#------------------------------------------------------------------------------ #$Date: 2016-05-11 07:48:00 +0300 (Wed, 11 May 2016) $ #$Revision: 182866 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543281.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_1543281 loop_ _publ_author_name 'Rosenzweig, Michael W.' 'Scheurer, Andreas' 'Heinemann, Frank' 'Alvarez Lamsfus, Carlos' 'Maron, Laurent' 'Andrez, Julie' 'Mazzanti, M.' 'Meyer, Karsten' _publ_section_title ; Uranium(IV) Terminal Hydrosulfido and Sulfido Complexes: The Nature of the Uranium--Sulfur Bond ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C6SC00677A _journal_year 2016 _chemical_absolute_configuration ad _chemical_formula_moiety '2(C60 H79 N3 O3 S1 U1), 6.5(C H2 Cl2)' _chemical_formula_sum 'C126.5 H171 Cl13 N6 O6 S2 U2' _chemical_formula_weight 2872.71 _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Oxygen-sensitive' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_Hall 'P 6c' _space_group_name_H-M_alt 'P 63' _symmetry_space_group_name_Hall 'P 6c' _symmetry_space_group_name_H-M 'P 63' _atom_sites_solution_hydrogens mixed _audit_creation_date 2015-09-29 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _audit_update_record ; 2016-02-11 deposited with the CCDC. 2016-05-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 20.258(5) _cell_length_b 20.258(5) _cell_length_c 18.302(4) _cell_measurement_reflns_used 9633 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.16 _cell_measurement_theta_min 2.23 _cell_volume 6505(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 83.33 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'Triumph curved graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_unetI/netI 0.0364 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 165921 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.741 _diffrn_reflns_theta_min 1.161 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.839 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.6466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0916 before and 0.0796 after correction. The Ratio of minimum to maximum transmission is 0.8670. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.467 _exptl_crystal_description prism _exptl_crystal_F_000 2914 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: dichloromethane/n-pentane' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.148 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.095 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.015(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 532 _refine_ls_number_reflns 11217 _refine_ls_number_restraints 182 _refine_ls_restrained_S_all 1.160 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0307 _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^)+(0.0266P)^2^+9.1836P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.0714 _reflns_Friedel_coverage 0.941 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 10199 _reflns_number_total 11217 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6sc00677a2.cif _cod_data_source_block mr1517 _cod_original_formula_sum 'C126.50 H171 Cl13 N6 O6 S2 U2' _cod_database_code 1543281 _shelxl_version_number 2014/6 _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 0.764 _shelx_estimated_absorpt_t_min 0.574 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.985(7) 0.015(7) 2. Fixed Uiso At 1.2 times of: All C(H) groups, {H14A,H14B} of C14, {H3A,H3B} of C3, {H10A,H10B} of C100, {H11A,H11B} of C110, {H20D,H20E} of C200, {H21C,H21D} of C210, {H15A,H15B} of C15, {H16A,H16B} of C16, {H17A,H17B} of C17, {H18A,H18B} of C18, {H19A,H19B} of C19, {H21A,H21B} of C21, {H23A,H23B} of C23, {H34A,H34B} of C34, {H35A, H35B} of C35, {H36A,H36B} of C36, {H37A,H37B} of C37, {H38A,H38B} of C38, {H39A,H39B} of C39 At 1.5 times of: All C(H,H,H) groups, {H2A,H2B} of C2, {H1A,H1B} of C1, {H22A,H22B} of C22, All S(H) groups 3. Restrained distances C100-Cl11 = C100-Cl12 = C110-Cl13 = C110-Cl14 1.8 with sigma of 0.01 Cl11-Cl12 = Cl13-Cl14 = Cl21-Cl22 = Cl23-Cl24 2.9 with sigma of 0.01 C200-Cl21 = C200-Cl22 = C210-Cl23 = C210-Cl24 1.8 with sigma of 0.01 C300-Cl31 1.8 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints C100 \\sim Cl11 \\sim Cl12 \\sim C110 \\sim Cl13 \\sim Cl14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 C200 \\sim Cl21 \\sim Cl22 \\sim C210 \\sim Cl23 \\sim Cl24: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 C300 \\sim Cl31: within 1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006 Uanis(C100) \\sim Ueq, Uanis(Cl11) \\sim Ueq, Uanis(Cl12) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(Cl13) \\sim Ueq, Uanis(Cl14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C200) \\sim Ueq, Uanis(Cl21) \\sim Ueq, Uanis(Cl22) \\sim Ueq, Uanis(C210) \\sim Ueq, Uanis(Cl23) \\sim Ueq, Uanis(Cl24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C300) \\sim Ueq, Uanis(Cl31) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006 5. Same fragment restrains {C110, Cl13, Cl14} sigma for 1-2: 0.02, 1-3: 0.04 as {C100, Cl11, Cl12} {C110, Cl13, Cl14} sigma for 1-2: 0.02, 1-3: 0.04 as {C200, Cl21, Cl22} {C110, Cl13, Cl14} sigma for 1-2: 0.02, 1-3: 0.04 as {C210, Cl23, Cl24} 6. Others Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(Cl13)=Sof(Cl14)=1-FVAR(1) Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(Cl11)=Sof(Cl12)=FVAR(1) Sof(C210)=Sof(H21C)=Sof(H21D)=Sof(Cl23)=Sof(Cl24)=1-FVAR(2) Sof(C200)=Sof(H20D)=Sof(H20E)=Sof(Cl21)=Sof(Cl22)=FVAR(2) Fixed