#------------------------------------------------------------------------------ #$Date: 2021-06-05 21:07:14 +0300 (Sat, 05 Jun 2021) $ #$Revision: 265940 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/24/7242498.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_7242498 loop_ _publ_author_name 'Wang, Hui-Sheng' 'Zhang, Ke' 'Wang, Jia' 'Hu, Zhaobo' 'Song, You' 'Zhang, Zaichao' 'Pan, Zhi-Quan' _publ_section_title ; Regulating the distortion degree of the square antiprism coordination geometry in Dy--Na single ion magnets ; _journal_issue 17 _journal_name_full CrystEngComm _journal_page_first 3175 _journal_page_last 3184 _journal_paper_doi 10.1039/D1CE00146A _journal_volume 23 _journal_year 2021 _chemical_formula_sum 'C46 H44 Dy N5 Na2 O13' _chemical_formula_weight 1083.34 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-12-31 deposited with the CCDC. 2021-03-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.4410(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.9971(4) _cell_length_b 29.7015(10) _cell_length_c 14.6760(4) _cell_measurement_reflns_used 6417 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.33 _cell_measurement_theta_min 2.74 _cell_volume 4461.9(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'PHOTON 100 CMOS detector' _diffrn_measurement_method 'omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 25671 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.872 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.767 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.613 _exptl_crystal_description block _exptl_crystal_F_000 2188 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _refine_diff_density_max 1.115 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 612 _refine_ls_number_reflns 7813 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0349 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+3.6837P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.0765 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6085 _reflns_number_total 7813 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce00146a2.cif _cod_data_source_block complex_2 _cod_depositor_comments 'Adding full bibliography for 7242497--7242498.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7242498 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P2(1)/c CELL 0.71073 10.9971 29.7015 14.6760 90.000 111.441 90.000 ZERR 4.00 0.0004 0.0010 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Na Dy UNIT 184 176 20 52 8 4 omit 0 3 1 omit 1 3 0 omit 1 14 1 omit -2 5 3 omit 0 2 4 omit -1 2 2 omit 0 1 3 omit 0 1 5 OMIT 0.00 50.00 L.S. 15 ACTA BOND $h FMAP 2 PLAN 20 HTAB O13 O12_$2 EQIV $2 x, y+1, z-1 HTAB O12 O6_$1 EQIV $1 x, y, z+1 HTAB C43 O10 isor 0.002 o13 htab isor 0.001 c46 FREE Dy1 Na1 FREE Dy1 Na2 free Na1 Na2 TEMP -100.250 WGHT 0.029700 3.683700 FVAR 0.07240 MOLE 1 C1 1 0.289666 0.110001 0.496271 11.00000 0.03347 0.01545 = 0.01873 0.00072 0.01105 0.00376 C2 1 0.404226 0.107914 0.582909 11.00000 0.03203 0.01957 = 0.02555 -0.00121 0.00820 0.00453 C3 1 0.410784 0.081788 0.661784 11.00000 0.04563 0.02406 = 0.02797 0.00601 0.00910 0.01097 AFIX 43 H3 2 0.490061 0.079976 0.716958 11.00000 -1.20000 AFIX 0 C4 1 0.301730 0.058033 0.660971 11.00000 0.05344 0.03161 = 0.03210 0.01074 0.01794 0.00896 AFIX 43 H4 2 0.305667 0.040646 0.716312 11.00000 -1.20000 AFIX 0 C5 1 0.188827 0.059642 0.580692 11.00000 0.04949 0.01972 = 0.04184 0.00322 0.02787 0.00070 AFIX 43 H5 2 0.114338 0.043659 0.581377 11.00000 -1.20000 AFIX 0 C6 1 0.180298 0.084695 0.496152 11.00000 0.03406 0.01907 = 0.03078 -0.00089 0.01615 0.00210 C7 1 0.056735 0.086467 0.415801 11.00000 0.03134 0.01997 = 0.03522 -0.00261 0.01821 -0.00357 AFIX 43 H7 2 -0.016153 0.073693 0.426453 11.00000 -1.20000 AFIX 0 MOLE 2 C8 1 -0.095103 0.105720 0.261235 11.00000 0.01390 0.03585 = 0.03070 -0.01001 0.01040 -0.00511 C9 1 -0.190601 0.073516 0.251861 11.00000 0.03182 0.05089 = 0.04099 -0.01531 0.01970 -0.01575 AFIX 43 H9 2 -0.171434 0.047936 0.293598 11.00000 -1.20000 AFIX 0 C10 1 -0.313629 0.079080 0.181264 11.00000 0.02723 0.06357 = 0.06295 -0.02254 0.01617 -0.02221 AFIX 43 H10 2 -0.379784 0.057526 0.175732 11.00000 -1.20000 AFIX 0 C11 1 -0.341629 0.115303 0.119013 11.00000 0.02698 0.07523 = 0.05194 -0.01630 0.00017 -0.00914 AFIX 43 H11 2 -0.426594 0.118284 0.070403 11.00000 -1.20000 AFIX 0 C12 1 -0.247274 0.147761 0.126068 11.00000 0.02795 0.04474 = 0.04261 -0.00817 0.00376 -0.00003 AFIX 43 H12 2 -0.266919 0.172597 0.082270 11.00000 -1.20000 AFIX 0 C13 1 -0.123006 0.143185 0.198764 11.00000 0.01562 0.03471 = 0.03004 -0.01314 0.00421 0.00145 MOLE 1 C14 1 -0.044272 0.216109 0.195986 11.00000 0.02305 0.03600 = 0.02104 -0.00141 0.00568 0.01044 AFIX 43 H14 2 -0.133756 0.224466 0.174460 11.00000 -1.20000 AFIX 0 C15 1 0.185397 0.245845 0.251887 11.00000 0.02759 0.02105 = 0.01713 -0.00185 0.00993 0.00359 C16 1 0.048431 0.252294 0.207116 11.00000 0.02836 0.02509 = 0.01597 -0.00035 0.00644 0.00802 C17 1 -0.001061 0.295571 0.175334 11.00000 0.03564 0.03941 = 0.02344 0.00754 0.00916 0.01389 AFIX 43 H17 2 -0.092913 0.299864 0.146941 11.00000 -1.20000 AFIX 0 C18 1 0.079220 0.331248 0.184283 11.00000 0.04721 0.02276 = 0.04654 0.01276 0.02426 0.01822 AFIX 43 H18 2 0.043399 0.360166 0.162604 11.00000 -1.20000 AFIX 0 C19 1 0.214097 0.325621 0.225181 11.00000 0.04913 0.01972 = 0.05603 0.00817 0.03081 0.00611 AFIX 43 H19 2 0.270370 0.350472 0.229623 11.00000 -1.20000 AFIX 0 C20 1 0.265851 0.283909 0.259229 11.00000 0.03367 0.01601 = 0.03753 0.00241 0.01730 0.00581 C21 1 0.630877 0.128713 0.649416 11.00000 0.02885 0.04798 = 0.03006 0.00151 -0.00192 0.01033 AFIX 137 H21A 2 0.630338 0.136723 0.714045 11.00000 -1.50000 H21B 2 0.693384 0.147900 0.634127 11.00000 -1.50000 H21C 2 0.656438 0.097095 0.649590 11.00000 -1.50000 AFIX 0 MOLE 2 C22 1 0.487956 0.309404 0.311282 11.00000 0.03984 0.02572 = 0.15977 0.00609 0.03994 -0.00591 AFIX 137 H22A 2 0.474802 0.322327 0.246927 11.00000 -1.50000 H22B 2 0.577435 0.297937 