#------------------------------------------------------------------------------ #$Date: 2020-01-03 03:49:58 +0200 (Fri, 03 Jan 2020) $ #$Revision: 246444 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/57/7125709.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7125709 loop_ _publ_author_name 'Maria, Leonor' 'Bandeira, Nuno A. G.' 'Mar\,calo, Joaquim' 'Santos, Isabel C.' 'Gibson, John K.' _publ_section_title ; CO2 conversion to phenyl isocyanates by uranium(vi) bis(imido) complexes. ; _journal_issue 3 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 431 _journal_page_last 434 _journal_paper_doi 10.1039/c9cc07411b _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C48 H75 N5 O3 U' _chemical_formula_sum 'C48 H75 N5 O3 U' _chemical_formula_weight 1008.16 _chemical_properties_physical Air-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-09-19 deposited with the CCDC. 2019-12-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.1120(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.5464(6) _cell_length_b 13.2994(5) _cell_length_c 23.2853(8) _cell_measurement_reflns_used 9507 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.36 _cell_measurement_theta_min 2.72 _cell_volume 4688.9(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Mercury Macrae et al,2008)' _computing_publication_material 'WinGX (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_unetI/netI 0.0580 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 37084 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.680 _diffrn_reflns_theta_min 3.126 _exptl_absorpt_coefficient_mu 3.506 _exptl_absorpt_correction_T_max 0.8172 _exptl_absorpt_correction_T_min 0.6396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.428 _exptl_crystal_description prism _exptl_crystal_F_000 2056 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.088 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.106 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 527 _refine_ls_number_reflns 8873 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0338 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.0739 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6940 _reflns_number_total 8873 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc07411b2.cif _cod_data_source_block comp_4 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7125709 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.640 _shelx_estimated_absorpt_t_max 0.817 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL LM220N in P2(1)/n CELL 0.71073 15.5464 13.2994 23.2853 90.000 103.112 90.000 ZERR 4.00 0.0006 0.0005 0.0008 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O U UNIT 192 300 20 12 4 MERG 2 OMIT 0.00 180.00 OMIT 1 1 2 OMIT 0 2 0 OMIT 2 1 0 OMIT -2 1 1 OMIT 0 1 3 OMIT 0 2 1 OMIT 1 0 3 OMIT -2 0 10 OMIT 6 1 7 OMIT 1 5 4 OMIT -2 1 11 OMIT 1 1 9 OMIT -2 2 9 shel 7 0.82 ISOR 0.0010 0.20 C36 FMAP 2 PLAN 3 SIZE 0.060 0.080 0.140 ACTA BOND $H L.S. 3 TEMP -123.00 WGHT 0.032400 FVAR 0.21550 U1 5 0.703534 0.364320 0.898548 11.00000 0.01305 0.01881 = 0.02088 0.00158 0.00128 -0.00079 O1 4 0.821048 0.388726 0.864988 11.00000 0.01409 0.02227 = 0.02640 0.00288 0.00305 0.00103 O2 4 0.634740 0.508909 0.893740 11.00000 0.01482 0.02368 = 0.02647 0.00065 0.00237 0.00402 O3 4 0.762662 0.397418 0.971196 11.00000 0.02218 0.02465 = 0.02287 0.00135 -0.00079 -0.00053 N1 3 0.546547 0.308294 0.927685 11.00000 0.01550 0.02870 = 0.02698 0.00444 0.00611 0.00001 N2 3 0.548915 0.084541 0.882661 11.00000 0.02261 0.02824 = 0.02988 0.00568 -0.00023 -0.01120 N3 3 0.797007 0.186852 0.925310 11.00000 0.01422 0.02106 = 0.02355 -0.00085 -0.00119 -0.00216 N4 3 0.724914 0.146060 1.038442 11.00000 0.02250 0.02355 = 0.02666 0.00588 0.00242 -0.00557 N5 3 0.642697 0.337821 0.820667 11.00000 0.01493 0.01645 = 0.02410 -0.00328 0.00059 -0.00137 C1 1 0.477202 0.257418 0.880434 11.00000 0.01424 0.03485 = 0.02974 0.00253 -0.00138 -0.00816 AFIX 23 H1A 2 