#------------------------------------------------------------------------------ #$Date: 2026-06-05 00:35:36 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306222 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721099.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_7721099 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 'C32 H30 N8 O14 Th, C2 H3 N, 1.5[H2O]' _chemical_formula_sum 'C34 H36 N9 O15.5 Th' _chemical_formula_weight 1050.76 _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 mixed _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 101.2730(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.0013(4) _cell_length_b 10.9427(3) _cell_length_c 28.4236(9) _cell_measurement_reflns_used 9854 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 30.407 _cell_measurement_theta_min 2.453 _cell_volume 3965.8(2) _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 0.0455 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 31043 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.999 _diffrn_reflns_theta_min 1.621 _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 3.842 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.2821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1209 before and 0.0554 after correction. The Ratio of minimum to maximum transmission is 0.3781. 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 1.760 _exptl_crystal_description prism _exptl_crystal_F_000 2068 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.718 _refine_diff_density_min -2.270 _refine_diff_density_rms 0.164 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 545 _refine_ls_number_reflns 8645 _refine_ls_number_restraints 64 _refine_ls_restrained_S_all 1.130 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0369 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+1.0159P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.0925 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7273 _reflns_number_total 8645 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00392c2.cif _cod_data_source_block uth2 _cod_original_formula_sum 'C34 H36 N9 O15.50 Th' _cod_database_code 7721099 _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 0.545 _shelx_estimated_absorpt_t_min 0.206 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N3-C17 1.43 with sigma of 0.01 C25A-C24 1.54 with sigma of 0.02 C23A-C20A = C23-C20 1.5 with sigma of 0.02 N4-C25A 2.45 with sigma of 0.02 N3-C17A 1.43 with sigma of 0.01 N3-C17 \\sim N3-C17A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C25A) = Uanis(C25) Uanis(C17) = Uanis(C17A) Uanis(C22A) = Uanis(C19A) Uanis(C22) = Uanis(C19) Uanis(C23) = Uanis(C23A) 4. Rigid body (RIGU) restrains C17, C18, C19, C20, C21, C22 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 C17A, C18A, C19A, C21A, C22A with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 5. Others Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1) Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1) Fixed Sof: C17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5) C17A(0.5) C18A(0.5) H18A(0.5) C19A(0.5) H19A(0.5) C20A(0.5) C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) 6.a Riding coordinates: C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F) 6.b Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C24(H24A,H24B), C24(H24C,H24D) 6.c Me refined with riding coordinates: C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F) 6.d Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C18(H18), C19(H19), C21(H21), C22(H22), C18A(H18A), C19A(H19A), C21A(H21A), C22A(H22A), C27(H27), C28(H28), C30(H30), C31(H31) 6.e Fitted hexagon refined as free rotating group: C17(C18,C19,C20,C21,C22), C17A(C18A,C19A,C20A,C21A,C22A) 6.f Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL uth2_a.res in P2(1)/n uth2.res created by SHELXL-2018/3 at 13:41:16 on 24-Oct-2025 REM Old TITL UTh2 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.085, Rweak 0.004, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C38 N10 O12 Th CELL 0.71073 13.0013 10.9427 28.4236 90 101.273 90 ZERR 4 0.0004 0.0003 0.0009 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Th UNIT 136 144 36 62 4 DFIX 1.43 0.01 N3 C17 DFIX 1.54 C25A C24 EADP C25A C25 DFIX 1.5 C23A C20A C23 C20 EADP C17 C17A DFIX 2.45 N4 C25A DFIX 1.43 0.01 N3 C17A SADI N3 C17 N3 C17A RIGU 0.002 0.002 C17 > C22 RIGU 0.002 0.002 C17A C18A C19A C21A C22A EADP C22A C19A EADP C22 C19 EADP C23 C23A L.S. 4 PLAN 50 SIZE 0.6 0.22 0.18 TEMP -173.15 CONF BOND $H list 4 MORE -1 ABIN fmap 2 acta OMIT -2 54 OMIT -2 1 2 OMIT 0 0 2 REM REM REM WGHT 0.046200 1.015900 FVAR 0.20125 0.91544 TH1 5 0.404453 0.288492 0.641586 11.00000 0.01842 0.01452 = 0.01028 -0.00047 0.00394 -0.00042 O1 4 0.375573 0.212356 0.718692 11.00000 0.02588 0.02043 = 0.01066 -0.00262 0.00458 -0.00322 O2 4 0.433288 0.370065 0.563231 11.00000 0.02071 0.02337 = 0.01196 0.00067 0.00415 0.00043 O3 4 0.222000 0.372236 0.654760 11.00000 0.02512 0.02043 = 0.01293 -0.00027 0.00391 -0.00064 O4 4 0.233189 0.344809 0.580550 11.00000 0.02382 0.02134 = 0.01485 -0.00125 0.00708 -0.00032 O5 4 0.107349 0.458611 0.597656 11.00000 0.02499 0.03012 = 0.02421 -0.00153 0.00222 0.00919 O6 4 0.263792 0.125145 0.634749 11.00000 0.02819 0.01747 = 0.01345 -0.00614 0.00574 -0.00516 O7 4 0.339350 0.129461 0.573537 11.00000 0.02240 0.02585 = 0.01771 0.00078 0.00815 -0.00296 O8 4 0.213907 -0.001433 0.575788 11.00000 0.03416 0.02239 = 0.02387 -0.00320 -0.00219 -0.00931 O9 4 0.478758 0.072238 0.658837 11.00000 0.03207 0.02161 = 0.01841 -0.00164 0.01281 -0.00278 O10 4 0.555821 0.183254 0.613426 11.00000 0.02628 0.01981 = 0.02414 0.00372 0.01282 0.00051 O11 4 0.605386 -0.006901 0.627143 11.00000 0.04496 0.02616 = 0.04634 0.00355 0.02213 0.02303 O12 4 0.574158 0.283198 0.707248 11.00000 0.02451 0.01968 = 0.01961 0.00383 0.00599 0.00099 O13 4 0.567295 0.426940 0.654053 11.00000 0.02231 0.01570 = 0.01991 0.00234 0.00246 -0.00356 O14 4 0.710025 0.402201 0.708845 11.00000 0.02110 0.03510 = 0.04659 0.00459 -0.00773 -0.00796 N1 3 0.396062 0.445826 0.712933 11.00000 0.01419 0.01528 = 0.01347 -0.00012 0.00076 -0.00306 N2 3 0.377050 0.528318 0.622207 11.00000 0.01402 0.02669 = 0.01265 -0.00308 0.00169 -0.00119 N3 3 0.444341 0.204335 0.797633 11.00000 0.03150 0.01954 = 0.01316 