data_sas189_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C278 H279 N3 O88 U8' _chemical_formula_weight 6974.28 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 24.8284(13) _cell_length_b 40.177(2) _cell_length_c 41.4124(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 41310(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9226 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 24.14 _exptl_crystal_description Needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13632 _exptl_absorpt_coefficient_mu 3.183 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 97093 _diffrn_reflns_av_R_equivalents 0.1530 _diffrn_reflns_av_sigmaI/netI 0.1519 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 24.37 _reflns_number_total 16698 _reflns_number_gt 7947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SIR2008' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16698 _refine_ls_number_parameters 839 _refine_ls_number_restraints 1489 _refine_ls_R_factor_all 0.2838 _refine_ls_R_factor_gt 0.1564 _refine_ls_wR_factor_ref 0.4272 _refine_ls_wR_factor_gt 0.3850 _refine_ls_goodness_of_fit_ref 2.240 _refine_ls_restrained_S_all 2.157 _refine_ls_shift/su_max 0.063 _refine_ls_shift/su_mean 0.001 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 -0.020 -0.003 18463 10265 ' ' _platon_squeeze_details ; ; 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 0.64960(3) 0.43859(2) 0.15295(2) 0.0488(3) Uani 1 1 d . . . U2 U 0.50347(5) 0.32545(3) 0.0000 0.0410(3) Uani 1 2 d S . . U3 U 0.18512(5) 0.43373(3) 0.0000 0.0505(4) Uani 1 2 d S . . O1U1 O 0.6825(5) 0.4292(3) 0.1879(3) 0.052(4) Uani 1 1 d U . . O1U2 O 0.5037(8) 0.2807(4) 0.0000 0.038(5) Uani 1 2 d SU . . O2U1 O 0.6153(6) 0.4491(3) 0.1172(4) 0.060(5) Uani 1 1 d U . . O2U2 O 0.5030(7) 0.3709(5) 0.0000 0.044(5) Uani 1 2 d SU . . O1U3 O 0.1125(9) 0.4195(5) 0.0000 0.072(7) Uani 1 2 d SU . . O2U3 O 0.2564(8) 0.4465(4) 0.0000 0.044(6) Uani 1 2 d SU . . C1 C 0.3872(8) 0.3996(5) 0.2422(5) 0.048(2) Uani 1 1 d U . . H1A H 0.4039 0.4169 0.2560 0.057 Uiso 1 1 calc R . . H1B H 0.3694 0.3832 0.2566 0.057 Uiso 1 1 calc R . . C2 C 0.4311(4) 0.3820(3) 0.2227(2) 0.047(2) Uani 1 1 d GU . . C3 C 0.4734(5) 0.4008(3) 0.2104(3) 0.048(2) Uani 1 1 d GU . . H3 H 0.4779 0.4233 0.2169 0.057 Uiso 1 1 calc R . . C4 C 0.5092(4) 0.3867(3) 0.1885(3) 0.047(2) Uani 1 1 d GU . . C5 C 0.5027(5) 0.3537(3) 0.1790(3) 0.046(2) Uani 1 1 d GU . . H5 H 0.5272 0.3441 0.1641 0.056 Uiso 1 1 calc R . . C6 C 0.4604(6) 0.3350(3) 0.1913(3) 0.048(2) Uani 1 1 d GU . . C7 C 0.4246(5) 0.3491(3) 0.2132(3) 0.053(2) Uani 1 1 d GU . . C8 C 0.5552(9) 0.4035(5) 0.1760(5) 0.049(2) Uani 1 1 d U . . C9 C 0.3884(11) 0.3198(3) 0.2575(3) 0.085(3) Uani 1 1 d DU . . H9A H 0.3549 0.3258 0.2691 0.103 Uiso 1 1 calc R . . H9B H 0.4179 0.3331 0.2671 0.103 Uiso 1 1 calc R . . C10 C 0.4001(12) 0.2831(3) 0.2647(3) 0.100(3) Uani 1 1 d DU . . H10A H 0.4369 0.2765 0.2580 0.120 Uiso 1 1 calc R . . H10B H 0.3734 0.2681 0.2545 0.120 Uiso 1 1 calc R . . C11 C 0.3941(13) 0.2839(8) 0.3016(3) 0.110(5) Uani 1 1 d DU . . H11A H 0.4190 0.3004 0.3107 0.165 Uiso 1 1 calc R . . H11B H 0.4025 0.2619 0.3105 0.165 Uiso 1 1 calc R . . H11C H 0.3570 0.2899 0.3073 0.165 Uiso 1 1 calc R . . C12 C 0.4503(8) 0.2978(5) 0.1785(5) 0.045(2) Uani 1 1 d U . . H12A H 0.4852 0.2862 0.1758 0.054 Uiso 1 1 calc R . . H12B H 0.4287 0.2853 0.1945 0.054 Uiso 1 1 calc R . . C13 C 0.4198(4) 0.2989(3) 0.1454(2) 0.045(2) Uani 1 1 d GU . . C14 C 0.4464(4) 0.3096(3) 0.1178(3) 0.044(2) Uani 1 1 d GU . . H14 H 0.4843 0.3130 0.1182 0.053 Uiso 1 1 calc R . . C15 C 0.4176(5) 0.3152(3) 0.0895(2) 0.043(2) Uani 1 1 d GU . . C16 C 0.3623(5) 0.3102(3) 0.0889(2) 0.042(2) Uani 1 1 d GU . . H16 H 0.3426 0.3141 0.0696 0.051 Uiso 1 1 calc R . . C17 C 0.3357(4) 0.2995(4) 0.1165(3) 0.044(2) Uani 1 1 d GU . . C18 C 0.3645(4) 0.2938(3) 0.1448(2) 0.046(2) Uani 1 1 d GU . . C19 C 0.4467(8) 