#------------------------------------------------------------------------------ #$Date: 2016-09-10 02:11:52 +0300 (Sat, 10 Sep 2016) $ #$Revision: 186330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543283.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_1543283 loop_ _publ_author_name 'Rosenzweig, Michael W.' 'Scheurer, Andreas' 'Lamsfus, Carlos A.' 'Heinemann, Frank W.' 'Maron, Laurent' 'Andrez, Julie' 'Mazzanti, Marinella' 'Meyer, Karsten' _publ_section_title ; Uranium(iv) terminal hydrosulfido and sulfido complexes: insights into the nature of the uranium--sulfur bond ; _journal_issue 9 _journal_name_full 'Chem. Sci.' _journal_page_first 5857 _journal_paper_doi 10.1039/C6SC00677A _journal_volume 7 _journal_year 2016 _chemical_absolute_configuration ad _chemical_formula_moiety 'C60 H78 N3 O3 S U, C18 H36 K N2 O6' _chemical_formula_sum 'C78 H114 K N5 O9 S U' _chemical_formula_weight 1574.93 _chemical_name_systematic ; ? ; _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 geom _audit_creation_date 2015-11-12 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _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 14.9009(19) _cell_length_b 14.9009(19) _cell_length_c 19.249(3) _cell_measurement_reflns_used 6303 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.62 _cell_measurement_theta_min 2.64 _cell_volume 3701.4(9) _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 100.15 _diffrn_detector_area_resol_mean 83.33 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'Quazar focussing montel optics' _diffrn_radiation_source 'ImuS micro-focus tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1475 _diffrn_reflns_av_unetI/netI 0.0690 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 71363 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.919 _diffrn_reflns_theta_min 1.578 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.337 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1097 before and 0.0835 after correction. The Ratio of minimum to maximum transmission is 0.8376. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1632 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: toluene/pyridin' _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.721 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.089 _refine_ls_abs_structure_details ; Flack x determined using 1752 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.002(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 5903 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+1.3460P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.0645 _reflns_Friedel_coverage 0.938 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 4066 _reflns_number_total 5903 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6sc00677a2.cif _cod_data_source_block mr1523 _cod_depositor_comments 'Adding full bibliography for 1543281--1543283.cif.' _cod_original_cell_volume 3701.4(13) _cod_database_code 1543283 _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 0.912 _shelx_estimated_absorpt_t_min 0.854 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H14A,H14B} of C14, {H15A,H15B} of C15, {H16A,H16B} of C16, {H17A,H17B} of C17, {H18A,H18B} of C18, {H19A,H19B} of C19, {H21A,H21B} of C21, {H22A,H22B} of C22, {H23A,H23B} of