data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Jonathan L. Sessler' _publ_contact_author_address ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; _publ_contact_author_email sessler@mail.utexas.edu _publ_contact_author_phone 0015124715009 _publ_contact_author_fax 0015124717550 loop_ _publ_author_name _publ_author_address P.J.Melfi ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; S.Camiolo ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; J.T.Lee ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; M.Ali ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; J.T.McDevitt ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; V.M.Lynch ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; ; J.L.Sessler ; ;The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78712 ; data_meoameth _database_code_depnum_ccdc_archive 'CCDC 661301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C48 H60 N6 O4 2+, 2 Cl 1-, 1/2 H2 O ' _chemical_formula_sum 'C48 H61 Cl2 N6 O4.50' _chemical_formula_weight 864.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 25.8233(3) _cell_length_b 10.4391(10) _cell_length_c 33.9936(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9163.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8791 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25.0 _exptl_crystal_description laths _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3688 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8068 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1920 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8068 _reflns_number_gt 3399 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A partial occupancy atom near Cl2 and O1 was refined as a half occupancy oxygen atom of a water molecule. The hydrogen atoms from this molecule could not be located in the difference electron density map and were excluded from the refinement model. ; _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^)+(0.0440P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00075(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8068 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2221 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.33011(4) 0.64877(10) 0.59429(3) 0.0454(4) Uani 1 1 d . . . Cl2 Cl 0.45422(4) 0.78617(10) 0.57974(4) 0.0494(4) Uani 1 1 d . . . O1 O 0.5266(2) 0.8402(5) 0.70373(14) 0.1151(17) Uani 1 1 d . . . O2 O 0.5827(2) 0.7410(6) 0.66523(17) 0.144(2) Uani 1 1 d . . . O3 O 0.3104(2) 0.4873(5) 0.81001(17) 0.161(2) Uani 1 1 d . . . O4 O 0.31591(19) 0.3214(5) 0.77228(15) 0.123(2) Uani 1 1 d . . . N1 N 0.34348(13) 0.9857(3) 0.60304(12) 0.0386(10) Uani 1 1 d . . . H1A H 0.3532 0.9049 0.6023 0.046 Uiso 1 1 calc R . . N2 N 0.35571(13) 0.8926(3) 0.52540(11) 0.0366(10) Uani 1 1 d . . . H2A H 0.3799 0.8617 0.5410 0.044 Uiso 1 1 calc R . . N3 N 0.37978(12) 0.6422(3) 0.50601(10) 0.0342(9) Uani 1 1 d . . . H3A H 0.3747 0.6542 0.5313 0.041 Uiso 1 1 calc R . . N4 N 0.43034(13) 0.4606(3) 0.55282(12) 0.0394(10) Uani 1 1 d . . . H4A H 0.4284 0.5367 0.5639 0.047 Uiso 1 1 calc R . . N5 N 0.42676(13) 0.5356(3) 0.64331(11) 0.0380(10) Uani 1 1 d . . . H5A H 0.4048 0.5606 0.6251 0.046 Uiso 1 1 calc R . . N6 N 0.39775(13) 0.8121(3) 0.66699(11) 0.0417(10) Uani 1 1 d . . . H6A H 0.4079 0.8202 0.6424 0.050 Uiso 1 1 calc R . . C1 C 0.34251(16) 1.0622(4) 0.63656(16) 0.0396(12) Uani 1 1 d . . . C2 C 0.32545(15) 1.1869(4) 0.62434(15) 0.0377(12) Uani 1 1 d . . . C3 C 0.31673(16) 1.1834(4) 0.58472(15) 0.0384(12) Uani 1 1 d . . . C4 C 0.32700(16) 1.0558(4) 0.57163(15) 0.0370(12) Uani 1 1 d . . . C5 C 0.32420(17) 0.9972(4) 0.53370(14) 0.0329(11) Uani 1 1 d . . . C6 C 0.29138(17) 1.0143(4) 0.50197(14) 0.0370(12) Uani 1 1 d . . . C7 C 0.30292(17) 0.9203(4) 0.47376(14) 0.0366(12) Uani 1 1 d . . . C8 C 0.34290(16) 0.8457(4) 0.48896(14) 0.0345(11) Uani 1 1 d . . . C9 C 0.36723(16) 0.7275(4) 0.47706(14) 0.0323(11) Uani 1 1 d . . . C10 C 0.38264(16) 0.6753(4) 0.44138(13) 0.0343(11) Uani 1 1 d . . . C11 C 0.40435(17) 0.5535(4) 0.44894(14) 0.0379(12) Uani 1 1 d . . . C12 C 0.40180(16) 0.5337(4) 0.48933(15) 0.0352(12) Uani 1 1 d . . . C13 C 0.41890(16) 0.4354(4) 0.51461(15) 0.0361(12) Uani 1 1 d . . . C14 C 0.42523(16) 0.3007(4) 0.50875(14) 0.0362(12) Uani 1 1 d . . . C15 C 0.44294(15) 0.2487(4) 0.54348(14) 0.0329(11) Uani 1 1 d . . . C16 C 0.44550(16) 0.3491(4) 0.57189(15) 0.0356(11) Uani 1 1 d . . . C17 C 0.45894(16) 0.3368(4) 0.61064(15) 0.0382(12) Uani 1 1 d . . . H17A H 0.4716 0.2545 0.6177 0.046 Uiso 1 1 calc R . . C18 C 0.45714(18) 0.4257(4) 0.64185(14) 0.0390(12) Uani 1 1 d . . . C19 C 0.48713(18) 0.4233(4) 0.67637(15) 0.0435(13) Uani 1 1 d . . . C20 C 0.47542(18) 0.5333(4) 0.69809(13) 0.0427(13) Uani 1 1 d . . . C21 C 0.43663(18) 0.5980(4) 0.67760(15) 0.0420(13) Uani 1 1 d . . . C22 C 0.40625(18) 0.7087(4) 0.69016(15) 0.0433(13) Uani 1 1 d . . . C23 C 0.38203(17) 0.7292(4) 0.72641(14) 0.0416(12) Uani 1 1 d . . . C24 C 0.36115(17) 0.8507(4) 0.72515(15) 0.0414(12) Uani 1 1 d . . . C25 C 0.37063(17) 0.9030(4) 0.68825(15) 0.0414(12) Uani 1 1 d . . . C26 C 0.35271(17) 1.0221(4) 0.67390(15) 0.0457(13) Uani 1 1 d . . . H26A H 0.3468 1.0849 0.6936 0.055 Uiso 1 1 calc R . . C27 C 0.31875(17) 1.2994(4) 0.65080(14) 0.0487(13) Uani 1 1 d . . . H27A H 0.3254 1.3790 0.6358 0.058 Uiso 1 1 calc R . . H27B H 0.3444 1.2947 0.6724 0.058 Uiso 1 1 calc R . . C28 C 0.26442(19) 1.3046(4) 0.66817(15) 0.0729(17) Uani 1 1 d . . . H28A H 0.2389 1.3060 0.6468 0.109 Uiso 1 1 calc R . . H28B H 0.2608 1.3822 0.6842 0.109 Uiso 1 1 calc R . . H28C H 0.2586 1.2290 0.6847 0.109 Uiso 1 1 calc R . . C29 C 0.30132(17) 1.2943(4) 0.55922(13) 0.0501(13) Uani 1 1 d . . . H29A H 0.2635 1.3008 0.5584 0.075 Uiso 1 1 calc R . . H29B H 0.3146 1.2810 0.5325 0.075 Uiso 1 1 calc R . . H29C H 0.3158 1.3736 0.5700 0.075 Uiso 1 1 calc R . . C30 C 0.24520(17) 1.1015(4) 0.49942(13) 0.0486(13) Uani 1 1 d . . . H30A H 0.2323 1.1195 0.5260 0.073 Uiso 1 1 calc R . . H30B H 0.2179 1.0599 0.4840 0.073 Uiso 1 1 calc R . . H30C H 0.2553 1.1819 0.4867 0.073 Uiso 1 1 calc R . . C31 C 0.27321(18) 0.8977(4) 0.43679(13) 0.0492(14) Uani 1 1 d . . . H31A H 0.2358 0.8954 0.4431 0.059 Uiso 1 1 calc R . . H31B H 0.2829 0.8129 0.4260 0.059 Uiso 1 1 calc R . . C32 C 0.2827(2) 1.0002(5) 0.40524(15) 0.0719(17) Uani 1 1 d . . . H32A H 0.2724 1.0842 0.4154 0.108 Uiso 1 1 calc R . . H32B H 0.2623 0.9800 0.3818 0.108 Uiso 1 1 calc R . . H32C H 0.3196 1.0018 0.3984 0.108 Uiso 1 1 calc R . . C33 C 0.38150(16) 0.7404(4) 0.40188(13) 0.0446(13) Uani 1 1 d . . . H33A H 0.4170 0.7410 0.3910 0.054 Uiso 1 1 calc R . . H33B H 0.3708 0.8307 0.4057 0.054 Uiso 1 1 calc R . . C34 C 0.34503(18) 0.6782(4) 0.37150(13) 0.0572(14) Uani 1 1 d . . . H34A H 0.3572 0.5915 0.3655 0.086 Uiso 1 1 calc R . . H34B H 0.3448 0.7296 0.3474 0.086 Uiso 1 1 calc R . . H34C H 0.3099 0.6740 0.3823 0.086 Uiso 1 1 calc R . . C35 C 0.43087(17) 0.4721(4) 0.41860(12) 0.0471(13) Uani 1 1 d . . . H35A H 0.4577 0.4200 0.4313 0.071 Uiso 1 1 calc R . . H35B H 0.4469 0.5273 0.3987 0.071 Uiso 1 1 calc R . . H35C H 0.4054 0.4158 0.4060 0.071 Uiso 1 1 calc R . . C36 C 0.40960(17) 0.2292(4) 0.47228(13) 0.0478(13) Uani 1 1 d . . . H36A H 0.4395 0.2214 0.4547 0.072 Uiso 1 1 calc R . . H36B H 0.3818 0.2758 0.4589 0.072 Uiso 1 1 calc R . . H36C H 0.3973 0.1435 0.4795 0.072 Uiso 1 1 calc R . . C37 C 0.45735(17) 0.1127(4) 0.55033(13) 0.0434(13) Uani 1 1 d . . . H37A H 0.4369 0.0570 0.5326 0.052 Uiso 1 1 calc R . . H37B H 0.4489 0.0889 0.5778 0.052 Uiso 1 1 calc R . . C38 C 0.51465(16) 0.0912(4) 0.54303(14) 0.0521(14) Uani 1 1 d . . . H38A H 0.5232 0.1166 0.5161 0.078 Uiso 1 1 calc R . . H38B H 0.5229 0.0003 0.5467 0.078 Uiso 1 1 calc R . . H38C H 0.5349 0.1428 0.5616 0.078 Uiso 1 1 calc R . . C39 C 0.52739(18) 0.3255(4) 0.68652(13) 0.0570(14) Uani 1 1 d . . . H39A H 0.5154 0.2404 0.6785 0.085 Uiso 1 1 calc R . . H39B H 0.5335 0.3262 0.7150 0.085 Uiso 1 1 calc R . . H39C H 0.5597 0.3458 0.6727 0.085 Uiso 1 1 calc R . . C40 C 0.5041(2) 0.5809(5) 0.73357(14) 0.0631(15) Uani 1 1 d . . . H40A H 0.5083 0.5096 0.7525 0.076 Uiso 1 1 calc R . . H40B H 0.4835 0.6488 0.7465 0.076 Uiso 1 1 calc R . . C41 C 0.5578(2) 0.6348(6) 0.72306(19) 0.087(2) Uani 1 1 d . . . H41A H 0.5762 0.6595 0.7475 0.105 Uiso 1 1 calc R . . H41B H 0.5785 0.5677 0.7097 0.105 Uiso 1 1 calc R . . C42 C 0.5530(3) 0.7504(8) 0.6964(2) 0.087(2) Uani 1 1 d . . . C43 C 0.5760(4) 0.8622(9) 0.6395(2) 0.212(6) Uani 1 1 d . . . H43A H 0.5790 0.9387 0.6561 0.318 Uiso 1 1 calc R . . H43B H 0.5419 0.8607 0.6270 0.318 Uiso 1 1 calc R . . H43C H 0.6030 0.8639 0.6192 0.318 Uiso 1 1 calc R . . C44 C 0.37451(18) 0.6316(4) 0.75854(14) 0.0582(14) Uani 1 1 d . . . H44A H 0.3583 0.6738 0.7816 0.070 Uiso 1 1 calc R . . H44B H 0.4087 0.5986 0.7669 0.070 Uiso 1 1 calc R . . C45 C 0.3410(2) 0.5205(5) 0.74568(16) 0.0829(19) Uani 1 1 d . . . H45A H 0.3109 0.5550 0.7310 0.100 Uiso 1 1 calc R . . H45B H 0.3612 0.4669 0.7272 0.100 Uiso 1 1 calc R . . C46 C 0.3212(3) 0.4367(9) 0.7781(2) 0.092(2) Uani 1 1 d . . . C47 C 0.2914(2) 0.2500(5) 0.80659(18) 0.107(2) Uani 1 1 d . . . H47A H 0.3183 0.2265 0.8256 0.160 Uiso 1 1 calc R . . H47B H 0.2744 0.1724 0.7969 0.160 Uiso 1 1 calc R . . H47C H 0.2657 0.3053 0.8194 0.160 Uiso 1 1 calc R . . C48 C 0.32900(18) 0.9136(4) 0.75687(13) 0.0563(14) Uani 1 1 d . . . H48A H 0.2929 0.8855 0.7545 0.084 Uiso 1 1 calc R . . H48B H 0.3308 1.0069 0.7539 0.084 Uiso 1 1 calc R . . H48C H 0.3424 0.8892 0.7828 0.084 Uiso 1 1 calc R . . O1W O 0.4884(3) 1.0225(8) 0.6447(3) 0.130(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0446(8) 0.0464(7) 0.0452(9) -0.0012(6) 0.0015(6) 0.0013(6) Cl2 0.0470(8) 0.0461(7) 0.0552(9) 0.0060(6) 0.0036(7) 0.0006(6) O1 0.136(5) 0.097(4) 0.112(4) 0.009(3) 0.008(3) 0.001(3) O2 0.112(4) 0.238(7) 0.082(4) -0.065(4) 0.021(3) -0.059(4) O3 0.244(7) 0.124(4) 0.114(5) 0.034(4) 0.075(5) -0.007(4) O4 0.143(5) 0.076(3) 0.149(5) 0.024(3) -0.048(4) -0.037(3) N1 0.041(3) 0.031(2) 0.044(3) -0.008(2) 0.003(2) 0.0070(18) N2 0.031(2) 0.031(2) 0.047(3) 0.003(2) -0.005(2) 0.0056(18) N3 0.043(2) 0.031(2) 0.028(2) -0.003(2) -0.0044(19) -0.0011(19) N4 0.047(3) 0.029(2) 0.042(3) -0.003(2) -0.002(2) 0.0057(19) N5 0.047(3) 0.034(2) 0.034(3) 0.006(2) -0.005(2) 0.009(2) N6 0.055(3) 0.041(2) 0.030(3) -0.003(2) 0.000(2) 0.005(2) C1 0.039(3) 0.037(3) 0.043(4) -0.009(3) 0.001(3) 0.010(2) C2 0.030(3) 0.038(3) 0.045(4) -0.007(3) 0.004(3) 0.003(2) C3 0.033(3) 0.029(3) 0.054(4) 0.000(3) 0.008(3) 0.003(2) C4 0.031(3) 0.036(3) 0.043(4) 0.003(3) 0.006(3) 0.000(2) C5 0.035(3) 0.033(3) 0.031(3) 0.002(2) 0.006(3) 0.003(2) C6 0.032(3) 0.040(3) 0.038(4) 0.004(3) 0.002(3) -0.002(2) C7 0.037(3) 0.036(3) 0.037(4) 0.009(3) -0.003(3) -0.001(2) C8 0.037(3) 0.030(3) 0.037(3) -0.001(2) 0.002(2) -0.005(2) C9 0.037(3) 0.032(3) 0.028(3) -0.001(3) 0.002(2) -0.002(2) C10 0.036(3) 0.039(3) 0.028(3) 0.000(3) 0.002(2) -0.008(2) C11 0.044(3) 0.035(3) 0.035(4) -0.005(3) 0.004(3) -0.001(2) C12 0.040(3) 0.031(3) 0.035(4) 0.000(3) 0.001(3) -0.001(2) C13 0.033(3) 0.041(3) 0.034(4) -0.001(3) 0.002(2) -0.008(2) C14 0.038(3) 0.029(3) 0.042(4) -0.010(3) 0.008(2) 0.001(2) C15 0.033(3) 0.028(3) 