#------------------------------------------------------------------------------ #$Date: 2018-03-17 08:06:32 +0200 (Sat, 17 Mar 2018) $ #$Revision: 207002 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/03/7230306.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_7230306 loop_ _publ_author_name 'Goel, Nidhi' 'Kumar, Naresh' _publ_section_title ; A dual-functional luminescent Tb(iii) metal--organic framework for the selective sensing of acetone and TNP in water ; _journal_issue 20 _journal_name_full 'RSC Advances' _journal_page_first 10746 _journal_paper_doi 10.1039/C7RA13494K _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C23 H18 N5 O8 Tb, C3 H7 N O' _chemical_formula_sum 'C26 H25 N6 O9 Tb' _chemical_formula_weight 724.45 _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_creation_method SHELXL-2014/7 _audit_update_record ; 2017-10-26 deposited with the CCDC. 2018-02-23 downloaded from the CCDC. ; _cell_angle_alpha 109.254(2) _cell_angle_beta 100.428(2) _cell_angle_gamma 108.162(2) _cell_formula_units_Z 2 _cell_length_a 10.4848(4) _cell_length_b 10.6394(4) _cell_length_c 13.7737(5) _cell_measurement_reflns_used 90 _cell_measurement_temperature 105(2) _cell_measurement_theta_max 28.315 _cell_measurement_theta_min 2.145 _cell_volume 1307.48(9) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 105(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 Venture CMOS diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_unetI/netI 0.0420 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 50672 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.315 _diffrn_reflns_theta_min 2.145 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2014)' _exptl_crystal_colour Yellow-orange _exptl_crystal_density_diffrn 1.840 _exptl_crystal_description Concave _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max 0.779 _exptl_transmission_factor_min 0.678 _refine_diff_density_max 1.904 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.146 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.779 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 383 _refine_ls_number_reflns 6491 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.779 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0320 _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^)+(0.1000P)^2^+0.5808P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.0994 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5654 _reflns_number_total 6491 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ra13494k2.cif _cod_data_source_block TPA-MOF _cod_database_code 7230306 _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_estimated_absorpt_t_min 0.677 _shelx_estimated_absorpt_t_max 0.778 _shelx_res_file ; DD05_0m_a.res created by SHELXL-2014/7 TITL DD05_0m_a.res in P-1 CELL 0.71073 10.4848 10.6394 13.7737 109.254 100.428 108.162 ZERR 15.000 0.0004 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O Tb UNIT 15 15 15 15 15 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 HTAB C25 O8_$7 HTAB C25 O6_$6 HTAB C25 O4_$6 HTAB C23 O8_$5 HTAB C22 O3_$5 HTAB C22 O9_$4 HTAB C21 O9_$4 HTAB C10 O2 HTAB C9 O4_$3 HTAB C2 O3_$2 HTAB C1 O7_$1 CONF HTAB EQIV $1 -x+1, -y, -z HTAB C1 O7_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C2 O3_$2 EQIV $3 -x+1, -y+1, -z HTAB C9 O4_$3 HTAB C10 O2 EQIV $4 -x+2, -y+1, -z+1 HTAB C21 O9_$4 HTAB C22 O9_$4 EQIV $5 x+1, y, z HTAB C22 O3_$5 HTAB C23 O8_$5 EQIV $6 -x+1, -y, -z+1 HTAB C25 O4_$6 HTAB C25 O6_$6 EQIV $7 x+1, y, z+1 HTAB C25 O8_$7 HTAB C1 O7_$1 HTAB C2 O3_$2 HTAB C9 O4_$3 HTAB C10 O2 HTAB C21 O9_$4 HTAB C22 O9_$4 HTAB C22 O3_$5 HTAB C23 O8_$5 HTAB C25 O4_$6 HTAB C25 O6_$6 HTAB C25 O8_$7 HTAB C1 O7_$1 HTAB C2 O3_$2 HTAB C9 O4_$3 HTAB C10 O2 HTAB C21 O9_$4 HTAB C22 O9_$4 HTAB C22 O3_$5 HTAB C23 O8_$5 HTAB C25 O4_$6 HTAB C25 O6_$6 HTAB C25 O8_$7 HTAB CONF TEMP -168.260 WGHT 0.100000 0.580830 FVAR 0.34885 TB1 5 0.580895 0.434690 0.179352 11.00000 0.01959 0.00491 = 0.00608 0.00356 0.00491 0.00485 O1 4 0.593995 0.366534 0.007171 11.00000 0.03089 0.01194 = 0.00748 0.00602 0.01044 0.01224 O2 4 0.552207 0.449661 -0.117961 11.00000 0.02186 0.00865 = 0.01210 0.00608 0.00706 0.00836 O3 4 0.379467 0.436143 0.264420 11.00000 0.02293 0.01878 = 0.01484 0.01008 0.00743 0.00936 O4 4 0.329654 0.262992 0.108538 11.00000 0.02594 0.01415 = 0.01482 0.00518 0.00392 0.00476 O5 4 0.816101 0.456175 0.235029 11.00000 0.02076 0.01471 = 0.02477 0.00719 0.00484 0.00724 O6 4 0.435564 -0.181459 -0.124878 11.00000 0.03003 0.00937 = 0.00906 0.00552 0.00969 0.00885 O7 4 0.428113 -0.302274 -0.291177 11.00000 0.03169 0.00918 = 0.01057 0.00599 0.00954 0.01063 O8 4 0.165348 0.270596 0.184145 11.00000 0.01697 0.06204 = 0.04043 0.01502 0.00803 0.00318 O9 4 0.859140 0.171093 0.775766 11.00000 0.03619 0.03217 = 0.02036 0.00914 0.00862 0.01521 N1 3 0.678003 0.631138 0.371054 11.00000 0.01800 0.00924 = 0.01238 0.00482 0.00552 0.00556 N2 3 0.744076 0.691537 0.204745 11.00000 0.01784 0.00997 = 0.01273 0.00654 0.00500 0.00481 N3 3 0.288037 0.322484 0.184894 11.00000 0.01850 0.02803 = 0.01696 0.01384 0.00470 0.00562 N4 3 0.517370 0.061460 -0.463833 11.00000 0.02059 0.01167 = 0.00825 0.00630 0.00708 0.00792 N5 3 1.040675 0.523911 0.335243 11.00000 0.01859 0.01505 = 0.02656 0.00755 0.00571 0.00655 N6 3 0.859021 0.187931 0.945966 11.00000 0.02271 0.02008 = 0.02634 0.00846 0.00620 0.00655 C1 1 0.647860 0.602967 0.453123 11.00000 0.02222 0.01082 = 0.01504 0.00714 0.00540 0.00479 AFIX 43 H1 2 0.600818 0.504391 0.440889 11.00000 -1.20000 AFIX 0 C2 1 0.681576 0.710508 0.556680 11.00000 0.02450 0.02175 = 0.01364 0.01079 0.00849 0.01133 AFIX 43 H2 2 0.658335 0.684581 0.612904 11.00000 -1.20000 AFIX 0 C3 1 0.748188 0.853043 0.576136 11.00000 0.02268 0.01617 = 0.01145 -0.00104 0.00337 0.00801 AFIX 43 H3 2 0.770600 0.927829 0.645532 11.00000 -1.20000 AFIX 0 C4 1 0.783094 0.886994 0.490906 11.00000 0.02052 0.01215 = 0.01348 0.00504 0.00417 0.00828 C5 1 0.851179 1.034827 0.505307 11.00000 0.02467 0.00770 = 0.01546 0.00064 0.00371 0.00693 AFIX 43 H5 2 0.873533 1.112136 0.573395 11.00000 -1.20000 AFIX 0 C6 1 0.883485 1.064336 0.422647 11.00000 0.02571 0.00711 = 0.02245 0.00390 0.00323 0.00362 AFIX 43 H6 2 0.928680 1.162587 0.433449 11.00000 -1.20000 AFIX 0 C7 1 0.850998 0.950483 0.318944 11.00000 0.02052 0.01152 = 0.01517 0.00516 0.00666 0.00653 C8 1 0.882410 0.977510 0.230979 11.00000 0.02599 0.00951 = 0.02039 0.00834 0.00278 0.00095 AFIX 43 H8 2 0.928927 1.074228 0.238899 11.00000 -1.20000 AFIX 0 C9 1 0.845199 0.862945 0.133980 11.00000 0.02588 0.01658 = 0.01735 0.01041 0.00811 