#------------------------------------------------------------------------------ #$Date: 2022-02-04 21:29:53 +0200 (Fri, 04 Feb 2022) $ #$Revision: 272643 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/89/7708923.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_7708923 loop_ _publ_author_name 'Gu, Qi' 'Wang, Wenqian' 'Lu, Hao' 'Chen, Xi' 'Wang, Shuaihua' 'Wu, Shaofan' _publ_section_title ; Isotypic lanthanide-organic frameworks and scintillating films with colour-tunable X-ray radioluminescence for imaging applications. ; _journal_issue 1 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 257 _journal_page_last 263 _journal_paper_doi 10.1039/d1dt03059k _journal_volume 51 _journal_year 2021 _chemical_formula_moiety 'C42 H27 N6 O6 Tb, H2 O' _chemical_formula_sum 'C42 H29 N6 O7 Tb' _chemical_formula_weight 888.64 _chemical_name_common '[Tb(bmb)3]H2O' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2021-06-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-09-07 deposited with the CCDC. 2021-11-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.4590(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.6637(2) _cell_length_b 22.0021(2) _cell_length_c 9.57190(10) _cell_measurement_reflns_used 25670 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 60.7740 _cell_measurement_theta_min 2.2200 _cell_volume 3708.75(7) _computing_cell_refinement 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -3.00 22.00 0.50 0.11 -- 72.03 -19.00 0.00 50 2 \w 27.00 106.00 0.50 0.11 -- 72.03 -99.00 -30.00 158 3 \w 33.00 106.00 0.50 0.11 -- 72.03-125.00 -30.00 146 4 \w 36.00 64.00 0.50 0.11 -- 72.03 -57.00 120.00 56 5 \w -96.00 -33.00 0.50 0.11 -- -75.46 125.00-150.00 126 6 \w -59.00 -28.00 0.50 0.11 -- -75.46 57.00-120.00 62 7 \w -97.00 -39.00 0.50 0.11 -- -75.46 125.00 90.00 116 8 \w -107.00 -21.00 0.50 0.11 -- -75.46 125.00 120.00 172 9 \w -89.00 -2.00 0.50 0.11 -- -75.46 77.00 90.00 174 10 \w -65.00 -3.00 0.50 0.11 -- -75.46 57.00 90.00 124 11 \w -42.00 -5.00 0.50 0.11 -- -75.46 38.00 150.00 74 12 \w -13.00 70.00 0.50 0.60 -- -1.72 38.00 120.00 166 13 \w -57.00 -5.00 0.50 0.11 -- -75.46 57.00 30.00 104 14 \w -31.00 -4.00 0.50 0.11 -- -75.46 38.00 0.00 54 15 \w -43.00 -3.00 0.50 0.11 -- -75.46 38.00 30.00 80 16 \w -26.00 -1.00 0.50 0.11 -- -75.46 19.00 0.00 50 17 \w -26.00 -1.00 0.50 0.11 -- -75.46 19.00 -90.00 50 18 \w -42.00 -6.00 0.50 0.11 -- -75.46 38.00-120.00 72 19 \w -37.00 -10.00 0.50 0.11 -- -75.46 38.00-150.00 54 20 \w -25.00 0.00 0.50 0.11 -- -75.46 19.00-150.00 50 21 \w -123.00 -2.00 0.50 0.11 -- -75.46 0.00-180.00 242 22 \w -72.00 15.00 0.50 0.60 -- -1.72 -57.00 -30.00 174 23 \w -60.00 -34.00 0.50 0.60 -- -1.72 -38.00 150.00 52 24 \w -24.00 7.00 0.50 0.60 -- -1.72 -38.00 150.00 62 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0530073000 _diffrn_orient_matrix_UB_12 0.0388805000 _diffrn_orient_matrix_UB_13 -0.0532331000 _diffrn_orient_matrix_UB_21 -0.0415767000 _diffrn_orient_matrix_UB_22 -0.0467112000 _diffrn_orient_matrix_UB_23 -0.0527252000 _diffrn_orient_matrix_UB_31 -0.0352602000 _diffrn_orient_matrix_UB_32 -0.0033817000 _diffrn_orient_matrix_UB_33 0.1186735000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 1.3405 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 46785 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 53.543 _diffrn_reflns_theta_max 60.604 _diffrn_reflns_theta_min 2.794 _diffrn_source 'micro-focus metaljet' _exptl_absorpt_coefficient_mu 10.221 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.53972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.590 _exptl_crystal_description block _exptl_crystal_F_000 1772 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O' _refine_diff_density_max 1.164 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 508 _refine_ls_number_reflns 8420 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0303 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+1.9532P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.0759 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7264 _reflns_number_total 8420 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03059k2.cif _cod_data_source_block LnOF-1 _cod_depositor_comments 'Adding full bibliography for 7708923--7708924.cif.' _cod_database_code 