#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:30:59 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270479 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060986.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_7060986 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 Cl4 Dy2 N5 O22 Zn2, 0.5(Cl O4)' _chemical_formula_sum 'C53 H52 Cl4.5 Dy2 N5 O24 Zn2' _chemical_formula_weight 1758.26 _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 90.1020(10) _cell_angle_beta 100.5900(10) _cell_angle_gamma 99.6450(10) _cell_formula_units_Z 2 _cell_length_a 11.58000(10) _cell_length_b 14.76280(10) _cell_length_c 19.97170(10) _cell_measurement_reflns_used 56739 _cell_measurement_temperature 219.99(16) _cell_measurement_theta_max 74.6320 _cell_measurement_theta_min 2.2470 _cell_volume 3306.77(4) _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _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 219.99(16) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 36.00 106.00 0.50 0.50 -- 47.57 28.00 81.00 140 2 \w 94.00 120.00 0.50 2.00 -- 103.25 28.00 81.00 52 3 \w 37.00 118.00 0.50 0.50 -- 47.57 38.00 150.00 162 4 \w 48.00 74.00 0.50 0.50 -- 70.00 76.00 89.18 52 5 \w 44.00 69.00 0.50 0.50 -- 66.00 78.00 48.06 50 6 \w 38.00 65.00 0.50 0.50 -- 62.00 80.00 -2.67 54 7 \w 44.00 69.00 0.50 0.50 -- 66.00 78.00 -39.18 50 8 \w 43.00 69.00 0.50 0.50 -- 66.00 78.00 21.78 52 9 \w 44.00 69.00 0.50 0.50 -- 66.00 78.00 64.67 50 10 \w 31.00 56.00 0.50 0.50 -- 54.00 80.00 106.77 50 11 \w 34.00 60.00 0.50 0.50 -- 58.00 79.00 132.45 52 12 \w 39.00 72.00 0.50 0.50 -- 62.00 79.00 154.57 66 13 \w 15.00 40.00 0.50 0.50 -- 42.00 87.00 46.01 50 14 \w 8.00 33.00 0.50 0.50 -- 38.00 92.00 91.85 50 15 \w -24.00 4.00 0.50 0.50 -- 10.00 103.00 -23.98 56 16 \w -8.00 27.00 0.50 0.50 -- 22.00 97.00 -85.86 70 17 \w 15.00 40.00 0.50 0.50 -- 42.00 87.00 -43.84 50 18 \w 31.00 56.00 0.50 0.50 -- 54.00 79.00 -43.65 50 19 \w 26.00 89.00 0.50 0.50 -- 50.00 80.00 -84.56 126 20 \w 88.00 138.00 0.50 0.50 -- 66.00 79.00-118.20 100 21 \w 90.00 115.00 0.50 0.50 -- 66.00 79.00-153.44 50 22 \w 61.00 88.00 0.50 2.00 -- 82.00 73.00-106.20 54 23 \w 38.00 78.00 0.50 0.50 -- 62.00 80.00-171.54 80 24 \w 42.00 80.00 0.50 0.50 -- 66.00 79.00-118.20 76 25 \w 42.00 68.00 0.50 0.50 -- 66.00 79.00-153.44 52 26 \w 13.00 38.00 0.50 0.50 -- 42.00 91.00-163.26 50 27 \w -8.00 25.00 0.50 0.50 -- 22.00 98.00-169.27 66 28 \w -19.00 6.00 0.50 0.50 -- 47.57 -28.00 -80.00 50 29 \w 34.00 60.00 0.50 2.00 -- 103.25 -94.00-150.00 52 30 \w 80.00 106.00 0.50 2.00 -- 103.25 -94.00-150.00 52 31 \w 76.00 105.00 0.50 2.00 -- 103.25 -94.00 -90.00 58 32 \w 68.00 99.00 0.50 2.00 -- 103.25 -94.00 0.00 62 33 \w 47.00 73.00 0.50 2.00 -- 103.25 -94.00 -90.00 52 34 \w 45.00 72.00 0.50 2.00 -- 103.25 -61.00-120.00 54 35 \w 33.00 98.00 0.50 2.00 -- 103.25 -94.00 -30.00 130 36 \w 56.00 111.00 0.50 2.00 -- 103.25-125.00 90.00 110 37 \w 32.00 103.00 0.50 2.00 -- 103.25-125.00 120.00 142 38 \w 38.00 73.00 0.50 2.00 -- 103.25 -61.00 150.00 70 39 \w 32.00 109.00 0.50 2.00 -- 103.25 -77.00 90.00 154 40 \w 32.00 77.00 0.50 2.00 -- 103.25 -77.00 0.00 90 41 \w 33.00 59.00 0.50 2.00 -- 103.25 -94.00 0.00 52 42 \w 33.00 66.00 0.50 2.00 -- 103.25 -61.00 30.00 66 43 \w 20.00 92.00 0.50 0.50 -- 47.57-125.00 0.00 144 44 \w -24.00 25.00 0.50 0.50 -- -47.57 28.00 81.00 98 45 \w -52.00 -25.00 0.50 0.50 -- -47.57 -77.00 60.00 54 46 \w -56.00 -30.00 0.50 0.50 -- -54.00 -79.00 18.61 52 47 \w -64.00 -30.00 0.50 0.50 -- -54.00 -79.00 -10.63 68 48 \w -80.00 -51.00 0.50 0.50 -- -47.57 -28.00 -80.00 58 49 \w -61.00 24.00 0.50 0.50 -- -47.57 57.00-120.00 170 50 \w -68.00 -42.00 0.50 2.00 -- -99.00 61.00-180.00 52 51 \w -112.00 -76.00 0.50 2.00 -- -99.00 125.00 -60.00 72 52 \w -93.00 -57.00 0.50 2.00 -- -99.00 77.00 -30.00 72 53 \w -125.00 -91.00 0.50 2.00 -- -99.00 144.00 51.21 68 54 \w -68.00 -26.00 0.50 2.00 -- -99.00 125.00 120.00 84 55 \w -68.00 -41.00 0.50 2.00 -- -99.00 153.00 160.36 54 56 \w -108.00 -45.00 0.50 2.00 -- -99.00 120.00 179.06 126 57 \w -112.00 -79.00 0.50 2.00 -- -99.00 125.00 120.00 66 58 \w -131.00 -73.00 0.50 2.00 -- -99.00 153.00 160.36 116 59 \w -69.00 -44.00 0.50 0.50 -- 6.00 167.00 122.35 50 60 \w -118.00 -82.00 0.50 0.50 -- -47.57 -28.00 -80.00 72 61 \w -89.00 -53.00 0.50 2.00 -- -74.00 -72.00 -80.44 72 62 \w -60.00 -35.00 0.50 0.50 -- -58.00 -77.00-102.89 50 63 \w -55.00 -30.00 0.50 0.50 -- -54.00 -80.00-116.52 50 64 \w -61.00 -34.00 0.50 0.50 -- -58.00 -80.00-153.76 54 65 \w -81.00 -47.00 0.50 0.50 -- -70.00 -76.00-134.96 68 66 \w -83.00 -48.00 0.50 0.50 -- -70.00 -75.00 -96.42 70 67 \w -79.00 -52.00 0.50 2.00 -- -74.00 -74.00 -50.12 54 68 \w -78.00 -52.00 0.50 2.00 -- -74.00 -74.00 -25.01 52 69 \w -78.00 -52.00 0.50 2.00 -- -74.00 -74.00 25.20 52 70 \w -76.00 -50.00 0.50 2.00 -- -74.00 -80.00 15.46 52 71 \w -83.00 -57.00 0.50 2.00 -- -78.00 -73.00 68.63 52 72 \w -73.00 -47.00 0.50 0.50 -- -70.00 -76.00 130.37 52 73 \w -81.00 -54.00 0.50 2.00 -- -78.00 -79.00 135.43 54 74 \w -86.00 -60.00 0.50 2.00 -- -82.00 -75.00 167.35 52 75 \w -88.00 -58.00 0.50 2.00 -- -82.00 -79.00 120.80 60 76 \w -91.00 -65.00 0.50 2.00 -- -86.00 -72.00 70.95 52 77 \w -90.00 -64.00 0.50 2.00 -- -86.00 -75.00 19.19 52 78 \w -87.00 -61.00 0.50 2.00 -- -82.00 -73.00 -3.78 52 79 \w -90.00 -64.00 0.50 2.00 -- -86.00 -75.00 -16.99 52 80 \w -93.00 -67.00 0.50 2.00 -- -90.00 -77.00 -21.87 52 81 \w -86.00 -57.00 0.50 2.00 -- -78.00 -72.00 -96.74 58 82 \w -82.00 -56.00 0.50 2.00 -- -78.00 -74.00-150.67 52 83 \w -83.00 -56.00 0.50 2.00 -- -78.00 -74.00-160.99 54 84 \w -85.00 -60.00 0.50 2.00 -- -82.00 -75.00-178.26 50 85 \w -89.00 -56.00 0.50 2.00 -- -78.00 -74.00-138.94 66 86 \w -89.00 -60.00 0.50 2.00 -- -82.00 -74.00-103.21 58 87 \w -100.00 -75.00 0.50 2.00 -- -94.00 -67.00-123.44 50 88 \w -112.00 -76.00 0.50 2.00 -- -94.00 -65.00-139.49 72 89 \w -140.00 -70.00 0.50 2.00 -- -94.00 -80.00 -46.45 140 90 \w -103.00 -67.00 0.50 2.00 -- -90.00 -76.00 2.57 72 91 \w -90.00 -64.00 0.50 2.00 -- -86.00 -74.00 61.32 52 92 \w -93.00 -65.00 0.50 2.00 -- -86.00 -74.00 100.84 56 93 \w -97.00 -66.00 0.50 2.00 -- -86.00 -73.00 179.24 62 94 \w -96.00 -71.00 0.50 2.00 -- -94.00 -76.00 179.85 50 95 \w -120.00 -68.00 0.50 2.00 -- -90.00 -74.00 41.69 104 96 \w -120.00 -73.00 0.50 2.00 -- -94.00 -72.00 -16.13 94 97 \w -139.00-101.00 0.50 2.00 -- -86.00 -75.00 19.19 76 98 \w -158.00-110.00 0.50 2.00 -- -86.00 -74.00 61.32 96 99 \w -150.00-125.00 0.50 2.00 -- -90.00 -74.00 41.69 50 100 \w -155.00-114.00 0.50 2.00 -- -90.00 -76.00 2.57 82 101 \w -148.00 -66.00 0.50 2.00 -- -90.00 -80.00 -37.25 164 102 \w -147.00 -71.00 0.50 2.00 -- -94.00 -77.00 -83.25 152 103 \w -162.00-127.00 0.50 2.00 -- -99.00 -28.00 -80.00 70 104 \w -162.00 -75.00 0.50 2.00 -- -90.00 -66.00-111.86 174 105 \w -162.00-114.00 0.50 2.00 -- -90.00 -77.00 -21.87 96 106 \w -158.00 -67.00 0.50 2.00 -- -90.00 -77.00 55.75 182 107 \w -143.00-117.00 0.50 2.00 -- -94.00 -76.00 179.85 52 108 \w -152.00 -71.00 0.50 2.00 -- -94.00 -77.00 139.35 162 109 \w -160.00 -68.00 0.50 2.00 -- -90.00 -74.00 14.69 184 110 \w -164.00-128.00 0.50 2.00 -- -94.00 -72.00 -16.13 72 111 \w -168.00 -75.00 0.50 2.00 -- -99.00 -80.00 -91.10 186 112 \w -166.00-127.00 0.50 2.00 -- -94.00 -67.00-123.44 78 113 \w -166.00 -74.00 0.50 2.00 -- -94.00 -70.00-156.61 184 114 \w -167.00 -71.00 0.50 2.00 -- -94.00 -77.00-135.00 192 115 \w -168.00 -75.00 0.50 2.00 -- -99.00 -79.00 103.53 186 116 \w -166.00 -79.00 0.50 2.00 -- -99.00 -75.00 171.75 174 117 \w -165.00 -75.00 0.50 2.00 -- -99.00 -79.00 113.13 180 118 \w -167.00 -79.00 0.50 2.00 -- -99.00 -70.00 157.25 176 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0681494000 _diffrn_orient_matrix_UB_12 -0.0768923000 _diffrn_orient_matrix_UB_13 0.0285357000 _diffrn_orient_matrix_UB_21 -0.1192603000 _diffrn_orient_matrix_UB_22 -0.0646169000 _diffrn_orient_matrix_UB_23 -0.0002418000 _diffrn_orient_matrix_UB_31 -0.0005495000 _diffrn_orient_matrix_UB_32 -0.0336036000 _diffrn_orient_matrix_UB_33 -0.0731489000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 112669 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.338 _diffrn_reflns_theta_min 2.252 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 15.061 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.46994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour dark _exptl_crystal_density_diffrn 1.766 _exptl_crystal_description block _exptl_crystal_F_000 1731 _exptl_crystal_preparation 'Magnetic properties' _refine_diff_density_max 2.447 _refine_diff_density_min -1.589 _refine_diff_density_rms 0.135 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 837 _refine_ls_number_reflns 13098 _refine_ls_number_restraints 40 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0611 _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^)+(0.1031P)^2^+7.9475P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1666 _refine_ls_wR_factor_ref 0.1720 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11192 _reflns_number_total 13098 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04299h2.