#------------------------------------------------------------------------------ #$Date: 2026-06-05 00:35:36 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306222 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721095.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_7721095 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 'C42 H44 Cl2 N8 O14 Th, C H2 Cl, 1[C2H4Cl2]' _chemical_formula_sum 'C43 H46 Cl3 N8 O14 Th' _chemical_formula_weight 1237.27 _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 2025-10-27 _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 99.142(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.1106(8) _cell_length_b 25.9428(18) _cell_length_c 16.7328(11) _cell_measurement_reflns_used 7815 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 25.674 _cell_measurement_theta_min 2.317 _cell_volume 5190.4(6) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'APEX3 v.2017.3_0 (Bruker AXS, 2017)' _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 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_unetI/netI 0.0820 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 30699 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.997 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_min 1.875 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_target Mo _diffrn_source_type 'fine-focus sealed X-ray tube' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 3.096 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1183 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.6973. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.583 _exptl_crystal_description block _exptl_crystal_F_000 2452 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.114 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.147 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 624 _refine_ls_number_reflns 9142 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0426 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.0836 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6508 _reflns_number_total 9142 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00392c2.cif _cod_data_source_block uth6 _cod_database_code 7721095 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.886 _shelx_estimated_absorpt_t_min 0.428 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid body (RIGU) restrains O2, N4, C13, C14 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Ternary CH refined with riding coordinates: C21(H21), C35(H35) 3.b Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A, H25B), C26(H26A,H26B), C29(H29A,H29B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C43(H43A,H43B) 3.c Aromatic/amide H refined with riding coordinates: C3(H3), C9(H9), C10(H10), C12(H12), C18(H18), C19(H19), C27(H27), C28(H28), C32(H32), C33(H33), C41(H41), C42(H42) 3.d Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C30(H30A,H30B,H30C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL uth6_a.res in P2(1)/n uth6.res created by SHELXL-2018/3 at 12:05:05 on 24-Oct-2025 REM Old TITL UTh6 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.115, Rweak 0.010, Alpha 0.075, Orientation as input REM Formula found by SHELXT: C45 N8 O16 Cl6 Th CELL 0.71073 12.1106 25.9428 16.7328 90 99.142 90 ZERR 4 0.0008 0.0018 0.0011 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl N O Th UNIT 172 184 12 32 56 4 RIGU O2 N4 C13 C14 L.S. 4 PLAN 8 SIZE 0.33 0.16 0.04 TEMP -173.15 CONF BOND $H list 4 MORE -1 ABIN fmap 2 acta OMIT -2 50 OMIT 0 1 1 REM REM REM WGHT 0.031700 FVAR 0.20311 TH1 6 0.238440 0.472647 0.730069 11.00000 0.01321 0.01593 = 0.01401 -0.00030 0.00165 -0.00054 CL1 3 0.444622 0.383963 0.374888 11.00000 0.03044 0.02898 = 0.02259 -0.00156 0.01361 0.00482 CL2 3 0.821075 0.515185 0.714426 11.00000 0.01360 0.04278 = 0.04544 0.00940 0.00178 -0.00711 O1 5 0.111053 0.456885 0.602938 11.00000 0.01551 0.01393 = 0.01509 -0.00209 0.00667 -0.00268 O2 5 0.373274 0.493023 0.851235 11.00000 0.01464 0.02003 = 0.01731 0.00019 -0.00239 -0.00738 O3 5 0.216131 0.375230 0.692961 11.00000 0.01015 0.01991 = 0.02283 0.00186 -0.00028 -0.00034 O4 5 0.379754 0.397867 0.755031 11.00000 0.01382 0.01324 = 0.02949 0.00434 0.00462 0.00115 O5 5 0.357309 0.321925 0.698805 11.00000 0.03240 0.01652 = 0.05992 -0.01141 0.01291 0.00808 O6 5 0.057605 0.431210 0.758724 11.00000 0.01886 0.02242 = 0.01114 0.00191 -0.00083 0.00374 O7 5 0.204025 0.418479 0.848808 11.00000 0.01129 0.03032 = 0.01196 -0.00075 -0.00077 -0.00300 O8 5 0.044655 0.382947 0.862409 11.00000 0.02248 0.04840 = 0.02210 0.01386 0.00651 -0.01282 O9 5 0.076589 0.536827 0.709646 11.00000 0.01859 0.02202 = 0.01746 -0.00513 0.00356 0.00139 O10 5 0.147635 0.523276 0.834503 11.00000 0.02025 0.02923 = 0.01591 -0.00277 -0.00054 0.00193 O11 5 0.021400 0.582748 0.805805 11.00000 0.03577 0.03100 = 0.03316 -0.01057 0.00759 0.01234 O12 5 0.298110 0.570515 0.743949 11.00000 0.01500 0.02689 = 0.01458 0.00514 -0.00026 0.00355 O13 5 0.258080 0.542111 0.621740 11.00000 0.01840 0.02007 = 0.01478 -0.00208 0.00656 0.00024 O14 5 0.289469 0.623910 0.641345 11.00000 0.03510 0.01152 = 0.02842 0.00336 0.00821 -0.00142 N1 4 0.320361 0.443977 0.596399 11.00000 0.01297 0.01120 = 0.02150 0.00322 0.00556 -0.00442 N2 4 0.455768 0.490621 0.718558 11.00000 0.00749 0.01976 = 0.01973 0.00238 -0.00237 -0.00053 N3 4 0.051779 