0.340842 11.00000 -1.50000 H22C 2 0.473555 0.332677 0.353595 11.00000 -1.50000 AFIX 0 C23 1 0.511990 0.113436 0.342407 11.00000 0.02029 0.02103 = 0.01979 0.00269 0.00806 0.00437 C24 1 0.632509 0.136122 0.387154 11.00000 0.02121 0.02388 = 0.01886 0.00288 0.00807 0.00228 C25 1 0.742768 0.114865 0.447700 11.00000 0.02019 0.03348 = 0.02595 0.00144 0.00584 0.00326 AFIX 43 H25 2 0.821955 0.131196 0.476279 11.00000 -1.20000 AFIX 0 C26 1 0.738189 0.068467 0.467487 11.00000 0.02029 0.03828 = 0.03068 0.01149 0.00777 0.01088 AFIX 43 H26 2 0.814438 0.053336 0.508967 11.00000 -1.20000 AFIX 0 C27 1 0.624090 0.045685 0.426809 11.00000 0.03191 0.02810 = 0.03383 0.01009 0.01439 0.00877 AFIX 43 H27 2 0.621806 0.014448 0.440006 11.00000 -1.20000 AFIX 0 C28 1 0.508556 0.067167 0.365340 11.00000 0.02103 0.02361 = 0.02570 -0.00006 0.01010 0.00345 C29 1 0.393172 0.039847 0.326459 11.00000 0.03001 0.01832 = 0.03033 0.00449 0.01119 0.00374 AFIX 43 H29 2 0.405647 0.008190 0.332992 11.00000 -1.20000 AFIX 0 MOLE 1 C30 1 0.171295 0.021498 0.249396 11.00000 0.03336 0.01901 = 0.03030 -0.00321 0.01819 -0.00446 C31 1 0.173450 -0.019711 0.294582 11.00000 0.03556 0.02748 = 0.04462 0.00611 0.01387 -0.00370 AFIX 43 H31 2 0.247140 -0.027948 0.350412 11.00000 -1.20000 AFIX 0 C32 1 0.068993 -0.048646 0.258614 11.00000 0.05559 0.01953 = 0.06215 0.00669 0.02520 -0.01046 AFIX 43 H32 2 0.071788 -0.077053 0.289063 11.00000 -1.20000 AFIX 0 C33 1 -0.039912 -0.036771 0.178634 11.00000 0.04462 0.02660 = 0.05866 -0.00256 0.01345 -0.01955 AFIX 43 H33 2 -0.111444 -0.057016 0.154324 11.00000 -1.20000 AFIX 0 C34 1 -0.044960 0.004402 0.134048 11.00000 0.03468 0.02850 = 0.04061 -0.00547 0.00721 -0.01117 AFIX 43 H34 2 -0.120315 0.012689 0.079547 11.00000 -1.20000 AFIX 0 C35 1 0.060602 0.033825 0.169041 11.00000 0.02518 0.01862 = 0.02680 -0.00319 0.01113 -0.00346 C36 1 -0.004574 0.086754 0.041068 11.00000 0.02680 0.03019 = 0.02162 -0.00651 0.00296 -0.00716 AFIX 43 H36 2 -0.054785 0.063119 0.001320 11.00000 -1.20000 AFIX 0 C37 1 0.090184 0.162932 0.035854 11.00000 0.01913 0.02842 = 0.01629 -0.00203 0.00679 0.00008 C38 1 -0.008972 0.130557 -0.003791 11.00000 0.02661 0.02700 = 0.01914 -0.00353 0.00494 -0.00150 C39 1 -0.116097 0.140318 -0.090488 11.00000 0.02584 0.03947 = 0.02153 -0.00423 0.00175 -0.00261 AFIX 43 H39 2 -0.180963 0.118046 -0.118817 11.00000 -1.20000 AFIX 0 C40 1 -0.126963 0.181419 -0.133677 11.00000 0.02467 0.04199 = 0.02244 -0.00079 0.00083 0.00172 AFIX 43 H40 2 -0.199962 0.187836 -0.191478 11.00000 -1.20000 AFIX 0 C41 1 -0.031174 0.214265 -0.093383 11.00000 0.03283 0.02584 = 0.02430 0.00564 0.01431 0.00794 AFIX 43 H41 2 -0.040612 0.243087 -0.123254 11.00000 -1.20000 AFIX 0 C42 1 0.076001 0.205295 -0.011363 11.00000 0.02010 0.02938 = 0.01803 -0.00002 0.00614 0.00191 MOLE 2 C43 1 0.745113 0.205288 0.393819 11.00000 0.02249 0.03367 = 0.03381 -0.00134 0.00400 -0.01082 AFIX 137 H43A 2 0.786356 0.205315 0.465378 11.00000 -1.50000 H43B 2 0.728781 0.236371 0.370060 11.00000 -1.50000 H43C 2 0.803169 0.190576 0.365755 11.00000 -1.50000 AFIX 0 MOLE 1 C44 1 0.163133 0.278892 -0.005544 11.00000 0.04245 0.02224 = 0.03259 0.00386 0.01561 0.00071 AFIX 137 H44A 2 0.156994 0.277760 -0.073825 11.00000 -1.50000 H44B 2 0.239639 0.296710 0.033058 11.00000 -1.50000 H44C 2 0.084046 0.292838 -0.002314 11.00000 -1.50000 AFIX 0 MOLE 2 C45 1 0.308402 0.120754 0.947102 11.00000 0.05289 0.10518 = 0.05474 -0.00943 0.01807 -0.02271 AFIX 137 H45A 2 0.352575 0.149611 0.969161 11.00000 -1.50000 H45B 2 0.215720 0.126105 0.908944 11.00000 -1.50000 H45C 2 0.348530 0.105255 0.906211 11.00000 -1.50000 AFIX 0 C46 1 0.382343 0.980255 0.094992 11.00000 0.11721 0.11332 = 0.10955 0.00766 0.04052 -0.00627 AFIX 137 H46A 2 0.464083 0.983911 0.151353 11.00000 -1.50000 H46B 2 0.373712 0.948889 0.072802 11.00000 -1.50000 H46C 2 0.308417 0.988178 0.114028 11.00000 -1.50000 AFIX 0 MOLE 1 DY1 6 0.194455 0.132996 0.260299 11.00000 0.01617 0.01585 = 0.01781 -0.00056 0.00400 -0.00075 N1 3 0.035379 0.103658 0.330989 11.00000 0.02144 0.02376 = 0.02907 -0.00622 0.01056 -0.00522 N2 3 -0.018942 0.173992 0.211983 11.00000 0.02034 0.02688 = 0.02198 -0.00310 0.00421 0.00242 N3 3 0.274445 0.053576 0.283636 11.00000 0.02574 0.01640 = 0.02565 -0.00029 0.01262 0.00030 N4 3 0.063106 0.077897 0.131370 11.00000 0.02222 0.01882 = 0.02431 -0.00127 0.00997 -0.00054 N5 3 0.567178 0.249129 0.601433 11.00000 0.03070 0.02892 = 0.03347 -0.00776 0.01254 -0.00673 MOLE 2 NA1 5 0.436492 0.198317 0.428462 11.00000 0.02191 0.03120 = 0.02857 -0.00734 0.00365 -0.00229 NA2 5 0.389485 0.202640 0.180162 11.00000 0.03298 0.02887 = 0.03211 0.00288 0.01564 -0.00208 MOLE 1 O1 4 0.289802 0.135874 0.425189 11.00000 0.02502 0.02272 = 0.01773 -0.00082 0.00562 -0.00379 O2 4 0.241960 0.207443 0.286607 11.00000 0.02066 0.01688 = 0.02608 0.00232 0.00231 0.00163 O3 4 0.504056 0.135117 0.577674 11.00000 0.02621 0.03577 = 0.02553 0.00355 -0.00273 -0.00293 O4 4 0.397521 0.273292 0.300304 11.00000 0.03054 0.02077 = 0.06418 0.00400 0.01800 -0.00266 MOLE 2 O5 4 0.411561 0.135883 0.283741 11.00000 0.01508 0.02329 = 0.02240 0.00378 0.00522 0.00221 MOLE 1 O6 4 0.197439 0.154805 0.112376 11.00000 0.02264 0.03015 = 0.01686 0.00387 0.00025 -0.00510 MOLE 2 O7 4 0.624577 0.181462 0.365144 11.00000 0.01916 0.02266 = 0.03040 0.00212 0.00514 -0.00336 MOLE 1 O8 4 0.175845 0.234241 0.033007 11.00000 0.02921 0.02521 = 0.02650 0.00473 0.01027 -0.00386 O9 4 0.448104 0.254446 0.556876 11.00000 0.02360 0.06887 = 0.05285 -0.01901 0.00943 0.00850 O10 4 0.633204 0.230622 0.558854 11.00000 0.02615 0.04755 = 0.05052 -0.01665 0.01716 -0.00171 O11 4 0.617092 0.262279 0.686442 11.00000 0.06012 0.08397 = 0.02978 -0.02428 0.01177 -0.01931 MOLE 2 O12 4 0.320130 0.094571 1.026859 11.00000 0.06989 0.10765 = 0.09024 -0.01181 0.03978 0.02221 AFIX 147 H12A 2 0.283172 0.107398 1.060755 11.00000 -1.50000 AFIX 0 O13 4 0.383533 1.009047 0.017576 11.00000 0.21298 0.21129 = 0.21193 -0.00581 0.07165 0.00275 AFIX 147 H13 2 0.353265 1.034363 