0.00535 AFIX 43 H9 2 0.866671 0.879112 0.073890 11.00000 -1.20000 AFIX 0 C10 1 0.775348 0.721865 0.123828 11.00000 0.01943 0.01490 = 0.01245 0.00570 0.00174 0.00520 AFIX 43 H10 2 0.748854 0.643550 0.055414 11.00000 -1.20000 AFIX 0 C11 1 0.747145 0.772743 0.389659 11.00000 0.01762 0.01334 = 0.01197 0.00581 0.00383 0.00604 C12 1 0.783017 0.805052 0.301855 11.00000 0.01791 0.00960 = 0.01290 0.00531 0.00491 0.00717 C13 1 0.560062 0.351123 -0.089868 11.00000 0.01484 0.00469 = 0.00942 0.00047 0.00596 0.00438 C14 1 0.530501 0.205976 -0.176834 11.00000 0.01308 0.00759 = 0.01122 0.00372 0.00448 0.00664 C15 1 0.498548 0.081650 -0.154889 11.00000 0.01565 0.01183 = 0.00738 0.00599 0.00500 0.00749 AFIX 43 H15 2 0.496306 0.088609 -0.084710 11.00000 -1.20000 AFIX 0 C16 1 0.470169 -0.052017 -0.237161 11.00000 0.01600 0.00873 = 0.00917 0.00651 0.00471 0.00609 C17 1 0.474493 -0.063082 -0.340380 11.00000 0.01843 0.00870 = 0.00784 0.00399 0.00468 0.00825 AFIX 43 H17 2 0.455741 -0.154327 -0.395868 11.00000 -1.20000 AFIX 0 C18 1 0.506448 0.060485 -0.361174 11.00000 0.01485 0.01426 = 0.00864 0.00540 0.00653 0.00735 C19 1 0.533236 0.193915 -0.280062 11.00000 0.01873 0.00878 = 0.01197 0.00647 0.00441 0.00706 AFIX 43 H19 2 0.553585 0.277572 -0.295280 11.00000 -1.20000 AFIX 0 C20 1 0.441815 -0.186169 -0.216192 11.00000 0.01334 0.00826 = 0.01091 0.00528 0.00541 0.00426 C21 1 0.942518 0.541311 0.273700 11.00000 0.03030 0.01381 = 0.02137 0.00636 0.01130 0.00876 AFIX 43 H21 2 0.969892 0.624253 0.257728 11.00000 -1.20000 AFIX 0 C22 1 1.189530 0.622882 0.374638 11.00000 0.01991 0.01862 = 0.05732 0.00361 0.00543 0.00294 AFIX 137 H22A 2 1.203988 0.685436 0.335474 11.00000 -1.50000 H22B 2 1.247918 0.566621 0.362555 11.00000 -1.50000 H22C 2 1.216611 0.683029 0.452332 11.00000 -1.50000 AFIX 0 C23 1 1.007567 0.398216 0.361459 11.00000 0.03851 0.02568 = 0.03657 0.01869 0.00855 0.01531 AFIX 137 H23A 2 0.904803 0.343377 0.335691 11.00000 -1.50000 H23B 2 1.043177 0.430590 0.440169 11.00000 -1.50000 H23C 2 1.052405 0.335954 0.326187 11.00000 -1.50000 AFIX 0 C24 1 0.829151 0.115809 0.842154 11.00000 0.02788 0.03715 = 0.03927 0.00748 0.01237 0.01087 AFIX 43 H24 2 0.780878 0.013214 0.813451 11.00000 -1.20000 AFIX 0 C25 1 0.816671 0.116997 1.016084 11.00000 0.04315 0.04661 = 0.03866 0.02076 0.01090 0.01203 AFIX 137 H25A 2 0.776003 0.011370 0.974727 11.00000 -1.50000 H25B 2 0.745967 0.146748 1.043436 11.00000 -1.50000 H25C 2 0.899581 0.145203 1.077212 11.00000 -1.50000 AFIX 0 C26 1 0.927450 0.344409 0.996889 11.00000 0.05371 0.03524 = 0.03849 0.00999 0.01578 0.01200 AFIX 137 H26A 2 0.945705 0.381279 0.942113 11.00000 -1.50000 H26B 2 1.017210 0.374454 1.052187 11.00000 -1.50000 H26C 2 0.865916 0.383786 1.030958 11.00000 -1.50000 AFIX 0 HKLF 4 REM DD05_0m_a.res in P-1 REM R1 = 0.0320 for 5654 Fo > 4sig(Fo) and 0.0432 for all 6491 data REM 383 parameters refined using 0 restraints END WGHT 0.0375 2.3410 REM Instructions for potential hydrogen bonds HTAB C1 O7_$1 HTAB C2 O3_$2 HTAB C9 O4_$3 HTAB C10 O2 HTAB C21 O9_$4 HTAB C22 O9_$4 HTAB C22 O3_$5 HTAB C23 O8_$5 HTAB C25 O4_$6 HTAB C25 O6_$6 HTAB C25 O8_$7 REM Highest difference peak 1.904, deepest hole -0.957, 1-sigma level 0.146 Q1 1 0.8767 0.2425 0.8603 11.00000 0.05 1.90 Q2 1 0.8726 0.2803 1.0460 11.00000 0.05 1.80 