0.396876 0.508959 11.00000 0.01599 0.01725 = 0.01984 -0.00156 0.00395 -0.00135 N4 4 0.487410 0.555574 0.907847 11.00000 0.02110 0.02118 = 0.02013 0.00242 -0.00199 -0.00931 N5 4 0.318279 0.362968 0.714894 11.00000 0.03311 0.02456 = 0.01414 -0.00162 0.00739 -0.00268 N6 4 0.098928 0.409787 0.825098 11.00000 0.02239 0.02635 = 0.02012 -0.00023 0.00111 0.00289 N7 4 0.079530 0.548755 0.784834 11.00000 0.01911 0.02271 = 0.02042 -0.00251 -0.00239 -0.00027 N8 4 0.281797 0.581217 0.668861 11.00000 0.01381 0.01889 = 0.02663 -0.00335 0.00342 0.00411 C1 1 0.130645 0.425085 0.550177 11.00000 0.01487 0.01557 = 0.01336 0.00382 0.00247 0.00126 C2 1 0.251060 0.423124 0.535172 11.00000 0.01536 0.01084 = 0.01871 0.00067 0.00683 -0.00118 C3 1 0.286352 0.405472 0.464740 11.00000 0.02002 0.01914 = 0.01684 0.00323 0.00072 0.00198 AFIX 43 H3 2 0.234466 0.392059 0.421140 11.00000 -1.20000 AFIX 0 C4 1 0.398962 0.408077 0.460293 11.00000 0.02061 0.01340 = 0.01965 0.00479 0.00976 0.00491 C5 1 0.474227 0.430209 0.522146 11.00000 0.01509 0.01603 = 0.02270 0.00630 0.00424 0.00822 C6 1 0.430184 0.448620 0.589944 11.00000 0.01532 0.00767 = 0.01413 0.00017 0.00299 -0.00028 C7 1 0.501586 0.473398 0.654900 11.00000 0.01427 0.01769 = 0.01806 0.00623 -0.00261 0.00142 C8 1 0.616034 0.479559 0.650015 11.00000 0.01368 0.01644 = 0.02186 0.00921 0.00065 0.00130 C9 1 0.658481 0.460432 0.581453 11.00000 0.01196 0.01551 = 0.02996 0.00236 0.00111 0.00001 AFIX 43 H9 2 0.735648 0.464703 0.578539 11.00000 -1.20000 AFIX 0 C10 1 0.592869 0.436579 0.520882 11.00000 0.02312 0.01523 = 0.02847 0.00872 0.01159 0.00656 AFIX 43 H10 2 0.624378 0.423625 0.476410 11.00000 -1.20000 AFIX 0 C11 1 0.682003 0.504113 0.715831 11.00000 0.01314 0.02201 = 0.03307 0.00618 0.00419 0.00225 C12 1 0.635249 0.519938 0.782340 11.00000 0.01251 0.01951 = 0.02503 0.00537 -0.01021 -0.00721 AFIX 43 H12 2 0.679792 0.535927 0.827409 11.00000 -1.20000 AFIX 0 C13 1 0.521307 0.511762 0.781271 11.00000 0.01977 0.01343 = 0.01848 0.00449 0.00008 0.00185 C14 1 0.457361 0.521143 0.850875 11.00000 0.01631 0.02917 = 0.00922 0.00334 -0.00709 -0.00669 C15 1 -0.064657 0.404178 0.522392 11.00000 0.01337 0.03020 = 0.02223 -0.00757 -0.00084 0.00095 AFIX 23 H15A 2 -0.116034 0.397983 0.471092 11.00000 -1.20000 H15B 2 -0.074983 0.440226 0.539159 11.00000 -1.20000 AFIX 0 C16 1 -0.094199 0.367269 0.587936 11.00000 0.01781 0.03964 = 0.03935 0.00050 0.00862 -0.00677 AFIX 137 H16A 2 -0.086812 0.331545 0.570494 11.00000 -1.50000 H16B 2 -0.171347 0.373524 0.596300 11.00000 -1.50000 H16C 2 -0.043235 0.373255 0.638717 11.00000 -1.50000 AFIX 0 C17 1 0.073365 0.352970 0.461344 11.00000 0.01978 0.01411 = 0.01549 -0.00652 0.00570 -0.00189 C18 1 0.131400 0.311289 0.499792 11.00000 0.02071 0.01820 = 0.02346 0.00145 -0.00010 -0.00580 AFIX 43 H18 2 0.154781 0.311377 0.556741 11.00000 -1.20000 AFIX 0 C19 1 0.154317 0.269810 0.453515 11.00000 0.01758 0.02040 = 0.02402 0.00506 -0.00068 0.00507 AFIX 43 H19 2 0.194597 0.241363 0.479353 11.00000 -1.20000 AFIX 0 C20 1 0.120289 0.268397 0.370351 11.00000 0.01534 0.01947 = 0.01820 -0.00072 0.00159 -0.00174 C21 1 0.152475 0.224265 0.318870 11.00000 0.03008 0.01313 = 0.01349 -0.00396 0.00185 0.00795 AFIX 13 H21 2 0.116205 0.230768 0.261801 11.00000 -1.20000 AFIX 0 C22 1 0.111633 0.171635 0.344071 11.00000 0.01612 0.02461 = 0.02601 -0.00188 -0.00134 -0.00096 AFIX 23 H22A 2 0.144084 0.164579 0.401124 11.00000 -1.20000 H22B 2 0.029194 0.172201 0.340027 11.00000 -1.20000 AFIX 0 C23 1 0.145513 0.129009 0.290150 11.00000 0.02476 0.01889 = 0.04460 -0.00879 0.00425 0.00231 AFIX 23 H23A 2 0.122668 0.095279 0.309865 11.00000 -1.20000 H23B 2 0.105503 0.133901 0.234308 11.00000 -1.20000 AFIX 0 C24 1 0.270824 0.128451 0.288931 11.00000 0.02410 0.02898 = 0.02992 -0.00331 0.00698 0.00316 AFIX 23 H24A 2 0.310721 0.119322 0.343392 11.00000 -1.20000 H24B 2 0.288271 0.101841 0.250403 11.00000 -1.20000 AFIX 0 C25 1 0.311431 0.180642 0.264194 11.00000 0.02226 0.02877 = 0.02899 -0.00822 0.00140 0.00264 AFIX 23 H25A 2 0.277660 0.188221 0.207584 11.00000 -1.20000 H25B 2 0.393707 0.179870 0.267125 11.00000 -1.20000 AFIX 0 C26 1 0.279518 0.222778 0.319768 11.00000 0.02486 0.01665 = 0.02390 -0.00335 0.00140 -0.00777 AFIX 23 H26A 2 0.304812 0.256584 0.302024 11.00000 -1.20000 H26B 2 0.317855 0.216466 0.375697 11.00000 -1.20000 AFIX 0 C27 1 0.062277 0.310519 0.334719 11.00000 0.01475 0.02677 = 0.02568 -0.00598 0.00065 -0.00198 AFIX 43 H27 2 0.039361 0.310599 0.277722 11.00000 -1.20000 AFIX 0 C28 1 0.036453 0.352471 0.379000 11.00000 0.01919 0.02594 = 0.01649 -0.00180 -0.00665 -0.00093 AFIX 43 H28 2 -0.005843 0.380410 0.353314 11.00000 -1.20000 AFIX 0 C29 1 0.416475 0.563684 0.971437 11.00000 0.03536 0.03521 = 0.01789 -0.00450 0.00808 -0.01033 AFIX 23 H29A 2 0.464761 0.572541 1.023049 11.00000 -1.20000 H29B 2 0.376788 0.531237 0.979744 11.00000 -1.20000 AFIX 0 C30 1 0.332061 0.606043 0.949261 11.00000 0.05026 0.03275 = 0.03745 -0.01494 0.01211 -0.00647 AFIX 137 H30A 2 0.285014 0.597734 0.897655 11.00000 -1.50000 H30B 2 0.371129 0.638660 0.944086 11.00000 -1.50000 H30C 2 0.285131 0.609288 0.991617 11.00000 -1.50000 AFIX 0 C31 1 0.575690 0.593314 0.906020 11.00000 0.03039 0.01971 = 0.01380 0.00101 -0.00280 -0.01170 C32 1 0.566303 0.629673 0.844252 11.00000 0.02686 0.02738 = 0.01804 0.00236 -0.00873 -0.00719 AFIX 43 H32 2 0.502355 0.630198 0.803214 