#------------------------------------------------------------------------------ #$Date: 2021-09-01 02:02:28 +0300 (Wed, 01 Sep 2021) $ #$Revision: 268337 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708160.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_7708160 loop_ _publ_author_name 'Ye, Hua-Jian' 'Zhang, Tian' 'Huang, Shu-Yuan' 'Liu, Xiao-Ling' 'Chen, Wen-Bin' 'Zhang, Yi-Quan' 'Tang, Jinkui' 'Dong, Wen' _publ_section_title ; Syntheses, structural modulation and slow magnetic relaxation of three dysprosium(III) complexes with mononuclear, dinuclear and one-dimensional structures ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02532E _journal_year 2021 _chemical_formula_moiety 'C16 H16 Dy N6 O8, 2(C3 H7 N O)' _chemical_formula_sum 'C22 H30 Dy N8 O10' _chemical_formula_weight 729.04 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-08-26 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2021-08-26 deposited with the CCDC. 2021-08-30 downloaded from the CCDC. ; _cell_angle_alpha 112.6490(10) _cell_angle_beta 100.3860(10) _cell_angle_gamma 98.7410(10) _cell_formula_units_Z 2 _cell_length_a 10.56300(10) _cell_length_b 11.32340(10) _cell_length_c 12.71470(10) _cell_measurement_reflns_used 14818 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 75.9100 _cell_measurement_theta_min 3.8920 _cell_volume 1338.83(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.00 _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 127.00 174.00 0.50 0.12 -- 106.06 36.00 38.00 94 2 \w 94.00 123.00 0.50 0.12 -- 106.06 36.00 38.00 58 3 \w 31.00 115.00 0.50 0.05 -- 46.00 36.00 38.00 168 4 \w 138.00 164.00 0.50 0.12 -- 106.06 30.00-180.00 52 5 \w 92.00 134.00 0.50 0.12 -- 106.06 30.00-180.00 84 6 \w 36.00 85.00 0.50 0.05 -- 46.00-125.00 60.00 98 7 \w 35.00 112.00 0.50 0.12 -- 106.06-125.00 150.00 154 8 \w 34.00 80.00 0.50 0.12 -- 106.06-125.00 120.00 92 9 \w 36.00 62.00 0.50 0.12 -- 106.06 -94.00 150.00 52 10 \w 45.00 101.00 0.50 0.12 -- 106.06 -94.00 0.00 112 11 \w 42.00 92.00 0.50 0.12 -- 106.06 -94.00 60.00 100 12 \w 63.00 89.00 0.50 0.12 -- 106.06 -94.00 -30.00 52 13 \w 52.00 78.00 0.50 0.12 -- 106.06 -94.00 -90.00 52 14 \w 37.00 112.00 0.50 0.12 -- 106.06-125.00-150.00 150 15 \w 49.00 86.00 0.50 0.12 -- 106.06 -94.00-180.00 74 16 \w 35.00 73.00 0.50 0.12 -- 106.06 -61.00-120.00 76 17 \w 37.00 71.00 0.50 0.12 -- 106.06 -61.00 -90.00 68 18 \w 41.00 71.00 0.50 0.12 -- 106.06 -61.00 -60.00 60 19 \w 42.00 73.00 0.50 0.12 -- 106.06 -61.00 60.00 62 20 \w 19.00 68.00 0.50 0.05 -- 46.00 -77.00-120.00 98 21 \w -22.00 43.00 0.50 0.05 -- 46.00 -36.00-118.00 130 22 \w -20.00 13.00 0.50 0.05 -- 46.00 -77.00-120.00 66 23 \w -24.00 44.00 0.50 0.05 -- 46.00 -37.00 120.00 136 24 \w -108.00 -30.00 0.50 0.12 -- -102.00 110.00 -37.74 156 25 \w -69.00 -44.00 0.50 0.12 -- -102.00 125.00 90.00 50 26 \w -120.00 -38.00 0.50 0.12 -- -102.00 137.00 -2.92 164 27 \w -59.00 -29.00 0.50 0.12 -- -102.00 125.00-120.00 60 28 \w -108.00 -68.00 0.50 0.12 -- -102.00 125.00-120.00 80 29 \w -108.00 -60.00 0.50 0.12 -- -102.00 110.00-141.11 96 30 \w -69.00 -30.00 0.50 0.12 -- -102.00 61.00 -90.00 78 31 \w -69.00 -29.00 0.50 0.12 -- -102.00 61.00-120.00 80 32 \w -175.00 -87.00 0.50 0.12 -- -102.00 -36.00-118.00 176 33 \w -173.00-101.00 0.50 0.12 -- -102.00 -30.00-180.00 144 34 \w -119.00 -60.00 0.50 0.05 -- -46.00 -36.00-118.00 118 35 \w -174.00 -87.00 0.50 0.12 -- -102.00 -30.00 -30.00 174 36 \w -175.00-140.00 0.50 0.12 -- -102.00 -30.00 120.00 70 37 \w -128.00 -86.00 0.50 0.12 -- -102.00 -30.00 120.00 84 38 \w -12.00 14.00 0.50 0.05 -- -46.00 36.00 38.00 52 39 \w -114.00 -89.00 0.50 0.05 -- -46.00-125.00 -30.