#------------------------------------------------------------------------------ #$Date: 2020-01-03 03:49:58 +0200 (Fri, 03 Jan 2020) $ #$Revision: 246444 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/57/7125708.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_7125708 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 'C55 H82 N6 O2 U' _chemical_formula_sum 'C55 H82 N6 O2 U' _chemical_formula_weight 1097.29 _chemical_properties_physical Air-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -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 103.238(3) _cell_angle_beta 108.535(2) _cell_angle_gamma 108.528(3) _cell_formula_units_Z 2 _cell_length_a 13.3531(7) _cell_length_b 13.9911(6) _cell_length_c 16.8717(9) _cell_measurement_reflns_used 3581 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 24.01 _cell_measurement_theta_min 2.74 _cell_volume 2635.8(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 0.871 _diffrn_measured_fraction_theta_max 0.871 _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 0.0436 _diffrn_reflns_av_unetI/netI 0.0890 _diffrn_reflns_Laue_measured_fraction_full 0.871 _diffrn_reflns_Laue_measured_fraction_max 0.871 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 12820 _diffrn_reflns_point_group_measured_fraction_full 0.871 _diffrn_reflns_point_group_measured_fraction_max 0.871 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 3.178 _exptl_absorpt_coefficient_mu 3.124 _exptl_absorpt_correction_T_max 0.8852 _exptl_absorpt_correction_T_min 0.6033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.383 _exptl_crystal_description prism _exptl_crystal_F_000 1124 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _refine_diff_density_max 3.146 _refine_diff_density_min -1.971 _refine_diff_density_rms 0.167 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 580 _refine_ls_number_reflns 8104 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0577 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0946P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1396 _refine_ls_wR_factor_ref 0.1496 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6370 _reflns_number_total 8104 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc07411b2.cif _cod_data_source_block comp_3 _cod_original_cell_volume 2635.8(2) _cod_database_code 7125708 _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 0.603 _shelx_estimated_absorpt_t_max 0.885 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL LM212N_a.res in P-1 CELL 0.71073 13.3531 13.9911 16.8717 103.238 108.535 108.528 ZERR 2.00 0.0007 0.0006 0.0009 0.003 0.002 0.003 LATT 1 SFAC C H N O U UNIT 110 164 12 4 2 MERG 2 OMIT 0.00 180.00 OMIT 4 -8 2 OMIT 1 6 4 OMIT -2 0 1 OMIT -2 1 2 OMIT -4 2 4 OMIT -4 2 3 OMIT -5 3 5 OMIT -5 1 5 OMIT -3 1 3 OMIT -3 2 3 OMIT 0 -5 8 OMIT 2 -7 3 OMIT -2 -5 4 OMIT -1 6 10 shel 6.5 0.84 ISOR 0.001 C21 C22 C23 FMAP 2 PLAN 5 SIZE 0.040 0.080 0.180 ACTA BOND $H L.S. 5 TEMP -123.00 WGHT 0.094600 FVAR 0.36558 U1 5 0.422788 0.481599 0.726512 11.00000 0.02329 0.02693 = 0.02492 0.00288 0.01440 0.01311 O1 4 0.303320 0.379420 0.587821 11.00000 0.02262 0.02820 = 0.02396 -0.00338 0.00901 0.00839 O2 4 0.314503 0.518044 0.789508 11.00000 0.02618 0.02695 = 0.02298 -0.00150 0.01419 0.01601 N1 3 0.567917 0.422982 0.663121 11.00000 0.03002 0.02397 = 0.02291 0.00716 0.01729 0.01332 N2 3 0.774412 0.739258 0.824708 11.00000 0.01323 0.02454 = 0.02823 -0.00087 0.00601 0.00104 N3 3 0.583469 0.634195 0.889292 11.00000 0.01929 0.03219 = 0.02264 0.00706 0.01101 0.01395 N4 3 0.739796 0.433881 0.847497 11.00000 0.02380 0.03629 = 0.02782 0.00806 0.01843 0.01675 N5 3 0.430160 0.600658 0.687885 11.00000 0.01551 0.01749 = 0.03017 0.00865 0.00845 0.00712 N6 3 0.397933 0.358972 0.762162 11.00000 0.03302 0.02511 = 0.03287 0.01222 0.02152 0.01891 C1 1 0.681835 0.516300 0.690559 11.00000 0.02043 0.02004 = 0.02222 -0.00186 0.00792 0.00908 AFIX 23 H1A 2 0.727722 0.488687 0.663529 11.00000 -1.20000 H1B 2 0.725118 0.542107 0.756618 11.00000 -1.20000 AFIX 0 C2 1 0.677637 0.614017 0.665830 11.00000 0.03509 0.04986 = 0.02812 0.01921 0.02301 0.02330 AFIX 23 H2A 2 0.681260 0.604788 