7708923 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_usercomment 'C H O N Tb' _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. ; _diffrn_oxdiff_digest_frames ; 012b79df8ddd20844afc8fd1478abb370200038de23 ; _diffrn_oxdiff_digest_hkl ; 011858c4278286b431ea2c905491bf5ef5861c ; _reflns_odcompleteness_completeness 99.99 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 56.82 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2.a Free rotating group: O56(H56a,H56b) 2.b Aromatic/amide H refined with riding coordinates: C37(H37), C31(H31), C15(H15), C27(H27), C40(H40), C46(H46), C36(H36), C42(H42), C11(H11), C34(H34), C8(H8), C29(H29), C43(H43), C35(H35), C28(H28), C13(H13), C49(H49), C44(H44), C7(H7), C2(H2), C12(H12), C6(H6), C5(H5), C55(H55), C51(H51), C52(H52), C50(H50) ; _shelx_res_file ; TITL exp_1981_a.res in P2(1)/c exp_1981.res created by SHELXL-2018/1 at 11:12:13 on 05-Jun-2021 REM Old TITL exp_1981 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.112, Rweak 0.037, Alpha 0.051, Orientation as input REM Formula found by SHELXT: C42 H28 N6 O7 Tb CELL 1.3405 17.6637 22.0021 9.5719 90 94.459 90 ZERR 4 0.0002 0.0002 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Tb DISP C 0.0147 0.007 57.608 DISP H -0 0 0.6481 DISP N 0.0253 0.0135 110.2408 DISP O 0.0412 0.025 193.4765 UNIT 168 112 24 28 4 L.S. 30 PLAN 5 CONF MORE -1 BOND $H fmap 2 acta OMIT 1 0 0 REM REM REM WGHT 0.041900 1.953200 FVAR 0.98882 TB1 5 0.549340 0.761641 0.469023 11.00000 0.04176 0.02625 = 0.02113 0.00006 0.00451 0.00158 O22 4 0.462743 0.791393 0.615739 11.00000 0.05392 0.05129 = 0.03507 0.00065 0.01405 0.00850 O20 4 0.449107 0.790438 0.843265 11.00000 0.04876 0.06083 = 0.03292 -0.00623 0.00069 0.01672 O19 4 0.665957 0.740181 0.108501 11.00000 0.05336 0.04728 = 0.03223 0.00406 0.00059 0.00229 O17 4 0.630219 0.724041 0.321682 11.00000 0.04588 0.05935 = 0.03365 -0.00576 0.00452 0.01585 O25 4 0.502569 0.671599 0.797623 11.00000 0.09264 0.03315 = 0.03465 -0.00417 -0.00449 -0.01562 O23 4 0.537960 0.670506 0.580053 11.00000 0.06748 0.03273 = 0.04187 0.01033 0.00027 -0.00690 N32 3 0.401938 0.456301 0.847292 11.00000 0.06233 0.02467 = 0.04498 0.00322 0.00776 -0.00192 N39 3 0.409344 0.369379 0.966769 11.00000 0.05867 0.03096 = 0.04252 0.00194 0.00747 -0.00152 C38 1 0.366740 0.410689 1.038293 11.00000 0.04532 0.03264 = 0.03968 -0.00149 0.00066 -0.00504 C21 1 0.422860 0.794821 0.718277 11.00000 0.04267 0.03135 = 0.03105 -0.00195 0.00315 0.00421 C26 1 0.461835 0.590521 0.651049 11.00000 0.05243 0.02490 = 0.03160 -0.00069 -0.00159 -0.00124 N1 3 0.860682 0.626811 0.583440 11.00000 0.05739 0.07313 = 0.05089 -0.00298 -0.01185 0.02268 C33 1 0.362118 0.465578 0.965170 11.00000 0.05139 0.03151 = 0.04327 -0.00285 0.00132 -0.00191 C10 1 0.749022 0.685602 0.268165 11.00000 0.04066 0.04771 = 0.03136 -0.00214 0.00322 0.00440 C37 1 0.330137 0.403457 1.161081 11.00000 0.05298 0.04915 = 0.04597 0.00009 0.00637 -0.00776 AFIX 43 H37 2 0.332771 0.367113 1.210827 11.00000 -1.20000 AFIX 0 C31 1 0.447278 0.552632 0.761854 11.00000 0.05980 0.02565 = 0.03258 -0.00028 -0.00386 -0.00254 AFIX 43 H31 2 0.460726 0.564498 0.853693 11.00000 -1.20000 AFIX 0 C18 1 0.677346 0.719461 0.230236 11.00000 0.04174 0.03485 = 0.03003 -0.00498 0.00088 0.00169 C15 1 0.770474 0.671712 0.407570 11.00000 0.04436 0.05534 = 0.03683 -0.00261 0.00203 0.01102 AFIX 43 H15 2 0.740175 0.683683 0.477891 11.00000 -1.20000 AFIX 0 C27 1 0.439859 0.572809 0.514826 11.00000 0.06707 0.03417 = 0.03336 0.00142 -0.00157 -0.00527 AFIX 43 H27 2 0.449155 0.598156 0.440312 11.00000 -1.20000 AFIX 0 C30 1 0.412751 0.497331 0.734509 11.00000 0.06008 0.02405 = 0.03865 0.00253 0.00150 -0.00300 C24 1 0.503905 0.648839 0.678300 11.00000 0.05631 0.02555 = 0.03507 0.00540 -0.00790 -0.00073 C40 1 0.427839 0.398688 0.855215 11.00000 0.06039 0.02807 = 0.04575 0.00145 0.01000 -0.00079 AFIX 43 H40 2 0.456223 0.381333 0.787723 11.00000 -1.20000 AFIX 0 C46 1 0.293687 0.811005 0.800310 11.00000 0.04690 0.04535 = 0.05631 0.01030 0.01041 0.00848 AFIX 43 H46 2 0.314111 0.807929 0.892560 11.00000 -1.20000 AFIX 0 C41 1 0.340172 0.806726 0.690003 11.00000 0.04475 0.03304 = 0.04245 0.00280 0.00172 0.00376 C45 1 0.216255 0.819949 0.770596 11.00000 0.04598 0.05145 = 0.09501 0.00778 