11.00000 -1.20000 AFIX 0 C33 1 0.651196 0.664913 0.843519 11.00000 0.04305 0.02573 = 0.01797 0.01012 -0.00147 -0.01161 AFIX 43 H33 2 0.644586 0.690015 0.801692 11.00000 -1.20000 AFIX 0 C34 1 0.746556 0.664785 0.902431 11.00000 0.03149 0.02272 = 0.01790 0.00038 -0.00288 -0.01498 C35 1 0.837241 0.704147 0.900923 11.00000 0.03146 0.02958 = 0.00850 0.00017 0.00123 -0.01318 AFIX 13 H35 2 0.831374 0.716836 0.843973 11.00000 -1.20000 AFIX 0 C36 1 0.819589 0.750632 0.954045 11.00000 0.02666 0.01953 = 0.04682 -0.00228 0.00255 -0.00351 AFIX 23 H36A 2 0.822928 0.739110 1.010783 11.00000 -1.20000 H36B 2 0.744391 0.765345 0.935763 11.00000 -1.20000 AFIX 0 C37 1 0.908607 0.792598 0.950290 11.00000 0.03492 0.02457 = 0.04487 0.00004 -0.00973 -0.00274 AFIX 23 H37A 2 0.899072 0.807147 0.894924 11.00000 -1.20000 H37B 2 0.897455 0.820816 0.988033 11.00000 -1.20000 AFIX 0 C38 1 1.026971 0.771493 0.972381 11.00000 0.03030 0.03147 = 0.02217 -0.00171 -0.00712 -0.01261 AFIX 23 H38A 2 1.040503 0.761338 1.030143 11.00000 -1.20000 H38B 2 1.081680 0.798602 0.964328 11.00000 -1.20000 AFIX 0 C39 1 1.042969 0.724676 0.919549 11.00000 0.03709 0.04144 = 0.03080 -0.01211 0.00625 -0.01137 AFIX 23 H39A 2 1.037793 0.735755 0.862458 11.00000 -1.20000 H39B 2 1.118371 0.709939 0.936904 11.00000 -1.20000 AFIX 0 C40 1 0.955109 0.683618 0.925815 11.00000 0.03323 0.02108 = 0.05157 -0.01481 0.02038 -0.00578 AFIX 23 H40A 2 0.967191 0.654117 0.890681 11.00000 -1.20000 H40B 2 0.963679 0.670974 0.982287 11.00000 -1.20000 AFIX 0 C41 1 0.751241 0.629459 0.965301 11.00000 0.03102 0.02612 = 0.01657 0.00141 -0.00593 -0.01112 AFIX 43 H41 2 0.813730 0.629785 1.007547 11.00000 -1.20000 AFIX 0 C42 1 0.666191 0.593547 0.967701 11.00000 0.02897 0.02159 = 0.02235 -0.00015 -0.00463 -0.01345 AFIX 43 H42 2 0.670426 0.569624 1.011066 11.00000 -1.20000 AFIX 0 CL3 3 0.842416 0.476022 0.933976 11.00000 0.04100 0.04727 = 0.04943 0.00180 -0.01074 -0.00271 C43 1 0.950203 0.515510 0.987156 11.00000 0.04543 0.04293 = 0.03336 -0.00671 0.00091 0.00632 AFIX 23 H43A 2 0.967994 0.543790 0.951565 11.00000 -1.20000 H43B 2 0.924473 0.531006 1.035043 11.00000 -1.20000 AFIX 0 HKLF 4 REM uth6_a.res in P2(1)/n REM wR2 = 0.0836, GooF = S = 1.028, Restrained GooF = 1.028 for all data REM R1 = 0.0426 for 6508 Fo > 4sig(Fo) and 0.0731 for all 9142 data REM 624 parameters refined using 18 restraints END WGHT 0.0317 0.0000 REM Highest difference peak 1.114, deepest hole -1.261, 1-sigma level 0.147 Q1 1 0.1619 0.4766 0.6421 11.00000 0.05 1.11 Q2 1 0.2367 0.4380 0.8077 11.00000 0.05 0.88 Q3 1 0.2795 0.5274 0.7375 11.00000 0.05 0.87 Q4 1 0.1792 0.5222 0.7016 11.00000 0.05 0.84 Q5 1 0.1869 0.4207 0.7113 11.00000 0.05 0.82 Q6 1 0.3188 0.5013 0.7841 11.00000 0.05 0.74 Q7 1 0.3211 0.4756 0.8235 11.00000 0.05 0.72 Q8 1 0.3022 0.4429 0.7961 11.00000 0.05 0.71 ; _shelx_res_checksum 5993 _shelx_fab_file ; -15 0 1 5.2647 -3.5469 -15 0 3 -6.5761 5.2225 -15 0 5 3.4252 -5.5465 -15 1 1 1.9298 1.3701 -15 1 2 2.2600 4.8179 -15 1 3 7.8419 -1.0933 -15 1 4 -2.5627 -4.5951 -15 1 5 -7.3820 1.3030 -15 1 6 1.0441 5.1340 -15 2 1 -4.6287 2.2677 -15 2 2 3.1413 -1.9342 -15 2 3 6.7684 -4.2344 -15 2 4 -2.3425 2.1069 -15 2 5 -3.2770 3.5886 -15 3 2 -4.1864 -2.2233 -15 3 3 -3.5018 0.9367 -15 3 4 5.0947 2.2259 -15 3 5 4.2044 -0.8619 -15 4 2 -4.8835 1.6761 -15 4 3 -6.9839 1.5465 -15 4 4 2.9441 -1.5818 -14 0 -4 -0.9907 0.5514 -14 0 -2 -6.6690 -1.9048 -14 0 0 8.6236 4.4836 -14 0 2 0.5676 -6.6348 -14 0 4 -8.4698 8.4767 -14 0 6 14.9569 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-0.6508 9 9 12 -3.3199 0.0616 9 9 13 0.7465 0.5465 9 10 9 -6.9381 -0.5890 9 10 10 4.4273 -0.0401 9 10 11 7.3736 0.0250 9 10 12 -3.6720 0.3042 9 10 13 -7.0638 0.7822 9 11 9 1.8137 0.4511 9 11 10 4.2283 0.4103 9 11 11 -5.8155 -0.3323 9 11 12 2.8319 0.8773 9 11 13 -2.3447 -1.0759 9 12 9 6.1084 0.0303 9 12 10 -6.7522 -1.1274 9 12 11 -2.7795 0.1003 9 12 12 8.2933 0.9170 9 13 9 -3.1057 -0.7993 9 13 10 -6.6285 0.7093 9 13 11 5.7312 0.1454 9 13 12 -1.9079 -1.9725 9 14 9 -4.1520 0.5283 9 14 10 5.1966 1.7005 9 14 11 0.1147 -0.1867 9 14 12 -8.2035 -0.9755 9 15 9 3.6084 0.3661 9 15 10 7.1601 -1.3748 9 15 11 -5.0623 0.4349 9 16 9 3.4297 -0.2474 9 16 10 -2.2311 -1.7544 9 16 11 0.1218 0.1814 9 17 9 -3.3171 -0.5026 9 17 10 -5.2460 1.3544 9 18 9 -3.4579 -0.4918 9 18 10 0.3559 1.4689 9 19 9 2.2456 0.8314 10 0 10 -11.9418 2.3197 10 0 12 -1.5830 -5.5201 10 1 10 11.2468 -0.7243 10 1 11 0.5940 -6.6442 10 1 12 -2.5379 0.8757 10 1 13 1.5888 4.5641 10 2 10 10.2458 -0.9212 10 2 11 -1.4087 0.5662 10 2 12 0.6539 3.6150 10 2 13 -3.8345 -0.0732 10 3 10 -11.1493 1.9151 10 3 11 -0.1774 2.6154 10 3 12 3.4549 -1.0576 10 3 13 -3.3084 -2.2519 10 4 10 -5.3896 -0.1587 10 4 11 3.1469 -0.4950 10 4 12 -0.5136 -1.0194 10 4 13 3.8356 0.3512 10 5 10 8.1660 -0.1260 10 5 11 -1.9094 -0.2065 10 5 12 -3.0310 0.1670 10 5 13 2.2705 0.1239 10 6 10 -0.8523 0.4043 10 6 11 -3.7181 -0.4241 10 6 12 4.0073 -0.1910 10 7 10 -2.2002 -1.3845 10 7 11 2.1447 0.5200 10 7 12 1.2198 0.3902 10 8 10 5.0965 -0.4115 10 8 11 1.4984 1.1097 10 8 12 -8.1613 0.1291 10 9 10 -2.9827 0.6179 10 9 11 0.3143 -1.1421 10 9 12 -0.5634 -0.2367 10 10 10 -5.6744 0.5326 10 10 11 2.4938 -0.4988 10 11 10 4.7120 0.6334 10 11 11 -1.9549 0.5088 10 12 10 4.4580 -0.4762 10 12 11 -5.1752 -0.9523 10 13 10 -4.0683 -0.4585 10 14 10 -3.6526 0.0920 10 15 10 3.0786 -0.3504 11 0 11 