Sof: H1(0.33333) H2(0.33333) C300(0.16667) Cl31(0.33333) 7.a Riding coordinates: S1(H1), S2(H2) 7.b Ternary CH refined with riding coordinates: C11(H11), C12(H12), C13(H13), C31(H31), C32(H32), C33(H33) 7.c Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A, H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C100(H10A,H10B), C110(H11A,H11B), C200(H20D,H20E), C210(H21C,H21D) 7.d Me refined with riding coordinates: C20(H20A,H20B,H20C), C40(H40A,H40B,H40C) 7.e Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9), C27(H27), C29(H29) ; _shelx_res_file ; TITL MR1517 in P6(3), ROSENZWEIG/MEYER, [U(SH)(Ad_ArO)3tacn)]*solv CELL 0.71073 20.2585 20.2585 18.3017 90 90 120 ZERR 2 0.0048 0.0048 0.0043 0 0 0 LATT -1 SYMM -Y+X,+X,0.5+Z SYMM +Y,-X+Y,0.5+Z SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -X,-Y,0.5+Z SFAC C H N O S U Cl UNIT 253 342 12 12 4 4 26 EQIV $1 2-Y,2+X-Y,+Z EQIV $2 +Y-X,2-X,+Z EQIV $3 2-Y,1+X-Y,+Z EQIV $4 1+Y-X,2-X,+Z DFIX 1.8 0.01 C100 Cl11 C100 Cl12 C110 Cl13 C110 Cl14 DFIX 2.9 0.01 Cl11 Cl12 Cl13 Cl14 Cl21 Cl22 Cl23 Cl24 DFIX 1.8 0.01 C200 Cl21 C200 Cl22 C210 Cl23 C210 Cl24 DFIX 1.8 0.01 C300 Cl31 SIMU 0.01 0.02 1.7 C100 > Cl14 SIMU 0.01 0.02 1.7 C200 > Cl24 SIMU 0.003 0.006 1.7 C300 Cl31 ISOR 0.01 0.02 C100 > Cl14 ISOR 0.01 0.02 C200 > Cl24 ISOR 0.003 0.006 C300 Cl31 L.S. 8 PLAN 20 SIZE 0.22 0.11 0.1 TEMP -173 MPLA 3 O1 O1_$1 O1_$2 U1 N1 MPLA 3 O2 O2_$3 O2_$4 U2 N2 BOND .5 $H CONF WPDB -1 LIST 4 MPLA 3 CONF HTAB MORE -1 acta fmap 2 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 2 0 REM REM REM WGHT 0.026600 9.183600 BASF 0.01454 FVAR 0.06812 0.65057 0.56799 U1 6 0.666667 0.333333 0.605383 10.33333 0.01350 0.01350 = 0.02317 0.00000 0.00000 0.00675 S1 5 0.666667 0.333333 0.760756 10.33333 0.04298 0.04298 = 0.03628 0.00000 0.00000 0.02149 AFIX 3 H1 2 0.654300 0.308400 0.806276 10.33333 -1.50000 AFIX 0 O1 4 0.760892 0.313712 0.620036 11.00000 0.01269 0.02249 = 0.03149 0.00943 0.00587 0.01052 N1 3 0.761539 0.390685 0.491137 11.00000 0.01877 0.01400 = 0.02772 0.00391 0.00122 0.00891 C1 1 0.752833 0.334049 0.433954 11.00000 0.01988 0.01872 = 0.02702 -0.00009 0.00367 0.01069 AFIX 23 H1A 2 0.803796 0.342205 0.420859 11.00000 -1.50000 H1B 2 0.730229 0.342584 0.389519 11.00000 -1.50000 AFIX 0 C2 1 0.747531 0.450434 0.459417 11.00000 0.01992 0.01679 = 0.03447 0.00739 0.00358 0.01130 AFIX 23 H2A 2 0.782310 0.474641 0.417493 11.00000 -1.50000 H2B 2 0.759477 0.490325 0.496638 11.00000 -1.50000 AFIX 0 C3 1 0.841638 0.430981 0.520603 11.00000 0.01804 0.01962 = 0.02954 0.00383 0.00221 0.00952 AFIX 23 H3A 2 0.876306 0.464515 0.481872 11.00000 -1.20000 H3B 2 0.844267 0.463938 0.561749 11.00000 -1.20000 AFIX 0 C4 1 0.870033 0.379299 0.546676 11.00000 0.01658 0.01496 = 0.02934 0.00019 -0.00044 0.00750 C5 1 0.829166 0.322448 0.599242 11.00000 0.01901 0.02129 = 0.02580 0.00036 0.00105 0.01289 C6 1 0.857420 0.277517 0.627550 11.00000 0.01881 0.02254 = 0.02304 -0.00032 0.00084 0.01271 C7 1 0.928282 0.291385 0.599963 11.00000 0.02350 0.02905 = 0.02640 0.00230 0.00392 0.01899 AFIX 43 H7 2 0.949141 0.261926 0.618540 11.00000 -1.20000 AFIX 0 C8 1 0.969165 0.346036 0.546916 11.00000 0.02031 0.03191 = 0.03065 0.00432 0.00430 0.01753 C9 1 0.939470 0.389901 0.520655 11.00000 0.01758 0.02546 = 0.03053 0.00662 0.00658 0.01062 AFIX 43 H9 2 0.966625 0.427609 0.484554 11.00000 -1.20000 AFIX 0 C10 1 0.814360 0.216483 0.685509 11.00000 0.02291 0.02807 = 0.02472 0.00409 0.00337 0.02045 C11 1 0.810471 0.113185 0.766592 11.00000 0.03757 0.04509 = 0.03453 0.01853 0.01142 0.03415 AFIX 13 H11 2 0.839362 0.087117 0.780991 11.00000 -1.20000 AFIX 0 C12 1 0.753960 0.190225 0.811055 11.00000 0.03036 0.03842 = 0.03023 0.00946 0.01290 0.02219 AFIX 13 H12 2 0.745309 0.214724 0.854629 11.00000 -1.20000 AFIX 0 C13 1 0.689680 0.095192 0.710890 11.00000 0.02658 0.02426 = 0.05872 0.01512 -0.00187 0.01103 AFIX 13 H13 2 0.639318 0.057189 0.689598 11.00000 -1.20000 AFIX 0 C14 1 0.856081 0.174346 0.709620 11.00000 0.02545 0.03348 = 0.02738 0.00665 0.00241 0.02245 AFIX 23 H14A 2 0.864966 0.150306 0.666498 11.00000 -1.20000 H14B 2 0.906334 0.211477 0.730330 11.00000 -1.20000 AFIX 0 C15 1 0.735884 0.155503 0.654578 11.00000 0.02636 0.02330 = 0.04072 0.00588 -0.00611 0.01528 AFIX 23 H15A 2 0.707112 0.180606 0.638616 11.00000 -1.20000 H15B 2 0.743936 0.131018 0.611328 11.00000 -1.20000 AFIX 0 C16 1 0.796744 0.149960 0.835268 11.00000 0.02842 0.05466 = 0.03537 0.01538 0.00775 0.02672 AFIX 23 H16A 2 0.766382 0.110202 0.871858 11.00000 -1.20000 H16B 2 0.846051 0.186971 0.857736 11.00000 -1.20000 AFIX 0 C17 1 0.677142 0.133230 0.778599 11.00000 0.02532 0.03807 = 0.05918 0.02362 0.01244 0.02026 AFIX 23 H17A 2 0.649107 0.159610 0.764310 11.00000 -1.20000 H17B 2 0.646361 0.093926 0.815406 11.00000 -1.20000 AFIX 0 C18 1 0.801918 0.252850 0.754350 11.00000 0.02338 0.03247 = 0.03123 0.00537 0.01054 0.01742 AFIX 23 H18A 2 0.775202 0.280787 0.740903 11.00000 -1.20000 H18B 2 0.851815 0.289704 0.775903 11.00000 -1.20000 AFIX 0 C19 1 0.733284 0.054645 0.735074 11.00000 0.04522 0.03215 = 0.04787 0.01537 0.00397 0.02305 AFIX 23 H19A 2 0.703408 0.015670 0.772464 11.00000 -1.20000 H19B 2 0.740791 0.028721 0.692705 11.00000 -1.20000 AFIX 0 C20 1 1.044971 0.357933 0.519978 11.00000 0.02843 0.04917 = 0.04495 0.01644 0.01755 0.02555 AFIX 33 H20A 2 