#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:57:10 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288790 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247702.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_7247702 loop_ _publ_author_name 'Zhao, Yuming' 'Zhang, Rudie' 'Xiao, Cheng' 'Yue, Dan' 'Qin, Bowen' 'Liu, Jinhui' 'Wang, Zhenling' 'Fu, Yu' _publ_section_title ; A dual-emission Tb-based MOF induced by ESPT for ratiometric ammonia sensing ; _journal_issue 47 _journal_name_full CrystEngComm _journal_page_first 6528 _journal_page_last 6532 _journal_paper_doi 10.1039/D3CE00902E _journal_volume 25 _journal_year 2023 _chemical_formula_moiety 'C18 H20 N2 O11 Tb, C3 H7 N O' _chemical_formula_sum 'C21 H27 N3 O12 Tb' _chemical_formula_weight 672.37 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2023-05-12 _audit_creation_method ; Olex2 1.5 (compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429) ; _audit_update_record ; 2023-05-12 deposited with the CCDC. 2023-11-09 downloaded from the CCDC. ; _cell_angle_alpha 104.646(2) _cell_angle_beta 108.134(2) _cell_angle_gamma 97.016(2) _cell_formula_units_Z 2 _cell_length_a 10.4819(7) _cell_length_b 10.9273(7) _cell_length_c 12.5634(7) _cell_measurement_reflns_used 9991 _cell_measurement_temperature 172.99 _cell_measurement_theta_max 25.10 _cell_measurement_theta_min 3.03 _cell_volume 1291.14(14) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 172.99 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_unetI/netI 0.0243 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12748 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.022 _diffrn_reflns_theta_max 25.022 _diffrn_reflns_theta_min 3.050 _diffrn_source_current 30.0 _diffrn_source_power 1.35 _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.805 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_correction_T_min 0.6675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.729 _exptl_crystal_description block _exptl_crystal_F_000 670 _refine_diff_density_max 1.115 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 373 _refine_ls_number_reflns 4474 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.139 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0190 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+2.0876P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0479 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4270 _reflns_number_total 4474 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00902e2.cif _cod_data_source_block mo_zym02_0m _cod_depositor_comments 'Adding full bibliography for 7247702.cif.' _cod_database_code 7247702 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Others Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C9A)=Sof(H9AA)=Sof(C19A)=Sof(H19D)= Sof(H19E)=Sof(H19F)=1-FVAR(1) Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C9)=Sof(H9A)=Sof(C19)=Sof(H19A)= Sof(H19B)=Sof(H19C)=FVAR(1) 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C13(H13), C16(H16), C18(H18), C21(H21), C9(H9A), C9A(H9AA) 