0.01805 0.00917 C36 1 0.290149 0.452187 1.205241 11.00000 0.05522 0.07506 = 0.05108 -0.00782 0.00907 -0.00228 AFIX 43 H36 2 0.264472 0.448489 1.286033 11.00000 -1.20000 AFIX 0 C9 1 0.887474 0.571795 0.639851 11.00000 0.04180 0.06718 = 0.06181 -0.00241 -0.01201 0.01179 C4 1 0.900465 0.582054 0.781901 11.00000 0.05654 0.07103 = 0.06001 -0.00099 -0.01765 0.00779 C42 1 0.308798 0.811105 0.552498 11.00000 0.05799 0.05551 = 0.04962 -0.00322 -0.00881 0.00627 AFIX 43 H42 2 0.339796 0.808149 0.478579 11.00000 -1.20000 AFIX 0 C14 1 0.837010 0.640049 0.440935 11.00000 0.04430 0.07616 = 0.04689 0.00379 -0.00214 0.01554 N47 3 0.167112 0.823133 0.881321 11.00000 0.05075 0.07163 = 0.12346 0.00737 0.03100 0.00708 N3 3 0.883600 0.641805 0.813792 11.00000 0.10571 0.08689 = 0.05646 -0.00788 -0.02299 0.02390 C11 1 0.793515 0.666090 0.163626 11.00000 0.06068 0.08908 = 0.03948 0.00458 0.01407 0.02273 AFIX 43 H11 2 0.779295 0.674698 0.070131 11.00000 -1.20000 AFIX 0 C34 1 0.322583 0.515211 1.011294 11.00000 0.08112 0.04070 = 0.05540 -0.00325 0.00205 0.01557 AFIX 43 H34 2 0.320418 0.551875 0.962802 11.00000 -1.20000 AFIX 0 C8 1 0.898503 0.515195 0.581570 11.00000 0.06267 0.07881 = 0.07972 -0.01236 -0.01635 0.01103 AFIX 43 H8 2 0.888955 0.508134 0.486031 11.00000 -1.20000 AFIX 0 C29 1 0.390516 0.479460 0.598913 11.00000 0.07598 0.03050 = 0.04861 -0.00445 -0.00534 -0.01267 AFIX 43 H29 2 0.366668 0.442222 0.581775 11.00000 -1.20000 AFIX 0 C43 1 0.232152 0.819783 0.525988 11.00000 0.06602 0.07775 = 0.07985 -0.00332 -0.02905 0.00943 AFIX 43 H43 2 0.211420 0.822485 0.433871 11.00000 -1.20000 AFIX 0 C35 1 0.286745 0.507355 1.132535 11.00000 0.07258 0.06474 = 0.06431 -0.01216 0.00304 0.02113 AFIX 43 H35 2 0.259578 0.539531 1.167002 11.00000 -1.20000 AFIX 0 C28 1 0.404226 0.517639 0.489707 11.00000 0.08872 0.03955 = 0.03646 -0.00804 -0.01045 -0.01286 AFIX 43 H28 2 0.389331 0.506133 0.398186 11.00000 -1.20000 AFIX 0 N54 3 0.062337 0.805058 0.990769 11.00000 0.06613 0.10613 = 0.18525 0.01257 0.05423 -0.00453 C48 1 0.175686 0.855417 1.002091 11.00000 0.05275 0.08451 = 0.09948 0.02706 0.01642 0.01639 C13 1 0.881461 0.621341 0.337579 11.00000 0.05699 0.12895 = 0.06853 0.00839 0.01236 0.04702 AFIX 43 H13 2 0.926422 0.600385 0.360679 11.00000 -1.20000 AFIX 0 C49 1 0.229012 0.894662 1.053213 11.00000 0.06023 0.14139 = 0.06840 0.00881 0.00853 0.01302 AFIX 43 H49 2 0.272735 0.901370 1.007222 11.00000 -1.20000 AFIX 0 C44 1 0.186177 0.824474 0.632862 11.00000 0.04238 0.07173 = 0.12743 -0.00267 -0.01995 0.00897 AFIX 43 H44 2 0.134351 0.830741 0.613545 11.00000 -1.20000 AFIX 0 C53 1 0.110004 0.843207 1.072203 11.00000 0.05472 0.09317 = 0.11321 0.02603 0.03280 0.02132 C7 1 0.924264 0.470050 0.672134 11.00000 0.07119 0.06366 = 0.12776 -0.00753 -0.02529 0.00949 AFIX 43 H7 2 0.932990 0.431587 0.636432 11.00000 -1.20000 AFIX 0 C2 1 0.860377 0.665886 0.693168 11.00000 0.09564 0.07297 = 0.06357 -0.00585 -0.02150 0.03168 AFIX 43 H2 2 0.845015 0.706192 0.683381 11.00000 -1.20000 AFIX 0 C12 1 0.859133 0.633757 0.199862 11.00000 0.07391 0.14410 = 0.06053 0.00723 0.02581 0.05473 AFIX 43 H12 2 0.888686 0.620168 0.129886 11.00000 -1.20000 AFIX 0 C6 1 0.937516 0.479656 0.812789 11.00000 0.07881 0.08058 = 0.11044 0.02139 -0.03398 0.00368 AFIX 43 H6 2 0.955156 0.447723 0.870082 11.00000 -1.20000 AFIX 0 C5 1 0.925485 0.535000 0.871220 11.00000 0.08250 0.09071 = 0.07452 0.01166 -0.03239 0.00641 AFIX 43 H5 2 0.933698 0.541109 0.967342 11.00000 -1.20000 AFIX 6 O56 4 0.992412 0.688871 1.029970 11.00000 0.24911 0.27896 = 0.16219 0.08037 -0.08259 -0.16389 H56A 2 1.000174 0.726332 1.014692 11.00000 -1.50000 H56B 2 0.953794 0.679949 0.975265 11.00000 -1.50000 AFIX 0 C55 1 0.098355 0.793638 0.885612 11.00000 0.06894 0.08627 = 0.19621 0.01392 0.05385 0.00561 AFIX 43 H55 2 0.079909 0.767091 0.815403 11.00000 -1.20000 AFIX 0 C51 1 0.152480 0.914539 1.247044 11.00000 0.09719 0.17970 = 0.08112 0.01659 0.01196 0.03281 AFIX 43 H51 2 0.145658 0.935351 1.329695 11.00000 -1.20000 AFIX 0 C52 1 0.097575 0.872925 1.194437 11.00000 0.08361 0.14887 = 0.10516 0.04393 0.03830 0.04543 AFIX 43 H52 2 0.054094 0.865632 1.240728 11.00000 -1.20000 AFIX 0 C50 1 0.216985 0.924977 1.176858 11.00000 0.08744 0.18459 = 0.07252 -0.00119 0.00748 0.01614 AFIX 43 H50 2 0.252912 0.952817 