0.606997 11.00000 -1.20000 H2B 2 0.602698 0.617289 0.659771 11.00000 -1.20000 AFIX 0 C3 1 0.777649 0.719855 0.736051 11.00000 0.03392 0.03698 = 0.04691 0.02215 0.02982 0.02292 AFIX 23 H3A 2 0.852651 0.717506 0.740994 11.00000 -1.20000 H3B 2 0.772917 0.780559 0.716688 11.00000 -1.20000 AFIX 0 C4 1 0.680483 0.772031 0.828194 11.00000 0.02105 0.01919 = 0.02847 0.00099 0.01186 0.00819 AFIX 23 H4A 2 0.614923 0.735424 0.767599 11.00000 -1.20000 H4B 2 0.709988 0.850937 0.841145 11.00000 -1.20000 AFIX 0 C5 1 0.632797 0.749415 0.894662 11.00000 0.02432 0.02490 = 0.02548 0.00320 0.00915 0.00913 AFIX 23 H5A 2 0.570763 0.775270 0.888253 11.00000 -1.20000 H5B 2 0.696000 0.793817 0.955707 11.00000 -1.20000 AFIX 0 C6 1 0.683770 0.608930 0.930995 11.00000 0.01303 0.03019 = 0.02758 0.00049 0.01018 0.00674 AFIX 23 H6A 2 0.737617 0.668228 0.989804 11.00000 -1.20000 H6B 2 0.726318 0.609347 0.892455 11.00000 -1.20000 AFIX 0 C7 1 0.655371 0.503131 0.945822 11.00000 0.02747 0.04535 = 0.02365 0.01066 0.01766 0.01976 AFIX 23 H7A 2 0.576375 0.450058 0.900276 11.00000 -1.20000 H7B 2 0.655285 0.514471 1.005909 11.00000 -1.20000 AFIX 0 C8 1 0.743878 0.457551 0.939308 11.00000 0.02693 0.04303 = 0.03335 0.01949 0.02258 0.02059 AFIX 23 H8A 2 0.823198 0.510783 0.984156 11.00000 -1.20000 H8B 2 0.725785 0.390311 0.952588 11.00000 -1.20000 AFIX 0 C9 1 0.635556 0.341563 0.781543 11.00000 0.02890 0.03328 = 0.03309 0.01181 0.02294 0.01995 AFIX 23 H9A 2 0.571891 0.339601 0.800114 11.00000 -1.20000 H9B 2 0.647640 0.275778 0.783637 11.00000 -1.20000 AFIX 0 C10 1 0.592842 0.333421 0.682811 11.00000 0.03555 0.02583 = 0.03527 0.00989 0.02631 0.01941 AFIX 23 H10A 2 0.652516 0.326777 0.661835 11.00000 -1.20000 H10B 2 0.520969 0.265446 0.646515 11.00000 -1.20000 AFIX 0 C11 1 0.886494 0.817726 0.897073 11.00000 0.03158 0.05054 = 0.04608 0.00561 0.02018 0.01540 AFIX 33 H11A 2 0.880924 0.828451 0.954725 11.00000 -1.50000 H11B 2 0.945902 0.790774 0.897288 11.00000 -1.50000 H11C 2 0.908167 0.886817 0.887960 11.00000 -1.50000 AFIX 0 C12 1 0.843960 0.424271 0.846518 11.00000 0.02215 0.03862 = 0.03907 0.00858 0.01935 0.01564 AFIX 33 H12A 2 0.912724 0.488892 0.892470 11.00000 -1.50000 H12B 2 0.846413 0.359885 0.859162 11.00000 -1.50000 H12C 2 0.843429 0.417514 0.787258 11.00000 -1.50000 AFIX 0 C13 1 0.501550 0.384664 0.563323 11.00000 0.04008 0.03118 = 0.02114 0.00705 0.02164 0.01161 AFIX 23 H13A 2 0.483527 0.443716 0.548970 11.00000 -1.20000 H13B 2 0.553225 0.372240 0.535109 11.00000 -1.20000 AFIX 0 C14 1 0.390580 0.284295 0.520809 11.00000 0.03305 0.02980 = 0.02786 0.01501 0.01832 0.01673 C15 1 0.381130 0.188745 0.464489 11.00000 0.03275 0.04246 = 0.02743 0.00437 0.01785 0.01873 AFIX 43 H15 2 0.448186 0.187865 0.456540 11.00000 -1.20000 AFIX 0 C16 1 0.279562 0.096090 0.420102 11.00000 0.03282 0.03054 = 0.03175 0.00639 0.01616 0.01512 C17 1 0.180209 0.101850 0.430850 11.00000 0.02576 0.01441 = 0.02898 -0.00059 0.01370 -0.00037 AFIX 43 H17 2 0.108137 0.039143 0.400271 11.00000 -1.20000 AFIX 0 C18 1 0.184811 0.197186 0.485203 11.00000 0.03153 0.03322 = 0.02603 0.00870 0.01571 0.01614 C19 1 0.291096 0.286621 0.531924 11.00000 0.02114 0.02326 = 0.01917 -0.00063 0.00873 0.00383 C20 1 0.269464 -0.010256 0.362878 11.00000 0.04298 0.02543 = 0.05058 0.00424 0.03153 0.01230 C21 1 0.369784 0.006563 0.334646 11.00000 0.08471 0.08485 = 0.08541 0.02763 0.04000 0.03509 AFIX 33 H21A 2 0.374212 0.059557 0.305164 11.00000 -1.50000 H21B 2 0.443189 0.033388 0.387879 11.00000 -1.50000 H21C 2 0.356311 -0.062468 0.292782 11.00000 -1.50000 AFIX 0 C22 1 0.163843 -0.060041 0.273474 11.00000 0.09427 0.09534 = 0.09613 0.03123 0.04054 0.04289 AFIX 33 H22A 2 0.169791 -0.009374 0.241748 11.00000 -1.50000 H22B 2 0.160286 -0.127640 0.237106 11.00000 -1.50000 H22C 2 0.093075 -0.075339 0.283690 11.00000 -1.50000 AFIX 0 C23 1 0.256954 -0.087146 0.406814 11.00000 0.10003 0.09929 = 0.09913 0.03586 0.04421 0.04143 AFIX 33 H23A 2 0.324234 -0.057195 0.465116 11.00000 -1.50000 H23B 2 0.185443 -0.102194 0.415939 11.00000 -1.50000 H23C 2 0.252654 -0.154495 0.369355 11.00000 -1.50000 AFIX 0 C24 1 0.071560 0.201524 0.488330 11.00000 0.02162 0.02179 = 