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 17175 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.674 _diffrn_reflns_theta_min 3.903 _exptl_absorpt_coefficient_mu 15.554 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.808 _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.126 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.112 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 405 _refine_ls_number_reflns 5387 _refine_ls_number_restraints 11 _refine_ls_restrained_S_all 1.114 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0288 _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^)+(0.0491P)^2^+0.3538P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.0774 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5222 _reflns_number_total 5387 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02532e2.cif _cod_data_source_block exp_756 _cod_original_cell_volume 1338.83(2) _cod_database_code 7708160 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Restrained distances O10-C22 1.25 with sigma of 0.01 O9-C22 1.25 with sigma of 0.01 C22-N8 1.32 with sigma of 0.01 O8-C18 \\sim O8A-C18A with sigma of 0.02 C17-C18 \\sim C17A-C18A with sigma of 0.04 N7-C17 \\sim N7A-C17A with sigma of 0.02 N7-C18 \\sim N7A-C18A with sigma of 0.02 N7-C19 \\sim N7A-C19A with sigma of 0.02 C17-C19 \\sim C17A-C19A with sigma of 0.04 O8-N7 \\sim O8A-N7A with sigma of 0.04 C18-C19 \\sim C18A-C19A with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(C18A) = Uanis(C17) Uanis(C19A) = Uanis(C19) Uanis(C18) = Uanis(C17A) Uanis(N7A) = Uanis(N7) Uanis(O8A) = Uanis(O8) 4. Others Sof(N7A)=Sof(O8A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)= Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1) Sof(O8)=Sof(N7)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)= Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1) Fixed Sof: H22(0.5) H22A(0.5) O9(0.6) O10(0.4) 5.a Rotating group: O7(H7A,H7B) 5.b Aromatic/amide H refined with riding coordinates: N5(H5), C4(H4), C5(H5A), C9(H9), C12(H12), C13(H13), C14(H14), C18(H18), C22(H22), C22(H22A), C18A(H18A) 5.c Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B, H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C17A(H17D,H17E,H17F), C19A(H19D,H19E,H19F) 5.d Idealised tetrahedral OH refined as rotating group: O11(H11) ; _shelx_res_file ; TITL exp_756_a.res in P-1 exp_756.res created by SHELXL-2018/3 at 11:09:39 on 26-Aug-2021 REM Old TITL exp_756_a.res in P-1 REM SHELXT solution in P-1: R1 0.060, Rweak 0.016, Alpha 0.066 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C25 Dy N5 O11 CELL 1.54184 10.563 11.3234 12.7147 112.649 100.386 98.741 ZERR 2 0.0001 0.0001 0.0001 0.001 0.001 0.001 LATT 1 SFAC C H Dy N O UNIT 44 60 2 16 20 SADI O8 C18 O8A C18A SADI 0.04 C17 C18 C17A C18A SADI N7 C17 N7A C17A SADI N7 C18 N7A C18A SADI N7 C19 N7A C19A SADI 0.04 C17 C19 C17A C19A SADI 0.04 O8 N7 O8A N7A SADI 0.04 C18 C19 C18A C19A DFIX 1.25 0.01 O10 C22 EADP C18A C17 DFIX 1.25 0.01 O9 C22 EADP C19A C19 DFIX 1.32 0.01 C22 N8 EADP C18 C17A EADP N7A N7 EADP O8A O8 L.S. 50 0 0 PLAN 5 TEMP -173.15 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.049100 0.353800 FVAR 0.48169 0.91015 DY1 3 0.578249 0.575686 0.665138 11.00000 0.01224 0.00729 = 0.00564 0.00269 0.00148 0.00334 O11 5 0.059763 0.665052 0.743987 11.00000 0.01730 0.02629 = 0.01103 0.01028 0.00723 0.01260 AFIX 147 H11 2 0.097673 0.631455 0.785315 11.00000 -1.50000 AFIX 0 O2 5 0.220216 0.556791 0.812097 11.00000 0.01703 0.02516 = 0.01106 0.01112 0.00621 0.00836 O3 5 0.370646 0.514209 0.521568 11.00000 0.01341 0.01085 = 0.00804 0.00395 0.00231 0.00424 O4 5 0.499922 0.346537 0.595178 11.00000 0.01724 0.00700 = 0.00957 0.00300 0.00188 0.00295 O5 5 0.434419 0.251872 0.396687 11.00000 0.01885 0.01010 = 0.00950 0.00514 0.00041 0.00380 O6 5 0.605380 0.780136 0.842405 11.00000 0.02806 0.01238 = 0.01443 0.00497 0.00833 0.00753 O1 5 0.404782 0.550080 0.752463 11.00000 0.01395 0.01691 = 0.01180 0.00785 0.00350 0.00666 O7 5 0.800700 0.708165 0.720007 11.00000 0.01342 0.01281 = 0.01730 0.00452 0.00320 0.00264 AFIX 7 H7A 2 0.855655 0.662359 0.727045 11.00000 -1.50000 H7B 2 