1.213253 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_1981_a.res in P2(1)/c REM R1 = 0.0303 for 7264 Fo > 4sig(Fo) and 0.0379 for all 8420 data REM 508 parameters refined using 0 restraints END WGHT 0.0419 1.9514 REM Highest difference peak 1.164, deepest hole -1.095, 1-sigma level 0.069 Q1 1 0.4968 0.7617 0.4526 11.00000 0.05 1.16 Q2 1 0.6090 0.7614 0.4807 11.00000 0.05 0.85 Q3 1 0.5311 0.7272 0.5505 11.00000 0.05 0.49 Q4 1 0.5845 0.7625 0.4048 11.00000 0.05 0.47 Q5 1 0.5663 0.7905 0.3898 11.00000 0.05 0.45 ; _shelx_res_checksum 24398 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.485 _oxdiff_exptl_absorpt_empirical_full_min 0.624 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Tb1 Tb 0.54934(2) 0.76164(2) 0.46902(2) 0.02961(5) Uani 1 1 d . . . . . O22 O 0.46274(12) 0.79139(11) 0.6157(2) 0.0462(5) Uani 1 1 d . . . . . O20 O 0.44911(12) 0.79044(11) 0.8433(2) 0.0476(5) Uani 1 1 d . . . . . O19 O 0.66596(13) 0.74018(10) 0.1085(2) 0.0444(5) Uani 1 1 d . . . . . O17 O 0.63022(12) 0.72404(11) 0.3217(2) 0.0462(5) Uani 1 1 d . . . . . O25 O 0.50257(15) 0.67160(10) 0.7976(2) 0.0540(6) Uani 1 1 d . . . . . O23 O 0.53796(13) 0.67051(9) 0.5801(2) 0.0476(5) Uani 1 1 d . . . . . N32 N 0.40194(15) 0.45630(11) 0.8473(3) 0.0438(6) Uani 1 1 d . . . . . N39 N 0.40934(15) 0.36938(11) 0.9668(3) 0.0439(6) Uani 1 1 d . . . . . C38 C 0.36674(17) 0.41069(14) 1.0383(3) 0.0394(6) Uani 1 1 d . . . . . C21 C 0.42286(16) 0.79482(13) 0.7183(3) 0.0350(6) Uani 1 1 d . . . . . C26 C 0.46183(17) 0.59052(13) 0.6510(3) 0.0366(6) Uani 1 1 d . . . . . N1 N 0.86068(16) 0.62681(16) 0.5834(3) 0.0613(8) Uani 1 1 d . . . . . C33 C 0.36212(18) 0.46558(14) 0.9652(3) 0.0422(7) Uani 1 1 d . . . . . C10 C 0.74902(16) 0.68560(15) 0.2682(3) 0.0399(7) Uani 1 1 d . . . . . C37 C 0.33014(18) 0.40346(16) 1.1611(3) 0.0492(8) Uani 1 1 d . . . . . H37 H 0.332771 0.367113 1.210827 0.059 Uiso 1 1 calc R . . . . C31 C 0.44728(17) 0.55263(13) 0.7619(3) 0.0397(6) Uani 1 1 d . . . . . H31 H 0.460726 0.564498 0.853693 0.048 Uiso 1 1 calc R . . . . C18 C 0.67735(16) 0.71946(14) 0.2302(3) 0.0356(6) Uani 1 1 d . . . . . C15 C 0.77047(17) 0.67171(16) 0.4076(3) 0.0456(7) Uani 1 1 d . . . . . H15 H 0.740175 0.683683 0.477891 0.055 Uiso 1 1 calc R . . . . C27 C 0.43986(18) 0.57281(15) 0.5148(3) 0.0452(7) Uani 1 1 d . . . . . H27 H 0.449155 0.598156 0.440312 0.054 Uiso 1 1 calc R . . . . C30 C 0.41275(18) 0.49733(13) 0.7345(3) 0.0410(7) Uani 1 1 d . . . . . C24 C 0.50391(17) 0.64884(13) 0.6783(3) 0.0396(6) Uani 1 1 d . . . . . C40 C 0.42784(18) 0.39869(14) 0.8552(3) 0.0444(7) Uani 1 1 d . . . . . H40 H 0.456223 0.381333 0.787723 0.053 Uiso 1 1 calc R . . . . C46 C 0.29369(18) 0.81101(15) 0.8003(4) 0.0492(8) Uani 1 1 d . . . . . H46 H 0.314111 0.807929 0.892560 0.059 Uiso 1 1 calc R . . . . C41 C 0.34017(17) 0.80673(14) 0.6900(3) 0.0402(6) Uani 1 1 d . . . . . C45 C 0.2163(2) 0.81995(18) 0.7706(5) 0.0635(10) Uani 1 1 d . . . . . C36 C 0.2901(2) 0.4522(2) 1.2052(4) 0.0602(9) Uani 1 1 d . . . . . H36 H 0.264472 0.448489 1.286033 0.072 Uiso 1 1 calc R . . . . C9 C 0.88747(19) 0.57180(19) 0.6399(4) 0.0578(9) Uani 1 1 d . . . . . C4 C 0.9005(2) 0.5821(2) 0.7819(4) 0.0637(10) Uani 1 1 d . . . . . C42 C 0.3088(2) 0.81111(17) 0.5525(4) 0.0551(9) Uani 1 1 d . . . . . H42 H 0.339796 0.808149 0.478579 0.066 Uiso 1 1 calc R . . . . C14 C 0.83701(19) 0.64005(19) 0.4409(4) 0.0561(9) Uani 1 1 d . . . . . N47 N 0.16711(18) 0.82313(18) 0.8813(5) 0.0807(11) Uani 1 1 d . . . . . N3 N 0.8836(2) 0.6418(2) 0.8138(4) 0.0845(11) Uani 1 1 d . . . . . C11 C 0.7935(2) 0.6661(2) 0.1636(4) 0.0625(10) Uani 1 1 d . . . . . H11 H 0.779295 0.674698 0.070131 0.075 Uiso 1 1 calc R . . . . C34 C 0.3226(2) 0.51521(17) 1.0113(4) 0.0592(9) Uani 1 1 d . . . . . H34 H 0.320418 0.551875 0.962802 0.071 Uiso 1 1 calc R . . . . C8 C 0.8985(2) 0.5152(2) 0.5816(5) 0.0749(12) Uani 1 1 d . . . . . H8 H 0.888955 0.508134 0.486031 0.090 Uiso 1 1 calc R . . . . C29 C 0.3905(2) 0.47946(15) 0.5989(3) 0.0522(8) Uani 1 1 d . . . . . H29 H 0.366668 0.442222 0.581775 0.063 Uiso 1 1 calc R . . . . C43 C 0.2322(2) 0.8198(2) 0.5260(5) 0.0764(12) Uani 1 1 d . . . . . H43 H 0.211420 0.822485 0.433871 0.092 Uiso 1 1 calc R . . . . C35 C 0.2867(2) 0.5074(2) 1.1325(4) 0.0673(11) Uani 1 1 d . . . . . H35 H 0.259578 0.539531 1.167002 0.081 Uiso 1 1 calc R . . . . C28 C 0.4042(2) 0.51764(16) 0.4897(3) 0.0557(9) Uani 1 1 d . . . . . H28 H 0.389331 0.506133 0.398186 0.067 Uiso 1 1 calc R . . . . N54 N 0.0623(2) 0.8051(3) 0.9908(6) 0.1169(19) Uani 1 1 d . . . . . C48 C 0.1757(2) 0.8554(2) 1.0021(6) 0.0784(13) Uani 1 1 d . . . . . C13 C 0.8815(2) 0.6213(3) 0.3376(5) 0.0844(16) Uani 1 1 d . . . . . H13 H 0.926422 0.600385 0.360679 0.101 Uiso 1 1 calc R . . . . C49 C 0.2290(3) 0.8947(3) 1.0532(5) 0.0898(16) Uani 1 1 d . . . . . H49 H 0.272735 0.901370 1.007222 0.108 Uiso 1 1 calc R . . . . C44 C 0.1862(2) 0.8245(2) 0.6329(6) 0.0819(14) Uani 1 1 d . . . . . H44 H 0.134351 0.830741 0.613545 0.098 Uiso 1 1 calc R . . . . C53 C 0.1100(3) 0.8432(3) 1.0722(6) 0.0857(15) Uani 1 1 d . . . . . C7 C 0.9243(2) 0.4701(2) 0.6721(6) 0.0893(15) Uani 1 1 d . . . . . H7 H 0.932990 0.431587 0.636432 0.107 Uiso 1 1 calc R . . . . C2 C 0.8604(3) 0.6659(2) 0.6932(4) 0.0788(13) Uani 1 1 d . . . . . H2 H 0.845015 0.706192 0.683381 0.095 Uiso 1 1 calc R . . . . C12 C 0.8591(3) 0.6338(3) 0.1999(5) 0.0918(17) Uani 1 1 d . . . . . H12 H 0.888686 0.620168 0.129886 0.110 Uiso 1 1 calc R . . . . C6 C 0.9375(3) 0.4797(3) 0.8128(6) 0.0921(15) Uani 1 1 d . . . . . H6 H 0.955156 0.447723 0.870082 0.111 Uiso 1 1 calc R . . . . C5 C 0.9255(3) 0.5350(2) 0.8712(5) 0.0846(14) Uani 1 1 d . . . . . H5 H 0.933698 0.541109 0.967342 0.102 Uiso 1 1 calc R . . . . O56 O 0.9924(5) 0.6889(4) 1.0300(8) 0.235(4) Uani 1 1 d . . . . . H56A H 1.000174 0.726332 1.014692 0.353 Uiso 1 1 d G . . . . H56B H 0.953794 0.679949 0.975265 0.353 Uiso 1 1 d G . . . . C55 C 0.0984(3) 0.7936(3) 0.8856(8) 0.115(2) Uani 1 1 d . . . . . H55 H 0.079909 0.767091 0.815403 0.138 Uiso 1 1 calc R . . . . C51 C 0.1525(4) 0.9145(4) 1.2470(6) 0.119(2) Uani 1 1 d . . . . . H51 H 0.145658 0.935351 1.329695 0.143 Uiso 1 1 calc R . . . . C52 C 0.0976(3) 0.8729(3) 1.1944(6) 0.111(2) Uani 1 1 d . . . . . H52 H 0.054094 0.865632 1.240728 0.133 Uiso 1 1 calc R . . . . C50 C 0.2170(3) 0.9250(4) 1.1769(5) 0.115(2) Uani 1 1 d . . . . . H50 H 0.252912 0.952817 1.213253 0.138 Uiso 1 1 calc R . . . . 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 0.04176(8) 0.02625(8) 0.02113(7) 0.00006(5) 0.00451(5) 0.00158(5) O22 0.0539(12) 0.0513(14) 0.0351(11) 0.0006(10) 0.0140(9) 0.0085(10) O20 0.0488(12) 0.0608(15) 0.0329(11) -0.0062(10) 0.0007(9) 0.0167(11) O19 0.0534(13) 0.0473(13) 0.0322(11) 0.0041(9) 0.0006(9) 0.0023(10) O17 0.0459(12) 0.0594(15) 0.0337(11) -0.0058(10) 0.0045(9) 0.0159(10) O25 0.0926(17) 0.0331(12) 0.0347(11) -0.0042(9) -0.0045(11) -0.0156(11) O23 0.0675(14) 0.0327(11) 0.0419(12) 0.0103(9) 0.0003(10) -0.0069(10) N32 0.0623(16) 0.0247(12) 0.0450(14) 0.0032(10) 0.0078(12) -0.0019(11) N39 0.0587(16) 0.0310(13) 0.0425(14) 0.0019(11) 0.0075(12) -0.0015(11) C38 0.0453(16) 0.0326(15) 0.0397(16) -0.0015(12) 0.0007(12) -0.0050(12) C21 0.0427(15) 0.0314(15) 0.0310(14) -0.0020(11) 0.0032(11) 0.0042(11) C26 0.0524(16) 0.0249(14) 0.0316(14) -0.0007(11) -0.0016(12) -0.0012(12) N1 0.0574(17) 0.073(2) 0.0509(17) -0.0030(15) -0.0118(14) 0.0227(16) C33 0.0514(17) 0.0315(15) 0.0433(17) -0.0029(13) 0.0013(14) -0.0019(13) C10 0.0407(15) 0.0477(18) 0.0314(14) -0.0021(13) 0.0032(12) 0.0044(13) C37 0.0530(18) 0.049(2) 0.0460(18) 0.0001(15) 0.0064(15) -0.0078(15) C31 0.0598(18) 0.0257(14) 0.0326(14) -0.0003(11) -0.0039(13) -0.0025(13) C18 0.0417(15) 0.0348(15) 0.0300(14) -0.0050(12) 0.0009(11) 0.0017(12) C15 0.0444(16) 0.055(2) 0.0368(16) -0.0026(14) 0.0020(13) 0.0110(14) C27 0.067(2) 0.0342(17) 0.0334(15) 0.0014(12) -0.0016(14) -0.0053(14) C30 0.0601(18) 0.0240(14) 0.0387(15) 0.0025(12) 0.0015(13) -0.0030(12) C24 0.0563(17) 0.0255(14) 0.0351(15) 0.0054(12) -0.0079(13) -0.0007(12) C40 0.0604(19) 0.0281(15) 0.0458(17) 0.0014(13) 0.0100(15) -0.0008(13) C46 0.0469(17) 0.0453(19) 0.056(2) 0.0103(15) 0.0104(15) 0.0085(14) C41 0.0448(16) 0.0330(15) 0.0424(16) 0.0028(13) 0.0017(13) 0.0038(12) C45 0.0460(19) 0.051(2) 0.095(3) 0.008(2) 0.018(2) 0.0092(16) C36 0.055(2) 0.075(3) 0.051(2) -0.0078(19) 0.0091(17) -0.0023(18) C9 0.0418(17) 0.067(3) 0.062(2) -0.0024(19) -0.0120(16) 0.0118(16) C4 0.057(2) 0.071(3) 0.060(2) -0.001(2) -0.0177(17) 0.0078(19) C42 0.058(2) 0.056(2) 0.0496(19) -0.0032(16) -0.0088(16) 