0.00163 0.00549 -0.00134 N4 3 0.357227 0.474796 0.497008 11.00000 0.02238 0.02631 = 0.01183 0.00135 0.00392 0.00332 N5 3 0.183834 0.392574 0.610463 11.00000 0.02050 0.01625 = 0.02021 0.00225 0.00771 -0.00070 N6 3 0.270419 0.081022 0.593691 11.00000 0.02122 0.01665 = 0.01555 -0.00290 -0.00053 0.00016 N7 3 0.550276 0.079219 0.633097 11.00000 0.02853 0.02239 = 0.01900 0.00068 0.00578 -0.00368 N8 3 0.621377 0.373401 0.690948 11.00000 0.02518 0.01937 = 0.02089 -0.00083 0.00471 0.00100 C1 1 0.406454 0.265682 0.758154 11.00000 0.01703 0.02290 = 0.01499 -0.00010 0.00445 -0.00087 C2 1 0.395747 0.403008 0.757035 11.00000 0.01504 0.01404 = 0.01493 -0.00326 0.00269 -0.00320 C3 1 0.377507 0.477313 0.794735 11.00000 0.01514 0.02327 = 0.01425 -0.00354 0.00090 -0.00161 AFIX 43 H3 2 0.375447 0.443353 0.825297 11.00000 -1.20000 AFIX 0 C4 1 0.362760 0.599677 0.786532 11.00000 0.01915 0.02222 = 0.01474 -0.00367 0.00663 0.00104 AFIX 43 H4 2 0.350554 0.651574 0.811669 11.00000 -1.20000 AFIX 0 C5 1 0.365500 0.649298 0.741285 11.00000 0.01731 0.02076 = 0.01888 -0.00372 0.00353 -0.00106 C6 1 0.379868 0.567665 0.705126 11.00000 0.01251 0.01762 = 0.01366 -0.00136 0.00204 -0.00150 C7 1 0.374445 0.610294 0.657035 11.00000 0.01643 0.01390 = 0.01888 0.00150 0.00611 0.00113 C8 1 0.365619 0.737388 0.647629 11.00000 0.01603 0.01757 = 0.02345 0.00129 0.00650 0.00366 C9 1 0.356711 0.820198 0.686308 11.00000 0.02367 0.01511 = 0.02858 -0.00094 0.00937 -0.00003 AFIX 43 H9 2 0.352417 0.905716 0.680499 11.00000 -1.20000 AFIX 0 C10 1 0.354445 0.776914 0.730678 11.00000 0.02507 0.01612 = 0.02562 -0.00502 0.00803 -0.00219 AFIX 43 H10 2 0.345335 0.832358 0.755255 11.00000 -1.20000 AFIX 0 C11 1 0.365839 0.774928 0.600828 11.00000 0.02789 0.01306 = 0.02744 0.00596 0.00984 0.00303 AFIX 43 H11 2 0.365396 0.859603 0.593415 11.00000 -1.20000 AFIX 0 C12 1 0.366690 0.690221 0.565495 11.00000 0.02832 0.02679 = 0.01683 0.00606 0.01109 0.00473 AFIX 43 H12 2 0.363774 0.715305 0.533263 11.00000 -1.20000 AFIX 0 C13 1 0.371883 0.567006 0.577464 11.00000 0.01693 0.01936 = 0.01653 0.00122 0.00445 0.00530 C14 1 0.385962 0.463652 0.544066 11.00000 0.01750 0.01555 = 0.01489 0.00379 0.00356 0.00206 C15 1 0.449196 0.069014 0.795946 11.00000 0.03499 0.01769 = 0.02008 0.00262 0.00530 -0.00316 AFIX 23 H15A 2 0.395706 0.039025 0.768711 11.00000 -1.20000 H15B 2 0.432317 0.035116 0.825830 11.00000 -1.20000 AFIX 0 C16 1 0.555218 0.023870 0.790435 11.00000 0.04140 0.02492 = 0.04166 -0.00258 0.00844 0.00889 AFIX 137 H16A 2 0.570490 0.053214 0.759953 11.00000 -1.50000 H16B 2 0.555767 -0.065682 0.790749 11.00000 -1.50000 H16C 2 0.608619 0.054605 0.817002 11.00000 -1.50000 AFIX 66 PART 1 C17 1 0.502323 0.262679 0.840993 10.50000 0.03587 0.02124 = 0.01527 -0.00011 -0.00193 0.01313 C18 1 0.471418 0.253055 0.884979 10.50000 0.04525 0.03151 = 0.01539 0.00072 -0.00244 0.00579 AFIX 43 H18 2 0.415540 0.199964 0.888411 10.50000 -1.20000 AFIX 65 C19 1 0.522270 0.321110 0.923945 10.50000 0.03844 0.03163 = 0.01705 -0.00209 -0.00295 0.00594 AFIX 43 H19 2 0.501147 0.314533 0.954008 10.50000 -1.20000 AFIX 65 C20 1 0.604028 0.398790 0.918925 10.50000 0.04783 0.03798 = 0.01518 0.00475 -0.00147 0.00030 C21 1 0.634934 0.408415 0.874939 10.50000 0.04773 0.02811 = 0.01145 0.00203 -0.00502 0.00344 AFIX 43 H21 2 0.690812 0.461506 0.871508 10.50000 -1.20000 AFIX 65 C22 1 0.584083 0.340360 0.835972 10.50000 0.03844 0.03163 = 0.01705 -0.00209 -0.00295 0.00594 AFIX 43 H22 2 0.605206 0.346938 0.805910 10.50000 -1.20000 AFIX 66 PART 2 C17A 1 0.488724 0.262919 0.841040 10.50000 0.03587 0.02124 = 0.01527 -0.00011 -0.00193 0.01313 C18A 1 0.440633 0.245950 0.880138 10.50000 0.03508 0.04048 = 0.01409 -0.00200 -0.00429 0.01161 AFIX 43 H18A 2 0.380048 0.195809 0.877136 10.50000 -1.20000 AFIX 65 C19A 1 0.481186 0.302346 0.923629 10.50000 0.02808 0.03432 = 0.01693 -0.00409 -0.00474 0.01399 AFIX 43 H19A 2 0.448318 0.290748 0.950350 10.50000 -1.20000 AFIX 65 C20A 1 0.569831 0.375711 0.928021 10.50000 0.03509 0.04268 = 0.01519 -0.00783 0.00141 0.01381 C21A 1 0.617923 0.392681 0.888923 10.50000 0.03884 0.03320 = 0.01324 -0.00253 -0.00374 0.01172 AFIX 43 H21A 2 0.678508 0.442823 0.891926 10.50000 -1.20000 AFIX 65 C22A 1 0.577371 0.336286 0.845433 10.50000 0.02808 0.03432 = 0.01693 -0.00409 -0.00474 0.01399 AFIX 43 H22A 2 0.610240 0.347884 0.818711 10.50000 -1.20000 AFIX 0 PART 1 C23 1 0.656770 0.470602 0.962919 10.50000 0.08579 0.07479 = 0.03359 -0.02342 -0.01839 0.01803 AFIX 3 H23A 2 0.604997 0.523154 0.973785 10.50000 -1.50000 H23B 2 0.686199 0.413353 0.988546 10.50000 -1.50000 H23C 2 0.713109 0.521135 0.954862 10.50000 -1.50000 AFIX 0 PART 2 C23A 1 0.614803 0.446624 0.973537 10.50000 0.08579 0.07479 = 0.03359 -0.02342 -0.01839 0.01803 AFIX 3 H23D 2 0.562098 0.503478 0.981099 10.50000 -1.50000 H23E 2 0.635261 0.389199 1.000182 10.50000 -1.50000 H23F 2 0.676535 0.492538 0.968594 10.50000 -1.50000 AFIX 0 PART 0 C24 1 0.388414 0.378085 0.466381 11.00000 0.03724 0.04634 = 0.01549 -0.00909 0.00541 0.00945 PART 1 AFIX 23 H24A 2 0.402536 0.415379 0.436549 21.00000 -1.20000 H24B 2 0.454141 0.339551 0.483381 21.00000 -1.20000 AFIX 23 PART 2 H24C 2 0.384099 0.298110 0.482163 -21.00000 -1.20000 H24D 2 0.462534 0.391251 0.463955 -21.00000 -1.20000 AFIX 0 PART 1 C25 1 0.307040 0.283196 0.453860 21.00000 0.04229 0.03940 = 0.03951 -0.01300 0.00848 -0.00880 AFIX 33 H25A 2 0.331055 0.221175 0.433589 21.00000 -1.50000 H25B 2 0.293808 0.244783 0.483252 21.00000 -1.50000 H25C 2 0.242206 0.320605 0.436423 21.00000 -1.50000 AFIX 0 PART 2 C25A 1 0.323152 0.372706 0.416760 -21.00000 0.04229 0.03940 = 0.03951 -0.01300 0.00848 -0.00880 AFIX 33 H25D 2 0.348597 0.306592 0.398772 -21.00000 -1.50000 H25E 2 0.249806 0.357358 0.418645 -21.00000 -1.50000 H25F 2 0.328366 0.450648 0.400407 -21.00000 -1.50000 AFIX 0 PART 0 C26 1 0.278125 0.558911 0.473765 11.00000 0.02214 0.03083 = 0.01111 0.00290 0.00037 0.00137 C27 1 0.297512 0.633438 0.437432 11.00000 0.02505 0.03431 = 0.01875 0.00409 0.00446 -0.00148 AFIX 43 H27 2 0.364958 0.634622 0.429268 11.00000 -1.20000 AFIX 0 C28 1 0.218085 0.706433 0.412967 11.00000 0.02930 0.03687 = 0.02280 0.01098 0.00366 -0.00161 AFIX 43 H28 2 0.231381 0.756255 0.387443 11.00000 -1.20000 AFIX 0 C29 1 0.118727 0.708960 0.424751 11.00000 0.02355 0.03571 = 0.03174 0.01240 -0.00445 -0.00455 