0.023617 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0349 for 6085 Fo > 4sig(Fo) and 0.0553 for all 7813 data REM 612 parameters refined using 12 restraints END WGHT 0.0302 3.4458 REM Instructions for potential hydrogen bonds HTAB C43 O10 EQIV $3 x, -y+1/2, z-1/2 HTAB C43 O11_$3 HTAB C44 O2_$3 HTAB O12 O6_$1 HTAB O13 O12_$2 REM Highest difference peak 1.115, deepest hole -0.794, 1-sigma level 0.099 Q1 1 0.2848 0.9988 0.0719 11.00000 0.05 1.10 Q2 1 0.5124 0.9697 0.1360 11.00000 0.05 0.82 Q3 1 0.3896 1.0082 0.1201 11.00000 0.05 0.50 Q4 1 0.0997 0.1352 0.1834 11.00000 0.05 0.50 Q5 1 0.2863 0.1322 0.3401 11.00000 0.05 0.50 Q6 1 0.1200 0.1352 0.3228 11.00000 0.05 0.46 Q7 1 0.2200 0.1326 0.3839 11.00000 0.05 0.46 Q8 1 0.4037 0.9704 0.0639 11.00000 0.05 0.44 Q9 1 -0.1869 0.1056 0.2463 11.00000 0.05 0.42 Q10 1 0.4095 0.1648 0.3155 11.00000 0.05 0.40 Q11 1 0.3646 0.0682 1.0982 11.00000 0.05 0.39 Q12 1 0.0806 0.1107 0.2594 11.00000 0.05 0.38 Q13 1 0.5958 0.2740 0.6418 11.00000 0.05 0.35 Q14 1 0.2273 0.1032 0.2958 11.00000 0.05 0.35 Q15 1 0.4184 0.1513 0.1622 11.00000 0.05 0.35 Q16 1 -0.2341 0.0840 0.2740 11.00000 0.05 0.34 Q17 1 0.2178 0.0378 0.2461 11.00000 0.05 0.34 Q18 1 0.2638 0.1484 0.1213 11.00000 0.05 0.34 Q19 1 0.6066 0.0534 0.5989 11.00000 0.05 0.33 Q20 1 0.2368 0.1243 0.1203 11.00000 0.05 0.33 ; _shelx_res_checksum 70724 _shelx_hkl_file ; 2 0 0 68.31 1.94 -2 0 0 70.93 1.99 -3 0 0 21.03 1.46 3 0 0 19.51 1.43 4 0 0 1.29 0.73 -4 0 0 1.12 0.77 -5 0 0 507.65 10.50 5 0 0 497.20 10.39 6 0 0 9.60 1.36 -6 0 0 11.84 1.54 -7 0 0 76.40 3.57 -8 0 0 79.13 3.87 -9 0 0 45.40 3.31 -10 0 0 91.99 4.76 -11 0 0 35.39 3.38 -12 0 0 6.24 2.08 -2 -1 0 120.54 2.90 2 -1 0 120.09 2.79 -2 1 0 117.68 2.80 2 1 0 120.15 2.87 -3 -1 0 37.39 1.73 3 -1 0 34.53 1.68 3 1 0 34.75 1.73 -3 1 0 36.29 1.72 -4 -1 0 315.73 7.08 4 -1 0 328.07 7.01 -4 1 0 319.83 6.99 4 1 0 326.59 7.06 5 -1 0 25.98 1.84 -5 -1 0 27.01 1.94 -5 1 0 27.07 1.90 -6 -1 0 52.97 2.72 6 -1 0 48.00 2.55 -6 1 0 54.39 3.25 7 -1 0 86.38 3.64 -7 -1 0 88.46 3.83 -7 1 0 88.12 3.75 -8 -1 0 1.57 1.33 -8 1 0 -0.82 1.12 -9 -1 0 169.45 6.11 -9 1 0 170.55 6.12 -10 -1 0 11.58 2.12 -10 1 0 8.37 1.92 -11 -1 0 8.42 2.01 -11 1 0 8.66 2.18 -12 -1 0 4.57 2.07 -12 1 0 3.60 1.89 2 -2 0 6.95 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28.74 3.07 -5 20 0 26.46 2.69 6 -20 0 29.00 2.68 -6 -20 0 36.46 3.36 -6 20 0 36.22 2.96 -7 -20 0 10.96 2.06 7 -20 0 17.07 2.23 -7 20 0 16.92 2.35 8 -20 0 3.97 2.50 -8 -20 0 10.44 2.15 -8 -20 0 8.69 2.10 -8 20 0 5.25 2.13 9 -20 0 1.31 1.29 -9 -20 0 -1.08 1.54 -9 -20 0 4.42 1.71 -9 20 0 -0.16 1.37 -10 -20 0 16.49 2.84 10 -20 0 11.80 2.18 -10 20 0 9.62 2.13 0 -21 0 1.20 1.36 0 21 0 0.64 1.25 -1 -21 0 67.21 3.79 1 -21 0 59.64 3.54 -1 21 0 62.14 3.45 1 21 0 60.62 3.58 -2 -21 0 86.28 4.36 2 -21 0 87.98 4.15 2 21 0 89.68 4.38 -2 21 0 82.71 3.94 -3 -21 0 33.11 3.15 3 -21 0 33.10 2.92 -3 21 0 31.45 2.77 3 21 0 35.35 3.11 4 -21 0 75.54 3.98 -4 -21 0 76.51 4.37 -4 21 0 71.13 3.81 4 21 0 76.25 4.25 5 -21 0 -1.44 1.23 -5 -21 0 2.94 1.61 -5 21 0 0.70 1.14 6 -21 0 33.21 2.89 -6 -21 0 37.12 3.36 -6 21 0 41.08 3.11 -7 -21 0 33.84 3.47 7 -21 0 36.94 2.97 -7 21 0 31.88 2.94 -8 -21 0 1.49 1.76 -8 -21 0 5.90 1.99 8 -21 0 5.54 1.66 -8 21 0 5.63 1.68 9 -21 0 54.72 3.70 -9 -21 0 59.58 4.28 -9 -21 0 48.04 7.04 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5.08 1 25 0 100.13 4.94 -2 -25 0 33.99 3.32 2 -25 0 34.61 3.24 -2 25 0 27.58 3.79 2 25 0 31.56 3.02 3 -25 0 41.59 3.43 -3 -25 0 43.02 3.71 -3 25 0 46.74 5.31 3 25 0 45.29 3.65 4 -25 0 61.94 4.84 -4 -25 0 50.21 3.90 4 25 0 52.74 3.97 -5 -25 0 -0.04 1.53 5 -25 0 0.95 1.51 -5 25 0 1.24 1.27 -6 -25 0 21.00 3.02 6 -25 0 17.49 2.63 -6 25 0 18.20 2.63 -7 -25 0 12.81 2.46 7 -25 0 9.38 2.02 -7 25 0 7.97 1.97 -8 -25 0 11.99 2.60 8 -25 0 5.05 1.91 -8 25 0 13.65 2.33 0 -26 0 110.87 5.44 0 26 0 117.66 5.40 1 -26 0 21.94 2.85 -1 -26 0 19.65 2.78 1 26 0 23.28 2.92 -1 26 0 26.07 2.72 2 -26 0 50.89 3.81 -2 -26 0 54.85 3.97 2 26 0 55.38 3.85 -2 26 0 53.61 3.68 3 -26 0 40.30 3.52 -3 -26 0 48.36 3.79 3 26 0 45.97 3.66 -3 26 0 45.31 3.34 -4 -26 0 8.13 2.14 4 -26 0 9.01 2.10 -4 26 0 5.88 1.71 4 26 0 6.31 1.90 -5 -26 0 59.45 4.34 5 -26 0 49.55 3.74 -5 26 0 49.71 3.58 6 -26 0 14.21 2.37 -6 -26 0 16.34 2.81 -6 26 0 17.20 2.46 -7 -26 0 7.88 2.18 7 -26 0 10.99 2.28 -7 26 0 10.48 2.00 8 -26 0 29.46 3.18 -8 -26 0 37.48 3.96 -8 26 0 31.67 3.31 0 -27 0 1.13 1.51 0 27 0 2.77 1.63 1 -27 0 18.83 2.69 -1 -27 0 23.74 3.06 -1 27 0 20.65 2.61 1 27 0 16.93 2.51 -2 -27 0 6.73 2.13 2 -27 0 9.84 2.25 2 27 0 4.27 1.77 -2 27 0 6.50 1.83 3 -27 0 23.54 2.95 -3 -27 0 18.86 2.79 3 27 0 20.89 2.98 -3 27 0 22.92 2.82 4 -27 0 11.37 2.14 -4 -27 0 9.38 2.36 4 27 0 8.90 2.10 -4 27 0 6.59 1.81 -5 -27 0 1.62 1.69 5 -27 0 -2.62 1.30 -5 27 0 1.48 1.36 6 -27 0 16.91 2.60 -6 -27 0 14.39 2.62 -6 27 0 17.96 2.52 7 -27 0 6.72 1.96 -7 -27 0 6.28 2.11 -7 27 0 8.73 1.94 8 -27 0 -1.48 1.46 -8 -27 0 0.95 1.73 -8 27 0 0.79 1.54 0 -28 0 -1.38 1.49 0 28 0 -0.08 1.16 1 -28 0 3.16 1.85 -1 -28 0 1.42 1.70 1 28 0 4.24 1.64 -1 28 0 3.26 1.50 -2 -28 0 4.65 1.86 2 -28 0 4.24 1.94 -2 28 0 4.62 1.73 2 28 0 8.50 2.14 3 -28 0 3.56 1.95 -3 -28 0 6.98 2.14 -3 28 0 5.85 1.70 3 28 0 8.78 2.24 4 -28 0 0.66 1.60 -4 -28 0 2.53 1.80 4 28 0 2.68 1.79 -4 28 0 3.58 1.46 -5 -28 0 6.98 2.18 5 -28 0 1.77 1.78 -5 28 0 5.10 1.67 6 -28 0 2.52 1.69 -6 -28 0 4.81 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45.52 2.62 0 7 3 41.40 2.13 0 7 -3 46.97 1.61 -1 -7 -3 93.50 3.12 1 -7 3 91.02 2.18 1 7 3 86.63 2.97 -1 7 -3 90.17 2.16 -2 -7 -3 27.10 1.78 2 -7 3 29.17 1.09 2 7 3 27.54 1.88 -2 7 -3 27.46 1.09 3 -7 3 0.88 0.45 -3 -7 -3 0.45 0.86 3 7 3 -1.09 0.79 -3 7 -3 0.54 0.48 -4 -7 -3 350.62 8.06 4 -7 3 331.96 6.77 -4 7 -3 335.49 6.86 -5 -7 -3 16.35 1.91 5 -7 3 13.57 1.81 -5 7 -3 15.10 1.48 -6 -7 -3 112.69 4.41 6 -7 3 118.48 3.62 -6 -7 -3 109.91 4.38 -6 7 -3 118.80 3.73 -7 -7 -3 53.79 3.24 -7 -7 -3 57.71 3.44 -7 7 -3 62.79 3.50 -8 -7 -3 9.90 1.84 -8 -7 -3 8.20 1.74 -8 7 -3 