####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_opl0911 _database_code_depnum_ccdc_archive 'CCDC 759475' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H76 N O5 U, C4 H10 O2' _chemical_formula_sum 'C62 H86 N O7 U' _chemical_formula_weight 1195.35 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(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.672(2) _cell_length_b 11.219(2) _cell_length_c 38.622(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.067(8) _cell_angle_gamma 90.00 _cell_volume 5477.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 191 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 3.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 0.60 \% and 33 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57996 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.10 _reflns_number_total 11997 _reflns_number_gt 8556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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 (AdArO)3N ligand is subjected to rotational disorder around the central U-N axis. Two preferred orientations were refined resulting in occupancies of 83.9(9) % for the major component and 16.1(3) % for the minor component (denoted by an additional A). SIMU, ISOR, SADI and FLAT restraints were applied in the refinement of the disordered structure parts. ; _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^)+(0.0325P)^2^+11.0330P] 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 11997 _refine_ls_number_parameters 834 _refine_ls_number_restraints 394 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.428549(13) 0.128036(15) 0.634891(4) 0.01965(6) Uani 1 1 d . . . O1 O 0.3441(3) 0.0157(3) 0.59481(10) 0.0236(9) Uani 0.839(3) 1 d PU A 1 O2 O 0.4022(3) 0.0816(3) 0.69042(10) 0.0269(9) Uani 0.839(3) 1 d PU A 1 O3 O 0.5963(3) 0.1437(3) 0.62415(12) 0.0249(9) Uani 0.839(3) 1 d PU A 1 O1A O 0.4061(16) 0.0450(17) 0.5798(5) 0.022(3) Uani 0.161(3) 1 d PU A 2 O2A O 0.3284(16) 0.0446(17) 0.6693(5) 0.023(3) Uani 0.161(3) 1 d PU A 2 O3A O 0.5923(15) 0.1535(17) 0.6476(6) 0.023(3) Uani 0.161(3) 1 d PU A 2 N1 N 0.5062(3) -0.0870(3) 0.64454(9) 0.0188(8) Uani 1 1 d . A . C1 C 0.4225(5) -0.1770(5) 0.63403(15) 0.0208(12) Uani 0.839(3) 1 d PU A 1 H1A H 0.4458 -0.2562 0.6429 0.025 Uiso 0.839(3) 1 calc PR A 1 H1B H 0.3568 -0.1559 0.6450 0.025 Uiso 0.839(3) 1 calc PR A 1 C2 C 0.3990(4) -0.1849(5) 0.59571(14) 0.0195(10) Uani 0.839(3) 1 d PU A 1 C3 C 0.3577(4) -0.0856(5) 0.57719(15) 0.0208(11) Uani 0.839(3) 1 d PU A 1 C4 C 0.3342(6) -0.0945(7) 0.54060(19) 0.0228(13) Uani 0.839(3) 1 d PU A 1 C5 C 0.3521(5) -0.2047(7) 0.52537(19) 0.0225(13) Uani 0.839(3) 1 d PU A 1 H5A H 0.3362 -0.2121 0.5010 0.027 Uiso 0.839(3) 1 calc PR A 1 C6 C 0.3914(6) -0.3043(6) 0.54334(17) 0.0235(13) Uani 0.839(3) 1 d PU A 1 C7 C 0.4162(4) -0.2914(5) 0.57828(15) 0.0215(11) Uani 0.839(3) 1 d PU A 1 H7A H 0.4459 -0.3571 0.5910 0.026 Uiso 0.839(3) 1 calc PR A 1 C1A C 0.553(2) -0.122(3) 0.6079(7) 0.021(3) Uani 0.161(3) 1 d PU A 2 H1AA H 0.5947 -0.0546 0.5999 0.025 Uiso 0.161(3) 1 calc PR A 2 H1AB H 0.6011 -0.1911 0.6117 0.025 Uiso 0.161(3) 1 calc PR A 2 C2A C 0.4676(16) -0.1547(17) 0.5790(5) 0.021(2) Uani 0.161(3) 1 d PGU A 2 C3A C 0.404(2) -0.0640(16) 0.5644(6) 0.020(3) Uani 0.161(3) 1 d PGU A 2 C4A C 0.333(2) -0.088(2) 0.5361(7) 0.021(3) Uani 0.161(3) 1 d PGU A 2 C5A C 0.326(2) -0.202(3) 0.5223(7) 0.021(3) Uani 0.161(3) 1 d PGU A 2 H5AA H 0.2776 -0.2184 0.5030 0.026 Uiso 0.161(3) 1 calc PR A 2 C6A C 0.390(2) -0.293(2) 0.5368(7) 0.021(2) Uani 0.161(3) 1 d PGU A 2 C7A C 0.4603(19) -0.2691(15) 0.5652(6) 0.021(2) Uani 0.161(3) 1 d PGU A 2 H7AA H 0.5037 -0.3310 0.5751 0.026 Uiso 0.161(3) 1 calc PR A 2 C8 C 0.5388(4) -0.1073(5) 0.68246(13) 0.0215(12) Uani 0.839(3) 1 d PU A 1 H8A H 0.5808 -0.1816 0.6847 0.026 Uiso 0.839(3) 1 calc PR A 1 H8B H 0.5853 -0.0408 0.6908 0.026 Uiso 0.839(3) 1 calc PR A 1 C9 C 0.4490(4) -0.1165(5) 0.70545(13) 0.0232(10) Uani 0.839(3) 1 d PU A 1 C10 C 0.3812(5) -0.0183(5) 0.70798(14) 0.0231(10) Uani 0.839(3) 1 d PU A 1 C11 C 0.2939(5) -0.0278(6) 0.72901(16) 0.0225(12) Uani 0.839(3) 1 d PU A 1 C12 C 0.2791(7) -0.1377(8) 0.74496(19) 0.0282(13) Uani 0.839(3) 1 d PDU A 1 H12A H 0.2191 -0.1464 0.7582 0.034 Uiso 0.839(3) 1 calc PR A 1 C13 C 0.3457(6) -0.2349(7) 0.74288(17) 0.0289(14) Uani 0.839(3) 1 d PDU A 1 C14 C 0.4299(5) -0.2227(5) 0.72242(14) 0.0253(11) Uani 0.839(3) 1 d PDU A 1 H14A H 0.4759 -0.2885 0.7199 0.030 Uiso 0.839(3) 1 calc PR A 1 C8A C 0.425(3) -0.174(3) 0.6502(9) 0.023(3) Uani 0.161(3) 1 d PU A 2 H8AA H 0.4552 -0.2549 0.6499 0.028 Uiso 0.161(3) 1 calc PR A 2 H8AB H 0.3678 -0.1679 0.6315 0.028 Uiso 0.161(3) 1 calc PR A 2 C9A C 0.3800(17) -0.1487(16) 0.6859(4) 0.0233(17) Uani 0.161(3) 1 d PGU A 2 C10A C 0.3248(18) -0.0453(16) 0.6928(6) 0.0230(17) Uani 0.161(3) 1 d PGU A 2 C11A C 0.271(2) -0.037(2) 0.7228(7) 0.023(3) Uani 0.161(3) 1 d PGU A 2 C12A C 0.272(3) -0.132(3) 0.7459(6) 0.025(3) Uani 0.161(3) 1 d PGDU A 2 H12B H 0.2349 -0.1265 0.7664 0.029 Uiso 0.161(3) 1 calc PR A 2 C13A C 0.327(3) -0.236(2) 0.7390(5) 0.025(2) Uani 0.161(3) 1 d PGDU A 2 C14A C 0.3812(19) -0.2438(16) 0.7090(5) 0.025(2) Uani 0.161(3) 1 d PGDU A 2 H14B H 0.4189 -0.3144 0.7043 0.030 Uiso 0.161(3) 1 calc PR A 2 C15 C 0.5974(4) -0.1071(5) 0.62388(15) 0.0211(12) Uani 0.839(3) 1 d PU A 1 H15A H 0.5736 -0.0939 0.5992 0.025 Uiso 0.839(3) 1 calc PR A 1 H15B H 0.6173 -0.1921 0.6263 0.025 Uiso 0.839(3) 1 calc PR A 1 C16 C 0.6954(4) -0.0344(5) 0.63166(14) 0.0200(10) Uani 0.839(3) 1 d PU A 1 C17 C 0.6915(4) 0.0901(5) 0.62759(15) 0.0202(10) Uani 0.839(3) 1 d PU A 1 C18 C 0.7877(6) 0.1550(6) 0.62630(18) 0.0216(12) Uani 0.839(3) 1 d PU A 1 C19 C 0.8802(6) 0.0900(8) 0.6313(3) 0.0239(12) Uani 0.839(3) 1 d PU A 1 H19A H 0.9451 0.1320 0.6308 0.029 Uiso 0.839(3) 1 calc PR A 1 C20 C 0.8852(5) -0.0308(7) 0.6368(2) 0.0228(12) Uani 0.839(3) 1 d PU A 1 C21 C 0.7921(4) -0.0922(5) 0.63675(15) 0.0215(11) Uani 0.839(3) 1 d PU A 1 H21A H 0.7936 -0.1760 0.6402 0.026 Uiso 0.839(3) 1 calc PR A 1 C15A C 0.593(2) -0.079(3) 0.6690(8) 0.020(3) Uani 0.161(3) 1 d PU A 2 H15C H 0.6122 -0.1608 0.6769 0.024 Uiso 0.161(3) 1 calc PR A 2 H15D H 0.5708 -0.0346 0.6894 0.024 Uiso 0.161(3) 1 calc PR A 2 C16A C 0.6911(14) -0.0193(17) 0.6563(6) 0.0202(16) Uani 0.161(3) 1 d PGU A 2 C17A C 0.6892(18) 0.0993(17) 0.6458(6) 0.0204(15) Uani 0.161(3) 1 d PGU A 2 C18A C 0.778(2) 0.150(2) 0.6329(9) 0.020(3) Uani 0.161(3) 1 d PGU A 2 C19A C 0.869(2) 0.083(3) 0.6304(12) 0.021(3) Uani 0.161(3) 1 d PGU A 2 H19B H 0.9302 0.1174 0.6215 0.025 Uiso 0.161(3) 1 calc PR A 2 C20A C 0.8712(17) -0.036(3) 0.6408(11) 0.021(2) Uani 0.161(3) 1 d PGU A 2 C21A C 0.7821(18) -0.0870(18) 0.6537(7) 0.021(2) Uani 0.161(3) 1 d PGU A 2 H21B H 0.7834 -0.1681 0.6609 0.025 Uiso 0.161(3) 1 calc PR A 2 C22 C 0.2912(4) 0.0126(4) 0.51837(12) 0.0296(12) Uani 1 1 d . . . C23 C 0.2348(7) 0.0921(7) 0.45843(17) 0.068(2) Uani 1 1 d . . . H23A H 0.2225 0.0695 0.4334 0.082 Uiso 1 1 calc R A . C24 C 0.3369(6) 0.2213(6) 0.49934(17) 0.065(2) Uani 1 1 d . . . H24A H 0.3920 0.2852 0.5014 0.078 Uiso 1 1 calc R A . C25 C 0.1513(5) 0.1725(6) 0.51147(15) 0.0480(16) Uani 1 1 d . . . H25A H 0.0844 0.2039 0.5203 0.058 Uiso 1 1 calc R A . C26 C 0.2696(6) -0.0208(6) 0.48025(14) 0.0552(19) Uani 1 1 d . A . H26A H 0.2130 -0.0817 0.4779 0.066 Uiso 1 1 calc R . . H26B H 0.3343 -0.0552 0.4713 0.066 Uiso 1 1 calc R . . C27 C 0.3180(8) 0.1867(7) 0.46218(18) 0.079(3) Uani 1 1 d . A . H27A H 0.3845 0.1566 0.4534 0.095 Uiso 1 1 calc R . . H27B H 0.2949 0.2573 0.4483 0.095 Uiso 1 1 calc R . . C28 C 0.2352(5) 0.2683(5) 0.51284(16) 0.0510(18) Uani 1 1 d . A . H28A H 0.2492 0.2959 0.5371 0.061 Uiso 1 1 calc R . . H28B H 0.2096 0.3373 0.4986 0.061 Uiso 1 1 calc R . . C29 C 0.1913(4) 0.0636(5) 0.53286(14) 0.0365(13) Uani 1 1 d . A . H29A H 0.2071 0.0874 0.5574 0.044 Uiso 1 1 calc R . . H29B H 0.1356 0.0016 0.5322 0.044 Uiso 1 1 calc R . . C30 C 0.1318(7) 0.1321(8) 0.47206(19) 0.086(3) Uani 1 1 d . A . H30A H 0.0801 0.0659 0.4703 0.104 Uiso 1 1 calc R . . H30B H 0.1022 0.1994 0.4579 0.104 Uiso 1 1 calc R . . C31 C 0.3764(5) 0.1126(5) 0.52045(17) 0.0480(16) Uani 1 1 d . A . H31A H 0.3924 0.1360 0.5450 0.058 Uiso 1 1 calc R . . H31B H 0.4424 0.0823 0.5113 0.058 Uiso 1 1 calc R . . C32 C 0.4027(5) -0.4211(5) 0.52451(14) 0.0415(15) Uani 1 1 d . . . H32A H 0.4064 -0.4866 0.5413 0.062 Uiso 0.839(3) 1 calc PR A 1 H32B H 0.4675 -0.4197 0.5121 0.062 Uiso 0.839(3) 1 calc PR A 1 H32C H 0.3415 -0.4327 0.5079 0.062 Uiso 0.839(3) 1 calc PR A 1 H32D H 0.4053 -0.4750 0.5445 0.062 Uiso 0.161(3) 1 calc PR A 2 H32E H 0.4685 -0.4280 0.5128 0.062 Uiso 0.161(3) 1 calc PR A 2 H32F H 0.3427 -0.4426 0.5083 0.062 Uiso 0.161(3) 1 calc PR A 2 C33 C 0.2173(4) 0.0772(5) 0.73286(12) 0.0258(11) Uani 1 1 d . . . C34 C 0.0539(7) 0.1529(7) 0.7596(2) 0.076(3) Uani 1 1 d . . . H34A H -0.0049 0.1287 0.7741 0.091 Uiso 1 1 calc R A . C35 C 0.0949(6) 0.2297(8) 0.70382(17) 0.067(2) Uani 1 1 d . . . H35A H 0.0642 0.2577 0.6807 0.081 Uiso 1 1 calc R A . C36 C 0.2051(5) 0.2887(6) 0.7559(2) 0.062(2) Uani 1 1 d . . . H36A H 0.2456 0.3552 0.7679 0.075 Uiso 1 1 calc R A . C37 C 0.1297(5) 0.0460(6) 0.75643(18) 0.0574(19) Uani 1 1 d . A . H37A H 0.1614 0.0240 0.7797 0.069 Uiso 1 1 calc R . . H37B H 0.0895 -0.0235 0.7468 0.069 Uiso 1 1 calc R . . C38 C 0.0082(6) 0.1943(7) 0.7251(3) 0.083(3) Uani 1 1 d . A . H38A H -0.0337 0.1295 0.7134 0.099 Uiso 1 1 calc R . . H38B H -0.0394 0.2630 0.7281 0.099 Uiso 1 1 calc R . . C39 C 0.1585(6) 0.3285(6) 0.72089(18) 0.059(2) Uani 1 1 d . A . H39A H 0.1127 0.3989 0.7236 0.070 Uiso 1 1 calc R . . H39B H 0.2159 0.3516 0.7062 0.070 Uiso 1 1 calc R . . C40 C 0.2791(5) 0.1804(5) 0.75046(17) 0.0453(15) Uani 1 1 d . A . H40A H 0.3366 0.2051 0.7359 0.054 Uiso 1 1 calc R . . H40B H 0.3117 0.1538 0.7732 0.054 Uiso 1 1 calc R . . C41 C 0.1154(6) 0.2476(8) 0.77759(16) 0.074(3) Uani 1 1 d . A . H41A H 0.1454 0.2180 0.8004 0.088 Uiso 1 1 calc R . . H41B H 0.0685 0.3159 0.7818 0.088 Uiso 1 1 calc R . . C42 C 0.1653(5) 0.1207(6) 0.69862(15) 0.0576(19) Uani 1 1 d . A . H42A H 0.1219 0.0558 0.6876 0.069 Uiso 1 1 calc R . . H42B H 0.2206 0.1420 0.6828 0.069 Uiso 1 1 calc R . . C43 C 0.3230(10) -0.3499(7) 0.7611(4) 0.044(2) Uani 0.839(3) 1 d PDU A 1 H43A H 0.3844 -0.4029 0.7607 0.067 Uiso 0.839(3) 1 calc PR A 1 H43B H 0.2612 -0.3885 0.7492 0.067 Uiso 0.839(3) 1 calc PR A 1 H43C H 0.3087 -0.3331 0.7852 0.067 Uiso 0.839(3) 1 calc PR A 1 C43A C 0.330(5) -0.347(3) 0.7631(19) 0.045(5) Uani 0.161(3) 1 d PDU A 2 H43D H 0.2590 -0.3626 0.7704 0.068 Uiso 0.161(3) 1 calc PR A 2 H43E H 0.3785 -0.3318 0.7836 0.068 Uiso 0.161(3) 1 calc PR A 2 H43F H 0.3549 -0.4159 0.7505 0.068 Uiso 0.161(3) 1 calc PR A 2 C44 C 0.7862(4) 0.2880(4) 0.61925(12) 0.0213(10) Uani 1 1 d . . . C45 C 0.8974(4) 0.4688(5) 0.60595(14) 0.0340(13) Uani 1 1 d . . . H45A H 0.9712 0.4960 0.6028 0.041 Uiso 1 1 calc R A . C46 C 0.7425(4) 0.4928(4) 0.64135(15) 0.0353(13) Uani 1 1 d . . . H46A H 0.7141 0.5370 0.6612 0.042 Uiso 1 1 calc R A . C47 C 0.7158(5) 0.4496(5) 0.57796(15) 0.0422(15) Uani 1 1 d . . . H47A H 0.6698 0.4656 0.5563 0.051 Uiso 1 1 calc R A . C48 C 0.8972(4) 0.3345(4) 0.61397(14) 0.0283(12) Uani 1 1 d . A . H48A H 0.9265 0.2906 0.5946 0.034 Uiso 1 1 calc R . . H48B H 0.9437 0.3191 0.6352 0.034 Uiso 1 1 calc R . . C49 C 0.8538(4) 0.5357(5) 0.63625(15) 0.0371(14) Uani 1 1 d . A . H49A H 0.8998 0.5215 0.6577 0.044 Uiso 1 1 calc R . . H49B H 0.8530 0.6223 0.6314 0.044 Uiso 1 1 calc R . . C50 C 0.6716(4) 0.5152(5) 0.60864(16) 0.0414(15) Uani 1 1 d . A . H50A H 0.6680 0.6018 0.6037 0.050 Uiso 1 1 calc R . . H50B H 0.5992 0.4865 0.6120 0.050 Uiso 1 1 calc R . . C51 C 0.7178(5) 0.3149(5) 0.58553(14) 0.0379(14) Uani 1 1 d . A . H51A H 0.7468 0.2720 0.5659 0.046 Uiso 1 1 calc R . . H51B H 0.6447 0.2862 0.5878 0.046 Uiso 1 1 calc R . . C52 C 0.8278(5) 0.4927(5) 0.57321(15) 0.0476(16) Uani 1 1 d . A . H52A H 0.8564 0.4507 0.5534 0.057 Uiso 1 1 calc R . . H52B H 0.8269 0.5792 0.5681 0.057 Uiso 1 1 calc R . . C53 C 0.7435(4) 0.3586(4) 0.64929(13) 0.0296(12) Uani 1 1 d . A . H53A H 0.7884 0.3433 0.6709 0.036 Uiso 1 1 calc R . . H53B H 0.6708 0.3317 0.6530 0.036 Uiso 1 1 calc R . . C54 C 0.9873(4) -0.0985(5) 0.63995(18) 0.0466(16) Uani 1 1 d . . . H54A H 0.9790 -0.1699 0.6541 0.070 Uiso 0.839(3) 1 calc PR A 1 H54B H 1.0431 -0.0479 0.6510 0.070 Uiso 0.839(3) 1 calc PR A 1 H54C H 1.0067 -0.1219 0.6168 0.070 Uiso 0.839(3) 1 calc PR A 1 H54D H 0.9887 -0.1723 0.6536 0.070 Uiso 0.161(3) 1 calc PR A 2 H54E H 1.0417 -0.0438 0.6499 0.070 Uiso 0.161(3) 1 calc PR A 2 H54F H 1.0013 -0.1169 0.6159 0.070 Uiso 0.161(3) 1 calc PR A 2 O4 O 0.4376(3) 0.3496(3) 0.65911(9) 0.0321(9) Uani 1 1 d . A . O5 O 0.2928(3) 0.2835(3) 0.60744(9) 0.0350(9) Uani 1 1 d . A . C55 C 0.4800(5) 0.3836(6) 0.69278(14) 0.0451(15) Uani 1 1 d . . . H55A H 0.5248 0.4542 0.6910 0.068 Uiso 1 1 calc R A . H55B H 0.5224 0.3180 0.7032 0.068 Uiso 1 1 calc R . . H55C H 0.4220 0.4020 0.7074 0.068 Uiso 1 1 calc R . . C56 C 0.3712(5) 0.4403(5) 0.64277(15) 0.0388(14) Uani 1 1 d . . . H56A H 0.4100 0.5168 0.6423 0.047 Uiso 1 1 calc R A . H56B H 0.3074 0.4522 0.6558 0.047 Uiso 1 1 calc R . . C57 C 0.3404(5) 0.3992(5) 0.60657(15) 0.0399(14) Uani 1 1 d . A . H57A H 0.2897 0.4564 0.5951 0.048 Uiso 1 1 calc R . . H57B H 0.4038 0.3959 0.5930 0.048 Uiso 1 1 calc R . . C58 C 0.1807(4) 0.2841(6) 0.60997(15) 0.0452(16) Uani 1 1 d . . . H58A H 0.1464 0.3241 0.5896 0.068 Uiso 1 1 calc R A . H58B H 0.1640 0.3267 0.6311 0.068 Uiso 1 1 calc R . . H58C H 0.1550 0.2019 0.6110 0.068 Uiso 1 1 calc R . . O6 O 0.1238(3) 0.6211(4) 0.64121(11) 0.0532(11) Uani 1 1 d . . . O7 O 0.1398(3) 0.5710(3) 0.56731(10) 0.0414(10) Uani 1 1 d . . . C59 C 0.1604(6) 0.6429(6) 0.67525(17) 0.0613(19) Uani 1 1 d . . . H59A H 0.1256 0.5885 0.6907 0.092 Uiso 1 1 calc R . . H59B H 0.1444 0.7254 0.6813 0.092 Uiso 1 1 calc R . . H59C H 0.2371 0.6302 0.6778 0.092 Uiso 1 1 calc R . . C60 C 0.1784(4) 0.6908(6) 0.61772(15) 0.0434(15) Uani 1 1 d . . . H60A H 0.2520 0.6614 0.6173 0.052 Uiso 1 1 calc R . . H60B H 0.1812 0.7746 0.6258 0.052 Uiso 1 1 calc R . . C61 C 0.1248(4) 0.6855(5) 0.58138(14) 0.0365(13) Uani 1 1 d . . . H61A H 0.0482 0.7018 0.5822 0.044 Uiso 1 1 calc R . . H61B H 0.1553 0.7467 0.5666 0.044 Uiso 1 1 calc R . . C62 C 0.0942(5) 0.5637(7) 0.53300(16) 0.0606(19) Uani 1 1 d . . . H62A H 0.1067 0.4842 0.5236 0.091 Uiso 1 1 calc R . . H62B H 0.1263 0.6239 0.5186 0.091 Uiso 1 1 calc R . . H62C H 0.0179 0.5781 0.5329 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02006(9) 0.01311(9) 0.02589(9) -0.00079(9) 0.00235(6) 0.00219(9) O1 0.029(2) 0.016(2) 0.024(2) 0.0014(17) -0.0044(17) 0.0005(18) O2 0.033(2) 0.020(2) 0.028(2) 0.0022(18) 0.0081(18) 0.0029(18) O3 0.0194(19) 0.012(2) 0.043(3) 0.006(2) 0.0021(19) 0.0031(16) O1A 0.028(5) 0.014(5) 0.023(5) 0.006(5) -0.005(5) -0.002(5) O2A 0.029(5) 0.016(5) 0.023(5) 0.002(5) 0.006(5) 0.004(5) O3A 0.019(5) 0.010(5) 0.040(5) 0.006(5) 0.006(5) 0.007(4) N1 0.019(2) 0.0145(19) 0.023(2) -0.0026(16) -0.0008(16) -0.0004(16) C1 0.026(3) 0.013(2) 0.023(3) 0.000(3) 0.001(3) 0.000(2) C2 0.021(2) 0.015(2) 0.022(2) -0.0011(19) 0.0018(19) -0.0017(19) C3 0.021(2) 0.015(2) 0.026(2) -0.001(2) 0.002(2) -0.003(2) C4 0.025(3) 0.019(3) 0.024(3) 0.000(2) 0.003(2) 0.001(2) C5 0.024(3) 0.024(3) 0.020(3) -0.003(2) 0.002(2) 0.001(3) C6 0.027(3) 0.017(3) 0.027(3) -0.003(2) 0.004(2) 0.000(2) C7 0.022(2) 0.016(2) 0.025(2) 0.001(2) -0.0006(19) 0.000(2) C1A 0.021(5) 0.019(5) 0.022(5) -0.001(4) 0.000(4) 0.003(4) C2A 0.023(4) 0.018(4) 0.023(4) 0.000(3) -0.002(3) 0.002(3) C3A 0.022(5) 0.018(5) 0.021(5) 0.000(5) -0.001(5) 0.003(5) C4A 0.023(6) 0.020(6) 0.021(6) -0.001(5) -0.002(5) 0.002(5) C5A 0.023(5) 0.019(5) 0.022(6) 0.000(5) -0.002(5) 0.002(5) C6A 0.024(4) 0.018(4) 0.022(4) 0.000(4) -0.001(4) 0.001(4) C7A 0.023(4) 0.017(4) 0.023(4) 0.001(4) -0.001(4) 0.002(4) C8 0.027(3) 0.018(3) 0.018(2) 0.001(2) -0.002(2) 0.004(2) C9 0.029(2) 0.022(2) 0.018(2) -0.001(2) -0.0049(18) 0.002(2) C10 0.027(2) 0.023(2) 0.019(2) -0.002(2) -0.0028(19) -0.001(2) C11 0.027(3) 0.024(2) 0.017(2) -0.001(2) -0.001(2) 0.000(2) C12 0.032(3) 0.033(3) 0.020(2) 0.000(2) 0.004(2) -0.003(3) C13 0.033(3) 0.029(3) 0.024(3) 0.003(2) -0.002(2) -0.002(2) C14 0.031(3) 0.023(2) 0.021(2) 0.001(2) -0.006(2) 0.002(2) C8A 0.026(6) 0.019(6) 0.023(6) 0.000(6) -0.004(6) 0.001(5) C9A 0.028(3) 0.022(3) 0.020(3) -0.001(3) -0.004(3) 0.000(3) C10A 0.027(3) 0.023(3) 0.018(3) -0.001(3) -0.004(3) 0.000(3) C11A 0.028(5) 0.022(5) 0.018(5) 0.000(5) -0.004(5) 0.000(5) C12A 0.030(5) 0.024(5) 0.019(5) 0.000(5) -0.003(5) 0.001(5) C13A 0.030(4) 0.023(4) 0.021(4) 0.002(4) -0.005(4) 0.001(4) C14A 0.031(4) 0.022(4) 0.021(4) 0.001(4) -0.005(3) 0.000(4) C15 0.027(3) 0.011(3) 0.025(3) 0.000(2) 0.004(2) 0.003(2) C16 0.025(2) 0.0140(19) 0.022(2) -0.0011(18) 0.0057(18) 0.0008(18) C17 0.023(2) 0.016(2) 0.022(2) 0.001(2) 0.004(2) 0.0040(18) C18 0.025(2) 0.017(2) 0.023(3) 0.000(2) 0.001(2) 0.001(2) C19 0.023(3) 0.020(3) 0.029(3) -0.002(2) 0.002(2) 0.001(2) C20 0.022(2) 0.018(2) 0.029(3) 0.000(2) 0.000(2) 0.000(2) C21 0.027(2) 0.013(2) 0.025(2) 0.001(2) 0.003(2) 0.0036(18) C15A 0.024(6) 0.014(5) 0.022(6) 0.003(5) 0.003(5) 0.002(5) C16A 0.024(3) 0.014(3) 0.022(3) 0.001(3) 0.004(3) 0.002(3) C17A 0.024(3) 0.015(3) 0.022(3) 0.000(3) 0.003(3) 0.002(3) C18A 0.024(5) 0.014(5) 0.022(5) 0.000(5) 0.002(5) 0.003(4) C19A 0.024(5) 0.015(5) 0.024(5) -0.001(5) 0.002(5) 0.002(5) C20A 0.025(4) 0.014(4) 0.024(4) 0.001(4) 0.002(4) 0.003(4) C21A 0.026(4) 0.013(3) 0.024(4) 0.002(4) 0.002(4) 0.003(3) C22 0.044(3) 0.023(3) 0.022(3) 0.003(2) 0.008(2) 0.005(2) C23 0.101(6) 0.073(6) 0.029(3) -0.006(3) 0.002(4) 0.023(5) C24 0.108(6) 0.034(4) 0.059(4) 0.019(3) 0.043(4) 0.021(4) C25 0.048(4) 0.053(4) 0.042(4) 0.007(3) -0.003(3) 0.026(3) C26 0.100(5) 0.040(4) 0.025(3) 0.004(3) 0.001(3) 0.030(4) C27 0.143(8) 0.051(5) 0.048(4) 0.019(4) 0.029(5) 0.023(5) C28 0.086(5) 0.032(3) 0.037(3) 0.013(3) 0.020(3) 0.032(4) C29 0.033(3) 0.040(3) 0.037(3) 0.006(3) 0.001(2) 0.011(3) C30 0.100(6) 0.097(7) 0.057(5) 0.020(5) -0.033(4) 0.030(6) C31 0.052(4) 0.028(3) 0.067(4) 0.006(3) 0.030(3) 0.005(3) C32 0.063(4) 0.029(3) 0.033(3) -0.008(3) 0.007(3) 0.007(3) C33 0.028(3) 0.029(3) 0.019(2) 0.002(2) 0.001(2) 0.000(2) C34 0.087(6) 0.062(5) 0.088(6) 0.003(5) 0.065(5) 0.006(4) C35 0.053(4) 0.108(7) 0.040(4) 0.008(4) -0.009(3) 0.041(5) C36 0.060(5) 0.028(3) 0.096(6) -0.011(4) -0.020(4) 0.005(3) C37 0.060(4) 0.048(4) 0.068(5) 0.010(4) 0.035(4) 0.012(3) C38 0.039(4) 0.069(5) 0.139(8) 0.007(6) -0.007(5) 0.021(4) C39 0.067(5) 0.039(4) 0.075(5) 0.018(4) 0.040(4) 0.022(4) C40 0.042(4) 0.028(3) 0.064(4) -0.003(3) -0.007(3) -0.001(3) C41 0.098(6) 0.098(7) 0.027(3) 0.001(4) 0.018(4) 0.058(5) C42 0.070(4) 0.067(5) 0.034(3) -0.013(4) -0.012(3) 0.036(4) C43 0.061(4) 0.034(4) 0.039(4) 0.012(3) 0.008(3) -0.006(3) C43A 0.056(8) 0.038(8) 0.043(8) 0.008(7) 0.008(7) -0.004(7) C44 0.022(3) 0.015(2) 0.027(3) -0.001(2) 0.002(2) -0.002(2) C45 0.034(3) 0.024(3) 0.045(3) 0.009(3) 0.012(3) 0.000(2) C46 0.045(3) 0.016(3) 0.046(3) -0.003(2) 0.016(3) 0.001(2) C47 0.055(4) 0.025(3) 0.044(4) 0.012(3) -0.018(3) 0.004(3) C48 0.028(3) 0.024(3) 0.034(3) 0.001(2) 0.009(2) 0.000(2) C49 0.042(3) 0.020(3) 0.050(4) -0.007(3) 0.007(3) -0.006(3) C50 0.037(3) 0.019(3) 0.069(4) 0.009(3) 0.006(3) 0.007(2) C51 0.049(4) 0.027(3) 0.036(3) -0.001(3) -0.012(3) 0.001(3) C52 0.071(4) 0.030(3) 0.042(4) 0.012(3) 0.008(3) 0.001(3) C53 0.038(3) 0.017(3) 0.035(3) 0.002(2) 0.012(2) -0.003(2) C54 0.035(3) 0.025(3) 0.080(5) 0.002(3) 0.003(3) 0.009(3) O4 0.040(2) 0.022(2) 0.033(2) -0.0042(16) -0.0037(16) 0.0078(16) O5 0.032(2) 0.029(2) 0.042(2) -0.0029(18) -0.0063(17) 0.0065(17) C55 0.054(4) 0.043(4) 0.036(3) -0.007(3) -0.005(3) 0.001(3) C56 0.045(4) 0.023(3) 0.049(4) 0.005(3) 0.004(3) 0.008(3) C57 0.049(4) 0.023(3) 0.047(4) 0.007(3) -0.003(3) 0.008(3) C58 0.029(3) 0.068(4) 0.039(3) 0.002(3) 0.004(3) 0.010(3) O6 0.051(2) 0.054(3) 0.056(3) 0.009(2) 0.008(2) -0.010(2) O7 0.042(2) 0.038(2) 0.043(2) -0.0137(19) -0.0059(19) 0.0066(19) C59 0.073(5) 0.062(5) 0.050(4) 0.000(4) 0.015(3) 0.017(4) C60 0.034(3) 0.043(4) 0.054(4) -0.019(3) 0.007(3) -0.007(3) C61 0.039(3) 0.030(3) 0.041(3) -0.002(3) 0.004(3) 0.003(3) C62 0.067(5) 0.065(5) 0.049(4) -0.018(4) -0.005(3) 0.012(4) _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 O3A 2.12(2) . ? U1 O2A 2.120(19) . ? U1 O3 2.201(4) . ? U1 O1 2.212(4) . ? U1 O2 2.255(4) . ? U1 O1A 2.32(2) . ? U1 O5 2.621(3) . ? U1 N1 2.622(4) . ? U1 O4 2.656(3) . ? O1 C3 1.343(6) . ? O2 C10 1.346(7) . ? O3 C17 1.346(7) . ? O1A C3A 1.36(3) . ? O2A C10A 1.36(3) . ? O3A C17A 1.38(3) . ? N1 C15A 1.40(3) . ? N1 C8A 1.44(4) . ? N1 C15 1.467(6) . ? N1 C1 1.499(7) . ? N1 C8 1.511(6) . ? N1 C1A 1.62(3) . ? C1 C2 1.492(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.395(7) . ? C2 C3 1.405(8) . ? C3 C4 1.427(9) . ? C4 C5 1.394(8) . ? C4 C22 1.553(8) . ? C5 C6 1.389(8) . ? C5 H5A 0.9500 . ? C6 C7 1.371(8) . ? C6 C32 1.510(8) . ? C7 H7A 0.9500 . ? C1A C2A 1.54(3) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A C3A 1.3900 . ? C2A C7A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C4A C22 1.40(2) . ? C5A C6A 1.3900 . ? C5A H5AA 0.9500 . ? C6A C7A 1.3900 . ? C6A C32 1.53(2) . ? C7A H7AA 0.9500 . ? C8 C9 1.495(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.390(8) . ? C9 C10 1.404(8) . ? C10 C11 1.422(8) . ? C11 C12 1.397(8) . ? C11 C33 1.540(8) . ? C12 C13 1.385(8) . ? C12 H12A 0.9500 . ? C13 C14 1.378(9) . ? C13 C43 1.506(9) . ? C14 H14A 0.9500 . ? C8A C9A 1.56(4) . ? C8A H8AA 0.9900 . ? C8A H8AB 0.9900 . ? C9A C10A 1.3900 . ? C9A C14A 1.3900 . ? C10A C11A 1.3900 . ? C11A C12A 1.3900 . ? C11A C33 1.51(2) . ? C12A C13A 1.3900 . ? C12A H12B 0.9500 . ? C13A C14A 1.3900 . ? C13A C43A 1.55(3) . ? C14A H14B 0.9500 . ? C15 C16 1.499(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.388(8) . ? C16 C17 1.406(7) . ? C17 C18 1.424(9) . ? C18 C19 1.383(8) . ? C18 C44 1.516(8) . ? C19 C20 1.372(8) . ? C19 H19A 0.9500 . ? C20 C21 1.366(9) . ? C20 C54 1.497(9) . ? C21 H21A 0.9500 . ? C15A C16A 1.53(3) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C16A C17A 1.3900 . ? C16A C21A 1.3900 . ? C17A C18A 1.3900 . ? C18A C19A 1.3900 . ? C18A C44 1.64(2) . ? C19A C20A 1.3900 . ? C19A H19B 0.9500 . ? C20A C21A 1.3900 . ? C20A C54 1.632(19) . ? C21A H21B 0.9500 . ? C22 C26 1.525(7) . ? C22 C29 1.531(7) . ? C22 C31 1.555(8) . ? C23 C27 1.496(11) . ? C23 C30 1.510(11) . ? C23 C26 1.567(9) . ? C23 H23A 1.0000 . ? C24 C27 1.490(10) . ? C24 C28 1.519(9) . ? C24 C31 1.531(8) . ? C24 H24A 1.0000 . ? C25 C28 1.510(9) . ? C25 C29 1.541(8) . ? C25 C30 1.591(9) . ? C25 H25A 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32 H32D 0.9800 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? C33 C42 1.516(7) . ? C33 C37 1.525(7) . ? C33 C40 1.530(7) . ? C34 C41 1.464(11) . ? C34 C38 1.490(11) . ? C34 C37 1.547(9) . ? C34 H34A 1.0000 . ? C35 C38 1.473(10) . ? C35 C39 1.495(10) . ? C35 C42 1.536(9) . ? C35 H35A 1.0000 . ? C36 C39 1.505(9) . ? C36 C41 1.529(10) . ? C36 C40 1.558(8) . ? C36 H36A 1.0000 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C44 C48 1.528(6) . ? C44 C53 1.535(6) . ? C44 C51 1.542(7) . ? C45 C52 1.513(8) . ? C45 C49 1.526(7) . ? C45 C48 1.538(7) . ? C45 H45A 1.0000 . ? C46 C49 1.516(7) . ? C46 C50 1.518(8) . ? C46 C53 1.537(7) . ? C46 H46A 1.0000 . ? C47 C52 1.522(8) . ? C47 C50 1.533(8) . ? C47 C51 1.539(7) . ? C47 H47A 1.0000 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? O4 C55 1.423(6) . ? O4 C56 1.438(6) . ? O5 C58 1.430(6) . ? O5 C57 1.433(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.497(8) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O6 C59 1.385(7) . ? O6 C60 1.415(7) . ? O7 C62 1.410(7) . ? O7 C61 1.413(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.517(8) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 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 O3A U1 O2A 122.3(8) . . ? O3A U1 O3 24.5(6) . . ? O2A U1 O3 141.5(5) . . ? O3A U1 O1 131.1(6) . . ? O2A U1 O1 84.6(6) . . ? O3 U1 O1 109.82(15) . . ? O3A U1 O2 91.1(7) . . ? O2A U1 O2 33.5(5) . . ? O3 U1 O2 114.08(15) . . ? O1 U1 O2 115.89(15) . . ? O3A U1 O1A 108.7(8) . . ? O2A U1 O1A 111.0(8) . . ? O3 U1 O1A 85.2(5) . . ? O1 U1 O1A 26.9(5) . . ? O2 U1 O1A 139.7(5) . . ? O3A U1 O5 127.5(5) . . ? O2A U1 O5 98.2(5) . . ? O3 U1 O5 119.06(13) . . ? O1 U1 O5 79.92(13) . . ? O2 U1 O5 113.65(13) . . ? O1A U1 O5 82.1(5) . . ? O3A U1 N1 74.9(5) . . ? O2A U1 N1 74.9(5) . . ? O3 U1 N1 75.08(12) . . ? O1 U1 N1 74.54(12) . . ? O2 U1 N1 74.43(13) . . ? O1A U1 N1 77.4(5) . . ? O5 U1 N1 154.01(11) . . ? O3A U1 O4 77.0(5) . . ? O2A U1 O4 101.9(5) . . ? O3 U1 O4 88.47(13) . . ? O1 U1 O4 141.85(12) . . ? O2 U1 O4 83.52(13) . . ? O1A U1 O4 134.2(5) . . ? O5 U1 O4 61.98(11) . . ? N1 U1 O4 143.58(11) . . ? C3 O1 U1 139.8(3) . . ? C10 O2 U1 136.0(3) . . ? C17 O3 U1 144.7(3) . . ? C3A O1A U1 139.3(16) . . ? C10A O2A U1 142.7(16) . . ? C17A O3A U1 142.3(17) . . ? C15A N1 C8A 118.3(19) . . ? C15A N1 C15 76.5(13) . . ? C8A N1 C15 125.2(15) . . ? C15A N1 C1 136.9(13) . . ? C15 N1 C1 108.5(4) . . ? C8A N1 C8 84.3(14) . . ? C15 N1 C8 109.4(4) . . ? C1 N1 C8 107.5(4) . . ? C15A N1 C1A 106.8(16) . . ? C8A N1 C1A 105.9(18) . . ? C1 N1 C1A 83.8(12) . . ? C8 N1 C1A 136.0(11) . . ? C15A N1 U1 107.9(12) . . ? C8A N1 U1 112.1(15) . . ? C15 N1 U1 111.5(3) . . ? C1 N1 U1 109.3(3) . . ? C8 N1 U1 110.5(3) . . ? C1A N1 U1 104.9(12) . . ? C2 C1 N1 113.4(5) . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? N1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C7 C2 C3 119.9(5) . . ? C7 C2 C1 120.2(5) . . ? C3 C2 C1 119.9(5) . . ? O1 C3 C2 118.0(5) . . ? O1 C3 C4 122.4(5) . . ? C2 C3 C4 119.5(5) . . ? C5 C4 C3 116.8(5) . . ? C5 C4 C22 120.9(5) . . ? C3 C4 C22 122.3(6) . . ? C6 C5 C4 124.4(5) . . ? C6 C5 H5A 117.8 . . ? C4 C5 H5A 117.8 . . ? C7 C6 C5 117.1(5) . . ? C7 C6 C32 122.9(6) . . ? C5 C6 C32 120.0(5) . . ? C6 C7 C2 122.2(5) . . ? C6 C7 H7A 118.9 . . ? C2 C7 H7A 118.9 . . ? C2A C1A N1 114.4(19) . . ? C2A C1A H1AA 108.7 . . ? N1 C1A H1AA 108.7 . . ? C2A C1A H1AB 108.7 . . ? N1 C1A H1AB 108.7 . . ? H1AA C1A H1AB 107.6 . . ? C3A C2A C7A 120.0 . . ? C3A C2A C1A 118.4(18) . . ? C7A C2A C1A 121.3(17) . . ? O1A C3A C2A 119.3(17) . . ? O1A C3A C4A 120.5(17) . . ? C2A C3A C4A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A C22 115.6(18) . . ? C5A C4A C22 122.7(18) . