#------------------------------------------------------------------------------ #$Date: 2018-01-25 05:48:15 +0200 (Thu, 25 Jan 2018) $ #$Revision: 205623 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045403.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_7045403 loop_ _publ_author_name 'Akhtar, Muhammad Nadeem' 'Lan, Yanhua' 'AlDamen, Murad A.' 'Zheng, Yan-Zhen' 'Anson, Christopher' 'Powell, Annie K.' _publ_section_title ; Effect of Ligand Substitution on the SMM Properties of Three Isostructural Families of Double-Cubane Mn4Ln2 ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT04304J _journal_year 2018 _chemical_formula_moiety 'C62 H74 Dy2 Mn4 N6 O28, 2(C2 H3 N)' _chemical_formula_sum 'C66 H80 Dy2 Mn4 N8 O28' _chemical_formula_weight 1978.14 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2018-01-10 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-01-12 deposited with the CCDC. 2018-01-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.213(1) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.9182(4) _cell_length_b 15.1094(4) _cell_length_c 18.6730(6) _cell_measurement_reflns_used 15326 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.14 _cell_measurement_theta_min 2.21 _cell_volume 3597.70(19) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0218 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 23771 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.146 _diffrn_reflns_theta_min 1.743 _diffrn_source 'rotating anode' _exptl_absorpt_coefficient_mu 2.822 _exptl_absorpt_correction_T_max 0.747 _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0493 before and 0.0201 after correction. The Ratio of minimum to maximum transmission is 0.8036. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.826 _exptl_crystal_description block _exptl_crystal_F_000 1976 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.670 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.097 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 494 _refine_ls_number_reflns 8163 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0249 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+4.8763P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.0606 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7330 _reflns_number_total 8163 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04304j2.cif _cod_data_source_block 16-mn4dy2 _cod_database_code 7045403 _shelx_shelxl_version_number 2017/1 _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 0.747 _shelx_estimated_absorpt_t_min 0.539 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All O(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O5-H5 = O3-H3 0.88 with sigma of 0.04 3.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B) 3.b Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31) 3.c Idealised Me refined as rotating group: C42(H42A,H42B,H42C) ; _shelx_res_file ; TITL p400rep in P2(1)/n p400rep.res created by SHELXL-2017/1 at 15:55:22 on 10-Jan-2018 CELL 0.71073 12.9182 15.1094 18.673 90 99.213 90 ZERR 2 0.0004 0.0004 0.0006 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Dy Mn N O UNIT 132 160 4 8 16 56 EQIV $1 1-X,1-Y,1-Z DFIX 0.88 0.04 O5 H5 O3 H3 L.S. 16 PLAN 20 SIZE 0.25 0.19 0.11 TEMP -173 HTAB O3 O11 HTAB O5 O11 RTAB M..M Mn1 Mn1_$1 RTAB M..M Mn1 Mn2 RTAB M..M Mn1 Mn2_$1 RTAB M..M Mn1 Dy1 RTAB M..M Mn1 Dy1_$1 RTAB M..M Mn2 Dy1 RTAB M..M Mn2 Dy1_$1 CONN 6 Mn1 CONN 7 Mn2 CONN 9 Dy1 BOND $H fmap 2 acta OMIT -1 1 1 OMIT -1 0 1 REM REM REM WGHT 0.029100 4.876300 FVAR 0.21667 DY1 3 0.400559 0.661168 0.425208 11.00000 0.01729 0.01515 = 0.01279 0.00126 0.00269 0.00314 MN1 4 0.541136 0.474339 0.435269 11.00000 0.01504 0.01524 = 0.01111 -0.00039 0.00196 0.00236 MN2 4 0.330448 