9.41 1.55 -9 -7 -3 69.17 4.00 -9 -7 -3 88.30 4.52 -9 7 -3 76.66 3.73 -10 -7 -3 0.79 1.19 -10 -7 -3 1.21 1.57 -10 7 -3 -0.80 1.29 -11 -7 -3 14.66 2.28 -11 -7 -3 11.83 2.44 -11 7 -3 11.51 2.41 -12 -8 3 -2.60 1.70 -12 -8 3 2.71 1.52 12 -8 -3 0.99 1.55 -12 8 3 -2.85 1.43 11 -8 -3 10.40 2.15 -11 -8 3 10.06 2.28 -11 8 3 4.18 1.90 -10 -8 3 1.40 1.52 10 -8 -3 -0.30 1.23 -10 8 3 0.72 1.58 9 -8 -3 0.70 1.20 -9 -8 3 4.75 1.78 -9 8 3 2.12 2.44 8 -8 -3 7.06 1.67 -8 -8 3 10.29 2.05 -8 8 3 8.17 1.79 7 -8 -3 5.79 1.51 -7 -8 3 6.93 1.67 -7 8 3 7.45 1.59 6 -8 -3 2.02 1.13 -6 -8 3 2.70 1.23 -6 8 3 4.07 1.38 5 -8 -3 1.33 1.07 -5 -8 3 2.30 1.09 -5 8 3 2.64 1.19 4 -8 -3 0.86 0.90 -4 -8 3 0.40 1.06 -4 8 3 0.52 0.99 -3 -8 3 32.72 1.99 3 -8 -3 32.53 2.14 -3 8 3 32.17 2.10 -2 -8 3 0.73 0.82 2 -8 -3 2.52 1.02 -2 8 3 0.93 1.03 -1 -8 3 2.06 0.77 1 -8 -3 3.49 1.07 -1 8 3 2.65 1.06 0 -8 -3 42.34 2.19 0 -8 3 40.60 1.63 0 8 -3 39.99 1.61 0 8 3 39.38 2.09 -1 -8 -3 1.14 0.92 1 -8 3 0.63 0.50 -1 8 -3 1.07 0.45 1 8 3 0.92 0.87 -2 -8 -3 1.86 0.91 2 -8 3 1.42 0.47 -2 8 -3 1.33 0.47 2 8 3 0.57 0.87 -3 -8 -3 63.12 2.78 3 -8 3 58.24 1.83 3 8 3 60.63 2.83 -3 8 -3 57.45 1.89 4 -8 3 35.45 1.57 -4 -8 -3 34.33 2.36 -4 8 -3 37.79 1.71 -5 -8 -3 14.70 1.83 5 -8 3 10.79 1.35 -5 8 -3 12.42 1.31 6 -8 3 15.86 1.50 -6 -8 -3 14.22 1.87 -6 -8 -3 15.85 2.02 -6 8 -3 15.93 1.69 -7 -8 -3 10.18 1.78 -7 -8 -3 11.20 1.91 7 -8 3 13.15 1.46 -7 8 -3 9.89 1.79 -8 -8 -3 9.65 1.91 -8 -8 -3 11.64 2.09 -8 8 -3 12.33 1.64 -9 -8 -3 2.95 1.51 -9 -8 -3 2.67 1.36 -9 8 -3 1.47 1.15 -10 -8 -3 7.64 1.77 -10 -8 -3 6.81 1.97 -10 8 -3 6.92 1.68 -11 -8 -3 2.53 1.81 -11 -8 -3 0.04 1.27 -12 -9 3 0.48 1.59 12 -9 -3 0.79 1.39 -12 9 3 -2.19 1.61 11 -9 -3 0.36 1.46 -11 -9 3 0.65 1.19 -11 -9 3 0.14 1.45 -11 9 3 0.74 1.68 10 -9 -3 2.93 1.45 -10 -9 3 0.13 1.37 -10 9 3 1.72 1.59 9 -9 -3 32.41 3.00 -9 -9 3 32.25 3.22 -9 9 3 37.06 5.08 8 -9 -3 3.97 1.50 -8 9 3 2.85 1.42 -7 -9 3 8.56 1.84 7 -9 -3 12.29 1.83 -7 9 3 8.01 1.81 -6 -9 3 -0.77 0.99 6 -9 -3 1.56 1.12 -6 9 3 0.08 1.17 -5 -9 3 4.24 1.28 5 -9 -3 2.51 1.79 -5 9 3 2.29 1.17 4 -9 -3 132.16 4.29 -4 -9 3 128.29 4.47 -4 9 3 129.75 6.17 3 -9 -3 3.60 1.16 -3 -9 3 4.37 1.10 -3 9 3 4.69 1.18 2 -9 -3 31.52 2.13 -2 -9 3 31.16 1.86 -2 9 3 24.59 1.92 1 -9 -3 2.29 1.06 -1 -9 3 3.63 0.88 -1 9 3 1.84 0.97 0 -9 3 0.18 0.59 0 -9 -3 1.82 1.00 0 9 3 0.20 0.89 0 9 -3 0.32 0.59 1 -9 3 73.77 2.17 -1 -9 -3 71.37 2.93 1 9 3 69.97 2.87 -1 9 -3 69.81 2.11 2 -9 3 48.48 1.67 -2 -9 -3 49.65 2.53 2 9 3 50.43 2.58 -2 9 -3 48.21 1.68 3 -9 3 50.29 1.79 -3 -9 -3 55.35 2.77 -3 9 -3 51.88 1.86 3 9 3 53.07 3.21 4 -9 3 1.59 0.62 -4 9 -3 1.38 0.67 5 -9 3 -0.61 0.56 -5 -9 -3 0.02 1.07 -5 9 -3 0.04 0.68 6 -9 3 32.76 1.93 -6 -9 -3 32.31 2.67 -6 9 -3 29.55 2.03 -7 -9 -3 12.08 1.96 -7 -9 -3 7.28 1.72 7 -9 3 7.39 1.23 -7 9 -3 7.67 1.64 -8 -9 -3 5.08 1.66 -8 9 -3 2.59 1.19 -9 -9 -3 0.60 1.33 -9 -9 -3 3.95 1.50 -9 9 -3 -0.08 1.17 -10 -9 -3 0.35 1.25 -10 -9 -3 -2.07 1.22 -10 9 -3 -1.27 1.13 -12 -10 3 4.33 2.36 -12 -10 3 7.25 2.48 12 -10 -3 2.94 1.76 -12 10 3 -0.25 1.64 -11 -10 3 13.49 2.57 -11 -10 3 9.87 2.18 11 -10 -3 9.13 2.04 -11 10 3 8.49 2.17 -10 -10 3 38.34 3.39 -10 -10 3 32.07 3.08 10 -10 -3 32.57 3.07 -10 10 3 35.29 3.43 9 -10 -3 -1.83 1.79 -9 -10 3 0.05 1.30 -9 -10 3 4.29 1.62 -9 10 3 2.86 1.54 -8 -10 3 78.75 4.34 8 -10 -3 76.89 3.99 -8 10 3 78.04 4.16 -7 -10 3 52.03 3.43 7 -10 -3 51.42 3.13 -7 10 3 55.05 3.44 -6 -10 3 57.76 3.30 6 -10 -3 60.90 3.20 -6 10 3 63.89 3.36 -5 -10 3 90.66 3.85 -5 -10 3 91.29 3.84 5 -10 -3 91.19 3.74 -5 10 3 89.33 3.73 -4 -10 3 13.63 1.70 4 -10 -3 13.56 1.71 -4 -10 3 13.05 1.75 -4 10 3 11.09 1.64 3 -10 -3 130.84 4.22 -3 -10 3 125.12 4.10 -3 10 3 121.80 4.12 2 -10 -3 8.06 1.36 -2 -10 3 6.21 1.13 -2 10 3 8.33 1.33 1 -10 -3 24.62 1.96 -1 -10 3 27.03 1.99 -1 10 3 24.24 1.91 1 10 -3 23.45 1.69 0 -10 -3 337.02 7.67 0 -10 3 340.96 6.90 0 10 3 319.31 7.50 0 10 -3 329.88 6.86 -1 -10 -3 5.71 1.24 1 -10 3 8.27 0.94 1 10 3 9.02 1.39 -1 10 -3 8.78 0.91 -2 -10 -3 22.75 1.99 2 -10 3 22.55 1.29 2 10 3 23.69 1.95 -2 10 -3 22.02 1.26 3 -10 3 100.50 2.75 -3 -10 -3 96.40 3.72 -3 10 -3 100.11 2.81 3 10 3 96.64 3.71 -4 -10 -3 28.75 2.22 4 -10 3 25.41 1.46 4 10 3 23.06 2.12 -4 10 -3 24.22 1.53 5 -10 3 105.47 3.20 -5 -10 -3 106.69 4.35 -5 10 -3 104.84 3.33 6 -10 3 0.72 0.80 -6 -10 -3 -0.72 1.16 -6 10 -3 -0.04 0.88 7 -10 3 74.13 3.05 -7 -10 -3 72.11 3.85 -7 -10 -3 71.18 3.94 8 -10 3 27.36 2.05 -8 -10 -3 27.24 2.80 -8 -10 -3 24.19 2.81 -8 10 -3 25.89 2.26 -9 -10 -3 0.34 1.25 -9 -10 -3 0.42 1.30 -9 10 -3 -0.91 1.09 -10 -10 -3 53.84 3.68 -10 -10 -3 44.74 3.75 -10 10 -3 41.15 3.13 -12 -11 3 26.58 4.45 12 -11 -3 22.73 3.05 -12 -11 3 24.46 3.60 -12 11 3 24.25 3.35 -11 -11 3 6.27 2.08 -11 -11 3 6.42 1.96 11 -11 -3 6.78 1.92 -11 11 3 5.47 1.99 10 -11 -3 13.28 2.28 -10 -11 3 15.26 2.42 -10 -11 3 15.14 2.53 -10 11 3 17.80 2.65 9 -11 -3 97.27 5.54 -9 -11 3 100.70 5.13 -9 -11 3 95.23 4.90 -9 11 3 104.98 4.95 -8 -11 3 4.85 1.73 -8 -11 3 1.65 1.49 8 -11 -3 1.69 1.41 -8 11 3 4.90 1.69 7 -11 -3 59.01 3.34 -7 -11 3 62.62 3.70 -7 -11 3 63.04 3.79 -7 11 3 61.77 3.68 -6 -11 3 57.41 3.33 6 -11 -3 56.97 3.16 -6 -11 3 56.75 3.30 -6 11 3 54.68 3.20 5 -11 -3 -0.04 1.00 -5 -11 3 -1.55 0.88 -5 -11 3 1.03 1.06 -5 11 3 -0.04 1.14 4 -11 -3 230.76 6.51 -4 -11 3 236.36 6.64 -4 11 3 226.08 6.34 3 -11 -3 6.47 1.38 -3 -11 3 5.61 1.23 2 -11 -3 157.34 4.73 -2 -11 3 155.32 4.51 -2 11 3 151.96 4.65 1 -11 -3 196.38 5.34 -1 -11 3 188.40 4.83 -1 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16 -0.08 1.97 9 -3 -16 0.92 1.65 9 3 -16 2.11 1.86 -9 3 16 3.41 2.32 8 -3 -16 3.93 1.78 -8 -3 16 1.21 1.86 -8 3 16 0.09 1.76 8 3 -16 0.25 1.44 7 -3 -16 8.87 2.10 -7 -3 16 7.43 2.14 -7 3 16 10.72 2.37 7 3 -16 9.75 2.09 6 -3 -16 2.69 1.43 -6 -3 16 0.34 1.48 6 3 -16 3.03 1.62 -6 3 16 0.66 1.64 5 -3 -16 28.90 3.01 -5 -3 16 27.64 2.90 -5 3 16 29.93 3.21 5 3 -16 27.19 4.31 -4 -3 16 0.77 1.21 4 -3 -16 -1.24 1.04 -4 3 16 -0.39 1.19 4 3 -16 -0.01 1.16 3 -3 -16 1.51 1.37 -3 -3 16 2.18 1.25 -3 3 16 3.51 1.42 3 3 -16 4.61 1.28 2 -3 -16 16.68 2.12 -2 -3 16 14.79 1.72 -2 3 16 22.44 2.36 -1 -3 16 -0.08 0.57 1 -3 -16 -1.00 0.98 -1 3 16 2.93 1.04 0 3 16 18.86 1.79 9 -4 -16 21.66 3.78 -9 -4 16 13.02 2.65 -9 4 16 13.61 2.88 9 4 -16 11.11 2.38 -8 -4 16 18.89 2.97 8 -4 -16 18.27 2.93 8 4 -16 18.18 2.82 -8 4 16 18.64 3.04 7 -4 -16 7.00 2.06 -7 -4 16 5.84 2.00 7 4 -16 8.57 2.01 -7 4 16 6.77 2.25 6 -4 -16 39.89 3.43 -6 -4 16 39.43 3.41 -6 4 16 39.75 3.68 6 4 -16 39.37 3.27 5 -4 -16 4.63 1.61 -5 -4 16 2.42 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21.08 2.57 -3 6 17 18.82 2.46 2 -6 -17 -3.62 1.77 -2 -6 17 1.65 0.67 -2 6 17 3.61 1.43 7 -7 -17 31.59 3.64 -7 -7 17 30.60 3.45 7 7 -17 32.75 3.24 -7 7 17 31.10 3.64 -6 -7 17 1.77 1.65 6 -7 -17 -2.18 1.40 -6 7 17 0.62 1.66 5 -7 -17 11.98 2.32 -5 -7 17 11.74 2.18 -5 7 17 11.18 2.50 -4 -7 17 4.26 1.54 4 -7 -17 3.14 1.57 -4 7 17 0.92 1.61 -3 -7 17 2.01 1.12 3 -7 -17 -0.25 1.50 -3 7 17 4.51 1.69 6 -8 -17 4.30 2.17 -6 -8 17 4.76 1.89 -6 8 17 5.48 2.06 -5 -8 17 -0.39 1.54 5 -8 -17 -1.15 1.42 -5 8 17 -1.06 1.52 4 -8 -17 -0.81 1.40 -4 -8 17 -2.62 1.05 -4 8 17 -1.34 1.38 3 -8 -17 -2.07 1.32 -3 -8 17 1.89 1.04 -3 8 17 3.25 1.56 6 -9 -17 -1.53 1.50 -6 -9 17 -0.03 1.55 -6 9 17 -1.70 1.74 5 -9 -17 2.43 1.91 -5 -9 17 3.48 2.24 -5 9 17 8.74 2.16 4 -9 -17 3.09 1.85 -4 -9 17 3.13 1.50 -4 9 17 7.76 2.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 48303 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 C1 C 0.2897(4) 0.11000(14) 0.4963(3) 0.0221(10) Uani 1 1 d . . . . . C2 C 0.4042(4) 0.10791(15) 0.5829(3) 0.0264(10) Uani 1 1 d . . . . . C3 C 0.4108(5) 0.08179(16) 0.6618(3) 0.0338(12) Uani 1 1 d . . . . . H3 H 0.4901 0.0800 0.7170 0.041 Uiso 1 1 calc R U . . . C4 C 0.3017(5) 0.05803(17) 0.6610(4) 0.0384(13) Uani 1 1 d . . . . . H4 H 0.3057 0.0406 0.7163 0.046 Uiso 1 1 calc R U . . . C5 C 0.1888(5) 0.05964(15) 0.5807(3) 0.0339(12) Uani 1 1 d . . . . . H5 H 0.1143 0.0437 0.5814 0.041 Uiso 1 1 calc R U . . . C6 C 0.1803(5) 0.08470(15) 0.4962(3) 0.0268(10) Uani 1 1 d . . . . . C7 C 0.0567(5) 0.08647(15) 0.4158(3) 0.0271(10) Uani 1 1 d . . . . . H7 H -0.0162 0.0737 0.4265 0.033 Uiso 1 1 calc R U . . . C8 C -0.0951(4) 0.10572(16) 0.2612(3) 0.0262(10) Uani 1 1 d . . . . . C9 C -0.1906(5) 0.07352(19) 0.2519(4) 0.0394(13) Uani 1 1 d . . . . . H9 H -0.1714 0.0479 0.2936 0.047 Uiso 1 1 calc R U . . . C10 C -0.3136(5) 0.0791(2) 0.1813(4) 0.0513(16) Uani 1 1 d . . . . . H10 H -0.3798 0.0575 0.1757 0.062 Uiso 1 1 calc R U . . . C11 C -0.3416(5) 0.1153(2) 0.1190(4) 0.0554(17) Uani 1 1 d . . . . . H11 H -0.4266 0.1183 0.0704 0.066 Uiso 1 1 calc R U . . . C12 C -0.2473(5) 0.14776(18) 0.1261(4) 0.0410(13) Uani 1 1 d . . . . . H12 H -0.2669 0.1726 0.0823 0.049 Uiso 1 1 calc R U . . . C13 C -0.1230(4) 0.14319(16) 0.1988(3) 0.0280(11) Uani 1 1 d . . . . . C14 C -0.0443(4) 0.21611(16) 0.1960(3) 0.0274(11) Uani 1 1 d . . . . . H14 H -0.1338 0.2245 0.1745 0.033 Uiso 1 1 calc R U . . . C15 C 0.1854(4) 0.24585(14) 0.2519(3) 0.0214(9) Uani 1 1 d . . . . . C16 C 0.0484(4) 0.25229(15) 0.2071(3) 0.0236(10) Uani 1 1 d . . . . . C17 C -0.0011(5) 0.29557(17) 0.1753(3) 0.0333(12) Uani 1 1 d . . . . . H17 H -0.0929 0.2999 0.1469 0.040 Uiso 1 1 calc R U . . . C18 C 0.0792(5) 0.33125(16) 0.1843(4) 0.0368(12) Uani 1 1 d . . . . . H18 H 0.0434 0.3602 0.1626 0.044 Uiso 1 1 calc R U . . . C19 C 0.2141(5) 0.32562(16) 0.2252(4) 0.0384(12) Uani 1 1 d . . . . . H19 H 0.2704 0.3505 0.2296 0.046 Uiso 1 1 calc R U . . . C20 C 0.2659(5) 0.28391(15) 0.2592(3) 0.0279(10) Uani 1 1 d . . . . . C21 C 0.6309(5) 0.12871(18) 0.6494(3) 0.0392(12) Uani 1 1 d . . . . . H21A H 0.6303 0.1367 0.7140 0.059 Uiso 1 1 calc R U . . . H21B H 0.6934 0.1479 0.6341 0.059 Uiso 1 1 calc R U . . . H21C H 0.6564 0.0971 0.6496 0.059 Uiso 1 1 calc R U . . . C22 C 0.4880(6) 0.30940(19) 0.3113(6) 0.074(2) Uani 1 1 d . . . . . H22A H 0.4748 0.3223 0.2469 0.111 Uiso 1 1 calc R U . . . H22B H 0.5774 0.2979 0.3408 0.111 Uiso 1 1 calc R U . . . H22C H 0.4736 0.3327 0.3536 0.111 Uiso 1 1 calc R U . . . C23 C 0.5120(4) 0.11344(14) 0.3424(3) 0.0202(9) Uani 1 1 d . . . . . C24 C 0.6325(4) 0.13612(15) 0.3872(3) 0.0211(9) Uani 1 1 d . . . . . C25 C 0.7428(4) 0.11486(16) 0.4477(3) 0.0273(10) Uani 1 1 d . . . . . H25 H 0.8220 0.1312 0.4763 0.033 Uiso 1 1 calc R U . . . C26 C 0.7382(4) 0.06847(16) 0.4675(3) 0.0302(11) Uani 1 1 d . . . . . H26 H 0.8144 0.0533 0.5090 0.036 Uiso 1 1 calc R U . . . C27 C 0.6241(4) 0.04569(16) 0.4268(3) 0.0306(11) Uani 1 1 d . . . . . H27 H 0.6218 0.0144 0.4400 0.037 Uiso 1 1 calc R U . . . C28 C 0.5086(4) 0.06717(15) 0.3653(3) 0.0230(10) Uani 1 1 d . . . . . C29 C 0.3932(4) 0.03985(15) 0.3265(3) 0.0262(10) Uani 1 1 d . . . . . H29 H 0.4056 0.0082 0.3330 0.031 Uiso 1 1 calc R U . . . C30 C 0.1713(4) 0.02150(14) 0.2494(3) 0.0257(10) Uani 1 1 d . . . . . C31 C 0.1734(5) -0.01971(16) 0.2946(4) 0.0361(12) Uani 1 1 d . . . . . H31 H 0.2471 -0.0279 0.3504 0.043 Uiso 1 1 calc R U . . . C32 C 0.0690(6) -0.04865(17) 0.2586(4) 0.0447(14) Uani 1 1 d . . . . . H32 H 0.0718 -0.0771 0.2891 0.054 Uiso 1 1 calc R U . . . C33 C -0.0399(5) -0.03677(17) 0.1786(4) 0.0448(14) Uani 1 1 d . . . . . H33 H -0.1114 -0.0570 0.1543 0.054 Uiso 1 1 calc R U . . . C34 C -0.0450(5) 0.00440(16) 0.1340(4) 0.0364(12) Uani 1 1 d . . . . . H34 H -0.1203 0.0127 0.0795 0.044 Uiso 1 1 calc R U . . . C35 C 0.0606(4) 0.03382(14) 0.1690(3) 0.0231(10) Uani 1 1 d . . . . . C36 C -0.0046(4) 0.08675(16) 0.0411(3) 0.0279(11) Uani 1 1 d . . . . . H36 H -0.0548 0.0631 0.0013 0.033 Uiso 1 1 calc R U . . . C37 C 0.0902(4) 0.16293(15) 0.0359(3) 0.0212(9) Uani 1 1 d . . . . . C38 C -0.0090(4) 0.13056(16) -0.0038(3) 0.0252(10) Uani 1 1 d . . . . . C39 C -0.1161(4) 0.14032(17) -0.0905(3) 0.0309(11) Uani 1 1 d . . . . . H39 H -0.1810 0.1180 -0.1188 0.037 Uiso 1 1 calc R U . . . C40 C -0.1270(4) 0.18142(17) -0.1337(3) 0.0319(11) Uani 1 1 d . . . . . H40 H -0.2000 0.1878 -0.1915 0.038 Uiso 1 1 calc R U . . . C41 C -0.0312(4) 