0.450537 0.309005 0.851119 11.00000 -1.20000 H1B 2 0.429939 0.232510 0.898980 11.00000 -1.20000 AFIX 0 C2 1 0.507271 0.170528 0.847595 11.00000 0.02062 0.03554 = 0.02738 -0.00180 -0.00259 -0.01392 AFIX 23 H2A 2 0.455294 0.145370 0.818301 11.00000 -1.20000 H2B 2 0.549575 0.197164 0.825375 11.00000 -1.20000 AFIX 0 C3 1 0.484432 0.021671 0.901294 11.00000 0.02854 0.04725 = 0.05062 0.01012 0.00504 -0.01546 AFIX 137 H3C 2 0.445742 -0.009196 0.866666 11.00000 -1.50000 H3B 2 0.449017 0.062705 0.922230 11.00000 -1.50000 H3A 2 0.514822 -0.031118 0.927617 11.00000 -1.50000 AFIX 0 C4 1 0.602990 0.026595 0.851338 11.00000 0.03286 0.02503 = 0.02794 -0.00432 -0.00076 -0.01449 AFIX 23 H4A 2 0.569489 0.014440 0.810418 11.00000 -1.20000 H4B 2 0.616920 -0.039460 0.870833 11.00000 -1.20000 AFIX 0 C5 1 0.688506 0.081345 0.850156 11.00000 0.02851 0.02232 = 0.02218 -0.00074 0.00369 0.00024 AFIX 23 H5B 2 0.675155 0.148142 0.831498 11.00000 -1.20000 H5A 2 0.722746 0.042354 0.826777 11.00000 -1.20000 AFIX 0 C6 1 0.742268 0.093717 0.913196 11.00000 0.02616 0.01609 = 0.02781 0.00384 -0.00140 -0.00384 AFIX 23 H6B 2 0.701135 0.092690 0.940010 11.00000 -1.20000 H6A 2 0.781860 0.034865 0.923062 11.00000 -1.20000 AFIX 0 C7 1 0.850692 0.178459 0.987460 11.00000 0.01971 0.02260 = 0.02564 0.00411 -0.00148 -0.00123 AFIX 23 H7B 2 0.901914 0.224246 0.991421 11.00000 -1.20000 H7A 2 0.874334 0.109141 0.992999 11.00000 -1.20000 AFIX 0 C8 1 0.806269 0.201007 1.037823 11.00000 0.02463 0.02442 = 0.02275 0.00558 -0.00386 -0.00622 AFIX 23 H8B 2 0.849284 0.187032 1.075347 11.00000 -1.20000 H8A 2 0.792863 0.273831 1.037056 11.00000 -1.20000 AFIX 0 C9 1 0.745082 0.043782 1.059084 11.00000 0.03665 0.02482 = 0.04663 0.00985 0.00444 -0.00589 AFIX 137 H9B 2 0.775516 0.044899 1.100832 11.00000 -1.50000 H9A 2 0.783211 0.012109 1.036061 11.00000 -1.50000 H9C 2 0.690122 0.005354 1.054282 11.00000 -1.50000 AFIX 0 C10 1 0.670299 0.198911 1.072031 11.00000 0.03757 0.03542 = 0.02297 0.00308 0.00721 -0.00841 AFIX 23 H10B 2 0.708343 0.224906 1.109021 11.00000 -1.20000 H10A 2 0.627683 0.151087 1.082712 11.00000 -1.20000 AFIX 0 C11 1 0.620049 0.285879 1.037419 11.00000 0.02463 0.03101 = 0.02554 0.00046 0.00500 0.00082 AFIX 23 H11B 2 0.662139 0.333946 1.026333 11.00000 -1.20000 H11A 2 0.585843 0.321837 1.062091 11.00000 -1.20000 AFIX 0 C12 1 0.557499 0.245265 0.981909 11.00000 0.02144 0.03157 = 0.03065 0.00682 0.00498 -0.00319 AFIX 23 H12B 2 0.579008 0.178162 0.973202 11.00000 -1.20000 H12A 2 0.498603 0.235760 0.990637 11.00000 -1.20000 AFIX 0 C13 1 0.859250 0.185807 0.884722 11.00000 0.02054 0.02106 = 0.02590 0.00021 0.00563 -0.00026 AFIX 23 H13A 2 0.888118 0.119080 0.887423 11.00000 -1.20000 H13B 2 0.824442 0.193983 0.843763 11.00000 -1.20000 AFIX 0 C14 1 0.929218 0.264505 0.896472 11.00000 0.01678 0.02128 = 0.02035 0.00059 0.00548 -0.00060 C15 1 1.017396 0.237518 0.916871 11.00000 0.01922 0.02003 = 0.02831 0.00266 0.00413 0.00620 AFIX 43 H15 2 1.031539 0.168416 0.923725 11.00000 -1.20000 AFIX 0 C16 1 1.085184 0.307038 0.927562 11.00000 0.01740 0.02703 = 0.01771 0.00005 0.00582 0.00452 C17 1 1.181889 0.272690 0.948337 11.00000 0.01739 0.03089 = 0.02921 -0.00036 0.00282 0.00313 C18 1 1.190957 0.199904 1.000469 11.00000 0.02567 0.03194 = 0.03865 0.00298 0.00224 0.00796 AFIX 137 H18C 2 1.252450 0.177567 1.012896 11.00000 -1.50000 H18B 2 1.152632 0.141526 0.988459 11.00000 -1.50000 H18A 2 1.173584 0.234116 1.033360 11.00000 -1.50000 AFIX 0 C19 1 1.207563 0.217405 0.896440 11.00000 0.02617 0.04494 = 0.04337 0.00051 0.01433 0.00980 AFIX 137 H19A 2 1.201956 0.263477 0.862947 11.00000 -1.50000 H19B 2 1.168284 0.159676 0.884852 11.00000 -1.50000 H19C 2 1.268762 0.193937 0.908547 11.00000 -1.50000 AFIX 0 C20 1 1.245348 0.360067 0.967827 11.00000 0.01446 0.04150 = 0.03898 0.00162 0.00788 0.00131 AFIX 137 H20A 2 1.225870 0.399072 0.998262 11.00000 -1.50000 H20C 2 1.246073 0.403419 0.933908 11.00000 -1.50000 H20B 2 1.304874 0.333850 0.983834 