0.038(3) -0.003(2) 0.008(2) 0.002(2) C16 0.036(3) 0.035(3) 0.036(4) 0.004(3) 0.007(2) 0.001(2) C17 0.043(3) 0.025(3) 0.047(4) 0.005(3) 0.008(3) -0.002(2) C18 0.048(3) 0.032(3) 0.037(4) 0.003(3) -0.001(3) 0.000(3) C19 0.050(3) 0.042(3) 0.039(4) 0.007(3) 0.003(3) 0.010(3) C20 0.056(4) 0.046(3) 0.027(3) 0.003(3) -0.005(3) 0.011(3) C21 0.049(3) 0.046(3) 0.032(4) -0.003(3) 0.003(3) 0.001(3) C22 0.050(3) 0.044(3) 0.036(4) -0.009(3) -0.002(3) 0.006(3) C23 0.050(3) 0.045(3) 0.030(3) 0.004(3) -0.005(3) 0.004(3) C24 0.040(3) 0.050(3) 0.034(4) -0.011(3) -0.003(3) 0.009(3) C25 0.043(3) 0.044(3) 0.038(4) -0.012(3) -0.003(3) 0.005(3) C26 0.048(3) 0.042(3) 0.048(4) -0.012(3) -0.006(3) 0.000(3) C27 0.051(4) 0.040(3) 0.055(4) -0.014(3) -0.002(3) 0.004(2) C28 0.065(4) 0.074(4) 0.080(5) -0.038(3) -0.003(3) 0.016(3) C29 0.051(3) 0.033(3) 0.066(4) 0.004(3) 0.005(3) 0.002(2) C30 0.047(3) 0.056(3) 0.043(4) 0.003(2) 0.001(3) 0.014(3) C31 0.050(3) 0.059(3) 0.039(4) 0.002(3) -0.006(3) 0.007(3) C32 0.091(5) 0.073(4) 0.051(4) 0.017(3) 0.000(3) 0.021(3) C33 0.039(3) 0.049(3) 0.046(4) -0.004(3) 0.002(3) 0.000(2) C34 0.061(4) 0.075(4) 0.036(3) 0.000(3) 0.001(3) -0.006(3) C35 0.055(3) 0.045(3) 0.041(3) -0.004(2) 0.008(3) 0.003(2) C36 0.054(3) 0.039(3) 0.051(4) -0.010(3) 0.003(3) 0.003(2) C37 0.045(3) 0.031(3) 0.054(4) -0.006(2) 0.000(3) 0.001(2) C38 0.042(3) 0.036(3) 0.078(4) -0.004(2) -0.003(3) 0.005(2) C39 0.071(4) 0.064(3) 0.035(3) 0.003(3) -0.006(3) 0.018(3) C40 0.077(4) 0.069(4) 0.044(4) -0.001(3) -0.012(3) 0.015(3) C41 0.067(5) 0.087(5) 0.108(6) -0.030(4) -0.034(4) 0.013(4) C42 0.073(6) 0.101(7) 0.088(7) -0.026(5) -0.013(5) -0.017(5) C43 0.289(13) 0.256(11) 0.091(7) 0.059(7) -0.047(7) -0.163(10) C44 0.059(4) 0.068(3) 0.048(4) 0.004(3) -0.003(3) 0.000(3) C45 0.129(6) 0.064(4) 0.056(5) 0.013(3) 0.014(4) -0.020(4) C46 0.072(5) 0.129(7) 0.074(6) 0.016(6) -0.002(4) 0.008(5) C47 0.104(5) 0.088(5) 0.129(6) 0.057(4) 0.026(4) -0.010(4) C48 0.054(3) 0.076(3) 0.038(4) -0.007(3) -0.006(3) 0.008(3) O1W 0.126(8) 0.099(6) 0.165(10) 0.005(6) 0.008(7) -0.005(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 O1 C42 1.185(7) . ? O2 C42 1.311(7) . ? O2 C43 1.547(9) . ? O3 C46 1.240(7) . ? O4 C46 1.227(8) . ? O4 C47 1.522(6) . ? N1 C4 1.363(5) . ? N1 C1 1.392(5) . ? N1 H1A 0.8800 . ? N2 C8 1.373(5) . ? N2 C5 1.390(5) . ? N2 H2A 0.8800 . ? N3 C9 1.366(5) . ? N3 C12 1.389(5) . ? N3 H3A 0.8800 . ? N4 C13 1.358(5) . ? N4 C16 1.389(5) . ? N4 H4A 0.8800 . ? N5 C21 1.359(5) . ? N5 C18 1.390(5) . ? N5 H5A 0.8800 . ? N6 C22 1.354(5) . ? N6 C25 1.383(5) . ? N6 H6A 0.8800 . ? C1 C26 1.362(6) . ? C1 C2 1.435(6) . ? C2 C3 1.366(5) . ? C2 C27 1.490(5) . ? C3 C4 1.430(5) . ? C3 C29 1.500(5) . ? C4 C5 1.429(6) . ? C5 C6 1.383(6) . ? C6 C7 1.404(6) . ? C6 C30 1.503(5) . ? C7 C8 1.393(5) . ? C7 C31 1.491(6) . ? C8 C9 1.443(5) . ? C9 C10 1.388(5) . ? C10 C11 1.413(5) . ? C10 C33 1.505(6) . ? C11 C12 1.390(5) . ? C11 C35 1.502(5) . ? C12 C13 1.409(6) . ? C13 C14 1.430(5) . ? C14 C15 1.378(5) . ? C14 C36 1.503(5) . ? C15 C16 1.427(6) . ? C15 C37 1.486(5) . ? C16 C17 1.368(5) . ? C17 C18 1.410(6) . ? C17 H17A 0.9500 . ? C18 C19 1.406(6) . ? C19 C20 1.399(5) . ? C19 C39 1.497(6) . ? C20 C21 1.394(6) . ? C20 C40 1.500(6) . ? C21 C22 1.461(6) . ? C22 C23 1.398(6) . ? C23 C24 1.379(5) . ? C23 C44 1.506(6) . ? C24 C25 1.390(6) . ? C24 C48 1.511(6) . ? C25 C26 1.414(6) . ? C26 H26A 0.9500 . ? C27 C28 1.523(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.535(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.541(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.517(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.539(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.515(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.512(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.495(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 C42 O2 C43 109.2(7) . . ? C46 O4 C47 113.8(6) . . ? C4 N1 C1 109.1(4) . . ? C4 N1 H1A 125.4 . . ? C1 N1 H1A 125.4 . . ? C8 N2 C5 108.8(4) . . ? C8 N2 H2A 125.6 . . ? C5 N2 H2A 125.6 . . ? C9 N3 C12 109.6(4) . . ? C9 N3 H3A 125.2 . . ? C12 N3 H3A 125.2 . . ? C13 N4 C16 110.2(4) . . ? C13 N4 H4A 124.9 . . ? C16 N4 H4A 124.9 . . ? C21 N5 C18 108.7(4) . . ? C21 N5 H5A 125.7 . . ? C18 N5 H5A 125.7 . . ? C22 N6 C25 108.9(4) . . ? C22 N6 H6A 125.5 . . ? C25 N6 H6A 125.5 . . ? C26 C1 N1 125.7(4) . . ? C26 C1 C2 127.4(4) . . ? N1 C1 C2 106.8(4) . . ? C3 C2 C1 108.2(4) . . ? C3 C2 C27 126.6(4) . . ? C1 C2 C27 125.2(5) . . ? C2 C3 C4 107.5(4) . . ? C2 C3 C29 126.4(4) . . ? C4 C3 C29 126.1(5) . . ? N1 C4 C5 119.5(4) . . ? N1 C4 C3 108.3(4) . . ? C5 C4 C3 132.1(5) . . ? C6 C5 N2 107.5(4) . . ? C6 C5 C4 132.8(4) . . ? N2 C5 C4 119.3(4) . . ? C5 C6 C7 108.2(4) . . ? C5 C6 C30 127.5(4) . . ? C7 C6 C30 123.5(4) . . ? C8 C7 C6 107.1(4) . . ? C8 C7 C31 127.3(4) . . ? C6 C7 C31 125.3(4) . . ? N2 C8 C7 108.3(4) . . ? N2 C8 C9 117.0(4) . . ? C7 C8 C9 134.2(5) . . ? N3 C9 C10 107.8(4) . . ? N3 C9 C8 117.3(4) . . ? C10 C9 C8 134.9(4) . . ? C9 C10 C11 107.9(4) . . ? C9 C10 C33 126.7(4) . . ? C11 C10 C33 125.2(4) . . ? C12 C11 C10 107.2(4) . . ? C12 C11 C35 128.0(4) . . ? C10 C11 C35 124.4(4) . . ? N3 C12 C11 107.5(4) . . ? N3 C12 C13 118.3(4) . . ? C11 C12 C13 134.1(4) . . ? N4 C13 C12 120.7(4) . . ? N4 C13 C14 107.4(4) . . ? C12 C13 C14 131.8(5) . . ? C15 C14 C13 107.9(4) . . ? C15 C14 C36 126.9(4) . . ? C13 C14 C36 125.0(4) . . ? C14 C15 C16 107.8(4) . . ? C14 C15 C37 126.5(4) . . ? C16 C15 C37 125.8(4) . . ? C17 C16 N4 126.9(4) . . ? C17 C16 C15 126.4(4) . . ? N4 C16 C15 106.7(4) . . ? C16 C17 C18 130.8(4) . . ? C16 C17 H17A 114.6 . . ? C18 C17 H17A 114.6 . . ? N5 C18 C19 107.2(4) . . ? N5 C18 C17 126.0(4) . . ? C19 C18 C17 126.7(4) . . ? C20 C19 C18 107.9(4) . . ? C20 C19 C39 126.0(5) . . ? C18 C19 C39 125.9(4) . . ? C21 C20 C19 106.8(4) . . ? C21 C20 C40 126.6(4) . . ? C19 C20 C40 126.1(4) . . ? N5 C21 C20 109.3(4) . . ? N5 C21 C22 121.9(4) . . ? C20 C21 C22 128.5(5) . . ? N6 C22 C23 108.5(4) . . ? N6 C22 C21 123.2(4) . . ? C23 C22 C21 128.2(5) . . ? C24 C23 C22 106.8(4) . . ? C24 C23 C44 126.4(5) . . ? C22 C23 C44 126.4(4) . . ? C23 C24 C25 108.7(4) . . ? C23 C24 C48 126.3(5) . . ? C25 C24 C48 124.8(4) . . ? N6 C25 C24 107.0(4) . . ? N6 C25 C26 126.1(5) . . ? C24 C25 C26 126.8(5) . . ? C1 C26 C25 130.9(4) . . ? C1 C26 H26A 114.5 . . ? C25 C26 H26A 114.5 . . ? C2 C27 C28 111.7(4) . . ? C2 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C2 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C3 C29 H29A 109.5 . . ? C3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C6 C30 H30A 109.5 . . ? C6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C7 C31 C32 113.3(4) . . ? C7 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? C7 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C10 C33 C34 114.8(4) . . ? C10 C33 H33A 108.6 . . ? C34 C33 H33A 108.6 . . ? C10 C33 H33B 108.6 . . ? C34 C33 H33B 108.6 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C11 C35 H35A 109.5 . . ? C11 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C11 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C14 C36 H36A 109.5 . . ? C14 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C14 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C15 C37 C38 111.1(3) . . ? C15 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? C15 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C19 C39 H39A 109.5 . . ? C19 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C19 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C20 C40 C41 112.3(4) . . ? C20 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? C20 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.9 . . ? C42 C41 C40 110.8(5) . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? O1 C42 O2 124.5(8) . . ? O1 C42 C41 123.4(8) . . ? O2 C42 C41 112.1(7) . . ? O2 C43 H43A 109.5 . . ? O2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C23 C44 C45 112.5(4) . . ? C23 C44 H44A 109.1 . . ? C45 C44 H44A 109.1 . . ? C23 C44 H44B 109.1 . . ? C45 C44 H44B 109.1 . . ? H44A C44 H44B 107.8 . . ? C46 C45 C44 115.5(5) . . ? C46 C45 H45A 108.4 . . ? C44 C45 H45A 108.4 . . ? C46 C45 H45B 108.4 . . ? C44 C45 H45B 108.4 . . ? H45A C45 H45B 107.5 . . ? O4 C46 O3 122.2(8) . . ? O4 C46 C45 119.6(7) . . ? O3 C46 C45 118.2(8) . . ? O4 C47 H47A 109.5 . . ? O4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C24 C48 H48A 109.5 . . ? C24 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C24 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C26 174.9(4) . . . . ? C4 N1 C1 C2 -1.3(4) . . . . ? C26 C1 C2 C3 -176.1(4) . . . . ? N1 C1 C2 C3 -0.1(5) . . . . ? C26 C1 C2 C27 3.9(7) . . . . ? N1 C1 C2 C27 -180.0(4) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? C27 C2 C3 C4 -178.7(4) . . . . ? C1 C2 C3 C29 -176.4(4) . . . . ? C27 C2 C3 C29 3.6(7) . . . . ? C1 N1 C4 C5 -179.5(4) . . . . ? C1 N1 C4 C3 2.1(4) . . . . ? C2 C3 C4 N1 -2.2(5) . . . . ? C29 C3 C4 N1 175.5(4) . . . . ? C2 C3 C4 C5 179.7(4) . . . . ? C29 C3 C4 C5 -2.6(7) . . . . ? C8 N2 C5 C6 0.3(4) . . . . ? C8 N2 C5 C4 174.4(4) . . . . ? N1 C4 C5 C6 147.2(5) . . . . ? C3 C4 C5 C6 -34.9(8) . . . . ? N1 C4 C5 N2 -25.2(6) . . . . ? C3 C4 C5 N2 152.8(4) . . . . ? N2 C5 C6 C7 -0.4(5) . . . . ? C4 C5 C6 C7 -173.4(4) . . . . ? N2 C5 C6 C30 170.0(4) . . . . ? C4 C5 C6 C30 -3.0(8) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? C30 C6 C7 C8 -170.5(4) . . . . ? C5 C6 C7 C31 174.0(4) . . . . ? C30 C6 C7 C31 3.2(7) . . . . ? C5 N2 C8 C7 -0.1(4) . . . . ? C5 N2 C8 C9 -172.9(3) . . . . ? C6 C7 C8 N2 -0.2(5) . . . . ? C31 C7 C8 N2 -173.7(4) . . . . ? C6 C7 C8 C9 170.8(4) . . . . ? C31 C7 C8 C9 -2.7(8) . . . . ? C12 N3 C9 C10 -1.7(4) . . . . ? C12 N3 C9 C8 178.9(3) . . . . ? N2 C8 C9 N3 30.4(5) . . . . ? C7 C8 C9 N3 -140.0(5) . . . . ? N2 C8 C9 C10 -148.7(5) . . . . ? C7 C8 C9 C10 40.9(8) . . . . ? N3 C9 C10 C11 1.1(5) . . . . ? C8 C9 C10 C11 -179.7(4) . . . . ? N3 C9 C10 C33 -173.5(4) . . . . ? C8 C9 C10 C33 5.7(8) . . . . ? C9 C10 C11 C12 -0.1(5) . . . . ? C33 C10 C11 C12 174.6(4) . . . . ? C9 C10 C11 C35 -173.0(4) . . . . ? C33 C10 C11 C35 1.7(7) . . . . ? C9 N3 C12 C11 1.7(4) . . . . ? C9 N3 C12 C13 178.1(4) . . . . ? C10 C11 C12 N3 -1.0(4) . . . . ? C35 C11 C12 N3 171.7(4) . . . . ? C10 C11 C12 C13 -176.6(4) . . . . ? C35 C11 C12 C13 -4.0(8) . . . . ? C16 N4 C13 C12 179.1(4) . . . . ? C16 N4 C13 C14 1.9(5) . . . . ? N3 C12 C13 N4 -22.2(6) . . . . ? C11 C12 C13 N4 153.0(4) . . . . ? N3 C12 C13 C14 154.1(4) . . . . ? C11 C12 C13 C14 -30.6(8) . . . . ? N4 C13 C14 C15 -2.9(5) . . . . ? C12 C13 C14 C15 -179.6(4) . . . . ? N4 C13 C14 C36 171.2(4) . . . . ? C12 C13 C14 C36 -5.6(7) . . . . ? C13 C14 C15 C16 2.7(5) . . . . ? C36 C14 C15 C16 -171.2(4) . . . . ? C13 C14 C15 C37 -176.8(4) . . . . ? C36 C14 C15 C37 9.3(7) . . . . ? C13 N4 C16 C17 -178.7(4) . . . . ? C13 N4 C16 C15 -0.3(4) . . . . ? C14 C15 C16 C17 176.8(4) . . . . ? C37 C15 C16 C17 -3.7(7) . . . . ? C14 C15 C16 N4 -1.6(5) . . . . ? C37 C15 C16 N4 178.0(4) . . . . ? N4 C16 C17 C18 6.1(7) . . . . ? C15 C16 C17 C18 -172.0(4) . . . . ? C21 N5 C18 C19 -1.0(5) . . . . ? C21 N5 C18 C17 -178.5(4) . . . . ? C16 