#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:41:58 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252627 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240602.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_7240602 loop_ _publ_author_name 'Bo, Qi-Bing' 'Wang, Jia-Yin' 'Shi, Yang' 'Tao, Dong-Liang' 'Yin, Guo-Yin' _publ_section_title ; 2D chain layer versus 1D chain: rigid aromatic benzoate disassembling flexible alicyclic dicarboxylate-based lanthanide coordination polymers with enhanced photoluminescence and characteristic behavior of single-molecule magnet. ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00583E _journal_year 2020 _chemical_formula_moiety 'C12 H11 O7 Tb' _chemical_formula_sum 'C12 H11 O7 Tb' _chemical_formula_weight 426.13 _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 direct _audit_creation_date 2019-11-02 _audit_creation_method ; Olex2 1.2-alpha (compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261) ; _audit_update_record ; 2019-11-02 deposited with the CCDC. 2020-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 148.12(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.790(8) _cell_length_b 7.4571(8) _cell_length_c 23.894(14) _cell_measurement_reflns_used 2357 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.6480 _cell_measurement_theta_min 3.9540 _cell_volume 1298(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0355 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.993 _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 -53.00 35.00 1.00 28.43 -- 15.86 -37.00-180.00 88 2 \w -3.00 85.00 1.00 28.43 -- 15.86 37.00 0.00 88 3 \w -25.00 22.00 1.00 28.43 -- -16.95 -99.00 -30.00 47 4 \w 32.00 88.00 1.00 28.43 -- 15.86-178.00 60.00 56 5 \w -85.00 -25.00 1.00 28.43 -- -16.95 -77.00 150.00 60 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0784973000 _diffrn_orient_matrix_UB_12 -0.0559732000 _diffrn_orient_matrix_UB_13 -0.0402796000 _diffrn_orient_matrix_UB_21 -0.0569317000 _diffrn_orient_matrix_UB_22 0.0737170000 _diffrn_orient_matrix_UB_23 -0.0206691000 _diffrn_orient_matrix_UB_31 -0.0095007000 _diffrn_orient_matrix_UB_32 0.0221258000 _diffrn_orient_matrix_UB_33 -0.0333761000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_unetI/netI 0.0768 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 7915 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.229 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 5.478 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear whiteish white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier whiteish _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 2.181 _exptl_crystal_description needle _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _refine_diff_density_max 4.709 _refine_diff_density_min -4.668 _refine_diff_density_rms 0.431 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 2633 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0759 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1323P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1850 _refine_ls_wR_factor_ref 0.2067 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2009 _reflns_number_total 2633 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 180502_bqb_d1_a.res in P2(1)/c REM Old TITL 180502_BQB_D1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.168, Rweak 0.258, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C11 O7 I CELL 0.71073 13.7899 7.4571 23.8937 90 148.12 90 ZERR 4 0.0081 0.0008 0.0137 0 0.146 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O Tb UNIT 48 44 28 4 EADP O3 O4 O1 O2 EADP C2 C1 L.S. 100 PLAN 10 htab BOND $H list 4 MORE -1 CONF fmap 2 acta SHEL 999 0.8 OMIT -2 3 4 OMIT -5 2 7 OMIT -1 3 1 OMIT -17 1 24 OMIT 0 2 1 OMIT -4 3 13 OMIT 0 8 6 OMIT -1 2 1 OMIT -1 3 3 OMIT 0 2 0 OMIT -1 2 2 OMIT -3 3 3 REM REM REM WGHT 0.132300 FVAR 0.35371 TB1 4 0.396548 0.559371 0.204237 11.00000 0.02608 0.00383 = 0.02830 -0.00021 0.02216 -0.00041 O3 3 0.596952 0.349061 0.346637 11.00000 0.03437 0.01183 = 0.03161 -0.00120 0.02670 -0.00052 O4 3 0.867341 0.266093 0.448872 11.00000 0.03437 0.01183 = 0.03161 -0.00120 0.02670 -0.00052 O5 3 0.594124 0.496634 0.228879 11.00000 0.04941 0.00899 = 0.05414 -0.00063 0.04509 0.00291 O1 3 0.662313 0.725224 0.356916 11.00000 0.03437 0.01183 = 0.03161 -0.00120 0.02670 -0.00052 O2 3 0.804680 0.944036 0.469949 11.00000 0.03437 0.01183 = 0.03161 -0.00120 0.02670 -0.00052 O7 3 0.159802 0.414752 0.140743 11.00000 0.03650 0.01176 = 0.03988 -0.00690 0.03123 -0.00934 AFIX 7 H7A 2 0.198973 0.389058 0.193033 11.00000 -1.50000 H7B 2 0.127069 0.317084 0.108171 11.00000 -1.50000 AFIX 0 O6 3 0.661138 0.217276 0.240106 11.00000 0.04495 0.01035 = 0.05249 0.00455 0.04269 0.00283 C2 1 0.772278 0.356203 0.435913 11.00000 0.02732 0.01048 = 0.02604 -0.00056 0.02071 0.00058 C4 1 0.867218 0.451403 0.529247 11.00000 0.03932 0.01339 = 0.03184 0.00891 0.02950 0.00894 AFIX 13 H4 2 0.980103 0.393901 0.597845 11.00000 -1.20000 AFIX 0 C1 1 0.773531 0.777707 0.448911 11.00000 0.02732 