data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ogden, Mark' _publ_contact_author_email m.ogden@curtin.edu.au _publ_section_title ; Cluster Control in Oligouranyl Complexes of p-t-Butylcalix[8]arene ; _publ_author_name M.Ogden # Attachment '- mo10b_1b.cif' data_mo10b _database_code_depnum_ccdc_archive 'CCDC 773076' #TrackingRef '- mo10b_1b.cif' _audit_creation_date 2008-08-04T20:51:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C115.50 H180 N10 O18 U2' _chemical_formula_moiety ; 2(C7 H19 N2),0.5(C7 H20 N2), C88 H107 O13 U2,5(H2 O),5(C2 H3 N) ; _chemical_formula_weight 2472.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.110(3) _cell_length_b 18.202(3) _cell_length_c 21.289(4) _cell_angle_alpha 94.390(4) _cell_angle_beta 102.742(4) _cell_angle_gamma 103.199(4) _cell_volume 6604(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6389 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max .32 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .17 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow_brown _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2542 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.508 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .46 _exptl_absorpt_correction_T_max .65 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_av_unetI/netI 0.1041 _diffrn_reflns_number 64740 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 29.37 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.895 _reflns_number_total 32531 _reflns_number_gt 18867 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1274P)^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_number_reflns 32531 _refine_ls_number_parameters 1287 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.2116 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 0.97 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.005 _refine_diff_density_max 3.664 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.19 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.239630(11) 0.502953(11) 0.506874(10) 0.02766(5) Uani 1 1 d . . . U2 U 0.314717(11) 0.651125(11) 0.700138(10) 0.03328(6) Uani 1 1 d . . . O0 O 0.31304(19) 0.56897(18) 0.60804(16) 0.0282(9) Uani 1 1 d . . . H0 H 0.363 0.5584 0.6151 0.034 Uiso 1 1 calc RD . . O101 O 0.3266(2) 0.4756(2) 0.5006(2) 0.0406(11) Uani 1 1 d . . . O102 O 0.1513(2) 0.5289(2) 0.51396(18) 0.0332(9) Uani 1 1 d . . . O201 O 0.4146(2) 0.6471(2) 0.7272(2) 0.0433(11) Uani 1 1 d . . . O202 O 0.2132(2) 0.6499(2) 0.67233(18) 0.0344(10) Uani 1 1 d . . . O11 O 0.2147(2) 0.5120(2) 0.39984(18) 0.0343(9) Uani 1 1 d . . . C11 C 0.2415(3) 0.4947(3) 0.3476(3) 0.0323(13) Uani 1 1 d . . . C12 C 0.3059(3) 0.5424(3) 0.3347(3) 0.0360(14) Uani 1 1 d . . . C13 C 0.3307(3) 0.5271(3) 0.2786(3) 0.0428(15) Uani 1 1 d . . . H13 H 0.3749 0.5613 0.2708 0.051 Uiso 1 1 calc R . . C14 C 0.2919(3) 0.4630(3) 0.2340(3) 0.0434(15) Uani 1 1 d . . . C141 C 0.3191(4) 0.4500(4) 0.1703(3) 0.0560(18) Uani 1 1 d . . . C142 C 0.4052(4) 0.4571(5) 0.1854(4) 0.075(2) Uani 1 1 d . . . H14A H 0.4167 0.4139 0.2069 0.113 Uiso 1 1 calc R . . H14B H 0.4326 0.5047 0.2142 0.113 Uiso 1 1 calc R . . H14C H 0.4227 0.4574 0.145 0.113 Uiso 1 1 calc R . . C143 C 0.2975(5) 0.5137(5) 0.1291(4) 0.090(3) Uani 1 1 d . . . H14D H 0.3258 0.5639 0.1533 0.135 Uiso 1 1 calc R . . H14E H 0.2411 0.5089 0.1207 0.135 Uiso 1 1 calc R . . H14F H 0.3123 0.508 0.0877 0.135 Uiso 1 1 calc R . . C144 C 0.2736(5) 0.3712(4) 0.1323(3) 0.066(2) Uani 1 1 d . . . H14G H 0.2976 0.3594 0.0971 0.1 Uiso 1 1 calc R . . H14H H 0.2191 0.3718 0.114 0.1 Uiso 1 1 calc R . . H14I H 0.2751 0.3325 0.1617 0.1 Uiso 1 1 calc R . . C15 C 0.2298(3) 0.4146(3) 0.2490(3) 0.0392(15) Uani 1 1 d . . . H15 H 0.204 0.3689 0.2202 0.047 Uiso 1 1 calc R . . C16 C 0.2028(3) 0.4287(3) 0.3035(2) 0.0338(14) Uani 1 1 d . . . C1 C 0.1380(3) 0.3718(3) 0.3178(3) 0.0375(16) Uani 1 1 d . . . H1A H 0.1022 0.3446 0.2763 0.045 Uiso 1 1 calc R . . H1B H 0.108 0.3987 0.3409 0.045 Uiso 1 1 calc R . . O21 O 0.2973(2) 0.63900(19) 0.49973(18) 0.0332(9) Uani 1 1 d . . . C21 C 0.2771(3) 0.6769(3) 0.4485(3) 0.0387(14) Uani 1 1 d . . . C22 C 0.2281(3) 0.7270(3) 0.4517(3) 0.0414(15) Uani 1 1 d . . . C23 C 0.2091(4) 0.7656(4) 0.4000(3) 0.0584(18) Uani 1 1 d . . . H23 H 0.1775 0.8001 0.4034 0.07 Uiso 1 1 calc R . . C24 C 0.2338(5) 0.7569(4) 0.3423(3) 0.064(2) Uani 1 1 d . . . C241 C 0.2059(6) 0.7977(4) 0.2849(4) 0.084(3) Uani 1 1 d . . . C242 C 0.1204(7) 0.7646(7) 0.2573(5) 0.149(5) Uani 1 1 d . . . H24A H 0.1116 0.7129 0.2353 0.224 Uiso 1 1 calc R . . H24B H 0.1 0.7963 0.226 0.224 Uiso 1 1 calc R . . H24C H 0.0932 0.7628 0.2924 0.224 Uiso 1 1 calc R . . C243 C 0.2189(7) 0.8792(7) 0.3079(6) 0.136(5) Uiso 1 1 d . . . H24D H 0.1825 0.8854 0.3347 0.204 Uiso 1 1 calc R . . H24E H 0.2099 0.9071 0.2705 0.204 Uiso 1 1 calc R . . H24F H 0.2728 0.8993 0.3339 0.204 Uiso 1 1 calc R . . C244 C 0.2555(8) 0.7901(6) 0.2340(4) 0.165(4) Uani 1 1 d . . . H24G H 0.2402 0.7376 0.2122 0.248 Uiso 1 1 calc R . . H24H H 0.3112 0.8034 0.2563 0.248 Uiso 1 1 calc R . . H24I H 0.2462 0.8247 0.2017 0.248 Uiso 1 1 calc R . . C25 C 0.2800(4) 0.7079(3) 0.3410(3) 0.0562(18) Uani 1 1 d . . . H25 H 0.2982 0.7007 0.303 0.067 Uiso 1 1 calc R . . C26 C 0.3028(3) 0.6670(3) 0.3923(3) 0.0422(15) Uani 1 1 d . . . C2 C 0.3514(3) 0.6108(3) 0.3846(3) 0.0458(16) Uani 1 1 d . . . H2A H 0.3687 0.5934 0.427 0.055 Uiso 1 1 calc R . . H2B H 0.3986 0.6367 0.3711 0.055 Uiso 1 1 calc R . . O31 O 0.3392(2) 0.72283(19) 0.60721(19) 0.0354(10) Uani 1 1 d . . . H31 H 0.3234 0.696 0.5706 0.042 Uiso 1 1 calc R . . C31 C 0.3328(3) 0.7959(3) 0.6005(3) 0.0374(14) Uani 1 1 d . . . C32 C 0.3922(3) 0.8570(4) 0.6356(3) 0.0468(16) Uani 1 1 d . A . C33 C 0.3828(4) 0.9323(4) 0.6245(3) 0.065(2) Uani 1 1 d . . . H33 H 0.4239 0.975 0.6464 0.078 Uiso 1 1 calc R . . C34 C 0.3183(4) 0.9454(4) 0.5845(3) 0.0628(18) Uani 1 1 d . . . C341 C 0.3165(5) 1.0281(4) 0.5788(4) 0.083(2) Uani 1 1 d D . . C342 C 0.3035(6) 1.0651(5) 0.6310(5) 0.113(4) Uani 1 1 d D . . H34A H 0.3469 1.0687 0.6689 0.17 Uiso 1 1 calc R . . H34B H 0.2546 1.037 0.6397 0.17 Uiso 1 1 calc R . . H34C H 0.2996 1.1163 0.6225 0.17 Uiso 1 1 calc R . . C343 C 0.3700(6) 1.0645(5) 0.5456(6) 0.130(4) Uani 1 1 d . . . H34D H 0.3568 1.1114 0.5327 0.195 Uiso 1 1 calc R . . H34E H 0.3678 1.0307 0.5068 0.195 Uiso 1 1 calc R . . H34F H 0.4229 1.0771 0.5741 0.195 Uiso 1 1 calc R . . C344 C 0.2328(7) 1.0255(5) 0.5280(6) 0.119(5) Uani 1 1 d . . . H34G H 0.236 1.0116 0.4835 0.178 Uiso 1 1 calc R . . H34H H 0.2218 1.0757 0.532 0.178 Uiso 1 1 calc R . . H34I H 0.1908 0.9876 0.5383 0.178 Uiso 1 1 calc R . . C35 C 0.2617(4) 0.8842(3) 0.5518(3) 0.0518(17) Uani 1 1 d . . . H35 H 0.2162 0.892 0.5239 0.062 Uiso 1 1 calc R . . C36 C 0.2677(3) 0.8087(3) 0.5574(3) 0.0398(14) Uani 1 1 d . . . C3 C 0.2059(3) 0.7449(3) 0.5151(3) 0.0405(14) Uani 1 1 d . . . H3A H 0.1554 0.7591 0.5057 0.049 Uiso 1 1 calc R . . H3B H 0.1997 0.6993 0.5378 0.049 Uiso 1 1 calc R . . O41 O 0.3500(2) 0.7724(2) 0.74124(19) 0.0392(11) Uani 1 1 d . . . C41 C 0.4085(3) 0.8265(3) 0.7795(3) 0.0436(17) Uani 1 1 d . . . C42 C 0.4127(4) 0.8435(3) 0.8453(3) 0.0461(18) Uani 1 1 d . B . C43 C 0.4750(4) 0.9023(3) 0.8830(4) 0.0534(19) Uani 1 1 d . . . H43 H 0.4768 0.9146 0.9276 0.064 Uiso 1 1 calc R . . C44 C 0.5347(4) 0.9437(4) 0.8576(4) 0.060(2) Uani 1 1 d D A . C441 C 0.6007(5) 1.0080(4) 0.9021(4) 0.101(3) Uani 1 1 d D . . C442 C 0.6152(12) 0.9976(12) 0.9726(6) 0.169(13) Uiso 0.5 1 d PD A 1 H44A H 0.5702 1.0038 0.989 0.254 Uiso 0.5 1 calc PR A 1 H44B H 0.6623 1.0358 0.9972 0.254 Uiso 0.5 1 calc PR A 1 H44C H 0.6227 0.9465 0.9776 0.254 Uiso 0.5 1 calc PR A 1 C443 C 0.5821(12) 1.0843(8) 0.8877(13) 0.26(2) Uiso 0.5 1 d PD A 1 H44D H 0.6265 1.1263 0.9107 0.393 Uiso 0.5 1 calc PR A 1 H44E H 0.5354 1.0884 0.9023 0.393 Uiso 0.5 1 calc PR A 1 H44F H 0.5727 1.0866 0.8408 0.393 Uiso 0.5 1 calc PR A 1 C444 C 0.6791(7) 1.0111(10) 0.8815(8) 0.087(6) Uiso 0.5 1 d PD A 1 H44G H 0.7228 1.0434 0.9153 0.131 Uiso 0.5 1 calc PR A 1 H44H H 0.6769 1.0323 0.8404 0.131 Uiso 0.5 1 calc PR A 1 H44I H 0.6865 0.9595 0.8761 0.131 Uiso 0.5 1 calc PR A 1 C445 C 0.6330(10) 0.9768(9) 0.9677(6) 0.100(7) Uiso 0.5 1 d PD A 2 H44J H 0.6344 0.9237 0.958 0.15 Uiso 0.5 1 calc PR A 2 H44K H 0.5987 0.9799 0.997 0.15 Uiso 0.5 1 calc PR A 2 H44L H 0.686 1.0077 0.9886 0.15 Uiso 0.5 1 calc PR A 2 C446 C 0.5683(7) 1.0733(6) 0.9246(7) 0.064(4) Uiso 0.5 1 d PD A 2 H44M H 0.5252 1.0532 0.9444 0.096 Uiso 0.5 1 calc PR A 2 H44N H 0.5492 1.0979 0.8871 0.096 Uiso 0.5 1 calc PR A 2 H44O H 0.6099 1.1106 0.9566 0.096 Uiso 0.5 1 calc PR A 2 C447 C 0.6642(6) 1.0357(8) 0.8686(6) 0.056(4) Uiso 0.5 1 d PD A 2 H44P H 0.7092 1.0699 0.8998 0.083 Uiso 0.5 1 calc PR A 2 H44Q H 0.6449 1.0632 0.8333 0.083 Uiso 0.5 1 calc PR A 2 H44R H 0.68 0.9922 0.8508 0.083 Uiso 0.5 1 calc PR A 2 C45 C 0.5290(4) 0.9242(4) 0.7924(4) 0.064(2) Uiso 1 1 d . . . H45 H 0.5685 0.9509 0.7738 0.077 Uiso 1 1 calc R A . C46 C 0.4664(4) 0.8657(4) 0.7516(4) 0.0522(19) Uani 1 1 d . A . C4 C 0.4653(4) 0.8462(4) 0.6825(3) 0.0527(19) Uani 1 1 d . . . H4A H 0.4677 0.7926 0.675 0.063 Uiso 1 1 calc R A . H4B H 0.5124 0.8787 0.6731 0.063 Uiso 1 1 calc R . . O51 O 0.2985(2) 0.6434(2) 0.80336(18) 0.0345(10) Uani 1 1 d . . . C51 C 0.3550(3) 0.6571(3) 0.8611(3) 0.0380(15) Uani 1 1 d . . . C52 C 0.3883(3) 0.5974(3) 0.8806(3) 0.0371(15) Uani 1 1 d . C . C53 C 0.4401(3) 0.6090(3) 0.9421(3) 0.0447(17) Uani 1 1 d . . . H53 H 0.4599 0.5677 0.9568 0.054 Uiso 1 1 calc R . . C54 C 0.4632(3) 0.6760(3) 0.9815(3) 0.0438(17) Uani 1 1 d . B . C541 C 0.5212(4) 0.6867(4) 1.0486(4) 0.062(2) Uani 1 1 d . . . C542 C 0.5955(7) 0.6603(7) 1.0400(6) 0.049(3) Uiso 0.5 1 d P B 1 H54A H 0.6295 0.6607 1.0828 0.074 Uiso 0.5 1 calc PR B 1 H54B H 0.624 0.6952 1.0155 0.074 Uiso 0.5 1 calc PR B 1 H54C H 0.5793 0.6087 1.0163 0.074 Uiso 0.5 1 calc PR B 1 C543 C 0.5453(8) 0.7620(7) 1.0849(6) 0.051(3) Uiso 0.5 1 d P B 1 H54D H 0.4999 0.7755 1.0961 0.076 Uiso 0.5 1 calc PR B 1 H54E H 0.5674 0.7988 1.0585 0.076 Uiso 0.5 1 calc PR B 1 H54F H 0.5849 0.7629 1.1248 0.076 Uiso 0.5 1 calc PR B 1 C544 C 0.4856(8) 0.6285(8) 1.0893(6) 0.052(3) Uiso 0.5 1 d P B 1 H54G H 0.4447 0.5874 1.0605 0.078 Uiso 0.5 1 calc PR B 1 H54H H 0.4627 0.6537 1.1198 0.078 Uiso 0.5 1 calc PR B 1 H54I H 0.5265 0.6073 1.1137 0.078 Uiso 0.5 1 calc PR B 1 C545 C 0.5405(15) 0.6235(15) 1.0633(13) 0.142(10) Uiso 0.5 1 d P B 2 H54J H 0.5519 0.5982 1.0256 0.213 Uiso 0.5 1 calc PR B 2 H54K H 0.497 0.5896 1.0755 0.213 Uiso 0.5 1 calc PR B 2 H54L H 0.5869 0.6357 1.0998 0.213 Uiso 0.5 1 calc PR B 2 C546 C 0.5885(12) 0.7606(12) 1.0579(10) 0.106(7) Uiso 0.5 1 d P B 2 H54M H 0.6258 0.7647 1.0998 0.159 Uiso 0.5 1 calc PR B 2 H54N H 0.5665 0.8051 1.0568 0.159 Uiso 0.5 1 calc PR B 2 H54O H 0.6153 0.7584 1.0228 0.159 Uiso 0.5 1 calc PR B 2 C547 C 0.4807(14) 0.7147(14) 1.1004(11) 0.127(9) Uiso 0.5 1 d P B 2 H54P H 0.505 0.7032 1.1431 0.19 Uiso 0.5 1 calc PR B 2 H54Q H 0.4249 0.6887 1.0884 0.19 Uiso 0.5 1 calc PR B 2 H54R H 0.487 0.7698 1.102 0.19 Uiso 0.5 1 calc PR B 2 C55 C 0.4331(4) 0.7356(4) 0.9599(3) 0.0480(18) Uani 1 1 d . . . H55 H 0.4499 0.7834 0.9867 0.058 Uiso 1 1 calc R B . C56 C 0.3788(3) 0.7281(3) 0.8999(3) 0.0379(15) Uani 1 1 d . B . C5 C 0.3561(4) 0.7981(3) 0.8772(3) 0.0386(15) Uani 1 1 d . . . H5A H 0.304 0.7824 0.8462 0.046 Uiso 1 1 calc R B . H5B H 0.3516 0.8306 0.9149 0.046 Uiso 1 1 calc R . . O61 O 0.2658(2) 0.50930(19) 0.70839(17) 0.0304(9) Uani 1 1 d . . . C61 C 0.2354(3) 0.4751(3) 0.7551(3) 0.0335(14) Uani 1 1 d . . . C62 C 0.1562(3) 0.4316(3) 0.7392(3) 0.0329(14) Uani 1 1 d . . . C63 C 0.1260(3) 0.3954(3) 0.7858(3) 0.0383(15) Uani 1 1 d . . . H63 H 0.0734 0.3657 0.7741 0.046 Uiso 1 1 calc R . . C64 C 0.1694(4) 0.4006(3) 0.8497(3) 0.0423(16) Uani 1 1 d . C . C641 C 0.1345(5) 0.3581(4) 0.8992(3) 0.061(2) Uani 1 1 d . . . C642 C 0.0503(10) 0.3083(10) 0.8728(9) 0.084(5) Uiso 0.5 1 d P C 1 H64A H 0.0502 0.2658 0.8417 0.126 Uiso 0.5 1 calc PR C 1 H64B H 0.017 0.3391 0.8511 0.126 Uiso 0.5 1 calc PR C 1 H64C H 0.0301 0.2886 0.9089 0.126 Uiso 0.5 1 calc PR C 1 C643 C 0.1272(9) 0.4167(9) 0.9556(8) 0.071(4) Uiso 0.5 1 d P C 1 H64D H 0.1028 0.3886 0.9863 0.107 Uiso 0.5 1 calc PR C 1 H64E H 0.0949 0.4498 0.9367 0.107 Uiso 0.5 1 calc PR C 1 H64F H 0.1794 0.4478 0.9784 0.107 Uiso 0.5 1 calc PR C 1 C644 C 0.1897(9) 0.3067(9) 0.9289(8) 0.071(4) Uiso 0.5 1 d P C 1 H64G H 0.1682 0.2795 0.9615 0.106 Uiso 0.5 1 calc PR C 1 H64H H 0.2421 0.3391 0.9495 0.106 Uiso 0.5 1 calc PR C 1 H64I H 0.193 0.2699 0.8942 0.106 Uiso 0.5 1 calc PR C 1 C645 C 0.1126(11) 0.2801(11) 0.8747(9) 0.092(6) Uiso 0.5 1 d P C 2 H64J H 0.1567 0.2576 0.8891 0.137 Uiso 0.5 1 calc PR C 2 H64K H 0.0977 0.274 0.8271 0.137 Uiso 0.5 1 calc PR C 2 H64L H 0.0681 0.2542 0.8907 0.137 Uiso 0.5 1 calc PR C 2 C646 C 0.0540(11) 0.3854(12) 0.9036(10) 0.099(6) Uiso 0.5 1 d P C 2 H64M H 0.0381 0.3702 0.9428 0.149 Uiso 0.5 1 calc PR C 2 H64N H 0.0119 0.3613 0.8652 0.149 Uiso 0.5 1 calc PR C 2 H64O H 0.0645 0.4409 0.9055 0.149 Uiso 0.5 1 calc PR C 2 C647 C 0.1858(13) 0.3917(13) 0.9658(10) 0.115(8) Uiso 0.5 1 d P C 2 H64P H 0.157 0.3771 0.9988 0.172 Uiso 0.5 1 calc PR C 2 H64Q H 0.2009 0.4473 0.9686 0.172 Uiso 0.5 1 calc PR C 2 H64R H 0.2329 0.3724 0.9734 0.172 Uiso 0.5 1 calc PR C 2 C65 C 0.2477(4) 0.4446(3) 0.8643(3) 0.0452(17) Uani 1 1 d . . . H65 H 0.2786 0.4498 0.9074 0.054 Uiso 1 1 calc R C . C66 C 0.2816(3) 0.4805(3) 0.8187(3) 0.0361(15) Uani 1 1 d . C . C6 C 0.3667(3) 0.5231(3) 0.8370(3) 0.0402(16) Uani 1 1 d . . . H6A H 0.3973 0.4894 0.8586 0.048 Uiso 1 1 calc R C . H6B H 0.3833 0.533 0.7965 0.048 Uiso 1 1 calc R . . O71 O 0.2254(2) 0.42561(19) 0.59808(16) 0.0310(10) Uani 1 1 d . . . H71 H 0.2356 0.453 0.634 0.037 Uiso 1 1 calc R . . C71 C 0.1798(3) 0.3559(3) 0.6011(3) 0.0312(14) Uani 1 1 d . . . C72 C 0.1918(3) 0.2899(3) 0.5704(2) 0.0330(14) Uani 1 1 d . . . C73 C 0.1452(4) 0.2194(3) 0.5745(3) 0.0389(15) Uani 1 1 d . . . H73 H 0.1545 0.1753 0.5542 0.047 Uiso 1 1 calc R . . C74 C 0.0860(3) 0.2100(3) 0.6067(3) 0.0371(15) Uani 1 1 d . . . C741 C 0.0359(4) 0.1328(3) 0.6124(3) 0.0495(19) Uani 1 1 d . . . C742 C 0.0405(6) 0.1250(4) 0.6860(3) 0.088(3) Uani 1 1 d . . . H74A H 0.0315 0.1706 0.7074 0.131 Uiso 1 1 calc R . . H74B H 0.0924 0.1193 0.7071 0.131 Uiso 1 1 calc R . . H74C H 0.0005 0.0801 0.6895 0.131 Uiso 1 1 calc R . . C743 C 0.0637(5) 0.0661(4) 0.5823(5) 0.083(3) Uani 1 1 d . . . H74D H 0.0291 0.0173 0.5857 0.125 Uiso 1 1 calc R . . H74E H 0.1173 0.0684 0.6058 0.125 Uiso 1 1 calc R . . H74F H 0.062 0.0706 0.5364 0.125 Uiso 1 1 calc R . . C744 C -0.0489(4) 0.1259(4) 0.5790(4) 0.060(2) Uani 1 1 d . . . H74G H -0.0665 0.1674 0.5982 0.09 Uiso 1 1 calc R . . H74H H -0.0811 0.0769 0.5847 0.09 Uiso 1 1 calc R . . H74I H -0.0538 0.1289 0.5326 0.09 Uiso 1 1 calc R . . C75 C 0.0735(3) 0.2778(3) 0.6368(3) 0.0344(14) Uani 1 1 d . . . H75 H 0.0334 0.2742 0.6595 0.041 Uiso 1 1 calc R . . C76 C 0.1198(3) 0.3485(3) 0.6330(3) 0.0340(14) Uani 1 1 d . . . C7 C 0.1086(3) 0.4192(3) 0.6696(2) 0.0329(14) Uani 1 1 d . . . H7A H 0.1255 0.4642 0.6481 0.039 Uiso 1 1 calc R . . H7B H 0.0526 0.4125 0.6686 0.039 Uiso 1 1 calc R . . O81 O 0.16763(19) 0.38333(19) 0.46098(17) 0.0277(9) Uani 1 1 d . . . C81 C 0.1866(3) 0.3256(3) 0.4265(3) 0.0293(13) Uani 1 1 d . D . C82 C 0.1655(3) 0.3135(3) 0.3589(2) 0.0274(12) Uani 1 1 d . . . C83 C 0.1811(3) 0.2505(3) 0.3259(3) 0.0356(14) Uani 1 1 d . D . H83 H 0.1677 0.2433 0.2797 0.043 Uiso 1 1 calc R . . C84 C 0.2150(4) 0.1992(3) 0.3583(3) 0.0579(19) Uani 1 1 d D . . C841 C 0.2108(6) 0.1200(6) 0.3240(5) 0.035(3) Uiso 0.5 1 d PD D 1 C842 C 0.1516(6) 0.0568(6) 0.3406(6) 0.050(3) Uiso 0.5 1 d PD D 1 H84A H 0.0988 0.0588 0.3182 0.075 Uiso 0.5 1 calc PR D 1 H84B H 0.1569 0.0628 0.3877 0.075 Uiso 0.5 1 calc PR D 1 H84C H 0.1605 0.0076 0.3268 0.075 Uiso 0.5 1 calc PR D 1 C843 C 0.1956(7) 0.1205(7) 0.2514(4) 0.047(3) Uiso 0.5 1 d PD D 1 H84D H 0.2013 0.0728 0.2308 0.071 Uiso 0.5 1 calc PR D 1 H84E H 0.2333 0.1635 0.2419 0.071 Uiso 0.5 1 calc PR D 1 H84F H 0.1423 0.1256 0.2344 0.071 Uiso 0.5 1 calc PR D 1 C844 C 0.2953(6) 0.1083(8) 0.3442(7) 0.065(4) Uiso 0.5 1 d PD D 1 H84G H 0.2992 0.0646 0.3163 0.097 Uiso 0.5 1 calc PR D 1 H84H H 0.3066 0.0988 0.3896 0.097 Uiso 0.5 1 calc PR D 1 H84I H 0.3332 0.1541 0.3394 0.097 Uiso 0.5 1 calc PR D 1 C845 C 0.2439(8) 0.1389(9) 0.3161(7) 0.083(5) Uiso 0.5 1 d PD D 2 C846 C 0.1678(10) 0.0840(10) 0.2784(10) 0.131(9) Uiso 0.5 1 d PD D 2 H84J H 0.1349 0.0678 0.3083 0.196 Uiso 0.5 1 calc PR D 2 H84K H 0.1791 0.0394 0.2575 0.196 Uiso 0.5 1 calc PR D 2 H84L H 0.1403 0.1093 0.2452 0.196 Uiso 0.5 1 calc PR D 2 C847 C 0.2845(8) 0.1747(9) 0.2665(6) 0.098(6) Uiso 0.5 1 d PD D 2 H84M H 0.3226 0.2225 0.2872 0.148 Uiso 0.5 1 calc PR D 2 H84N H 0.2456 0.185 0.2306 0.148 Uiso 0.5 1 calc PR D 2 H84O H 0.3116 0.1397 0.2496 0.148 Uiso 0.5 1 calc PR D 2 C848 C 0.2987(7) 0.1018(7) 0.3586(6) 0.053(4) Uiso 0.5 1 d PD D 2 H84P H 0.2906 0.1054 0.4027 0.079 Uiso 0.5 1 calc PRD D 2 H84Q H 0.3528 0.1278 0.36 0.079 Uiso 0.5 1 calc PR D 2 H84R H 0.2882 0.0481 0.3409 0.079 Uiso 0.5 1 calc PR D 2 C85 C 0.2366(4) 0.2145(3) 0.4262(3) 0.0558(19) Uani 1 1 d . D . H85 H 0.2605 0.1803 0.4498 0.067 Uiso 1 1 calc RD . . C86 C 0.2247(3) 0.2777(3) 0.4615(3) 0.0405(15) Uani 1 1 d . . . C8 C 0.2550(3) 0.2942(3) 0.5335(3) 0.0383(15) Uani 1 1 d . D . H8A H 0.2908 0.3458 0.5446 0.046 Uiso 1 1 calc R . . H8B H 0.2858 0.2575 0.5481 0.046 Uiso 1 1 calc R . . N101 N 0.5436(10) 0.6105(9) 0.5906(11) 0.236(15) Uiso 0.5 1 d PD E -1 H101 H 0.5572 0.6172 0.6358 0.283 Uiso 0.5 1 calc PR E -1 C104 C 0.4784(7) 0.6474(7) 0.5670(7) 0.060(4) Uiso 0.5 1 d PD E -1 H10A H 0.4331 0.609 0.5399 0.089 Uiso 0.5 1 calc PR E -1 H10B H 0.4958 0.6874 0.5413 0.089 Uiso 0.5 1 calc PR E -1 H10C H 0.4638 0.6698 0.6043 0.089 Uiso 0.5 1 calc PRD E -1 C105 C 0.6122(8) 0.6529(9) 0.5656(8) 0.074(5) Uiso 0.5 1 d PD E -1 H10D H 0.5974 0.6467 0.518 0.111 Uiso 0.5 1 calc PR E -1 H10E H 0.6575 0.6321 0.5803 0.111 Uiso 0.5 1 calc PR E -1 H10F H 0.6257 0.7072 0.5826 0.111 Uiso 0.5 1 calc PR E -1 C101 C 0.5246(9) 0.5270(7) 0.5658(6) 0.069(4) Uiso 0.5 1 d PD E -1 H10G H 0.5719 0.5093 0.5832 0.083 Uiso 0.5 1 calc PR E -1 H10H H 0.4836 0.5009 0.5862 0.083 Uiso 0.5 1 calc PR E -1 C102 C 0.5 0.5 0.5 0.083(4) Uiso 1 2 d SD E -1 H10I H 0.54 0.5273 0.4791 0.1 Uiso 0.5 1 calc PR E -1 H10J H 0.4514 0.5158 0.4828 0.1 Uiso 0.5 1 calc PR E -1 C103 C 0.4846(10) 0.4193(7) 0.4771(6) 0.076(5) Uiso 0.5 1 d PD E -1 H10K H 0.5337 0.4039 0.4928 0.092 Uiso 0.5 1 calc PR E -1 H10L H 0.4461 0.3917 0.4993 0.092 Uiso 0.5 1 calc PR E -1 N102 N 0.4564(4) 0.3908(4) 0.4087(4) 0.0212(18) Uiso 0.5 1 d PD E -1 H102 H 0.4832 0.4308 0.3912 0.025 Uiso 0.5 1 calc PR E -1 C106 C 0.3768(6) 0.3857(7) 0.3738(6) 0.050(3) Uiso 0.5 1 d PD E -1 H10M H 0.3741 0.385 0.3272 0.075 Uiso 0.5 1 calc PR E -1 H10N H 0.3602 0.4299 0.3895 0.075 Uiso 0.5 1 calc PR E -1 H10O H 0.3422 0.3389 0.3809 0.075 Uiso 0.5 1 calc PR E -1 C107 C 0.4891(9) 0.3291(9) 0.3876(8) 0.080(5) Uiso 0.5 1 d PD E -1 H10P H 0.4701 0.2837 0.4071 0.121 Uiso 0.5 1 calc PR E -1 H10Q H 0.5463 0.3452 0.4014 0.121 Uiso 0.5 1 calc PR E -1 H10R H 0.4726 0.3174 0.3401 0.121 Uiso 0.5 1 calc PR E -1 N201 N 0.1577(3) 0.6646(3) 0.8130(2) 0.0416(13) Uani 1 1 d . . . H201 H 0.2074 0.6614 0.8105 0.05 Uiso 1 1 calc R . . C204 C 0.1007(4) 0.5923(4) 0.7763(3) 0.055(2) Uani 1 1 d . . . H20A H 0.1145 0.5484 0.7953 0.083 Uiso 1 1 calc R . . H20B H 0.1029 0.5882 0.7306 0.083 Uiso 1 1 calc R . . H20C H 0.0476 0.5932 0.7791 0.083 Uiso 1 1 calc R . . C205 C 0.1418(4) 0.7318(3) 0.7810(3) 0.0473(17) Uani 1 1 d . . . H20D H 0.0879 0.7341 0.7793 0.071 Uiso 1 1 calc R . . H20E H 0.149 0.7266 0.7367 0.071 Uiso 1 1 calc R . . H20F H 0.178 0.7786 0.8059 0.071 Uiso 1 1 calc R . . C201 C 0.1585(4) 0.6765(4) 0.8834(3) 0.0537(19) Uani 1 1 d . . . H20G H 0.1056 0.6786 0.8876 0.064 Uiso 1 1 calc R . . H20H H 0.1952 0.726 0.9037 0.064 Uiso 1 1 calc R . . C202 C 0.1826(4) 0.6141(4) 0.9188(3) 0.064(2) Uani 1 1 d . . . H20I H 0.1348 0.5744 0.9182 0.077 Uiso 1 1 calc R . . H20J H 0.2139 0.5907 0.8944 0.077 Uiso 1 1 calc R . . C203 C 0.2268(7) 0.6364(6) 0.9847(4) 0.128(4) Uani 1 1 d D . . H20K H 0.2813 0.663 0.9856 0.154 Uiso 1 1 calc R . . H20L H 0.2282 0.5904 1.0066 0.154 Uiso 1 1 calc R . . N202 N 0.1911(6) 0.6885(6) 1.0210(5) 0.117(3) Uiso 1 1 d . . . C206 C 0.2446(16) 0.7233(8) 1.0785(7) 0.356(17) Uani 1 1 d D . . H20M H 0.2266 0.7644 1.0979 0.534 Uiso 1 1 calc R . . H20N H 0.2956 0.7444 1.0696 0.534 Uiso 1 1 calc R . . H20O H 0.2497 0.6857 1.1087 0.534 Uiso 1 1 calc R . . C207 C 0.1313(10) 0.6468(10) 1.0337(8) 0.201(8) Uiso 1 1 d . . . H20P H 0.1477 0.6207 1.0709 0.301 Uiso 1 1 calc R . . H20Q H 0.1026 0.609 0.9958 0.301 Uiso 1 1 calc R . . H20R H 0.0973 0.6784 1.0441 0.301 Uiso 1 1 calc R . . N301 N 0.0112(2) 0.3701(2) 0.4384(2) 0.0290(11) Uani 1 1 d . . . H301 H 0.0646 0.3743 0.4446 0.035 Uiso 1 1 calc R . . C304 C -0.0059(3) 0.3738(3) 0.5034(3) 0.0385(15) Uani 1 1 d . . . H30A H -0.0603 0.376 0.4989 0.058 Uiso 1 1 calc R . . H30B H 0.0291 0.4194 0.5312 0.058 Uiso 1 1 calc R . . H30C H 0.0023 0.3284 0.523 0.058 Uiso 1 1 calc R . . C305 C -0.0067(3) 0.4359(3) 0.4055(3) 0.0316(13) Uani 1 1 d . . . H30D H -0.0614 0.4362 0.4026 0.047 Uiso 1 1 calc R . . H30E H 0.002 0.4311 0.3617 0.047 Uiso 1 1 calc R . . H30F H 0.0277 0.4836 0.4306 0.047 Uiso 1 1 calc R . . C301 C -0.0317(3) 0.2964(3) 0.3948(3) 0.0334(14) Uani 1 1 d . G . H30G H -0.0886 0.291 0.3881 0.04 Uiso 1 1 calc R . . H30H H -0.0193 0.2996 0.3519 0.04 Uiso 1 1 calc R . . C302 C -0.0131(4) 0.2254(3) 0.4197(3) 0.0427(16) Uani 1 1 d . . . H30I H 0.0392 0.2398 0.4503 0.051 Uiso 0.5 1 calc PR F 1 H30J H -0.0517 0.2039 0.4441 0.051 Uiso 0.5 1 calc PR F 1 H31I H 0.0391 0.2228 0.4141 0.051 Uiso 0.5 1 calc PR F 2 H31J H -0.0109 0.2288 0.4667 0.051 Uiso 0.5 1 calc PR F 2 C303 C -0.0138(6) 0.1652(6) 0.3672(5) 0.036(3) Uiso 0.5 1 d P G 1 H30K H 0.0325 0.1815 0.3495 0.044 Uiso 0.5 1 calc PR G 1 H30L H -0.0109 0.1174 0.3859 0.044 Uiso 0.5 1 calc PR G 1 C313 C -0.0718(8) 0.1545(8) 0.3854(6) 0.054(3) Uiso 0.5 1 d P G 2 H31A H -0.0534 0.1098 0.3994 0.065 Uiso 0.5 1 calc PR G 2 H31B H -0.1219 0.1524 0.3975 0.065 Uiso 0.5 1 calc PR G 2 N302 N -0.0847(3) 0.1511(3) 0.3150(3) 0.0486(15) Uani 1 1 d D . . C306 C -0.1483(8) 0.1225(8) 0.3354(6) 0.059(4) Uani 0.5 1 d P G 1 H30M H -0.1946 0.1124 0.2989 0.088 Uiso 0.5 1 calc PR G 1 H30N H -0.1532 0.1591 0.3695 0.088 Uiso 0.5 1 calc PR G 1 H30O H -0.1441 0.0749 0.3528 0.088 Uiso 0.5 1 calc PR G 1 C307 C -0.0584(9) 0.1128(7) 0.2683(7) 0.090(4) Uani 0.5 1 d PD G 1 H30P H -0.0421 0.0689 0.2852 0.135 Uiso 0.5 1 calc PR G 1 H30Q H -0.0138 0.1474 0.2581 0.135 Uiso 0.5 1 calc PR G 1 H30R H -0.1007 0.0953 0.2287 0.135 Uiso 0.5 1 calc PR G 1 C316 C -0.1543(10) 0.0972(11) 0.2941(10) 0.095(6) Uiso 0.5 1 d PD G 2 H31C H -0.1745 0.0962 0.2473 0.142 Uiso 0.5 1 calc PR G 2 H31D H -0.192 0.1095 0.3172 0.142 Uiso 0.5 1 calc PR G 2 H31E H -0.1462 0.0471 0.3028 0.142 Uiso 0.5 1 calc PR G 2 C317 C -0.0221(18) 0.125(3) 0.304(2) 0.31(3) Uiso 0.5 1 d PD G 2 H31F H 0.0267 0.164 0.3228 0.466 Uiso 0.5 1 calc PR G 2 H31G H -0.0281 0.1141 0.2569 0.466 Uiso 0.5 1 calc PR G 2 H31H H -0.0205 0.0784 0.3237 0.466 Uiso 0.5 1 calc PR G 2 N011 N 0.3860(7) 0.3639(7) 0.7121(6) 0.205(6) Uiso 1 1 d D . . C011 C 0.3329(7) 0.3238(8) 0.7328(7) 0.159(6) Uiso 1 1 d D . . C012 C 0.2595(5) 0.2775(5) 0.7481(4) 0.089(3) Uiso 1 1 d D . . H01A H 0.2468 0.3062 0.7833 0.134 Uiso 1 1 calc R . . H01B H 0.2684 0.2293 0.7615 0.134 Uiso 1 1 calc R . . H01C H 0.216 0.2671 0.7093 0.134 Uiso 1 1 calc R . . N021 N -0.0399(7) 0.5742(8) 0.8815(6) 0.183(6) Uani 1 1 d . . . C021 C -0.0742(6) 0.5231(7) 0.8456(5) 0.097(4) Uani 1 1 d . . . C022 C -0.1185(5) 0.4548(5) 0.7983(4) 0.095(3) Uani 1 1 d . . . H02A H -0.0957 0.412 0.8084 0.142 Uiso 1 1 calc R . . H02B H -0.116 0.4655 0.7543 0.142 Uiso 1 1 calc R . . H02C H -0.1733 0.4419 0.8009 0.142 Uiso 1 1 calc R . . N031 N 0.5119(7) 0.7634(7) 0.4742(7) 0.210(6) Uiso 1 1 d D . . C031 C 0.4698(6) 0.8113(6) 0.4747(6) 0.124(4) Uiso 1 1 d D . . C032 C 0.4188(6) 0.8667(6) 0.4669(5) 0.109(4) Uiso 1 1 d D . . H03A H 0.4307 0.8981 0.4333 0.163 Uiso 1 1 calc R . . H03B H 0.4289 0.8994 0.5082 0.163 Uiso 1 1 calc R . . H03C H 0.3636 0.8384 0.4541 0.163 Uiso 1 1 calc R . . N041 N 0.7106(9) 0.8215(9) 0.9117(8) 0.230(7) Uiso 1 1 d . . . C041 C 0.6438(8) 0.7884(8) 0.8943(7) 0.143(5) Uiso 1 1 d . . . C042 C 0.5697(5) 0.7492(5) 0.8569(4) 0.079(3) Uiso 1 1 d . . . H04A H 0.5717 0.7391 0.8115 0.119 Uiso 1 1 calc R . . H04B H 0.5324 0.7801 0.8597 0.119 Uiso 1 1 calc R . . H04C H 0.5529 0.7008 0.8733 0.119 Uiso 1 1 calc R . . N051 N 0.1712(9) 0.8895(12) 0.9259(9) 0.150(8) Uiso 0.5 1 d PD H 1 C051 C 0.2262(11) 0.9205(16) 0.9029(11) 0.173(13) Uiso 0.5 1 d PD H 1 C052 C 0.2802(10) 0.9481(12) 0.8613(9) 0.108(7) Uiso 0.5 1 d PD H 1 H05A H 0.2937 1.0039 0.8665 0.161 Uiso 0.5 1 calc PR H 1 H05B H 0.2545 0.9281 0.8157 0.161 Uiso 0.5 1 calc PR H 1 H05C H 0.3279 0.9305 0.8744 0.161 Uiso 0.5 1 calc PR H 1 N061 N 0.2567(9) 1.1040(10) 0.8079(11) 0.144(8) Uiso 0.5 1 d PD I 2 C061 C 0.3073(9) 1.0646(9) 0.8074(10) 0.099(6) Uiso 0.5 1 d PD I 2 C062 C 0.3491(7) 1.0025(7) 0.8057(7) 0.054(3) Uiso 0.5 1 d PD I 2 H06A H 0.3304 0.9644 0.8325 0.081 Uiso 0.5 1 calc PR I 2 H06B H 0.4055 1.0242 0.8226 0.081 Uiso 0.5 1 calc PR I 2 H06C H 0.3387 0.9784 0.7608 0.081 Uiso 0.5 1 calc PR I 2 O1 O 0.4339(4) 0.4936(6) 0.6673(4) 0.188(3) Uani 1 1 d D . . O2 O 0.0937(2) 0.5828(3) 0.3524(2) 0.0588(14) Uani 1 1 d . . . O3 O 0.6016(6) 0.7095(6) 0.6986(5) 0.0513(13) Uani 0.5 1 d P . . O3' O 0.6039(7) 0.7102(6) 0.7051(6) 0.0513(13) Uani 0.5 1 d P . . O4 O 0.5577(12) 0.2785(12) 0.7630(10) 0.170(8) Uiso 0.5 1 d P . . O5 O 0.4687(11) 0.8728(11) 0.2753(9) 0.159(7) Uiso 0.5 1 d P . . O6 O -0.0473(8) 0.7713(8) 0.8548(7) 0.115(5) Uiso 0.5 1 d P . . O7 O 0.1433(14) 0.8476(14) 0.9705(12) 0.215(10) Uiso 0.5 1 d P J 2 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 0.02382(8) 0.02749(9) 0.03332(10) 0.00288(8) 0.00575(7) 0.01133(7) U2 0.02885(10) 0.03373(10) 0.03694(11) -0.00001(9) 0.00241(8) 0.01429(8) O0 0.0245(16) 0.0275(17) 0.0346(19) 0.0062(14) 0.0045(14) 0.0125(13) O101 0.0304(18) 0.0338(19) 0.058(2) -0.0069(18) 0.0108(17) 0.0123(16) O102 0.0286(17) 0.0362(19) 0.036(2) -0.0025(16) 0.0065(15) 0.0150(15) O201 0.0355(19) 0.044(2) 0.049(2) -0.0056(19) 0.0042(18) 0.0173(17) O202 0.0319(18) 0.0313(18) 0.042(2) 0.0071(16) 0.0058(16) 0.0132(15) O11 0.0406(19) 0.0301(18) 0.038(2) 0.0082(15) 0.0137(16) 0.0154(15) C11 0.040(3) 0.029(2) 0.038(3) 0.010(2) 0.017(2) 0.019(2) C12 0.047(3) 0.025(2) 0.043(3) 0.010(2) 0.018(2) 0.016(2) C13 0.057(3) 0.039(3) 0.052(3) 0.017(2) 0.035(2) 0.029(2) C14 0.058(3) 0.048(3) 0.041(3) 0.018(2) 0.028(2) 0.028(3) C141 0.080(4) 0.063(4) 0.049(3) 0.023(3) 0.038(3) 0.040(3) C142 0.075(4) 0.104(6) 0.062(4) -0.002(4) 0.040(3) 0.035(4) C143 0.133(6) 0.107(6) 0.067(4) 0.046(4) 0.060(4) 0.060(5) C144 0.100(5) 0.063(4) 0.049(4) 0.003(3) 0.041(3) 0.026(4) C15 0.046(3) 0.045(3) 0.031(3) 0.003(2) 0.008(2) 0.021(3) C16 0.048(3) 0.033(3) 0.024(2) 0.013(2) 0.008(2) 0.016(2) C1 0.051(3) 0.027(3) 0.024(3) 0.013(2) 0.002(2) -0.008(2) O21 0.0384(18) 0.0264(17) 0.040(2) 0.0066(15) 0.0137(16) 0.0142(15) C21 0.048(3) 0.033(3) 0.048(3) 0.017(2) 0.025(2) 0.020(2) C22 0.055(3) 0.037(3) 0.044(3) 0.017(2) 0.021(3) 0.023(2) C23 0.096(4) 0.050(3) 0.056(4) 0.023(3) 0.037(3) 0.050(3) C24 0.125(5) 0.052(3) 0.044(3) 0.029(3) 0.047(3) 0.049(3) C241 0.165(7) 0.052(4) 0.055(4) 0.017(3) 0.049(5) 0.045(5) C242 0.154(11) 0.179(10) 0.113(8) 0.093(7) -0.001(8) 0.045(9) C244 0.340(12) 0.170(7) 0.092(5) 0.098(5) 0.127(6) 0.179(7) C25 0.096(4) 0.037(3) 0.058(3) 0.024(3) 0.050(3) 0.027(3) C26 0.055(3) 0.030(3) 0.054(3) 0.015(2) 0.032(3) 0.016(2) C2 0.050(3) 0.032(3) 0.065(4) 0.009(3) 0.036(3) 0.008(3) O31 0.0381(19) 0.0238(17) 0.046(2) 0.0051(16) 0.0100(17) 0.0112(15) C31 0.051(3) 0.026(2) 0.047(3) 0.007(2) 0.031(2) 0.014(2) C32 0.050(3) 0.046(3) 0.056(3) 0.008(3) 0.033(3) 0.017(3) C33 0.094(4) 0.029(3) 0.082(4) -0.004(3) 0.065(3) -0.004(3) C34 0.110(4) 0.044(3) 0.069(4) 0.032(3) 0.060(3) 0.043(3) C341 0.141(6) 0.044(4) 0.099(5) 0.035(3) 0.073(5) 0.044(4) C342 0.171(8) 0.056(4) 0.148(9) 0.034(5) 0.068(7) 0.062(5) C343 0.138(7) 0.078(5) 0.231(10) 0.105(5) 0.106(7) 0.052(5) C344 0.151(10) 0.049(5) 0.140(9) 0.023(6) 0.004(8) 0.019(6) C35 0.082(4) 0.038(3) 0.057(4) 0.020(3) 0.038(3) 0.033(3) C36 0.055(3) 0.036(3) 0.049(3) 0.022(2) 0.033(2) 0.025(2) C3 0.050(3) 0.043(3) 0.051(3) 0.023(2) 0.030(2) 0.033(2) O41 0.0363(19) 0.041(2) 0.040(2) 0.0036(17) 0.0047(17) 0.0133(17) C41 0.038(3) 0.027(3) 0.065(4) -0.009(3) 0.014(3) 0.009(2) C42 0.052(3) 0.024(3) 0.057(4) -0.003(3) -0.007(3) 0.019(2) C43 0.060(4) 0.036(3) 0.066(4) -0.006(3) 0.012(3) 0.024(3) C44 0.048(4) 0.042(4) 0.080(5) -0.016(3) 0.013(4) 0.001(3) C441 0.089(6) 0.065(5) 0.129(8) -0.046(5) 0.025(6) 0.003(5) C46 0.050(3) 0.037(3) 0.074(4) 0.000(3) 0.023(3) 0.015(3) C4 0.042(3) 0.035(3) 0.081(5) -0.005(3) 0.030(3) 0.000(3) O51 0.0351(18) 0.0325(18) 0.033(2) 0.0034(15) -0.0047(16) 0.0158(15) C51 0.036(3) 0.039(3) 0.035(3) 0.002(2) -0.001(2) 0.011(2) C52 0.040(3) 0.033(3) 0.037(3) 0.005(2) -0.001(2) 0.018(2) C53 0.040(3) 0.039(3) 0.052(4) 0.008(3) -0.005(3) 0.019(2) C54 0.040(3) 0.044(3) 0.039(3) -0.006(3) -0.010(3) 0.016(3) C541 0.063(4) 0.057(4) 0.053(4) -0.004(3) -0.014(3) 0.024(3) C55 0.044(3) 0.043(3) 0.047(4) -0.006(3) -0.001(3) 0.007(3) C56 0.043(3) 0.031(3) 0.040(3) -0.003(2) 0.002(2) 0.019(2) C5 0.055(3) 0.028(3) 0.035(3) 0.005(2) 0.012(3) 0.015(2) O61 0.0328(18) 0.0238(16) 0.0343(19) 0.0067(15) 0.0046(15) 0.0090(14) C61 0.049(3) 0.026(2) 0.026(3) 0.003(2) 0.001(2) 0.020(2) C62 0.041(3) 0.028(2) 0.031(3) 0.010(2) 0.004(2) 0.015(2) C63 0.044(3) 0.036(3) 0.036(3) 0.007(2) 0.011(2) 0.010(2) C64 0.061(3) 0.037(3) 0.034(3) 0.012(2) 0.012(3) 0.020(3) C641 0.081(5) 0.061(4) 0.040(3) 0.022(3) 0.019(3) 0.008(4) C65 0.072(4) 0.034(3) 0.028(3) 0.004(2) 0.003(3) 0.018(3) C66 0.049(3) 0.021(2) 0.033(3) -0.001(2) -0.003(2) 0.011(2) C6 0.042(3) 0.035(3) 0.042(3) 0.002(2) -0.001(3) 0.018(2) O71 0.040(2) 0.0210(16) 0.0220(17) -0.0009(14) -0.0081(15) 0.0048(15) C71 0.040(3) 0.021(2) 0.028(3) 0.008(2) -0.001(2) 0.009(2) C72 0.048(3) 0.024(2) 0.024(3) 0.006(2) -0.003(2) 0.015(2) C73 0.058(3) 0.025(2) 0.030(3) 0.010(2) -0.005(3) 0.017(2) C74 0.044(3) 0.028(3) 0.036(3) 0.011(2) -0.002(2) 0.011(2) C741 0.062(4) 0.029(3) 0.053(4) 0.014(3) 0.008(3) 0.006(3) C742 0.125(7) 0.060(4) 0.049(4) 0.032(3) 0.003(5) -0.025(5) C743 0.082(5) 0.032(4) 0.138(8) 0.014(4) 0.033(5) 0.012(4) C744 0.057(4) 0.049(4) 0.062(4) 0.018(3) 0.001(4) 0.003(3) C75 0.039(3) 0.033(3) 0.029(3) 0.012(2) 0.001(2) 0.010(2) C76 0.043(3) 0.031(3) 0.026(3) 0.005(2) -0.003(2) 0.014(2) C7 0.033(3) 0.035(3) 0.030(3) 0.003(2) 0.001(2) 0.013(2) O81 0.0249(16) 0.0256(16) 0.0349(19) 0.0053(14) 0.0066(14) 0.0115(13) C81 0.033(2) 0.024(2) 0.032(3) 0.002(2) 0.010(2) 0.008(2) C82 0.032(2) 0.025(2) 0.028(3) 0.0094(19) 0.005(2) 0.0132(19) C83 0.045(3) 0.024(2) 0.034(3) -0.003(2) 0.006(2) 0.009(2) C84 0.089(4) 0.043(3) 0.047(4) -0.006(3) 0.007(3) 0.042(3) C85 0.100(4) 0.038(3) 0.043(3) 0.010(2) 0.011(3) 0.048(3) C86 0.047(3) 0.033(3) 0.048(3) 0.010(2) 0.012(3) 0.020(2) C8 0.049(3) 0.032(3) 0.033(3) 0.005(2) -0.005(2) 0.024(2) N201 0.047(3) 0.048(3) 0.035(3) 0.009(2) 0.008(2) 0.024(2) C204 0.058(4) 0.066(4) 0.040(3) 0.002(3) 0.016(3) 0.009(3) C205 0.049(3) 0.052(3) 0.052(4) 0.019(3) 0.011(3) 0.032(3) C201 0.078(4) 0.058(4) 0.030(3) 0.008(3) 0.014(3) 0.027(3) C202 0.098(4) 0.071(4) 0.050(4) 0.034(3) 0.031(3) 0.055(3) C203 0.177(10) 0.148(8) 0.085(6) 0.067(6) 0.025(7) 0.083(7) C206 0.73(5) 0.103(10) 0.136(13) -0.048(10) -0.08(2) 0.121(18) N301 0.029(2) 0.031(2) 0.030(2) 0.0059(17) 0.0053(17) 0.0146(17) C304 0.038(3) 0.047(3) 0.033(3) 0.008(2) 0.006(2) 0.019(2) C305 0.035(2) 0.028(2) 0.030(3) 0.004(2) -0.002(2) 0.015(2) C301 0.037(3) 0.028(2) 0.035(3) 0.009(2) 0.005(2) 0.010(2) C302 0.045(3) 0.040(3) 0.044(3) 0.010(3) 0.005(3) 0.016(3) N302 0.065(3) 0.034(3) 0.043(3) 0.005(2) 0.010(3) 0.010(2) C306 0.070(9) 0.059(9) 0.037(7) 0.000(6) 0.005(7) 0.006(7) C307 0.168(9) 0.076(6) 0.104(9) 0.070(6) 0.102(7) 0.102(6) N021 0.116(9) 0.220(14) 0.168(11) -0.010(10) -0.002(8) -0.001(9) C021 0.083(6) 0.144(9) 0.072(6) 0.045(6) 0.028(5) 0.027(6) C022 0.126(6) 0.114(5) 0.092(5) 0.064(4) 0.053(5) 0.084(5) O1 0.183(5) 0.340(9) 0.143(6) 0.099(6) 0.080(5) 0.208(5) O2 0.044(2) 0.069(3) 0.074(3) 0.031(2) 0.013(2) 0.028(2) O3 0.051(2) 0.034(2) 0.064(3) -0.015(2) 0.018(2) 0.0039(19) O3' 0.051(2) 0.034(2) 0.064(3) -0.015(2) 0.018(2) 0.0039(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O101 1.786(4) . ? U1 O102 1.801(4) . ? U1 O11 2.250(4) . ? U1 O81 2.283(3) . ? U1 O0 2.337(3) . ? U1 O21 2.489(3) . ? U2 O201 1.793(4) . ? U2 O202 1.797(4) . ? U2 O41 2.205(4) . ? U2 O51 2.291(4) . ? U2 O0 2.363(3) . ? U2 O61 2.564(3) . ? O0 H0 0.95 . ? O11 C11 1.350(7) . ? C11 C12 1.380(8) . ? C11 C16 1.405(7) . ? C12 C13 1.396(8) . ? C12 C2 1.518(7) . ? C13 C14 1.385(8) . ? C13 H13 0.95 . ? C14 C15 1.376(8) . ? C14 C141 1.562(9) . ? C141 C142 1.493(10) . ? C141 C144 1.542(9) . ? C141 C143 1.573(11) . ? C142 H14A 0.98 . ? C142 H14B 0.98 . ? C142 H14C 0.98 . ? C143 H14D 0.98 . ? C143 H14E 0.98 . ? C143 H14F 0.98 . ? C144 H14G 0.98 . ? C144 H14H 0.98 . ? C144 H14I 0.98 . ? C15 C16 1.384(8) . ? C15 H15 0.95 . ? C16 C1 1.481(8) . ? C1 C82 1.527(7) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? O21 C21 1.362(7) . ? C21 C26 1.390(9) . ? C21 C22 1.418(8) . ? C22 C23 1.373(9) . ? C22 C3 1.523(8) . ? C23 C24 1.408(10) . ? C23 H23 0.95 . ? C24 C25 1.357(10) . ? C24 C241 1.530(10) . ? C241 C243 1.476(14) . ? C241 C242 1.491(14) . ? C241 C244 1.569(14) . ? C242 H24A 0.98 . ? C242 H24B 0.98 . ? C242 H24C 0.98 . ? C243 H24D 0.98 . ? C243 H24E 0.98 . ? C243 H24F 0.98 . ? C244 H24G 0.98 . ? C244 H24H 0.98 . ? C244 H24I 0.98 . ? C25 C26 1.408(9) . ? C25 H25 0.95 . ? C26 C2 1.514(9) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O31 C31 1.376(6) . ? O31 H31 0.84 . ? C31 C32 1.388(8) . ? C31 C36 1.403(8) . ? C32 C33 1.450(9) . ? C32 C4 1.534(9) . ? C33 C34 1.367(10) . ? C33 H33 0.95 . ? C34 C35 1.350(9) . ? C34 C341 1.527(10) . ? C341 C342 1.348(12) . ? C341 C343 1.400(13) . ? C341 C344 1.644(13) . ? C342 H34A 0.98 . ? C342 H34B 0.98 . ? C342 H34C 0.98 . ? C343 H34D 0.98 . ? C343 H34E 0.98 . ? C343 H34F 0.98 . ? C344 H34G 0.98 . ? C344 H34H 0.98 . ? C344 H34I 0.98 . ? C35 C36 1.414(8) . ? C35 H35 0.95 . ? C36 C3 1.488(7) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O41 C41 1.333(6) . ? C41 C42 1.394(9) . ? C41 C46 1.398(9) . ? C42 C43 1.408(8) . ? C42 C5 1.482(9) . ? C43 C44 1.407(10) . ? C43 H43 0.95 . ? C44 C45 1.381(10) . ? C44 C441 1.545(9) . ? C441 C447 1.496(13) . ? C441 C442 1.499(14) . ? C441 C446 1.530(13) . ? C441 C443 1.539(16) . ? C441 C444 1.565(14) . ? C441 C445 1.590(14) . ? C442 H44A 0.98 . ? C442 H44B 0.98 . ? C442 H44C 0.98 . ? C443 H44D 0.98 . ? C443 H44E 0.98 . ? C443 H44F 0.98 . ? C444 H44G 0.98 . ? C444 H44H 0.98 . ? C444 H44I 0.98 . ? C445 H44J 0.98 . ? C445 H44K 0.98 . ? C445 H44L 0.98 . ? C446 H44M 0.98 . ? C446 H44N 0.98 . ? C446 H44O 0.98 . ? C447 H44P 0.98 . ? C447 H44Q 0.98 . ? C447 H44R 0.98 . ? C45 C46 1.431(9) . ? C45 H45 0.95 . ? C46 C4 1.481(10) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? O51 C51 1.378(6) . ? C51 C56 1.401(8) . ? C51 C52 1.406(8) . ? C52 C53 1.402(8) . ? C52 C6 1.500(8) . ? C53 C54 1.350(8) . ? C53 H53 0.95 . ? C54 C55 1.384(9) . ? C54 C541 1.543(9) . ? C541 C545 1.32(3) . ? C541 C543 1.443(14) . ? C541 C544 1.538(16) . ? C541 C546 1.56(2) . ? C541 C547 1.57(3) . ? C541 C542 1.570(16) . ? C542 H54A 0.98 . ? C542 H54B 0.98 . ? C542 H54C 0.98 . ? C543 H54D 0.98 . ? C543 H54E 0.98 . ? C543 H54F 0.98 . ? C544 H54G 0.98 . ? C544 H54H 0.98 . ? C544 H54I 0.98 . ? C545 H54J 0.98 . ? C545 H54K 0.98 . ? C545 H54L 0.98 . ? C546 H54M 0.98 . ? C546 H54N 0.98 . ? C546 H54O 0.98 . ? C547 H54P 0.98 . ? C547 H54Q 0.98 . ? C547 H54R 0.98 . ? C55 C56 1.405(8) . ? C55 H55 0.95 . ? C56 C5 1.509(8) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? O61 C61 1.363(7) . ? C61 C66 1.409(7) . ? C61 C62 1.423(7) . ? C62 C63 1.375(8) . ? C62 C7 1.513(7) . ? C63 C64 1.397(8) . ? C63 H63 0.95 . ? C64 C65 1.412(9) . ? C64 C641 1.517(9) . ? C641 C645 1.409(19) . ? C641 C647 1.51(2) . ? C641 C642 1.541(17) . ? C641 C644 1.585(18) . ? C641 C643 1.592(18) . ? C641 C646 1.66(2) . ? C642 H64A 0.98 . ? C642 H64B 0.98 . ? C642 H64C 0.98 . ? C643 H64D 0.98 . ? C643 H64E 0.98 . ? C643 H64F 0.98 . ? C644 H64G 0.98 . ? C644 H64H 0.98 . ? C644 H64I 0.98 . ? C645 H64J 0.98 . ? C645 H64K 0.98 . ? C645 H64L 0.98 . ? C646 H64M 0.98 . ? C646 H64N 0.98 . ? C646 H64O 0.98 . ? C647 H64P 0.98 . ? C647 H64Q 0.98 . ? C647 H64R 0.98 . ? C65 C66 1.386(9) . ? C65 H65 0.95 . ? C66 C6 1.508(8) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O71 C71 1.361(6) . ? O71 H71 0.84 . ? C71 C76 1.390(8) . ? C71 C72 1.408(8) . ? C72 C73 1.386(7) . ? C72 C8 1.516(9) . ? C73 C74 1.381(9) . ? C73 H73 0.95 . ? C74 C75 1.433(8) . ? C74 C741 1.519(8) . ? C741 C744 1.515(9) . ? C741 C743 1.562(11) . ? C741 C742 1.569(10) . ? C742 H74A 0.98 . ? C742 H74B 0.98 . ? C742 H74C 0.98 . ? C743 H74D 0.98 . ? C743 H74E 0.98 . ? C743 H74F 0.98 . ? C744 H74G 0.98 . ? C744 H74H 0.98 . ? C744 H74I 0.98 . ? C75 C76 1.385(7) . ? C75 H75 0.95 . ? C76 C7 1.529(8) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? O81 C81 1.384(6) . ? C81 C82 1.391(7) . ? C81 C86 1.394(8) . ? C82 C83 1.415(7) . ? C83 C84 1.376(8) . ? C83 H83 0.95 . ? C84 C85 1.400(9) . ? C84 C841 1.544(12) . ? C84 C845 1.613(18) . ? C841 C842 1.504(13) . ? C841 C843 1.510(13) . ? C841 C844 1.564(14) . ? C842 H84A 0.98 . ? C842 H84B 0.98 . ? C842 H84C 0.98 . ? C843 H84D 0.98 . ? C843 H84E 0.98 . ? C843 H84F 0.98 . ? C844 H84G 0.98 . ? C844 H84H 0.98 . ? C844 H84I 0.98 . ? C845 C848 1.503(17) . ? C845 C846 1.517(17) . ? C845 C847 1.521(17) . ? C846 H84J 0.98 . ? C846 H84K 0.98 . ? C846 H84L 0.98 . ? C847 H84M 0.98 . ? C847 H84N 0.98 . ? C847 H84O 0.98 . ? C848 H84P 0.98 . ? C848 H84Q 0.98 . ? C848 H84R 0.98 . ? C85 C86 1.410(8) . ? C85 H85 0.95 . ? C86 C8 1.490(8) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? N101 C104 1.500(19) . ? N101 C101 1.504(18) . ? N101 C105 1.53(2) . ? N101 H101 0.93 . ? C104 H10A 0.98 . ? C104 H10B 0.98 . ? C104 H10C 0.98 . ? C105 H10D 0.98 . ? C105 H10E 0.98 . ? C105 H10F 0.98 . ? C101 C102 1.386(12) . ? C101 H10G 0.99 . ? C101 H10H 0.99 . ? C102 C103 1.456(12) . ? C102 H10I 0.99 . ? C102 H10J 0.99 . ? C103 N102 1.443(13) . ? C103 H10K 0.99 . ? C103 H10L 0.99 . ? N102 C106 1.447(11) . ? N102 C107 1.469(18) . ? N102 H102 0.93 . ? C106 H10M 0.98 . ? C106 H10N 0.98 . ? C106 H10O 0.98 . ? C107 H10P 0.98 . ? C107 H10Q 0.98 . ? C107 H10R 0.98 . ? N201 C201 1.494(8) . ? N201 C205 1.497(8) . ? N201 C204 1.509(8) . ? N201 H201 0.93 . ? C204 H20A 0.98 . ? C204 H20B 0.98 . ? C204 H20C 0.98 . ? C205 H20D 0.98 . ? C205 H20E 0.98 . ? C205 H20F 0.98 . ? C201 C202 1.503(9) . ? C201 H20G 0.99 . ? C201 H20H 0.99 . ? C202 C203 1.430(11) . ? C202 H20I 0.99 . ? C202 H20J 0.99 . ? C203 N202 1.519(15) . ? C203 H20K 0.99 . ? C203 H20L 0.99 . ? N202 C207 1.268(18) . ? N202 C206 1.384(18) . ? C206 H20M 0.98 . ? C206 H20N 0.98 . ? C206 H20O 0.98 . ? C207 H20P 0.98 . ? C207 H20Q 0.98 . ? C207 H20R 0.98 . ? N301 C304 1.482(7) . ? N301 C305 1.495(7) . ? N301 C301 1.512(6) . ? N301 H301 0.93 . ? C304 H30A 0.98 . ? C304 H30B 0.98 . ? C304 H30C 0.98 . ? C305 H30D 0.98 . ? C305 H30E 0.98 . ? C305 H30F 0.98 . ? C301 C302 1.511(8) . ? C301 H30G 0.99 . ? C301 H30H 0.99 . ? C302 C313 1.489(13) . ? C302 C303 1.500(13) . ? C302 H30I 0.99 . ? C302 H30J 0.99 . ? C302 H31I 0.99 . ? C302 H31J 0.99 . ? C303 N302 1.458(11) . ? C303 H30K 0.99 . ? C303 H30L 0.99 . ? C313 N302 1.459(14) . ? C313 H31A 0.99 . ? C313 H31B 0.99 . ? N302 C306 1.330(16) . ? N302 C316 1.369(17) . ? N302 C317 1.38(3) . ? N302 C307 1.400(15) . ? C306 H30M 0.98 . ? C306 H30N 0.98 . ? C306 H30O 0.98 . ? C307 H30P 0.98 . ? C307 H30Q 0.98 . ? C307 H30R 0.98 . ? C316 H31C 0.98 . ? C316 H31D 0.98 . ? C316 H31E 0.98 . ? C317 H31F 0.98 . ? C317 H31G 0.98 . ? C317 H31H 0.98 . ? N011 C011 1.252(13) . ? C011 C012 1.518(13) . ? C012 H01A 0.98 . ? C012 H01B 0.98 . ? C012 H01C 0.98 . ? N021 C021 1.119(15) . ? C021 C022 1.483(13) . ? C022 H02A 0.98 . ? C022 H02B 0.98 . ? C022 H02C 0.98 . ? N031 C031 1.283(14) . ? C031 C032 1.511(13) . ? C032 H03A 0.98 . ? C032 H03B 0.98 . ? C032 H03C 0.98 . ? N041 C041 1.183(19) . ? C041 C042 1.395(14) . ? C042 H04A 0.98 . ? C042 H04B 0.98 . ? C042 H04C 0.98 . ? N051 C051 1.245(19) . ? C051 C052 1.49(2) . ? C052 H05A 0.98 . ? C052 H05B 0.98 . ? C052 H05C 0.98 . ? N061 C061 1.288(18) . ? C061 C062 1.499(17) . ? C062 H06A 0.98 . ? C062 H06B 0.98 . ? C062 H06C 0.98 . ? 