Q3 1 0.4930 0.4213 0.1636 11.00000 0.05 1.67 Q4 1 0.8416 0.0422 0.9174 11.00000 0.05 1.64 Q5 1 0.6778 0.4579 0.1991 11.00000 0.05 1.42 ; _shelx_res_checksum 853 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 Tb1 Tb 0.58090(2) 0.43469(2) 0.17935(2) 0.00971(7) Uani 1 1 d . . O1 O 0.5940(3) 0.3665(3) 0.0072(2) 0.0146(6) Uani 1 1 d . . O2 O 0.5522(3) 0.4497(3) -0.1180(2) 0.0128(5) Uani 1 1 d . . O3 O 0.3795(3) 0.4361(3) 0.2644(2) 0.0175(6) Uani 1 1 d . . O4 O 0.3297(3) 0.2630(3) 0.1085(2) 0.0198(6) Uani 1 1 d . . O5 O 0.8161(3) 0.4562(3) 0.2350(2) 0.0207(6) Uani 1 1 d . . O6 O 0.4356(3) -0.1815(3) -0.1249(2) 0.0149(6) Uani 1 1 d . . O7 O 0.4281(3) -0.3023(3) -0.2912(2) 0.0155(6) Uani 1 1 d . . O8 O 0.1653(4) 0.2706(5) 0.1841(3) 0.0451(10) Uani 1 1 d . . O9 O 0.8591(4) 0.1711(4) 0.7758(3) 0.0297(7) Uani 1 1 d . . N1 N 0.6780(3) 0.6311(3) 0.3711(3) 0.0130(6) Uani 1 1 d . . N2 N 0.7441(3) 0.6915(3) 0.2047(3) 0.0132(6) Uani 1 1 d . . N3 N 0.2880(4) 0.3225(4) 0.1849(3) 0.0210(7) Uani 1 1 d . . N4 N 0.5174(3) 0.0615(3) -0.4638(2) 0.0121(6) Uani 1 1 d . . N5 N 1.0407(4) 0.5239(4) 0.3352(3) 0.0206(7) Uani 1 1 d . . N6 N 0.8590(4) 0.1879(4) 0.9460(3) 0.0241(8) Uani 1 1 d . . C1 C 0.6479(4) 0.6030(4) 0.4531(3) 0.0161(8) Uani 1 1 d . . H1 H 0.6008 0.5044 0.4409 0.019 Uiso 1 1 calc R U C2 C 0.6816(4) 0.7105(5) 0.5567(3) 0.0181(8) Uani 1 1 d . . H2 H 0.6583 0.6846 0.6129 0.022 Uiso 1 1 calc R U C3 C 0.7482(4) 0.8530(5) 0.5761(3) 0.0189(8) Uani 1 1 d . . H3 H 0.7706 0.9278 0.6455 0.023 Uiso 1 1 calc R U C4 C 0.7831(4) 0.8870(4) 0.4909(3) 0.0152(8) Uani 1 1 d . . C5 C 0.8512(4) 1.0348(4) 0.5053(3) 0.0174(8) Uani 1 1 d . . H5 H 0.8735 1.1121 0.5734 0.021 Uiso 1 1 calc R U C6 C 0.8835(5) 1.0643(4) 0.4226(3) 0.0205(9) Uani 1 1 d . . H6 H 0.9287 1.1626 0.4334 0.025 Uiso 1 1 calc R U C7 C 0.8510(4) 0.9505(4) 0.3189(3) 0.0157(8) Uani 1 1 d . . C8 C 0.8824(5) 0.9775(4) 0.2310(3) 0.0203(9) Uani 1 1 d . . H8 H 0.9289 1.0742 0.2389 0.024 Uiso 1 1 calc R U C9 C 0.8452(4) 0.8629(4) 0.1340(3) 0.0196(8) Uani 1 1 d . . H9 H 0.8667 0.8791 0.0739 0.024 Uiso 1 1 calc R U C10 C 0.7753(4) 0.7219(4) 0.1238(3) 0.0165(8) Uani 1 1 d . . H10 H 0.7489 0.6436 0.0554 0.020 Uiso 1 1 calc R U C11 C 0.7471(4) 0.7727(4) 0.3897(3) 0.0143(7) Uani 1 1 d . . C12 C 0.7830(4) 0.8051(4) 0.3019(3) 0.0128(7) Uani 1 1 d . . C13 C 0.5601(4) 0.3511(4) -0.0899(3) 0.0099(7) Uani 1 1 d . . C14 C 0.5305(4) 0.2060(4) -0.1768(3) 0.0099(7) Uani 1 1 d . . C15 C 0.4985(4) 0.0816(4) -0.1549(3) 0.0103(7) Uani 1 1 d . . H15 H 0.4963 0.0886 -0.0847 0.012 Uiso 1 1 calc R U C16 C 0.4702(4) -0.0520(4) -0.2372(3) 0.0101(7) Uani 1 1 d . . C17 C 0.4745(4) -0.0631(4) -0.3404(3) 0.0107(7) Uani 1 1 d . . H17 H 0.4557 -0.1543 -0.3959 0.013 Uiso 1 1 calc R U C18 C 0.5064(4) 0.0605(4) -0.3612(3) 0.0116(7) Uani 1 1 d . . C19 C 0.5332(4) 0.1939(4) -0.2801(3) 0.0122(7) Uani 1 1 d . . H19 H 0.5536 0.2776 -0.2953 0.015 Uiso 1 1 calc R U C20 C 0.4418(4) -0.1862(4) -0.2162(3) 0.0102(7) Uani 1 1 d . . C21 C 0.9425(5) 0.5413(5) 0.2737(3) 0.0216(9) Uani 1 1 d . . H21 H 0.9699 0.6243 0.2577 0.026 Uiso 1 1 calc R U C22 C 1.1895(5) 0.6229(5) 0.3746(5) 0.0377(13) Uani 1 1 d . . H22A H 1.2040 0.6854 0.3355 0.056 Uiso 1 1 calc R U H22B H 1.2479 0.5666 0.3626 0.056 Uiso 1 1 calc R U H22C H 1.2166 0.6830 0.4523 