#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:30:59 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270479 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060987.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_7060987 loop_ _publ_author_name 'Liu, Cai-Ming' 'Hao, Xiang' _publ_section_title ; Magnetic relaxation in two chain-like Zn2Dy2 Schiff base coordination polymers bridged by tetraoxolene and its one-electron reduced radical ; _journal_issue 42 _journal_name_full 'New Journal of Chemistry' _journal_page_first 19868 _journal_page_last 19875 _journal_paper_doi 10.1039/D1NJ04299H _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C53 H52 Br4 Dy2 N5 O22 Zn2, 0.5(Cl O4)' _chemical_formula_sum 'C53 H52 Br4 Cl0.5 Dy2 N5 O24 Zn2' _chemical_formula_weight 1936.10 _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 _atom_sites_solution_primary iterative _audit_creation_date 2021-09-02 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-09-03 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _cell_angle_alpha 89.624(2) _cell_angle_beta 80.033(2) _cell_angle_gamma 79.843(2) _cell_formula_units_Z 2 _cell_length_a 11.5601(2) _cell_length_b 14.8370(3) _cell_length_c 20.0015(5) _cell_measurement_reflns_used 32301 _cell_measurement_temperature 169.9(5) _cell_measurement_theta_max 33.2380 _cell_measurement_theta_min 1.7040 _cell_volume 3324.86(13) _computing_cell_refinement 'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)' _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 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 169.9(5) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.937 _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 -105.00 65.00 0.50 6.00 -- -20.00 45.00 0.00 340 2 \w -105.00 65.00 0.50 6.00 -- -20.00 45.00 90.00 340 3 \w -105.00 65.00 0.50 6.00 -- -20.00 45.00 180.00 340 4 \w -97.00 73.00 0.50 6.00 -- -8.00 45.00 270.00 340 5 \w -125.00 45.00 0.50 6.00 -- -40.00 45.00 0.00 340 6 \w -125.00 45.00 0.50 6.00 -- -40.00 45.00 45.00 340 7 \w -125.00 45.00 0.50 6.00 -- -40.00 45.00 135.00 340 8 \w -125.00 45.00 0.50 6.00 -- -40.00 45.00 205.00 340 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC10 (RCD3): fixed-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0204413000 _diffrn_orient_matrix_UB_12 0.0017006000 _diffrn_orient_matrix_UB_13 -0.0315167000 _diffrn_orient_matrix_UB_21 0.0530234000 _diffrn_orient_matrix_UB_22 0.0146891000 _diffrn_orient_matrix_UB_23 -0.0159036000 _diffrn_orient_matrix_UB_31 0.0279029000 _diffrn_orient_matrix_UB_32 -0.0462771000 _diffrn_orient_matrix_UB_33 -0.0071406000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_unetI/netI 0.1198 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.937 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 180466 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.937 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 42.292 _diffrn_reflns_theta_min 1.716 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 5.437 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.934 _exptl_crystal_description block _exptl_crystal_F_000 1875 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 4.487 _refine_diff_density_min -1.554 _refine_diff_density_rms 0.207 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 846 _refine_ls_number_reflns 44285 _refine_ls_number_restraints 39 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0821 _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^)+(0.0600P)^2^+9.0706P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1518 _refine_ls_wR_factor_ref 0.1755 _reflns_Friedel_coverage 0.000 _reflns_number_gt 22907 _reflns_number_total 44285 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04299h2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7060986--7060987.cif.' _cod_original_cell_volume 3324.86(12) _cod_original_formula_sum 'C53 H52 Br4 Cl0.50 Dy2 N5 O24 Zn2' _cod_database_code 7060987 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHNOBrZnDy _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. ; _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _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 C(H,H,H) groups, All O(H) groups 2. Restrained distances O17-H17 0.85 with sigma of 0.01 O18-H18 0.85 with sigma of 0.01 O22-H22 0.85 with sigma of 0.01 C88-H17 1.890315 with sigma of 0.02 Zn2-H17 2.7107 with sigma of 0.02 C87-H18 1.919971 with sigma of 0.02 Dy2-H18 3.114065 with sigma of 0.02 C89-H22 1.867615 with sigma of 0.02 Zn1-H22 2.780913 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O25) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4. Others Fixed Sof: Cl1(0.5) O25(0.5) O26(0.5) O27(0.5) O28(0.5) 5.a : Cl1(O25,O26,O27,O28) 5.b Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B) 5.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16), C22(H22A), C23(H23), C24(H24), C27(H27), C31(H31), C33(H33), C34(H34), C35(H35) 5.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B, H38C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL mx9346_a.res in P-1 2.res created by SHELXL-2018/3 at 18:13:04 on 02-Sep-2021 REM Old TITL mx9346 in P-1 REM SHELXT solution in P-1: R1 0.151, Rweak 0.007, Alpha 0.072 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C120 N17 O38 Zn1 Br10 Dy4 CELL 0.71073 11.5601 14.837 20.0015 89.624 80.033 79.843 ZERR 2 0.0002 0.0003 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H Br Cl Dy N O Zn UNIT 106 104 8 1 4 10 48 4 DFIX 0.85 0.01 O17 H17 DFIX 0.85 0.01 O18 H18 DFIX 0.85 0.01 O22 H22 DANG 1.890315 0.02 C88 H17 DANG 2.7107 0.02 Zn2 H17 DANG 1.919971 0.02 C87 H18 DANG 3.114065 0.02 Dy2 H18 DANG 1.867615 0.02 C89 H22 DANG 2.780913 0.02 Zn1 H22 ISOR 0.005 0.01 O25 Cl1 O27 O26 O28 L.S. 20 PLAN 8 CONF BOND LIST 4 MORE -1 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.060000 9.070600 FVAR 0.17083 DY1 5 0.144473 0.895167 0.213790 11.00000 0.01674 0.01724 = 0.03145 0.00119 -0.00861 -0.00233 DY2 5 0.524962 0.341787 0.250777 11.00000 0.01655 0.01742 = 0.04946 -0.00275 -0.01402 -0.00129 BR1 3 0.567680 0.704434 0.262688 11.00000 0.03390 0.02502 = 0.09651 0.00975 -0.03919 -0.01140 BR2 3 0.102402 0.534133 0.198381 11.00000 0.02645 0.02675 = 0.06811 0.00465 -0.02243 -0.01033 BR3 3 0.270389 1.112318 0.399915 11.00000 0.04003 0.04759 = 0.02920 0.00137 -0.00958 -0.01476 BR4 3 0.388121 1.130770 0.063176 11.00000 0.05034 0.08416 = 0.02891 0.00779 -0.00954 -0.04017 ZN1 8 -0.138727 0.905007 0.181049 11.00000 0.01740 0.03178 = 0.03331 0.00167 -0.00734 -0.00268 ZN2 8 0.814452 0.350983 0.279864 11.00000 0.01460 0.02781 = 0.03239 -0.00191 -0.00730 -0.00187 O1 7 0.558610 0.392760 0.131135 11.00000 0.04865 0.03599 = 0.04054 0.01546 -0.02814 -0.01817 O2 7 0.722736 0.344219 0.202685 11.00000 0.02543 0.02699 = 0.02381 0.00270 -0.00556 -0.00506 O3 7 0.645434 0.349059 0.330820 11.00000 0.01703 0.02994 = 0.02681 -0.00195 -0.00403 -0.00410 O4 7 0.420523 0.399444 0.371326 11.00000 0.01793 0.04213 = 0.04569 -0.01734 0.00407 -0.00794 O5 7 0.108008 0.835652 0.334348 11.00000 0.03533 0.03825 = 0.03562 0.01095 -0.01744 -0.01112 O6 7 -0.049898 0.886635 0.260531 11.00000 0.02287 0.02779 = 0.03005 0.00919 -0.00781 -0.00658 O7 7 0.031419 0.900148 0.131263 11.00000 0.01809 0.02880 = 0.02799 -0.00060 -0.00616 -0.00349 O8 7 0.253944 0.832714 0.094154 11.00000 0.02218 