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 7060986--7060987.cif.' _cod_original_cell_volume 3306.76(4) _cod_original_formula_sum 'C53 H52 Cl4.50 Dy2 N5 O24 Zn2' _cod_database_code 7060986 _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. ; _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, H22 of O22, H8 of O8, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, H21 of O21 2. Restrained distances O21-H21 0.85 with sigma of 0.01 O8-C32 1.43 with sigma of 0.01 C53-H21 1.950919 with sigma of 0.02 Dy2-H21 3.11378 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O27) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4. Others Fixed Sof: Cl5(0.5) O24(0.5) O25(0.5) O26(0.5) O27(0.5) 5.a Riding coordinates: O8(H8), O21(H21), O22(H22) 5.b : Cl5(O24,O25,O26,O27) 5.c Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B) 5.d Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C8(H8A), C12(H12), C14(H14), C15(H15), C16(H16), C35(H35), C36(H36), C37(H37), C40(H40), C44(H44), C46(H46), C47(H47), C48(H48) 5.e Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,H33B, H33C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL tx5448a_a.res in P-1 1.res created by SHELXL-2018/3 at 18:57:47 on 02-Sep-2021 REM Old TITL TX5448A in P-1 REM SHELXT solution in P-1: R1 0.244, Rweak 0.016, Alpha 0.089 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C107 N10 O58 I4 CELL 1.54184 11.58 14.7628 19.9717 90.102 100.59 99.645 ZERR 2 0.0001 0.0001 0.0001 0.001 0.001 0.001 LATT 1 SFAC C H Cl Dy N O Zn UNIT 106 104 9 4 10 48 4 DFIX 0.85 0.01 O21 H21 DFIX 1.43 0.01 O8 C32 DANG 1.950919 0.02 C53 H21 DANG 3.11378 0.02 Dy2 H21 ISOR 0.005 0.01 O27 O26 O25 Cl5 O24 C32 L.S. 20 PLAN 8 CONF BOND LIST 4 MORE -1 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.103100 7.947500 FVAR 0.21334 DY1 4 0.141502 0.110981 0.288544 11.00000 0.04058 0.03377 = 0.05313 0.00008 0.01476 0.00240 DY2 4 0.521523 0.661073 0.245764 11.00000 0.03710 0.03513 = 0.06222 -0.00274 0.01712 0.00148 ZN1 7 -0.141853 0.105770 0.319936 11.00000 0.04230 0.06608 = 0.06082 0.00139 0.01277 0.00256 ZN2 7 0.811229 0.649239 0.220637 11.00000 0.03881 0.05028 = 0.06405 -0.00352 0.01529 0.00192 CL1 3 0.262668 -0.109471 0.107274 11.00000 0.08459 0.07581 = 0.04588 -0.00044 0.01312 0.02634 CL2 3 0.393150 -0.123676 0.430083 11.00000 0.08520 0.09391 = 0.04679 0.00260 0.01401 0.04240 CL3 3 0.550187 0.299767 0.235493 11.00000 0.06287 0.04834 = 0.13272 0.00600 0.05069 0.01647 CL4 3 0.116355 0.471280 0.303160 11.00000 0.05648 0.04842 = 0.11453 0.00261 0.04078 0.01501 O1 6 0.106045 0.170267 0.167338 11.00000 0.09911 0.05433 = 0.05553 0.01196 0.03126 0.01459 O2 6 -0.052783 0.123767 0.241604 11.00000 0.04675 0.05099 = 0.04967 0.00994 0.00262 0.00707 O3 6 0.027678 0.105804 0.370354 11.00000 0.04756 0.04881 = 0.04457 -0.00554 0.00973 0.00908 O4 6 0.250877 0.169824 0.410341 11.00000 0.04543 0.05636 = 0.06007 -0.01095 0.00088 0.00964 O5 6 -0.161638 -0.049412 0.289306 11.00000 0.06546 0.06220 = 0.07280 -0.00393 0.02812 0.00947 O6 6 0.022315 -0.049721 0.274390 11.00000 0.04733 0.03842 = 0.09246 -0.00948 0.02100 -0.00077 O7 6 -0.121434 -0.163758 0.239299 11.00000 0.08688 0.04619 = 0.13811 -0.02258 0.01814 0.00410 O8 6 -0.103597 0.257696 0.329645 11.00000 0.09556 0.06342 = 0.13876 -0.02296 0.01106 0.00734 AFIX 3 0.8500 H8 2 -0.028667 0.270976 0.331755 11.00000 -1.20000 AFIX 0 O9 6 0.321631 0.201718 0.272623 11.00000 0.04806 0.02914 = 0.08496 0.00088 0.02625 0.00477 O10 6 0.142496 0.273172 0.297886 11.00000 0.04716 0.02981 = 0.07607 0.00032 0.02325 0.00594 O11 6 0.523911 0.497190 0.238693 11.00000 0.03714 0.03912 = 0.08088 0.00025 0.02487 0.00297 O12 6 0.341834 0.568762 0.260858 11.00000 0.04074 0.03233 = 0.09637 0.00034 0.02491 0.00201 O13 6 0.215196 0.018179 0.213621 11.00000 0.05798 0.04491 = 0.05503 0.00589 0.01316 0.01546 O14 6 0.259340 0.006863 0.345699 11.00000 0.05076 0.04629 = 0.05483 -0.00780 0.01428 0.01284 O15 6 0.386628 -0.244174 0.192109 11.00000 0.04779 0.03849 = 0.06108 -0.00884 0.00939 0.00893 O16 6 0.457524 -0.241106 0.323384 11.00000 0.06160 0.04677 = 0.05618 0.00255 0.01758 0.01665 O17 6 0.552148 0.607419 0.367685 11.00000 0.08223 0.05953 = 0.06344 0.01009 0.03904 0.01862 O18 6 0.716440 0.654914 0.296997 11.00000 0.05323 0.04978 = 0.04399 0.00194 0.01102 0.00713 O19 6 0.643924 0.652946 0.167657 11.00000 0.04072 0.04911 = 0.04797 -0.00314 0.00943 0.00407 O20 6 0.419888 0.606643 0.123764 11.00000 0.04454 0.06572 = 0.06535 -0.02044 -0.00014 0.01532 O21 6 0.626187 0.820545 0.233876 11.00000 0.05360 0.04096 = 0.08248 -0.00525 0.02346 -0.00833 AFIX 3 H21 2 0.691027 0.847575 0.259746 11.00000 -1.50000 AFIX 0 O22 6 0.774778 0.504669 0.219802 11.00000 0.08186 0.05179 = 0.11962 -0.01308 0.03417 0.01037 AFIX 3 0.8500 H22 2 0.699308 0.491449 0.214832 11.00000 -1.20000 AFIX 0 N1 5 -0.301448 0.101961 0.254655 11.00000 0.04677 0.04551 = 0.09688 -0.00467 -0.00076 0.00867 N2 5 -0.203031 0.067484 0.406732 11.00000 0.05412 0.05119 = 0.08262 -0.00995 0.03468 0.00250 N3 5 -0.084209 -0.085732 0.267838 11.00000 0.06111 0.04758 = 0.05757 0.00147 0.01237 0.00392 N4 5 0.966240 0.667986 0.290091 11.00000 0.04256 0.04452 = 0.10453 -0.00392 0.00717 0.00520 N5 5 0.879182 0.684917 0.136140 11.00000 0.06350 0.04733 = 0.08263 -0.00740 0.03935 -0.00298 C1 1 0.189674 0.182180 0.121959 11.00000 0.11485 0.08255 = 0.07656 0.02117 0.05390 0.00572 AFIX 137 H1A 2 0.262107 0.162467 0.143379 11.00000 -1.50000 H1B 2 0.206474 0.245884 0.111365 11.00000 -1.50000 H1C 2 0.156427 0.146163 0.080752 11.00000 -1.50000 AFIX 0 C2 1 -0.009576 0.187630 0.140986 11.00000 0.10379 0.05480 = 0.04914 0.01258 0.01415 0.03113 C3 1 -0.042984 0.228400 0.080153 11.00000 0.15500 0.09118 = 0.06263 0.02154 0.03119 0.03285 AFIX 43 H3 2 0.013630 0.247928 0.053379 11.00000 -1.20000 AFIX 0 C4 1 -0.157044 0.240430 0.058810 11.00000 0.16009 0.13154 = 0.05658 0.02182 0.00246 0.08707 AFIX 43 H4 2 -0.178021 0.270671 0.018741 11.00000 -1.20000 AFIX 0 C5 1 -0.240855 0.207877 0.096506 11.00000 0.12369 0.08615 = 0.07409 -0.00586 -0.02090 0.04899 AFIX 43 H5 2 -0.320063 0.212118 0.079574 11.00000 -1.20000 AFIX 0 C6 1 -0.212419 0.168146 0.159951 11.00000 0.09024 0.05485 = 0.06280 -0.01034 -0.01668 0.03636 C7 1 -0.091879 0.160036 0.183062 11.00000 0.08235 0.03054 = 0.05441 -0.00171 -0.00201 0.00877 C8 1 -0.306993 0.132206 0.195774 11.00000 0.06442 0.05695 = 0.08551 -0.01543 -0.01347 0.02020 AFIX 43 H8A 2 -0.383764 0.131396 0.171391 11.00000 -1.20000 AFIX 0 C9 1 -0.412451 0.064085 0.276342 11.00000 0.04181 0.05849 = 0.14695 -0.00629 0.00356 0.00947 AFIX 23 H9A 2 -0.428795 -0.001924 0.267683 11.00000 -1.20000 H9B 2 -0.477093 0.089732 0.249398 11.00000 -1.20000 AFIX 0 C10 1 -0.409118 0.084026 0.351671 11.00000 0.05357 0.06446 = 0.15116 -0.03659 0.03963 -0.00226 AFIX 23 H10A 2 -0.489746 0.070122 0.360464 11.00000 -1.20000 H10B 2 -0.380870 0.149189 0.361439 11.00000 -1.20000 AFIX 0 C11 1 -0.330180 0.030053 0.400439 11.00000 0.06929 0.06726 = 0.11512 -0.01979 0.05677 -0.01046 AFIX 23 H11A 2 -0.351860 0.031160 0.445056 11.00000 -1.20000 H11B 2 -0.344577 -0.033521 0.384158 11.00000 -1.20000 AFIX 0 C12 1 -0.139689 0.077801 0.466704 11.00000 0.10308 0.04827 = 0.06577 -0.00892 0.04698 0.00053 AFIX 43 H12 2 -0.179232 0.061146 0.502514 11.00000 -1.20000 AFIX 0 C13 1 -0.013815 0.112395 0.484823 11.00000 0.08466 0.04009 = 0.05214 0.00054 0.02076 0.00590 C14 1 0.036301 0.133252 0.554846 11.00000 0.12883 0.06286 = 0.04614 0.00296 0.03122 0.01437 AFIX 43 H14 2 -0.012926 0.123697 0.586991 11.00000 -1.20000 AFIX 0 C15 1 0.153435 0.166542 0.575805 11.00000 0.13278 0.06535 = 0.04912 -0.00557 0.00114 -0.00143 AFIX 43 H15 2 0.182822 0.181416 0.621733 11.00000 -1.20000 AFIX 0 C16 1 0.230584 0.178856 0.529671 11.00000 0.09276 