C30 1 0.102558 0.635000 0.462667 11.00000 0.01883 0.04101 = 0.03105 0.00899 0.00401 0.00264 AFIX 43 H30 2 0.036413 0.637111 0.472115 11.00000 -1.20000 AFIX 0 C31 1 0.179390 0.559363 0.486682 11.00000 0.02591 0.03554 = 0.02244 0.00842 0.00389 -0.00188 AFIX 43 H31 2 0.165893 0.507980 0.511726 11.00000 -1.20000 AFIX 0 C32 1 0.031056 0.782582 0.396042 11.00000 0.02630 0.04705 = 0.05130 0.02859 -0.00014 0.00196 AFIX 137 H32A 2 0.059981 0.854622 0.382779 11.00000 -1.50000 H32B 2 -0.016783 0.808717 0.416804 11.00000 -1.50000 H32C 2 -0.007301 0.732500 0.369788 11.00000 -1.50000 AFIX 0 N9 3 0.625110 0.619632 0.782687 11.00000 0.05248 0.08446 = 0.11049 0.00585 0.03273 -0.01349 C33 1 0.645210 0.663217 0.749479 11.00000 0.03004 0.04574 = 0.08513 -0.01248 0.01321 -0.00667 C34 1 0.669017 0.718810 0.707152 11.00000 0.05461 0.05533 = 0.06034 -0.01032 0.00587 -0.00687 AFIX 137 H34A 2 0.651820 0.661845 0.680152 11.00000 -1.50000 H34B 2 0.743869 0.738878 0.712580 11.00000 -1.50000 H34C 2 0.627621 0.793675 0.699814 11.00000 -1.50000 AFIX 0 HKLF 4 REM uth2_a.res in P2(1)/n REM wR2 = 0.0925, GooF = S = 1.132, Restrained GooF = 1.130 for all data REM R1 = 0.0369 for 7273 Fo > 4sig(Fo) and 0.0465 for all 8645 data REM 545 parameters refined using 64 restraints END WGHT 0.0462 1.0242 REM Highest difference peak 1.718, deepest hole -2.270, 1-sigma level 0.164 Q1 1 0.3620 0.4022 0.6336 11.00000 0.05 1.72 Q2 1 0.4192 0.2902 0.6742 11.00000 0.05 1.63 Q3 1 0.3591 0.1774 0.6348 11.00000 0.05 1.54 Q4 1 0.4499 0.4035 0.6482 11.00000 0.05 1.47 Q5 1 0.4492 0.1756 0.6493 11.00000 0.05 1.46 Q6 1 0.3927 0.2861 0.6099 11.00000 0.05 1.31 Q7 1 0.4824 0.2895 0.6230 11.00000 0.05 0.99 Q8 1 0.4991 0.2465 0.6682 11.00000 0.05 0.88 Q9 1 0.5003 0.3298 0.6684 11.00000 0.05 0.88 Q10 1 0.3373 0.2873 0.6649 11.00000 0.05 0.87 Q11 1 0.3023 0.3782 0.6427 11.00000 0.05 0.86 Q12 1 0.3013 0.1950 0.6427 11.00000 0.05 0.84 Q13 1 0.4984 0.3847 0.6373 11.00000 0.05 0.81 Q14 1 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0.5598 0.6328 10 2 11 1.0993 -0.2917 10 2 12 0.2811 0.2594 10 2 13 1.2253 -0.2879 10 2 14 0.1553 -0.1328 10 2 15 1.0110 -0.1156 10 2 16 0.2168 -0.3226 10 2 17 0.6688 0.0767 10 2 18 0.4868 -0.2635 10 2 19 0.5277 0.1540 10 2 20 0.9402 -0.0735 10 2 21 0.7720 0.1044 10 2 22 1.4622 0.0937 10 2 23 1.2953 0.0379 10 2 24 1.8600 0.1738 10 2 25 1.7761 0.0791 10 2 26 1.9521 0.2111 10 2 27 1.9077 0.2486 10 2 28 1.6827 0.2763 10 3 10 -0.4609 0.2340 10 3 11 -0.1604 0.3511 10 3 12 -0.5893 0.3336 10 3 13 -0.0978 0.3527 10 3 14 -0.3775 0.2461 10 3 15 -0.3422 0.2884 10 3 16 0.0962 0.0678 10 3 17 -0.7480 0.1392 10 3 18 0.5320 -0.0592 10 3 19 -1.1743 -0.0442 10 3 20 0.6415 -0.0808 10 3 21 -1.5235 -0.1956 10 3 22 0.3615 -0.0752 10 3 23 -1.7306 -0.2937 10 3 24 -0.1175 -0.1687 10 3 25 -1.7489 -0.3687 10 3 26 -0.5088 -0.4005 10 3 27 -1.5636 -0.4526 10 3 28 -0.6310 -0.6628 10 4 10 0.4853 -0.1211 10 4 11 0.3384 -0.0831 10 4 12 0.4506 -0.1656 10 4 13 0.3513 -0.0661 10 4 14 0.7486 -0.1755 10 4 15 0.0624 -0.0016 10 4 16 1.1304 -0.1408 10 4 17 -0.3890 0.0273 10 4 18 1.3284 -0.0823 10 4 19 -0.7899 -0.0162 10 4 20 1.2073 -0.0215 10 4 21 -1.0127 -0.0637 10 4 22 0.8139 0.0485 10 4 23 -1.0705 0.0089 10 4 24 0.3183 0.1560 10 4 25 -1.0448 0.2610 10 4 26 -0.0933 0.3087 10 4 27 -0.9797 0.6059 10 5 10 -0.8123 -0.1092 10 5 11 -0.3591 -0.1114 10 5 12 -1.0117 -0.1504 10 5 13 -0.7759 0.0276 10 5 14 -0.9448 -0.1637 10 5 15 -1.2749 0.1280 10 5 16 -0.6978 -0.1063 10 5 17 -1.5180 0.2007 10 5 18 -0.3862 0.0369 10 5 19 -1.2735 0.2623 10 5 20 -0.0508 0.2051 10 5 21 -0.5569 0.3012 10 5 22 0.3423 0.2785 10 5 23 0.3750 0.2772 10 5 24 0.8032 0.1657 10 5 25 1.1614 0.1602 10 5 26 1.2309 -0.1104 10 6 10 -0.3037 -0.0137 10 6 11 1.8174 0.0571 10 6 12 0.0890 -0.0847 10 6 13 1.5492 0.0987 10 6 14 0.5901 -0.1220 10 6 15 1.1375 0.0899 10 6 16 0.9520 -0.1521 10 6 17 0.8232 0.0053 10 6 18 0.9313 -0.2155 10 6 19 0.6774 -0.1386 10 6 20 0.4495 -0.3213 10 6 21 0.5752 -0.2725 10 6 22 -0.3314 -0.4277 10 6 23 0.3365 -0.3123 10 6 24 -1.0783 -0.4672 10 6 25 -0.0895 -0.2229 10 7 10 -2.2711 0.1366 10 7 11 0.2264 0.2464 10 7 12 -1.6998 0.0990 10 7 13 0.0413 0.1584 10 7 14 -0.7656 0.0396 10 7 15 -0.0936 0.0784 10 7 16 0.0759 -0.0155 10 7 17 -0.0715 0.0609 10 7 18 0.4781 -0.0392 10 7 19 0.1839 0.1310 10 7 20 0.3921 -0.0269 10 7 21 0.6156 0.2636 10 7 22 0.0493 -0.0009 10 7 23 1.0211 0.3939 10 7 24 -0.2333 0.0104 10 8 10 0.3898 -0.1617 10 8 11 1.5249 -0.0922 10 8 12 0.2942 -0.0768 10 8 13 0.6326 -0.0532 10 8 14 0.1516 -0.0161 10 8 15 -0.5738 0.0234 10 8 16 -0.0338 -0.0126 10 8 17 -1.5914 0.1196 10 8 18 -0.3120 -0.0655 10 8 19 -2.0184 0.2103 10 8 20 -0.6813 -0.1462 10 8 21 -1.7634 0.2726 10 8 22 -1.0188 -0.2198 10 9 10 -0.8004 -0.0300 10 9 11 -0.5578 -0.1371 10 9 12 -0.8293 -0.0417 10 9 13 -0.5451 -0.1109 10 9 14 -0.2522 -0.0482 10 9 15 -0.6179 -0.0200 10 9 16 0.7403 -0.0616 10 9 17 -0.6023 0.0925 10 9 18 1.6944 -0.0967 10 9 19 -0.3547 0.1626 10 9 20 2.1602 -0.1535 10 10 10 -0.4932 0.2078 10 10 11 0.6866 0.0005 10 10 12 -0.2277 0.1892 10 10 13 1.1763 -0.0009 10 10 14 0.4291 0.0945 10 10 15 1.0390 -0.0512 10 10 16 1.1032 -0.0394 10 10 17 0.3611 -0.1045 10 11 10 -0.3731 0.1460 10 11 11 1.6731 -0.0901 10 11 12 -1.1728 0.0927 10 11 13 0.7763 -0.1022 10 11 14 -1.6745 0.1091 11 0 11 1.5531 2.6987 11 0 13 0.5847 1.4818 11 0 15 -0.3931 0.3241 11 0 17 -1.2244 -0.3214 11 0 19 -1.8199 -0.3835 11 0 21 -2.1219 -0.1276 11 0 23 -2.1019 0.1012 11 0 25 -1.7848 0.1262 11 0 27 -1.2612 0.0040 11 1 11 -0.8303 0.0741 11 1 12 -0.5254 -1.5169 11 1 13 -0.7572 0.0914 11 1 14 0.1690 -0.5679 11 1 15 -0.4914 0.0407 11 1 16 0.6974 0.1152 11 1 17 -0.2786 -0.0290 11 1 18 1.0069 0.3221 11 1 19 -0.3462 -0.0526 11 1 20 1.0917 0.1656 11 1 21 -0.7288 -0.0082 11 1 22 0.9701 -0.0710 11 1 23 -1.2309 0.0582 11 1 24 0.6900 -0.1701 11 1 25 -1.5567 0.0688 11 1 26 0.3333 -0.1105 11 1 27 -1.5095 -0.0175 11 2 11 -0.2960 0.5465 11 2 12 0.5426 -0.2258 11 2 13 -0.5413 0.2088 11 2 14 0.1873 -0.1914 11 2 15 -0.4840 -0.0798 11 2 16 -0.2603 -0.0629 11 2 17 -0.1706 -0.1397 11 2 18 -0.3958 0.0368 11 2 19 0.3110 0.0162 11 2 20 0.0183 0.0286 11 2 21 0.8576 0.2262 11 2 22 0.8564 -0.0572 11 2 23 1.3505 0.3280 11 2 24 1.6977 -0.1131 11 2 25 1.6638 0.2797 11 2 26 2.1037 -0.0546 11 2 27 1.7065 0.1625 11 3 11 0.3319 0.2224 11 3 12 0.7404 0.1940 11 