3.b Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F) 3.c Idealised tetrahedral OH refined as rotating group: O2(H2), O5(H5), O9(H9) ; _shelx_res_file ; TITL mo_zym02_0m_a.res in P-1 mo_zym02_0m.res created by SHELXL-2018/3 at 10:34:40 on 12-May-2023 REM Old TITL mo_ZYM02_0m_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.062, Rweak 0.008, Alpha 0.058, Orientation as input REM Formula found by SHELXT: C24 N4 O7 Tb CELL 0.71073 10.4819 10.9273 12.5634 104.646 108.134 97.016 ZERR 2 0.0007 0.0007 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H N O Tb UNIT 42 54 6 24 2 L.S. 10 PLAN 1 TEMP -100.16 CONF list 4 MORE -1 fmap 2 ACTA BOND $H OMIT -1 -1 1 REM REM REM WGHT 0.013100 2.087600 FVAR 0.50484 0.63349 TB1 5 0.596165 0.546992 0.682524 11.00000 0.00883 0.00865 = 0.01296 0.00294 0.00101 0.00097 O1 4 0.466982 0.335184 0.586635 11.00000 0.02108 0.00971 = 0.01600 0.00189 0.00544 0.00060 O2 4 0.838656 0.393645 0.264571 11.00000 0.01393 0.07225 = 0.01327 0.00298 0.00104 0.00378 AFIX 147 H2 2 0.755043 0.389871 0.254570 11.00000 -1.50000 AFIX 0 O3 4 0.666230 0.762890 0.849768 11.00000 0.01678 0.02084 = 0.01769 0.00202 0.00445 -0.00365 O4 4 0.419697 0.273676 0.392106 11.00000 0.02585 0.01166 = 0.01504 0.00516 0.00164 0.00332 O5 4 0.454749 0.048218 0.287364 11.00000 0.08110 0.02365 = 0.01694 0.01261 0.01989 0.02652 AFIX 147 H5 2 0.437733 0.122028 0.291150 11.00000 -1.50000 AFIX 0 O6 4 0.655893 0.486565 0.517590 11.00000 0.01391 0.01805 = 0.02695 0.00483 0.01039 0.00468 O7 4 0.751108 0.407037 0.734967 11.00000 0.02249 0.03200 = 0.04276 0.01795 0.00509 0.01512 O8 4 0.629513 0.423659 0.329418 11.00000 0.00995 0.02682 = 0.01937 0.00558 0.00197 0.00473 O9 4 0.734321 1.002776 0.994161 11.00000 0.02106 0.03311 = 0.03827 -0.00248 0.00980 -0.00069 AFIX 147 H9 2 0.679529 0.933777 0.947046 11.00000 -1.50000 AFIX 0 O10 4 0.821131 0.681528 0.785982 11.00000 0.01506 0.01633 = 0.02561 -0.00269 -0.00134 -0.00026 O12 4 0.558909 0.484561 0.840448 11.00000 0.03421 0.02313 = 0.01940 0.00892 0.00797 0.00195 N1 3 0.489299 0.310566 0.892046 11.00000 0.04211 0.02657 = 0.02588 0.01491 0.01370 0.00867 N3 3 0.928940 0.331025 0.830295 11.00000 0.03195 0.04067 = 0.03688 0.02254 0.00990 0.02207 C1 1 0.706116 0.462786 0.437629 11.00000 0.01386 0.01325 = 0.02070 0.00681 0.00757 0.00477 C2 1 1.076988 0.362252 0.901164 11.00000 0.04023 0.07089 = 0.05964 0.02169 0.00084 0.02401 AFIX 137 H2A 2 1.116675 0.452270 0.911326 11.00000 -1.50000 H2B 2 1.123250 0.304190 0.860799 11.00000 -1.50000 H2C 2 1.089433 0.351051 0.978469 11.00000 -1.50000 AFIX 0 C3 1 0.942704 0.535153 0.585550 11.00000 0.01496 0.02974 = 0.01652 0.00548 0.00756 0.00543 AFIX 43 H3 2 0.903290 0.559763 0.644207 11.00000 -1.20000 AFIX 0 C4 1 0.451928 0.252736 0.490704 11.00000 0.01259 0.00998 = 0.01764 0.00571 0.00183 -0.00080 C6 1 0.788940 0.772006 0.850529 11.00000 0.01912 0.01300 = 0.01242 0.00473 -0.00086 -0.00045 C7 1 0.381333 0.201456 0.872220 11.00000 0.05840 0.04250 = 0.05898 0.02844 0.03194 0.00692 AFIX 137 H7A 2 0.353671 0.214371 0.941234 