C 0.4045(3) 0.0919(3) 0.43551(18) 0.0408(12) Uani 1 1 d . . . C22A C 0.4400(3) 0.0116(3) 0.4144(2) 0.0466(12) Uani 1 1 d . . . H22A H 0.5034 0.0035 0.4274 0.056 Uiso 1 1 calc R . . C23A C 0.3805(4) -0.0559(3) 0.3739(2) 0.0580(15) Uani 1 1 d . . . H23A H 0.4040 -0.1102 0.3597 0.070 Uiso 1 1 calc R . . C24A C 0.2883(3) -0.0451(3) 0.3543(2) 0.0503(14) Uani 1 1 d . . . H24A H 0.2485 -0.0907 0.3261 0.060 Uiso 1 1 calc R . . C25A C 0.2531(3) 0.0384(2) 0.37807(17) 0.0362(11) Uani 1 1 d . . . C26A C 0.1525(3) 0.0518(3) 0.36024(18) 0.0390(11) Uani 1 1 d . . . C27A C 0.0880(3) -0.0158(3) 0.3191(2) 0.0502(14) Uani 1 1 d . . . H27A H 0.1082 -0.0708 0.3027 0.060 Uiso 1 1 calc R . . C28A C -0.0047(3) 0.0007(3) 0.3038(3) 0.0631(17) Uani 1 1 d . . . H28A H -0.0483 -0.0431 0.2769 0.076 Uiso 1 1 calc R . . C29A C -0.0324(4) 0.0818(3) 0.3281(2) 0.0584(15) Uani 1 1 d . . . H29A H -0.0950 0.0942 0.3174 0.070 Uiso 1 1 calc R . . C30A C 0.0317(3) 0.1446(3) 0.3681(2) 0.0422(12) Uani 1 1 d . . . H30A H 0.0112 0.1995 0.3844 0.051 Uiso 1 1 calc R . . C31A C 0.2430(3) 0.3582(3) 0.6366(2) 0.0540(15) Uani 1 1 d . . . H31A H 0.1997 0.3881 0.6114 0.065 Uiso 1 1 calc R . . C32A C 0.2620(3) 0.3871(3) 0.70391(19) 0.0539(14) Uani 1 1 d . . . H32A H 0.2322 0.4344 0.7230 0.065 Uiso 1 1 calc R . . C33A C 0.3261(4) 0.3428(3) 0.7400(2) 0.0661(17) Uani 1 1 d . . . H33A H 0.3384 0.3573 0.7850 0.079 Uiso 1 1 calc R . . C34A C 0.3722(4) 0.2775(3) 0.7101(2) 0.0574(15) Uani 1 1 d . . . H34A H 0.4200 0.2511 0.7343 0.069 Uiso 1 1 calc R . . C35A C 0.3482(3) 0.2508(3) 0.6443(2) 0.0534(14) Uani 1 1 d . . . H35A H 0.3783 0.2035 0.6254 0.064 Uiso 1 1 calc R . . C36A C 0.3878(3) 0.5550(3) 0.5744(2) 0.0523(14) Uani 1 1 d . . . C37A C 0.1697(3) -0.0606(3) 0.52716(19) 0.0419(12) Uani 1 1 d . . . U1B U 0.251935(11) 0.253747(9) 0.014028(7) 0.03701(4) Uani 1 1 d . . . S1B S -0.01498(8) 0.22313(7) -0.01744(5) 0.0486(3) Uani 1 1 d . . . S2B S 0.46671(8) 0.25908(7) -0.07140(5) 0.0427(3) Uani 1 1 d . . . S3B S 0.17931(9) 0.69453(8) 0.27785(6) 0.0586(4) Uani 1 1 d . . . O1B O 0.08187(19) 0.19848(18) -0.01291(13) 0.0455(9) Uani 1 1 d . . . O2B O -0.0533(2) 0.2235(2) 0.04065(14) 0.0593(10) Uani 1 1 d . . . O3B O -0.0326(2) 0.2984(2) -0.05095(17) 0.0679(12) Uani 1 1 d . . . O4B O 0.3957(2) 0.28061(18) -0.03205(12) 0.0473(8) Uani 1 1 d . . . O5B O 0.4497(2) 0.2926(2) -0.13252(13) 0.0539(9) Uani 1 1 d . . . O6B O 0.4918(3) 0.1696(2) -0.07312(17) 0.0732(12) Uani 1 1 d . . . N1B N 0.2009(2) 0.2114(2) 0.11943(15) 0.0425(10) Uani 1 1 d . . . N2B N 0.1579(2) 0.3693(2) 0.07641(15) 0.0395(10) Uani 1 1 d . . . N3B N 0.2326(2) 0.4108(2) -0.02578(15) 0.0414(10) Uani 1 1 d . . . N4B N 0.2467(3) 0.0775(2) -0.02052(17) 0.0492(11) Uani 1 1 d . . . N5B N 0.3909(2) 0.1714(2) 0.06972(15) 0.0404(10) Uani 1 1 d . . . N6B N 0.3806(2) 0.3550(2) 0.10290(15) 0.0446(10) Uani 1 1 d . . . N7B N 0.1974(2) 0.2217(2) -0.11513(16) 0.0461(10) Uani 1 1 d . . . C1B C 0.2162(3) 0.1300(3) 0.1382(2) 0.0548(14) Uani 1 1 d . . . H1BA H 0.2562 0.0944 0.1179 0.066 Uiso 1 1 calc R . . C2B C 0.1774(4) 0.0963(3) 0.1845(2) 0.0645(16) Uani 1 1 d . . . H2BB H 0.1928 0.0414 0.1970 0.077 Uiso 1 1 calc R . . C3B C 0.1154(3) 0.1463(3) 0.2115(2) 0.0593(14) Uani 1 1 d . . . H3BB H 0.0862 0.1248 0.2424 0.071 Uiso 1 1 calc R . . C4B C 0.0945(3) 0.2304(3) 0.1933(2) 0.0528(14) Uani 1 1 d . . . H4BA H 0.0511 0.2644 0.2111 0.063 Uiso 1 1 calc R . . C5B C 0.1406(3) 0.2609(3) 0.14803(18) 0.0394(12) Uani 1 1 d . . . C6B C 0.1205(3) 0.3480(3) 0.12670(19) 0.0420(12) Uani 1 1 d . . . C7B C 0.0621(3) 0.4050(3) 0.1569(2) 0.0462(13) Uani 1 1 d . . . H7BB H 0.0363 0.3885 0.1909 0.055 Uiso 1 1 calc R . . C8B C 0.0438(3) 0.4850(3) 0.1357(2) 0.0531(14) Uani 1 1 d . . . H8BB H 0.0061 0.5238 0.1558 0.064 Uiso 1 1 calc R . . C9B C 0.0804(3) 0.5077(3) 0.0856(2) 0.0482(13) Uani 1 1 d . . . H9BB H 0.0675 0.5619 0.0709 0.058 Uiso 1 1 calc R . . C10B C 0.1375(3) 0.4498(3) 0.05595(19) 0.0434(12) Uani 1 1 d . . . C11B C 0.1783(3) 0.4709(3) -0.00049(19) 0.0410(12) Uani 1 1 d . . . C12B C 0.1609(3) 0.5512(3) -0.0237(2) 0.0536(14) Uani 1 1 d . . . H12B H 0.1250 0.5926 -0.0042 0.064 Uiso 1 1 calc R . . C13B C 0.1985(3) 0.5679(3) -0.0765(2) 0.0560(15) Uani 1 1 d . . . H13B H 0.1852 0.6198 -0.0942 0.067 Uiso 1 1 calc R . . C14B C 0.2555(3) 0.5084(3) -0.1031(2) 0.0478(13) Uani 1 1 d . . . H14B H 0.2823 0.5195 -0.1380 0.057 Uiso 1 1 calc R . . C15B C 0.2708(3) 0.4311(3) -0.0755(2) 0.0479(13) Uani 1 1 d . . . H15B H 0.3101 0.3909 -0.0924 0.057 Uiso 1 1 calc R . . C16B C 0.1737(3) 0.0310(3) -0.0631(2) 0.0484(13) Uani 1 1 d . . . H16B H 0.1245 0.0631 -0.0799 0.058 Uiso 1 1 calc R . . C17B C 0.1672(4) -0.0595(3) -0.0832(2) 0.0603(16) Uani 1 1 d . . . H17B H 0.1155 -0.0879 -0.1138 0.072 Uiso 1 1 calc R . . C18B C 0.2374(3) -0.1091(3) -0.0582(2) 0.0560(15) Uani 1 1 d . . . H18B H 0.2344 -0.1713 -0.0716 0.067 Uiso 1 1 calc R . . C19B C 0.3125(4) -0.0651(3) -0.0126(2) 0.0601(15) Uani 1 1 d . . . H19B H 0.3601 -0.0972 0.0064 0.072 Uiso 1 1 calc R . . C20B C 0.3155(3) 0.0284(3) 0.0042(2) 0.0484(13) Uani 1 1 d . . . C21B C 0.3984(3) 0.0803(3) 0.05153(19) 0.0477(12) Uani 1 1 d . . . C22B C 0.4739(3) 0.0373(3) 0.0760(2) 0.0498(13) Uani 1 1 d . . . H22B H 0.4758 -0.0246 0.0633 0.060 Uiso 1 1 calc R . . C23B C 0.5471(3) 0.0868(3) 0.1198(2) 0.0606(14) Uani 1 1 d . . . H23B H 0.5992 0.0582 0.1365 0.073 Uiso 1 1 calc R . . C24B C 0.5443(4) 0.1768(3) 0.1388(2) 0.0599(16) Uani 1 1 d . . . H24B H 0.5938 0.2105 0.1683 0.072 Uiso 1 1 calc R . . C25B C 0.4635(3) 0.2184(3) 0.11230(19) 0.0478(13) Uani 1 1 d . . . C26B C 0.4598(3) 0.3163(3) 0.13181(19) 0.0437(12) Uani 1 1 d . . . C27B C 0.5309(4) 0.3702(3) 0.1753(2) 0.0636(16) Uani 1 1 d . . . H27B H 0.5822 0.3436 0.1955 0.076 Uiso 1 1 calc R . . C28B C 0.5276(3) 0.4625(3) 0.1894(2) 0.0662(17) Uani 1 1 d . . . H28B H 0.5765 0.4984 0.2181 0.079 Uiso 1 1 calc R . . C29B C 0.4498(3) 0.5005(3) 0.1599(2) 0.0499(14) Uani 1 1 d . . . H29B H 0.4448 0.5625 0.1692 0.060 Uiso 1 1 calc R . . C30B C 0.3802(3) 0.4456(3) 0.1169(2) 0.0436(12) Uani 1 1 d . . . H30B H 0.3296 0.4725 0.0961 0.052 Uiso 1 1 calc R . . C31B C 0.1242(3) 0.2599(3) -0.1453(2) 0.0547(15) Uani 1 1 d . . . H31B H 0.0890 0.2934 -0.1193 0.066 Uiso 1 1 calc R . . C32B C 0.0966(4) 0.2538(3) -0.2116(2) 0.0620(16) Uani 1 1 d . . . H32B H 0.0477 0.2853 -0.2296 0.074 Uiso 1 1 calc R . . C33B C 0.1454(4) 0.1983(3) -0.2505(2) 0.0688(18) Uani 1 1 d . . . H33B H 0.1285 0.1913 -0.2954 0.083 Uiso 1 1 calc R . . C34B C 0.2185(4) 0.1538(3) -0.2222(2) 0.0607(16) Uani 1 1 d . . . H34B H 0.2501 0.1155 -0.2479 0.073 Uiso 1 1 calc R . . C35B C 0.2447(3) 0.1667(3) -0.1548(2) 0.0482(13) Uani 1 1 d . . . H35B H 0.2951 0.1376 -0.1360 0.058 Uiso 1 1 calc R . . C36B C -0.0812(3) 0.1274(3) -0.0734(2) 0.0606(16) Uani 1 1 d . . . C37B C 0.5701(4) 0.3300(4) -0.0238(2) 0.0662(16) Uani 1 1 d . . . N8 N 0.4974(2) 0.10771(18) 0.28919(12) 0.112(2) Uani 1 1 d G . . C39 C 0.5665(2) 0.0614(2) 0.29811(16) 0.143(3) Uani 1 1 d G . . H39 H 0.6206 0.0876 0.3271 0.172 Uiso 1 1 calc R . . C40 C 0.5667(3) -0.0177(2) 0.2704(2) 0.098(2) Uani 1 1 d G . . H40 H 0.6224 -0.0455 0.2782 0.118 Uiso 1 1 calc R . . C41 C 0.4872(4) -0.06968(19) 0.22719(19) 0.096(2) Uani 1 1 d G . . H41 H 0.4877 -0.1304 0.2099 0.115 Uiso 1 1 calc R . . C42 C 0.3992(3) -0.0136(2) 0.21200(18) 0.101(2) Uani 1 1 d G . . H42 H 0.3430 -0.0344 0.1833 0.121 Uiso 1 1 calc R . . C43 C 0.4206(2) 0.0742(2) 0.24978(15) 0.0694(18) Uani 1 1 d G . . H43 H 0.3727 0.1128 0.2455 0.083 Uiso 1 1 calc R . . F3A F 0.46526(18) 0.54579(17) 0.55137(13) 0.0617(9) Uani 1 1 d . . . F2A F 0.3805(2) 0.64556(16) 0.58740(13) 0.0629(9) Uani 1 1 d . . . F5A F 0.07848(19) -0.05230(17) 0.51809(14) 0.0648(9) Uani 1 1 d . . . F1A F 0.39679(19) 0.52193(16) 0.62974(12) 0.0598(9) Uani 1 1 d . . . F5B F 0.6001(2) 0.29902(19) 0.03025(13) 0.0708(10) Uani 1 1 d . . . F6A F 0.1929(2) -0.08885(16) 0.46858(12) 0.0609(8) Uani 1 1 d . . . F4A F 0.1884(2) -0.12686(16) 0.56162(13) 0.0728(10) Uani 1 1 d . . . F2B F -0.0488(2) 0.11686(19) -0.13088(13) 0.0698(10) Uani 1 1 d . . . F3B F -0.0674(2) 0.04996(18) -0.05063(14) 0.0742(10) Uani 1 1 d . . . F1B F -0.1711(2) 0.1359(2) -0.08588(15) 0.0788(11) Uani 1 1 d . . . F6B F 0.5539(3) 0.41453(19) -0.01222(16) 0.0907(13) Uani 1 1 d . . . F4B F 0.6394(2) 0.3269(3) -0.05672(16) 0.1069(13) Uani 1 1 d . . . F8A F -0.1775(3) 0.2785(2) 0.35083(15) 0.0961(13) Uani 1 1 d . . . F9A F -0.3178(3) 0.2772(3) 0.29470(16) 0.1060(14) Uani 1 1 d . . . O8A O -0.2468(3) 0.2921(2) 0.17576(16) 0.0727(12) Uani 1 1 d . . . O9B O 0.1069(3) 0.6232(3) 0.25551(19) 0.0952(15) Uani 1 1 d . . . O9A O -0.0937(3) 0.2903(3) 0.2388(2) 0.1088(18) Uani 1 1 d . . . F7A F -0.2417(4) 0.1745(3) 0.2705(3) 0.186(3) Uani 1 1 d . . . O8B O 0.2405(4) 0.6996(6) 0.3378(2) 0.200(3) Uani 1 1 d . . . O7B O 0.1462(4) 0.7787(3) 0.2768(3) 0.155(3) Uani 1 1 d . . . C38A C -0.2276(4) 0.2787(5) 0.2940(3) 0.095(2) Uani 1 1 d . . . O7A O -0.1903(6) 0.4119(3) 0.2662(4) 0.231(4) Uani 1 1 d . . . F8B F 0.3262(3) 0.7508(3) 0.2350(2) 0.1255(16) Uani 1 1 d . . . F9B F 0.2075(4) 0.6904(3) 0.1610(2) 0.156(2) Uani 1 1 d . . . F7B F 0.2809(3) 0.6082(3) 0.2071(3) 0.183(2) Uani 1 1 d . . . C38B C 0.2533(5) 0.6929(4) 0.2207(3) 0.088(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1A 0.03581(7) 0.03901(7) 0.03241(7) 0.00811(5) 0.00939(6) 0.00689(6) S1A 0.0458(6) 0.0414(5) 0.0447(5) 0.0070(4) 0.0069(5) 0.0042(4) S2A 0.0399(5) 0.0430(5) 0.0371(5) 0.0069(4) 0.0099(4) 0.0044(4) S3A 0.0524(8) 0.1848(16) 0.0554(8) 0.0261(9) 0.0075(7) -0.0054(10) O1A 0.0361(14) 0.0414(14) 0.0492(15) 0.0089(11) 0.0075(12) 0.0036(12) O2A 0.078(2) 0.0573(16) 0.0437(15) 0.0204(12) -0.0008(16) -0.0088(16) O3A 0.0415(16) 0.0569(16) 0.080(2) 0.0134(15) 0.0217(15) 0.0146(13) O4A 0.0551(16) 0.0340(13) 0.0437(13) 0.0086(10) 0.0231(12) 0.0066(12) O5A 0.0645(18) 0.0537(16) 0.0390(14) 0.0073(12) 0.0185(13) 0.0034(14) O6A 0.0407(16) 0.0590(16) 0.0580(18) 0.0072(14) 0.0034(15) 0.0105(14) N2A 0.0361(17) 0.0361(16) 0.0369(16) 0.0038(13) 0.0109(14) 0.0064(13) N3A 0.0450(18) 0.0426(16) 0.0381(16) 0.0100(13) 0.0121(15) 0.0099(14) N4A 0.0446(19) 0.0347(16) 0.0403(17) 0.0049(13) 0.0082(15) 0.0076(14) N5A 0.0414(17) 0.0363(15) 0.0371(15) 0.0099(12) 0.0169(13) 0.0071(13) N6A 0.0502(18) 0.0396(16) 0.0309(14) 0.0068(12) 0.0204(13) 0.0118(14) N1A 0.0447(18) 0.0525(18) 0.0327(15) 0.0120(13) 0.0144(14) 0.0126(15) N7A 0.0388(19) 0.0480(17) 0.0489(18) 0.0200(14) -0.0020(16) -0.0031(15) C1A 0.069(3) 0.054(2) 0.054(2) 0.0164(19) 0.022(2) 0.012(2) C2A 0.069(3) 0.065(3) 0.061(2) 0.023(2) 0.036(2) 0.023(2) C3A 0.076(3) 0.100(3) 0.074(3) 0.045(2) 0.040(2) 0.033(3) C4A 0.078(3) 0.047(2) 0.052(2) 0.0252(17) 0.018(2) 0.000(2) C5A 0.055(2) 0.050(2) 0.0282(18) 0.0080(16) 0.0115(18) 0.0042(19) C6A 0.045(2) 0.044(2) 0.0376(19) 0.0119(16) 0.0072(18) 0.0007(18) C7A 0.054(2) 0.051(2) 0.0271(18) 0.0105(16) 0.0075(18) 0.0012(19) C8A 0.047(2) 0.044(2) 0.066(3) 0.0192(18) 0.007(2) 0.0062(19) C9A 0.057(3) 0.055(2) 0.040(2) 0.0123(17) 0.006(2) 0.0229(19) C10A 0.050(2) 0.0308(19) 0.041(2) 0.0049(16) 0.0016(19) -0.0045(17) C11A 0.052(2) 0.042(2) 0.0326(19) -0.0029(17) 0.0050(19) 0.0007(19) C12A 0.041(2) 0.047(2) 0.060(2) 0.0109(19) 0.018(2) 0.0089(18) C13A 0.049(2) 0.041(2) 0.042(2) 0.0013(17) 0.0183(18) 0.0013(18) C14A 0.052(2) 0.050(2) 0.0405(19) 0.0061(17) 0.0259(17) 0.0010(19) C15A 0.048(2) 0.047(2) 0.0339(19) 0.0132(16) 0.0052(18) -0.0003(18) C16A 0.044(2) 0.053(2) 0.057(2) 0.0185(18) 0.015(2) 0.0139(19) C17A 0.042(2) 0.047(2) 0.054(2) 0.0114(18) 0.003(2) -0.0045(19) C18A 0.036(2) 0.064(3) 0.065(3) 0.014(2) 0.004(2) -0.002(2) C19A 0.050(3) 0.066(3) 0.059(3) 0.018(2) 0.016(2) 0.020(2) C20A 0.046(2) 0.0417(19) 0.055(2) 0.0211(16) 0.0243(18) 0.0088(17) C21A 0.042(2) 0.049(2) 0.0355(18) 0.0131(16) 0.0134(17) 0.0021(18) C22A 0.044(2) 0.056(2) 0.049(2) 0.0109(18) 0.0230(18) 0.0271(18) C23A 0.074(3) 0.050(2) 0.052(3) 0.007(2) 0.016(2) 0.018(2) C24A 0.065(3) 0.037(2) 0.050(2) 0.0049(17) 0.015(2) 0.0113(19) C25A 0.047(2) 0.0368(18) 0.0321(17) 0.0138(14) 0.0200(16) 0.0049(16) C26A 0.039(2) 0.045(2) 0.0379(18) 0.0115(15) 0.0177(16) 0.0032(17) C27A 0.048(2) 0.042(2) 0.059(3) -0.0010(19) 0.013(2) 0.0041(19) C28A 0.056(3) 0.040(2) 0.084(3) -0.004(2) 0.002(3) 0.003(2) C29A 0.058(3) 0.072(3) 0.047(2) 0.011(2) 0.016(2) -0.001(2) C30A 0.033(2) 0.042(2) 0.053(2) 0.0037(17) 0.0122(18) 0.0070(17) C31A 0.063(3) 0.049(2) 0.048(2) 0.0036(19) 0.013(2) 0.000(2) C32A 0.067(3) 0.062(3) 0.037(2) 0.0150(18) 0.018(2) 0.005(2) C33A 0.098(4) 0.053(3) 0.045(2) 0.006(2) 0.013(3) -0.009(3) C34A 0.069(3) 0.055(2) 0.040(2) 0.0128(19) -0.011(2) 0.001(2) C35A 0.051(3) 0.059(2) 0.050(2) 0.0143(19) 0.006(2) -0.004(2) C36A 0.056(3) 0.049(2) 0.049(2) -0.0033(19) 0.013(2) 0.003(2) C37A 0.043(2) 0.049(2) 0.0391(19) 0.0125(16) 0.0179(17) 0.0060(18) U1B 0.04130(8) 0.03919(7) 0.03294(7) 0.00764(6) 0.01133(6) 0.00566(6) S1B 0.0468(6) 0.0483(6) 0.0489(6) 0.0014(5) 0.0112(5) 0.0003(5) S2B 0.0482(6) 0.0453(5) 0.0386(5) 0.0114(4) 0.0134(4) 0.0084(4) S3B 0.0568(7) 0.0682(7) 0.0464(6) -0.0009(5) 0.0062(6) 0.0083(6) O1B 0.0408(15) 0.0538(15) 0.0421(15) 0.0049(12) 0.0111(13) 0.0045(13) O2B 0.0567(18) 0.078(2) 0.0437(16) -0.0003(15) 0.0212(14) 0.0000(16) O3B 0.071(2) 0.0599(18) 0.072(2) 0.0130(16) 0.0059(18) 0.0145(16) O4B 0.0473(15) 0.0651(16) 0.0395(13) 0.0189(12) 0.0243(12) 0.0088(13) O5B 0.0534(17) 0.0783(18) 0.0357(14) 0.0152(13) 0.0184(13) 0.0059(15) O6B 0.101(3) 0.0496(16) 0.078(2) 0.0190(15) 0.0268(19) 0.0305(16) N1B 0.0467(19) 0.0449(17) 0.0395(16) 0.0100(13) 0.0156(15) 0.0024(15) N2B 0.0458(19) 0.0414(17) 0.0293(15) 0.0020(13) 0.0057(15) 0.0030(15) N3B 0.053(2) 0.0370(16) 0.0360(16) 0.0061(13) 0.0122(15) 0.0086(15) N4B 0.054(2) 0.0458(19) 0.0461(19) -0.0043(15) 0.0134(17) 0.0066(16) N5B 0.0388(18) 0.0528(17) 0.0341(15) 0.0176(13) 0.0108(14) 0.0012(15) N6B 0.049(2) 0.0592(19) 0.0273(15) 0.0108(14) 0.0094(15) 0.0073(16) N7B 0.0488(19) 0.0466(18) 0.0483(18) 0.0139(14) 0.0198(15) -0.0004(16) C1B 0.063(3) 0.055(2) 0.051(2) 0.0148(19) 0.014(2) 0.017(2) C2B 0.065(3) 0.072(3) 0.068(3) 0.026(2) 0.029(2) 0.015(2) C3B 0.064(3) 0.080(3) 0.046(2) 0.0310(19) 0.024(2) 0.014(2) C4B 0.054(3) 0.067(3) 0.043(2) 0.0112(19) 0.0220(19) 0.009(2) C5B 0.037(2) 0.051(2) 0.0324(18) 0.0065(16) 0.0104(17) 0.0074(17) C6B 0.043(2) 0.044(2) 0.035(2) -0.0029(17) 0.0064(18) 0.0039(18) C7B 0.052(2) 0.053(2) 0.036(2) -0.0001(17) 0.0173(18) 0.0091(19) C8B 0.064(3) 0.041(2) 0.052(2) -0.0068(19) 0.014(2) 0.014(2) C9B 0.062(3) 0.033(2) 0.048(2) 0.0060(17) 0.005(2) 0.0137(19) C10B 0.037(2) 0.057(2) 0.033(2) 0.0054(17) -0.0015(18) 0.0092(19) C11B 0.040(2) 0.043(2) 0.0347(19) 0.0100(16) -0.0065(18) -0.0011(18) C12B 0.042(2) 0.060(2) 0.064(3) 0.017(2) 0.014(2) 0.010(2) C13B 0.060(3) 0.046(2) 0.066(3) 0.0187(19) 0.016(2) 0.005(2) C14B 0.049(2) 0.052(2) 0.046(2) 0.0147(17) 0.0142(19) 0.0064(19) C15B 0.042(2) 0.062(2) 0.038(2) 0.0078(19) 0.0060(19) 0.005(2) C16B 0.063(3) 0.035(2) 0.054(2) 0.0057(17) 0.028(2) 0.0081(19) C17B 0.071(3) 0.047(2) 0.061(3) 0.007(2) 0.014(2) -0.009(2) C18B 0.062(3) 0.023(2) 0.084(3) 0.0033(19) 0.022(2) 0.0009(19) C19B 0.065(3) 0.054(2) 0.069(3) 0.021(2) 0.025(2) 0.009(2) C20B 0.058(2) 0.047(2) 0.053(2) 0.0165(17) 0.0296(19) 0.0232(18) C21B 0.063(2) 0.051(2) 0.0403(19) 0.0157(16) 0.0261(18) 0.0266(18) C22B 0.058(2) 0.055(2) 0.042(2) 0.0059(18) 0.0211(19) 0.023(2) C23B 0.072(3) 0.071(2) 0.056(2) 0.0279(19) 0.030(2) 0.039(2) C24B 0.058(3) 0.058(2) 0.064(3) 0.018(2) 0.003(2) 0.011(2) C25B 0.049(2) 0.060(2) 0.039(2) 0.0184(17) 0.0104(19) 0.014(2) C26B 0.041(2) 0.053(2) 0.044(2) 0.0122(17) 0.0200(17) 0.0083(18) C27B 0.050(3) 0.086(3) 0.056(3) 0.030(2) -0.001(2) 0.003(2) C28B 0.043(3) 0.089(3) 0.061(3) 0.011(3) -0.001(2) -0.003(3) C29B 0.062(3) 0.044(2) 0.044(2) 0.0038(18) 0.017(2) -0.002(2) C30B 0.036(2) 0.050(2) 0.046(2) 0.0178(17) 0.0022(18) 0.0038(18) C31B 0.045(3) 0.061(3) 0.058(3) 0.015(2) 0.008(2) 0.003(2) C32B 0.075(3) 0.081(3) 0.0277(19) 0.0167(19) 0.004(2) -0.009(3) C33B 0.076(3) 0.075(3) 0.049(3) 0.011(2) 0.004(3) -0.016(3) C34B 0.074(3) 0.074(3) 0.035(2) 0.007(2) 0.014(2) 0.011(3) C35B 0.057(3) 0.050(2) 0.038(2) 0.0061(18) 0.008(2) 0.012(2) C36B 0.040(2) 0.078(3) 0.063(3) 0.008(2) 0.015(2) -0.008(2) C37B 0.054(3) 0.112(4) 0.041(2) 0.028(2) 0.018(2) 0.014(3) N8 0.115(4) 0.147(4) 0.078(3) 0.055(3) 0.007(3) -0.015(4) C39 0.104(5) 0.219(6) 0.139(5) 0.115(4) 0.035(4) 0.027(5) C40 0.073(3) 0.135(5) 0.101(4) 0.031(4) 0.032(3) 0.048(3) C41 0.170(5) 0.059(3) 0.083(3) 0.034(2) 0.068(3) 0.013(3) C42 0.105(5) 0.131(4) 0.064(3) 0.030(3) 0.012(3) -0.040(4) C43 0.065(3) 0.084(3) 0.057(3) 0.013(2) 0.002(3) 0.015(3) F3A 0.0496(14) 0.0667(15) 0.0671(16) 0.0013(13) 0.0182(13) -0.0051(12) F2A 0.0727(17) 0.0475(14) 0.0633(16) -0.0034(12) 0.0113(14) 0.0001(13) F5A 0.0524(15) 0.0669(16) 0.0721(17) 0.0005(13) 0.0144(14) 0.0008(13) F1A 0.0675(17) 0.0625(14) 0.0450(13) 0.0112(11) -0.0007(13) -0.0012(13) F5B 0.0598(17) 0.0959(18) 0.0571(15) 0.0241(13) 0.0053(14) -0.0007(15) F6A 0.0798(17) 0.0518(14) 0.0540(14) 0.0033(11) 0.0274(13) -0.0025(13) F4A 0.115(2) 0.0487(14) 0.0609(15) 0.0198(11) 0.0252(15) 0.0000(14) F2B 0.0719(18) 0.0843(18) 0.0490(15) -0.0012(13) 0.0126(14) 0.0000(15) F3B 0.087(2) 0.0649(16) 0.0685(17) 0.0083(13) 0.0175(16) -0.0103(15) F1B 0.0524(17) 0.101(2) 0.0711(19) -0.0092(16) 0.0052(15) -0.0116(16) F6B 0.108(3) 0.0650(17) 0.088(2) 0.0145(15) -0.004(2) -0.0143(17) F4B 0.0680(19) 0.187(3) 0.0726(18) 0.0426(19) 0.0242(15) -0.018(2) F8A 0.113(3) 0.103(2) 0.0612(17) 0.0294(15) -0.0201(18) -0.007(2) F9A 0.089(2) 0.159(3) 0.077(2) 0.029(2) 0.0319(17) -0.004(2) O8A 0.079(2) 0.088(2) 0.0531(18) 0.0220(16) 0.0142(17) -0.0059(19) O9B 0.122(3) 0.091(3) 0.072(2) -0.003(2) 0.038(2) -0.018(2) O9A 0.067(2) 0.146(4) 0.123(3) 0.020(3) 0.043(2) 0.012(3) F7A 0.205(5) 0.136(3) 0.189(4) 0.064(3) -0.048(4) -0.035(3) O8B 0.081(3) 0.451(9) 0.075(3) 0.079(4) 0.017(3) -0.012(5) O7B 0.118(4) 0.066(3) 0.270(7) -0.027(3) 0.056(4) 0.003(3) C38A 0.067(4) 0.148(5) 0.073(3) 0.044(3) 0.004(3) 0.006(4) O7A 0.281(7) 0.067(3) 0.262(7) -0.045(4) -0.116(6) 0.048(4) F8B 0.110(3) 0.154(3) 0.102(3) -0.013(2) 0.036(2) -0.042(2) F9B 0.181(4) 0.192(4) 0.086(3) 0.028(3) 0.022(3) -0.051(3) F7B 0.152(3) 0.173(4) 0.222(5) -0.048(4) 0.088(3) 0.038(3) C38B 0.104(4) 0.085(4) 0.070(3) -0.021(3) 0.029(3) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1A O1A 2.495(3) . ? U1A O4A 2.499(3) . ? U1A N4A 2.606(3) . ? U1A N1A 2.619(3) . ? U1A N2A 2.618(3) . ? U1A N5A 2.624(3) . ? U1A N3A 2.635(4) . ? U1A N6A 2.639(3) . ? U1A N7A 2.695(3) . ? S1A O2A 1.435(3) . ? S1A O3A 1.435(4) . ? S1A O1A 1.476(3) . ? S1A C36A 1.826(4) . ? S2A O6A 1.433(3) . ? S2A O5A 1.456(3) . ? S2A O4A 1.467(3) . ? S2A C37A 1.812(4) . ? S3A O9A 1.317(4) . ? S3A O8A 1.350(4) . ? S3A O7A 1.644(6) . ? S3A C38A 1.678(7) . ? N2A C6A 1.348(5) . ? N2A C10A 1.375(6) . ? N3A C11A 1.354(5) . ? N3A C15A 1.370(5) . ? N4A C16A 1.339(5) . ? N4A C20A 1.382(5) . ? N5A C25A 1.351(4) . ? N5A C21A 1.380(5) . ? N6A C30A 1.347(5) . ? N6A C26A 1.355(5) . ? N1A C5A 1.354(5) . ? N1A C1A 1.372(6) . ? N7A C35A 1.342(6) . ? N7A C31A 1.366(6) . ? C1A C2A 1.394(7) . ? C2A C3A 1.371(7) . ? C3A C4A 1.347(8) . ? C4A C5A 1.364(6) . ? C5A C6A 1.493(6) . ? C6A C7A 1.401(6) . ? C7A C8A 1.355(7) . ? C8A C9A 1.382(7) . ? C9A C10A 1.407(6) . ? C10A C11A 1.455(6) . ? C11A C12A 1.392(6) . ? C12A C13A 1.381(6) . ? C13A C14A 1.382(6) . ? C14A C15A 1.349(6) . ? C16A C17A 1.393(6) . ? C17A C18A 1.366(6) . ? C18A C19A 1.394(6) . ? C19A C20A 1.396(6) . ? C20A C21A 1.474(5) . ? C21A C22A 1.381(6) . ? C22A C23A 1.370(6) . ? C23A C24A 1.353(7) . ? C24A C25A 1.434(6) . ? C25A C26A 1.471(6) . ? C26A C27A 1.412(5) . ? C27A C28A 1.369(7) . ? C28A C29A 1.360(7) . ? C29A C30A 1.358(6) . ? C31A C32A 1.402(6) . ? C32A C33A 1.363(7) . ? C33A C34A 1.360(7) . ? C34A C35A 1.370(6) . ? C36A F3A 1.309(6) . ? C36A F1A 1.333(5) . ? C36A F2A 1.358(5) . ? C37A F5A 1.316(5) . ? C37A F4A 1.333(5) . ? C37A F6A 1.362(5) . ? U1B O1B 2.489(3) . ? U1B O4B 2.495(3) . ? U1B N5B 2.615(3) . ? U1B N2B 2.618(3) . ? U1B N6B 2.623(3) . ? U1B N4B 2.628(3) . ? U1B N3B 2.633(3) . ? U1B N1B 2.637(4) . ? U1B N7B 2.678(3) . ? S1B O3B 1.435(4) . ? S1B O2B 1.443(3) . ? S1B O1B 1.461(3) . ? S1B C36B 1.820(5) . ? S2B O6B 1.407(3) . ? S2B O5B 1.448(3) . ? S2B O4B 1.461(3) . ? S2B C37B 1.828(5) . ? S3B O7B 1.377(5) . ? S3B O8B 1.404(5) . ? S3B O9B 1.418(4) . ? S3B C38B 1.760(7) . ? N1B C5B 1.347(5) . ? N1B C1B 1.359(5) . ? N2B C6B 1.354(6) . ? N2B C10B 1.373(5) . ? N3B C11B 1.345(5) . ? N3B C15B 1.345(6) . ? N4B C16B 1.342(5) . ? N4B C20B 1.349(6) . ? N5B C25B 1.342(5) . ? N5B C21B 1.379(5) . ? N6B C30B 1.347(5) . ? N6B C26B 1.400(5) . ? N7B C31B 1.340(6) . ? N7B C35B 1.388(6) . ? C1B C2B 1.364(7) . ? C2B C3B 1.353(7) . ? C3B C4B 1.408(7) . ? C4B C5B 1.383(6) . ? C5B C6B 1.473(6) . ? C6B C7B 1.405(6) . ? C7B C8B 1.367(6) . ? C8B C9B 1.353(7) . ? C9B C10B 1.394(6) . ? C10B C11B 1.497(6) . ? C11B C12B 1.386(6) . ? C12B C13B 1.383(7) . ? C13B C14B 1.378(6) . ? C14B C15B 1.387(6) . ? C16B C17B 1.354(6) . ? C17B C18B 1.371(7) . ? C18B C19B 1.379(6) . ? C19B C20B 1.390(6) . ? C20B C21B 1.509(5) . ? C21B C22B 1.364(6) . ? C22B C23B 1.373(6) . ? C23B C24B 1.355(6) . ? C24B C25B 1.423(6) . ? C25B C26B 1.471(6) . ? C26B C27B 1.378(6) . ? C27B C28B 1.376(7) . ? C28B C29B 1.382(7) . ? C29B C30B 1.369(5) . ? C31B C32B 1.383(6) . ? C32B C33B 1.395(7) . ? C33B C34B 1.378(7) . ? C34B C35B 1.396(6) . ? C36B F1B 1.299(5) . ? C36B F3B 1.336(6) . ? C36B F2B 1.377(6) . ? C37B F6B 1.297(6) . ? C37B F4B 1.324(6) . ? C37B F5B 1.315(6) . ? N8 C39 1.2536 . ? N8 C43 1.2896 . ? C39 C40 1.2418 . ? C40 C41 1.4408 . ? C41 C42 1.5785 . ? C42 C43 1.4204 . ? F8A C38A 1.293(7) . ? F9A C38A 1.309(7) . ? F7A C38A 1.557(8) . ? F8B C38B 1.288(7) . ? F9B C38B 1.315(7) . ? F7B C38B 1.359(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A U1A O4A 142.46(9) . . ? O1A U1A N4A 74.41(9) . . ? O4A U1A N4A 92.50(10) . . ? O1A U1A N1A 71.90(10) . . ? O4A U1A N1A 142.42(9) . . ? N4A U1A N1A 82.79(11) . . ? O1A U1A N2A 70.45(9) . . ? O4A U1A N2A 131.18(10) . . ? N4A U1A N2A 136.30(10) . . ? N1A U1A N2A 62.28(11) . . ? O1A U1A N5A 128.89(10) . . ? O4A U1A N5A 68.66(10) . . ? N4A U1A N5A 62.69(9) . . ? N1A U1A N5A 76.23(10) . . ? N2A U1A N5A 125.55(9) . . ? O1A U1A N3A 97.04(10) . . ? O4A U1A N3A 75.70(10) . . ? N4A U1A N3A 148.35(10) . . ? N1A U1A N3A 124.21(10) . . ? N2A U1A N3A 62.55(10) . . ? N5A U1A N3A 134.03(10) . . ? O1A U1A N6A 143.61(9) . . ? O4A U1A N6A 72.34(9) . . ? N4A U1A N6A 125.14(10) . . ? N1A U1A N6A 80.11(10) . . ? N2A U1A N6A 76.18(9) . . ? N5A U1A N6A 62.68(10) . . ? N3A U1A N6A 79.70(10) . . ? O1A U1A N7A 71.04(10) . . ? O4A U1A N7A 71.60(9) . . ? N4A U1A N7A 75.01(11) . . ? N1A U1A N7A 140.65(10) . . ? N2A U1A N7A 115.52(10) . . ? N5A U1A N7A 118.93(10) . . ? N3A U1A N7A 73.41(10) . . ? N6A U1A N7A 139.15(10) . . ? O2A S1A O3A 116.4(2) . . ? O2A S1A O1A 114.52(18) . . ? O3A S1A O1A 113.61(18) . . ? O2A S1A C36A 104.8(2) . . ? O3A S1A C36A 104.2(2) . . ? O1A S1A C36A 101.01(18) . . ? O6A S2A O5A 117.89(18) . . ? O6A S2A O4A 113.02(19) . . ? O5A S2A O4A 112.75(17) . . ? O6A S2A C37A 105.34(18) . . ? O5A S2A C37A 103.27(18) . . ? O4A S2A C37A 102.44(17) . . ? O9A S3A O8A 126.2(3) . . ? O9A S3A O7A 109.7(4) . . ? O8A S3A O7A 106.9(3) . . ? O9A S3A C38A 109.4(3) . . ? O8A S3A C38A 112.1(3) . . ? O7A S3A C38A 84.4(4) . . ? S1A O1A U1A 143.75(16) . . ? S2A O4A U1A 149.78(16) . . ? C6A N2A C10A 119.1(3) . . ? C6A N2A U1A 120.2(3) . . ? C10A N2A U1A 120.4(3) . . ? C11A N3A C15A 117.3(4) . . ? C11A N3A U1A 121.1(3) . . ? C15A N3A U1A 121.5(3) . . ? C16A N4A C20A 116.8(3) . . ? C16A N4A U1A 121.0(3) . . ? C20A N4A U1A 122.2(2) . . ? C25A N5A C21A 118.0(3) . . ? C25A N5A U1A 120.3(3) . . ? C21A N5A U1A 121.0(2) . . ? C30A N6A C26A 117.5(3) . . ? C30A N6A U1A 122.0(2) . . ? C26A N6A U1A 120.1(2) . . ? C5A N1A C1A 115.4(4) . . ? C5A N1A U1A 121.6(3) . . ? C1A N1A U1A 121.0(3) . . ? C35A N7A C31A 114.9(4) . . ? C35A N7A U1A 125.2(3) . . ? C31A N7A U1A 119.8(3) . . ? N1A C1A C2A 124.3(4) . . ? C3A C2A C1A 115.8(5) . . ? C4A C3A C2A 121.9(5) . . ? C3A C4A C5A 119.3(4) . . ? N1A C5A C4A 123.2(4) . . ? N1A C5A C6A 114.2(4) . . ? C4A C5A C6A 122.6(4) . . ? N2A C6A C7A 121.1(4) . . ? N2A C6A C5A 119.0(4) . . ? C7A C6A C5A 119.9(4) . . ? C8A C7A C6A 120.3(4) . . ? C7A C8A C9A 119.7(4) . . ? C8A C9A C10A 119.2(4) . . ? N2A C10A C9A 120.6(4) . . ? N2A C10A C11A 118.2(4) . . ? C9A C10A C11A 121.3(4) . . ? N3A C11A C12A 120.8(4) . . ? N3A C11A C10A 117.4(4) . . ? C12A C11A C10A 121.8(4) . . ? C13A C12A C11A 120.5(4) . . ? C12A C13A C14A 118.4(4) . . ? C15A C14A C13A 119.0(4) . . ? C14A C15A N3A 124.0(4) . . ? N4A C16A C17A 124.7(4) . . ? C18A C17A C16A 117.3(4) . . ? C17A C18A C19A 120.8(4) . . ? C18A C19A C20A 118.5(4) . . ? N4A C20A C19A 121.7(3) . . ? N4A C20A C21A 116.4(4) . . ? C19A C20A C21A 122.0(4) . . ? N5A C21A C22A 122.1(3) . . ? N5A C21A C20A 117.1(3) . . ? C22A C21A C20A 120.9(4) . . ? C23A C22A C21A 119.0(4) . . ? C24A C23A C22A 121.2(4) . . ? C23A C24A C25A 118.4(4) . . ? N5A C25A C24A 121.2(4) . . ? N5A C25A C26A 118.4(3) . . ? C24A C25A C26A 120.4(3) . . ? N6A C26A C27A 120.9(4) . . ? N6A C26A C25A 117.4(3) . . ? C27A C26A C25A 121.6(4) . . ? C28A C27A C26A 119.1(4) . . ? C29A C28A C27A 119.4(4) . . ? C28A C29A C30A 119.7(5) . . ? N6A C30A C29A 123.4(4) . . ? N7A C31A C32A 124.5(4) . . ? C33A C32A C31A 116.9(4) . . ? C32A C33A C34A 119.9(4) . . ? C33A C34A C35A 120.0(4) . . ? N7A C35A C34A 123.6(4) . . ? F3A C36A F1A 109.1(4) . . ? F3A C36A F2A 106.0(4) . . ? F1A C36A F2A 108.7(3) . . ? F3A C36A S1A 111.8(3) . . ? F1A C36A S1A 111.6(3) . . ? F2A C36A S1A 109.5(3) . . ? F5A C37A F4A 108.5(4) . . ? F5A C37A F6A 108.5(3) . . ? F4A C37A F6A 105.9(3) . . ? F5A C37A S2A 112.8(3) . . ? F4A C37A S2A 110.8(3) . . ? F6A C37A S2A 110.1(3) . . ? O1B U1B O4B 144.53(9) . . ? O1B U1B N5B 126.93(10) . . ? O4B U1B N5B 69.47(10) . . ? O1B U1B N2B 71.14(9) . . ? O4B U1B N2B 129.82(10) . . ? N5B U1B N2B 124.32(10) . . ? O1B U1B N6B 143.12(10) . . ? O4B U1B N6B 70.89(10) . . ? N5B U1B N6B 63.51(10) . . ? N2B U1B N6B 75.19(10) . . ? O1B U1B N4B 74.33(11) . . ? O4B U1B N4B 92.35(11) . . ? N5B U1B N4B 62.61(10) . . ? N2B U1B N4B 137.78(11) . . ? N6B U1B N4B 126.07(11) . . ? O1B U1B N3B 96.76(10) . . ? O4B U1B N3B 75.97(11) . . ? N5B U1B N3B 136.25(10) . . ? N2B U1B N3B 62.73(11) . . ? N6B U1B N3B 80.55(10) . . ? N4B U1B N3B 146.07(10) . . ? O1B U1B N1B 71.41(10) . . ? O4B U1B N1B 140.98(10) . . ? N5B U1B N1B 74.52(11) . . ? N2B U1B N1B 62.55(10) . . ? N6B U1B N1B 80.10(10) . . ? N4B U1B N1B 83.98(11) . . ? N3B U1B N1B 124.90(11) . . ? O1B U1B N7B 71.51(10) . . ? O4B U1B N7B 73.25(10) . . ? N5B U1B N7B 120.00(10) . . ? N2B U1B N7B 115.67(10) . . ? N6B U1B N7B 139.05(11) . . ? N4B U1B N7B 74.04(11) . . ? N3B U1B N7B 72.10(10) . . ? N1B U1B N7B 140.73(10) . . ? O3B S1B O2B 116.4(2) . . ? O3B S1B O1B 112.7(2) . . ? O2B S1B O1B 115.61(19) . . ? O3B S1B C36B 103.7(2) . . ? O2B S1B C36B 103.8(2) . . ? O1B S1B C36B 102.17(19) . . ? O6B S2B O5B 116.9(2) . . ? O6B S2B O4B 113.3(2) . . ? O5B S2B O4B 113.54(18) . . ? O6B S2B C37B 105.2(2) . . ? O5B S2B C37B 104.2(2) . . ? O4B S2B C37B 101.62(19) . . ? O7B S3B O8B 106.4(4) . . ? O7B S3B O9B 112.6(3) . . ? O8B S3B O9B 121.1(4) . . ? O7B S3B C38B 101.0(4) . . ? O8B S3B C38B 105.0(3) . . ? O9B S3B C38B 108.6(3) . . ? S1B O1B U1B 146.18(16) . . ? S2B O4B U1B 156.88(16) . . ? C5B N1B C1B 116.6(4) . . ? C5B N1B U1B 120.1(3) . . ? C1B N1B U1B 121.6(3) . . ? C6B N2B C10B 117.5(4) . . ? C6B N2B U1B 120.8(2) . . ? C10B N2B U1B 121.4(3) . . ? C11B N3B C15B 117.3(4) . . ? C11B N3B U1B 121.3(3) . . ? C15B N3B U1B 121.2(3) . . ? C16B N4B C20B 116.3(3) . . ? C16B N4B U1B 121.3(3) . . ? C20B N4B U1B 122.4(2) . . ? C25B N5B C21B 116.9(3) . . ? C25B N5B U1B 120.8(3) . . ? C21B N5B U1B 121.8(2) . . ? C30B N6B C26B 117.2(3) . . ? C30B N6B U1B 122.9(3) . . ? C26B N6B U1B 119.5(2) . . ? C31B N7B C35B 116.2(4) . . ? C31B N7B U1B 121.8(3) . . ? C35B N7B U1B 122.0(3) . . ? N1B C1B C2B 125.1(5) . . ? C3B C2B C1B 117.1(5) . . ? C2B C3B C4B 120.8(5) . . ? C5B C4B C3B 118.0(4) . . ? N1B C5B C4B 122.3(4) . . ? N1B C5B C6B 117.5(4) . . ? C4B C5B C6B 120.1(4) . . ? N2B C6B C7B 121.9(4) . . ? N2B C6B C5B 117.8(4) . . ? C7B C6B C5B 120.3(4) . . ? C8B C7B C6B 119.0(4) . . ? C7B C8B C9B 120.1(4) . . ? C8B C9B C10B 119.8(4) . . ? N2B C10B C9B 121.5(4) . . ? N2B C10B C11B 116.5(4) . . ? C9B C10B C11B 122.0(4) . . ? N3B C11B C12B 122.7(4) . . ? N3B C11B C10B 117.6(4) . . ? C12B C11B C10B 119.7(4) . . ? C13B C12B C11B 118.1(4) . . ? C14B C13B C12B 120.7(4) . . ? C13B C14B C15B 116.9(4) . . ? N3B C15B C14B 124.1(4) . . ? N4B C16B C17B 124.2(4) . . ? C16B C17B C18B 119.3(4) . . ? C17B C18B C19B 118.8(4) . . ? C20B C19B C18B 118.4(4) . . ? N4B C20B C19B 122.9(4) . . ? N4B C20B C21B 116.6(3) . . ? C19B C20B C21B 120.5(4) . . ? C22B C21B N5B 123.0(4) . . ? C22B C21B C20B 120.8(4) . . ? N5B C21B C20B 116.1(4) . . ? C23B C22B C21B 118.9(4) . . ? C24B C23B C22B 120.7(4) . . ? C23B C24B C25B 118.3(4) . . ? N5B C25B C24B 122.2(4) . . ? N5B C25B C26B 118.9(4) . . ? C24B C25B C26B 119.0(3) . . ? C27B C26B N6B 119.8(4) . . ? C27B C26B C25B 123.1(4) . . ? N6B C26B C25B 117.0(3) . . ? C28B C27B C26B 121.5(4) . . ? C27B C28B C29B 118.5(4) . . ? C30B C29B C28B 119.0(4) . . ? N6B C30B C29B 124.0(4) . . ? N7B C31B C32B 125.6(5) . . ? C31B C32B C33B 117.0(5) . . ? C34B C33B C32B 119.9(5) . . ? C33B C34B C35B 119.5(5) . . ? N7B C35B C34B 121.6(4) . . ? F1B C36B F3B 108.6(4) . . ? F1B C36B F2B 108.7(4) . . ? F3B C36B F2B 105.2(4) . . ? F1B C36B S1B 112.9(3) . . ? F3B C36B S1B 111.1(3) . . ? F2B C36B S1B 110.0(3) . . ? F6B C37B F4B 106.2(5) . . ? F6B C37B F5B 111.3(4) . . ? F4B C37B F5B 107.2(4) . . ? F6B C37B S2B 112.2(4) . . ? F4B C37B S2B 109.6(3) . . ? F5B C37B S2B 110.1(4) . . ? C39 N8 C43 120.5 . . ? C40 C39 N8 123.6 . . ? C39 C40 C41 125.1 . . ? C40 C41 C42 113.5 . . ? C43 C42 C41 108.2 . . ? N8 C43 C42 129.0 . . ? F8A C38A F9A 112.2(5) . . ? F8A C38A F7A 98.2(5) . . ? F9A C38A F7A 88.2(5) . . ? F8A C38A S3A 123.5(5) . . ? F9A C38A S3A 122.1(5) . . ? F7A C38A S3A 97.9(4) . . ? F8B C38B F9B 112.2(6) . . ? F8B C38B F7B 109.4(6) . . ? F9B C38B F7B 92.7(5) . . ? F8B C38B S3B 116.8(4) . . ? F9B C38B S3B 113.5(5) . . ? F7B C38B S3B 109.5(5) . . ? #===END data_7.2py _database_code_depnum_ccdc_archive 'CCDC 251217' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H34 Ce F9 N8 O10 S3' _chemical_formula_weight 1230.