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5AA 120.0 . . ? C4A C5A H5AA 120.0 . . ? C5A C6A C7A 120.0 . . ? C5A C6A C32 129.5(16) . . ? C7A C6A C32 110.3(16) . . ? C6A C7A C2A 120.0 . . ? C6A C7A H7AA 120.0 . . ? C2A C7A H7AA 120.0 . . ? C9 C8 N1 114.8(4) . . ? C9 C8 H8A 108.6 . . ? N1 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? N1 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C14 C9 C10 120.8(5) . . ? C14 C9 C8 120.3(5) . . ? C10 C9 C8 118.8(5) . . ? O2 C10 C9 118.3(5) . . ? O2 C10 C11 122.7(5) . . ? C9 C10 C11 119.0(5) . . ? C12 C11 C10 116.9(5) . . ? C12 C11 C33 121.8(5) . . ? C10 C11 C33 121.2(6) . . ? C13 C12 C11 124.6(6) . . ? C13 C12 H12A 117.7 . . ? C11 C12 H12A 117.7 . . ? C14 C13 C12 117.1(6) . . ? C14 C13 C43 122.3(7) . . ? C12 C13 C43 120.6(7) . . ? C13 C14 C9 121.6(6) . . ? C13 C14 H14A 119.2 . . ? C9 C14 H14A 119.2 . . ? N1 C8A C9A 109(2) . . ? N1 C8A H8AA 109.9 . . ? C9A C8A H8AA 109.9 . . ? N1 C8A H8AB 109.9 . . ? C9A C8A H8AB 109.9 . . ? H8AA C8A H8AB 108.3 . . ? C10A C9A C14A 120.0 . . ? C10A C9A C8A 122.8(17) . . ? C14A C9A C8A 116.3(17) . . ? O2A C10A C11A 123.3(16) . . ? O2A C10A C9A 116.7(16) . . ? C11A C10A C9A 120.0 . . ? C10A C11A C12A 120.0 . . ? C10A C11A C33 121.7(17) . . ? C12A C11A C33 118.1(17) . . ? C13A C12A C11A 120.0 . . ? C13A C12A H12B 120.0 . . ? C11A C12A H12B 120.0 . . ? C12A C13A C14A 120.0 . . ? C12A C13A C43A 123(3) . . ? C14A C13A C43A 117(3) . . ? C13A C14A C9A 120.0 . . ? C13A C14A H14B 120.0 . . ? C9A C14A H14B 120.0 . . ? N1 C15 C16 118.7(4) . . ? N1 C15 H15A 107.6 . . ? C16 C15 H15A 107.6 . . ? N1 C15 H15B 107.6 . . ? C16 C15 H15B 107.6 . . ? H15A C15 H15B 107.1 . . ? C21 C16 C17 120.2(5) . . ? C21 C16 C15 119.0(5) . . ? C17 C16 C15 119.7(5) . . ? O3 C17 C16 118.6(5) . . ? O3 C17 C18 122.1(5) . . ? C16 C17 C18 119.3(5) . . ? C19 C18 C17 116.4(5) . . ? C19 C18 C44 122.9(6) . . ? C17 C18 C44 120.7(6) . . ? C20 C19 C18 124.9(6) . . ? C20 C19 H19A 117.5 . . ? C18 C19 H19A 117.5 . . ? C21 C20 C19 117.8(6) . . ? C21 C20 C54 119.0(6) . . ? C19 C20 C54 122.9(6) . . ? C20 C21 C16 121.2(5) . . ? C20 C21 H21A 119.4 . . ? C16 C21 H21A 119.4 . . ? N1 C15A C16A 115(2) . . ? N1 C15A H15C 108.4 . . ? C16A C15A H15C 108.4 . . ? N1 C15A H15D 108.4 . . ? C16A C15A H15D 108.4 . . ? H15C C15A H15D 107.5 . . ? C17A C16A C21A 120.0 . . ? C17A C16A C15A 121.1(17) . . ? C21A C16A C15A 118.8(17) . . ? O3A C17A C18A 125.9(17) . . ? O3A C17A C16A 113.9(17) . . ? C18A C17A C16A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A C44 125.0(18) . . ? C19A C18A C44 115.0(18) . . ? C18A C19A C20A 120.0 . . ? C18A C19A H19B 120.0 . . ? C20A C19A H19B 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A C54 113.7(19) . . ? C21A C20A C54 126.0(19) . . ? C20A C21A C16A 120.0 . . ? C20A C21A H21B 120.0 . . ? C16A C21A H21B 120.0 . . ? C4A C22 C26 108.1(13) . . ? C4A C22 C29 114.6(15) . . ? C26 C22 C29 110.4(5) . . ? C26 C22 C4 112.1(5) . . ? C29 C22 C4 110.7(5) . . ? C4A C22 C31 108.4(13) . . ? C26 C22 C31 107.7(5) . . ? C29 C22 C31 107.5(4) . . ? C4 C22 C31 108.3(5) . . ? C27 C23 C30 112.1(7) . . ? C27 C23 C26 110.6(6) . . ? C30 C23 C26 105.7(6) . . ? C27 C23 H23A 109.5 . . ? C30 C23 H23A 109.5 . . ? C26 C23 H23A 109.5 . . ? C27 C24 C28 109.8(7) . . ? C27 C24 C31 109.3(6) . . ? C28 C24 C31 110.3(5) . . ? C27 C24 H24A 109.2 . . ? C28 C24 H24A 109.2 . . ? C31 C24 H24A 109.2 . . ? C28 C25 C29 109.9(5) . . ? C28 C25 C30 107.3(6) . . ? C29 C25 C30 108.0(5) . . ? C28 C25 H25A 110.5 . . ? C29 C25 H25A 110.5 . . ? C30 C25 H25A 110.5 . . ? C22 C26 C23 110.2(5) . . ? C22 C26 H26A 109.6 . . ? C23 C26 H26A 109.6 . . ? C22 C26 H26B 109.6 . . ? C23 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C24 C27 C23 110.0(6) . . ? C24 C27 H27A 109.7 . . ? C23 C27 H27A 109.7 . . ? C24 C27 H27B 109.7 . . ? C23 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C25 C28 C24 110.7(5) . . ? C25 C28 H28A 109.5 . . ? C24 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C22 C29 C25 110.5(4) . . ? C22 C29 H29A 109.6 . . ? C25 C29 H29A 109.6 . . ? C22 C29 H29B 109.6 . . ? C25 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C23 C30 C25 109.8(6) . . ? C23 C30 H30A 109.7 . . ? C25 C30 H30A 109.7 . . ? C23 C30 H30B 109.7 . . ? C25 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C24 C31 C22 110.3(5) . . ? C24 C31 H31A 109.6 . . ? C22 C31 H31A 109.6 . . ? C24 C31 H31B 109.6 . . ? C22 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C6 C32 H32A 109.5 . . ? C6A C32 H32A 120.1 . . ? C6 C32 H32B 109.5 . . ? C6A C32 H32B 104.6 . . ? H32A C32 H32B 109.5 . . ? C6 C32 H32C 109.5 . . ? C6A C32 H32C 103.3 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C6 C32 H32D 98.9 . . ? C6A C32 H32D 109.5 . . ? H32B C32 H32D 114.4 . . ? H32C C32 H32D 114.6 . . ? C6 C32 H32E 113.8 . . ? C6A C32 H32E 109.5 . . ? H32A C32 H32E 104.1 . . ? H32C C32 H32E 110.3 . . ? H32D C32 H32E 109.5 . . ? C6 C32 H32F 115.2 . . ? C6A C32 H32F 109.5 . . ? H32A C32 H32F 103.8 . . ? H32B C32 H32F 109.3 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? C11A C33 C42 103.0(11) . . ? C11A C33 C37 108.4(12) . . ? C42 C33 C37 107.7(5) . . ? C11A C33 C40 122.1(13) . . ? C42 C33 C40 108.7(5) . . ? C37 C33 C40 106.2(5) . . ? C42 C33 C11 113.6(4) . . ? C37 C33 C11 111.9(5) . . ? C40 C33 C11 108.5(4) . . ? C41 C34 C38 110.9(7) . . ? C41 C34 C37 106.7(7) . . ? C38 C34 C37 112.0(6) . . ? C41 C34 H34A 109.0 . . ? C38 C34 H34A 109.0 . . ? C37 C34 H34A 109.0 . . ? C38 C35 C39 110.7(6) . . ? C38 C35 C42 108.8(7) . . ? C39 C35 C42 110.4(6) . . ? C38 C35 H35A 109.0 . . ? C39 C35 H35A 109.0 . . ? C42 C35 H35A 109.0 . . ? C39 C36 C41 108.8(6) . . ? C39 C36 C40 108.1(6) . . ? C41 C36 C40 108.4(6) . . ? C39 C36 H36A 110.5 . . ? C41 C36 H36A 110.5 . . ? C40 C36 H36A 110.5 . . ? C33 C37 C34 110.7(5) . . ? C33 C37 H37A 109.5 . . ? C34 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C35 C38 C34 109.0(6) . . ? C35 C38 H38A 109.9 . . ? C34 C38 H38A 109.9 . . ? C35 C38 H38B 109.9 . . ? C34 C38 H38B 109.9 . . ? H38A C38 H38B 108.3 . . ? C35 C39 C36 110.0(5) . . ? C35 C39 H39A 109.7 . . ? C36 C39 H39A 109.7 . . ? C35 C39 H39B 109.7 . . ? C36 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C33 C40 C36 110.9(5) . . ? C33 C40 H40A 109.5 . . ? C36 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 108.0 . . ? C34 C41 C36 110.6(5) . . ? C34 C41 H41A 109.5 . . ? C36 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C33 C42 C35 111.3(5) . . ? C33 C42 H42A 109.4 . . ? C35 C42 H42A 109.4 . . ? C33 C42 H42B 109.4 . . ? C35 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C13 C43 H43A 109.5 . . ? C13 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C13 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C13A C43A H43D 109.5 . . ? C13A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C13A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C18 C44 C48 111.1(4) . . ? C18 C44 C53 111.9(4) . . ? C48 C44 C53 107.6(4) . . ? C18 C44 C51 110.1(5) . . ? C48 C44 C51 106.8(4) . . ? C53 C44 C51 109.3(4) . . ? C48 C44 C18A 116.3(11) . . ? C53 C44 C18A 102.2(12) . . ? C51 C44 C18A 114.4(14) . . ? C52 C45 C49 109.4(5) . . ? C52 C45 C48 109.5(5) . . ? C49 C45 C48 108.7(4) . . ? C52 C45 H45A 109.7 . . ? C49 C45 H45A 109.7 . . ? C48 C45 H45A 109.7 . . ? C49 C46 C50 109.9(5) . . ? C49 C46 C53 110.0(4) . . ? C50 C46 C53 108.9(4) . . ? C49 C46 H46A 109.3 . . ? C50 C46 H46A 109.3 . . ? C53 C46 H46A 109.3 . . ? C52 C47 C50 109.6(5) . . ? C52 C47 C51 109.4(5) . . ? C50 C47 C51 109.0(5) . . ? C52 C47 H47A 109.6 . . ? C50 C47 H47A 109.6 . . ? C51 C47 H47A 109.6 . . ? C44 C48 C45 112.1(4) . . ? C44 C48 H48A 109.2 . . ? C45 C48 H48A 109.2 . . ? C44 C48 H48B 109.2 . . ? C45 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C46 C49 C45 109.5(4) . . ? C46 C49 H49A 109.8 . . ? C45 C49 H49A 109.8 . . ? C46 C49 H49B 109.8 . . ? C45 C49 H49B 109.8 . . ? H49A C49 H49B 108.2 . . ? C46 C50 C47 109.7(4) . . ? C46 C50 H50A 109.7 . . ? C47 C50 H50A 109.7 . . ? C46 C50 H50B 109.7 . . ? C47 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? C47 C51 C44 110.7(4) . . ? C47 C51 H51A 109.5 . . ? C44 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? C44 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C45 C52 C47 109.6(5) . . ? C45 C52 H52A 109.7 . . ? C47 C52 H52A 109.7 . . ? C45 C52 H52B 109.7 . . ? C47 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? C44 C53 C46 110.7(4) . . ? C44 C53 H53A 109.5 . . ? C46 C53 H53A 109.5 . . ? C44 C53 H53B 109.5 . . ? C46 C53 H53B 109.5 . . ? H53A C53 H53B 108.1 . . ? C20 C54 H54A 109.5 . . ? C20A C54 H54A 102.0 . . ? C20 C54 H54B 109.5 . . ? C20A C54 H54B 111.5 . . ? H54A C54 H54B 109.5 . . ? C20 C54 H54C 109.5 . . ? C20A C54 H54C 114.7 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C20 C54 H54D 117.0 . . ? C20A C54 H54D 109.5 . . ? H54B C54 H54D 105.7 . . ? H54C C54 H54D 105.5 . . ? C20 C54 H54E 107.1 . . ? C20A C54 H54E 109.5 . . ? H54A C54 H54E 113.2 . . ? H54C C54 H54E 108.1 . . ? H54D C54 H54E 109.5 . . ? C20 C54 H54F 104.1 . . ? C20A C54 H54F 109.5 . . ? H54A C54 H54F 113.0 . . ? H54B C54 H54F 111.2 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? C55 O4 C56 112.5(4) . . ? C55 O4 U1 125.2(3) . . ? C56 O4 U1 119.9(3) . . ? C58 O5 C57 114.8(4) . . ? C58 O5 U1 127.0(3) . . ? C57 O5 U1 110.3(3) . . ? O4 C55 H55A 109.5 . . ? O4 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O4 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O4 C56 C57 107.3(4) . . ? O4 C56 H56A 110.3 . . ? C57 C56 H56A 110.3 . . ? O4 C56 H56B 110.3 . . ? C57 C56 H56B 110.3 . . ? H56A C56 H56B 108.5 . . ? O5 C57 C56 109.8(4) . . ? O5 C57 H57A 109.7 . . ? C56 C57 H57A 109.7 . . ? O5 C57 H57B 109.7 . . ? C56 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? O5 C58 H58A 109.5 . . ? O5 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O5 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C59 O6 C60 111.4(5) . . ? C62 O7 C61 110.9(4) . . ? O6 C59 H59A 109.5 . . ? O6 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O6 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O6 C60 C61 111.3(5) . . ? O6 C60 H60A 109.4 . . ? C61 C60 H60A 109.4 . . ? O6 C60 H60B 109.4 . . ? C61 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? O7 C61 C60 109.2(5) . . ? O7 C61 H61A 109.8 . . ? C60 C61 H61A 109.8 . . ? O7 C61 H61B 109.8 . . ? C60 C61 H61B 109.8 . . ? H61A C61 H61B 108.3 . . ? O7 C62 H62A 109.5 . . ? O7 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O7 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 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 O3A U1 O1 C3 28.3(10) . . . . ? O2A U1 O1 C3 -100.8(7) . . . . ? O3 U1 O1 C3 42.5(6) . . . . ? O2 U1 O1 C3 -88.6(6) . . . . ? O1A U1 O1 C3 67.6(12) . . . . ? O5 U1 O1 C3 159.9(6) . . . . ? N1 U1 O1 C3 -24.9(5) . . . . ? O4 U1 O1 C3 156.9(5) . . . . ? O3A U1 O2 C10 -107.3(7) . . . . ? O2A U1 O2 C10 52.8(10) . . . . ? O3 U1 O2 C10 -98.7(5) . . . . ? O1 U1 O2 C10 30.4(5) . . . . ? O1A U1 O2 C10 13.9(10) . . . . ? O5 U1 O2 C10 120.4(5) . . . . ? N1 U1 O2 C10 -33.3(5) . . . . ? O4 U1 O2 C10 175.9(5) . . . . ? O3A U1 O3 C17 71.5(14) . . . . ? O2A U1 O3 C17 25.1(11) . . . . ? O1 U1 O3 C17 -81.9(7) . . . . ? O2 U1 O3 C17 50.1(7) . . . . ? O1A U1 O3 C17 -93.0(8) . . . . ? O5 U1 O3 C17 -171.2(6) . . . . ? N1 U1 O3 C17 -14.8(6) . . . . ? O4 U1 O3 C17 132.4(7) . . . . ? O3A U1 O1A C3A 87(3) . . . . ? O2A U1 O1A C3A -50(3) . . . . ? O3 U1 O1A C3A 94(3) . . . . ? O1 U1 O1A C3A -63(2) . . . . ? O2 U1 O1A C3A -29(3) . . . . ? O5 U1 O1A C3A -146(3) . . . . ? N1 U1 O1A C3A 18(3) . . . . ? O4 U1 O1A C3A 177(2) . . . . ? O3A U1 O2A C10A -38(3) . . . . ? O3 U1 O2A C10A -17(3) . . . . ? O1 U1 O2A C10A 98(3) . . . . ? O2 U1 O2A C10A -62(2) . . . . ? O1A U1 O2A C10A 92(3) . . . . ? O5 U1 O2A C10A 177(3) . . . . ? N1 U1 O2A C10A 23(2) . . . . ? O4 U1 O2A C10A -120(3) . . . . ? O2A U1 O3A C17A 89(3) . . . . ? O3 U1 O3A C17A -59(3) . . . . ? O1 U1 O3A C17A -25(3) . . . . ? O2 U1 O3A C17A 102(3) . . . . ? O1A U1 O3A C17A -43(3) . . . . ? O5 U1 O3A C17A -137(3) . . . . ? N1 U1 O3A C17A 28(3) . . . . ? O4 U1 O3A C17A -175(3) . . . . ? O3A U1 N1 C15A 30.2(15) . . . . ? O2A U1 N1 C15A -100.1(14) . . . . ? O3 U1 N1 C15A 55.5(13) . . . . ? O1 U1 N1 C15A 171.5(13) . . . . ? O2 U1 N1 C15A -65.3(13) . . . . ? O1A U1 N1 C15A 143.8(14) . . . . ? O5 U1 N1 C15A -177.6(13) . . . . ? O4 U1 N1 C15A -10.4(13) . . . . ? O3A U1 N1 C8A 162.1(16) . . . . ? O2A U1 N1 C8A 31.9(15) . . . . ? O3 U1 N1 C8A -172.5(14) . . . . ? O1 U1 N1 C8A -56.6(14) . . . . ? O2 U1 N1 C8A 66.6(14) . . . . ? O1A U1 N1 C8A -84.2(15) . . . . ? O5 U1 N1 C8A -45.6(15) . . . . ? O4 U1 N1 C8A 121.5(14) . . . . ? O3A U1 N1 C15 -51.9(7) . . . . ? O2A U1 N1 C15 177.8(7) . . . . ? O3 U1 N1 C15 -26.6(3) . . . . ? O1 U1 N1 C15 89.4(3) . . . . ? O2 U1 N1 C15 -147.4(3) . . . . ? O1A U1 N1 C15 61.7(6) . . . . ? O5 U1 N1 C15 100.3(4) . . . . ? O4 U1 N1 C15 -92.5(4) . . . . ? O3A U1 N1 C1 -171.9(7) . . . . ? O2A U1 N1 C1 57.8(6) . . . . ? O3 U1 N1 C1 -146.6(3) . . . . ? O1 U1 N1 C1 -30.6(3) . . . . ? O2 U1 N1 C1 92.6(3) . . . . ? O1A U1 N1 C1 -58.3(6) . . . . ? O5 U1 N1 C1 -19.7(5) . . . . ? O4 U1 N1 C1 147.5(3) . . . . ? O3A U1 N1 C8 70.0(7) . . . . ? O2A U1 N1 C8 -60.3(6) . . . . ? O3 U1 N1 C8 95.3(3) . . . . ? O1 U1 N1 C8 -148.7(3) . . . . ? O2 U1 N1 C8 -25.5(3) . . . . ? O1A U1 N1 C8 -176.4(6) . . . . ? O5 U1 N1 C8 -137.8(3) . . . . ? O4 U1 N1 C8 29.4(4) . . . . ? O3A U1 N1 C1A -83.4(13) . . . . ? O2A U1 N1 C1A 146.4(13) . . . . ? O3 U1 N1 C1A -58.1(12) . . . . ? O1 U1 N1 C1A 57.9(12) . . . . ? O2 U1 N1 C1A -178.9(12) . . . . ? O1A U1 N1 C1A 30.3(13) . . . . ? O5 U1 N1 C1A 68.8(12) . . . . ? O4 U1 N1 C1A -124.0(12) . . . . ? C15A N1 C1 C2 -139.4(19) . . . . ? C8A N1 C1 C2 174(4) . . . . ? C15 N1 C1 C2 -49.5(6) . . . . ? C8 N1 C1 C2 -167.7(5) . . . . ? C1A N1 C1 C2 -31.4(12) . . . . ? U1 N1 C1 C2 72.3(5) . . . . ? N1 C1 C2 C7 118.3(6) . . . . ? N1 C1 C2 C3 -62.8(7) . . . . ? U1 O1 C3 C2 44.2(8) . . . . ? U1 O1 C3 C4 -134.2(6) . . . . ? C7 C2 C3 O1 -178.9(5) . . . . ? C1 C2 C3 O1 2.3(8) . . . . ? C7 C2 C3 C4 -0.4(9) . . . . ? C1 C2 C3 C4 -179.2(6) . . . . ? O1 C3 C4 C5 179.8(5) . . . . ? C2 C3 C4 C5 1.4(10) . . . . ? O1 C3 C4 C22 0.1(11) . . . . ? C2 C3 C4 C22 -178.3(5) . . . . ? C3 C4 C5 C6 -0.5(10) . . . . ? C22 C4 C5 C6 179.2(6) . . . . ? C4 C5 C6 C7 -1.5(10) . . . . ? C4 C5 C6 C32 177.0(6) . . . . ? C5 C6 C7 C2 2.6(10) . . . . ? C32 C6 C7 C2 -175.9(6) . . . . ? C3 C2 C7 C6 -1.7(9) . . . . ? C1 C2 C7 C6 177.1(6) . . . . ? C15A N1 C1A C2A 171(2) . . . . ? C8A N1 C1A C2A 44(3) . . . . ? C15 N1 C1A C2A 178(4) . . . . ? C1 N1 C1A C2A 33(2) . . . . ? C8 N1 C1A C2A 142.2(14) . . . . ? U1 N1 C1A C2A -75(2) . . . . ? N1 C1A C2A C3A 71(3) . . . . ? N1 C1A C2A C7A -115(2) . . . . ? U1 O1A C3A C2A -33(4) . . . . ? U1 O1A C3A C4A 142(2) . . . . ? C7A C2A C3A O1A 175(3) . . . . ? C1A C2A C3A O1A -11(3) . . . . ? C7A C2A C3A C4A 0.0 . . . . ? C1A C2A C3A C4A 174(2) . . . . ? O1A C3A C4A C5A -175(3) . . . . ? C2A C3A C4A C5A 0.0 . . . . ? O1A C3A C4A C22 19(3) . . . . ? C2A C3A C4A C22 -166(3) . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C22 C4A C5A C6A 165(3) . . . . ? C4A C5A C6A C7A 0.0 . . . . ? C4A C5A C6A C32 -174(3) . . . . ? C5A C6A C7A C2A 0.0 . . . . ? C32 C6A C7A C2A 175(2) . . . . ? C3A C2A C7A C6A 0.0 . . . . ? C1A C2A C7A C6A -174(2) . . . . ? C15A N1 C8 C9 163(2) . . . . ? C8A N1 C8 C9 -41.6(16) . . . . ? C15 N1 C8 C9 -167.0(4) . . . . ? C1 N1 C8 C9 -49.3(6) . . . . ? C1A N1 C8 C9 -148.7(17) . . . . ? U1 N1 C8 C9 69.9(5) . . . . ? N1 C8 C9 C14 114.9(5) . . . . ? N1 C8 C9 C10 -61.5(7) . . . . ? U1 O2 C10 C9 54.1(8) . . . . ? U1 O2 C10 C11 -126.3(5) . . . . ? C14 C9 C10 O2 -178.6(5) . . . . ? C8 C9 C10 O2 -2.2(8) . . . . ? C14 C9 C10 C11 1.8(8) . . . . ? C8 C9 C10 C11 178.2(5) . . . . ? O2 C10 C11 C12 178.0(6) . . . . ? C9 C10 C11 C12 -2.4(9) . . . . ? O2 C10 C11 C33 0.1(9) . . . . ? C9 C10 C11 C33 179.7(5) . . . . ? C10 C11 C12 C13 3.0(10) . . . . ? C33 C11 C12 C13 -179.1(6) . . . . ? C11 C12 C13 C14 -2.7(10) . . . . ? C11 C12 C13 C43 179.9(8) . . . . ? C12 C13 C14 C9 1.9(9) . . . . ? C43 C13 C14 C9 179.2(8) . . . . ? C10 C9 C14 C13 -1.6(9) . . . . ? C8 C9 C14 C13 -177.9(6) . . . . ? C15A N1 C8A C9A 58(3) . . . . ? C15 N1 C8A C9A 150.9(14) . . . . ? C1 N1 C8A C9A -157(5) . . . . ? C8 N1 C8A C9A 41(2) . . . . ? C1A N1 C8A C9A 177(2) . . . . ? U1 N1 C8A C9A -69(2) . . . . ? N1 C8A C9A C10A 65(3) . . . . ? N1 C8A C9A C14A -126(2) . . . . ? U1 O2A C10A C11A 144(2) . . . . ? U1 O2A C10A C9A -35(3) . . . . ? C14A C9A C10A O2A 179(2) . . . . ? C8A C9A C10A O2A -12(3) . . . . ? C14A C9A C10A C11A 0.0 . . . . ? C8A C9A C10A C11A 169(3) . . . . ? O2A C10A C11A C12A -179(2) . . . . ? C9A C10A C11A C12A 0.0 . . . . ? O2A C10A C11A C33 -4(3) . . . . ? C9A C10A C11A C33 175(2) . . . . ? C10A C11A C12A C13A 0.0 . . . . ? C33 C11A C12A C13A -175(2) . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C11A C12A C13A C43A -179(3) . . . . ? C12A C13A C14A C9A 0.0 . . . . ? C43A C13A C14A C9A 179(2) . . . . ? C10A C9A C14A C13A 0.0 . . . . ? C8A C9A C14A C13A -169(3) . . . . ? C15A N1 C15 C16 -39.6(13) . . . . ? C8A N1 C15 C16 -154.9(17) . . . . ? C1 N1 C15 C16 -175.0(5) . . . . ? C8 N1 C15 C16 -58.0(6) . . . . ? C1A N1 C15 C16 147(3) . . . . ? U1 N1 C15 C16 64.5(5) . . . . ? N1 C15 C16 C21 129.0(5) . . . . ? N1 C15 C16 C17 -62.4(7) . . . . ? U1 O3 C17 C16 23.6(10) . . . . ? U1 O3 C17 C18 -158.1(5) . . . . ? C21 C16 C17 O3 -177.3(5) . . . . ? C15 C16 C17 O3 14.2(8) . . . . ? C21 C16 C17 C18 4.4(9) . . . . ? C15 C16 C17 C18 -164.1(6) . . . . ? O3 C17 C18 C19 178.1(6) . . . . ? C16 C17 C18 C19 -3.7(9) . . . . ? O3 C17 C18 C44 -2.9(10) . . . . ? C16 C17 C18 C44 175.4(5) . . . . ? C17 C18 C19 C20 0.7(9) . . . . ? C44 C18 C19 C20 -178.3(7) . . . . ? C18 C19 C20 C21 1.5(10) . . . . ? C18 C19 C20 C54 176.2(8) . . . . ? C19 C20 C21 C16 -0.9(10) . . . . ? C54 C20 C21 C16 -175.8(6) . . . . ? C17 C16 C21 C20 -2.1(10) . . . . ? C15 C16 C21 C20 166.5(6) . . . . ? C8A N1 C15A C16A 160(2) . . . . ? C15 N1 C15A C16A 37.3(18) . . . . ? C1 N1 C15A C16A 140.1(15) . . . . ? C8 N1 C15A C16A -172(4) . . . . ? C1A N1 C15A C16A 41(3) . . . . ? U1 N1 C15A C16A -71(2) . . . . ? N1 C15A C16A C17A 63(3) . . . . ? N1 C15A C16A C21A -114(2) . . . . ? U1 O3A C17A C18A 130(3) . . . . ? U1 O3A C17A C16A -46(4) . . . . ? C21A C16A C17A O3A 176(2) . . . . ? C15A C16A C17A O3A -1(3) . . . . ? C21A C16A C17A C18A 0.0 . . . . ? C15A C16A C17A C18A -177(3) . . . . ? O3A C17A C18A C19A -176(3) . . . . ? C16A C17A C18A C19A 0.0 . . . . ? O3A C17A C18A C44 4(4) . . . . ? C16A C17A C18A C44 179(3) . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C44 C18A C19A C20A -179(3) . . . . ? C18A C19A C20A C21A 0.0 . . . . ? C18A C19A C20A C54 -174(3) . . . . ? C19A C20A C21A C16A 0.0 . . . . ? C54 C20A C21A C16A 173(3) . . . . ? C17A C16A C21A C20A 0.0 . . . . ? C15A C16A C21A C20A 177(3) . . . . ? C3A C4A C22 C26 148.9(14) . . . . ? C5A C4A C22 C26 -16(2) . . . . ? C3A C4A C22 C29 -87.6(18) . . . . ? C5A C4A C22 C29 107.2(16) . . . . ? C3A C4A C22 C4 -58(18) . . . . ? C5A C4A C22 C4 137(20) . . . . ? C3A C4A C22 C31 32(2) . . . . ? C5A C4A C22 C31 -132.8(15) . . . . ? C5 C4 C22 C4A -25(19) . . . . ? C3 C4 C22 C4A 154(20) . . . . ? C5 C4 C22 C26 1.9(8) . . . . ? C3 C4 C22 C26 -178.4(7) . . . . ? C5 C4 C22 C29 125.6(6) . . . . ? C3 C4 C22 C29 -54.7(9) . . . . ? C5 C4 C22 C31 -116.8(6) . . . . ? C3 C4 C22 C31 62.9(8) . . . . ? C4A C22 C26 C23 -173.5(16) . . . . ? C29 C22 C26 C23 60.5(7) . . . . ? C4 C22 C26 C23 -175.7(6) . . . . ? C31 C22 C26 C23 -56.6(7) . . . . ? C27 C23 C26 C22 57.9(8) . . . . ? C30 C23 C26 C22 -63.6(8) . . . . ? C28 C24 C27 C23 -59.7(8) . . . . ? C31 C24 C27 C23 61.3(8) . . . . ? C30 C23 C27 C24 58.3(8) . . . . ? C26 C23 C27 C24 -59.4(8) . . . . ? C29 C25 C28 C24 57.9(7) . . . . ? C30 C25 C28 C24 -59.4(6) . . . . ? C27 C24 C28 C25 62.7(7) . . . . ? C31 C24 C28 C25 -57.8(8) . . . . ? C4A C22 C29 C25 -179.6(13) . . . . ? C26 C22 C29 C25 -57.3(6) . . . . ? C4 C22 C29 C25 178.0(5) . . . . ? C31 C22 C29 C25 59.9(6) . . . . ? C28 C25 C29 C22 -60.1(6) . . . . ? C30 C25 C29 C22 56.7(7) . . . . ? C27 C23 C30 C25 -56.3(8) . . . . ? C26 C23 C30 C25 64.2(8) . . . . ? C28 C25 C30 C23 56.1(8) . . . . ? C29 C25 C30 C23 -62.4(8) . . . . ? C27 C24 C31 C22 -61.9(7) . . . . ? C28 C24 C31 C22 58.8(7) . . . . ? C4A C22 C31 C24 176.2(15) . . . . ? C26 C22 C31 C24 59.5(6) . . . . ? C29 C22 C31 C24 -59.4(6) . . . . ? C4 C22 C31 C24 -179.1(5) . . . . ? C7 C6 C32 C6A -166(8) . . . . ? C5 C6 C32 C6A 16(7) . . . . ? C5A C6A C32 C6 -142(8) . . . . ? C7A C6A C32 C6 43(6) . . . . ? C10A C11A C33 C42 42(2) . . . . ? C12A C11A C33 C42 -142.8(12) . . . . ? C10A C11A C33 C37 156.2(17) . . . . ? C12A C11A C33 C37 -28.9(15) . . . . ? C10A C11A C33 C40 -80(2) . . . . ? C12A C11A C33 C40 94.9(15) . . . . ? C10A C11A C33 C11 -97(6) . . . . ? C12A C11A C33 C11 78(5) . . . . ? C12 C11 C33 C11A -77(5) . . . . ? C10 C11 C33 C11A 101(5) . . . . ? C12 C11 C33 C42 -120.4(7) . . . . ? C10 C11 C33 C42 57.4(7) . . . . ? C12 C11 C33 C37 1.8(8) . . . . ? C10 C11 C33 C37 179.6(6) . . . . ? C12 C11 C33 C40 118.6(7) . . . . ? C10 C11 C33 C40 -63.6(7) . . . . ? C11A C33 C37 C34 -165.0(13) . . . . ? C42 C33 C37 C34 -54.2(8) . . . . ? C40 C33 C37 C34 62.1(7) . . . . ? C11 C33 C37 C34 -179.7(6) . . . . ? C41 C34 C37 C33 -65.5(8) . . . . ? C38 C34 C37 C33 56.1(9) . . . . ? C39 C35 C38 C34 -60.0(8) . . . . ? C42 C35 C38 C34 61.4(8) . . . . ? C41 C34 C38 C35 60.0(9) . . . . ? C37 C34 C38 C35 -59.1(9) . . . . ? C38 C35 C39 C36 59.8(7) . . . . ? C42 C35 C39 C36 -60.6(7) . . . . ? C41 C36 C39 C35 -56.6(7) . . . . ? C40 C36 C39 C35 61.0(7) . . . . ? C11A C33 C40 C36 176.9(13) . . . . ? C42 C33 C40 C36 57.4(7) . . . . ? C37 C33 C40 C36 -58.3(7) . . . . ? C11 C33 C40 C36 -178.6(5) . . . . ? C39 C36 C40 C33 -60.1(7) . . . . ? C41 C36 C40 C33 57.6(7) . . . . ? C38 C34 C41 C36 -58.8(8) . . . . ? C37 C34 C41 C36 63.4(7) . . . . ? C39 C36 C41 C34 56.8(8) . . . . ? C40 C36 C41 C34 -60.6(8) . . . . ? C11A C33 C42 C35 173.2(14) . . . . ? C37 C33 C42 C35 58.8(7) . . . . ? C40 C33 C42 C35 -55.9(7) . . . . ? C11 C33 C42 C35 -176.8(6) . . . . ? C38 C35 C42 C33 -63.4(8) . . . . ? C39 C35 C42 C33 58.2(8) . . . . ? C19 C18 C44 C48 7.1(8) . . . . ? C17 C18 C44 C48 -171.9(6) . . . . ? C19 C18 C44 C53 -113.1(6) . . . . ? C17 C18 C44 C53 67.9(8) . . . . ? C19 C18 C44 C51 125.2(6) . . . . ? C17 C18 C44 C51 -53.8(8) . . . . ? C19 C18 C44 C18A -117(9) . . . . ? C17 C18 C44 C18A 64(9) . . . . ? C17A C18A C44 C18 -134(10) . . . . ? C19A C18A C44 C18 45(8) . . . . ? C17A C18A C44 C48 166.4(19) . . . . ? C19A C18A C44 C48 -14.4(17) . . . . ? C17A C18A C44 C53 50(3) . . . . ? C19A C18A C44 C53 -131.2(13) . . . . ? C17A C18A C44 C51 -68(3) . . . . ? C19A C18A C44 C51 110.8(14) . . . . ? C18 C44 C48 C45 178.7(5) . . . . ? C53 C44 C48 C45 -58.5(5) . . . . ? C51 C44 C48 C45 58.6(5) . . . . ? C18A C44 C48 C45 -172.3(15) . . . . ? C52 C45 C48 C44 -59.7(6) . . . . ? C49 C45 C48 C44 59.8(6) . . . . ? C50 C46 C49 C45 -59.8(6) . . . . ? C53 C46 C49 C45 60.1(6) . . . . ? C52 C45 C49 C46 60.4(6) . . . . ? C48 C45 C49 C46 -59.1(6) . . . . ? C49 C46 C50 C47 58.9(6) . . . . ? C53 C46 C50 C47 -61.7(6) . . . . ? C52 C47 C50 C46 -58.6(6) . . . . ? C51 C47 C50 C46 61.1(6) . . . . ? C52 C47 C51 C44 61.1(6) . . . . ? C50 C47 C51 C44 -58.7(6) . . . . ? C18 C44 C51 C47 -179.8(5) . . . . ? C48 C44 C51 C47 -59.1(6) . . . . ? C53 C44 C51 C47 56.9(6) . . . . ? C18A C44 C51 C47 170.8(12) . . . . ? C49 C45 C52 C47 -60.4(6) . . . . ? C48 C45 C52 C47 58.7(6) . . . . ? C50 C47 C52 C45 59.5(6) . . . . ? C51 C47 C52 C45 -59.9(6) . . . . ? C18 C44 C53 C46 -179.8(5) . . . . ? C48 C44 C53 C46 57.9(5) . . . . ? C51 C44 C53 C46 -57.6(5) . . . . ? C18A C44 C53 C46 -179.1(13) . . . . ? C49 C46 C53 C44 -60.2(6) . . . . ? C50 C46 C53 C44 60.3(6) . . . . ? C21 C20 C54 C20A -46(13) . . . . ? C19 C20 C54 C20A 140(13) . . . . ? C19A C20A C54 C20 -29(13) . . . . ? C21A C20A C54 C20 157(15) . . . . ? O3A U1 O4 C55 -58.3(8) . . . . ? O2A U1 O4 C55 62.5(7) . . . . ? O3 U1 O4 C55 -80.1(4) . . . . ? O1 U1 O4 C55 158.9(4) . . . . ? O2 U1 O4 C55 34.3(4) . . . . ? O1A U1 O4 C55 -161.9(8) . . . . ? O5 U1 O4 C55 155.5(4) . . . . ? N1 U1 O4 C55 -18.1(5) . . . . ? O3A U1 O4 C56 140.6(7) . . . . ? O2A U1 O4 C56 -98.6(7) . . . . ? O3 U1 O4 C56 118.8(4) . . . . ? O1 U1 O4 C56 -2.2(4) . . . . ? O2 U1 O4 C56 -126.8(4) . . . . ? O1A U1 O4 C56 37.0(8) . . . . ? O5 U1 O4 C56 -5.6(3) . . . . ? N1 U1 O4 C56 -179.2(3) . . . . ? O3A U1 O5 C58 -155.9(9) . . . . ? O2A U1 O5 C58 -13.6(7) . . . . ? O3 U1 O5 C58 176.5(4) . . . . ? O1 U1 O5 C58 69.3(4) . . . . ? O2 U1 O5 C58 -44.7(4) . . . . ? O1A U1 O5 C58 96.5(7) . . . . ? N1 U1 O5 C58 58.6(5) . . . . ? O4 U1 O5 C58 -112.8(4) . . . . ? O3A U1 O5 C57 -8.9(9) . . . . ? O2A U1 O5 C57 133.4(6) . . . . ? O3 U1 O5 C57 -36.5(4) . . . . ? O1 U1 O5 C57 -143.7(3) . . . . ? O2 U1 O5 C57 102.3(3) . . . . ? O1A U1 O5 C57 -116.5(6) . . . . ? N1 U1 O5 C57 -154.4(3) . . . . ? O4 U1 O5 C57 34.2(3) . . . . ? C55 O4 C56 C57 174.7(5) . . . . ? U1 O4 C56 C57 -22.0(5) . . . . ? C58 O5 C57 C56 89.1(5) . . . . ? U1 O5 C57 C56 -62.2(5) . . . . ? O4 C56 C57 O5 54.8(6) . . . . ? C59 O6 C60 C61 -168.9(5) . . . . ? C62 O7 C61 C60 -177.9(5) . . . . ? O6 C60 C61 O7 -70.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.189 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.125 data_sd0803a _database_code_depnum_ccdc_archive 'CCDC 759476' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C109 H150 O9 U2, C7 H8, 1.5(C4 H10 O)' _chemical_formula_sum 'C122 H173 O10.50 U2' _chemical_formula_weight 2283.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.4828(18) _cell_length_b 25.766(2) _cell_length_c 25.784(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11614.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 399 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4692 _exptl_absorpt_coefficient_mu 2.