11.00000 -1.50000 H7B 2 0.415556 0.121457 0.859226 11.00000 -1.50000 H7C 2 0.301916 0.194912 0.802820 11.00000 -1.50000 AFIX 0 C8 1 0.474377 0.120940 0.492949 11.00000 0.01612 0.01136 = 0.01526 0.00469 0.00244 0.00085 C10 1 0.857428 0.481685 0.468492 11.00000 0.01211 0.01815 = 0.01715 0.00620 0.00546 0.00436 C11 1 0.915435 0.446654 0.381465 11.00000 0.01604 0.02571 = 0.01374 0.00389 0.00392 0.00328 C12 1 0.864335 0.997868 0.995790 11.00000 0.01425 0.02003 = 0.01581 0.00526 0.00334 0.00077 C13 1 0.871977 0.422846 0.795610 11.00000 0.03019 0.03187 = 0.03290 0.01328 0.01161 0.00927 AFIX 43 H13 2 0.929034 0.506696 0.819537 11.00000 -1.20000 AFIX 0 C14 1 0.896326 0.890909 0.927743 11.00000 0.01767 0.01511 = 0.01396 0.00546 0.00245 -0.00049 C15 1 0.616620 0.330220 0.988294 11.00000 0.06382 0.06318 = 0.04843 0.03700 -0.00307 0.01167 AFIX 137 H15A 2 0.680963 0.406859 0.994287 11.00000 -1.50000 H15B 2 0.656783 0.253985 0.974042 11.00000 -1.50000 H15C 2 0.598558 0.343158 1.061901 11.00000 -1.50000 AFIX 0 C16 1 1.032430 0.894608 0.933000 11.00000 0.01925 0.01544 = 0.01515 0.00171 0.00434 0.00221 AFIX 43 H16 2 1.053860 0.822259 0.887009 11.00000 -1.20000 AFIX 0 C17 1 0.854189 0.201200 0.798125 11.00000 0.06505 0.04170 = 0.05703 0.02327 0.00431 0.01308 AFIX 137 H17A 2 0.834796 0.186330 0.865817 11.00000 -1.50000 H17B 2 0.908971 0.140842 0.773496 11.00000 -1.50000 H17C 2 0.767399 0.187157 0.732940 11.00000 -1.50000 AFIX 0 C18 1 0.497596 0.090683 0.597159 11.00000 0.03134 0.01471 = 0.01434 0.00267 0.00714 0.00588 AFIX 43 H18 2 0.495931 0.153605 0.664248 11.00000 -1.20000 AFIX 0 C20 1 0.476862 0.028261 0.393327 11.00000 0.02789 0.01732 = 0.01495 0.00653 0.00425 0.00495 C21 1 0.470873 0.388270 0.827259 11.00000 0.03306 0.02837 = 0.02023 0.01048 0.01323 0.00983 AFIX 43 H21 2 0.384319 0.370252 0.765708 11.00000 -1.20000 AFIX 0 O11 4 1.107294 0.225291 0.647637 11.00000 0.09746 0.10773 = 0.04823 0.02465 0.00576 0.02731 N2 3 0.976675 0.152227 0.453765 11.00000 0.05259 0.04141 = 0.04233 0.01683 0.01230 0.00246 PART 1 C5 1 0.847023 0.138439 0.474734 21.00000 0.05912 0.06626 = 0.08839 0.03282 0.02224 0.00583 AFIX 137 H5A 2 0.806901 0.046284 0.455732 21.00000 -1.50000 H5B 2 0.783142 0.177042 0.424860 21.00000 -1.50000 H5C 2 0.864007 0.182737 0.557683 21.00000 -1.50000 AFIX 0 PART 2 C5A 1 0.844357 0.117891 0.358113 -21.00000 0.06780 0.06997 = 0.09509 0.03713 -0.01583 -0.02434 AFIX 137 H5AA 2 0.771047 0.125974 0.390725 -21.00000 -1.50000 H5AB 2 0.829190 0.028314 0.308903 -21.00000 -1.50000 H5AC 2 0.843687 0.176254 0.310268 -21.00000 -1.50000 AFIX 0 PART 1 C9 1 1.094794 0.193391 0.544897 21.00000 0.06342 0.06092 = 0.07491 0.03392 0.02542 0.01675 AFIX 43 H9A 2 1.176983 0.198178 0.527673 21.00000 -1.20000 AFIX 0 PART 2 C9A 1 0.997911 0.201595 0.564633 -21.00000 0.07556 0.04772 = 0.06580 0.02685 0.02940 0.02531 AFIX 43 H9AA 2 0.920645 0.221708 0.583998 -21.00000 -1.20000 AFIX 0 PART 1 C19 1 0.968003 0.112512 0.334979 21.00000 0.11673 0.05667 = 0.05542 0.01621 0.03193 0.01424 AFIX 137 H19A 2 1.059967 0.132830 0.331387 21.00000 -1.50000 H19B 2 0.907633 0.158306 0.290609 21.00000 -1.50000 H19C 2 0.930403 0.018895 0.300669 21.00000 -1.50000 AFIX 0 PART 2 C19A 1 1.100573 0.144324 0.419514 -21.00000 0.07628 0.07571 = 0.07604 0.02612 0.04702 0.03220 AFIX 137 H19D 2 1.183968 0.181775 0.489775 -21.00000 -1.50000 H19E 2 1.099764 0.192623 0.363436 -21.00000 -1.50000 H19F 2 1.099192 0.053393 0.382883 -21.00000 -1.50000 AFIX 0 HKLF 4 REM mo_zym02_0m_a.res in P-1 REM wR2 = 0.0479, GooF = S = 1.139, Restrained GooF = 1.139 for all data REM R1 = 0.0190 for 4270 Fo > 4sig(Fo) and 0.0207 for all 4474 data REM 373 parameters refined using 0 restraints END WGHT 0.0131 2.0876 REM Highest difference peak 1.115, deepest hole -0.805, 1-sigma level 0.084 Q1 1 1.0920 0.8014 0.8833 11.00000 0.05 1.12 ; _shelx_res_checksum 8954 _olex2_submission_special_instructions 'No special instructions were received' 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 Tb1 Tb 0.59616(2) 0.54699(2) 0.68252(2) 0.01102(5) Uani 1 1 d . . . . . O1 O 0.46698(19) 0.33518(18) 0.58664(16) 0.0166(4) Uani 1 1 d . . . . . O2 O 0.8387(2) 0.3936(3) 0.26457(18) 0.0366(6) Uani 1 1 d . . . . . H2 H 0.755043 0.389871 0.254570 0.055 Uiso 1 1 calc R U . . . O3 O 0.66623(19) 0.76289(19) 0.84977(17) 0.0204(4) Uani 1 1 d . . . . . O4 O 0.4197(2) 0.27368(18) 0.39211(16) 0.0188(4) Uani 1 1 d . . . . . O5 O 0.4547(3) 0.0482(2) 0.28736(19) 0.0373(6) Uani 1 1 d . . . . . H5 H 0.437733 0.122028 0.291150 0.056 Uiso 1 1 calc R U . . . O6 O 0.65589(19) 0.48656(19) 0.51759(18) 0.0192(4) Uani 1 1 d . . . . . O7 O 0.7511(2) 0.4070(2) 0.7350(2) 0.0319(5) Uani 1 1 d . . . . . O8 O 0.62951(19) 0.4237(2) 0.32942(17) 0.0198(4) Uani 1 1 d . . . . . O9 O 0.7343(2) 1.0028(2) 0.9942(2) 0.0343(6) Uani 1 1 d . . . . . H9 H 0.679529 0.933777 0.947046 0.051 Uiso 1 1 calc R U . . . O10 O 0.8211(2) 0.68153(19) 0.78598(18) 0.0233(5) Uani 1 1 d . . . . . O12 O 0.5589(2) 0.4846(2) 0.84045(18) 0.0259(5) Uani 1 1 d . . . . . N1 N 0.4893(3) 0.3106(3) 0.8920(2) 0.0297(6) Uani 1 1 d . . . . . N3 N 0.9289(3) 0.3310(3) 0.8303(3) 0.0337(7) Uani 1 1 d . . . . . C1 C 0.7061(3) 0.4628(3) 0.4376(2) 0.0151(6) Uani 1 1 d . . . . . C2 C 1.0770(4) 0.3623(5) 0.9012(4) 0.0597(12) Uani 1 1 d . . . . . H2A H 1.116675 0.452270 0.911326 0.090 Uiso 1 1 calc R U . . . H2B H 1.123250 0.304190 0.860799 0.090 Uiso 1 1 calc R U . . . H2C H 1.089433 0.351051 0.978469 0.090 Uiso 1 1 calc R U . . . C3 C 0.9427(3) 0.5352(3) 0.5856(2) 0.0202(6) Uani 1 1 d . . . . . H3 H 0.903290 0.559763 0.644207 0.024 Uiso 1 1 calc R U . . . C4 C 0.4519(3) 0.2527(3) 0.4907(2) 0.0143(6) Uani 1 1 d . . . . . C6 C 0.7889(3) 0.7720(3) 0.8505(2) 0.0167(6) Uani 1 1 d . . . . . C7 C 0.3813(4) 0.2015(4) 0.8722(4) 0.0484(10) Uani 1 1 d . . . . . H7A H 0.353671 0.214371 0.941234 0.073 Uiso 1 1 calc R U . . . H7B H 0.415556 0.121457 0.859226 0.073 Uiso 1 1 calc R U . . . H7C H 0.301916 0.194912 0.802820 0.073 Uiso 1 1 calc R U . . . C8 C 0.4744(3) 0.1209(3) 0.4929(2) 0.0151(6) Uani 1 1 d . . . . . C10 C 0.8574(3) 0.4817(3) 0.4685(2) 0.0155(6) Uani 1 1 d . . . . . C11 C 0.9154(3) 0.4467(3) 0.3815(2) 0.0194(6) Uani 1 1 d . . . . . C12 C 0.8643(3) 0.9979(3) 0.9958(2) 0.0175(6) Uani 1 1 d . . . . . C13 C 0.8720(3) 0.4228(3) 0.7956(3) 0.0307(7) Uani 1 1 d . . . . . H13 H 0.929034 0.506696 0.819537 0.037 Uiso 1 1 calc R U . . . C14 C 0.8963(3) 0.8909(3) 0.9277(2) 0.0166(6) Uani 1 1 d . . . . . C15 C 0.6166(5) 0.3302(5) 0.9883(4) 0.0605(13) Uani 1 1 d . . . . . H15A H 0.680963 0.406859 0.994287 0.091 Uiso 1 1 calc R U . . . H15B H 0.656783 0.253985 0.974042 0.091 Uiso 1 1 calc R U . . . H15C H 0.598558 0.343158 1.061901 0.091 Uiso 1 1 calc R U . . . C16 C 1.0324(3) 0.8946(3) 0.9330(2) 0.0178(6) Uani 1 1 d . . . . . H16 H 1.053860 0.822259 0.887009 0.021 Uiso 1 1 calc R U . . . C17 C 0.8542(5) 0.2012(4) 0.7981(4) 0.0572(12) Uani 1 1 d . . . . . H17A H 0.834796 0.186330 0.865817 0.086 Uiso 1 1 calc R U . . . H17B H 0.908971 0.140842 0.773496 0.086 Uiso 1 1 calc R U . . . H17C H 0.767399 0.187157 0.732940 0.086 Uiso 1 1 calc R U . . . C18 C 0.4976(3) 0.0907(3) 0.5972(3) 0.0207(6) Uani 1 1 d . . . . . H18 H 0.495931 0.153605 0.664248 0.025 Uiso 1 1 calc R U . . . C20 C 0.4769(3) 0.0283(3) 0.3933(2) 0.0206(6) Uani 1 1 d . . . . . C21 C 0.4709(3) 0.3883(3) 0.8273(3) 0.0254(7) Uani 1 1 d . . . . . H21 H 0.384319 0.370252 0.765708 0.031 Uiso 1 1 calc R U . . . O11 O 1.1073(5) 0.2253(4) 0.6476(3) 0.0889(12) Uani 1 1 d . . . . . N2 N 0.9767(4) 0.1522(3) 0.4538(3) 0.0465(8) Uani 1 1 d . . . . . C5 C 0.8470(8) 0.1384(8) 0.4747(9) 0.071(3) Uani 0.633(9) 1 d . . P A 1 H5A H 0.806901 0.046284 0.455732 0.107 Uiso 0.633(9) 1 calc R U P A 1 H5B H 0.783142 0.177042 0.424860 0.107 Uiso 0.633(9) 1 calc R U P A 1 H5C H 0.864007 0.182737 0.557683 0.107 Uiso 0.633(9) 1 calc R U P A 1 C5A C 0.8444(17) 0.1179(16) 0.3581(16) 0.090(7) Uani 0.367(9) 1 d . . P A 2 H5AA H 0.771047 0.125974 0.390725 0.135 Uiso 0.367(9) 1 calc R U P A 2 H5AB H 0.829190 0.028314 0.308903 0.135 Uiso 0.367(9) 1 calc R U P A 2 H5AC H 0.843687 0.176254 0.310268 0.135 Uiso 0.367(9) 1 calc R U P A 2 C9 C 1.0948(9) 0.1934(8) 0.5449(8) 0.063(2) Uani 0.633(9) 1 d . . P A 1 H9A H 1.176983 0.198178 0.527673 0.076 Uiso 0.633(9) 1 calc R U P A 1 C9A C 0.9979(17) 0.2016(12) 0.5646(12) 0.059(4) Uani 0.367(9) 1 d . . P A 2 H9AA H 0.920645 0.221708 0.583998 0.071 Uiso 0.367(9) 1 calc R U P A 2 C19 C 0.9680(12) 0.1125(8) 0.3350(7) 0.077(3) Uani 0.633(9) 1 d . . P A 1 H19A H 1.059967 0.132830 0.331387 0.115 Uiso 0.633(9) 1 calc R U P A 1 H19B H 0.907633 0.158306 0.290609 0.115 Uiso 0.633(9) 1 calc R U P A 1 H19C H 0.930403 0.018895 0.300669 0.115 Uiso 0.633(9) 1 calc R U P A 1 C19A C 1.1006(16) 0.1443(15) 0.4195(14) 0.069(5) Uani 0.367(9) 1 d . . P A 2 H19D H 1.183968 0.181775 0.489775 0.104 Uiso 0.367(9) 1 calc R U P A 2 H19E H 1.099764 0.192623 0.363436 0.104 Uiso 0.367(9) 1 calc R U P A 2 H19F H 1.099192 0.053393 0.382883 0.104 Uiso 0.367(9) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.00883(7) 0.00865(8) 0.01296(8) 0.00294(5) 0.00101(5) 0.00097(5) O1 0.0211(10) 0.0097(9) 0.0160(10) 0.0019(8) 0.0054(8) 