C17 C18 N5 21.0(7) . . . . ? C16 C17 C18 C19 -156.0(5) . . . . ? N5 C18 C19 C20 -1.2(5) . . . . ? C17 C18 C19 C20 176.2(4) . . . . ? N5 C18 C19 C39 -176.9(4) . . . . ? C17 C18 C19 C39 0.5(7) . . . . ? C18 C19 C20 C21 3.0(5) . . . . ? C39 C19 C20 C21 178.6(4) . . . . ? C18 C19 C20 C40 -169.6(4) . . . . ? C39 C19 C20 C40 6.1(8) . . . . ? C18 N5 C21 C20 3.0(5) . . . . ? C18 N5 C21 C22 -172.4(4) . . . . ? C19 C20 C21 N5 -3.7(5) . . . . ? C40 C20 C21 N5 168.8(4) . . . . ? C19 C20 C21 C22 171.3(4) . . . . ? C40 C20 C21 C22 -16.2(8) . . . . ? C25 N6 C22 C23 3.1(5) . . . . ? C25 N6 C22 C21 -176.2(4) . . . . ? N5 C21 C22 N6 -52.0(6) . . . . ? C20 C21 C22 N6 133.6(5) . . . . ? N5 C21 C22 C23 128.8(5) . . . . ? C20 C21 C22 C23 -45.6(7) . . . . ? N6 C22 C23 C24 -3.2(5) . . . . ? C21 C22 C23 C24 176.1(4) . . . . ? N6 C22 C23 C44 169.9(4) . . . . ? C21 C22 C23 C44 -10.8(8) . . . . ? C22 C23 C24 C25 2.1(5) . . . . ? C44 C23 C24 C25 -171.0(4) . . . . ? C22 C23 C24 C48 176.9(4) . . . . ? C44 C23 C24 C48 3.9(7) . . . . ? C22 N6 C25 C24 -1.8(5) . . . . ? C22 N6 C25 C26 -177.4(4) . . . . ? C23 C24 C25 N6 -0.2(5) . . . . ? C48 C24 C25 N6 -175.2(4) . . . . ? C23 C24 C25 C26 175.4(4) . . . . ? C48 C24 C25 C26 0.4(7) . . . . ? N1 C1 C26 C25 6.3(8) . . . . ? C2 C1 C26 C25 -178.4(4) . . . . ? N6 C25 C26 C1 22.6(8) . . . . ? C24 C25 C26 C1 -152.2(5) . . . . ? C3 C2 C27 C28 90.8(5) . . . . ? C1 C2 C27 C28 -89.3(5) . . . . ? C8 C7 C31 C32 -113.5(5) . . . . ? C6 C7 C31 C32 74.2(6) . . . . ? C9 C10 C33 C34 -116.5(5) . . . . ? C11 C10 C33 C34 69.8(5) . . . . ? C14 C15 C37 C38 92.1(5) . . . . ? C16 C15 C37 C38 -87.3(5) . . . . ? C21 C20 C40 C41 -99.9(6) . . . . ? C19 C20 C40 C41 71.2(6) . . . . ? C20 C40 C41 C42 62.9(6) . . . . ? C43 O2 C42 O1 -2.1(9) . . . . ? C43 O2 C42 C41 -179.7(5) . . . . ? C40 C41 C42 O1 52.6(8) . . . . ? C40 C41 C42 O2 -129.8(5) . . . . ? C24 C23 C44 C45 109.2(6) . . . . ? C22 C23 C44 C45 -62.5(6) . . . . ? C23 C44 C45 C46 -165.9(5) . . . . ? C47 O4 C46 O3 4.2(10) . . . . ? C47 O4 C46 C45 -175.2(5) . . . . ? C44 C45 C46 O4 -145.9(6) . . . . ? C44 C45 C46 O3 34.7(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Cl1 0.88 2.75 3.546(4) 150.7 . N3 H3A Cl1 0.88 2.43 3.265(4) 158.2 . N5 H5A Cl1 0.88 2.38 3.225(4) 161.3 . N2 H2A Cl2 0.88 2.46 3.335(4) 173.9 . N4 H4A Cl2 0.88 2.74 3.573(3) 158.0 . N6 H6A Cl2 0.88 2.47 3.316(4) 161.7 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.414 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.061 # Attachment 'jtuo2-final.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 661302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '5 C48 H54 N6 O4 U O2, C6 H14' _chemical_formula_sum 'C123 H142 N15 O15 U2.50' _chemical_formula_weight 2665.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 40.592(2) _cell_length_b 16.1043(6) _cell_length_c 17.9271(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.662(2) _cell_angle_gamma 90.00 _cell_volume 11680.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15170 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_crystal_description laths _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5340 _exptl_absorpt_coefficient_mu 3.528 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.450 _exptl_absorpt_correction_T_max 0.872 _exptl_absorpt_process_details 'Xprep, Shelxltl/Plus, Siemens Analytical' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24946 _diffrn_reflns_av_R_equivalents 0.1038 _diffrn_reflns_av_sigmaI/netI 0.2011 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 23.75 _reflns_number_total 17431 _reflns_number_gt 8211 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The methyl ester moieties were poorly defined in many instances. Disorder models were unsuccessfully applied. These moieties appeared to be suffering from very high displacement. The geometry of the methyl ester moieties were restrained to be equivalent throughout the refinement process. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17431 _refine_ls_number_parameters 1366 _refine_ls_number_restraints 942 _refine_ls_R_factor_all 0.2297 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.517 _refine_ls_restrained_S_all 1.524 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.033 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 0.106460(14) 0.84974(5) 0.29708(3) 0.0584(2) Uani 1 1 d . . . U2 U 0.302913(14) 0.72384(4) 0.34706(3) 0.0538(2) Uani 1 1 d . . . U3 U 0.5000 0.62766(7) 0.2500 0.0675(4) Uani 1 2 d S . . O1 O 0.0774(2) 0.8110(6) 0.3543(5) 0.059(3) Uani 1 1 d U . . O2 O 0.1364(2) 0.8865(6) 0.2389(4) 0.050(3) Uani 1 1 d U . . N1 N 0.0721(3) 0.7535(9) 0.2009(7) 0.066(4) Uani 1 1 d U . . N2 N 0.0579(3) 0.9264(8) 0.2090(6) 0.046(3) Uani 1 1 d U . . N3 N 0.0949(3) 1.0029(9) 0.3067(7) 0.057(4) Uani 1 1 d U . . N4 N 0.1255(3) 0.9340(9) 0.4138(7) 0.056(4) Uani 1 1 d U . . N5 N 0.1535(3) 0.7923(8) 0.3978(6) 0.054(4) Uani 1 1 d U . . N6 N 0.1324(3) 0.7083(8) 0.2615(6) 0.060(4) Uani 1 1 d U . . C1 C 0.0830(4) 0.6768(11) 0.1897(8) 0.056(5) Uani 1 1 d U . . C2 C 0.0576(5) 0.6186(12) 0.1661(9) 0.073(5) Uani 1 1 d U . . C3 C 0.0291(4) 0.6624(11) 0.1633(8) 0.054(5) Uani 1 1 d U . . C4 C 0.0369(4) 0.7460(11) 0.1822(8) 0.050(5) Uani 1 1 d U . . C5 C 0.0183(4) 0.8176(12) 0.1714(8) 0.064(5) Uani 1 1 d U . . H5 H -0.0043 0.8081 0.1563 0.076 Uiso 1 1 d R . . C6 C 0.0274(4) 0.8981(12) 0.1766(8) 0.049(4) Uani 1 1 d U . . C7 C 0.0083(4) 0.9693(11) 0.1467(8) 0.056(5) Uani 1 1 d U . . C8 C 0.0259(4) 1.0372(11) 0.1629(8) 0.052(5) Uani 1 1 d U . . C9 C 0.0567(3) 1.0088(11) 0.2037(8) 0.042(4) Uani 1 1 d U . . C10 C 0.0803(4) 1.0550(12) 0.2503(9) 0.060(5) Uani 1 1 d U . . C11 C 0.0867(4) 1.1368(12) 0.2672(9) 0.062(5) Uani 1 1 d U . . C12 C 0.1036(3) 1.1434(11) 0.3383(8) 0.050(4) Uani 1 1 d U . . C13 C 0.1067(3) 1.0570(11) 0.3603(9) 0.045(4) Uani 1 1 d U . . C14 C 0.1199(3) 1.0116(11) 0.4264(9) 0.043(4) Uani 1 1 d U . . C15 C 0.1248(3) 1.0325(11) 0.5064(9) 0.046(4) Uani 1 1 d U . . C16 C 0.1368(3) 0.9629(11) 0.5353(8) 0.047(4) Uani 1 1 d U . . C17 C 0.1394(3) 0.8980(11) 0.4784(9) 0.052(5) Uani 1 1 d U . . C18 C 0.1552(3) 0.8242(10) 0.4682(8) 0.046(4) Uani 1 1 d U . . C19 C 0.1805(4) 0.7766(11) 0.5156(8) 0.057(5) Uani 1 1 d U . . C20 C 0.1943(3) 0.7251(10) 0.4693(8) 0.052(4) Uani 1 1 d U . . C21 C 0.1778(4) 0.7371(10) 0.3960(8) 0.049(4) Uani 1 1 d U . . C22 C 0.1856(3) 0.6906(9) 0.3328(8) 0.053(5) Uani 1 1 d U . . H22 H 0.2071 0.6671 0.3343 0.064 Uiso 1 1 d R . . C23 C 0.1653(4) 0.6799(10) 0.2685(8) 0.054(5) Uani 1 1 d U . . C24 C 0.1713(4) 0.6252(10) 0.2094(9) 0.057(5) Uani 1 1 d U . . C25 C 0.1416(4) 0.6115(10) 0.1672(9) 0.064(5) Uani 1 1 d U . . C26 C 0.1192(4) 0.6634(10) 0.2052(9) 0.054(5) Uani 1 1 d U . . C27 C 0.0584(4) 0.5291(8) 0.1638(8) 0.084(6) Uani 1 1 d DU . . H27C H 0.0424 0.5072 0.1977 0.101 Uiso 1 1 d R . . H27D H 0.0808 0.5122 0.1844 0.101 Uiso 1 1 d R . . C28 C 0.0518(4) 0.4893(8) 0.0869(7) 0.114(7) Uani 1 1 d DU . . H28C H 0.0275 0.4869 0.0747 0.137 Uiso 1 1 d R . . H28D H 0.0612 0.5242 0.0485 0.137 Uiso 1 1 d R . . C29 C 0.0660(4) 0.4042(8) 0.0829(7) 0.181(12) Uani 1 1 d DU . . C30 C 0.0821(5) 0.3009(12) 0.0009(10) 0.199(12) Uani 1 1 d DU . . H30A H 0.1037 0.3102 0.0284 0.298 Uiso 1 1 d R . . H30B H 0.0847 0.3009 -0.0530 0.298 Uiso 1 1 d R . . H30C H 0.0732 0.2473 0.0155 0.298 Uiso 1 1 d R . . O3 O 0.0897(4) 0.3827(8) 0.1237(7) 0.203(8) Uani 1 1 d DU . . O4 O 0.0599(4) 0.3683(9) 0.0164(7) 0.201(8) Uani 1 1 d DU . . C31 C -0.0056(4) 0.6341(10) 0.1426(8) 0.086(6) Uani 1 1 d U . . H31A H -0.0102 0.6358 0.0881 0.130 Uiso 1 1 d R . . H31B H -0.0209 0.6710 0.1660 0.130 Uiso 1 1 d R . . H31C H -0.0083 0.5772 0.1604 0.130 Uiso 1 1 d R . . C32 C -0.0260(3) 0.9611(9) 0.1126(8) 0.055(5) Uani 1 1 d U . . H32A H -0.0355 1.0175 0.1067 0.066 Uiso 1 1 d R . . H32B H -0.0392 0.9301 0.1473 0.066 Uiso 1 1 d R . . C33 C -0.0294(3) 0.9181(9) 0.0384(8) 0.067(5) Uani 1 1 d U . . H33A H -0.0176 0.9503 0.0026 0.100 Uiso 1 1 d R . . H33B H -0.0528 0.9139 0.0205 0.100 Uiso 1 1 d R . . H33C H -0.0199 0.8623 0.0434 0.100 Uiso 1 1 d R . . C34 C 0.0156(3) 1.1254(10) 0.1474(8) 0.069(5) Uani 1 1 d U . . H34A H -0.0081 1.1274 0.1311 0.103 Uiso 1 1 d R . . H34B H 0.0282 1.1498 0.1086 0.103 Uiso 1 1 d R . . H34C H 0.0197 1.1569 0.1939 0.103 Uiso 1 1 d R . . C35 C 0.0816(4) 1.2128(10) 0.2141(8) 0.088(6) Uani 1 1 d U . . H35A H 0.0851 1.1946 0.1632 0.131 Uiso 1 1 d R . . H35B H 0.0971 1.2575 0.2290 0.131 Uiso 1 1 d R . . H35C H 0.0589 1.2331 0.2155 0.131 Uiso 1 1 d R . . C36 C 0.1152(3) 1.2209(10) 0.3757(8) 0.061(5) Uani 1 1 d U . . H36A H 0.1080 1.2230 0.4271 0.074 Uiso 1 1 d R . . H36B H 0.1058 1.2697 0.3479 0.074 Uiso 1 1 d R . . C37 C 0.1538(4) 1.2230(10) 0.3804(8) 0.085(6) Uani 1 1 d U . . H37A H 0.1631 1.1775 0.4116 0.128 Uiso 1 1 d R . . H37B H 0.1616 1.2762 0.4017 0.128 Uiso 1 1 d R . . H37C H 0.1609 1.2173 0.3296 0.128 Uiso 1 1 d R . . C38 C 0.1151(3) 1.1109(9) 0.5431(8) 0.054(5) Uani 1 1 d U . . H38A H 0.1276 1.1582 0.5242 0.064 Uiso 1 1 d R . . H38B H 0.1213 1.1061 0.5975 0.064 Uiso 1 1 d R . . C39 C 0.0775(3) 1.1318(9) 0.5296(7) 0.052(4) Uani 1 1 d U . . H39A H 0.0713 1.1398 0.4761 0.078 Uiso 1 1 d R . . H39B H 0.0728 1.1826 0.5569 0.078 Uiso 1 1 d R . . H39C H 0.0648 1.0856 0.5483 0.078 Uiso 1 1 d R . . C40 C 0.1441(3) 0.9485(10) 0.6198(7) 0.073(5) Uani 1 1 d U . . H40A H 0.1675 0.9575 0.6354 0.109 Uiso 1 1 d R . . H40B H 0.1380 0.8912 0.6312 0.109 Uiso 1 1 d R . . H40C H 0.1306 0.9870 0.6468 0.109 Uiso 1 1 d R . . C41 C 0.1901(4) 0.7894(10) 0.5993(7) 0.078(5) Uani 1 1 d U . . H41A H 0.1715 0.7746 0.6281 0.117 Uiso 1 1 d R . . H41B H 0.1962 0.8475 0.6091 0.117 Uiso 1 1 d R . . H41C H 0.2090 0.7535 0.6141 0.117 Uiso 1 1 d R . . C42 C 0.2201(3) 0.6620(9) 0.4901(8) 0.055(5) Uani 1 1 d U . . H42A H 0.2341 0.6824 0.5340 0.066 Uiso 1 1 d R . . H42B H 0.2343 0.6551 0.4483 0.066 Uiso 1 1 d R . . C43 C 0.2052(4) 0.5767(10) 0.5079(9) 0.089(6) Uani 1 1 d U . . H43A H 0.1920 0.5824 0.5510 0.133 Uiso 1 1 d R . . H43B H 0.2233 0.5374 0.5200 0.133 Uiso 1 1 d R . . H43C H 0.1912 0.5561 0.4648 0.133 Uiso 1 1 d R . . C44 C 0.2040(4) 0.5911(10) 0.1943(8) 0.072(5) Uani 1 1 d U . . H44A H 0.2021 0.5308 0.1884 0.108 Uiso 1 1 d R . . H44B H 0.2201 0.6038 0.2366 0.108 Uiso 1 1 d R . . H44C H 0.2115 0.6154 0.1485 0.108 Uiso 1 1 d R . . C45 C 0.1370(4) 0.5576(10) 0.0964(6) 0.082(6) Uani 1 1 d DU . . H45C H 0.1570 0.5230 0.0925 0.099 Uiso 1 1 d R . . H45D H 0.1180 0.5197 0.0995 0.099 Uiso 1 1 d R . . C46 C 0.1327(4) 0.6134(7) 0.0279(7) 0.118(7) Uani 1 1 d DU . . H46C H 0.1127 0.6480 0.0323 0.142 Uiso 1 1 d R . . H46D H 0.1517 0.6515 0.0254 0.142 Uiso 1 1 d R . . C47 C 0.1278(4) 0.5691(8) -0.0444(6) 0.118(8) Uani 1 1 d DU . . C48 C 0.1087(5) 0.4524(10) -0.1125(9) 0.177 Uiso 1 1 d D . . H48A H 0.0864 0.4287 -0.1183 0.177 Uiso 1 1 d R . . H48B H 0.1250 0.4075 -0.1116 0.177 Uiso 1 1 d R . . H48C H 0.1118 0.4897 -0.1545 0.177 Uiso 1 1 d R . . O5 O 0.1449(4) 0.5801(10) -0.0955(8) 0.244(10) Uani 1 1 d DU . . O6 O 0.1103(3) 0.4990(8) -0.0422(7) 0.177(6) Uani 1 1 d DU . . O1A O 0.2701(2) 0.6524(6) 0.3290(5) 0.053(3) Uani 1 1 d U . . O2A O 0.3360(2) 0.7953(6) 0.3651(5) 