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.20 \% and 360 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116536 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.10 _reflns_number_total 25130 _reflns_number_gt 18640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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 compound crystallizes with one molecule of toluene and 1.5 molecules of diethylether per formula unit. SIMU restraints were applied in the refinement of the solvent molecules and of two of the tBu groups of the ligand (C51 \^a C54 and C105 \^a C108). ; _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^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 11461 Friedel pairs used in the refinement of Flack parameter ; _refine_ls_abs_structure_Flack 0.011(4) _refine_ls_number_reflns 25130 _refine_ls_number_parameters 1278 _refine_ls_number_restraints 193 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.453869(11) 0.325490(8) 0.032540(8) 0.01592(5) Uani 1 1 d . . . U2 U 0.284898(11) 0.376104(8) 0.193231(9) 0.02211(6) Uani 1 1 d . . . O1 O 0.45168(19) 0.40836(13) 0.02720(15) 0.0202(8) Uani 1 1 d . . . O2 O 0.4513(2) 0.31089(13) -0.04963(14) 0.0204(9) Uani 1 1 d . . . O3 O 0.4534(2) 0.24390(13) 0.04938(14) 0.0193(9) Uani 1 1 d . . . O4 O 0.3584(2) 0.31930(15) 0.22978(15) 0.0264(10) Uani 1 1 d . . . O5 O 0.1871(2) 0.35621(15) 0.23790(16) 0.0276(10) Uani 1 1 d . . . O6 O 0.22946(19) 0.43560(14) 0.14854(15) 0.0245(9) Uani 1 1 d . . . O7 O 0.32261(18) 0.31788(15) 0.04667(14) 0.0198(9) Uani 1 1 d . . . O8 O 0.3757(2) 0.35245(15) 0.11681(16) 0.0262(9) Uani 1 1 d . . . O9 O 0.25496(18) 0.32582(16) 0.12076(15) 0.0237(9) Uani 1 1 d . . . C1 C 0.5916(3) 0.3347(2) 0.0945(2) 0.0195(14) Uani 1 1 d . . . C2 C 0.5970(3) 0.3785(2) 0.0619(2) 0.0181(13) Uani 1 1 d . . . C3 C 0.6068(3) 0.3727(2) 0.0080(2) 0.0177(13) Uani 1 1 d . . . C4 C 0.6083(2) 0.3222(2) -0.0137(2) 0.0166(13) Uani 1 1 d . . . C5 C 0.6095(3) 0.2780(2) 0.0192(2) 0.0188(14) Uani 1 1 d . . . C6 C 0.5974(3) 0.2846(2) 0.0730(2) 0.0186(14) Uani 1 1 d . . . C7 C 0.5805(4) 0.3410(3) 0.1525(2) 0.0392(18) Uani 1 1 d . . . H7A H 0.6089 0.3715 0.1645 0.059 Uiso 1 1 calc R . . H7B H 0.5995 0.3100 0.1703 0.059 Uiso 1 1 calc R . . H7C H 0.5260 0.3455 0.1601 0.059 Uiso 1 1 calc R . . C8 C 0.6180(3) 0.4187(2) -0.0275(3) 0.0260(14) Uani 1 1 d . . . H8A H 0.6437 0.4466 -0.0086 0.039 Uiso 1 1 calc R . . H8B H 0.5681 0.4309 -0.0398 0.039 Uiso 1 1 calc R . . H8C H 0.6494 0.4083 -0.0573 0.039 Uiso 1 1 calc R . . C9 C 0.6255(3) 0.2251(2) -0.0043(2) 0.0247(14) Uani 1 1 d . . . H9A H 0.6685 0.2277 -0.0286 0.037 Uiso 1 1 calc R . . H9B H 0.5800 0.2130 -0.0229 0.037 Uiso 1 1 calc R . . H9C H 0.6382 0.2005 0.0233 0.037 Uiso 1 1 calc R . . C10 C 0.5953(3) 0.4323(2) 0.0842(2) 0.0256(15) Uani 1 1 d . . . H10A H 0.6464 0.4478 0.0783 0.031 Uiso 1 1 calc R . . H10B H 0.5889 0.4288 0.1222 0.031 Uiso 1 1 calc R . . C11 C 0.5353(3) 0.4719(2) 0.0653(2) 0.0217(14) Uani 1 1 d . . . C12 C 0.4680(3) 0.4591(2) 0.0384(2) 0.0239(14) Uani 1 1 d . . . C13 C 0.4177(3) 0.4996(2) 0.0216(2) 0.0210(14) Uani 1 1 d . . . C14 C 0.4363(3) 0.5504(2) 0.0362(3) 0.0262(14) Uani 1 1 d . . . H14A H 0.4027 0.5775 0.0259 0.031 Uiso 1 1 calc R . . C15 C 0.5005(3) 0.5637(2) 0.0647(3) 0.0298(16) Uani 1 1 d . . . C16 C 0.5498(4) 0.5234(2) 0.0778(2) 0.0279(14) Uani 1 1 d . . . H16A H 0.5955 0.5314 0.0962 0.034 Uiso 1 1 calc R . . C17 C 0.3499(3) 0.4892(2) -0.0145(2) 0.0208(14) Uani 1 1 d . . . C18 C 0.3058(3) 0.5391(2) -0.0269(2) 0.0283(15) Uani 1 1 d . . . H18A H 0.2791 0.5511 0.0043 0.042 Uiso 1 1 calc R . . H18B H 0.2684 0.5322 -0.0543 0.042 Uiso 1 1 calc R . . H18C H 0.3416 0.5659 -0.0385 0.042 Uiso 1 1 calc R . . C19 C 0.3824(3) 0.4679(2) -0.0661(2) 0.0313(16) Uani 1 1 d . . . H19A H 0.4056 0.4338 -0.0602 0.047 Uiso 1 1 calc R . . H19B H 0.4213 0.4919 -0.0794 0.047 Uiso 1 1 calc R . . H19C H 0.3410 0.4646 -0.0915 0.047 Uiso 1 1 calc R . . C20 C 0.2927(3) 0.4511(2) 0.0097(2) 0.0273(14) Uani 1 1 d . . . H20A H 0.3172 0.4173 0.0143 0.041 Uiso 1 1 calc R . . H20B H 0.2483 0.4475 -0.0133 0.041 Uiso 1 1 calc R . . H20C H 0.2759 0.4644 0.0434 0.041 Uiso 1 1 calc R . . C21 C 0.5195(4) 0.6190(3) 0.0819(3) 0.0397(17) Uani 1 1 d . . . C22 C 0.4619(5) 0.6579(2) 0.0604(3) 0.063(2) Uani 1 1 d . . . H22A H 0.4107 0.6495 0.0735 0.094 Uiso 1 1 calc R . . H22B H 0.4618 0.6561 0.0224 0.094 Uiso 1 1 calc R . . H22C H 0.4761 0.6930 0.0714 0.094 Uiso 1 1 calc R . . C23 C 0.5993(4) 0.6348(3) 0.0624(3) 0.056(2) Uani 1 1 d . . . H23A H 0.6090 0.6712 0.0713 0.084 Uiso 1 1 calc R . . H23B H 0.6017 0.6304 0.0247 0.084 Uiso 1 1 calc R . . H23C H 0.6381 0.6128 0.0789 0.084 Uiso 1 1 calc R . . C24 C 0.5171(4) 0.6213(3) 0.1407(3) 0.053(2) Uani 1 1 d . . . H24A H 0.4668 0.6097 0.1529 0.080 Uiso 1 1 calc R . . H24B H 0.5262 0.6570 0.1522 0.080 Uiso 1 1 calc R . . H24C H 0.5568 0.5985 0.1550 0.080 Uiso 1 1 calc R . . C25 C 0.6123(3) 0.3154(2) -0.0724(2) 0.0233(15) Uani 1 1 d . . . H25A H 0.6108 0.2777 -0.0800 0.028 Uiso 1 1 calc R . . H25B H 0.6626 0.3284 -0.0843 0.028 Uiso 1 1 calc R . . C26 C 0.5503(3) 0.3418(2) -0.1050(2) 0.0203(13) Uani 1 1 d . . . C27 C 0.5734(3) 0.3710(2) -0.1474(2) 0.0205(13) Uani 1 1 d . . . H27A H 0.6265 0.3766 -0.1530 0.025 Uiso 1 1 calc R . . C28 C 0.5214(3) 0.3921(2) -0.1820(2) 0.0222(14) Uani 1 1 d . . . C29 C 0.4443(3) 0.3795(2) -0.1739(2) 0.0208(13) Uani 1 1 d . . . H29A H 0.4078 0.3921 -0.1981 0.025 Uiso 1 1 calc R . . C30 C 0.4178(3) 0.3500(2) -0.1327(2) 0.0164(13) Uani 1 1 d . . . C31 C 0.4722(3) 0.3335(2) -0.0953(2) 0.0156(13) Uani 1 1 d . . . C32 C 0.5459(4) 0.4283(2) -0.2270(2) 0.0315(15) Uani 1 1 d . . . C33 C 0.5218(4) 0.4842(3) -0.2130(3) 0.050(2) Uani 1 1 d . . . H33A H 0.5497 0.4955 -0.1821 0.075 Uiso 1 1 calc R . . H33B H 0.4667 0.4851 -0.2061 0.075 Uiso 1 1 calc R . . H33C H 0.5337 0.5073 -0.2420 0.075 Uiso 1 1 calc R . . C34 C 0.6319(4) 0.4281(3) -0.2355(3) 0.064(3) Uani 1 1 d . . . H34A H 0.6486 0.3929 -0.2446 0.096 Uiso 1 1 calc R . . H34B H 0.6577 0.4392 -0.2037 0.096 Uiso 1 1 calc R . . H34C H 0.6447 0.4519 -0.2638 0.096 Uiso 1 1 calc R . . C35 C 0.5050(4) 0.4131(3) -0.2772(3) 0.048(2) Uani 1 1 d . . . H35A H 0.5194 0.3776 -0.2868 0.073 Uiso 1 1 calc R . . H35B H 0.5199 0.4370 -0.3049 0.073 Uiso 1 1 calc R . . H35C H 0.4496 0.4149 -0.2720 0.073 Uiso 1 1 calc R . . C36 C 0.3348(3) 0.3297(2) -0.1307(2) 0.0206(13) Uani 1 1 d . . . C37 C 0.3373(3) 0.2708(2) -0.1374(3) 0.0351(17) Uani 1 1 d . . . H37A H 0.3658 0.2553 -0.1086 0.053 Uiso 1 1 calc R . . H37B H 0.3626 0.2623 -0.1703 0.053 Uiso 1 1 calc R . . H37C H 0.2850 0.2571 -0.1377 0.053 Uiso 1 1 calc R . . C38 C 0.2866(3) 0.3513(3) -0.1756(2) 0.0375(17) Uani 1 1 d . . . H38A H 0.2358 0.3353 -0.1751 0.056 Uiso 1 1 calc R . . H38B H 0.3118 0.3435 -0.2087 0.056 Uiso 1 1 calc R . . H38C H 0.2815 0.3890 -0.1718 0.056 Uiso 1 1 calc R . . C39 C 0.2928(3) 0.3420(3) -0.0807(2) 0.0386(18) Uani 1 1 d . . . H39A H 0.3147 0.3216 -0.0523 0.058 Uiso 1 1 calc R . . H39B H 0.2385 0.3333 -0.0846 0.058 Uiso 1 1 calc R . . H39C H 0.2979 0.3791 -0.0729 0.058 Uiso 1 1 calc R . . C40 C 0.5900(3) 0.2373(2) 0.1094(3) 0.0279(15) Uani 1 1 d . . . H40A H 0.6424 0.2252 0.1176 0.033 Uiso 1 1 calc R . . H40B H 0.5672 0.2497 0.1423 0.033 Uiso 1 1 calc R . . C41 C 0.5444(3) 0.1904(2) 0.0921(2) 0.0217(13) Uani 1 1 d . . . C42 C 0.4777(3) 0.1948(2) 0.0628(2) 0.0224(15) Uani 1 1 d . . . C43 C 0.4381(3) 0.1500(2) 0.0475(2) 0.0201(14) Uani 1 1 d . . . C44 C 0.4640(3) 0.1026(2) 0.0652(2) 0.0261(15) Uani 1 1 d . . . H44A H 0.4363 0.0723 0.0560 0.031 Uiso 1 1 calc R . . C45 C 0.5293(3) 0.0974(2) 0.0959(3) 0.0307(16) Uani 1 1 d . . . C46 C 0.5688(3) 0.1413(2) 0.1073(2) 0.0219(14) Uani 1 1 d . . . H46A H 0.6150 0.1384 0.1265 0.026 Uiso 1 1 calc R . . C47 C 0.3670(3) 0.1526(2) 0.0108(2) 0.0224(14) Uani 1 1 d . . . C48 C 0.3049(3) 0.1868(2) 0.0342(3) 0.0347(16) Uani 1 1 d . . . H48A H 0.3240 0.2223 0.0377 0.052 Uiso 1 1 calc R . . H48B H 0.2907 0.1734 0.0685 0.052 Uiso 1 1 calc R . . H48C H 0.2599 0.1866 0.0115 0.052 Uiso 1 1 calc R . . C49 C 0.3314(3) 0.0993(2) 0.0011(3) 0.0280(15) Uani 1 1 d . . . H49A H 0.3119 0.0852 0.0338 0.042 Uiso 1 1 calc R . . H49B H 0.3703 0.0758 -0.0131 0.042 Uiso 1 1 calc R . . H49C H 0.2893 0.1027 -0.0238 0.042 Uiso 1 1 calc R . . C50 C 0.3918(3) 0.1745(2) -0.0412(2) 0.0325(15) Uani 1 1 d . . . H50A H 0.4100 0.2102 -0.0366 0.049 Uiso 1 1 calc R . . H50B H 0.3483 0.1743 -0.0652 0.049 Uiso 1 1 calc R . . H50C H 0.4331 0.1532 -0.0555 0.049 Uiso 1 1 calc R . . C51 C 0.5540(4) 0.0437(3) 0.1172(3) 0.0498(18) Uani 1 1 d U . . C52 C 0.5590(6) 0.0040(3) 0.0735(4) 0.082(3) Uani 1 1 d U . . H52A H 0.5880 0.0187 0.0444 0.124 Uiso 1 1 calc R . . H52B H 0.5074 -0.0051 0.0618 0.124 Uiso 1 1 calc R . . H52C H 0.5850 -0.0273 0.0861 0.124 Uiso 1 1 calc R . . C53 C 0.6318(5) 0.0433(3) 0.1399(5) 0.095(3) Uani 1 1 d U . . H53A H 0.6349 0.0695 0.1674 0.142 Uiso 1 1 calc R . . H53B H 0.6694 0.0514 0.1129 0.142 Uiso 1 1 calc R . . H53C H 0.6426 0.0090 0.1544 0.142 Uiso 1 1 calc R . . C54 C 0.4980(5) 0.0255(4) 0.1568(4) 0.089(3) Uani 1 1 d U . . H54A H 0.5125 -0.0092 0.1687 0.134 Uiso 1 1 calc R . . H54B H 0.4468 0.0242 0.1414 0.134 Uiso 1 1 calc R . . H54C H 0.4979 0.0495 0.1862 0.134 Uiso 1 1 calc R . . C55 C 0.3958(3) 0.4524(2) 0.2272(2) 0.0258(15) Uani 1 1 d . . . C56 C 0.3939(3) 0.4174(2) 0.2695(2) 0.0258(15) Uani 1 1 d . . . C57 C 0.3261(4) 0.4100(2) 0.2979(2) 0.0284(15) Uani 1 1 d . . . C58 C 0.2623(3) 0.4421(2) 0.2881(2) 0.0271(16) Uani 1 1 d . . . C59 C 0.2663(3) 0.4801(2) 0.2502(3) 0.0276(16) Uani 1 1 d . . . C60 C 0.3300(3) 0.4838(2) 0.2167(2) 0.0252(15) Uani 1 1 d . . . C61 C 0.4664(3) 0.4575(2) 0.1930(3) 0.0387(16) Uani 1 1 d . . . H61A H 0.4884 0.4922 0.1972 0.058 Uiso 1 1 calc R . . H61B H 0.4520 0.4522 0.1567 0.058 Uiso 1 1 calc R . . H61C H 0.5043 0.4314 0.2032 0.058 Uiso 1 1 calc R . . C62 C 0.3219(4) 0.3690(3) 0.3389(2) 0.0439(18) Uani 1 1 d . . . H62A H 0.3305 0.3848 0.3730 0.066 Uiso 1 1 calc R . . H62B H 0.3613 0.3427 0.3324 0.066 Uiso 1 1 calc R . . H62C H 0.2713 0.3527 0.3382 0.066 Uiso 1 1 calc R . . C63 C 0.2010(3) 0.5198(3) 0.2459(3) 0.0389(18) Uani 1 1 d . . . H63A H 0.1867 0.5318 0.2806 0.058 Uiso 1 1 calc R . . H63B H 0.1567 0.5035 0.2292 0.058 Uiso 1 1 calc R . . H63C H 0.2180 0.5495 0.2251 0.058 Uiso 1 1 calc R . . C64 C 0.4647(3) 0.3893(2) 0.2866(3) 0.0333(16) Uani 1 1 d . . . H64A H 0.4651 0.3897 0.3250 0.040 Uiso 1 1 calc R . . H64B H 0.5090 0.4103 0.2751 0.040 Uiso 1 1 calc R . . C65 C 0.4802(3) 0.3332(2) 0.2697(2) 0.0248(14) Uani 1 1 d . . . C66 C 0.4271(3) 0.2995(2) 0.2459(2) 0.0271(15) Uani 1 1 d . . . C67 C 0.4441(3) 0.2463(2) 0.2399(2) 0.0244(14) Uani 1 1 d . . . C68 C 0.5176(3) 0.2306(2) 0.2547(2) 0.0287(15) Uani 1 1 d . . . H68A H 0.5299 0.1949 0.2503 0.034 Uiso 1 1 calc R . . C69 C 0.5734(3) 0.2621(3) 0.2751(2) 0.0293(16) Uani 1 1 d . . . C70 C 0.5514(4) 0.3139(2) 0.2832(2) 0.0319(15) Uani 1 1 d . . . H70A H 0.5872 0.3369 0.2987 0.038 Uiso 1 1 calc R . . C71 C 0.3829(3) 0.2068(2) 0.2240(3) 0.0282(15) Uani 1 1 d . . . C72 C 0.4166(4) 0.1517(2) 0.2165(3) 0.0443(19) Uani 1 1 d . . . H72A H 0.4404 0.1402 0.2489 0.066 Uiso 1 1 calc R . . H72B H 0.4552 0.1525 0.1889 0.066 Uiso 1 1 calc R . . H72C H 0.3756 0.1276 0.2069 0.066 Uiso 1 1 calc R . . C73 C 0.3440(4) 0.2196(2) 0.1719(2) 0.0348(17) Uani 1 1 d . . . H73A H 0.3833 0.2268 0.1457 0.052 Uiso 1 1 calc R . . H73B H 0.3113 0.2502 0.1761 0.052 Uiso 1 1 calc R . . H73C H 0.3129 0.1900 0.1607 0.052 Uiso 1 1 calc R . . C74 C 0.3228(4) 0.2044(3) 0.2675(3) 0.0408(18) Uani 1 1 d . . . H74A H 0.3478 0.1956 0.3004 0.061 Uiso 1 1 calc R . . H74B H 0.2845 0.1779 0.2592 0.061 Uiso 1 1 calc R . . H74C H 0.2976 0.2383 0.2708 0.061 Uiso 1 1 calc R . . C75 C 0.6544(4) 0.2449(3) 0.2900(3) 0.0389(18) Uani 1 1 d . . . C76 C 0.6735(4) 0.2621(3) 0.3461(3) 0.062(2) Uani 1 1 d . . . H76A H 0.6340 0.2492 0.3698 0.094 Uiso 1 1 calc R . . H76B H 0.6752 0.3001 0.3477 0.094 Uiso 1 1 calc R . . H76C H 0.7233 0.2479 0.3562 0.094 Uiso 1 1 calc R . . C77 C 0.7121(4) 0.2693(3) 0.2544(3) 0.0470(19) Uani 1 1 d . . . H77A H 0.7045 0.2563 0.2191 0.071 Uiso 1 1 calc R . . H77B H 0.7638 0.2606 0.2662 0.071 Uiso 1 1 calc R . . H77C H 0.7056 0.3071 0.2548 0.071 Uiso 1 1 calc R . . C78 C 0.6634(4) 0.1859(3) 0.2866(3) 0.049(2) Uani 1 1 d . . . H78A H 0.6495 0.1742 0.2517 0.073 Uiso 1 1 calc R . . H78B H 0.6299 0.1693 0.3121 0.073 Uiso 1 1 calc R . . H78C H 0.7167 0.1765 0.2937 0.073 Uiso 1 1 calc R . . C79 C 0.1923(3) 0.4364(3) 0.3221(3) 0.0387(18) Uani 1 1 d . . . H79A H 0.1685 0.4713 0.3243 0.046 Uiso 1 1 calc R . . H79B H 0.2110 0.4280 0.3574 0.046 Uiso 1 1 calc R . . C80 C 0.1274(3) 0.3980(2) 0.3103(3) 0.0286(15) Uani 1 1 d . . . C81 C 0.1283(3) 0.3596(2) 0.2723(2) 0.0269(15) Uani 1 1 d . . . C82 C 0.0664(3) 0.3235(2) 0.2696(2) 0.0286(14) Uani 1 1 d . . . C83 C 0.0051(3) 0.3308(2) 0.3033(3) 0.0334(15) Uani 1 1 d . . . H83A H -0.0370 0.3076 0.3008 0.040 Uiso 1 1 calc R . . C84 C 0.0014(3) 0.3702(3) 0.3407(2) 0.0338(16) Uani 1 1 d . . . C85 C 0.0645(3) 0.4026(2) 0.3436(2) 0.0314(16) Uani 1 1 d . . . H85A H 0.0651 0.4291 0.3693 0.038 Uiso 1 1 calc R . . C86 C 0.0655(3) 0.2770(2) 0.2319(3) 0.0333(17) Uani 1 1 d . . . C87 C 0.1380(4) 0.2456(3) 0.2371(3) 0.053(2) Uani 1 1 d . . . H87A H 0.1419 0.2321 0.2725 0.079 Uiso 1 1 calc R . . H87B H 0.1822 0.2678 0.2297 0.079 Uiso 1 1 calc R . . H87C H 0.1369 0.2166 0.2125 0.079 Uiso 1 1 calc R . . C88 C -0.0033(4) 0.2408(3) 0.2418(3) 0.047(2) Uani 1 1 d . . . H88A H -0.0029 0.2293 0.2780 0.070 Uiso 1 1 calc R . . H88B H 0.0001 0.2105 0.2189 0.070 Uiso 1 1 calc R . . H88C H -0.0510 0.2595 0.2347 0.070 Uiso 1 1 calc R . . C89 C 0.0585(4) 0.2961(3) 0.1748(3) 0.0443(19) Uani 1 1 d . . . H89A H 0.1006 0.3200 0.1670 0.066 Uiso 1 1 calc R . . H89B H 0.0096 0.3140 0.1701 0.066 Uiso 1 1 calc R . . H89C H 0.0610 0.2662 0.1513 0.066 Uiso 1 1 calc R . . C90 C -0.0691(4) 0.3745(3) 0.3758(3) 0.052(2) Uani 1 1 d . . . C91 C -0.0616(4) 0.4187(3) 0.4145(3) 0.050(2) Uani 1 1 d . . . H91A H -0.0174 0.4125 0.4370 0.075 Uiso 1 1 calc R . . H91B H -0.1081 0.4207 0.4356 0.075 Uiso 1 1 calc R . . H91C H -0.0546 0.4515 0.3958 0.075 Uiso 1 1 calc R . . C92 C -0.1406(4) 0.3852(4) 0.3415(3) 0.077(3) Uani 1 1 d . . . H92A H -0.1320 0.4166 0.3208 0.116 Uiso 1 1 calc R . . H92B H -0.1854 0.3903 0.3638 0.116 Uiso 1 1 calc R . . H92C H -0.1494 0.3557 0.3184 0.116 Uiso 1 1 calc R . . C93 C -0.0808(5) 0.3239(3) 0.4058(3) 0.074(3) Uani 1 1 d . . . H93A H -0.0361 0.3173 0.4277 0.111 Uiso 1 1 calc R . . H93B H -0.0873 0.2952 0.3812 0.111 Uiso 1 1 calc R . . H93C H -0.1265 0.3268 0.4275 0.111 Uiso 1 1 calc R . . C94 C 0.3321(3) 0.5188(3) 0.1690(3) 0.0356(17) Uani 1 1 d . . . H94A H 0.3493 0.5537 0.1802 0.043 Uiso 1 1 calc R . . H94B H 0.3714 0.5051 0.1450 0.043 Uiso 1 1 calc R . . C95 C 0.2582(3) 0.5254(3) 0.1387(3) 0.0308(16) Uani 1 1 d . . . C96 C 0.2072(3) 0.4831(2) 0.1309(2) 0.0238(14) Uani 1 1 d . . . C97 C 0.1370(3) 0.4916(2) 0.1064(2) 0.0259(15) Uani 1 1 d . . . C98 C 0.1223(3) 0.5399(3) 0.0876(3) 0.0373(18) Uani 1 1 d . . . H98A H 0.0741 0.5454 0.0715 0.045 Uiso 1 1 calc R . . C99 C 0.1734(4) 0.5828(2) 0.0902(3) 0.0406(18) Uani 1 1 d . . . C100 C 0.2401(3) 0.5737(3) 0.1179(3) 0.0375(18) Uani 1 1 d . . . H10C H 0.2748 0.6016 0.1229 0.045 Uiso 1 1 calc R . . C101 C 0.0747(3) 0.4488(2) 0.1045(3) 0.0325(17) Uani 1 1 d . . . C102 C 0.0021(3) 0.4682(3) 0.0783(3) 0.047(2) Uani 1 1 d . . . H10D H 0.0136 0.4782 0.0425 0.071 Uiso 1 1 calc R . . H10E H -0.0177 0.4983 0.0972 0.071 Uiso 1 1 calc R . . H10F H -0.0364 0.4405 0.0783 0.071 Uiso 1 1 calc R . . C103 C 0.1031(3) 0.4022(2) 0.0722(3) 0.0336(17) Uani 1 1 d . . . H10G H 0.1063 0.4123 0.0356 0.050 Uiso 1 1 calc R . . H10H H 0.0672 0.3732 0.0759 0.050 Uiso 1 1 calc R . . H10I H 0.1537 0.3916 0.0845 0.050 Uiso 1 1 calc R . . C104 C 0.0540(3) 0.4335(3) 0.1602(3) 0.0375(17) Uani 1 1 d . . . H10J H 0.0110 0.4090 0.1596 0.056 Uiso 1 1 calc R . . H10K H 0.0395 0.4646 0.1797 0.056 Uiso 1 1 calc R . . H10L H 0.0982 0.4170 0.1767 0.056 Uiso 1 1 calc R . . C105 C 0.1535(5) 0.6354(3) 0.0680(4) 0.072(2) Uani 1 1 d U . . C106 C 0.2234(5) 0.6687(3) 0.0582(4) 0.087(3) Uani 1 1 d U . . H10M H 0.2483 0.6768 0.0912 0.131 Uiso 1 1 calc R . . H10N H 0.2078 0.7010 0.0411 0.131 Uiso 1 1 calc R . . H10O H 0.2592 0.6499 0.0358 0.131 Uiso 1 1 calc R . . C107 C 0.0999(7) 0.6628(4) 0.1037(5) 0.125(4) Uani 1 1 d U . . H10P H 0.1227 0.6650 0.1383 0.188 Uiso 1 1 calc R . . H10Q H 0.0516 0.6435 0.1056 0.188 Uiso 1 1 calc R . . H10R H 0.0901 0.6979 0.0906 0.188 Uiso 1 1 calc R . . C108 C 0.1174(5) 0.6303(4) 0.0125(4) 0.099(3) Uani 1 1 d U . . H10S H 0.1056 0.6650 -0.0010 0.149 Uiso 1 1 calc R . . H10T H 0.0703 0.6098 0.0146 0.149 Uiso 1 1 calc R . . H10U H 0.1538 0.6131 -0.0107 0.149 Uiso 1 1 calc R . . C109 C 0.3167(3) 0.3312(2) 0.0943(3) 0.0225(14) Uani 1 1 d . . . C201 C 0.7779(6) 0.5636(5) 0.7311(5) 0.123(3) Uani 1 1 d U . . H201 H 0.7810 0.5934 0.7526 0.147 Uiso 1 1 calc R . . C202 C 0.8236(7) 0.5211(6) 0.7441(6) 0.129(3) Uani 1 1 d U . . H202 H 0.8564 0.5200 0.7735 0.155 Uiso 1 1 calc R . . C203 C 0.8152(7) 0.4802(6) 0.7087(6) 0.130(3) Uani 1 1 d U . . H203 H 0.8453 0.4500 0.7142 0.156 Uiso 1 1 calc R . . C204 C 0.7688(7) 0.4804(6) 0.6683(6) 0.133(3) Uani 1 1 d U . . H204 H 0.7643 0.4500 0.6477 0.159 Uiso 1 1 calc R . . C205 C 0.7272(7) 0.5233(6) 0.6557(6) 0.128(3) Uani 1 1 d U . . H205 H 0.6975 0.5248 0.6249 0.153 Uiso 1 1 calc R . . C206 C 0.7304(7) 0.5656(6) 0.6908(6) 0.121(3) Uani 1 1 d U . . C207 C 0.6848(6) 0.6117(5) 0.6784(5) 0.135(4) Uani 1 1 d U . . H20D H 0.6531 0.6210 0.7083 0.202 Uiso 1 1 calc R . . H20E H 0.6518 0.6042 0.6486 0.202 Uiso 1 1 calc R . . H20F H 0.7190 0.6406 0.6699 0.202 Uiso 1 1 calc R . . C301 C 0.1484(15) 0.1111(10) 0.4084(11) 0.353(8) Uani 1 1 d DU . . H30A H 0.1886 0.0868 0.3977 0.530 Uiso 1 1 calc R . . H30B H 0.0984 0.0943 0.4050 0.530 Uiso 1 1 calc R . . H30C H 0.1567 0.1213 0.4445 0.530 Uiso 1 1 calc R . . C302 C 0.1510(16) 0.1588(11) 0.3741(11) 0.344(7) Uani 1 1 d DU . . H30D H 0.1961 0.1593 0.3508 0.413 Uiso 1 1 calc R . . H30E H 0.1035 0.1636 0.3537 0.413 Uiso 1 1 calc R . . O303 O 0.1578(11) 0.1969(9) 0.4185(8) 0.343(7) Uani 1 1 d DU . . C304 C 0.1557(17) 0.2467(11) 0.3923(10) 0.344(7) Uani 1 1 d DU . . H30F H 0.1064 0.2503 0.3737 0.413 Uiso 1 1 calc R . . H30G H 0.1974 0.2483 0.3664 0.413 Uiso 1 1 calc R . . C305 C 0.1646(15) 0.2918(10) 0.4312(11) 0.344(8) Uani 1 1 d DU . . H30H H 0.1913 0.2794 0.4622 0.516 Uiso 1 1 calc R . . H30I H 0.1140 0.3049 0.4409 0.516 Uiso 1 1 calc R . . H30J H 0.1943 0.3198 0.4151 0.516 Uiso 1 1 calc R . . C401 C 0.7288(18) 0.4860(12) 0.3946(13) 0.197(8) Uani 0.50 1 d PDU . . H40C H 0.7614 0.5156 0.4035 0.296 Uiso 0.50 1 calc PR . . H40D H 0.6808 0.4986 0.3795 0.296 Uiso 0.50 1 calc PR . . H40E H 0.7552 0.4639 0.3693 0.296 Uiso 0.50 1 calc PR . . C402 C 0.711(2) 0.4539(13) 0.4443(13) 0.205(7) Uani 0.50 1 d PDU . . H40F H 0.7550 0.4331 0.4570 0.246 Uiso 0.50 1 calc PR . . H40G H 0.6882 0.4745 0.4727 0.246 Uiso 0.50 1 calc PR . . O403 O 0.6531(13) 0.4228(9) 0.4124(10) 0.209(7) Uani 0.50 1 d PDU . . C404 C 0.6313(19) 0.3894(13) 0.4584(13) 0.210(7) Uani 0.50 1 d PDU . . H40H H 0.6096 0.4101 0.4872 0.252 Uiso 0.50 1 calc PR . . H40I H 0.6746 0.3682 0.4710 0.252 Uiso 0.50 1 calc PR . . C405 C 0.5696(18) 0.3562(12) 0.4303(13) 0.209(8) Uani 0.50 1 d PDU . . H40J H 0.5396 0.3370 0.4561 0.314 Uiso 0.50 1 calc PR . . H40K H 0.5947 0.3316 0.4068 0.314 Uiso 0.50 1 calc PR . . H40L H 0.5358 0.3790 0.4103 0.314 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01241(10) 0.01848(11) 0.01687(12) 0.00110(11) -0.00194(9) 0.00122(9) U2 0.02215(11) 0.02312(12) 0.02107(13) -0.00803(11) 0.00048(10) -0.00136(10) O1 0.0193(18) 0.021(2) 0.020(2) 0.0022(18) -0.002(2) 0.0033(17) O2 0.0187(18) 0.025(2) 0.017(2) 0.0068(17) -0.0027(17) 0.0005(17) O3 0.0127(18) 0.021(2) 0.024(2) -0.0006(17) -0.0005(17) 0.0007(17) O4 0.028(2) 0.025(2) 0.026(3) -0.006(2) -0.0024(18) 0.0041(19) O5 0.027(2) 0.029(2) 0.027(3) -0.010(2) 0.0057(18) -0.0095(17) O6 0.023(2) 0.023(2) 0.028(3) -0.003(2) -0.0030(18) -0.0038(17) O7 0.0128(18) 0.028(2) 0.018(2) -0.0021(19) 0.0001(15) -0.0004(16) O8 0.017(2) 0.032(2) 0.029(3) -0.007(2) -0.0047(18) -0.0005(17) O9 0.0167(19) 0.030(2) 0.024(2) -0.007(2) 0.0023(17) -0.0031(18) C1 0.016(3) 0.030(4) 0.013(3) 0.002(3) -0.004(2) 0.006(3) C2 0.013(3) 0.029(3) 0.012(3) -0.001(3) -0.007(2) -0.001(3) C3 0.007(3) 0.022(3) 0.024(3) 0.001(3) -0.002(2) -0.001(3) C4 0.001(2) 0.030(3) 0.018(3) 0.000(3) -0.002(2) -0.002(2) C5 0.004(3) 0.021(3) 0.032(4) -0.002(3) -0.004(2) -0.003(2) C6 0.010(3) 0.030(4) 0.017(4) -0.003(3) -0.008(2) -0.003(2) C7 0.067(5) 0.031(4) 0.020(4) 0.003(3) -0.001(3) 0.010(3) C8 0.021(3) 0.023(3) 0.034(4) 0.002(3) 0.004(3) -0.004(2) C9 0.016(3) 0.028(4) 0.030(4) 0.003(3) 0.004(3) 0.005(3) C10 0.023(3) 0.028(4) 0.026(4) 0.001(3) -0.007(3) 0.000(3) C11 0.020(3) 0.024(3) 0.022(4) 0.002(3) -0.005(3) 0.000(3) C12 0.025(3) 0.025(3) 0.022(4) -0.003(3) 0.004(3) -0.001(2) C13 0.019(3) 0.024(3) 0.020(4) 0.001(3) 0.004(2) 0.004(2) C14 0.027(3) 0.023(3) 0.029(4) 0.005(3) 0.000(3) 0.001(2) C15 0.042(4) 0.017(3) 0.030(4) -0.005(3) 0.006(3) 0.003(3) C16 0.030(3) 0.025(3) 0.028(4) -0.004(3) -0.004(3) 0.000(3) C17 0.019(3) 0.023(3) 0.020(4) 0.003(3) 0.000(2) 0.007(2) C18 0.029(3) 0.031(4) 0.025(4) -0.001(3) -0.005(3) 0.003(3) C19 0.037(4) 0.030(4) 0.027(4) 0.004(3) -0.002(3) -0.002(3) C20 0.022(3) 0.034(4) 0.026(4) -0.007(3) 0.000(3) 0.000(3) C21 0.049(4) 0.020(4) 0.050(5) -0.006(4) -0.006(3) -0.004(3) C22 0.080(6) 0.022(4) 0.087(7) -0.017(4) -0.037(5) 0.003(4) C23 0.070(5) 0.023(4) 0.075(6) -0.014(4) 0.013(4) -0.014(4) C24 0.075(5) 0.036(4) 0.050(5) -0.023(4) -0.009(4) 0.003(4) C25 0.017(3) 0.031(4) 0.022(4) -0.007(3) -0.002(2) 0.009(3) C26 0.010(3) 0.028(3) 0.022(3) 0.001(3) -0.002(3) 0.000(3) C27 0.016(3) 0.025(3) 0.020(3) -0.005(3) 0.002(2) 0.004(3) C28 0.021(3) 0.024(3) 0.022(4) -0.006(3) 0.006(2) 0.006(2) C29 0.019(3) 0.026(3) 0.018(3) 0.000(3) -0.010(2) 0.011(3) C30 0.015(3) 0.018(3) 0.016(3) 0.002(3) -0.006(2) 0.001(2) C31 0.022(3) 0.011(3) 0.013(3) -0.002(2) 0.006(2) 0.000(2) C32 0.031(3) 0.035(4) 0.029(4) 0.012(3) -0.001(3) 0.005(3) C33 0.070(5) 0.031(4) 0.049(5) 0.012(4) -0.003(4) -0.010(3) C34 0.035(4) 0.096(7) 0.061(6) 0.049(5) 0.016(4) 0.005(4) C35 0.065(5) 0.048(5) 0.032(5) 0.010(4) 0.013(4) 0.004(4) C36 0.018(3) 0.024(3) 0.020(3) 0.005(3) -0.004(2) 0.002(3) C37 0.024(3) 0.035(4) 0.046(5) 0.004(4) -0.008(3) -0.007(3) C38 0.020(3) 0.053(4) 0.039(4) 0.015(3) -0.009(3) -0.004(3) C39 0.027(3) 0.061(5) 0.028(4) -0.012(3) 0.006(3) -0.022(3) C40 0.027(3) 0.026(4) 0.030(4) 0.005(3) -0.004(3) 0.003(3) C41 0.013(3) 0.022(3) 0.030(4) 0.004(3) 0.003(3) -0.002(3) C42 0.015(3) 0.024(3) 0.028(4) 0.012(3) -0.001(3) 0.003(2) C43 0.016(3) 0.018(3) 0.027(4) 0.002(3) 0.004(2) 0.001(2) C44 0.016(3) 0.028(4) 0.035(4) 0.007(3) 0.004(3) -0.005(3) C45 0.023(4) 0.029(4) 0.041(4) 0.013(3) 0.005(3) 0.002(3) C46 0.010(3) 0.028(4) 0.028(4) 0.013(3) 0.000(2) -0.002(2) C47 0.016(3) 0.026(3) 0.025(4) -0.001(3) 0.001(3) 0.002(2) C48 0.014(3) 0.037(4) 0.053(5) -0.004(4) -0.001(3) -0.001(2) C49 0.020(3) 0.032(4) 0.032(4) 0.002(3) -0.004(3) -0.003(3) C50 0.033(3) 0.032(3) 0.033(4) -0.004(4) -0.007(3) -0.009(3) C51 0.042(4) 0.024(3) 0.083(5) 0.030(3) -0.001(4) 0.006(3) C52 0.109(6) 0.045(5) 0.093(7) 0.023(5) 0.000(6) 0.023(5) C53 0.073(5) 0.054(5) 0.157(8) 0.056(5) -0.038(6) -0.001(4) C54 0.093(6) 0.065(5) 0.109(7) 0.061(5) 0.022(5) 0.019(5) C55 0.022(3) 0.029(4) 0.026(4) -0.016(3) -0.001(3) -0.006(3) C56 0.029(3) 0.024(4) 0.024(4) -0.011(3) -0.004(3) 0.000(3) C57 0.046(4) 0.021(3) 0.019(4) -0.011(3) -0.008(3) -0.009(3) C58 0.031(4) 0.028(4) 0.022(4) -0.022(3) 0.001(3) -0.008(3) C59 0.023(3) 0.030(4) 0.030(4) -0.019(3) -0.004(3) -0.004(3) C60 0.027(3) 0.022(4) 0.027(4) -0.007(3) 0.000(3) -0.003(3) C61 0.027(3) 0.050(4) 0.039(4) 0.000(4) 0.005(3) 0.004(3) C62 0.057(4) 0.052(5) 0.022(4) -0.007(4) 0.002(3) -0.007(4) C63 0.031(4) 0.040(4) 0.045(5) -0.024(4) 0.002(3) 0.009(3) C64 0.033(4) 0.034(4) 0.033(4) -0.007(3) -0.008(3) 0.008(3) C65 0.033(3) 0.023(4) 0.018(3) -0.004(3) -0.001(3) -0.001(3) C66 0.030(4) 0.036(4) 0.016(4) -0.003(3) 0.006(3) 0.006(3) C67 0.034(4) 0.026(3) 0.013(3) -0.001(3) 0.007(3) 0.005(3) C68 0.045(4) 0.024(4) 0.018(4) 0.005(3) 0.010(3) 0.006(3) C69 0.031(4) 0.037(4) 0.020(4) 0.003(3) 0.008(3) 0.005(3) C70 0.037(4) 0.038(4) 0.020(3) 0.004(3) -0.001(3) -0.003(3) C71 0.042(4) 0.018(3) 0.024(4) -0.001(3) -0.003(3) 0.007(3) C72 0.068(5) 0.022(4) 0.043(5) 0.002(3) -0.002(4) -0.007(3) C73 0.052(4) 0.026(4) 0.027(4) -0.007(3) 0.001(3) -0.007(3) C74 0.038(4) 0.053(5) 0.031(4) -0.007(4) 0.007(3) -0.012(3) C75 0.036(4) 0.042(4) 0.039(5) 0.008(4) 0.003(3) 0.011(3) C76 0.058(5) 0.087(7) 0.043(6) -0.001(5) -0.019(4) 0.030(5) C77 0.035(4) 0.047(4) 0.059(5) 0.005(4) 0.002(4) 0.002(4) C78 0.043(4) 0.041(5) 0.063(6) 0.004(4) 0.011(4) 0.011(3) C79 0.038(4) 0.038(4) 0.040(5) -0.015(3) 0.014(3) -0.013(3) C80 0.024(3) 0.029(3) 0.033(4) -0.005(3) -0.002(3) 0.000(3) C81 0.019(3) 0.037(4) 0.025(4) -0.007(3) 0.004(3) -0.008(3) C82 0.038(4) 0.027(3) 0.021(4) -0.005(3) 0.000(3) -0.005(3) C83 0.030(3) 0.035(4) 0.035(4) -0.005(4) 0.005(3) -0.014(3) C84 0.036(4) 0.035(4) 0.031(4) -0.014(4) 0.010(3) -0.007(3) C85 0.044(4) 0.028(4) 0.022(4) -0.012(3) 0.006(3) -0.002(3) C86 0.038(4) 0.030(4) 0.032(4) -0.010(3) 0.005(3) -0.007(3) C87 0.048(5) 0.039(5) 0.071(6) -0.018(4) 0.010(4) -0.007(4) C88 0.046(4) 0.041(5) 0.053(5) -0.017(4) 0.008(4) -0.024(3) C89 0.053(5) 0.038(4) 0.042(5) -0.018(4) 0.001(4) -0.013(4) C90 0.045(4) 0.062(5) 0.050(5) -0.021(5) 0.020(4) -0.017(4) C91 0.048(5) 0.062(5) 0.039(5) -0.013(4) 0.025(4) -0.012(4) C92 0.037(5) 0.111(8) 0.083(7) -0.052(6) 0.005(4) -0.011(5) C93 0.096(6) 0.057(6) 0.070(7) -0.025(5) 0.051(5) -0.034(5) C94 0.028(4) 0.031(4) 0.048(5) 0.006(4) -0.007(3) -0.006(3) C95 0.031(4) 0.029(4) 0.032(4) -0.005(3) 0.001(3) -0.001(3) C96 0.028(3) 0.023(3) 0.021(4) -0.009(3) 0.001(3) 0.002(3) C97 0.030(4) 0.021(4) 0.027(4) -0.010(3) -0.005(3) 0.008(3) C98 0.027(4) 0.040(4) 0.045(5) -0.018(4) -0.009(3) 0.011(3) C99 0.049(4) 0.025(4) 0.048(5) -0.008(4) -0.019(4) 0.003(3) C100 0.037(4) 0.027(4) 0.049(5) -0.006(4) -0.009(3) -0.003(3) C101 0.021(3) 0.028(4) 0.048(5) -0.016(3) -0.008(3) 0.000(3) C102 0.033(4) 0.042(5) 0.066(6) -0.017(4) -0.020(4) 0.002(3) C103 0.033(4) 0.030(4) 0.038(5) -0.010(3) -0.003(3) 0.001(3) C104 0.021(3) 0.040(4) 0.051(5) -0.008(4) 0.010(3) -0.008(3) C105 0.085(5) 0.030(4) 0.100(6) 0.017(4) -0.020(4) 0.011(4) C106 0.110(6) 0.036(4) 0.116(7) 0.029(5) -0.038(6) -0.010(5) C107 0.160(8) 0.061(6) 0.154(9) 0.028(6) 0.051(7) 0.047(6) C108 0.110(6) 0.068(6) 0.120(8) 0.034(6) -0.059(6) -0.002(5) C109 0.019(3) 0.012(3) 0.037(4) -0.004(3) -0.003(3) 0.006(3) C201 0.082(5) 0.132(6) 0.154(7) 0.061(5) 0.024(5) -0.011(5) C202 0.085(5) 0.144(6) 0.158(7) 0.057(6) 0.039(5) -0.007(5) C203 0.084(5) 0.149(6) 0.158(8) 0.054(6) 0.059(5) -0.002(5) C204 0.094(5) 0.152(6) 0.153(7) 0.049(6) 0.063(5) -0.007(5) C205 0.091(5) 0.143(6) 0.150(7) 0.052(6) 0.048(5) -0.014(5) C206 0.086(5) 0.130(6) 0.146(7) 0.058(5) 0.025(5) -0.015(5) C207 0.108(7) 0.144(9) 0.152(9) 0.063(7) -0.035(6) -0.025(7) C301 0.352(10) 0.349(10) 0.360(10) 0.004(7) -0.001(7) -0.007(7) C302 0.346(7) 0.344(8) 0.344(8) 0.002(4) -0.002(4) -0.001(4) O303 0.344(7) 0.342(7) 0.342(7) 0.000(4) -0.001(4) 0.000(4) C304 0.346(7) 0.344(8) 0.342(8) -0.002(4) -0.002(4) -0.001(4) C305 0.350(10) 0.341(10) 0.340(10) -0.001(7) 0.002(7) 0.006(7) C401 0.193(10) 0.199(10) 0.199(10) -0.020(7) -0.001(7) 0.019(7) C402 0.203(7) 0.204(8) 0.209(8) -0.006(4) 0.003(4) 0.007(4) O403 0.209(7) 0.209(7) 0.211(7) -0.004(4) 0.005(4) 0.010(4) C404 0.210(7) 0.209(8) 0.211(8) -0.002(4) 0.007(4) 0.007(4) C405 0.210(10) 0.212(10) 0.205(10) -0.011(7) 0.011(7) 0.022(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.140(3) . ? U1 O3 2.147(3) . ? U1 O2 2.152(4) . ? U1 O7 2.332(3) . ? U1 O8 2.659(4) . ? U1 C109 2.882(6) . ? U1 C1 2.899(5) . ? U1 C6 2.914(5) . ? U1 C2 2.949(5) . ? U1 C4 2.952(5) . ? U1 C5 3.004(5) . ? U1 C3 3.005(5) . ? U2 O5 2.125(4) . ? U2 O6 2.149(4) . ? U2 O4 2.163(4) . ? U2 O9 2.333(4) . ? U2 O8 2.603(4) . ? U2 C109 2.856(6) . ? U2 C55 2.897(5) . ? U2 C57 2.928(6) . ? U2 C56 2.939(6) . ? U2 C60 2.947(6) . ? U2 C58 3.007(6) . ? O1 C12 1.369(6) . ? O2 C31 1.364(6) . ? O3 C42 1.377(6) . ? O4 C66 1.371(7) . ? O5 C81 1.359(6) . ? O6 C96 1.362(7) . ? O7 C109 1.279(7) . ? O8 C109 1.305(6) . ? O9 C109 1.285(6) . ? C1 C6 1.408(8) . ? C1 C2 1.409(8) . ? C1 C7 1.516(8) . ? C2 C3 1.408(7) . ? C2 C10 1.501(8) . ? C3 C4 1.417(8) . ? C3 C8 1.511(8) . ? C4 C5 1.418(8) . ? C4 C25 1.526(8) . ? C5 C6 1.415(8) . ? C5 C9 1.519(8) . ? C6 C40 1.543(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.545(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.388(8) . ? C11 C12 1.405(8) . ? C12 C13 1.429(8) . ? C13 C14 1.401(8) . ? C13 C17 1.531(8) . ? C14 C15 1.384(8) . ? C14 H14A 0.9500 . ? C15 C16 1.393(8) . ? C15 C21 1.529(9) . ? C16 H16A 0.9500 . ? C17 C20 1.532(8) . ? C17 C18 1.535(7) . ? C17 C19 1.548(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.518(9) . ? C21 C22 1.526(9) . ? C21 C23 1.538(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.532(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.387(7) . ? C26 C31 1.405(7) . ? C27 C28 1.384(7) . ? C27 H27A 0.9500 . ? C28 C29 1.402(7) . ? C28 C32 1.549(8) . ? C29 C30 1.385(7) . ? C29 H29A 0.9500 . ? C30 C31 1.420(7) . ? C30 C36 1.543(7) . ? C32 C34 1.520(9) . ? C32 C35 1.529(9) . ? C32 C33 1.542(9) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 C39 1.518(8) . ? C36 C37 1.528(8) . ? C36 C38 1.537(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 1.515(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.391(7) . ? C41 C42 1.393(8) . ? C42 C43 1.404(8) . ? C43 C44 1.380(7) . ? C43 C47 1.562(8) . ? C44 C45 1.397(8) . ? C44 H44A 0.9500 . ? C45 C46 1.359(8) . ? C45 C51 1.549(8) . ? C46 H46A 0.9500 . ? C47 C50 1.519(8) . ? C47 C48 1.523(8) . ? C47 C49 1.529(8) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C53 1.481(10) . ? C51 C54 1.490(10) . ? C51 C52 1.525(11) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.417(8) . ? C55 C60 1.431(8) . ? C55 C61 1.522(8) . ? C56 C57 1.406(8) . ? C56 C64 1.499(8) . ? C57 C58 1.412(8) . ? C57 C62 1.497(9) . ? C58 C59 1.386(9) . ? C58 C79 1.513(8) . ? C59 C60 1.413(8) . ? C59 C63 1.537(8) . ? C60 C94 1.526(8) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.534(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C70 1.386(8) . ? C65 C66 1.412(8) . ? C66 C67 1.410(8) . ? C67 C68 1.400(8) . ? C67 C71 1.534(8) . ? C68 C69 1.375(8) . ? C68 H68A 0.9500 . ? C69 C70 1.404(8) . ? C69 C75 1.533(8) . ? C70 H70A 0.9500 . ? C71 C74 1.539(8) . ? C71 C73 1.541(8) . ? C71 C72 1.548(8) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C77 1.502(9) . ? C75 C78 1.530(9) . ? C75 C76 1.548(10) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.536(8) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.395(8) . ? C80 C85 1.401(8) . ? C81 C82 1.429(8) . ? C82 C83 1.392(8) . ? C82 C86 1.545(8) . ? C83 C84 1.403(8) . ? C83 H83A 0.9500 . ? C84 C85 1.385(8) . ? C84 C90 1.534(8) . ? C85 H85A 0.9500 . ? C86 C87 1.509(9) . ? C86 C88 1.543(8) . ? C86 C89 1.557(9) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 C91 1.519(10) . ? C90 C93 1.528(11) . ? C90 C92 1.555(10) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.519(8) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C100 1.392(9) . ? C95 C96 1.423(8) . ? C96 C97 1.397(8) . ? C97 C98 1.360(8) . ? C97 C101 1.552(8) . ? C98 C99 1.423(9) . ? C98 H98A 0.9500 . ? C99 C100 1.388(8) . ? C99 C105 1.511(10) . ? C100 H10C 0.9500 . ? C101 C102 1.522(8) . ? C101 C104 1.532(9) . ? C101 C103 1.542(8) . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C103 H10G 0.9800 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? C104 H10J 0.9800 . ? C104 H10K 0.9800 . ? C104 H10L 0.9800 . ? C105 C107 1.492(13) . ? C105 C106 1.514(11) . ? C105 C108 1.569(12) . ? C106 H10M 0.9800 . ? C106 H10N 0.9800 . ? C106 H10O 0.9800 . ? C107 H10P 0.9800 . ? C107 H10Q 0.9800 . ? C107 H10R 0.9800 . ? C108 H10S 0.9800 . ? C108 H10T 0.9800 . ? C108 H10U 0.9800 . ? C201 C206 1.330(17) . ? C201 C202 1.396(16) . ? C201 H201 0.9500 . ? C202 C203 1.401(18) . ? C202 H202 0.9500 . ? C203 C204 1.321(17) . ? C203 H203 0.9500 . ? C204 C205 1.363(16) . ? C204 H204 0.9500 . ? C205 C206 1.418(18) . ? C205 H205 0.9500 . ? C206 C207 1.466(15) . ? C207 H20D 0.9800 . ? C207 H20E 0.9800 . ? C207 H20F 0.9800 . ? C301 C302 1.52(3) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 O303 1.51(2) . ? C302 H30D 0.9900 . ? C302 H30E 0.9900 . ? O303 C304 1.45(2) . ? C304 C305 1.54(2) . ? C304 H30F 0.9900 . ? C304 H30G 0.9900 . ? C305 H30H 0.9800 . ? C305 H30I 0.9800 . ? C305 H30J 0.9800 . ? C401 C402 1.56(3) . ? C401 H40C 0.9800 . ? C401 H40D 0.9800 . ? C401 H40E 0.9800 . ? C402 O403 1.53(3) . ? C402 H40F 0.9900 . ? C402 H40G 0.9900 . ? O403 C404 1.51(3) . ? C404 C405 1.56(3) . ? C404 H40H 0.9900 . ? C404 H40I 0.9900 . ? C405 H40J 0.9800 . ? C405 H40K 0.9800 . ? C405 H40L 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 O1 U1 O3 171.93(14) . . ? O1 U1 O2 96.36(14) . . ? O3 U1 O2 91.60(13) . . ? O1 U1 O7 94.38(13) . . ? O3 U1 O7 83.25(13) . . ? O2 U1 O7 96.81(13) . . ? O1 U1 O8 77.46(13) . . ? O3 U1 O8 95.09(13) . . ? O2 U1 O8 147.07(12) . . ? O7 U1 O8 52.32(12) . . ? O1 U1 C109 88.27(15) . . ? O3 U1 C109 86.29(15) . . ? O2 U1 C109 122.35(15) . . ? O7 U1 C109 25.72(14) . . ? O8 U1 C109 26.86(14) . . ? O1 U1 C1 88.20(15) . . ? O3 U1 C1 88.38(15) . . ? O2 U1 C1 125.05(15) . . ? O7 U1 C1 137.55(14) . . ? O8 U1 C1 87.40(14) . . ? C109 U1 C1 112.48(15) . . ? O1 U1 C6 113.52(14) . . ? O3 U1 C6 64.95(14) . . ? O2 U1 C6 107.91(15) . . ? O7 U1 C6 139.53(15) . . ? O8 U1 C6 104.12(14) . . ? C109 U1 C6 122.47(16) . . ? C1 U1 C6 28.04(15) . . ? O1 U1 C2 64.53(15) . . ? O3 U1 C2 113.84(15) . . ? O2 U1 C2 110.59(14) . . ? O7 U1 C2 146.48(14) . . ? O8 U1 C2 96.02(13) . . ? C109 U1 C2 122.71(16) . . ? C1 U1 C2 27.87(15) . . ? C6 U1 C2 49.07(16) . . ? O1 U1 C4 91.10(15) . . ? O3 U1 C4 93.24(15) . . ? O2 U1 C4 67.46(14) . . ? O7 U1 C4 163.86(14) . . ? O8 U1 C4 143.83(13) . . ? C109 U1 C4 170.17(16) . . ? C1 U1 C4 57.70(15) . . ? C6 U1 C4 49.23(15) . . ? C2 U1 C4 48.80(15) . . ? O1 U1 C5 114.51(14) . . ? O3 U1 C5 68.15(14) . . ? O2 U1 C5 80.49(15) . . ? O7 U1 C5 151.10(14) . . ? O8 U1 C5 131.74(14) . . ? C109 U1 C5 146.95(16) . . ? C1 U1 C5 49.02(15) . . ? C6 U1 C5 27.62(16) . . ? C2 U1 C5 56.57(15) . . ? C4 U1 C5 27.53(15) . . ? O1 U1 C3 66.33(14) . . ? O3 U1 C3 116.24(14) . . ? O2 U1 C3 83.25(14) . . ? O7 U1 C3 160.51(14) . . ? O8 U1 C3 121.55(14) . . ? C109 U1 C3 146.72(16) . . ? C1 U1 C3 48.99(15) . . ? C6 U1 C3 57.01(16) . . ? C2 U1 C3 27.34(14) . . ? C4 U1 C3 27.51(15) . . ? C5 U1 C3 48.25(14) . . ? O5 U2 O6 95.72(14) . . ? O5 U2 O4 94.50(15) . . ? O6 U2 O4 169.77(14) . . ? O5 U2 O9 96.87(13) . . ? O6 U2 O9 82.27(14) . . ? O4 U2 O9 96.11(14) . . ? O5 U2 O8 147.67(13) . . ? O6 U2 O8 92.08(13) . . ? O4 U2 O8 79.00(13) . . ? O9 U2 O8 53.18(12) . . ? O5 U2 C109 122.90(15) . . ? O6 U2 C109 84.13(15) . . ? O4 U2 C109 89.98(15) . . ? O9 U2 C109 26.27(13) . . ? O8 U2 C109 27.15(13) . . ? O5 U2 C55 122.59(16) . . ? O6 U2 C55 88.84(16) . . ? O4 U2 C55 85.99(16) . . ? O9 U2 C55 140.27(15) . . ? O8 U2 C55 88.82(14) . . ? C109 U2 C55 114.50(16) . . ? O5 U2 C57 76.73(16) . . ? O6 U2 C57 113.11(16) . . ? O4 U2 C57 69.77(16) . . ? O9 U2 C57 163.63(16) . . ? O8 U2 C57 128.14(14) . . ? C109 U2 C57 153.73(16) . . ? C55 U2 C57 49.74(17) . . ? O5 U2 C56 104.27(16) . . ? O6 U2 C56 113.16(15) . . ? O4 U2 C56 64.42(15) . . ? O9 U2 C56 151.96(14) . . ? O8 U2 C56 101.29(14) . . ? C109 U2 C56 128.20(16) . . ? C55 U2 C56 28.09(17) . . ? C57 U2 C56 27.73(16) . . ? O5 U2 C60 109.35(15) . . ? O6 U2 C60 63.85(15) . . ? O4 U2 C60 112.86(15) . . ? O9 U2 C60 138.35(16) . . ? O8 U2 C60 102.27(14) . . ? C109 U2 C60 120.84(17) . . ? C55 U2 C60 28.34(16) . . ? C57 U2 C60 57.56(17) . . ? C56 U2 C60 49.31(17) . . ? O5 U2 C58 65.76(15) . . ? O6 U2 C58 88.49(17) . . ? O4 U2 C58 96.10(16) . . ? O9 U2 C58 159.49(13) . . ? O8 U2 C58 145.98(13) . . ? C109 U2 C58 169.10(17) . . ? C55 U2 C58 57.18(16) . . ? C57 U2 C58 27.48(16) . . ? C56 U2 C58 48.35(16) . . ? C60 U2 C58 48.35(17) . . ? C12 O1 U1 159.4(4) . . ? C31 O2 U1 140.3(3) . . ? C42 O3 U1 161.5(3) . . ? C66 O4 U2 154.8(4) . . ? C81 O5 U2 161.1(4) . . ? C96 O6 U2 161.6(3) . . ? C109 O7 U1 102.0(3) . . ? C109 O8 U2 87.3(3) . . ? C109 O8 U1 86.1(3) . . ? U2 O8 U1 173.30(16) . . ? C109 O9 U2 100.2(3) . . ? C6 C1 C2 119.6(5) . . ? C6 C1 C7 119.6(5) . . ? C2 C1 C7 120.8(5) . . ? C6 C1 U1 76.6(3) . . ? C2 C1 U1 78.0(3) . . ? C7 C1 U1 116.5(4) . . ? C3 C2 C1 120.8(6) . . ? C3 C2 C10 118.5(6) . . ? C1 C2 C10 120.6(5) . . ? C3 C2 U1 78.6(3) . . ? C1 C2 U1 74.1(3) . . ? C10 C2 U1 120.6(3) . . ? C2 C3 C4 119.2(6) . . ? C2 C3 C8 122.2(6) . . ? C4 C3 C8 118.6(5) . . ? C2 C3 U1 74.1(3) . . ? C4 C3 U1 74.1(3) . . ? C8 C3 U1 124.1(3) . . ? C3 C4 C5 120.1(5) . . ? C3 C4 C25 119.9(5) . . ? C5 C4 C25 120.0(6) . . ? C3 C4 U1 78.4(3) . . ? C5 C4 U1 78.3(3) . . ? C25 C4 U1 116.5(3) . . ? C6 C5 C4 119.2(5) . . ? C6 C5 C9 121.8(5) . . ? C4 C5 C9 119.0(5) . . ? C6 C5 U1 72.7(3) . . ? C4 C5 U1 74.2(3) . . ? C9 C5 U1 125.3(3) . . ? C1 C6 C5 120.4(5) . . ? C1 C6 C40 118.6(5) . . ? C5 C6 C40 121.0(5) . . ? C1 C6 U1 75.4(3) . . ? C5 C6 U1 79.7(3) . . ? C40 C6 U1 115.5(3) . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 120.2(5) . . ? C2 C10 H10A 107.3 . . ? C11 C10 H10A 107.3 . . ? C2 C10 H10B 107.3 . . ? C11 C10 H10B 107.3 . . ? H10A C10 H10B 106.9 . . ? C16 C11 C12 119.5(5) . . ? C16 C11 C10 115.7(5) . . ? C12 C11 C10 124.8(5) . . ? O1 C12 C11 120.1(5) . . ? O1 C12 C13 120.4(5) . . ? C11 C12 C13 119.5(5) . . ? C14 C13 C12 117.3(5) . . ? C14 C13 C17 120.4(5) . . ? C12 C13 C17 122.1(5) . . ? C15 C14 C13 124.1(5) . . ? C15 C14 H14A 117.9 . . ? C13 C14 H14A 117.9 . . ? C14 C15 C16 116.5(5) . . ? C14 C15 C21 124.1(5) . . ? C16 C15 C21 119.4(6) . . ? C11 C16 C15 122.8(6) . . ? C11 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? C13 C17 C20 111.8(5) . . ? C13 C17 C18 111.7(5) . . ? C20 C17 C18 106.9(4) . . ? C13 C17 C19 107.5(4) . . ? C20 C17 C19 111.3(5) . . ? C18 C17 C19 107.6(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C22 108.7(6) . . ? C24 C21 C15 108.7(6) . . ? C22 C21 C15 111.3(5) . . ? C24 C21 C23 109.9(6) . . ? C22 C21 C23 107.9(6) . . ? C15 C21 C23 110.4(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C4 C25 C26 117.5(4) . . ? C4 C25 H25A 107.9 . . ? C26 C25 H25A 107.9 . . ? C4 C25 H25B 107.9 . . ? C26 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? C27 C26 C31 120.4(5) . . ? C27 C26 C25 117.9(5) . . ? C31 C26 C25 121.4(5) . . ? C28 C27 C26 121.9(5) . . ? C28 C27 H27A 119.0 . . ? C26 C27 H27A 119.0 . . ? C27 C28 C29 116.5(5) . . ? C27 C28 C32 122.5(5) . . ? C29 C28 C32 121.0(5) . . ? C30 C29 C28 124.2(5) . . ? C30 C29 H29A 117.9 . . ? C28 C29 H29A 117.9 . . ? C29 C30 C31 117.5(5) . . ? C29 C30 C36 121.7(5) . . ? C31 C30 C36 120.4(5) . . ? O2 C31 C26 118.7(5) . . ? O2 C31 C30 122.4(4) . . ? C26 C31 C30 118.9(5) . . ? C34 C32 C35 109.7(6) . . ? C34 C32 C33 107.9(6) . . ? C35 C32 C33 108.0(5) . . ? C34 C32 C28 112.3(5) . . ? C35 C32 C28 110.5(5) . . ? C33 C32 C28 108.2(5) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C37 108.5(5) . . ? C39 C36 C38 107.4(5) . . ? C37 C36 C38 106.8(5) . . ? C39 C36 C30 114.4(5) . . ? C37 C36 C30 107.8(4) . . ? C38 C36 C30 111.6(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C6 119.6(5) . . ? C41 C40 H40A 107.4 . . ? C6 C40 H40A 107.4 . . ? C41 C40 H40B 107.4 . . ? C6 C40 H40B 107.4 . . ? H40A C40 H40B 106.9 . . ? C46 C41 C42 119.0(5) . . ? C46 C41 C40 118.6(5) . . ? C42 C41 C40 122.3(5) . . ? O3 C42 C41 118.0(5) . . ? O3 C42 C43 122.1(5) . . ? C41 C42 C43 119.8(5) . . ? C44 C43 C42 118.2(5) . . ? C44 C43 C47 119.9(5) . . ? C42 C43 C47 121.8(5) . . ? C43 C44 C45 122.8(5) . . ? C43 C44 H44A 118.6 . . ? C45 C44 H44A 118.6 . . ? C46 C45 C44 117.3(5) . . ? C46 C45 C51 121.7(5) . . ? C44 C45 C51 121.0(6) . . ? C45 C46 C41 122.6(5) . . ? C45 C46 H46A 118.7 . . ? C41 C46 H46A 118.7 . . ? C50 C47 C48 109.8(5) . . ? C50 C47 C49 107.7(5) . . ? C48 C47 C49 107.1(4) . . ? C50 C47 C43 108.9(4) . . ? C48 C47 C43 110.6(5) . . ? C49 C47 C43 112.6(5) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C53 C51 C54 109.3(8) . . ? C53 C51 C52 103.6(7) . . ? C54 C51 C52 109.4(7) . . ? C53 C51 C45 113.7(6) . . ? C54 C51 C45 109.9(6) . . ? C52 C51 C45 110.8(6) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 119.1(5) . . ? C56 C55 C61 121.3(5) . . ? C60 C55 C61 119.6(6) . . ? C56 C55 U2 77.6(3) . . ? C60 C55 U2 77.7(3) . . ? C61 C55 U2 115.2(4) . . ? C57 C56 C55 120.4(5) . . ? C57 C56 C64 118.6(6) . . ? C55 C56 C64 120.9(5) . . ? C57 C56 U2 75.7(3) . . ? C55 C56 U2 74.3(3) . . ? C64 C56 U2 123.8(4) . . ? C56 C57 C58 119.6(6) . . ? C56 C57 C62 120.3(6) . . ? C58 C57 C62 120.1(6) . . ? C56 C57 U2 76.6(3) . . ? C58 C57 U2 79.4(3) . . ? C62 C57 U2 115.3(4) . . ? C59 C58 C57 120.0(5) . . ? C59 C58 C79 121.2(6) . . ? C57 C58 C79 118.7(6) . . ? C59 C58 U2 79.5(3) . . ? C57 C58 U2 73.2(3) . . ? C79 C58 U2 121.5(4) . . ? C58 C59 C60 121.2(6) . . ? C58 C59 C63 118.9(5) . . ? C60 C59 C63 119.8(6) . . ? C59 C60 C55 118.7(6) . . ? C59 C60 C94 123.4(5) . . ? C55 C60 C94 117.9(5) . . ? C59 C60 U2 81.5(3) . . ? C55 C60 U2 73.9(3) . . ? C94 C60 U2 113.5(4) . . ? C55 C61 H61A 109.5 . . ? C55 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C55 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C59 C63 H63A 109.5 . . ? C59 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C59 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C56 C64 C65 121.1(5) . . ? C56 C64 H64A 107.0 . . ? C65 C64 H64A 107.0 . . ? C56 C64 H64B 107.0 . . ? C65 C64 H64B 107.0 . . ? H64A C64 H64B 106.8 . . ? C70 C65 C66 118.6(5) . . ? C70 C65 C64 115.2(5) . . ? C66 C65 C64 126.0(5) . . ? O4 C66 C67 120.9(5) . . ? O4 C66 C65 118.6(5) . . ? C67 C66 C65 120.5(5) . . ? C68 C67 C66 116.4(6) . . ? C68 C67 C71 121.4(5) . . ? C66 C67 C71 121.8(5) . . ? C69 C68 C67 125.7(6) . . ? C69 C68 H68A 117.1 . . ? C67 C68 H68A 117.1 . . ? C68 C69 C70 115.1(5) . . ? C68 C69 C75 125.5(6) . . ? C70 C69 C75 119.4(6) . . ? C65 C70 C69 123.4(6) . . ? C65 C70 H70A 118.3 . . ? C69 C70 H70A 118.3 . . ? C67 C71 C74 107.9(5) . . ? C67 C71 C73 113.4(5) . . ? C74 C71 C73 110.1(5) . . ? C67 C71 C72 112.1(5) . . ? C74 C71 C72 108.4(5) . . ? C73 C71 C72 104.8(5) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C77 C75 C78 108.1(6) . . ? C77 C75 C69 110.2(5) . . ? C78 C75 C69 111.7(6) . . ? C77 C75 C76 107.8(6) . . ? C78 C75 C76 108.4(6) . . ? C69 C75 C76 110.5(5) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C58 C79 C80 123.0(5) . . ? C58 C79 H79A 106.6 . . ? C80 C79 H79A 106.6 . . ? C58 C79 H79B 106.6 . . ? C80 C79 H79B 106.6 . . ? H79A C79 H79B 106.5 . . ? C81 C80 C85 120.0(5) . . ? C81 C80 C79 126.1(5) . . ? C85 C80 C79 113.8(5) . . ? O5 C81 C80 120.8(5) . . ? O5 C81 C82 120.0(5) . . ? C80 C81 C82 119.1(5) . . ? C83 C82 C81 117.8(6) . . ? C83 C82 C86 119.3(5) . . ? C81 C82 C86 122.9(5) . . ? C82 C83 C84 124.2(5) . . ? C82 C83 H83A 117.9 . . ? C84 C83 H83A 117.9 . . ? C85 C84 C83 116.0(5) . . ? C85 C84 C90 124.4(6) . . ? C83 C84 C90 119.6(5) . . ? C84 C85 C80 122.7(6) . . ? C84 C85 H85A 118.6 . . ? C80 C85 H85A 118.6 . . ? C87 C86 C88 108.5(6) . . ? C87 C86 C82 110.5(5) . . ? C88 C86 C82 111.9(5) . . ? C87 C86 C89 108.6(6) . . ? C88 C86 C89 106.6(5) . . ? C82 C86 C89 110.6(5) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C86 C89 H89A 109.5 . . ? C86 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C86 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C91 C90 C93 108.6(6) . . ? C91 C90 C84 111.8(5) . . ? C93 C90 C84 110.1(6) . . ? C91 C90 C92 108.0(6) . . ? C93 C90 C92 109.4(7) . . ? C84 C90 C92 108.9(6) . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C90 C93 H93A 109.5 . . ? C90 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C90 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C95 C94 C60 117.4(5) . . ? C95 C94 H94A 108.0 . . ? C60 C94 H94A 108.0 . . ? C95 C94 H94B 108.0 . . ? C60 C94 H94B 108.0 . . ? H94A C94 H94B 107.2 . . ? C100 C95 C96 119.2(5) . . ? C100 C95 C94 119.4(6) . . ? C96 C95 C94 121.4(6) . . ? O6 C96 C97 123.0(5) . . ? O6 C96 C95 117.4(5) . . ? C97 C96 C95 119.6(5) . . ? C98 C97 C96 118.1(6) . . ? C98 C97 C101 120.4(5) . . ? C96 C97 C101 121.2(5) . . ? C97 C98 C99 125.1(6) . . ? C97 C98 H98A 117.4 . . ? C99 C98 H98A 117.4 . . ? C100 C99 C98 114.8(6) . . ? C100 C99 C105 122.7(6) . . ? C98 C99 C105 122.3(6) . . ? C99 C100 C95 122.8(6) . . ? C99 C100 H10C 118.6 . . ? C95 C100 H10C 118.6 . . ? C102 C101 C104 107.6(5) . . ? C102 C101 C103 106.5(5) . . ? C104 C101 C103 112.5(5) . . ? C102 C101 C97 111.5(5) . . ? C104 C101 C97 108.5(5) . . ? C103 C101 C97 110.2(5) . . ? C101 C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C101 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? C101 C103 H10G 109.5 . . ? C101 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? C101 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C101 C104 H10J 109.5 . . ? C101 C104 H10K 109.5 . . ? H10J C104 H10K 109.5 . . ? C101 C104 H10L 109.5 . . ? H10J C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? C107 C105 C99 109.6(8) . . ? C107 C105 C106 110.0(8) . . ? C99 C105 C106 112.8(7) . . ? C107 C105 C108 110.4(8) . . ? C99 C105 C108 111.2(7) . . ? C106 C105 C108 102.7(8) . . ? C105 C106 H10M 109.5 . . ? C105 C106 H10N 109.5 . . ? H10M C106 H10N 109.5 . . ? C105 C106 H10O 109.5 . . ? H10M C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? C105 C107 H10P 109.5 . . ? C105 C107 H10Q 109.5 . . ? H10P C107 H10Q 109.5 . . ? C105 C107 H10R 109.5 . . ? H10P C107 H10R 109.5 . . ? H10Q C107 H10R 109.5 . . ? C105 C108 H10S 109.5 . . ? C105 C108 H10T 109.5 . . ? H10S C108 H10T 109.5 . . ? C105 C108 H10U 109.5 . . ? H10S C108 H10U 109.5 . . ? H10T C108 H10U 109.5 . . ? O7 C109 O9 123.3(5) . . ? O7 C109 O8 118.4(5) . . ? O9 C109 O8 118.2(6) . . ? O7 C109 U2 169.1(4) . . ? O9 C109 U2 53.5(3) . . ? O8 C109 U2 65.5(3) . . ? O7 C109 U1 52.3(3) . . ? O9 C109 U1 170.8(4) . . ? O8 C109 U1 67.0(3) . . ? U2 C109 U1 132.5(2) . . ? C206 C201 C202 125.2(16) . . ? C206 C201 H201 117.4 . . ? C202 C201 H201 117.4 . . ? C201 C202 C203 111.8(15) . . ? C201 C202 H202 124.1 . . ? C203 C202 H202 124.1 . . ? C204 C203 C202 125.2(17) . . ? C204 C203 H203 117.4 . . ? C202 C203 H203 117.4 . . ? C203 C204 C205 121.2(18) . . ? C203 C204 H204 119.4 . . ? C205 C204 H204 119.4 . . ? C204 C205 C206 116.8(16) . . ? C204 C205 H205 121.6 . . ? C206 C205 H205 121.6 . . ? C201 C206 C205 119.5(15) . . ? C201 C206 C207 122.9(16) . . ? C205 C206 C207 117.4(15) . . ? C206 C207 H20D 109.5 . . ? C206 C207 H20E 109.5 . . ? H20D C207 H20E 109.5 . . ? C206 C207 H20F 109.5 . . ? H20D C207 H20F 109.5 . . ? H20E C207 H20F 109.5 . . ? C302 C301 H30A 109.5 . . ? C302 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? O303 C302 C301 95(2) . . ? O303 C302 H30D 112.7 . . ? C301 C302 H30D 112.7 . . ? O303 C302 H30E 112.7 . . ? C301 C302 H30E 112.7 . . ? H30D C302 H30E 110.2 . . ? C304 O303 C302 103(2) . . ? O303 C304 C305 111(2) . . ? O303 C304 H30F 109.4 . . ? C305 C304 H30F 109.4 . . ? O303 C304 H30G 109.4 . . ? C305 C304 H30G 109.4 . . ? H30F C304 H30G 108.0 . . ? C304 C305 H30H 109.5 . . ? C304 C305 H30I 109.5 . . ? H30H C305 H30I 109.5 . . ? C304 C305 H30J 109.5 . . ? H30H C305 H30J 109.5 . . ? H30I C305 H30J 109.5 . . ? C402 C401 H40C 109.5 . . ? C402 C401 H40D 109.5 . . ? H40C C401 H40D 109.5 . . ? C402 C401 H40E 109.5 . . ? H40C C401 H40E 109.5 . . ? H40D C401 H40E 109.5 . . ? O403 C402 C401 88(2) . . ? O403 C402 H40F 114.0 . . ? C401 C402 H40F 114.0 . . ? O403 C402 H40G 114.0 . . ? C401 C402 H40G 114.0 . . ? H40F C402 H40G 111.2 . . ? C404 O403 C402 93(2) . . ? O403 C404 C405 97(2) . . ? O403 C404 H40H 112.3 . . ? C405 C404 H40H 112.3 . . ? O403 C404 H40I 112.3 . . ? C405 C404 H40I 112.3 . . ? H40H C404 H40I 109.9 . . ? C404 C405 H40J 109.5 . . ? C404 C405 H40K 109.5 . . ? H40J C405 H40K 109.5 . . ? C404 C405 H40L 109.5 . . ? H40J C405 H40L 109.5 . . ? H40K C405 H40L 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.339 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.131 data_opl0917 _database_code_depnum_ccdc_archive 'CCDC 759477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C117 H152 N2 O13 U2, 3(C4 H10 O2)' _chemical_formula_sum 'C129 H182 N2 O19 U2' _chemical_formula_weight 2540.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.680(3) _cell_length_b 24.539(4) _cell_length_c 25.430(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.041(9) _cell_angle_gamma 90.00 _cell_volume 12716(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 210 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5224 _exptl_absorpt_coefficient_mu 2.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.30 \% and 325 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 152032 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 26.37 _reflns_number_total 25808 _reflns_number_gt 17947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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 compound crystallizes with a total of three molecules of DME, one of which is disordered over two independent sites that are occupied by approximately 50 % each. SAME, SIMU and ISOR restraints were applied in the refinement of the solvent molecules. Further solvent accessible voids were detected in the structure. However, attempts to treat these by the SQUEEZE procedure did not produce physically meaningful results. The very large second parameter in the weighting scheme is due to the observed disorder and to electron density that could not be properly assigned due to missing and obviously highly disordered solvents that might be present in the voids discussed above. All remaining significant residual density peaks are located in close vicinity of the two U centres (in a distance between 0.8 to 1.65 \~A). ; _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^)+(0.0112P)^2^+187.4647P] 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 25808 _refine_ls_number_parameters 1439 _refine_ls_number_restraints 261 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _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 U1 U 0.258004(14) 0.622864(12) 0.231985(13) 0.01876(8) Uani 1 1 d . . . O1 O 0.2403(3) 0.6982(2) 0.1833(2) 0.0225(12) Uani 1 1 d . . . O2 O 0.2257(3) 0.6666(2) 0.2903(2) 0.0222(12) Uani 1 1 d . . . O3 O 0.2320(3) 0.5590(2) 0.1666(2) 0.0234(12) Uani 1 1 d . . . O4 O 0.3413(3) 0.6267(2) 0.1818(3) 0.0269(13) Uani 1 1 d . . . O5 O 0.3786(3) 0.6529(3) 0.2936(3) 0.0312(14) Uani 1 1 d . . . O6 O 0.2102(3) 0.5518(2) 0.2665(2) 0.0247(13) Uani 1 1 d . . . O7 O 0.3180(3) 0.5537(2) 0.3047(3) 0.0255(13) Uani 1 1 d . . . N1 N 0.1339(3) 0.6306(3) 0.1633(3) 0.0209(14) Uani 1 1 d . . . C1 C 0.1250(4) 0.6489(4) 0.1045(4) 0.0258(18) Uani 1 1 d . . . H1A H 0.0792 0.6412 0.0759 0.031 Uiso 1 1 calc R . . H1B H 0.1541 0.6268 0.0931 0.031 Uiso 1 1 calc R . . C2 C 0.1390(4) 0.7084(4) 0.0998(4) 0.0265(19) Uani 1 1 d . . . C3 C 0.1978(4) 0.7319(4) 0.1412(4) 0.0240(18) Uani 1 1 d . . . C4 C 0.2085(4) 0.7877(3) 0.1392(4) 0.0250(18) Uani 1 1 d . . . C5 C 0.1615(5) 0.8171(4) 0.0916(4) 0.032(2) Uani 1 1 d . . . H5A H 0.1691 0.8548 0.0887 0.039 Uiso 1 1 calc R . . C6 C 0.1048(5) 0.7942(4) 0.0486(4) 0.034(2) Uani 1 1 d . . . C7 C 0.0938(4) 0.7397(4) 0.0543(4) 0.032(2) Uani 1 1 d . . . H7A H 0.0546 0.7232 0.0265 0.038 Uiso 1 1 calc R . . C8 C 0.1048(4) 0.6709(3) 0.1893(4) 0.0249(18) Uani 1 1 d . . . H8A H 0.0578 0.6753 0.1619 0.030 Uiso 1 1 calc R . . H8B H 0.1264 0.7065 0.1918 0.030 Uiso 1 1 calc R . . C9 C 0.1095(4) 0.6578(3) 0.2484(4) 0.0223(17) Uani 1 1 d . . . C10 C 0.1707(4) 0.6608(3) 0.2993(4) 0.0232(17) Uani 1 1 d . . . C11 C 0.1716(4) 0.6593(3) 0.3549(4) 0.0243(18) Uani 1 1 d . . . C12 C 0.1119(4) 0.6488(4) 0.3574(4) 0.030(2) Uani 1 1 d . . . H12A H 0.1123 0.6468 0.3948 0.036 Uiso 1 1 calc R . . C13 C 0.0523(4) 0.6412(4) 0.3084(4) 0.0273(19) Uani 1 1 d . . . C14 C 0.0521(4) 0.6471(4) 0.2543(4) 0.030(2) Uani 1 1 d . . . H14A H 0.0117 0.6438 0.2201 0.036 Uiso 1 1 calc R . . C15 C 0.0992(4) 0.5778(4) 0.1558(4) 0.0255(18) Uani 1 1 d . . . H15A H 0.0517 0.5844 0.1321 0.031 Uiso 1 1 calc R . . H15B H 0.1053 0.5652 0.1948 0.031 Uiso 1 1 calc R . . C16 C 0.1199(4) 0.5319(3) 0.1271(4) 0.0217(17) Uani 1 1 d . . . C17 C 0.1849(4) 0.5221(3) 0.1363(4) 0.0218(17) Uani 1 1 d . . . C18 C 0.1999(4) 0.4735(4) 0.1151(4) 0.0260(19) Uani 1 1 d . . . C19 C 0.1488(4) 0.4382(4) 0.0826(4) 0.0269(19) Uani 1 1 d . . . H19A H 0.1587 0.4053 0.0686 0.032 Uiso 1 1 calc R . . C20 C 0.0839(4) 0.4491(4) 0.0699(4) 0.030(2) Uani 1 1 d . . . C21 C 0.0704(4) 0.4954(4) 0.0934(4) 0.029(2) Uani 1 1 d . . . H21A H 0.0265 0.5026 0.0865 0.035 Uiso 1 1 calc R . . C22 C 0.2651(4) 0.8171(3) 0.1906(4) 0.0281(19) Uani 1 1 d . . . C23 C 0.3231(6) 0.9071(4) 0.2298(5) 0.053(3) Uani 1 1 d . . . H23A H 0.3233 0.9469 0.2214 0.063 Uiso 1 1 calc R . . C24 C 0.3880(5) 0.8211(5) 0.2526(5) 0.052(3) Uani 1 1 d . . . H24A H 0.4308 0.8043 0.2592 0.063 Uiso 1 1 calc R . . C25 C 0.3121(7) 0.8383(5) 0.2982(5) 0.055(3) Uani 1 1 d . . . H25A H 0.3059 0.8336 0.3345 0.066 Uiso 1 1 calc R . . C26 C 0.2677(5) 0.8786(4) 0.1780(5) 0.040(2) Uani 1 1 d . . . H26A H 0.2748 0.8831 0.1425 0.048 Uiso 1 1 calc R . . H26B H 0.2253 0.8958 0.1705 0.048 Uiso 1 1 calc R . . C27 C 0.3890(6) 0.8814(5) 0.2398(6) 0.064(4) Uani 1 1 d . . . H27A H 0.3964 0.8863 0.2045 0.076 Uiso 1 1 calc R . . H27B H 0.4252 0.8995 0.2731 0.076 Uiso 1 1 calc R . . C28 C 0.3764(6) 0.8129(5) 0.3067(5) 0.061(4) Uani 1 1 d . . . H28A H 0.3758 0.7735 0.3145 0.073 Uiso 1 1 calc R . . H28B H 0.4128 0.8297 0.3410 0.073 Uiso 1 1 calc R . . C29 C 0.2561(5) 0.8104(4) 0.2466(4) 0.039(2) Uani 1 1 d . . . H29A H 0.2137 0.8266 0.2407 0.047 Uiso 1 1 calc R . . H29B H 0.2552 0.7711 0.2552 0.047 Uiso 1 1 calc R . . C30 C 0.3133(7) 0.8989(5) 0.2848(6) 0.063(4) Uani 1 1 d . . . H30A H 0.2714 0.9159 0.2793 0.075 Uiso 1 1 calc R . . H30B H 0.3493 0.9170 0.3183 0.075 Uiso 1 1 calc R . . C31 C 0.3322(4) 0.7935(4) 0.2003(4) 0.035(2) Uani 1 1 d . . . H31A H 0.3329 0.7538 0.2075 0.042 Uiso 1 1 calc R . . H31B H 0.3387 0.7992 0.1646 0.042 Uiso 1 1 calc R . . C32 C 0.0560(5) 0.8280(5) -0.0018(5) 0.050(3) Uani 1 1 d . . . H32A H 0.0290 0.8039 -0.0342 0.076 Uiso 1 1 calc R . . H32B H 0.0798 0.8536 -0.0151 0.076 Uiso 1 1 calc R . . H32C H 0.0277 0.8483 0.0113 0.076 Uiso 1 1 calc R . . C33 C 0.2333(4) 0.6713(4) 0.4124(4) 0.0228(18) Uani 1 1 d . . . C34 C 0.2782(5) 0.6882(5) 0.5222(4) 0.043(3) Uani 1 1 d . . . H34A H 0.2658 0.6902 0.5553 0.051 Uiso 1 1 calc R . . C35 C 0.3256(5) 0.7398(4) 0.4655(4) 0.039(2) Uani 1 1 d . . . H35A H 0.3447 0.7754 0.4616 0.046 Uiso 1 1 calc R . . C36 C 0.3476(4) 0.6395(4) 0.4829(4) 0.036(2) Uani 1 1 d . . . H36A H 0.3812 0.6103 0.4908 0.043 Uiso 1 1 calc R . . C37 C 0.2176(4) 0.6742(4) 0.4649(4) 0.034(2) Uani 1 1 d . . . H37A H 0.1997 0.6387 0.4694 0.041 Uiso 1 1 calc R . . H37B H 0.1834 0.7022 0.4574 0.041 Uiso 1 1 calc R . . C38 C 0.3068(5) 0.7432(5) 0.5152(5) 0.047(3) Uani 1 1 d . . . H38A H 0.2738 0.7723 0.5073 0.057 Uiso 1 1 calc R . . H38B H 0.3459 0.7523 0.5518 0.057 Uiso 1 1 calc R . . C39 C 0.3769(5) 0.6949(5) 0.4784(5) 0.041(2) Uani 1 1 d . . . H39A H 0.4158 0.7029 0.5156 0.049 Uiso 1 1 calc R . . H39B H 0.3911 0.6935 0.4468 0.049 Uiso 1 1 calc R . . C40 C 0.2874(4) 0.6269(4) 0.4258(4) 0.033(2) Uani 1 1 d . . . H40A H 0.2696 0.5908 0.4288 0.039 Uiso 1 1 calc R . . H40B H 0.3002 0.6254 0.3933 0.039 Uiso 1 1 calc R . . C41 C 0.3292(5) 0.6424(5) 0.5336(4) 0.042(3) Uani 1 1 d . . . H41A H 0.3688 0.6497 0.5704 0.051 Uiso 1 1 calc R . . H41B H 0.3105 0.6070 0.5377 0.051 Uiso 1 1 calc R . . C42 C 0.2638(5) 0.7271(4) 0.4071(4) 0.029(2) Uani 1 1 d . . . H42A H 0.2763 0.7255 0.3745 0.035 Uiso 1 1 calc R . . H42B H 0.2309 0.7565 0.3987 0.035 Uiso 1 1 calc R . . C43 C -0.0095(4) 0.6282(5) 0.3143(5) 0.045(3) Uani 1 1 d . . . H43A H -0.0478 0.6374 0.2777 0.067 Uiso 1 1 calc R . . H43B H -0.0104 0.6495 0.3465 0.067 Uiso 1 1 calc R . . H43C H -0.0104 0.5892 0.3224 0.067 Uiso 1 1 calc R . . C44 C 0.2713(4) 0.4582(4) 0.1283(4) 0.0267(14) Uani 1 1 d U . . C45 C 0.3465(4) 0.3876(4) 0.1147(4) 0.0350(16) Uani 1 1 d U . . H45A H 0.3461 0.3519 0.0956 0.042 Uiso 1 1 calc R . . C46 C 0.3852(4) 0.4380(4) 0.2100(4) 0.0327(16) Uani 1 1 d U . . H46A H 0.4114 0.4353 0.2534 0.039 Uiso 1 1 calc R . . C47 C 0.3740(4) 0.4864(4) 0.1193(4) 0.0341(16) Uani 1 1 d U . . H47A H 0.3932 0.5151 0.1035 0.041 Uiso 1 1 calc R . . C48 C 0.2744(4) 0.4058(3) 0.0999(4) 0.0271(16) Uani 1 1 d U . . H48A H 0.2494 0.4097 0.0569 0.033 Uiso 1 1 calc R . . H48B H 0.2531 0.3769 0.1127 0.033 Uiso 1 1 calc R . . C49 C 0.3869(4) 0.3829(4) 0.1816(4) 0.0355(17) Uani 1 1 d U . . H49A H 0.4329 0.3731 0.1911 0.043 Uiso 1 1 calc R . . H49B H 0.3683 0.3540 0.1970 0.043 Uiso 1 1 calc R . . C50 C 0.4144(4) 0.4830(4) 0.1859(4) 0.0353(17) Uani 1 1 d U . . H50A H 0.4132 0.5185 0.2040 0.042 Uiso 1 1 calc R . . H50B H 0.4606 0.4744 0.1956 0.042 Uiso 1 1 calc R . . C51 C 0.3024(4) 0.5018(4) 0.1047(4) 0.0306(16) Uani 1 1 d U . . H51A H 0.3016 0.5376 0.1224 0.037 Uiso 1 1 calc R . . H51B H 0.2766 0.5050 0.0618 0.037 Uiso 1 1 calc R . . C52 C 0.3760(5) 0.4315(4) 0.0915(4) 0.0371(17) Uani 1 1 d U . . H52A H 0.3509 0.4340 0.0484 0.045 Uiso 1 1 calc R . . H52B H 0.4219 0.4221 0.1008 0.045 Uiso 1 1 calc R . . C53 C 0.3140(4) 0.4528(4) 0.1955(4) 0.0280(16) Uani 1 1 d U . . H53A H 0.3133 0.4876 0.2148 0.034 Uiso 1 1 calc R . . H53B H 0.2952 0.4242 0.2111 0.034 Uiso 1 1 calc R . . C54 C 0.0295(5) 0.4098(5) 0.0320(5) 0.046(3) Uani 1 1 d . . . H54A H -0.0133 0.4257 0.0239 0.069 Uiso 1 1 calc R . . H54B H 0.0348 0.3752 0.0527 0.069 Uiso 1 1 calc R . . H54C H 0.0321 0.4035 -0.0050 0.069 Uiso 1 1 calc R . . C55 C 0.3167(6) 0.6451(4) 0.1228(4) 0.041(2) Uani 1 1 d . . . H55A H 0.3432 0.6296 0.1047 0.062 Uiso 1 1 calc R . . H55B H 0.3190 0.6850 0.1222 0.062 Uiso 1 1 calc R . . H55C H 0.2710 0.6334 0.1009 0.062 Uiso 1 1 calc R . . C56 C 0.4079(5) 0.6426(4) 0.2163(5) 0.041(3) Uani 1 1 d . . . H56A H 0.4126 0.6825 0.2134 0.049 Uiso 1 1 calc R . . H56B H 0.4370 0.6240 0.2021 0.049 Uiso 1 1 calc R . . C57 C 0.4259(5) 0.6272(5) 0.2771(5) 0.042(3) Uani 1 1 d . . . H57A H 0.4245 0.5871 0.2806 0.050 Uiso 1 1 calc R . . H57B H 0.4709 0.6399 0.3029 0.050 Uiso 1 1 calc R . . C58 C 0.4014(5) 0.6558(5) 0.3559(4) 0.046(3) Uani 1 1 d . . . H58A H 0.4414 0.6779 0.3732 0.069 Uiso 1 1 calc R . . H58B H 0.4109 0.6189 0.3725 0.069 Uiso 1 1 calc R . . H58C H 0.3674 0.6724 0.3647 0.069 Uiso 1 1 calc R . . C59 C 0.2650(4) 0.5307(4) 0.2995(4) 0.0257(19) Uani 1 1 d . . . U2 U 0.249252(14) 0.411508(12) 0.367409(14) 0.02056(8) Uani 1 1 d . . . O8 O 0.2675(3) 0.4847(3) 0.3261(3) 0.0353(15) Uani 1 1 d . . . O9 O 0.2667(3) 0.3430(2) 0.4257(3) 0.0238(13) Uani 1 1 d . . . O10 O 0.2627(3) 0.4613(3) 0.4422(3) 0.0292(14) Uani 1 1 d . . . O11 O 0.2870(3) 0.3623(2) 0.3186(3) 0.0257(13) Uani 1 1 d . . . O12 O 0.1463(3) 0.3834(3) 0.2722(3) 0.0346(15) Uani 1 1 d . . . O13 O 0.1339(3) 0.4597(3) 0.3399(3) 0.0392(17) Uani 1 1 d . . . N2 N 0.3741(3) 0.4159(3) 0.4270(3) 0.0230(15) Uani 1 1 d . . . C61 C 0.4020(4) 0.3726(4) 0.4725(4) 0.0289(19) Uani 1 1 d . . . H61A H 0.3951 0.3844 0.5066 0.035 Uiso 1 1 calc R . . H61B H 0.4500 0.3720 0.4853 0.035 Uiso 1 1 calc R . . C62 C 0.3778(5) 0.3149(4) 0.4587(4) 0.035(2) Uani 1 1 d . . . C63 C 0.3118(4) 0.3019(4) 0.4439(4) 0.0257(18) Uani 1 1 d . . . C64 C 0.2927(5) 0.2470(4) 0.4475(4) 0.032(2) Uani 1 1 d . . . C65 C 0.3405(5) 0.2070(5) 0.4581(7) 0.060(4) Uani 1 1 d . . . H65A H 0.3287 0.1700 0.4592 0.072 Uiso 1 1 calc R . . C66 C 0.4040(6) 0.2183(5) 0.4670(8) 0.073(5) Uani 1 1 