1.056543 0.321927 0.544559 11.00000 -1.50000 H20B 2 1.042385 0.349382 0.467095 11.00000 -1.50000 H20C 2 1.085083 0.410195 0.530833 11.00000 -1.50000 AFIX 0 U2 6 1.000000 0.000000 0.504596 10.33333 0.01139 0.01139 = 0.00752 0.00000 0.00000 0.00569 S2 5 1.000000 0.000000 0.352980 10.33333 0.03323 0.03323 = 0.00704 0.00000 0.00000 0.01662 AFIX 3 H2 2 1.017600 0.018800 0.307020 10.33333 -1.50000 AFIX 0 O2 4 0.889611 -0.006884 0.489204 11.00000 0.01043 0.01995 = 0.01004 0.00382 0.00247 0.00828 N2 3 0.911144 -0.074657 0.616840 11.00000 0.01646 0.01277 = 0.00825 -0.00004 -0.00195 0.00714 C21 1 0.904129 -0.025268 0.673650 11.00000 0.01324 0.01654 = 0.00868 -0.00003 0.00147 0.00734 AFIX 23 H21A 2 0.930877 -0.026336 0.718518 11.00000 -1.20000 H21B 2 0.849623 -0.046513 0.685968 11.00000 -1.20000 AFIX 0 C22 1 0.936788 0.056573 0.649163 11.00000 0.01122 0.01609 = 0.01371 -0.00195 0.00090 0.00623 AFIX 23 H22A 2 0.902205 0.059224 0.612560 11.00000 -1.50000 H22B 2 0.939268 0.088016 0.691620 11.00000 -1.50000 AFIX 0 C23 1 0.835245 -0.129407 0.583998 11.00000 0.01424 0.01633 = 0.01304 -0.00127 -0.00144 0.00681 AFIX 23 H23A 2 0.843594 -0.152480 0.539813 11.00000 -1.20000 H23B 2 0.806031 -0.170951 0.619392 11.00000 -1.20000 AFIX 0 C24 1 0.788654 -0.093485 0.563505 11.00000 0.01606 0.01796 = 0.01057 0.00128 0.00215 0.00723 C25 1 0.817980 -0.032698 0.513189 11.00000 0.01639 0.02046 = 0.00928 0.00084 0.00303 0.01077 C26 1 0.771907 -0.002090 0.491210 11.00000 0.01407 0.02062 = 0.01335 0.00045 -0.00005 0.00927 C27 1 0.700641 -0.031419 0.524038 11.00000 0.01765 0.02880 = 0.02052 0.00366 0.00363 0.01423 AFIX 43 H27 2 0.669644 -0.010584 0.510112 11.00000 -1.20000 AFIX 0 C28 1 0.671983 -0.089491 0.576093 11.00000 0.01534 0.03431 = 0.02463 0.01046 0.00609 0.01362 C29 1 0.716675 -0.120985 0.594185 11.00000 0.01615 0.02246 = 0.01603 0.00594 0.00332 0.00736 AFIX 43 H29 2 0.697986 -0.161980 0.628038 11.00000 -1.20000 AFIX 0 C30 1 0.796686 0.056481 0.428789 11.00000 0.01482 0.01729 = 0.01203 0.00122 0.00050 0.00966 C31 1 0.759393 0.135918 0.349322 11.00000 0.02291 0.03047 = 0.01703 0.00368 0.00261 0.01955 AFIX 13 H31 2 0.719628 0.150594 0.341013 11.00000 -1.20000 AFIX 0 C32 1 0.828501 0.073988 0.293802 11.00000 0.02065 0.01826 = 0.01122 -0.00068 0.00126 0.01058 AFIX 13 H32 2 0.833992 0.048851 0.249022 11.00000 -1.20000 AFIX 0 C33 1 0.897357 0.185389 0.381030 11.00000 0.02381 0.01450 = 0.02009 -0.00133 0.00393 0.00854 AFIX 13 H33 2 0.947094 0.231884 0.392826 11.00000 -1.20000 AFIX 0 C34 1 0.735961 0.080510 0.413654 11.00000 0.02255 0.02438 = 0.01505 0.00341 0.00245 0.01574 AFIX 23 H34A 2 0.686335 0.034602 0.402805 11.00000 -1.20000 H34B 2 0.729612 0.104976 0.457846 11.00000 -1.20000 AFIX 0 C35 1 0.872727 0.129684 0.444777 11.00000 0.01925 0.01786 = 0.01069 -0.00165 -0.00150 0.00982 AFIX 23 H35A 2 0.867137 0.154439 0.489132 11.00000 -1.20000 H35B 2 0.912665 0.116259 0.454469 11.00000 -1.20000 AFIX 0 C36 1 0.768091 0.098055 0.280315 11.00000 0.02391 0.02854 = 0.01407 0.00179 0.00066 0.01710 AFIX 23 H36A 2 0.784033 0.134190 0.238834 11.00000 -1.20000 H36B 2 0.718607 0.052731 0.267791 11.00000 -1.20000 AFIX 0 C37 1 0.906450 0.146606 0.312027 11.00000 0.01857 0.01827 = 0.01613 0.00192 0.00577 0.01093 AFIX 23 H37A 2 0.945786 0.132110 0.320635 11.00000 -1.20000 H37B 2 0.923023 0.182522 0.270334 11.00000 -1.20000 AFIX 0 C38 1 0.805163 0.019119 0.358405 11.00000 0.01782 0.01513 = 0.01399 -0.00187 -0.00079 0.00967 AFIX 23 H38A 2 0.844118 0.003950 0.366197 11.00000 -1.20000 H38B 2 0.756140 -0.027426 0.347325 11.00000 -1.20000 AFIX 0 C39 1 0.836806 0.208173 0.366298 11.00000 0.03684 0.01963 = 0.02022 -0.00028 0.00379 0.01826 AFIX 23 H39A 2 0.852628 0.243719 0.324342 11.00000 -1.20000 H39B 2 0.831541 0.234450 0.409618 11.00000 -1.20000 AFIX 0 C40 1 0.594512 -0.117879 0.610447 11.00000 0.02396 0.06053 = 0.04907 0.03463 0.02322 0.02499 AFIX 33 H40A 2 0.571610 -0.088864 0.590980 11.00000 -1.50000 H40B 2 0.561596 -0.172047 0.599081 11.00000 -1.50000 H40C 2 0.600122 -0.111122 0.663543 11.00000 -1.50000 AFIX 0 SAME 0.02 0.04 C110 > Cl14 PART 1 C100 1 0.566835 0.192250 0.924605 21.00000 0.11490 0.12574 = 0.09392 0.02877 0.01695 0.07714 AFIX 23 H10A 2 0.595244 0.213826 0.878585 21.00000 -1.20000 H10B 2 0.539502 0.219750 0.937375 21.00000 -1.20000 AFIX 0 CL11 7 0.630979 0.201848 0.996323 21.00000 0.19068 0.18163 = 0.16996 0.09992 0.02795 0.10065 CL12 7 0.499871 0.091470 0.913659 21.00000 0.10360 0.14376 = 0.12272 0.07103 0.04113 0.07572 PART 0 PART 2 C110 1 0.570014 0.179741 0.902806 -21.00000 0.11895 0.13188 = 0.10987 0.02417 0.01411 0.06753 AFIX 23 H11A 2 0.582238 0.226099 0.874449 -21.00000 -1.20000 H11B 2 0.574183 0.143217 0.869886 -21.00000 -1.20000 AFIX 0 CL13 7 0.475668 0.138094 0.938836 -21.00000 0.11954 0.15610 = 0.09015 0.03996 0.02585 0.06073 CL14 7 0.635138 0.203765 0.977940 -21.00000 0.10558 0.17079 = 0.07998 0.02361 0.02823 0.10576 SAME 0.02 0.04 C110 > Cl14 PART 0 PART 1 C200 1 0.529373 0.006461 0.258487 31.00000 0.17090 0.20379 = 0.21551 -0.00064 -0.01739 0.09573 AFIX 23 H20D 2 0.569701 -0.003005 0.277350 31.00000 -1.20000 H20E 2 0.480685 -0.042522 0.256525 31.00000 -1.20000 AFIX 0 CL21 7 0.553859 0.049522 0.171354 31.00000 0.14852 0.32732 = 0.20624 -0.10322 -0.00973 0.14550 CL22 7 0.520310 0.074814 0.315486 31.00000 0.22049 0.17705 = 0.23922 -0.05689 0.02071 0.09841 SAME 0.02 0.04 C110 > Cl14 PART 0 PART 2 C210 1 0.544216 0.092639 0.268113 -31.00000 0.18024 0.19773 = 0.20541 -0.00309 -0.00604 0.09888 AFIX 23 H21C 2 0.492481 0.082226 0.254926 -31.00000 -1.20000 H21D 2 0.564512 0.131966 0.306899 -31.00000 -1.20000 AFIX 0 CL23 7 0.604680 0.125362 0.190299 -31.00000 0.29889 0.36788 = 0.25275 0.01090 -0.06533 0.19216 CL24 7 0.540260 0.006618 0.300343 -31.00000 0.11935 0.23511 = 0.29560 -0.02366 -0.00728 0.06734 PART 0 C300 1 0.666667 0.333333 0.220806 10.16667 0.42493 0.42493 = 0.42483 0.00000 0.00000 0.21246 CL31 7 0.703178 0.268192 0.231532 10.33333 0.09752 0.12652 = 0.06096 -0.00113 0.01220 0.04660 HKLF 4 REM MR1517 in P6(3), ROSENZWEIG/MEYER, [U(SH)(Ad_ArO)3tacn)]*solv REM R1 = 0.0307 for 10199 Fo > 4sig(Fo) and 0.0385 for all 11217 data REM 532 parameters refined using 182 restraints END WGHT 0.0243 9.0782 REM Instructions for potential hydrogen bonds EQIV $5 -y+1, x-y, z HTAB C2 O1_$5 EQIV $6 x-y, x-1, z+1/2 HTAB C21 S2_$6 HTAB C22 O2 HTAB C100 S1 EQIV $7 -x+y+1, -x+1, z HTAB C100 Cl11_$7 HTAB C110 S1 REM Highest difference peak 1.148, deepest hole -0.803, 1-sigma level 0.095 Q1 1 1.0000 0.0000 0.4608 10.33333 0.05 1.15 Q2 1 1.0000 0.0000 0.4048 10.33333 0.05 1.00 Q3 1 0.6732 0.1976 0.1903 11.00000 0.05 0.99 Q4 1 0.6667 0.3333 0.6518 10.33333 0.05 0.80 Q5 1 1.0000 0.0000 0.5483 10.33333 0.05 0.79 Q6 1 0.9653 -0.0159 0.6021 11.00000 0.05 0.64 Q7 1 0.5466 0.0107 0.2141 11.00000 0.05 0.62 Q8 1 0.6768 0.2839 0.6267 11.00000 0.05 0.58 Q9 1 0.6667 0.3333 0.9123 10.33333 0.05 0.58 Q10 1 0.6897 0.3690 0.5058 11.00000 0.05 0.58 Q11 1 0.6337 0.3864 0.1820 11.00000 0.05 0.56 Q12 1 0.6771 0.2895 0.2266 11.00000 0.05 0.56 Q13 1 0.6667 0.3333 0.5570 10.33333 0.05 0.54 Q14 1 0.6475 0.3005 0.6041 11.00000 0.05 0.54 Q15 1 0.7262 0.3321 0.6039 11.00000 0.05 0.53 Q16 1 0.9601 -0.0408 0.5029 11.00000 0.05 0.52 Q17 1 0.9447 -0.0050 0.4809 11.00000 0.05 0.52 Q18 1 0.6486 0.2770 0.1799 11.00000 0.05 0.51 Q19 1 0.6667 0.3333 0.7100 10.33333 0.05 0.50 Q20 1 0.6667 0.3333 0.4487 10.33333 0.05 0.48 ; _shelx_res_checksum 95930 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.6667 0.3333 0.60538(2) 0.01672(8) Uani 1 3 d S T P . . S1 S 0.6667 0.3333 0.7608(2) 0.0407(7) Uani 1 3 d S T P . . H1 H 0.6543 0.3084 0.8063 0.061 Uiso 0.3333 1 d R . . . . O1 O 0.7609(2) 0.3137(2) 0.6200(2) 0.0215(9) Uani 1 1 d . . . . . N1 N 0.7615(3) 0.3907(3) 0.4911(3) 0.0198(10) Uani 1 1 d . . . . . C1 C 0.7528(3) 0.3340(3) 0.4340(3) 0.0214(12) Uani 1 1 d . . . . . H1A H 0.8038 0.3422 0.4209 0.032 Uiso 1 1 calc R . . . . H1B H 0.7302 0.3426 0.3895 0.032 Uiso 1 1 calc R . . . . C2 C 0.7475(3) 0.4504(3) 0.4594(4) 0.0228(12) Uani 1 1 d . . . . . H2A H 0.7823 0.4746 0.4175 0.034 Uiso 1 1 calc R . . . . H2B H 0.7595 0.4903 0.4966 0.034 Uiso 1 1 calc R . . . . C3 C 0.8416(3) 0.4310(3) 0.5206(3) 0.0224(12) Uani 1 1 d . . . . . H3A H 0.8763 0.4645 0.4819 0.027 Uiso 1 1 calc R . . . . H3B H 0.8443 0.4639 0.5617 0.027 Uiso 1 1 calc R . . . . C4 C 0.8700(3) 0.3793(3) 0.5467(3) 0.0205(11) Uani 1 1 d . . . . . C5 C 0.8292(3) 0.3224(3) 0.5992(4) 0.0208(10) Uani 1 1 d . . . . . C6 C 0.8574(3) 0.2775(3) 0.6275(3) 0.0204(12) Uani 1 1 d . . . . . C7 C 0.9283(3) 0.2914(3) 0.6000(4) 0.0237(11) Uani 1 1 d . . . . . H7 H 0.9491 0.2619 0.6185 0.028 Uiso 1 1 calc R . . . . C8 C 0.9692(3) 0.3460(4) 0.5469(3) 0.0256(13) Uani 1 1 d . . . . . C9 C 0.9395(3) 0.3899(3) 0.5207(3) 0.0246(13) Uani 1 1 d . . . . . H9 H 0.9666 0.4276 0.4846 0.030 Uiso 1 1 calc R . . . . C10 C 0.8144(3) 0.2165(3) 0.6855(3) 0.0218(11) Uani 1 1 d . . . . . C11 C 0.8105(4) 0.1132(4) 0.7666(4) 0.0331(16) Uani 1 1 d . . . . . H11 H 0.8394 0.0871 0.7810 0.040 Uiso 1 1 calc R . . . . C12 C 0.7540(4) 0.1902(4) 0.8111(4) 0.0308(14) Uani 1 1 d . . . . . H12 H 0.7453 0.2147 0.8546 0.037 Uiso 1 1 calc R . . . . C13 C 0.6897(4) 0.0952(4) 0.7109(4) 0.0373(16) Uani 1 1 d . . . . . H13 H 0.6393 0.0572 0.6896 0.045 Uiso 1 1 calc R . . . . C14 C 0.8561(3) 0.1743(4) 0.7096(3) 0.0253(12) Uani 1 1 d . . . . . H14A H 0.8650 0.1503 0.6665 0.030 Uiso 1 1 calc R . . . . H14B H 0.9063 0.2115 0.7303 0.030 Uiso 1 1 calc R . . . . C15 C 0.7359(3) 0.1555(3) 0.6546(4) 0.0289(13) Uani 1 1 d . . . . . H15A H 0.7071 0.1806 0.6386 0.035 Uiso 1 1 calc R . . . . H15B H 0.7439 0.1310 0.6113 0.035 Uiso 1 1 calc R . . . . C16 C 0.7967(4) 0.1500(5) 0.8353(4) 0.0368(16) Uani 1 1 d . . . . . H16A H 0.7664 0.1102 0.8719 0.044 Uiso 1 1 calc R . . . . H16B H 0.8461 0.1870 0.8577 0.044 Uiso 1 1 calc R . . . . C17 C 0.6771(4) 0.1332(4) 0.7786(4) 0.0389(18) Uani 1 1 d . . . . . H17A H 0.6491 0.1596 0.7643 0.047 Uiso 1 1 calc R . . . . H17B H 0.6464 0.0939 0.8154 0.047 Uiso 1 1 calc R . . . . C18 C 0.8019(3) 0.2529(3) 0.7543(4) 0.0275(12) Uani 1 1 d . . . . . H18A H 0.7752 0.2808 0.7409 0.033 Uiso 1 1 calc R . . . . H18B H 0.8518 0.2897 0.7759 0.033 Uiso 1 1 calc R . . . . C19 C 0.7333(4) 0.0546(4) 0.7351(4) 0.0401(18) Uani 1 1 d . . . . . H19A H 0.7034 0.0157 0.7725 0.048 Uiso 1 1 calc R . . . . H19B H 0.7408 0.0287 0.6927 0.048 Uiso 1 1 calc R . . . . C20 C 1.0450(4) 0.3579(4) 0.5200(4) 0.0381(18) Uani 1 1 d . . . . . H20A H 1.0565 0.3219 0.5446 0.057 Uiso 1 1 calc R . . . . H20B H 1.0424 0.3494 0.4671 0.057 Uiso 1 1 calc R . . . . H20C H 1.0851 0.4102 0.5308 0.057 Uiso 1 1 calc R . . . . U2 U 1.0000 0.0000 0.50460(2) 0.01010(6) Uani 1 3 d S T P . . S2 S 1.0000 0.0000 0.35298(13) 0.0245(5) Uani 1 3 d S T P . . H2 H 1.0176 0.0188 0.3070 0.037 Uiso 0.3333 1 d R . . . . O2 O 