0.816474 0.770102 0.788758 11.00000 -1.50000 AFIX 0 N1 4 0.240399 0.556621 0.346083 11.00000 0.01272 0.01073 = 0.00916 0.00456 0.00139 0.00246 N2 4 0.187097 0.589619 0.266508 11.00000 0.01823 0.01434 = 0.00824 0.00521 0.00298 0.00552 N3 4 0.332607 0.470438 0.161358 11.00000 0.01413 0.01349 = 0.00957 0.00446 0.00311 0.00438 N4 4 0.209177 0.576372 0.080609 11.00000 0.01882 0.01832 = 0.01058 0.00704 0.00474 0.00731 N5 4 0.284294 0.516558 0.009795 11.00000 0.02165 0.01669 = 0.00685 0.00665 0.00454 0.00747 AFIX 43 H5 2 0.285344 0.518766 -0.058478 11.00000 -1.20000 AFIX 0 N6 4 0.641846 1.000522 0.955265 11.00000 0.02710 0.01117 = 0.01396 0.00292 0.00664 0.00706 C1 1 0.289079 0.565541 0.740764 11.00000 0.01814 0.01004 = 0.00718 0.00188 0.00279 0.00364 C2 1 0.224583 0.595616 0.643098 11.00000 0.01292 0.01328 = 0.01117 0.00698 0.00343 0.00458 C3 1 0.111491 0.647010 0.651307 11.00000 0.01503 0.01139 = 0.00907 0.00277 0.00373 0.00409 C4 1 0.046686 0.679844 0.563012 11.00000 0.01717 0.02042 = 0.01420 0.00892 0.00653 0.01039 AFIX 43 H4 2 -0.025572 0.720106 0.572927 11.00000 -1.20000 AFIX 0 C5 1 0.089693 0.652699 0.462681 11.00000 0.01898 0.01472 = 0.01199 0.00706 0.00350 0.00849 AFIX 43 H5A 2 0.046165 0.673542 0.402263 11.00000 -1.20000 AFIX 0 C6 1 0.197586 0.594305 0.448052 11.00000 0.01677 0.01244 = 0.00927 0.00570 0.00278 0.00384 C7 1 0.270450 0.566890 0.538459 11.00000 0.01209 0.00530 = 0.01007 0.00174 0.00210 0.00095 C8 1 0.242365 0.545166 0.170500 11.00000 0.01638 0.01394 = 0.00827 0.00498 0.00339 0.00494 C9 1 0.356385 0.453896 0.058056 11.00000 0.01634 0.01631 = 0.00971 0.00546 0.00368 0.00531 AFIX 43 H9 2 0.415474 0.405091 0.023761 11.00000 -1.20000 AFIX 0 C10 1 0.471842 0.249710 0.496009 11.00000 0.01276 0.01129 = 0.01333 0.00605 0.00304 0.00440 C11 1 0.485061 0.119380 0.497586 11.00000 0.01793 0.01027 = 0.01127 0.00546 0.00510 0.00588 C12 1 0.420514 0.000333 0.400469 11.00000 0.02085 0.01375 = 0.01121 0.00680 0.00169 0.00574 AFIX 43 H12 2 0.365891 0.000494 0.332449 11.00000 -1.20000 AFIX 0 C13 1 0.435564 -0.118493 0.402533 11.00000 0.02299 0.00926 = 0.01146 0.00272 0.00242 0.00444 AFIX 43 H13 2 0.391747 -0.199279 0.335837 11.00000 -1.20000 AFIX 0 C14 1 0.595998 0.892457 0.855004 11.00000 0.01934 0.01791 = 0.01218 0.00649 0.00663 0.00628 AFIX 43 H14 2 0.552478 0.901618 0.787358 11.00000 -1.20000 AFIX 0 C15 1 0.634882 1.130505 0.960056 11.00000 0.02973 0.01193 = 0.02384 0.00441 0.00903 0.00831 AFIX 137 H15A 2 0.724771 1.183990 0.978151 11.00000 -1.50000 H15B 2 0.592113 1.174348 1.021662 11.00000 -1.50000 H15C 2 0.583099 1.120236 0.883562 11.00000 -1.50000 AFIX 0 C16 1 0.712666 0.995367 1.062353 11.00000 0.03068 0.02141 = 0.01598 0.00527 0.00065 0.00476 AFIX 137 H16A 2 0.690762 0.904697 1.054765 11.00000 -1.50000 H16B 2 0.686403 1.053669 1.130206 11.00000 -1.50000 H16C 2 0.808454 1.024269 1.074094 11.00000 -1.50000 AFIX 0 PART 1 O8 5 0.409132 0.228884 0.833546 21.00000 0.03481 0.02733 = 0.01815 0.01070 0.00480 0.01088 N7 4 0.258936 0.152052 0.654119 21.00000 0.01900 0.01724 = 0.01662 0.00694 0.00676 0.00844 C17 1 0.189850 0.183080 0.562398 21.00000 0.02450 0.03238 = 0.02145 0.01431 0.00594 0.01305 AFIX 137 H17A 2 0.094295 0.162675 0.555274 21.00000 -1.50000 H17B 2 0.206940 0.130434 0.487081 21.00000 -1.50000 H17C 2 0.221624 0.277100 0.582852 21.00000 -1.50000 AFIX 0 C18 1 0.347465 0.246391 0.750850 21.00000 0.01835 0.02191 = 0.01723 0.00841 0.00881 0.01131 AFIX 43 H18 2 0.364005 0.333596 0.756117 21.00000 -1.20000 AFIX 0 C19 1 0.230774 0.015071 0.636234 21.00000 0.03167 0.02003 = 0.02915 0.00956 0.01057 0.00586 AFIX 137 H19A 2 0.139362 -0.012246 0.639154 21.00000 -1.50000 H19B 2 0.292214 0.005547 0.698447 21.00000 -1.50000 H19C 2 0.241744 -0.040509 0.559034 21.00000 -1.50000 AFIX 0 PART 0 N8 4 0.018454 -0.157536 0.125679 11.00000 0.02642 0.01979 = 0.01933 0.00868 0.00423 0.00623 C20 1 -0.007274 -0.219126 0.202379 11.00000 0.05385 0.03790 = 0.03924 0.02455 0.02319 0.02148 AFIX 137 H20A 2 -0.103248 -0.245470 0.191202 11.00000 -1.50000 H20B 2 0.034849 -0.156576 0.284693 11.00000 -1.50000 H20C 2 0.029064 -0.297252 0.183447 11.00000 -1.50000 AFIX 0 C21 1 -0.023912 -0.238150 0.000067 11.00000 0.03513 0.02484 = 0.02493 0.00543 0.00351 -0.00011 AFIX 137 H21A 2 0.003642 -0.321041 -0.017587 11.00000 -1.50000 H21B 2 0.016606 -0.190926 -0.040637 11.00000 -1.50000 H21C 2 -0.120776 -0.257266 -0.026938 11.00000 -1.50000 AFIX 0 C22 1 0.074366 -0.031020 0.168384 11.00000 0.02333 0.02925 = 0.02593 0.00329 -0.00354 0.00859 PART 1 AFIX 43 H22 2 0.080746 0.000263 0.109643 10.50000 -1.20000 AFIX 43 PART 2 H22A 2 0.099367 0.012149 0.252202 10.50000 -1.20000 AFIX 0 PART 1 O9 5 0.118341 0.051443 0.266330 10.60000 0.04027 0.02058 = 0.02600 0.00829 -0.00014 0.00184 PART 2 O10 5 0.098924 0.037691 0.123689 10.40000 0.02923 0.00957 = 0.02583 0.00017 0.01271 -0.00410 N7A 4 0.281271 0.141244 0.643054 -21.00000 0.01900 0.01724 = 0.01662 0.00694 0.00676 0.00844 O8A 5 0.117542 0.101160 0.476393 -21.00000 0.03481 0.02733 = 0.01815 0.01070 0.00480 0.01088 C18A 1 0.199990 0.176090 0.571567 -21.00000 0.02450 0.03238 = 0.02145 0.01431 0.00594 0.01305 AFIX 43 H18A 2 0.206364 0.267887 0.596598 -21.00000 -1.20000 AFIX 0 C17A 1 0.373924 0.238414 0.752825 -21.00000 0.01835 0.02191 = 0.01723 0.00841 0.00881 0.01131 AFIX 137 H17D 2 0.448388 0.283689 0.735255 -21.00000 -1.50000 H17E 2 0.407258 0.194103 0.800832 -21.00000 -1.50000 H17F 2 0.328578 0.302947 0.796375 -21.00000 -1.50000 AFIX 0 C19A 1 0.246273 0.006831 0.633135 -21.00000 0.03167 0.02003 = 0.02915 0.00956 0.01057 0.00586 AFIX 137 H19D 2 0.186267 -0.050872 0.555150 -21.00000 -1.50000 H19E 2 0.202112 0.006038 0.694437 -21.00000 -1.50000 H19F 2 0.326959 -0.024858 0.643164 -21.00000 -1.50000 AFIX 0 HKLF 4 REM exp_756_a.res in P-1 REM wR2 = 0.0774, GooF = S = 1.101, Restrained GooF = 1.114 for all data REM R1 = 0.0288 for 5222 Fo > 4sig(Fo) and 0.0295 for all 5387 data REM 405 parameters refined using 11 restraints END WGHT 0.0489 0.3632 REM Highest difference peak 1.126, deepest hole -1.256, 1-sigma level 0.112 Q1 1 0.5448 0.4621 0.6198 11.00000 0.05 1.13 Q2 1 0.6061 0.6792 0.7065 11.00000 0.05 1.12 Q3 1 0.8245 0.7832 0.7213 11.00000 0.05 0.54 Q4 1 0.5498 0.7546 0.7847 11.00000 0.05 0.49 Q5 1 0.3378 0.4034 0.4775 11.00000 0.05 0.46 ; _shelx_res_checksum 54101 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Dy1 Dy 0.57825(2) 0.57569(2) 0.66514(2) 0.00841(7) Uani 1 1 d . . . . . O11 O 0.0598(2) 0.6651(2) 0.74399(17) 0.0161(4) Uani 1 1 d . . . . . H11 H 0.097673 0.631455 0.785315 0.024 Uiso 1 1 calc R U . . . O2 O 0.2202(2) 0.5568(2) 0.81210(17) 0.0159(4) Uani 1 1 d . . . . . O3 O 0.37065(19) 0.51421(19) 0.52157(16) 0.0107(4) Uani 1 1 d . . . . . O4 O 0.4999(2) 0.34654(19) 0.59518(16) 0.0117(4) Uani 1 1 d . . . . . O5 O 0.4344(2) 0.25187(19) 0.39669(17) 0.0129(4) Uani 1 1 d . . . . . O6 O 0.6054(2) 0.7801(2) 0.84241(18) 0.0178(4) Uani 1 1 d . . . . . O1 O 0.4048(2) 0.5501(2) 0.75246(17) 0.0133(4) Uani 1 1 d . . . . . O7 O 0.8007(2) 0.7082(2) 0.72001(18) 0.0153(4) Uani 1 1 d . . . . . H7A H 0.855655 0.662359 0.727045 0.023 Uiso 1 1 d R U . . . H7B H 0.816474 0.770102 0.788758 0.023 Uiso 1 1 d R U . . . N1 N 0.2404(2) 0.5566(2) 0.3461(2) 0.0110(4) Uani 1 1 d . . . . . N2 N 0.1871(2) 0.5896(2) 0.2665(2) 0.0134(5) Uani 1 1 d . . . . . N3 N 0.3326(2) 0.4704(2) 0.1614(2) 0.0124(5) Uani 1 1 d . . . . . N4 N 0.2092(3) 0.5764(2) 0.0806(2) 0.0152(5) Uani 1 1 d . . . . . N5 N 0.2843(3) 0.5166(2) 0.0098(2) 0.0141(5) Uani 1 1 d . . . . . H5 H 0.285344 0.518766 -0.058478 0.017 Uiso 1 1 calc R U . . . N6 N 0.6418(3) 1.0005(2) 0.9553(2) 0.0177(5) Uani 1 1 d . . . . . C1 C 0.2891(3) 0.5655(3) 0.7408(2) 0.0124(5) Uani 1 1 d . . . . . C2 C 0.2246(3) 0.5956(3) 0.6431(2) 0.0117(5) Uani 1 1 d . . . . . C3 C 0.1115(3) 0.6470(3) 0.6513(2) 0.0122(5) Uani 1 1 d . . . . . C4 