11.00000 -1.50000 AFIX 0 C21 1 1.061667 0.406717 0.916574 11.00000 0.01761 0.02544 = 0.02185 -0.00245 0.00527 -0.00393 AFIX 43 H21 2 1.107564 0.455416 0.923989 11.00000 -1.20000 AFIX 0 C22 1 0.974895 0.441154 0.895259 11.00000 0.01601 0.02062 = 0.01606 -0.00181 0.00401 -0.00064 C23 1 0.953204 0.551711 0.880118 11.00000 0.01753 0.02444 = 0.02814 0.00377 0.00639 -0.00109 C24 1 0.885148 0.593154 0.912589 11.00000 0.02596 0.02715 = 0.03401 -0.00429 0.00926 0.00248 AFIX 137 H24A 2 0.908105 0.586512 0.955233 11.00000 -1.50000 H24B 2 0.829950 0.555163 0.900732 11.00000 -1.50000 H24C 2 0.873954 0.664237 0.902525 11.00000 -1.50000 AFIX 0 C25 1 0.918526 0.561070 0.813419 11.00000 0.03352 0.03207 = 0.03107 0.00884 0.01168 0.00329 AFIX 137 H25B 2 0.902780 0.631244 0.803284 11.00000 -1.50000 H25A 2 0.866180 0.518490 0.800872 11.00000 -1.50000 H25C 2 0.964393 0.539473 0.793355 11.00000 -1.50000 AFIX 0 C26 1 1.034929 0.618099 0.898146 11.00000 0.02548 0.02285 = 0.06505 -0.00383 0.00908 -0.00285 AFIX 137 H26C 2 1.060003 0.610482 0.940499 11.00000 -1.50000 H26A 2 1.018424 0.688508 0.889408 11.00000 -1.50000 H26B 2 1.078853 0.597947 0.876109 11.00000 -1.50000 AFIX 0 C27 1 0.907693 0.366163 0.886122 11.00000 0.01440 0.02502 = 0.02030 0.00263 0.00479 0.00078 C28 1 0.509315 0.407667 0.940173 11.00000 0.01398 0.03156 = 0.02764 0.00035 0.00629 0.00339 AFIX 23 H28A 2 0.553203 0.441639 0.971655 11.00000 -1.20000 H28B 2 0.456042 0.395152 0.955695 11.00000 -1.20000 AFIX 0 C29 1 0.484757 0.478119 0.888591 11.00000 0.02126 0.03172 = 0.02353 0.00113 0.00389 0.00774 C30 1 0.550165 0.530865 0.868266 11.00000 0.01557 0.02253 = 0.02149 -0.00157 0.00195 0.00340 C31 1 0.526425 0.605408 0.824094 11.00000 0.02676 0.02189 = 0.02095 -0.00237 0.00055 0.00346 C32 1 0.436510 0.614045 0.798116 11.00000 0.03060 0.03093 = 0.01867 -0.00192 0.00295 0.01262 AFIX 43 H32 2 0.419408 0.662102 0.767464 11.00000 -1.20000 AFIX 0 C33 1 0.370647 0.557962 0.813658 11.00000 0.02124 0.04668 = 0.02438 -0.00381 0.00634 0.01298 C34 1 0.395598 0.491670 0.860862 11.00000 0.01840 0.04423 = 0.02290 -0.00089 0.00460 -0.00057 AFIX 43 H34 2 0.351561 0.455159 0.874433 11.00000 -1.20000 AFIX 0 C35 1 0.274340 0.564472 0.778295 11.00000 0.01764 0.07756 = 0.02950 0.00375 0.00548 0.01286 C36 1 0.209950 0.526507 0.810441 11.00000 0.02828 10.10538 = 0.09275 0.03934 0.00984 0.00677 AFIX 137 H36A 2 0.150496 0.548204 0.790337 11.00000 -1.50000 H36B 2 0.224077 0.553100 0.850741 11.00000 -1.50000 H36C 2 0.212313 0.452885 0.811693 11.00000 -1.50000 AFIX 0 C37 1 0.248601 0.678275 0.765469 11.00000 0.04825 0.09727 = 0.08968 -0.01307 -0.02162 0.03502 AFIX 137 H37A 2 0.189867 0.682430 0.739049 11.00000 -1.50000 H37B 2 0.291956 0.710499 0.746782 11.00000 -1.50000 H37C 2 0.247979 0.712633 0.802605 11.00000 -1.50000 AFIX 0 C38 1 0.266787 0.514667 0.720593 11.00000 0.03578 0.10254 = 0.06160 -0.02816 -0.00477 -0.00539 AFIX 137 H38A 2 0.273912 0.441901 0.726422 11.00000 -1.50000 H38B 2 0.312858 0.540244 0.701872 11.00000 -1.50000 H38C 2 0.208586 0.528845 0.695241 11.00000 -1.50000 AFIX 0 C39 1 0.595185 0.674010 0.807171 11.00000 0.03160 0.01958 = 0.03068 0.00528 0.00201 0.00208 C40 1 0.552897 0.755797 0.762258 11.00000 0.04196 0.02928 = 0.04081 0.01228 0.00365 0.00287 AFIX 137 H40A 2 0.509414 0.793864 0.778013 11.00000 -1.50000 H40B 2 0.523581 0.723810 0.725044 11.00000 -1.50000 H40C 2 0.598930 0.801486 0.755288 11.00000 -1.50000 AFIX 0 C41 1 0.645881 0.728171 0.862213 11.00000 0.04095 0.03027 = 0.03656 0.00060 -0.00016 -0.00311 AFIX 137 H41A 2 0.604861 0.768956 0.878743 11.00000 -1.50000 H41B 2 0.690816 0.771804 0.851800 11.00000 -1.50000 H41C 2 0.674552 0.678567 0.891477 11.00000 -1.50000 AFIX 0 C42 1 0.659059 0.613076 0.778997 11.00000 0.03715 0.02713 = 0.03545 0.00237 0.00895 -0.00585 AFIX 137 H42A 2 0.701733 0.658657 0.767473 11.00000 -1.50000 H42B 2 0.625589 0.577840 0.744051 11.00000 -1.50000 H42C 2 0.690527 0.563931 0.807527 11.00000 -1.50000 