0.02803 -0.00513 0.01018 0.00273 C25 1 -0.036542 0.095776 0.427287 11.00000 0.02810 0.04791 = 0.04216 -0.00183 0.01713 0.01627 AFIX 33 H25A 2 -0.027848 0.036691 0.446418 11.00000 -1.50000 H25B 2 -0.105563 0.103161 0.431187 11.00000 -1.50000 H25C 2 -0.045574 0.079627 0.365090 11.00000 -1.50000 AFIX 0 C26 1 0.051745 0.288929 0.454671 11.00000 0.02693 0.04092 = 0.04773 0.01418 0.01271 0.01289 AFIX 33 H26A 2 0.119211 0.358739 0.491964 11.00000 -1.50000 H26B 2 0.041627 0.270398 0.392138 11.00000 -1.50000 H26C 2 -0.018361 0.293932 0.458235 11.00000 -1.50000 AFIX 0 C27 1 0.080635 0.224709 0.584527 11.00000 0.03062 0.03641 = 0.03956 0.00619 0.02397 0.01588 AFIX 33 H27A 2 0.093360 0.167577 0.604864 11.00000 -1.50000 H27B 2 0.146130 0.294881 0.624628 11.00000 -1.50000 H27C 2 0.008200 0.226450 0.585419 11.00000 -1.50000 AFIX 0 C28 1 0.518497 0.631744 0.948159 11.00000 0.03604 0.03677 = 0.02551 0.01282 0.02034 0.02789 AFIX 23 H28A 2 0.486094 0.556849 0.946783 11.00000 -1.20000 H28B 2 0.575626 0.678688 1.010744 11.00000 -1.20000 AFIX 0 C29 1 0.420423 0.666801 0.924822 11.00000 0.02871 0.03686 = 0.02958 0.01830 0.02163 0.01898 C30 1 0.427830 0.757008 0.987785 11.00000 0.02708 0.02271 = 0.01982 0.00103 0.01355 0.00971 AFIX 43 H30 2 0.497151 0.798316 1.041720 11.00000 -1.20000 AFIX 0 C31 1 0.335875 0.787063 0.972812 11.00000 0.03523 0.02520 = 0.02242 0.00546 0.02011 0.01518 C32 1 0.236591 0.724003 0.893441 11.00000 0.02613 0.02566 = 0.02980 0.00934 0.01783 0.01416 AFIX 43 H32 2 0.173893 0.744908 0.882137 11.00000 -1.20000 AFIX 0 C33 1 0.221737 0.630487 0.827818 11.00000 0.02404 0.01867 = 0.02490 0.00753 0.01374 0.00932 C34 1 0.318736 0.605620 0.846747 11.00000 0.02903 0.02894 = 0.02825 0.01084 0.02241 0.01331 C35 1 0.338812 0.883867 1.040298 11.00000 0.03439 0.01902 = 0.03335 0.00150 0.01747 0.00937 C36 1 0.446316 0.935864 1.128234 11.00000 0.06141 0.04920 = 0.03708 0.00015 0.02221 0.03428 AFIX 33 H36A 2 0.450305 0.882010 1.155957 11.00000 -1.50000 H36B 2 0.515827 0.963350 1.117172 11.00000 -1.50000 H36C 2 0.442605 0.995986 1.168658 11.00000 -1.50000 AFIX 0 C37 1 0.334648 0.968748 0.998789 11.00000 0.09704 0.04921 = 0.05185 0.01554 0.03906 0.04651 AFIX 33 H37A 2 0.265237 0.936234 0.941549 11.00000 -1.50000 H37B 2 0.331398 1.028736 1.039747 11.00000 -1.50000 H37C 2 0.404620 0.996100 0.988261 11.00000 -1.50000 AFIX 0 C38 1 0.233074 0.846823 1.061131 11.00000 0.06076 0.06411 = 0.05941 0.01230 0.04294 0.03976 AFIX 33 H38A 2 0.161746 0.812629 1.005108 11.00000 -1.50000 H38B 2 0.236889 0.794475 1.090591 11.00000 -1.50000 H38C 2 0.232550 0.909528 1.101099 11.00000 -1.50000 AFIX 0 C39 1 0.104700 0.559652 0.746240 11.00000 0.02218 0.04465 = 0.02748 0.00886 0.01527 0.02131 C40 1 0.013977 0.606767 0.743502 11.00000 0.02597 0.05139 = 0.03414 0.01568 0.01740 0.02348 AFIX 137 H40A 2 -0.057434 0.562023 0.688127 11.00000 -1.50000 H40B 2 0.045710 0.681034 0.745068 11.00000 -1.50000 H40C 2 -0.003854 0.607111 0.795576 11.00000 -1.50000 AFIX 0 C41 1 0.057083 0.446786 0.749702 11.00000 0.02439 0.03805 = 0.04824 0.01186 0.01984 0.01709 AFIX 137 H41A 2 0.112337 0.414769 0.748585 11.00000 -1.50000 H41B 2 -0.017928 0.400932 0.697651 11.00000 -1.50000 H41C 2 0.046263 0.452179 0.805093 11.00000 -1.50000 AFIX 0 C42 1 0.118132 0.551478 0.657866 11.00000 0.02695 0.05188 = 0.03225 0.00927 0.01626 0.01882 AFIX 137 H42A 2 0.180209 0.528270 0.658380 11.00000 -1.50000 H42B 2 0.138121 0.622457 0.652014 11.00000 -1.50000 H42C 2 0.044609 0.498507 0.606987 11.00000 -1.50000 AFIX 0 C43 1 0.380116 0.657536 0.644418 11.00000 0.01771 0.03370 = 0.02694 0.00987 0.01447 0.00966 C44 1 0.399023 0.762228 0.692263 11.00000 0.02966 0.03139 = 0.04664 0.00934 0.00887 0.01229 AFIX 43 H44 2 0.449406 0.796012 0.754598 11.00000 -1.20000 AFIX 0 C45 1 0.344664 0.816538 0.649128 11.00000 0.03922 0.03706 = 0.07927 0.02123 0.02238 0.02015 AFIX 43 H45 2 0.356373 0.887192 0.681758 11.00000 -1.20000 AFIX 0 C46 1 0.272851 0.767369 0.557877 11.00000 0.03710 0.07662 = 0.06520 0.05047 0.02807 0.03522 AFIX 43 H46 2 0.236628 0.805179 0.527696 11.00000 -1.20000 AFIX 0 C47 1 0.253873 0.665377 0.511238 11.00000 0.04236 0.07622 = 0.03814 0.03091 