0.056 Uiso 1 1 calc R U C23 C 1.0076(6) 0.3982(5) 0.3615(4) 0.0318(11) Uani 1 1 d . . H23A H 0.9048 0.3434 0.3357 0.048 Uiso 1 1 calc R U H23B H 1.0432 0.4306 0.4402 0.048 Uiso 1 1 calc R U H23C H 1.0524 0.3360 0.3262 0.048 Uiso 1 1 calc R U C24 C 0.8292(5) 0.1158(6) 0.8422(5) 0.0374(12) Uani 1 1 d . . H24 H 0.7809 0.0132 0.8135 0.045 Uiso 1 1 calc R U C25 C 0.8167(6) 0.1170(7) 1.0161(5) 0.0438(14) Uani 1 1 d . . H25A H 0.7760 0.0114 0.9747 0.066 Uiso 1 1 calc R U H25B H 0.7460 0.1467 1.0434 0.066 Uiso 1 1 calc R U H25C H 0.8996 0.1452 1.0772 0.066 Uiso 1 1 calc R U C26 C 0.9274(7) 0.3444(6) 0.9969(5) 0.0453(14) Uani 1 1 d . . H26A H 0.9457 0.3813 0.9421 0.068 Uiso 1 1 calc R U H26B H 1.0172 0.3745 1.0522 0.068 Uiso 1 1 calc R U H26C H 0.8659 0.3838 1.0310 0.068 Uiso 1 1 calc R U 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 0.01959(11) 0.00491(10) 0.00608(10) 0.00356(7) 0.00491(7) 0.00485(7) O1 0.0309(16) 0.0119(13) 0.0075(12) 0.0060(10) 0.0104(11) 0.0122(12) O2 0.0219(14) 0.0086(12) 0.0121(12) 0.0061(10) 0.0071(11) 0.0084(11) O3 0.0229(15) 0.0188(14) 0.0148(14) 0.0101(12) 0.0074(12) 0.0094(12) O4 0.0259(16) 0.0141(14) 0.0148(14) 0.0052(11) 0.0039(12) 0.0048(12) O5 0.0208(15) 0.0147(14) 0.0248(15) 0.0072(12) 0.0048(12) 0.0072(12) O6 0.0300(15) 0.0094(13) 0.0091(12) 0.0055(10) 0.0097(11) 0.0089(12) O7 0.0317(16) 0.0092(13) 0.0106(13) 0.0060(11) 0.0095(12) 0.0106(12) O8 0.0170(17) 0.062(3) 0.040(2) 0.015(2) 0.0080(15) 0.0032(17) O9 0.0362(19) 0.0322(19) 0.0204(16) 0.0091(14) 0.0086(14) 0.0152(16) N1 0.0180(16) 0.0092(15) 0.0124(15) 0.0048(12) 0.0055(13) 0.0056(13) N2 0.0178(16) 0.0100(15) 0.0127(15) 0.0065(13) 0.0050(13) 0.0048(13) N3 0.0185(17) 0.028(2) 0.0170(17) 0.0138(16) 0.0047(14) 0.0056(15) N4 0.0206(16) 0.0117(15) 0.0083(14) 0.0063(12) 0.0071(12) 0.0079(13) N5 0.0186(17) 0.0151(17) 0.0266(19) 0.0076(15) 0.0057(15) 0.0066(14) N6 0.0227(19) 0.0201(19) 0.026(2) 0.0085(16) 0.0062(16) 0.0065(16) C1 0.022(2) 0.0108(18) 0.0150(18) 0.0071(15) 0.0054(16) 0.0048(16) C2 0.025(2) 0.022(2) 0.0136(18) 0.0108(17) 0.0085(16) 0.0113(18) C3 0.023(2) 0.016(2) 0.0114(18) -0.0010(15) 0.0034(16) 0.0080(17) C4 0.021(2) 0.0122(18) 0.0135(18) 0.0050(15) 0.0042(15) 0.0083(16) C5 0.025(2) 0.0077(17) 0.0155(18) 0.0006(15) 0.0037(16) 0.0069(16) C6 0.026(2) 0.0071(18) 0.022(2) 0.0039(16) 0.0032(17) 0.0036(16) C7 0.021(2) 0.0115(18) 0.0152(18) 0.0052(15) 0.0067(16) 0.0065(16) C8 0.026(2) 0.0095(19) 0.020(2) 0.0083(16) 0.0028(17) 0.0009(16) C9 0.026(2) 0.017(2) 0.017(2) 0.0104(17) 0.0081(17) 0.0054(17) C10 0.0194(19) 0.0149(19) 0.0124(18) 0.0057(15) 0.0017(15) 0.0052(16) C11 0.0176(19) 0.0133(18) 0.0120(18) 0.0058(15) 0.0038(15) 0.0060(15) C12 0.0179(19) 0.0096(17) 0.0129(17) 0.0053(14) 0.0049(15) 0.0072(15) C13 0.0148(17) 0.0047(16) 0.0094(16) 0.0005(13) 0.0060(14) 0.0044(14) C14 0.0131(17) 0.0076(16) 0.0112(17) 0.0037(14) 0.0045(14) 0.0066(14) C15 0.0156(18) 0.0118(17) 0.0074(16) 0.0060(14) 0.0050(14) 0.0075(15) C16 0.0160(18) 0.0087(17) 0.0092(16) 0.0065(14) 0.0047(14) 0.0061(14) C17 0.0184(18) 0.0087(17) 0.0078(16) 0.0040(13) 0.0047(14) 0.0082(14) C18 0.0148(18) 0.0143(18) 0.0086(16) 0.0054(14) 0.0065(14) 0.0074(15) C19 0.0187(19) 0.0088(17) 0.0120(17) 0.0065(14) 0.0044(14) 0.0071(15) C20 0.0133(17) 0.0083(16) 0.0109(16) 0.0053(14) 0.0054(14) 0.0043(14) C21 0.030(2) 0.014(2) 0.021(2) 0.0064(17) 0.0113(18) 0.0088(18) C22 0.020(2) 0.019(2) 0.057(4) 0.004(2) 0.005(2) 0.0029(19) C23 0.039(3) 0.026(3) 0.037(3) 0.019(2) 0.009(2) 0.015(2) C24 0.028(3) 0.037(3) 0.039(3) 0.007(2) 0.012(2) 0.011(2) C25 0.043(3) 0.047(4) 0.039(3) 0.021(3) 0.011(3) 0.012(3) C26 0.054(4) 0.035(3) 0.038(3) 0.010(3) 0.016(3) 0.012(3) 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 O1 Tb1 O2 82.11(9) . 