#------------------------------------------------------------------------------ #$Date: 2020-08-21 04:43:26 +0300 (Fri, 21 Aug 2020) $ #$Revision: 255505 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705229.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_7705229 loop_ _publ_author_name 'Li, Meng-Hua' 'Lv, Shu-Li' 'You, Ming-Hua' 'Lin, Mei-Jin' _publ_section_title ; Three-component D-A hybrid heterostructures with enhanced photochromic, photomodulated luminescent and selectively anion-sensing properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02390F _journal_year 2020 _chemical_formula_moiety 'C14 H20 Dy N2 O8, C6 Co N6, H2 O' _chemical_formula_sum 'C20 H22 Co Dy N8 O9' _chemical_formula_weight 739.88 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-07-30 _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _audit_update_record ; 2020-07-30 deposited with the CCDC. 2020-08-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 130.46(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 31.279(5) _cell_length_b 11.3714(10) _cell_length_c 21.267(4) _cell_measurement_reflns_used 7937 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.7470 _cell_measurement_theta_min 1.9250 _cell_volume 5755(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _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 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -31.00 6.00 0.50 10.00 -- 5.00 28.00 -43.00 74 2 \w -18.00 15.00 0.50 10.00 -- 5.00 55.00-150.00 66 3 \w 5.00 31.00 0.50 10.00 -- -9.60 43.00 150.00 52 4 \w 34.00 59.00 0.50 10.00 -- -9.60 43.00 150.00 50 5 \w -99.00 -8.00 0.50 10.00 -- -9.60 43.00 150.00 182 6 \w -94.00 75.00 0.50 10.00 -- -9.60 55.00-120.00 338 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0246652000 _diffrn_orient_matrix_UB_12 0.0201527000 _diffrn_orient_matrix_UB_13 -0.0080670000 _diffrn_orient_matrix_UB_21 0.0164846000 _diffrn_orient_matrix_UB_22 0.0208223000 _diffrn_orient_matrix_UB_23 0.0412604000 _diffrn_orient_matrix_UB_31 0.0027451000 _diffrn_orient_matrix_UB_32 0.0552793000 _diffrn_orient_matrix_UB_33 -0.0123254000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1530 _diffrn_reflns_av_unetI/netI 0.0852 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 22758 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 1.917 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.211 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.16777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.708 _exptl_crystal_description block _exptl_crystal_F_000 2904 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _refine_diff_density_max 2.085 _refine_diff_density_min -3.583 _refine_diff_density_rms 0.337 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 5090 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0667 _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^)+(0.1880P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1912 _refine_ls_wR_factor_ref 0.2527 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3784 _reflns_number_total 5090 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02390f2.cif _cod_data_source_block co-dy-3 _cod_original_cell_volume 5756(2) _cod_database_code 7705229 _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. ; _shelx_estimated_absorpt_t_max 0.680 _shelx_estimated_absorpt_t_min 0.489 _reflns_odcompleteness_completeness 99.50 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances Dy3-H7a \\sim Dy3-H7b with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 4.a Free rotating group: O7(H7a,H7b), O9(H9a,H9b) 4.b Rotating group: O5(H5a,H5b), O8(H8a,H8b), O2(H2a,H2b) 