#------------------------------------------------------------------------------ #$Date: 2026-06-05 00:35:36 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306222 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721100.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_7721100 loop_ _publ_author_name 'Gutorova, Svetlana' 'Matveev, Petr I.' 'Evsiunina, Mariia V.' 'Wang, Qiushi' 'Lemport, Pavel S.' 'Kalle, Paulina' 'Koshelev, Daniil S.' 'Utochnikova, Valentina V.' 'Averin, Alexey A.' 'Poliakova, Tatiana R.' 'Gerasimov, Mikhail A.' 'Petrov, Vladimir G.' 'Ustynyuk, Yuri' 'Kalmykov, Stepan' 'Nenajdenko, Valentine' _publ_section_title ; Competitive Coordination of Uranium(VI) and Thorium(IV) by Tetradentate Phenanthroline Ligands: Structural and Spectroscopic Investigation of U(VI)-Th(IV) Mixed Ion Pair Formation ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00392C _journal_year 2026 _chemical_formula_moiety 'C30 H40 Cl2 N5 O7 U, N3 O11 U' _chemical_formula_sum 'C30 H40 Cl2 N8 O18 U2' _chemical_formula_weight 1347.66 _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 _atom_sites_solution_primary dual _audit_creation_date 2025-10-31 _audit_creation_method ; Olex2 1.5 (compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188) ; _audit_update_record ; 2025-11-02 deposited with the CCDC. 2026-05-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 112.367(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.0546(16) _cell_length_b 16.1875(14) _cell_length_c 18.9986(19) _cell_measurement_reflns_used 9824 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 25.853 _cell_measurement_theta_min 2.318 _cell_volume 4566.0(8) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 29810 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 1.711 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.277 _exptl_absorpt_correction_T_max 0.0123 _exptl_absorpt_correction_T_min 0.0009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1573 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.0732. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.960 _exptl_crystal_description plate _exptl_crystal_F_000 2552 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _refine_diff_density_max 3.100 _refine_diff_density_min -2.446 _refine_diff_density_rms 0.261 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 554 _refine_ls_number_reflns 8031 _refine_ls_number_restraints 47 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0777 _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^)+(0.1491P)^2^+23.9837P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2096 _refine_ls_wR_factor_ref 0.2336 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5851 _reflns_number_total 8031 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00392c2.cif _cod_data_source_block sg3_7 _cod_database_code 7721100 _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. ; _olex2_refinement_description ; 1. Restrained distances C22A-C21 = C22-C21 1.54 with sigma of 0.02 N4-C27 1.43 with sigma of 0.01 N4-C28A 2.5 with sigma of 0.02 N4-C28 2.5 with sigma of 0.02 C27-C28 1.54 with sigma of 0.01 C27-C29 2.5 with sigma of 0.02 C29A-C30 = C30-C29 1.54 with sigma of 0.01 C27-C28A 1.54 with sigma of 0.01 C28A-C30 2.5 with sigma of 0.02 C28A-C29A 1.54 with sigma of 0.02 C25A-C24 = C25-C24 = C26-C25 1.54 with sigma of 0.01 C28-C30 2.5 with sigma of 0.02 C28-C29 1.54 with sigma of 0.01 C25A-C26A 1.54 with sigma of 0.02 C22-C21 1.54 with sigma of 0.02 C17-C16 1.54 with sigma of 0.02 2. Uiso/Uaniso restraints and constraints C25 \\sim C26: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A Uanis(C27) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uiso(C28) = Uiso(C28A) = Uiso(C29) = Uiso(C29A) Uanis(C22) = Uanis(C22A) 3. Rigid body (RIGU) restrains N4, C12, C27 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: H21A(0.65) H21B(0.65) H21C(0.35) H21D(0.35) H24A(0.5) H24B(0.5) H24C(0.5) H24D(0.5) H27A(0.5) H27B(0.5) H27C(0.5) H27D(0.5) H30D(0.5) H30E(0.5) H30F(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C22(0.65) H22A(0.65) H22B(0.65) H22C(0.65) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29C(0.5) H29D(0.5) C22A(0.35) H22D(0.35) H22E(0.35) H22F(0.35) C25A(0.5) H25C(0.5) H25D(0.5) C26A(0.5) H26D(0.5) H26E(0.5) H26F(0.5) C28A(0.5) H28C(0.5) H28D(0.5) C29A(0.5) H29A(0.5) H29B(0.5) O16(0.5) O17(0.5) O18(0.5) N8(0.5) O19(0.5) O20(0.5) O21(0.5) N9(0.5) 5.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A, H20B), C21(H21A,H21B), C21(H21C,H21D), C23(H23A,H23B), C24(H24A,H24B), C24(H24C,H24D), C27(H27A,H27B), C27(H27C,H27D), C25(H25A,H25B), C28(H28A,H28B), C29(H29C,H29D), C25A(H25C,H25D), C28A(H28C,H28D), C29A(H29A,H29B) 5.b Me refined with riding coordinates: C30(H30D,H30E,H30F), C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C26(H26A,H26B, H26C), C22A(H22D,H22E,H22F), C26A(H26D,H26E,H26F) 5.c Aromatic/amide H refined with riding coordinates: C3(H3), C10(H10), C13(H13), C14(H14) 5.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; sg3_7.res created by SHELXL-2014/7 TITL sg3_7_a.res in P2(1)/n REM Old TITL SG3_7 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.160, Rweak 0.011, Alpha 0.064, Orientation as input REM Formula found by SHELXT: C26 N7 O15 Cl2 U2 CELL 0.71073 16.0546 16.1875 18.9986 90 112.367 90 ZERR 4 0.0016 0.0014 0.0019 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl N O U UNIT 120 160 8 32 72 8 DFIX 1.54 C22A C21 C22 C21 DFIX 1.43 0.01 N4 C27 DFIX 2.5 N4 C28A DFIX 2.5 N4 C28 RIGU N4 C12 C27 DFIX 1.54 0.01 C27 C28 DFIX 2.5 C27 C29 DFIX 1.54 0.01 C29A C30 C30 C29 DFIX 1.54 0.01 C27 C28A ISOR 0.01 0.02 C27 C30 DFIX 2.5 C28A C30 EADP C28 C28A C29 C29A DFIX 1.54 C28A C29A DFIX 1.54 0.01 C25A C24 C25 C24 C26 C25 DFIX 2.5 C28 C30 DFIX 1.54 0.01 C28 C29 DFIX 1.54 C25A C26A SIMU 0.02 0.04 2 C25 C26 DFIX 1.54 C22 C21 EADP C22 C22A DFIX 1.54 C17 C16 L.S. 6 PLAN 50 TEMP -173.15 CONF CONN 10 U2 CONN 8 U1 list 4 MORE -1 BOND $H ABIN fmap 2 53 acta OMIT -2 50 REM REM REM WGHT 0.149100 23.983700 FVAR 0.13384 U1 6 0.582073 0.362034 0.383855 11.00000 0.05776 0.07549 = 0.05214 0.00009 0.02004 -0.00148 CL1 3 0.399415 0.216138 0.643936 11.00000 0.10191 0.10428 = 0.08330 -0.00480 0.05463 -0.01778 CL2 3 0.407823 -0.042284 0.315239 11.00000 0.10763 