3 13 0.4929 0.2493 11 3 14 0.3702 0.1955 11 3 15 0.9151 0.1602 11 3 16 -0.2074 0.1106 11 3 17 1.2816 0.0513 11 3 18 -0.8339 -0.0680 11 3 19 1.2353 0.0127 11 3 20 -1.4111 -0.2658 11 3 21 0.6624 0.0430 11 3 22 -1.8723 -0.3903 11 3 23 -0.2078 0.0549 11 3 24 -2.1399 -0.4018 11 3 25 -0.9581 -0.0343 11 3 26 -2.1335 -0.3312 11 4 11 -0.5577 -0.0935 11 4 12 -0.4794 -0.0406 11 4 13 0.0869 -0.1574 11 4 14 -0.4983 -0.0334 11 4 15 0.7998 -0.1722 11 4 16 -0.7713 -0.0327 11 4 17 1.2843 -0.1244 11 4 18 -1.0736 -0.0798 11 4 19 1.4351 -0.0355 11 4 20 -1.1723 -0.1568 11 4 21 1.3278 0.0609 11 4 22 -0.9961 -0.1810 11 4 23 1.1056 0.1441 11 4 24 -0.6560 -0.0758 11 4 25 0.8706 0.2078 11 5 11 -0.3823 -0.1427 11 5 12 -0.0740 -0.0319 11 5 13 -0.7653 -0.1484 11 5 14 -1.2055 0.1047 11 5 15 -0.8340 -0.0802 11 5 16 -1.9368 0.2174 11 5 17 -0.5927 0.0731 11 5 18 -2.0020 0.3052 11 5 19 -0.1659 0.2736 11 5 20 -1.4659 0.3566 11 5 21 0.2981 0.4263 11 5 22 -0.6404 0.3447 11 5 23 0.6843 0.4331 11 5 24 0.1073 0.2517 11 6 11 -0.7683 0.0228 11 6 12 1.7481 0.0867 11 6 13 0.5985 -0.0127 11 6 14 1.8059 0.0984 11 6 15 1.7351 -0.0816 11 6 16 1.6515 0.0154 11 6 17 2.2269 -0.2090 11 6 18 1.3454 -0.1604 11 6 19 1.9496 -0.3807 11 6 20 0.9400 -0.3681 11 6 21 1.1184 -0.5321 11 6 22 0.4764 -0.5090 11 6 23 0.1625 -0.5837 11 7 11 -2.0411 0.0899 11 7 12 0.1214 0.0663 11 7 13 -1.6583 -0.0131 11 7 14 -0.7760 -0.0170 11 7 15 -1.1132 -0.0948 11 7 16 -1.3949 0.0008 11 7 17 -0.6654 -0.1043 11 7 18 -1.5166 0.1364 11 7 19 -0.4578 -0.0265 11 7 20 -1.1375 0.3365 11 7 21 -0.4563 0.0982 11 7 22 -0.4968 0.5035 11 8 11 0.2862 -0.0809 11 8 12 1.3921 0.0321 11 8 13 0.4336 0.0093 11 8 14 0.4843 0.1358 11 8 15 0.5920 0.0309 11 8 16 -0.4762 0.2366 11 8 17 0.6517 -0.0351 11 8 18 -1.0546 0.2886 11 8 19 0.5106 -0.1565 11 8 20 -1.0495 0.2726 11 9 11 -1.3937 -0.1659 11 9 12 -0.6346 -0.0936 11 9 13 -0.9492 -0.1556 11 9 14 -0.5000 -0.0306 11 9 15 0.0350 -0.1549 11 9 16 -0.4290 0.0659 11 9 17 1.0690 -0.1662 11 10 11 -0.0272 0.2172 11 10 12 1.5407 0.1222 11 10 13 0.1687 0.1356 11 10 14 1.3207 0.0181 11 11 11 -1.1352 -0.0494 12 0 12 0.9222 1.5940 12 0 14 0.1999 0.5708 12 0 16 -0.5509 -0.1720 12 0 18 -1.4179 -0.3696 12 0 20 -2.2990 -0.1318 12 0 22 -2.8915 0.2018 12 0 24 -2.8883 0.3369 12 1 12 -0.4124 -0.0538 12 1 13 -0.1200 -0.6906 12 1 14 -0.0022 -0.0296 12 1 15 0.2554 0.0008 12 1 16 0.3686 -0.0592 12 1 17 0.6436 0.3037 12 1 18 0.4786 -0.0877 12 1 19 1.1083 0.1766 12 1 20 0.2576 -0.0565 12 1 21 1.5299 -0.1440 12 1 22 -0.1674 0.0369 12 1 23 1.6797 -0.3586 12 1 24 -0.5580 0.1295 12 1 25 1.4081 -0.3265 12 2 12 -0.6863 0.2484 12 2 13 -0.2037 -0.0980 12 2 14 -0.5515 -0.0322 12 2 15 -0.7789 -0.0559 12 2 16 -0.2182 -0.1522 12 2 17 -1.1006 0.0230 12 2 18 0.1504 -0.0218 12 2 19 -0.9148 0.0355 12 2 20 0.4544 0.2444 12 2 21 -0.2590 -0.0588 12 2 22 0.6786 0.4362 12 2 23 0.5517 -0.1991 12 2 24 0.8390 0.4198 12 3 12 0.5918 0.1307 12 3 13 0.8000 0.1692 12 3 14 0.9707 0.1215 12 3 15 0.2136 0.1260 12 3 16 1.3774 0.0470 12 3 17 -0.4566 -0.0369 12 3 18 1.4714 -0.0067 12 3 19 -1.1031 -0.2683 12 3 20 1.0662 0.0215 12 3 21 -1.6345 -0.4444 12 3 22 0.2777 0.1105 12 3 23 -1.9503 -0.4655 12 3 24 -0.5440 0.1770 12 4 12 -0.4621 -0.0978 12 4 13 -0.3956 -0.0005 12 4 14 0.2935 -0.1299 12 4 15 -0.5727 -0.0203 12 4 16 0.8653 -0.0843 12 4 17 -0.9239 -0.0425 12 4 18 1.2005 0.0271 12 4 19 -1.1420 -0.0909 12 4 20 1.3648 0.1499 12 4 21 -1.0237 -0.1521 12 4 22 1.4193 0.2255 12 4 23 -0.5995 -0.1782 12 5 12 -0.6955 -0.1340 12 5 13 -0.8189 -0.0386 12 5 14 -0.9956 -0.0490 12 5 15 -1.7454 0.0694 12 5 16 -0.7604 0.0804 12 5 17 -1.9893 0.1519 12 5 18 -0.1782 0.2318 12 5 19 -1.6618 0.1997 12 5 20 0.4176 0.3654 12 5 21 -1.0728 0.2015 12 5 22 0.7576 0.4291 12 6 12 0.2688 0.2157 12 6 13 1.9728 0.0760 12 6 14 1.8313 0.1567 12 6 15 2.0407 -0.0112 12 6 16 2.6034 0.0152 12 6 17 1.6205 -0.1633 12 6 18 2.4549 -0.1821 12 6 19 0.9442 -0.3448 12 6 20 1.6566 -0.3629 12 6 21 0.3041 -0.4928 12 7 12 -1.8142 -0.0994 12 7 13 -0.8479 -0.2550 12 7 14 -1.8939 -0.1592 12 7 15 -1.9122 -0.2369 12 7 16 -1.6369 -0.1487 12 7 17 -2.2697 -0.0739 12 7 18 -1.2262 -0.0508 12 7 19 -1.9035 0.1669 12 8 12 0.1688 0.1268 12 8 13 1.2503 0.3103 12 8 14 0.7001 0.1894 12 8 15 0.8294 0.3781 12 8 16 1.0801 0.1387 12 8 17 0.3557 0.3765 12 9 12 -1.2160 -0.3541 12 9 13 -0.0978 -0.0561 12 9 14 -0.7610 -0.3231 13 0 13 1.1232 0.5402 13 0 15 0.9268 -0.1589 13 0 17 0.2368 -0.4427 13 0 19 -0.8854 -0.2573 13 0 21 -1.9911 0.1503 13 1 13 -0.0958 -0.1553 13 1 14 -0.6358 0.0765 13 1 15 0.3456 -0.1665 13 1 16 -0.5173 0.4316 13 1 17 0.7065 -0.2076 13 1 18 0.0300 0.3676 13 1 19 0.8794 -0.2041 13 1 20 0.8413 0.0104 13 1 21 0.8364 -0.1141 13 1 22 1.5012 -0.3432 13 2 13 -0.3881 -0.1078 13 2 14 -0.1092 -0.0486 13 2 15 0.0567 -0.2758 13 2 16 -0.6202 0.0220 13 2 17 0.3802 -0.2167 13 2 18 -0.9459 0.0850 13 2 19 0.4516 0.0391 13 2 20 -0.9686 0.0503 13 2 21 0.3166 0.3068 13 2 22 -0.7150 -0.0883 13 3 13 -0.3219 0.1332 13 3 14 0.3228 0.1666 13 3 15 0.0329 0.0836 13 3 16 -0.2255 0.0559 13 3 17 0.4274 -0.0111 13 3 18 -0.7550 -0.1438 13 3 19 0.6290 -0.0589 13 3 20 -1.1424 -0.3287 13 3 21 0.5237 -0.0065 13 4 13 0.3873 -0.0791 13 4 14 0.7622 -0.0738 13 4 15 0.7141 -0.0231 13 4 16 0.3532 -0.0515 13 4 17 0.9302 0.0902 13 4 18 -0.1739 -0.0036 13 4 19 1.0834 0.2066 13 4 20 -0.4977 0.0143 13 4 21 1.1653 0.2609 13 5 13 -1.5839 0.0627 13 5 14 -1.8297 -0.0946 13 5 15 -1.3680 0.1600 13 5 16 -1.8500 -0.0586 13 5 17 -0.6488 0.2035 13 5 18 -1.4456 -0.0331 13 5 19 0.1412 0.2071 13 6 13 2.0197 0.3622 13 6 14 2.1349 -0.1332 13 6 15 2.5368 0.2620 13 6 16 1.6378 -0.2274 13 6 17 2.1790 0.0973 13 6 18 0.7831 -0.2907 13 7 13 -2.0537 -0.1388 13 7 14 -1.8715 -0.4624 13 7 15 -1.9594 -0.1078 13 7 16 -2.0674 -0.3132 13 8 13 0.5334 0.3626 13 8 14 1.5143 0.4624 14 0 14 1.5856 -0.1552 14 0 16 1.4860 -0.5100 14 0 18 0.7548 -0.4634 14 0 20 -0.2389 -0.1129 14 1 14 -0.1917 -0.0936 14 1 15 -1.0599 0.4440 14 1 16 0.2476 -0.1948 14 1 17 -0.8688 0.5140 14 1 18 0.7273 -0.2784 14 1 19 -0.2222 0.2628 14 1 20 1.0789 -0.2687 14 2 14 -0.1322 -0.2422 14 2 15 0.6517 -0.1578 14 2 16 0.2595 -0.2966 14 2 17 0.0120 -0.0175 14 2 18 0.3356 -0.1638 14 2 19 -0.6499 0.0807 14 3 14 -1.7548 0.2666 14 3 15 -0.0149 0.0585 14 3 16 -1.3245 0.1538 14 3 17 -0.3358 -0.0472 14 3 18 -0.6326 0.0028 14 3 19 -0.5163 -0.1545 14 4 14 1.1539 