0.02602 0.03341 AFIX 43 H47 2 0.202713 0.632319 0.449058 11.00000 -1.20000 AFIX 0 C48 1 0.307354 0.608454 0.552203 11.00000 0.04046 0.05553 = 0.04198 0.02431 0.03163 0.02971 AFIX 43 H48 2 0.294967 0.537950 0.518586 11.00000 -1.20000 AFIX 0 C50 1 0.250410 0.286078 0.814003 11.00000 0.02664 0.03665 = 0.02588 0.00848 0.01402 0.01205 AFIX 43 H50 2 0.244561 0.353243 0.828504 11.00000 -1.20000 AFIX 0 C49 1 0.328802 0.273757 0.777846 11.00000 0.01947 0.04498 = 0.02256 0.01344 0.01181 0.01495 C51 1 0.182225 0.201313 0.828439 11.00000 0.03492 0.06091 = 0.02630 0.01175 0.01594 0.01397 AFIX 43 H51 2 0.128393 0.210918 0.851556 11.00000 -1.20000 AFIX 0 C52 1 0.188662 0.102362 0.810696 11.00000 0.03140 0.03739 = 0.02966 0.01077 0.00312 -0.00459 C53 1 0.269289 0.093129 0.778196 11.00000 0.04055 0.02699 = 0.05135 0.01484 0.00872 0.00462 AFIX 43 H53 2 0.279358 0.027855 0.768670 11.00000 -1.20000 AFIX 0 C54 1 0.336305 0.175198 0.758833 11.00000 0.02388 0.03214 = 0.04138 0.01083 0.01268 0.00795 AFIX 43 H54 2 0.386950 0.163811 0.732723 11.00000 -1.20000 AFIX 0 C55 1 0.111858 0.009674 0.826284 11.00000 0.06202 0.07127 = 0.06837 0.04107 0.01796 -0.00045 AFIX 33 H55A 2 0.129417 -0.052952 0.809811 11.00000 -1.50000 H55B 2 0.126537 0.031844 0.889857 11.00000 -1.50000 H55C 2 0.029829 -0.009960 0.789289 11.00000 -1.50000 AFIX 0 HKLF 4 REM LM212N_a.res in P-1 REM R1 = 0.0577 for 6370 Fo > 4sig(Fo) and 0.0826 for all 8104 data REM 580 parameters refined using 18 restraints END WGHT 0.0934 0.0000 REM Highest difference peak 3.146, deepest hole -1.971, 1-sigma level 0.167 Q1 1 0.3552 0.3893 0.6968 11.00000 0.05 3.15 Q2 1 0.4777 0.5658 0.7545 11.00000 0.05 3.05 Q3 1 0.7354 0.5559 0.8263 11.00000 0.05 2.53 Q4 1 0.4250 0.5363 0.6950 11.00000 0.05 2.17 Q5 1 0.4081 0.4196 0.7435 11.00000 0.05 2.06 ; _shelx_res_checksum 7400 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.42279(3) 0.48160(3) 0.72651(2) 0.02448(13) Uani 1 1 d . . O1 O 0.3033(5) 0.3794(5) 0.5878(4) 0.0284(14) Uani 1 1 d . . O2 O 0.3145(5) 0.5180(5) 0.7895(4) 0.0251(14) Uani 1 1 d . . N1 N 0.5679(6) 0.4230(6) 0.6631(4) 0.0237(16) Uani 1 1 d . . N2 N 0.7744(6) 0.7393(6) 0.8247(5) 0.0268(17) Uani 1 1 d . . N3 N 0.5835(6) 0.6342(6) 0.8893(4) 0.0238(16) Uani 1 1 d . . N4 N 0.7398(6) 0.4339(6) 0.8475(5) 0.0268(18) Uani 1 1 d . . N5 N 0.4302(6) 0.6007(6) 0.6879(5) 0.0214(15) Uani 1 1 d . . N6 N 0.3979(6) 0.3590(6) 0.7622(5) 0.0261(17) Uani 1 1 d . . C1 C 0.6818(7) 0.5163(7) 0.6906(5) 0.0230(19) Uani 1 1 d . . H1A H 0.7277 0.4887 0.6635 0.028 Uiso 1 1 calc R U H1B H 0.7251 0.5421 0.7566 0.028 Uiso 1 1 calc R U C2 C 0.6776(8) 0.6140(8) 0.6658(6) 0.033(2) Uani 1 1 d . . H2A H 0.6813 0.6048 0.6070 0.039 Uiso 1 1 calc R U H2B H 0.6027 0.6173 0.6598 0.039 Uiso 1 1 calc R U C3 C 0.7776(8) 0.7199(8) 0.7361(6) 0.032(2) Uani 1 1 d . . H3A H 0.8527 0.7175 0.7410 0.039 Uiso 1 1 calc R U H3B H 0.7729 0.7806 0.7167 0.039 Uiso 1 1 calc R U C4 C 0.6805(7) 0.7720(7) 0.8282(6) 0.0241(19) Uani 1 1 d . . H4A H 0.6149 0.7354 0.7676 0.029 Uiso 1 1 calc R U H4B H 0.7100 0.8509 0.8411 0.029 Uiso 1 1 calc R U C5 C 0.6328(8) 0.7494(8) 0.8947(6) 0.027(2) Uani 1 1 d . . H5A H 0.5708 0.7753 0.8883 0.032 Uiso 1 1 calc R U H5B H 0.6960 0.7938 0.9557 0.032 Uiso 1 1 calc R U C6 C 0.6838(7) 0.6089(8) 0.9310(6) 0.026(2) Uani 1 1 d . . H6A H 0.7376 0.6682 0.9898 0.031 Uiso 1 1 calc R U H6B H 0.7263 0.6093 0.8925 0.031 Uiso 1 1 calc R U C7 C 0.6554(8) 0.5031(8) 0.9458(6) 0.029(2) Uani 1 1 d . . H7A H 0.5764 0.4501 0.9003 0.035 Uiso 1 1 calc R U H7B H 0.6553 0.5145 1.0059 0.035 Uiso 1 1 calc R U C8 C 0.7439(8) 0.4576(8) 0.9393(6) 0.029(2) Uani 1 1 d . . H8A H 0.8232 0.5108 0.9842 0.035 Uiso 1 1 calc R U H8B H 0.7258 0.3903 0.9526 0.035 Uiso 1 1 calc R U C9 C 0.6356(8) 0.3416(8) 0.7815(6) 0.027(2) Uani 1 1 d . . H9A H 0.5719 0.3396 0.8001 0.033 Uiso 1 1 calc R U H9B H 0.6476 0.2758 0.7836 0.033 Uiso 1 1 calc R U C10 C 0.5928(8) 0.3334(8) 0.6828(6) 0.028(2) Uani 1 1 d . . H10A H 0.6525 0.3268 0.6618 0.033 Uiso 1 1 calc R U H10B H 0.5210 0.2654 0.6465 0.033 Uiso 1 1 calc R U C11 C 0.8865(9) 0.8177(10) 0.8971(7) 0.045(3) Uani 1 1 d . . H11A H 0.8809 0.8285 0.9547 0.067 