0.0063(16) C14 0.0443(18) 0.076(3) 0.0469(19) 0.0038(18) -0.0021(14) 0.0155(17) N47 0.0508(19) 0.072(3) 0.123(3) 0.007(2) 0.031(2) 0.0071(16) N3 0.106(3) 0.087(3) 0.056(2) -0.0079(19) -0.0230(19) 0.024(2) C11 0.061(2) 0.089(3) 0.0395(18) 0.0046(18) 0.0141(16) 0.023(2) C34 0.081(3) 0.041(2) 0.055(2) -0.0033(16) 0.0021(19) 0.0156(17) C8 0.063(2) 0.079(3) 0.080(3) -0.012(2) -0.016(2) 0.011(2) C29 0.076(2) 0.0305(16) 0.0486(19) -0.0045(14) -0.0053(16) -0.0127(15) C43 0.066(3) 0.078(3) 0.080(3) -0.003(2) -0.029(2) 0.009(2) C35 0.073(2) 0.065(3) 0.064(2) -0.012(2) 0.003(2) 0.021(2) C28 0.089(3) 0.0395(19) 0.0365(16) -0.0080(14) -0.0105(16) -0.0129(17) N54 0.066(3) 0.106(4) 0.185(5) 0.013(3) 0.054(3) -0.005(2) C48 0.053(2) 0.085(3) 0.099(4) 0.027(3) 0.016(2) 0.016(2) C13 0.057(2) 0.129(4) 0.069(3) 0.008(3) 0.012(2) 0.047(3) C49 0.060(3) 0.141(5) 0.068(3) 0.009(3) 0.009(2) 0.013(3) C44 0.042(2) 0.072(3) 0.127(4) -0.003(3) -0.020(2) 0.0090(19) C53 0.055(2) 0.093(4) 0.113(4) 0.026(3) 0.033(3) 0.021(2) C7 0.071(3) 0.064(3) 0.128(4) -0.008(3) -0.025(3) 0.009(2) C2 0.096(3) 0.073(3) 0.064(3) -0.006(2) -0.021(2) 0.032(2) C12 0.074(3) 0.144(5) 0.061(3) 0.007(3) 0.026(2) 0.055(3) C6 0.079(3) 0.081(4) 0.110(4) 0.021(3) -0.034(3) 0.004(3) C5 0.083(3) 0.091(4) 0.075(3) 0.012(3) -0.032(2) 0.006(3) O56 0.249(7) 0.279(9) 0.162(5) 0.080(6) -0.083(5) -0.164(7) C55 0.069(3) 0.086(4) 0.196(7) 0.014(4) 0.054(4) 0.006(3) C51 0.097(4) 0.180(7) 0.081(4) 0.017(4) 0.012(3) 0.033(5) C52 0.084(4) 0.149(6) 0.105(4) 0.044(4) 0.038(3) 0.045(4) C50 0.087(4) 0.185(7) 0.073(3) -0.001(4) 0.007(3) 0.016(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0147 0.0070 '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 0.0253 0.0135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -4.4782 11.8047 '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 O22 Tb1 O20 86.57(8) . 4_575 ? O22 Tb1 O19 104.88(8) . 4_576 ? O22 Tb1 O25 92.03(8) . 4_575 ? O22 Tb1 O23 82.91(8) . . ? O22 Tb1 N39 76.96(8) . 2_656 ? O20 Tb1 O19 149.94(8) 4_575 4_576 ? O20 Tb1 N39 140.03(9) 4_575 2_656 ? O19 Tb1 N39 70.02(8) 4_576 2_656 ? O17 Tb1 O22 174.91(8) . . ? O17 Tb1 O20 89.40(8) . 4_575 ? O17 Tb1 O19 77.25(8) . 4_576 ? O17 Tb1 O25 89.89(8) . 4_575 ? O17 Tb1 O23 92.99(8) . . ? O17 Tb1 N39 108.13(9) . 2_656 ? O25 Tb1 O20 74.53(8) 4_575 4_575 ? O25 Tb1 O19 131.30(9) 4_575 4_576 ? O25 Tb1 N39 70.02(8) 4_575 2_656 ? O23 Tb1 O20 73.83(8) . 4_575 ? O23 Tb1 O19 80.04(8) . 4_576 ? O23 Tb1 O25 148.19(8) . 4_575 ? O23 Tb1 N39 137.71(8) . 2_656 ? C21 O22 Tb1 162.8(2) . . ? C21 O20 Tb1 137.06(18) . 4_576 ? C18 O19 Tb1 126.04(19) . 4_575 ? C18 O17 Tb1 162.9(2) . . ? C24 O25 Tb1 151.0(2) . 4_576 ? C24 O23 Tb1 138.6(2) . . ? C33 N32 C30 128.7(3) . . ? C40 N32 C33 106.5(2) . . ? C40 N32 C30 124.8(3) . . ? C38 N39 Tb1 130.20(19) . 2_646 ? C40 N39 Tb1 124.8(2) . 2_646 ? C40 N39 C38 104.9(3) . . ? N39 C38 C33 109.3(3) . . ? C37 C38 N39 130.1(3) . . ? C37 C38 C33 120.6(3) . . ? O22 C21 C41 118.1(2) . . ? O20 C21 O22 123.6(3) . . ? O20 C21 C41 118.2(2) . . ? C31 C26 C24 120.1(2) . . ? C27 C26 C31 119.6(3) . . ? C27 C26 C24 120.3(3) . . ? C9 N1 C14 127.9(3) . . ? C2 N1 C9 105.8(3) . . ? C2 N1 C14 126.3(3) . . ? N32 C33 C38 105.5(3) . . ? C34 C33 N32 132.3(3) . . ? C34 C33 C38 122.2(3) . . ? C15 C10 C18 120.4(3) . . ? C11 C10 C18 119.8(3) . . ? C11 C10 C15 119.7(3) . . ? C38 C37 H37 121.5 . . ? C36 C37 C38 117.1(3) . . ? C36 C37 H37 121.5 . . ? C26 C31 H31 120.3 . . ? C30 C31 C26 119.4(3) . . ? C30 C31 H31 120.3 . . ? O19 C18 O17 123.4(3) . . ? O19 C18 C10 118.7(3) . . ? O17 C18 C10 117.8(3) . . ? C10 C15 H15 120.2 . . ? C14 C15 C10 119.7(3) . . ? C14 C15 H15 120.2 . . ? C26 C27 H27 120.0 . . ? C28 C27 C26 120.1(3) . . ? C28 C27 H27 120.0 . . ? C31 C30 N32 119.8(3) . . ? C31 C30 C29 121.2(3) . . ? C29 C30 N32 118.9(3) . . ? O25 C24 C26 117.3(3) . . ? O23 C24 O25 125.4(3) . . ? O23 C24 C26 117.2(3) . . ? N32 C40 H40 123.1 . . ? N39 C40 N32 113.8(3) . . ? N39 C40 H40 123.1 . . ? C41 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C45 C46 C41 119.0(3) . . ? C46 C41 C21 120.2(3) . . ? C42 C41 C21 119.8(3) . . ? C42 C41 C46 119.9(3) . . ? C46 C45 N47 120.2(4) . . ? C44 C45 C46 120.2(4) . . ? C44 C45 N47 119.6(4) . . ? C37 C36 H36 119.0 . . ? C37 C36 C35 