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 9.1240(18) _cell_length_b 25.703(5) _cell_length_c 21.133(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.36(3) _cell_angle_gamma 90.00 _cell_volume 4875.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 29862 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29862 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 24.72 _reflns_number_total 7840 _reflns_number_gt 5993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0382P)^2^+9.6554P] 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 7840 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.723 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.097 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 Ce Ce 1.21596(3) 0.969392(10) 0.250140(12) 0.01663(9) Uani 1 1 d . . . S1 S 1.43743(13) 0.97786(5) 0.12266(6) 0.0217(3) Uani 1 1 d . . . S2 S 1.16070(13) 1.05503(5) 0.38934(6) 0.0219(3) Uani 1 1 d . . . S3 S 0.71278(16) 0.75134(5) 0.44826(6) 0.0323(3) Uani 1 1 d . . . F1 F 1.5937(3) 0.89708(13) 0.09798(15) 0.0452(9) Uani 1 1 d . . . F2 F 1.5055(4) 0.94335(13) 0.01552(14) 0.0437(8) Uani 1 1 d . . . F3 F 1.3610(3) 0.89298(12) 0.05648(14) 0.0400(8) Uani 1 1 d . . . F4 F 1.1268(4) 1.14481(13) 0.33038(17) 0.0512(9) Uani 1 1 d . . . F5 F 1.0882(4) 1.14646(14) 0.42758(17) 0.0562(10) Uani 1 1 d . . . F6 F 0.9250(4) 1.11265(14) 0.35298(17) 0.0522(9) Uani 1 1 d . . . F7 F 0.4426(5) 0.7679(3) 0.4661(3) 0.130(2) Uani 1 1 d . . . F8 F 0.5484(9) 0.8335(2) 0.4338(3) 0.156(3) Uani 1 1 d . . . F9 F 0.6039(5) 0.80877(17) 0.5309(2) 0.0718(12) Uani 1 1 d . . . O1 O 1.4019(3) 0.94961(13) 0.17796(15) 0.0224(7) Uani 1 1 d . . . O2 O 1.3110(4) 1.00377(14) 0.08558(16) 0.0275(8) Uani 1 1 d . . . O3 O 1.5743(4) 1.00634(15) 0.13606(17) 0.0345(9) Uani 1 1 d . . . O4 O 1.1186(3) 1.02990(13) 0.32654(14) 0.0221(7) Uani 1 1 d . . . O5 O 1.3169(4) 1.06686(14) 0.40677(17) 0.0319(9) Uani 1 1 d . . . O6 O 1.0915(4) 1.03269(15) 0.43862(16) 0.0331(8) Uani 1 1 d . . . O7 O 0.6612(5) 0.74141(17) 0.38150(18) 0.0492(11) Uani 1 1 d . . . O8 O 0.7163(5) 0.70772(16) 0.4901(2) 0.0531(11) Uani 1 1 d . . . O9 O 0.8448(5) 0.78358(17) 0.4620(2) 0.0546(12) Uani 1 1 d . . . O10 O 1.3292(4) 1.05478(13) 0.23348(16) 0.0251(8) Uani 1 1 d . . . N1 N 1.2519(4) 0.86717(15) 0.23330(18) 0.0207(9) Uani 1 1 d . . . N2 N 1.0728(4) 0.92603(15) 0.14138(17) 0.0186(9) Uani 1 1 d . . . N3 N 1.0115(4) 1.02488(16) 0.17425(18) 0.0221(9) Uani 1 1 d . . . N4 N 1.4801(4) 0.97207(16) 0.32705(18) 0.0220(9) Uani 1 1 d . . . N5 N 1.2441(4) 0.92673(15) 0.36716(18) 0.0189(9) Uani 1 1 d . . . N6 N 0.9768(4) 0.92180(16) 0.28019(18) 0.0217(9) Uani 1 1 d . . . N7 N 1.3147(5) 1.13092(18) 0.1434(2) 0.0380(11) Uani 1 1 d . . . N8 N -0.4549(5) 1.1251(2) 0.2925(2) 0.0442(13) Uani 1 1 d . . . C1 C 1.3468(5) 0.83933(19) 0.2759(2) 0.0254(11) Uani 1 1 d . . . H1A H 1.3761 0.8531 0.3170 0.030 Uiso 1 1 calc R . . C2 C 1.4039(6) 0.7917(2) 0.2630(3) 0.0327(13) Uani 1 1 d . . . H2B H 1.4652 0.7731 0.2951 0.039 Uiso 1 1 calc R . . C3 C 1.3676(6) 0.7723(2) 0.2012(3) 0.0420(15) Uani 1 1 d . . . H3B H 1.4094 0.7414 0.1901 0.050 Uiso 1 1 calc R . . C4 C 1.2685(6) 0.7996(2) 0.1561(3) 0.0392(14) Uani 1 1 d . . . H4A H 1.2417 0.7870 0.1143 0.047 Uiso 1 1 calc R . . C5 C 1.2083(5) 0.84662(19) 0.1741(2) 0.0264(12) Uani 1 1 d . . . C6 C 1.0951(5) 0.87562(19) 0.1281(2) 0.0243(11) Uani 1 1 d . . . C7 C 1.0197(6) 0.8518(2) 0.0731(2) 0.0310(12) Uani 1 1 d . . . H7C H 1.0363 0.8168 0.0654 0.037 Uiso 1 1 calc R . . C8 C 0.9209(6) 0.8797(2) 0.0301(3) 0.0344(13) Uani 1 1 d . . . H8C H 0.8693 0.8639 -0.0068 0.041 Uiso 1 1 calc R . . C9 C 0.8976(5) 0.9317(2) 0.0416(2) 0.0290(12) Uani 1 1 d . . . H9B H 0.8320 0.9514 0.0124 0.035 Uiso 1 1 calc R . . C10 C 0.9755(5) 0.95394(19) 0.0984(2) 0.0216(11) Uani 1 1 d . . . C11 C 0.9518(5) 1.0090(2) 0.1141(2) 0.0207(11) Uani 1 1 d . . . C12 C 0.8716(6) 1.0433(2) 0.0698(2) 0.0285(12) Uani 1 1 d . . . H12A H 0.8318 1.0318 0.0286 0.034 Uiso 1 1 calc R . . C13 C 0.8508(6) 1.0943(2) 0.0870(2) 0.0317(13) Uani 1 1 d . . . H13A H 0.7977 1.1174 0.0577 0.038 Uiso 1 1 calc R . . C14 C 0.9106(6) 1.1098(2) 0.1483(3) 0.0300(12) Uani 1 1 d . . . H14A H 0.8981 1.1438 0.1615 0.036 Uiso 1 1 calc R . . C15 C 0.9891(5) 1.0744(2) 0.1898(2) 0.0284(12) Uani 1 1 d . . . H15A H 1.0292 1.0855 0.2312 0.034 Uiso 1 1 calc R . . C16 C 1.5984(5) 0.9917(2) 0.3058(2) 0.0258(11) Uani 1 1 d . . . H16A H 1.5866 1.0020 0.2630 0.031 Uiso 1 1 calc R . . C17 C 1.7376(5) 0.9974(2) 0.3443(2) 0.0264(12) Uani 1 1 d . . . H17A H 1.8164 1.0116 0.3278 0.032 Uiso 1 1 calc R . . C18 C 1.7567(6) 0.9816(2) 0.4070(2) 0.0294(13) Uani 1 1 d . . . H18A H 1.8492 0.9847 0.4337 0.035 Uiso 1 1 calc R . . C19 C 1.6362(5) 0.96098(19) 0.4303(2) 0.0238(11) Uani 1 1 d . . . H19A H 1.6477 0.9496 0.4727 0.029 Uiso 1 1 calc R . . C20 C 1.4983(5) 0.95742(19) 0.3899(2) 0.0216(11) Uani 1 1 d . . . C21 C 1.3661(5) 0.93609(19) 0.4125(2) 0.0209(11) Uani 1 1 d . . . C22 C 1.3680(5) 0.9262(2) 0.4772(2) 0.0258(12) Uani 1 1 d . . . H22A H 1.4529 0.9334 0.5075 0.031 Uiso 1 1 calc R . . C23 C 1.2428(6) 0.9057(2) 0.4962(2) 0.0310(12) Uani 1 1 d . . . H23A H 1.2416 0.8996 0.5395 0.037 Uiso 1 1 calc R . . C24 C 1.1195(6) 0.8946(2) 0.4501(2) 0.0284(12) Uani 1 1 d . . . H24A H 1.0346 0.8803 0.4617 0.034 Uiso 1 1 calc R . . C25 C 1.1243(5) 0.90500(19) 0.3859(2) 0.0221(11) Uani 1 1 d . . . C26 C 0.9915(5) 0.8947(2) 0.3355(2) 0.0250(11) Uani 1 1 d . . . C27 C 0.8864(5) 0.8583(2) 0.3464(3) 0.0333(13) Uani 1 1 d . . . H27A H 0.9016 0.8389 0.3842 0.040 Uiso 1 1 calc R . . C28 C 0.7601(6) 0.8509(2) 0.3012(3) 0.0410(15) Uani 1 1 d . . . H28A H 0.6901 0.8260 0.3073 0.049 Uiso 1 1 calc R . . C29 C 0.7390(5) 0.8813(2) 0.2464(3) 0.0343(13) Uani 1 1 d . . . H29A H 0.6519 0.8786 0.2160 0.041 Uiso 1 1 calc R . . C30 C 0.8502(5) 0.9158(2) 0.2375(2) 0.0241(11) Uani 1 1 d . . . H30A H 0.8364 0.9357 0.2001 0.029 Uiso 1 1 calc R . . C31 C 1.4759(6) 0.9252(2) 0.0706(2) 0.0292(12) Uani 1 1 d . . . C32 C 1.0719(6) 1.1181(2) 0.3745(3) 0.0370(14) Uani 1 1 d . . . C33 C 0.5733(8) 0.7929(3) 0.4700(3) 0.0575(19) Uani 1 1 d . . . C34 C 1.4015(6) 1.1300(2) 0.0987(3) 0.0367(14) Uani 1 1 d . . . H34A H 1.4349 1.0980 0.0866 0.044 Uiso 1 1 calc R . . C35 C 1.4434(6) 1.1741(2) 0.0701(3) 0.0396(14) Uani 1 1 d . . . H35A H 1.5020 1.1719 0.0384 0.048 Uiso 1 1 calc R . . C36 C 1.3982(7) 1.2207(2) 0.0886(3) 0.0530(18) Uani 1 1 d . . . H36A H 1.4278 1.2512 0.0707 0.064 Uiso 1 1 calc R . . C37 C 1.3080(8) 1.2228(3) 0.1340(4) 0.068(2) Uani 1 1 d . . . H37A H 1.2727 1.2543 0.1466 0.082 Uiso 1 1 calc R . . C38 C 1.2717(7) 1.1768(2) 0.1600(3) 0.0505(17) Uani 1 1 d . . . H38A H 1.2128 1.1782 0.1916 0.061 Uiso 1 1 calc R . . C39 C -0.4647(7) 1.1548(3) 0.3428(3) 0.0477(16) Uani 1 1 d . . . H39A H -0.5188 1.1430 0.3733 0.057 Uiso 1 1 calc R . . C40 C -0.3967(8) 1.2027(3) 0.3511(4) 0.065(2) Uani 1 1 d . . . H40A H -0.3990 1.2216 0.3885 0.077 Uiso 1 1 calc R . . C41 C -0.3267(9) 1.2223(3) 0.3054(4) 0.067(2) Uani 1 1 d . . . H41A H -0.2871 1.2558 0.3096 0.081 Uiso 1 1 calc R . . C42 C -0.3145(7) 1.1935(3) 0.2540(3) 0.0536(18) Uani 1 1 d . . . H42A H -0.2643 1.2060 0.2225 0.064 Uiso 1 1 calc R . . C43 C -0.3778(7) 1.1448(3) 0.2488(3) 0.0477(16) Uani 1 1 d . . . H43A H -0.3673 1.1244 0.2135 0.057 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 Ce 0.01695(14) 0.01987(15) 0.01259(14) 0.00016(12) 0.00136(9) -0.00071(12) S1 0.0226(6) 0.0263(7) 0.0163(6) 0.0005(5) 0.0039(5) -0.0009(5) S2 0.0227(6) 0.0259(7) 0.0169(6) -0.0004(5) 0.0024(5) 0.0000(5) S3 0.0475(9) 0.0262(8) 0.0239(7) 0.0037(6) 0.0081(6) 0.0006(6) F1 0.0451(19) 0.058(2) 0.0330(19) -0.0008(16) 0.0076(15) 0.0251(17) F2 0.063(2) 0.052(2) 0.0206(17) 0.0016(15) 0.0198(15) 0.0057(17) F3 0.050(2) 0.039(2) 0.0313(18) -0.0108(15) 0.0084(15) -0.0069(15) F4 0.074(2) 0.0278(19) 0.051(2) 0.0095(17) 0.0092(19) 0.0019(17) F5 0.073(2) 0.042(2) 0.048(2) -0.0264(18) -0.0015(18) 0.0149(18) F6 0.0370(19) 0.051(2) 0.064(2) -0.0080(19) -0.0054(17) 0.0178(16) F7 0.041(3) 0.210(7) 0.137(5) -0.062(5) 0.011(3) 0.006(3) F8 0.279(8) 0.114(5) 0.094(4) 0.051(4) 0.087(5) 0.153(6) F9 0.081(3) 0.083(3) 0.061(3) -0.028(2) 0.037(2) 0.001(2) O1 0.0236(18) 0.030(2) 0.0149(17) 0.0003(14) 0.0057(14) 0.0001(14) O2 0.0277(19) 0.030(2) 0.0235(19) 0.0041(16) 0.0003(15) 0.0044(15) O3 0.026(2) 0.048(2) 0.030(2) -0.0001(18) 0.0049(16) -0.0139(17) O4 0.0300(18) 0.0238(18) 0.0116(16) -0.0033(15) 0.0012(13) 0.0050(15) O5 0.0217(18) 0.041(2) 0.030(2) 0.0025(17) -0.0036(15) -0.0078(16) O6 0.037(2) 0.045(2) 0.0182(18) 0.0061(18) 0.0071(15) -0.0043(18) O7 0.067(3) 0.054(3) 0.022(2) -0.001(2) -0.0043(19) 0.011(2) O8 0.079(3) 0.039(3) 0.043(3) 0.013(2) 0.015(2) 0.003(2) O9 0.059(3) 0.059(3) 0.050(3) -0.009(2) 0.021(2) -0.019(2) O10 0.0293(19) 0.0231(19) 0.0230(19) -0.0005(15) 0.0051(15) -0.0058(15) N1 0.020(2) 0.024(2) 0.019(2) -0.0021(18) 0.0062(17) -0.0025(16) N2 0.017(2) 0.024(2) 0.014(2) -0.0021(17) 0.0016(16) -0.0030(16) N3 0.023(2) 0.027(3) 0.017(2) 0.0012(18) 0.0030(16) 0.0013(17) N4 0.020(2) 0.029(2) 0.016(2) 0.0004(19) 0.0038(16) -0.0010(18) N5 0.018(2) 0.021(2) 0.018(2) 0.0043(17) 0.0029(17) 0.0023(16) N6 0.019(2) 0.028(2) 0.019(2) 0.0015(18) 0.0045(17) -0.0029(17) N7 0.044(3) 0.033(3) 0.037(3) 0.006(2) 0.007(2) -0.005(2) N8 0.038(3) 0.052(3) 0.041(3) 0.003(3) 0.004(2) -0.005(2) C1 0.025(3) 0.027(3) 0.023(3) 0.001(2) 0.002(2) -0.003(2) C2 0.034(3) 0.024(3) 0.037(3) 0.006(2) -0.003(2) 0.003(2) C3 0.046(3) 0.030(3) 0.045(4) -0.009(3) -0.006(3) 0.007(3) C4 0.047(3) 0.029(3) 0.036(3) -0.010(3) -0.006(3) 0.001(3) C5 0.027(3) 0.020(3) 0.032(3) -0.003(2) 0.005(2) 0.002(2) C6 0.024(3) 0.026(3) 0.024(3) -0.006(2) 0.006(2) -0.001(2) C7 0.036(3) 0.029(3) 0.026(3) -0.008(2) -0.001(2) -0.001(2) C8 0.034(3) 0.041(4) 0.024(3) -0.012(3) -0.005(2) 0.000(2) C9 0.025(3) 0.043(4) 0.017(3) -0.001(2) -0.002(2) -0.001(2) C10 0.019(3) 0.035(3) 0.011(2) 0.002(2) 0.004(2) -0.003(2) C11 0.013(2) 0.034(3) 0.016(3) 0.003(2) 0.0035(19) -0.002(2) C12 0.029(3) 0.037(3) 0.019(3) 0.005(2) 0.000(2) 0.004(2) C13 0.029(3) 0.038(3) 0.026(3) 0.010(3) 0.000(2) 0.009(2) C14 0.032(3) 0.026(3) 0.032(3) 0.006(2) 0.006(2) 0.007(2) C15 0.032(3) 0.030(3) 0.021(3) 0.003(2) -0.002(2) 0.004(2) C16 0.024(3) 0.034(3) 0.021(3) -0.001(2) 0.008(2) 0.001(2) C17 0.020(3) 0.033(3) 0.027(3) -0.008(2) 0.006(2) -0.001(2) C18 0.023(3) 0.038(4) 0.025(3) -0.006(2) -0.002(2) 0.000(2) C19 0.022(3) 0.031(3) 0.017(3) 0.003(2) 0.000(2) 0.000(2) C20 0.022(3) 0.028(3) 0.013(2) -0.003(2) 0.0007(19) 0.002(2) C21 0.017(2) 0.025(3) 0.020(3) 0.001(2) 0.001(2) 0.0052(19) C22 0.024(3) 0.037(3) 0.016(3) 0.003(2) 0.000(2) 0.005(2) C23 0.034(3) 0.042(3) 0.018(3) 0.004(2) 0.007(2) 0.004(2) C24 0.027(3) 0.038(3) 0.020(3) 0.007(2) 0.002(2) 0.000(2) C25 0.020(3) 0.027(3) 0.019(3) 0.003(2) 0.002(2) 0.005(2) C26 0.019(3) 0.030(3) 0.027(3) 0.001(2) 0.005(2) 0.001(2) C27 0.026(3) 0.039(3) 0.034(3) 0.016(3) 0.003(2) -0.007(2) C28 0.025(3) 0.047(4) 0.048(4) 0.019(3) -0.002(3) -0.011(3) C29 0.022(3) 0.042(3) 0.035(3) 0.004(3) -0.007(2) -0.008(2) C30 0.019(2) 0.034(3) 0.020(3) 0.004(2) 0.005(2) -0.001(2) C31 0.032(3) 0.037(3) 0.019(3) 0.000(2) 0.006(2) 0.004(2) C32 0.042(4) 0.035(3) 0.032(3) -0.013(3) 0.002(3) 0.005(3) C33 0.057(5) 0.074(5) 0.043(4) 0.011(4) 0.016(3) 0.020(4) C34 0.054(4) 0.026(3) 0.031(3) 0.001(3) 0.009(3) 0.000(3) C35 0.046(4) 0.038(4) 0.037(3) 0.003(3) 0.014(3) -0.005(3) C36 0.061(4) 0.031(4) 0.071(5) 0.014(3) 0.022(4) 0.002(3) C37 0.073(5) 0.039(4) 0.106(7) 0.011(4) 0.054(5) 0.013(3) C38 0.050(4) 0.037(4) 0.072(5) 0.007(3) 0.032(3) 0.006(3) C39 0.051(4) 0.061(5) 0.036(4) -0.001(3) 0.019(3) -0.007(3) C40 0.082(5) 0.053(5) 0.067(5) -0.018(4) 0.035(4) -0.027(4) C41 0.083(6) 0.045(5) 0.079(6) 0.002(4) 0.029(5) -0.018(4) C42 0.050(4) 0.064(5) 0.051(4) 0.013(4) 0.020(3) -0.004(3) C43 0.044(4) 0.057(4) 0.043(4) -0.001(3) 0.011(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O10 2.478(3) . ? Ce O4 2.516(3) . ? Ce O1 2.529(3) . ? Ce N3 2.648(4) . ? Ce N4 2.655(4) . ? Ce N2 2.674(4) . ? Ce N5 2.675(4) . ? Ce N6 2.676(4) . ? Ce N1 2.679(4) . ? S1 O3 1.432(3) . ? S1 O2 1.437(3) . ? S1 O1 1.461(3) . ? S1 C31 1.818(5) . ? S2 O6 1.431(3) . ? S2 O5 1.439(3) . ? S2 O4 1.464(3) . ? S2 C32 1.814(6) . ? S3 O8 1.425(4) . ? S3 O7 1.428(4) . ? S3 O9 1.448(4) . ? S3 C33 1.784(7) . ? F1 C31 1.338(6) . ? F2 C31 1.326(6) . ? F3 C31 1.326(6) . ? F4 C32 1.327(7) . ? F5 C32 1.324(6) . ? F6 C32 1.343(6) . ? F7 C33 1.344(9) . ? F8 C33 1.289(8) . ? F9 C33 1.331(8) . ? N1 C1 1.339(6) . ? N1 C5 1.350(6) . ? N2 C6 1.349(6) . ? N2 C10 1.356(6) . ? N3 C15 1.340(6) . ? N3 C11 1.353(6) . ? N4 C16 1.340(6) . ? N4 C20 1.363(6) . ? N5 C25 1.348(6) . ? N5 C21 1.353(6) . ? N6 C30 1.341(6) . ? N6 C26 1.346(6) . ? N7 C38 1.311(7) . ? N7 C34 1.336(7) . ? N8 C39 1.326(7) . ? N8 C43 1.356(7) . ? C1 C2 1.377(7) . ? C2 C3 1.382(8) . ? C3 C4 1.381(8) . ? C4 C5 1.408(7) . ? C5 C6 1.485(7) . ? C6 C7 1.385(7) . ? C7 C8 1.364(7) . ? C8 C9 1.380(7) . ? C9 C10 1.402(7) . ? C10 C11 1.479(7) . ? C11 C12 1.393(7) . ? C12 C13 1.380(7) . ? C13 C14 1.372(7) . ? C14 C15 1.373(7) . ? C16 C17 1.387(7) . ? C17 C18 1.366(7) . ? C18 C19 1.388(7) . ? C19 C20 1.390(7) . ? C20 C21 1.480(7) . ? C21 C22 1.389(7) . ? C22 C23 1.382(7) . ? C23 C24 1.380(7) . ? C24 C25 1.392(7) . ? C25 C26 1.486(7) . ? C26 C27 1.389(7) . ? C27 C28 1.371(7) . ? C28 C29 1.381(7) . ? C29 C30 1.385(7) . ? C34 C35 1.374(8) . ? C35 C36 1.347(8) . ? C36 C37 1.373(9) . ? C37 C38 1.369(9) . ? C39 C40 1.375(9) . ? C40 C41 1.349(9) . ? C41 C42 1.337(10) . ? C42 C43 1.374(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Ce O4 75.41(11) . . ? O10 Ce O1 75.54(11) . . ? O4 Ce O1 149.77(11) . . ? O10 Ce N3 72.73(12) . . ? O4 Ce N3 76.36(11) . . ? O1 Ce N3 102.65(11) . . ? O10 Ce N4 73.03(12) . . ? O4 Ce N4 88.72(11) . . ? O1 Ce N4 74.98(11) . . ? N3 Ce N4 145.10(12) . . ? O10 Ce N2 113.50(11) . . ? O4 Ce N2 129.40(11) . . ? O1 Ce N2 71.02(11) . . ? N3 Ce N2 61.43(12) . . ? N4 Ce N2 141.86(12) . . ? O10 Ce N5 121.42(11) . . ? O4 Ce N5 69.29(11) . . ? O1 Ce N5 120.80(11) . . ? N3 Ce N5 136.12(11) . . ? N4 Ce N5 61.25(11) . . ? N2 Ce N5 125.07(12) . . ? O10 Ce N6 144.82(12) . . ? O4 Ce N6 74.52(12) . . ? O1 Ce N6 135.68(11) . . ? N3 Ce N6 82.77(12) . . ? N4 Ce N6 123.78(12) . . ? N2 Ce N6 73.75(11) . . ? N5 Ce N6 62.61(12) . . ? O10 Ce N1 141.78(11) . . ? O4 Ce N1 139.21(11) . . ? O1 Ce N1 67.13(11) . . ? N3 Ce N1 122.51(12) . . ? N4 Ce N1 89.28(12) . . ? N2 Ce N1 61.95(12) . . ? N5 Ce N1 74.17(11) . . ? N6 Ce N1 73.00(12) . . ? O3 S1 O2 117.2(2) . . ? O3 S1 O1 114.0(2) . . ? O2 S1 O1 113.3(2) . . ? O3 S1 C31 104.1(2) . . ? O2 S1 C31 103.8(2) . . ? O1 S1 C31 102.0(2) . . ? O6 S2 O5 116.4(2) . . ? O6 S2 O4 113.8(2) . . ? O5 S2 O4 114.3(2) . . ? O6 S2 C32 104.0(3) . . ? O5 S2 C32 104.3(2) . . ? O4 S2 C32 101.6(2) . . ? O8 S3 O7 116.1(3) . . ? O8 S3 O9 113.6(3) . . ? O7 S3 O9 114.6(3) . . ? O8 S3 C33 104.4(3) . . ? O7 S3 C33 103.8(3) . . ? O9 S3 C33 102.2(3) . . ? S1 O1 Ce 130.69(19) . . ? S2 O4 Ce 142.09(19) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Ce 120.9(3) . . ? C5 N1 Ce 119.0(3) . . ? C6 N2 C10 118.3(4) . . ? C6 N2 Ce 120.7(3) . . ? C10 N2 Ce 121.0(3) . . ? C15 N3 C11 117.6(4) . . ? C15 N3 Ce 119.0(3) . . ? C11 N3 Ce 121.8(3) . . ? C16 N4 C20 117.8(4) . . ? C16 N4 Ce 120.1(3) . . ? C20 N4 Ce 121.9(3) . . ? C25 N5 C21 118.3(4) . . ? C25 N5 Ce 119.5(3) . . ? C21 N5 Ce 120.8(3) . . ? C30 N6 C26 117.6(4) . . ? C30 N6 Ce 122.2(3) . . ? C26 N6 Ce 119.0(3) . . ? C38 N7 C34 116.7(5) . . ? C39 N8 C43 116.7(6) . . ? N1 C1 C2 124.3(5) . . ? C1 C2 C3 118.2(5) . . ? C4 C3 C2 119.1(5) . . ? C3 C4 C5 119.2(5) . . ? N1 C5 C4 121.5(5) . . ? N1 C5 C6 117.7(4) . . ? C4 C5 C6 120.8(5) . . ? N2 C6 C7 122.0(5) . . ? N2 C6 C5 117.4(4) . . ? C7 C6 C5 120.7(5) . . ? C8 C7 C6 119.7(5) . . ? C7 C8 C9 119.8(5) . . ? C8 C9 C10 118.4(5) . . ? N2 C10 C9 121.9(5) . . ? N2 C10 C11 117.4(4) . . ? C9 C10 C11 120.7(4) . . ? N3 C11 C12 120.9(5) . . ? N3 C11 C10 116.7(4) . . ? C12 C11 C10 122.4(4) . . ? C13 C12 C11 120.3(5) . . ? C14 C13 C12 118.3(5) . . ? C13 C14 C15 118.9(5) . . ? N3 C15 C14 123.9(5) . . ? N4 C16 C17 123.4(5) . . ? C18 C17 C16 118.8(5) . . ? C17 C18 C19 119.1(5) . . ? C18 C19 C20 119.7(5) . . ? N4 C20 C19 121.2(4) . . ? N4 C20 C21 116.9(4) . . ? C19 C20 C21 121.9(4) . . ? N5 C21 C22 121.9(4) . . ? N5 C21 C20 116.9(4) . . ? C22 C21 C20 121.2(4) . . ? C23 C22 C21 119.4(5) . . ? C24 C23 C22 119.1(5) . . ? C23 C24 C25 119.0(5) . . ? N5 C25 C24 122.3(4) . . ? N5 C25 C26 117.6(4) . . ? C24 C25 C26 120.0(4) . . ? N6 C26 C27 122.0(5) . . ? N6 C26 C25 118.1(4) . . ? C27 C26 C25 120.0(5) . . ? C28 C27 C26 119.7(5) . . ? C27 C28 C29 118.7(5) . . ? C28 C29 C30 118.7(5) . . ? N6 C30 C29 123.1(5) . . ? F2 C31 F3 107.5(4) . . ? F2 C31 F1 107.1(4) . . ? F3 C31 F1 107.5(4) . . ? F2 C31 S1 111.2(4) . . ? F3 C31 S1 111.7(3) . . ? F1 C31 S1 111.6(3) . . ? F5 C32 F4 108.1(5) . . ? F5 C32 F6 107.3(4) . . ? F4 C32 F6 107.2(5) . . ? F5 C32 S2 111.5(4) . . ? F4 C32 S2 111.8(4) . . ? F6 C32 S2 110.7(4) . . ? F8 C33 F9 108.0(7) . . ? F8 C33 F7 106.9(7) . . ? F9 C33 F7 103.6(5) . . ? F8 C33 S3 113.0(5) . . ? F9 C33 S3 113.4(5) . . ? F7 C33 S3 111.3(6) . . ? N7 C34 C35 122.9(5) . . ? C36 C35 C34 118.9(6) . . ? C35 C36 C37 119.3(6) . . ? C38 C37 C36 117.9(6) . . ? N7 C38 C37 124.2(6) . . ? N8 C39 C40 121.7(6) . . ? C41 C40 C39 120.3(7) . . ? C42 C41 C40 119.6(7) . . ? C41 C42 C43 118.3(6) . . ? N8 C43 C42 123.3(6) . . ? #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 251218' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H22 Ce F9 N6 O9 S3' _chemical_formula_weight 1053.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.630(2) _cell_length_b 11.749(2) _cell_length_c 15.546(3) _cell_angle_alpha 85.14(3) _cell_angle_beta 88.79(3) _cell_angle_gamma 70.03(3) _cell_volume 1989.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12295 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10s exposure by frame.The crystal to detector distance was 30mm ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12295 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 24.72 _reflns_number_total 6240 _reflns_number_gt 5000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0724P)^2^+9.8521P] 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 6240 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.949 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.148 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 Ce Ce 0.73398(4) 1.77639(4) 0.75235(3) 0.02044(15) Uani 1 1 d . . . S1 S 0.54728(17) 2.12359(17) 0.71247(11) 0.0237(4) Uani 1 1 d . . . S2 S 1.0592(2) 1.5577(2) 0.73166(17) 0.0509(7) Uani 1 1 d . . . S3 S 0.96860(17) 1.94175(19) 0.76296(13) 0.0302(5) Uani 1 1 d . . . F1 F 0.3332(5) 2.2631(5) 0.6518(4) 0.0599(16) Uani 1 1 d . . . F2 F 0.3329(4) 2.0972(5) 0.7201(3) 0.0501(14) Uani 1 1 d . . . F3 F 0.4072(5) 2.0955(5) 0.5928(3) 0.0475(13) Uani 1 1 d . . . F4 F 1.2676(5) 1.4317(6) 0.8038(4) 0.0736(19) Uani 1 1 d . . . F5 F 1.1941(6) 1.6168(6) 0.8401(5) 0.076(2) Uani 1 1 d . . . F6 F 1.1220(7) 1.4869(6) 0.8930(4) 0.084(2) Uani 1 1 d . . . F7 F 0.8570(7) 2.1117(6) 0.8643(4) 0.076(2) Uani 1 1 d . . . F8 F 0.8319(6) 2.1681(5) 0.7288(4) 0.0667(17) Uani 1 1 d . . . F9 F 1.0004(6) 2.1453(6) 0.7893(4) 0.0659(17) Uani 1 1 d . . . O1 O 0.6016(5) 1.9907(5) 0.7202(4) 0.0353(13) Uani 1 1 d . . . O2 O 0.6032(5) 2.1825(5) 0.6484(3) 0.0359(13) Uani 1 1 d . . . O3 O 0.5199(5) 2.1772(5) 0.7934(3) 0.0357(13) Uani 1 1 d . . . O4 O 0.9485(5) 1.6437(5) 0.7662(4) 0.0366(14) Uani 1 1 d . . . O5 O 1.0473(7) 1.4488(7) 0.7131(6) 0.079(3) Uani 1 1 d . . . O6 O 1.1179(7) 1.6169(8) 0.6655(5) 0.074(2) Uani 1 1 d . . . O7 O 0.8561(4) 1.9112(5) 0.7648(3) 0.0286(12) Uani 1 1 d . . . O8 O 1.0517(5) 1.8804(6) 0.8310(4) 0.0472(16) Uani 1 1 d . . . O9 O 1.0191(5) 1.9473(6) 0.6790(4) 0.0415(15) Uani 1 1 d . . . N1 N 0.5195(5) 1.7918(5) 0.6877(4) 0.0245(14) Uani 1 1 d . . . N2 N 0.5444(5) 1.8137(5) 0.8601(4) 0.0202(13) Uani 1 1 d . . . N3 N 0.7713(6) 1.7872(6) 0.9174(4) 0.0263(14) Uani 1 1 d . . . N4 N 0.7944(6) 1.8160(6) 0.5910(4) 0.0263(14) Uani 1 1 d . . . N5 N 0.7618(5) 1.6033(5) 0.6465(4) 0.0247(14) Uani 1 1 d . . . N6 N 0.7180(6) 1.5614(6) 0.8161(4) 0.0280(14) Uani 1 1 d . . . C1 C 0.5053(8) 1.7837(7) 0.6035(5) 0.0294(18) Uani 1 1 d . . . H1A H 0.5710 1.7800 0.5673 0.035 Uiso 1 1 calc R . . C2 C 0.3998(7) 1.7807(7) 0.5669(5) 0.0311(18) Uani 1 1 d . . . H2B H 0.3941 1.7768 0.5077 0.037 Uiso 1 1 calc R . . C3 C 0.3033(7) 1.7835(7) 0.6198(5) 0.0319(18) Uani 1 1 d . . . H3B H 0.2318 1.7782 0.5976 0.038 Uiso 1 1 calc R . . C4 C 0.3144(7) 1.7943(7) 0.7065(5) 0.0299(18) Uani 1 1 d . . . H4A H 0.2495 1.7974 0.7432 0.036 Uiso 1 1 calc R . . C5 C 0.4218(7) 1.8008(7) 0.7396(5) 0.0248(16) Uani 1 1 d . . . C6 C 0.4335(7) 1.8231(7) 0.8303(5) 0.0238(16) Uani 1 1 d . . . C7 C 0.3294(7) 1.8546(8) 0.8831(5) 0.0314(18) Uani 1 1 d . . . H7A H 0.2537 1.8592 0.8617 0.038 Uiso 1 1 calc R . . C8 C 0.3414(7) 1.8789(8) 0.9677(5) 0.0344(19) Uani 1 1 d . . . H8B H 0.2731 1.9029 1.0029 0.041 Uiso 1 1 calc R . . C9 C 0.4545(7) 1.8671(7) 0.9991(5) 0.0285(17) Uani 1 1 d . . . H9B H 0.4638 1.8816 1.0560 0.034 Uiso 1 1 calc R . . C10 C 0.5549(7) 1.8333(6) 0.9449(5) 0.0227(16) Uani 1 1 d . . . C11 C 0.6803(7) 1.8129(7) 0.9773(5) 0.0248(16) Uani 1 1 d . . . C12 C 0.7032(7) 1.8174(8) 1.0634(5) 0.0323(18) Uani 1 1 d . . . H12A H 0.6396 1.8359 1.1028 0.039 Uiso 1 1 calc R . . C13 C 0.8219(8) 1.7942(9) 1.0900(5) 0.041(2) Uani 1 1 d . . . H13A H 0.8393 1.7956 1.1479 0.050 Uiso 1 1 calc R . . C14 C 0.9139(8) 1.7693(8) 1.0309(5) 0.038(2) Uani 1 1 d . . . H14A H 0.9942 1.7552 1.0477 0.045 Uiso 1 1 calc R . . C15 C 0.8850(7) 1.7656(8) 0.9456(5) 0.0312(18) Uani 1 1 d . . . H15A H 0.9482 1.7471 0.9057 0.037 Uiso 1 1 calc R . . C16 C 0.8139(7) 1.9188(7) 0.5658(5) 0.0309(18) Uani 1 1 d . . . H16A H 0.7843 1.9834 0.6003 0.037 Uiso 1 1 calc R . . C17 C 0.8756(7) 1.9355(8) 0.4916(5) 0.036(2) Uani 1 1 d . . . H17A H 0.8868 2.0093 0.4767 0.043 Uiso 1 1 calc R . . C18 C 0.9203(8) 1.8400(8) 0.4397(6) 0.040(2) Uani 1 1 d . . . H18A H 0.9627 1.8485 0.3896 0.048 Uiso 1 1 calc R . . C19 C 0.9012(7) 1.7320(8) 0.4635(5) 0.036(2) Uani 1 1 d . . . H19A H 0.9307 1.6667 0.4295 0.044 Uiso 1 1 calc R . . C20 C 0.8366(7) 1.7217(7) 0.5395(5) 0.0263(17) Uani 1 1 d . . . C21 C 0.8034(7) 1.6141(7) 0.5653(5) 0.0284(17) Uani 1 1 d . . . C22 C 0.8095(9) 1.5288(8) 0.5064(5) 0.040(2) Uani 1 1 d . . . H22A H 0.8388 1.5379 0.4511 0.048 Uiso 1 1 calc R . . C23 C 0.7727(10) 1.4322(8) 0.5299(6) 0.048(2) Uani 1 1 d . . . H23A H 0.7780 1.3740 0.4915 0.058 Uiso 1 1 calc R . . C24 C 0.7274(9) 1.4229(7) 0.6121(6) 0.042(2) Uani 1 1 d . . . H24A H 0.6973 1.3605 0.6287 0.050 Uiso 1 1 calc R . . C25 C 0.7270(7) 1.5071(7) 0.6696(5) 0.0316(18) Uani 1 1 d . . . C26 C 0.6870(7) 1.4940(7) 0.7606(5) 0.0305(18) Uani 1 1 d . . . C27 C 0.6273(8) 1.4121(8) 0.7880(6) 0.043(2) Uani 1 1 d . . . H27A H 0.6026 1.3702 0.7481 0.051 Uiso 1 1 calc R . . C28 C 0.6056(10) 1.3946(8) 0.8745(6) 0.050(3) Uani 1 1 d . . . H28A H 0.5630 1.3433 0.8938 0.060 Uiso 1 1 calc R . . C29 C 0.6480(10) 1.4545(8) 0.9323(6) 0.051(3) Uani 1 1 d . . . H29A H 0.6409 1.4388 0.9915 0.062 Uiso 1 1 calc R . . C30 C 0.7007(8) 1.5373(7) 