#------------------------------------------------------------------------------ #$Date: 2019-01-16 01:02:24 +0200 (Wed, 16 Jan 2019) $ #$Revision: 213083 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/28/7122839.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_7122839 loop_ _publ_author_name 'Feng, Lu' 'Wang, Hui-Sheng' 'Xu, Hailong' 'Huang, Wentao' 'Zeng, Tianyu' 'Cheng, Qing rong' 'Pan, Zhi-Quan' 'Zhou, Hong' _publ_section_title ; A water stable layered Tb(III) polycarboxylate with high proton conductivity over 10-2 S•cm-1 in a wide temperature range ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C8CC08706G _journal_year 2019 _chemical_formula_sum 'C30 H46 N12 O35 Tb4' _chemical_formula_weight 1770.47 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc20z97k _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-01-08 deposited with the CCDC. 2019-01-15 downloaded from the CCDC. ; _cell_angle_alpha 62.703(2) _cell_angle_beta 74.569(2) _cell_angle_gamma 68.667(2) _cell_formula_units_Z 1 _cell_length_a 10.7095(7) _cell_length_b 11.3590(6) _cell_length_c 12.0866(7) _cell_measurement_reflns_used 3509 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.3312 _cell_measurement_theta_min 2.9703 _cell_volume 1208.29(13) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'PHOTON 100 CMOS detector' _diffrn_measurement_method 'omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_unetI/netI 0.0756 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12685 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.364 _exptl_absorpt_coefficient_mu 5.905 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.433 _exptl_crystal_description plate _exptl_crystal_F_000 850 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.033 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.207 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 4228 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0389 _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^)+(0.0187P)^2^+1.0080P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.0634 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3109 _reflns_number_total 4228 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8cc08706g2.cif _cod_data_source_block 1 _cod_database_code 7122839 _shelx_shelxl_version_number 2014/7 _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_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P1 New: P-1 CELL 0.71073 10.7095 11.3590 12.0866 62.703 74.569 68.667 ZERR 1 0.0007 0.0006 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H N O Tb UNIT 30 46 12 35 4 omit -1 0 1 omit 1 3 1 omit 0 3 2 omit -2 -2 1 omit -1 1 1 omit -3 -3 10 omit -1 1 0 omit -3 2 0 omit -1 2 2 omit 1 4 4 omit -3 8 3 OMIT 0.00 50.00 L.S. 25 ACTA BOND $H FMAP 2 PLAN 0 isor 0.001 c3 isor 0.001 n3 isor 0.001 c1 isor 0.001 c2 isor 0.001 c4 isor 0.001 c9 isor 0.001 c7 isor 0.001 c14 isor 0.001 c6 CONF isor 0.001 n6 n4 isor 0.005 o18 htab TEMP -100 WGHT 0.018700 1.008000 FVAR 