C 0.0467(3) 0.6798(3) 0.5630(3) 0.0157(6) Uani 1 1 d . . . . . H4 H -0.025572 0.720106 0.572927 0.019 Uiso 1 1 calc R U . . . C5 C 0.0897(3) 0.6527(3) 0.4627(2) 0.0143(5) Uani 1 1 d . . . . . H5A H 0.046165 0.673542 0.402263 0.017 Uiso 1 1 calc R U . . . C6 C 0.1976(3) 0.5943(3) 0.4481(2) 0.0125(5) Uani 1 1 d . . . . . C7 C 0.2704(3) 0.5669(2) 0.5385(2) 0.0099(5) Uani 1 1 d . . . . . C8 C 0.2424(3) 0.5452(3) 0.1705(2) 0.0126(5) Uani 1 1 d . . . . . C9 C 0.3564(3) 0.4539(3) 0.0581(2) 0.0139(5) Uani 1 1 d . . . . . H9 H 0.415474 0.405091 0.023761 0.017 Uiso 1 1 calc R U . . . C10 C 0.4718(3) 0.2497(3) 0.4960(2) 0.0121(5) Uani 1 1 d . . . . . C11 C 0.4851(3) 0.1194(3) 0.4976(2) 0.0124(5) Uani 1 1 d . . . . . C12 C 0.4205(3) 0.0003(3) 0.4005(2) 0.0150(5) Uani 1 1 d . . . . . H12 H 0.365891 0.000494 0.332449 0.018 Uiso 1 1 calc R U . . . C13 C 0.4356(3) -0.1185(3) 0.4025(2) 0.0153(6) Uani 1 1 d . . . . . H13 H 0.391747 -0.199279 0.335837 0.018 Uiso 1 1 calc R U . . . C14 C 0.5960(3) 0.8925(3) 0.8550(3) 0.0159(6) Uani 1 1 d . . . . . H14 H 0.552478 0.901618 0.787358 0.019 Uiso 1 1 calc R U . . . C15 C 0.6349(4) 1.1305(3) 0.9601(3) 0.0222(6) Uani 1 1 d . . . . . H15A H 0.724771 1.183990 0.978151 0.033 Uiso 1 1 calc R U . . . H15B H 0.592113 1.174348 1.021662 0.033 Uiso 1 1 calc R U . . . H15C H 0.583099 1.120236 0.883562 0.033 Uiso 1 1 calc R U . . . C16 C 0.7127(4) 0.9954(3) 1.0624(3) 0.0245(7) Uani 1 1 d . . . . . H16A H 0.690762 0.904697 1.054765 0.037 Uiso 1 1 calc R U . . . H16B H 0.686403 1.053669 1.130206 0.037 Uiso 1 1 calc R U . . . H16C H 0.808454 1.024269 1.074094 0.037 Uiso 1 1 calc R U . . . O8 O 0.4091(3) 0.2289(3) 0.8335(2) 0.0263(6) Uani 0.910(6) 1 d D . P A 1 N7 N 0.2589(4) 0.1521(4) 0.6541(4) 0.0169(9) Uani 0.910(6) 1 d D . P A 1 C17 C 0.1898(12) 0.1831(6) 0.5624(8) 0.0245(9) Uani 0.910(6) 1 d D . P A 1 H17A H 0.094295 0.162675 0.555274 0.037 Uiso 0.910(6) 1 calc R U P A 1 H17B H 0.206940 0.130434 0.487081 0.037 Uiso 0.910(6) 1 calc R U P A 1 H17C H 0.221624 0.277100 0.582852 0.037 Uiso 0.910(6) 1 calc R U P A 1 C18 C 0.3475(4) 0.2464(6) 0.7509(5) 0.0178(10) Uani 0.910(6) 1 d D . P A 1 H18 H 0.364005 0.333596 0.756117 0.021 Uiso 0.910(6) 1 calc R U P A 1 C19 C 0.2308(10) 0.0151(6) 0.6362(9) 0.0269(17) Uani 0.910(6) 1 d D . P A 1 H19A H 0.139362 -0.012246 0.639154 0.040 Uiso 0.910(6) 1 calc R U P A 1 H19B H 0.292214 0.005547 0.698447 0.040 Uiso 0.910(6) 1 calc R U P A 1 H19C H 0.241744 -0.040509 0.559034 0.040 Uiso 0.910(6) 1 calc R U P A 1 N8 N 0.0185(3) -0.1575(3) 0.1257(2) 0.0219(5) Uani 1 1 d D . . . . C20 C -0.0073(5) -0.2191(4) 0.2024(4) 0.0382(9) Uani 1 1 d . . . . . H20A H -0.103248 -0.245470 0.191202 0.057 Uiso 1 1 calc R U . . . H20B H 0.034849 -0.156576 0.284693 0.057 Uiso 1 1 calc R U . . . H20C H 0.029064 -0.297252 0.183447 0.057 Uiso 1 1 calc R U . . . C21 C -0.0239(4) -0.2382(4) 0.0001(3) 0.0314(8) Uani 1 1 d . . . . . H21A H 0.003642 -0.321041 -0.017587 0.047 Uiso 1 1 calc R U . . . H21B H 0.016606 -0.190926 -0.040637 0.047 Uiso 1 1 calc R U . . . H21C H -0.120776 -0.257266 -0.026938 0.047 Uiso 1 1 calc R U . . . C22 C 0.0744(4) -0.0310(3) 0.1684(3) 0.0300(8) Uani 1 1 d D . . . . H22 H 0.080746 0.000263 0.109643 0.036 Uiso 0.5 1 calc R U P B 1 H22A H 0.099367 0.012149 0.252202 0.036 Uiso 0.5 1 calc R U P C 2 O9 O 0.1183(5) 0.0514(4) 0.2663(3) 0.0314(9) Uani 0.6 1 d D . P D 1 O10 O 0.0989(6) 0.0377(5) 0.1237(5) 0.0242(12) Uani 0.4 1 d D . P D 2 N7A N 0.281(5) 0.141(5) 0.643(4) 0.0169(9) Uani 0.090(6) 1 d D . P A 2 O8A O 0.118(3) 0.101(3) 0.476(2) 0.0263(6) Uani 0.090(6) 1 d D . P A 2 C18A C 0.200(13) 0.176(5) 0.572(8) 0.0245(9) Uani 0.090(6) 1 d D . P A 2 H18A H 0.206364 0.267887 0.596598 0.029 Uiso 0.090(6) 1 calc R U P A 2 C17A C 0.374(6) 0.238(7) 0.753(5) 0.0178(10) Uani 0.090(6) 1 d D . P A 2 H17D H 0.448388 0.283689 0.735255 0.027 Uiso 0.090(6) 1 calc R U P A 2 H17E H 0.407258 0.194103 0.800832 