0.3195(5) 0.0585(5) 0.043(2) Uani 1 1 d U . . C20 C 0.3523(6) 0.2431(2) 0.1753(4) 0.062(3) Uani 1 1 d DU . . H20A H 0.3453 0.2372 0.1981 0.074 Uiso 1 1 calc R . . H20B H 0.3912 0.2395 0.1712 0.074 Uiso 1 1 calc R . . C21 C 0.3196(4) 0.2195(5) 0.1534(4) 0.072(3) Uani 1 1 d DU . . H21A H 0.3221 0.2276 0.1309 0.086 Uiso 1 1 calc R . . H21B H 0.3363 0.1971 0.1541 0.086 Uiso 1 1 calc R . . C22 C 0.2597(5) 0.2162(7) 0.1624(6) 0.085(5) Uani 1 1 d DU . . H22A H 0.2438 0.1975 0.1506 0.127 Uiso 1 1 calc R . . H22B H 0.2407 0.2367 0.1567 0.127 Uiso 1 1 calc R . . H22C H 0.2564 0.2122 0.1857 0.127 Uiso 1 1 calc R . . C23 C 0.2753(8) 0.2975(5) 0.1153(5) 0.045(2) Uani 1 1 d U . . H23A H 0.2626 0.2834 0.1334 0.054 Uiso 1 1 calc R . . H23B H 0.2645 0.2865 0.0949 0.054 Uiso 1 1 calc R . . C24 C 0.2470(4) 0.3323(2) 0.1175(2) 0.047(2) Uani 1 1 d GU . . C25 C 0.2362(5) 0.3490(3) 0.0889(2) 0.049(2) Uani 1 1 d GU . . H25 H 0.2435 0.3387 0.0687 0.058 Uiso 1 1 calc R . . C26 C 0.2147(6) 0.3810(3) 0.0897(2) 0.051(2) Uani 1 1 d GU . . C27 C 0.2040(5) 0.3961(2) 0.1192(3) 0.050(2) Uani 1 1 d GU . . H27 H 0.1893 0.4179 0.1197 0.060 Uiso 1 1 calc R . . C28 C 0.2148(6) 0.3794(3) 0.1478(2) 0.047(2) Uani 1 1 d GDU . . C29 C 0.2363(5) 0.3474(3) 0.1470(2) 0.048(2) Uani 1 1 d GU . . C30 C 0.2013(9) 0.4001(6) 0.0602(5) 0.054(2) Uani 1 1 d U . . C31 C 0.2109(4) 0.3143(4) 0.1894(3) 0.061(3) Uani 1 1 d DU . . H31A H 0.1948 0.2976 0.1748 0.073 Uiso 1 1 calc R . . H31B H 0.1825 0.3295 0.1975 0.073 Uiso 1 1 calc R . . C32 C 0.2427(5) 0.2980(5) 0.2172(4) 0.068(3) Uani 1 1 d DU . . H32A H 0.2687 0.2814 0.2087 0.082 Uiso 1 1 calc R . . H32B H 0.2626 0.3149 0.2298 0.082 Uiso 1 1 calc R . . C33 C 0.1996(8) 0.2810(6) 0.2379(5) 0.083(5) Uani 1 1 d DU . . H33A H 0.1651 0.2925 0.2350 0.125 Uiso 1 1 calc R . . H33B H 0.2101 0.2820 0.2607 0.125 Uiso 1 1 calc R . . H33C H 0.1958 0.2577 0.2313 0.125 Uiso 1 1 calc R . . C34 C 0.2066(4) 0.3974(4) 0.1800(3) 0.050(2) Uani 1 1 d DU . . H34A H 0.1955 0.3810 0.1966 0.060 Uiso 1 1 calc R . . H34B H 0.1771 0.4138 0.1777 0.060 Uiso 1 1 calc R . . C35 C 0.2580(3) 0.4155(3) 0.1917(3) 0.049(2) Uani 1 1 d GDU . . C36 C 0.2722(4) 0.4444(3) 0.1754(3) 0.047(3) Uani 1 1 d GU . . H36 H 0.2480 0.4540 0.1602 0.056 Uiso 1 1 calc R . . C37 C 0.3217(5) 0.4594(3) 0.1812(3) 0.046(3) Uani 1 1 d GU . . C38 C 0.3571(4) 0.4454(3) 0.2034(3) 0.046(3) Uani 1 1 d GU . . H38 H 0.3910 0.4556 0.2074 0.055 Uiso 1 1 calc R . . C39 C 0.3430(4) 0.4164(3) 0.2197(3) 0.047(2) Uani 1 1 d GU . . C40 C 0.2935(4) 0.4015(3) 0.2139(3) 0.051(2) Uani 1 1 d GU . . C41 C 0.6657(9) 0.5066(5) 0.1696(5) 0.052(3) Uani 1 1 d U . . C42 C 0.2426(6) 0.3904(3) 0.2587(3) 0.073(3) Uani 1 1 d DU . . H42A H 0.2063 0.3953 0.2499 0.088 Uiso 1 1 calc R . . H42B H 0.2580 0.4115 0.2669 0.088 Uiso 1 1 calc R . . C43 C 0.2379(7) 0.3654(4) 0.2865(3) 0.083(3) Uani 1 1 d DU . . H43A H 0.2747 0.3593 0.2937 0.099 Uiso 1 1 calc R . . H43B H 0.2206 0.3449 0.2782 0.099 Uiso 1 1 calc R . . C44 C 0.2058(10) 0.3776(7) 0.3161(5) 0.100(5) Uani 1 1 d DU . . H44A H 0.2190 0.3996 0.3226 0.149 Uiso 1 1 calc R . . H44B H 0.2104 0.3618 0.3340 0.149 Uiso 1 1 calc R . . H44C H 0.1675 0.3791 0.3105 0.149 Uiso 1 1 calc R . . O1 O 0.3823(6) 0.3304(4) 0.2248(3) 0.065(2) Uani 1 1 d DU . . O2 O 0.5633(5) 0.4351(3) 0.1823(3) 0.048(3) Uani 1 1 d U . . O3 O 0.5917(6) 0.3895(4) 0.1597(3) 0.054(3) Uani 1 1 d U . . O4 O 0.3401(5) 0.2774(2) 0.1707(3) 0.051(2) Uani 1 1 d DU . . O5 O 0.4995(5) 0.3238(3) 0.0588(3) 0.040(3) Uani 1 1 d U . . O6 O 0.4208(5) 0.3253(3) 0.0328(3) 0.040(2) Uani 1 1 d U . . O7 O 0.2540(5) 0.3320(3) 0.1744(3) 0.055(2) Uani 1 1 d DU . . O8 O 0.2078(6) 0.3841(4) 0.0321(3) 0.054(3) Uani 1 1 d U . . O9 O 0.1866(6) 0.4291(4) 0.0594(3) 0.055(3) Uani 1 1 d U . . O10 O 0.2762(5) 0.3774(4) 0.2336(3) 0.059(2) Uani 1 1 d DU . . O11 O 0.7011(6) 0.4917(4) 0.1511(4) 0.057(3) Uani 1 1 d U . . O12 O 0.6218(6) 0.4923(3) 