0.01048 = 0.02604 -0.00056 0.02071 0.00058 C5 1 0.754705 0.538838 0.518469 11.00000 0.06368 0.01533 = 0.05163 0.00837 0.05113 0.00812 AFIX 23 H5A 2 0.797116 0.528890 0.577612 11.00000 -1.20000 H5B 2 0.622319 0.537126 0.449177 11.00000 -1.20000 AFIX 0 C7 1 0.695656 0.436701 0.187329 11.00000 0.03991 0.02028 = 0.03719 0.00406 0.03213 0.00660 C3 1 0.864443 0.656964 0.532797 11.00000 0.04276 0.02182 = 0.03306 0.00145 0.03224 0.00394 AFIX 13 H3 2 0.975728 0.707377 0.604190 11.00000 -1.20000 AFIX 0 C6 1 0.648605 0.381753 0.221940 11.00000 0.03582 0.01526 = 0.03342 0.00118 0.02928 0.00287 C8 1 0.757357 0.314489 0.178273 11.00000 0.07076 0.02362 = 0.06223 -0.01060 0.06100 -0.00831 AFIX 43 H8 2 0.771076 0.194520 0.194774 11.00000 -1.20000 AFIX 0 C12 1 0.677081 0.617230 0.163350 11.00000 0.07591 0.02336 = 0.08420 0.00945 0.07106 0.00172 AFIX 43 H12 2 0.639982 0.702110 0.171348 11.00000 -1.20000 AFIX 0 C11 1 0.715545 0.666818 0.127163 11.00000 0.11947 0.04836 = 0.09724 -0.00174 0.09818 -0.01316 AFIX 43 H11 2 0.700766 0.786024 0.109406 11.00000 -1.20000 AFIX 0 C10 1 0.774635 0.544834 0.116953 11.00000 0.12213 0.06767 = 0.10173 -0.01657 0.10337 -0.03093 AFIX 43 H10 2 0.797686 0.580560 0.091626 11.00000 -1.20000 AFIX 0 C9 1 0.798976 0.370398 0.144561 11.00000 0.08350 0.06392 = 0.09496 -0.00309 0.08282 0.00381 AFIX 43 H9 2 0.843911 0.287930 0.140797 11.00000 -1.20000 AFIX 0 HKLF 4 REM 180502_bqb_d1_a.res in P2(1)/c REM R1 = 0.0759 for 2009 Fo > 4sig(Fo) and 0.0957 for all 2633 data REM 158 parameters refined using 0 restraints END WGHT 0.1323 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 x-1, -y+1/2, z-1/2 HTAB O7 O4_$1 EQIV $2 -x+1, y-1/2, -z+1/2 HTAB O7 O1_$2 REM Highest difference peak 4.709, deepest hole -4.668, 1-sigma level 0.431 Q1 1 0.5203 0.5579 0.2766 11.00000 0.05 4.58 Q2 1 0.3904 0.5646 0.2377 11.00000 0.05 4.52 Q3 1 0.2800 0.5751 0.1343 11.00000 0.05 4.21 Q4 1 0.4105 0.5622 0.1750 11.00000 0.05 4.16 Q5 1 0.8089 0.5565 0.3879 11.00000 0.05 2.86 Q6 1 0.3027 0.5195 0.1803 11.00000 0.05 1.80 Q7 1 0.4987 0.4949 0.2231 11.00000 0.05 1.32 Q8 1 0.9585 0.2743 0.5132 11.00000 0.05 1.18 Q9 1 0.6175 0.8500 0.2954 11.00000 0.05 1.04 Q10 1 0.9083 0.2810 0.4360 11.00000 0.05 1.01 REM The information below was added by Olex2. REM REM R1 = 0.0759 for 2009 Fo > 4sig(Fo) and 0.0957 for all 9032 data REM n/a parameters refined using n/a restraints REM Highest difference peak 4.71, deepest hole -4.67 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0957 REM R1_gt = 0.0759 REM