0.07007 = 0.06444 -0.00561 0.01462 -0.00537 O1 5 0.578756 0.450216 0.486672 11.00000 0.07424 0.07337 = 0.06126 -0.00029 0.02419 -0.00837 O2 5 0.603330 0.278144 0.287243 11.00000 0.08128 0.08879 = 0.07137 0.00104 0.04420 0.00092 O3 5 0.464397 0.372564 0.333844 11.00000 0.05232 0.08590 = 0.05640 -0.01219 0.01747 0.00244 O4 5 0.699336 0.349689 0.435835 11.00000 0.05663 0.09008 = 0.06970 0.00991 0.02209 0.00124 O5 5 0.596616 0.514243 0.368685 11.00000 0.07443 0.09656 = 0.05881 0.00488 0.02541 -0.00467 O6 5 0.608616 0.438213 0.280053 11.00000 0.08561 0.08786 = 0.07545 0.00178 0.04513 0.00275 O7 5 0.608694 0.572174 0.268753 11.00000 0.12084 0.09834 = 0.12093 0.02407 0.07679 0.00907 N1 4 0.538184 0.296755 0.489936 11.00000 0.05010 0.07508 = 0.05177 0.00067 0.01055 -0.00078 N2 4 0.550672 0.203071 0.380509 11.00000 0.07007 0.05269 = 0.05126 -0.00273 0.01922 -0.00195 N3 4 0.641706 0.456819 0.615335 11.00000 0.06944 0.06962 = 0.05439 -0.00483 0.01982 0.00422 N4 4 0.665910 0.164704 0.263247 11.00000 0.12044 0.11194 = 0.13041 -0.02177 0.07845 0.00341 N5 4 0.604622 0.510080 0.304450 11.00000 0.07320 0.08388 = 0.08263 0.00720 0.03903 -0.00119 C1 1 0.588722 0.422285 0.552405 11.00000 0.05443 0.08529 = 0.04825 -0.00306 0.01824 -0.00349 C2 1 0.540372 0.341732 0.548419 11.00000 0.06400 0.06185 = 0.04996 -0.00048 0.02056 0.00038 C3 1 0.497475 0.319329 0.596656 11.00000 0.07498 0.07501 = 0.05896 -0.00714 0.02212 -0.00474 AFIX 43 H3 2 0.498228 0.354859 0.636692 11.00000 -1.20000 AFIX 0 C4 1 0.453869 0.244471 0.585089 11.00000 0.06617 0.11193 = 0.04935 0.01261 0.02695 -0.00449 C5 1 0.452532 0.193407 0.524873 11.00000 0.06183 0.07578 = 0.05952 -0.00155 0.02261 -0.00041 C6 1 0.496245 0.221669 0.481316 11.00000 0.05269 0.07330 = 0.04840 -0.00386 0.01603 0.00104 C7 1 0.501081 0.172029 0.419145 11.00000 0.05749 0.06690 = 0.05084 0.00810 0.01588 0.00685 C8 1 0.456595 0.092913 0.404244 11.00000 0.05978 0.06858 = 0.05252 -0.00257 0.00816 0.00874 C9 1 0.465215 0.051244 0.342922 11.00000 0.06292 0.07146 = 0.05775 -0.00100 0.01191 0.00064 C10 1 0.514734 0.078937 0.303243 11.00000 0.08574 0.06496 = 0.05991 -0.01258 0.01008 0.01054 AFIX 43 H10 2 0.520639 0.047286 0.263288 11.00000 -1.20000 AFIX 0 C11 1 0.556465 0.155879 0.323827 11.00000 0.04920 0.10267 = 0.05886 0.00828 0.02150 0.01682 C12 1 0.612570 0.200904 0.287926 11.00000 0.07756 0.09730 = 0.06428 -0.00648 0.02951 0.01357 C13 1 0.410201 0.068844 0.450333 11.00000 0.07243 0.07551 = 0.05048 -0.00029 0.01337 0.00503 AFIX 43 H13 2 0.378502 0.017865 0.439886 11.00000 -1.20000 AFIX 0 C14 1 0.408847 0.114500 0.507971 11.00000 0.07575 0.07633 = 0.05910 0.01115 0.02021 -0.00691 AFIX 43 H14 2 0.378300 0.094454 0.538630 11.00000 -1.20000 AFIX 0 C15 1 0.687848 0.536847 0.609689 11.00000 0.06713 0.07921 = 0.06416 -0.00909 0.02846 -0.01823 AFIX 23 H15A 2 0.703824 0.568605 0.657574 11.00000 -1.20000 H15B 2 0.646808 0.570955 0.567471 11.00000 -1.20000 AFIX 0 C16 1 0.774013 0.515942 0.595096 11.00000 0.09336 0.08611 = 0.07935 -0.02683 0.02037 -0.02300 AFIX 23 H16A 2 0.814137 0.481116 0.637182 11.00000 -1.20000 H16B 2 0.757361 0.483936 0.547287 11.00000 -1.20000 AFIX 0 C17 1 0.825026 0.595065 0.589071 11.00000 0.10709 0.09932 = 0.07961 -0.01275 0.02636 -0.04019 AFIX 23 H17A 2 0.879806 0.578995 0.580319 11.00000 -1.20000 H17B 2 0.844492 0.625136 0.638080 11.00000 -1.20000 AFIX 0 C18 1 0.767831 0.653906 0.524317 11.00000 0.13746 0.12297 = 0.08903 0.01285 0.02278 -0.03036 AFIX 137 H18A 2 0.742294 0.622927 0.476535 11.00000 -1.50000 H18B 2 0.806080 0.698494 0.518616 11.00000 -1.50000 H18C 2 0.718970 0.677486 0.536874 11.00000 -1.50000 AFIX 0 C19 1 0.674170 0.418669 0.689449 11.00000 0.06928 0.06574 = 0.04915 -0.00316 0.01568 -0.00278 AFIX 23 H19A 2 0.740807 0.420887 0.710768 11.00000 -1.20000 H19B 2 0.656439 0.359714 0.683299 11.00000 -1.20000 AFIX 0 C20 1 0.640666 0.457025 0.745984 11.00000 0.07495 0.08203 = 0.05796 -0.00335 0.01894 0.00044 AFIX 23 H20A 2 0.574011 0.458556 0.723900 11.00000 -1.20000 H20B 2 0.662730 0.514621 0.756204 11.00000 -1.20000 AFIX 0 C21 1 0.673351 0.407320 0.823318 11.00000 0.11889 0.09591 = 0.06157 -0.00144 0.02669 0.02756 PART 1 AFIX 23 H21A 2 0.737996 0.393701 0.838753 10.65000 -1.20000 H21B 2 0.666771 0.442536 0.863494 10.65000 -1.20000 AFIX 23 PART 2 H21C 2 0.660798 0.348126 0.810600 10.35000 -1.20000 H21D 2 0.739591 0.413378 0.847638 10.35000 -1.20000 AFIX 0 PART 0 C23 1 0.690931 0.075478 0.272561 11.00000 0.09830 0.11900 = 0.10291 -0.00880 0.06126 0.01609 AFIX 23 H23A 2 0.675214 0.052357 0.314158 11.00000 -1.20000 H23B 2 0.756983 0.070618 0.287985 11.00000 -1.20000 AFIX 0 C24 1 0.644391 0.023542 0.200178 11.00000 0.13974 0.09990 = 0.11003 0.00577 0.05916 0.01562 PART 1 AFIX 23 H24A 2 0.657618 -0.035430 0.213586 10.50000 -1.20000 H24B 2 0.578483 0.031038 0.183664 10.50000 -1.20000 AFIX 23 PART 2 H24C 2 0.578374 0.027816 0.185324 10.50000 -1.20000 H24D 2 0.659209 0.047461 0.158404 10.50000 -1.20000 AFIX 0 PART 0 C27 1 0.732053 0.214033 0.248503 11.00000 0.13262 0.15175 = 0.15560 -0.00697 0.08031 -0.00090 PART 1 AFIX 23 H27A 2 0.700039 0.255704 0.209419 10.50000 -1.20000 H27B 2 0.765620 0.177759 0.226556 10.50000 -1.20000 AFIX 23 PART 3 H27C 2 0.713517 0.272779 0.242914 10.50000 -1.20000 H27D 2 0.737184 0.195842 0.200564 10.50000 -1.20000 AFIX 0 PART 0 C30 1 0.969457 0.267736 0.394224 11.00000 0.21249 0.21428 = 0.21580 0.00247 0.08313 -0.00676 PART 3 AFIX 33 H30D 2 1.015032 0.309152 0.396755 10.50000 -1.50000 H30E 2 0.945319 0.279515 0.433411 10.50000 -1.50000 H30F 2 0.996947 0.212696 0.402828 10.50000 -1.50000 AFIX 33 PART 1 H30A 2 1.024642 0.234807 0.415684 10.50000 -1.50000 H30B 2 0.976036 0.308205 0.358321 10.50000 -1.50000 H30C 2 0.958740 0.296649 0.435317 10.50000 -1.50000 AFIX 0 C22 1 0.620038 0.327780 0.816689 10.65000 0.07661 0.09757 = 0.08861 0.00634 0.04597 -0.00912 AFIX 33 H22A 2 0.642362 0.298921 0.865722 10.65000 -1.50000 H22B 2 0.556138 0.341056 0.802409 10.65000 -1.50000 H22C 2 0.627343 0.292234 0.777675 10.65000 -1.50000 AFIX 0 C25 1 0.670873 0.042984 0.132336 10.50000 0.11418 0.18873 = 0.15087 -0.05212 0.09278 -0.03396 AFIX 23 H25A 2 0.736914 0.038043 0.147724 10.50000 -1.20000 H25B 2 0.652934 0.100132 0.114408 10.50000 -1.20000 AFIX 0 C26 1 0.622475 -0.018861 0.068358 10.50000 0.14349 0.15557 = 0.14526 -0.06446 0.07416 -0.05588 AFIX 33 H26A 2 0.638515 -0.007484 0.024427 10.50000 -1.50000 H26B 2 0.640875 -0.075193 0.086536 10.50000 -1.50000 H26C 2 0.557190 -0.013321 0.053337 10.50000 -1.50000 AFIX 0 C28 1 0.800665 0.259317 0.317495 10.50000 0.21980 AFIX 23 H28A 2 0.813593 0.314404 0.301396 10.50000 -1.20000 H28B 2 0.774568 0.267506 0.356545 10.50000 -1.20000 AFIX 0 C29 1 0.888772 0.210118 0.352100 10.50000 0.21980 AFIX 23 H29C 2 0.900142 0.180250 0.311160 10.50000 -1.20000 H29D 2 0.882829 0.168683 0.388233 10.50000 -1.20000 AFIX 0 PART 2 C22A 1 0.633503 0.429587 0.884230 10.35000 0.07661 0.09757 = 0.08861 0.00634 0.04597 -0.00912 AFIX 33 H22D 2 0.660186 0.393622 0.928686 10.35000 -1.50000 H22E 2 0.647276 0.487354 0.899722 10.35000 -1.50000 H22F 2 0.568057 0.421749 0.862484 10.35000 -1.50000 AFIX 0 C25A 1 0.670632 -0.068178 0.208376 10.50000 0.16510 AFIX 23 H25C 2 0.736275 -0.073448 0.221503 10.50000 -1.20000 H25D 2 0.656509 -0.092842 0.250224 10.50000 -1.20000 AFIX 0 C26A 1 0.619678 -0.114939 0.134233 10.50000 0.16469 AFIX 33 H26D 2 0.637357 -0.173261 0.140654 10.50000 -1.50000 H26E 2 0.554721 -0.110409 0.121660 10.50000 -1.50000 H26F 2 0.634378 -0.091042 0.092979 10.50000 -1.50000 AFIX 0 PART 3 C28A 1 0.824226 0.204235 0.315762 10.50000 0.21980 AFIX 23 H28C 2 0.814960 0.207653 0.364304 10.50000 -1.20000 H28D 2 0.849151 0.148929 0.313035 10.50000 -1.20000 AFIX 0 C29A 1 0.892715 0.270628 0.315295 10.50000 0.21980 AFIX 23 H29A 2 0.916031 0.258732 0.275036 10.50000 -1.20000 H29B 2 0.864144 0.325887 0.305773 10.50000 -1.20000 AFIX 0 PART 0 U2 6 0.823676 0.219897 0.623300 11.00000 0.06237 0.07212 = 0.05178 0.00230 0.01683 -0.00147 O8 5 0.735069 0.291380 0.592029 11.00000 0.08580 0.08625 = 0.05782 0.00020 0.03448 0.01405 O9 5 0.910333 0.147281 0.656677 11.00000 0.07846 0.09302 = 0.07203 -0.00471 0.03888 0.00920 O10 5 0.859746 0.278455 0.751193 11.00000 0.07874 0.06721 = 0.04661 0.00415 0.01928 -0.00320 O11 5 0.766826 0.177561 0.721337 11.00000 0.06875 0.08936 = 0.06076 -0.00546 0.01266 -0.00818 O12 5 0.806818 0.234096 0.834183 11.00000 0.08239 0.09876 = 0.05137 0.00701 0.02852 0.00557 O13 5 0.716148 0.105623 0.572947 11.00000 0.08470 0.10003 = 0.05717 0.00058 0.03391 -0.01795 O14 5 0.773063 0.154364 0.495798 11.00000 0.07707 0.07554 = 0.06527 -0.00086 0.02785 -0.00479 O15 5 0.683907 0.048351 0.461252 11.00000 0.09508 0.08492 = 0.05958 -0.00058 0.00786 -0.01661 N6 4 0.810470 0.229697 0.771702 11.00000 0.06455 0.05956 = 0.06161 0.00914 0.01660 0.01169 N7 4 0.722153 0.100913 0.507787 11.00000 0.07217 0.07599 = 0.06386 0.00283 0.01863 -0.00339 PART 1 O16 5 0.916442 0.345787 0.648393 10.50000 0.07068 O17 5 0.879310 0.293083 0.537111 10.50000 0.07732 0.05665 = 0.06354 0.01137 0.02423 0.02044 O18 5 0.955651 0.406744 0.563997 10.50000 0.10959 N8 4 0.923028 0.349101 0.584712 10.50000 0.07956 PART 2 O19 5 0.946232 0.321901 0.652894 10.50000 0.07643 O20 5 0.901625 0.262802 0.541827 10.50000 0.07995 0.05520 = 0.04839 -0.00331 0.00997 -0.00222 O21 5 1.009468 0.357633 0.574534 10.50000 0.12394 N9 4 0.954181 0.314186 0.589550 10.50000 0.08746 HKLF 4 REM sg3_7_a.res in P2(1)/n REM R1 = 0.0777 for 5851 Fo > 4sig(Fo) and 0.0995 for all 8031 data REM 554 parameters refined using 47 restraints END WGHT 0.1491 23.9654 REM Highest difference peak 3.100, deepest hole -2.446, 1-sigma level 0.261 Q1 1 0.6227 0.3914 0.4153 11.00000 0.05 3.10 Q2 1 0.6170 0.3771 0.3601 11.00000 0.05 2.92 Q3 1 0.8598 0.2009 0.6004 11.00000 0.05 2.89 Q4 1 0.7802 0.1968 0.6398 11.00000 0.05 2.76 Q5 1 0.7742 0.2471 0.5833 11.00000 0.05 2.71 Q6 1 0.7758 0.1917 0.5833 11.00000 0.05 2.69 Q7 1 0.5306 0.3841 0.3463 11.00000 0.05 2.68 Q8 1 0.5397 0.3793 0.4024 11.00000 0.05 2.52 Q9 1 0.8739 0.2009 0.6657 11.00000 0.05 2.49 Q10 1 0.8635 0.2544 0.6559 11.00000 0.05 2.25 Q11 1 0.6853 0.2196 0.1988 11.00000 0.05 1.07 Q12 1 0.4407 0.2196 0.6184 11.00000 0.05 0.94 Q13 1 0.7855 0.2752 0.2792 11.00000 0.05 0.80 Q14 1 0.5707 0.1404 0.3602 11.00000 0.05 0.77 Q15 1 0.3365 0.2352 0.6046 11.00000 0.05 0.72 Q16 1 0.6761 0.5583 0.8809 11.00000 0.05 0.64 Q17 1 0.5769 0.4597 0.9177 11.00000 0.05 0.59 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-0.1741 6 9 14 1.0075 0.0207 6 9 15 -0.2395 -0.0638 6 10 6 1.6538 -0.1114 6 10 7 -0.5070 -0.1876 6 10 8 -0.2520 -0.0502 6 10 9 -0.4032 -0.0889 6 10 10 1.1241 0.0517 6 10 11 0.0374 -0.1330 6 10 12 2.4838 0.1455 6 10 13 0.4245 -0.0753 6 10 14 0.8687 -0.0301 6 10 15 0.4188 0.2789 6 11 6 -0.7182 -0.0569 6 11 7 0.7296 -0.0295 6 11 8 -0.8971 -0.0224 6 11 9 0.9089 -0.0707 6 11 10 1.6342 -0.0591 6 11 11 -0.5797 -0.1923 6 11 12 0.3052 0.0886 6 11 13 -1.7152 -0.0712 6 11 14 -1.3405 -0.1393 6 12 6 -1.3738 0.0811 6 12 7 2.7838 0.0731 6 12 8 0.1710 -0.0423 6 12 9 -0.1088 0.0824 6 12 10 0.1554 0.0799 6 12 11 -1.7512 -0.0108 6 12 12 -0.0139 0.0668 6 12 13 -0.3281 -0.0902 6 13 6 -1.4713 -0.1098 6 13 7 0.7747 0.0839 6 13 8 -0.3772 0.0105 6 13 9 -1.3728 0.1530 6 13 10 -0.0443 0.0198 6 13 11 -0.2318 -0.0354 6 13 12 0.6201 0.0600 6 14 6 -0.8260 0.0732 6 14 7 -1.0709 0.0713 6 14 8 -0.1725 -0.1054 6 14 9 -0.1615 -0.2201 6 14 10 -0.0319 -0.0116 6 14 11 1.0795 -0.1257 6 15 6 -0.2331 -0.1106 6 15 7 0.0701 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0.0559 7 4 8 -1.0454 -0.0191 7 4 9 -1.3328 0.1441 7 4 10 -1.1663 -0.1772 7 4 11 -0.3630 0.1266 7 4 12 0.9281 0.3967 7 4 13 0.8340 0.3747 7 4 14 0.7732 0.2346 7 4 15 1.1434 0.0706 7 4 16 -0.7305 -0.1489 7 5 7 -1.3605 -0.2858 7 5 8 1.4368 -0.2777 7 5 9 0.5909 -0.1004 7 5 10 1.5097 -0.0337 7 5 11 -0.9091 0.0315 7 5 12 0.2195 -0.2667 7 5 13 -2.3392 -0.2140 7 5 14 -2.4299 -0.2098 7 5 15 -1.3458 0.0404 7 5 16 -0.7554 0.0691 7 6 7 -1.6845 0.0489 7 6 8 0.2109 0.1622 7 6 9 -3.4058 -0.0355 7 6 10 0.3848 -0.1462 7 6 11 -3.3188 -0.1581 7 6 12 1.2639 -0.1421 7 6 13 0.2059 0.0606 7 6 14 1.8114 0.0735 7 6 15 1.4156 -0.1381 7 6 16 1.8485 -0.0591 7 7 7 -1.6241 -0.0324 7 7 8 2.3701 0.0915 7 7 9 -1.0648 -0.0477 7 7 10 3.9334 0.1680 7 7 11 -0.6950 0.1296 7 7 12 1.8925 0.0533 7 7 13 -0.0730 -0.1450 7 7 14 0.6223 -0.0376 7 7 15 -0.9534 -0.1551 7 8 7 0.8706 -0.0826 7 8 8 2.2556 0.0196 7 8 9 -1.8180 -0.1143 7 8 10 1.4189 -0.0474 7 8 11 -0.9135 -0.0790 7 8 12 0.9885 0.1126 7 8 13 -0.0113 0.0412 7 8 14 0.0960 0.1502 7 8 15 -1.1969 0.1091 7 9 7 -1.7805 -0.1375 7 9 8 0.4154 0.0144 7 