4.c Secondary CH2 refined with riding coordinates: C2(H2c,H2d), C13(H13a,H13b) 4.d Aromatic/amide H refined with riding coordinates: C4(H4), C12(H12), C11(H11), C9(H9), C10(H10), C7(H7), C3(H3), C6(H6) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL co-dy-3_a.res in C2/c co-dy-3.res created by SHELXL-2018/3 at 14:21:57 on 30-Jul-2020 REM Old TITL Co-Dy-3 in C2/c REM SHELXT solution in C2/c REM R1 0.161, Rweak 0.006, Alpha 0.082, Orientation as input REM Formula found by SHELXT: C40 N21 O17 Co2 Dy2 CELL 0.71073 31.2793 11.3714 21.2666 90 130.455 90 ZERR 8 0.0052 0.001 0.0035 0 0.027 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Co Dy N O UNIT 160 176 8 8 64 72 SADI Dy3 H7a Dy3 H7b ISOR 0.001 0.002 N1 L.S. 4 0 0 PLAN 30 SIZE 0.26 0.18 0.13 CONF BOND $H list 4 MORE -1 ABIN fmap 2 53 acta SHEL 999 0.84 REM REM REM WGHT 0.188000 FVAR 0.12834 DY3 4 0.575219 0.052020 0.510790 11.00000 0.02881 0.03964 = 0.03196 0.00227 0.01699 0.00191 CO02 3 0.361845 0.475349 0.213292 11.00000 0.04498 0.03935 = 0.03304 0.00210 0.02759 -0.00114 O3 6 0.398890 0.034617 0.366088 11.00000 0.04581 0.06559 = 0.03798 0.00540 0.02604 -0.00048 N8 5 0.065596 -0.136735 -0.012565 11.00000 0.03239 0.03725 = 0.03330 0.00096 0.01731 0.00174 AFIX 6 O7 6 0.654927 0.168740 0.614545 11.00000 0.04496 0.05296 = 0.06004 -0.01874 0.03412 -0.01505 H7A 2 0.641153 0.226718 0.621319 11.00000 -1.50000 H7B 2 0.666053 0.197921 0.590557 11.00000 -1.50000 AFIX 0 O5 6 0.568394 0.237576 0.449873 11.00000 0.04326 0.08605 = 0.08867 0.04002 0.03895 0.01157 AFIX 7 H5A 2 0.535083 0.245679 0.401525 11.00000 -1.50000 H5B 2 0.590832 0.239104 0.438759 11.00000 -1.50000 AFIX 0 O1 6 -0.044759 -0.319636 -0.061064 11.00000 0.03805 0.06510 = 0.06610 0.00550 0.03286 -0.00995 O8 6 0.658918 -0.057413 0.570641 11.00000 0.05552 0.06544 = 0.07645 0.00220 0.04984 0.00941 AFIX 7 H8A 2 0.683517 -0.013254 0.575138 11.00000 -1.50000 H8B 2 0.652387 -0.113166 0.537292 11.00000 -1.50000 AFIX 0 N7 5 0.345896 -0.000974 0.203076 11.00000 0.03675 0.05241 = 0.03527 0.00043 0.02152 -0.00770 N2 5 0.352645 0.624797 0.322532 11.00000 0.05307 0.06432 = 0.06311 -0.01927 0.03885 -0.00670 C19 1 0.356710 0.566243 0.282032 11.00000 0.03165 0.03819 = 0.03555 0.00455 0.01906 0.00757 O6 6 0.037861 -0.360051 -0.028660 11.00000 0.03937 0.06922 = 0.06370 0.00159 0.03452 -0.00301 AFIX 6 O9 6 0.731657 -0.098551 0.730873 11.00000 0.05525 0.10957 = 0.07628 0.02186 0.04181 0.00846 H9A 2 0.716876 -0.052224 0.690136 11.00000 -1.50000 H9B 2 0.728770 -0.069121 0.764701 11.00000 -1.50000 AFIX 0 C8 1 0.234805 -0.059818 0.105898 11.00000 0.03130 0.03963 = 0.02168 -0.00988 0.01282 -0.00546 C5 1 0.175306 -0.089586 0.062583 11.00000 0.03235 0.04312 = 0.02274 -0.00710 0.01410 -0.00795 C1 1 0.000310 -0.294118 -0.044757 11.00000 0.03069 0.04328 = 0.03610 0.00418 0.01690 -0.00621 O4 6 0.480556 0.074976 0.398948 11.00000 0.02399 0.08715 = 0.04406 0.01606 0.00519 -0.00437 C4 1 0.161636 -0.136031 0.107555 11.00000 0.03384 0.07794 = 0.02051 0.00179 0.01397 -0.00680 AFIX 43 H4 2 0.189628 -0.151502 0.163638 11.00000 -1.20000 AFIX 0 C12 1 0.249797 0.038545 0.089231 11.00000 0.04919 0.04403 = 0.03696 0.00589 0.02355 -0.00946 AFIX 43 H12 2 0.222612 0.085826 0.044644 11.00000 -1.20000 AFIX 0 N3 5 0.470587 0.371270 0.366583 11.00000 0.06570 0.11982 = 0.06681 0.04210 0.04220 0.05160 O2 6 0.573252 0.007032 0.400828 11.00000 0.11371 0.07020 = 0.06612 0.00171 0.06325 -0.00163 AFIX 7 H2A 2 0.568748 0.059876 0.362081 11.00000 -1.50000 H2B 2 0.577017 -0.068342 0.385134 11.00000 -1.50000 AFIX 0 C11 1 0.306083 0.068697 0.139093 11.00000 0.04954 0.04656 = 0.03587 