#------------------------------------------------------------------------------ #$Date: 2017-05-02 04:55:00 +0300 (Tue, 02 May 2017) $ #$Revision: 195887 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/28/7042834.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_7042834 loop_ _publ_author_name 'Xie, Zhen-ni' 'Mei, Lei' 'Wu, Qunyan' 'Hu, Kong-qiu' 'Xia, Liang-Shu' 'Chai, Zhifang' 'Shi, Weiqun' _publ_section_title ; Temperature-induced Reversible Single-Crystal-to-Single-Crystal Isomerisation of Uranyl Polyrotaxane: An Exquisite Case of Coordination Variability of Uranyl Center ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT01034F _journal_year 2017 _chemical_formula_sum 'C108 H112 Br2 N52 O34 U' _chemical_formula_weight 3080.34 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _audit_update_record ; 2017-02-22 deposited with the CCDC. 2017-05-01 downloaded from the CCDC. ; _cell_angle_alpha 91.261(2) _cell_angle_beta 97.291(2) _cell_angle_gamma 93.699(2) _cell_formula_units_Z 1 _cell_length_a 12.7846(5) _cell_length_b 14.7915(6) _cell_length_c 17.0792(7) _cell_measurement_reflns_used 9577 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.60 _cell_measurement_theta_min 3.03 _cell_volume 3195.5(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 72367 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_min 2.978 _exptl_absorpt_coefficient_mu 1.995 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.601 _exptl_crystal_description block _exptl_crystal_F_000 1558 _refine_diff_density_max 1.963 _refine_diff_density_min -3.379 _refine_diff_density_rms 0.155 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 889 _refine_ls_number_reflns 14613 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0573 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+9.7677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1614 _refine_ls_wR_factor_ref 0.1683 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13732 _reflns_number_total 14613 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01034f2.cif _cod_data_source_block 5-bUP-296K _cod_database_code 7042834 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL mo_20160512_XZN_40_2_273_0m_a.res in P-1 REM Old TITL mo_20160512_XZN_40_2_273_0m in P1 REM SHELXT solution in P-1 REM R1 0.120, Rweak 0.031, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C132 N32 O32 U CELL 0.71073 12.7846 14.7915 17.0792 91.261 97.291 93.699 ZERR 1 0.0005 0.0006 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H N O U Br UNIT 108 112 52 34 1 2 TEMP -0.010 L.S. 10 BOND $H acta LIST 6 FMAP 2 isor 0.01 Br1 PLAN 20 WGHT 0.110000 9.767700 FVAR 0.11216 U1 5 1.000000 0.000000 0.500000 10.50000 0.02586 0.03009 = 0.02494 0.00225 0.01180 0.00101 N1 3 0.694555 0.327316 0.375322 11.00000 0.03168 0.02906 = 0.01991 -0.00478 0.00192 0.00816 C1 1 0.944678 0.155688 0.360691 11.00000 0.02111 0.04968 = 0.03039 -0.00130 -0.00285 0.00912 O1 4 1.070554 0.099728 0.540319 11.00000 0.03511 0.05463 = 0.07033 -0.01752 0.01983 -0.01169 N2 3 0.625214 0.059863 0.775212 11.00000 0.03795 0.02918 = 0.02124 0.01038 0.01948 0.01033 C2 1 0.856277 0.217274 0.367787 11.00000 0.02290 0.03650 = 0.01698 -0.00212 -0.00245 0.00185 O2 4 0.934296 0.078903 0.394493 11.00000 0.06374 0.07047 = 0.03795 0.02322 0.01640 0.03694 O3 4 1.012153 0.177461 0.320250 11.00000 0.02406 0.06417 = 0.08537 0.00908 0.01978 0.00731 N3 3 0.858183 0.543125 0.608799 11.00000 0.03026 0.03741 = 0.02491 0.00085 0.00655 0.00581 C3 1 0.859483 0.301561 0.335319 11.00000 0.02192 0.03409 = 0.03177 -0.00174 0.00289 -0.00691 AFIX 43 H3 2 0.916747 0.321013 0.309973 11.00000 -1.20000 AFIX 0 O4 4 0.867452 0.038805 0.571141 11.00000 0.03573 0.04802 = 0.04429 -0.00188 0.02450 0.00521 N4 3 0.801017 0.424197 0.672253 11.00000 0.03445 0.03391 = 0.02922 0.00240 0.00967 0.00535 C4 1 0.778247 0.357084 0.340257 11.00000 0.03991 0.02549 = 0.02969 -0.00280 0.00513 -0.00405 AFIX 43 H4 2 0.781100 0.414691 0.319556 11.00000 -1.20000 AFIX 0 O5 4 0.714316 -0.024933 0.511021 11.00000 0.05869 0.09928 = 0.03957 -0.03096 0.02185 -0.01936 N5 3 0.674794 0.297862 0.684437 11.00000 0.03466 0.03725 = 0.02708 0.00171 0.00864 0.00203 C5 1 0.688194 0.245537 0.406715 11.00000 0.03211 0.03897 = 0.02314 0.00640 0.00884 0.00713 AFIX 43 H5 2 0.628745 0.226707 0.429839 11.00000 -1.20000 AFIX 0 O6 4 0.666819 0.218060 0.566033 11.00000 0.05288 0.04173 = 0.02863 0.00204 0.01044 0.01349 N6 3 0.523680 0.224185 0.635649 11.00000 0.03790 0.02885 = 0.03037 -0.00285 0.00453 0.00342 C6 1 0.769592 0.188899 0.404936 11.00000 0.03285 0.03588 = 0.02431 0.00984 0.00555 0.00541 AFIX 43 H6 2 0.766562 0.132683 0.428186 11.00000 -1.20000 AFIX 0 N7 3 0.374509 0.221885 0.533964 11.00000 0.03913 0.02558 = 0.03085 -0.00030 0.00523 0.00372 C7 1 0.604674 0.385667 0.377632 11.00000 0.03937 0.04016 = 0.02510 -0.00096 0.00033 0.01834 AFIX 23 H7A 2 0.539131 0.350464 0.359348 11.00000 -1.20000 H7B 2 0.611876 0.435247 0.342041 11.00000 -1.20000 AFIX 0 C55 1 0.376265 0.231030 0.454186 11.00000 0.03490 0.01648 = 0.03240 -0.00246 0.00328 -0.00476 O8 4 0.447472 0.213238 0.417615 11.00000 0.03769 0.03685 = 0.04001 -0.00283 0.01015 0.00770 N8 3 0.281178 0.263202 0.423917 11.00000 0.03169 0.03156 = 0.02691 0.00397 0.00722 -0.00024 C8 1 0.599629 0.423794 0.459893 11.00000 0.03406 0.03418 = 0.02697 -0.00230 0.00318 0.01097 AFIX 23 H8A 2 0.664168 0.460470 0.478014 11.00000 -1.20000 H8B 2 0.593249 0.374579 0.495962 11.00000 -1.20000 AFIX 0 O9 4 0.603855 0.635767 0.749954 11.00000 0.03080 0.02872 = 0.03232 -0.00190 0.01211 0.00349 N9 3 0.180988 