0.380586 0.465138 11.00000 0.01638 0.01654 = 0.01461 0.00021 0.00200 0.00021 O1 6 0.411460 0.516005 0.464655 11.00000 0.01712 0.01569 = 0.01299 0.00093 0.00136 0.00080 N1 5 0.293965 0.256410 0.392325 11.00000 0.02220 0.01911 = 0.01761 0.00019 0.00125 -0.00179 C1 1 0.210965 0.204677 0.419598 11.00000 0.02825 0.01969 = 0.02543 -0.00163 0.00157 -0.00542 AFIX 23 H1A 2 0.208900 0.144335 0.398755 11.00000 -1.20000 H1B 2 0.142192 0.232892 0.402817 11.00000 -1.20000 AFIX 0 C2 1 0.227955 0.197976 0.501565 11.00000 0.02797 0.01789 = 0.02585 0.00159 0.00494 -0.00439 AFIX 23 H2A 2 0.168696 0.165330 0.516807 11.00000 -1.20000 H2B 2 0.292954 0.164097 0.518209 11.00000 -1.20000 AFIX 0 N2 5 0.236409 0.286791 0.536328 11.00000 0.02021 0.02034 = 0.01931 0.00147 0.00195 -0.00107 C3 1 0.395831 0.209733 0.399618 11.00000 0.02691 0.01852 = 0.02065 -0.00274 0.00110 0.00307 AFIX 23 H3A 2 0.394558 0.167207 0.359152 11.00000 -1.20000 H3B 2 0.407335 0.175960 0.445640 11.00000 -1.20000 AFIX 0 C4 1 0.485219 0.274853 0.398872 11.00000 0.02318 0.02183 = 0.01689 -0.00463 0.00317 0.00219 AFIX 23 H4A 2 0.552608 0.242336 0.405414 11.00000 -1.20000 H4B 2 0.476700 0.305128 0.351271 11.00000 -1.20000 AFIX 0 O2 6 0.487590 0.339259 0.455194 11.00000 0.01958 0.01729 = 0.01341 -0.00307 0.00174 0.00283 C5 1 0.255456 0.280605 0.315115 11.00000 0.02600 0.02515 = 0.01656 -0.00268 -0.00025 -0.00251 AFIX 23 H5A 2 0.208649 0.233466 0.291647 11.00000 -1.20000 H5B 2 0.315644 0.286106 0.288589 11.00000 -1.20000 AFIX 0 C6 1 0.196926 0.366659 0.311680 11.00000 0.02154 0.02663 = 0.02203 0.00419 -0.00446 -0.00520 AFIX 23 H6A 2 0.173462 0.384642 0.260683 11.00000 -1.20000 H6B 2 0.134803 0.361589 0.336332 11.00000 -1.20000 AFIX 0 O3 6 0.270431 0.429469 0.348261 11.00000 0.02191 0.01831 = 0.02166 -0.00128 -0.00213 -0.00048 H3 2 0.242745 0.480182 0.348468 11.00000 -1.20000 C7 1 0.298016 0.281863 0.610609 11.00000 0.02026 0.02376 = 0.01812 0.00446 0.00313 -0.00077 AFIX 23 H7A 2 0.347104 0.231226 0.613151 11.00000 -1.20000 H7B 2 0.249648 0.270878 0.645759 11.00000 -1.20000 AFIX 0 C8 1 0.359931 0.365820 0.632079 11.00000 0.01891 0.02302 = 0.01514 0.00171 0.00373 0.00102 AFIX 23 H8A 2 0.311232 0.414784 0.638314 11.00000 -1.20000 H8B 2 0.406860 0.356596 0.678848 11.00000 -1.20000 AFIX 0 O4 6 0.420494 0.388434 0.577359 11.00000 0.01841 0.01874 = 0.01370 0.00069 0.00420 -0.00002 C9 1 0.129902 0.324261 0.536413 11.00000 0.01898 0.02753 = 0.02312 0.00405 0.00246 -0.00159 AFIX 23 H9A 2 0.103762 0.304574 0.580830 11.00000 -1.20000 H9B 2 0.081722 0.300774 0.494101 11.00000 -1.20000 AFIX 0 C10 1 0.128294 0.423981 0.533487 11.00000 0.02053 0.02690 = 0.02615 0.00245 0.00642 0.00127 AFIX 23 H10A 2 0.055296 0.446203 0.527013 11.00000 -1.20000 H10B 2 0.167456 0.449148 0.578824 11.00000 -1.20000 AFIX 0 O5 6 0.177273 0.447936 0.472699 11.00000 0.02485 0.02244 = 0.02584 0.00652 0.00701 0.00302 H5 2 0.171740 0.499156 0.463816 11.00000 -1.20000 O6 6 0.493338 0.468171 0.330712 11.00000 0.02211 0.01914 = 0.01292 0.00084 0.00189 0.00246 O7 6 0.391717 0.589268 0.311804 11.00000 0.02027 0.01864 = 0.01578 0.00089 0.00216 0.00190 C11 1 0.432246 0.521056 0.290978 11.00000 0.01511 0.01940 = 0.01611 0.00107 0.00290 -0.00355 C12 1 0.411413 0.497304 0.211992 11.00000 0.02910 0.01206 = 0.01418 0.00195 0.00055 -0.00106 C13 1 0.494649 0.481201 0.175080 11.00000 0.03099 0.02270 = 0.01922 -0.00044 0.00343 -0.00222 AFIX 43 H13 2 0.564785 0.484888 0.199746 11.00000 -1.20000 AFIX 0 C14 1 0.474595 0.459562 0.101500 11.00000 0.04440 0.02726 = 0.02079 -0.00063 0.01152 0.00191 AFIX 43 H14 2 0.531201 0.451113 0.075408 11.00000 -1.20000 AFIX 0 C15 1 0.372442 0.450416 0.066560 11.00000 0.05350 0.02346 = 0.01572 -0.00170 0.00038 -0.00499 AFIX 43 H15 2 0.359108 0.434902 0.016629 