#------------------------------------------------------------------------------ #$Date: 2021-04-22 04:49:30 +0300 (Thu, 22 Apr 2021) $ #$Revision: 264381 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707166.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_7707166 loop_ _publ_author_name 'Zeng, Min' 'Hu, kong-Qiu' 'Liu, Cai-Ming' 'Kou, Hui-Zhong' _publ_section_title ; Heterotrimetallic Ni2Ln2Fe3 chain complexes based on [Fe(1-CH3im)(CN)5]2- ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00693B _journal_year 2021 _chemical_formula_moiety 'C80 H95 Dy2 Fe3 N30 Ni2 O14, 4[C3H7NO], 12[H2O]' _chemical_formula_sum 'C92 H147 Dy2 Fe3 N34 Ni2 O30' _chemical_formula_weight 2819.40 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2021-03-20 _audit_creation_method ; Olex2 1.5-dev (compiled 2021.02.10 svn.rb'16c95d35' for OlexSys, GUI svn.r6225) ; _audit_update_record ; 2021-04-09 deposited with the CCDC. 2021-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.35(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.924(5) _cell_length_b 13.097(3) _cell_length_c 39.319(8) _cell_measurement_reflns_used 23771 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 29.1138 _cell_measurement_theta_min 1.9563 _cell_volume 13639(5) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'Olex2 1.5-dev (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-dev (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution SHELXS-93 _diffrn_ambient_temperature 153.15 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_number 66883 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.999 _diffrn_reflns_theta_min 1.956 _exptl_absorpt_coefficient_mu 1.736 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6473 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.373 _exptl_crystal_description prism _exptl_crystal_F_000 5772 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.973 _refine_diff_density_min -1.706 _refine_diff_density_rms 0.106 _refine_ls_extinction_coef 0.00018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 692 _refine_ls_number_reflns 14834 _refine_ls_number_restraints 206 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0664 _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^+73.3072P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1585 _refine_ls_wR_factor_ref 0.1611 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13654 _reflns_number_total 14834 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00693b2.cif _cod_data_source_block 2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7707166 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.846 _shelx_estimated_absorpt_t_min 0.380 _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 2. Shared sites {O7, O1W} 3. Restrained distances N14-C30 = C30-N17 = N17-C43 = C43-C42 = C42-N14 1.36 with sigma of 0.01 N17-C40 1.42 with sigma of 0.02 C40-C43 = C40-C30 2.5 with sigma of 0.02 Fe2-C41 = Fe2-C47 = Fe2-C31 1.95 with sigma of 0.02 Fe2-N19 = Fe2-N16 = Fe2-N13 3.1 with sigma of 0.02 O7-C52 1.28 with sigma of 0.01 N21-C52 = N21-C53 = N21-C54 1.38 with sigma of 0.02 C53-C52 = C54-C53 = C52-C54 2.4 with sigma of 0.02 O7-N21 2.3 with sigma of 0.02 C6-C23 \\sim C42-C30 with sigma of 0.001 4. Restrained planarity N14, N17, C30, C42, C43, C40 with sigma of 0.1 5. Uiso/Uaniso restraints and constraints Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01 Uanis(C54) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(N19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 6. Rigid body (RIGU) restrains O7, N21, C52, C53, C54 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 Fe2, C9, C30, C31, C40, C41, C42, C43, C47, N10, N13, N14, N16, N17, N19 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 7. Others Fixed Sof: C30(0.5) H30(0.5) C31(0.5) C36(0.58) H36(0.58) C37(0.58) H37A(0.58) H37B(0.58) H37C(0.58) C38(0.58) H38A(0.58) H38B(0.58) H38C(0.58) C36A(0.42) H36A(0.42) C37A(0.42) H37D(0.42) H37E(0.42) H37F(0.42) C38A(0.42) H38D(0.42) H38E(0.42) H38F(0.42) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C47(0.5) N13(0.5) N14(0.5) N16(0.5) N17(0.5) N19(0.5) N21(0.5) C52(0.5) H52(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) 8.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B) 8.b Me refined with riding coordinates: C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B, H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C37A(H37D,H37E,H37F), C38A(H38D,H38E,H38F), C40(H40A,H40B,H40C), C53(H53A,H53B,H53C), C54(H54A,H54B, H54C) 8.c Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C23(H23), C25(H25), C30(H30), C36(H36), C36A(H36A), C42(H42), C43(H43), C52(H52) 8.d Idealised Me refined as rotating group: C4(H4A,H4B,H4C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 1129 electrons were found in a volume of 4715\%A^3^ in 1 void per unit cell. This is consistent with the presence of 4[C3H7NO], 12[H2O] per Formula Unit which account for 1120 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 2 in C2/c 2.res created by SHELXL-2018/3 at 11:35:27 on 20-Mar-2021 CELL 0.71073 26.9237 13.0968 39.3193 90 100.352 90 ZERR 4 0.0054 0.0026 0.0079 0 0.03 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C Dy Fe H N Ni O UNIT 368 8 12 588 136 8 120 EQIV $1 -X,3-Y,1-Z EQIV $2 -X,+Y,0.5-Z FLAT N14 N17 C30 C42 C43 C40 DFIX 1.36 0.01 N14 C30 C30 N17 N17 C43 C43 C42 C42 N14 DFIX 1.42 N17 C40 DFIX 2.5 C40 C43 C40 C30 DFIX 1.95 Fe2 C41 Fe2 C47 Fe2 C31 DFIX 3.1 Fe2 N19 Fe2 N16 Fe2 N13 DFIX 1.28 0.01 O7 C52 DFIX 1.38 N21 C52 N21 C53 N21 C54 DFIX 2.4 C53 C52 C54 C53 C52 C54 DFIX 2.3 O7 N21 ISOR 0.05 0.01 C42 C43 C40 C53 SADI 0.001 C6 C23 C42 C30 RIGU 0.001 0.001 O7 N21 C52 C53 C54 RIGU 0.001 0.001 Fe2 C9 C30 C31 C40 C41 C42 C43 C47 N10 N13 N14 N16 N17 N19 ISOR 0.01 0.02 C54 N16 N19 EXYZ o7 o1w EADP o7 o1w L.S. 6 PLAN 42 SIZE 0.69 0.21 0.1 TEMP -120 RTAB rdis Ni1 Dy1 RTAB rdis Ni1 Fe1 RTAB rdis Ni1 Fe2 RTAB rdis Dy1 Fe1_$1 FREE Dy1 Ni1 FREE C31 C41_$2 FREE C31 C47_$2 FREE N19 C42_$2 FREE N19 N14_$2 FREE C41 C41_$2 FREE C41 C31_$2 FREE C42 N19_$2 FREE C42 C47_$2 FREE N14 C47_$2 FREE N14 N19_$2 FREE C47 N14_$2 FREE C47 C42_$2 FREE C47 C31_$2 bond $h htab DAMP 0.01 BOND fmap 2 acta ABIN OMIT 0 54 OMIT -2 0 4 OMIT 1 1 2 OMIT -3 3 8 OMIT 2 0 10 OMIT -4 0 2 OMIT 0 2 9 OMIT -3 1 1 OMIT -5 3 7 OMIT -2 2 3 OMIT -4 0 8 OMIT -1 1 3 OMIT 1 1 9 REM REM REM > REM REM > REM > REM REM WGHT 0.060000 73.307205 EXTI 0.000178 FVAR 0.09080 DY1 2 -0.114292 1.541122 0.402836 11.00000 0.03376 0.03766 = 0.05959 0.01354 0.01297 -0.00567 NI1 6 -0.005010 1.618917 0.377633 11.00000 0.03949 