0.00118 0.02723 -0.01395 AFIX 43 H11 2 0.316594 0.137385 0.128507 11.00000 -1.20000 AFIX 0 C16 1 0.367912 0.373361 0.146675 11.00000 0.07657 0.06611 = 0.05060 0.01587 0.04751 -0.00058 C9 1 0.277869 -0.138099 0.170082 11.00000 0.03419 0.03957 = 0.03614 -0.00266 0.01752 -0.00793 AFIX 43 H9 2 0.268729 -0.209952 0.179569 11.00000 -1.20000 AFIX 0 C10 1 0.333067 -0.102626 0.216874 11.00000 0.03730 0.05086 = 0.04362 0.01015 0.02263 0.00090 AFIX 43 H10 2 0.361649 -0.151212 0.258788 11.00000 -1.20000 AFIX 0 C18 1 0.404920 0.596473 0.218628 11.00000 0.05280 0.05630 = 0.03847 0.00612 0.03049 0.00512 C14 1 0.430242 0.047870 0.349432 11.00000 0.03228 0.03666 = 0.03825 0.00737 0.01920 0.00272 C2 1 0.007792 -0.167291 -0.049614 11.00000 0.02969 0.04352 = 0.05266 0.00480 0.02077 0.00474 AFIX 23 H2C 2 -0.017611 -0.143321 -0.107141 11.00000 -1.20000 H2D 2 -0.002222 -0.123839 -0.021555 11.00000 -1.20000 AFIX 0 C20 1 0.428757 0.410615 0.308919 11.00000 0.09179 0.02374 = 0.05890 0.00308 0.05985 0.01186 N5 5 0.372930 0.310855 0.109450 11.00000 0.12272 0.06240 = 0.07394 -0.01127 0.08114 -0.00326 C7 1 0.078024 -0.093494 -0.057282 11.00000 0.04008 0.08047 = 0.03164 0.01319 0.01845 -0.00796 AFIX 43 H7 2 0.049770 -0.082531 -0.113879 11.00000 -1.20000 AFIX 0 C3 1 0.107115 -0.158913 0.069363 11.00000 0.06329 0.05375 = 0.04265 -0.00307 0.04126 -0.00730 AFIX 43 H3 2 0.097959 -0.190290 0.099687 11.00000 -1.20000 AFIX 0 N4 5 0.429369 0.683028 0.224107 11.00000 0.08666 0.08868 = 0.07464 -0.00526 0.05498 -0.03280 C13 1 0.404594 0.037181 0.258489 11.00000 0.03659 0.09291 = 0.04757 -0.01143 0.02910 -0.01818 AFIX 23 H13A 2 0.407055 0.112867 0.239980 11.00000 -1.20000 H13B 2 0.426537 -0.018622 0.255202 11.00000 -1.20000 AFIX 0 C6 1 0.130885 -0.066047 -0.020854 11.00000 0.04055 0.09774 = 0.03263 0.01978 0.01583 -0.01753 AFIX 43 H6 2 0.138510 -0.030057 -0.051907 11.00000 -1.20000 AFIX 0 C15 1 0.315742 0.363034 0.208117 11.00000 0.08776 0.08669 = 0.05252 -0.03199 0.05645 -0.04282 N6 5 0.257681 0.590947 0.061500 11.00000 0.10150 0.21012 = 0.04046 0.01642 0.03479 0.04354 C17 1 0.296997 0.543531 0.118701 11.00000 0.06646 0.08458 = 0.04167 -0.00326 0.03626 -0.00622 N1 5 0.283469 0.297253 0.200705 11.00000 0.08595 0.08555 = 0.08275 -0.00101 0.05604 -0.00267 HKLF 4 REM co-dy-3_a.res in C2/c REM wR2 = 0.2527, GooF = S = 1.049, Restrained GooF = 1.049 for all data REM R1 = 0.0667 for 3784 Fo > 4sig(Fo) and 0.0918 for all 5090 data REM 361 parameters refined using 7 restraints END WGHT 0.1880 0.0000 REM Highest difference peak 2.085, deepest hole -3.583, 1-sigma level 0.337 Q1 1 0.5581 0.0994 0.4601 11.00000 0.05 2.09 Q2 1 0.6033 0.0953 0.5154 11.00000 0.05 2.00 Q3 1 0.5574 0.0052 0.4576 11.00000 0.05 1.77 Q4 1 0.5797 0.1854 0.5144 11.00000 0.05 1.74 Q5 1 0.0830 -0.4179 0.0129 11.00000 0.05 1.70 Q6 1 0.6003 0.0978 0.5622 11.00000 0.05 1.70 Q7 1 0.5411 0.2010 0.4450 11.00000 0.05 1.53 Q8 1 0.5980 0.0054 0.5660 11.00000 0.05 1.51 Q9 1 0.6060 0.0067 0.5167 11.00000 0.05 1.50 Q10 1 0.0735 -0.3212 0.0091 11.00000 0.05 1.44 Q11 1 0.6024 0.1999 0.5512 11.00000 0.05 1.38 Q12 1 0.3186 0.2536 0.2392 11.00000 0.05 1.37 Q13 1 0.5585 0.1962 0.4818 11.00000 0.05 1.36 Q14 1 0.5977 0.2809 0.5235 11.00000 0.05 1.25 Q15 1 0.5774 -0.1821 0.3968 11.00000 0.05 1.08 Q16 1 0.5392 0.0003 0.4958 11.00000 0.05 1.04 Q17 1 0.5397 -0.0958 0.3553 11.00000 0.05 1.02 Q18 1 0.5692 0.2804 0.4987 11.00000 0.05 1.00 Q19 1 0.5548 0.2150 0.3882 11.00000 0.05 0.94 Q20 1 0.6791 0.2530 0.5596 11.00000 0.05 0.90 Q21 1 0.0393 -0.3199 -0.0755 11.00000 0.05 0.89 Q22 1 0.7757 -0.1939 0.7989 11.00000 0.05 0.88 Q23 1 -0.0265 -0.3212 0.0252 11.00000 0.05 