1.3005 3.4497 11 1 11 -1.5282 -0.2305 11 2 11 -0.9472 -1.9728 11 3 11 -2.3568 0.4703 11 4 11 0.8960 0.4351 11 5 11 4.5321 0.6190 11 6 11 -2.1358 0.1620 11 7 11 -2.8735 -1.3329 0 0 0 0.0 0.0 ; _shelx_fab_checksum 9495 _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 Th1 Th 0.23844(2) 0.47265(2) 0.73007(2) 0.01444(7) Uani 1 1 d . . . . . Cl1 Cl 0.44462(13) 0.38396(6) 0.37489(9) 0.0263(4) Uani 1 1 d . . . . . Cl2 Cl 0.82107(13) 0.51518(6) 0.71443(11) 0.0343(5) Uani 1 1 d . . . . . O1 O 0.1111(3) 0.45689(13) 0.6029(2) 0.0144(9) Uani 1 1 d . . . . . O2 O 0.3733(3) 0.49302(14) 0.8512(2) 0.0179(9) Uani 1 1 d . . . . . O3 O 0.2161(3) 0.37523(14) 0.6930(2) 0.0179(9) Uani 1 1 d . . . . . O4 O 0.3798(3) 0.39787(14) 0.7550(2) 0.0187(10) Uani 1 1 d . . . . . O5 O 0.3573(4) 0.32193(16) 0.6988(3) 0.0357(13) Uani 1 1 d . . . . . O6 O 0.0576(3) 0.43121(14) 0.7587(2) 0.0178(10) Uani 1 1 d . . . . . O7 O 0.2040(3) 0.41848(15) 0.8488(2) 0.0181(10) Uani 1 1 d . . . . . O8 O 0.0447(3) 0.38295(17) 0.8624(3) 0.0307(12) Uani 1 1 d . . . . . O9 O 0.0766(3) 0.53683(14) 0.7096(2) 0.0193(10) Uani 1 1 d . . . . . O10 O 0.1476(3) 0.52328(16) 0.8345(2) 0.0222(10) Uani 1 1 d . . . . . O11 O 0.0214(4) 0.58275(16) 0.8058(3) 0.0331(12) Uani 1 1 d . . . . . O12 O 0.2981(3) 0.57052(15) 0.7439(2) 0.0191(10) Uani 1 1 d . . . . . O13 O 0.2581(3) 0.54211(14) 0.6217(2) 0.0173(10) Uani 1 1 d . . . . . O14 O 0.2895(3) 0.62391(15) 0.6413(2) 0.0247(11) Uani 1 1 d . . . . . N1 N 0.3204(4) 0.44398(17) 0.5964(3) 0.0149(11) Uani 1 1 d . . . . . N2 N 0.4558(4) 0.49062(17) 0.7186(3) 0.0162(12) Uani 1 1 d . . . . . N3 N 0.0518(4) 0.39688(17) 0.5090(3) 0.0176(12) Uani 1 1 d . . . . . N4 N 0.4874(4) 0.55557(18) 0.9078(3) 0.0214(12) Uani 1 1 d . . . . . N5 N 0.3183(4) 0.3630(2) 0.7149(3) 0.0235(13) Uani 1 1 d . . . . . N6 N 0.0989(4) 0.40979(19) 0.8251(3) 0.0232(13) Uani 1 1 d . . . . . N7 N 0.0795(4) 0.54876(19) 0.7848(3) 0.0213(13) Uani 1 1 d . . . . . N8 N 0.2818(4) 0.58122(19) 0.6689(3) 0.0198(12) Uani 1 1 d . . . . . C1 C 0.1306(5) 0.4251(2) 0.5502(3) 0.0146(13) Uani 1 1 d . . . . . C2 C 0.2511(5) 0.4231(2) 0.5352(4) 0.0145(13) Uani 1 1 d . . . . . C3 C 0.2864(5) 0.4055(2) 0.4647(4) 0.0189(14) Uani 1 1 d . . . . . H3 H 0.234466 0.392059 0.421140 0.023 Uiso 1 1 calc R U . . . C4 C 0.3990(5) 0.4081(2) 0.4603(4) 0.0172(14) Uani 1 1 d . . . . . C5 C 0.4742(5) 0.4302(2) 0.5221(4) 0.0178(14) Uani 1 1 d . . . . . C6 C 0.4302(5) 0.4486(2) 0.5899(3) 0.0123(13) Uani 1 1 d . . . . . C7 C 0.5016(4) 0.4734(2) 0.6549(3) 0.0172(13) Uani 1 1 d . . . . . C8 C 0.6160(5) 0.4796(2) 0.6500(4) 0.0176(14) Uani 1 1 d . . . . . C9 C 0.6585(5) 0.4604(2) 0.5815(4) 0.0194(15) Uani 1 1 d . . . . . H9 H 0.735648 0.464703 0.578539 0.023 Uiso 1 1 calc R U . . . C10 C 0.5929(5) 0.4366(2) 0.5209(4) 0.0215(15) Uani 1 1 d . . . . . H10 H 0.624378 0.423625 0.476410 0.026 Uiso 1 1 calc R U . . . C11 C 0.6820(5) 0.5041(2) 0.7158(4) 0.0227(15) Uani 1 1 d . . . . . C12 C 0.6352(5) 0.5199(2) 0.7823(4) 0.0204(15) Uani 1 1 d . . . . . H12 H 0.679792 0.535927 0.827409 0.025 Uiso 1 1 calc R U . . . C13 C 0.5213(5) 0.5118(2) 0.7813(4) 0.0175(14) Uani 1 1 d . . . . . C14 C 0.4574(5) 0.5211(2) 0.8509(3) 0.0192(14) Uani 1 1 d . . . . . C15 C -0.0647(5) 0.4042(2) 0.5224(4) 0.0223(15) Uani 1 1 d . . . . . H15A H -0.116034 0.397983 0.471092 0.027 Uiso 1 1 calc R U . . . H15B H -0.074983 0.440226 0.539159 0.027 Uiso 1 1 calc R U . . . C16 C -0.0942(5) 0.3673(2) 0.5879(4) 0.0318(17) Uani 1 1 d . . . . . H16A H -0.086812 0.331545 0.570494 0.048 Uiso 1 1 calc R U . . . H16B H -0.171347 0.373524 0.596300 0.048 Uiso 1 1 calc R U . . . H16C H -0.043235 0.373255 0.638717 0.048 Uiso 1 1 calc R U . . . C17 C 0.0734(5) 0.3530(2) 0.4613(4) 0.0161(14) Uani 1 1 d . . . . . C18 C 0.1314(5) 0.3113(2) 0.4998(4) 0.0212(15) Uani 1 1 d . . . . . H18 H 0.154781 0.311377 0.556741 0.025 Uiso 1 1 calc R U . . . C19 C 0.1543(5) 0.2698(2) 0.4535(4) 0.0211(15) Uani 1 1 d . . . . . H19 H 0.194597 0.241363 0.479353 0.025 Uiso 1 1 calc R U . . . C20 C 0.1203(5) 0.2684(2) 0.3704(4) 0.0178(14) Uani 1 1 d . . . . . C21 C 0.1525(5) 0.2243(2) 0.3189(4) 0.0191(15) Uani 1 1 d . . . . . H21 H 0.116205 0.230768 0.261801 0.023 Uiso 1 1 calc R U . . . C22 C 0.1116(5) 0.1716(2) 0.3441(4) 0.0228(16) Uani 1 1 d . . . . . H22A H 0.144084 0.164579 0.401124 0.027 Uiso 1 1 calc R U . . . H22B H 0.029194 0.172201 0.340027 0.027 Uiso 1 1 calc R U . . . C23 C 0.1455(5) 0.1290(2) 0.2902(4) 0.0296(17) Uani 1 1 d . . . . . H23A H 0.122668 0.095279 0.309865 0.035 Uiso 1 1 calc R U . . . H23B H 0.105503 0.133901 0.234308 0.035 Uiso 1 1 calc R U . . . C24 C 0.2708(5) 0.1285(2) 0.2889(4) 0.0274(17) Uani 1 1 d . . . . . H24A H 0.310721 0.119322 0.343392 0.033 Uiso 1 1 calc R U . . . H24B H 0.288271 0.101841 0.250403 0.033 Uiso 1 1 calc R U . . . C25 C 0.3114(5) 0.1806(2) 0.2642(4) 0.0270(16) Uani 1 1 d . . . . . H25A H 0.277660 0.188221 0.207584 0.032 Uiso 1 1 calc R U . . . H25B H 0.393707 0.179870 0.267125 0.032 Uiso 1 1 calc R U . . . C26 C 0.2795(5) 0.2228(2) 0.3198(4) 0.0221(15) Uani 1 1 d . . . . . H26A H 0.304812 0.256584 0.302024 0.026 Uiso 1 1 calc R U . . . H26B H 0.317855 0.216466 0.375697 0.026 Uiso 1 1 calc R U . . . C27 C 0.0623(5) 0.3105(2) 0.3347(4) 0.0227(15) Uani 1 1 d . . . . . H27 H 0.039361 0.310599 0.277722 0.027 Uiso 1 1 calc R U . . . C28 C 0.0365(5) 0.3525(2) 0.3790(4) 