0.05839 = 0.05599 -0.00059 -0.00338 0.00409 AFIX 43 H16 2 0.311588 0.200198 0.544399 11.00000 -1.20000 AFIX 0 C17 1 0.184626 0.158810 0.461716 11.00000 0.06525 0.03689 = 0.05099 -0.00107 0.00261 0.01002 C18 1 0.063387 0.125002 0.437778 11.00000 0.07111 0.03592 = 0.04411 0.00149 0.01099 0.01407 C19 1 0.378735 0.191556 0.432357 11.00000 0.04589 0.11468 = 0.08622 -0.01695 -0.00627 0.00539 AFIX 137 H19A 2 0.404766 0.146633 0.463699 11.00000 -1.50000 H19B 2 0.399601 0.251398 0.454461 11.00000 -1.50000 H19C 2 0.416753 0.191069 0.393533 11.00000 -1.50000 AFIX 0 C20 1 0.333246 0.288770 0.269094 11.00000 0.04381 0.03867 = 0.06435 0.00146 0.01472 0.00253 C21 1 0.431082 0.346199 0.252584 11.00000 0.04767 0.03871 = 0.07374 -0.00210 0.02075 0.01011 C22 1 0.437184 0.440288 0.251079 11.00000 0.03951 0.03066 = 0.06677 -0.00153 0.01771 -0.00011 C23 1 0.331225 0.483341 0.266212 11.00000 0.03922 0.03204 = 0.07010 -0.00428 0.01576 0.00410 C24 1 0.234073 0.425529 0.283906 11.00000 0.03803 0.03799 = 0.07509 -0.00002 0.02057 0.00393 C25 1 0.228788 0.330453 0.285001 11.00000 0.03930 0.03697 = 0.05929 -0.00293 0.01149 0.00374 C26 1 0.266243 -0.046819 0.235746 11.00000 0.04254 0.03901 = 0.05029 -0.00176 0.01226 -0.00318 C27 1 0.300726 -0.111673 0.195405 11.00000 0.04683 0.04513 = 0.04539 -0.00521 0.00980 0.00365 C28 1 0.359068 -0.180180 0.224689 11.00000 0.03277 0.04097 = 0.05479 -0.00348 0.01345 -0.00034 C29 1 0.395460 -0.181812 0.301875 11.00000 0.03484 0.03801 = 0.05949 0.00294 0.01638 0.00208 C30 1 0.357617 -0.119411 0.342161 11.00000 0.04576 0.04565 = 0.04876 -0.00133 0.01145 0.01340 C31 1 0.294597 -0.052385 0.312956 11.00000 0.03501 0.03773 = 0.05814 -0.00310 0.01439 0.00109 C32 1 -0.126464 0.318287 0.376034 11.00000 0.15108 0.14633 = 0.16454 -0.01875 0.05156 0.02380 AFIX 137 H32A 2 -0.148742 0.371549 0.353029 11.00000 -1.50000 H32B 2 -0.056224 0.336498 0.410203 11.00000 -1.50000 H32C 2 -0.190374 0.289066 0.397220 11.00000 -1.50000 AFIX 0 C33 1 0.460348 0.595509 0.409663 11.00000 0.13775 0.09496 = 0.08005 0.00490 0.05850 -0.00466 AFIX 137 H33A 2 0.485513 0.636374 0.449009 11.00000 -1.50000 H33B 2 0.447802 0.533143 0.423953 11.00000 -1.50000 H33C 2 0.387337 0.609175 0.383644 11.00000 -1.50000 AFIX 0 C34 1 0.667087 0.597319 0.398306 11.00000 0.09330 0.06468 = 0.05648 0.01554 0.02050 0.02004 C35 1 0.695009 0.564369 0.462369 11.00000 0.15691 0.12962 = 0.08011 0.05165 0.03547 0.02677 AFIX 43 H35 2 0.635207 0.546336 0.487345 11.00000 -1.20000 AFIX 0 C36 1 0.811945 0.557881 0.489954 11.00000 0.17886 0.20577 = 0.09226 0.07820 0.00891 0.07822 AFIX 43 H36 2 0.830691 0.536313 0.533658 11.00000 -1.20000 AFIX 0 C37 1 0.900874 0.583380 0.452695 11.00000 0.12309 0.16155 = 0.09317 0.04330 -0.03300 0.03259 AFIX 43 H37 2 0.979579 0.579454 0.471240 11.00000 -1.20000 AFIX 0 C38 1 0.870810 0.615931 0.385226 11.00000 0.09113 0.07184 = 0.07347 0.01479 0.00087 0.02445 C39 1 0.751808 0.623028 0.358628 11.00000 0.07269 0.04800 = 0.05418 0.00171 -0.00310 0.01086 C40 1 0.970246 0.646414 0.351748 11.00000 0.06169 0.05632 = 0.10121 -0.00009 -0.01665 0.01473 AFIX 43 H40 2 1.045828 0.650696 0.378496 11.00000 -1.20000 AFIX 0 C41 1 1.080439 0.701262 0.269107 11.00000 0.04177 0.04914 = 0.15658 -0.00408 0.00482 0.00009 AFIX 23 H41A 2 1.143455 0.677708 0.299291 11.00000 -1.20000 H41B 2 1.097434 0.767839 0.273455 11.00000 -1.20000 AFIX 0 C42 1 1.079893 0.672034 0.196592 11.00000 0.04847 0.06365 = 0.16149 -0.02804 0.04437 -0.00187 AFIX 23 H42A 2 1.161591 0.682095 0.189381 11.00000 -1.20000 H42B 2 1.050222 0.606485 0.191086 11.00000 -1.20000 AFIX 0 C43 1 1.007457 0.719687 0.142150 11.00000 0.05632 0.07164 = 0.12453 -0.01083 0.05005 -0.00398 AFIX 23 H43A 2 1.023138 0.785232 0.152826 11.00000 -1.20000 H43B 2 1.031092 0.710195 0.098874 11.00000 -1.20000 AFIX 0 C44 1 0.818501 0.676517 0.075037 11.00000 0.08732 0.05851 = 0.07025 -0.00561 0.04988 -0.00504 AFIX 43 H44 2 0.861513 0.688239 0.040077 11.00000 -1.20000 AFIX 0 C45 1 0.690520 0.650798 0.054768 11.00000 0.08557 0.04990 = 0.05890 0.00051 0.03076 -0.00058 C46 1 0.642507 0.637359 -0.016104 11.00000 0.13165 0.06485 = 0.05870 0.00542 0.03597 0.00249 AFIX 43 H46 2 0.694176 0.642230 -0.046985 11.00000 -1.20000 AFIX 0 C47 1 0.522258 0.617456 -0.039942 11.00000 0.12900 0.08074 = 0.05234 0.00229 0.00257 0.01544 AFIX 43 H47 2 0.493235 0.610746 -0.086611 11.00000 -1.20000 AFIX 0 C48 1 0.443619 0.607259 0.004986 11.00000 0.09599 0.07552 = 0.05861 -0.00478 -0.00751 0.02043 AFIX 43 H48 2 0.361879 0.592953 -0.011123 11.00000 -1.20000 AFIX 0 C49 1 0.488190 0.618631 0.074287 11.00000 0.07101 0.04790 = 0.05756 -0.00679 -0.00312 0.01284 C50 1 0.611031 0.640539 0.100822 11.00000 0.06537 0.03642 = 0.05048 -0.00375 0.01485 0.00823 C51 1 0.292516 0.587704 0.100724 11.00000 0.04973 0.09872 = 0.09699 -0.04198 -0.01310 0.01788 AFIX 137 H51A 2 0.253543 0.595607 0.138279 11.00000 -1.50000 H51B 2 0.269067 0.525601 0.082841 11.00000 -1.50000 H51C 2 0.270100 0.629289 0.065705 11.00000 -1.50000 AFIX 0 C52 1 0.804967 0.441680 0.177395 11.00000 0.07168 0.07680 = 0.15998 -0.03981 0.02288 0.01279 AFIX 137 H52A 2 0.745123 0.430524 0.136721 11.00000 -1.50000 H52B 2 0.810073 0.385122 0.200507 11.00000 -1.50000 H52C 2 0.880623 0.465745 0.165569 11.00000 -1.50000 AFIX 0 C53 1 0.619733 0.862281 0.166380 11.00000 0.09434 0.08086 = 0.09571 -0.00050 0.03349 0.00234 AFIX 137 H53A 2 0.541704 0.842814 0.139485 11.00000 -1.50000 H53B 2 0.678294 0.843093 0.143720 11.00000 -1.50000 H53C 2 0.635009 0.928048 0.172085 11.00000 -1.50000 AFIX 9 PART -1 CL5 3 -0.001854 0.485898 0.019456 10.50000 0.08948 0.09481 = 0.11958 -0.02851 0.00022 -0.00795 O24 6 -0.012503 0.437184 -0.045741 10.50000 0.21711 0.21445 = 0.20887 -0.04730 0.06825 0.04460 O25 6 -0.117266 0.481440 0.037055 10.50000 0.11582 0.15288 = 0.14514 -0.02283 0.02569 0.02188 O26 6 0.043681 0.579045 0.014514 10.50000 0.12800 0.10734 = 0.12383 -0.00538 0.02089 0.01090 O27 6 0.069305 0.444675 0.074677 10.50000 0.16399 0.17050 = 0.19195 0.01639 0.01606 0.00671 AFIX 0 HKLF 4 REM tx5448a_a.res in P-1 REM wR2 = 0.1720, GooF = S = 1.024, Restrained GooF = 1.032 for all data REM R1 = 0.0611 for 11192 Fo > 4sig(Fo) and 0.0682 for all 13098 data REM 837 parameters refined using 40 restraints END WGHT 0.1031 7.9483 REM Highest difference peak 2.447, deepest hole -1.589, 1-sigma level 0.135 Q1 1 0.5269 0.6547 0.2888 11.00000 0.05 2.45 Q2 1 0.1242 0.1180 0.2456 11.00000 0.05 2.43 Q3 1 0.1487 0.0995 0.3385 11.00000 0.05 1.39 Q4 1 0.2164 0.0996 0.2910 11.00000 0.05 1.38 Q5 1 -0.1605 0.1180 0.2802 11.00000 0.05 1.22 Q6 1 0.5081 0.6717 0.1958 11.00000 0.05 1.14 Q7 1 0.1161 0.1174 0.3235 11.00000 0.05 1.12 Q8 1 0.8137 0.6396 0.2695 11.00000 0.05 1.04 ; _shelx_res_checksum 24660 _shelx_fab_file ; -14 -1 5 -0.0867 0.0695 -14 0 3 -0.3039 -0.4885 -14 0 4 -0.0542 0.2108 -14 0 5 -0.7831 -0.3560 -14 0 6 -0.6277 -0.1483 -14 0 7 -1.5391 -0.0804 -14 0 8 0.2232 0.1844 -14 1 1 0.6201 2.7973 -14 1 2 1.1839 0.6503 -14 1 3 -0.2239 0.6082 -14 1 4 0.5304 0.3503 -14 1 5 -0.6143 -0.3977 -14 1 6 -0.5331 0.3133 -14 1 7 -0.2906 0.1070 -14 1 8 -0.4315 0.0220 -14 1 9 -0.0651 0.0542 -14 2 1 0.8546 1.3865 -14 2 2 -0.2171 0.5206 -14 2 3 0.7644 1.0975 -14 2 4 0.0501 -0.4135 -14 2 5 0.4298 0.5950 -14 2 6 0.5714 -0.1422 -14 2 7 0.4070 0.1975 -14 2 9 1.1226 -0.1830 -14 2 10 -0.1596 0.0426 -14 3 1 0.0016 -0.4782 -14 3 2 -0.3504 1.2816 -14 3 3 0.3641 -0.5518 -14 3 4 -0.2223 0.7106 -14 3 5 1.5209 -0.0744 -14 3 6 0.1319 0.0993 -14 3 7 1.5145 -0.0002 -14 3 8 0.9287 -0.3491 -14 3 9 0.6227 0.2404 -14 3 10 0.9223 -0.0547 -14 4 1 -0.8395 0.5966 -14 4 2 -0.1601 -1.1787 -14 4 3 -1.0646 0.2705 -14 4 4 0.6776 0.0622 -14 4 5 -0.4512 0.0738 -14 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-6 6 1.0707 -0.2096 11 -6 7 0.9182 -0.6303 11 -6 8 -0.2453 -0.5181 11 -6 9 -0.4113 0.0637 11 -6 10 -0.0008 -0.3391 11 -6 11 -2.0664 0.1906 11 -5 0 -1.1046 -0.8718 11 -5 1 0.1507 -2.9387 11 -5 2 -0.3340 -0.1920 11 -5 3 1.5916 -1.0744 11 -5 4 1.2575 -0.0393 11 -5 5 1.3836 0.0645 11 -5 6 1.2558 -0.3858 11 -5 7 0.7682 -0.6010 11 -5 8 -0.0721 -0.0586 11 -5 9 1.3071 -0.3615 11 -5 10 -1.5045 0.5073 11 -5 11 1.3229 0.1991 11 -4 0 -0.8395 -2.2924 11 -4 1 -1.4122 -0.1452 11 -4 2 0.0657 -1.5465 11 -4 3 -0.0766 -0.8137 11 -4 4 0.9899 0.1235 11 -4 5 -0.0025 -0.3501 11 -4 6 0.8222 -0.1310 11 -4 7 -0.9216 -0.0401 11 -4 8 1.2625 -0.2788 11 -4 9 -1.0697 0.4365 11 -4 10 1.6567 0.4757 11 -4 11 -0.7991 0.8459 11 -3 0 -0.8275 