11.00000 -1.20000 AFIX 0 C16 1 0.289835 0.463681 0.103766 11.00000 0.04092 0.02727 = 0.02123 0.00332 -0.00669 -0.00891 AFIX 43 H16 2 0.219881 0.455172 0.079927 11.00000 -1.20000 AFIX 0 C17 1 0.308748 0.489504 0.176153 11.00000 0.02928 0.02518 = 0.02061 0.00282 0.00265 -0.00287 AFIX 43 H17 2 0.251760 0.501784 0.201067 11.00000 -1.20000 AFIX 0 O8 6 0.677279 0.427731 0.411360 11.00000 0.02054 0.01925 = 0.01883 0.00114 0.00514 0.00286 O9 6 0.703904 0.310601 0.485877 11.00000 0.02169 0.02374 = 0.01767 0.00358 0.00637 0.00582 C18 1 0.722228 0.355072 0.432786 11.00000 0.01701 0.02114 = 0.01469 -0.00382 0.00209 -0.00246 C19 1 0.802502 0.319940 0.390584 11.00000 0.01611 0.02010 = 0.01714 -0.00427 0.00139 -0.00298 C20 1 0.820610 0.361406 0.326813 11.00000 0.02135 0.02269 = 0.02020 -0.00098 0.00397 -0.00321 AFIX 43 H20 2 0.783206 0.413600 0.310330 11.00000 -1.20000 AFIX 0 C21 1 0.893648 0.325897 0.287597 11.00000 0.02487 0.03424 = 0.01679 -0.00408 0.00553 -0.00566 AFIX 43 H21 2 0.907293 0.354395 0.244726 11.00000 -1.20000 AFIX 0 C22 1 0.946243 0.249086 0.311201 11.00000 0.01648 0.03567 = 0.02610 -0.01201 0.00628 -0.00291 AFIX 43 H22 2 0.995366 0.224507 0.283970 11.00000 -1.20000 AFIX 0 C23 1 0.928186 0.207493 0.374111 11.00000 0.02043 0.02443 = 0.03016 -0.00416 0.00205 0.00320 AFIX 43 H23 2 0.964671 0.154577 0.389739 11.00000 -1.20000 AFIX 0 C24 1 0.856503 0.243240 0.414509 11.00000 0.01833 0.02249 = 0.02136 -0.00148 0.00401 -0.00104 AFIX 43 H24 2 0.844658 0.215366 0.458077 11.00000 -1.20000 AFIX 0 O10 6 0.243050 0.729779 0.360415 11.00000 0.01938 0.02006 = 0.02013 0.00373 0.00159 0.00224 O11 6 0.218579 0.591370 0.391092 11.00000 0.02418 0.01779 = 0.02104 0.00395 0.00062 0.00285 C25 1 0.184427 0.663972 0.360586 11.00000 0.02104 0.01961 = 0.01629 -0.00052 0.00560 0.00428 C26 1 0.072662 0.668857 0.323631 11.00000 0.01947 0.02232 = 0.01718 0.00217 0.00522 0.00170 C27 1 0.028870 0.750566 0.301923 11.00000 0.02049 0.02145 = 0.01929 0.00222 0.00388 0.00262 AFIX 43 H27 2 0.069432 0.802913 0.311612 11.00000 -1.20000 AFIX 0 C28 1 -0.073996 0.756052 0.266101 11.00000 0.02533 0.02835 = 0.02089 0.00536 0.00375 0.00690 AFIX 43 H28 2 -0.103881 0.812076 0.251983 11.00000 -1.20000 AFIX 0 C29 1 -0.132796 0.679622 0.251050 11.00000 0.01730 0.04087 = 0.02147 0.00391 -0.00064 0.00201 AFIX 43 H29 2 -0.202456 0.683156 0.225524 11.00000 -1.20000 AFIX 0 C30 1 -0.089950 0.597727 0.273273 11.00000 0.02798 0.03003 = 0.02638 -0.00044 0.00060 -0.00784 AFIX 43 H30 2 -0.130600 0.545453 0.263420 11.00000 -1.20000 AFIX 0 C31 1 0.012548 0.592461 0.309960 11.00000 0.02720 0.02213 = 0.02601 0.00142 0.00222 0.00258 AFIX 43 H31 2 0.041501 0.536633 0.325686 11.00000 -1.20000 AFIX 0 N3 5 0.451126 0.838167 0.383342 11.00000 0.02028 0.02216 = 0.02511 0.00255 0.00158 0.00003 O12 6 0.455147 0.773063 0.341377 11.00000 0.02538 0.01975 = 0.02217 0.00146 0.00685 0.00145 O13 6 0.436584 0.820582 0.447687 11.00000 0.03495 0.02246 = 0.01772 0.00079 0.00207 0.00224 O14 6 0.460964 0.914471 0.363114 11.00000 0.04308 0.02088 = 0.04114 0.00758 0.00507 -0.00603 N41 5 0.243981 0.037743 0.640107 11.00000 0.04576 0.05466 = 0.04508 0.00396 0.00741 0.00884 C41 1 0.300109 -0.003861 0.612567 11.00000 0.03569 0.03561 = 0.03041 0.00557 -0.00057 0.00056 C42 1 0.372429 -0.056574 0.578449 11.00000 0.04168 0.03680 = 0.03571 -0.00540 -0.00371 0.00331 AFIX 137 H42A 2 0.400516 -0.020606 0.542324 11.00000 -1.50000 H42B 2 0.335475 -0.107933 0.554594 11.00000 -1.50000 H42C 2 0.430160 -0.076800 0.615376 11.00000 -1.50000 AFIX 0 HKLF 4 REM p400rep in P2(1)/n REM R1 = 0.0249 for 7330 Fo > 4sig(Fo) and 0.0295 for all 8163 data REM 494 parameters refined using 2 restraints END WGHT 0.0291 4.8660 REM Highest difference peak 1.670, deepest hole -0.507, 1-sigma level 