0.02940 = 0.03665 -0.00556 -0.00071 -0.00446 O9 7 0.529227 0.504196 0.256853 11.00000 0.02086 0.01552 = 0.05319 -0.00124 -0.01505 -0.00044 O10 7 0.344908 0.436120 0.234427 11.00000 0.02324 0.01667 = 0.07476 0.00111 -0.01981 -0.00334 O11 7 0.323937 0.801398 0.229803 11.00000 0.02302 0.01632 = 0.04873 0.00291 -0.01388 -0.00329 O12 7 0.141064 0.733571 0.205919 11.00000 0.01957 0.02216 = 0.04428 0.00174 -0.01180 -0.00363 O13 7 0.221579 0.985770 0.287327 11.00000 0.02632 0.02292 = 0.03432 0.00439 -0.00901 -0.00590 O14 7 0.261110 0.996752 0.155968 11.00000 0.02512 0.02696 = 0.03146 -0.00641 -0.00344 -0.01108 O15 7 0.389051 1.249505 0.305415 11.00000 0.02071 0.02259 = 0.04010 -0.00970 -0.00693 -0.00305 O16 7 0.456592 1.245174 0.175242 11.00000 0.02510 0.02626 = 0.03932 0.00638 -0.00962 -0.01154 O17 7 0.778199 0.496536 0.280364 11.00000 0.02895 0.02392 = 0.05238 -0.00249 -0.01807 -0.00152 H17 2 0.718834 0.526038 0.264546 11.00000 -1.50000 O18 7 0.627616 0.181784 0.264842 11.00000 0.02149 0.02650 = 0.04237 -0.00078 -0.00927 0.00368 H18 2 0.692948 0.155285 0.239628 11.00000 -1.50000 O19 7 0.027175 1.055027 0.224852 11.00000 0.01913 0.02067 = 0.05474 -0.00293 -0.00869 0.00022 O20 7 -0.155487 1.056607 0.207909 11.00000 0.02674 0.02835 = 0.03975 0.00405 -0.01352 -0.00508 O21 7 -0.115073 1.166171 0.263808 11.00000 0.03329 0.02443 = 0.09166 -0.01850 -0.00681 -0.00215 O22 7 -0.103149 0.752480 0.172608 11.00000 0.04307 0.02803 = 0.06956 -0.00723 -0.01988 -0.00645 H22 2 -0.052980 0.719413 0.193689 11.00000 -1.50000 N1 6 0.971086 0.332376 0.212086 11.00000 0.01878 0.02846 = 0.05349 -0.00515 -0.00054 -0.00609 N2 6 0.878586 0.315072 0.366671 11.00000 0.02846 0.02387 = 0.04750 0.00121 -0.01994 0.00005 N3 6 -0.298113 0.907843 0.245377 11.00000 0.02210 0.02331 = 0.05049 -0.00032 -0.00470 -0.00435 N4 6 -0.200887 0.939558 0.093527 11.00000 0.02520 0.02824 = 0.05114 -0.00431 -0.02070 -0.00373 N5 6 -0.080203 1.092575 0.232248 11.00000 0.02246 0.01899 = 0.03298 0.00339 -0.00516 -0.00264 C1 1 0.465593 0.407553 0.087532 11.00000 0.08981 0.07036 = 0.08414 0.02427 -0.05093 -0.01051 AFIX 137 H1A 2 0.391130 0.397177 0.113243 11.00000 -1.50000 H1B 2 0.488929 0.365724 0.049192 11.00000 -1.50000 H1C 2 0.456569 0.469325 0.071965 11.00000 -1.50000 AFIX 0 C2 1 0.672767 0.401648 0.100557 11.00000 0.05587 0.04666 = 0.03343 0.01552 -0.01686 -0.02323 C3 1 0.703959 0.429779 0.035202 11.00000 0.09565 0.12258 = 0.05051 0.04999 -0.03699 -0.05911 AFIX 43 H3 2 0.646181 0.444814 0.007949 11.00000 -1.20000 AFIX 0 C4 1 0.822482 0.435602 0.010117 11.00000 0.11713 0.16976 = 0.05725 0.06349 -0.02128 -0.07949 AFIX 43 H4 2 0.843141 0.456344 -0.033554 11.00000 -1.20000 AFIX 0 C5 1 0.907463 0.411529 0.048406 11.00000 0.08373 0.11749 = 0.04344 0.02546 0.00495 -0.05700 AFIX 43 H5 2 0.986497 0.414253 0.030413 11.00000 -1.20000 AFIX 0 C6 1 0.878278 0.382323 0.115248 11.00000 0.04606 0.05357 = 0.03509 0.00361 0.00211 -0.02237 C7 1 0.758692 0.376485 0.142005 11.00000 0.04029 0.03079 = 0.03127 0.00173 -0.00415 -0.01546 C8 1 0.977011 0.353227 0.150975 11.00000 0.02901 0.04238 = 0.05974 -0.00849 0.00527 -0.01291 AFIX 43 H8 2 1.053229 0.349661 0.125664 11.00000 -1.20000 AFIX 0 C9 1 1.084562 0.298502 0.235812 11.00000 0.01197 0.03342 = 0.08299 0.00038 -0.00252 0.00054 AFIX 23 H9A 2 1.148543 0.321339 0.206519 11.00000 -1.20000 H9B 2 1.101445 0.232159 0.231999 11.00000 -1.20000 AFIX 0 C10 1 1.082856 0.327188 0.308218 11.00000 0.02188 0.03355 = 0.10687 -0.01199 -0.02922 -0.00094 AFIX 23 H10A 2 1.164188 0.315971 0.316758 11.00000 -1.20000 H10B 2 1.053695 0.392636 0.313299 11.00000 -1.20000 AFIX 0 C11 1 1.008042 0.279751 0.361227 11.00000 0.02844 0.03709 = 0.07570 0.00187 -0.03144 0.00276 AFIX 23 H11A 2 1.023614 0.214679 0.350207 11.00000 -1.20000 H11B 2 1.031235 0.287642 0.404866 11.00000 -1.20000 AFIX 0 C12 1 0.817163 0.323560 0.425407 11.00000 0.05182 0.03511 = 0.03593 0.00136 -0.02711 -0.00103 AFIX 43 H12 2 0.859320 0.311413 0.461020 11.00000 -1.20000 AFIX 0 C13 1 0.688288 0.350035 0.444562 11.00000 0.04844 0.03070 = 0.02902 -0.00006 -0.01057 -0.00052 C14 1 0.640044 0.361875 0.514491 11.00000 0.08807 0.03981 = 0.02928 0.00062 -0.01621 -0.00306 AFIX 43 H14 2 0.690898 0.355563 0.546181 11.00000 -1.20000 AFIX 0 C15 1 0.519296 0.382527 0.536026 11.00000 0.07908 0.06203 = 0.03249 -0.00326 0.00964 -0.00597 AFIX 43 H15 2 0.489078 0.388045 0.582316 11.00000 -1.20000 AFIX 0 C16 1 0.441751 0.395280 0.490413 11.00000 0.05730 0.05415 = 0.03729 -0.01086 0.01503 -0.01351 AFIX 43 H16 2 0.359839 0.410049 0.505571 11.00000 -1.20000 AFIX 0 C17 1 0.487073 0.385882 0.422146 11.00000 0.03651 0.03021 = 0.04087 -0.00723 0.00640 -0.01279 C18 1 0.610691 0.361683 0.397420 11.00000 0.03237 0.01932 = 0.02895 -0.00189 0.00146 -0.00452 C19 1 0.292654 0.418752 0.393864 11.00000 0.02084 0.06014 = 0.07346 -0.03197 0.01437 -0.01069 AFIX 137 H19A 2 0.253385 0.425197 0.355109 11.00000 -1.50000 H19B 2 0.271274 0.474560 0.420651 11.00000 -1.50000 H19C 2 0.268432 0.369312 0.420791 11.00000 -1.50000 AFIX 0 C20 1 0.193493 0.819746 0.379452 11.00000 0.05630 0.06196 = 0.03296 0.01963 -0.02824 -0.01181 AFIX 137 H20A 2 0.215369 0.755099 0.385422 11.00000 -1.50000 H20B 2 0.158933 0.849320 0.422627 11.00000 -1.50000 H20C 2 0.263221 0.844203 0.360405 11.00000 -1.50000 AFIX 0 C21 1 -0.004201 0.816089 0.358652 11.00000 0.04801 0.02960 = 0.02814 0.00288 -0.01203 -0.00982 C22 1 -0.034930 0.770594 0.418298 11.00000 0.06107 0.04406 = 0.03442 0.00966 -0.01278 -0.01831 AFIX 43 H22A 2 0.022570 0.748360 0.444445 11.00000 -1.20000 AFIX 0 C23 1 -0.152506 0.758618 0.438532 11.00000 0.07284 0.05180 = 0.03455 0.01109 -0.00003 -0.02594 AFIX 43 H23 2 -0.173388 0.726863 0.477737 11.00000 -1.20000 AFIX 0 C24 1 -0.236878 0.793263 0.401080 11.00000 0.05230 0.04167 = 0.03716 -0.00407 0.01040 -0.02196 AFIX 43 H24 2 -0.315854 0.787501 0.416375 11.00000 -1.20000 AFIX 0 C25 1 -0.207336 0.837871 0.339389 11.00000 0.03757 0.02635 = 0.03504 -0.00262 0.00416 -0.01012 C26 1 -0.087926 0.847520 0.317564 11.00000 0.03361 0.02105 = 0.02443 0.00205 -0.00342 -0.00632 C27 1 -0.305530 0.875494 0.304926 11.00000 0.02591 0.02403 = 0.05513 -0.00864 0.00273 -0.00830 AFIX 43 H27 2 -0.382106 0.876018 0.328945 11.00000 -1.20000 AFIX 0 C28 1 -0.410969 0.946281 0.222410 11.00000 0.01600 0.02933 = 0.07358 -0.00184 -0.00424 -0.00210 AFIX 23 H28A 2 -0.428292 1.011968 0.230995 11.00000 -1.20000 H28B 2 -0.475375 0.920302 0.248602 11.00000 -1.20000 AFIX 0 C29 1 -0.406305 0.927157 0.147436 11.00000 0.02054 0.03173 = 0.08565 -0.01206 -0.02083 -0.00255 AFIX 23 H29A 2 -0.378088 0.862180 0.138130 11.00000 -1.20000 H29B 2 -0.486749 0.941615 0.137673 11.00000 -1.20000 AFIX 0 C30 1 -0.327614 0.979747 0.099836 11.00000 0.03142 0.03451 = 0.05961 -0.00659 -0.02851 0.00355 AFIX 23 H30A 2 -0.350417 0.980593 0.055359 11.00000 -1.20000 H30B 2 -0.340032 1.042577 0.116490 11.00000 -1.20000 AFIX 0 C31 1 -0.137376 0.927112 0.033955 11.00000 0.03813 0.02811 = 0.03538 -0.00287 -0.01969 -0.00292 AFIX 43 H31 2 -0.176230 0.943732 -0.002461 11.00000 -1.20000 AFIX 0 C32 1 -0.011066 0.889704 0.017859 11.00000 0.03881 0.02356 = 0.03066 -0.00161 -0.00940 -0.00566 C33 1 0.035672 0.866028 -0.051051 11.00000 0.05641 0.03302 = 0.02289 0.00311 -0.00978 -0.00491 AFIX 43 H33 2 -0.014741 0.873935 -0.082978 11.00000 -1.20000 AFIX 0 C34 1 0.154478 0.831561 -0.071243 11.00000 