1.3621 11 -3 1 -0.6218 -0.0414 11 -3 2 -0.3714 -1.1092 11 -3 3 0.4408 0.2962 11 -3 4 -0.7485 -0.8754 11 -3 5 0.3197 0.2366 11 -3 6 -1.7891 -0.0417 11 -3 7 -0.0291 0.0777 11 -3 8 -0.7270 0.0490 11 -3 9 0.4973 0.4402 11 -3 10 0.4846 0.4083 11 -3 11 0.2866 0.6054 11 -2 0 -0.4745 2.5912 11 -2 1 -0.0859 0.1308 11 -2 2 -0.0200 1.4805 11 -2 3 -0.0998 -0.5922 11 -2 4 -0.8610 0.1259 11 -2 5 -1.2636 0.1396 11 -2 6 -2.2317 0.1808 11 -2 7 -0.3457 0.0908 11 -2 8 -1.5502 0.5431 11 -2 9 1.6847 -0.2131 11 -2 10 -0.5627 0.4525 11 -2 11 1.5352 -0.0759 11 -1 0 -0.5310 0.9404 11 -1 1 0.2449 2.9469 11 -1 2 -0.0242 0.8384 11 -1 3 -1.2165 0.3740 11 -1 4 -0.9600 0.7467 11 -1 5 -3.7431 -0.1975 11 -1 6 -0.7510 0.3970 11 -1 7 -3.1657 0.5838 11 -1 8 0.8865 -0.0019 11 -1 9 -0.4417 0.3731 11 -1 10 1.4130 -0.1988 11 -1 11 0.3363 0.0158 11 0 0 0.1728 2.2821 11 0 1 0.0126 1.5769 11 0 2 -0.0394 0.8360 11 0 3 -1.4318 1.5795 11 0 4 -3.0178 -0.2688 11 0 5 -1.9951 0.3257 11 0 6 -3.2259 0.2058 11 0 7 -0.7784 0.1782 11 0 8 -0.1141 0.2308 11 0 9 -0.0964 0.4708 11 0 10 1.9828 -0.4174 11 0 11 0.0264 0.0889 11 1 0 0.6104 0.4766 11 1 1 1.0775 -0.2102 11 1 2 -0.5636 1.8292 11 1 3 -0.9250 -0.0277 11 1 4 -2.2509 0.2885 11 1 5 -2.0223 -0.1486 11 1 6 -1.1176 -0.3648 11 1 7 0.0949 -0.2450 11 1 8 -0.0673 0.5495 11 1 9 1.8210 -0.3873 11 1 10 0.0596 0.3711 11 2 0 0.6205 -2.4513 11 2 1 0.7909 0.6426 11 2 2 0.5513 -0.5396 11 2 3 -0.5051 0.2403 11 2 4 -1.1530 0.0131 11 2 5 -0.4089 -0.6919 11 2 6 0.0800 -0.5657 11 2 7 0.9164 -0.1383 11 2 8 1.4102 -0.1459 11 2 9 0.9147 0.0048 11 2 10 0.5011 0.3338 11 3 0 -0.3645 -0.9912 11 3 1 0.4722 -1.7163 11 3 2 1.3231 -0.8824 11 3 3 -1.1006 0.1233 11 3 4 0.2384 -0.7415 11 3 5 -1.3499 -0.1581 11 3 6 0.3535 -0.4737 11 3 7 0.9558 -0.0164 11 3 8 0.4444 -0.3672 11 3 9 0.7379 0.9800 11 4 0 -0.4029 -1.7895 11 4 1 1.0019 -2.3286 11 4 2 -0.4386 -0.3178 11 4 3 0.4925 -1.4190 11 4 4 -2.7630 0.1742 11 4 5 -1.4205 -0.3307 11 4 6 -1.1725 -0.0129 11 4 7 -1.2170 -0.2617 11 4 8 0.5956 0.4927 11 5 0 -0.3079 -2.0989 11 5 1 0.7604 0.0885 11 5 2 0.5995 -2.0410 11 5 3 -1.3799 -0.0931 11 5 4 -2.0882 -0.3072 11 5 5 -2.4108 -0.3225 11 5 6 -2.6236 0.0747 11 5 7 -0.6872 -0.4546 11 6 0 0.6665 2.1203 11 6 1 0.8825 -1.0171 11 6 2 0.6746 0.3485 11 6 3 -0.4231 -0.0300 11 6 4 -0.6639 -0.5868 11 6 5 -2.2106 0.3069 11 6 6 -0.5904 -0.7624 11 7 0 0.6052 1.1988 11 7 1 0.4438 1.5550 11 7 2 1.2802 1.4911 11 7 3 1.0858 -0.2678 11 7 4 -0.0030 0.7445 11 7 5 0.7601 -0.3104 11 8 0 -0.4506 1.5765 12 -12 0 -0.8159 0.4816 12 -11 0 -0.5313 1.2977 12 -11 1 0.3494 2.1322 12 -10 0 0.1882 2.2459 12 -10 1 -0.7517 -0.1314 12 -10 2 -0.0869 1.7530 12 -10 3 0.1086 0.2107 12 -10 4 -0.2524 -0.0200 12 -9 0 -0.6078 -0.8971 12 -9 1 -0.0226 0.2381 12 -9 2 -0.3532 0.7334 12 -9 3 0.5672 -0.2518 12 -9 4 0.4275 0.4802 12 -9 5 0.4877 -0.4036 12 -9 6 0.7510 -0.2580 12 -8 0 0.0760 -2.2652 12 -8 1 -1.3700 0.3779 12 -8 2 0.7450 -1.3485 12 -8 3 -0.4458 0.7413 12 -8 4 1.5655 -0.0228 12 -8 5 0.4656 -0.0620 12 -8 6 1.0283 -0.2826 12 -8 7 0.6989 -0.1217 12 -7 0 -1.7199 -0.4041 12 -7 1 -0.0214 -2.2668 12 -7 2 -1.1585 -0.5180 12 -7 3 0.7341 0.0395 12 -7 4 0.0478 -0.2673 12 -7 5 0.8890 0.3166 12 -7 6 0.0231 -0.0306 12 -7 7 1.3203 -0.4913 12 -7 8 -0.5778 0.1331 12 -6 0 -0.0707 -1.5458 12 -6 1 -0.7031 -1.8140 12 -6 2 -0.3938 -0.3927 12 -6 3 0.2262 -1.3461 12 -6 4 -0.4290 0.2394 12 -6 5 -0.1665 0.0305 12 -6 6 -0.0026 -0.1988 12 -6 7 -0.7887 0.1879 12 -6 8 1.1309 0.1195 12 -5 0 0.4098 -1.1642 12 -5 1 -0.0141 0.0386 12 -5 2 0.7194 -1.9704 12 -5 3 -0.2891 -0.4824 12 -5 4 -0.2336 -0.2980 12 -5 5 -0.4729 -0.2400 12 -5 6 -0.8566 0.2594 12 -5 7 0.2334 0.2148 12 -5 8 0.2041 -0.1289 12 -5 9 0.7741 0.3465 12 -4 0 0.1735 1.8304 12 -4 1 1.3288 -0.7942 12 -4 2 0.3984 -0.4426 12 -4 3 0.2844 -0.2145 12 -4 4 -0.1420 -0.5654 12 -4 5 -0.4697 0.3357 12 -4 6 -0.2127 0.4961 12 -4 7 0.8586 -0.2354 12 -4 8 0.5220 0.2527 12 -4 9 1.8722 -0.4722 12 -3 0 1.0729 1.0294 12 -3 1 0.4074 0.5340 12 -3 2 1.0610 1.0992 12 -3 3 -0.5764 -0.6518 12 -3 4 0.7135 0.6973 12 -3 5 -1.4491 0.5087 12 -3 6 1.5356 0.1120 12 -3 7 -0.4591 0.5769 12 -3 8 2.3475 -0.4819 12 -3 9 0.4422 -0.1416 12 -2 0 0.9917 0.6449 12 -2 1 0.6879 2.3944 12 -2 2 -0.1115 -0.1760 12 -2 3 0.9387 1.2782 12 -2 4 -1.8849 0.3854 12 -2 5 1.2535 0.3332 12 -2 6 -1.2488 0.5378 12 -2 7 1.2353 0.0734 12 -2 8 0.5432 -0.1840 12 -1 0 0.2666 1.9344 12 -1 1 1.3215 0.0848 12 -1 2 0.4053 1.2603 12 -1 3 -0.1322 0.8961 12 -1 4 0.0043 0.0717 12 -1 5 -0.1831 0.3785 12 -1 6 -0.7016 0.1957 12 -1 7 1.0337 -0.5539 12 -1 8 -0.9598 0.2335 12 0 0 0.9207 -0.6963 12 0 1 1.1590 0.1398 12 0 2 1.0392 1.3256 12 0 3 0.3554 -0.3514 12 0 4 0.9884 0.7298 12 0 5 -1.2025 -0.0520 12 0 6 1.1693 -0.6232 12 0 7 -1.8200 0.1623 12 1 0 1.5400 -1.5856 12 1 1 0.3628 0.5183 12 1 2 2.6306 -1.0993 12 1 3 0.7568 0.7289 12 1 4 0.2866 -0.0510 12 1 5 0.1828 -0.2518 12 1 6 -1.4604 -0.0829 12 1 7 -0.8046 -0.2167 12 2 0 -0.3926 -0.4718 12 2 1 3.7715 -2.3846 12 2 2 1.1798 -0.3051 12 2 3 2.3283 -0.4337 12 2 4 -0.2073 -0.2629 12 2 5 -1.1804 -0.0677 12 2 6 -1.4363 0.0701 12 2 7 -1.5918 -0.9219 12 3 0 2.3208 -2.6480 12 3 1 2.6645 -1.0925 12 3 2 3.4961 -1.1433 12 3 3 2.0282 -0.9234 12 3 4 -0.2523 -0.2169 12 3 5 -0.5692 -0.1730 12 3 6 -1.9366 -0.6881 12 4 0 2.2568 -0.2941 12 4 1 2.7045 -0.3964 12 4 2 4.7164 -1.1686 12 4 3 1.6025 -0.1027 12 4 4 2.1430 -0.6084 12 5 0 0.4135 1.6815 12 5 1 3.6132 -0.2251 12 5 2 2.4144 0.9810 12 6 0 -0.0746 0.4879 13 -9 0 -1.1376 -0.4284 13 -9 1 -0.7266 -1.2490 13 -8 0 0.5689 -0.9712 13 -8 1 -0.4365 -1.3375 13 -7 0 1.1864 -1.9721 13 -7 1 -0.2663 -0.1222 13 -7 2 1.0445 -1.0863 13 -7 3 -0.2334 -0.3467 13 -7 4 0.8823 0.0743 13 -6 0 -0.9389 0.2238 13 -6 1 0.7868 -0.3094 13 -6 2 -0.4924 -1.1166 13 -6 3 1.2686 -0.0260 13 -6 4 0.5588 -0.2967 13 -6 5 1.6740 -0.3499 13 -5 0 -0.7575 1.7392 13 -5 1 -1.2086 -0.7213 13 -5 2 -0.1170 0.8696 13 -5 3 0.3991 -0.4173 13 -5 4 1.3771 -0.2391 13 -5 5 1.1051 0.3122 13 -4 0 -1.7652 0.2446 13 -4 1 -1.1794 1.8502 13 -4 2 -0.7167 0.4274 13 -4 3 0.8362 0.0349 13 -4 4 0.2405 0.3937 13 -4 5 1.2829 -0.4049 13 -4 6 0.1595 -0.4020 13 -3 0 -1.8959 1.4829 13 -3 1 -1.1399 1.5317 13 -3 2 0.0581 0.1871 13 -3 3 -0.1886 1.0243 13 -3 4 0.7037 -0.2788 13 -3 5 -0.1617 -0.4376 13 -3 6 -0.6783 0.0213 13 -2 0 -1.2662 1.5319 13 -2 1 -1.1159 -0.4254 13 -2 2 0.3166 1.7864 13 -2 3 -0.4812 -0.1500 13 -2 4 0.9611 0.0033 13 -2 5 -1.7679 0.3478 13 -1 0 -0.7708 -1.7660 13 -1 1 -0.4880 1.1454 13 -1 2 -0.3844 -0.3615 13 -1 3 1.3830 0.2271 13 -1 4 -1.6895 0.5938 13 -1 5 0.2092 -0.1441 13 0 0 -1.7433 -0.8050 13 0 1 1.0710 -1.0303 13 0 2 0.6102 -1.0244 13 0 3 0.1967 0.4476 13 0 4 -0.3052 -0.1963 13 1 0 0.2264 -1.2947 13 1 1 0.7744 -2.4545 13 1 2 1.1617 -0.0873 13 2 0 0.2731 -1.9032 13 2 1 -0.9923 0.0212 13 2 2 1.5576 -0.9882 13 3 0 -4.4393 1.2300 13 3 1 0.3651 0.1961 14 -5 0 -0.9800 0.4391 14 -3 0 0.1347 -1.4068 14 -3 1 0.8651 -0.7591 14 -2 0 0.6802 -2.0534 0 0 0 0.0 0.0 ; _shelx_fab_checksum 42657 _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 2.456 _oxdiff_exptl_absorpt_empirical_full_min 0.489 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 0.14150(3) 0.11098(2) 0.28854(2) 0.04218(12) Uani 1 1 d . . . . . Dy2 Dy 0.52152(3) 0.66107(2) 0.24576(2) 0.04436(12) Uani 1 1 d D . . . . Zn1 Zn -0.14185(8) 0.10577(7) 0.31994(5) 0.0568(2) Uani 1 1 d . . . . . Zn2 Zn 0.81123(7) 0.64924(6) 0.22064(5) 0.0510(2) Uani 1 1 d . . . . . Cl1 Cl 0.26267(19) -0.10947(14) 0.10727(8) 0.0672(5) Uani 1 1 d . . . . . Cl2 Cl 0.39315(19) -0.12368(15) 0.43008(8) 0.0719(5) Uani 1 1 d . . . . . Cl3 Cl 0.55019(18) 0.29977(12) 0.23549(13) 0.0763(6) Uani 1 1 d . . . . . Cl4 Cl 0.11635(16) 0.47128(12) 0.30316(12) 0.0692(5) Uani 1 1 d . . . . . O1 O 0.1060(6) 0.1703(3) 0.1673(2) 0.0673(14) Uani 1 1 d . . . . . O2 O -0.0528(4) 0.1238(3) 0.2416(2) 0.0501(10) Uani 1 1 d . . . . . O3 O 0.0277(4) 0.1058(3) 0.3704(2) 0.0467(9) Uani 1 1 d . . . . . O4 O 0.2509(4) 0.1698(3) 0.4103(2) 0.0550(11) Uani 1 1 d . . . . . O5 O -0.1616(5) -0.0494(4) 0.2893(3) 0.0650(13) Uani 1 1 d . . . . . O6 O 0.0223(4) -0.0497(3) 0.2744(3) 0.0593(12) Uani 1 1 d . . . . . O7 O -0.1214(6) -0.1638(4) 0.2393(4) 0.092(2) Uani 1 1 d . . . . . O8 O -0.1036(7) 0.2577(4) 0.3296(4) 0.101(2) Uani 1 1 d D . . . . H8 H -0.028667 0.270976 0.331755 0.122 Uiso 1 1 d R U . . . O9 O 0.3216(4) 0.2017(3) 0.2726(3) 0.0525(11) Uani 1 1 d . . . . . O10 O 0.1425(4) 0.2732(3) 0.2979(2) 0.0496(10) Uani 1 1 d . . . . . O11 O 