0.057(3) Uani 1 1 d U . . O3A O 0.2748(3) 0.6632(8) -0.1015(6) 0.141(5) Uani 1 1 d DU . . O4A O 0.2293(3) 0.5916(9) -0.0893(7) 0.191(7) Uani 1 1 d DU . . O5A O 0.3643(3) 0.8843(8) -0.1360(7) 0.155(6) Uani 1 1 d DU . . O6A O 0.3176(2) 0.9268(7) -0.0928(6) 0.103(4) Uani 1 1 d DU . . N1A N 0.2728(3) 0.7993(7) 0.2278(6) 0.050(4) Uani 1 1 d U . . N2A N 0.2598(3) 0.8448(7) 0.3775(6) 0.049(3) Uani 1 1 d U . . N3A N 0.2917(3) 0.7594(8) 0.4794(6) 0.051(4) Uani 1 1 d U . . N4A N 0.3186(3) 0.6238(8) 0.4569(6) 0.049(4) Uani 1 1 d U . . N5A N 0.3453(3) 0.5967(7) 0.3333(6) 0.042(3) Uani 1 1 d U . . N6A N 0.3301(3) 0.7156(8) 0.2167(6) 0.056(4) Uani 1 1 d U . . C1A C 0.2833(4) 0.7816(10) 0.1601(8) 0.054(4) Uani 1 1 d U . . C2A C 0.2581(4) 0.7938(10) 0.0998(8) 0.054(5) Uani 1 1 d U . . C3A C 0.2310(3) 0.8109(9) 0.1350(8) 0.046(4) Uani 1 1 d U . . C4A C 0.2398(4) 0.8202(10) 0.2163(8) 0.053(5) Uani 1 1 d U . . C5A C 0.2224(3) 0.8638(9) 0.2660(8) 0.057(5) Uani 1 1 d U . . H5A H 0.2004 0.8794 0.2499 0.068 Uiso 1 1 d R . . C6A C 0.2340(4) 0.8865(10) 0.3399(9) 0.052(5) Uani 1 1 d U . . C7A C 0.2208(4) 0.9494(10) 0.3819(9) 0.053(5) Uani 1 1 d U . . C8A C 0.2382(4) 0.9488(10) 0.4473(9) 0.054(5) Uani 1 1 d U . . C9A C 0.2602(3) 0.8802(10) 0.4450(9) 0.046(4) Uani 1 1 d U . . C10A C 0.2811(3) 0.8367(11) 0.5016(8) 0.051(4) Uani 1 1 d U . . C11A C 0.2900(4) 0.8483(12) 0.5822(9) 0.069(5) Uani 1 1 d U . . C12A C 0.3019(4) 0.7744(13) 0.6043(10) 0.076(5) Uani 1 1 d U . . C13A C 0.3041(3) 0.7175(11) 0.5433(8) 0.044(4) Uani 1 1 d U . . C14A C 0.3131(3) 0.6374(11) 0.5296(8) 0.045(4) Uani 1 1 d U . . C15A C 0.3195(3) 0.5644(11) 0.5696(8) 0.045(4) Uani 1 1 d U . . C16A C 0.3288(3) 0.5040(11) 0.5224(8) 0.045(4) Uani 1 1 d U . . C17A C 0.3301(3) 0.5468(10) 0.4500(9) 0.046(4) Uani 1 1 d U . . C18A C 0.3444(3) 0.5291(10) 0.3807(9) 0.048(4) Uani 1 1 d U . . C19A C 0.3669(4) 0.4670(10) 0.3605(8) 0.050(4) Uani 1 1 d U . . C20A C 0.3830(3) 0.5003(10) 0.3037(8) 0.047(4) Uani 1 1 d U . . C21A C 0.3700(4) 0.5807(10) 0.2859(8) 0.046(4) Uani 1 1 d U . . C22A C 0.3795(3) 0.6331(10) 0.2325(8) 0.047(4) Uani 1 1 d U . . H22A H 0.4008 0.6241 0.2152 0.056 Uiso 1 1 d R . . C23A C 0.3626(4) 0.6993(10) 0.2014(8) 0.045(4) Uani 1 1 d U . . C24A C 0.3707(3) 0.7465(9) 0.1360(8) 0.049(4) Uani 1 1 d U . . C25A C 0.3428(4) 0.7853(10) 0.1086(8) 0.048(4) Uani 1 1 d U . . C26A C 0.3187(4) 0.7640(10) 0.1578(9) 0.062(5) Uani 1 1 d U . . C27A C 0.2597(3) 0.7711(7) 0.0217(6) 0.061(5) Uani 1 1 d DU . . H27A H 0.2827 0.7751 0.0076 0.073 Uiso 1 1 d R . . H27B H 0.2459 0.8095 -0.0108 0.073 Uiso 1 1 d R . . C28A C 0.2471(3) 0.6834(7) 0.0082(5) 0.077(6) Uani 1 1 d DU . . H28A H 0.2594 0.6462 0.0445 0.093 Uiso 1 1 d R . . H28B H 0.2234 0.6810 0.0182 0.093 Uiso 1 1 d R . . C29A C 0.2505(3) 0.6519(9) -0.0688(7) 0.107(7) Uani 1 1 d DU . . C30A C 0.2340(5) 0.5516(12) -0.1598(10) 0.231(14) Uani 1 1 d DU . . H30D H 0.2294 0.5923 -0.2000 0.346 Uiso 1 1 d R . . H30E H 0.2187 0.5047 -0.1675 0.346 Uiso 1 1 d R . . H30F H 0.2568 0.5318 -0.1603 0.346 Uiso 1 1 d R . . C31A C 0.1950(3) 0.8254(9) 0.1028(7) 0.059(5) Uani 1 1 d U . . H31D H 0.1937 0.8175 0.0485 0.088 Uiso 1 1 d R . . H31E H 0.1885 0.8823 0.1141 0.088 Uiso 1 1 d R . . H31F H 0.1802 0.7861 0.1250 0.088 Uiso 1 1 d R . . C32A C 0.1961(4) 1.0093(10) 0.3486(8) 0.071(5) Uani 1 1 d U . . H32C H 0.1851 1.0360 0.3897 0.086 Uiso 1 1 d R . . H32D H 0.1791 0.9781 0.3171 0.086 Uiso 1 1 d R . . C33A C 0.2111(4) 1.0765(10) 0.3007(8) 0.083(6) Uani 1 1 d U . . H33D H 0.2245 1.1142 0.3334 0.124 Uiso 1 1 d R . . H33E H 0.1934 1.1080 0.2730 0.124 Uiso 1 1 d R . . H33F H 0.2250 1.0502 0.2653 0.124 Uiso 1 1 d R . . C34A C 0.2305(4) 1.0022(10) 0.5108(8) 0.081(6) Uani 1 1 d U . . H34D H 0.2101 1.0328 0.4970 0.121 Uiso 1 1 d R . . H34E H 0.2486 1.0416 0.5227 0.121 Uiso 1 1 d R . . H34F H 0.2276 0.9676 0.5547 0.121 Uiso 1 1 d R . . C35A C 0.2879(4) 0.9296(10) 0.6266(8) 0.088(6) Uani 1 1 d U . . H35D H 0.2668 0.9338 0.6495 0.132 Uiso 1 1 d R . . H35E H 0.2900 0.9763 0.5922 0.132 Uiso 1 1 d R . . H35F H 0.3062 0.9310 0.6658 0.132 Uiso 1 1 d R . . C36A C 0.3184(4) 0.7616(11) 0.6841(8) 0.084(6) Uani 1 1 d U . . H36C H 0.3331 0.7126 0.6851 0.100 Uiso 1 1 d R . . H36D H 0.3321 0.8108 0.6987 0.100 Uiso 1 1 d R . . C37A C 0.2934(4) 0.7473(11) 0.7393(9) 0.114(7) Uani 1 1 d U . . H37D H 0.2787 0.7956 0.7382 0.171 Uiso 1 1 d R . . H37E H 0.3046 0.7412 0.7896 0.171 Uiso 1 1 d R . . H37F H 0.2805 0.6973 0.7263 0.171 Uiso 1 1 d R . . C38A C 0.3130(3) 0.5465(10) 0.6493(8) 0.062(5) Uani 1 1 d U . . H38C H 0.3172 0.5979 0.6788 0.075 Uiso 1 1 d R . . H38D H 0.3285 0.5035 0.6701 0.075 Uiso 1 1 d R . . C39A C 0.2773(3) 0.5184(10) 0.6597(8) 0.080(6) Uani 1 1 d U . . H39D H 0.2621 0.5652 0.6508 0.120 Uiso 1 1 d R . . H39E H 0.2758 0.4971 0.7105 0.120 Uiso 1 1 d R . . H39F H 0.2714 0.4743 0.6234 0.120 Uiso 1 1 d R . . C40A C 0.3349(3) 0.4154(10) 0.5379(8) 0.067(5) Uani 1 1 d U . . H40D H 0.3585 0.4076 0.5524 0.101 Uiso 1 1 d R . . H40E H 0.3285 0.3823 0.4932 0.101 Uiso 1 1 d R . . H40F H 0.3220 0.3976 0.5790 0.101 Uiso 1 1 d R . . C41A C 0.3699(4) 0.3761(10) 0.3900(8) 0.078(5) Uani 1 1 d U . . H41D H 0.3478 0.3513 0.3893 0.117 Uiso 1 1 d R . . H41E H 0.3802 0.3765 0.4413 0.117 Uiso 1 1 d R . . H41F H 0.3835 0.3436 0.3580 0.117 Uiso 1 1 d R . . C42A C 0.4095(3) 0.4547(9) 0.2640(7) 0.053(4) Uani 1 1 d U . . H42C H 0.4240 0.4975 0.2443 0.064 Uiso 1 1 d R . . H42D H 0.4232 0.4224 0.3019 0.064 Uiso 1 1 d R . . C43A C 0.3981(3) 0.3958(9) 0.2007(8) 0.069(5) Uani 1 1 d U . . H43D H 0.3881 0.3460 0.2207 0.104 Uiso 1 1 d R . . H43E H 0.4174 0.3798 0.1742 0.104 Uiso 1 1 d R . . H43F H 0.3819 0.4239 0.1660 0.104 Uiso 1 1 d R . . C44A C 0.4051(3) 0.7476(9) 0.1088(7) 0.054(5) Uani 1 1 d U . . H44D H 0.4051 0.7132 0.0637 0.081 Uiso 1 1 d R . . H44E H 0.4215 0.7258 0.1472 0.081 Uiso 1 1 d R . . H44F H 0.4108 0.8049 0.0967 0.081 Uiso 1 1 d R . . C45A C 0.3399(3) 0.8507(8) 0.0461(5) 0.048(4) Uani 1 1 d DU . . H45A H 0.3177 0.8768 0.0444 0.057 Uiso 1 1 d R . . H45B H 0.3565 0.8948 0.0580 0.057 Uiso 1 1 d R . . C46A C 0.3460(3) 0.8155(6) -0.0302(6) 0.085(6) Uani 1 1 d DU . . H46A H 0.3679 0.7881 -0.0283 0.102 Uiso 1 1 d R . . H46B H 0.3291 0.7725 -0.0427 0.102 Uiso 1 1 d R . . C47A C 0.3438(3) 0.8774(8) -0.0917(6) 0.096(7) Uani 1 1 d DU . . C48A C 0.3139(3) 0.9877(8) -0.1523(7) 0.088(6) Uani 1 1 d DU . . H48D H 0.3268 1.0378 -0.1394 0.131 Uiso 1 1 d R . . H48E H 0.2904 1.0024 -0.1608 0.131 Uiso 1 1 d R . . H48F H 0.3214 0.9630 -0.1979 0.131 Uiso 1 1 d R . . O1B O 0.4650(2) 0.6267(6) 0.1828(5) 0.067(3) Uani 1 1 d U . . N1B N 0.4731(3) 0.7692(9) 0.2863(7) 0.065(4) Uani 1 1 d U . . N2B N 0.4594(3) 0.6202(9) 0.3623(7) 0.055(4) Uani 1 1 d U . . N3B N 0.4891(3) 0.4934(9) 0.3107(7) 0.061(4) Uani 1 1 d U . . C1B C 0.4834(3) 0.8413(12) 0.2615(9) 0.061(5) Uani 1 1 d U . . C2B C 0.4592(5) 0.9105(14) 0.2530(9) 0.087(6) Uani 1 1 d U . . C3B C 0.4311(4) 0.8707(12) 0.2817(9) 0.065(5) Uani 1 1 d U . . C4B C 0.4404(4) 0.7918(13) 0.3046(9) 0.071(5) Uani 1 1 d U . . C5B C 0.4252(4) 0.7391(12) 0.3551(9) 0.071(5) Uani 1 1 d U . . H5B H 0.4043 0.7574 0.3688 0.085 Uiso 1 1 d R . . C6B C 0.4366(4) 0.6698(12) 0.3877(9) 0.060(5) Uani 1 1 d U . . C7B C 0.4237(4) 0.6334(11) 0.4532(8) 0.056(5) Uani 1 1 d U . . C8B C 0.4396(4) 0.5643(12) 0.4682(9) 0.066(5) Uani 1 1 d U . . C9B C 0.4614(4) 0.5507(12) 0.4083(9) 0.058(5) Uani 1 1 d U . . C10B C 0.4777(4) 0.4803(12) 0.3838(10) 0.057(5) Uani 1 1 d U . . C11B C 0.4813(4) 0.3992(12) 0.4029(9) 0.058(5) Uani 1 1 d U . . C12B C 0.4916(4) 0.3529(12) 0.3454(10) 0.063(5) Uani 1 1 d U . . C13B C 0.4951(3) 0.4159(12) 0.2886(8) 0.056(5) Uani 1 1 d U . . C18B C 0.3960(4) 0.9097(10) 0.2844(9) 0.092(6) Uani 1 1 d U . . H18A H 0.3820 0.8933 0.2397 0.138 Uiso 1 1 d R . . H18B H 0.3988 0.9701 0.2849 0.138 Uiso 1 1 d R . . H18C H 0.3856 0.8922 0.3292 0.138 Uiso 1 1 d R . . C19B C 0.3981(4) 0.6778(10) 0.4946(8) 0.065(5) Uani 1 1 d U . . H19A H 0.3808 0.7019 0.4590 0.078 Uiso 1 1 d R . . H19B H 0.3875 0.6362 0.5254 0.078 Uiso 1 1 d R . . C20B C 0.4123(4) 0.7449(11) 0.5435(9) 0.103(7) Uani 1 1 d U . . H20A H 0.4303 0.7221 0.5770 0.155 Uiso 1 1 d R . . H20B H 0.3952 0.7677 0.5732 0.155 Uiso 1 1 d R . . H20C H 0.4209 0.7891 0.5129 0.155 Uiso 1 1 d R . . C21B C 0.4337(4) 0.5054(10) 0.5339(8) 0.078(5) Uani 1 1 d U . . H21A H 0.4547 0.4848 0.5580 0.117 Uiso 1 1 d R . . H21B H 0.4202 0.4584 0.5148 0.117 Uiso 1 1 d R . . H21C H 0.4219 0.5363 0.5704 0.117 Uiso 1 1 d R . . C22B C 0.4757(4) 0.3550(10) 0.4764(8) 0.088(6) Uani 1 1 d U . . H22B H 0.4524 0.3395 0.4772 0.131 Uiso 1 1 d R . . H22C H 0.4819 0.3920 0.5186 0.131 Uiso 1 1 d R . . H22D H 0.4894 0.3049 0.4805 0.131 Uiso 1 1 d R . . C23B C 0.4961(4) 0.2604(11) 0.3426(9) 0.091(6) Uani 1 1 d U . . H23A H 0.5076 0.2418 0.3905 0.109 Uiso 1 1 d R . . H23B H 0.5102 0.2467 0.3018 0.109 Uiso 1 1 d R . . C24B C 0.4620(5) 0.2126(13) 0.3278(10) 0.142(8) Uani 1 1 d U . . H24A H 0.4481 0.2272 0.3680 0.213 Uiso 1 1 d R . . H24B H 0.4655 0.1524 0.3276 0.213 Uiso 1 1 d R . . H24C H 0.4511 0.2300 0.2796 0.213 Uiso 1 1 d R . . C14B C 0.4565(8) 1.007(3) 0.2297(14) 0.413(6) Uani 1 1 d DU . . H14A H 0.4338 1.0299 0.2290 0.496 Uiso 1 1 d R . . H14B H 0.4710 1.0423 0.2640 0.496 Uiso 1 1 d R . . O2B O 0.4181(4) 0.976(2) 0.0971(13) 0.496 Uiso 1 1 d DU . . O3B O 0.4603(6) 0.973(2) 0.0264(14) 0.496 Uiso 1 1 d DU . . C15B C 0.4711(6) 1.006(3) 0.1544(15) 0.496 Uiso 1 1 d DU . . H15A H 0.4773 1.0638 0.1447 0.496 Uiso 1 1 d R . . H15B H 0.4912 0.9709 0.1517 0.496 Uiso 1 1 d R . . C16B C 0.4475(4) 0.9751(17) 0.0923(12) 0.496 Uiso 1 1 d DU . . C17B C 0.4373(8) 0.973(3) -0.0393(12) 0.620 Uiso 1 1 d DU . . H17A H 0.4163 0.9968 -0.0260 0.620 Uiso 1 1 d R . . H17B H 0.4345 0.9138 -0.0494 0.620 Uiso 1 1 d R . . H17C H 0.4442 1.0012 -0.0841 0.620 Uiso 1 1 d R . . C1D C 0.0023(7) 0.6377(16) -0.2091(11) 0.196(13) Uani 1 1 d U . . H1DA H -0.0116 0.6822 -0.1947 0.236 Uiso 1 1 d R . . H1DB H -0.0082 0.5873 -0.1947 0.236 Uiso 1 1 d R . . C2D C 0.0315(6) 0.6451(17) -0.1599(16) 0.199(12) Uani 1 1 d U . . H2DA H 0.0429 0.6931 -0.1764 0.239 Uiso 1 1 d R . . H2DB H 0.0447 0.5980 -0.1709 0.239 Uiso 1 1 d R . . C3D C 0.0307(6) 0.6543(17) -0.0805(15) 0.219(13) Uani 1 1 d U . . H3D1 H 0.0093 0.6352 -0.0658 0.329 Uiso 1 1 d R . . H3D2 H 0.0341 0.7123 -0.0652 0.329 Uiso 1 1 d R . . H3D3 H 0.0483 0.6199 -0.0560 0.329 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0327(4) 0.0995(6) 0.0424(4) 0.0035(4) -0.0002(3) 0.0017(4) U2 0.0323(4) 0.0828(6) 0.0457(4) 0.0003(4) -0.0005(3) 0.0026(4) U3 0.0315(5) 0.1244(10) 0.0455(6) 0.000 -0.0029(4) 0.000 O1 0.053(6) 0.070(7) 0.052(6) 0.009(5) -0.006(5) 0.006(5) O2 0.045(5) 0.068(7) 0.037(5) 0.006(5) 0.001(4) 0.006(5) N1 0.060(7) 0.078(9) 0.059(7) -0.011(7) 0.001(6) 0.002(7) N2 0.039(6) 0.065(8) 0.033(6) -0.005(6) -0.010(5) 0.005(6) N3 0.039(6) 0.087(8) 0.045(7) 0.011(7) 0.003(6) -0.015(6) N4 0.044(7) 0.069(8) 0.056(7) -0.003(7) 0.002(6) -0.005(6) N5 0.044(7) 0.068(8) 0.047(7) -0.010(6) -0.011(6) 0.000(6) N6 0.057(7) 0.077(8) 0.047(7) -0.004(7) 0.000(6) 0.008(7) C1 0.056(8) 0.064(9) 0.049(8) -0.003(7) -0.003(7) -0.006(8) C2 0.076(9) 0.069(10) 0.072(9) 0.005(8) -0.002(8) 