C23, {H24A,H24B} of C24, {H25A,H25B} of C25, {H26A,H26B} of C26, {H3A,H3B} of C3 At 1.5 times of: All C(H,H,H) groups, {H2A,H2B} of C2, {H1A,H1B} of C1 2.a Ternary CH refined with riding coordinates: C11(H11), C12(H12), C13(H13) 2.b 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), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B) 2.c Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9) 2.d Idealised Me refined as rotating group: C20(H20A,H20B,H20C) ; _shelx_res_file ; TITL MR1523 in P6(3), ROSI/MEYER, [U(S)((Ad_ArO)3tacn)][K(2,2,2crypt)] CELL 0.71073 14.9009 14.9009 19.2485 90 90 120 ZERR 2 0.0019 0.0019 0.0025 0 0 0 LATT -1 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -X,-Y,0.5+Z SYMM +Y,-X+Y,0.5+Z SYMM -Y+X,+X,0.5+Z SFAC C H N O S K U UNIT 156 228 10 18 2 2 2 L.S. 8 PLAN 20 SIZE 0.07 0.06 0.04 TEMP -173 BOND .5 $h HTAB CONF WPDB -1 LIST 4 fmap 2 acta MORE -1 REM REM REM WGHT 0.009000 1.346000 FVAR 0.08913 U1 7 0.000000 0.000000 0.749211 10.33333 0.01300 0.01300 = 0.01698 0.00000 0.00000 0.00650 S1 5 0.000000 0.000000 0.880948 10.33333 0.02297 0.02297 = 0.01640 0.00000 0.00000 0.01148 O1 4 -0.020129 0.137919 0.753656 11.00000 0.02166 0.01914 = 0.02005 -0.00582 -0.00633 0.01348 N1 3 -0.103130 0.016818 0.629579 11.00000 0.01565 0.01248 = 0.01936 -0.00055 -0.00008 0.00756 C1 1 -0.161809 -0.088094 0.599751 11.00000 0.01753 0.01493 = 0.01552 0.00163 -0.00214 0.00830 AFIX 23 H1A 2 -0.203743 -0.086956 0.560227 11.00000 -1.50000 H1B 2 -0.210062 -0.135877 0.635296 11.00000 -1.50000 AFIX 0 C2 1 -0.036010 0.092750 0.574896 11.00000 0.01862 0.01928 = 0.01226 0.00173 0.00004 0.00958 AFIX 23 H2A 2 -0.066140 0.136230 0.561357 11.00000 -1.50000 H2B 2 -0.035144 0.054281 0.533206 11.00000 -1.50000 AFIX 0 C3 1 -0.178285 0.045354 0.657555 11.00000 0.01522 0.02205 = 0.01883 -0.00400 -0.00618 0.01027 AFIX 23 H3A 2 -0.211391 0.003160 0.699492 11.00000 -1.20000 H3B 2 -0.233308 0.027839 0.622560 11.00000 -1.20000 AFIX 0 C4 1 -0.130804 0.158045 0.676169 11.00000 0.01707 0.02212 = 0.01108 0.00073 0.00495 0.01086 C5 1 -0.055216 0.197721 0.729052 11.00000 0.01782 0.02075 = 0.01711 0.00340 0.00371 0.01030 C6 1 -0.017763 0.301634 0.752394 11.00000 0.01628 0.01998 = 0.01373 0.00302 0.00432 0.00957 C7 1 -0.047028 0.362011 0.714788 11.00000 0.02498 0.01578 = 0.02121 0.00208 0.00756 0.01170 AFIX 43 H7 2 -0.019782 0.432194 0.728392 11.00000 -1.20000 AFIX 0 C8 1 -0.114402 0.325634 0.657914 11.00000 0.02570 0.02689 = 0.01630 0.00559 0.00378 0.01706 C9 1 -0.158030 0.222543 0.641358 11.00000 0.02083 0.03399 = 0.01698 -0.00465 -0.00276 0.02040 AFIX 43 H9 2 -0.208049 0.194685 0.605213 11.00000 -1.20000 AFIX 0 C10 1 0.047370 0.340465 0.818667 11.00000 0.01927 0.01374 = 0.01885 -0.00023 -0.00179 0.00961 C11 1 0.219334 0.393248 0.875243 11.00000 0.01133 0.02480 = 0.02299 0.00078 0.00075 0.00983 AFIX 13 H11 2 0.289531 0.401840 0.867297 11.00000 -1.20000 AFIX 0 C12 1 0.056791 0.300121 0.945424 11.00000 0.02560 0.01703 = 0.01271 0.00433 0.00188 0.01111 AFIX 13 H12 2 0.020618 0.247895 0.983007 11.00000 -1.20000 AFIX 0 C13 1 0.122757 0.483667 0.909251 11.00000 0.02011 0.01662 = 0.02955 -0.00660 -0.00710 0.00802 AFIX 13 H13 2 0.129950 0.551738 0.922837 11.00000 -1.20000 AFIX 0 C14 1 0.156340 0.354881 0.808553 11.00000 0.02064 0.01871 = 0.02181 