0.06832 0.03861 = 0.02046 -0.00028 -0.00052 -0.00054 AFIX 43 H34 2 0.184147 0.817088 -0.116871 11.00000 -1.20000 AFIX 0 C35 1 0.230842 0.818023 -0.024600 11.00000 0.04709 0.02876 = 0.03440 -0.00022 0.00704 -0.00313 AFIX 43 H35 2 0.311057 0.793095 -0.038457 11.00000 -1.20000 AFIX 0 C36 1 0.187041 0.841761 0.042413 11.00000 0.02874 0.02455 = 0.02793 0.00032 -0.00049 -0.00825 C37 1 0.066098 0.877831 0.065298 11.00000 0.03139 0.01678 = 0.02618 0.00138 -0.00539 -0.00653 C38 1 0.380761 0.810694 0.072822 11.00000 0.02205 0.07019 = 0.05466 -0.00187 0.00155 -0.00287 AFIX 137 H38A 2 0.405767 0.853101 0.039257 11.00000 -1.50000 H38B 2 0.401985 0.749593 0.053723 11.00000 -1.50000 H38C 2 0.419470 0.814638 0.111199 11.00000 -1.50000 AFIX 0 C39 1 0.435230 0.656660 0.245980 11.00000 0.02162 0.02000 = 0.05198 0.00171 -0.01801 -0.00549 C40 1 0.441945 0.561931 0.245768 11.00000 0.01815 0.01979 = 0.03684 -0.00118 -0.00859 -0.00160 C41 1 0.334347 0.521804 0.231662 11.00000 0.01907 0.02162 = 0.04363 0.00004 -0.00879 -0.00314 C42 1 0.233885 0.581645 0.217371 11.00000 0.01786 0.01989 = 0.04315 0.00149 -0.00882 -0.00432 C43 1 0.228249 0.675877 0.217290 11.00000 0.02011 0.01987 = 0.02861 0.00340 -0.00694 -0.00538 C44 1 0.335703 0.715353 0.231614 11.00000 0.01991 0.02057 = 0.03728 0.00179 -0.01078 -0.00348 C45 1 0.271447 1.050891 0.265380 11.00000 0.01513 0.01823 = 0.03376 0.00182 -0.00849 -0.00135 C46 1 0.306141 1.116274 0.304318 11.00000 0.01832 0.02189 = 0.02938 -0.00215 -0.00630 0.00006 C47 1 0.361773 1.185108 0.274669 11.00000 0.01633 0.01800 = 0.03272 -0.00152 -0.00880 -0.00217 C48 1 0.395295 1.186354 0.196963 11.00000 0.01762 0.02013 = 0.03710 0.00199 -0.01046 -0.00238 C49 1 0.355321 1.125283 0.158009 11.00000 0.02265 0.03064 = 0.02792 0.00017 -0.00696 -0.00839 C50 1 0.296100 1.057073 0.187693 11.00000 0.01328 0.02370 = 0.02982 -0.00454 -0.00397 -0.00144 C87 1 0.625118 0.141353 0.330852 11.00000 0.03660 0.03166 = 0.05024 0.00571 -0.01436 -0.00050 AFIX 137 H87A 2 0.644944 0.075887 0.325572 11.00000 -1.50000 H87B 2 0.546691 0.158202 0.357401 11.00000 -1.50000 H87C 2 0.682059 0.163100 0.353454 11.00000 -1.50000 AFIX 0 C88 1 0.807520 0.554609 0.329139 11.00000 0.03686 0.03886 = 0.06126 -0.02055 -0.01635 0.00084 AFIX 137 H88A 2 0.812167 0.613773 0.310239 11.00000 -1.50000 H88B 2 0.883119 0.528173 0.340875 11.00000 -1.50000 H88C 2 0.746995 0.560936 0.369106 11.00000 -1.50000 AFIX 0 C89 1 -0.126161 0.695675 0.122259 11.00000 0.07057 0.04820 = 0.09765 -0.02077 -0.04593 0.00289 AFIX 137 H89A 2 -0.058713 0.685063 0.085981 11.00000 -1.50000 H89B 2 -0.195448 0.724909 0.104920 11.00000 -1.50000 H89C 2 -0.140029 0.638280 0.141510 11.00000 -1.50000 AFIX 9 PART -1 CL1 4 0.004998 0.495555 0.509049 10.50000 0.03167 0.06024 = 0.05696 -0.02911 -0.00560 0.00305 O25 7 0.117559 0.483395 0.527338 10.50000 0.04637 0.12514 = 0.05616 -0.00860 -0.00964 -0.00557 O26 7 -0.065891 0.444824 0.549439 10.50000 0.08011 0.10515 = 0.18069 0.03771 0.01250 -0.00762 O27 7 0.013518 0.465536 0.445349 10.50000 0.15928 0.19522 = 0.16119 -0.05863 -0.07786 -0.02350 O28 7 -0.053023 0.585635 0.517990 10.50000 0.07040 0.05728 = 0.10784 0.00854 0.02119 0.00428 AFIX 0 HKLF 4 REM mx9346_a.res in P-1 REM wR2 = 0.1755, GooF = S = 1.018, Restrained GooF = 1.021 for all data REM R1 = 0.0821 for 22907 Fo > 4sig(Fo) and 0.1646 for all 44285 data REM 846 parameters refined using 39 restraints END WGHT 0.0599 9.0873 REM Highest difference peak 4.487, deepest hole -1.554, 1-sigma level 0.207 Q1 1 0.5396 0.3481 0.2179 11.00000 0.05 4.49 Q2 1 0.5379 0.3822 0.2590 11.00000 0.05 3.75 Q3 1 0.1259 0.8517 0.2175 11.00000 0.05 3.14 Q4 1 0.5789 0.6966 0.2272 11.00000 0.05 2.48 Q5 1 0.1595 0.9096 0.1794 11.00000 0.05 2.41 Q6 1 0.1205 0.8913 0.2505 11.00000 0.05 2.36 Q7 1 0.5168 0.2954 0.2545 11.00000 0.05 2.22 Q8 1 0.1575 0.8614 0.2424 11.00000 0.05 2.10 ; _shelx_res_checksum 99010 _shelx_fab_file ; -21 -9 1 4.4075 -0.8803 -21 -8 1 3.0276 -0.3878 -21 -8 2 4.8599 0.5029 -21 -7 1 -7.4207 -0.1799 -21 -7 2 -3.9622 -0.0913 -21 -6 1 1.3484 0.5172 -21 -6 2 5.4030 -0.0304 -21 -5 1 2.1595 0.5155 -21 -5 2 7.8521 0.0070 -21 -4 1 -3.4979 -0.0090 -21 -4 2 -2.9598 -0.4204 -21 -4 3 -7.3223 -0.5620 -21 -3 1 1.1257 0.7172 -21 -3 2 1.5717 0.3066 -21 -2 1 0.2581 -0.0274 -21 -2 2 0.6694 0.3373 -21 -1 1 0.4637 -0.7171 -20 -14 1 -3.2862 -0.4301 -20 -13 1 -3.4741 0.6099 -20 -13 2 7.1384 -0.0393 -20 -13 3 -2.2147 0.0328 -20 -13 4 4.6085 0.0732 -20 -12 1 -9.2237 0.6142 -20 -12 2 8.5321 -0.2711 -20 -12 3 -6.9005 0.3643 -20 -12 4 2.1920 0.1811 -20 -12 5 -3.9621 0.1118 -20 -11 1 -15.9027 0.2997 -20 -11 2 6.5416 -0.6668 -20 -11 3 -7.5115 0.2535 -20 -11 4 -0.0185 -0.3235 -20 -11 5 1.5414 -0.1142 -20 -11 6 -0.8629 0.0303 -20 -10 1 -8.4209 0.3064 -20 -10 2 8.6998 -0.3576 -20 -10 3 -0.6631 0.5189 -20 -10 4 -2.6024 -0.3157 -20 -10 5 5.1878 0.1458 -20 -10 6 -3.5297 0.0549 -20 -10 7 0.8329 -0.1450 -20 -9 1 -0.0365 -0.2014 -20 -9 2 6.9134 -0.0470 -20 -9 3 6.7113 0.2810 -20 -9 4 -2.5491 -0.2826 -20 -9 5 10.9217 0.2454 -20 -9 6 -4.1800 -0.0970 -20 -9 7 2.7633 0.1393 -20 -8 1 -6.0441 -0.7550 -20 -8 2 -8.3579 0.3456 -20 -8 3 -0.3165 -0.2862 -20 -8 4 -15.7253 -0.1398 -20 -8 5 7.4265 0.1448 -20 -8 6 -12.7156 -0.2027 -20 -8 7 5.2296 0.1455 -20 -8 8 -0.4483 -0.1875 -20 -7 1 0.8638 -0.6404 -20 -7 2 -4.1286 0.9570 -20 -7 3 8.8657 -0.3445 -20 -7 4 -12.9313 0.2270 -20 -7 5 14.3053 0.1047 -20 -7 6 -14.9123 -0.0916 -20 -7 7 7.8784 0.0820 -20 -7 8 -9.5064 0.0682 -20 -6 1 3.8249 -0.6690 -20 -6 2 1.1084 0.6249 -20 -6 3 14.0169 -0.3918 -20 -6 4 -4.8712 0.2318 -20 -6 5 18.8674 0.0801 -20 -6 6 -7.1276 -0.1475 -20 -6 7 14.5769 -0.1423 -20 -6 8 -5.8463 0.0438 -20 -5 1 -1.8575 -0.3034 -20 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0.2176 21 2 10 -2.9551 -0.0243 21 2 11 5.6798 0.0385 21 2 12 -2.5350 0.1780 21 2 13 -1.3041 -0.1188 21 2 14 -1.1215 0.2491 21 3 0 -0.4493 -0.0130 21 3 1 1.1067 -0.7620 21 3 2 -5.4353 -0.0287 21 3 3 1.2911 -0.1837 21 3 4 -1.4674 0.0346 21 3 9 -2.2875 0.1283 21 3 10 -8.0985 -0.1014 21 3 11 -2.4980 0.0165 21 3 12 -3.2137 0.0906 21 3 13 -3.5558 -0.1848 21 3 14 0.9413 0.1139 21 4 0 -1.9677 0.9768 21 4 1 6.0946 -0.2417 21 4 2 -0.7672 0.2722 21 4 3 4.8435 -0.0613 21 4 4 -0.6747 -0.1665 21 4 5 -2.3332 -0.1980 21 4 6 0.2375 0.0701 21 4 11 2.0297 -0.1060 21 4 12 5.1938 -0.0165 21 4 13 -0.5645 -0.1238 21 4 14 6.3052 -0.1358 21 5 0 -1.1722 0.5631 21 5 1 3.4048 -0.3552 21 5 2 -1.8647 0.3247 21 5 3 2.8683 0.2788 21 5 4 4.7121 0.0289 21 5 5 1.9838 0.1465 21 5 6 4.6816 0.2542 21 5 7 2.1768 -0.1511 21 5 8 1.3171 0.3408 21 5 13 -6.3462 0.1312 21 5 14 1.8356 -0.0943 21 6 0 1.0428 0.1909 21 6 1 1.3987 -0.5936 21 6 2 -0.6745 -0.0902 21 6 3 -5.6911 -0.0307 21 6 4 0.3199 -0.2080 21 6 5 -6.1700 0.1483 21 6 6 -0.8230 0.0949 21 6 7 -2.3513 -0.1410 21 6 8 -3.1574 0.1564 21 6 9 -2.4442 -0.2078 21 6 10 -2.5350 0.1101 21 6 11 -3.2011 -0.0206 21 7 0 -5.4225 0.3238 21 7 1 -4.3337 0.0947 21 7 2 -0.2425 0.1764 21 7 3 -5.5759 0.0455 21 7 4 2.5302 -0.2497 21 7 5 -5.3494 -0.0334 21 7 6 0.7260 -0.2294 21 7 7 -1.6086 -0.0839 21 7 8 0.5059 -0.0017 21 7 9 1.1296 -0.1163 21 7 10 -1.2098 -0.0065 21 7 11 -0.3430 -0.1544 21 7 12 -3.1154 -0.1464 21 7 13 -3.8227 0.1906 21 8 0 1.2550 -0.5525 21 8 1 3.9425 0.1287 21 8 2 1.7479 -0.1122 21 8 3 2.2376 0.1114 21 8 4 6.0426 0.0744 21 8 5 0.3860 0.2579 21 8 6 6.1359 -0.0428 21 8 7 -0.6071 0.1682 21 8 8 2.8110 -0.0596 21 8 9 2.5440 0.0485 21 8 10 0.0794 0.0964 21 8 11 6.5114 0.0099 21 8 12 -0.3518 -0.0564 21 8 13 2.7971 0.1957 21 9 0 -0.7379 -0.7485 21 9 1 8.5840 0.4649 21 9 2 -2.9975 -0.3239 21 9 3 3.1592 -0.0672 21 9 4 0.8720 -0.1305 21 9 5 -4.1860 0.0307 21 9 6 3.2396 -0.0899 21 9 7 -5.2855 0.2655 21 9 8 -1.3691 -0.0323 21 9 9 -1.6903 0.1596 21 9 10 -5.6285 0.0527 21 9 11 2.4033 0.0007 21 9 12 -1.4106 0.0313 21 10 0 -9.5853 -0.5704 21 10 1 2.8177 0.6408 21 10 2 -9.2877 -0.0293 21 10 3 -1.6529 0.1594 21 10 4 -0.7733 0.1295 21 10 5 -6.6024 -0.0653 21 10 6 4.8014 -0.1866 21 10 7 -1.2478 -0.0385 21 10 8 2.7252 -0.3267 21 10 9 3.6983 0.0334 21 10 10 -2.3375 -0.1386 21 10 11 -1.1820 -0.0671 21 11 2 -0.4069 -0.0936 21 11 3 1.2475 -0.1872 21 11 4 7.0992 0.2348 21 11 5 -4.0975 -0.0932 21 11 6 4.6961 0.1413 21 11 7 -2.7238 0.1165 21 11 8 -0.4468 -0.1635 21 11 9 2.5578 0.1130 0 0 0 0.0 0.0 ; _shelx_fab_checksum 2441 _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 2.066 _oxdiff_exptl_absorpt_empirical_full_min 0.558 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 0.14447(2) 0.89517(2) 0.21379(2) 0.02137(4) Uani 1 1 d . . . . . Dy2 Dy 0.52496(2) 0.34179(2) 0.25078(2) 0.02701(5) Uani 1 1 d D . . . . Br1 Br 0.56768(5) 0.70443(3) 0.26269(4) 0.04773(15) Uani 1 1 d . . . . . Br2 Br 0.10240(4) 0.53413(3) 0.19838(3) 0.03805(11) Uani 1 1 d . . . . . Br3 Br 0.27039(5) 1.11232(4) 0.39992(2) 0.03765(11) Uani 1 1 d . . . . . Br4 Br 0.38812(5) 1.13077(5) 0.06318(3) 0.05070(15) Uani 1 1 d . . . . . Zn1 Zn -0.13873(4) 0.90501(4) 0.18105(3) 0.02736(10) Uani 1 1 d D . . . . Zn2 Zn 0.81445(4) 0.35098(3) 0.27986(3) 0.02477(10) Uani 1 1 d D . . . . O1 O 0.5586(3) 0.3928(2) 0.13113(18) 0.0380(8) Uani 1 1 d . . . . . O2 O 0.7227(3) 0.3442(2) 0.20269(14) 0.0252(6) Uani 1 1 d . . . . . O3 O 0.6454(2) 0.3491(2) 0.33082(15) 0.0246(6) Uani 1 1 d . . . . . O4 O 0.4205(3) 0.3994(2) 0.37133(18) 0.0360(8) Uani 1 1 d . . . . . O5 O 0.1080(3) 0.8357(2) 0.33435(17) 0.0345(7) Uani 1 1 d . . . . . O6 O -0.0499(3) 0.8866(2) 0.26053(15) 0.0263(6) Uani 1 1 d . . . . . O7 O 0.0314(2) 0.9001(2) 0.13126(15) 0.0248(6) Uani 1 1 d . . . . . O8 O 0.2539(3) 0.8327(2) 0.09415(17) 0.0299(6) Uani 1 1 d . . . . . O9 O 0.5292(3) 0.50420(19) 0.25685(18) 0.0292(6) Uani 1 1 d . . . . . O10 O 0.3449(3) 0.4361(2) 0.2344(2) 0.0369(8) Uani 1 1 d . . . . . O11 O 0.3239(3) 0.80140(19) 0.22980(17) 0.0285(6) Uani 1 1 d . . . . . O12 O 0.1411(3) 0.7336(2) 0.20592(17) 0.0279(6) Uani 1 1 d . . . . . O13 O 0.2216(3) 0.9858(2) 0.28733(16) 0.0272(6) Uani 1 1 d . . . . . O14 O 0.2611(3) 0.9968(2) 0.15597(16) 0.0272(6) Uani 1 1 d . . . . . O15 O 0.3891(3) 1.2495(2) 0.30541(16) 0.0277(6) Uani 1 1 d . . . . . O16 O 0.4566(3) 1.2452(2) 0.17524(17) 0.0289(6) Uani 1 1 d . . . . . O17 O 0.7782(3) 0.4965(2) 0.28036(19) 0.0341(7) Uani 1 1 d D . . . . H17 H 0.719(3) 0.5260(13) 0.265(2) 0.051 Uiso 1 1 d D U . . . O18 O 0.6276(3) 0.1818(2) 0.26484(17) 0.0306(6) Uani 1 1 d D . . . . H18 H 0.693(3) 0.155(2) 0.2396(13) 0.046 Uiso 1 1 d D U . . . O19 O 0.0272(3) 1.0550(2) 0.22485(18) 0.0317(7) Uani 1 1 d . . . . . O20 O -0.1555(3) 1.0566(2) 0.20791(17) 0.0307(6) Uani 1 1 d . . . . . O21 O -0.1151(3) 1.1662(2) 0.2638(2) 0.0506(11) Uani 1 1 d . . . . . O22 O -0.1031(3) 0.7525(2) 0.1726(2) 0.0456(9) Uani 1 1 d D . . . . H22 H -0.053(5) 0.7194(13) 0.194(3) 0.068 Uiso 1 1 d D U . . . N1 N 0.9711(3) 0.3324(3) 0.2121(2) 0.0340(9) Uani 1 1 d . . . . . N2 N 0.8786(3) 0.3151(3) 0.3667(2) 0.0323(8) Uani 1 1 d . . . . . N3 N -0.2981(3) 0.9078(3) 0.2454(2) 0.0321(8) Uani 1 1 d . . . . . N4 N -0.2009(3) 0.9396(3) 0.0935(2) 0.0333(8) Uani 1 1 d . . . . . N5 N -0.0802(3) 1.0926(2) 0.23225(19) 0.0249(7) Uani 1 1 d . . . . . C1 C 0.4656(8) 0.4076(6) 0.0875(4) 0.078(2) Uani 1 1 d . . . . . H1A H 0.391130 0.397177 0.113243 0.117 Uiso 1 1 calc R U . . . H1B H 0.488929 0.365724 0.049192 0.117 Uiso 1 1 calc R U . . . H1C H 0.456569 0.469325 0.071965 0.117 Uiso 1 1 calc R U . . . C2 C 0.6728(5) 0.4016(4) 0.1006(3) 0.0426(12) Uani 1 1 d . . . . . C3 C 0.7040(8) 0.4298(7) 0.0352(4) 0.082(3) Uani 1 1 d . . . . . H3 H 0.646181 0.444814 0.007949 0.098 Uiso 1 1 calc R U . . . C4 C 0.8225(9) 0.4356(8) 0.0101(4) 0.108(4) Uani 1 1 d . . . . . H4 H 0.843141 0.456344 -0.033554 0.129 Uiso 1 1 calc R U . . . C5 C 0.9075(8) 0.4115(6) 0.0484(4) 0.079(3) Uani 1 1 d . . . . . H5 H 0.986497 0.414253 0.030413 0.095 Uiso 1 1 calc R U . . . C6 C 0.8783(5) 0.3823(4) 0.1152(3) 0.0444(12) Uani 1 1 d . . . . . C7 C 0.7587(4) 0.3765(3) 0.1420(2) 0.0332(9) Uani 1 1 d . . . . . C8 C 0.9770(5) 0.3532(4) 0.1510(3) 0.0444(13) Uani 1 1 d . . . . . H8 H 1.053229 0.349661 0.125664 0.053 Uiso 1 1 calc R U . . . C9 C 1.0846(4) 0.2985(4) 0.2358(3) 0.0440(13) Uani 1 1 d . . . . . H9A H 1.148543 0.321339 0.206519 0.053 Uiso 1 1 calc R U . . . H9B H 1.101445 0.232159 0.231999 0.053 Uiso 1 1 calc R U . . . C10 C 1.0829(4) 0.3272(4) 0.3082(4) 0.0524(17) Uani 1 1 d . . . . . H10A H 1.164188 0.315971 0.316758 0.063 Uiso 1 1 calc R U . . . H10B H 1.053695 0.392636 0.313299 0.063 Uiso 1 1 calc R U . . . C11 C 1.0080(4) 0.2798(4) 0.3612(3) 0.0454(13) Uani 1 1 d . . . . . H11A H 1.023614 0.214679 0.350207 0.055 Uiso 1 1 calc R U . . . H11B H 1.031235 0.287642 0.404866 0.055 Uiso 1 1 calc R U . . . C12 C 0.8172(5) 0.3236(3) 0.4254(3) 0.0394(11) Uani 1 1 d . . . . . H12 H 0.859320 0.311413 0.461020 0.047 Uiso 1 1 calc R U . . . C13 C 0.6883(5) 0.3500(3) 0.4446(2) 0.0364(10) Uani 1 1 d . . . . . C14 C 0.6400(7) 0.3619(4) 0.5145(3) 0.0527(16) Uani 1 1 d . . . . . H14 H 0.690898 0.355563 0.546181 0.063 Uiso 1 1 calc R U . . . C15 C 0.5193(7) 0.3825(5) 0.5360(3) 0.0610(18) Uani 1 1 d . . . . . H15 H 0.489078 0.388045 0.582316 0.073 Uiso 1 1 calc R U . . . C16 C 0.4418(6) 0.3953(4) 0.4904(3) 0.0519(15) Uani 1 1 d . . . . . H16 H 0.359839 0.410049 0.505571 0.062 Uiso 1 1 calc R U . . . C17 C 0.4871(4) 0.3859(3) 0.4221(3) 0.0366(10) Uani 1 1 d . . . . . C18 C 0.6107(4) 0.3617(3) 0.3974(2) 0.0277(8) Uani 1 1 d . . . . . C19 C 0.2927(4) 0.4188(4) 0.3939(3) 0.0536(17) Uani 1 1 d . . . . . H19A H 0.253385 0.425197 0.355109 0.080 Uiso 1 1 calc R U . . . H19B H 0.271274 0.474560 0.420651 0.080 Uiso 1 1 calc R U . . . H19C H 0.268432 0.369312 0.420791 0.080 Uiso 1 1 calc R U . . . C20 C 0.1935(5) 0.8197(4) 0.3795(3) 0.0479(14) Uani 1 1 d . . . . . H20A H 0.215369 0.755099 0.385422 0.072 Uiso 1 1 calc R U . . . H20B H 0.158933 0.849320 0.422627 0.072 Uiso 1 1 calc R U . . . H20C H 0.263221 0.844203 0.360405 0.072 Uiso 1 1 calc R U . . . C21 C -0.0042(5) 0.8161(3) 0.3587(2) 0.0342(10) Uani 1 1 d . . . . . C22 C -0.0349(6) 0.7706(4) 0.4183(3) 0.0449(12) Uani 1 1 d . . . . . H22A H 0.022570 0.748360 0.444445 0.054 Uiso 1 1 calc R U . . . C23 C -0.1525(6) 0.7586(4) 0.4385(3) 0.0524(15) Uani 1 1 d . . . . . H23 H -0.173388 0.726863 0.477737 0.063 Uiso 1 1 calc R U . . . C24 C -0.2369(5) 0.7933(4) 0.4011(3) 0.0442(13) Uani 1 1 d . . . . . H24 H -0.315854 0.787501 0.416375 0.053 Uiso 1 1 calc R U . . . C25 C -0.2073(4) 0.8379(3) 0.3394(2) 0.0337(10) Uani 1 1 d . . . . . C26 C -0.0879(4) 0.8475(3) 0.3176(2) 0.0264(8) Uani 1 1 d . . . . . C27 C -0.3055(4) 0.8755(3) 0.3049(3) 0.0357(10) Uani 1 1 d . . . . . H27 H -0.382106 0.876018 0.328945 0.043 Uiso 1 1 calc R U . . . C28 C -0.4110(4) 0.9463(3) 0.2224(3) 0.0403(12) Uani 