0.11465 C1 1 0.368047 0.101894 0.102299 11.00000 0.00932 0.00818 = 0.00873 -0.00426 -0.00094 -0.00256 C2 1 0.590203 0.069849 0.060061 11.00000 0.00862 0.00872 = 0.00791 -0.00363 -0.00159 -0.00247 C3 1 0.501326 -0.082129 0.233499 11.00000 0.00502 0.00515 = 0.00516 -0.00250 -0.00125 -0.00180 C4 1 0.654600 -0.269219 0.379653 11.00000 0.00689 0.00730 = 0.00816 -0.00202 -0.00120 -0.00281 AFIX 23 H4A 2 0.715943 -0.287690 0.308482 11.00000 -1.20000 H4B 2 0.652168 -0.359746 0.449248 11.00000 -1.20000 AFIX 0 C5 1 0.714790 -0.198138 0.421002 11.00000 0.01138 0.01437 = 0.00404 -0.00093 0.00093 -0.00728 C6 1 0.409577 -0.254830 0.419858 11.00000 0.01019 0.01033 = 0.00948 -0.00411 -0.00111 -0.00291 AFIX 23 H6A 2 0.438094 -0.355462 0.442079 11.00000 -1.20000 H6B 2 0.330885 -0.212626 0.372405 11.00000 -1.20000 AFIX 0 C7 1 0.367884 -0.228712 0.541236 11.00000 0.01257 0.01213 = 0.01344 -0.00478 -0.00139 -0.00407 C8 1 0.824472 0.053668 0.042306 11.00000 0.00590 0.00565 = 0.00903 -0.00315 0.00366 -0.00454 AFIX 23 H8A 2 0.892810 0.096614 -0.021196 11.00000 -1.20000 H8B 2 0.856578 -0.046424 0.061643 11.00000 -1.20000 AFIX 0 C9 1 0.815177 0.073069 0.159767 11.00000 0.00800 0.00776 = 0.00826 -0.00292 -0.00071 -0.00267 C10 1 0.686902 0.226361 -0.132527 11.00000 0.00724 0.00939 = 0.00341 -0.00227 -0.00075 -0.00361 AFIX 23 H10A 2 0.626042 0.217492 -0.175468 11.00000 -1.20000 H10B 2 0.776908 0.217094 -0.182541 11.00000 -1.20000 AFIX 0 C11 1 0.635734 0.369504 -0.135566 11.00000 0.00568 0.01207 = 0.00515 -0.00361 -0.00059 -0.00196 C12 1 0.125357 0.149043 0.163094 11.00000 0.01510 0.01379 = 0.00713 -0.00386 -0.00621 -0.00374 AFIX 23 H12A 2 0.124853 0.061351 0.164572 11.00000 -1.20000 H12B 2 0.042613 0.220024 0.128238 11.00000 -1.20000 AFIX 0 C13 1 0.116832 0.129989 0.296030 11.00000 0.00919 0.00691 = 0.01345 -0.00678 0.00102 0.00191 C14 1 0.228063 0.326898 -0.023181 11.00000 0.00855 0.00833 = 0.00875 -0.00308 -0.00144 -0.00233 AFIX 23 H14A 2 0.131046 0.377738 -0.027292 11.00000 -1.20000 H14B 2 0.265587 0.317486 -0.103881 11.00000 -1.20000 AFIX 0 C15 1 0.299789 0.411832 -0.007507 11.00000 0.00675 0.00721 = 0.01415 -0.00172 0.00333 -0.00454 N1 3 0.469555 0.146322 0.020879 11.00000 0.01066 0.00822 = 0.00570 -0.00307 -0.00084 -0.00288 N2 3 0.614739 -0.045679 0.165737 11.00000 0.01332 0.00447 = 0.00288 -0.00029 -0.00250 -0.00387 N3 3 0.375408 -0.013489 0.206397 11.00000 0.00674 0.00637 = 0.00638 -0.00228 0.00007 -0.00142 N4 3 0.519458 -0.197021 0.341395 11.00000 0.00694 0.00703 = 0.00790 -0.00251 -0.00120 -0.00251 N5 3 0.699097 0.111480 -0.011176 11.00000 0.01286 0.00344 = 0.00548 0.00103 -0.00347 -0.00266 N6 3 0.240831 0.188954 0.077855 11.00000 0.00611 0.00719 = 0.00705 -0.00169 -0.00150 -0.00317 O1 4 0.657167 -0.080740 0.421364 11.00000 0.00777 0.01170 = 0.01266 -0.00478 -0.00180 -0.00314 O2 4 0.834010 -0.260855 0.452212 11.00000 0.01011 0.01461 = 0.02105 -0.00570 -0.00756 -0.00412 O3 4 0.429997 -0.313837 0.632741 11.00000 0.02526 0.01386 = 0.01190 -0.00387 -0.00967 0.00105 