0.1777(3) 0.050(3) Uani 1 1 d U . . C45 C 0.7865(8) 0.2977(5) 0.0608(5) 0.042(2) Uani 1 1 d U . . H45A H 0.8201 0.2847 0.0583 0.050 Uiso 1 1 calc R . . H45B H 0.7632 0.2860 0.0765 0.050 Uiso 1 1 calc R . . C46 C 0.8002(5) 0.3328(2) 0.0738(3) 0.044(2) Uani 1 1 d GU . . C47 C 0.7611(4) 0.3512(3) 0.0898(3) 0.045(2) Uani 1 1 d GU . . H47 H 0.7279 0.3411 0.0957 0.054 Uiso 1 1 calc R . . C48 C 0.7705(5) 0.3844(3) 0.0973(3) 0.049(2) Uani 1 1 d GU . . C49 C 0.8191(5) 0.3993(2) 0.0888(3) 0.047(2) Uani 1 1 d GU . . H49 H 0.8255 0.4220 0.0939 0.056 Uiso 1 1 calc R . . C50 C 0.8582(4) 0.3808(3) 0.0727(3) 0.045(2) Uani 1 1 d GU . . C51 C 0.8488(4) 0.3476(3) 0.0652(3) 0.045(2) Uani 1 1 d GU . . C52 C 0.7263(9) 0.4026(6) 0.1144(5) 0.053(2) Uani 1 1 d U . . C53 C 0.9205(5) 0.3118(3) 0.0701(3) 0.053(3) Uani 1 1 d DU . . H53A H 0.9004 0.3015 0.0882 0.063 Uiso 1 1 calc R . . H53B H 0.9472 0.3276 0.0792 0.063 Uiso 1 1 calc R . . C54 C 0.9488(5) 0.2850(4) 0.0498(4) 0.058(3) Uani 1 1 d DU . . H54A H 0.9646 0.2956 0.0304 0.070 Uiso 1 1 calc R . . H54B H 0.9216 0.2687 0.0423 0.070 Uiso 1 1 calc R . . C55 C 0.9933(7) 0.2665(6) 0.0682(5) 0.073(5) Uani 1 1 d DU . . H55A H 1.0224 0.2821 0.0736 0.109 Uiso 1 1 calc R . . H55B H 1.0076 0.2485 0.0547 0.109 Uiso 1 1 calc R . . H55C H 0.9785 0.2571 0.0882 0.109 Uiso 1 1 calc R . . C56 C 0.9082(8) 0.3977(5) 0.0628(5) 0.048(2) Uani 1 1 d U . . H56A H 0.9373 0.3810 0.0610 0.057 Uiso 1 1 calc R . . H56B H 0.9187 0.4138 0.0797 0.057 Uiso 1 1 calc R . . C57 C 0.9030(9) 0.4163(6) 0.0302(5) 0.053(2) Uani 1 1 d U . . C58 C 0.8791(8) 0.4470(5) 0.0291(5) 0.051(3) Uani 1 1 d U . . H58 H 0.8712 0.4580 0.0488 0.061 Uiso 1 1 calc R . . C59 C 0.8657(12) 0.4628(8) 0.0000 0.051(4) Uani 1 2 d SU . . C60 C 0.9239(14) 0.4029(9) 0.0000 0.063(3) Uani 1 2 d SU . . C61 C 0.1518(13) 0.5011(8) 0.0000 0.057(4) Uani 1 2 d SU . . C62 C 1.0011(3) 0.3851(3) 0.0000 0.085(3) Uani 1 2 d SDU . . H62A H 1.0089 0.3986 0.0195 0.102 Uiso 0.50 1 calc PR . . H62B H 1.0089 0.3986 -0.0195 0.102 Uiso 0.50 1 calc PR . . C63 C 1.0338(4) 0.3526(3) 0.0000 0.092(4) Uani 1 2 d SDU . . H63A H 1.0253 0.3393 0.0194 0.110 Uiso 0.50 1 calc PR . . H63B H 1.0253 0.3393 -0.0194 0.110 Uiso 0.50 1 calc PR . . C64 C 1.0933(4) 0.3628(6) 0.0000 0.104(5) Uani 1 2 d SDU . . H64A H 1.1004 0.3774 0.0185 0.156 Uiso 0.50 1 calc PR . . H64B H 1.1016 0.3746 -0.0201 0.156 Uiso 0.50 1 calc PR . . H64C H 1.1158 0.3428 0.0016 0.156 Uiso 0.50 1 calc PR . . C65 C 0.6738(11) 0.3154(7) 0.0000 0.043(3) Uani 1 2 d SU . . C66 C 0.7029(8) 0.3109(5) 0.0290(5) 0.043(3) Uani 1 1 d U . . H66 H 0.6852 0.3154 0.0489 0.052 Uiso 1 1 calc R . . C67 C 0.7589(8) 0.2998(5) 0.0298(5) 0.041(2) Uani 1 1 d U . . C68 C 0.7850(11) 0.2945(7) 0.0000 0.043(3) Uani 1 2 d SU . . C69 C 0.6217(12) 0.3240(7) 0.0000 0.043(3) Uani 1 2 d SU . . C70 C 0.8332(8) 0.2450(3) -0.0106(5) 0.048(3) Uani 0.50 1 d PDU A -1 H70A H 0.8710 0.2372 -0.0107 0.057 Uiso 0.50 1 calc PR A -1 H70B H 0.8193 0.2437 -0.0330 0.057 Uiso 0.50 1 calc PR A -1 C71 C 0.7994(14) 0.2221(3) 0.0114(7) 0.047(4) Uani 0.25 1 d PDU A -1 H71A H 0.8163 0.2205 0.0330 0.056 Uiso 0.25 1 calc PR A -1 H71B H 0.7627 0.2314 0.0141 0.056 Uiso 0.25 1 calc PR A -1 C72 C 0.7963(13) 0.1875(5) -0.0043(10) 0.048(5) Uani 0.50 1 d PDU A -1 H72A H 0.8320 0.1770 -0.0039 0.073 Uiso 0.25 1 calc PR A -1 H72B H 0.7842 0.1897 -0.0268 0.073 Uiso 0.25 1 calc PR A -1 H72C H 0.7707 0.1736 0.0076 0.073 Uiso 0.25 1 calc PR A -1 O13 O 0.8847(5) 0.3286(3) 0.0489(3) 0.049(2) Uani 1 1 d DU . . O14 O 0.6855(6) 0.3887(4) 0.1263(3) 0.053(3) Uani 1 1 d U . . O15 O 0.7357(6) 0.4356(4) 0.1236(3) 0.054(3) Uani 1 1 d U . . O16 O 0.9466(5) 0.3735(5) 0.0000 0.071(3) Uani 1 2 d SDU . . O17 O 0.1609(6) 0.4865(4) 0.0272(3) 0.057(3) Uani 1 1 d U . . O18 O 0.8317(8) 0.2790(3) 0.0000 0.045(3) Uani 1 2 d SDU . . O19 O 0.5938(5) 0.3252(3) 0.0272(3) 0.045(3) Uani 1 1 d U . . N1N N 0.47194(15) 0.5001(7) 0.22095(8) 0.086(4) Uani 0.25 1 d PDU . 