0.003(8) C3 0.051(8) 0.056(9) 0.055(8) 0.009(7) 0.004(7) -0.001(7) C4 0.050(8) 0.054(9) 0.048(8) 0.010(7) 0.011(7) 0.000(7) C5 0.051(8) 0.077(10) 0.063(8) -0.003(8) 0.004(7) 0.002(8) C6 0.051(8) 0.056(9) 0.041(8) 0.011(7) 0.010(7) -0.002(7) C7 0.050(8) 0.063(9) 0.056(8) 0.005(7) 0.009(7) 0.004(8) C8 0.046(8) 0.051(9) 0.058(8) 0.003(7) 0.007(7) 0.004(7) C9 0.027(7) 0.051(9) 0.048(8) 0.001(7) 0.004(6) -0.006(7) C10 0.051(8) 0.065(9) 0.066(8) 0.005(8) 0.027(7) -0.006(7) C11 0.049(8) 0.069(9) 0.070(8) 0.004(8) 0.007(7) 0.004(7) C12 0.042(7) 0.059(9) 0.049(8) -0.006(8) 0.003(6) 0.007(7) C13 0.034(7) 0.049(9) 0.055(8) -0.002(8) 0.015(7) -0.002(7) C14 0.023(7) 0.051(9) 0.054(8) 0.003(8) -0.001(6) -0.017(7) C15 0.026(7) 0.059(9) 0.053(8) 0.002(8) 0.001(6) -0.005(7) C16 0.048(8) 0.049(9) 0.047(8) 0.005(8) 0.013(7) -0.016(7) C17 0.041(8) 0.059(9) 0.055(8) -0.005(8) -0.009(7) 0.002(7) C18 0.039(7) 0.055(9) 0.043(8) -0.009(7) 0.002(6) -0.003(7) C19 0.059(8) 0.065(9) 0.044(8) 0.004(8) -0.003(7) -0.013(7) C20 0.039(7) 0.063(9) 0.054(8) 0.005(8) -0.007(7) 0.004(7) C21 0.048(8) 0.048(9) 0.048(8) -0.002(7) -0.006(7) -0.005(7) C22 0.042(7) 0.057(9) 0.061(8) 0.007(7) 0.002(7) 0.010(7) C23 0.052(8) 0.069(9) 0.041(8) -0.003(7) 0.006(7) 0.007(7) C24 0.044(8) 0.062(9) 0.063(8) -0.004(7) -0.003(7) 0.015(7) C25 0.059(8) 0.069(9) 0.062(8) -0.009(7) -0.004(7) 0.001(7) C26 0.039(7) 0.062(9) 0.061(8) -0.004(7) 0.006(7) -0.005(7) C27 0.070(9) 0.095(10) 0.085(9) -0.013(8) -0.006(7) -0.010(8) C28 0.112(10) 0.114(11) 0.115(10) 0.004(9) 0.005(8) 0.016(8) C29 0.192(14) 0.170(14) 0.178(14) -0.012(10) 0.005(10) 0.006(10) C30 0.207(15) 0.200(15) 0.189(14) -0.013(10) 0.016(9) 0.017(10) O3 0.206(11) 0.198(11) 0.207(11) -0.001(9) 0.029(9) 0.017(9) O4 0.215(11) 0.200(11) 0.182(10) -0.018(9) -0.011(8) 0.032(9) C31 0.072(9) 0.093(10) 0.093(9) 0.007(8) 0.000(8) -0.005(8) C32 0.037(7) 0.066(9) 0.060(8) -0.003(7) -0.001(7) 0.005(7) C33 0.048(8) 0.083(9) 0.067(8) -0.001(8) -0.003(7) 0.001(7) C34 0.061(8) 0.078(9) 0.066(8) -0.005(8) 0.000(7) -0.001(7) C35 0.083(9) 0.089(10) 0.091(9) 0.001(8) 0.006(8) -0.019(8) C36 0.049(8) 0.069(9) 0.064(8) -0.002(8) -0.004(7) -0.008(7) C37 0.073(9) 0.091(10) 0.091(9) 0.000(8) 0.002(7) -0.010(8) C38 0.031(7) 0.069(9) 0.059(8) -0.007(7) -0.003(6) 0.003(7) C39 0.045(7) 0.062(9) 0.047(7) -0.020(7) -0.001(6) 0.006(7) C40 0.070(8) 0.085(9) 0.064(8) -0.010(8) 0.010(7) 0.004(7) C41 0.082(9) 0.086(9) 0.064(8) 0.007(8) -0.014(7) 0.011(8) C42 0.045(7) 0.066(9) 0.055(8) 0.009(7) 0.005(6) 0.003(7) C43 0.078(9) 0.094(10) 0.092(9) 0.004(8) -0.005(8) 0.003(8) C44 0.071(9) 0.077(9) 0.067(8) -0.001(7) 0.000(7) 0.015(7) C45 0.080(9) 0.088(10) 0.076(9) 0.006(8) -0.004(8) 0.011(8) C46 0.136(11) 0.122(11) 0.097(10) -0.012(9) 0.012(8) -0.001(9) C47 0.127(11) 0.106(11) 0.120(11) 0.005(9) -0.002(9) -0.020(9) O5 0.251(13) 0.245(13) 0.236(12) 0.000(9) 0.030(9) 0.003(9) O6 0.196(10) 0.197(10) 0.135(9) -0.069(8) 0.000(8) -0.024(8) O1A 0.047(5) 0.056(6) 0.055(5) -0.002(5) 0.000(5) 0.005(5) O2A 0.048(5) 0.070(7) 0.053(5) -0.017(5) 0.016(5) -0.007(5) O3A 0.143(9) 0.166(10) 0.113(8) -0.014(7) 0.010(7) -0.015(8) O4A 0.209(11) 0.192(11) 0.176(10) -0.014(8) 0.042(8) -0.025(9) O5A 0.144(9) 0.171(10) 0.155(9) 0.031(8) 0.045(8) 0.029(8) O6A 0.086(7) 0.112(8) 0.111(8) 0.026(7) 0.023(6) 0.021(7) N1A 0.035(6) 0.056(8) 0.059(7) 0.001(6) 0.004(6) 0.021(6) N2A 0.042(6) 0.066(8) 0.041(6) -0.008(6) 0.007(6) 0.005(6) N3A 0.047(7) 0.060(8) 0.047(7) 0.004(6) 0.010(6) 0.001(6) N4A 0.046(6) 0.061(8) 0.039(7) 0.003(6) -0.004(5) -0.004(6) N5A 0.033(6) 0.058(8) 0.036(6) 0.008(6) 0.000(5) -0.005(6) N6A 0.042(7) 0.067(8) 0.060(7) 0.007(7) 0.015(6) 0.012(6) C1A 0.048(8) 0.070(9) 0.044(8) -0.003(7) 0.007(7) 0.005(7) C2A 0.049(8) 0.063(9) 0.050(8) 0.002(7) 0.006(7) -0.006(7) C3A 0.034(7) 0.054(9) 0.049(8) -0.007(7) -0.002(6) -0.004(6) C4A 0.041(7) 0.065(9) 0.054(8) 0.002(7) 0.003(7) 0.010(7) C5A 0.040(7) 0.067(9) 0.065(8) -0.006(8) 0.007(7) 0.014(7) C6A 0.055(8) 0.054(9) 0.049(8) -0.002(7) 0.011(7) 0.001(7) C7A 0.040(7) 0.056(9) 0.065(8) -0.002(8) 0.018(7) 0.004(7) C8A 0.052(8) 0.053(9) 0.057(8) -0.004(8) -0.004(7) -0.008(7) C9A 0.045(7) 0.043(9) 0.051(8) 0.001(7) 0.013(7) 0.006(7) C10A 0.043(7) 0.056(9) 0.052(8) 0.001(8) 0.000(7) -0.013(7) C11A 0.075(9) 0.071(9) 0.063(8) 0.002(8) 0.013(7) 0.006(8) C12A 0.076(9) 0.079(10) 0.070(9) -0.003(8) -0.006(7) 0.006(8) C13A 0.049(7) 0.049(9) 0.035(7) 0.002(8) 0.005(6) -0.001(7) C14A 0.045(7) 0.053(9) 0.037(7) -0.004(8) 0.006(6) -0.009(7) C15A 0.038(7) 0.052(9) 0.045(8) 0.015(8) -0.001(6) 0.000(7) C16A 0.039(7) 0.047(9) 0.045(8) 0.004(8) -0.010(6) -0.001(7) C17A 0.033(7) 0.049(9) 0.058(8) -0.001(8) 0.005(7) 0.004(7) C18A 0.039(7) 0.048(9) 0.054(8) -0.001(7) -0.008(7) 0.005(7) C19A 0.047(8) 0.054(9) 0.047(8) 0.001(7) -0.006(7) 0.003(7) C20A 0.038(7) 0.048(9) 0.053(8) -0.002(7) -0.010(7) 0.000(7) C21A 0.041(7) 0.050(9) 0.046(8) 0.002(7) -0.001(7) -0.002(7) C22A 0.043(7) 0.050(9) 0.046(7) 0.003(7) 0.002(6) -0.004(7) C23A 0.042(7) 0.048(9) 0.045(8) 0.005(7) -0.004(7) 0.000(7) C24A 0.037(7) 0.061(9) 0.049(8) 0.005(7) 0.004(6) -0.001(7) C25A 0.045(7) 0.058(9) 0.042(7) 0.007(7) 0.011(7) 0.000(7) C26A 0.058(8) 0.063(9) 0.064(8) 0.001(8) -0.002(7) 0.005(7) C27A 0.049(8) 0.071(9) 0.063(8) 0.005(8) 0.010(7) 0.008(7) C28A 0.079(9) 0.083(10) 0.071(9) -0.004(8) 0.009(7) 0.003(8) C29A 0.097(10) 0.128(11) 0.096(10) -0.021(9) 0.008(8) -0.024(9) C30A 0.241(16) 0.227(16) 0.227(16) -0.020(10) 0.034(10) -0.014(10) C31A 0.049(8) 0.078(9) 0.050(8) -0.005(7) 0.008(6) -0.006(7) C32A 0.079(9) 0.066(9) 0.071(9) 0.000(8) 0.018(7) 0.013(8) C33A 0.087(9) 0.082(10) 0.079(9) 0.005(8) 0.009(8) 0.005(8) C34A 0.075(9) 0.088(10) 0.080(9) -0.007(8) 0.008(7) 0.009(8) C35A 0.094(9) 0.085(10) 0.085(9) -0.008(8) 0.003(8) -0.006(8) C36A 0.079(9) 0.099(10) 0.072(9) -0.005(8) 0.002(8) 0.011(8) C37A 0.113(10) 0.129(11) 0.101(10) 0.009(8) 0.015(8) -0.004(8) C38A 0.051(8) 0.070(9) 0.065(8) 0.002(7) -0.001(7) 0.001(7) C39A 0.072(9) 0.094(10) 0.073(9) 0.012(8) 0.003(7) -0.009(8) C40A 0.063(8) 0.077(9) 0.061(8) 0.003(8) 0.004(7) -0.004(7) C41A 0.083(9) 0.080(10) 0.071(8) 0.010(8) 0.008(7) -0.001(8) C42A 0.041(7) 0.060(9) 0.059(8) -0.002(7) 0.008(7) 0.002(7) C43A 0.061(8) 0.079(9) 0.067(8) -0.018(8) 0.003(7) 0.001(7) C44A 0.041(7) 0.069(9) 0.054(8) 0.009(7) 0.008(6) 0.003(7) C45A 0.044(7) 0.058(9) 0.043(7) 0.002(7) 0.020(6) 0.011(7) C46A 0.077(9) 0.088(10) 0.090(9) 0.000(8) 0.005(8) 0.016(8) C47A 0.090(10) 0.100(11) 0.099(10) 0.011(9) 0.018(8) 0.015(8) C48A 0.094(9) 0.085(10) 0.083(9) 0.021(8) 0.006(8) -0.013(8) O1B 0.055(6) 0.089(7) 0.053(6) -0.011(6) -0.012(5) 0.004(5) N1B 0.055(7) 0.081(8) 0.061(7) -0.007(7) 0.007(6) 0.005(7) N2B 0.046(7) 0.064(8) 0.052(7) -0.017(7) -0.006(6) -0.006(6) N3B 0.028(6) 0.084(8) 0.069(7) -0.036(7) -0.010(6) 0.012(6) C1B 0.060(8) 0.068(9) 0.054(8) 0.003(8) -0.002(7) -0.007(7) C2B 0.076(9) 0.103(10) 0.081(9) -0.023(8) 0.013(8) -0.009(8) C3B 0.068(8) 0.065(9) 0.064(8) -0.008(8) 0.007(7) -0.006(8) C4B 0.070(9) 0.077(10) 0.064(9) 0.008(8) -0.002(7) 0.003(8) C5B 0.062(8) 0.087(10) 0.063(8) -0.004(8) 0.000(7) -0.006(8) C6B 0.058(8) 0.061(9) 0.060(9) -0.008(8) 0.000(7) -0.004(7) C7B 0.059(8) 0.062(9) 0.046(8) -0.002(8) -0.003(7) 0.000(7) C8B 0.065(8) 0.071(9) 0.061(8) -0.001(8) 0.004(7) 0.003(8) C9B 0.047(8) 0.072(9) 0.053(8) -0.016(8) -0.007(7) -0.003(7) C10B 0.053(8) 0.053(9) 0.062(9) -0.007(8) -0.014(7) -0.008(7) C11B 0.048(8) 0.071(9) 0.053(8) 0.002(8) -0.004(7) -0.010(7) C12B 0.047(8) 0.068(9) 0.074(9) -0.011(8) -0.001(7) -0.004(7) C13B 0.035(7) 0.068(9) 0.064(9) 0.006(8) -0.009(7) -0.004(7) C18B 0.070(9) 0.101(10) 0.108(10) -0.005(8) 0.021(8) 0.013(8) C19B 0.061(8) 0.067(9) 0.064(8) -0.009(7) -0.011(7) -0.010(7) C20B 0.097(10) 0.113(11) 0.101(10) 0.003(8) 0.018(8) -0.002(8) C21B 0.080(9) 0.086(9) 0.068(9) 0.012(8) 0.002(7) -0.011(8) C22B 0.080(9) 0.099(10) 0.082(9) 0.011(8) -0.004(7) -0.008(8) C23B 0.083(9) 0.094(10) 0.094(9) 0.004(8) -0.001(8) -0.002(8) C24B 0.141(11) 0.144(12) 0.141(11) -0.015(9) 0.017(9) -0.003(9) C14B 0.409(8) 0.414(8) 0.417(8) 0.000(7) 0.034(7) 0.000(7) C1D 0.185(14) 0.210(15) 0.194(16) 0.005(9) 0.013(10) -0.005(10) C2D 0.196(15) 0.198(15) 0.202(15) 0.003(10) 0.014(10) -0.006(10) C3D 0.221(16) 0.218(16) 0.217(15) 0.003(10) 0.009(10) -0.005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.740(9) . ? U1 O2 1.768(9) . ? U1 N3 2.519(14) . ? U1 N4 2.560(12) . ? U1 N6 2.610(13) . ? U1 N1 2.632(12) . ? U1 N5 2.684(11) . ? U1 N2 2.720(11) . ? U2 O1A 1.768(9) . ? U2 O2A 1.778(9) . ? U2 N3A 2.517(11) . ? U2 N4A 2.583(11) . ? U2 N6A 2.668(11) . ? U2 N1A 2.667(11) . ? U2 N5A 2.700(12) . ? U2 N2A 2.705(12) . ? U3 O1B 1.786(8) 2_655 ? U3 O1B 1.786(8) . ? U3 N3B 2.477(15) 2_655 ? U3 N3B 2.477(15) . ? U3 N1B 2.631(13) . ? U3 N1B 2.631(13) 2_655 ? U3 N2B 2.707(13) . ? U3 N2B 2.707(13) 2_655 ? N1 C1 1.332(17) . ? N1 C4 1.449(17) . ? N2 C9 1.330(16) . ? N2 C6 1.401(16) . ? N3 C13 1.356(16) . ? N3 C10 1.407(17) . ? N4 C14 1.294(16) . ? N4 C17 1.374(16) . ? N5 C21 1.328(16) . ? N5 C18 1.359(15) . ? N6 C26 1.320(15) . ? N6 C23 1.409(16) . ? C1 C2 1.43(2) . ? C1 C26 1.486(18) . ? C2 C3 1.354(19) . ? C2 C27 1.442(19) . ? C3 C4 1.417(18) . ? C3 C31 1.497(18) . ? C4 C5 1.381(19) . ? C5 C6 1.349(19) . ? C6 C7 1.463(19) . ? C7 C8 1.326(18) . ? C7 C32 1.480(17) . ? C8 C9 1.469(17) . ? C8 C34 1.501(18) . ? C9 C10 1.429(19) . ? C10 C11 1.371(19) . ? C11 C12 1.402(18) . ? C11 C35 1.555(19) . ? C12 C13 1.448(19) . ? C12 C36 1.475(18) . ? C13 C14 1.458(18) . ? C14 C15 1.469(18) . ? C15 C16 1.312(17) . ? C15 C38 1.491(18) . ? C16 C17 1.470(19) . ? C16 C40 1.538(17) . ? C17 C18 1.369(18) . ? C18 C19 1.492(18) . ? C19 C20 1.330(18) . ? C19 C41 1.532(17) . ? C20 C21 1.440(17) . ? C20 C42 1.484(17) . ? C21 C22 1.416(17) . ? C22 C23 1.370(16) . ? C23 C24 1.414(18) . ? C24 C25 1.388(17) . ? C24 C44 1.482(17) . ? C25 C26 1.447(19) . ? C25 C45 1.536(17) . ? C27 C28 1.524(5) . ? C28 C29 1.492(5) . ? C29 O3 1.209(5) . ? C29 O4 1.330(5) . ? C30 O4 1.453(5) . ? C32 C33 1.495(16) . ? C36 C37 1.564(17) . ? C38 C39 1.562(15) . ? C42 C43 1.543(18) . ? C45 C46 1.520(5) . ? C46 C47 1.479(4) . ? C47 O5 1.207(5) . ? C47 O6 1.335(5) . ? C48 O6 1.463(5) . ? O3A C29A 1.200(5) . ? O4A C29A 1.331(5) . ? O4A C30A 1.445(5) . ? O5A C47A 1.201(4) . ? O6A C47A 1.326(4) . ? O6A C48A 1.448(5) . ? N1A C1A 1.350(15) . ? N1A C4A 1.382(15) . ? N2A C9A 1.336(15) . ? N2A C6A 1.373(16) . ? N3A C13A 1.388(15) . ? N3A C10A 1.386(16) . ? N4A C17A 1.333(16) . ? N4A C14A 1.358(15) . ? N5A C21A 1.388(16) . ? N5A C18A 1.383(16) . ? N6A C26A 1.364(16) . ? N6A C23A 1.393(15) . ? C1A C2A 1.441(17) . ? C1A C26A 1.466(18) . ? C2A C3A 1.341(17) . ? C2A C27A 1.454(16) . ? C3A C4A 1.480(17) . ? C3A C31A 1.543(16) . ? C4A C5A 1.373(17) . ? C5A C6A 1.418(17) . ? C6A C7A 1.395(18) . ? C7A C8A 1.317(17) . ? C7A C32A 1.481(18) . ? C8A C9A 1.424(18) . ? C8A C34A 1.480(18) . ? C9A C10A 1.451(18) . ? C10A C11A 1.471(18) . ? C11A C12A 1.33(2) . ? C11A C35A 1.54(2) . ? C12A C13A 1.436(19) . ? C12A C36A 1.541(18) . ? C13A C14A 1.368(18) . ? C14A C15A 1.390(18) . ? C15A C16A 1.364(18) . ? C15A C38A 1.501(17) . ? C16A C40A 