0.0216(15) Uani 1 1 d . . . . . H28 H -0.005843 0.380410 0.353314 0.026 Uiso 1 1 calc R U . . . C29 C 0.4165(5) 0.5637(2) 0.9714(4) 0.0291(17) Uani 1 1 d . . . . . H29A H 0.464761 0.572541 1.023049 0.035 Uiso 1 1 calc R U . . . H29B H 0.376788 0.531237 0.979744 0.035 Uiso 1 1 calc R U . . . C30 C 0.3321(6) 0.6060(2) 0.9493(4) 0.040(2) Uani 1 1 d . . . . . H30A H 0.285014 0.597734 0.897655 0.059 Uiso 1 1 calc R U . . . H30B H 0.371129 0.638660 0.944086 0.059 Uiso 1 1 calc R U . . . H30C H 0.285131 0.609288 0.991617 0.059 Uiso 1 1 calc R U . . . C31 C 0.5757(5) 0.5933(2) 0.9060(4) 0.0220(15) Uani 1 1 d . . . . . C32 C 0.5663(5) 0.6297(2) 0.8443(4) 0.0254(16) Uani 1 1 d . . . . . H32 H 0.502355 0.630198 0.803214 0.031 Uiso 1 1 calc R U . . . C33 C 0.6512(5) 0.6649(2) 0.8435(4) 0.0296(17) Uani 1 1 d . . . . . H33 H 0.644586 0.690015 0.801692 0.036 Uiso 1 1 calc R U . . . C34 C 0.7466(5) 0.6648(2) 0.9024(4) 0.0248(16) Uani 1 1 d . . . . . C35 C 0.8372(5) 0.7041(2) 0.9009(4) 0.0234(15) Uani 1 1 d . . . . . H35 H 0.831374 0.716836 0.843973 0.028 Uiso 1 1 calc R U . . . C36 C 0.8196(5) 0.7506(2) 0.9540(4) 0.0314(18) Uani 1 1 d . . . . . H36A H 0.822928 0.739110 1.010783 0.038 Uiso 1 1 calc R U . . . H36B H 0.744391 0.765345 0.935763 0.038 Uiso 1 1 calc R U . . . C37 C 0.9086(5) 0.7926(2) 0.9503(4) 0.0365(19) Uani 1 1 d . . . . . H37A H 0.899072 0.807147 0.894924 0.044 Uiso 1 1 calc R U . . . H37B H 0.897455 0.820816 0.988033 0.044 Uiso 1 1 calc R U . . . C38 C 1.0270(5) 0.7715(2) 0.9724(4) 0.0292(17) Uani 1 1 d . . . . . H38A H 1.040503 0.761338 1.030143 0.035 Uiso 1 1 calc R U . . . H38B H 1.081680 0.798602 0.964328 0.035 Uiso 1 1 calc R U . . . C39 C 1.0430(6) 0.7247(2) 0.9195(4) 0.0364(19) Uani 1 1 d . . . . . H39A H 1.037793 0.735755 0.862458 0.044 Uiso 1 1 calc R U . . . H39B H 1.118371 0.709939 0.936904 0.044 Uiso 1 1 calc R U . . . C40 C 0.9551(5) 0.6836(2) 0.9258(4) 0.0338(18) Uani 1 1 d . . . . . H40A H 0.967191 0.654117 0.890681 0.041 Uiso 1 1 calc R U . . . H40B H 0.963679 0.670974 0.982287 0.041 Uiso 1 1 calc R U . . . C41 C 0.7512(5) 0.6295(2) 0.9653(4) 0.0256(16) Uani 1 1 d . . . . . H41 H 0.813730 0.629785 1.007547 0.031 Uiso 1 1 calc R U . . . C42 C 0.6662(5) 0.5935(2) 0.9677(4) 0.0252(16) Uani 1 1 d . . . . . H42 H 0.670426 0.569624 1.011066 0.030 Uiso 1 1 calc R U . . . Cl3 Cl 0.84242(15) 0.47602(7) 0.93398(12) 0.0478(5) Uani 1 1 d . . . . . C43 C 0.9502(5) 0.5155(2) 0.9872(4) 0.041(2) Uani 1 1 d . . . . . H43A H 0.967994 0.543790 0.951565 0.049 Uiso 1 1 calc R U . . . H43B H 0.924473 0.531006 1.035043 0.049 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.01321(11) 0.01593(11) 0.01401(13) -0.00030(11) 0.00165(8) -0.00054(12) Cl1 0.0304(9) 0.0290(9) 0.0226(10) -0.0016(7) 0.0136(8) 0.0048(8) Cl2 0.0136(8) 0.0428(12) 0.0454(12) 0.0094(8) 0.0018(8) -0.0071(8) O1 0.016(2) 0.014(2) 0.015(3) -0.0021(17) 0.0067(18) -0.0027(17) O2 0.015(2) 0.020(2) 0.017(3) 0.0002(18) -0.0024(18) -0.0074(18) O3 0.010(2) 0.020(2) 0.023(3) 0.0019(19) -0.0003(18) -0.0003(19) O4 0.014(2) 0.013(2) 0.029(3) 0.0043(19) 0.005(2) 0.0012(19) O5 0.032(3) 0.017(3) 0.060(4) -0.011(2) 0.013(3) 0.008(2) O6 0.019(2) 0.022(2) 0.011(3) 0.0019(18) -0.0008(18) 0.0037(19) O7 0.011(2) 0.030(3) 0.012(3) -0.0008(19) -0.0008(18) -0.003(2) O8 0.022(3) 0.048(3) 0.022(3) 0.014(2) 0.007(2) -0.013(2) O9 0.019(2) 0.022(3) 0.017(3) -0.0051(19) 0.0036(19) 0.0014(19) O10 0.020(2) 0.029(3) 0.016(3) -0.003(2) -0.0005(19) 0.002(2) O11 0.036(3) 0.031(3) 0.033(3) -0.011(2) 0.008(2) 0.012(2) O12 0.015(2) 0.027(3) 0.015(3) 0.0051(19) -0.0003(18) 0.004(2) O13 0.018(2) 0.020(2) 0.015(3) -0.0021(17) 0.0066(18) 0.0002(18) O14 0.035(3) 0.012(2) 0.028(3) 0.0034(19) 0.008(2) -0.001(2) N1 0.013(3) 0.011(3) 0.022(3) 0.003(2) 0.006(2) -0.004(2) N2 0.007(3) 0.020(3) 0.020(3) 0.002(2) -0.002(2) -0.001(2) N3 0.016(3) 0.017(3) 0.020(3) -0.002(2) 0.004(2) -0.001(2) N4 0.021(3) 0.021(3) 0.020(3) 0.002(2) -0.002(2) -0.009(2) N5 0.033(4) 0.025(3) 0.014(3) -0.002(2) 0.007(3) -0.003(3) N6 0.022(3) 0.026(3) 0.020(4) 0.000(3) 0.001(3) 0.003(3) N7 0.019(3) 0.023(3) 0.020(4) -0.003(3) -0.002(3) 0.000(3) N8 0.014(3) 0.019(3) 0.027(4) -0.003(3) 0.003(2) 0.004(2) C1 0.015(3) 0.016(3) 0.013(4) 0.004(3) 0.002(3) 0.001(3) C2 0.015(3) 0.011(3) 0.019(4) 0.001(3) 0.007(3) -0.001(3) C3 0.020(3) 0.019(3) 0.017(4) 0.003(3) 0.001(3) 0.002(3) C4 0.021(3) 0.013(3) 0.020(4) 0.005(3) 0.010(3) 0.005(3) C5 0.015(3) 0.016(3) 0.023(4) 0.006(3) 0.004(3) 0.008(3) C6 0.015(3) 0.008(3) 0.014(4) 0.000(2) 0.003(3) 0.000(3) C7 0.014(3) 0.018(3) 0.018(4) 0.006(3) -0.003(3) 0.001(3) C8 0.014(3) 0.016(3) 0.022(4) 0.009(3) 0.001(3) 0.001(3) C9 0.012(3) 0.016(4) 0.030(4) 0.002(3) 0.001(3) 0.000(3) C10 0.023(4) 0.015(3) 0.028(4) 0.009(3) 0.012(3) 0.007(3) C11 0.013(3) 0.022(4) 0.033(5) 0.006(3) 0.004(3) 0.002(3) C12 0.013(3) 0.020(4) 0.025(4) 0.005(3) -0.010(3) -0.007(3) C13 0.020(3) 0.013(3) 0.018(4) 0.004(2) 0.000(3) 0.002(3) C14 0.016(3) 0.029(4) 0.009(3) 0.003(3) -0.007(2) -0.007(3) C15 0.013(3) 0.030(4) 0.022(4) -0.008(3) -0.001(3) 0.001(3) C16 0.018(4) 0.040(4) 0.039(5) 0.001(3) 0.009(3) -0.007(3) C17 0.020(3) 0.014(3) 0.015(4) -0.007(3) 0.006(3) -0.002(3) C18 0.021(4) 0.018(3) 0.023(4) 0.001(3) 0.000(3) -0.006(3) C19 0.018(4) 0.020(4) 0.024(4) 0.005(3) -0.001(3) 0.005(3) C20 0.015(3) 0.019(3) 0.018(4) -0.001(3) 0.002(3) -0.002(3) C21 