0.0006(8) O2 0.0139(11) 0.0722(18) 0.0133(10) 0.0030(11) 0.0010(9) 0.0038(11) O3 0.0168(10) 0.0208(11) 0.0177(10) 0.0020(9) 0.0044(8) -0.0037(8) O4 0.0259(11) 0.0117(10) 0.0150(10) 0.0052(8) 0.0016(8) 0.0033(8) O5 0.0811(19) 0.0237(12) 0.0169(11) 0.0126(10) 0.0199(12) 0.0265(13) O6 0.0139(10) 0.0181(10) 0.0269(11) 0.0048(9) 0.0104(9) 0.0047(8) O7 0.0225(12) 0.0320(13) 0.0428(14) 0.0179(11) 0.0051(11) 0.0151(10) O8 0.0099(9) 0.0268(11) 0.0194(10) 0.0056(9) 0.0020(8) 0.0047(8) O9 0.0211(11) 0.0331(13) 0.0383(14) -0.0025(11) 0.0098(10) -0.0007(10) O10 0.0151(10) 0.0163(10) 0.0256(11) -0.0027(9) -0.0013(9) -0.0003(8) O12 0.0342(12) 0.0231(11) 0.0194(11) 0.0089(9) 0.0080(9) 0.0020(10) N1 0.0421(16) 0.0266(15) 0.0259(14) 0.0149(12) 0.0137(13) 0.0087(13) N3 0.0319(15) 0.0407(17) 0.0369(16) 0.0225(14) 0.0099(13) 0.0221(14) C1 0.0139(13) 0.0132(13) 0.0207(15) 0.0068(12) 0.0076(12) 0.0048(11) C2 0.040(2) 0.071(3) 0.060(3) 0.022(3) 0.001(2) 0.024(2) C3 0.0150(14) 0.0297(17) 0.0165(14) 0.0055(13) 0.0076(12) 0.0054(12) C4 0.0126(13) 0.0100(13) 0.0176(14) 0.0057(12) 0.0018(11) -0.0008(11) C6 0.0191(15) 0.0130(14) 0.0124(13) 0.0047(12) -0.0009(11) -0.0004(11) C7 0.058(3) 0.042(2) 0.059(3) 0.028(2) 0.032(2) 0.007(2) C8 0.0161(13) 0.0114(13) 0.0153(13) 0.0047(11) 0.0024(11) 0.0009(11) C10 0.0121(13) 0.0182(14) 0.0172(14) 0.0062(12) 0.0055(11) 0.0044(11) C11 0.0160(14) 0.0257(16) 0.0137(14) 0.0039(13) 0.0039(11) 0.0033(12) C12 0.0142(13) 0.0200(15) 0.0158(14) 0.0053(12) 0.0033(11) 0.0008(12) C13 0.0302(18) 0.0319(18) 0.0329(18) 0.0133(15) 0.0116(15) 0.0093(15) C14 0.0177(14) 0.0151(14) 0.0140(13) 0.0055(12) 0.0025(11) -0.0005(11) C15 0.064(3) 0.063(3) 0.048(3) 0.037(2) -0.003(2) 0.012(2) C16 0.0192(14) 0.0154(14) 0.0152(14) 0.0017(12) 0.0043(12) 0.0022(12) C17 0.065(3) 0.042(2) 0.057(3) 0.023(2) 0.004(2) 0.013(2) C18 0.0313(16) 0.0147(14) 0.0143(14) 0.0027(12) 0.0071(12) 0.0059(12) C20 0.0279(16) 0.0173(15) 0.0149(14) 0.0065(12) 0.0043(12) 0.0050(12) C21 0.0331(17) 0.0284(17) 0.0202(15) 0.0105(14) 0.0132(14) 0.0098(14) O11 0.097(3) 0.108(3) 0.048(2) 0.025(2) 0.006(2) 0.027(3) N2 0.053(2) 0.0414(19) 0.042(2) 0.0168(16) 0.0123(17) 0.0025(16) C5 0.059(5) 0.066(5) 0.088(7) 0.033(5) 0.022(5) 0.006(4) C5A 0.068(10) 0.070(10) 0.095(13) 0.037(10) -0.016(9) -0.024(8) C9 0.063(5) 0.061(5) 0.075(6) 0.034(5) 0.025(5) 0.017(4) C9A 0.076(10) 0.048(7) 0.066(9) 0.027(7) 0.029(8) 0.025(7) C19 0.117(9) 0.057(5) 0.055(5) 0.016(4) 0.032(5) 0.014(5) C19A 0.076(10) 0.076(10) 0.076(10) 0.026(8) 0.047(9) 0.032(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 Tb1 O3 151.43(6) . . ? O1 Tb1 O4 126.62(7) . 2_666 ? O1 Tb1 O7 73.99(7) . . ? O1 Tb1 O8 78.78(7) . 2_666 ? O1 Tb1 O10 145.89(7) . . ? O1 Tb1 O12 78.18(7) . . ? O1 Tb1 C6 163.29(7) . . ? O3 Tb1 C6 26.62(7) . . ? O4 Tb1 O3 68.50(6) 2_666 . ? O4 Tb1 O7 141.16(7) 2_666 . ? O4 Tb1 O8 77.94(7) 2_666 2_666 ? O4 Tb1 O10 77.84(7) 2_666 . ? O4 Tb1 C6 70.08(7) 2_666 . ? O6 Tb1 O1 77.23(7) . . ? O6 Tb1 O3 131.24(6) . . ? O6 Tb1 O4 76.03(7) . 2_666 ? O6 Tb1 O7 78.27(8) . . ? O6 Tb1 O8 122.30(7) . 