1.470(18) . ? C16A C17A 1.474(18) . ? C17A C18A 1.443(18) . ? C18A C19A 1.424(18) . ? C19A C20A 1.362(18) . ? C19A C41A 1.557(18) . ? C20A C21A 1.423(18) . ? C20A C42A 1.527(17) . ? C21A C22A 1.356(17) . ? C22A C23A 1.363(17) . ? C23A C24A 1.456(17) . ? C24A C25A 1.351(16) . ? C24A C44A 1.519(17) . ? C25A C26A 1.411(18) . ? C25A C45A 1.535(16) . ? C27A C28A 1.515(5) . ? C28A C29A 1.487(5) . ? C32A C33A 1.538(18) . ? C36A C37A 1.490(19) . ? C38A C39A 1.544(17) . ? C42A C43A 1.522(16) . ? C45A C46A 1.521(5) . ? C46A C47A 1.484(4) . ? N1B C1B 1.324(17) . ? N1B C4B 1.441(18) . ? N2B C6B 1.330(17) . ? N2B C9B 1.388(17) . ? N3B C13B 1.338(17) . ? N3B C10B 1.439(17) . ? C1B C1B 1.44(3) 2_655 ? C1B C2B 1.49(2) . ? C2B C3B 1.44(2) . ? C2B C14B 1.62(4) . ? C3B C4B 1.38(2) . ? C3B C18B 1.559(19) . ? C4B C5B 1.42(2) . ? C5B C6B 1.324(19) . ? C6B C7B 1.449(19) . ? C7B C8B 1.304(19) . ? C7B C19B 1.504(19) . ? C8B C9B 1.463(19) . ? C8B C21B 1.544(19) . ? C9B C10B 1.40(2) . ? C10B C11B 1.356(19) . ? C11B C12B 1.366(19) . ? C11B C22B 1.530(18) . ? C12B C13B 1.454(19) . ? C12B C23B 1.50(2) . ? C13B C13B 1.47(3) 2_655 ? C19B C20B 1.478(18) . ? C23B C24B 1.59(2) . ? C14B C15B 1.518(5) . ? O2B C16B 1.202(5) . ? O3B C16B 1.330(5) . ? O3B C17B 1.442(6) . ? C15B C16B 1.492(5) . ? C1D C2D 1.42(3) . ? C1D C1D 1.46(4) 2_554 ? C2D C3D 1.43(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 178.5(4) . . ? O1 U1 N3 99.9(4) . . ? O2 U1 N3 81.5(4) . . ? O1 U1 N4 83.2(4) . . ? O2 U1 N4 97.3(4) . . ? N3 U1 N4 58.0(4) . . ? O1 U1 N6 97.9(4) . . ? O2 U1 N6 80.7(4) . . ? N3 U1 N6 162.2(4) . . ? N4 U1 N6 124.1(4) . . ? O1 U1 N1 80.1(4) . . ? O2 U1 N1 99.4(4) . . ? N3 U1 N1 122.0(4) . . ? N4 U1 N1 163.0(4) . . ? N6 U1 N1 61.9(4) . . ? O1 U1 N5 87.6(4) . . ? O2 U1 N5 91.5(4) . . ? N3 U1 N5 114.7(4) . . ? N4 U1 N5 58.8(4) . . ? N6 U1 N5 65.5(4) . . ? N1 U1 N5 123.2(4) . . ? O1 U1 N2 90.7(4) . . ? O2 U1 N2 90.3(4) . . ? N3 U1 N2 57.7(4) . . ? N4 U1 N2 113.0(4) . . ? N6 U1 N2 122.8(4) . . ? N1 U1 N2 64.3(4) . . ? N5 U1 N2 171.7(4) . . ? O1A U2 O2A 179.8(4) . . ? O1A U2 N3A 97.4(4) . . ? O2A U2 N3A 82.7(4) . . ? O1A U2 N4A 82.5(4) . . ? O2A U2 N4A 97.4(4) . . ? N3A U2 N4A 58.4(4) . . ? O1A U2 N6A 99.6(4) . . ? O2A U2 N6A 80.3(4) . . ? N3A U2 N6A 162.9(4) . . ? N4A U2 N6A 122.8(4) . . ? O1A U2 N1A 82.0(4) . . ? O2A U2 N1A 98.1(4) . . ? N3A U2 N1A 123.1(4) . . ? N4A U2 N1A 164.5(3) . . ? N6A U2 N1A 61.0(4) . . ? O1A U2 N5A 88.1(4) . . ? O2A U2 N5A 91.7(4) . . ? N3A U2 N5A 115.1(4) . . ? N4A U2 N5A 58.5(4) . . ? N6A U2 N5A 64.5(4) . . ? N1A U2 N5A 121.7(3) . . ? O1A U2 N2A 90.9(4) . . ? O2A U2 N2A 89.3(4) . . ? N3A U2 N2A 58.4(4) . . ? N4A U2 N2A 114.8(4) . . ? N6A U2 N2A 122.3(4) . . ? N1A U2 N2A 64.6(3) . . ? N5A U2 N2A 173.3(3) . . ? O1B U3 O1B 179.0(7) 2_655 . ? O1B U3 N3B 97.3(4) 2_655 2_655 ? O1B U3 N3B 81.8(4) . 2_655 ? O1B U3 N3B 81.8(4) 2_655 . ? O1B U3 N3B 97.3(4) . . ? N3B U3 N3B 58.4(6) 2_655 . ? O1B U3 N1B 99.4(4) 2_655 . ? O1B U3 N1B 81.4(4) . . ? N3B U3 N1B 163.2(4) 2_655 . ? N3B U3 N1B 123.7(4) . . ? O1B U3 N1B 81.4(4) 2_655 2_655 ? O1B U3 N1B 99.4(4) . 2_655 ? N3B U3 N1B 123.7(4) 2_655 2_655 ? N3B U3 N1B 163.2(4) . 2_655 ? N1B U3 N1B 60.0(6) . 2_655 ? O1B U3 N2B 89.8(4) 2_655 . ? O1B U3 N2B 90.1(4) . . ? N3B U3 N2B 115.5(4) 2_655 . ? N3B U3 N2B 59.5(4) . . ? N1B U3 N2B 64.2(4) . . ? N1B U3 N2B 120.8(4) 2_655 . ? O1B U3 N2B 90.1(4) 2_655 2_655 ? O1B U3 N2B 89.8(4) . 2_655 ? N3B U3 N2B 59.5(4) 2_655 2_655 ? N3B U3 N2B 115.5(4) . 2_655 ? N1B U3 N2B 120.8(4) . 2_655 ? N1B U3 N2B 64.2(4) 2_655 2_655 ? N2B U3 N2B 174.9(6) . 2_655 ? C1 N1 C4 102.8(13) . . ? C1 N1 U1 118.7(11) . . ? C4 N1 U1 131.4(10) . . ? C9 N2 C6 105.6(13) . . ? C9 N2 U1 121.0(10) . . ? C6 N2 U1 131.8(11) . . ? C13 N3 C10 103.3(14) . . ? C13 N3 U1 128.4(11) . . ? C10 N3 U1 127.2(11) . . ? C14 N4 C17 109.0(15) . . ? C14 N4 U1 127.5(11) . . ? C17 N4 U1 122.8(12) . . ? C21 N5 C18 107.2(13) . . ? C21 N5 U1 134.6(10) . . ? C18 N5 U1 118.2(10) . . ? C26 N6 C23 102.4(13) . . ? C26 N6 U1 121.2(10) . . ? C23 N6 U1 131.3(11) . . ? N1 C1 C2 114.3(15) . . ? N1 C1 C26 116.2(15) . . ? C2 C1 C26 129.4(17) . . ? C3 C2 C1 105.2(17) . . ? C3 C2 C27 122.7(18) . . ? C1 C2 C27 130.3(17) . . ? C2 C3 C4 108.2(16) . . ? C2 C3 C31 129.4(18) . . ? C4 C3 C31 122.3(15) . . ? C5 C4 C3 130.6(16) . . ? C5 C4 N1 118.6(15) . . ? C3 C4 N1 109.3(14) . . ? C6 C5 C4 130.5(16) . . ? C5 C6 N2 124.7(16) . . ? C5 C6 C7 126.5(16) . . ? N2 C6 C7 108.7(15) . . ? C8 C7 C6 107.8(15) . . ? C8 C7 C32 129.6(16) . . ? C6 C7 C32 122.3(16) . . ? C7 C8 C9 105.9(15) . . ? C7 C8 C34 127.0(15) . . ? C9 C8 C34 127.0(15) . . ? N2 C9 C10 117.3(15) . . ? N2 C9 C8 111.8(14) . . ? C10 C9 C8 129.2(16) . . ? C11 C10 N3 110.7(16) . . ? C11 C10 C9 137.3(18) . . ? N3 C10 C9 109.5(16) . . ? C10 C11 C12 110.1(17) . . ? C10 C11 C35 127.4(16) . . ? C12 C11 C35 121.9(17) . . ? C11 C12 C13 101.5(15) . . ? C11 C12 C36 126.2(17) . . ? C13 C12 C36 132.2(14) . . ? N3 C13 C12 114.0(14) . . ? N3 C13 C14 109.8(15) . . ? C12 C13 C14 136.2(16) . . ? N4 C14 C13 113.6(15) . . ? N4 C14 C15 112.3(15) . . ? C13 C14 C15 133.6(16) . . ? C16 C15 C14 101.9(15) . . ? C16 C15 C38 130.7(15) . . ? C14 C15 C38 127.2(15) . . ? C15 C16 C17 112.3(15) . . ? C15 C16 C40 123.6(16) . . ? C17 C16 C40 123.9(15) . . ? C18 C17 N4 114.7(16) . . ? C18 C17 C16 140.4(16) . . ? N4 C17 C16 103.7(14) . . ? N5 C18 C17 117.6(15) . . ? N5 C18 C19 108.3(13) . . ? C17 C18 C19 132.7(15) . . ? C20 C19 C18 105.7(13) . . ? C20 C19 C41 127.6(15) . . ? C18 C19 C41 126.6(15) . . ? C19 C20 C21 107.3(14) . . ? C19 C20 C42 126.4(15) . . ? C21 C20 C42 126.1(16) . . ? N5 C21 C22 126.0(14) . . ? N5 C21 C20 111.1(14) . . ? C22 C21 C20 122.8(15) . . ? C23 C22 C21 125.5(14) . . ? C22 C23 N6 122.3(15) . . ? C22 C23 C24 125.4(15) . . ? N6 C23 C24 110.7(13) . . ? C25 C24 C23 108.3(14) . . ? C25 C24 C44 126.3(16) . . ? C23 C24 C44 125.4(14) . . ? C24 C25 C26 101.7(14) . . ? C24 C25 C45 125.6(16) . . ? C26 C25 C45 132.6(15) . . ? N6 C26 C25 116.4(14) . . ? N6 C26 C1 113.4(15) . . ? C25 C26 C1 130.3(15) . . ? C2 C27 C28 116.3(12) . . ? C29 C28 C27 112.9(5) . . ? O3 C29 O4 120.0(6) . . ? O3 C29 C28 121.7(6) . . ? O4 C29 C28 113.4(5) . . ? C29 O4 C30 114.9(6) . . ? C7 C32 C33 115.3(12) . . ? C12 C36 C37 108.8(12) . . ? C15 C38 C39 113.8(11) . . ? C20 C42 C43 112.5(12) . . ? C46 C45 C25 109.4(11) . . ? C47 C46 C45 114.9(5) . . ? O5 C47 O6 119.1(6) . . ? O5 C47 C46 123.4(6) . . ? O6 C47 C46 114.5(4) . . ? C47 O6 C48 113.3(5) . . ? C29A O4A C30A 116.0(6) . . ? C47A O6A C48A 116.9(5) . . ? C1A N1A C4A 106.9(12) . . ? C1A N1A U2 117.9(9) . . ? C4A N1A U2 127.3(10) . . ? C9A N2A C6A 100.9(12) . . ? C9A N2A U2 121.9(10) . . ? C6A N2A U2 137.2(10) . . ? C13A N3A C10A 107.4(13) . . ? C13A N3A U2 125.9(10) . . ? C10A N3A U2 124.0(10) . . ? C17A N4A C14A 108.9(14) . . ? C17A N4A U2 125.2(10) . . ? C14A N4A U2 125.5(11) . . ? C21A N5A C18A 106.7(13) . . ? C21A N5A U2 134.0(10) . . ? C18A N5A U2 119.4(9) . . ? C26A N6A C23A 102.9(12) . . ? C26A N6A U2 120.7(10) . . ? C23A N6A U2 130.4(10) . . ? N1A C1A C2A 112.9(13) . . ? N1A C1A C26A 116.5(13) . . ? C2A C1A C26A 130.1(14) . . ? C3A C2A C1A 103.7(13) . . ? C3A C2A C27A 127.4(14) . . ? C1A C2A C27A 127.1(14) . . ? C2A C3A C4A 110.0(13) . . ? C2A C3A C31A 130.0(13) . . ? C4A C3A C31A 119.9(13) . . ? C5A C4A N1A 124.8(14) . . ? C5A C4A C3A 126.5(14) . . ? N1A C4A C3A 106.0(13) . . ? C4A C5A C6A 126.2(14) . . ? N2A C6A C7A 113.6(14) . . ? N2A C6A C5A 120.9(15) . . ? C7A C6A C5A 125.4(16) . . ? C8A C7A C6A 105.9(15) . . ? C8A C7A C32A 131.2(17) . . ? C6A C7A C32A 122.1(15) . . ? C7A C8A C9A 105.8(15) . . ? C7A C8A C34A 123.4(16) . . ? C9A C8A C34A 130.0(15) . . ? N2A C9A C8A 113.3(14) . . ? N2A C9A C10A 113.0(14) . . ? C8A C9A C10A 133.5(16) . . ? N3A C10A C9A 114.2(14) . . ? N3A C10A C11A 109.9(15) . . ? C9A C10A C11A 135.0(16) . . ? C12A C11A C10A 103.4(16) . . ? C12A C11A C35A 129.8(16) . . ? C10A C11A C35A 126.6(16) . . ? C11A C12A C13A 112.7(16) . . ? C11A C12A C36A 121.0(17) . . ? C13A C12A C36A 124.9(17) . . ? C14A C13A N3A 113.2(14) . . ? C14A C13A C12A 140.6(16) . . ? N3A C13A C12A 106.2(15) . . ? C13A C14A N4A 113.0(15) . . ? C13A C14A C15A 138.2(15) . . ? N4A C14A C15A 108.7(15) . . ? C16A C15A C14A 109.4(14) . . ? C16A C15A C38A 122.2(16) . . ? C14A C15A C38A 127.9(15) . . ? C15A C16A C40A 128.8(15) . . ? C15A C16A C17A 104.1(14) . . ? C40A C16A C17A 127.1(15) . . ? N4A C17A C18A 115.5(15) . . ? N4A C17A C16A 108.5(14) . . ? C18A C17A C16A 135.4(16) . . ? N5A C18A C19A 110.2(14) . . ? N5A C18A C17A 114.1(14) . . ? C19A C18A C17A 132.1(15) . . ? C20A C19A C18A 105.6(15) . . ? C20A C19A C41A 126.6(15) . . ? C18A C19A C41A 127.4(15) . . ? C19A C20A C21A 109.6(15) . . ? C19A C20A C42A 123.8(15) . . ? C21A C20A C42A 126.6(15) . . ? C22A C21A N5A 125.3(16) . . ? C22A C21A C20A 127.0(16) . . ? N5A C21A C20A 107.7(14) . . ? C21A C22A C23A 127.7(15) . . ? C22A C23A N6A 121.4(14) . . ? C22A C23A C24A 126.8(15) . . ? N6A C23A C24A 109.8(13) . . ? C25A C24A C23A 107.3(13) . . ? C25A C24A C44A 130.2(14) . . ? C23A C24A C44A 122.5(13) . . ? C24A C25A C26A 105.3(14) . . ? C24A C25A C45A 126.5(14) . . ? C26A C25A C45A 127.4(14) . . ? N6A C26A C25A 114.4(14) . . ? N6A C26A C1A 111.2(15) . . ? C25A C26A C1A 134.4(16) . . ? C2A C27A C28A 110.3(10) . . ? C29A C28A C27A 114.2(5) . . ? O3A C29A O4A 121.0(5) . . ? O3A C29A C28A 122.9(6) . . ? O4A C29A C28A 113.4(5) . . ? C7A C32A C33A 113.5(13) . . ? C37A C36A C12A 111.7(14) . . ? C15A C38A C39A 114.3(11) . . ? C20A C42A C43A 117.7(12) . . ? C46A C45A C25A 113.1(10) . . ? C47A C46A C45A 114.4(5) . . ? O5A C47A O6A 122.2(5) . . ? O5A C47A C46A 123.3(5) . . ? O6A C47A C46A 114.5(4) . . ? C1B N1B C4B 100.2(14) . . ? C1B N1B U3 121.8(11) . . ? C4B N1B U3 133.2(12) . . ? C6B N2B C9B 106.9(15) . . ? C6B N2B U3 135.2(13) . . ? C9B N2B U3 117.9(11) . . ? C13B N3B C10B 102.4(14) . . ? C13B N3B U3 129.7(11) . . ? C10B N3B U3 127.6(11) . . ? N1B C1B C1B 115.2(10) . 2_655 ? N1B C1B C2B 117.9(15) . . ? C1B C1B C2B 126.7(12) 2_655 . ? C3B C2B C1B 99.6(17) . . ? C3B C2B C14B 119(2) . . ? C1B C2B C14B 141(2) . . ? C4B C3B C2B 108.1(17) . . ? C4B C3B C18B 126.2(17) . . ? C2B C3B C18B 125.7(18) . . ? C3B C4B C5B 128.3(19) . . ? C3B C4B N1B 113.7(17) . . ? C5B C4B N1B 116.7(17) . . ? C6B C5B C4B 129.3(18) . . ? C5B C6B N2B 125.6(18) . . ? C5B C6B C7B 124.2(18) . . ? N2B C6B C7B 109.9(17) . . ? C8B C7B C6B 107.9(17) . . ? C8B C7B C19B 130.8(17) . . ? C6B C7B C19B 121.1(17) . . ? C7B C8B C9B 107.1(17) . . ? C7B C8B C21B 125.3(17) . . ? C9B C8B C21B 127.4(17) . . ? N2B C9B C10B 118.2(16) . . ? N2B C9B C8B 107.8(16) . . ? C10B C9B C8B 132.9(19) . . ? C11B C10B C9B 138.1(19) . . ? C11B C10B N3B 109.6(16) . . ? C9B C10B N3B 111.2(16) . . ? C10B C11B C12B 111.6(17) . . ? C10B C11B C22B 130.2(18) . . ? C12B C11B C22B 118.2(18) . . ? C11B C12B C13B 101.7(16) . . ? C11B C12B C23B 127.7(18) . . ? C13B C12B C23B 130.5(17) . . ? N3B C13B C12B 114.3(14) . . ? N3B C13B C13B 110.5(9) . 2_655 ? C12B C13B C13B 135.2(11) . 2_655 ? C20B C19B C7B 112.9(13) . . ? C12B C23B C24B 112.2(15) . . ? C15B C14B C2B 101(3) . . ? C16B O3B C17B 116.8(7) . . ? C16B C15B C14B 113.3(6) . . ? O2B C16B O3B 121.8(7) . . ? O2B C16B C15B 121.5(7) . . ? O3B C16B C15B 113.3(6) . . ? C2D C1D C1D 131(4) . 