0.0327 14 4 15 1.9576 -0.1802 14 4 16 1.0352 0.1409 14 4 17 1.3189 -0.0585 14 4 18 0.9141 0.2154 14 5 14 -1.9987 0.3027 14 5 15 -2.2997 -0.1788 14 5 16 -1.3554 0.2750 14 6 14 2.7972 0.3398 14 6 15 1.5033 -0.3807 15 0 15 1.3926 -0.3762 15 0 17 1.2856 -0.5048 15 1 15 -0.2434 0.1050 15 1 16 -0.7362 0.3653 15 1 17 0.2360 -0.0929 15 2 15 -0.4129 -0.1098 15 2 16 0.8398 -0.3117 15 3 15 -2.1292 0.3897 0 0 0 0.0 0.0 ; _shelx_fab_checksum 71207 _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 0.40445(2) 0.28849(2) 0.64159(2) 0.01425(6) Uani 1 1 d . . . . . O1 O 0.3756(3) 0.2124(3) 0.71869(11) 0.0189(7) Uani 1 1 d . . . . . O2 O 0.4333(2) 0.3701(3) 0.56323(10) 0.0185(7) Uani 1 1 d . . . . . O3 O 0.2220(2) 0.3722(3) 0.65476(10) 0.0195(7) Uani 1 1 d . . . . . O4 O 0.2332(2) 0.3448(3) 0.58055(11) 0.0196(7) Uani 1 1 d . . . . . O5 O 0.1073(3) 0.4586(3) 0.59766(12) 0.0268(8) Uani 1 1 d . . . . . O6 O 0.2638(2) 0.1251(3) 0.63475(11) 0.0195(7) Uani 1 1 d . . . . . O7 O 0.3393(2) 0.1295(3) 0.57354(11) 0.0214(7) Uani 1 1 d . . . . . O8 O 0.2139(3) -0.0014(3) 0.57579(12) 0.0279(8) Uani 1 1 d . . . . . O9 O 0.4788(3) 0.0722(3) 0.65884(11) 0.0230(7) Uani 1 1 d . . . . . O10 O 0.5558(3) 0.1833(3) 0.61343(12) 0.0223(7) Uani 1 1 d . . . . . O11 O 0.6054(3) -0.0069(3) 0.62714(14) 0.0374(10) Uani 1 1 d . . . . . O12 O 0.5742(3) 0.2832(3) 0.70725(12) 0.0210(7) Uani 1 1 d . . . . . O13 O 0.5673(2) 0.4269(3) 0.65405(11) 0.0195(7) Uani 1 1 d . . . . . O14 O 0.7100(3) 0.4022(3) 0.70884(14) 0.0362(9) Uani 1 1 d . . . . . N1 N 0.3961(3) 0.4458(3) 0.71293(12) 0.0146(8) Uani 1 1 d . . . . . N2 N 0.3771(3) 0.5283(4) 0.62221(13) 0.0179(8) Uani 1 1 d . . . . . N3 N 0.4443(3) 0.2043(3) 0.79763(13) 0.0212(9) Uani 1 1 d D . . . . N4 N 0.3572(3) 0.4748(4) 0.49701(13) 0.0201(9) Uani 1 1 d D . . . . N5 N 0.1838(3) 0.3926(3) 0.61046(14) 0.0185(8) Uani 1 1 d . . . . . N6 N 0.2704(3) 0.0810(3) 0.59369(13) 0.0184(8) Uani 1 1 d . . . . . N7 N 0.5503(3) 0.0792(4) 0.63310(14) 0.0232(9) Uani 1 1 d . . . . . N8 N 0.6214(3) 0.3734(4) 0.69095(14) 0.0218(9) Uani 1 1 d . . . . . C1 C 0.4065(4) 0.2657(4) 0.75815(16) 0.0181(10) Uani 1 1 d . . . . . C2 C 0.3957(3) 0.4030(4) 0.75703(15) 0.0147(9) Uani 1 1 d . . . . . C3 C 0.3775(3) 0.4773(4) 0.79474(16) 0.0178(10) Uani 1 1 d . . . . . H3 H 0.375447 0.443353 0.825297 0.021 Uiso 1 1 calc R U . . . C4 C 0.3628(3) 0.5997(4) 0.78653(16) 0.0183(10) Uani 1 1 d . . . . . H4 H 0.350554 0.651574 0.811669 0.022 Uiso 1 1 calc R U . . . C5 C 0.3655(3) 0.6493(4) 0.74128(16) 0.0190(10) Uani 1 1 d . . . . . C6 C 0.3799(3) 0.5677(4) 0.70513(15) 0.0147(9) Uani 1 1 d . . . . . C7 C 0.3744(3) 0.6103(4) 0.65703(16) 0.0160(9) Uani 1 1 d . . . . . C8 C 0.3656(4) 0.7374(4) 0.64763(17) 0.0187(10) Uani 1 1 d . . . . . C9 C 0.3567(4) 0.8202(4) 0.68631(18) 0.0219(11) Uani 1 1 d . . . . . H9 H 0.352417 0.905716 0.680499 0.026 Uiso 1 1 calc R U . . . C10 C 0.3544(4) 0.7769(4) 0.73068(18) 0.0219(10) Uani 1 1 d . . . . . H10 H 0.345335 0.832358 0.755255 0.026 Uiso 1 1 calc R U . . . C11 C 0.3658(4) 0.7749(4) 0.60083(18) 0.0222(11) Uani 1 1 d . . . . . H11 H 0.365396 0.859603 0.593415 0.027 Uiso 1 1 calc R U . . . C12 C 0.3667(4) 0.6902(4) 0.56549(17) 0.0231(11) Uani 1 1 d . . . . . H12 H 0.363774 0.715305 0.533263 0.028 Uiso 1 1 calc R U . . . C13 C 0.3719(3) 0.5670(4) 0.57746(16) 0.0174(10) Uani 1 1 d . . . . . C14 C 0.3860(3) 0.4637(4) 0.54407(15) 0.0159(9) Uani 1 1 d . . . . . C15 C 0.4492(4) 0.0690(4) 0.79595(17) 0.0243(11) Uani 1 1 d . . . . . H15A H 0.395706 0.039025 0.768711 0.029 Uiso 1 1 calc R U . . . H15B H 0.432317 0.035116 0.825830 0.029 Uiso 1 1 calc R U . . . C16 C 0.5552(4) 0.0239(5) 0.7904(2) 0.0360(13) Uani 1 1 d . . . . . H16A H 0.570490 0.053214 0.759953 0.054 Uiso 1 1 calc R U . . . H16B H 0.555767 -0.065682 0.790749 0.054 Uiso 1 1 calc R U . . . H16C H 0.608619 0.054605 0.817002 0.054 Uiso 1 1 calc R U . . . C17 C 0.5023(14) 0.2627(16) 0.8410(4) 0.0251(15) Uani 0.5 1 d DG . P A 1 C18 C 0.4714(10) 0.2531(13) 0.8850(5) 0.032(3) Uani 0.5 1 d G . P A 1 H18 H 0.415540 0.199964 0.888411 0.038 Uiso 0.5 1 calc R U P A 1 C19 C 0.5223(7) 0.3211(9) 0.9239(3) 0.030(2) Uani 0.5 1 d G . P A 1 H19 H 0.501147 0.314533 0.954008 0.036 Uiso 0.5 1 calc R U P A 1 C20 C 0.6040(8) 0.3988(9) 0.9189(2) 0.035(3) Uani 0.5 1 d DG . P A 1 C21 C 0.6349(11) 0.4084(12) 0.8749(3) 0.031(3) Uani 0.5 1 d G . P A 1 H21 H 0.690812 0.461506 0.871508 0.037 Uiso 0.5 1 calc R U P A 1 C22 C 0.5841(14) 0.3404(15) 0.8360(2) 0.030(2) Uani 0.5 1 d G . P A 1 H22 H 0.605206 0.346938 0.805910 0.036 Uiso 0.5 1 calc R U P A 1 C17A C 0.4887(14) 0.2629(16) 0.8410(3) 0.0251(15) Uani 0.5 1 d DG . P A 2 C18A C 0.4406(10) 0.2460(13) 0.8801(5) 0.031(3) Uani 0.5 1 d G . P A 2 H18A H 0.380048 0.195809 0.877136 0.037 Uiso 0.5 1 calc R U P A 2 C19A C 0.4812(7) 0.3023(9) 0.9236(3) 0.0277(19) Uani 0.5 1 d G . P A 2 H19A H 0.448318 0.290748 0.950350 0.033 Uiso 0.5 1 calc R U P A 2 C20A C 0.5698(7) 0.3757(9) 0.9280(2) 0.031(3) Uani 0.5 1 d DG . P A 2 C21A C 0.6179(9) 0.3927(11) 0.8889(3) 0.030(3) Uani 0.5 1 d G . P A 2 H21A H 0.678508 0.442823 0.891926 0.036 Uiso 0.5 1 calc R U P A 2 C22A C 0.5774(13) 0.3363(14) 0.8454(3) 0.0277(19) Uani 0.5 1 d G . P A 2 H22A H 0.610240 0.347884 0.818711 0.033 Uiso 0.5 1 calc R U P A 2 C23 C 0.657(2) 0.471(3) 0.9629(7) 0.069(7) Uani 0.5 1 d D . P A 1 H23A H 0.604997 0.523154 0.973785 0.103 Uiso 0.5 1 d R U P A 1 H23B H 0.686199 0.413353 0.988546 0.103 Uiso 0.5 1 d R U P A 1 H23C H 0.713109 0.521135 0.954862 0.103 Uiso 0.5 1 d R U P A 1 C23A C 0.615(2) 0.447(3) 0.9735(7) 0.069(7) Uani 0.5 1 d D . P A 2 H23D H 0.562098 0.503478 0.981099 0.103 Uiso 0.5 1 d R U P A 2 H23E H 0.635261 0.389199 1.000182 0.103 Uiso 0.5 1 d R U P A 2 H23F H 0.676535 0.492538 0.968594 0.103 Uiso 0.5 1 d R U P A 2 C24 C 0.3884(4) 0.3781(5) 0.46638(17) 0.0330(13) Uani 1 1 d D . . . . H24A H 0.402536 0.415379 0.436549 0.040 Uiso 0.915(9) 1 calc R U P B 1 H24B H 0.454141 0.339551 0.483381 0.040 Uiso 0.915(9) 1 calc R U P B 1 H24C H 0.384099 0.298110 0.482163 0.040 Uiso 0.085(9) 1 calc R U P B 2 H24D H 0.462534 0.391251 0.463955 0.040 Uiso 0.085(9) 1 calc R U P B 2 C25 C 0.3070(5) 0.2832(6) 0.4539(2) 0.0403(17) Uani 0.915(9) 1 d . . P B 1 H25A H 0.331055 0.221175 0.433589 0.061 Uiso 0.915(9) 1 calc R U P B 1 H25B H 0.293808 0.244783 0.483252 