0.030(4) 0.013(3) 0.013(4) -0.004(2) 0.002(3) 0.008(3) C22 0.016(4) 0.025(4) 0.026(4) -0.002(3) -0.001(3) -0.001(3) C23 0.025(4) 0.019(4) 0.045(5) -0.009(3) 0.004(3) 0.002(3) C24 0.024(4) 0.029(4) 0.030(5) -0.003(3) 0.007(3) 0.003(3) C25 0.022(4) 0.029(4) 0.029(5) -0.008(3) 0.001(3) 0.003(3) C26 0.025(4) 0.017(3) 0.024(4) -0.003(3) 0.001(3) -0.008(3) C27 0.015(3) 0.027(4) 0.026(4) -0.006(3) 0.001(3) -0.002(3) C28 0.019(4) 0.026(4) 0.016(4) -0.002(3) -0.007(3) -0.001(3) C29 0.035(4) 0.035(4) 0.018(4) -0.005(3) 0.008(3) -0.010(3) C30 0.050(5) 0.033(4) 0.037(5) -0.015(3) 0.012(4) -0.006(4) C31 0.030(4) 0.020(4) 0.014(4) 0.001(3) -0.003(3) -0.012(3) C32 0.027(4) 0.027(4) 0.018(4) 0.002(3) -0.009(3) -0.007(3) C33 0.043(5) 0.026(4) 0.018(4) 0.010(3) -0.001(3) -0.012(3) C34 0.031(4) 0.023(4) 0.018(4) 0.000(3) -0.003(3) -0.015(3) C35 0.031(4) 0.030(4) 0.008(4) 0.000(3) 0.001(3) -0.013(3) C36 0.027(4) 0.020(4) 0.047(5) -0.002(3) 0.003(4) -0.004(3) C37 0.035(4) 0.025(4) 0.045(5) 0.000(3) -0.010(4) -0.003(3) C38 0.030(4) 0.031(4) 0.022(4) -0.002(3) -0.007(3) -0.013(3) C39 0.037(4) 0.041(5) 0.031(5) -0.012(3) 0.006(4) -0.011(4) C40 0.033(4) 0.021(4) 0.052(5) -0.015(3) 0.020(4) -0.006(3) C41 0.031(4) 0.026(4) 0.017(4) 0.001(3) -0.006(3) -0.011(3) C42 0.029(4) 0.022(4) 0.022(4) 0.000(3) -0.005(3) -0.013(3) Cl3 0.0410(11) 0.0473(12) 0.0494(13) 0.0018(10) -0.0107(9) -0.0027(10) C43 0.045(5) 0.043(5) 0.033(5) -0.007(4) 0.001(4) 0.006(4) 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' Th Th -7.2400 8.8979 '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 Th1 O3 66.74(12) . . ? O1 Th1 O4 108.95(12) . . ? O1 Th1 O6 69.69(12) . . ? O1 Th1 O7 115.47(12) . . ? O1 Th1 O9 68.24(12) . . ? O1 Th1 O10 113.36(12) . . ? O1 Th1 O12 111.22(12) . . ? O1 Th1 O13 67.98(12) . . ? O1 Th1 N1 59.86(13) . . ? O1 Th1 N2 116.79(13) . . ? O2 Th1 O1 175.61(12) . . ? O2 Th1 O3 115.88(12) . . ? O2 Th1 O4 71.95(13) . . ? O2 Th1 O6 114.47(12) . . ? O2 Th1 O7 68.91(12) . . ? O2 Th1 O9 111.50(12) . . ? O2 Th1 O10 68.15(12) . . ? O2 Th1 O12 65.33(12) . . ? O2 Th1 O13 107.78(12) . . ? O2 Th1 N1 117.52(13) . . ? O2 Th1 N2 59.64(13) . . ? O3 Th1 O12 165.97(12) . . ? O3 Th1 N1 64.66(12) . . ? O3 Th1 N2 102.42(13) . . ? O4 Th1 O3 49.43(12) . . ? O4 Th1 O12 122.98(12) . . ? O4 Th1 O13 120.27(12) . . ? O4 Th1 N1 66.65(13) . . ? O4 Th1 N2 60.89(13) . . ? O6 Th1 O3 64.96(12) . . ? O6 Th1 O4 102.71(12) . . ? O6 Th1 O9 68.68(12) . . ? O6 Th1 O10 67.34(12) . . ? O6 Th1 O12 128.28(12) . . ? O6 Th1 O13 126.91(12) . . ? O6 Th1 N1 118.70(13) . . ? O6 Th1 N2 163.31(13) . . ? O7 Th1 O3 67.88(12) . . ? O7 Th1 O4 68.99(12) . . ? O7 Th1 O6 50.44(12) . . ? O7 Th1 O9 104.44(12) . . ? O7 Th1 O10 66.84(12) . . ? O7 Th1 O12 122.94(12) . . ? O7 Th1 O13 169.37(12) . . ? O7 Th1 N1 129.02(13) . . ? O7 Th1 N2 115.84(13) . . ? O9 Th1 O3 123.52(12) . . ? O9 Th1 O4 171.38(12) . . ? O9 Th1 O10 49.84(12) . . ? O9 Th1 O12 65.05(12) . . ? O9 Th1 O13 66.86(12) . . ? O9 Th1 N1 116.45(13) . . ? O9 Th1 N2 127.73(13) . . ? O10 Th1 O3 128.21(12) . . ? O10 Th1 O4 128.30(13) . . ? O10 Th1 O12 65.74(12) . . ? O10 Th1 O13 102.52(12) . . ? O10 Th1 N1 163.88(13) . . ? O10 Th1 N2 119.08(13) . . ? O12 Th1 N1 101.95(13) . . ? O12 Th1 N2 65.50(13) . . ? O13 Th1 O3 121.66(12) . . ? O13 Th1 O12 48.63(12) . . ? O13 Th1 N1 61.60(12) . . ? O13 Th1 N2 68.46(13) . . ? N1 Th1 N2 59.87(14) . . ? C1 O1 Th1 123.7(4) . . ? C14 O2 Th1 123.8(3) . . ? N5 O3 Th1 96.6(3) . . ? N5 O4 Th1 97.5(3) . . ? N6 O6 Th1 96.8(3) . . ? N6 O7 Th1 97.7(3) . . ? N7 O9 Th1 97.1(3) . . ? N7 O10 Th1 97.2(3) . . ? N8 O12 Th1 97.2(3) . . ? N8 O13 Th1 99.0(3) . . ? C2 N1 Th1 118.8(3) . . ? C2 N1 C6 118.7(5) . . ? C6 N1 Th1 122.5(4) . . ? C7 N2 Th1 121.6(4) . . ? C13 N2 Th1 118.7(4) . . ? C13 N2 C7 119.3(5) . . ? C1 N3 C15 118.9(5) . . ? C1 N3 C17 123.6(5) . . ? C17 N3 C15 116.7(5) . . ? C14 N4 C29 119.4(5) . . ? C14 N4 C31 124.2(5) . . ? C31 N4 C29 115.5(5) . . ? O3 N5 Th1 58.7(3) . . ? O3 N5 O4 115.4(5) . . ? O4 N5 Th1 57.5(3) . . ? O5 N5 Th1 169.9(4) . . ? O5 N5 O3 123.4(5) . . ? O5 N5 O4 121.2(5) . . ? O6 N6 Th1 58.2(3) . . ? O6 N6 O7 115.1(5) . . ? O7 N6 Th1 56.9(3) . . ? O8 N6 Th1 177.6(4) . . ? O8 N6 O6 122.5(5) . . ? O8 N6 O7 122.5(5) . . ? O9 N7 Th1 57.6(3) . . ? O10 N7 Th1 58.1(3) . . ? O10 N7 O9 115.5(5) . . ? O11 N7 Th1 174.6(4) . . ? O11 N7 O9 121.9(5) . . ? O11 N7 O10 122.6(5) . . ? O12 N8 O13 114.7(5) . . ? O14 N8 O12 124.6(5) . . ? O14 N8 O13 120.8(5) . . ? O1 C1 N3 122.2(5) . . ? O1 C1 C2 115.5(5) . . ? N3 C1 C2 122.2(5) . . ? N1 C2 C1 111.3(5) . . ? N1 C2 C3 122.9(5) . . ? C3 C2 C1 125.6(5) . . ? C2 C3 H3 121.0 . . ? C4 C3 C2 117.9(6) . . ? C4 C3 H3 121.0 . . ? C3 C4 Cl1 118.4(5) . . ? C3 C4 C5 121.1(5) . . ? C5 C4 Cl1 120.5(4) . . ? C4 C5 C6 116.8(5) . . ? C4 C5 C10 124.8(6) . . ? C6 C5 C10 118.4(6) . . ? N1 C6 C5 122.3(5) . . ? N1 C6 C7 117.5(5) . . ? C5 C6 C7 120.2(5) . . ? N2 C7 C6 118.2(5) . . ? N2 C7 C8 122.5(5) . . ? C8 C7 C6 119.2(5) . . ? C7 C8 C9 119.5(5) . . ? C11 C8 C7 116.6(5) . . ? C11 C8 C9 123.9(5) . . ? C8 C9 H9 119.1 . . ? C10 C9 C8 121.8(6) . . ? C10 C9 H9 119.1 . . ? C5 C10 H10 119.6 . . ? C9 C10 C5 120.9(6) . . ? C9 C10 H10 119.6 . . ? C8 C11 Cl2 120.2(5) . . ? C12 C11 Cl2 119.3(5) . . ? C12 C11 C8 120.6(5) . . ? C11 C12 H12 120.9 . . ? C11 C12 C13 118.3(6) . . ? C13 C12 H12 120.9 . . ? N2 C13 C12 122.6(6) . . ? N2 C13 C14 