AFIX 0 C43 1 0.611000 0.356550 0.760388 11.00000 0.02406 0.01507 = 0.02468 -0.00345 0.00741 -0.00073 C44 1 0.523082 0.383330 0.738113 11.00000 0.02451 0.02806 = 0.02901 -0.00403 0.00416 -0.00201 AFIX 43 H44 2 0.483474 0.386071 0.763717 11.00000 -1.20000 AFIX 0 C45 1 0.493151 0.405922 0.679015 11.00000 0.03024 0.03908 = 0.02937 -0.00306 -0.00645 0.00011 AFIX 43 H45 2 0.433330 0.425154 0.664407 11.00000 -1.20000 AFIX 0 C46 1 0.548908 0.400812 0.641460 11.00000 0.04606 0.03196 = 0.02578 -0.00464 -0.00226 -0.00254 AFIX 43 H46 2 0.527942 0.416077 0.600833 11.00000 -1.20000 AFIX 0 C47 1 0.636289 0.373220 0.662956 11.00000 0.04403 0.02996 = 0.03053 -0.00642 0.01475 0.00027 AFIX 43 H47 2 0.675210 0.369394 0.636926 11.00000 -1.20000 AFIX 0 C48 1 0.667089 0.351225 0.722149 11.00000 0.02451 0.02171 = 0.03313 -0.00062 0.00825 0.00302 AFIX 43 H48 2 0.727051 0.332382 0.736566 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM LM220N in P2(1)/n REM R1 = 0.0338 for 6940 Fo > 4sig(Fo) and 0.0532 for all 8873 data REM 527 parameters refined using 6 restraints END WGHT 0.0326 0.0000 REM Highest difference peak 1.088, deepest hole -0.816, 1-sigma level 0.106 Q1 1 0.7301 0.3842 0.9352 11.00000 0.05 1.09 Q2 1 0.6770 0.3673 0.8551 11.00000 0.05 0.96 Q3 1 0.6754 0.3154 0.9204 11.00000 0.05 0.74 ; _shelx_res_checksum 15802 loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp U1 U 0.70353(2) 0.36432(2) 0.89855(2) 0.01799(6) Uani 1 1 d . . O1 O 0.82105(18) 0.3887(2) 0.86499(12) 0.0212(7) Uani 1 1 d . . O2 O 0.63474(18) 0.5089(2) 0.89374(12) 0.0220(7) Uani 1 1 d . . O3 O 0.76266(19) 0.3974(2) 0.97120(12) 0.0242(7) Uani 1 1 d . . N1 N 0.5465(2) 0.3083(3) 0.92769(15) 0.0235(8) Uani 1 1 d . . N2 N 0.5489(2) 0.0845(3) 0.88266(15) 0.0279(9) Uani 1 1 d . . N3 N 0.7970(2) 0.1869(3) 0.92531(14) 0.0205(8) Uani 1 1 d . . N4 N 0.7249(2) 0.1461(3) 1.03844(15) 0.0247(8) Uani 1 1 d . . N5 N 0.6427(2) 0.3378(2) 0.82067(14) 0.0191(8) Uani 1 1 d . . C1 C 0.4772(3) 0.2574(4) 0.88043(19) 0.0273(11) Uani 1 1 d . . H1A H 0.4505 0.3090 0.8511 0.033 Uiso 1 1 calc R U H1B H 0.4299 0.2325 0.8990 0.033 Uiso 1 1 calc R U C2 C 0.5073(3) 0.1705(4) 0.84759(19) 0.0291(11) Uani 1 1 d . . H2A H 0.4553 0.1454 0.8183 0.035 Uiso 1 1 calc R U H2B H 0.5496 0.1972 0.8254 0.035 Uiso 1 1 calc R U C3 C 0.4844(3) 0.0217(4) 0.9013(2) 0.0428(14) Uani 1 1 d . . H3C H 0.4457 -0.0092 0.8667 0.064 Uiso 1 1 calc R U H3B H 0.4490 0.0627 0.9222 0.064 Uiso 1 1 calc R U H3A H 0.5148 -0.0311 0.9276 0.064 Uiso 1 1 calc R U C4 C 0.6030(3) 0.0266(4) 0.85134(19) 0.0298(11) Uani 1 1 d . . H4A H 0.5695 0.0144 0.8104 0.036 Uiso 1 1 calc R U H4B H 0.6169 -0.0395 0.8708 0.036 Uiso 1 1 calc R U C5 C 0.6885(3) 0.0813(3) 0.85016(17) 0.0247(10) Uani 1 1 d . . H5B H 0.6752 0.1481 0.8315 0.030 Uiso 1 1 calc R U H5A H 0.7227 0.0424 0.8268 0.030 Uiso 1 1 calc R U C6 C 0.7423(3) 0.0937(3) 0.91320(18) 0.0246(10) Uani 1 1 d . . H6B H 0.7011 0.0927 0.9400 0.029 Uiso 1 1 calc R U H6A H 0.7819 0.0349 0.9231 0.029 Uiso 1 1 calc R U C7 C 0.8507(3) 0.1785(3) 0.98746(17) 0.0237(10) Uani 1 1 d . . H7B H 0.9019 0.2242 0.9914 0.028 Uiso 1 1 calc R U H7A H 0.8743 0.1091 0.9930 0.028 Uiso 1 1 calc R U C8 C 0.8063(3) 0.2010(3) 1.03782(17) 0.0254(10) Uani 1 1 d . . H8B H 0.8493 0.1870 1.0753 0.030 Uiso 1 1 calc R U H8A H 0.7929 0.2738 1.0371 0.030 Uiso 1 1 calc R U C9 C 0.7451(3) 0.0438(4) 1.0591(2) 0.0368(12) Uani 1 1 d . . H9B H 0.7755 0.0449 1.1008 0.055 Uiso 1 1 calc R U H9A H 0.7832 0.0121 1.0361 0.055 Uiso 1 1 calc R U H9C H 0.6901 0.0054 1.0543 0.055 Uiso 1 1 calc R U C10 C 0.6703(3) 0.1989(4) 1.07203(19) 0.0319(12) Uani 1 1 d . . H10B H 0.7083 0.2249 1.1090 0.038 Uiso 1 1 calc R U H10A H 0.6277 0.1511 1.0827 0.038 Uiso 1 1 calc R U C11 C 0.6200(3) 0.2859(4) 1.03742(18) 0.0272(11) Uani 1 1 d . . H11B H 0.6621 0.3339 1.0263 0.033 Uiso 1 1 calc R U H11A H 0.5858 0.3218 1.0621 0.033 Uiso 1 1 calc R U C12 C 0.5575(3) 0.2453(4) 0.98191(18) 0.0280(11) Uani 1 1 d . . H12B