1 H1N H 0.4542 0.5004 0.2025 0.103 Uiso 0.75 1 calc PR . 1 C1N C 0.47194(15) 0.5001(7) 0.22095(8) 0.086(4) Uani 0.75 1 d PDU . 2 H1N1 H 0.4528 0.5004 0.2011 0.103 Uiso 0.75 1 calc PR . 2 C2N C 0.44399(15) 0.5000 0.2500 0.098(4) Uani 1 2 d SDU . . H2N H 0.4057 0.5000 0.2500 0.118 Uiso 1 2 calc SR . 1 N1P N 1.1611(7) 0.3136(3) 0.01679(10) 0.163(7) Uani 0.50 1 d PDU . 1 H1P H 1.1777 0.3296 0.0274 0.195 Uiso 0.50 1 calc PR . 1 C1P C 1.1611(7) 0.3136(3) 0.01679(10) 0.163(7) Uani 0.50 1 d PDU . 2 H1P1 H 1.1791 0.3308 0.0283 0.195 Uiso 0.50 1 calc PR . 2 C2P C 1.1348(7) 0.2885(3) 0.03358(9) 0.177(9) Uani 1 1 d DU . . H2P H 1.1335 0.2890 0.0565 0.212 Uiso 1 1 calc R . 1 C3P C 1.1105(10) 0.2624(4) 0.01683(10) 0.189(12) Uani 1 1 d DU . . H3P H 1.0940 0.2447 0.0283 0.227 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 0.0554(5) 0.0405(5) 0.0505(5) -0.0033(5) 0.0066(4) -0.0005(4) U2 0.0430(7) 0.0454(8) 0.0346(6) 0.000 0.000 0.0003(6) U3 0.0717(9) 0.0373(8) 0.0424(7) 0.000 0.000 0.0106(7) O1U1 0.040(8) 0.049(9) 0.069(10) 0.015(8) 0.012(8) -0.007(7) O1U2 0.061(12) 0.038(12) 0.017(9) 0.000 0.000 -0.006(10) O2U1 0.063(10) 0.034(9) 0.081(11) 0.002(8) 0.015(9) -0.007(8) O2U2 0.018(9) 0.056(13) 0.057(12) 0.000 0.000 -0.010(10) O1U3 0.067(15) 0.052(14) 0.096(17) 0.000 0.000 0.038(12) O2U3 0.072(13) 0.015(10) 0.046(11) 0.000 0.000 0.022(10) C1 0.047(4) 0.048(4) 0.048(5) 0.001(4) 0.002(3) -0.003(4) C2 0.048(4) 0.049(4) 0.044(4) -0.001(4) 0.001(3) -0.001(3) C3 0.048(4) 0.048(4) 0.047(5) -0.002(4) 0.001(4) -0.001(4) C4 0.047(4) 0.045(4) 0.049(4) 0.000(4) 0.003(3) -0.003(3) C5 0.050(4) 0.043(4) 0.046(5) 0.001(4) -0.001(4) -0.005(4) C6 0.051(4) 0.046(4) 0.047(4) 0.000(3) -0.001(3) -0.005(3) C7 0.053(4) 0.052(4) 0.055(4) -0.004(3) 0.000(3) -0.001(3) C8 0.048(4) 0.044(4) 0.054(4) -0.003(4) 0.008(4) -0.005(3) C9 0.090(5) 0.085(5) 0.081(4) 0.004(4) 0.002(4) -0.008(5) C10 0.106(6) 0.096(5) 0.098(5) 0.009(5) -0.004(5) -0.003(5) C11 0.117(8) 0.112(8) 0.101(6) 0.016(6) -0.004(7) -0.007(7) C12 0.047(4) 0.044(4) 0.044(4) 0.001(4) 0.001(4) -0.003(4) C13 0.048(4) 0.045(4) 0.043(3) 0.002(4) 0.001(3) -0.001(4) C14 0.047(4) 0.043(5) 0.043(4) 0.000(4) 0.001(3) 0.000(4) C15 0.045(4) 0.043(4) 0.041(3) 0.001(4) 0.002(3) 0.000(4) C16 0.044(4) 0.041(5) 0.042(4) -0.001(4) 0.002(3) 0.001(4) C17 0.046(3) 0.043(4) 0.043(4) 0.002(4) 0.000(3) -0.001(4) C18 0.048(3) 0.045(4) 0.044(4) 0.002(4) -0.001(3) -0.001(4) C19 0.042(4) 0.046(4) 0.040(3) 0.000(4) 0.001(3) 0.001(4) C20 0.070(5) 0.055(4) 0.062(5) 0.009(4) -0.002(4) 0.004(4) C21 0.078(5) 0.063(5) 0.074(6) 0.002(5) -0.005(5) 0.000(5) C22 0.084(6) 0.085(8) 0.086(8) 0.001(7) 0.002(6) -0.009(6) C23 0.047(4) 0.044(4) 0.043(5) 0.001(4) -0.001(4) -0.004(4) C24 0.048(4) 0.047(4) 0.047(3) 0.002(3) -0.001(4) -0.002(3) C25 0.051(5) 0.048(4) 0.047(4) 0.003(4) 0.000(4) -0.001(4) C26 0.055(4) 0.050(4) 0.049(3) 0.003(3) 0.000(4) 0.002(4) C27 0.049(5) 0.049(4) 0.051(3) 0.000(4) 0.000(4) -0.001(4) C28 0.046(4) 0.048(4) 0.048(3) 0.001(3) 0.003(4) -0.006(4) C29 0.049(4) 0.048(4) 0.048(3) -0.001(3) 0.000(4) -0.004(4) C30 0.060(4) 0.052(4) 0.050(4) 0.003(3) 0.003(4) 0.006(4) C31 0.065(5) 0.062(5) 0.056(4) 0.000(4) 0.003(4) -0.003(4) C32 0.074(6) 0.066(6) 0.065(5) 0.004(4) 0.002(5) 0.000(5) C33 0.087(8) 0.082(8) 0.079(7) 0.010(6) 0.005(6) -0.004(6) C34 0.050(4) 0.049(4) 0.052(4) -0.001(4) 0.002(4) -0.002(4) C35 0.048(4) 0.048(4) 0.049(4) 0.000(3) 0.001(3) -0.003(3) C36 0.048(4) 0.047(4) 0.046(5) 0.001(4) -0.002(4) -0.001(4) C37 0.046(4) 0.047(5) 0.046(5) 0.002(4) 0.003(4) -0.001(4) C38 0.047(4) 0.047(4) 0.043(5) 0.000(4) 0.003(4) 0.001(4) C39 0.049(4) 0.047(4) 0.046(4) 0.000(4) 0.002(4) 0.000(3) C40 0.052(4) 0.049(4) 0.052(4) 0.003(3) -0.002(3) -0.002(3) C41 0.049(5) 0.047(5) 0.060(5) -0.004(4) 0.004(4) -0.007(4) C42 0.074(5) 0.073(5) 0.073(4) 0.002(4) 0.005(4) -0.003(5) C43 0.086(6) 0.085(6) 