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 O101 U1 O102 178.87(18) . . ? O101 U1 O11 88.66(17) . . ? O102 U1 O11 92.03(15) . . ? O101 U1 O81 89.46(14) . . ? O102 U1 O81 89.82(14) . . ? O11 U1 O81 76.96(13) . . ? O101 U1 O0 85.71(15) . . ? O102 U1 O0 94.27(14) . . ? O11 U1 O0 142.48(12) . . ? O81 U1 O0 139.90(12) . . ? O101 U1 O21 93.05(15) . . ? O102 U1 O21 87.99(14) . . ? O11 U1 O21 75.05(12) . . ? O81 U1 O21 151.82(12) . . ? O0 U1 O21 68.27(12) . . ? O201 U2 O202 177.03(17) . . ? O201 U2 O41 88.95(16) . . ? O202 U2 O41 93.95(15) . . ? O201 U2 O51 90.33(17) . . ? O202 U2 O51 89.56(16) . . ? O41 U2 O51 78.82(14) . . ? O201 U2 O0 84.79(15) . . ? O202 U2 O0 93.34(14) . . ? O41 U2 O0 141.70(14) . . ? O51 U2 O0 138.79(12) . . ? O201 U2 O61 91.29(15) . . ? O202 U2 O61 85.83(14) . . ? O41 U2 O61 152.16(14) . . ? O51 U2 O61 73.34(12) . . ? O0 U2 O61 65.91(12) . . ? U1 O0 U2 146.06(16) . . ? U1 O0 H0 107 . . ? U2 O0 H0 107 . . ? C11 O11 U1 139.3(3) . . ? O11 C11 C12 121.3(5) . . ? O11 C11 C16 120.8(5) . . ? C12 C11 C16 117.9(5) . . ? C11 C12 C13 121.5(5) . . ? C11 C12 C2 118.1(5) . . ? C13 C12 C2 120.4(5) . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 116.7(6) . . ? C15 C14 C141 123.8(5) . . ? C13 C14 C141 119.5(5) . . ? C142 C141 C144 110.8(6) . . ? C142 C141 C14 110.6(5) . . ? C144 C141 C14 110.0(5) . . ? C142 C141 C143 110.8(6) . . ? C144 C141 C143 109.1(6) . . ? C14 C141 C143 105.4(6) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C14 C15 C16 123.7(5) . . ? C14 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C15 C16 C11 119.1(5) . . ? C15 C16 C1 120.3(5) . . ? C11 C16 C1 120.4(5) . . ? C16 C1 C82 113.5(5) . . ? C16 C1 H1A 108.9 . . ? C82 C1 H1A 108.9 . . ? C16 C1 H1B 108.9 . . ? C82 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C21 O21 U1 125.9(3) . . ? O21 C21 C26 121.3(5) . . ? O21 C21 C22 119.8(5) . . ? C26 C21 C22 118.9(5) . . ? C23 C22 C21 119.1(6) . . ? C23 C22 C3 120.7(6) . . ? C21 C22 C3 119.7(5) . . ? C22 C23 C24 123.6(6) . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C25 C24 C23 115.3(6) . . ? C25 C24 C241 123.8(7) . . ? C23 C24 C241 120.8(7) . . ? C243 C241 C242 108.6(9) . . ? C243 C241 C24 109.2(7) . . ? C242 C241 C24 109.0(7) . . ? C243 C241 C244 108.5(8) . . ? C242 C241 C244 112.9(8) . . ? C24 C241 C244 108.7(8) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? H24A C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? H24D C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? H24D C243 H24F 109.5 . . ? H24E C243 H24F 109.5 . . ? C241 C244 H24G 109.5 . . ? C241 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C241 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C24 C25 C26 124.4(6) . . ? C24 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C21 C26 C25 118.7(6) . . ? C21 C26 C2 121.1(6) . . ? C25 C26 C2 120.1(6) . . ? C26 C2 C12 111.9(5) . . ? C26 C2 H2A 109.2 . . ? C12 C2 H2A 109.2 . . ? C26 C2 H2B 109.2 . . ? C12 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C31 O31 H31 109.5 . . ? O31 C31 C32 119.5(5) . . ? O31 C31 C36 120.5(5) . . ? C32 C31 C36 120.1(5) . . ? C31 C32 C33 116.5(6) . . ? C31 C32 C4 122.3(6) . . ? C33 C32 C4 121.2(5) . . ? C34 C33 C32 123.8(6) . . ? C34 C33 H33 118.1 . . ? C32 C33 H33 118.1 . . ? C35 C34 C33 117.5(6) . . ? C35 C34 C341 124.9(7) . . ? C33 C34 C341 117.6(6) . . ? C342 C341 C343 121.1(8) . . ? C342 C341 C34 114.5(7) . . ? C343 C341 C34 112.9(8) . . ? C342 C341 C344 97.1(8) . . ? C343 C341 C344 101.2(8) . . ? C34 C341 C344 106.3(6) . . ? C341 C342 H34A 109.5 . . ? C341 C342 H34B 109.5 . . ? H34A C342 H34B 109.5 . . ? C341 C342 H34C 109.5 . . ? H34A C342 H34C 109.5 . . ? H34B C342 H34C 109.5 . . ? C341 C343 H34D 109.5 . . ? C341 C343 H34E 109.5 . . ? H34D C343 H34E 109.5 . . ? C341 C343 H34F 109.5 . . ? H34D C343 H34F 109.5 . . ? H34E C343 H34F 109.5 . . ? C341 C344 H34G 109.5 . . ? C341 C344 H34H 109.5 . . ? H34G C344 H34H 109.5 . . ? C341 C344 H34I 109.5 . . ? H34G C344 H34I 109.5 . . ? H34H C344 H34I 109.5 . . ? C34 C35 C36 122.4(6) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C31 C36 C35 119.6(5) . . ? C31 C36 C3 121.6(5) . . ? C35 C36 C3 118.7(5) . . ? C36 C3 C22 109.9(5) . . ? C36 C3 H3A 109.7 . . ? C22 C3 H3A 109.7 . . ? C36 C3 H3B 109.7 . . ? C22 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C41 O41 U2 143.5(4) . . ? O41 C41 C42 121.4(6) . . ? O41 C41 C46 117.9(6) . . ? C42 C41 C46 120.7(5) . . ? C41 C42 C43 118.9(6) . . ? C41 C42 C5 121.6(5) . . ? C43 C42 C5 119.5(6) . . ? C44 C43 C42 122.9(7) . . ? C44 C43 H43 118.5 . . ? C42 C43 H43 118.5 . . ? C45 C44 C43 116.3(6) . . ? C45 C44 C441 123.9(7) . . ? C43 C44 C441 119.7(7) . . ? C447 C441 C446 111.2(9) . . ? C442 C441 C443 114.1(13) . . ? C447 C441 C44 110.8(7) . . ? C442 C441 C44 113.5(10) . . ? C446 C441 C44 110.9(7) . . ? C443 C441 C44 107.7(9) . . ? C442 C441 C444 107.2(11) . . ? C443 C441 C444 104.4(11) . . ? C44 C441 C444 109.5(8) . . ? C447 C441 C445 111.6(9) . . ? C446 C441 C445 103.6(9) . . ? C44 C441 C445 108.6(8) . . ? C441 C442 H44A 109.5 . . ? C441 C442 H44B 109.5 . . ? C441 C442 H44C 109.5 . . ? C441 C443 H44D 109.5 . . ? C441 C443 H44E 109.5 . . ? C441 C443 H44F 109.5 . . ? C441 C444 H44G 109.5 . . ? C441 C444 H44H 109.5 . . ? C441 C444 H44I 109.5 . . ? C441 C445 H44J 109.5 . . ? C441 C445 H44K 109.5 . . ? H44J C445 H44K 109.5 . . ? C441 C445 H44L 109.5 . . ? H44J C445 H44L 109.5 . . ? H44K C445 H44L 109.5 . . ? C441 C446 H44M 109.5 . . ? C441 C446 H44N 109.5 . . ? H44M C446 H44N 109.5 . . ? C441 C446 H44O 109.5 . . ? H44M C446 H44O 109.5 . . ? H44N C446 H44O 109.5 . . ? C441 C447 H44P 109.5 . . ? C441 C447 H44Q 109.5 . . ? H44P C447 H44Q 109.5 . . ? C441 C447 H44R 109.5 . . ? H44P C447 H44R 109.5 . . ? H44Q C447 H44R 109.5 . . ? C44 C45 C46 123.1(7) . . ? C44 C45 H45 118.4 . . ? C46 C45 H45 118.4 . . ? C41 C46 C45 118.1(7) . . ? C41 C46 C4 121.8(5) . . ? C45 C46 C4 120.1(6) . . ? C46 C4 C32 112.8(6) . . ? C46 C4 H4A 109 . . ? C32 C4 H4A 109 . . ? C46 C4 H4B 109 . . ? C32 C4 H4B 109 . . ? H4A C4 H4B 107.8 . . ? C51 O51 U2 128.6(4) . . ? O51 C51 C56 121.6(5) . . ? O51 C51 C52 118.2(5) . . ? C56 C51 C52 120.2(5) . . ? C53 C52 C51 118.1(5) . . ? C53 C52 C6 121.7(5) . . ? C51 C52 C6 120.2(5) . . ? C54 C53 C52 123.2(6) . . ? C54 C53 H53 118.4 . . ? C52 C53 H53 118.4 . . ? C53 C54 C55 117.9(5) . . ? C53 C54 C541 121.6(6) . . ? C55 C54 C541 120.6(5) . . ? C543 C541 C544 110.0(9) . . ? C545 C541 C54 112.9(12) . . ? C543 C541 C54 116.8(8) . . ? C544 C541 C54 108.2(7) . . ? C545 C541 C546 117.8(15) . . ? C54 C541 C546 111.1(10) . . ? C545 C541 C547 109.2(17) . . ? C54 C541 C547 107.3(10) . . ? C546 C541 C547 96.9(13) . . ? C543 C541 C542 109.3(8) . . ? C544 C541 C542 102.7(9) . . ? C54 C541 C542 108.9(7) . . ? C541 C542 H54A 109.5 . . ? C541 C542 H54B 109.5 . . ? C541 C542 H54C 109.5 . . ? C541 C543 H54D 109.5 . . ? C541 C543 H54E 109.5 . . ? C541 C543 H54F 109.5 . . ? C541 C544 H54G 109.5 . . ? C541 C544 H54H 109.5 . . ? C541 C544 H54I 109.5 . . ? C541 C545 H54J 109.5 . . ? C541 C545 H54K 109.5 . . ? H54J C545 H54K 109.5 . . ? C541 C545 H54L 109.5 . . ? H54J C545 H54L 109.5 . . ? H54K C545 H54L 109.5 . . ? C541 C546 H54M 109.5 . . ? C541 C546 H54N 109.5 . . ? H54M C546 H54N 109.5 . . ? C541 C546 H54O 109.5 . . ? H54M C546 H54O 109.5 . . ? H54N C546 H54O 109.5 . . ? C541 C547 H54P 109.5 . . ? C541 C547 H54Q 109.5 . . ? H54P C547 H54Q 109.5 . . ? C541 C547 H54R 109.5 . . ? H54P C547 H54R 109.5 . . ? H54Q C547 H54R 109.5 . . ? C54 C55 C56 122.7(5) . . ? C54 C55 H55 118.7 . . ? C56 C55 H55 118.7 . . ? C51 C56 C55 117.8(5) . . ? C51 C56 C5 123.0(5) . . ? C55 C56 C5 118.8(5) . . ? C42 C5 C56 113.2(5) . . ? C42 C5 H5A 108.9 . . ? C56 C5 H5A 108.9 . . ? C42 C5 H5B 108.9 . . ? C56 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C61 O61 U2 129.8(3) . . ? O61 C61 C66 121.2(5) . . ? O61 C61 C62 119.7(4) . . ? C66 C61 C62 119.1(5) . . ? C63 C62 C61 119.8(5) . . ? C63 C62 C7 120.6(5) . . ? C61 C62 C7 119.3(5) . . ? C62 C63 C64 122.8(5) . . ? C62 C63 H63 118.6 . . ? C64 C63 H63 118.6 . . ? C63 C64 C65 116.2(6) . . ? C63 C64 C641 121.1(6) . . ? C65 C64 C641 122.6(5) . . ? C645 C641 C647 124.7(13) . . ? C645 C641 C64 107.0(10) . . ? C647 C641 C64 107.9(10) . . ? C64 C641 C642 115.0(9) . . ? C64 C641 C644 108.6(8) . . ? C642 C641 C644 109.4(10) . . ? C64 C641 C643 110.3(8) . . ? C642 C641 C643 103.6(10) . . ? C644 C641 C643 109.8(9) . . ? C645 C641 C646 108.3(12) . . ? C647 C641 C646 100.1(12) . . ? C64 C641 C646 107.7(9) . . ? C641 C642 H64A 109.5 . . ? C641 C642 H64B 109.5 . . ? C641 C642 H64C 109.5 . . ? C641 C643 H64D 109.5 . . ? C641 C643 H64E 109.5 . . ? C641 C643 H64F 109.5 . . ? C641 C644 H64G 109.5 . . ? C641 C644 H64H 109.5 . . ? C641 C644 H64I 109.5 . . ? C641 C645 H64J 109.5 . . ? C641 C645 H64K 109.5 . . ? H64J C645 H64K 109.5 . . ? C641 C645 H64L 109.5 . . ? H64J C645 H64L 109.5 . . ? H64K C645 H64L 109.5 . . ? C641 C646 H64M 109.5 . . ? C641 C646 H64N 109.5 . . ? H64M C646 H64N 109.5 . . ? C641 C646 H64O 109.5 . . ? H64M C646 H64O 109.5 . . ? H64N C646 H64O 109.5 . . ? C641 C647 H64P 109.5 . . ? C641 C647 H64Q 109.5 . . ? H64P C647 H64Q 109.5 . . ? C641 C647 H64R 109.5 . . ? H64P C647 H64R 109.5 . . ? H64Q C647 H64R 109.5 . . ? C66 C65 C64 123.3(5) . . ? C66 C65 H65 118.3 . . ? C64 C65 H65 118.3 . . ? C65 C66 C61 118.7(5) . . ? C65 C66 C6 120.2(5) . . ? C61 C66 C6 121.0(5) . . ? C52 C6 C66 116.9(5) . . ? C52 C6 H6A 108.1 . . ? C66 C6 H6A 108.1 . . ? C52 C6 H6B 108.1 . . ? C66 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C71 O71 H71 109.5 . . ? O71 C71 C76 121.1(5) . . ? O71 C71 C72 120.1(5) . . ? C76 C71 C72 118.8(5) . . ? C73 C72 C71 119.1(6) . . ? C73 C72 C8 119.4(5) . . ? C71 C72 C8 121.4(5) . . ? C74 C73 C72 123.5(5) . . ? C74 C73 H73 118.3 . . ? C72 C73 H73 118.3 . . ? C73 C74 C75 116.8(5) . . ? C73 C74 C741 123.5(5) . . ? C75 C74 C741 119.6(6) . . ? C744 C741 C74 110.0(5) . . ? C744 C741 C743 109.4(6) . . ? C74 C741 C743 111.8(6) . . ? C744 C741 C742 107.7(7) . . ? C74 C741 C742 109.4(5) . . ? C743 C741 C742 108.4(6) . . ? C741 C742 H74A 109.5 . . ? C741 C742 H74B 109.5 . . ? H74A C742 H74B 109.5 . . ? C741 C742 H74C 109.5 . . ? H74A C742 H74C 109.5 . . ? H74B C742 H74C 109.5 . . ? C741 C743 H74D 109.5 . . ? C741 C743 H74E 109.5 . . ? H74D C743 H74E 109.5 . . ? C741 C743 H74F 109.5 . . ? H74D C743 H74F 109.5 . . ? H74E C743 H74F 109.5 . . ? C741 C744 H74G 109.5 . . ? C741 C744 H74H 109.5 . . ? H74G C744 H74H 109.5 . . ? C741 C744 H74I 109.5 . . ? H74G C744 H74I 109.5 . . ? H74H C744 H74I 109.5 . . ? C76 C75 C74 120.2(6) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 C71 121.5(5) . . ? C75 C76 C7 118.8(5) . . ? C71 C76 C7 119.5(5) . . ? C62 C7 C76 109.9(4) . . ? C62 C7 H7A 109.7 . . ? C76 C7 H7A 109.7 . . ? C62 C7 H7B 109.7 . . ? C76 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C81 O81 U1 131.1(3) . . ? O81 C81 C82 121.3(5) . . ? O81 C81 C86 118.0(5) . . ? C82 C81 C86 120.6(5) . . ? C81 C82 C83 119.3(5) . . ? C81 C82 C1 122.9(5) . . ? C83 C82 C1 117.1(5) . . ? C84 C83 C82 122.4(5) . . ? C84 C83 H83 118.8 . . ? C82 C83 H83 118.8 . . ? C83 C84 C85 116.3(5) . . ? C83 C84 C841 121.7(6) . . ? C85 C84 C841 120.3(6) . . ? C83 C84 C845 117.6(7) . . ? C85 C84 C845 124.6(7) . . ? C842 C841 C843 111.0(8) . . ? C842 C841 C84 113.3(9) . . ? C843 C841 C84 110.1(8) . . ? C842 C841 C844 111.7(9) . . ? C843 C841 C844 104.3(9) . . ? C84 C841 C844 106.0(8) . . ? C848 C845 C846 113.9(14) . . ? C848 C845 C847 108.3(12) . . ? C846 C845 C847 107.0(12) . . ? C848 C845 C84 111.7(10) . . ? C846 C845 C84 103.1(12) . . ? C847 C845 C84 112.7(12) . . ? C845 C846 H84J 109.5 . . ? C845 C846 H84K 109.5 . . ? H84J C846 H84K 109.5 . . ? C845 C846 H84L 109.5 . . ? H84J C846 H84L 109.5 . . ? H84K C846 H84L 109.5 . . ? C845 C847 H84M 109.5 . . ? C845 C847 H84N 109.5 . . ? H84M C847 H84N 109.5 . . ? C845 C847 H84O 109.5 . . ? H84M C847 H84O 109.5 . . ? H84N C847 H84O 109.5 . . ? C845 C848 H84P 109.5 . . ? C845 C848 H84Q 109.5 . . ? H84P C848 H84Q 109.5 . . ? C845 C848 H84R 109.5 . . ? H84P C848 H84R 109.5 . . ? H84Q C848 H84R 109.5 . . ? C84 C85 C86 123.7(6) . . ? C84 C85 H85 118.2 . . ? C86 C85 H85 118.2 . . ? C81 C86 C85 117.6(5) . . ? C81 C86 C8 121.4(5) . . ? C85 C86 C8 120.9(5) . . ? C86 C8 C72 114.1(5) . . ? C86 C8 H8A 108.7 . . ? C72 C8 H8A 108.7 . . ? C86 C8 H8B 108.7 . . ? C72 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C104 N101 C101 113.9(13) . . ? C104 N101 C105 105.3(14) . . ? C101 N101 C105 109.1(15) . . ? C104 N101 H101 109.5 . . ? C101 N101 H101 109.5 . . ? C105 N101 H101 109.5 . . ? C102 C101 N101 122.0(13) . . ? C102 C101 H10G 106.8 . . ? N101 C101 H10G 106.8 . . ? C102 C101 H10H 106.8 . . ? N101 C101 H10H 106.8 . . ? H10G C101 H10H 106.7 . . ? C101 C102 C103 121.0(7) . . ? C101 C102 H10I 107.1 . . ? C103 C102 H10I 107.1 . . ? C101 C102 H10J 107.1 . . ? C103 C102 H10J 107.1 . . ? H10I C102 H10J 106.8 . . ? N102 C103 C102 121.0(10) . . ? N102 C103 H10K 107.1 . . ? C102 C103 H10K 107.1 . . ? N102 C103 H10L 107.1 . . ? C102 C103 H10L 107.1 . . ? H10K C103 H10L 106.8 . . ? C103 N102 C106 121.8(10) . . ? C103 N102 C107 114.2(10) . . ? C106 N102 C107 114.6(9) . . ? C103 N102 H102 100.3 . . ? C106 N102 H102 100.3 . . ? C107 N102 H102 100.3 . . ? C201 N201 C205 110.5(5) . . ? C201 N201 C204 113.7(5) . . ? C205 N201 C204 110.2(5) . . ? C201 N201 H201 107.4 . . ? C205 N201 H201 107.4 . . ? C204 N201 H201 107.4 . . ? N201 C204 H20A 109.5 . . ? N201 C204 H20B 109.5 . . ? H20A C204 H20B 109.5 . . ? N201 C204 H20C 109.5 . . ? H20A C204 H20C 109.5 . . ? H20B C204 H20C 109.5 . . ? N201 C205 H20D 109.5 . . ? N201 C205 H20E 109.5 . . ? H20D C205 H20E 109.5 . . ? N201 C205 H20F 109.5 . . ? H20D C205 H20F 109.5 . . ? H20E C205 H20F 109.5 . . ? N201 C201 C202 112.1(6) . . ? N201 C201 H20G 109.2 . . ? C202 C201 H20G 109.2 . . ? N201 C201 H20H 109.2 . . ? C202 C201 H20H 109.2 . . ? H20G C201 H20H 107.9 . . ? C203 C202 C201 116.1(7) . . ? C203 C202 H20I 108.3 . . ? C201 C202 H20I 108.3 . . ? C203 C202 H20J 108.2 . . ? C201 C202 H20J 108.3 . . ? H20I C202 H20J 107.4 . . ? C202 C203 N202 110.9(9) . . ? C202 C203 H20K 109.5 . . ? N202 C203 H20K 109.5 . . ? C202 C203 H20L 109.5 . . ? N202 C203 H20L 109.5 . . ? H20K C203 H20L 108.1 . . ? C207 N202 C206 109.5(14) . . ? C207 N202 C203 106.8(12) . . ? C206 N202 C203 109.0(13) . . ? N202 C206 H20M 109.5 . . ? N202 C206 H20N 109.4 . . ? H20M C206 H20N 109.5 . . ? N202 C206 H20O 109.5 . . ? H20M C206 H20O 109.5 . . ? H20N C206 H20O 109.5 . . ? N202 C207 H20P 109.5 . . ? N202 C207 H20Q 109.5 . . ? H20P C207 H20Q 109.5 . . ? N202 C207 H20R 109.5 . . ? H20P C207 H20R 109.5 . . ? H20Q C207 H20R 109.5 . . ? C304 N301 C305 110.4(4) . . ? C304 N301 C301 113.5(4) . . ? C305 N301 C301 109.8(4) . . ? C304 N301 H301 107.6 . . ? C305 N301 H301 107.6 . . ? C301 N301 H301 107.6 . . ? N301 C304 H30A 109.5 . . ? N301 C304 H30B 109.5 . . ? H30A C304 H30B 109.5 . . ? N301 C304 H30C 109.5 . . ? H30A C304 H30C 109.5 . . ? H30B C304 H30C 109.5 . . ? N301 C305 H30D 109.5 . . ? N301 C305 H30E 109.5 . . ? H30D C305 H30E 109.5 . . ? N301 C305 H30F 109.5 . . ? H30D C305 H30F 109.5 . . ? H30E C305 H30F 109.5 . . ? C302 C301 N301 115.3(4) . . ? C302 C301 H30G 108.4 . . ? N301 C301 H30G 108.4 . . ? C302 C301 H30H 108.4 . . ? N301 C301 H30H 108.4 . . ? H30G C301 H30H 107.5 . . ? C313 C302 C301 112.7(7) . . ? C303 C302 C301 113.9(6) . . ? C313 C302 H30I 137.9 . . ? C303 C302 H30I 108.8 . . ? C301 C302 H30I 108.8 . . ? C303 C302 H30J 108.8 . . ? C301 C302 H30J 108.8 . . ? H30I C302 H30J 107.7 . . ? C313 C302 H31I 109.1 . . ? C301 C302 H31I 109.1 . . ? C313 C302 H31J 109.1 . . ? C301 C302 H31J 109.1 . . ? H31I C302 H31J 107.8 . . ? N302 C303 C302 111.0(8) . . ? N302 C303 H30K 109.5 . . ? C302 C303 H30K 109.5 . . ? N302 C303 H30L 109.4 . . ? C302 C303 H30L 109.4 . . ? H30K C303 H30L 108 . . ? N302 C313 C302 111.5(10) . . ? N302 C313 H31A 109.3 . . ? C302 C313 H31A 109.3 . . ? N302 C313 H31B 109.3 . . ? C302 C313 H31B 109.3 . . ? H31A C313 H31B 108 . . ? C316 N302 C317 112.6(19) . . ? C306 N302 C307 124.7(9) . . ? C306 N302 C303 111.6(8) . . ? C307 N302 C303 97.1(9) . . ? C316 N302 C313 101.5(11) . . ? C317 N302 C313 102(2) . . ? N302 C306 H30M 109.5 . . ? N302 C306 H30N 109.5 . . ? N302 C306 H30O 109.5 . . ? N302 C307 H30P 109.5 . . ? N302 C307 H30Q 109.5 . . ? N302 C307 H30R 109.5 . . ? N302 C316 H31C 109.5 . . ? N302 C316 H31D 109.4 . . ? H31C C316 H31D 109.5 . . ? N302 C316 H31E 109.5 . . ? H31C C316 H31E 109.5 . . ? H31D C316 H31E 109.5 . . ? N302 C317 H31F 109.4 . . ? N302 C317 H31G 109.5 . . ? H31F C317 H31G 109.5 . . ? N302 C317 H31H 109.5 . . ? H31F C317 H31H 109.5 . . ? H31G C317 H31H 109.5 . . ? N011 C011 C012 170.6(14) . . ? C011 C012 H01A 109.5 . . ? C011 C012 H01B 109.5 . . ? H01A C012 H01B 109.5 . . ? C011 C012 H01C 109.5 . . ? H01A C012 H01C 109.5 . . ? H01B C012 H01C 109.5 . . ? N021 C021 C022 179.1(14) . . ? C021 C022 H02A 109.5 . . ? C021 C022 H02B 109.5 . . ? H02A C022 H02B 109.5 . . ? C021 C022 H02C 109.5 . . ? H02A C022 H02C 109.5 . . ? H02B C022 H02C 109.5 . . ? N031 C031 C032 173.4(14) . . ? C031 C032 H03A 109.5 . . ? C031 C032 H03B 109.5 . . ? H03A C032 H03B 109.5 . . ? C031 C032 H03C 109.5 . . ? H03A C032 H03C 109.5 . . ? H03B C032 H03C 109.5 . . ? N041 C041 C042 164.2(17) . . ? C041 C042 H04A 109.5 . . ? C041 C042 H04B 109.5 . . ? H04A C042 H04B 109.5 . . ? C041 C042 H04C 109.5 . . ? H04A C042 H04C 109.5 . . ? H04B C042 H04C 109.5 . . ? N051 C051 C052 167(2) . . ? N061 C061 C062 165.7(17) . . ? C061 C062 H06A 109.5 . . ? C061 C062 H06B 109.5 . . ? H06A C062 H06B 109.5 . . ? C061 C062 H06C 109.5 . . ? H06A C062 H06C 109.5 . . ? H06B C062 H06C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O0 H0 O1 0.95 2.13 2.947(9) 143.2 . O31 H31 O21 0.84 1.67 2.512(5) 175.5 . O71 H71 O61 0.84 1.72 2.561(5) 174.6 . N101 H101 O3 0.93 1.95 2.66(2) 131.1 . N101 H101 O3' 0.93 2.04 2.77(2) 134 . N201 H201 O51 0.93 1.79 2.714(7) 173.3 . N301 H301 O81 0.93 1.79 2.717(5) 176.9 . #===END # Attachment '- mo6c_1c.cif' data_mo6c _database_code_depnum_ccdc_archive 'CCDC 773077' #TrackingRef '- mo6c_1c.cif' _audit_creation_date 2008-07-30T12:42:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C114.50 H182 Cl8 N8 O13 U2' _chemical_formula_moiety ; 2(C12 H18 N2),2(C6 H17 N2),C88 H107 O13 U2,3(Cl),2.5(C H2 Cl2) ; _chemical_formula_weight 2638.34 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc 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 28.445(3) _cell_length_b 33.934(3) _cell_length_c 30.148(3) _cell_angle_alpha 90 _cell_angle_beta 93.050(2) _cell_angle_gamma 90 _cell_volume 29059(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 28.3 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_size_max .15 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .11 _exptl_crystal_size_rad ? _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10792 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.424 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .56 _exptl_absorpt_correction_T_max .766 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_av_unetI/netI 0.1241 _diffrn_reflns_number 142456 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 29.37 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.93 _reflns_number_total 37265 _reflns_number_gt 17848 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0948P)^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_number_reflns 37265 _refine_ls_number_parameters 1358 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.175 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.9 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.978 _refine_diff_density_min -6.697 _refine_diff_density_rms 0.149 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.572349(6) 0.724986(5) 0.588987(6) 0.03786(5) Uani 1 1 d . . . U2 U 0.639352(6) 0.836372(5) 0.640342(5) 0.03759(5) Uani 1 1 d . . . O0 O 0.61939(10) 0.78124(8) 0.59713(9) 0.0360(8) Uani 1 1 d . . . H0 H 0.6385 0.782 0.5723 0.043 Uiso 1 1 calc R . . O101 O 0.60116(11) 0.71731(9) 0.53808(10) 0.0432(9) Uani 1 1 d . . . O102 O 0.54223(11) 0.73169(9) 0.63952(10) 0.0427(9) Uani 1 1 d . . . O201 O 0.68140(10) 0.84622(9) 0.59999(9) 0.0401(8) Uani 1 1 d . . . O202 O 0.59788(11) 0.82784(9) 0.68185(10) 0.0424(9) Uani 1 1 d . . . O11 O 0.50258(10) 0.70636(8) 0.55477(10) 0.0396(8) Uani 1 1 d . . . C11 C 0.49156(15) 0.68806(14) 0.51592(15) 0.0390(12) Uani 1 1 d . . . C12 C 0.48519(15) 0.71081(13) 0.47693(15) 0.0388(12) Uani 1 1 d . A . C13 C 0.47133(16) 0.69198(15) 0.43733(16) 0.0486(14) Uani 1 1 d . . . H13 H 0.4668 0.7074 0.4111 0.058 Uiso 1 1 calc R . . C14 C 0.46384(17) 0.65122(14) 0.43467(16) 0.0478(14) Uani 1 1 d . . . C141 C 0.4468(2) 0.62996(17) 0.39175(19) 0.0720(18) Uani 1 1 d . . . C142 C 0.4048(3) 0.6088(3) 0.3990(3) 0.134(3) Uiso 1 1 d . . . H14A H 0.3979 0.6104 0.4304 0.201 Uiso 1 1 calc R . . H14B H 0.4088 0.5812 0.3906 0.201 Uiso 1 1 calc R . . H14C H 0.3786 0.6203 0.3808 0.201 Uiso 1 1 calc RD . . C143 C 0.4793(3) 0.5980(2) 0.3808(3) 0.118(3) Uiso 1 1 d . . . H14D H 0.4726 0.5897 0.35 0.176 Uiso 1 1 calc R . . H14E H 0.4751 0.5757 0.4007 0.176 Uiso 1 1 calc R . . H14F H 0.5118 0.6075 0.3843 0.176 Uiso 1 1 calc R . . C144 C 0.4378(3) 0.6582(3) 0.3547(3) 0.142(3) Uiso 1 1 d . . . H14G H 0.4676 0.6704 0.3471 0.213 Uiso 1 1 calc R . . H14H H 0.416 0.6786 0.3637 0.213 Uiso 1 1 calc R . . H14I H 0.424 0.6441 0.3287 0.213 Uiso 1 1 calc R . . C15 C 0.47088(15) 0.63035(14) 0.47378(16) 0.0444(13) Uani 1 1 d . . . H15 H 0.4657 0.6027 0.4729 0.053 Uiso 1 1 calc R . . C16 C 0.48493(15) 0.64695(14) 0.51392(15) 0.0406(12) Uani 1 1 d . . . C1 C 0.49573(16) 0.62140(13) 0.55451(16) 0.0434(13) Uani 1 1 d . . . H1A H 0.4734 0.599 0.5544 0.052 Uiso 1 1 calc R . . H1B H 0.4915 0.6371 0.5817 0.052 Uiso 1 1 calc R . . O21 O 0.53095(10) 0.78782(8) 0.56028(10) 0.0383(8) Uani 1 1 d . . . C21 C 0.48474(15) 0.79385(12) 0.54842(15) 0.0361(11) Uani 1 1 d . . . C22 C 0.45638(15) 0.81648(12) 0.57572(14) 0.0374(12) Uani 1 1 d . . . C23 C 0.40859(15) 0.82208(13) 0.56277(14) 0.0371(12) Uani 1 1 d . . . H23 H 0.3893 0.8371 0.5813 0.044 Uiso 1 1 calc R . . C24 C 0.38870(17) 0.80603(13) 0.52310(16) 0.0464(13) Uani 1 1 d . A . C241 C 0.33657(17) 0.81439(15) 0.50989(18) 0.0563(15) Uani 1 1 d . . . C242 C 0.3268(4) 0.8593(3) 0.5074(4) 0.073(3) Uiso 0.5 1 d P A 1 H24A H 0.2928 0.8638 0.5034 0.11 Uiso 0.5 1 calc PR A 1 H24B H 0.3425 0.8705 0.4821 0.11 Uiso 0.5 1 calc PR A 1 H24C H 0.3388 0.8719 0.5349 0.11 Uiso 0.5 1 calc PR A 1 C243 C 0.3058(3) 0.7981(3) 0.5474(3) 0.054(3) Uiso 0.5 1 d P A 1 H24D H 0.3152 0.811 0.5756 0.081 Uiso 0.5 1 calc PR A 1 H24E H 0.3105 0.7696 0.5503 0.081 Uiso 0.5 1 calc PR A 1 H24F H 0.2726 0.8037 0.5399 0.081 Uiso 0.5 1 calc PR A 1 C244 C 0.3229(5) 0.7992(5) 0.4649(5) 0.106(5) Uiso 0.5 1 d P A 1 H24G H 0.3262 0.7705 0.4646 0.159 Uiso 0.5 1 calc PR A 1 H24H H 0.3434 0.8108 0.4432 0.159 Uiso 0.5 1 calc PR A 1 H24I H 0.2901 0.8063 0.4571 0.159 Uiso 0.5 1 calc PR A 1 C245 C 0.3119(5) 0.8400(5) 0.5401(5) 0.104(5) Uiso 0.5 1 d P A 2 H24J H 0.2782 0.8403 0.5314 0.156 Uiso 0.5 1 calc PR A 2 H24K H 0.3245 0.8668 0.5386 0.156 Uiso 0.5 1 calc PR A 2 H24L H 0.3165 0.8301 0.5705 0.156 Uiso 0.5 1 calc PR A 2 C246 C 0.3115(5) 0.7733(4) 0.5011(5) 0.094(4) Uiso 0.5 1 d P A 2 H24M H 0.303 0.7618 0.5295 0.142 Uiso 0.5 1 calc PR A 2 H24N H 0.3329 0.7554 0.4866 0.142 Uiso 0.5 1 calc PR A 2 H24O H 0.2829 0.7771 0.482 0.142 Uiso 0.5 1 calc PR A 2 C247 C 0.3333(4) 0.8337(4) 0.4604(4) 0.076(4) Uiso 0.5 1 d P A 2 H24P H 0.3002 0.8354 0.4497 0.114 Uiso 0.5 1 calc PR A 2 H24Q H 0.3506 0.8172 0.4402 0.114 Uiso 0.5 1 calc PR A 2 H24R H 0.3471 0.8602 0.4615 0.114 Uiso 0.5 1 calc PR A 2 C25 C 0.41806(17) 0.78369(13) 0.49731(15) 0.0420(13) Uani 1 1 d . . . H25 H 0.4052 0.7723 0.4705 0.05 Uiso 1 1 calc R A . C26 C 0.46540(15) 0.77736(12) 0.50927(14) 0.0341(11) Uani 1 1 d . A . C2 C 0.49500(17) 0.75401(14) 0.47901(15) 0.0448(13) Uani 1 1 d . . . H2A H 0.4905 0.765 0.4486 0.054 Uiso 1 1 calc R A . H2B H 0.5285 0.7578 0.4887 0.054 Uiso 1 1 calc R . . O31 O 0.57214(11) 0.85019(9) 0.58785(10) 0.0432(9) Uani 1 1 d . . . H31 H 0.5572 0.8293 0.5822 0.065 Uiso 1 1 calc R . . C31 C 0.54125(15) 0.88165(12) 0.58679(13) 0.0330(11) Uani 1 1 d . . . C32 C 0.55664(16) 0.91845(13) 0.57052(14) 0.0379(12) Uani 1 1 d . . . C33 C 0.52525(16) 0.94964(13) 0.56910(14) 0.0406(12) Uani 1 1 d . . . H33 H 0.5356 0.9744 0.5585 0.049 Uiso 1 1 calc R . . C34 C 0.48010(16) 0.94671(13) 0.58216(14) 0.0400(12) Uani 1 1 d . . . C341 C 0.44452(18) 0.98111(14) 0.57834(17) 0.0499(14) Uani 1 1 d . . . C342 C 0.4254(3) 0.9902(2) 0.6209(2) 0.116(3) Uani 1 1 d . . . H34A H 0.4038 0.9692 0.629 0.175 Uiso 1 1 calc R . . H34B H 0.4083 1.0152 0.6188 0.175 Uiso 1 1 calc R . . H34C H 0.4511 0.9923 0.6437 0.175 Uiso 1 1 calc R . . C343 C 0.4063(3) 0.9709(2) 0.5422(3) 0.133(3) Uani 1 1 d . . . H34D H 0.3893 0.9473 0.5509 0.199 Uiso 1 1 calc R . . H34E H 0.421 0.966 0.514 0.199 Uiso 1 1 calc R . . H34F H 0.3842 0.993 0.5385 0.199 Uiso 1 1 calc R . . C344 C 0.4669(3) 1.01894(18) 0.5625(2) 0.098(3) Uani 1 1 d . . . H34G H 0.4464 1.0413 0.5686 0.147 Uiso 1 1 calc R . . H34H H 0.471 1.0172 0.5305 0.147 Uiso 1 1 calc R . . H34I H 0.4976 1.0226 0.5782 0.147 Uiso 1 1 calc R . . C35 C 0.46609(15) 0.91024(13) 0.59793(13) 0.0364(12) Uani 1 1 d . . . H35 H 0.4349 0.9073 0.6073 0.044 Uiso 1 1 calc R . . C36 C 0.49612(15) 0.87812(12) 0.60047(13) 0.0341(11) Uani 1 1 d . . . C3 C 0.47745(15) 0.83845(12) 0.61569(14) 0.0369(12) Uani 1 1 d . . . H3A H 0.5034 0.8228 0.6301 0.044 Uiso 1 1 calc R . . H3B H 0.4532 0.8426 0.6376 0.044 Uiso 1 1 calc R . . O41 O 0.62491(10) 0.90231(8) 0.64525(9) 0.0335(8) Uani 1 1 d . . . C41 C 0.64914(15) 0.93380(13) 0.62922(14) 0.0348(11) Uani 1 1 d . . . C42 C 0.68180(14) 0.95424(12) 0.65713(14) 0.0329(11) Uani 1 1 d . B . C43 C 0.70371(16) 0.98680(13) 0.64060(15) 0.0411(12) Uani 1 1 d . . . H43 H 0.7258 1.0007 0.6594 0.049 Uiso 1 1 calc R . . C44 C 0.69476(16) 1.00016(13) 0.59719(15) 0.0418(12) Uani 1 1 d . . . C441 C 0.72129(18) 1.03691(15) 0.58044(17) 0.0545(15) Uani 1 1 d . . . C442 C 0.7025(2) 1.07426(15) 0.6035(2) 0.082(2) Uani 1 1 d . . . H44A H 0.668 1.0732 0.6031 0.122 Uiso 1 1 calc R . . H44B H 0.7122 1.0978 0.5876 0.122 Uiso 1 1 calc R . . H44C H 0.7152 1.0753 0.6343 0.122 Uiso 1 1 calc R . . C443 C 0.77355(18) 1.03311(17) 0.5929(2) 0.081(2) Uani 1 1 d . . . H44D H 0.7781 1.0281 0.6249 0.121 Uiso 1 1 calc R . . H44E H 0.7896 1.0576 0.5855 0.121 Uiso 1 1 calc R . . H44F H 0.7867 1.0112 0.5765 0.121 Uiso 1 1 calc R . . C444 C 0.7130(3) 1.04229(19) 0.53110(18) 0.098(2) Uani 1 1 d . . . H44G H 0.7257 1.0196 0.5156 0.147 Uiso 1 1 calc R . . H44H H 0.7287 1.0664 0.5218 0.147 Uiso 1 1 calc R . . H44I H 0.6791 1.0444 0.5237 0.147 Uiso 1 1 calc R . . C45 C 0.66261(15) 0.97944(13) 0.57056(15) 0.0413(12) Uani 1 1 d . . . H45 H 0.656 0.9878 0.5408 0.05 Uiso 1 1 calc R . . C46 C 0.63970(15) 0.94667(12) 0.58622(14) 0.0360(11) Uani 1 1 d . . . C4 C 0.60672(15) 0.92334(14) 0.55443(14) 0.0417(13) Uani 1 1 d . . . H4A H 0.6204 0.8969 0.55 0.05 Uiso 1 1 calc R . . H4B H 0.6048 0.9368 0.5253 0.05 Uiso 1 1 calc R . . O51 O 0.69283(10) 0.85487(8) 0.69509(10) 0.0385(8) Uani 1 1 d . . . C51 C 0.73536(16) 0.87280(13) 0.69555(14) 0.0400(12) Uani 1 1 d . . . C52 C 0.77670(16) 0.85014(14) 0.68961(15) 0.0421(13) Uani 1 1 d . . . C53 C 0.82044(18) 0.86910(15) 0.69229(15) 0.0504(14) Uani 1 1 d . . . H53 H 0.8479 0.8538 0.6884 0.061 Uiso 1 1 calc R . . C54 C 0.82573(17) 0.90913(14) 0.70040(16) 0.0476(14) Uani 1 1 d . B . C541 C 0.87528(18) 0.92774(16) 0.70462(19) 0.0610(17) Uani 1 1 d . . . C542 C 0.8992(4) 0.9190(3) 0.6614(3) 0.059(3) Uiso 0.5 1 d P B 1 H54A H 0.9297 0.9326 0.6617 0.088 Uiso 0.5 1 calc PR B 1 H54B H 0.8792 0.9284 0.6361 0.088 Uiso 0.5 1 calc PR B 1 H54C H 0.9042 0.8906 0.6587 0.088 Uiso 0.5 1 calc PR B 1 C543 C 0.8727(3) 0.9715(3) 0.7099(3) 0.047(2) Uiso 0.5 1 d P B 1 H54D H 0.8522 0.9779 0.734 0.07 Uiso 0.5 1 calc PR B 1 H54E H 0.8598 0.9833 0.6821 0.07 Uiso 0.5 1 calc PR B 1 H54F H 0.9043 0.982 0.7169 0.07 Uiso 0.5 1 calc PR B 1 C544 C 0.9010(4) 0.9085(3) 0.7456(3) 0.052(3) Uiso 0.5 1 d P B 1 H54G H 0.904 0.8801 0.7407 0.078 Uiso 0.5 1 calc PR B 1 H54H H 0.883 0.9131 0.7719 0.078 Uiso 0.5 1 calc PR B 1 H54I H 0.9324 0.9202 0.7502 0.078 Uiso 0.5 1 calc PR B 1 C545 C 0.9148(5) 0.8990(4) 0.7120(5) 0.105(5) Uiso 0.5 1 d P B 2 H54J H 0.9448 0.9122 0.7072 0.158 Uiso 0.5 1 calc PR B 2 H54K H 0.9105 0.877 0.6912 0.158 Uiso 0.5 1 calc PR B 2 H54L H 0.9151 0.8891 0.7426 0.158 Uiso 0.5 1 calc PR B 2 C546 C 0.8755(7) 0.9622(6) 0.6711(6) 0.151(7) Uiso 0.5 1 d P B 2 H54M H 0.9046 0.9773 0.6759 0.227 Uiso 0.5 1 calc PR B 2 H54N H 0.8484 0.9793 0.6754 0.227 Uiso 0.5 1 calc PR B 2 H54O H 0.8735 0.9517 0.6408 0.227 Uiso 0.5 1 calc PR B 2 C547 C 0.8807(5) 0.9517(5) 0.7510(5) 0.111(5) Uiso 0.5 1 d P B 2 H54P H 0.8778 0.9333 0.7758 0.166 Uiso 0.5 1 calc PR B 2 H54Q H 0.8558 0.9716 0.7518 0.166 Uiso 0.5 1 calc PR B 2 H54R H 0.9115 0.9645 0.7535 0.166 Uiso 0.5 1 calc PR B 2 C55 C 0.78481(16) 0.93081(14) 0.70498(15) 0.0430(13) Uani 1 1 d . . . H55 H 0.7873 0.9583 0.7105 0.052 Uiso 1 1 calc R B . C56 C 0.74016(16) 0.91351(13) 0.70180(14) 0.0393(12) Uani 1 1 d . B . C5 C 0.69650(15) 0.93902(13) 0.70287(14) 0.0403(12) Uani 1 1 d . . . H5A H 0.6705 0.9234 0.7146 0.048 Uiso 1 1 calc R B . H5B H 0.7029 0.9616 0.7231 0.048 Uiso 1 1 calc R . . O61 O 0.68054(11) 0.77319(8) 0.66851(10) 0.0422(9) Uani 1 1 d D . . C61 C 0.70567(17) 0.76701(13) 0.70752(15) 0.0428(13) Uani 1 1 d . . . C62 C 0.68679(18) 0.74290(14) 0.74059(15) 0.0476(14) Uani 1 1 d . . . C63 C 0.7127(2) 0.73719(16) 0.78040(17) 0.0665(18) Uani 1 1 d . . . H63 H 0.6995 0.7216 0.8028 0.08 Uiso 1 1 calc R . . C64 C 0.7572(2) 0.75348(17) 0.78877(18) 0.0691(18) Uani 1 1 d . . . C641 C 0.7845(2) 0.7445(2) 0.8326(2) 0.090(2) Uani 1 1 d . . . C642 C 0.7560(3) 0.7551(3) 0.8707(2) 0.121(3) Uani 1 1 d . . . H64A H 0.7515 0.7838 0.8714 0.182 Uiso 1 1 calc R . . H64B H 0.7724 0.7465 0.8985 0.182 Uiso 1 1 calc R . . H64C H 0.7253 0.7421 0.8674 0.182 Uiso 1 1 calc R . . C643 C 0.8306(3) 0.7646(3) 0.8368(3) 0.138(3) Uani 1 1 d . . . H64D H 0.8474 0.7606 0.8096 0.206 Uiso 1 1 calc R . . H64E H 0.8492 0.7538 0.8622 0.206 Uiso 1 1 calc R . . H64F H 0.8257 0.7929 0.8414 0.206 Uiso 1 1 calc R . . C644 C 0.7929(3) 0.6989(2) 0.8347(2) 0.135(3) Uani 1 1 d . . . H64G H 0.7627 0.6852 0.8306 0.203 Uiso 1 1 calc R . . H64H H 0.8078 0.6919 0.8637 0.203 Uiso 1 1 calc R . . H64I H 0.8135 0.6912 0.8112 0.203 Uiso 1 1 calc R . . C65 C 0.7745(2) 0.77628(15) 0.75591(18) 0.0612(16) Uani 1 1 d . . . H65 H 0.8048 0.7877 0.7607 0.073 Uiso 1 1 calc R . . C66 C 0.74918(18) 0.78344(13) 0.71556(17) 0.0492(14) Uani 1 1 d . . . C6 C 0.77205(17) 0.80736(14) 0.67928(17) 0.0489(14) Uani 1 1 d . . . H6A H 0.8037 0.7964 0.6748 0.059 Uiso 1 1 calc R . . H6B H 0.753 0.8042 0.6511 0.059 Uiso 1 1 calc R . . O71 O 0.64302(10) 0.71146(8) 0.63604(9) 0.0326(7) Uani 1 1 d . . . H71 H 0.665 0.728 0.6363 0.049 Uiso 1 1 calc RD . . C71 C 0.65727(16) 0.67916(13) 0.66020(14) 0.0423(13) Uani 1 1 d . . . C72 C 0.67126(16) 0.64468(13) 0.63993(16) 0.0406(12) Uani 1 1 d . . . C73 C 0.68508(19) 0.61308(15) 0.66667(17) 0.0552(15) Uani 1 1 d . . . H73 H 0.6943 0.5895 0.6525 0.066 Uiso 1 1 calc R . . C74 C 0.6864(2) 0.61352(15) 0.71234(19) 0.0665(18) Uani 1 1 d . . . C741 C 0.7041(3) 0.57901(17) 0.7421(2) 0.087(2) Uani 1 1 d . . . C742 C 0.6656(3) 0.5666(2) 0.7720(2) 0.143(4) Uani 1 1 d . . . H74A H 0.6361 0.563 0.7541 0.214 Uiso 1 1 calc R . . H74B H 0.6614 0.587 0.7944 0.214 Uiso 1 1 calc R . . H74C H 0.6744 0.5417 0.7867 0.214 Uiso 1 1 calc R . . C743 C 0.7518(3) 0.5929(3) 0.7680(3) 0.134(3) Uiso 1 1 d . . . H74D H 0.7657 0.5707 0.7847 0.202 Uiso 1 1 calc R . . H74E H 0.7448 0.6143 0.7885 0.202 Uiso 1 1 calc R . . H74F H 0.7739 0.6023 0.7465 0.202 Uiso 1 1 calc R . . C744 C 0.7163(3) 0.54378(18) 0.7164(2) 0.118(3) Uani 1 1 d . . . H74G H 0.6874 0.532 0.703 0.176 Uiso 1 1 calc RD . . H74H H 0.7323 0.5246 0.7363 0.176 Uiso 1 1 calc R . . H74I H 0.7371 0.5513 0.693 0.176 Uiso 1 1 calc R . . C75 C 0.6708(2) 0.64852(14) 0.73233(18) 0.0606(17) Uani 1 1 d . . . H75 H 0.6705 0.6497 0.7638 0.073 Uiso 1 1 calc R . . C76 C 0.65570(17) 0.68145(13) 0.70760(16) 0.0457(13) Uani 1 1 d . . . C7 C 0.64214(18) 0.71862(13) 0.73100(16) 0.0472(14) Uani 1 1 d . . . H7A H 0.6274 0.7121 0.7591 0.057 Uiso 1 1 calc R . . H7B H 0.6192 0.7338 0.712 0.057 Uiso 1 1 calc R . . O81 O 0.57388(10) 0.65899(9) 0.60206(10) 0.0402(8) Uani 1 1 d . . . C81 C 0.58287(16) 0.62760(12) 0.57622(14) 0.0363(12) Uani 1 1 d . . . C82 C 0.54577(15) 0.60567(12) 0.55515(14) 0.0362(11) Uani 1 1 d . . . C83 C 0.55661(16) 0.57129(13) 0.53285(15) 0.0410(13) Uani 1 1 d . . . H83 H 0.5315 0.5567 0.5187 0.049 Uiso 1 1 calc R . . C84 C 0.60160(16) 0.55734(13) 0.53012(15) 0.0413(12) Uani 1 1 d . . . C841 C 0.61150(18) 0.51911(15) 0.50484(18) 0.0550(15) Uani 1 1 d . . . C842 C 0.5714(3) 0.49049(18) 0.5052(3) 0.112(3) Uani 1 1 d . . . H84A H 0.5815 0.465 0.4939 0.167 Uiso 1 1 calc R . . H84B H 0.5449 0.5005 0.4863 0.167 Uiso 1 1 calc R . . H84C H 0.5616 0.4873 0.5356 0.167 Uiso 1 1 calc R . . C843 C 0.6554(3) 0.4986(2) 0.5241(3) 0.149(3) Uani 1 1 d . . . H84D H 0.6489 0.4868 0.5528 0.223 Uiso 1 1 calc R . . H84E H 0.681 0.5178 0.5282 0.223 Uiso 1 1 calc R . . H84F H 0.6647 0.4779 0.5036 0.223 Uiso 1 1 calc R . . C844 C 0.6167(3) 0.53003(18) 0.4563(2) 0.096(2) Uani 1 1 d . . . H84G H 0.6428 0.5486 0.4541 0.145 Uiso 1 1 calc R . . H84H H 0.5875 0.5423 0.4443 0.145 Uiso 1 1 calc R . . H84I H 0.6231 0.5062 0.4392 0.145 Uiso 1 1 calc R . . C85 C 0.63770(17) 0.58030(13) 0.54859(15) 0.0432(13) Uani 1 1 d . . . H85 H 0.6693 0.5721 0.5457 0.052 Uiso 1 1 calc R . . C86 C 0.62914(15) 0.61565(13) 0.57167(14) 0.0361(11) Uani 1 1 d . . . C8 C 0.66933(16) 0.64072(13) 0.59065(16) 0.0421(13) Uani 1 1 d . . . H8A H 0.6994 0.6291 0.5818 0.05 Uiso 1 1 calc R . . H8B H 0.6666 0.6673 0.5773 0.05 Uiso 1 1 calc R . . N101 N 0.5532(3) 0.6460(3) 0.6901(3) 0.0580(16) Uani 0.5 1 d PD C 1 H10A H 0.5545 0.649 0.6602 0.087 Uiso 0.5 1 calc PR C 1 H10B H 0.5747 0.6621 0.7043 0.087 Uiso 0.5 1 calc PR C 1 H10C H 0.5239 0.6523 0.6985 0.087 Uiso 0.5 1 calc PR C 1 C102 C 0.5637(4) 0.6050(3) 0.7020(4) 0.063(4) Uani 0.5 1 d PD C 1 H10D H 0.5588 0.6011 0.734 0.075 Uiso 0.5 1 calc PR C 1 H10E H 0.5971 0.5994 0.6971 0.075 Uiso 0.5 1 calc PR C 1 C103 C 0.5336(4) 0.5769(3) 0.6757(4) 0.080(4) Uani 0.5 1 d PD C 1 H10F H 0.501 0.5791 0.6856 0.096 Uiso 0.5 1 calc PR C 1 H10G H 0.533 0.5851 0.6442 0.096 Uiso 0.5 1 calc PR C 1 N104 N 0.5471(3) 0.5366(3) 0.6783(3) 0.073(3) Uani 0.5 1 d PD C 1 C105 C 0.5877(4) 0.5338(3) 0.6485(4) 0.072(3) Uiso 0.5 1 d PD C 1 H10H H 0.6086 0.5567 0.6546 0.087 Uiso 0.5 1 calc PR C 1 H10I H 0.5752 0.536 0.6173 0.087 Uiso 0.5 1 calc PR C 1 C106 C 0.6169(5) 0.4970(4) 0.6528(4) 0.093(4) Uiso 0.5 1 d PD C 1 H10J H 0.6201 0.489 0.6841 0.139 Uiso 0.5 1 calc PR C 1 H10K H 0.6482 0.502 0.6419 0.139 Uiso 0.5 1 calc PRD C 1 H10L H 0.6015 0.4758 0.6353 0.139 Uiso 0.5 1 calc PR C 1 C107 C 0.5098(5) 0.5084(4) 0.6734(4) 0.103(5) Uiso 0.5 1 d PD C 1 H10M H 0.4845 0.5154 0.6933 0.124 Uiso 0.5 1 calc PR C 1 H10N H 0.5218 0.482 0.6819 0.124 Uiso 0.5 1 calc PR C 1 C108 C 0.4899(5) 0.5075(4) 0.6261(4) 0.098(5) Uiso 0.5 1 d PD C 1 H10O H 0.4817 0.5343 0.6164 0.147 Uiso 0.5 1 calc PR C 1 H10P H 0.4617 0.4909 0.6242 0.147 Uiso 0.5 1 calc PR C 1 H10Q H 0.5135 0.4966 0.6069 0.147 Uiso 0.5 1 calc PR C 1 N111 N 0.5429(3) 0.6477(3) 0.6909(4) 0.0580(16) Uani 0.5 1 d PD D 2 H11A H 0.5543 0.6525 0.6638 0.087 Uiso 0.5 1 calc PR D 2 H11B H 0.5602 0.6613 0.7121 0.087 Uiso 0.5 1 calc PR D 2 H11C H 0.5123 0.6555 0.6909 0.087 Uiso 0.5 1 calc PR D 2 C112 C 0.5459(5) 0.6056(3) 0.7004(4) 0.071(4) Uiso 0.5 1 d PD D 2 H11D H 0.5351 0.6002 0.7305 0.085 Uiso 0.5 1 calc PR D 2 H11E H 0.5789 0.5965 0.6992 0.085 Uiso 0.5 1 calc PR D 2 C113 C 0.5146(5) 0.5842(4) 0.6655(5) 0.088(5) Uiso 0.5 1 d PD D 2 H11F H 0.4879 0.6018 0.6569 0.106 Uiso 0.5 1 calc PR D 2 H11G H 0.533 0.5807 0.6388 0.106 Uiso 0.5 1 calc PR D 2 N114 N 0.4950(5) 0.5459(4) 0.6764(5) 0.165(6) Uiso 0.5 1 d PD D 2 C115 C 0.5326(7) 0.5195(7) 0.6800(7) 0.195(12) Uiso 0.5 1 d PD D 2 H11H H 0.5188 0.4931 0.6838 0.234 Uiso 0.5 1 calc PR D 2 H11I H 0.5503 0.5258 0.7083 0.234 Uiso 0.5 1 calc PR D 2 C116 C 0.5692(7) 0.5151(7) 0.6450(7) 0.184(10) Uiso 0.5 1 d PD D 2 H11J H 0.5541 0.5043 0.6177 0.275 Uiso 0.5 1 calc PR D 2 H11K H 0.5942 0.4972 0.6562 0.275 Uiso 0.5 1 calc PR D 2 H11L H 0.5828 0.5409 0.6388 0.275 Uiso 0.5 1 calc PR D 2 C117 C 0.4609(5) 0.5333(5) 0.6393(5) 0.123(6) Uiso 0.5 1 d PD D 2 H11M H 0.4555 0.5046 0.6418 0.148 Uiso 0.5 1 calc PR D 2 H11N H 0.4755 0.538 0.6107 0.148 Uiso 0.5 1 calc PR D 2 C118 C 0.4140(6) 0.5541(6) 0.6384(6) 0.158(8) Uiso 0.5 1 d PD D 2 H11O H 0.4057 0.5598 0.6689 0.237 Uiso 0.5 1 calc PR D 2 H11P H 0.3898 0.5372 0.624 0.237 Uiso 0.5 1 calc PR D 2 H11Q H 0.416 0.5788 0.6218 0.237 Uiso 0.5 1 calc PR D 2 N201 N 0.6449(4) 0.8405(3) 0.7720(3) 0.0577(14) Uani 0.5 1 d PD E 1 H20A H 0.6187 0.8559 0.7721 0.087 Uiso 0.5 1 calc PR E 1 H20B H 0.6363 0.8147 0.7701 0.087 Uiso 0.5 1 calc PR E 1 H20C H 0.6618 0.847 0.7482 0.087 Uiso 0.5 1 calc PR E 1 C202 C 0.6735(4) 0.8469(3) 0.8127(3) 0.046(3) Uiso 0.5 1 d PD E 1 H20D H 0.7012 0.8293 0.813 0.055 Uiso 0.5 1 calc PR E 1 H20E H 0.6549 0.84 0.8384 0.055 Uiso 0.5 1 calc PR E 1 C203 C 0.6897(4) 0.8889(3) 0.8172(3) 0.057(3) Uiso 0.5 1 d PD E 1 H20F H 0.708 0.8959 0.7913 0.068 Uiso 0.5 1 calc PR E 1 H20G H 0.6619 0.9065 0.8171 0.068 Uiso 0.5 1 calc PR E 1 N204 N 0.7196(3) 0.8955(3) 0.8590(3) 0.079(3) Uiso 0.5 1 d PD E 1 C205 C 0.7656(4) 0.8756(4) 0.8549(4) 0.091(4) Uiso 0.5 1 d PD E 1 H20H H 0.7586 0.847 0.853 0.109 Uiso 0.5 1 calc PR E 1 H20I H 0.7835 0.8797 0.8836 0.109 Uiso 0.5 1 calc PR E 