0.9010(5) 0.036(2) Uani 1 1 d . . . H30A H 0.7260 1.5794 0.9404 0.043 Uiso 1 1 calc R . . C31 C 0.3968(8) 2.1463(7) 0.6670(5) 0.0351(19) Uani 1 1 d . . . C32 C 1.1661(8) 1.5227(9) 0.8203(8) 0.056(3) Uani 1 1 d . . . C33 C 0.9100(9) 2.1012(9) 0.7889(6) 0.045(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.0219(2) 0.0242(2) 0.0180(2) -0.00095(16) 0.00338(16) -0.01169(17) S1 0.0268(9) 0.0261(10) 0.0196(9) -0.0005(8) 0.0029(8) -0.0112(8) S2 0.0412(13) 0.0533(15) 0.0475(14) -0.0209(12) -0.0062(12) 0.0020(12) S3 0.0250(10) 0.0401(11) 0.0320(11) -0.0002(9) 0.0014(8) -0.0202(9) F1 0.050(3) 0.038(3) 0.079(4) 0.002(3) -0.027(3) 0.002(3) F2 0.033(3) 0.069(4) 0.054(3) -0.003(3) 0.002(2) -0.025(3) F3 0.046(3) 0.066(3) 0.033(3) -0.013(3) -0.010(2) -0.019(3) F4 0.039(3) 0.067(4) 0.085(5) 0.000(4) 0.000(3) 0.018(3) F5 0.065(4) 0.067(4) 0.093(5) -0.007(4) -0.030(4) -0.017(3) F6 0.092(5) 0.081(5) 0.056(4) 0.020(4) 0.001(4) -0.007(4) F7 0.105(5) 0.079(4) 0.062(4) -0.037(4) 0.049(4) -0.051(4) F8 0.070(4) 0.040(3) 0.084(5) -0.004(3) -0.009(4) -0.012(3) F9 0.078(4) 0.074(4) 0.071(4) -0.020(3) 0.002(3) -0.056(4) O1 0.031(3) 0.029(3) 0.037(3) 0.007(3) 0.007(3) 0.000(2) O2 0.047(3) 0.039(3) 0.028(3) 0.000(3) 0.006(3) -0.024(3) O3 0.047(3) 0.049(3) 0.018(3) -0.010(3) 0.008(3) -0.023(3) O4 0.035(3) 0.034(3) 0.038(3) -0.012(3) 0.004(3) -0.005(3) O5 0.052(4) 0.051(4) 0.134(8) -0.027(5) -0.015(5) -0.015(4) O6 0.073(5) 0.109(7) 0.044(4) -0.009(4) 0.023(4) -0.037(5) O7 0.024(3) 0.038(3) 0.032(3) 0.000(2) 0.001(2) -0.022(2) O8 0.027(3) 0.070(4) 0.044(4) 0.017(3) -0.011(3) -0.021(3) O9 0.034(3) 0.057(4) 0.038(3) -0.004(3) 0.015(3) -0.022(3) N1 0.026(3) 0.027(3) 0.023(3) 0.001(3) 0.004(3) -0.015(3) N2 0.021(3) 0.022(3) 0.019(3) -0.002(3) 0.000(3) -0.010(3) N3 0.029(3) 0.037(4) 0.017(3) 0.003(3) 0.003(3) -0.019(3) N4 0.029(3) 0.028(3) 0.027(3) -0.001(3) -0.001(3) -0.016(3) N5 0.027(3) 0.024(3) 0.025(3) 0.000(3) 0.005(3) -0.012(3) N6 0.036(4) 0.026(3) 0.024(3) 0.000(3) 0.009(3) -0.015(3) C1 0.041(5) 0.033(4) 0.019(4) -0.005(3) 0.007(4) -0.019(4) C2 0.035(4) 0.040(5) 0.022(4) -0.003(4) -0.003(4) -0.016(4) C3 0.030(4) 0.033(4) 0.036(5) -0.007(4) -0.006(4) -0.014(4) C4 0.026(4) 0.043(5) 0.025(4) -0.004(4) 0.003(3) -0.017(4) C5 0.028(4) 0.030(4) 0.026(4) -0.001(3) 0.004(3) -0.022(3) C6 0.028(4) 0.025(4) 0.020(4) 0.003(3) -0.003(3) -0.014(3) C7 0.025(4) 0.052(5) 0.022(4) -0.004(4) 0.000(3) -0.019(4) C8 0.030(4) 0.054(5) 0.023(4) -0.009(4) 0.003(4) -0.018(4) C9 0.030(4) 0.035(4) 0.019(4) 0.000(3) 0.005(3) -0.010(4) C10 0.029(4) 0.018(4) 0.021(4) 0.002(3) 0.001(3) -0.008(3) C11 0.032(4) 0.027(4) 0.018(4) -0.002(3) 0.003(3) -0.014(3) C12 0.030(4) 0.046(5) 0.023(4) -0.002(4) 0.000(3) -0.016(4) C13 0.040(5) 0.064(6) 0.023(4) 0.000(4) -0.001(4) -0.023(5) C14 0.027(4) 0.056(6) 0.031(4) -0.006(4) -0.002(4) -0.013(4) C15 0.028(4) 0.047(5) 0.020(4) -0.005(4) 0.005(3) -0.014(4) C16 0.038(4) 0.036(5) 0.025(4) 0.001(4) 0.000(4) -0.021(4) C17 0.036(5) 0.043(5) 0.033(5) 0.004(4) 0.002(4) -0.023(4) C18 0.040(5) 0.055(6) 0.029(4) 0.000(4) 0.005(4) -0.021(5) C19 0.032(4) 0.044(5) 0.030(4) -0.005(4) 0.004(4) -0.008(4) C20 0.026(4) 0.035(4) 0.020(4) 0.001(3) -0.002(3) -0.013(3) C21 0.024(4) 0.032(4) 0.028(4) -0.009(4) 0.003(3) -0.006(3) C22 0.057(6) 0.041(5) 0.025(4) -0.009(4) 0.008(4) -0.019(5) C23 0.074(7) 0.040(5) 0.032(5) -0.010(4) -0.005(5) -0.020(5) C24 0.063(6) 0.025(4) 0.043(5) -0.006(4) 0.001(5) -0.022(4) C25 0.035(4) 0.032(4) 0.028(4) -0.006(4) 0.006(4) -0.011(4) C26 0.038(5) 0.026(4) 0.032(4) 0.000(3) 0.006(4) -0.017(4) C27 0.049(5) 0.039(5) 0.046(5) -0.004(4) -0.001(5) -0.022(4) C28 0.068(7) 0.040(5) 0.051(6) 0.007(5) 0.016(5) -0.033(5) C29 0.077(7) 0.037(5) 0.041(5) 0.003(4) 0.018(5) -0.023(5) C30 0.044(5) 0.029(4) 0.036(5) -0.004(4) 0.012(4) -0.014(4) C31 0.037(5) 0.032(5) 0.034(5) 0.003(4) -0.001(4) -0.010(4) C32 0.029(5) 0.044(6) 0.088(9) 0.008(6) -0.007(5) -0.005(4) C33 0.055(6) 0.054(6) 0.044(5) -0.015(5) 0.008(5) -0.040(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O4 2.451(6) . ? Ce O1 2.476(5) . ? Ce O7 2.483(5) . ? Ce N3 2.632(6) . ? Ce N4 2.637(6) . ? Ce N1 2.651(6) . ? Ce N5 2.653(6) . ? Ce N2 2.677(6) . ? Ce N6 2.699(6) . ? S1 O2 1.434(6) . ? S1 O3 1.436(5) . ? S1 O1 1.466(6) . ? S1 C31 1.827(9) . ? S2 O5 1.387(8) . ? S2 O4 1.463(6) . ? S2 O6 1.477(8) . ? S2 C32 1.800(11) . ? S3 O8 1.418(6) . ? S3 O9 1.426(6) . ? S3 O7 1.469(5) . ? S3 C33 1.838(10) . ? F1 C31 1.321(9) . ? F2 C31 1.323(10) . ? F3 C31 1.327(10) . ? F4 C32 1.332(11) . ? F5 C32 1.316(12) . ? F6 C32 1.326(13) . ? F7 C33 1.308(10) . ? F8 C33 1.320(11) . ? F9 C33 1.322(10) . ? N1 C1 1.339(9) . ? N1 C5 1.358(9) . ? N2 C6 1.346(9) . ? N2 C10 1.373(9) . ? N3 C15 1.335(10) . ? N3 C11 1.368(9) . ? N4 C16 1.329(10) . ? N4 C20 1.368(10) . ? N5 C25 1.345(10) . ? N5 C21 1.353(10) . ? N6 C26 1.351(10) . ? N6 C30 1.352(10) . ? C1 C2 1.376(11) . ? C2 C3 1.370(11) . ? C3 C4 1.378(11) . ? C4 C5 1.389(10) . ? C5 C6 1.474(10) . ? C6 C7 1.407(11) . ? C7 C8 1.389(11) . ? C8 C9 1.370(11) . ? C9 C10 1.389(10) . ? C10 C11 1.486(10) . ? C11 C12 1.378(10) . ? C12 C13 1.378(12) . ? C13 C14 1.365(12) . ? C14 C15 1.383(11) . ? C16 C17 1.381(11) . ? C17 C18 1.384(12) . ? C18 C19 1.381(12) . ? C19 C20 1.406(11) . ? C20 C21 1.467(11) . ? C21 C22 1.397(11) . ? C22 C23 1.364(13) . ? C23 C24 1.382(13) . ? C24 C25 1.388(11) . ? C25 C26 1.493(11) . ? C26 C27 1.401(12) . ? C27 C28 1.375(13) . ? C28 C29 1.382(14) . ? C29 C30 1.369(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ce O1 142.71(19) . . ? O4 Ce O7 73.50(18) . . ? O1 Ce O7 70.55(18) . . ? O4 Ce N3 80.04(19) . . ? O1 Ce N3 97.7(2) . . ? O7 Ce N3 71.85(18) . . ? O4 Ce N4 83.6(2) . . ? O1 Ce N4 79.19(19) . . ? O7 Ce N4 77.15(18) . . ? N3 Ce N4 147.94(19) . . ? O4 Ce N1 142.64(19) . . ? O1 Ce N1 68.62(19) . . ? O7 Ce N1 137.90(18) . . ? N3 Ce N1 123.34(19) . . ? N4 Ce N1 85.59(18) . . ? O4 Ce N5 73.80(19) . . ? O1 Ce N5 123.88(19) . . ? O7 Ce N5 129.51(18) . . ? N3 Ce N5 136.71(19) . . ? N4 Ce N5 61.89(18) . . ? N1 Ce N5 69.56(19) . . ? O4 Ce N2 132.23(19) . . ? O1 Ce N2 73.87(18) . . ? O7 Ce N2 115.10(17) . . ? N3 Ce N2 61.39(18) . . ? N4 Ce N2 143.53(19) . . ? N1 Ce N2 62.00(18) . . ? N5 Ce N2 115.38(18) . . ? O4 Ce N6 76.8(2) . . ? O1 Ce N6 139.92(19) . . ? O7 Ce N6 141.98(19) . . ? N3 Ce N6 80.13(19) . . ? N4 Ce N6 122.53(19) . . ? N1 Ce N6 79.26(19) . . ? N5 Ce N6 60.83(18) . . ? N2 Ce N6 70.09(18) . . ? O2 S1 O3 116.4(3) . . ? O2 S1 O1 114.1(3) . . ? O3 S1 O1 114.5(3) . . ? O2 S1 C31 104.2(4) . . ? O3 S1 C31 103.7(4) . . ? O1 S1 C31 101.5(4) . . ? O5 S2 O4 114.2(5) . . ? O5 S2 O6 116.8(6) . . ? O4 S2 O6 112.3(4) . . ? O5 S2 C32 106.7(5) . . ? O4 S2 C32 102.9(4) . . ? O6 S2 C32 101.8(5) . . ? O8 S3 O9 116.8(4) . . ? O8 S3 O7 113.6(3) . . ? O9 S3 O7 114.0(3) . . ? O8 S3 C33 104.6(4) . . ? O9 S3 C33 103.8(4) . . ? O7 S3 C33 101.6(4) . . ? S1 O1 Ce 165.8(4) . . ? S2 O4 Ce 151.6(4) . . ? S3 O7 Ce 155.1(3) . . ? C1 N1 C5 117.3(6) . . ? C1 N1 Ce 121.3(5) . . ? C5 N1 Ce 121.3(5) . . ? C6 N2 C10 118.2(6) . . ? C6 N2 Ce 120.3(4) . . ? C10 N2 Ce 121.3(4) . . ? C15 N3 C11 117.1(6) . . ? C15 N3 Ce 119.2(5) . . ? C11 N3 Ce 123.7(5) . . ? C16 N4 C20 117.8(6) . . ? C16 N4 Ce 119.8(5) . . ? C20 N4 Ce 120.2(5) . . ? C25 N5 C21 118.0(6) . . ? C25 N5 Ce 121.2(5) . . ? C21 N5 Ce 120.6(5) . . ? C26 N6 C30 116.9(7) . . ? C26 N6 Ce 117.6(5) . . ? C30 N6 Ce 122.0(5) . . ? N1 C1 C2 124.3(7) . . ? C3 C2 C1 118.4(7) . . ? C2 C3 C4 118.6(7) . . ? C3 C4 C5 120.6(7) . . ? N1 C5 C4 120.7(7) . . ? N1 C5 C6 117.1(6) . . ? C4 C5 C6 122.1(6) . . ? N2 C6 C7 121.8(6) . . ? N2 C6 C5 118.5(6) . . ? C7 C6 C5 119.7(7) . . ? C8 C7 C6 118.9(7) . . ? C9 C8 C7 119.7(7) . . ? C8 C9 C10 119.1(7) . . ? N2 C10 C9 122.2(7) . . ? N2 C10 C11 116.7(6) . . ? C9 C10 C11 121.1(7) . . ? N3 C11 C12 122.1(7) . . ? N3 C11 C10 116.2(6) . . ? C12 C11 C10 121.6(7) . . ? C11 C12 C13 119.0(8) . . ? C14 C13 C12 119.7(8) . . ? C13 C14 C15 118.6(8) . . ? N3 C15 C14 123.5(7) . . ? N4 C16 C17 124.0(8) . . ? C16 C17 C18 118.6(8) . . ? C19 C18 C17 119.1(8) . . ? C18 C19 C20 119.3(8) . . ? N4 C20 C19 121.2(7) . . ? N4 C20 C21 116.1(6) . . ? C19 C20 C21 122.6(7) . . ? N5 C21 C22 121.5(7) . . ? N5 C21 C20 117.8(6) . . ? C22 C21 C20 120.7(7) . . ? C23 C22 C21 120.2(8) . . ? C22 C23 C24 118.3(8) . . ? C23 C24 C25 119.6(8) . . ? N5 C25 C24 122.2(7) . . ? N5 C25 C26 117.1(7) . . ? C24 C25 C26 120.6(7) . . ? N6 C26 C27 122.1(7) . . ? N6 C26 C25 115.6(7) . . ? C27 C26 C25 122.3(7) . . ? C28 C27 C26 119.1(8) . . ? C27 C28 C29 118.9(8) . . ? C30 C29 C28 118.9(9) . . ? N6 C30 C29 123.7(8) . . ? F1 C31 F2 108.1(7) . . ? F1 C31 F3 107.7(7) . . ? F2 C31 F3 107.7(7) . . ? F1 C31 S1 111.1(6) . . ? F2 C31 S1 111.2(6) . . ? F3 C31 S1 110.8(6) . . ? F5 C32 F6 104.1(10) . . ? F5 C32 F4 109.8(8) . . ? F6 C32 F4 106.1(8) . . ? F5 C32 S2 113.3(7) . . ? F6 C32 S2 112.5(7) . . ? F4 C32 S2 110.7(8) . . ? F7 C33 F8 109.8(8) . . ? F7 C33 F9 109.0(7) . . ? F8 C33 F9 106.4(8) . . ? F7 C33 S3 111.2(7) . . ? F8 C33 S3 110.1(6) . . ? F9 C33 S3 110.1(7) . . ? #===END data_4.MeCN _database_code_depnum_ccdc_archive 'CCDC 251219' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H25 Ce F9 N7 O9 S3' _chemical_formula_weight 1094.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6590(19) _cell_length_b 11.359(2) _cell_length_c 18.675(4) _cell_angle_alpha 94.35(3) _cell_angle_beta 96.38(3) _cell_angle_gamma 102.16(3) _cell_volume 1980.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11045 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 1.415 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11045 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 24.73 _reflns_number_total 5925 _reflns_number_gt 4223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0701P)^2^+13.7596P] 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 5925 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.874 _refine_diff_density_max 0.712 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.138 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 Ce Ce -0.28174(6) 0.81244(5) 0.74112(3) 0.02658(19) Uani 1 1 d . . . S1 S -0.0700(3) 0.7358(2) 0.59025(13) 0.0329(6) Uani 1 1 d . . . S2 S -0.3730(3) 0.8061(2) 0.92627(13) 0.0317(6) Uani 1 1 d . . . S3 S -0.2332(3) 0.5110(2) 0.81825(15) 0.0413(7) Uani 1 1 d . . . F1 F 0.1302(6) 0.6444(6) 0.5413(3) 0.0501(16) Uani 1 1 d . . . F2 F -0.0173(7) 0.5173(5) 0.5916(3) 0.0535(17) Uani 1 1 d . . . F3 F 0.1407(6) 0.6568(6) 0.6571(3) 0.0492(16) Uani 1 1 d . . . F4 F -0.4764(7) 0.5753(5) 0.9355(3) 0.0526(16) Uani 1 1 d . . . F5 F -0.4560(7) 0.6904(6) 1.0350(3) 0.0513(16) Uani 1 1 d . . . F6 F -0.6251(6) 0.6904(6) 0.9496(3) 0.0517(16) Uani 1 1 d . . . F7 F -0.1713(9) 0.3108(6) 0.7686(5) 0.083(3) Uani 1 1 d . . . F8 F -0.0438(7) 0.4700(6) 0.7353(4) 0.0615(19) Uani 1 1 d . . . F9 F -0.2620(8) 0.4071(7) 0.6863(4) 0.073(2) Uani 1 1 d . . . O1 O -0.1353(7) 0.7234(6) 0.6564(3) 0.0365(16) Uani 1 1 d . . . O2 O 0.0238(7) 0.8503(6) 0.5877(4) 0.0398(17) Uani 1 1 d . . . O3 O -0.1662(7) 0.6881(6) 0.5261(3) 0.0387(17) Uani 1 1 d . . . O4 O -0.4174(6) 0.7807(5) 0.8497(3) 0.0288(14) Uani 1 1 d . . . O5 O -0.2311(7) 0.7895(6) 0.9471(4) 0.0368(16) Uani 1 1 d . . . O6 O -0.4097(7) 0.9127(6) 0.9578(4) 0.0370(16) Uani 1 1 d . . . O7 O -0.2435(7) 0.6190(5) 0.7828(4) 0.0350(16) Uani 1 1 d . . . O8 O -0.3678(8) 0.4373(6) 0.8287(4) 0.053(2) Uani 1 1 d . . . O9 O -0.1197(10) 0.5303(8) 0.8762(4) 0.064(2) Uani 1 1 d . . . N1 N -0.1740(8) 0.9948(7) 0.6661(4) 0.0323(19) Uani 1 1 d . . . N2 N -0.3915(8) 0.8107(7) 0.6014(4) 0.0304(18) Uani 1 1 d . . . N3 N -0.5120(8) 0.6453(7) 0.6874(4) 0.0281(18) Uani 1 1 d . . . N4 N -0.0270(8) 0.8655(7) 0.8163(4) 0.0298(18) Uani 1 1 d . . . N5 N -0.2128(8) 1.0130(7) 0.8321(4) 0.0288(18) Uani 1 1 d . . . N6 N -0.4657(8) 0.9571(7) 0.7416(4) 0.0285(17) Uani 1 1 d . . . N7 N -0.1745(11) 0.7102(10) 1.1667(6) 0.059(3) Uani 1 1 d . . . C1 C -0.0657(10) 1.0843(8) 0.6975(5) 0.033(2) Uani 1 1 d . . . H1A H -0.0278 1.0791 0.7449 0.040 Uiso 1 1 calc R . . C2 C -0.0070(11) 1.1831(9) 0.6642(5) 0.036(2) Uani 1 1 d . . . H2B H 0.0671 1.2436 0.6886 0.043 Uiso 1 1 calc R . . C3 C -0.0600(12) 1.1898(10) 0.5950(6) 0.047(3) Uani 1 1 d . . . H3B H -0.0228 1.2558 0.5711 0.056 Uiso 1 1 calc R . . C4 C -0.1707(11) 1.0976(10) 0.5592(6) 0.043(3) Uani 1 1 d . . . H4A H -0.2072 1.1011 0.5114 0.052 Uiso 1 1 calc R . . C5 C -0.2253(10) 1.0006(8) 0.5966(5) 0.030(2) Uani 1 1 d . . . C6 C -0.3418(10) 0.8996(8) 0.5605(5) 0.030(2) Uani 1 1 d . . . C7 C -0.3926(11) 0.8933(9) 0.4872(6) 0.041(3) Uani 1 1 d . . . H7A H -0.3562 0.9549 0.4599 0.049 Uiso 1 1 calc R . . C8 C -0.4973(12) 0.7952(9) 0.4552(5) 0.040(3) Uani 1 1 d . . . H8B H -0.5327 0.7905 0.4065 0.048 Uiso 1 1 calc R . . C9 C -0.5477(11) 0.7055(9) 0.4963(5) 0.033(2) Uani 1 1 d . . . H9B H -0.6182 0.6390 0.4755 0.040 Uiso 1 1 calc R . . C10 C -0.4945(10) 0.7129(8) 0.5687(5) 0.032(2) Uani 1 1 d . . . C11 C -0.5433(10) 0.6177(8) 0.6157(5) 0.027(2) Uani 1 1 d . . . C12 C -0.6252(10) 0.5040(8) 0.5857(5) 0.032(2) Uani 1 1 d . . . H12A H -0.6438 0.4847 0.5358 0.038 Uiso 1 1 calc R . . C13 C -0.6772(10) 0.4216(9) 0.6320(5) 0.034(2) Uani 1 1 d . . . H13A H -0.7316 0.3456 0.6133 0.040 Uiso 1 1 calc R . . C14 C -0.6492(10) 0.4508(9) 0.7057(5) 0.033(2) Uani 1 1 d . . . H14A H -0.6850 0.3965 0.7376 0.040 Uiso 1 1 calc R . . C15 C -0.5668(10) 0.5627(9) 0.7302(5) 0.034(2) Uani 1 1 d . . . H15A H -0.5474 0.5831 0.7801 0.040 Uiso 1 1 calc R . . C16 C 0.0682(10) 0.7981(9) 0.8031(5) 0.030(2) Uani 1 1 d . . . H16A H 0.0400 0.7317 0.7683 0.036 Uiso 1 1 calc R . . C17 C 0.2060(10) 0.8229(9) 0.8390(5) 0.036(2) Uani 1 1 d . . . H17A H 0.2674 0.7720 0.8301 0.044 Uiso 1 1 calc R . . C18 C 0.2503(11) 0.9237(9) 0.8881(5) 0.039(2) Uani 1 1 d . . . H18A H 0.3433 0.9436 0.9118 0.046 Uiso 1 1 calc R . . C19 C 0.1564(10) 0.9946(9) 0.9017(5) 0.035(2) Uani 1 1 d . . . H19A H 0.1852 1.0634 0.9347 0.042 Uiso 1 1 calc R . . C20 C 0.0167(9) 0.9631(8) 0.8658(5) 0.026(2) Uani 1 1 d . . . C21 C -0.0911(10) 1.0353(8) 0.8805(5) 0.028(2) Uani 1 1 d . . . C22 C -0.0661(10) 1.1222(8) 0.9393(5) 0.029(2) Uani 1 1 d . . . H22A H 0.0158 1.1334 0.9726 0.035 Uiso 1 1 calc R . . C23 C -0.1647(10) 1.1912(8) 0.9475(5) 0.034(2) Uani 1 1 d . . . H23A H -0.1499 1.2503 0.9866 0.041 Uiso 1 1 calc R . . C24 C -0.2850(11) 1.1733(9) 0.8980(5) 0.037(2) Uani 1 1 d . . . H24A H -0.3517 1.2206 0.9032 0.044 Uiso 1 1 calc R . . C25 C -0.3070(9) 1.0841(8) 0.8401(5) 0.025(2) Uani 1 1 d . . . C26 C -0.4371(10) 1.0594(8) 0.7860(5) 0.029(2) Uani 1 1 d . . . C27 C -0.5304(10) 1.1386(9) 0.7851(6) 0.037(2) Uani 1 1 d . . . H27A H -0.5080 1.2101 0.8159 0.044 Uiso 1 1 calc R . . C28 C -0.6552(11) 1.1095(10) 0.7382(6) 0.041(3) Uani 1 1 d . . . H28A H -0.7162 1.1628 0.7358 0.049 Uiso 1 1 calc R . . C29 C -0.6903(11) 1.0007(9) 0.6943(6) 0.036(2) Uani 1 1 d . . . H29A H -0.7768 0.9762 0.6642 0.043 Uiso 1 1 calc R . . C30 C -0.5891(10) 0.9304(9) 0.6979(5) 0.030(2) Uani 1 1 d . . . H30A H -0.6089 0.8588 0.6672 0.036 Uiso 1 1 calc R . . C31 C 0.0518(12) 0.6304(10) 0.5960(5) 0.040(3) Uani 1 1 d . . . C32 C -0.4850(10) 0.6836(9) 0.9631(6) 0.037(2) Uani 1 1 d . . . C33 C -0.1754(13) 0.4200(10) 0.7474(7) 0.048(3) Uani 1 1 d . . . C34 C -0.1632(11) 0.6521(10) 1.1168(7) 0.044(3) Uani 1 1 d . . . C35 C -0.1489(12) 0.5767(10) 1.0500(6) 0.048(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.0204(3) 0.0280(3) 0.0317(3) 0.0036(2) 0.0041(2) 0.0057(2) S1 0.0266(14) 0.0394(15) 0.0334(14) -0.0018(10) 0.0029(11) 0.0113(11) S2 0.0237(14) 0.0346(14) 0.0359(15) 0.0027(10) 0.0031(10) 0.0049(10) S3 0.0445(18) 0.0402(16) 0.0455(17) 0.0089(12) 0.0125(13) 0.0185(13) F1 0.041(4) 0.072(4) 0.050(4) 0.020(3) 0.017(3) 0.029(3) F2 0.058(4) 0.036(4) 0.068(5) 0.004(3) 0.013(3) 0.012(3) F3 0.041(4) 0.071(4) 0.042(4) 0.004(3) 0.004(3) 0.030(3) F4 0.058(4) 0.047(4) 0.058(4) 0.011(3) 0.020(3) 0.013(3) F5 0.053(4) 0.067(4) 0.040(4) 0.013(3) 0.011(3) 0.022(3) F6 0.033(4) 0.060(4) 0.063(4) 0.018(3) 0.006(3) 0.007(3) F7 0.109(7) 0.045(5) 0.124(7) 0.035(4) 0.077(6) 0.038(4) F8 0.058(5) 0.062(4) 0.079(5) 0.025(4) 0.037(4) 0.025(4) F9 0.076(6) 0.074(5) 0.064(5) -0.015(4) 0.012(4) 0.011(4) O1 0.026(4) 0.049(4) 0.038(4) 0.002(3) 0.008(3) 0.015(3) O2 0.040(4) 0.033(4) 0.047(4) 0.004(3) 0.015(3) 0.006(3) O3 0.027(4) 0.058(5) 0.030(4) -0.005(3) 0.004(3) 0.011(3) O4 0.020(4) 0.026(3) 0.040(4) 0.006(3) 0.013(3) 0.000(3) O5 0.025(4) 0.047(4) 0.041(4) 0.008(3) 0.006(3) 0.013(3) O6 0.031(4) 0.035(4) 0.046(4) 0.006(3) 0.002(3) 0.010(3) O7 0.030(4) 0.024(4) 0.052(4) 0.006(3) 0.003(3) 0.010(3) O8 0.047(5) 0.039(4) 0.083(6) 0.026(4) 0.039(4) 0.011(4) O9 0.082(7) 0.074(6) 0.046(5) 0.010(4) 0.000(4) 0.041(5) N1 0.030(5) 0.036(5) 0.033(5) 0.003(3) 0.009(4) 0.011(4) N2 0.012(4) 0.037(5) 0.047(5) 0.010(4) 0.009(3) 0.011(3) N3 0.022(4) 0.028(4) 0.034(5) 0.002(3) 0.001(3) 0.007(3) N4 0.024(5) 0.028(4) 0.039(5) 0.007(3) 0.008(3) 0.008(3) N5 0.015(4) 0.039(5) 0.035(5) 0.011(3) 0.002(3) 0.008(3) N6 0.015(4) 0.035(5) 0.034(5) -0.001(3) 0.004(3) 0.004(3) N7 0.055(7) 0.078(8) 0.046(6) 0.001(6) 0.013(5) 0.018(6) C1 0.033(6) 0.035(6) 0.031(6) 0.007(4) 0.002(4) 0.008(5) C2 0.030(6) 0.037(6) 0.045(7) 0.012(4) 0.008(5) 0.011(5) C3 0.042(7) 0.042(7) 0.053(7) 0.021(5) 0.007(6) -0.005(5) C4 0.037(7) 0.052(7) 0.037(6) 0.015(5) -0.002(5) 0.003(5) C5 0.026(6) 0.035(6) 0.028(6) -0.002(4) 0.002(4) 0.008(4) C6 0.029(6) 0.028(5) 0.037(6) 0.007(4) 0.008(4) 0.013(4) C7 0.048(7) 0.037(6) 0.045(7) 0.013(5) 0.011(5) 0.019(5) C8 0.053(7) 0.042(6) 0.027(6) -0.002(4) 0.003(5) 0.015(5) C9 0.038(6) 0.033(6) 0.028(6) 0.004(4) 0.000(4) 0.007(5) C10 0.021(5) 0.034(6) 0.044(6) -0.005(4) 0.010(4) 0.010(4) C11 0.025(6) 0.023(5) 0.036(6) 0.000(4) 0.006(4) 0.010(4) C12 0.023(6) 0.032(5) 0.039(6) -0.002(4) 0.005(4) 0.004(4) C13 0.018(5) 0.029(5) 0.050(7) 0.002(4) 0.006(4) -0.002(4) C14 0.024(6) 0.035(6) 0.041(6) 0.005(4) 0.003(4) 0.005(4) C15 0.028(6) 0.038(6) 0.036(6) 0.005(4) 0.006(4) 0.010(5) C16 0.021(6) 0.035(6) 0.034(6) 0.003(4) 0.003(4) 0.006(4) C17 0.030(6) 0.048(7) 0.037(6) 0.008(5) 0.005(5) 0.022(5) C18 0.029(6) 0.054(7) 0.030(6) 0.004(5) -0.002(4) 0.006(5) C19 0.022(6) 0.039(6) 0.043(6) 0.000(4) 0.002(4) 0.006(4) C20 0.021(5) 0.032(5) 0.026(5) 0.007(4) 0.010(4) 0.006(4) C21 0.026(6) 0.032(5) 0.028(5) 0.006(4) 0.006(4) 0.008(4) C22 0.029(6) 0.029(5) 0.028(5) 0.007(4) -0.003(4) 0.006(4) C23 0.034(6) 0.029(5) 0.040(6) 0.000(4) 0.011(5) 0.005(4) C24 0.027(6) 0.041(6) 0.045(6) -0.001(5) 0.013(5) 0.012(5) C25 0.023(5) 0.025(5) 0.028(5) 0.007(4) 0.014(4) 0.003(4) C26 0.030(6) 0.029(5) 0.028(5) 0.008(4) 0.005(4) 0.005(4) C27 0.026(6) 0.034(6) 0.052(7) 0.002(4) -0.006(5) 0.015(4) C28 0.025(6) 0.052(7) 0.051(7) 0.005(5) 0.004(5) 0.022(5) C29 0.025(6) 0.040(6) 0.047(6) 0.008(5) 0.015(5) 0.011(5) C30 0.022(6) 0.040(6) 0.025(5) 0.002(4) 0.003(4) 0.000(4) C31 0.048(7) 0.050(7) 0.028(6) 0.004(5) 0.006(5) 0.026(6) C32 0.017(6) 0.042(6) 0.056(7) -0.001(5) 0.006(5) 0.012(4) C33 0.049(8) 0.038(7) 0.059(8) 0.009(5) 0.022(6) 0.000(5) C34 0.036(7) 0.047(7) 0.054(8) 0.027(6) 0.008(5) 0.011(5) C35 0.044(7) 0.057(7) 0.046(7) 0.003(5) 0.005(5) 0.019(6) _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 Ce O7 2.472(6) . ? Ce O1 2.527(6) . ? Ce O4 2.542(6) . ? Ce N4 2.620(8) . ? Ce N3 2.644(8) . ? Ce N5 2.653(8) . ? Ce N6 2.663(7) . ? Ce N1 2.682(8) . ? Ce N2 2.702(8) . ? S1 O3 1.425(7) . ? S1 O2 1.427(7) . ? S1 O1 1.451(7) . ? S1 C31 1.848(10) . ? S2 O6 1.435(7) . ? S2 O4 1.436(7) . ? S2 O5 1.437(7) . ? S2 C32 1.804(11) . ? S3 O9 1.421(8) . ? S3 O8 1.433(8) . ? S3 O7 1.453(7) . ? S3 C33 1.826(12) . ? F1 C31 1.338(11) . ? F2 C31 1.309(12) . ? F3 C31 1.324(11) . ? F4 C32 1.320(11) . ? F5 C32 1.333(12) . ? F6 C32 1.368(11) . ? F7 C33 1.338(12) . ? F8 C33 1.329(13) . ? F9 C33 1.317(14) . ? N1 C1 1.340(12) . ? N1 C5 1.349(12) . ? N2 C6 1.352(11) . ? N2 C10 1.377(12) . ? N3 C11 1.338(11) . ? N3 C15 1.341(12) . ? N4 C16 1.346(11) . ? N4 C20 1.349(12) . ? N5 C25 1.350(11) . ? N5 C21 1.367(11) . ? N6 C30 1.332(11) . ? N6 C26 1.334(11) . ? N7 C34 1.129(14) . ? C1 C2 1.373(13) . ? C2 C3 1.351(14) . ? C3 C4 1.395(15) . ? C4 C5 1.391(13) . ? C5 C6 1.485(13) . ? C6 C7 1.393(13) . ? C7 C8 1.383(15) . ? C8 C9 1.361(13) . ? C9 C10 1.383(13) . ? C10 C11 1.477(13) . ? C11 C12 1.403(13) . ? C12 C13 1.377(13) . ? C13 C14 1.374(13) . ? C14 C15 1.366(13) . ? C16 C17 1.384(13) . ? C17 C18 1.371(14) . ? C18 C19 1.365(13) . ? C19 C20 1.400(13) . ? C20 C21 1.491(12) . ? C21 C22 1.383(13) . ? C22 C23 1.369(12) . ? C23 C24 1.371(14) . ? C24 C25 1.391(13) . ? C25 C26 1.485(12) . ? C26 C27 1.401(12) . ? C27 C28 1.372(13) . ? C28 C29 1.387(14) . ? C29 C30 1.385(13) . ? C34 C35 1.495(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 O7 Ce O1 71.5(2) . . ? O7 Ce O4 74.3(2) . . ? O1 Ce O4 145.7(2) . . ? O7 Ce N4 74.8(2) . . ? O1 Ce N4 77.9(2) . . ? O4 Ce N4 95.6(2) . . ? O7 Ce N3 73.4(2) . . ? O1 Ce N3 90.7(2) . . ? O4 Ce N3 77.2(2) . . ? N4 Ce N3 148.2(2) . . ? O7 Ce N5 120.1(2) . . ? O1 Ce N5 130.3(2) . . ? O4 Ce N5 70.8(2) . . ? N4 Ce N5 62.2(2) . . ? N3 Ce N5 138.6(2) . . ? O7 Ce N6 141.5(2) . . ? O1 Ce N6 140.3(2) . . ? O4 Ce N6 70.8(2) . . ? N4 Ce N6 123.9(2) . . ? N3 Ce N6 83.4(2) . . ? N5 Ce N6 62.0(2) . . ? O7 Ce N1 143.5(2) . . ? O1 Ce N1 75.1(2) . . ? O4 Ce N1 138.4(2) . . ? N4 Ce N1 84.3(2) . . ? N3 Ce N1 121.7(2) . . ? N5 Ce N1 72.6(2) . . ? N6 Ce N1 75.0(2) . . ? O7 Ce N2 117.7(2) . . ? O1 Ce N2 69.0(2) . . ? O4 Ce N2 127.6(2) . . ? N4 Ce N2 136.5(2) . . ? N3 Ce N2 61.2(2) . . ? N5 Ce N2 122.2(2) . . ? N6 Ce N2 73.9(2) . . ? N1 Ce N2 60.9(2) . . ? O3 S1 O2 116.3(4) . . ? O3 S1 O1 113.8(4) . . ? O2 S1 O1 114.6(4) . . ? O3 S1 C31 103.4(4) . . ? O2 S1 C31 103.3(5) . . ? O1 S1 C31 103.0(4) . . ? O6 S2 O4 113.9(4) . . ? O6 S2 O5 117.5(4) . . ? O4 S2 O5 112.8(4) . . ? O6 S2 C32 104.0(4) . . ? O4 S2 C32 103.1(4) . . ? O5 S2 C32 103.4(4) . . ? O9 S3 O8 117.7(5) . . ? O9 S3 O7 113.7(5) . . ? O8 S3 O7 114.5(4) . . ? O9 S3 C33 104.1(5) . . ? O8 S3 C33 102.7(5) . . ? O7 S3 C33 101.2(5) . . ? S1 O1 Ce 145.5(4) . . ? S2 O4 Ce 132.2(3) . . ? S3 O7 Ce 169.9(4) . . ? C1 N1 C5 117.7(8) . . ? C1 N1 Ce 120.2(6) . . ? C5 N1 Ce 122.1(6) . . ? C6 N2 C10 118.2(8) . . ? C6 N2 Ce 122.1(6) . . ? C10 N2 Ce 119.6(6) . . ? C11 N3 C15 117.9(8) . . ? C11 N3 Ce 119.9(6) . . ? C15 N3 Ce 118.4(6) . . ? C16 N4 C20 117.7(8) . . ? C16 N4 Ce 119.8(6) . . ? C20 N4 Ce 122.5(6) . . ? C25 N5 C21 118.0(8) . . ? C25 N5 Ce 121.0(6) . . ? C21 N5 Ce 120.1(5) . . ? C30 N6 C26 117.6(8) . . ? C30 N6 Ce 121.5(6) . . ? C26 N6 Ce 120.9(6) . . ? N1 C1 C2 124.2(9) . . ? C3 C2 C1 118.0(10) . . ? C2 C3 C4 120.1(10) . . ? C5 C4 C3 118.7(9) . . ? N1 C5 C4 121.3(9) . . ? N1 C5 C6 118.1(8) . . ? C4 C5 C6 120.6(8) . . ? N2 C6 C7 121.4(9) . . ? N2 C6 C5 116.7(8) . . ? C7 C6 C5 121.8(9) . . ? C8 C7 C6 119.8(9) . . ? C9 C8 C7 118.9(9) . . ? C8 C9 C10 120.3(9) . . ? N2 C10 C9 121.3(9) . . ? N2 C10 C11 115.8(8) . . ? C9 C10 C11 122.8(9) . . ? N3 C11 C12 121.4(8) . . ? N3 C11 C10 117.9(8) . . ? C12 C11 C10 120.7(8) . . ? C13 C12 C11 118.4(9) . . ? C14 C13 C12 120.4(9) . . ? C15 C14 C13 117.3(9) . . ? N3 C15 C14 124.5(9) . . ? N4 C16 C17 123.1(9) . . ? C18 C17 C16 118.8(9) . . ? C19 C18 C17 119.3(9) . . ? C18 C19 C20 119.6(9) . . ? N4 C20 C19 121.5(8) . . ? N4 C20 C21 116.8(8) . . ? C19 C20 C21 121.6(8) . . ? N5 C21 C22 122.4(8) . . ? N5 C21 C20 116.4(8) . . ? C22 C21 C20 121.1(8) . . ? C23 C22 C21 118.6(9) . . ? C22 C23 C24 119.9(9) . . ? C23 C24 C25 119.8(9) . . ? N5 C25 C24 121.2(9) . . ? N5 C25 C26 117.0(8) . . ? C24 C25 C26 121.8(8) . . ? N6 C26 C27 121.6(9) . . ? N6 C26 C25 118.1(8) . . ? C27 C26 C25 120.3(8) . . ? C28 C27 C26 119.3(9) . . ? C27 C28 C29 120.0(9) . . ? C30 C29 C28 116.2(9) . . ? N6 C30 C29 125.2(9) . . ? F2 C31 F3 109.3(8) . . ? F2 C31 F1 108.8(8) . . ? F3 C31 F1 107.5(9) . . ? F2 C31 S1 112.3(7) . . ? F3 C31 S1 110.5(7) . . ? F1 C31 S1 108.2(6) . . ? F4 C32 F5 108.6(8) . . ? F4 C32 F6 106.9(8) . . ? F5 C32 F6 105.6(8) . . ? F4 C32 S2 113.6(7) . . ? F5 C32 S2 111.7(7) . . ? F6 C32 S2 110.0(7) . . ? F9 C33 F8 108.7(9) . . ? F9 C33 F7 109.3(10) . . ? F8 C33 F7 106.7(10) . . ? F9 C33 S3 111.3(8) . . ? F8 C33 S3 111.0(8) . . ? F7 C33 S3 109.7(8) . . ? N7 C34 C35 179.0(12) . . ? #===END data_5.0.5MeCN _database_code_depnum_ccdc_archive 'CCDC 251220' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H23.50 F9 N6.50 Nd O9 S3' _chemical_formula_weight 1078.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 14.080(3) _cell_length_b 19.188(4) _cell_length_c 15.061(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.03(3) _cell_angle_gamma 90.00 _cell_volume 4058.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25346 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25346 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 24.73 _reflns_number_total 6578 _reflns_number_gt 4727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms. Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. One CF~3~SO~3~ molecule (S3) is found disordered on two positions with 0.8 and 0.2 occupations factors ; _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^)+(0.0795P)^2^+22.7324P] 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 6578 _refine_ls_number_parameters 605 _refine_ls_number_restraints 128 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.099 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.125 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 Nd Nd 0.48988(3) 0.75303(2) -0.26398(3) 0.03430(17) Uani 1 1 d . . . S1 S 0.74419(15) 0.68519(11) -0.24644(13) 0.0388(5) Uani 1 1 d . . . S2 S 0.23218(19) 0.69912(18) -0.2740(2) 0.0756(9) Uani 1 1 d . . . S3A S 0.4491(2) 0.55980(15) -0.2138(2) 0.0539(12) Uani 0.809(9) 1 d P . . S3B S 0.4998(13) 0.5494(9) -0.2718(13) 0.079(6) Uani 0.191(9) 1 d PU . . F1 F 0.8225(5) 0.7567(3) -0.1127(4) 0.0794(19) Uani 1 1 d . . . F2 F 0.8223(5) 0.8085(3) -0.2386(4) 0.0746(17) Uani 1 1 d . . . F3 F 0.9189(5) 0.7260(4) -0.2100(5) 0.094(2) Uani 1 1 d U . . F4 F 0.0846(9) 0.6531(6) -0.3669(8) 0.168(4) Uani 1 1 d U . . F5 F 0.2181(6) 0.6028(5) -0.3960(6) 0.114(3) Uani 1 1 d U . . F6 F 0.1935(9) 0.7107(7) -0.4409(8) 0.166(4) Uani 1 1 d U . . F7 F 0.6123(5) 0.5259(4) -0.1339(5) 0.0853(19) Uani 1 1 d U . . F8A F 0.6001(7) 0.5096(5) -0.2741(8) 0.094(3) Uani 0.809(9) 1 d PU . . F8B F 0.451(3) 0.521(2) -0.134(3) 0.092(14) Uani 0.191(9) 1 d PU . . F9 F 0.5292(7) 0.4396(5) -0.1910(7) 0.137(3) Uani 1 1 d U . . O1 O 0.6554(4) 0.7183(3) -0.2278(4) 0.0440(14) Uani 1 1 d . . . O2 O 0.7643(5) 0.6229(3) -0.1971(4) 0.0547(16) Uani 1 1 d . . . O3 O 0.7600(5) 0.6822(4) -0.3390(4) 0.0630(18) Uani 1 1 d . . . O4 O 0.3287(4) 0.7095(3) -0.2914(4) 0.0542(16) Uani 1 1 d . . . O5 O 0.2191(8) 0.6354(6) -0.2155(7) 0.114(3) Uani 1 1 d U . . O6 O 0.1807(6) 0.7588(5) -0.2509(7) 0.101(3) Uani 1 1 d . . . O7 O 0.4909(4) 0.6264(3) -0.2372(4) 0.0500(15) Uani 1 1 d . . . O8A O 0.4114(8) 0.5561(6) -0.1260(6) 0.075(3) Uani 0.809(9) 1 d P . . O8B O 0.597(2) 0.5317(18) -0.320(2) 0.046(8) Uani 0.191(9) 1 d PU . . O9 O 0.3969(5) 0.5275(4) -0.2891(5) 0.076(2) Uani 1 1 d . . . N1 N 0.5880(5) 0.8650(3) -0.2124(4) 0.0406(16) Uani 1 1 d . . . N2 N 0.5972(5) 0.8111(3) -0.3804(4) 0.0409(16) Uani 1 1 d . . . N3 N 0.4944(5) 0.6953(4) -0.4212(5) 0.0471(18) Uani 1 1 d . . . N4 N 0.4974(5) 0.7324(3) -0.0926(4) 0.0398(16) Uani 1 1 d . . . N5 N 0.3805(5) 0.8309(3) -0.1698(4) 0.0381(15) Uani 1 1 d . . . N6 N 0.3883(5) 0.8496(4) -0.3480(4) 0.0421(16) Uani 1 1 d . . . C1 C 0.5856(7) 0.8904(4) -0.1298(6) 0.049(2) Uani 1 1 d . . . H1A H 0.5545 0.8645 -0.0884 0.059 Uiso 1 1 calc R . . C2 C 0.6265(8) 0.9525(6) -0.1030(7) 0.069(3) Uani 1 1 d U . . H2B H 0.6233 0.9679 -0.0447 0.082 Uiso 1 1 calc R . . C3 C 0.6721(9) 0.9918(7) -0.1632(9) 0.087(4) Uani 1 1 d U . . H3B H 0.6984 1.0348 -0.1473 0.104 Uiso 1 1 calc R . . C4 C 0.6781(8) 0.9654(6) -0.2492(7) 0.071(3) Uani 1 1 d U . . H4A H 0.7106 0.9900 -0.2908 0.085 Uiso 1 1 calc R . . C5 C 0.6347(7) 0.9019(4) -0.2718(6) 0.048(2) Uani 1 1 d . . . C6 C 0.6454(7) 0.8706(4) -0.3593(5) 0.044(2) Uani 1 1 d . . . C7 C 0.7087(8) 0.8988(5) -0.4171(7) 0.065(3) Uani 1 1 d . . . H7A H 0.7430 0.9389 -0.4012 0.079 Uiso 1 1 calc R . . C8 C 0.7201(9) 0.8673(6) -0.4969(7) 0.070(3) Uani 1 1 d . . . H8A H 0.7610 0.8863 -0.5364 0.085 Uiso 1 1 calc R . . C9 C 0.6706(8) 0.8073(5) -0.5184(6) 0.060(3) Uani 1 1 d . . . H9A H 0.6784 0.7850 -0.5722 0.072 Uiso 1 1 calc R . . C10 C 0.6096(6) 0.7804(4) -0.4599(5) 0.0408(19) Uani 1 1 d . . . C11 C 0.5568(6) 0.7155(5) -0.4810(5) 0.042(2) Uani 1 1 d . . . C12 C 0.5672(7) 0.6772(5) -0.5578(6) 0.055(2) Uani 1 1 d . . . H12A H 0.6108 0.6916 -0.5976 0.066 Uiso 1 1 calc R . . C13 C 0.5144(8) 0.6189(5) -0.5754(6) 0.062(3) Uani 1 1 d . . . H13A H 0.5209 0.5936 -0.6273 0.075 Uiso 1 1 calc R . . C14 C 0.4515(8) 0.5980(5) -0.5156(7) 0.062(3) Uani 1 1 d . . . H14A H 0.4153 0.5579 -0.5259 0.074 Uiso 1 1 calc R . . C15 C 0.4421(8) 0.6375(5) -0.4393(6) 0.057(3) Uani 1 1 d . . . H15A H 0.3983 0.6236 -0.3994 0.068 Uiso 1 1 calc R . . C16 C 0.5525(7) 0.6825(5) -0.0554(6) 0.053(2) Uani 1 1 d . . . H16A H 0.5964 0.6615 -0.0902 0.064 Uiso 1 1 calc R . . C17 C 0.5493(8) 0.6601(6) 0.0302(7) 0.066(3) Uani 1 1 d . . . H17A H 0.5898 0.6252 0.0530 0.080 Uiso 1 1 calc R . . C18 C 0.4836(8) 0.6908(6) 0.0822(7) 0.069(3) Uani 1 1 d U . . H18A H 0.4803 0.6778 0.1414 0.082 Uiso 1 1 calc R . . C19 C 0.4238(8) 0.7406(5) 0.0451(7) 0.067(3) Uani 1 1 d . . . H19A H 0.3772 0.7602 0.0781 0.080 Uiso 1 1 calc R . . C20 C 0.4329(6) 0.7618(4) -0.0413(6) 0.044(2) Uani 1 1 d . . . C21 C 0.3761(6) 0.8199(4) -0.0814(5) 0.0409(19) Uani 1 1 d . . . C22 C 0.3227(7) 0.8622(5) -0.0298(6) 0.052(2) Uani 1 1 d . . . H22A H 0.3194 0.8530 0.0305 0.063 Uiso 1 1 calc R . . C23 C 0.2747(7) 0.9178(5) -0.0682(6) 0.058(3) Uani 1 1 d . . . H23A H 0.2395 0.9470 -0.0338 0.069 Uiso 1 1 calc R . . C24 C 0.2786(7) 0.9305(5) -0.1572(6) 0.052(2) Uani 1 1 d . . . H24A H 0.2471 0.9683 -0.1842 0.063 Uiso 1 1 calc R . . C25 C 0.3315(6) 0.8845(4) -0.2063(5) 0.0409(19) Uani 1 1 d . . . C26 C 0.3312(6) 0.8925(4) -0.3049(5) 0.0384(18) Uani 1 1 d . . . C27 C 0.2707(6) 0.9406(5) -0.3500(6) 0.048(2) Uani 1 1 d . . . H27A H 0.2339 0.9709 -0.3186 0.058 Uiso 1 1 calc R . . C28 C 0.2665(6) 0.9424(5) -0.4414(6) 0.054(2) Uani 1 1 d . . . H28A H 0.2267 0.9741 -0.4723 0.064 Uiso 1 1 calc R . . C29 C 0.3207(6) 0.8977(5) -0.4870(6) 0.048(2) Uani 1 1 d . . . H29A H 0.3168 0.8970 -0.5488 0.058 Uiso 1 1 calc R . . C30 C 0.3817(7) 0.8532(5) -0.4380(5) 0.048(2) Uani 1 1 d . . . H30A H 0.4205 0.8240 -0.4689 0.057 Uiso 1 1 calc R . . C31 C 0.8312(6) 0.7478(5) -0.1983(7) 0.057(2) Uani 1 1 d . . . C32 C 0.1809(13) 0.6669(10) -0.3824(12) 0.118(5) Uani 1 1 d U . . C33 C 0.5501(11) 0.5091(8) -0.2011(10) 0.093(4) Uani 1 1 d U . . N7 N 0.9760(17) 0.4335(13) 0.1953(14) 0.105(6) Uani 0.50 1 d PDU . . C34 C 0.987(2) 0.4643(15) 0.1175(15) 0.110(7) Uani 0.50 1 d PDU . . C35 C 1.0105(18) 0.5044(12) 0.0347(12) 0.077(7) Uani 0.50 1 d PDU . . 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 Nd 0.0430(3) 0.0295(2) 0.0311(2) 0.00158(18) 0.00721(18) -0.00159(19) S1 0.0437(11) 0.0410(11) 0.0326(10) -0.0004(8) 0.0103(9) 0.0030(9) S2 0.0482(15) 0.105(2) 0.0759(19) -0.0367(17) 0.0196(14) -0.0116(15) S3A 0.056(2) 0.0452(18) 0.060(2) 0.0131(14) 0.0031(16) -0.0163(14) S3B 0.079(7) 0.075(7) 0.083(7) -0.002(3) 0.004(3) 0.003(3) F1 0.111(5) 0.075(4) 0.049(3) -0.007(3) -0.012(3) -0.030(4) F2 0.087(4) 0.053(4) 0.085(4) 0.012(3) 0.011(4) -0.022(3) F3 0.080(3) 0.097(3) 0.105(3) -0.005(3) 0.003(3) -0.003(2) F4 0.160(5) 0.171(5) 0.174(5) -0.013(3) 0.005(3) -0.001(3) F5 0.112(4) 0.110(4) 0.118(4) -0.018(3) -0.002(3) 0.002(3) F6 0.169(5) 0.168(5) 0.160(5) 0.006(3) 0.005(3) 0.007(3) F7 0.086(3) 0.079(3) 0.089(3) 0.006(2) -0.007(2) 0.008(2) F8A 0.092(4) 0.093(4) 0.097(4) -0.011(3) 0.007(3) 0.007(3) F8B 0.092(15) 0.092(15) 0.092(15) 0.000(3) 0.007(3) 0.000(3) F9 0.142(4) 0.121(4) 0.146(4) 0.008(3) 0.000(3) -0.004(3) O1 0.043(3) 0.044(3) 0.046(3) 0.006(3) 0.013(3) 0.007(3) O2 0.075(4) 0.043(3) 0.045(3) -0.001(3) -0.008(3) 0.015(3) O3 0.073(4) 0.081(5) 0.038(3) -0.008(3) 0.027(3) -0.008(4) O4 0.044(3) 0.052(4) 0.067(4) -0.010(3) 0.009(3) -0.009(3) O5 0.116(4) 0.118(4) 0.109(4) 0.007(3) 0.016(3) -0.004(3) O6 0.064(5) 0.112(7) 0.130(8) -0.057(6) 0.021(5) 0.004(5) O7 0.072(4) 0.027(3) 0.051(4) 0.009(2) 0.000(3) -0.006(3) O8A 0.078(7) 0.089(8) 0.060(6) 0.011(5) 0.022(5) -0.028(6) O8B 0.048(9) 0.046(9) 0.045(9) 0.000(3) 0.005(3) 0.000(3) O9 0.081(5) 0.051(4) 0.092(6) 0.006(4) -0.016(4) -0.026(4) N1 0.050(4) 0.036(4) 0.037(4) 0.001(3) 0.006(3) -0.002(3) N2 0.049(4) 0.039(4) 0.035(4) 0.009(3) 0.003(3) -0.005(3) N3 0.063(5) 0.038(4) 0.042(4) -0.005(3) 0.015(4) -0.004(3) N4 0.041(4) 0.045(4) 0.035(4) 0.007(3) 0.012(3) 0.004(3) N5 0.043(4) 0.043(4) 0.029(3) 0.000(3) 0.007(3) 0.003(3) N6 0.050(4) 0.044(4) 0.032(4) -0.001(3) 0.001(3) 0.008(3) C1 0.073(6) 0.037(5) 0.039(5) -0.007(4) 0.012(5) -0.011(4) C2 0.075(4) 0.068(4) 0.063(4) -0.003(3) 0.008(3) -0.008(3) C3 0.094(4) 0.084(4) 0.084(4) -0.001(3) 0.008(3) -0.008(3) C4 0.079(4) 0.068(4) 0.067(4) -0.001(3) 0.008(3) -0.005(3) C5 0.067(6) 0.028(4) 0.051(5) 0.008(4) 0.010(5) -0.005(4) C6 0.060(5) 0.036(5) 0.036(4) 0.007(3) 0.005(4) -0.011(4) C7 0.087(8) 0.057(6) 0.053(6) 0.003(5) 0.011(6) -0.030(6) C8 0.091(8) 0.068(7) 0.055(6) 0.006(5) 0.028(6) -0.019(6) C9 0.081(7) 0.062(6) 0.040(5) 0.003(4) 0.025(5) -0.009(5) C10 0.051(5) 0.037(4) 0.035(4) 0.005(4) 0.005(4) 0.001(4) C11 0.054(5) 0.042(5) 0.031(4) 0.004(4) 0.008(4) 0.001(4) C12 0.068(6) 0.057(6) 0.042(5) -0.008(4) 0.011(5) 0.000(5) C13 0.087(8) 0.055(6) 0.046(6) -0.020(5) 0.013(6) -0.006(5) C14 0.079(7) 0.050(6) 0.059(6) -0.014(5) 0.020(6) -0.008(5) C15 0.080(7) 0.041(5) 0.052(6) -0.011(4) 0.021(5) -0.018(5) C16 0.055(5) 0.067(6) 0.039(5) 0.011(4) 0.014(4) 0.017(5) C17 0.077(7) 0.073(7) 0.052(6) 0.019(5) 0.020(6) 0.033(6) C18 0.073(4) 0.071(4) 0.063(4) 0.006(3) 0.012(3) 0.007(3) C19 0.080(7) 0.073(7) 0.051(6) 0.028(5) 0.035(6) 0.043(6) C20 0.049(5) 0.046(5) 0.037(4) 0.009(4) 0.010(4) 0.002(4) C21 0.039(4) 0.045(5) 0.040(5) 0.003(4) 0.012(4) 0.001(4) C22 0.054(5) 0.062(6) 0.042(5) 0.002(4) 0.007(4) 0.011(5) C23 0.070(6) 0.057(6) 0.047(6) -0.010(4) 0.011(5) 0.020(5) C24 0.055(6) 0.049(5) 0.051(6) -0.006(4) -0.002(5) 0.015(4) C25 0.041(5) 0.040(5) 0.041(5) 0.001(4) 0.000(4) -0.001(4) C26 0.042(5) 0.036(4) 0.037(4) 0.001(3) 0.000(4) -0.007(4) C27 0.045(5) 0.048(5) 0.052(5) 0.008(4) 0.007(4) 0.004(4) C28 0.046(5) 0.063(6) 0.051(6) 0.027(5) -0.003(4) 0.004(5) C29 0.054(5) 0.049(5) 0.041(5) 0.005(4) -0.007(4) -0.002(4) C30 0.057(6) 0.049(5) 0.036(5) 0.000(4) 0.000(4) 0.001(4) C31 0.040(5) 0.061(6) 0.068(7) -0.001(5) 0.002(5) 0.008(5) C32 0.116(6) 0.117(6) 0.121(6) -0.002(3) 0.010(3) -0.002(3) C33 0.094(5) 0.087(5) 0.096(5) 0.000(3) 0.002(3) -0.001(3) N7 0.103(7) 0.105(7) 0.106(7) 0.002(3) 0.008(3) -0.002(3) C34 0.108(7) 0.110(7) 0.110(7) -0.003(3) 0.006(3) 0.002(3) C35 0.075(7) 0.077(7) 0.078(7) -0.001(3) 0.005(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O4 2.427(6) . ? Nd O1 2.449(6) . ? Nd O7 2.463(5) . ? Nd N4 2.605(7) . ? Nd N6 2.614(7) . ? Nd N3 2.619(7) . ? Nd N5 2.631(6) . ? Nd N2 2.640(6) . ? Nd N1 2.642(7) . ? S1 O2 1.425(6) . ? S1 O3 1.429(6) . ? S1 O1 1.447(6) . ? S1 C31 1.829(10) . ? S2 O6 1.411(9) . ? S2 O4 1.416(6) . ? S2 O5 1.526(11) . ? S2 C32 1.845(18) . ? S3A O9 1.446(8) . ? S3A O8A 1.460(9) . ? S3A O7 1.461(6) . ? S3A C33 1.722(15) . ? S3B C33 1.46(2) . ? S3B O9 1.513(19) . ? S3B O7 1.575(19) . ? S3B O8B 1.63(4) . ? F1 C31 1.315(12) . ? F2 C31 1.313(11) . ? F3 C31 1.328(11) . ? F4 C32 1.416(19) . ? F5 C32 1.359(18) . ? F6 C32 1.239(18) . ? F7 C33 1.331(15) . ? F8A C33 1.347(16) . ? F8B C33 1.80(5) . ? F9 C33 1.377(16) . ? N1 C1 1.338(10) . ? N1 C5 1.348(10) . ? N2 C6 1.354(10) . ? N2 C10 1.357(10) . ? N3 C15 1.347(11) . ? N3 C11 1.359(10) . ? N4 C16 1.332(11) . ? N4 C20 1.356(11) . ? N5 C25 1.335(10) . ? N5 C21 1.353(10) . ? N6 C26 1.349(10) . ? N6 C30 1.354(10) . ? C1 C2 1.373(13) . ? C2 C3 1.372(15) . ? C3 C4 1.398(16) . ? C4 C5 1.395(14) . ? C5 C6 1.465(12) . ? C6 C7 1.398(12) . ? C7 C8 1.366(14) . ? C8 C9 1.372(14) . ? C9 C10 1.373(12) . ? C10 C11 1.474(12) . ? C11 C12 1.386(12) . ? C12 C13 1.360(13) . ? C13 C14 1.366(13) . ? C14 C15 1.391(12) . ? C16 C17 1.363(12) . ? C17 C18 1.384(14) . ? C18 C19 1.367(14) . ? C19 C20 1.379(13) . ? C20 C21 1.476(12) . ? C21 C22 1.383(12) . ? C22 C23 1.370(13) . ? C23 C24 1.366(13) . ? C24 C25 1.400(12) . ? C25 C26 1.492(11) . ? C26 C27 1.399(12) . ? C27 C28 1.375(12) . ? C28 C29 1.364(13) . ? C29 C30 1.385(12) . ? N7 C34 1.332(10) . ? C34 C35 1.5197(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Nd O1 143.9(2) . . ? O4 Nd O7 71.5(2) . . ? O1 Nd O7 72.6(2) . . ? O4 Nd N4 95.1(2) . . ? O1 Nd N4 76.5(2) . . ? O7 Nd N4 71.9(2) . . ? O4 Nd N6 71.8(2) . . ? O1 Nd N6 141.4(2) . . ? O7 Nd N6 140.9(2) . . ? N4 Nd N6 124.8(2) . . ? O4 Nd N3 77.4(2) . . ? O1 Nd N3 90.2(2) . . ? O7 Nd N3 74.3(2) . . ? N4 Nd N3 146.0(2) . . ? N6 Nd N3 84.8(2) . . ? O4 Nd N5 73.2(2) . . ? O1 Nd N5 128.2(2) . . ? O7 Nd N5 118.0(2) . . ? N4 Nd N5 62.4(2) . . ? N6 Nd N5 62.4(2) . . ? N3 Nd N5 141.3(2) . . ? O4 Nd N2 127.2(2) . . ? O1 Nd N2 71.5(2) . . ? O7 Nd N2 121.9(2) . . ? N4 Nd N2 137.4(2) . . ? N6 Nd N2 72.5(2) . . ? N3 Nd N2 61.8(2) . . ? N5 Nd N2 120.2(2) . . ? O4 Nd N1 142.5(2) . . ? O1 Nd N1 71.7(2) . . ? O7 Nd N1 139.2(2) . . ? N4 Nd N1 81.3(2) . . ? N6 Nd N1 79.8(2) . . ? N3 Nd N1 124.4(2) . . ? N5 Nd N1 72.1(2) . . ? N2 Nd N1 62.6(2) . . ? O2 S1 O3 115.8(4) . . ? O2 S1 O1 114.2(4) . . ? O3 S1 O1 113.8(4) . . ? O2 S1 C31 104.0(4) . . ? O3 S1 C31 105.5(4) . . ? O1 S1 C31 101.4(4) . . ? O6 S2 O4 116.6(5) . . ? O6 S2 O5 115.1(6) . . ? O4 S2 O5 112.0(5) . . ? O6 S2 C32 108.3(7) . . ? O4 S2 C32 101.8(6) . . ? O5 S2 C32 100.8(7) . . ? O9 S3A O8A 119.5(5) . . ? O9 S3A O7 112.2(4) . . ? O8A S3A O7 116.1(5) . . ? O9 S3A C33 102.4(6) . . ? O8A S3A C33 102.8(7) . . ? O7 S3A C33 100.2(6) . . ? C33 S3B O9 112.9(14) . . ? C33 S3B O7 107.5(13) . . ? O9 S3B O7 102.7(11) . . ? C33 S3B O8B 80.3(17) . . ? O9 S3B O8B 133.8(17) . . ? O7 S3B O8B 115.4(16) . . ? C1 N1 C5 118.2(7) . . ? C1 N1 Nd 121.5(5) . . ? C5 N1 Nd 120.0(5) . . ? C6 N2 C10 118.6(7) . . ? C6 N2 Nd 120.1(5) . . ? C10 N2 Nd 121.2(5) . . ? C15 N3 C11 118.0(7) . . ? C15 N3 Nd 118.9(5) . . ? C11 N3 Nd 122.4(5) . . ? C16 N4 C20 116.9(7) . . ? C16 N4 Nd 120.6(5) . . ? C20 N4 Nd 121.3(5) . . ? C25 N5 C21 117.9(7) . . ? C25 N5 Nd 121.3(5) . . ? C21 N5 Nd 120.7(5) . . ? C26 N6 C30 116.8(7) . . ? C26 N6 Nd 121.6(5) . . ? C30 N6 Nd 121.2(5) . . ? N1 C1 C2 123.5(8) . . ? C3 C2 C1 119.2(11) . . ? C2 C3 C4 118.4(12) . . ? C5 C4 C3 119.3(11) . . ? N1 C5 C4 121.4(9) . . ? N1 C5 C6 117.9(7) . . ? C4 C5 C6 120.5(8) . . ? N2 C6 C7 120.8(8) . . ? N2 C6 C5 118.3(7) . . ? C7 C6 C5 120.8(8) . . ? C8 C7 C6 119.7(9) . . ? C7 C8 C9 119.3(9) . . ? C8 C9 C10 119.7(9) . . ? N2 C10 C9 121.9(8) . . ? N2 C10 C11 117.5(7) . . ? C9 C10 C11 120.6(8) . . ? N3 C11 C12 120.9(8) . . ? N3 C11 C10 116.0(7) . . ? C12 C11 C10 123.1(8) . . ? C13 C12 C11 120.7(9) . . ? C12 C13 C14 118.9(9) . . ? C13 C14 C15 119.3(9) . . ? N3 C15 C14 122.2(9) . . ? N4 C16 C17 124.6(8) . . ? C16 C17 C18 117.9(9) . . ? C19 C18 C17 118.9(10) . . ? C18 C19 C20 119.7(9) . . ? N4 C20 C19 121.8(8) . . ? N4 C20 C21 116.5(7) . . ? C19 C20 C21 121.6(8) . . ? N5 C21 C22 121.7(8) . . ? N5 C21 C20 117.3(7) . . ? C22 C21 C20 120.9(7) . . ? C23 C22 C21 119.4(8) . . ? C24 C23 C22 120.0(8) . . ? C23 C24 C25 117.8(8) . . ? N5 C25 C24 123.1(8) . . ? N5 C25 C26 117.1(7) . . ? C24 C25 C26 119.7(8) . . ? N6 C26 C27 122.1(7) . . ? N6 C26 C25 117.1(7) . . ? C27 C26 C25 120.7(7) . . ? C28 C27 C26 118.9(8) . . ? C29 C28 C27 120.2(8) . . ? C28 C29 C30 117.9(8) . . ? N6 C30 C29 124.1(8) . . ? F2 C31 F1 109.0(8) . . ? F2 C31 F3 106.1(9) . . ? F1 C31 F3 108.8(9) . . ? F2 C31 S1 111.1(7) . . ? F1 C31 S1 111.5(7) . . ? F3 C31 S1 110.1(7) . . ? F6 C32 F5 115.5(16) . . ? F6 C32 F4 115.5(17) . . ? F5 C32 F4 103.9(14) . . ? F6 C32 S2 109.6(14) . . ? F5 C32 S2 107.8(12) . . ? F4 C32 S2 103.7(12) . . ? F7 C33 F8A 105.4(12) . . ? F7 C33 F9 106.5(12) . . ? F8A C33 F9 103.0(12) . . ? F7 C33 S3B 133.4(14) . . ? F9 C33 S3B 119.9(14) . . ? F7 C33 S3A 116.2(10) . . ? F8A C33 S3A 112.4(11) . . ? F9 C33 S3A 112.2(10) . . ? F7 C33 F8B 92.1(17) . . ? F9 C33 F8B 83.3(17) . . ? S3B C33 F8B 89.2(19) . . ? N7 C34 C35 173(3) . . ? #===END data_6.MeCN _database_code_depnum_ccdc_archive 'CCDC 251221' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H25 F9 N7 O9 S3 U' _chemical_formula_weight 1192.83 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.6780(19) _cell_length_b 11.341(2) _cell_length_c 18.659(4) _cell_angle_alpha 94.51(3) _cell_angle_beta 96.33(3) _cell_angle_gamma 102.13(3) _cell_volume 1979.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12381 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1154 _exptl_absorpt_coefficient_mu 4.366 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%. A 180\% range in \f was scanned during data collection with 2\%\f steps and 8 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12381 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 24.71 _reflns_number_total 6215 _reflns_number_gt 5385 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0180P)^2^+9.8960P] 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 6215 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.906 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.131 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 U U -0.28078(2) 0.81378(2) 0.740117(12) 0.01654(8) Uani 1 1 d . . . S1 S -0.06918(17) 0.73509(15) 0.58940(8) 0.0242(4) Uani 1 1 d . . . S2 S -0.37262(16) 0.80633(14) 0.92642(8) 0.0211(3) Uani 1 1 d . . . S3 S -0.2309(2) 0.51169(16) 0.81842(10) 0.0348(4) Uani 1 1 d . . . F1 F 0.1331(4) 0.6472(4) 0.5404(2) 0.0408(10) Uani 1 1 d . . . F2 F -0.0133(5) 0.5181(4) 0.5904(2) 0.0451(11) Uani 1 1 d . . . F3 F 0.1438(4) 0.6597(4) 0.6567(2) 0.0381(10) Uani 1 1 d . . . F4 F -0.4765(5) 0.5753(3) 0.9351(2) 0.0413(11) Uani 1 1 d . . . F5 F -0.4564(4) 0.6910(4) 1.0349(2) 0.0386(10) Uani 1 1 d . . . F6 F -0.6248(4) 0.6915(4) 0.9496(2) 0.0416(10) Uani 1 1 d . . . F7 F -0.1717(7) 0.3114(4) 0.7674(3) 0.080(2) Uani 1 1 d . . . F8 F -0.0437(5) 0.4720(4) 0.7335(3) 0.0547(13) Uani 1 1 d . . . F9 F -0.2622(6) 0.4089(5) 0.6852(3) 0.0701(16) Uani 1 1 d . . . O1 O -0.1335(5) 0.7226(4) 0.6563(2) 0.0250(10) Uani 1 1 d . . . O2 O 0.0225(5) 0.8510(4) 0.5868(3) 0.0326(11) Uani 1 1 d . . . O3 O -0.1664(5) 0.6865(4) 0.5241(2) 0.0335(11) Uani 1 1 d . . . O4 O -0.4171(4) 0.7795(4) 0.8482(2) 0.0229(10) Uani 1 1 d . . . O5 O -0.2309(5) 0.7895(4) 0.9480(2) 0.0283(10) Uani 1 1 d . . . O6 O -0.4086(5) 0.9129(4) 0.9578(2) 0.0267(10) Uani 1 1 d . . . O7 O -0.2419(5) 0.6208(4) 0.7829(3) 0.0300(11) Uani 1 1 d . . . O8 O -0.3651(6) 0.4378(5) 0.8299(3) 0.0526(16) Uani 1 1 d . . . O9 O -0.1173(7) 0.5304(6) 0.8759(3) 0.0628(18) Uani 1 1 d . . . N1 N -0.1720(6) 0.9952(4) 0.6677(3) 0.0205(11) Uani 1 1 d . . . N2 N -0.3880(5) 0.8112(4) 0.6027(3) 0.0194(11) Uani 1 1 d . . . N3 N -0.5083(5) 0.6469(4) 0.6888(3) 0.0212(11) Uani 1 1 d . . . N4 N -0.0282(5) 0.8649(4) 0.8151(3) 0.0202(11) Uani 1 1 d . . . N5 N -0.2129(5) 1.0123(4) 0.8315(3) 0.0173(11) Uani 1 1 d . . . N6 N -0.4655(5) 0.9544(4) 0.7408(3) 0.0207(11) Uani 1 1 d . . . N7 N -0.1765(7) 0.7098(6) 1.1657(4) 0.0471(17) Uani 1 1 d . . . C1 C -0.0635(7) 1.0832(6) 0.6989(4) 0.0267(15) Uani 1 1 d . . . H1A H -0.0250 1.0770 0.7461 0.032 Uiso 1 1 calc R . . C2 C -0.0042(7) 1.1833(6) 0.6659(4) 0.0302(16) Uani 1 1 d . . . H2B H 0.0702 1.2432 0.6906 0.036 Uiso 1 1 calc R . . C3 C -0.0578(8) 1.1920(7) 0.5959(4) 0.0385(18) Uani 1 1 d . . . H3B H -0.0208 1.2581 0.5719 0.046 Uiso 1 1 calc R . . C4 C -0.1683(7) 1.1002(6) 0.5618(4) 0.0319(16) Uani 1 1 d . . . H4A H -0.2063 1.1043 0.5143 0.038 Uiso 1 1 calc R . . C5 C -0.2229(7) 1.0019(6) 0.5978(3) 0.0225(14) Uani 1 1 d . . . C6 C -0.3383(7) 0.9008(5) 0.5618(3) 0.0216(14) Uani 1 1 d . . . C7 C -0.3884(7) 0.8959(6) 0.4885(4) 0.0303(16) Uani 1 1 d . . . H7A H -0.3518 0.9580 0.4615 0.036 Uiso 1 1 calc R . . C8 C -0.4931(7) 0.7979(6) 0.4561(4) 0.0333(17) Uani 1 1 d . . . H8B H -0.5286 0.7940 0.4074 0.040 Uiso 1 1 calc R . . C9 C -0.5443(7) 0.7060(6) 0.4971(4) 0.0298(16) Uani 1 1 d . . . H9B H -0.6152 0.6396 0.4764 0.036 Uiso 1 1 calc R . . C10 C -0.4882(6) 0.7142(5) 0.5697(3) 0.0193(13) Uani 1 1 d . . . C11 C -0.5414(6) 0.6170(6) 0.6152(3) 0.0219(14) Uani 1 1 d . . . C12 C -0.6238(7) 0.5045(6) 0.5861(4) 0.0267(15) Uani 1 1 d . . . H12A H -0.6433 0.4850 0.5361 0.032 Uiso 1 1 calc R . . C13 C -0.6766(7) 0.4214(6) 0.6329(4) 0.0318(16) Uani 1 1 d . . . H13A H -0.7317 0.3455 0.6143 0.038 Uiso 1 1 calc R . . C14 C -0.6480(7) 0.4511(6) 0.7054(4) 0.0289(15) Uani 1 1 d . . . H14A H -0.6843 0.3967 0.7371 0.035 Uiso 1 1 calc R . . C15 C -0.5628(7) 0.5649(6) 0.7319(4) 0.0268(15) Uani 1 1 d . . . H15A H -0.5430 0.5847 0.7819 0.032 Uiso 1 1 calc R . . C16 C 0.0662(7) 0.7961(6) 0.8024(3) 0.0220(14) Uani 1 1 d . . . H16A H 0.0365 0.7286 0.7683 0.026 Uiso 1 1 calc R . . C17 C 0.2037(7) 0.8198(6) 0.8370(3) 0.0229(14) Uani 1 1 d . . . H17A H 0.2648 0.7694 0.8265 0.027 Uiso 1 1 calc R . . C18 C 0.2491(7) 0.9209(6) 0.8879(4) 0.0286(15) Uani 1 1 d . . . H18A H 0.3420 0.9408 0.9114 0.034 Uiso 1 1 calc R . . C19 C 0.1524(7) 0.9915(6) 0.9026(4) 0.0256(15) Uani 1 1 d . . . H19A H 0.1792 1.0585 0.9372 0.031 Uiso 1 1 calc R . . C20 C 0.0152(6) 0.9611(5) 0.8654(3) 0.0185(13) Uani 1 1 d . . . C21 C -0.0925(6) 1.0337(5) 0.8791(3) 0.0198(13) Uani 1 1 d . . . C22 C -0.0671(7) 1.1219(6) 0.9382(3) 0.0232(14) Uani 1 1 d . . . H22A H 0.0144 1.1326 0.9716 0.028 Uiso 1 1 calc R . . C23 C -0.1653(7) 1.1930(6) 0.9464(3) 0.0249(15) Uani 1 1 d . . . H23A H -0.1503 1.2526 0.9854 0.030 Uiso 1 1 calc R . . C24 C -0.2854(7) 1.1749(6) 0.8965(4) 0.0256(14) Uani 1 1 d . . . H24A H -0.3514 1.2233 0.9003 0.031 Uiso 1 1 calc R . . C25 C -0.3061(6) 1.0828(5) 0.8402(3) 0.0203(13) Uani 1 1 d . . . C26 C -0.4386(7) 1.0584(5) 0.7868(3) 0.0209(13) Uani 1 1 d . . . C27 C -0.5311(7) 1.1367(6) 0.7844(4) 0.0272(15) Uani 1 1 d . . . H27A H -0.5079 1.2096 0.8142 0.033 Uiso 1 1 calc R . . C28 C -0.6577(8) 1.1068(6) 0.7378(4) 0.0343(17) Uani 1 1 d . . . H28A H -0.7205 1.1586 0.7363 0.041 Uiso 1 1 calc R . . C29 C -0.6891(7) 0.9972(6) 0.6932(4) 0.0261(15) Uani 1 1 d . . . H29A H -0.7744 0.9733 0.6623 0.031 Uiso 1 1 calc R . . C30 C -0.5902(6) 0.9254(6) 0.6963(3) 0.0204(13) Uani 1 1 d . . . H30A H -0.6106 0.8530 0.6661 0.025 Uiso 1 1 calc R . . C31 C 0.0539(8) 0.6342(6) 0.5948(4) 0.0317(16) Uani 1 1 d . . . C32 C -0.4881(7) 0.6838(6) 0.9625(3) 0.0250(14) Uani 1 1 d . . . C33 C -0.1755(10) 0.4214(7) 0.7468(5) 0.044(2) Uani 1 1 d . . . C34 C -0.1652(7) 0.6510(7) 1.1148(4) 0.0336(17) Uani 1 1 d . . . C35 C -0.1485(8) 0.5769(7) 1.0499(4) 0.0400(18) 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 U 0.01818(13) 0.01438(12) 0.01593(12) 0.00049(8) -0.00021(8) 0.00271(8) S1 0.0228(8) 0.0277(9) 0.0199(8) -0.0042(7) -0.0016(6) 0.0052(7) S2 0.0215(8) 0.0204(8) 0.0196(8) 0.0012(6) 0.0007(6) 0.0019(6) S3 0.0493(12) 0.0309(10) 0.0326(10) 0.0116(8) 0.0140(8) 0.0203(9) F1 0.043(3) 0.059(3) 0.034(2) 0.011(2) 0.0173(19) 0.031(2) F2 0.062(3) 0.031(2) 0.045(3) 0.002(2) 0.010(2) 0.014(2) F3 0.034(2) 0.054(3) 0.030(2) 0.0003(19) -0.0003(18) 0.023(2) F4 0.062(3) 0.020(2) 0.042(3) 0.0075(18) 0.018(2) 0.0033(19) F5 0.046(3) 0.049(3) 0.024(2) 0.0136(19) 0.0072(18) 0.014(2) F6 0.029(2) 0.047(3) 0.049(3) 0.014(2) 0.0082(19) 0.004(2) F7 0.133(5) 0.030(3) 0.102(5) 0.023(3) 0.077(4) 0.038(3) F8 0.058(3) 0.050(3) 0.068(3) 0.017(2) 0.035(3) 0.020(2) F9 0.087(4) 0.065(3) 0.050(3) -0.022(3) 0.013(3) 0.005(3) O1 0.026(2) 0.035(3) 0.017(2) -0.0023(19) 0.0037(18) 0.016(2) O2 0.033(3) 0.030(3) 0.032(3) -0.001(2) 0.004(2) 0.004(2) O3 0.031(3) 0.042(3) 0.024(3) -0.006(2) -0.005(2) 0.008(2) O4 0.029(2) 0.024(2) 0.012(2) 0.0028(18) 0.0028(17) -0.0013(19) O5 0.023(2) 0.035(3) 0.024(3) 0.000(2) -0.0017(19) 0.005(2) O6 0.027(3) 0.025(2) 0.026(3) -0.0021(19) 0.0017(19) 0.005(2) O7 0.034(3) 0.017(2) 0.041(3) 0.012(2) 0.005(2) 0.008(2) O8 0.063(4) 0.036(3) 0.072(4) 0.021(3) 0.038(3) 0.019(3) O9 0.080(5) 0.075(4) 0.041(4) 0.015(3) -0.006(3) 0.042(4) N1 0.028(3) 0.020(3) 0.015(3) 0.004(2) 0.004(2) 0.008(2) N2 0.018(3) 0.018(3) 0.023(3) 0.003(2) 0.004(2) 0.005(2) N3 0.024(3) 0.019(3) 0.019(3) 0.000(2) -0.001(2) 0.002(2) N4 0.022(3) 0.017(3) 0.018(3) -0.002(2) -0.002(2) 0.000(2) N5 0.016(3) 0.016(3) 0.019(3) 0.001(2) 0.002(2) 0.000(2) N6 0.023(3) 0.020(3) 0.018(3) 0.002(2) 0.003(2) 0.004(2) N7 0.050(4) 0.053(4) 0.039(4) 0.005(4) 0.014(3) 0.009(3) C1 0.030(4) 0.026(4) 0.022(4) 0.003(3) 0.004(3) 0.001(3) C2 0.027(4) 0.028(4) 0.034(4) 0.004(3) 0.002(3) 0.004(3) C3 0.035(4) 0.036(4) 0.042(5) 0.015(4) -0.001(3) 0.004(3) C4 0.030(4) 0.037(4) 0.025(4) 0.008(3) -0.003(3) 0.000(3) C5 0.020(3) 0.023(3) 0.025(4) 0.005(3) 0.003(3) 0.007(3) C6 0.023(3) 0.019(3) 0.022(3) -0.001(3) -0.001(3) 0.007(3) C7 0.037(4) 0.033(4) 0.022(4) 0.009(3) 0.003(3) 0.010(3) C8 0.035(4) 0.035(4) 0.027(4) 0.000(3) -0.005(3) 0.007(3) C9 0.033(4) 0.030(4) 0.024(4) -0.002(3) 0.003(3) 0.004(3) C10 0.018(3) 0.022(3) 0.019(3) -0.002(3) 0.002(2) 0.008(3) C11 0.022(3) 0.023(3) 0.018(3) -0.001(3) -0.001(3) 0.003(3) C12 0.024(4) 0.025(4) 0.027(4) -0.003(3) 0.000(3) 0.001(3) C13 0.029(4) 0.025(4) 0.038(4) -0.002(3) 0.003(3) 0.000(3) C14 0.033(4) 0.022(3) 0.027(4) 0.004(3) 0.002(3) -0.005(3) C15 0.025(4) 0.019(3) 0.034(4) -0.003(3) 0.005(3) 0.003(3) C16 0.025(3) 0.028(4) 0.015(3) 0.002(3) 0.003(3) 0.010(3) C17 0.019(3) 0.030(4) 0.023(3) 0.006(3) 0.002(3) 0.013(3) C18 0.021(3) 0.035(4) 0.029(4) 0.009(3) 0.000(3) 0.005(3) C19 0.026(4) 0.025(3) 0.023(4) -0.003(3) -0.005(3) 0.005(3) C20 0.020(3) 0.017(3) 0.017(3) 0.008(2) -0.001(2) 0.000(3) C21 0.023(3) 0.021(3) 0.015(3) 0.004(2) 0.002(2) 0.004(3) C22 0.024(3) 0.028(3) 0.015(3) 0.001(3) 0.001(3) 0.001(3) C23 0.030(4) 0.020(3) 0.021(3) -0.007(3) 0.003(3) -0.001(3) C24 0.029(4) 0.018(3) 0.030(4) 0.001(3) 0.007(3) 0.005(3) C25 0.022(3) 0.018(3) 0.020(3) 0.002(3) 0.005(2) 0.001(3) C26 0.023(3) 0.016(3) 0.023(3) 0.003(3) 0.006(3) -0.001(3) C27 0.030(4) 0.021(3) 0.028(4) -0.005(3) -0.004(3) 0.006(3) C28 0.031(4) 0.032(4) 0.044(5) -0.001(3) 0.002(3) 0.019(3) C29 0.027(4) 0.023(3) 0.024(4) 0.001(3) -0.006(3) 0.001(3) C30 0.020(3) 0.023(3) 0.019(3) 0.001(3) -0.001(2) 0.007(3) C31 0.034(4) 0.036(4) 0.026(4) -0.003(3) 0.008(3) 0.010(3) C32 0.028(4) 0.028(4) 0.020(4) 0.001(3) 0.003(3) 0.008(3) C33 0.071(6) 0.024(4) 0.045(5) 0.011(4) 0.024(4) 0.018(4) C34 0.030(4) 0.033(4) 0.037(5) 0.012(4) 0.004(3) 0.002(3) C35 0.045(5) 0.032(4) 0.039(5) -0.007(3) 0.002(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O7 2.475(4) . ? U O1 2.530(4) . ? U O4 2.540(4) . ? U N4 2.606(5) . ? U N3 2.617(5) . ? U N5 2.634(5) . ? U N6 2.634(5) . ? U N1 2.647(5) . ? U N2 2.654(5) . ? S1 O2 1.431(5) . ? S1 O3 1.448(5) . ? S1 O1 1.459(5) . ? S1 C31 1.818(7) . ? S2 O6 1.428(5) . ? S2 O5 1.442(5) . ? S2 O4 1.465(4) . ? S2 C32 1.815(7) . ? S3 O9 1.419(6) . ? S3 O8 1.438(6) . ? S3 O7 1.466(4) . ? S3 C33 1.815(8) . ? F1 C31 1.336(8) . ? F2 C31 1.332(8) . ? F3 C31 1.339(8) . ? F4 C32 1.327(7) . ? F5 C32 1.343(7) . ? F6 C32 1.340(8) . ? F7 C33 1.341(8) . ? F8 C33 1.343(9) . ? F9 C33 1.326(10) . ? N1 C1 1.332(8) . ? N1 C5 1.355(8) . ? N2 C10 1.358(8) . ? N2 C6 1.358(8) . ? N3 C15 1.340(8) . ? N3 C11 1.373(8) . ? N4 C20 1.345(8) . ? N4 C16 1.347(8) . ? N5 C25 1.339(8) . ? N5 C21 1.350(8) . ? N6 C30 1.350(8) . ? N6 C26 1.363(8) . ? N7 C34 1.144(10) . ? C1 C2 1.383(9) . ? C2 C3 1.371(10) . ? C3 C4 1.382(10) . ? C4 C5 1.387(9) . ? C5 C6 1.479(9) . ? C6 C7 1.392(9) . ? C7 C8 1.382(10) . ? C8 C9 1.381(10) . ? C9 C10 1.391(9) . ? C10 C11 1.486(9) . ? C11 C12 1.388(9) . ? C12 C13 1.392(10) . ? C13 C14 1.351(10) . ? C14 C15 1.398(9) . ? C16 C17 1.375(9) . ? C17 C18 1.391(9) . ? C18 C19 1.389(9) . ? C19 C20 1.389(8) . ? C20 C21 1.489(9) . ? C21 C22 1.393(9) . ? C22 C23 1.383(9) . ? C23 C24 1.376(9) . ? C24 C25 1.389(9) . ? C25 C26 1.497(9) . ? C26 C27 1.387(9) . ? C27 C28 1.384(9) . ? C28 C29 1.398(9) . ? C29 C30 1.381(9) . ? C34 C35 1.463(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 U O1 71.13(15) . . ? O7 U O4 73.46(15) . . ? O1 U O4 144.47(14) . . ? O7 U N4 74.01(15) . . ? O1 U N4 77.38(15) . . ? O4 U N4 95.70(15) . . ? O7 U N3 73.17(16) . . ? O1 U N3 91.17(15) . . ? O4 U N3 75.84(15) . . ? N4 U N3 147.16(16) . . ? O7 U N5 119.12(15) . . ? O1 U N5 130.53(15) . . ? O4 U N5 71.03(14) . . ? N4 U N5 62.46(15) . . ? N3 U N5 138.12(15) . . ? O7 U N6 140.67(16) . . ? O1 U N6 141.22(15) . . ? O4 U N6 70.73(15) . . ? N4 U N6 124.96(15) . . ? N3 U N6 82.75(16) . . ? N5 U N6 62.70(15) . . ? O7 U N1 143.45(16) . . ? O1 U N1 75.86(15) . . ? O4 U N1 138.74(14) . . ? N4 U N1 83.97(16) . . ? N3 U N1 123.35(16) . . ? N5 U N1 72.50(15) . . ? N6 U N1 75.88(16) . . ? O7 U N2 118.05(15) . . ? O1 U N2 69.44(14) . . ? O4 U N2 127.46(14) . . ? N4 U N2 136.64(16) . . ? N3 U N2 62.05(16) . . ? N5 U N2 122.83(15) . . ? N6 U N2 73.98(15) . . ? N1 U N2 61.76(15) . . ? O2 S1 O3 115.7(3) . . ? O2 S1 O1 114.2(3) . . ? O3 S1 O1 114.4(3) . . ? O2 S1 C31 103.0(3) . . ? O3 S1 C31 104.0(3) . . ? O1 S1 C31 103.4(3) . . ? O6 S2 O5 117.1(3) . . ? O6 S2 O4 114.3(3) . . ? O5 S2 O4 112.9(3) . . ? O6 S2 C32 103.7(3) . . ? O5 S2 C32 104.1(3) . . ? O4 S2 C32 102.4(3) . . ? O9 S3 O8 117.1(4) . . ? O9 S3 O7 114.1(3) . . ? O8 S3 O7 114.7(3) . . ? O9 S3 C33 104.4(4) . . ? O8 S3 C33 102.9(4) . . ? O7 S3 C33 100.8(3) . . ? S1 O1 U 144.5(3) . . ? S2 O4 U 132.0(2) . . ? S3 O7 U 170.5(3) . . ? C1 N1 C5 117.5(5) . . ? C1 N1 U 120.6(4) . . ? C5 N1 U 121.8(4) . . ? C10 N2 C6 117.9(5) . . ? C10 N2 U 120.0(4) . . ? C6 