0.077(5) 0.006(5) 0.010(5) -0.007(5) C44 0.101(8) 0.106(8) 0.092(6) 0.002(6) 0.014(6) 0.004(7) O1 0.067(4) 0.062(4) 0.065(4) -0.004(4) 0.008(4) -0.008(4) O2 0.043(5) 0.045(4) 0.055(5) -0.002(4) 0.009(4) -0.006(4) O3 0.052(5) 0.046(5) 0.064(5) -0.006(4) 0.014(4) -0.009(4) O4 0.054(4) 0.048(4) 0.050(4) 0.007(4) 0.001(4) 0.000(4) O5 0.041(4) 0.045(5) 0.034(5) -0.001(4) -0.001(4) 0.002(5) O6 0.038(3) 0.044(4) 0.037(3) 0.000(3) 0.003(3) 0.000(3) O7 0.061(5) 0.055(4) 0.049(4) 0.000(4) 0.001(4) -0.002(4) O8 0.061(5) 0.053(5) 0.048(4) 0.004(4) 0.007(5) 0.007(5) O9 0.064(5) 0.052(4) 0.051(5) 0.003(4) 0.006(5) 0.008(5) O10 0.059(4) 0.059(4) 0.058(4) 0.007(4) -0.002(4) -0.005(4) O11 0.051(5) 0.053(5) 0.068(5) 0.001(5) 0.012(4) -0.014(5) O12 0.049(5) 0.039(5) 0.061(5) -0.004(5) 0.012(4) -0.005(4) C45 0.042(4) 0.040(4) 0.043(4) 0.001(4) 0.002(4) 0.003(4) C46 0.044(4) 0.044(4) 0.043(4) 0.000(3) -0.003(3) -0.001(3) C47 0.044(4) 0.043(4) 0.047(5) -0.001(4) -0.003(4) -0.001(4) C48 0.047(4) 0.047(4) 0.053(4) -0.002(4) 0.001(3) -0.001(3) C49 0.047(4) 0.043(4) 0.051(5) 0.001(4) 0.000(4) 0.000(4) C50 0.044(4) 0.044(4) 0.047(4) 0.001(4) -0.003(4) 0.002(3) C51 0.045(4) 0.046(4) 0.043(4) -0.001(4) -0.004(4) -0.001(3) C52 0.052(4) 0.051(4) 0.057(4) -0.004(4) 0.007(4) 0.000(4) C53 0.054(5) 0.051(5) 0.053(5) -0.002(4) -0.002(4) 0.000(4) C54 0.061(5) 0.053(5) 0.060(6) -0.004(5) -0.003(5) 0.002(4) C55 0.073(7) 0.069(7) 0.076(8) -0.001(6) -0.006(6) 0.010(5) C56 0.046(4) 0.046(4) 0.052(4) -0.001(4) -0.005(4) 0.001(4) C57 0.052(4) 0.051(4) 0.054(4) 0.004(3) -0.004(4) -0.001(4) C58 0.052(5) 0.049(4) 0.052(5) 0.003(4) -0.001(4) -0.001(4) C59 0.052(6) 0.049(6) 0.052(6) 0.000 0.000 0.002(5) C60 0.068(5) 0.061(5) 0.060(4) 0.000 0.000 0.002(4) C61 0.062(6) 0.055(6) 0.054(6) 0.000 0.000 0.006(6) C62 0.082(4) 0.084(5) 0.089(5) 0.000 0.000 0.002(4) C63 0.088(5) 0.092(6) 0.097(6) 0.000 0.000 0.008(5) C64 0.096(6) 0.106(9) 0.110(9) 0.000 0.000 0.007(6) C65 0.041(4) 0.042(5) 0.045(5) 0.000 0.000 0.000(4) C66 0.044(4) 0.041(5) 0.044(4) 0.001(4) 0.003(3) 0.002(4) C67 0.042(4) 0.038(4) 0.042(4) 0.002(4) 0.000(3) 0.000(4) C68 0.044(4) 0.041(5) 0.044(4) 0.000 0.000 0.001(4) C69 0.041(4) 0.047(5) 0.043(5) 0.000 0.000 -0.002(5) C70 0.047(5) 0.047(4) 0.049(5) -0.002(4) -0.001(4) 0.004(4) C71 0.047(6) 0.046(5) 0.048(6) -0.001(5) -0.001(5) 0.003(5) C72 0.048(8) 0.049(6) 0.049(9) -0.003(6) 0.003(7) 0.004(6) O13 0.047(4) 0.048(4) 0.053(4) -0.004(4) -0.002(4) -0.002(4) O14 0.049(5) 0.053(5) 0.057(5) -0.005(5) 0.012(4) 0.000(4) O15 0.054(5) 0.052(4) 0.057(5) -0.006(4) 0.008(5) 0.000(4) O16 0.075(4) 0.067(5) 0.072(5) 0.000 0.000 0.006(4) O17 0.065(6) 0.057(6) 0.050(5) 0.000(4) 0.004(5) 0.006(5) O18 0.043(4) 0.044(4) 0.049(5) 0.000 0.000 0.001(4) O19 0.039(5) 0.052(5) 0.042(5) 0.005(5) -0.001(4) -0.002(5) N1N 0.091(6) 0.082(6) 0.086(6) -0.005(5) -0.007(4) 0.000(5) C1N 0.091(6) 0.082(6) 0.086(6) -0.005(5) -0.007(4) 0.000(5) C2N 0.110(6) 0.093(5) 0.092(7) 0.000(7) 0.000 0.000 N1P 0.189(14) 0.174(10) 0.125(15) -0.052(10) -0.014(13) 0.007(10) C1P 0.189(14) 0.174(10) 0.125(15) -0.052(10) -0.014(13) 0.007(10) C2P 0.218(18) 0.167(13) 0.145(18) -0.036(10) -0.025(15) 0.004(13) C3P 0.25(3) 0.166(17) 0.15(2) -0.028(16) -0.04(2) -0.004(15) _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 O1U1 1.703(14) . ? U1 O2U1 1.761(16) . ? U1 O3 2.456(14) . ? U1 O14 2.456(14) . ? U1 O15 2.463(14) . ? U1 O2 2.467(13) . ? U1 O12 2.485(13) . ? U1 O11 2.489(14) . ? U1 C41 2.85(2) . ? U1 C52 2.87(2) . ? U1 C8 2.90(2) . ? U2 O1U2 1.797(18) . ? U2 O2U2 1.83(2) . ? U2 O5 2.440(12) . ? U2 O5 2.440(12) 10 ? U2 O6 2.461(12) 10 ? U2 O6 2.461(12) . ? U2 O19 2.509(13) 10 ? U2 O19 2.509(13) . ? U2 C19 2.81(2) 10 ? U2 C19 2.81(2) . ? U2 C69 2.94(3) . ? U3 O2U3 1.84(2) . ? U3 O1U3 1.89(2) . ? U3 O8 2.461(14) 10 ? U3 O8 2.461(14) . ? U3 O9 2.469(14) 10 ? U3 O9 2.469(14) . ? U3 O17 2.476(15) . ? U3 O17 2.476(15) 10 ? U3 C61 2.83(3) . ? U3 C30 2.86(2) 10 ? U3 C30 2.86(2) . ? C1 C2 1.53(2) . ? C1 C39 1.59(2) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C4 C8 1.42(2) . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C6 C12 1.60(2) . ? C7 O1 1.379(17) . ? C8 O3 1.26(2) . ? C8 O2 1.31(2) . ? C9 O1 1.427(9) . ? C9 C10 1.534(9) . ? C10 C11 1.539(9) . ? C12 C13 1.56(2) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 C19 1.48(2) . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C17 C23 1.50(2) . ? C18 O4 1.397(15) . ? C19 O6 1.27(2) . ? C19 O5 1.32(2) . ? C20 O4 1.423(8) . ? C20 C21 1.543(9) . ? C21 C22 1.541(9) . ? C23 C24 1.57(2) . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C26 C30 1.48(2) . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C28 C34 1.532(9) . ? C29 O7 1.366(16) . ? C30 O9 1.22(2) . ? C30 O8 1.34(2) . ? C31 O7 1.428(9) . ? C31 C32 1.542(9) . ? C32 C33 1.532(9) . ? C34 C35 1.548(8) . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C37 C41 1.48(2) 2_665 ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 O10 1.338(17) . ? C41 O12 1.28(2) . ? C41 O11 1.31(2) . ? C41 C37 1.48(5) 2_665 ? C42 O10 1.434(9) . ? C42 C43 1.536(9) . ? C43 C44 1.541(9) . ? C45 C67 1.46(3) . ? C45 C46 1.55(2) . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C48 C52 1.50(2) . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C50 C56 1.47(2) . ? C51 O13 1.354(16) . ? C52 O14 1.26(2) . ? C52 O15 1.40(3) . ? C53 O13 1.421(9) . ? C53 C54 1.536(9) . ? C54 C55 1.537(9) . ? C56 C57 1.55(3) . ? C57 C58 1.37(3) . ? C57 C60 1.46(3) . ? C58 C59 1.40(3) . ? C59 C58 1.40(3) 10 ? C59 C61 1.52(4) 9_665 ? C60 O16 1.31(4) . ? C60 C57 1.46(3) 10 ? C61 O17 1.29(2) 10 ? C61 O17 1.29(2) . ? C61 C59 1.52(4) 9_665 ? C62 O16 1.430(9) . ? C62 C63 1.536(9) . ? C63 C64 1.533(9) . ? C65 C69 1.34(4) . ? C65 C66 1.41(2) 10 ? C65 C66 1.41(2) . ? C66 C67 1.46(3) . ? C67 C68 1.41(2) . ? C68 O18 1.32(3) . ? C68 C67 1.41(2) 10 ? C69 O19 1.322(19) 10 ? C69 O19 1.322(19) . ? C70 O18 1.434(9) . ? C70 C71 1.543(10) . ? C71 C72 1.541(10) . ? O18 C70 1.434(9) 10 ? N1N C2N 1.389(4) . ? N1N N1N 1.393(8) 2_665 ? C2N C1N 1.389(4) 8_455 ? C2N N1N 1.389(4) 8_455 ? N1P C2P 1.389(7) . ? N1P N1P 1.391(8) 10 ? C1P C2P 1.389(7) . ? C1P C1P 1.391(8) 10 ? C2P C3P 1.393(7) . ? C3P C3P 1.394(8) 10 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1U1 U1 O2U1 178.8(7) . . ? O1U1 U1 O3 90.4(6) . . ? O2U1 U1 O3 90.3(6) . . ? O1U1 U1 O14 91.6(6) . . ? O2U1 U1 O14 89.6(6) . . ? O3 U1 O14 66.9(5) . . ? O1U1 U1 O15 89.6(6) . . ? O2U1 U1 O15 90.9(6) . . ? O3 U1 O15 121.7(5) . . ? O14 U1 O15 54.8(5) . . ? O1U1 U1 O2 89.2(5) . . ? O2U1 U1 O2 90.5(6) . . ? O3 U1 O2 52.5(5) . . ? O14 U1 O2 119.4(5) . . ? O15 U1 O2 174.0(5) . . ? O1U1 U1 O12 88.6(6) . . ? O2U1 U1 O12 90.2(6) . . ? O3 U1 O12 119.2(5) . . ? O14 U1 O12 173.9(5) . . ? O15 U1 O12 119.1(5) . . ? O2 U1 O12 66.7(4) . . ? O1U1 U1 O11 88.2(6) . . ? O2U1 U1 O11 91.0(6) . . ? O3 U1 O11 173.0(5) . . ? O14 U1 O11 120.0(5) . . ? O15 U1 O11 65.2(5) . . ? O2 U1 O11 120.6(5) . . ? O12 U1 O11 53.9(5) . . ? O1U1 U1 C41 86.5(7) . . ? O2U1 U1 C41 92.4(6) . . ? O3 U1 C41 145.6(6) . . ? O14 U1 C41 147.3(6) . . ? O15 U1 C41 92.5(6) . . ? O2 U1 C41 93.2(5) . . ? O12 U1 C41 26.6(5) . . ? O11 U1 C41 27.4(5) . . ? O1U1 U1 C52 92.4(6) . . ? O2U1 U1 C52 88.6(6) . . ? O3 U1 C52 92.7(6) . . ? O14 U1 C52 25.8(5) . . ? O15 U1 C52 29.1(5) . . ? O2 U1 C52 145.1(6) . . ? O12 U1 C52 148.2(6) . . ? O11 U1 C52 94.3(6) . . ? C41 U1 C52 121.6(6) . . ? O1U1 U1 C8 90.0(6) . . ? O2U1 U1 C8 90.2(6) . . ? O3 U1 C8 25.6(5) . . ? O14 U1 C8 92.6(5) . . ? O15 U1 C8 147.3(5) . . ? O2 U1 C8 26.9(5) . . ? O12 U1 C8 93.5(5) . . ? O11 U1 C8 147.5(5) . . ? C41 U1 C8 120.1(6) . . ? C52 U1 C8 118.3(6) . . ? O1U2 U2 O2U2 179.9(8) . . ? O1U2 U2 O5 88.5(3) . . ? O2U2 U2 O5 91.5(3) . . ? O1U2 U2 O5 88.5(3) . 10 ? O2U2 U2 O5 91.5(3) . 10 ? O5 U2 O5 174.4(6) . 