0.097 Q1 1 0.3548 0.6435 0.3969 11.00000 0.05 1.67 Q2 1 0.4389 0.6658 0.3962 11.00000 0.05 1.01 Q3 1 0.3583 0.6539 0.4537 11.00000 0.05 0.89 Q4 1 0.4538 0.6703 0.4644 11.00000 0.05 0.78 Q5 1 0.5569 0.5166 0.4149 11.00000 0.05 0.71 Q6 1 0.2817 0.5980 0.3820 11.00000 0.05 0.69 Q7 1 0.5189 0.3411 0.4861 11.00000 0.05 0.45 Q8 1 0.2064 0.3308 0.2717 11.00000 0.05 0.45 Q9 1 0.3601 0.4044 0.5045 11.00000 0.05 0.43 Q10 1 0.7729 0.3454 0.4113 11.00000 0.05 0.42 Q11 1 0.2042 0.6189 0.3789 11.00000 0.05 0.42 Q12 1 0.5818 0.4648 0.4118 11.00000 0.05 0.41 Q13 1 0.2427 0.2077 0.4620 11.00000 0.05 0.41 Q14 1 0.5406 0.9194 0.3899 11.00000 0.05 0.40 Q15 1 0.0984 0.5194 0.0770 11.00000 0.05 0.40 Q16 1 0.4252 0.5166 0.2481 11.00000 0.05 0.40 Q17 1 0.4243 0.4403 0.0948 11.00000 0.05 0.40 Q18 1 0.2193 0.6988 0.3476 11.00000 0.05 0.39 Q19 1 0.8022 0.3348 0.3585 11.00000 0.05 0.39 Q20 1 0.4542 0.4745 0.2007 11.00000 0.05 0.39 ; _shelx_res_checksum 29678 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Dy1 Dy 0.40056(2) 0.66117(2) 0.42521(2) 0.01505(4) Uani 1 1 d . Mn1 Mn 0.54114(3) 0.47434(2) 0.43527(2) 0.01381(8) Uani 1 1 d . Mn2 Mn 0.33045(3) 0.38059(3) 0.46514(2) 0.01590(8) Uani 1 1 d . O1 O 0.41146(13) 0.51601(11) 0.46466(9) 0.0154(3) Uani 1 1 d . N1 N 0.29397(17) 0.25641(15) 0.39232(11) 0.0199(4) Uani 1 1 d . C1 C 0.2110(2) 0.20468(19) 0.41960(15) 0.0248(6) Uani 1 1 d . H1A H 0.208900 0.144335 0.398755 0.030 Uiso 1 1 calc R H1B H 0.142192 0.232892 0.402817 0.030 Uiso 1 1 calc R C2 C 0.2280(2) 0.19798(18) 0.50157(15) 0.0238(6) Uani 1 1 d . H2A H 0.168696 0.165330 0.516807 0.029 Uiso 1 1 calc R H2B H 0.292954 0.164097 0.518209 0.029 Uiso 1 1 calc R N2 N 0.23641(17) 0.28679(15) 0.53633(11) 0.0201(4) Uani 1 1 d . C3 C 0.3958(2) 0.20973(18) 0.39962(14) 0.0223(5) Uani 1 1 d . H3A H 0.394558 0.167207 0.359152 0.027 Uiso 1 1 calc R H3B H 0.407335 0.175960 0.445640 0.027 Uiso 1 1 calc R C4 C 0.4852(2) 0.27485(18) 0.39887(14) 0.0206(5) Uani 1 1 d . H4A H 0.552608 0.242336 0.405414 0.025 Uiso 1 1 calc R H4B H 0.476700 0.305128 0.351271 0.025 Uiso 1 1 calc R O2 O 0.48759(14) 0.33926(11) 0.45519(9) 0.0169(4) Uani 1 1 d . C5 C 0.2555(2) 0.28061(18) 0.31511(14) 0.0230(6) Uani 1 1 d . H5A H 0.208649 0.233466 0.291647 0.028 Uiso 1 1 calc R H5B H 0.315644 0.286106 0.288589 0.028 Uiso 1 1 calc R C6 C 0.1969(2) 0.36666(19) 0.31168(15) 0.0243(6) Uani 1 1 d . H6A H 0.173462 0.384642 0.260683 0.029 Uiso 1 1 calc R H6B H 0.134803 0.361589 0.336332 0.029 Uiso 1 1 calc R O3 O 0.27043(15) 0.42947(13) 0.34826(10) 0.0212(4) Uani 1 1 d D H3 H 0.243(2) 0.4802(19) 0.3485(17) 0.025 Uiso 1 1 d DR C7 C 0.2980(2) 0.28186(18) 0.61061(14) 0.0207(5) Uani 1 1 d . H7A H 0.347104 0.231226 0.613151 0.025 Uiso 1 1 calc R H7B H 0.249648 0.270878 0.645759 0.025 Uiso 1 1 calc R C8 C 0.3599(2) 0.36582(18) 0.63208(13) 0.0189(5) Uani 1 1 d . H8A H 0.311232 0.414784 0.638314 0.023 Uiso 1 1 calc R H8B H 0.406860 0.356596 0.678848 0.023 Uiso 1 1 calc R O4 O 0.42049(14) 0.38843(12) 0.57736(9) 0.0168(3) Uani 1 1 d . C9 C 0.1299(2) 0.32426(19) 0.53641(15) 0.0233(6) Uani 1 1 d . H9A H 0.103762 0.304574 0.580830 0.028 Uiso 1 1 calc R H9B H 0.081722 0.300774 0.494101 0.028 Uiso 1 1 calc R C10 C 0.1283(2) 0.42398(19) 0.53349(15) 0.0242(6) Uani 1 1 d . H10A H 0.055296 0.446203 0.527013 0.029 Uiso 1 1 calc R H10B H 0.167456 0.449148 0.578824 0.029 Uiso 1 1 calc R O5 O 0.17727(16) 0.44794(14) 0.47270(11) 0.0241(4) Uani 1 1 d D H5 H 0.172(3) 0.4992(18) 0.4638(18) 0.029 Uiso 1 1 d DR O6 O 0.49334(14) 0.46817(12) 0.33071(9) 0.0182(4) Uani 1 1 d . O7 O 0.39172(14) 0.58927(12) 0.31180(9) 0.0183(4) Uani 1 1 d . C11 C 0.43225(19) 0.52106(17) 0.29098(13) 0.0168(5) Uani 1 1 d . C12 C 0.4114(2) 0.49730(16) 0.21199(13) 0.0188(5) Uani 1 1 d . C13 C 0.4946(2) 