9 9 -0.6230 0.0090 7 9 10 1.6382 0.1295 7 9 11 -0.6465 -0.0609 7 9 12 -0.2658 0.0773 7 9 13 -1.1603 -0.0560 7 9 14 -0.6928 -0.1072 7 10 7 0.7607 0.1333 7 10 8 0.7640 0.1273 7 10 9 -1.3360 -0.0381 7 10 10 0.0008 0.0166 7 10 11 -2.2805 -0.1290 7 10 12 -0.3091 0.0130 7 10 13 -0.1366 0.0794 7 10 14 0.0777 -0.1293 7 11 7 -0.2161 -0.0041 7 11 8 -0.3803 -0.0107 7 11 9 -2.3091 0.0836 7 11 10 0.9272 0.0975 7 11 11 -0.7048 0.0784 7 11 12 1.7120 0.0110 7 11 13 0.7357 0.0544 7 12 7 -1.1115 -0.0494 7 12 8 0.8225 -0.1038 7 12 9 -0.2466 -0.0683 7 12 10 2.7447 -0.1171 7 12 11 0.0149 -0.0095 7 12 12 1.2350 0.0103 7 13 7 1.0155 -0.0632 7 13 8 1.6850 0.0399 7 13 9 -0.3104 -0.0080 7 13 10 -0.0758 0.1246 7 13 11 -1.8258 -0.0002 7 14 7 -0.3021 -0.0093 7 14 8 -0.8596 0.2465 7 14 9 -0.0281 -0.1582 7 14 10 -0.2884 0.0778 7 15 7 0.5692 -0.2004 7 15 8 -0.6028 -0.1103 7 15 9 1.2740 -0.3116 7 16 7 0.5984 0.3075 8 0 8 -0.5345 1.7341 8 0 10 3.1850 0.5544 8 0 12 3.3856 0.5257 8 0 14 0.4869 -0.3672 8 0 16 -0.1067 -0.3502 8 1 8 1.9817 0.4503 8 1 9 -0.2779 -0.5484 8 1 10 0.4147 0.4531 8 1 11 -3.0745 -0.1030 8 1 12 0.3443 0.3000 8 1 13 -1.3703 -0.0451 8 1 14 0.3587 -0.1265 8 1 15 1.0979 0.3140 8 1 16 -0.0798 0.2076 8 2 8 -0.6271 0.1218 8 2 9 -2.3163 0.4025 8 2 10 0.6801 -0.2448 8 2 11 -1.3294 -0.1748 8 2 12 1.9305 -0.0418 8 2 13 -0.9364 0.2191 8 2 14 -1.2666 0.1195 8 2 15 -0.4626 0.1197 8 2 16 -1.2711 0.0732 8 3 8 1.4221 -0.9503 8 3 9 -1.0330 0.0080 8 3 10 2.2647 -0.4519 8 3 11 -1.8703 0.1608 8 3 12 1.5320 -0.0327 8 3 13 -0.0811 -0.1302 8 3 14 0.4875 -0.3694 8 3 15 1.2042 -0.2484 8 3 16 0.8420 -0.2778 8 4 8 3.1035 -0.0122 8 4 9 -1.5494 0.4529 8 4 10 1.8088 -0.0617 8 4 11 -1.8530 -0.1401 8 4 12 0.5473 -0.4380 8 4 13 -0.7426 -0.0685 8 4 14 -0.9965 -0.0135 8 4 15 -0.6373 0.1817 8 5 8 1.1862 -0.0046 8 5 9 -1.8801 -0.0519 8 5 10 1.1743 -0.0744 8 5 11 -0.5703 0.3790 8 5 12 0.7685 0.2223 8 5 13 1.5521 0.4056 8 5 14 1.2954 0.0867 8 5 15 0.5107 0.0012 8 6 8 2.7988 0.0327 8 6 9 0.5816 0.1049 8 6 10 1.9130 0.0673 8 6 11 0.9340 0.1397 8 6 12 -0.1827 -0.1798 8 6 13 -0.3015 -0.0680 8 6 14 -0.4767 -0.0116 8 6 15 -1.9476 0.0261 8 7 8 -1.2193 0.0204 8 7 9 -2.7008 -0.0476 8 7 10 -1.8897 -0.1164 8 7 11 -1.3395 0.0331 8 7 12 -1.7064 0.0206 8 7 13 -1.3518 0.0583 8 7 14 0.1616 0.0198 8 8 8 1.4030 -0.0001 8 8 9 0.4727 0.0766 8 8 10 0.6906 -0.0646 8 8 11 0.4392 -0.1200 8 8 12 0.4972 -0.1654 8 8 13 0.6406 -0.1193 8 8 14 1.3401 -0.1388 8 9 8 0.2823 -0.1072 8 9 9 -1.4810 -0.0622 8 9 10 0.5835 0.0067 8 9 11 0.2546 0.0809 8 9 12 0.9672 0.1758 8 9 13 0.7316 0.1631 8 10 8 1.9432 -0.0386 8 10 9 -0.7095 0.1158 8 10 10 1.9486 0.0491 8 10 11 -0.2261 0.0243 8 10 12 -0.4388 -0.1069 8 10 13 -0.2457 -0.1033 8 11 8 2.7472 -0.1031 8 11 9 -0.8608 0.0053 8 11 10 0.9874 -0.2114 8 11 11 -0.8082 0.0082 8 11 12 -0.2859 -0.0340 8 12 8 -0.4770 0.0345 8 12 9 -2.2823 0.1052 8 12 10 -0.7960 -0.0502 8 12 11 -1.3913 0.0554 8 13 8 -0.5630 0.0542 8 13 9 1.0591 -0.0684 8 13 10 1.8635 0.0188 8 14 8 -0.8303 0.1267 8 14 9 -0.2091 0.0567 9 0 9 -5.6838 -1.7344 9 0 11 -3.9330 -1.7247 9 0 13 -0.1829 -0.2016 9 0 15 0.3494 0.1670 9 1 9 -0.7511 -0.4279 9 1 10 4.4918 1.0360 9 1 11 0.4803 -0.3711 9 1 12 2.0499 0.4919 9 1 13 -0.3002 0.0913 9 1 14 -0.9868 -0.2811 9 1 15 -0.0752 0.0039 9 2 9 -1.6435 0.1030 9 2 10 1.6844 0.2549 9 2 11 -3.4115 -0.0473 9 2 12 0.8142 -0.1417 9 2 13 0.0661 0.0942 9 2 14 0.6286 -0.0303 9 2 15 1.2566 0.0042 9 3 9 -4.0330 0.3475 9 3 10 2.5623 -0.0699 9 3 11 -1.9052 0.1978 9 3 12 1.3131 0.1081 9 3 13 -0.4420 0.3133 9 3 14 -1.1988 0.2243 9 3 15 -0.8361 0.1766 9 4 9 -1.4452 -0.1304 9 4 10 1.6074 -0.0902 9 4 11 -0.8534 0.1454 9 4 12 -0.5640 -0.1365 9 4 13 1.2208 -0.1400 9 4 14 0.2738 -0.1497 9 5 9 -0.2211 0.0315 9 5 10 -0.8867 -0.2022 9 5 11 1.8014 -0.0523 9 5 12 -1.8015 -0.2341 9 5 13 0.5019 -0.0455 9 5 14 -1.0441 -0.0795 9 6 9 0.9388 -0.0311 9 6 10 -2.8413 -0.1190 9 6 11 1.2650 0.0910 9 6 12 -1.7083 -0.0860 9 6 13 0.3293 -0.0088 9 6 14 1.2194 -0.0340 9 7 9 3.1464 0.0690 9 7 10 0.3445 -0.0487 9 7 11 2.6592 0.1527 9 7 12 1.6862 0.1671 9 7 13 0.2409 0.1999 9 8 9 -0.6166 0.1740 9 8 10 -1.1373 0.0814 9 8 11 -1.3935 0.0412 9 8 12 -0.6701 -0.0005 9 8 13 -1.8467 -0.2324 9 9 9 -0.5863 -0.0356 9 9 10 0.2990 -0.1309 9 9 11 -0.7555 -0.2724 9 9 12 -0.0074 0.0380 9 10 9 -1.4226 0.0413 9 10 10 0.3820 0.0343 9 10 11 0.6323 0.0583 9 10 12 -0.0769 0.2617 9 11 9 -0.5287 0.2522 9 11 10 -0.3454 0.0284 9 11 11 0.3021 0.0830 9 12 9 1.6882 0.0605 9 12 10 1.0948 -0.2088 9 13 9 -1.3064 0.0017 10 0 10 4.0366 2.7698 10 0 12 0.4221 1.0222 10 0 14 -0.4743 0.1125 10 1 10 -1.1229 0.2279 10 1 11 -2.6279 -1.0762 10 1 12 0.1649 -0.2176 10 1 13 0.4786 0.0306 10 1 14 0.1199 -0.2495 10 2 10 3.8544 0.1000 10 2 11 -0.0712 0.0401 10 2 12 1.0682 -0.2809 10 2 13 -0.0981 -0.0709 10 2 14 -1.2687 -0.1257 10 3 10 0.7729 -0.0888 10 3 11 -1.6817 0.0657 10 3 12 -0.9681 0.0330 10 3 13 1.2176 0.0114 10 3 14 -0.2838 0.0895 10 4 10 0.0574 0.1348 10 4 11 2.8252 0.1378 10 4 12 -1.4943 0.2243 10 4 13 1.6749 -0.0371 10 5 10 -3.6837 -0.0794 10 5 11 1.8169 -0.1156 10 5 12 -2.8246 -0.0180 10 5 13 1.0485 0.0766 10 6 10 -1.7001 0.0680 10 6 11 2.4812 0.1798 10 6 12 0.3974 0.1525 10 6 13 -0.5201 -0.0059 10 7 10 -1.7749 -0.2095 10 7 11 -2.0888 -0.3955 10 7 12 0.4624 -0.2694 10 8 10 1.8127 0.2415 10 8 11 -0.2835 0.1089 10 8 12 2.2467 0.6623 10 9 10 0.8315 0.2133 10 9 11 -0.5151 -0.4291 10 10 10 -0.5682 0.0969 10 11 10 -0.1639 -0.1610 11 0 11 -0.1592 -1.4261 11 0 13 0.6859 -0.1497 11 1 11 0.2645 0.7025 11 1 12 -0.3809 0.1989 11 1 13 -0.0028 0.7097 11 2 11 -1.0772 0.2688 11 2 12 -0.6975 -0.1962 11 2 13 1.4482 0.0992 11 3 11 2.2510 -0.3077 11 3 12 -1.2480 -0.1275 11 4 11 0.9443 -0.2559 11 4 12 -2.9404 0.2720 11 5 11 3.6060 0.0342 11 5 12 0.0767 0.0719 11 6 11 -1.8910 -0.2477 11 7 11 -1.2672 0.0845 0 0 0 0.0 0.0 ; _shelx_fab_checksum 57350 _olex2_submission_special_instructions 'No special instructions were received' 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.58207(4) 0.36203(4) 0.38386(3) 0.0621(2) Uani 1 1 d . . . . . Cl1 Cl 0.3994(4) 0.2161(3) 0.6439(3) 0.0907(13) Uani 1 1 d . . . . . Cl2 Cl 0.4078(3) -0.0423(3) 0.3152(2) 0.0861(13) Uani 1 1 d . . . . . O1 O 0.5788(7) 0.4502(7) 0.4867(6) 0.070(3) Uani 1 1 d . . . . . O2 O 0.6033(8) 0.2781(8) 0.2872(6) 0.076(3) Uani 1 1 d . . . . . O3 O 0.4644(7) 