122.0(3) . . ? C35 C36 H36 119.0 . . ? C4 C9 N1 105.4(3) . . ? C4 C9 C8 121.8(4) . . ? C8 C9 N1 132.8(4) . . ? C9 C4 N3 110.5(4) . . ? C9 C4 C5 120.3(4) . . ? N3 C4 C5 129.3(4) . . ? C41 C42 H42 120.0 . . ? C43 C42 C41 120.0(4) . . ? C43 C42 H42 120.0 . . ? C15 C14 N1 120.3(3) . . ? C13 C14 N1 119.1(3) . . ? C13 C14 C15 120.5(3) . . ? C48 N47 C45 128.8(4) . . ? C48 N47 C55 105.1(4) . . ? C55 N47 C45 126.0(5) . . ? C2 N3 C4 104.3(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 C10 119.3(3) . . ? C12 C11 H11 120.3 . . ? C33 C34 H34 121.8 . . ? C35 C34 C33 116.5(3) . . ? C35 C34 H34 121.8 . . ? C9 C8 H8 121.7 . . ? C7 C8 C9 116.5(4) . . ? C7 C8 H8 121.7 . . ? C30 C29 H29 120.5 . . ? C28 C29 C30 119.0(3) . . ? C28 C29 H29 120.5 . . ? C42 C43 H43 119.6 . . ? C44 C43 C42 120.7(4) . . ? C44 C43 H43 119.6 . . ? C36 C35 H35 119.2 . . ? C34 C35 C36 121.6(4) . . ? C34 C35 H35 119.2 . . ? C27 C28 H28 119.7 . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28 119.7 . . ? C55 N54 C53 104.4(5) . . ? N47 C48 C53 105.3(5) . . ? C49 C48 N47 132.6(4) . . ? C49 C48 C53 121.9(6) . . ? C14 C13 H13 120.2 . . ? C14 C13 C12 119.6(4) . . ? C12 C13 H13 120.2 . . ? C48 C49 H49 121.0 . . ? C48 C49 C50 118.0(5) . . ? C50 C49 H49 121.0 . . ? C45 C44 H44 119.9 . . ? C43 C44 C45 120.2(4) . . ? C43 C44 H44 119.9 . . ? N54 C53 C48 109.5(5) . . ? C52 C53 N54 129.6(5) . . ? C52 C53 C48 120.4(6) . . ? C8 C7 H7 118.9 . . ? C6 C7 C8 122.3(5) . . ? C6 C7 H7 118.9 . . ? N1 C2 H2 123.0 . . ? N3 C2 N1 114.0(4) . . ? N3 C2 H2 123.0 . . ? C11 C12 H12 119.5 . . ? C13 C12 C11 121.1(4) . . ? C13 C12 H12 119.5 . . ? C7 C6 H6 119.2 . . ? C7 C6 C5 121.5(5) . . ? C5 C6 H6 119.2 . . ? C4 C5 H5 121.2 . . ? C6 C5 C4 117.7(4) . . ? C6 C5 H5 121.2 . . ? H56A O56 H56B 104.5 . . ? N47 C55 H55 122.2 . . ? N54 C55 N47 115.5(6) . . ? N54 C55 H55 122.2 . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C50 C51 C52 120.5(6) . . ? C53 C52 C51 117.8(5) . . ? C53 C52 H52 121.1 . . ? C51 C52 H52 121.1 . . ? C49 C50 H50 119.4 . . ? C51 C50 C49 121.3(7) . . ? C51 C50 H50 119.4 . . ? 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 O22 2.2527(19) . ? Tb1 O20 2.359(2) 4_575 ? Tb1 O19 2.366(2) 4_576 ? Tb1 O17 2.242(2) . ? Tb1 O25 2.307(2) 4_575 ? Tb1 O23 2.286(2) . ? Tb1 N39 2.542(3) 2_656 ? O22 C21 1.254(3) . ? O20 C21 1.253(3) . ? O19 C18 1.253(3) . ? O17 C18 1.258(3) . ? O25 C24 1.249(3) . ? O23 C24 1.250(3) . ? N32 C33 1.390(4) . ? N32 C30 1.431(4) . ? N32 C40 1.348(4) . ? N39 C38 1.393(4) . ? N39 C40 1.310(4) . ? C38 C33 1.395(4) . ? C38 C37 1.394(4) . ? C21 C41 1.488(4) . ? C26 C31 1.389(4) . ? C26 C27 1.387(4) . ? C26 C24 1.495(4) . ? N1 C9 1.393(5) . ? N1 C14 1.425(4) . ? N1 C2 1.358(5) . ? C33 C34 1.387(4) . ? C10 C18 1.489(4) . ? C10 C15 1.392(4) . ? C10 C11 1.388(4) . ? C37 H37 0.9300 . ? C37 C36 1.369(5) . ? C31 H31 0.9300 . ? C31 C30 1.377(4) . ? C15 H15 0.9300 . ? C15 C14 1.382(4) . ? C27 H27 0.9300 . ? C27 C28 1.380(4) . ? C30 C29 1.384(4) . ? C40 H40 0.9300 . ? C46 H46 0.9300 . ? C46 C41 1.390(4) . ? C46 C45 1.389(5) . ? C41 C42 1.391(4) . ? C45 N47 1.423(5) . ? C45 C44 1.386(6) . ? C36 H36 0.9300 . ? C36 C35 1.398(6) . ? C9 C4 1.380(5) . ? C9 C8 1.385(6) . ? C4 N3 1.387(6) . ? C4 C5 1.393(6) . ? C42 H42 0.9300 . ? C42 C43 1.371(5) . ? C14 C13 1.373(5) . ? N47 C48 1.355(6) . ? N47 C55 1.380(6) . ? N3 C2 1.307(5) . ? C11 H11 0.9300 . ? C11 C12 1.381(5) . ? C34 H34 0.9300 . ? C34 C35 1.375(5) . ? C8 H8 0.9300 . ? C8 C7 1.373(6) . ? C29 H29 0.9300 . ? C29 C28 1.377(4) . ? C43 H43 0.9300 . ? C43 C44 1.359(6) . ? C35 H35 0.9300 . ? C28 H28 0.9300 . ? N54 C53 1.385(7) . ? N54 C55 1.257(7) . ? C48 C49 1.342(7) . ? C48 C53 1.411(6) . ? C13 H13 0.9300 . ? C13 C12 1.374(6) . ? C49 H49 0.9300 . ? C49 C50 1.389(7) . ? C44 H44 0.9300 . ? C53 C52 1.373(8) . ? C7 H7 0.9300 . ? C7 C6 1.365(7) . ? C2 H2 0.9300 . ? C12 H12 0.9300 . ? C6 H6 0.9300 . ? C6 C5 1.364(7) . ? C5 H5 0.9300 . ? O56 H56A 0.8501 . ? O56 H56B 0.8500 . ? C55 H55 0.9300 . ? C51 H51 0.9300 . ? C51 C52 1.399(9) . ? C51 C50 1.386(8) . ? C52 H52 0.9300 . ? C50 H50 0.9300 . ? 