O4 4 0.273599 -0.121919 0.537860 11.00000 0.01958 0.01623 = 0.01537 -0.00842 -0.00516 0.00018 O5 4 0.900124 -0.012696 0.234398 11.00000 0.01465 0.02016 = 0.01113 -0.00447 -0.00368 -0.00701 O6 4 0.725691 0.174745 0.177105 11.00000 0.01351 0.01230 = 0.00995 -0.00374 0.00033 -0.00404 O7 4 0.581216 0.390433 -0.038278 11.00000 0.01164 0.00972 = 0.01039 -0.00519 -0.00003 -0.00226 O8 4 0.638604 0.470860 -0.241340 11.00000 0.01785 0.00852 = 0.00578 0.00052 -0.00018 -0.00107 O9 4 0.036325 0.064774 0.378408 11.00000 0.00929 0.01697 = 0.00909 -0.00634 0.00308 -0.00709 O10 4 0.185628 0.176187 0.328962 11.00000 0.01047 0.01026 = 0.01619 -0.00730 -0.00068 -0.00383 O11 4 0.320945 0.514071 -0.108129 11.00000 0.01828 0.01009 = 0.00957 0.00103 -0.00355 -0.00925 O12 4 1.082162 -0.246596 0.474263 11.00000 0.00572 0.01483 = 0.02656 -0.00712 -0.00113 -0.00188 O13 4 0.543725 -0.159141 0.698499 11.00000 0.01772 0.00954 = 0.00917 -0.00048 -0.00098 -0.00778 O14 4 0.329954 0.379975 0.097840 11.00000 0.01807 0.01127 = 0.00691 -0.00026 -0.00618 -0.00537 O15 4 0.002653 0.722166 0.206865 10.50000 0.03448 0.04077 = 0.03431 -0.00489 0.00011 -0.00310 O16 4 0.131873 0.540259 0.407747 11.00000 0.01747 0.01561 = 0.02860 -0.00757 0.00196 0.00058 O17 4 0.849499 0.398189 0.294323 11.00000 0.11362 0.06631 = 0.07152 0.02871 -0.06738 -0.06235 O18 4 0.050483 0.519231 0.176201 11.00000 0.03430 0.11261 = 0.07716 0.00460 -0.01067 -0.00445 TB1 5 0.878354 -0.065729 0.446299 11.00000 0.00878 0.00890 = 0.00854 -0.00332 -0.00114 -0.00370 TB2 5 0.471158 -0.354336 0.829653 11.00000 0.00995 0.00714 = 0.00512 -0.00156 -0.00128 -0.00279 HKLF 4 REM 1 in P1 New: P-1 REM R1 = 0.0389 for 3109 Fo > 4sig(Fo) and 0.0700 for all 4228 data REM 370 parameters refined using 72 restraints END WGHT 0.0187 1.0093 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z HTAB C8 O15_$1 EQIV $2 x+1, y-1, z HTAB C8 O15_$2 EQIV $3 -x+1, -y, -z HTAB C10 N3_$3 HTAB C10 O15_$1 EQIV $4 x-1, y, z HTAB C12 O5_$4 EQIV $5 -x, -y+1, -z HTAB C14 O18_$5 REM Highest difference peak 1.033, deepest hole -0.915, 1-sigma level 0.207 Q1 1 0.0391 0.4763 0.1553 11.00000 0.05 1.03 Q2 1 0.2941 0.1332 0.0836 11.00000 0.05 0.96 Q3 1 0.4912 0.3947 -0.2358 11.00000 0.05 0.86 Q4 1 0.7595 0.4020 -0.1153 11.00000 0.05 0.84 Q5 1 0.9230 -0.0956 0.0972 11.00000 0.05 0.80 Q6 1 0.9185 0.0380 -0.0677 11.00000 0.05 0.77 Q7 1 0.0421 0.5838 0.1748 11.00000 0.05 0.76 Q8 1 0.4738 -0.1987 0.3865 11.00000 0.05 0.76 Q9 1 1.1098 -0.2807 0.5485 11.00000 0.05 0.75 Q10 1 1.1057 -0.3165 0.4372 11.00000 0.05 0.75 Q11 1 0.9380 0.4021 0.2634 11.00000 0.05 0.73 Q12 1 0.2862 0.0234 0.1045 11.00000 0.05 0.73 Q13 1 0.3854 -0.0404 0.0836 11.00000 0.05 0.72 Q14 1 0.8176 0.4206 0.3519 11.00000 0.05 0.72 Q15 1 0.0178 0.4762 0.2629 11.00000 0.05 0.71 Q16 1 0.5000 -0.5000 0.5000 10.50000 0.05 0.71 Q17 1 0.3548 -0.2843 0.7907 11.00000 0.05 0.71 Q18 1 0.4783 0.3118 -0.1676 11.00000 0.05 0.69 Q19 1 0.1142 0.4601 0.4520 11.00000 0.05 0.68 Q20 1 0.1580 0.4592 0.1610 11.00000 