0.48120(19) 0.17508(14) 0.0244(6) Uani 1 1 d . H13 H 0.564785 0.484888 0.199746 0.029 Uiso 1 1 calc R C14 C 0.4746(3) 0.4596(2) 0.10150(15) 0.0301(7) Uani 1 1 d . H14 H 0.531201 0.451113 0.075408 0.036 Uiso 1 1 calc R C15 C 0.3724(3) 0.4504(2) 0.06656(15) 0.0315(7) Uani 1 1 d . H15 H 0.359108 0.434902 0.016629 0.038 Uiso 1 1 calc R C16 C 0.2898(3) 0.4637(2) 0.10377(15) 0.0311(7) Uani 1 1 d . H16 H 0.219881 0.455172 0.079927 0.037 Uiso 1 1 calc R C17 C 0.3087(2) 0.48950(19) 0.17615(14) 0.0252(6) Uani 1 1 d . H17 H 0.251760 0.501784 0.201067 0.030 Uiso 1 1 calc R O8 O 0.67728(14) 0.42773(12) 0.41136(9) 0.0193(4) Uani 1 1 d . O9 O 0.70390(14) 0.31060(13) 0.48588(9) 0.0207(4) Uani 1 1 d . C18 C 0.7222(2) 0.35507(17) 0.43279(13) 0.0177(5) Uani 1 1 d . C19 C 0.8025(2) 0.31994(17) 0.39058(13) 0.0179(5) Uani 1 1 d . C20 C 0.8206(2) 0.36141(19) 0.32681(14) 0.0213(5) Uani 1 1 d . H20 H 0.783206 0.413600 0.310330 0.026 Uiso 1 1 calc R C21 C 0.8936(2) 0.3259(2) 0.28760(14) 0.0251(6) Uani 1 1 d . H21 H 0.907293 0.354395 0.244726 0.030 Uiso 1 1 calc R C22 C 0.9462(2) 0.2491(2) 0.31120(15) 0.0258(6) Uani 1 1 d . H22 H 0.995366 0.224507 0.283970 0.031 Uiso 1 1 calc R C23 C 0.9282(2) 0.20749(19) 0.37411(15) 0.0252(6) Uani 1 1 d . H23 H 0.964671 0.154577 0.389739 0.030 Uiso 1 1 calc R C24 C 0.8565(2) 0.24324(18) 0.41451(14) 0.0206(5) Uani 1 1 d . H24 H 0.844658 0.215366 0.458077 0.025 Uiso 1 1 calc R O10 O 0.24305(14) 0.72978(12) 0.36042(10) 0.0200(4) Uani 1 1 d . O11 O 0.21858(15) 0.59137(12) 0.39109(10) 0.0213(4) Uani 1 1 d . C25 C 0.1844(2) 0.66397(17) 0.36059(13) 0.0187(5) Uani 1 1 d . C26 C 0.0727(2) 0.66886(17) 0.32363(14) 0.0194(5) Uani 1 1 d . C27 C 0.0289(2) 0.75057(18) 0.30192(14) 0.0203(5) Uani 1 1 d . H27 H 0.069432 0.802913 0.311612 0.024 Uiso 1 1 calc R C28 C -0.0740(2) 0.7561(2) 0.26610(14) 0.0249(6) Uani 1 1 d . H28 H -0.103881 0.812076 0.251983 0.030 Uiso 1 1 calc R C29 C -0.1328(2) 0.6796(2) 0.25105(15) 0.0270(6) Uani 1 1 d . H29 H -0.202456 0.683156 0.225524 0.032 Uiso 1 1 calc R C30 C -0.0899(2) 0.5977(2) 0.27327(15) 0.0285(6) Uani 1 1 d . H30 H -0.130600 0.545453 0.263420 0.034 Uiso 1 1 calc R C31 C 0.0125(2) 0.59246(19) 0.30996(15) 0.0253(6) Uani 1 1 d . H31 H 0.041501 0.536633 0.325686 0.030 Uiso 1 1 calc R N3 N 0.45113(18) 0.83817(15) 0.38334(13) 0.0227(5) Uani 1 1 d . O12 O 0.45515(15) 0.77306(12) 0.34138(10) 0.0221(4) Uani 1 1 d . O13 O 0.43658(16) 0.82058(13) 0.44769(10) 0.0253(4) Uani 1 1 d . O14 O 0.46096(18) 0.91447(14) 0.36311(12) 0.0352(5) Uani 1 1 d . N41 N 0.2440(3) 0.0377(2) 0.64011(17) 0.0485(8) Uani 1 1 d . C41 C 0.3001(3) -0.0039(2) 0.61257(17) 0.0345(7) Uani 1 1 d . C42 C 0.3724(3) -0.0566(2) 0.57845(18) 0.0391(8) Uani 1 1 d . H42A H 0.400516 -0.020606 0.542324 0.059 Uiso 1 1 calc GR H42B H 0.335475 -0.107933 0.554594 0.059 Uiso 1 1 calc GR H42C H 0.430160 -0.076800 0.615376 0.059 Uiso 1 1 calc GR 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 Dy1 0.01729(7) 0.01515(6) 0.01279(6) 0.00126(4) 0.00269(4) 0.00314(4) Mn1 0.01504(18) 0.01524(18) 0.01111(16) -0.00039(13) 0.00196(13) 0.00236(14) Mn2 0.01638(18) 0.01654(19) 0.01461(17) 0.00021(14) 0.00200(14) 0.00021(15) O1 0.0171(8) 0.0157(8) 0.0130(8) 0.0009(6) 0.0014(7) 0.0008(7) N1 0.0222(11) 0.0191(11) 0.0176(10) 0.0002(8) 0.0013(9) -0.0018(9) C1 0.0283(15) 0.0197(14) 0.0254(13) -0.0016(11) 0.0016(11) -0.0054(11) C2 0.0280(14) 0.0179(13) 0.0258(13) 0.0016(10) 0.0049(11) -0.0044(11) N2 0.0202(11) 0.0203(11) 0.0193(10) 0.0015(8) 0.0019(9) -0.0011(9) C3 0.0269(14) 0.0185(13) 0.0207(12) -0.0027(10) 0.0011(11) 0.0031(11) C4 0.0232(13) 0.0218(13) 0.0169(11) -0.0046(10) 0.0032(10) 0.0022(11) O2 0.0196(9) 0.0173(9) 0.0134(8) -0.0031(6) 0.0017(7) 0.0028(7) C5 0.0260(14) 0.0251(14) 