1 C206 C 0.8001(4) 0.8844(3) 0.8184(3) 0.059(3) Uiso 0.5 1 d PD E 1 H20J H 0.7849 0.8784 0.7893 0.089 Uiso 0.5 1 calc PR E 1 H20K H 0.8284 0.8681 0.8233 0.089 Uiso 0.5 1 calc PR E 1 H20L H 0.8089 0.9123 0.8196 0.089 Uiso 0.5 1 calc PR E 1 C207 C 0.7237(6) 0.9382(4) 0.8633(5) 0.126(6) Uiso 0.5 1 d PD E 1 H20M H 0.6918 0.9498 0.8617 0.152 Uiso 0.5 1 calc PR E 1 H20N H 0.7405 0.9485 0.8378 0.152 Uiso 0.5 1 calc PR E 1 C208 C 0.7489(8) 0.9516(7) 0.9051(7) 0.209(11) Uiso 0.5 1 d PD E 1 H20O H 0.726 0.9581 0.927 0.314 Uiso 0.5 1 calc PR E 1 H20P H 0.7678 0.9749 0.899 0.314 Uiso 0.5 1 calc PR E 1 H20Q H 0.7696 0.9304 0.9167 0.314 Uiso 0.5 1 calc PR E 1 N211 N 0.6505(4) 0.8413(4) 0.7725(3) 0.0577(14) Uani 0.5 1 d PD F 2 H21A H 0.6264 0.8584 0.7763 0.087 Uiso 0.5 1 calc PR F 2 H21B H 0.639 0.8163 0.7706 0.087 Uiso 0.5 1 calc PR F 2 H21C H 0.6648 0.8474 0.7471 0.087 Uiso 0.5 1 calc PR F 2 C212 C 0.6847(5) 0.8441(4) 0.8103(5) 0.080(5) Uiso 0.5 1 d PD F 2 H21D H 0.7106 0.825 0.8071 0.096 Uiso 0.5 1 calc PR F 2 H21E H 0.6694 0.8385 0.8384 0.096 Uiso 0.5 1 calc PR F 2 C213 C 0.7033(4) 0.8863(3) 0.8100(4) 0.067(4) Uiso 0.5 1 d PD F 2 H21F H 0.7224 0.8897 0.7838 0.081 Uiso 0.5 1 calc PR F 2 H21G H 0.6762 0.9045 0.8065 0.081 Uiso 0.5 1 calc PR F 2 N214 N 0.7309(3) 0.8975(3) 0.8482(3) 0.076(3) Uiso 0.5 1 d PD F 2 C215 C 0.7813(5) 0.9052(4) 0.8382(6) 0.113(5) Uiso 0.5 1 d PD F 2 H21H H 0.8022 0.8999 0.8649 0.135 Uiso 0.5 1 calc PR F 2 H21I H 0.7907 0.8875 0.814 0.135 Uiso 0.5 1 calc PR F 2 C216 C 0.7858(9) 0.9446(6) 0.8252(8) 0.230(12) Uiso 0.5 1 d PD F 2 H21J H 0.792 0.9457 0.7935 0.345 Uiso 0.5 1 calc PR F 2 H21K H 0.812 0.9568 0.8426 0.345 Uiso 0.5 1 calc PR F 2 H21L H 0.7566 0.9587 0.8304 0.345 Uiso 0.5 1 calc PR F 2 C217 C 0.7054(5) 0.9205(5) 0.8794(5) 0.118(6) Uiso 0.5 1 d PD F 2 H21M H 0.6749 0.9077 0.8848 0.142 Uiso 0.5 1 calc PR F 2 H21N H 0.6989 0.9472 0.8673 0.142 Uiso 0.5 1 calc PR F 2 C218 C 0.7348(8) 0.9230(7) 0.9212(6) 0.192(10) Uiso 0.5 1 d PD F 2 H21O H 0.7459 0.8967 0.9298 0.289 Uiso 0.5 1 calc PR F 2 H21P H 0.7161 0.9339 0.9447 0.289 Uiso 0.5 1 calc PR F 2 H21Q H 0.7618 0.9402 0.9168 0.289 Uiso 0.5 1 calc PR F 2 N301 N 0.5464(3) 0.9137(2) 0.6911(3) 0.0431(19) Uani 0.5 1 d PD G 1 H30A H 0.575 0.9096 0.6796 0.065 Uiso 0.5 1 calc PR G 1 H30B H 0.5235 0.9025 0.6731 0.065 Uiso 0.5 1 calc PR G 1 H30C H 0.5462 0.9027 0.7186 0.065 Uiso 0.5 1 calc PR G 1 C302 C 0.5380(4) 0.9548(3) 0.6943(4) 0.060(3) Uiso 0.5 1 d PD G 1 H30D H 0.5094 0.9592 0.7109 0.072 Uiso 0.5 1 calc PR G 1 H30E H 0.5322 0.9658 0.664 0.072 Uiso 0.5 1 calc PR G 1 C303 C 0.5796(4) 0.9767(3) 0.7177(4) 0.069(4) Uiso 0.5 1 d PD G 1 H30F H 0.5857 0.9648 0.7474 0.083 Uiso 0.5 1 calc PR G 1 H30G H 0.6079 0.972 0.7007 0.083 Uiso 0.5 1 calc PR G 1 N304 N 0.5743(4) 1.0179(3) 0.7231(4) 0.115(5) Uiso 0.5 1 d PD G 1 C305 C 0.6212(5) 1.0404(5) 0.7377(4) 0.110(5) Uiso 0.5 1 d PD G 1 H30H H 0.6159 1.0693 0.7379 0.132 Uiso 0.5 1 calc PR G 1 H30I H 0.6463 1.0344 0.7173 0.132 Uiso 0.5 1 calc PR G 1 C306 C 0.6354(5) 1.0247(4) 0.7871(4) 0.080(4) Uiso 0.5 1 d PD G 1 H30J H 0.6097 1.0304 0.8066 0.12 Uiso 0.5 1 calc PR G 1 H30K H 0.6641 1.0381 0.7984 0.12 Uiso 0.5 1 calc PR G 1 H30L H 0.6409 0.9963 0.7862 0.12 Uiso 0.5 1 calc PR G 1 C307 C 0.5548(8) 1.0447(8) 0.6889(6) 0.269(15) Uiso 0.5 1 d PD G 1 H30M H 0.5545 1.072 0.7005 0.323 Uiso 0.5 1 calc PR G 1 H30N H 0.522 1.037 0.6801 0.323 Uiso 0.5 1 calc PR G 1 C308 C 0.5853(7) 1.0425(6) 0.6487(6) 0.156(8) Uiso 0.5 1 d PD G 1 H30O H 0.6187 1.0432 0.6589 0.235 Uiso 0.5 1 calc PR G 1 H30P H 0.5783 1.065 0.6291 0.235 Uiso 0.5 1 calc PR G 1 H30Q H 0.5787 1.0179 0.6325 0.235 Uiso 0.5 1 calc PR G 1 N311 N 0.5442(3) 0.9298(2) 0.6876(3) 0.0431(19) Uani 0.5 1 d PD H 2 H31A H 0.5633 0.9221 0.6659 0.065 Uiso 0.5 1 calc PR H 2 H31B H 0.5147 0.9202 0.6816 0.065 Uiso 0.5 1 calc PR H 2 H31C H 0.5558 0.9203 0.7142 0.065 Uiso 0.5 1 calc PR H 2 C312 C 0.5427(3) 0.9714(3) 0.6893(3) 0.049(3) Uiso 0.5 1 d PD H 2 H31D H 0.5142 0.9799 0.7043 0.059 Uiso 0.5 1 calc PR H 2 H31E H 0.5407 0.9822 0.6587 0.059 Uiso 0.5 1 calc PR H 2 C313 C 0.5847(4) 0.9868(3) 0.7135(4) 0.059(3) Uiso 0.5 1 d PD H 2 H31F H 0.5886 0.9741 0.743 0.071 Uiso 0.5 1 calc PR H 2 H31G H 0.613 0.981 0.6969 0.071 Uiso 0.5 1 calc PR H 2 N314 N 0.5793(4) 1.0287(3) 0.7185(3) 0.062(3) Uiso 0.5 1 d PD H 2 C315 C 0.5938(5) 1.0442(5) 0.7636(5) 0.133(6) Uiso 0.5 1 d PD H 2 H31H H 0.59 1.0731 0.7656 0.16 Uiso 0.5 1 calc PR H 2 H31I H 0.5766 1.0312 0.7873 0.16 Uiso 0.5 1 calc PR H 2 C316 C 0.6438(6) 1.0323(7) 0.7644(8) 0.191(11) Uiso 0.5 1 d PD H 2 H31J H 0.653 1.0275 0.734 0.287 Uiso 0.5 1 calc PR H 2 H31K H 0.6483 1.0082 0.782 0.287 Uiso 0.5 1 calc PR H 2 H31L H 0.6634 1.0534 0.7778 0.287 Uiso 0.5 1 calc PR H 2 C317 C 0.6001(6) 1.0455(4) 0.6804(5) 0.110(5) Uiso 0.5 1 d PD H 2 H31M H 0.5865 1.0326 0.6532 0.132 Uiso 0.5 1 calc PR H 2 H31N H 0.6344 1.0401 0.6823 0.132 Uiso 0.5 1 calc PR H 2 C318 C 0.5919(6) 1.0904(4) 0.6770(5) 0.117(6) Uiso 0.5 1 d PD H 2 H31O H 0.5592 1.0964 0.683 0.176 Uiso 0.5 1 calc PR H 2 H31P H 0.5983 1.0994 0.647 0.176 Uiso 0.5 1 calc PR H 2 H31Q H 0.613 1.104 0.6987 0.176 Uiso 0.5 1 calc PR H 2 N401 N 0.4367(3) 0.7161(2) 0.6224(3) 0.0417(12) Uiso 0.5 1 d PD I 1 H40A H 0.4383 0.6956 0.642 0.063 Uiso 0.5 1 calc PR I 1 H40B H 0.4476 0.7384 0.6363 0.063 Uiso 0.5 1 calc PR I 1 H40C H 0.4547 0.7106 0.5991 0.063 Uiso 0.5 1 calc PR I 1 C402 C 0.3866(3) 0.7222(3) 0.6058(4) 0.051(3) Uiso 0.5 1 d PD I 1 H40D H 0.3863 0.7353 0.5765 0.061 Uiso 0.5 1 calc PR I 1 H40E H 0.371 0.7399 0.6265 0.061 Uiso 0.5 1 calc PR I 1 C403 C 0.3588(6) 0.6844(5) 0.6013(6) 0.155(6) Uiso 0.5 1 d PD I 1 H40F H 0.36 0.6699 0.6299 0.186 Uiso 0.5 1 calc PR I 1 H40G H 0.3255 0.69 0.5924 0.186 Uiso 0.5 1 calc PR I 1 N404 N 0.3807(3) 0.6614(3) 0.5673(3) 0.065(3) Uiso 0.5 1 d PD I 1 C405 C 0.3709(5) 0.6736(5) 0.5191(4) 0.102(5) Uiso 0.5 1 d PD I 1 H40H H 0.3747 0.7024 0.5161 0.122 Uiso 0.5 1 calc PR I 1 H40I H 0.3936 0.6605 0.5001 0.122 Uiso 0.5 1 calc PR I 1 C406 C 0.3215(5) 0.6619(5) 0.5043(6) 0.130(6) Uiso 0.5 1 d PD I 1 H40J H 0.305 0.6522 0.5299 0.194 Uiso 0.5 1 calc PR I 1 H40K H 0.3225 0.641 0.4819 0.194 Uiso 0.5 1 calc PR I 1 H40L H 0.3048 0.6848 0.4915 0.194 Uiso 0.5 1 calc PR I 1 C407 C 0.3673(6) 0.6196(4) 0.5659(5) 0.108(5) Uiso 0.5 1 d PD I 1 H40M H 0.3808 0.6071 0.5398 0.13 Uiso 0.5 1 calc PR I 1 H40N H 0.3326 0.6175 0.5622 0.13 Uiso 0.5 1 calc PR I 1 C408 C 0.3843(5) 0.5971(4) 0.6081(4) 0.086(4) Uiso 0.5 1 d PD I 1 H40O H 0.4188 0.5968 0.6104 0.129 Uiso 0.5 1 calc PR I 1 H40P H 0.3726 0.5699 0.6065 0.129 Uiso 0.5 1 calc PR I 1 H40Q H 0.3724 0.6101 0.6342 0.129 Uiso 0.5 1 calc PR I 1 N411 N 0.4355(3) 0.7228(2) 0.6116(3) 0.0417(12) Uiso 0.5 1 d PD J 2 H41A H 0.441 0.7069 0.6356 0.063 Uiso 0.5 1 calc PR J 2 H41B H 0.4384 0.7484 0.6201 0.063 Uiso 0.5 1 calc PR J 2 H41C H 0.4568 0.7174 0.5909 0.063 Uiso 0.5 1 calc PR J 2 C412 C 0.3878(4) 0.7158(3) 0.5923(4) 0.068(4) Uiso 0.5 1 d PD J 2 H41D H 0.3821 0.7328 0.5659 0.081 Uiso 0.5 1 calc PR J 2 H41E H 0.3646 0.7229 0.6143 0.081 Uiso 0.5 1 calc PR J 2 C413 C 0.3813(7) 0.6728(6) 0.5791(8) 0.210(9) Uiso 0.5 1 d PD J 2 H41F H 0.4085 0.6646 0.562 0.251 Uiso 0.5 1 calc PR J 2 H41G H 0.3817 0.6566 0.6064 0.251 Uiso 0.5 1 calc PR J 2 N414 N 0.3388(5) 0.6647(4) 0.5530(4) 0.128(5) Uiso 0.5 1 d PD J 2 C415 C 0.3418(10) 0.6397(6) 0.5124(6) 0.210(9) Uiso 0.5 1 d PD J 2 H41H H 0.3152 0.6211 0.5083 0.251 Uiso 0.5 1 calc PR J 2 H41I H 0.3721 0.6256 0.5113 0.251 Uiso 0.5 1 calc PR J 2 C416 C 0.3378(7) 0.6748(5) 0.4807(6) 0.155(6) Uiso 0.5 1 d PD J 2 H41J H 0.3158 0.6684 0.4556 0.232 Uiso 0.5 1 calc PR J 2 H41K H 0.3688 0.6807 0.4696 0.232 Uiso 0.5 1 calc PR J 2 H41L H 0.3263 0.6978 0.4964 0.232 Uiso 0.5 1 calc PR J 2 C417 C 0.3142(8) 0.6468(5) 0.5844(6) 0.238(13) Uiso 0.5 1 d PD J 2 H41M H 0.3154 0.6185 0.5763 0.286 Uiso 0.5 1 calc PRD J 2 H41N H 0.2813 0.6551 0.5771 0.286 Uiso 0.5 1 calc PR J 2 C418 C 0.3175(6) 0.6462(6) 0.6326(5) 0.148(7) Uiso 0.5 1 d PD J 2 H41O H 0.3504 0.6426 0.6431 0.222 Uiso 0.5 1 calc PR J 2 H41P H 0.2984 0.6245 0.6433 0.222 Uiso 0.5 1 calc PR J 2 H41Q H 0.3058 0.6713 0.6439 0.222 Uiso 0.5 1 calc PRD J 2 Cl1 Cl 0.43622(6) 0.89985(7) 0.71178(5) 0.0952(6) Uani 1 1 d . . . Cl2 Cl 0.44177(6) 0.66378(7) 0.70107(6) 0.1124(8) Uani 1 1 d . . . Cl3 Cl 0.42318(12) 0.77927(8) 0.69635(10) 0.1702(12) Uani 1 1 d . . . Cl11 Cl 0.52773(11) 0.86629(9) 0.46124(10) 0.1699(12) Uani 1 1 d D . . Cl12 Cl 0.43677(11) 0.90465(12) 0.44309(10) 0.2081(16) Uani 1 1 d D . . C10 C 0.4737(2) 0.88284(17) 0.48195(18) 0.0684(18) Uani 1 1 d D . . H10R H 0.4574 0.86 0.4947 0.082 Uiso 1 1 calc R . . H10S H 0.4808 0.9019 0.5063 0.082 Uiso 1 1 calc R . . Cl21 Cl 0.6768(5) 0.9041(4) 0.3811(3) 0.374(8) Uani 0.5 1 d PD K 1 Cl22 Cl 0.7081(4) 0.9453(2) 0.4559(4) 0.330(6) Uani 0.5 1 d PD K 1 C20 C 0.6833(9) 0.9011(6) 0.4369(6) 0.222(12) Uiso 0.5 1 d PD K 1 H20R H 0.7042 0.8787 0.4457 0.266 Uiso 0.5 1 calc PR K 1 H20S H 0.6524 0.8969 0.4497 0.266 Uiso 0.5 1 calc PR K 1 Cl23 Cl 0.64205(17) 0.91002(17) 0.4279(2) 0.178(3) Uani 0.5 1 d PD L 2 Cl24 Cl 0.72268(19) 0.95544(17) 0.4033(2) 0.155(2) Uani 0.5 1 d PD L 2 C20' C 0.6975(4) 0.9117(4) 0.4102(6) 0.101(5) Uiso 0.5 1 d PD L 2 H20T H 0.718 0.8966 0.4316 0.122 Uiso 0.5 1 calc PR L 2 H20U H 0.6975 0.8976 0.3815 0.122 Uiso 0.5 1 calc PR L 2 Cl31 Cl 0.7894(2) 0.6970(2) 0.6497(3) 0.231(4) Uani 0.5 1 d PD . . Cl32 Cl 0.8361(3) 0.6579(2) 0.7164(3) 0.211(3) Uani 0.5 1 d PD . . C30 C 0.7841(3) 0.6822(3) 0.6982(3) 0.0329(19) Uiso 0.5 1 d PD . . H30R H 0.7571 0.664 0.6992 0.039 Uiso 0.5 1 calc PR . . H30S H 0.7784 0.7049 0.718 0.039 Uiso 0.5 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 0.04302(9) 0.03146(8) 0.03865(9) -0.00459(8) -0.00195(7) -0.00062(8) U2 0.04428(9) 0.03465(9) 0.03325(9) 0.00162(7) -0.00338(7) -0.00668(8) O0 0.0429(16) 0.0320(16) 0.0323(15) 0.0015(13) -0.0065(13) 0.0081(13) O101 0.0426(17) 0.0371(17) 0.0496(19) 0.0002(15) 0.0004(15) -0.0007(14) O102 0.0504(18) 0.0383(17) 0.0388(17) -0.0048(14) -0.0031(15) 0.0017(15) O201 0.0451(17) 0.0372(17) 0.0372(17) -0.0005(14) -0.0046(14) -0.0060(14) O202 0.0478(18) 0.0407(18) 0.0380(17) 0.0055(14) -0.0033(15) -0.0070(15) O11 0.0406(17) 0.0334(16) 0.0439(17) -0.0109(14) -0.0049(14) -0.0005(14) C11 0.028(2) 0.047(3) 0.041(3) -0.004(2) 0.001(2) 0.004(2) C12 0.036(2) 0.033(2) 0.048(3) -0.002(2) -0.002(2) 0.003(2) C13 0.046(3) 0.056(3) 0.043(3) -0.002(2) -0.005(2) 0.008(2) C14 0.043(3) 0.047(3) 0.052(3) -0.018(2) -0.004(2) 0.003(2) C141 0.069(3) 0.071(4) 0.071(4) -0.025(3) -0.040(3) 0.014(3) C15 0.036(2) 0.034(2) 0.061(3) -0.004(2) -0.014(2) -0.002(2) C16 0.031(2) 0.041(3) 0.049(3) -0.005(2) -0.002(2) -0.001(2) C1 0.042(3) 0.032(2) 0.057(3) -0.001(2) 0.002(2) -0.012(2) O21 0.0354(16) 0.0336(16) 0.0445(17) -0.0014(14) -0.0110(14) 0.0024(14) C21 0.037(2) 0.024(2) 0.046(3) 0.007(2) -0.006(2) 0.0058(19) C22 0.040(2) 0.029(2) 0.042(3) 0.004(2) -0.008(2) -0.007(2) C23 0.037(2) 0.032(2) 0.041(3) 0.001(2) -0.001(2) 0.001(2) C24 0.054(3) 0.035(2) 0.048(3) 0.003(2) -0.021(2) -0.002(2) C241 0.046(3) 0.051(3) 0.068(3) -0.010(3) -0.027(3) -0.003(3) C25 0.056(3) 0.036(2) 0.031(2) -0.004(2) -0.013(2) -0.006(2) C26 0.036(2) 0.029(2) 0.036(2) 0.0009(19) -0.0065(19) 0.0022(19) C2 0.047(3) 0.045(3) 0.043(3) 0.003(2) 0.002(2) -0.002(2) O31 0.0491(18) 0.0362(16) 0.0429(18) 0.0051(15) -0.0103(15) -0.0070(15) C31 0.038(2) 0.032(2) 0.028(2) 0.0015(18) -0.0103(19) 0.003(2) C32 0.046(3) 0.037(2) 0.028(2) 0.0045(19) -0.017(2) -0.001(2) C33 0.054(3) 0.031(2) 0.034(2) 0.005(2) -0.013(2) 0.001(2) C34 0.043(3) 0.038(2) 0.037(2) 0.002(2) -0.011(2) 0.003(2) C341 0.053(3) 0.041(3) 0.054(3) 0.003(2) -0.010(3) 0.009(2) C342 0.143(6) 0.104(5) 0.104(6) 0.026(4) 0.025(5) 0.072(5) C343 0.141(6) 0.106(5) 0.142(6) -0.035(5) -0.085(5) 0.074(5) C344 0.110(5) 0.060(4) 0.124(6) 0.009(4) -0.005(5) 0.020(4) C35 0.037(2) 0.039(2) 0.032(2) -0.003(2) -0.0077(19) -0.006(2) C36 0.041(2) 0.033(2) 0.028(2) -0.0001(18) -0.0098(19) 0.001(2) C3 0.039(2) 0.033(2) 0.038(2) -0.002(2) -0.006(2) -0.001(2) O41 0.0376(15) 0.0316(15) 0.0307(15) 0.0057(13) -0.0039(13) -0.0047(13) C41 0.033(2) 0.036(2) 0.036(2) -0.001(2) 0.0019(19) 0.004(2) C42 0.030(2) 0.030(2) 0.038(2) 0.0014(19) -0.0030(19) -0.0028(19) C43 0.044(3) 0.037(3) 0.041(3) 0.002(2) -0.008(2) 0.000(2) C44 0.045(3) 0.033(2) 0.047(3) 0.007(2) 0.001(2) -0.010(2) C441 0.055(3) 0.050(3) 0.057(3) 0.018(3) -0.005(3) -0.012(3) C442 0.097(5) 0.037(3) 0.112(5) 0.020(3) 0.013(4) -0.007(3) C443 0.048(3) 0.065(4) 0.130(5) 0.042(4) 0.005(3) -0.013(3) C444 0.148(6) 0.090(4) 0.055(4) 0.021(3) -0.002(4) -0.063(4) C45 0.043(3) 0.044(3) 0.036(2) 0.008(2) 0.001(2) -0.002(2) C46 0.043(2) 0.030(2) 0.036(2) 0.0036(19) 0.002(2) -0.002(2) C4 0.046(3) 0.048(3) 0.031(2) 0.010(2) -0.004(2) -0.007(2) O51 0.0423(17) 0.0313(16) 0.0415(17) 0.0009(14) -0.0030(14) -0.0016(14) C51 0.046(3) 0.040(3) 0.033(2) 0.006(2) -0.005(2) -0.005(2) C52 0.039(2) 0.045(3) 0.041(3) 0.001(2) -0.007(2) 0.007(2) C53 0.051(3) 0.056(3) 0.043(3) 0.000(2) -0.012(2) 0.001(3) C54 0.042(3) 0.045(3) 0.054(3) 0.006(2) -0.007(2) -0.009(2) C541 0.049(3) 0.062(3) 0.071(4) -0.001(3) -0.004(3) -0.011(3) C55 0.048(3) 0.039(3) 0.041(3) 0.001(2) -0.007(2) -0.009(2) C56 0.047(3) 0.040(3) 0.030(2) 0.000(2) -0.004(2) 0.000(2) C5 0.042(3) 0.039(2) 0.039(3) -0.007(2) -0.009(2) -0.004(2) O61 0.0535(19) 0.0286(16) 0.0424(17) 0.0023(14) -0.0161(15) 0.0012(15) C61 0.057(3) 0.030(2) 0.039(3) 0.000(2) -0.019(2) 0.001(2) C62 0.062(3) 0.038(3) 0.041(3) -0.002(2) -0.016(2) 0.004(2) C63 0.095(4) 0.060(3) 0.043(3) 0.004(3) -0.014(3) -0.012(3) C64 0.090(4) 0.055(3) 0.059(3) 0.010(3) -0.031(3) -0.003(3) C641 0.096(4) 0.096(5) 0.072(4) 0.010(4) -0.052(3) 0.001(4) C642 0.135(6) 0.165(8) 0.060(4) -0.009(5) -0.043(4) -0.003(6) C643 0.152(7) 0.150(8) 0.102(5) 0.016(5) -0.082(5) -0.020(6) C644 0.214(8) 0.087(5) 0.094(5) 0.013(4) -0.090(5) 0.018(6) C65 0.068(3) 0.045(3) 0.067(3) -0.002(3) -0.032(3) -0.004(3) C66 0.054(3) 0.027(2) 0.064(3) 0.002(2) -0.021(3) -0.002(2) C6 0.042(3) 0.042(3) 0.061(3) -0.003(2) -0.003(2) 0.002(2) O71 0.0413(16) 0.0172(13) 0.0378(16) 0.0057(12) -0.0105(13) -0.0031(12) C71 0.053(3) 0.036(2) 0.035(2) 0.004(2) -0.021(2) -0.005(2) C72 0.039(2) 0.031(2) 0.051(3) 0.000(2) -0.013(2) 0.003(2) C73 0.075(4) 0.036(3) 0.053(3) -0.003(2) -0.014(3) 0.003(3) C74 0.097(4) 0.037(3) 0.063(4) 0.006(3) -0.015(3) 0.000(3) C741 0.130(5) 0.041(3) 0.085(4) 0.012(3) -0.046(4) 0.000(4) C742 0.255(11) 0.077(5) 0.097(5) 0.055(4) 0.017(6) 0.027(6) C744 0.188(8) 0.050(4) 0.108(5) 0.017(4) -0.047(5) 0.030(5) C75 0.095(4) 0.034(3) 0.051(3) 0.010(2) -0.012(3) -0.015(3) C76 0.056(3) 0.031(2) 0.049(3) 0.003(2) -0.015(2) -0.004(2) C7 0.065(3) 0.040(3) 0.036(3) 0.002(2) -0.003(2) -0.006(2) O81 0.0371(16) 0.0390(17) 0.0440(17) -0.0072(14) -0.0036(14) 0.0028(14) C81 0.049(3) 0.021(2) 0.038(2) -0.0003(18) 0.000(2) 0.004(2) C82 0.035(2) 0.031(2) 0.041(2) 0.004(2) -0.006(2) 0.000(2) C83 0.047(3) 0.035(2) 0.040(3) 0.000(2) -0.005(2) 0.000(2) C84 0.048(3) 0.033(2) 0.043(3) -0.006(2) 0.005(2) 0.007(2) C841 0.053(3) 0.045(3) 0.067(3) -0.013(3) 0.005(3) 0.000(3) C842 0.129(6) 0.051(4) 0.160(7) -0.044(4) 0.063(5) -0.019(4) C843 0.157(6) 0.087(4) 0.191(7) -0.084(5) -0.093(6) 0.077(4) C844 0.142(6) 0.061(4) 0.090(5) -0.029(3) 0.045(4) 0.004(4) C85 0.049(3) 0.033(2) 0.048(3) -0.003(2) 0.009(2) 0.010(2) C86 0.039(2) 0.033(2) 0.036(2) 0.003(2) -0.003(2) 0.002(2) C8 0.038(2) 0.028(2) 0.059(3) -0.002(2) -0.002(2) 0.000(2) N101 0.043(3) 0.082(3) 0.049(3) 0.004(2) 0.007(2) 0.000(3) C102 0.033(5) 0.093(9) 0.060(7) 0.014(6) -0.004(5) -0.010(6) C103 0.053(7) 0.093(9) 0.093(9) 0.031(8) -0.014(7) 0.018(7) N104 0.111(8) 0.058(6) 0.051(6) 0.001(5) 0.008(6) -0.012(6) N111 0.043(3) 0.082(3) 0.049(3) 0.004(2) 0.007(2) 0.000(3) N201 0.072(3) 0.066(3) 0.034(2) 0.010(2) -0.004(2) -0.009(3) N211 0.072(3) 0.066(3) 0.034(2) 0.010(2) -0.004(2) -0.009(3) N301 0.044(2) 0.041(5) 0.045(3) -0.013(3) 0.002(2) 0.007(3) N311 0.044(2) 0.041(5) 0.045(3) -0.013(3) 0.002(2) 0.007(3) Cl1 0.0628(9) 0.1688(18) 0.0552(9) 0.0095(11) 0.0154(8) -0.0111(11) Cl2 0.0719(10) 0.203(2) 0.0628(10) 0.0022(13) 0.0108(9) -0.0075(13) Cl3 0.249(3) 0.1164(19) 0.153(2) -0.0072(16) 0.084(2) -0.005(2) Cl11 0.198(3) 0.153(2) 0.163(2) 0.004(2) 0.049(2) -0.016(2) Cl12 0.174(3) 0.295(4) 0.149(2) 0.074(3) -0.054(2) -0.049(3) C10 0.093(4) 0.062(4) 0.050(3) 0.004(3) 0.002(3) -0.005(3) Cl21 0.536(19) 0.418(15) 0.158(7) -0.096(8) -0.063(9) 0.076(14) Cl22 0.410(13) 0.181(6) 0.393(13) -0.083(8) -0.024(11) 0.127(8) Cl23 0.109(3) 0.156(4) 0.275(7) 0.061(5) 0.068(4) 0.049(3) Cl24 0.135(4) 0.159(5) 0.169(5) 0.029(4) -0.002(4) -0.007(4) Cl31 0.156(5) 0.182(6) 0.353(10) -0.047(7) 0.000(6) 0.047(5) Cl32 0.227(7) 0.187(6) 0.224(7) 0.045(5) 0.061(6) 0.027(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O101 1.797(3) . ? U1 O102 1.802(3) . ? U1 O81 2.274(3) . ? U1 O11 2.277(3) . ? U1 O0 2.336(3) . ? U1 O21 2.564(3) . ? U2 O201 1.782(3) . ? U2 O202 1.788(3) . ? U2 O51 2.273(3) . ? U2 O41 2.281(3) . ? U2 O0 2.333(3) . ? U2 O61 2.566(3) . ? O0 H0 0.95 . ? O11 C11 1.348(5) . ? C11 C16 1.409(6) . ? C11 C12 1.410(6) . ? C12 C13 1.393(6) . ? C12 C2 1.493(6) . ? C13 C14 1.401(7) . ? C13 H13 0.95 . ? C14 C15 1.381(7) . ? C14 C141 1.537(7) . ? C141 C142 1.422(10) . ? C141 C143 1.473(9) . ? C141 C144 1.483(10) . ? C142 H14A 0.98 . ? C142 H14B 0.98 . ? C142 H14C 0.98 . ? C143 H14D 0.98 . ? C143 H14E 0.98 . ? C143 H14F 0.98 . ? C144 H14G 0.98 . ? C144 H14H 0.98 . ? C144 H14I 0.98 . ? C15 C16 1.375(6) . ? C15 H15 0.95 . ? C16 C1 1.518(6) . ? C1 C82 1.519(6) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? O21 C21 1.359(5) . ? C21 C26 1.393(6) . ? C21 C22 1.410(6) . ? C22 C23 1.407(6) . ? C22 C3 1.513(6) . ? C23 C24 1.405(6) . ? C23 H23 0.95 . ? C24 C25 1.395(7) . ? C24 C241 1.541(7) . ? C241 C245 1.465(15) . ? C241 C244 1.484(15) . ? C241 C242 1.549(13) . ? C241 C243 1.567(11) . ? C241 C246 1.583(14) . ? C241 C247 1.628(13) . ? C242 H24A 0.98 . ? C242 H24B 0.98 . ? C242 H24C 0.98 . ? C243 H24D 0.98 . ? C243 H24E 0.98 . ? C243 H24F 0.98 . ? C244 H24G 0.98 . ? C244 H24H 0.98 . ? C244 H24I 0.98 . ? C245 H24J 0.98 . ? C245 H24K 0.98 . ? C245 H24L 0.98 . ? C246 H24M 0.98 . ? C246 H24N 0.98 . ? C246 H24O 0.98 . ? C247 H24P 0.98 . ? C247 H24Q 0.98 . ? C247 H24R 0.98 . ? C25 C26 1.392(6) . ? C25 H25 0.95 . ? C26 C2 1.500(6) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O31 C31 1.382(5) . ? O31 H31 0.84 . ? C31 C36 1.374(6) . ? C31 C32 1.419(6) . ? C32 C33 1.384(6) . ? C32 C4 1.538(6) . ? C33 C34 1.367(6) . ? C33 H33 0.95 . ? C34 C35 1.392(6) . ? C34 C341 1.545(6) . ? C341 C342 1.454(8) . ? C341 C344 1.521(8) . ? C341 C343 1.538(8) . ? C342 H34A 0.98 . ? C342 H34B 0.98 . ? C342 H34C 0.98 . ? C343 H34D 0.98 . ? C343 H34E 0.98 . ? C343 H34F 0.98 . ? C344 H34G 0.98 . ? C344 H34H 0.98 . ? C344 H34I 0.98 . ? C35 C36 1.385(6) . ? C35 H35 0.95 . ? C36 C3 1.527(6) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O41 C41 1.373(5) . ? C41 C46 1.381(6) . ? C41 C42 1.403(6) . ? C42 C43 1.375(6) . ? C42 C5 1.511(6) . ? C43 C44 1.396(6) . ? C43 H43 0.95 . ? C44 C45 1.377(6) . ? C44 C441 1.556(7) . ? C441 C444 1.505(7) . ? C441 C443 1.520(7) . ? C441 C442 1.554(8) . ? C442 H44A 0.98 . ? C442 H44B 0.98 . ? C442 H44C 0.98 . ? C443 H44D 0.98 . ? C443 H44E 0.98 . ? C443 H44F 0.98 . ? C444 H44G 0.98 . ? C444 H44H 0.98 . ? C444 H44I 0.98 . ? C45 C46 1.385(6) . ? C45 H45 0.95 . ? C46 C4 1.526(6) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? O51 C51 1.353(5) . ? C51 C56 1.400(6) . ? C51 C52 1.424(6) . ? C52 C53 1.399(7) . ? C52 C6 1.489(7) . ? C53 C54 1.387(7) . ? C53 H53 0.95 . ? C54 C55 1.390(7) . ? C54 C541 1.543(7) . ? C541 C543 1.495(11) . ? C541 C545 1.496(15) . ? C541 C542 1.532(11) . ? C541 C546 1.545(19) . ? C541 C544 1.546(11) . ? C541 C547 1.618(16) . ? C542 H54A 0.98 . ? C542 H54B 0.98 . ? C542 H54C 0.98 . ? C543 H54D 0.98 . ? C543 H54E 0.98 . ? C543 H54F 0.98 . ? C544 H54G 0.98 . ? C544 H54H 0.98 . ? C544 H54I 0.98 . ? C545 H54J 0.98 . ? C545 H54K 0.98 . ? C545 H54L 0.98 . ? C546 H54M 0.98 . ? C546 H54N 0.98 . ? C546 H54O 0.98 . ? C547 H54P 0.98 . ? C547 H54Q 0.98 . ? C547 H54R 0.98 . ? C55 C56 1.398(6) . ? C55 H55 0.95 . ? C56 C5 1.515(6) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? O61 C61 1.360(5) . ? C61 C66 1.367(7) . ? C61 C62 1.417(7) . ? C62 C63 1.388(7) . ? C62 C7 1.529(7) . ? C63 C64 1.392(8) . ? C63 H63 0.95 . ? C64 C65 1.369(8) . ? C64 C641 1.529(8) . ? C641 C643 1.478(10) . ? C641 C642 1.485(10) . ? C641 C644 1.565(10) . ? C642 H64A 0.98 . ? C642 H64B 0.98 . ? C642 H64C 0.98 . ? C643 H64D 0.98 . ? C643 H64E 0.98 . ? C643 H64F 0.98 . ? C644 H64G 0.98 . ? C644 H64H 0.98 . ? C644 H64I 0.98 . ? C65 C66 1.401(7) . ? C65 H65 0.95 . ? C66 C6 1.534(7) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O71 C71 1.365(5) . ? O71 H71 0.84 . ? C71 C72 1.388(6) . ? C71 C76 1.434(6) . ? C72 C73 1.386(6) . ? C72 C8 1.490(6) . ? C73 C74 1.375(7) . ? C73 H73 0.95 . ? C74 C75 1.414(7) . ? C74 C741 1.544(8) . ? C741 C744 1.475(9) . ? C741 C742 1.515(11) . ? C741 C743 1.597(10) . ? C742 H74A 0.98 . ? C742 H74B 0.98 . ? C742 H74C 0.98 . ? C743 H74D 0.98 . ? C743 H74E 0.98 . ? C743 H74F 0.98 . ? C744 H74G 0.98 . ? C744 H74H 0.98 . ? C744 H74I 0.98 . ? C75 C76 1.398(7) . ? C75 H75 0.95 . ? C76 C7 1.506(6) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? O81 C81 1.352(5) . ? C81 C86 1.391(6) . ? C81 C82 1.414(6) . ? C82 C83 1.389(6) . ? C83 C84 1.371(6) . ? C83 H83 0.95 . ? C84 C85 1.382(6) . ? C84 C841 1.538(7) . ? C841 C842 1.499(8) . ? C841 C843 1.519(8) . ? C841 C844 1.525(8) . ? C842 H84A 0.98 . ? C842 H84B 0.98 . ? C842 H84C 0.98 . ? C843 H84D 0.98 . ? C843 H84E 0.98 . ? C843 H84F 0.98 . ? C844 H84G 0.98 . ? C844 H84H 0.98 . ? C844 H84I 0.98 . ? C85 C86 1.414(6) . ? C85 H85 0.95 . ? C86 C8 1.513(6) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? N101 C102 1.463(13) . ? N101 H10A 0.91 . ? N101 H10B 0.91 . ? N101 H10C 0.91 . ? C102 C103 1.484(14) . ? C102 H10D 0.99 . ? C102 H10E 0.99 . ? C103 N104 1.420(13) . ? C103 H10F 0.99 . ? C103 H10G 0.99 . ? N104 C107 1.432(15) . ? N104 C105 1.502(13) . ? C105 C106 1.503(15) . ? C105 H10H 0.99 . ? C105 H10I 0.99 . ? C106 H10J 0.98 . ? C106 H10K 0.98 . ? C106 H10L 0.98 . ? C107 C108 1.505(15) . ? C107 H10M 0.99 . ? C107 H10N 0.99 . ? C108 H10O 0.98 . ? C108 H10P 0.98 . ? C108 H10Q 0.98 . ? N111 C112 1.458(14) . ? N111 H11A 0.91 . ? N111 H11B 0.91 . ? N111 H11C 0.91 . ? C112 C113 1.528(16) . ? C112 H11D 0.99 . ? C112 H11E 0.99 . ? C113 N114 1.459(17) . ? C113 H11F 0.99 . ? C113 H11G 0.99 . ? N114 C115 1.40(2) . ? N114 C117 1.503(17) . ? C115 C116 1.53(2) . ? C115 H11H 0.99 . ? C115 H11I 0.99 . ? C116 H11J 0.98 . ? C116 H11K 0.98 . ? C116 H11L 0.98 . ? C117 C118 1.510(18) . ? C117 H11M 0.99 . ? C117 H11N 0.99 . ? C118 H11O 0.98 . ? C118 H11P 0.98 . ? C118 H11Q 0.98 . ? N201 C202 1.452(12) . ? N201 H20A 0.91 . ? N201 H20B 0.91 . ? N201 H20C 0.91 . ? C202 C203 1.502(13) . ? C202 H20D 0.99 . ? C202 H20E 0.99 . ? C203 N204 1.498(13) . ? C203 H20F 0.99 . ? C203 H20G 0.99 . ? N204 C207 1.458(16) . ? N204 C205 1.484(14) . ? C205 C206 1.543(14) . ? C205 H20H 0.99 . ? C205 H20I 0.99 . ? C206 H20J 0.98 . ? C206 H20K 0.98 . ? C206 H20L 0.98 . ? C207 C208 1.49(2) . ? C207 H20M 0.99 . ? C207 H20N 0.99 . ? C208 H20O 0.98 . ? C208 H20P 0.98 . ? C208 H20Q 0.98 . ? N211 C212 1.460(15) . ? N211 H21A 0.91 . ? N211 H21B 0.91 . ? N211 H21C 0.91 . ? C212 C213 1.528(15) . ? C212 H21D 0.99 . ? C212 H21E 0.99 . ? C213 N214 1.409(14) . ? C213 H21F 0.99 . ? C213 H21G 0.99 . ? N214 C217 1.448(16) . ? N214 C215 1.503(15) . ? C215 C216 1.400(19) . ? C215 H21H 0.99 . ? C215 H21I 0.99 . ? C216 H21J 0.98 . ? C216 H21K 0.98 . ? C216 H21L 0.98 . ? C217 C218 1.478(19) . ? C217 H21M 0.99 . ? C217 H21N 0.99 . ? C218 H21O 0.98 . ? C218 H21P 0.98 . ? C218 H21Q 0.98 . ? N301 C302 1.418(12) . ? N301 H30A 0.91 . ? N301 H30B 0.91 . ? N301 H30C 0.91 . ? C302 C303 1.537(14) . ? C302 H30D 0.99 . ? C302 H30E 0.99 . ? C303 N304 1.419(14) . ? C303 H30F 0.99 . ? C303 H30G 0.99 . ? N304 C307 1.46(2) . ? N304 C305 1.579(16) . ? C305 C306 1.611(16) . ? C305 H30H 0.99 . ? C305 H30I 0.99 . ? C306 H30J 0.98 . ? C306 H30K 0.98 . ? C306 H30L 0.98 . ? C307 C308 1.53(2) . ? C307 H30M 0.99 . ? C307 H30N 0.99 . ? C308 H30O 0.98 . ? C308 H30P 0.98 . ? C308 H30Q 0.98 . ? N311 C312 1.413(11) . ? N311 H31A 0.91 . ? N311 H31B 0.91 . ? N311 H31C 0.91 . ? C312 C313 1.464(14) . ? C312 H31D 0.99 . ? C312 H31E 0.99 . ? C313 N314 1.440(13) . ? C313 H31F 0.99 . ? C313 H31G 0.99 . ? N314 C317 1.435(15) . ? N314 C315 1.495(16) . ? C315 C316 1.478(19) . ? C315 H31H 0.99 . ? C315 H31I 0.99 . ? C316 H31J 0.98 . ? C316 H31K 0.98 . ? C316 H31L 0.98 . ? C317 C318 1.547(17) . ? C317 H31M 0.99 . ? C317 H31N 0.99 . ? C318 H31O 0.98 . ? C318 H31P 0.98 . ? C318 H31Q 0.98 . ? N401 C402 1.501(11) . ? N401 H40A 0.91 . ? N401 H40B 0.91 . ? N401 H40C 0.91 . ? C402 C403 1.507(17) . ? C402 H40D 0.99 . ? C402 H40E 0.99 . ? C403 N404 1.455(17) . ? C403 H40F 0.99 . ? C403 H40G 0.99 . ? N404 C407 1.469(14) . ? N404 C405 1.523(14) . ? C405 C406 1.504(17) . ? C405 H40H 0.99 . ? C405 H40I 0.99 . ? C406 H40J 0.98 . ? C406 H40K 0.98 . ? C406 H40L 0.98 . ? C407 C408 1.539(16) . ? C407 H40M 0.99 . ? C407 H40N 0.99 . ? C408 H40O 0.98 . ? C408 H40P 0.98 . ? C408 H40Q 0.98 . ? N411 C412 1.466(13) . ? N411 H41A 0.91 . ? N411 H41B 0.91 . ? N411 H41C 0.91 . ? C412 C413 1.520(19) . ? C412 H41D 0.99 . ? C412 H41E 0.99 . ? C413 N414 1.43(2) . ? C413 H41F 0.99 . ? C413 H41G 0.99 . ? N414 C417 1.352(18) . ? N414 C415 1.493(19) . ? C415 C416 1.53(2) . ? C415 H41H 0.99 . ? C415 H41I 0.99 . ? C416 H41J 0.98 . ? C416 H41K 0.98 . ? C416 H41L 0.98 . ? C417 C418 1.450(19) . ? C417 H41M 0.99 . ? C417 H41N 0.99 . ? C418 H41O 0.98 . ? C418 H41P 0.98 . ? C418 H41Q 0.98 . ? Cl11 C10 1.780(6) . ? Cl12 C10 1.701(6) . ? C10 H10R 0.99 . ? C10 H10S 0.99 . ? Cl21 C20 1.687(17) . ? Cl22 C20 1.743(19) . ? C20 H20R 0.99 . ? C20 H20S 0.99 . ? Cl23 C20' 1.693(13) . ? Cl24 C20' 1.665(14) . ? C20' H20T 0.99 . ? C20' H20U 0.99 . ? Cl31 C30 1.561(11) . ? Cl32 C30 1.756(10) . ? C30 H30R 0.99 . ? C30 H30S 0.99 . ? 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 O101 U1 O102 178.40(14) . . ? O101 U1 O81 89.99(12) . . ? O102 U1 O81 89.05(12) . . ? O101 U1 O11 89.94(12) . . ? O102 U1 O11 88.62(12) . . ? O81 U1 O11 79.24(10) . . ? O101 U1 O0 85.61(12) . . ? O102 U1 O0 95.94(12) . . ? O81 U1 O0 141.34(10) . . ? O11 U1 O0 139.01(10) . . ? O101 U1 O21 93.12(12) . . ? O102 U1 O21 87.13(12) . . ? O81 U1 O21 151.85(10) . . ? O11 U1 O21 72.80(10) . . ? O0 U1 O21 66.81(9) . . ? O201 U2 O202 178.14(14) . . ? O201 U2 O51 89.79(12) . . ? O202 U2 O51 88.71(12) . . ? O201 U2 O41 89.44(12) . . ? O202 U2 O41 89.18(12) . . ? O51 U2 O41 78.34(10) . . ? O201 U2 O0 85.49(12) . . ? O202 U2 O0 96.37(12) . . ? O51 U2 O0 139.53(10) . . ? O41 U2 O0 141.59(9) . . ? O201 U2 O61 94.08(12) . . ? O202 U2 O61 86.54(12) . . ? O51 U2 O61 73.40(10) . . ? O41 U2 O61 151.49(9) . . ? O0 U2 O61 66.92(9) . . ? U2 O0 U1 146.61(14) . . ? U2 O0 H0 106.7 . . ? U1 O0 H0 106.7 . . ? C11 O11 U1 132.7(3) . . ? O11 C11 C16 121.2(4) . . ? O11 C11 C12 119.1(4) . . ? C16 C11 C12 119.7(4) . . ? C13 C12 C11 118.8(4) . . ? C13 C12 C2 122.0(4) . . ? C11 C12 C2 119.2(4) . . ? C12 C13 C14 122.5(5) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 116.3(4) . . ? C15 C14 C141 120.2(5) . . ? C13 C14 C141 123.5(5) . . ? C142 C141 C143 101.9(6) . . ? C142 C141 C144 109.2(6) . . ? C143 C141 C144 113.0(6) . . ? C142 C141 C14 109.8(6) . . ? C143 C141 C14 111.2(5) . . ? C144 C141 C14 111.4(6) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C16 C15 C14 124.3(4) . . ? C16 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? C15 C16 C11 118.4(4) . . ? C15 C16 C1 120.8(4) . . ? C11 C16 C1 120.7(4) . . ? C16 C1 C82 111.1(4) . . ? C16 C1 H1A 109.4 . . ? C82 C1 H1A 109.4 . . ? C16 C1 H1B 109.4 . . ? C82 C1 H1B 109.4 . . ? H1A C1 H1B 108 . . ? C21 O21 U1 129.4(2) . . ? O21 C21 C26 119.7(4) . . ? O21 C21 C22 120.2(4) . . ? C26 C21 C22 120.1(4) . . ? C23 C22 C21 119.1(4) . . ? C23 C22 C3 119.4(4) . . ? C21 C22 C3 121.2(4) . . ? C24 C23 C22 121.5(4) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C23 117.3(4) . . ? C25 C24 C241 123.5(4) . . ? C23 C24 C241 119.1(4) . . ? C245 C241 C244 131.6(9) . . ? C245 C241 C24 115.8(7) . . ? C244 C241 C24 112.0(7) . . ? C245 C241 C242 50.0(7) . . ? C244 C241 C242 105.0(8) . . ? C24 C241 C242 111.2(6) . . ? C245 C241 C243 57.0(7) . . ? C244 C241 C243 114.2(8) . . ? C24 C241 C243 108.3(5) . . ? C242 C241 C243 106.0(7) . . ? C245 C241 C246 113.5(9) . . ? C244 C241 C246 56.5(8) . . ? C24 C241 C246 107.5(6) . . ? C242 C241 C246 141.2(8) . . ? C243 C241 C246 63.0(7) . . ? C245 C241 C247 108.9(8) . . ? C244 C241 C247 45.7(7) . . ? C24 C241 C247 108.6(6) . . ? C242 C241 C247 63.7(7) . . ? C243 C241 C247 142.8(7) . . ? C246 C241 C247 101.5(7) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? C241 C244 H24G 109.5 . . ? C241 C244 H24H 109.5 . . ? C241 C244 H24I 109.5 . . ? C241 C245 H24J 109.5 . . ? C241 C245 H24K 109.5 . . ? H24J C245 H24K 109.5 . . ? C241 C245 H24L 109.5 . . ? H24J C245 H24L 109.5 . . ? H24K C245 H24L 109.5 . . ? C241 C246 H24M 109.5 . . ? C241 C246 H24N 109.5 . . ? H24M C246 H24N 109.5 . . ? C241 C246 H24O 109.5 . . ? H24M C246 H24O 109.5 . . ? H24N C246 H24O 109.5 . . ? C241 C247 H24P 109.5 . . ? C241 C247 H24Q 109.5 . . ? H24P C247 H24Q 109.5 . . ? C241 C247 H24R 109.5 . . ? H24P C247 H24R 109.5 . . ? H24Q C247 H24R 109.5 . . ? C26 C25 C24 122.6(4) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C25 C26 C21 119.4(4) . . ? C25 C26 C2 119.4(4) . . ? C21 C26 C2 121.2(4) . . ? C12 C2 C26 115.7(4) . . ? C12 C2 H2A 108.3 . . ? C26 C2 H2A 108.3 . . ? C12 C2 H2B 108.3 . . ? C26 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C31 O31 H31 109.5 . . ? C36 C31 O31 121.9(4) . . ? C36 C31 C32 119.4(4) . . ? O31 C31 C32 118.7(4) . . ? C33 C32 C31 118.2(4) . . ? C33 C32 C4 121.0(4) . . ? C31 C32 C4 120.8(4) . . ? C34 C33 C32 123.4(4) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C33 C34 C35 117.0(4) . . ? C33 C34 C341 123.1(4) . . ? C35 C34 C341 119.9(4) . . ? C342 C341 C344 106.3(5) . . ? C342 C341 C343 112.9(5) . . ? C344 C341 C343 105.0(5) . . ? C342 C341 C34 111.6(4) . . ? C344 C341 C34 112.2(4) . . ? C343 C341 C34 108.6(4) . . ? C341 C342 H34A 109.5 . . ? C341 C342 H34B 109.5 . . ? H34A C342 H34B 109.5 . . ? C341 C342 H34C 109.5 . . ? H34A C342 H34C 109.5 . . ? H34B C342 H34C 109.5 . . ? C341 C343 H34D 109.5 . . ? C341 C343 H34E 109.5 . . ? H34D C343 H34E 109.5 . . ? C341 C343 H34F 109.5 . . ? H34D C343 H34F 109.5 . . ? H34E C343 H34F 109.5 . . ? C341 C344 H34G 109.5 . . ? C341 C344 H34H 109.5 . . ? H34G C344 H34H 109.5 . . ? C341 C344 H34I 109.5 . . ? H34G C344 H34I 109.5 . . ? H34H C344 H34I 109.5 . . ? C36 C35 C34 122.1(4) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C31 C36 C35 119.9(4) . . ? C31 C36 C3 120.8(4) . . ? C35 C36 C3 119.2(4) . . ? C22 C3 C36 108.9(3) . . ? C22 C3 H3A 109.9 . . ? C36 C3 H3A 109.9 . . ? C22 C3 H3B 109.9 . . ? C36 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C41 O41 U2 130.2(2) . . ? O41 C41 C46 120.0(4) . . ? O41 C41 C42 120.2(4) . . ? C46 C41 C42 119.7(4) . . ? C43 C42 C41 118.6(4) . . ? C43 C42 C5 119.8(4) . . ? C41 C42 C5 121.4(4) . . ? C42 C43 C44 122.5(4) . . ? C42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C45 C44 C43 117.6(4) . . ? C45 C44 C441 122.6(4) . . ? C43 C44 C441 119.8(4) . . ? C444 C441 C443 110.8(5) . . ? C444 C441 C442 107.6(5) . . ? C443 C441 C442 108.3(5) . . ? C444 C441 C44 111.4(4) . . ? C443 C441 C44 109.7(4) . . ? C442 C441 C44 108.9(4) . . ? C441 C442 H44A 109.5 . . ? C441 C442 H44B 109.5 . . ? H44A C442 H44B 109.5 . . ? C441 C442 H44C 109.5 . . ? H44A C442 H44C 109.5 . . ? H44B C442 H44C 109.5 . . ? C441 C443 H44D 109.5 . . ? C441 C443 H44E 109.5 . . ? H44D C443 H44E 109.5 . . ? C441 C443 H44F 109.5 . . ? H44D C443 H44F 109.5 . . ? H44E C443 H44F 109.5 . . ? C441 C444 H44G 109.5 . . ? C441 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C441 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C44 C45 C46 121.4(4) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C41 C46 C45 120.2(4) . . ? C41 C46 C4 120.5(4) . . ? C45 C46 C4 119.2(4) . . ? C46 C4 C32 114.0(4) . . ? C46 C4 H4A 108.8 . . ? C32 C4 H4A 108.8 . . ? C46 C4 H4B 108.8 . . ? C32 C4 H4B 108.8 . . ? H4A C4 H4B 107.6 . . ? C51 O51 U2 134.0(3) . . ? O51 C51 C56 121.7(4) . . ? O51 C51 C52 120.0(4) . . ? C56 C51 C52 118.3(4) . . ? C53 C52 C51 118.8(4) . . ? C53 C52 C6 121.9(4) . . ? C51 C52 C6 119.2(4) . . ? C54 C53 C52 123.2(5) . . ? C54 C53 H53 118.4 . . ? C52 C53 H53 118.4 . . ? C53 C54 C55 116.9(4) . . ? C53 C54 C541 120.4(5) . . ? C55 C54 C541 122.8(4) . . ? C543 C541 C542 108.0(7) . . ? C543 C541 C54 111.4(5) . . ? C545 C541 C54 115.0(7) . . ? C542 C541 C54 107.3(6) . . ? C545 C541 C546 124.2(10) . . ? C54 C541 C546 106.9(8) . . ? C543 C541 C544 111.0(6) . . ? C542 C541 C544 112.7(6) . . ? C54 C541 C544 106.6(5) . . ? C545 C541 C547 99.3(9) . . ? C54 C541 C547 108.7(7) . . ? C546 C541 C547 100.6(10) . . ? C541 C542 H54A 109.5 . . ? C541 C542 H54B 109.5 . . ? C541 C542 H54C 109.5 . . ? C541 C543 H54D 109.5 . . ? C541 C543 H54E 109.5 . . ? C541 C543 H54F 109.5 . . ? C541 C544 H54G 109.5 . . ? C541 C544 H54H 109.5 . . ? C541 C544 H54I 109.5 . . ? C541 C545 H54J 109.5 . . ? C541 C545 H54K 109.5 . . ? H54J C545 H54K 109.5 . . ? C541 C545 H54L 109.5 . . ? H54J C545 H54L 109.5 . . ? H54K C545 H54L 109.5 . . ? C541 C546 H54M 109.5 . . ? C541 C546 H54N 109.5 . . ? H54M C546 H54N 109.5 . . ? C541 C546 H54O 109.5 . . ? H54M C546 H54O 109.5 . . ? H54N C546 H54O 109.5 . . ? C541 C547 H54P 109.5 . . ? C541 C547 H54Q 109.5 . . ? H54P C547 H54Q 109.5 . . ? C541 C547 H54R 109.5 . . ? H54P C547 H54R 109.5 . . ? H54Q C547 H54R 109.5 . . ? C54 C55 C56 122.3(4) . . ? C54 C55 H55 118.9 . . ? C56 C55 H55 118.9 . . ? C55 C56 C51 120.3(4) . . ? C55 C56 C5 120.1(4) . . ? C51 C56 C5 119.5(4) . . ? C42 C5 C56 111.3(4) . . ? C42 C5 H5A 109.4 . . ? C56 C5 H5A 109.4 . . ? C42 C5 H5B 109.4 . . ? C56 C5 H5B 109.4 . . ? H5A C5 H5B 108 . . ? C61 O61 U2 128.7(2) . . ? O61 C61 C66 121.3(4) . . ? O61 C61 C62 119.7(4) . . ? C66 C61 C62 119.0(4) . . ? C63 C62 C61 119.1(5) . . ? C63 C62 C7 119.0(5) . . ? C61 C62 C7 121.4(4) . . ? C62 C63 C64 122.5(5) . . ? C62 C63 H63 118.8 . . ? C64 C63 H63 118.8 . . ? C65 C64 C63 116.9(5) . . ? C65 C64 C641 123.5(6) . . ? C63 C64 C641 119.6(5) . . ? C643 C641 C642 109.9(6) . . ? C643 C641 C64 113.0(6) . . ? C642 C641 C64 110.3(6) . . ? C643 C641 C644 108.7(6) . . ? C642 C641 C644 107.3(6) . . ? C64 C641 C644 107.5(5) . . ? C641 C642 H64A 109.5 . . ? C641 C642 H64B 109.5 . . ? H64A C642 H64B 109.5 . . ? C641 C642 H64C 109.5 . . ? H64A C642 H64C 109.5 . . ? H64B C642 H64C 109.5 . . ? C641 C643 H64D 109.5 . . ? C641 C643 H64E 109.5 . . ? H64D C643 H64E 109.5 . . ? C641 C643 H64F 109.5 . . ? H64D C643 H64F 109.5 . . ? H64E C643 H64F 109.5 . . ? C641 C644 H64G 109.5 . . ? C641 C644 H64H 109.5 . . ? H64G C644 H64H 109.5 . . ? C641 C644 H64I 109.5 . . ? H64G C644 H64I 109.5 . . ? H64H C644 H64I 109.5 . . ? C64 C65 C66 122.6(5) . . ? C64 C65 H65 118.7 . . ? C66 C65 H65 118.7 . . ? C61 C66 C65 120.1(5) . . ? C61 C66 C6 120.2(4) . . ? C65 C66 C6 119.6(5) . . ? C52 C6 C66 113.8(4) . . ? C52 C6 H6A 108.8 . . ? C66 C6 H6A 108.8 . . ? C52 C6 H6B 108.8 . . ? C66 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C71 O71 H71 109.5 . . ? O71 C71 C72 121.7(4) . . ? O71 C71 C76 117.6(4) . . ? C72 C71 C76 120.6(4) . . ? C73 C72 C71 118.4(4) . . ? C73 C72 C8 120.3(4) . . ? C71 C72 C8 121.3(4) . . ? C74 C73 C72 124.5(5) . . ? C74 C73 H73 117.8 . . ? C72 C73 H73 117.8 . . ? C73 C74 C75 116.3(5) . . ? C73 C74 C741 124.3(5) . . ? C75 C74 C741 119.3(5) . . ? C744 C741 C742 106.4(6) . . ? C744 C741 C74 112.9(5) . . ? C742 C741 C74 109.4(6) . . ? C744 C741 C743 106.2(6) . . ? C742 C741 C743 114.4(6) . . ? C74 C741 C743 107.6(5) . . ? C741 C742 H74A 109.5 . . ? C741 C742 H74B 109.5 . . ? H74A C742 H74B 109.5 . . ? C741 C742 H74C 109.5 . . ? H74A C742 H74C 109.5 . . ? H74B C742 H74C 109.5 . . ? C741 C743 H74D 109.5 . . ? C741 C743 H74E 109.5 . . ? H74D C743 H74E 109.5 . . ? C741 C743 H74F 109.5 . . ? H74D C743 H74F 109.5 . . ? H74E C743 H74F 109.5 . . ? C741 C744 H74G 109.5 . . ? C741 C744 H74H 109.5 . . ? H74G C744 H74H 109.5 . . ? C741 C744 H74I 109.5 . . ? H74G C744 H74I 109.5 . . ? H74H C744 H74I 109.5 . . ? C76 C75 C74 122.6(5) . . ? C76 C75 H75 118.7 . . ? C74 C75 H75 118.7 . . ? C75 C76 C71 117.6(4) . . ? C75 C76 C7 119.9(4) . . ? C71 C76 C7 122.3(4) . . ? C76 C7 C62 108.0(4) . . ? C76 C7 H7A 110.1 . . ? C62 C7 H7A 110.1 . . ? C76 C7 H7B 110.1 . . ? C62 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C81 O81 U1 132.7(3) . . ? O81 C81 C86 119.7(4) . . ? O81 C81 C82 120.9(4) . . ? C86 C81 C82 119.3(4) . . ? C83 C82 C81 118.7(4) . . ? C83 C82 C1 121.4(4) . . ? C81 C82 C1 119.8(4) . . ? C84 C83 C82 123.4(4) . . ? C84 C83 H83 118.3 . . ? C82 C83 H83 118.3 . . ? C83 C84 C85 117.2(4) . . ? C83 C84 C841 121.1(4) . . ? C85 C84 C841 121.5(4) . . ? C842 C841 C843 108.1(5) . . ? C842 C841 C844 106.1(5) . . ? C843 C841 C844 111.0(5) . . ? C842 C841 C84 112.5(4) . . ? C843 C841 C84 111.5(5) . . ? C844 C841 C84 107.5(4) . . ? C841 C842 H84A 109.5 . . ? C841 C842 H84B 109.5 . . ? H84A C842 H84B 109.5 . . ? C841 C842 H84C 109.5 . . ? H84A C842 H84C 109.5 . . ? H84B C842 H84C 109.5 . . ? C841 C843 H84D 109.5 . . ? C841 C843 H84E 109.5 . . ? H84D C843 H84E 109.5 . . ? C841 C843 H84F 109.5 . . ? H84D C843 H84F 109.5 . . ? H84E C843 H84F 109.5 . . ? C841 C844 H84G 109.5 . . ? C841 C844 H84H 109.5 . . ? H84G C844 H84H 109.5 . . ? C841 C844 H84I 109.5 . . ? H84G C844 H84I 109.5 . . ? H84H C844 H84I 109.5 . . ? C84 C85 C86 122.2(4) . . ? C84 C85 H85 118.9 . . ? C86 C85 H85 118.9 . . ? C81 C86 C85 119.0(4) . . ? C81 C86 C8 119.9(4) . . ? C85 C86 C8 121.1(4) . . ? C72 C8 C86 114.5(4) . . ? C72 C8 H8A 108.6 . . ? C86 C8 H8A 108.6 . . ? C72 C8 H8B 108.6 . . ? C86 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N101 C102 C103 112.1(9) . . ? N101 C102 H10D 109.2 . . ? C103 C102 H10D 109.2 . . ? N101 C102 H10E 109.2 . . ? C103 C102 H10E 109.2 . . ? H10D C102 H10E 107.9 . . ? N104 C103 C102 116.2(9) . . ? N104 C103 H10F 108.2 . . ? C102 C103 H10F 108.2 . . ? N104 C103 H10G 108.2 . . ? C102 C103 H10G 108.2 . . ? H10F C103 H10G 107.4 . . ? C103 N104 C107 116.0(10) . . ? C103 N104 C105 104.1(9) . . ? C107 N104 C105 119.0(9) . . ? N104 C105 C106 116.1(10) . . ? N104 C105 H10H 108.3 . . ? C106 C105 H10H 108.3 . . ? N104 C105 H10I 108.3 . . ? C106 C105 H10I 108.3 . . ? H10H C105 H10I 107.4 . . ? N104 C107 C108 110.6(11) . . ? N104 C107 H10M 109.5 . . ? C108 C107 H10M 109.5 . . ? N104 C107 H10N 109.5 . . ? C108 C107 H10N 109.5 . . ? H10M C107 H10N 108.1 . . ? C112 N111 H11A 109.5 . . ? C112 N111 H11B 109.5 . . ? H11A N111 H11B 109.5 . . ? C112 N111 H11C 109.5 . . ? H11A N111 H11C 109.5 . . ? H11B N111 H11C 109.5 . . ? N111 C112 C113 107.7(10) . . ? N111 C112 H11D 110.2 . . ? C113 C112 H11D 110.2 . . ? N111 C112 H11E 110.2 . . ? C113 C112 H11E 110.2 . . ? H11D C112 H11E 108.5 . . ? N114 C113 C112 119.0(12) . . ? N114 C113 H11F 107.6 . . ? C112 C113 H11F 107.6 . . ? N114 C113 H11G 107.6 . . ? C112 C113 H11G 107.6 . . ? H11F C113 H11G 