2_554 ? C1D C2D C3D 123(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 U1 N1 C1 -95.9(12) . . . . ? O2 U1 N1 C1 82.7(12) . . . . ? N3 U1 N1 C1 168.6(11) . . . . ? N4 U1 N1 C1 -106.6(18) . . . . ? N6 U1 N1 C1 8.7(11) . . . . ? N5 U1 N1 C1 -15.4(13) . . . . ? N2 U1 N1 C1 168.5(13) . . . . ? O1 U1 N1 C4 49.2(13) . . . . ? O2 U1 N1 C4 -132.2(13) . . . . ? N3 U1 N1 C4 -46.4(14) . . . . ? N4 U1 N1 C4 38(2) . . . . ? N6 U1 N1 C4 153.7(14) . . . . ? N5 U1 N1 C4 129.6(12) . . . . ? N2 U1 N1 C4 -46.5(12) . . . . ? O1 U1 N2 C9 115.6(11) . . . . ? O2 U1 N2 C9 -65.4(11) . . . . ? N3 U1 N2 C9 14.3(10) . . . . ? N4 U1 N2 C9 32.7(11) . . . . ? N6 U1 N2 C9 -144.5(10) . . . . ? N1 U1 N2 C9 -165.7(12) . . . . ? N5 U1 N2 C9 38(3) . . . . ? O1 U1 N2 C6 -48.0(12) . . . . ? O2 U1 N2 C6 130.9(12) . . . . ? N3 U1 N2 C6 -149.4(13) . . . . ? N4 U1 N2 C6 -131.0(12) . . . . ? N6 U1 N2 C6 51.8(13) . . . . ? N1 U1 N2 C6 30.6(11) . . . . ? N5 U1 N2 C6 -126(2) . . . . ? O1 U1 N3 C13 84.3(11) . . . . ? O2 U1 N3 C13 -95.5(11) . . . . ? N4 U1 N3 C13 8.7(10) . . . . ? N6 U1 N3 C13 -94.0(17) . . . . ? N1 U1 N3 C13 168.7(10) . . . . ? N5 U1 N3 C13 -7.7(12) . . . . ? N2 U1 N3 C13 168.7(12) . . . . ? O1 U1 N3 C10 -109.9(11) . . . . ? O2 U1 N3 C10 70.3(11) . . . . ? N4 U1 N3 C10 174.5(12) . . . . ? N6 U1 N3 C10 71.8(18) . . . . ? N1 U1 N3 C10 -25.5(12) . . . . ? N5 U1 N3 C10 158.1(10) . . . . ? N2 U1 N3 C10 -25.5(10) . . . . ? O1 U1 N4 C14 -103.0(12) . . . . ? O2 U1 N4 C14 78.3(12) . . . . ? N3 U1 N4 C14 3.1(11) . . . . ? N6 U1 N4 C14 162.0(11) . . . . ? N1 U1 N4 C14 -92(2) . . . . ? N5 U1 N4 C14 165.7(14) . . . . ? N2 U1 N4 C14 -15.2(13) . . . . ? O1 U1 N4 C17 66.4(11) . . . . ? O2 U1 N4 C17 -112.3(11) . . . . ? N3 U1 N4 C17 172.5(12) . . . . ? N6 U1 N4 C17 -28.6(12) . . . . ? N1 U1 N4 C17 77.0(19) . . . . ? N5 U1 N4 C17 -25.0(10) . . . . ? N2 U1 N4 C17 154.2(10) . . . . ? O1 U1 N5 C21 118.8(14) . . . . ? O2 U1 N5 C21 -60.0(15) . . . . ? N3 U1 N5 C21 -141.4(14) . . . . ? N4 U1 N5 C21 -157.7(16) . . . . ? N6 U1 N5 C21 19.0(14) . . . . ? N1 U1 N5 C21 42.3(15) . . . . ? N2 U1 N5 C21 -163(2) . . . . ? O1 U1 N5 C18 -62.5(11) . . . . ? O2 U1 N5 C18 118.8(11) . . . . ? N3 U1 N5 C18 37.4(11) . . . . ? N4 U1 N5 C18 21.1(10) . . . . ? N6 U1 N5 C18 -162.2(12) . . . . ? N1 U1 N5 C18 -138.9(10) . . . . ? N2 U1 N5 C18 16(3) . . . . ? O1 U1 N6 C26 85.3(11) . . . . ? O2 U1 N6 C26 -94.9(11) . . . . ? N3 U1 N6 C26 -96.4(17) . . . . ? N4 U1 N6 C26 172.5(10) . . . . ? N1 U1 N6 C26 11.1(11) . . . . ? N5 U1 N6 C26 169.0(12) . . . . ? N2 U1 N6 C26 -10.6(13) . . . . ? O1 U1 N6 C23 -124.7(12) . . . . ? O2 U1 N6 C23 55.1(12) . . . . ? N3 U1 N6 C23 54(2) . . . . ? N4 U1 N6 C23 -37.5(14) . . . . ? N1 U1 N6 C23 161.1(13) . . . . ? N5 U1 N6 C23 -41.0(12) . . . . ? N2 U1 N6 C23 139.4(12) . . . . ? C4 N1 C1 C2 -0.8(18) . . . . ? U1 N1 C1 C2 153.0(10) . . . . ? C4 N1 C1 C26 -179.4(12) . . . . ? U1 N1 C1 C26 -25.5(18) . . . . ? N1 C1 C2 C3 -1(2) . . . . ? C26 C1 C2 C3 177.6(15) . . . . ? N1 C1 C2 C27 -165.3(16) . . . . ? C26 C1 C2 C27 13(3) . . . . ? C1 C2 C3 C4 1.9(18) . . . . ? C27 C2 C3 C4 168.0(14) . . . . ? C1 C2 C3 C31 -179.6(15) . . . . ? C27 C2 C3 C31 -14(3) . . . . ? C2 C3 C4 C5 163.2(16) . . . . ? C31 C3 C4 C5 -15(3) . . . . ? C2 C3 C4 N1 -2.6(18) . . . . ? C31 C3 C4 N1 178.9(13) . . . . ? C1 N1 C4 C5 -165.7(14) . . . . ? U1 N1 C4 C5 45.3(19) . . . . ? C1 N1 C4 C3 2.0(16) . . . . ? U1 N1 C4 C3 -146.9(11) . . . . ? C3 C4 C5 C6 -166.2(16) . . . . ? N1 C4 C5 C6 -2(3) . . . . ? C4 C5 C6 N2 -13(3) . . . . ? C4 C5 C6 C7 163.8(15) . . . . ? C9 N2 C6 C5 -179.2(15) . . . . ? U1 N2 C6 C5 -14(2) . . . . ? C9 N2 C6 C7 3.6(16) . . . . ? U1 N2 C6 C7 169.1(9) . . . . ? C5 C6 C7 C8 -179.3(15) . . . . ? N2 C6 C7 C8 -2.1(17) . . . . ? C5 C6 C7 C32 6(2) . . . . ? N2 C6 C7 C32 -176.4(12) . . . . ? C6 C7 C8 C9 -0.1(17) . . . . ? C32 C7 C8 C9 173.6(14) . . . . ? C6 C7 C8 C34 -176.2(13) . . . . ? C32 C7 C8 C34 -2(3) . . . . ? C6 N2 C9 C10 162.8(12) . . . . ? U1 N2 C9 C10 -4.6(17) . . . . ? C6 N2 C9 C8 -3.7(16) . . . . ? U1 N2 C9 C8 -171.1(8) . . . . ? C7 C8 C9 N2 2.5(18) . . . . ? C34 C8 C9 N2 178.6(13) . . . . ? C7 C8 C9 C10 -162.0(15) . . . . ? C34 C8 C9 C10 14(3) . . . . ? C13 N3 C10 C11 6.4(16) . . . . ? U1 N3 C10 C11 -162.2(10) . . . . ? C13 N3 C10 C9 -158.6(12) . . . . ? U1 N3 C10 C9 32.7(16) . . . . ? N2 C9 C10 C11 -174.2(18) . . . . ? C8 C9 C10 C11 -10(3) . . . . ? N2 C9 C10 N3 -15.0(18) . . . . ? C8 C9 C10 N3 148.8(15) . . . . ? N3 C10 C11 C12 -4.5(18) . . . . ? C9 C10 C11 C12 154.5(17) . . . . ? N3 C10 C11 C35 166.5(14) . . . . ? C9 C10 C11 C35 -35(3) . . . . ? C10 C11 C12 C13 0.6(16) . . . . ? C35 C11 C12 C13 -170.9(13) . . . . ? C10 C11 C12 C36 179.1(13) . . . . ? C35 C11 C12 C36 8(2) . . . . ? C10 N3 C13 C12 -6.2(15) . . . . ? U1 N3 C13 C12 162.2(9) . . . . ? C10 N3 C13 C14 174.4(11) . . . . ? U1 N3 C13 C14 -17.2(16) . . . . ? C11 C12 C13 N3 3.7(16) . . . . ? C36 C12 C13 N3 -174.7(14) . . . . ? C11 C12 C13 C14 -177.2(16) . . . . ? C36 C12 C13 C14 4(3) . . . . ? C17 N4 C14 C13 177.0(11) . . . . ? U1 N4 C14 C13 -12.4(18) . . . . ? C17 N4 C14 C15 -9.4(17) . . . . ? U1 N4 C14 C15 161.2(9) . . . . ? N3 C13 C14 N4 17.1(17) . . . . ? C12 C13 C14 N4 -162.1(15) . . . . ? N3 C13 C14 C15 -154.8(14) . . . . ? C12 C13 C14 C15 26(3) . . . . ? N4 C14 C15 C16 6.4(16) . . . . ? C13 C14 C15 C16 178.3(14) . . . . ? N4 C14 C15 C38 -168.5(13) . . . . ? C13 C14 C15 C38 3(2) . . . . ? C14 C15 C16 C17 -1.0(16) . . . . ? C38 C15 C16 C17 173.7(13) . . . . ? C14 C15 C16 C40 -175.3(12) . . . . ? C38 C15 C16 C40 -1(2) . . . . ? C14 N4 C17 C18 -161.8(13) . . . . ? U1 N4 C17 C18 27.0(17) . . . . ? C14 N4 C17 C16 8.0(16) . . . . ? U1 N4 C17 C16 -163.1(8) . . . . ? C15 C16 C17 C18 161.4(19) . . . . ? C40 C16 C17 C18 -24(3) . . . . ? C15 C16 C17 N4 -4.1(17) . . . . ? C40 C16 C17 N4 170.1(12) . . . . ? C21 N5 C18 C17 161.6(14) . . . . ? U1 N5 C18 C17 -17.5(18) . . . . ? C21 N5 C18 C19 -7.0(17) . . . . ? U1 N5 C18 C19 173.9(8) . . . . ? N4 C17 C18 N5 -5(2) . . . . ? C16 C17 C18 N5 -169.0(17) . . . . ? N4 C17 C18 C19 160.6(15) . . . . ? C16 C17 C18 C19 -4(3) . . . . ? N5 C18 C19 C20 5.6(18) . . . . ? C17 C18 C19 C20 -160.6(17) . . . . ? N5 C18 C19 C41 -178.3(14) . . . . ? C17 C18 C19 C41 16(3) . . . . ? C18 C19 C20 C21 -2.0(17) . . . . ? C41 C19 C20 C21 -178.0(14) . . . . ? C18 C19 C20 C42 -177.2(14) . . . . ? C41 C19 C20 C42 7(3) . . . . ? C18 N5 C21 C22 -178.2(14) . . . . ? U1 N5 C21 C22 1(2) . . . . ? C18 N5 C21 C20 6.0(18) . . . . ? U1 N5 C21 C20 -175.2(9) . . . . ? C19 C20 C21 N5 -2.4(19) . . . . ? C42 C20 C21 N5 172.9(14) . . . . ? C19 C20 C21 C22 -178.4(15) . . . . ? C42 C20 C21 C22 -3(2) . . . . ? N5 C21 C22 C23 -16(3) . . . . ? C20 C21 C22 C23 159.2(15) . . . . ? C21 C22 C23 N6 -7(3) . . . . ? C21 C22 C23 C24 -171.4(16) . . . . ? C26 N6 C23 C22 -160.0(15) . . . . ? U1 N6 C23 C22 46(2) . . . . ? C26 N6 C23 C24 6.9(17) . . . . ? U1 N6 C23 C24 -147.1(11) . . . . ? C22 C23 C24 C25 161.1(15) . . . . ? N6 C23 C24 C25 -5.3(19) . . . . ? C22 C23 C24 C44 -21(3) . . . . ? N6 C23 C24 C44 172.8(14) . . . . ? C23 C24 C25 C26 1.4(18) . . . . ? C44 C24 C25 C26 -176.7(15) . . . . ? C23 C24 C25 C45 178.3(14) . . . . ? C44 C24 C25 C45 0(3) . . . . ? C23 N6 C26 C25 -6.3(18) . . . . ? U1 N6 C26 C25 151.1(11) . . . . ? C23 N6 C26 C1 175.5(13) . . . . ? U1 N6 C26 C1 -27.2(17) . . . . ? C24 C25 C26 N6 3.3(19) . . . . ? C45 C25 C26 N6 -173.4(15) . . . . ? C24 C25 C26 C1 -178.8(16) . . . . ? C45 C25 C26 C1 5(3) . . . . ? N1 C1 C26 N6 34(2) . . . . ? C2 C1 C26 N6 -143.7(16) . . . . ? N1 C1 C26 C25 -143.5(17) . . . . ? C2 C1 C26 C25 38(3) . . . . ? C3 C2 C27 C28 79(2) . . . . ? C1 C2 C27 C28 -118.6(19) . . . . ? C2 C27 C28 C29 156.3(16) . . . . ? C27 C28 C29 O3 -26(3) . . . . ? C27 C28 C29 O4 178.9(17) . . . . ? O3 C29 O4 C30 3(3) . . . . ? C28 C29 O4 C30 159(2) . . . . ? C8 C7 C32 C33 116.8(19) . . . . ? C6 C7 C32 C33 -70.3(19) . . . . ? C11 C12 C36 C37 -111.2(16) . . . . ? C13 C12 C36 C37 66.9(19) . . . . ? C16 C15 C38 C39 -116.5(17) . . . . ? C14 C15 C38 C39 56.9(19) . . . . ? C19 C20 C42 C43 91(2) . . . . ? C21 C20 C42 C43 -83.9(18) . . . . ? C24 C25 C45 C46 -104.6(18) . . . . ? C26 C25 C45 C46 71(2) . . . . ? C25 C45 C46 C47 -179.6(12) . . . . ? C45 C46 C47 O5 -125(2) . . . . ? C45 C46 C47 O6 35(2) . . . . ? O5 C47 O6 C48 -13(3) . . . . ? C46 C47 O6 C48 -174.3(15) . . . . ? O1A U2 N1A C1A -93.3(11) . . . . ? O2A U2 N1A C1A 86.5(11) . . . . ? N3A U2 N1A C1A 173.0(10) . . . . ? N4A U2 N1A C1A -96.5(17) . . . . ? N6A U2 N1A C1A 12.3(10) . . . . ? N5A U2 N1A C1A -10.6(12) . . . . ? N2A U2 N1A C1A 171.9(12) . . . . ? O1A U2 N1A C4A 51.4(12) . . . . ? O2A U2 N1A C4A -128.8(12) . . . . ? N3A U2 N1A C4A -42.3(13) . . . . ? N4A U2 N1A C4A 48(2) . . . . ? N6A U2 N1A C4A 157.0(13) . . . . ? N5A U2 N1A C4A 134.1(11) . . . . ? N2A U2 N1A C4A -43.4(11) . . . . ? O1A U2 N2A C9A 117.3(11) . . . . ? O2A U2 N2A C9A -62.7(11) . . . . ? N3A U2 N2A C9A 19.1(10) . . . . ? N4A U2 N2A C9A 35.2(12) . . . . ? N6A U2 N2A C9A -140.8(10) . . . . ? N1A U2 N2A C9A -162.0(12) . . . . ? N5A U2 N2A C9A 36(3) . . . . ? O1A U2 N2A C6A -62.3(14) . . . . ? O2A U2 N2A C6A 117.7(14) . . . . ? N3A U2 N2A C6A -160.5(15) . . . . ? N4A U2 N2A C6A -144.5(13) . . . . ? N6A U2 N2A C6A 39.6(15) . . . . ? N1A U2 N2A C6A 18.4(13) . . . . ? N5A U2 N2A C6A -143(3) . . . . ? O1A U2 N3A C13A 88.3(11) . . . . ? O2A U2 N3A C13A -91.5(11) . . . . ? N4A U2 N3A C13A 12.0(10) . . . . ? N6A U2 N3A C13A -87.5(18) . . . . ? N1A U2 N3A C13A 173.6(10) . . . . ? N5A U2 N3A C13A -3.0(12) . . . . ? N2A U2 N3A C13A 174.8(12) . . . . ? O1A U2 N3A C10A -112.8(11) . . . . ? O2A U2 N3A C10A 67.4(11) . . . . ? N4A U2 N3A C10A 170.8(12) . . . . ? N6A U2 N3A C10A 71.4(18) . . . . ? N1A U2 N3A C10A -27.5(12) . . . . ? N5A U2 N3A C10A 155.9(10) . . . . ? N2A U2 N3A C10A -26.3(10) . . . . ? O1A U2 N4A C17A 69.6(11) . . . . ? O2A U2 N4A C17A -110.2(11) . . . . ? N3A U2 N4A C17A 173.1(12) . . . . ? N6A U2 N4A C17A -27.0(12) . . . . ? N1A U2 N4A C17A 72.8(19) . . . . ? N5A U2 N4A C17A -22.8(10) . . . . ? N2A U2 N4A C17A 157.0(10) . . . . ? O1A U2 N4A C14A -102.7(11) . . . . ? O2A U2 N4A C14A 77.5(11) . . . . ? N3A U2 N4A C14A 0.9(10) . . . . ? N6A U2 N4A C14A 160.7(10) . . . . ? N1A U2 N4A C14A -99.4(17) . . . . ? N5A U2 N4A C14A 165.0(12) . . . . ? N2A U2 N4A C14A -15.2(12) . . . . ? O1A U2 N5A C21A 120.0(12) . . . . ? O2A U2 N5A C21A -60.0(12) . . . . ? N3A U2 N5A C21A -142.7(11) . . . . ? N4A U2 N5A C21A -157.7(12) . . . . ? N6A U2 N5A C21A 18.4(11) . . . . ? N1A U2 N5A C21A 40.6(12) . . . . ? N2A U2 N5A C21A -159(3) . . . . ? O1A U2 N5A C18A -59.6(9) . . . . ? O2A U2 N5A C18A 120.4(9) . . . . ? N3A U2 N5A C18A 37.7(10) . . . . ? N4A U2 N5A C18A 22.8(9) . . . . ? N6A U2 N5A C18A -161.2(10) . . . . ? N1A U2 N5A C18A -139.0(9) . . . . ? N2A U2 N5A C18A 22(3) . . . . ? O1A U2 N6A C26A 86.0(11) . . . . ? O2A U2 N6A C26A -94.2(11) . . . . ? N3A U2 N6A C26A -98.1(17) . . . . ? N4A U2 N6A C26A 173.2(10) . . . . ? N1A U2 N6A C26A 10.8(10) . . . . ? N5A U2 N6A C26A 169.2(12) . . . . ? N2A