0.3726(7) 0.3338(6) 0.066(3) Uani 1 1 d . . . . . O4 O 0.6993(7) 0.3497(7) 0.4358(6) 0.073(3) Uani 1 1 d . . . . . O5 O 0.5966(8) 0.5142(8) 0.3687(6) 0.077(3) Uani 1 1 d . . . . . O6 O 0.6086(8) 0.4382(8) 0.2801(7) 0.079(3) Uani 1 1 d . . . . . O7 O 0.6087(11) 0.5722(9) 0.2688(9) 0.104(4) Uani 1 1 d . . . . . N1 N 0.5382(8) 0.2968(8) 0.4899(7) 0.062(3) Uani 1 1 d . . . . . N2 N 0.5507(8) 0.2031(7) 0.3805(6) 0.059(3) Uani 1 1 d . . . . . N3 N 0.6417(9) 0.4568(8) 0.6153(7) 0.066(3) Uani 1 1 d . . . . . N4 N 0.6659(12) 0.1647(12) 0.2632(11) 0.112(6) Uani 1 1 d D U . . . N5 N 0.6046(10) 0.5101(10) 0.3044(8) 0.077(4) Uani 1 1 d . . . . . C1 C 0.5887(10) 0.4223(10) 0.5524(8) 0.063(4) Uani 1 1 d . . . . . C2 C 0.5404(10) 0.3417(9) 0.5484(8) 0.059(3) Uani 1 1 d . . . . . C3 C 0.4975(11) 0.3193(10) 0.5967(9) 0.071(4) Uani 1 1 d . . . . . H3 H 0.4982 0.3549 0.6367 0.085 Uiso 1 1 calc R U . . . C4 C 0.4539(11) 0.2445(13) 0.5851(8) 0.074(4) Uani 1 1 d . . . . . C5 C 0.4525(10) 0.1934(10) 0.5249(8) 0.066(4) Uani 1 1 d . . . . . C6 C 0.4962(10) 0.2217(9) 0.4813(8) 0.059(3) Uani 1 1 d . . . . . C7 C 0.5011(10) 0.1720(9) 0.4191(8) 0.060(3) Uani 1 1 d . . . . . C8 C 0.4566(10) 0.0929(9) 0.4042(8) 0.064(4) Uani 1 1 d . . . . . C9 C 0.4652(11) 0.0512(10) 0.3429(8) 0.067(4) Uani 1 1 d . . . . . C10 C 0.5147(12) 0.0789(10) 0.3032(9) 0.075(5) Uani 1 1 d . . . . . H10 H 0.5206 0.0473 0.2633 0.091 Uiso 1 1 calc R U . . . C11 C 0.5565(10) 0.1559(11) 0.3238(9) 0.070(4) Uani 1 1 d . . . . . C12 C 0.6126(12) 0.2009(13) 0.2879(9) 0.079(4) Uani 1 1 d . U . . . C13 C 0.4102(11) 0.0688(10) 0.4503(8) 0.069(4) Uani 1 1 d . . . . . H13 H 0.3785 0.0179 0.4399 0.083 Uiso 1 1 calc R U . . . C14 C 0.4088(11) 0.1145(10) 0.5080(9) 0.072(4) Uani 1 1 d . . . . . H14 H 0.3783 0.0945 0.5386 0.086 Uiso 1 1 calc R U . . . C15 C 0.6878(11) 0.5368(10) 0.6097(9) 0.069(4) Uani 1 1 d . . . . . H15A H 0.7038 0.5686 0.6576 0.083 Uiso 1 1 calc R U . . . H15B H 0.6468 0.5710 0.5675 0.083 Uiso 1 1 calc R U . . . C16 C 0.7740(13) 0.5159(11) 0.5951(11) 0.090(5) Uani 1 1 d D . . . . H16A H 0.8141 0.4811 0.6372 0.108 Uiso 1 1 calc R U . . . H16B H 0.7574 0.4839 0.5473 0.108 Uiso 1 1 calc R U . . . C17 C 0.8250(15) 0.5951(12) 0.5891(11) 0.098(6) Uani 1 1 d D . . . . H17A H 0.8798 0.5790 0.5803 0.118 Uiso 1 1 calc R U . . . H17B H 0.8445 0.6251 0.6381 0.118 Uiso 1 1 calc R U . . . C18 C 0.7678(17) 0.6539(15) 0.5243(13) 0.123(9) Uani 1 1 d . . . . . H18A H 0.7423 0.6229 0.4765 0.184 Uiso 1 1 calc R U . . . H18B H 0.8061 0.6985 0.5186 0.184 Uiso 1 1 calc R U . . . H18C H 0.7190 0.6775 0.5369 0.184 Uiso 1 1 calc R U . . . C19 C 0.6742(11) 0.4187(9) 0.6894(7) 0.063(4) Uani 1 1 d . . . . . H19A H 0.7408 0.4209 0.7108 0.076 Uiso 1 1 calc R U . . . H19B H 0.6564 0.3597 0.6833 0.076 Uiso 1 1 calc R U . . . C20 C 0.6407(12) 0.4570(11) 0.7460(9) 0.074(4) Uani 1 1 d . . . . . H20A H 0.5740 0.4586 0.7239 0.088 Uiso 1 1 calc R U . . . H20B H 0.6627 0.5146 0.7562 0.088 Uiso 1 1 calc R U . . . C21 C 0.6734(14) 0.4073(11) 0.8233(10) 0.094(6) Uani 1 1 d D . . . . H21A H 0.7380 0.3937 0.8388 0.113 Uiso 0.65 1 calc R U P A 1 H21B H 0.6668 0.4425 0.8635 0.113 Uiso 0.65 1 calc R U P A 1 H21C H 0.6608 0.3481 0.8106 0.113 Uiso 0.35 1 calc R U P B 2 H21D H 0.7396 0.4134 0.8476 0.113 Uiso 0.35 1 calc R U P B 2 C23 C 0.6909(15) 0.0755(14) 0.2726(12) 0.100(6) Uani 1 1 d . . . . . H23A H 0.6752 0.0524 0.3142 0.120 Uiso 1 1 calc R U . . . H23B H 0.7570 0.0706 0.2880 0.120 Uiso 1 1 calc R U . . . C24 C 0.6444(18) 0.0235(14) 0.2002(13) 0.113(7) Uani 1 1 d D . . . . H24A H 0.6576 -0.0354 0.2136 0.136 Uiso 0.5 1 calc R U P C 1 H24B H 0.5785 0.0310 0.1837 0.136 Uiso 0.5 1 calc R U P C 1 H24C H 0.5784 0.0278 0.1853 0.136 Uiso 0.5 1 calc R U P D 2 H24D H 0.6592 0.0475 0.1584 0.136 Uiso 0.5 1 calc R U P D 2 C27 C 0.7321(15) 0.2140(16) 0.2485(14) 0.139(8) Uani 1 1 d D U . . . H27A H 0.7000 0.2557 0.2094 0.167 Uiso 0.5 1 calc R U P E 1 H27B H 0.7656 0.1778 0.2266 0.167 Uiso 0.5 1 calc R U P E 1 H27C H 0.7135 0.2728 0.2429 0.167 Uiso 0.5 1 calc R U P F 3 H27D H 0.7372 0.1958 0.2006 0.167 Uiso 0.5 1 calc R U P F 3 C30 C 0.9695(18) 0.268(2) 0.394(2) 0.214(18) Uani 1 1 d D U . . . H30D H 1.0150 0.3092 0.3968 0.321 Uiso 0.5 1 calc R U P G 3 H30E H 0.9453 0.2795 0.4334 0.321 Uiso 0.5 1 calc R U P G 3 H30F H 0.9969 0.2127 0.4028 0.321 Uiso 0.5 1 calc R U P G 3 H30A H 1.0246 0.2348 0.4157 0.321 Uiso 0.5 1 calc R U P H 1 H30B H 0.9760 0.3082 0.3583 0.321 Uiso 0.5 1 calc R U P H 1 H30C H 0.9587 0.2966 0.4353 0.321 Uiso 0.5 1 calc R U P H 1 C22 C 0.6200(18) 0.3278(15) 0.8167(16) 0.083(7) Uani 0.65 1 d D . P I 1 H22A H 0.6424 0.2989 0.8657 0.125 Uiso 0.65 1 calc R U P I 1 H22B H 0.5561 0.3411 0.8024 0.125 Uiso 0.65 1 calc R U P I 1 H22C H 0.6273 0.2922 0.7777 0.125 Uiso 0.65 1 calc R U P I 1 C25 C 0.671(3) 0.043(3) 0.132(2) 0.139(17) Uani 0.5 1 d D U P J 1 H25A H 0.7369 0.0380 0.1477 0.166 Uiso 0.5 1 calc R U P J 1 H25B H 0.6529 0.1001 0.1144 0.166 Uiso 0.5 1 calc R U P J 1 C26 C 0.622(4) -0.019(3) 0.068(3) 0.142(17) Uani 0.5 1 d D U P J 1 H26A H 0.6385 -0.0075 0.0244 0.214 Uiso 0.5 1 calc R U P J 1 H26B H 0.6409 -0.0752 0.0865 0.214 Uiso 0.5 1 calc R U P J 1 H26C H 0.5572 -0.0133 0.0533 0.214 Uiso 0.5 1 calc R U P J 1 C28 C 0.8007(19) 0.259(3) 0.317(3) 0.22(2) Uiso 0.5 1 d D . P K 1 H28A H 0.8136 0.3144 0.3014 0.264 Uiso 0.5 1 calc R U P K 1 H28B H 0.7746 0.2675 0.3565 0.264 Uiso 0.5 1 calc R U P K 1 C29 C 0.889(3) 0.210(2) 0.352(4) 0.22(2) Uiso 0.5 1 d D . P K 1 H29C H 0.9001 0.1803 0.3112 0.264 Uiso 0.5 1 calc R U P K 1 H29D H 0.8828 0.1687 0.3882 0.264 Uiso 0.5 1 calc R U P K 1 C22A C 0.634(3) 0.430(3) 0.884(2) 0.083(7) Uani 0.35 1 d D . P I 2 H22D H 0.6602 0.3936 0.9287 0.125 Uiso 0.35 1 calc R U P I 2 H22E H 0.6473 0.4874 0.8997 0.125 Uiso 0.35 1 calc R U P I 2 H22F H 0.5681 0.4217 0.8625 0.125 Uiso 0.35 1 calc R U P I 2 C25A C 0.671(4) -0.0682(18) 0.208(3) 0.17(2) Uiso 0.5 1 d D . P J 2 H25C H 0.7363 -0.0734 0.2215 0.198 Uiso 0.5 1 calc R U P J 2 H25D H 0.6565 -0.0928 0.2502 0.198 Uiso 0.5 1 calc R U P J 2 C26A C 0.620(5) -0.115(4) 0.134(3) 0.16(2) Uiso 0.5 1 d D . P J 2 H26D H 0.6374 -0.1733 0.1407 0.247 Uiso 0.5 1 calc R U P J 2 H26E H 0.5547 -0.1104 0.1217 0.247 Uiso 0.5 1 calc R U P J 2 H26F H 0.6344 -0.0910 0.0930 0.247 Uiso 0.5 1 calc R U P J 2 C28A