0.88961(19) -0.0069(2) 0.48920(17) 0.0132(7) Uani 1 1 d . . . . . N2 N 0.9111(2) -0.0747(2) 0.6168(2) 0.0126(8) Uani 1 1 d . . . . . C21 C 0.9041(3) -0.0253(3) 0.6737(3) 0.0129(10) Uani 1 1 d . . . . . H21A H 0.9309 -0.0263 0.7185 0.015 Uiso 1 1 calc R . . . . H21B H 0.8496 -0.0465 0.6860 0.015 Uiso 1 1 calc R . . . . C22 C 0.9368(3) 0.0566(3) 0.6492(3) 0.0139(10) Uani 1 1 d . . . . . H22A H 0.9022 0.0592 0.6126 0.021 Uiso 1 1 calc R . . . . H22B H 0.9393 0.0880 0.6916 0.021 Uiso 1 1 calc R . . . . C23 C 0.8352(3) -0.1294(3) 0.5840(3) 0.0149(10) Uani 1 1 d . . . . . H23A H 0.8436 -0.1525 0.5398 0.018 Uiso 1 1 calc R . . . . H23B H 0.8060 -0.1710 0.6194 0.018 Uiso 1 1 calc R . . . . C24 C 0.7887(3) -0.0935(3) 0.5635(3) 0.0154(10) Uani 1 1 d . . . . . C25 C 0.8180(3) -0.0327(3) 0.5132(3) 0.0147(10) Uani 1 1 d . . . . . C26 C 0.7719(3) -0.0021(3) 0.4912(3) 0.0157(10) Uani 1 1 d . . . . . C27 C 0.7006(3) -0.0314(3) 0.5240(3) 0.0212(12) Uani 1 1 d . . . . . H27 H 0.6696 -0.0106 0.5101 0.025 Uiso 1 1 calc R . . . . C28 C 0.6720(3) -0.0895(4) 0.5761(3) 0.0242(12) Uani 1 1 d . . . . . C29 C 0.7167(3) -0.1210(3) 0.5942(3) 0.0192(11) Uani 1 1 d . . . . . H29 H 0.6980 -0.1620 0.6280 0.023 Uiso 1 1 calc R . . . . C30 C 0.7967(3) 0.0565(3) 0.4288(3) 0.0140(10) Uani 1 1 d . . . . . C31 C 0.7594(4) 0.1359(4) 0.3493(3) 0.0207(13) Uani 1 1 d . . . . . H31 H 0.7196 0.1506 0.3410 0.025 Uiso 1 1 calc R . . . . C32 C 0.8285(3) 0.0740(3) 0.2938(3) 0.0163(10) Uani 1 1 d . . . . . H32 H 0.8340 0.0489 0.2490 0.020 Uiso 1 1 calc R . . . . C33 C 0.8974(3) 0.1854(3) 0.3810(3) 0.0199(11) Uani 1 1 d . . . . . H33 H 0.9471 0.2319 0.3928 0.024 Uiso 1 1 calc R . . . . C34 C 0.7360(3) 0.0805(3) 0.4137(3) 0.0189(11) Uani 1 1 d . . . . . H34A H 0.6863 0.0346 0.4028 0.023 Uiso 1 1 calc R . . . . H34B H 0.7296 0.1050 0.4578 0.023 Uiso 1 1 calc R . . . . C35 C 0.8727(3) 0.1297(3) 0.4448(3) 0.0157(10) Uani 1 1 d . . . . . H35A H 0.8671 0.1544 0.4891 0.019 Uiso 1 1 calc R . . . . H35B H 0.9127 0.1163 0.4545 0.019 Uiso 1 1 calc R . . . . C36 C 0.7681(3) 0.0981(4) 0.2803(3) 0.0204(11) Uani 1 1 d . . . . . H36A H 0.7840 0.1342 0.2388 0.024 Uiso 1 1 calc R . . . . H36B H 0.7186 0.0527 0.2678 0.024 Uiso 1 1 calc R . . . . C37 C 0.9065(3) 0.1466(3) 0.3120(3) 0.0169(10) Uani 1 1 d . . . . . H37A H 0.9458 0.1321 0.3206 0.020 Uiso 1 1 calc R . . . . H37B H 0.9230 0.1825 0.2703 0.020 Uiso 1 1 calc R . . . . C38 C 0.8052(4) 0.0191(4) 0.3584(2) 0.0150(12) Uani 1 1 d . . . . . H38A H 0.8441 0.0039 0.3662 0.018 Uiso 1 1 calc R . . . . H38B H 0.7561 -0.0274 0.3473 0.018 Uiso 1 1 calc R . . . . C39 C 0.8368(4) 0.2082(4) 0.3663(3) 0.0237(13) Uani 1 1 d . . . . . H39A H 0.8526 0.2437 0.3243 0.028 Uiso 1 1 calc R . . . . H39B H 0.8315 0.2345 0.4096 0.028 Uiso 1 1 calc R . . . . C40 C 0.5945(4) -0.1179(4) 0.6104(5) 0.0428(18) Uani 1 1 d . . . . . H40A H 0.5716 -0.0889 0.5910 0.064 Uiso 1 1 calc R . . . . H40B H 0.5616 -0.1720 0.5991 0.064 Uiso 1 1 calc R . . . . H40C H 0.6001 -0.1111 0.6635 0.064 Uiso 1 1 calc R . . . . C100 C 0.5668(11) 0.1922(8) 0.9246(11) 0.104(6) Uani 0.651(11) 1 d D U . A 1 H10A H 0.5952 0.2138 0.8786 0.125 Uiso 0.651(11) 1 calc R . . A 1 H10B H 0.5395 0.2198 0.9374 0.125 Uiso 0.651(11) 1 calc R . . A 1 Cl11 Cl 0.6310(7) 0.2018(9) 0.9963(8) 0.177(6) Uani 0.651(11) 1 d D U . A 1 Cl12 Cl 0.4999(4) 0.0915(4) 0.9137(4) 0.117(3) Uani 0.651(11) 1 d D U . A 1 C110 C 0.5700(10) 0.180(3) 0.9028(11) 0.118(9) Uani 0.349(11) 1 d D U . A 2 H11A H 0.5822 0.2261 0.8744 0.142 Uiso 0.349(11) 1 calc R . . A 2 H11B H 0.5742 0.1432 0.8699 0.142 Uiso 0.349(11) 1 calc R . . A 2 Cl13 Cl 0.4757(7) 0.1381(9) 0.9388(6) 0.126(6) Uani 0.349(11) 1 d D U . A 2 Cl14 Cl 0.6351(8) 0.2038(13) 0.9779(10) 0.102(4) Uani 0.349(11) 1 d D U . A 2 C200 C 0.529(3) 0.0065(18) 0.2585(13) 0.196(11) Uani 0.568(11) 1 d D U . B 1 H20D H 0.5697 -0.0030 0.2774 0.235 Uiso 0.568(11) 1 calc R . . B 1 H20E H 0.4807 -0.0425 0.2565 0.235 Uiso 0.568(11) 1 calc R . . B 1 Cl21 Cl 0.5539(7) 0.0495(11) 0.1714(7) 0.216(6) Uani 0.568(11) 1 d D U . B 1 Cl22 Cl 0.5203(10) 0.0748(8) 0.3155(8) 0.213(6) Uani 0.568(11) 1 d D U . B 1 C210 C 0.544(3) 0.093(3) 0.268(3) 0.193(12) Uani 0.432(11) 1 d D U . B 2 H21C H 0.4925 0.0822 0.2549 0.231 Uiso 0.432(11) 1 calc R . . B 2 H21D H 0.5645 0.1320 0.3069 0.231 Uiso 0.432(11) 1 calc R . . B 2 Cl23 Cl 0.6047(16) 0.1254(17) 0.1903(15) 0.295(11) Uani 0.432(11) 1 d D U . B 2 Cl24 Cl 0.5403(11) 0.0066(12) 0.3003(13) 0.226(8) Uani 0.432(11) 1 d D U . B 2 C300 C 0.6667 0.3333 0.221(8) 0.425(6) Uani 0.5 3 d DS TU P . . Cl31 Cl 0.7032(6) 0.2682(7) 0.2315(5) 0.099(3) Uani 0.3333 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01350(9) 0.01350(9) 0.02317(16) 0.000 0.000 0.00675(5) S1 0.0430(11) 0.0430(11) 0.0363(17) 0.000 0.000 0.0215(5) O1 0.0127(17) 0.0225(19) 0.031(2) 0.0094(17) 0.0059(16) 0.0105(15) N1 0.019(2) 0.014(2) 0.028(3) 0.0039(19) 0.0012(19) 0.0089(18) C1 0.020(3) 0.019(3) 0.027(3) 0.000(2) 0.004(2) 0.011(2) C2 0.020(3) 0.017(3) 0.034(3) 0.007(2) 0.004(3) 0.011(2) C3 0.018(3) 0.020(3) 0.030(3) 0.004(2) 0.002(2) 0.010(2) C4 0.017(3) 0.015(3) 0.029(3) 0.000(2) 0.000(2) 0.007(2) C5 0.019(2) 0.021(2) 0.026(3) 0.000(2) 0.001(2) 0.013(2) C6 0.019(3) 0.023(3) 0.023(3) 0.000(2) 0.001(2) 0.013(2) C7 0.023(3) 0.029(3) 0.026(3) 0.002(3) 0.004(3) 0.019(2) C8 0.020(3) 0.032(3) 0.031(3) 0.004(3) 0.004(2) 0.018(3) C9 0.018(3) 0.025(3) 0.031(4) 0.007(2) 0.007(2) 0.011(2) C10 