0.05 0.68 ; _shelx_res_checksum 34645 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 C1 C 0.3680(7) 0.1019(7) 0.1023(7) 0.0084(16) Uani 1 1 d . U . C2 C 0.5902(7) 0.0698(7) 0.0601(7) 0.0082(16) Uani 1 1 d . U . C3 C 0.5013(7) -0.0821(6) 0.2335(6) 0.0047(15) Uani 1 1 d . U . C4 C 0.6546(7) -0.2692(6) 0.3797(7) 0.0076(15) Uani 1 1 d . U . H4A H 0.7159 -0.2877 0.3085 0.009 Uiso 1 1 calc R U . H4B H 0.6522 -0.3597 0.4492 0.009 Uiso 1 1 calc R U . C5 C 0.7148(7) -0.1981(7) 0.4210(7) 0.0103(16) Uani 1 1 d . . . C6 C 0.4096(7) -0.2548(7) 0.4199(7) 0.0100(16) Uani 1 1 d . U . H6A H 0.4381 -0.3555 0.4421 0.012 Uiso 1 1 calc R U . H6B H 0.3309 -0.2126 0.3724 0.012 Uiso 1 1 calc R U . C7 C 0.3679(8) -0.2287(7) 0.5412(7) 0.0127(17) Uani 1 1 d . U . C8 C 0.8245(7) 0.0537(7) 0.0423(7) 0.0069(16) Uani 1 1 d . . . H8A H 0.8928 0.0966 -0.0212 0.008 Uiso 1 1 calc R U . H8B H 0.8566 -0.0464 0.0616 0.008 Uiso 1 1 calc R U . C9 C 0.8152(7) 0.0731(7) 0.1598(7) 0.0081(16) Uani 1 1 d . U . C10 C 0.6869(7) 0.2264(6) -0.1325(6) 0.0064(15) Uani 1 1 d . . . H10A H 0.6260 0.2175 -0.1755 0.008 Uiso 1 1 calc R U . H10B H 0.7769 0.2171 -0.1825 0.008 Uiso 1 1 calc R U . C11 C 0.6357(7) 0.3695(7) -0.1356(7) 0.0078(16) Uani 1 1 d . . . C12 C 0.1254(7) 0.1490(7) 0.1631(7) 0.0112(17) Uani 1 1 d . . . H12A H 0.1249 0.0614 0.1646 0.013 Uiso 1 1 calc R U . H12B H 0.0426 0.2200 0.1282 0.013 Uiso 1 1 calc R U . C13 C 0.1168(7) 0.1300(7) 0.2960(7) 0.0106(17) Uani 1 1 d . . . C14 C 0.2281(7) 0.3269(6) -0.0232(7) 0.0086(16) Uani 1 1 d . U . H14A H 0.1310 0.3777 -0.0273 0.010 Uiso 1 1 calc R U . H14B H 0.2656 0.3175 -0.1039 0.010 Uiso 1 1 calc R U . C15 C 0.2998(7) 0.4118(7) -0.0075(7) 0.0106(17) Uani 1 1 d . . . N1 N 0.4696(6) 0.1463(5) 0.0209(5) 0.0080(14) Uani 1 1 d . . . N2 N 0.6147(6) -0.0457(5) 0.1657(5) 0.0066(13) Uani 1 1 d . . . N3 N 0.3754(6) -0.0135(5) 0.2064(5) 0.0069(13) Uani 1 1 d . U . N4 N 0.5195(6) -0.1970(5) 0.3414(5) 0.0073(13) Uani 1 1 d . U . N5 N 0.6991(6) 0.1115(5) -0.0112(5) 0.0078(13) Uani 1 1 d . . . N6 N 0.2408(6) 0.1890(5) 0.0779(5) 0.0067(13) Uani 1 1 d . U . O1 O 0.6572(5) -0.0807(5) 0.4214(5) 0.0105(11) Uani 1 1 d . . . O2 O 0.8340(5) -0.2609(5) 0.4522(5) 0.0144(12) Uani 1 1 d . . . O3 O 0.4300(5) -0.3138(5) 0.6327(5) 0.0179(13) Uani 1 1 d . . . O4 O 0.2736(5) -0.1219(5) 0.5379(5) 0.0172(13) Uani 1 1 d . . . O5 O 0.9001(5) -0.0127(5) 0.2344(5) 0.0150(12) Uani 1 1 d . . . O6 O 0.7257(5) 0.1747(5) 0.1771(5) 0.0125(12) Uani 1 1 d . . . O7 O 0.5812(5) 0.3904(5) -0.0383(5) 0.0106(12) Uani 1 1 d . . . O8 O 0.6386(5) 0.4709(4) -0.2413(5) 0.0132(12) Uani 1 1 d . . . O9 O 0.0363(5) 0.0648(5) 0.3784(5) 0.0112(12) Uani 1 1 d . . . O10 O 0.1856(5) 0.1762(4) 0.3290(5) 0.0114(12) Uani 1 1 d . . . O11 O 0.3209(5) 0.5141(5) -0.1081(5) 0.0127(12) Uani 1 1 d . . . O12 O 1.0822(5) -0.2466(5) 0.4743(5) 0.0167(13) Uani 1 1 d . . . O13 O 0.5437(5) -0.1591(4) 0.6985(5) 0.0124(12) Uani 1 1 d . . . O14 O 0.3300(5) 0.3800(4) 0.0978(5) 0.0121(12) Uani 1 1 d . . . O15 O 0.0027(13) 0.7222(12) 0.2069(12) 0.044(4) Uani 0.5 1 d . . P O16 O 0.1319(5) 0.5403(5) 0.4077(5) 0.0237(14) Uani 1 1 d . . . O17 O 0.8495(9) 0.3982(7) 0.2943(8) 0.083(3) Uani 1 1 d . . . O18 O 0.0505(8) 0.5192(9) 0.1762(9) 0.096(3) Uani 1 1 d . U . Tb1 Tb 0.87835(4) -0.06573(3) 0.44630(3) 0.00842(11) Uani 1 1 d . . . Tb2 Tb 0.47116(4) -0.35434(3) 0.82965(3) 0.00757(10) Uani 1 1 d . . . 