C 0.824(2) 0.204(4) 0.316(3) 0.22(2) Uiso 0.5 1 d D . P K 3 H28C H 0.8150 0.2077 0.3643 0.264 Uiso 0.5 1 calc R U P K 3 H28D H 0.8492 0.1489 0.3130 0.264 Uiso 0.5 1 calc R U P K 3 C29A C 0.893(4) 0.271(4) 0.315(3) 0.22(2) Uiso 0.5 1 d D . P K 3 H29A H 0.9160 0.2587 0.2750 0.264 Uiso 0.5 1 calc R U P K 3 H29B H 0.8641 0.3259 0.3058 0.264 Uiso 0.5 1 calc R U P K 3 U2 U 0.82368(4) 0.21990(4) 0.62330(3) 0.0635(2) Uani 1 1 d . . . . . O8 O 0.7351(8) 0.2914(7) 0.5920(6) 0.075(3) Uani 1 1 d . . . . . O9 O 0.9103(8) 0.1473(7) 0.6567(7) 0.078(3) Uani 1 1 d . . . . . O10 O 0.8597(7) 0.2785(6) 0.7512(5) 0.066(3) Uani 1 1 d . . . . . O11 O 0.7668(7) 0.1776(7) 0.7213(6) 0.077(3) Uani 1 1 d . . . . . O12 O 0.8068(8) 0.2341(8) 0.8342(6) 0.077(3) Uani 1 1 d . . . . . O13 O 0.7161(8) 0.1056(8) 0.5729(6) 0.079(3) Uani 1 1 d . . . . . O14 O 0.7731(8) 0.1544(7) 0.4958(6) 0.072(3) Uani 1 1 d . . . . . O15 O 0.6839(9) 0.0484(8) 0.4613(6) 0.086(3) Uani 1 1 d . . . . . N6 N 0.8105(9) 0.2297(8) 0.7717(7) 0.064(3) Uani 1 1 d . . . . . N7 N 0.7222(10) 0.1009(9) 0.5078(8) 0.073(3) Uani 1 1 d . . . . . O16 O 0.9164(18) 0.3458(16) 0.6484(14) 0.071(6) Uiso 0.5 1 d . . P L 1 O17 O 0.879(3) 0.293(2) 0.537(2) 0.067(9) Uani 0.5 1 d . . P L 1 O18 O 0.956(2) 0.407(2) 0.5640(18) 0.110(9) Uiso 0.5 1 d . . P L 1 N8 N 0.923(2) 0.349(2) 0.5847(19) 0.080(8) Uiso 0.5 1 d . . P L 1 O19 O 0.9462(19) 0.3219(17) 0.6529(15) 0.076(7) Uiso 0.5 1 d . . P L 2 O20 O 0.902(3) 0.263(2) 0.542(2) 0.065(8) Uani 0.5 1 d . . P L 2 O21 O 1.009(3) 0.358(2) 0.575(2) 0.124(11) Uiso 0.5 1 d . . P L 2 N9 N 0.954(3) 0.314(2) 0.590(2) 0.087(9) Uiso 0.5 1 d . . P L 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0578(4) 0.0755(4) 0.0521(3) 0.0001(2) 0.0200(3) -0.0015(2) Cl1 0.102(3) 0.104(3) 0.083(3) -0.005(2) 0.055(3) -0.018(3) Cl2 0.108(3) 0.070(2) 0.064(2) -0.0056(18) 0.015(2) -0.005(2) O1 0.074(7) 0.073(6) 0.061(6) 0.000(5) 0.024(5) -0.008(5) O2 0.081(8) 0.089(9) 0.071(7) 0.001(5) 0.044(6) 0.001(6) O3 0.052(5) 0.086(7) 0.056(5) -0.012(5) 0.017(5) 0.002(5) O4 0.057(6) 0.090(8) 0.070(6) 0.010(5) 0.022(5) 0.001(5) O5 0.074(7) 0.097(8) 0.059(6) 0.005(5) 0.025(5) -0.005(6) O6 0.086(8) 0.088(8) 0.075(7) 0.002(6) 0.045(6) 0.003(6) O7 0.121(11) 0.098(10) 0.121(11) 0.024(8) 0.077(10) 0.009(8) N1 0.050(6) 0.075(8) 0.052(6) 0.001(6) 0.011(5) -0.001(6) N2 0.070(7) 0.053(6) 0.051(6) -0.003(5) 0.019(6) -0.002(5) N3 0.069(8) 0.070(8) 0.054(6) -0.005(5) 0.020(6) 0.004(6) N4 0.120(11) 0.112(11) 0.130(14) -0.022(9) 0.078(11) 0.003(8) N5 0.073(9) 0.084(10) 0.083(9) 0.007(8) 0.039(8) -0.001(7) C1 0.054(8) 0.085(10) 0.048(7) -0.003(7) 0.018(6) -0.003(7) C2 0.064(9) 0.062(8) 0.050(7) 0.000(6) 0.021(7) 0.000(6) C3 0.075(10) 0.075(10) 0.059(8) -0.007(7) 0.022(8) -0.005(8) C4 0.066(9) 0.112(13) 0.049(7) 0.013(8) 0.027(7) -0.004(9) C5 0.062(9) 0.076(9) 0.060(8) -0.002(7) 0.023(7) 0.000(7) C6 0.053(8) 0.073(9) 0.048(7) -0.004(6) 0.016(6) 0.001(6) C7 0.057(8) 0.067(9) 0.051(7) 0.008(6) 0.016(6) 0.007(7) C8 0.060(8) 0.069(9) 0.053(7) -0.003(6) 0.008(7) 0.009(7) C9 0.063(9) 0.071(9) 0.058(8) -0.001(7) 0.012(7) 0.001(7) C10 0.086(11) 0.065(10) 0.060(8) -0.013(7) 0.010(8) 0.011(8) C11 0.049(8) 0.103(12) 0.059(8) 0.008(8) 0.021(7) 0.017(8) C12 0.078(9) 0.097(12) 0.064(9) -0.006(8) 0.030(8) 0.014(8) C13 0.072(10) 0.076(10) 0.050(7) 0.000(7) 0.013(7) 0.005(8) C14 0.076(10) 0.076(10) 0.059(8) 0.011(7) 0.020(8) -0.007(8) C15 0.067(9) 0.079(10) 0.064(8) -0.009(7) 0.028(8) -0.018(8) C16 0.093(13) 0.086(12) 0.079(11) -0.027(9) 0.020(10) -0.023(10) C17 0.107(15) 0.099(14) 0.080(12) -0.013(10) 0.026(11) -0.040(12) C18 0.14(2) 0.123(18) 0.089(14) 0.013(13) 0.023(14) -0.030(16) C19 0.069(9) 0.066(9) 0.049(7) -0.003(6) 0.016(7) -0.003(7) C20 0.075(10) 0.082(11) 0.058(8) -0.003(7) 0.019(8) 0.000(8) C21 0.119(16) 0.096(13) 0.062(9) -0.001(9) 0.027(10) 0.028(12) C23 0.098(14) 0.119(17) 0.103(14) -0.009(12) 0.061(13) 0.016(12) C24 0.14(2) 0.100(16) 0.110(16) 0.006(13) 0.059(16) 0.016(14) C27 0.133(10) 0.152(12) 0.156(12) -0.007(8) 0.080(9) -0.001(7) C30 0.212(19) 0.21(2) 0.22(2) 0.002(10) 0.083(11) -0.007(10) C22 0.077(15) 0.098(18) 0.089(16) 0.006(13) 0.046(13) -0.009(13) C25 0.11(3) 0.19(4) 0.15(4) -0.05(3) 0.09(3) -0.03(3) C26 0.14(4) 0.16(4) 0.15(4) -0.06(3) 0.07(3) -0.06(3) C22A 0.077(15) 0.098(18) 0.089(16) 0.006(13) 0.046(13) -0.009(13) U2 0.0624(4) 0.0721(4) 0.0518(3) 0.0023(2) 0.0168(3) -0.0015(2) O8 0.086(8) 0.086(8) 0.058(6) 0.000(5) 0.034(6) 0.014(6) O9 0.078(7) 0.093(8) 0.072(7) -0.005(6) 0.039(6) 0.009(6) O10 0.079(7) 0.067(6) 0.047(5) 0.004(4) 0.019(5) -0.003(5) O11 0.069(7) 0.089(8) 0.061(6) -0.005(6) 0.013(5) -0.008(6) O12 0.082(8) 0.099(8) 0.051(6) 0.007(5) 0.029(5) 0.006(6) O13 0.085(8) 0.100(8) 0.057(6) 0.001(6) 0.034(6) -0.018(6) O14 0.077(7) 0.076(7) 0.065(6) -0.001(5) 0.028(6) -0.005(6) O15 0.095(8) 0.085(8) 0.060(6) -0.001(6) 0.008(6) -0.017(6) N6 0.065(8) 0.060(7) 0.062(7) 0.009(6) 0.017(6) 0.012(6) N7 0.072(8) 0.076(9) 0.064(8) 0.003(7) 0.019(7) -0.003(7) O17 0.08(2) 0.06(2) 0.064(14) 0.011(16) 0.024(14) 0.020(14) O20 0.08(2) 0.06(2) 0.048(12) -0.003(15) 0.010(14) -0.002(14) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O5 63.1(4) . . ? O1 U1 O6 114.0(4) . . ? O1 U1 N1 61.4(4) . . ? O1 U1 N2 122.2(4) . . ? O2 U1 O1 173.5(4) . . ? O2 U1 O5 114.9(4) . . ? O2 U1 O6 63.9(4) . . ? O2 U1 N1 121.4(4) . . ? O2 U1 N2 60.6(4) . . ? O3 U1 O1 91.7(4) . . ? O3 U1 O2 94.4(4) . . ? O3 U1 O4 178.4(5) . . ? O3 U1 O5 88.3(4) . . ? O3 U1 O6 89.8(5) . . ? O3 U1 N1 84.6(4) . . ? O3 U1 N2 85.7(4) . . ? O4 U1 O1 87.8(5) . . ? O4 U1 O2 86.1(5) . . ? O4 U1 O5 92.8(4) . . ? O4 U1 O6 91.8(5) . . ? O4 U1 N1 93.8(4) . . ? O4 U1 N2 93.2(5) . . ? O5 U1 N1 123.7(4) . . ? O5 U1 N2 172.1(3) . . ? O6 U1 O5 51.0(4) . . ? O6 U1 N1 172.6(4) . . ? O6 U1 N2 123.7(4) . . ? N1 U1 N2 60.8(4) . . ? C1 O1 U1 122.9(10) . . ? C12 O2 U1 127.0(11) . . ? N5 O5 U1 96.1(10) . . ? N5 O6 U1 96.7(9) . . ? C2 N1 U1 120.1(10) . . ? C2 N1 C6 116.5(13) . . ? C6 N1 U1 122.3(9) . . ? C7 N2 U1 119.6(9) . . ? C11 N2 U1 120.2(10) . . ? C11 N2 C7 116.8(13) . . ? C1 N3 C15 117.9(13) . . ? C1 N3 C19 125.5(13) . . ? C19 N3 C15 115.5(12) . . ? C12 N4 C23 126.4(19) . . ? C12 N4 C27 118(2) . . ? C27 N4 C23 112.0(18) . . ? O5 N5 U1 58.2(8) . . ? O6 N5 U1 57.9(8) . . ? O6 N5 O5 115.9(14) . . ? O7 N5 U1 