2_666 ? O6 Tb1 O10 88.49(7) . . ? O6 Tb1 O12 145.88(7) . . ? O6 Tb1 C6 109.79(7) . . ? O7 Tb1 O3 110.22(7) . . ? O7 Tb1 C6 92.27(8) . . ? O8 Tb1 O3 81.99(6) 2_666 . ? O8 Tb1 O7 140.87(7) 2_666 . ? O8 Tb1 C6 108.05(8) 2_666 . ? O10 Tb1 O3 52.67(6) . . ? O10 Tb1 O7 72.84(7) . . ? O10 Tb1 O8 133.89(7) . 2_666 ? O10 Tb1 C6 26.11(8) . . ? O12 Tb1 O3 76.52(7) . . ? O12 Tb1 O4 138.07(7) . 2_666 ? O12 Tb1 O7 72.44(8) . . ? O12 Tb1 O8 74.89(7) . 2_666 ? O12 Tb1 O10 99.02(7) . . ? O12 Tb1 C6 88.76(8) . . ? C4 O1 Tb1 133.12(17) . . ? C11 O2 H2 109.5 . . ? C6 O3 Tb1 88.57(16) . . ? C4 O4 Tb1 138.54(17) . 2_666 ? C20 O5 H5 109.5 . . ? C1 O6 Tb1 171.52(19) . . ? C13 O7 Tb1 135.7(2) . . ? C1 O8 Tb1 107.81(16) . 2_666 ? C12 O9 H9 109.5 . . ? C6 O10 Tb1 97.68(17) . . ? C21 O12 Tb1 124.17(19) . . ? C15 N1 C7 116.5(3) . . ? C21 N1 C7 121.6(3) . . ? C21 N1 C15 121.9(3) . . ? C13 N3 C2 119.1(3) . . ? C13 N3 C17 122.7(3) . . ? C17 N3 C2 118.2(3) . . ? O6 C1 O8 121.2(2) . . ? O6 C1 C10 120.2(2) . . ? O8 C1 C10 118.6(2) . . ? N3 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? N3 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C10 C3 H3 119.4 . . ? C10 C3 C11 121.2(3) . 2_766 ? C11 C3 H3 119.4 2_766 . ? O1 C4 O4 124.7(2) . . ? O1 C4 C8 118.0(2) . . ? O4 C4 C8 117.4(2) . . ? O3 C6 Tb1 64.81(14) . . ? O3 C6 C14 120.0(2) . . ? O10 C6 Tb1 56.21(14) . . ? O10 C6 O3 120.8(3) . . ? O10 C6 C14 119.2(3) . . ? C14 C6 Tb1 173.42(19) . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C18 C8 C4 119.0(3) . . ? C18 C8 C20 119.2(3) . . ? C20 C8 C4 121.8(2) . . ? C3 C10 C1 119.2(2) . . ? C3 C10 C11 119.5(3) . . ? C11 C10 C1 121.2(2) . . ? O2 C11 C3 117.6(3) . 2_766 ? O2 C11 C10 123.1(3) . . ? C3 C11 C10 119.3(3) 2_766 . ? O9 C12 C14 123.3(3) . . ? O9 C12 C16 117.2(3) . 2_777 ? C16 C12 C14 119.5(3) 2_777 . ? O7 C13 N3 124.5(3) . . ? O7 C13 H13 117.7 . . ? N3 C13 H13 117.7 . . ? C12 C14 C6 121.6(3) . . ? C16 C14 C6 118.7(3) . . ? C16 C14 C12 119.7(3) . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C14 120.8(3) 2_777 . ? C12 C16 H16 119.6 2_777 . ? C14 C16 H16 119.6 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C8 C18 H18 118.9 . . ? C20 C18 C8 122.2(3) 2_656 . ? C20 C18 H18 118.9 2_656 . ? O5 C20 C8 123.7(3) . . ? O5 C20 C18 117.7(3) . 2_656 ? C18 C20 C8 118.6(3) 2_656 . ? O12 C21 N1 124.8(3) . . ? O12 C21 H21 117.6 . . ? N1 C21 H21 117.6 . . ? C5A N2 C19A 116.6(11) . . ? C9 N2 C5 119.5(6) . . ? C9 N2 C19 123.7(7) . . ? C9A N2 C5A 125.8(12) . . ? C9A N2 C19A 117.2(10) . . ? C19 N2 C5 116.7(6) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C5A H5AA 109.5 . . ? N2 C5A H5AB 109.5 . . ? N2 C5A H5AC 109.5 . . ? H5AA C5A H5AB 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? O11 C9 N2 126.0(8) . . ? O11 C9 H9A 117.0 . . ? N2 C9 H9A 117.0 . . ? O11 C9A N2 127.1(13) . . ? O11 C9A H9AA 116.5 . . ? N2 C9A H9AA 116.