N2 U 121.9(4) . . ? C15 N3 C11 117.6(5) . . ? C15 N3 U 119.0(4) . . ? C11 N3 U 119.7(4) . . ? C20 N4 C16 117.5(5) . . ? C20 N4 U 122.4(4) . . ? C16 N4 U 120.1(4) . . ? C25 N5 C21 118.2(5) . . ? C25 N5 U 121.1(4) . . ? C21 N5 U 119.8(4) . . ? C30 N6 C26 117.9(5) . . ? C30 N6 U 121.3(4) . . ? C26 N6 U 120.9(4) . . ? N1 C1 C2 124.2(6) . . ? C3 C2 C1 118.4(7) . . ? C2 C3 C4 118.3(7) . . ? C3 C4 C5 120.5(6) . . ? N1 C5 C4 120.9(6) . . ? N1 C5 C6 117.6(5) . . ? C4 C5 C6 121.5(6) . . ? N2 C6 C7 121.9(6) . . ? N2 C6 C5 116.8(5) . . ? C7 C6 C5 121.2(6) . . ? C8 C7 C6 119.5(6) . . ? C9 C8 C7 119.2(6) . . ? C8 C9 C10 119.0(6) . . ? N2 C10 C9 122.5(6) . . ? N2 C10 C11 117.2(5) . . ? C9 C10 C11 120.3(6) . . ? N3 C11 C12 121.6(6) . . ? N3 C11 C10 115.7(5) . . ? C12 C11 C10 122.7(6) . . ? C11 C12 C13 118.9(6) . . ? C14 C13 C12 120.0(6) . . ? C13 C14 C15 118.8(6) . . ? N3 C15 C14 123.1(6) . . ? N4 C16 C17 123.9(6) . . ? C16 C17 C18 118.4(6) . . ? C19 C18 C17 118.4(6) . . ? C20 C19 C18 119.5(6) . . ? N4 C20 C19 122.2(6) . . ? N4 C20 C21 116.1(5) . . ? C19 C20 C21 121.7(5) . . ? N5 C21 C22 121.9(6) . . ? N5 C21 C20 117.6(5) . . ? C22 C21 C20 120.5(5) . . ? C23 C22 C21 118.9(6) . . ? C24 C23 C22 119.4(6) . . ? C23 C24 C25 118.5(6) . . ? N5 C25 C24 123.0(6) . . ? N5 C25 C26 117.6(5) . . ? C24 C25 C26 119.5(6) . . ? N6 C26 C27 121.2(6) . . ? N6 C26 C25 116.9(5) . . ? C27 C26 C25 121.9(5) . . ? C28 C27 C26 120.2(6) . . ? C27 C28 C29 118.7(6) . . ? C30 C29 C28 118.2(6) . . ? N6 C30 C29 123.6(6) . . ? F2 C31 F1 107.9(5) . . ? F2 C31 F3 107.9(6) . . ? F1 C31 F3 107.1(6) . . ? F2 C31 S1 112.3(5) . . ? F1 C31 S1 109.8(5) . . ? F3 C31 S1 111.6(5) . . ? F4 C32 F6 108.6(5) . . ? F4 C32 F5 107.8(5) . . ? F6 C32 F5 106.5(5) . . ? F4 C32 S2 112.4(4) . . ? F6 C32 S2 110.8(4) . . ? F5 C32 S2 110.4(4) . . ? F9 C33 F7 109.1(7) . . ? F9 C33 F8 107.6(7) . . ? F7 C33 F8 107.1(7) . . ? F9 C33 S3 112.0(6) . . ? F7 C33 S3 109.6(5) . . ? F8 C33 S3 111.2(6) . . ? N7 C34 C35 179.1(8) . . ? #===END data_8.2MeCN.H~2~O _database_code_depnum_ccdc_archive 'CCDC 251222' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H63 I8 N17 O3 U3' _chemical_formula_weight 3027.75 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' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 '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 12.451(3) _cell_length_b 16.542(3) _cell_length_c 24.314(5) _cell_angle_alpha 105.59(3) _cell_angle_beta 93.73(3) _cell_angle_gamma 110.57(3) _cell_volume 4445.1(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25847 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 8.284 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_T_max 0.447 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25847 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1555 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.69 _reflns_number_total 13709 _reflns_number_gt 7636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of water molecule) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. One iodure atom (I8)is found disordered on three positions with 0.398(4),0.308(5) and 0.293(5) occupations factors. ; _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^)+(0.1052P)^2^+60.3167P] 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 13709 _refine_ls_number_parameters 1012 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1746 _refine_ls_R_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.2400 _refine_ls_wR_factor_gt 0.1956 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.014 _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.881 _refine_diff_density_min -0.951 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 -0.06594(3) 0.83776(2) 0.119660(16) 0.03056(11) Uani 1 1 d . . . U2 U -0.02434(3) 0.72251(2) 0.248202(17) 0.03590(12) Uani 1 1 d . . . U3 U -0.04296(3) 0.59963(2) 0.377530(17) 0.03643(12) Uani 1 1 d . . . I8A I 0.26118(13) 1.33432(12) 0.32244(8) 0.0435(6) Uani 0.3986(4) 1 d P . . I8C I 0.2716(4) 1.3329(3) 0.3047(3) 0.166(2) Uani 0.3082(5) 1 d P . . I8B I 0.2554(3) 1.2998(3) 0.31804(17) 0.0923(15) Uani 0.2934(5) 1 d P . . I1 I 0.06782(8) 0.77091(6) 0.03338(5) 0.0846(4) Uani 1 1 d . . . I2 I 0.06257(8) 0.91246(6) 0.33764(4) 0.0799(4) Uani 1 1 d . . . I3 I 0.24165(7) 0.76282(6) 0.27084(4) 0.0804(3) Uani 1 1 d . . . I4 I 0.21756(8) 0.66754(7) 0.41734(5) 0.0870(4) Uani 1 1 d . . . I5 I 0.65540(6) 1.13541(5) 0.11953(3) 0.0475(2) Uani 1 1 d . . . I6 I 0.61356(7) 1.06373(6) 0.33033(5) 0.0795(4) Uani 1 1 d . . . I7 I 0.30813(5) 0.43023(5) 0.11271(3) 0.0465(2) Uani 1 1 d . . . O1 O -0.0299(5) 0.7838(4) 0.1805(2) 0.0310(19) Uani 1 1 d . . . O1W O -0.6177(7) 0.3051(5) 0.1957(4) 0.077(4) Uani 1 1 d . . . O2 O -0.0339(5) 0.6683(4) 0.3160(3) 0.043(2) Uani 1 1 d . . . N1 N 0.1502(6) 0.9477(5) 0.1595(4) 0.040(3) Uani 1 1 d . . . N2 N 0.0082(6) 0.9902(5) 0.0937(3) 0.032(2) Uani 1 1 d . . . N3 N -0.1850(6) 0.8531(4) 0.0347(3) 0.032(2) Uani 1 1 d . . . N4 N -0.0847(6) 0.9637(5) 0.2008(4) 0.044(3) Uani 1 1 d . . . N5 N -0.2734(5) 0.8103(4) 0.1380(4) 0.036(2) Uani 1 1 d . . . N6 N -0.2176(7) 0.6751(5) 0.0804(3) 0.039(3) Uani 1 1 d . . . N7 N -0.2336(6) 0.7256(5) 0.2587(4) 0.045(3) Uani 1 1 d . . . N8 N -0.2056(7) 0.5735(5) 0.1994(3) 0.044(3) Uani 1 1 d . . . N9 N 0.0079(7) 0.6096(6) 0.1625(4) 0.059(3) Uani 1 1 d . . . N10 N -0.2435(6) 0.6139(5) 0.3717(3) 0.045(3) Uani 1 1 d . . . N11 N -0.2235(6) 0.4591(5) 0.3198(3) 0.033(2) Uani 1 1 d . . . N12 N -0.0117(5) 0.4837(5) 0.2926(3) 0.034(2) Uani 1 1 d . . . N13 N -0.0199(8) 0.7401(5) 0.4604(4) 0.054(3) Uani 1 1 d . . . N14 N -0.1311(6) 0.5727(5) 0.4667(4) 0.043(3) Uani 1 1 d . . . N15 N -0.0404(7) 0.4675(5) 0.4122(3) 0.040(3) Uani 1 1 d . . . N16 N -0.6169(13) 0.8806(7) 0.0448(6) 0.125(6) Uani 1 1 d . . . N17 N -0.5205(12) 0.2867(9) 0.4591(8) 0.147(8) Uani 1 1 d . . . C1 C 0.2191(8) 0.9209(7) 0.1869(5) 0.048(4) Uani 1 1 d . . . H1A H 0.1863 0.8634 0.1911 0.058 Uiso 1 1 calc R . . C2 C 0.3360(8) 0.9704(6) 0.2101(5) 0.044(3) Uani 1 1 d . . . H2A H 0.3783 0.9509 0.2328 0.053 Uiso 1 1 calc R . . C3 C 0.3868(8) 1.0516(7) 0.1971(5) 0.057(4) Uani 1 1 d . . . H3A H 0.4666 1.0850 0.2080 0.068 Uiso 1 1 calc R . . C4 C 0.3169(8) 1.0820(7) 0.1680(4) 0.041(3) Uani 1 1 d . . . H4A H 0.3483 1.1380 0.1617 0.049 Uiso 1 1 calc R . . C5 C 0.1928(8) 1.0246(6) 0.1471(4) 0.039(3) Uani 1 1 d . . . C6 C 0.1145(7) 1.0504(5) 0.1164(4) 0.031(3) Uani 1 1 d . . . C7 C 0.1429(7) 1.1404(6) 0.1157(4) 0.042(4) Uani 1 1 d . . . H7A H 0.2169 1.1841 0.1328 0.051 Uiso 1 1 calc R . . C8 C 0.0605(8) 1.1641(6) 0.0896(5) 0.051(3) Uani 1 1 d . . . H8A H 0.0789 1.2236 0.0893 0.062 Uiso 1 1 calc R . . C9 C -0.0517(8) 1.0965(6) 0.0634(5) 0.050(4) Uani 1 1 d . . . H9A H -0.1095 1.1093 0.0456 0.060 Uiso 1 1 calc R . . C10 C -0.0696(8) 1.0099(6) 0.0659(4) 0.039(3) Uani 1 1 d . . . C11 C -0.1828(6) 0.9354(5) 0.0364(4) 0.030(3) Uani 1 1 d . . . C12 C -0.2705(8) 0.9469(6) 0.0065(4) 0.042(3) Uani 1 1 d . . . H12A H -0.2649 1.0052 0.0087 0.051 Uiso 1 1 calc R . . C13 C -0.3657(8) 0.8740(7) -0.0263(5) 0.054(4) Uani 1 1 d . . . H13A H -0.4280 0.8820 -0.0440 0.065 Uiso 1 1 calc R . . C14 C -0.3678(7) 0.7867(6) -0.0328(4) 0.040(3) Uani 1 1 d . . . H14A H -0.4265 0.7352 -0.0584 0.048 Uiso 1 1 calc R . . C15 C -0.2793(8) 0.7806(6) 0.0005(5) 0.045(4) Uani 1 1 d . . . H15A H -0.2839 0.7229 -0.0005 0.053 Uiso 1 1 calc R . . C16 C -0.0033(10) 1.0283(7) 0.2349(5) 0.064(4) Uani 1 1 d . . . H16C H 0.0665 1.0198 0.2387 0.077 Uiso 1 1 calc R . . C17 C 0.0005(12) 1.1138(9) 0.2694(6) 0.087(6) Uani 1 1 d . . . H17A H 0.0672 1.1582 0.2944 0.105 Uiso 1 1 calc R . . C18 C -0.0998(13) 1.1248(8) 0.2627(5) 0.089(6) Uani 1 1 d . . . H18A H -0.1046 1.1790 0.2837 0.107 Uiso 1 1 calc R . . C19 C -0.1972(9) 1.0571(6) 0.2251(4) 0.085(3) Uani 1 1 d . . . H19A H -0.2638 1.0680 0.2169 0.102 Uiso 1 1 calc R . . C20 C -0.1934(10) 0.9690(6) 0.1990(4) 0.046(4) Uani 1 1 d . . . C21 C -0.2911(7) 0.8854(6) 0.1680(4) 0.038(3) Uani 1 1 d . . . C22 C -0.4088(9) 0.8823(8) 0.1707(6) 0.066(4) Uani 1 1 d . . . H22A H -0.4221 0.9349 0.1869 0.079 Uiso 1 1 calc R . . C23 C -0.4966(9) 0.8022(9) 0.1495(5) 0.080(5) Uani 1 1 d . . . H23A H -0.5719 0.7982 0.1533 0.096 Uiso 1 1 calc R . . C24 C -0.4783(9) 0.7214(9) 0.1207(5) 0.071(5) Uani 1 1 d . . . H24A H -0.5413 0.6662 0.1051 0.085 Uiso 1 1 calc R . . C25 C -0.3647(8) 0.7264(6) 0.1164(4) 0.042(3) Uani 1 1 d . . . C26 C -0.3328(9) 0.6533(8) 0.0913(4) 0.052(4) Uani 1 1 d . . . C27 C -0.4053(9) 0.5605(7) 0.0773(4) 0.051(4) Uani 1 1 d . . . H27A H -0.4792 0.5462 0.0871 0.061 Uiso 1 1 calc R . . C28 C -0.3755(9) 0.4922(7) 0.0512(5) 0.060(4) Uani 1 1 d . . . H28A H -0.4271 0.4321 0.0419 0.072 Uiso 1 1 calc R . . C29 C -0.2620(10) 0.5148(6) 0.0382(4) 0.054(4) Uani 1 1 d . . . H29A H -0.2379 0.4698 0.0180 0.065 Uiso 1 1 calc R . . C30 C -0.1888(9) 0.6033(6) 0.0556(5) 0.049(4) Uani 1 1 d . . . H30A H -0.1121 0.6161 0.0501 0.059 Uiso 1 1 calc R . . C31 C -0.2494(10) 0.8049(7) 0.2795(5) 0.065(4) Uani 1 1 d . . . H31A H -0.1851 0.8596 0.2905 0.078 Uiso 1 1 calc R . . C32 C -0.3566(8) 0.8060(6) 0.2844(5) 0.050(3) Uani 1 1 d . . . H32A H -0.3654 0.8609 0.2991 0.061 Uiso 1 1 calc R . . C33 C -0.4480(9) 0.7292(7) 0.2683(5) 0.054(4) Uani 1 1 d . . . H33A H -0.5218 0.7293 0.2722 0.065 Uiso 1 1 calc R . . C34 C -0.4338(9) 0.6458(7) 0.2450(5) 0.061(4) Uani 1 1 d . . . H34A H -0.4966 0.5901 0.2334 0.073 Uiso 1 1 calc R . . C35 C -0.3232(8) 0.6519(7) 0.2406(5) 0.053(4) Uani 1 1 d . . . C36 C -0.3053(8) 0.5631(6) 0.2159(4) 0.042(3) Uani 1 1 d . . . C37 C -0.3859(8) 0.4758(6) 0.2075(5) 0.053(4) Uani 1 1 d . . . H37A H -0.4549 0.4679 0.2220 0.063 Uiso 1 1 calc R . . C38 C -0.3655(9) 0.4030(6) 0.1790(4) 0.051(3) Uani 1 1 d . . . H38A H -0.4227 0.3453 0.1717 0.061 Uiso 1 1 calc R . . C39 C -0.2693(9) 0.4113(7) 0.1616(5) 0.063(4) Uani 1 1 d . . . H39A H -0.2556 0.3597 0.1432 0.076 Uiso 1 1 calc R . . C40 C -0.1837(8) 0.4978(6) 0.1699(4) 0.045(3) Uani 1 1 d . . . C41 C -0.0717(7) 0.5197(6) 0.1447(5) 0.050(3) Uani 1 1 d . . . C42 C -0.0503(9) 0.4508(7) 0.1003(5) 0.060(4) Uani 1 1 d . . . H42A H -0.1021 0.3904 0.0886 0.072 Uiso 1 1 calc R . . C43 C 0.0406(9) 0.4749(9) 0.0781(7) 0.097(6) Uani 1 1 d . . . H43A H 0.0565 0.4290 0.0528 0.117 Uiso 1 1 calc R . . C44 C 0.1153(12) 0.5596(8) 0.0875(4) 0.077(5) Uani 1 1 d . . . H44A H 0.1756 0.5754 0.0669 0.092 Uiso 1 1 calc R . . C45 C 0.0919(9) 0.6256(8) 0.1342(5) 0.060(4) Uani 1 1 d . . . H45A H 0.1441 0.6857 0.1442 0.072 Uiso 1 1 calc R . . C46 C -0.2565(7) 0.6927(7) 0.3906(4) 0.047(3) Uani 1 1 d . . . H46A H -0.1906 0.7457 0.3978 0.057 Uiso 1 1 calc R . . C47 C -0.3592(12) 0.7017(7) 0.4000(6) 0.084(5) Uani 1 1 d . . . H47A H -0.3625 0.7590 0.4124 0.101 Uiso 1 1 calc R . . C48 C -0.4587(8) 0.6241(6) 0.3909(5) 0.054(3) Uani 1 1 d . . . H48A H -0.5287 0.6285 0.3991 0.065 Uiso 1 1 calc R . . C49 C -0.4516(9) 0.5348(7) 0.3680(4) 0.054(4) Uani 1 1 d . . . H49A H -0.5158 0.4802 0.3588 0.065 Uiso 1 1 calc R . . C50 C -0.3405(7) 0.5397(6) 0.3615(4) 0.042(3) Uani 1 1 d . . . C51 C -0.3260(8) 0.4515(7) 0.3350(4) 0.041(3) Uani 1 1 d . . . C52 C -0.4103(8) 0.3679(6) 0.3299(4) 0.044(3) Uani 1 1 d . . . H52A H -0.4775 0.3640 0.3455 0.053 Uiso 1 1 calc R . . C53 C -0.3924(8) 0.2845(6) 0.2992(5) 0.051(3) Uani 1 1 d . . . H53A H -0.4492 0.2269 0.2931 0.061 Uiso 1 1 calc R . . C54 C -0.2931(9) 0.2953(6) 0.2811(5) 0.048(4) Uani 1 1 d . . . H54A H -0.2800 0.2437 0.2621 0.057 Uiso 1 1 calc R . . C55 C -0.2037(8) 0.3822(5) 0.2890(4) 0.034(3) Uani 1 1 d . . . C56 C -0.0935(7) 0.4002(6) 0.2681(4) 0.031(3) Uani 1 1 d . . . C57 C -0.0743(8) 0.3373(6) 0.2264(5) 0.050(4) Uani 1 1 d . . . H57A H -0.1317 0.2792 0.2107 0.059 Uiso 1 1 calc R . . C58 C 0.0332(9) 0.3594(7) 0.2064(5) 0.067(4) Uani 1 1 d . . . H58A H 0.0477 0.3171 0.1772 0.080 Uiso 1 1 calc R . . C59 C 0.1138(8) 0.4441(7) 0.2311(5) 0.047(4) Uani 1 1 d . . . H59A H 0.1861 0.4591 0.2196 0.057 Uiso 1 1 calc R . . C60 C 0.0923(7) 0.5137(6) 0.2754(4) 0.040(3) Uani 1 1 d . . . H60A H 0.1456 0.5734 0.2904 0.047 Uiso 1 1 calc R . . C61 C 0.0478(11) 0.8183(8) 0.4660(5) 0.070(5) Uani 1 1 d . . . H61A H 0.0976 0.8243 0.4391 0.084 Uiso 1 1 calc R . . C62 C 0.0584(13) 0.8960(9) 0.5061(6) 0.087(6) Uani 1 1 d . . . H62A H 0.1134 0.9506 0.5052 0.104 Uiso 1 1 calc R . . C63 C -0.0099(17) 0.8970(9) 0.5487(8) 0.134(8) Uani 1 1 d . . . H63A H -0.0020 0.9499 0.5774 0.160 Uiso 1 1 calc R . . C64 C -0.0951(11) 0.8082(7) 0.5447(7) 0.143(5) Uani 1 1 d . . . H64A H -0.1494 0.8017 0.5694 0.172 Uiso 1 1 calc R . . C65 C -0.0925(11) 0.7314(7) 0.5016(5) 0.067(5) Uani 1 1 d . . . C66 C -0.1624(9) 0.6390(8) 0.4951(4) 0.065(4) Uani 1 1 d . . . C67 C -0.2667(10) 0.6177(8) 0.5218(6) 0.111(4) Uani 1 1 d . . . H67A H -0.2922 0.6630 0.5401 0.134 Uiso 1 1 calc R . . C68 C -0.3249(11) 0.5304(9) 0.5191(6) 0.100(6) Uani 1 1 d . . . H68A H -0.3892 0.5150 0.5372 0.121 Uiso 1 1 calc R . . C69 C -0.2850(10) 0.4590(9) 0.4867(5) 0.071(5) Uani 1 1 d . . . H69A H -0.3267 0.3983 0.4830 0.086 Uiso 1 1 calc R . . C70 C -0.1900(7) 0.4821(6) 0.4632(4) 0.036(3) Uani 1 1 d . . . C71 C -0.1403(8) 0.4197(6) 0.4348(5) 0.045(3) Uani 1 1 d . . . C72 C -0.1730(10) 0.3344(7) 0.4312(5) 0.062(4) Uani 1 1 d . . . H72A H -0.2397 0.3094 0.4458 0.074 Uiso 1 1 calc R . . C73 C -0.1187(8) 0.2784(6) 0.4078(5) 0.049(4) Uani 1 1 d . . . H73A H -0.1478 0.2168 0.4041 0.059 Uiso 1 1 calc R . . C74 C -0.0166(8) 0.3210(5) 0.3902(4) 0.034(3) Uani 1 1 d . . . H74A H 0.0294 0.2883 0.3777 0.041 Uiso 1 1 calc R . . C75 C 0.0203(9) 0.4106(6) 0.3904(4) 0.044(3) Uani 1 1 d . . . H75A H 0.0874 0.4344 0.3758 0.053 Uiso 1 1 calc R . . C76 C -0.6340(12) 0.7827(8) 0.0257(6) 0.087(5) Uani 1 1 d . . . C77 C -0.6581(10) 0.7093(6) 0.0091(6) 0.068(5) Uani 1 1 d . . . H77A H -0.5930 0.6947 0.0195 0.103 Uiso 1 1 calc R . . H77B H -0.6798 0.6891 -0.0324 0.103 Uiso 1 1 calc R . . H77C H -0.7228 0.6794 0.0256 0.103 Uiso 1 1 calc R . . C78 C -0.5725(10) 0.2192(10) 0.4321(7) 0.107(6) Uani 1 1 d . . . C79 C -0.6568(15) 0.1260(10) 0.3773(9) 0.150(10) Uani 1 1 d . . . H79A H -0.6738 0.0733 0.3899 0.224 Uiso 1 1 calc R . . H79B H -0.6164 0.1198 0.3451 0.224 Uiso 1 1 calc R . . H79C H -0.7282 0.1317 0.3657 0.224 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 0.03235(15) 0.02479(14) 0.03475(19) 0.00825(13) 0.00491(14) 0.01217(11) U2 0.04280(17) 0.03190(15) 0.0342(2) 0.00917(14) 0.00414(15) 0.01698(13) U3 0.04312(17) 0.03270(16) 0.0331(2) 0.00827(15) 0.00374(15) 0.01605(13) I8A 0.0254(7) 0.0507(9) 0.0424(9) 0.0123(8) 0.0057(7) 0.0025(7) I8C 0.087(3) 0.141(3) 0.220(5) 0.087(3) -0.054(3) -0.021(3) I8B 0.0662(18) 0.121(3) 0.087(2) 0.048(2) 0.0161(17) 0.0208(18) I1 0.0903(5) 0.0762(5) 0.0889(7) 0.0294(5) 0.0194(5) 0.0304(4) I2 0.1026(6) 0.0553(4) 0.0670(6) 0.0037(4) 0.0036(5) 0.0266(4) I3 0.0612(4) 0.0949(5) 0.0984(6) 0.0478(4) 0.0128(4) 0.0324(4) I4 0.0840(5) 0.0907(5) 0.0849(7) 0.0322(5) 0.0058(5) 0.0300(4) I5 0.0424(3) 0.0426(3) 0.0461(4) 0.0028(3) -0.0009(3) 0.0128(3) I6 0.0650(5) 0.0556(4) 0.0997(7) 0.0104(5) -0.0067(5) 0.0159(4) I7 0.0380(3) 0.0519(3) 0.0480(4) 0.0155(3) 0.0112(3) 0.0146(3) O1 0.048(3) 0.026(3) 0.014(3) 0.001(2) 0.006(2) 0.012(2) O1W 0.047(4) 0.049(5) 0.096(7) 0.010(5) 0.002(4) -0.014(4) O2 0.047(3) 0.044(3) 0.042(4) 0.011(3) 0.009(3) 0.025(2) N1 0.024(3) 0.027(3) 0.059(6) 0.006(4) -0.017(4) 0.006(3) N2 0.036(4) 0.021(3) 0.030(4) 0.010(3) -0.003(3) 0.000(3) N3 0.052(4) 0.016(3) 0.024(4) 0.005(3) 0.001(3) 0.009(3) N4 0.045(4) 0.022(3) 0.061(6) 0.005(4) 0.002(4) 0.015(3) N5 0.025(3) 0.038(3) 0.064(5) 0.029(3) 0.014(3) 0.021(2) N6 0.055(4) 0.037(4) 0.014(4) 0.006(3) -0.010(3) 0.010(3) N7 0.032(3) 0.041(3) 0.075(6) 0.026(4) 0.003(4) 0.022(3) N8 0.057(5) 0.046(4) 0.021(4) 0.012(3) -0.010(4) 0.013(3) N9 0.061(5) 0.068(5) 0.037(5) 0.000(4) -0.012(4) 0.028(4) N10 0.053(4) 0.060(4) 0.030(4) 0.010(4) 0.015(3) 0.035(3) N11 0.022(3) 0.029(3) 0.040(4) 0.012(3) -0.002(3) 0.001(3) N12 0.032(3) 0.064(4) 0.032(4) 0.030(3) 0.020(3) 0.034(3) N13 0.103(6) 0.031(4) 0.022(5) -0.003(3) 0.005(4) 0.029(4) N14 0.036(4) 0.047(4) 0.042(5) 0.014(4) 0.007(4) 0.012(3) N15 0.050(4) 0.033(3) 0.039(5) 0.018(3) 0.002(4) 0.012(3) N16 0.204(12) 0.040(6) 0.084(8) 0.007(6) -0.068(8) 0.018(7) N17 0.115(9) 0.090(9) 0.176(15) -0.028(10) 0.041(9) 0.019(8) C1 0.032(5) 0.042(5) 0.062(7) 0.011(5) 0.007(5) 0.007(4) C2 0.044(5) 0.034(4) 0.053(6) 0.004(4) 0.021(4) 0.018(4) C3 0.040(5) 0.084(6) 0.067(7) 0.039(5) 0.019(5) 0.034(4) C4 0.034(5) 0.042(5) 0.036(5) 0.018(4) 0.010(4) -0.003(4) C5 0.057(5) 0.046(5) 0.016(5) 0.006(4) 0.002(4) 0.026(4) C6 0.028(4) 0.007(3) 0.056(6) 0.006(4) 0.001(4) 0.009(3) C7 0.031(4) 0.040(5) 0.030(5) -0.009(5) 0.015(4) -0.004(4) C8 0.076(5) 0.055(4) 0.054(6) 0.022(4) 0.034(4) 0.054(3) C9 0.028(4) 0.045(5) 0.087(7) 0.044(4) 0.013(5) 0.009(4) C10 0.048(5) 0.048(5) 0.020(5) 0.008(4) 0.006(4) 0.020(4) C11 0.020(3) 0.034(4) 0.049(5) 0.024(4) 0.018(3) 0.016(3) C12 0.050(5) 0.021(4) 0.034(6) -0.012(4) -0.010(5) 0.006(4) C13 0.044(5) 0.055(5) 0.067(8) 0.012(5) 0.003(5) 0.031(4) C14 0.022(4) 0.038(5) 0.036(6) 0.007(4) -0.002(4) -0.011(4) C15 0.032(5) 0.012(4) 0.082(8) 0.014(4) 0.003(5) 0.002(3) C16 0.063(6) 0.024(5) 0.071(7) -0.003(5) 0.037(5) -0.014(5) C17 0.068(8) 0.075(8) 0.092(9) 0.044(7) 0.007(7) -0.017(7) C18 0.135(10) 0.058(7) 0.036(8) -0.033(6) -0.032(7) 0.036(6) C19 0.186(5) 0.128(4) 0.023(5) 0.025(4) 0.030(5) 0.151(3) C20 0.095(7) 0.019(4) 0.016(5) 0.006(4) 0.015(5) 0.013(4) C21 0.043(4) 0.048(4) 0.046(5) 0.033(4) 0.027(4) 0.026(3) C22 0.054(6) 0.059(6) 0.095(8) 0.045(6) 0.029(6) 0.015(5) C23 0.047(5) 0.139(9) 0.069(8) 0.025(7) 0.035(5) 0.055(5) C24 0.028(5) 0.121(9) 0.046(6) 0.049(6) -0.009(5) -0.008(6) C25 0.043(5) 0.039(5) 0.037(6) 0.005(4) 0.009(4) 0.014(4) C26 0.045(6) 0.064(7) 0.019(5) 0.007(5) -0.021(5) -0.002(5) C27 0.040(5) 0.065(7) 0.023(5) 0.010(5) -0.007(4) -0.002(5) C28 0.053(6) 0.037(5) 0.076(8) 0.019(5) -0.007(6) 0.004(5) C29 0.093(7) 0.029(4) 0.031(6) 0.010(4) -0.025(5) 0.017(4) C30 0.054(6) 0.039(5) 0.051(6) 0.022(4) -0.002(5) 0.011(4) C31 0.098(7) 0.055(5) 0.067(7) 0.036(5) 0.013(6) 0.045(4) C32 0.077(5) 0.038(4) 0.063(7) 0.014(4) 0.024(5) 0.053(3) C33 0.044(5) 0.073(6) 0.048(6) 0.033(5) 0.018(5) 0.013(5) C34 0.066(6) 0.055(6) 0.049(7) -0.003(5) -0.017(6) 0.028(4) C35 0.038(5) 0.045(5) 0.049(7) -0.018(5) -0.027(5) 0.013(4) C36 0.060(5) 0.056(5) 0.019(5) 0.018(4) 0.011(4) 0.028(4) C37 0.028(4) 0.026(4) 0.108(9) 0.025(5) 0.023(5) 0.008(3) C38 0.064(6) 0.061(5) 0.038(5) 0.037(4) -0.012(5) 0.022(4) C39 0.054(6) 0.038(5) 0.063(8) -0.016(6) -0.041(6) 0.010(4) C40 0.058(5) 0.038(5) 0.032(6) 0.002(4) -0.013(5) 0.023(4) C41 0.051(4) 0.076(4) 0.051(6) 0.033(4) -0.002(4) 0.050(3) C42 0.064(6) 0.049(5) 0.055(8) -0.004(5) -0.027(5) 0.029(4) C43 0.066(6) 0.128(8) 0.124(11) 0.026(8) 0.050(6) 0.073(5) C44 0.128(8) 0.113(8) 0.011(5) 0.027(5) 0.027(5) 0.063(6) C45 0.055(6) 0.069(6) 0.054(7) 0.009(6) 0.011(5) 0.029(5) C46 0.045(4) 0.071(5) 0.048(6) 0.022(5) 0.033(4) 0.040(4) C47 0.150(9) 0.052(5) 0.075(9) 0.016(6) 0.026(7) 0.068(5) C48 0.056(4) 0.066(4) 0.063(7) 0.017(5) 0.004(5) 0.055(3) C49 0.070(6) 0.069(6) 0.039(6) 0.035(4) 0.010(5) 0.029(5) C50 0.047(4) 0.053(4) 0.042(6) 0.021(4) 0.006(4) 0.036(3) C51 0.043(5) 0.055(5) 0.024(5) 0.014(4) -0.004(4) 0.018(4) C52 0.026(4) 0.051(5) 0.055(6) 0.028(5) 0.018(4) 0.005(4) C53 0.038(5) 0.040(4) 0.090(7) 0.050(4) 0.022(5) 0.009(4) C54 0.072(6) 0.001(4) 0.047(6) -0.001(4) -0.017(5) -0.001(4) C55 0.051(4) 0.024(4) 0.036(5) 0.016(3) 0.006(4) 0.021(3) C56 0.030(4) 0.025(4) 0.034(5) 0.009(4) -0.005(4) 0.006(3) C57 0.049(4) 0.048(5) 0.062(7) 0.008(5) 0.024(4) 0.035(3) C58 0.076(6) 0.070(5) 0.041(7) -0.023(5) -0.032(5) 0.050(4) C59 0.031(4) 0.066(6) 0.040(6) 0.004(5) -0.003(4) 0.025(4) C60 0.037(4) 0.046(4) 0.050(6) 0.026(4) 0.008(4) 0.025(3) C61 0.092(8) 0.051(6) 0.042(7) -0.018(6) -0.011(6) 0.026(5) C62 0.111(10) 0.076(8) 0.066(8) 0.041(6) -0.003(8) 0.015(7) C63 0.245(16) 0.028(6) 0.112(14) -0.005(8) 0.039(13) 0.052(7) C64 0.266(7) 0.128(5) 0.070(10) -0.036(6) -0.045(7) 0.180(4) C65 0.111(8) 0.042(5) 0.037(7) 0.007(5) -0.007(6) 0.027(5) C66 0.105(6) 0.111(7) 0.009(5) 0.015(5) 0.019(4) 0.076(5) C67 0.167(6) 0.179(6) 0.056(8) 0.020(6) 0.002(6) 0.161(4) C68 0.115(7) 0.145(8) 0.096(10) 0.045(8) 0.062(6) 0.100(6) C69 0.048(6) 0.099(8) 0.061(7) 0.046(6) -0.008(6) 0.007(6) C70 0.029(4) 0.061(5) 0.021(4) 0.025(4) 0.013(3) 0.010(4) C71 0.055(5) 0.035(4) 0.052(6) 0.019(4) 0.009(5) 0.023(4) C72 0.057(6) 0.059(6) 0.079(7) 0.052(5) 0.025(5) 0.008(5) C73 0.055(5) 0.031(4) 0.063(7) 0.009(5) 0.001(5) 0.025(3) C74 0.054(5) 0.013(4) 0.023(5) -0.004(3) -0.021(4) 0.009(3) C75 0.070(5) 0.031(4) 0.034(6) 0.003(4) 0.005(5) 0.028(4) C76 0.132(8) 0.095(7) 0.059(8) 0.025(6) 0.008(7) 0.075(5) C77 0.083(7) 0.026(4) 0.102(9) 0.039(5) 0.006(7) 0.015(4) C78 0.075(6) 0.132(9) 0.173(12) 0.080(9) 0.085(6) 0.073(6) C79 0.131(13) 0.067(10) 0.21(2) 0.004(12) 0.065(13) 0.020(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.022(7) . ? U1 N4 2.545(8) . ? U1 N5 2.552(7) . ? U1 N6 2.556(7) . ? U1 N3 2.584(8) . ? U1 N1 2.601(6) . ? U1 N2 2.627(8) . ? U1 I1 2.9833(15) . ? U2 O2 2.070(8) . ? U2 O1 2.162(7) . ? U2 N9 2.557(9) . ? U2 N8 2.599(7) . ? U2 N7 2.651(8) . ? U2 I2 3.0669(16) . ? U2 I3 3.1193(12) . ? U3 O2 2.093(8) . ? U3 N13 2.545(8) . ? U3 N15 2.555(9) . ? U3 N14 2.567(9) . ? U3 N11 2.568(6) . ? U3 N12 2.568(7) . ? U3 N10 2.588(9) . ? U3 I4 3.0279(15) . ? I8A I8B 0.528(5) . ? I8C I8B 0.686(8) . ? N1 C1 1.315(15) . ? N1 C5 1.320(13) . ? N2 C6 1.316(9) . ? N2 C10 1.326(14) . ? N3 C11 1.341(12) . ? N3 C15 1.362(10) . ? N4 C16 1.229(11) . ? N4 C20 1.385(15) . ? N5 C21 1.359(12) . ? N5 C25 1.384(10) . ? N6 C30 1.357(14) . ? N6 C26 1.413(14) . ? N7 C35 1.272(10) . ? N7 C31 1.363(14) . ? N8 C36 1.298(13) . ? N8 C40 1.393(14) . ? N9 C45 1.279(15) . ? N9 C41 1.394(11) . ? N10 C46 1.332(14) . ? N10 C50 1.335(10) . ? N11 C51 1.324(12) . ? N11 C55 1.405(12) . ? N12 C56 1.338(9) . ? N12 C60 1.352(11) . ? N13 C61 1.237(13) . ? N13 C65 1.395(16) . ? N14 C66 1.326(15) . ? N14 C70 1.394(12) . ? N15 C75 1.421(14) . ? N15 C71 1.450(13) . ? N16 C76 1.491(18) . ? N17 C78 1.067(17) . ? C1 C2 1.383(12) . ? C2 C3 1.401(16) . ? C3 C4 1.389(17) . ? C4 C5 1.467(12) . ? C5 C6 1.436(15) . ? C6 C7 1.409(13) . ? C7 C8 1.394(16) . ? C8 C9 1.418(11) . ? C9 C10 1.389(15) . ? C10 C11 1.481(10) . ? C11 C12 1.368(14) . ? C12 C13 1.360(11) . ? C13 C14 1.401(16) . ? C14 C15 1.372(15) . ? C16 C17 1.421(18) . ? C17 C18 1.33(2) . ? C18 C19 1.383(14) . ? C19 C20 1.444(14) . ? C20 C21 1.449(11) . ? C21 C22 1.454(15) . ? C22 C23 1.327(14) . ? C23 C24 1.43(2) . ? C24 C25 1.400(15) . ? C25 C26 1.402(16) . ? C26 C27 1.411(15) . ? C27 C28 1.325(17) . ? C28 C29 1.409(16) . ? C29 C30 1.354(12) . ? C31 C32 1.353(16) . ? C32 C33 1.313(12) . ? C33 C34 1.422(17) . ? C34 C35 1.358(16) . ? C35 C36 1.530(16) . ? C36 C37 1.389(12) . ? C37 C38 1.336(15) . ? C38 C39 1.270(16) . ? C39 C40 1.403(13) . ? C40 C41 1.525(14) . ? C41 C42 1.458(15) . ? C42 C43 1.269(17) . ? C43 C44 1.328(17) . ? C44 C45 1.472(17) . ? C46 C47 1.365(18) . ? C47 C48 1.388(14) . ? C48 C49 1.468(15) . ? C49 C50 1.379(15) . ? C50 C51 1.507(14) . ? C51 C52 1.378(13) . ? C52 C53 1.483(15) . ? C53 C54 1.308(15) . ? C54 C55 1.428(11) . ? C55 C56 1.454(13) . ? C56 C57 1.345(13) . ? C57 C58 1.413(15) . ? C58 C59 1.346(12) . ? C59 C60 1.464(14) . ? C61 C62 1.345(18) . ? C62 C63 1.38(2) . ? C63 C64 1.451(18) . ? C64 C65 1.426(17) . ? C65 C66 1.427(16) . ? C66 C67 1.464(17) . ? C67 C68 1.349(19) . ? C68 C69 1.49(2) . ? C69 C70 1.326(15) . ? C70 C71 1.430(15) . ? C71 C72 1.300(15) . ? C72 C73 1.358(17) . ? C73 C74 1.378(14) . ? C74 C75 1.388(13) . ? C76 C77 1.092(15) . ? C78 C79 1.68(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 N4 88.2(3) . . ? O1 U1 N5 93.4(3) . . ? N4 U1 N5 65.2(2) . . ? O1 U1 N6 78.6(2) . . ? N4 U1 N6 124.7(3) . . ? N5 U1 N6 62.3(3) . . ? O1 U1 N3 158.0(2) . . ? N4 U1 N3 98.0(3) . . ? N5 U1 N3 70.5(3) . . ? N6 U1 N3 80.6(2) . . ? O1 U1 N1 81.3(3) . . ? N4 U1 N1 77.7(2) . . ? N5 U1 N1 142.7(2) . . ? N6 U1 N1 149.0(3) . . ? N3 U1 N1 120.6(3) . . ? O1 U1 N2 140.5(2) . . ? N4 U1 N2 70.7(3) . . ? N5 U1 N2 106.4(3) . . ? N6 U1 N2 140.9(2) . . ? N3 U1 N2 60.8(2) . . ? N1 U1 N2 62.2(3) . . ? O1 U1 I1 97.96(18) . . ? N4 U1 I1 150.76(17) . . ? N5 U1 I1 142.00(16) . . ? N6 U1 I1 84.58(19) . . ? N3 U1 I1 86.95(18) . . ? N1 U1 I1 75.11(19) . . ? N2 U1 I1 87.19(18) . . ? O2 U2 O1 173.6(3) . . ? O2 U2 N9 106.4(3) . . ? O1 U2 N9 78.6(3) . . ? O2 U2 N8 82.0(2) . . ? O1 U2 N8 96.7(2) . . ? N9 U2 N8 65.2(3) . . ? O2 U2 N7 88.0(3) . . ? O1 U2 N7 85.8(3) . . ? N9 U2 N7 122.0(2) . . ? N8 U2 N7 61.8(3) . . ? O2 U2 I2 88.71(16) . . ? O1 U2 I2 88.74(14) . . ? N9 U2 I2 149.53(19) . . ? N8 U2 I2 144.6(2) . . ? N7 U2 I2 83.95(15) . . ? O2 U2 I3 85.80(17) . . ? O1 U2 I3 99.58(16) . . ? N9 U2 I3 74.74(19) . . ? N8 U2 I3 132.4(2) . . ? N7 U2 I3 163.23(16) . . ? I2 U2 I3 80.34(5) . . ? O2 U3 N13 92.3(3) . . ? O2 U3 N15 153.9(3) . . ? N13 U3 N15 113.0(3) . . ? O2 U3 N14 144.6(3) . . ? N13 U3 N14 63.2(3) . . ? N15 U3 N14 59.2(3) . . ? O2 U3 N11 95.5(2) . . ? N13 U3 N11 131.7(3) . . ? N15 U3 N11 72.7(2) . . ? N14 U3 N11 84.7(2) . . ? O2 U3 N12 81.6(3) . . ? N13 U3 N12 165.0(2) . . ? N15 U3 N12 72.4(3) . . ? N14 U3 N12 128.0(3) . . ? N11 U3 N12 62.9(2) . . ? O2 U3 N10 78.5(3) . . ? N13 U3 N10 73.7(3) . . ? N15 U3 N10 113.5(3) . . ? N14 U3 N10 70.5(3) . . ? N11 U3 N10 61.6(2) . . ? N12 U3 N10 118.0(2) . . ? O2 U3 I4 96.16(16) . . ? N13 U3 I4 82.0(2) . . ? N15 U3 I4 82.00(17) . . ? N14 U3 I4 104.51(17) . . ? N11 U3 I4 143.64(19) . . ? N12 U3 I4 85.04(14) . . ? N10 U3 I4 154.75(16) . . ? U1 O1 U2 169.3(3) . . ? U2 O2 U3 173.2(3) . . ? C1 N1 C5 120.5(8) . . ? C1 N1 U1 118.6(6) . . ? C5 N1 U1 120.5(6) . . ? C6 N2 C10 121.7(8) . . ? C6 N2 U1 119.6(7) . . ? C10 N2 U1 117.7(5) . . ? C11 N3 C15 116.1(8) . . ? C11 N3 U1 119.1(5) . . ? C15 N3 U1 120.6(7) . . ? C16 N4 C20 116.9(9) . . ? C16 N4 U1 125.6(8) . . ? C20 N4 U1 116.3(5) . . ? C21 N5 C25 121.2(8) . . ? C21 N5 U1 115.4(5) . . ? C25 N5 U1 123.2(6) . . ? C30 N6 C26 115.8(8) . . ? C30 N6 U1 122.3(6) . . ? C26 N6 U1 121.2(6) . . ? C35 N7 C31 118.2(9) . . ? C35 N7 U2 119.7(7) . . ? C31 N7 U2 121.9(6) . . ? C36 N8 C40 120.0(8) . . ? C36 N8 U2 120.5(6) . . ? C40 N8 U2 116.3(6) . . ? C45 N9 C41 115.0(9) . . ? C45 N9 U2 127.1(7) . . ? C41 N9 U2 117.9(7) . . ? C46 N10 C50 115.5(8) . . ? C46 N10 U3 123.4(5) . . ? C50 N10 U3 119.5(7) . . ? C51 N11 C55 121.0(7) . . ? C51 N11 U3 118.5(5) . . ? C55 N11 U3 116.6(5) . . ? C56 N12 C60 123.7(8) . . ? C56 N12 U3 121.4(6) . . ? C60 N12 U3 114.9(5) . . ? C61 N13 C65 115.7(10) . . ? C61 N13 U3 125.1(8) . . ? C65 N13 U3 119.2(6) . . ? C66 N14 C70 123.0(9) . . ? C66 N14 U3 113.3(7) . . ? C70 N14 U3 115.8(6) . . ? C75 N15 C71 110.8(8) . . ? C75 N15 U3 125.1(7) . . ? C71 N15 U3 118.6(7) . . ? N1 C1 C2 125.9(10) . . ? C1 C2 C3 115.9(11) . . ? C4 C3 C2 119.5(8) . . ? C3 C4 C5 119.3(10) . . ? N1 C5 C6 118.5(8) . . ? N1 C5 C4 118.5(10) . . ? C6 C5 C4 123.0(9) . . ? N2 C6 C7 119.0(9) . . ? N2 C6 C5 118.4(8) . . ? C7 C6 C5 122.1(7) . . ? C8 C7 C6 120.2(7) . . ? C7 C8 C9 119.2(10) . . ? C10 C9 C8 115.7(10) . . ? N2 C10 C9 123.9(8) . . ? N2 C10 C11 118.0(9) . . ? C9 C10 C11 118.1(9) . . ? N3 C11 C12 122.5(7) . . ? N3 C11 C10 113.1(8) . . ? C12 C11 C10 123.7(9) . . ? C13 C12 C11 120.9(10) . . ? C12 C13 C14 118.6(10) . . ? C15 C14 C13 116.8(8) . . ? N3 C15 C14 124.7(9) . . ? N4 C16 C17 129.9(13) . . ? C18 C17 C16 114.0(10) . . ? C17 C18 C19 121.3(12) . . ? C18 C19 C20 118.6(11) . . ? N4 C20 C19 117.3(8) . . ? N4 C20 C21 115.7(9) . . ? C19 C20 C21 126.9(11) . . ? N5 C21 C20 120.7(9) . . ? N5 C21 C22 120.4(7) . . ? C20 C21 C22 118.9(9) . . ? C23 C22 C21 118.0(12) . . ? C22 C23 C24 121.7(11) . . ? C25 C24 C23 119.4(9) . . ? N5 C25 C24 118.7(10) . . ? N5 C25 C26 115.4(9) . . ? C24 C25 C26 125.9(9) . . ? C25 C26 C27 125.5(10) . . ? C25 C26 N6 116.7(9) . . ? C27 C26 N6 117.8(11) . . ? C28 C27 C26 124.6(11) . . ? C27 C28 C29 117.0(9) . . ? C30 C29 C28 118.7(11) . . ? C29 C30 N6 125.7(11) . . ? C32 C31 N7 121.6(8) . . ? C33 C32 C31 119.6(10) . . ? C32 C33 C34 119.7(11) . . ? C35 C34 C33 116.3(9) . . ? N7 C35 C34 124.4(11) . . ? N7 C35 C36 118.1(9) . . ? C34 C35 C36 117.3(8) . . ? N8 C36 C37 119.1(10) . . ? N8 C36 C35 114.3(8) . . ? C37 C36 C35 126.6(9) . . ? C38 C37 C36 120.9(10) . . ? C39 C38 C37 121.1(9) . . ? C38 C39 C40 120.5(11) . . ? N8 C40 C39 118.2(10) . . ? N8 C40 C41 114.6(8) . . ? C39 C40 C41 127.0(10) . . ? N9 C41 C42 119.9(9) . . ? N9 C41 C40 118.2(9) . . ? C42 C41 C40 121.7(7) . . ? C43 C42 C41 118.6(10) . . ? C42 C43 C44 126.2(14) . . ? C43 C44 C45 112.5(12) . . ? N9 C45 C44 127.2(10) . . ? N10 C46 C47 124.9(8) . . ? C46 C47 C48 119.0(11) . . ? C47 C48 C49 118.9(10) . . ? C50 C49 C48 113.5(8) . . ? N10 C50 C49 128.2(10) . . ? N10 C50 C51 114.5(9) . . ? C49 C50 C51 117.2(8) . . ? N11 C51 C52 121.3(10) . . ? N11 C51 C50 115.7(8) . . ? C52 C51 C50 122.8(9) . . ? C51 C52 C53 119.1(9) . . ? C54 C53 C52 117.0(8) . . ? C53 C54 C55 123.6(9) . . ? N11 C55 C54 117.2(9) . . ? N11 C55 C56 115.7(7) . . ? C54 C55 C56 127.0(9) . . ? N12 C56 C57 121.5(8) . . ? N12 C56 C55 116.1(8) . . ? C57 C56 C55 122.4(7) . . ? C56 C57 C58 120.0(8) . . ? C59 C58 C57 117.6(10) . . ? C58 C59 C60 122.7(9) . . ? N12 C60 C59 114.3(7) . . ? N13 C61 C62 128.1(13) . . ? C61 C62 C63 122.0(13) . . ? C62 C63 C64 114.2(13) . . ? C65 C64 C63 117.5(14) . . ? N13 C65 C66 112.8(10) . . ? N13 C65 C64 122.3(10) . . ? C66 C65 C64 124.9(12) . . ? N14 C66 C65 120.3(11) . . ? N14 C66 C67 120.0(10) . . ? C65 C66 C67 119.7(11) . . ? C68 C67 C66 118.0(12) . . ? C67 C68 C69 119.4(13) . . ? C70 C69 C68 120.0(12) . . ? C69 C70 N14 119.5(10) . . ? C69 C70 C71 124.2(10) . . ? N14 C70 C71 116.2(8) . . ? C72 C71 C70 127.2(11) . . ? C72 C71 N15 123.5(10) . . ? C70 C71 N15 109.3(8) . . ? C71 C72 C73 126.0(11) . . ? C72 C73 C74 114.0(9) . . ? C73 C74 C75 122.7(10) . . ? C74 C75 N15 122.7(9) . . ? C77 C76 N16 172.5(16) . . ? N17 C78 C79 166(2) . . ? #===END data_8.2py _database_code_depnum_ccdc_archive 'CCDC 251223' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H65 I8 N17 O2 U3' _chemical_formula_weight 3085.83 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' I I -0.4742 1.8119 '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 14.575(3) _cell_length_b 18.653(4) _cell_length_c 21.026(4) _cell_angle_alpha 66.26(3) _cell_angle_beta 88.75(3) _cell_angle_gamma 86.59(3) _cell_volume 5223.