0.358742 0.501121 11.00000 0.02832 0.02976 = 0.02434 -0.00031 0.00003 0.00139 C9 1 0.505535 0.481187 0.459336 11.00000 0.03754 0.03607 = 0.02787 -0.00319 0.00189 0.01432 AFIX 23 H9A 2 0.513330 0.530993 0.424063 11.00000 -1.20000 H9B 2 0.441664 0.444672 0.439139 11.00000 -1.20000 AFIX 0 O00D 4 0.849898 0.401267 0.548000 11.00000 0.04846 0.04294 = 0.03592 -0.00339 0.01274 0.01051 O10 4 0.430539 0.474033 0.768425 11.00000 0.03832 0.03200 = 0.03713 0.00137 0.00668 0.00596 N10 3 0.272814 0.315890 0.610892 11.00000 0.03139 0.03144 = 0.02212 0.00118 0.00296 0.00311 C10 1 0.769623 0.009415 0.568211 11.00000 0.04220 0.03202 = 0.03030 -0.00349 0.02047 -0.00050 O11 4 0.191720 0.449907 0.613724 11.00000 0.04497 0.03388 = 0.03173 -0.00515 0.00253 0.00606 N11 3 0.429284 0.332836 0.706611 11.00000 0.03154 0.03138 = 0.02280 0.00095 0.00257 0.00587 C11 1 0.722510 0.026662 0.644193 11.00000 0.03181 0.02297 = 0.02498 0.00672 0.01532 0.00779 O12 4 0.637256 -0.149469 0.799408 11.00000 0.03425 0.02978 = 0.02414 0.00292 0.00991 0.00388 N12 3 0.582124 0.398673 0.763219 11.00000 0.03244 0.02454 = 0.02954 0.00283 0.00717 0.00133 C12 1 0.618819 -0.003685 0.646934 11.00000 0.03710 0.03055 = 0.02808 0.00003 0.01562 -0.00238 AFIX 43 H12 2 0.580434 -0.035807 0.604116 11.00000 -1.20000 AFIX 0 O13 4 0.363352 -0.072877 0.737750 11.00000 0.02872 0.04278 = 0.04116 0.00497 0.01142 -0.00432 N13 3 0.716556 0.520751 0.761140 11.00000 0.02679 0.03058 = 0.02699 0.00511 0.00939 0.00157 C13 1 0.572893 0.013991 0.713449 11.00000 0.03383 0.03472 = 0.03628 0.00609 0.02102 -0.00049 AFIX 43 H13 2 0.503045 -0.006828 0.715213 11.00000 -1.20000 AFIX 0 O14 4 0.315039 0.134235 0.794484 11.00000 0.05251 0.03484 = 0.03135 0.00664 0.01814 -0.00056 N14 3 0.750245 0.634744 0.684045 11.00000 0.02377 0.02998 = 0.02935 0.00276 0.00767 0.00154 C14 1 0.727841 0.087982 0.775480 11.00000 0.03650 0.04112 = 0.02082 0.00344 0.00815 0.00650 AFIX 43 H14 2 0.764957 0.118248 0.819794 11.00000 -1.20000 AFIX 0 O15 4 0.506004 0.285482 0.891497 11.00000 0.05690 0.04402 = 0.02292 0.00478 0.01896 0.00836 N15 3 0.535623 0.315001 1.025656 11.00000 0.03150 0.04282 = 0.02192 0.00457 0.01136 0.00650 C15 1 0.777678 0.071754 0.709861 11.00000 0.02696 0.04203 = 0.03218 0.00612 0.01329 0.00701 AFIX 43 H15 2 0.848337 0.091192 0.709928 11.00000 -1.20000 AFIX 0 O16 4 0.237888 -0.206049 1.053145 11.00000 0.05409 0.05804 = 0.03059 0.00032 0.01955 0.00881 N16 3 0.370435 0.285228 0.969348 11.00000 0.03867 0.03667 = 0.01726 0.00203 0.00589 0.00437 C16 1 0.568253 0.082376 0.843652 11.00000 0.05750 0.03187 = 0.03195 0.01129 0.03305 0.01677 AFIX 23 H16A 2 0.496354 0.095025 0.823783 11.00000 -1.20000 H16B 2 0.602369 0.137110 0.870318 11.00000 -1.20000 AFIX 0 O17 4 0.156896 0.013073 1.101487 11.00000 0.03763 0.04691 = 0.03193 0.00819 0.01037 0.00461 N17 3 0.233987 0.184301 0.898686 11.00000 0.04535 0.03243 = 0.02744 0.00141 0.01023 0.00166 C17 1 0.564989 0.008425 0.902946 11.00000 0.03721 0.03081 = 0.02044 0.00768 0.01758 0.01255 AFIX 23 H17A 2 0.636483 -0.004451 0.923742 11.00000 -1.20000 H17B 2 0.529949 -0.046487 0.877214 11.00000 -1.20000 AFIX 0 N18 3 0.181329 0.049541 0.842724 11.00000 0.02870 0.03666 = 0.02917 -0.00184 0.00937 0.00000 C18 1 0.505633 0.037617 0.970688 11.00000 0.04383 0.03102 = 0.02401 0.00785 0.02155 0.01320 AFIX 23 H18A 2 0.543311 0.090482 0.998114 11.00000 -1.20000 H18B 2 0.435940 0.054517 0.949192 11.00000 -1.20000 AFIX 0 N19 3 0.218807 -0.101544 0.802984 11.00000 0.02301 0.03396 = 0.03630 -0.00018 0.00902 -0.00082 C19 1 0.681602 0.600755 0.733009 11.00000 0.02435 0.02464 = 0.01912 -0.00546 0.00205 -0.00502 N22 3 0.688099 -0.234672 0.907167 11.00000 0.02775 0.03644 = 0.02253 0.00341 0.00519 0.00262 C22 1 0.837817 0.450804 0.603870 11.00000 0.02110 0.03810 = 0.02798 0.00334 0.00327 0.00851 N21 3 0.517934 -0.243066 0.856765 11.00000 0.02491 0.03008 = 0.01792 -0.00284 0.00670 0.00369 C21 1 0.812910 0.497167 0.731474 11.00000 0.02153 0.03693 = 0.02577 0.00458 0.00109 0.00423 AFIX 13 H21 2 0.868607 0.486754 0.774650 11.00000 -1.20000 AFIX 0 N20 3 0.342187 -0.200338 0.809869 11.00000 0.02349 0.04059 = 0.02775 0.00172 0.01038 0.00154 C20 1 0.842137 0.581046 0.684716 11.00000 0.01817 0.03864 = 0.02443 0.00101 0.00141 -0.00132 AFIX 13 H20 2 0.906347 0.614555 0.710571 11.00000 -1.20000 AFIX 0 N23 3 0.294734 -0.252034 0.936590 11.00000 0.02888 0.03985 = 0.02623 0.00150 0.01067 0.00424 C23 1 0.655445 0.463990 0.808706 11.00000 0.03491 0.03569 = 0.01790 0.00078 0.00630 -0.00118 AFIX 23 H23A 2 0.703407 0.431984 0.845140 11.00000 -1.20000 H23B 2 0.616345 0.502208 0.839740 11.00000 -1.20000 AFIX 0 N24 3 0.177762 -0.147216 0.933008 11.00000 0.02806 0.04417 = 0.03197 -0.00209 0.01291 0.00563 C24 1 0.784750 0.329416 0.690171 11.00000 0.03242 0.03357 = 0.03854 0.00706 0.00621 0.01148 AFIX 23 H24A 2 0.818975 0.293250 0.654116 11.00000 -1.20000 H24B 2 0.818380 0.320115 0.743288 11.00000 -1.20000 AFIX 0 N25 3 0.121862 0.000914 0.966113 11.00000 0.03553 0.03705 = 0.03122 -0.00089 0.01015 0.00128 C25 1 0.475777 0.408997 0.748436 11.00000 0.03327 0.02904 = 0.02047 0.00730 0.00620 0.00252 N26 3 0.170721 0.135879 1.021457 11.00000 0.02888 0.03773 = 0.02598 0.00023 0.00443 0.00085 C26 1 0.608401 0.307917 0.746383 11.00000 0.03171 0.02603 = 0.02142 0.00704 0.00417 0.00389 AFIX 13 H26 2 0.637251 0.278682 0.794602 11.00000 -1.20000 AFIX 0 C29 1 0.316090 0.316305 0.693192 11.00000 0.03283 0.03904 = 0.02223 0.00841 0.00981 0.00400 AFIX 23 H29A 2 0.284258 0.362646 0.721519 11.00000 -1.20000 H29B 2 0.297100 0.258266 0.714728 11.00000 -1.20000 AFIX 0 