2_665 O1 Tb1 O5 86.77(10) . . O2 Tb1 O5 141.45(10) 2_665 . O1 Tb1 O7 128.55(9) . 2_655 O2 Tb1 O7 137.04(9) 2_665 2_655 O5 Tb1 O7 76.93(10) . 2_655 O1 Tb1 O4 90.10(10) . . O2 Tb1 O4 72.92(9) 2_665 . O5 Tb1 O4 144.15(10) . . O7 Tb1 O4 77.34(10) 2_655 . O1 Tb1 O6 75.27(9) . 2_655 O2 Tb1 O6 136.16(9) 2_665 2_655 O5 Tb1 O6 74.55(10) . 2_655 O7 Tb1 O6 53.44(8) 2_655 2_655 O4 Tb1 O6 70.13(10) . 2_655 O1 Tb1 N1 147.01(10) . . O2 Tb1 N1 92.20(10) 2_665 . O5 Tb1 N1 77.59(10) . . O7 Tb1 N1 76.12(9) 2_655 . O4 Tb1 N1 119.36(10) . . O6 Tb1 N1 126.32(9) 2_655 . O1 Tb1 O3 135.14(10) . . O2 Tb1 O3 67.88(9) 2_665 . O5 Tb1 O3 137.13(10) . . O7 Tb1 O3 69.33(9) 2_655 . O4 Tb1 O3 50.34(9) . . O6 Tb1 O3 103.76(9) 2_655 . N1 Tb1 O3 69.38(10) . . O1 Tb1 N2 83.81(10) . . O2 Tb1 N2 69.04(10) 2_665 . O5 Tb1 N2 73.15(10) . . O7 Tb1 N2 134.02(10) 2_655 . O4 Tb1 N2 141.94(10) . . O6 Tb1 N2 142.20(10) 2_655 . N1 Tb1 N2 63.98(10) . . O3 Tb1 N2 113.20(9) . . O1 Tb1 C20 101.92(10) . 2_655 O2 Tb1 C20 143.18(10) 2_665 2_655 O5 Tb1 C20 75.24(10) . 2_655 O7 Tb1 C20 26.83(9) 2_655 2_655 O4 Tb1 C20 70.52(10) . 2_655 O6 Tb1 C20 26.66(9) 2_655 2_655 N1 Tb1 C20 101.87(10) . 2_655 O3 Tb1 C20 85.42(9) . 2_655 N2 Tb1 C20 147.48(10) . 2_655 O1 Tb1 N3 112.82(10) . . O2 Tb1 N3 68.00(10) 2_665 . O5 Tb1 N3 148.81(10) . . O7 Tb1 N3 71.88(10) 2_655 . O4 Tb1 N3 24.99(10) . . O6 Tb1 N3 86.85(10) 2_655 . N1 Tb1 N3 94.60(10) . . O3 Tb1 N3 25.36(10) . . N2 Tb1 N3 130.63(10) . . C20 Tb1 N3 77.01(10) 2_655 . C13 O1 Tb1 154.6(2) . . C13 O2 Tb1 150.6(2) . 2_665 N3 O3 Tb1 93.3(2) . . N3 O4 Tb1 99.2(2) . . C21 O5 Tb1 145.1(3) . . C20 O6 Tb1 90.7(2) . 2_655 C20 O7 Tb1 94.4(2) . 2_655 C1 N1 C11 117.8(3) . . C1 N1 Tb1 121.6(3) . . C11 N1 Tb1 120.0(2) . . C10 N2 C12 117.4(3) . . C10 N2 Tb1 123.3(3) . . C12 N2 Tb1 118.6(2) . . O8 N3 O4 121.8(4) . . O8 N3 O3 121.0(4) . . O4 N3 O3 117.2(3) . . O8 N3 Tb1 177.5(3) . . O4 N3 Tb1 55.81(19) . . O3 N3 Tb1 61.36(19) . . N4 N4 C18 113.7(4) 2_654 . C21 N5 C23 121.2(4) . . C21 N5 C22 122.3(4) . . C23 N5 C22 116.4(4) . . C24 N6 C26 121.5(5) . . C24 N6 C25 122.3(5) . . C26 N6 C25 116.0(4) . . N1 C1 C2 123.6(4) . . N1 C1 H1 118.2 . . C2 C1 H1 118.2 . . C3 C2 C1 119.4(4) . . C3 C2 H2 120.3 . . C1 C2 H2 120.3 . . C2 C3 C4 118.6(4) . . C2 C3 H3 120.7 . . C4 C3 H3 120.7 . . C11 C4 C3 118.6(4) . . C11 C4 C5 119.9(4) . . C3 C4 C5 121.5(4) . . C6 C5 C4 120.3(4) . . C6 C5 H5 119.8 . . C4 C5 H5 119.8 . . C5 C6 C7 121.3(4) . . C5 C6 H6 119.4 . . C7 C6 H6 119.4 . . C12 C7 C8 117.5(3) . . C12 C7 C6 119.8(4) . . C8 C7 C6 122.7(4) . . C9 C8 C7 119.1(4) . . C9 C8 H8 120.4 . . C7 C8 H8 120.4 . . C8 C9 C10 119.5(4) . . C8 C9 H9 120.3 . . C10 C9 H9 120.3 . . N2 C10 C9 123.4(4) . . N2 C10 H10 118.3 . . C9 C10 H10 118.3 . . N1 C11 C4 122.0(3) . . N1 C11 C12 118.5(3) . . C4 C11 C12 119.5(3) . . N2 C12 C7 123.2(3) . . N2 C12 C11 