#------------------------------------------------------------------------------ #$Date: 2019-11-17 12:09:43 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229792 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045422.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_7045422 loop_ _publ_author_name 'Cadman, Laura K.' 'Mahon, Mary F.' 'Burrows, Andrew D.' _publ_section_title ; The effect of metal distribution on the luminescence properties of mixed-lanthanide metal-organic frameworks. ; _journal_issue 7 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 2360 _journal_page_last 2367 _journal_paper_doi 10.1039/c7dt04583b _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C16 H9 O10 Tb, H2 O, O' _chemical_formula_sum 'C16 H13 O12 Tb' _chemical_formula_weight 556.18 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2017-11-21 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2017-11-21 deposited with the CCDC. 2018-01-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.8140(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8243(2) _cell_length_b 12.7350(3) _cell_length_c 13.9772(3) _cell_measurement_reflns_used 3136 _cell_measurement_temperature 150.01(10) _cell_measurement_theta_max 72.7740 _cell_measurement_theta_min 4.6890 _cell_volume 1744.85(7) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 150.00(10) _diffrn_detector_area_resol_mean 8.1150 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 7002 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.836 _diffrn_reflns_theta_min 4.702 _exptl_absorpt_coefficient_mu 20.585 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.117 _exptl_crystal_description block _exptl_crystal_F_000 1080 _exptl_crystal_size_max 0.079 _exptl_crystal_size_mid 0.054 _exptl_crystal_size_min 0.029 _refine_diff_density_max 0.541 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.122 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 270 _refine_ls_number_reflns 3383 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0382 _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^)+(0.0230P)^2^+4.8480P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.0824 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2881 _reflns_number_total 3383 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL s16lkc10 in P21/n #14 REM reset to P21/n #14 CELL 1.54184 9.824269 12.735004 13.977234 90 93.814 90 ZERR 4 0.000223 0.00029 0.00031 0 0.0019 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O Tb UNIT 64 52 48 4 DFIX 