0.0166(12) -0.0027(10) -0.0002(10) -0.0025(11) C6 0.0215(13) 0.0266(14) 0.0220(13) 0.0042(11) -0.0045(11) -0.0052(11) O3 0.0219(10) 0.0183(9) 0.0217(9) -0.0013(7) -0.0021(7) -0.0005(8) C7 0.0203(13) 0.0238(14) 0.0181(12) 0.0045(10) 0.0031(10) -0.0008(11) C8 0.0189(12) 0.0230(13) 0.0151(11) 0.0017(10) 0.0037(10) 0.0010(10) O4 0.0184(9) 0.0187(9) 0.0137(8) 0.0007(7) 0.0042(7) 0.0000(7) C9 0.0190(13) 0.0275(15) 0.0231(13) 0.0041(11) 0.0025(10) -0.0016(11) C10 0.0205(13) 0.0269(15) 0.0261(13) 0.0025(11) 0.0064(11) 0.0013(11) O5 0.0248(10) 0.0224(10) 0.0258(10) 0.0065(8) 0.0070(8) 0.0030(8) O6 0.0221(9) 0.0191(9) 0.0129(8) 0.0008(7) 0.0019(7) 0.0025(7) O7 0.0203(9) 0.0186(9) 0.0158(8) 0.0009(7) 0.0022(7) 0.0019(7) C11 0.0151(12) 0.0194(12) 0.0161(11) 0.0011(9) 0.0029(9) -0.0035(10) C12 0.0291(14) 0.0121(11) 0.0142(11) 0.0020(9) 0.0006(10) -0.0011(10) C13 0.0310(15) 0.0227(14) 0.0192(12) -0.0004(10) 0.0034(11) -0.0022(12) C14 0.0444(18) 0.0273(15) 0.0208(13) -0.0006(11) 0.0115(13) 0.0019(13) C15 0.054(2) 0.0235(15) 0.0157(12) -0.0017(11) 0.0004(13) -0.0050(14) C16 0.0409(18) 0.0273(15) 0.0212(13) 0.0033(11) -0.0067(12) -0.0089(13) C17 0.0293(15) 0.0252(14) 0.0206(13) 0.0028(11) 0.0027(11) -0.0029(12) O8 0.0205(9) 0.0193(9) 0.0188(8) 0.0011(7) 0.0051(7) 0.0029(7) O9 0.0217(9) 0.0237(10) 0.0177(8) 0.0036(7) 0.0064(7) 0.0058(8) C18 0.0170(12) 0.0211(13) 0.0147(11) -0.0038(9) 0.0021(9) -0.0025(10) C19 0.0161(12) 0.0201(13) 0.0171(11) -0.0043(9) 0.0014(10) -0.0030(10) C20 0.0213(13) 0.0227(13) 0.0202(12) -0.0010(10) 0.0040(10) -0.0032(11) C21 0.0249(14) 0.0342(16) 0.0168(12) -0.0041(11) 0.0055(11) -0.0057(12) C22 0.0165(13) 0.0357(16) 0.0261(13) -0.0120(12) 0.0063(11) -0.0029(11) C23 0.0204(13) 0.0244(14) 0.0302(14) -0.0042(11) 0.0021(11) 0.0032(11) C24 0.0183(12) 0.0225(13) 0.0214(12) -0.0015(10) 0.0040(10) -0.0010(10) O10 0.0194(9) 0.0201(9) 0.0201(9) 0.0037(7) 0.0016(7) 0.0022(7) O11 0.0242(10) 0.0178(9) 0.0210(9) 0.0039(7) 0.0006(7) 0.0028(8) C25 0.0210(13) 0.0196(13) 0.0163(11) -0.0005(9) 0.0056(10) 0.0043(10) C26 0.0195(13) 0.0223(13) 0.0172(11) 0.0022(10) 0.0052(10) 0.0017(10) C27 0.0205(13) 0.0215(13) 0.0193(12) 0.0022(10) 0.0039(10) 0.0026(10) C28 0.0253(14) 0.0284(15) 0.0209(13) 0.0054(11) 0.0038(11) 0.0069(12) C29 0.0173(13) 0.0409(17) 0.0215(13) 0.0039(12) -0.0006(11) 0.0020(12) C30 0.0280(15) 0.0300(16) 0.0264(14) -0.0004(12) 0.0006(12) -0.0078(12) C31 0.0272(15) 0.0221(14) 0.0260(13) 0.0014(11) 0.0022(11) 0.0026(11) N3 0.0203(11) 0.0222(12) 0.0251(11) 0.0025(9) 0.0016(9) 0.0000(9) O12 0.0254(10) 0.0197(9) 0.0222(9) 0.0015(7) 0.0068(8) 0.0014(8) O13 0.0350(11) 0.0225(10) 0.0177(9) 0.0008(7) 0.0021(8) 0.0022(8) O14 0.0431(13) 0.0209(11) 0.0411(12) 0.0076(9) 0.0051(10) -0.0060(9) N41 0.0458(18) 0.055(2) 0.0451(17) 0.0040(15) 0.0074(15) 0.0088(16) C41 0.0357(17) 0.0356(18) 0.0304(15) 0.0056(13) -0.0006(13) 0.0006(14) C42 0.0417(19) 0.0368(18) 0.0357(17) -0.0054(14) -0.0037(15) 0.0033(15) 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' 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 Dy1 O2 73.20(6) . 3_666 O1 Dy1 O4 72.84(6) . 3_666 O1 Dy1 O7 80.87(6) . . O1 Dy1 O9 87.68(6) . 3_666 O1 Dy1 O10 124.59(6) . . O1 Dy1 O11 72.26(6) . . O1 Dy1 O12 147.00(6) . . O1 Dy1 O13 150.34(6) . . O2 Dy1 O11 127.39(6) 3_666 . O2 Dy1 O12 112.94(6) 3_666 . O2 Dy1 O13 77.37(6) 3_666 . O4 Dy1 O2 66.15(6) 3_666 3_666 O4 Dy1 O11 134.73(6) 3_666 . O4 Dy1 O12 80.27(6) 3_666 . O4 Dy1 O13 98.58(6) 3_666 . O7 Dy1 O2 138.50(6) . 3_666 O7 Dy1 O4 75.60(6) . 3_666 O7 Dy1 O10 80.42(6) . . O7 Dy1 O11 71.19(6) . . O7 Dy1 O12 74.11(6) . . O7 Dy1 O13 125.38(6) . . O9 Dy1 O2 71.20(6) 3_666 3_666 O9 Dy1 O4 136.57(6) 3_666 3_666 O9 Dy1 O7 140.16(7) 3_666 . O9 Dy1 O10 75.12(6) 3_666 . O9 Dy1 O11 68.97(6) 3_666 . O9 Dy1 O12 125.29(6) 3_666 . O9 Dy1 O13 79.43(7) 3_666 . O10 Dy1 O2 141.08(6) . 