0.023(3) 0.028(3) 0.025(3) 0.004(2) 0.003(2) 0.020(2) C11 0.038(3) 0.045(4) 0.035(4) 0.019(3) 0.011(3) 0.034(3) C12 0.030(3) 0.038(4) 0.030(3) 0.009(3) 0.013(3) 0.022(3) C13 0.027(3) 0.024(3) 0.059(5) 0.015(3) -0.002(3) 0.011(3) C14 0.025(3) 0.033(3) 0.027(3) 0.007(3) 0.002(2) 0.022(3) C15 0.026(3) 0.023(3) 0.041(4) 0.006(3) -0.006(3) 0.015(3) C16 0.028(4) 0.055(5) 0.035(4) 0.015(4) 0.008(3) 0.027(4) C17 0.025(3) 0.038(4) 0.059(5) 0.024(3) 0.012(3) 0.020(3) C18 0.023(3) 0.032(3) 0.031(3) 0.005(3) 0.011(3) 0.017(2) C19 0.045(4) 0.032(4) 0.048(5) 0.015(3) 0.004(3) 0.023(3) C20 0.028(3) 0.049(4) 0.045(5) 0.016(3) 0.018(3) 0.026(3) U2 0.01139(8) 0.01139(8) 0.00752(11) 0.000 0.000 0.00569(4) S2 0.0332(9) 0.0332(9) 0.0070(10) 0.000 0.000 0.0166(4) O2 0.0104(16) 0.0200(18) 0.0100(18) 0.0038(13) 0.0025(12) 0.0083(14) N2 0.016(2) 0.0128(19) 0.008(2) 0.0000(16) -0.0020(16) 0.0071(16) C21 0.013(2) 0.017(2) 0.009(2) 0.0000(18) 0.0015(18) 0.007(2) C22 0.011(2) 0.016(2) 0.014(2) -0.0019(19) 0.0009(19) 0.006(2) C23 0.014(2) 0.016(2) 0.013(2) -0.0013(18) -0.0014(17) 0.007(2) C24 0.016(2) 0.018(3) 0.011(2) 0.0013(19) 0.0021(19) 0.007(2) C25 0.016(2) 0.020(2) 0.009(2) 0.001(2) 0.0030(19) 0.011(2) C26 0.014(2) 0.021(3) 0.013(3) 0.0004(19) 0.0000(18) 0.009(2) C27 0.018(3) 0.029(3) 0.021(3) 0.004(2) 0.004(2) 0.014(2) C28 0.015(3) 0.034(3) 0.025(3) 0.010(2) 0.006(2) 0.014(2) C29 0.016(2) 0.022(3) 0.016(3) 0.006(2) 0.003(2) 0.007(2) C30 0.015(2) 0.017(3) 0.012(2) 0.0012(19) 0.0005(19) 0.010(2) C31 0.023(3) 0.030(4) 0.017(3) 0.004(2) 0.003(2) 0.020(3) C32 0.021(3) 0.018(3) 0.011(2) -0.0007(19) 0.001(2) 0.011(2) C33 0.024(3) 0.015(3) 0.020(3) -0.001(2) 0.004(2) 0.009(2) C34 0.023(3) 0.024(3) 0.015(3) 0.003(2) 0.002(2) 0.016(2) C35 0.019(3) 0.018(2) 0.011(2) -0.002(2) -0.001(2) 0.010(2) C36 0.024(3) 0.029(3) 0.014(2) 0.002(2) 0.001(2) 0.017(3) C37 0.019(3) 0.018(3) 0.016(2) 0.002(2) 0.006(2) 0.011(2) C38 0.018(3) 0.015(3) 0.014(3) -0.0019(17) -0.0008(17) 0.010(3) C39 0.037(4) 0.020(3) 0.020(3) 0.000(2) 0.004(3) 0.018(3) C40 0.024(3) 0.061(4) 0.049(4) 0.035(4) 0.023(4) 0.025(3) C100 0.115(9) 0.126(9) 0.094(9) 0.029(8) 0.017(8) 0.077(7) Cl11 0.191(9) 0.182(9) 0.170(11) 0.100(8) 0.028(8) 0.101(7) Cl12 0.104(4) 0.144(6) 0.123(5) 0.071(4) 0.041(4) 0.076(4) C110 0.119(11) 0.132(11) 0.110(12) 0.024(10) 0.014(10) 0.068(8) Cl13 0.120(8) 0.156(10) 0.090(7) 0.040(7) 0.026(6) 0.061(7) Cl14 0.106(7) 0.171(11) 0.080(7) 0.024(8) 0.028(5) 0.106(7) C200 0.171(14) 0.204(14) 0.216(15) -0.001(11) -0.017(11) 0.096(10) Cl21 0.149(9) 0.327(16) 0.206(11) -0.103(10) -0.010(8) 0.146(10) Cl22 0.220(11) 0.177(10) 0.239(12) -0.057(9) 0.021(10) 0.098(9) C210 0.180(14) 0.198(14) 0.205(15) -0.003(11) -0.006(11) 0.099(10) Cl23 0.299(18) 0.37(2) 0.253(17) 0.011(16) -0.065(15) 0.192(15) Cl24 0.119(9) 0.235(14) 0.296(16) -0.024(13) -0.007(12) 0.067(9) C300 0.425(5) 0.425(5) 0.425(7) 0.000 0.000 0.212(3) Cl31 0.098(6) 0.127(7) 0.061(5) -0.001(4) 0.012(4) 0.047(5) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 U1 S1 82.84(11) . . O1 U1 S1 82.84(11) 5_665 . O1 U1 S1 82.84(11) 4_655 . O1 U1 O1 118.47(5) . 5_665 O1 U1 O1 118.47(5) 5_665 4_655 O1 U1 O1 118.47(5) . 4_655 O1 U1 N1 70.57(14) . . O1 U1 N1 85.67(15) . 5_665 O1 U1 N1 85.67(15) 5_665 4_655 O1 U1 N1 70.57(14) 4_655 4_655 O1 U1 N1 70.57(14) 5_665 5_665 O1 U1 N1 134.42(15) 4_655 5_665 O1 U1 N1 134.42(15) 5_665 . O1 U1 N1 85.67(15) 4_655 . O1 U1 N1 134.42(15) . 4_655 N1 U1 S1 141.28(10) . . N1 U1 S1 141.28(10) 4_655 . N1 U1 S1 141.27(10) 5_665 . N1 U1 N1 65.61(16) . 4_655 N1 U1 N1 65.61(16) 5_665 4_655 N1 U1 N1 65.61(16) 5_665 . U1 S1 H1 152.3 . . C5 O1 U1 151.7(4) . . C1 N1 U1 115.4(3) . . C1 N1 C3 110.4(4) . . C2 N1 U1 105.6(3) . . C2 N1 C1 110.6(5) . . C2 N1 C3 106.9(4) . . C3 N1 U1 107.5(3) . . N1 C1 H1A 109.1 . . N1 C1 H1B 109.1 . . N1 C1 C2 112.3(5) . 5_665 H1A C1 H1B 107.9 . . C2 C1 H1A 109.1 5_665 . C2 C1 H1B 109.1 5_665 . N1 C2 C1 112.7(5) . 4_655 N1 C2 H2A 109.1 . . N1 C2 H2B 109.1 . . C1 C2 H2A 109.1 4_655 . C1 C2 H2B 109.1 4_655 . H2A C2 H2B 107.8 . . N1 C3 H3A 108.6 . . N1 C3 H3B 108.6 . . H3A C3 H3B 107.5 . . C4 C3 N1 114.9(5) . . C4 C3 H3A 108.6 . . C4 C3 H3B 108.6 . . C5 C4 C3 120.9(5) . . C9 C4 C3 119.5(5) . . C9 C4 C5 119.6(5) . . O1 C5 C4 116.2(5) . . O1 C5 C6 122.3(5) . . C6 C5 C4 121.5(5) . . C5 C6 C7 116.5(5) . . C5 C6 C10 122.1(5) . . C7 C6 C10 121.4(5) . . C6 C7 H7 118.3 . . C8 C7 C6 123.3(5) . . C8 C7 H7 118.3 . . C7 C8 C20 120.5(5) . . C9 C8 C7 118.4(5) . . C9 C8 C20 121.1(6) . . C4 C9 H9 119.7 . . C8 C9 C4 120.7(5) . . C8 C9 H9 119.7 . . C6 C10 C14 113.5(5) . . C6 C10 C15 109.5(5) . . C6 C10 C18 110.1(5) . . C14 C10 C15 107.0(5) . . C14 C10 C18 107.3(5) . . C18 C10 C15 109.3(5) . . C14 C11 H11 109.4 . . C14 C11 C16 110.1(6) . . C16 C11 H11 109.4 . . C19 C11 H11 109.4 . . C19 C11 C14 110.0(5) . . C19 C11 C16 108.6(6) . . C16 C12 H12 108.8 . . C16 C12 C18 110.0(5) . . C17 C12 H12 108.8 . . C17 C12 C16 110.3(6) . . C17 C12 C18 110.2(6) . . C18 C12 H12 108.8 . . C15 C13 H13 109.7 . . C15 C13 C17 109.5(5) . . C15 C13 C19 109.8(6) . . C17 C13 H13 109.7 . . C19 C13 H13 109.7 . . C19 C13 C17 108.4(6) . . C10 C14 H14A 109.3 . . C10 C14 H14B 109.3 . . C11 C14 C10 111.7(5) . . C11 C14 H14A 109.3 . . C11 C14 H14B 109.3 . . H14A C14 H14B 107.9 . . C10 C15 H15A 109.3 . . C10 C15 H15B 109.3 . . C13 C15 C10 111.6(5) . . C13 C15 H15A 109.3 . . C13 C15 H15B 109.3 . . H15A C15 H15B 108.0 . . C11 C16 H16A 110.1 . . C11 C16 H16B 110.1 . . C12 C16 C11 107.9(6) . . C12 C16 H16A 110.1 . . C12 C16 H16B 110.1 . . H16A C16 H16B 108.4 . . C12 C17 C13 109.3(5) . . C12 C17 H17A 109.8 . . C12 C17 H17B 109.8 . . C13 C17 H17A 109.8 . . C13 C17 H17B 109.8 . . H17A C17 H17B 108.3 . . C10 C18 C12 110.0(5) . . C10 C18 H18A 109.7 . . C10 C18 H18B 109.7 . . C12 C18 H18A 109.7 . . C12 C18 H18B 109.7 . . H18A C18 H18B 108.2 . . C11 C19 C13 109.4(6) . . C11 C19 H19A 109.8 . . C11 C19 H19B 109.8 . . C13 C19 H19A 109.8 . . C13 C19 H19B 109.8 . . H19A C19 H19B 108.2 . . C8 C20 H20A 109.5 . . C8 C20 H20B 109.5 . . C8 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . O2 U2 S2 82.60(8) 5_765 . O2 U2 S2 82.60(8) 4_645 . O2 U2 S2 82.60(8) . . O2 U2 O2 118.37(4) 5_765 . O2 U2 O2 118.37(4) 4_645 . O2 U2 O2 118.37(4) 5_765 4_645 O2 U2 N2 84.46(13) 5_765 4_645 O2 U2 N2 84.46(13) 4_645 . O2 U2 N2 71.49(12) 5_765 5_765 O2 U2 N2 71.49(12) 4_645 4_645 O2 U2 N2 84.46(12) . 5_765 O2 U2 N2 135.51(12) . 4_645 O2 U2 N2 135.51(12) 4_645 5_765 O2 U2 N2 135.50(12) 5_765 . O2 U2 N2 71.49(12) . . N2 U2 S2 140.81(9) . . N2 U2 S2 140.81(9) 4_645 . N2 U2 S2 140.81(9) 5_765 . N2 U2 N2 66.36(14) 4_645 . N2 U2 N2 66.36(14) 5_765 4_645 N2 U2 N2 66.36(14) 5_765 . U2 S2 H2 156.3 . . C25 O2 U2 148.4(3) . . C21 N2 U2 114.9(3) . . C21 N2 C23 111.6(4) . . C22 N2 U2 106.1(3) 4_645 . C22 N2 C21 110.6(4) 4_645 . C22 N2 C23 107.9(4) 4_645 . C23 N2 U2 105.3(3) . . N2 C21 H21A 109.0 . . N2 C21 H21B 109.0 . . N2 C21 C22 113.0(4) . . H21A C21 H21B 107.8 . . C22 C21 H21A 109.0 . . C22 C21 H21B 109.0 . . N2 C22 C21 112.8(4) 5_765 . N2 C22 H22A 109.0 5_765 . N2 C22 H22B 109.0 5_765 . C21 C22 H22A 109.0 . . C21 C22 H22B 109.0 . . H22A C22 H22B 107.8 . . N2 C23 H23A 108.8 . . N2 C23 H23B 108.8 . . H23A C23 H23B 107.7 . . C24 C23 N2 113.7(4) . . C24 C23 H23A 108.8 . . C24 C23 H23B 108.8 . . C25 C24 C23 119.7(5) . . C29 C24 C23 119.5(5) . . C29 C24 C25 120.8(5) . . O2 C25 C24 117.0(4) . . O2 C25 C26 123.8(4) . . C24 C25 C26 119.2(5) . . C25 C26 C30 121.1(4) . . C27 C26 C25 117.5(5) . . C27 C26 C30 121.2(5) . . C26 C27 H27 118.0 . . C26 C27 C28 124.0(5) . . C28 C27 H27 118.0 . . C27 C28 C40 121.3(5) . . C29 C28 C27 117.4(5) . . C29 C28 C40 121.3(5) . . C24 C29 H29 119.5 . . C28 C29 C24 121.0(5) . . C28 C29 H29 119.5 . . C26 C30 C34 111.6(4) . . C26 C30 C35 112.6(4) . . C26 C30 C38 108.3(4) . . C35 C30 C34 107.4(4) . . C35 C30 C38 109.1(4) . . C38 C30 C34 107.6(4) . . C34 C31 H31 109.6 . . C34 C31 C36 109.8(5) . . C34 C31 C39 109.6(5) . . C36 C31 H31 109.6 . . C36 C31 C39 108.8(5) . . C39 C31 H31 109.6 . . C36 C32 H32 109.7 . . C36 C32 C37 108.9(4) . . C37 C32 H32 109.7 . . C38 C32 H32 109.7 . . C38 C32 C36 110.3(5) . . C38 C32 C37 108.6(4) . . C35 C33 H33 109.6 . . C35 C33 C37 109.1(4) . . C35 C33 C39 110.0(5) . . C37 C33 H33 109.6 . . C39 C33 H33 109.6 . . C39 C33 C37 109.0(5) . . C30 C34 H34A 109.4 . . C30 C34 H34B 109.4 . . C31 C34 C30 111.3(5) . . C31 C34 H34A 109.4 . . C31 C34 H34B 109.4 . . H34A C34 H34B 108.0 . . C30 C35 H35A 109.3 . . C30 C35 H35B 109.3 . . C33 C35 C30 111.5(4) . . C33 C35 H35A 109.3 . . C33 C35 H35B 109.3 . . H35A C35 H35B 108.0 . . C31 C36 C32 109.5(5) . . C31 C36 H36A 109.8 . . C31 C36 H36B 109.8 . . C32 C36 H36A 109.8 . . C32 C36 H36B 109.8 . . H36A C36 H36B 108.2 . . C32 C37 H37A 109.8 . . C32 C37 H37B 109.8 . . C33 C37 C32 109.4(4) . . C33 C37 H37A 109.8 . . C33 C37 H37B 109.8 . . H37A C37 H37B 108.3 . . C30 C38 H38A 109.4 . . C30 C38 H38B 109.4 . . C32 C38 C30 111.0(5) . . C32 C38 H38A 109.4 . . C32 C38 H38B 109.4 . . H38A C38 H38B 108.0 . . C31 C39 H39A 109.8 . . C31 C39 H39B 109.8 . . C33 C39 C31 109.5(5) . . C33 C39 H39A 109.8 . . C33 C39 H39B 109.8 . . H39A C39 H39B 108.2 . . C28 C40 H40A 109.5 . . C28 C40 H40B 109.5 . . C28 C40 H40C 109.5 . . H40A C40 H40B 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . H10A C100 H10B 108.5 . . Cl11 C100 H10A 110.2 . . Cl11 C100 H10B 110.2 . . Cl11 C100 Cl12 107.3(9) . . Cl12 C100 H10A 110.2 . . Cl12 C100 H10B 110.2 . . H11A C110 H11B 108.4 . . Cl13 C110 H11A 110.1 . . Cl13 C110 H11B 110.0 . . Cl13 C110 Cl14 108.2(10) . . Cl14 C110 H11A 110.1 . . Cl14 C110 H11B 110.0 . . H20D C200 H20E 108.9 . . Cl21 C200 H20D 110.8 . . Cl21 C200 H20E 110.8 . . Cl21 C200 Cl22 104.6(9) . . Cl22 C200 H20D 110.8 . . Cl22 C200 H20E 110.8 . . H21C C210 H21D 108.4 . . Cl23 C210 H21C 110.1 . . Cl23 C210 H21D 110.1 . . Cl23 C210 Cl24 108.2(11) . . Cl24 C210 H21C 110.1 . . Cl24 C210 H21D 110.1 . . Cl31 C300 Cl31 118.9(16) . 5_665 Cl31 C300 Cl31 118.8(16) 4_655 5_665 Cl31 C300 Cl31 118.8(16) . 4_655 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 S1 2.844(4) . U1 O1 2.152(4) . U1 O1 2.152(4) 5_665 U1 O1 2.152(4) 4_655 U1 N1 2.680(5) 4_655 U1 N1 2.680(5) . U1 N1 2.680(5) 5_665 S1 H1 0.9410 . O1 C5 1.358(6) . N1 C1 1.497(7) . N1 C2 1.492(7) . N1 C3 1.505(7) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.517(8) 5_665 C2 C1 1.517(8) 4_655 C2 H2A 0.9900 . C2 H2B 0.9900 . C3 H3A 0.9900 . C3 H3B 0.9900 . C3 C4 1.502(8) . C4 C5 1.409(8) . C4 C9 1.396(8) . C5 C6 1.395(7) . C6 C7 1.411(7) . C6 C10 1.529(8) . C7 H7 0.9500 . C7 C8 1.392(8) . C8 C9 1.385(8) . C8 C20 1.513(8) . C9 H9 0.9500 . C10 C14 1.536(7) . C10 C15 1.552(8) . C10 C18 1.543(9) . C11 H11 1.0000 . C11 C14 1.527(8) . C11 C16 1.555(10) . C11 C19 1.526(10) . C12 H12 1.0000 . C12 C16 1.523(9) . C12 C17 1.520(10) . C12 C18 1.549(9) . C13 