Uiso 1 1 calc R U H11B H 0.9459 0.7908 0.8973 0.067 Uiso 1 1 calc R U H11C H 0.9082 0.8868 0.8880 0.067 Uiso 1 1 calc R U C12 C 0.8440(8) 0.4243(8) 0.8465(6) 0.032(2) Uani 1 1 d . . H12A H 0.9127 0.4889 0.8925 0.048 Uiso 1 1 calc R U H12B H 0.8464 0.3599 0.8592 0.048 Uiso 1 1 calc R U H12C H 0.8434 0.4175 0.7873 0.048 Uiso 1 1 calc R U C13 C 0.5015(8) 0.3847(8) 0.5633(5) 0.030(2) Uani 1 1 d . . H13A H 0.4835 0.4437 0.5490 0.036 Uiso 1 1 calc R U H13B H 0.5532 0.3722 0.5351 0.036 Uiso 1 1 calc R U C14 C 0.3906(8) 0.2843(8) 0.5208(6) 0.027(2) Uani 1 1 d . . C15 C 0.3811(9) 0.1887(9) 0.4645(6) 0.034(2) Uani 1 1 d . . H15 H 0.4482 0.1879 0.4565 0.040 Uiso 1 1 calc R U C16 C 0.2796(9) 0.0961(8) 0.4201(6) 0.032(2) Uani 1 1 d . . C17 C 0.1802(8) 0.1018(8) 0.4308(6) 0.027(2) Uani 1 1 d . . H17 H 0.1081 0.0391 0.4003 0.032 Uiso 1 1 calc R U C18 C 0.1848(8) 0.1972(8) 0.4852(6) 0.029(2) Uani 1 1 d . . C19 C 0.2911(8) 0.2866(8) 0.5319(5) 0.024(2) Uani 1 1 d . . C20 C 0.2695(9) -0.0103(8) 0.3629(7) 0.039(2) Uani 1 1 d . . C21 C 0.3698(14) 0.0066(14) 0.3346(10) 0.085(4) Uani 1 1 d . U H21A H 0.3742 0.0596 0.3052 0.127 Uiso 1 1 calc R U H21B H 0.4432 0.0334 0.3879 0.127 Uiso 1 1 calc R U H21C H 0.3563 -0.0625 0.2928 0.127 Uiso 1 1 calc R U C22 C 0.1638(15) -0.0600(15) 0.2735(11) 0.095(5) Uani 1 1 d . U H22A H 0.1698 -0.0094 0.2417 0.143 Uiso 1 1 calc R U H22B H 0.1603 -0.1276 0.2371 0.143 Uiso 1 1 calc R U H22C H 0.0931 -0.0753 0.2837 0.143 Uiso 1 1 calc R U C23 C 0.2570(15) -0.0871(15) 0.4068(11) 0.099(5) Uani 1 1 d . U H23A H 0.3242 -0.0572 0.4651 0.149 Uiso 1 1 calc R U H23B H 0.1854 -0.1022 0.4159 0.149 Uiso 1 1 calc R U H23C H 0.2527 -0.1545 0.3694 0.149 Uiso 1 1 calc R U C24 C 0.0716(8) 0.2015(8) 0.4883(6) 0.029(2) Uani 1 1 d . . C25 C -0.0365(8) 0.0958(9) 0.4273(7) 0.042(3) Uani 1 1 d . . H25A H -0.0278 0.0367 0.4464 0.063 Uiso 1 1 calc R U H25B H -0.1056 0.1032 0.4312 0.063 Uiso 1 1 calc R U H25C H -0.0456 0.0796 0.3651 0.063 Uiso 1 1 calc R U C26 C 0.0517(9) 0.2889(9) 0.4547(7) 0.040(2) Uani 1 1 d . . H26A H 0.1192 0.3587 0.4920 0.060 Uiso 1 1 calc R U H26B H 0.0416 0.2704 0.3921 0.060 Uiso 1 1 calc R U H26C H -0.0184 0.2939 0.4582 0.060 Uiso 1 1 calc R U C27 C 0.0806(8) 0.2247(9) 0.5845(6) 0.034(2) Uani 1 1 d . . H27A H 0.0934 0.1676 0.6049 0.051 Uiso 1 1 calc R U H27B H 0.1461 0.2949 0.6246 0.051 Uiso 1 1 calc R U H27C H 0.0082 0.2265 0.5854 0.051 Uiso 1 1 calc R U C28 C 0.5185(8) 0.6317(8) 0.9482(5) 0.027(2) Uani 1 1 d . . H28A H 0.4861 0.5568 0.9468 0.032 Uiso 1 1 calc R U H28B H 0.5756 0.6787 1.0107 0.032 Uiso 1 1 calc R U C29 C 0.4204(8) 0.6668(8) 0.9248(6) 0.026(2) Uani 1 1 d . . C30 C 0.4278(8) 0.7570(7) 0.9878(5) 0.0238(19) Uani 1 1 d . . H30 H 0.4972 0.7983 1.0417 0.029 Uiso 1 1 calc R U C31 C 0.3359(8) 0.7871(8) 0.9728(5) 0.025(2) Uani 1 1 d . . C32 C 0.2366(8) 0.7240(7) 0.8934(6) 0.025(2) Uani 1 1 d . . H32 H 0.1739 0.7449 0.8821 0.030 Uiso 1 1 calc R U C33 C 0.2217(8) 0.6305(7) 0.8278(5) 0.0216(18) Uani 1 1 d . . C34 C 0.3187(8) 0.6056(8) 0.8467(6) 0.026(2) Uani 1 1 d . . C35 C 0.3388(8) 0.8839(8) 1.0403(6) 0.030(2) Uani 1 1 d . . C36 C 0.4463(10) 0.9359(10) 1.1282(6) 0.049(3) Uani 1 1 d . . H36A H 0.4503 0.8820 1.1560 0.073 Uiso 1 1 calc R U H36B H 0.5158 0.9633 1.1172 0.073 Uiso 1 1 calc R U H36C H 0.4426 0.9960 1.1687 0.073 Uiso 1 1 calc R U C37 C 0.3346(12) 0.9687(10) 0.9988(7) 0.060(4) Uani 1 1 d . . H37A H 0.2652 0.9362 0.9415 0.090 Uiso 1 1 calc R U H37B H 0.3314 1.0287 1.0397 0.090 Uiso 1 1 calc R U H37C H 0.4046 0.9961 0.9883 0.090 Uiso 1 1 calc R U C38 C 0.2331(10) 0.8468(10) 1.0611(8) 0.055(3) Uani 1 1 d . . H38A H 0.1617 0.8126 1.0051 0.082 Uiso 1 1 calc R U H38B H 0.2369 0.7945 1.0906 0.082 Uiso 1 1 calc R U H38C H 0.2326 0.9095 1.1011 0.082 Uiso 1 1 calc R U C39 C 0.1047(8) 0.5597(8) 0.7462(6) 0.029(2) Uani 1 1 d . . C40 C 0.0140(8) 0.6068(9) 0.7435(6) 0.034(2) Uani 1 1 d . . H40A H -0.0574 0.5620 0.6881 0.051 Uiso 1 1 calc R U H40B H 0.0457 0.6810 0.7451 0.051 Uiso 1 1 calc R U H40C H -0.0039 0.6071 0.7956 0.051 Uiso 1 1 calc R U C41 C 0.0571(8) 0.4468(8) 0.7497(7) 0.035(2) Uani 1 1 d . . H41A H 0.1123 0.4148 0.7486 0.053 Uiso 1 1 