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C19A H19D 109.5 . . ? N2 C19A H19E 109.5 . . ? N2 C19A H19F 109.5 . . ? H19D C19A H19E 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.3347(18) . ? Tb1 O3 2.575(2) . ? Tb1 O4 2.3788(19) 2_666 ? Tb1 O6 2.3105(19) . ? Tb1 O7 2.421(2) . ? Tb1 O8 2.3895(18) 2_666 ? Tb1 O10 2.3854(19) . ? Tb1 O12 2.378(2) . ? Tb1 C6 2.844(3) . ? O1 C4 1.260(3) . ? O2 H2 0.8400 . ? O2 C11 1.364(4) . ? O3 C6 1.275(3) . ? O4 C4 1.266(3) . ? O5 H5 0.8400 . ? O5 C20 1.357(4) . ? O6 C1 1.259(3) . ? O7 C13 1.223(4) . ? O8 C1 1.272(3) . ? O9 H9 0.8400 . ? O9 C12 1.364(4) . ? O10 C6 1.263(3) . ? O12 C21 1.251(4) . ? N1 C7 1.452(5) . ? N1 C15 1.443(5) . ? N1 C21 1.309(4) . ? N3 C2 1.475(5) . ? N3 C13 1.326(4) . ? N3 C17 1.425(5) . ? C1 C10 1.485(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 0.9500 . ? C3 C10 1.387(4) . ? C3 C11 1.387(4) 2_766 ? C4 C8 1.493(4) . ? C6 C14 1.491(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C18 1.387(4) . ? C8 C20 1.407(4) . ? C10 C11 1.404(4) . ? C12 C14 1.407(4) . ? C12 C16 1.381(4) 2_777 ? C13 H13 0.9500 . ? C14 C16 1.403(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 0.9500 . ? C18 C20 1.385(4) 2_656 ? C21 H21 0.9500 . ? O11 C9 1.209(9) . ? O11 C9A 1.231(15) . ? N2 C5 1.460(9) . ? N2 C5A 1.455(15) . ? N2 C9 1.329(9) . ? N2 C9A 1.296(14) . ? N2 C19 1.415(9) . ? N2 C19A 1.495(13) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? C9 H9A 0.9500 . ? C9A H9AA 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tb1 O1 C4 O4 -52.1(4) . . . . ? Tb1 O1 C4 C8 127.6(2) . . . . ? Tb1 O3 C6 O10 -4.7(3) . . . . ? Tb1 O3 C6 C14 174.9(2) . . . . ? Tb1 O4 C4 O1 12.6(4) 2_666 . . . ? Tb1 O4 C4 C8 -167.00(18) 2_666 . . . ? Tb1 O7 C13 N3 166.0(2) . . . . ? Tb1 O8 C1 O6 12.2(3) 2_666 . . . ? Tb1 O8 C1 C10 -167.08(19) 2_666 . . . ? Tb1 O10 C6 O3 5.1(3) . . . . ? Tb1 O10 C6 C14 -174.5(2) . . . . ? Tb1 O12 C21 N1 141.0(3) . . . . ? O1 C4 C8 C18 6.1(4) . . . . ? O1 C4 C8 C20 -171.9(3) . . . . ? O3 C6 C14 C12 -3.7(4) . . . . ? O3 C6 C14 C16 175.6(3) . . . . ? O4 C4 C8 C18 -174.3(3) . . . . ? O4 C4 C8 C20 7.8(4) . . . . ? O6 C1 C10 C3 -5.0(4) . . . . ? O6 C1 C10 C11 175.1(3) . . . . ? O8 C1 C10 C3 174.3(3) . . . . ? O8 C1 C10 C11 -5.6(4) . . . . ? O9 C12 C14 C6 -1.9(4) . . . . ? O9 C12 C14 C16 178.9(3) . . . . ? O10 C6 C14 C12 176.0(3) . . . . ? O10 C6 C14 C16 -4.8(4) . . . . ? C1 C10 C11 O2 -0.1(4) . . . . ? C1 C10 C11 C3 -179.4(3) . . . 2_766 ? C2 N3 C13 O7 178.6(4) . . . . ? C3 C10 C11 O2 -180.0(3) . . . . ? C3 C10 C11 C3 0.7(5) . . . 2_766 ? C4 C8 C18 C20 -178.1(3) . . . 2_656 ? C4 C8 C20 O5 -2.4(5) . . . . ? C4 C8 C20 C18 178.0(3) . . . 2_656 ? C6 C14 C16 C12 -179.3(3) . . . 2_777 ? C7 N1 C21 O12 179.2(3) . . . . ? C11 C3 C10 C1 179.3(3) 2_766 . . . ? C11 C3 C10 C11 -0.8(5) 2_766 . . . ? C12 C14 C16 C12 0.0(5) . . . 2_777 ? C15 N1 C21 O12 0.5(5) . . . . ? C16 C12 C14 C6 179.3(3) 2_777 . . . ? C16 C12 C14 C16 0.0(4) 2_777 . . . ? C17 N3 C13 O7 1.1(6) . . . . ? C18 C8 C20 O5 179.7(3) . . . . ? C18 C8 C20 C18 0.1(5) . . . 2_656 ? C20 C8 C18 C20 -0.1(5) . . . 2_656 ? C5 N2 C9 O11 -2.2(11) . . . . ? C5A N2 C9A O11 176.0(11) . . . . ? C19 N2 C9 O11 -178.1(7) . . . . ? C19A N2 C9A O11 -11.8(16) . . . . ?