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 C1 0.0093(18) 0.0082(18) 0.0087(18) -0.0043(11) -0.0009(10) -0.0026(10) C2 0.0086(18) 0.0087(18) 0.0079(18) -0.0036(11) -0.0016(10) -0.0025(10) C3 0.0050(17) 0.0052(17) 0.0052(17) -0.0025(11) -0.0013(10) -0.0018(10) C4 0.0069(18) 0.0073(18) 0.0082(18) -0.0020(11) -0.0012(10) -0.0028(10) C5 0.011(4) 0.014(4) 0.004(4) -0.001(3) 0.001(3) -0.007(3) C6 0.0102(19) 0.0103(18) 0.0095(19) -0.0041(11) -0.0011(10) -0.0029(10) C7 0.0126(19) 0.0121(19) 0.0134(19) -0.0048(11) -0.0014(10) -0.0041(11) C8 0.006(4) 0.006(3) 0.009(4) -0.003(3) 0.004(3) -0.005(3) C9 0.0080(18) 0.0078(18) 0.0083(18) -0.0029(11) -0.0007(10) -0.0027(10) C10 0.007(4) 0.009(4) 0.003(4) -0.002(3) -0.001(3) -0.004(3) C11 0.006(4) 0.012(4) 0.005(4) -0.004(3) -0.001(3) -0.002(3) C12 0.015(4) 0.014(4) 0.007(4) -0.004(3) -0.006(3) -0.004(3) C13 0.009(4) 0.007(4) 0.013(4) -0.007(3) 0.001(4) 0.002(3) C14 0.0086(18) 0.0083(18) 0.0088(18) -0.0031(11) -0.0014(10) -0.0023(10) C15 0.007(4) 0.007(4) 0.014(5) -0.002(3) 0.003(3) -0.005(3) N1 0.011(3) 0.008(3) 0.006(3) -0.003(3) -0.001(3) -0.003(3) N2 0.013(3) 0.004(3) 0.003(3) 0.000(2) -0.003(3) -0.004(3) N3 0.0067(16) 0.0064(15) 0.0064(16) -0.0023(10) 0.0001(10) -0.0014(10) N4 0.0069(16) 0.0070(15) 0.0079(16) -0.0025(10) -0.0012(10) -0.0025(10) N5 0.013(3) 0.003(3) 0.005(3) 0.001(3) -0.003(3) -0.003(2) N6 0.0061(16) 0.0072(15) 0.0071(16) -0.0017(10) -0.0015(10) -0.0032(10) O1 0.008(3) 0.012(3) 0.013(3) -0.005(2) -0.002(2) -0.003(2) O2 0.010(3) 0.015(3) 0.021(3) -0.006(2) -0.008(2) -0.004(2) O3 0.025(3) 0.014(3) 0.012(3) -0.004(2) -0.010(3) 0.001(2) O4 0.020(3) 0.016(3) 0.015(3) -0.008(2) -0.005(3) 0.000(2) O5 0.015(3) 0.020(3) 0.011(3) -0.004(2) -0.004(2) -0.007(2) O6 0.014(3) 0.012(3) 0.010(3) -0.004(2) 0.000(2) -0.004(2) O7 0.012(3) 0.010(3) 0.010(3) -0.005(2) 0.000(2) -0.002(2) O8 0.018(3) 0.009(3) 0.006(3) 0.001(2) 0.000(2) -0.001(2) O9 0.009(3) 0.017(3) 0.009(3) -0.006(2) 0.003(2) -0.007(2) O10 0.010(3) 0.010(3) 0.016(3) -0.007(2) -0.001(2) -0.004(2) O11 0.018(3) 0.010(3) 0.010(3) 0.001(2) -0.004(2) -0.009(2) O12 0.006(3) 0.015(3) 0.027(3) -0.007(3) -0.001(3) -0.002(2) O13 0.018(3) 0.010(2) 0.009(3) 0.000(2) -0.001(2) -0.008(2) O14 0.018(3) 0.011(3) 0.007(3) 0.000(2) -0.006(2) -0.005(2) O15 0.034(8) 0.041(8) 0.034(9) -0.005(7) 0.000(7) -0.003(6) O16 0.017(3) 0.016(3) 0.029(4) -0.008(3) 0.002(3) 0.001(2) O17 0.114(7) 0.066(5) 0.072(6) 0.029(5) -0.067(6) -0.062(5) O18 0.034(5) 0.113(6) 0.077(6) 0.005(5) -0.011(4) -0.004(4) Tb1 0.0088(2) 0.0089(2) 0.0085(2) -0.00332(17) -0.00114(17) -0.00370(17) Tb2 