wR_ref = 0.2067 REM GOOF = 1.068 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 9032 REM Reflections_gt = 2009 REM Parameters = n/a REM Hole = -4.67 REM Peak = 4.71 REM Flack = n/a ; _cod_data_source_file d0ce00583e2.cif _cod_data_source_block cpdc-bc-Tb _cod_original_cell_volume 1298(3) _cod_database_code 7240602 _shelxl_version_number 2013-2 _chemical_oxdiff_formula 'C H O Tb Ba' _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. ; _reflns_odcompleteness_completeness 99.51 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O3) = Uanis(O4) = Uanis(O1) = Uanis(O2) Uanis(C2) = Uanis(C1) 3.a Rotating group: O7(H7A,H7B) 3.b Ternary CH refined with riding coordinates: C4(H4), C3(H3) 3.c Secondary CH2 refined with riding coordinates: C5(H5A,H5B) 3.d Aromatic/amide H refined with riding coordinates: C8(H8), C12(H12), C11(H11), C10(H10), C9(H9) ; _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 1.273 _oxdiff_exptl_absorpt_empirical_full_min 0.797 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 0.39655(7) 0.55937(7) 0.20424(4) 0.0213(3) Uani 1 1 d . . . . . O3 O 0.5970(11) 0.3491(11) 0.3466(6) 0.0286(10) Uani 1 1 d . . . . . O4 O 0.8673(11) 0.2661(11) 0.4489(6) 0.0286(10) Uani 1 1 d . . . . . O5 O 0.5941(14) 0.4966(12) 0.2289(8) 0.035(2) Uani 1 1 d . . . . . O1 O 0.6623(11) 0.7252(11) 0.3569(6) 0.0286(10) Uani 1 1 d . . . . . O2 O 0.8047(12) 0.9440(10) 0.4699(7) 0.0286(10) Uani 1 1 d . . . . . O7 O 0.1598(12) 0.4148(11) 0.1407(7) 0.032(2) Uani 1 1 d . . . . . H7A H 0.1990 0.3891 0.1930 0.048 Uiso 1 1 d GR . . . . H7B H 0.1271 0.3171 0.1082 0.048 Uiso 1 1 d GR . . . . O6 O 0.6611(12) 0.2173(11) 0.2401(7) 0.033(2) Uani 1 1 d . . . . . C2 C 0.7723(16) 0.3562(15) 0.4359(9) 0.0252(18) Uani 1 1 d . . . . . C4 C 0.8672(19) 0.4514(15) 0.5292(10) 0.030(3) Uani 1 1 d . . . . . H4 H 0.9801 0.3939 0.5978 0.036 Uiso 1 1 calc R . . . . C1 C 0.7735(16) 0.7777(15) 0.4489(8) 0.0252(18) Uani 1 1 d . . . . . C5 C 0.755(2) 0.5388(17) 0.5185(13) 0.039(3) Uani 1 1 d . . . . . H5A H 0.7971 0.5289 0.5776 0.047 Uiso 1 1 calc R . . . . H5B H 0.6223 0.5371 0.4492 0.047 Uiso 1 1 calc R . . . . C7 C 0.696(2) 0.4367(16) 0.1873(11) 0.034(3) Uani 1 1 d . . . . . C3 C 0.8644(18) 0.6570(18) 0.5328(10) 0.032(3) Uani 1 1 d . . . . . H3 H 0.9757 0.7074 0.6042 0.039 Uiso 1 1 calc R . . . . C6 C 0.6486(17) 0.3818(17) 0.2219(9) 0.028(3) Uani 1 1 d . . . . . C8 C 0.757(2) 0.314(2) 0.1783(11) 0.043(3) Uani 1 1 d . . . . . H8 H 0.7711 0.1945 0.1948 0.052 Uiso 1 1 calc R . . . . C12 C 0.677(2) 