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 24436 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2820 _exptl_absorpt_coefficient_mu 7.051 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.272 _exptl_absorpt_correction_T_max 0.332 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24436 _diffrn_reflns_av_R_equivalents 0.152 _diffrn_reflns_av_sigmaI/netI 0.224 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.77 _reflns_number_total 15416 _reflns_number_gt 6718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all U and I atoms. Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. one iodure atom is found disordered on two positions (I5A and I5B) with 0.7 and 0.3 occupancy factors. ; _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^)+(0.1804P)^2^+44.0959P] 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 15366 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2500 _refine_ls_R_factor_gt 0.1249 _refine_ls_wR_factor_ref 0.3757 _refine_ls_wR_factor_gt 0.2972 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 3.182 _refine_diff_density_min -2.017 _refine_diff_density_rms 0.319 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 0.12947(11) 1.03373(8) 0.66371(9) 0.0599(5) Uani 1 1 d . . . U2 U 0.19983(10) 1.09872(8) 0.82197(8) 0.0543(5) Uani 1 1 d . . . U3 U 0.31937(10) 1.21211(8) 0.93048(8) 0.0536(5) Uani 1 1 d . . . I1 I -0.0464(2) 0.95597(18) 0.72403(18) 0.0803(10) Uani 1 1 d . . . I2 I 0.00263(18) 1.06249(15) 0.88112(16) 0.0693(9) Uani 1 1 d . . . I3 I 0.23288(18) 0.92744(14) 0.93097(15) 0.0620(8) Uani 1 1 d . . . I4 I 0.50756(18) 1.12892(16) 0.94934(17) 0.0700(8) Uani 1 1 d . . . I5A I 0.3216(4) 1.7828(3) 0.3921(3) 0.1031(17) Uani 0.70 1 d P . . I5B I 0.4465(9) 1.7745(6) 0.5022(7) 0.108(5) Uani 0.30 1 d P . . I6 I -0.1488(2) 1.51907(16) 0.56861(19) 0.0886(11) Uani 1 1 d . . . I7 I 0.3113(2) 1.13449(19) 1.31425(17) 0.0829(10) Uani 1 1 d . . . I8 I 0.81680(19) 1.42401(15) 1.01524(16) 0.0732(9) Uani 1 1 d . . . O1 O 0.2653(16) 1.1450(14) 0.8837(13) 0.056(7) Uiso 1 1 d . . . O2 O 0.1744(16) 1.0550(14) 0.7473(13) 0.055(6) Uiso 1 1 d . . . N1 N 0.036(3) 1.072(2) 0.547(2) 0.080(11) Uiso 1 1 d . . . N2 N 0.167(2) 0.9617(18) 0.5869(17) 0.059(8) Uiso 1 1 d . . . N3 N 0.186(2) 0.8871(18) 0.7217(17) 0.056(8) Uiso 1 1 d . . . N4 N 0.046(2) 1.1640(18) 0.6354(16) 0.056(8) Uiso 1 1 d . . . N5 N 0.197(2) 1.1504(19) 0.5695(17) 0.064(9) Uiso 1 1 d . . . N6 N 0.302(2) 1.0279(19) 0.6403(18) 0.066(9) Uiso 1 1 d . . . N7 N 0.112(2) 1.2404(19) 0.7741(17) 0.063(9) Uiso 1 1 d . . . N8 N 0.2677(19) 1.2067(17) 0.7109(15) 0.051(8) Uiso 1 1 d . . . N9 N 0.373(2) 1.082(2) 0.7912(18) 0.068(9) Uiso 1 1 d . . . N10 N 0.148(2) 1.2203(17) 0.9645(16) 0.055(8) Uiso 1 1 d . . . N11 N 0.226(2) 1.3397(17) 0.8664(16) 0.053(8) Uiso 1 1 d . . . N12 N 0.374(2) 1.300(2) 0.8043(18) 0.067(9) Uiso 1 1 d . . . N13 N 0.2925(18) 1.1007(16) 1.0442(15) 0.046(7) Uiso 1 1 d . . . N14 N 0.3076(17) 1.2477(15) 1.0383(13) 0.037(6) Uiso 1 1 d . . . N15 N 0.414(2) 1.3250(17) 0.9348(16) 0.054(8) Uiso 1 1 d . . . C1 C -0.044(3) 1.123(3) 0.542(3) 0.093(15) Uiso 1 1 d . . . H1 H -0.0808 1.1224 0.5788 0.111 Uiso 1 1 calc R . . C2 C -0.058(4) 1.176(3) 0.467(3) 0.104(17) Uiso 1 1 d . . . H2 H -0.1025 1.2168 0.4580 0.125 Uiso 1 1 calc R . . C3 C -0.010(3) 1.172(3) 0.408(3) 0.090(15) Uiso 1 1 d . . . H3 H -0.0206 1.2100 0.3635 0.108 Uiso 1 1 calc R . . C4 C 0.053(4) 1.108(3) 0.422(3) 0.099(16) Uiso 1 1 d . . . H4 H 0.0775 1.0938 0.3870 0.119 Uiso 1 1 calc R . . C5 C 0.077(3) 1.066(2) 0.493(2) 0.063(11) Uiso 1 1 d . . . C6 C 0.151(3) 1.003(3) 0.519(3) 0.083(14) Uiso 1 1 d . . . C7 C 0.200(3) 0.980(3) 0.471(3) 0.085(14) Uiso 1 1 d . . . H7 H 0.1836 1.0033 0.4240 0.102 Uiso 1 1 calc R . . C8 C 0.276(4) 0.921(3) 0.494(3) 0.102(17) Uiso 1 1 d . . . H8 H 0.3196 0.9143 0.4631 0.122 Uiso 1 1 calc R . . C9 C 0.278(3) 0.874(3) 0.564(3) 0.085(14) Uiso 1 1 d . . . H9 H 0.3155 0.8286 0.5813 0.102 Uiso 1 1 calc R . . C10 C 0.223(3) 0.897(2) 0.608(2) 0.067(11) Uiso 1 1 d . . . C11 C 0.220(3) 0.850(2) 0.682(2) 0.058(10) Uiso 1 1 d . . . C12 C 0.252(3) 0.774(3) 0.715(3) 0.086(14) Uiso 1 1 d . . . H12 H 0.2727 0.7475 0.6876 0.104 Uiso 1 1 calc R . . C13 C 0.255(3) 0.732(2) 0.788(2) 0.056(10) Uiso 1 1 d . . . H13 H 0.2808 0.6809 0.8091 0.068 Uiso 1 1 calc R . . C14 C 0.217(2) 0.770(2) 0.825(2) 0.052(9) Uiso 1 1 d . . . H14 H 0.2112 0.7454 0.8732 0.063 Uiso 1 1 calc R . . C15 C 0.184(2) 0.851(2) 0.788(2) 0.055(10) Uiso 1 1 d . . . H15 H 0.1617 0.8787 0.8142 0.065 Uiso 1 1 calc R . . C16 C -0.014(3) 1.170(3) 0.680(3) 0.096(16) Uiso 1 1 d . . . H16 H -0.0193 1.1276 0.7225 0.115 Uiso 1 1 calc R . . C17 C -0.078(3) 1.246(3) 0.666(3) 0.083(14) Uiso 1 1 d . . . H17 H -0.1291 1.2480 0.6927 0.100 Uiso 1 1 calc R . . C18 C -0.052(3) 1.307(3) 0.611(2) 0.073(12) Uiso 1 1 d . . . H18 H -0.0772 1.3569 0.6020 0.087 Uiso 1 1 calc R . . C19 C 0.014(3) 1.296(3) 0.567(3) 0.093(15) Uiso 1 1 d . . . H19 H 0.0219 1.3386 0.5251 0.111 Uiso 1 1 calc R . . C20 C 0.069(3) 1.230(3) 0.580(2) 0.068(12) Uiso 1 1 d . . . C21 C 0.135(3) 1.218(3) 0.539(2) 0.074(12) Uiso 1 1 d . . . C22 C 0.153(3) 1.266(3) 0.470(3) 0.081(13) Uiso 1 1 d . . . H22 H 0.1116 1.3077 0.4466 0.097 Uiso 1 1 calc R . . C23 C 0.225(3) 1.254(3) 0.439(2) 0.076(13) Uiso 1 1 d . . . H23 H 0.2363 1.2918 0.3944 0.091 Uiso 1 1 calc R . . C24 C 0.288(3) 1.192(3) 0.465(2) 0.082(14) Uiso 1 1 d . . . H24 H 0.3378 1.1852 0.4389 0.098 Uiso 1 1 calc R . . C25 C 0.271(3) 1.134(2) 0.537(2) 0.066(11) Uiso 1 1 d . . . C26 C 0.337(3) 1.075(3) 0.572(2) 0.073(12) Uiso 1 1 d . . . C27 C 0.424(3) 1.060(3) 0.555(2) 0.070(12) Uiso 1 1 d . . . H27 H 0.4467 1.0945 0.5129 0.084 Uiso 1 1 calc R . . C28 C 0.477(3) 1.002(2) 0.592(2) 0.072(12) Uiso 1 1 d . . . H28 H 0.5323 0.9906 0.5740 0.086 Uiso 1 1 calc R . . C29 C 0.451(3) 0.954(3) 0.662(2) 0.073(12) Uiso 1 1 d . . . H29 H 0.4897 0.9144 0.6929 0.088 Uiso 1 1 calc R . . C30 C 0.362(3) 0.974(2) 0.680(2) 0.061(11) Uiso 1 1 d . . . H30 H 0.3431 0.9455 0.7251 0.073 Uiso 1 1 calc R . . C31 C 0.050(3) 1.257(3) 0.809(2) 0.069(12) Uiso 1 1 d . . . H31 H 0.0338 1.2187 0.8517 0.083 Uiso 1 1 calc R . . C32 C 0.002(3) 1.333(2) 0.787(2) 0.072(12) Uiso 1 1 d . . . H32 H -0.0462 1.3413 0.8133 0.087 Uiso 1 1 calc R . . C33 C 0.025(4) 1.390(3) 0.731(3) 0.102(17) Uiso 1 1 d . . . H33 H -0.0045 1.4390 0.7169 0.122 Uiso 1 1 calc R . . C34 C 0.098(3) 1.375(3) 0.690(3) 0.094(16) Uiso 1 1 d . . . H34 H 0.1140 1.4154 0.6482 0.113 Uiso 1 1 calc R . . C35 C 0.150(3) 1.294(2) 0.713(2) 0.070(12) Uiso 1 1 d . . . C36 C 0.226(3) 1.272(2) 0.677(2) 0.058(10) Uiso 1 1 d . . . C37 C 0.241(3) 1.320(3) 0.610(2) 0.072(12) Uiso 1 1 d . . . H37 H 0.2024 1.3635 0.5847 0.087 Uiso 1 1 calc R . . C38 C 0.315(4) 1.300(3) 0.583(3) 0.097(16) Uiso 1 1 d . . . H38 H 0.3338 1.3345 0.5388 0.117 Uiso 1 1 calc R . . C39 C 0.364(3) 1.233(2) 0.615(2) 0.062(11) Uiso 1 1 d . . . H39 H 0.4116 1.2188 0.5920 0.074 Uiso 1 1 calc R . . C40 C 0.344(3) 1.187(3) 0.680(2) 0.076(13) Uiso 1 1 d . . . C41 C 0.403(3) 1.115(3) 0.728(2) 0.072(12) Uiso 1 1 d . . . C42 C 0.485(3) 1.098(3) 0.706(3) 0.093(15) Uiso 1 1 d . . . H42 H 0.5017 1.1242 0.6597 0.111 Uiso 1 1 calc R . . C43 C 0.547(3) 1.041(2) 0.753(2) 0.067(11) Uiso 1 1 d . . . H43 H 0.6057 1.0280 0.7423 0.080 Uiso 1 1 calc R . . C44 C 0.505(3) 1.006(2) 0.821(2) 0.065(11) Uiso 1 1 d . . . H44 H 0.5381 0.9651 0.8547 0.078 Uiso 1 1 calc R . . C45 C 0.429(2) 1.0265(19) 0.8374(19) 0.043(8) Uiso 1 1 d . . . H45 H 0.4098 1.0025 0.8833 0.052 Uiso 1 1 calc R . . C46 C 0.100(2) 1.1612(19) 1.0009(17) 0.040(8) Uiso 1 1 d . . . H46 H 0.1250 1.1108 1.0112 0.048 Uiso 1 1 calc R . . C47 C 0.015(3) 1.169(3) 1.024(2) 0.068(12) Uiso 1 1 d . . . H47 H -0.0170 1.1246 1.0469 0.082 Uiso 1 1 calc R . . C48 C -0.026(3) 1.241(2) 1.017(2) 0.060(11) Uiso 1 1 d . . . H48 H -0.0836 1.2463 1.0350 0.072 Uiso 1 1 calc R . . C49 C 0.029(3) 1.305(3) 0.979(2) 0.075(13) Uiso 1 1 d . . . H49 H 0.0062 1.3546 0.9733 0.090 Uiso 1 1 calc R . . C50 C 0.112(3) 1.298(2) 0.951(2) 0.067(11) Uiso 1 1 d . . . C51 C 0.164(3) 1.359(2) 0.905(2) 0.067(11) Uiso 1 1 d . . . C52 C 0.142(3) 1.441(2) 0.893(2) 0.066(11) Uiso 1 1 d . . . H52 H 0.1014 1.4541 0.9220 0.079 Uiso 1 1 calc R . . C53 C 0.183(3) 1.496(3) 0.841(2) 0.077(13) Uiso 1 1 d . . . H53 H 0.1704 1.5484 0.8317 0.092 Uiso 1 1 calc R . . C54 C 0.243(2) 1.477(2) 0.8006(19) 0.050(9) Uiso 1 1 d . . . H54 H 0.2672 1.5163 0.7621 0.060 Uiso 1 1 calc R . . C55 C 0.269(2) 1.400(2) 0.8145(19) 0.047(9) Uiso 1 1 d . . . C56 C 0.346(2) 1.374(2) 0.7764(19) 0.049(9) Uiso 1 1 d . . . C57 C 0.370(3) 1.423(2) 0.711(2) 0.058(10) Uiso 1 1 d . . . H57 H 0.3447 1.4744 0.6913 0.069 Uiso 1 1 calc R . . C58 C 0.431(4) 1.397(3) 0.673(3) 0.100(16) Uiso 1 1 d . . . H58 H 0.4478 1.4273 0.6275 0.120 Uiso 1 1 calc R . . C59 C 0.469(3) 1.317(3) 0.710(2) 0.078(13) Uiso 1 1 d . . . H59 H 0.5188 1.2976 0.6922 0.094 Uiso 1 1 calc R . . C60 C 0.432(3) 1.272(2) 0.768(2) 0.057(10) Uiso 1 1 d . . . H60 H 0.4462 1.2181 0.7848 0.068 Uiso 1 1 calc R . . C61 C 0.297(2) 1.0266(19) 1.0503(18) 0.045(9) Uiso 1 1 d . . . H61 H 0.3218 1.0150 1.0144 0.054 Uiso 1 1 calc R . . C62 C 0.262(2) 0.963(2) 1.1120(18) 0.048(9) Uiso 1 1 d . . . H62 H 0.2578 0.9127 1.1140 0.058 Uiso 1 1 calc R . . C63 C 0.239(2) 0.981(2) 1.163(2) 0.054(10) Uiso 1 1 d . . . H63 H 0.2194 0.9409 1.2033 0.065 Uiso 1 1 calc R . . C64 C 0.242(3) 1.054(2) 1.164(2) 0.060(10) Uiso 1 1 d . . . H64 H 0.2259 1.0634 1.2029 0.072 Uiso 1 1 calc R . . C65 C 0.269(2) 1.114(2) 1.102(2) 0.055(10) Uiso 1 1 d . . . C66 C 0.266(2) 1.200(2) 1.0934(19) 0.049(9) Uiso 1 1 d . . . C67 C 0.224(2) 1.227(2) 1.1394(19) 0.046(9) Uiso 1 1 d . . . H67 H 0.1946 1.1936 1.1788 0.056 Uiso 1 1 calc R . . C68 C 0.229(3) 1.300(2) 1.126(2) 0.067(11) Uiso 1 1 d . . . H68 H 0.1968 1.3206 1.1542 0.080 Uiso 1 1 calc R . . C69 C 0.276(3) 1.348(3) 1.074(2) 0.069(12) Uiso 1 1 d . . . H69 H 0.2832 1.3987 1.0705 0.083 Uiso 1 1 calc R . . C70 C 0.316(2) 1.326(2) 1.0242(19) 0.048(9) Uiso 1 1 d . . . C71 C 0.378(2) 1.364(2) 0.970(2) 0.054(10) Uiso 1 1 d . . . C72 C 0.409(3) 1.441(3) 0.954(2) 0.077(13) Uiso 1 1 d . . . H72 H 0.3815 1.4704 0.9765 0.092 Uiso 1 1 calc R . . C73 C 0.472(3) 1.473(2) 0.909(2) 0.064(11) Uiso 1 1 d . . . H73 H 0.4896 1.5235 0.8983 0.077 Uiso 1 1 calc R . . C74 C 0.510(3) 1.429(3) 0.879(2) 0.076(13) Uiso 1 1 d . . . H74 H 0.5611 1.4459 0.8506 0.091 Uiso 1 1 calc R . . C75 C 0.477(3) 1.362(3) 0.891(2) 0.077(13) Uiso 1 1 d . . . H75 H 0.5011 1.3364 0.8636 0.092 Uiso 1 1 calc R . . N16 N 0.2274(11) 0.6489(8) 0.6404(8) 0.069(9) Uiso 1 1 d G . . C76 C 0.2636(12) 0.6272(12) 0.5888(10) 0.093(15) Uiso 1 1 d G . . H76 H 0.3243 0.6367 0.5748 0.112 Uiso 1 1 calc R . . C77 C 0.2093(14) 0.5912(13) 0.5581(11) 0.079(13) Uiso 1 1 d G . . H77 H 0.2336 0.5767 0.5235 0.095 Uiso 1 1 calc R . . C78 C 0.1188(15) 0.5771(11) 0.5790(11) 0.070(12) Uiso 1 1 d G . . H78 H 0.0824 0.5530 0.5584 0.083 Uiso 1 1 calc R . . C79 C 0.0826(14) 0.5988(13) 0.6307(11) 0.083(14) Uiso 1 1 d G . . H79 H 0.0219 0.5893 0.6447 0.100 Uiso 1 1 calc R . . C80 C 0.1369(11) 0.6348(11) 0.6614(10) 0.066(11) Uiso 1 1 d G . . H80 H 0.1127 0.6493 0.6960 0.080 Uiso 1 1 calc R . . N17 N 0.4839(12) 0.6664(9) 0.8828(9) 0.060(9) Uiso 1 1 d G . . C81 C 0.4245(13) 0.6722(11) 0.9230(8) 0.068(12) Uiso 1 1 d G . . H81 H 0.3895 0.6291 0.9457 0.082 Uiso 1 1 calc R . . C82 C 0.4060(12) 0.7369(14) 0.9371(10) 0.082(14) Uiso 1 1 d G . . H82 H 0.3674 0.7353 0.9734 0.099 Uiso 1 1 calc R . . C83 C 0.4461(13) 0.8035(12) 0.8959(11) 0.086(14) Uiso 1 1 d G . . H83 H 0.4287 0.8507 0.8992 0.104 Uiso 1 1 calc R . . C84 C 0.5080(14) 0.8017(11) 0.8525(9) 0.046(9) Uiso 1 1 d G . . H84 H 0.5415 0.8453 0.8279 0.055 Uiso 1 1 calc R . . C85 C 0.5235(10) 0.7309(11) 0.8434(9) 0.059(10) Uiso 1 1 d G . . H85 H 0.5630 0.7300 0.8084 0.070 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 0.0680(11) 0.0382(8) 0.0624(11) -0.0085(7) -0.0065(8) -0.0018(7) U2 0.0587(9) 0.0340(8) 0.0587(10) -0.0065(7) -0.0021(7) -0.0020(6) U3 0.0550(9) 0.0356(8) 0.0605(11) -0.0097(7) 0.0028(7) 0.0001(6) I1 0.068(2) 0.0680(19) 0.102(3) -0.0308(18) 0.0092(16) -0.0130(14) I2 0.0593(17) 0.0472(15) 0.088(2) -0.0127(14) 0.0058(14) -0.0053(12) I3 0.0587(16) 0.0382(13) 0.0692(19) -0.0007(12) 0.0005(13) -0.0046(11) I4 0.0568(17) 0.0543(16) 0.095(2) -0.0272(15) 0.0009(14) 0.0044(12) I5A 0.104(4) 0.077(3) 0.127(5) -0.040(3) 0.033(3) -0.026(3) I5B 0.119(10) 0.054(6) 0.139(11) -0.029(7) 0.061(8) -0.027(6) I6 0.099(2) 0.0453(16) 0.098(3) -0.0040(16) -0.0185(19) 0.0058(15) I7 0.072(2) 0.091(2) 0.076(2) -0.0235(18) 0.0072(16) -0.0110(16) I8 0.0705(18) 0.0425(15) 0.085(2) -0.0051(14) 0.0099(15) 0.0039(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.08(3) . ? U1 N4 2.50(3) . ? U1 N5 2.51(3) . ? U1 N2 2.52(3) . ? U1 N6 2.56(3) . ? U1 N3 2.59(3) . ? U1 N1 2.65(4) . ? U1 I1 3.016(3) . ? U2 O2 2.09(3) . ? U2 O1 2.10(3) . ? U2 N8 2.61(3) . ? U2 N9 2.62(3) . ? U2 N7 2.67(3) . ? U2 I3 3.108(3) . ? U2 I2 3.109(3) . ? U3 O1 2.07(3) . ? U3 N13 2.50(3) . ? U3 N11 2.54(3) . ? U3 N10 2.60(3) . ? U3 N14 2.61(3) . ? U3 N15 2.62(3) . ? U3 N12 2.63(3) . ? U3 I4 3.022(3) . ? N1 C5 1.30(5) . ? N1 C1 1.44(6) . ? N2 C6 1.33(5) . ? N2 C10 1.34(5) . ? N3 C15 1.29(4) . ? N3 C11 1.35(5) . ? N4 C16 1.30(5) . ? N4 C20 1.37(5) . ? N5 C25 1.36(5) . ? N5 C21 1.43(5) . ? N6 C30 1.30(5) . ? N6 C26 1.45(5) . ? N7 C31 1.26(5) . ? N7 C35 1.40(5) . ? N8 C36 1.27(4) . ? N8 C40 1.39(5) . ? N9 C41 1.30(5) . ? N9 C45 1.34(4) . ? N10 C46 1.30(4) . ? N10 C50 1.42(5) . ? N11 C51 1.33(5) . ? N11 C55 1.38(4) . ? N12 C56 1.31(4) . ? N12 C60 1.35(5) . ? N13 C61 1.33(4) . ? N13 C65 1.37(5) . ? N14 C66 1.31(4) . ? N14 C70 1.38(4) . ? N15 C75 1.30(5) . ? N15 C71 1.32(4) . ? C1 C2 1.49(7) . ? C2 C3 1.44(7) . ? C3 C4 1.40(6) . ? C4 C5 1.43(6) . ? C5 C6 1.48(6) . ? C6 C7 1.42(6) . ? C7 C8 1.46(6) . ? C8 C9 1.38(6) . ? C9 C10 1.39(6) . ? C10 C11 1.45(5) . ? C11 C12 1.36(5) . ? C12 C13 1.42(6) . ? C13 C14 1.35(5) . ? C14 C15 1.44(5) . ? C16 C17 1.58(6) . ? C17 C18 1.32(6) . ? C18 C19 1.37(6) . ? C19 C20 1.37(6) . ? C20 C21 1.36(6) . ? C21 C22 1.38(6) . ? C22 C23 1.29(6) . ? C23 C24 1.37(6) . ? C24 C25 1.49(6) . ? C25 C26 1.39(6) . ? C26 C27 1.35(5) . ? C27 C28 1.28(5) . ? C28 C29 1.43(6) . ? C29 C30 1.42(5) . ? C31 C32 1.44(5) . ? C32 C33 1.28(6) . ? C33 C34 1.43(7) . ? C34 C35 1.54(6) . ? C35 C36 1.45(5) . ? C36 C37 1.36(5) . ? C37 C38 1.31(6) . ? C38 C39 1.33(6) . ? C39 C40 1.32(5) . ? C40 C41 1.53(6) . ? C41 C42 1.34(6) . ? C42 C43 1.42(6) . ? C43 C44 1.44(5) . ? C44 C45 1.24(5) . ? C46 C47 1.34(5) . ? C47 C48 1.38(5) . ? C48 C49 1.42(5) . ? C49 C50 1.36(6) . ? C50 C51 1.42(5) . ? C51 C52 1.46(5) . ? C52 C53 1.33(5) . ? C53 C54 1.33(5) . ? C54 C55 1.38(5) . ? C55 C56 1.52(5) . ? C56 C57 1.37(5) . ? C57 C58 1.39(6) . ? C58 C59 1.45(6) . ? C59 C60 1.29(5) . ? C61 C62 1.46(5) . ? C62 C63 1.28(5) . ? C63 C64 1.37(5) . ? C64 C65 1.39(5) . ? C65 C66 1.54(5) . ? C66 C67 1.37(5) . ? C67 C68 1.28(5) . ? C68 C69 1.31(5) . ? C69 C70 1.38(5) . ? C70 C71 1.40(5) . ? C71 C72 1.44(5) . ? C72 C73 1.29(5) . ? C73 C74 1.30(5) . ? C74 C75 1.31(6) . ? N16 C80 1.388(4) . ? N16 C76 1.388(4) . ? C76 C77 1.388(4) . ? C77 C78 1.388(4) . ? C78 C79 1.388(4) . ? C79 C80 1.388(4) . ? N17 C81 1.227(4) . ? N17 C85 1.314(4) . ? C81 C82 1.365(4) . ? C82 C83 1.355(4) . ? C83 C84 1.277(4) . ? C84 C85 1.414(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 N4 81.6(10) . . ? O2 U1 N5 97.0(10) . . ? N4 U1 N5 63.2(10) . . ? O2 U1 N2 144.7(10) . . ? N4 U1 N2 129.6(10) . . ? N5 U1 N2 86.4(11) . . ? O2 U1 N6 82.1(10) . . ? N4 U1 N6 119.3(10) . . ? N5 U1 N6 61.6(10) . . ? N2 U1 N6 68.6(10) . . ? O2 U1 N3 92.0(10) . . ? N4 U1 N3 164.3(10) . . ? N5 U1 N3 132.2(10) . . ? N2 U1 N3 61.6(10) . . ? N6 U1 N3 73.5(10) . . ? O2 U1 N1 153.1(10) . . ? N4 U1 N1 71.5(11) . . ? N5 U1 N1 70.3(11) . . ? N2 U1 N1 60.4(11) . . ? N6 U1 N1 110.0(11) . . ? N3 U1 N1 114.2(11) . . ? O2 U1 I1 99.6(6) . . ? N4 U1 I1 88.8(7) . . ? N5 U1 I1 144.7(7) . . ? N2 U1 I1 97.4(7) . . ? N6 U1 I1 151.6(7) . . ? N3 U1 I1 78.1(7) . . ? N1 U1 I1 81.1(8) . . ? O2 U2 O1 162.5(9) . . ? O2 U2 N8 79.0(9) . . ? O1 U2 N8 89.6(9) . . ? O2 U2 N9 84.2(10) . . ? O1 U2 N9 78.7(10) . . ? N8 U2 N9 61.4(10) . . ? O2 U2 N7 104.4(10) . . ? O1 U2 N7 81.7(10) . . ? N8 U2 N7 63.2(9) . . ? N9 U2 N7 120.8(10) . . ? O2 U2 I3 89.0(6) . . ? O1 U2 I3 92.6(6) . . ? N8 U2 I3 143.7(6) . . ? N9 U2 I3 83.6(7) . . ? N7 U2 I3 152.8(7) . . ? O2 U2 I2 90.7(6) . . ? O1 U2 I2 106.7(7) . . ? N8 U2 I2 134.3(6) . . ? N9 U2 I2 162.2(7) . . ? N7 U2 I2 77.0(7) . . ? I3 U2 I2 79.28(8) . . ? O1 U3 N13 87.0(10) . . ? O1 U3 N11 98.8(10) . . ? N13 U3 N11 131.1(9) . . ? O1 U3 N10 80.7(10) . . ? N13 U3 N10 71.3(9) . . ? N11 U3 N10 62.1(9) . . ? O1 U3 N14 144.3(9) . . ? N13 U3 N14 64.3(9) . . ? N11 U3 N14 86.3(9) . . ? N10 U3 N14 70.6(9) . . ? O1 U3 N15 155.1(10) . . ? N13 U3 N15 116.3(9) . . ? N11 U3 N15 73.0(9) . . ? N10 U3 N15 113.7(10) . . ? N14 U3 N15 60.0(9) . . ? O1 U3 N12 84.5(10) . . ? N13 U3 N12 164.5(10) . . ? N11 U3 N12 63.3(10) . . ? N10 U3 N12 119.9(10) . . ? N14 U3 N12 128.0(9) . . ? N15 U3 N12 70.8(10) . . ? O1 U3 I4 93.6(7) . . ? N13 U3 I4 81.5(6) . . ? N11 U3 I4 145.3(7) . . ? N10 U3 I4 152.4(7) . . ? N14 U3 I4 102.1(5) . . ? N15 U3 I4 82.2(6) . . ? N12 U3 I4 86.0(7) . . ? U3 O1 U2 168.5(13) . . ? U1 O2 U2 167.2(13) . . ? C5 N1 C1 124(4) . . ? C5 N1 U1 120(3) . . ? C1 N1 U1 113(3) . . ? C6 N2 C10 120(4) . . ? C6 N2 U1 115(3) . . ? C10 N2 U1 122(3) . . ? C15 N3 C11 120(3) . . ? C15 N3 U1 120(3) . . ? C11 N3 U1 120(2) . . ? C16 N4 C20 119(4) . . ? C16 N4 U1 118(3) . . ? C20 N4 U1 122(3) . . ? C25 N5 C21 124(4) . . ? C25 N5 U1 115(3) . . ? C21 N5 U1 116(3) . . ? C30 N6 C26 114(4) . . ? C30 N6 U1 125(3) . . ? C26 N6 U1 119(3) . . ? C31 N7 C35 125(4) . . ? C31 N7 U2 121(3) . . ? C35 N7 U2 114(3) . . ? C36 N8 C40 117(3) . . ? C36 N8 U2 123(2) . . ? C40 N8 U2 119(2) . . ? C41 N9 C45 117(4) . . ? C41 N9 U2 121(3) . . ? C45 N9 U2 120(3) . . ? C46 N10 C50 119(3) . . ? C46 N10 U3 126(2) . . ? C50 N10 U3 114(2) . . ? C51 N11 C55 117(3) . . ? C51 N11 U3 115(2) . . ? C55 N11 U3 118(2) . . ? C56 N12 C60 119(3) . . ? C56 N12 U3 119(3) . . ? C60 N12 U3 123(3) . . ? C61 N13 C65 117(3) . . ? C61 N13 U3 122(2) . . ? C65 N13 U3 121(2) . . ? C66 N14 C70 123(3) . . ? C66 N14 U3 118(2) . . ? C70 N14 U3 115(2) . . ? C75 N15 C71 114(4) . . ? C75 N15 U3 126(3) . . ? C71 N15 U3 116(2) . . ? N1 C1 C2 108(4) . . ? C3 C2 C1 128(5) . . ? C4 C3 C2 116(5) . . ? C5 C4 C3 115(5) . . ? N1 C5 C4 127(4) . . ? N1 C5 C6 108(4) . . ? C4 C5 C6 125(4) . . ? N2 C6 C7 118(4) . . ? N2 C6 C5 123(4) . . ? C7 C6 C5 118(4) . . ? C6 C7 C8 120(5) . . ? C9 C8 C7 115(5) . . ? C8 C9 C10 119(5) . . ? N2 C10 C9 124(4) . . ? N2 C10 C11 114(4) . . ? C9 C10 C11 122(4) . . ? N3 C11 C12 118(4) . . ? N3 C11 C10 116(4) . . ? C12 C11 C10 126(4) . . ? C11 C12 C13 124(5) . . ? C14 C13 C12 115(4) . . ? C13 C14 C15 118(4) . . ? N3 C15 C14 123(4) . . ? N4 C16 C17 123(5) . . ? C18 C17 C16 112(5) . . ? C17 C18 C19 120(5) . . ? C18 C19 C20 126(5) . . ? C21 C20 N4 115(4) . . ? C21 C20 C19 128(5) . . ? N4 C20 C19 117(4) . . ? C20 C21 C22 127(4) . . ? C20 C21 N5 117(4) . . ? C22 C21 N5 116(4) . . ? C23 C22 C21 122(5) . . ? C22 C23 C24 126(5) . . ? C23 C24 C25 116(4) . . ? N5 C25 C26 122(4) . . ? N5 C25 C24 116(4) . . ? C26 C25 C24 121(4) . . ? C27 C26 C25 132(4) . . ? C27 C26 N6 119(4) . . ? C25 C26 N6 109(4) . . ? C28 C27 C26 126(5) . . ? C27 C28 C29 119(4) . . ? C30 C29 C28 114(4) . . ? N6 C30 C29 128(4) . . ? N7 C31 C32 124(4) . . ? C33 C32 C31 120(5) . . ? C32 C33 C34 119(5) . . ? C33 C34 C35 121(5) . . ? N7 C35 C36 122(4) . . ? N7 C35 C34 111(4) . . ? C36 C35 C34 127(4) . . ? N8 C36 C37 125(4) . . ? N8 C36 C35 116(4) . . ? C37 C36 C35 118(4) . . ? C38 C37 C36 115(5) . . ? C37 C38 C39 122(5) . . ? C40 C39 C38 121(5) . . ? C39 C40 N8 118(4) . . ? C39 C40 C41 127(4) . . ? N8 C40 C41 115(4) . . ? N9 C41 C42 124(5) . . ? N9 C41 C40 116(4) . . ? C42 C41 C40 119(4) . . ? C41 C42 C43 120(5) . . ? C42 C43 C44 110(4) . . ? C45 C44 C43 126(4) . . ? C44 C45 N9 122(4) . . ? N10 C46 C47 123(3) . . ? C46 C47 C48 124(4) . . ? C47 C48 C49 113(4) . . ? C50 C49 C48 124(4) . . ? C49 C50 N10 117(4) . . ? C49 C50 C51 127(4) . . ? N10 C50 C51 116(4) . . ? N11 C51 C50 116(4) . . ? N11 C51 C52 122(4) . . ? C50 C51 C52 122(4) . . ? C53 C52 C51 117(4) . . ? C54 C53 C52 121(5) . . ? C53 C54 C55 122(4) . . ? N11 C55 C54 120(3) . . ? N11 C55 C56 115(3) . . ? C54 C55 C56 124(3) . . ? N12 C56 C57 122(4) . . ? N12 C56 C55 117(3) . . ? C57 C56 C55 120(3) . . ? C56 C57 C58 120(4) . . ? C57 C58 C59 115(5) . . ? C60 C59 C58 120(5) . . ? C59 C60 N12 123(4) . . ? N13 C61 C62 122(3) . . ? C63 C62 C61 116(4) . . ? C62 C63 C64 126(4) . . ? C63 C64 C65 116(4) . . ? N13 C65 C64 122(4) . . ? N13 C65 C66 116(3) . . ? C64 C65 C66 122(4) . . ? N14 C66 C67 121(3) . . ? N14 C66 C65 115(3) . . ? C67 C66 C65 124(3) . . ? C68 C67 C66 117(4) . . ? C67 C68 C69 123(4) . . ? C68 C69 C70 122(4) . . ? N14 C70 C69 113(3) . . ? N14 C70 C71 115(3) . . ? C69 C70 C71 131(4) . . ? N15 C71 C70 118(3) . . ? N15 C71 C72 117(4) . . ? C70 C71 C72 125(4) . . ? C73 C72 C71 125(5) . . ? C72 C73 C74 116(5) . . ? C73 C74 C75 119(5) . . ? N15 C75 C74 129(5) . . ? C80 N16 C76 120.0 . . ? C77 C76 N16 120.0 . . ? C76 C77 C78 120.0 . . ? C79 C78 C77 120.0 . . ? C78 C79 C80 120.0 . . ? N16 C80 C79 120.0 . . ? C81 N17 C85 116.9 . . ? N17 C81 C82 125.2 . . ? C83 C82 C81 117.1 . . ? C84 C83 C82 120.1 . . ? C83 C84 C85 117.5 . . ? N17 C85 C84 122.1 . . ? #===END data_9.py.MeCN _database_code_depnum_ccdc_archive 'CCDC 251224' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H74 F30 N20 O33 S10 U4' _chemical_formula_weight 4010.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.987(4) _cell_length_b 22.810(5) _cell_length_c 28.435(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.70(3) _cell_angle_gamma 90.00 _cell_volume 13545(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 64014 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7672 _exptl_absorpt_coefficient_mu 5.044 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.621 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 1998)' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 12 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f scans with 2\% steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64014 _diffrn_reflns_av_R_equivalents 0.1750 _diffrn_reflns_av_sigmaI/netI 0.2445 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 24.74 _reflns_number_total 21020 _reflns_number_gt 9247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for U,S,F and O atoms.Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH)or 1.5 (CH~3~) times that of the parent atom. ; _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^)+(0.0667P)^2^+433.9644P] 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 21020 _refine_ls_number_parameters 1220 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.2520 _refine_ls_R_factor_gt 0.1094 _refine_ls_wR_factor_ref 0.2562 _refine_ls_wR_factor_gt 0.1939 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.902 _refine_diff_density_min -1.440 _refine_diff_density_rms 0.237 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 0.17931(5) 1.11056(4) 0.91151(4) 0.0407(3) Uani 1 1 d . . . U2 U 0.19520(5) 1.04929(4) 0.77383(3) 0.0403(3) Uani 1 1 d . . . U3 U 0.21652(5) 0.95296(4) 0.65377(3) 0.0395(3) Uani 1 1 d . . . U4 U 0.26599(5) 0.87665(4) 0.52787(4) 0.0412(3) Uani 1 1 d . . . S1 S 0.0476(6) 1.1620(5) 0.9821(4) 0.093(3) Uani 1 1 d U . . S2 S 0.0648(4) 1.1512(3) 0.8086(3) 0.054(2) Uani 1 1 d . . . S3 S 0.0750(4) 0.9407(4) 0.7316(3) 0.058(2) Uani 1 1 d . . . S4 S 0.1491(4) 1.1006(3) 0.6487(3) 0.054(2) Uani 1 1 d . . . S5 S 0.1035(4) 0.8792(4) 0.5664(3) 0.056(2) Uani 1 1 d . . . S6 S 0.1967(6) 0.8106(5) 0.4086(4) 0.090(3) Uani 1 1 d U . . S7 S 0.4466(5) 0.6849(4) 0.7833(3) 0.071(3) Uani 1 1 d . . . S8 S 0.5853(5) 0.0967(3) 0.9117(3) 0.066(3) Uani 1 1 d . . . S9 S 0.6349(5) 0.9009(3) 0.7102(3) 0.060(2) Uani 1 1 d . . . S10 S 0.6279(5) 0.8503(4) 0.5494(4) 0.078(3) Uani 1 1 d . . . F1 F 0.0845(12) 1.2630(10) 1.0113(8) 0.119(8) Uani 1 1 d U . . F2 F -0.0134(15) 1.2396(12) 1.0194(11) 0.156(10) Uani 1 1 d U . . F3 F 0.0164(14) 1.2558(12) 0.9465(11) 0.152(10) Uani 1 1 d U . . F4 F -0.0512(11) 1.1738(9) 0.8275(8) 0.111(7) Uani 1 1 d U . . F5 F -0.0448(11) 1.1485(9) 0.7573(8) 0.110(7) Uani 1 1 d U . . F6 F -0.0356(9) 1.0843(9) 0.8102(8) 0.098(7) Uani 1 1 d . . . F7 F -0.0381(11) 0.9753(9) 0.7449(8) 0.112(7) Uani 1 1 d U . . F8 F 0.0022(13) 1.0245(11) 0.6932(9) 0.138(9) Uani 1 1 d U . . F9 F -0.0316(11) 0.9366(10) 0.6782(8) 0.113(7) Uani 1 1 d U . . F10 F 0.0453(14) 1.1582(12) 0.6464(10) 0.151(10) Uani 1 1 d U . . F11 F 0.0310(10) 1.0753(12) 0.6120(10) 0.135(10) Uani 1 1 d . . . F12 F 0.0779(12) 1.1455(10) 0.5784(8) 0.120(8) Uani 1 1 d U . . F13 F -0.0169(12) 0.9084(10) 0.5662(8) 0.120(8) Uani 1 1 d U . . F14 F 0.0343(12) 0.9549(11) 0.5166(9) 0.130(8) Uani 1 1 d U . . F15 F 0.0081(11) 0.8691(9) 0.5012(8) 0.108(7) Uani 1 1 d U . . F16 F 0.0797(14) 0.8356(12) 0.4179(10) 0.145(10) Uani 1 1 d U . . F17 F 0.1349(19) 0.9014(19) 0.3916(14) 0.220(16) Uani 1 1 d U . . F18 F 0.1063(17) 0.8330(15) 0.3469(14) 0.200(14) Uani 1 1 d U . . F19 F 0.4165(13) 0.5836(12) 0.7433(9) 0.141(9) Uani 1 1 d U . . F20 F 0.3533(12) 0.6563(10) 0.7205(8) 0.116(8) Uani 1 1 d U . . F21 F 0.3473(11) 0.6142(10) 0.7860(8) 0.115(7) Uani 1 1 d U . . F22 F 0.6050(12) 0.0047(9) 0.8625(8) 0.119(8) Uani 1 1 d . . . F23 F 0.6817(11) 0.0638(10) 0.8681(8) 0.110(7) Uani 1 1 d . . . F24 F 0.6648(11) 0.0094(9) 0.9244(7) 0.113(8) Uani 1 1 d . . . F25 F 0.6875(12) 0.8876(10) 0.7957(7) 0.115(8) Uani 1 1 d . . . F26 F 0.6719(10) 0.9741(8) 0.7776(7) 0.090(6) Uani 1 1 d . . . F27 F 0.5966(11) 0.9170(9) 0.7939(8) 0.103(7) Uani 1 1 d U . . F28 F 0.5624(12) 0.7565(11) 0.5228(9) 0.133(9) Uani 1 1 d U . . F29 F 0.5104(11) 0.8328(9) 0.5106(7) 0.107(8) Uani 1 1 d . . . F30 F 0.5771(12) 0.8109(10) 0.4695(9) 0.129(8) Uani 1 1 d U . . O1 O 0.1037(8) 1.1631(7) 0.9529(7) 0.052(5) Uani 1 1 d . . . O2 O 0.0708(12) 1.1485(10) 1.0367(8) 0.092(8) Uani 1 1 d U . . O3 O -0.0057(9) 1.1327(10) 0.9616(6) 0.069(6) Uani 1 1 d . . . O4 O 0.0801(8) 1.1396(7) 0.8585(6) 0.045(5) Uani 1 1 d . . . O5 O 0.0898(10) 1.1053(8) 0.7784(6) 0.064(6) Uani 1 1 d . . . O6 O 0.0725(11) 1.2105(8) 0.7946(7) 0.075(7) Uani 1 1 d . . . O7 O 0.1024(9) 0.9843(8) 0.7651(6) 0.050(5) Uani 1 1 d . . . O8 O 0.1074(9) 0.9394(9) 0.6903(7) 0.064(6) Uani 1 1 d . . . O9 O 0.0625(11) 0.8864(9) 0.7529(8) 0.083(7) Uani 1 1 d . . . O10 O 0.1391(9) 1.0933(7) 0.6982(6) 0.049(5) Uani 1 1 d . . . O11 O 0.1623(8) 1.0451(6) 0.6249(5) 0.038(4) Uani 1 1 d . . . O1-2 O 0.1934(8) 1.0788(7) 0.8461(6) 0.042(5) Uani 1 1 d . . . O12 O 0.1910(12) 1.1479(8) 0.6384(7) 0.080(8) Uani 1 1 d . . . O13 O 0.1180(9) 0.9254(8) 0.5993(7) 0.060(6) Uani 1 1 d . . . O14 O 0.1449(9) 0.8774(7) 0.5294(6) 0.056(5) Uani 1 1 d . . . O15 O 0.0913(10) 0.8250(9) 0.5874(8) 0.073(6) Uani 1 1 d . . . O16 O 0.2132(9) 0.8330(8) 0.4580(6) 0.056(5) Uani 1 1 d . . . O17 O 0.1812(18) 0.7549(17) 0.4117(13) 0.170(14) Uani 1 1 d U . . O18 O 0.2423(17) 0.8264(15) 0.3761(12) 0.158(13) Uani 1 1 d U . . O19 O 0.4059(11) 0.7306(9) 0.7981(9) 0.090(8) Uani 1 1 d . . . O20 O 0.4780(10) 0.6521(10) 0.8205(8) 0.083(7) Uani 1 1 d . . . O21 O 0.4850(12) 0.6988(10) 0.7459(8) 0.093(8) Uani 1 1 d . . . O22 O 0.6301(11) 0.1330(9) 0.9399(9) 0.088(8) Uani 1 1 d . . . O2-3 O 0.2237(8) 0.9995(7) 0.7186(6) 0.046(5) Uani 1 1 d . . . O23 O 0.5423(11) 0.0629(9) 0.9376(7) 0.083(7) Uani 1 1 d . . . O24 O 0.5553(11) 0.1237(9) 0.8699(7) 0.077(7) Uani 1 1 d . . . O25 O 0.5836(11) 0.9406(9) 0.6935(8) 0.081(7) Uani 1 1 d . . . O26 O 0.6152(11) 0.8402(8) 0.7122(7) 0.077(7) Uani 1 1 d . . . O27 O 0.6954(10) 0.9137(9) 0.6922(7) 0.064(6) Uani 1 1 d . . . O28 O 0.6223(13) 0.9061(12) 0.5363(9) 0.111(9) Uani 1 1 d U . . O29 O 0.6839(12) 0.8179(9) 0.5516(9) 0.094(8) Uani 1 1 d . . . O30 O 0.6007(15) 0.8439(13) 0.5979(12) 0.142(11) Uani 1 1 d U . . O3-4 O 0.2482(7) 0.9171(7) 0.5915(6) 0.043(5) Uani 1 1 d . . . N1 N 0.2335(11) 1.1581(10) 0.9918(8) 0.053(6) Uiso 1 1 d . . . N2 N 0.1616(11) 1.0571(9) 0.9929(8) 0.048(6) Uiso 1 1 d . . . N3 N 0.1025(11) 1.0220(9) 0.9093(8) 0.047(6) Uiso 1 1 d . . . N4 N 0.1901(10) 1.2192(8) 0.8852(7) 0.038(5) Uiso 1 1 d . . . N5 N 0.2923(11) 1.1457(9) 0.8973(8) 0.048(6) Uiso 1 1 d . . . N6 N 0.2715(11) 1.0382(9) 0.9325(7) 0.043(6) Uiso 1 1 d . . . N7 N 0.2559(11) 1.1438(8) 0.7577(7) 0.040(5) Uiso 1 1 d . . . N8 N 0.3148(11) 1.0470(9) 0.7922(7) 0.047(6) Uiso 1 1 d . . . N9 N 0.2392(10) 0.9581(8) 0.8196(7) 0.040(5) Uiso 1 1 d . . . N10 N 0.3082(12) 1.0213(9) 0.6368(8) 0.051(6) Uiso 1 1 d . . . N11 N 0.3283(10) 0.9241(8) 0.6925(7) 0.041(6) Uiso 1 1 d . . . N12 N 0.2234(12) 0.8540(9) 0.6931(8) 0.051(6) Uiso 1 1 d . . . N13 N 0.2245(11) 0.9773(9) 0.4957(8) 0.051(6) Uiso 1 1 d . . . N14 N 0.3107(11) 0.9173(9) 0.4503(7) 0.042(6) Uiso 1 1 d . . . N15 N 0.3474(11) 0.8093(9) 0.4859(8) 0.047(6) Uiso 1 1 d . . . N16 N 0.2353(12) 0.7742(10) 0.5571(9) 0.060(7) Uiso 1 1 d . . . N17 N 0.3479(12) 0.8263(9) 0.5897(8) 0.053(6) Uiso 1 1 d . . . N18 N 0.3745(11) 0.9295(9) 0.5503(8) 0.050(6) Uiso 1 1 d . . . N19 N 0.192(2) 0.580(2) 0.6957(19) 0.17(2) Uiso 1 1 d . . . N30 N 0.4984(18) 0.8763(16) 0.8721(13) 0.124(12) Uiso 1 1 d G . . C1 C 0.2572(14) 1.2138(12) 0.9914(11) 0.059(8) Uiso 1 1 d . . . H1A H 0.2705 1.2292 0.9637 0.071 Uiso 1 1 calc R . . C2 C 0.2618(16) 1.2489(15) 1.0336(12) 0.076(10) Uiso 1 1 d . . . H2B H 0.2749 1.2878 1.0319 0.092 Uiso 1 1 calc R . . C3 C 0.2474(19) 1.2269(17) 1.0766(15) 0.104(13) Uiso 1 1 d . . . H3 H 0.2496 1.2488 1.1043 0.124 Uiso 1 1 calc R . . C4 C 0.2291(18) 1.1679(16) 1.0736(14) 0.092(12) Uiso 1 1 d . . . H4A H 0.2213 1.1488 1.1014 0.110 Uiso 1 1 calc R . . C5 C 0.2221(16) 1.1373(13) 1.0328(12) 0.066(9) Uiso 1 1 d . . . C6 C 0.1937(15) 1.0775(12) 1.0334(10) 0.057(8) Uiso 1 1 d . . . C7 C 0.1906(15) 1.0451(13) 1.0752(11) 0.066(9) Uiso 1 1 d . . . H7A H 0.2112 1.0593 1.1033 0.080 Uiso 1 1 calc R . . C8 C 0.1583(16) 0.9939(14) 1.0753(12) 0.075(10) Uiso 1 1 d . . . H8A H 0.1620 0.9708 1.1024 0.090 Uiso 1 1 calc R . . C9 C 0.1194(15) 0.9750(12) 1.0354(10) 0.059(8) Uiso 1 1 d . . . H9 H 0.0930 0.9424 1.0361 0.070 Uiso 1 1 calc R . . C10 C 0.1228(14) 1.0092(11) 0.9929(10) 0.048(7) Uiso 1 1 d . . . C11 C 0.0868(14) 0.9937(12) 0.9488(10) 0.050(8) Uiso 1 1 d . . . C12 C 0.0379(19) 0.9525(17) 0.9494(15) 0.104(13) Uiso 1 1 d . . . H12 H 0.0290 0.9333 0.9769 0.125 Uiso 1 1 calc R . . C13 C 0.003(2) 0.9422(17) 0.9061(15) 0.109(14) Uiso 1 1 d . . . H13A H -0.0329 0.9185 0.9048 0.131 Uiso 1 1 calc R . . C14 C 0.022(2) 0.9665(17) 0.8638(15) 0.107(14) Uiso 1 1 d . . . H14A H 0.0036 0.9541 0.8342 0.128 Uiso 1 1 calc R . . C15 C 0.0685(15) 1.0103(12) 0.8688(11) 0.059(8) Uiso 1 1 d . . . H15B H 0.0761 1.0322 0.8424 0.071 Uiso 1 1 calc R . . C16 C 0.1396(15) 1.2551(11) 0.8827(10) 0.053(8) Uiso 1 1 d . . . H16A H 0.1018 1.2430 0.8943 0.063 Uiso 1 1 calc R . . C17 C 0.1435(18) 1.3099(14) 0.8630(11) 0.076(10) Uiso 1 1 d . . . H17B H 0.1089 1.3354 0.8625 0.091 Uiso 1 1 calc R . . C18 C 0.1977(16) 1.3270(14) 0.8444(11) 0.067(9) Uiso 1 1 d . . . H18B H 0.1990 1.3627 0.8287 0.081 Uiso 1 1 calc R . . C19 C 0.2513(15) 1.2906(12) 0.8490(9) 0.055(8) Uiso 1 1 d . . . H19B H 0.2903 1.3027 0.8393 0.066 Uiso 1 1 calc R . . C20 C 0.2445(12) 1.2369(10) 0.8681(8) 0.033(6) Uiso 1 1 d . . . C21 C 0.2979(13) 1.2012(11) 0.8751(9) 0.041(7) Uiso 1 1 d . . . C22 C 0.3622(15) 1.2167(13) 0.8652(10) 0.060(9) Uiso 1 1 d . . . H22B H 0.3690 1.2518 0.8498 0.072 Uiso 1 1 calc R . . C23 C 0.4123(16) 1.1810(12) 0.8780(10) 0.059(8) Uiso 1 1 d . . . H23B H 0.4526 1.1939 0.8715 0.071 Uiso 1 1 calc R . . C24 C 0.4094(14) 1.1272(11) 0.8997(9) 0.048(7) Uiso 1 1 d . . . H24 H 0.4447 1.1033 0.9076 0.057 Uiso 1 1 calc R . . C25 C 0.3434(15) 1.1123(12) 0.9090(10) 0.057(8) Uiso 1 1 d . . . C26 C 0.3349(16) 1.0529(13) 0.9310(10) 0.061(8) Uiso 1 1 d . . . C27 C 0.3854(17) 1.0175(13) 0.9474(11) 0.070(10) Uiso 1 1 d . . . H27B H 0.4277 1.0299 0.9472 0.084 Uiso 1 1 calc R . . C28 C 0.3703(17) 0.9621(14) 0.9645(11) 0.074(10) Uiso 1 1 d . . . H28A H 0.4032 0.9372 0.9765 0.089 Uiso 1 1 calc R . . C29 C 0.3088(15) 0.9442(13) 0.9638(10) 0.060(8) Uiso 1 1 d . . . H29B H 0.2986 0.9067 0.9735 0.072 Uiso 1 1 calc R . . C30 C 0.2618(16) 0.9839(12) 0.9481(10) 0.060(9) Uiso 1 1 d . . . H30B H 0.2195 0.9718 0.9484 0.072 Uiso 1 1 calc R . . C31 C 0.2232(13) 1.1906(10) 0.7430(8) 0.041(7) Uiso 1 1 d . . . H31A H 0.1788 1.1909 0.7425 0.049 Uiso 1 1 calc R . . C32 C 0.2548(14) 1.2393(12) 0.7282(9) 0.050(8) Uiso 1 1 d . . . H32A H 0.2318 1.2732 0.7198 0.060 Uiso 1 1 calc R . . C33 C 0.3171(16) 1.2382(13) 0.7261(11) 0.065(9) Uiso 1 1 d . . . H33A H 0.3377 1.2698 0.7136 0.078 Uiso 1 1 calc R . . C34 C 0.3508(18) 1.1907(14) 0.7421(12) 0.082(11) Uiso 1 1 d . . . H34A H 0.3951 1.1896 0.7417 0.098 Uiso 1 1 calc R . . C35 C 0.3173(15) 1.1416(11) 0.7601(10) 0.049(8) Uiso 1 1 d . . . C36 C 0.3531(14) 1.0898(11) 0.7796(9) 0.043(7) Uiso 1 1 d . . . C37 C 0.4225(14) 1.0852(12) 0.7855(9) 0.050(8) Uiso 1 1 d . . . H37A H 0.4481 1.1149 0.7753 0.060 Uiso 1 1 calc R . . C38 C 0.4488(16) 1.0363(12) 0.8065(10) 0.060(9) Uiso 1 1 d . . . H38A H 0.4931 1.0327 0.8114 0.073 Uiso 1 1 calc R . . C39 C 0.4109(15) 0.9924(12) 0.8206(10) 0.057(8) Uiso 1 1 d . . . H39A H 0.4286 0.9585 0.8346 0.068 Uiso 1 1 calc R . . C40 C 0.3439(14) 0.9999(11) 0.8130(10) 0.050(8) Uiso 1 1 d . . . C41 C 0.3031(12) 0.9489(10) 0.8277(8) 0.035(6) Uiso 1 1 d . . . C42 C 0.3271(16) 0.8971(13) 0.8479(10) 0.066(9) Uiso 1 1 d . . . H42A H 0.3712 0.8918 0.8531 0.079 Uiso 1 1 calc R . . C43 C 0.2860(16) 0.8530(13) 0.8604(10) 0.062(9) Uiso 1 1 d . . . H43A H 0.3020 0.8175 0.8725 0.074 Uiso 1 1 calc R . . C44 C 0.2218(17) 0.8635(14) 0.8545(11) 0.073(10) Uiso 1 1 d . . . H44A H 0.1926 0.8366 0.8645 0.087 Uiso 1 1 calc R . . C45 C 0.2012(16) 0.9169(12) 0.8324(10) 0.058(8) Uiso 1 1 d . . . H45A H 0.1573 0.9231 0.8265 0.069 Uiso 1 1 calc R . . C46 C 0.2960(15) 1.0652(12) 0.6067(10) 0.060(9) Uiso 1 1 d . . . H46A H 0.2562 1.0676 0.5891 0.071 Uiso 1 1 calc R . . C47 C 0.3428(15) 1.1084(13) 0.6012(10) 0.062(9) Uiso 1 1 d . . . H47A H 0.3346 1.1391 0.5800 0.074 Uiso 1 1 calc R . . C48 C 0.3990(16) 1.1040(13) 0.6271(10) 0.062(9) Uiso 1 1 d . . . H48A H 0.4291 1.1336 0.6251 0.074 Uiso 1 1 calc R . . C49 C 0.4149(16) 1.0561(13) 0.6576(11) 0.066(9) Uiso 1 1 d . . . H49 H 0.4547 1.0534 0.6750 0.080 Uiso 1 1 calc R . . C50 C 0.3685(15) 1.0131(12) 0.6603(10) 0.050(8) Uiso 1 1 d . . . C51 C 0.3794(13) 0.9595(10) 0.6882(8) 0.036(6) Uiso 1 1 d . . . C52 C 0.4364(14) 0.9458(11) 0.7082(9) 0.048(7) Uiso 1 1 d . . . H52A H 0.4704 0.9713 0.7055 0.058 Uiso 1 1 calc R . . C53 C 0.4469(15) 0.8950(12) 0.7330(10) 0.058(8) Uiso 1 1 d . . . H53A H 0.4882 0.8852 0.7455 0.070 Uiso 1 1 calc R . . C54 C 0.3965(14) 0.8583(12) 0.7398(10) 0.054(8) Uiso 1 1 d . . . H54A H 0.4024 0.8242 0.7576 0.064 Uiso 1 1 calc R . . C55 C 0.3362(15) 0.8746(12) 0.7185(10) 0.056(8) Uiso 1 1 d . . . C56 C 0.2788(15) 0.8379(12) 0.7186(10) 0.054(8) Uiso 1 1 d . . . C57 C 0.2804(15) 0.7853(11) 0.7486(9) 0.050(8) Uiso 1 1 d . . . H57 H 0.3173 0.7741 0.7673 0.059 Uiso 1 1 calc R . . C58 C 0.2257(18) 0.7541(15) 0.7477(12) 0.082(11) Uiso 1 1 d . . . H58A H 0.2254 0.7213 0.7672 0.098 Uiso 1 1 calc R . . C59 C 0.1696(17) 0.7678(13) 0.7196(11) 0.071(10) Uiso 1 1 d . . . H59A H 0.1337 0.7437 0.7179 0.085 Uiso 1 1 calc R . . C60 C 0.1706(15) 0.8195(12) 0.6942(10) 0.054(8) Uiso 1 1 d . . . H60A H 0.1330 0.8314 0.6768 0.064 Uiso 1 1 calc R . . C61 C 0.1795(15) 1.0062(13) 0.5145(11) 0.062(9) Uiso 1 1 d . . . H61A H 0.1609 0.9871 0.5386 0.075 Uiso 1 1 calc R . . C62 C 0.1562(16) 1.0619(13) 0.5028(11) 0.072(10) Uiso 1 1 d . . . H62A H 0.1270 1.0816 0.5195 0.087 Uiso 1 1 calc R . . C63 C 0.1812(17) 1.0845(15) 0.4639(12) 0.079(10) Uiso 1 1 d . . . H63A H 0.1686 1.1220 0.4540 0.094 Uiso 1 1 calc R . . C64 C 0.2223(16) 1.0560(13) 0.4394(11) 0.069(9) Uiso 1 1 d . . . H64A H 0.2350 1.0719 0.4116 0.083 Uiso 1 1 calc R . . C65 C 0.2457(14) 1.0026(12) 0.4558(10) 0.050(8) Uiso 1 1 d . . . C66 C 0.2944(13) 0.9714(11) 0.4325(9) 0.044(7) Uiso 1 1 d . . . C67 C 0.3167(16) 0.9904(14) 0.3910(11) 0.070(9) Uiso 1 1 d . . . H67A H 0.3001 1.0241 0.3759 0.084 Uiso 1 1 calc R . . C68 C 0.3630(16) 0.9590(13) 0.3725(11) 0.069(9) Uiso 1 1 d . . . H68A H 0.3821 0.9738 0.3469 0.083 Uiso 1 1 calc R . . C69 C 0.3812(15) 0.9084(12) 0.3903(10) 0.059(8) Uiso 1 1 d . . . H69A H 0.4125 0.8870 0.3769 0.070 Uiso 1 1 calc R . . C70 C 0.3537(14) 0.8857(12) 0.4298(10) 0.050(7) Uiso 1 1 d . . . C71 C 0.3734(14) 0.8282(11) 0.4463(10) 0.048(7) Uiso 1 1 d . . . C72 C 0.4074(15) 0.7911(13) 0.4226(11) 0.063(9) Uiso 1 1 d . . . H72A H 0.4231 0.8045 0.3951 0.075 Uiso 1 1 calc R . . C73 C 0.4201(17) 0.7361(14) 0.4359(12) 0.077(10) Uiso 1 1 d . . . H73A H 0.4431 0.7115 0.4177 0.092 Uiso 1 1 calc R . . C74 C 0.3982(15) 0.7160(14) 0.4779(11) 0.068(9) Uiso 1 1 d . . . H74A H 0.4081 0.6786 0.4893 0.082 Uiso 1 1 calc R . . C75 C 0.3607(14) 0.7545(12) 0.5023(10) 0.056(8) Uiso 1 1 d . . . H75A H 0.3448 0.7421 0.5301 0.068 Uiso 1 1 calc R . . C76 C 0.1829(16) 0.7491(13) 0.5381(11) 0.066(9) Uiso 1 1 d . . . H76A H 0.1630 0.7649 0.5103 0.079 Uiso 1 1 calc R . . C77 C 0.1553(19) 0.7010(15) 0.5567(13) 0.088(11) Uiso 1 1 d . . . H77A H 0.1195 0.6829 0.5411 0.106 Uiso 1 1 calc R . . C78 C 0.1820(17) 0.6817(14) 0.5980(12) 0.074(10) Uiso 1 1 d . . . H78A H 0.1609 0.6532 0.6140 0.089 Uiso 1 1 calc R . . C79 C 0.2402(16) 0.7027(13) 0.6180(12) 0.072(10) Uiso 1 1 d . . . H79 H 0.2625 0.6861 0.6446 0.086 Uiso 1 1 calc R . . C80 C 0.2629(14) 0.7518(12) 0.5943(10) 0.048(7) Uiso 1 1 d . . . C81 C 0.3279(16) 0.7763(13) 0.6120(11) 0.060(8) Uiso 1 1 d . . . C82 C 0.3724(15) 0.7469(12) 0.6420(10) 0.055(8) Uiso 1 1 d . . . H82A H 0.3607 0.7113 0.6545 0.066 Uiso 1 1 calc R . . C83 C 0.4330(18) 0.7674(14) 0.6544(12) 0.080(11) Uiso 1 1 d . . . H83A H 0.4616 0.7480 0.6761 0.096 Uiso 1 1 calc R . . C84 C 0.4494(16) 0.8199(13) 0.6320(11) 0.066(9) Uiso 1 1 d . . . H84A H 0.4904 0.8353 0.6384 0.080 Uiso 1 1 calc R . . C85 C 0.4061(15) 0.8481(11) 0.6014(10) 0.049(7) Uiso 1 1 d . . . C86 C 0.4175(13) 0.9039(10) 0.5793(9) 0.039(7) Uiso 1 1 d . . . C87 C 0.4791(15) 0.9298(12) 0.5886(10) 0.057(8) Uiso 1 1 d . . . H87A H 0.5106 0.9115 0.6087 0.069 Uiso 1 1 calc R . . C88 C 0.4916(17) 0.9824(14) 0.5673(11) 0.072(10) Uiso 1 1 d . . . H88A H 0.5330 0.9973 0.5711 0.087 Uiso 1 1 calc R . . C89 C 0.4456(14) 1.0131(12) 0.5412(9) 0.049(7) Uiso 1 1 d . . . H89A H 0.4524 1.0503 0.5293 0.059 Uiso 1 1 calc R . . C90 C 0.3865(14) 0.9833(11) 0.5336(9) 0.045(7) Uiso 1 1 d . . . H90A H 0.3532 1.0023 0.5157 0.055 Uiso 1 1 calc R . . C91 C 0.035(4) 1.236(3) 0.991(3) 0.22(3) Uiso 1 1 d . . . C92 C -0.0170(19) 1.1383(16) 0.8019(13) 0.077(10) Uiso 1 1 d . . . C93 C -0.003(2) 0.9726(18) 0.7111(15) 0.097(13) Uiso 1 1 d . . . C94 C 0.068(2) 1.1138(18) 0.6215(14) 0.086(12) Uiso 1 1 d . . . C95 C 0.0264(19) 0.9045(17) 0.5338(14) 0.084(11) Uiso 1 1 d . . . C96 C 0.121(3) 0.852(3) 0.391(2) 0.139(19) Uiso 1 1 d . . . C97 C 0.390(3) 0.632(2) 0.7559(18) 0.126(16) Uiso 1 1 d . . . C98 C 0.6385(19) 0.0423(16) 0.8917(13) 0.072(10) Uiso 1 1 d . . . C99 C 0.651(2) 0.9217(17) 0.7717(14) 0.078(11) Uiso 1 1 d . . . C100 C 0.567(2) 0.8138(16) 0.5207(13) 0.079(11) Uiso 1 1 d . . . C101 C 0.195(3) 0.575(3) 0.730(2) 0.16(2) Uiso 1 1 d . . . C102 C 0.205(2) 0.5493(18) 0.7808(15) 0.126(16) Uiso 1 1 d . . . H10A H 0.1978 0.5795 0.8031 0.189 Uiso 1 1 calc R . . H10B H 0.2484 0.5352 0.7870 0.189 Uiso 1 1 calc R . . H10C H 0.1760 0.5175 0.7839 0.189 Uiso 1 1 calc R . . C103 C 0.523(3) 0.825(2) 0.8519(19) 0.146(19) Uiso 1 1 d G . . H103 H 0.5071 0.8070 0.8236 0.175 Uiso 1 1 calc R . . C104 C 0.579(3) 0.804(3) 0.885(2) 0.20(3) Uiso 1 1 d G . . H10F H 0.6023 0.7709 0.8782 0.244 Uiso 1 1 calc R . . C105 C 0.594(3) 0.838(3) 0.927(2) 0.17(2) Uiso 1 1 d G . . H10G H 0.6279 0.8236 0.9474 0.208 Uiso 1 1 calc R . . C106 C 0.563(4) 0.890(3) 0.944(3) 0.23(3) Uiso 1 1 d G . . H10H H 0.5731 0.9091 0.9730 0.276 Uiso 1 1 calc R . . C107 C 0.521(2) 0.9058(17) 0.9125(14) 0.092(12) Uiso 1 1 d G . . H10I H 0.5026 0.9422 0.9167 0.110 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 0.0444(8) 0.0415(6) 0.0385(6) -0.0033(5) 0.0151(5) -0.0045(5) U2 0.0457(8) 0.0402(6) 0.0361(6) -0.0032(5) 0.0093(5) 0.0011(6) U3 0.0403(7) 0.0420(6) 0.0369(6) -0.0052(5) 0.0063(5) 0.0035(5) U4 0.0430(8) 0.0423(6) 0.0390(6) -0.0064(5) 0.0070(5) 0.0037(5) S1 0.092(4) 0.093(4) 0.096(4) -0.009(3) 0.016(3) 0.000(3) S2 0.050(6) 0.065(5) 0.048(5) -0.002(4) 0.009(4) 0.003(4) S3 0.052(6) 0.067(5) 0.056(5) -0.012(4) 0.012(4) -0.008(4) S4 0.078(7) 0.042(4) 0.041(5) -0.005(3) 0.004(4) 0.019(4) S5 0.051(6) 0.071(5) 0.047(5) -0.013(4) 0.010(4) 0.001(5) S6 0.089(4) 0.093(4) 0.088(4) -0.011(3) 0.008(3) -0.002(3) S7 0.072(7) 0.082(6) 0.063(6) 0.029(5) 0.023(5) 0.021(5) S8 0.087(8) 0.056(5) 0.056(6) 0.002(4) 0.011(5) -0.011(5) S9 0.068(7) 0.050(5) 0.061(5) -0.007(4) 0.008(5) 0.006(5) S10 0.081(8) 0.053(5) 0.093(7) -0.013(5) -0.020(6) 0.018(5) F1 0.119(8) 0.119(8) 0.119(8) -0.005(3) 0.012(3) 0.001(3) F2 0.156(11) 0.157(11) 0.157(11) -0.002(3) 0.017(3) 0.001(3) F3 0.152(10) 0.153(10) 0.152(10) 0.001(3) 0.017(3) 0.002(3) F4 0.110(8) 0.111(8) 0.111(8) -0.002(3) 0.011(3) 0.002(3) F5 0.109(8) 0.110(8) 0.109(8) 0.000(3) 0.009(3) 0.002(3) F6 0.050(14) 0.106(16) 0.136(19) -0.019(13) -0.003(13) -0.029(12) F7 0.111(8) 0.114(8) 0.112(8) -0.002(3) 0.012(3) 0.000(3) F8 0.137(9) 0.137(9) 0.139(9) 0.001(3) 0.012(3) 0.000(3) F9 0.113(8) 0.115(8) 0.113(8) -0.002(3) 0.011(3) -0.001(3) F10 0.151(10) 0.152(10) 0.151(10) -0.001(3) 0.013(3) 0.003(3) F11 0.044(15) 0.16(2) 0.19(3) -0.003(19) -0.041(16) 0.004(15) F12 0.121(8) 0.120(8) 0.120(8) 0.001(3) 0.011(3) 0.002(3) F13 0.118(8) 0.122(8) 0.119(8) -0.002(3) 0.011(3) 0.001(3) F14 0.130(9) 0.130(9) 0.130(9) 0.001(3) 0.010(3) 0.002(3) F15 0.108(8) 0.110(7) 0.108(7) -0.002(3) 0.009(3) 0.000(3) F16 0.145(10) 0.147(10) 0.144(10) -0.001(3) 0.015(3) 0.000(3) F17 0.220(16) 0.219(16) 0.219(16) 0.001(3) 0.021(3) 0.000(3) F18 0.200(14) 0.202(14) 0.199(14) 0.000(3) 0.019(3) -0.001(3) F19 0.141(10) 0.140(9) 0.141(9) -0.001(3) 0.015(3) -0.001(3) F20 0.116(8) 0.117(8) 0.115(8) 0.002(3) 0.011(3) -0.001(3) F21 0.114(8) 0.117(8) 0.115(8) 0.003(3) 0.012(3) -0.002(3) F22 0.16(2) 0.102(16) 0.096(17) -0.034(13) 0.011(16) -0.003(16) F23 0.097(18) 0.131(18) 0.106(17) -0.014(14) 0.032(15) 0.004(15) F24 0.13(2) 0.111(16) 0.093(16) 0.029(13) 0.000(15) 0.044(15) F25 0.15(2) 0.122(18) 0.063(13) -0.004(13) -0.015(14) -0.016(17) F26 0.099(17) 0.068(12) 0.106(16) -0.039(11) 0.020(13) -0.009(11) F27 0.103(7) 0.105(7) 0.103(7) -0.002(3) 0.012(3) -0.003(3) F28 0.134(9) 0.132(9) 0.133(9) 0.001(3) 0.011(3) -0.002(3) F29 0.074(17) 0.126(17) 0.115(18) -0.061(14) -0.015(14) -0.025(14) F30 0.129(9) 0.129(9) 0.128(9) -0.001(3) 0.013(3) -0.001(3) O1 0.022(12) 0.055(11) 0.082(15) -0.003(10) 0.024(11) 0.006(9) O2 0.092(8) 0.093(8) 0.091(8) 0.002(3) 0.009(3) 0.001(3) O3 0.039(14) 0.118(17) 0.047(13) -0.016(12) -0.011(10) -0.019(13) O4 0.034(12) 0.058(11) 0.043(12) -0.003(9) 0.005(9) -0.006(9) O5 0.076(16) 0.079(14) 0.038(12) -0.010(10) 0.000(11) 0.032(12) O6 0.10(2) 0.058(14) 0.071(15) 0.005(11) 0.008(13) 0.005(12) O7 0.049(14) 0.060(12) 0.041(11) 0.006(9) 0.007(10) 0.001(10) O8 0.049(14) 0.088(15) 0.055(13) -0.027(11) -0.001(11) -0.021(12) O9 0.10(2) 0.067(14) 0.088(17) 0.021(12) 0.029(14) -0.021(13) O10 0.072(15) 0.044(11) 0.033(11) 0.002(8) 0.014(10) 0.016(10) O11 0.047(12) 0.034(9) 0.036(10) 0.003(8) 0.022(9) 0.010(9) O1-2 0.050(13) 0.037(9) 0.039(11) 0.009(8) 0.004(9) 0.005(9) O12 0.15(2) 0.035(11) 0.058(14) 0.005(9) 0.036(15) -0.011(13) O13 0.038(13) 0.079(14) 0.060(13) -0.028(11) -0.008(10) 0.016(11) O14 0.064(15) 0.046(11) 0.056(13) -0.004(9) 0.003(11) 0.021(10) O15 0.071(18) 0.069(14) 0.081(16) -0.007(12) 0.019(13) -0.005(12) O16 0.068(16) 0.066(12) 0.034(11) -0.023(9) 0.004(10) -0.003(11) O17 0.171(14) 0.170(14) 0.170(14) 0.000(3) 0.017(3) 0.001(3) O18 0.157(13) 0.159(13) 0.156(13) -0.002(3) 0.016(3) -0.001(3) O19 0.076(19) 0.074(15) 0.12(2) 0.014(14) 0.034(16) 0.043(14) O20 0.061(17) 0.104(17) 0.080(17) 0.032(14) -0.009(13) 0.028(14) O21 0.12(2) 0.095(17) 0.074(16) 0.014(13) 0.043(16) -0.010(16) O22 0.080(19) 0.066(14) 0.12(2) -0.044(13) 0.008(15) -0.026(13) O2-3 0.036(13) 0.052(11) 0.053(12) 0.001(9) 0.012(10) 0.003(9) O23 0.09(2) 0.085(16) 0.069(16) 0.013(12) 0.005(14) -0.012(14) O24 0.081(18) 0.089(16) 0.060(14) 0.033(12) 0.009(13) 0.003(13) O25 0.078(18) 0.082(16) 0.084(17) 0.019(13) 0.015(14) 0.021(14) O26 0.11(2) 0.049(13) 0.071(15) -0.017(10) 0.034(14) -0.018(12) O27 0.052(15) 0.088(15) 0.057(14) 0.007(11) 0.023(12) 0.009(12) O28 0.111(9) 0.110(9) 0.112(9) 0.000(3) 0.009(3) 0.000(3) O29 0.08(2) 0.064(15) 0.14(2) -0.026(14) 0.020(17) 0.021(14) O30 0.142(12) 0.143(12) 0.141(12) 0.000(3) 0.014(3) 0.000(3) O3-4 0.009(11) 0.048(10) 0.068(13) 0.003(9) -0.012(9) 0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1-2 2.044(16) . ? U1 O1 2.390(17) . ? U1 O4 2.535(18) . ? U1 N6 2.57(2) . ? U1 N5 2.57(2) . ? U1 N3 2.58(2) . ? U1 N4 2.604(19) . ? U1 N2 2.68(2) . ? U1 N1 2.68(2) . ? U2 O2-3 2.075(17) . ? U2 O1-2 2.167(16) . ? U2 O7 2.441(18) . ? U2 N8 2.51(2) . ? U2 O10 2.553(17) . ? U2 N7 2.57(2) . ? U2 O5 2.570(19) . ? U2 N9 2.58(2) . ? U3 O3-4 2.116(18) . ? U3 O2-3 2.119(17) . ? U3 O11 2.490(15) . ? U3 N12 2.52(2) . ? U3 O13 2.537(18) . ? U3 N10 2.56(2) . ? U3 N11 2.58(2) . ? U3 O8 2.63(2) . ? U4 O3-4 2.098(17) . ? U4 O16 2.392(17) . ? U4 O14 2.55(2) . ? U4 N16 2.58(2) . ? U4 N13 2.59(2) . ? U4 N17 2.60(2) . ? U4 N18 2.60(2) . ? U4 N14 2.65(2) . ? U4 N15 2.67(2) . ? S1 O3 1.380(19) . ? S1 O1 1.506(18) . ? S1 O2 1.61(2) . ? S1 C91 1.73(7) . ? S2 O6 1.42(2) . ? S2 O4 1.446(18) . ? S2 O5 1.481(18) . ? S2 C92 1.73(4) . ? S3 O9 1.414(19) . ? S3 O8 1.41(2) . ? S3 O7 1.455(19) . ? S3 C93 1.83(4) . ? S4 O12 1.44(2) . ? S4 O10 1.453(17) . ? S4 O11 1.477(15) . ? S4 C94 1.82(4) . ? S5 O15 1.41(2) . ? S5 O13 1.422(18) . ? S5 O14 1.43(2) . ? S5 C95 1.87(4) . ? S6 O17 1.32(4) . ? S6 O18 1.44(3) . ? S6 O16 1.503(18) . ? S6 C96 1.87(6) . ? S7 O20 1.40(2) . ? S7 O21 1.43(2) . ? S7 O19 1.44(2) . ? S7 C97 1.81(5) . ? S8 O24 1.43(2) . ? S8 O22 1.44(2) . ? S8 O23 1.44(2) . ? S8 C98 1.80(4) . ? S9 O26 1.446(19) . ? S9 O27 1.45(2) . ? S9 O25 1.45(2) . ? S9 C99 1.81(4) . ? S10 O28 1.33(3) . ? S10 O29 1.39(2) . ? S10 O30 1.55(3) . ? S10 C100 1.67(4) . ? F1 C91 1.30(8) . ? F2 C91 1.36(8) . ? F3 C91 1.35(8) . ? F4 C92 1.34(4) . ? F5 C92 1.36(4) . ? F6 C92 1.32(4) . ? F7 C93 1.27(4) . ? F8 C93 1.30(4) . ? F9 C93 1.34(4) . ? F10 C94 1.35(4) . ? F11 C94 1.19(4) . ? F12 C94 1.45(4) . ? F13 C95 1.36(4) . ? F14 C95 1.27(4) . ? F15 C95 1.26(4) . ? F16 C96 1.27(6) . ? F17 C96 1.16(6) . ? F18 C96 1.34(6) . ? F19 C97 1.30(5) . ? F20 C97 1.33(5) . ? F21 C97 1.37(5) . ? F22 C98 1.34(4) . ? F23 C98 1.28(4) . ? F24 C98 1.28(4) . ? F24 U1 6.08(2) 3_667 ? F25 C99 1.25(4) . ? F26 C99 1.28(4) . ? F27 C99 1.36(4) . ? F28 C100 1.31(4) . ? F29 C100 1.27(4) . ? F30 C100 1.49(4) . ? O22 U4 6.007(19) 2_646 ? O28 U4 5.85(3) 3_676 ? O29 U1 5.58(2) 2_646 ? N1 C5 1.30(3) . ? N1 C1 1.37(3) . ? N2 C10 1.36(3) . ? N2 C6 1.36(3) . ? N3 C15 1.32(3) . ? N3 C11 1.36(3) . ? N4 C16 1.34(3) . ? N4 C20 1.35(3) . ? N5 C25 1.33(3) . ? N5 C21 1.42(3) . ? N6 C30 1.34(3) . ? N6 C26 1.38(3) . ? N7 C35 1.28(3) . ? N7 C31 1.32(3) . ? N8 C36 1.34(3) . ? N8 C40 1.34(3) . ? N9 C45 1.31(3) . ? N9 C41 1.35(3) . ? N10 C46 1.32(3) . ? N10 C50 1.38(3) . ? N11 C55 1.35(3) . ? N11 C51 1.36(3) . ? N12 C56 1.36(3) . ? N12 C60 1.36(3) . ? N13 C61 1.31(3) . ? N13 C65 1.39(3) . ? N14 C70 1.33(3) . ? N14 C66 1.36(3) . ? N15 C75 1.35(3) . ? N15 C71 1.37(3) . ? N16 C80 1.26(3) . ? N16 C76 1.31(3) . ? N17 C85 1.33(3) . ? N17 C81 1.39(3) . ? N18 C86 1.30(3) . ? N18 C90 1.35(3) . ? N19 C101 0.97(7) . ? N30 C107 1.37(4) . ? N30 C103 1.43(5) . ? C1 C2 1.44(4) . ? C2 C3 1.38(4) . ? C3 C4 1.40(5) . ? C4 C5 1.35(4) . ? C5 C6 1.49(4) . ? C6 C7 1.41(4) . ? C7 C8 1.35(4) . ? C8 C9 1.40(4) . ? C9 C10 1.44(4) . ? C10 C11 1.44(4) . ? C11 C12 1.39(4) . ? C12 C13 1.39(5) . ? C13 C14 1.41(5) . ? C14 C15 1.40(4) . ? C16 C17 1.37(4) . ? C17 C18 1.36(4) . ? C18 C19 1.40(4) . ? C19 C20 1.35(3) . ? C20 C21 1.38(3) . ? C21 C22 1.45(4) . ? C22 C23 1.35(4) . ? C23 C24 1.38(3) . ? C24 C25 1.47(4) . ? C25 C26 1.51(4) . ? C26 C27 1.38(4) . ? C27 C28 1.40(4) . ? C28 C29 1.35(4) . ? C29 C30 1.38(4) . ? C31 C32 1.38(3) . ? C32 C33 1.32(4) . ? C33 C34 1.35(4) . ? C34 C35 1.44(4) . ? C35 C36 1.48(3) . ? C36 C37 1.45(4) . ? C37 C38 1.36(3) . ? C38 C39 1.36(4) . ? C39 C40 1.41(4) . ? C40 C41 1.53(3) . ? C41 C42 1.39(3) . ? C42 C43 1.39(4) . ? C43 C44 1.36(4) . ? C44 C45 1.42(4) . ? C46 C47 1.41(4) . ? C47 C48 1.33(4) . ? C48 C49 1.41(4) . ? C49 C50 1.39(4) . ? C50 C51 1.46(3) . ? C51 C52 1.31(3) . ? C52 C53 1.36(3) . ? C53 C54 1.38(4) . ? C54 C55 1.40(4) . ? C55 C56 1.47(4) . ? C56 C57 1.47(4) . ? C57 C58 1.35(4) . ? C58 C59 1.39(4) . ? C59 C60 1.38(4) . ? C61 C62 1.39(4) . ? C62 C63 1.37(4) . ? C63 C64 1.33(4) . ? C64 C65 1.38(4) . ? C65 C66 1.46(4) . ? C66 C67 1.38(4) . ? C67 C68 1.35(4) . ? C68 C69 1.30(4) . ? C69 C70 1.41(4) . ? C70 C71 1.44(3) . ? C71 C72 1.33(4) . ? C72 C73 1.33(4) . ? C73 C74 1.40(4) . ? C74 C75 1.41(4) . ? C76 C77 1.37(4) . ? C77 C78 1.33(4) . ? C78 C79 1.38(4) . ? C79 C80 1.41(4) . ? C80 C81 1.51(4) . ? C81 C82 1.38(4) . ? C82 C83 1.37(4) . ? C83 C84 1.42(4) . ? C84 C85 1.36(4) . ? C85 C86 1.45(3) . ? C86 C87 1.42(4) . ? C87 C88 1.38(4) . ? C88 C89 1.35(4) . ? C89 C90 1.41(3) . ? C101 C102 1.56(7) . ? C103 C104 1.50(7) . ? C104 C105 1.44(7) . ? C105 C106 1.47(8) . ? C106 C107 1.24(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1-2 U1 O1 142.0(7) . . ? O1-2 U1 O4 74.7(6) . . ? O1 U1 O4 67.4(6) . . ? O1-2 U1 N6 79.0(6) . . ? O1 U1 N6 136.9(6) . . ? O4 U1 N6 149.5(6) . . ? O1-2 U1 N5 75.5(7) . . ? O1 U1 N5 126.0(6) . . ? O4 U1 N5 122.8(6) . . ? N6 U1 N5 63.3(7) . . ? O1-2 U1 N3 81.2(7) . . ? O1 U1 N3 87.8(6) . . ? O4 U1 N3 