calc R U H41B H -0.0179 0.4009 0.6977 0.053 Uiso 1 1 calc R U H41C H 0.0463 0.4522 0.8051 0.053 Uiso 1 1 calc R U C42 C 0.1181(8) 0.5515(9) 0.6579(6) 0.037(2) Uani 1 1 d . . H42A H 0.1802 0.5283 0.6584 0.055 Uiso 1 1 calc R U H42B H 0.1381 0.6225 0.6520 0.055 Uiso 1 1 calc R U H42C H 0.0446 0.4985 0.6070 0.055 Uiso 1 1 calc R U C43 C 0.3801(7) 0.6575(8) 0.6444(6) 0.025(2) Uani 1 1 d . . C44 C 0.3990(9) 0.7622(9) 0.6923(7) 0.039(2) Uani 1 1 d . . H44 H 0.4494 0.7960 0.7546 0.047 Uiso 1 1 calc R U C45 C 0.3447(10) 0.8165(10) 0.6491(8) 0.052(3) Uani 1 1 d . . H45 H 0.3564 0.8872 0.6818 0.062 Uiso 1 1 calc R U C46 C 0.2729(9) 0.7674(11) 0.5579(8) 0.050(3) Uani 1 1 d . . H46 H 0.2366 0.8052 0.5277 0.060 Uiso 1 1 calc R U C47 C 0.2539(9) 0.6654(11) 0.5112(7) 0.045(3) Uani 1 1 d . . H47 H 0.2027 0.6323 0.4491 0.055 Uiso 1 1 calc R U C48 C 0.3074(8) 0.6085(9) 0.5522(6) 0.038(3) Uani 1 1 d . . H48 H 0.2950 0.5380 0.5186 0.046 Uiso 1 1 calc R U C50 C 0.2504(8) 0.2861(8) 0.8140(6) 0.030(2) Uani 1 1 d . . H50 H 0.2446 0.3532 0.8285 0.036 Uiso 1 1 calc R U C49 C 0.3288(7) 0.2738(8) 0.7778(6) 0.028(2) Uani 1 1 d . . C51 C 0.1822(9) 0.2013(10) 0.8284(6) 0.042(3) Uani 1 1 d . . H51 H 0.1284 0.2109 0.8516 0.051 Uiso 1 1 calc R U C52 C 0.1887(9) 0.1024(9) 0.8107(6) 0.041(3) Uani 1 1 d . . C53 C 0.2693(9) 0.0931(9) 0.7782(7) 0.045(3) Uani 1 1 d . . H53 H 0.2794 0.0279 0.7687 0.054 Uiso 1 1 calc R U C54 C 0.3363(8) 0.1752(8) 0.7588(6) 0.034(2) Uani 1 1 d . . H54 H 0.3869 0.1638 0.7327 0.041 Uiso 1 1 calc R U C55 C 0.1119(12) 0.0097(12) 0.8263(9) 0.075(4) Uani 1 1 d . . H55A H 0.1294 -0.0530 0.8098 0.112 Uiso 1 1 calc R U H55B H 0.1265 0.0318 0.8899 0.112 Uiso 1 1 calc R U H55C H 0.0298 -0.0100 0.7893 0.112 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 0.0233(2) 0.0269(2) 0.02492(19) 0.00288(15) 0.01440(15) 0.01311(17) O1 0.023(3) 0.028(4) 0.024(3) -0.003(3) 0.009(3) 0.008(3) O2 0.026(3) 0.027(4) 0.023(3) -0.001(3) 0.014(3) 0.016(3) N1 0.030(4) 0.024(5) 0.023(4) 0.007(3) 0.017(3) 0.013(4) N2 0.013(4) 0.025(5) 0.028(4) -0.001(4) 0.006(3) 0.001(4) N3 0.019(4) 0.032(5) 0.023(4) 0.007(4) 0.011(3) 0.014(4) N4 0.024(4) 0.036(5) 0.028(4) 0.008(4) 0.018(4) 0.017(4) N5 0.016(4) 0.017(4) 0.030(4) 0.009(3) 0.008(3) 0.007(4) N6 0.033(5) 0.025(5) 0.033(4) 0.012(4) 0.022(4) 0.019(4) C1 0.020(5) 0.020(5) 0.022(4) -0.002(4) 0.008(4) 0.009(5) C2 0.035(6) 0.050(7) 0.028(5) 0.019(5) 0.023(5) 0.023(6) C3 0.034(6) 0.037(7) 0.047(6) 0.022(5) 0.030(5) 0.023(6) C4 0.021(5) 0.019(5) 0.028(4) 0.001(4) 0.012(4) 0.008(5) C5 0.024(5) 0.025(6) 0.025(4) 0.003(4) 0.009(4) 0.009(5) C6 0.013(4) 0.030(6) 0.028(4) 0.000(4) 0.010(4) 0.007(5) C7 0.027(5) 0.045(7) 0.024(4) 0.011(5) 0.018(4) 0.020(5) C8 0.027(5) 0.043(7) 0.033(5) 0.019(5) 0.023(4) 0.021(5) C9 0.029(5) 0.033(6) 0.033(5) 0.012(5) 0.023(4) 0.020(5) C10 0.036(6) 0.026(6) 0.035(5) 0.010(4) 0.026(5) 0.019(5) C11 0.032(6) 0.051(8) 0.046(6) 0.006(6) 0.020(5) 0.015(6) C12 0.022(5) 0.039(7) 0.039(5) 0.009(5) 0.019(4) 0.016(5) C13 0.040(6) 0.031(6) 0.021(4) 0.007(4) 0.022(4) 0.012(5) C14 0.033(6) 0.030(6) 0.028(5) 0.015(4) 0.018(4) 0.017(5) C15 0.033(6) 0.042(7) 0.027(5) 0.004(5) 0.018(5) 0.019(6) C16 0.033(6) 0.031(7) 0.032(5) 0.006(5) 0.016(5) 0.015(6) C17 0.026(5) 0.014(5) 0.029(5) -0.001(4) 0.014(4) 0.000(5) C18 0.032(6) 0.033(6) 0.026(5) 0.009(5) 0.016(4) 0.016(6) C19 0.021(5) 0.023(6) 0.019(4) -0.001(4) 0.009(4) 0.004(5) C20 0.043(6) 0.025(6) 0.051(6) 0.004(5) 0.032(5) 0.012(6) C21 0.085(5) 0.085(5) 0.085(5) 0.028(2) 0.040(3) 0.035(3) C22 0.094(5) 0.095(5) 0.096(5) 0.031(3) 0.041(3) 0.043(3) C23 0.100(6) 0.099(6) 0.099(6) 0.036(3) 0.044(3) 0.041(3) C24 0.022(5) 0.022(6) 0.028(5) -0.005(4) 0.010(4) 0.003(5) C25 0.028(6) 0.048(8) 0.042(6) -0.002(5) 0.017(5) 0.016(6) C26 0.027(6) 0.041(7) 0.048(6) 0.014(6) 0.013(5) 0.013(6) C27 0.031(5) 0.036(6) 0.040(5) 0.006(5) 0.024(5) 0.016(5) C28 0.036(5) 0.037(6) 0.026(4) 0.013(4) 0.020(4) 0.028(5) C29 0.029(5) 0.037(6) 0.030(5) 0.018(5) 0.022(4) 0.019(5) C30 0.027(5) 0.023(5) 0.020(4) 0.001(4) 0.014(4) 0.010(5) C31 0.035(6) 0.025(6) 0.022(4) 0.005(4) 0.020(4) 0.015(5) C32 0.026(5) 0.026(6) 0.030(5) 0.009(4) 