C28 1 0.625851 0.245046 0.622090 11.00000 0.04223 0.02518 = 0.02240 0.00819 0.00210 0.01004 C27 1 0.501302 0.260347 0.710553 11.00000 0.03637 0.02285 = 0.02442 0.00977 0.00496 0.00307 AFIX 13 H27 2 0.478795 0.211875 0.744193 11.00000 -1.20000 AFIX 0 C30 1 0.449393 0.169404 0.580689 11.00000 0.04872 0.01776 = 0.03877 -0.00132 -0.00054 0.00560 AFIX 23 H30A 2 0.411094 0.125655 0.609807 11.00000 -1.20000 H30B 2 0.488062 0.136018 0.545608 11.00000 -1.20000 AFIX 0 C31 1 0.213758 0.382091 0.579053 11.00000 0.02414 0.02753 = 0.02595 0.00112 0.00427 -0.00638 C32 1 0.273060 0.237597 0.557617 11.00000 0.03637 0.02058 = 0.02570 0.00262 0.00548 -0.00422 AFIX 13 H32 2 0.240148 0.182897 0.578131 11.00000 -1.20000 AFIX 0 C33 1 0.207644 0.268266 0.480875 11.00000 0.02641 0.02541 = 0.02542 -0.00053 0.00379 -0.00874 AFIX 13 H33 2 0.144184 0.227797 0.465791 11.00000 -1.20000 AFIX 0 C34 1 0.102211 0.406701 0.453946 11.00000 0.02108 0.04559 = 0.02726 0.00578 0.00601 0.00241 AFIX 23 H34A 2 0.072157 0.448405 0.488140 11.00000 -1.20000 H34B 2 0.045785 0.363391 0.431107 11.00000 -1.20000 AFIX 0 C35 1 0.251324 0.271963 0.339798 11.00000 0.03440 0.02503 = 0.02668 -0.00260 0.00625 -0.00477 AFIX 23 H35A 2 0.300679 0.241344 0.311531 11.00000 -1.20000 H35B 2 0.181703 0.241927 0.324896 11.00000 -1.20000 AFIX 0 C36 1 0.648862 0.328413 1.032565 11.00000 0.03612 0.03533 = 0.03361 0.00637 0.01684 0.00156 AFIX 23 H36A 2 0.671227 0.381136 1.066821 11.00000 -1.20000 H36B 2 0.668870 0.341442 0.980859 11.00000 -1.20000 AFIX 0 C37 1 0.474245 0.293101 0.955389 11.00000 0.04436 0.02423 = 0.02406 0.00300 0.01156 0.00775 C38 1 0.474282 0.318741 1.091209 11.00000 0.03097 0.02683 = 0.02137 -0.00339 0.00998 0.00404 AFIX 13 H38 2 0.488351 0.376699 1.120782 11.00000 -1.20000 AFIX 0 C39 1 0.284113 0.274249 0.906425 11.00000 0.04820 0.03068 = 0.02427 0.00758 0.00227 0.00485 AFIX 23 H39A 2 0.231823 0.316614 0.915655 11.00000 -1.20000 H39B 2 0.310171 0.289411 0.857099 11.00000 -1.20000 AFIX 0 C40 1 0.250926 0.123878 0.840421 11.00000 0.03470 0.02961 = 0.02338 0.00780 0.00382 0.00639 C41 1 0.144898 0.155455 0.939115 11.00000 0.02608 0.03784 = 0.02614 0.00244 0.00215 0.00838 AFIX 13 H41 2 0.088423 0.197357 0.931194 11.00000 -1.20000 AFIX 0 C42 1 0.109346 0.060917 0.900074 11.00000 0.02011 0.04259 = 0.03121 -0.00246 0.00385 0.00516 AFIX 13 H42 2 0.035847 0.058598 0.875018 11.00000 -1.20000 AFIX 0 C43 1 0.201515 0.205002 1.083682 11.00000 0.02530 0.04426 = 0.02538 -0.00221 0.00940 0.00809 AFIX 23 H43A 2 0.160225 0.256996 1.072283 11.00000 -1.20000 H43B 2 0.184317 0.181210 1.133304 11.00000 -1.20000 AFIX 0 C44 1 0.152023 0.046498 1.036725 11.00000 0.01806 0.04315 = 0.03113 0.00348 0.00798 0.00749 C45 1 0.096006 -0.096055 0.960013 11.00000 0.02697 0.04132 = 0.04613 -0.00115 0.02100 -0.00082 AFIX 23 H45A 2 0.082487 -0.117181 1.011384 11.00000 -1.20000 H45B 2 0.031452 -0.107955 0.923837 11.00000 -1.20000 AFIX 0 C46 1 0.166668 -0.020413 0.781666 11.00000 0.02794 0.04176 = 0.02593 -0.00437 -0.00165 0.00238 AFIX 23 H46A 2 0.193000 0.003354 0.734877 11.00000 -1.20000 H46B 2 0.091580 -0.036107 0.768282 11.00000 -1.20000 AFIX 0 C47 1 0.236742 -0.202367 0.981960 11.00000 0.02812 0.03656 = 0.03323 -0.00211 0.01359 -0.00216 C48 1 0.178201 -0.171985 0.849977 11.00000 0.01892 0.03517 = 0.03109 -0.00432 0.00585 -0.00311 AFIX 13 H48 2 0.108768 -0.197853 0.825866 11.00000 -1.20000 AFIX 0 C49 1 0.262375 -0.242846 0.852953 11.00000 0.02579 0.03072 = 0.02742 -0.00352 0.00788 -0.00283 AFIX 13 H49 2 0.232892 -0.300669 0.827709 11.00000 -1.20000 AFIX 0 C50 1 0.314265 -0.119725 0.779860 11.00000 0.02273 0.03467 = 0.02312 -0.00472 0.00243 -0.00372 C51 1 0.434262 -0.244155 0.791153 11.00000 0.03020 0.03840 = 0.01831 -0.00250 0.00824 0.00545 AFIX 23 H51A 2 0.461157 -0.214038 0.747192 11.00000 -1.20000 H51B 2 0.413408 -0.306543 0.774516 11.00000 -1.20000 AFIX 0 C52 1 0.616762 -0.203261 0.848497 11.00000 0.02786 0.02465 = 0.01832 -0.00526 0.00729 0.00497 C53 1 0.642074 -0.307110 0.949653 11.00000 0.03207 0.02802 = 0.02118 -0.00124 0.00639 0.00692 AFIX 13 H53 2 0.678616 -0.362895 0.945328 11.00000 -1.20000 AFIX 0 BR1 6 0.033009 0.616420 0.880185 11.00000 0.21155 0.25958 = 0.25390 0.10882 -0.06134 -0.12488 HKLF 4 REM mo_20160512_XZN_40_2_273_0m_a.res in P-1 REM R1 = 0.0573 for 13732 Fo > 4sig(Fo) and 0.0627 for all 14613 data REM 889 parameters refined using 6 restraints END WGHT 0.1073 8.6552 REM Highest difference peak 1.963, deepest hole -3.379, 1-sigma level 0.155 Q1 1 0.8251 -0.4697 0.9846 11.00000 0.05 1.95 Q2 1 0.9972 0.2636 0.5987 11.00000 0.05 1.93 Q3 1 -0.0619 0.2991 0.8772 11.00000 0.05 1.64 Q4 1 0.9819 0.1238 0.4326 11.00000 0.05 1.36 Q5 1 0.1205 0.4200 0.9766 11.00000 0.05 1.23 Q6 1 1.0419 0.1997 0.7535 11.00000 0.05 1.00 Q7 1 1.0986 0.0540 0.5751 11.00000 0.05 0.96 Q8 1 0.0401 0.6991 0.9353 11.00000 0.05 0.88 Q9 1 1.0577 0.4223 0.7475 11.00000 0.05 0.87 Q10 1 -0.0668 0.5820 0.8919 11.00000 0.05 0.87 Q11 1 0.0000 0.5000 1.0000 10.50000 0.05 0.85 Q12 1 -0.0037 0.6782 0.8400 11.00000 0.05 0.71 Q13 1 0.0955 0.6196 0.9396 11.00000 0.05 0.69 Q14 1 0.9497 -0.0248 0.4860 11.00000 0.05 0.62 Q15 1 0.0628 0.6445 0.8151 11.00000 0.05 0.58 Q16 1 1.0009 0.1000 0.4990 11.00000 0.05 0.49 Q17 1 0.9029 0.1968 0.3733 11.00000 0.05 0.46 Q18 1 1.0275 0.2004 0.3602 11.00000 0.05 0.45 Q19 1 0.7474 0.4998 1.1516 11.00000 0.05 0.43 Q20 1 0.7830 0.6222 0.6832 11.00000 0.05 0.42 ; _shelx_res_checksum 98725 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 _atom_site_refinement_flags_occupancy U1 U 1.0000 0.0000 0.5000 0.02624(9) Uani 1 2 d S . P N1 N 0.6946(3) 0.3273(3) 0.3753(2) 0.0268(7) Uani 1 1 d . . . C1 C 0.9447(4) 0.1557(4) 0.3607(3) 0.0340(10) Uani 1 1 d . . . O1 O 1.0706(3) 0.0997(3) 0.5403(3) 0.0532(11) Uani 1 1 d . . . N2 N 0.6252(3) 0.0599(3) 0.7752(2) 0.0276(8) Uani 1 1 d . . . C2 C 0.8563(3) 0.2173(3) 0.3678(2) 0.0259(8) Uani 1 1 d . . . O2 O 0.9343(4) 0.0789(3) 0.3945(2) 0.0548(12) Uani 1 1 d . . . O3 O 1.0122(3) 0.1775(3) 0.3202(3) 0.0565(12) Uani 1 1 d . . . N3 N 0.8582(3) 0.5431(3) 0.6088(2) 0.0304(8) Uani 1 1 d . . . C3 C 0.8595(3) 0.3016(3) 0.3353(3) 0.0297(9) Uani 1 1 d . . . H3 H 0.9167 0.3210 0.3100 0.036 Uiso 1 1 calc R U . O4 O 0.8675(3) 0.0388(3) 0.5711(2) 0.0410(8) Uani 1 1 d . . . N4 N 0.8010(3) 0.4242(3) 0.6723(2) 0.0319(8) Uani 1 1 d . . . C4 C 0.7782(4) 0.3571(3) 0.3403(3) 0.0320(9) Uani 1 1 d . . . H4 H 0.7811 0.4147 0.3196 0.038 Uiso 1 1 calc R U . O5 O 0.7143(4) -0.0249(4) 0.5110(3) 0.0661(15) Uani 1 1 d . . . N5 N 0.6748(3) 0.2979(3) 0.6844(2) 0.0326(8) Uani 1 1 d . . . C5 C 0.6882(4) 0.2455(3) 0.4067(3) 0.0307(9) Uani 1 1 d . . . H5 H 0.6287 0.2267 0.4298 0.037 Uiso 1 1 calc R U . O6 O 0.6668(3) 0.2181(3) 0.5660(2) 0.0402(8) Uani 1 1 d . . . N6 N 0.5237(3) 0.2242(3) 0.6356(2) 0.0324(8) Uani 1 1 d . . . C6 C 0.7696(4) 0.1889(3) 0.4049(3) 0.0306(9) Uani 1 1 d . . . H6 H 0.7666 0.1327 0.4282 0.037 Uiso 1 1 calc R U . N7 N 0.3745(3) 0.2219(3) 0.5340(2) 0.0317(8) Uani 1 1 d . . . C7 C 0.6047(4) 0.3857(4) 0.3776(3) 0.0346(10) Uani 1 1 d . . . H7A H 0.5391 0.3505 0.3593 0.041 Uiso 1 1 calc R U . H7B H 0.6119 0.4352 0.3420 0.041 Uiso 1 1 calc R U . C55 C 0.3763(4) 0.2310(3) 0.4542(3) 0.0283(9) Uani 1 1 d . . . O8 O 0.4475(3) 0.2132(2) 0.4176(2) 0.0376(8) Uani 1 1 d . . . N8 N 0.2812(3) 0.2632(3) 0.4239(2) 0.0298(8) Uani 1 1 d . . . C8 C 0.5996(4) 0.4238(3) 0.4599(3) 0.0315(9) Uani 1 1 d . . . H8A H 0.6642 0.4605 0.4780 0.038 Uiso 1 1 calc R U . H8B H 0.5932 0.3746 0.4960 0.038 Uiso 1 1 calc R U . O9 O 0.6039(3) 0.6358(2) 0.7500(2) 0.0299(7) Uani 1 1 d . . . N9 N 0.1810(3) 0.3587(3) 0.5011(2) 0.0278(7) Uani 1 1 d . . . C9 C 0.5055(4) 0.4812(3) 0.4593(3) 0.0336(10) Uani 1 1 d . . . H9A H 0.5133 0.5310 0.4241 0.040 Uiso 1 1 calc R U . H9B H 0.4417 0.4447 0.4391 0.040 Uiso 1 1 calc R U . O00D O 0.8499(3) 0.4013(3) 0.5480(2) 0.0416(8) Uani 1 1 d . . . O10 O 0.4305(3) 0.4740(2) 0.7684(2) 0.0355(7) Uani 1 1 d . . . N10 N 0.2728(3) 0.3159(3) 0.6109(2) 0.0283(8) Uani 1 1 d . . . C10 C 0.7696(4) 0.0094(3) 0.5682(3) 0.0337(10) Uani 1 1 d . . . O11 O 0.1917(3) 0.4499(2) 0.6137(2) 0.0370(8) Uani 1 1 d . . . N11 N 0.4293(3) 0.3328(3) 0.7066(2) 0.0285(8) Uani 1 1 d . . . C11 C 0.7225(4) 0.0267(3) 0.6442(3) 0.0252(8) Uani 1 1 d . . . O12 O 0.6373(3) -0.1495(2) 0.79941(18) 0.0288(6) Uani 1 1 d . . . N12 N 0.5821(3) 0.3987(3) 0.7632(2) 0.0286(8) Uani 1 1 d . . . C12 C 0.6188(4) -0.0037(3) 0.6469(3) 0.0311(9) Uani 1 1 d . . . H12 H 0.5804 -0.0358 0.6041 0.037 Uiso 1 1 calc R U . O13 O 0.3634(3) -0.0729(3) 0.7377(2) 0.0372(8) Uani 1 1 d . . . N13 N 0.7166(3) 0.5208(3) 0.7611(2) 0.0276(7) Uani 1 1 d . . . C13 C 0.5729(4) 0.0140(3) 0.7134(3) 0.0336(10) Uani 1 1 d . . . H13 H 0.5030 -0.0068 0.7152 0.040 Uiso 1 1 calc R U . O14 O 0.3150(3) 0.1342(2) 0.7945(2) 0.0385(8) Uani 1 1 d . . . N14 N 0.7502(3) 0.6347(3) 0.6840(2) 0.0273(7) Uani 1 1 d . . . C14 C 0.7278(4) 0.0880(3) 0.7755(3) 0.0322(9) Uani 1 1 d . . . H14 H 0.7650 0.1182 0.8198 0.039 Uiso 1 1 calc R U . O15 O 0.5060(3) 0.2855(3) 0.8915(2) 0.0398(8) Uani 1 1 d . . . N15 N 0.5356(3) 0.3150(3) 1.0257(2) 0.0312(8) Uani 1 1 d . . . C15 C 0.7777(4) 0.0718(3) 0.7099(3) 0.0326(10) Uani 1 1 d . . . H15 H 0.8483 0.0912 0.7099 0.039 Uiso 1 1 calc R U . O16 O 0.2379(3) -0.2060(3) 1.0531(2) 0.0462(9) Uani 1 1 d . . . N16 N 0.3704(3) 0.2852(3) 0.9693(2) 0.0306(8) Uani 1 1 d . . . C16 C 0.5683(5) 0.0824(3) 0.8437(3) 0.0373(12) Uani 1 1 d . . . H16A H 0.4964 0.0950 0.8238 0.045 Uiso 1 1 calc R U . H16B H 0.6024 0.1371 0.8703 0.045 Uiso 1 1 calc R U . O17 O 0.1569(3) 0.0131(3) 1.1015(2) 0.0381(8) Uani 1 1 d . . . N17 N 0.2340(4) 0.1843(3) 0.8987(2) 0.0346(9) Uani 1 1 d . . . C17 C 0.5650(4) 0.0084(3) 0.9029(3) 0.0277(9) Uani 1 1 d . . . H17A H 0.6365 -0.0045 0.9237 0.033 Uiso 1 1 calc R U . H17B H 0.5299 -0.0465 0.8772 0.033 Uiso 1 1 calc R U . N18 N 0.1813(3) 0.0495(3) 0.8427(2) 0.0312(8) Uani 1 1 d . . . C18 C 0.5056(4) 0.0376(3) 0.9707(3) 0.0309(10) Uani 1 1 d . . . H18A H 0.5433 0.0905 0.9981 0.037 Uiso 1 1 calc R U . H18B H 0.4359 0.0545 0.9492 0.037 Uiso 1 1 calc R U . N19 N 0.2188(3) -0.1015(3) 0.8030(2) 0.0308(8) Uani 1 1 d . . . C19 C 0.6816(3) 0.6008(3) 0.7330(2) 0.0231(8) Uani 1 1 d . . . N22 N 0.6881(3) -0.2347(3) 0.9072(2) 0.0287(8) Uani 1 1 d . . . C22 C 0.8378(3) 0.4508(3) 0.6039(3) 0.0287(9) Uani 1 1 d . . . N21 N 0.5179(3) -0.2431(2) 0.8568(2) 0.0239(7) Uani 1 1 d . . . C21 C 0.8129(3) 0.4972(3) 0.7315(3) 0.0281(9) Uani 1 1 d . . . H21 H 0.8686 0.4868 0.7747 0.034 Uiso 1 1 calc R U . N20 N 0.3422(3) -0.2003(3) 0.8099(2) 0.0300(8) Uani 1 1 d . . . C20 C 0.8421(3) 0.5810(3) 0.6847(3) 0.0273(9) Uani 1 1 d . . . H20 H 0.9063 0.6146 0.7106 0.033 Uiso 1 1 calc R U . N23 N 0.2947(3) -0.2520(3) 0.9366(2) 0.0310(8) Uani 1 1 d . . . C23 C 0.6554(4) 0.4640(3) 0.8087(3) 0.0294(9) Uani 1 1 d . . . H23A H 0.7034 0.4320 0.8451 0.035 Uiso 1 1 calc R U . H23B H 0.6163 0.5022 0.8397 0.035 Uiso 1 1 calc R U . N24 N 0.1778(3) -0.1472(3) 0.9330(2) 0.0339(9) Uani 1 1 d . . . C24 C 0.7848(4) 0.3294(3) 0.6902(3) 0.0342(10) Uani 1 1 d . . . H24A H 0.8190 0.2933 0.6541 0.041 Uiso 1 1 calc R U . H24B H 0.8184 0.3201 0.7433 0.041 Uiso 1 1 calc