3_666 O10 Dy1 O4 147.50(6) . 3_666 O10 Dy1 O11 52.36(6) . . O10 Dy1 O12 72.23(6) . . O10 Dy1 O13 77.81(6) . . O12 Dy1 O11 117.75(6) . . O13 Dy1 O11 125.63(6) . . O13 Dy1 O12 51.66(6) . . O1 Mn1 O1 81.53(8) 3_666 . O1 Mn1 O2 86.82(7) . . O1 Mn1 O2 88.00(7) 3_666 . O1 Mn1 O4 89.43(7) 3_666 3_666 O1 Mn1 O4 86.74(7) . 3_666 O1 Mn1 O6 178.16(8) 3_666 . O1 Mn1 O6 98.54(7) . . O1 Mn1 O8 95.21(7) 3_666 . O1 Mn1 O8 176.28(7) . . O4 Mn1 O2 173.35(7) 3_666 . O6 Mn1 O2 93.84(7) . . O6 Mn1 O4 88.74(7) . 3_666 O6 Mn1 O8 84.78(7) . . O8 Mn1 O2 91.29(7) . . O8 Mn1 O4 95.05(7) . 3_666 O1 Mn2 N1 140.10(7) . . O1 Mn2 N2 142.97(7) . . O1 Mn2 O3 78.26(6) . . N1 Mn2 N2 76.94(8) . . O2 Mn2 O1 79.76(6) . . O2 Mn2 N1 79.71(7) . . O2 Mn2 N2 116.27(7) . . O2 Mn2 O3 100.87(7) . . O2 Mn2 O4 74.95(6) . . O2 Mn2 O5 169.86(7) . . O3 Mn2 N1 72.54(7) . . O3 Mn2 N2 125.93(7) . . O4 Mn2 O1 77.71(6) . . O4 Mn2 N1 128.29(7) . . O4 Mn2 N2 75.25(7) . . O4 Mn2 O3 155.97(7) . . O4 Mn2 O5 104.39(7) . . O5 Mn2 O1 90.18(7) . . O5 Mn2 N1 107.72(8) . . O5 Mn2 N2 72.80(7) . . O5 Mn2 O3 75.51(7) . . Mn1 O1 Dy1 103.72(8) 3_666 . Mn1 O1 Dy1 103.19(7) . . Mn1 O1 Mn1 98.47(8) 3_666 . Mn1 O1 Mn2 97.24(7) . . Mn1 O1 Mn2 98.13(7) 3_666 . Mn2 O1 Dy1 147.30(8) . . C1 N1 Mn2 108.39(16) . . C1 N1 C5 108.3(2) . . C3 N1 Mn2 103.72(15) . . C3 N1 C1 113.5(2) . . C3 N1 C5 111.1(2) . . C5 N1 Mn2 111.88(16) . . N1 C1 H1A 109.0 . . N1 C1 H1B 109.0 . . N1 C1 C2 112.8(2) . . H1A C1 H1B 107.8 . . C2 C1 H1A 109.0 . . C2 C1 H1B 109.0 . . C1 C2 H2A 109.3 . . C1 C2 H2B 109.3 . . H2A C2 H2B 107.9 . . N2 C2 C1 111.7(2) . . N2 C2 H2A 109.3 . . N2 C2 H2B 109.3 . . C2 N2 Mn2 107.41(15) . . C2 N2 C9 109.9(2) . . C7 N2 Mn2 107.66(15) . . C7 N2 C2 110.7(2) . . C7 N2 C9 112.0(2) . . C9 N2 Mn2 109.01(15) . . N1 C3 H3A 109.5 . . N1 C3 H3B 109.5 . . N1 C3 C4 110.9(2) . . H3A C3 H3B 108.0 . . C4 C3 H3A 109.5 . . C4 C3 H3B 109.5 . . C3 C4 H4A 109.4 . . C3 C4 H4B 109.4 . . H4A C4 H4B 108.0 . . O2 C4 C3 111.2(2) . . O2 C4 H4A 109.4 . . O2 C4 H4B 109.4 . . Mn1 O2 Dy1 90.06(6) . 3_666 Mn2 O2 Dy1 110.27(7) . 3_666 Mn2 O2 Mn1 94.10(7) . . C4 O2 Dy1 127.36(15) . 3_666 C4 O2 Mn1 118.43(15) . . C4 O2 Mn2 110.50(15) . . N1 C5 H5A 109.7 . . N1 C5 H5B 109.7 . . N1 C5 C6 109.9(2) . . H5A C5 H5B 108.2 . . C6 C5 H5A 109.7 . . C6 C5 H5B 109.7 . . C5 C6 H6A 110.7 . . C5 C6 H6B 110.7 . . H6A C6 H6B 108.8 . . O3 C6 C5 105.2(2) . . O3 C6 H6A 110.7 . . O3 C6 H6B 110.7 . . Mn2 O3 H3 111(2) . . C6 O3 Mn2 109.48(15) . . C6 O3 H3 111(2) . . N2 C7 H7A 109.1 . . N2 C7 H7B 109.1 . . N2 C7 C8 112.7(2) . . H7A C7 H7B 107.8 . . C8 C7 H7A 109.1 . . C8 C7 H7B 109.1 . . C7 C8 H8A 109.7 . . C7 C8 H8B 109.7 . . H8A C8 H8B 108.2 . . O4 C8 C7 109.7(2) . . O4 C8 H8A 109.7 . . O4 C8 H8B 109.7 . . Mn1 O4 Dy1 93.34(6) 3_666 3_666 Mn1 O4 Mn2 92.46(7) 3_666 . Mn2 O4 Dy1 108.58(7) . 3_666 C8 O4 Dy1 124.88(14) . 3_666 C8 O4 Mn1 118.16(15) . 3_666 C8 O4 Mn2 113.41(14) . . N2 C9 H9A 109.0 . . N2 C9 H9B 109.0 . . N2 C9 C10 112.8(2) . . H9A C9 H9B 107.8 . . C10 C9 H9A 109.0 . . C10 C9 H9B 109.0 . . C9 C10 H10A 110.5 . . C9 C10 H10B 110.5 . . H10A C10 H10B 108.7 . . O5 C10 C9 106.0(2) . . O5 C10 H10A 110.5 . . O5 C10 H10B 110.5 . . Mn2 O5 H5 119(3) . . C10 O5 Mn2 116.12(16) . . C10 O5 H5 112(2) . . C11 O6 Mn1 128.25(16) . . C11 O7 Dy1 134.14(16) . . O6 C11 C12 114.8(2) . . O7 C11 O6 126.1(2) . . O7 C11 C12 119.1(2) . . C13 C12 C11 119.9(2) . . C13 C12 C17 120.0(2) . . C17 C12 C11 120.0(2) . . C12 C13 H13 120.2 . . C12 C13 C14 119.6(3) . . C14 C13 H13 120.2 . . C13 C14 H14 120.0 . . C15 C14 C13 120.1(3) . . C15 C14 H14 120.0 . . C14 C15 H15 119.8 . . C16 C15 C14 120.4(3) . . C16 C15 H15 119.8 . . C15 C16 H16 120.0 . . C15 C16 C17 120.1(3) . . C17 C16 H16 120.0 . . C12 C17 H17 120.1 . . C16 C17 C12 119.8(3) . . C16 C17 H17 120.1 . . C18 O8 Mn1 127.03(16) . . C18 O9 Dy1 131.91(17) . 