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 O22 C21 O20 44.6(9) . . . . ? Tb1 O22 C21 C41 -137.4(6) . . . . ? Tb1 O20 C21 O22 -32.1(5) 4_576 . . . ? Tb1 O20 C21 C41 149.9(2) 4_576 . . . ? Tb1 O19 C18 O17 -39.0(4) 4_575 . . . ? Tb1 O19 C18 C10 138.7(2) 4_575 . . . ? Tb1 O17 C18 O19 -55.3(8) . . . . ? Tb1 O17 C18 C10 126.9(6) . . . . ? Tb1 O25 C24 O23 -15.2(7) 4_576 . . . ? Tb1 O25 C24 C26 164.2(3) 4_576 . . . ? Tb1 O23 C24 O25 -49.2(5) . . . . ? Tb1 O23 C24 C26 131.4(3) . . . . ? Tb1 N39 C38 C33 176.8(2) 2_646 . . . ? Tb1 N39 C38 C37 -4.9(5) 2_646 . . . ? Tb1 N39 C40 N32 -177.1(2) 2_646 . . . ? O22 C21 C41 C46 -179.9(3) . . . . ? O22 C21 C41 C42 2.7(4) . . . . ? O20 C21 C41 C46 -1.8(4) . . . . ? O20 C21 C41 C42 -179.2(3) . . . . ? N32 C33 C34 C35 177.4(4) . . . . ? N32 C30 C29 C28 -176.9(3) . . . . ? N39 C38 C33 N32 0.7(3) . . . . ? N39 C38 C33 C34 179.6(3) . . . . ? N39 C38 C37 C36 -178.1(3) . . . . ? C38 N39 C40 N32 0.8(4) . . . . ? C38 C33 C34 C35 -1.0(5) . . . . ? C38 C37 C36 C35 -1.0(5) . . . . ? C21 C41 C42 C43 177.5(3) . . . . ? C26 C31 C30 N32 176.0(3) . . . . ? C26 C31 C30 C29 -1.7(5) . . . . ? C26 C27 C28 C29 -0.4(6) . . . . ? N1 C9 C4 N3 -0.9(5) . . . . ? N1 C9 C4 C5 177.8(4) . . . . ? N1 C9 C8 C7 -178.0(4) . . . . ? N1 C14 C13 C12 179.9(5) . . . . ? C33 N32 C30 C31 58.9(4) . . . . ? C33 N32 C30 C29 -123.4(4) . . . . ? C33 N32 C40 N39 -0.3(4) . . . . ? C33 C38 C37 C36 0.0(5) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? C10 C15 C14 N1 178.4(3) . . . . ? C10 C15 C14 C13 -1.1(6) . . . . ? C10 C11 C12 C13 -0.9(8) . . . . ? C37 C38 C33 N32 -177.8(3) . . . . ? C37 C38 C33 C34 1.0(5) . . . . ? C37 C36 C35 C34 1.0(6) . . . . ? C31 C26 C27 C28 -0.5(5) . . . . ? C31 C26 C24 O25 -23.5(4) . . . . ? C31 C26 C24 O23 156.0(3) . . . . ? C31 C30 C29 C28 0.8(5) . . . . ? C18 C10 C15 C14 179.7(3) . . . . ? C18 C10 C11 C12 -178.8(4) . . . . ? C15 C10 C18 O19 168.1(3) . . . . ? C15 C10 C18 O17 -14.1(4) . . . . ? C15 C10 C11 C12 -0.8(6) . . . . ? C15 C14 C13 C12 -0.6(8) . . . . ? C27 C26 C31 C30 1.5(5) . . . . ? C27 C26 C24 O25 159.2(3) . . . . ? C27 C26 C24 O23 -21.4(4) . . . . ? C30 N32 C33 C38 177.7(3) . . . . ? C30 N32 C33 C34 -0.9(6) . . . . ? C30 N32 C40 N39 -178.4(3) . . . . ? C30 C29 C28 C27 0.2(6) . . . . ? C24 C26 C31 C30 -175.9(3) . . . . ? C24 C26 C27 C28 176.9(3) . . . . ? C40 N32 C33 C38 -0.3(3) . . . . ? C40 N32 C33 C34 -178.9(4) . . . . ? C40 N32 C30 C31 -123.5(4) . . . . ? C40 N32 C30 C29 54.2(5) . . . . ? C40 N39 C38 C33 -0.9(3) . . . . ? C40 N39 C38 C37 177.4(3) . . . . ? C46 C41 C42 C43 0.2(5) . . . . ? C46 C45 N47 C48 47.1(6) . . . . ? C46 C45 N47 C55 -134.1(5) . . . . ? C46 C45 C44 C43 0.4(7) . . . . ? C41 C46 C45 N47 178.6(3) . . . . ? C41 C46 C45 C44 0.0(6) . . . . ? C41 C42 C43 C44 0.3(7) . . . . ? C45 C46 C41 C21 -177.7(3) . . . . ? C45 C46 C41 C42 -0.3(5) . . . . ? C45 N47 C48 C49 2.5(9) . . . . ? C45 N47 C48 C53 178.7(4) . . . . ? C45 N47 C55 N54 -176.8(5) . . . . ? C9 N1 C14 C15 134.1(4) . . . . ? C9 N1 C14 C13 -46.3(6) . . . . ? C9 N1 C2 N3 -0.4(5) . . . . ? C9 C4 N3 C2 0.7(5) . . . . ? C9 C4 C5 C6 1.0(7) . . . . ? C9 C8 C7 C6 0.9(7) . . . . ? C4 C9 C8 C7 -1.1(6) . . . . ? C4 N3 C2 N1 -0.2(6) . . . . ? C42 C43 C44 C45 -0.6(7) . . . . ? C14 N1 C9 C4 -178.3(3) . . . . ? C14 N1 C9 C8 -0.9(7) . . . . ? C14 N1 C2 N3 178.7(4) . . . . ? C14 C13 C12 C11 1.6(9) . . . . ? N47 C45 C44 C43 -178.1(4) . . . . ? N47 C48 C49 C50 173.8(5) . . . . ? N47 C48 C53 N54 -1.5(6) . . . . ? N47 C48 C53 C52 -174.8(5) . . . . ? N3 C4 C5 C6 179.5(5) . . . . ? C11 C10 C18 O19 -14.0(5) . . . . ? C11 C10 C18 O17 163.8(3) . . . . ? C11 C10 C15 C14 1.8(5) . . . . ? C8 C9 C4 N3 -178.6(4) . . . . ? C8 C9 C4 C5 0.1(6) . . . . ? C8 C7 C6 C5 0.3(8) . . . . ? N54 C53 C52 C51 -172.7(6) . . . . ? C48 N47 C55 N54 2.3(7) . . . . ? C48 C49 C50 C51 1.0(9) . . . . ? C48 C53 C52 C51 -0.9(8) . . . . ? C49 C48 C53 N54 175.2(5) . . . . ? C49 C48 C53 C52 1.9(8) . . . . ? C44 C45 N47 C48 -134.3(5) . . . . ? C44 C45 N47 C55 44.5(6) . . . . ? C53 N54 C55 N47 -3.1(7) . . . . ? C53 C48 C49 C50 -1.9(8) . . . . ? C7 C6 C5 C4 -1.2(8) . . . . ? C2 N1 C9 C4 0.8(4) . . . . ? C2 N1 C9 C8 178.1(5) . . . . ? C2 N1 C14 C15 -44.7(6) . . . . ? C2 N1 C14 C13 134.8(5) . . . . ? C5 C4 N3 C2 -177.9(5) . . . . ? C55 N47 C48 C49 -176.5(6) . . . . ? C55 N47 C48 C53 -0.3(5) . . . . ? C55 N54 C53 C48 2.8(6) . . . . ? C55 N54 C53 C52 175.2(6) . . . . ? C52 C51 C50 C49 0.0(10) . . . . ? C50 C51 C52 C53 0.0(9) . . . . ?