R U . N25 N 0.1219(3) 0.0009(3) 0.9661(2) 0.0342(9) Uani 1 1 d . . . C25 C 0.4758(4) 0.4090(3) 0.7484(3) 0.0272(9) Uani 1 1 d . . . N26 N 0.1707(3) 0.1359(3) 1.0215(2) 0.0309(8) Uani 1 1 d . . . C26 C 0.6084(4) 0.3079(3) 0.7464(3) 0.0261(8) Uani 1 1 d . . . H26 H 0.6373 0.2787 0.7946 0.031 Uiso 1 1 calc R U . C29 C 0.3161(4) 0.3163(3) 0.6932(3) 0.0306(9) Uani 1 1 d . . . H29A H 0.2843 0.3626 0.7215 0.037 Uiso 1 1 calc R U . H29B H 0.2971 0.2583 0.7147 0.037 Uiso 1 1 calc R U . C28 C 0.6259(4) 0.2450(3) 0.6221(3) 0.0297(9) Uani 1 1 d . . . C27 C 0.5013(4) 0.2603(3) 0.7106(3) 0.0276(9) Uani 1 1 d . . . H27 H 0.4788 0.2119 0.7442 0.033 Uiso 1 1 calc R U . C30 C 0.4494(4) 0.1694(3) 0.5807(3) 0.0355(10) Uani 1 1 d . . . H30A H 0.4111 0.1257 0.6098 0.043 Uiso 1 1 calc R U . H30B H 0.4881 0.1360 0.5456 0.043 Uiso 1 1 calc R U . C31 C 0.2138(3) 0.3821(3) 0.5791(3) 0.0261(8) Uani 1 1 d . . . C32 C 0.2731(4) 0.2376(3) 0.5576(3) 0.0277(9) Uani 1 1 d . . . H32 H 0.2401 0.1829 0.5781 0.033 Uiso 1 1 calc R U . C33 C 0.2076(3) 0.2683(3) 0.4809(3) 0.0262(8) Uani 1 1 d . . . H33 H 0.1442 0.2278 0.4658 0.031 Uiso 1 1 calc R U . C34 C 0.1022(3) 0.4067(4) 0.4539(3) 0.0310(9) Uani 1 1 d . . . H34A H 0.0722 0.4484 0.4881 0.037 Uiso 1 1 calc R U . H34B H 0.0458 0.3634 0.4311 0.037 Uiso 1 1 calc R U . C35 C 0.2513(4) 0.2720(3) 0.3398(3) 0.0288(9) Uani 1 1 d . . . H35A H 0.3007 0.2413 0.3115 0.035 Uiso 1 1 calc R U . H35B H 0.1817 0.2419 0.3249 0.035 Uiso 1 1 calc R U . C36 C 0.6489(4) 0.3284(3) 1.0326(3) 0.0339(10) Uani 1 1 d . . . H36A H 0.6712 0.3811 1.0668 0.041 Uiso 1 1 calc R U . H36B H 0.6689 0.3414 0.9809 0.041 Uiso 1 1 calc R U . C37 C 0.4742(4) 0.2931(3) 0.9554(3) 0.0300(9) Uani 1 1 d . . . C38 C 0.4743(4) 0.3187(3) 1.0912(2) 0.0258(8) Uani 1 1 d . . . H38 H 0.4884 0.3767 1.1208 0.031 Uiso 1 1 calc R U . C39 C 0.2841(4) 0.2742(3) 0.9064(3) 0.0344(10) Uani 1 1 d . . . H39A H 0.2318 0.3166 0.9157 0.041 Uiso 1 1 calc R U . H39B H 0.3102 0.2894 0.8571 0.041 Uiso 1 1 calc R U . C40 C 0.2509(4) 0.1239(3) 0.8404(3) 0.0289(9) Uani 1 1 d . . . C41 C 0.1449(4) 0.1555(3) 0.9391(3) 0.0298(9) Uani 1 1 d . . . H41 H 0.0884 0.1974 0.9312 0.036 Uiso 1 1 calc R U . C42 C 0.1093(3) 0.0609(3) 0.9001(3) 0.0312(9) Uani 1 1 d . . . H42 H 0.0358 0.0586 0.8750 0.037 Uiso 1 1 calc R U . C43 C 0.2015(4) 0.2050(3) 1.0837(3) 0.0309(9) Uani 1 1 d . . . H43A H 0.1602 0.2570 1.0723 0.037 Uiso 1 1 calc R U . H43B H 0.1843 0.1812 1.1333 0.037 Uiso 1 1 calc R U . C44 C 0.1520(3) 0.0465(3) 1.0367(3) 0.0301(9) Uani 1 1 d . . . C45 C 0.0960(4) -0.0961(4) 0.9600(3) 0.0369(11) Uani 1 1 d . . . H45A H 0.0825 -0.1172 1.0114 0.044 Uiso 1 1 calc R U . H45B H 0.0315 -0.1080 0.9238 0.044 Uiso 1 1 calc R U . C46 C 0.1667(4) -0.0204(3) 0.7817(3) 0.0324(10) Uani 1 1 d . . . H46A H 0.1930 0.0034 0.7349 0.039 Uiso 1 1 calc R U . H46B H 0.0916 -0.0361 0.7683 0.039 Uiso 1 1 calc R U . C47 C 0.2367(4) -0.2024(3) 0.9820(3) 0.0320(9) Uani 1 1 d . . . C48 C 0.1782(3) -0.1720(3) 0.8500(3) 0.0285(9) Uani 1 1 d . . . H48 H 0.1088 -0.1979 0.8259 0.034 Uiso 1 1 calc R U . C49 C 0.2624(3) -0.2428(3) 0.8530(3) 0.0279(9) Uani 1 1 d . . . H49 H 0.2329 -0.3007 0.8277 0.033 Uiso 1 1 calc R U . C50 C 0.3143(3) -0.1197(3) 0.7799(3) 0.0272(9) Uani 1 1 d . . . C51 C 0.4343(4) -0.2442(3) 0.7912(3) 0.0284(9) Uani 1 1 d . . . H51A H 0.4612 -0.2140 0.7472 0.034 Uiso 1 1 calc R U . H51B H 0.4134 -0.3065 0.7745 0.034 Uiso 1 1 calc R U . C52 C 0.6168(3) -0.2033(3) 0.8485(2) 0.0232(8) Uani 1 1 d . . . C53 C 0.6421(4) -0.3071(3) 0.9497(3) 0.0266(8) Uani 1 1 d . . . H53 H 0.6786 -0.3629 0.9453 0.032 Uiso 1 1 calc R U . Br1 Br 0.0330(2) 0.6164(2) 0.88019(19) 0.2542(18) Uani 1 1 d . 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 0.02586(13) 0.03009(13) 0.02494(13) 0.00225(8) 0.01180(8) 0.00101(8) N1 0.0317(19) 0.0291(18) 0.0199(17) -0.0048(14) 0.0019(14) 0.0082(15) C1 0.021(2) 0.050(3) 0.030(2) -0.001(2) -0.0029(17) 0.0091(19) O1 0.035(2) 0.055(2) 0.070(3) -0.018(2) 0.0198(19) -0.0117(18) N2 0.038(2) 0.0292(18) 0.0212(17) 0.0104(14) 0.0195(15) 0.0103(15) C2 0.0229(19) 0.036(2) 0.0170(18) -0.0021(16) -0.0024(15) 0.0019(16) O2 0.064(3) 0.070(3) 0.038(2) 0.023(2) 0.0164(19) 0.037(2) O3 0.0241(18) 0.064(3) 0.085(3) 0.009(2) 0.0198(19) 0.0073(17) N3 0.0303(19) 0.037(2) 0.0249(18) 0.0008(15) 0.0066(15) 0.0058(16) C3 0.0219(19) 0.034(2) 0.032(2) -0.0017(18) 0.0029(16) -0.0069(16) O4 0.0357(19) 0.048(2) 0.044(2) -0.0019(16) 0.0245(16) 0.0052(16) N4 0.034(2) 0.034(2) 0.029(2) 0.0024(16) 0.0097(16) 0.0054(16) C4 0.040(2) 0.025(2) 0.030(2) -0.0028(17) 0.0051(19) -0.0040(18) O5 0.059(3) 0.099(4) 0.040(2) -0.031(2) 0.022(2) -0.019(3) N5 0.035(2) 0.037(2) 0.0271(19) 0.0017(16) 0.0086(16) 0.0020(16) C5 0.032(2) 0.039(2) 0.023(2) 0.0064(18) 0.0088(17) 0.0071(18) O6 0.053(2) 0.0417(19) 0.0286(17) 0.0020(15) 0.0104(16) 0.0135(17) N6 0.038(2) 0.0289(19) 0.030(2) -0.0029(15) 0.0045(16) 0.0034(16) C6 0.033(2) 0.036(2) 0.024(2) 0.0098(17) 0.0055(17) 0.0054(18) N7 0.039(2) 0.0256(18) 0.031(2) -0.0003(15) 0.0052(16) 0.0037(15) C7 0.039(3) 0.040(3) 0.025(2) -0.0010(18) 0.0003(19) 0.018(2) C55 0.035(2) 0.0165(18) 0.032(2) -0.0025(16) 0.0033(18) -0.0048(16) O8 0.0377(19) 0.0369(18) 0.0400(19) -0.0028(15) 0.0101(15) 0.0077(14) N8 0.0317(19) 0.0316(19) 0.0269(19) 0.0040(15) 0.0072(15) -0.0002(15) C8 0.034(2) 0.034(2) 0.027(2) -0.0023(18) 0.0032(18) 0.0110(18) O9 0.0308(16) 0.0287(15) 0.0323(17) -0.0019(13) 0.0121(13) 0.0035(12) N9 0.0283(18) 0.0298(18) 0.0243(18) -0.0003(14) 0.0000(14) 0.0014(14) C9 0.038(2) 0.036(2) 0.028(2) -0.0032(19) 0.0019(18) 0.0143(19) O00D 