0.027 Uiso 0.090(6) 1 calc R U P A 2 H17F H 0.328578 0.302947 0.796375 0.027 Uiso 0.090(6) 1 calc R U P A 2 C19A C 0.246(13) 0.007(6) 0.633(10) 0.0269(17) Uani 0.090(6) 1 d D . P A 2 H19D H 0.186267 -0.050872 0.555150 0.040 Uiso 0.090(6) 1 calc R U P A 2 H19E H 0.202112 0.006038 0.694437 0.040 Uiso 0.090(6) 1 calc R U P A 2 H19F H 0.326959 -0.024858 0.643164 0.040 Uiso 0.090(6) 1 calc R U P A 2 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 0.01224(10) 0.00729(10) 0.00564(10) 0.00269(6) 0.00148(6) 0.00334(6) O11 0.0173(10) 0.0263(11) 0.0110(9) 0.0103(8) 0.0072(8) 0.0126(9) O2 0.0170(10) 0.0252(11) 0.0111(9) 0.0111(8) 0.0062(8) 0.0084(9) O3 0.0134(9) 0.0108(9) 0.0080(8) 0.0039(7) 0.0023(7) 0.0042(7) O4 0.0172(10) 0.0070(9) 0.0096(9) 0.0030(7) 0.0019(7) 0.0029(7) O5 0.0189(10) 0.0101(9) 0.0095(9) 0.0051(7) 0.0004(8) 0.0038(8) O6 0.0281(12) 0.0124(10) 0.0144(10) 0.0050(8) 0.0083(9) 0.0075(9) O1 0.0140(9) 0.0169(10) 0.0118(9) 0.0079(8) 0.0035(7) 0.0067(8) O7 0.0134(10) 0.0128(9) 0.0173(10) 0.0045(8) 0.0032(8) 0.0026(8) N1 0.0127(11) 0.0107(11) 0.0092(10) 0.0046(9) 0.0014(9) 0.0025(9) N2 0.0182(12) 0.0143(11) 0.0082(10) 0.0052(9) 0.0030(9) 0.0055(10) N3 0.0141(11) 0.0135(11) 0.0096(10) 0.0045(9) 0.0031(9) 0.0044(9) N4 0.0188(12) 0.0183(12) 0.0106(11) 0.0070(10) 0.0047(9) 0.0073(10) N5 0.0217(12) 0.0167(12) 0.0069(10) 0.0067(9) 0.0045(9) 0.0075(10) N6 0.0271(14) 0.0112(11) 0.0140(12) 0.0029(10) 0.0066(10) 0.0071(10) C1 0.0181(14) 0.0100(12) 0.0072(12) 0.0019(10) 0.0028(10) 0.0036(11) C2 0.0129(13) 0.0133(13) 0.0112(12) 0.0070(10) 0.0034(10) 0.0046(11) C3 0.0150(13) 0.0114(12) 0.0091(12) 0.0028(10) 0.0037(10) 0.0041(11) C4 0.0172(14) 0.0204(14) 0.0142(13) 0.0089(11) 0.0065(11) 0.0104(12) C5 0.0190(14) 0.0147(13) 0.0120(13) 0.0071(11) 0.0035(11) 0.0085(11) C6 0.0168(13) 0.0124(13) 0.0093(12) 0.0057(10) 0.0028(10) 0.0038(11) C7 0.0121(12) 0.0053(11) 0.0101(12) 0.0017(9) 0.0021(10) 0.0010(10) C8 0.0164(13) 0.0139(13) 0.0083(12) 0.0050(10) 0.0034(10) 0.0049(11) C9 0.0163(13) 0.0163(13) 0.0097(12) 0.0055(11) 0.0037(11) 0.0053(11) C10 0.0128(13) 0.0113(12) 0.0133(13) 0.0061(10) 0.0030(10) 0.0044(10) C11 0.0179(13) 0.0103(12) 0.0113(12) 0.0055(10) 0.0051(11) 0.0059(11) C12 0.0208(14) 0.0138(13) 0.0112(13) 0.0068(11) 0.0017(11) 0.0057(11) C13 0.0230(15) 0.0093(12) 0.0115(13) 0.0027(10) 0.0024(11) 0.0044(11) C14 0.0193(14) 0.0179(14) 0.0122(13) 0.0065(11) 0.0066(11) 0.0063(12) C15 0.0297(17) 0.0119(14) 0.0238(15) 0.0044(12) 0.0090(13) 0.0083(13) C16 0.0307(17) 0.0214(16) 0.0160(15) 0.0053(12) 0.0007(13) 0.0048(13) O8 0.0348(15) 0.0273(14) 0.0182(13) 0.0107(11) 0.0048(11) 0.0109(12) N7 0.0190(19) 0.0172(15) 0.0166(15) 0.0069(12) 0.0068(13) 0.0084(13) C17 0.025(3) 0.0324(19) 0.021(2) 0.0143(16) 0.0059(15) 0.0131(17) C18 0.018(2) 0.0219(17) 0.0172(14) 0.0084(13) 0.0088(16) 0.0113(18) C19 0.032(3) 0.0200(19) 0.0292(19) 0.0096(17) 0.011(2) 0.0059(19) N8 0.0264(14) 0.0198(13) 0.0193(13) 0.0087(11) 0.0042(11) 0.0062(11) C20 0.054(3) 0.038(2) 0.039(2) 0.0246(18) 0.0232(19) 0.021(2) C21 0.035(2) 0.0248(17) 0.0249(17) 0.0054(14) 0.0035(15) -0.0001(15) C22 0.0233(17) 0.0293(18) 0.0259(18) 0.0033(15) -0.0035(14) 0.0086(15) O9 0.040(2) 0.021(2) 0.026(2) 0.0083(17) -0.0001(18) 0.0018(18) O10 0.029(3) 0.010(2) 0.026(3) 0.000(2) 0.013(2) -0.004(2) N7A 0.0190(19) 0.0172(15) 0.0166(15) 0.0069(12) 0.0068(13) 0.0084(13) O8A 0.0348(15) 0.0273(14) 0.0182(13) 0.0107(11) 0.0048(11) 0.0109(12) C18A 0.025(3) 0.0324(19) 0.021(2) 0.0143(16) 0.0059(15) 0.0131(17) C17A 0.018(2) 0.0219(17) 0.0172(14) 0.0084(13) 0.0088(16) 0.0113(18) C19A 0.032(3) 0.0200(19) 0.0292(19) 0.0096(17) 0.011(2) 0.0059(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 O3 Dy1 Dy1 37.62(5) 2_666 2_666 ? O3 Dy1 Dy1 37.59(4) . 2_666 ? O3 Dy1 O3 75.22(7) 2_666 . ? O3 Dy1 O6 113.31(7) . . ? O3 Dy1 O6 144.39(7) 2_666 . ? O3 Dy1 O7 80.93(7) 2_666 . ? O3 Dy1 O7 140.24(7) . . ? O3 Dy1 N1 126.63(7) . 