d . . . C67 C 0.4220(5) 0.2725(5) 0.4690(6) 0.054(3) Uani 1 1 d . . . H67A H 0.4662 0.2809 0.4778 0.065 Uiso 1 1 calc R . . C68 C 0.3913(4) 0.4706(4) 0.4562(4) 0.031(2) Uani 1 1 d . . . H68A H 0.4392 0.4762 0.4710 0.037 Uiso 1 1 calc R . . H68B H 0.3690 0.4990 0.4263 0.037 Uiso 1 1 calc R . . C69 C 0.3736(4) 0.4790(4) 0.5058(4) 0.029(2) Uani 1 1 d . . . C70 C 0.3074(4) 0.4741(4) 0.4974(4) 0.0253(18) Uani 1 1 d . . . C71 C 0.2925(4) 0.4816(3) 0.5456(4) 0.0259(19) Uani 1 1 d . . . C72 C 0.3439(4) 0.4966(4) 0.5989(4) 0.030(2) Uani 1 1 d . . . H72A H 0.3343 0.5026 0.6313 0.036 Uiso 1 1 calc R . . C73 C 0.4088(4) 0.5032(4) 0.6076(4) 0.032(2) Uani 1 1 d . . . C74 C 0.4227(4) 0.4937(4) 0.5607(4) 0.034(2) Uani 1 1 d . . . H74A H 0.4667 0.4972 0.5659 0.041 Uiso 1 1 calc R . . C75 C 0.4048(4) 0.4146(4) 0.3854(4) 0.0282(19) Uani 1 1 d . . . H75A H 0.3828 0.4424 0.3548 0.034 Uiso 1 1 calc R . . H75B H 0.4513 0.4255 0.4072 0.034 Uiso 1 1 calc R . . C76 C 0.4025(4) 0.3620(4) 0.3560(4) 0.029(2) Uani 1 1 d . . . C77 C 0.3415(4) 0.3368(4) 0.3206(4) 0.0252(18) Uani 1 1 d . . . C78 C 0.3386(4) 0.2884(4) 0.2902(4) 0.029(2) Uani 1 1 d . . . C79 C 0.3988(5) 0.2657(5) 0.2977(4) 0.040(2) Uani 1 1 d . . . H79A H 0.3980 0.2327 0.2779 0.047 Uiso 1 1 calc R . . C80 C 0.4592(5) 0.2892(5) 0.3326(5) 0.043(3) Uani 1 1 d . . . C81 C 0.4600(4) 0.3374(4) 0.3612(4) 0.031(2) Uani 1 1 d . . . H81A H 0.5010 0.3541 0.3849 0.037 Uiso 1 1 calc R . . C82 C 0.2238(4) 0.2327(4) 0.4415(4) 0.0269(19) Uani 1 1 d . . . C83 C 0.1515(5) 0.1588(4) 0.4520(4) 0.033(2) Uani 1 1 d . . . H83A H 0.1501 0.1197 0.4626 0.040 Uiso 1 1 calc R . . C84 C 0.1020(5) 0.2283(4) 0.3729(4) 0.034(2) Uani 1 1 d . . . H84A H 0.0686 0.2349 0.3317 0.041 Uiso 1 1 calc R . . C85 C 0.1388(5) 0.2545(4) 0.4773(4) 0.032(2) Uani 1 1 d . . . H85A H 0.1291 0.2781 0.5046 0.039 Uiso 1 1 calc R . . C86 C 0.2201(4) 0.1718(4) 0.4564(4) 0.034(2) Uani 1 1 d . . . H86A H 0.2288 0.1483 0.4290 0.041 Uiso 1 1 calc R . . H86B H 0.2539 0.1640 0.4966 0.041 Uiso 1 1 calc R . . C87 C 0.1007(5) 0.1682(4) 0.3887(4) 0.037(2) Uani 1 1 d . . . H87A H 0.0564 0.1585 0.3844 0.044 Uiso 1 1 calc R . . H87B H 0.1108 0.1448 0.3620 0.044 Uiso 1 1 calc R . . C88 C 0.0881(4) 0.2652(4) 0.4146(4) 0.034(2) Uani 1 1 d . . . H88A H 0.0900 0.3038 0.4044 0.041 Uiso 1 1 calc R . . H88B H 0.0435 0.2577 0.4109 0.041 Uiso 1 1 calc R . . C89 C 0.2082(4) 0.2678(4) 0.4835(4) 0.029(2) Uani 1 1 d . . . H89A H 0.2106 0.3069 0.4747 0.035 Uiso 1 1 calc R . . H89B H 0.2411 0.2609 0.5243 0.035 Uiso 1 1 calc R . . C90 C 0.1363(5) 0.1948(4) 0.4929(4) 0.033(2) Uani 1 1 d . . . H90A H 0.1688 0.1881 0.5338 0.039 Uiso 1 1 calc R . . H90B H 0.0922 0.1859 0.4894 0.039 Uiso 1 1 calc R . . C91 C 0.1710(5) 0.2413(4) 0.3786(4) 0.032(2) Uani 1 1 d . . . H91A H 0.1805 0.2175 0.3518 0.039 Uiso 1 1 calc R . . H91B H 0.1723 0.2795 0.3669 0.039 Uiso 1 1 calc R . . C93 C 0.2216(4) 0.4752(3) 0.5379(4) 0.0253(18) Uani 1 1 d . . . C92 C 0.4523(8) 0.1733(7) 0.4753(9) 0.093(5) Uani 1 1 d U . . H92A H 0.4285 0.1396 0.4579 0.139 Uiso 1 1 calc R . . H92B H 0.4798 0.1676 0.5172 0.139 Uiso 1 1 calc R . . H92C H 0.4801 0.1833 0.4563 0.139 Uiso 1 1 calc R . . C94 C 0.1442(5) 0.4758(5) 0.5860(4) 0.039(2) Uani 1 1 d . . . H94A H 0.1420 0.4799 0.6242 0.047 Uiso 1 1 calc R . . C95 C 0.1068(4) 0.5142(4) 0.4870(5) 0.036(2) Uani 1 1 d . . . H95A H 0.0794 0.5432 0.4594 0.043 Uiso 1 1 calc R . . C96 C 0.1218(4) 0.4133(4) 0.5026(4) 0.034(2) Uani 1 1 d . . . H96A H 0.1040 0.3769 0.4853 0.040 Uiso 1 1 calc R . . C97 C 0.2164(4) 0.4811(4) 0.5965(4) 0.033(2) Uani 1 1 d . . . H97A H 0.2432 0.4526 0.6242 0.040 Uiso 1 1 calc R . . H97B H 0.2338 0.5171 0.6141 0.040 Uiso 1 1 calc R . . C98 C 0.1030(5) 0.5201(4) 0.5444(5) 0.039(2) Uani 1 1 d . . . H98A H 0.0568 0.5168 0.5381 0.047 Uiso 1 1 calc R . . H98B H 0.1195 0.5564 0.5615 0.047 Uiso 1 1 calc R . . C99 C 0.0814(4) 0.4582(4) 0.4603(4) 0.035(2) Uani 1 1 d . . . H99A H 0.0846 0.4546 0.4228 0.042 Uiso 1 1 calc R . . H99B H 0.0346 0.4545 0.4520 0.042 Uiso 1 1 calc R . . C100 C 0.1939(4) 0.4176(4) 0.5138(4) 0.030(2) Uani 1 1 d . . . H10A H 0.1974 0.4110 0.4769 0.036 Uiso 1 1 calc R . . H10B H 0.2201 0.3895 0.5424 0.036 Uiso 1 1 calc R . . C101 C 0.1173(5) 0.4197(4) 0.5603(5) 0.038(2) Uani 1 1 d . . . H10C H 0.1431 0.3908 0.5880 0.045 Uiso 1 1 calc R . . H10D H 0.0710 0.4164 0.5537 0.045 Uiso 1 1 calc R . . C102 C 0.1780(4) 0.5200(4) 0.4965(4) 0.032(2) Uani 1 1 d . . . H10E H 0.1950 0.5562 0.5135 0.039 Uiso 1 1 calc R . . H10F H 0.1798 0.5174 0.4584 0.039 Uiso 1 1 calc R . . C103 C 0.4616(4) 0.5201(4) 0.6662(4) 0.040(2) Uani 1 1 d . . . H10G H 0.5006 0.4974 0.6760 0.059 Uiso 1 1 calc R . . H10H H 0.4458 0.5155 0.6961 0.059 Uiso 1 1 calc R . . H10I H 0.4729 0.5584 0.6646 0.059 Uiso 1 1 calc R . . C104 C 0.2743(4) 0.2606(4) 0.2496(4) 0.030(2) Uani 1 1 d . . . C105 C 0.2210(5) 0.1820(5) 0.1799(5) 0.048(3) Uani 1 1 d . . . H10J H 0.2311 0.1484 0.1632 0.058 Uiso 1 1 calc R . . C106 C 0.1663(6) 0.2192(6) 0.2367(5) 0.055(4) Uani 1 1 d . . . H10K H 0.1389 0.2105 0.2576 0.066 Uiso 1 1 calc R . . C107 C 0.1810(6) 0.1669(5) 0.2112(5) 0.051(3) Uani 1 1 d . . . H10L H 0.2054 0.1407 0.2430 0.061 Uiso 1 1 calc R . . H10M H 0.1394 0.1495 0.1836 0.061 Uiso 1 1 calc R . . C108 C 0.2850(6) 0.2086(5) 0.2223(5) 0.057(3) Uani 1 1 d . . . H10N H 0.3116 0.2171 0.2013 0.068 Uiso 1 1 calc R . . H10O H 0.3100 0.1824 0.2539 0.068 Uiso 1 1 calc R . . C109 C 0.1692(6) 0.2729(6) 0.1555(6) 0.062(4) Uani 1 1 d . . . H10P H 0.1443 0.2990 0.1230 0.074 Uiso 1 1 calc R . . C110 C 0.1305(5) 0.2601(5) 0.1877(6) 0.064(4) Uani 1 1 d . . . H11A H 0.0875 0.2449 0.1603 0.077 Uiso 1 1 calc R . . H11B H 0.1223 0.2940 0.2046 0.077 Uiso 1 1 calc R . . C111 C 0.2353(6) 0.2985(5) 0.1978(5) 0.054(3) Uani 1 1 d . . . H11C H 0.2616 0.3063 0.1763 0.065 Uiso 1 1 calc R . . H11D H 0.2269 0.3335 0.2128 0.065 Uiso 1 1 calc R . . C112 C 0.1831(6) 0.2214(6) 0.1308(5) 0.057(3) Uani 1 1 d . . . H11E H 0.2090 0.2301 0.1091 0.068 Uiso 1 1 calc R . . H11F H 0.1413 0.2044 0.1032 0.068 Uiso 1 1 calc R . . C113 C 0.2331(5) 0.2442(5) 0.2804(5) 0.048(3) Uani 1 1 d . . . H11G H 0.2250 0.2766 0.2995 0.057 Uiso 1 1 calc R . . H11H H 0.2575 0.2172 0.3112 0.057 Uiso 1 1 calc R . . C114 C 0.5216(5) 0.2625(6) 0.3374(6) 0.074(5) Uani 1 1 d . . . H11I H 0.5525 0.2907 0.3379 0.111 Uiso 1 1 calc R . . H11J H 0.5113 0.2384 0.3038 0.111 Uiso 1 1 calc R . . H11K H 0.5414 0.2412 0.3736 0.111 Uiso 1 1 calc R . . C115 C 0.1378(6) 0.4129(5) 0.2210(4) 0.049(3) Uani 1 1 d . . . H11L H 0.0997 0.3985 0.1871 0.074 Uiso 1 1 calc R . . H11M H 0.1771 0.4088 0.2145 0.074 Uiso 1 1 calc R . . H11N H 0.1309 0.4515 0.2261 0.074 Uiso 1 1 calc R . . C116 C 0.0888(5) 0.3817(4) 0.2833(5) 0.042(3) Uani 1 1 d . . . H11O H 0.0969 0.3568 0.3164 0.051 Uiso 1 1 calc R . . H11P H 0.0509 0.3676 0.2483 0.051 Uiso 1 1 calc R . . C117 C 0.0735(4) 0.4371(5) 0.2974(5) 0.048(3) Uani 1 1 d . . . H11Q H 0.0552 0.4600 0.2618 0.058 Uiso 1 1 calc R . . H11R H 0.0410 0.4349 0.3136 0.058 Uiso 1 1 calc R . . C118 C 0.1289(5) 0.5176(4) 0.3419(5) 0.041(2) Uani 1 1 d . . . H11S H 0.0950 0.5270 0.3545 0.061 Uiso 1 1 calc R . . H11T H 0.1170 0.5328 0.3029 0.061 Uiso 1 1 calc R . . H11U H 0.1711 0.5327 0.3697 0.061 Uiso 1 1 calc R . . C201 C -0.0572(8) 0.3592(9) 0.3335(8) 0.115(6) Uani 1 1 d DU . . H20A H -0.0786 0.3950 0.3249 0.173 Uiso 1 1 calc R . . H20B H -0.0166 0.3613 0.3699 0.173 Uiso 1 1 calc R . . H20C H -0.0867 0.3323 0.3378 0.173 Uiso 1 1 calc R . . O202 O -0.0426(7) 0.3436(7) 0.2878(6) 0.129(4) Uani 1 1 d DU . . C203 C -0.0827(10) 0.3109(9) 0.2484(9) 0.116(4) Uani 1 1 d DU . . H20D H -0.1266 0.3282 0.2323 0.139 Uiso 1 1 calc R . . H20E H -0.0855 0.2775 0.2689 0.139 Uiso 1 1 calc R . . C204 C -0.0715(11) 0.2942(8) 0.2002(9) 0.117(5) Uani 1 1 d DU . . H20F H -0.0351 0.2675 0.2146 0.140 Uiso 1 1 calc R . . H20G H -0.1112 0.2748 0.1722 0.140 Uiso 1 1 calc R . . O205 O -0.0571(7) 0.3329(6) 0.1706(6) 0.113(4) Uani 1 1 d DU . . C206 C -0.0578(12) 0.3170(9) 0.1174(9) 0.131(7) Uani 1 1 d DU . . H20H H -0.0156 0.3259 0.1178 0.197 Uiso 1 1 calc R . . H20I H -0.0930 0.3363 0.0852 0.197 Uiso 1 1 calc R . . H20J H -0.0654 0.2776 0.1122 0.197 Uiso 1 1 calc R . . C207 C 0.4517(10) 0.2595(9) 0.1152(10) 0.140(8) Uani 1 1 d U . . H20K H 0.4160 0.2667 0.0764 0.211 Uiso 1 1 calc R . . H20L H 0.4940 0.2654 0.1142 0.211 Uiso 1 1 calc R . . H20M H 0.4479 0.2843 0.1438 0.211 Uiso 1 1 calc R . . O208 O 0.4478(5) 0.2040(6) 0.1316(6) 0.102(4) Uani 1 1 d U . . C209 C 0.3857(7) 0.1970(8) 0.1222(9) 0.105(4) Uani 1 1 d U . . H20N H 0.3566 0.1950 0.0797 0.126 Uiso 1 1 calc R . . H20O H 0.3712 0.2276 0.1390 0.126 Uiso 1 1 calc R . . C210 C 0.3835(8) 0.1402(8) 0.1539(9) 0.106(4) Uani 1 1 d U . . H21B H 0.3377 0.1303 0.1448 0.127 Uiso 1 1 calc R . . H21C H 0.4032 0.1103 0.1407 0.127 Uiso 1 1 calc R . . O211 O 0.4197(6) 0.1496(6) 0.2135(7) 0.116(4) Uani 1 1 d U . . C212 C 0.4161(11) 0.0997(8) 0.2438(11) 0.125(7) Uani 1 1 d U . . H21D H 0.3704 0.0875 0.2281 0.188 Uiso 1 1 calc R . . H21E H 0.4328 0.1071 0.2858 0.188 Uiso 1 1 calc R . . H21F H 0.4428 0.0712 0.2377 0.188 Uiso 1 1 calc R . . C213 C -0.1220(19) 0.4990(18) 0.2596(16) 0.120(10) Uani 0.50 1 d PDU . . H21G H -0.1621 0.5186 0.2341 0.180 Uiso 0.50 1 calc PR . . H21H H -0.1019 0.5167 0.2981 0.180 Uiso 0.50 1 calc PR . . H21I H -0.1330 0.4612 0.2641 0.180 Uiso 0.50 1 calc PR . . O214 O -0.0785(13) 0.4996(12) 0.2351(12) 0.120(7) Uani 0.50 1 d PDU . . C215 C -0.1031(18) 0.509(2) 0.1818(14) 0.134(7) Uani 0.50 1 d PDU . . H21J H -0.1200 0.5473 0.1762 0.160 Uiso 0.50 1 calc PR . . H21K H -0.1415 0.4852 0.1624 0.160 Uiso 0.50 1 calc PR . . C216 C -0.0642(18) 0.5044(19) 0.1516(14) 0.137(8) Uani 0.50 1 d PDU . . H21L H -0.0243 0.5268 0.1722 0.165 Uiso 0.50 1 calc PR . . H21M H -0.0498 0.4659 0.1545 0.165 Uiso 0.50 1 calc PR . . O217 O -0.0913(16) 0.5184(13) 0.0952(13) 0.152(8) Uani 0.50 1 d PDU . . C218 C -0.1245(17) 0.4798(16) 0.0509(15) 0.109(9) Uani 0.50 1 d PDU . . H21N H -0.1608 0.4640 0.0569 0.164 Uiso 0.50 1 calc PR . . H21O H -0.0939 0.4509 0.0526 0.164 Uiso 0.50 1 calc PR . . H21P H -0.1418 0.4977 0.0126 0.164 Uiso 0.50 1 calc PR . . C219 C 0.273(2) 0.6135(13) -0.0566(19) 0.140(11) Uani 0.50 1 d PDU . . H21Q H 0.3202 0.6180 -0.0317 0.210 Uiso 0.50 1 calc PR . . H21R H 0.2492 0.6167 -0.0326 0.210 Uiso 0.50 1 calc PR . . H21S H 0.2580 0.6418 -0.0868 0.210 Uiso 0.50 1 calc PR . . O220 O 0.2617(16) 0.5638(11) -0.0823(13) 0.138(7) Uani 0.50 1 d PDU . . C221 C 0.3108(18) 0.5316(13) -0.0594(15) 0.121(7) Uani 0.50 1 d PDU . . H22A H 0.3248 0.5298 -0.0167 0.145 Uiso 0.50 1 calc PR . . H22B H 0.3478 0.5470 -0.0655 0.145 Uiso 0.50 1 calc PR . . C222 C 0.298(2) 0.4772(12) -0.0829(14) 0.119(7) Uani 0.50 1 d PDU . . H22C H 0.3345 0.4531 -0.0582 0.143 Uiso 0.50 1 calc PR . . H22D H 0.2574 0.4634 -0.0816 0.143 Uiso 0.50 1 calc PR . . O223 O 0.2903(15) 0.4752(10) -0.1381(11) 0.122(7) Uani 0.50 1 d PDU . . C224 C 0.291(2) 0.4221(13) -0.1579(17) 0.125(11) Uani 0.50 1 d PDU . . H22E H 0.3101 0.3973 -0.1243 0.188 Uiso 0.50 1 calc PR . . H22F H 0.3184 0.4213 -0.1792 0.188 Uiso 0.50 1 calc PR . . H22G H 0.2466 0.4107 -0.1840 0.188 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01536(14) 0.01917(15) 0.02002(15) 0.00104(12) 0.00618(11) -0.00155(11) O1 0.018(3) 0.020(3) 0.025(3) 0.003(2) 0.006(2) -0.003(2) O2 0.021(3) 0.021(3) 0.025(3) 0.000(2) 0.010(2) -0.004(2) O3 0.016(3) 0.028(3) 0.024(3) -0.004(2) 0.006(2) -0.004(2) O4 0.027(3) 0.023(3) 0.036(3) -0.001(3) 0.018(3) -0.006(2) O5 0.023(3) 0.042(4) 0.028(3) -0.008(3) 0.012(3) -0.006(3) O6 0.017(3) 0.032(3) 0.019(3) 0.005(2) 0.003(2) 0.002(2) O7 0.020(3) 0.030(3) 0.027(3) 0.005(3) 0.010(3) -0.002(2) N1 0.017(3) 0.020(4) 0.024(3) -0.004(3) 0.007(3) -0.002(3) C1 0.022(4) 0.031(5) 0.022(4) -0.001(4) 0.007(4) -0.001(4) C2 0.025(4) 0.032(5) 0.025(4) 0.003(4) 0.013(4) 0.001(4) C3 0.027(4) 0.031(5) 0.019(4) 0.007(3) 0.015(4) 0.005(4) C4 0.028(4) 0.024(5) 0.025(4) 0.002(3) 0.014(4) -0.002(4) C5 0.036(5) 0.020(5) 0.041(5) 0.008(4) 0.018(4) 0.007(4) C6 0.031(5) 0.034(5) 0.035(5) 0.007(4) 0.012(4) 0.005(4) C7 0.028(5) 0.035(5) 0.022(4) 0.002(4) 0.002(4) 0.003(4) C8 0.016(4) 0.022(4) 0.030(5) 0.002(3) 0.003(4) 0.001(3) C9 0.020(4) 0.020(4) 0.025(4) -0.002(3) 0.008(3) 0.005(3) C10 0.022(4) 0.020(4) 0.026(4) 0.001(3) 0.009(4) -0.002(3) C11 0.021(4) 0.021(4) 0.026(4) 0.000(3) 0.005(4) 0.006(3) C12 0.024(4) 0.041(6) 0.031(5) 0.005(4) 0.017(4) 0.008(4) C13 0.019(4) 0.027(5) 0.035(5) -0.001(4) 0.011(4) 0.003(3) C14 0.022(4) 0.029(5) 0.034(5) -0.002(4) 0.008(4) 0.002(4) C15 0.014(4) 0.029(5) 0.031(5) -0.002(4) 0.008(4) 0.001(3) C16 0.021(4) 0.021(4) 0.023(4) -0.002(3) 0.010(3) -0.001(3) C17 0.027(4) 0.017(4) 0.024(4) -0.001(3) 0.013(4) -0.001(3) C18 0.021(4) 0.029(5) 0.026(4) 0.006(4) 0.008(4) 0.004(3) C19 0.029(5) 0.024(5) 0.029(5) -0.007(4) 0.013(4) -0.001(4) C20 0.023(4) 0.029(5) 0.035(5) -0.003(4) 0.009(4) -0.003(4) C21 0.022(4) 0.029(5) 0.031(5) -0.005(4) 0.006(4) -0.001(4) C22 0.032(5) 0.018(4) 0.032(5) -0.003(4) 0.011(4) -0.007(4) C23 0.059(7) 0.024(5) 0.066(8) 0.001(5) 0.019(6) -0.012(5) C24 0.033(6) 0.050(7) 0.061(8) -0.002(6) 0.009(5) -0.010(5) C25 0.078(9) 0.048(7) 0.038(6) -0.008(5) 0.023(6) -0.017(6) C26 0.037(5) 0.030(5) 0.045(6) 0.004(5) 0.009(5) -0.002(4) C27 0.057(8) 0.055(8) 0.062(8) -0.003(6) 0.011(7) -0.026(6) C28 0.066(8) 0.039(7) 0.044(7) -0.004(5) -0.007(6) -0.015(6) C29 0.043(6) 0.037(6) 0.035(5) 0.002(4) 0.016(5) -0.007(5) C30 0.079(9) 0.037(7) 0.056(8) -0.018(6) 0.015(7) -0.014(6) C31 0.030(5) 0.032(5) 0.039(5) -0.001(4) 0.010(4) -0.009(4) C32 0.042(6) 0.046(7) 0.046(6) 0.019(5) 0.003(5) 0.005(5) C33 0.017(4) 0.032(5) 0.026(4) -0.007(4) 0.015(4) 0.001(3) C34 0.030(5) 0.075(8) 0.022(5) -0.005(5) 0.010(4) 0.002(5) C35 0.037(5) 0.034(6) 0.033(5) -0.008(4) 0.005(4) -0.012(4) C36 0.020(4) 0.047(6) 0.034(5) -0.004(4) 0.005(4) 0.006(4) C37 0.018(4) 0.053(6) 0.026(5) -0.009(4) 0.005(4) -0.003(4) C38 0.042(6) 0.058(7) 0.034(6) -0.024(5) 0.009(5) 0.000(5) C39 0.027(5) 0.056(7) 0.036(5) -0.012(5) 0.011(4) -0.009(5) C40 0.020(4) 0.039(5) 0.041(5) -0.009(4) 0.015(4) -0.012(4) C41 0.028(5) 0.056(7) 0.029(5) 0.001(5) 0.000(4) -0.005(5) C42 0.039(5) 0.029(5) 0.021(4) -0.006(4) 0.016(4) -0.007(4) C43 0.020(5) 0.072(8) 0.047(6) -0.002(6) 0.018(5) 0.000(5) C44 0.021(3) 0.030(3) 0.028(3) -0.005(3) 0.010(2) 0.001(2) C45 0.026(3) 0.036(3) 0.037(3) -0.010(3) 0.009(3) 0.003(3) C46 0.022(3) 0.038(3) 0.034(3) -0.006(3) 0.008(3) 0.001(3) C47 0.027(3) 0.041(3) 0.035(3) -0.004(3) 0.014(3) -0.002(3) C48 0.022(3) 0.017(3) 0.033(3) -0.014(3) 0.004(3) -0.004(3) C49 0.024(3) 0.039(3) 0.038(3) -0.005(3) 0.008(3) 0.004(3) C50 0.025(3) 0.041(4) 0.037(3) -0.008(3) 0.010(3) -0.003(3) C51 0.026(3) 0.036(3) 0.029(3) -0.003(3) 0.011(3) -0.001(3) C52 0.028(3) 0.044(4) 0.039(3) -0.006(3) 0.015(3) 0.003(3) C53 0.021(3) 0.032(3) 0.027(3) -0.006(3) 0.008(3) 0.001(3) C54 0.025(5) 0.042(6) 0.060(7) -0.020(5) 0.009(5) -0.004(4) C55 0.055(7) 0.040(6) 0.036(5) 0.004(4) 0.027(5) -0.004(5) C56 0.027(5) 0.046(6) 0.060(7) -0.016(5) 0.028(5) -0.013(4) C57 0.022(5) 0.048(6) 0.051(6) -0.016(5) 0.012(5) -0.006(4) C58 0.032(5) 0.075(8) 0.032(5) -0.009(5) 0.014(5) -0.022(5) C59 0.023(4) 0.028(5) 0.027(5) -0.006(4) 0.012(4) -0.004(4) U2 0.01457(14) 0.02013(15) 0.02430(16) 0.00268(12) 0.00608(12) -0.00103(12) O8 0.033(3) 0.023(3) 0.048(4) 0.011(3) 0.016(3) 0.000(3) O9 0.013(3) 0.024(3) 0.030(3) 0.011(2) 0.005(2) 0.003(2) O10 0.016(3) 0.032(3) 0.030(3) 0.004(3) 0.001(3) 0.001(2) O11 0.016(3) 0.030(3) 0.029(3) -0.008(3) 0.007(2) -0.005(2) O12 0.019(3) 0.050(4) 0.029(3) 0.000(3) 0.006(3) 0.004(3) O13 0.022(3) 0.043(4) 0.044(4) -0.006(3) 0.007(3) 0.003(3) N2 0.015(3) 0.026(4) 0.025(4) -0.002(3) 0.007(3) -0.003(3) C61 0.015(4) 0.036(5) 0.031(5) 0.004(4) 0.005(4) 0.004(4) C62 0.026(5) 0.034(5) 0.041(6) 0.010(4) 0.012(4) 0.005(4) C63 0.020(4) 0.029(5) 0.025(4) 0.005(4) 0.006(4) -0.002(3) C64 0.031(5) 0.029(5) 0.040(5) 0.001(4) 0.019(4) 0.005(4) C65 0.039(6) 0.033(6) 0.111(11) 0.016(7) 0.034(7) 0.006(5) C66 0.037(6) 0.037(7) 0.152(15) 0.029(8) 0.050(8) 0.015(5) C67 0.026(5) 0.046(7) 0.094(10) 0.021(6) 0.029(6) 0.008(5) C68 0.019(4) 0.036(5) 0.037(5) -0.002(4) 0.011(4) -0.007(4) C69 0.022(4) 0.028(5) 0.038(5) -0.006(4) 0.013(4) -0.005(4) C70 0.019(4) 0.028(5) 0.027(4) -0.005(4) 0.009(4) -0.003(3) C71 0.019(4) 0.023(4) 0.029(5) -0.003(4) 0.003(4) 0.003(3) C72 0.023(4) 0.035(5) 0.030(5) -0.007(4) 0.010(4) -0.003(4) C73 0.020(4) 0.034(5) 0.035(5) -0.002(4) 0.006(4) -0.003(4) C74 0.019(4) 0.038(6) 0.040(5) -0.010(4) 0.009(4) -0.007(4) C75 0.017(4) 0.028(5) 0.039(5) 0.005(4) 0.011(4) -0.006(3) C76 0.023(4) 0.036(5) 0.026(5) 0.003(4) 0.010(4) -0.002(4) C77 0.018(4) 0.032(5) 0.030(5) 0.001(4) 0.015(4) 0.001(3) C78 0.021(4) 0.038(5) 0.028(5) -0.007(4) 0.011(4) -0.008(4) C79 0.026(5) 0.050(6) 0.039(6) -0.012(5) 0.011(4) 0.004(4) C80 0.022(5) 0.060(7) 0.046(6) -0.014(5) 0.014(5) 0.002(5) C81 0.015(4) 0.041(6) 0.034(5) -0.008(4) 0.009(4) -0.005(4) C82 0.024(4) 0.032(5) 0.030(5) 0.006(4) 0.016(4) 0.000(4) C83 0.035(5) 0.029(5) 0.036(5) 0.009(4) 0.015(4) -0.010(4) C84 0.029(5) 0.048(6) 0.025(5) 0.005(4) 0.011(4) -0.004(4) C85 0.038(5) 0.038(5) 0.025(5) -0.001(4) 0.017(4) -0.001(4) C86 0.028(5) 0.035(5) 0.027(5) 0.006(4) 0.002(4) -0.003(4) C87 0.034(5) 0.044(6) 0.030(5) -0.005(4) 0.012(4) -0.008(4) C88 0.020(4) 0.038(6) 0.043(6) 0.011(4) 0.013(4) -0.001(4) C89 0.025(4) 0.029(5) 0.029(5) 0.004(4) 0.009(4) -0.005(4) C90 0.030(5) 0.040(6) 0.030(5) 0.003(4) 0.016(4) -0.005(4) C91 0.037(5) 0.029(5) 0.032(5) 0.006(4) 0.017(4) 0.001(4) C93 0.018(4) 0.023(4) 0.032(5) -0.005(4) 0.008(4) -0.001(3) C92 0.065(7) 0.079(8) 0.135(10) 0.006(7) 0.044(7) 0.015(6) C94 0.032(5) 0.056(7) 0.034(5) -0.012(5) 0.018(4) -0.002(5) C95 0.026(5) 0.031(5) 0.047(6) 0.013(4) 0.014(4) 0.011(4) C96 0.028(5) 0.030(5) 0.045(6) -0.009(4) 0.018(4) -0.012(4) C97 0.025(5) 0.043(6) 0.033(5) -0.006(4) 0.014(4) -0.003(4) C98 0.024(5) 0.040(6) 0.052(6) -0.011(5) 0.017(5) -0.001(4) C99 0.017(4) 0.047(6) 0.038(5) -0.001(4) 0.010(4) 0.002(4) C100 0.017(4) 0.029(5) 0.042(5) 0.000(4) 0.012(4) 0.001(4) C101 0.025(5) 0.042(6) 0.048(6) 0.004(5) 0.017(5) 0.001(4) C102 0.024(4) 0.027(5) 0.040(5) 0.003(4) 0.009(4) 0.006(4) C103 0.023(5) 0.047(6) 0.038(6) -0.007(5) 0.002(4) -0.002(4) C104 0.024(4) 0.040(5) 0.025(5) -0.010(4) 0.010(4) -0.005(4) C105 0.034(5) 0.056(7) 0.056(7) -0.036(6) 0.021(5) -0.006(5) C106 0.055(7) 0.086(9) 0.042(6) -0.035(6) 0.037(6) -0.046(7) C107 0.051(7) 0.045(7) 0.044(6) 0.001(5) 0.009(5) -0.015(5) C108 0.052(7) 0.056(8) 0.046(7) -0.035(6) 0.007(6) -0.001(6) C109 0.041(7) 0.062(8) 0.052(7) 0.014(6) -0.008(6) -0.009(6) C110 0.025(5) 0.060(8) 0.084(10) -0.036(7) 0.003(6) 0.001(5) C111 0.048(7) 0.051(7) 0.045(7) 0.005(5) 0.005(6) -0.016(6) C112 0.050(7) 0.089(10) 0.031(6) -0.009(6) 0.017(5) -0.028(7) C113 0.044(6) 0.062(8) 0.039(6) -0.017(5) 0.020(5) -0.022(5) C114 0.027(6) 0.097(11) 0.086(10) -0.051(9) 0.013(6) 0.002(6) C115 0.046(6) 0.062(8) 0.028(5) -0.002(5) 0.006(5) 0.006(6) C116 0.023(5) 0.045(6) 0.052(6) -0.004(5) 0.010(5) -0.009(4) C117 0.015(4) 0.073(8) 0.053(7) -0.006(6) 0.011(5) -0.004(5) C118 0.037(5) 0.040(6) 0.045(6) 0.015(5) 0.018(5) 0.007(5) C201 0.071(9) 0.187(16) 0.111(12) -0.016(12) 0.061(9) -0.035(10) O202 0.114(8) 0.164(10) 0.120(9) -0.021(8) 0.060(7) -0.075(7) C203 0.111(8) 0.126(9) 0.127(9) -0.025(8) 0.067(7) -0.060(7) C204 0.124(8) 0.107(9) 0.119(9) -0.025(8) 0.053(8) -0.055(7) O205 0.120(8) 0.112(8) 0.116(8) -0.033(7) 0.059(7) -0.046(7) C206 0.144(14) 0.132(15) 0.111(13) -0.029(12) 0.051(12) -0.007(12) C207 0.101(12) 0.121(14) 0.145(15) -0.012(13) 0.005(12) 0.049(12) O208 0.049(5) 0.115(8) 0.120(8) -0.009(7) 0.018(5) 0.029(6) C209 0.049(6) 0.125(8) 0.126(8) -0.029(8) 0.025(6) 0.022(7) C210 0.049(6) 0.117(8) 0.135(9) -0.048(8) 0.026(6) 0.008(7) O211 0.066(6) 0.124(8) 0.147(9) -0.034(8) 0.037(6) 0.003(6) C212 0.115(12) 0.089(12) 0.178(16) -0.014(12) 0.070(12) -0.020(11) C213 0.118(15) 0.118(15) 0.129(15) 0.004(13) 0.058(12) -0.015(13) O214 0.123(9) 0.121(9) 0.123(9) -0.003(7) 0.059(7) -0.006(7) C215 0.132(9) 0.133(9) 0.134(9) 0.002(7) 0.057(7) -0.002(7) C216 0.136(9) 0.139(9) 0.139(9) 0.004(7) 0.061(7) 0.004(7) O217 0.145(10) 0.150(10) 0.152(10) 0.005(7) 0.057(7) 0.009(7) C218 0.091(13) 0.143(16) 0.125(15) 0.003(13) 0.075(12) -0.001(12) C219 0.21(2) 0.10(2) 0.14(2) -0.061(17) 0.099(19) -0.014(19) O220 0.188(18) 0.117(15) 0.126(15) -0.023(12) 0.085(15) -0.007(14) C221 0.171(17) 0.109(14) 0.114(14) -0.013(12) 0.090(14) -0.006(13) C222 0.163(17) 0.103(14) 0.115(14) -0.011(12) 0.081(14) -0.017(13) O223 0.163(16) 0.101(13) 0.118(14) -0.016(12) 0.075(14) -0.022(13) C224 0.16(2) 0.100(19) 0.12(2) -0.022(17) 0.071(19) -0.022(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.163(5) . ? U1 O3 2.170(6) . ? U1 O2 2.200(6) . ? U1 O6 2.414(6) . ? U1 O7 2.439(6) . ? U1 N1 2.586(6) . ? U1 O5 2.592(6) . ? U1 O4 2.706(6) . ? U1 C59 2.801(9) . ? O1 C3 1.361(10) . ? O2 C10 1.371(10) . ? O3 C17 1.353(10) . ? O4 C55 1.424(11) . ? O4 C56 1.430(11) . ? O5 C58 1.438(11) . ? O5 C57 1.455(11) . ? O6 C59 1.263(10) . ? O7 C59 1.281(10) . ? N1 C15 1.483(11) . ? N1 C1 1.489(11) . ? N1 C8 1.494(11) . ? C1 C2 1.509(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.392(12) . ? C2 C3 1.411(12) . ? C3 C4 1.394(12) . ? C4 C5 1.412(12) . ? C4 C22 1.550(12) . ? C5 C6 1.389(13) . ? C5 H5A 0.9500 . ? C6 C7 1.380(13) . ? C6 C32 1.521(13) . ? C7 H7A 0.9500 . ? C8 C9 1.495(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.399(12) . ? C9 C10 1.424(11) . ? C10 C11 1.406(12) . ? C11 C12 1.405(12) . ? C11 C33 1.544(11) . ? C12 C13 1.392(12) . ? C12 H12A 0.9500 . ? C13 C14 1.379(13) . ? C13 C43 1.507(12) . ? C14 H14A 0.9500 . ? C15 C16 1.525(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.397(12) . ? C16 C17 1.407(11) . ? C17 C18 1.410(12) . ? C18 C19 1.391(12) . ? C18 C44 1.550(12) . ? C19 C20 1.386(12) . ? C19 H19A 0.9500 . ? C20 C21 1.380(13) . ? C20 C54 1.528(12) . ? C21 H21A 0.9500 . ? C22 C29 1.534(13) . ? C22 C31 1.543(13) . ? C22 C26 1.550(13) . ? C23 C30 1.524(18) . ? C23 C26 1.532(15) . ? C23 C27 1.537(18) . ? C23 H23A 1.0000 . ? C24 C27 1.516(17) . ? C24 C28 1.522(18) . ? C24 C31 1.535(14) . ? C24 H24A 1.0000 . ? C25 C28 1.512(19) . ? C25 C30 1.529(16) . ? C25 C29 1.530(15) . ? C25 H25A 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C37 1.526(12) . ? C33 C40 1.563(12) . ? C33 C42 1.565(12) . ? C34 C37 1.541(12) . ? C34 C38 1.541(16) . ? C34 C41 1.546(15) . ? C34 H34A 1.0000 . ? C35 C38 1.502(15) . ? C35 C39 1.530(15) . ? C35 C42 1.560(12) . ? C35 H35A 1.0000 . ? C36 C41 1.520(14) . ? C36 C40 1.526(12) . ? C36 C39 1.538(15) . ? C36 H36A 1.0000 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C48 1.492(11) . ? C44 C51 1.541(13) . ? C44 C53 1.556(12) . ? C45 C52 1.517(14) . ? C45 C49 1.542(13) . ? C45 C48 1.573(12) . ? C45 H45A 1.0000 . ? C46 C53 1.532(12) . ? C46 C49 1.542(13) . ? C46 C50 1.547(14) . ? C46 H46A 1.0000 . ? C47 C52 1.531(13) . ? C47 C50 1.533(13) . ? C47 C51 1.544(12) . ? C47 H47A 1.0000 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.466(15) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 O8 1.305(11) . ? U2 O9 2.159(5) . ? U2 O11 2.160(6) . ? U2 O10 2.166(6) . ? U2 O8 2.210(6) . ? U2 N2 2.561(6) . ? U2 O12 2.613(6) . ? U2 O13 2.668(6) . ? O9 C63 1.366(10) . ? O10 C70 1.361(10) . ? O11 C77 1.367(10) . ? O12 C115 1.428(12) . ? O12 C116 1.452(11) . ? O13 C118 1.429(12) . ? O13 C117 1.432(11) . ? N2 C61 1.491(11) . ? N2 C75 1.499(11) . ? N2 C68 1.502(11) . ? C61 C62 1.504(13) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C67 1.387(14) . ? C62 C63 1.411(12) . ? C63 C64 1.429(13) . ? C64 C65 1.400(14) . ? C64 C82 1.541(12) . ? C65 C66 1.384(15) . ? C65 H65A 0.9500 . ? C66 C67 1.387(16) . ? C66 C92 1.504(18) . ? C67 H67A 0.9500 . ? C68 C69 1.498(13) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C74 1.398(13) . ? C69 C70 1.425(12) . ? C70 C71 1.418(12) . ? C71 C72 1.396(12) . ? C71 C93 1.541(12) . ? C72 C73 1.397(12) . ? C72 H72A 0.9500 . ? C73 C74 1.380(14) . ? C73 C103 1.503(12) . ? C74 H74A 0.9500 . ? C75 C76 1.482(13) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C81 1.391(12) . ? C76 C77 1.418(12) . ? C77 C78 1.403(13) . ? C78 C79 1.407(13) . ? C78 C104 1.529(12) . ? C79 C80 1.389(14) . ? C79 H79A 0.9500 . ? C80 C81 1.385(14) . ? C80 C114 1.515(14) . ? C81 H81A 0.9500 . ? C82 C89 1.531(13) . ? C82 C91 1.534(12) . ? C82 C86 1.554(12) . ? C83 C90 1.516(14) . ? C83 C87 1.530(13) . ? C83 C86 1.541(13) . ? C83 H83A 1.0000 . ? C84 C88 1.529(14) . ? C84 C87 1.533(14) . ? C84 C91 1.540(13) . ? C84 H84A 1.0000 . ? C85 C88 1.525(13) . ? C85 C90 1.526(13) . ? C85 C89 1.546(12) . ? C85 H85A 1.0000 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C93 C102 1.543(12) . ? C93 C97 1.553(13) . ? C93 C100 1.557(12) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C94 C98 1.518(15) . ? C94 C101 1.530(14) . ? C94 C97 1.544(13) . ? C94 H94A 1.0000 . ? C95 C98 1.507(14) . ? C95 C99 1.529(14) . ? C95 C102 1.532(12) . ? C95 H95A 1.0000 . ? C96 C101 1.523(14) . ? C96 C99 1.532(14) . ? C96 C100 1.536(12) . ? C96 H96A 1.0000 . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? C103 H10G 0.9800 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? C104 C113 1.514(14) . ? C104 C108 1.523(13) . ? C104 C111 1.535(14) . ? C105 C107 1.493(16) . ? C105 C112 1.512(17) . ? C105 C108 1.522(14) . ? C105 H10J 1.0000 . ? C106 C110 1.527(19) . ? C106 C107 1.541(17) . ? C106 C113 1.559(14) . ? C106 H10K 1.0000 . ? C107 H10L 0.9900 . ? C107 H10M 0.9900 . ? C108 H10N 0.9900 . ? C108 H10O 0.9900 . ? C109 C110 1.472(19) . ? C109 C112 1.505(19) . ? C109 C111 1.544(15) . ? C109 H10P 1.0000 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9800 . ? C114 H11J 0.9800 . ? C114 H11K 0.9800 . ? C115 H11L 0.9800 . ? C115 H11M 0.9800 . ? C115 H11N 0.9800 . ? C116 C117 1.485(16) . ? C116 H11O 0.9900 . ? C116 H11P 0.9900 . ? C117 H11Q 0.9900 . ? C117 H11R 0.9900 . ? C118 H11S 0.9800 . ? C118 H11T 0.9800 . ? C118 H11U 0.9800 . ? C201 O202 1.394(18) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? O202 C203 1.294(18) . ? C203 C204 1.42(2) . ? C203 H20D 0.9900 . ? C203 H20E 0.9900 . ? C204 O205 1.336(19) . ? C204 H20F 0.9900 . ? C204 H20G 0.9900 . ? O205 C206 1.401(19) . ? C206 H20H 0.9800 . ? C206 H20I 0.9800 . ? C206 H20J 0.9800 . ? C207 O208 1.44(2) . ? C207 H20K 0.9800 . ? C207 H20L 0.9800 . ? C207 H20M 0.9800 . ? O208 C209 1.332(18) . ? C209 C210 1.62(3) . ? C209 H20N 0.9900 . ? C209 H20O 0.9900 . ? C210 O211 1.39(2) . ? C210 H21B 0.9900 . ? C210 H21C 0.9900 . ? O211 C212 1.47(2) . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? C213 O214 1.38(2) . ? C213 H21G 0.9800 . ? C213 H21H 0.9800 . ? C213 H21I 0.9800 . ? O214 C215 1.24(2) . ? C215 C216 1.41(3) . ? C215 H21J 0.9900 . ? C215 H21K 0.9900 . ? C216 O217 1.34(2) . ? C216 H21L 0.9900 . ? C216 H21M 0.9900 . ? O217 C218 1.41(2) . ? C218 H21N 0.9800 . ? C218 H21O 0.9800 . ? C218 H21P 0.9800 . ? C219 O220 1.36(2) . ? C219 H21Q 0.9800 . ? C219 H21R 0.9800 . ? C219 H21S 0.9800 . ? O220 C221 1.28(2) . ? C221 C222 1.44(3) . ? C221 H22A 0.9900 . ? C221 H22B 0.9900 . ? C222 O223 1.34(2) . ? C222 H22C 0.9900 . ? C222 H22D 0.9900 . ? O223 C224 1.40(2) . ? C224 H22E 0.9800 . ? C224 H22F 0.9800 . ? C224 H22G 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 O1 U1 O3 105.0(2) . . ? O1 U1 O2 86.3(2) . . ? O3 U1 O2 144.1(2) . . ? O1 U1 O6 145.73(19) . . ? O3 U1 O6 75.1(2) . . ? O2 U1 O6 76.8(2) . . ? O1 U1 O7 158.63(19) . . ? O3 U1 O7 87.2(2) . . ? O2 U1 O7 93.9(2) . . ? O6 U1 O7 53.88(18) . . ? O1 U1 N1 71.2(2) . . ? O3 U1 N1 71.7(2) . . ? O2 U1 N1 80.4(2) . . ? O6 U1 N1 76.7(2) . . ? O7 U1 N1 130.0(2) . . ? O1 U1 O5 89.1(2) . . ? O3 U1 O5 121.9(2) . . ? O2 U1 O5 91.7(2) . . ? O6 U1 O5 120.59(19) . . ? O7 U1 O5 69.5(2) . . ? N1 U1 O5 159.1(2) . . ? O1 U1 O4 72.1(2) . . ? O3 U1 O4 71.00(19) . . ? O2 U1 O4 144.01(19) . . ? O6 U1 O4 135.61(19) . . ? O7 U1 O4 96.30(19) . . ? N1 U1 O4 117.2(2) . . ? O5 U1 O4 60.34(19) . . ? O1 U1 C59 170.9(2) . . ? O3 U1 C59 79.1(2) . . ? O2 U1 C59 85.8(2) . . ? O6 U1 C59 26.7(2) . . ? O7 U1 C59 27.2(2) . . ? N1 U1 C59 103.0(2) . . ? O5 U1 C59 95.7(2) . . ? O4 U1 C59 117.0(2) . . ? C3 O1 U1 149.2(5) . . ? C10 O2 U1 131.3(5) . . ? C17 O3 U1 143.2(5) . . ? C55 O4 C56 112.3(7) . . ? C55 O4 U1 118.5(5) . . ? C56 O4 U1 119.3(5) . . ? C58 O5 C57 112.7(8) . . ? C58 O5 U1 116.9(5) . . ? C57 O5 U1 114.8(5) . . ? C59 O6 U1 94.0(5) . . ? C59 O7 U1 92.4(5) . . ? C15 N1 C1 107.7(6) . . ? C15 N1 C8 108.8(6) . . ? C1 N1 C8 110.7(6) . . ? C15 N1 U1 112.5(5) . . ? C1 N1 U1 109.2(5) . . ? C8 N1 U1 108.1(4) . . ? N1 C1 C2 115.6(7) . . ? N1 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? N1 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C7 C2 C3 120.3(8) . . ? C7 C2 C1 119.8(8) . . ? C3 C2 C1 120.0(7) . . ? O1 C3 C4 123.4(8) . . ? O1 C3 C2 116.7(8) . . ? C4 C3 C2 119.8(8) . . ? C3 C4 C5 117.1(8) . . ? C3 C4 C22 121.3(7) . . ? C5 C4 C22 121.2(8) . . ? C6 C5 C4 123.9(9) . . ? C6 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? C7 C6 C5 117.2(8) . . ? C7 C6 C32 121.3(9) . . ? C5 C6 C32 121.5(9) . . ? C6 C7 C2 121.4(9) . . ? C6 C7 H7A 119.3 . . ? C2 C7 H7A 119.3 . . ? N1 C8 C9 117.0(7) . . ? N1 C8 H8A 108.1 . . ? C9 C8 H8A 108.1 . . ? N1 C8 H8B 108.1 . . ? C9 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C14 C9 C10 119.6(8) . . ? C14 C9 C8 119.3(7) . . ? C10 C9 C8 120.8(7) . . ? O2 C10 C11 124.0(7) . . ? O2 C10 C9 116.7(7) . . ? C11 C10 C9 119.3(8) . . ? C12 C11 C10 117.4(8) . . ? C12 C11 C33 118.9(8) . . ? C10 C11 C33 123.6(7) . . ? C13 C12 C11 124.1(8) . . ? C13 C12 H12A 117.9 . . ? C11 C12 H12A 117.9 . . ? C14 C13 C12 117.0(8) . . ? C14 C13 C43 121.6(8) . . ? C12 C13 C43 121.3(9) . . ? C13 C14 C9 122.0(8) . . ? C13 C14 H14A 119.0 . . ? C9 C14 H14A 119.0 . . ? N1 C15 C16 116.7(7) . . ? N1 C15 H15A 108.1 . . ? C16 C15 H15A 108.1 . . ? N1 C15 H15B 108.1 . . ? C16 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C21 C16 C17 119.6(8) . . ? C21 C16 C15 115.7(7) . . ? C17 C16 C15 124.6(7) . . ? O3 C17 C16 119.2(7) . . ? O3 C17 C18 121.4(7) . . ? C16 C17 C18 119.4(7) . . ? C19 C18 C17 118.4(8) . . ? C19 C18 C44 119.9(8) . . ? C17 C18 C44 121.7(8) . . ? C20 C19 C18 122.8(8) . . ? C20 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? C21 C20 C19 118.1(8) . . ? C21 C20 C54 121.4(8) . . ? C19 C20 C54 120.4(8) . . ? C20 C21 C16 121.5(8) . . ? C20 C21 H21A 119.3 . . ? C16 C21 H21A 119.3 . . ? C29 C22 C31 109.6(8) . . ? C29 C22 C4 109.5(7) . . ? C31 C22 C4 110.7(7) . . ? C29 C22 C26 109.1(8) . . ? C31 C22 C26 105.9(7) . . ? C4 C22 C26 111.9(7) . . ? C30 C23 C26 109.5(10) . . ? C30 C23 C27 108.4(11) . . ? C26 C23 C27 109.0(10) . . ? C30 C23 H23A 110.0 . . ? C26 C23 H23A 110.0 . . ? C27 C23 H23A 110.0 . . ? C27 C24 C28 110.3(11) . . ? C27 C24 C31 109.2(10) . . ? C28 C24 C31 108.8(9) . . ? C27 C24 H24A 109.5 . . ? C28 C24 H24A 109.5 . . ? C31 C24 H24A 109.5 . . ? C28 C25 C30 108.7(11) . . ? C28 C25 C29 108.9(10) . . ? C30 C25 C29 109.4(10) . . ? C28 C25 H25A 109.9 . . ? C30 C25 H25A 109.9 . . ? C29 C25 H25A 109.9 . . ? C23 C26 C22 111.1(8) . . ? C23 C26 H26A 109.4 . . ? C22 C26 H26A 109.4 . . ? C23 C26 H26B 109.4 . . ? C22 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C24 C27 C23 109.4(10) . . ? C24 C27 H27A 109.8 . . ? C23 C27 H27A 109.8 . . ? C24 C27 H27B 109.8 . . ? C23 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? C25 C28 C24 110.8(10) . . ? C25 C28 H28A 109.5 . . ? C24 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C25 C29 C22 110.5(8) . . ? C25 C29 H29A 109.6 . . ? C22 C29 H29A 109.6 . . ? C25 C29 H29B 109.6 . . ? C22 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C23 C30 C25 111.0(10) . . ? C23 C30 H30A 109.4 . . ? C25 C30 H30A 109.4 . . ? C23 C30 H30B 109.4 . . ? C25 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C24 C31 C22 110.6(9) . . ? C24 C31 H31A 109.5 . . ? C22 C31 H31A 109.5 . . ? C24 C31 H31B 109.5 . . ? C22 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C6 C32 H32A 109.5 . . ? C6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C37 C33 C11 112.0(7) . . ? C37 C33 C40 107.6(7) . . ? C11 C33 C40 111.8(7) . . ? C37 C33 C42 108.4(7) . . ? C11 C33 C42 109.7(7) . . ? C40 C33 C42 107.2(7) . . ? C37 C34 C38 109.3(9) . . ? C37 C34 C41 107.3(9) . . ? C38 C34 C41 109.9(9) . . ? C37 C34 H34A 110.1 . . ? C38 C34 H34A 110.1 . . ? C41 C34 H34A 110.1 . . ? C38 C35 C39 109.2(9) . . ? C38 C35 C42 110.1(8) . . ? C39 C35 C42 110.0(8) . . ? C38 C35 H35A 109.2 . . ? C39 C35 H35A 109.2 . . ? C42 C35 H35A 109.2 . . ? C41 C36 C40 110.6(8) . . ? C41 C36 C39 108.1(8) . . ? C40 C36 C39 110.1(8) . . ? C41 C36 H36A 109.4 . . ? C40 C36 H36A 109.4 . . ? C39 C36 H36A 109.4 . . ? C33 C37 C34 112.6(7) . . ? C33 C37 H37A 109.1 . . ? C34 C37 H37A 109.1 . . ? C33 C37 H37B 109.1 . . ? C34 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C35 C38 C34 109.8(8) . . ? C35 C38 H38A 109.7 . . ? C34 C38 H38A 109.7 . . ? C35 C38 H38B 109.7 . . ? C34 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C35 C39 C36 109.9(8) . . ? C35 C39 H39A 109.7 . . ? C36 C39 H39A 109.7 . . ? C35 C39 H39B 109.7 . . ? C36 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C36 C40 C33 110.8(8) . . ? C36 C40 H40A 109.5 . . ? C33 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C36 C41 C34 109.6(8) . . ? C36 C41 H41A 109.7 . . ? C34 C41 H41A 109.7 . . ? C36 C41 H41B 109.7 . . ? C34 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? C35 C42 C33 109.8(7) . . ? C35 C42 H42A 109.7 . . ? C33 C42 H42A 109.7 . . ? C35 C42 H42B 109.7 . . ? C33 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C13 C43 H43A 109.5 . . ? C13 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C13 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C48 C44 C51 106.4(7) . . ? C48 C44 C18 111.7(7) . . ? C51 C44 C18 111.2(7) . . ? C48 C44 C53 108.6(7) . . ? C51 C44 C53 108.5(7) . . ? C18 C44 C53 110.3(7) . . ? C52 C45 C49 109.4(8) . . ? C52 C45 C48 107.1(8) . . ? C49 C45 C48 109.7(8) . . ? C52 C45 H45A 110.2 . . ? C49 C45 H45A 110.2 . . ? C48 C45 H45A 110.2 . . ? C53 C46 C49 109.6(7) . . ? C53 C46 C50 108.9(8) . . ? C49 C46 C50 109.7(8) . . ? C53 C46 H46A 109.5 . . ? C49 C46 H46A 109.5 . . ? C50 C46 H46A 109.5 . . ? C52 C47 C50 109.7(8) . . ? C52 C47 C51 110.2(8) . . ? C50 C47 C51 109.6(8) . . ? C52 C47 H47A 109.1 . . ? C50 C47 H47A 109.1 . . ? C51 C47 H47A 109.1 . . ? C44 C48 C45 113.2(7) . . ? C44 C48 H48A 108.9 . . ? C45 C48 H48A 108.9 . . ? C44 C48 H48B 108.9 . . ? C45 C48 H48B 108.9 . . ? H48A C48 H48B 107.8 . . ? C45 C49 C46 109.0(8) . . ? C45 C49 H49A 109.9 . . ? C46 C49 H49A 109.9 . . ? C45 C49 H49B 109.9 . . ? C46 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? C47 C50 C46 108.9(8) . . ? C47 C50 H50A 109.9 . . ? C46 C50 H50A 109.9 . . ? C47 C50 H50B 109.9 . . ? C46 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? C44 C51 C47 110.4(8) . . ? C44 C51 H51A 109.6 . . ? C47 C51 H51A 109.6 . . ? C44 C51 H51B 109.6 . . ? C47 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? C45 C52 C47 109.7(8) . . ? C45 C52 H52A 109.7 . . ? C47 C52 H52A 109.7 . . ? C45 C52 H52B 109.7 . . ? C47 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? C46 C53 C44 111.5(7) . . ? C46 C53 H53A 109.3 . . ? C44 C53 H53A 109.3 . . ? C46 C53 H53B 109.3 . . ? C44 C53 H53B 109.3 . . ? H53A C53 H53B 108.0 . . ? C20 C54 H54A 109.5 . . ? C20 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C20 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O4 C55 H55A 109.5 . . ? O4 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O4 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O4 C56 C57 107.9(8) . . ? O4 C56 H56A 110.1 . . ? C57 C56 H56A 110.1 . . ? O4 C56 H56B 110.1 . . ? C57 C56 H56B 110.1 . . ? H56A C56 H56B 108.4 . . ? O5 C57 C56 107.0(8) . . ? O5 C57 H57A 110.3 . . ? C56 C57 H57A 110.3 . . ? O5 C57 H57B 110.3 . . ? C56 C57 H57B 110.3 . . ? H57A C57 H57B 108.6 . . ? O5 C58 H58A 109.5 . . ? O5 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O5 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O6 C59 O7 119.6(8) . . ? O6 C59 O8 120.3(8) . . ? O7 C59 O8 120.0(8) . . ? O6 C59 U1 59.3(4) . . ? O7 C59 U1 60.5(4) . . ? O8 C59 U1 173.9(6) . . ? O9 U2 O11 87.7(2) . . ? O9 U2 O10 85.7(2) . . ? O11 U2 O10 151.8(2) . . ? O9 U2 O8 160.5(2) . . ? O11 U2 O8 88.7(2) . . ? O10 U2 O8 88.6(2) . . ? O9 U2 N2 78.7(2) . . ? O11 U2 N2 75.5(2) . . ? O10 U2 N2 76.4(2) . . ? O8 U2 N2 81.8(2) . . ? O9 U2 O12 104.5(2) . . ? O11 U2 O12 74.8(2) . . ? O10 U2 O12 133.4(2) . . ? O8 U2 O12 93.0(2) . . ? N2 U2 O12 149.9(2) . . ? O9 U2 O13 112.8(2) . . ? O11 U2 O13 133.4(2) . . ? O10 U2 O13 74.0(2) . . ? O8 U2 O13 83.2(2) . . ? N2 U2 O13 147.0(2) . . ? O12 U2 O13 60.0(2) . . ? C59 O8 U2 167.2(6) . . ? C63 O9 U2 133.9(5) . . ? C70 O10 U2 142.2(5) . . ? C77 O11 U2 144.6(5) . . ? C115 O12 C116 114.8(8) . . ? C115 O12 U2 114.8(6) . . ? C116 O12 U2 109.9(5) . . ? C118 O13 C117 110.3(8) . . ? C118 O13 U2 121.1(5) . . ? C117 O13 U2 122.0(6) . . ? C61 N2 C75 111.3(7) . . ? C61 N2 C68 108.9(7) . . ? C75 N2 C68 105.5(6) . . ? C61 N2 U2 114.3(5) . . ? C75 N2 U2 108.5(5) . . ? C68 N2 U2 108.0(5) . . ? N2 C61 C62 120.1(7) . . ? N2 C61 H61A 107.3 . . ? C62 C61 H61A 107.3 . . ? N2 C61 H61B 107.3 . . ? C62 C61 H61B 107.3 . . ? H61A C61 H61B 106.9 . . ? C67 C62 C63 118.3(9) . . ? C67 C62 C61 120.2(9) . . ? C63 C62 C61 120.7(8) . . ? O9 C63 C62 118.1(8) . . ? O9 C63 C64 121.0(7) . . ? C62 C63 C64 120.9(8) . . ? C65 C64 C63 116.2(9) . . ? C65 C64 C82 121.6(9) . . ? C63 C64 C82 122.1(8) . . ? C66 C65 C64 123.6(11) . . ? C66 C65 H65A 118.2 . . ? C64 C65 H65A 118.2 . . ? C65 C66 C67 117.8(10) . . ? C65 C66 C92 121.2(12) . . ? C67 C66 C92 121.0(11) . . ? C66 C67 C62 122.4(10) . . ? C66 C67 H67A 118.8 . . ? C62 C67 H67A 118.8 . . ? C69 C68 N2 115.6(7) . . ? C69 C68 H68A 108.4 . . ? N2 C68 H68A 108.4 . . ? C69 C68 H68B 108.4 . . ? N2 C68 H68B 108.4 . . ? H68A C68 H68B 107.4 . . ? C74 C69 C70 119.8(9) . . ? C74 C69 C68 119.1(8) . . ? C70 C69 C68 121.1(8) . . ? O10 C70 C71 124.7(7) . . ? O10 C70 C69 115.7(8) . . ? C71 C70 C69 119.7(8) . . ? C72 C71 C70 117.3(8) . . ? C72 C71 C93 122.1(8) . . ? C70 C71 C93 120.6(7) . . ? C71 C72 C73 123.8(9) . . ? C71 C72 H72A 118.1 . . ? C73 C72 H72A 118.1 . . ? C74 C73 C72 117.9(8) . . ? C74 C73 C103 121.1(8) . . ? C72 C73 C103 121.0(9) . . ? C73 C74 C69 121.4(8) . . ? C73 C74 H74A 119.3 . . ? C69 C74 H74A 119.3 . . ? C76 C75 N2 116.7(7) . . ? C76 C75 H75A 108.1 . . ? N2 C75 H75A 108.1 . . ? C76 C75 H75B 108.1 . . ? N2 C75 H75B 108.1 . . ? H75A C75 H75B 107.3 . . ? C81 C76 C77 119.0(8) . . ? C81 C76 C75 120.4(8) . . ? C77 C76 C75 120.6(8) . . ? O11 C77 C78 123.0(7) . . ? O11 C77 C76 116.0(8) . . ? C78 C77 C76 121.0(8) . . ? C77 C78 C79 116.9(8) . . ? C77 C78 C104 123.4(8) . . ? C79 C78 C104 119.7(8) . . ? C80 C79 C78 123.2(9) . . ? C80 C79 H79A 118.4 . . ? C78 C79 H79A 118.4 . . ? C81 C80 C79 118.3(9) . . ? C81 C80 C114 121.9(9) . . ? C79 C80 C114 119.8(10) . . ? C80 C81 C76 121.6(8) . . ? C80 C81 H81A 119.2 . . ? C76 C81 H81A 119.2 . . ? C89 C82 C91 109.7(7) . . ? C89 C82 C64 109.6(7) . . ? C91 C82 C64 111.5(7) . . ? C89 C82 C86 108.5(7) . . ? C91 C82 C86 106.6(7) . . ? C64 C82 C86 110.9(7) . . ? C90 C83 C87 109.9(8) . . ? C90 C83 C86 110.8(8) . . ? C87 C83 C86 108.5(8) . . ? C90 C83 H83A 109.2 . . ? C87 C83 H83A 109.2 . . ? C86 C83 H83A 109.2 . . ? C88 C84 C87 110.6(8) . . ? C88 C84 C91 108.9(8) . . ? C87 C84 C91 108.1(8) . . ? C88 C84 H84A 109.8 . . ? C87 C84 H84A 109.8 . . ? C91 C84 H84A 109.8 . . ? C88 C85 C90 109.8(8) . . ? C88 C85 C89 109.7(7) . . ? C90 C85 C89 109.2(8) . . ? C88 C85 H85A 109.4 . . ? C90 C85 H85A 109.4 . . ? C89 C85 H85A 109.4 . . ? C83 C86 C82 110.0(8) . . ? C83 C86 H86A 109.7 . . ? C82 C86 H86A 109.7 . . ? C83 C86 H86B 109.7 . . ? C82 C86 H86B 109.7 . . ? H86A C86 H86B 108.2 . . ? C83 C87 C84 109.2(8) . . ? C83 C87 H87A 109.8 . . ? C84 C87 H87A 109.8 . . ? C83 C87 H87B 109.8 . . ? C84 C87 H87B 109.8 . . ? H87A C87 H87B 108.3 . . ? C85 C88 C84 109.5(8) . . ? C85 C88 H88A 109.8 . . ? C84 C88 H88A 109.8 . . ? C85 C88 H88B 109.8 . . ? C84 C88 H88B 109.8 . . ? H88A C88 H88B 108.2 . . ? C82 C89 C85 110.3(7) . . ? C82 C89 H89A 109.6 . . ? C85 C89 H89A 109.6 . . ? C82 C89 H89B 109.6 . . ? C85 C89 H89B 109.6 . . ? H89A C89 H89B 108.1 . . ? C83 C90 C85 109.7(7) . . ? C83 C90 H90A 109.7 . . ? C85 C90 H90A 109.7 . . ? C83 C90 H90B 109.7 . . ? C85 C90 H90B 109.7 . . ? H90A C90 H90B 108.2 . . ? C82 C91 C84 111.5(7) . . ? C82 C91 H91A 109.3 . . ? C84 C91 H91A 109.3 . . ? C82 C91 H91B 109.3 . . ? C84 C91 H91B 109.3 . . ? H91A C91 H91B 108.0 . . ? C71 C93 C102 109.5(7) . . ? C71 C93 C97 112.5(7) . . ? C102 C93 C97 107.0(7) . . ? C71 C93 C100 111.1(7) . . ? C102 C93 C100 110.6(7) . . ? C97 C93 C100 106.0(7) . . ? C66 C92 H92A 109.5 . . ? C66 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C66 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C98 C94 C101 109.8(8) . . ? C98 C94 C97 110.0(9) . . ? C101 C94 C97 110.2(8) . . ? C98 C94 H94A 108.9 . . ? C101 C94 H94A 108.9 . . ? C97 C94 H94A 108.9 . . ? C98 C95 C99 110.2(8) . . ? C98 C95 C102 110.1(8) . . ? C99 C95 C102 108.6(8) . . ? C98 C95 H95A 109.3 . . ? C99 C95 H95A 109.3 . . ? C102 C95 H95A 109.3 . . ? C101 C96 C99 109.3(8) . . ? C101 C96 C100 109.3(8) . . ? C99 C96 C100 109.9(8) . . ? C101 C96 H96A 109.4 . . ? C99 C96 H96A 109.4 . . ? C100 C96 H96A 109.4 . . ? C94 C97 C93 110.2(7) . . ? C94 C97 H97A 109.6 . . ? C93 C97 H97A 109.6 . . ? C94 C97 H97B 109.6 . . ? C93 C97 H97B 109.6 . . ? H97A C97 H97B 108.1 . . ? C95 C98 C94 109.1(8) . . ? C95 C98 H98A 109.9 . . ? C94 C98 H98A 109.9 . . ? C95 C98 H98B 109.9 . . ? C94 C98 H98B 109.9 . . ? H98A C98 H98B 108.3 . . ? C95 C99 C96 110.0(8) . . ? C95 C99 H99A 109.7 . . ? C96 C99 H99A 109.7 . . ? C95 C99 H99B 109.7 . . ? C96 C99 H99B 109.7 . . ? H99A C99 H99B 108.2 . . ? C96 C100 C93 110.3(7) . . ? C96 C100 H10A 109.6 . . ? C93 C100 H10A 109.6 . . ? C96 C100 H10B 109.6 . . ? C93 C100 H10B 109.6 . . ? H10A C100 H10B 108.1 . . ? C96 C101 C94 108.7(8) . . ? C96 C101 H10C 110.0 . . ? C94 C101 H10C 110.0 . . ? C96 C101 H10D 110.0 . . ? C94 C101 H10D 110.0 . . ? H10C C101 H10D 108.3 . . ? C95 C102 C93 110.9(8) . . ? C95 C102 H10E 109.5 . . ? C93 C102 H10E 109.5 . . ? C95 C102 H10F 109.5 . . ? C93 C102 H10F 109.5 . . ? H10E C102 H10F 108.1 . . ? C73 C103 H10G 109.5 . . ? C73 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? C73 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C113 C104 C108 105.6(9) . . ? C113 C104 C78 113.0(7) . . ? C108 C104 C78 112.7(8) . . ? C113 C104 C111 110.5(9) . . ? C108 C104 C111 105.4(9) . . ? C78 C104 C111 109.2(8) . . ? C107 C105 C112 109.9(9) . . ? C107 C105 C108 110.1(10) . . ? C112 C105 C108 109.3(10) . . ? C107 C105 H10J 109.2 . . ? C112 C105 H10J 109.2 . . ? C108 C105 H10J 109.2 . . ? C110 C106 C107 109.8(9) . . ? C110 C106 C113 109.0(10) . . ? C107 C106 C113 107.7(10) . . ? C110 C106 H10K 110.1 . . ? C107 C106 H10K 110.1 . . ? C113 C106 H10K 110.1 . . ? C105 C107 C106 108.2(9) . . ? C105 C107 H10L 110.1 . . ? C106 C107 H10L 110.1 . . ? C105 C107 H10M 110.1 . . ? C106 C107 H10M 110.1 . . ? H10L C107 H10M 108.4 . . ? C105 C108 C104 112.9(9) . . ? C105 C108 H10N 109.0 . . ? C104 C108 H10N 109.0 . . ? C105 C108 H10O 109.0 . . ? C104 C108 H10O 109.0 . . ? H10N C108 H10O 107.8 . . ? C110 C109 C112 109.8(11) . . ? C110 C109 C111 109.4(11) . . ? C112 C109 C111 108.4(11) . . ? C110 C109 H10P 109.7 . . ? C112 C109 H10P 109.7 . . ? C111 C109 H10P 109.7 . . ? C109 C110 C106 111.2(9) . . ? C109 C110 H11A 109.4 . . ? C106 C110 H11A 109.4 . . ? C109 C110 H11B 109.4 . . ? C106 C110 H11B 109.4 . . ? H11A C110 H11B 108.0 . . ? C104 C111 C109 111.6(9) . . ? C104 C111 H11C 109.3 . . ? C109 C111 H11C 109.3 . . ? C104 C111 H11D 109.3 . . ? C109 C111 H11D 109.3 . . ? H11C C111 H11D 108.0 . . ? C109 C112 C105 109.8(9) . . ? C109 C112 H11E 109.7 . . ? C105 C112 H11E 109.7 . . ? C109 C112 H11F 109.7 . . ? C105 C112 H11F 109.7 . . ? H11E C112 H11F 108.2 . . ? C104 C113 C106 111.4(8) . . ? C104 C113 H11G 109.4 . . ? C106 C113 H11G 109.4 . . ? C104 C113 H11H 109.4 . . ? C106 C113 H11H 109.4 . . ? H11G C113 H11H 108.0 . . ? C80 C114 H11I 109.5 . . ? C80 C114 H11J 109.5 . . ? H11I C114 H11J 109.5 . . ? C80 C114 H11K 109.5 . . ? H11I C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? O12 C115 H11L 109.5 . . ? O12 C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? O12 C115 H11N 109.5 . . ? H11L C115 H11N 109.5 . . ? H11M C115 H11N 109.5 . . ? O12 C116 C117 110.3(8) . . ? O12 C116 H11O 109.6 . . ? C117 C116 H11O 109.6 . . ? O12 C116 H11P 109.6 . . ? C117 C116 H11P 109.6 . . ? H11O C116 H11P 108.1 . . ? O13 C117 C116 106.8(8) . . ? O13 C117 H11Q 110.4 . . ? C116 C117 H11Q 110.4 . . ? O13 C117 H11R 110.4 . . ? C116 C117 H11R 110.4 . . ? H11Q C117 H11R 108.6 . . ? O13 C118 H11S 109.5 . . ? O13 C118 H11T 109.5 . . ? H11S C118 H11T 109.5 . . ? O13 C118 H11U 109.5 . . ? H11S C118 H11U 109.5 . . ? H11T C118 H11U 109.5 . . ? O202 C201 H20A 109.5 . . ? O202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? O202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C203 O202 C201 118.1(14) . . ? O202 C203 C204 121.1(16) . . ? O202 C203 H20D 107.0 . . ? C204 C203 H20D 107.0 . . ? O202 C203 H20E 107.0 . . ? C204 C203 H20E 107.0 . . ? H20D C203 H20E 106.8 . . ? O205 C204 C203 117.5(17) . . ? O205 C204 H20F 107.9 . . ? C203 C204 H20F 107.9 . . ? O205 C204 H20G 107.9 . . ? C203 C204 H20G 107.9 . . ? H20F C204 H20G 107.2 . . ? C204 O205 C206 116.3(15) . . ? O205 C206 H20H 109.5 . . ? O205 C206 H20I 109.5 . . ? H20H C206 H20I 109.5 . . ? O205 C206 H20J 109.5 . . ? H20H C206 H20J 109.5 . . ? H20I C206 H20J 109.5 . . ? O208 C207 H20K 109.5 . . ? O208 C207 H20L 109.5 . . ? H20K C207 H20L 109.5 . . ? O208 C207 H20M 109.5 . . ? H20K C207 H20M 109.5 . . ? H20L C207 H20M 109.5 . . ? C209 O208 C207 105.4(14) . . ? O208 C209 C210 106.5(14) . . ? O208 C209 H20N 110.4 . . ? C210 C209 H20N 110.4 . . ? O208 C209 H20O 110.4 . . ? C210 C209 H20O 110.4 . . ? H20N C209 H20O 108.6 . . ? O211 C210 C209 105.5(15) . . ? O211 C210 H21B 110.6 . . ? C209 C210 H21B 110.6 . . ? O211 C210 H21C 110.6 . . ? C209 C210 H21C 110.6 . . ? H21B C210 H21C 108.8 . . ? C210 O211 C212 106.9(16) . . ? O211 C212 H21D 109.5 . . ? O211 C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? O211 C212 H21F 109.5 . . ? H21D C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? O214 C213 H21G 109.5 . . ? O214 C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? O214 C213 H21I 109.5 . . ? H21G C213 H21I 109.5 . . ? H21H C213 H21I 109.5 . . ? C215 O214 C213 115(3) . . ? O214 C215 C216 119(3) . . ? O214 C215 H21J 107.5 . . ? C216 C215 H21J 107.5 . . ? O214 C215 H21K 107.5 . . ? C216 C215 H21K 107.5 . . ? H21J C215 H21K 107.0 . . ? O217 C216 C215 117(3) . . ? O217 C216 H21L 107.9 . . ? C215 C216 H21L 107.9 . . ? O217 C216 H21M 107.9 . . ? C215 C216 H21M 108.0 . . ? H21L C216 H21M 107.2 . . ? C216 O217 C218 121(3) . . ? O217 C218 H21N 109.5 . . ? O217 C218 H21O 109.5 . . ? H21N C218 H21O 109.5 . . ? O217 C218 H21P 109.5 . . ? H21N C218 H21P 109.5 . . ? H21O C218 H21P 109.5 . . ? O220 C219 H21Q 109.5 . . ? O220 C219 H21R 109.5 . . ? H21Q C219 H21R 109.5 . . ? O220 C219 H21S 109.5 . . ? H21Q C219 H21S 109.5 . . ? H21R C219 H21S 109.5 . . ? C221 O220 C219 113(3) . . ? O220 C221 C222 114(3) . . ? O220 C221 H22A 108.8 . . ? C222 C221 H22A 108.8 . . ? O220 C221 H22B 108.8 . . ? C222 C221 H22B 108.8 . . ? H22A C221 H22B 107.7 . . ? O223 C222 C221 112(2) . . ? O223 C222 H22C 109.2 . . ? C221 C222 H22C 109.2 . . ? O223 C222 H22D 109.2 . . ? C221 C222 H22D 109.2 . . ? H22C C222 H22D 107.9 . . ? C222 O223 C224 113(2) . . ? O223 C224 H22E 109.5 . . ? O223 C224 H22F 109.5 . . ? H22E C224 H22F 109.5 . . ? O223 C224 H22G 109.5 . . ? H22E C224 H22G 109.5 . . ? H22F C224 H22G 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 O3 U1 O1 C3 60.2(10) . . . . ? O2 U1 O1 C3 -85.1(10) . . . . ? O6 U1 O1 C3 -25.2(12) . . . . ? O7 U1 O1 C3 -176.5(9) . . . . ? N1 U1 O1 C3 -4.0(10) . . . . ? O5 U1 O1 C3 -176.9(10) . . . . ? O4 U1 O1 C3 124.1(10) . . . . ? O1 U1 O2 C10 111.3(7) . . . . ? O3 U1 O2 C10 0.6(8) . . . . ? O6 U1 O2 C10 -38.7(6) . . . . ? O7 U1 O2 C10 -90.1(7) . . . . ? N1 U1 O2 C10 39.8(6) . . . . ? O5 U1 O2 C10 -159.7(7) . . . . ? O4 U1 O2 C10 163.5(6) . . . . ? C59 U1 O2 C10 -64.2(7) . . . . ? O1 U1 O3 C17 -103.7(9) . . . . ? O2 U1 O3 C17 1.2(10) . . . . ? O6 U1 O3 C17 40.8(8) . . . . ? O7 U1 O3 C17 94.1(9) . . . . ? N1 U1 O3 C17 -39.8(8) . . . . ? O5 U1 O3 C17 157.8(8) . . . . ? O4 U1 O3 C17 -168.3(9) . . . . ? C59 U1 O3 C17 67.9(9) . . . . ? O1 U1 O4 C55 -42.6(6) . . . . ? O3 U1 O4 C55 70.9(6) . . . . ? O2 U1 O4 C55 -98.6(7) . . . . ? O6 U1 O4 C55 113.1(6) . . . . ? O7 U1 O4 C55 155.8(6) . . . . ? N1 U1 O4 C55 14.3(7) . . . . ? O5 U1 O4 C55 -142.1(7) . . . . ? C59 U1 O4 C55 137.3(6) . . . . ? O1 U1 O4 C56 100.3(7) . . . . ? O3 U1 O4 C56 -146.2(7) . . . . ? O2 U1 O4 C56 44.3(8) . . . . ? O6 U1 O4 C56 -104.0(6) . . . . ? O7 U1 O4 C56 -61.3(7) . . . . ? N1 U1 O4 C56 157.2(6) . . . . ? O5 U1 O4 C56 0.8(6) . . . . ? C59 U1 O4 C56 -79.8(7) . . . . ? O1 U1 O5 C58 122.8(7) . . . . ? O3 U1 O5 C58 -130.0(7) . . . . ? O2 U1 O5 C58 36.5(7) . . . . ? O6 U1 O5 C58 -39.1(8) . . . . ? O7 U1 O5 C58 -57.0(7) . . . . ? N1 U1 O5 C58 103.7(9) . . . . ? O4 U1 O5 C58 -167.3(8) . . . . ? C59 U1 O5 C58 -49.4(7) . . . . ? O1 U1 O5 C57 -101.9(7) . . . . ? O3 U1 O5 C57 5.3(7) . . . . ? O2 U1 O5 C57 171.8(6) . . . . ? O6 U1 O5 C57 96.1(7) . . . . ? O7 U1 O5 C57 78.3(7) . . . . ? N1 U1 O5 C57 -121.0(8) . . . . ? O4 U1 O5 C57 -32.1(6) . . . . ? C59 U1 O5 C57 85.9(7) . . . . ? O1 U1 O6 C59 -169.9(5) . . . . ? O3 U1 O6 C59 95.3(5) . . . . ? O2 U1 O6 C59 -107.3(5) . . . . ? O7 U1 O6 C59 -2.3(5) . . . . ? N1 U1 O6 C59 169.6(5) . . . . ? O5 U1 O6 C59 -23.2(6) . . . . ? O4 U1 O6 C59 54.2(6) . . . . ? O1 U1 O7 C59 162.8(6) . . . . ? O3 U1 O7 C59 -71.2(5) . . . . ? O2 U1 O7 C59 72.8(5) . . . . ? O6 U1 O7 C59 2.3(5) . . . . ? N1 U1 O7 C59 -8.0(6) . . . . ? O5 U1 O7 C59 163.2(5) . . . . ? O4 U1 O7 C59 -141.7(5) . . . . ? O1 U1 N1 C15 164.0(6) . . . . ? O3 U1 N1 C15 50.4(5) . . . . ? O2 U1 N1 C15 -106.7(5) . . . . ? O6 U1 N1 C15 -28.1(5) . . . . ? O7 U1 N1 C15 -19.6(6) . . . . ? O5 U1 N1 C15 -175.8(5) . . . . ? O4 U1 N1 C15 106.7(5) . . . . ? C59 U1 N1 C15 -23.3(6) . . . . ? O1 U1 N1 C1 44.5(5) . . . . ? O3 U1 N1 C1 -69.1(5) . . . . ? O2 U1 N1 C1 133.9(5) . . . . ? O6 U1 N1 C1 -147.5(5) . . . . ? O7 U1 N1 C1 -139.0(5) . . . . ? O5 U1 N1 C1 64.8(8) . . . . ? O4 U1 N1 C1 -12.8(6) . . . . ? C59 U1 N1 C1 -142.7(5) . . . . ? O1 U1 N1 C8 -75.9(5) . . . . ? O3 U1 N1 C8 170.5(5) . . . . ? O2 U1 N1 C8 13.5(5) . . . . ? O6 U1 N1 C8 92.1(5) . . . . ? O7 U1 N1 C8 100.6(5) . . . . ? O5 U1 N1 C8 -55.6(8) . . . . ? O4 U1 N1 C8 -133.2(5) . . . . ? C59 U1 N1 C8 96.8(5) . . . . ? C15 N1 C1 C2 162.7(7) . . . . ? C8 N1 C1 C2 43.9(9) . . . . ? U1 N1 C1 C2 -74.9(7) . . . . ? N1 C1 C2 C7 -131.0(8) . . . . ? N1 C1 C2 C3 49.3(11) . . . . ? U1 O1 C3 C4 157.7(7) . . . . ? U1 O1 C3 C2 -19.5(14) . . . . ? C7 C2 C3 O1 -177.9(8) . . . . ? C1 C2 C3 O1 1.7(12) . . . . ? C7 C2 C3 C4 4.8(13) . . . . ? C1 C2 C3 C4 -175.5(8) . . . . ? O1 C3 C4 C5 177.2(8) . . . . ? C2 C3 C4 C5 -5.7(12) . . . . ? O1 C3 C4 C22 -9.5(13) . . . . ? C2 C3 C4 C22 167.5(8) . . . . ? C3 C4 C5 C6 2.6(14) . . . . ? C22 C4 C5 C6 -170.7(9) . . . . ? C4 C5 C6 C7 1.6(15) . . . . ? C4 C5 C6 C32 -179.9(10) . . . . ? C5 C6 C7 C2 -2.7(15) . . . . ? C32 C6 C7 C2 178.9(10) . . . . ? C3 C2 C7 C6 -0.5(14) . . . . ? C1 C2 C7 C6 179.9(9) . . . . ? C15 N1 C8 C9 61.5(9) . . . . ? C1 N1 C8 C9 179.5(7) . . . . ? U1 N1 C8 C9 -61.0(8) . . . . ? N1 C8 C9 C14 -113.8(9) . . . . ? N1 C8 C9 C10 71.7(10) . . . . ? U1 O2 C10 C11 134.2(7) . . . . ? U1 O2 C10 C9 -47.6(10) . . . . ? C14 C9 C10 O2 174.3(7) . . . . ? C8 C9 C10 O2 -11.1(12) . . . . ? C14 C9 C10 C11 -7.4(12) . . . . ? C8 C9 C10 C11 167.1(8) . . . . ? O2 C10 C11 C12 -175.0(8) . . . . ? C9 C10 C11 C12 6.9(12) . . . . ? O2 C10 C11 C33 8.2(13) . . . . ? C9 C10 C11 C33 -169.9(8) . . . . ? C10 C11 C12 C13 -1.5(14) . . . . ? C33 C11 C12 C13 175.4(8) . . . . ? C11 C12 C13 C14 -3.4(14) . . . . ? C11 C12 C13 C43 177.9(9) . . . . ? C12 C13 C14 C9 2.9(13) . . . . ? C43 C13 C14 C9 -178.4(9) . . . . ? C10 C9 C14 C13 2.3(13) . . . . ? C8 C9 C14 C13 -172.3(8) . . . . ? C1 N1 C15 C16 57.3(9) . . . . ? C8 N1 C15 C16 177.3(7) . . . . ? U1 N1 C15 C16 -63.0(8) . . . . ? N1 C15 C16 C21 -147.9(8) . . . . ? N1 C15 C16 C17 37.4(12) . . . . ? U1 O3 C17 C16 25.2(13) . . . . ? U1 O3 C17 C18 -153.2(7) . . . . ? C21 C16 C17 O3 176.8(8) . . . . ? C15 C16 C17 O3 -8.7(13) . . . . ? C21 C16 C17 C18 -4.8(12) . . . . ? C15 C16 C17 C18 169.7(8) . . . . ? O3 C17 C18 C19 -177.9(8) . . . . ? C16 C17 C18 C19 3.7(12) . . . . ? O3 C17 C18 C44 3.5(12) . . . . ? C16 C17 C18 C44 -174.8(8) . . . . ? C17 C18 C19 C20 0.6(14) . . . . ? C44 C18 C19 C20 179.2(8) . . . . ? C18 C19 C20 C21 -3.8(14) . . . . ? C18 C19 C20 C54 177.6(9) . . . . ? C19 C20 C21 C16 2.8(14) . . . . ? C54 C20 C21 C16 -178.7(9) . . . . ? C17 C16 C21 C20 1.5(14) . . . . ? C15 C16 C21 C20 -173.5(9) . . . . ? C3 C4 C22 C29 -59.5(11) . . . . ? C5 C4 C22 C29 113.4(9) . . . . ? C3 C4 C22 C31 61.5(11) . . . . ? C5 C4 C22 C31 -125.6(9) . . . . ? C3 C4 C22 C26 179.3(8) . . . . ? C5 C4 C22 C26 -7.7(12) . . . . ? C30 C23 C26 C22 -57.5(13) . . . . ? C27 C23 C26 C22 60.9(12) . . . . ? C29 C22 C26 C23 57.5(11) . . . . ? C31 C22 C26 C23 -60.4(11) . . . . ? C4 C22 C26 C23 178.8(9) . . . . ? C28 C24 C27 C23 -59.3(13) . . . . ? C31 C24 C27 C23 60.2(14) . . . . ? C30 C23 C27 C24 59.6(13) . . . . ? C26 C23 C27 C24 -59.5(13) . . . . ? C30 C25 C28 C24 -57.8(12) . . . . ? C29 C25 C28 C24 61.3(12) . . . . ? C27 C24 C28 C25 59.1(12) . . . . ? C31 C24 C28 C25 -60.7(12) . . . . ? C28 C25 C29 C22 -59.4(12) . . . . ? C30 C25 C29 C22 59.4(13) . . . . ? C31 C22 C29 C25 57.4(11) . . . . ? C4 C22 C29 C25 179.0(9) . . . . ? C26 C22 C29 C25 -58.2(11) . . . . ? C26 C23 C30 C25 58.5(14) . . . . ? C27 C23 C30 C25 -60.3(13) . . . . ? C28 C25 C30 C23 59.4(13) . . . . ? C29 C25 C30 C23 -59.5(14) . . . . ? C27 C24 C31 C22 -62.4(12) . . . . ? C28 C24 C31 C22 58.1(12) . . . . ? C29 C22 C31 C24 -56.9(10) . . . . ? C4 C22 C31 C24 -177.8(8) . . . . ? C26 C22 C31 C24 60.7(10) . . . . ? C12 C11 C33 C37 -4.5(11) . . . . ? C10 C11 C33 C37 172.3(8) . . . . ? C12 C11 C33 C40 116.4(9) . . . . ? C10 C11 C33 C40 -66.9(11) . . . . ? C12 C11 C33 C42 -124.9(8) . . . . ? C10 C11 C33 C42 51.9(10) . . . . ? C11 C33 C37 C34 -178.0(8) . . . . ? C40 C33 C37 C34 58.8(10) . . . . ? C42 C33 C37 C34 -56.8(11) . . . . ? C38 C34 C37 C33 58.2(11) . . . . ? C41 C34 C37 C33 -61.1(11) . . . . ? C39 C35 C38 C34 -59.7(10) . . . . ? C42 C35 C38 C34 61.0(11) . . . . ? C37 C34 C38 C35 -59.1(11) . . . . ? C41 C34 C38 C35 58.5(11) . . . . ? C38 C35 C39 C36 62.1(10) . . . . ? C42 C35 C39 C36 -58.8(11) . . . . ? C41 C36 C39 C35 -61.8(10) . . . . ? C40 C36 C39 C35 59.1(11) . . . . ? C41 C36 C40 C33 58.8(11) . . . . ? C39 C36 C40 C33 -60.5(10) . . . . ? C37 C33 C40 C36 -56.3(10) . . . . ? C11 C33 C40 C36 -179.7(8) . . . . ? C42 C33 C40 C36 60.1(9) . . . . ? C40 C36 C41 C34 -60.7(11) . . . . ? C39 C36 C41 C34 59.9(10) . . . . ? C37 C34 C41 C36 60.0(11) . . . . ? C38 C34 C41 C36 -58.8(10) . . . . ? C38 C35 C42 C33 -60.3(10) . . . . ? C39 C35 C42 C33 60.0(10) . . . . ? C37 C33 C42 C35 56.6(9) . . . . ? C11 C33 C42 C35 179.2(7) . . . . ? C40 C33 C42 C35 -59.2(9) . . . . ? C19 C18 C44 C48 3.0(12) . . . . ? C17 C18 C44 C48 -178.4(8) . . . . ? C19 C18 C44 C51 121.7(9) . . . . ? C17 C18 C44 C51 -59.7(11) . . . . ? C19 C18 C44 C53 -117.9(9) . . . . ? C17 C18 C44 C53 60.7(11) . . . . ? C51 C44 C48 C45 61.1(10) . . . . ? C18 C44 C48 C45 -177.4(8) . . . . ? C53 C44 C48 C45 -55.5(10) . . . . ? C52 C45 C48 C44 -61.7(10) . . . . ? C49 C45 C48 C44 57.0(11) . . . . ? C52 C45 C49 C46 60.2(10) . . . . ? C48 C45 C49 C46 -57.0(10) . . . . ? C53 C46 C49 C45 60.0(10) . . . . ? C50 C46 C49 C45 -59.6(10) . . . . ? C52 C47 C50 C46 -59.6(10) . . . . ? C51 C47 C50 C46 61.5(10) . . . . ? C53 C46 C50 C47 -60.6(10) . . . . ? C49 C46 C50 C47 59.4(10) . . . . ? C48 C44 C51 C47 -59.2(9) . . . . ? C18 