0.048(2) 0.043(2) 0.0359(19) -0.0034(16) 0.0127(16) 0.0105(16) O10 0.0383(18) 0.0320(17) 0.0371(19) 0.0014(14) 0.0067(14) 0.0060(14) N10 0.0314(19) 0.0314(19) 0.0221(18) 0.0012(14) 0.0030(14) 0.0031(15) C10 0.042(3) 0.032(2) 0.030(2) -0.0035(18) 0.020(2) -0.0005(19) O11 0.045(2) 0.0339(18) 0.0317(18) -0.0052(14) 0.0025(15) 0.0061(15) N11 0.0315(19) 0.0314(19) 0.0228(17) 0.0010(14) 0.0026(14) 0.0059(15) C11 0.032(2) 0.0230(19) 0.025(2) 0.0067(15) 0.0153(17) 0.0078(16) O12 0.0343(16) 0.0298(15) 0.0241(15) 0.0029(12) 0.0099(12) 0.0039(13) N12 0.0324(19) 0.0245(17) 0.0295(19) 0.0028(14) 0.0072(15) 0.0013(14) C12 0.037(2) 0.031(2) 0.028(2) 0.0000(17) 0.0156(18) -0.0024(18) O13 0.0287(17) 0.0428(19) 0.0412(19) 0.0050(15) 0.0114(14) -0.0043(14) N13 0.0268(18) 0.0306(18) 0.0270(18) 0.0051(15) 0.0094(14) 0.0016(14) C13 0.034(2) 0.035(2) 0.036(3) 0.0061(19) 0.021(2) -0.0005(18) O14 0.053(2) 0.0348(18) 0.0313(18) 0.0066(14) 0.0181(16) -0.0006(15) N14 0.0238(17) 0.0300(18) 0.0293(19) 0.0028(15) 0.0077(14) 0.0015(14) C14 0.036(2) 0.041(3) 0.021(2) 0.0034(18) 0.0082(18) 0.0065(19) O15 0.057(2) 0.044(2) 0.0229(16) 0.0048(14) 0.0190(15) 0.0084(17) N15 0.031(2) 0.043(2) 0.0219(18) 0.0046(16) 0.0114(15) 0.0065(16) C15 0.027(2) 0.042(3) 0.032(2) 0.0061(19) 0.0133(18) 0.0070(18) O16 0.054(2) 0.058(2) 0.0306(19) 0.0003(17) 0.0196(17) 0.0088(19) N16 0.039(2) 0.037(2) 0.0173(17) 0.0020(14) 0.0059(15) 0.0044(16) C16 0.057(3) 0.032(2) 0.032(2) 0.0113(19) 0.033(2) 0.017(2) O17 0.0376(18) 0.047(2) 0.0319(18) 0.0082(15) 0.0104(14) 0.0046(15) N17 0.045(2) 0.032(2) 0.027(2) 0.0014(16) 0.0102(17) 0.0017(17) C17 0.037(2) 0.031(2) 0.0204(19) 0.0077(16) 0.0176(17) 0.0126(18) N18 0.0287(19) 0.037(2) 0.0292(19) -0.0018(16) 0.0094(15) 0.0000(15) C18 0.044(3) 0.031(2) 0.024(2) 0.0079(18) 0.0215(19) 0.0132(19) N19 0.0230(17) 0.034(2) 0.036(2) -0.0002(16) 0.0090(15) -0.0008(15) C19 0.0244(19) 0.0246(19) 0.0191(18) -0.0055(15) 0.0021(15) -0.0050(15) N22 0.0277(18) 0.036(2) 0.0225(18) 0.0034(15) 0.0052(14) 0.0026(15) C22 0.0211(19) 0.038(2) 0.028(2) 0.0033(18) 0.0033(16) 0.0085(17) N21 0.0249(17) 0.0301(18) 0.0179(16) -0.0028(13) 0.0067(13) 0.0037(14) C21 0.0215(19) 0.037(2) 0.026(2) 0.0046(17) 0.0011(16) 0.0042(16) N20 0.0235(18) 0.041(2) 0.0278(19) 0.0017(16) 0.0104(15) 0.0015(15) C20 0.0182(18) 0.039(2) 0.024(2) 0.0010(17) 0.0014(15) -0.0013(16) N23 0.0289(19) 0.040(2) 0.0262(19) 0.0015(16) 0.0107(15) 0.0042(16) C23 0.035(2) 0.036(2) 0.0179(19) 0.0008(16) 0.0063(17) -0.0012(18) N24 0.0281(19) 0.044(2) 0.032(2) -0.0021(17) 0.0129(16) 0.0056(17) C24 0.032(2) 0.034(2) 0.039(3) 0.0071(19) 0.0062(19) 0.0115(19) N25 0.036(2) 0.037(2) 0.031(2) -0.0009(16) 0.0102(16) 0.0013(17) C25 0.033(2) 0.029(2) 0.0205(19) 0.0073(16) 0.0062(16) 0.0025(17) N26 0.0289(19) 0.038(2) 0.0260(19) 0.0002(16) 0.0044(15) 0.0008(15) C26 0.032(2) 0.026(2) 0.0214(19) 0.0070(15) 0.0042(16) 0.0039(16) C29 0.033(2) 0.039(2) 0.022(2) 0.0084(17) 0.0098(17) 0.0040(18) C28 0.042(2) 0.025(2) 0.022(2) 0.0082(16) 0.0021(18) 0.0100(18) C27 0.036(2) 0.0228(19) 0.024(2) 0.0098(16) 0.0050(17) 0.0031(17) C30 0.049(3) 0.0178(19) 0.039(3) -0.0013(17) -0.001(2) 0.0056(18) C31 0.0241(19) 0.028(2) 0.026(2) 0.0011(16) 0.0043(16) -0.0064(16) C32 0.036(2) 0.0206(19) 0.026(2) 0.0026(16) 0.0055(17) -0.0042(16) C33 0.026(2) 0.025(2) 0.025(2) -0.0005(16) 0.0038(16) -0.0087(16) C34 0.0211(19) 0.046(3) 0.027(2) 0.0058(19) 0.0060(16) 0.0024(18) C35 0.034(2) 0.025(2) 0.027(2) -0.0026(16) 0.0063(17) -0.0048(17) C36 0.036(2) 0.035(2) 0.034(2) 0.0064(19) 0.0168(19) 0.0016(19) C37 0.044(3) 0.024(2) 0.024(2) 0.0030(16) 0.0116(18) 0.0077(18) C38 0.031(2) 0.027(2) 0.0214(19) -0.0034(15) 0.0100(16) 0.0040(16) C39 0.048(3) 0.031(2) 0.024(2) 0.0076(17) 0.0023(19) 0.005(2) C40 0.035(2) 0.030(2) 0.023(2) 0.0078(16) 0.0038(17) 0.0064(17) C41 0.026(2) 0.038(2) 0.026(2) 0.0024(18) 0.0021(17) 0.0084(17) C42 0.0201(19) 0.043(3) 0.031(2) -0.0025(19) 0.0038(17) 0.0052(17) C43 0.025(2) 0.044(3) 0.025(2) -0.0022(18) 0.0094(17) 0.0081(18) C44 0.0181(18) 0.043(3) 0.031(2) 0.0035(19) 0.0080(16) 0.0075(17) C45 0.027(2) 0.041(3) 0.046(3) -0.001(2) 0.021(2) -0.0008(19) C46 0.028(2) 0.042(3) 0.026(2) -0.0044(19) -0.0017(17) 0.0024(18) C47 0.028(2) 0.037(2) 0.033(2) -0.0021(19) 0.0136(18) -0.0022(18) C48 0.0189(18) 0.035(2) 0.031(2) -0.0043(18) 0.0058(16) -0.0031(16) C49 0.026(2) 0.031(2) 0.027(2) -0.0035(17) 0.0079(16) -0.0028(16) C50 0.0227(19) 0.035(2) 0.023(2) -0.0047(17) 0.0024(16) -0.0037(16) C51 0.030(2) 0.038(2) 0.0183(19) -0.0025(16) 0.0082(16) 0.0055(18) C52 0.028(2) 0.0247(19) 0.0183(18) -0.0053(15) 0.0073(15) 0.0050(15) C53 0.032(2) 0.028(2) 0.021(2) -0.0012(16) 0.0064(16) 0.0069(17) Br1 0.212(3) 0.260(3) 0.254(3) 0.109(2) -0.061(2) -0.125(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' Br Br -0.2901 2.4595 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 U1 O1 180.0 . 2_756 O1 U1 O2 89.2(2) . . O1 U1 O2 90.8(2) 2_756 . O1 U1 O2 90.8(2) . 2_756 O1 U1 O2 89.2(2) 2_756 2_756 O2 U1 O2 180.00(14) . 2_756 O1 U1 O4 93.45(17) . 2_756 O1 U1 O4 86.55(17) 2_756 2_756 O2 U1 O4 87.76(15) . 2_756 O2 U1 O4 92.24(15) 2_756 2_756 O1 U1 O4 86.55(17) . . O1 U1 O4 93.45(17) 2_756 . O2 U1 O4 92.24(15) . . O2 U1 O4 87.76(15) 2_756 . O4 U1 O4 180.0 2_756 . C5 N1 C4 122.1(4) . . C5 N1 C7 118.5(4) . . C4 N1 C7 119.4(4) . . O3 C1 O2 125.8(5) . . O3 C1 C2 119.3(5) . . O2 C1 C2 114.6(4) . . C13 N2 C14 120.4(4) . . C13 N2 C16 119.1(4) . . C14 N2 C16 120.5(4) . . C3 C2 C6 119.2(4) . . C3 C2 C1 120.0(4) . . C6 C2 C1 120.8(4) . . C1 O2 U1 142.8(4) . . C22 N3 C34 122.3(4) . 