0.00509 0.00670 0.00990 AFIX 23 H14A 2 0.150246 0.288060 0.794723 11.00000 -1.20000 H14B 2 0.192523 0.405492 0.770829 11.00000 -1.20000 AFIX 0 C15 1 0.061052 0.446706 0.841599 11.00000 0.02459 0.01389 = 0.02527 0.00152 -0.00151 0.01071 AFIX 23 H15A 2 0.097639 0.498676 0.804666 11.00000 -1.20000 H15B 2 -0.007919 0.440012 0.848259 11.00000 -1.20000 AFIX 0 C16 1 0.164298 0.313104 0.933103 11.00000 0.02262 0.02138 = 0.01425 -0.00298 -0.00550 0.01238 AFIX 23 H16A 2 0.157351 0.245856 0.919456 11.00000 -1.20000 H16B 2 0.205573 0.336614 0.976400 11.00000 -1.20000 AFIX 0 C17 1 0.066811 0.405047 0.967077 11.00000 0.02947 0.02818 = 0.01964 -0.01067 -0.00902 0.01897 AFIX 23 H17A 2 -0.002800 0.396403 0.974642 11.00000 -1.20000 H17B 2 0.106461 0.429687 1.010950 11.00000 -1.20000 AFIX 0 C18 1 -0.006469 0.263359 0.878945 11.00000 0.01529 0.01458 = 0.01943 0.00236 0.00215 0.00819 AFIX 23 H18A 2 -0.075699 0.255360 0.887106 11.00000 -1.20000 H18B 2 -0.016314 0.194743 0.865885 11.00000 -1.20000 AFIX 0 C19 1 0.231386 0.497688 0.897465 11.00000 0.02023 0.01910 = 0.03288 0.00274 -0.00394 0.00513 AFIX 23 H19A 2 0.268221 0.550233 0.860894 11.00000 -1.20000 H19B 2 0.272430 0.521834 0.940827 11.00000 -1.20000 AFIX 0 C20 1 -0.139233 0.397179 0.617200 11.00000 0.04509 0.03051 = 0.02649 0.00152 -0.00843 0.02406 AFIX 137 H20A 2 -0.211789 0.359163 0.602227 11.00000 -1.50000 H20B 2 -0.094089 0.423177 0.576345 11.00000 -1.50000 H20C 2 -0.127929 0.455611 0.646615 11.00000 -1.50000 AFIX 0 K1 6 0.666667 0.333333 0.974859 10.33333 0.02025 0.02025 = 0.01541 0.00000 0.00000 0.01012 O2 4 0.802884 0.516093 0.904058 11.00000 0.02164 0.01951 = 0.04923 0.00332 0.00418 0.00525 O3 4 0.828143 0.505619 1.047452 11.00000 0.03927 0.03815 = 0.04135 -0.01823 -0.01031 0.01861 N2 3 0.666667 0.333333 0.823648 10.33333 0.03247 0.03247 = 0.02099 0.00000 0.00000 0.01623 N3 3 0.666667 0.333333 1.129815 10.33333 0.06461 0.06461 = 0.01541 0.00000 0.00000 0.03230 C21 1 0.714061 0.441198 0.798862 11.00000 0.04653 0.04773 = 0.02697 0.01658 0.01064 0.02531 AFIX 23 H21A 2 0.665575 0.466962 0.808350 11.00000 -1.20000 H21B 2 0.723001 0.441704 0.747872 11.00000 -1.20000 AFIX 0 C22 1 0.818245 0.515613 0.831387 11.00000 0.03511 0.03558 = 0.04530 0.01661 0.01655 0.01949 AFIX 23 H22A 2 0.868883 0.492706 0.821438 11.00000 -1.20000 H22B 2 0.845302 0.586111 0.812119 11.00000 -1.20000 AFIX 0 C23 1 0.896309 0.587732 0.937865 11.00000 0.02375 0.02314 = 0.07207 -0.00649 0.00329 0.00533 AFIX 23 H23A 2 0.928611 0.655108 0.913292 11.00000 -1.20000 H23B 2 0.945637 0.561517 0.937261 11.00000 -1.20000 AFIX 0 C24 1 0.872618 0.601359 1.010456 11.00000 0.02900 0.02487 = 0.08148 -0.02380 -0.00422 0.00732 AFIX 23 H24A 2 0.937081 0.652922 1.033986 11.00000 -1.20000 H24B 2 0.823709 0.628091 1.010657 11.00000 -1.20000 AFIX 0 C25 1 0.803538 0.518749 1.115635 11.00000 0.06128 0.05418 = 0.04527 -0.03002 -0.02810 0.02460 AFIX 23 H25A 2 0.748422 0.537400 1.115080 11.00000 -1.20000 H25B 2 0.865382 0.575443 1.138619 11.00000 -1.20000 AFIX 0 C26 1 0.766936 0.418993 1.154995 11.00000 0.08147 0.08084 = 0.02622 -0.02376 -0.02071 0.03973 AFIX 23 H26A 2 0.820024 0.397835 1.151130 11.00000 -1.20000 H26B 2 0.760098 0.431305 1.204754 11.00000 -1.20000 AFIX 0 HKLF 4 REM MR1523 in P6(3), ROSI/MEYER, [U(S)((Ad_ArO)3tacn)][K(2,2,2crypt)] REM