0.03804 = 0.05170 0.00626 0.01745 -0.00868 FE1 3 0.086448 1.743399 0.492937 11.00000 0.03074 0.03202 = 0.05321 0.00807 0.01412 -0.00076 FE2 3 0.000000 1.588728 0.250000 10.50000 0.09372 0.05755 = 0.05445 0.00000 0.00638 0.00000 C1 1 -0.113592 1.973025 0.400251 11.00000 0.06570 0.03408 = 0.11390 0.00867 0.02218 -0.00077 AFIX 43 H1 4 -0.123311 2.040991 0.404384 11.00000 -1.20000 AFIX 0 C2 1 0.106820 1.589037 0.372546 11.00000 0.04924 0.05421 = 0.08194 -0.00561 0.03009 -0.01081 AFIX 23 H2A 4 0.134728 1.553887 0.387957 11.00000 -1.20000 H2B 4 0.112878 1.581367 0.348577 11.00000 -1.20000 AFIX 0 C3 1 -0.010519 1.194645 0.361234 11.00000 0.10012 0.02371 = 0.11205 -0.00740 0.05150 -0.00167 AFIX 43 H3 4 -0.002908 1.125442 0.357058 11.00000 -1.20000 AFIX 0 C4 1 -0.156841 1.289205 0.372043 11.00000 0.05082 0.05930 = 0.09016 0.00048 0.01012 -0.02031 AFIX 137 H4A 4 -0.159957 1.258218 0.349070 11.00000 -1.50000 H4B 4 -0.187951 1.326223 0.373695 11.00000 -1.50000 H4C 4 -0.151178 1.235609 0.389709 11.00000 -1.50000 AFIX 0 C5 1 -0.147737 1.892820 0.401026 11.00000 0.05264 0.05854 = 0.10178 0.01405 0.02556 0.00709 AFIX 43 H5 4 -0.180628 1.905461 0.405649 11.00000 -1.20000 AFIX 0 C6 1 0.022573 1.839121 0.540331 11.00000 0.04573 0.07623 = 0.05253 0.00006 0.00853 0.01490 AFIX 43 H6 4 0.046729 1.827368 0.560729 11.00000 -1.20000 AFIX 0 C7 1 0.109196 1.698451 0.381287 11.00000 0.05333 0.07238 = 0.10434 -0.00247 0.03367 -0.02158 AFIX 23 H7A 4 0.143179 1.722793 0.378818 11.00000 -1.20000 H7B 4 0.107205 1.703906 0.406119 11.00000 -1.20000 AFIX 0 C8 1 0.072045 1.772210 0.362475 11.00000 0.06381 0.06098 = 0.06942 0.00409 0.03286 -0.01774 AFIX 23 H8A 4 0.084451 1.842575 0.367847 11.00000 -1.20000 H8B 4 0.069349 1.761513 0.337284 11.00000 -1.20000 AFIX 0 C9 1 -0.016486 1.594639 0.296058 11.00000 0.07510 0.05408 = 0.05959 0.00680 0.00525 -0.02175 C10 1 -0.023404 1.880068 0.539250 11.00000 0.04444 0.06602 = 0.07111 -0.00774 0.01807 0.01292 AFIX 43 H10 4 -0.037553 1.902612 0.558403 11.00000 -1.20000 AFIX 0 C11 1 0.026615 1.266814 0.363779 11.00000 0.06713 0.04004 = 0.09251 -0.00485 0.03691 -0.00347 AFIX 43 H11 4 0.059215 1.247680 0.359984 11.00000 -1.20000 AFIX 0 C12 1 0.059639 1.439281 0.372643 11.00000 0.05223 0.03989 = 0.06295 -0.00352 0.02427 -0.00133 AFIX 43 H12 4 0.091368 1.409734 0.371060 11.00000 -1.20000 AFIX 0 C13 1 -0.059843 1.221737 0.364729 11.00000 0.07945 0.03525 = 0.06972 -0.00201 0.02359 -0.01039 AFIX 43 H13 4 -0.086232 1.172608 0.361454 11.00000 -1.20000 AFIX 0 C14 1 -0.068866 1.320268 0.372937 11.00000 0.05870 0.04046 = 0.04663 -0.00002 0.01284 -0.00763 C15 1 -0.132682 1.796182 0.394994 11.00000 0.04609 0.04076 = 0.08380 0.02436 0.01542 -0.00108 C16 1 -0.000449 1.843489 0.377900 11.00000 0.05437 0.04027 = 0.05926 0.00775 0.01482 -0.01892 AFIX 43 H16 4 0.017691 1.905047 0.376386 11.00000 -1.20000 AFIX 0 C17 1 -0.065967 1.953941 0.393525 11.00000 0.06468 0.03067 = 0.09283 0.01450 0.02484 -0.00230 AFIX 43 H17 4 -0.043116 2.009057 0.393206 11.00000 -1.20000 AFIX 0 C18 1 -0.030643 1.397686 0.376792 11.00000 0.04720 0.02824 = 0.04430 0.00244 0.01390 -0.00379 C19 1 -0.084327 1.772088 0.388091 11.00000 0.04333 0.03563 = 0.05682 0.01229 0.00973 -0.00590 C20 1 0.017566 1.368023 0.371843 11.00000 0.05765 0.03254 = 0.05932 0.00292 0.01966 0.00704 C21 1 0.092924 1.848856 0.458732 11.00000 0.03157 0.03977 = 0.06262 0.00409 0.01774 0.00498 C22 1 0.136868 1.813059 0.526810 11.00000 0.03889 0.04123 = 0.06425 0.01034 0.02033 0.00436 C23 1 -0.013366 1.845210 0.487282 11.00000 0.03499 0.04072 = 0.05622 0.00820 0.00542 0.00334 AFIX 43 H23 4 -0.019934 1.839189 0.462806 11.00000 -1.20000 AFIX 0 C24 1 -0.050624 1.854089 0.387120 11.00000 0.04815 0.03653 = 0.06587 0.01371 0.01471 -0.00565 C25 1 -0.207847 1.434579 0.436590 11.00000 0.03359 0.07135 = 0.07803 0.02332 0.00903 -0.01772 AFIX 43 H25 4 -0.186341 1.417865 0.457754 11.00000 -1.20000 AFIX 0 C26 1 0.042126 1.673419 0.455714 11.00000 0.03234 0.03746 = 0.05562 0.01497 0.02286 0.00234 C27 1 0.084003 1.640955 0.528477 11.00000 0.02556 0.03367 = 0.06780 0.00032 0.01353 -0.00045 C29 1 0.139354 1.663306 0.479085 11.00000 0.04051 0.04433 = 0.05747 0.01288 0.01655 -0.00537 PART -1 C30 1 0.042889 1.381622 0.230893 10.50000 0.16618 0.09884 = 0.08969 -0.01029 0.02838 0.01258 AFIX 43 H30 4 0.028382 1.387046 0.207085 10.50000 -1.20000 AFIX 0 C31 1 0.066313 1.649926 0.267507 10.50000 0.09873 0.07414 = 0.04155 -0.00844 0.03146 -0.00809 PART 0 C32 1 -0.097331 1.917865 0.491902 11.00000 0.03869 0.04641 = 0.10979 -0.01440 0.00646 0.00719 AFIX 33 H32A 4 -0.112985 1.942300 0.511041 11.00000 -1.50000 H32B 4 -0.096283 1.973532 0.475390 11.00000 -1.50000 H32C 4 -0.117163 1.861060 0.480255 11.00000 -1.50000 AFIX 0 C33 1 -0.271154 1.328066 0.455055 11.00000 0.04676 0.10680 = 0.14935 0.07789 0.03182 -0.00563 AFIX 33 H33A 4 -0.306506 1.311097 0.445991 11.00000 -1.50000 H33B 4 -0.250781 1.265617 0.457104 11.00000 -1.50000 H33C 4 -0.268590 1.359890 0.477862 11.00000 -1.50000 AFIX 0 C34 1 -0.286600 1.418204 0.398341 11.00000 0.05627 0.09956 = 0.13115 0.03842 -0.00371 -0.02102 AFIX 33 H34A 4 -0.319426 1.386005 0.398456 11.00000 -1.50000 H34B 4 -0.291169 1.491988 0.394999 11.00000 -1.50000 H34C 4 -0.271631 1.389666 0.379466 11.00000 -1.50000 AFIX 0 C35 1 -0.214719 1.724294 0.397843 11.00000 0.04154 0.05592 = 0.22202 0.04498 0.03536 0.01113 AFIX 33 H35A 4 -0.231535 1.657836 0.397474 11.00000 -1.50000 H35B 4 -0.216486 1.759278 0.419626 11.00000 -1.50000 H35C 4 -0.231571 1.765816 0.378418 11.00000 -1.50000 AFIX 0 PART 1 C36 1 -0.075196 1.622093 0.482542 10.58000 0.04134 0.03530 = 0.05885 0.01088 0.01678 -0.00452 AFIX 43 H36 4 -0.039922 1.609758 0.485365 10.58000 -1.20000 AFIX 0 C37 1 -0.150385 1.645311 0.506496 10.58000 0.07310 0.06955 = 0.10917 -0.00160 0.05376 -0.00774 AFIX 33 H37A 4 -0.160944 1.646211 0.529083 10.58000 -1.50000 H37B 4 -0.157964 1.711470 0.495098 10.58000 -1.50000 H37C 4 -0.168631 1.591296 0.492148 10.58000 -1.50000 AFIX 0 C38 1 -0.066942 1.610244 0.544738 10.58000 0.08181 0.05749 = 0.07504 0.00020 0.02091 -0.00287 AFIX 33 H38A 4 -0.088491 1.615793 0.562264 10.58000 -1.50000 H38B 4 -0.051678 1.542122 0.545829 10.58000 -1.50000 H38C 4 -0.040259 1.661981 0.549110 10.58000 -1.50000 AFIX 0 PART 2 C36A 1 -0.121890 1.635666 0.480932 10.42000 0.05280 0.04069 = 0.06137 -0.00222 0.01718 -0.00665 AFIX 43 H36A 4 -0.157460 1.644474 0.477602 10.42000 -1.20000 AFIX 0 C37A 1 -0.127295 1.633512 0.541596 10.42000 0.05719 0.07694 = 0.06279 -0.00659 0.00794 -0.00344 AFIX 33 H37D 4 -0.104211 1.625062 0.563711 10.42000 -1.50000 H37E 4 -0.143728 1.700415 0.541015 