10 ? O1U2 U2 O6 90.1(6) . 10 ? O2U2 U2 O6 89.8(5) . 10 ? O5 U2 O6 121.2(4) . 10 ? O5 U2 O6 54.2(4) 10 10 ? O1U2 U2 O6 90.1(6) . . ? O2U2 U2 O6 89.8(5) . . ? O5 U2 O6 54.2(4) . . ? O5 U2 O6 121.2(4) 10 . ? O6 U2 O6 67.0(6) 10 . ? O1U2 U2 O19 89.6(6) . 10 ? O2U2 U2 O19 90.5(6) . 10 ? O5 U2 O19 119.0(4) . 10 ? O5 U2 O19 65.7(4) 10 10 ? O6 U2 O19 119.9(4) 10 10 ? O6 U2 O19 173.1(4) . 10 ? O1U2 U2 O19 89.6(6) . . ? O2U2 U2 O19 90.5(6) . . ? O5 U2 O19 65.7(4) . . ? O5 U2 O19 119.0(4) 10 . ? O6 U2 O19 173.1(4) 10 . ? O6 U2 O19 119.9(4) . . ? O19 U2 O19 53.3(6) 10 . ? O1U2 U2 C19 85.2(5) . 10 ? O2U2 U2 C19 94.7(5) . 10 ? O5 U2 C19 146.9(5) . 10 ? O5 U2 C19 28.0(5) 10 10 ? O6 U2 C19 26.7(5) 10 10 ? O6 U2 C19 93.3(5) . 10 ? O19 U2 C19 93.5(5) 10 10 ? O19 U2 C19 146.5(5) . 10 ? O1U2 U2 C19 85.3(5) . . ? O2U2 U2 C19 94.7(5) . . ? O5 U2 C19 28.0(5) . . ? O5 U2 C19 146.9(5) 10 . ? O6 U2 C19 93.3(5) 10 . ? O6 U2 C19 26.7(5) . . ? O19 U2 C19 146.5(5) 10 . ? O19 U2 C19 93.5(5) . . ? C19 U2 C19 119.0(8) 10 . ? O1U2 U2 C69 88.6(8) . . ? O2U2 U2 C69 91.5(8) . . ? O5 U2 C69 92.3(3) . . ? O5 U2 C69 92.3(3) 10 . ? O6 U2 C69 146.5(3) 10 . ? O6 U2 C69 146.5(3) . . ? O19 U2 C69 26.6(3) 10 . ? O19 U2 C69 26.7(3) . . ? C19 U2 C69 119.9(4) 10 . ? C19 U2 C69 119.9(4) . . ? O2U3 U3 O1U3 178.7(8) . . ? O2U3 U3 O8 90.4(6) . 10 ? O1U3 U3 O8 88.5(6) . 10 ? O2U3 U3 O8 90.4(6) . . ? O1U3 U3 O8 88.5(6) . . ? O8 U3 O8 65.3(7) 10 . ? O2U3 U3 O9 90.4(3) . 10 ? O1U3 U3 O9 89.5(3) . 10 ? O8 U3 O9 53.0(5) 10 10 ? O8 U3 O9 118.3(5) . 10 ? O2U3 U3 O9 90.4(3) . . ? O1U3 U3 O9 89.5(3) . . ? O8 U3 O9 118.3(5) 10 . ? O8 U3 O9 53.0(5) . . ? O9 U3 O9 171.3(7) 10 . ? O2U3 U3 O17 89.6(6) . . ? O1U3 U3 O17 91.5(7) . . ? O8 U3 O17 174.5(5) 10 . ? O8 U3 O17 120.2(5) . . ? O9 U3 O17 121.5(5) 10 . ? O9 U3 O17 67.2(5) . . ? O2U3 U3 O17 89.6(6) . 10 ? O1U3 U3 O17 91.5(7) . 10 ? O8 U3 O17 120.2(5) 10 10 ? O8 U3 O17 174.4(5) . 10 ? O9 U3 O17 67.2(5) 10 10 ? O9 U3 O17 121.5(5) . 10 ? O17 U3 O17 54.2(7) . 10 ? O2U3 U3 C61 90.8(8) . . ? O1U3 U3 C61 90.5(9) . . ? O8 U3 C61 147.3(3) 10 . ? O8 U3 C61 147.3(3) . . ? O9 U3 C61 94.3(3) 10 . ? O9 U3 C61 94.3(3) . . ? O17 U3 C61 27.1(3) . . ? O17 U3 C61 27.1(3) 10 . ? O2U3 U3 C30 89.9(5) . 10 ? O1U3 U3 C30 89.5(5) . 10 ? O8 U3 C30 27.9(5) 10 10 ? O8 U3 C30 93.2(6) . 10 ? O9 U3 C30 25.1(5) 10 10 ? O9 U3 C30 146.2(6) . 10 ? O17 U3 C30 146.6(6) . 10 ? O17 U3 C30 92.3(6) 10 10 ? C61 U3 C30 119.4(5) . 10 ? O2U3 U3 C30 89.9(5) . . ? O1U3 U3 C30 89.5(5) . . ? O8 U3 C30 93.2(6) 10 . ? O8 U3 C30 27.9(5) . . ? O9 U3 C30 146.2(6) 10 . ? O9 U3 C30 25.1(5) . . ? O17 U3 C30 92.3(6) . . ? O17 U3 C30 146.5(6) 10 . ? C61 U3 C30 119.4(5) . . ? C30 U3 C30 121.1(9) 10 . ? C2 C1 C39 112.2(14) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.9(11) . . ? C7 C2 C1 120.4(11) . . ? C2 C3 C4 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 C8 123.7(12) . . ? C5 C4 C8 116.2(12) . . ? C4 C5 C6 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C12 119.8(11) . . ? C5 C6 C12 120.1(11) . . ? O1 C7 C6 119.4(10) . . ? O1 C7 C2 120.6(10) . . ? C6 C7 C2 120.0 . . ? O3 C8 O2 115.2(18) . . ? O3 C8 C4 124.0(19) . . ? O2 C8 C4 120.7(18) . . ? O3 C8 U1 57.2(10) . . ? O2 C8 U1 58.0(10) . . ? C4 C8 U1 177.8(14) . . ? O1 C9 C10 119.4(11) . . ? C9 C10 C11 98.9(14) . . ? C13 C12 C6 109.9(14) . . ? C14 C13 C18 120.0 . . ? C14 C13 C12 120.0(10) . . ? C18 C13 C12 119.3(10) . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 C19 119.8(11) . . ? C16 C15 C19 118.9(11) . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 C23 122.2(11) . . ? C16 C17 C23 117.6(11) . . ? C17 C18 C13 120.0 . . ? C17 C18 O4 120.1(9) . . ? C13 C18 O4 118.9(9) . . ? O6 C19 O5 119.2(17) . . ? O6 C19 C15 120.1(17) . . ? O5 C19 C15 119.3(16) . . ? O6 C19 U2 61.0(10) . . ? O5 C19 U2 60.1(9) . . ? C15 C19 U2 178.0(14) . . ? O4 C20 C21 113.7(14) . . ? C22 C21 C20 114.7(16) . . ? C17 C23 C24 113.4(15) . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 118.0(10) . . ? C29 C24 C23 121.8(10) . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 C30 116.9(11) . . ? C25 C26 C30 123.1(11) . . ? C28 C27 C26 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 C34 120.6(10) . . ? C27 C28 C34 119.3(10) . . ? O7 C29 C28 121.3(9) . . ? O7 C29 C24 118.1(9) . . ? C28 C29 C24 120.0 . . ? O9 C30 O8 118.1(19) . . ? O9 C30 C26 125.8(19) . . ? O8 C30 C26 116.0(18) . . ? O9 C30 U3 59.0(11) . . ? O8 C30 U3 59.1(10) . . ? C26 C30 U3 173.7(14) . . ? O7 C31 C32 98.8(10) . . ? C33 C32 C31 104.4(13) . . ? C28 C34 C35 112.6(10) . . ? C36 C35 C40 120.0 . . ? C36 C35 C34 116.7(9) . . ? C40 C35 C34 122.5(9) . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 C41 121.9(11) . 2_665 ? C38 C37 C41 117.0(12) . 2_665 ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 C1 121.9(11) . . ? C38 C39 C1 117.9(11) . . ? O10 C40 C39 119.3(10) . . ? O10 C40 C35 119.6(9) . . ? C39 C40 C35 120.0 . . ? O12 C41 O11 121.3(19) . . ? O12 C41 C37 121(2) . 2_665 ? O11 C41 C37 118(2) . 2_665 ? O12 C41 U1 60.7(11) . . ? O11 C41 U1 61.0(11) . . ? C37 C41 U1 174(3) 2_665 . ? O10 C42 C43 110.3(11) . . ? C42 C43 C44 115.2(15) . . ? C7 O1 C9 114.3(15) . . ? C8 O2 U1 95.2(12) . . ? C8 O3 U1 97.2(13) . . ? C18 O4 C20 118.1(13) . . ? C19 O5 U2 91.9(10) . . ? C19 O6 U2 92.3(11) . . ? C29 O7 C31 110.3(11) . . ? C30 O8 U3 93.0(12) . . ? C30 O9 U3 95.9(13) . . ? C40 O10 C42 111.3(12) . . ? C41 O11 U1 91.6(12) . . ? C41 O12 U1 92.6(12) . . ? C67 C45 C46 110.9(16) . . ? C47 C46 C51 120.0 . . ? C47 C46 C45 119.8(10) . . ? C51 C46 C45 119.5(10) . . ? C48 C47 C46 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 C52 116.7(12) . . ? C49 C48 C52 123.3(12) . . ? C48 C49 C50 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 C56 118.6(11) . . ? C51 C50 C56 121.4(11) . . ? O13 C51 C50 122.8(9) . . ? O13 C51 C46 117.2(9) . . ? C50 C51 C46 120.0 . . ? O14 C52 O15 116.8(19) . . ? O14 C52 C48 124.1(19) . . ? O15 C52 C48 117.9(17) . . ? O14 C52 U1 58.2(11) . . ? O15 C52 U1 58.9(10) . . ? C48 C52 U1 173.8(14) . . ? O13 C53 C54 106.3(10) . . ? C53 C54 C55 113.3(13) . . ? C50 C56 C57 113.3(16) . . ? C58 C57 C60 117(2) . . ? C58 C57 C56 120(2) . . ? C60 C57 C56 123(2) . . ? C57 C58 C59 123(2) . . ? C58 C59 C58 119(3) . 10 ? C58 C59 C61 120.1(15) . 9_665 ? C58 C59 C61 120.1(15) 10 9_665 ? O16 C60 C57 119.2(16) . . ? O16 C60 C57 119.2(16) . 10 ? C57 C60 C57 118(3) . 10 ? O17 C61 O17 122(3) 10 . ? O17 C61 C59 119.0(15) 10 9_665 ? O17 C61 C59 119.0(15) . 9_665 ? O17 C61 U3 61.0(15) 10 . ? O17 C61 U3 61.0(15) . . ? C59 C61 U3 180(2) 9_665 . ? O16 C62 C63 102.9(11) . . ? C64 C63 C62 106.4(8) . . ? C69 C65 C66 121.8(13) . 10 ? C69 C65 C66 121.8(13) . . ? C66 C65 C66 116(3) 10 . ? C65 C66 C67 123(2) . . ? C68 C67 C45 123.2(19) . . ? C68 C67 C66 117.5(19) . . ? C45 C67 C66 119.1(17) . . ? O18 C68 C67 118.4(14) . 10 ? O18 C68 C67 118.4(14) . . ? C67 C68 C67 122(3) 10 . ? O19 C69 O19 117(2) 10 . ? O19 C69 C65 121.0(13) 10 . ? O19 C69 C65 121.0(13) . . ? O19 C69 U2 58.4(12) 10 . ? O19 C69 U2 58.4(12) . . ? C65 C69 U2 166(2) . . ? O18 C70 C71 111.8(13) . . ? C72 C71 C70 108.4(18) . . ? C51 O13 C53 111.8(11) . . ? C52 O14 U1 96.1(13) . . ? C52 O15 U1 92.0(11) . . ? C60 O16 C62 96.6(19) . . ? C61 O17 U3 91.9(15) . . ? C68 O18 C70 118.3(19) . . ? C68 O18 C70 118.3(19) . 10 ? C70 O18 C70 35.7(17) . 10 ? C69 O19 U2 95.0(13) . . ? C2N N1N N1N 120.0(2) . 2_665 ? C1N C2N N1N 0.00(14) 8_455 8_455 ? C1N C2N N1N 120.0(4) 8_455 . ? N1N C2N N1N 120.0(4) 8_455 . ? C2P N1P N1P 120.0(3) . 10 ? C2P C1P C1P 120.0(3) . 10 ? N1P C2P C1P 0.0(11) . . ? N1P C2P C3P 120.1(4) . . ? C1P C2P C3P 120.1(4) . . ? C2P C3P C3P 119.9(3) . 10 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 24.37 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 18.388 _refine_diff_density_min -2.667 _refine_diff_density_rms 0.482