R1 = 0.0319 for 4066 Fo > 4sig(Fo) and 0.0687 for all 5903 data REM 287 parameters refined using 1 restraints END WGHT 0.0067 1.4316 REM Instructions for potential hydrogen bonds EQIV $1 -y, x-y, z HTAB C1 O1_$1 REM Highest difference peak 0.721, deepest hole -0.626, 1-sigma level 0.089 Q1 1 -0.0781 -0.0174 0.7501 11.00000 0.05 0.72 Q2 1 0.0000 0.0000 0.6981 10.33333 0.05 0.71 Q3 1 0.0000 0.0000 0.9275 10.33333 0.05 0.66 Q4 1 0.0000 0.0000 0.8012 10.33333 0.05 0.66 Q5 1 -0.0174 0.0652 0.7483 11.00000 0.05 0.65 Q6 1 0.0000 0.0000 0.5710 10.33333 0.05 0.53 Q7 1 0.0268 0.3120 0.8545 11.00000 0.05 0.42 Q8 1 0.0425 0.3824 0.8304 11.00000 0.05 0.42 Q9 1 0.6667 0.3333 0.9135 10.33333 0.05 0.36 Q10 1 0.0208 -0.0344 0.8400 11.00000 0.05 0.35 Q11 1 0.7986 0.4529 1.1249 11.00000 0.05 0.35 Q12 1 -0.0405 0.0260 0.8403 11.00000 0.05 0.35 Q13 1 0.8969 0.5424 1.1296 11.00000 0.05 0.34 Q14 1 -0.0841 0.0566 0.6063 11.00000 0.05 0.34 Q15 1 0.6619 0.3742 0.8173 11.00000 0.05 0.33 Q16 1 -0.1047 0.1706 0.7072 11.00000 0.05 0.32 Q17 1 -0.1543 0.3457 0.6526 11.00000 0.05 0.32 Q18 1 0.1442 0.2811 0.9090 11.00000 0.05 0.32 Q19 1 -0.0381 0.2968 0.9755 11.00000 0.05 0.32 Q20 1 -0.1963 0.3593 0.5625 11.00000 0.05 0.32 ; _shelx_res_checksum 91934 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, 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 U1 U 0.0000 0.0000 0.74921(3) 0.01433(8) Uani 1 3 d S T P S1 S 0.0000 0.0000 0.88095(12) 0.0208(5) Uani 1 3 d S T P O1 O -0.0201(3) 0.1379(3) 0.7537(4) 0.0188(8) Uani 1 1 d . . . N1 N -0.1031(4) 0.0168(4) 0.6296(3) 0.0156(11) Uani 1 1 d . . . C1 C -0.1618(5) -0.0881(5) 0.5998(3) 0.0159(13) Uani 1 1 d . . . H1A H -0.2037 -0.0870 0.5602 0.024 Uiso 1 1 calc R . . H1B H -0.2101 -0.1359 0.6353 0.024 Uiso 1 1 calc R . . C2 C -0.0360(5) 0.0928(5) 0.5749(3) 0.0167(13) Uani 1 1 d . . . H2A H -0.0661 0.1362 0.5614 0.025 Uiso 1 1 calc R . . H2B H -0.0351 0.0543 0.5332 0.025 Uiso 1 1 calc R . . C3 C -0.1783(5) 0.0454(5) 0.6576(3) 0.0183(14) Uani 1 1 d . . . H3A H -0.2114 0.0032 0.6995 0.022 Uiso 1 1 calc R . . H3B H -0.2333 0.0278 0.6226 0.022 Uiso 1 1 calc R . . C4 C -0.1308(5) 0.1580(5) 0.6762(3) 0.0163(13) Uani 1 1 d . . . C5 C -0.0552(5) 0.1977(5) 0.7291(3) 0.0183(15) Uani 1 1 d . . . C6 C -0.0178(4) 0.3016(4) 0.7524(5) 0.0164(11) Uani 1 1 d . . . C7 C -0.0470(5) 0.3620(5) 0.7148(3) 0.0200(14) Uani 1 1 d . . . H7 H -0.0198 0.4322 0.7284 0.024 Uiso 1 1 calc R . . C8 C -0.1144(5) 0.3256(5) 0.6579(3) 0.0212(14) Uani 1 1 d . . . C9 C -0.1580(6) 0.2225(6) 0.6414(4) 0.0210(18) Uani 1 1 d . . . H9 H -0.2080 0.1947 0.6052 0.025 Uiso 1 1 calc R . . C10 C 0.0474(5) 0.3405(4) 0.8187(3) 0.0167(13) Uani 1 1 d . . . C11 C 0.2193(5) 0.3932(6) 0.8752(4) 0.0194(16) Uani 1 1 d . . . H11 H 0.2895 0.4018 0.8673 0.023 Uiso 1 1 calc R . . C12 C 0.0568(5) 0.3001(5) 0.9454(3) 0.0182(14) Uani 1 1 d . . . H12 H 0.0206 0.2479 0.9830 0.022 Uiso 1 1 calc R . . C13 C 0.1228(5) 0.4837(5) 0.9093(4) 0.0226(15) Uani 1 1 d . . . H13 H 0.1300 0.5517 0.9228 0.027 Uiso 1 1 calc R . . C14 C 0.1563(5) 0.3549(5) 0.8086(3) 0.0204(14) Uani 1 1 d . . . H14A H 0.1502 0.2881 0.7947 0.024 Uiso 1 1 calc R . . H14B H 0.1925 0.4055 0.7708 0.024 Uiso 1 1 calc R . . C15 C 0.0611(5) 0.4467(5) 0.8416(3) 0.0208(14) Uani 1 1 d . . . H15A H 0.0976 