0.21426(16) -0.0934(3) 0.0266(10) Uani 1 1 d . . . . . H41 H -0.0406 0.2431 -0.1233 0.032 Uiso 1 1 calc R U . . . C42 C 0.0760(4) 0.20530(15) -0.0114(3) 0.0227(10) Uani 1 1 d . . . . . C43 C 0.7451(4) 0.20529(16) 0.3938(3) 0.0318(11) Uani 1 1 d . . . . . H43A H 0.7864 0.2053 0.4654 0.048 Uiso 1 1 calc R U . . . H43B H 0.7288 0.2364 0.3701 0.048 Uiso 1 1 calc R U . . . H43C H 0.8032 0.1906 0.3658 0.048 Uiso 1 1 calc R U . . . C44 C 0.1631(5) 0.27889(15) -0.0055(3) 0.0319(11) Uani 1 1 d . . . . . H44A H 0.1570 0.2778 -0.0738 0.048 Uiso 1 1 calc R U . . . H44B H 0.2396 0.2967 0.0331 0.048 Uiso 1 1 calc R U . . . H44C H 0.0840 0.2928 -0.0023 0.048 Uiso 1 1 calc R U . . . C45 C 0.3084(6) 0.1208(3) 0.9471(5) 0.071(2) Uani 1 1 d . . . . . H45A H 0.3526 0.1496 0.9692 0.107 Uiso 1 1 calc R U . . . H45B H 0.2157 0.1261 0.9089 0.107 Uiso 1 1 calc R U . . . H45C H 0.3485 0.1053 0.9062 0.107 Uiso 1 1 calc R U . . . C46 C 0.3823(9) 0.9803(3) 0.0950(7) 0.114(3) Uani 1 1 d . U . . . H46A H 0.4641 0.9839 0.1514 0.170 Uiso 1 1 calc R U . . . H46B H 0.3737 0.9489 0.0728 0.170 Uiso 1 1 calc R U . . . H46C H 0.3084 0.9882 0.1140 0.170 Uiso 1 1 calc R U . . . Dy1 Dy 0.19446(2) 0.13300(2) 0.26030(2) 0.01723(6) Uani 1 1 d . . . . . N1 N 0.0354(3) 0.10366(12) 0.3310(3) 0.0244(8) Uani 1 1 d . . . . . N2 N -0.0189(3) 0.17399(12) 0.2120(2) 0.0241(8) Uani 1 1 d . . . . . N3 N 0.2744(3) 0.05358(11) 0.2836(2) 0.0217(8) Uani 1 1 d . . . . . N4 N 0.0631(3) 0.07790(12) 0.1314(2) 0.0214(8) Uani 1 1 d . . . . . N5 N 0.5672(4) 0.24913(13) 0.6014(3) 0.0308(9) Uani 1 1 d . . . . . Na1 Na 0.43649(16) 0.19832(6) 0.42846(12) 0.0288(4) Uani 1 1 d . . . . . Na2 Na 0.38949(18) 0.20264(6) 0.18016(13) 0.0303(4) Uani 1 1 d . . . . . O1 O 0.2898(3) 0.13587(10) 0.42519(19) 0.0224(6) Uani 1 1 d . . . . . O2 O 0.2420(3) 0.20744(9) 0.2866(2) 0.0230(7) Uani 1 1 d . . . . . O3 O 0.5041(3) 0.13512(11) 0.5777(2) 0.0326(8) Uani 1 1 d . . . . . O4 O 0.3975(3) 0.27329(11) 0.3003(3) 0.0383(9) Uani 1 1 d . . . . . O5 O 0.4116(3) 0.13588(10) 0.28374(19) 0.0207(6) Uani 1 1 d . . . . . O6 O 0.1974(3) 0.15480(10) 0.11238(19) 0.0252(7) Uani 1 1 d . . . . . O7 O 0.6246(3) 0.18146(10) 0.3651(2) 0.0252(7) Uani 1 1 d . . . . . O8 O 0.1758(3) 0.23424(10) 0.0330(2) 0.0269(7) Uani 1 1 d . . . . . O9 O 0.4481(3) 0.25445(14) 0.5569(3) 0.0497(10) Uani 1 1 d . . . . . O10 O 0.6332(3) 0.23062(12) 0.5589(3) 0.0405(9) Uani 1 1 d . . . . . O11 O 0.6171(4) 0.26228(15) 0.6864(3) 0.0593(12) Uani 1 1 d . . . . . O12 O 0.3201(5) 0.09457(19) 1.0269(4) 0.0863(16) Uani 1 1 d . . . . . H12A H 0.2832 0.1074 1.0608 0.129 Uiso 1 1 calc R U . . . O13 O 0.3835(12) 1.0090(4) 0.0176(8) 0.214(4) Uani 1 1 d . U . . . H13 H 0.3533 1.0344 0.0236 0.321 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 C1 0.033(3) 0.015(2) 0.019(2) 0.0007(17) 0.0111(19) 0.0038(19) C2 0.032(3) 0.020(2) 0.026(2) -0.0012(19) 0.008(2) 0.005(2) C3 0.046(3) 0.024(3) 0.028(3) 0.006(2) 0.009(2) 0.011(2) C4 0.053(3) 0.032(3) 0.032(3) 0.011(2) 0.018(3) 0.009(3) C5 0.049(3) 0.020(2) 0.042(3) 0.003(2) 0.028(3) 0.001(2) C6 0.034(3) 0.019(2) 0.031(2) -0.0009(19) 0.016(2) 0.002(2) C7 0.031(3) 0.020(2) 0.035(3) -0.003(2) 0.018(2) -0.004(2) C8 0.014(2) 0.036(3) 0.031(2) -0.010(2) 0.0104(19) -0.005(2) C9 0.032(3) 0.051(3) 0.041(3) -0.015(3) 0.020(2) -0.016(3) C10 0.027(3) 0.064(4) 0.063(4) -0.023(3) 0.016(3) -0.022(3) C11 0.027(3) 0.075(5) 0.052(4) -0.016(3) 0.000(3) -0.009(3) C12 0.028(3) 0.045(3) 0.043(3) -0.008(2) 0.004(2) 0.000(2) C13 0.016(2) 0.035(3) 0.030(2) -0.013(2) 0.0042(19) 0.0015(19) C14 0.023(2) 0.036(3) 0.021(2) -0.001(2) 0.0057(19) 0.010(2) C15 0.028(2) 0.021(2) 0.017(2) -0.0018(18) 0.0099(18) 0.004(2) C16 0.028(2) 0.025(2) 0.016(2) -0.0004(18) 0.0064(19) 0.008(2) C17 0.036(3) 0.039(3) 0.023(2) 0.008(2) 0.009(2) 0.014(2) C18 0.047(3) 0.023(3) 0.047(3) 0.013(2) 0.024(3) 0.018(2) C19 0.049(3) 0.020(3) 0.056(3) 0.008(2) 0.031(3) 0.006(2) C20 0.034(3) 0.016(2) 0.038(3) 0.0024(19) 0.017(2) 0.006(2) C21 0.029(3) 0.048(3) 0.030(3) 0.002(2) -0.002(2) 0.010(2) C22 0.040(4) 0.026(3) 0.160(7) 0.006(4) 0.040(4) -0.006(3) C23 0.020(2) 0.021(2) 0.020(2) 0.0027(17) 0.0081(18) 0.0044(18) C24 0.021(2) 0.024(2) 0.019(2) 0.0029(19) 0.0081(17) 0.0023(19) C25 0.020(2) 0.033(3) 0.026(2) 0.001(2) 0.0058(19) 0.003(2) C26 0.020(2) 0.038(3) 0.031(3) 0.011(2) 0.008(2) 0.011(2) C27 0.032(3) 0.028(3) 0.034(3) 0.010(2) 0.014(2) 0.009(2) C28 0.021(2) 0.024(2) 0.026(2) -0.0001(18) 0.0101(19) 0.0035(19) C29 0.030(3) 0.018(2) 0.030(2) 0.0045(19) 0.011(2) 0.004(2) C30 0.033(3) 0.019(2) 0.030(2) -0.0032(19) 0.018(2) -0.004(2) C31 0.036(3) 0.027(3) 0.045(3) 0.006(2) 0.014(2) -0.004(2) C32 0.056(4) 0.020(3) 0.062(4) 0.007(2) 0.025(3) -0.010(2) C33 0.045(3) 0.027(3) 0.059(4) -0.003(3) 0.013(3) -0.020(2) C34 0.035(3) 0.028(3) 0.041(3) -0.005(2) 0.007(2) -0.011(2) C35 0.025(2) 0.019(2) 0.027(2) -0.0032(18) 0.0111(19) -0.0035(19) C36 0.027(2) 0.030(3) 0.022(2) -0.0065(19) 0.003(2) -0.007(2) C37 0.019(2) 0.028(2) 0.016(2) -0.0020(18) 0.0068(18) 0.0001(18) C38 0.027(2) 0.027(2) 0.019(2) -0.004(2) 0.0049(18) -0.002(2) C39 0.026(2) 0.039(3) 0.022(2) -0.004(2) 0.0017(19) -0.003(2) C40 0.025(3) 0.042(3) 0.022(2) -0.001(2) 0.001(2) 0.002(2) C41 0.033(3) 0.026(3) 0.024(2) 0.0056(19) 0.014(2) 0.008(2) C42 0.020(2) 0.029(3) 0.018(2) 0.0000(18) 0.0061(18) 0.0019(19) C43 0.022(2) 0.034(3) 0.034(3) -0.001(2) 0.004(2) -0.011(2) C44 0.042(3) 0.022(3) 0.033(3) 0.004(2) 0.016(2) 0.001(2) C45 0.053(4) 0.105(6) 0.055(4) -0.009(4) 0.018(3) -0.023(4) C46 0.117(4) 0.113(4) 0.110(4) 0.008(2) 0.041(2) -0.006(2) Dy1 0.01617(10) 0.01585(10) 0.01781(10) -0.00056(9) 0.00400(7) -0.00075(9) N1 0.0214(19) 0.024(2) 0.029(2) -0.0062(17) 0.0106(16) -0.0052(16) N2 0.0203(19) 0.027(2) 0.0220(19) -0.0031(16) 0.0042(16) 0.0024(16) N3 0.026(2) 0.0164(19) 0.0257(19) -0.0003(15) 0.0126(16) 0.0003(15) N4 0.022(2) 0.0188(19) 0.024(2) -0.0013(15) 0.0100(16) -0.0005(15) N5 0.031(2) 0.029(2) 0.033(2) -0.0078(18) 0.0125(19) -0.0067(18) Na1 0.0219(9) 0.0312(10) 