0.5239(4) 0.4972(3) 0.2387(2) 0.0510(10) Uani 1 1 d . . . . . O12 O 0.3418(4) 0.5688(3) 0.2609(3) 0.0554(11) Uani 1 1 d . . . . . O13 O 0.2152(4) 0.0182(3) 0.2136(2) 0.0515(10) Uani 1 1 d . . . . . O14 O 0.2593(4) 0.0069(3) 0.3457(2) 0.0495(10) Uani 1 1 d . . . . . O15 O 0.3866(4) -0.2442(3) 0.1921(2) 0.0491(10) Uani 1 1 d . . . . . O16 O 0.4575(4) -0.2411(3) 0.3234(2) 0.0531(10) Uani 1 1 d . . . . . O17 O 0.5521(5) 0.6074(3) 0.3677(3) 0.0644(13) Uani 1 1 d . . . . . O18 O 0.7164(4) 0.6549(3) 0.2970(2) 0.0489(10) Uani 1 1 d . . . . . O19 O 0.6439(4) 0.6529(3) 0.1677(2) 0.0462(9) Uani 1 1 d . . . . . O20 O 0.4199(4) 0.6066(3) 0.1238(2) 0.0592(12) Uani 1 1 d . . . . . O21 O 0.6262(4) 0.8205(3) 0.2339(3) 0.0596(12) Uani 1 1 d D . . . . H21 H 0.691027 0.847575 0.259746 0.089 Uiso 1 1 d DR U . . . O22 O 0.7748(6) 0.5047(4) 0.2198(4) 0.0826(17) Uani 1 1 d . . . . . H22 H 0.699308 0.491449 0.214832 0.099 Uiso 1 1 d R U . . . N1 N -0.3014(5) 0.1020(4) 0.2547(4) 0.0648(16) Uani 1 1 d . . . . . N2 N -0.2030(5) 0.0675(4) 0.4067(3) 0.0606(15) Uani 1 1 d . . . . . N3 N -0.0842(5) -0.0857(4) 0.2678(3) 0.0559(13) Uani 1 1 d . . . . . N4 N 0.9662(5) 0.6680(4) 0.2901(4) 0.0650(17) Uani 1 1 d . . . . . N5 N 0.8792(6) 0.6849(4) 0.1361(4) 0.0626(16) Uani 1 1 d . . . . . C1 C 0.1897(10) 0.1822(7) 0.1220(5) 0.088(3) Uani 1 1 d . . . . . H1A H 0.262107 0.162467 0.143379 0.132 Uiso 1 1 calc R U . . . H1B H 0.206474 0.245884 0.111365 0.132 Uiso 1 1 calc R U . . . H1C H 0.156427 0.146163 0.080752 0.132 Uiso 1 1 calc R U . . . C2 C -0.0096(9) 0.1876(5) 0.1410(4) 0.067(2) Uani 1 1 d . . . . . C3 C -0.0430(12) 0.2284(8) 0.0802(5) 0.100(4) Uani 1 1 d . . . . . H3 H 0.013630 0.247928 0.053379 0.120 Uiso 1 1 calc R U . . . C4 C -0.1570(13) 0.2404(9) 0.0588(5) 0.111(4) Uani 1 1 d . . . . . H4 H -0.178021 0.270671 0.018741 0.133 Uiso 1 1 calc R U . . . C5 C -0.2409(12) 0.2079(7) 0.0965(5) 0.096(3) Uani 1 1 d . . . . . H5 H -0.320063 0.212118 0.079574 0.115 Uiso 1 1 calc R U . . . C6 C -0.2124(8) 0.1681(5) 0.1600(4) 0.070(2) Uani 1 1 d . . . . . C7 C -0.0919(7) 0.1600(4) 0.1831(3) 0.0578(17) Uani 1 1 d . . . . . C8 C -0.3070(8) 0.1322(6) 0.1958(5) 0.071(2) Uani 1 1 d . . . . . H8A H -0.383764 0.131396 0.171391 0.086 Uiso 1 1 calc R U . . . C9 C -0.4125(7) 0.0641(6) 0.2763(6) 0.084(3) Uani 1 1 d . . . . . H9A H -0.428795 -0.001924 0.267683 0.101 Uiso 1 1 calc R U . . . H9B H -0.477093 0.089732 0.249398 0.101 Uiso 1 1 calc R U . . . C10 C -0.4091(8) 0.0840(6) 0.3517(6) 0.089(3) Uani 1 1 d . . . . . H10A H -0.489746 0.070122 0.360464 0.106 Uiso 1 1 calc R U . . . H10B H -0.380870 0.149189 0.361439 0.106 Uiso 1 1 calc R U . . . C11 C -0.3302(8) 0.0301(6) 0.4004(5) 0.081(3) Uani 1 1 d . . . . . H11A H -0.351860 0.031160 0.445056 0.098 Uiso 1 1 calc R U . . . H11B H -0.344577 -0.033521 0.384158 0.098 Uiso 1 1 calc R U . . . C12 C -0.1397(8) 0.0778(5) 0.4667(4) 0.070(2) Uani 1 1 d . . . . . H12 H -0.179232 0.061146 0.502514 0.084 Uiso 1 1 calc R U . . . C13 C -0.0138(7) 0.1124(4) 0.4848(3) 0.0585(17) Uani 1 1 d . . . . . C14 C 0.0363(10) 0.1333(6) 0.5548(4) 0.078(3) Uani 1 1 d . . . . . H14 H -0.012926 0.123697 0.586991 0.093 Uiso 1 1 calc R U . . . C15 C 0.1534(11) 0.1665(6) 0.5758(4) 0.087(3) Uani 1 1 d . . . . . H15 H 0.182822 0.181416 0.621733 0.104 Uiso 1 1 calc R U . . . C16 C 0.2306(9) 0.1789(5) 0.5297(4) 0.072(2) Uani 1 1 d . . . . . H16 H 0.311588 0.200198 0.544399 0.087 Uiso 1 1 calc R U . . . C17 C 0.1846(7) 0.1588(4) 0.4617(3) 0.0520(15) Uani 1 1 d . . . . . C18 C 0.0634(7) 0.1250(4) 0.4378(3) 0.0498(15) Uani 1 1 d . . . . . C19 C 0.3787(7) 0.1916(8) 0.4324(5) 0.086(3) Uani 1 1 d . . . . . H19A H 0.404766 0.146633 0.463699 0.128 Uiso 1 1 calc R U . . . H19B H 0.399601 0.251398 0.454461 0.128 Uiso 1 1 calc R U . . . H19C H 0.416753 0.191069 0.393533 0.128 Uiso 1 1 calc R U . . . C20 C 0.3332(6) 0.2888(4) 0.2691(3) 0.0489(14) Uani 1 1 d . . . . . C21 C 0.4311(6) 0.3462(4) 0.2526(4) 0.0518(15) Uani 1 1 d . . . . . C22 C 0.4372(5) 0.4403(4) 0.2511(3) 0.0454(13) Uani 1 1 d . . . . . C23 C 0.3312(5) 0.4833(4) 0.2662(3) 0.0466(13) Uani 1 1 d . . . . . C24 C 0.2341(6) 0.4255(4) 0.2839(4) 0.0494(14) Uani 1 1 d . . . . . C25 C 0.2288(5) 0.3305(4) 0.2850(3) 0.0452(13) Uani 1 1 d . . . . . C26 C 0.2662(5) -0.0468(4) 0.2357(3) 0.0447(13) Uani 1 1 d . . . . . C27 C 0.3007(6) -0.1117(4) 0.1954(3) 0.0461(13) Uani 1 1 d . . . . . C28 C 0.3591(5) -0.1802(4) 0.2247(3) 0.0429(12) Uani 1 1 d . . . . . C29 C 0.3955(5) -0.1818(4) 0.3019(3) 0.0436(13) Uani 1 1 d . . . . . C30 C 0.3576(6) -0.1194(4) 0.3422(3) 0.0457(13) Uani 1 1 d . . . . . C31 C 0.2946(5) -0.0524(4) 0.3130(3) 0.0435(13) Uani 1 1 d . . . . . C32 C -0.1265(15) 0.3183(11) 0.3760(8) 0.151(6) Uani 1 1 d D U . . . H32A H -0.148742 0.371549 0.353029 0.227 Uiso 1 1 calc R U . . . H32B H -0.056224 0.336498 0.410203 0.227 Uiso 1 1 calc R U . . . H32C H -0.190374 0.289066 0.397220 0.227 Uiso 1 1 calc R U . . . C33 C 0.4603(11) 0.5955(8) 0.4097(5) 0.102(4) Uani 1 1 d . . . . . H33A H 0.485513 0.636374 0.449009 0.153 Uiso 1 1 calc R U . . . H33B H 0.447802 0.533143 0.423953 0.153 Uiso 1 1 calc R U . . . H33C H 0.387337 0.609175 0.383644 0.153 Uiso 1 1 calc R U . . . C34 C 0.6671(9) 0.5973(6) 0.3983(4) 0.070(2) Uani 1 1 d . . . . . C35 C 0.6950(14) 0.5644(9) 0.4624(6) 0.120(5) Uani 1 1 d . . . . . H35 H 0.635207 0.546336 0.487345 0.144 Uiso 1 1 calc R U . . . C36 C 0.8119(17) 0.5579(13) 0.4900(7) 0.156(7) Uani 1 1 d . . . . . H36 H 0.830691 0.536313 0.533658 0.187 Uiso 1 1 calc R U . . . C37 C 0.9009(14) 0.5834(11) 0.4527(7) 0.132(5) Uani 1 1 d . . . . . H37 H 0.979579 0.579454 0.471240 0.158 Uiso 1 1 calc R U . . . C38 C 0.8708(9) 0.6159(6) 0.3852(5) 0.079(2) Uani 1 1 d . . . . . C39 C 0.7518(7) 0.6230(5) 0.3586(4) 0.0601(18) Uani 1 1 d . . . . . C40 C 0.9702(8) 0.6464(6) 0.3517(5) 0.077(2) Uani 1 1 d . . . . . H40 H 1.045828 0.650696 0.378496 0.092 Uiso 1 1 calc R U . . . C41 C 1.0804(7) 0.7013(6) 0.2691(6) 0.085(3) Uani 1 1 d . . . . . H41A H 1.143455 0.677708 0.299291 0.102 Uiso 1 1 calc R U . . . H41B H 1.097434 0.767839 0.273455 0.102 Uiso 1 1 calc R U . . . C42 C 1.0799(8) 0.6720(6) 0.1966(6) 0.089(3) Uani 1 1 d . . . . . H42A H 1.161591 0.682095 0.189381 0.107 Uiso 1 1 calc R U . . . H42B H 1.050222 0.606485 0.191086 0.107 Uiso 1 1 calc R U . . . C43 C 1.0075(7) 0.7197(6) 0.1422(5) 0.082(3) Uani 1 1 d . . . . . H43A H 1.023138 0.785232 0.152826 0.098 Uiso 1 1 calc R U . . . H43B H 1.031092 0.710195 0.098874 0.098 Uiso 1 1 calc R U . . . C44 C 0.8185(8) 0.6765(5) 0.0750(4) 0.070(2) Uani 1 1 d . . . . . H44 H 0.861513 0.688239 0.040077 0.083 Uiso 1 1 calc R U . . . C45 C 0.6905(8) 0.6508(5) 0.0548(4) 0.0640(19) Uani 1 1 d . . . . . C46 C 0.6425(11) 0.6374(6) -0.0161(4) 0.084(3) Uani 1 1 d . . . . . H46 H 0.694176 0.642230 -0.046985 0.101 Uiso 1 1 calc R U . . . C47 C 0.5223(11) 0.6175(7) -0.0399(4) 0.089(3) Uani 1 1 d . . . . . H47 H 0.493235 0.610746 -0.086611 0.107 Uiso 1 1 calc R U . . . C48 C 0.4436(10) 0.6073(6) 0.0050(4) 0.079(2) Uani 1 1 d . . . . . H48 H 0.361879 0.592953 -0.011123 0.095 Uiso 1 1 calc R U . . . C49 C 0.4882(7) 0.6186(5) 0.0743(4) 0.0605(18) Uani 1 1 d . . . . . C50 C 0.6110(6) 0.6405(4) 0.1008(3) 0.0503(15) Uani 1 1 d . . . . . C51 C 0.2925(7) 0.5877(7) 0.1007(5) 0.085(3) Uani 1 1 d . . . . . H51A H 0.253543 0.595607 0.138279 0.127 Uiso 1 1 calc R U . . . H51B H 0.269067 0.525601 0.082841 0.127 Uiso 1 1 calc R U . . . H51C H 0.270100 0.629289 0.065705 0.127 Uiso 1 1 calc R U . . . C52 C 0.8050(9) 0.4417(7) 0.1774(7) 0.103(4) Uani 1 1 d . . . . . H52A H 0.745123 0.430524 0.136721 0.154 Uiso 1 1 calc R U . . . H52B H 0.810073 0.385122 0.200507 0.154 Uiso 1 1 calc R U . . . H52C H 0.880623 0.465745 0.165569 0.154 Uiso 1 1 calc R U . . . C53 C 0.6197(9) 0.8623(7) 0.1664(5) 0.090(3) Uani 1 1 d D . . . . H53A H 0.541704 0.842814 0.139485 0.135 Uiso 1 1 calc R U . . . H53B H 0.678294 0.843093 0.143720 0.135 Uiso 1 1 calc R U . . . H53C H 0.635009 0.928048 0.172085 0.135 Uiso 1 1 calc R U . . . Cl5 Cl -0.0019(6) 0.4859(4) 0.0195(3) 0.1066(19) Uani 0.5 1 d G U P A -1 O24 O -0.0125(16) 0.4372(13) -0.0457(8) 0.209(13) Uani 0.5 1 d G U P A -1 O25 O -0.1173(11) 0.4814(11) 0.0371(8) 0.138(6) Uani 0.5 1 d G U P A -1 O26 O 0.0437(13) 0.5790(8) 0.0145(9) 0.121(5) Uani 0.5 1 d G U P A -1 O27 O 0.0693(13) 0.4447(11) 0.0747(8) 0.180(9) 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 0.0406(2) 0.03377(18) 0.0531(2) 