117.5(3) . . C7 C12 C11 119.2(3) . . O2 C13 O1 124.1(3) . . O2 C13 C14 118.2(3) . . O1 C13 C14 117.7(3) . . C19 C14 C15 119.6(3) . . C19 C14 C13 120.0(3) . . C15 C14 C13 120.4(3) . . C16 C15 C14 119.4(3) . . C16 C15 H15 120.3 . . C14 C15 H15 120.3 . . C15 C16 C17 120.7(3) . . C15 C16 C20 121.2(3) . . C17 C16 C20 118.0(3) . . C18 C17 C16 119.5(3) . . C18 C17 H17 120.3 . . C16 C17 H17 120.3 . . C17 C18 C19 120.3(3) . . C17 C18 N4 123.8(3) . . C19 C18 N4 115.9(3) . . C18 C19 C14 120.6(3) . . C18 C19 H19 119.7 . . C14 C19 H19 119.7 . . O6 C20 O7 121.2(3) . . O6 C20 C16 120.1(3) . . O7 C20 C16 118.7(3) . . O6 C20 Tb1 62.60(19) . 2_655 O7 C20 Tb1 58.76(18) . 2_655 C16 C20 Tb1 173.5(2) . 2_655 O5 C21 N5 124.1(4) . . O5 C21 H21 118.0 . . N5 C21 H21 118.0 . . N5 C22 H22A 109.5 . . N5 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . N5 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . N5 C23 H23A 109.5 . . N5 C23 H23B 109.5 . . H23A C23 H23B 109.5 . . N5 C23 H23C 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . O9 C24 N6 125.6(5) . . O9 C24 H24 117.2 . . N6 C24 H24 117.2 . . N6 C25 H25A 109.5 . . N6 C25 H25B 109.5 . . H25A C25 H25B 109.5 . . N6 C25 H25C 109.5 . . H25A C25 H25C 109.5 . . H25B C25 H25C 109.5 . . N6 C26 H26A 109.5 . . N6 C26 H26B 109.5 . . H26A C26 H26B 109.5 . . N6 C26 H26C 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Tb1 O1 2.284(2) . Tb1 O2 2.347(3) 2_665 Tb1 O5 2.360(3) . Tb1 O7 2.401(3) 2_655 Tb1 O4 2.474(3) . Tb1 O6 2.486(3) 2_655 Tb1 N1 2.537(3) . Tb1 O3 2.596(3) . Tb1 N2 2.599(3) . Tb1 C20 2.800(4) 2_655 Tb1 N3 2.953(3) . O1 C13 1.260(4) . O2 C13 1.251(4) . O2 Tb1 2.346(3) 2_665 O3 N3 1.267(5) . O4 N3 1.263(5) . O5 C21 1.240(5) . O6 C20 1.257(4) . O6 Tb1 2.486(3) 2_655 O7 C20 1.268(4) . O7 Tb1 2.401(3) 2_655 O8 N3 1.228(5) . O9 C24 1.275(7) . N1 C1 1.327(5) . N1 C11 1.363(5) . N2 C10 1.326(5) . N2 C12 1.358(5) . N4 N4 1.244(6) 2_654 N4 C18 1.442(4) . N5 C21 1.311(6) . N5 C23 1.454(6) . N5 C22 1.460(6) . N6 C24 1.302(7) . N6 C26 1.443(7) . N6 C25 1.458(7) . C1 C2 1.399(6) . C1 H1 0.9500 . C2 C3 1.365(6) . C2 H2 0.9500 . C3 C4 1.413(6) . C3 H3 0.9500 . C4 C11 1.404(5) . C4 C5 1.437(6) . C5 C6 1.349(6) . C5 H5 0.9500 . C6 C7 1.431(5) . C6 H6 0.9500 . C7 C12 1.403(5) . C7 C8 1.405(6) . C8 C9 1.365(6) . C8 H8 0.9500 . C9 C10 1.396(6) . C9 H9 0.9500 . C10 H10 0.9500 . C11 C12 1.442(5) . C13 C14 1.504(5) . C14 C19 1.391(5) . C14 C15 1.406(5) . C15 C16 1.395(5) . C15 H15 0.9500 . C16 C17 1.398(5) . C16 C20 1.499(5) . C17 C18 1.390(5) . C17 H17 0.9500 . C18 C19 1.391(5) . C19 H19 0.9500 . C20 Tb1 2.800(4) 2_655 C21 H21 0.9500 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C24 H24 0.9500 . C25 H25A 0.9800 . C25 H25B 0.9800 . C25 H25C 0.9800 . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C25 H25C O8 0.98 2.57 3.480(7) 154.1 1_656 C25 H25B O6 0.98 2.44 3.406(6) 168.2 2_656 C25 H25A O4 0.98 2.53 3.500(7) 172.5 2_656 C23 H23C O8 0.98 2.48 3.350(7) 147.2 1_655 C22 H22B O3 0.98 2.51 3.434(6) 157.5 1_655 C22 H22A O9 0.98 2.63 3.559(7) 158.1 2_766 C21 H21 O9 0.95 2.59 3.475(6) 155.5 2_766 C10 H10 O2 0.95 2.55 3.398(5) 148.0 . C9 H9 O4 0.95 2.55 3.101(5) 116.9 2_665 C2 H2 O3 0.95 2.45 3.376(5) 163.9 2_666 C1 H1 O7 0.95 2.33 2.984(5) 125.9 2_655 C1 H1 O7 0.95 2.33 2.984(5) 125.9 2_655 C2 