0.617(2) 0.1634(14) 0.055(4) Uani 1 1 d . . . . . H12 H 0.6400 0.7021 0.1713 0.066 Uiso 1 1 calc R . . . . C11 C 0.716(3) 0.667(3) 0.1272(15) 0.076(6) Uani 1 1 d . . . . . H11 H 0.7008 0.7860 0.1094 0.091 Uiso 1 1 calc R . . . . C10 C 0.775(3) 0.545(3) 0.1170(19) 0.080(7) Uani 1 1 d . . . . . H10 H 0.7977 0.5806 0.0916 0.096 Uiso 1 1 calc R . . . . C9 C 0.799(3) 0.370(3) 0.1446(15) 0.066(5) Uani 1 1 d . . . . . H9 H 0.8439 0.2879 0.1408 0.080 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 0.0261(4) 0.0038(4) 0.0283(4) -0.0002(2) 0.0222(4) -0.0004(2) O3 0.034(2) 0.012(2) 0.032(2) -0.0012(18) 0.027(2) -0.0005(18) O4 0.034(2) 0.012(2) 0.032(2) -0.0012(18) 0.027(2) -0.0005(18) O5 0.049(6) 0.009(4) 0.054(6) -0.001(4) 0.045(5) 0.003(4) O1 0.034(2) 0.012(2) 0.032(2) -0.0012(18) 0.027(2) -0.0005(18) O2 0.034(2) 0.012(2) 0.032(2) -0.0012(18) 0.027(2) -0.0005(18) O7 0.037(5) 0.012(4) 0.040(5) -0.007(4) 0.031(5) -0.009(4) O6 0.045(5) 0.010(4) 0.052(5) 0.005(4) 0.043(5) 0.003(4) C2 0.027(4) 0.010(4) 0.026(4) -0.001(3) 0.021(4) 0.001(3) C4 0.039(7) 0.013(6) 0.032(6) 0.009(5) 0.030(6) 0.009(5) C1 0.027(4) 0.010(4) 0.026(4) -0.001(3) 0.021(4) 0.001(3) C5 0.064(10) 0.015(6) 0.052(8) 0.008(6) 0.051(8) 0.008(6) C7 0.040(8) 0.020(7) 0.037(7) 0.004(5) 0.032(7) 0.007(5) C3 0.043(7) 0.022(7) 0.033(6) 0.001(5) 0.032(6) 0.004(6) C6 0.036(7) 0.015(6) 0.033(6) 0.001(5) 0.029(6) 0.003(5) C8 0.071(10) 0.024(7) 0.062(8) -0.011(7) 0.061(9) -0.008(7) C12 0.076(12) 0.023(7) 0.084(11) 0.009(8) 0.071(11) 0.002(8) C11 0.119(17) 0.048(11) 0.097(14) -0.002(11) 0.098(15) -0.013(12) C10 0.122(19) 0.068(15) 0.102(16) -0.017(12) 0.103(17) -0.031(13) C9 0.083(13) 0.064(13) 0.095(13) -0.003(12) 0.083(13) 0.004(12) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O3 141.15(17) . 2_655 ? O3 Tb1 O4 164.6(3) . 2_655 ? O3 Tb1 O4 51.4(3) 2_655 2_655 ? O3 Tb1 O1 67.0(3) . 2_645 ? O3 Tb1 O1 131.5(3) 2_655 2_645 ? O3 Tb1 O2 117.1(3) . 2_645 ? O3 Tb1 O7 85.0(4) . . ? O3 Tb1 C2 26.4(3) 2_655 2_655 ? O3 Tb1 C2 167.5(3) . 2_655 ? O3 Tb1 C1 109.2(3) 2_655 2_645 ? O3 Tb1 C1 92.2(3) . 2_645 ? O4 Tb1 O1 112.7(3) 2_655 2_645 ? O4 Tb1 C2 25.8(3) 2_655 2_655 ? O4 Tb1 C1 89.3(4) 2_655 2_645 ? O5 Tb1 O3 79.3(4) . . ? O5 Tb1 O3 77.1(3) . 2_655 ? O5 Tb1 O4 115.6(3) . 2_655 ? O5 Tb1 O1 71.9(3) . 2_645 ? O5 Tb1 O1 76.3(4) . . ? O5 Tb1 O2 75.7(4) . 2_645 ? O5 Tb1 O7 139.0(3) . . ? O5 Tb1 O6 148.3(3) . 2_655 ? O5 Tb1 C2 93.8(4) . 2_655 ? O5 Tb1 C1 72.2(4) . 2_645 ? O1 Tb1 O3 75.1(4) . . ? O1 Tb1 O3 69.6(3) . 