1 1 d . . . . . H28A H -0.428292 1.011968 0.230995 0.048 Uiso 1 1 calc R U . . . H28B H -0.475375 0.920302 0.248602 0.048 Uiso 1 1 calc R U . . . C29 C -0.4063(4) 0.9272(4) 0.1474(3) 0.0448(14) Uani 1 1 d . . . . . H29A H -0.378088 0.862180 0.138130 0.054 Uiso 1 1 calc R U . . . H29B H -0.486749 0.941615 0.137673 0.054 Uiso 1 1 calc R U . . . C30 C -0.3276(4) 0.9797(3) 0.0998(3) 0.0405(12) Uani 1 1 d . . . . . H30A H -0.350417 0.980593 0.055359 0.049 Uiso 1 1 calc R U . . . H30B H -0.340032 1.042577 0.116490 0.049 Uiso 1 1 calc R U . . . C31 C -0.1374(4) 0.9271(3) 0.0340(2) 0.0326(9) Uani 1 1 d . . . . . H31 H -0.176230 0.943732 -0.002461 0.039 Uiso 1 1 calc R U . . . C32 C -0.0111(4) 0.8897(3) 0.0179(2) 0.0306(9) Uani 1 1 d . . . . . C33 C 0.0357(5) 0.8660(3) -0.0511(2) 0.0375(11) Uani 1 1 d . . . . . H33 H -0.014741 0.873935 -0.082978 0.045 Uiso 1 1 calc R U . . . C34 C 0.1545(6) 0.8316(4) -0.0712(2) 0.0444(13) Uani 1 1 d . . . . . H34 H 0.184147 0.817088 -0.116871 0.053 Uiso 1 1 calc R U . . . C35 C 0.2308(5) 0.8180(3) -0.0246(3) 0.0389(11) Uani 1 1 d . . . . . H35 H 0.311057 0.793095 -0.038457 0.047 Uiso 1 1 calc R U . . . C36 C 0.1870(4) 0.8418(3) 0.0424(2) 0.0272(8) Uani 1 1 d . . . . . C37 C 0.0661(4) 0.8778(3) 0.0653(2) 0.0245(7) Uani 1 1 d . . . . . C38 C 0.3808(4) 0.8107(5) 0.0728(3) 0.0506(14) Uani 1 1 d . . . . . H38A H 0.405767 0.853101 0.039257 0.076 Uiso 1 1 calc R U . . . H38B H 0.401985 0.749593 0.053723 0.076 Uiso 1 1 calc R U . . . H38C H 0.419470 0.814638 0.111199 0.076 Uiso 1 1 calc R U . . . C39 C 0.4352(4) 0.6567(3) 0.2460(3) 0.0296(9) Uani 1 1 d . . . . . C40 C 0.4419(3) 0.5619(3) 0.2458(2) 0.0247(8) Uani 1 1 d . . . . . C41 C 0.3343(4) 0.5218(3) 0.2317(2) 0.0278(8) Uani 1 1 d . . . . . C42 C 0.2339(3) 0.5816(3) 0.2174(2) 0.0264(8) Uani 1 1 d . . . . . C43 C 0.2282(3) 0.6759(3) 0.2173(2) 0.0223(7) Uani 1 1 d . . . . . C44 C 0.3357(3) 0.7154(3) 0.2316(2) 0.0252(8) Uani 1 1 d . . . . . C45 C 0.2714(3) 1.0509(3) 0.2654(2) 0.0221(7) Uani 1 1 d . . . . . C46 C 0.3061(3) 1.1163(3) 0.3043(2) 0.0234(7) Uani 1 1 d . . . . . C47 C 0.3618(3) 1.1851(3) 0.2747(2) 0.0219(7) Uani 1 1 d . . . . . C48 C 0.3953(3) 1.1864(3) 0.1970(2) 0.0244(8) Uani 1 1 d . . . . . C49 C 0.3553(4) 1.1253(3) 0.1580(2) 0.0263(8) Uani 1 1 d . . . . . C50 C 0.2961(3) 1.0571(3) 0.1877(2) 0.0224(7) Uani 1 1 d . . . . . C87 C 0.6251(5) 0.1414(3) 0.3309(3) 0.0394(11) Uani 1 1 d D . . . . H87A H 0.644944 0.075887 0.325572 0.059 Uiso 1 1 calc R U . . . H87B H 0.546691 0.158202 0.357401 0.059 Uiso 1 1 calc R U . . . H87C H 0.682059 0.163100 0.353454 0.059 Uiso 1 1 calc R U . . . C88 C 0.8075(5) 0.5546(4) 0.3291(3) 0.0456(13) Uani 1 1 d D . . . . H88A H 0.812167 0.613773 0.310239 0.068 Uiso 1 1 calc R U . . . H88B H 0.883119 0.528173 0.340875 0.068 Uiso 1 1 calc R U . . . H88C H 0.746995 0.560936 0.369106 0.068 Uiso 1 1 calc R U . . . C89 C -0.1262(7) 0.6957(5) 0.1223(4) 0.070(2) Uani 1 1 d D . . . . H89A H -0.058713 0.685063 0.085981 0.105 Uiso 1 1 calc R U . . . H89B H -0.195448 0.724909 0.104920 0.105 Uiso 1 1 calc R U . . . H89C H -0.140029 0.638280 0.141510 0.105 Uiso 1 1 calc R U . . . Cl1 Cl 0.0050(5) 0.4956(5) 0.5090(3) 0.0511(11) Uani 0.5 1 d G U P A -1 O25 O 0.1176(7) 0.4834(7) 0.5273(5) 0.077(3) Uani 0.5 1 d G U P A -1 O26 O -0.0659(8) 0.4448(7) 0.5494(7) 0.127(5) Uani 0.5 1 d G U P A -1 O27 O 0.0135(11) 0.4655(11) 0.4453(5) 0.167(7) Uani 0.5 1 d G U P A -1 O28 O -0.0530(8) 0.5856(6) 0.5180(6) 0.085(3) Uani 0.5 1 d G U P A -1 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 0.01674(8) 0.01724(8) 0.03145(10) 0.00119(6) -0.00861(6) -0.00233(6) Dy2 0.01655(8) 0.01742(9) 0.04946(13) -0.00275(8) -0.01402(8) -0.00129(6) Br1 0.0339(2) 0.0250(2) 0.0965(5) 0.0097(2) -0.0392(3) -0.01140(18) Br2 0.0264(2) 0.0268(2) 0.0681(3) 0.0047(2) -0.0224(2) -0.01033(17) Br3 0.0400(3) 0.0476(3) 0.0292(2) 0.00137(19) -0.00958(18) -0.0148(2) Br4 0.0503(3) 0.0842(4) 0.0289(2) 0.0078(3) -0.0095(2) -0.0402(3) Zn1 0.0174(2) 0.0318(3) 0.0333(3) 0.0017(2) -0.00734(18) -0.00268(18) Zn2 0.01460(19) 0.0278(2) 0.0324(2) -0.00191(19) -0.00730(17) -0.00187(16) O1 0.049(2) 0.0360(18) 0.0405(18) 0.0155(14) -0.0281(16) -0.0182(15) O2 0.0254(14) 0.0270(14) 0.0238(13) 0.0027(11) -0.0056(11) -0.0051(11) O3 0.0170(12) 0.0299(15) 0.0268(14) -0.0019(11) -0.0040(10) -0.0041(11) O4 0.0179(13) 0.0421(19) 0.0457(19) -0.0173(15) 0.0041(13) -0.0079(13) O5 0.0353(17) 0.0383(18) 0.0356(17) 0.0110(14) -0.0174(14) -0.0111(14) O6 0.0229(13) 0.0278(15) 0.0301(15) 0.0092(12) -0.0078(11) -0.0066(11) O7 0.0181(12) 0.0288(15) 0.0280(14) -0.0006(11) -0.0062(10) -0.0035(11) O8 0.0222(14) 0.0294(16) 0.0366(17) -0.0056(13) -0.0007(12) -0.0045(12) O9 0.0209(13) 0.0155(12) 0.0532(19) -0.0012(12) -0.0150(13) -0.0004(10) O10 0.0232(14) 0.0167(13) 0.075(3) 0.0011(14) -0.0198(15) -0.0033(11) O11 0.0230(13) 0.0163(13) 0.0487(19) 0.0029(12) -0.0139(13) -0.0033(10) O12 0.0196(13) 0.0222(14) 0.0443(18) 0.0017(12) -0.0118(12) -0.0036(11) O13 0.0263(14) 0.0229(14) 0.0343(16) 0.0044(12) -0.0090(12) -0.0059(11) O14 0.0251(14) 0.0270(15) 0.0315(15) -0.0064(12) -0.0034(11) -0.0111(11) O15 0.0207(13) 0.0226(14) 0.0401(17) -0.0097(12) -0.0069(12) -0.0030(11) O16 0.0251(14) 0.0263(15) 0.0393(17) 0.0064(12) -0.0096(12) -0.0115(12) O17 0.0289(16) 0.0239(15) 0.052(2) -0.0025(14) -0.0181(14) -0.0015(12) O18 0.0215(14) 0.0265(15) 0.0424(18) -0.0008(13) -0.0093(12) 0.0037(11) O19 0.0191(13) 0.0207(14) 0.055(2) -0.0029(13) -0.0087(13) 0.0002(11) O20 0.0267(15) 0.0283(15) 0.0398(17) 0.0040(13) -0.0135(13) -0.0051(12) O21 0.0333(18) 0.0244(17) 0.092(3) -0.0185(18) -0.0068(19) -0.0022(14) O22 0.043(2) 0.0280(17) 0.070(3) -0.0072(17) -0.0199(19) -0.0064(15) N1 0.0188(16) 0.0285(19) 0.053(3) -0.0051(17) -0.0005(16) -0.0061(14) N2 0.0285(18) 0.0239(17) 0.047(2) 0.0012(16) -0.0199(17) 0.0001(14) N3 0.0221(16) 0.0233(17) 0.050(2) -0.0003(16) -0.0047(16) -0.0043(13) N4 0.0252(17) 0.0282(18) 0.051(2) -0.0043(16) -0.0207(17) -0.0037(14) N5 0.0225(15) 0.0190(15) 0.0330(18) 0.0034(13) -0.0052(13) -0.0026(12) C1 0.090(6) 0.070(5) 0.084(6) 0.024(4) -0.051(5) -0.011(4) C2 0.056(3) 0.047(3) 0.033(2) 0.016(2) -0.017(2) -0.023(3) C3 0.096(6) 0.123(7) 0.051(4) 0.050(4) -0.037(4) -0.059(5) C4 0.117(8) 0.170(11) 0.057(5) 0.063(6) -0.021(5) -0.079(8) C5 0.084(5) 0.117(7) 0.043(4) 0.025(4) 0.005(3) -0.057(5) C6 0.046(3) 0.054(3) 0.035(3) 0.004(2) 0.002(2) -0.022(3) C7 0.040(2) 0.031(2) 0.031(2) 0.0017(17) -0.0042(18) -0.0155(19) C8 0.029(2) 0.042(3) 0.060(4) -0.008(2) 0.005(2) -0.013(2) C9 0.0120(17) 0.033(2) 0.083(4) 0.000(3) -0.003(2) 0.0005(16) C10 0.022(2) 0.034(3) 0.107(5) -0.012(3) -0.029(3) -0.0009(19) C11 0.028(2) 0.037(3) 0.076(4) 0.002(3) -0.031(2) 0.0028(19) C12 0.052(3) 0.035(2) 0.036(2) 0.0014(19) -0.027(2) -0.001(2) C13 0.048(3) 0.031(2) 0.029(2) -0.0001(18) -0.011(2) -0.001(2) C14 0.088(5) 0.040(3) 0.029(2) 0.001(2) -0.016(3) -0.003(3) C15 0.079(5) 0.062(4) 0.032(3) -0.003(3) 0.010(3) -0.006(4) C16 0.057(4) 0.054(4) 0.037(3) -0.011(2) 0.015(3) -0.014(3) C17 0.037(2) 0.030(2) 0.041(3) -0.0072(19) 0.006(2) -0.0128(19) C18 0.032(2) 0.0193(18) 0.029(2) -0.0019(15) 0.0015(16) -0.0045(15) C19 0.021(2) 0.060(4) 0.073(4) -0.032(3) 0.014(2) -0.011(2) C20 0.056(3) 0.062(4) 0.033(2) 0.020(2) -0.028(2) -0.012(3) C21 0.048(3) 0.030(2) 0.028(2) 0.0029(17) -0.0120(19) -0.010(2) C22 0.061(4) 