0.4987 0.8047 0.025 Uiso 1 1 calc R . . H15B H -0.0079 0.4400 0.8483 0.025 Uiso 1 1 calc R . . C16 C 0.1643(5) 0.3131(5) 0.9331(3) 0.0188(14) Uani 1 1 d . . . H16A H 0.1574 0.2459 0.9195 0.023 Uiso 1 1 calc R . . H16B H 0.2056 0.3366 0.9764 0.023 Uiso 1 1 calc R . . C17 C 0.0668(5) 0.4050(5) 0.9671(4) 0.0237(15) Uani 1 1 d . . . H17A H -0.0028 0.3964 0.9746 0.028 Uiso 1 1 calc R . . H17B H 0.1065 0.4297 1.0109 0.028 Uiso 1 1 calc R . . C18 C -0.0065(4) 0.2634(5) 0.8789(3) 0.0161(13) Uani 1 1 d . . . H18A H -0.0757 0.2554 0.8871 0.019 Uiso 1 1 calc R . . H18B H -0.0163 0.1947 0.8659 0.019 Uiso 1 1 calc R . . C19 C 0.2314(5) 0.4977(5) 0.8975(4) 0.0262(19) Uani 1 1 d . . . H19A H 0.2682 0.5502 0.8609 0.031 Uiso 1 1 calc R . . H19B H 0.2724 0.5218 0.9408 0.031 Uiso 1 1 calc R . . C20 C -0.1392(6) 0.3972(5) 0.6172(4) 0.0317(18) Uani 1 1 d . . . H20A H -0.2118 0.3592 0.6022 0.048 Uiso 1 1 calc GR . . H20B H -0.0941 0.4232 0.5763 0.048 Uiso 1 1 calc GR . . H20C H -0.1279 0.4556 0.6466 0.048 Uiso 1 1 calc GR . . K1 K 0.6667 0.3333 0.97486(12) 0.0186(5) Uani 1 3 d S T P O2 O 0.8029(4) 0.5161(4) 0.9041(3) 0.0324(14) Uani 1 1 d . . . O3 O 0.8281(4) 0.5056(4) 1.0475(3) 0.0399(14) Uani 1 1 d . . . N2 N 0.6667 0.3333 0.8236(6) 0.029(2) Uani 1 3 d S T P N3 N 0.6667 0.3333 1.1298(6) 0.048(3) Uani 1 3 d S T P C21 C 0.7141(6) 0.4412(6) 0.7989(4) 0.040(2) Uani 1 1 d . . . H21A H 0.6656 0.4670 0.8084 0.048 Uiso 1 1 calc R . . H21B H 0.7230 0.4417 0.7479 0.048 Uiso 1 1 calc R . . C22 C 0.8182(6) 0.5156(6) 0.8314(4) 0.038(2) Uani 1 1 d . . . H22A H 0.8689 0.4927 0.8214 0.045 Uiso 1 1 calc R . . H22B H 0.8453 0.5861 0.8121 0.045 Uiso 1 1 calc R . . C23 C 0.8963(6) 0.5877(6) 0.9379(5) 0.042(2) Uani 1 1 d . . . H23A H 0.9286 0.6551 0.9133 0.051 Uiso 1 1 calc R . . H23B H 0.9456 0.5615 0.9373 0.051 Uiso 1 1 calc R . . C24 C 0.8726(6) 0.6014(5) 1.0105(5) 0.048(3) Uani 1 1 d . . . H24A H 0.9371 0.6529 1.0340 0.057 Uiso 1 1 calc R . . H24B H 0.8237 0.6281 1.0107 0.057 Uiso 1 1 calc R . . C25 C 0.8035(9) 0.5187(9) 1.1156(6) 0.055(3) Uani 1 1 d . . . H25A H 0.7484 0.5374 1.1151 0.067 Uiso 1 1 calc R . . H25B H 0.8654 0.5754 1.1386 0.067 Uiso 1 1 calc R . . C26 C 0.7669(8) 0.4190(8) 1.1550(5) 0.063(3) Uani 1 1 d . . . H26A H 0.8200 0.3978 1.1511 0.076 Uiso 1 1 calc R . . H26B H 0.7601 0.4313 1.2048 0.076 Uiso 1 1 calc R . . 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 0.01300(9) 0.01300(9) 0.01698(14) 0.000 0.000 0.00650(5) S1 0.0230(7) 0.0230(7) 0.0164(12) 0.000 0.000 0.0115(4) O1 0.0217(19) 0.0191(18) 0.020(2) -0.006(3) -0.006(3) 0.0135(16) N1 0.016(3) 0.012(3) 0.019(3) -0.001(2) 0.000(2) 0.008(2) C1 0.018(3) 0.015(3) 0.016(3) 0.002(3) -0.002(3) 0.008(3) C2 0.019(3) 0.019(3) 0.012(3) 0.002(3) 0.000(3) 0.010(3) C3 0.015(3) 0.022(3) 0.019(4) -0.004(3) -0.006(3) 0.010(3) C4 0.017(3) 0.022(3) 0.011(3) 0.001(3) 0.005(3) 0.011(3) C5 0.018(3) 0.021(3) 0.017(4) 0.003(2) 0.004(2) 0.010(3) C6 0.016(2) 0.020(3) 0.014(3) 0.003(4) 0.004(4) 0.010(2) C7 0.025(4) 0.016(3) 0.021(4) 0.002(3) 0.008(3) 0.012(3) C8 0.026(4) 0.027(4) 0.016(3) 0.006(3) 0.004(3) 0.017(3) C9 0.021(4) 0.034(4) 0.017(4) -0.005(3) -0.003(3) 0.020(3) C10 0.019(3) 0.014(3) 0.019(3) 0.000(3) -0.002(3) 0.010(3) C11 0.011(3) 0.025(4) 0.023(4) 0.001(3) 0.001(3) 0.010(3) C12 0.026(4) 