107 . . ? C115 N114 C113 106.7(15) . . ? C115 N114 C117 109.7(15) . . ? C113 N114 C117 108.9(13) . . ? N114 C115 C116 124.0(19) . . ? N114 C115 H11H 106.3 . . ? C116 C115 H11H 106.3 . . ? N114 C115 H11I 106.3 . . ? C116 C115 H11I 106.3 . . ? H11H C115 H11I 106.4 . . ? C115 C116 H11J 109.5 . . ? C115 C116 H11K 109.5 . . ? H11J C116 H11K 109.5 . . ? C115 C116 H11L 109.5 . . ? H11J C116 H11L 109.5 . . ? H11K C116 H11L 109.5 . . ? N114 C117 C118 114.5(14) . . ? N114 C117 H11M 108.6 . . ? C118 C117 H11M 108.6 . . ? N114 C117 H11N 108.6 . . ? C118 C117 H11N 108.6 . . ? H11M C117 H11N 107.6 . . ? C117 C118 H11O 109.5 . . ? C117 C118 H11P 109.5 . . ? H11O C118 H11P 109.5 . . ? C117 C118 H11Q 109.5 . . ? H11O C118 H11Q 109.5 . . ? H11P C118 H11Q 109.5 . . ? N201 C202 C203 112.0(8) . . ? N201 C202 H20D 109.2 . . ? C203 C202 H20D 109.2 . . ? N201 C202 H20E 109.2 . . ? C203 C202 H20E 109.2 . . ? H20D C202 H20E 107.9 . . ? N204 C203 C202 112.1(8) . . ? N204 C203 H20F 109.2 . . ? C202 C203 H20F 109.2 . . ? N204 C203 H20G 109.2 . . ? C202 C203 H20G 109.2 . . ? H20F C203 H20G 107.9 . . ? C207 N204 C205 113.1(11) . . ? C207 N204 C203 105.3(9) . . ? C205 N204 C203 109.0(9) . . ? N204 C205 C206 124.6(11) . . ? N204 C205 H20H 106.2 . . ? C206 C205 H20H 106.2 . . ? N204 C205 H20I 106.2 . . ? C206 C205 H20I 106.2 . . ? H20H C205 H20I 106.4 . . ? N204 C207 C208 114.4(15) . . ? N204 C207 H20M 108.7 . . ? C208 C207 H20M 108.7 . . ? N204 C207 H20N 108.7 . . ? C208 C207 H20N 108.7 . . ? H20M C207 H20N 107.6 . . ? C212 N211 H21A 109.5 . . ? C212 N211 H21B 109.5 . . ? H21A N211 H21B 109.5 . . ? C212 N211 H21C 109.5 . . ? H21A N211 H21C 109.5 . . ? H21B N211 H21C 109.5 . . ? N211 C212 C213 106.0(10) . . ? N211 C212 H21D 110.5 . . ? C213 C212 H21D 110.5 . . ? N211 C212 H21E 110.5 . . ? C213 C212 H21E 110.5 . . ? H21D C212 H21E 108.7 . . ? N214 C213 C212 115.3(10) . . ? N214 C213 H21F 108.5 . . ? C212 C213 H21F 108.5 . . ? N214 C213 H21G 108.5 . . ? C212 C213 H21G 108.5 . . ? H21F C213 H21G 107.5 . . ? C213 N214 C217 113.4(10) . . ? C213 N214 C215 112.2(11) . . ? C217 N214 C215 123.7(12) . . ? C216 C215 N214 108.8(15) . . ? C216 C215 H21H 109.9 . . ? N214 C215 H21H 109.9 . . ? C216 C215 H21I 109.9 . . ? N214 C215 H21I 109.9 . . ? H21H C215 H21I 108.3 . . ? C215 C216 H21J 109.5 . . ? C215 C216 H21K 109.5 . . ? H21J C216 H21K 109.5 . . ? C215 C216 H21L 109.5 . . ? H21J C216 H21L 109.5 . . ? H21K C216 H21L 109.5 . . ? N214 C217 C218 107.7(14) . . ? N214 C217 H21M 110.2 . . ? C218 C217 H21M 110.2 . . ? N214 C217 H21N 110.2 . . ? C218 C217 H21N 110.2 . . ? H21M C217 H21N 108.5 . . ? C217 C218 H21O 109.5 . . ? C217 C218 H21P 109.5 . . ? H21O C218 H21P 109.5 . . ? C217 C218 H21Q 109.5 . . ? H21O C218 H21Q 109.5 . . ? H21P C218 H21Q 109.5 . . ? N301 C302 C303 112.1(9) . . ? N301 C302 H30D 109.2 . . ? C303 C302 H30D 109.2 . . ? N301 C302 H30E 109.2 . . ? C303 C302 H30E 109.2 . . ? H30D C302 H30E 107.9 . . ? N304 C303 C302 116.4(10) . . ? N304 C303 H30F 108.2 . . ? C302 C303 H30F 108.2 . . ? N304 C303 H30G 108.2 . . ? C302 C303 H30G 108.2 . . ? H30F C303 H30G 107.3 . . ? C303 N304 C307 124.8(15) . . ? C303 N304 C305 114.5(11) . . ? C307 N304 C305 100.4(14) . . ? N304 C305 C306 105.3(11) . . ? N304 C305 H30H 110.7 . . ? C306 C305 H30H 110.7 . . ? N304 C305 H30I 110.7 . . ? C306 C305 H30I 110.7 . . ? H30H C305 H30I 108.8 . . ? N304 C307 C308 108.5(17) . . ? N304 C307 H30M 110 . . ? C308 C307 H30M 110 . . ? N304 C307 H30N 110 . . ? C308 C307 H30N 110 . . ? H30M C307 H30N 108.4 . . ? C312 N311 H31A 109.5 . . ? C312 N311 H31B 109.5 . . ? H31A N311 H31B 109.5 . . ? C312 N311 H31C 109.5 . . ? H31A N311 H31C 109.5 . . ? H31B N311 H31C 109.5 . . ? N311 C312 C313 110.4(9) . . ? N311 C312 H31D 109.6 . . ? C313 C312 H31D 109.6 . . ? N311 C312 H31E 109.6 . . ? C313 C312 H31E 109.6 . . ? H31D C312 H31E 108.1 . . ? N314 C313 C312 108.5(9) . . ? N314 C313 H31F 110 . . ? C312 C313 H31F 110 . . ? N314 C313 H31G 110 . . ? C312 C313 H31G 110 . . ? H31F C313 H31G 108.4 . . ? C317 N314 C313 104.9(10) . . ? C317 N314 C315 118.9(11) . . ? C313 N314 C315 114.6(11) . . ? C316 C315 N314 97.9(14) . . ? C316 C315 H31H 112.2 . . ? N314 C315 H31H 112.2 . . ? C316 C315 H31I 112.2 . . ? N314 C315 H31I 112.2 . . ? H31H C315 H31I 109.8 . . ? C315 C316 H31J 109.5 . . ? C315 C316 H31K 109.5 . . ? H31J C316 H31K 109.5 . . ? C315 C316 H31L 109.5 . . ? H31J C316 H31L 109.5 . . ? H31K C316 H31L 109.5 . . ? N314 C317 C318 112.1(12) . . ? N314 C317 H31M 109.2 . . ? C318 C317 H31M 109.2 . . ? N314 C317 H31N 109.2 . . ? C318 C317 H31N 109.2 . . ? H31M C317 H31N 107.9 . . ? C317 C318 H31O 109.5 . . ? C317 C318 H31P 109.5 . . ? H31O C318 H31P 109.5 . . ? C317 C318 H31Q 109.5 . . ? H31O C318 H31Q 109.5 . . ? H31P C318 H31Q 109.5 . . ? N401 C402 C403 113.4(10) . . ? N401 C402 H40D 108.9 . . ? C403 C402 H40D 108.9 . . ? N401 C402 H40E 108.9 . . ? C403 C402 H40E 108.9 . . ? H40D C402 H40E 107.7 . . ? N404 C403 C402 106.1(12) . . ? N404 C403 H40F 110.5 . . ? C402 C403 H40F 110.5 . . ? N404 C403 H40G 110.5 . . ? C402 C403 H40G 110.5 . . ? H40F C403 H40G 108.7 . . ? C403 N404 C407 114.7(11) . . ? C403 N404 C405 117.6(11) . . ? C407 N404 C405 101.6(9) . . ? C406 C405 N404 109.4(12) . . ? C406 C405 H40H 109.8 . . ? N404 C405 H40H 109.8 . . ? C406 C405 H40I 109.8 . . ? N404 C405 H40I 109.8 . . ? H40H C405 H40I 108.2 . . ? N404 C407 C408 112.7(11) . . ? N404 C407 H40M 109 . . ? C408 C407 H40M 109 . . ? N404 C407 H40N 109 . . ? C408 C407 H40N 109 . . ? H40M C407 H40N 107.8 . . ? C412 N411 H41A 109.5 . . ? C412 N411 H41B 109.5 . . ? H41A N411 H41B 109.5 . . ? C412 N411 H41C 109.5 . . ? H41A N411 H41C 109.5 . . ? H41B N411 H41C 109.5 . . ? N411 C412 C413 110.8(11) . . ? N411 C412 H41D 109.5 . . ? C413 C412 H41D 109.5 . . ? N411 C412 H41E 109.5 . . ? C413 C412 H41E 109.5 . . ? H41D C412 H41E 108.1 . . ? N414 C413 C412 114.6(15) . . ? N414 C413 H41F 108.6 . . ? C412 C413 H41F 108.6 . . ? N414 C413 H41G 108.6 . . ? C412 C413 H41G 108.6 . . ? H41F C413 H41G 107.6 . . ? C417 N414 C413 98.9(16) . . ? C417 N414 C415 111.9(15) . . ? C413 N414 C415 118.5(17) . . ? N414 C415 C416 93.8(14) . . ? N414 C415 H41H 113 . . ? C416 C415 H41H 113 . . ? N414 C415 H41I 113 . . ? C416 C415 H41I 113 . . ? H41H C415 H41I 110.4 . . ? C415 C416 H41J 109.5 . . ? C415 C416 H41K 109.5 . . ? H41J C416 H41K 109.5 . . ? C415 C416 H41L 109.5 . . ? H41J C416 H41L 109.5 . . ? H41K C416 H41L 109.5 . . ? N414 C417 C418 134.4(18) . . ? N414 C417 H41M 103.6 . . ? C418 C417 H41M 103.6 . . ? N414 C417 H41N 103.6 . . ? C418 C417 H41N 103.6 . . ? H41M C417 H41N 105.3 . . ? C417 C418 H41O 109.5 . . ? C417 C418 H41P 109.5 . . ? H41O C418 H41P 109.5 . . ? C417 C418 H41Q 109.5 . . ? H41O C418 H41Q 109.5 . . ? H41P C418 H41Q 109.5 . . ? Cl12 C10 Cl11 114.1(3) . . ? Cl12 C10 H10R 108.7 . . ? Cl11 C10 H10R 108.7 . . ? Cl12 C10 H10S 108.7 . . ? Cl11 C10 H10S 108.7 . . ? H10R C10 H10S 107.6 . . ? Cl21 C20 Cl22 107.3(12) . . ? Cl21 C20 H20R 110.3 . . ? Cl22 C20 H20R 110.3 . . ? Cl21 C20 H20S 110.3 . . ? Cl22 C20 H20S 110.3 . . ? H20R C20 H20S 108.5 . . ? Cl24 C20' Cl23 118.9(9) . . ? Cl24 C20' H20T 107.6 . . ? Cl23 C20' H20T 107.6 . . ? Cl24 C20' H20U 107.6 . . ? Cl23 C20' H20U 107.6 . . ? H20T C20' H20U 107 . . ? Cl31 C30 Cl32 108.8(6) . . ? Cl31 C30 H30R 109.9 . . ? Cl32 C30 H30R 109.9 . . ? Cl31 C30 H30S 109.9 . . ? Cl32 C30 H30S 109.9 . . ? H30R C30 H30S 108.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N101 H10A O81 0.91 1.9 2.785(10) 164.9 . N101 H10A O102 0.91 2.89 3.292(10) 108.3 . N101 H10B Cl2 0.91 2.92 3.331(10) 109.3 2_656 N101 H10C Cl2 0.91 2.37 3.261(9) 165.2 . N111 H11A O81 0.91 1.98 2.890(11) 173.8 . N111 H11B Cl2 0.91 2.62 3.308(11) 132.6 2_656 N111 H11C Cl2 0.91 2.07 2.960(10) 167.5 . N201 H20A Cl1 0.91 2.23 3.120(10) 165.2 2_656 N201 H20B Cl3 0.91 2.35 3.030(10) 131.5 2_656 N201 H20C O51 0.91 1.89 2.794(10) 172.5 . N211 H21A Cl1 0.91 2.31 3.223(12) 177.4 2_656 N211 H21B Cl3 0.91 2.43 3.148(12) 136.3 2_656 N211 H21C O51 0.91 1.81 2.722(11) 174.7 . N301 H30A O41 0.91 1.82 2.716(9) 167.7 . N301 H30B Cl1 0.91 2.8 3.263(8) 112.8 . N301 H30C Cl1 0.91 2.13 2.980(8) 154.5 2_656 N311 H31A O41 0.91 2.01 2.842(9) 151.8 . N311 H31B Cl1 0.91 2.55 3.353(9) 147.5 . N311 H31C Cl1 0.91 2.34 3.219(9) 163.7 2_656 N401 H40A Cl2 0.91 2.08 2.959(8) 161.5 . N401 H40B Cl3 0.91 2.41 3.131(8) 135.8 . N401 H40C O11 0.91 1.96 2.861(8) 168.2 . N411 H41A Cl2 0.91 2.46 3.358(8) 170.7 . N411 H41B Cl3 0.91 2.58 3.229(9) 128.5 . N411 H41C O11 0.91 1.78 2.689(9) 174.6 . #===END # Attachment '- mo7c_1a.cif' data_mo7c _database_code_depnum_ccdc_archive 'CCDC 773078' #TrackingRef '- mo7c_1a.cif' _audit_creation_date 2010-04-14T13:00:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C117 H179 N11 O16 S0.50 U2' _chemical_formula_moiety ; 3(C6 H17 N2), C88 H105 O13 U2, 0.5(C2 H6 S O), 5(C2 H3 N), 5/2( H2 O) ; _chemical_formula_weight 2493.87 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 21.4450(10) _cell_length_b 23.3490(10) _cell_length_c 28.256(2) _cell_angle_alpha 89.153(2) _cell_angle_beta 76.002(2) _cell_angle_gamma 66.2570(10) _cell_volume 12511.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 20.3 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description bar _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5139 _exptl_special_details ; ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .46 _exptl_absorpt_correction_T_max .65 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_unetI/netI 0.1914 _diffrn_reflns_number 217684 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 35.1 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.926 _reflns_number_total 102812 _reflns_number_gt 40756 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP2 _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 102812 _refine_ls_number_parameters 2746 _refine_ls_number_restraints 616 _refine_ls_R_factor_all 0.1693 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.128 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 4.536 _refine_diff_density_min -1.719 _refine_diff_density_rms 0.17 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 U11 U 0.403036(9) 0.189148(8) 0.451945(6) 0.01921(4) Uani 1 1 d . . . U12 U 0.209743(9) 0.155419(9) 0.457229(6) 0.02118(4) Uani 1 1 d . . . U21 U 0.799370(8) 0.344751(9) 0.026070(6) 0.02006(4) Uani 1 1 d . . . U22 U 0.605986(8) 0.311206(8) 0.036075(6) 0.01750(4) Uani 1 1 d . . . O10 O 0.28802(15) 0.20349(15) 0.45309(10) 0.0205(7) Uani 1 1 d . . . H10 H 0.2623 0.247 0.451 0.025 Uiso 1 1 calc R . . O101 O 0.37226(16) 0.27195(14) 0.44571(11) 0.0237(7) Uani 1 1 d . . . O102 O 0.43254(17) 0.10651(15) 0.46060(11) 0.0257(8) Uani 1 1 d . . . O103 O 0.14770(16) 0.23286(16) 0.45157(12) 0.0289(8) Uani 1 1 d . . . O104 O 0.27320(16) 0.07859(15) 0.46257(12) 0.0266(8) Uani 1 1 d . . . O20 O 0.72287(15) 0.29493(15) 0.03206(10) 0.0180(7) Uani 1 1 d . . . H20 H 0.7491 0.2513 0.0334 0.022 Uiso 1 1 calc R . . O201 O 0.86405(16) 0.26742(15) 0.02844(12) 0.0270(8) Uani 1 1 d . . . O202 O 0.73596(15) 0.42122(15) 0.02120(11) 0.0250(8) Uani 1 1 d . . . O203 O 0.63581(16) 0.22873(14) 0.04294(11) 0.0229(7) Uani 1 1 d . . . O204 O 0.57671(16) 0.39376(14) 0.02928(11) 0.0225(7) Uani 1 1 d . . . O111 O 0.50955(15) 0.17447(14) 0.40443(10) 0.0205(7) Uani 1 1 d . . . C111 C 0.5425(2) 0.2115(2) 0.38501(15) 0.0194(10) Uani 1 1 d . . . C112 C 0.5297(2) 0.2410(2) 0.34212(15) 0.0185(9) Uani 1 1 d . . . C113 C 0.5669(2) 0.2753(2) 0.32126(16) 0.0204(10) Uani 1 1 d . . . H113 H 0.5593 0.2931 0.2916 0.024 Uiso 1 1 calc R . . C114 C 0.6154(2) 0.2849(2) 0.34187(16) 0.0200(10) Uani 1 1 d . . . C117 C 0.6585(3) 0.3210(2) 0.31613(18) 0.0302(11) Uani 1 1 d U . . C118 C 0.6106(3) 0.3833(3) 0.3024(3) 0.073(2) Uani 1 1 d U . . H11A H 0.574 0.4074 0.3317 0.11 Uiso 1 1 calc R . . H11B H 0.5885 0.3758 0.278 0.11 Uiso 1 1 calc R . . H11C H 0.6384 0.4071 0.2887 0.11 Uiso 1 1 calc R . . C119 C 0.7060(4) 0.2844(4) 0.2675(3) 0.083(3) Uani 1 1 d U . . H11D H 0.7286 0.3096 0.2488 0.125 Uiso 1 1 calc R . . H11E H 0.6778 0.2748 0.2489 0.125 Uiso 1 1 calc R . . H11F H 0.7423 0.2451 0.2736 0.125 Uiso 1 1 calc R . . C110 C 0.6976(4) 0.3357(3) 0.3476(2) 0.0683(18) Uani 1 1 d U . . H11G H 0.7316 0.2965 0.3557 0.102 Uiso 1 1 calc R . . H11H H 0.6642 0.3604 0.3778 0.102 Uiso 1 1 calc R . . H11I H 0.7226 0.3598 0.3299 0.102 Uiso 1 1 calc R . . C115 C 0.6259(2) 0.2573(2) 0.38511(16) 0.0199(10) Uani 1 1 d . . . H115 H 0.659 0.2627 0.3997 0.024 Uiso 1 1 calc R . . C116 C 0.5900(2) 0.2226(2) 0.40748(14) 0.0160(9) Uani 1 1 d . . . C11 C 0.5970(2) 0.1977(2) 0.45612(15) 0.0245(11) Uani 1 1 d . . . H11J H 0.5886 0.1589 0.4583 0.029 Uiso 1 1 calc R . . H11K H 0.6455 0.1869 0.4589 0.029 Uiso 1 1 calc R . . O121 O 0.39784(15) 0.16383(14) 0.37013(10) 0.0193(7) Uani 1 1 d U . . C121 C 0.4536(2) 0.1333(2) 0.33170(15) 0.0182(9) Uani 1 1 d U . . C122 C 0.4721(2) 0.0703(2) 0.31647(15) 0.0176(9) Uani 1 1 d . . . C123 C 0.5307(2) 0.0400(2) 0.27642(17) 0.0229(10) Uani 1 1 d . . . H123 H 0.543 -0.0027 0.2665 0.027 Uiso 1 1 calc R . . C124 C 0.5711(2) 0.0695(2) 0.25085(16) 0.0225(10) Uani 1 1 d . . . C127 C 0.6353(3) 0.0335(2) 0.20709(18) 0.0281(12) Uani 1 1 d . . . C128 C 0.6947(3) -0.0143(3) 0.2270(2) 0.0401(15) Uani 1 1 d . . . H12A H 0.6772 -0.042 0.247 0.06 Uiso 1 1 calc R . . H12B H 0.7105 0.0082 0.2472 0.06 Uiso 1 1 calc R . . H12C H 0.7344 -0.0394 0.1996 0.06 Uiso 1 1 calc R . . C129 C 0.6148(3) -0.0008(3) 0.17224(18) 0.0344(13) Uani 1 1 d . . . H12D H 0.576 0.0296 0.1603 0.052 Uiso 1 1 calc R . . H12E H 0.5996 -0.0316 0.1896 0.052 Uiso 1 1 calc R . . H12F H 0.6555 -0.0225 0.1444 0.052 Uiso 1 1 calc R . . C120 C 0.6635(3) 0.0781(3) 0.1789(2) 0.0443(16) Uani 1 1 d . . . H12G H 0.7015 0.0547 0.1501 0.066 Uiso 1 1 calc R . . H12H H 0.6818 0.0967 0.2001 0.066 Uiso 1 1 calc R . . H12I H 0.6254 0.1115 0.1685 0.066 Uiso 1 1 calc R . . C125 C 0.5515(2) 0.1318(2) 0.26682(15) 0.0189(9) Uani 1 1 d . . . H125 H 0.5791 0.153 0.2505 0.023 Uiso 1 1 calc R . . C126 C 0.4934(2) 0.1646(2) 0.30557(15) 0.0179(9) Uani 1 1 d . . . C12 C 0.4760(2) 0.2322(2) 0.32007(15) 0.0177(9) Uani 1 1 d . . . H12J H 0.4294 0.2504 0.3441 0.021 Uiso 1 1 calc R . . H12K H 0.4724 0.2559 0.2908 0.021 Uiso 1 1 calc R . . O131 O 0.29182(15) 0.14401(15) 0.37067(11) 0.0211(7) Uani 1 1 d U . . C131 C 0.3044(2) 0.1000(2) 0.33257(16) 0.0232(10) Uani 1 1 d U . . C132 C 0.2517(2) 0.1124(2) 0.30749(16) 0.0214(10) Uani 1 1 d . . . C133 C 0.2629(2) 0.0673(2) 0.27120(16) 0.0255(11) Uani 1 1 d . . . H133 H 0.2275 0.0748 0.2543 0.031 Uiso 1 1 calc R . . C134 C 0.3222(3) 0.0128(2) 0.25866(17) 0.0299(12) Uani 1 1 d . . . C137 C 0.3312(3) -0.0362(3) 0.2183(2) 0.0412(14) Uani 1 1 d U . . C138 C 0.2756(4) -0.0634(3) 0.2354(3) 0.065(2) Uani 1 1 d U . . H13A H 0.2835 -0.0857 0.2645 0.098 Uiso 1 1 calc R . . H13B H 0.2796 -0.0927 0.2092 0.098 Uiso 1 1 calc R . . H13C H 0.2283 -0.0291 0.2434 0.098 Uiso 1 1 calc R . . C139 C 0.3181(4) -0.0021(3) 0.1709(2) 0.062(2) Uani 1 1 d U . . H13D H 0.2717 0.0333 0.179 0.092 Uiso 1 1 calc R . . H13E H 0.3198 -0.0318 0.1459 0.092 Uiso 1 1 calc R . . H13F H 0.3546 0.0134 0.1583 0.092 Uiso 1 1 calc R . . C130 C 0.4042(3) -0.0898(3) 0.2056(2) 0.0545(18) Uani 1 1 d U . . H13G H 0.44 -0.0727 0.1971 0.082 Uiso 1 1 calc R . . H13H H 0.409 -0.117 0.1777 0.082 Uiso 1 1 calc R . . H13I H 0.4108 -0.1143 0.2339 0.082 Uiso 1 1 calc R . . C135 C 0.3757(3) 0.0030(2) 0.28228(16) 0.0271(11) Uani 1 1 d . . . H135 H 0.4185 -0.0337 0.2729 0.032 Uiso 1 1 calc R . . C136 C 0.3671(2) 0.0465(2) 0.31943(16) 0.0228(10) Uani 1 1 d . . . C13 C 0.4273(2) 0.0382(2) 0.34148(16) 0.0217(10) Uani 1 1 d . . . H13J H 0.4078 0.0548 0.3764 0.026 Uiso 1 1 calc R . . H13K H 0.4572 -0.0072 0.3401 0.026 Uiso 1 1 calc R . . O141 O 0.16762(16) 0.11863(16) 0.40533(11) 0.0249(8) Uani 1 1 d . . . C141 C 0.1145(2) 0.1366(2) 0.38398(17) 0.0261(11) Uani 1 1 d . . . C142 C 0.0525(3) 0.1280(3) 0.40420(18) 0.0318(12) Uani 1 1 d . A . C143 C -0.0018(3) 0.1481(3) 0.38044(19) 0.0355(13) Uani 1 1 d . . . H143 H -0.0439 0.143 0.3951 0.043 Uiso 1 1 calc R . . C144 C 0.0031(3) 0.1754(3) 0.33621(19) 0.0354(13) Uani 1 1 d . . . C147 C -0.0552(3) 0.1934(4) 0.3097(3) 0.071(2) Uani 1 1 d U . . C148 C -0.0776(4) 0.2609(4) 0.2978(4) 0.111(3) Uani 1 1 d U . . H14A H -0.1066 0.2689 0.2745 0.166 Uiso 1 1 calc R . . H14B H -0.0357 0.2687 0.2833 0.166 Uiso 1 1 calc R . . H14C H -0.1049 0.2889 0.3279 0.166 Uiso 1 1 calc R . . C149 C -0.1126(4) 0.1782(4) 0.3314(3) 0.102(3) Uani 1 1 d U . . H14D H -0.1407 0.2058 0.3616 0.152 Uiso 1 1 calc R . . H14E H -0.0947 0.1344 0.3392 0.152 Uiso 1 1 calc R . . H14F H -0.142 0.1839 0.3086 0.152 Uiso 1 1 calc R . . C140 C -0.0261(4) 0.1580(5) 0.2570(3) 0.108(3) Uani 1 1 d U . . H14G H -0.0009 0.1129 0.259 0.162 Uiso 1 1 calc R . . H14H H 0.0062 0.174 0.2365 0.162 Uiso 1 1 calc R . . H14I H -0.0655 0.1651 0.2425 0.162 Uiso 1 1 calc R . . C145 C 0.0654(2) 0.1835(2) 0.31646(18) 0.0301(12) Uani 1 1 d . . . H145 H 0.0702 0.2026 0.2867 0.036 Uiso 1 1 calc R . . C146 C 0.1204(2) 0.1642(2) 0.33948(16) 0.0242(10) Uani 1 1 d . . . C14 C 0.1866(2) 0.1730(2) 0.31764(17) 0.0264(11) Uani 1 1 d . . . H14J H 0.1914 0.202 0.3404 0.032 Uiso 1 1 calc R . . H14K H 0.1828 0.1928 0.2866 0.032 Uiso 1 1 calc R . . O151 O 0.12117(16) 0.13626(16) 0.51015(11) 0.0253(8) Uani 1 1 d . . . C151 C 0.0501(2) 0.1704(3) 0.51900(17) 0.0297(12) Uani 1 1 d U . . C152 C 0.0168(3) 0.2228(3) 0.55398(18) 0.0366(13) Uani 1 1 d U . . C153 C -0.0568(3) 0.2537(3) 0.56617(19) 0.0400(15) Uani 1 1 d U . . H153 H -0.0794 0.288 0.5909 0.048 Uiso 1 1 calc R . . C154 C -0.0982(3) 0.2363(3) 0.5435(2) 0.0475(17) Uani 1 1 d U A . C157 C -0.1792(3) 0.2721(4) 0.5578(2) 0.0618(19) Uani 1 1 d U . . C158 C -0.2009(7) 0.3422(6) 0.5540(5) 0.058(3) Uiso 0.5 1 d PU A 1 H15A H -0.2524 0.3636 0.5613 0.087 Uiso 0.5 1 calc PR A 1 H15B H -0.1802 0.3492 0.5207 0.087 Uiso 0.5 1 calc PR A 1 H15C H -0.1841 0.3589 0.5774 0.087 Uiso 0.5 1 calc PR A 1 C159 C -0.2142(7) 0.2448(7) 0.5265(5) 0.060(4) Uiso 0.5 1 d PU A 1 H15D H -0.2655 0.2684 0.5365 0.09 Uiso 0.5 1 calc PR A 1 H15E H -0.2023 0.2004 0.5317 0.09 Uiso 0.5 1 calc PR A 1 H15F H -0.1967 0.2485 0.4917 0.09 Uiso 0.5 1 calc PR A 1 C150 C -0.2074(8) 0.2613(7) 0.6108(5) 0.061(4) Uiso 0.5 1 d PU A 1 H15G H -0.194 0.2835 0.633 0.091 Uiso 0.5 1 calc PR A 1 H15H H -0.1873 0.2162 0.6147 0.091 Uiso 0.5 1 calc PR A 1 H15I H -0.2589 0.2773 0.6186 0.091 Uiso 0.5 1 calc PR A 1 C15A C -0.2063(10) 0.3252(9) 0.5920(7) 0.107(5) Uiso 0.5 1 d PU A 2 H15J H -0.1964 0.3593 0.5759 0.16 Uiso 0.5 1 calc PR A 2 H15K H -0.1838 0.3143 0.6191 0.16 Uiso 0.5 1 calc PR A 2 H15L H -0.2573 0.339 0.6046 0.16 Uiso 0.5 1 calc PR A 2 C15B C -0.2082(9) 0.2876(8) 0.5161(6) 0.087(5) Uiso 0.5 1 d PU A 2 H15M H -0.2598 0.3051 0.5271 0.13 Uiso 0.5 1 calc PR A 2 H15N H -0.1911 0.2496 0.4938 0.13 Uiso 0.5 1 calc PR A 2 H15O H -0.1935 0.3187 0.499 0.13 Uiso 0.5 1 calc PR A 2 C15C C -0.2082(11) 0.2262(9) 0.5884(7) 0.110(6) Uiso 0.5 1 d PU A 2 H15P H -0.203 0.2277 0.6218 0.165 Uiso 0.5 1 calc PR A 2 H15Q H -0.1813 0.1832 0.5728 0.165 Uiso 0.5 1 calc PR A 2 H15R H -0.2581 0.2394 0.5895 0.165 Uiso 0.5 1 calc PR A 2 C155 C -0.0646(3) 0.1861(3) 0.50780(19) 0.0423(15) Uani 1 1 d U . . H155 H -0.0918 0.1735 0.4917 0.051 Uiso 1 1 calc R A . C156 C 0.0092(3) 0.1534(3) 0.49495(18) 0.0379(14) Uani 1 1 d U A . C15 C 0.0405(3) 0.1041(2) 0.45473(17) 0.0302(11) Uani 1 1 d . . . H15S H 0.0094 0.0819 0.4564 0.036 Uiso 1 1 calc R A . H15T H 0.0863 0.0733 0.4589 0.036 Uiso 1 1 calc R . . O161 O 0.21152(16) 0.18575(16) 0.54075(11) 0.0256(8) Uani 1 1 d . . . C161 C 0.1815(2) 0.1725(2) 0.58528(15) 0.0242(11) Uani 1 1 d . . . C162 C 0.2244(2) 0.1326(2) 0.61326(16) 0.0243(11) Uani 1 1 d . . . C163 C 0.1936(2) 0.1190(2) 0.65919(16) 0.0243(11) Uani 1 1 d . . . H163 H 0.2233 0.0918 0.6776 0.029 Uiso 1 1 calc R . . C164 C 0.1196(2) 0.1445(2) 0.67890(17) 0.0281(11) Uani 1 1 d . . . C167 C 0.0900(3) 0.1269(3) 0.72921(17) 0.0312(12) Uani 1 1 d . . . C168 C 0.1174(3) 0.0546(3) 0.7296(2) 0.0435(15) Uani 1 1 d . . . H16A H 0.1029 0.0378 0.7047 0.065 Uiso 1 1 calc R . . H16B H 0.0976 0.0443 0.762 0.065 Uiso 1 1 calc R . . H16C H 0.1689 0.036 0.7226 0.065 Uiso 1 1 calc R . . C169 C 0.0087(3) 0.1546(3) 0.74341(18) 0.0378(14) Uani 1 1 d . . . H16D H -0.01 0.2005 0.7439 0.057 Uiso 1 1 calc R . . H16E H -0.0081 0.143 0.7759 0.057 Uiso 1 1 calc R . . H16F H -0.0073 0.1379 0.7194 0.057 Uiso 1 1 calc R . . C160 C 0.1140(3) 0.1530(3) 0.76747(18) 0.0406(15) Uani 1 1 d . . . H16G H 0.1655 0.1377 0.7578 0.061 Uiso 1 1 calc R . . H16H H 0.0992 0.1389 0.7994 0.061 Uiso 1 1 calc R . . H16I H 0.0927 0.199 0.7696 0.061 Uiso 1 1 calc R . . C165 C 0.0787(2) 0.1842(3) 0.65044(17) 0.0321(13) Uani 1 1 d . . . H165 H 0.0289 0.2025 0.663 0.039 Uiso 1 1 calc R . . C166 C 0.1078(3) 0.1985(3) 0.60385(17) 0.0301(12) Uani 1 1 d . . . C16 C 0.0600(3) 0.2462(3) 0.57751(17) 0.0323(13) Uani 1 1 d . . . H16J H 0.0891 0.2608 0.5517 0.039 Uiso 1 1 calc R . . H16K H 0.0272 0.283 0.6011 0.039 Uiso 1 1 calc R . . O171 O 0.31849(16) 0.20659(16) 0.53862(10) 0.0244(8) Uani 1 1 d U . . C171 C 0.3317(2) 0.2046(2) 0.58415(16) 0.0228(10) Uani 1 1 d U . . C172 C 0.3496(2) 0.2506(2) 0.60057(16) 0.0222(10) Uani 1 1 d . . . C173 C 0.3641(2) 0.2480(2) 0.64580(16) 0.0240(11) Uani 1 1 d . . . H173 H 0.3769 0.2792 0.6565 0.029 Uiso 1 1 calc R . . C174 C 0.3608(2) 0.2013(2) 0.67638(16) 0.0242(11) Uani 1 1 d . . . C177 C 0.3763(3) 0.2012(3) 0.72657(18) 0.0351(12) Uani 1 1 d U . . C178 C 0.3210(5) 0.2617(4) 0.7571(2) 0.096(3) Uani 1 1 d U . . H17A H 0.3307 0.2638 0.789 0.144 Uiso 1 1 calc R . . H17B H 0.274 0.2621 0.7618 0.144 Uiso 1 1 calc R . . H17C H 0.3229 0.298 0.7399 0.144 Uiso 1 1 calc R . . C179 C 0.4428(4) 0.2079(5) 0.7230(3) 0.095(3) Uani 1 1 d U . . H17D H 0.4826 0.1701 0.7051 0.142 Uiso 1 1 calc R . . H17E H 0.4479 0.2135 0.756 0.142 Uiso 1 1 calc R . . H17F H 0.4421 0.2446 0.7055 0.142 Uiso 1 1 calc R . . C170 C 0.3728(5) 0.1459(4) 0.7536(2) 0.095(3) Uani 1 1 d . . . H17G H 0.4121 0.1072 0.7367 0.142 Uiso 1 1 calc R . . H17H H 0.3281 0.1433 0.7546 0.142 Uiso 1 1 calc R . . H17I H 0.3761 0.1514 0.7871 0.142 Uiso 1 1 calc R . . C175 C 0.3425(2) 0.1562(2) 0.65863(16) 0.0224(10) Uani 1 1 d . . . H175 H 0.3402 0.1235 0.6785 0.027 Uiso 1 1 calc R . . C176 C 0.3276(2) 0.1567(2) 0.61333(15) 0.0189(10) Uani 1 1 d . . . C17 C 0.3041(2) 0.1095(2) 0.59703(17) 0.0224(10) Uani 1 1 d . . . H17J H 0.3262 0.0693 0.611 0.027 Uiso 1 1 calc R . . H17K H 0.32 0.1015 0.5609 0.027 Uiso 1 1 calc R . . O181 O 0.46162(15) 0.19892(14) 0.50797(10) 0.0195(7) Uani 1 1 d U . . C181 C 0.4786(2) 0.2461(2) 0.51864(15) 0.0205(10) Uani 1 1 d U . . C182 C 0.5452(2) 0.2454(2) 0.49730(15) 0.0211(10) Uani 1 1 d . . . C183 C 0.5616(2) 0.2939(2) 0.51230(16) 0.0231(10) Uani 1 1 d . . . H183 H 0.6077 0.2918 0.4989 0.028 Uiso 1 1 calc R . . C184 C 0.5133(2) 0.3449(2) 0.54590(17) 0.0247(11) Uani 1 1 d . . . C187 C 0.5350(3) 0.3943(3) 0.5628(2) 0.0373(14) Uani 1 1 d . . . C188 C 0.5705(4) 0.3711(4) 0.6032(3) 0.073(2) Uani 1 1 d . . . H18A H 0.5398 0.3591 0.6292 0.11 Uiso 1 1 calc R . . H18B H 0.5797 0.4046 0.6166 0.11 Uiso 1 1 calc R . . H18C H 0.6151 0.3346 0.5903 0.11 Uiso 1 1 calc R . . C189 C 0.5849(4) 0.4083(4) 0.5194(3) 0.081(2) Uani 1 1 d . . . H18D H 0.5928 0.4443 0.5294 0.121 Uiso 1 1 calc R . . H18E H 0.5636 0.4179 0.4917 0.121 Uiso 1 1 calc R . . H18F H 0.6301 0.3714 0.5097 0.121 Uiso 1 1 calc R . . C180 C 0.4716(3) 0.4567(3) 0.5829(3) 0.060(2) Uani 1 1 d . . . H18G H 0.4374 0.4492 0.6093 0.091 Uiso 1 1 calc R . . H18H H 0.4494 0.475 0.5566 0.091 Uiso 1 1 calc R . . H18I H 0.4875 0.4858 0.5957 0.091 Uiso 1 1 calc R . . C185 C 0.4462(3) 0.3464(2) 0.56388(17) 0.0268(11) Uani 1 1 d . . . H185 H 0.4115 0.3812 0.5858 0.032 Uiso 1 1 calc R . . C186 C 0.4276(2) 0.2989(2) 0.55099(15) 0.0220(10) Uani 1 1 d . . . C18 C 0.3539(2) 0.3031(2) 0.57007(16) 0.0229(10) Uani 1 1 d . . . H18J H 0.3243 0.3437 0.5901 0.027 Uiso 1 1 calc R . . H18K H 0.334 0.3026 0.5419 0.027 Uiso 1 1 calc R . . O211 O 0.85006(15) 0.38051(15) 0.07047(11) 0.0227(7) Uani 1 1 d . . . C211 C 0.9093(2) 0.3578(2) 0.08659(16) 0.0195(9) Uani 1 1 d U . . C212 C 0.9094(2) 0.3283(2) 0.13039(16) 0.0227(10) Uani 1 1 d U . . C213 C 0.9711(2) 0.3054(2) 0.14589(17) 0.0274(11) Uani 1 1 d U . . H213 H 0.9711 0.2853 0.1753 0.033 Uiso 1 1 calc R . . C214 C 1.0327(2) 0.3104(3) 0.12079(17) 0.0299(12) Uani 1 1 d U . . C217 C 1.0995(3) 0.2825(3) 0.1388(2) 0.0412(14) Uani 1 1 d U . . C218 C 1.1174(4) 0.2121(4) 0.1460(3) 0.079(2) Uani 1 1 d U . . H21A H 1.1572 0.1951 0.161 0.119 Uiso 1 1 calc R . . H21B H 1.1299 0.1886 0.1142 0.119 Uiso 1 1 calc R . . H21C H 1.0762 0.208 0.1675 0.119 Uiso 1 1 calc R . . C219 C 1.0884(3) 0.3158(4) 0.1873(2) 0.074(2) Uani 1 1 d U . . H21D H 1.0851 0.3584 0.1825 0.111 Uiso 1 1 calc R . . H21E H 1.1282 0.2927 0.2013 0.111 Uiso 1 1 calc R . . H21F H 1.0447 0.3178 0.2097 0.111 Uiso 1 1 calc R . . C210 C 1.1644(3) 0.2835(4) 0.1015(2) 0.0586(19) Uani 1 1 d U . . H21G H 1.1587 0.3271 0.0982 0.088 Uiso 1 1 calc R . . H21H H 1.1691 0.2639 0.0696 0.088 Uiso 1 1 calc R . . H21I H 1.2068 0.2602 0.1127 0.088 Uiso 1 1 calc R . . C215 C 1.0297(2) 0.3418(2) 0.07886(17) 0.0265(11) Uani 1 1 d U . . H215 H 1.0701 0.3479 0.0618 0.032 Uiso 1 1 calc R . . C216 C 0.9702(2) 0.3648(2) 0.06045(16) 0.0204(10) Uani 1 1 d U . . C21 C 0.9741(3) 0.3911(2) 0.01202(15) 0.0258(11) Uani 1 1 d . . . H21J H 0.9268 0.4229 0.0114 0.031 Uiso 1 1 calc R . . H21K H 1.0067 0.4122 0.0072 0.031 Uiso 1 1 calc R . . O221 O 0.72995(15) 0.35453(15) 0.11252(10) 0.0208(7) Uani 1 1 d . . . C221 C 0.7239(2) 0.3943(2) 0.15040(15) 0.0211(10) Uani 1 1 d . . . C222 C 0.6634(2) 0.4484(2) 0.16751(16) 0.0204(10) Uani 1 1 d . . . C223 C 0.6594(2) 0.4891(2) 0.20470(15) 0.0214(10) Uani 1 1 d . . . H223 H 0.6173 0.5261 0.2157 0.026 Uiso 1 1 calc R . . C224 C 0.7146(2) 0.4776(2) 0.22658(16) 0.0259(11) Uani 1 1 d . . . C227 C 0.7123(3) 0.5234(2) 0.26529(18) 0.0312(12) Uani 1 1 d . . . C228 C 0.7271(4) 0.4908(3) 0.3109(2) 0.0559(19) Uani 1 1 d . . . H22A H 0.6906 0.4757 0.3248 0.084 Uiso 1 1 calc R . . H22B H 0.7268 0.5206 0.3351 0.084 Uiso 1 1 calc R . . H22C H 0.7733 0.4552 0.3021 0.084 Uiso 1 1 calc R . . C229 C 0.6399(3) 0.5790(3) 0.2821(2) 0.0475(16) Uani 1 1 d . . . H22D H 0.6287 0.6027 0.2541 0.071 Uiso 1 1 calc R . . H22E H 0.6409 0.6066 0.3074 0.071 Uiso 1 1 calc R . . H22F H 0.6038 0.5633 0.2954 0.071 Uiso 1 1 calc R . . C220 C 0.7671(3) 0.5497(3) 0.2451(2) 0.0539(17) Uani 1 1 d . . . H22G H 0.8141 0.5151 0.2358 0.081 Uiso 1 1 calc R . . H22H H 0.7655 0.579 0.2703 0.081 Uiso 1 1 calc R . . H22I H 0.7568 0.5718 0.2163 0.081 Uiso 1 1 calc R . . C225 C 0.7737(2) 0.4215(2) 0.20962(15) 0.0235(10) Uani 1 1 d . . . H225 H 0.812 0.4112 0.2242 0.028 Uiso 1 1 calc R . . C226 C 0.7798(2) 0.3801(2) 0.17275(15) 0.0213(10) Uani 1 1 d . . . C22 C 0.8450(2) 0.3190(2) 0.15735(17) 0.0236(10) Uani 1 1 d . . . H22J H 0.8544 0.2973 0.1869 0.028 Uiso 1 1 calc R . . H22K H 0.8359 0.2916 0.1361 0.028 Uiso 1 1 calc R . . O231 O 0.62284(15) 0.33631(14) 0.11773(10) 0.0185(7) Uani 1 1 d . . . C231 C 0.5701(2) 0.3669(2) 0.15984(15) 0.0176(9) Uani 1 1 d . . . C232 C 0.5336(2) 0.3344(2) 0.18638(14) 0.0181(9) Uani 1 1 d . . . C233 C 0.4781(2) 0.3669(2) 0.22702(15) 0.0202(10) Uani 1 1 d . . . H233 H 0.4513 0.3458 0.2445 0.024 Uiso 1 1 calc R . . C234 C 0.4603(2) 0.4287(2) 0.24308(15) 0.0204(10) Uani 1 1 d . . . C237 C 0.3973(2) 0.4641(2) 0.28719(17) 0.0258(11) Uani 1 1 d . . . C238 C 0.3377(3) 0.5157(2) 0.26803(19) 0.0361(14) Uani 1 1 d . . . H23A H 0.3259 0.4962 0.243 0.054 Uiso 1 1 calc R . . H23B H 0.3541 0.5473 0.2538 0.054 Uiso 1 1 calc R . . H23C H 0.2957 0.5359 0.2953 0.054 Uiso 1 1 calc R . . C239 C 0.3679(3) 0.4211(3) 0.31630(18) 0.0354(14) Uani 1 1 d . . . H23D H 0.3488 0.4026 0.2956 0.053 Uiso 1 1 calc R . . H23E H 0.3304 0.4454 0.3451 0.053 Uiso 1 1 calc R . . H23F H 0.4057 0.3875 0.3269 0.053 Uiso 1 1 calc R . . C230 C 0.4195(3) 0.4976(3) 0.32224(18) 0.0379(14) Uani 1 1 d . . . H23G H 0.3778 0.5245 0.3477 0.057 Uiso 1 1 calc R . . H23H H 0.4416 0.5235 0.3038 0.057 Uiso 1 1 calc R . . H23I H 0.4532 0.4662 0.3375 0.057 Uiso 1 1 calc R . . C235 C 0.5001(2) 0.4584(2) 0.21593(15) 0.0194(9) Uani 1 1 d . . . H235 H 0.4893 0.5007 0.2259 0.023 Uiso 1 1 calc R . . C236 C 0.5552(2) 0.4280(2) 0.17466(15) 0.0170(9) Uani 1 1 d . . . C23 C 0.5988(2) 0.4622(2) 0.14798(15) 0.0198(10) Uani 1 1 d . . . H23J H 0.5694 0.508 0.1524 0.024 Uiso 1 1 calc R . . H23K H 0.6142 0.4486 0.1125 0.024 Uiso 1 1 calc R . . O241 O 0.50385(15) 0.32797(14) 0.09186(10) 0.0178(7) Uani 1 1 d U . . C241 C 0.4717(2) 0.29158(19) 0.11422(14) 0.0146(9) Uani 1 1 d U . . C242 C 0.4184(2) 0.2849(2) 0.09813(15) 0.0171(9) Uani 1 1 d . . . C243 C 0.3830(2) 0.2503(2) 0.12322(16) 0.0204(10) Uani 1 1 d . . . H243 H 0.3466 0.2462 0.1118 0.024 Uiso 1 1 calc R . . C244 C 0.4000(2) 0.2215(2) 0.16467(16) 0.0209(10) Uani 1 1 d . . . C247 C 0.3609(2) 0.1844(2) 0.19461(17) 0.0269(11) Uani 1 1 d . . . C248 C 0.4130(3) 0.1170(2) 0.1958(2) 0.0361(13) Uani 1 1 d . . . H24A H 0.3888 0.0947 0.2172 0.054 Uiso 1 1 calc R . . H24B H 0.4516 0.1173 0.2084 0.054 Uiso 1 1 calc R . . H24C H 0.432 0.0956 0.1626 0.054 Uiso 1 1 calc R . . C249 C 0.3021(3) 0.1834(3) 0.17541(19) 0.0364(13) Uani 1 1 d . . . H24D H 0.3209 0.1639 0.1416 0.055 Uiso 1 1 calc R . . H24E H 0.2671 0.2265 0.1762 0.055 Uiso 1 1 calc R . . H24F H 0.2797 0.1591 0.1958 0.055 Uiso 1 1 calc R . . C240 C 0.3296(3) 0.2162(2) 0.24825(17) 0.0313(12) Uani 1 1 d . . . H24G H 0.2924 0.2581 0.2488 0.047 Uiso 1 1 calc R . . H24H H 0.367 0.22 0.2605 0.047 Uiso 1 1 calc R . . H24I H 0.3098 0.1906 0.2691 0.047 Uiso 1 1 calc R . . C245 C 0.4551(2) 0.2270(2) 0.17930(15) 0.0186(9) Uani 1 1 d . . . H245 H 0.4688 0.2064 0.2067 0.022 Uiso 1 1 calc R . . C246 C 0.4908(2) 0.2618(2) 0.15486(15) 0.0193(10) Uani 1 1 d . . . C24 C 0.5504(2) 0.2672(2) 0.17170(16) 0.0187(9) Uani 1 1 d . . . H24J H 0.5586 0.2421 0.1999 0.022 Uiso 1 1 calc R . . H24K H 0.5943 0.25 0.1448 0.022 Uiso 1 1 calc R . . O251 O 0.53301(15) 0.30607(14) -0.01087(10) 0.0194(7) Uani 1 1 d . . . C251 C 0.5134(2) 0.2590(2) -0.01762(16) 0.0209(10) Uani 1 1 d U . . C252 C 0.5585(2) 0.2068(2) -0.05152(16) 0.0216(10) Uani 1 1 d U . . C253 C 0.5352(3) 0.1610(2) -0.05968(16) 0.0229(10) Uani 1 1 d U . . H253 H 0.5662 0.1258 -0.0825 0.027 Uiso 1 1 calc R . . C254 C 0.4689(3) 0.1644(2) -0.03606(16) 0.0243(10) Uani 1 1 d U . . C257 C 0.4442(3) 0.1142(3) -0.0479(2) 0.0359(12) Uani 1 1 d U . . C258 C 0.5058(4) 0.0491(3) -0.0579(3) 0.0576(18) Uani 1 1 d U . . H25A H 0.5249 0.0394 -0.0291 0.086 Uiso 1 1 calc R . . H25B H 0.5428 0.0488 -0.0862 0.086 Uiso 1 1 calc R . . H25C H 0.4892 0.0174 -0.0646 0.086 Uiso 1 1 calc R . . C259 C 0.4179(3) 0.1296(3) -0.0945(2) 0.0540(17) Uani 1 1 d U . . H25D H 0.402 0.098 -0.1027 0.081 Uiso 1 1 calc R . . H25E H 0.4564 0.1294 -0.1217 0.081 Uiso 1 1 calc R . . H25F H 0.3786 0.1712 -0.0889 0.081 Uiso 1 1 calc R . . C250 C 0.3850(3) 0.1118(3) -0.0075(2) 0.065(2) Uani 1 1 d U . . H25G H 0.4016 0.0995 0.022 0.097 Uiso 1 1 calc R . . H25H H 0.3694 0.0811 -0.0178 0.097 Uiso 1 1 calc R . . H25I H 0.3456 0.1534 -0.0005 0.097 Uiso 1 1 calc R . . C255 C 0.4256(2) 0.2159(2) -0.00173(16) 0.0228(10) Uani 1 1 d U . . H255 H 0.38 0.2194 0.0152 0.027 Uiso 1 1 calc R . . C256 C 0.4466(2) 0.2624(2) 0.00855(14) 0.0168(9) Uani 1 1 d U . . C25 C 0.4006(2) 0.3126(2) 0.05139(15) 0.0206(10) Uani 1 1 d . . . H25J H 0.4101 0.3506 0.0465 0.025 Uiso 1 1 calc R . . H25K H 0.3501 0.3244 0.0536 0.025 Uiso 1 1 calc R . . O261 O 0.67676(15) 0.29368(15) -0.04989(10) 0.0200(7) Uani 1 1 d U . . C261 C 0.6568(2) 0.2971(2) -0.09238(16) 0.0203(10) Uani 1 1 d U . . C262 C 0.6607(2) 0.3430(2) -0.12388(15) 0.0178(9) Uani 1 1 d U . . C263 C 0.6423(2) 0.3442(2) -0.16847(17) 0.0233(10) Uani 1 1 d U . . H263 H 0.6439 0.3765 -0.1889 0.028 Uiso 1 1 calc R . . C264 C 0.6217(3) 0.2998(2) -0.18370(16) 0.0257(11) Uani 1 1 d U . . C267 C 0.6032(3) 0.3017(3) -0.23371(18) 0.0334(12) Uani 1 1 d U . . C268 C 0.5433(3) 0.3640(3) -0.2353(2) 0.0546(18) Uani 1 1 d U . . H26A H 0.5315 0.3647 -0.2668 0.082 Uiso 1 1 calc R . . H26B H 0.5576 0.3982 -0.2316 0.082 Uiso 1 1 calc R . . H26C H 0.5019 0.3693 -0.2086 0.082 Uiso 1 1 calc R . . C269 C 0.6655(4) 0.2967(4) -0.2749(2) 0.077(3) Uani 1 1 d U . . H26D H 0.7028 0.2541 -0.2786 0.116 Uiso 1 1 calc R . . H26E H 0.6833 0.3272 -0.2673 0.116 Uiso 1 1 calc R . . H26F H 0.6509 0.3056 -0.3054 0.116 Uiso 1 1 calc R . . C260 C 0.5794(4) 0.2513(3) -0.2421(2) 0.075(2) Uani 1 1 d U . . H26G H 0.5748 0.2504 -0.2757 0.112 Uiso 1 1 calc R . . H26H H 0.5336 0.2601 -0.219 0.112 Uiso 1 1 calc R . . H26I H 0.6141 0.2104 -0.237 0.112 Uiso 1 1 calc R . . C265 C 0.6177(2) 0.2537(2) -0.15191(16) 0.0239(10) Uani 1 1 d U . . H265 H 0.6021 0.2237 -0.1608 0.029 Uiso 1 1 calc R . . C266 C 0.6363(2) 0.2512(2) -0.10704(15) 0.0209(10) Uani 1 1 d U . . C26 C 0.6321(2) 0.1996(2) -0.07544(16) 0.0239(11) Uani 1 1 d . . . H26J H 0.6577 0.159 -0.0959 0.029 Uiso 1 1 calc R . . H26K H 0.6566 0.1982 -0.0496 0.029 Uiso 1 1 calc R . . O271 O 0.78622(16) 0.31343(15) -0.05822(10) 0.0221(7) Uani 1 1 d U . . C271 C 0.8109(2) 0.3270(2) -0.10499(15) 0.0190(9) Uani 1 1 d U . . C272 C 0.8846(2) 0.2993(2) -0.12679(15) 0.0214(10) Uani 1 1 d U . . C273 C 0.9096(2) 0.3156(2) -0.17327(15) 0.0222(10) Uani 1 1 d U . . H273 H 0.959 0.2982 -0.1875 0.027 Uiso 1 1 calc R . . C274 C 0.8659(2) 0.3557(2) -0.19953(15) 0.0207(10) Uani 1 1 d U . . C277 C 0.8919(3) 0.3729(2) -0.25088(16) 0.0274(11) Uani 1 1 d U . . C278 C 0.8614(3) 0.4448(3) -0.25134(19) 0.0393(14) Uani 1 1 d U . . H27A H 0.881 0.4558 -0.2834 0.059 Uiso 1 1 calc R . . H27B H 0.8738 0.4631 -0.2259 0.059 Uiso 1 1 calc R . . H27C H 0.81 0.4615 -0.245 0.059 Uiso 1 1 calc R . . C279 C 0.9728(3) 0.3482(3) -0.26694(18) 0.0354(13) Uani 1 1 d U . . H27D H 0.9937 0.3022 -0.2697 0.053 Uiso 1 1 calc R . . H27E H 0.9892 0.3639 -0.2426 0.053 Uiso 1 1 calc R . . H27F H 0.9871 0.3628 -0.2988 0.053 Uiso 1 1 calc R . . C270 C 0.8681(3) 0.3455(3) -0.28759(18) 0.0412(15) Uani 1 1 d U . . H27G H 0.8872 0.2997 -0.2873 0.062 Uiso 1 1 calc R . . H27H H 0.8851 0.3563 -0.3204 0.062 Uiso 1 1 calc R . . H27I H 0.8164 0.3627 -0.2789 0.062 Uiso 1 1 calc R . . C275 C 0.7925(2) 0.3801(2) -0.17761(17) 0.0250(11) Uani 1 1 d U . . H275 H 0.7606 0.4067 -0.1949 0.03 Uiso 1 1 calc R . . C276 C 0.7660(2) 0.3658(2) -0.13086(15) 0.0200(10) Uani 1 1 d U . . C27 C 0.6857(2) 0.3919(2) -0.11033(16) 0.0213(10) Uani 1 1 d . . . H27J H 0.6732 0.4005 -0.0743 0.026 Uiso 1 1 calc R . . H27K H 0.6627 0.4317 -0.1244 0.026 Uiso 1 1 calc R . . O281 O 0.88248(15) 0.36079(15) -0.03478(10) 0.0219(7) Uani 1 1 d . . . C281 C 0.9535(2) 0.3253(2) -0.04825(16) 0.0213(10) Uani 1 1 d . . . C282 C 0.9991(2) 0.3407(2) -0.02834(16) 0.0240(10) Uani 1 1 d . . . C283 C 1.0713(2) 0.3061(2) -0.04514(17) 0.0269(11) Uani 1 1 d . . . H283 H 1.1017 0.3184 -0.0325 0.032 Uiso 1 1 calc R . . C284 C 1.1014(2) 0.2540(3) -0.07961(17) 0.0314(13) Uani 1 1 d . . . C287 C 1.1810(3) 0.2145(3) -0.09316(19) 0.0401(15) Uani 1 1 d . . . C288 C 1.2207(3) 0.2568(4) -0.1060(3) 0.083(3) Uani 1 1 d . . . H28A H 1.207 0.2877 -0.0781 0.125 Uiso 1 1 calc R . . H28B H 1.209 0.2787 -0.1346 0.125 Uiso 1 1 calc R . . H28C H 1.2716 0.2311 -0.1135 0.125 Uiso 1 1 calc R . . C289 C 1.2030(3) 0.1778(4) -0.0521(3) 0.092(3) Uani 1 1 d . . . H28D H 1.1734 0.1549 -0.0409 0.138 Uiso 1 1 calc R . . H28E H 1.1977 0.2064 -0.0249 0.138 Uiso 1 1 calc R . . H28F H 1.2524 0.1478 -0.0633 0.138 Uiso 1 1 calc R . . C280 C 1.2062(3) 0.1681(3) -0.1369(3) 0.070(2) Uani 1 1 d . . . H28G H 1.2578 0.1481 -0.1461 0.106 Uiso 1 1 calc R . . H28H H 1.1895 0.1898 -0.1643 0.106 Uiso 1 1 calc R . . H28I H 1.1877 0.136 -0.1289 0.106 Uiso 1 1 calc R . . C285 C 1.0554(2) 0.2385(2) -0.09799(17) 0.0276(12) Uani 1 1 d . . . H285 H 1.0743 0.2034 -0.1217 0.033 Uiso 1 1 calc R . . C286 C 0.9820(2) 0.2724(2) -0.08297(16) 0.0218(10) Uani 1 1 d . . . C28 C 0.9340(2) 0.2512(2) -0.10187(16) 0.0242(11) Uani 1 1 d . . . H28J H 0.9635 0.2135 -0.1253 0.029 Uiso 1 1 calc R . . H28K H 0.9057 0.2386 -0.074 0.029 Uiso 1 1 calc R . . N101 N 0.9984(2) 0.3505(2) 0.42820(17) 0.0443(13) Uani 1 1 d . . . H101 H 0.9585 0.3827 0.4227 0.053 Uiso 1 1 calc R . . C103 C 1.0062(4) 0.3690(4) 0.4768(2) 0.070(2) Uani 1 1 d . . . H10A H 0.9673 0.3685 0.5033 0.105 Uiso 1 1 calc R . . H10B H 1.0051 0.4114 0.4767 0.105 Uiso 1 1 calc R . . H10C H 1.0511 0.3392 0.482 0.105 Uiso 1 1 calc R . . C104 C 0.9859(3) 0.2928(3) 0.4296(2) 0.0513(18) Uani 1 1 d . . . H10D H 0.9792 0.2832 0.398 0.077 Uiso 1 1 calc R . . H10E H 0.9436 0.299 0.4557 0.077 Uiso 1 1 calc R . . H10F H 1.0266 0.2578 0.436 0.077 Uiso 1 1 calc R . . C101 C 1.0587(3) 0.3459(3) 0.3870(2) 0.0455(16) Uani 1 1 d . . . H10G H 1.0975 0.3036 0.3839 0.055 Uiso 1 1 calc R . . H10H H 1.0764 0.3772 0.3939 0.055 Uiso 1 1 calc R . . C102 C 1.0373(3) 0.3573(3) 0.3391(2) 0.0482(17) Uani 1 1 d . . . H10I H 1.078 0.3549 0.3123 0.058 Uiso 1 1 calc R . . H10J H 1.0222 0.3247 0.331 0.058 Uiso 1 1 calc R . . N102 N 0.9789(3) 0.4201(3) 0.3442(2) 0.0562(16) Uani 1 1 d . . . C105 C 1.0047(5) 0.4692(3) 0.3387(4) 0.105(3) Uani 1 1 d . . . H10K H 1.04 0.4609 0.3573 0.157 Uiso 1 1 calc R . . H10L H 0.9653 0.51 0.3512 0.157 Uiso 1 1 calc RD . . H10M H 1.0261 0.4699 0.304 0.157 Uiso 1 1 calc R . . C106 C 0.9399(4) 0.4251(4) 0.3080(3) 0.070(2) Uani 1 1 d . . . H10N H 0.9689 0.4258 0.2756 0.105 Uiso 1 1 calc R . . H10O H 0.8967 0.4639 0.316 0.105 Uiso 1 1 calc R . . H10P H 0.9277 0.3889 0.308 0.105 Uiso 1 1 calc R . . N201 N 0.44669(19) 0.42220(18) -0.02806(13) 0.0199(8) Uani 1 1 d . . . H201 H 0.4704 0.3821 -0.0194 0.024 Uiso 1 1 calc R . . C203 C 0.4984(2) 0.4386(2) -0.06532(17) 0.0261(11) Uani 1 1 d . . . H20A H 0.5168 0.4093 -0.0948 0.039 Uiso 1 1 calc R . . H20B H 0.5374 0.4357 -0.0518 0.039 Uiso 1 1 calc R . . H20C H 0.4747 0.4815 -0.0737 0.039 Uiso 1 1 calc R . . C204 C 0.4174(2) 0.4678(2) 0.01731(16) 0.0232(10) Uani 1 1 d . . . H20D H 0.3944 0.5107 0.0085 0.035 Uiso 1 1 calc R . . H20E H 0.4559 0.4649 0.0315 0.035 Uiso 1 1 calc R . . H20F H 0.3829 0.4575 0.0413 0.035 Uiso 1 1 calc R . . C201 C 0.3875(2) 0.4225(2) -0.04703(17) 0.0251(11) Uani 1 1 d . . . H20G H 0.3632 0.4646 -0.0575 0.03 Uiso 1 1 calc R . . H20H H 0.3532 0.4151 -0.0201 0.03 Uiso 1 1 calc R . . C202 C 0.4103(3) 0.3738(3) -0.08954(18) 0.0337(13) Uani 1 1 d . . . H20I H 0.4372 0.3849 -0.1191 0.04 Uiso 1 1 calc R . . H20J H 0.4407 0.332 -0.0816 0.04 Uiso 1 1 calc R . . N202 N 0.3453(3) 0.3727(3) -0.09836(18) 0.0713(17) Uani 1 1 d . . . C205 C 0.3571(5) 0.3453(5) -0.1455(3) 0.139(4) Uani 1 1 d . . . H20K H 0.3727 0.3699 -0.1701 0.209 Uiso 1 1 calc R . . H20L H 0.3132 0.3445 -0.1494 0.209 Uiso 1 1 calc R . . H20M H 0.3935 0.3022 -0.1497 0.209 Uiso 1 1 calc R . . C206 C 0.3149(4) 0.3387(4) -0.0638(3) 0.093(3) Uani 1 1 d . . . H20N H 0.2683 0.3457 -0.0677 0.139 Uiso 1 1 calc R . . H20O H 0.3103 0.3536 -0.0303 0.139 Uiso 1 1 calc R . . H20P H 0.3456 0.2937 -0.0699 0.139 Uiso 1 1 calc R . . N301 N 0.1450(3) 0.0220(2) 0.54381(18) 0.0484(14) Uani 1 1 d . . . H301 H 0.1319 0.0586 0.5281 0.058 Uiso 1 1 calc R . . C303 C 0.2202(3) -0.0010(4) 0.5422(3) 0.081(3) Uani 1 1 d . . . H30A H 0.2302 0.0339 0.5519 0.122 Uiso 1 1 calc R . . H30B H 0.2486 -0.0186 0.5088 0.122 Uiso 1 1 calc R . . H30C H 0.232 -0.0336 0.5648 0.122 Uiso 1 1 