0.044(3) 0.034(3) 0.010(2) -0.013(2) -0.018(3) C23 0.073(4) 0.052(3) 0.035(3) 0.011(2) 0.000(3) -0.026(3) C24 0.052(3) 0.042(3) 0.037(3) -0.004(2) 0.010(2) -0.022(2) C25 0.038(2) 0.026(2) 0.035(2) -0.0026(17) 0.0042(19) -0.0101(18) C26 0.034(2) 0.0211(18) 0.0244(18) 0.0021(14) -0.0034(16) -0.0063(16) C27 0.026(2) 0.024(2) 0.055(3) -0.009(2) 0.0027(19) -0.0083(16) C28 0.0160(18) 0.029(2) 0.074(4) -0.002(2) -0.004(2) -0.0021(16) C29 0.021(2) 0.032(2) 0.086(4) -0.012(3) -0.021(2) -0.0026(17) C30 0.031(2) 0.035(2) 0.060(3) -0.007(2) -0.029(2) 0.0036(19) C31 0.038(2) 0.028(2) 0.035(2) -0.0029(17) -0.0197(19) -0.0029(18) C32 0.039(2) 0.024(2) 0.031(2) -0.0016(16) -0.0094(18) -0.0057(17) C33 0.056(3) 0.033(2) 0.023(2) 0.0031(17) -0.010(2) -0.005(2) C34 0.068(4) 0.039(3) 0.020(2) -0.0003(18) -0.001(2) -0.001(3) C35 0.047(3) 0.029(2) 0.034(2) -0.0002(18) 0.007(2) -0.003(2) C36 0.029(2) 0.0245(19) 0.028(2) 0.0003(15) -0.0005(15) -0.0083(16) C37 0.031(2) 0.0168(16) 0.0262(19) 0.0014(14) -0.0054(15) -0.0065(14) C38 0.022(2) 0.070(4) 0.055(3) -0.002(3) 0.002(2) -0.003(2) C39 0.0216(18) 0.0200(18) 0.052(3) 0.0017(17) -0.0180(18) -0.0055(14) C40 0.0181(16) 0.0198(17) 0.037(2) -0.0012(15) -0.0086(15) -0.0016(13) C41 0.0191(17) 0.0216(18) 0.044(2) 0.0000(16) -0.0088(16) -0.0031(14) C42 0.0179(16) 0.0199(18) 0.043(2) 0.0015(16) -0.0088(16) -0.0043(13) C43 0.0201(16) 0.0199(17) 0.0286(19) 0.0034(14) -0.0069(14) -0.0054(13) C44 0.0199(17) 0.0206(18) 0.037(2) 0.0018(15) -0.0108(15) -0.0035(14) C45 0.0151(15) 0.0182(16) 0.034(2) 0.0018(14) -0.0085(14) -0.0013(12) C46 0.0183(16) 0.0219(18) 0.0294(19) -0.0021(14) -0.0063(14) 0.0001(13) C47 0.0163(15) 0.0180(16) 0.033(2) -0.0015(14) -0.0088(14) -0.0022(12) C48 0.0176(16) 0.0201(17) 0.037(2) 0.0020(15) -0.0105(15) -0.0024(13) C49 0.0226(18) 0.031(2) 0.0279(19) 0.0002(16) -0.0070(15) -0.0084(15) C50 0.0133(14) 0.0237(18) 0.0298(19) -0.0045(14) -0.0040(13) -0.0014(13) C87 0.037(3) 0.032(2) 0.050(3) 0.006(2) -0.014(2) -0.0005(19) C88 0.037(3) 0.039(3) 0.061(3) -0.021(2) -0.016(2) 0.001(2) C89 0.071(5) 0.048(4) 0.098(6) -0.021(4) -0.046(4) 0.003(3) Cl1 0.0317(12) 0.0602(17) 0.057(3) -0.0291(19) -0.0056(15) 0.0031(11) O25 0.046(5) 0.125(7) 0.056(5) -0.009(5) -0.010(4) -0.006(5) O26 0.080(7) 0.105(8) 0.181(10) 0.038(7) 0.012(7) -0.008(6) O27 0.159(10) 0.195(11) 0.161(10) -0.059(8) -0.078(8) -0.023(8) O28 0.070(6) 0.057(5) 0.108(7) 0.009(5) 0.021(5) 0.004(5) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Zn Zn 0.2839 1.4301 '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 O5 Dy1 Zn1 97.49(7) . . ? O5 Dy1 O8 137.73(11) . . ? O6 Dy1 Zn1 35.01(7) . . ? O6 Dy1 O5 63.14(10) . . ? O6 Dy1 O8 125.68(10) . . ? O6 Dy1 O11 129.86(10) . . ? O6 Dy1 O12 77.15(10) . . ? O6 Dy1 O13 108.84(11) . . ? O6 Dy1 O14 141.33(10) . . ? O6 Dy1 O19 72.33(10) . . ? O7 Dy1 Zn1 34.92(7) . . ? O7 Dy1 O5 129.81(10) . . ? O7 Dy1 O6 69.68(10) . . ? O7 Dy1 O8 63.34(10) . . ? O7 Dy1 O11 133.00(11) . . ? O7 Dy1 O12 82.03(10) . . ? O7 Dy1 O13 144.41(10) . . ? O7 Dy1 O14 92.27(10) . . ? O7 Dy1 O19 76.48(11) . . ? O8 Dy1 Zn1 95.99(7) . . ? O11 Dy1 Zn1 146.87(7) . . ? O11 Dy1 O5 73.34(11) . . ? O11 Dy1 O8 73.59(11) . . ? O11 Dy1 O12 66.40(9) . . ? O11 Dy1 O13 76.70(10) . . ? O11 Dy1 O14 87.70(11) . . ? O11 Dy1 O19 144.97(10) . . ? O12 Dy1 Zn1 80.46(7) . . ? O12 Dy1 O5 72.07(11) . . ? O12 Dy1 O8 71.00(11) . . ? O12 Dy1 O19 147.22(10) . . ? O13 Dy1 Zn1 131.24(7) . . ? O13 Dy1 O5 70.57(10) . . ? O13 Dy1 O8 125.13(10) . . ? O13 Dy1 O12 133.27(10) . . ? O13 Dy1 O19 69.70(10) . . ? O14 Dy1 Zn1 117.82(8) . . ? O14 Dy1 O5 135.89(10) . . ? O14 Dy1 O8 67.35(10) . . ? O14 Dy1 O12 135.70(11) . . ? O14 Dy1 O13 66.39(10) . . ? O14 Dy1 O19 70.24(10) . . ? O19 Dy1 Zn1 67.73(7) . . ? O19 Dy1 O5 103.55(12) . . ? O19 Dy1 O8 118.63(11) . . ? O1 Dy2 Zn2 95.74(8) . . ? O1 Dy2 O4 141.54(12) . . ? O1 Dy2 O18 113.14(12) . . ? O2 Dy2 Zn2 33.37(7) . . ? O2 Dy2 O1 64.38(11) . . ? O2 Dy2 O4 126.35(10) . . ? O2 Dy2 O9 78.97(10) . . ? O2 Dy2 O10 131.27(11) . . ? O2 Dy2 O15 145.10(10) . 1_545 ? O2 Dy2 O16 104.94(10) . 1_545 ? O2 Dy2 O18 76.72(10) . . ? O3 Dy2 Zn2 33.64(7) . . ? O3 Dy2 O1 127.15(10) . . ? O3 Dy2 O2 67.01(10) . . ? O3 Dy2 O4 62.91(10) . . ? O3 Dy2 O9 77.79(10) . . ? O3 Dy2 O10 131.28(11) . . ? O3 Dy2 O15 101.92(10) . 1_545 ? O3 Dy2 O16 146.46(10) . 1_545 ? O3 Dy2 O18 73.30(10) . . ? O4 Dy2 Zn2 94.83(7) . . ? O9 Dy2 Zn2 75.94(7) . . ? O9 Dy2 O1 73.91(11) . . ? O9 Dy2 O4 73.05(11) . . ? O9 Dy2 O18 147.69(10) . . ? O10 Dy2 Zn2 142.20(7) . . ? O10 Dy2 O1 73.58(13) . . ? O10 Dy2 O4 75.49(13) . . ? O10 Dy2 O9 66.27(10) . . ? O10 Dy2 O15 81.65(11) . 1_545 ? O10 Dy2 O16 79.47(11) . 1_545 ? O10 Dy2 O18 145.69(10) . . ? O15 Dy2 Zn2 128.15(7) 1_545 . ? O15 Dy2 O1 129.96(10) 1_545 . ? O15 Dy2 O4 65.86(10) 1_545 . ? O15 Dy2 O9 132.89(10) 1_545 . ? O15 Dy2 O16 65.23(10) 1_545 1_545 ? O15 Dy2 O18 68.38(10) 1_545 . ? O16 Dy2 Zn2 130.84(7) 1_545 . ? O16 Dy2 O1 67.87(10) 1_545 . ? O16 Dy2 O4 127.38(10) 1_545 . ? O16 Dy2 O9 134.34(10) 1_545 . ? O16 Dy2 O18 73.16(10) 1_545 . ? O18 Dy2 Zn2 72.03(7) . . ? O18 Dy2 O4 105.30(12) . . ? O6 Zn1 Dy1 40.67(8) . . ? O6 Zn1 O7 80.04(12) . . ? O6 Zn1 O20 83.51(12) . . ? O6 Zn1 O22 84.91(13) . . ? O6 Zn1 N3 90.58(15) . . ? O6 Zn1 N4 167.78(14) . . ? O7 Zn1 Dy1 39.68(8) . . ? O7 Zn1 O20 91.16(12) . . ? O7 Zn1 O22 87.01(14) . . ? O7 Zn1 N3 170.61(14) . . ? O20 Zn1 Dy1 82.77(8) . . ? O22 Zn1 Dy1 88.57(10) . . ? O22 Zn1 O20 168.43(13) . . ? N3 Zn1 Dy1 130.95(12) . . ? N3 Zn1 O20 87.36(13) . . ? N3 Zn1 O22 92.58(15) . . ? N4 Zn1 Dy1 128.40(12) . . ? N4 Zn1 O7 89.93(14) . . ? N4 Zn1 O20 89.79(13) . . ? N4 Zn1 O22 101.63(15) . . ? N4 Zn1 N3 99.34(17) . . ? O2 Zn2 Dy2 39.10(8) . . ? O2 Zn2 O3 77.83(11) . . ? O2 Zn2 O17 91.27(12) . . ? O2 Zn2 N1 90.15(15) . . ? O2 Zn2 N2 158.26(14) . . ? O3 Zn2 Dy2 38.73(8) . . ? O3 Zn2 O17 90.49(13) . . ? O17 Zn2 Dy2 91.03(8) . . ? N1 Zn2 Dy2 128.84(12) . . ? N1 Zn2 O3 165.68(14) . . ? N1 Zn2 O17 97.63(15) . . ? N2 Zn2 Dy2 125.91(12) . . ? N2 Zn2 O3 89.23(14) . . ? N2 Zn2 O17 106.41(14) . . ? N2 Zn2 N1 99.68(17) . . ? C1 O1 Dy2 124.3(4) . . ? C2 O1 Dy2 119.0(3) . . ? C2 O1 C1 116.5(5) . . ? Zn2 O2 Dy2 107.53(12) . . ? C7 O2 Dy2 125.1(3) . . ? C7 O2 Zn2 121.2(3) . . ? Zn2 O3 Dy2 107.63(12) . . ? C18 O3 Dy2 127.0(3) . . ? C18 O3 Zn2 124.9(3) . . ? C17 O4 Dy2 117.3(3) . . ? C17 O4 C19 115.2(4) . . ? C19 O4 Dy2 124.8(3) . . ? C20 O5 Dy1 126.2(3) . . ? C21 O5 Dy1 117.2(3) . . ? C21 O5 C20 116.7(4) . . ? Zn1 O6 Dy1 104.32(12) . . ? C26 O6 Dy1 127.5(3) . . ? C26 O6 Zn1 124.4(3) . . ? Zn1 O7 Dy1 105.41(12) . . ? C37 O7 Dy1 128.7(2) . . ? C37 O7 Zn1 123.2(2) . . ? C36 O8 Dy1 116.8(2) . . ? C36 O8 C38 115.6(4) . . ? C38 O8 Dy1 125.7(3) . . ? C40 O9 Dy2 120.5(2) . . ? C41 O10 Dy2 122.0(3) . . ? C44 O11 Dy1 122.3(2) . . ? C43 O12 Dy1 120.3(2) . . ? C45 O13 Dy1 121.2(3) . . ? C50 O14 Dy1 121.3(3) . . ? C47 O15 Dy2 121.9(3) . 1_565 ? C48 O16 Dy2 121.8(3) . 