0.0100(2) 0.00714(19) 0.0051(2) -0.00156(16) -0.00128(17) -0.00279(16) 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 N3 C1 N1 127.9(6) . . N3 C1 N6 116.3(7) . . N1 C1 N6 115.7(6) . . N1 C2 N2 126.3(7) . . N1 C2 N5 117.8(6) . . N2 C2 N5 115.9(6) . . N3 C3 N4 117.6(6) . . N3 C3 N2 126.4(6) . . N4 C3 N2 115.9(6) . . N4 C4 C5 117.0(5) . . N4 C4 H4A 108.1 . . C5 C4 H4A 108.1 . . N4 C4 H4B 108.1 . . C5 C4 H4B 108.1 . . H4A C4 H4B 107.3 . . O1 C5 O2 119.6(6) . . O1 C5 C4 123.7(6) . . O2 C5 C4 116.6(6) . . O1 C5 Tb1 63.6(4) . . O2 C5 Tb1 57.1(3) . . C4 C5 Tb1 165.4(5) . . N4 C6 C7 111.3(6) . . N4 C6 H6A 109.4 . . C7 C6 H6A 109.4 . . N4 C6 H6B 109.4 . . C7 C6 H6B 109.4 . . H6A C6 H6B 108.0 . . O3 C7 O4 125.8(7) . . O3 C7 C6 117.8(6) . . O4 C7 C6 116.5(6) . . N5 C8 C9 114.4(6) . . N5 C8 H8A 108.7 . . C9 C8 H8A 108.7 . . N5 C8 H8B 108.7 . . C9 C8 H8B 108.7 . . H8A C8 H8B 107.6 . . O5 C9 O6 123.6(7) . . O5 C9 C8 117.1(6) . . O6 C9 C8 119.3(6) . . N5 C10 C11 117.7(6) . . N5 C10 H10A 107.9 . . C11 C10 H10A 107.9 . . N5 C10 H10B 107.9 . . C11 C10 H10B 107.9 . . H10A C10 H10B 107.2 . . O7 C11 O8 120.1(6) . . O7 C11 C10 121.3(6) . . O8 C11 C10 118.3(6) . . O7 C11 Tb2 63.3(3) . 1_564 O8 C11 Tb2 58.2(3) . 1_564 C10 C11 Tb2 162.7(5) . 1_564 N6 C12 C13 117.0(6) . . N6 C12 H12A 108.0 . . C13 C12 H12A 108.0 . . N6 C12 H12B 108.0 . . C13 C12 H12B 108.0 . . H12A C12 H12B 107.3 . . O10 C13 O9 119.1(7) . . O10 C13 C12 123.0(7) . . O9 C13 C12 117.9(6) . . O10 C13 Tb1 57.7(4) . 2_656 O9 C13 Tb1 61.8(4) . 2_656 C12 C13 Tb1 173.9(5) . 2_656 N6 C14 C15 113.8(6) . . N6 C14 H14A 108.8 . . C15 C14 H14A 108.8 . . N6 C14 H14B 108.8 . . C15 C14 H14B 108.8 . . H14A C14 H14B 107.7 . . O14 C15 O11 125.9(6) . . O14 C15 C14 120.1(6) . . O11 C15 C14 114.0(6) . . C1 N1 C2 113.0(6) . . C2 N2 C3 113.2(6) . . C3 N3 C1 112.8(6) . . C3 N4 C6 122.5(6) . . C3 N4 C4 119.4(6) . . C6 N4 C4 118.0(5) . . C2 N5 C8 119.0(6) . . C2 N5 C10 120.8(6) . . C8 N5 C10 119.5(6) . . C1 N6 C12 119.0(6) . . C1 N6 C14 118.5(6) . . C12 N6 C14 122.0(5) . . C5 O1 Tb1 90.3(4) . . C5 O2 Tb1 96.3(4) . . C7 O3 Tb2 144.5(5) . . C7 O4 Tb1 171.3(5) . 2_656 C9 O5 Tb1 126.8(5) . . C9 O6 Tb2 162.8(5) . 2_656 C11 O7 Tb2 160.4(4) . 2_656 C11 O7 Tb2 90.9(4) . 1_564 Tb2 O7 Tb2 108.38(18) 2_656 1_564 C11 O8 Tb2 95.7(4) . 1_564 C13 O9 Tb1 152.9(5) . 1_455 C13 O9 Tb1 91.9(4) . 2_656 Tb1 O9 Tb1 114.6(2) 1_455 2_656 C13 O10 Tb1 96.2(4) . 2_656 C15 O11 Tb2 132.6(4) . 1_564 C15 O14 Tb2 134.0(5) . 2_656 O4 Tb1 O5 102.30(18) 2_656 . O4 Tb1 O12 157.50(18) 2_656 . O5 Tb1 O12 92.62(18) . . O4 Tb1 O9 85.09(18) 2_656 1_655 O5 Tb1 O9 82.57(17) . 1_655 O12 Tb1 O9 80.20(16) . 1_655 O4 Tb1 O2 126.68(18) 2_656 . O5 Tb1 O2 79.29(17) . . O12 Tb1 O2 72.29(16) . . O9 Tb1 O2 146.07(17) 1_655 . O4 Tb1 O10 84.62(17) 2_656 2_656 O5 Tb1 O10 159.36(16) . 2_656 O12 Tb1 O10 87.23(17) . 2_656 O9 Tb1 O10 117.65(16) 1_655 2_656 O2 Tb1 O10 81.02(16) . 2_656 O4 Tb1 O9 81.32(16) 2_656 2_656 O5 Tb1 O9 147.46(17) . 2_656 O12 Tb1 O9 77.12(17) . 