0.061 Uiso 0.915(9) 1 calc R U P B 1 H25C H 0.242206 0.320605 0.436423 0.061 Uiso 0.915(9) 1 calc R U P B 1 C25A C 0.323(4) 0.373(5) 0.4168(10) 0.0403(17) Uani 0.085(9) 1 d D . P B 2 H25D H 0.348597 0.306592 0.398772 0.061 Uiso 0.085(9) 1 calc R U P B 2 H25E H 0.249806 0.357358 0.418645 0.061 Uiso 0.085(9) 1 calc R U P B 2 H25F H 0.328366 0.450648 0.400407 0.061 Uiso 0.085(9) 1 calc R U P B 2 C26 C 0.2781(4) 0.5589(5) 0.47376(16) 0.0218(10) Uani 1 1 d . . . . . C27 C 0.2975(4) 0.6334(5) 0.43743(16) 0.0260(11) Uani 1 1 d . . . . . H27 H 0.364958 0.634622 0.429268 0.031 Uiso 1 1 calc R U . . . C28 C 0.2181(4) 0.7064(5) 0.41297(19) 0.0299(12) Uani 1 1 d . . . . . H28 H 0.231381 0.756255 0.387443 0.036 Uiso 1 1 calc R U . . . C29 C 0.1187(4) 0.7090(5) 0.4248(2) 0.0317(13) Uani 1 1 d . . . . . C30 C 0.1026(4) 0.6350(5) 0.46267(18) 0.0304(12) Uani 1 1 d . . . . . H30 H 0.036413 0.637111 0.472115 0.036 Uiso 1 1 calc R U . . . C31 C 0.1794(4) 0.5594(5) 0.48668(18) 0.0281(12) Uani 1 1 d . . . . . H31 H 0.165893 0.507980 0.511726 0.034 Uiso 1 1 calc R U . . . C32 C 0.0311(4) 0.7826(5) 0.3960(2) 0.0426(16) Uani 1 1 d . . . . . H32A H 0.059981 0.854622 0.382779 0.064 Uiso 1 1 calc R U . . . H32B H -0.016783 0.808717 0.416804 0.064 Uiso 1 1 calc R U . . . H32C H -0.007301 0.732500 0.369788 0.064 Uiso 1 1 calc R U . . . N9 N 0.6251(5) 0.6196(7) 0.7827(3) 0.080(2) Uani 1 1 d . . . . . C33 C 0.6452(5) 0.6632(7) 0.7495(3) 0.0534(19) Uani 1 1 d . . . . . C34 C 0.6690(6) 0.7188(6) 0.7072(3) 0.0575(19) Uani 1 1 d . . . . . H34A H 0.651820 0.661845 0.680152 0.086 Uiso 1 1 calc R U . . . H34B H 0.743869 0.738878 0.712580 0.086 Uiso 1 1 calc R U . . . H34C H 0.627621 0.793675 0.699814 0.086 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 0.01842(10) 0.01452(10) 0.01028(9) -0.00047(6) 0.00394(6) -0.00042(7) O1 0.0259(18) 0.0204(18) 0.0107(15) -0.0026(13) 0.0046(13) -0.0032(14) O2 0.0207(17) 0.0234(17) 0.0120(15) 0.0007(13) 0.0042(13) 0.0004(14) O3 0.0251(18) 0.0204(17) 0.0129(15) -0.0003(13) 0.0039(13) -0.0006(14) O4 0.0238(18) 0.0213(17) 0.0148(16) -0.0012(13) 0.0071(13) -0.0003(14) O5 0.0250(19) 0.030(2) 0.0242(18) -0.0015(15) 0.0022(15) 0.0092(16) O6 0.0282(18) 0.0175(16) 0.0135(15) -0.0061(13) 0.0057(13) -0.0052(14) O7 0.0224(17) 0.0259(18) 0.0177(16) 0.0008(14) 0.0082(14) -0.0030(15) O8 0.034(2) 0.0224(19) 0.0239(19) -0.0032(15) -0.0022(15) -0.0093(16) O9 0.032(2) 0.0216(18) 0.0184(17) -0.0016(14) 0.0128(15) -0.0028(15) O10 0.0263(19) 0.0198(17) 0.0241(18) 0.0037(14) 0.0128(15) 0.0005(14) O11 0.045(2) 0.026(2) 0.046(2) 0.0035(18) 0.022(2) 0.0230(18) O12 0.0245(18) 0.0197(18) 0.0196(17) 0.0038(13) 0.0060(14) 0.0010(14) O13 0.0223(18) 0.0157(17) 0.0199(17) 0.0023(13) 0.0025(14) -0.0036(14) O14 0.021(2) 0.035(2) 0.047(2) 0.0046(18) -0.0077(17) -0.0080(16) N1 0.0142(19) 0.0153(19) 0.0135(18) -0.0001(15) 0.0008(15) -0.0031(15) N2 0.0140(19) 0.027(2) 0.0126(18) -0.0031(16) 0.0017(15) -0.0012(16) N3 0.032(2) 0.020(2) 0.0132(19) 0.0016(16) 0.0055(17) -0.0013(17) N4 0.022(2) 0.026(2) 0.0118(19) 0.0013(16) 0.0039(16) 0.0033(17) N5 0.020(2) 0.016(2) 0.020(2) 0.0022(16) 0.0077(17) -0.0007(16) N6 0.021(2) 0.017(2) 0.0156(19) -0.0029(16) -0.0005(16) 0.0002(16) N7 0.029(2) 0.022(2) 0.019(2) 0.0007(17) 0.0058(18) -0.0037(18) N8 0.025(2) 0.019(2) 0.021(2) -0.0008(17) 0.0047(17) 0.0010(18) C1 0.017(2) 0.023(2) 0.015(2) -0.0001(19) 0.0045(18) -0.0009(19) C2 0.015(2) 0.014(2) 0.015(2) -0.0033(17) 0.0027(17) -0.0032(17) C3 0.015(2) 0.023(2) 0.014(2) -0.0035(19) 0.0009(18) -0.0016(19) C4 0.019(2) 0.022(2) 0.015(2) -0.0037(18) 0.0066(18) 0.0010(19) C5 0.017(2) 0.021(2) 0.019(2) -0.0037(19) 0.0035(18) -0.0011(19) C6 0.013(2) 0.018(2) 0.014(2) -0.0014(17) 0.0020(17) -0.0015(18) C7 0.016(2) 0.014(2) 0.019(2) 0.0015(18) 0.0061(18) 0.0011(18) C8 0.016(2) 0.018(2) 0.023(2) 0.0013(19) 0.0065(19) 0.0037(19) C9 0.024(3) 0.015(2) 0.029(3) -0.0009(19) 0.009(2) 0.0000(19) C10 0.025(3) 0.016(2) 0.026(3) -0.0050(19) 0.008(2) -0.002(2) C11 0.028(3) 0.013(2) 0.027(3) 0.0060(19) 0.010(2) 0.0030(19) C12 0.028(3) 0.027(3) 0.017(2) 0.006(2) 0.011(2) 0.005(2) C13 0.017(2) 0.019(2) 0.017(2) 0.0012(18) 0.0045(18) 0.0053(19) C14 0.017(2) 0.016(2) 0.015(2) 0.0038(18) 0.0036(18) 0.0021(18) C15 0.035(3) 0.018(2) 0.020(2) 0.003(2) 0.005(2) -0.003(2) C16 0.041(3) 0.025(3) 0.042(3) -0.003(2) 0.008(3) 0.009(3) C17 0.036(4) 0.021(2) 0.015(2) -0.0001(18) -0.002(2) 0.013(2) C18 0.045(8) 0.032(6) 0.015(4) 0.001(3) -0.002(4) 0.006(5) C19 0.038(4) 0.032(4) 0.017(3) -0.002(3) -0.003(3) 0.006(3) C20 0.048(7) 0.038(6) 0.015(5) 0.005(5) -0.001(5) 0.000(5) C21 0.048(7) 0.028(6) 0.011(5) 0.002(4) -0.005(4) 0.003(4) C22 0.038(4) 0.032(4) 0.017(3) -0.002(3) -0.003(3) 0.006(3) C17A 0.036(4) 0.021(2) 0.015(2) -0.0001(18) -0.002(2) 0.013(2) C18A 0.035(7) 0.040(7) 0.014(4) -0.002(4) -0.004(4) 0.012(5) C19A 0.028(4) 0.034(5) 0.017(3) -0.004(3) -0.005(3) 0.014(3) C20A 0.035(8) 0.043(8) 0.015(5) -0.008(5) 0.001(5) 0.014(6) C21A 0.039(7) 0.033(7) 0.013(5) -0.003(5) -0.004(5) 0.012(5) C22A 0.028(4) 0.034(5) 0.017(3) -0.004(3) -0.005(3) 0.014(3) C23 0.086(18) 0.075(12) 0.034(9) -0.023(9) -0.018(8) 0.018(11) C23A 0.086(18) 0.075(12) 0.034(9) -0.023(9) -0.018(8) 0.018(11) C24 0.037(3) 0.046(3) 0.015(2) -0.009(2) 0.005(2) 0.009(3) C25 0.042(4) 0.039(4) 0.040(4) -0.013(3) 0.008(3) -0.009(3) C25A 0.042(4) 0.039(4) 0.040(4) -0.013(3) 0.008(3) -0.009(3) C26 0.022(3) 0.031(3) 0.011(2) 0.003(2) 0.0004(18) 0.001(2) C27 0.025(3) 0.034(3) 0.019(2) 0.004(2) 0.004(2) -0.001(2) C28 0.029(3) 0.037(3) 0.023(3) 0.011(2) 0.004(2) -0.002(2) C29 0.024(3) 0.036(3) 0.032(3) 0.012(2) -0.004(2) -0.005(2) C30 0.019(3) 0.041(3) 0.031(3) 0.009(3) 0.004(2) 0.003(2) C31 0.026(3) 0.036(3) 0.022(3) 0.008(2) 0.004(2) -0.002(2) C32 0.026(3) 0.047(4) 0.051(4) 0.029(3) 0.000(3) 0.002(3) N9 0.052(4) 0.084(5) 0.110(6) 0.006(5) 0.033(4) -0.013(4) C33 0.030(4) 0.046(4) 0.085(6) -0.012(4) 0.013(4) -0.007(3) C34 0.055(5) 0.055(5) 0.060(5) -0.010(4) 0.006(4) -0.007(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 178.98(10) . . ? O1 Th1 O3 71.98(10) . . ? O1 Th1 O4 114.56(10) . . ? O1 Th1 O6 66.00(10) . . ? O1 Th1 O7 110.63(10) . . ? O1 Th1 O9 68.41(10) . . ? O1 Th1 O10 113.12(11) . . ? O1 Th1 O12 66.76(10) . . ? O1 Th1 O13 110.14(10) . . ? O1 Th1 N1 60.23(10) . . ? O1 Th1 N2 118.63(10) . . ? O2 