2_655 ? O1 Tb1 O4 110.8(4) . 2_655 ? O1 Tb1 O1 133.9(2) . 2_645 ? O1 Tb1 O2 146.3(3) . 2_645 ? O1 Tb1 O7 135.2(3) . . ? O1 Tb1 O6 72.0(3) . 2_655 ? O1 Tb1 C2 93.2(4) . 2_655 ? O1 Tb1 C2 121.1(3) 2_645 2_655 ? O1 Tb1 C1 147.7(3) . 2_645 ? O1 Tb1 C1 25.4(3) 2_645 2_645 ? O2 Tb1 O3 86.3(3) 2_645 2_655 ? O2 Tb1 O4 66.3(3) 2_645 2_655 ? O2 Tb1 O1 50.5(2) 2_645 2_645 ? O2 Tb1 C2 70.6(3) 2_645 2_655 ? O2 Tb1 C1 25.1(3) 2_645 2_645 ? O7 Tb1 O3 132.1(3) . 2_655 ? O7 Tb1 O4 81.1(4) . 2_655 ? O7 Tb1 O1 67.1(3) . 2_645 ? O7 Tb1 O2 78.4(4) . 2_645 ? O7 Tb1 C2 106.8(4) . 2_655 ? O7 Tb1 C1 70.9(4) . 2_645 ? O6 Tb1 O3 90.6(3) 2_655 2_655 ? O6 Tb1 O3 93.5(3) 2_655 . ? O6 Tb1 O4 75.6(3) 2_655 2_655 ? O6 Tb1 O1 133.5(3) 2_655 2_645 ? O6 Tb1 O2 133.3(3) 2_655 2_645 ? O6 Tb1 O7 69.6(3) 2_655 . ? O6 Tb1 C2 86.9(3) 2_655 2_655 ? O6 Tb1 C1 139.4(3) 2_655 2_645 ? C2 Tb1 C1 95.7(4) 2_655 2_645 ? Tb1 O3 Tb1 110.4(3) . 2_645 ? C2 O3 Tb1 127.6(7) . . ? C2 O3 Tb1 92.8(7) . 2_645 ? C2 O4 Tb1 92.9(7) . 2_645 ? C6 O5 Tb1 146.0(9) . . ? Tb1 O1 Tb1 107.1(3) . 2_655 ? C1 O1 Tb1 91.1(7) . 2_655 ? C1 O1 Tb1 147.7(8) . . ? C1 O2 Tb1 98.9(7) . 2_655 ? Tb1 O7 H7A 110.1 . . ? Tb1 O7 H7B 109.9 . . ? H7A O7 H7B 108.9 . . ? C6 O6 Tb1 131.6(8) . 2_645 ? O3 C2 Tb1 60.8(6) . 2_645 ? O3 C2 C4 121.9(11) . . ? O4 C2 Tb1 61.3(6) . 2_645 ? O4 C2 O3 119.2(10) . . ? O4 C2 C4 118.6(11) . . ? C4 C2 Tb1 156.8(8) . 2_645 ? C2 C4 H4 115.0 . . ? C2 C4 C3 121.6(10) . . ? C5 C4 C2 119.1(12) . . ? C5 C4 H4 115.0 . . ? C5 C4 C3 60.1(8) . . ? C3 C4 H4 115.0 . . ? O1 C1 Tb1 63.5(6) . 2_655 ? O1 C1 C3 123.6(11) . . ? O2 C1 Tb1 56.0(6) . 2_655 ? O2 C1 O1 119.5(11) . . ? O2 C1 C3 116.9(10) . . ? C3 C1 Tb1 172.7(8) . 2_655 ? C4 C5 H5A 117.6 . . ? C4 C5 H5B 117.6 . . ? C4 C5 C3 61.5(9) . . ? H5A C5 H5B 114.7 . . ? C3 C5 H5A 117.6 . . ? C3 C5 H5B 117.6 . . ? C8 C7 C6 121.7(12) . . ? C8 C7 C12 119.5(14) . . ? C12 C7 C6 118.8(13) . . ? C4 C3 H3 113.8 . . ? C1 C3 C4 124.9(10) . . ? C1 C3 C5 121.3(12) . . ? C1 C3 H3 113.8 . . ? C5 C3 C4 58.4(9) . . ? C5 C3 H3 113.8 . . ? O5 C6 O6 123.1(13) . . ? O5 C6 C7 119.1(12) . . ? O6 C6 C7 117.7(11) . . ? C7 C8 H8 119.9 . . ? C7 C8 C9 120.3(15) . . ? C9 C8 H8 119.9 . . ? C7 C12 H12 120.8 . . ? C11 C12 C7 118.4(17) . . ? C11 C12 H12 120.8 . . ? C12 C11 H11 119.0 . . ? C10 C11 C12 122.0(19) . . ? C10 C11 H11 119.0 . . ? C11 C10 H10 120.5 . . ? C9 C10 C11 119.0(18) . . ? C9 C10 H10 120.5 . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.8(18) . . ? C10 C9 H9 119.6 . . ? 