H 0.5790 0.1782 0.9732 0.034 Uiso 1 1 calc R U H12A H 0.4986 0.2358 0.9906 0.034 Uiso 1 1 calc R U C13 C 0.8593(3) 0.1858(3) 0.88472(18) 0.0224(10) Uani 1 1 d . . H13A H 0.8881 0.1191 0.8874 0.027 Uiso 1 1 calc R U H13B H 0.8244 0.1940 0.8438 0.027 Uiso 1 1 calc R U C14 C 0.9292(3) 0.2645(3) 0.89647(17) 0.0193(9) Uani 1 1 d . . C15 C 1.0174(3) 0.2375(3) 0.91687(17) 0.0227(10) Uani 1 1 d . . H15 H 1.0315 0.1684 0.9237 0.027 Uiso 1 1 calc R U C16 C 1.0852(3) 0.3070(3) 0.92756(17) 0.0204(10) Uani 1 1 d . . C17 C 1.1819(3) 0.2727(4) 0.94834(19) 0.0262(10) Uani 1 1 d . . C18 C 1.1910(3) 0.1999(4) 1.00047(19) 0.0329(12) Uani 1 1 d . . H18C H 1.2525 0.1776 1.0129 0.049 Uiso 1 1 calc R U H18B H 1.1526 0.1415 0.9885 0.049 Uiso 1 1 calc R U H18A H 1.1736 0.2341 1.0334 0.049 Uiso 1 1 calc R U C19 C 1.2076(3) 0.2174(4) 0.8964(2) 0.0371(12) Uani 1 1 d . . H19A H 1.2020 0.2635 0.8629 0.056 Uiso 1 1 calc R U H19B H 1.1683 0.1597 0.8849 0.056 Uiso 1 1 calc R U H19C H 1.2688 0.1939 0.9085 0.056 Uiso 1 1 calc R U C20 C 1.2453(3) 0.3601(4) 0.9678(2) 0.0314(11) Uani 1 1 d . . H20A H 1.2259 0.3991 0.9983 0.047 Uiso 1 1 calc R U H20C H 1.2461 0.4034 0.9339 0.047 Uiso 1 1 calc R U H20B H 1.3049 0.3339 0.9838 0.047 Uiso 1 1 calc R U C21 C 1.0617(3) 0.4067(3) 0.91657(16) 0.0215(9) Uani 1 1 d . . H21 H 1.1076 0.4554 0.9240 0.026 Uiso 1 1 calc R U C22 C 0.9749(3) 0.4412(3) 0.89526(16) 0.0175(9) Uani 1 1 d . . C23 C 0.9532(3) 0.5517(3) 0.88012(18) 0.0232(10) Uani 1 1 d . . C24 C 0.8851(3) 0.5932(4) 0.91259(19) 0.0286(10) Uani 1 1 d . . H24A H 0.9081 0.5865 0.9552 0.043 Uiso 1 1 calc R U H24B H 0.8300 0.5552 0.9007 0.043 Uiso 1 1 calc R U H24C H 0.8740 0.6642 0.9025 0.043 Uiso 1 1 calc R U C25 C 0.9185(3) 0.5611(4) 0.81342(18) 0.0315(11) Uani 1 1 d . . H25B H 0.9028 0.6312 0.8033 0.047 Uiso 1 1 calc R U H25A H 0.8662 0.5185 0.8009 0.047 Uiso 1 1 calc R U H25C H 0.9644 0.5395 0.7934 0.047 Uiso 1 1 calc R U C26 C 1.0349(3) 0.6181(3) 0.8981(2) 0.0380(13) Uani 1 1 d . . H26C H 1.0600 0.6105 0.9405 0.057 Uiso 1 1 calc R U H26A H 1.0184 0.6885 0.8894 0.057 Uiso 1 1 calc R U H26B H 1.0789 0.5979 0.8761 0.057 Uiso 1 1 calc R U C27 C 0.9077(3) 0.3662(3) 0.88612(17) 0.0198(9) Uani 1 1 d . . C28 C 0.5093(3) 0.4077(3) 0.94017(18) 0.0241(10) Uani 1 1 d . . H28A H 0.5532 0.4416 0.9717 0.029 Uiso 1 1 calc R U H28B H 0.4560 0.3952 0.9557 0.029 Uiso 1 1 calc R U C29 C 0.4848(3) 0.4781(4) 0.88859(18) 0.0257(11) Uani 1 1 d . . C30 C 0.5502(3) 0.5309(3) 0.86827(17) 0.0202(9) Uani 1 1 d . . C31 C 0.5264(3) 0.6054(3) 0.82409(17) 0.0240(10) Uani 1 1 d . . C32 C 0.4365(3) 0.6140(3) 0.79812(18) 0.0272(11) Uani 1 1 d . . H32 H 0.4194 0.6621 0.7675 0.033 Uiso 1 1 calc R U C33 C 0.3706(3) 0.5580(4) 0.81366(18) 0.0306(12) Uani 1 1 d . . C34 C 0.3956(3) 0.4917(4) 0.86086(18) 0.0285(11) Uani 1 1 d . . H34 H 0.3516 0.4552 0.8744 0.034 Uiso 1 1 calc R U C35 C 0.2743(3) 0.5645(5) 0.7783(2) 0.0415(14) Uani 1 1 d . . C36 C 0.2099(4) 0.5265(6) 0.8104(3) 0.0761(17) Uani 1 1 d . U H36A H 0.1505 0.5482 0.7903 0.114 Uiso 1 1 calc R U H36B H 0.2241 0.5531 0.8507 0.114 Uiso 1 1 calc R U H36C H 0.2123 0.4529 0.8117 0.114 Uiso 1 1 calc R U C37 C 0.2486(4) 0.6783(6) 0.7655(3) 0.084(2) Uani 1 1 d . . H37A H 0.1899 0.6824 0.7390 0.127 Uiso 1 1 calc R U H37B H 0.2920 0.7105 0.7468 0.127 Uiso 1 1 calc R U H37C H 0.2480 0.7126 0.8026 0.127 Uiso 1 1 calc R U C38 C 0.2668(4) 0.5147(5) 0.7206(2) 0.069(2) Uani 1 1 d . . H38A H 0.2739 0.4419 0.7264 0.104 Uiso 1 1 calc R U H38B H 0.3129 0.5402 0.7019 0.104 Uiso 1 1 calc R U H38C H 0.2086 0.5288 0.6952 0.104 Uiso 1 1 calc R U C39 C 0.5952(3) 0.6740(3) 0.80717(19) 0.0281(11) Uani 1 1 d . . C40 C 0.5529(3) 0.7558(4) 0.7623(2) 0.0383(13) Uani 1 1 d . . H40A H 0.5094 0.7939 0.7780 0.057 Uiso 1 1 calc R U H40B H 0.5236 0.7238 0.7250 0.057 Uiso 1 1 calc R U H40C H 0.5989 0.8015 0.7553 0.057 Uiso 1 1 calc R U C41 C 0.6459(3) 0.7282(4) 0.8622(2) 0.0374(12) Uani 1 1 d . . H41A H 0.6049 0.7690 0.8787 0.056 