Th1 O3 107.38(9) . . ? O2 Th1 O4 65.19(9) . . ? O2 Th1 O6 114.55(10) . . ? O2 Th1 O7 70.21(10) . . ? O2 Th1 O9 112.57(10) . . ? O2 Th1 O10 67.67(10) . . ? O2 Th1 O12 113.25(10) . . ? O2 Th1 O13 69.44(10) . . ? O2 Th1 N1 118.77(10) . . ? O2 Th1 N2 60.35(11) . . ? O3 Th1 N1 59.88(10) . . ? O3 Th1 N2 66.63(10) . . ? O4 Th1 O3 48.65(9) . . ? O4 Th1 O7 63.63(10) . . ? O4 Th1 N1 101.27(10) . . ? O4 Th1 N2 64.71(10) . . ? O6 Th1 O3 66.47(10) . . ? O6 Th1 O4 66.90(10) . . ? O6 Th1 O7 49.51(9) . . ? O6 Th1 O9 66.66(10) . . ? O6 Th1 O10 104.34(10) . . ? O6 Th1 O12 122.53(10) . . ? O6 Th1 O13 170.91(10) . . ? O6 Th1 N1 112.05(10) . . ? O6 Th1 N2 127.36(11) . . ? O7 Th1 O3 99.56(10) . . ? O7 Th1 N1 158.75(10) . . ? O7 Th1 N2 119.12(10) . . ? O9 Th1 O3 127.49(10) . . ? O9 Th1 O4 125.73(10) . . ? O9 Th1 O7 65.37(10) . . ? O9 Th1 O12 66.86(10) . . ? O9 Th1 O13 104.35(10) . . ? O9 Th1 N1 121.16(10) . . ? O9 Th1 N2 165.48(10) . . ? O10 Th1 O3 167.38(10) . . ? O10 Th1 O4 120.62(10) . . ? O10 Th1 O7 67.93(10) . . ? O10 Th1 O9 49.95(10) . . ? O10 Th1 O12 67.34(10) . . ? O10 Th1 O13 69.07(10) . . ? O10 Th1 N1 132.73(11) . . ? O10 Th1 N2 117.21(10) . . ? O12 Th1 O3 124.55(9) . . ? O12 Th1 O4 167.34(10) . . ? O12 Th1 O7 128.54(10) . . ? O12 Th1 N1 67.97(10) . . ? O12 Th1 N2 103.22(10) . . ? O13 Th1 O3 121.00(10) . . ? O13 Th1 O4 121.60(10) . . ? O13 Th1 O7 129.23(10) . . ? O13 Th1 O12 49.69(10) . . ? O13 Th1 N1 70.80(10) . . ? O13 Th1 N2 61.71(10) . . ? N1 Th1 N2 60.32(11) . . ? C1 O1 Th1 124.3(3) . . ? C14 O2 Th1 122.0(3) . . ? N5 O3 Th1 96.2(2) . . ? N5 O4 Th1 97.4(2) . . ? N6 O6 Th1 99.2(2) . . ? N6 O7 Th1 95.7(2) . . ? N7 O9 Th1 97.1(2) . . ? N7 O10 Th1 98.8(2) . . ? N8 O12 Th1 97.0(2) . . ? N8 O13 Th1 98.5(2) . . ? C2 N1 Th1 119.5(3) . . ? C2 N1 C6 117.8(4) . . ? C6 N1 Th1 122.3(3) . . ? C7 N2 Th1 121.5(3) . . ? C13 N2 Th1 119.1(3) . . ? C13 N2 C7 119.3(4) . . ? C1 N3 C15 119.5(4) . . ? C1 N3 C17 122.8(8) . . ? C1 N3 C17A 122.3(9) . . ? C17 N3 C15 116.5(8) . . ? C17A N3 C15 118.0(9) . . ? C14 N4 C24 118.3(4) . . ? C14 N4 C26 123.9(4) . . ? C26 N4 C24 116.2(4) . . ? O4 N5 O3 115.9(4) . . ? O5 N5 O3 122.1(4) . . ? O5 N5 O4 122.0(4) . . ? O6 N6 Th1 56.1(2) . . ? O7 N6 Th1 59.6(2) . . ? O7 N6 O6 115.6(3) . . ? O8 N6 Th1 177.3(3) . . ? O8 N6 O6 121.3(4) . . ? O8 N6 O7 123.0(4) . . ? O9 N7 Th1 57.7(2) . . ? O10 N7 Th1 56.5(2) . . ? O10 N7 O9 114.1(4) . . ? O11 N7 Th1 176.2(3) . . ? O11 N7 O9 122.8(4) . . ? O11 N7 O10 123.0(4) . . ? O12 N8 Th1 58.0(2) . . ? O13 N8 Th1 56.8(2) . . ? O13 N8 O12 114.7(4) . . ? O14 N8 Th1 176.0(3) . . ? O14 N8 O12 121.9(4) . . ? O14 N8 O13 123.4(4) . . ? O1 C1 N3 121.6(4) . . ? O1 C1 C2 115.5(4) . . ? N3 C1 C2 122.9(4) . . ? N1 C2 C1 110.6(4) . . ? N1 C2 C3 123.0(4) . . ? C3 C2 C1 126.2(4) . . ? C2 C3 H3 120.8 . . ? C4 C3 C2 118.5(4) . . ? C4 C3 H3 120.8 . . ? C3 C4 H4 119.7 . . ? C3 C4 C5 120.5(4) . . ? C5 C4 H4 119.7 . . ? C4 C5 C10 123.5(4) . . ? C6 C5 C4 117.2(4) . . ? C6 C5 C10 119.4(4) . . ? N1 C6 C5 122.9(4) . . ? N1 C6 C7 116.8(4) . . ? C5 C6 C7 120.2(4) . . ? N2 C7 C6 118.9(4) . . ? N2 C7 C8 122.0(4) . . ? C8 C7 C6 119.1(4) . . ? C7 C8 C9 119.1(4) . . ? C11 C8 C7 117.0(4) . . ? C11 C8 C9 123.8(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C5 C10 H10 119.4 . . ? C9 C10 C5 121.3(4) . . ? C9 C10 H10 119.4 . . ? C8 C11 H11 119.9 . . ? C12 C11 C8 120.2(4) . . ? C12 C11 H11 119.9 . . ? C11 C12 H12 120.5 . . ? C11 C12 C13 119.0(4) . . ? C13 C12 H12 120.5 . . ? N2 C13 C12 122.3(4) . . ? N2 C13 C14 111.9(4) . . ? C12 C13 C14 125.4(4) . . ? O2 C14 N4 121.9(4) . . ? O2 C14 C13 116.4(4) . . ? N4 C14 C13 121.4(4) . . ? N3 C15 H15A 109.2 . . ? N3 C15 H15B 109.2 . . ? N3 C15 C16 112.2(4) . . ? H15A C15 H15B 107.9 . . ? C16 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? 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 122.3(11) . . ? C18 C17 C22 120.0 . . ? C22 C17 N3 117.4(10) . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 H19 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 C23 117.5(11) . . ? C21 C20 C23 122.5(11) . . ? C20 C21 H21 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 H22 120.0 . . ? C21 C22 C17 120.0 . . ? C21 C22 H22 120.0 . . ? C18A C17A N3 117.9(11) . . ? C18A C17A C22A 120.0 . . ? C22A C17A N3 122.1(11) . . ? C17A C18A H18A 120.0 . . ? C19A C18A C17A 120.0 . . ? C19A C18A H18A 120.0 . . ? C18A C19A H19A 120.0 . . ? C18A C19A C20A 120.0 . . ? C20A C19A H19A 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A C23A 123.0(10) . . ? C21A C20A C23A 116.9(10) . . ? C20A C21A H21A 120.0 . . ? C22A C21A C20A 120.0 . . ? C22A C21A H21A 120.0 . . ? C17A C22A H22A 120.0 . . ? C21A C22A C17A 120.0 . . ? C21A C22A H22A 120.0 . . ? C20 C23 H23A 109.6 . . ? C20 C23 H23B 109.2 . . ? C20 C23 H23C 109.7 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20A C23A H23D 109.9 . . ? C20A C23A H23E 109.3 . . ? C20A C23A H23F 109.2 . . ? H23D C23A H23E 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? N4 C24 H24A 109.1 . . ? N4 C24 H24B 109.1 . . ? N4 C24 H24C 108.7 . . ? N4 C24 H24D 108.7 . . ? N4 C24 C25A 114.4(16) . . ? H24A C24 H24B 107.9 . . ? H24C C24 H24D 107.6 . . ? C25 C24 N4 112.3(5) . . ? C25 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C25A C24 H24C 108.7 . . ? C25A C24 H24D 108.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C25A H25D 109.5 . . ? C24 C25A H25E 109.5 . . ? C24 C25A H25F 109.5 . . ? H25D C25A H25E 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C27 C26 N4 120.2(4) . . ? C27 C26 C31 120.3(4) . . ? C31 C26 N4 119.3(4) . . ? C26 C27 H27 120.3 . . ? C26 C27 C28 119.4(5) . . ? C28 C27 H27 120.3 . . ? C27 C28 H28 119.1 . . ? C27 C28 C29 121.8(5) . . ? C29 C28 H28 119.1 . . ? C28 C29 C32 121.3(5) . . ? C30 C29 C28 117.4(5) . . ? C30 C29 C32 121.2(5) . . ? C29 C30 H30 119.0 . . ? C31 C30 C29 121.9(5) . . ? C31 C30 H30 119.0 . . ? C26 C31 H31 120.4 . . ? C30 C31 C26 119.1(5) . . ? C30 C31 H31 120.4 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N9 C33 C34 179.1(8) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 2.441(3) . ? Th1 O2 2.495(3) . ? Th1 O3 2.637(3) . ? Th1 O4 2.615(3) . ? Th1 O6 2.537(3) . ? Th1 O7 2.616(3) . ? Th1 O9 2.567(3) . ? Th1 O10 2.541(3) . ? Th1 O12 2.597(3) . ? Th1 O13 2.571(3) . ? Th1 N1 2.679(4) . ? Th1 N2 2.691(4) . ? O1 C1 1.258(5) . ? O2 C14 