10.42000 -1.50000 H37F 4 -0.152986 1.579692 0.539035 10.42000 -1.50000 AFIX 0 C38A 1 -0.044307 1.606215 0.522140 10.42000 0.04676 0.03733 = 0.09373 0.00245 0.01428 -0.00037 AFIX 33 H38D 4 -0.036577 1.603226 0.547445 10.42000 -1.50000 H38E 4 -0.035689 1.540823 0.512566 10.42000 -1.50000 H38F 4 -0.024572 1.660930 0.513968 10.42000 -1.50000 AFIX 0 PART -1 C40 1 0.094716 1.229853 0.227284 10.50000 0.16577 0.13034 = 0.13131 -0.02485 0.01846 0.02933 AFIX 33 H40A 4 0.112922 1.180417 0.243655 10.50000 -1.50000 H40B 4 0.069114 1.194210 0.210611 10.50000 -1.50000 H40C 4 0.118555 1.264269 0.214987 10.50000 -1.50000 AFIX 0 C41 1 -0.024988 1.722729 0.239474 10.50000 0.12049 0.09582 = 0.05689 0.01811 0.04126 0.02280 C42 1 0.065220 1.414704 0.284697 10.50000 0.20534 0.08505 = 0.08266 0.01322 0.01423 0.03609 AFIX 43 H42 4 0.069930 1.448495 0.306419 10.50000 -1.20000 AFIX 0 C43 1 0.085572 1.321537 0.279537 10.50000 0.18137 0.07460 = 0.11052 0.01020 0.03174 0.01632 AFIX 43 H43 4 0.105324 1.279640 0.296527 10.50000 -1.20000 AFIX 0 C47 1 -0.057335 1.522971 0.225220 10.50000 0.11060 0.13307 = 0.04558 0.00689 0.01935 -0.03056 PART 0 N1 5 0.017947 1.637136 0.431344 11.00000 0.03932 0.03761 = 0.05275 0.00733 0.01748 -0.00159 N2 5 0.167423 1.854755 0.546228 11.00000 0.03983 0.04707 = 0.07678 -0.00182 0.00840 -0.00876 N3 5 0.095961 1.912169 0.439254 11.00000 0.05318 0.04867 = 0.06541 0.01774 0.02392 -0.00004 N4 5 0.170525 1.612067 0.470659 11.00000 0.04198 0.04919 = 0.07695 0.01009 0.02192 0.00734 N5 5 0.085987 1.582295 0.550685 11.00000 0.04349 0.03829 = 0.05949 0.01575 0.01306 0.00172 N6 5 0.029216 1.816764 0.507085 11.00000 0.03285 0.03073 = 0.05980 0.00376 0.01204 -0.00106 N7 5 -0.045730 1.882956 0.505414 11.00000 0.03392 0.03750 = 0.07270 -0.00430 0.01340 -0.00081 N8 5 0.021614 1.761405 0.371693 11.00000 0.04653 0.03289 = 0.05721 0.00813 0.02023 -0.01174 N9 5 0.058781 1.535947 0.375204 11.00000 0.04091 0.05011 = 0.05401 -0.00298 0.01974 -0.01316 N10 5 -0.024001 1.601414 0.323825 11.00000 0.06034 0.05282 = 0.05830 0.00973 0.00218 -0.01863 N11 5 -0.096744 1.626077 0.511154 11.00000 0.05133 0.04641 = 0.06190 0.00001 0.01480 -0.00980 PART -1 N13 5 0.106230 1.684286 0.279797 10.50000 0.10196 0.11976 = 0.05693 -0.02667 0.03768 -0.02225 N14 5 0.037321 1.453705 0.255044 10.50000 0.12272 0.06808 = 0.06457 0.01137 0.03086 -0.01448 PART 0 N15 5 -0.252776 1.398526 0.431673 11.00000 0.03257 0.06833 = 0.10609 0.03132 0.02159 -0.00592 PART -1 N16 5 -0.044416 1.798568 0.232583 10.50000 0.20310 0.11954 = 0.10053 0.03032 0.05018 0.06609 N17 5 0.071759 1.300594 0.244876 10.50000 0.20892 0.10759 = 0.11653 -0.00823 0.02716 0.03699 N19 5 -0.095323 1.487040 0.210952 10.50000 0.13509 0.19701 = 0.09231 0.00617 0.00182 -0.06381 PART 0 O1 7 -0.073943 1.676120 0.382707 11.00000 0.03950 0.03074 = 0.06244 0.01567 0.01654 -0.00585 O2 7 -0.043237 1.489226 0.384964 11.00000 0.03935 0.03385 = 0.06032 0.00158 0.01917 -0.00885 O3 7 -0.115033 1.358826 0.377392 11.00000 0.04270 0.03736 = 0.07802 0.00210 0.01266 -0.01503 O4 7 -0.162554 1.709502 0.394916 11.00000 0.03440 0.04254 = 0.10247 0.02647 0.01647 0.00246 O5 7 -0.189990 1.489621 0.415999 11.00000 0.03515 0.05568 = 0.08523 0.02039 0.01975 -0.00802 O6 7 -0.098723 1.633472 0.453746 11.00000 0.06367 0.03886 = 0.06825 0.00369 0.01789 -0.00346 O1W 7 -0.163019 1.540859 0.348234 10.50000 0.05587 0.05794 = 0.09564 0.01545 -0.00810 -0.00715 O7 7 -0.163019 1.540859 0.348234 10.50000 0.05587 0.05794 = 0.09564 0.01545 -0.00810 -0.00715 PART -1 N21 5 -0.190446 1.532861 0.291258 10.50000 0.10349 0.15010 = 0.09791 0.00390 0.00040 -0.02646 C52 1 -0.153809 1.544715 0.318481 10.50000 0.10297 0.10452 = 0.09869 0.00671 0.00468 -0.02687 AFIX 43 H52 4 -0.120192 1.556270 0.315122 10.50000 -1.20000 AFIX 0 C53 1 -0.178280 1.520947 0.258296 10.50000 0.17269 0.17885 = 0.10658 -0.00934 0.01897 -0.01622 AFIX 33 H53A 4 -0.209360 1.513154 0.241199 10.50000 -1.50000 H53B 4 -0.159812 1.581238 0.252621 10.50000 -1.50000 H53C 4 -0.157160 1.460116 0.258019 10.50000 -1.50000 AFIX 0 C54 1 -0.241341 1.530900 0.293411 10.50000 0.10320 0.23201 = 0.17212 0.03496 0.00859 -0.02304 AFIX 33 H54A 4 -0.261485 1.521415 0.270266 10.50000 -1.50000 H54B 4 -0.247773 1.474366 0.308363 10.50000 -1.50000 H54C 4 -0.250693 1.595534 0.303125 10.50000 -1.50000 AFIX 0 HKLF 4 REM 2 in C2/c REM wR2 = 0.1611, GooF = S = 1.105, Restrained GooF = 1.111 for all data REM R1 = 0.0664 for 13654 Fo > 4sig(Fo) and 0.0706 for all 14834 data REM 692 parameters refined using 195 restraints END WGHT 0.0600 73.3086 REM Instructions for potential hydrogen bonds HTAB C2 N19_$2 HTAB C35 O5 HTAB C38 N1_$1 HTAB C37A N4_$1 HTAB C38A N6 HTAB C52 N10 REM Highest difference peak 0.973, deepest hole -1.706, 1-sigma level 0.106 Q1 1 -0.1576 1.4124 0.2926 11.00000 0.05 0.97 Q2 1 0.0999 1.6886 0.3530 11.00000 0.05 0.90 Q3 1 0.1069 1.3649 0.2130 11.00000 0.05 0.90 Q4 1 -0.1164 1.4218 0.4069 11.00000 0.05 0.85 Q5 1 0.0970 1.2985 0.2246 11.00000 0.05 0.85 Q6 1 -0.1991 1.5335 0.3277 11.00000 0.05 0.71 Q7 1 -0.1575 1.4702 0.2849 11.00000 0.05 0.69 Q8 1 0.1412 1.2151 0.2396 11.00000 0.05 0.66 Q9 1 0.0496 1.2741 0.2245 11.00000 0.05 0.65 Q10 1 0.0601 1.2232 0.2331 11.00000 0.05 0.64 Q11 1 0.0202 1.6982 0.3684 11.00000 0.05 0.61 Q12 1 -0.2056 1.5770 0.2964 11.00000 0.05 0.59 Q13 1 -0.1211 1.6223 0.3790 11.00000 0.05 0.57 Q14 1 -0.1885 1.5057 0.2973 11.00000 0.05 0.57 Q15 1 -0.1228 1.5752 0.3999 11.00000 0.05 0.55 Q16 1 -0.1216 1.5239 0.4371 11.00000 0.05 0.54 Q17 1 -0.0890 1.6202 0.3881 11.00000 0.05 0.52 Q18 1 0.0000 1.4472 0.2500 10.50000 0.05 0.52 Q19 1 0.0997 1.5371 0.5729 11.00000 0.05 0.51 Q20 1 -0.1922 1.5934 0.2917 11.00000 0.05 0.49 Q21 1 -0.3086 1.3420 0.4618 11.00000 0.05 0.49 Q22 1 -0.1791 1.5756 0.2880 11.00000 0.05 0.48 Q23 1 -0.1595 1.5269 0.3224 11.00000 0.05 0.47 Q24 1 -0.1052 1.5195 0.3925 11.00000 0.05 0.47 Q25 1 -0.1317 1.3225 0.4077 11.00000 0.05 0.46 Q26 1 -0.0147 1.3460 0.3794 11.00000 0.05 0.44 Q27 1 -0.1188 1.6454 0.3938 11.00000 0.05 0.44 Q28 1 0.0035 1.5168 0.3718 11.00000 0.05 0.44 Q29 1 -0.1002 1.5541 0.4168 11.00000 0.05 0.43 Q30 1 -0.1426 1.6259 0.4160 11.00000 0.05 0.42 Q31 1 -0.1182 1.9162 0.3993 11.00000 0.05 0.42 Q32 1 -0.1502 1.5030 0.3764 11.00000 0.05 0.42 Q33 1 -0.1476 1.5967 0.3762 11.00000 0.05 0.42 Q34 1 0.2490 1.4994 0.4549 11.00000 0.05 0.42 Q35 1 -0.1421 1.7121 0.4771 11.00000 0.05 0.41 Q36 1 -0.0661 1.5472 0.4054 11.00000 0.05 0.41 Q37 1 0.0149 1.5683 0.2417 11.00000 0.05 0.40 Q38 1 -0.2410 1.3037 0.4774 11.00000 0.05 0.40 Q39 1 0.0000 1.7494 0.2500 10.50000 0.05 0.40 Q40 1 0.0013 1.4136 0.3696 11.00000 0.05 