0.87 Q24 1 0.6345 -0.0781 0.5644 11.00000 0.05 0.87 Q25 1 0.7255 -0.2107 0.6982 11.00000 0.05 0.86 Q26 1 0.7187 -0.1364 0.7423 11.00000 0.05 0.86 Q27 1 0.6441 0.2533 0.5233 11.00000 0.05 0.85 Q28 1 0.4998 0.7629 0.3051 11.00000 0.05 0.84 Q29 1 0.6560 -0.0540 0.5345 11.00000 0.05 0.84 Q30 1 0.2772 -0.2769 0.2251 11.00000 0.05 0.81 ; _shelx_res_checksum 80537 _shelx_fab_file ; -37 1 15 -0.4656 0.3613 -37 1 16 -4.0108 0.2604 -37 1 17 2.2538 0.4674 -36 0 12 1.5485 -0.0942 -36 0 14 -4.0652 -0.1480 -36 0 16 -0.9337 -0.2353 -36 0 18 -2.5358 -0.2550 -36 0 20 2.9855 -0.0449 -36 2 12 -2.2343 -0.4508 -36 2 13 1.7297 -0.4441 -36 2 14 0.6087 -0.0049 -36 2 15 -0.4742 -0.2025 -36 2 16 0.8771 -0.3461 -36 2 17 -1.8920 -0.3375 -36 2 18 2.1083 -0.2167 -36 2 19 0.7717 -0.1559 -35 1 10 4.1492 0.2925 -35 1 11 -0.8973 -0.1845 -35 1 12 -0.9721 0.1730 -35 1 13 -2.9548 -0.0479 -35 1 14 5.4125 0.2136 -35 1 15 -2.7156 -0.2034 -35 1 16 -0.0890 -0.1435 -35 1 17 0.9636 0.0136 -35 1 18 0.6902 0.1432 -35 1 19 -0.1087 -0.1166 -35 1 20 -1.6261 0.5295 -35 1 21 1.7116 0.2328 -35 3 11 -0.9110 0.2332 -35 3 12 1.1298 -0.0410 -35 3 13 0.3391 0.1936 -35 3 14 -2.9461 0.1925 -35 3 15 3.5485 0.4657 -35 3 16 -1.9600 0.0952 -35 3 17 0.8986 0.0727 -35 3 18 -4.6421 -0.1261 -35 3 19 -1.1871 0.3216 -35 3 20 1.6433 -0.0275 -34 0 8 3.1930 0.1488 -34 0 10 -0.9539 -0.1034 -34 0 12 3.1658 0.0170 -34 0 14 0.9127 0.1691 -34 0 16 0.5790 0.1192 -34 0 18 -4.1990 -0.0398 -34 0 20 0.4681 0.1277 -34 0 22 -0.0678 -0.1321 -34 2 8 0.8479 -0.4112 -34 2 9 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0.1233 17 7 3 1.7560 -0.0228 17 7 4 -3.7747 -0.1374 17 7 5 3.0497 0.1440 17 7 6 0.4722 0.1775 17 9 0 -1.2599 -0.0997 17 9 1 -2.3491 0.0170 17 9 2 -1.3357 -0.0175 17 9 3 -2.4608 -0.0526 18 0 0 9.1526 0.4261 18 0 2 -11.5577 -0.5785 18 0 4 1.8405 0.2431 18 0 6 -3.0187 -0.0562 18 0 8 0.3100 -0.1108 18 2 0 -2.9184 -0.2329 18 2 1 7.2956 0.0249 18 2 2 -1.9923 0.3177 18 2 3 -4.8748 -0.0659 18 2 4 1.8260 -0.0299 18 2 5 -3.1354 0.0091 18 2 6 -1.8970 -0.0028 18 2 7 -4.1251 -0.1316 18 2 8 1.9168 0.0377 18 4 0 -2.5444 0.0009 18 4 1 -0.1227 0.2994 18 4 2 11.1737 -0.0230 18 4 3 0.9810 -0.0737 18 4 4 -2.0596 0.0121 18 4 5 3.5896 -0.0742 18 4 6 6.2842 0.1783 18 4 7 4.7321 0.2912 18 6 0 1.0802 -0.0227 18 6 1 -0.8241 -0.0617 18 6 2 -5.9238 -0.1399 18 6 3 1.2093 -0.0774 18 6 4 1.3785 0.0500 18 6 5 3.4344 0.0647 18 6 6 -1.6674 -0.3916 18 8 0 0.3318 0.0557 18 8 1 1.6882 -0.0167 18 8 2 -0.8790 -0.0708 18 8 3 -6.3127 -0.0067 18 8 4 1.2101 0.2152 18 10 0 -4.7625 0.0532 18 10 1 0.9687 -0.0484 19 1 0 -6.2123 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20 4 2 2.4807 -0.0248 20 4 3 -5.2457 -0.0071 20 4 4 -7.7695 -0.1319 20 4 5 -8.2156 -0.2745 20 4 6 6.5884 -0.2694 20 6 0 6.2772 0.0689 20 6 1 0.4383 -0.0283 20 6 2 -0.6885 -0.0688 20 6 3 -4.5321 0.0078 20 6 4 5.4436 0.4399 20 6 5 1.9044 0.1992 20 8 0 -0.8279 0.0652 20 8 1 4.7642 0.0369 20 8 2 -1.3589 -0.1927 21 1 0 -3.0517 0.1507 21 1 1 2.5671 0.8025 21 1 2 -0.5180 -0.1296 21 1 3 -0.8771 -0.2852 21 1 4 -4.5483 0.0175 21 1 5 -5.2465 -0.3293 21 1 6 3.7715 -0.0592 21 3 0 1.9712 0.1168 21 3 1 1.8598 -0.0902 21 3 2 1.4796 0.1305 21 3 3 -3.4526 0.0669 21 3 4 0.3964 -0.0244 21 3 5 -0.3586 -0.0177 21 3 6 -3.1232 0.3466 21 5 0 3.4029 -0.3134 21 5 1 -3.7556 -0.0159 21 5 2 -1.2190 -0.0284 21 5 3 10.4674 0.0076 21 5 4 7.9042 0.1310 21 7 0 -7.4290 -0.0819 21 7 1 -0.4324 0.0430 21 7 2 1.5541 0.0535 21 7 3 -3.7991 -0.0015 21 9 0 0.5191 0.0925 22 0 0 3.9774 0.0752 22 0 2 -2.2616 -0.1285 22 0 4 5.9611 -0.0602 22 2 0 2.2315 -0.1038 22 2 1 -4.3913 -0.1506 22 2 2 -2.0969 0.1008 22 2 3 -6.4407 -0.2031 22 2 