0.017(3) 0.013(3) 0.004(3) 0.002(3) 0.011(3) C13 0.020(4) 0.017(3) 0.030(4) -0.007(3) -0.007(3) 0.008(3) C14 0.021(3) 0.019(3) 0.022(4) 0.005(3) 0.007(3) 0.010(3) C15 0.025(3) 0.014(3) 0.025(4) 0.002(3) -0.002(3) 0.011(3) C16 0.023(3) 0.021(3) 0.014(3) -0.003(3) -0.005(3) 0.012(3) C17 0.029(4) 0.028(4) 0.020(4) -0.011(3) -0.009(3) 0.019(3) C18 0.015(3) 0.015(3) 0.019(4) 0.002(3) 0.002(3) 0.008(3) C19 0.020(4) 0.019(4) 0.033(5) 0.003(4) -0.004(4) 0.005(3) C20 0.045(5) 0.031(4) 0.026(4) 0.002(3) -0.008(4) 0.024(4) K1 0.0202(7) 0.0202(7) 0.0154(12) 0.000 0.000 0.0101(3) O2 0.022(3) 0.020(3) 0.049(4) 0.003(3) 0.004(3) 0.005(3) O3 0.039(3) 0.038(3) 0.041(4) -0.018(3) -0.010(3) 0.019(3) N2 0.032(4) 0.032(4) 0.021(6) 0.000 0.000 0.0162(18) N3 0.065(6) 0.065(6) 0.015(6) 0.000 0.000 0.032(3) C21 0.047(5) 0.048(5) 0.027(5) 0.017(4) 0.011(4) 0.025(4) C22 0.035(4) 0.036(4) 0.045(6) 0.017(4) 0.017(4) 0.019(4) C23 0.024(4) 0.023(4) 0.072(7) -0.006(4) 0.003(4) 0.005(4) C24 0.029(4) 0.025(4) 0.081(9) -0.024(5) -0.004(5) 0.007(3) C25 0.061(7) 0.054(7) 0.045(7) -0.030(5) -0.028(6) 0.025(6) C26 0.081(8) 0.081(8) 0.026(5) -0.024(5) -0.021(5) 0.040(7) 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 S1 U1 N1 143.95(11) . 3 S1 U1 N1 143.95(10) . 2 S1 U1 N1 143.95(10) . . O1 U1 S1 87.79(18) 2 . O1 U1 S1 87.79(18) . . O1 U1 S1 87.79(18) 3 . O1 U1 O1 119.85(3) . 3 O1 U1 O1 119.85(2) 2 3 O1 U1 O1 119.85(2) 2 . O1 U1 N1 127.0(2) 2 3 O1 U1 N1 82.57(19) 2 . O1 U1 N1 82.57(19) . 3 O1 U1 N1 67.76(19) 2 2 O1 U1 N1 127.0(2) . 2 O1 U1 N1 67.76(19) 3 3 O1 U1 N1 67.76(19) . . O1 U1 N1 127.0(2) 3 . O1 U1 N1 82.57(19) 3 2 N1 U1 N1 61.28(17) . 2 N1 U1 N1 61.28(17) 2 3 N1 U1 N1 61.28(17) . 3 C5 O1 U1 152.7(5) . . C1 N1 U1 106.4(3) . . C1 N1 C2 110.2(5) . . C1 N1 C3 108.2(5) . . C2 N1 U1 116.6(3) . . C3 N1 U1 104.5(4) . . C3 N1 C2 110.6(5) . . N1 C1 H1A 109.0 . . N1 C1 H1B 109.0 . . N1 C1 C2 112.8(5) . 2 H1A C1 H1B 107.8 . . C2 C1 H1A 109.0 2 . C2 C1 H1B 109.0 2 . N1 C2 C1 112.2(5) . 3 N1 C2 H2A 109.2 . . N1 C2 H2B 109.2 . . C1 C2 H2A 109.2 3 . C1 C2 H2B 109.2 3 . H2A C2 H2B 107.9 . . N1 C3 H3A 108.8 . . N1 C3 H3B 108.8 . . N1 C3 C4 113.9(5) . . H3A C3 H3B 107.7 . . C4 C3 H3A 108.8 . . C4 C3 H3B 108.8 . . C5 C4 C3 118.1(6) . . C9 C4 C3 121.4(6) . . C9 C4 C5 120.5(6) . . O1 C5 C4 118.5(6) . . O1 C5 C6 122.9(6) . . C4 C5 C6 118.6(6) . . C5 C6 C10 120.1(5) . . C7 C6 C5 117.4(7) . . C7 C6 C10 122.4(5) . . C6 C7 H7 118.1 . . C6 C7 C8 123.8(6) . . C8 C7 H7 118.1 . . C7 C8 C20 120.9(6) . . C9 C8 C7 117.5(6) . . C9 C8 C20 121.5(6) . . C4 C9 H9 119.2 . . C8 C9 C4 121.6(6) . . C8 C9 H9 119.2 . . C6 C10 C14 111.9(5) . . C6 C10 C15 110.9(5) . . C6 C10 C18 110.4(5) . . C14 C10 C15 107.5(5) . . C14 C10 C18 108.5(5) . . C18 C10 C15 107.4(5) . . C14 C11 H11 109.2 . . C14 C11 C16 109.3(6) . . C14 C11 C19 110.7(6) . . C16 C11 H11 109.2 . . C19 C11 H11 109.2 . . C19 C11 C16 109.4(6) . . C16 C12 H12 109.4 . . C16 C12 C17 110.3(5) . . C17 C12 H12 109.4 . . C18 C12 H12 109.4 . . C18 C12 C16 109.6(5) . . C18 C12 C17 108.6(5) . . C15 C13 H13 109.2 . . C15 C13 C19 109.0(6) . . C17 C13 H13 109.2 . . C17 C13 C15 110.2(5) . . C17 C13 C19 110.2(6) . . C19 C13 H13 109.2 . . C10 C14 H14A 109.5 . . C10 C14 H14B 109.5 . . C11 C14 C10 110.8(5) . . C11 C14 H14A 109.5 . . C11 C14 H14B 