calc R . . C304 C 0.1276(5) -0.0232(4) 0.5213(3) 0.089(3) Uani 1 1 d . . . H30D H 0.128 -0.0149 0.4871 0.133 Uiso 1 1 calc RD . . H30E H 0.0807 -0.0193 0.5391 0.133 Uiso 1 1 calc R . . H30F H 0.1625 -0.0658 0.5223 0.133 Uiso 1 1 calc R . . C301 C 0.1053(4) 0.0367(4) 0.5962(3) 0.073(2) Uani 1 1 d . . . H30G H 0.1204 0.0648 0.6119 0.087 Uiso 1 1 calc R . . H30H H 0.1181 -0.0028 0.6124 0.087 Uiso 1 1 calc R . . C302 C 0.0243(4) 0.0683(4) 0.6052(3) 0.071(2) Uani 1 1 d . . . H30I H 0.0048 0.0991 0.6344 0.085 Uiso 1 1 calc R . . H30J H 0.013 0.0919 0.5769 0.085 Uiso 1 1 calc R . . N302 N -0.0105(4) 0.0275(3) 0.6126(3) 0.083(2) Uani 1 1 d . . . C305 C -0.0174(5) 0.0054(4) 0.6621(3) 0.114(4) Uani 1 1 d . . . H30K H 0.0296 -0.0202 0.6665 0.171 Uiso 1 1 calc R . . H30L H -0.045 -0.0198 0.6659 0.171 Uiso 1 1 calc R . . H30M H -0.0412 0.0417 0.6867 0.171 Uiso 1 1 calc R . . C306 C -0.0808(4) 0.0617(6) 0.6022(5) 0.165(6) Uani 1 1 d . . . H30N H -0.0981 0.1067 0.6117 0.248 Uiso 1 1 calc R . . H30O H -0.1142 0.0457 0.6209 0.248 Uiso 1 1 calc R . . H30P H -0.0762 0.0551 0.5671 0.248 Uiso 1 1 calc R . . N401 N 0.5482(2) 0.0844(2) 0.53044(17) 0.0461(14) Uani 1 1 d D . . H401 H 0.5284 0.125 0.5214 0.055 Uiso 1 1 calc R B 1 C403 C 0.4953(3) 0.0688(3) 0.5652(2) 0.065(2) Uani 1 1 d . C . H40A H 0.5188 0.0282 0.5774 0.097 Uiso 1 1 calc R . . H40B H 0.4611 0.0664 0.5487 0.097 Uiso 1 1 calc R . . H40C H 0.4708 0.1015 0.5928 0.097 Uiso 1 1 calc R . . C404 C 0.5868(4) 0.0385(3) 0.4875(3) 0.081(3) Uani 1 1 d . C . H40D H 0.6124 0.0561 0.4623 0.122 Uiso 1 1 calc R . . H40E H 0.5535 0.0286 0.4745 0.122 Uiso 1 1 calc R . . H40F H 0.6204 0 0.4969 0.122 Uiso 1 1 calc R . . C401 C 0.6075(5) 0.0743(5) 0.5468(4) 0.027(2) Uani 0.5 1 d P C 1 H40G H 0.6444 0.0793 0.5204 0.032 Uiso 0.5 1 calc PR C 1 H40H H 0.627 0.0315 0.5573 0.032 Uiso 0.5 1 calc PR C 1 C402 C 0.5827(5) 0.1254(5) 0.5917(4) 0.034(3) Uani 0.5 1 d P C 1 H40I H 0.5533 0.1675 0.5836 0.041 Uiso 0.5 1 calc PR C 1 H40J H 0.555 0.1146 0.6211 0.041 Uiso 0.5 1 calc PR C 1 N402 N 0.6488(5) 0.1239(4) 0.6001(3) 0.034(2) Uiso 0.5 1 d P C 1 C405 C 0.6338(9) 0.1497(7) 0.6498(6) 0.087(5) Uani 0.5 1 d P C 1 H40K H 0.6648 0.1706 0.6513 0.13 Uiso 0.5 1 calc PR C 1 H40L H 0.6418 0.1158 0.6715 0.13 Uiso 0.5 1 calc PR C 1 H40M H 0.5845 0.1803 0.6602 0.13 Uiso 0.5 1 calc PR C 1 C406 C 0.6778(8) 0.1570(7) 0.5687(5) 0.069(4) Uani 0.5 1 d P C 1 H40N H 0.6809 0.1447 0.5349 0.104 Uiso 0.5 1 calc PR C 1 H40O H 0.7252 0.148 0.5722 0.104 Uiso 0.5 1 calc PR C 1 H40P H 0.6482 0.2021 0.5766 0.104 Uiso 0.5 1 calc PR C 1 C407 C 0.5908(6) 0.1139(6) 0.5582(4) 0.040(3) Uani 0.5 1 d PD C 2 H40Q H 0.6221 0.1267 0.5328 0.048 Uiso 0.5 1 calc PR C 2 H40R H 0.5556 0.1522 0.5793 0.048 Uiso 0.5 1 calc PR C 2 C408 C 0.6344(6) 0.0705(5) 0.5891(4) 0.045(3) Uani 0.5 1 d PD C 2 H40S H 0.6032 0.0742 0.6221 0.055 Uiso 0.5 1 calc PR C 2 H40T H 0.6515 0.0268 0.5747 0.055 Uiso 0.5 1 calc PR C 2 N403 N 0.6962(5) 0.0808(5) 0.5950(4) 0.049(3) Uiso 0.5 1 d PD C 2 C409 C 0.6731(11) 0.1484(8) 0.6137(8) 0.126(9) Uiso 0.5 1 d PD C 2 H40U H 0.6851 0.1717 0.5865 0.189 Uiso 0.5 1 calc PR C 2 H40V H 0.697 0.15 0.6388 0.189 Uiso 0.5 1 calc PR C 2 H40W H 0.6219 0.1673 0.6279 0.189 Uiso 0.5 1 calc PR C 2 C400 C 0.7727(7) 0.0250(6) 0.5932(5) 0.063(4) Uiso 0.5 1 d PD C 2 H40X H 0.7788 -0.0125 0.5742 0.095 Uiso 0.5 1 calc PR C 2 H40Y H 0.7759 0.0151 0.6266 0.095 Uiso 0.5 1 calc PR C 2 H40Z H 0.8098 0.0387 0.5777 0.095 Uiso 0.5 1 calc PR C 2 N501 N 0.8538(2) 0.4756(2) 0.93192(17) 0.0384(12) Uani 1 1 d D . . H501 H 0.8695 0.4386 0.9469 0.046 Uiso 1 1 calc R D 1 C503 C 0.7789(5) 0.4927(6) 0.9301(5) 0.041(3) Uani 0.5 1 d PD E 1 H50A H 0.7575 0.5368 0.9235 0.061 Uiso 0.5 1 calc PR E 1 H50B H 0.752 0.4865 0.9616 0.061 Uiso 0.5 1 calc PR E 1 H50C H 0.7784 0.4658 0.904 0.061 Uiso 0.5 1 calc PR E 1 C504 C 0.8587(7) 0.5228(5) 0.9581(4) 0.044(3) Uani 0.5 1 d PD E 1 H50D H 0.8356 0.5632 0.9457 0.065 Uiso 0.5 1 calc PR E 1 H50E H 0.9085 0.5138 0.9543 0.065 Uiso 0.5 1 calc PR E 1 H50F H 0.8356 0.5245 0.9928 0.065 Uiso 0.5 1 calc PR E 1 C501 C 0.8981(5) 0.4645(5) 0.8780(4) 0.035(3) Uani 0.5 1 d PD E 1 H50G H 0.888 0.4347 0.8598 0.042 Uiso 0.5 1 calc PR E 1 H50H H 0.8833 0.5047 0.8629 0.042 Uiso 0.5 1 calc PR E 1 C502 C 0.9754(6) 0.4390(8) 0.8731(4) 0.026(3) Uani 0.5 1 d PD E 1 H50I H 0.9859 0.47 0.8895 0.031 Uiso 0.5 1 calc PR E 1 H50J H 0.9897 0.4001 0.89 0.031 Uiso 0.5 1 calc PR E 1 N502 N 1.0162(6) 0.4253(6) 0.8228(4) 0.070(4) Uani 0.5 1 d PD E 1 C505 C 1.0903(7) 0.3825(9) 0.8181(8) 0.073(7) Uani 0.5 1 d PD E 1 H50K H 1.1113 0.4017 0.8367 0.109 Uiso 0.5 1 calc PR E 1 H50L H 1.1164 0.3745 0.7835 0.109 Uiso 0.5 1 calc PR E 1 H50M H 1.0927 0.3427 0.8311 0.109 Uiso 0.5 1 calc PR E 1 C506 C 1.0169(8) 0.4838(7) 0.8014(6) 0.090(6) Uani 0.5 1 d PD E 1 H50O H 0.9766 0.5032 0.7872 0.136 Uiso 0.5 1 calc PR E 1 H50P H 1.0608 0.4735 0.7757 0.136 Uiso 0.5 1 calc PR E 1 H50Q H 1.0139 0.5133 0.8271 0.136 Uiso 0.5 1 calc PR E 1 N503 N 1.0359(5) 0.4434(5) 0.8641(4) 0.048(3) Uani 0.5 1 d PD E 2 C507 C 0.9128(6) 0.4900(5) 0.9133(4) 0.041(3) Uani 0.5 1 d PD E 2 H50R H 0.935 0.491 0.9399 0.049 Uiso 0.5 1 calc PR E 2 H50S H 0.8968 0.5322 0.9012 0.049 Uiso 0.5 1 calc PR E 2 C508 C 0.9658(9) 0.4428(10) 0.8726(8) 0.074(9) Uani 0.5 1 d PD E 2 H50T H 0.9691 0.4004 0.8805 0.089 Uiso 0.5 1 calc PR E 2 H50U H 0.9498 0.4518 0.8421 0.089 Uiso 0.5 1 calc PR E 2 C509 C 0.8116(7) 0.4734(6) 0.9029(5) 0.051(3) Uani 0.5 1 d PD E 2 H50V H 0.7868 0.4473 0.9168 0.076 Uiso 0.5 1 calc PR E 2 H50W H 0.8408 0.4553 0.8698 0.076 Uiso 0.5 1 calc PR E 2 H50X H 0.7771 0.516 0.9014 0.076 Uiso 0.5 1 calc PR E 2 C50A C 0.8040(6) 0.5258(6) 0.9762(5) 0.055(4) Uani 0.5 1 d PD E 2 H50Y H 0.774 0.5638 0.964 0.082 Uiso 0.5 1 calc PR E 2 H50Z H 0.8326 0.5362 0.994 0.082 Uiso 0.5 1 calc PR E 2 H500 H 0.7744 0.5086 0.9983 0.082 Uiso 0.5 1 calc PR E 2 C50B C 1.0383(8) 0.5034(6) 0.8474(5) 0.068(5) Uani 0.5 1 d PD E 2 H502 H 1.0468 0.502 0.8117 0.103 Uiso 0.5 1 calc PR E 2 H503 H 1.0765 0.5093 0.857 0.103 Uiso 0.5 1 calc PR E 2 H504 H 0.9933 0.5385 0.8626 0.103 Uiso 0.5 1 calc PR E 2 C50C C 1.0863(14) 0.3855(12) 0.8283(9) 0.108(11) Uani 0.5 1 d PD E 2 H505 H 1.1349 0.3749 0.8299 0.162 Uiso 0.5 1 calc PR E 2 H506 H 1.0823 0.3947 0.795 0.162 Uiso 0.5 1 calc PR E 2 H507 H 1.0741 0.35 0.8372 0.162 Uiso 0.5 1 calc PR E 2 N601 N 0.9793(3) 0.1545(3) 0.03972(19) 0.0651(18) Uani 1 1 d D . . H601 H 0.937 0.1793 0.0324 0.078 Uiso 1 1 calc R . . C603 C 1.0235(3) 0.1914(3) 0.0307(2) 0.0489(18) Uani 1 1 d D . . H60A H 1.0014 0.2288 0.0543 0.073 Uiso 1 1 calc R . . H60B H 1.0274 0.2043 -0.0026 0.073 Uiso 1 1 calc R . . H60C H 1.0706 0.1653 0.0346 0.073 Uiso 1 1 calc R . . C604 C 0.9614(4) 0.1439(4) 0.0922(2) 0.071(2) Uani 1 1 d D . . H60D H 1.0049 0.1229 0.1028 0.106 Uiso 1 1 calc R . . H60E H 0.9351 0.1174 0.0968 0.106 Uiso 1 1 calc R . . H60F H 0.9325 0.1844 0.1117 0.106 Uiso 1 1 calc R . . C601 C 1.0086(5) 0.0945(4) 0.0090(3) 0.103(3) Uani 1 1 d D . . H60G H 1.0558 0.0685 0.0137 0.123 Uiso 1 1 calc R . . H60H H 0.9782 0.072 0.0208 0.123 Uiso 1 1 calc R . . C602 C 1.0152(6) 0.0998(4) -0.0430(3) 0.139(5) Uani 1 1 d D . . H60I H 1.0442 0.1237 -0.054 0.167 Uiso 1 1 calc R . . H60J H 0.9676 0.1255 -0.0472 0.167 Uiso 1 1 calc R . . N602 N 1.0481(7) 0.0369(6) -0.0793(5) 0.245(7) Uiso 1 1 d D . . C605 C 1.1256(8) 0.0165(13) -0.0849(10) 0.28(1) Uiso 1 1 d D . . H60K H 1.1327 0.0352 -0.0569 0.420 Uiso 1 1 calc R . . H60L H 1.1462 0.0304 -0.1153 0.420 Uiso 1 1 calc R . . H60M H 1.1484 -0.0294 -0.0861 0.420 Uiso 1 1 calc R . . C606 C 1.0143(7) 0.0379(7) -0.1240(5) 0.208(7) Uiso 1 1 d D . . H60N H 1.003 0.0787 -0.1375 0.312 Uiso 1 1 calc R . . H60O H 0.9711 0.0311 -0.1125 0.312 Uiso 1 1 calc R . . H60P H 1.048 0.0045 -0.1495 0.312 Uiso 1 1 calc R . . N011 N 0.1976(3) 0.3950(3) 0.3187(2) 0.073(2) Uani 1 1 d . . . C011 C 0.2256(3) 0.3567(3) 0.3413(2) 0.0433(15) Uani 1 1 d . . . C012 C 0.2616(3) 0.3071(3) 0.3689(2) 0.0577(19) Uani 1 1 d . . . H01A H 0.2268 0.2984 0.3939 0.087 Uiso 1 1 calc R . . H01B H 0.2902 0.3203 0.3848 0.087 Uiso 1 1 calc R . . H01C H 0.2922 0.2691 0.3468 0.087 Uiso 1 1 calc R . . N021 N 0.3282(5) 0.4727(5) 0.4503(3) 0.180(6) Uani 1 1 d . . . C021 C 0.3805(4) 0.4313(4) 0.4431(2) 0.072(3) Uani 1 1 d . . . C022 C 0.4462(3) 0.3757(3) 0.4337(2) 0.0437(15) Uani 1 1 d . . . H02A H 0.4363 0.3387 0.4419 0.066 Uiso 1 1 calc R . . H02B H 0.4755 0.3801 0.4539 0.066 Uiso 1 1 calc R . . H02C H 0.4712 0.3705 0.399 0.066 Uiso 1 1 calc R . . N031 N 0.1706(4) 0.3926(3) 0.6615(3) 0.090(2) Uani 1 1 d . . . C031 C 0.1698(4) 0.3443(4) 0.6726(3) 0.063(2) Uani 1 1 d . . . C032 C 0.1675(3) 0.2850(3) 0.6863(3) 0.060(2) Uani 1 1 d . . . H03A H 0.1507 0.2871 0.722 0.089 Uiso 1 1 calc R . . H03B H 0.2149 0.2512 0.6754 0.089 Uiso 1 1 calc R . . H03C H 0.1354 0.2766 0.6708 0.089 Uiso 1 1 calc R . . N041 N 0.7793(4) 0.1101(3) 0.3794(3) 0.089(2) Uani 1 1 d . . . C041 C 0.7519(4) 0.1127(4) 0.3473(3) 0.066(2) Uani 1 1 d . . . C042 C 0.7203(3) 0.1155(3) 0.3077(2) 0.0525(18) Uani 1 1 d . . . H04A H 0.6836 0.1578 0.3088 0.079 Uiso 1 1 calc R . . H04B H 0.6993 0.0848 0.3107 0.079 Uiso 1 1 calc R . . H04C H 0.7564 0.1057 0.2765 0.079 Uiso 1 1 calc R . . N051 N 0.8338(4) 0.1232(4) 0.1908(3) 0.107(3) Uani 1 1 d . . . C051 C 0.7953(4) 0.1600(4) 0.1696(3) 0.073(3) Uani 1 1 d . . . C052 C 0.7490(4) 0.2052(4) 0.1451(3) 0.087(3) Uani 1 1 d . . . H05A H 0.7315 0.2471 0.1621 0.13 Uiso 1 1 calc R . . H05B H 0.7091 0.1946 0.1452 0.13 Uiso 1 1 calc R . . H05C H 0.7746 0.2049 0.1112 0.13 Uiso 1 1 calc R . . N061 N 0.6644(5) 0.0231(4) 0.0324(4) 0.146(4) Uani 1 1 d . . . C061 C 0.6171(4) 0.0700(4) 0.0467(3) 0.068(2) Uani 1 1 d . . . C062 C 0.5580(3) 0.1270(3) 0.0648(2) 0.0428(15) Uani 1 1 d . . . H06A H 0.5738 0.1597 0.0703 0.064 Uiso 1 1 calc R . . H06B H 0.5295 0.1213 0.0958 0.064 Uiso 1 1 calc R . . H06C H 0.5295 0.1395 0.041 0.064 Uiso 1 1 calc R . . N071 N 0.2142(4) 0.3920(3) 0.1479(3) 0.092(2) Uani 1 1 d . . . C071 C 0.2506(4) 0.3911(3) 0.1707(3) 0.0521(18) Uani 1 1 d . . . C072 C 0.2984(3) 0.3910(3) 0.1997(2) 0.0426(15) Uani 1 1 d . . . H07A H 0.3244 0.4157 0.1848 0.064 Uiso 1 1 calc R . . H07B H 0.3318 0.3477 0.2006 0.064 Uiso 1 1 calc R . . H07C H 0.2712 0.4095 0.2331 0.064 Uiso 1 1 calc R . . N081 N 0.1401(6) 0.0514(6) 0.0758(5) 0.206(6) Uani 1 1 d . . . C081 C 0.1960(7) 0.0570(6) 0.0713(4) 0.121(4) Uiso 1 1 d . . . C082 C 0.2562(5) 0.0704(6) 0.0694(4) 0.152(5) Uani 1 1 d . . . H08A H 0.2646 0.0925 0.0404 0.228 Uiso 1 1 calc R . . H08B H 0.2977 0.031 0.0675 0.228 Uiso 1 1 calc R . . H08C H 0.2474 0.0969 0.0989 0.228 Uiso 1 1 calc R . . N091 N 0.8418(6) 0.1452(5) 0.0283(4) 0.167(5) Uiso 1 1 d . . . C091 C 0.8289(7) 0.1178(6) 0.0029(5) 0.140(5) Uiso 1 1 d . . . C092 C 0.7812(9) 0.1013(8) -0.0231(6) 0.249(9) Uiso 1 1 d . . . H09A H 0.7335 0.116 -0.0016 0.374 Uiso 1 1 calc R . . H09B H 0.8006 0.0556 -0.0307 0.374 Uiso 1 1 calc R . . H09C H 0.7797 0.1218 -0.0536 0.374 Uiso 1 1 calc R . . N0A1 N 0.1840(5) 0.3564(7) 0.4958(4) 0.094(5) Uiso 0.5 1 d PD F 1 C0A1 C 0.1463(6) 0.3646(7) 0.5396(4) 0.078(5) Uiso 0.5 1 d PD F 1 C0A2 C 0.0680(7) 0.3928(9) 0.5737(5) 0.126(8) Uiso 0.5 1 d PD F 1 H0A1 H 0.0686 0.3813 0.6071 0.189 Uiso 0.5 1 calc PR F 1 H0A2 H 0.0396 0.3758 0.561 0.189 Uiso 0.5 1 calc PR F 1 H0A3 H 0.0475 0.4387 0.5739 0.189 Uiso 0.5 1 calc PR F 1 N0B1 N 1.1029(6) 0.4471(6) 0.4572(7) 0.179(9) Uiso 0.5 1 d PD G 2 C0B1 C 1.1267(6) 0.4841(5) 0.4349(4) 0.053(3) Uiso 0.5 1 d PD G 2 C0B2 C 1.1584(7) 0.5236(6) 0.4064(5) 0.061(4) Uiso 0.5 1 d PD G 2 H0B1 H 1.121 0.5632 0.4021 0.091 Uiso 0.5 1 calc PR G 2 H0B2 H 1.1872 0.5013 0.3742 0.091 Uiso 0.5 1 calc PR G 2 H0B3 H 1.1882 0.5324 0.424 0.091 Uiso 0.5 1 calc PR G 2 O01 O 0.6072(2) 0.04955(18) 0.36897(15) 0.0484(11) Uani 1 1 d . . . O02 O 0.41165(19) 0.45152(17) 0.13132(12) 0.0347(9) Uani 1 1 d . . . O03 O 0.1150(3) 0.4344(3) 0.9421(2) 0.107(2) Uani 1 1 d D . . O04 O 0.1993(5) 0.4858(3) 0.9022(4) 0.217(5) Uani 1 1 d D . . O05 O 0.1829(4) 0.7927(4) 0.1958(3) 0.154(3) Uiso 1 1 d . . . O0S O 0.8644(12) 0.3990(11) 0.4461(8) 0.284(9) Uiso 1 1 d U . . S0S S 0.8191(4) 0.4453(3) 0.4282(3) 0.251(6) Uani 1 1 d DU . . C01S C 0.7695(8) 0.5309(6) 0.4401(6) 0.247(9) Uiso 1 1 d DU . . H01D H 0.8025 0.5511 0.435 0.37 Uiso 1 1 calc R . . H01E H 0.7404 0.5414 0.4739 0.37 Uiso 1 1 calc R . . H01F H 0.7391 0.5459 0.4176 0.37 Uiso 1 1 calc R . . C02S C 0.7234(8) 0.4433(7) 0.4421(5) 0.212(7) Uiso 1 1 d U . . H02D H 0.7288 0.4004 0.4346 0.318 Uiso 1 1 calc R . . H02E H 0.6958 0.4717 0.4216 0.318 Uiso 1 1 calc R . . H02F H 0.6989 0.4569 0.4767 0.318 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 U11 0.01770(7) 0.02328(9) 0.01849(8) 0.00404(7) -0.00436(6) -0.01050(7) U12 0.01611(7) 0.02706(10) 0.01984(9) 0.00127(7) -0.00268(7) -0.00942(7) U21 0.01355(7) 0.02422(10) 0.02359(9) 0.00441(7) -0.00450(6) -0.00918(7) U22 0.01508(7) 0.02109(9) 0.01891(8) 0.00525(7) -0.00526(6) -0.00964(7) O10 0.0207(15) 0.0235(17) 0.0147(14) -0.0011(13) -0.0024(12) -0.0076(13) O101 0.0227(15) 0.0180(17) 0.0273(17) -0.0043(13) -0.0060(13) -0.0051(13) O102 0.0248(16) 0.0241(18) 0.0270(17) 0.0062(14) -0.0040(14) -0.0107(14) O103 0.0200(15) 0.035(2) 0.0321(18) -0.0001(15) -0.0036(14) -0.0137(15) O104 0.0188(15) 0.0266(19) 0.0297(18) 0.0013(15) -0.0024(14) -0.0067(14) O20 0.0182(13) 0.0268(17) 0.0109(14) -0.0001(12) -0.0019(11) -0.0121(13) O201 0.0173(15) 0.0237(18) 0.0349(19) 0.0038(15) -0.0032(14) -0.0054(14) O202 0.0145(14) 0.0311(19) 0.0284(17) 0.0027(14) -0.0055(13) -0.0083(14) O203 0.0186(15) 0.0185(17) 0.0287(17) 0.0053(13) -0.0070(13) -0.0043(13) O204 0.0209(15) 0.0206(17) 0.0259(17) 0.0033(13) -0.0047(13) -0.0091(13) O111 0.0224(14) 0.0239(17) 0.0178(15) 0.0047(13) -0.0026(12) -0.0136(13) C111 0.0193(19) 0.022(2) 0.016(2) 0.0037(18) -0.0024(16) -0.0094(18) C112 0.0179(19) 0.016(2) 0.017(2) 0.0010(17) -0.0023(16) -0.0038(17) C113 0.021(2) 0.019(2) 0.019(2) 0.0047(18) -0.0023(17) -0.0083(18) C114 0.021(2) 0.019(2) 0.018(2) 0.0023(18) -0.0014(17) -0.0085(18) C117 0.030(2) 0.037(3) 0.035(3) 0.016(2) -0.011(2) -0.024(2) C118 0.059(4) 0.068(4) 0.124(6) 0.065(4) -0.048(4) -0.045(3) C119 0.076(4) 0.083(5) 0.083(5) -0.004(4) 0.036(4) -0.056(4) C110 0.082(4) 0.098(5) 0.076(4) 0.055(4) -0.044(3) -0.076(4) C115 0.0173(19) 0.020(2) 0.023(2) -0.0007(18) -0.0036(17) -0.0085(17) C116 0.0125(17) 0.023(2) 0.0068(18) 0.0058(16) 0.0000(14) -0.0030(16) C11 0.0173(18) 0.050(3) 0.0099(19) -0.006(2) -0.0025(16) -0.018(2) O121 0.0164(14) 0.0244(17) 0.0118(14) -0.0038(12) 0.0008(11) -0.0054(13) C121 0.0202(19) 0.022(2) 0.0119(19) 0.0012(17) -0.0045(16) -0.0075(17) C122 0.0175(19) 0.018(2) 0.015(2) 0.0011(17) -0.0043(16) -0.0051(17) C123 0.021(2) 0.013(2) 0.030(2) 0.0014(19) -0.0062(19) -0.0037(18) C124 0.0155(19) 0.025(3) 0.020(2) 0.0013(19) -0.0019(17) -0.0031(18) C127 0.023(2) 0.020(3) 0.027(3) -0.002(2) 0.006(2) -0.002(2) C128 0.021(2) 0.041(3) 0.044(3) -0.012(3) -0.003(2) -0.001(2) C129 0.031(3) 0.038(3) 0.027(3) 0.001(2) -0.003(2) -0.009(2) C120 0.042(3) 0.033(3) 0.038(3) -0.011(3) 0.022(3) -0.012(3) C125 0.0186(19) 0.023(2) 0.016(2) 0.0028(17) -0.0037(16) -0.0099(17) C126 0.022(2) 0.020(2) 0.0116(19) 0.0020(17) -0.0070(16) -0.0067(17) C12 0.022(2) 0.017(2) 0.0133(19) -0.0006(16) -0.0015(16) -0.0088(17) O131 0.0188(14) 0.0241(17) 0.0180(15) -0.0038(13) -0.0019(12) -0.0080(13) C131 0.025(2) 0.031(3) 0.017(2) 0.0066(19) -0.0030(17) -0.0169(19) C132 0.022(2) 0.031(3) 0.017(2) 0.0067(19) -0.0054(17) -0.0167(19) C133 0.028(2) 0.038(3) 0.019(2) 0.005(2) -0.0053(18) -0.023(2) C134 0.039(3) 0.035(3) 0.024(2) 0.001(2) -0.001(2) -0.027(2) C137 0.059(3) 0.037(3) 0.032(3) -0.005(2) -0.011(3) -0.024(3) C138 0.078(4) 0.063(4) 0.072(5) -0.019(3) -0.013(4) -0.049(4) C139 0.101(5) 0.045(4) 0.032(3) -0.008(3) -0.023(3) -0.019(4) C130 0.074(4) 0.041(4) 0.045(3) -0.023(3) 0.001(3) -0.029(3) C135 0.033(2) 0.028(3) 0.020(2) 0.000(2) 0.002(2) -0.017(2) C136 0.028(2) 0.027(2) 0.017(2) 0.0010(19) 0.0002(18) -0.0187(19) C13 0.023(2) 0.016(2) 0.023(2) 0.0004(18) -0.0046(18) -0.0055(18) O141 0.0203(14) 0.041(2) 0.0184(15) 0.0002(14) -0.0041(12) -0.0184(14) C141 0.021(2) 0.035(3) 0.028(2) 0.002(2) -0.0049(19) -0.018(2) C142 0.024(2) 0.041(3) 0.032(3) 0.006(2) -0.001(2) -0.019(2) C143 0.020(2) 0.049(3) 0.039(3) 0.016(3) -0.005(2) -0.018(2) C144 0.023(2) 0.047(3) 0.038(3) 0.013(3) -0.009(2) -0.015(2) C147 0.043(3) 0.108(5) 0.087(4) 0.068(4) -0.039(3) -0.047(3) C148 0.092(5) 0.120(6) 0.180(7) 0.096(5) -0.105(5) -0.066(5) C149 0.096(5) 0.143(7) 0.131(6) 0.088(5) -0.083(4) -0.086(5) C140 0.081(5) 0.170(8) 0.109(6) 0.046(6) -0.068(4) -0.063(6) C145 0.024(2) 0.040(3) 0.024(2) 0.010(2) -0.0039(19) -0.014(2) C146 0.021(2) 0.033(3) 0.021(2) -0.004(2) -0.0017(18) -0.0152(19) C14 0.023(2) 0.037(3) 0.020(2) -0.004(2) 0.0001(18) -0.016(2) O151 0.0165(14) 0.040(2) 0.0186(15) 0.0080(14) -0.0060(12) -0.0103(14) C151 0.0150(19) 0.048(3) 0.023(2) 0.009(2) -0.0019(18) -0.012(2) C152 0.023(2) 0.055(3) 0.028(3) 0.015(2) -0.004(2) -0.013(2) C153 0.018(2) 0.055(4) 0.029(3) 0.002(3) 0.004(2) -0.002(2) C154 0.016(2) 0.079(4) 0.033(3) 0.006(3) -0.002(2) -0.008(3) C157 0.032(3) 0.097(5) 0.048(3) 0.001(3) -0.007(3) -0.019(3) C155 0.020(2) 0.072(4) 0.032(3) 0.019(3) -0.003(2) -0.019(2) C156 0.029(2) 0.063(4) 0.019(2) 0.015(2) -0.004(2) -0.018(3) C15 0.043(2) 0.047(3) 0.027(2) 0.025(2) -0.024(2) -0.038(2) O161 0.0196(15) 0.038(2) 0.0150(15) 0.0003(14) 0.0014(12) -0.0115(14) C161 0.024(2) 0.033(3) 0.013(2) -0.0051(19) -0.0011(17) -0.010(2) C162 0.020(2) 0.029(3) 0.020(2) -0.004(2) 0.0025(18) -0.0101(19) C163 0.025(2) 0.028(3) 0.018(2) 0.0039(19) -0.0005(18) -0.011(2) C164 0.022(2) 0.039(3) 0.024(2) 0.001(2) 0.0008(19) -0.017(2) C167 0.027(2) 0.043(3) 0.022(2) 0.010(2) -0.002(2) -0.015(2) C168 0.042(3) 0.052(4) 0.032(3) 0.011(3) 0.003(2) -0.023(3) C169 0.034(3) 0.050(4) 0.025(3) 0.003(2) 0.005(2) -0.020(3) C160 0.040(3) 0.057(4) 0.022(3) 0.005(3) -0.004(2) -0.020(3) C165 0.018(2) 0.047(3) 0.022(2) 0.001(2) 0.0061(19) -0.011(2) C166 0.025(2) 0.043(3) 0.018(2) 0.004(2) -0.0027(19) -0.011(2) C16 0.024(2) 0.039(3) 0.020(2) 0.004(2) 0.0021(19) -0.004(2) O171 0.0250(15) 0.038(2) 0.0128(14) 0.0010(13) -0.0025(12) -0.0169(14) C171 0.0125(18) 0.031(3) 0.021(2) 0.001(2) -0.0019(17) -0.0070(18) C172 0.0164(19) 0.025(2) 0.017(2) 0.0049(19) 0.0038(17) -0.0059(18) C173 0.027(2) 0.024(2) 0.019(2) -0.0004(19) -0.0002(18) -0.0109(19) C174 0.025(2) 0.023(3) 0.018(2) 0.0011(19) -0.0006(18) -0.0064(19) C177 0.057(3) 0.036(3) 0.026(3) 0.009(2) -0.018(2) -0.029(3) C178 0.144(7) 0.071(6) 0.041(4) -0.002(4) -0.031(5) -0.008(5) C179 0.096(5) 0.172(8) 0.060(4) 0.044(5) -0.049(4) -0.084(5) C170 0.189(9) 0.085(6) 0.051(4) 0.030(4) -0.071(5) -0.077(6) C175 0.018(2) 0.028(3) 0.016(2) 0.0031(19) -0.0004(17) -0.0059(19) C176 0.0127(18) 0.020(2) 0.016(2) -0.0010(17) 0.0022(16) -0.0023(16) C17 0.0158(19) 0.025(2) 0.022(2) -0.0025(19) -0.0015(17) -0.0053(18) O181 0.0209(14) 0.0228(17) 0.0164(15) 0.0048(12) -0.0041(12) -0.0110(13) C181 0.021(2) 0.030(3) 0.013(2) 0.0091(18) -0.0071(16) -0.0112(18) C182 0.0181(19) 0.035(3) 0.0117(19) 0.0105(18) -0.0042(16) -0.0124(19) C183 0.019(2) 0.032(3) 0.020(2) 0.004(2) -0.0077(17) -0.0116(19) C184 0.026(2) 0.029(3) 0.024(2) 0.006(2) -0.0073(19) -0.015(2) C187 0.037(3) 0.033(3) 0.047(3) -0.002(3) -0.007(3) -0.020(2) C188 0.084(5) 0.076(5) 0.088(5) -0.002(4) -0.058(4) -0.040(4) C189 0.099(5) 0.102(5) 0.066(5) -0.018(4) 0.021(4) -0.090(4) C180 0.039(3) 0.034(3) 0.103(6) -0.024(4) -0.005(4) -0.017(3) C185 0.026(2) 0.028(3) 0.022(2) 0.006(2) -0.0039(19) -0.008(2) C186 0.023(2) 0.032(3) 0.014(2) 0.0064(18) -0.0042(17) -0.0142(19) C18 0.023(2) 0.026(3) 0.019(2) 0.0048(19) -0.0049(18) -0.0106(19) O211 0.0188(14) 0.0321(18) 0.0218(16) 0.0110(14) -0.0095(12) -0.0132(13) C211 0.0182(19) 0.019(2) 0.021(2) 0.0035(18) -0.0069(17) -0.0062(17) C212 0.0186(19) 0.030(3) 0.019(2) 0.0036(19) -0.0072(17) -0.0087(19) C213 0.023(2) 0.038(3) 0.021(2) 0.004(2) -0.0064(18) -0.013(2) C214 0.019(2) 0.047(3) 0.025(2) -0.002(2) -0.0060(18) -0.014(2) C217 0.023(2) 0.063(4) 0.038(3) 0.014(3) -0.015(2) -0.015(2) C218 0.044(4) 0.085(5) 0.116(6) 0.041(4) -0.042(4) -0.022(4) C219 0.040(3) 0.122(6) 0.048(4) -0.012(4) -0.024(3) -0.015(4) C210 0.023(3) 0.104(5) 0.047(3) 0.016(4) -0.011(3) -0.025(3) C215 0.0156(19) 0.038(3) 0.024(2) 0.002(2) -0.0034(17) -0.0106(19) C216 0.0180(19) 0.017(2) 0.025(2) 0.0003(18) -0.0053(17) -0.0065(17) C21 0.039(2) 0.026(2) 0.017(2) -0.0041(18) 0.0100(19) -0.028(2) O221 0.0217(14) 0.0276(17) 0.0178(15) 0.0005(13) -0.0032(12) -0.0159(13) C221 0.025(2) 0.028(2) 0.013(2) 0.0000(18) -0.0006(17) -0.0156(19) C222 0.022(2) 0.027(2) 0.018(2) 0.0092(18) -0.0054(17) -0.0157(18) C223 0.028(2) 0.022(2) 0.019(2) 0.0039(18) -0.0037(18) -0.0158(19) C224 0.029(2) 0.039(3) 0.021(2) 0.005(2) -0.0052(18) -0.026(2) C227 0.040(3) 0.036(3) 0.027(3) -0.003(2) -0.009(2) -0.025(2) C228 0.088(5) 0.059(4) 0.032(3) -0.002(3) -0.026(3) -0.035(4) C229 0.069(4) 0.042(4) 0.037(3) -0.010(3) -0.011(3) -0.028(3) C220 0.080(4) 0.065(4) 0.046(4) 0.006(3) -0.019(3) -0.058(3) C225 0.029(2) 0.039(3) 0.014(2) 0.0069(19) -0.0086(17) -0.025(2) C226 0.0199(19) 0.033(3) 0.016(2) 0.0080(19) -0.0044(16) -0.0167(19) C22 0.021(2) 0.030(3) 0.021(2) 0.0065(19) -0.0066(18) -0.0117(19) O231 0.0187(14) 0.0209(16) 0.0150(14) -0.0001(12) -0.0025(12) -0.0082(12) C231 0.0168(18) 0.023(2) 0.015(2) 0.0020(17) -0.0048(16) -0.0096(17) C232 0.027(2) 0.024(2) 0.0105(19) 0.0061(17) -0.0081(16) -0.0161(18) C233 0.0176(19) 0.029(3) 0.016(2) 0.0048(18) -0.0050(16) -0.0116(18) C234 0.021(2) 0.022(2) 0.016(2) 0.0020(18) -0.0049(17) -0.0068(18) C237 0.024(2) 0.030(3) 0.020(2) 0.001(2) -0.0002(18) -0.011(2) C238 0.029(3) 0.029(3) 0.034(3) 0.002(2) -0.001(2) 0.000(2) C239 0.035(3) 0.039(3) 0.025(3) -0.001(2) 0.010(2) -0.017(2) C230 0.044(3) 0.047(3) 0.024(3) -0.005(2) -0.002(2) -0.023(3) C235 0.0190(19) 0.022(2) 0.016(2) 0.0003(17) -0.0021(16) -0.0089(18) C236 0.0178(18) 0.020(2) 0.016(2) 0.0037(17) -0.0056(16) -0.0096(17) C23 0.0211(19) 0.024(2) 0.017(2) 0.0025(18) -0.0026(17) -0.0133(18) O241 0.0185(13) 0.0233(16) 0.0144(14) 0.0070(12) -0.0034(11) -0.0121(12) C241 0.0153(18) 0.011(2) 0.0127(19) -0.0010(15) -0.0011(15) -0.0015(15) C242 0.0114(17) 0.019(2) 0.017(2) 0.0052(17) -0.0005(15) -0.0042(16) C243 0.0149(18) 0.027(2) 0.022(2) 0.0054(19) -0.0066(17) -0.0099(17) C244 0.0163(18) 0.025(2) 0.024(2) 0.0037(19) -0.0034(17) -0.0125(17) C247 0.025(2) 0.036(3) 0.027(2) 0.018(2) -0.0107(19) -0.018(2) C248 0.038(3) 0.032(3) 0.045(3) 0.024(2) -0.015(2) -0.020(2) C249 0.031(2) 0.055(3) 0.042(3) 0.021(3) -0.017(2) -0.033(2) C240 0.031(2) 0.042(3) 0.024(2) 0.012(2) -0.004(2) -0.021(2) C245 0.0211(19) 0.022(2) 0.016(2) 0.0075(17) -0.0075(16) -0.0111(18) C246 0.0197(19) 0.021(2) 0.018(2) 0.0002(18) -0.0019(17) -0.0099(17) C24 0.0186(19) 0.016(2) 0.022(2) 0.0047(17) -0.0067(17) -0.0067(17) O251 0.0165(14) 0.0223(17) 0.0189(15) 0.0047(13) -0.0036(12) -0.0082(12) C251 0.027(2) 0.023(2) 0.016(2) 0.0065(18) -0.0045(17) -0.0147(18) C252 0.023(2) 0.025(2) 0.017(2) 0.0107(18) -0.0056(17) -0.0102(18) C253 0.035(2) 0.018(2) 0.018(2) 0.0012(18) -0.0084(18) -0.0126(19) C254 0.032(2) 0.027(2) 0.021(2) 0.0054(19) -0.0086(19) -0.0179(19) C257 0.040(3) 0.039(3) 0.040(3) -0.001(2) -0.010(2) -0.027(2) C258 0.069(4) 0.044(4) 0.077(5) 0.009(3) -0.027(4) -0.037(3) C259 0.058(3) 0.059(4) 0.068(4) 0.001(3) -0.032(3) -0.038(3) C250 0.070(4) 0.067(4) 0.066(4) -0.018(3) 0.013(4) -0.052(3) C255 0.024(2) 0.024(2) 0.022(2) 0.0075(19) -0.0063(18) -0.0112(18) C256 0.024(2) 0.020(2) 0.0095(18) 0.0060(16) -0.0096(16) -0.0097(17) C25 0.024(2) 0.027(2) 0.014(2) 0.0043(18) -0.0050(17) -0.0141(19) O261 0.0215(14) 0.0299(18) 0.0132(14) -0.0008(13) -0.0055(12) -0.0144(13) C261 0.0183(19) 0.022(2) 0.017(2) -0.0018(17) 0.0004(16) -0.0075(17) C262 0.0147(18) 0.019(2) 0.015(2) -0.0027(17) 0.0019(16) -0.0052(16) C263 0.019(2) 0.021(2) 0.025(2) 0.0023(19) -0.0006(18) -0.0068(18) C264 0.027(2) 0.027(3) 0.016(2) 0.0006(19) -0.0021(18) -0.007(2) C267 0.050(3) 0.038(3) 0.026(2) 0.012(2) -0.021(2) -0.027(2) C268 0.068(4) 0.054(4) 0.046(3) 0.017(3) -0.037(3) -0.018(3) C269 0.066(4) 0.132(7) 0.018(3) -0.014(4) -0.005(3) -0.026(5) C260 0.154(6) 0.056(4) 0.058(4) 0.022(3) -0.074(4) -0.061(4) C265 0.023(2) 0.024(2) 0.025(2) -0.0029(19) -0.0036(18) -0.0111(19) C266 0.0181(19) 0.025(2) 0.015(2) 0.0049(18) 0.0010(16) -0.0069(18) C26 0.029(2) 0.022(2) 0.020(2) 0.0011(19) -0.0020(19) -0.0112(19) O271 0.0203(15) 0.0365(19) 0.0092(14) 0.0037(13) -0.0013(12) -0.0129(14) C271 0.0167(18) 0.023(2) 0.016(2) -0.0019(17) -0.0018(16) -0.0072(17) C272 0.0163(19) 0.029(3) 0.016(2) 0.0018(18) -0.0020(16) -0.0073(18) C273 0.0180(19) 0.029(2) 0.018(2) -0.0011(18) 0.0027(16) -0.0118(18) C274 0.0201(19) 0.025(2) 0.0138(19) -0.0016(17) 0.0010(16) -0.0086(18) C277 0.025(2) 0.037(3) 0.017(2) 0.010(2) -0.0019(18) -0.012(2) C278 0.037(3) 0.047(3) 0.033(3) 0.016(2) -0.004(2) -0.020(3) C279 0.032(2) 0.048(3) 0.027(3) 0.009(2) 0.002(2) -0.021(2) C270 0.041(3) 0.057(4) 0.023(3) 0.006(3) -0.005(2) -0.020(3) C275 0.022(2) 0.027(2) 0.028(2) 0.006(2) -0.0059(18) -0.0117(19) C276 0.0181(18) 0.025(2) 0.017(2) -0.0004(18) 0.0014(16) -0.0120(17) C27 0.0143(18) 0.025(2) 0.022(2) 0.0024(19) -0.0037(17) -0.0055(18) O281 0.0137(13) 0.0324(19) 0.0182(15) 0.0047(13) -0.0022(12) -0.0093(13) C281 0.0154(18) 0.024(2) 0.023(2) 0.0104(19) -0.0029(17) -0.0079(17) C282 0.020(2) 0.039(3) 0.018(2) 0.008(2) -0.0044(17) -0.018(2) C283 0.0155(19) 0.040(3) 0.025(2) 0.005(2) -0.0051(18) -0.011(2) C284 0.018(2) 0.052(3) 0.017(2) 0.007(2) -0.0003(18) -0.010(2) C287 0.019(2) 0.060(4) 0.033(3) -0.002(3) -0.004(2) -0.009(3) C288 0.019(3) 0.088(6) 0.121(7) -0.035(5) 0.022(4) -0.021(3) C289 0.026(3) 0.128(8) 0.075(5) 0.034(5) -0.008(4) 0.013(4) C280 0.023(3) 0.076(5) 0.083(5) -0.039(4) 0.002(3) 0.001(3) C285 0.021(2) 0.036(3) 0.020(2) 0.004(2) -0.0029(18) -0.008(2) C286 0.0154(19) 0.025(2) 0.020(2) 0.0077(19) -0.0029(17) -0.0054(18) C28 0.022(2) 0.025(3) 0.019(2) 0.0045(19) -0.0003(18) -0.0056(19) N101 0.033(3) 0.041(3) 0.046(3) -0.001(2) -0.012(2) 0.000(2) C103 0.056(4) 0.094(6) 0.040(4) -0.012(4) -0.013(3) -0.011(4) C104 0.044(4) 0.050(4) 0.053(4) 0.003(3) -0.008(3) -0.015(3) C101 0.033(3) 0.043(4) 0.050(4) 0.003(3) -0.007(3) -0.006(3) C102 0.041(3) 0.045(4) 0.048(4) 0.004(3) -0.008(3) -0.010(3) N102 0.044(3) 0.049(3) 0.065(4) -0.002(3) -0.019(3) -0.004(3) C105 0.097(6) 0.030(4) 0.205(10) 0.022(5) -0.084(7) -0.019(4) C106 0.071(5) 0.078(6) 0.061(5) 0.003(4) -0.028(4) -0.026(4) N201 0.0204(17) 0.0185(19) 0.0194(18) 0.0025(15) -0.0043(15) -0.0070(15) C203 0.020(2) 0.035(3) 0.024(2) 0.005(2) -0.0043(18) -0.013(2) C204 0.025(2) 0.024(3) 0.021(2) -0.0005(19) -0.0057(18) -0.0100(19) C201 0.023(2) 0.034(3) 0.023(2) 0.004(2) -0.0084(18) -0.015(2) C202 0.053(3) 0.033(3) 0.024(3) 0.000(2) -0.013(2) -0.025(3) N202 0.113(4) 0.117(4) 0.031(3) -0.004(3) -0.007(3) -0.101(4) C205 0.177(7) 0.233(11) 0.116(8) 0.036(7) -0.069(7) -0.175(7) C206 0.100(6) 0.105(7) 0.121(7) 0.023(5) -0.069(5) -0.067(5) N301 0.054(3) 0.041(3) 0.044(3) 0.003(2) -0.015(3) -0.013(3) C303 0.043(4) 0.095(6) 0.111(6) 0.064(5) -0.023(4) -0.034(4) C304 0.135(8) 0.082(6) 0.080(6) 0.022(5) -0.048(5) -0.065(6) C301 0.048(4) 0.076(6) 0.073(5) -0.009(4) 0.001(4) -0.014(4) C302 0.069(5) 0.076(5) 0.079(5) 0.031(4) -0.020(4) -0.041(4) N302 0.074(4) 0.080(5) 0.107(6) 0.014(4) -0.017(4) -0.046(4) C305 0.154(10) 0.111(8) 0.080(6) 0.034(6) -0.004(6) -0.073(7) C306 0.041(5) 0.195(13) 0.253(15) -0.054(11) -0.035(7) -0.041(7) N401 0.024(2) 0.055(3) 0.048(3) 0.031(2) -0.009(2) -0.006(2) C403 0.029(3) 0.083(5) 0.061(4) 0.044(4) -0.004(3) -0.007(3) C404 0.059(5) 0.051(4) 0.069(5) 0.028(4) 0.023(4) 0.019(4) C401 0.027(5) 0.018(5) 0.027(5) 0.004(4) -0.003(4) -0.002(4) C402 0.029(5) 0.041(7) 0.025(5) 0.000(5) -0.010(4) -0.006(5) C405 0.146(13) 0.054(9) 0.106(12) 0.015(8) -0.093(11) -0.053(10) C406 0.082(9) 0.093(11) 0.074(9) 0.048(8) -0.048(8) -0.062(8) C407 0.036(6) 0.051(8) 0.035(7) 0.006(6) -0.020(5) -0.014(6) C408 0.057(7) 0.052(8) 0.033(6) 0.002(6) -0.009(6) -0.030(6) N501 0.038(3) 0.026(2) 0.049(3) 0.008(2) -0.008(2) -0.012(2) C503 0.028(6) 0.025(6) 0.050(7) 0.014(5) -0.005(5) 0.006(5) C504 0.060(8) 0.032(7) 0.029(6) 0.002(5) -0.010(6) -0.010(6) C501 0.033(5) 0.038(6) 0.032(6) 0.006(5) -0.002(5) -0.018(5) C502 0.028(5) 0.046(9) 0.009(5) 0.005(5) -0.004(4) -0.022(5) N502 0.060(8) 0.082(9) 0.071(8) 0.049(7) -0.019(6) -0.033(7) C505 0.024(6) 0.088(12) 0.108(15) 0.049(10) -0.012(8) -0.029(7) C506 0.061(9) 0.105(12) 0.095(12) 0.068(10) 0.001(9) -0.039(9) N503 0.053(6) 0.056(7) 0.039(6) 0.004(5) -0.005(5) -0.031(5) C507 0.057(7) 0.044(7) 0.030(6) 0.006(5) -0.014(5) -0.027(6) C508 0.100(18) 0.044(12) 0.072(15) 0.004(11) 0.008(13) -0.039(12) C509 0.054(7) 0.040(7) 0.081(10) 0.033(7) -0.043(7) -0.029(6) C50A 0.032(6) 0.037(7) 0.083(10) -0.006(7) -0.001(7) -0.009(6) C50B 0.080(10) 0.055(9) 0.059(9) -0.017(7) 0.030(8) -0.043(8) C50C 0.11(2) 0.12(2) 0.039(10) -0.015(13) 0.016(11) -0.016(17) N601 0.062(4) 0.064(4) 0.050(3) 0.015(3) -0.001(3) -0.015(3) C603 0.037(3) 0.047(4) 0.046(4) 0.014(3) -0.001(3) -0.006(3) C604 0.054(4) 0.095(6) 0.053(4) 0.013(4) -0.004(4) -0.026(4) C601 0.134(8) 0.110(7) 0.058(5) -0.025(5) 0.031(5) -0.073(6) C602 0.214(13) 0.083(7) 0.074(7) -0.013(5) 0.023(7) -0.048(8) N011 0.056(4) 0.075(4) 0.074(4) 0.036(3) -0.009(3) -0.019(3) C011 0.038(3) 0.047(4) 0.042(3) 0.008(3) -0.002(3) -0.020(3) C012 0.057(4) 0.060(5) 0.057(4) 0.014(3) -0.029(3) -0.017(4) N021 0.133(8) 0.162(9) 0.079(6) 0.009(6) 0.030(6) 0.074(7) C021 0.069(5) 0.068(5) 0.037(4) 0.004(4) -0.001(4) 0.006(4) C022 0.044(3) 0.041(4) 0.049(4) 0.010(3) -0.020(3) -0.017(3) N031 0.114(6) 0.061(4) 0.112(6) 0.012(4) -0.053(5) -0.040(4) C031 0.049(4) 0.057(5) 0.067(5) -0.016(4) -0.027(4) 0.003(4) C032 0.046(4) 0.036(4) 0.083(5) -0.007(4) -0.003(4) -0.011(3) N041 0.054(4) 0.091(5) 0.118(6) 0.039(5) -0.016(4) -0.030(4) C041 0.044(4) 0.057(5) 0.082(6) 0.020(4) 0.005(4) -0.017(4) C042 0.048(4) 0.032(4) 0.061(4) -0.001(3) -0.003(3) -0.006(3) N051 0.085(6) 0.090(6) 0.116(6) 0.012(5) -0.018(5) -0.009(5) C051 0.050(4) 0.068(5) 0.081(6) 0.018(4) 0.005(4) -0.018(4) C052 0.065(5) 0.074(6) 0.132(7) 0.053(5) -0.051(5) -0.025(4) N061 0.112(8) 0.086(6) 0.161(9) -0.034(6) 0.006(7) 0.015(6) C061 0.070(5) 0.062(5) 0.050(4) -0.016(4) 0.002(4) -0.016(4) C062 0.051(4) 0.037(3) 0.036(3) 0.007(3) -0.010(3) -0.015(3) N071 0.106(5) 0.062(5) 0.134(6) 0.035(4) -0.083(5) -0.030(4) C071 0.051(4) 0.035(4) 0.069(4) 0.019(3) -0.025(3) -0.013(3) C072 0.042(3) 0.039(3) 0.036(3) 0.006(3) -0.003(3) -0.010(3) N081 0.149(9) 0.259(14) 0.256(15) 0.059(11) -0.047(10) -0.134(10) C082 0.091(8) 0.252(15) 0.109(9) -0.036(9) -0.011(7) -0.075(9) O01 0.044(2) 0.035(2) 0.059(3) 0.009(2) -0.019(2) -0.0054(19) O02 0.038(2) 0.032(2) 0.0298(19) 0.0070(16) -0.0151(16) -0.0071(17) O03 0.109(5) 0.129(5) 0.091(4) -0.032(4) -0.024(4) -0.056(4) O04 0.156(8) 0.068(5) 0.336(13) 0.000(6) 0.084(8) -0.038(5) S0S 0.131(7) 0.191(5) 0.290(9) 0.079(6) 0.077(7) -0.003(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 U11 O101 1.795(3) . ? U11 O102 1.806(3) . ? U11 O111 2.244(3) . ? U11 O181 2.311(3) . ? U11 O10 2.344(3) . ? U11 O121 2.434(3) . ? U11 O171 2.596(3) . ? U12 O104 1.794(3) . ? U12 O103 1.795(3) . ? U12 O141 2.238(3) . ? U12 O151 2.310(3) . ? U12 O10 2.347(3) . ? U12 O161 2.487(3) . ? U12 O131 2.590(3) . ? U21 O202 1.784(3) . ? U21 O201 1.793(3) . ? U21 O211 2.208(3) . ? U21 O281 2.304(3) . ? U21 O20 2.339(3) . ? U21 O221 2.494(3) . ? U21 O271 2.613(3) . ? U22 O203 1.792(3) . ? U22 O204 1.794(3) . ? U22 O241 2.257(3) . ? U22 O251 2.320(3) . ? U22 O20 2.353(3) . ? U22 O261 2.473(3) . ? U22 O231 2.532(3) . ? O10 H10 0.95 . ? O20 H20 0.95 . ? O111 C111 1.356(5) . ? C111 C112 1.414(6) . ? C111 C116 1.427(6) . ? C112 C113 1.377(6) . ? C112 C12 1.516(6) . ? C113 C114 1.399(6) . ? C113 H113 0.95 . ? C114 C115 1.397(6) . ? C114 C117 1.541(6) . ? C117 C110 1.486(8) . ? C117 C118 1.515(8) . ? C117 C119 1.520(8) . ? C118 H11A 0.98 . ? C118 H11B 0.98 . ? C118 H11C 0.98 . ? C119 H11D 0.98 . ? C119 H11E 0.98 . ? C119 H11F 0.98 . ? C110 H11G 0.98 . ? C110 H11H 0.98 . ? C110 H11I 0.98 . ? C115 C116 1.380(6) . ? C115 H115 0.95 . ? C116 C11 1.501(6) . ? C11 C182 1.498(6) . ? C11 H11J 0.99 . ? C11 H11K 0.99 . ? O121 C121 1.351(5) . ? C121 C122 1.404(6) . ? C121 C126 1.410(6) . ? C122 C123 1.407(6) . ? C122 C13 1.490(6) . ? C123 C124 1.382(6) . ? C123 H123 0.95 . ? C124 C125 1.390(6) . ? C124 C127 1.551(6) . ? C127 C129 1.524(7) . ? C127 C120 1.528(7) . ? C127 C128 1.540(7) . ? C128 H12A 0.98 . ? C128 H12B 0.98 . ? C128 H12C 0.98 . ? C129 H12D 0.98 . ? C129 H12E 0.98 . ? C129 H12F 0.98 . ? C120 H12G 0.98 . ? C120 H12H 0.98 . ? C120 H12I 0.98 . ? C125 C126 1.390(6) . ? C125 H125 0.95 . ? C126 C12 1.508(6) . ? C12 H12J 0.99 . ? C12 H12K 0.99 . ? O131 C131 1.399(6) . ? C131 C136 1.388(6) . ? C131 C132 1.408(6) . ? C132 C133 1.388(7) . ? C132 C14 1.503(6) . ? C133 C134 1.361(7) . ? C133 H133 0.95 . ? C134 C135 1.404(7) . ? C134 C137 1.550(7) . ? C137 C130 1.520(8) . ? C137 C138 1.543(9) . ? C137 C139 1.572(8) . ? C138 H13A 0.98 . ? C138 H13B 0.98 . ? C138 H13C 0.98 . ? C139 H13D 0.98 . ? C139 H13E 0.98 . ? C139 H13F 0.98 . ? C130 H13G 0.98 . ? C130 H13H 0.98 . ? C130 H13I 0.98 . ? C135 C136 1.398(7) . ? C135 H135 0.95 . ? C136 C13 1.509(7) . ? C13 H13J 0.99 . ? C13 H13K 0.99 . ? O141 C141 1.334(6) . ? C141 C142 1.406(6) . ? C141 C146 1.407(7) . ? C142 C143 1.398(7) . ? C142 C15 1.527(7) . ? C143 C144 1.394(7) . ? C143 H143 0.95 . ? C144 C145 1.405(7) . ? C144 C147 1.523(8) . ? C147 C149 1.413(9) . ? C147 C148 1.509(10) . ? C147 C140 1.570(11) . ? C148 H14A 0.98 . ? C148 H14B 0.98 . ? C148 H14C 0.98 . ? C149 H14D 0.98 . ? C149 H14E 0.98 . ? C149 H14F 0.98 . ? C140 H14G 0.98 . ? C140 H14H 0.98 . ? C140 H14I 0.98 . ? C145 C146 1.398(7) . ? C145 H145 0.95 . ? C146 C14 1.499(6) . ? C14 H14J 0.99 . ? C14 H14K 0.99 . ? O151 C151 1.366(5) . ? C151 C156 1.401(8) . ? C151 C152 1.404(7) . ? C152 C153 1.400(7) . ? C152 C16 1.522(8) . ? C153 C154 1.394(8) . ? C153 H153 0.95 . ? C154 C155 1.383(8) . ? C154 C157 1.543(8) . ? C157 C15A 1.414(19) . ? C157 C15B 1.436(18) . ? C157 C158 1.521(15) . ? C157 C150 1.532(15) . ? C157 C159 1.573(15) . ? C157 C15C 1.59(2) . ? C158 H15A 0.98 . ? C158 H15B 0.98 . ? C158 H15C 0.98 . ? C159 H15D 0.98 . ? C159 H15E 0.98 . ? C159 H15F 0.98 . ? C150 H15G 0.98 . ? C150 H15H 0.98 . ? C150 H15I 0.98 . ? C15A H15J 0.98 . ? C15A H15K 0.98 . ? C15A H15L 0.98 . ? C15B H15M 0.98 . ? C15B H15N 0.98 . ? C15B H15O 0.98 . ? C15C H15P 0.98 . ? C15C H15Q 0.98 . ? C15C H15R 0.98 . ? C155 C156 1.407(7) . ? C155 H155 0.95 . ? C156 C15 1.454(7) . ? C15 H15S 0.99 . ? C15 H15T 0.99 . ? O161 C161 1.360(5) . ? C161 C162 1.407(7) . ? C161 C166 1.407(6) . ? C162 C163 1.401(6) . ? C162 C17 1.520(6) . ? C163 C164 1.416(6) . ? C163 H163 0.95 . ? C164 C165 1.393(7) . ? C164 C167 1.533(6) . ? C167 C160 1.532(8) . ? C167 C169 1.542(7) . ? C167 C168 1.548(8) . ? C168 H16A 0.98 . ? C168 H16B 0.98 . ? C168 H16C 0.98 . ? C169 H16D 0.98 . ? C169 H16E 0.98 . ? C169 H16F 0.98 . ? C160 H16G 0.98 . ? C160 H16H 0.98 . ? C160 H16I 0.98 . ? C165 C166 1.411(6) . ? C165 H165 0.95 . ? C166 C16 1.506(7) . ? C16 H16J 0.99 . ? C16 H16K 0.99 . ? O171 C171 1.379(5) . ? C171 C172 1.396(7) . ? C171 C176 1.399(6) . ? C172 C173 1.382(6) . ? C172 C18 1.507(6) . ? C173 C174 1.394(6) . ? C173 H173 0.95 . ? C174 C175 1.400(7) . ? C174 C177 1.532(7) . ? C177 C179 1.478(9) . ? C177 C170 1.508(9) . ? C177 C178 1.529(9) . ? C178 H17A 0.98 . ? C178 H17B 0.98 . ? C178 H17C 0.98 . ? C179 H17D 0.98 . ? C179 H17E 0.98 . ? C179 H17F 0.98 . ? C170 H17G 0.98 . ? C170 H17H 0.98 . ? C170 H17I 0.98 . ? C175 C176 1.391(6) . ? C175 H175 0.95 . ? C176 C17 1.502(7) . ? C17 H17J 0.99 . ? C17 H17K 0.99 . ? O181 C181 1.350(6) . ? C181 C182 1.403(6) . ? C181 C186 1.420(6) . ? C182 C183 1.410(7) . ? C183 C184 1.399(6) . ? C183 H183 0.95 . ? C184 C185 1.391(6) . ? C184 C187 1.527(7) . ? C187 C188 1.498(9) . ? C187 C180 1.533(7) . ? C187 C189 1.546(8) . ? C188 H18A 0.98 . ? C188 H18B 0.98 . ? C188 H18C 0.98 . ? C189 H18D 0.98 . ? C189 H18E 0.98 . ? C189 H18F 0.98 . ? C180 H18G 0.98 . ? C180 H18H 0.98 . ? C180 H18I 0.98 . ? C185 C186 1.400(7) . ? C185 H185 0.95 . ? C186 C18 1.507(6) . ? C18 H18J 0.99 . ? C18 H18K 0.99 . ? O211 C211 1.353(5) . ? C211 C216 1.406(6) . ? C211 C212 1.407(6) . ? C212 C213 1.389(6) . ? C212 C22 1.504(6) . ? C213 C214 1.389(7) . ? C213 H213 0.95 . ? C214 C215 1.385(7) . ? C214 C217 1.527(7) . ? C217 C219 1.502(8) . ? C217 C210 1.539(8) . ? C217 C218 1.554(9) . ? C218 H21A 0.98 . ? C218 H21B 0.98 . ? C218 H21C 0.98 . ? C219 H21D 0.98 . ? C219 H21E 0.98 . ? C219 H21F 0.98 . ? C210 H21G 0.98 . ? C210 H21H 0.98 . ? C210 H21I 0.98 . ? C215 C216 1.396(6) . ? C215 H215 0.95 . ? C216 C21 1.489(6) . ? C21 C282 1.486(6) . ? C21 H21J 0.99 . ? C21 H21K 0.99 . ? O221 C221 1.375(5) . ? C221 C222 1.381(6) . ? C221 C226 1.408(6) . ? C222 C223 1.390(6) . ? C222 C23 1.527(6) . ? C223 C224 1.397(6) . ? C223 H223 0.95 . ? C224 C225 1.393(6) . ? C224 C227 1.519(7) . ? C227 C228 1.521(8) . ? C227 C220 1.526(7) . ? C227 C229 1.537(8) . ? C228 H22A 0.98 . ? C228 H22B 0.98 . ? C228 H22C 0.98 . ? C229 H22D 0.98 . ? C229 H22E 0.98 . ? C229 H22F 0.98 . ? C220 H22G 0.98 . ? C220 H22H 0.98 . ? C220 H22I 0.98 . ? C225 C226 1.378(6) . ? C225 H225 0.95 . ? C226 C22 1.516(6) . ? C22 H22J 0.99 . ? C22 H22K 0.99 . ? O231 C231 1.389(5) . ? C231 C236 1.378(6) . ? C231 C232 1.389(6) . ? C232 C233 1.396(6) . ? C232 C24 1.501(6) . ? C233 C234 1.386(6) . ? C233 H233 0.95 . ? C234 C235 1.394(6) . ? C234 C237 1.542(6) . ? C237 C239 1.523(7) . ? C237 C230 1.539(7) . ? C237 C238 1.566(7) . ? C238 H23A 0.98 . ? C238 H23B 0.98 . ? C238 H23C 0.98 . ? C239 H23D 0.98 . ? C239 H23E 0.98 . ? C239 H23F 0.98 . ? C230 H23G 0.98 . ? C230 H23H 0.98 . ? C230 H23I 0.98 . ? C235 C236 1.393(6) . ? C235 H235 0.95 . ? C236 C23 1.524(6) . ? C23 H23J 0.99 . ? C23 H23K 0.99 . ? O241 C241 1.357(5) . ? C241 C242 1.390(6) . ? C241 C246 1.394(6) . ? C242 C243 1.397(6) . ? C242 C25 1.526(6) . ? C243 C244 1.393(6) . ? C243 H243 0.95 . ? C244 C245 1.394(6) . ? C244 C247 1.546(6) . ? C247 C249 1.498(7) . ? C247 C248 1.524(7) . ? C247 C240 1.562(7) . ? C248 H24A 0.98 . ? C248 H24B 0.98 . ? C248 H24C 0.98 . ? C249 H24D 0.98 . ? C249 H24E 0.98 . ? C249 H24F 0.98 . ? C240 H24G 0.98 . ? C240 H24H 0.98 . ? C240 H24I 0.98 . ? C245 C246 1.397(6) . ? C245 H245 0.95 . ? C246 C24 1.519(6) . ? C24 H24J 0.99 . ? C24 H24K 0.99 . ? O251 C251 1.357(5) . ? C251 C252 1.405(6) . ? C251 C256 1.414(6) . ? C252 C253 1.391(7) . ? C252 C26 1.501(6) . ? C253 C254 1.389(6) . ? C253 H253 0.95 . ? C254 C255 1.397(6) . ? C254 C257 1.538(7) . ? C257 C250 1.507(8) . ? C257 C258 1.533(8) . ? C257 C259 1.536(8) . ? C258 H25A 0.98 . ? C258 H25B 0.98 . ? C258 H25C 0.98 . ? C259 H25D 0.98 . ? C259 H25E 0.98 . ? C259 H25F 0.98 . ? C250 H25G 0.98 . ? C250 H25H 0.98 . ? C250 H25I 0.98 . ? C255 C256 1.390(6) . ? C255 H255 0.95 . ? C256 C25 1.531(6) . ? C25 H25J 0.99 . ? C25 H25K 0.99 . ? O261 C261 1.360(5) . ? C261 C262 1.398(6) . ? C261 C266 1.410(7) . ? C262 C263 1.406(6) . ? C262 C27 1.531(6) . ? C263 C264 1.386(7) . ? C263 H263 0.95 . ? C264 C265 1.408(7) . ? C264 C267 1.554(7) . ? C267 C260 1.501(8) . ? C267 C269 1.511(8) . ? C267 