0.98 0.005 O9 H9 EADP O12A O12 L.S. 10 PLAN 2 TEMP -100 HTAB GRID MORE -1 BOND $H CONF fmap 2 acta MERG 2 OMIT 6 1 0 OMIT 6 8 1 REM REM REM WGHT 0.023000 4.848000 FVAR 3.32242 TB1 4 0.228015 0.003136 0.416487 11.00000 0.00779 0.00654 = 0.00747 0.00078 0.00061 0.00171 O1 3 0.077773 -0.020152 0.277423 11.00000 0.01520 0.00839 = 0.01249 0.00466 -0.00237 -0.00150 O2 3 0.210505 0.119194 0.271387 11.00000 0.01250 0.01103 = 0.00989 0.00040 -0.00295 0.00063 O3 3 0.107171 0.388179 0.015904 11.00000 0.01175 0.01171 = 0.01367 0.00195 -0.00324 -0.00631 O4 3 -0.090488 0.378631 -0.070203 11.00000 0.01191 0.01009 = 0.01055 0.00313 -0.00149 -0.00082 O5 3 -0.247227 0.009719 -0.021241 11.00000 0.01608 0.01082 = 0.00866 -0.00022 0.00151 -0.00645 O6 3 -0.401762 -0.364331 -0.042165 11.00000 0.01787 0.00817 = 0.01905 -0.00462 0.00365 -0.00232 O7 3 -0.570677 -0.373136 0.055943 11.00000 0.01597 0.01337 = 0.01485 -0.00335 0.00681 -0.00695 O8 3 -0.632761 -0.069001 0.285972 11.00000 0.01427 0.01065 = 0.00882 0.00118 0.00186 0.00065 O9 3 -0.466518 0.051417 0.284774 11.00000 0.01738 0.01787 = 0.02222 -0.01251 0.00721 -0.00732 AFIX 147 0.9500 H9 2 -0.508772 0.076802 0.339432 11.00000 -1.50000 AFIX 0 O10 3 0.240303 0.036257 0.586300 11.00000 0.03033 0.02970 = 0.01430 -0.00369 0.00087 0.01966 AFIX 7 H10A 2 0.314985 0.007349 0.613930 11.00000 -1.50000 H10B 2 0.224780 0.088897 0.612070 11.00000 -1.50000 AFIX 6 O11 3 0.060047 -0.230350 0.237479 11.00000 0.06581 0.02859 = 0.05425 -0.01156 0.02353 -0.00542 H11A 2 0.131995 -0.269793 0.234925 11.00000 -1.50000 H11B 2 0.084969 -0.165611 0.247982 11.00000 -1.50000 AFIX 0 PART 1 O12 3 -0.177649 -0.222711 0.326902 10.80000 0.04098 0.03138 = 0.04136 -0.00952 0.02021 -0.00581 PART 0 PART 2 O12A 3 -0.140185 -0.178352 0.286965 10.20000 0.04098 0.03138 = 0.04136 -0.00952 0.02021 -0.00581 PART 0 C1 1 0.110624 0.065119 0.237475 11.00000 0.01225 0.01072 = 0.00797 0.00117 -0.00023 0.00249 C2 1 0.026024 0.103476 0.151415 11.00000 0.00896 0.01239 = 0.00833 0.00040 0.00166 0.00253 C3 1 0.049461 0.202105 0.113581 11.00000 0.00831 0.00942 = 0.01081 -0.00170 0.00034 -0.00174 AFIX 43 H3 2 0.119281 0.245795 0.142092 11.00000 -1.20000 AFIX 0 C4 1 -0.029877 0.236452 0.033762 11.00000 0.00999 0.00468 = 0.01201 0.00235 0.00225 -0.00168 C5 1 -0.131567 0.172665 -0.009427 11.00000 0.00580 0.01083 = 0.01115 0.00280 0.00036 -0.00030 AFIX 43 H5 2 -0.185730 0.196479 -0.063978 11.00000 -1.20000 AFIX 0 C6 1 -0.152264 0.074079 0.028512 11.00000 0.00927 0.01100 = 0.00863 -0.00155 0.00435 -0.00204 C7 1 -0.075335 0.038670 0.108373 11.00000 0.01022 0.00876 = 0.00956 0.00172 0.00280 0.00135 AFIX 43 H7 2 -0.091152 -0.029087 0.133813 11.00000 -1.20000 AFIX 0 C8 1 -0.002105 0.342101 -0.009001 11.00000 0.01152 0.00768 = 0.00598 0.00283 0.00259 -0.00157 C9 1 -0.329636 -0.051108 0.032740 11.00000 0.00840 0.00942 = 0.01002 0.00001 -0.00144 -0.00269 C10 1 -0.359678 -0.152805 0.001144 11.00000 0.00608 0.01097 = 0.01051 -0.00129 0.00303 0.00206 AFIX 43 H10 2 -0.319900 -0.179792 -0.053889 11.00000 -1.20000 AFIX 0 C11 1 -0.447984 -0.214382 0.050512 11.00000 0.00857 0.00708 = 0.01302 -0.00325 0.00267 -0.00102 C12 1 -0.506834 -0.175688 0.130806 11.00000 0.00962 0.01093 = 0.01204 0.00237 0.00130 -0.00036 AFIX 43 H12 2 -0.568399 -0.217688 0.163857 11.00000 -1.20000 AFIX 0 C13 1 -0.474316 -0.073934 0.162501 11.00000 0.00836 0.01040 = 0.01028 0.00103 0.00192 0.00259 C14 1 -0.385199 -0.011955 0.113530 11.00000 0.01051 0.00897 = 0.01347 -0.00421 0.00040 0.00202 AFIX 43 H14 2 -0.362783 0.056857 0.135594 11.00000 -1.20000 AFIX 0 C15 1 -0.475197 -0.325744 0.018575 11.00000 0.01097 0.00884 = 0.00948 -0.00177 -0.00126 -0.00289 C16 1 -0.534624 -0.031305 0.249431 11.00000 0.01193 0.00693 = 0.01278 0.00010 -0.00118 0.00367 HKLF 4 REM s16lkc10 in P21/n #14 REM R1 = 0.0382 for 2881 Fo > 4sig(Fo) and 0.0460 for all 3383 data REM 270 parameters refined using 1 restraints END WGHT 0.0233 4.8480 REM Instructions for potential hydrogen bonds EQIV $1 x-1/2, -y+1/2, z+1/2 HTAB O9 O4_$1 EQIV $2 -x, -y, -z+1 HTAB O10 O9_$2 HTAB O10 O12_$2 HTAB O10 O12A_$2 EQIV $3 -x+1/2, y-1/2, -z+1/2 HTAB O11 O2_$3 HTAB O11 O1 REM Highest difference peak 0.541, deepest hole -0.557, 1-sigma level 0.122 Q1 1 0.1213 -0.0156 0.4158 11.00000 0.05 0.54 Q2 1 0.0573 0.0195 0.5891 11.00000 0.05 0.51 REM The information below was added by Olex2. REM REM R1 = 0.0382 for 2881 Fo > 4sig(Fo) and 0.0460 for all 7233 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.54, deepest hole -0.56 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0460 REM R1_gt = 0.0382 REM wR_ref = 0.0824 REM GOOF = 1.143 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 7233 REM Reflections_gt = 2881 REM Parameters = n/a REM Hole = -0.56 REM Peak = 0.54 REM Flack = n/a ; _cod_data_source_file c7dt04583b2.cif _cod_data_source_block s16lkc10-Cpd-4 _cod_depositor_comments 'Adding full bibliography for 7045418--7045423.cif.' _cod_database_code 7045422 _shelxl_version_number 2014-3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2. Restrained distances O9-H9 0.98 with sigma of 0.005 3. Uiso/Uaniso restraints and constraints Uanis(O12A) = Uanis(O12) 4. Others Fixed Sof: O12(0.8) O12A(0.2) 5.a Free rotating group: O11(H11A,H11B) 5.b Rotating group: O10(H10A,H10B) 5.