Uiso 1 1 calc R U H41B H 0.6908 0.7718 0.8518 0.056 Uiso 1 1 calc R U H41C H 0.6746 0.6786 0.8915 0.056 Uiso 1 1 calc R U C42 C 0.6591(3) 0.6131(3) 0.7790(2) 0.0331(12) Uani 1 1 d . . H42A H 0.7017 0.6587 0.7675 0.050 Uiso 1 1 calc R U H42B H 0.6256 0.5778 0.7441 0.050 Uiso 1 1 calc R U H42C H 0.6905 0.5639 0.8075 0.050 Uiso 1 1 calc R U C43 C 0.6110(3) 0.3565(3) 0.76039(17) 0.0210(9) Uani 1 1 d . . C44 C 0.5231(3) 0.3833(3) 0.73811(19) 0.0275(11) Uani 1 1 d . . H44 H 0.4835 0.3861 0.7637 0.033 Uiso 1 1 calc R U C45 C 0.4932(3) 0.4059(4) 0.67902(19) 0.0350(12) Uani 1 1 d . . H45 H 0.4333 0.4252 0.6644 0.042 Uiso 1 1 calc R U C46 C 0.5489(3) 0.4008(4) 0.6415(2) 0.0363(12) Uani 1 1 d . . H46 H 0.5279 0.4161 0.6008 0.044 Uiso 1 1 calc R U C47 C 0.6363(3) 0.3732(3) 0.6630(2) 0.0338(12) Uani 1 1 d . . H47 H 0.6752 0.3694 0.6369 0.041 Uiso 1 1 calc R U C48 C 0.6671(3) 0.3512(3) 0.72215(19) 0.0262(10) Uani 1 1 d . . H48 H 0.7271 0.3324 0.7366 0.031 Uiso 1 1 calc R U 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 0.01305(8) 0.01881(9) 0.02088(9) 0.00158(8) 0.00128(6) -0.00079(8) O1 0.0141(14) 0.0223(18) 0.0264(15) 0.0029(12) 0.0030(12) 0.0010(12) O2 0.0148(15) 0.0237(17) 0.0265(16) 0.0007(13) 0.0024(12) 0.0040(13) O3 0.0222(16) 0.0246(18) 0.0229(15) 0.0013(13) -0.0008(13) -0.0005(13) N1 0.0155(19) 0.029(2) 0.0270(19) 0.0044(17) 0.0061(16) 0.0000(17) N2 0.023(2) 0.028(2) 0.030(2) 0.0057(18) -0.0002(17) -0.0112(18) N3 0.0142(18) 0.021(2) 0.0236(18) -0.0009(16) -0.0012(15) -0.0022(16) N4 0.0225(19) 0.024(2) 0.0267(19) 0.0059(17) 0.0024(16) -0.0056(17) N5 0.0149(18) 0.016(2) 0.0241(18) -0.0033(14) 0.0006(15) -0.0014(14) C1 0.014(2) 0.035(3) 0.030(2) 0.003(2) -0.0014(19) -0.008(2) C2 0.021(2) 0.036(3) 0.027(2) -0.002(2) -0.003(2) -0.014(2) C3 0.029(3) 0.047(4) 0.051(3) 0.010(3) 0.005(2) -0.015(3) C4 0.033(3) 0.025(3) 0.028(2) -0.004(2) -0.001(2) -0.014(2) C5 0.029(2) 0.022(3) 0.022(2) -0.0007(19) 0.0037(19) 0.000(2) C6 0.026(2) 0.016(2) 0.028(2) 0.004(2) -0.0014(19) -0.004(2) C7 0.020(2) 0.023(2) 0.026(2) 0.0041(19) -0.0015(19) -0.001(2) C8 0.025(2) 0.024(3) 0.023(2) 0.0056(19) -0.0039(19) -0.006(2) C9 0.037(3) 0.025(3) 0.047(3) 0.010(2) 0.004(2) -0.006(2) C10 0.038(3) 0.035(3) 0.023(2) 0.003(2) 0.007(2) -0.008(2) C11 0.025(2) 0.031(3) 0.026(2) 0.000(2) 0.005(2) 0.001(2) C12 0.021(2) 0.032(3) 0.031(2) 0.007(2) 0.005(2) -0.003(2) C13 0.021(2) 0.021(3) 0.026(2) 0.0002(19) 0.0056(19) 0.000(2) C14 0.017(2) 0.021(2) 0.020(2) 0.0006(18) 0.0055(18) -0.0006(19) C15 0.019(2) 0.020(2) 0.028(2) 0.0027(19) 0.0041(19) 0.0062(19) C16 0.017(2) 0.027(3) 0.018(2) 0.0001(19) 0.0058(18) 0.005(2) C17 0.017(2) 0.031(3) 0.029(2) 0.000(2) 0.0028(19) 0.003(2) C18 0.026(3) 0.032(3) 0.039(3) 0.003(2) 0.002(2) 0.008(2) C19 0.026(3) 0.045(3) 0.043(3) 0.001(3) 0.014(2) 0.010(3) C20 0.014(2) 0.042(3) 0.039(3) 0.002(2) 0.008(2) 0.001(2) C21 0.018(2) 0.025(2) 0.022(2) -0.0024(19) 0.0053(18) -0.004(2) C22 0.016(2) 0.021(2) 0.016(2) -0.0018(17) 0.0040(17) -0.0006(18) C23 0.018(2) 0.024(3) 0.028(2) 0.0038(19) 0.0064(19) -0.0011(19) C24 0.026(2) 0.027(3) 0.034(2) -0.004(2) 0.009(2) 0.002(2) C25 0.034(3) 0.032(3) 0.031(3) 0.009(2) 0.012(2) 0.003(2) C26 0.025(3) 0.023(3) 0.065(3) -0.004(2) 0.009(2) -0.003(2) C27 0.014(2) 0.025(2) 0.020(2) 0.0026(19) 0.0048(17) 0.001(2) C28 0.014(2) 0.032(3) 0.028(2) 0.000(2) 0.0063(18) 0.003(2) C29 0.021(2) 0.032(3) 0.024(2) 0.001(2) 0.0039(19) 0.008(2) C30 0.016(2) 0.023(3) 0.021(2) -0.0016(18) 0.0020(18) 0.0034(19) C31 0.027(2) 0.022(3) 0.021(2) -0.0024(18) 0.0005(19) 0.003(2) C32 0.031(3) 0.031(3) 0.019(2) -0.0019(19) 0.0030(19) 0.013(2) C33 0.021(2) 0.047(3) 0.024(2) -0.004(2) 0.006(2) 0.013(2) C34 0.018(2) 0.044(3) 0.023(2) -0.001(2) 0.0046(19) -0.001(2) C35 0.018(2) 0.078(5) 0.030(3) 0.004(3) 0.005(2) 0.013(3) C36 0.028(3) 0.105 0.093(5) 0.039(4) 0.010(3) 0.007(4) C37 0.048(4) 0.097(6) 0.090(5) -0.013(4) -0.022(4) 0.035(4) C38 0.036(3) 0.103(6) 0.062(4) -0.028(4) -0.005(3) -0.005(4) C39 