C268 1.513(8) . ? C268 H26A 0.98 . ? C268 H26B 0.98 . ? C268 H26C 0.98 . ? C269 H26D 0.98 . ? C269 H26E 0.98 . ? C269 H26F 0.98 . ? C260 H26G 0.98 . ? C260 H26H 0.98 . ? C260 H26I 0.98 . ? C265 C266 1.412(6) . ? C265 H265 0.95 . ? C266 C26 1.508(6) . ? C26 H26J 0.99 . ? C26 H26K 0.99 . ? O271 C271 1.383(5) . ? C271 C276 1.379(6) . ? C271 C272 1.419(6) . ? C272 C273 1.402(6) . ? C272 C28 1.503(6) . ? C273 C274 1.383(6) . ? C273 H273 0.95 . ? C274 C275 1.416(6) . ? C274 C277 1.533(6) . ? C277 C270 1.512(7) . ? C277 C278 1.538(7) . ? C277 C279 1.540(7) . ? C278 H27A 0.98 . ? C278 H27B 0.98 . ? C278 H27C 0.98 . ? C279 H27D 0.98 . ? C279 H27E 0.98 . ? C279 H27F 0.98 . ? C270 H27G 0.98 . ? C270 H27H 0.98 . ? C270 H27I 0.98 . ? C275 C276 1.399(6) . ? C275 H275 0.95 . ? C276 C27 1.534(6) . ? C27 H27J 0.99 . ? C27 H27K 0.99 . ? O281 C281 1.365(5) . ? C281 C282 1.399(7) . ? C281 C286 1.414(6) . ? C282 C283 1.388(6) . ? C283 C284 1.393(7) . ? C283 H283 0.95 . ? C284 C285 1.384(7) . ? C284 C287 1.529(7) . ? C287 C289 1.489(9) . ? C287 C280 1.496(8) . ? C287 C288 1.533(9) . ? C288 H28A 0.98 . ? C288 H28B 0.98 . ? C288 H28C 0.98 . ? C289 H28D 0.98 . ? C289 H28E 0.98 . ? C289 H28F 0.98 . ? C280 H28G 0.98 . ? C280 H28H 0.98 . ? C280 H28I 0.98 . ? C285 C286 1.403(6) . ? C285 H285 0.95 . ? C286 C28 1.507(7) . ? C28 H28J 0.99 . ? C28 H28K 0.99 . ? N101 C104 1.476(8) . ? N101 C101 1.484(7) . ? N101 C103 1.512(8) . ? N101 H101 0.93 . ? C103 H10A 0.98 . ? C103 H10B 0.98 . ? C103 H10C 0.98 . ? C104 H10D 0.98 . ? C104 H10E 0.98 . ? C104 H10F 0.98 . ? C101 C102 1.516(8) . ? C101 H10G 0.99 . ? C101 H10H 0.99 . ? C102 N102 1.477(7) . ? C102 H10I 0.99 . ? C102 H10J 0.99 . ? N102 C106 1.444(8) . ? N102 C105 1.452(9) . ? C105 H10K 0.98 . ? C105 H10L 0.98 . ? C105 H10M 0.98 . ? C106 H10N 0.98 . ? C106 H10O 0.98 . ? C106 H10P 0.98 . ? N201 C201 1.490(6) . ? N201 C203 1.500(6) . ? N201 C204 1.512(6) . ? N201 H201 0.93 . ? C203 H20A 0.98 . ? C203 H20B 0.98 . ? C203 H20C 0.98 . ? C204 H20D 0.98 . ? C204 H20E 0.98 . ? C204 H20F 0.98 . ? C201 C202 1.511(7) . ? C201 H20G 0.99 . ? C201 H20H 0.99 . ? C202 N202 1.484(8) . ? C202 H20I 0.99 . ? C202 H20J 0.99 . ? N202 C205 1.407(10) . ? N202 C206 1.448(9) . ? C205 H20K 0.98 . ? C205 H20L 0.98 . ? C205 H20M 0.98 . ? C206 H20N 0.98 . ? C206 H20O 0.98 . ? C206 H20P 0.98 . ? N301 C304 1.452(9) . ? N301 C303 1.469(8) . ? N301 C301 1.485(8) . ? N301 H301 0.93 . ? C303 H30A 0.98 . ? C303 H30B 0.98 . ? C303 H30C 0.98 . ? C304 H30D 0.9802 . ? C304 H30E 0.9802 . ? C304 H30F 0.9802 . ? C301 C302 1.544(10) . ? C301 H30G 0.99 . ? C301 H30H 0.99 . ? C302 N302 1.413(9) . ? C302 H30I 0.99 . ? C302 H30J 0.99 . ? N302 C305 1.479(10) . ? N302 C306 1.495(11) . ? C305 H30K 0.98 . ? C305 H30L 0.98 . ? C305 H30M 0.98 . ? C306 H30N 0.98 . ? C306 H30O 0.98 . ? C306 H30P 0.98 . ? N401 C401 1.390(12) . ? N401 C404 1.465(8) . ? N401 C403 1.471(7) . ? N401 C407 1.671(12) . ? N401 H401 0.93 . ? C403 H40A 0.98 . ? C403 H40B 0.98 . ? C403 H40C 0.98 . ? C404 H40D 0.98 . ? C404 H40E 0.98 . ? C404 H40F 0.98 . ? C401 C402 1.586(14) . ? C401 H40G 0.99 . ? C401 H40H 0.99 . ? C402 N402 1.481(14) . ? C402 H40I 0.99 . ? C402 H40J 0.99 . ? N402 C406 1.369(16) . ? N402 C405 1.445(17) . ? C405 H40K 0.98 . ? C405 H40L 0.98 . ? C405 H40M 0.98 . ? C406 H40N 0.98 . ? C406 H40O 0.98 . ? C406 H40P 0.98 . ? C407 C408 1.507(14) . ? C407 H40Q 0.99 . ? C407 H40R 0.99 . ? C408 N403 1.485(13) . ? C408 H40S 0.99 . ? C408 H40T 0.99 . ? N403 C409 1.511(16) . ? N403 C400 1.622(14) . ? C409 H40U 0.98 . ? C409 H40V 0.98 . ? C409 H40W 0.98 . ? C400 H40X 0.9801 . ? C400 H40Y 0.9801 . ? C400 H40Z 0.9801 . ? N501 C509 1.375(12) . ? N501 C504 1.388(12) . ? N501 C507 1.416(11) . ? N501 C503 1.505(12) . ? N501 C501 1.549(10) . ? N501 C50A 1.571(12) . ? N501 H501 0.93 . ? C503 H50A 0.98 . ? C503 H50B 0.98 . ? C503 H50C 0.98 . ? C504 H50D 0.98 . ? C504 H50E 0.98 . ? C504 H50F 0.98 . ? C501 C502 1.489(14) . ? C501 H50G 0.99 . ? C501 H50H 0.99 . ? C502 N502 1.440(15) . ? C502 H50I 0.99 . ? C502 H50J 0.99 . ? N502 C505 1.471(17) . ? N502 C506 1.492(15) . ? C505 H50K 0.98 . ? C505 H50L 0.98 . ? C505 H50M 0.98 . ? C506 H50O 0.98 . ? C506 H50P 0.98 . ? C506 H50Q 0.98 . ? N503 C508 1.469(19) . ? N503 C50B 1.489(14) . ? N503 C50C 1.534(19) . ? C507 C508 1.492(18) . ? C507 H50R 0.99 . ? C507 H50S 0.99 . ? C508 H50T 0.99 . ? C508 H50U 0.99 . ? C509 H50V 0.98 . ? C509 H50W 0.98 . ? C509 H50X 0.98 . ? C50A H50Y 0.98 . ? C50A H50Z 0.98 . ? C50A H500 0.98 . ? C50B H502 0.98 . ? C50B H503 0.98 . ? C50B H504 0.98 . ? C50C H505 0.98 . ? C50C H506 0.98 . ? C50C H507 0.98 . ? N601 C601 1.473(8) . ? N601 C604 1.482(7) . ? N601 C603 1.497(8) . ? N601 H601 0.93 . ? C603 H60A 0.98 . ? C603 H60B 0.98 . ? C603 H60C 0.98 . ? C604 H60D 0.98 . ? C604 H60E 0.98 . ? C604 H60F 0.98 . ? C601 C602 1.450(10) . ? C601 H60G 0.99 . ? C601 H60H 0.99 . ? C602 N602 1.602(12) . ? C602 H60I 0.99 . ? C602 H60J 0.99 . ? N602 C605 1.500(15) . ? N602 C606 1.597(13) . ? C605 H60K 0.98 . ? C605 H60L 0.98 . ? C605 H60M 0.98 . ? C606 H60N 0.98 . ? C606 H60O 0.98 . ? C606 H60P 0.98 . ? N011 C011 1.142(8) . ? C011 C012 1.445(9) . ? C012 H01A 0.98 . ? C012 H01B 0.98 . ? C012 H01C 0.98 . ? N021 C021 1.121(10) . ? C021 C022 1.448(9) . ? C022 H02A 0.98 . ? C022 H02B 0.98 . ? C022 H02C 0.98 . ? N031 C031 1.172(10) . ? C031 C032 1.449(10) . ? C032 H03A 0.98 . ? C032 H03B 0.98 . ? C032 H03C 0.98 . ? N041 C041 1.182(11) . ? C041 C042 1.429(11) . ? C042 H04A 0.98 . ? C042 H04B 0.98 . ? C042 H04C 0.98 . ? N051 C051 1.198(10) . ? C051 C052 1.430(10) . ? C052 H05A 0.98 . ? C052 H05B 0.98 . ? C052 H05C 0.98 . ? N061 C061 1.145(9) . ? C061 C062 1.410(9) . ? C062 H06A 0.98 . ? C062 H06B 0.98 . ? C062 H06C 0.98 . ? N071 C071 1.122(9) . ? C071 C072 1.457(9) . ? C072 H07A 0.98 . ? C072 H07B 0.98 . ? C072 H07C 0.98 . ? N081 C081 1.232(15) . ? C081 C082 1.434(15) . ? C082 H08A 0.98 . ? C082 H08B 0.98 . ? C082 H08C 0.98 . ? N091 C091 1.119(16) . ? C091 C092 1.558(19) . ? C092 H09A 0.98 . ? C092 H09B 0.98 . ? C092 H09C 0.98 . ? N0A1 C0A1 1.272(8) . ? C0A1 C0A2 1.590(8) . ? C0A2 H0A1 0.98 . ? C0A2 H0A2 0.98 . ? C0A2 H0A3 0.98 . ? N0B1 C0B1 1.260(7) . ? C0B1 C0B2 1.476(7) . ? C0B2 H0B1 0.98 . ? C0B2 H0B2 0.98 . ? C0B2 H0B3 0.98 . ? O0S S0S 1.32(2) . ? S0S C01S 1.838(12) . ? S0S C02S 2.015(16) . ? C01S H01D 0.98 . ? C01S H01E 0.98 . ? C01S H01F 0.98 . ? C02S H02D 0.98 . ? C02S H02E 0.98 . ? C02S H02F 0.98 . ? 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 O101 U11 O102 177.91(14) . . ? O101 U11 O111 89.78(13) . . ? O102 U11 O111 91.65(13) . . ? O101 U11 O181 90.16(13) . . ? O102 U11 O181 88.68(13) . . ? O111 U11 O181 77.11(11) . . ? O101 U11 O10 85.08(13) . . ? O102 U11 O10 94.58(13) . . ? O111 U11 O10 145.44(10) . . ? O181 U11 O10 136.90(10) . . ? O101 U11 O121 93.71(12) . . ? O102 U11 O121 88.12(13) . . ? O111 U11 O121 76.17(11) . . ? O181 U11 O121 152.98(10) . . ? O10 U11 O121 70.11(10) . . ? O101 U11 O171 92.61(12) . . ? O102 U11 O171 85.38(12) . . ? O111 U11 O171 149.56(11) . . ? O181 U11 O171 72.55(10) . . ? O10 U11 O171 64.95(10) . . ? O121 U11 O171 133.82(10) . . ? O104 U12 O103 178.80(15) . . ? O104 U12 O141 92.95(14) . . ? O103 U12 O141 87.78(14) . . ? O104 U12 O151 90.66(13) . . ? O103 U12 O151 90.42(13) . . ? O141 U12 O151 78.11(11) . . ? O104 U12 O10 94.30(13) . . ? O103 U12 O10 84.52(13) . . ? O141 U12 O10 137.79(10) . . ? O151 U12 O10 143.18(11) . . ? O104 U12 O161 87.24(13) . . ? O103 U12 O161 92.55(13) . . ? O141 U12 O161 152.76(11) . . ? O151 U12 O161 74.65(11) . . ? O10 U12 O161 69.19(10) . . ? O104 U12 O131 84.94(12) . . ? O103 U12 O131 94.37(12) . . ? O141 U12 O131 73.35(10) . . ? O151 U12 O131 150.83(11) . . ? O10 U12 O131 65.99(10) . . ? O161 U12 O131 133.66(10) . . ? O202 U21 O201 177.79(14) . . ? O202 U21 O211 93.69(13) . . ? O201 U21 O211 87.60(14) . . ? O202 U21 O281 89.75(12) . . ? O201 U21 O281 88.72(13) . . ? O211 U21 O281 79.46(11) . . ? O202 U21 O20 95.58(13) . . ? O201 U21 O20 84.47(13) . . ? O211 U21 O20 142.13(10) . . ? O281 U21 O20 137.09(10) . . ? O202 U21 O221 87.28(12) . . ? O201 U21 O221 94.79(12) . . ? O211 U21 O221 74.61(10) . . ? O281 U21 O221 153.64(11) . . ? O20 U21 O221 69.27(10) . . ? O202 U21 O271 85.88(13) . . ? O201 U21 O271 92.13(13) . . ? O211 U21 O271 151.59(10) . . ? O281 U21 O271 72.13(10) . . ? O20 U21 O271 65.87(9) . . ? O221 U21 O271 133.62(10) . . ? O203 U22 O204 179.58(15) . . ? O203 U22 O241 89.33(12) . . ? O204 U22 O241 90.93(12) . . ? O203 U22 O251 91.19(13) . . ? O204 U22 O251 89.20(13) . . ? O241 U22 O251 76.25(10) . . ? O203 U22 O20 84.91(13) . . ? O204 U22 O20 94.68(13) . . ? O241 U22 O20 140.23(10) . . ? O251 U22 O20 143.03(9) . . ? O203 U22 O261 92.99(12) . . ? O204 U22 O261 86.94(12) . . ? O241 U22 O261 150.78(10) . . ? O251 U22 O261 74.58(10) . . ? O20 U22 O261 68.95(9) . . ? O203 U22 O231 93.40(12) . . ? O204 U22 O231 86.35(12) . . ? O241 U22 O231 74.19(10) . . ? O251 U22 O231 150.01(9) . . ? O20 U22 O231 66.95(9) . . ? O261 U22 O231 134.60(10) . . ? U11 O10 U12 146.24(15) . . ? U11 O10 H10 106.9 . . ? U12 O10 H10 106.9 . . ? U21 O20 U22 144.20(14) . . ? U21 O20 H20 107.9 . . ? U22 O20 H20 107.9 . . ? C111 O111 U11 136.4(3) . . ? O111 C111 C112 120.6(4) . . ? O111 C111 C116 121.1(4) . . ? C112 C111 C116 118.2(4) . . ? C113 C112 C111 119.7(4) . . ? C113 C112 C12 122.3(4) . . ? C111 C112 C12 118.0(4) . . ? C112 C113 C114 122.8(4) . . ? C112 C113 H113 118.6 . . ? C114 C113 H113 118.6 . . ? C115 C114 C113 117.1(4) . . ? C115 C114 C117 121.7(4) . . ? C113 C114 C117 121.1(4) . . ? C110 C117 C118 106.4(5) . . ? C110 C117 C119 113.0(5) . . ? C118 C117 C119 104.8(5) . . ? C110 C117 C114 112.8(4) . . ? C118 C117 C114 110.7(4) . . ? C119 C117 C114 108.8(5) . . ? C117 C118 H11A 109.5 . . ? C117 C118 H11B 109.5 . . ? H11A C118 H11B 109.5 . . ? C117 C118 H11C 109.5 . . ? H11A C118 H11C 109.5 . . ? H11B C118 H11C 109.5 . . ? C117 C119 H11D 109.5 . . ? C117 C119 H11E 109.5 . . ? H11D C119 H11E 109.5 . . ? C117 C119 H11F 109.5 . . ? H11D C119 H11F 109.5 . . ? H11E C119 H11F 109.5 . . ? C117 C110 H11G 109.5 . . ? C117 C110 H11H 109.5 . . ? H11G C110 H11H 109.5 . . ? C117 C110 H11I 109.5 . . ? H11G C110 H11I 109.5 . . ? H11H C110 H11I 109.5 . . ? C116 C115 C114 122.4(4) . . ? C116 C115 H115 118.8 . . ? C114 C115 H115 118.8 . . ? C115 C116 C111 119.6(4) . . ? C115 C116 C11 122.0(4) . . ? C111 C116 C11 118.3(4) . . ? C182 C11 C116 110.8(4) . . ? C182 C11 H11J 109.5 . . ? C116 C11 H11J 109.5 . . ? C182 C11 H11K 109.5 . . ? C116 C11 H11K 109.5 . . ? H11J C11 H11K 108.1 . . ? C121 O121 U11 126.1(3) . . ? O121 C121 C122 120.6(4) . . ? O121 C121 C126 120.5(4) . . ? C122 C121 C126 118.8(4) . . ? C121 C122 C123 119.0(4) . . ? C121 C122 C13 119.3(4) . . ? C123 C122 C13 121.6(4) . . ? C124 C123 C122 123.0(4) . . ? C124 C123 H123 118.5 . . ? C122 C123 H123 118.5 . . ? C123 C124 C125 116.6(4) . . ? C123 C124 C127 120.6(4) . . ? C125 C124 C127 122.8(4) . . ? C129 C127 C120 109.1(4) . . ? C129 C127 C128 109.7(4) . . ? C120 C127 C128 107.7(5) . . ? C129 C127 C124 110.3(4) . . ? C120 C127 C124 111.2(4) . . ? C128 C127 C124 108.7(4) . . ? C127 C128 H12A 109.5 . . ? C127 C128 H12B 109.5 . . ? H12A C128 H12B 109.5 . . ? C127 C128 H12C 109.5 . . ? H12A C128 H12C 109.5 . . ? H12B C128 H12C 109.5 . . ? C127 C129 H12D 109.5 . . ? C127 C129 H12E 109.5 . . ? H12D C129 H12E 109.5 . . ? C127 C129 H12F 109.5 . . ? H12D C129 H12F 109.5 . . ? H12E C129 H12F 109.5 . . ? C127 C120 H12G 109.5 . . ? C127 C120 H12H 109.5 . . ? H12G C120 H12H 109.5 . . ? C127 C120 H12I 109.5 . . ? H12G C120 H12I 109.5 . . ? H12H C120 H12I 109.5 . . ? C124 C125 C126 123.0(4) . . ? C124 C125 H125 118.5 . . ? C126 C125 H125 118.5 . . ? C125 C126 C121 119.5(4) . . ? C125 C126 C12 119.2(4) . . ? C121 C126 C12 121.3(4) . . ? C126 C12 C112 113.9(4) . . ? C126 C12 H12J 108.8 . . ? C112 C12 H12J 108.8 . . ? C126 C12 H12K 108.8 . . ? C112 C12 H12K 108.8 . . ? H12J C12 H12K 107.7 . . ? C131 O131 U12 124.4(3) . . ? C136 C131 O131 121.2(4) . . ? C136 C131 C132 121.1(4) . . ? O131 C131 C132 117.7(4) . . ? C133 C132 C131 117.5(4) . . ? C133 C132 C14 120.3(4) . . ? C131 C132 C14 122.1(4) . . ? C134 C133 C132 123.2(5) . . ? C134 C133 H133 118.4 . . ? C132 C133 H133 118.4 . . ? C133 C134 C135 118.3(5) . . ? C133 C134 C137 120.8(5) . . ? C135 C134 C137 120.9(5) . . ? C130 C137 C138 109.0(5) . . ? C130 C137 C134 112.5(5) . . ? C138 C137 C134 109.5(5) . . ? C130 C137 C139 108.9(5) . . ? C138 C137 C139 108.2(6) . . ? C134 C137 C139 108.6(5) . . ? C137 C138 H13A 109.5 . . ? C137 C138 H13B 109.5 . . ? H13A C138 H13B 109.5 . . ? C137 C138 H13C 109.5 . . ? H13A C138 H13C 109.5 . . ? H13B C138 H13C 109.5 . . ? C137 C139 H13D 109.5 . . ? C137 C139 H13E 109.5 . . ? H13D C139 H13E 109.5 . . ? C137 C139 H13F 109.5 . . ? H13D C139 H13F 109.5 . . ? H13E C139 H13F 109.5 . . ? C137 C130 H13G 109.5 . . ? C137 C130 H13H 109.5 . . ? H13G C130 H13H 109.5 . . ? C137 C130 H13I 109.5 . . ? H13G C130 H13I 109.5 . . ? H13H C130 H13I 109.5 . . ? C136 C135 C134 121.0(5) . . ? C136 C135 H135 119.5 . . ? C134 C135 H135 119.5 . . ? C131 C136 C135 118.7(5) . . ? C131 C136 C13 120.7(4) . . ? C135 C136 C13 120.4(4) . . ? C122 C13 C136 113.7(4) . . ? C122 C13 H13J 108.8 . . ? C136 C13 H13J 108.8 . . ? C122 C13 H13K 108.8 . . ? C136 C13 H13K 108.8 . . ? H13J C13 H13K 107.7 . . ? C141 O141 U12 141.4(3) . . ? O141 C141 C142 122.1(4) . . ? O141 C141 C146 119.5(4) . . ? C142 C141 C146 118.4(4) . . ? C143 C142 C141 119.7(5) . . ? C143 C142 C15 119.6(4) . . ? C141 C142 C15 120.3(5) . . ? C144 C143 C142 122.8(5) . . ? C144 C143 H143 118.6 . . ? C142 C143 H143 118.6 . . ? C143 C144 C145 116.7(5) . . ? C143 C144 C147 121.7(5) . . ? C145 C144 C147 121.5(5) . . ? C149 C147 C148 113.3(7) . . ? C149 C147 C144 115.9(6) . . ? C148 C147 C144 110.6(6) . . ? C149 C147 C140 103.9(7) . . ? C148 C147 C140 101.0(6) . . ? C144 C147 C140 110.7(6) . . ? C147 C148 H14A 109.5 . . ? C147 C148 H14B 109.5 . . ? H14A C148 H14B 109.5 . . ? C147 C148 H14C 109.5 . . ? H14A C148 H14C 109.5 . . ? H14B C148 H14C 109.5 . . ? C147 C149 H14D 109.5 . . ? C147 C149 H14E 109.5 . . ? H14D C149 H14E 109.5 . . ? C147 C149 H14F 109.5 . . ? H14D C149 H14F 109.5 . . ? H14E C149 H14F 109.5 . . ? C147 C140 H14G 109.5 . . ? C147 C140 H14H 109.5 . . ? H14G C140 H14H 109.5 . . ? C147 C140 H14I 109.5 . . ? H14G C140 H14I 109.5 . . ? H14H C140 H14I 109.5 . . ? C146 C145 C144 121.7(5) . . ? C146 C145 H145 119.1 . . ? C144 C145 H145 119.1 . . ? C145 C146 C141 120.6(4) . . ? C145 C146 C14 120.9(4) . . ? C141 C146 C14 118.5(4) . . ? C146 C14 C132 113.0(4) . . ? C146 C14 H14J 109 . . ? C132 C14 H14J 109 . . ? C146 C14 H14K 109 . . ? C132 C14 H14K 109 . . ? H14J C14 H14K 107.8 . . ? C151 O151 U12 127.7(3) . . ? O151 C151 C156 121.5(5) . . ? O151 C151 C152 119.3(5) . . ? C156 C151 C152 119.2(5) . . ? C153 C152 C151 118.7(5) . . ? C153 C152 C16 120.5(5) . . ? C151 C152 C16 120.7(4) . . ? C154 C153 C152 122.6(5) . . ? C154 C153 H153 118.7 . . ? C152 C153 H153 118.7 . . ? C155 C154 C153 118.0(5) . . ? C155 C154 C157 121.1(6) . . ? C153 C154 C157 120.9(6) . . ? C15A C157 C15B 110.8(12) . . ? C158 C157 C150 109.0(9) . . ? C15A C157 C154 115.2(10) . . ? C15B C157 C154 113.0(8) . . ? C158 C157 C154 110.9(8) . . ? C150 C157 C154 108.3(7) . . ? C158 C157 C159 111.5(9) . . ? C150 C157 C159 105.2(9) . . ? C154 C157 C159 111.5(7) . . ? C15A C157 C15C 101.8(12) . . ? C15B C157 C15C 109.8(12) . . ? C154 C157 C15C 105.4(9) . . ? C157 C158 H15A 109.5 . . ? C157 C158 H15B 109.5 . . ? C157 C158 H15C 109.5 . . ? C157 C159 H15D 109.5 . . ? C157 C159 H15E 109.5 . . ? C157 C159 H15F 109.5 . . ? C157 C150 H15G 109.5 . . ? C157 C150 H15H 109.5 . . ? C157 C150 H15I 109.5 . . ? C157 C15A H15J 109.5 . . ? C157 C15A H15K 109.4 . . ? H15J C15A H15K 109.5 . . ? C157 C15A H15L 109.5 . . ? H15J C15A H15L 109.5 . . ? H15K C15A H15L 109.5 . . ? C157 C15B H15M 109.5 . . ? C157 C15B H15N 109.5 . . ? H15M C15B H15N 109.5 . . ? C157 C15B H15O 109.4 . . ? H15M C15B H15O 109.5 . . ? H15N C15B H15O 109.5 . . ? C157 C15C H15P 109.4 . . ? C157 C15C H15Q 109.5 . . ? H15P C15C H15Q 109.5 . . ? C157 C15C H15R 109.5 . . ? H15P C15C H15R 109.5 . . ? H15Q C15C H15R 109.5 . . ? C154 C155 C156 121.0(6) . . ? C154 C155 H155 119.5 . . ? C156 C155 H155 119.5 . . ? C151 C156 C155 120.3(5) . . ? C151 C156 C15 122.3(5) . . ? C155 C156 C15 117.3(5) . . ? C156 C15 C142 113.8(4) . . ? C156 C15 H15S 108.8 . . ? C142 C15 H15S 108.8 . . ? C156 C15 H15T 108.8 . . ? C142 C15 H15T 108.8 . . ? H15S C15 H15T 107.7 . . ? C161 O161 U12 130.2(3) . . ? O161 C161 C162 119.9(4) . . ? O161 C161 C166 120.7(4) . . ? C162 C161 C166 119.4(4) . . ? C163 C162 C161 120.1(4) . . ? C163 C162 C17 118.8(4) . . ? C161 C162 C17 120.8(4) . . ? C162 C163 C164 121.8(4) . . ? C162 C163 H163 119.1 . . ? C164 C163 H163 119.1 . . ? C165 C164 C163 116.7(4) . . ? C165 C164 C167 124.6(4) . . ? C163 C164 C167 118.7(4) . . ? C160 C167 C164 108.2(4) . . ? C160 C167 C169 108.6(4) . . ? C164 C167 C169 112.0(4) . . ? C160 C167 C168 109.5(5) . . ? C164 C167 C168 110.7(4) . . ? C169 C167 C168 107.8(5) . . ? C167 C168 H16A 109.5 . . ? C167 C168 H16B 109.5 . . ? H16A C168 H16B 109.5 . . ? C167 C168 H16C 109.5 . . ? H16A C168 H16C 109.5 . . ? H16B C168 H16C 109.5 . . ? C167 C169 H16D 109.5 . . ? C167 C169 H16E 109.5 . . ? H16D C169 H16E 109.5 . . ? C167 C169 H16F 109.5 . . ? H16D C169 H16F 109.5 . . ? H16E C169 H16F 109.5 . . ? C167 C160 H16G 109.5 . . ? C167 C160 H16H 109.5 . . ? H16G C160 H16H 109.5 . . ? C167 C160 H16I 109.5 . . ? H16G C160 H16I 109.5 . . ? H16H C160 H16I 109.5 . . ? C164 C165 C166 123.1(4) . . ? C164 C165 H165 118.5 . . ? C166 C165 H165 118.5 . . ? C161 C166 C165 118.9(5) . . ? C161 C166 C16 121.3(4) . . ? C165 C166 C16 119.4(4) . . ? C166 C16 C152 115.0(5) . . ? C166 C16 H16J 108.5 . . ? C152 C16 H16J 108.5 . . ? C166 C16 H16K 108.5 . . ? C152 C16 H16K 108.5 . . ? H16J C16 H16K 107.5 . . ? C171 O171 U11 130.1(3) . . ? O171 C171 C172 119.3(4) . . ? O171 C171 C176 120.1(4) . . ? C172 C171 C176 120.5(4) . . ? C173 C172 C171 119.3(4) . . ? C173 C172 C18 119.0(5) . . ? C171 C172 C18 121.7(4) . . ? C172 C173 C174 122.5(5) . . ? C172 C173 H173 118.7 . . ? C174 C173 H173 118.7 . . ? C173 C174 C175 116.4(4) . . ? C173 C174 C177 120.4(5) . . ? C175 C174 C177 123.2(4) . . ? C179 C177 C170 112.7(6) . . ? C179 C177 C178 102.6(6) . . ? C170 C177 C178 108.7(6) . . ? C179 C177 C174 111.6(5) . . ? C170 C177 C174 113.0(5) . . ? C178 C177 C174 107.6(5) . . ? C177 C178 H17A 109.5 . . ? C177 C178 H17B 109.5 . . ? H17A C178 H17B 109.5 . . ? C177 C178 H17C 109.5 . . ? H17A C178 H17C 109.5 . . ? H17B C178 H17C 109.5 . . ? C177 C179 H17D 109.5 . . ? C177 C179 H17E 109.5 . . ? H17D C179 H17E 109.5 . . ? C177 C179 H17F 109.5 . . ? H17D C179 H17F 109.5 . . ? H17E C179 H17F 109.5 . . ? C177 C170 H17G 109.5 . . ? C177 C170 H17H 109.5 . . ? H17G C170 H17H 109.5 . . ? C177 C170 H17I 109.5 . . ? H17G C170 H17I 109.5 . . ? H17H C170 H17I 109.5 . . ? C176 C175 C174 123.2(4) . . ? C176 C175 H175 118.4 . . ? C174 C175 H175 118.4 . . ? C175 C176 C171 118.0(4) . . ? C175 C176 C17 121.4(4) . . ? C171 C176 C17 120.5(4) . . ? C176 C17 C162 111.3(4) . . ? C176 C17 H17J 109.4 . . ? C162 C17 H17J 109.4 . . ? C176 C17 H17K 109.4 . . ? C162 C17 H17K 109.4 . . ? H17J C17 H17K 108 . . ? C181 O181 U11 130.7(3) . . ? O181 C181 C182 121.6(4) . . ? O181 C181 C186 119.8(4) . . ? C182 C181 C186 118.5(4) . . ? C181 C182 C183 119.1(4) . . ? C181 C182 C11 121.6(4) . . ? C183 C182 C11 119.1(4) . . ? C184 C183 C182 123.2(4) . . ? C184 C183 H183 118.4 . . ? C182 C183 H183 118.4 . . ? C185 C184 C183 116.3(5) . . ? C185 C184 C187 122.7(4) . . ? C183 C184 C187 121.0(4) . . ? C188 C187 C184 109.4(5) . . ? C188 C187 C180 107.3(5) . . ? C184 C187 C180 112.3(5) . . ? C188 C187 C189 110.4(6) . . ? C184 C187 C189 110.2(5) . . ? C180 C187 C189 107.2(5) . . ? C187 C188 H18A 109.5 . . ? C187 C188 H18B 109.5 . . ? H18A C188 H18B 109.5 . . ? C187 C188 H18C 109.5 . . ? H18A C188 H18C 109.5 . . ? H18B C188 H18C 109.5 . . ? C187 C189 H18D 109.5 . . ? C187 C189 H18E 109.5 . . ? H18D C189 H18E 109.5 . . ? C187 C189 H18F 109.5 . . ? H18D C189 H18F 109.5 . . ? H18E C189 H18F 109.5 . . ? C187 C180 H18G 109.5 . . ? C187 C180 H18H 109.5 . . ? H18G C180 H18H 109.5 . . ? C187 C180 H18I 109.5 . . ? H18G C180 H18I 109.5 . . ? H18H C180 H18I 109.5 . . ? C184 C185 C186 122.8(4) . . ? C184 C185 H185 118.6 . . ? C186 C185 H185 118.6 . . ? C185 C186 C181 119.8(4) . . ? C185 C186 C18 121.3(4) . . ? C181 C186 C18 118.8(4) . . ? C172 C18 C186 113.8(4) . . ? C172 C18 H18J 108.8 . . ? C186 C18 H18J 108.8 . . ? C172 C18 H18K 108.8 . . ? C186 C18 H18K 108.8 . . ? H18J C18 H18K 107.7 . . ? C211 O211 U21 137.6(3) . . ? O211 C211 C216 120.4(4) . . ? O211 C211 C212 119.8(4) . . ? C216 C211 C212 119.8(4) . . ? C213 C212 C211 118.4(4) . . ? C213 C212 C22 121.9(4) . . ? C211 C212 C22 119.6(4) . . ? C214 C213 C212 123.8(5) . . ? C214 C213 H213 118.1 . . ? C212 C213 H213 118.1 . . ? C215 C214 C213 116.2(4) . . ? C215 C214 C217 122.5(4) . . ? C213 C214 C217 121.3(5) . . ? C219 C217 C214 110.4(5) . . ? C219 C217 C210 110.7(6) . . ? C214 C217 C210 112.7(5) . . ? C219 C217 C218 108.2(6) . . ? C214 C217 C218 109.1(5) . . ? C210 C217 C218 105.6(5) . . ? C217 C218 H21A 109.5 . . ? C217 C218 H21B 109.5 . . ? H21A C218 H21B 109.5 . . ? C217 C218 H21C 109.5 . . ? H21A C218 H21C 109.5 . . ? H21B C218 H21C 109.5 . . ? C217 C219 H21D 109.5 . . ? C217 C219 H21E 109.5 . . ? H21D C219 H21E 109.5 . . ? C217 C219 H21F 109.5 . . ? H21D C219 H21F 109.5 . . ? H21E C219 H21F 109.5 . . ? C217 C210 H21G 109.5 . . ? C217 C210 H21H 109.5 . . ? H21G C210 H21H 109.5 . . ? C217 C210 H21I 109.5 . . ? H21G C210 H21I 109.5 . . ? H21H C210 H21I 109.5 . . ? C214 C215 C216 123.3(4) . . ? C214 C215 H215 118.4 . . ? C216 C215 H215 118.4 . . ? C215 C216 C211 118.6(4) . . ? C215 C216 C21 119.8(4) . . ? C211 C216 C21 121.4(4) . . ? C282 C21 C216 110.9(4) . . ? C282 C21 H21J 109.5 . . ? C216 C21 H21J 109.5 . . ? C282 C21 H21K 109.5 . . ? C216 C21 H21K 109.5 . . ? H21J C21 H21K 108.1 . . ? C221 O221 U21 126.2(3) . . ? O221 C221 C222 121.1(4) . . ? O221 C221 C226 120.1(4) . . ? C222 C221 C226 118.7(4) . . ? C221 C222 C223 120.2(4) . . ? C221 C222 C23 120.4(4) . . ? C223 C222 C23 119.3(4) . . ? C222 C223 C224 122.7(4) . . ? C222 C223 H223 118.7 . . ? C224 C223 H223 118.7 . . ? C225 C224 C223 115.4(4) . . ? C225 C224 C227 121.4(4) . . ? C223 C224 C227 123.1(4) . . ? C224 C227 C228 110.5(5) . . ? C224 C227 C220 109.8(4) . . ? C228 C227 C220 109.4(5) . . ? C224 C227 C229 112.7(4) . . ? C228 C227 C229 106.3(5) . . ? C220 C227 C229 108.0(5) . . ? C227 C228 H22A 109.5 . . ? C227 C228 H22B 109.5 . . ? H22A C228 H22B 109.5 . . ? C227 C228 H22C 109.5 . . ? H22A C228 H22C 109.5 . . ? H22B C228 H22C 109.5 . . ? C227 C229 H22D 109.5 . . ? C227 C229 H22E 109.5 . . ? H22D C229 H22E 109.5 . . ? C227 C229 H22F 109.5 . . ? H22D C229 H22F 109.5 . . ? H22E C229 H22F 109.5 . . ? C227 C220 H22G 109.5 . . ? C227 C220 H22H 109.5 . . ? H22G C220 H22H 109.5 . . ? C227 C220 H22I 109.5 . . ? H22G C220 H22I 109.5 . . ? H22H C220 H22I 109.5 . . ? C226 C225 C224 123.5(4) . . ? C226 C225 H225 118.2 . . ? C224 C225 H225 118.2 . . ? C225 C226 C221 119.4(4) . . ? C225 C226 C22 120.3(4) . . ? C221 C226 C22 120.3(4) . . ? C212 C22 C226 113.1(4) . . ? C212 C22 H22J 109 . . ? C226 C22 H22J 109 . . ? C212 C22 H22K 109 . . ? C226 C22 H22K 109 . . ? H22J C22 H22K 107.8 . . ? C231 O231 U22 126.6(3) . . ? C236 C231 C232 121.4(4) . . ? C236 C231 O231 120.1(4) . . ? C232 C231 O231 118.5(4) . . ? C231 C232 C233 117.7(4) . . ? C231 C232 C24 122.3(4) . . ? C233 C232 C24 120.0(4) . . ? C234 C233 C232 123.1(4) . . ? C234 C233 H233 118.5 . . ? C232 C233 H233 118.5 . . ? C233 C234 C235 116.6(4) . . ? C233 C234 C237 122.0(4) . . ? C235 C234 C237 121.3(4) . . ? C239 C237 C230 108.0(4) . . ? C239 C237 C234 112.8(4) . . ? C230 C237 C234 110.2(4) . . ? C239 C237 C238 109.3(4) . . ? C230 C237 C238 107.7(4) . . ? C234 C237 C238 108.7(4) . . ? C237 C238 H23A 109.5 . . ? C237 C238 H23B 109.5 . . ? H23A C238 H23B 109.5 . . ? C237 C238 H23C 109.5 . . ? H23A C238 H23C 109.5 . . ? H23B C238 H23C 109.5 . . ? C237 C239 H23D 109.5 . . ? C237 C239 H23E 109.5 . . ? H23D C239 H23E 109.5 . . ? C237 C239 H23F 109.5 . . ? H23D C239 H23F 109.5 . . ? H23E C239 H23F 109.5 . . ? C237 C230 H23G 109.5 . . ? C237 C230 H23H 109.5 . . ? H23G C230 H23H 109.5 . . ? C237 C230 H23I 109.5 . . ? H23G C230 H23I 109.5 . . ? H23H C230 H23I 109.5 . . ? C236 C235 C234 122.2(4) . . ? C236 C235 H235 118.9 . . ? C234 C235 H235 118.9 . . ? C231 C236 C235 118.8(4) . . ? C231 C236 C23 121.6(4) . . ? C235 C236 C23 119.5(4) . . ? C236 C23 C222 110.9(4) . . ? C236 C23 H23J 109.5 . . ? C222 C23 H23J 109.5 . . ? C236 C23 H23K 109.5 . . ? C222 C23 H23K 109.5 . . ? H23J C23 H23K 108.1 . . ? C241 O241 U22 135.9(2) . . ? O241 C241 C242 121.0(4) . . ? O241 C241 C246 119.7(4) . . ? C242 C241 C246 119.2(4) . . ? C241 C242 C243 120.4(4) . . ? C241 C242 C25 120.3(4) . . ? C243 C242 C25 119.3(4) . . ? C244 C243 C242 121.3(4) . . ? C244 C243 H243 119.4 . . ? C242 C243 H243 119.4 . . ? C245 C244 C243 117.5(4) . . ? C245 C244 C247 119.2(4) . . ? C243 C244 C247 123.2(4) . . ? C249 C247 C248 109.0(5) . . ? C249 C247 C244 113.6(4) . . ? C248 C247 C244 109.8(4) . . ? C249 C247 C240 108.6(4) . . ? C248 C247 C240 108.1(4) . . ? C244 C247 C240 107.6(4) . . ? C247 C248 H24A 109.5 . . ? C247 C248 H24B 109.5 . . ? H24A C248 H24B 109.5 . . ? C247 C248 H24C 109.5 . . ? H24A C248 H24C 109.5 . . ? H24B C248 H24C 109.5 . . ? C247 C249 H24D 109.5 . . ? C247 C249 H24E 109.5 . . ? H24D C249 H24E 109.5 . . ? C247 C249 H24F 109.5 . . ? H24D C249 H24F 109.5 . . ? H24E C249 H24F 109.5 . . ? C247 C240 H24G 109.5 . . ? C247 C240 H24H 109.5 . . ? H24G C240 H24H 109.5 . . ? C247 C240 H24I 109.5 . . ? H24G C240 H24I 109.5 . . ? H24H C240 H24I 109.5 . . ? C244 C245 C246 121.9(4) . . ? C244 C245 H245 119 . . ? C246 C245 H245 119 . . ? C241 C246 C245 119.6(4) . . ? C241 C246 C24 119.5(4) . . ? C245 C246 C24 120.9(4) . . ? C232 C24 C246 111.1(4) . . ? C232 C24 H24J 109.4 . . ? C246 C24 H24J 109.4 . . ? C232 C24 H24K 109.4 . . ? C246 C24 H24K 109.4 . . ? H24J C24 H24K 108 . . ? C251 O251 U22 129.1(3) . . ? O251 C251 C252 120.4(4) . . ? O251 C251 C256 120.4(4) . . ? C252 C251 C256 119.1(4) . . ? C253 C252 C251 119.0(4) . . ? C253 C252 C26 121.6(4) . . ? C251 C252 C26 119.2(4) . . ? C254 C253 C252 123.2(4) . . ? C254 C253 H253 118.4 . . ? C252 C253 H253 118.4 . . ? C253 C254 C255 116.8(4) . . ? C253 C254 C257 121.3(4) . . ? C255 C254 C257 121.9(4) . . ? C250 C257 C258 108.7(5) . . ? C250 C257 C259 108.2(5) . . ? C258 C257 C259 108.3(5) . . ? C250 C257 C254 112.9(5) . . ? C258 C257 C254 110.3(5) . . ? C259 C257 C254 108.3(5) . . ? C257 C258 H25A 109.5 . . ? C257 C258 H25B 109.5 . . ? H25A C258 H25B 109.5 . . ? C257 C258 H25C 109.5 . . ? H25A C258 H25C 109.5 . . ? H25B C258 H25C 109.5 . . ? C257 C259 H25D 109.5 . . ? C257 C259 H25E 109.5 . . ? H25D C259 H25E 109.5 . . ? C257 C259 H25F 109.5 . . ? H25D C259 H25F 109.5 . . ? H25E C259 H25F 109.5 . . ? C257 C250 H25G 109.5 . . ? C257 C250 H25H 109.5 . . ? H25G C250 H25H 109.5 . . ? C257 C250 H25I 109.5 . . ? H25G C250 H25I 109.5 . . ? H25H C250 H25I 109.5 . . ? C256 C255 C254 122.5(4) . . ? C256 C255 H255 118.8 . . ? C254 C255 H255 118.8 . . ? C255 C256 C251 119.3(4) . . ? C255 C256 C25 119.4(4) . . ? C251 C256 C25 121.0(4) . . ? C242 C25 C256 107.7(4) . . ? C242 C25 H25J 110.2 . . ? C256 C25 H25J 110.2 . . ? C242 C25 H25K 110.2 . . ? C256 C25 H25K 110.2 . . ? H25J C25 H25K 108.5 . . ? C261 O261 U22 130.1(3) . . ? O261 C261 C262 121.1(4) . . ? O261 C261 C266 120.0(4) . . ? C262 C261 C266 118.7(4) . . ? C261 C262 C263 120.1(4) . . ? C261 C262 C27 120.3(4) . . ? C263 C262 C27 119.5(4) . . ? C264 C263 C262 122.3(4) . . ? C264 C263 H263 118.8 . . ? C262 C263 H263 118.8 . . ? C263 C264 C265 117.4(4) . . ? C263 C264 C267 121.0(4) . . ? C265 C264 C267 121.5(5) . . ? C260 C267 C269 110.5(5) . . ? C260 C267 C268 106.9(5) . . ? C269 C267 C268 107.0(5) . . ? C260 C267 C264 112.4(4) . . ? C269 C267 C264 110.1(5) . . ? C268 C267 C264 109.8(4) . . ? C267 C268 H26A 109.5 . . ? C267 C268 H26B 109.5 . . ? H26A C268 H26B 109.5 . . ? C267 C268 H26C 109.5 . . ? H26A C268 H26C 109.5 . . ? H26B C268 H26C 109.5 . . ? C267 C269 H26D 109.5 . . ? C267 C269 H26E 109.5 . . ? H26D C269 H26E 109.5 . . ? C267 C269 H26F 109.5 . . ? H26D C269 H26F 109.5 . . ? H26E C269 H26F 109.5 . . ? C267 C260 H26G 109.5 . . ? C267 C260 H26H 109.5 . . ? H26G C260 H26H 109.5 . . ? C267 C260 H26I 109.5 . . ? H26G C260 H26I 109.5 . . ? H26H C260 H26I 109.5 . . ? C264 C265 C266 121.4(5) . . ? C264 C265 H265 119.3 . . ? C266 C265 H265 119.3 . . ? C261 C266 C265 119.9(4) . . ? C261 C266 C26 121.8(4) . . ? C265 C266 C26 118.3(4) . . ? C252 C26 C266 114.5(4) . . ? C252 C26 H26J 108.6 . . ? C266 C26 H26J 108.6 . . ? C252 C26 H26K 108.6 . . ? C266 C26 H26K 108.6 . . ? H26J C26 H26K 107.6 . . ? C271 O271 U21 130.8(3) . . ? C276 C271 O271 121.9(4) . . ? C276 C271 C272 119.7(4) . . ? O271 C271 C272 118.4(4) . . ? C273 C272 C271 118.2(4) . . ? C273 C272 C28 120.9(4) . . ? C271 C272 C28 120.8(4) . . ? C274 C273 C272 123.4(4) . . ? C274 C273 H273 118.3 . . ? C272 C273 H273 118.3 . . ? C273 C274 C275 116.9(4) . . ? C273 C274 C277 124.3(4) . . ? C275 C274 C277 118.8(4) . . ? C270 C277 C274 109.7(4) . . ? C270 C277 C278 109.2(4) . . ? C274 C277 C278 109.7(4) . . ? C270 C277 C279 108.6(4) . . ? C274 C277 C279 112.0(4) . . ? C278 C277 C279 107.6(4) . . ? C277 C278 H27A 109.5 . . ? C277 C278 H27B 109.5 . . ? H27A C278 H27B 109.5 . . ? C277 C278 H27C 109.5 . . ? H27A C278 H27C 109.5 . . ? H27B C278 H27C 109.5 . . ? C277 C279 H27D 109.5 . . ? C277 C279 H27E 109.5 . . ? H27D C279 H27E 109.5 . . ? C277 C279 H27F 109.5 . . ? H27D C279 H27F 109.5 . . ? H27E C279 H27F 109.5 . . ? C277 C270 H27G 109.5 . . ? C277 C270 H27H 109.5 . . ? H27G C270 H27H 109.5 . . ? C277 C270 H27I 109.5 . . ? H27G C270 H27I 109.5 . . ? H27H C270 H27I 109.5 . . ? C276 C275 C274 121.1(4) . . ? C276 C275 H275 119.4 . . ? C274 C275 H275 119.4 . . ? C271 C276 C275 120.7(4) . . ? C271 C276 C27 121.1(4) . . ? C275 C276 C27 118.2(4) . . ? C262 C27 C276 108.3(4) . . ? C262 C27 H27J 110 . . ? C276 C27 H27J 110 . . ? C262 C27 H27K 110 . . ? C276 C27 H27K 110 . . ? H27J C27 H27K 108.4 . . ? C281 O281 U21 127.5(3) . . ? O281 C281 C282 120.8(4) . . ? O281 C281 C286 120.1(4) . . ? C282 C281 C286 119.1(4) . . ? C283 C282 C281 119.3(4) . . ? C283 C282 C21 117.4(4) . . ? C281 C282 C21 123.2(4) . . ? C282 C283 C284 123.2(5) . . ? C282 C283 H283 118.4 . . ? C284 C283 H283 118.4 . . ? C285 C284 C283 116.7(4) . . ? C285 C284 C287 122.8(5) . . ? C283 C284 C287 120.4(5) . . ? C289 C287 C280 106.5(6) . . ? C289 C287 C284 110.9(5) . . ? C280 C287 C284 113.5(5) . . ? C289 C287 C288 109.3(6) . . ? C280 C287 C288 106.0(5) . . ? C284 C287 C288 110.4(5) . . ? C287 C288 H28A 109.5 . . ? C287 C288 H28B 109.5 . . ? H28A C288 H28B 109.5 . . ? C287 C288 H28C 109.5 . . ? H28A C288 H28C 109.5 . . ? H28B C288 H28C 109.5 . . ? C287 C289 H28D 109.5 . . ? C287 C289 H28E 109.5 . . ? H28D C289 H28E 109.5 . . ? C287 C289 H28F 109.5 . . ? H28D C289 H28F 109.5 . . ? H28E C289 H28F 109.5 . . ? C287 C280 H28G 109.5 . . ? C287 C280 H28H 109.5 . . ? H28G C280 H28H 109.5 . . ? C287 C280 H28I 109.5 . . ? H28G C280 H28I 109.5 . . ? H28H C280 H28I 109.5 . . ? C284 C285 C286 122.7(5) . . ? C284 C285 H285 118.7 . . ? C286 C285 H285 118.7 . . ? C285 C286 C281 119.0(5) . . ? C285 C286 C28 120.6(4) . . ? C281 C286 C28 120.4(4) . . ? C272 C28 C286 115.3(4) . . ? C272 C28 H28J 108.5 . . ? C286 C28 H28J 108.5 . . ? C272 C28 H28K 108.5 . . ? C286 C28 H28K 108.5 . . ? H28J C28 H28K 107.5 . . ? C104 N101 C101 112.2(5) . . ? C104 N101 C103 111.7(5) . . ? C101 N101 C103 112.0(5) . . ? C104 N101 H101 106.9 . . ? C101 N101 H101 106.9 . . ? C103 N101 H101 106.8 . . ? N101 C103 H10A 109.5 . . ? N101 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? N101 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 109.5 . . ? N101 C104 H10D 109.5 . . ? N101 C104 H10E 109.5 . . ? H10D C104 H10E 109.5 . . ? N101 C104 H10F 109.5 . . ? H10D C104 H10F 109.5 . . ? H10E C104 H10F 109.5 . . ? N101 C101 C102 111.3(5) . . ? N101 C101 H10G 109.4 . . ? C102 C101 H10G 109.4 . . ? N101 C101 H10H 109.4 . . ? C102 C101 H10H 109.4 . . ? H10G C101 H10H 108 . . ? N102 C102 C101 109.1(5) . . ? N102 C102 H10I 109.8 . . ? C101 C102 H10I 109.9 . . ? N102 C102 H10J 109.9 . . ? C101 C102 H10J 109.9 . . ? H10I C102 H10J 108.3 . . ? C106 N102 C105 108.2(6) . . ? C106 N102 C102 111.5(5) . . ? C105 N102 C102 111.3(6) . . ? N102 C105 H10K 109.5 . . ? N102 C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? N102 C105 H10M 109.5 . . ? H10K C105 H10M 109.5 . . ? H10L C105 H10M 109.5 . . ? N102 C106 H10N 109.5 . . ? N102 C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? N102 C106 H10P 109.5 . . ? H10N C106 H10P 109.5 . . ? H10O C106 H10P 109.5 . . ? C201 N201 C203 112.5(4) . . ? C201 N201 C204 109.4(3) . . ? C203 N201 C204 109.7(4) . . ? C201 N201 H201 108.3 . . ? C203 N201 H201 108.3 . . ? C204 N201 H201 108.3 . . ? N201 C203 H20A 109.5 . . ? N201 C203 H20B 109.5 . . ? H20A C203 H20B 109.5 . . ? N201 C203 H20C 109.5 . . ? H20A C203 H20C 109.5 . . ? H20B C203 H20C 109.5 . . ? N201 C204 H20D 109.5 . . ? N201 C204 H20E 109.5 . . ? H20D C204 H20E 109.5 . . ? N201 C204 H20F 109.5 . . ? H20D C204 H20F 109.5 . . ? H20E C204 H20F 109.5 . . ? N201 C201 C202 113.9(4) . . ? N201 C201 H20G 108.8 . . ? C202 C201 H20G 108.8 . . ? N201 C201 H20H 108.8 . . ? C202 C201 H20H 108.8 . . ? H20G C201 H20H 107.7 . . ? N202 C202 C201 107.1(4) . . ? N202 C202 H20I 110.3 . . ? C201 C202 H20I 110.3 . . ? N202 C202 H20J 110.3 . . ? C201 C202 H20J 110.3 . . ? H20I C202 H20J 108.5 . . ? C205 N202 C206 106.9(7) . . ? C205 N202 C202 112.2(6) . . ? C206 N202 C202 113.3(6) . . ? N202 C205 H20K 109.5 . . ? N202 C205 H20L 109.5 . . ? H20K C205 H20L 109.5 . . ? N202 C205 H20M 109.4 . . ? H20K C205 H20M 109.5 . . ? H20L C205 H20M 109.5 . . ? N202 C206 H20N 109.5 . . ? N202 C206 H20O 109.5 . . ? H20N C206 H20O 109.5 . . ? N202 C206 H20P 109.5 . . ? H20N C206 H20P 109.5 . . ? H20O C206 H20P 109.5 . . ? C304 N301 C303 113.4(6) . . ? C304 N301 C301 109.1(6) . . ? C303 N301 C301 107.2(5) . . ? C304 N301 H301 109 . . ? C303 N301 H301 109 . . ? C301 N301 H301 109 . . ? N301 C303 H30A 109.5 . . ? N301 C303 H30B 109.5 . . ? H30A C303 H30B 109.5 . . ? N301 C303 H30C 109.5 . . ? H30A C303 H30C 109.5 . . ? H30B C303 H30C 109.5 . . ? N301 C304 H30D 109.5 . . ? N301 C304 H30E 109.5 . . ? H30D C304 H30E 109.4 . . ? N301 C304 H30F 109.5 . . ? H30D C304 H30F 109.5 . . ? H30E C304 H30F 109.4 . . ? N301 C301 C302 114.8(6) . . ? N301 C301 H30G 108.6 . . ? C302 C301 H30G 108.6 . . ? N301 C301 H30H 108.6 . . ? C302 C301 H30H 108.6 . . ? H30G C301 H30H 107.5 . . ? N302 C302 C301 116.0(7) . . ? N302 C302 H30I 108.3 . . ? C301 C302 H30I 108.3 . . ? N302 C302 H30J 108.3 . . ? C301 C302 H30J 108.3 . . ? H30I C302 H30J 107.4 . . ? C302 N302 C305 113.1(7) . . ? C302 N302 C306 107.3(7) . . ? C305 N302 C306 111.7(8) . . ? N302 C305 H30K 109.5 . . ? N302 C305 H30L 109.5 . . ? H30K C305 H30L 109.5 . . ? N302 C305 H30M 109.5 . . ? H30K C305 H30M 109.5 . . ? H30L C305 H30M 109.5 . . ? N302 C306 H30N 109.5 . . ? N302 C306 H30O 109.5 . . ? H30N C306 H30O 109.5 . . ? N302 C306 H30P 109.5 . . ? H30N C306 H30P 109.5 . . ? H30O C306 H30P 109.5 . . ? C401 N401 C404 94.7(6) . . ? C401 N401 C403 113.4(6) . . ? C404 N401 C403 113.4(6) . . ? C404 N401 C407 120.3(6) . . ? C403 N401 C407 112.8(6) . . ? C401 N401 H401 111.5 . . ? C404 N401 H401 111.4 . . ? C403 N401 H401 111.4 . . ? N401 C403 H40A 109.5 . . ? N401 C403 H40B 109.5 . . ? H40A C403 H40B 109.5 . . ? N401 C403 H40C 109.5 . . ? H40A C403 H40C 109.5 . . ? H40B C403 H40C 109.5 . . ? N401 C404 H40D 109.5 . . ? N401 C404 H40E 109.5 . . ? H40D C404 H40E 109.5 . . ? N401 C404 H40F 109.5 . . ? H40D C404 H40F 109.5 . . ? H40E C404 H40F 109.5 . . ? N401 C401 C402 106.4(8) . . ? N401 C401 H40G 110.4 . . ? C402 C401 H40G 110.4 . . ? N401 C401 H40H 110.4 . . ? C402 C401 H40H 110.4 . . ? H40G C401 H40H 108.6 . . ? N402 C402 C401 104.7(8) . . ? N402 C402 H40I 110.8 . . ? C401 C402 H40I 110.8 . . ? N402 C402 H40J 110.8 . . ? C401 C402 H40J 110.8 . . ? H40I C402 H40J 108.9 . . ? C406 N402 C405 108.8(12) . . ? C406 N402 C402 113.6(10) . . ? C405 N402 C402 108.2(10) . . ? C408 C407 N401 115.9(9) . . ? C408 C407 H40Q 108.3 . . ? N401 C407 H40Q 108.3 . . ? C408 C407 H40R 108.3 . . ? N401 C407 H40R 108.3 . . ? H40Q C407 H40R 107.4 . . ? N403 C408 C407 116.9(10) . . ? N403 C408 H40S 108.1 . . ? C407 C408 H40S 108.1 . . ? N403 C408 H40T 108 . . ? C407 C408 H40T 108.1 . . ? H40S C408 H40T 107.3 . . ? C408 N403 C409 109.7(10) . . ? C408 N403 C400 124.5(10) . . ? C409 N403 C400 124.6(12) . . ? N403 C409 H40U 109.5 . . ? N403 C409 H40V 109.4 . . ? H40U C409 H40V 109.5 . . ? N403 C409 H40W 109.5 . . ? H40U C409 H40W 109.5 . . ? H40V C409 H40W 109.5 . . ? N403 C400 H40X 109.4 . . ? N403 C400 H40Y 109.4 . . ? H40X C400 H40Y 109.5 . . ? N403 C400 H40Z 109.6 . . ? H40X C400 H40Z 109.5 . . ? H40Y C400 H40Z 109.5 . . ? C509 N501 C504 135.5(8) . . ? C509 N501 C507 121.5(8) . . ? C504 N501 C503 111.1(8) . . ? C504 N501 C501 111.9(7) . . ? C503 N501 C501 106.4(7) . . ? C509 N501 C50A 106.2(8) . . ? C507 N501 C50A 107.0(7) . . ? C509 N501 H501 110.5 . . ? C504 N501 H501 109.1 . . ? C507 N501 H501 107.1 . . ? C503 N501 H501 109.1 . . ? C501 N501 H501 109.1 . . ? C50A N501 H501 103 . . ? N501 C503 H50A 109.5 . . ? N501 C503 H50B 109.5 . . ? N501 C503 H50C 109.5 . . ? N501 C504 H50D 109.5 . . ? N501 C504 H50E 109.5 . . ? N501 C504 H50F 109.5 . . ? C502 C501 N501 113.3(9) . . ? C502 C501 H50G 108.9 . . ? N501 C501 H50G 108.9 . . ? C502 C501 H50H 108.9 . . ? N501 C501 H50H 108.9 . . ? H50G C501 H50H 107.7 . . ? N502 C502 C501 112.8(10) . . ? N502 C502 H50I 109 . . ? C501 C502 H50I 109 . . ? N502 C502 H50J 109 . . ? C501 C502 H50J 109 . . ? H50I C502 H50J 107.8 . . ? C502 N502 C505 111.9(13) . . ? C502 N502 C506 110.6(12) . . ? C505 N502 C506 106.4(12) . . ? C508 N503 C50B 113.6(13) . . ? C508 N503 C50C 105.8(16) . . ? C50B N503 C50C 113.9(14) . . ? N501 C507 C508 111.5(11) . . ? N501 C507 H50R 109.3 . . ? C508 C507 H50R 109.3 . . ? N501 C507 H50S 109.3 . . ? C508 C507 H50S 109.3 . . ? H50R C507 H50S 108 . . ? N503 C508 C507 112.2(16) . . ? N503 C508 H50T 109.1 . . ? C507 C508 H50T 109.1 . . ? N503 C508 H50U 109.2 . . ? C507 C508 H50U 109.2 . . ? H50T C508 H50U 107.9 . . ? N501 C509 H50V 109.5 . . ? N501 C509 H50W 109.5 . . ? H50V C509 H50W 109.5 . . ? N501 C509 H50X 109.4 . . ? H50V C509 H50X 109.5 . . ? H50W C509 H50X 109.5 . . ? N501 C50A H50Y 109.5 . . ? N501 C50A H50Z 109.5 . . ? H50Y C50A H50Z 109.5 . . ? N501 C50A H500 109.5 . . ? H50Y C50A H500 109.5 . . ? H50Z C50A H500 109.5 . . ? N503 C50B H502 109.5 . . ? N503 C50B H503 109.5 . . ? H502 C50B H503 109.5 . . ? N503 C50B H504 109.5 . . ? H502 C50B H504 109.5 . . ? H503 C50B H504 109.5 . . ? N503 C50C H505 109.5 . . ? N503 C50C H506 109.5 . . ? H505 C50C H506 109.5 . . ? N503 C50C H507 109.3 . . ? H505 C50C H507 109.5 . . ? H506 C50C H507 109.5 . . ? C601 N601 C604 110.1(6) . . ? C601 N601 C603 115.6(6) . . ? C604 N601 C603 111.1(6) . . ? C601 N601 H601 106.5 . . ? C604 N601 H601 106.5 . . ? C603 N601 H601 106.5 . . ? N601 C603 H60A 109.5 . . ? N601 C603 H60B 109.5 . . ? H60A C603 H60B 109.5 . . ? N601 C603 H60C 109.5 . . ? H60A C603 H60C 109.5 . . ? H60B C603 H60C 109.5 . . ? N601 C604 H60D 109.5 . . ? N601 C604 H60E 109.5 . . ? H60D C604 H60E 109.5 . . ? N601 C604 H60F 109.5 . . ? H60D C604 H60F 109.5 . . ? H60E C604 H60F 109.5 . . ? C602 C601 N601 115.5(7) . . ? C602 C601 H60G 108.4 . . ? N601 C601 H60G 108.4 . . ? C602 C601 H60H 108.4 . . ? N601 C601 H60H 108.4 . . ? H60G C601 H60H 107.5 . . ? C601 C602 N602 119.0(9) . . ? C601 C602 H60I 107.6 . . ? N602 C602 H60I 107.6 . . ? C601 C602 H60J 107.6 . . ? N602 C602 H60J 107.6 . . ? H60I C602 H60J 107 . . ? C605 N602 C606 123.8(14) . . ? C605 N602 C602 101.7(13) . . ? C606 N602 C602 117.4(11) . . ? N602 C605 H60K 109.5 . . ? N602 C605 H60L 109.4 . . ? H60K C605 H60L 109.5 . . ? N602 C605 H60M 109.5 . . ? H60K C605 H60M 109.5 . . ? H60L C605 H60M 109.5 . . ? N602 C606 H60N 109.4 . . ? N602 C606 H60O 109.5 . . ? H60N C606 H60O 109.5 . . ? N602 C606 H60P 109.5 . . ? H60N C606 H60P 109.5 . . ? H60O C606 H60P 109.5 . . ? N011 C011 C012 178.6(7) . . ? C011 C012 H01A 109.5 . . ? C011 C012 H01B 109.5 . . ? H01A C012 H01B 109.5 . . ? C011 C012 H01C 109.5 . . ? H01A C012 H01C 109.5 . . ? H01B C012 H01C 109.5 . . ? N021 C021 C022 176.9(12) . . ? C021 C022 H02A 109.5 . . ? C021 C022 H02B 109.5 . . ? H02A C022 H02B 109.5 . . ? C021 C022 H02C 109.5 . . ? H02A C022 H02C 109.5 . . ? H02B C022 H02C 109.5 . . ? N031 C031 C032 178.9(9) . . ? C031 C032 H03A 109.5 . . ? C031 C032 H03B 109.5 . . ? H03A C032 H03B 109.5 . . ? C031 C032 H03C 109.5 . . ? H03A C032 H03C 109.5 . . ? H03B C032 H03C 109.5 . . ? N041 C041 C042 178.7(8) . . ? C041 C042 H04A 109.5 . . ? C041 C042 H04B 109.5 . . ? H04A C042 H04B 109.5 . . ? C041 C042 H04C 109.5 . . ? H04A C042 H04C 109.5 . . ? H04B C042 H04C 109.5 . . ? N051 C051 C052 178.4(11) . . ? C051 C052 H05A 109.5 . . ? C051 C052 H05B 109.5 . . ? H05A C052 H05B 109.5 . . ? C051 C052 H05C 109.5 . . ? H05A C052 H05C 109.5 . . ? H05B C052 H05C 109.5 . . ? N061 C061 C062 178.5(11) . . ? C061 C062 H06A 109.5 . . ? C061 C062 H06B 109.5 . . ? H06A C062 H06B 109.5 . . ? C061 C062 H06C 109.5 . . ? H06A C062 H06C 109.5 . . ? H06B C062 H06C 109.5 . . ? N071 C071 C072 178.6(8) . . ? C071 C072 H07A 109.5 . . ? C071 C072 H07B 109.5 . . ? H07A C072 H07B 109.5 . . ? C071 C072 H07C 109.5 . . ? H07A C072 H07C 109.5 . . ? H07B C072 H07C 109.5 . . ? N081 C081 C082 173.4(14) . . ? C081 C082 H08A 109.5 . . ? C081 C082 H08B 109.5 . . ? H08A C082 H08B 109.5 . . ? C081 C082 H08C 109.5 . . ? H08A C082 H08C 109.5 . . ? H08B C082 H08C 109.5 . . ? N091 C091 C092 156.8(15) . . ? C091 C092 H09A 109.5 . . ? C091 C092 H09B 109.5 . . ? H09A C092 H09B 109.5 . . ? C091 C092 H09C 109.5 . . ? H09A C092 H09C 109.5 . . ? H09B C092 H09C 109.5 . . ? N0A1 C0A1 C0A2 144.8(12) . . ? C0A1 C0A2 H0A1 109.5 . . ? C0A1 C0A2 H0A2 109.5 . . ? H0A1 C0A2 H0A2 109.5 . . ? C0A1 C0A2 H0A3 109.5 . . ? H0A1 C0A2 H0A3 109.5 . . ? H0A2 C0A2 H0A3 109.5 . . ? N0B1 C0B1 C0B2 176.0(14) . . ? C0B1 C0B2 H0B1 109.5 . . ? C0B1 C0B2 H0B2 109.5 . . ? H0B1 C0B2 H0B2 109.5 . . ? C0B1 C0B2 H0B3 109.5 . . ? H0B1 C0B2 H0B3 109.5 . . ? H0B2 C0B2 H0B3 109.5 . . ? O0S S0S C01S 138.7(16) . . ? O0S S0S C02S 113.0(12) . . ? C01S S0S C02S 84.8(7) . . ? S0S C01S H01D 109.4 . . ? S0S C01S H01E 109.4 . . ? H01D C01S H01E 109.5 . . ? S0S C01S H01F 109.6 . . ? H01D C01S H01F 109.5 . . ? H01E C01S H01F 109.5 . . ? S0S C02S H02D 109.5 . . ? S0S C02S H02E 109.6 . . ? H02D C02S H02E 109.5 . . ? S0S C02S H02F 109.3 . . ? H02D C02S H02F 109.5 . . ? H02E C02S H02F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10 N0A1 0.95 2.56 3.405(13) 148 . O20 H20 N091 0.95 2.45 3.382(11) 165.8 . N101 H101 O0S 0.93 1.84 2.54(2) 130.5 . N101 H101 N102 0.93 2.38 2.876(8) 113.2 . N201 H201 O251 0.93 1.8 2.715(5) 167.5 . N301 H301 O151 0.93 1.81 2.710(6) 161.3 . N401 H401 O181 0.93 1.85 2.743(6) 159.7 . N501 H501 O281 0.93 1.81 2.708(6) 161.2 1_556 N601 H601 O201 0.93 2.04 2.877(7) 148.2 . N601 H601 N091 0.93 2.5 3.135(14) 125.7 . #===END # Attachment '- ucal8_2.cif' data_ucal8 _database_code_depnum_ccdc_archive 'CCDC 773079' #TrackingRef '- ucal8_2.cif' _audit_creation_date 2009-01-14T13:53:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C108 H149 N7 O17 S2 U3' _chemical_formula_moiety 'C92 H119 O17 S2 U3, C4 H12 N, 6(C2 H3 N) ' _chemical_formula_weight 2595.55 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.668(2) _cell_length_b 21.255(2) _cell_length_c 33.054(3) _cell_angle_alpha 90 _cell_angle_beta 100.644(2) _cell_angle_gamma 90 _cell_volume 11509(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 25.2 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_size_max .5 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.309 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .22 _exptl_absorpt_correction_T_max .55 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_unetI/netI 0.0532 _diffrn_reflns_number 110060 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 29.22 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.93 _reflns_number_total 29059 _reflns_number_gt 20917 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution xtal _computing_molecular_graphics ortep2 _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0643P)^2^+8.1349P] 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_number_reflns 29059 _refine_ls_number_parameters 1246 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1768 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.1 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 7.353 _refine_diff_density_min -2.5 _refine_diff_density_rms 0.236 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.663912(19) 0.798621(16) 0.338169(9) 0.02199(8) Uani 1 1 d . . . U2 U 0.810095(19) 0.816984(16) 0.244559(9) 0.02126(8) Uani 1 1 d . . . U3 U 0.74945(2) 0.673868(16) 0.287075(9) 0.02297(8) Uani 1 1 d . . . O0 O 0.7391(3) 0.7798(3) 0.29050(17) 0.0222(12) Uani 1 1 d . . . O1 O 0.6659(3) 0.7121(3) 0.33728(16) 0.0200(12) Uani 1 1 d . . . O2 O 0.8199(4) 0.7309(3) 0.23973(17) 0.0233(13) Uani 1 1 d . . . O3 O 0.6645(4) 0.8824(3) 0.33836(19) 0.0241(13) Uani 1 1 d . . . O4 O 0.7984(4) 0.8999(3) 0.25099(17) 0.0249(13) Uani 1 1 d . . . O5 O 0.6587(4) 0.6680(3) 0.24971(18) 0.0312(15) Uani 1 1 d . . . O6 O 0.8411(4) 0.6729(3) 0.3244(2) 0.0284(14) Uani 1 1 d . . . O11 O 0.5791(4) 0.8041(3) 0.26900(17) 0.0231(13) Uani 1 1 d . . . C11 C 0.5029(5) 0.8290(4) 0.2565(2) 0.0232(18) Uani 1 1 d . . . C12 C 0.4350(5) 0.7957(4) 0.2646(2) 0.0218(17) Uani 1 1 d . . . C13 C 0.3573(5) 0.8230(4) 0.2538(3) 0.0239(17) Uani 1 1 d . . . H13 H 0.3117 0.8017 0.2608 0.029 Uiso 1 1 calc R . . C14 C 0.3450(5) 0.8801(4) 0.2331(2) 0.0249(18) Uani 1 1 d . . . C141 C 0.2597(6) 0.9095(5) 0.2197(3) 0.032(2) Uani 1 1 d . . . C142 C 0.2610(7) 0.9790(5) 0.2330(3) 0.037(2) Uani 1 1 d . . . H14A H 0.3023 1.0018 0.2211 0.056 Uiso 1 1 calc R . . H14B H 0.2743 0.9817 0.2631 0.056 Uiso 1 1 calc R . . H14C H 0.2072 0.9978 0.2232 0.056 Uiso 1 1 calc R . . C143 C 0.1936(6) 0.8758(5) 0.2385(3) 0.038(2) Uani 1 1 d . . . H14D H 0.1418 0.8985 0.2311 0.057 Uiso 1 1 calc R . . H14E H 0.21 0.8747 0.2685 0.057 Uiso 1 1 calc R . . H14F H 0.1868 0.8327 0.2279 0.057 Uiso 1 1 calc R . . C144 C 0.2354(7) 0.9065(6) 0.1729(3) 0.046(3) Uani 1 1 d . . . H14G H 0.2791 0.9245 0.1603 0.07 Uiso 1 1 calc R . . H14H H 0.185 0.9305 0.164 0.07 Uiso 1 1 calc R . . H14I H 0.2265 0.8625 0.1642 0.07 Uiso 1 1 calc R . . C15 C 0.4130(5) 0.9096(5) 0.2232(3) 0.0268(19) Uani 1 1 d . . . H15 H 0.4056 0.948 0.2082 0.032 Uiso 1 1 calc R . . C16 C 0.4918(5) 0.8854(4) 0.2342(2) 0.0228(17) Uani 1 1 d . . . C1 C 0.5628(5) 0.9180(5) 0.2201(3) 0.0256(18) Uani 1 1 d . . . H1A H 0.5512 0.9635 0.2166 0.031 Uiso 1 1 calc R . . H1B H 0.6129 0.9129 0.2413 0.031 Uiso 1 1 calc R . . O21 O 0.5307(4) 0.8024(3) 0.34757(18) 0.0285(14) Uani 1 1 d . . . C21 C 0.4732(5) 0.7638(4) 0.3576(2) 0.0227(17) Uani 1 1 d . . . C22 C 0.4592(5) 0.7609(4) 0.3982(2) 0.0208(17) Uani 1 1 d . . . C23 C 0.4001(5) 0.7201(4) 0.4070(2) 0.0243(18) Uani 1 1 d . . . H23 H 0.3909 0.7182 0.4345 0.029 Uiso 1 1 calc R . . C24 C 0.3525(5) 0.6810(4) 0.3770(3) 0.0238(17) Uani 1 1 d . . . C241 C 0.2882(6) 0.6372(5) 0.3892(3) 0.030(2) Uani 1 1 d . . . C242 C 0.2485(9) 0.5955(7) 0.3539(4) 0.064(4) Uani 1 1 d . . . H24A H 0.2163 0.6215 0.3323 0.095 Uiso 1 1 calc R . . H24B H 0.2127 0.565 0.3639 0.095 Uiso 1 1 calc R . . H24C H 0.2909 0.5732 0.3426 0.095 Uiso 1 1 calc R . . C243 C 0.2207(7) 0.6755(6) 0.4027(4) 0.049(3) Uani 1 1 d . . . H24D H 0.244 0.7015 0.4265 0.074 Uiso 1 1 calc R . . H24E H 0.1798 0.647 0.4104 0.074 Uiso 1 1 calc R . . H24F H 0.195 0.7027 0.3801 0.074 Uiso 1 1 calc R . . C244 C 0.3272(8) 0.5950(6) 0.4249(4) 0.054(3) Uani 1 1 d . . . H24G H 0.3639 0.5649 0.4152 0.082 Uiso 1 1 calc R . . H24H H 0.2844 0.5721 0.4355 0.082 Uiso 1 1 calc R . . H24I H 0.3583 0.6209 0.4469 0.082 Uiso 1 1 calc R . . C25 C 0.3681(5) 0.6862(4) 0.3369(3) 0.0266(19) Uani 1 1 d . . . H25 H 0.3372 0.6613 0.3158 0.032 Uiso 1 1 calc R . . C26 C 0.4267(5) 0.7263(4) 0.3269(3) 0.0221(17) Uani 1 1 d . . . C2 C 0.4442(5) 0.7311(4) 0.2839(2) 0.0233(17) Uani 1 1 d . . . H2A H 0.4073 0.7019 0.266 0.028 Uiso 1 1 calc R . . H2B H 0.5008 0.7165 0.2844 0.028 Uiso 1 1 calc R . . O31 O 0.6703(4) 0.8010(3) 0.40947(19) 0.0329(16) Uani 1 1 d . . . C31 C 0.6581(5) 0.7584(4) 0.4387(2) 0.0257(19) Uani 1 1 d . . . C32 C 0.7191(5) 0.7166(4) 0.4540(2) 0.0207(17) Uani 1 1 d . . . C33 C 0.7094(5) 0.6738(4) 0.4840(3) 0.0256(18) Uani 1 1 d . . . H33 H 0.753 0.6461 0.4944 0.031 Uiso 1 1 calc R . . C34 C 0.6377(6) 0.6701(4) 0.4995(3) 0.0268(19) Uani 1 1 d . . . C341 C 0.6234(7) 0.6226(6) 0.5321(3) 0.040(3) Uani 1 1 d . . . C342 C 0.5646(9) 0.5721(7) 0.5117(5) 0.067(4) Uani 1 1 d . . . H34A H 0.5138 0.5919 0.4979 0.101 Uiso 1 1 calc R . . H34B H 0.5527 0.5428 0.5327 0.101 Uiso 1 1 calc R . . H34C H 0.5895 0.5491 0.4915 0.101 Uiso 1 1 calc R . . C343 C 0.7024(8) 0.5885(6) 0.5523(4) 0.053(3) Uani 1 1 d . . . H34D H 0.7266 0.5675 0.5311 0.08 Uiso 1 1 calc R . . H34E H 0.6896 0.5572 0.5719 0.08 Uiso 1 1 calc R . . H34F H 0.7412 0.6192 0.5669 0.08 Uiso 1 1 calc R . . C344 C 0.5930(12) 0.6568(7) 0.5672(4) 0.083(6) Uani 1 1 d . . . H34G H 0.6374 0.6822 0.5827 0.124 Uiso 1 1 calc R . . H34H H 0.575 0.6258 0.5856 0.124 Uiso 1 1 calc R . . H34I H 0.5471 0.6842 0.5558 0.124 Uiso 1 1 calc R . . C35 C 0.5747(6) 0.7132(5) 0.4825(3) 0.030(2) Uani 1 1 d . . . H35 H 0.5247 0.7123 0.4923 0.037 Uiso 1 1 calc R . . C36 C 0.5835(5) 0.7559(4) 0.4523(2) 0.0235(18) Uani 1 1 d . . . C3 C 0.5132(5) 0.7972(5) 0.4327(3) 0.028(2) Uani 1 1 d . . . H3A H 0.5343 0.8358 0.4215 0.034 Uiso 1 1 calc R . . H3B H 0.4808 0.8099 0.4537 0.034 Uiso 1 1 calc R . . O41 O 0.8054(3) 0.8035(3) 0.36970(16) 0.0233(13) Uani 1 1 d . . . C41 C 0.8448(5) 0.8205(5) 0.4077(2) 0.0227(17) Uani 1 1 d . . . C42 C 0.8909(5) 0.8768(4) 0.4132(3) 0.0237(18) Uani 1 1 d . . . C43 C 0.9306(5) 0.8938(4) 0.4521(3) 0.0263(19) Uani 1 1 d . . . H43 H 0.9607 0.932 0.4553 0.032 Uiso 1 1 calc R . . C44 C 0.9284(6) 0.8564(5) 0.4873(3) 0.0278(19) Uani 1 1 d . . . C441 C 0.9741(7) 0.8773(5) 0.5297(3) 0.036(2) Uani 1 1 d . . . C442 C 0.9338(9) 0.9365(6) 0.5423(4) 0.057(3) Uani 1 1 d . . . H44A H 0.8764 0.9278 0.5431 0.086 Uiso 1 1 calc R . . H44B H 0.9372 0.97 0.5223 0.086 Uiso 1 1 calc R . . H44C H 0.9619 0.95 0.5696 0.086 Uiso 1 1 calc R . . C443 C 1.0645(7) 0.8914(8) 0.5278(4) 0.061(4) Uani 1 1 d . . . H44D H 1.0919 0.9086 0.5543 0.091 Uiso 1 1 calc R . . H44E H 1.0671 0.9221 0.506 0.091 Uiso 1 1 calc R . . H44F H 1.0917 0.8524 0.5221 0.091 Uiso 1 1 calc R . . C444 C 0.9745(10) 0.8268(6) 0.5622(3) 0.061(4) Uani 1 1 d . . . H44G H 1.0088 0.8406 0.5881 0.092 Uiso 1 1 calc R . . H44H H 0.9964 0.7877 0.553 0.092 Uiso 1 1 calc R . . H44I H 0.9187 0.8197 0.5666 0.092 Uiso 1 1 calc R . . C45 C 0.8841(5) 0.8007(5) 0.4806(2) 0.0248(18) Uani 1 1 d . . . H45 H 0.8819 0.7742 0.5035 0.03 Uiso 1 1 calc R . . C46 C 0.8424(5) 0.7817(4) 0.4418(2) 0.0208(17) Uani 1 1 d . . . C4 C 0.7995(5) 0.7184(4) 0.4372(3) 0.0228(17) Uani 1 1 d . . . H4A H 0.837 0.6862 0.4517 0.027 Uiso 1 1 calc R . . H4B H 0.7876 0.7071 0.4076 0.027 Uiso 1 1 calc R . . O51 O 0.8928(3) 0.8143(3) 0.31658(17) 0.0238(13) Uani 1 1 d . . . C51 C 0.9687(5) 0.8379(4) 0.3331(2) 0.0216(17) Uani 1 1 d . . . C52 C 1.0388(5) 0.8083(4) 0.3237(2) 0.0241(18) Uani 1 1 d . . . C53 C 1.1155(5) 0.8336(5) 0.3400(3) 0.0260(19) Uani 1 1 d . . . H53 H 1.1626 0.8141 0.3332 0.031 Uiso 1 1 calc R . . C54 C 1.1258(5) 0.8855(5) 0.3656(3) 0.0262(19) Uani 1 1 d . . . C541 C 1.2096(6) 0.9130(5) 0.3840(3) 0.035(2) Uani 1 1 d . . . C542 C 1.2192(8) 0.9772(6) 0.3665(4) 0.053(3) Uani 1 1 d . . . H54A H 1.2742 0.9931 0.3772 0.079 Uiso 1 1 calc R . . H54B H 1.1787 1.0059 0.3745 0.079 Uiso 1 1 calc R . . H54C H 1.2108 0.9746 0.3364 0.079 Uiso 1 1 calc R . . C543 C 1.2790(6) 0.8703(7) 0.3766(4) 0.054(3) Uani 1 1 d . . . H54D H 1.2777 0.8664 0.3469 0.081 Uiso 1 1 calc R . . H54E H 1.2726 0.8285 0.3882 0.081 Uiso 1 1 calc R . . H54F H 1.3314 0.8884 0.3898 0.081 Uiso 1 1 calc R . . C545 C 1.2160(7) 0.9195(7) 0.4303(3) 0.049(3) Uani 1 1 d . . . H54G H 1.2686 0.9387 0.4422 0.073 Uiso 1 1 calc R . . H54H H 1.212 0.8779 0.4425 0.073 Uiso 1 1 calc R . . H54I H 1.1716 0.9463 0.436 0.073 Uiso 1 1 calc R . . C55 C 1.0549(5) 0.9126(4) 0.3753(3) 0.0260(19) Uani 1 1 d . . . H55 H 1.0603 0.9483 0.3929 0.031 Uiso 1 1 calc R . . C56 C 0.9765(5) 0.8893(4) 0.3600(2) 0.0234(18) Uani 1 1 d . . . C5 C 0.9033(5) 0.9152(4) 0.3759(2) 0.0233(18) Uani 1 1 d . . . H5A H 0.854 0.9126 0.3541 0.028 Uiso 1 1 calc R . . H5B H 0.9127 0.9599 0.3838 0.028 Uiso 1 1 calc R . . O61 O 0.9447(4) 0.8302(3) 0.24137(17) 0.0246(13) Uani 1 1 d . . . C61 C 1.0005(5) 0.7919(4) 0.2283(2) 0.0212(17) Uani 1 1 d . . . C62 C 1.0130(5) 0.7945(4) 0.1877(2) 0.0219(17) Uani 1 1 d . . . C63 C 1.0714(5) 0.7544(5) 0.1761(3) 0.029(2) Uani 1 1 d . . . H63 H 1.08 0.7563 0.1485 0.035 Uiso 1 1 calc R . . C64 C 1.1166(6) 0.7126(5) 0.2024(3) 0.029(2) Uani 1 1 d . . . C641 C 1.1757(7) 0.6665(6) 0.1874(3) 0.043(3) Uani 1 1 d . . . C642 C 1.1271(16) 0.6156(13) 0.1665(8) 0.141(9) Uiso 1 1 d . . . H64A H 1.0713 0.6305 0.1565 0.212 Uiso 1 1 calc R . . H64B H 1.1261 0.5806 0.1856 0.212 Uiso 1 1 calc R . . H64C H 1.1511 0.6014 0.1431 0.212 Uiso 1 1 calc R . . C643 C 1.2207(15) 0.6971(12) 0.1583(8) 0.176(15) Uani 1 1 d . . . H64D H 1.2677 0.6711 0.1551 0.253 Uiso 1 1 calc R . . H64E H 1.2397 0.7386 0.169 0.253 Uiso 1 1 calc R . . H64F H 1.1845 0.702 0.1316 0.253 Uiso 1 1 calc R . . C644 C 1.2391(9) 0.6425(8) 0.2206(4) 0.074(5) Uani 1 1 d . . . H64G H 1.2781 0.617 0.2088 0.111 Uiso 1 1 calc R . . H64H H 1.2138 0.6164 0.2392 0.111 Uiso 1 1 calc R . . H64I H 1.2677 0.6778 0.2359 0.111 Uiso 1 1 calc R . . C65 C 1.1045(6) 0.7120(5) 0.2433(3) 0.034(2) Uani 1 1 d . . . H65 H 1.136 0.6842 0.2625 0.041 Uiso 1 1 calc R . . C66 C 1.0475(5) 0.7512(5) 0.2565(3) 0.0253(18) Uani 1 1 d . . . C6 C 1.0315(6) 0.7469(5) 0.3000(3) 0.0260(18) Uani 1 1 d . . . H6A H 0.9758 0.73 0.299 0.031 Uiso 1 1 calc R . . H6B H 1.0704 0.7164 0.3155 0.031 Uiso 1 1 calc R . . O71 O 0.8022(3) 0.8257(3) 0.17803(16) 0.0225(12) Uani 1 1 d . . . C71 C 0.8157(5) 0.7904(4) 0.1462(2) 0.0238(18) Uani 1 1 d . . . C72 C 0.7535(5) 0.7500(5) 0.1255(3) 0.0273(19) Uani 1 1 d . . . C73 C 0.7705(6) 0.7132(5) 0.0929(3) 0.032(2) Uani 1 1 d . . . H73 H 0.729 0.686 0.0793 0.038 Uiso 1 1 calc R . . C74 C 0.8443(6) 0.7143(5) 0.0794(3) 0.031(2) Uani 1 1 d . . . C741 C 0.8605(7) 0.6766(5) 0.0432(3) 0.036(2) Uani 1 1 d . . . C742 C 0.8298(8) 0.7129(6) 0.0037(3) 0.047(3) Uani 1 1 d . . . H74A H 0.7709 0.7201 0.0008 0.071 Uiso 1 1 calc R . . H74B H 0.8407 0.6887 -0.0199 0.071 Uiso 1 1 calc R . . H74C H 0.858 0.7535 0.0047 0.071 Uiso 1 1 calc R . . C743 C 0.8137(10) 0.6124(6) 0.0405(4) 0.059(4) Uani 1 1 d . . . H74D H 0.827 0.5907 0.0671 0.089 Uiso 1 1 calc R . . H74E H 0.8301 0.5862 0.0191 0.089 Uiso 1 1 calc R . . H74F H 0.7548 0.6202 0.0338 0.089 Uiso 1 1 calc R . . C744 C 0.9519(7) 0.6627(7) 0.0453(4) 0.061(4) Uani 1 1 d . . . H74G H 0.9817 0.7023 0.045 0.092 Uiso 1 1 calc R . . H74H H 0.9589 0.637 0.0216 0.092 Uiso 1 1 calc R . . H74I H 0.9732 0.6398 0.0708 0.092 Uiso 1 1 calc R . . C75 C 0.9035(6) 0.7564(5) 0.1001(3) 0.030(2) Uani 1 1 d . . . H75 H 0.9548 0.7587 0.0916 0.036 Uiso 1 1 calc R . . C76 C 0.8904(5) 0.7945(5) 0.1324(2) 0.0250(18) Uani 1 1 d . . . C7 C 0.9591(5) 0.8351(4) 0.1553(2) 0.0203(16) Uiso 1 1 d . . . H7A H 0.9362 0.8707 0.1688 0.024 Uiso 1 1 calc R . . H7B H 0.9919 0.8524 0.1358 0.024 Uiso 1 1 calc R . . O81 O 0.6641(3) 0.8110(3) 0.21523(17) 0.0251(13) Uani 1 1 d . . . C81 C 0.6238(5) 0.8360(4) 0.1791(2) 0.0214(17) Uani 1 1 d . . . C82 C 0.5762(5) 0.8901(4) 0.1797(3) 0.0245(18) Uani 1 1 d . . . C83 C 0.5344(5) 0.9141(5) 0.1421(3) 0.0270(19) Uani 1 1 d . . . H83 H 0.5015 0.9505 0.1425 0.032 Uiso 1 1 calc R . . C84 C 0.5393(5) 0.8868(5) 0.1043(3) 0.027(2) Uani 1 1 d . . . C841 C 0.4908(6) 0.9120(5) 0.0634(3) 0.035(2) Uani 1 1 d . . . C842 C 0.4348(7) 0.8605(6) 0.0430(4) 0.053(3) Uani 1 1 d . . . H84A H 0.3928 0.8519 0.0595 0.079 Uiso 1 1 calc R . . H84B H 0.4667 0.8222 0.0411 0.079 Uiso 1 1 calc R . . H84C H 0.4088 0.874 0.0154 0.079 Uiso 1 1 calc R . . C843 C 0.4416(7) 0.9685(6) 0.0684(3) 0.050(3) Uani 1 1 d . . . H84D H 0.4031 0.9586 0.0866 0.075 Uiso 1 1 calc R . . H84E H 0.4112 0.9816 0.0414 0.075 Uiso 1 1 calc R . . H84F H 0.4778 1.0027 0.0804 0.075 Uiso 1 1 calc R . . C844 C 0.5508(8) 0.9280(6) 0.0343(3) 0.048(3) Uani 1 1 d . . . H84G H 0.5199 0.9398 0.0072 0.072 Uiso 1 1 calc R . . H84H H 0.5848 0.8912 0.0315 0.072 Uiso 1 1 calc R . . H84I H 0.5857 0.9632 0.0458 0.072 Uiso 1 1 calc R . . C85 C 0.5880(6) 0.8334(5) 0.1052(3) 0.030(2) Uani 1 1 d . . . H85 H 0.593 0.8142 0.0798 0.035 Uiso 1 1 calc R . . C86 C 0.6298(5) 0.8070(5) 0.1416(3) 0.0245(18) Uani 1 1 d . . . C8 C 0.6741(5) 0.7459(5) 0.1411(3) 0.0281(19) Uani 1 1 d . . . H8A H 0.6377 0.7158 0.1237 0.034 Uiso 1 1 calc R . . H8B H 0.6854 0.7288 0.1695 0.034 Uiso 1 1 calc R . . O10 O 0.7200(4) 0.5750(3) 0.3174(2) 0.0301(14) Uani 1 1 d . . . S10 S 0.79155(18) 0.53165(13) 0.33742(9) 0.0411(6) Uani 1 1 d . . . C101 C 0.7400(8) 0.4622(5) 0.3484(4) 0.048(3) Uani 1 1 d . . . H10A H 0.6922 0.4737 0.3602 0.071 Uiso 1 1 calc R . . H10B H 0.777 0.4363 0.3681 0.071 Uiso 1 1 calc R . . H10C H 0.7223 0.4384 0.3229 0.071 Uiso 1 1 calc R . . C102 C 0.8231(10) 0.5615(6) 0.3877(4) 0.065(4) Uani 1 1 d . . . H10D H 0.845 0.6041 0.3862 0.097 Uiso 1 1 calc R . . H10E H 0.8655 0.5342 0.403 0.097 Uiso 1 1 calc R . . H10F H 0.7764 0.5629 0.4018 0.097 Uiso 1 1 calc R . . O20 O 0.8095(5) 0.5989(4) 0.2478(3) 0.048(2) Uani 1 1 d . . . S20 S 0.7958(2) 0.59596(18) 0.20099(9) 0.0599(9) Uani 1 1 d . . . C201 C 0.8893(12) 0.6254(8) 0.1864(4) 0.086(6) Uani 1 1 d . . . H20A H 0.8941 0.6707 0.1918 0.129 Uiso 1 1 calc R . . H20B H 0.8875 0.6177 0.157 0.129 Uiso 1 1 calc R . . H20C H 0.9364 0.6036 0.2025 0.129 Uiso 1 1 calc R . . C202 C 0.8077(11) 0.5144(7) 0.1913(5) 0.077(5) Uani 1 1 d . . . H20D H 0.8586 0.4992 0.2082 0.115 Uiso 1 1 calc R . . H20E H 0.8096 0.5082 0.1622 0.115 Uiso 1 1 calc R . . H20F H 0.7615 0.491 0.1983 0.115 Uiso 1 1 calc R . . N30 N 0.9877(6) 1.0124(5) 0.2555(3) 0.048(3) Uani 1 1 d D . . C301 C 1.0609(8) 1.0033(10) 0.2846(5) 0.099(7) Uani 1 1 d D . . H30A H 1.0589 0.9625 0.2982 0.149 Uiso 1 1 calc R . . H30B H 1.0667 1.0369 0.3052 0.149 Uiso 1 1 calc R . . H30C H 1.1077 1.0042 0.2705 0.149 Uiso 1 1 calc R . . C302 C 0.9698(9) 0.9640(8) 0.2253(4) 0.074(5) Uani 1 1 d D . . H30D H 1.0093 0.9657 0.2068 0.111 Uiso 1 1 calc R . . H30E H 0.9146 0.9702 0.2095 0.111 Uiso 1 1 calc R . . H30F H 0.9731 0.9229 0.239 0.111 Uiso 1 1 calc R . . C303 C 0.9992(9) 1.0772(7) 0.2347(4) 0.070(4) Uani 1 1 d D . . H30G H 1.015 1.1093 0.256 0.105 Uiso 1 1 calc R . . H30H H 0.9478 1.0895 0.2169 0.105 Uiso 1 1 calc R . . H30I H 1.042 1.0734 0.2181 0.105 Uiso 1 1 calc R . . C304 C 0.9183(7) 1.0237(6) 0.2792(4) 0.053(3) Uani 1 1 d D . . H30J H 0.9079 0.985 0.2936 0.079 Uiso 1 1 calc R . . H30K H 0.8688 1.0358 0.2599 0.079 Uiso 1 1 calc R . . H30L H 0.9337 1.0575 0.2993 0.079 Uiso 1 1 calc R . . N01 N 0.7318(16) 0.4964(9) 0.4597(7) 0.148(9) Uani 1 1 d . . . C011 C 0.7225(11) 0.4436(9) 0.4588(5) 0.074(5) Uani 1 1 d . . . C012 C 0.7181(15) 0.3761(9) 0.4579(5) 0.108(8) Uani 1 1 d . . . H01A H 0.7501 0.3591 0.4835 0.162 Uiso 1 1 calc R . . H01B H 0.7402 0.3602 0.4344 0.162 Uiso 1 1 calc R . . H01C H 0.6611 0.3629 0.4554 0.162 Uiso 1 1 calc R . . N02 N 0.6129(13) 0.7803(11) -0.0014(6) 0.137(8) Uani 1 1 d . . . C021 C 0.5792(12) 0.7682(11) -0.0348(6) 0.096(6) Uani 1 1 d . . . C022 C 0.5467(9) 0.7480(9) -0.0728(5) 0.076(5) Uani 1 1 d . . . H02A H 0.5904 0.7343 -0.087 0.114 Uiso 1 1 calc R . . H02B H 0.516 0.7823 -0.0884 0.114 Uiso 1 1 calc R . . H02C H 0.5099 0.7126 -0.0709 0.114 Uiso 1 1 calc R . . N03 N 0.9497(11) 0.8469(9) 0.6718(5) 0.107(6) Uani 1 1 d . . . C031 C 0.9383(11) 0.7947(10) 0.6644(4) 0.078(5) Uani 1 1 d . . . C032 C 0.9186(9) 0.7318(7) 0.6522(4) 0.063(4) Uani 1 1 d . . . H03A H 0.9166 0.7061 0.6766 0.094 Uiso 1 1 calc R . . H03B H 0.9602 0.7151 0.6377 0.094 Uiso 1 1 calc R . . H03C H 0.8652 0.7309 0.6338 0.094 Uiso 1 1 calc R . . N04 N 0.496(2) 0.5040(10) 0.3748(9) 0.221(17) Uani 1 1 d . . . C041 C 0.5298(13) 0.5481(8) 0.3832(5) 0.091(6) Uani 1 1 d . . . C042 C 0.5687(8) 0.6067(5) 0.3915(4) 0.046(3) Uani 1 1 d . . . H04A H 0.6101 0.6118 0.3742 0.069 Uiso 1 1 calc R . . H04B H 0.5949 0.6086 0.4206 0.069 Uiso 1 1 calc R . . H04C H 0.5282 0.6405 0.3855 0.069 Uiso 1 1 calc R . . N05 N 0.649(2) 0.9330(13) 0.5442(13) 0.29(2) Uiso 1 1 d D . . C051 C 0.6812(17) 0.8798(11) 0.5431(9) 0.140(9) Uiso 1 1 d D . . C052 C 0.7224(15) 0.8195(11) 0.5453(8) 0.127(8) Uiso 1 1 d D . . H05A H 0.6846 0.7863 0.5503 0.19 Uiso 1 1 calc R . . H05B H 0.7697 0.8201 0.5679 0.19 Uiso 1 1 calc R . . H05C H 0.7408 0.8114 0.5193 0.19 Uiso 1 1 calc R . . N06 N 0.4552(11) 0.9398(9) 0.3309(5) 0.046(5) Uiso 0.5 1 d PD . . C061 C 0.5039(14) 0.9635(13) 0.3602(7) 0.060(7) Uiso 0.5 1 d PD . . C062 C 0.5634(16) 0.9922(15) 0.3924(8) 0.073(8) Uiso 0.5 1 d PD . . H06A H 0.5904 1.027 0.3809 0.109 Uiso 0.5 1 calc PR . . H06B H 0.6042 0.9608 0.4041 0.109 Uiso 0.5 1 calc PR . . H06C H 0.5358 1.0081 0.4141 0.109 Uiso 0.5 1 calc PR . . N07 N 1.038(2) 0.567(2) 0.2627(8) 0.138(14) Uiso 0.5 1 d PD . . C071 C 1.021(2) 0.5827(15) 0.2969(7) 0.080(9) Uiso 0.5 1 d PD . . C072 C 1.0136(18) 0.5925(14) 0.3395(7) 0.064(7) Uiso 0.5 1 d PD . . H07A H 1.0677 0.5904 0.3572 0.096 Uiso 0.5 1 calc PR . . H07B H 0.9785 0.5597 0.3478 0.096 Uiso 0.5 1 calc PR . . H07C H 0.9894 0.6339 0.3424 0.096 Uiso 0.5 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 0.02283(15) 0.02749(17) 0.01597(14) 0.00069(12) 0.00440(11) -0.00046(13) U2 0.02339(15) 0.02714(17) 0.01298(13) 0.00280(11) 0.00262(11) -0.00030(12) U3 0.02520(16) 0.02591(17) 0.01802(15) 0.00212(12) 0.00457(12) -0.00055(13) O0 0.015(3) 0.033(3) 0.019(3) 0.007(2) 0.004(2) -0.003(2) O1 0.021(3) 0.029(3) 0.010(2) 0.001(2) 0.003(2) -0.003(2) O2 0.025(3) 0.029(3) 0.015(3) 0.006(2) 0.002(2) -0.002(3) O3 0.027(3) 0.015(3) 0.033(3) -0.002(2) 0.012(3) 0.001(2) O4 0.032(3) 0.029(3) 0.013(3) -0.002(2) 0.002(2) -0.005(3) O5 0.029(3) 0.047(4) 0.016(3) -0.001(3) 0.002(2) -0.006(3) O6 0.025(3) 0.031(4) 0.029(3) 0.008(3) 0.003(3) -0.002(3) O11 0.023(3) 0.032(3) 0.014(3) 0.007(2) 0.001(2) 0.003(3) C11 0.025(4) 0.033(5) 0.014(4) 0.005(3) 0.008(3) 0.003(4) C12 0.021(4) 0.033(5) 0.012(3) 0.001(3) 0.005(3) 0.005(4) C13 0.021(4) 0.032(5) 0.019(4) 0.002(3) 0.005(3) 0.003(4) C14 0.024(4) 0.034(5) 0.015(4) 0.003(3) -0.001(3) 0.008(4) C141 0.029(5) 0.041(6) 0.023(4) 0.002(4) 0.000(4) 0.010(4) C142 0.041(6) 0.036(6) 0.036(5) 0.003(4) 0.007(4) 0.006(5) C143 0.024(5) 0.045(6) 0.044(6) 0.001(5) 0.003(4) 0.008(4) C144 0.034(6) 0.070(8) 0.029(5) -0.006(5) -0.009(4) 0.013(5) C15 0.025(4) 0.031(5) 0.024(4) 0.003(4) 0.002(3) 0.006(4) C16 0.020(4) 0.035(5) 0.013(4) 0.002(3) 0.002(3) 0.000(4) C1 0.022(4) 0.032(5) 0.022(4) 0.006(4) 0.002(3) 0.002(4) O21 0.029(3) 0.040(4) 0.018(3) 0.000(3) 0.009(2) -0.010(3) C21 0.029(4) 0.028(5) 0.011(4) 0.003(3) 0.006(3) 0.004(4) C22 0.022(4) 0.023(4) 0.017(4) 0.005(3) 0.004(3) 0.008(3) C23 0.029(4) 0.035(5) 0.012(4) 0.002(3) 0.012(3) -0.001(4) C24 0.024(4) 0.028(5) 0.020(4) 0.006(3) 0.008(3) 0.002(4) C241 0.029(5) 0.039(6) 0.024(4) 0.007(4) 0.006(4) -0.007(4) C242 0.076(9) 0.067(9) 0.054(8) -0.019(7) 0.029(7) -0.043(8) C243 0.033(6) 0.056(8) 0.061(8) -0.001(6) 0.017(5) -0.007(5) C244 0.051(7) 0.058(8) 0.054(7) 0.028(6) 0.011(6) -0.012(6) C25 0.027(4) 0.032(5) 0.021(4) 0.004(4) 0.004(3) 0.005(4) C26 0.021(4) 0.024(4) 0.020(4) 0.006(3) 0.000(3) 0.007(3) C2 0.025(4) 0.027(5) 0.017(4) 0.002(3) 0.001(3) 0.002(3) O31 0.025(3) 0.053(4) 0.023(3) 0.019(3) 0.009(3) 0.011(3) C31 0.030(5) 0.034(5) 0.012(4) 0.007(3) 0.000(3) -0.005(4) C32 0.023(4) 0.034(5) 0.006(3) -0.002(3) 0.003(3) 0.001(3) C33 0.026(4) 0.028(5) 0.022(4) 0.006(3) 0.001(3) 0.004(4) C34 0.031(5) 0.032(5) 0.018(4) 0.001(3) 0.006(3) -0.005(4) C341 0.041(6) 0.055(7) 0.027(5) 0.016(5) 0.014(4) -0.002(5) C342 0.060(8) 0.071(10) 0.068(9) 0.030(8) 0.004(7) -0.024(7) C343 0.061(8) 0.059(8) 0.041(6) 0.022(6) 0.015(6) 0.005(6) C344 0.140(15) 0.073(10) 0.057(8) 0.039(8) 0.073(10) 0.045(10) C35 0.037(5) 0.038(6) 0.017(4) 0.005(4) 0.008(4) -0.001(4) C36 0.023(4) 0.033(5) 0.014(4) -0.002(3) 0.001(3) 0.005(4) C3 0.009(3) 0.061(6) 0.016(4) -0.003(4) 0.005(3) -0.007(4) O41 0.019(3) 0.039(4) 0.011(2) 0.000(2) 0.002(2) -0.005(3) C41 0.015(4) 0.041(5) 0.011(3) 0.000(3) 0.001(3) 0.002(4) C42 0.018(4) 0.036(5) 0.018(4) 0.004(3) 0.008(3) 0.006(4) C43 0.027(4) 0.030(5) 0.021(4) -0.001(4) 0.002(3) 0.000(4) C44 0.033(5) 0.038(5) 0.012(4) -0.001(3) 0.002(3) 0.002(4) C441 0.044(6) 0.043(6) 0.018(4) -0.001(4) -0.001(4) -0.007(5) C442 0.074(9) 0.060(8) 0.035(6) -0.021(6) 0.002(6) -0.001(7) C443 0.043(7) 0.096(11) 0.036(6) 0.001(7) -0.010(5) -0.017(7) C444 0.094(11) 0.058(8) 0.021(5) 0.007(5) -0.017(6) -0.025(7) C45 0.025(4) 0.038(5) 0.012(4) 0.003(3) 0.005(3) 0.002(4) C46 0.017(4) 0.032(5) 0.012(3) 0.001(3) 0.001(3) 0.001(3) C4 0.020(4) 0.033(5) 0.016(4) 0.001(3) 0.004(3) 0.006(3) O51 0.019(3) 0.041(4) 0.011(2) 0.002(2) 0.001(2) -0.001(3) C51 0.018(4) 0.032(5) 0.014(4) 0.007(3) -0.001(3) -0.004(3) C52 0.023(4) 0.036(5) 0.014(4) 0.002(3) 0.006(3) 0.000(4) C53 0.017(4) 0.042(6) 0.019(4) 0.006(4) 0.004(3) 0.003(4) C54 0.019(4) 0.043(6) 0.017(4) 0.008(4) 0.004(3) -0.003(4) C541 0.021(4) 0.050(6) 0.031(5) 0.001(4) 0.001(4) -0.008(4) C542 0.045(7) 0.060(8) 0.052(7) 0.011(6) 0.003(6) -0.022(6) C543 0.020(5) 0.068(9) 0.072(9) -0.012(7) 0.002(5) -0.004(5) C545 0.042(6) 0.073(9) 0.028(5) 0.000(5) -0.004(5) -0.017(6) C55 0.030(5) 0.032(5) 0.014(4) 0.002(3) -0.001(3) -0.006(4) C56 0.024(4) 0.032(5) 0.015(4) 0.006(3) 0.006(3) -0.001(4) C5 0.021(4) 0.034(5) 0.016(4) 0.002(3) 0.005(3) 0.002(4) O61 0.026(3) 0.034(4) 0.015(3) 0.004(2) 0.007(2) 0.002(3) C61 0.016(4) 0.029(5) 0.019(4) -0.003(3) 0.003(3) -0.003(3) C62 0.020(4) 0.031(5) 0.016(4) -0.003(3) 0.007(3) -0.003(3) C63 0.023(4) 0.043(6) 0.021(4) -0.002(4) 0.006(3) 0.005(4) C64 0.029(5) 0.035(5) 0.024(4) -0.006(4) 0.007(4) 0.004(4) C641 0.038(6) 0.059(8) 0.030(5) -0.012(5) 0.004(4) 0.015(5) C643 0.20(2) 0.19(2) 0.17(2) 0.100(19) 0.12(2) 0.12(2) C644 0.071(9) 0.106(13) 0.044(7) -0.005(8) 0.008(7) 0.060(9) C65 0.034(5) 0.044(6) 0.022(4) 0.001(4) 0.000(4) 0.005(4) C66 0.023(4) 0.037(5) 0.016(4) -0.002(3) 0.003(3) -0.002(4) C6 0.026(4) 0.034(5) 0.018(4) 0.002(4) 0.006(3) 0.001(4) O71 0.021(3) 0.035(3) 0.011(3) -0.001(2) 0.003(2) -0.002(3) C71 0.026(4) 0.033(5) 0.010(3) 0.004(3) 0.000(3) 0.001(4) C72 0.023(4) 0.035(5) 0.023(4) 0.004(4) 0.000(3) 0.007(4) C73 0.027(5) 0.038(6) 0.027(5) -0.004(4) -0.004(4) 0.005(4) C74 0.033(5) 0.042(6) 0.016(4) -0.005(4) 0.001(4) 0.000(4) C741 0.045(6) 0.044(6) 0.018(4) -0.009(4) 0.003(4) -0.005(5) C742 0.055(7) 0.072(8) 0.016(4) -0.004(5) 0.011(5) 0.003(6) C743 0.099(11) 0.050(8) 0.033(6) -0.013(5) 0.024(7) -0.012(7) C744 0.030(6) 0.085(10) 0.062(8) -0.049(7) -0.008(5) 0.017(6) C75 0.029(5) 0.045(6) 0.015(4) -0.002(4) 0.004(3) 0.002(4) C76 0.019(4) 0.041(5) 0.015(4) 0.004(4) 0.003(3) 0.006(4) O81 0.017(3) 0.043(4) 0.013(3) 0.009(2) -0.002(2) 0.002(3) C81 0.017(4) 0.030(5) 0.017(4) 0.008(3) 0.002(3) -0.001(3) C82 0.023(4) 0.033(5) 0.018(4) 0.010(3) 0.004(3) -0.002(4) C83 0.023(4) 0.031(5) 0.026(4) 0.009(4) 0.001(3) -0.002(4) C84 0.022(4) 0.043(6) 0.014(4) 0.011(4) -0.005(3) -0.006(4) C841 0.041(5) 0.044(6) 0.015(4) 0.012(4) -0.006(4) -0.005(5) C842 0.044(7) 0.062(8) 0.040(6) 0.016(6) -0.024(5) -0.009(6) C843 0.054(7) 0.061(8) 0.028(5) 0.016(5) -0.011(5) 0.001(6) C844 0.057(7) 0.058(8) 0.025(5) 0.010(5) -0.001(5) -0.006(6) C85 0.028(5) 0.045(6) 0.013(4) 0.000(4) -0.001(3) -0.011(4) C86 0.012(3) 0.043(6) 0.020(4) 0.000(4) 0.006(3) -0.005(3) C8 0.028(5) 0.039(5) 0.016(4) 0.004(4) 0.000(3) 0.000(4) O10 0.040(4) 0.025(3) 0.028(3) 0.006(3) 0.012(3) 0.001(3) S10 0.0471(15) 0.0388(15) 0.0405(14) 0.0124(12) 0.0164(12) 0.0083(12) C101 0.078(9) 0.031(6) 0.037(6) 0.006(5) 0.020(6) -0.003(6) C102 0.090(11) 0.045(7) 0.046(7) 0.015(6) -0.021(7) -0.002(7) O20 0.066(5) 0.035(4) 0.052(5) -0.004(4) 0.034(4) -0.007(4) S20 0.084(2) 0.065(2) 0.0326(15) -0.0037(14) 0.0145(15) 0.0281(19) C201 0.134(15) 0.096(13) 0.044(8) 0.003(8) 0.060(10) 0.021(11) C202 0.123(14) 0.058(9) 0.054(9) -0.024(7) 0.027(9) 0.008(9) N30 0.049(6) 0.077(7) 0.024(4) -0.019(4) 0.024(4) -0.032(5) C301 0.099(14) 0.119(16) 0.096(14) 0.041(12) 0.061(12) 0.038(12) C302 0.056(8) 0.113(14) 0.057(9) -0.027(9) 0.020(7) -0.027(9) C303 0.071(9) 0.084(11) 0.058(8) 0.021(8) 0.018(7) -0.029(8) C304 0.046(7) 0.044(7) 0.071(9) 0.009(6) 0.018(6) 0.003(5) N01 0.24(3) 0.084(13) 0.16(2) 0.012(13) 0.137(19) 0.034(15) C011 0.097(12) 0.078(12) 0.056(9) 0.010(8) 0.039(8) 0.021(10) C012 0.18(2) 0.092(14) 0.060(10) -0.026(10) 0.036(12) -0.058(14) N02 0.134(17) 0.16(2) 0.108(15) -0.052(14) 0.016(13) -0.029(15) C021 0.089(13) 0.124(17) 0.081(13) -0.037(12) 0.029(11) -0.036(12) C022 0.057(8) 0.113(13) 0.065(9) -0.041(9) 0.029(7) -0.043(9) N03 0.119(14) 0.123(14) 0.088(11) -0.050(11) 0.045(10) -0.053(12) C031 0.098(13) 0.104(14) 0.039(7) -0.022(8) 0.034(8) -0.029(11) C032 0.071(9) 0.072(10) 0.050(8) 0.014(7) 0.022(7) 0.016(8) N04 0.36(4) 0.116(17) 0.25(3) -0.119(19) 0.24(3) -0.14(2) C041 0.148(17) 0.066(11) 0.082(12) -0.024(9) 0.082(12) -0.030(11) C042 0.061(8) 0.037(6) 0.040(6) 0.002(5) 0.008(5) -0.001(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O3 1.781(6) . ? U1 O1 1.839(6) . ? U1 O0 2.223(6) . ? U1 O21 2.299(6) . ? U1 O31 2.340(6) . ? U1 O41 2.398(6) . ? U1 O11 2.459(6) . ? U1 U3 3.5786(5) . ? U2 O4 1.791(6) . ? U2 O2 1.846(6) . ? U2 O71 2.187(5) . ? U2 O0 2.235(5) . ? U2 O61 2.282(6) . ? U2 O81 2.451(6) . ? U2 O51 2.522(5) . ? U2 U3 3.5742(5) . ? U3 O5 1.772(6) . ? U3 O6 1.778(6) . ? U3 O0 2.262(6) . ? U3 O20 2.388(8) . ? U3 O10 2.418(6) . ? U3 O2 2.445(6) . ? U3 O1 2.492(6) . ? O11 C11 1.367(10) . ? C11 C16 1.400(12) . ? C11 C12 1.401(12) . ? C12 C13 1.403(11) . ? C12 C2 1.512(12) . ? C13 C14 1.389(12) . ? C13 H13 0.95 . ? C14 C15 1.387(13) . ? C14 C141 1.541(12) . ? C141 C144 1.527(13) . ? C141 C143 1.539(14) . ? C141 C142 1.541(15) . ? C142 H14A 0.98 . ? C142 H14B 0.98 . ? C142 H14C 0.98 . ? C143 H14D 0.98 . ? C143 H14E 0.98 . ? C143 H14F 0.98 . ? C144 H14G 0.98 . ? C144 H14H 0.98 . ? C144 H14I 0.98 . ? C15 C16 1.396(12) . ? C15 H15 0.95 . ? C16 C1 1.518(12) . ? C1 C82 1.515(12) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? O21 C21 1.351(10) . ? C21 C22 1.403(11) . ? C21 C26 1.405(12) . ? C22 C23 1.384(12) . ? C22 C3 1.526(12) . ? C23 C24 1.418(12) . ? C23 H23 0.95 . ? C24 C25 1.401(12) . ? C24 C241 1.528(12) . ? C241 C242 1.518(15) . ? C241 C243 1.520(15) . ? C241 C244 1.529(14) . ? C242 H24A 0.98 . ? C242 H24B 0.98 . ? C242 H24C 0.98 . ? C243 H24D 0.98 . ? C243 H24E 0.98 . ? C243 H24F 0.98 . ? C244 H24G 0.98 . ? C244 H24H 0.98 . ? C244 H24I 0.98 . ? C25 C26 1.380(13) . ? C25 H25 0.95 . ? C26 C2 1.508(11) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O31 C31 1.366(10) . ? C31 C32 1.376(12) . ? C31 C36 1.398(12) . ? C32 C33 1.378(12) . ? C32 C4 1.543(11) . ? C33 C34 1.386(12) . ? C33 H33 0.95 . ? C34 C35 1.429(13) . ? C34 C341 1.526(13) . ? C341 C342 1.524(18) . ? C341 C344 1.533(17) . ? C341 C343 1.543(16) . ? C342 H34A 0.98 . ? C342 H34B 0.98 . ? C342 H34C 0.98 . ? C343 H34D 0.98 . ? C343 H34E 0.98 . ? C343 H34F 0.98 . ? C344 H34G 0.98 . ? C344 H34H 0.98 . ? C344 H34I 0.98 . ? C35 C36 1.378(12) . ? C35 H35 0.95 . ? C36 C3 1.511(12) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O41 C41 1.353(9) . ? C41 C46 1.405(11) . ? C41 C42 1.416(13) . ? C42 C43 1.379(12) . ? C42 C5 1.523(11) . ? C43 C44 1.417(12) . ? C43 H43 0.95 . ? C44 C45 1.391(13) . ? C44 C441 1.530(12) . ? C441 C444 1.518(15) . ? C441 C442 1.521(17) . ? C441 C443 1.549(16) . ? C442 H44A 0.98 . ? C442 H44B 0.98 . ? C442 H44C 0.98 . ? C443 H44D 0.98 . ? C443 H44E 0.98 . ? C443 H44F 0.98 . ? C444 H44G 0.98 . ? C444 H44H 0.98 . ? C444 H44I 0.98 . ? C45 C46 1.401(11) . ? C45 H45 0.95 . ? C46 C4 1.517(12) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? O51 C51 1.376(10) . ? C51 C56 1.400(12) . ? C51 C52 1.411(12) . ? C52 C53 1.401(12) . ? C52 C6 1.514(13) . ? C53 C54 1.382(13) . ? C53 H53 0.95 . ? C54 C55 1.403(13) . ? C54 C541 1.533(12) . ? C541 C542 1.503(16) . ? C541 C545 1.519(14) . ? C541 C543 1.527(15) . ? C542 H54A 0.98 . ? C542 H54B 0.98 . ? C542 H54C 0.98 . ? C543 H54D 0.98 . ? C543 H54E 0.98 . ? C543 H54F 0.98 . ? C545 H54G 0.98 . ? C545 H54H 0.98 . ? C545 H54I 0.98 . ? C55 C56 1.401(12) . ? C55 H55 0.95 . ? C56 C5 1.519(12) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? O61 C61 1.365(10) . ? C61 C62 1.397(11) . ? C61 C66 1.399(12) . ? C62 C63 1.400(12) . ? C62 C7 1.530(12) . ? C63 C64 1.368(13) . ? C63 H63 0.95 . ? C64 C65 1.405(13) . ? C64 C641 1.535(13) . ? C641 C642 1.45(3) . ? C641 C644 1.467(16) . ? C641 C643 1.47(2) . ? C642 H64A 0.98 . ? C642 H64B 0.98 . ? C642 H64C 0.98 . ? C643 H64D 0.98 . ? C643 H64E 0.98 . ? C643 H64F 0.98 . ? C644 H64G 0.98 . ? C644 H64H 0.98 . ? C644 H64I 0.98 . ? C65 C66 1.393(13) . ? C65 H65 0.95 . ? C66 C6 1.514(11) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O71 C71 1.346(10) . ? C71 C76 1.405(12) . ? C71 C72 1.421(13) . ? C72 C73 1.401(13) . ? C72 C8 1.510(12) . ? C73 C74 1.383(14) . ? C73 H73 0.95 . ? C74 C75 1.411(13) . ? C74 C741 1.507(13) . ? C741 C742 1.523(15) . ? C741 C744 1.540(15) . ? C741 C743 1.565(16) . ? C742 H74A 0.98 . ? C742 H74B 0.98 . ? C742 H74C 0.98 . ? C743 H74D 0.98 . ? C743 H74E 0.98 . ? C743 H74F 0.98 . ? C744 H74G 0.98 . ? C744 H74H 0.98 . ? C744 H74I 0.98 . ? C75 C76 1.388(12) . ? C75 H75 0.95 . ? C76 C7 1.520(12) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? O81 C81 1.364(9) . ? C81 C82 1.398(13) . ? C81 C86 1.406(12) . ? C82 C83 1.404(11) . ? C83 C84 1.396(13) . ? C83 H83 0.95 . ? C84 C85 1.392(14) . ? C84 C841 1.537(11) . ? C841 C843 1.481(16) . ? C841 C842 1.513(15) . ? C841 C844 1.548(15) . ? C842 H84A 0.98 . ? C842 H84B 0.98 . ? C842 H84C 0.98 . ? C843 H84D 0.98 . ? C843 H84E 0.98 . ? C843 H84F 0.98 . ? C844 H84G 0.98 . ? C844 H84H 0.98 . ? C844 H84I 0.98 . ? C85 C86 1.392(12) . ? C85 H85 0.95 . ? C86 C8 1.494(13) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? O10 S10 1.554(7) . ? S10 C102 1.766(13) . ? S10 C101 1.779(11) . ? C101 H10A 0.98 . ? C101 H10B 0.98 . ? C101 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? C102 H10F 0.98 . ? O20 S20 1.524(9) . ? S20 C202 1.780(14) . ? S20 C201 1.825(17) . ? C201 H20A 0.98 . ? C201 H20B 0.98 . ? C201 H20C 0.98 . ? C202 H20D 0.98 . ? C202 H20E 0.98 . ? C202 H20F 0.98 . ? N30 C301 1.421(9) . ? N30 C302 1.426(14) . ? N30 C304 1.531(13) . ? N30 C303 1.569(15) . ? C301 H30A 0.98 . ? C301 H30B 0.98 . ? C301 H30C 0.98 . ? C302 H30D 0.98 . ? C302 H30E 0.98 . ? C302 H30F 0.98 . ? C303 H30G 0.98 . ? C303 H30H 0.98 . ? C303 H30I 0.98 . ? C304 H30J 0.98 . ? C304 H30K 0.98 . ? C304 H30L 0.98 . ? N01 C011 1.13(2) . ? C011 C012 1.44(2) . ? C012 H01A 0.98 . ? C012 H01B 0.98 . ? C012 H01C 0.98 . ? N02 C021 1.17(2) . ? C021 C022 1.34(2) . ? C022 H02A 0.98 . ? C022 H02B 0.98 . ? C022 H02C 0.98 . ? N03 C031 1.14(2) . ? C031 C032 1.42(2) . ? C032 H03A 0.98 . ? C032 H03B 0.98 . ? C032 H03C 0.98 . ? N04 C041 1.10(2) . ? C041 C042 1.41(2) . ? C042 H04A 0.98 . ? C042 H04B 0.98 . ? C042 H04C 0.98 . ? N05 C051 1.26(4) . ? C051 C052 1.45(3) . ? C052 H05A 0.98 . ? C052 H05B 0.98 . ? C052 H05C 0.98 . ? N06 C061 1.249(4) . ? C061 C062 1.448(4) . ? C062 H06A 0.98 . ? C062 H06B 0.98 . ? C062 H06C 0.98 . ? N07 C071 1.253(5) . ? C071 C072 1.453(5) . ? C072 H07A 0.98 . ? C072 H07B 0.98 . ? C072 H07C 0.98 . ? 