0.39 Q41 1 -0.0886 1.7783 0.5106 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4.8869 -0.2173 26 10 4 1.0860 0.4474 26 10 5 4.9304 0.7133 26 10 6 1.8512 0.4980 27 1 0 -9.6036 -3.4826 27 1 1 1.4369 -1.2650 27 1 2 0.1205 1.0859 27 1 3 0.2575 0.7231 27 1 4 7.3985 0.2071 27 1 5 -0.3409 0.6664 27 1 6 -5.8409 -0.8358 27 1 7 4.2178 -0.3228 27 1 8 -1.4595 0.5080 27 1 9 7.6699 0.2355 27 1 10 3.2852 0.5267 27 1 11 6.2666 0.0342 27 1 12 4.1194 -0.6047 27 1 13 -4.3517 -0.1758 27 1 14 2.3367 -0.0457 27 1 15 -3.2453 0.0375 27 1 16 -4.4283 0.0849 27 1 17 -0.9216 0.0164 27 1 18 -2.6267 0.2250 27 1 19 1.9416 -0.2307 27 1 20 5.0900 -0.7813 27 1 21 3.6013 0.1011 27 1 22 -8.0544 -0.1153 27 1 23 -2.9639 0.0154 27 3 0 -4.2764 -0.0733 27 3 1 -1.6267 0.3793 27 3 2 0.9117 -0.2061 27 3 3 -4.6663 -0.1525 27 3 4 -4.6132 0.3276 27 3 5 4.5059 -0.2600 27 3 6 -4.2660 0.2764 27 3 7 -3.8742 0.3843 27 3 8 8.9610 -0.2566 27 3 9 2.5064 -0.2069 27 3 10 -4.5485 0.0529 27 3 11 6.9274 -0.0778 27 3 12 3.4006 -0.1380 27 3 13 -3.6651 0.0150 27 3 14 -2.4910 -0.3244 27 3 15 1.3995 0.1773 27 3 16 -0.4996 0.1601 27 3 17 3.1480 -0.1785 27 3 18 3.0564 -0.0225 27 3 19 -5.1133 -0.2263 27 3 20 2.3972 -0.1705 27 3 21 2.4237 0.2731 27 3 22 -0.1592 0.0187 27 5 0 -3.2183 0.1418 27 5 1 2.9783 0.1211 27 5 2 -2.4533 -0.1783 27 5 3 11.1906 -0.0921 27 5 4 11.2731 -0.1655 27 5 5 3.1568 -0.0969 27 5 6 10.2298 0.2397 27 5 7 -5.0252 0.0934 27 5 8 -1.4988 0.0728 27 5 9 1.1764 0.4109 27 5 10 2.2873 0.1881 27 5 11 4.0457 -0.1967 27 5 12 -4.2289 0.1265 27 5 13 -4.6862 0.2008 27 5 14 -1.8879 0.0921 27 5 15 -0.6248 0.2546 27 5 16 0.6396 0.2001 27 5 17 6.1231 -0.1504 27 5 18 -2.3269 -0.0093 27 5 19 2.1335 0.1392 27 7 0 -2.2009 -0.0706 27 7 1 -9.0340 -0.3832 27 7 2 -11.9526 0.0866 27 7 3 14.7465 -0.3075 27 7 4 -9.4912 0.2392 27 7 5 1.3897 0.1093 27 7 6 -3.4789 -0.2373 27 7 7 3.1666 -0.1066 27 7 8 3.3597 -0.1519 27 7 9 -1.3505 -0.4065 27 7 10 -1.7935 0.0157 27 7 11 -2.1854 0.3898 27 7 12 14.3751 -0.1356 27 7 13 7.9801 0.1325 27 7 14 -4.9862 -0.2413 27 7 15 -7.7821 -0.3575 27 9 0 -9.6941 0.4971 27 9 1 -1.1063 0.0337 27 9 2 5.0517 0.1190 27 9 3 9.7266 0.4540 27 9 4 -6.2331 -0.2179 27 9 5 -4.6975 -0.7825 27 9 6 -3.2078 -0.0605 27 9 7 0.0731 -0.2324 27 9 8 7.2465 0.4066 28 0 0 6.9458 -3.5227 28 0 2 10.0639 1.6758 28 0 4 -9.7153 -0.7874 28 0 6 -6.7781 -0.7457 28 0 8 0.0161 0.7072 28 0 10 -8.6744 0.1254 28 0 12 -1.1697 -0.6163 28 0 14 1.1452 0.0570 28 0 16 -0.0421 0.1909 28 0 18 4.0802 -0.0598 28 0 20 -0.0384 -0.8710 28 2 0 -4.5293 -0.7620 28 2 1 10.0623 -0.3970 28 2 2 -2.5735 0.2975 28 2 3 3.9274 -0.2054 28 2 4 3.7964 0.3772 28 2 5 -0.8896 -0.0814 28 2 6 -6.1436 -0.2503 28 2 7 3.6836 0.2149 28 2 8 5.9363 0.0968 28 2 9 1.9746 0.0036 28 2 10 2.8466 0.1655 28 2 11 -0.5413 0.3972 28 2 12 -1.3400 -0.2676 28 2 13 5.0910 0.0897 28 2 14 -5.5561 0.0263 28 2 15 -0.5046 -0.3542 28 2 16 4.5813 0.0306 28 2 17 -0.1553 0.0522 28 2 18 -3.2294 -0.0639 28 2 19 0.1891 0.2995 28 2 20 4.8847 0.1319 28 4 0 -5.4169 -0.0661 28 4 1 -4.0952 0.2606 28 4 2 5.0737 -0.1385 28 4 3 0.1765 -0.0924 28 4 4 -1.8700 -0.0736 28 4 5 -2.0840 -0.0201 28 4 6 -7.8259 0.4403 28 4 7 -1.7801 -0.1896 28 4 8 10.4233 -0.3800 28 4 9 10.9107 0.0164 28 4 10 -3.2672 -0.0140 28 4 11 5.8795 -0.2328 28 4 12 2.0107 -0.1484 28 4 13 -11.9096 -0.2568 28 4 14 1.4682 -0.2436 28 4 15 3.8684 0.4700 28 4 16 -6.8371 -0.2115 28 4 17 4.3646 0.0918 28 4 18 3.4226 0.1792 28 6 0 -5.4215 0.2073 28 6 1 18.3248 0.5457 28 6 2 9.7876 -0.2635 28 6 3 30.9652 0.0051 28 6 4 3.7496 0.0676 28 6 5 3.1465 -0.2393 28 6 6 2.4668 0.0226 28 6 7 -1.7738 0.4333 28 6 8 1.9719 0.4576 28 6 9 9.6305 0.4834 28 6 10 -1.1449 -0.0578 28 6 11 -9.2871 -0.5046 28 6 12 -8.2776 0.0684 28 6 13 -5.2469 0.0366 28 6 14 -10.7142 -0.0396 28 6 15 3.7531 0.5895 28 8 0 -1.1764 -0.2745 28 8 1 -12.7426 -0.6274 28 8 2 9.1238 0.2726 28 8 3 9.7578 -0.4333 28 8 4 -2.9391 -0.0265 28 8 5 -2.6118 0.2889 28 8 6 -1.6619 -0.2781 28 8 7 2.9883 -0.2469 28 8 8 1.9794 -0.5084 29 1 0 3.2442 -0.3553 29 1 1 10.4723 -1.2406 29 1 2 0.2943 0.8319 29 1 3 -4.7613 0.3630 29 1 4 -3.3095 -0.6558 29 1 5 -0.6225 -0.1115 29 1 6 0.1925 -0.4462 29 1 7 -4.6206 -0.0442 29 1 8 1.2529 0.6445 29 1 9 -6.2587 -0.0660 29 1 10 -7.2307 -0.0995 29 1 11 1.1301 0.1849 29 1 12 -1.7738 -0.2731 29 1 13 4.5765 -0.0602 29 1 14 2.1767 0.6012 29 1 15 2.8791 0.0454 29 1 16 6.2106 -0.0682 29 1 17 -2.5863 0.0436 29 1 18 -0.3561 -0.1620 29 3 0 2.4872 -0.2991 29 3 1 1.7196 0.0988 29 3 2 5.4256 0.0308 29 3 3 -2.1315 -0.4900 29 3 4 1.1034 -0.1416 29 3 5 -4.7826 0.2253 29 3 6 -2.8524 0.1192 29 3 7 5.5374 0.2182 29 3 8 -2.7323 0.1317 29 3 9 -5.0729 -0.1875 29 3 10 5.6493 0.2469 29 3 11 -0.1937 0.4893 29 3 12 -0.2186 -0.0020 29 3 13 1.7141 0.2168 29 3 14 -3.7802 0.0118 29 3 15 1.9843 -0.2306 29 3 16 1.8429 0.0332 29 3 17 0.4173 0.3381 29 5 0 5.2176 0.2672 29 5 1 -13.7455 0.0693 29 5 2 3.5813 -0.0120 29 5 3 -17.4275 0.1272 29 5 4 -25.1055 -0.0582 29 5 5 4.5292 -0.1765 29 5 6 -6.8294 -0.2613 29 5 7 -1.9260 -0.6726 29 5 8 12.7353 -0.3782 29 5 9 1.9106 0.3303 29 5 10 -8.3744 -0.0195 29 5 11 3.1276 0.0730 29 5 12 -0.6370 0.2528 29 5 13 -3.3810 -0.4695 29 5 14 2.4984 -0.4165 29 7 0 2.1284 0.3259 29 7 1 -11.8239 0.7119 29 7 2 31.3707 -0.3640 29 7 3 -2.2710 0.2058 29 7 4 6.5240 0.2084 29 7 5 -1.2969 -0.0392 29 7 6 -1.3911 0.3076 29 7 7 -4.2821 0.5176 29 7 8 0.9168 0.3849 29 7 9 2.9308 0.4937 30 0 0 -11.2917 2.2204 30 0 2 -3.0546 0.9086 30 0 4 16.7542 -1.8032 30 0 6 0.3172 0.6773 30 0 8 -2.9360 0.4473 30 0 10 8.1356 -0.7950 30 0 12 -7.8800 0.1308 30 0 14 5.3586 0.9955 30 0 16 3.3152 -0.6616 30 2 0 16.5056 -0.0964 30 2 1 -11.7002 0.1871 30 2 2 8.4189 0.2007 30 2 3 1.9466 -0.0740 30 2 4 -2.1420 0.4576 30 2 5 -4.3936 -0.3875 30 2 6 -0.3788 -0.6111 30 2 7 -4.4279 -0.0550 30 2 8 -1.2606 0.2462 30 2 9 -2.8534 0.1762 30 2 10 -2.3791 0.2670 30 2 11 0.7304 -0.1341 30 2 12 3.7731 -0.5089 30 2 13 -0.8317 -0.0296 30 2 14 -1.0449 -0.0771 30 2 15 6.4925 0.2981 30 4 0 6.6522 -0.0622 30 4 1 10.9948 -0.3886 30 4 2 -0.6574 0.3047 30 4 3 -17.4383 -0.1275 30 4 4 -0.5492 -0.3327 30 4 5 6.1948 0.4004 30 4 6 3.5943 -0.0067 30 4 7 -2.6894 0.3589 30 4 8 -3.3835 0.4107 30 4 9 -12.8249 -0.4578 30 4 10 1.0229 0.2976 30 4 11 8.5316 0.5013 30 4 12 0.4133 0.1843 30 4 13 5.8342 0.3078 30 6 0 -1.8627 -0.1396 30 6 1 -73.8001 -0.2533 30 6 2 -3.6902 0.0481 30 6 3 -14.3097 -0.0870 30 6 4 -10.0720 -0.2379 30 6 5 5.0856 -0.5466 30 6 6 -2.3082 -0.3381 30 6 7 -9.8005 -0.2618 30 6 8 3.2905 -0.3871 31 1 0 -4.9395 1.9441 31 1 1 -10.8362 0.7602 31 1 2 5.5651 0.3217 31 1 3 6.4705 -0.8096 31 1 4 4.7762 -0.2295 31 1 5 1.7510 -0.6910 31 1 6 -5.8105 -0.2450 31 1 7 0.3799 0.3304 31 1 8 6.4200 -0.6300 31 1 9 0.2344 0.4017 31 1 10 2.9181 0.3399 31 1 11 1.5473 -0.2048 31 1 12 -3.3511 0.0619 31 1 13 -6.4214 -0.0921 31 3 0 -1.8883 0.0191 31 3 1 2.5035 0.1393 31 3 2 -0.6476 0.4853 31 3 3 0.8064 -0.0702 31 3 4 8.3511 -0.0683 31 3 5 -3.7305 -0.1555 31 3 6 -2.9074 -0.5908 31 3 7 4.2195 -0.3090 31 3 8 0.1915 0.2536 31 3 9 -1.0267 -0.0042 31 3 10 -2.8021 0.3992 31 3 11 -2.6218 -0.4111 31 5 0 -8.6649 -0.3758 31 5 1 23.7311 -0.0543 31 5 2 11.2134 -0.0160 31 5 3 2.3224 -0.2562 31 5 4 16.2352 0.4172 31 5 5 0.0322 0.6128 31 5 6 -2.4104 0.2489 31 5 7 -1.3912 0.7900 32 0 0 3.4790 2.5206 32 0 2 -2.5648 -0.0558 32 0 4 -8.5500 -0.1865 32 0 6 -4.4585 0.1423 32 0 8 12.2073 -0.7305 32 2 0 -41.0959 -0.1250 32 2 1 1.7483 0.2017 32 2 2 10.5899 -0.6557 32 2 3 0.9131 0.1725 32 2 4 2.3079 0.0172 32 2 5 4.5019 -0.0787 32 2 6 -4.6197 -0.0302 32 2 7 5.7664 -0.5019 32 2 8 1.9094 -0.2878 32 4 0 -10.3706 -0.2740 32 4 1 2.2174 0.4646 32 4 3 14.6202 -0.0378 32 4 4 4.5003 0.1620 32 4 5 -2.0485 -0.5959 33 1 0 -13.3488 -0.5017 33 1 1 2.3211 1.6619 33 1 2 6.2673 -0.9929 33 1 3 -3.7541 0.1750 33 1 4 -5.3721 0.6908 33 3 0 -27.9316 -0.6271 33 3 1 -4.2880 -0.3737 33 3 2 13.1017 -0.3580 0 0 0 0.0 0.0 ; _shelx_fab_checksum 6077 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy -0.11429(2) 1.54112(2) 0.40284(2) 0.04310(10) Uani 1 1 d . . . . . Ni1 Ni -0.00501(3) 1.61892(5) 0.37763(2) 0.04193(17) Uani 1 1 d . . . . . Fe1 Fe 0.08645(3) 1.74340(5) 0.49294(2) 0.03784(18) Uani 1 1 d . . . . . Fe2 Fe 0.000000 1.58873(11) 0.250000 0.0694(4) Uani 1 2 d DS T P . . C1 C -0.1136(3) 1.9730(5) 0.4003(2) 0.070(2) Uani 1 1 d . . . . . H1 H -0.123311 2.040991 0.404384 0.085 Uiso 1 1 calc R U . . . C2 C 0.1068(2) 1.5890(5) 0.37255(19) 0.0595(16) Uani 1 1 d . . . . . H2A H 0.134728 1.553887 0.387957 0.071 Uiso 1 1 calc R U . . . H2B H 0.112878 1.581367 0.348577 0.071 Uiso 1 1 calc R U . . . C3 C -0.0105(3) 1.1946(4) 0.3612(2) 0.075(2) Uani 1 1 d . . . . . H3 H -0.002908 1.125442 0.357058 0.090 Uiso 1 1 calc R U . . . C4 C -0.1568(2) 1.2892(5) 0.3720(2) 0.0671(18) Uani 1 1 d . . . . . H4A H -0.159957 1.258218 0.349070 0.101 Uiso 1 1 calc R U . . . H4B H -0.187951 1.326223 0.373695 0.101 Uiso 1 1 calc R U . . . H4C H -0.151178 1.235609 0.389709 0.101 Uiso 1 1 calc R U . . . C5 C -0.1477(3) 1.8928(5) 0.4010(2) 0.0695(19) Uani 1 1 d . . . . . H5 H -0.180628 1.905461 0.405649 0.083 Uiso 1 1 calc R U . . . C6 C 0.0226(2) 1.8391(5) 0.54033(16) 0.0582(16) Uani 1 1 d D . . . . H6 H 0.046729 1.827368 0.560729 0.070 Uiso 1 1 calc R U . . . C7 C 0.1092(3) 1.6985(6) 0.3813(2) 0.074(2) Uani 1 1 d . . . . . H7A H 0.143179 1.722793 0.378818 0.089 Uiso 1 1 calc R U . . . H7B H 0.107205 1.703906 0.406119 0.089 Uiso 1 1 calc R U . . . C8 C 0.0720(2) 1.7722(5) 0.36247(18) 0.0621(17) Uani 1 1 d . . . . . H8A H 0.084451 1.842575 0.367847 0.075 Uiso 1 1 calc R U . . . H8B H 0.069349 1.761513 0.337284 0.075 Uiso 1 1 calc R U . . . C9 C -0.0165(3) 1.5946(5) 0.29606(18) 0.0638(15) Uani 1 1 d . . . . . C10 C -0.0234(2) 1.8801(5) 0.53925(18) 0.0596(16) Uani 1 1 d . . . . . H10 H -0.037553 1.902612 0.558403 0.071 Uiso 1 1 calc R U . . . C11 C 0.0266(3) 1.2668(5) 0.36378(19) 0.0638(18) Uani 1 1 d . . . . . H11 H 0.059215 1.247680 0.359984 0.077 Uiso 1 1 calc R U . . . C12 C 0.0596(2) 1.4393(4) 0.37264(16) 0.0500(13) Uani 1 1 d . . . . . H12 H 0.091368 1.409734 0.371060 0.060 Uiso 1 1 calc R U . . . C13 C -0.0598(3) 1.2217(4) 0.36473(17) 0.0602(16) Uani 1 1 d . . . . . H13 H -0.086232 1.172608 0.361454 0.072 Uiso 1 1 calc R U . . . C14 C -0.0689(2) 1.3203(4) 0.37294(14) 0.0482(13) Uani 1 1 d . . . . . C15 C -0.1327(2) 1.7962(4) 0.39499(18) 0.0564(16) Uani 1 1 d . . . . . C16 C -0.0004(2) 1.8435(4) 0.37790(15) 0.0507(14) Uani 1 1 d . . . . . H16 H 0.017691 1.905047 0.376386 0.061 Uiso 1 1 calc R U . . . C17 C -0.0660(3) 1.9539(4) 0.39353(19) 0.0614(17) Uani 1 1 d . . . . . H17 H -0.043116 2.009057 0.393206 0.074 Uiso 1 1 calc R U . . . C18 C -0.0306(2) 1.3977(4) 0.37679(13) 0.0392(11) Uani 1 1 d . . . . . C19 C -0.0843(2) 1.7721(4) 0.38809(15) 0.0452(12) Uani 1 1 d . . . . . C20 C 0.0176(2) 1.3680(4) 0.37184(15) 0.0487(13) Uani 1 1 d . . . . . C21 C 0.09292(19) 1.8489(4) 0.45873(15) 0.0435(12) Uani 1 1 d . . . . . C22 C 0.1369(2) 1.8131(4) 0.52681(16) 0.0468(13) Uani 1 1 d . . . . . C23 C -0.01337(19) 1.8452(4) 0.48728(15) 0.0443(12) Uani 1 1 d D . . . . H23 H -0.019934 1.839189 0.462806 0.053 Uiso 1 1 calc R U . . . C24 C -0.0506(2) 1.8541(4) 0.38712(16) 0.0496(13) Uani 1 1 d . . . . . C25 C -0.2078(2) 1.4346(5) 0.43659(18) 0.0611(17) Uani 1 1 d . . . . . H25 H -0.186341 1.417865 0.457754 0.073 Uiso 1 1 calc R U . . . C26 C 0.04213(19) 1.6734(4) 0.45571(14) 0.0400(11) Uani 1 1 d . . . . . C27 C 0.08400(18) 1.6410(4) 0.52848(15) 0.0417(12) Uani 1 1 d . . . . . C29 C 0.1394(2) 1.6633(4) 0.47908(15) 0.0465(13) Uani 1 1 d . . . . . C30 C 0.0429(7) 1.3816(11) 0.2309(3) 0.118(6) Uani 0.5 1 d D . P A -1 H30 H 0.028382 1.387046 0.207085 0.141 Uiso 0.5 1 calc R U P A -1 C31 C 0.0663(5) 1.6499(12) 0.2675(3) 0.069(3) Uani 0.5 1 d D . P B -1 C32 C -0.0973(2) 1.9179(5) 0.4919(2) 0.0658(19) Uani 1 1 d . . . . . H32A H -0.112985 1.942300 0.511041 0.099 Uiso 1 1 calc R U . . . H32B H -0.096283 1.973532 0.475390 0.099 Uiso 1 1 calc R U . . . H32C H -0.117163 1.861060 0.480255 0.099 Uiso 1 1 calc R U . . . C33 C -0.2712(3) 1.3281(7) 0.4551(3) 0.099(3) Uani 1 1 d . . . . . H33A H -0.306506 1.311097 0.445991 0.149 Uiso 1 1 calc R U . . . H33B H -0.250781 1.265617 0.457104 0.149 Uiso 1 1 calc R U . . . H33C H -0.268590 1.359890 0.477862 0.149 Uiso 1 1 calc R U . . . C34 C -0.2866(3) 1.4182(7) 0.3983(3) 0.098(3) Uani 1 1 d . . . . . H34A H -0.319426 1.386005 0.398456 0.147 Uiso 1 1 calc R U . . . H34B H -0.291169 1.491988 0.394999 0.147 Uiso 1 1 calc R U . . . H34C H -0.271631 1.389666 0.379466 0.147 Uiso 1 1 calc R U . . . C35 C -0.2147(3) 1.7243(6) 0.3978(3) 0.105(4) Uani 1 1 d . . . . . H35A H -0.231535 1.657836 0.397474 0.158 Uiso 1 1 calc R U . . . H35B H -0.216486 1.759278 0.419626 0.158 Uiso 1 1 calc R U . . . H35C H -0.231571 1.765816 0.378418 0.158 Uiso 1 1 calc R U . . . C36 C -0.0752(4) 1.6221(7) 0.4825(3) 0.044(2) Uani 0.58 1 d . . P C 1 H36 H -0.039922 1.609758 0.485365 0.053 Uiso 0.58 1 calc R U P C 1 C37 C -0.1504(5) 1.6453(10) 0.5065(4) 0.079(4) Uani 0.58 1 d . . P C 1 H37A H -0.160944 1.646211 0.529083 0.119 Uiso 0.58 1 calc R U P C 1 H37B H -0.157964 1.711470 0.495098 0.119 Uiso 0.58 1 calc R U P C 1 H37C H -0.168631 1.591296 0.492148 0.119 Uiso 0.58 1 calc R U P C 1 C38 C -0.0669(5) 