4 2.2755 0.1135 22 2 5 0.3175 0.3894 22 4 0 -2.4485 0.0587 22 4 1 5.4309 0.0998 22 4 2 8.6782 0.0733 22 4 3 7.0052 0.1426 22 4 4 -9.4907 0.1455 22 6 0 -0.0954 0.1258 22 6 1 6.6723 -0.0261 22 6 2 -7.4488 -0.2822 22 6 3 -4.5000 -0.1848 22 8 0 0.5202 0.1540 23 1 0 1.7915 0.2002 23 1 1 5.6404 0.2237 23 1 2 4.4707 -0.0703 23 1 3 6.3804 0.2850 23 1 4 -5.4228 -0.1517 23 3 0 -3.8036 -0.0800 23 3 1 2.5044 0.0275 23 3 2 -2.3471 -0.0547 23 3 3 -0.9321 0.0557 23 3 4 3.5835 -0.3602 23 5 0 2.4571 -0.0576 23 5 1 -10.6708 0.0368 23 5 2 -6.3243 -0.0183 23 5 3 -1.2043 -0.1201 23 7 0 -2.9383 -0.0753 23 7 1 5.4118 0.0155 24 0 0 1.0225 0.0984 24 0 2 -8.9457 -0.0427 24 0 4 5.7221 -0.3936 24 2 0 3.2435 0.0309 24 2 1 4.5474 0.2238 24 2 2 -1.9606 0.0560 24 2 3 -3.1009 -0.2719 24 4 0 -8.1933 -0.0448 24 4 1 -2.0367 -0.0452 24 4 2 11.5841 -0.0501 24 6 0 5.9339 0.0432 24 6 1 4.8935 0.0936 25 1 0 -4.1765 -0.0460 25 1 1 -5.3944 -0.2419 25 1 2 6.2569 0.2439 25 1 3 1.4145 0.2874 25 3 0 4.6342 0.0130 25 3 1 2.1848 -0.0557 25 3 2 -3.5306 0.1940 25 5 0 3.1395 0.0156 25 5 1 0.0552 -0.0432 26 0 0 12.0623 0.0969 26 0 2 -9.4766 0.5824 26 2 0 0.8275 -0.0754 26 2 1 5.5192 0.1161 26 2 2 4.2056 -0.3624 26 4 0 -12.2319 0.0097 26 4 1 -2.0804 -0.1618 27 1 0 -6.5901 -0.1767 27 1 1 -1.7563 -0.2963 27 3 0 4.1891 0.0216 28 0 0 11.4036 -0.6214 28 2 0 -4.0820 0.3060 0 0 0 0.0 0.0 ; _shelx_fab_checksum 28493 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 4.110 _oxdiff_exptl_absorpt_empirical_full_min 0.567 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy3 Dy 0.57522(2) 0.05202(4) 0.51079(3) 0.0355(3) Uani 1 1 d D . . . . Co02 Co 0.36184(6) 0.47535(14) 0.21329(8) 0.0374(4) Uani 1 1 d . . . . . O3 O 0.3989(3) 0.0346(7) 0.3661(5) 0.051(2) Uani 1 1 d . . . . . N8 N 0.0656(3) -0.1367(8) -0.0126(5) 0.037(2) Uani 1 1 d . . . . . O7 O 0.6549(3) 0.1687(8) 0.6145(5) 0.053(2) Uani 1 1 d G . . . . H7A H 0.641153 0.226718 0.621319 0.079 Uiso 1 1 d DG U . . . H7B H 0.666053 0.197921 0.590557 0.079 Uiso 1 1 d DG U . . . O5 O 0.5684(3) 0.2376(9) 0.4499(6) 0.076(3) Uani 1 1 d . . . . . H5A H 0.535083 0.245679 0.401525 0.113 Uiso 1 1 d R U . . . H5B H 0.590832 0.239104 0.438759 0.113 Uiso 1 1 d R U . . . O1 O -0.0448(3) -0.3196(8) -0.0611(5) 0.057(2) Uani 1 1 d . . . . . O8 O 0.6589(4) -0.0574(8) 0.5706(6) 0.061(2) Uani 1 1 d . . . . . H8A H 0.683517 -0.013254 0.575138 0.091 Uiso 1 1 d R U . . . H8B H 0.652387 -0.113166 0.537292 0.091 Uiso 1 1 d R U . . . N7 N 0.3459(4) -0.0010(9) 0.2031(5) 0.043(2) Uani 1 1 d . . . . . N2 N 0.3526(4) 0.6248(10) 0.3225(6) 0.059(3) Uani 1 1 d . . . . . C19 C 0.3567(4) 0.5662(9) 0.2820(6) 0.037(2) Uani 1 1 d . . . . . O6 O 0.0379(3) -0.3601(8) -0.0287(5) 0.057(2) Uani 1 1 d . . . . . O9 O 0.7317(4) -0.0986(12) 0.7309(7) 0.081(3) Uani 1 1 d G . . . . H9A H 0.716876 -0.052224 0.690136 0.122 Uiso 1 1 d G U . . . H9B H 0.728770 -0.069121 0.764701 0.122 Uiso 1 1 d G U . . . C8 C 0.2348(4) -0.0598(9) 0.1059(6) 0.034(2) Uani 1 1 d . . . . . C5 C 0.1753(4) -0.0896(10) 0.0626(5) 0.036(2) Uani 1 1 d . . . . . C1 C 0.0003(4) -0.2941(10) -0.0448(6) 0.040(2) Uani 1 1 d . . . . . O4 O 0.4806(3) 0.0750(9) 0.3989(5) 0.064(3) Uani 1 1 d . . . . . C4 C 0.1616(4) -0.1360(12) 0.1076(6) 0.047(3) Uani 1 1 d . . . . . H4 H 0.189628 -0.151502 0.163638 0.056 Uiso 1 1 calc R U . . . C12 C 0.2498(5) 0.0385(10) 0.0892(7) 0.047(3) Uani 1 1 d . . . . . H12 H 0.222612 0.085826 0.044644 0.056 Uiso 1 1 calc R U . . . N3 N 0.4706(5) 0.3713(14) 0.3666(7) 0.085(4) Uani 1 1 d . . . . . O2 O 0.5733(5) 0.0070(10) 0.4008(6) 0.080(3) Uani 1 1 d . . . . . H2A H 0.568748 0.059876 0.362081 0.120 Uiso 1 1 d R U . . . H2B