0.00008(13) 0.01476(15) 0.00240(13) Dy2 0.0371(2) 0.03513(19) 0.0622(2) -0.00274(14) 0.01712(15) 0.00148(13) Zn1 0.0423(5) 0.0661(6) 0.0608(5) 0.0014(4) 0.0128(4) 0.0026(4) Zn2 0.0388(4) 0.0503(5) 0.0640(5) -0.0035(4) 0.0153(4) 0.0019(3) Cl1 0.0846(13) 0.0758(11) 0.0459(8) -0.0004(7) 0.0131(8) 0.0263(10) Cl2 0.0852(13) 0.0939(14) 0.0468(8) 0.0026(8) 0.0140(8) 0.0424(11) Cl3 0.0629(11) 0.0483(9) 0.1327(17) 0.0060(10) 0.0507(11) 0.0165(8) Cl4 0.0565(10) 0.0484(8) 0.1145(15) 0.0026(9) 0.0408(10) 0.0150(7) O1 0.099(4) 0.054(3) 0.056(3) 0.012(2) 0.031(3) 0.015(3) O2 0.047(2) 0.051(2) 0.050(2) 0.0099(18) 0.0026(18) 0.0071(19) O3 0.048(2) 0.049(2) 0.045(2) -0.0055(17) 0.0097(18) 0.0091(19) O4 0.045(2) 0.056(3) 0.060(3) -0.011(2) 0.001(2) 0.010(2) O5 0.065(3) 0.062(3) 0.073(3) -0.004(2) 0.028(3) 0.009(2) O6 0.047(3) 0.038(2) 0.092(3) -0.009(2) 0.021(2) -0.0008(19) O7 0.087(4) 0.046(3) 0.138(6) -0.023(3) 0.018(4) 0.004(3) O8 0.096(5) 0.063(4) 0.139(6) -0.023(4) 0.011(4) 0.007(3) O9 0.048(2) 0.029(2) 0.085(3) 0.0009(19) 0.026(2) 0.0048(17) O10 0.047(2) 0.0298(19) 0.076(3) 0.0003(18) 0.023(2) 0.0059(17) O11 0.037(2) 0.039(2) 0.081(3) 0.000(2) 0.025(2) 0.0030(17) O12 0.041(2) 0.032(2) 0.096(3) 0.000(2) 0.025(2) 0.0020(17) O13 0.058(3) 0.045(2) 0.055(2) 0.0059(18) 0.013(2) 0.015(2) O14 0.051(2) 0.046(2) 0.055(2) -0.0078(18) 0.0143(19) 0.0128(19) O15 0.048(2) 0.038(2) 0.061(2) -0.0088(18) 0.0094(19) 0.0089(18) O16 0.062(3) 0.047(2) 0.056(2) 0.0026(19) 0.018(2) 0.017(2) O17 0.082(4) 0.060(3) 0.063(3) 0.010(2) 0.039(3) 0.019(3) O18 0.053(3) 0.050(2) 0.044(2) 0.0019(17) 0.0110(18) 0.0071(19) O19 0.041(2) 0.049(2) 0.048(2) -0.0031(17) 0.0094(17) 0.0041(18) O20 0.045(3) 0.066(3) 0.065(3) -0.020(2) 0.000(2) 0.015(2) O21 0.054(3) 0.041(2) 0.082(3) -0.005(2) 0.023(2) -0.008(2) O22 0.082(4) 0.052(3) 0.120(5) -0.013(3) 0.034(4) 0.010(3) N1 0.047(3) 0.046(3) 0.097(5) -0.005(3) -0.001(3) 0.009(3) N2 0.054(3) 0.051(3) 0.083(4) -0.010(3) 0.035(3) 0.002(3) N3 0.061(4) 0.048(3) 0.058(3) 0.001(2) 0.012(3) 0.004(3) N4 0.043(3) 0.045(3) 0.105(5) -0.004(3) 0.007(3) 0.005(2) N5 0.063(4) 0.047(3) 0.083(4) -0.007(3) 0.039(3) -0.003(3) C1 0.115(8) 0.083(6) 0.077(5) 0.021(4) 0.054(5) 0.006(5) C2 0.104(7) 0.055(4) 0.049(4) 0.013(3) 0.014(4) 0.031(4) C3 0.155(11) 0.091(7) 0.063(5) 0.022(5) 0.031(6) 0.033(7) C4 0.160(12) 0.132(10) 0.057(5) 0.022(6) 0.002(6) 0.087(9) C5 0.124(9) 0.086(7) 0.074(6) -0.006(5) -0.021(6) 0.049(6) C6 0.090(6) 0.055(4) 0.063(4) -0.010(3) -0.017(4) 0.036(4) C7 0.082(5) 0.031(3) 0.054(4) -0.002(2) -0.002(3) 0.009(3) C8 0.064(5) 0.057(4) 0.086(6) -0.015(4) -0.013(4) 0.020(4) C9 0.042(4) 0.058(5) 0.147(9) -0.006(5) 0.004(5) 0.009(3) C10 0.054(5) 0.064(5) 0.151(9) -0.037(6) 0.040(5) -0.002(4) C11 0.069(5) 0.067(5) 0.115(7) -0.020(5) 0.057(5) -0.010(4) C12 0.103(7) 0.048(4) 0.066(5) -0.009(3) 0.047(5) 0.001(4) C13 0.085(5) 0.040(3) 0.052(4) 0.001(3) 0.021(3) 0.006(3) C14 0.129(8) 0.063(5) 0.046(4) 0.003(3) 0.031(5) 0.014(5) C15 0.133(9) 0.065(5) 0.049(4) -0.006(3) 0.001(5) -0.001(5) C16 0.093(6) 0.058(4) 0.056(4) -0.001(3) -0.003(4) 0.004(4) C17 0.065(4) 0.037(3) 0.051(3) -0.001(2) 0.003(3) 0.010(3) C18 0.071(4) 0.036(3) 0.044(3) 0.001(2) 0.011(3) 0.014(3) C19 0.046(4) 0.115(8) 0.086(6) -0.017(5) -0.006(4) 0.005(5) C20 0.044(3) 0.039(3) 0.064(4) 0.001(3) 0.015(3) 0.003(3) C21 0.048(4) 0.039(3) 0.074(4) -0.002(3) 0.021(3) 0.010(3) C22 0.040(3) 0.031(3) 0.067(4) -0.002(2) 0.018(3) 0.000(2) C23 0.039(3) 0.032(3) 0.070(4) -0.004(3) 0.016(3) 0.004(2) C24 0.038(3) 0.038(3) 0.075(4) 0.000(3) 0.021(3) 0.004(2) C25 0.039(3) 0.037(3) 0.059(3) -0.003(2) 0.011(3) 0.004(2) C26 0.043(3) 0.039(3) 0.050(3) -0.002(2) 0.012(3) -0.003(2) C27 0.047(3) 0.045(3) 0.045(3) -0.005(2) 0.010(3) 0.004(3) C28 0.033(3) 0.041(3) 0.055(3) -0.003(2) 0.013(2) 0.000(2) C29 0.035(3) 0.038(3) 0.059(3) 0.003(2) 0.016(2) 0.002(2) C30 0.046(3) 0.046(3) 0.049(3) -0.001(2) 0.011(3) 0.013(3) C31 0.035(3) 0.038(3) 0.058(3) -0.003(2) 0.014(2) 0.001(2) C32 0.151(9) 0.146(9) 0.165(9) -0.019(7) 0.052(8) 0.024(7) C33 0.138(10) 0.095(7) 0.080(6) 0.005(5) 0.059(6) -0.005(7) C34 0.093(6) 0.065(5) 0.056(4) 0.016(3) 0.020(4) 0.020(4) C35 0.157(13) 0.130(10) 0.080(7) 0.052(7) 0.035(8) 0.027(9) C36 0.179(16) 0.206(18) 0.092(9) 0.078(10) 0.009(10) 0.078(14) C37 0.123(11) 0.162(13) 0.093(8) 0.043(8) -0.033(8) 0.033(9) C38 0.091(7) 0.072(5) 0.073(5) 0.015(4) 0.001(5) 0.024(5) C39 0.073(5) 0.048(4) 0.054(4) 0.002(3) -0.003(3) 0.011(3) C40 0.062(5) 0.056(4) 0.101(7) 0.000(4) -0.017(5) 0.015(4) C41 0.042(4) 0.049(4) 0.157(9) -0.004(5) 0.005(5) 0.000(3) C42 0.048(5) 0.064(5) 0.161(10) -0.028(6) 0.044(6) -0.002(4) C43 0.056(5) 0.072(5) 0.125(8) -0.011(5) 0.050(5) -0.004(4) C44 0.087(6) 0.059(4) 0.070(5) -0.006(3) 0.050(4) -0.005(4) C45 0.086(6) 0.050(4) 0.059(4) 0.001(3) 0.031(4) -0.001(4) C46 0.132(9) 0.065(5) 0.059(5) 0.005(4) 0.036(5) 0.002(5) C47 0.129(9) 0.081(6) 0.052(4) 0.002(4) 0.003(5) 0.015(6) C48 0.096(7) 0.076(5) 0.059(4) -0.005(4) -0.008(4) 0.020(5) C49 0.071(5) 0.048(4) 0.058(4) -0.007(3) -0.003(3) 0.013(3) C50 0.065(4) 0.036(3) 0.050(3) -0.004(2) 0.015(3) 0.008(3) C51 0.050(4) 0.099(7) 0.097(6) -0.042(5) -0.013(4) 0.018(4) C52 0.072(6) 0.077(6) 0.160(10) -0.040(6) 0.023(6) 0.013(5) C53 0.094(7) 0.081(6) 0.096(7) 0.000(5) 0.033(5) 0.002(5) Cl5 0.089(3) 0.095(3) 0.120(4) -0.029(3) 0.000(3) -0.008(3) O24 0.217(16) 0.214(16) 0.209(15) -0.047(9) 0.068(10) 0.045(10) O25 0.116(9) 0.153(10) 0.145(9) -0.023(8) 0.026(8) 0.022(8) O26 0.128(9) 0.107(9) 0.124(9) -0.005(7) 0.021(8) 0.011(7) O27 0.164(12) 0.171(12) 0.192(12) 0.016(9) 0.016(9) 0.007(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 Zn1 97.67(14) . . ? O1 Dy1 O4 139.00(17) . . ? O2 Dy1 Zn1 34.58(11) . . ? O2 Dy1 O1 63.60(17) . . ? O2 Dy1 O4 125.05(15) . . ? O2 Dy1 O6 72.92(16) . . ? O2 Dy1 O9 129.60(15) . . ? O2 Dy1 O10 77.12(15) . . ? O2 Dy1 O13 108.96(16) . . ? O2 Dy1 O14 142.23(15) . . ? O3 Dy1 Zn1 34.68(11) . . ? O3 Dy1 O1 130.20(17) . . ? O3 Dy1 O2 69.05(15) . . ? O3 Dy1 O4 63.35(15) . . ? O3 Dy1 O6 76.40(15) . . ? O3 Dy1 O9 134.49(16) . . ? O3 Dy1 O10 82.94(15) . . ? O3 Dy1 O13 143.64(15) . . ? O3 Dy1 O14 92.82(15) . . ? O4 Dy1 Zn1 95.66(11) . . ? O6 Dy1 Zn1 68.35(11) . . ? O6 Dy1 O1 102.80(18) . . ? O6 Dy1 O4 118.16(17) . . ? O9 Dy1 Zn1 147.21(10) . . ? O9 Dy1 O1 72.83(18) . . ? O9 Dy1 O4 75.06(16) . . ? O9 Dy1 O6 143.81(14) . . ? O9 Dy1 O10 66.41(14) . . ? O9 Dy1 O13 76.28(15) . . ? O9 Dy1 O14 87.00(15) . . ? O10 Dy1 Zn1 80.80(10) . . ? O10 Dy1 O1 72.66(16) . . ? O10 Dy1 O4 71.51(15) . . ? O10 Dy1 O6 148.10(15) . . ? O13 Dy1 Zn1 130.87(12) . . ? O13 Dy1 O1 69.74(16) . . ? O13 Dy1 O4 125.52(15) . . ? O13 Dy1 O6 68.83(15) . . ? O13 Dy1 O10 133.04(15) . . ? O14 Dy1 Zn1 118.75(11) . . ? O14 Dy1 O1 134.74(16) . . ? O14 Dy1 O4 66.93(14) . . ? O14 Dy1 O6 70.63(16) . . ? O14 Dy1 O10 135.17(15) . . ? O14 Dy1 O13 66.23(14) . . ? O11 Dy2 Zn2 76.21(10) . . ? O11 Dy2 O17 73.66(16) . . ? O11 Dy2 O20 73.66(16) . . ? O11 Dy2 O21 147.65(15) . . ? O12 Dy2 Zn2 142.42(10) . . ? O12 Dy2 O11 66.26(14) . . ? O12 Dy2 O15 81.54(15) . 1_565 ? O12 Dy2 O16 79.74(16) . 1_565 ? O12 Dy2 O17 72.55(18) . . ? O12 Dy2 O20 76.74(18) . . ? O12 Dy2 O21 145.81(15) . . ? O15 Dy2 Zn2 128.97(11) 1_565 . ? O15 Dy2 O11 133.17(15) 1_565 . ? O15 Dy2 O16 65.65(15) 1_565 1_565 ? O15 Dy2 O17 128.89(15) 1_565 . ? O15 Dy2 O20 66.22(14) 1_565 . ? O15 Dy2 O21 68.64(16) 1_565 . ? O16 Dy2 Zn2 129.35(12) 1_565 . ? O16 Dy2 O11 133.92(15) 1_565 . ? O16 Dy2 O17 66.84(15) 1_565 . ? O16 Dy2 O20 128.69(15) 1_565 . ? O16 Dy2 O21 73.09(16) 1_565 . ? O17 Dy2 Zn2 95.82(12) . . ? O17 Dy2 O20 141.90(18) . . ? O18 Dy2 Zn2 33.78(10) . . ? O18 Dy2 O11 78.61(15) . . ? O18 Dy2 O12 130.00(16) . . ? O18 Dy2 O15 145.87(15) . 1_565 ? O18 Dy2 O16 103.26(16) . 1_565 ? O18 Dy2 O17 63.88(16) . . ? O18 Dy2 O20 126.73(15) . . ? O18 Dy2 O21 77.27(16) . . ? O19 Dy2 Zn2 33.55(10) . . ? O19 Dy2 O11 78.02(15) . . ? O19 Dy2 O12 132.17(16) . . ? O19 Dy2 O15 103.03(15) . 1_565 ? O19 Dy2 O16 146.00(15) . 