2_656 O9 Tb1 O9 65.4(2) 1_655 2_656 O2 Tb1 O9 124.72(16) . 2_656 O10 Tb1 O9 52.28(15) 2_656 2_656 O4 Tb1 O1 75.62(16) 2_656 . O5 Tb1 O1 77.25(17) . . O12 Tb1 O1 124.68(16) . . O9 Tb1 O1 148.18(15) 1_655 . O2 Tb1 O1 52.40(15) . . O10 Tb1 O1 85.86(16) 2_656 . O9 Tb1 O1 133.86(16) 2_656 . O4 Tb1 C5 101.65(19) 2_656 . O5 Tb1 C5 73.94(19) . . O12 Tb1 C5 98.59(18) . . O9 Tb1 C5 156.43(19) 1_655 . O2 Tb1 C5 26.55(17) . . O10 Tb1 C5 85.66(18) 2_656 . O9 Tb1 C5 137.65(18) 2_656 . O1 Tb1 C5 26.16(17) . . O4 Tb1 C13 80.36(18) 2_656 2_656 O5 Tb1 C13 173.30(19) . 2_656 O12 Tb1 C13 83.11(19) . 2_656 O9 Tb1 C13 91.6(2) 1_655 2_656 O2 Tb1 C13 104.17(19) . 2_656 O10 Tb1 C13 26.08(18) 2_656 2_656 O9 Tb1 C13 26.32(18) 2_656 2_656 O1 Tb1 C13 109.43(19) . 2_656 C5 Tb1 C13 111.7(2) . 2_656 O7 Tb2 O13 115.31(16) 2_656 . O7 Tb2 O6 79.14(17) 2_656 2_656 O13 Tb2 O6 77.23(17) . 2_656 O7 Tb2 O11 80.43(17) 2_656 1_546 O13 Tb2 O11 151.84(16) . 1_546 O6 Tb2 O11 83.61(17) 2_656 1_546 O7 Tb2 O3 156.17(18) 2_656 . O13 Tb2 O3 77.65(17) . . O6 Tb2 O3 84.91(17) 2_656 . O11 Tb2 O3 80.29(18) 1_546 . O7 Tb2 O14 72.29(17) 2_656 2_656 O13 Tb2 O14 72.80(16) . 2_656 O6 Tb2 O14 123.39(16) 2_656 2_656 O11 Tb2 O14 135.37(16) 1_546 2_656 O3 Tb2 O14 131.54(19) . 2_656 O7 Tb2 O8 122.23(15) 2_656 1_546 O13 Tb2 O8 101.36(17) . 1_546 O6 Tb2 O8 155.08(16) 2_656 1_546 O11 Tb2 O8 87.46(17) 1_546 1_546 O3 Tb2 O8 70.64(16) . 1_546 O14 Tb2 O8 78.55(16) 2_656 1_546 O7 Tb2 O7 71.62(18) 2_656 1_546 O13 Tb2 O7 136.64(16) . 1_546 O6 Tb2 O7 142.50(17) 2_656 1_546 O11 Tb2 O7 69.02(16) 1_546 1_546 O3 Tb2 O7 113.74(16) . 1_546 O14 Tb2 O7 69.16(15) 2_656 1_546 O8 Tb2 O7 51.49(16) 1_546 1_546 O7 Tb2 C11 97.38(19) 2_656 1_546 O13 Tb2 C11 123.21(19) . 1_546 O6 Tb2 C11 157.64(19) 2_656 1_546 O11 Tb2 C11 74.04(18) 1_546 1_546 O3 Tb2 C11 90.64(18) . 1_546 O14 Tb2 C11 75.23(17) 2_656 1_546 O8 Tb2 C11 26.07(18) 1_546 1_546 O7 Tb2 C11 25.80(17) 1_546 1_546 O7 Tb2 Tb2 38.08(11) 2_656 2_647 O13 Tb2 Tb2 136.17(11) . 2_647 O6 Tb2 Tb2 113.95(13) 2_656 2_647 O11 Tb2 Tb2 70.76(11) 1_546 2_647 O3 Tb2 Tb2 142.58(12) . 2_647 O14 Tb2 Tb2 65.90(11) 2_656 2_647 O8 Tb2 Tb2 84.60(11) 1_546 2_647 O7 Tb2 Tb2 33.54(11) 1_546 2_647 C11 Tb2 Tb2 59.32(14) 1_546 2_647 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N3 1.331(8) . C1 N1 1.334(9) . C1 N6 1.374(8) . C2 N1 1.334(8) . C2 N2 1.346(8) . C2 N5 1.348(9) . C3 N3 1.330(8) . C3 N4 1.353(8) . C3 N2 1.358(9) . C4 N4 1.458(8) . C4 C5 1.496(9) . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 O1 1.251(8) . C5 O2 1.276(8) . C5 Tb1 2.837(7) . C6 N4 1.453(9) . C6 C7 1.547(10) . C6 H6A 0.9900 . C6 H6B 0.9900 . C7 O3 1.242(8) . C7 O4 1.256(8) . C8 N5 1.443(8) . C8 C9 1.507(9) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 O5 1.255(8) . C9 O6 1.267(8) . C10 N5 1.447(8) . C10 C11 1.501(9) . C10 H10A 0.9900 . C10 H10B 0.9900 . C11 O7 1.253(8) . C11 O8 1.271(8) . C11 Tb2 2.878(7) 1_564 C12 N6 1.448(9) . C12 C13 1.501(10) . C12 H12A 0.9900 . C12 H12B 0.9900 . C13 O10 1.267(8) . C13 O9 