176.2(13) . . ? O7 N5 O5 122.0(16) . . ? O7 N5 O6 122.0(15) . . ? O1 C1 N3 122.7(14) . . ? O1 C1 C2 112.7(12) . . ? N3 C1 C2 124.3(13) . . ? N1 C2 C1 111.7(13) . . ? N1 C2 C3 123.5(14) . . ? C3 C2 C1 124.7(13) . . ? C2 C3 H3 120.8 . . ? C4 C3 C2 118.4(15) . . ? C4 C3 H3 120.8 . . ? C3 C4 Cl1 119.0(14) . . ? C3 C4 C5 119.9(15) . . ? C5 C4 Cl1 121.2(14) . . ? C4 C5 C14 124.1(15) . . ? C6 C5 C4 116.7(15) . . ? C6 C5 C14 119.2(14) . . ? N1 C6 C7 114.3(13) . . ? C5 C6 N1 125.0(14) . . ? C5 C6 C7 120.7(14) . . ? N2 C7 C6 117.0(13) . . ? N2 C7 C8 124.6(13) . . ? C8 C7 C6 118.3(14) . . ? C9 C8 C7 113.2(15) . . ? C9 C8 C13 129.1(15) . . ? C13 C8 C7 117.7(14) . . ? C8 C9 Cl2 117.5(13) . . ? C10 C9 Cl2 118.1(12) . . ? C10 C9 C8 124.5(15) . . ? C9 C10 H10 121.4 . . ? C9 C10 C11 117.2(15) . . ? C11 C10 H10 121.4 . . ? N2 C11 C10 123.7(16) . . ? N2 C11 C12 108.7(15) . . ? C10 C11 C12 127.5(16) . . ? O2 C12 N4 123(2) . . ? O2 C12 C11 113.4(15) . . ? N4 C12 C11 123.3(19) . . ? C8 C13 H13 118.7 . . ? C14 C13 C8 122.6(16) . . ? C14 C13 H13 118.7 . . ? C5 C14 H14 119.3 . . ? C13 C14 C5 121.4(16) . . ? C13 C14 H14 119.3 . . ? N3 C15 H15A 110.0 . . ? N3 C15 H15B 110.0 . . ? N3 C15 C16 108.7(13) . . ? H15A C15 H15B 108.3 . . ? C16 C15 H15A 110.0 . . ? C16 C15 H15B 110.0 . . ? C15 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C17 C16 C15 111.5(16) . . ? C17 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C16 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C16 C17 C18 113.4(17) . . ? H17A C17 H17B 107.7 . . ? C18 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 108.5 . . ? N3 C19 H19B 108.5 . . ? N3 C19 C20 115.2(13) . . ? H19A C19 H19B 107.5 . . ? C20 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? C19 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? C19 C20 C21 111.8(14) . . ? H20A C20 H20B 107.9 . . ? C21 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C20 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C20 C21 H21C 107.5 . . ? C20 C21 H21D 107.5 . . ? H21A C21 H21B 107.9 . . ? H21C C21 H21D 107.0 . . ? C22 C21 C20 112.1(17) . . ? C22 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C22A C21 C20 119(2) . . ? C22A C21 H21C 107.5 . . ? C22A C21 H21D 107.5 . . ? N4 C23 H23A 108.8 . . ? N4 C23 H23B 108.8 . . ? N4 C23 C24 113.9(19) . . ? H23A C23 H23B 107.7 . . ? C24 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C23 C24 H24A 108.2 . . ? C23 C24 H24B 108.2 . . ? C23 C24 H24C 108.6 . . ? C23 C24 H24D 108.6 . . ? H24A C24 H24B 107.4 . . ? H24C C24 H24D 107.6 . . ? C25 C24 C23 116(2) . . ? C25 C24 H24A 108.2 . . ? C25 C24 H24B 108.2 . . ? C25A C24 C23 115(3) . . ? C25A C24 H24C 108.6 . . ? C25A C24 H24D 108.6 . . ? N4 C27 H27A 108.3 . . ? N4 C27 H27B 108.3 . . ? N4 C27 H27C 109.9 . . ? N4 C27 H27D 109.9 . . ? N4 C27 C28 116.1(16) . . ? N4 C27 C28A 109.0(14) . . ? H27A C27 H27B 107.4 . . ? H27C C27 H27D 108.3 . . ? C28 C27 H27A 108.3 . . ? C28 C27 H27B 108.3 . . ? C28A C27 H27C 109.9 . . ? C28A C27 H27D 109.9 . . ? H30D C30 H30E 109.5 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? C29A C30 H30D 109.5 . . ? C29A C30 H30E 109.5 . . ? C29A C30 H30F 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C25 H25A 110.1 . . ? C24 C25 H25B 110.1 . . ? C24 C25 C26 108(3) . . ? H25A C25 H25B 108.4 . . ? C26 C25 H25A 110.1 . . ? C26 C25 H25B 110.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C29 C28 C27 111.2(15) . . ? C29 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C30 C29 H29C 109.4 . . ? C30 C29 H29D 109.4 . . ? C28 C29 C30 111.2(15) . . ? C28 C29 H29C 109.4 . . ? C28 C29 H29D 109.4 . . ? H29C C29 H29D 108.0 . . ? C21 C22A H22D 109.5 . . ? C21 C22A H22E 109.5 . . ? C21 C22A H22F 109.5 . . ? H22D C22A H22E 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C24 C25A H25C 109.5 . . ? C24 C25A H25D 109.5 . . ? H25C C25A H25D 108.1 . . ? C26A C25A C24 111(4) . . ? C26A C25A H25C 109.5 . . ? C26A C25A H25D 109.5 . . ? C25A C26A H26D 109.5 . . ? C25A C26A H26E 109.5 . . ? C25A C26A H26F 109.5 . . ? H26D C26A H26E 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C27 C28A H28C 109.1 . . ? C27 C28A H28D 109.1 . . ? H28C C28A H28D 107.8 . . ? C29A C28A C27 113(3) . . ? C29A C28A H28C 109.1 . . ? C29A C28A H28D 109.1 . . ? C30 C29A C28A 106.4(16) . . ? C30 C29A H29A 110.5 . . ? C30 C29A H29B 110.5 . . ? C28A C29A H29A 110.5 . . ? C28A C29A H29B 110.5 . . ? H29A C29A H29B 108.6 . . ? O8 U2 O10 86.3(4) . . ? O8 U2 O11 87.3(5) . . ? O8 U2 O13 90.3(5) . . ? O8 U2 O14 91.7(4) . . ? O8 U2 O16 82.7(8) . . ? O8 U2 O17 84.8(8) . . ? O8 U2 O19 96.3(8) . . ? O8 U2 O20 98.3(8) . . ? O9 U2 O8 178.0(5) . . ? O9 U2 O10 92.6(4) . . ? O9 U2 O11 90.7(5) . . ? O9 U2 O13 88.8(5) . . ? O9 U2 O14 89.2(5) . . ? O9 U2 O16 98.5(7) . . ? O9 U2 O17 97.2(8) . . ? O9 U2 O19 84.9(8) . . ? O9 U2 O20 83.8(8) . . ? O10 U2 O14 173.9(4) . . ? O10 U2 O19 69.5(7) . . ? O11 U2 O10 51.4(4) . . ? O11 U2 O14 122.8(4) . . ? O11 U2 O19 120.5(7) . . ? O13 U2 O10 122.6(3) . . ? O13 U2 O11 71.2(4) . . ? O13 U2 O14 51.6(3) . . ? O13 U2 O19 166.7(7) . . ? O16 U2 O10 66.0(6) . . ? O16 U2 O11 117.1(7) . . ? O16 U2 O13 168.7(7) . . ? O16 U2 O14 119.5(6) . . ? O17 U2 O10 117.7(11) . . ? O17 U2 O11 167.1(9) . . ? O17 U2 O13 118.9(11) . . ? O17 U2 O14 67.7(11) . . ? O17 U2 O16 51.8(12) . . ? O19 U2 O14 116.5(7) . . ? O20 U2 O10 122.2(9) . . ? O20 U2 O11 171.5(9) . . ? O20 U2 O13 114.9(9) . . ? O20 U2 O14 63.7(9) . . ? O20 U2 O19 52.7(11) . . ? N6 O10 U2 97.0(8) . . ? N6 O11 U2 97.4(9) . . ? N7 O13 U2 96.9(9) . . ? N7 O14 U2 96.3(9) . . ? O10 N6 U2 57.1(7) . . ? O11 N6 U2 57.0(8) . . ? O11 N6 O10 114.1(12) . . ? O12 N6 U2 178.7(11) . . ? O12 N6 O10 121.9(13) . . ? O12 N6 O11 124.0(14) . . ? O13 N7 U2 57.2(8) . . ? O14 N7 U2 58.0(7) . . ? O14 N7 O13 115.1(13) . . ? O15 N7 U2 176.3(12) . . ? O15 N7 O13 122.9(15) . . ? O15 N7 O14 122.0(14) . . ? N8 O16 U2 97(2) . . ? N8 O17 U2 96(3) . . ? O16 N8 U2 57.8(18) . . ? O16 N8 O17 115(4) . . ? O17 N8 U2 57(2) . . ? O18 N8 U2 173(3) . . ? O18 N8 O16 124(4) . . ? O18 N8 O17 120(4) . . ? N9 O19 U2 94(2) . . ? N9 O20 U2 95(3) . . ? O19 N9 U2 59.4(19) . . ? O19 N9 O20 117(4) . . ? O20 N9 U2 58(2) . . ? O21 N9 U2 178(3) . . ? O21 N9 O19 120(4) . . ? O21 N9 O20 123(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.436(11) . ? U1 O2 2.410(11) . ? U1 O3 1.771(10) . ? U1 O4 1.773(10) . ? U1 O5 2.502(12) . ? U1 O6 2.496(11) . ? U1 N1 2.599(13) . ? U1 N2 2.618(11) . ? Cl1 C4 1.723(16) . ? Cl2 C9 1.746(16) . ? O1 C1 1.280(17) . ? O2 C12 1.26(2) . ? O5 N5 1.277(18) . ? O6 N5 1.263(18) . ? O7 N5 1.228(18) . ? N1 C2 1.318(18) . ? N1 C6 1.369(19) . ? N2 C7 1.367(19) . ? N2 C11 1.35(2) . ? N3 C1 1.301(18) . ? N3 C15 1.52(2) . ? N3 C19 1.441(18) . ? N4 C12 1.27(2) . ? N4 C23 1.49(3) . ? N4 C27 1.439(10) . ? C1 C2 1.50(2) . ? C2 C3 1.39(2) . ? C3 H3 0.9500 . ? C3 C4 1.37(2) . ? C4 C5 1.40(2) . ? C5 C6 1.35(2) . ? C5 C14 1.43(2) . ? C6 C7 1.45(2) . ? C7 C8 1.44(2) . ? C8 C9 1.40(2) . ? C8 C13 1.40(2) . ? C9 C10 1.36(2) . ? C10 H10 0.9500 . ? C10 C11 1.40(2) . ? C11 C12 1.51(3) . ? C13 H13 0.9500 . ? C13 C14 1.33(2) . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.55(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.548(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.55(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.51(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.58(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C21 C22 1.525(14) . ? C21 C22A 1.563(19) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.54(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9900 . ? C24 H24D 0.9900 . ? C24 C25 1.536(10) . ? C24 C25A 1.535(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 H27C 0.9900 . ? C27 H27D 0.9900 . ? C27 C28 1.539(10) . ? C27 C28A 1.552(10) . ? C30 H30D 0.9800 . ? C30 H30E 0.9800 . ? C30 H30F 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 C29 1.549(10) . ? C30 C29A 1.537(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.538(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C29 1.536(10) . ? C29 H29C 0.9900 . ? C29 H29D 0.9900 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C25A C26A 1.53(2) . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C28A H28C 0.9900 . ? C28A H28D 0.9900 . ? C28A C29A 1.54(2) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? U2 O8 1.753(11) . ? U2 O9 1.746(12) . ? U2 O10 2.463(9) . ? U2 O11 2.463(12) . ? U2 O13 2.462(12) . ? U2 O14 2.481(11) . ? U2 O16 2.46(2) . ? U2 O17 2.45(5) . ? U2 O19 2.46(3) . ? U2 O20 2.43(5) . ? O10 N6 1.279(16) . ? O11 N6 1.268(16) . ? O12 N6 1.213(16) . ? O13 N7 1.280(17) . ? O14 N7 1.269(17) . ? O15 N7 1.212(17) . ? O16 N8 1.26(4) . ? O17 N8 1.28(6) . ? O18 N8 1.21(4) . ? O19 N9 1.26(4) . ? O20 N9 1.28(5) . ? O21 N9 1.25(4) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 O1 C1 N3 133.8(13) . . . . ? U1 O1 C1 C2 -40.4(16) . . . . ? U1 O2 C12 N4 -141.8(16) . . . . ? U1 O2 C12 C11 36(2) . . . . ? U1 O5 N5 O6 -4.8(14) . . . . ? U1 O5 N5 O7 175.6(15) . . . . ? U1 O6 N5 O5 4.8(14) . . . . ? U1 O6 N5 O7 -175.5(15) . . . . ? U1 N1 C2 C1 -12.5(16) . . . . ? U1 N1 C2 C3 163.2(11) . . . . ? U1 N1 C6 C5 -163.1(12) . . . . ? U1 N1 C6 C7 16.4(16) . . . . ? U1 N2 C7 C6 -22.0(16) . . . . ? U1 N2 C7 C8 160.4(10) . . . . ? U1 N2 C11 C10 -158.9(12) . . . . ? U1 N2 C11 C12 20.1(15) . . . . ? Cl1 C4 C5 C6 179.1(12) . . . . ? Cl1 C4 C5 C14 -1(2) . . . . ? Cl2 C9 C10 C11 176.9(11) . . . . ? O1 C1 C2 N1 32.4(18) . . . . ? O1 C1 C2 C3 -143.2(15) . . . . ? N1 C2 C3 C4 3(2) . . . . ? N1 C6 C7 N2 4.0(18) . . . . ? N1 C6 C7 C8 -178.2(12) . . . . ? N2 C7 C8 C9 -3(2) . . . . ? N2 C7 C8 C13 178.3(13) . . . . ? N2 C11 C12 O2 -33.6(19) . . . . ? N2 C11 C12 N4 144.1(18) . . . . ? N3 C1 C2 N1 -141.7(15) . . . . ? N3 C1 C2 C3 43(2) . . . . ? N3 C15 C16 C17 -179.7(13) . . . . ? N3 C19 C20 C21 175.6(14) . . . . ? N4 C23 C24 C25 66(4) . . . . ? N4 C23 C24 C25A 179(4) . . . . ? N4 C27 C28 C29 97(4) . . . . ? N4 C27 C28A C29A -165(5) . . . . ? C1 N3 C15 C16 -83.7(17) . . . . ? C1 N3 C19 C20 -114.0(17) . . . . ? C1 C2 C3 C4 178.3(14) . . . . ? C2 N1 C6 C5 5(2) . . . . ? C2 N1 C6 C7 -175.9(12) . . . . ? C2 C3 C4 Cl1 -179.4(12) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C3 C4 C5 C14 -179.9(15) . . . . ? C4 C5 C6 N1 -3(2) . . . . ? C4 C5 C6 C7 178.0(14) . . . . ? C4 C5 C14 C13 -179.7(16) . . . . ? C5 C6 C7 N2 -176.5(13) . . . . ? C5 C6 C7 C8 1(2) . . . . ? C6 N1 C2 C1 179.5(12) . . . . ? C6 N1 C2 C3 -5(2) . . . . ? C6 C5 C14 C13 0(2) . . . . ? C6 C7 C8 C9 179.5(12) . . . . ? C6 C7 C8 C13 0.7(19) . . . . ? C7 N2 C11 C10 0(2) . . . . ? C7 N2 C11 C12 179.3(13) . . . . ? C7 C8 C9 Cl2 -175.8(10) . . . . ? C7 C8 C9 C10 4(2) . . . . ? C7 C8 C13 C14 -3(2) . . . . ? C8 C9 C10 C11 -3(2) . . . . ? C8 C13 C14 C5 2(2) . . . . ? C9 C8 C13 C14 178.9(15) . . . . ? C9 C10 C11 N2 0(2) . . . . ? C9 C10 C11 C12 -178.4(15) . . . . ? C10 C11 C12 O2 145.3(16) . . . . ? C10 C11 C12 N4 -37(3) . . . . ? C11 N2 C7 C6 178.7(12) . . . . ? C11 N2 C7 C8 1(2) . . . . ? C12 N4 C23 C24 104(3) . . . . ? C12 N4 C27 C28 62(3) . . . . ? C12 N4 C27 C28A 101(4) . . . . ? C13 C8 C9 Cl2 3(2) . . . . ? C13 C8 C9 C10 -177.6(15) . . . . ? C14 C5 C6 N1 177.9(14) . . . . ? C14 C5 C6 C7 -2(2) . . . . ? C15 N3 C1 O1 5(2) . . . . ? C15 N3 C1 C2 178.1(13) . . . . ? C15 N3 C19 C20 78.1(17) . . . . ? C15 C16 C17 C18 -59(2) . . . . ? C19 N3 C1 O1 -163.1(15) . . . . ? C19 N3 C1 C2 10(2) . . . . ? C19 N3 C15 C16 85.2(16) . . . . ? C19 C20 C21 C22 -76(2) . . . . ? C19 C20 C21 C22A -171(3) . . . . ? C23 N4 C12 O2 170.1(19) . . . . ? C23 N4 C12 C11 -7(3) . . . . ? C23 N4 C27 C28 -98(3) . . . . ? C23 N4 C27 C28A -59(4) . . . . ? C23 C24 C25 C26 176(4) . . . . ? C23 C24 C25A C26A 179(4) . . . . ? C27 N4 C12 O2 13(3) . . . . ? C27 N4 C12 C11 -164.3(17) . . . . ? C27 N4 C23 C24 -98(2) . . . . ? C27 C28 C29 C30 154(5) . . . . ? C27 C28A C29A C30 165(6) . . . . ? U2 O10 N6 O11 -1.0(12) . . . . ? U2 O10 N6 O12 179.0(11) . . . . ? U2 O11 N6 O10 1.0(12) . . . . ? U2 O11 N6 O12 -179.0(12) . . . . ? U2 O13 N7 O14 -2.8(14) . . . . ? U2 O13 N7 O15 175.6(14) . . . . ? U2 O14 N7 O13 2.7(14) . . . . ? U2 O14 N7 O15 -175.7(13) . . . . ? U2 O16 N8 O17 3(4) . . . . ? U2 O16 N8 O18 172(4) . . . . ? U2 O17 N8 O16 -3(4) . . . . ? U2 O17 N8 O18 -172(3) . . . . ? U2 O19 N9 O20 0(4) . . . . ? U2 O19 N9 O21 178(4) . . . . ? U2 O20 N9 O19 0(4) . . . . ? U2 O20 N9 O21 -178(4) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.500 263.7 80.7 ? 2 0.000 0.389 0.281 7.3 0.0 ? 3 0.000 0.611 0.719 7.3 0.0 ? 4 0.500 0.500 0.000 263.7 80.7 ? 5 0.500 0.111 0.781 7.3 0.0 ? 6 0.500 0.889 0.219 7.3 0.0 ?