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14) 5.d Idealised tetrahedral OH refined as rotating group: O9(H9) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.22802(3) 0.00314(2) 0.41649(2) 0.00726(9) Uani 1 1 d . . . . O1 O 0.0778(3) -0.0202(3) 0.2774(2) 0.0122(7) Uani 1 1 d . . . . O2 O 0.2105(3) 0.1192(3) 0.2714(2) 0.0113(7) Uani 1 1 d . . . . O3 O 0.1072(3) 0.3882(3) 0.0159(2) 0.0126(7) Uani 1 1 d . . . . O4 O -0.0905(3) 0.3786(3) -0.0702(2) 0.0109(7) Uani 1 1 d . . . . O5 O -0.2472(3) 0.0097(3) -0.0212(2) 0.0118(7) Uani 1 1 d . . . . O6 O -0.4018(4) -0.3643(3) -0.0422(3) 0.0149(7) Uani 1 1 d . . . . O7 O -0.5707(4) -0.3731(3) 0.0559(3) 0.0145(7) Uani 1 1 d . . . . O8 O -0.6328(3) -0.0690(3) 0.2860(2) 0.0112(7) Uani 1 1 d . . . . O9 O -0.4665(4) 0.0514(3) 0.2848(3) 0.0189(8) Uani 1 1 d D . . . H9 H -0.5088 0.0768 0.3394 0.028 Uiso 1 1 calc DGR . . . O10 O 0.2403(4) 0.0363(3) 0.5863(3) 0.0248(9) Uani 1 1 d . . . . H10A H 0.3150 0.0073 0.6139 0.037 Uiso 1 1 d GR . . . H10B H 0.2248 0.0889 0.6121 0.037 Uiso 1 1 d GR . . . O11 O 0.0600(6) -0.2303(4) 0.2375(4) 0.0487(14) Uani 1 1 d . . . . H11A H 0.1320 -0.2698 0.2349 0.073 Uiso 1 1 d G . . . H11B H 0.0850 -0.1656 0.2480 0.073 Uiso 1 1 d G . . . O12 O -0.1776(6) -0.2227(5) 0.3269(5) 0.0371(14) Uani 0.8 1 d . P A 1 O12A O -0.140(3) -0.178(2) 0.2870(19) 0.0371(14) Uani 0.2 1 d . P B 2 C1 C 0.1106(5) 0.0651(4) 0.2375(3) 0.0104(9) Uani 1 1 d . . . . C2 C 0.0260(5) 0.1035(4) 0.1514(3) 0.0098(9) Uani 1 1 d . . . . C3 C 0.0495(5) 0.2021(4) 0.1136(3) 0.0095(9) Uani 1 1 d . . . . H3 H 0.1193 0.2458 0.1421 0.011 Uiso 1 1 calc R . . . C4 C -0.0299(5) 0.2365(4) 0.0338(3) 0.0088(9) Uani 1 1 d . . . . C5 C -0.1316(5) 0.1727(4) -0.0094(3) 0.0093(9) Uani 1 1 d . . . . H5 H -0.1857 0.1965 -0.0640 0.011 Uiso 1 1 calc R . . . C6 C -0.1523(5) 0.0741(4) 0.0285(3) 0.0095(9) Uani 1 1 d . . . . C7 C -0.0753(5) 0.0387(4) 0.1084(3) 0.0094(9) Uani 1 1 d . . . . H7 H -0.0912 -0.0291 0.1338 0.011 Uiso 1 1 calc R . . . C8 C -0.0021(5) 0.3421(4) -0.0090(3) 0.0083(9) Uani 1 1 d . . . . C9 C -0.3296(5) -0.0511(4) 0.0327(3) 0.0094(9) Uani 1 1 d . . . . C10 C -0.3597(5) -0.1528(4) 0.0011(3) 0.0091(9) Uani 1 1 d . . . . H10 H -0.3199 -0.1798 -0.0539 0.011 Uiso 1 1 calc R . . . C11 C -0.4480(5) -0.2144(4) 0.0505(3) 0.0095(9) Uani 1 1 d . . . . C12 C -0.5068(5) -0.1757(4) 0.1308(3) 0.0108(9) Uani 1 1 d . . . . H12 H -0.5684 -0.2177 0.1639 0.013 Uiso 1 1 calc R . . . C13 C -0.4743(5) -0.0739(4) 0.1625(3) 0.0096(9) Uani 1 1 d . . . . C14 C -0.3852(5) -0.0120(4) 0.1135(3) 0.0110(9) Uani 1 1 d . . . . H14 H -0.3628 0.0569 0.1356 0.013 Uiso 1 1 calc R . . . C15 C -0.4752(5) -0.3257(4) 0.0186(3) 0.0099(9) Uani 1 1 d . . . . C16 C -0.5346(5) -0.0313(4) 0.2494(3) 0.0106(9) 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 Tb1 0.00779(14) 0.00654(14) 0.00747(13) 0.00078(11) 0.00061(9) 0.00171(11) O1 0.0152(17) 0.0084(16) 0.0125(16) 0.0047(13) -0.0024(13) -0.0015(13) O2 0.0125(16) 0.0110(16) 0.0099(15) 0.0004(13) -0.0029(12) 0.0006(14) O3 0.0118(17) 0.0117(16) 0.0137(16) 0.0019(14) -0.0032(13) -0.0063(14) O4 0.0119(16) 0.0101(16) 0.0105(16) 0.0031(13) -0.0015(12) -0.0008(13) O5 0.0161(17) 0.0108(16) 0.0087(15) -0.0002(13) 0.0015(12) -0.0064(14) O6 0.0179(18) 0.0082(16) 0.0190(18) -0.0046(14) 0.0037(14) -0.0023(14) O7 0.0160(18) 0.0134(17) 0.0148(17) -0.0033(14) 0.0068(14) -0.0069(14) O8 0.0143(17) 0.0106(16) 0.0088(16) 0.0012(13) 0.0019(13) 0.0006(14) O9 0.0174(18) 0.0179(18) 0.0222(19) -0.0125(16) 0.0072(15) -0.0073(16) O10 0.030(2) 0.030(2) 0.0143(18) -0.0037(16) 0.0009(15) 0.0197(18) O11 0.066(4) 0.029(3) 0.054(3) -0.012(3) 0.024(3) -0.005(3) O12 0.041(3) 0.031(3) 0.041(4) -0.010(3) 0.020(3) -0.006(3) O12A 0.041(3) 0.031(3) 0.041(4) -0.010(3) 0.020(3) -0.006(3) C1 0.012(2) 0.011(2) 0.008(2) 0.0012(18) -0.0002(17) 0.0025(18) C2 0.009(2) 0.012(2) 0.008(2) 0.0004(18) 0.0017(17) 0.0025(18) C3 0.008(2) 0.009(2) 0.011(2) -0.0017(18) 0.0003(17) -0.0017(18) C4 0.010(2) 0.005(2) 0.012(2) 0.0023(18) 0.0023(17) -0.0017(17) C5 0.006(2) 0.011(2) 0.011(2) 0.0028(18) 0.0004(17) -0.0003(18) C6 0.009(2) 0.011(2) 0.009(2) -0.0016(18) 0.0043(17) -0.0020(18) C7 0.010(2) 0.009(2) 0.010(2) 0.0017(18) 0.0028(17) 0.0013(18) C8 0.012(2) 0.008(2) 0.006(2) 0.0028(17) 0.0026(16) -0.0016(18) C9 0.008(2) 0.009(2) 0.010(2) 0.0000(18) -0.0014(17) -0.0027(18) C10 0.006(2) 0.011(2) 0.011(2) -0.0013(18) 0.0030(16) 0.0021(18) C11 0.009(2) 0.007(2) 0.013(2) -0.0032(18) 0.0027(17) -0.0010(17) C12 0.010(2) 0.011(2) 0.012(2) 0.0024(19) 0.0013(17) -0.0004(18) C13 0.008(2) 0.010(2) 0.010(2) 0.0010(18) 0.0019(17) 0.0026(18) C14 0.011(2) 0.009(2) 0.013(2) -0.0042(19) 0.0004(17) 0.0020(18) C15 0.011(2) 0.009(2) 0.009(2) -0.0018(18) -0.0013(17) -0.0029(18) C16 0.012(2) 0.007(2) 0.013(2) 0.0001(18) -0.0012(18) 0.0037(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -9.1472 9.1891 '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 53.63(11) . . O1 Tb1 O8 72.60(11) . 