0.018(4) 0.014(5) C33 0.024(5) 0.019(5) 0.025(4) 0.008(4) 0.014(4) 0.009(5) C34 0.029(5) 0.029(6) 0.028(5) 0.011(4) 0.022(4) 0.013(5) C35 0.034(6) 0.019(6) 0.033(5) 0.002(4) 0.017(5) 0.009(5) C36 0.061(8) 0.049(8) 0.037(6) 0.000(5) 0.022(6) 0.034(7) C37 0.097(11) 0.049(8) 0.052(7) 0.016(6) 0.039(7) 0.047(9) C38 0.061(8) 0.064(9) 0.059(7) 0.012(7) 0.043(7) 0.040(8) C39 0.022(5) 0.045(7) 0.027(5) 0.009(5) 0.015(4) 0.021(5) C40 0.026(5) 0.051(7) 0.034(5) 0.016(5) 0.017(4) 0.023(6) C41 0.024(5) 0.038(7) 0.048(6) 0.012(5) 0.020(5) 0.017(5) C42 0.027(5) 0.052(8) 0.032(5) 0.009(5) 0.016(4) 0.019(6) C43 0.018(5) 0.034(6) 0.027(4) 0.010(4) 0.014(4) 0.010(5) C44 0.030(6) 0.031(7) 0.047(6) 0.009(5) 0.009(5) 0.012(6) C45 0.039(7) 0.037(8) 0.079(8) 0.021(7) 0.022(7) 0.020(7) C46 0.037(6) 0.077(10) 0.065(8) 0.050(8) 0.028(6) 0.035(7) C47 0.042(7) 0.076(10) 0.038(6) 0.031(6) 0.026(5) 0.033(7) C48 0.040(6) 0.056(8) 0.042(6) 0.024(6) 0.032(5) 0.030(6) C50 0.027(5) 0.037(6) 0.026(5) 0.008(5) 0.014(4) 0.012(5) C49 0.019(5) 0.045(7) 0.023(4) 0.013(5) 0.012(4) 0.015(5) C51 0.035(6) 0.061(8) 0.026(5) 0.012(6) 0.016(5) 0.014(6) C52 0.031(6) 0.037(7) 0.030(5) 0.011(5) 0.003(5) -0.005(6) C53 0.041(7) 0.027(7) 0.051(6) 0.015(6) 0.009(6) 0.005(6) C54 0.024(5) 0.032(7) 0.041(5) 0.011(5) 0.013(5) 0.008(5) C55 0.062(9) 0.071(11) 0.068(9) 0.041(9) 0.018(8) 0.000(9) 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 N5 U1 N6 173.7(3) N5 U1 O2 88.6(2) N6 U1 O2 86.6(2) N5 U1 O1 85.9(3) N6 U1 O1 91.5(3) O2 U1 O1 105.1(2) N5 U1 N3 85.5(3) N6 U1 N3 97.4(3) O2 U1 N3 77.8(2) O1 U1 N3 170.8(2) N5 U1 N1 98.3(2) N6 U1 N1 86.7(2) O2 U1 N1 172.35(19) O1 U1 N1 78.8(2) N3 U1 N1 99.4(2) C19 O1 U1 132.9(5) C34 O2 U1 137.2(6) C10 N1 C13 107.1(7) C10 N1 C1 108.0(6) C13 N1 C1 108.1(6) C10 N1 U1 117.1(4) C13 N1 U1 102.8(5) C1 N1 U1 113.1(5) C11 N2 C3 111.9(7) C11 N2 C4 110.9(7) C3 N2 C4 112.0(6) C6 N3 C5 107.5(7) C6 N3 C28 107.4(6) C5 N3 C28 106.2(6) C6 N3 U1 113.5(5) C5 N3 U1 117.2(5) C28 N3 U1 104.4(5) C9 N4 C12 112.3(7) C9 N4 C8 112.3(7) C12 N4 C8 111.1(7) C43 N5 U1 152.9(6) C49 N6 U1 152.1(6) N1 C1 C2 117.5(7) N1 C1 H1A 107.9 C2 C1 H1A 107.9 N1 C1 H1B 107.9 C2 C1 H1B 107.9 H1A C1 H1B 107.2 C3 C2 C1 112.0(7) C3 C2 H2A 109.2 C1 C2 H2A 109.2 C3 C2 H2B 109.2 C1 C2 H2B 109.2 H2A C2 H2B 107.9 N2 C3 C2 111.5(7) N2 C3 H3A 109.3 C2 C3 H3A 109.3 N2 C3 H3B 109.3 C2 C3 H3B 109.3 H3A C3 H3B 108.0 N2 C4 C5 117.7(7) N2 C4 H4A 107.9 C5 C4 H4A 107.9 N2 C4 H4B 107.9 C5 C4 H4B 107.9 H4A C4 H4B 107.2 C4 C5 N3 118.0(7) C4 C5 H5A 107.8 N3 C5 H5A 107.8 C4 C5 H5B 107.8 N3 C5 H5B 107.8 H5A C5 H5B 107.1 N3 C6 C7 116.8(7) N3 C6 H6A 108.1 C7 C6 H6A 108.1 N3 C6 H6B 108.1 C7 C6 H6B 108.1 H6A C6 H6B 107.3 C6 C7 C8 111.3(7) C6 C7 H7A 109.4 C8 C7 H7A 109.4 C6 C7 H7B 109.4 C8 C7 H7B 109.4 H7A C7 H7B 108.0 N4 C8 C7 109.9(6) N4 C8 H8A 109.7 C7 C8 H8A 109.7 N4 C8 H8B 109.7 C7 C8 H8B 109.7 H8A C8 H8B 108.2 N4 C9 C10 118.3(7) N4 C9 H9A 107.7 C10 C9 H9A 107.7 N4 C9 H9B 107.7 C10 C9 H9B 107.7 H9A C9 H9B 107.1 N1 C10 C9 117.4(7) N1 C10 H10A 107.9 C9 C10 H10A 107.9 N1 C10 H10B 107.9 C9 C10 H10B 107.9 H10A C10 H10B 107.2 N2 C11 H11A 109.5 N2 C11 H11B 109.5 H11A C11 H11B 109.5 N2 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 N4 C12 H12A 109.5 N4 C12 H12B 109.5 H12A C12 H12B 109.5 N4 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C14 C13 N1 116.6(7) C14 C13 H13A 108.1 N1 C13 H13A 108.1 C14 C13 H13B 108.1 N1 C13 H13B 108.1 H13A C13 H13B 107.3 C15 C14 C19 118.8(10) C15 C14 C13 120.6(8) C19 C14 C13 120.4(8) C16 C15 C14 122.9(8) C16 C15 H15 118.5 C14 C15 H15 118.5 C15 C16 C17 116.9(9) C15 C16 C20 123.6(8) C17 C16 C20 119.5(9) C18 C17 C16 122.2(10) C18 C17 H17 118.9 C16 C17 H17 118.9 C19 C18 C17 118.3(8) C19 C18 C24 121.7(8) C17 C18 C24 119.9(9) O1 C19 C18 121.8(7) O1 C19 C14 117.5(9) C18 C19 C14 120.7(8) C23 C20 C22 107.5(12) C23 C20 C16 110.9(10) C22 C20 C16 111.0(9) C23 C20 C21 113.0(11) C22 C20 C21 102.5(10) C16 C20 C21 111.6(10) C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C20 C23 H23A 109.5 C20 C23 H23B 109.5 H23A C23 H23B 109.5 C20 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C26 C24 C25 106.4(8) C26 C24 C27 