0.0286(9) -0.0073(8) 0.0037(8) -0.0023(8) Na2 0.0330(10) 0.0289(10) 0.0321(10) 0.0029(8) 0.0156(8) -0.0021(8) O1 0.0250(16) 0.0227(16) 0.0177(14) -0.0008(13) 0.0056(12) -0.0038(14) O2 0.0207(16) 0.0169(16) 0.0261(16) 0.0023(12) 0.0023(13) 0.0016(12) O3 0.0262(17) 0.0358(19) 0.0255(16) 0.0036(15) -0.0027(13) -0.0029(16) O4 0.0305(19) 0.0208(18) 0.064(2) 0.0040(16) 0.0180(17) -0.0027(15) O5 0.0151(14) 0.0233(16) 0.0224(14) 0.0038(13) 0.0052(12) 0.0022(13) O6 0.0226(16) 0.0301(17) 0.0169(15) 0.0039(13) 0.0003(13) -0.0051(14) O7 0.0192(16) 0.0227(17) 0.0304(17) 0.0021(13) 0.0051(13) -0.0034(13) O8 0.0292(17) 0.0252(17) 0.0265(16) 0.0047(13) 0.0103(14) -0.0039(14) O9 0.024(2) 0.069(3) 0.053(2) -0.019(2) 0.0094(17) 0.0085(18) O10 0.0262(19) 0.048(2) 0.051(2) -0.0166(18) 0.0172(17) -0.0017(16) O11 0.060(3) 0.084(3) 0.030(2) -0.024(2) 0.0118(19) -0.019(2) O12 0.070(4) 0.108(5) 0.090(4) -0.012(3) 0.040(3) 0.022(3) O13 0.213(5) 0.211(5) 0.212(5) -0.006(4) 0.072(4) 0.003(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 C1 C6 124.3(4) . . ? O1 C1 C2 118.8(4) . . ? C6 C1 C2 116.8(4) . . ? C3 C2 O3 125.2(4) . . ? C3 C2 C1 122.2(4) . . ? O3 C2 C1 112.6(4) . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.4(4) . . ? C1 C6 C7 121.9(4) . . ? C5 C6 C7 118.4(4) . . ? N1 C7 C6 126.3(4) . . ? N1 C7 H7 116.8 . . ? C6 C7 H7 116.8 . . ? C9 C8 C13 120.3(4) . . ? C9 C8 N1 124.5(5) . . ? C13 C8 N1 115.2(4) . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.9(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 118.9(5) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C8 119.7(4) . . ? C12 C13 N2 123.7(4) . . ? C8 C13 N2 116.6(4) . . ? N2 C14 C16 127.2(4) . . ? N2 C14 H14 116.4 . . ? C16 C14 H14 116.4 . . ? O2 C15 C20 118.1(4) . . ? O2 C15 C16 124.8(4) . . ? C20 C15 C16 117.1(4) . . ? O2 C15 Na2 57.9(2) . . ? C20 C15 Na2 81.1(3) . . ? C16 C15 Na2 132.8(3) . . ? C17 C16 C15 119.6(4) . . ? C17 C16 C14 118.0(4) . . ? C15 C16 C14 122.4(4) . . ? C18 C17 C16 121.5(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 119.9(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 O4 126.1(4) . . ? C19 C20 C15 121.8(4) . . ? O4 C20 C15 112.1(4) . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 119.0(4) . . ? O5 C23 C28 124.1(4) . . ? C24 C23 C28 116.9(4) . . ? O5 C23 Na1 64.0(2) . . ? C24 C23 Na1 76.5(2) . . ? C28 C23 Na1 131.6(3) . . ? C25 C24 O7 124.6(4) . . ? C25 C24 C23 122.6(4) . . ? O7 C24 C23 112.8(3) . . ? C25 C24 Na1 132.1(3) . . ? O7 C24 Na1 57.9(2) . . ? C23 C24 Na1 76.8(2) . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 119.5(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 121.8(4) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C27 C28 C23 119.5(4) . . ? C27 C28 C29 117.1(4) . . ? C23 C28 C29 123.3(4) . . ? N3 C29 C28 127.2(4) . . ? N3 C29 H29 116.4 . . ? C28 C29 H29 116.4 . . ? C31 C30 C35 119.4(4) . . ? C31 C30 N3 123.3(4) . . ? C35 C30 N3 117.2(4) . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.6(5) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.1(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C30 119.9(4) . . ? C34 C35 N4 124.4(4) . . ? C30 C35 N4 115.7(4) . . ? N4 C36 C38 124.1(4) . . ? N4 C36 H36 117.9 . . ? C38 C36 H36 117.9 . . ? O6 C37 C38 122.8(4) . . ? O6 C37 C42 118.9(4) . . ? C38 C37 C42 118.3(4) . . ? C37 C38 C39 119.8(4) . . ? C37 C38 C36 122.1(4) . . ? C39 C38 C36 118.1(4) . . ? C40 C39 C38 120.4(4) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.6(4) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? O8 C42 C41 125.7(4) . . ? O8 C42 C37 113.7(3) . . ? C41 C42 C37 120.6(4) . . ? O7 C43 H43A 109.5 . . ? O7 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O7 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O8 C44 H44A 109.5 . . ? O8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O12 C45 H45A 109.5 . . ? O12 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O12 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O13 C46 H46A 109.5 . . ? O13 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O13 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O1 Dy1 O2 78.08(10) . . ? O1 Dy1 O6 147.92(10) . . ? O2 Dy1 O6 78.62(11) . . ? O1 Dy1 O5 77.71(10) . . ? O2 Dy1 O5 77.02(10) . . ? O6 Dy1 O5 75.79(10) . . ? O1 Dy1 N1 71.90(11) . . ? O2 Dy1 N1 114.95(11) . . ? O6 Dy1 N1 138.81(11) . . ? O5 Dy1 N1 143.43(11) . . ? O1 Dy1 N3 83.49(11) . . ? O2 Dy1 N3 148.03(11) . . ? O6 Dy1 N3 105.80(11) . . ? O5 Dy1 N3 73.66(11) . . ? N1 Dy1 N3 83.02(12) . . ? O1 Dy1 N2 107.74(11) . . ? O2 Dy1 N2 73.05(11) . . ? O6 Dy1 N2 86.01(11) . . ? O5 Dy1 N2 147.47(11) . . ? N1 Dy1 N2 63.94(12) . . ? N3 Dy1 N2 138.12(12) . . ? O1 Dy1 N4 137.99(11) . . ? O2 Dy1 N4 142.45(10) . . ? O6 Dy1 N4 70.91(11) . . ? O5 Dy1 N4 114.71(11) . . ? N1 Dy1 N4 77.80(11) . . ? N3 Dy1 N4 64.27(11) . . ? N2 Dy1 N4 83.26(11) . . ? C7 N1 C8 119.4(4) . . ? C7 N1 Dy1 129.3(3) . . ? C8 N1 Dy1 111.1(3) . . ? C14 N2 C13 119.5(4) . . ? C14 N2 Dy1 130.0(3) . . ? C13 N2 Dy1 110.5(3) . . ? C29 N3 C30 119.6(4) . . ? C29 N3 Dy1 127.5(3) . . ? C30 N3 Dy1 112.8(3) . . ? C36 N4 C35 120.1(4) . . ? C36 N4 Dy1 126.7(3) . . ? C35 N4 Dy1 113.1(2) . . ? O11 N5 O9 119.2(4) . . ? O11 N5 O10 121.6(4) . . ? O9 N5 O10 119.2(4) . . ? O11 N5 Na1 164.9(3) . . ? O9 N5 Na1 60.4(2) . . ? O10 N5 Na1 61.1(2) . . ? O11 N5 Na2 64.3(3) . 4_566 ? O9 N5 Na2 55.1(2) . 4_566 ? O10 N5 Na2 173.3(3) . 4_566 ? Na1 N5 Na2 114.33(14) . 