2_666 C22 N3 C20 112.2(4) . . C34 N3 C20 125.3(4) 2_666 . C4 C3 C2 120.2(4) . . C4 C3 H3 119.9 . . C2 C3 H3 119.9 . . C10 O4 U1 132.3(3) . . C22 N4 C24 121.8(4) . . C22 N4 C21 111.9(4) . . C24 N4 C21 123.6(4) . . N1 C4 C3 119.4(4) . . N1 C4 H4 120.3 . . C3 C4 H4 120.3 . . C28 N5 C24 122.1(4) . . C28 N5 C26 112.5(4) . . C24 N5 C26 124.9(4) . . N1 C5 C6 120.2(4) . . N1 C5 H5 119.9 . . C6 C5 H5 119.9 . . C28 N6 C30 122.2(4) . . C28 N6 C27 112.9(4) . . C30 N6 C27 124.8(4) . . C5 C6 C2 118.9(4) . . C5 C6 H6 120.5 . . C2 C6 H6 120.5 . . C55 N7 C32 112.5(4) . . C55 N7 C30 121.6(4) . . C32 N7 C30 121.8(4) . . N1 C7 C8 111.9(4) . . N1 C7 H7A 109.2 . . C8 C7 H7A 109.2 . . N1 C7 H7B 109.2 . . C8 C7 H7B 109.2 . . H7A C7 H7B 107.9 . . O8 C55 N7 126.3(5) . . O8 C55 N8 126.6(4) . . N7 C55 N8 107.1(4) . . C55 N8 C33 113.4(4) . . C55 N8 C35 122.1(4) . . C33 N8 C35 123.2(4) . . C7 C8 C9 109.8(4) . . C7 C8 H8A 109.7 . . C9 C8 H8A 109.7 . . C7 C8 H8B 109.7 . . C9 C8 H8B 109.7 . . H8A C8 H8B 108.2 . . C31 N9 C34 122.0(4) . . C31 N9 C33 112.1(4) . . C34 N9 C33 123.3(4) . . C9 C9 C8 112.2(5) 2_666 . C9 C9 H9A 109.2 2_666 . C8 C9 H9A 109.2 . . C9 C9 H9B 109.2 2_666 . C8 C9 H9B 109.2 . . H9A C9 H9B 107.9 . . C31 N10 C29 123.1(4) . . C31 N10 C32 113.2(4) . . C29 N10 C32 122.9(4) . . O5 C10 O4 126.2(5) . . O5 C10 C11 119.8(5) . . O4 C10 C11 113.9(4) . . C25 N11 C29 121.1(4) . . C25 N11 C27 110.8(4) . . C29 N11 C27 122.9(4) . . C12 C11 C15 118.5(4) . . C12 C11 C10 118.0(4) . . C15 C11 C10 123.5(4) . . C25 N12 C26 112.6(4) . . C25 N12 C23 123.2(4) . . C26 N12 C23 122.6(4) . . C13 C12 C11 119.3(5) . . C13 C12 H12 120.3 . . C11 C12 H12 120.3 . . C19 N13 C23 121.5(4) . . C19 N13 C21 112.8(4) . . C23 N13 C21 125.4(4) . . N2 C13 C12 121.8(4) . . N2 C13 H13 119.1 . . C12 C13 H13 119.1 . . C19 N14 C35 120.7(4) . 2_666 C19 N14 C20 111.7(4) . . C35 N14 C20 123.8(4) 2_666 . N2 C14 C15 119.9(5) . . N2 C14 H14 120.0 . . C15 C14 H14 120.0 . . C37 N15 C36 122.7(4) . . C37 N15 C38 112.5(4) . . C36 N15 C38 124.7(4) . . C11 C15 C14 119.9(4) . . C11 C15 H15 120.0 . . C14 C15 H15 120.0 . . C37 N16 C39 122.2(4) . . C37 N16 C53 112.8(4) . 2_657 C39 N16 C53 123.8(4) . 2_657 N2 C16 C17 114.0(4) . . N2 C16 H16A 108.7 . . C17 C16 H16A 108.7 . . N2 C16 H16B 108.7 . . C17 C16 H16B 108.7 . . H16A C16 H16B 107.6 . . C40 N17 C39 122.4(4) . . C40 N17 C41 112.8(4) . . C39 N17 C41 123.4(4) . . C16 C17 C18 110.3(3) . . C16 C17 H17A 109.6 . . C18 C17 H17A 109.6 . . C16 C17 H17B 109.6 . . C18 C17 H17B 109.6 . . H17A C17 H17B 108.1 . . C40 N18 C46 122.1(4) . . C40 N18 C42 112.4(4) . . C46 N18 C42 123.8(4) . . C18 C18 C17 112.0(4) 2_657 . C18 C18 H18A 109.2 2_657 . C17 C18 H18A 109.2 . . C18 C18 H18B 109.2 2_657 . C17 C18 H18B 109.2 . . H18A C18 H18B 107.9 . . C50 N19 C48 112.4(4) . . C50 N19 C46 122.7(4) . . C48 N19 C46 124.9(4) . . O9 C19 N13 125.5(4) . . O9 C19 N14 126.3(4) . . N13 C19 N14 108.2(4) . . C52 N22 C43 122.0(4) . 2_657 C52 N22 C53 112.4(4) . . C43 N22 C53 125.1(4) 2_657 . O00D C22 N4 126.1(5) . . O00D C22 N3 125.9(4) . . N4 C22 N3 108.0(4) . . C52 N21 C38 111.3(3) . 2_657 C52 N21 C51 119.5(4) . . C38 N21 C51 120.3(4) 2_657 . N13 C21 N4 115.7(4) . . N13 C21 C20 102.9(4) . . N4 C21 C20 103.2(4) . . N13 C21 H21 111.5 . . N4 C21 H21 111.5 . . C20 C21 H21 111.5 . . C50 N20 C51 123.0(4) . . C50 N20 C49 112.6(4) . . C51 N20 C49 123.8(4) . . N3 C20 N14 115.1(4) . . N3 C20 C21 103.5(4) . . N14 C20 C21 103.5(3) . . N3 C20 H20 111.4 . . N14 C20 H20 111.4 . . C21 C20 H20 111.4 . . C47 N23 C49 112.1(4) . . C47 N23 C36 122.0(4) . 2_657 C49 N23 C36 122.2(4) . 2_657 N12 C23 N13 113.7(4) . . N12 C23 H23A 108.8 . . N13 C23 H23A 108.8 . . N12 C23 H23B 108.8 . . N13 C23 H23B 108.8 . . H23A C23 H23B 107.7 . . C47 N24 C45 122.0(4) . . C47 N24 C48 112.0(4) . . C45 N24 C48 122.2(4) . . N5 C24 N4 113.6(4) . . N5 C24 H24A 108.9 . . N4 C24 H24A 108.9 . . N5 C24 H24B 108.9 . . N4 C24 H24B 108.9 . . H24A C24 H24B 107.7 . . C44 N25 C45 122.8(4) . . C44 N25 C42 112.7(4) . . C45 N25 C42 124.2(4) . . O10 C25 N12 126.0(4) . . O10 C25 N11 126.2(4) . . N12 C25 N11 107.8(4) . . C44 N26 C41 113.0(4) . . C44 N26 C43 122.7(4) . . C41 N26 C43 123.9(4) . . N12 C26 N5 115.9(4) . . N12 C26 C27 103.3(4) . . N5 C26 C27 103.5(4) . . N12 C26 H26 111.2 . . N5 C26 H26 111.2 . . C27 C26 H26 111.2 . . N11 C29 N10 113.6(4) . . N11 C29 H29A 108.8 . . N10 C29 H29A 108.8 . . N11 C29 H29B 108.8 . . N10 C29 H29B 108.8 . . H29A C29 H29B 107.7 . . O6 C28 N5 126.1(5) . . O6 C28 N6 126.0(5) . . N5 C28 N6 107.8(4) . . N6 C27 N11 116.0(4) . . N6 C27 C26 103.1(4) . . N11 C27 C26 103.6(3) . . N6 C27 H27 111.2 . . N11 C27 H27 111.2 . . C26 C27 H27 111.2 . . N6 C30 N7 113.1(4) . . N6 C30 H30A 109.0 . . N7 C30 H30A 109.0 . . N6 C30 H30B 109.0 . . N7 C30 H30B 109.0 . . H30A C30 H30B 107.8 . . O11 C31 N10 126.1(4) . . O11 C31 N9 125.7(4) . . N10 C31 N9 108.1(4) . . N7 C32 N10 114.6(4) . . N7 C32 C33 104.0(4) . . N10 C32 C33 102.3(3) . . N7 C32 H32 111.8 . . N10 C32 H32 111.8 . . C33 C32 H32 111.8 . . N8 C33 N9 115.4(4) . . N8 C33 C32 102.5(4) . . N9 C33 C32 103.8(3) . . N8 C33 H33 111.5 . . N9 C33 H33 111.5 . . C32 C33 H33 111.5 . . N9 C34 N3 114.1(4) . 2_666 N9 C34 H34A 108.7 . . N3 C34 H34A 108.7 2_666 . N9 C34 H34B 108.7 . . N3 C34 H34B 108.7 2_666 . H34A C34 H34B 107.6 . . N14 C35 N8 113.2(4) 2_666 . N14 C35 H35A 108.9 2_666 . N8 C35 H35A 108.9 . . N14 C35 H35B 108.9 2_666 . N8 C35 H35B 108.9 . . H35A C35 H35B 107.8 . . N15 C36 N23 114.7(4) . 