1_565 ? Zn2 O17 H17 121.7(16) . . ? C88 O17 Zn2 124.9(3) . . ? C88 O17 H17 107.9(16) . . ? Dy2 O18 H18 124.8(16) . . ? C87 O18 Dy2 121.7(3) . . ? C87 O18 H18 106.6(15) . . ? N5 O19 Dy1 137.3(3) . . ? N5 O20 Zn1 126.0(2) . . ? Zn1 O22 H22 122.1(15) . . ? C89 O22 Zn1 128.8(4) . . ? C89 O22 H22 106.8(15) . . ? C8 N1 Zn2 123.0(4) . . ? C8 N1 C9 117.3(4) . . ? C9 N1 Zn2 119.6(4) . . ? C11 N2 Zn2 118.1(4) . . ? C12 N2 Zn2 124.9(3) . . ? C12 N2 C11 116.9(4) . . ? C27 N3 Zn1 122.9(3) . . ? C27 N3 C28 117.3(4) . . ? C28 N3 Zn1 119.8(3) . . ? C30 N4 Zn1 117.0(3) . . ? C31 N4 Zn1 124.5(3) . . ? C31 N4 C30 118.5(4) . . ? O19 N5 O20 121.4(3) . . ? O21 N5 O19 120.4(4) . . ? O21 N5 O20 118.2(4) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C7 113.6(4) . . ? C3 C2 O1 125.1(5) . . ? C3 C2 C7 121.2(6) . . ? C2 C3 H3 120.2 . . ? C2 C3 C4 119.7(7) . . ? C4 C3 H3 120.2 . . ? C3 C4 H4 119.6 . . ? C5 C4 C3 120.7(7) . . ? C5 C4 H4 119.6 . . ? C4 C5 H5 119.6 . . ? C4 C5 C6 120.9(7) . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 119.5(6) . . ? C5 C6 C8 116.6(6) . . ? C7 C6 C8 123.8(5) . . ? O2 C7 C2 117.5(4) . . ? O2 C7 C6 124.4(5) . . ? C2 C7 C6 118.0(5) . . ? N1 C8 C6 127.3(5) . . ? N1 C8 H8 116.4 . . ? C6 C8 H8 116.4 . . ? N1 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? N1 C9 C10 113.0(4) . . ? H9A C9 H9B 107.8 . . ? C10 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C9 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C11 C10 C9 115.3(4) . . ? C11 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? N2 C11 C10 112.7(4) . . ? N2 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C10 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N2 C12 H12 116.0 . . ? N2 C12 C13 128.1(4) . . ? C13 C12 H12 116.0 . . ? C14 C13 C12 117.7(5) . . ? C18 C13 C12 123.2(4) . . ? C18 C13 C14 119.0(5) . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 119.4 . . ? C14 C15 C16 121.2(5) . . ? C16 C15 H15 119.4 . . ? C15 C16 H16 120.5 . . ? C17 C16 C15 119.0(6) . . ? C17 C16 H16 120.5 . . ? O4 C17 C16 125.1(5) . . ? O4 C17 C18 112.9(4) . . ? C16 C17 C18 122.0(5) . . ? O3 C18 C13 124.3(4) . . ? O3 C18 C17 117.6(4) . . ? C13 C18 C17 118.1(4) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? O5 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C22 125.1(5) . . ? O5 C21 C26 113.5(4) . . ? C22 C21 C26 121.3(5) . . ? C21 C22 H22A 120.3 . . ? C21 C22 C23 119.4(5) . . ? C23 C22 H22A 120.3 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.1(5) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 119.2 . . ? C23 C24 C25 121.5(5) . . ? C25 C24 H24 119.2 . . ? C24 C25 C27 116.8(5) . . ? C26 C25 C24 118.6(5) . . ? C26 C25 C27 124.5(4) . . ? O6 C26 C21 117.3(4) . . ? O6 C26 C25 123.8(4) . . ? C21 C26 C25 118.9(4) . . ? N3 C27 C25 127.1(4) . . ? N3 C27 H27 116.4 . . ? C25 C27 H27 116.4 . . ? N3 C28 H28A 109.1 . . ? N3 C28 H28B 109.1 . . ? N3 C28 C29 112.5(4) . . ? H28A C28 H28B 107.8 . . ? C29 C28 H28A 109.1 . . ? C29 C28 H28B 109.1 . . ? C28 C29 H29A 108.5 . . ? C28 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C30 C29 C28 114.9(4) . . ? C30 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? N4 C30 C29 112.2(4) . . ? N4 C30 H30A 109.2 . . ? N4 C30 H30B 109.2 . . ? C29 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? N4 C31 H31 116.8 . . ? N4 C31 C32 126.4(4) . . ? C32 C31 H31 116.8 . . ? C33 C32 C31 116.5(4) . . ? C37 C32 C31 124.5(4) . . ? C37 C32 C33 119.0(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 C32 120.6(5) . . ? C34 C33 H33 119.7 . . ? C33 C34 H34 119.6 . . ? C33 C34 C35 120.8(5) . . ? C35 C34 H34 119.6 . . ? C34 C35 H35 120.3 . . ? C36 C35 C34 119.3(5) . . ? C36 C35 H35 120.3 . . ? O8 C36 C37 113.0(4) . . ? C35 C36 O8 125.2(4) . . ? C35 C36 C37 121.9(4) . . ? O7 C37 C32 123.7(4) . . ? O7 C37 C36 117.9(4) . . ? C32 C37 C36 118.4(4) . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 Br1 118.5(3) . . ? C44 C39 Br1 119.8(3) . . ? C44 C39 C40 121.7(4) . . ? O9 C40 C39 125.7(4) . . ? O9 C40 C41 115.2(3) . . ? C39 C40 C41 119.1(3) . . ? O10 C41 C40 115.7(3) . . ? O10 C41 C42 125.4(4) . . ? C42 C41 C40 118.9(4) . . ? C41 C42 Br2 119.7(3) . . ? C43 C42 Br2 118.7(3) . . ? C43 C42 C41 121.7(4) . . ? O12 C43 C42 125.3(4) . . ? O12 C43 C44 115.6(3) . . ? C42 C43 C44 119.1(3) . . ? O11 C44 C39 125.3(4) . . ? O11 C44 C43 115.2(3) . . ? C39 C44 C43 119.5(3) . . ? O13 C45 C46 126.6(4) . . ? O13 C45 C50 114.8(3) . . ? C46 C45 C50 118.6(3) . . ? C45 C46 Br3 118.9(3) . . ? C47 C46 Br3 119.3(3) . . ? C47 C46 C45 121.7(4) . . ? O15 C47 C46 126.0(4) . . ? O15 C47 C48 114.6(3) . . ? C46 C47 C48 119.4(3) . . ? O16 C48 C47 114.6(4) . . ? O16 C48 C49 126.4(4) . . ? C49 C48 C47 119.0(4) . . ? C48 C49 Br4 119.3(3) . . ? C48 C49 C50 121.5(4) . . ? C50 C49 Br4 119.1(3) . . ? O14 C50 C45 115.2(3) . . ? O14 C50 C49 125.5(4) . . ? C49 C50 C45 119.3(3) . . ? O18 C87 H87A 109.5 . . ? O18 C87 H87B 109.5 . . ? O18 C87 H87C 109.5 . . ? H87A C87 H87B 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? O17 C88 H88A 109.5 . . ? O17 C88 H88B 109.5 . . ? O17 C88 H88C 109.5 . . ? H88A C88 H88B 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? O22 C89 H89A 109.5 . . ? O22 C89 H89B 109.5 . . ? O22 C89 H89C 109.5 . . ? H89A C89 H89B 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? O26 Cl1 O25 110.1 . . ? O26 Cl1 O28 106.2 . . ? O27 Cl1 O25 110.2 . . ? O27 Cl1 O26 106.7 . . ? O27 Cl1 O28 111.4 . . ? O28 Cl1 O25 111.9 . . ? 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 Zn1 3.4264(5) . ? Dy1 O5 2.554(3) . ? Dy1 O6 2.304(3) . ? Dy1 O7 2.269(3) . ? Dy1 O8 2.599(3) . ? Dy1 O11 2.356(3) . ? Dy1 O12 2.411(3) . ? Dy1 O13 2.381(3) . ? Dy1 O14 2.362(3) . ? Dy1 O19 2.506(3) . ? Dy2 Zn2 3.5203(5) . ? Dy2 O1 2.492(3) . ? Dy2 O2 2.328(3) . ? Dy2 O3 2.311(3) . ? Dy2 O4 2.580(3) . ? Dy2 O9 2.423(3) . ? Dy2 O10 2.367(3) . ? Dy2 O15 2.384(3) 1_545 ? Dy2 O16 2.409(3) 1_545 ? Dy2 O18 2.497(3) . ? Br1 C39 1.877(4) . ? Br2 C42 1.880(4) . ? Br3 C46 1.888(4) . ? Br4 C49 1.873(4) . ? Zn1 O6 2.029(3) . ? Zn1 O7 2.034(3) . ? Zn1 O20 2.283(3) . ? Zn1 O22 2.230(4) . ? Zn1 N3 2.051(4) . ? Zn1 N4 2.034(4) . ? Zn2 O2 2.031(3) . ? Zn2 O3 2.046(3) . ? Zn2 O17 2.126(3) . ? Zn2 N1 2.042(4) . ? Zn2 N2 2.035(4) . ? O1 C1 1.485(7) . ? O1 C2 1.383(7) . ? O2 C7 1.328(5) . ? O3 C18 1.328(5) . ? O4 C17 1.371(7) . ? O4 C19 1.446(5) . ? O5 C20 1.439(5) . ? O5 C21 1.384(6) . ? O6 C26 1.319(5) . ? O7 C37 1.337(5) . ? O8 C36 1.388(5) . ? O8 C38 1.433(6) . ? O9 C40 1.253(5) . ? O10 C41 1.257(5) . ? O11 C44 1.261(5) . ? O12 C43 1.254(5) . ? O13 C45 1.250(5) . ? O14 C50 1.261(5) . ? O15 C47 1.254(5) . ? O16 C48 1.249(5) . ? O17 H17 0.854(9) . ? O17 C88 1.427(6) . ? O18 H18 0.863(9) . ? O18 C87 1.444(6) . ? O19 N5 1.252(4) . ? O20 N5 1.262(4) . ? O21 N5 1.232(5) . ? O22 H22 0.858(9) . ? O22 C89 1.406(7) . ? N1 C8 1.252(7) . ? N1 C9 1.476(6) . ? N2 C11 1.481(6) . ? N2 C12 1.258(7) . ? N3 C27 1.276(7) . ? N3 C28 1.476(6) . ? N4 C30 1.465(6) . ? N4 C31 1.283(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.377(8) . ? C2 C7 1.401(7) . ? C3 H3 0.9300 . ? C3 C4 1.393(12) . ? C4 H4 0.9300 . ? C4 C5 1.346(12) . ? C5 H5 0.9300 . ? C5 C6 1.406(8) . ? C6 C7 1.411(7) . ? C6 C8 1.451(8) . ? C8 H8 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.508(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.502(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12 0.9300 . ? C12 C13 1.456(8) . ? C13 C14 1.413(7) . ? C13 C18 1.400(7) . ? C14 H14 0.9300 . ? C14 C15 1.368(10) . ? C15 H15 0.9300 . ? C15 C16 1.376(10) . ? C16 H16 0.9300 . ? C16 C17 1.374(7) . ? C17 C18 1.412(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.390(7) . ? C21 C26 1.393(6) . ? C22 H22A 0.9300 . ? C22 C23 1.392(9) . ? C23 H23 0.9300 . ? C23 C24 1.359(9) . ? C24 H24 0.9300 . ? C24 C25 1.414(7) . ? C25 C26 1.406(6) . ? C25 C27 1.455(7) . ? C27 H27 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.518(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.511(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31 0.9300 . ? C31 C32 1.448(7) . ? C32 C33 1.413(6) . ? C32 C37 1.401(6) . ? C33 H33 0.9300 . ? C33 C34 1.369(8) . ? C34 H34 0.9300 . ? C34 C35 1.382(8) . ? C35 H35 0.9300 . ? C35 C36 1.373(6) . ? C36 C37 1.403(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.394(6) . ? C39 C44 1.387(5) . ? C40 C41 1.538(5) . ? C41 C42 1.402(6) . ? C42 C43 1.388(6) . ? C43 C44 1.533(5) . ? C45 C46 1.401(5) . ? C45 C50 1.536(6) . ? C46 C47 1.378(6) . ? C47 C48 1.536(6) . ? C48 C49 1.387(6) . ? C49 C50 1.393(6) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? Cl1 O25 1.393(6) . ? Cl1 O26 1.368(6) . ? Cl1 O27 1.334(5) . ? Cl1 O28 1.383(6) . ? 