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 O3 2.517(8) 2_655 ? Tb1 O3 2.388(10) . ? Tb1 O4 2.528(10) 2_655 ? Tb1 O5 2.294(10) . ? Tb1 O1 2.644(8) 2_645 ? Tb1 O1 2.359(11) . ? Tb1 O2 2.479(11) 2_645 ? Tb1 O7 2.390(9) . ? Tb1 O6 2.363(8) 2_655 ? Tb1 C2 2.880(12) 2_655 ? Tb1 C1 2.954(12) 2_645 ? O3 Tb1 2.517(8) 2_645 ? O3 C2 1.281(15) . ? O4 Tb1 2.528(10) 2_645 ? O4 C2 1.256(14) . ? O5 C6 1.240(15) . ? O1 Tb1 2.644(8) 2_655 ? O1 C1 1.270(13) . ? O2 Tb1 2.479(11) 2_655 ? O2 C1 1.268(13) . ? O7 H7A 0.8622 . ? O7 H7B 0.8621 . ? O6 Tb1 2.363(8) 2_645 ? O6 C6 1.263(15) . ? C2 Tb1 2.880(12) 2_645 ? C2 C4 1.494(17) . ? C4 H4 0.9800 . ? C4 C5 1.49(2) . ? C4 C3 1.538(18) . ? C1 Tb1 2.954(12) 2_655 ? C1 C3 1.460(16) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C3 1.52(2) . ? C7 C6 1.478(19) . ? C7 C8 1.383(19) . ? C7 C12 1.399(19) . ? C3 H3 0.9800 . ? C8 H8 0.9300 . ? C8 C9 1.39(2) . ? C12 H12 0.9300 . ? C12 C11 1.39(2) . ? C11 H11 0.9300 . ? C11 C10 1.37(3) . ? C10 H10 0.9300 . ? C10 C9 1.37(3) . ? C9 H9 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 O3 C2 Tb1 -118.5(8) . . . 2_645 ? Tb1 O3 C2 O4 -99.0(11) . . . . ? Tb1 O3 C2 O4 19.5(11) 2_645 . . . ? Tb1 O3 C2 C4 88.3(13) . . . . ? Tb1 O3 C2 C4 -153.2(10) 2_645 . . . ? Tb1 O4 C2 O3 -19.4(11) 2_645 . . . ? Tb1 O4 C2 C4 153.5(10) 2_645 . . . ? Tb1 O5 C6 O6 -36(2) . . . . ? Tb1 O5 C6 C7 142.2(13) . . . . ? Tb1 O1 C1 Tb1 -125.6(14) . . . 2_655 ? Tb1 O1 C1 O2 -125.2(13) . . . . ? Tb1 O1 C1 O2 0.4(12) 2_655 . . . ? Tb1 O1 C1 C3 177.8(11) 2_655 . . . ? Tb1 O1 C1 C3 52(2) . . . . ? Tb1 O2 C1 O1 -0.4(13) 2_655 . . . ? Tb1 O2 C1 C3 -178.0(10) 2_655 . . . ? Tb1 O6 C6 O5 -2(2) 2_645 . . . ? Tb1 O6 C6 C7 -179.9(8) 2_645 . . . ? Tb1 C2 C4 C5 -89(2) 2_645 . . . ? Tb1 C2 C4 C3 -159.9(16) 2_645 . . . ? O3 C2 C4 C5 0.7(17) . . . . ? O3 C2 C4 C3 -70.3(17) . . . . ? O4 C2 C4 C5 -172.1(11) . . . . ? O4 C2 C4 C3 116.9(13) . . . . ? O1 C1 C3 C4 12(2) . . . . ? O1 C1 C3 C5 -59.3(18) . . . . ? O2 C1 C3 C4 -170.8(12) . . . . ? O2 C1 C3 C5 118.1(13) . . . . ? C2 C4 C5 C3 -111.9(12) . . . . ? C2 C4 C3 C1 -1(2) . . . . ? C2 C4 C3 C5 107.7(15) . . . . ? C4 C5 C3 C1 114.3(13) . . . . ? C5 C4 C3 C1 -108.3(15) . . . . ? C7 C8 C9 C10 -2(3) . . . . ? C7 C12 C11 C10 -2(3) . . . . ? C6 C7 C8 C9 179.4(14) . . . . ? C6 C7 C12 C11 -177.8(15) . . . . ? C8 C7 C6 O5 179.9(13) . . . . ? C8 C7 C6 O6 -2(2) . . . . ? C8 C7 C12 C11 2(2) . . . . ? C12 C7 C6 O5 0(2) . . . . ? C12 C7 C6 O6 177.9(13) . . . . ? C12 C7 C8 C9 -1(2) . . . . ? C12 C11 C10 C9 -1(4) . . . . ? C11 C10 C9 C8 3(3) . . . . ?