1.271(9) . C13 Tb1 2.865(8) 2_656 C14 N6 1.464(8) . C14 C15 1.530(9) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 O14 1.252(8) . C15 O11 1.276(8) . O1 Tb1 2.540(5) . O2 Tb1 2.397(4) . O3 Tb2 2.340(5) . O4 Tb1 2.217(5) 2_656 O5 Tb1 2.312(5) . O6 Tb2 2.329(5) 2_656 O7 Tb2 2.304(5) 2_656 O7 Tb2 2.572(4) 1_564 O8 Tb2 2.459(5) 1_564 O9 Tb1 2.388(5) 1_455 O9 Tb1 2.526(5) 2_656 O10 Tb1 2.435(5) 2_656 O11 Tb2 2.337(5) 1_564 O12 Tb1 2.365(5) . O13 Tb2 2.325(5) . O14 Tb2 2.387(5) 2_656 Tb1 O4 2.217(5) 2_656 Tb1 O9 2.388(5) 1_655 Tb1 O10 2.435(5) 2_656 Tb1 O9 2.526(5) 2_656 Tb1 C13 2.865(8) 2_656 Tb2 O7 2.304(5) 2_656 Tb2 O6 2.329(5) 2_656 Tb2 O11 2.337(5) 1_546 Tb2 O14 2.387(5) 2_656 Tb2 O8 2.459(5) 1_546 Tb2 O7 2.572(4) 1_546 Tb2 C11 2.878(7) 1_546 Tb2 Tb2 3.9569(7) 2_647 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_4 N4 C4 C5 O1 -1.8(11) . . N4 C4 C5 O2 -178.8(6) . . N4 C4 C5 Tb1 -117.8(17) . . N4 C6 C7 O3 -86.9(8) . . N4 C6 C7 O4 92.9(8) . . N5 C8 C9 O5 154.7(6) . . N5 C8 C9 O6 -26.7(9) . . N5 C10 C11 O7 -13.5(10) . . N5 C10 C11 O8 172.3(6) . . N5 C10 C11 Tb2 -114.1(16) . 1_564 N6 C12 C13 O10 16.5(10) . . N6 C12 C13 O9 -163.7(6) . . N6 C14 C15 O14 -19.3(9) . . N6 C14 C15 O11 162.0(6) . . N3 C1 N1 C2 -7.8(10) . . N6 C1 N1 C2 169.4(6) . . N2 C2 N1 C1 3.8(10) . . N5 C2 N1 C1 -175.5(6) . . N1 C2 N2 C3 0.6(10) . . N5 C2 N2 C3 179.9(6) . . N3 C3 N2 C2 -2.2(9) . . N4 C3 N2 C2 -179.5(6) . . N4 C3 N3 C1 176.4(6) . . N2 C3 N3 C1 -0.9(10) . . N1 C1 N3 C3 6.5(10) . . N6 C1 N3 C3 -170.7(6) . . N3 C3 N4 C6 6.8(9) . . N2 C3 N4 C6 -175.6(6) . . N3 C3 N4 C4 -175.2(5) . . N2 C3 N4 C4 2.4(9) . . C7 C6 N4 C3 -107.1(7) . . C7 C6 N4 C4 74.9(7) . . C5 C4 N4 C3 69.8(8) . . C5 C4 N4 C6 -112.1(7) . . N1 C2 N5 C8 164.3(6) . . N2 C2 N5 C8 -15.0(9) . . N1 C2 N5 C10 -6.6(9) . . N2 C2 N5 C10 174.0(6) . . C9 C8 N5 C2 -57.0(8) . . C9 C8 N5 C10 114.1(7) . . C11 C10 N5 C2 80.2(8) . . C11 C10 N5 C8 -90.7(8) . . N3 C1 N6 C12 -1.5(9) . . N1 C1 N6 C12 -179.0(6) . . N3 C1 N6 C14 170.0(6) . . N1 C1 N6 C14 -7.5(9) . . C13 C12 N6 C1 61.7(8) . . C13 C12 N6 C14 -109.5(7) . . C15 C14 N6 C1 -56.7(8) . . C15 C14 N6 C12 114.5(7) . . O2 C5 O1 Tb1 11.6(7) . . C4 C5 O1 Tb1 -165.4(7) . . O1 C5 O2 Tb1 -12.3(7) . . C4 C5 O2 Tb1 164.8(5) . . O4 C7 O3 Tb2 -13.1(14) . . C6 C7 O3 Tb2 166.6(6) . . O6 C9 O5 Tb1 24.3(10) . . C8 C9 O5 Tb1 -157.3(5) . . O5 C9 O6 Tb2 -155.3(12) . 2_656 C8 C9 O6 Tb2 26(2) . 2_656 O8 C11 O7 Tb2 -157.6(10) . 2_656 C10 C11 O7 Tb2 28.3(18) . 2_656 Tb2 C11 O7 Tb2 -170.7(14) 1_564 2_656 O8 C11 O7 Tb2 13.1(6) . 1_564 C10 C11 O7 Tb2 -160.9(6) . 1_564 O7 C11 O8 Tb2 -13.8(7) . 1_564 C10 C11 O8 Tb2 160.4(5) . 1_564 O10 C13 O9 Tb1 -175.8(6) . 1_455 C12 C13 O9 Tb1 4.4(14) . 1_455 Tb1 C13 O9 Tb1 -168.6(10) 2_656 1_455 O10 C13 O9 Tb1 -7.1(6) . 2_656 C12 C13 O9 Tb1 173.1(5) . 2_656 O9 C13 O10 Tb1 7.4(7) . 2_656 C12 C13 O10 Tb1 -172.8(6) . 2_656 O14 C15 O11 Tb2 21.6(11) . 1_564 C14 C15 O11 Tb2 -159.8(4) . 1_564 O11 C15 O14 Tb2 -48.0(10) . 2_656 C14 C15 O14 Tb2 133.5(6) . 2_656