73.5(6) . . ? N6 U1 N3 87.6(7) . . ? N5 U1 N3 145.4(7) . . ? O1-2 U1 N4 92.9(6) . . ? O1 U1 N4 75.2(6) . . ? O4 U1 N4 70.7(6) . . ? N6 U1 N4 126.4(7) . . ? N5 U1 N4 63.3(7) . . ? N3 U1 N4 144.0(7) . . ? O1-2 U1 N2 132.1(6) . . ? O1 U1 N2 69.3(6) . . ? O4 U1 N2 117.2(6) . . ? N6 U1 N2 70.9(7) . . ? N5 U1 N2 119.1(7) . . ? N3 U1 N2 61.6(7) . . ? N4 U1 N2 134.9(6) . . ? O1-2 U1 N1 146.3(7) . . ? O1 U1 N1 67.9(7) . . ? O4 U1 N1 131.0(6) . . ? N6 U1 N1 79.4(7) . . ? N5 U1 N1 71.8(7) . . ? N3 U1 N1 123.3(7) . . ? N4 U1 N1 79.5(6) . . ? N2 U1 N1 62.0(7) . . ? O1-2 U1 S2 60.8(5) . . ? O1 U1 S2 81.5(5) . . ? O4 U1 S2 15.7(4) . . ? N6 U1 S2 139.2(5) . . ? N5 U1 S2 109.5(5) . . ? N3 U1 S2 79.8(5) . . ? N4 U1 S2 66.7(5) . . ? N2 U1 S2 131.4(5) . . ? N1 U1 S2 139.2(5) . . ? O1-2 U1 S1 140.9(5) . . ? O1 U1 S1 12.0(4) . . ? O4 U1 S1 68.4(4) . . ? N6 U1 S1 130.8(5) . . ? N5 U1 S1 136.4(5) . . ? N3 U1 S1 76.5(5) . . ? N4 U1 S1 86.9(5) . . ? N2 U1 S1 60.5(5) . . ? N1 U1 S1 72.0(5) . . ? S2 U1 S1 83.7(2) . . ? O1-2 U1 O5 40.2(5) . . ? O1 U1 O5 101.8(5) . . ? O4 U1 O5 34.5(5) . . ? N6 U1 O5 117.8(5) . . ? N5 U1 O5 102.2(6) . . ? N3 U1 O5 74.0(6) . . ? N4 U1 O5 78.8(5) . . ? N2 U1 O5 134.6(6) . . ? N1 U1 O5 157.8(5) . . ? S2 U1 O5 21.4(3) . . ? S1 U1 O5 102.1(3) . . ? O1-2 U1 O3 124.1(6) . . ? O1 U1 O3 27.3(5) . . ? O4 U1 O3 56.7(5) . . ? N6 U1 O3 133.1(6) . . ? N5 U1 O3 153.2(5) . . ? N3 U1 O3 61.1(6) . . ? N4 U1 O3 95.2(6) . . ? N2 U1 O3 63.8(6) . . ? N1 U1 O3 89.5(6) . . ? S2 U1 O3 72.3(3) . . ? S1 U1 O3 18.2(3) . . ? O5 U1 O3 87.8(4) . . ? O1-2 U1 O6 67.0(5) . . ? O1 U1 O6 78.5(5) . . ? O4 U1 O6 25.6(5) . . ? N6 U1 O6 144.6(5) . . ? N5 U1 O6 97.3(6) . . ? N3 U1 O6 96.7(6) . . ? N4 U1 O6 49.4(5) . . ? N2 U1 O6 141.0(6) . . ? N1 U1 O6 124.7(5) . . ? S2 U1 O6 17.3(3) . . ? S1 U1 O6 84.1(3) . . ? O5 U1 O6 33.4(4) . . ? O3 U1 O6 77.4(4) . . ? O1-2 U1 O2 156.7(6) . . ? O1 U1 O2 25.9(5) . . ? O4 U1 O2 88.3(5) . . ? N6 U1 O2 111.7(5) . . ? N5 U1 O2 127.7(6) . . ? N3 U1 O2 78.8(6) . . ? N4 U1 O2 96.3(5) . . ? N2 U1 O2 43.8(5) . . ? N1 U1 O2 56.8(6) . . ? S2 U1 O2 103.7(3) . . ? S1 U1 O2 20.1(3) . . ? O5 U1 O2 121.3(4) . . ? O3 U1 O2 33.9(4) . . ? O6 U1 O2 103.7(4) . . ? O1-2 U1 N9 31.0(5) . . ? O1 U1 N9 153.0(5) . . ? O4 U1 N9 96.6(5) . . ? N6 U1 N9 53.4(5) . . ? N5 U1 N9 80.7(5) . . ? N3 U1 N9 66.4(5) . . ? N4 U1 N9 121.3(5) . . ? N2 U1 N9 102.5(5) . . ? N1 U1 N9 132.4(6) . . ? S2 U1 N9 86.2(3) . . ? S1 U1 N9 142.7(3) . . ? O5 U1 N9 64.9(4) . . ? O3 U1 N9 125.8(4) . . ? O6 U1 N9 96.2(4) . . ? O2 U1 N9 141.6(4) . . ? O2-3 U2 O1-2 157.2(6) . . ? O2-3 U2 O7 83.0(6) . . ? O1-2 U2 O7 101.3(6) . . ? O2-3 U2 N8 77.8(7) . . ? O1-2 U2 N8 85.4(7) . . ? O7 U2 N8 141.2(6) . . ? O2-3 U2 O10 73.8(6) . . ? O1-2 U2 O10 128.8(5) . . ? O7 U2 O10 81.7(6) . . ? N8 U2 O10 123.5(6) . . ? O2-3 U2 N7 98.0(6) . . ? O1-2 U2 N7 88.0(6) . . ? O7 U2 N7 153.7(6) . . ? N8 U2 N7 63.4(7) . . ? O10 U2 N7 73.4(6) . . ? O2-3 U2 O5 128.7(6) . . ? O1-2 U2 O5 72.6(6) . . ? O7 U2 O5 68.0(6) . . ? N8 U2 O5 147.9(7) . . ? O10 U2 O5 61.3(6) . . ? N7 U2 O5 92.1(7) . . ? O2-3 U2 N9 79.9(6) . . ? O1-2 U2 N9 79.0(6) . . ? O7 U2 N9 78.7(6) . . ? N8 U2 N9 65.0(7) . . ? O10 U2 N9 148.8(6) . . ? N7 U2 N9 127.5(7) . . ? O5 U2 N9 130.0(7) . . ? O2-3 U2 S3 67.8(5) . . ? O1-2 U2 S3 116.5(5) . . ? O7 U2 S3 15.5(4) . . ? N8 U2 S3 134.2(5) . . ? O10 U2 S3 75.1(4) . . ? N7 U2 S3 148.1(5) . . ? O5 U2 S3 77.5(5) . . ? N9 U2 S3 79.6(5) . . ? O2-3 U2 S4 61.5(5) . . ? O1-2 U2 S4 140.3(4) . . ? O7 U2 S4 88.0(4) . . ? N8 U2 S4 111.1(5) . . ? O10 U2 S4 14.4(4) . . ? N7 U2 S4 69.9(5) . . ? O5 U2 S4 75.7(4) . . ? N9 U2 S4 140.5(4) . . ? S3 U2 S4 78.27(19) . . ? O2-3 U2 S2 143.4(5) . . ? O1-2 U2 S2 58.8(5) . . ? O7 U2 S2 79.0(4) . . ? N8 U2 S2 133.6(5) . . ? O10 U2 S2 72.2(4) . . ? N7 U2 S2 85.2(5) . . ? O5 U2 S2 15.3(4) . . ? N9 U2 S2 126.4(5) . . ? S3 U2 S2 90.48(18) . . ? S4 U2 S2 86.08(16) . . ? O2-3 U2 O8 47.5(6) . . ? O1-2 U2 O8 138.1(5) . . ? O7 U2 O8 37.2(5) . . ? N8 U2 O8 121.9(6) . . ? O10 U2 O8 65.1(5) . . ? N7 U2 O8 131.3(5) . . ? O5 U2 O8 89.6(5) . . ? N9 U2 O8 84.9(6) . . ? S3 U2 O8 21.8(3) . . ? S4 U2 O8 63.5(3) . . ? S2 U2 O8 104.4(3) . . ? O2-3 U2 O4 160.9(5) . . ? O1-2 U2 O4 39.2(5) . . ? O7 U2 O4 81.7(5) . . ? N8 U2 O4 121.3(5) . . ? O10 U2 O4 92.7(4) . . ? N7 U2 O4 90.9(5) . . ? O5 U2 O4 33.4(5) . . ? N9 U2 O4 108.0(5) . . ? S3 U2 O4 96.0(3) . . ? S4 U2 O4 106.5(3) . . ? S2 U2 O4 20.5(3) . . ? O8 U2 O4 114.7(4) . . ? O2-3 U2 O11 42.2(5) . . ? O1-2 U2 O11 160.4(5) . . ? O7 U2 O11 80.5(5) . . ? N8 U2 O11 105.6(5) . . ? O10 U2 O11 31.6(4) . . ? N7 U2 O11 82.8(5) . . ? O5 U2 O11 90.4(4) . . ? N9 U2 O11 120.2(5) . . ? S3 U2 O11 67.4(3) . . ? S4 U2 O11 20.3(2) . . ? S2 U2 O11 103.0(2) . . ? O8 U2 O11 48.5(4) . . ? O4 U2 O11 123.3(3) . . ? O2-3 U2 O12 66.7(5) . . ? O1-2 U2 O12 131.5(5) . . ? O7 U2 O12 105.8(5) . . ? N8 U2 O12 97.1(6) . . ? O10 U2 O12 26.5(5) . . ? N7 U2 O12 52.3(5) . . ? O5 U2 O12 81.4(5) . . ? N9 U2 O12 145.1(5) . . ? S3 U2 O12 96.0(3) . . ? S4 U2 O12 17.9(3) . . ? S2 U2 O12 87.9(3) . . ? O8 U2 O12 80.0(4) . . ? U3 U2 O12 63.1(2) . . ? O4 U2 O12 106.8(4) . . ? O11 U2 O12 32.6(3) . . ? O2-3 U2 N5 136.3(6) . . ? O1-2 U2 N5 31.8(5) . . ? O7 U2 N5 132.6(5) . . ? N8 U2 N5 58.5(6) . . ? O10 U2 N5 127.3(5) . . ? N7 U2 N5 62.1(5) . . ? O5 U2 N5 92.5(5) . . ? N9 U2 N5 83.5(5) . . ? S3 U2 N5 147.1(3) . . ? S4 U2 N5 130.0(3) . . ? S2 U2 N5 77.2(3) . . ? O8 U2 N5 166.4(4) . . ? O4 U2 N5 62.8(4) . . ? O11 U2 N5 144.8(4) . . ? O12 U2 N5 113.6(4) . . ? O2-3 U2 N3 138.5(5) . . ? O1-2 U2 N3 35.5(5) . . ? O7 U2 N3 66.2(5) . . ? N8 U2 N3 109.0(6) . . ? O10 U2 N3 124.7(5) . . ? N7 U2 N3 122.0(5) . . ? O5 U2 N3 65.2(5) . . ? N9 U2 N3 67.8(5) . . ? S3 U2 N3 81.1(3) . . ? S4 U2 N3 138.8(3) . . ? S2 U2 N3 58.7(3) . . ? O8 U2 N3 102.6(4) . . ? O4 U2 N3 41.1(4) . . ? O11 U2 N3 144.0(4) . . ? O12 U2 N3 146.3(4) . . ? N5 U2 N3 66.4(4) . . ? O2-3 U2 O6 138.5(5) . . ? O1-2 U2 O6 64.1(5) . . ? O7 U2 O6 92.7(5) . . ? N8 U2 O6 123.7(6) . . ? O10 U2 O6 64.7(4) . . ? N7 U2 O6 69.1(6) . . ? O5 U2 O6 24.8(5) . . ? N9 U2 O6 139.8(5) . . ? S3 U2 O6 102.1(3) . . ? S4 U2 O6 77.1(3) . . ? S2 U2 O6 16.6(3) . . ? O8 U2 O6 111.6(4) . . ? O4 U2 O6 31.9(3) . . ? O11 U2 O6 96.3(3) . . ? O12 U2 O6 75.0(4) . . ? N5 U2 O6 73.8(4) . . ? N3 U2 O6 72.8(4) . . ? O2-3 U2 N6 127.5(5) . . ? O1-2 U2 N6 29.7(5) . . ? O7 U2 N6 105.1(5) . . ? N8 U2 N6 63.6(5) . . ? O10 U2 N6 157.8(4) . . ? N7 U2 N6 95.2(5) . . ? O5 U2 N6 101.1(5) . . ? N9 U2 N6 52.6(5) . . ? S3 U2 N6 116.3(3) . . ? S4 U2 N6 164.4(3) . . ? S2 U2 N6 88.2(3) . . ? O8 U2 N6 132.1(4) . . ? O4 U2 N6 68.0(4) . . ? U1 U2 N6 33.3(3) . . ? O11 U2 N6 168.4(3) . . ? O12 U2 N6 147.5(4) . . ? N5 U2 N6 34.4(4) . . ? N3 U2 N6 45.7(4) . . ? O6 U2 N6 93.6(4) . . ? O2-3 U2 O9 71.3(6) . . ? O1-2 U2 O9 107.7(5) . . ? O7 U2 O9 16.1(5) . . ? N8 U2 O9 125.7(6) . . ? O10 U2 O9 89.2(5) . . ? N7 U2 O9 161.8(5) . . ? O5 U2 O9 84.0(6) . . ? N9 U2 O9 66.4(6) . . ? S3 U2 O9 14.0(3) . . ? S4 U2 O9 91.9(3) . . ? S2 U2 O9 94.8(3) . . ? O8 U2 O9 31.3(4) . . ? C15 U2 O9 59.2(5) . . ? O4 U2 O9 95.5(4) . . ? O11 U2 O9 79.4(3) . . ? O12 U2 O9 109.4(4) . . ? N5 U2 O9 135.8(4) . . ? N3 U2 O9 72.3(4) . . ? O6 U2 O9 108.8(4) . . ? N6 U2 O9 103.1(4) . . ? O3-4 U3 O2-3 156.9(6) . . ? O3-4 U3 O11 102.8(5) . . ? O2-3 U3 O11 81.7(6) . . ? O3-4 U3 N12 90.9(7) . . ? O2-3 U3 N12 93.8(7) . . ? O11 U3 N12 155.2(7) . . ? O3-4 U3 O13 72.5(6) . . ? O2-3 U3 O13 129.7(6) . . ? O11 U3 O13 71.9(6) . . ? N12 U3 O13 93.2(7) . . ? O3-4 U3 N10 76.9(7) . . ? O2-3 U3 N10 82.5(7) . . ? O11 U3 N10 75.6(6) . . ? N12 U3 N10 128.3(8) . . ? O13 U3 N10 128.2(7) . . ? O3-4 U3 N11 84.8(6) . . ? O2-3 U3 N11 76.8(6) . . ? O11 U3 N11 136.3(6) . . ? N12 U3 N11 64.6(7) . . ? O13 U3 N11 148.3(6) . . ? N10 U3 N11 64.3(7) . . ? O3-4 U3 O8 130.2(6) . . ? O2-3 U3 O8 72.8(6) . . ? O11 U3 O8 80.9(6) . . ? N12 U3 O8 74.4(7) . . ? O13 U3 O8 61.5(6) . . ? N10 U3 O8 148.0(6) . . ? N11 U3 O8 126.4(6) . . ? O3-4 U3 S4 118.5(4) . . ? O2-3 U3 S4 64.3(5) . . ? O11 U3 S4 17.4(4) . . ? N12 U3 S4 148.2(5) . . ? O13 U3 S4 85.1(4) . . ? N10 U3 S4 74.1(5) . . ? N11 U3 S4 125.8(5) . . ? O8 U3 S4 77.0(5) . . ? O3-4 U3 S5 59.5(5) . . ? O2-3 U3 S5 143.6(5) . . ? O11 U3 S5 85.4(4) . . ? N12 U3 S5 84.0(5) . . ? O13 U3 S5 16.2(4) . . ? N10 U3 S5 126.8(5) . . ? N11 U3 S5 132.3(5) . . ? O8 U3 S5 71.6(4) . . ? C56 U3 S5 101.6(5) . . ? C46 U3 S5 112.8(5) . . ? C60 U3 S5 68.6(5) . . ? C55 U3 S5 120.6(5) . . ? C50 U3 S5 138.5(5) . . ? C51 U3 S5 139.9(4) . . ? S4 U3 S5 100.03(18) . . ? O3-4 U3 O10 140.6(5) . . ? O2-3 U3 O10 45.3(5) . . ? O11 U3 O10 38.2(4) . . ? N12 U3 O10 127.2(6) . . ? O13 U3 O10 93.5(5) . . ? N10 U3 O10 84.6(6) . . ? N11 U3 O10 117.8(5) . . ? O8 U3 O10 63.6(5) . . ? C56 U3 O10 128.0(5) . . ? C46 U3 O10 75.1(5) . . ? C60 U3 O10 119.0(5) . . ? C55 U3 O10 124.2(5) . . ? C50 U3 O10 94.0(5) . . ? C51 U3 O10 107.9(5) . . ? S4 U3 O10 22.1(3) . . ? S5 U3 O10 109.7(3) . . ? O3-4 U3 S3 140.4(5) . . ? O2-3 U3 S3 62.2(5) . . ? O11 U3 S3 84.2(4) . . ? N12 U3 S3 72.3(6) . . ? O13 U3 S3 73.0(5) . . ? N10 U3 S3 141.5(5) . . ? N11 U3 S3 116.9(5) . . ? O8 U3 S3 11.5(4) . . ? C56 U3 S3 84.8(5) . . ? C46 U3 S3 135.3(5) . . ? C60 U3 S3 59.3(5) . . ? C55 U3 S3 102.4(5) . . ? C50 U3 S3 138.6(5) . . ? C51 U3 S3 129.1(4) . . ? S4 U3 S3 76.90(18) . . ? S5 U3 S3 82.75(18) . . ? O10 U3 S3 60.2(3) . . ? O3-4 U3 O14 39.8(5) . . ? O2-3 U3 O14 162.3(5) . . ? O11 U3 O14 87.3(4) . . ? N12 U3 O14 90.4(6) . . ? O13 U3 O14 32.8(5) . . ? N10 U3 O14 108.2(6) . . ? N11 U3 O14 120.3(5) . . ? O8 U3 O14 91.9(5) . . ? S4 U3 O14 104.3(3) . . ? S5 U3 O14 20.3(3) . . ? O10 U3 O14 120.2(4) . . ? S3 U3 O14 103.1(3) . . ? O3-4 U3 O7 160.5(5) . . ? O2-3 U3 O7 42.2(5) . . ? O11 U3 O7 80.2(4) . . ? N12 U3 O7 80.2(6) . . ? O13 U3 O7 90.6(5) . . ? N10 U3 O7 122.1(5) . . ? N11 U3 O7 106.5(5) . . ? O8 U3 O7 30.7(4) . . ? C56 U3 O7 86.6(5) . . ? C46 U3 O7 120.3(5) . . ? C60 U3 O7 72.5(5) . . ? C55 U3 O7 97.2(5) . . ? C50 U3 O7 118.8(5) . . ? C51 U3 O7 113.5(5) . . ? S4 U3 O7 68.0(3) . . ? S5 U3 O7 102.1(3) . . ? O10 U3 O7 47.5(3) . . ? S3 U3 O7 20.2(3) . . ? O14 U3 O7 122.3(4) . . ? O3-4 U3 O15 66.1(5) . . ? O2-3 U3 O15 136.0(5) . . ? O11 U3 O15 101.0(5) . . ? N12 U3 O15 65.6(6) . . ? O13 U3 O15 29.1(5) . . ? N10 U3 O15 141.2(6) . . ? N11 U3 O15 120.8(5) . . ? O8 U3 O15 64.5(5) . . ? S4 U3 O15 113.4(3) . . ? S5 U3 O15 18.8(3) . . ? O10 U3 O15 117.0(4) . . ? S3 U3 O15 74.3(3) . . ? O14 U3 O15 33.5(4) . . ? O7 U3 O15 94.4(4) . . ? O3-4 U3 O12 110.2(5) . . ? O2-3 U3 O12 65.6(5) . . ? O11 U3 O12 24.1(5) . . ? N12 U3 O12 158.6(6) . . ? O13 U3 O12 96.0(5) . . ? N10 U3 O12 57.6(6) . . ? N11 U3 O12 112.9(5) . . ? O8 U3 O12 93.1(5) . . ? S4 U3 O12 16.6(3) . . ? S5 U3 O12 109.0(3) . . ? O10 U3 O12 33.0(4) . . ? S3 U3 O12 92.1(3) . . ? O14 U3 O12 107.7(4) . . ? O7 U3 O12 80.4(3) . . ? O15 U3 O12 125.1(4) . . ? O3-4 U3 N17 32.6(5) . . ? O2-3 U3 N17 132.8(6) . . ? O11 U3 N17 133.3(4) . . ? N12 U3 N17 66.1(6) . . ? O13 U3 N17 95.1(5) . . ? N10 U3 N17 79.2(6) . . ? N11 U3 N17 56.0(5) . . ? O8 U3 N17 132.7(5) . . ? S4 U3 N17 145.8(3) . . ? S5 U3 N17 79.2(3) . . ? O10 U3 N17 163.7(4) . . ? S3 U3 N17 135.9(3) . . ? O14 U3 N17 64.3(4) . . ? O7 U3 N17 146.0(4) . . ? O15 U3 N17 75.9(4) . . ? O12 U3 N17 131.9(4) . . ? O3-4 U3 N13 34.5(5) . . ? O2-3 U3 N13 142.4(5) . . ? O11 U3 N13 68.4(4) . . ? N12 U3 N13 122.9(6) . . ? O13 U3 N13 62.3(5) . . ? N10 U3 N13 68.7(6) . . ? N11 U3 N13 109.4(5) . . ? O8 U3 N13 121.7(5) . . ? S4 U3 N13 84.3(3) . . ? S5 U3 N13 58.1(3) . . ? O10 U3 N13 106.3(4) . . ? S3 U3 N13 132.6(3) . . ? O14 U3 N13 40.7(4) . . ? O7 U3 N13 143.2(4) . . ? O15 U3 N13 74.1(4) . . ? O12 U3 N13 78.4(4) . . ? N17 U3 N13 66.1(4) . . ? O3-4 U3 N18 29.3(5) . . ? O2-3 U3 N18 127.6(6) . . ? O11 U3 N18 102.6(4) . . ? N12 U3 N18 99.5(6) . . ? O13 U3 N18 100.0(5) . . ? N10 U3 N18 50.0(5) . . ? N11 U3 N18 64.4(5) . . ? O8 U3 N18 159.5(5) . . ? S4 U3 N18 112.1(3) . . ? S5 U3 N18 88.4(3) . . ? O10 U3 N18 130.4(4) . . ? S3 U3 N18 168.5(3) . . ? O14 U3 N18 68.3(4) . . ? O7 U3 N18 169.4(4) . . ? O15 U3 N18 95.1(4) . . ? O12 U3 N18 97.9(4) . . ? N17 U3 N18 34.0(4) . . ? N13 U3 N18 45.1(4) . . ? O3-4 U3 N9 147.2(5) . . ? O2-3 U3 N9 28.6(5) . . ? O11 U3 N9 107.9(4) . . ? N12 U3 N9 65.2(5) . . ? O13 U3 N9 128.0(5) . . ? N10 U3 N9 99.9(6) . . ? N11 U3 N9 65.1(5) . . ? O8 U3 N9 67.1(5) . . ? S4 U3 N9 91.0(3) . . ? S5 U3 N9 133.4(3) . . ? O10 U3 N9 69.8(3) . . ? S3 U3 N9 55.7(3) . . ? O14 U3 N9 150.7(4) . . ? O7 U3 N9 41.4(4) . . ? O15 U3 N9 117.4(4) . . ? O12 U3 N9 94.1(3) . . ? N17 U3 N9 114.7(4) . . ? N13 U3 N9 168.4(4) . . ? N18 U3 N9 128.8(4) . . ? O3-4 U4 O16 142.4(6) . . ? O3-4 U4 O14 73.7(6) . . ? O16 U4 O14 68.7(6) . . ? O3-4 U4 N16 92.8(7) . . ? O16 U4 N16 77.4(7) . . ? O14 U4 N16 73.7(7) . . ? O3-4 U4 N13 80.4(7) . . ? O16 U4 N13 87.9(7) . . ? O14 U4 N13 72.5(7) . . ? N16 U4 N13 146.1(8) . . ? O3-4 U4 N17 76.9(6) . . ? O16 U4 N17 126.7(7) . . ? O14 U4 N17 125.8(7) . . ? N16 U4 N17 63.4(8) . . ? N13 U4 N17 143.8(7) . . ? O3-4 U4 N18 79.1(7) . . ? O16 U4 N18 136.0(7) . . ? O14 U4 N18 147.6(6) . . ? N16 U4 N18 125.5(8) . . ? N13 U4 N18 86.1(7) . . ? N17 U4 N18 62.3(7) . . ? O3-4 U4 N14 132.3(6) . . ? O16 U4 N14 68.1(6) . . ? O14 U4 N14 116.6(6) . . ? N16 U4 N14 134.8(7) . . ? N13 U4 N14 62.0(7) . . ? N17 U4 N14 116.9(7) . . ? N18 U4 N14 70.6(7) . . ? O3-4 U4 N15 144.7(6) . . ? O16 U4 N15 69.7(7) . . ? O14 U4 N15 134.1(6) . . ? N16 U4 N15 79.3(7) . . ? N13 U4 N15 124.1(7) . . ? N17 U4 N15 68.8(7) . . ? N18 U4 N15 78.0(7) . . ? N14 U4 N15 62.2(6) . . ? O3-4 U4 C76 99.5(7) . . ? O3-4 U4 S5 59.2(5) . . ? O16 U4 S5 83.5(5) . . ? O14 U4 S5 16.2(4) . . ? N16 U4 S5 69.6(6) . . ? N13 U4 S5 78.6(5) . . ? N17 U4 S5 112.0(5) . . ? N18 U4 S5 137.2(5) . . ? N14 U4 S5 131.0(5) . . ? N15 U4 S5 142.7(5) . . ? O3-4 U4 S6 147.8(5) . . ? O16 U4 S6 6.1(5) . . ? O14 U4 S6 74.2(4) . . ? N16 U4 S6 81.1(6) . . ? N13 U4 S6 87.2(5) . . ? N17 U4 S6 126.0(5) . . ? N18 U4 S6 129.9(5) . . ? N14 U4 S6 62.5(5) . . ? N15 U4 S6 65.4(5) . . ? S5 U4 S6 89.3(2) . . ? O3-4 U4 O13 39.9(5) . . ? O16 U4 O13 102.5(5) . . ? O14 U4 O13 33.9(5) . . ? N16 U4 O13 81.9(6) . . ? N13 U4 O13 71.6(6) . . ? N17 U4 O13 105.8(6) . . ? N18 U4 O13 116.6(5) . . ? N14 U4 O13 132.6(5) . . ? N15 U4 O13 160.7(5) . . ? S5 U4 O13 20.6(3) . . ? S6 U4 O13 107.9(3) . . ? O3-4 U4 O15 63.5(5) . . ? O16 U4 O15 82.7(5) . . ? O14 U4 O15 27.6(5) . . ? N16 U4 O15 51.9(6) . . ? N13 U4 O15 96.4(6) . . ? N17 U4 O15 98.2(6) . . ? N18 U4 O15 141.4(6) . . ? N14 U4 O15 143.2(6) . . ? N15 U4 O15 128.3(5) . . ? S5 U4 O15 17.8(3) . . ? S6 U4 O15 88.7(3) . . ? O13 U4 O15 32.6(4) . . ? U3 U4 O15 59.4(3) . . ? O3-4 U4 O18 159.9(6) . . ? O16 U4 O18 24.3(6) . . ? O14 U4 O18 90.1(6) . . ? N16 U4 O18 94.1(7) . . ? N13 U4 O18 83.3(7) . . ? N17 U4 O18 123.0(7) . . ? N18 U4 O18 111.7(7) . . ? N14 U4 O18 45.3(6) . . ? N15 U4 O18 55.4(6) . . ? S5 U4 O18 105.9(5) . . ? S6 U4 O18 18.3(4) . . ? O13 U4 O18 122.8(5) . . ? O15 U4 O18 106.9(5) . . ? O3-4 U4 N10 30.0(5) . . ? O16 U4 N10 155.4(5) . . ? O14 U4 N10 96.4(5) . . ? N16 U4 N10 118.4(6) . . ? N13 U4 N10 68.5(6) . . ? N17 U4 N10 77.8(6) . . ? N18 U4 N10 52.4(6) . . ? N14 U4 N10 104.6(5) . . ? N15 U4 N10 129.2(6) . . ? S5 U4 N10 84.8(3) . . ? S6 U4 N10 155.7(3) . . ? O13 U4 N10 64.2(4) . . ? O15 U4 N10 92.6(4) . . ? O18 U4 N10 147.4(5) . . ? O3-4 U4 O17 143.7(7) . . ? O16 U4 O17 13.2(6) . . ? O14 U4 O17 72.3(6) . . ? N16 U4 O17 65.7(7) . . ? N13 U4 O17 101.0(7) . . ? N17 U4 O17 114.0(7) . . ? N18 U4 O17 137.1(7) . . ? N14 U4 O17 75.7(6) . . ? N15 U4 O17 62.9(7) . . ? S5 U4 O17 85.3(5) . . ? S6 U4 O17 15.5(5) . . ? O13 U4 O17 105.6(5) . . ? O15 U4 O17 80.4(5) . . ? O18 U4 O17 30.5(6) . . ? N10 U4 O17 166.9(6) . . ? O3 S1 O1 114.8(13) . . ? O3 S1 O2 118.0(14) . . ? O1 S1 O2 110.9(14) . . ? O3 S1 C91 113(3) . . ? O1 S1 C91 102(3) . . ? O2 S1 C91 95(3) . . ? O6 S2 O4 115.3(12) . . ? O6 S2 O5 116.9(13) . . ? O4 S2 O5 112.4(11) . . ? O6 S2 C92 105.6(16) . . ? O4 S2 C92 101.4(15) . . ? O5 S2 C92 102.7(16) . . ? O9 S3 O8 117.4(13) . . ? O9 S3 O7 113.4(13) . . ? O8 S3 O7 111.5(11) . . ? O9 S3 C93 106.7(18) . . ? O8 S3 C93 103.4(17) . . ? O7 S3 C93 102.7(16) . . ? O12 S4 O10 115.7(12) . . ? O12 S4 O11 113.8(11) . . ? O10 S4 O11 113.4(9) . . ? O12 S4 C94 110.7(16) . . ? O10 S4 C94 102.3(16) . . ? O11 S4 C94 99.0(15) . . ? O15 S5 O13 113.9(13) . . ? O15 S5 O14 115.9(12) . . ? O13 S5 O14 113.6(12) . . ? O15 S5 C95 107.2(16) . . ? O13 S5 C95 102.4(15) . . ? O14 S5 C95 101.7(15) . . ? O17 S6 O18 118(2) . . ? O17 S6 O16 108(2) . . ? O18 S6 O16 114.1(18) . . ? O17 S6 C96 107(3) . . ? O18 S6 C96 108(2) . . ? O16 S6 C96 101(2) . . ? O20 S7 O21 114.9(15) . . ? O20 S7 O19 114.5(15) . . ? O21 S7 O19 116.8(14) . . ? O20 S7 C97 102(2) . . ? O21 S7 C97 103(2) . . ? O19 S7 C97 103(2) . . ? O24 S8 O22 115.3(15) . . ? O24 S8 O23 114.1(14) . . ? O22 S8 O23 115.6(14) . . ? O24 S8 C98 105.7(16) . . ? O22 S8 C98 100.5(16) . . ? O23 S8 C98 103.4(16) . . ? O26 S9 O27 118.1(13) . . ? O26 S9 O25 113.9(15) . . ? O27 S9 O25 114.0(13) . . ? O26 S9 C99 103.8(16) . . ? O27 S9 C99 101.9(17) . . ? O25 S9 C99 102.2(16) . . ? O28 S10 O29 125.1(19) . . ? O28 S10 O30 108.1(18) . . ? O29 S10 O30 107.2(17) . . ? O28 S10 C100 107.4(19) . . ? O29 S10 C100 111.1(18) . . ? O30 S10 C100 93.2(19) . . ? S1 O1 U1 148.8(11) . . ? S1 O2 U1 53.3(8) . . ? S1 O3 U1 58.4(9) . . ? S2 O4 U1 136.1(11) . . ? S2 O4 U2 66.8(7) . . ? U1 O4 U2 73.9(4) . . ? S2 O5 U2 137.4(12) . . ? S2 O5 U1 66.2(7) . . ? U2 O5 U1 75.0(4) . . ? S2 O5 U3 171.1(11) . . ? U1 O5 U3 113.0(4) . . ? S2 O6 U1 50.7(8) . . ? S2 O6 U2 49.6(8) . . ? U1 O6 U2 55.6(2) . . ? S3 O7 U2 137.8(11) . . ? S3 O7 U3 67.0(7) . . ? U2 O7 U3 70.9(4) . . ? S3 O7 U1 167.4(9) . . ? U2 O7 U1 53.1(3) . . ? U3 O7 U1 122.8(4) . . ? S3 O8 U3 146.8(11) . . ? S3 O8 U2 73.2(7) . . ? U3 O8 U2 77.4(4) . . ? S3 O8 U4 166.7(11) . . ? U2 O8 U4 111.1(4) . . ? S3 O9 U3 45.6(8) . . ? U2 O9 U3 52.1(2) . . ? S4 O10 U2 139.7(11) . . ? S4 O10 U3 70.9(6) . . ? U2 O10 U3 77.0(4) . . ? S4 O10 U1 160.7(10) . . ? U3 O10 U1 111.1(3) . . ? S4 O11 U3 132.3(9) . . ? S4 O11 U2 62.6(6) . . ? U3 O11 U2 70.4(3) . . ? S4 O11 U4 164.4(9) . . ? U3 O11 U4 50.5(3) . . ? U2 O11 U4 120.1(3) . . ? U1 O1-2 U2 172.2(9) . . ? S4 O12 U2 53.6(7) . . ? S4 O12 U3 46.3(7) . . ? U2 O12 U3 54.9(2) . . ? S5 O13 U3 133.9(11) . . ? S5 O13 U4 65.7(8) . . ? U3 O13 U4 75.7(4) . . ? S5 O13 U2 161.4(10) . . ? U4 O13 U2 113.7(4) . . ? S5 O14 U4 133.9(11) . . ? S5 O14 U3 63.2(7) . . ? U4 O14 U3 74.6(4) . . ? S5 O15 U3 56.9(8) . . ? S5 O15 U4 53.2(8) . . ? U3 O15 U4 58.5(3) . . ? S6 O16 U4 164.2(13) . . ? S6 O17 U4 51.4(15) . . ? S6 O18 U4 57.2(13) . . ? S8 O22 U4 145.7(12) . 2_646 ? U2 O2-3 U3 158.7(9) . . ? S10 O28 U4 150.7(16) . 3_676 ? S10 O29 U1 151.6(13) . 2_646 ? U4 O3-4 U3 171.6(9) . . ? C5 N1 C1 117(3) . . ? C5 N1 U1 121(2) . . ? C1 N1 U1 119.6(18) . . ? C10 N2 C6 122(2) . . ? C10 N2 U1 119.9(17) . . ? C6 N2 U1 118.5(18) . . ? C15 N3 C11 118(3) . . ? C15 N3 U1 117.5(19) . . ? C11 N3 U1 123.5(18) . . ? C15 N3 U2 61.7(17) . . ? C11 N3 U2 157.7(17) . . ? U1 N3 U2 66.0(5) . . ? C16 N4 C20 120(2) . . ? C16 N4 U1 120.5(18) . . ? C20 N4 U1 119.3(16) . . ? C16 N4 U2 120.5(15) . . ? C20 N4 U2 86.1(13) . . ? U1 N4 U2 56.9(4) . . ? C25 N5 C21 121(2) . . ? C25 N5 U1 121.0(18) . . ? C21 N5 U1 117.7(17) . . ? C25 N5 U2 102.0(16) . . ? C21 N5 U2 98.1(14) . . ? U1 N5 U2 67.3(5) . . ? C30 N6 C26 114(2) . . ? C30 N6 U1 122.4(19) . . ? C26 N6 U1 123.1(18) . . ? C30 N6 U2 108.9(16) . . ? C26 N6 U2 101.5(16) . . ? U1 N6 U2 63.9(4) . . ? C35 N7 C31 123(2) . . ? C35 N7 U2 118.1(17) . . ? C31 N7 U2 119.1(18) . . ? C35 N7 U1 111.4(16) . . ? C31 N7 U1 101.7(15) . . ? U2 N7 U1 59.6(4) . . ? C35 N7 U3 95.6(15) . . ? C31 N7 U3 116.4(15) . . ? U2 N7 U3 49.9(3) . . ? U1 N7 U3 109.1(4) . . ? C36 N8 C40 116(2) . . ? C36 N8 U2 123.0(17) . . ? C40 N8 U2 120.7(18) . . ? C36 N8 U3 109.2(15) . . ? C40 N8 U3 98.4(15) . . ? U2 N8 U3 59.8(4) . . ? C36 N8 U1 112.3(15) . . ? C40 N8 U1 101.7(16) . . ? U2 N8 U1 59.8(4) . . ? U3 N8 U1 118.4(5) . . ? C45 N9 C41 118(2) . . ? C45 N9 U2 121.5(19) . . ? C41 N9 U2 120.8(16) . . ? C45 N9 U1 100.2(16) . . ? C41 N9 U1 110.1(14) . . ? U2 N9 U1 64.7(4) . . ? C45 N9 U3 104.8(16) . . ? C41 N9 U3 99.6(13) . . ? U2 N9 U3 61.1(4) . . ? U1 N9 U3 125.7(4) . . ? C46 N10 C50 122(3) . . ? C46 N10 U3 119(2) . . ? C50 N10 U3 119.6(17) . . ? C46 N10 U4 95.6(16) . . ? C50 N10 U4 109.8(15) . . ? U3 N10 U4 65.6(4) . . ? C46 N10 U2 110.1(17) . . ? C50 N10 U2 97.2(15) . . ? U3 N10 U2 59.1(4) . . ? U4 N10 U2 124.7(5) . . ? C55 N11 C51 119(2) . . ? C55 N11 U3 120.3(19) . . ? C51 N11 U3 120.2(16) . . ? C55 N11 U2 106.4(16) . . ? C51 N11 U2 101.2(14) . . ? U3 N11 U2 60.0(4) . . ? C55 N11 U4 110.3(15) . . ? C51 N11 U4 100.6(14) . . ? U3 N11 U4 59.9(4) . . ? U2 N11 U4 119.2(4) . . ? C56 N12 C60 119(2) . . ? C56 N12 U3 119.2(18) . . ? C60 N12 U3 121.2(19) . . ? C56 N12 U4 108.1(17) . . ? C60 N12 U4 108.0(16) . . ? U3 N12 U4 59.1(4) . . ? C56 N12 U2 97.4(16) . . ? C60 N12 U2 111.5(16) . . ? U3 N12 U2 53.8(4) . . ? U4 N12 U2 112.5(4) . . ? C61 N13 C65 115(2) . . ? C61 N13 U4 122(2) . . ? C65 N13 U4 122.3(18) . . ? C61 N13 U3 63.8(17) . . ? C65 N13 U3 155.0(17) . . ? U4 N13 U3 65.6(5) . . ? C70 N14 C66 119(2) . . ? C70 N14 U4 119.1(17) . . ? C66 N14 U4 121.9(17) . . ? C75 N15 C71 119(2) . . ? C75 N15 U4 119.8(18) . . ? C71 N15 U4 120.8(17) . . ? C80 N16 C76 118(3) . . ? C80 N16 U4 122(2) . . ? C76 N16 U4 119(2) . . ? C80 N16 U3 85.6(17) . . ? C76 N16 U3 118.6(19) . . ? U4 N16 U3 58.0(4) . . ? C85 N17 C81 120(3) . . ? C85 N17 U4 122.2(18) . . ? C81 N17 U4 117.4(19) . . ? C85 N17 U3 104.1(16) . . ? C81 N17 U3 96.8(16) . . ? U4 N17 U3 66.4(5) . . ? C86 N18 C90 119(3) . . ? C86 N18 U4 118.9(18) . . ? C90 N18 U4 121.6(19) . . ? C86 N18 U3 98.3(16) . . ? C90 N18 U3 106.6(15) . . ? U4 N18 U3 63.2(5) . . ? C107 N30 C103 129(4) . . ? N1 C1 C2 120(3) . . ? C3 C2 C1 122(3) . . ? C2 C3 C4 112(4) . . ? C5 C4 C3 124(4) . . ? N1 C5 C4 124(3) . . ? N1 C5 C6 117(3) . . ? C4 C5 C6 118(3) . . ? N2 C6 C7 118(3) . . ? N2 C6 C5 118(3) . . ? C7 C6 C5 123(3) . . ? C8 C7 C6 121(3) . . ? C7 C8 C9 121(3) . . ? C8 C9 C10 116(3) . . ? N2 C10 C11 117(2) . . ? N2 C10 C9 121(3) . . ? C11 C10 C9 122(3) . . ? N3 C11 C12 125(3) . . ? N3 C11 C10 117(3) . . ? C12 C11 C10 118(3) . . ? C11 C12 C13 115(4) . . ? C12 C13 C14 122(4) . . ? C15 C14 C13 116(4) . . ? N3 C15 C14 123(3) . . ? N4 C16 C17 120(3) . . ? C18 C17 C16 120(3) . . ? C17 C18 C19 119(3) . . ? C20 C19 C18 117(3) . . ? N4 C20 C19 123(3) . . ? N4 C20 C21 118(2) . . ? C19 C20 C21 118(3) . . ? C20 C21 N5 119(2) . . ? C20 C21 C22 126(2) . . ? N5 C21 C22 115(2) . . ? C23 C22 C21 121(3) . . ? C22 C23 C24 126(3) . . ? C23 C24 C25 112(3) . . ? N5 C25 C24 125(3) . . ? N5 C25 C26 119(3) . . ? C24 C25 C26 116(3) . . ? N6 C26 C27 124(3) . . ? N6 C26 C25 113(3) . . ? C27 C26 C25 123(3) . . ? C26 C27 C28 117(3) . . ? C29 C28 C27 121(3) . . ? C28 C29 C30 117(3) . . ? N6 C30 C29 126(3) . . ? N7 C31 C32 120(3) . . ? C33 C32 C31 121(3) . . ? C32 C33 C34 119(3) . . ? C33 C34 C35 119(3) . . ? N7 C35 C34 118(3) . . ? N7 C35 C36 121(2) . . ? C34 C35 C36 120(3) . . ? N8 C36 C37 123(2) . . ? N8 C36 C35 113(2) . . ? C37 C36 C35 125(2) . . ? C38 C37 C36 118(3) . . ? C37 C38 C39 121(3) . . ? C38 C39 C40 118(3) . . ? N8 C40 C39 125(3) . . ? N8 C40 C41 119(3) . . ? C39 C40 C41 116(2) . . ? N9 C41 C42 121(2) . . ? N9 C41 C40 114(2) . . ? C42 C41 C40 125(3) . . ? C41 C42 C43 121(3) . . ? C44 C43 C42 118(3) . . ? C43 C44 C45 117(3) . . ? N9 C45 C44 125(3) . . ? N10 C46 C47 120(3) . . ? C48 C47 C46 118(3) . . ? C47 C48 C49 123(3) . . ? C50 C49 C48 117(3) . . ? N10 C50 C49 119(3) . . ? N10 C50 C51 118(2) . . ? C49 C50 C51 123(3) . . ? C52 C51 N11 121(2) . . ? C52 C51 C50 121(3) . . ? N11 C51 C50 118(2) . . ? C51 C52 C53 121(3) . . ? C52 C53 C54 120(3) . . ? C53 C54 C55 117(3) . . ? N11 C55 C54 121(3) . . ? N11 C55 C56 115(3) . . ? C54 C55 C56 124(3) . . ? N12 C56 C57 120(3) . . ? N12 C56 C55 120(3) . . ? C57 C56 C55 120(3) . . ? C58 C57 C56 117(3) . . ? C57 C58 C59 124(3) . . ? C60 C59 C58 116(3) . . ? N12 C60 C59 124(3) . . ? N13 C61 C62 128(3) . . ? C63 C62 C61 113(3) . . ? C64 C63 C62 124(4) . . ? C63 C64 C65 119(3) . . ? N13 C65 C64 121(3) . . ? N13 C65 C66 118(2) . . ? C64 C65 C66 121(3) . . ? N14 C66 C67 120(3) . . ? N14 C66 C65 116(2) . . ? C67 C66 C65 123(3) . . ? C68 C67 C66 119(3) . . ? C69 C68 C67 121(3) . . ? C68 C69 C70 120(3) . . ? N14 C70 C69 120(3) . . ? N14 C70 C71 122(3) . . ? C69 C70 C71 118(3) . . ? C72 C71 N15 120(3) . . ? C72 C71 C70 124(3) . . ? N15 C71 C70 116(2) . . ? C71 C72 C73 124(3) . . ? C72 C73 C74 118(3) . . ? C73 C74 C75 118(3) . . ? N15 C75 C74 121(3) . . ? N16 C76 C77 124(3) . . ? C78 C77 C76 117(4) . . ? C77 C78 C79 122(4) . . ? C78 C79 C80 114(3) . . ? N16 C80 C79 125(3) . . ? N16 C80 C81 117(3) . . ? C79 C80 C81 118(3) . . ? C82 C81 N17 118(3) . . ? C82 C81 C80 124(3) . . ? N17 C81 C80 117(3) . . ? C83 C82 C81 123(3) . . ? C82 C83 C84 116(3) . . ? C85 C84 C83 121(3) . . ? N17 C85 C84 121(3) . . ? N17 C85 C86 114(3) . . ? C84 C85 C86 125(3) . . ? N18 C86 C87 119(2) . . ? N18 C86 C85 122(3) . . ? C87 C86 C85 118(3) . . ? C88 C87 C86 119(3) . . ? C89 C88 C87 122(3) . . ? C88 C89 C90 114(3) . . ? N18 C90 C89 125(3) . . ? F1 C91 F3 113(7) . . ? F1 C91 F2 108(6) . . ? F3 C91 F2 112(6) . . ? F1 C91 S1 113(6) . . ? F3 C91 S1 103(5) . . ? F2 C91 S1 106(5) . . ? F6 C92 F4 106(3) . . ? F6 C92 F5 103(3) . . ? F4 C92 F5 102(3) . . ? F6 C92 S2 116(3) . . ? F4 C92 S2 114(3) . . ? F5 C92 S2 114(3) . . ? F7 C93 F8 109(4) . . ? F7 C93 F9 107(4) . . ? F8 C93 F9 109(4) . . ? F7 C93 S3 110(3) . . ? F8 C93 S3 113(3) . . ? F9 C93 S3 108(3) . . ? F11 C94 F10 114(4) . . ? F11 C94 F12 109(4) . . ? F10 C94 F12 99(3) . . ? F11 C94 S4 123(3) . . ? F10 C94 S4 106(3) . . ? F12 C94 S4 104(3) . . ? F15 C95 F14 110(3) . . ? F15 C95 F13 111(3) . . ? F14 C95 F13 109(3) . . ? F15 C95 S5 111(3) . . ? F14 C95 S5 109(3) . . ? F13 C95 S5 107(3) . . ? F17 C96 F16 118(6) . . ? F17 C96 F18 111(6) . . ? F16 C96 F18 111(5) . . ? F17 C96 S6 107(5) . . ? F16 C96 S6 108(4) . . ? F18 C96 S6 101(4) . . ? F19 C97 F20 112(4) . . ? F19 C97 F21 104(4) . . ? F20 C97 F21 103(4) . . ? F19 C97 S7 114(4) . . ? F20 C97 S7 111(3) . . ? F21 C97 S7 112(3) . . ? F24 C98 F23 109(3) . . ? F24 C98 F22 104(3) . . ? F23 C98 F22 106(3) . . ? F24 C98 S8 114(3) . . ? F23 C98 S8 113(3) . . ? F22 C98 S8 109(3) . . ? F25 C99 F26 109(3) . . ? F25 C99 F27 101(3) . . ? F26 C99 F27 108(3) . . ? F25 C99 S9 114(3) . . ? F26 C99 S9 113(3) . . ? F27 C99 S9 110(3) . . ? F29 C100 F28 106(3) . . ? F29 C100 F30 91(3) . . ? F28 C100 F30 91(3) . . ? F29 C100 S10 126(3) . . ? F28 C100 S10 122(3) . . ? F30 C100 S10 109(3) . . ? N19 C101 C102 165(8) . . ? N30 C103 C104 107(5) . . ? C105 C104 C103 116(6) . . ? C104 C105 C106 130(7) . . ? C107 C106 C105 107(7) . . ? C106 C107 N30 129(6) . . ?