0.032(3) 0.020(2) 0.031(2) 0.005(2) 0.002(2) 0.002(2) C40 0.042(3) 0.029(3) 0.041(3) 0.012(2) 0.004(2) 0.003(2) C41 0.041(3) 0.030(3) 0.037(3) 0.001(2) 0.000(2) -0.003(2) C42 0.037(3) 0.027(3) 0.035(3) 0.002(2) 0.009(2) -0.006(2) C43 0.024(2) 0.015(2) 0.025(2) -0.0035(19) 0.0074(18) -0.0007(19) C44 0.025(2) 0.028(3) 0.029(2) -0.004(2) 0.004(2) -0.002(2) C45 0.030(3) 0.039(3) 0.029(3) -0.003(2) -0.006(2) 0.000(2) C46 0.046(3) 0.032(3) 0.026(2) -0.005(2) -0.002(2) -0.003(3) C47 0.044(3) 0.030(3) 0.031(2) -0.006(2) 0.015(2) 0.000(2) C48 0.025(2) 0.022(3) 0.033(2) -0.001(2) 0.008(2) 0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O3 U1 N5 176.37(14) O3 U1 O1 90.56(12) N5 U1 O1 87.77(13) O3 U1 O2 88.42(12) N5 U1 O2 88.99(12) O1 U1 O2 106.96(10) O3 U1 N3 82.29(11) N5 U1 N3 100.43(12) O1 U1 N3 76.50(10) O2 U1 N3 170.17(10) O3 U1 N1 97.27(12) N5 U1 N1 84.70(12) O1 U1 N1 170.59(10) O2 U1 N1 78.59(11) N3 U1 N1 99.31(10) C27 O1 U1 133.1(2) C30 O2 U1 129.0(3) C12 N1 C28 107.8(3) C12 N1 C1 106.8(3) C28 N1 C1 107.0(3) C12 N1 U1 114.8(2) C28 N1 U1 102.1(2) C1 N1 U1 117.5(2) C3 N2 C4 111.3(4) C3 N2 C2 111.7(4) C4 N2 C2 111.5(3) C6 N3 C13 107.2(3) C6 N3 C7 106.8(3) C13 N3 C7 108.1(3) C6 N3 U1 114.7(2) C13 N3 U1 104.3(2) C7 N3 U1 115.4(2) C9 N4 C10 112.5(4) C9 N4 C8 110.4(4) C10 N4 C8 112.0(4) C43 N5 U1 156.9(3) N1 C1 C2 117.2(4) N1 C1 H1A 108.0 C2 C1 H1A 108.0 N1 C1 H1B 108.0 C2 C1 H1B 108.0 H1A C1 H1B 107.2 N2 C2 C1 117.4(4) N2 C2 H2A 107.9 C1 C2 H2A 107.9 N2 C2 H2B 107.9 C1 C2 H2B 107.9 H2A C2 H2B 107.2 N2 C3 H3C 109.5 N2 C3 H3B 109.5 H3C C3 H3B 109.5 N2 C3 H3A 109.5 H3C C3 H3A 109.5 H3B C3 H3A 109.5 N2 C4 C5 111.3(4) N2 C4 H4A 109.4 C5 C4 H4A 109.4 N2 C4 H4B 109.4 C5 C4 H4B 109.4 H4A C4 H4B 108.0 C4 C5 C6 108.9(3) C4 C5 H5B 109.9 C6 C5 H5B 109.9 C4 C5 H5A 109.9 C6 C5 H5A 109.9 H5B C5 H5A 108.3 N3 C6 C5 115.8(3) N3 C6 H6B 108.3 C5 C6 H6B 108.3 N3 C6 H6A 108.3 C5 C6 H6A 108.3 H6B C6 H6A 107.4 N3 C7 C8 118.6(4) N3 C7 H7B 107.7 C8 C7 H7B 107.7 N3 C7 H7A 107.7 C8 C7 H7A 107.7 H7B C7 H7A 107.1 N4 C8 C7 117.0(4) N4 C8 H8B 108.0 C7 C8 H8B 108.0 N4 C8 H8A 108.0 C7 C8 H8A 108.0 H8B C8 H8A 107.3 N4 C9 H9B 109.5 N4 C9 H9A 109.5 H9B C9 H9A 109.5 N4 C9 H9C 109.5 H9B C9 H9C 109.5 H9A C9 H9C 109.5 N4 C10 C11 112.0(3) N4 C10 H10B 109.2 C11 C10 H10B 109.2 N4 C10 H10A 109.2 C11 C10 H10A 109.2 H10B C10 H10A 107.9 C10 C11 C12 109.3(4) C10 C11 H11B 109.8 C12 C11 H11B 109.8 C10 C11 H11A 109.8 C12 C11 H11A 109.8 H11B C11 H11A 108.3 N1 C12 C11 116.4(4) N1 C12 H12B 108.2 C11 C12 H12B 108.2 N1 C12 H12A 108.2 C11 C12 H12A 108.2 H12B C12 H12A 107.3 C14 C13 N3 115.3(3) C14 C13 H13A 108.5 N3 C13 H13A 108.5 C14 C13 H13B 108.5 N3 C13 H13B 108.5 H13A C13 H13B 107.5 C15 C14 C27 119.1(4) C15 C14 C13 120.2(4) C27 C14 C13 120.7(4) C16 C15 C14 122.7(4) C16 C15 H15 118.6 C14 C15 H15 118.6 C15 C16 C21 116.7(4) C15 C16 C17 120.6(4) C21 C16 C17 122.7(4) C20 C17 C18 108.0(4) C20 C17 C16 112.8(4) C18 C17 C16 110.1(4) C20 C17 C19 109.4(4) C18 C17 C19 109.0(4) C16 C17 C19 107.6(3) C17 C18 H18C 109.5 C17 C18 H18B 109.5 H18C C18 H18B 109.5 C17 C18 H18A 109.5 H18C C18 H18A 109.5 H18B C18 H18A 109.5 C17 C19 H19A 109.5 C17 C19 H19B 109.5 H19A C19 H19B 109.5 C17 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C17 C20 H20A 109.5 C17 C20 H20C 109.5 H20A C20 H20C 109.5 C17 C20 H20B 109.5 H20A C20 H20B 109.5 H20C C20 H20B 109.5 C16 C21 C22 124.8(4) C16 C21 H21 117.6 C22 C21 H21 117.6 C21 C22 C27 115.9(4) C21 C22 C23 122.6(4) C27 C22 C23 121.5(4) C26 C23 C25 108.2(4) C26 C23 C22 111.5(4) C25 C23 C22 108.7(4) C26 C23 C24 106.3(4) C25 C23 C24 110.3(4) C22 C23 C24 111.8(3) C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25B 109.5 C23 C25 H25A 109.5 H25B C25 H25A 109.5 C23 C25 H25C 109.5 H25B C25 H25C 109.5 H25A C25 H25C 109.5 C23 C26 H26C 109.5 C23 C26 H26A 109.5 H26C C26 H26A 109.5 C23 C26 H26B 109.5 H26C C26 H26B 109.5 H26A C26 H26B 109.5 O1 C27 C14 117.0(4) O1 C27 C22 122.2(4) C14 C27 C22 120.8(4) N1 