1_655 O1 Tb1 O10 144.62(13) . . O1 Tb1 C1 26.93(13) . . O2 Tb1 O8 68.97(11) . 1_655 O2 Tb1 C1 26.87(13) . . O3 Tb1 O1 128.91(12) 2_545 . O3 Tb1 O2 134.87(12) 2_545 . O3 Tb1 O8 70.73(11) 2_545 1_655 O3 Tb1 O10 73.90(12) 2_545 . O3 Tb1 C1 140.54(13) 2_545 . O4 Tb1 O1 125.11(11) 4_666 . O4 Tb1 O2 72.22(11) 4_666 . O4 Tb1 O3 82.33(12) 4_666 2_545 O4 Tb1 O8 81.05(11) 4_666 1_655 O4 Tb1 O10 79.64(14) 4_666 . O4 Tb1 C1 99.02(13) 4_666 . O6 Tb1 O1 77.48(12) 4_656 . O6 Tb1 O2 130.84(12) 4_656 . O6 Tb1 O3 78.20(13) 4_656 2_545 O6 Tb1 O4 156.84(12) 4_656 4_666 O6 Tb1 O8 103.91(12) 4_656 1_655 O6 Tb1 O10 82.98(14) 4_656 . O6 Tb1 C1 103.98(14) 4_656 . O7 Tb1 O1 80.32(13) 2_455 . O7 Tb1 O2 73.48(12) 2_455 . O7 Tb1 O3 146.34(12) 2_455 2_545 O7 Tb1 O4 93.69(12) 2_455 4_666 O7 Tb1 O6 95.58(13) 2_455 4_656 O7 Tb1 O8 141.91(11) 2_455 1_655 O7 Tb1 O10 72.50(13) 2_455 . O7 Tb1 C1 73.12(13) 2_455 . O8 Tb1 C1 70.58(12) 1_655 . O10 Tb1 O2 133.73(12) . . O10 Tb1 O8 141.50(12) . 1_655 O10 Tb1 C1 145.42(13) . . C1 O1 Tb1 95.2(3) . . C1 O2 Tb1 89.5(3) . . C8 O3 Tb1 164.7(3) . 2 C8 O4 Tb1 141.0(3) . 4_565 C9 O5 C6 117.1(4) . . C15 O6 Tb1 146.7(3) . 4 C15 O7 Tb1 160.6(3) . 2_445 C16 O8 Tb1 129.9(3) . 1_455 C16 O9 H9 109.5 . . Tb1 O10 H10A 110.1 . . Tb1 O10 H10B 127.4 . . H10A O10 H10B 109.7 . . H11A O11 H11B 109.5 . . O1 C1 Tb1 57.9(2) . . O1 C1 C2 119.2(4) . . O2 C1 Tb1 63.6(2) . . O2 C1 O1 120.9(4) . . O2 C1 C2 119.9(4) . . C2 C1 Tb1 169.7(3) . . C3 C2 C1 120.3(4) . . C3 C2 C7 120.1(4) . . C7 C2 C1 119.6(4) . . C2 C3 H3 120.2 . . C2 C3 C4 119.5(4) . . C4 C3 H3 120.2 . . C3 C4 C5 120.8(4) . . C3 C4 C8 119.6(4) . . C5 C4 C8 119.5(4) . . C4 C5 H5 120.6 . . C6 C5 C4 118.8(4) . . C6 C5 H5 120.6 . . C5 C6 O5 117.0(4) . . C7 C6 O5 121.6(4) . . C7 C6 C5 121.3(4) . . C2 C7 H7 120.3 . . C6 C7 C2 119.4(4) . . C6 C7 H7 120.3 . . O3 C8 O4 123.5(4) . . O3 C8 C4 118.9(4) . . O4 C8 C4 117.6(4) . . O5 C9 C10 117.9(4) . . C14 C9 O5 121.5(4) . . C14 C9 C10 120.5(4) . . C9 C10 H10 120.2 . . C11 C10 C9 119.6(4) . . C11 C10 H10 120.2 . . C10 C11 C15 119.3(4) . . C12 C11 C10 120.7(4) . . C12 C11 C15 120.0(4) . . C11 C12 H12 120.4 . . C11 C12 C13 119.1(4) . . C13 C12 H12 120.4 . . C12 C13 C16 120.1(4) . . C14 C13 C12 120.5(4) . . C14 C13 C16 119.5(4) . . C9 C14 C13 119.6(4) . . C9 C14 H14 120.2 . . C13 C14 H14 120.2 . . O6 C15 O7 125.0(5) . . O6 C15 C11 118.2(4) . . O7 C15 C11 116.8(4) . . O8 C16 O9 123.4(5) . . O8 C16 C13 124.5(4) . . O9 