U2 N6A C26A -11.1(12) . . . . ? O1A U2 N6A C23A -126.2(13) . . . . ? O2A U2 N6A C23A 53.6(13) . . . . ? N3A U2 N6A C23A 50(2) . . . . ? N4A U2 N6A C23A -39.1(14) . . . . ? N1A U2 N6A C23A 158.5(14) . . . . ? N5A U2 N6A C23A -43.0(12) . . . . ? N2A U2 N6A C23A 136.6(12) . . . . ? C4A N1A C1A C2A 2.8(18) . . . . ? U2 N1A C1A C2A 154.1(10) . . . . ? C4A N1A C1A C26A 175.2(14) . . . . ? U2 N1A C1A C26A -33.5(18) . . . . ? N1A C1A C2A C3A -6.5(19) . . . . ? C26A C1A C2A C3A -177.6(16) . . . . ? N1A C1A C2A C27A -171.9(14) . . . . ? C26A C1A C2A C27A 17(3) . . . . ? C1A C2A C3A C4A 7.3(18) . . . . ? C27A C2A C3A C4A 172.6(14) . . . . ? C1A C2A C3A C31A -176.2(14) . . . . ? C27A C2A C3A C31A -11(3) . . . . ? C1A N1A C4A C5A -160.9(15) . . . . ? U2 N1A C4A C5A 51(2) . . . . ? C1A N1A C4A C3A 1.7(16) . . . . ? U2 N1A C4A C3A -146.0(9) . . . . ? C2A C3A C4A C5A 156.2(16) . . . . ? C31A C3A C4A C5A -21(2) . . . . ? C2A C3A C4A N1A -6.0(18) . . . . ? C31A C3A C4A N1A 177.0(12) . . . . ? N1A C4A C5A C6A -8(3) . . . . ? C3A C4A C5A C6A -166.6(15) . . . . ? C9A N2A C6A C7A 4.3(17) . . . . ? U2 N2A C6A C7A -176.0(10) . . . . ? C9A N2A C6A C5A -174.5(14) . . . . ? U2 N2A C6A C5A 5(2) . . . . ? C4A C5A C6A N2A -21(2) . . . . ? C4A C5A C6A C7A 160.3(16) . . . . ? N2A C6A C7A C8A 0.2(19) . . . . ? C5A C6A C7A C8A 178.8(15) . . . . ? N2A C6A C7A C32A 171.3(13) . . . . ? C5A C6A C7A C32A -10(2) . . . . ? C6A C7A C8A C9A -4.3(17) . . . . ? C32A C7A C8A C9A -174.3(15) . . . . ? C6A C7A C8A C34A -175.2(15) . . . . ? C32A C7A C8A C34A 15(3) . . . . ? C6A N2A C9A C8A -7.1(17) . . . . ? U2 N2A C9A C8A 173.2(9) . . . . ? C6A N2A C9A C10A 168.5(12) . . . . ? U2 N2A C9A C10A -11.3(17) . . . . ? C7A C8A C9A N2A 7.7(19) . . . . ? C34A C8A C9A N2A 177.7(15) . . . . ? C7A C8A C9A C10A -166.7(16) . . . . ? C34A C8A C9A C10A 3(3) . . . . ? C13A N3A C10A C9A -165.5(11) . . . . ? U2 N3A C10A C9A 32.3(16) . . . . ? C13A N3A C10A C11A 5.6(16) . . . . ? U2 N3A C10A C11A -156.6(9) . . . . ? N2A C9A C10A N3A -11.4(18) . . . . ? C8A C9A C10A N3A 163.0(16) . . . . ? N2A C9A C10A C11A -179.5(16) . . . . ? C8A C9A C10A C11A -5(3) . . . . ? N3A C10A C11A C12A -6.5(18) . . . . ? C9A C10A C11A C12A 162.0(17) . . . . ? N3A C10A C11A C35A 169.5(14) . . . . ? C9A C10A C11A C35A -22(3) . . . . ? C10A C11A C12A C13A 4.9(19) . . . . ? C35A C11A C12A C13A -170.9(15) . . . . ? C10A C11A C12A C36A 172.2(14) . . . . ? C35A C11A C12A C36A -4(3) . . . . ? C10A N3A C13A C14A 175.2(12) . . . . ? U2 N3A C13A C14A -23.0(17) . . . . ? C10A N3A C13A C12A -2.5(16) . . . . ? U2 N3A C13A C12A 159.2(10) . . . . ? C11A C12A C13A C14A -178.5(18) . . . . ? C36A C12A C13A C14A 15(3) . . . . ? C11A C12A C13A N3A -1.8(19) . . . . ? C36A C12A C13A N3A -168.4(14) . . . . ? N3A C13A C14A N4A 20.7(18) . . . . ? C12A C13A C14A N4A -162.7(18) . . . . ? N3A C13A C14A C15A -162.0(16) . . . . ? C12A C13A C14A C15A 15(3) . . . . ? C17A N4A C14A C13A 174.4(12) . . . . ? U2 N4A C14A C13A -12.3(17) . . . . ? C17A N4A C14A C15A -3.7(16) . . . . ? U2 N4A C14A C15A 169.6(8) . . . . ? C13A C14A C15A C16A -177.9(17) . . . . ? N4A C14A C15A C16A -0.5(17) . . . . ? C13A C14A C15A C38A 11(3) . . . . ? N4A C14A C15A C38A -172.0(13) . . . . ? C14A C15A C16A C40A -173.8(13) . . . . ? C38A C15A C16A C40A -2(2) . . . . ? C14A C15A C16A C17A 4.0(16) . . . . ? C38A C15A C16A C17A 176.0(12) . . . . ? C14A N4A C17A C18A -166.0(12) . . . . ? U2 N4A C17A C18A 20.7(17) . . . . ? C14A N4A C17A C16A 6.2(16) . . . . ? U2 N4A C17A C16A -167.2(8) . . . . ? C15A C16A C17A N4A -6.3(16) . . . . ? C40A C16A C17A N4A 171.5(13) . . . . ? C15A C16A C17A C18A 163.6(16) . . . . ? C40A C16A C17A C18A -19(3) . . . . ? C21A N5A C18A C19A -3.9(15) . . . . ? U2 N5A C18A C19A 175.8(8) . . . . ? C21A N5A C18A C17A 157.4(11) . . . . ? U2 N5A C18A C17A -22.9(15) . . . . ? N4A C17A C18A N5A 2.9(18) . . . . ? C16A C17A C18A N5A -166.5(15) . . . . ? N4A C17A C18A C19A 159.0(15) . . . . ? C16A C17A C18A C19A -10(3) . . . . ? N5A C18A C19A C20A 3.9(16) . . . . ? C17A C18A C19A C20A -152.8(16) . . . . ? N5A C18A C19A C41A -169.4(12) . . . . ? C17A C18A C19A C41A 34(3) . . . . ? C18A C19A C20A C21A -2.4(16) . . . . ? C41A C19A C20A C21A 171.0(13) . . . . ? C18A C19A C20A C42A -179.5(12) . . . . ? C41A C19A C20A C42A -6(2) . . . . ? C18A N5A C21A C22A -177.7(13) . . . . ? U2 N5A C21A C22A 3(2) . . . . ? C18A N5A C21A C20A 2.3(15) . . . . ? U2 N5A C21A C20A -177.3(8) . . . . ? C19A C20A C21A C22A -179.9(14) . . . . ? C42A C20A C21A C22A -3(2) . . . . ? C19A C20A C21A N5A 0.1(16) . . . . ? C42A C20A C21A N5A 177.1(12) . . . . ? N5A C21A C22A C23A -18(2) . . . . ? C20A C21A C22A C23A 161.7(14) . . . . ? C21A C22A C23A N6A -7(2) . . . . ? C21A C22A C23A C24A -169.1(14) . . . . ? C26A N6A C23A C22A -158.9(14) . . . . ? U2 N6A C23A C22A 49.2(19) . . . . ? C26A N6A C23A C24A 5.7(16) . . . . ? U2 N6A C23A C24A -146.2(10) . . . . ? C22A C23A C24A C25A 158.7(14) . . . . ? N6A C23A C24A C25A -4.9(17) . . . . ? C22A C23A C24A C44A -21(2) . . . . ? N6A C23A C24A C44A 175.0(12) . . . . ? C23A C24A C25A C26A 1.8(17) . . . . ? C44A C24A C25A C26A -178.0(14) . . . . ? C23A C24A C25A C45A 171.8(13) . . . . ? C44A C24A C25A C45A -8(3) . . . . ? C23A N6A C26A C25A -4.8(17) . . . . ? U2 N6A C26A C25A 150.5(10) . . . . ? C23A N6A C26A C1A 174.6(13) . . . . ? U2 N6A C26A C1A -30.0(17) . . . . ? C24A C25A C26A N6A 1.9(19) . . . . ? C45A C25A C26A N6A -167.9(13) . . . . ? C24A C25A C26A C1A -177.3(17) . . . . ? C45A C25A C26A C1A 13(3) . . . . ? N1A C1A C26A N6A 42(2) . . . . ? C2A C1A C26A N6A -147.6(16) . . . . ? N1A C1A C26A C25A -139.2(18) . . . . ? C2A C1A C26A C25A 32(3) . . . . ? C3A C2A C27A C28A -72(2) . . . . ? C1A C2A C27A C28A 89.5(18) . . . . ? C2A C27A C28A C29A -174.9(12) . . . . ? C30A O4A C29A O3A -11(3) . . . . ? C30A O4A C29A C28A -172.9(18) . . . . ? C27A C28A C29A O3A 42(2) . . . . ? C27A C28A C29A O4A -156.1(16) . . . . ? C8A C7A C32A C33A 93(2) . . . . ? C6A C7A C32A C33A -76(2) . . . . ? C11A C12A C36A C37A 82(2) . . . . ? C13A C12A C36A C37A -111.9(19) . . . . ? C16A C15A C38A C39A -86.7(18) . . . . ? C14A C15A C38A C39A 83.7(19) . . . . ? C19A C20A C42A C43A 83.7(18) . . . . ? C21A C20A C42A C43A -93.0(18) . . . . ? C24A C25A C45A C46A 68.3(19) . . . . ? C26A C25A C45A C46A -123.8(16) . . . . ? C25A C45A C46A C47A -179.4(11) . . . . ? C48A O6A C47A O5A 3(3) . . . . ? C48A O6A C47A C46A -179.2(12) . . . . ? C45A C46A C47A O5A 131.8(18) . . . . ? C45A C46A C47A O6A -46.3(18) . . . . ? O1B U3 N1B C1B 82.6(12) 2_655 . . . ? O1B U3 N1B C1B -97.9(12) . . . . ? N3B U3 N1B C1B -99.4(18) 2_655 . . . ? N3B U3 N1B C1B 168.9(11) . . . . ? N1B U3 N1B C1B 8.3(9) 2_655 . . . ? N2B U3 N1B C1B 167.8(13) . . . . ? N2B U3 N1B C1B -13.3(13) 2_655 . . . ? O1B U3 N1B C4B -127.1(14) 2_655 . . . ? O1B U3 N1B C4B 52.4(14) . . . . ? N3B U3 N1B C4B 51(2) 2_655 . . . ? N3B U3 N1B C4B -40.7(15) . . . . ? N1B U3 N1B C4B 158.6(17) 2_655 . . . ? N2B U3 N1B C4B -41.9(13) . . . . ? N2B U3 N1B C4B 137.1(13) 2_655 . . . ? O1B U3 N2B C6B 116.5(14) 2_655 . . . ? O1B U3 N2B C6B -64.5(14) . . . . ? N3B U3 N2B C6B -145.5(13) 2_655 . . . ? N3B U3 N2B C6B -163.0(14) . . . . ? N1B U3 N2B C6B 15.9(13) . . . . ? N1B U3 N2B C6B 36.6(14) 2_655 . . . ? N2B U3 N2B C6B -154.0(13) 2_655 . . . ? O1B U3 N2B C9B -62.3(10) 2_655 . . . ? O1B U3 N2B C9B 116.7(10) . . . . ? N3B U3 N2B C9B 35.8(11) 2_655 . . . ? N3B U3 N2B C9B 18.3(9) . . . . ? N1B U3 N2B C9B -162.8(11) . . . . ? N1B U3 N2B C9B -142.2(9) 2_655 . . . ? N2B U3 N2B C9B 27.3(9) 2_655 . . . ? O1B U3 N3B C13B -99.7(12) 2_655 . . . ? O1B U3 N3B C13B 79.8(12) . . . . ? N3B U3 N3B C13B 4.2(9) 2_655 . . . ? N1B U3 N3B C13B 164.4(11) . . . . ? N1B U3 N3B C13B -98.3(18) 2_655 . . . ? N2B U3 N3B C13B 165.6(13) . . . . ? N2B U3 N3B C13B -13.5(13) 2_655 . . . ? O1B U3 N3B C10B 72.9(11) 2_655 . . . ? O1B U3 N3B C10B -107.6(11) . . . . ? N3B U3 N3B C10B 176.8(14) 2_655 . . . ? N1B U3 N3B C10B -23.0(12) . . . . ? N1B U3 N3B C10B 74.3(19) 2_655 . . . ? N2B U3 N3B C10B -21.8(10) . . . . ? N2B U3 N3B C10B 159.0(10) 2_655 . . . ? C4B N1B C1B C1B 179.2(16) . . . 2_655 ? U3 N1B C1B C1B -22(2) . . . 2_655 ? C4B N1B C1B C2B -6.6(19) . . . . ? U3 N1B C1B C2B 151.9(11) . . . . ? N1B C1B C2B C3B 3(2) . . . . ? C1B C1B C2B C3B 176.7(19) 2_655 . . . ? N1B C1B C2B C14B 178(2) . . . . ? C1B C1B C2B C14B -9(4) 2_655 . . . ? C1B C2B C3B C4B 2.0(18) . . . . ? C14B C2B C3B C4B -173.9(15) . . . . ? C1B C2B C3B C18B -176.6(15) . . . . ? C14B C2B C3B C18B 8(3) . . . . ? C2B C3B C4B C5B 159.7(16) . . . . ? C18B C3B C4B C5B -22(3) . . . . ? C2B C3B C4B N1B -6(2) . . . . ? C18B C3B C4B N1B 172.2(14) . . . . ? C1B N1B C4B C3B 7.8(18) . . . . ? U3 N1B C4B C3B -146.9(12) . . . . ? C1B N1B C4B C5B -160.0(15) . . . . ? U3 N1B C4B C5B 45(2) . . . . ? C3B C4B C5B C6B -167.2(17) . . . . ? N1B C4B C5B C6B -2(3) . . . . ? C4B C5B C6B N2B -24(3) . . . . ? C4B C5B C6B C7B 162.0(16) . . . . ? C9B N2B C6B C5B -173.7(15) . . . . ? U3 N2B C6B C5B 7(3) . . . . ? C9B N2B C6B C7B 1.4(17) . . . . ? U3 N2B C6B C7B -177.4(9) . . . . ? C5B C6B C7B C8B 177.4(16) . . . . ? N2B C6B C7B C8B 2.3(19) . . . . ? C5B C6B C7B C19B -6(2) . . . . ? N2B C6B C7B C19B 178.3(13) . . . . ? C6B C7B C8B C9B -4.7(18) . . . . ? C19B C7B C8B C9B 179.7(15) . . . . ? C6B C7B C8B C21B 179.8(14) . . . . ? C19B C7B C8B C21B 4(3) . . . . ? C6B N2B C9B C10B 165.1(13) . . . . ? U3 N2B C9B C10B -15.8(17) . . . . ? C6B N2B C9B C8B -4.2(16) . . . . ? U3 N2B C9B C8B 174.9(9) . . . . ? C7B C8B C9B N2B 5.7(18) . . . . ? C21B C8B C9B N2B -179.0(14) . . . . ? C7B C8B C9B C10B -161.4(16) . . . . ? C21B C8B C9B C10B 14(3) . . . . ? N2B C9B C10B C11B -167.8(17) . . . . ? C8B C9B C10B C11B -2(3) . . . . ? N2B C9B C10B N3B -1.6(19) . . . . ? C8B C9B C10B N3B 164.5(15) . . . . ? C13B N3B C10B C11B 6.8(16) . . . . ? U3 N3B C10B C11B -167.4(9) . . . . ? C13B N3B C10B C9B -163.4(12) . . . . ? U3 N3B C10B C9B 22.4(17) . . . . ? C9B C10B C11B C12B 160.6(18) . . . . ? N3B C10B C11B C12B -5.7(18) . . . . ? C9B C10B C11B C22B -19(3) . . . . ? N3B C10B C11B C22B 174.3(14) . . . . ? C10B C11B C12B C13B 2.0(17) . . . . ? C22B C11B C12B C13B -177.9(12) . . . . ? C10B C11B C12B C23B -175.5(14) . . . . ? C22B C11B C12B C23B 5(2) . . . . ? C10B N3B C13B C12B -5.7(16) . . . . ? U3 N3B C13B C12B 168.2(9) . . . . ? C10B N3B C13B C13B 175.8(14) . . . 2_655 ? U3 N3B C13B C13B -10(2) . . . 2_655 ? C11B C12B C13B N3B 2.6(17) . . . . ? C23B C12B C13B N3B -179.9(14) . . . . ? C11B C12B C13B C13B -179(2) . . . 2_655 ? C23B C12B C13B C13B -2(3) . . . 2_655 ? C8B C7B C19B C20B 97(2) . . . . ? C6B C7B C19B C20B -78.0(18) . . . . ? C11B C12B C23B C24B 78(2) . . . . ? C13B C12B C23B C24B -99(2) . . . . ? C3B C2B C14B C15B -133.9(16) . . . . ? C1B C2B C14B C15B 53(3) . . . . ? C2B C14B C15B C16B 79(4) . . . . ? C17B O3B C16B O2B 1(5) . . . . ? C17B O3B C16B C15B -159(4) . . . . ? C14B C15B C16B O2B 21(5) . . . . ? C14B C15B C16B O3B -180(4) . . . . ? C1D C1D C2D C3D 171.9(19) 2_554 . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 23.75 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.808 _refine_diff_density_min -1.426 _refine_diff_density_rms 0.165