1.6102(10) 0.5447(3) 0.071(3) Uani 0.58 1 d . . P C 1 H38A H -0.088491 1.615793 0.562264 0.106 Uiso 0.58 1 calc R U P C 1 H38B H -0.051678 1.542122 0.545829 0.106 Uiso 0.58 1 calc R U P C 1 H38C H -0.040259 1.661981 0.549110 0.106 Uiso 0.58 1 calc R U P C 1 C36A C -0.1219(6) 1.6357(10) 0.4809(4) 0.051(3) Uani 0.42 1 d . . P C 2 H36A H -0.157460 1.644474 0.477602 0.061 Uiso 0.42 1 calc R U P C 2 C37A C -0.1273(6) 1.6335(14) 0.5416(4) 0.066(4) Uani 0.42 1 d . . P C 2 H37D H -0.104211 1.625062 0.563711 0.099 Uiso 0.42 1 calc R U P C 2 H37E H -0.143728 1.700415 0.541015 0.099 Uiso 0.42 1 calc R U P C 2 H37F H -0.152986 1.579692 0.539035 0.099 Uiso 0.42 1 calc R U P C 2 C38A C -0.0443(5) 1.6062(11) 0.5221(5) 0.059(4) Uani 0.42 1 d . . P C 2 H38D H -0.036577 1.603226 0.547445 0.089 Uiso 0.42 1 calc R U P C 2 H38E H -0.035689 1.540823 0.512566 0.089 Uiso 0.42 1 calc R U P C 2 H38F H -0.024572 1.660930 0.513968 0.089 Uiso 0.42 1 calc R U P C 2 C40 C 0.0947(9) 1.2299(16) 0.2273(5) 0.143(7) Uani 0.5 1 d D U P A -1 H40A H 0.112922 1.180417 0.243655 0.215 Uiso 0.5 1 calc R U P A -1 H40B H 0.069114 1.194210 0.210611 0.215 Uiso 0.5 1 calc R U P A -1 H40C H 0.118555 1.264269 0.214987 0.215 Uiso 0.5 1 calc R U P A -1 C41 C -0.0250(7) 1.7227(11) 0.2395(4) 0.088(4) Uani 0.5 1 d D . P B -1 C42 C 0.0652(9) 1.4147(13) 0.2847(3) 0.126(8) Uani 0.5 1 d D U P A -1 H42 H 0.069930 1.448495 0.306419 0.151 Uiso 0.5 1 calc R U P A -1 C43 C 0.0856(9) 1.3215(13) 0.2795(4) 0.121(6) Uani 0.5 1 d D U P A -1 H43 H 0.105324 1.279640 0.296527 0.146 Uiso 0.5 1 calc R U P A -1 C47 C -0.0573(7) 1.5230(16) 0.2252(4) 0.096(4) Uani 0.5 1 d D . P B -1 N1 N 0.01795(16) 1.6371(3) 0.43134(12) 0.0421(10) Uani 1 1 d . . . . . N2 N 0.16742(18) 1.8548(4) 0.54623(14) 0.0548(12) Uani 1 1 d . . . . . N3 N 0.09596(19) 1.9122(4) 0.43925(13) 0.0541(12) Uani 1 1 d . . . . . N4 N 0.17053(18) 1.6121(4) 0.47066(14) 0.0546(12) Uani 1 1 d . . . . . N5 N 0.08599(17) 1.5823(3) 0.55069(12) 0.0466(11) Uani 1 1 d . . . . . N6 N 0.02922(15) 1.8168(3) 0.50709(12) 0.0407(10) Uani 1 1 d . . . . . N7 N -0.04573(16) 1.8830(3) 0.50541(13) 0.0476(11) Uani 1 1 d . . . . . N8 N 0.02161(17) 1.7614(3) 0.37169(12) 0.0442(10) Uani 1 1 d . . . . . N9 N 0.05878(17) 1.5359(4) 0.37520(12) 0.0470(11) Uani 1 1 d . . . . . N10 N -0.0240(2) 1.6014(4) 0.32382(14) 0.0582(12) Uani 1 1 d . . . . . N11 N -0.09674(19) 1.6261(4) 0.51115(14) 0.0526(12) Uani 1 1 d . . . . . N13 N 0.1062(5) 1.6843(12) 0.2798(3) 0.090(4) Uani 0.5 1 d D . P B -1 N14 N 0.0373(5) 1.4537(8) 0.2550(3) 0.083(3) Uani 0.5 1 d D . P A -1 N15 N -0.25278(18) 1.3985(4) 0.43167(17) 0.0679(16) Uani 1 1 d . . . . . N16 N -0.0444(9) 1.7986(13) 0.2326(5) 0.138(7) Uani 0.5 1 d D U P B -1 N17 N 0.0718(7) 1.3006(13) 0.2449(4) 0.145(7) Uani 0.5 1 d D . P A -1 N19 N -0.0953(7) 1.487(2) 0.2110(5) 0.144(7) Uani 0.5 1 d D U P B -1 O1 O -0.07394(13) 1.6761(3) 0.38271(10) 0.0433(8) Uani 1 1 d . . . . . O2 O -0.04324(13) 1.4892(3) 0.38496(10) 0.0432(8) Uani 1 1 d . . . . . O3 O -0.11503(14) 1.3588(3) 0.37739(11) 0.0525(10) Uani 1 1 d . . . . . O4 O -0.16255(14) 1.7095(3) 0.39492(13) 0.0593(12) Uani 1 1 d . . . . . O5 O -0.18999(14) 1.4896(3) 0.41600(12) 0.0576(11) Uani 1 1 d . . . . . O6 O -0.09872(17) 1.6335(3) 0.45375(12) 0.0562(10) Uani 1 1 d . . . . . O7 O -0.16302(18) 1.5409(4) 0.34823(14) 0.0725(13) Uani 1 1 d D . . . . N21 N -0.1904(6) 1.5329(15) 0.2913(3) 0.119(6) Uani 0.5 1 d D . P D -1 C52 C -0.1538(6) 1.5447(15) 0.3185(3) 0.104(5) Uani 0.5 1 d D . P D -1 H52 H -0.120192 1.556270 0.315122 0.124 Uiso 0.5 1 calc R U P D -1 C53 C -0.1783(9) 1.521(2) 0.2583(4) 0.153(7) Uani 0.5 1 d D U P D -1 H53A H -0.209360 1.513154 0.241199 0.230 Uiso 0.5 1 calc R U P D -1 H53B H -0.159812 1.581238 0.252621 0.230 Uiso 0.5 1 calc R U P D -1 H53C H -0.157160 1.460116 0.258019 0.230 Uiso 0.5 1 calc R U P D -1 C54 C -0.2413(6) 1.531(3) 0.2934(6) 0.171(9) Uani 0.5 1 d D U P D -1 H54A H -0.261485 1.521415 0.270266 0.257 Uiso 0.5 1 calc R U P D -1 H54B H -0.247773 1.474366 0.308363 0.257 Uiso 0.5 1 calc R U P D -1 H54C H -0.250693 1.595534 0.303125 0.257 Uiso 0.5 1 calc R U P D -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 0.03376(15) 0.03766(15) 0.05959(18) 0.01354(11) 0.01297(11) -0.00567(10) Ni1 0.0395(4) 0.0380(3) 0.0517(4) 0.0063(3) 0.0175(3) -0.0087(3) Fe1 0.0307(4) 0.0320(3) 0.0532(4) 0.0081(3) 0.0141(3) -0.0008(3) Fe2 0.0937(11) 0.0575(8) 0.0545(8) 0.000 0.0064(7) 0.000 C1 0.066(5) 0.034(3) 0.114(6) 0.009(3) 0.022(4) -0.001(3) C2 0.049(3) 0.054(4) 0.082(4) -0.006(3) 0.030(3) -0.011(3) C3 0.100(6) 0.024(3) 0.112(6) -0.007(3) 0.051(5) -0.002(3) C4 0.051(4) 0.059(4) 0.090(5) 0.000(3) 0.010(3) -0.020(3) C5 0.053(4) 0.059(4) 0.102(6) 0.014(4) 0.026(4) 0.007(3) C6 0.046(3) 0.076(4) 0.053(3) 0.000(3) 0.009(3) 0.015(3) C7 0.053(4) 0.072(5) 0.104(6) -0.002(4) 0.034(4) -0.022(4) C8 0.064(4) 0.061(4) 0.069(4) 0.004(3) 0.033(3) -0.018(3) C9 0.075(4) 0.054(3) 0.060(2) 0.007(2) 0.005(3) -0.022(3) C10 0.044(3) 0.066(4) 0.071(4) -0.008(3) 0.018(3) 0.013(3) C11 0.067(4) 0.040(3) 0.093(5) -0.005(3) 0.037(4) -0.003(3) C12 0.052(3) 0.040(3) 0.063(4) -0.004(2) 0.024(3) -0.001(2) C13 0.079(5) 0.035(3) 0.070(4) -0.002(3) 0.024(3) -0.010(3) C14 0.059(3) 0.040(3) 0.047(3) 0.000(2) 0.013(3) -0.008(3) C15 0.046(3) 0.041(3) 0.084(4) 0.024(3) 0.015(3) -0.001(3) C16 0.054(3) 0.040(3) 0.059(3) 0.008(2) 0.015(3) -0.019(3) C17 0.065(4) 0.031(3) 0.093(5) 0.014(3) 0.025(4) -0.002(3) C18 0.047(3) 0.028(2) 0.044(3) 0.0024(19) 0.014(2) -0.004(2) C19 0.043(3) 0.036(3) 0.057(3) 0.012(2) 0.010(2) -0.006(2) C20 0.058(3) 0.033(3) 0.059(3) 0.003(2) 0.020(3) 0.007(2) C21 0.032(3) 0.040(3) 0.063(3) 0.004(2) 0.018(2) 0.005(2) C22 0.039(3) 0.041(3) 0.064(4) 0.010(2) 0.020(3) 0.004(2) C23 0.035(3) 0.041(3) 0.056(3) 0.008(2) 0.005(2) 0.003(2) C24 0.048(3) 0.037(3) 0.066(4) 0.014(2) 0.015(3) -0.006(2) C25 0.034(3) 0.071(4) 0.078(4) 0.023(3) 0.009(3) -0.018(3) C26 0.032(2) 0.037(3) 0.056(3) 0.015(2) 0.023(2) 0.002(2) C27 0.026(2) 0.034(2) 0.068(3) 0.000(2) 0.014(2) -0.0004(19) C29 0.041(3) 0.044(3) 0.057(3) 0.013(2) 0.017(2) -0.005(2) C30 0.166(16) 0.099(8) 0.090(6) -0.010(5) 0.028(7) 0.013(9) C31 0.099(5) 0.074(6) 0.042(6) -0.008(5) 0.031(4) -0.008(5) C32 0.039(3) 0.046(3) 0.110(6) -0.014(3) 0.006(3) 0.007(3) C33 0.047(4) 0.107(7) 0.149(8) 0.078(6) 0.032(5) -0.006(4) C34 0.056(4) 0.100(7) 0.131(8) 0.038(6) -0.004(5) -0.021(4) C35 0.042(4) 0.056(4) 0.222(11) 0.045(6) 0.035(5) 0.011(3) C36 0.041(5) 0.035(4) 0.059(6) 0.011(4) 0.017(4) -0.005(4) C37 0.073(8) 0.070(8) 0.109(11) -0.002(7) 0.054(8) -0.008(7) C38 0.082(9) 0.057(7) 0.075(8) 0.000(6) 