109.5 . . H14A C14 H14B 108.1 . . C10 C15 H15A 109.5 . . C10 C15 H15B 109.5 . . C13 C15 C10 110.9(5) . . C13 C15 H15A 109.5 . . C13 C15 H15B 109.5 . . H15A C15 H15B 108.0 . . C11 C16 H16A 109.8 . . C11 C16 H16B 109.8 . . C12 C16 C11 109.2(5) . . C12 C16 H16A 109.8 . . C12 C16 H16B 109.8 . . H16A C16 H16B 108.3 . . C12 C17 H17A 110.0 . . C12 C17 H17B 110.0 . . C13 C17 C12 108.5(5) . . C13 C17 H17A 110.0 . . C13 C17 H17B 110.0 . . H17A C17 H17B 108.4 . . C10 C18 H18A 109.3 . . C10 C18 H18B 109.3 . . C12 C18 C10 111.5(5) . . C12 C18 H18A 109.3 . . C12 C18 H18B 109.3 . . H18A C18 H18B 108.0 . . C11 C19 C13 108.7(5) . . C11 C19 H19A 109.9 . . C11 C19 H19B 109.9 . . C13 C19 H19A 109.9 . . C13 C19 H19B 109.9 . . H19A C19 H19B 108.3 . . 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 K1 O2 98.39(17) 3_665 2_655 O2 K1 O2 98.39(17) 3_665 . O2 K1 O2 98.39(17) . 2_655 O2 K1 O3 59.30(18) 3_665 3_665 O2 K1 O3 59.30(18) . . O2 K1 O3 119.10(15) . 2_655 O2 K1 O3 137.52(15) . 3_665 O2 K1 O3 137.52(16) 3_665 2_655 O2 K1 O3 119.09(16) 2_655 3_665 O2 K1 O3 59.30(18) 2_655 2_655 O2 K1 O3 119.09(16) 3_665 . O2 K1 O3 137.52(15) 2_655 . O2 K1 N2 60.93(13) . . O2 K1 N2 60.93(13) 2_655 . O2 K1 N2 60.93(13) 3_665 . O2 K1 N3 119.07(13) . . O2 K1 N3 119.07(13) 2_655 . O2 K1 N3 119.07(13) 3_665 . O3 K1 O3 98.10(16) . 2_655 O3 K1 O3 98.10(17) 3_665 2_655 O3 K1 O3 98.10(17) 3_665 . O3 K1 N2 119.29(13) 3_665 . O3 K1 N2 119.29(13) . . O3 K1 N2 119.29(13) 2_655 . O3 K1 N3 60.71(13) . . O3 K1 N3 60.71(13) 2_655 . O3 K1 N3 60.71(13) 3_665 . N2 K1 N3 180.0 . . C22 O2 K1 121.0(4) . . C22 O2 C23 110.9(6) . . C23 O2 K1 118.0(5) . . C24 O3 K1 114.6(5) . . C25 O3 K1 114.9(5) . . C25 O3 C24 110.5(7) . . C21 N2 K1 108.9(5) . . C21 N2 K1 108.9(5) 2_655 . C21 N2 K1 108.9(5) 3_665 . C21 N2 C21 110.1(5) 3_665 2_655 C21 N2 C21 110.1(5) 3_665 . C21 N2 C21 110.1(5) 2_655 . C26 N3 K1 109.1(6) . . C26 N3 K1 109.1(6) 3_665 . C26 N3 K1 109.1(6) 2_655 . C26 N3 C26 109.8(6) . 2_655 C26 N3 C26 109.8(6) 3_665 . C26 N3 C26 109.8(6) 3_665 2_655 N2 C21 H21A 108.6 . . N2 C21 H21B 108.6 . . N2 C21 C22 114.8(6) . . H21A C21 H21B 107.5 . . C22 C21 H21A 108.6 . . C22 C21 H21B 108.6 . . O2 C22 C21 107.5(6) . . O2 C22 H22A 110.2 . . O2 C22 H22B 110.2 . . C21 C22 H22A 110.2 . . C21 C22 H22B 110.2 . . H22A C22 H22B 108.5 . . O2 C23 H23A 109.9 . . O2 C23 H23B 109.9 . . O2 C23 C24 108.9(6) . . H23A C23 H23B 108.3 . . C24 C23 H23A 109.9 . . C24 C23 H23B 109.9 . . O3 C24 C23 110.9(6) . . O3 C24 H24A 109.5 . . O3 C24 H24B 109.5 . . C23 C24 H24A 109.5 . . C23 C24 H24B 109.5 . . H24A C24 H24B 108.0 . . O3 C25 H25A 109.9 . . O3 C25 H25B 109.9 . . O3 C25 C26 108.9(9) . . H25A C25 H25B 108.3 . . C26 C25 H25A 109.9 . . C26 C25 H25B 109.9 . . N3 C26 C25 113.4(8) . . N3 C26 H26A 108.9 . . N3 C26 H26B 108.9 . . C25 C26 H26A 108.9 . . C25 C26 H26B 108.9 . . H26A C26 H26B 107.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 S1 2.536(2) . U1 O1 2.222(3) 2 U1 O1 2.222(3) . U1 O1 2.222(3) 3 U1 N1 2.848(5) 2 U1 N1 2.848(5) 3 U1 N1 2.848(5) . O1 C5 1.326(7) . N1 C1 1.473(7) . N1 C2 1.502(8) . N1 C3 1.484(7) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.510(8) 2 C2 C1 1.510(8) 3 C2 H2A 0.9900 . C2 H2B 0.9900 . C3 H3A 0.9900 . C3 H3B 0.9900 . C3 C4 1.504(8) . C4 C5 1.410(8) . C4 C9 1.388(9) . C5 C6 1.431(8) . C6 C7 1.384(9) . C6 C10 1.531(10) . C7 H7 0.9500 . C7 C8 1.399(9) . C8 C9 1.373(10) . C8 C20 1.511(9) . C9 H9 0.9500 . C10 C14 1.540(8) . C10 C15 1.556(8) . C10 C18 1.545(8) . C11 H11 1.0000 . C11 C14 1.523(9) . C11 C16 1.536(9) . C11 C19 1.535(10) . C12 H12 1.0000 . C12 C16 1.533(8) . C12 C17 1.551(8) . C12 C18 1.520(8) . C13 H13 1.0000 . C13 C15 1.529(9) . C13 C17 1.526(9) . 