3_666 O8 C18 C19 117.3(2) . . O9 C18 O8 125.2(2) . . O9 C18 C19 117.5(2) . . C20 C19 C18 120.9(2) . . C24 C19 C18 118.8(2) . . C24 C19 C20 120.3(2) . . C19 C20 H20 120.1 . . C21 C20 C19 119.7(3) . . C21 C20 H20 120.1 . . C20 C21 H21 120.1 . . C22 C21 C20 119.8(3) . . C22 C21 H21 120.1 . . C21 C22 H22 119.6 . . C21 C22 C23 120.7(3) . . C23 C22 H22 119.6 . . C22 C23 H23 120.0 . . C22 C23 C24 120.0(3) . . C24 C23 H23 120.0 . . C19 C24 C23 119.5(3) . . C19 C24 H24 120.3 . . C23 C24 H24 120.3 . . C25 O10 Dy1 96.83(15) . . C25 O11 Dy1 89.72(15) . . O10 C25 Dy1 57.44(13) . . O10 C25 O11 121.1(2) . . O10 C25 C26 119.9(2) . . O11 C25 Dy1 63.66(14) . . O11 C25 C26 119.0(2) . . C26 C25 Dy1 176.86(18) . . C27 C26 C25 119.6(2) . . C27 C26 C31 119.6(3) . . C31 C26 C25 120.8(2) . . C26 C27 H27 119.8 . . C26 C27 C28 120.4(3) . . C28 C27 H27 119.8 . . C27 C28 H28 120.1 . . C29 C28 C27 119.9(3) . . C29 C28 H28 120.1 . . C28 C29 H29 119.9 . . C28 C29 C30 120.1(3) . . C30 C29 H29 119.9 . . C29 C30 H30 120.0 . . C29 C30 C31 119.9(3) . . C31 C30 H30 120.0 . . C26 C31 C30 120.1(3) . . C26 C31 H31 119.9 . . C30 C31 H31 119.9 . . O12 N3 Dy1 58.74(12) . . O12 N3 O13 116.7(2) . . O13 N3 Dy1 58.53(13) . . O14 N3 Dy1 172.95(19) . . O14 N3 O12 121.6(2) . . O14 N3 O13 121.7(2) . . N3 O12 Dy1 95.46(14) . . N3 O13 Dy1 95.46(15) . . N41 C41 C42 179.2(4) . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42B 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O1 2.3108(17) . Dy1 O2 2.4580(17) 3_666 Dy1 O4 2.4379(17) 3_666 Dy1 O7 2.3664(17) . Dy1 O9 2.3404(17) 3_666 Dy1 O10 2.4270(18) . Dy1 O11 2.5622(19) . Dy1 O12 2.4818(18) . Dy1 O13 2.476(2) . Mn1 O1 1.8766(16) 3_666 Mn1 O1 1.9488(17) . Mn1 O2 2.2057(18) . Mn1 O4 2.1536(18) 3_666 Mn1 O6 1.9534(17) . Mn1 O8 2.0099(18) . Mn2 O1 2.2989(18) . Mn2 N1 2.321(2) . Mn2 N2 2.402(2) . Mn2 O2 2.1601(18) . Mn2 O3 2.3169(19) . Mn2 O4 2.2311(17) . Mn2 O5 2.250(2) . N1 C1 1.482(3) . N1 C3 1.480(3) . N1 C5 1.493(3) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.514(4) . C2 H2A 0.9900 . C2 H2B 0.9900 . C2 N2 1.487(3) . N2 C7 1.486(3) . N2 C9 1.488(3) . C3 H3A 0.9900 . C3 H3B 0.9900 . C3 C4 1.519(4) . C4 H4A 0.9900 . C4 H4B 0.9900 . C4 O2 1.430(3) . C5 H5A 0.9900 . C5 H5B 0.9900 . C5 C6 1.500(4) . C6 H6A 0.9900 . C6 H6B 0.9900 . C6 O3 1.436(3) . O3 H3 0.85(3) . C7 H7A 0.9900 . C7 H7B 0.9900 . C7 C8 1.519(4) . C8 H8A 0.9900 . C8 H8B 0.9900 . C8 O4 1.424(3) . C9 H9A 0.9900 . C9 H9B 0.9900 . C9 C10 1.508(4) . C10 H10A 0.9900 . C10 H10B 0.9900 . C10 O5 1.432(3) . O5 H5 0.79(3) . O6 C11 1.274(3) . O7 C11 1.246(3) . C11 C12 1.500(3) . C12 C13 1.388(4) . C12 C17 1.392(4) . C13 H13 0.9500 . C13 C14 1.396(4) . C14 H14 0.9500 . C14 C15 1.382(5) . C15 H15 0.9500 . C15 C16 1.378(5) . C16 H16 0.9500 . C16 C17 1.390(4) . C17 H17 0.9500 . O8 C18 1.276(3) . O9 C18 1.251(3) . C18 C19 1.497(3) . C19 C20 1.398(4) . C19 C24 1.389(4) . C20 H20 0.9500 . C20 C21 1.391(4) . C21 H21 0.9500 . C21 C22 1.381(4) . C22 H22 0.9500 . C22 C23 1.385(4) . C23 H23 0.9500 . C23 C24 1.394(4) . C24 H24 0.9500 . O10 C25 1.250(3) . O11 C25 1.281(3) . C25 C26 1.499(4) . C26 C27 1.391(4) . C26 C31 1.392(4) . C27 H27 0.9500 . C27 C28 1.391(4) . C28 H28 0.9500 . C28 C29 1.386(4) . C29 H29 0.9500 . C29 C30 1.391(4) . C30 H30 0.9500 . C30 C31 1.392(4) . C31 H31 0.9500 . N3 O12 1.264(3) . N3 O13 1.274(3) . N3 O14 1.226(3) . N41 C41 1.142(5) . C41 C42 1.450(5) . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . 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_publ_flag O3 H3 O11 0.85(3) 1.91(3) 2.691(3) 154(3) yes O5 H5 O11 0.79(3) 2.10(3) 2.750(3) 139(3) yes