1.262(5) . ? O3 N5 1.279(5) . ? O4 N5 1.273(5) . ? O5 N5 1.226(5) . ? O6 N6 1.281(5) . ? O7 N6 1.270(5) . ? O8 N6 1.211(5) . ? O9 N7 1.293(5) . ? O10 N7 1.277(5) . ? O11 N7 1.216(5) . ? O12 N8 1.295(5) . ? O13 N8 1.284(5) . ? O14 N8 1.207(5) . ? N1 C2 1.339(5) . ? N1 C6 1.361(6) . ? N2 C7 1.341(6) . ? N2 C13 1.330(5) . ? N3 C1 1.318(6) . ? N3 C15 1.483(6) . ? N3 C17 1.460(6) . ? N3 C17A 1.410(6) . ? N4 C14 1.322(5) . ? N4 C24 1.477(6) . ? N4 C26 1.441(6) . ? C1 C2 1.509(6) . ? C2 C3 1.402(6) . ? C3 H3 0.9500 . ? C3 C4 1.366(6) . ? C4 H4 0.9500 . ? C4 C5 1.403(6) . ? C5 C6 1.401(6) . ? C5 C10 1.430(7) . ? C6 C7 1.433(6) . ? C7 C8 1.417(6) . ? C8 C9 1.447(7) . ? C8 C11 1.393(7) . ? C9 H9 0.9500 . ? C9 C10 1.353(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C11 C12 1.368(7) . ? C12 H12 0.9500 . ? C12 C13 1.389(6) . ? C13 C14 1.511(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.501(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 H18 0.9500 . ? C18 C19 1.3900 . ? C19 H19 0.9500 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 C23 1.522(15) . ? C21 H21 0.9500 . ? C21 C22 1.3900 . ? C22 H22 0.9500 . ? C17A C18A 1.3900 . ? C17A C22A 1.3900 . ? C18A H18A 0.9500 . ? C18A C19A 1.3900 . ? C19A H19A 0.9500 . ? C19A C20A 1.3900 . ? C20A C21A 1.3900 . ? C20A C23A 1.524(15) . ? C21A H21A 0.9500 . ? C21A C22A 1.3900 . ? C22A H22A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9900 . ? C24 H24D 0.9900 . ? C24 C25 1.475(8) . ? C24 C25A 1.498(19) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26 C27 1.377(6) . ? C26 C31 1.402(7) . ? C27 H27 0.9500 . ? C27 C28 1.381(7) . ? C28 H28 0.9500 . ? C28 C29 1.397(8) . ? C29 C30 1.396(7) . ? C29 C32 1.500(7) . ? C30 H30 0.9500 . ? C30 C31 1.372(7) . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N9 C33 1.133(9) . ? C33 C34 1.435(10) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 -140.8(4) . . . . ? Th1 O1 C1 C2 39.9(5) . . . . ? Th1 O2 C14 N4 -145.6(3) . . . . ? Th1 O2 C14 C13 39.4(5) . . . . ? Th1 O3 N5 O4 13.7(4) . . . . ? Th1 O3 N5 O5 -163.0(4) . . . . ? Th1 O4 N5 O3 -13.8(4) . . . . ? Th1 O4 N5 O5 162.9(4) . . . . ? Th1 O6 N6 O7 0.8(4) . . . . ? Th1 O6 N6 O8 -179.1(3) . . . . ? Th1 O7 N6 O6 -0.8(4) . . . . ? Th1 O7 N6 O8 179.2(4) . . . . ? Th1 O9 N7 O10 2.6(4) . . . . ? Th1 O9 N7 O11 -175.5(4) . . . . ? Th1 O10 N7 O9 -2.6(4) . . . . ? Th1 O10 N7 O11 175.5(4) . . . . ? Th1 O12 N8 O13 3.3(4) . . . . ? Th1 O12 N8 O14 -175.3(4) . . . . ? Th1 O13 N8 O12 -3.3(4) . . . . ? Th1 O13 N8 O14 175.3(4) . . . . ? Th1 N1 C2 C1 3.1(5) . . . . ? Th1 N1 C2 C3 -171.2(3) . . . . ? Th1 N1 C6 C5 173.8(3) . . . . ? Th1 N1 C6 C7 -4.1(5) . . . . ? Th1 N2 C7 C6 -3.9(5) . . . . ? Th1 N2 C7 C8 176.6(3) . . . . ? Th1 N2 C13 C12 -174.5(4) . . . . ? Th1 N2 C13 C14 -1.6(5) . . . . ? O1 C1 C2 N1 -25.2(6) . . . . ? O1 C1 C2 C3 148.9(4) . . . . ? N1 C2 C3 C4 -2.2(7) . . . . ? N1 C6 C7 N2 5.2(6) . . . . ? N1 C6 C7 C8 -175.3(4) . . . . ? N2 C7 C8 C9 176.2(4) . . . . ? N2 C7 C8 C11 -3.6(7) . . . . ? N2 C13 C14 O2 -22.7(6) . . . . ? N2 C13 C14 N4 162.3(4) . . . . ? N3 C1 C2 N1 155.6(4) . . . . ? N3 C1 C2 C3 -30.4(7) . . . . ? N3 C17 C18 C19 -172.9(16) . . . . ? N3 C17 C22 C21 173.2(15) . . . . ? N3 C17A C18A C19A -179.7(15) . . . . ? N3 C17A C22A C21A 179.7(16) . . . . ? N4 C26 C27 C28 174.9(5) . . . . ? N4 C26 C31 C30 -176.6(5) . . . . ? C1 N3 C15 C16 96.5(5) . . . . ? C1 N3 C17 C18 123.3(8) . . . . ? C1 N3 C17 C22 -49.8(13) . . . . ? C1 N3 C17A C18A 117.7(8) . . . . ? C1 N3 C17A C22A -62.0(13) . . . . ? C1 C2 C3 C4 -175.6(4) . . . . ? C2 N1 C6 C5 1.5(6) . . . . ? C2 N1 C6 C7 -176.5(4) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C3 C4 C5 C6 2.3(7) . . . . ? C3 C4 C5 C10 -177.7(4) . . . . ? C4 C5 C6 N1 -3.3(7) . . . . ? C4 C5 C6 C7 174.6(4) . . . . ? C4 C5 C10 C9 -179.4(5) . . . . ? C5 C6 C7 N2 -172.8(4) . . . . ? C5 C6 C7 C8 6.7(6) . . . . ? C6 N1 C2 C1 175.6(4) . . . . ? C6 N1 C2 C3 1.3(6) . . . . ? C6 C5 C10 C9 0.6(7) . . . . ? C6 C7 C8 C9 -3.3(7) . . . . ? C6 C7 C8 C11 176.9(4) . . . . ? C7 N2 C13 C12 1.8(7) . . . . ? C7 N2 C13 C14 174.7(4) . . . . ? C7 C8 C9 C10 -1.5(7) . . . . ? C7 C8 C11 C12 4.7(7) . . . . ? C8 C9 C10 C5 2.9(7) . . . . ? C8 C11 C12 C13 -2.7(8) . . . . ? C9 C8 C11 C12 -175.1(5) . . . . ? C10 C5 C6 N1 176.7(4) . . . . ? C10 C5 C6 C7 -5.4(6) . . . . ? C11 C8 C9 C10 178.4(5) . . . . ? C11 C12 C13 N2 -0.6(7) . . . . ? C11 C12 C13 C14 -172.6(4) . . . . ? C12 C13 C14 O2 149.9(5) . . . . ? C12 C13 C14 N4 -25.1(7) . . . . ? C13 N2 C7 C6 179.9(4) . . . . ? C13 N2 C7 C8 0.4(7) . . . . ? C14 N4 C24 C25 93.3(6) . . . . ? C14 N4 C24 C25A 159(3) . . . . ? C14 N4 C26 C27 131.5(5) . . . . ? C14 N4 C26 C31 -51.9(7) . . . . ? C15 N3 C1 O1 -1.1(7) . . . . ? C15 N3 C1 C2 178.1(4) . . . . ? C15 N3 C17 C18 -69.7(12) . . . . ? C15 N3 C17 C22 117.3(9) . . . . ? C15 N3 C17A C18A -67.5(11) . . . . ? C15 N3 C17A C22A 112.8(10) . . . . ? C17 N3 C1 O1 165.6(10) . . . . ? C17 N3 C1 C2 -15.2(11) . . . . ? C17 N3 C15 C16 -71.0(10) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C17 C22 C21 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C18 C19 C20 C23 -180(2) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C17 0.0 . . . . ? C22 C17 C18 C19 0.0 . . . . ? C17A N3 C1 O1 173.6(10) . . . . ? C17A N3 C1 C2 -7.2(11) . . . . ? C17A N3 C15 C16 -78.5(10) . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C18A C17A C22A C21A 0.0 . . . . ? C18A C19A C20A C21A 0.0 . . . . ? C18A C19A C20A C23A 176(2) . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C20A C21A C22A C17A 0.0 . . . . ? C22A C17A C18A C19A 0.0 . . . . ? C23 C20 C21 C22 180(2) . . . . ? C23A C20A C21A C22A -176.4(19) . . . . ? C24 N4 C14 O2 -4.3(7) . . . . ? C24 N4 C14 C13 170.5(4) . . . . ? C24 N4 C26 C27 -63.1(6) . . . . ? C24 N4 C26 C31 113.5(5) . . . . ? C26 N4 C14 O2 160.8(4) . . . . ? C26 N4 C14 C13 -24.4(7) . . . . ? C26 N4 C24 C25 -73.0(6) . . . . ? C26 N4 C24 C25A -7(3) . . . . ? C26 C27 C28 C29 1.5(8) . . . . ? C27 C26 C31 C30 0.0(8) . . . . ? C27 C28 C29 C30 0.4(8) . . . . ? C27 C28 C29 C32 -176.2(5) . . . . ? C28 C29 C30 C31 -2.1(8) . . . . ? C29 C30 C31 C26 2.0(8) . . . . ? C31 C26 C27 C28 -1.6(8) . . . . ? C32 C29 C30 C31 174.4(5) . . . . ? 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 0.500 0.000 82.8 27.5 '3 H2O' 2 0.500 1.000 0.500 82.8 27.5 '3 H2O'