H2 O3 0.95 2.45 3.376(5) 163.9 2_666 C9 H9 O4 0.95 2.55 3.101(5) 116.9 2_665 C10 H10 O2 0.95 2.55 3.398(5) 148.0 . C21 H21 O9 0.95 2.59 3.475(6) 155.5 2_766 C22 H22A O9 0.98 2.63 3.559(7) 158.1 2_766 C22 H22B O3 0.98 2.51 3.434(6) 157.5 1_655 C23 H23C O8 0.98 2.48 3.350(7) 147.2 1_655 C25 H25A O4 0.98 2.53 3.500(7) 172.5 2_656 C25 H25B O6 0.98 2.44 3.406(6) 168.2 2_656 C25 H25C O8 0.98 2.57 3.480(7) 154.1 1_656 C1 H1 O7 0.95 2.33 2.984(5) 125.9 2_655 C2 H2 O3 0.95 2.45 3.376(5) 163.9 2_666 C9 H9 O4 0.95 2.55 3.101(5) 116.9 2_665 C10 H10 O2 0.95 2.55 3.398(5) 148.0 . C21 H21 O9 0.95 2.59 3.475(6) 155.5 2_766 C22 H22A O9 0.98 2.63 3.559(7) 158.1 2_766 C22 H22B O3 0.98 2.51 3.434(6) 157.5 1_655 C23 H23C O8 0.98 2.48 3.350(7) 147.2 1_655 C25 H25A O4 0.98 2.53 3.500(7) 172.5 2_656 C25 H25B O6 0.98 2.44 3.406(6) 168.2 2_656 C25 H25C O8 0.98 2.57 3.480(7) 154.1 1_656 C1 H1 O7 0.95 2.33 2.984(5) 125.9 2_655 C2 H2 O3 0.95 2.45 3.376(5) 163.9 2_666 C9 H9 O4 0.95 2.55 3.101(5) 116.9 2_665 C10 H10 O2 0.95 2.55 3.398(5) 148.0 . C21 H21 O9 0.95 2.59 3.475(6) 155.5 2_766 C22 H22A O9 0.98 2.63 3.559(7) 158.1 2_766 C22 H22B O3 0.98 2.51 3.434(6) 157.5 1_655 C23 H23C O8 0.98 2.48 3.350(7) 147.2 1_655 C25 H25A O4 0.98 2.53 3.500(7) 172.5 2_656 C25 H25B O6 0.98 2.44 3.406(6) 168.2 2_656 C25 H25C O8 0.98 2.57 3.480(7) 154.1 1_656 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 Tb1 O4 N3 O8 -179.1(4) . Tb1 O4 N3 O3 -1.2(4) . Tb1 O3 N3 O8 179.0(4) . Tb1 O3 N3 O4 1.1(4) . C11 N1 C1 C2 0.8(6) . Tb1 N1 C1 C2 -170.5(3) . N1 C1 C2 C3 0.5(6) . C1 C2 C3 C4 -1.1(6) . C2 C3 C4 C11 0.3(6) . C2 C3 C4 C5 179.0(4) . C11 C4 C5 C6 -1.4(6) . C3 C4 C5 C6 180.0(4) . C4 C5 C6 C7 0.1(6) . C5 C6 C7 C12 0.6(6) . C5 C6 C7 C8 179.6(4) . C12 C7 C8 C9 0.4(6) . C6 C7 C8 C9 -178.6(4) . C7 C8 C9 C10 0.8(6) . C12 N2 C10 C9 -0.1(6) . Tb1 N2 C10 C9 170.2(3) . C8 C9 C10 N2 -1.0(6) . C1 N1 C11 C4 -1.6(6) . Tb1 N1 C11 C4 169.8(3) . C1 N1 C11 C12 178.9(3) . Tb1 N1 C11 C12 -9.7(5) . C3 C4 C11 N1 1.0(6) . C5 C4 C11 N1 -177.6(4) . C3 C4 C11 C12 -179.4(4) . C5 C4 C11 C12 1.9(6) . C10 N2 C12 C7 1.4(6) . Tb1 N2 C12 C7 -169.3(3) . C10 N2 C12 C11 179.0(3) . Tb1 N2 C12 C11 8.3(4) . C8 C7 C12 N2 -1.6(6) . C6 C7 C12 N2 177.5(4) . C8 C7 C12 C11 -179.1(4) . C6 C7 C12 C11 -0.1(6) . N1 C11 C12 N2 0.7(5) . C4 C11 C12 N2 -178.8(3) . N1 C11 C12 C7 178.4(4) . C4 C11 C12 C7 -1.1(6) . Tb1 O2 C13 O1 -97.2(6) 2_665 Tb1 O2 C13 C14 84.2(5) 2_665 Tb1 O1 C13 O2 49.3(8) . Tb1 O1 C13 C14 -132.2(5) . O2 C13 C14 C19 17.3(5) . O1 C13 C14 C19 -161.3(3) . O2 C13 C14 C15 -162.0(3) . O1 C13 C14 C15 19.3(5) . C19 C14 C15 C16 0.1(5) . C13 C14 C15 C16 179.4(3) . C14 C15 C16 C17 0.6(5) . C14 C15 C16 C20 177.3(3) . C15 C16 C17 C18 -0.5(6) . C20 C16 C17 C18 -177.3(3) . C16 C17 C18 C19 -0.3(6) . C16 C17 C18 N4 178.2(3) . N4 N4 C18 C17 6.3(6) 2_654 N4 N4 C18 C19 -175.1(4) 2_654 C17 C18 C19 C14 1.0(6) . N4 C18 C19 C14 -177.7(3) . C15 C14 C19 C18 -0.8(6) . C13 C14 C19 C18 179.8(3) . Tb1 O6 C20 O7 5.0(4) 2_655 Tb1 O6 C20 C16 -173.2(3) 2_655 Tb1 O7 C20 O6 -5.1(4) 2_655 Tb1 O7 C20 C16 173.0(3) 2_655 C15 C16 C20 O6 3.9(5) . C17 C16 C20 O6 -179.3(3) . C15 C16 C20 O7 -174.3(3) . C17 C16 C20 O7 2.5(5) . Tb1 O5 C21 N5 148.9(4) . C23 N5 C21 O5 1.3(7) . C22 N5 C21 O5 176.9(4) . C26 N6 C24 O9 2.3(8) . C25 N6 C24 O9 177.8(5) .