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 O5 C21 C22 169.8(4) . . . . ? Dy1 O5 C21 C26 -10.9(5) . . . . ? Dy1 O6 C26 C21 7.6(6) . . . . ? Dy1 O6 C26 C25 -173.8(3) . . . . ? Dy1 O7 C37 C32 -175.4(3) . . . . ? Dy1 O7 C37 C36 3.6(5) . . . . ? Dy1 O8 C36 C35 175.9(4) . . . . ? Dy1 O8 C36 C37 -4.7(4) . . . . ? Dy1 O11 C44 C39 -174.8(4) . . . . ? Dy1 O11 C44 C43 4.4(5) . . . . ? Dy1 O12 C43 C42 176.8(3) . . . . ? Dy1 O12 C43 C44 -3.5(5) . . . . ? Dy1 O13 C45 C46 171.0(3) . . . . ? Dy1 O13 C45 C50 -9.3(4) . . . . ? Dy1 O14 C50 C45 7.6(4) . . . . ? Dy1 O14 C50 C49 -173.6(3) . . . . ? Dy1 O19 N5 O20 -31.2(6) . . . . ? Dy1 O19 N5 O21 148.8(4) . . . . ? Dy2 O1 C2 C3 -179.4(6) . . . . ? Dy2 O1 C2 C7 2.3(6) . . . . ? Dy2 O2 C7 C2 -7.5(6) . . . . ? Dy2 O2 C7 C6 176.2(4) . . . . ? Dy2 O3 C18 C13 168.6(3) . . . . ? Dy2 O3 C18 C17 -9.5(5) . . . . ? Dy2 O4 C17 C16 -166.6(4) . . . . ? Dy2 O4 C17 C18 14.2(5) . . . . ? Dy2 O9 C40 C39 -178.2(4) . . . . ? Dy2 O9 C40 C41 2.5(5) . . . . ? Dy2 O10 C41 C40 -5.1(6) . . . . ? Dy2 O10 C41 C42 175.2(4) . . . . ? Dy2 O15 C47 C46 164.9(3) 1_565 . . . ? Dy2 O15 C47 C48 -15.2(4) 1_565 . . . ? Dy2 O16 C48 C47 3.4(4) 1_565 . . . ? Dy2 O16 C48 C49 -177.5(3) 1_565 . . . ? Br1 C39 C40 O9 1.1(7) . . . . ? Br1 C39 C40 C41 -179.6(3) . . . . ? Br1 C39 C44 O11 -1.4(7) . . . . ? Br1 C39 C44 C43 179.4(3) . . . . ? Br2 C42 C43 O12 0.6(6) . . . . ? Br2 C42 C43 C44 -179.1(3) . . . . ? Br3 C46 C47 O15 -2.4(5) . . . . ? Br3 C46 C47 C48 177.7(3) . . . . ? Br4 C49 C50 O14 -0.1(6) . . . . ? Br4 C49 C50 C45 178.6(3) . . . . ? Zn1 O6 C26 C21 161.9(3) . . . . ? Zn1 O6 C26 C25 -19.5(6) . . . . ? Zn1 O7 C37 C32 25.7(5) . . . . ? Zn1 O7 C37 C36 -155.3(3) . . . . ? Zn1 O20 N5 O19 22.8(5) . . . . ? Zn1 O20 N5 O21 -157.2(3) . . . . ? Zn1 N3 C27 C25 4.5(7) . . . . ? Zn1 N3 C28 C29 34.8(5) . . . . ? Zn1 N4 C30 C29 -46.3(5) . . . . ? Zn1 N4 C31 C32 -2.1(7) . . . . ? Zn2 O2 C7 C2 -156.3(4) . . . . ? Zn2 O2 C7 C6 27.3(6) . . . . ? Zn2 O3 C18 C13 -20.7(6) . . . . ? Zn2 O3 C18 C17 161.2(3) . . . . ? Zn2 N1 C8 C6 -8.1(8) . . . . ? Zn2 N1 C9 C10 -30.4(6) . . . . ? Zn2 N2 C11 C10 37.0(6) . . . . ? Zn2 N2 C12 C13 7.5(8) . . . . ? O1 C2 C3 C4 -179.7(8) . . . . ? O1 C2 C7 O2 2.8(7) . . . . ? O1 C2 C7 C6 179.5(5) . . . . ? O4 C17 C18 O3 -4.6(6) . . . . ? O4 C17 C18 C13 177.2(4) . . . . ? O5 C21 C22 C23 177.3(5) . . . . ? O5 C21 C26 O6 3.3(6) . . . . ? O5 C21 C26 C25 -175.3(4) . . . . ? O8 C36 C37 O7 1.3(5) . . . . ? O8 C36 C37 C32 -179.6(4) . . . . ? O9 C40 C41 O10 1.6(6) . . . . ? O9 C40 C41 C42 -178.7(4) . . . . ? O10 C41 C42 Br2 -1.5(7) . . . . ? O10 C41 C42 C43 178.1(5) . . . . ? O12 C43 C44 O11 -0.5(6) . . . . ? O12 C43 C44 C39 178.8(4) . . . . ? O13 C45 C46 Br3 -2.9(5) . . . . ? O13 C45 C46 C47 179.4(4) . . . . ? O13 C45 C50 O14 1.2(5) . . . . ? O13 C45 C50 C49 -177.7(4) . . . . ? O15 C47 C48 O16 7.5(5) . . . . ? O15 C47 C48 C49 -171.7(4) . . . . ? O16 C48 C49 Br4 -2.6(6) . . . . ? O16 C48 C49 C50 174.3(4) . . . . ? N1 C9 C10 C11 72.0(6) . . . . ? N2 C12 C13 C14 -175.2(5) . . . . ? N2 C12 C13 C18 6.6(9) . . . . ? N3 C28 C29 C30 -70.8(5) . . . . ? N4 C31 C32 C33 168.4(5) . . . . ? N4 C31 C32 C37 -13.1(8) . . . . ? C1 O1 C2 C3 5.3(9) . . . . ? C1 O1 C2 C7 -173.0(5) . . . . ? C2 C3 C4 C5 1.9(17) . . . . ? C3 C2 C7 O2 -175.5(6) . . . . ? C3 C2 C7 C6 1.1(9) . . . . ? C3 C4 C5 C6 -1.7(17) . . . . ? C4 C5 C6 C7 1.3(13) . . . . ? C4 C5 C6 C8 176.8(9) . . . . ? C5 C6 C7 O2 175.4(6) . . . . ? C5 C6 C7 C2 -0.9(9) . . . . ? C5 C6 C8 N1 173.3(7) . . . . ? C7 C2 C3 C4 -1.6(13) . . . . ? C7 C6 C8 N1 -11.3(10) . . . . ? C8 N1 C9 C10 145.7(5) . . . . ? C8 C6 C7 O2 0.3(9) . . . . ? C8 C6 C7 C2 -176.1(5) . . . . ? C9 N1 C8 C6 175.8(5) . . . . ? C9 C10 C11 N2 -76.3(6) . . . . ? C11 N2 C12 C13 -175.1(5) . . . . ? C12 N2 C11 C10 -140.5(5) . . . . ? C12 C13 C14 C15 -176.9(6) . . . . ? C12 C13 C18 O3 0.8(7) . . . . ? C12 C13 C18 C17 178.9(5) . . . . ? C13 C14 C15 C16 -2.1(10) . . . . ? C14 C13 C18 O3 -177.4(5) . . . . ? C14 C13 C18 C17 0.7(7) . . . . ? C14 C15 C16 C17 0.8(10) . . . . ? C15 C16 C17 O4 -177.8(5) . . . . ? C15 C16 C17 C18 1.3(9) . . . . ? C16 C17 C18 O3 176.2(5) . . . . ? C16 C17 C18 C13 -2.0(7) . . . . ? C18 C13 C14 C15 1.3(8) . . . . ? C19 O4 C17 C16 -4.5(7) . . . . ? C19 O4 C17 C18 176.3(4) . . . . ? C20 O5 C21 C22 -9.8(7) . . . . ? C20 O5 C21 C26 169.6(4) . . . . ? C21 C22 C23 C24 -1.7(9) . . . . ? C22 C21 C26 O6 -177.3(4) . . . . ? C22 C21 C26 C25 4.0(7) . . . . ? C22 C23 C24 C25 3.2(9) . . . . ? C23 C24 C25 C26 -1.1(8) . . . . ? C23 C24 C25 C27 -177.6(5) . . . . ? C24 C25 C26 O6 179.0(4) . . . . ? C24 C25 C26 C21 -2.5(7) . . . . ? C24 C25 C27 N3 -170.5(5) . . . . ? C26 C21 C22 C23 -2.0(8) . . . . ? C26 C25 C27 N3 13.2(8) . . . . ? C27 N3 C28 C29 -143.6(4) . . . . ? C27 C25 C26 O6 -4.8(7) . . . . ? C27 C25 C26 C21 173.7(4) . . . . ? C28 N3 C27 C25 -177.2(4) . . . . ? C28 C29 C30 N4 78.6(5) . . . . ? C30 N4 C31 C32 179.1(4) . . . . ? C31 N4 C30 C29 132.6(5) . . . . ? C31 C32 C33 C34 178.9(5) . . . . ? C31 C32 C37 O7 -0.2(7) . . . . ? C31 C32 C37 C36 -179.2(4) . . . . ? C32 C33 C34 C35 0.9(8) . . . . ? C33 C32 C37 O7 178.3(4) . . . . ? C33 C32 C37 C36 -0.7(6) . . . . ? C33 C34 C35 C36 -1.7(8) . . . . ? C34 C35 C36 O8 -179.3(4) . . . . ? C34 C35 C36 C37 1.3(7) . . . . ? C35 C36 C37 O7 -179.2(4) . . . . ? C35 C36 C37 C32 -0.1(6) . . . . ? C37 C32 C33 C34 0.3(7) . . . . ? C38 O8 C36 C35 10.4(6) . . . . ? C38 O8 C36 C37 -170.1(4) . . . . ? C39 C40 C41 O10 -177.8(5) . . . . ? C39 C40 C41 C42 1.9(7) . . . . ? C40 C39 C44 O11 -178.8(5) . . . . ? C40 C39 C44 C43 2.0(7) . . . . ? C40 C41 C42 Br2 178.9(3) . . . . ? C40 C41 C42 C43 -1.6(7) . . . . ? C41 C42 C43 O12 -179.0(4) . . . . ? C41 C42 C43 C44 1.4(7) . . . . ? C42 C43 C44 O11 179.2(4) . . . . ? C42 C43 C44 C39 -1.6(6) . . . . ? C44 C39 C40 O9 178.5(5) . . . . ? C44 C39 C40 C41 -2.2(7) . . . . ? C45 C46 C47 O15 175.3(4) . . . . ? C45 C46 C47 C48 -4.7(5) . . . . ? C46 C45 C50 O14 -179.1(3) . . . . ? C46 C45 C50 C49 2.0(5) . . . . ? C46 C47 C48 O16 -172.6(3) . . . . ? C46 C47 C48 C49 8.2(5) . . . . ? C47 C48 C49 Br4 176.5(3) . . . . ? C47 C48 C49 C50 -6.6(6) . . . . ? C48 C49 C50 O14 -177.1(4) . . . . ? C48 C49 C50 C45 1.7(6) . . . . ? C50 C45 C46 Br3 177.4(3) . . . . ? C50 C45 C46 C47 -0.3(5) . . . . ? 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 -0.468 0.000 0.500 292.8 77.0 ? 2 0.317 0.340 -0.033 70.7 13.9 ? 3 0.683 0.660 0.033 70.7 13.2 ?