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 O3 U1 O1 178.4(3) . . ? O3 U1 O0 100.3(2) . . ? O1 U1 O0 78.1(2) . . ? O3 U1 O21 88.2(3) . . ? O1 U1 O21 93.3(2) . . ? O0 U1 O21 141.9(2) . . ? O3 U1 O31 88.6(3) . . ? O1 U1 O31 92.3(2) . . ? O0 U1 O31 142.3(2) . . ? O21 U1 O31 74.2(2) . . ? O3 U1 O41 87.2(3) . . ? O1 U1 O41 91.8(2) . . ? O0 U1 O41 71.22(19) . . ? O21 U1 O41 146.8(2) . . ? O31 U1 O41 72.7(2) . . ? O3 U1 O11 87.6(3) . . ? O1 U1 O11 92.4(2) . . ? O0 U1 O11 69.6(2) . . ? O21 U1 O11 73.8(2) . . ? O31 U1 O11 147.9(2) . . ? O41 U1 O11 138.81(19) . . ? O3 U1 U3 137.76(19) . . ? O1 U1 U3 40.70(17) . . ? O0 U1 U3 37.45(16) . . ? O21 U1 U3 124.67(16) . . ? O31 U1 U3 122.94(17) . . ? O41 U1 U3 77.97(15) . . ? O11 U1 U3 78.89(14) . . ? O4 U2 O2 177.6(3) . . ? O4 U2 O71 92.8(2) . . ? O2 U2 O71 89.2(2) . . ? O4 U2 O0 100.6(3) . . ? O2 U2 O0 77.0(2) . . ? O71 U2 O0 140.6(2) . . ? O4 U2 O61 90.8(3) . . ? O2 U2 O61 90.8(2) . . ? O71 U2 O61 79.6(2) . . ? O0 U2 O61 136.3(2) . . ? O4 U2 O81 88.6(2) . . ? O2 U2 O81 90.7(2) . . ? O71 U2 O81 74.7(2) . . ? O0 U2 O81 68.82(19) . . ? O61 U2 O81 154.24(19) . . ? O4 U2 O51 87.9(2) . . ? O2 U2 O51 91.0(2) . . ? O71 U2 O51 150.7(2) . . ? O0 U2 O51 67.45(19) . . ? O61 U2 O51 71.07(19) . . ? O81 U2 O51 134.60(18) . . ? O4 U2 U3 138.27(19) . . ? O2 U2 U3 39.35(18) . . ? O71 U2 U3 119.91(16) . . ? O0 U2 U3 37.63(16) . . ? O61 U2 U3 118.34(15) . . ? O81 U2 U3 77.24(14) . . ? O51 U2 U3 75.79(14) . . ? O5 U3 O6 175.3(3) . . ? O5 U3 O0 92.4(3) . . ? O6 U3 O0 92.3(3) . . ? O5 U3 O20 87.9(3) . . ? O6 U3 O20 88.7(3) . . ? O0 U3 O20 137.3(2) . . ? O5 U3 O10 90.9(3) . . ? O6 U3 O10 85.2(3) . . ? O0 U3 O10 145.2(2) . . ? O20 U3 O10 77.4(2) . . ? O5 U3 O2 92.2(2) . . ? O6 U3 O2 89.8(2) . . ? O0 U3 O2 65.7(2) . . ? O20 U3 O2 71.6(2) . . ? O10 U3 O2 148.7(2) . . ? O5 U3 O1 88.7(2) . . ? O6 U3 O1 93.2(2) . . ? O0 U3 O1 65.45(19) . . ? O20 U3 O1 157.1(2) . . ? O10 U3 O1 80.0(2) . . ? O2 U3 O1 131.1(2) . . ? O5 U3 U2 93.0(2) . . ? O6 U3 U2 90.7(2) . . ? O0 U3 U2 37.11(14) . . ? O20 U3 U2 100.23(18) . . ? O10 U3 U2 175.36(16) . . ? O2 U3 U2 28.60(15) . . ? O1 U3 U2 102.56(14) . . ? O5 U3 U1 91.0(2) . . ? O6 U3 U1 92.7(2) . . ? O0 U3 U1 36.70(14) . . ? O20 U3 U1 173.89(18) . . ? O10 U3 U1 108.63(15) . . ? O2 U3 U1 102.40(15) . . ? O1 U3 U1 28.76(14) . . ? U2 U3 U1 73.811(12) . . ? U1 O0 U2 148.9(3) . . ? U1 O0 U3 105.9(2) . . ? U2 O0 U3 105.3(2) . . ? U1 O1 U3 110.5(2) . . ? U2 O2 U3 112.1(3) . . ? C11 O11 U1 130.0(5) . . ? O11 C11 C16 121.0(8) . . ? O11 C11 C12 119.0(8) . . ? C16 C11 C12 119.9(8) . . ? C11 C12 C13 118.9(8) . . ? C11 C12 C2 121.1(7) . . ? C13 C12 C2 119.9(8) . . ? C14 C13 C12 122.1(8) . . ? C14 C13 H13 119 . . ? C12 C13 H13 119 . . ? C15 C14 C13 117.3(8) . . ? C15 C14 C141 119.9(8) . . ? C13 C14 C141 122.7(8) . . ? C144 C141 C143 108.4(9) . . ? C144 C141 C14 109.4(8) . . ? C143 C141 C14 112.7(8) . . ? C144 C141 C142 108.4(9) . . ? C143 C141 C142 107.7(8) . . ? C14 C141 C142 110.1(8) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C14 C15 C16 122.8(9) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C11 118.7(8) . . ? C15 C16 C1 120.1(8) . . ? C11 C16 C1 121.2(8) . . ? C82 C1 C16 110.0(7) . . ? C82 C1 H1A 109.7 . . ? C16 C1 H1A 109.7 . . ? C82 C1 H1B 109.7 . . ? C16 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C21 O21 U1 139.4(6) . . ? O21 C21 C22 120.8(8) . . ? O21 C21 C26 119.3(7) . . ? C22 C21 C26 119.9(8) . . ? C23 C22 C21 118.5(8) . . ? C23 C22 C3 120.3(7) . . ? C21 C22 C3 121.0(8) . . ? C22 C23 C24 123.3(7) . . ? C22 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C25 C24 C23 115.8(8) . . ? C25 C24 C241 124.0(8) . . ? C23 C24 C241 120.1(7) . . ? C242 C241 C243 107.4(10) . . ? C242 C241 C24 112.3(8) . . ? C243 C241 C24 110.2(9) . . ? C242 C241 C244 108.3(10) . . ? C243 C241 C244 108.6(9) . . ? C24 C241 C244 110.0(8) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? H24A C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? H24D C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? H24D C243 H24F 109.5 . . ? H24E C243 H24F 109.5 . . ? C241 C244 H24G 109.5 . . ? C241 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C241 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C26 C25 C24 122.6(9) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C25 C26 C21 119.8(8) . . ? C25 C26 C2 122.4(8) . . ? C21 C26 C2 117.7(8) . . ? C26 C2 C12 116.0(7) . . ? C26 C2 H2A 108.3 . . ? C12 C2 H2A 108.3 . . ? C26 C2 H2B 108.3 . . ? C12 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C31 O31 U1 135.4(6) . . ? O31 C31 C32 119.5(8) . . ? O31 C31 C36 120.6(8) . . ? C32 C31 C36 119.9(8) . . ? C31 C32 C33 120.9(8) . . ? C31 C32 C4 118.9(7) . . ? C33 C32 C4 120.1(8) . . ? C32 C33 C34 121.9(8) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C35 116.0(8) . . ? C33 C34 C341 123.8(9) . . ? C35 C34 C341 120.2(8) . . ? C342 C341 C34 109.1(9) . . ? C342 C341 C344 113.1(12) . . ? C34 C341 C344 109.7(10) . . ? C342 C341 C343 106.8(11) . . ? C34 C341 C343 112.6(9) . . ? C344 C341 C343 105.6(10) . . ? C341 C342 H34A 109.5 . . ? C341 C342 H34B 109.5 . . ? H34A C342 H34B 109.5 . . ? C341 C342 H34C 109.5 . . ? H34A C342 H34C 109.5 . . ? H34B C342 H34C 109.5 . . ? C341 C343 H34D 109.5 . . ? C341 C343 H34E 109.5 . . ? H34D C343 H34E 109.5 . . ? C341 C343 H34F 109.5 . . ? H34D C343 H34F 109.5 . . ? H34E C343 H34F 109.5 . . ? C341 C344 H34G 109.5 . . ? C341 C344 H34H 109.5 . . ? H34G C344 H34H 109.5 . . ? C341 C344 H34I 109.5 . . ? H34G C344 H34I 109.5 . . ? H34H C344 H34I 109.5 . . ? C36 C35 C34 122.6(9) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C35 C36 C31 118.6(8) . . ? C35 C36 C3 121.0(8) . . ? C31 C36 C3 120.4(8) . . ? C36 C3 C22 109.2(8) . . ? C36 C3 H3A 109.8 . . ? C22 C3 H3A 109.8 . . ? C36 C3 H3B 109.8 . . ? C22 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C41 O41 U1 133.2(5) . . ? O41 C41 C46 120.4(8) . . ? O41 C41 C42 120.3(7) . . ? C46 C41 C42 119.2(7) . . ? C43 C42 C41 119.8(8) . . ? C43 C42 C5 120.0(8) . . ? C41 C42 C5 119.9(8) . . ? C42 C43 C44 122.5(9) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 116.1(8) . . ? C45 C44 C441 123.6(8) . . ? C43 C44 C441 120.4(9) . . ? C444 C441 C442 109.6(10) . . ? C444 C441 C44 112.3(9) . . ? C442 C441 C44 108.6(9) . . ? C444 C441 C443 106.7(10) . . ? C442 C441 C443 109.4(10) . . ? C44 C441 C443 110.1(8) . . ? C441 C442 H44A 109.5 . . ? C441 C442 H44B 109.5 . . ? H44A C442 H44B 109.5 . . ? C441 C442 H44C 109.5 . . ? H44A C442 H44C 109.5 . . ? H44B C442 H44C 109.5 . . ? C441 C443 H44D 109.5 . . ? C441 C443 H44E 109.5 . . ? H44D C443 H44E 109.5 . . ? C441 C443 H44F 109.5 . . ? H44D C443 H44F 109.5 . . ? H44E C443 H44F 109.5 . . ? C441 C444 H44G 109.5 . . ? C441 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C441 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C44 C45 C46 123.4(8) . . ? C44 C45 H45 118.3 . . ? C46 C45 H45 118.3 . . ? C45 C46 C41 118.9(8) . . ? C45 C46 C4 119.5(7) . . ? C41 C46 C4 121.5(7) . . ? C46 C4 C32 114.3(7) . . ? C46 C4 H4A 108.7 . . ? C32 C4 H4A 108.7 . . ? C46 C4 H4B 108.7 . . ? C32 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C51 O51 U2 131.9(5) . . ? O51 C51 C56 120.5(8) . . ? O51 C51 C52 119.2(8) . . ? C56 C51 C52 120.3(8) . . ? C53 C52 C51 118.6(8) . . ? C53 C52 C6 120.6(8) . . ? C51 C52 C6 120.5(8) . . ? C54 C53 C52 122.9(8) . . ? C54 C53 H53 118.5 . . ? C52 C53 H53 118.5 . . ? C53 C54 C55 116.9(8) . . ? C53 C54 C541 123.3(8) . . ? C55 C54 C541 119.8(9) . . ? C542 C541 C545 108.2(10) . . ? C542 C541 C543 109.9(10) . . ? C545 C541 C543 107.7(10) . . ? C542 C541 C54 110.3(9) . . ? C545 C541 C54 108.9(8) . . ? C543 C541 C54 111.8(9) . . ? C541 C542 H54A 109.5 . . ? C541 C542 H54B 109.5 . . ? H54A C542 H54B 109.5 . . ? C541 C542 H54C 109.5 . . ? H54A C542 H54C 109.5 . . ? H54B C542 H54C 109.5 . . ? C541 C543 H54D 109.5 . . ? C541 C543 H54E 109.5 . . ? H54D C543 H54E 109.5 . . ? C541 C543 H54F 109.5 . . ? H54D C543 H54F 109.5 . . ? H54E C543 H54F 109.5 . . ? C541 C545 H54G 109.5 . . ? C541 C545 H54H 109.5 . . ? H54G C545 H54H 109.5 . . ? C541 C545 H54I 109.5 . . ? H54G C545 H54I 109.5 . . ? H54H C545 H54I 109.5 . . ? C56 C55 C54 122.8(9) . . ? C56 C55 H55 118.6 . . ? C54 C55 H55 118.6 . . ? C51 C56 C55 118.4(8) . . ? C51 C56 C5 121.1(8) . . ? C55 C56 C5 120.2(8) . . ? C56 C5 C42 108.9(7) . . ? C56 C5 H5A 109.9 . . ? C42 C5 H5A 109.9 . . ? C56 C5 H5B 109.9 . . ? C42 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C61 O61 U2 132.4(5) . . ? O61 C61 C62 120.7(8) . . ? O61 C61 C66 119.3(7) . . ? C62 C61 C66 120.0(8) . . ? C61 C62 C63 118.3(8) . . ? C61 C62 C7 121.5(7) . . ? C63 C62 C7 119.9(7) . . ? C64 C63 C62 123.4(8) . . ? C64 C63 H63 118.3 . . ? C62 C63 H63 118.3 . . ? C63 C64 C65 117.3(9) . . ? C63 C64 C641 121.4(8) . . ? C65 C64 C641 121.3(9) . . ? C642 C641 C644 111.1(16) . . ? C642 C641 C643 109.0(18) . . ? C644 C641 C643 105.0(14) . . ? C642 C641 C64 107.2(13) . . ? C644 C641 C64 113.4(9) . . ? C643 C641 C64 111.2(11) . . ? C641 C642 H64A 109.5 . . ? C641 C642 H64B 109.5 . . ? H64A C642 H64B 109.5 . . ? C641 C642 H64C 109.5 . . ? H64A C642 H64C 109.5 . . ? H64B C642 H64C 109.5 . . ? C641 C643 H64D 109.5 . . ? C641 C643 H64E 109.5 . . ? H64D C643 H64E 109.5 . . ? C641 C643 H64F 109.5 . . ? H64D C643 H64F 109.5 . . ? H64E C643 H64F 109.5 . . ? C641 C644 H64G 109.5 . . ? C641 C644 H64H 109.5 . . ? H64G C644 H64H 109.5 . . ? C641 C644 H64I 109.5 . . ? H64G C644 H64I 109.5 . . ? H64H C644 H64I 109.5 . . ? C66 C65 C64 121.6(9) . . ? C66 C65 H65 119.2 . . ? C64 C65 H65 119.2 . . ? C65 C66 C61 119.5(8) . . ? C65 C66 C6 120.8(8) . . ? C61 C66 C6 119.6(8) . . ? C52 C6 C66 115.4(8) . . ? C52 C6 H6A 108.4 . . ? C66 C6 H6A 108.4 . . ? C52 C6 H6B 108.4 . . ? C66 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C71 O71 U2 138.8(5) . . ? O71 C71 C76 120.4(8) . . ? O71 C71 C72 120.1(8) . . ? C76 C71 C72 119.6(8) . . ? C73 C72 C71 118.2(8) . . ? C73 C72 C8 123.1(9) . . ? C71 C72 C8 118.5(8) . . ? C74 C73 C72 123.8(9) . . ? C74 C73 H73 118.1 . . ? C72 C73 H73 118.1 . . ? C73 C74 C75 116.0(9) . . ? C73 C74 C741 123.2(9) . . ? C75 C74 C741 120.7(9) . . ? C74 C741 C742 109.3(9) . . ? C74 C741 C744 112.8(8) . . ? C742 C741 C744 108.0(10) . . ? C74 C741 C743 110.4(9) . . ? C742 C741 C743 108.0(9) . . ? C744 C741 C743 108.3(11) . . ? C741 C742 H74A 109.5 . . ? C741 C742 H74B 109.5 . . ? H74A C742 H74B 109.5 . . ? C741 C742 H74C 109.5 . . ? H74A C742 H74C 109.5 . . ? H74B C742 H74C 109.5 . . ? C741 C743 H74D 109.5 . . ? C741 C743 H74E 109.5 . . ? H74D C743 H74E 109.5 . . ? C741 C743 H74F 109.5 . . ? H74D C743 H74F 109.5 . . ? H74E C743 H74F 109.5 . . ? C741 C744 H74G 109.5 . . ? C741 C744 H74H 109.5 . . ? H74G C744 H74H 109.5 . . ? C741 C744 H74I 109.5 . . ? H74G C744 H74I 109.5 . . ? H74H C744 H74I 109.5 . . ? C76 C75 C74 123.2(9) . . ? C76 C75 H75 118.4 . . ? C74 C75 H75 118.4 . . ? C75 C76 C71 119.1(9) . . ? C75 C76 C7 120.3(8) . . ? C71 C76 C7 120.3(8) . . ? C76 C7 C62 108.7(7) . . ? C76 C7 H7A 110 . . ? C62 C7 H7A 110 . . ? C76 C7 H7B 110 . . ? C62 C7 H7B 110 . . ? H7A C7 H7B 108.3 . . ? C81 O81 U2 128.2(5) . . ? O81 C81 C82 119.8(8) . . ? O81 C81 C86 119.8(8) . . ? C82 C81 C86 120.4(8) . . ? C81 C82 C83 118.5(8) . . ? C81 C82 C1 120.7(7) . . ? C83 C82 C1 120.5(8) . . ? C84 C83 C82 122.7(9) . . ? C84 C83 H83 118.7 . . ? C82 C83 H83 118.7 . . ? C85 C84 C83 116.8(8) . . ? C85 C84 C841 120.8(8) . . ? C83 C84 C841 122.3(9) . . ? C843 C841 C842 109.1(10) . . ? C843 C841 C84 113.4(9) . . ? C842 C841 C84 108.6(8) . . ? C843 C841 C844 109.0(9) . . ? C842 C841 C844 107.4(9) . . ? C84 C841 C844 109.1(8) . . ? C841 C842 H84A 109.5 . . ? C841 C842 H84B 109.5 . . ? H84A C842 H84B 109.5 . . ? C841 C842 H84C 109.5 . . ? H84A C842 H84C 109.5 . . ? H84B C842 H84C 109.5 . . ? C841 C843 H84D 109.5 . . ? C841 C843 H84E 109.5 . . ? H84D C843 H84E 109.5 . . ? C841 C843 H84F 109.5 . . ? H84D C843 H84F 109.5 . . ? H84E C843 H84F 109.5 . . ? C841 C844 H84G 109.5 . . ? C841 C844 H84H 109.5 . . ? H84G C844 H84H 109.5 . . ? C841 C844 H84I 109.5 . . ? H84G C844 H84I 109.5 . . ? H84H C844 H84I 109.5 . . ? C84 C85 C86 122.9(8) . . ? C84 C85 H85 118.5 . . ? C86 C85 H85 118.5 . . ? C85 C86 C81 118.7(9) . . ? C85 C86 C8 120.7(8) . . ? C81 C86 C8 120.4(8) . . ? C86 C8 C72 114.8(8) . . ? C86 C8 H8A 108.6 . . ? C72 C8 H8A 108.6 . . ? C86 C8 H8B 108.6 . . ? C72 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? S10 O10 U3 119.5(4) . . ? O10 S10 C102 105.0(6) . . ? O10 S10 C101 102.5(5) . . ? C102 S10 C101 100.3(6) . . ? S10 C101 H10A 109.5 . . ? S10 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? S10 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? S10 C102 H10D 109.5 . . ? S10 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? S10 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? S20 O20 U3 125.4(5) . . ? O20 S20 C202 102.7(6) . . ? O20 S20 C201 106.3(6) . . ? C202 S20 C201 99.0(8) . . ? S20 C201 H20A 109.5 . . ? S20 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? S20 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? S20 C202 H20D 109.5 . . ? S20 C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? S20 C202 H20F 109.5 . . ? H20D C202 H20F 109.5 . . ? H20E C202 H20F 109.5 . . ? C301 N30 C302 114.8(14) . . ? C301 N30 C304 108.2(10) . . ? C302 N30 C304 113.0(9) . . ? C301 N30 C303 104.9(11) . . ? C302 N30 C303 110.6(11) . . ? C304 N30 C303 104.6(10) . . ? N30 C301 H30A 109.5 . . ? N30 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? N30 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? N30 C302 H30D 109.5 . . ? N30 C302 H30E 109.5 . . ? H30D C302 H30E 109.5 . . ? N30 C302 H30F 109.5 . . ? H30D C302 H30F 109.5 . . ? H30E C302 H30F 109.5 . . ? N30 C303 H30G 109.5 . . ? N30 C303 H30H 109.5 . . ? H30G C303 H30H 109.5 . . ? N30 C303 H30I 109.5 . . ? H30G C303 H30I 109.5 . . ? H30H C303 H30I 109.5 . . ? N30 C304 H30J 109.5 . . ? N30 C304 H30K 109.5 . . ? H30J C304 H30K 109.5 . . ? N30 C304 H30L 109.5 . . ? H30J C304 H30L 109.5 . . ? H30K C304 H30L 109.5 . . ? N01 C011 C012 175(2) . . ? C011 C012 H01A 109.5 . . ? C011 C012 H01B 109.5 . . ? H01A C012 H01B 109.5 . . ? C011 C012 H01C 109.5 . . ? H01A C012 H01C 109.5 . . ? H01B C012 H01C 109.5 . . ? N02 C021 C022 173(3) . . ? C021 C022 H02A 109.5 . . ? C021 C022 H02B 109.5 . . ? H02A C022 H02B 109.5 . . ? C021 C022 H02C 109.5 . . ? H02A C022 H02C 109.5 . . ? H02B C022 H02C 109.5 . . ? N03 C031 C032 175(2) . . ? C031 C032 H03A 109.5 . . ? C031 C032 H03B 109.5 . . ? H03A C032 H03B 109.5 . . ? C031 C032 H03C 109.5 . . ? H03A C032 H03C 109.5 . . ? H03B C032 H03C 109.5 . . ? N04 C041 C042 176(3) . . ? C041 C042 H04A 109.5 . . ? C041 C042 H04B 109.5 . . ? H04A C042 H04B 109.5 . . ? C041 C042 H04C 109.5 . . ? H04A C042 H04C 109.5 . . ? H04B C042 H04C 109.5 . . ? N05 C051 C052 175(4) . . ? C051 C052 H05A 109.5 . . ? C051 C052 H05B 109.5 . . ? H05A C052 H05B 109.5 . . ? C051 C052 H05C 109.5 . . ? H05A C052 H05C 109.5 . . ? H05B C052 H05C 109.5 . . ? N06 C061 C062 177(3) . . ? C061 C062 H06A 109.5 . . ? C061 C062 H06B 109.5 . . ? H06A C062 H06B 109.5 . . ? C061 C062 H06C 109.5 . . ? H06A C062 H06C 109.5 . . ? H06B C062 H06C 109.5 . . ? N07 C071 C072 170(3) . . ? C071 C072 H07A 109.5 . . ? C071 C072 H07B 109.5 . . ? H07A C072 H07B 109.5 . . ? C071 C072 H07C 109.5 . . ? H07A C072 H07C 109.5 . . ? H07B C072 H07C 109.5 . . ? #===END # Attachment '- udmso_alpha.cif' data_udmso _database_code_depnum_ccdc_archive 'CCDC 773902' #TrackingRef '- udmso_alpha.cif' _audit_creation_date 2010-03-11T13:35:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H30 Cl2 O15 S5 U' _chemical_formula_moiety 'C10 H30 O7 S5 U, 2(Cl O4)' _chemical_formula_weight 859.57 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_space_group_name_Hall c_-2yc 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' _cell_length_a 22.2250(9) _cell_length_b 12.1538(3) _cell_length_c 11.9704(6) _cell_angle_alpha 90 _cell_angle_beta 113.670(5) _cell_angle_gamma 90 _cell_volume 2961.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10518 _cell_measurement_theta_min 3.8118 _cell_measurement_theta_max 32.6315 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.0585 1 0 0 0.0999 -1 1 0 0.1119 1 -1 0 0.1139 18 -14 -5 0.0963 -21 13 4 0.1324 -4 -12 11 0.1778 9 -8 -15 0.0902 9 3 -16 0.1057 -11 -1 17 0.2119 1 1 0 0.1189 18 14 -7 0.1174 -6 11 13 0.1679 0 -15 -8 0.0944 -3 -17 3 0.1382 31 2 -9 0.0871 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.07 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.249 _exptl_absorpt_correction_T_max 0.437 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0276980146 _diffrn_orient_matrix_ub_12 0.0353860955 _diffrn_orient_matrix_ub_13 0.020883853 _diffrn_orient_matrix_ub_21 0.0207636809 _diffrn_orient_matrix_ub_22 -0.0454702133 _diffrn_orient_matrix_ub_23 0.0038622524 _diffrn_orient_matrix_ub_31 -0.0040132431 _diffrn_orient_matrix_ub_32 0.0092113642 _diffrn_orient_matrix_ub_33 -0.0611452453 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_number 31414 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 32.69 _diffrn_reflns_theta_full 32 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.948 _reflns_number_total 10027 _reflns_number_gt 5306 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10027 _refine_ls_number_parameters 334 _refine_ls_number_restraints 353 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 0.832 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.005 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_diff_density_max 0.984 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.74797(5) 0.953755(10) 0.47246(8) 0.06687(4) Uani 1 1 d . A . O10 O 0.6988(3) 0.9571(4) 0.3176(5) 0.103(2) Uani 1 1 d . . . O20 O 0.7884(4) 0.9489(4) 0.6332(6) 0.1006(19) Uani 1 1 d . . . O1 O 0.72269(16) 0.7640(3) 0.4471(4) 0.0868(11) Uani 1 1 d DU . . S1 S 0.72427(16) 0.6656(2) 0.4207(3) 0.0735(11) Uani 0.5 1 d PDU A 1 C11 C 0.7672(5) 0.5914(10) 0.3615(10) 0.082(3) Uiso 0.5 1 d PDU A 1 H11A H 0.774 0.6335 0.2996 0.122 Uiso 0.5 1 calc PR A 1 H11B H 0.7435 0.5254 0.3261 0.122 Uiso 0.5 1 calc PR A 1 H11C H 0.809 0.5726 0.4246 0.122 Uiso 0.5 1 calc PR A 1 C12 C 0.7234(6) 0.5648(8) 0.5388(10) 0.070(3) Uiso 0.5 1 d PDU A 1 H12A H 0.6997 0.5957 0.583 0.104 Uiso 0.5 1 calc PR A 1 H12B H 0.7677 0.5491 0.5943 0.104 Uiso 0.5 1 calc PR A 1 H12C H 0.7023 0.4981 0.4995 0.104 Uiso 0.5 1 calc PR A 1 S1' S 0.77032(18) 0.6768(3) 0.5155(3) 0.0783(12) Uani 0.5 1 d PDU A 2 C11' C 0.7885(7) 0.5838(11) 0.4293(12) 0.090(3) Uiso 0.5 1 d PDU A 2 H11D H 0.8244 0.6103 0.4118 0.135 Uiso 0.5 1 calc PR A 2 H11E H 0.7508 0.5727 0.3543 0.135 Uiso 0.5 1 calc PR A 2 H11F H 0.8005 0.5153 0.4727 0.135 Uiso 0.5 1 calc PR A 2 C12' C 0.7049(5) 0.5945(10) 0.5400(11) 0.068(3) Uiso 0.5 1 d PDU A 2 H12D H 0.6882 0.6358 0.5898 0.103 Uiso 0.5 1 calc PR A 2 H12E H 0.7233 0.5266 0.5801 0.103 Uiso 0.5 1 calc PR A 2 H12F H 0.6697 0.5791 0.4627 0.103 Uiso 0.5 1 calc PR A 2 O2 O 0.66489(15) 0.8624(3) 0.5117(4) 0.0834(11) Uani 1 1 d DU . . S2 S 0.59552(14) 0.8973(3) 0.4662(4) 0.0818(11) Uani 0.5 1 d PDU A 1 C21 C 0.5549(7) 0.7889(9) 0.3801(11) 0.084(3) Uiso 0.5 1 d PDU A 1 H21A H 0.5637 0.7852 0.308 0.126 Uiso 0.5 1 calc PR A 1 H21B H 0.5086 0.7978 0.3575 0.126 Uiso 0.5 1 calc PR A 1 H21C H 0.5695 0.7222 0.4261 0.126 Uiso 0.5 1 calc PR A 1 C22 C 0.5680(6) 0.8775(11) 0.5938(9) 0.078(3) Uiso 0.5 1 d PDU A 1 H22A H 0.5851 0.9359 0.6521 0.117 Uiso 0.5 1 calc PR A 1 H22B H 0.5839 0.8082 0.6329 0.117 Uiso 0.5 1 calc PR A 1 H22C H 0.5209 0.8784 0.5617 0.117 Uiso 0.5 1 calc PR A 1 S2' S 0.61675(15) 0.8265(3) 0.5421(4) 0.0831(10) Uani 0.5 1 d PDU A 2 C21' C 0.5612(6) 0.7544(10) 0.4340(11) 0.083(3) Uiso 0.5 1 d PDU A 2 H21D H 0.5824 0.6988 0.4058 0.125 Uiso 0.5 1 calc PR A 2 H21E H 0.5363 0.8021 0.3675 0.125 Uiso 0.5 1 calc PR A 2 H21F H 0.5323 0.7202 0.4654 0.125 Uiso 0.5 1 calc PR A 2 C22' C 0.5685(6) 0.9179(11) 0.5965(11) 0.080(4) Uiso 0.5 1 d PDU A 2 H22D H 0.5976 0.966 0.6583 0.12 Uiso 0.5 1 calc PR A 2 H22E H 0.5437 0.8747 0.63 0.12 Uiso 0.5 1 calc PR A 2 H22F H 0.5391 0.961 0.5296 0.12 Uiso 0.5 1 calc PR A 2 O3 O 0.6852(2) 1.1136(4) 0.4595(4) 0.1296(19) Uani 1 1 d DU . . S3 S 0.6710(2) 1.2200(3) 0.4791(4) 0.0946(13) Uani 0.5 1 d PDU A 1 C31 C 0.5965(5) 1.2634(12) 0.4199(13) 0.100(3) Uiso 0.5 1 d PDU A 1 H31A H 0.5795 1.2555 0.3329 0.15 Uiso 0.5 1 calc PR A 1 H31B H 0.5953 1.3396 0.4403 0.15 Uiso 0.5 1 calc PR A 1 H31C H 0.5702 1.2211 0.4512 0.15 Uiso 0.5 1 calc PR A 1 C32 C 0.6936(8) 1.2557(13) 0.6401(10) 0.112(4) Uiso 0.5 1 d PDU A 1 H32A H 0.7369 1.2287 0.6882 0.168 Uiso 0.5 1 calc PR A 1 H32B H 0.6628 1.2229 0.668 0.168 Uiso 0.5 1 calc PR A 1 H32C H 0.6928 1.3343 0.6483 0.168 Uiso 0.5 1 calc PR A 1 S3' S 0.65929(18) 1.1695(3) 0.5414(3) 0.0897(10) Uani 0.5 1 d PDU A 2 C31' C 0.5934(6) 1.2372(12) 0.4517(13) 0.091(3) Uiso 0.5 1 d PDU A 2 H31D H 0.5588 1.186 0.4096 0.136 Uiso 0.5 1 calc PR A 2 H31E H 0.6034 1.2792 0.3934 0.136 Uiso 0.5 1 calc PR A 2 H31F H 0.5795 1.286 0.4999 0.136 Uiso 0.5 1 calc PR A 2 C32' C 0.7164(6) 1.2802(9) 0.6170(11) 0.080(3) Uiso 0.5 1 d PDU A 2 H32D H 0.7552 1.2499 0.6795 0.12 Uiso 0.5 1 calc PR A 2 H32E H 0.696 1.3305 0.653 0.12 Uiso 0.5 1 calc PR A 2 H32F H 0.728 1.3184 0.5584 0.12 Uiso 0.5 1 calc PR A 2 O4 O 0.8017(3) 1.0956(5) 0.4302(6) 0.123(2) Uani 1 1 d DU . . S4 S 0.8420(2) 1.1691(4) 0.4016(5) 0.1010(14) Uani 0.5 1 d PDU A 1 C41 C 0.7839(7) 1.2463(13) 0.3229(14) 0.111(3) Uiso 0.5 1 d PDU A 1 H41A H 0.7483 1.2026 0.2683 0.167 Uiso 0.5 1 calc PR A 1 H41B H 0.7986 1.2959 0.2766 0.167 Uiso 0.5 1 calc PR A 1 H41C H 0.7694 1.2878 0.3756 0.167 Uiso 0.5 1 calc PR A 1 C42 C 0.9132(7) 1.2112(13) 0.5343(12) 0.110(5) Uiso 0.5 1 d PDU A 1 H42A H 0.9375 1.1473 0.5751 0.165 Uiso 0.5 1 calc PR A 1 H42B H 0.8992 1.2512 0.5888 0.165 Uiso 0.5 1 calc PR A 1 H42C H 0.9406 1.2574 0.5095 0.165 Uiso 0.5 1 calc PR A 1 S4' S 0.8246(2) 1.2063(4) 0.4701(5) 0.1062(15) Uani 0.5 1 d PDU A 2 C41' C 0.8046(8) 1.3231(11) 0.3938(15) 0.126(4) Uiso 0.5 1 d PDU A 2 H41D H 0.7619 1.346 0.3871 0.19 Uiso 0.5 1 calc PR A 2 H41E H 0.8039 1.3129 0.3138 0.19 Uiso 0.5 1 calc PR A 2 H41F H 0.8364 1.3785 0.4363 0.19 Uiso 0.5 1 calc PR A 2 C42' C 0.9037(6) 1.2064(14) 0.4460(16) 0.124(4) Uiso 0.5 1 d PDU A 2 H42D H 0.9299 1.144 0.4865 0.185 Uiso 0.5 1 calc PR A 2 H42E H 0.9277 1.2728 0.4789 0.185 Uiso 0.5 1 calc PR A 2 H42F H 0.8938 1.2024 0.3602 0.185 Uiso 0.5 1 calc PR A 2 O5 O 0.85086(19) 0.9276(4) 0.4603(5) 0.0938(13) Uani 1 1 d DU . . S5 S 0.87340(18) 0.8390(4) 0.4078(4) 0.0846(12) Uani 0.5 1 d PDU A 1 C51 C 0.9134(6) 0.8755(11) 0.3206(10) 0.084(3) Uiso 0.5 1 d PDU A 1 H51A H 0.8821 0.8932 0.24 0.125 Uiso 0.5 1 calc PR A 1 H51B H 0.9405 0.8156 0.3162 0.125 Uiso 0.5 1 calc PR A 1 H51C H 0.9404 0.9386 0.3556 0.125 Uiso 0.5 1 calc PR A 1 C52 C 0.9487(6) 0.7929(12) 0.5422(11) 0.089(3) Uiso 0.5 1 d PDU A 1 H52A H 0.9361 0.7654 0.6048 0.133 Uiso 0.5 1 calc PR A 1 H52B H 0.978 0.8541 0.5732 0.133 Uiso 0.5 1 calc PR A 1 H52C H 0.9704 0.7357 0.5171 0.133 Uiso 0.5 1 calc PR A 1 S5' S 0.90833(17) 0.8947(4) 0.4895(4) 0.0815(11) Uani 0.5 1 d PDU A 2 C51' C 0.9345(7) 0.9112(13) 0.3831(11) 0.092(3) Uiso 0.5 1 d PDU A 2 H51D H 0.9188 0.9801 0.3427 0.138 Uiso 0.5 1 calc PR A 2 H51E H 0.9186 0.8523 0.3251 0.138 Uiso 0.5 1 calc PR A 2 H51F H 0.9817 0.911 0.418 0.138 Uiso 0.5 1 calc PR A 2 C52' C 0.9383(6) 0.7563(8) 0.5454(11) 0.063(3) Uiso 0.5 1 d PDU A 2 H52D H 0.9265 0.7382 0.6121 0.095 Uiso 0.5 1 calc PR A 2 H52E H 0.9852 0.7543 0.5727 0.095 Uiso 0.5 1 calc PR A 2 H52F H 0.9188 0.704 0.4808 0.095 Uiso 0.5 1 calc PR A 2 Cl1 Cl 0.91490(9) 0.47075(15) 0.75189(18) 0.0840(8) Uani 1 1 d D . . O11 O 0.9386(5) 0.5025(10) 0.6692(9) 0.281(3) Uani 1 1 d D . . O12 O 0.8623(4) 0.4062(7) 0.6938(10) 0.228(4) Uani 1 1 d D . . O13 O 0.9074(5) 0.5548(6) 0.8120(9) 0.254(4) Uani 1 1 d D . . O14 O 0.9467(6) 0.3855(7) 0.7921(10) 0.264(6) Uani 1 1 d D . . Cl2 Cl 0.58097(12) 0.47171(18) 0.1948(2) 0.0938(9) Uani 1 1 d D . . O21 O 0.6438(3) 0.4389(8) 0.2415(8) 0.182(4) Uani 1 1 d D . . O22 O 0.5393(4) 0.4562(11) 0.2423(12) 0.314(6) Uani 1 1 d D . . O23 O 0.5514(5) 0.4556(9) 0.0718(6) 0.227(5) Uani 1 1 d D . . O24 O 0.5894(7) 0.5743(7) 0.2179(12) 0.269(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.05800(7) 0.05652(7) 0.09688(10) 0.0014(2) 0.04237(6) -0.0018(2) O10 0.075(3) 0.150(5) 0.074(3) 0.019(2) 0.021(2) 0.034(3) O20 0.104(4) 0.104(4) 0.110(4) 0.037(2) 0.060(3) 0.018(3) O1 0.063(2) 0.0641(18) 0.125(3) -0.001(2) 0.029(2) -0.0094(15) S1 0.0663(16) 0.0587(15) 0.089(2) -0.0025(14) 0.0238(15) -0.0104(13) S1' 0.068(2) 0.0744(19) 0.092(2) 0.0122(16) 0.0315(17) -0.0074(16) O2 0.0535(16) 0.081(2) 0.125(3) 0.016(2) 0.0452(17) -0.0132(17) S2 0.0409(13) 0.0698(18) 0.129(2) 0.0145(18) 0.0283(15) -0.0028(13) S2' 0.0545(13) 0.0808(18) 0.124(2) 0.0224(16) 0.0459(14) 0.0016(14) O3 0.136(3) 0.097(2) 0.124(3) -0.014(2) 0.018(3) 0.086(2) S3 0.084(2) 0.097(2) 0.101(2) 0.0221(18) 0.0354(18) 0.0310(18) S3' 0.1219(18) 0.092(2) 0.0869(16) 0.0326(15) 0.0752(14) 0.0310(18) O4 0.106(4) 0.098(3) 0.134(4) 0.016(3) 0.024(3) -0.041(3) S4 0.107(2) 0.077(2) 0.129(3) -0.006(2) 0.058(2) -0.0283(19) S4' 0.085(2) 0.109(3) 0.141(3) 0.025(2) 0.062(2) -0.002(2) O5 0.062(2) 0.093(3) 0.135(3) -0.015(2) 0.048(2) -0.006(2) S5 0.0544(17) 0.101(2) 0.101(2) -0.0004(19) 0.0346(17) 0.0117(17) S5' 0.0532(16) 0.087(2) 0.111(2) -0.0012(19) 0.0400(16) 0.0030(16) Cl1 0.0589(9) 0.0796(11) 0.1046(14) 0.0182(9) 0.0234(10) 0.0030(8) O11 0.459(8) 0.205(6) 0.367(7) 0.091(6) 0.361(6) 0.059(8) O12 0.174(7) 0.210(6) 0.305(10) -0.151(6) 0.101(7) -0.097(6) O13 0.272(8) 0.202(6) 0.357(8) -0.167(6) 0.197(7) -0.017(6) O14 0.319(12) 0.197(7) 0.234(9) 0.081(7) 0.067(9) 0.130(8) Cl2 0.0949(15) 0.0869(15) 0.1080(16) -0.0020(11) 0.0495(13) -0.0031(11) O21 0.059(3) 0.300(12) 0.174(7) -0.013(6) 0.034(4) 0.034(5) O22 0.169(5) 0.436(17) 0.432(12) 0.227(11) 0.221(6) 0.105(8) O23 0.173(8) 0.356(14) 0.093(4) -0.082(6) -0.009(5) 0.054(8) O24 0.288(13) 0.149(6) 0.343(13) -0.129(7) 0.098(10) -0.041(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O10 1.733(5) . ? U1 O20 1.768(7) . ? U1 O4 2.266(6) . ? U1 O2 2.358(3) . ? U1 O3 2.360(4) . ? U1 O1 2.364(3) . ? U1 O5 2.371(4) . ? O1 S1 1.241(4) . ? O1 S1' 1.490(5) . ? S1 C11 1.664(11) . ? S1 C12 1.877(10) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? S1' C11' 1.685(12) . ? S1' C12' 1.883(11) . ? C11' H11D 0.96 . ? C11' H11E 0.96 . ? C11' H11F 0.96 . ? C12' H12D 0.96 . ? C12' H12E 0.96 . ? C12' H12F 0.96 . ? O2 S2' 1.334(5) . ? O2 S2 1.476(4) . ? S2 C21 1.692(10) . ? S2 C22 1.875(11) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? S2' C21' 1.638(10) . ? S2' C22' 1.834(11) . ? C21' H21D 0.96 . ? C21' H21E 0.96 . ? C21' H21F 0.96 . ? C22' H22D 0.96 . ? C22' H22E 0.96 . ? C22' H22F 0.96 . ? O3 S3 1.374(5) . ? O3 S3' 1.486(6) . ? S3 C31 1.605(11) . ? S3 C32 1.838(11) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? S3' C31' 1.647(11) . ? S3' C32' 1.821(10) . ? C31' H31D 0.96 . ? C31' H31E 0.96 . ? C31' H31F 0.96 . ? C32' H32D 0.96 . ? C32' H32E 0.96 . ? C32' H32F 0.96 . ? O4 S4 1.402(7) . ? O4 S4' 1.450(7) . ? S4 C41 1.568(12) . ? S4 C42 1.808(11) . ? C41 H41A 0.96 . ? C41 H41B 0.96 . ? C41 H41C 0.96 . ? C42 H42A 0.96 . ? C42 H42B 0.96 . ? C42 H42C 0.96 . ? S4' C41' 1.650(12) . ? S4' C42' 1.893(13) . ? C41' H41D 0.96 . ? C41' H41E 0.96 . ? C41' H41F 0.96 . ? C42' H42D 0.96 . ? C42' H42E 0.96 . ? C42' H42F 0.96 . ? O5 S5' 1.247(5) . ? O5 S5 1.435(6) . ? S5 C51 1.680(12) . ? S5 C52 1.882(11) . ? C51 H51A 0.96 . ? C51 H51B 0.96 . ? C51 H51C 0.96 . ? C52 H52A 0.96 . ? C52 H52B 0.96 . ? C52 H52C 0.96 . ? S5' C51' 1.612(12) . ? S5' C52' 1.833(10) . ? C51' H51D 0.96 . ? C51' H51E 0.96 . ? C51' H51F 0.96 . ? C52' H52D 0.96 . ? C52' H52E 0.96 . ? C52' H52F 0.96 . ? Cl1 O14 1.238(8) . ? Cl1 O13 1.298(6) . ? Cl1 O12 1.347(8) . ? Cl1 O11 1.351(8) . ? Cl2 O24 1.275(8) . ? Cl2 O22 1.279(10) . ? Cl2 O21 1.339(7) . ? Cl2 O23 1.365(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 U1 O20 172.4(4) . . ? O10 U1 O4 84.6(2) . . ? O20 U1 O4 100.7(3) . . ? O10 U1 O2 90.9(2) . . ? O20 U1 O2 82.2(3) . . ? O4 U1 O2 158.0(2) . . ? O10 U1 O3 78.9(2) . . ? O20 U1 O3 97.3(2) . . ? O4 U1 O3 73.1(2) . . ? O2 U1 O3 84.91(17) . . ? O10 U1 O1 82.56(19) . . ? O20 U1 O1 95.62(19) . . ? O4 U1 O1 146.3(2) . . ? O2 U1 O1 53.25(14) . . ? O3 U1 O1 133.70(16) . . ? O10 U1 O5 98.5(3) . . ? O20 U1 O5 88.9(3) . . ? O4 U1 O5 58.7(2) . . ? O2 U1 O5 143.24(16) . . ? O3 U1 O5 131.72(19) . . ? O1 U1 O5 92.67(15) . . ? S1 O1 U1 160.6(4) . . ? S1' O1 U1 123.0(2) . . ? O1 S1 C11 135.2(6) . . ? O1 S1 C12 115.3(5) . . ? C11 S1 C12 98.5(6) . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 S1' C11' 115.7(6) . . ? O1 S1' C12' 92.3(5) . . ? C11' S1' C12' 97.4(6) . . ? S1' C11' H11D 109.5 . . ? S1' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? S1' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? S1' C12' H12D 109.5 . . ? S1' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? S1' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? S2' O2 U1 170.5(3) . . ? S2 O2 U1 125.2(3) . . ? O2 S2 C21 102.9(5) . . ? O2 S2 C22 107.3(4) . . ? C21 S2 C22 97.4(6) . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 S2' C21' 113.1(6) . . ? O2 S2' C22' 123.0(5) . . ? C21' S2' C22' 104.0(6) . . ? S2' C21' H21D 109.5 . . ? S2' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? S2' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? S2' C22' H22D 109.5 . . ? S2' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? S2' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? S3 O3 U1 159.1(4) . . ? S3' O3 U1 135.1(3) . . ? O3 S3 C31 120.1(6) . . ? O3 S3 C32 114.6(6) . . ? C31 S3 C32 100.6(8) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O3 S3' C31' 106.1(6) . . ? O3 S3' C32' 106.7(6) . . ? C31' S3' C32' 102.4(6) . . ? S3' C31' H31D 109.5 . . ? S3' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? S3' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? S3' C32' H32D 109.5 . . ? S3' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? S3' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? S4 O4 U1 170.0(5) . . ? S4' O4 U1 141.1(5) . . ? O4 S4 C41 94.3(8) . . ? O4 S4 C42 112.6(7) . . ? C41 S4 C42 125.2(8) . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 S4' C41' 129.4(7) . . ? O4 S4' C42' 100.1(7) . . ? C41' S4' C42' 88.6(8) . . ? S4' C41' H41D 109.5 . . ? S4' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? S4' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? S4' C42' H42D 109.5 . . ? S4' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? S4' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? S5' O5 U1 158.5(4) . . ? S5 O5 U1 130.0(3) . . ? O5 S5 C51 116.0(6) . . ? O5 S5 C52 101.3(6) . . ? C51 S5 C52 95.7(6) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O5 S5' C51' 113.1(6) . . ? O5 S5' C52' 125.3(5) . . ? C51' S5' C52' 102.1(7) . . ? S5' C51' H51D 109.5 . . ? S5' C51' H51E 109.5 . . ? H51D C51' H51E 109.5 . . ? S5' C51' H51F 109.5 . . ? H51D C51' H51F 109.5 . . ? H51E C51' H51F 109.5 . . ? S5' C52' H52D 109.5 . . ? S5' C52' H52E 109.5 . . ? H52D C52' H52E 109.5 . . ? S5' C52' H52F 109.5 . . ? H52D C52' H52F 109.5 . . ? H52E C52' H52F 109.5 . . ? O14 Cl1 O13 128.6(7) . . ? O14 Cl1 O12 87.4(7) . . ? O13 Cl1 O12 117.8(6) . . ? O14 Cl1 O11 101.2(8) . . ? O13 Cl1 O11 110.8(7) . . ? O12 Cl1 O11 107.6(7) . . ? O24 Cl2 O22 96.7(9) . . ? O24 Cl2 O21 99.4(7) . . ? O22 Cl2 O21 126.1(7) . . ? O24 Cl2 O23 109.8(8) . . ? O22 Cl2 O23 109.7(8) . . ? O21 Cl2 O23 112.2(6) . . ? #===END # END of CIF data_udmso5 _database_code_depnum_ccdc_archive 'CCDC 773903' #TrackingRef '- udmso5_beta.cif' _audit_creation_date 2010-03-10T20:52:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H30 Cl2 O15 S5 U' _chemical_formula_moiety 'C10 H30 O7 S5 U, 2(Cl O4)' _chemical_formula_weight 859.57 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall P_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.5740(9) _cell_length_b 12.0952(12) _cell_length_c 19.8514(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2779.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3040 _cell_measurement_theta_min 3.6589 _cell_measurement_theta_max 67.1711 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 7 0 2 0.0004 -7 0 -2 0.0138 -1 -3 -12 0.0094 3 -2 11 0.0108 1 -8 -3 0.0103 0 7 5 0.0188 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 22.283 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.523 _exptl_absorpt_correction_T_max 0.758 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0543721688 _diffrn_orient_matrix_ub_12 0.038670633 _diffrn_orient_matrix_ub_13 0.066490127 _diffrn_orient_matrix_ub_21 -0.1083420594 _diffrn_orient_matrix_ub_22 -0.0383287277 _diffrn_orient_matrix_ub_23 0.038269946 _diffrn_orient_matrix_ub_31 0.0542771485 _diffrn_orient_matrix_ub_32 -0.1148870583 _diffrn_orient_matrix_ub_33 0.0100224726 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.1275 _diffrn_reflns_av_unetI/netI 0.0983 _diffrn_reflns_number 24664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 67.81 _diffrn_reflns_theta_full 67.81 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 4954 _reflns_number_gt 3963 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0106P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4954 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.036(8) _refine_diff_density_max 1.587 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.179 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.77584(3) 0.26506(3) 0.655585(17) 0.02151(9) Uani 1 1 d . . . O10 O 0.8884(6) 0.1721(6) 0.6730(3) 0.0244(18) Uani 1 1 d . . . O20 O 0.6637(6) 0.3598(6) 0.6370(4) 0.0230(18) Uani 1 1 d . . . O1 O 0.6394(8) 0.1501(7) 0.7129(4) 0.033(2) Uani 1 1 d . . . S1 S 0.5720(3) 0.1682(2) 0.77890(14) 0.0257(6) Uani 1 1 d . . . C11 C 0.6531(10) 0.0947(9) 0.8403(6) 0.033(3) Uani 1 1 d . . . H11A H 0.6676 0.0193 0.8243 0.05 Uiso 1 1 calc R . . H11B H 0.6096 0.0919 0.8826 0.05 Uiso 1 1 calc R . . H11C H 0.727 0.1324 0.8479 0.05 Uiso 1 1 calc R . . C12 C 0.4548(11) 0.0738(10) 0.7702(7) 0.037(3) Uani 1 1 d . . . H12A H 0.3944 0.1072 0.7422 0.055 Uiso 1 1 calc R . . H12B H 0.4231 0.0566 0.8148 0.055 Uiso 1 1 calc R . . H12C H 0.4823 0.0056 0.7489 0.055 Uiso 1 1 calc R . . O2 O 0.6963(8) 0.1395(6) 0.5783(4) 0.032(2) Uani 1 1 d . . . S2 S 0.6566(3) 0.0184(2) 0.57176(14) 0.0262(6) Uani 1 1 d . . . C21 C 0.7509(11) -0.0590(8) 0.6252(6) 0.035(4) Uani 1 1 d . . . H21A H 0.8312 -0.0395 0.6153 0.053 Uiso 1 1 calc R . . H21B H 0.7393 -0.1382 0.6173 0.053 Uiso 1 1 calc R . . H21C H 0.7337 -0.0419 0.6724 0.053 Uiso 1 1 calc R . . C22 C 0.7160(14) -0.0228(9) 0.4921(5) 0.035(3) Uani 1 1 d . . . H22A H 0.6911 0.0293 0.4572 0.053 Uiso 1 1 calc R . . H22B H 0.6887 -0.0972 0.4808 0.053 Uiso 1 1 calc R . . H22C H 0.8005 -0.0228 0.4949 0.053 Uiso 1 1 calc R . . O3 O 0.8600(7) 0.3091(6) 0.5507(4) 0.0281(19) Uani 1 1 d . . . S3 S 0.9688(3) 0.3012(2) 0.50656(15) 0.0291(7) Uani 1 1 d . . . C31 C 1.0433(11) 0.1815(10) 0.5341(6) 0.035(3) Uani 1 1 d . . . H31A H 1.0707 0.1927 0.5803 0.053 Uiso 1 1 calc R . . H31B H 1.1095 0.1678 0.5044 0.053 Uiso 1 1 calc R . . H31C H 0.991 0.1178 0.5328 0.053 Uiso 1 1 calc R . . C32 C 0.9149(9) 0.2511(12) 0.4279(5) 0.035(3) Uani 1 1 d . . . H32A H 0.8688 0.1843 0.4356 0.052 Uiso 1 1 calc R . . H32B H 0.9798 0.2336 0.3981 0.052 Uiso 1 1 calc R . . H32C H 0.8665 0.3079 0.4069 0.052 Uiso 1 1 calc R . . O4 O 0.8950(6) 0.4214(6) 0.6741(4) 0.0219(18) Uani 1 1 d . . . S4 S 0.9409(3) 0.5137(2) 0.62718(14) 0.0281(7) Uani 1 1 d . . . C41 C 1.0212(12) 0.5986(10) 0.6827(7) 0.038(3) Uani 1 1 d . . . H41A H 0.9701 0.6267 0.7182 0.056 Uiso 1 1 calc R . . H41B H 1.0542 0.6608 0.6577 0.056 Uiso 1 1 calc R . . H41C H 1.0836 0.5552 0.7031 0.056 Uiso 1 1 calc R . . C42 C 0.8201(12) 0.6021(11) 0.6121(7) 0.044(4) Uani 1 1 d . . . H42A H 0.7578 0.5596 0.5909 0.066 Uiso 1 1 calc R . . H42B H 0.8433 0.6625 0.5821 0.066 Uiso 1 1 calc R . . H42C H 0.7928 0.6327 0.6549 0.066 Uiso 1 1 calc R . . O5 O 0.7746(9) 0.3112(5) 0.7729(3) 0.0329(18) Uani 1 1 d . . . S5 S 0.7820(3) 0.4300(2) 0.80119(13) 0.0277(6) Uani 1 1 d . . . C51 C 0.9270(10) 0.4437(8) 0.8323(6) 0.027(3) Uani 1 1 d . . . H51A H 0.9378 0.3946 0.871 0.041 Uiso 1 1 calc R . . H51B H 0.9406 0.5204 0.846 0.041 Uiso 1 1 calc R . . H51C H 0.9817 0.4235 0.7967 0.041 Uiso 1 1 calc R . . C52 C 0.7056(14) 0.4195(10) 0.8801(6) 0.040(4) Uani 1 1 d . . . H52A H 0.6236 0.4049 0.8713 0.06 Uiso 1 1 calc R . . H52B H 0.7133 0.489 0.905 0.06 Uiso 1 1 calc R . . H52C H 0.7382 0.3589 0.9068 0.06 Uiso 1 1 calc R . . Cl1 Cl 0.7887(3) 0.79440(19) 0.79871(13) 0.0271(6) Uani 1 1 d . . . O11 O 0.8282(7) 0.8626(6) 0.8540(4) 0.033(2) Uani 1 1 d . . . O12 O 0.6721(8) 0.8216(7) 0.7820(4) 0.038(2) Uani 1 1 d . . . O13 O 0.8632(8) 0.8122(7) 0.7420(4) 0.040(2) Uani 1 1 d . . . O14 O 0.7946(9) 0.6791(6) 0.8192(4) 0.035(2) Uani 1 1 d . . . Cl2 Cl 0.4787(3) 0.2005(2) 0.98579(14) 0.0337(7) Uani 1 1 d . . . O21 O 0.4314(7) 0.2446(9) 0.9248(4) 0.053(2) Uani 1 1 d . . . O22 O 0.5993(8) 0.2257(9) 0.9883(5) 0.056(3) Uani 1 1 d . . . O23 O 0.4220(8) 0.2518(9) 1.0424(4) 0.055(3) Uani 1 1 d . . . O24 O 0.4650(11) 0.0816(7) 0.9870(6) 0.058(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02241(14) 0.02597(17) 0.01616(13) 0.00003(16) -0.00017(18) -0.00165(16) O10 0.023(4) 0.030(4) 0.020(4) 0.003(3) -0.006(3) 0.006(3) O20 0.020(4) 0.022(4) 0.027(5) -0.003(3) -0.003(3) 0.000(3) O1 0.041(6) 0.038(5) 0.018(4) 0.001(4) 0.001(4) -0.011(4) S1 0.0265(16) 0.0260(16) 0.0245(15) 0.0028(12) 0.0002(12) -0.0013(12) C11 0.032(7) 0.050(7) 0.018(6) 0.006(7) -0.011(6) 0.011(5) C12 0.032(8) 0.031(7) 0.047(8) -0.001(6) 0.019(6) -0.011(6) O2 0.057(7) 0.019(4) 0.021(4) -0.004(3) -0.007(4) -0.008(4) S2 0.0256(17) 0.0302(17) 0.0228(14) -0.0001(12) 0.0004(12) -0.0006(12) C21 0.050(12) 0.023(6) 0.033(6) 0.013(5) -0.003(6) -0.001(5) C22 0.055(8) 0.027(6) 0.023(6) -0.009(5) -0.010(7) 0.005(7) O3 0.034(5) 0.035(5) 0.015(4) 0.005(3) 0.005(4) -0.004(3) S3 0.0305(16) 0.0321(17) 0.0248(14) 0.0011(12) 0.0028(13) -0.0023(13) C31 0.029(8) 0.055(9) 0.022(6) 0.006(6) -0.008(6) 0.008(6) C32 0.038(7) 0.052(9) 0.014(5) -0.003(6) -0.006(4) 0.012(7) O4 0.027(4) 0.014(4) 0.025(5) -0.007(3) -0.003(3) -0.012(3) S4 0.0305(17) 0.0292(17) 0.0246(14) 0.0004(12) 0.0031(12) -0.0057(13) C41 0.041(9) 0.025(7) 0.047(8) 0.005(6) -0.007(7) -0.018(6) C42 0.041(9) 0.046(9) 0.045(9) 0.005(7) -0.015(7) -0.003(6) O5 0.044(5) 0.030(4) 0.025(4) 0.002(3) 0.001(4) -0.010(4) S5 0.0282(15) 0.0309(15) 0.0239(14) -0.0037(10) -0.0010(15) -0.0018(15) C51 0.031(7) 0.017(6) 0.033(8) -0.002(5) 0.006(6) -0.006(5) C52 0.060(11) 0.035(7) 0.024(6) -0.006(5) 0.019(7) -0.010(7) Cl1 0.0317(18) 0.0263(15) 0.0232(12) -0.0009(10) 0.0014(13) 0.0015(13) O11 0.042(5) 0.028(4) 0.028(5) -0.010(4) -0.003(4) 0.000(3) O12 0.034(5) 0.046(6) 0.034(5) -0.001(4) -0.003(4) 0.005(4) O13 0.031(5) 0.062(6) 0.026(5) 0.008(4) 0.003(4) 0.001(4) O14 0.046(6) 0.022(4) 0.036(5) -0.002(3) -0.003(4) 0.005(4) Cl2 0.0399(18) 0.0358(19) 0.0254(15) 0.0033(12) -0.0013(14) 0.0055(13) O21 0.061(6) 0.062(7) 0.035(4) 0.001(5) -0.007(4) 0.013(6) O22 0.037(5) 0.068(7) 0.062(6) -0.017(6) -0.015(5) 0.000(5) O23 0.082(7) 0.052(6) 0.029(4) 0.010(5) 0.018(4) 0.020(6) O24 0.078(8) 0.027(6) 0.070(8) 0.000(5) 0.022(6) -0.003(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O10 1.755(7) . ? U1 O20 1.770(7) . ? U1 O2 2.346(7) . ? U1 O3 2.360(7) . ? U1 O4 2.369(7) . ? U1 O1 2.392(8) . ? U1 O5 2.396(7) . ? O1 S1 1.540(9) . ? S1 C11 1.778(11) . ? S1 C12 1.782(12) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? O2 S2 1.541(8) . ? S2 C21 1.787(11) . ? S2 C22 1.794(12) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? O3 S3 1.536(8) . ? S3 C31 1.772(12) . ? S3 C32 1.788(10) . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? O4 S4 1.548(8) . ? S4 C41 1.770(12) . ? S4 C42 1.786(14) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? O5 S5 1.545(7) . ? S5 C51 1.796(12) . ? S5 C52 1.804(11) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? Cl1 O12 1.429(9) . ? Cl1 O13 1.434(9) . ? Cl1 O11 1.447(8) . ? Cl1 O14 1.454(7) . ? Cl2 O22 1.430(10) . ? Cl2 O21 1.431(9) . ? Cl2 O23 1.442(9) . ? Cl2 O24 1.448(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 U1 O20 179.1(4) . . ? O10 U1 O2 90.3(3) . . ? O20 U1 O2 89.7(3) . . ? O10 U1 O3 90.7(3) . . ? O20 U1 O3 88.4(3) . . ? O2 U1 O3 74.4(3) . . ? O10 U1 O4 92.8(3) . . ? O20 U1 O4 86.7(3) . . ? O2 U1 O4 147.8(3) . . ? O3 U1 O4 73.5(3) . . ? O10 U1 O1 91.4(3) . . ? O20 U1 O1 89.5(3) . . ? O2 U1 O1 71.1(3) . . ? O3 U1 O1 145.4(3) . . ? O4 U1 O1 140.8(3) . . ? O10 U1 O5 87.8(3) . . ? O20 U1 O5 92.7(3) . . ? O2 U1 O5 141.6(3) . . ? O3 U1 O5 143.9(3) . . ? O4 U1 O5 70.5(3) . . ? O1 U1 O5 70.6(3) . . ? S1 O1 U1 131.0(5) . . ? O1 S1 C11 104.2(6) . . ? O1 S1 C12 102.2(5) . . ? C11 S1 C12 98.5(6) . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S2 O2 U1 142.0(4) . . ? O2 S2 C21 105.4(5) . . ? O2 S2 C22 103.0(5) . . ? C21 S2 C22 98.3(6) . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S3 O3 U1 145.8(5) . . ? O3 S3 C31 105.9(5) . . ? O3 S3 C32 103.5(5) . . ? C31 S3 C32 99.3(6) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? S4 O4 U1 133.0(4) . . ? O4 S4 C41 102.9(5) . . ? O4 S4 C42 105.3(6) . . ? C41 S4 C42 99.7(7) . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? S5 O5 U1 124.7(4) . . ? O5 S5 C51 105.2(5) . . ? O5 S5 C52 102.8(5) . . ? C51 S5 C52 99.6(7) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O12 Cl1 O13 110.6(5) . . ? O12 Cl1 O11 110.1(5) . . ? O13 Cl1 O11 108.7(5) . . ? O12 Cl1 O14 109.3(6) . . ? O13 Cl1 O14 109.6(5) . . ? O11 Cl1 O14 108.6(5) . . ? O22 Cl2 O21 108.9(6) . . ? O22 Cl2 O23 109.0(6) . . ? O21 Cl2 O23 109.0(5) . . ? O22 Cl2 O24 108.5(7) . . ? O21 Cl2 O24 110.0(7) . . ? O23 Cl2 O24 111.4(6) . . ?