C16 C13 112.0(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Tb1 O1 2.380(3) . Tb1 O2 2.506(3) . Tb1 O3 2.335(3) 2_545 Tb1 O4 2.332(3) 4_666 Tb1 O6 2.277(3) 4_656 Tb1 O7 2.258(3) 2_455 Tb1 O8 2.525(3) 1_655 Tb1 O10 2.406(4) . Tb1 C1 2.798(5) . O1 C1 1.272(6) . O2 C1 1.265(6) . O3 Tb1 2.336(3) 2 O3 C8 1.252(6) . O4 Tb1 2.332(3) 4_565 O4 C8 1.266(6) . O5 C6 1.393(6) . O5 C9 1.381(6) . O6 Tb1 2.276(3) 4 O6 C15 1.251(6) . O7 Tb1 2.258(3) 2_445 O7 C15 1.258(6) . O8 Tb1 2.525(3) 1_455 O8 C16 1.219(6) . O9 H9 0.9501 . O9 C16 1.326(6) . O10 H10A 0.8862 . O10 H10B 0.7808 . O11 H11A 0.8698 . O11 H11B 0.8697 . C1 C2 1.498(6) . C2 C3 1.388(7) . C2 C7 1.398(7) . C3 H3 0.9500 . C3 C4 1.388(7) . C4 C5 1.394(6) . C4 C8 1.505(6) . C5 H5 0.9500 . C5 C6 1.383(7) . C6 C7 1.381(7) . C7 H7 0.9500 . C9 C10 1.394(7) . C9 C14 1.380(6) . C10 H10 0.9500 . C10 C11 1.387(7) . C11 C12 1.387(6) . C11 C15 1.505(6) . C12 H12 0.9500 . C12 C13 1.400(7) . C13 C14 1.392(7) . C13 C16 1.489(6) . C14 H14 0.9500 . 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 O1 C1 O2 9.1(5) . Tb1 O1 C1 C2 -168.5(4) . Tb1 O2 C1 O1 -8.6(5) . Tb1 O2 C1 C2 169.0(4) . Tb1 O3 C8 O4 73.1(13) 2 Tb1 O3 C8 C4 -108.4(12) 2 Tb1 O4 C8 O3 -82.0(6) 4_565 Tb1 O4 C8 C4 99.4(5) 4_565 Tb1 O6 C15 O7 -48.2(9) 4 Tb1 O6 C15 C11 131.5(5) 4 Tb1 O7 C15 O6 -10.9(14) 2_445 Tb1 O7 C15 C11 169.5(8) 2_445 Tb1 O8 C16 O9 12.0(7) 1_455 Tb1 O8 C16 C13 -170.1(3) 1_455 Tb1 C1 C2 C3 101.7(19) . Tb1 C1 C2 C7 -79(2) . O1 C1 C2 C3 172.2(4) . O1 C1 C2 C7 -8.9(7) . O2 C1 C2 C3 -5.5(7) . O2 C1 C2 C7 173.5(4) . O5 C6 C7 C2 175.1(4) . O5 C9 C10 C11 -176.5(4) . O5 C9 C14 C13 176.1(4) . C1 C2 C3 C4 180.0(4) . C1 C2 C7 C6 -179.4(4) . C2 C3 C4 C5 -0.8(7) . C2 C3 C4 C8 -178.3(4) . C3 C2 C7 C6 -0.5(7) . C3 C4 C5 C6 -0.1(7) . C3 C4 C8 O3 13.7(7) . C3 C4 C8 O4 -167.7(4) . C4 C5 C6 O5 -175.0(4) . C4 C5 C6 C7 0.7(7) . C5 C4 C8 O3 -163.9(4) . C5 C4 C8 O4 14.7(7) . C5 C6 C7 C2 -0.4(7) . C6 O5 C9 C10 -141.2(4) . C6 O5 C9 C14 41.2(6) . C7 C2 C3 C4 1.0(7) . C8 C4 C5 C6 177.5(4) . C9 O5 C6 C5 -141.3(4) . C9 O5 C6 C7 43.1(6) . C9 C10 C11 C12 0.1(7) . C9 C10 C11 C15 -177.3(4) . C10 C9 C14 C13 -1.4(7) . C10 C11 C12 C13 -1.0(7) . C10 C11 C15 O6 10.7(7) . C10 C11 C15 O7 -169.6(4) . C11 C12 C13 C14 0.7(7) . C11 C12 C13 C16 -179.1(4) . C12 C11 C15 O6 -166.8(4) . C12 C11 C15 O7 12.9(7) . C12 C13 C14 C9 0.5(7) . C12 C13 C16 O8 -15.8(7) . C12 C13 C16 O9 162.4(4) . C14 C9 C10 C11 1.1(7) . C14 C13 C16 O8 164.5(5) . C14 C13 C16 O9 -17.3(6) . C15 C11 C12 C13 176.5(4) . C16 C13 C14 C9 -179.7(4) .