111.0(5) . . ? C12 C13 C14 126.2(6) . . ? O2 C14 N4 121.6(5) . . ? O2 C14 C13 115.1(5) . . ? N4 C14 C13 123.3(5) . . ? N3 C15 H15A 109.4 . . ? N3 C15 H15B 109.4 . . ? N3 C15 C16 111.4(5) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N3 118.9(5) . . ? C28 C17 N3 120.2(5) . . ? C28 C17 C18 121.0(5) . . ? C17 C18 H18 120.7 . . ? C19 C18 C17 118.6(6) . . ? C19 C18 H18 120.7 . . ? C18 C19 H19 119.0 . . ? C18 C19 C20 122.0(6) . . ? C20 C19 H19 119.0 . . ? C19 C20 C21 121.7(5) . . ? C27 C20 C19 117.5(5) . . ? C27 C20 C21 120.6(6) . . ? C20 C21 H21 107.5 . . ? C20 C21 C22 113.1(5) . . ? C20 C21 C26 111.1(5) . . ? C22 C21 H21 107.5 . . ? C22 C21 C26 109.9(5) . . ? C26 C21 H21 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C23 C22 C21 110.7(5) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C22 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C24 C23 C22 112.2(5) . . ? C24 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C23 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C25 C24 C23 111.2(5) . . ? C25 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C24 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C24 C25 C26 110.4(5) . . ? H25A C25 H25B 108.1 . . ? C26 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? C21 C26 H26A 109.4 . . ? C21 C26 H26B 109.4 . . ? C25 C26 C21 111.3(5) . . ? C25 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C20 C27 H27 118.8 . . ? C28 C27 C20 122.3(6) . . ? C28 C27 H27 118.8 . . ? C17 C28 C27 118.6(6) . . ? C17 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? N4 C29 H29A 109.2 . . ? N4 C29 H29B 109.2 . . ? N4 C29 C30 112.0(5) . . ? H29A C29 H29B 107.9 . . ? C30 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N4 119.9(5) . . ? C42 C31 N4 119.1(5) . . ? C42 C31 C32 120.9(6) . . ? C31 C32 H32 120.5 . . ? C33 C32 C31 118.9(6) . . ? C33 C32 H32 120.5 . . ? C32 C33 H33 119.1 . . ? C32 C33 C34 121.9(6) . . ? C34 C33 H33 119.1 . . ? C33 C34 C35 120.8(6) . . ? C41 C34 C33 117.8(6) . . ? C41 C34 C35 121.3(6) . . ? C34 C35 H35 107.4 . . ? C34 C35 C36 110.8(5) . . ? C34 C35 C40 114.5(5) . . ? C36 C35 H35 107.4 . . ? C40 C35 H35 107.4 . . ? C40 C35 C36 109.2(5) . . ? C35 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C35 C36 C37 111.7(5) . . ? H36A C36 H36B 107.9 . . ? C37 C36 H36A 109.3 . . ? C37 C36 H36B 109.3 . . ? C36 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C38 C37 C36 111.9(5) . . ? C38 C37 H37A 109.2 . . ? C38 C37 H37B 109.2 . . ? C37 C38 H38A 109.6 . . ? C37 C38 H38B 109.6 . . ? C37 C38 C39 110.2(5) . . ? H38A C38 H38B 108.1 . . ? C39 C38 H38A 109.6 . . ? C39 C38 H38B 109.6 . . ? C38 C39 H39A 109.4 . . ? C38 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C40 C39 C38 111.2(6) . . ? C40 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? C35 C40 C39 111.9(5) . . ? C35 C40 H40A 109.2 . . ? C35 C40 H40B 109.2 . . ? C39 C40 H40A 109.2 . . ? C39 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C34 C41 H41 119.3 . . ? C34 C41 C42 121.4(6) . . ? C42 C41 H41 119.3 . . ? C31 C42 C41 118.9(6) . . ? C31 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? Cl3 C43 H43A 109.7 . . ? Cl3 C43 H43B 109.7 . . ? C43 C43 Cl3 109.6(6) 3_767 . ? C43 C43 H43A 109.7 3_767 . ? C43 C43 H43B 109.7 3_767 . ? H43A C43 H43B 108.2 . . ? 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 Th1 O1 2.456(4) . ? Th1 O2 2.450(4) . ? Th1 O3 2.606(4) . ? Th1 O4 2.577(4) . ? Th1 O6 2.553(4) . ? Th1 O7 2.522(4) . ? Th1 O9 2.553(4) . ? Th1 O10 2.569(4) . ? Th1 O12 2.640(4) . ? Th1 O13 2.594(4) . ? Th1 N1 2.692(5) . ? Th1 N2 2.710(4) . ? Cl1 C4 1.729(6) . ? Cl2 C11 1.712(6) . ? O1 C1 1.258(6) . ? O2 C14 1.253(6) . ? O3 N5 1.274(6) . ? O4 N5 1.291(6) . ? O5 N5 1.212(6) . ? O6 N6 1.271(6) . ? O7 N6 1.291(6) . ? O8 N6 1.199(6) . ? O9 N7 1.291(6) . ? O10 N7 1.261(6) . ? O11 N7 1.214(6) . ? O12 N8 1.271(6) . ? O13 N8 1.289(6) . ? O14 N8 1.209(6) . ? N1 C2 1.332(7) . ? N1 C6 1.357(7) . ? N2 C7 1.353(7) . ? N2 C13 1.329(7) . ? N3 C1 1.309(7) . ? N3 C15 1.475(7) . ? N3 C17 1.438(7) . ? N4 C14 1.315(7) . ? N4 C29 1.485(7) . ? N4 C31 1.454(7) . ? C1 C2 1.519(7) . ? C2 C3 1.393(7) . ? C3 H3 0.9500 . ? C3 C4 1.379(8) . ? C4 C5 1.390(8) . ? C5 C6 1.411(7) . ? C5 C10 1.450(8) . ? C6 C7 1.430(8) . ? C7 C8 1.410(7) . ? C8 C9 1.419(8) . ? C8 C11 1.406(8) . ? C9 H9 0.9500 . ? C9 C10 1.336(8) . ? C10 H10 0.9500 . ? C11 C12 1.388(8) . ? C12 H12 0.9500 . ? C12 C13 1.393(8) . ? C13 C14 1.517(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.540(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.390(8) . ? C17 C28 1.379(7) . ? C18 H18 0.9500 . ? C18 C19 1.379(8) . ? C19 H19 0.9500 . ? C19 C20 1.388(8) . ? C20 C21 1.520(7) . ? C20 C27 1.382(8) . ? C21 H21 1.0000 . ? C21 C22 1.534(7) . ? C21 C26 1.537(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.524(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.521(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C25 1.520(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.524(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27 0.9500 . ? C27 C28 1.380(8) . ? C28 H28 0.9500 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.507(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.391(8) . ? C31 C42 1.381(8) . ? C32 H32 0.9500 . ? C32 C33 1.377(8) . ? C33 H33 0.9500 . ? C33 C34 1.394(8) . ? C34 C35 1.503(8) . ? C34 C41 1.390(8) . ? C35 H35 1.0000 . ? C35 C36 1.533(8) . ? C35 C40 1.518(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 C37 1.540(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.524(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.533(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.521(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41 0.9500 . ? C41 C42 1.394(8) . ? C42 H42 0.9500 . ? Cl3 C43 1.782(7) . ? C43 C43 1.457(12) 3_767 ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? 