0.021(7) -0.003(6) C36A 0.053(8) 0.041(7) 0.061(9) -0.002(6) 0.017(7) -0.007(6) C37A 0.057(9) 0.077(11) 0.063(10) -0.007(8) 0.008(8) -0.003(8) C38A 0.047(8) 0.037(7) 0.094(12) 0.002(7) 0.014(8) 0.000(6) C40 0.166(11) 0.130(9) 0.131(9) -0.025(7) 0.018(8) 0.029(8) C41 0.120(9) 0.096(6) 0.057(8) 0.018(5) 0.041(7) 0.023(6) C42 0.205(17) 0.085(8) 0.083(6) 0.013(5) 0.014(8) 0.036(11) C43 0.181(16) 0.075(8) 0.111(7) 0.010(6) 0.032(9) 0.016(9) C47 0.111(7) 0.133(10) 0.046(5) 0.007(6) 0.019(5) -0.031(6) N1 0.039(2) 0.038(2) 0.053(3) 0.0073(19) 0.017(2) -0.0016(19) N2 0.040(3) 0.047(3) 0.077(3) -0.002(2) 0.008(2) -0.009(2) N3 0.053(3) 0.049(3) 0.065(3) 0.018(2) 0.024(2) 0.000(2) N4 0.042(3) 0.049(3) 0.077(3) 0.010(2) 0.022(2) 0.007(2) N5 0.043(3) 0.038(2) 0.059(3) 0.016(2) 0.013(2) 0.0017(19) N6 0.033(2) 0.031(2) 0.060(3) 0.0038(18) 0.0120(19) -0.0011(17) N7 0.034(2) 0.038(2) 0.073(3) -0.004(2) 0.013(2) -0.0008(18) N8 0.047(3) 0.033(2) 0.057(3) 0.0081(19) 0.020(2) -0.0117(19) N9 0.041(2) 0.050(3) 0.054(3) -0.003(2) 0.020(2) -0.013(2) N10 0.060(3) 0.053(3) 0.058(2) 0.010(2) 0.002(2) -0.019(2) N11 0.051(3) 0.046(3) 0.062(3) 0.000(2) 0.015(2) -0.010(2) N13 0.102(6) 0.120(11) 0.057(6) -0.027(7) 0.038(5) -0.022(6) N14 0.123(8) 0.068(4) 0.065(6) 0.011(4) 0.031(5) -0.014(4) N15 0.033(3) 0.068(4) 0.106(5) 0.031(3) 0.022(3) -0.006(2) N16 0.203(14) 0.120(8) 0.101(10) 0.030(7) 0.050(10) 0.066(9) N17 0.209(17) 0.108(8) 0.117(7) -0.008(6) 0.027(9) 0.037(10) N19 0.135(9) 0.197(15) 0.092(10) 0.006(11) 0.002(7) -0.064(10) O1 0.0395(19) 0.0307(17) 0.062(2) 0.0157(16) 0.0165(17) -0.0059(15) O2 0.0394(19) 0.0339(18) 0.060(2) 0.0016(16) 0.0192(17) -0.0088(15) O3 0.043(2) 0.037(2) 0.078(3) 0.0021(18) 0.0127(19) -0.0150(17) O4 0.034(2) 0.043(2) 0.102(3) 0.026(2) 0.016(2) 0.0025(17) O5 0.035(2) 0.056(2) 0.085(3) 0.020(2) 0.020(2) -0.0080(18) O6 0.064(3) 0.039(2) 0.068(3) 0.0037(18) 0.018(2) -0.0035(19) O7 0.056(3) 0.058(3) 0.096(3) 0.015(3) -0.008(3) -0.007(2) N21 0.103(7) 0.150(16) 0.098(4) 0.004(7) 0.000(5) -0.026(8) C52 0.103(8) 0.105(14) 0.099(4) 0.007(5) 0.005(4) -0.027(9) C53 0.173(10) 0.179(12) 0.107(5) -0.009(7) 0.019(6) -0.016(9) C54 0.103(7) 0.23(2) 0.172(13) 0.035(14) 0.009(7) -0.023(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Fe Fe 0.3463 0.8444 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Dy1 O3 70.14(15) 5_586 . y N5 Dy1 O4 138.00(16) 5_586 . y O1 Dy1 N5 131.48(14) . 5_586 y O1 Dy1 O3 123.38(13) . . y O1 Dy1 O4 63.45(12) . . y O1 Dy1 O5 143.28(14) . . y O1 Dy1 O6 82.64(14) . . y O1 Dy1 O7 84.56(15) . . y O2 Dy1 N5 82.33(14) . 5_586 y O2 Dy1 O1 69.13(13) . . y O2 Dy1 O3 63.26(12) . . y O2 Dy1 O4 131.60(13) . . y O2 Dy1 O5 144.98(15) . . y O2 Dy1 O6 113.27(15) . . y O2 Dy1 O7 94.70(17) . . y O4 Dy1 O3 141.48(14) . . y O5 Dy1 N5 78.93(15) . 5_586 y O5 Dy1 O3 82.55(15) . . y O5 Dy1 O4 80.09(14) . . y O5 Dy1 O6 89.35(16) . . y O5 Dy1 O7 80.19(18) . . y O6 Dy1 N5 73.52(16) . 5_586 y O6 Dy1 O3 143.63(14) . . y O6 Dy1 O4 70.27(16) . . y O7 Dy1 N5 137.75(16) . 5_586 y O7 Dy1 O3 71.04(15) . . y O7 Dy1 O4 72.27(17) . . y O7 Dy1 O6 142.30(17) . . y N8 Ni1 N1 88.00(18) . . y N8 Ni1 N9 99.56(18) . . y N8 Ni1 N10 90.66(19) . . y N8 Ni1 O1 91.14(16) . . y N8 Ni1 O2 169.63(17) . . y N9 Ni1 N1 90.54(18) . . y N9 Ni1 N10 87.1(2) . . y N10 Ni1 N1 177.06(19) . . y O1 Ni1 N1 88.20(16) . . y O1 Ni1 N9 169.18(16) . . y O1 Ni1 N10 94.4(2) . . y O2 Ni1 N1 90.99(16) . . y O2 Ni1 N9 90.77(16) . . y O2 Ni1 N10 90.79(17) . . y O2 Ni1 O1 78.51(14) . . y C21 Fe1 N6 91.18(19) . . y C22 Fe1 C21 90.1(2) . . y C22 Fe1 N6 93.6(2) . . y C26 Fe1 C21 86.2(2) . . y C26 Fe1 C22 173.3(2) . . y C26 Fe1 C27 96.9(2) . . y C26 Fe1 N6 92.1(2) . . y C27 Fe1 C21 176.5(2) . . y C27 Fe1 C22 86.6(2) . . y C27 Fe1 N6 90.25(19) . . y C29 Fe1 C21 91.6(2) . . y C29 Fe1 C22 89.3(2) . . y C29 Fe1 C26 85.1(2) . . y C29 Fe1 C27 87.1(2) . . y C29 Fe1 N6 175.9(2) . . y C9 Fe2 C9 175.4(4) 2 . y C9 Fe2 C31 90.1(4) 2 2 y C9 Fe2 C31 88.0(4) . 2 y C9 Fe2 C31 90.1(4) . . y C9 Fe2 C31 88.0(4) 2 . y C9 Fe2 N14 97.8(4) . . y C9 Fe2 N14 86.2(4) . 2 y C9 Fe2 N14 86.2(4) 2 . y C9 Fe2 N14 97.8(4) 2 2 y C31 Fe2 C31 131.9(10) . 2 y C31 Fe2 N14 85.3(6) . . y C31 Fe2 N14 85.3(6) 2 2 y C31 Fe2 N14 142.5(6) 2 . y C31 Fe2 N14 142.5(6) . 2 y C41 Fe2 C9 83.8(5) . 2 y C41 Fe2 C9 92.0(5) 2 2 y C41 Fe2 C9 83.8(5) 2 . y C41 Fe2 C9 92.0(5) . . y C41 Fe2 C31 87.9(8) 2 2 y C41 Fe2 C31 87.9(8) . . y C41 Fe2 C31 44.2(7) . 2 y C41 Fe2 C31 44.2(7) 2 . y C41 Fe2 C41 44.8(12) 2 . y C41 Fe2 N14 129.5(7) . 2 y C41 Fe2 N14 168.1(6) 2 2 y C41 Fe2 N14 129.5(7) 2 . y C41 Fe2 N14 168.1(6) . . y C47 Fe2 C9 101.4(5) 2 2 y C47 Fe2 C9 101.4(5) . . y C47 Fe2 C9 80.7(5) 2 . y C47 Fe2 C9 80.7(5) . 2 y C47 Fe2 C31 52.8(8) 2 . y C47 Fe2 C31 168.0(7) . . y C47 Fe2 C31 52.8(8) . 2 y C47 Fe2 C31 168.0(7) 2 2 y C47 Fe2 C41 139.7(9) . 2 y C47 Fe2 C41 139.7(9) 2 . y C47 Fe2 C41 94.9(9) 2 2 y C47 Fe2 C41 94.9(9) . . y C47 Fe2 C47 125.5(14) . 2 y C47 Fe2 N14 89.9(8) . . y C47 Fe2 N14 37.1(7) 2 . y C47 Fe2 N14 89.9(8) 2 2 y C47 Fe2 N14 37.1(7) . 2 y N14 Fe2 N14 58.4(8) 2 . y C5 C1 H1 119.8 . . ? C17 C1 H1 119.8 . . ? C17 C1 C5 120.4(6) . . ? H2A C2 H2B 107.4 . . ? C7 C2 H2A 108.3 . . ? C7 C2 H2B 108.3 . . ? C7 C2 N9 116.1(5) . . ? N9 C2 H2A 108.3 . . ? N9 C2 H2B 108.3 . . ? C11 C3 H3 119.7 . . ? C11 C3 C13 120.7(6) . . ? C13 C3 H3 119.7 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? O3 C4 H4C 109.5 . . ? C1 C5 H5 120.8 . . ? C15 C5 C1 118.4(6) . . ? C15 C5 H5 120.8 . . ? C10 C6 H6 125.4 . . ? C10 C6 N6 109.3(5) . . ? N6 C6 H6 125.4 . . ? C2 C7 H7A 107.0 . . ? C2 C7 H7B 107.0 . . ? C2 C7 C8 121.2(7) . . ? H7A C7 H7B 106.8 . . ? C8 C7 H7A 107.0 . . ? C8 C7 H7B 107.0 . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N8 C8 C7 112.5(5) . . ? N8 C8 H8A 109.1 . . ? N8 C8 H8B 109.1 . . ? N10 C9 Fe2 176.3(6) . . ? C6 C10 H10 126.7 . . ? C6 C10 N7 106.6(6) . . ? N7 C10 H10 126.7 . . ? C3 C11 H11 119.4 . . ? C3 C11 C20 121.2(6) . . ? C20 C11 H11 119.4 . . ? C20 C12 H12 116.1 . . ? N9 C12 H12 116.1 . . ? N9 C12 C20 127.7(5) . . ? C3 C13 H13 120.8 . . ? C14 C13 C3 118.3(6) . . ? C14 C13 H13 120.8 . . ? C13 C14 C18 122.7(6) . . ? C13 C14 O3 125.4(5) . . ? O3 C14 C18 111.9(5) . . ? C5 C15 C19 123.7(6) . . ? C5 C15 O4 124.6(6) . . ? O4 C15 C19 111.7(5) . . ? C24 C16 H16 116.2 . . ? N8 C16 H16 116.2 . . ? N8 C16 C24 127.6(5) . . ? C1 C17 H17 119.5 . . ? C1 C17 C24 121.1(6) . . ? C24 C17 H17 119.5 . . ? C20 C18 C14 117.0(5) . . ? O2 C18 C14 117.6(5) . . ? O2 C18 C20 125.3(5) . . ? C24 C19 C15 117.0(5) . . ? O1 C19 C15 118.4(5) . . ? O1 C19 C24 124.6(5) . . ? C11 C20 C12 116.4(5) . . ? C11 C20 C18 119.9(6) . . ? C18 C20 C12 123.6(5) . . ? N3 C21 Fe1 178.1(5) . . ? N2 C22 Fe1 178.3(5) . . ? N6 C23 H23 124.0 . . ? N7 C23 H23 124.0 . . ? N7 C23 N6 112.1(5) . . ? C17 C24 C16 116.4(5) . . ? C17 C24 C19 119.4(6) . . ? C19 C24 C16 124.1(5) . . ? N15 C25 H25 117.2 . . ? O5 C25 H25 117.2 . . ? O5 C25 N15 125.5(6) . . ? N1 C26 Fe1 173.4(4) . . ? N5 C27 Fe1 175.1(5) . . ? N4 C29 Fe1 177.9(5) . . ? N14 C30 H30 123.8 . . ? N14 C30 N17 112.4(12) . . ? N17 C30 H30 123.8 . . ? N13 C31 Fe2 176.3(13) . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C32 H32A 109.5 . . ? N7 C32 H32B 109.5 . . ? N7 C32 H32C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N15 C33 H33A 109.5 . . ? N15 C33 H33B 109.5 . . ? N15 C33 H33C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N15 C34 H34A 109.5 . . ? N15 C34 H34B 109.5 . . ? N15 C34 H34C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O4 C35 H35A 109.5 . . ? O4 C35 H35B 109.5 . . ? O4 C35 H35C 109.5 . . ? N11 C36 H36 118.5 . . ? O6 C36 H36 118.5 . . ? O6 C36 N11 123.0(8) . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N11 C37 H37A 109.5 . . ? N11 C37 H37B 109.5 . . ? N11 C37 H37C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N11 C38 H38A 109.5 . . ? N11 C38 H38B 109.5 . . ? N11 C38 H38C 109.5 . . ? N11 C36A H36A 119.9 . . ? N11 C36A O6 120.2(12) . . ? O6 C36A H36A 119.9 . . ? H37D C37A H37E 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? N11 C37A H37D 109.5 . . ? N11 C37A H37E 109.5 . . ? N11 C37A H37F 109.5 . . ? H38D C38A H38E 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? N11 C38A H38D 109.5 . . ? N11 C38A H38E 109.5 . . ? N11 C38A H38F 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N17 C40 H40A 109.5 . . ? N17 C40 H40B 109.5 . . ? N17 C40 H40C 109.5 . . ? N16 C41 Fe2 173(2) . . ? C43 C42 H42 123.8 . . ? C43 C42 N14 112.3(12) . . ? N14 C42 H42 123.8 . . ? C42 C43 H43 126.8 . . ? C42 C43 N17 106.3(16) . . ? N17 C43 H43 126.8 . . ? N19 C47 Fe2 175(2) . . ? C26 N1 Ni1 153.6(4) . . ? C27 N5 Dy1 164.7(4) . 5_586 ? C6 N6 Fe1 127.5(4) . . ? C23 N6 Fe1 127.6(4) . . ? C23 N6 C6 104.6(5) . . ? C10 N7 C32 125.9(5) . . ? C23 N7 C10 107.5(5) . . ? C23 N7 C32 126.6(6) . . ? C8 N8 Ni1 118.5(4) . . ? C16 N8 Ni1 124.6(4) . . ? C16 N8 C8 116.6(5) . . ? C2 N9 Ni1 120.1(4) . . ? C12 N9 Ni1 124.0(4) . . ? C12 N9 C2 115.6(5) . . ? C9 N10 Ni1 156.1(5) . . ? C36 N11 C37 117.9(8) . . ? C36 N11 C38 120.5(8) . . ? C38 N11 C37 121.6(9) . . ? C36A N11 C37A 116.4(10) . . ? C36A N11 C38A 129.6(11) . . ? C38A N11 C37A 114.0(10) . . ? C30 N14 Fe2 130.5(9) . . ? C30 N14 C42 102.9(8) . . ? C42 N14 Fe2 126.6(9) . . ? C25 N15 C33 124.0(6) . . ? C25 N15 C34 119.0(6) . . ? C33 N15 C34 116.5(6) . . ? C30 N17 C43 106.0(15) . . ? C40 N17 C30 126.6(14) . . ? C40 N17 C43 124.8(14) . . ? Ni1 O1 Dy1 104.26(14) . . ? C19 O1 Dy1 123.7(3) . . ? C19 O1 Ni1 126.2(3) . . ? Ni1 O2 Dy1 105.75(16) . . ? C18 O2 Dy1 128.8(3) . . ? C18 O2 Ni1 125.0(3) . . ? C4 O3 Dy1 126.5(4) . . ? C14 O3 Dy1 116.2(3) . . ? C14 O3 C4 116.7(5) . . ? C15 O4 Dy1 115.1(3) . . ? C15 O4 C35 117.5(5) . . ? C35 O4 Dy1 126.0(4) . . ? C25 O5 Dy1 141.4(4) . . ? C36 O6 Dy1 137.1(5) . . ? C36A O6 Dy1 131.9(7) . . ? C52 O7 Dy1 134.6(8) . . ? C52 N21 C53 119.7(14) . . ? C52 N21 C54 123.5(13) . . ? C54 N21 C53 116.8(13) . . ? O7 C52 N21 120.7(13) . . ? O7 C52 H52 119.7 . . ? N21 C52 H52 119.7 . . ? N21 C53 H53A 109.5 . . ? N21 C53 H53B 109.5 . . ? N21 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N21 C54 H54A 109.5 . . ? N21 C54 H54B 109.5 . . ? N21 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N5 2.456(4) 5_586 y Dy1 O1 2.289(3) . y Dy1 O2 2.258(4) . y Dy1 O3 2.587(4) . y Dy1 O4 2.550(4) . y Dy1 O5 2.293(4) . y Dy1 O6 2.312(4) . y Dy1 O7 2.306(5) . y Ni1 N1 2.105(5) . y Ni1 N8 2.028(4) . y Ni1 N9 2.049(5) . y Ni1 N10 2.098(5) . y Ni1 O1 2.044(4) . y Ni1 O2 2.033(3) . y Fe1 C21 1.957(6) . y Fe1 C22 1.949(6) . y Fe1 C26 1.944(6) . y Fe1 C27 1.947(5) . y Fe1 C29 1.925(6) . y Fe1 N6 1.979(4) . y Fe2 C9 1.942(7) . y Fe2 C9 1.942(7) 2 y Fe2 C31 1.965(13) 2 y Fe2 C31 1.965(13) . y Fe2 C41 1.898(13) 2 y Fe2 C41 1.898(13) . y Fe2 C47 1.880(14) 2 y Fe2 C47 1.880(14) . y Fe2 N14 2.026(11) 2 y Fe2 N14 2.026(11) . y C1 H1 0.9500 . ? C1 C5 1.400(9) . ? C1 C17 1.378(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C7 1.472(9) . ? C2 N9 1.489(7) . ? C3 H3 0.9500 . ? C3 C11 1.366(9) . ? C3 C13 1.405(10) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4 O3 1.434(7) . ? C5 H5 0.9500 . ? C5 C15 1.363(9) . ? C6 H6 0.9500 . ? C6 C10 1.343(8) . ? C6 N6 1.382(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.488(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N8 1.474(7) . ? C9 N10 1.149(8) . ? C10 H10 0.9500 . ? C10 N7 1.358(8) . ? C11 H11 0.9500 . ? C11 C20 1.394(8) . ? C12 H12 0.9500 . ? C12 C20 1.464(8) . ? C12 N9 1.271(7) . ? C13 H13 0.9500 . ? C13 C14 1.363(8) . ? C14 C18 1.433(7) . ? C14 O3 1.382(7) . ? C15 C19 1.412(8) . ? C15 O4 1.391(7) . ? C16 H16 0.9500 . ? C16 C24 1.467(8) . ? C16 N8 1.273(7) . ? C17 H17 0.9500 . ? C17 C24 1.408(8) . ? C18 C20 1.402(8) . ? C18 O2 1.302(6) . ? C19 C24 1.411(7) . ? C19 O1 1.313(6) . ? C21 N3 1.142(7) . ? C22 N2 1.154(7) . ? C23 H23 0.9500 . ? C23 N6 1.319(6) . ? C23 N7 1.317(7) . ? C25 H25 0.9500 . ? C25 N15 1.280(7) . ? C25 O5 1.243(7) . ? C26 N1 1.159(7) . ? C27 N5 1.157(7) . ? C29 N4 1.168(7) . ? C30 H30 0.9500 . ? C30 N14 1.366(9) . ? C30 N17 1.371(9) . ? C31 N13 1.185(16) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32 N7 1.468(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33 N15 1.451(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34 N15 1.478(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 O4 1.443(7) . ? C36 H36 0.9500 . ? C36 N11 1.356(11) . ? C36 O6 1.203(10) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C37 N11 1.445(13) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38 N11 1.432(14) . ? C36A H36A 0.9500 . ? C36A N11 1.264(15) . ? C36A O6 1.331(14) . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? C37A N11 1.572(17) . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C38A N11 1.424(15) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C40 N17 1.368(14) . ? C41 N16 1.133(17) . ? C42 H42 0.9500 . ? C42 C43 1.368(10) . ? C42 N14 1.367(9) . ? C43 H43 0.9500 . ? C43 N17 1.374(9) . ? C47 N19 1.173(18) . ? O7 C52 1.240(9) . ? N21 C52 1.328(13) . ? N21 C53 1.401(14) . ? N21 C54 1.388(15) . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? 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 -0.013 -0.986 -0.953 4715.4 1129.0 '16 DMF,48 water'