2_666 ? O3 Dy1 N1 64.00(7) 2_666 2_666 ? O3 Dy1 N3 136.91(7) . 2_666 ? O3 Dy1 N3 124.80(7) 2_666 2_666 ? O4 Dy1 Dy1 70.26(5) . 2_666 ? O4 Dy1 O3 73.41(7) . . ? O4 Dy1 O3 75.55(7) . 2_666 ? O4 Dy1 O5 140.57(6) . 2_666 ? O4 Dy1 O6 139.80(7) . . ? O4 Dy1 O7 130.25(7) . . ? O4 Dy1 N1 64.48(7) . 2_666 ? O4 Dy1 N3 76.02(7) . 2_666 ? O5 Dy1 Dy1 71.05(5) 2_666 2_666 ? O5 Dy1 O3 71.48(7) 2_666 . ? O5 Dy1 O3 78.66(7) 2_666 2_666 ? O5 Dy1 O6 72.41(7) 2_666 . ? O5 Dy1 O7 72.96(7) 2_666 . ? O5 Dy1 N1 127.29(7) 2_666 2_666 ? O5 Dy1 N3 143.33(7) 2_666 2_666 ? O6 Dy1 Dy1 139.72(5) . 2_666 ? O6 Dy1 N1 119.95(7) . 2_666 ? O6 Dy1 N3 73.92(7) . 2_666 ? O1 Dy1 Dy1 106.18(5) . 2_666 ? O1 Dy1 O3 70.95(7) . . ? O1 Dy1 O3 140.21(7) . 2_666 ? O1 Dy1 O4 75.22(7) . . ? O1 Dy1 O5 108.93(7) . 2_666 ? O1 Dy1 O6 70.66(7) . . ? O1 Dy1 O7 138.87(7) . . ? O1 Dy1 N1 123.66(7) . 2_666 ? O1 Dy1 N3 72.39(7) . 2_666 ? O7 Dy1 Dy1 112.70(5) . 2_666 ? O7 Dy1 O6 71.18(7) . . ? O7 Dy1 N1 65.84(7) . 2_666 ? O7 Dy1 N3 82.85(7) . 2_666 ? N1 Dy1 Dy1 95.75(5) 2_666 2_666 ? N3 Dy1 Dy1 145.20(5) 2_666 2_666 ? N3 Dy1 N1 61.18(7) 2_666 2_666 ? C3 O11 H11 109.5 . . ? Dy1 O3 Dy1 104.78(7) 2_666 . ? C7 O3 Dy1 125.53(16) . . ? C7 O3 Dy1 124.03(16) . 2_666 ? C10 O4 Dy1 134.95(17) . . ? C10 O5 Dy1 133.74(18) . 2_666 ? C14 O6 Dy1 131.90(18) . . ? C1 O1 Dy1 136.35(17) . . ? Dy1 O7 H7A 109.4 . . ? Dy1 O7 H7B 109.4 . . ? H7A O7 H7B 104.5 . . ? N2 N1 Dy1 126.23(18) . 2_666 ? N2 N1 C6 117.2(2) . . ? C6 N1 Dy1 116.57(17) . 2_666 ? N1 N2 C8 109.8(2) . . ? C8 N3 Dy1 118.24(17) . 2_666 ? C9 N3 Dy1 138.41(19) . 2_666 ? C9 N3 C8 102.9(2) . . ? C8 N4 N5 101.6(2) . . ? N4 N5 H5 124.6 . . ? C9 N5 N4 110.8(2) . . ? C9 N5 H5 124.6 . . ? C14 N6 C15 121.4(3) . . ? C14 N6 C16 120.8(3) . . ? C16 N6 C15 117.6(3) . . ? O2 C1 C2 116.6(2) . . ? O1 C1 O2 122.0(2) . . ? O1 C1 C2 121.4(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 C7 119.4(2) . . ? C7 C2 C1 121.5(2) . . ? O11 C3 C2 120.8(2) . . ? O11 C3 C4 117.2(2) . . ? C2 C3 C4 122.0(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C4 C5 H5A 119.6 . . ? C4 C5 C6 120.8(3) . . ? C6 C5 H5A 119.6 . . ? N1 C6 C5 123.7(2) . . ? N1 C6 C7 114.5(2) . . ? C5 C6 C7 121.8(2) . . ? O3 C7 C2 123.4(2) . . ? O3 C7 C6 119.7(2) . . ? C6 C7 C2 116.9(2) . . ? N3 C8 N2 124.4(2) . . ? N4 C8 N2 120.5(3) . . ? N4 C8 N3 115.1(2) . . ? N3 C9 N5 109.5(3) . . ? N3 C9 H9 125.2 . . ? N5 C9 H9 125.2 . . ? O4 C10 O5 126.2(3) . . ? O4 C10 C11 116.0(2) . . ? O5 C10 C11 117.8(2) . . ? C12 C11 C10 121.1(2) . . ? C12 C11 C13 119.6(3) . 2_656 ? C13 C11 C10 119.3(3) 2_656 . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C13 H13 120.0 2_656 . ? C12 C13 C11 120.1(3) . 2_656 ? C12 C13 H13 120.0 . . ? O6 C14 N6 125.2(3) . . ? O6 C14 H14 117.4 . . ? N6 C14 H14 117.4 . . ? N6 C15 H15A 109.5 . . ? N6 C15 H15B 109.5 . . ? N6 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 N7 C19 117.6(4) . . ? C18 N7 C17 121.0(4) . . ? C18 N7 C19 121.4(4) . . ? N7 C17 H17A 109.5 . . ? N7 C17 H17B 109.5 . . ? N7 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O8 C18 N7 125.2(5) . . ? O8 C18 H18 117.4 . . ? N7 C18 H18 117.4 . . ? N7 C19 H19A 109.5 . . ? N7 C19 H19B 109.5 . . ? N7 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 N8 C21 117.9(3) . . ? C22 N8 C20 121.1(3) . . ? C22 N8 C21 121.0(3) . . ? N8 C20 H20A 109.5 . . ? N8 C20 H20B 109.5 . . ? N8 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N8 C21 H21A 109.5 . . ? N8 C21 H21B 109.5 . . ? N8 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N8 C22 H22 113.9 . . ? N8 C22 H22A 113.8 . . ? O9 C22 N8 132.1(4) . . ? O9 C22 H22 113.9 . . ? O10 C22 N8 132.3(4) . . ? O10 C22 H22A 113.8 . . ? C18A N7A C17A 122(3) . . ? C18A N7A C19A 118(3) . . ? C17A N7A C19A 116(3) . . ? N7A C18A H18A 116.5 . . ? O8A C18A N7A 127(4) . . ? O8A C18A H18A 116.5 . . ? N7A C17A H17D 109.5 . . ? N7A C17A H17E 109.5 . . ? N7A C17A H17F 109.5 . . ? H17D C17A H17E 