H 0.577017 -0.068342 0.385134 0.120 Uiso 1 1 d R U . . . C11 C 0.3061(5) 0.0687(10) 0.1391(7) 0.044(3) Uani 1 1 d . . . . . H11 H 0.316594 0.137385 0.128507 0.053 Uiso 1 1 calc R U . . . C16 C 0.3679(6) 0.3734(13) 0.1467(7) 0.060(3) Uani 1 1 d . . . . . C9 C 0.2779(4) -0.1381(10) 0.1701(6) 0.041(2) Uani 1 1 d . . . . . H9 H 0.268729 -0.209952 0.179569 0.049 Uiso 1 1 calc R U . . . C10 C 0.3331(4) -0.1026(11) 0.2169(6) 0.047(3) Uani 1 1 d . . . . . H10 H 0.361649 -0.151212 0.258788 0.056 Uiso 1 1 calc R U . . . C18 C 0.4049(5) 0.5965(12) 0.2186(6) 0.049(3) Uani 1 1 d . . . . . C14 C 0.4302(4) 0.0479(9) 0.3494(7) 0.038(3) Uani 1 1 d . . . . . C2 C 0.0078(4) -0.1673(10) -0.0496(7) 0.046(3) Uani 1 1 d . . . . . H2C H -0.017611 -0.143321 -0.107141 0.056 Uiso 1 1 calc R U . . . H2D H -0.002222 -0.123839 -0.021555 0.056 Uiso 1 1 calc R U . . . C20 C 0.4288(6) 0.4106(10) 0.3089(8) 0.050(3) Uani 1 1 d . . . . . N5 N 0.3729(5) 0.3109(11) 0.1094(7) 0.073(3) Uani 1 1 d . . . . . C7 C 0.0780(5) -0.0935(13) -0.0573(6) 0.054(3) Uani 1 1 d . . . . . H7 H 0.049770 -0.082531 -0.113879 0.065 Uiso 1 1 calc R U . . . C3 C 0.1071(5) -0.1589(11) 0.0694(6) 0.048(3) Uani 1 1 d . . . . . H3 H 0.097959 -0.190290 0.099687 0.058 Uiso 1 1 calc R U . . . N4 N 0.4294(6) 0.6830(13) 0.2241(7) 0.081(4) Uani 1 1 d . . . . . C13 C 0.4046(5) 0.0372(13) 0.2585(7) 0.058(4) Uani 1 1 d . . . . . H13A H 0.407055 0.112867 0.239980 0.069 Uiso 1 1 calc R U . . . H13B H 0.426537 -0.018622 0.255202 0.069 Uiso 1 1 calc R U . . . C6 C 0.1309(5) -0.0660(12) -0.0209(7) 0.063(4) Uani 1 1 d . . . . . H6 H 0.138510 -0.030057 -0.051907 0.075 Uiso 1 1 calc R U . . . C15 C 0.3157(6) 0.3630(14) 0.2081(7) 0.067(4) Uani 1 1 d . . . . . N6 N 0.2577(7) 0.5909(19) 0.0615(8) 0.126(7) Uani 1 1 d . . . . . C17 C 0.2970(6) 0.5435(13) 0.1187(8) 0.063(4) Uani 1 1 d . . . . . N1 N 0.2835(6) 0.2973(14) 0.2007(8) 0.084(4) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy3 0.0288(4) 0.0396(5) 0.0320(4) 0.00227(18) 0.0170(3) 0.00191(18) Co02 0.0450(9) 0.0394(9) 0.0330(7) 0.0021(6) 0.0276(7) -0.0011(6) O3 0.046(5) 0.066(6) 0.038(4) 0.005(4) 0.026(4) 0.000(4) N8 0.032(4) 0.037(5) 0.033(4) 0.001(4) 0.017(4) 0.002(4) O7 0.045(4) 0.053(5) 0.060(5) -0.019(4) 0.034(4) -0.015(4) O5 0.043(5) 0.086(8) 0.089(6) 0.040(6) 0.039(5) 0.012(5) O1 0.038(4) 0.065(6) 0.066(5) 0.005(4) 0.033(4) -0.010(4) O8 0.056(5) 0.065(7) 0.076(6) 0.002(4) 0.050(5) 0.009(4) N7 0.037(5) 0.052(6) 0.035(5) 0.000(4) 0.022(4) -0.008(5) N2 0.053(6) 0.064(8) 0.063(6) -0.019(6) 0.039(6) -0.007(5) C19 0.032(5) 0.038(7) 0.036(5) 0.005(4) 0.019(5) 0.008(4) O6 0.039(4) 0.069(6) 0.064(5) 0.002(4) 0.035(4) -0.003(4) O9 0.055(6) 0.110(9) 0.076(7) 0.022(7) 0.042(6) 0.008(6) C8 0.031(5) 0.040(7) 0.022(4) -0.010(4) 0.013(4) -0.005(4) C5 0.032(5) 0.043(6) 0.023(4) -0.007(4) 0.014(4) -0.008(5) C1 0.031(5) 0.043(7) 0.036(5) 0.004(5) 0.017(4) -0.006(5) O4 0.024(4) 0.087(7) 0.044(4) 0.016(4) 0.005(4) -0.004(4) C4 0.034(5) 0.078(9) 0.021(4) 0.002(5) 0.014(4) -0.007(5) C12 0.049(7) 0.044(8) 0.037(6) 0.006(5) 0.024(5) -0.009(5) N3 0.066(7) 0.120(13) 0.067(7) 0.042(8) 0.042(6) 0.052(8) O2 0.114(9) 0.070(7) 0.066(6) 0.002(6) 0.063(7) -0.002(7) C11 0.050(7) 0.047(8) 0.036(6) 0.001(5) 0.027(5) -0.014(5) C16 0.077(8) 0.066(10) 0.051(7) 0.016(6) 0.048(7) -0.001(7) C9 0.034(5) 0.040(7) 0.036(5) -0.003(5) 0.018(4) -0.008(5) C10 0.037(6) 0.051(8) 0.044(6) 0.010(5) 0.023(5) 0.001(5) C18 0.053(7) 0.056(8) 0.038(6) 0.006(5) 0.030(5) 0.005(6) C14 0.032(6) 0.037(7) 0.038(6) 0.007(4) 0.019(5) 0.003(4) C2 0.030(5) 0.044(7) 0.053(6) 0.005(5) 0.021(5) 0.005(5) C20 0.092(10) 0.024(6) 0.059(7) 0.003(5) 