4_566 ? O2 Na1 O1 72.27(10) . . ? O2 Na1 O9 111.45(13) . . ? O1 Na1 O9 111.98(13) . . ? O2 Na1 O10 150.64(14) . . ? O1 Na1 O10 133.35(13) . . ? O9 Na1 O10 51.02(11) . . ? O2 Na1 O7 106.56(11) . . ? O1 Na1 O7 116.79(12) . . ? O9 Na1 O7 124.87(13) . . ? O10 Na1 O7 76.65(11) . . ? O2 Na1 O5 66.45(10) . . ? O1 Na1 O5 66.16(10) . . ? O9 Na1 O5 177.41(12) . . ? O10 Na1 O5 131.55(12) . . ? O7 Na1 O5 57.63(9) . . ? O2 Na1 O3 131.32(12) . . ? O1 Na1 O3 59.11(10) . . ? O9 Na1 O3 86.02(13) . . ? O10 Na1 O3 75.39(11) . . ? O7 Na1 O3 97.65(11) . . ? O5 Na1 O3 94.33(10) . . ? O2 Na1 O4 57.69(10) . . ? O1 Na1 O4 129.90(11) . . ? O9 Na1 O4 85.97(13) . . ? O10 Na1 O4 94.87(12) . . ? O7 Na1 O4 82.07(11) . . ? O5 Na1 O4 93.94(11) . . ? O3 Na1 O4 169.98(12) . . ? O2 Na1 N5 135.59(13) . . ? O1 Na1 N5 122.21(12) . . ? O9 Na1 N5 25.77(11) . . ? O10 Na1 N5 25.88(11) . . ? O7 Na1 N5 102.22(12) . . ? O5 Na1 N5 156.69(12) . . ? O3 Na1 N5 75.68(11) . . ? O4 Na1 N5 94.56(12) . . ? O2 Na1 C24 111.47(12) . . ? O1 Na1 C24 92.61(12) . . ? O9 Na1 C24 135.25(13) . . ? O10 Na1 C24 84.73(12) . . ? O7 Na1 C24 26.65(10) . . ? O5 Na1 C24 47.22(10) . . ? O3 Na1 C24 75.11(11) . . ? O4 Na1 C24 106.74(12) . . ? N5 Na1 C24 109.48(12) . . ? O2 Na1 C23 91.45(11) . . ? O1 Na1 C23 69.18(11) . . ? O9 Na1 C23 156.55(13) . . ? O10 Na1 C23 110.02(13) . . ? O7 Na1 C23 47.62(11) . . ? O5 Na1 C23 25.24(9) . . ? O3 Na1 C23 74.57(11) . . ? O4 Na1 C23 111.67(12) . . ? N5 Na1 C23 132.68(13) . . ? C24 Na1 C23 26.71(11) . . ? O6 Na2 O5 69.92(10) . . ? O6 Na2 O9 114.78(12) . 4_565 ? O5 Na2 O9 150.71(14) . 4_565 ? O6 Na2 O2 69.14(10) . . ? O5 Na2 O2 67.65(10) . . ? O9 Na2 O2 141.64(14) 4_565 . ? O6 Na2 O11 154.13(14) . 4_565 ? O5 Na2 O11 114.37(12) . 4_565 ? O9 Na2 O11 48.54(11) 4_565 4_565 ? O2 Na2 O11 136.70(13) . 4_565 ? O6 Na2 O8 60.48(10) . . ? O5 Na2 O8 129.28(11) . . ? O9 Na2 O8 67.80(11) 4_565 . ? O2 Na2 O8 84.92(10) . . ? O11 Na2 O8 114.77(12) 4_565 . ? O6 Na2 O4 122.17(12) . . ? O5 Na2 O4 104.42(11) . . ? O9 Na2 O4 96.93(14) 4_565 . ? O2 Na2 O4 57.01(10) . . ? O11 Na2 O4 82.49(13) 4_565 . ? O8 Na2 O4 93.59(11) . . ? O6 Na2 N5 135.77(12) . 4_565 ? O5 Na2 N5 134.31(12) . 4_565 ? O9 Na2 N5 24.20(10) 4_565 4_565 ? O2 Na2 N5 146.92(12) . 4_565 ? O11 Na2 N5 24.38(10) 4_565 4_565 ? O8 Na2 N5 91.43(11) . 4_565 ? O4 Na2 N5 90.57(12) . 4_565 ? O6 Na2 C15 75.62(12) . . ? O5 Na2 C15 92.54(11) . . ? O9 Na2 C15 116.75(14) 4_565 . ? O2 Na2 C15 24.91(10) . . ? O11 Na2 C15 127.80(14) 4_565 . ? O8 Na2 C15 66.50(11) . . ? O4 Na2 C15 46.66(11) . . ? N5 Na2 C15 126.52(12) 4_565 . ? C1 O1 Dy1 134.7(3) . . ? C1 O1 Na1 128.9(3) . . ? Dy1 O1 Na1 95.40(11) . . ? C15 O2 Dy1 137.2(3) . . ? C15 O2 Na1 125.7(3) . . ? Dy1 O2 Na1 96.57(11) . . ? C15 O2 Na2 97.1(3) . . ? Dy1 O2 Na2 89.98(11) . . ? Na1 O2 Na2 87.78(11) . . ? C2 O3 C21 117.6(4) . . ? C2 O3 Na1 116.7(2) . . ? C21 O3 Na1 125.7(3) . . ? C20 O4 C22 116.8(4) . . ? C20 O4 Na2 96.4(3) . . ? C22 O4 Na2 120.5(4) . . ? C20 O4 Na1 110.3(3) . . ? C22 O4 Na1 125.6(4) . . ? Na2 O4 Na1 77.65(10) . . ? C23 O5 Dy1 131.6(3) . . ? C23 O5 Na2 133.4(3) . . ? Dy1 O5 Na2 94.34(10) . . ? C23 O5 Na1 90.8(2) . . ? Dy1 O5 Na1 86.87(10) . . ? Na2 O5 Na1 83.87(10) . . ? C37 O6 Dy1 122.9(3) . . ? C37 O6 Na2 127.8(3) . . ? Dy1 O6 Na2 95.11(10) . . ? C24 O7 C43 116.3(3) . . ? C24 O7 Na1 95.4(2) . . ? C43 O7 Na1 125.0(3) . . ? C42 O8 C44 116.9(3) . . ? C42 O8 Na2 118.4(3) . . ? C44 O8 Na2 124.6(3) . . ? N5 O9 Na2 100.7(3) . 4_566 ? N5 O9 Na1 93.8(3) . . ? Na2 O9 Na1 160.42(18) 4_566 . ? N5 O10 Na1 93.1(3) . . ? N5 O11 Na2 91.4(3) . 4_566 ? C45 O12 H12A 109.5 . . ? C46 O13 H13 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 C1 O1 1.296(5) . ? C1 C6 1.418(6) . ? C1 C2 1.427(6) . ? C2 C3 1.373(6) . ? C2 O3 1.388(6) . ? C3 C4 1.388(7) . ? C3 H3 0.9500 . ? C4 C5 1.365(7) . ? C4 H4 0.9500 . ? C5 C6 1.420(6) . ? C5 H5 0.9500 . ? C6 C7 1.438(6) . ? C7 N1 1.285(6) . ? C7 H7 0.9500 . ? C8 C9 1.390(6) . ? C8 C13 1.403(7) . ? C8 N1 1.427(5) . ? C9 C10 1.381(7) . ? C9 H9 0.9500 . ? C10 C11 1.372(8) . ? C10 H10 0.9500 . ? C11 C12 1.392(8) . ? C11 H11 0.9500 . ? C12 C13 1.399(6) . ? C12 H12 0.9500 . ? C13 N2 1.422(6) . ? C14 N2 1.284(6) . ? C14 C16 1.449(6) . ? C14 H14 0.9500 . ? C15 O2 1.310(5) . ? C15 C20 1.415(6) . ? C15 C16 1.419(6) . ? C15 Na2 3.085(5) . ? C16 C17 1.407(6) . ? C17 C18 1.355(7) . ? C17 H17 0.9500 . ? C18 C19 1.392(7) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C19 H19 0.9500 . ? C20 O4 1.386(6) . ? C21 O3 1.420(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O4 1.431(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O5 1.308(5) . ? C23 C24 1.416(6) . ? C23 C28 1.419(6) . ? C23 Na1 3.067(5) . ? C24 C25 1.368(6) . ? C24 O7 1.380(5) . ? C24 Na1 3.063(5) . ? C25 C26 1.413(7) . ? C25 H25 0.9500 . ? C26 C27 1.357(6) . ? C26 H26 0.9500 . ? C27 C28 1.413(6) . ? C27 H27 0.9500 . ? C28 C29 1.437(6) . ? C29 N3 1.291(5) . ? C29 H29 0.9500 . ? C30 C31 1.388(6) . ? C30 C35 1.399(6) . ? C30 N3 1.425(5) . ? C31 C32 1.376(7) . ? C31 H31 0.9500 . ? C32 C33 1.382(7) . ? C32 H32 0.9500 . ? C33 C34 1.378(7) . ? C33 H33 0.9500 . ? C34 C35 1.393(6) . ? C34 H34 0.9500 . ? C35 N4 1.425(5) . ? C36 N4 1.288(5) . ? C36 C38 1.451(6) . ? C36 H36 0.9500 . ? C37 O6 1.320(5) . ? C37 C38 1.410(6) . ? C37 C42 1.417(6) . ? C38 C39 1.412(6) . ? C39 C40 1.360(7) . ? C39 H39 0.9500 . ? C40 C41 1.398(6) . ? C40 H40 0.9500 . ? C41 C42 1.368(6) . ? C41 H41 0.9500 . ? C42 O8 1.359(5) . ? C43 O7 1.424(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 O8 1.429(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 O12 1.372(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 O13 1.426(11) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? Dy1 O1 2.260(3) . ? Dy1 O2 2.272(3) . ? Dy1 O6 2.277(3) . ? Dy1 O5 2.286(3) . ? Dy1 N1 2.495(4) . ? Dy1 N3 2.497(3) . ? Dy1 N2 2.505(4) . ? Dy1 N4 2.519(3) . ? N5 O11 1.229(5) . ? N5 O9 1.241(5) . ? N5 O10 1.246(5) . ? N5 Na1 2.850(4) . ? N5 Na2 2.976(4) 4_566 ? Na1 O2 2.393(3) . ? Na1 O1 2.447(3) . ? Na1 O9 2.484(4) . ? Na1 O10 2.497(4) . ? Na1 O7 2.607(4) . ? Na1 O5 2.757(3) . ? Na1 O3 2.772(4) . ? Na1 O4 2.844(4) . ? Na2 O6 2.436(3) . ? Na2 O5 2.456(3) . ? Na2 O9 2.483(4) 4_565 ? Na2 O2 2.635(4) . ? Na2 O11 2.681(5) 4_565 ? Na2 O8 2.712(3) . ? Na2 O4 2.721(4) . ? Na2 N5 2.976(4) 4_565 ? O9 Na2 2.483(4) 4_566 ? O11 Na2 2.682(5) 4_566 ? O12 H12A 0.8400 . ? O13 H13 0.8400 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O12 0.84 1.83 2.651(12) 165.5 1_564 O12 H12A O6 0.84 1.99 2.799(6) 160.8 1_556 C43 H43A O10 0.98 2.64 3.182(6) 115.1 .