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 Th1 O1 C1 N3 142.6(4) . . . . ? Th1 O1 C1 C2 -39.7(6) . . . . ? Th1 O2 C14 N4 138.0(5) . . . . ? Th1 O2 C14 C13 -42.8(7) . . . . ? Th1 O3 N5 O4 10.6(5) . . . . ? Th1 O3 N5 O5 -168.3(5) . . . . ? Th1 O4 N5 O3 -10.7(5) . . . . ? Th1 O4 N5 O5 168.2(5) . . . . ? Th1 O6 N6 O7 1.8(5) . . . . ? Th1 O6 N6 O8 -177.3(5) . . . . ? Th1 O7 N6 O6 -1.8(5) . . . . ? Th1 O7 N6 O8 177.3(5) . . . . ? Th1 O9 N7 O10 -5.5(5) . . . . ? Th1 O9 N7 O11 173.6(5) . . . . ? Th1 O10 N7 O9 5.5(5) . . . . ? Th1 O10 N7 O11 -173.6(5) . . . . ? Th1 O12 N8 O13 -7.2(4) . . . . ? Th1 O12 N8 O14 174.4(5) . . . . ? Th1 O13 N8 O12 7.3(5) . . . . ? Th1 O13 N8 O14 -174.1(4) . . . . ? Th1 N1 C2 C1 6.5(6) . . . . ? Th1 N1 C2 C3 -177.7(4) . . . . ? Th1 N1 C6 C5 175.4(4) . . . . ? Th1 N1 C6 C7 -4.9(7) . . . . ? Th1 N2 C7 C6 4.7(7) . . . . ? Th1 N2 C7 C8 -176.0(4) . . . . ? Th1 N2 C13 C12 176.6(4) . . . . ? Th1 N2 C13 C14 1.0(6) . . . . ? Cl1 C4 C5 C6 -179.6(4) . . . . ? Cl1 C4 C5 C10 1.8(8) . . . . ? Cl2 C11 C12 C13 178.3(4) . . . . ? O1 C1 C2 N1 18.6(7) . . . . ? O1 C1 C2 C3 -157.0(5) . . . . ? N1 C2 C3 C4 2.6(9) . . . . ? N1 C6 C7 N2 0.0(8) . . . . ? N1 C6 C7 C8 -179.2(5) . . . . ? N2 C7 C8 C9 179.9(5) . . . . ? N2 C7 C8 C11 0.9(9) . . . . ? N2 C13 C14 O2 24.0(7) . . . . ? N2 C13 C14 N4 -156.9(6) . . . . ? N3 C1 C2 N1 -163.7(5) . . . . ? N3 C1 C2 C3 20.7(9) . . . . ? N3 C17 C18 C19 -178.4(5) . . . . ? N3 C17 C28 C27 177.6(5) . . . . ? N4 C31 C32 C33 -179.7(6) . . . . ? N4 C31 C42 C41 179.3(5) . . . . ? C1 N3 C15 C16 -92.0(7) . . . . ? C1 N3 C17 C18 61.4(8) . . . . ? C1 N3 C17 C28 -118.8(7) . . . . ? C1 C2 C3 C4 177.8(5) . . . . ? C2 N1 C6 C5 -2.7(8) . . . . ? C2 N1 C6 C7 177.0(5) . . . . ? C2 C3 C4 Cl1 177.5(4) . . . . ? C2 C3 C4 C5 -3.5(9) . . . . ? C3 C4 C5 C6 1.4(8) . . . . ? C3 C4 C5 C10 -177.2(5) . . . . ? C4 C5 C6 N1 1.8(8) . . . . ? C4 C5 C6 C7 -178.0(5) . . . . ? C4 C5 C10 C9 176.9(6) . . . . ? C5 C6 C7 N2 179.8(5) . . . . ? C5 C6 C7 C8 0.5(9) . . . . ? C6 N1 C2 C1 -175.4(5) . . . . ? C6 N1 C2 C3 0.4(8) . . . . ? C6 C5 C10 C9 -1.6(8) . . . . ? C6 C7 C8 C9 -0.9(8) . . . . ? C6 C7 C8 C11 -179.9(5) . . . . ? C7 N2 C13 C12 4.1(8) . . . . ? C7 N2 C13 C14 -171.5(5) . . . . ? C7 C8 C9 C10 0.0(9) . . . . ? C7 C8 C11 Cl2 -178.0(4) . . . . ? C7 C8 C11 C12 1.5(9) . . . . ? C8 C9 C10 C5 1.3(9) . . . . ? C8 C11 C12 C13 -1.3(9) . . . . ? C9 C8 C11 Cl2 3.1(9) . . . . ? C9 C8 C11 C12 -177.4(5) . . . . ? C10 C5 C6 N1 -179.6(5) . . . . ? C10 C5 C6 C7 0.7(8) . . . . ? C11 C8 C9 C10 178.9(6) . . . . ? C11 C12 C13 N2 -1.6(9) . . . . ? C11 C12 C13 C14 173.3(5) . . . . ? C12 C13 C14 O2 -151.4(5) . . . . ? C12 C13 C14 N4 27.7(9) . . . . ? C13 N2 C7 C6 177.1(5) . . . . ? C13 N2 C7 C8 -3.7(9) . . . . ? C14 N4 C29 C30 -92.5(7) . . . . ? C14 N4 C31 C32 61.8(9) . . . . ? C14 N4 C31 C42 -120.5(7) . . . . ? C15 N3 C1 O1 2.6(9) . . . . ? C15 N3 C1 C2 -174.9(5) . . . . ? C15 N3 C17 C18 -107.7(6) . . . . ? C15 N3 C17 C28 72.1(7) . . . . ? C17 N3 C1 O1 -166.3(5) . . . . ? C17 N3 C1 C2 16.2(9) . . . . ? C17 N3 C15 C16 77.6(7) . . . . ? C17 C18 C19 C20 -0.6(9) . . . . ? C18 C17 C28 C27 -2.6(9) . . . . ? C18 C19 C20 C21 175.8(5) . . . . ? C18 C19 C20 C27 0.3(9) . . . . ? C19 C20 C21 C22 59.2(7) . . . . ? C19 C20 C21 C26 -65.0(7) . . . . ? C19 C20 C27 C28 -1.1(9) . . . . ? C20 C21 C22 C23 179.6(5) . . . . ? C20 C21 C26 C25 -176.6(5) . . . . ? C20 C27 C28 C17 2.3(9) . . . . ? C21 C20 C27 C28 -176.7(5) . . . . ? C21 C22 C23 C24 55.1(7) . . . . ? C22 C21 C26 C25 57.5(7) . . . . ? C22 C23 C24 C25 -55.2(7) . . . . ? C23 C24 C25 C26 55.8(7) . . . . ? C24 C25 C26 C21 -57.6(7) . . . . ? C26 C21 C22 C23 -55.6(7) . . . . ? C27 C20 C21 C22 -125.4(6) . . . . ? C27 C20 C21 C26 110.4(6) . . . . ? C28 C17 C18 C19 1.8(9) . . . . ? C29 N4 C14 O2 -3.8(9) . . . . ? C29 N4 C14 C13 177.1(5) . . . . ? C29 N4 C31 C32 -107.4(7) . . . . ? C29 N4 C31 C42 70.4(8) . . . . ? C31 N4 C14 O2 -172.5(5) . . . . ? C31 N4 C14 C13 8.4(9) . . . . ? C31 N4 C29 C30 77.2(7) . . . . ? C31 C32 C33 C34 0.7(10) . . . . ? C32 C31 C42 C41 -2.9(10) . . . . ? C32 C33 C34 C35 -179.1(6) . . . . ? C32 C33 C34 C41 -3.4(10) . . . . ? C33 C34 C35 C36 93.6(7) . . . . ? C33 C34 C35 C40 -142.4(6) . . . . ? C33 C34 C41 C42 3.1(10) . . . . ? C34 C35 C36 C37 -177.4(5) . . . . ? C34 C35 C40 C39 177.6(5) . . . . ? C34 C41 C42 C31 0.0(10) . . . . ? C35 C34 C41 C42 178.7(6) . . . . ? C35 C36 C37 C38 -55.2(8) . . . . ? C36 C35 C40 C39 -57.6(7) . . . . ? C36 C37 C38 C39 54.0(8) . . . . ? C37 C38 C39 C40 -55.3(8) . . . . ? C38 C39 C40 C35 58.4(8) . . . . ? C40 C35 C36 C37 55.6(7) . . . . ? C41 C34 C35 C36 -82.0(8) . . . . ? C41 C34 C35 C40 42.0(8) . . . . ? C42 C31 C32 C33 2.6(10) . . . . ? 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 -0.141 0.250 -0.562 367.2 95.8 '2 C2H4Cl2' 2 -0.747 0.750 -0.326 367.2 97.3 '2 C2H4Cl2'