C28 C29 115.7(3) N1 C28 H28A 108.3 C29 C28 H28A 108.3 N1 C28 H28B 108.3 C29 C28 H28B 108.3 H28A C28 H28B 107.4 C34 C29 C30 119.8(4) C34 C29 C28 119.6(4) C30 C29 C28 120.6(4) O2 C30 C29 116.9(4) O2 C30 C31 122.7(4) C29 C30 C31 120.4(4) C32 C31 C30 116.3(4) C32 C31 C39 122.1(4) C30 C31 C39 121.6(4) C33 C32 C31 124.9(4) C33 C32 H32 117.6 C31 C32 H32 117.6 C32 C33 C34 117.3(4) C32 C33 C35 121.3(4) C34 C33 C35 121.4(4) C33 C34 C29 120.9(4) C33 C34 H34 119.5 C29 C34 H34 119.5 C36 C35 C38 112.7(6) C36 C35 C33 113.6(4) C38 C35 C33 109.2(4) C36 C35 C37 104.7(5) C38 C35 C37 107.1(5) C33 C35 C37 109.3(5) C35 C36 H36A 109.5 C35 C36 H36B 109.5 H36A C36 H36B 109.5 C35 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C35 C37 H37A 109.5 C35 C37 H37B 109.5 H37A C37 H37B 109.5 C35 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C35 C38 H38A 109.5 C35 C38 H38B 109.5 H38A C38 H38B 109.5 C35 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C31 C39 C41 108.9(4) C31 C39 C42 110.7(4) C41 C39 C42 110.3(4) C31 C39 C40 112.3(4) C41 C39 C40 107.2(4) C42 C39 C40 107.3(4) C39 C40 H40A 109.5 C39 C40 H40B 109.5 H40A C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C39 C41 H41A 109.5 C39 C41 H41B 109.5 H41A C41 H41B 109.5 C39 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C39 C42 H42A 109.5 C39 C42 H42B 109.5 H42A C42 H42B 109.5 C39 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C48 C43 C44 118.8(4) C48 C43 N5 120.4(4) C44 C43 N5 120.7(4) C45 C44 C43 120.4(4) C45 C44 H44 119.8 C43 C44 H44 119.8 C46 C45 C44 120.5(5) C46 C45 H45 119.7 C44 C45 H45 119.7 C45 C46 C47 119.6(4) C45 C46 H46 120.2 C47 C46 H46 120.2 C48 C47 C46 120.3(4) C48 C47 H47 119.8 C46 C47 H47 119.8 C43 C48 C47 120.3(4) C43 C48 H48 119.9 C47 C48 H48 119.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance U1 O3 1.787(3) U1 N5 1.879(3) U1 O1 2.168(3) U1 O2 2.191(3) U1 N3 2.768(3) U1 N1 2.779(3) O1 C27 1.359(5) O2 C30 1.346(5) N1 C12 1.493(5) N1 C28 1.498(6) N1 C1 1.514(5) N2 C3 1.446(5) N2 C4 1.453(6) N2 C2 1.468(6) N3 C6 1.493(5) N3 C13 1.498(5) N3 C7 1.502(5) N4 C9 1.453(5) N4 C10 1.459(6) N4 C8 1.464(5) N5 C43 1.400(5) C1 C2 1.517(6) C1 H1A 0.9900 C1 H1B 0.9900 C2 H2A 0.9900 C2 H2B 0.9900 C3 H3C 0.9800 C3 H3B 0.9800 C3 H3A 0.9800 C4 C5 1.522(6) C4 H4A 0.9900 C4 H4B 0.9900 C5 C6 1.524(5) C5 H5B 0.9900 C5 H5A 0.9900 C6 H6B 0.9900 C6 H6A 0.9900 C7 C8 1.520(6) C7 H7B 0.9900 C7 H7A 0.9900 C8 H8B 0.9900 C8 H8A 0.9900 C9 H9B 0.9800 C9 H9A 0.9800 C9 H9C 0.9800 C10 C11 1.521(6) C10 H10B 0.9900 C10 H10A 0.9900 C11 C12 1.529(6) C11 H11B 0.9900 C11 H11A 0.9900 C12 H12B 0.9900 C12 H12A 0.9900 C13 C14 1.489(6) C13 H13A 0.9900 C13 H13B 0.9900 C14 C15 1.392(6) C14 C27 1.400(6) C15 C16 1.381(6) C15 H15 0.9500 C16 C21 1.384(6) C16 C17 1.540(6) C17 C20 1.525(6) C17 C18 1.534(6) C17 C19 1.542(6) C18 H18C 0.9800 C18 H18B 0.9800 C18 H18A 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20C 0.9800 C20 H20B 0.9800 C21 C22 1.404(5) C21 H21 0.9500 C22 C27 1.425(6) C22 C23 1.532(6) C23 C26 1.526(6) C23 C25 1.529(6) C23 C24 1.536(6) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25B 0.9800 C25 H25A 0.9800 C25 H25C 0.9800 C26 H26C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C28 C29 1.503(6) C28 H28A 0.9900 C28 H28B 0.9900 C29 C34 1.402(6) C29 C30 1.403(6) C30 C31 1.416(6) C31 C32 1.396(6) C31 C39 1.524(6) C32 C33 1.380(6) C32 H32 0.9500 C33 C34 1.394(6) C33 C35 1.539(6) C34 H34 0.9500 C35 C36 1.469(7) C35 C38 1.479(7) C35 C37 1.577(9) C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C38 H38A 0.9800 C38 H38B 0.9800 C38 H38C 0.9800 C39 C41 1.525(6) C39 C42 1.539(6) C39 C40 1.548(6) C40 H40A 0.9800 C40 H40B 0.9800 C40 H40C 0.9800 C41 H41A 0.9800 C41 H41B 0.9800 C41 H41C 0.9800 C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C43 C48 1.382(6) C43 C44 1.394(6) C44 C45 1.382(6) C44 H44 0.9500 C45 C46 1.366(6) C45 H45 0.9500 C46 C47 1.386(7) C46 H46 0.9500 C47 C48 1.384(6) C47 H47 0.9500 C48 H48 0.9500