1_565 ? O19 Dy2 O17 127.10(16) . . ? O19 Dy2 O18 67.33(14) . . ? O19 Dy2 O20 62.99(15) . . ? O19 Dy2 O21 72.96(15) . . ? O20 Dy2 Zn2 94.93(11) . . ? O21 Dy2 Zn2 71.74(11) . . ? O21 Dy2 O17 113.51(17) . . ? O21 Dy2 O20 104.58(17) . . ? O2 Zn1 Dy1 40.48(12) . . ? O2 Zn1 O3 79.70(17) . . ? O2 Zn1 O5 83.15(18) . . ? O2 Zn1 O8 84.4(2) . . ? O2 Zn1 N1 91.0(2) . . ? O2 Zn1 N2 166.3(2) . . ? O3 Zn1 Dy1 39.48(11) . . ? O3 Zn1 O5 90.56(18) . . ? O3 Zn1 O8 87.8(2) . . ? O3 Zn1 N1 170.3(2) . . ? O3 Zn1 N2 89.3(2) . . ? O5 Zn1 Dy1 82.43(13) . . ? O8 Zn1 Dy1 88.5(2) . . ? O8 Zn1 O5 167.5(2) . . ? N1 Zn1 Dy1 131.0(2) . . ? N1 Zn1 O5 85.6(2) . . ? N1 Zn1 O8 94.1(3) . . ? N2 Zn1 Dy1 127.48(19) . . ? N2 Zn1 O5 88.8(2) . . ? N2 Zn1 O8 103.6(3) . . ? N2 Zn1 N1 99.4(3) . . ? O18 Zn2 Dy2 39.05(12) . . ? O18 Zn2 O22 90.1(2) . . ? O19 Zn2 Dy2 38.71(11) . . ? O19 Zn2 O18 77.76(17) . . ? O19 Zn2 O22 90.8(2) . . ? O22 Zn2 Dy2 90.94(17) . . ? N4 Zn2 Dy2 128.8(2) . . ? N4 Zn2 O18 90.4(2) . . ? N4 Zn2 O19 165.3(2) . . ? N4 Zn2 O22 97.9(3) . . ? N5 Zn2 Dy2 126.5(2) . . ? N5 Zn2 O18 159.2(2) . . ? N5 Zn2 O19 89.9(2) . . ? N5 Zn2 O22 107.0(2) . . ? N5 Zn2 N4 98.7(3) . . ? C1 O1 Dy1 126.5(6) . . ? C2 O1 Dy1 116.8(4) . . ? C2 O1 C1 116.6(6) . . ? Zn1 O2 Dy1 104.94(17) . . ? C7 O2 Dy1 127.8(5) . . ? C7 O2 Zn1 124.8(5) . . ? Zn1 O3 Dy1 105.83(17) . . ? C18 O3 Dy1 128.3(4) . . ? C18 O3 Zn1 123.4(4) . . ? C17 O4 Dy1 117.0(4) . . ? C17 O4 C19 115.9(6) . . ? C19 O4 Dy1 125.3(5) . . ? N3 O5 Zn1 125.2(4) . . ? N3 O6 Dy1 136.9(4) . . ? Zn1 O8 H8 104.1 . . ? C32 O8 Zn1 131.8(9) . . ? C32 O8 H8 104.0 . . ? C20 O9 Dy1 121.8(4) . . ? C25 O10 Dy1 120.9(4) . . ? C22 O11 Dy2 120.2(4) . . ? C23 O12 Dy2 122.5(4) . . ? C26 O13 Dy1 120.7(4) . . ? C31 O14 Dy1 121.0(4) . . ? C28 O15 Dy2 121.5(4) . 1_545 ? C29 O16 Dy2 121.1(4) . 1_545 ? C33 O17 Dy2 124.4(6) . . ? C34 O17 Dy2 117.5(4) . . ? C34 O17 C33 117.9(7) . . ? Zn2 O18 Dy2 107.17(18) . . ? C39 O18 Dy2 126.1(5) . . ? C39 O18 Zn2 121.6(5) . . ? Zn2 O19 Dy2 107.74(18) . . ? C50 O19 Dy2 127.0(4) . . ? C50 O19 Zn2 124.7(4) . . ? C49 O20 Dy2 117.4(4) . . ? C49 O20 C51 116.5(6) . . ? C51 O20 Dy2 123.9(5) . . ? Dy2 O21 H21 126.0 . . ? C53 O21 Dy2 120.8(5) . . ? C53 O21 H21 107.6 . . ? Zn2 O22 H22 104.6 . . ? C52 O22 Zn2 129.2(7) . . ? C52 O22 H22 104.5 . . ? C8 N1 Zn1 121.7(6) . . ? C8 N1 C9 118.2(8) . . ? C9 N1 Zn1 120.1(6) . . ? C11 N2 Zn1 117.7(6) . . ? C12 N2 Zn1 124.7(5) . . ? C12 N2 C11 117.6(7) . . ? O5 N3 O7 115.1(6) . . ? O6 N3 O5 124.0(6) . . ? O6 N3 O7 120.9(6) . . ? C40 N4 Zn2 122.3(6) . . ? C40 N4 C41 116.9(8) . . ? C41 N4 Zn2 120.6(6) . . ? C43 N5 Zn2 119.9(6) . . ? C44 N5 Zn2 124.6(5) . . ? C44 N5 C43 115.5(7) . . ? 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 . . ? C3 C2 O1 125.5(9) . . ? C3 C2 C7 120.8(9) . . ? C7 C2 O1 113.7(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 C2 120.9(11) . . ? C4 C3 H3 119.6 . . ? C3 C4 H4 120.3 . . ? C3 C4 C5 119.4(9) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 118.7 . . ? C4 C5 C6 122.6(10) . . ? C6 C5 H5 118.7 . . ? C5 C6 C7 117.2(10) . . ? C5 C6 C8 119.3(9) . . ? C7 C6 C8 123.4(7) . . ? O2 C7 C2 117.5(7) . . ? O2 C7 C6 123.6(7) . . ? C2 C7 C6 118.9(7) . . ? N1 C8 C6 129.9(8) . . ? N1 C8 H8A 115.0 . . ? C6 C8 H8A 115.0 . . ? N1 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? N1 C9 C10 112.8(7) . . ? H9A C9 H9B 107.8 . . ? C10 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C9 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? C9 C10 C11 114.5(7) . . ? H10A C10 H10B 107.6 . . ? C11 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? N2 C11 C10 112.4(7) . . ? N2 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C10 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N2 C12 H12 116.5 . . ? N2 C12 C13 127.1(7) . . ? C13 C12 H12 116.5 . . ? C14 C13 C12 118.2(7) . . ? C18 C13 C12 124.0(6) . . ? C18 C13 C14 117.8(8) . . ? C13 C14 H14 119.1 . . ? C15 C14 C13 121.7(8) . . ? C15 C14 H14 119.1 . . ? C14 C15 H15 119.6 . . ? C14 C15 C16 120.9(8) . . ? C16 C15 H15 119.6 . . ? C15 C16 H16 120.7 . . ? C17 C16 C15 118.6(8) . . ? C17 C16 H16 120.7 . . ? O4 C17 C18 113.2(5) . . ? C16 C17 O4 124.5(7) . . ? C16 C17 C18 122.3(7) . . ? O3 C18 C13 123.6(7) . . ? O3 C18 C17 117.7(6) . . ? C17 C18 C13 118.7(6) . . ? 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 . . ? O9 C20 C21 125.5(6) . . ? O9 C20 C25 115.2(5) . . ? C21 C20 C25 119.3(5) . . ? C20 C21 Cl3 119.6(5) . . ? C22 C21 Cl3 118.7(5) . . ? C22 C21 C20 121.7(6) . . ? O11 C22 C21 125.6(6) . . ? O11 C22 C23 114.8(5) . . ? C21 C22 C23 119.6(5) . . ? O12 C23 C22 115.4(5) . . ? O12 C23 C24 126.0(6) . . ? C24 C23 C22 118.5(5) . . ? C23 C24 Cl4 119.8(5) . . ? C23 C24 C25 121.3(6) . . ? C25 C24 Cl4 118.9(5) . . ? O10 C25 C20 115.1(5) . . ? O10 C25 C24 125.3(6) . . ? C24 C25 C20 119.6(5) . . ? O13 C26 C27 125.3(6) . . ? O13 C26 C31 115.7(5) . . ? C27 C26 C31 119.0(5) . . ? C26 C27 Cl1 119.5(5) . . ? C28 C27 Cl1 119.4(5) . . ? C28 C27 C26 121.1(6) . . ? O15 C28 C27 124.9(6) . . ? O15 C28 C29 115.1(5) . . ? C27 C28 C29 120.0(5) . . ? O16 C29 C28 115.4(5) . . ? O16 C29 C30 125.8(6) . . ? C30 C29 C28 118.8(5) . . ? C29 C30 Cl2 119.3(5) . . ? C31 C30 Cl2 119.5(5) . . ? C31 C30 C29 121.2(6) . . ? O14 C31 C26 115.5(5) . . ? O14 C31 C30 124.9(6) . . ? C30 C31 C26 119.6(5) . . ? O8 C32 H32A 109.5 . . ? O8 C32 H32B 109.5 . . ? O8 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O17 C33 H33A 109.5 . . ? O17 C33 H33B 109.5 . . ? O17 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 O17 123.5(9) . . ? C35 C34 C39 122.2(10) . . ? C39 C34 O17 114.3(6) . . ? C34 C35 H35 119.9 . . ? C34 C35 C36 120.2(12) . . ? C36 C35 H35 119.9 . . ? C35 C36 H36 119.9 . . ? C37 C36 C35 120.1(10) . . ? C37 C36 H36 119.9 . . ? C36 C37 H37 120.3 . . ? C36 C37 C38 119.4(12) . . ? C38 C37 H37 120.3 . . ? C37 C38 C40 115.6(10) . . ? C39 C38 C37 119.4(11) . . ? C39 C38 C40 124.8(8) . . ? O18 C39 C34 118.0(7) . . ? O18 C39 C38 123.4(8) . . ? C34 C39 C38 118.6(7) . . ? N4 C40 C38 127.4(8) . . ? N4 C40 H40 116.3 . . ? C38 C40 H40 116.3 . . ? N4 C41 H41A 109.2 . . ? N4 C41 H41B 109.2 . . ? N4 C41 C42 112.2(7) . . ? H41A C41 H41B 107.9 . . ? C42 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C41 C42 H42A 108.3 . . ? C41 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C43 C42 C41 116.0(7) . . ? C43 C42 H42A 108.3 . . ? C43 C42 H42B 108.3 . . ? N5 C43 C42 111.3(7) . . ? N5 C43 H43A 109.4 . . ? N5 C43 H43B 109.4 . . ? C42 C43 H43A 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N5 C44 H44 116.5 . . ? N5 C44 C45 127.1(6) . . ? C45 C44 H44 116.5 . . ? C46 C45 C44 117.8(7) . . ? C50 C45 C44 123.9(7) . . ? C50 C45 C46 118.3(8) . . ? C45 C46 H46 119.2 . . ? C47 C46 C45 121.6(9) . . ? C47 C46 H46 119.2 . . ? C46 C47 H47 119.8 . . ? C46 C47 C48 120.3(8) . . ? C48 C47 H47 119.8 . . ? C47 C48 H48 120.4 . . ? C47 C48 C49 119.1(9) . . ? C49 C48 H48 120.4 . . ? O20 C49 C48 124.5(8) . . ? O20 C49 C50 113.1(6) . . ? C48 C49 C50 122.3(8) . . ? O19 C50 C45 124.3(7) . . ? O19 C50 C49 117.4(6) . . ? C49 C50 C45 118.2(7) . . ? O20 C51 H51A 109.5 . . ? O20 C51 H51B 109.5 . . ? O20 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O22 C52 H52A 109.5 . . ? O22 C52 H52B 109.5 . . ? O22 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O21 C53 H53A 109.5 . . ? O21 C53 H53B 109.5 . . ? O21 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O25 Cl5 O24 110.1 . . ? O25 Cl5 O27 106.3 . . ? O26 Cl5 O24 110.2 . . ? O26 Cl5 O25 106.7 . . ? O26 Cl5 O27 111.5 . . ? O27 Cl5 O24 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 3.4405(9) . ? Dy1 O1 2.561(5) . ? Dy1 O2 2.312(4) . ? Dy1 O3 2.274(4) . ? Dy1 O4 2.601(4) . ? Dy1 O6 2.524(4) . ? Dy1 O9 2.357(4) . ? Dy1 O10 2.399(4) . ? Dy1 O13 2.387(4) . ? Dy1 O14 2.380(4) . ? Dy2 Zn2 3.5145(9) . ? Dy2 O11 2.428(4) . ? Dy2 O12 2.358(4) . ? Dy2 O15 2.381(4) 1_565 ? Dy2 O16 2.411(4) 1_565 ? Dy2 O17 2.543(5) . ? Dy2 O18 2.317(4) . ? Dy2 O19 2.308(4) . ? Dy2 O20 2.567(5) . ? Dy2 O21 2.494(4) . ? Zn1 O2 2.021(4) . ? Zn1 O3 2.035(4) . ? Zn1 O5 2.333(5) . ? Zn1 O8 2.213(6) . ? Zn1 N1 2.049(6) . ? Zn1 N2 2.036(6) . ? Zn2 O18 2.045(4) . ? Zn2 O19 2.039(4) . ? Zn2 O22 2.104(6) . ? Zn2 N4 2.035(7) . ? Zn2 N5 2.024(6) . ? Cl1 C27 1.736(6) . ? Cl2 C30 1.732(6) . ? Cl3 C21 1.726(6) . ? Cl4 C24 1.721(6) . ? O1 C1 1.434(9) . ? O1 C2 1.411(10) . ? O2 C7 1.322(8) . ? O3 C18 1.349(7) . ? O4 C17 1.384(9) . ? O4 C19 1.446(9) . ? O5 N3 1.256(7) . ? O6 N3 1.242(7) . ? O7 N3 1.256(8) . ? O8 H8 0.8501 . ? O8 C32 1.377(9) . ? O9 C20 1.273(7) . ? O10 C25 1.262(7) . ? O11 C22 1.259(7) . ? O12 C23 1.253(7) . ? O13 C26 1.249(8) . ? O14 C31 1.255(7) . ? O15 C28 1.262(7) . ? O16 C29 1.251(7) . ? O17 C33 1.459(10) . ? O17 C34 1.391(10) . ? O18 C39 1.336(8) . ? O19 C50 1.323(8) . ? O20 C49 1.369(10) . ? O20 C51 1.441(9) . ? O21 H21 0.8638 . ? O21 C53 1.478(9) . ? O22 H22 0.8501 . ? O22 C52 1.385(11) . ? N1 C8 1.253(12) . ? N1 C9 1.455(11) . ? N2 C11 1.466(10) . ? N2 C12 1.279(11) . ? N4 C40 1.267(12) . ? N4 C41 1.467(11) . ? N5 C43 1.471(10) . ? N5 C44 1.286(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.377(11) . ? C2 C7 1.395(11) . ? C3 H3 0.9300 . ? C3 C4 1.353(17) . ? C4 H4 0.9300 . ? C4 C5 1.361(17) . ? C5 H5 0.9300 . ? C5 C6 1.404(12) . ? C6 C7 1.413(11) . ? C6 C8 1.445(14) . ? C8 H8A 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.525(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.529(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12 0.9300 . ? C12 C13 1.440(12) . ? C13 C14 1.424(11) . ? C13 C18 1.404(10) . ? C14 H14 0.9300 . ? C14 C15 1.350(14) . ? C15 H15 0.9300 . ? C15 C16 1.389(14) . ? C16 H16 0.9300 . ? C16 C17 1.376(10) . ? C17 C18 1.402(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.388(9) . ? C20 C25 1.527(9) . ? C21 C22 1.380(8) . ? C22 C23 1.548(8) . ? C23 C24 1.394(8) . ? C24 C25 1.395(8) . ? C26 C27 1.403(8) . ? C26 C31 1.522(9) . ? C27 C28 1.381(9) . ? C28 C29 1.523(9) . ? C29 C30 1.397(8) . ? C30 C31 1.393(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.372(12) . ? C34 C39 1.377(12) . ? C35 H35 0.9300 . ? C35 C36 1.38(2) . ? C36 H36 0.9300 . ? C36 C37 1.38(2) . ? C37 H37 0.9300 . ? C37 C38 1.433(14) . ? C38 C39 1.404(12) . ? C38 C40 1.444(14) . ? C40 H40 0.9300 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 C42 1.509(15) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 C43 1.499(15) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44 0.9300 . ? C44 C45 1.447(12) . ? C45 C46 1.423(12) . ? C45 C50 1.408(10) . ? C46 H46 0.9300 . ? C46 C47 1.368(15) . ? C47 H47 0.9300 . ? C47 C48 1.383(15) . ? C48 H48 0.9300 . ? C48 C49 1.385(11) . ? C49 C50 1.406(11) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? Cl5 O24 1.461(10) . ? Cl5 O25 1.434(9) . ? Cl5 O26 1.398(9) . ? Cl5 O27 1.450(10) . ? 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 O1 C2 C3 172.9(8) . . . . ? Dy1 O1 C2 C7 -6.6(8) . . . . ? Dy1 O2 C7 C2 5.8(8) . . . . ? Dy1 O2 C7 C6 -177.3(5) . . . . ? Dy1 O3 C18 C13 -174.6(4) . . . . ? Dy1 O3 C18 C17 4.9(8) . . . . ? Dy1 O4 C17 C16 174.3(6) . . . . ? Dy1 O4 C17 C18 -6.0(6) . . . . ? Dy1 O6 N3 O5 -25.6(10) . . . . ? Dy1 O6 N3 O7 155.5(6) . . . . ? Dy1 O9 C20 C21 -172.7(5) . . . . ? Dy1 O9 C20 C25 7.6(8) . . . . ? Dy1 O10 C25 C20 -4.6(7) . . . . ? Dy1 O10 C25 C24 174.9(5) . . . . ? Dy1 O13 C26 C27 172.4(5) . . . . ? Dy1 O13 C26 C31 -9.2(7) . . . . ? Dy1 O14 C31 C26 5.2(7) . . . . ? Dy1 O14 C31 C30 -176.0(5) . . . . ? Dy2 O11 C22 C21 -176.1(5) . . . . ? Dy2 O11 C22 C23 3.4(8) . . . . ? Dy2 O12 C23 C22 -9.2(8) . . . . ? Dy2 O12 C23 C24 171.2(5) . . . . ? Dy2 O15 C28 C27 166.9(5) 1_545 . . . ? Dy2 O15 C28 C29 -12.8(7) 1_545 . . . ? Dy2 O16 C29 C28 3.1(7) 1_545 . . . ? Dy2 O16 C29 C30 -177.3(5) 1_545 . . . ? Dy2 O17 C34 C35 -176.5(9) . . . . ? Dy2 O17 C34 C39 3.3(9) . . . . ? Dy2 O18 C39 C34 -5.1(9) . . . . ? Dy2 O18 C39 C38 176.0(6) . . . . ? Dy2 O19 C50 C45 169.3(5) . . . . ? Dy2 O19 C50 C49 -8.5(8) . . . . ? Dy2 O20 C49 C48 -168.9(6) . . . . ? Dy2 O20 C49 C50 13.5(7) . . . . ? Zn1 O2 C7 C2 165.2(5) . . . . ? Zn1 O2 C7 C6 -17.8(8) . . . . ? Zn1 O3 C18 C13 25.5(8) . . . . ? Zn1 O3 C18 C17 -154.9(4) . . . . ? Zn1 O5 N3 O6 17.1(9) . . . . ? Zn1 O5 N3 O7 -163.9(5) . . . . ? Zn1 N1 C8 C6 4.5(12) . . . . ? Zn1 N1 C9 C10 35.0(9) . . . . ? Zn1 N2 C11 C10 -42.7(8) . . . . ? Zn1 N2 C12 C13 -4.0(11) . . . . ? Zn2 O18 C39 C34 -156.3(6) . . . . ? Zn2 O18 C39 C38 24.8(9) . . . . ? Zn2 O19 C50 C45 -20.3(9) . . . . ? Zn2 O19 C50 C49 161.9(4) . . . . ? Zn2 N4 C40 C38 -7.3(12) . . . . ? Zn2 N4 C41 C42 -30.1(9) . . . . ? Zn2 N5 C43 C42 36.2(9) . . . . ? Zn2 N5 C44 C45 7.6(12) . . . . ? Cl1 C27 C28 O15 -1.1(9) . . . . ? Cl1 C27 C28 C29 178.7(4) . . . . ? Cl2 C30 C31 O14 -0.5(9) . . . . ? Cl2 C30 C31 C26 178.3(4) . . . . ? Cl3 C21 C22 O11 -0.7(10) . . . . ? Cl3 C21 C22 C23 180.0(5) . . . . ? Cl4 C24 C25 O10 1.4(10) . . . . ? Cl4 C24 C25 C20 -179.1(5) . . . . ? O1 C2 C3 C4 178.7(10) . . . . ? O1 C2 C7 O2 1.4(9) . . . . ? O1 C2 C7 C6 -175.7(6) . . . . ? O4 C17 C18 O3 1.6(8) . . . . ? O4 C17 C18 C13 -178.8(5) . . . . ? O9 C20 C21 Cl3 -0.5(10) . . . . ? O9 C20 C21 C22 -178.9(7) . . . . ? O9 C20 C25 O10 -1.8(9) . . . . ? O9 C20 C25 C24 178.7(6) . . . . ? O11 C22 C23 O12 3.6(9) . . . . ? O11 C22 C23 C24 -176.7(6) . . . . ? O12 C23 C24 Cl4 -1.9(11) . . . . ? O12 C23 C24 C25 176.7(7) . . . . ? O13 C26 C27 Cl1 -4.7(9) . . . . ? O13 C26 C27 C28 178.7(6) . . . . ? O13 C26 C31 O14 2.7(8) . . . . ? O13 C26 C31 C30 -176.3(6) . . . . ? O15 C28 C29 O16 6.2(8) . . . . ? O15 C28 C29 C30 -173.4(5) . . . . ? O16 C29 C30 Cl2 -2.2(9) . . . . ? O16 C29 C30 C31 176.1(6) . . . . ? O17 C34 C35 C36 -178.8(13) . . . . ? O17 C34 C39 O18 0.6(10) . . . . ? O17 C34 C39 C38 179.6(7) . . . . ? O20 C49 C50 O19 -4.6(9) . . . . ? O20 C49 C50 C45 177.5(6) . . . . ? N1 C9 C10 C11 -71.5(10) . . . . ? N2 C12 C13 C14 169.5(7) . . . . ? N2 C12 C13 C18 -11.9(12) . . . . ? N4 C41 C42 C43 72.2(9) . . . . ? N5 C44 C45 C46 -174.3(8) . . . . ? N5 C44 C45 C50 7.2(13) . . . . ? C1 O1 C2 C3 -10.9(12) . . . . ? C1 O1 C2 C7 169.7(7) . . . . ? C2 C3 C4 C5 -3.1(18) . . . . ? C3 C2 C7 O2 -178.1(8) . . . . ? C3 C2 C7 C6 4.8(12) . . . . ? C3 C4 C5 C6 5.1(18) . . . . ? C4 C5 C6 C7 -2.0(14) . . . . ? C4 C5 C6 C8 -177.8(10) . . . . ? C5 C6 C7 O2 -179.8(7) . . . . ? C5 C6 C7 C2 -2.8(10) . . . . ? C5 C6 C8 N1 -172.8(9) . . . . ? C7 C2 C3 C4 -1.8(16) . . . . ? C7 C6 C8 N1 11.7(13) . . . . ? C8 N1 C9 C10 -144.6(8) . . . . ? C8 C6 C7 O2 -4.2(11) . . . . ? C8 C6 C7 C2 172.7(7) . . . . ? C9 N1 C8 C6 -176.0(8) . . . . ? C9 C10 C11 N2 76.7(9) . . . . ? C11 N2 C12 C13 179.5(7) . . . . ? C12 N2 C11 C10 134.1(8) . . . . ? C12 C13 C14 C15 -179.5(8) . . . . ? C12 C13 C18 O3 -0.1(10) . . . . ? C12 C13 C18 C17 -179.7(6) . . . . ? C13 C14 C15 C16 -2.2(14) . . . . ? C14 C13 C18 O3 178.4(6) . . . . ? C14 C13 C18 C17 -1.1(9) . . . . ? C14 C15 C16 C17 1.8(13) . . . . ? C15 C16 C17 O4 178.5(7) . . . . ? C15 C16 C17 C18 -1.1(11) . . . . ? C16 C17 C18 O3 -178.7(6) . . . . ? C16 C17 C18 C13 0.9(10) . . . . ? C18 C13 C14 C15 1.8(12) . . . . ? C19 O4 C17 C16 9.0(10) . . . . ? C19 O4 C17 C18 -171.3(7) . . . . ? C20 C21 C22 O11 177.7(7) . . . . ? C20 C21 C22 C23 -1.7(11) . . . . ? C21 C20 C25 O10 178.4(6) . . . . ? C21 C20 C25 C24 -1.1(10) . . . . ? C21 C22 C23 O12 -177.0(6) . . . . ? C21 C22 C23 C24 2.7(10) . . . . ? C22 C23 C24 Cl4 178.4(5) . . . . ? C22 C23 C24 C25 -3.0(10) . . . . ? C23 C24 C25 O10 -177.2(7) . . . . ? C23 C24 C25 C20 2.3(10) . . . . ? C25 C20 C21 Cl3 179.3(5) . . . . ? C25 C20 C21 C22 0.9(11) . . . . ? C26 C27 C28 O15 175.5(6) . . . . ? C26 C27 C28 C29 -4.7(9) . . . . ? C27 C26 C31 O14 -178.8(5) . . . . ? C27 C26 C31 C30 2.2(8) . . . . ? C27 C28 C29 O16 -173.6(6) . . . . ? C27 C28 C29 C30 6.9(8) . . . . ? C28 C29 C30 Cl2 177.3(4) . . . . ? C28 C29 C30 C31 -4.3(9) . . . . ? C29 C30 C31 O14 -178.8(6) . . . . ? C29 C30 C31 C26 0.0(9) . . . . ? C31 C26 C27 Cl1 176.9(4) . . . . ? C31 C26 C27 C28 0.3(9) . . . . ? C33 O17 C34 C35 9.5(13) . . . . ? C33 O17 C34 C39 -170.7(7) . . . . ? C34 C35 C36 C37 -1(3) . . . . ? C35 C34 C39 O18 -179.6(9) . . . . ? C35 C34 C39 C38 -0.6(14) . . . . ? C35 C36 C37 C38 0(3) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C36 C37 C38 C40 176.3(14) . . . . ? C37 C38 C39 O18 178.2(10) . . . . ? C37 C38 C39 C34 -0.7(14) . . . . ? C37 C38 C40 N4 171.3(10) . . . . ? C39 C34 C35 C36 1(2) . . . . ? C39 C38 C40 N4 -13.9(15) . . . . ? C40 N4 C41 C42 145.6(8) . . . . ? C40 C38 C39 O18 3.6(14) . . . . ? C40 C38 C39 C34 -175.3(8) . . . . ? C41 N4 C40 C38 177.1(8) . . . . ? C41 C42 C43 N5 -75.8(9) . . . . ? C43 N5 C44 C45 -175.0(8) . . . . ? C44 N5 C43 C42 -141.4(8) . . . . ? C44 C45 C46 C47 -176.7(8) . . . . ? C44 C45 C50 O19 -0.2(11) . . . . ? C44 C45 C50 C49 177.6(7) . . . . ? C45 C46 C47 C48 -1.8(15) . . . . ? C46 C45 C50 O19 -178.6(7) . . . . ? C46 C45 C50 C49 -0.8(10) . . . . ? C46 C47 C48 C49 0.8(14) . . . . ? C47 C48 C49 O20 -177.2(8) . . . . ? C47 C48 C49 C50 0.2(12) . . . . ? C48 C49 C50 O19 177.8(7) . . . . ? C48 C49 C50 C45 -0.2(10) . . . . ? C50 C45 C46 C47 1.8(13) . . . . ? C51 O20 C49 C48 -4.9(11) . . . . ? C51 O20 C49 C50 177.5(6) . . . . ? 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 -0.113 0.000 0.000 295.9 68.4 ? 2 0.325 0.668 0.533 69.6 15.1 ? 3 0.675 0.332 0.467 69.6 12.7 ?