C44 C51 C47 179.0(7) . . . . ? C53 C44 C51 C47 57.5(9) . . . . ? C52 C47 C51 C44 60.0(10) . . . . ? C50 C47 C51 C44 -60.8(10) . . . . ? C49 C45 C52 C47 -60.9(10) . . . . ? C48 C45 C52 C47 58.0(10) . . . . ? C50 C47 C52 C45 60.9(10) . . . . ? C51 C47 C52 C45 -59.8(10) . . . . ? C49 C46 C53 C44 -60.6(10) . . . . ? C50 C46 C53 C44 59.4(10) . . . . ? C48 C44 C53 C46 57.6(10) . . . . ? C51 C44 C53 C46 -57.6(10) . . . . ? C18 C44 C53 C46 -179.7(7) . . . . ? C55 O4 C56 C57 173.7(8) . . . . ? U1 O4 C56 C57 28.7(10) . . . . ? C58 O5 C57 C56 -161.6(8) . . . . ? U1 O5 C57 C56 61.2(9) . . . . ? O4 C56 C57 O5 -55.9(10) . . . . ? U1 O6 C59 O7 4.1(8) . . . . ? U1 O6 C59 O8 -172.9(7) . . . . ? U1 O7 C59 O6 -4.1(8) . . . . ? U1 O7 C59 O8 172.9(7) . . . . ? O3 U1 C59 O6 -78.5(5) . . . . ? O2 U1 C59 O6 68.8(5) . . . . ? O7 U1 C59 O6 175.9(8) . . . . ? N1 U1 C59 O6 -10.4(5) . . . . ? O5 U1 C59 O6 160.1(5) . . . . ? O4 U1 C59 O6 -140.4(4) . . . . ? O3 U1 C59 O7 105.6(5) . . . . ? O2 U1 C59 O7 -107.1(5) . . . . ? O6 U1 C59 O7 -175.9(8) . . . . ? N1 U1 C59 O7 173.8(5) . . . . ? O5 U1 C59 O7 -15.8(5) . . . . ? O4 U1 C59 O7 43.7(5) . . . . ? O6 C59 O8 U2 -20(3) . . . . ? O7 C59 O8 U2 163(2) . . . . ? O9 U2 O8 C59 -149(3) . . . . ? O11 U2 O8 C59 132(3) . . . . ? O10 U2 O8 C59 -76(3) . . . . ? N2 U2 O8 C59 -153(3) . . . . ? O12 U2 O8 C59 57(3) . . . . ? O13 U2 O8 C59 -2(3) . . . . ? O11 U2 O9 C63 31.0(7) . . . . ? O10 U2 O9 C63 -121.6(7) . . . . ? O8 U2 O9 C63 -48.5(12) . . . . ? N2 U2 O9 C63 -44.6(7) . . . . ? O12 U2 O9 C63 104.7(7) . . . . ? O13 U2 O9 C63 167.8(7) . . . . ? O9 U2 O10 C70 60.7(9) . . . . ? O11 U2 O10 C70 -16.2(12) . . . . ? O8 U2 O10 C70 -100.7(9) . . . . ? N2 U2 O10 C70 -18.7(9) . . . . ? O12 U2 O10 C70 166.6(8) . . . . ? O13 U2 O10 C70 176.0(9) . . . . ? O9 U2 O11 C77 -65.5(9) . . . . ? O10 U2 O11 C77 10.9(12) . . . . ? O8 U2 O11 C77 95.4(9) . . . . ? N2 U2 O11 C77 13.5(9) . . . . ? O12 U2 O11 C77 -171.2(10) . . . . ? O13 U2 O11 C77 174.7(8) . . . . ? O9 U2 O12 C115 -160.2(6) . . . . ? O11 U2 O12 C115 -76.7(7) . . . . ? O10 U2 O12 C115 102.0(7) . . . . ? O8 U2 O12 C115 11.1(7) . . . . ? N2 U2 O12 C115 -67.7(8) . . . . ? O13 U2 O12 C115 91.6(7) . . . . ? O9 U2 O12 C116 68.7(6) . . . . ? O11 U2 O12 C116 152.2(6) . . . . ? O10 U2 O12 C116 -29.2(7) . . . . ? O8 U2 O12 C116 -120.0(6) . . . . ? N2 U2 O12 C116 161.2(6) . . . . ? O13 U2 O12 C116 -39.6(6) . . . . ? O9 U2 O13 C118 133.4(7) . . . . ? O11 U2 O13 C118 -116.8(7) . . . . ? O10 U2 O13 C118 55.3(7) . . . . ? O8 U2 O13 C118 -35.1(7) . . . . ? N2 U2 O13 C118 28.4(9) . . . . ? O12 U2 O13 C118 -132.6(7) . . . . ? O9 U2 O13 C117 -77.9(8) . . . . ? O11 U2 O13 C117 31.8(9) . . . . ? O10 U2 O13 C117 -156.0(8) . . . . ? O8 U2 O13 C117 113.5(8) . . . . ? N2 U2 O13 C117 177.0(7) . . . . ? O12 U2 O13 C117 16.1(7) . . . . ? O9 U2 N2 C61 -0.2(6) . . . . ? O11 U2 N2 C61 -90.8(6) . . . . ? O10 U2 N2 C61 88.0(6) . . . . ? O8 U2 N2 C61 178.5(6) . . . . ? O12 U2 N2 C61 -99.7(7) . . . . ? O13 U2 N2 C61 114.6(6) . . . . ? O9 U2 N2 C75 124.6(5) . . . . ? O11 U2 N2 C75 34.0(5) . . . . ? O10 U2 N2 C75 -147.2(5) . . . . ? O8 U2 N2 C75 -56.7(5) . . . . ? O12 U2 N2 C75 25.0(8) . . . . ? O13 U2 N2 C75 -120.6(6) . . . . ? O9 U2 N2 C68 -121.5(6) . . . . ? O11 U2 N2 C68 147.9(6) . . . . ? O10 U2 N2 C68 -33.3(5) . . . . ? O8 U2 N2 C68 57.2(5) . . . . ? O12 U2 N2 C68 138.9(5) . . . . ? O13 U2 N2 C68 -6.7(8) . . . . ? C75 N2 C61 C62 -80.6(9) . . . . ? C68 N2 C61 C62 163.6(8) . . . . ? U2 N2 C61 C62 42.7(10) . . . . ? N2 C61 C62 C67 127.3(11) . . . . ? N2 C61 C62 C63 -62.8(12) . . . . ? U2 O9 C63 C62 42.6(12) . . . . ? U2 O9 C63 C64 -136.8(7) . . . . ? C67 C62 C63 O9 -170.8(10) . . . . ? C61 C62 C63 O9 19.1(13) . . . . ? C67 C62 C63 C64 8.6(15) . . . . ? C61 C62 C63 C64 -161.5(9) . . . . ? O9 C63 C64 C65 170.7(10) . . . . ? C62 C63 C64 C65 -8.7(15) . . . . ? O9 C63 C64 C82 -10.6(14) . . . . ? C62 C63 C64 C82 170.0(9) . . . . ? C63 C64 C65 C66 2(2) . . . . ? C82 C64 C65 C66 -176.4(13) . . . . ? C64 C65 C66 C67 4(3) . . . . ? C64 C65 C66 C92 -177.0(15) . . . . ? C65 C66 C67 C62 -4(2) . . . . ? C92 C66 C67 C62 176.7(15) . . . . ? C63 C62 C67 C66 -2(2) . . . . ? C61 C62 C67 C66 168.3(13) . . . . ? C61 N2 C68 C69 -52.7(9) . . . . ? C75 N2 C68 C69 -172.2(7) . . . . ? U2 N2 C68 C69 72.0(8) . . . . ? N2 C68 C69 C74 123.5(9) . . . . ? N2 C68 C69 C70 -58.7(12) . . . . ? U2 O10 C70 C71 -140.0(8) . . . . ? U2 O10 C70 C69 38.9(13) . . . . ? C74 C69 C70 O10 178.0(8) . . . . ? C68 C69 C70 O10 0.2(13) . . . . ? C74 C69 C70 C71 -3.0(14) . . . . ? C68 C69 C70 C71 179.2(8) . . . . ? O10 C70 C71 C72 -177.7(8) . . . . ? C69 C70 C71 C72 3.4(13) . . . . ? O10 C70 C71 C93 0.3(13) . . . . ? C69 C70 C71 C93 -178.6(8) . . . . ? C70 C71 C72 C73 -1.6(14) . . . . ? C93 C71 C72 C73 -179.6(9) . . . . ? C71 C72 C73 C74 -0.8(15) . . . . ? C71 C72 C73 C103 179.2(9) . . . . ? C72 C73 C74 C69 1.3(15) . . . . ? C103 C73 C74 C69 -178.7(9) . . . . ? C70 C69 C74 C73 0.6(15) . . . . ? C68 C69 C74 C73 178.5(9) . . . . ? C61 N2 C75 C76 54.6(9) . . . . ? C68 N2 C75 C76 172.5(7) . . . . ? U2 N2 C75 C76 -72.0(8) . . . . ? N2 C75 C76 C81 -123.2(9) . . . . ? N2 C75 C76 C77 59.0(11) . . . . ? U2 O11 C77 C78 147.9(8) . . . . ? U2 O11 C77 C76 -31.7(14) . . . . ? C81 C76 C77 O11 178.4(8) . . . . ? C75 C76 C77 O11 -3.7(12) . . . . ? C81 C76 C77 C78 -1.2(14) . . . . ? C75 C76 C77 C78 176.7(8) . . . . ? O11 C77 C78 C79 -178.1(9) . . . . ? C76 C77 C78 C79 1.5(14) . . . . ? O11 C77 C78 C104 2.9(14) . . . . ? C76 C77 C78 C104 -177.5(8) . . . . ? C77 C78 C79 C80 -0.8(16) . . . . ? C104 C78 C79 C80 178.3(10) . . . . ? C78 C79 C80 C81 -0.2(17) . . . . ? C78 C79 C80 C114 -178.9(12) . . . . ? C79 C80 C81 C76 0.6(16) . . . . ? C114 C80 C81 C76 179.2(12) . . . . ? C77 C76 C81 C80 0.1(15) . . . . ? C75 C76 C81 C80 -177.8(10) . . . . ? C65 C64 C82 C89 127.0(11) . . . . ? C63 C64 C82 C89 -51.7(11) . . . . ? C65 C64 C82 C91 -111.4(12) . . . . ? C63 C64 C82 C91 69.9(11) . . . . ? C65 C64 C82 C86 7.2(14) . . . . ? C63 C64 C82 C86 -171.4(8) . . . . ? C90 C83 C86 C82 -58.4(10) . . . . ? C87 C83 C86 C82 62.3(10) . . . . ? C89 C82 C86 C83 57.8(9) . . . . ? C91 C82 C86 C83 -60.2(10) . . . . ? C64 C82 C86 C83 178.2(8) . . . . ? C90 C83 C87 C84 59.2(10) . . . . ? C86 C83 C87 C84 -62.0(10) . . . . ? C88 C84 C87 C83 -58.2(10) . . . . ? C91 C84 C87 C83 60.9(10) . . . . ? C90 C85 C88 C84 -58.8(10) . . . . ? C89 C85 C88 C84 61.2(10) . . . . ? C87 C84 C88 C85 58.2(10) . . . . ? C91 C84 C88 C85 -60.4(10) . . . . ? C91 C82 C89 C85 56.5(9) . . . . ? C64 C82 C89 C85 179.2(7) . . . . ? C86 C82 C89 C85 -59.6(9) . . . . ? C88 C85 C89 C82 -59.3(10) . . . . ? C90 C85 C89 C82 61.1(9) . . . . ? C87 C83 C90 C85 -60.5(10) . . . . ? C86 C83 C90 C85 59.3(10) . . . . ? C88 C85 C90 C83 60.4(10) . . . . ? C89 C85 C90 C83 -60.0(10) . . . . ? C89 C82 C91 C84 -57.0(10) . . . . ? C64 C82 C91 C84 -178.6(8) . . . . ? C86 C82 C91 C84 60.2(10) . . . . ? C88 C84 C91 C82 58.8(10) . . . . ? C87 C84 C91 C82 -61.4(10) . . . . ? C72 C71 C93 C102 112.8(10) . . . . ? C70 C71 C93 C102 -65.1(10) . . . . ? C72 C71 C93 C97 -6.0(12) . . . . ? C70 C71 C93 C97 176.1(8) . . . . ? C72 C71 C93 C100 -124.7(9) . . . . ? C70 C71 C93 C100 57.4(11) . . . . ? C98 C94 C97 C93 -60.4(10) . . . . ? C101 C94 C97 C93 60.8(11) . . . . ? C71 C93 C97 C94 178.6(8) . . . . ? C102 C93 C97 C94 58.3(10) . . . . ? C100 C93 C97 C94 -59.8(10) . . . . ? C99 C95 C98 C94 59.5(10) . . . . ? C102 C95 C98 C94 -60.2(10) . . . . ? C101 C94 C98 C95 -61.3(10) . . . . ? C97 C94 C98 C95 60.1(10) . . . . ? C98 C95 C99 C96 -58.6(10) . . . . ? C102 C95 C99 C96 62.1(10) . . . . ? C101 C96 C99 C95 58.6(10) . . . . ? C100 C96 C99 C95 -61.4(10) . . . . ? C101 C96 C100 C93 -63.0(10) . . . . ? C99 C96 C100 C93 57.0(10) . . . . ? C71 C93 C100 C96 -176.3(8) . . . . ? C102 C93 C100 C96 -54.5(10) . . . . ? C97 C93 C100 C96 61.2(9) . . . . ? C99 C96 C101 C94 -59.9(10) . . . . ? C100 C96 C101 C94 60.5(10) . . . . ? C98 C94 C101 C96 61.7(10) . . . . ? C97 C94 C101 C96 -59.7(11) . . . . ? C98 C95 C102 C93 61.1(10) . . . . ? C99 C95 C102 C93 -59.6(10) . . . . ? C71 C93 C102 C95 179.0(8) . . . . ? C97 C93 C102 C95 -58.8(10) . . . . ? C100 C93 C102 C95 56.3(10) . . . . ? C77 C78 C104 C113 -60.0(13) . . . . ? C79 C78 C104 C113 121.1(11) . . . . ? C77 C78 C104 C108 -179.7(10) . . . . ? C79 C78 C104 C108 1.4(14) . . . . ? C77 C78 C104 C111 63.5(12) . . . . ? C79 C78 C104 C111 -115.5(11) . . . . ? C112 C105 C107 C106 -60.5(12) . . . . ? C108 C105 C107 C106 60.0(13) . . . . ? C110 C106 C107 C105 57.9(12) . . . . ? C113 C106 C107 C105 -60.7(12) . . . . ? C107 C105 C108 C104 -60.8(14) . . . . ? C112 C105 C108 C104 60.0(13) . . . . ? C113 C104 C108 C105 58.4(13) . . . . ? C78 C104 C108 C105 -177.7(10) . . . . ? C111 C104 C108 C105 -58.6(13) . . . . ? C112 C109 C110 C106 57.8(12) . . . . ? C111 C109 C110 C106 -61.0(13) . . . . ? C107 C106 C110 C109 -57.5(12) . . . . ? C113 C106 C110 C109 60.3(12) . . . . ? C113 C104 C111 C109 -54.3(13) . . . . ? C108 C104 C111 C109 59.3(13) . . . . ? C78 C104 C111 C109 -179.3(10) . . . . ? C110 C109 C111 C104 57.8(15) . . . . ? C112 C109 C111 C104 -61.9(14) . . . . ? C110 C109 C112 C105 -59.6(12) . . . . ? C111 C109 C112 C105 59.9(13) . . . . ? C107 C105 C112 C109 61.9(12) . . . . ? C108 C105 C112 C109 -59.0(12) . . . . ? C108 C104 C113 C106 -59.7(12) . . . . ? C78 C104 C113 C106 176.6(10) . . . . ? C111 C104 C113 C106 53.8(13) . . . . ? C110 C106 C113 C104 -56.2(13) . . . . ? C107 C106 C113 C104 62.9(13) . . . . ? C115 O12 C116 C117 -66.4(11) . . . . ? U2 O12 C116 C117 64.8(9) . . . . ? C118 O13 C117 C116 161.2(9) . . . . ? U2 O13 C117 C116 9.5(12) . . . . ? O12 C116 C117 O13 -47.3(12) . . . . ? C201 O202 C203 C204 179(2) . . . . ? O202 C203 C204 O205 -48(3) . . . . ? C203 C204 O205 C206 -169.0(19) . . . . ? C207 O208 C209 C210 -167.3(16) . . . . ? O208 C209 C210 O211 66.7(18) . . . . ? C209 C210 O211 C212 177.4(13) . . . . ? C213 O214 C215 C216 -172(4) . . . . ? O214 C215 C216 O217 -176(4) . . . . ? C215 C216 O217 C218 -91(5) . . . . ? C219 O220 C221 C222 175(3) . . . . ? O220 C221 C222 O223 70(5) . . . . ? C221 C222 O223 C224 167(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.990 _refine_diff_density_min -2.498 _refine_diff_density_rms 0.203 data_opl0941 _database_code_depnum_ccdc_archive 'CCDC 759478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C116 H152 N2 O11 U2, 3(C4 H10 O2)' _chemical_formula_sum 'C128 H182 N2 O17 U2' _chemical_formula_weight 2496.82 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 C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.734(2) _cell_length_b 15.847(2) _cell_length_c 22.159(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.575(8) _cell_angle_gamma 90.00 _cell_volume 11483(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 371 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 2.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.461 _exptl_absorpt_correction_T_max 0.562 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.50 \% and 60 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78453 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.10 _reflns_number_total 12648 _reflns_number_gt 8273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0115P)^2^+55.9295P] 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 12648 _refine_ls_number_parameters 822 _refine_ls_number_restraints 290 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.090 _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 U1 U 0.064195(5) 0.787254(12) 0.260383(6) 0.03159(6) Uani 1 1 d . . . O1 O 0.07081(8) 0.85884(19) 0.17536(11) 0.0270(7) Uani 1 1 d . . . O2 O 0.06135(9) 0.6677(2) 0.31264(12) 0.0334(8) Uani 1 1 d . . . O3 O 0.13056(8) 0.7794(2) 0.26222(11) 0.0305(7) Uani 1 1 d . . . O4 O 0.0000 0.7873(3) 0.2500 0.0329(10) Uani 1 2 d S . . N1 N 0.07454(12) 0.6738(3) 0.18087(15) 0.0388(10) Uani 1 1 d . . . C1 C 0.05546(15) 0.7039(3) 0.12164(17) 0.0412(12) Uani 1 1 d . . . H1A H 0.0526 0.6549 0.0940 0.049 Uiso 1 1 calc R B . H1B H 0.0276 0.7247 0.1288 0.049 Uiso 1 1 calc R . . C2 C 0.07826(14) 0.7720(3) 0.09059(17) 0.0380(12) Uani 1 1 d . . . C3 C 0.08594(13) 0.8494(3) 0.11967(17) 0.0298(11) Uani 1 1 d . . . C4 C 0.10826(13) 0.9129(3) 0.09146(18) 0.0308(11) Uani 1 1 d . . . C5 C 0.12099(15) 0.8956(3) 0.03298(19) 0.0421(13) Uani 1 1 d . . . H5A H 0.1356 0.9382 0.0129 0.051 Uiso 1 1 calc R B . C6 C 0.11352(17) 0.8200(3) 0.0028(2) 0.0469(14) Uani 1 1 d . . . C7 C 0.09198(16) 0.7587(3) 0.03230(19) 0.0463(14) Uani 1 1 d . . . H7A H 0.0863 0.7064 0.0127 0.056 Uiso 1 1 calc R B . C8 C 0.04970(16) 0.5986(3) 0.19772(18) 0.0414(13) Uani 1 1 d . . . H8A H 0.0220 0.6182 0.2072 0.050 Uiso 1 1 calc R B . H8B H 0.0467 0.5610 0.1621 0.050 Uiso 1 1 calc R . . C9 C 0.06651(16) 0.5482(3) 0.24977(19) 0.0396(12) Uani 1 1 d . . . C10 C 0.07080(14) 0.5847(3) 0.30762(19) 0.0352(12) Uani 1 1 d . . . C11 C 0.08522(15) 0.5341(3) 0.35698(19) 0.0378(12) Uani 1 1 d . A . C12 C 0.09830(16) 0.4529(3) 0.3442(2) 0.0480(14) Uani 1 1 d . . . H12A H 0.1094 0.4198 0.3767 0.058 Uiso 1 1 calc R B . C13 C 0.09616(18) 0.4169(3) 0.2867(2) 0.0503(14) Uani 1 1 d . . . C14 C 0.07917(17) 0.4659(3) 0.2404(2) 0.0518(15) Uani 1 1 d . . . H14A H 0.0761 0.4424 0.2010 0.062 Uiso 1 1 calc R B . C15 C 0.11870(15) 0.6522(3) 0.17347(18) 0.0421(13) Uani 1 1 d . . . H15A H 0.1307 0.6971 0.1487 0.051 Uiso 1 1 calc R B . H15B H 0.1197 0.5992 0.1499 0.051 Uiso 1 1 calc R . . C16 C 0.14604(14) 0.6412(3) 0.22994(18) 0.0365(11) Uani 1 1 d . . . C17 C 0.15394(13) 0.7093(3) 0.26931(16) 0.0331(10) Uani 1 1 d . . . C18 C 0.18547(12) 0.7040(3) 0.31533(17) 0.0320(10) Uani 1 1 d . . . C19 C 0.20351(14) 0.6245(3) 0.3238(2) 0.0368(12) Uani 1 1 d . . . H19A H 0.2233 0.6180 0.3562 0.044 Uiso 1 1 calc R B . C20 C 0.19432(16) 0.5546(3) 0.2880(2) 0.0401(12) Uani 1 1 d . . . C21 C 0.16664(16) 0.5652(3) 0.2396(2) 0.0436(13) Uani 1 1 d . . . H21A H 0.1616 0.5197 0.2124 0.052 Uiso 1 1 calc R B . C22 C 0.11995(12) 0.9948(3) 0.12310(17) 0.0264(10) Uani 1 1 d . . . C23 C 0.15478(17) 1.1374(3) 0.1178(2) 0.0496(14) Uani 1 1 d . . . H23A H 0.1700 1.1757 0.0909 0.060 Uiso 1 1 calc R B . C24 C 0.1585(2) 1.0566(4) 0.2141(2) 0.0702(19) Uani 1 1 d U . . H24A H 0.1762 1.0423 0.2506 0.084 Uiso 1 1 calc R B . C25 C 0.0934(2) 1.1223(3) 0.1776(3) 0.0698(18) Uani 1 1 d U . . H25A H 0.0680 1.1510 0.1907 0.084 Uiso 1 1 calc R B . C26 C 0.14358(15) 1.0564(3) 0.08349(19) 0.0387(12) Uani 1 1 d . . . H26A H 0.1688 1.0287 0.0705 0.046 Uiso 1 1 calc R . . H26B H 0.1265 1.0706 0.0468 0.046 Uiso 1 1 calc R . . C27 C 0.1821(2) 1.1153(4) 0.1729(3) 0.074(2) Uani 1 1 d . . . H27A H 0.1901 1.1673 0.1951 0.089 Uiso 1 1 calc R . . H27B H 0.2072 1.0869 0.1601 0.089 Uiso 1 1 calc R . . C28 C 0.1204(2) 1.0993(4) 0.2331(2) 0.0788(19) Uani 1 1 d U . . H28A H 0.1276 1.1510 0.2563 0.095 Uiso 1 1 calc R . . H28B H 0.1053 1.0612 0.2597 0.095 Uiso 1 1 calc R . . C29 C 0.08172(14) 1.0423(3) 0.1427(2) 0.0406(12) Uani 1 1 d . . . H29A H 0.0644 1.0573 0.1066 0.049 Uiso 1 1 calc R . . H29B H 0.0656 1.0050 0.1685 0.049 Uiso 1 1 calc R . . C30 C 0.1164(2) 1.1813(3) 0.1365(3) 0.072(2) Uani 1 1 d . . . H30A H 0.0990 1.1958 0.1004 0.087 Uiso 1 1 calc R . . H30B H 0.1236 1.2342 0.1583 0.087 Uiso 1 1 calc R . . C31 C 0.14760(14) 0.9763(3) 0.1796(2) 0.0390(12) Uani 1 1 d . . . H31A H 0.1333 0.9371 0.2064 0.047 Uiso 1 1 calc R . . H31B H 0.1730 0.9484 0.1673 0.047 Uiso 1 1 calc R . . C32 C 0.12911(19) 0.8060(4) -0.0602(2) 0.0640(18) Uani 1 1 d . . . H32A H 0.1235 0.7477 -0.0729 0.096 Uiso 1 1 calc R B . H32B H 0.1586 0.8164 -0.0596 0.096 Uiso 1 1 calc R . . H32C H 0.1152 0.8448 -0.0887 0.096 Uiso 1 1 calc R . . C33 C 0.0850(2) 0.5631(12) 0.4223(8) 0.0308(18) Uani 0.766(4) 1 d PD A 1 C34 C 0.0377(2) 0.6097(5) 0.5043(3) 0.0518(17) Uani 0.766(4) 1 d PU A 1 H34A H 0.0086 0.6208 0.5133 0.062 Uiso 0.766(4) 1 calc PR A 1 C35 C 0.1079(3) 0.6731(5) 0.5010(3) 0.0410(15) Uani 0.766(4) 1 d PU A 1 H35A H 0.1241 0.7260 0.5078 0.049 Uiso 0.766(4) 1 calc PR A 1 C36 C 0.0985(3) 0.5249(6) 0.5339(3) 0.0546(18) Uani 0.766(4) 1 d PU A 1 H36A H 0.1094 0.4793 0.5614 0.066 Uiso 0.766(4) 1 calc PR A 1 C37 C 0.0406(2) 0.5829(5) 0.4383(2) 0.0483(17) Uani 0.766(4) 1 d PDU A 1 H37A H 0.0298 0.6287 0.4117 0.058 Uiso 0.766(4) 1 calc PR A 1 H37B H 0.0234 0.5323 0.4307 0.058 Uiso 0.766(4) 1 calc PR A 1 C38 C 0.0551(3) 0.5409(7) 0.5464(3) 0.0606(19) Uani 0.766(4) 1 d PU A 1 H38A H 0.0530 0.5589 0.5890 0.073 Uiso 0.766(4) 1 calc PR A 1 H38B H 0.0391 0.4884 0.5404 0.073 Uiso 0.766(4) 1 calc PR A 1 C39 C 0.1242(2) 0.6038(5) 0.5440(3) 0.0466(16) Uani 0.766(4) 1 d PU A 1 H39A H 0.1531 0.5916 0.5363 0.056 Uiso 0.766(4) 1 calc PR A 1 H39B H 0.1226 0.6229 0.5864 0.056 Uiso 0.766(4) 1 calc PR A 1 C40 C 0.1010(2) 0.4953(5) 0.4679(3) 0.0523(17) Uani 0.766(4) 1 d PDU A 1 H40A H 0.0847 0.4431 0.4620 0.063 Uiso 0.766(4) 1 calc PR A 1 H40B H 0.1298 0.4818 0.4598 0.063 Uiso 0.766(4) 1 calc PR A 1 C41 C 0.0627(2) 0.6890(5) 0.5144(3) 0.0502(18) Uani 0.766(4) 1 d PU A 1 H41A H 0.0607 0.7079 0.5567 0.060 Uiso 0.766(4) 1 calc PR A 1 H41B H 0.0515 0.7344 0.4876 0.060 Uiso 0.766(4) 1 calc PR A 1 C42 C 0.11129(19) 0.6435(4) 0.4351(2) 0.0353(14) Uani 0.766(4) 1 d PU A 1 H42A H 0.1402 0.6312 0.4274 0.042 Uiso 0.766(4) 1 calc PR A 1 H42B H 0.1019 0.6892 0.4073 0.042 Uiso 0.766(4) 1 calc PR A 1 C33A C 0.0910(8) 0.562(5) 0.426(3) 0.045(3) Uani 0.234(4) 1 d PDU A 2 C34A C 0.0729(10) 0.517(2) 0.5289(11) 0.051(3) Uani 0.234(4) 1 d PU A 2 H34B H 0.0580 0.4733 0.5517 0.061 Uiso 0.234(4) 1 calc PR A 2 C35A C 0.0815(10) 0.6716(19) 0.5049(10) 0.044(3) Uani 0.234(4) 1 d PU A 2 H35B H 0.0728 0.7312 0.5117 0.052 Uiso 0.234(4) 1 calc PR A 2 C36A C 0.1419(7) 0.5687(16) 0.5131(9) 0.048(3) Uani 0.234(4) 1 d PU A 2 H36B H 0.1713 0.5646 0.5272 0.058 Uiso 0.234(4) 1 calc PR A 2 C37A C 0.0671(8) 0.4971(16) 0.4622(9) 0.048(3) Uani 0.234(4) 1 d PDU A 2 H37C H 0.0377 0.4993 0.4497 0.058 Uiso 0.234(4) 1 calc PR A 2 H37D H 0.0773 0.4395 0.4541 0.058 Uiso 0.234(4) 1 calc PR A 2 C38A C 0.1173(8) 0.5084(19) 0.5454(11) 0.050(3) Uani 0.234(4) 1 d PU A 2 H38C H 0.1218 0.5173 0.5894 0.060 Uiso 0.234(4) 1 calc PR A 2 H38D H 0.1263 0.4504 0.5359 0.060 Uiso 0.234(4) 1 calc PR A 2 C39A C 0.1257(8) 0.6576(18) 0.5233(10) 0.041(3) Uani 0.234(4) 1 d PU A 2 H39C H 0.1297 0.6713 0.5667 0.050 Uiso 0.234(4) 1 calc PR A 2 H39D H 0.1424 0.6977 0.5007 0.050 Uiso 0.234(4) 1 calc PR A 2 C40A C 0.1370(7) 0.5492(16) 0.4443(8) 0.048(3) Uani 0.234(4) 1 d PDU A 2 H40C H 0.1541 0.5878 0.4212 0.058 Uiso 0.234(4) 1 calc PR A 2 H40D H 0.1453 0.4904 0.4361 0.058 Uiso 0.234(4) 1 calc PR A 2 C41A C 0.0538(8) 0.6031(18) 0.5424(10) 0.050(3) Uani 0.234(4) 1 d PU A 2 H41C H 0.0555 0.6152 0.5863 0.060 Uiso 0.234(4) 1 calc PR A 2 H41D H 0.0248 0.6050 0.5279 0.060 Uiso 0.234(4) 1 calc PR A 2 C42A C 0.0766(7) 0.6452(15) 0.4361(8) 0.044(3) Uani 0.234(4) 1 d PU A 2 H42C H 0.0474 0.6486 0.4227 0.053 Uiso 0.234(4) 1 calc PR A 2 H42D H 0.0920 0.6853 0.4115 0.053 Uiso 0.234(4) 1 calc PR A 2 C43 C 0.1132(2) 0.3303(4) 0.2765(2) 0.0664(17) Uani 1 1 d . . . H43A H 0.1245 0.3277 0.2364 0.100 Uiso 1 1 calc R B . H43B H 0.0913 0.2884 0.2791 0.100 Uiso 1 1 calc R . . H43C H 0.1347 0.3183 0.3074 0.100 Uiso 1 1 calc R . . C44 C 0.20106(12) 0.7812(3) 0.35122(16) 0.0304(10) Uani 1 1 d . . . C45 C 0.19812(13) 0.9649(3) 0.37776(18) 0.0342(11) Uani 1 1 d . . . H45A H 0.2084 1.0158 0.3993 0.041 Uiso 1 1 calc R . . H45B H 0.1747 0.9817 0.3506 0.041 Uiso 1 1 calc R . . C46 C 0.18429(13) 0.8998(3) 0.42319(18) 0.0333(11) Uani 1 1 d . . . H46A H 0.1621 0.9245 0.4472 0.040 Uiso 1 1 calc R B . C47 C 0.23187(13) 0.9274(3) 0.34065(18) 0.0336(11) Uani 1 1 d . . . H47A H 0.2408 0.9703 0.3109 0.040 Uiso 1 1 calc R B . C48 C 0.23787(14) 0.7598(3) 0.39476(19) 0.0389(12) Uani 1 1 d . . . H48A H 0.2294 0.7173 0.4245 0.047 Uiso 1 1 calc R . . H48B H 0.2600 0.7348 0.3715 0.047 Uiso 1 1 calc R . . C49 C 0.22044(14) 0.8753(3) 0.46575(18) 0.0412(12) Uani 1 1 d . . . H49A H 0.2116 0.8333 0.4956 0.049 Uiso 1 1 calc R . . H49B H 0.2309 0.9257 0.4879 0.049 Uiso 1 1 calc R . . C50 C 0.25412(14) 0.8378(3) 0.4282(2) 0.0424(13) Uani 1 1 d . . . H50A H 0.2778 0.8213 0.4557 0.051 Uiso 1 1 calc R B . C51 C 0.21552(13) 0.8492(3) 0.30666(17) 0.0299(10) Uani 1 1 d . . . H51A H 0.2373 0.8254 0.2822 0.036 Uiso 1 1 calc R . . H51B H 0.1924 0.8657 0.2789 0.036 Uiso 1 1 calc R . . C52 C 0.26830(13) 0.9030(3) 0.3828(2) 0.0405(12) Uani 1 1 d . . . H52A H 0.2904 0.8790 0.3590 0.049 Uiso 1 1 calc R . . H52B H 0.2791 0.9536 0.4044 0.049 Uiso 1 1 calc R . . C53 C 0.16816(13) 0.8205(3) 0.39026(17) 0.0311(11) Uani 1 1 d . . . H53A H 0.1439 0.8354 0.3642 0.037 Uiso 1 1 calc R . . H53B H 0.1596 0.7785 0.4203 0.037 Uiso 1 1 calc R . . C54 C 0.21313(18) 0.4687(4) 0.3021(2) 0.0569(16) Uani 1 1 d . . . H54A H 0.2092 0.4318 0.2668 0.085 Uiso 1 1 calc R B . H54B H 0.1998 0.4436 0.3366 0.085 Uiso 1 1 calc R . . H54C H 0.2424 0.4753 0.3120 0.085 Uiso 1 1 calc R . . C55 C 0.0258(4) 0.8470(8) 0.3993(5) 0.041(3) Uani 0.50 1 d P B 1 H55A H 0.0292 0.8691 0.4405 0.061 Uiso 0.50 1 calc PR B 1 H55B H 0.0217 0.7858 0.4007 0.061 Uiso 0.50 1 calc PR B 1 H55C H 0.0021 0.8737 0.3787 0.061 Uiso 0.50 1 calc PR B 1 O5 O 0.0620(5) 0.8653(10) 0.3668(5) 0.019(2) Uani 0.50 1 d P B 1 C56 C 0.0725(4) 0.9553(12) 0.3695(6) 0.033(3) Uani 0.50 1 d P B 1 H56A H 0.1001 0.9640 0.3542 0.040 Uiso 0.50 1 calc PR B 1 H56B H 0.0728 0.9749 0.4120 0.040 Uiso 0.50 1 calc PR B 1 C57 C 0.0418(3) 1.0054(5) 0.3323(4) 0.0266(19) Uani 0.50 1 d P B 1 H57A H 0.0154 1.0077 0.3523 0.032 Uiso 0.50 1 calc PR B 1 H57B H 0.0518 1.0637 0.3266 0.032 Uiso 0.50 1 calc PR B 1 O6 O 0.03695(15) 0.9629(3) 0.2748(2) 0.0220(12) Uani 0.50 1 d P B 1 C58 C 0.0000 0.9974(5) 0.2500 0.067(3) Uani 1 2 d S B 1 H58A H 0.0035 1.0580 0.2434 0.100 Uiso 0.50 1 calc PR B 1 H58B H -0.0219 0.9882 0.2780 0.100 Uiso 0.50 1 calc PR B 1 H58C H -0.0072 0.9697 0.2114 0.100 Uiso 0.50 1 calc PR B 1 C55A C 0.0139(3) 1.0270(8) 0.4894(5) 0.064(4) Uani 0.50 1 d P B 2 H55D H 0.0284 1.0788 0.5016 0.095 Uiso 0.50 1 calc PR B 2 H55E H 0.0044 0.9981 0.5253 0.095 Uiso 0.50 1 calc PR B 2 H55F H -0.0096 1.0410 0.4623 0.095 Uiso 0.50 1 calc PR B 2 O5A O 0.0410(2) 0.9729(5) 0.4588(3) 0.063(2) Uani 0.50 1 d P B 2 C56A C 0.0213(3) 0.9001(8) 0.4334(5) 0.049(3) Uani 0.50 1 d P B 2 H56C H -0.0003 0.9169 0.4030 0.058 Uiso 0.50 1 calc PR B 2 H56D H 0.0084 0.8670 0.4654 0.058 Uiso 0.50 1 calc PR B 2 C57A C 0.0535(4) 0.8480(7) 0.4043(5) 0.034(2) Uani 0.50 1 d P B 2 H57C H 0.0775 0.8440 0.4330 0.041 Uiso 0.50 1 calc PR B 2 H57D H 0.0427 0.7902 0.3980 0.041 Uiso 0.50 1 calc PR B 2 O6A O 0.0675(5) 0.8785(12) 0.3471(6) 0.031(3) Uani 0.50 1 d P B 2 C58A C 0.0873(4) 0.9561(12) 0.3513(6) 0.035(3) Uani 0.50 1 d P B 2 H58D H 0.1051 0.9575 0.3881 0.052 Uiso 0.50 1 calc PR B 2 H58E H 0.0670 1.0014 0.3528 0.052 Uiso 0.50 1 calc PR B 2 H58F H 0.1038 0.9641 0.3160 0.052 Uiso 0.50 1 calc PR B 2 C101 C 0.2694(5) 0.0913(9) 0.5438(5) 0.227(6) Uani 1 1 d U . . H10A H 0.2800 0.0374 0.5595 0.341 Uiso 1 1 calc R . . H10B H 0.2401 0.0954 0.5510 0.341 Uiso 1 1 calc R . . H10C H 0.2840 0.1379 0.5643 0.341 Uiso 1 1 calc R . . O102 O 0.2745(3) 0.0954(5) 0.4886(4) 0.183(3) Uani 1 1 d U . . C103 C 0.2947(3) 0.1637(7) 0.4651(5) 0.138(3) Uani 1 1 d U . . H10D H 0.3246 0.1536 0.4691 0.166 Uiso 1 1 calc R . . H10E H 0.2886 0.2147 0.4889 0.166 Uiso 1 1 calc R . . C104 C 0.2823(3) 0.1793(6) 0.3985(4) 0.122(3) Uani 1 1 d U . . H10F H 0.2987 0.2265 0.3833 0.147 Uiso 1 1 calc R . . H10G H 0.2887 0.1283 0.3748 0.147 Uiso 1 1 calc R . . O105 O 0.24162(15) 0.1980(4) 0.3895(2) 0.1004(16) Uani 1 1 d U . . C106 C 0.2292(3) 0.2007(6) 0.3281(3) 0.126(3) Uani 1 1 d U . . H10H H 0.1997 0.2116 0.3241 0.189 Uiso 1 1 calc R . . H10I H 0.2353 0.1465 0.3091 0.189 Uiso 1 1 calc R . . H10J H 0.2440 0.2458 0.3081 0.189 Uiso 1 1 calc R . . O202 O 0.02031(14) 0.2221(3) 0.3092(3) 0.1062(18) Uani 1 1 d . . . C203 C -0.0012(2) 0.2926(4) 0.2835(3) 0.090(2) Uani 1 1 d . . . H20A H 0.0108 0.3455 0.3002 0.108 Uiso 1 1 calc R . . H20B H -0.0302 0.2902 0.2943 0.108 Uiso 1 1 calc R . . C201 C 0.0196(3) 0.2213(7) 0.3741(5) 0.147(4) Uani 1 1 d . . . H20D H 0.0351 0.1725 0.3900 0.221 Uiso 1 1 calc R . . H20E H -0.0087 0.2177 0.3864 0.221 Uiso 1 1 calc R . . H20F H 0.0321 0.2733 0.3903 0.221 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.03382(9) 0.04761(11) 0.01316(7) -0.00258(9) -0.00098(5) -0.01693(10) O1 0.0289(16) 0.0358(19) 0.0168(13) -0.0041(13) 0.0059(12) -0.0050(14) O2 0.0427(19) 0.038(2) 0.0187(14) -0.0039(14) -0.0022(13) -0.0103(16) O3 0.0320(17) 0.038(2) 0.0211(13) -0.0007(14) -0.0043(12) -0.0040(16) O4 0.044(3) 0.019(2) 0.037(2) 0.000 0.0123(19) 0.000 N1 0.053(3) 0.046(3) 0.0167(17) -0.0018(17) -0.0037(17) -0.019(2) C1 0.064(3) 0.042(3) 0.0166(19) -0.010(2) -0.005(2) -0.016(3) C2 0.052(3) 0.045(3) 0.0166(19) -0.004(2) 0.0010(19) -0.011(3) C3 0.034(3) 0.040(3) 0.0158(19) -0.004(2) 0.0025(18) -0.002(2) C4 0.032(3) 0.039(3) 0.022(2) 0.000(2) 0.0054(19) 0.000(2) C5 0.052(3) 0.050(3) 0.026(2) 0.002(2) 0.014(2) -0.002(3) C6 0.069(4) 0.049(3) 0.024(2) -0.007(2) 0.015(2) -0.003(3) C7 0.074(4) 0.044(3) 0.021(2) -0.008(2) 0.004(2) -0.006(3) C8 0.060(3) 0.045(3) 0.019(2) -0.006(2) -0.006(2) -0.020(3) C9 0.050(3) 0.041(3) 0.028(3) -0.006(2) -0.005(2) -0.018(3) C10 0.042(3) 0.040(3) 0.023(2) 0.000(2) -0.004(2) -0.019(2) C11 0.050(3) 0.039(3) 0.024(2) 0.000(2) -0.003(2) -0.012(3) C12 0.064(4) 0.045(4) 0.034(3) 0.003(2) -0.008(2) -0.013(3) C13 0.074(4) 0.036(3) 0.041(3) -0.004(2) -0.005(3) -0.010(3) C14 0.079(4) 0.049(4) 0.027(2) -0.004(2) -0.008(3) -0.020(3) C15 0.058(3) 0.050(3) 0.019(2) -0.006(2) 0.004(2) -0.009(3) C16 0.044(3) 0.045(3) 0.020(2) -0.003(2) 0.007(2) -0.005(3) C17 0.037(2) 0.045(3) 0.0181(18) 0.000(2) 0.0069(17) -0.008(3) C18 0.030(2) 0.045(3) 0.0217(19) -0.006(2) 0.0079(17) 0.000(2) C19 0.034(3) 0.048(4) 0.029(2) -0.004(2) 0.008(2) 0.001(2) C20 0.047(3) 0.035(3) 0.039(3) -0.003(2) 0.015(2) 0.003(3) C21 0.056(3) 0.048(4) 0.028(2) -0.012(2) 0.014(2) -0.009(3) C22 0.026(2) 0.032(3) 0.021(2) 0.0033(19) 0.0031(17) 0.001(2) C23 0.071(4) 0.038(3) 0.040(3) 0.009(2) 0.011(3) -0.021(3) C24 0.122(5) 0.053(4) 0.034(3) 0.015(3) -0.024(3) -0.045(4) C25 0.120(5) 0.025(3) 0.069(4) 0.002(3) 0.055(4) 0.009(3) C26 0.043(3) 0.042(3) 0.031(2) 0.005(2) 0.009(2) -0.002(2) C27 0.103(5) 0.063(4) 0.053(3) 0.013(3) -0.020(3) -0.050(4) C28 0.163(6) 0.039(3) 0.038(3) -0.007(3) 0.035(3) -0.042(4) C29 0.039(3) 0.038(3) 0.046(3) 0.015(2) 0.012(2) 0.014(2) C30 0.129(6) 0.031(3) 0.060(4) 0.009(3) 0.043(4) 0.006(4) C31 0.037(3) 0.039(3) 0.039(3) 0.012(2) -0.008(2) -0.006(2) C32 0.097(5) 0.068(5) 0.029(2) -0.006(3) 0.023(3) 0.003(4) C33 0.035(4) 0.039(4) 0.018(4) 0.001(3) -0.010(4) -0.012(4) C34 0.045(3) 0.086(4) 0.024(3) 0.000(3) 0.000(3) -0.014(3) C35 0.044(4) 0.060(4) 0.018(3) -0.001(3) -0.009(3) -0.011(3) C36 0.064(4) 0.070(4) 0.028(3) 0.011(3) -0.015(3) -0.009(4) C37 0.045(3) 0.077(4) 0.022(3) 0.005(3) -0.005(3) -0.016(3) C38 0.069(4) 0.084(5) 0.027(3) 0.010(4) -0.005(3) -0.020(4) C39 0.046(3) 0.070(4) 0.022(3) 0.004(3) -0.015(3) -0.006(3) C40 0.068(4) 0.058(4) 0.029(3) 0.007(3) -0.014(3) -0.011(4) C41 0.055(4) 0.077(4) 0.018(3) 0.002(3) 0.001(3) 0.002(4) C42 0.037(3) 0.048(4) 0.021(2) -0.001(3) -0.002(2) -0.015(3) C33A 0.051(5) 0.058(5) 0.024(5) 0.001(5) -0.005(5) -0.010(5) C34A 0.056(5) 0.069(5) 0.026(5) 0.008(5) -0.006(5) -0.006(5) C35A 0.049(5) 0.064(5) 0.017(5) -0.003(5) -0.005(5) -0.006(5) C36A 0.052(5) 0.065(5) 0.026(5) 0.004(5) -0.012(5) -0.008(5) C37A 0.055(5) 0.063(6) 0.027(5) 0.004(5) -0.003(5) -0.007(5) C38A 0.054(6) 0.068(6) 0.026(5) 0.004(5) -0.011(5) -0.006(6) C39A 0.046(6) 0.060(6) 0.018(5) -0.003(5) -0.006(5) -0.008(6) C40A 0.054(6) 0.061(6) 0.029(6) 0.000(6) -0.006(6) -0.013(6) C41A 0.056(5) 0.072(5) 0.021(4) 0.004(5) -0.007(4) -0.003(5) C42A 0.048(5) 0.062(5) 0.021(5) -0.002(5) -0.006(5) -0.011(5) C43 0.098(5) 0.051(4) 0.049(3) -0.012(3) -0.004(3) -0.006(4) C44 0.027(2) 0.044(3) 0.0199(18) -0.003(2) -0.0014(16) 0.002(2) C45 0.032(3) 0.043(3) 0.027(2) -0.007(2) -0.0042(19) -0.004(2) C46 0.028(2) 0.048(3) 0.025(2) -0.009(2) 0.0006(19) 0.003(2) C47 0.028(2) 0.047(3) 0.025(2) 0.000(2) 0.0006(19) -0.006(2) C48 0.034(3) 0.051(3) 0.030(2) 0.000(2) -0.006(2) 0.007(2) C49 0.045(3) 0.057(4) 0.021(2) -0.004(2) -0.005(2) -0.002(3) C50 0.032(3) 0.061(4) 0.033(2) -0.003(2) -0.014(2) 0.003(3) C51 0.025(2) 0.042(3) 0.023(2) -0.006(2) 0.0008(18) -0.005(2) C52 0.022(2) 0.059(4) 0.040(3) -0.010(2) -0.006(2) -0.001(2) C53 0.029(2) 0.045(3) 0.020(2) -0.0016(19) 0.0008(18) -0.001(2) C54 0.067(4) 0.050(4) 0.055(3) -0.008(3) 0.019(3) 0.002(3) C55 0.036(6) 0.053(8) 0.034(6) -0.002(5) 0.014(5) -0.006(6) O5 0.024(5) 0.017(7) 0.017(6) -0.001(5) 0.008(5) -0.003(4) C56 0.030(8) 0.037(8) 0.033(7) -0.019(6) 0.000(5) 0.003(7) C57 0.027(5) 0.022(5) 0.031(4) -0.012(4) 0.004(4) 0.008(4) O6 0.018(3) 0.023(3) 0.025(3) -0.003(2) 0.003(2) 0.006(2) C58 0.057(5) 0.032(5) 0.107(7) 0.000 -0.045(5) 0.000 C55A 0.066(9) 0.074(10) 0.052(7) -0.022(7) 0.007(6) 0.027(7) O5A 0.045(4) 0.080(6) 0.064(5) -0.033(5) 0.010(4) 0.013(4) C56A 0.045(7) 0.068(9) 0.034(5) 0.004(6) 0.007(5) -0.007(6) C57A 0.038(7) 0.032(7) 0.032(6) -0.002(5) 0.010(6) -0.008(6) O6A 0.034(6) 0.026(6) 0.033(7) 0.010(6) 0.006(6) -0.010(4) C58A 0.030(8) 0.028(7) 0.044(9) -0.010(7) -0.015(6) 0.003(7) C101 0.379(15) 0.212(12) 0.089(7) -0.017(9) -0.004(10) -0.059(12) O102 0.278(8) 0.152(6) 0.119(5) -0.018(5) 0.011(6) -0.044(6) C103 0.136(6) 0.154(7) 0.126(6) -0.033(6) 0.020(5) -0.019(6) C104 0.096(5) 0.157(6) 0.117(5) -0.030(5) 0.044(5) -0.004(5) O105 0.079(3) 0.142(4) 0.082(3) -0.022(3) 0.019(3) 0.000(3) C106 0.164(8) 0.149(8) 0.066(5) 0.007(5) 0.009(5) -0.022(7) O202 0.067(3) 0.070(4) 0.181(6) 0.011(4) 0.006(4) 0.002(3) C203 0.066(4) 0.046(4) 0.159(7) 0.001(4) 0.019(5) 0.000(4) C201 0.095(7) 0.180(11) 0.166(10) 0.027(10) -0.005(7) 0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O4 2.1036(2) . ? U1 O3 2.175(3) . ? U1 O1 2.218(3) . ? U1 O2 2.224(3) . ? U1 O6A 2.404(18) . ? U1 N1 2.550(4) . ? U1 O5 2.667(13) . ? U1 O6 2.945(5) . ? O1 C3 1.358(4) . ? O2 C10 1.357(6) . ? O3 C17 1.354(6) . ? O4 U1 2.1036(2) 2 ? N1 C8 1.500(6) . ? N1 C15 1.502(6) . ? N1 C1 1.505(5) . ? C1 C2 1.498(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.402(6) . ? C2 C7 1.403(6) . ? C3 C4 1.407(6) . ? C4 C5 1.406(6) . ? C4 C22 1.516(6) . ? C5 C6 1.388(7) . ? C5 H5A 0.9500 . ? C6 C7 1.381(7) . ? C6 C32 1.525(6) . ? C7 H7A 0.9500 . ? C8 C9 1.488(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.387(7) . ? C9 C10 1.408(6) . ? C10 C11 1.420(6) . ? C11 C12 1.389(7) . ? C11 C33 1.52(2) . ? C11 C33A 1.60(8) . ? C12 C13 1.396(7) . ? C12 H12A 0.9500 . ? C13 C14 1.382(7) . ? C13 C43 1.502(8) . ? C14 H14A 0.9500 . ? C15 C16 1.515(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.392(7) . ? C16 C17 1.405(6) . ? C17 C18 1.420(6) . ? C18 C19 1.401(7) . ? C18 C44 1.534(6) . ? C19 C20 1.388(6) . ? C19 H19A 0.9500 . ? C20 C21 1.383(7) . ? C20 C54 1.521(7) . ? C21 H21A 0.9500 . ? C22 C31 1.540(6) . ? C22 C29 1.540(6) . ? C22 C26 1.543(6) . ? C23 C30 1.510(8) . ? C23 C27 1.520(7) . ? C23 C26 1.528(7) . ? C23 H23A 1.0000 . ? C24 C28 1.498(9) . ? C24 C31 1.519(7) . ? C24 C27 1.534(7) . ? C24 H24A 1.0000 . ? C25 C29 1.524(7) . ? C25 C28 1.527(9) . ? C25 C30 1.528(7) . ? C25 H25A 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C37 1.544(14) . ? C33 C40 1.550(10) . ? C33 C42 1.557(18) . ? C34 C41 1.510(10) . ? C34 C38 1.528(11) . ? C34 C37 1.530(8) . ? C34 H34A 1.0000 . ? C35 C39 1.534(10) . ? C35 C42 1.542(8) . ? C35 C41 1.544(10) . ? C35 H35A 1.0000 . ? C36 C38 1.481(12) . ? C36 C39 1.518(11) . ? C36 C40 1.542(9) . ? C36 H36A 1.0000 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C33A C42A 1.41(8) . ? C33A C37A 1.54(2) . ? C33A C40A 1.552(19) . ? C34A C38A 1.49(4) . ? C34A C37A 1.51(3) . ? C34A C41A 1.53(4) . ? C34A H34B 1.0000 . ? C35A C39A 1.50(3) . ? C35A C42A 1.58(3) . ? C35A C41A 1.66(4) . ? C35A H35B 1.0000 . ? C36A C38A 1.46(3) . ? C36A C39A 1.52(4) . ? C36A C40A 1.56(3) . ? C36A H36B 1.0000 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C38A H38C 0.9900 . ? C38A H38D 0.9900 . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C53 1.542(6) . ? C44 C48 1.547(6) . ? C44 C51 1.550(6) . ? C45 C46 1.524(6) . ? C45 C47 1.527(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C49 1.530(6) . ? C46 C53 1.535(6) . ? C46 H46A 1.0000 . ? C47 C52 1.531(6) . ? C47 C51 1.534(6) . ? C47 H47A 1.0000 . ? C48 C50 1.526(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.530(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C52 1.529(7) . ? C50 H50A 1.0000 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 O5 1.442(14) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? O5 C56 1.47(3) . ? C56 C57 1.498(18) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 O6 1.443(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? O6 C58 1.415(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C55A O5A 1.425(12) . ? C55A H55D 0.9800 . ? C55A H55E 0.9800 . ? C55A H55F 0.9800 . ? O5A C56A 1.427(13) . ? C56A C57A 1.508(15) . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? C57A O6A 1.448(12) . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? O6A C58A 1.39(3) . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C101 O102 1.243(11) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? O102 C103 1.382(11) . ? C103 C104 1.534(12) . ? C103 H10D 0.9900 . ? C103 H10E 0.9900 . ? C104 O105 1.370(9) . ? C104 H10F 0.9900 . ? C104 H10G 0.9900 . ? O105 C106 1.405(8) . ? C106 H10H 0.9800 . ? C106 H10I 0.9800 . ? C106 H10J 0.9800 . ? O202 C203 1.427(8) . ? O202 C201 1.439(10) . ? C203 C203 1.491(14) 2 ? C203 H20A 0.9900 . ? C203 H20B 0.9900 . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? C201 H20F 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 O4 U1 O3 173.87(9) . . ? O4 U1 O1 92.41(9) . . ? O3 U1 O1 84.81(10) . . ? O4 U1 O2 89.56(13) . . ? O3 U1 O2 90.38(11) . . ? O1 U1 O2 152.34(10) . . ? O4 U1 O6A 95.5(4) . . ? O3 U1 O6A 90.6(4) . . ? O1 U1 O6A 111.6(3) . . ? O2 U1 O6A 95.6(3) . . ? O4 U1 N1 95.03(12) . . ? O3 U1 N1 78.99(12) . . ? O1 U1 N1 75.67(11) . . ? O2 U1 N1 76.67(11) . . ? O6A U1 N1 166.9(4) . . ? O4 U1 O5 91.7(3) . . ? O3 U1 O5 94.4(3) . . ? O1 U1 O5 121.4(3) . . ? O2 U1 O5 86.0(3) . . ? O6A U1 O5 10.3(5) . . ? N1 U1 O5 161.4(3) . . ? O4 U1 O6 72.88(16) . . ? O3 U1 O6 111.05(13) . . ? O1 U1 O6 69.52(12) . . ? O2 U1 O6 136.78(13) . . ? O6A U1 O6 49.3(4) . . ? N1 U1 O6 142.30(13) . . ? O5 U1 O6 56.3(3) . . ? C3 O1 U1 140.2(3) . . ? C10 O2 U1 140.2(3) . . ? C17 O3 U1 127.5(3) . . ? U1 O4 U1 180.0(2) . 2 ? C8 N1 C15 112.4(4) . . ? C8 N1 C1 105.1(3) . . ? C15 N1 C1 109.9(3) . . ? C8 N1 U1 107.4(3) . . ? C15 N1 U1 113.2(3) . . ? C1 N1 U1 108.5(3) . . ? C2 C1 N1 115.6(4) . . ? C2 C1 H1A 108.4 . . ? N1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? N1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C3 C2 C7 119.8(4) . . ? C3 C2 C1 120.1(4) . . ? C7 C2 C1 120.1(4) . . ? O1 C3 C2 116.7(4) . . ? O1 C3 C4 122.8(4) . . ? C2 C3 C4 120.5(4) . . ? C5 C4 C3 116.8(4) . . ? C5 C4 C22 121.0(4) . . ? C3 C4 C22 122.2(3) . . ? C6 C5 C4 124.0(5) . . ? C6 C5 H5A 118.0 . . ? C4 C5 H5A 118.0 . . ? C7 C6 C5 117.5(4) . . ? C7 C6 C32 122.0(5) . . ? C5 C6 C32 120.5(5) . . ? C6 C7 C2 121.4(5) . . ? C6 C7 H7A 119.3 . . ? C2 C7 H7A 119.3 . . ? C9 C8 N1 115.7(4) . . ? C9 C8 H8A 108.3 . . ? N1 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? N1 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C14 C9 C10 120.3(5) . . ? C14 C9 C8 119.4(4) . . ? C10 C9 C8 120.2(4) . . ? O2 C10 C9 117.4(4) . . ? O2 C10 C11 123.6(4) . . ? C9 C10 C11 119.0(5) . . ? C12 C11 C10 117.4(4) . . ? C12 C11 C33 119.3(7) . . ? C10 C11 C33 123.2(7) . . ? C12 C11 C33A 115(2) . . ? C10 C11 C33A 127(2) . . ? C11 C12 C13 124.2(5) . . ? C11 C12 H12A 117.9 . . ? C13 C12 H12A 117.9 . . ? C14 C13 C12 116.8(5) . . ? C14 C13 C43 122.8(5) . . ? C12 C13 C43 120.4(5) . . ? C13 C14 C9 122.0(5) . . ? C13 C14 H14A 119.0 . . ? C9 C14 H14A 119.0 . . ? N1 C15 C16 118.1(3) . . ? N1 C15 H15A 107.8 . . ? C16 C15 H15A 107.8 . . ? N1 C15 H15B 107.8 . . ? C16 C15 H15B 107.8 . . ? H15A C15 H15B 107.1 . . ? C21 C16 C17 119.7(4) . . ? C21 C16 C15 119.4(4) . . ? C17 C16 C15 120.6(4) . . ? O3 C17 C16 118.1(4) . . ? O3 C17 C18 121.4(4) . . ? C16 C17 C18 120.5(5) . . ? C19 C18 C17 116.0(4) . . ? C19 C18 C44 121.3(4) . . ? C17 C18 C44 122.6(4) . . ? C20 C19 C18 124.2(4) . . ? C20 C19 H19A 117.9 . . ? C18 C19 H19A 117.9 . . ? C21 C20 C19 117.7(5) . . ? C21 C20 C54 120.9(5) . . ? C19 C20 C54 121.4(5) . . ? C20 C21 C16 121.3(4) . . ? C20 C21 H21A 119.3 . . ? C16 C21 H21A 119.3 . . ? C4 C22 C31 109.8(4) . . ? C4 C22 C29 111.0(4) . . ? C31 C22 C29 108.6(4) . . ? C4 C22 C26 113.6(3) . . ? C31 C22 C26 107.0(4) . . ? C29 C22 C26 106.6(4) . . ? C30 C23 C27 110.6(5) . . ? C30 C23 C26 109.9(5) . . ? C27 C23 C26 109.0(5) . . ? C30 C23 H23A 109.1 . . ? C27 C23 H23A 109.1 . . ? C26 C23 H23A 109.1 . . ? C28 C24 C31 109.9(5) . . ? C28 C24 C27 109.9(5) . . ? C31 C24 C27 108.8(5) . . ? C28 C24 H24A 109.4 . . ? C31 C24 H24A 109.4 . . ? C27 C24 H24A 109.4 . . ? C29 C25 C28 109.4(4) . . ? C29 C25 C30 109.0(4) . . ? C28 C25 C30 110.0(6) . . ? C29 C25 H25A 109.5 . . ? C28 C25 H25A 109.5 . . ? C30 C25 H25A 109.5 . . ? C23 C26 C22 111.3(4) . . ? C23 C26 H26A 109.4 . . ? C22 C26 H26A 109.4 . . ? C23 C26 H26B 109.4 . . ? C22 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C23 C27 C24 108.9(5) . . ? C23 C27 H27A 109.9 . . ? C24 C27 H27A 109.9 . . ? C23 C27 H27B 109.9 . . ? C24 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C24 C28 C25 109.9(4) . . ? C24 C28 H28A 109.7 . . ? C25 C28 H28A 109.7 . . ? C24 C28 H28B 109.7 . . ? C25 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C25 C29 C22 111.2(4) . . ? C25 C29 H29A 109.4 . . ? C22 C29 H29A 109.4 . . ? C25 C29 H29B 109.4 . . ? C22 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C23 C30 C25 108.7(5) . . ? C23 C30 H30A 109.9 . . ? C25 C30 H30A 109.9 . . ? C23 C30 H30B 109.9 . . ? C25 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C24 C31 C22 111.4(4) . . ? C24 C31 H31A 109.3 . . ? C22 C31 H31A 109.3 . . ? C24 C31 H31B 109.3 . . ? C22 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C6 C32 H32A 109.5 . . ? C6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C11 C33 C37 109.0(7) . . ? C11 C33 C40 113.3(14) . . ? C37 C33 C40 106.6(7) . . ? C11 C33 C42 113.3(6) . . ? C37 C33 C42 108.0(14) . . ? C40 C33 C42 106.3(8) . . ? C41 C34 C38 108.7(6) . . ? C41 C34 C37 108.4(5) . . ? C38 C34 C37 110.4(7) . . ? C41 C34 H34A 109.8 . . ? C38 C34 H34A 109.8 . . ? C37 C34 H34A 109.8 . . ? C39 C35 C42 109.5(6) . . ? C39 C35 C41 107.9(6) . . ? C42 C35 C41 110.0(6) . . ? C39 C35 H35A 109.8 . . ? C42 C35 H35A 109.8 . . ? C41 C35 H35A 109.8 . . ? C38 C36 C39 111.1(8) . . ? C38 C36 C40 108.8(8) . . ? C39 C36 C40 109.8(6) . . ? C38 C36 H36A 109.0 . . ? C39 C36 H36A 109.0 . . ? C40 C36 H36A 109.0 . . ? C34 C37 C33 112.0(8) . . ? C34 C37 H37A 109.2 . . ? C33 C37 H37A 109.2 . . ? C34 C37 H37B 109.2 . . ? C33 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C36 C38 C34 110.0(6) . . ? C36 C38 H38A 109.7 . . ? C34 C38 H38A 109.7 . . ? C36 C38 H38B 109.7 . . ? C34 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C36 C39 C35 108.8(6) . . ? C36 C39 H39A 109.9 . . ? C35 C39 H39A 109.9 . . ? C36 C39 H39B 109.9 . . ? C35 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C36 C40 C33 112.1(10) . . ? C36 C40 H40A 109.2 . . ? C33 C40 H40A 109.2 . . ? C36 C40 H40B 109.2 . . ? C33 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C34 C41 C35 110.6(7) . . ? C34 C41 H41A 109.5 . . ? C35 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? C35 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C35 C42 C33 111.0(8) . . ? C35 C42 H42A 109.4 . . ? C33 C42 H42A 109.4 . . ? C35 C42 H42B 109.4 . . ? C33 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C42A C33A C37A 111(4) . . ? C42A C33A C40A 114(5) . . ? C37A C33A C40A 107(2) . . ? C42A C33A C11 112(2) . . ? C37A C33A C11 105(5) . . ? C40A C33A C11 106(4) . . ? C38A C34A C37A 107(2) . . ? C38A C34A C41A 116(3) . . ? C37A C34A C41A 110(2) . . ? C38A C34A H34B 107.7 . . ? C37A C34A H34B 107.7 . . ? C41A C34A H34B 107.7 . . ? C39A C35A C42A 106(2) . . ? C39A C35A C41A 108(2) . . ? C42A C35A C41A 106(2) . . ? C39A C35A H35B 112.1 . . ? C42A C35A H35B 112.1 . . ? C41A C35A H35B 112.1 . . ? C38A C36A C39A 109(2) . . ? C38A C36A C40A 108(2) . . ? C39A C36A C40A 107.8(19) . . ? C38A C36A H36B 110.4 . . ? C39A C36A H36B 110.4 . . ? C40A C36A H36B 110.4 . . ? C34A C37A C33A 109(4) . . ? C34A C37A H37C 110.0 . . ? C33A C37A H37C 110.0 . . ? C34A C37A H37D 110.0 . . ? C33A C37A H37D 110.0 . . ? H37C C37A H37D 108.4 . . ? C36A C38A C34A 112(2) . . ? C36A C38A H38C 109.2 . . ? C34A C38A H38C 109.2 . . ? C36A C38A H38D 109.2 . . ? C34A C38A H38D 109.2 . . ? H38C C38A H38D 107.9 . . ? C35A C39A C36A 116(2) . . ? C35A C39A H39C 108.4 . . ? C36A C39A H39C 108.4 . . ? C35A C39A H39D 108.4 . . ? C36A C39A H39D 108.4 . . ? H39C C39A H39D 107.4 . . ? C33A C40A C36A 106(3) . . ? C33A C40A H40C 110.5 . . ? C36A C40A H40C 110.5 . . ? C33A C40A H40D 110.5 . . ? C36A C40A H40D 110.5 . . ? H40C C40A H40D 108.6 . . ? C34A C41A C35A 104(2) . . ? C34A C41A H41C 110.9 . . ? C35A C41A H41C 110.9 . . ? C34A C41A H41D 110.9 . . ? C35A C41A H41D 110.9 . . ? H41C C41A H41D 108.9 . . ? C33A C42A C35A 112(3) . . ? C33A C42A H42C 109.2 . . ? C35A C42A H42C 109.2 . . ? C33A C42A H42D 109.2 . . ? C35A C42A H42D 109.2 . . ? H42C C42A H42D 107.9 . . ? C13 C43 H43A 109.5 . . ? C13 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C13 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C18 C44 C53 112.8(3) . . ? C18 C44 C48 112.3(4) . . ? C53 C44 C48 106.4(3) . . ? C18 C44 C51 109.2(3) . . ? C53 C44 C51 108.5(4) . . ? C48 C44 C51 107.3(3) . . ? C46 C45 C47 109.6(4) . . ? C46 C45 H45A 109.7 . . ? C47 C45 H45A 109.7 . . ? C46 C45 H45B 109.7 . . ? C47 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C45 C46 C49 109.5(4) . . ? C45 C46 C53 110.3(3) . . ? C49 C46 C53 109.0(4) . . ? C45 C46 H46A 109.3 . . ? C49 C46 H46A 109.3 . . ? C53 C46 H46A 109.3 . . ? C45 C47 C52 109.4(3) . . ? C45 C47 C51 109.5(4) . . ? C52 C47 C51 109.9(4) . . ? C45 C47 H47A 109.3 . . ? C52 C47 H47A 109.3 . . ? C51 C47 H47A 109.3 . . ? C50 C48 C44 111.7(4) . . ? C50 C48 H48A 109.3 . . ? C44 C48 H48A 109.3 . . ? C50 C48 H48B 109.3 . . ? C44 C48 H48B 109.3 . . ? H48A C48 H48B 107.9 . . ? C46 C49 C50 108.6(3) . . ? C46 C49 H49A 110.0 . . ? C50 C49 H49A 110.0 . . ? C46 C49 H49B 110.0 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 108.3 . . ? C48 C50 C52 109.7(4) . . ? C48 C50 C49 109.5(4) . . ? C52 C50 C49 110.1(4) . . ? C48 C50 H50A 109.2 . . ? C52 C50 H50A 109.2 . . ? C49 C50 H50A 109.2 . . ? C47 C51 C44 111.0(3) . . ? C47 C51 H51A 109.4 . . ? C44 C51 H51A 109.4 . . ? C47 C51 H51B 109.4 . . ? C44 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C50 C52 C47 108.7(4) . . ? C50 C52 H52A 109.9 . . ? C47 C52 H52A 109.9 . . ? C50 C52 H52B 109.9 . . ? C47 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C46 C53 C44 111.3(4) . . ? C46 C53 H53A 109.4 . . ? C44 C53 H53A 109.4 . . ? C46 C53 H53B 109.4 . . ? C44 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C20 C54 H54A 109.5 . . ? C20 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C20 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C55 O5 C56 111.7(11) . . ? C55 O5 U1 113.8(10) . . ? C56 O5 U1 118.1(7) . . ? O5 C56 C57 110.0(12) . . ? O5 C56 H56A 109.7 . . ? C57 C56 H56A 109.7 . . ? O5 C56 H56B 109.7 . . ? C57 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? O6 C57 C56 106.6(8) . . ? O6 C57 H57A 110.4 . . ? C56 C57 H57A 110.4 . . ? O6 C57 H57B 110.4 . . ? C56 C57 H57B 110.4 . . ? H57A C57 H57B 108.6 . . ? C58 O6 C57 102.8(5) . . ? C58 O6 U1 125.5(4) . . ? C57 O6 U1 120.9(4) . . ? O5A C55A H55D 109.5 . . ? O5A C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? O5A C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? C55A O5A C56A 113.1(8) . . ? O5A C56A C57A 107.2(9) . . ? O5A C56A H56C 110.3 . . ? C57A C56A H56C 110.3 . . ? O5A C56A H56D 110.3 . . ? C57A C56A H56D 110.3 . . ? H56C C56A H56D 108.5 . . ? O6A C57A C56A 116.5(13) . . ? O6A C57A H57C 108.2 . . ? C56A C57A H57C 108.2 . . ? O6A C57A H57D 108.2 . . ? C56A C57A H57D 108.2 . . ? H57C C57A H57D 107.3 . . ? C58A O6A C57A 113.6(15) . . ? C58A O6A U1 126.1(8) . . ? C57A O6A U1 119.6(12) . . ? O6A C58A H58D 109.5 . . ? O6A C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? O6A C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? O102 C101 H10A 109.5 . . ? O102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? O102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C101 O102 C103 119.9(11) . . ? O102 C103 C104 112.2(9) . . ? O102 C103 H10D 109.2 . . ? C104 C103 H10D 109.2 . . ? O102 C103 H10E 109.2 . . ? C104 C103 H10E 109.2 . . ? H10D C103 H10E 107.9 . . ? O105 C104 C103 112.9(7) . . ? O105 C104 H10F 109.0 . . ? C103 C104 H10F 109.0 . . ? O105 C104 H10G 109.0 . . ? C103 C104 H10G 109.0 . . ? H10F C104 H10G 107.8 . . ? C104 O105 C106 112.6(6) . . ? O105 C106 H10H 109.5 . . ? O105 C106 H10I 109.5 . . ? H10H C106 H10I 109.5 . . ? O105 C106 H10J 109.5 . . ? H10H C106 H10J 109.5 . . ? H10I C106 H10J 109.5 . . ? C203 O202 C201 112.1(7) . . ? O202 C203 C203 110.5(5) . 2 ? O202 C203 H20A 109.5 . . ? C203 C203 H20A 109.5 2 . ? O202 C203 H20B 109.5 . . ? C203 C203 H20B 109.5 2 . ? H20A C203 H20B 108.1 . . ? O202 C201 H20D 109.5 . . ? O202 C201 H20E 109.5 . . ? H20D C201 H20E 109.5 . . ? O202 C201 H20F 109.5 . . ? H20D C201 H20F 109.5 . . ? H20E C201 H20F 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 O4 U1 O1 C3 -115.1(4) . . . . ? O3 U1 O1 C3 59.4(4) . . . . ? O2 U1 O1 C3 -21.5(5) . . . . ? O6A U1 O1 C3 148.0(6) . . . . ? N1 U1 O1 C3 -20.6(4) . . . . ? O5 U1 O1 C3 151.4(5) . . . . ? O6 U1 O1 C3 174.2(4) . . . . ? O4 U1 O2 C10 110.8(4) . . . . ? O3 U1 O2 C10 -63.1(4) . . . . ? O1 U1 O2 C10 16.4(5) . . . . ? O6A U1 O2 C10 -153.7(6) . . . . ? N1 U1 O2 C10 15.5(4) . . . . ? O5 U1 O2 C10 -157.4(5) . . . . ? O6 U1 O2 C10 174.8(4) . . . . ? O1 U1 O3 C17 -128.9(3) . . . . ? O2 U1 O3 C17 23.8(3) . . . . ? O6A U1 O3 C17 119.4(4) . . . . ? N1 U1 O3 C17 -52.5(3) . . . . ? O5 U1 O3 C17 109.9(4) . . . . ? O6 U1 O3 C17 165.4(3) . . . . ? O4 U1 N1 C8 -54.8(3) . . . . ? O3 U1 N1 C8 126.6(3) . . . . ? O1 U1 N1 C8 -146.0(3) . . . . ? O2 U1 N1 C8 33.6(3) . . . . ? O6A U1 N1 C8 88.5(14) . . . . ? O5 U1 N1 C8 56.0(11) . . . . ? O6 U1 N1 C8 -123.1(3) . . . . ? O4 U1 N1 C15 -179.4(3) . . . . ? O3 U1 N1 C15 2.0(3) . . . . ? O1 U1 N1 C15 89.4(3) . . . . ? O2 U1 N1 C15 -91.1(3) . . . . ? O6A U1 N1 C15 -36.1(15) . . . . ? O5 U1 N1 C15 -68.6(11) . . . . ? O6 U1 N1 C15 112.3(3) . . . . ? O4 U1 N1 C1 58.3(3) . . . . ? O3 U1 N1 C1 -120.3(3) . . . . ? O1 U1 N1 C1 -32.9(3) . . . . ? O2 U1 N1 C1 146.6(3) . . . . ? O6A U1 N1 C1 -158.4(14) . . . . ? O5 U1 N1 C1 169.1(10) . . . . ? O6 U1 N1 C1 -10.0(4) . . . . ? C8 N1 C1 C2 -172.0(4) . . . . ? C15 N1 C1 C2 -50.8(5) . . . . ? U1 N1 C1 C2 73.4(4) . . . . ? N1 C1 C2 C3 -59.1(6) . . . . ? N1 C1 C2 C7 120.9(5) . . . . ? U1 O1 C3 C2 42.1(6) . . . . ? U1 O1 C3 C4 -138.0(4) . . . . ? C7 C2 C3 O1 178.2(4) . . . . ? C1 C2 C3 O1 -1.7(6) . . . . ? C7 C2 C3 C4 -1.7(7) . . . . ? C1 C2 C3 C4 178.4(4) . . . . ? O1 C3 C4 C5 -178.0(4) . . . . ? C2 C3 C4 C5 1.9(7) . . . . ? O1 C3 C4 C22 4.7(7) . . . . ? C2 C3 C4 C22 -175.4(4) . . . . ? C3 C4 C5 C6 -1.3(7) . . . . ? C22 C4 C5 C6 175.9(5) . . . . ? C4 C5 C6 C7 0.5(8) . . . . ? C4 C5 C6 C32 -178.9(5) . . . . ? C5 C6 C7 C2 -0.3(8) . . . . ? C32 C6 C7 C2 179.2(5) . . . . ? C3 C2 C7 C6 0.8(8) . . . . ? C1 C2 C7 C6 -179.2(5) . . . . ? C15 N1 C8 C9 50.7(5) . . . . ? C1 N1 C8 C9 170.2(4) . . . . ? U1 N1 C8 C9 -74.4(5) . . . . ? N1 C8 C9 C14 -114.7(5) . . . . ? N1 C8 C9 C10 63.1(6) . . . . ? U1 O2 C10 C9 -34.0(7) . . . . ? U1 O2 C10 C11 145.0(4) . . . . ? C14 C9 C10 O2 174.1(4) . . . . ? C8 C9 C10 O2 -3.8(7) . . . . ? C14 C9 C10 C11 -4.9(7) . . . . ? C8 C9 C10 C11 177.2(4) . . . . ? O2 C10 C11 C12 -172.5(4) . . . . ? C9 C10 C11 C12 6.4(7) . . . . ? O2 C10 C11 C33 10.5(8) . . . . ? C9 C10 C11 C33 -170.6(5) . . . . ? O2 C10 C11 C33A 3.0(13) . . . . ? C9 C10 C11 C33A -178.1(12) . . . . ? C10 C11 C12 C13 -3.4(8) . . . . ? C33 C11 C12 C13 173.7(5) . . . . ? C33A C11 C12 C13 -179.5(11) . . . . ? C11 C12 C13 C14 -1.2(8) . . . . ? C11 C12 C13 C43 176.6(5) . . . . ? C12 C13 C14 C9 2.9(8) . . . . ? C43 C13 C14 C9 -174.9(5) . . . . ? C10 C9 C14 C13 0.2(8) . . . . ? C8 C9 C14 C13 178.0(5) . . . . ? C8 N1 C15 C16 -77.9(5) . . . . ? C1 N1 C15 C16 165.4(4) . . . . ? U1 N1 C15 C16 43.9(5) . . . . ? N1 C15 C16 C21 122.3(5) . . . . ? N1 C15 C16 C17 -64.0(6) . . . . ? U1 O3 C17 C16 54.1(5) . . . . ? U1 O3 C17 C18 -125.5(4) . . . . ? C21 C16 C17 O3 -173.6(4) . . . . ? C15 C16 C17 O3 12.8(6) . . . . ? C21 C16 C17 C18 6.0(6) . . . . ? C15 C16 C17 C18 -167.6(4) . . . . ? O3 C17 C18 C19 171.1(4) . . . . ? C16 C17 C18 C19 -8.5(6) . . . . ? O3 C17 C18 C44 -12.7(6) . . . . ? C16 C17 C18 C44 167.7(4) . . . . ? C17 C18 C19 C20 4.4(6) . . . . ? C44 C18 C19 C20 -171.8(4) . . . . ? C18 C19 C20 C21 2.4(7) . . . . ? C18 C19 C20 C54 -176.2(4) . . . . ? C19 C20 C21 C16 -5.3(7) . . . . ? C54 C20 C21 C16 173.2(4) . . . . ? C17 C16 C21 C20 1.2(7) . . . . ? C15 C16 C21 C20 174.9(4) . . . . ? C5 C4 C22 C31 -115.7(5) . . . . ? C3 C4 C22 C31 61.4(5) . . . . ? C5 C4 C22 C29 124.2(4) . . . . ? C3 C4 C22 C29 -58.7(5) . . . . ? C5 C4 C22 C26 4.1(6) . . . . ? C3 C4 C22 C26 -178.8(4) . . . . ? C30 C23 C26 C22 -60.5(5) . . . . ? C27 C23 C26 C22 60.8(6) . . . . ? C4 C22 C26 C23 -179.6(4) . . . . ? C31 C22 C26 C23 -58.2(5) . . . . ? C29 C22 C26 C23 57.8(5) . . . . ? C30 C23 C27 C24 59.9(7) . . . . ? C26 C23 C27 C24 -60.9(6) . . . . ? C28 C24 C27 C23 -59.2(6) . . . . ? C31 C24 C27 C23 61.2(7) . . . . ? C31 C24 C28 C25 -60.5(6) . . . . ? C27 C24 C28 C25 59.3(6) . . . . ? C29 C25 C28 C24 60.2(6) . . . . ? C30 C25 C28 C24 -59.5(6) . . . . ? C28 C25 C29 C22 -58.6(6) . . . . ? C30 C25 C29 C22 61.8(6) . . . . ? C4 C22 C29 C25 176.9(4) . . . . ? C31 C22 C29 C25 56.1(5) . . . . ? C26 C22 C29 C25 -58.9(5) . . . . ? C27 C23 C30 C25 -60.0(6) . . . . ? C26 C23 C30 C25 60.4(6) . . . . ? C29 C25 C30 C23 -60.9(7) . . . . ? C28 C25 C30 C23 59.1(6) . . . . ? C28 C24 C31 C22 59.2(5) . . . . ? C27 C24 C31 C22 -61.2(7) . . . . ? C4 C22 C31 C24 -177.6(4) . . . . ? C29 C22 C31 C24 -56.1(5) . . . . ? C26 C22 C31 C24 58.6(5) . . . . ? C12 C11 C33 C37 -117.3(8) . . . . ? C10 C11 C33 C37 59.6(10) . . . . ? C33A C11 C33 C37 -177(20) . . . . ? C12 C11 C33 C40 1.2(8) . . . . ? C10 C11 C33 C40 178.1(5) . . . . ? C33A C11 C33 C40 -58(19) . . . . ? C12 C11 C33 C42 122.4(8) . . . . ? C10 C11 C33 C42 -60.7(9) . . . . ? C33A C11 C33 C42 63(19) . . . . ? C41 C34 C37 C33 61.3(10) . . . . ? C38 C34 C37 C33 -57.7(9) . . . . ? C11 C33 C37 C34 178.0(7) . . . . ? C40 C33 C37 C34 55.4(14) . . . . ? C42 C33 C37 C34 -58.5(8) . . . . ? C39 C36 C38 C34 60.5(9) . . . . ? C40 C36 C38 C34 -60.5(10) . . . . ? C41 C34 C38 C36 -59.3(9) . . . . ? C37 C34 C38 C36 59.5(9) . . . . ? C38 C36 C39 C35 -60.8(8) . . . . ? C40 C36 C39 C35 59.6(9) . . . . ? C42 C35 C39 C36 -60.8(8) . . . . ? C41 C35 C39 C36 58.9(8) . . . . ? C38 C36 C40 C33 61.6(9) . . . . ? C39 C36 C40 C33 -60.1(9) . . . . ? C11 C33 C40 C36 -177.3(6) . . . . ? C37 C33 C40 C36 -57.4(13) . . . . ? C42 C33 C40 C36 57.7(12) . . . . ? C38 C34 C41 C35 59.8(7) . . . . ? C37 C34 C41 C35 -60.3(7) . . . . ? C39 C35 C41 C34 -60.3(7) . . . . ? C42 C35 C41 C34 59.1(7) . . . . ? C39 C35 C42 C33 61.6(9) . . . . ? C41 C35 C42 C33 -56.8(8) . . . . ? C11 C33 C42 C35 176.6(7) . . . . ? C37 C33 C42 C35 55.8(8) . . . . ? C40 C33 C42 C35 -58.3(12) . . . . ? C12 C11 C33A C42A -179.3(15) . . . . ? C10 C11 C33A C42A 5(2) . . . . ? C33 C11 C33A C42A -55(19) . . . . ? C12 C11 C33A C37A -58(3) . . . . ? C10 C11 C33A C37A 127(3) . . . . ? C33 C11 C33A C37A 66(18) . . . . ? C12 C11 C33A C40A 55(3) . . . . ? C10 C11 C33A C40A -121(3) . . . . ? C38A C34A C37A C33A -62(3) . . . . ? C41A C34A C37A C33A 65(4) . . . . ? C42A C33A C37A C34A -61(4) . . . . ? C40A C33A C37A C34A 65(6) . . . . ? C11 C33A C37A C34A 177(2) . . . . ? C39A C36A C38A C34A 54(3) . . . . ? C40A C36A C38A C34A -63(3) . . . . ? C37A C34A C38A C36A 63(3) . . . . ? C41A C34A C38A C36A -61(3) . . . . ? C42A C35A C39A C36A -56(3) . . . . ? C41A C35A C39A C36A 57(3) . . . . ? C38A C36A C39A C35A -57(3) . . . . ? C40A C36A C39A C35A 60(3) . . . . ? C42A C33A C40A C36A 61(3) . . . . ? C37A C33A C40A C36A -63(6) . . . . ? C11 C33A C40A C36A -175(2) . . . . ? C38A C36A C40A C33A 62(3) . . . . ? C39A C36A C40A C33A -56(3) . . . . ? C38A C34A C41A C35A 57(3) . . . . ? C37A C34A C41A C35A -65(3) . . . . ? C39A C35A C41A C34A -53(2) . . . . ? C42A C35A C41A C34A 60(2) . . . . ? C37A C33A C42A C35A 61(4) . . . . ? C40A C33A C42A C35A -60(4) . . . . ? C11 C33A C42A C35A 178.6(18) . . . . ? C39A C35A C42A C33A 54(3) . . . . ? C41A C35A C42A C33A -61(3) . . . . ? C19 C18 C44 C53 -119.4(4) . . . . ? C17 C18 C44 C53 64.6(5) . . . . ? C19 C18 C44 C48 0.9(5) . . . . ? C17 C18 C44 C48 -175.1(4) . . . . ? C19 C18 C44 C51 119.8(4) . . . . ? C17 C18 C44 C51 -56.2(5) . . . . ? C47 C45 C46 C49 60.5(5) . . . . ? C47 C45 C46 C53 -59.5(4) . . . . ? C46 C45 C47 C52 -60.4(5) . . . . ? C46 C45 C47 C51 60.1(4) . . . . ? C18 C44 C48 C50 177.7(3) . . . . ? C53 C44 C48 C50 -58.4(5) . . . . ? C51 C44 C48 C50 57.7(5) . . . . ? C45 C46 C49 C50 -60.0(5) . . . . ? C53 C46 C49 C50 60.7(5) . . . . ? C44 C48 C50 C52 -60.4(5) . . . . ? C44 C48 C50 C49 60.6(5) . . . . ? C46 C49 C50 C48 -60.2(5) . . . . ? C46 C49 C50 C52 60.5(5) . . . . ? C45 C47 C51 C44 -59.9(5) . . . . ? C52 C47 C51 C44 60.3(5) . . . . ? C18 C44 C51 C47 -179.4(3) . . . . ? C53 C44 C51 C47 57.3(4) . . . . ? C48 C44 C51 C47 -57.4(5) . . . . ? C48 C50 C52 C47 60.1(5) . . . . ? C49 C50 C52 C47 -60.6(5) . . . . ? C45 C47 C52 C50 60.0(5) . . . . ? C51 C47 C52 C50 -60.3(5) . . . . ? C45 C46 C53 C44 58.4(5) . . . . ? C49 C46 C53 C44 -61.9(4) . . . . ? C18 C44 C53 C46 -177.4(4) . . . . ? C48 C44 C53 C46 59.0(5) . . . . ? C51 C44 C53 C46 -56.3(4) . . . . ? O4 U1 O5 C55 29.5(10) . . . . ? O3 U1 O5 C55 -150.0(9) . . . . ? O1 U1 O5 C55 123.4(9) . . . . ? O2 U1 O5 C55 -59.9(9) . . . . ? O6A U1 O5 C55 141(5) . . . . ? N1 U1 O5 C55 -81.8(15) . . . . ? O6 U1 O5 C55 97.5(10) . . . . ? O4 U1 O5 C56 -104.5(11) . . . . ? O3 U1 O5 C56 76.0(11) . . . . ? O1 U1 O5 C56 -10.6(12) . . . . ? O2 U1 O5 C56 166.1(11) . . . . ? O6A U1 O5 C56 7(3) . . . . ? N1 U1 O5 C56 144.2(8) . . . . ? O6 U1 O5 C56 -36.4(9) . . . . ? C55 O5 C56 C57 -70.6(13) . . . . ? U1 O5 C56 C57 64.2(11) . . . . ? O5 C56 C57 O6 -47.9(10) . . . . ? C56 C57 O6 C58 163.2(8) . . . . ? C56 C57 O6 U1 17.0(9) . . . . ? O4 U1 O6 C58 -25.2(3) . . . . ? O3 U1 O6 C58 149.8(3) . . . . ? O1 U1 O6 C58 74.1(3) . . . . ? O2 U1 O6 C58 -95.4(4) . . . . ? O6A U1 O6 C58 -138.7(6) . . . . ? N1 U1 O6 C58 50.4(5) . . . . ? O5 U1 O6 C58 -129.3(5) . . . . ? O4 U1 O6 C57 112.9(5) . . . . ? O3 U1 O6 C57 -72.1(5) . . . . ? O1 U1 O6 C57 -147.8(5) . . . . ? O2 U1 O6 C57 42.7(6) . . . . ? O6A U1 O6 C57 -0.6(7) . . . . ? N1 U1 O6 C57 -171.5(5) . . . . ? O5 U1 O6 C57 8.8(6) . . . . ? C55A O5A C56A C57A -178.5(9) . . . . ? O5A C56A C57A O6A -75.6(15) . . . . ? C56A C57A O6A C58A 64(2) . . . . ? C56A C57A O6A U1 -124.8(11) . . . . ? O4 U1 O6A C58A -120.8(15) . . . . ? O3 U1 O6A C58A 58.7(15) . . . . ? O1 U1 O6A C58A -26.0(16) . . . . ? O2 U1 O6A C58A 149.2(15) . . . . ? N1 U1 O6A C58A 96.0(18) . . . . ? O5 U1 O6A C58A 170(5) . . . . ? O6 U1 O6A C58A -59.0(13) . . . . ? O4 U1 O6A C57A 69.5(14) . . . . ? O3 U1 O6A C57A -111.1(14) . . . . ? O1 U1 O6A C57A 164.3(12) . . . . ? O2 U1 O6A C57A -20.6(14) . . . . ? N1 U1 O6A C57A -74(2) . . . . ? O5 U1 O6A C57A 1(3) . . . . ? O6 U1 O6A C57A 131.2(16) . . . . ? C101 O102 C103 C104 -154.6(12) . . . . ? O102 C103 C104 O105 61.9(12) . . . . ? C103 C104 O105 C106 -171.8(8) . . . . ? C201 O202 C203 C203 178.3(7) . . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.413 _refine_diff_density_min -1.596 _refine_diff_density_rms 0.119 #===END OF ALL DATA