2_657 N15 C36 H36A 108.6 . . N23 C36 H36A 108.6 2_657 . N15 C36 H36B 108.6 . . N23 C36 H36B 108.6 2_657 . H36A C36 H36B 107.6 . . O15 C37 N15 125.7(5) . . O15 C37 N16 126.3(5) . . N15 C37 N16 107.9(4) . . N21 C38 N15 115.4(4) 2_657 . N21 C38 C53 103.3(3) 2_657 2_657 N15 C38 C53 103.3(3) . 2_657 N21 C38 H38 111.4 2_657 . N15 C38 H38 111.4 . . C53 C38 H38 111.4 2_657 . N17 C39 N16 113.6(4) . . N17 C39 H39A 108.8 . . N16 C39 H39A 108.8 . . N17 C39 H39B 108.8 . . N16 C39 H39B 108.8 . . H39A C39 H39B 107.7 . . O14 C40 N17 126.2(5) . . O14 C40 N18 125.9(5) . . N17 C40 N18 107.9(4) . . N26 C41 N17 115.4(4) . . N26 C41 C42 103.3(4) . . N17 C41 C42 102.8(4) . . N26 C41 H41 111.6 . . N17 C41 H41 111.6 . . C42 C41 H41 111.6 . . N18 C42 N25 114.9(4) . . N18 C42 C41 103.9(4) . . N25 C42 C41 103.0(4) . . N18 C42 H42 111.5 . . N25 C42 H42 111.5 . . C41 C42 H42 111.5 . . N22 C43 N26 114.0(4) 2_657 . N22 C43 H43A 108.7 2_657 . N26 C43 H43A 108.7 . . N22 C43 H43B 108.7 2_657 . N26 C43 H43B 108.7 . . H43A C43 H43B 107.6 . . O17 C44 N26 126.6(5) . . O17 C44 N25 125.5(5) . . N26 C44 N25 107.8(4) . . N24 C45 N25 113.9(4) . . N24 C45 H45A 108.8 . . N25 C45 H45A 108.8 . . N24 C45 H45B 108.8 . . N25 C45 H45B 108.8 . . H45A C45 H45B 107.7 . . N18 C46 N19 114.0(4) . . N18 C46 H46A 108.7 . . N19 C46 H46A 108.7 . . N18 C46 H46B 108.7 . . N19 C46 H46B 108.7 . . H46A C46 H46B 107.6 . . O16 C47 N23 126.1(5) . . O16 C47 N24 126.0(5) . . N23 C47 N24 108.0(4) . . N19 C48 N24 115.1(4) . . N19 C48 C49 103.6(3) . . N24 C48 C49 102.9(4) . . N19 C48 H48 111.5 . . N24 C48 H48 111.5 . . C49 C48 H48 111.5 . . N23 C49 N20 115.1(4) . . N23 C49 C48 103.8(4) . . N20 C49 C48 103.0(4) . . N23 C49 H49 111.5 . . N20 C49 H49 111.5 . . C48 C49 H49 111.5 . . O13 C50 N20 126.2(4) . . O13 C50 N19 125.5(5) . . N20 C50 N19 108.3(4) . . N20 C51 N21 113.3(4) . . N20 C51 H51A 108.9 . . N21 C51 H51A 108.9 . . N20 C51 H51B 108.9 . . N21 C51 H51B 108.9 . . H51A C51 H51B 107.7 . . O12 C52 N22 125.7(4) . . O12 C52 N21 126.5(4) . . N22 C52 N21 107.8(4) . . N22 C53 N16 115.5(4) . 2_657 N22 C53 C38 103.2(3) . 2_657 N16 C53 C38 102.7(3) 2_657 2_657 N22 C53 H53 111.6 . . N16 C53 H53 111.6 2_657 . C38 C53 H53 111.6 2_657 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 O1 1.758(4) . U1 O1 1.758(4) 2_756 U1 O2 2.269(4) . U1 O2 2.269(4) 2_756 U1 O4 2.301(3) 2_756 U1 O4 2.301(3) . N1 C5 1.336(6) . N1 C4 1.346(6) . N1 C7 1.485(6) . C1 O3 1.204(7) . C1 O2 1.292(7) . C1 C2 1.511(6) . N2 C13 1.323(7) . N2 C14 1.350(6) . N2 C16 1.496(5) . C2 C3 1.376(7) . C2 C6 1.392(6) . N3 C22 1.372(6) . N3 C34 1.442(6) 2_666 N3 C20 1.445(6) . C3 C4 1.375(7) . C3 H3 0.9300 . O4 C10 1.292(6) . N4 C22 1.370(6) . N4 C24 1.449(6) . N4 C21 1.450(6) . C4 H4 0.9300 . O5 C10 1.212(7) . N5 C28 1.366(6) . N5 C24 1.443(6) . N5 C26 1.449(6) . C5 C6 1.380(7) . C5 H5 0.9300 . O6 C28 1.220(6) . N6 C28 1.372(7) . N6 C30 1.442(6) . N6 C27 1.445(6) . C6 H6 0.9300 . N7 C55 1.375(6) . N7 C32 1.438(6) . N7 C30 1.444(6) . C7 C8 1.513(6) . C7 H7A 0.9700 . C7 H7B 0.9700 . C55 O8 1.207(6) . C55 N8 1.377(6) . N8 C33 1.440(6) . N8 C35 1.450(6) . C8 C9 1.516(6) . C8 H8A 0.9700 . C8 H8B 0.9700 . O9 C19 1.214(5) . N9 C31 1.373(6) . N9 C34 1.442(6) . N9 C33 1.447(6) . C9 C9 1.512(9) 2_666 C9 H9A 0.9700 . C9 H9B 0.9700 . O00D C22 1.222(6) . O10 C25 1.218(6) . N10 C31 1.356(6) . N10 C29 1.443(6) . N10 C32 1.457(6) . C10 C11 1.522(6) . O11 C31 1.220(6) . N11 C25 1.380(6) . N11 C29 1.440(6) . N11 C27 1.455(6) . C11 C12 1.379(6) . C11 C15 1.381(7) . O12 C52 1.209(5) . N12 C25 1.370(6) . N12 C26 1.436(6) . N12 C23 1.443(6) . C12 C13 1.371(6) . C12 H12 0.9300 . O13 C50 1.213(6) . N13 C19 1.367(6) . N13 C23 1.443(6) . N13 C21 1.450(6) . C13 H13 0.9300 . O14 C40 1.210(6) . N14 C19 1.368(5) . N14 C35 1.448(6) 2_666 N14 C20 1.459(6) . C14 C15 1.382(6) . C14 H14 0.9300 . O15 C37 1.217(6) . N15 C37 1.368(6) . N15 C36 1.438(6) . N15 C38 1.448(5) . C15 H15 0.9300 . O16 C47 1.216(6) . N16 C37 1.376(6) . N16 C39 1.438(6) . N16 C53 1.445(5) 2_657 C16 C17 1.509(6) . C16 H16A 0.9700 . C16 H16B 0.9700 . O17 C44 1.217(6) . N17 C40 1.370(6) . N17 C39 1.435(6) . N17 C41 1.451(6) . C17 C18 1.531(5) . C17 H17A 0.9700 . C17 H17B 0.9700 . N18 C40 1.374(6) . N18 C46 1.439(6) . N18 C42 1.441(6) . C18 C18 1.525(8) 2_657 C18 H18A 0.9700 . C18 H18B 0.9700 . N19 C50 1.370(6) . N19 C48 1.439(6) . N19 C46 1.441(6) . N22 C52 1.377(6) . N22 C43 1.439(6) 2_657 N22 C53 1.443(6) . N21 C52 1.384(6) . N21 C38 1.445(6) 2_657 N21 C51 1.447(6) . C21 C20 1.541(6) . C21 H21 0.9800 . N20 C50 1.359(6) . N20 C51 1.447(6) . N20 C49 1.451(5) . C20 H20 0.9800 . N23 C47 1.371(6) . N23 C49 1.448(6) . N23 C36 1.452(6) 2_657 C23 H23A 0.9700 . C23 H23B 0.9700 . N24 C47 1.372(7) . N24 C45 1.445(6) . N24 C48 1.458(6) . C24 H24A 0.9700 . C24 H24B 0.9700 . N25 C44 1.368(7) . N25 C45 1.449(7) . N25 C42 1.450(6) . N26 C44 1.365(6) . N26 C41 1.443(6) . N26 C43 1.457(6) . C26 C27 1.545(6) . C26 H26 0.9800 . C29 H29A 0.9700 . C29 H29B 0.9700 . C27 H27 0.9800 . C30 H30A 0.9700 . C30 H30B 0.9700 . C32 C33 1.556(6) . C32 H32 0.9800 . C33 H33 0.9800 . C34 N3 1.442(6) 2_666 C34 H34A 0.9700 . C34 H34B 0.9700 . C35 N14 1.448(6) 2_666 C35 H35A 0.9700 . C35 H35B 0.9700 . C36 N23 1.452(6) 2_657 C36 H36A 0.9700 . C36 H36B 0.9700 . C38 N21 1.445(6) 2_657 C38 C53 1.558(6) 2_657 C38 H38 0.9800 . C39 H39A 0.9700 . C39 H39B 0.9700 . C41 C42 1.551(7) . C41 H41 0.9800 . C42 H42 0.9800 . C43 N22 1.439(6) 2_657 C43 H43A 0.9700 . C43 H43B 0.9700 . C45 H45A 0.9700 . C45 H45B 0.9700 . C46 H46A 0.9700 . C46 H46B 0.9700 . C48 C49 1.547(6) . C48 H48 0.9800 . C49 H49 0.9800 . C51 H51A 0.9700 . C51 H51B 0.9700 . C53 N16 1.445(5) 2_657 C53 C38 1.558(6) 2_657 C53 H53 0.9800 .