H13 1.0000 . C13 C15 1.512(9) . C13 C17 1.546(11) . C13 C19 1.542(9) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 H15A 0.9900 . C15 H15B 0.9900 . C16 H16A 0.9900 . C16 H16B 0.9900 . C17 H17A 0.9900 . C17 H17B 0.9900 . C18 H18A 0.9900 . C18 H18B 0.9900 . C19 H19A 0.9900 . C19 H19B 0.9900 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . U2 S2 2.775(2) . U2 O2 2.188(3) . U2 O2 2.188(3) 5_765 U2 O2 2.188(3) 4_645 U2 N2 2.650(4) 4_645 U2 N2 2.651(4) . U2 N2 2.650(4) 5_765 S2 H2 0.9186 . O2 C25 1.347(6) . N2 C21 1.498(6) . N2 C22 1.487(6) 4_645 N2 C23 1.500(6) . C21 H21A 0.9900 . C21 H21B 0.9900 . C21 C22 1.513(7) . C22 N2 1.487(6) 5_765 C22 H22A 0.9900 . C22 H22B 0.9900 . C23 H23A 0.9900 . C23 H23B 0.9900 . C23 C24 1.499(7) . C24 C25 1.409(7) . C24 C29 1.393(7) . C25 C26 1.413(7) . C26 C27 1.393(7) . C26 C30 1.539(7) . C27 H27 0.9500 . C27 C28 1.395(8) . C28 C29 1.384(8) . C28 C40 1.512(8) . C29 H29 0.9500 . C30 C34 1.558(7) . C30 C35 1.541(7) . C30 C38 1.546(7) . C31 H31 1.0000 . C31 C34 1.529(8) . C31 C36 1.533(8) . C31 C39 1.550(10) . C32 H32 1.0000 . C32 C36 1.547(8) . C32 C37 1.564(8) . C32 C38 1.527(7) . C33 H33 1.0000 . C33 C35 1.523(8) . C33 C37 1.546(8) . C33 C39 1.535(9) . C34 H34A 0.9900 . C34 H34B 0.9900 . C35 H35A 0.9900 . C35 H35B 0.9900 . C36 H36A 0.9900 . C36 H36B 0.9900 . C37 H37A 0.9900 . C37 H37B 0.9900 . C38 H38A 0.9900 . C38 H38B 0.9900 . C39 H39A 0.9900 . C39 H39B 0.9900 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C100 H10A 0.9900 . C100 H10B 0.9900 . C100 Cl11 1.788(11) . C100 Cl12 1.811(12) . C110 H11A 0.9900 . C110 H11B 0.9900 . C110 Cl13 1.785(12) . C110 Cl14 1.796(12) . C200 H20D 0.9900 . C200 H20E 0.9900 . C200 Cl21 1.766(12) . C200 Cl22 1.815(12) . C210 H21C 0.9900 . C210 H21D 0.9900 . C210 Cl23 1.777(12) . C210 Cl24 1.803(12) . C300 Cl31 1.817(13) . C300 Cl31 1.817(13) 5_665 C300 Cl31 1.817(13) 4_655 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_4 U1 O1 C5 C4 14.2(11) . . U1 O1 C5 C6 -165.3(5) . . U1 N1 C1 C2 -11.9(6) . 5_665 U1 N1 C2 C1 -60.2(5) . 4_655 U1 N1 C3 C4 74.3(5) . . O1 C5 C6 C7 178.6(5) . . O1 C5 C6 C10 -1.6(9) . . N1 C3 C4 C5 -54.9(7) . . N1 C3 C4 C9 127.8(6) . . C1 N1 C2 C1 65.3(6) . 4_655 C1 N1 C3 C4 -52.4(6) . . C2 N1 C1 C2 -131.7(5) . 5_665 C2 N1 C3 C4 -172.8(5) . . C3 N1 C1 C2 110.2(5) . 5_665 C3 N1 C2 C1 -174.5(5) . 4_655 C3 C4 C5 O1 4.9(8) . . C3 C4 C5 C6 -175.6(5) . . C3 C4 C9 C8 176.2(6) . . C4 C5 C6 C7 -0.9(9) . . C4 C5 C6 C10 179.0(5) . . C5 C4 C9 C8 -1.1(9) . . C5 C6 C7 C8 -0.5(9) . . C5 C6 C10 C14 -179.4(5) . . C5 C6 C10 C15 61.2(7) . . C5 C6 C10 C18 -59.0(7) . . C6 C7 C8 C9 1.1(10) . . C6 C7 C8 C20 179.9(6) . . C6 C10 C14 C11 -179.1(5) . . C6 C10 C15 C13 -177.9(5) . . C6 C10 C18 C12 176.5(5) . . C7 C6 C10 C14 0.5(8) . . C7 C6 C10 C15 -118.9(6) . . C7 C6 C10 C18 120.8(6) . . C7 C8 C9 C4 -0.2(9) . . C9 C4 C5 O1 -177.8(5) . . C9 C4 C5 C6 1.7(9) . . C10 C6 C7 C8 179.6(6) . . C14 C10 C15 C13 58.7(7) . . C14 C10 C18 C12 -59.5(6) . . C14 C11 C16 C12 58.8(7) . . C14 C11 C19 C13 -58.3(7) . . C15 C10 C14 C11 -58.2(7) . . C15 C10 C18 C12 56.2(6) . . C15 C13 C17 C12 -60.2(7) . . C15 C13 C19 C11 58.6(8) . . C16 C11 C14 C10 -59.7(7) . . C16 C11 C19 C13 62.3(7) . . C16 C12 C17 C13 -61.1(7) . . C16 C12 C18 C10 62.5(7) . . C17 C12 C16 C11 61.5(7) . . C17 C12 C18 C10 -59.3(6) . . C17 C13 C15 C10 58.8(7) . . C17 C13 C19 C11 -60.9(7) . . C18 C10 C14 C11 59.0(7) . . C18 C10 C15 C13 -57.2(6) . . C18 C12 C16 C11 -60.3(8) . . C18 C12 C17 C13 60.6(7) . . C19 C11 C14 C10 59.9(7) . . C19 C11 C16 C12 -61.7(7) . . C19 C13 C15 C10 -60.1(8) . . C19 C13 C17 C12 59.5(7) . . C20 C8 C9 C4 -179.0(6) . . U2 O2 C25 C24 -18.1(9) . . U2 O2 C25 C26 161.4(4) . . U2 N2 C21 C22 11.2(5) . . U2 N2 C23 C24 -79.3(4) . . O2 C25 C26 C27 -176.1(5) . . O2 C25 C26 C30 9.0(8) . . N2 C21 C22 N2 -48.3(6) . 5_765 N2 C23 C24 C25 58.8(6) . . N2 C23 C24 C29 -121.6(5) . . C21 N2 C23 C24 46.0(5) . . C22 N2 C21 C22 131.2(4) 4_645 . C22 N2 C23 C24 167.7(4) 4_645 . C23 N2 C21 C22 -108.6(5) . . C23 C24 C25 O2 -3.9(7) . . C23 C24 C25 C26 176.5(5) . . C23 C24 C29 C28 -179.6(5) . . C24 C25 C26 C27 3.5(7) . . C24 C25 C26 C30 -171.5(5) . . C25 C24 C29 C28 0.1(8) . . C25 C26 C27 C28 -1.0(8) . . C25 C26 C30 C34 178.9(5) . . C25 C26 C30 C35 -60.2(6) . . C25 C26 C30 C38 60.5(6) . . C26 C27 C28 C29 -2.0(9) . . C26 C27 C28 C40 179.1(6) . . C26 C30 C34 C31 -177.4(5) . . C26 C30 C35 C33 177.9(4) . . C26 C30 C38 C32 179.1(5) . . C27 C26 C30 C34 4.2(7) . . C27 C26 C30 C35 125.1(5) . . C27 C26 C30 C38 -114.2(6) . . C27 C28 C29 C24 2.4(9) . . C29 C24 C25 O2 176.5(5) . . C29 C24 C25 C26 -3.1(8) . . C30 C26 C27 C28 174.0(5) . . C34 C30 C35 C33 -58.8(5) . . C34 C30 C38 C32 58.2(6) . . C34 C31 C36 C32 -58.6(6) . . C34 C31 C39 C33 58.3(6) . . C35 C30 C34 C31 58.7(6) . . C35 C30 C38 C32 -58.0(6) . . C35 C33 C37 C32 60.1(6) . . C35 C33 C39 C31 -58.5(6) . . C36 C31 C34 C30 60.0(6) . . C36 C31 C39 C33 -61.7(6) . . C36 C32 C37 C33 59.7(6) . . C36 C32 C38 C30 -59.5(6) . . C37 C32 C36 C31 -60.5(6) . . C37 C32 C38 C30 59.8(6) . . C37 C33 C35 C30 -59.3(6) . . C37 C33 C39 C31 61.1(6) . . C38 C30 C34 C31 -58.7(6) . . C38 C30 C35 C33 57.6(6) . . C38 C32 C36 C31 58.6(6) . . C38 C32 C37 C33 -60.5(6) . . C39 C31 C34 C30 -59.5(6) . . C39 C31 C36 C32 61.3(6) . . C39 C33 C35 C30 60.2(6) . . C39 C33 C37 C32 -60.1(6) . . C40 C28 C29 C24 -178.6(6) . . loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.985(7) 2 0.015(7)