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 . K1 O2 2.805(5) 3_665 K1 O2 2.805(5) 2_655 K1 O2 2.805(6) . K1 O3 2.856(5) . K1 O3 2.856(5) 2_655 K1 O3 2.856(5) 3_665 K1 N2 2.911(11) . K1 N3 2.983(11) . O2 C22 1.418(9) . O2 C23 1.419(9) . O3 C24 1.427(9) . O3 C25 1.402(11) . N2 C21 1.475(8) . N2 C21 1.475(8) 3_665 N2 C21 1.475(8) 2_655 N3 C26 1.480(10) . N3 C26 1.480(9) 2_655 N3 C26 1.480(9) 3_665 C21 H21A 0.9900 . C21 H21B 0.9900 . C21 C22 1.520(11) . C22 H22A 0.9900 . C22 H22B 0.9900 . C23 H23A 0.9900 . C23 H23B 0.9900 . C23 C24 1.480(12) . C24 H24A 0.9900 . C24 H24B 0.9900 . C25 H25A 0.9900 . C25 H25B 0.9900 . C25 C26 1.507(14) . C26 H26A 0.9900 . C26 H26B 0.9900 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 U1 O1 C5 C4 14.1(13) . . U1 O1 C5 C6 -164.1(7) . . U1 N1 C1 C2 -63.5(5) . 2 U1 N1 C2 C1 -10.8(6) . 3 U1 N1 C3 C4 79.0(5) . . O1 C5 C6 C7 169.2(6) . . O1 C5 C6 C10 -13.9(9) . . N1 C3 C4 C5 -62.8(7) . . N1 C3 C4 C9 115.5(7) . . C1 N1 C2 C1 -132.1(5) . 3 C1 N1 C3 C4 -168.0(5) . . C2 N1 C1 C2 63.7(6) . 2 C2 N1 C3 C4 -47.2(7) . . C3 N1 C1 C2 -175.3(5) . 2 C3 N1 C2 C1 108.3(5) . 3 C3 C4 C5 O1 8.4(9) . . C3 C4 C5 C6 -173.3(6) . . C3 C4 C9 C8 -179.6(6) . . C4 C5 C6 C7 -9.1(9) . . C4 C5 C6 C10 167.9(5) . . C5 C4 C9 C8 -1.3(10) . . C5 C6 C7 C8 3.1(10) . . C5 C6 C10 C14 71.0(7) . . C5 C6 C10 C15 -169.0(6) . . C5 C6 C10 C18 -50.0(7) . . C6 C7 C8 C9 3.8(10) . . C6 C7 C8 C20 -177.2(6) . . C6 C10 C14 C11 -179.9(5) . . C6 C10 C15 C13 177.9(5) . . C6 C10 C18 C12 179.9(5) . . C7 C6 C10 C14 -112.2(7) . . C7 C6 C10 C15 7.8(8) . . C7 C6 C10 C18 126.8(6) . . C7 C8 C9 C4 -4.7(10) . . C9 C4 C5 O1 -169.9(6) . . C9 C4 C5 C6 8.4(9) . . C10 C6 C7 C8 -173.8(6) . . C14 C10 C15 C13 -59.5(7) . . C14 C10 C18 C12 57.0(6) . . C14 C11 C16 C12 -60.8(7) . . C14 C11 C19 C13 59.6(8) . . C15 C10 C14 C11 58.1(7) . . C15 C10 C18 C12 -59.0(6) . . C15 C13 C17 C12 60.4(7) . . C15 C13 C19 C11 -59.8(7) . . C16 C11 C14 C10 60.6(7) . . C16 C11 C19 C13 -60.9(7) . . C16 C12 C17 C13 59.2(7) . . C16 C12 C18 C10 -58.8(6) . . C17 C12 C16 C11 -59.7(7) . . C17 C12 C18 C10 61.8(6) . . C17 C13 C15 C10 -59.8(7) . . C17 C13 C19 C11 61.3(7) . . C18 C10 C14 C11 -57.7(6) . . C18 C10 C15 C13 57.2(7) . . C18 C12 C16 C11 59.9(7) . . C18 C12 C17 C13 -60.9(6) . . C19 C11 C14 C10 -59.9(7) . . C19 C11 C16 C12 60.5(7) . . C19 C13 C15 C10 61.2(7) . . C19 C13 C17 C12 -59.8(7) . . C20 C8 C9 C4 176.3(6) . . K1 O2 C22 C21 38.2(7) . . K1 O2 C23 C24 -45.6(8) . . K1 O3 C24 C23 -46.7(7) . . K1 O3 C25 C26 54.0(9) . . K1 N2 C21 C22 50.4(7) . . K1 N3 C26 C25 43.1(9) . . O2 C23 C24 O3 60.9(8) . . O3 C25 C26 N3 -67.4(11) . . N2 C21 C22 O2 -60.2(8) . . C21 N2 C21 C22 -68.9(11) 3_665 . C21 N2 C21 C22 169.6(6) 2_655 . C22 O2 C23 C24 168.7(6) . . C23 O2 C22 C21 -177.3(6) . . C24 O3 C25 C26 -174.4(7) . . C25 O3 C24 C23 -178.5(7) . . C26 N3 C26 C25 -76.5(14) 2_655 . C26 N3 C26 C25 162.7(9) 3_665 .