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? N7A C19A H19D 109.5 . . ? N7A C19A H19E 109.5 . . ? N7A C19A H19F 109.5 . . ? H19D C19A H19E 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 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 Dy1 Dy1 3.7944(3) 2_666 ? Dy1 O3 2.3958(19) . ? Dy1 O3 2.3939(18) 2_666 ? Dy1 O4 2.3480(19) . ? Dy1 O5 2.3817(19) 2_666 ? Dy1 O6 2.463(2) . ? Dy1 O1 2.344(2) . ? Dy1 O7 2.406(2) . ? Dy1 N1 2.596(2) 2_666 ? Dy1 N3 2.513(2) 2_666 ? O11 H11 0.8400 . ? O11 C3 1.345(3) . ? O2 C1 1.283(3) . ? O3 C7 1.303(3) . ? O4 C10 1.258(3) . ? O5 C10 1.264(3) . ? O6 C14 1.241(4) . ? O1 C1 1.251(4) . ? O7 H7A 0.8500 . ? O7 H7B 0.8506 . ? N1 N2 1.277(3) . ? N1 C6 1.383(4) . ? N2 C8 1.399(4) . ? N3 C8 1.359(4) . ? N3 C9 1.329(4) . ? N4 N5 1.360(4) . ? N4 C8 1.326(4) . ? N5 H5 0.8800 . ? N5 C9 1.338(4) . ? N6 C14 1.324(4) . ? N6 C15 1.463(4) . ? N6 C16 1.457(4) . ? C1 C2 1.488(4) . ? C2 C3 1.409(4) . ? C2 C7 1.434(4) . ? C3 C4 1.410(4) . ? C4 H4 0.9500 . ? C4 C5 1.370(4) . ? C5 H5A 0.9500 . ? C5 C6 1.408(4) . ? C6 C7 1.428(4) . ? C9 H9 0.9500 . ? C10 C11 1.511(4) . ? C11 C12 1.394(4) . ? C11 C13 1.394(4) 2_656 ? C12 H12 0.9500 . ? C12 C13 1.388(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O8 C18 1.234(6) . ? N7 C17 1.450(6) . ? N7 C18 1.341(5) . ? N7 C19 1.453(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N8 C20 1.440(5) . ? N8 C21 1.442(4) . ? N8 C22 1.313(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22 0.9500 . ? C22 H22A 0.9500 . ? C22 O9 1.184(5) . ? C22 O10 1.152(6) . ? N7A C18A 1.35(2) . ? N7A C17A 1.45(2) . ? N7A C19A 1.461(19) . ? O8A C18A 1.24(2) . ? C18A H18A 0.9500 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 O3 C7 C2 -43.9(3) . . . . ? Dy1 O3 C7 C2 166.75(19) 2_666 . . . ? Dy1 O3 C7 C6 -10.9(3) 2_666 . . . ? Dy1 O3 C7 C6 138.4(2) . . . . ? Dy1 O4 C10 O5 -27.0(5) . . . . ? Dy1 O4 C10 C11 152.80(19) . . . . ? Dy1 O5 C10 O4 9.2(5) 2_666 . . . ? Dy1 O5 C10 C11 -170.67(18) 2_666 . . . ? Dy1 O6 C14 N6 -163.8(2) . . . . ? Dy1 O1 C1 O2 -172.17(19) . . . . ? Dy1 O1 C1 C2 7.6(4) . . . . ? Dy1 N1 N2 C8 -0.8(3) 2_666 . . . ? Dy1 N1 C6 C5 -172.3(2) 2_666 . . . ? Dy1 N1 C6 C7 6.5(3) 2_666 . . . ? Dy1 N3 C8 N2 -5.5(4) 2_666 . . . ? Dy1 N3 C8 N4 173.74(19) 2_666 . . . ? Dy1 N3 C9 N5 -171.6(2) 2_666 . . . ? O11 C3 C4 C5 -174.7(3) . . . . ? O2 C1 C2 C3 16.9(4) . . . . ? O2 C1 C2 C7 -159.7(3) . . . . ? O4 C10 C11 C12 160.2(3) . . . . ? O4 C10 C11 C13 -20.5(4) . . . 2_656 ? O5 C10 C11 C12 -19.9(4) . . . . ? O5 C10 C11 C13 159.3(3) . . . 2_656 ? O1 C1 C2 C3 -162.9(3) . . . . ? O1 C1 C2 C7 20.6(4) . . . . ? N1 N2 C8 N3 4.1(4) . . . . ? N1 N2 C8 N4 -175.1(3) . . . . ? N1 C6 C7 O3 2.0(4) . . . . ? N1 C6 C7 C2 -175.8(2) . . . . ? N2 N1 C6 C5 7.5(4) . . . . ? N2 N1 C6 C7 -173.7(2) . . . . ? N4 N5 C9 N3 -0.4(3) . . . . ? N5 N4 C8 N2 179.3(3) . . . . ? N5 N4 C8 N3 0.0(3) . . . . ? C1 C2 C3 O11 -2.0(4) . . . . ? C1 C2 C3 C4 178.9(3) . . . . ? C1 C2 C7 O3 -0.5(4) . . . . ? C1 C2 C7 C6 177.2(2) . . . . ? C2 C3 C4 C5 4.4(4) . . . . ? C3 C2 C7 O3 -177.1(2) . . . . ? C3 C2 C7 C6 0.7(4) . . . . ? C3 C4 C5 C6 -0.7(4) . . . . ? C4 C5 C6 N1 175.7(3) . . . . ? C4 C5 C6 C7 -3.1(4) . . . . ? C5 C6 C7 O3 -179.2(3) . . . . ? C5 C6 C7 C2 3.0(4) . . . . ? C6 N1 N2 C8 179.4(2) . . . . ? C7 C2 C3 O11 174.6(2) . . . . ? C7 C2 C3 C4 -4.4(4) . . . . ? C8 N3 C9 N5 0.4(3) . . . . ? C8 N4 N5 C9 0.2(3) . . . . ? C9 N3 C8 N2 -179.5(3) . . . . ? C9 N3 C8 N4 -0.3(3) . . . . ? C10 C11 C12 C13 178.9(3) . . . . ? C11 C12 C13 C11 0.4(5) . . . 2_656 ? C13 C11 C12 C13 -0.4(5) 2_656 . . . ? C15 N6 C14 O6 175.5(3) . . . . ? C16 N6 C14 O6 1.5(5) . . . . ? C17 N7 C18 O8 179.0(9) . . . . ? C19 N7 C18 O8 -2.3(8) . . . . ? C20 N8 C22 O9 4.3(7) . . . . ? C20 N8 C22 O10 -176.7(6) . . . . ? C21 N8 C22 O9 -178.2(5) . . . . ? C21 N8 C22 O10 0.8(8) . . . . ? C17A N7A C18A O8A -180(13) . . . . ? C19A N7A C18A O8A -21(22) . . . . ?