0.060(8) 0.012(6) N5 0.123(10) 0.062(8) 0.074(7) -0.011(6) 0.081(8) -0.003(7) C7 0.040(6) 0.080(9) 0.032(5) 0.013(6) 0.018(5) -0.008(6) C3 0.063(7) 0.054(8) 0.043(6) -0.003(5) 0.041(6) -0.007(6) N4 0.087(8) 0.089(10) 0.075(8) -0.005(7) 0.055(7) -0.033(8) C13 0.037(6) 0.093(12) 0.048(7) -0.011(6) 0.029(6) -0.018(6) C6 0.041(7) 0.098(12) 0.033(6) 0.020(6) 0.016(5) -0.018(6) C15 0.088(9) 0.087(11) 0.053(7) -0.032(7) 0.056(7) -0.043(8) N6 0.102(12) 0.21(2) 0.040(7) 0.016(10) 0.035(8) 0.044(13) C17 0.066(9) 0.085(12) 0.042(7) -0.003(6) 0.036(7) -0.006(7) N1 0.086(4) 0.086(4) 0.083(4) -0.0010(19) 0.056(3) -0.003(2) 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' Co Co 0.3494 0.9721 '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' 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 _geom_angle_publ_flag O3 Dy3 O5 142.8(3) 5_656 . ? O7 Dy3 O3 79.0(3) . 5_656 ? O7 Dy3 O5 71.7(3) . . ? O1 Dy3 O3 72.9(3) 4 5_656 ? O1 Dy3 O7 73.9(3) 4 . ? O1 Dy3 O5 77.3(3) 4 . ? O1 Dy3 O8 135.3(3) 4 . ? O1 Dy3 O6 118.9(3) 4 8_546 ? O1 Dy3 O2 146.2(4) 4 . ? O8 Dy3 O3 74.1(3) . 5_656 ? O8 Dy3 O7 70.8(3) . . ? O8 Dy3 O5 115.3(3) . . ? O6 Dy3 O3 75.3(3) 8_546 5_656 ? O6 Dy3 O7 145.3(3) 8_546 . ? O6 Dy3 O5 140.2(3) 8_546 . ? O6 Dy3 O8 80.0(3) 8_546 . ? O4 Dy3 O3 118.0(3) . 5_656 ? O4 Dy3 O7 139.4(3) . . ? O4 Dy3 O5 75.0(3) . . ? O4 Dy3 O1 76.8(3) . 4 ? O4 Dy3 O8 146.7(4) . . ? O4 Dy3 O6 74.4(3) . 8_546 ? O4 Dy3 O2 79.2(4) . . ? O2 Dy3 O3 140.3(4) . 5_656 ? O2 Dy3 O7 112.1(3) . . ? O2 Dy3 O5 73.8(4) . . ? O2 Dy3 O8 74.3(4) . . ? O2 Dy3 O6 76.0(3) . 8_546 ? C19 Co02 C16 176.4(5) . . ? C18 Co02 C19 88.3(5) . . ? C18 Co02 C16 94.4(5) . . ? C18 Co02 C20 88.3(5) . . ? C20 Co02 C19 88.3(4) . . ? C20 Co02 C16 89.3(5) . . ? C15 Co02 C19 88.3(5) . . ? C15 Co02 C16 89.2(5) . . ? C15 Co02 C18 175.7(6) . . ? C15 Co02 C20 94.1(6) . . ? C17 Co02 C19 91.6(5) . . ? C17 Co02 C16 90.8(6) . . ? C17 Co02 C18 89.8(6) . . ? C17 Co02 C20 178.1(6) . . ? C17 Co02 C15 87.9(6) . . ? C14 O3 Dy3 126.1(7) . 5_656 ? C7 N8 C2 122.1(9) . . ? C7 N8 C3 120.3(9) . . ? C3 N8 C2 117.6(9) . . ? Dy3 O7 H7A 104.3 . . ? Dy3 O7 H7B 104.5 . . ? H7A O7 H7B 104.4 . . ? Dy3 O5 H5A 110.3 . . ? Dy3 O5 H5B 110.8 . . ? H5A O5 H5B 103.5 . . ? C1 O1 Dy3 137.5(7) . 4_545 ? Dy3 O8 H8A 110.1 . . ? Dy3 O8 H8B 110.4 . . ? H8A O8 H8B 103.5 . . ? C11 N7 C13 119.4(10) . . ? C10 N7 C11 121.5(9) . . ? C10 N7 C13 119.0(10) . . ? N2 C19 Co02 177.9(11) . . ? C1 O6 Dy3 145.1(7) . 8_445 ? H9A O9 H9B 109.4 . . ? C12 C8 C5 122.5(10) . . ? C12 C8 C9 119.4(10) . . ? C9 C8 C5 118.1(9) . . ? C4 C5 C8 119.0(8) . . ? C4 C5 C6 117.0(9) . . ? C6 C5 C8 123.9(9) . . ? O1 C1 C2 114.2(10) . . ? O6 C1 O1 129.3(11) . . ? O6 C1 C2 116.5(9) . . ? C14 O4 Dy3 156.9(8) . . ? C5 C4 H4 120.2 . . ? C3 C4 C5 119.5(9) . . ? C3 C4 H4 120.2 . . ? C8 C12 H12 120.3 . . ? C8 C12 C11 119.4(11) . . ? C11 C12 H12 120.3 . . ? Dy3 O2 H2A 128.0 . . ? Dy3 O2 H2B 127.8 . . ? H2A O2 H2B 104.3 . . ? N7 C11 C12 120.5(10) . . ? N7 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? N5 C16 Co02 177.7(13) . . ? C8 C9 H9 121.1 . . ? C10 C9 C8 117.7(10) . . ? C10 C9 H9 121.2 . . ? N7 C10 C9 121.0(10) . . ? N7 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? N4 C18 Co02 172.1(12) . . ? O3 C14 C13 118.7(9) . . ? O4 C14 O3 126.0(11) . . ? O4 C14 C13 115.2(10) . . ? N8 C2 C1 112.9(9) . . ? N8 C2 H2C 109.0 . . ? N8 C2 H2D 109.0 . . ? C1 C2 H2C 109.0 . . ? C1 C2 H2D 109.0 . . ? H2C C2 H2D 107.8 . . ? N3 C20 Co02 177.9(11) . . ? N8 C7 H7 120.0 . . ? C6 C7 N8 119.9(10) . . ? C6 C7 H7 120.0 . . ? N8 C3 H3 119.5 . . ? C4 C3 N8 121.1(9) . . ? C4 C3 H3 119.5 . . ? N7 C13 C14 113.1(9) . . ? N7 C13 H13A 109.0 . . ? N7 C13 H13B 109.0 . . ? C14 C13 H13A 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C5 C6 H6 119.0 . . ? C7 C6 C5 122.1(10) . . ? C7 C6 H6 119.0 . . ? N1 C15 Co02 175.2(16) . . ? N6 C17 Co02 176.9(17) . . ? 