110.8(7) C25 C24 C27 107.6(8) C26 C24 C18 108.8(8) C25 C24 C18 112.8(8) C27 C24 C18 110.3(7) C24 C25 H25A 109.5 C24 C25 H25B 109.5 H25A C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 H26A C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C24 C27 H27A 109.5 C24 C27 H27B 109.5 H27A C27 H27B 109.5 C24 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C29 C28 N3 117.1(6) C29 C28 H28A 108.0 N3 C28 H28A 108.0 C29 C28 H28B 108.0 N3 C28 H28B 108.0 H28A C28 H28B 107.3 C34 C29 C30 119.4(7) C34 C29 C28 121.2(8) C30 C29 C28 119.1(8) C31 C30 C29 121.3(9) C31 C30 H30 119.3 C29 C30 H30 119.3 C32 C31 C30 117.1(8) C32 C31 C35 119.5(7) C30 C31 C35 123.3(8) C31 C32 C33 124.7(7) C31 C32 H32 117.6 C33 C32 H32 117.6 C34 C33 C32 115.1(8) C34 C33 C39 123.8(8) C32 C33 C39 121.0(7) O2 C34 C29 117.2(7) O2 C34 C33 120.4(8) C29 C34 C33 122.3(8) C36 C35 C37 108.4(9) C36 C35 C38 107.6(8) C37 C35 C38 108.8(8) C36 C35 C31 113.2(7) C37 C35 C31 108.9(7) C38 C35 C31 109.7(8) 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 C41 C39 C33 109.0(7) C41 C39 C42 109.8(8) C33 C39 C42 111.1(7) C41 C39 C40 108.8(7) C33 C39 C40 112.2(7) C42 C39 C40 105.9(7) 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 N5 C43 C48 119.5(9) N5 C43 C44 120.5(8) C48 C43 C44 119.9(8) C45 C44 C43 120.1(10) C45 C44 H44 119.9 C43 C44 H44 119.9 C44 C45 C46 119.6(11) C44 C45 H45 120.2 C46 C45 H45 120.2 C47 C46 C45 120.5(9) C47 C46 H46 119.8 C45 C46 H46 119.8 C46 C47 C48 121.6(10) C46 C47 H47 119.2 C48 C47 H47 119.2 C47 C48 C43 118.3(10) C47 C48 H48 120.8 C43 C48 H48 120.8 C51 C50 C49 120.1(9) C51 C50 H50 119.9 C49 C50 H50 119.9 C54 C49 N6 120.9(7) C54 C49 C50 118.3(9) N6 C49 C50 120.7(8) C50 C51 C52 122.7(9) C50 C51 H51 118.7 C52 C51 H51 118.7 C51 C52 C53 116.3(10) C51 C52 C55 121.8(11) C53 C52 C55 121.9(11) C52 C53 C54 122.8(10) C52 C53 H53 118.6 C54 C53 H53 118.6 C49 C54 C53 119.6(9) C49 C54 H54 120.2 C53 C54 H54 120.2 C52 C55 H55A 109.5 C52 C55 H55B 109.5 H55A C55 H55B 109.5 C52 C55 H55C 109.5 H55A C55 H55C 109.5 H55B C55 H55C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance U1 N5 1.909(6) U1 N6 1.911(7) U1 O2 2.163(5) U1 O1 2.170(6) U1 N3 2.713(8) U1 N1 2.738(6) O1 C19 1.345(10) O2 C34 1.348(10) N1 C10 1.475(10) N1 C13 1.498(10) N1 C1 1.499(11) N2 C11 1.455(13) N2 C3 1.475(10) N2 C4 1.479(10) N3 C6 1.493(10) N3 C5 1.504(12) N3 C28 1.512(9) N4 C9 1.435(12) N4 C12 1.444(9) N4 C8 1.487(10) N5 C43 1.383(10) N6 C49 1.394(12) C1 C2 1.530(12) C1 H1A 0.9900 C1 H1B 0.9900 C2 C3 1.521(14) C2 H2A 0.9900 C2 H2B 0.9900 C3 H3A 0.9900 C3 H3B 0.9900 C4 C5 1.501(11) C4 H4A 0.9900 C4 H4B 0.9900 C5 H5A 0.9900 C5 H5B 0.9900 C6 C7 1.507(13) C6 H6A 0.9900 C6 H6B 0.9900 C7 C8 1.531(10) C7 H7A 0.9900 C7 H7B 0.9900 C8 H8A 0.9900 C8 H8B 0.9900 C9 C10 1.543(11) C9 H9A 0.9900 C9 H9B 0.9900 C10 H10A 0.9900 C10 H10B 0.9900 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 C14 1.491(14) C13 H13A 0.9900 C13 H13B 0.9900 C14 C15 1.393(13) C14 C19 1.409(11) C15 C16 1.369(14) C15 H15 0.9500 C16 C17 1.419(12) C16 C20 1.515(13) C17 C18 1.406(12) C17 H17 0.9500 C18 C19 1.382(14) C18 C24 1.549(11) C20 C23 1.437(17) C20 C22 1.514(18) C20 C21 1.528(16) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 C26 1.522(13) C24 C25 1.527(14) C24 C27 1.537(11) C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 C29 1.510(10) C28 H28A 0.9900 C28 H28B 0.9900 C29 C34 1.385(13) C29 C30 1.404(12) C30 C31 1.389(11) C30 H30 0.9500 C31 C32 1.384(13) C31 C35 1.538(11) C32 C33 1.417(12) C32 H32 0.9500 C33 C34 1.405(11) C33 C39 1.530(13) C35 C36 1.510(14) C35 C37 1.517(13) C35 C38 1.523(13) 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 1.526(14) C39 C42 1.541(11) C39 C40 1.546(10) 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 1.401(13) C43 C44 1.398(14) C44 C45 1.379(13) C44 H44 0.9500 C45 C46 1.386(16) C45 H45 0.9500 C46 C47 1.360(17) C46 H46 0.9500 C47 C48 1.386(13) C47 H47 0.9500 C48 H48 0.9500 C50 C51 1.372(14) C50 C49 1.404(11) C50 H50 0.9500 C49 C54 1.386(13) C51 C52 1.384(16) C51 H51 0.9500 C52 C53 1.381(15) C52 C55 1.512(15) C53 C54 1.389(14) C53 H53 0.9500 C54 H54 0.9500 C55 H55A 0.9800 C55 H55B 0.9800 C55 H55C 0.9800