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 Dy3 O3 2.394(7) 5_656 ? Dy3 O7 2.389(8) . ? Dy3 O5 2.412(9) . ? Dy3 O1 2.346(7) 4 ? Dy3 O8 2.387(8) . ? Dy3 O6 2.359(9) 8_546 ? Dy3 O4 2.314(8) . ? Dy3 O2 2.355(9) . ? Co02 C19 1.880(11) . ? Co02 C16 1.933(14) . ? Co02 C18 1.878(13) . ? Co02 C20 1.880(13) . ? Co02 C15 1.875(13) . ? Co02 C17 1.862(15) . ? O3 C14 1.249(13) . ? N8 C2 1.470(13) . ? N8 C7 1.333(13) . ? N8 C3 1.360(13) . ? O7 H7A 0.8494 . ? O7 H7B 0.8496 . ? O5 H5A 0.8724 . ? O5 H5B 0.8741 . ? O1 C1 1.248(12) . ? O8 H8A 0.8705 . ? O8 H8B 0.8710 . ? N7 C11 1.353(15) . ? N7 C10 1.318(16) . ? N7 C13 1.463(14) . ? N2 C19 1.159(13) . ? O6 C1 1.240(14) . ? O9 H9A 0.8497 . ? O9 H9B 0.8497 . ? C8 C5 1.484(14) . ? C8 C12 1.346(15) . ? C8 C9 1.444(15) . ? C5 C4 1.381(14) . ? C5 C6 1.397(15) . ? C1 C2 1.475(16) . ? O4 C14 1.237(13) . ? C4 H4 0.9300 . ? C4 C3 1.356(15) . ? C12 H12 0.9300 . ? C12 C11 1.385(16) . ? N3 C20 1.155(16) . ? O2 H2A 0.9535 . ? O2 H2B 0.9544 . ? C11 H11 0.9300 . ? C16 N5 1.148(16) . ? C9 H9 0.9300 . ? C9 C10 1.380(14) . ? C10 H10 0.9300 . ? C18 N4 1.205(17) . ? C14 C13 1.544(16) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C7 H7 0.9300 . ? C7 C6 1.330(17) . ? C3 H3 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C6 H6 0.9300 . ? C15 N1 1.182(18) . ? N6 C17 1.16(2) . ? 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 Dy3 O3 C14 O4 -37.9(15) 5_656 . . . ? Dy3 O3 C14 C13 145.9(8) 5_656 . . . ? Dy3 O1 C1 O6 43.8(18) 4_545 . . . ? Dy3 O1 C1 C2 -139.4(9) 4_545 . . . ? Dy3 O6 C1 O1 -16(2) 8_445 . . . ? Dy3 O6 C1 C2 167.2(9) 8_445 . . . ? Dy3 O4 C14 O3 66(3) . . . . ? Dy3 O4 C14 C13 -118(2) . . . . ? O3 C14 C13 N7 -6.4(16) . . . . ? N8 C7 C6 C5 5(2) . . . . ? O1 C1 C2 N8 167.1(9) . . . . ? O6 C1 C2 N8 -15.7(14) . . . . ? C8 C5 C4 C3 177.2(11) . . . . ? C8 C5 C6 C7 -179.6(13) . . . . ? C8 C12 C11 N7 1.3(17) . . . . ? C8 C9 C10 N7 -0.3(16) . . . . ? C5 C8 C12 C11 171.7(10) . . . . ? C5 C8 C9 C10 -172.2(9) . . . . ? C5 C4 C3 N8 -0.1(19) . . . . ? O4 C14 C13 N7 177.0(11) . . . . ? C4 C5 C6 C7 -4(2) . . . . ? C12 C8 C5 C4 -139.0(12) . . . . ? C12 C8 C5 C6 36.3(17) . . . . ? C12 C8 C9 C10 5.8(15) . . . . ? C11 N7 C10 C9 -4.8(17) . . . . ? C11 N7 C13 C14 120.9(11) . . . . ? C9 C8 C5 C4 38.9(15) . . . . ? C9 C8 C5 C6 -145.8(12) . . . . ? C9 C8 C12 C11 -6.2(16) . . . . ? C10 N7 C11 C12 4.4(17) . . . . ? C10 N7 C13 C14 -59.0(15) . . . . ? C2 N8 C7 C6 179.3(13) . . . . ? C2 N8 C3 C4 178.3(11) . . . . ? C7 N8 C2 C1 115.6(12) . . . . ? C7 N8 C3 C4 1.1(18) . . . . ? C3 N8 C2 C1 -61.6(13) . . . . ? C3 N8 C7 C6 -4(2) . . . . ? C13 N7 C11 C12 -175.5(11) . . . . ? C13 N7 C10 C9 175.1(10) . . . . ? C6 C5 C4 C3 1.5(18) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.207 0.250 45.4 15.0 ? 2 0.000 0.207 0.750 45.4 15.0 ? 3 0.000 0.377 0.250 11.3 15.2 ? 4 0.000 0.623 0.750 11.3 15.3 ? 5 0.159 0.305 0.424 20.0 15.2 ? 6 0.159 0.695 0.924 20.0 15.2 ? 7 0.250 0.250 1.000 40.2 1.4 ? 8 0.250 0.750 0.500 40.2 1.4 ? 9 0.341 0.195 0.576 20.0 15.7 ? 10 0.341 0.805 0.076 20.0 15.7 ? 11 0.500 0.293 0.250 45.4 15.0 ? 12 0.500 0.707 0.750 45.4 15.0 ? 13 0.500 0.123 0.750 11.3 15.3 ? 14 0.500 0.877 0.250 11.3 15.2 ? 15 0.659 0.195 0.924 20.0 15.2 ? 16 0.659 0.805 0.424 20.0 15.2 ? 17 0.750 0.250 0.500 40.2 1.4 ? 18 0.750 0.750 1.000 40.2 1.4 ? 19 0.841 0.305 0.076 20.0 15.7 ? 20 0.841 0.695 0.576 20.0 15.7 ?