#------------------------------------------------------------------------------ #$Date: 2019-10-11 06:18:30 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219270 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234539.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_7234539 loop_ _publ_author_name 'Han, Mei-rong' 'Zhang, Han-tao' 'Wang, Jia-nan' 'Feng, Si-si' 'Lu, Li-ping' _publ_section_title ; Three chiral one-dimensional lanthanide--ditoluoyl-tartrate bifunctional polymers exhibiting luminescence and magnetic behaviors ; _journal_issue 55 _journal_name_full 'RSC Advances' _journal_page_first 32288 _journal_paper_doi 10.1039/C9RA06920H _journal_volume 9 _journal_year 2019 _chemical_absolute_configuration rm _chemical_formula_moiety 'C63 H63 O27 Tb' _chemical_formula_sum 'C63 H63 O27 Tb' _chemical_formula_weight 1411.05 _chemical_name_systematic 1 _space_group_crystal_system trigonal _space_group_IT_number 146 _space_group_name_Hall 'R 3' _space_group_name_H-M_alt 'R 3 :H' _symmetry_space_group_name_Hall 'R 3' _symmetry_space_group_name_H-M 'R 3 :H' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-07-13 deposited with the CCDC. 2019-10-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 27.1871(7) _cell_length_b 27.1871(7) _cell_length_c 7.6178(4) _cell_measurement_reflns_used 11383 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 2.796 _cell_measurement_theta_min 25.040 _cell_volume 4876.3(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 300(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_unetI/netI 0.0511 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 11383 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.040 _diffrn_reflns_theta_max 25.040 _diffrn_reflns_theta_min 2.810 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.442 _exptl_crystal_description needle-shaped _exptl_crystal_F_000 2166 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.793 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.081 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.08(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 3426 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 0.986 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0383 _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^)+(0.0688P)^2^+0.3333P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.0935 _reflns_Friedel_coverage 1.000 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 3415 _reflns_number_total 3426 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra06920h2.cif _cod_data_source_block 1 _cod_original_cell_volume 4876.2(4) _cod_database_code 7234539 _shelx_shelxl_version_number 2016/6 _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 0.720 _shelx_estimated_absorpt_t_max 0.892 _shelx_res_file ; TITL 1 in R3 1.res created by SHELXL-2016/6 at 09:47:23 on 21-May-2019 CELL 0.71073 27.1871 27.1871 7.6178 90 90 120 ZERR 3 0.0007 0.0007 0.0004 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H O Tb UNIT 189 189 81 3 OMIT -3 50.1 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 HTAB O9 O6_$3 EQIV $3 -x+y, -x+1, z HTAB O2 O3_$4 EQIV $4 x, y, z-1 TWIN -1 0 0 0 -1 0 0 0 -1 2 SIZE 0.3 0.1 0.1 DFIX 1.49 0.01 C17 C20 C9 C12 DELU 0.02 0.02 C8 C9 SIMU 0.01 0.02 2 C8 C9 TEMP 27.48 WGHT 0.068800 0.333333 BASF 0.07808 FVAR 0.05298 0.24355 TB1 4 0.333333 0.666667 0.084128 10.33330 0.03588 0.03588 = 0.01521 0.00000 0.00000 0.01794 O1 3 0.307243 0.594943 0.295293 11.00000 0.05720 0.04025 = 0.03017 0.01165 -0.00230 0.01066 O2 3 0.233793 0.507709 0.261883 11.00000 0.08921 0.04936 = 0.02387 -0.00670 0.00850 0.00250 AFIX 3 H2 2 0.237165 0.507641 0.153286 11.00000 -1.50000 AFIX 0 O3 3 0.255130 0.501726 0.949840 11.00000 0.09430 0.05129 = 0.02583 0.00089 0.00232 0.02727 O4 3 0.301319 0.594037 0.882456 11.00000 0.08233 0.04600 = 0.02913 -0.01189 -0.01519 0.01919 O5 3 0.193548 0.513160 0.583808 11.00000 0.04921 0.04865 = 0.03177 0.00609 0.00184 0.02334 O6 3 0.172192 0.572563 0.448121 11.00000 0.10770 0.08905 = 0.07808 0.03111 0.00621 0.06112 O7 3 0.262443 0.474049 0.617804 11.00000 0.07233 0.05503 = 0.03293 -0.00238 -0.00913 0.03004 O8 3 0.342293 0.480647 0.741355 11.00000 0.10417 0.10441 = 0.08855 0.00077 -0.02294 0.06430 O9 3 0.381011 0.774805 0.096680 11.00000 0.09744 0.06625 = 0.05852 0.00441 -0.00121 0.03327 AFIX 43 H9 2 0.394012 0.787484 0.209831 11.00000 -1.50000 AFIX 0 C1 1 0.265712 0.552036 0.349420 11.00000 0.06191 0.03655 = 0.02446 0.00392 -0.00480 0.01736 C2 1 0.252553 0.550856 0.543039 11.00000 0.05073 0.03235 = 0.02469 -0.00053 -0.00035 0.01038 AFIX 13 H2A 2 0.262779 0.589352 0.579867 11.00000 -1.20000 AFIX 0 C3 1 0.285334 0.531391 0.651890 11.00000 0.04926 0.05615 = 0.02722 -0.00436 -0.00070 0.02142 AFIX 13 H3 2 0.325384 0.551933 0.616906 11.00000 -1.20000 AFIX 0 C4 1 0.280021 0.543113 0.846536 11.00000 0.05592 0.04628 = 0.02652 -0.00619 -0.01041 0.01999 C5 1 0.155944 0.529580 0.535051 11.00000 0.07569 0.05484 = 0.03364 -0.00090 -0.01125 0.02697 AFIX 66 C6 1 0.098995 0.489451 0.594126 11.00000 0.04836 0.07051 = 0.06881 -0.00943 -0.00492 0.02913 C7 1 0.057761 0.505282 0.582643 11.00000 0.09635 0.16677 = 0.12330 0.02064 0.00851 0.09824 AFIX 43 H7 2 0.066196 0.539316 0.528782 11.00000 -1.20000 AFIX 65 C8 1 0.003920 0.470245 0.651660 11.00000 0.09276 0.23642 = 0.12129 0.00326 0.00347 0.11742 AFIX 43 H8 2 -0.023668 0.480837 0.643976 11.00000 -1.20000 AFIX 65 C9 1 -0.008687 0.419377 0.732162 11.00000 0.08643 0.22264 = 0.09929 -0.00294 0.01206 0.09759 C10 1 0.032546 0.403546 0.743647 11.00000 0.06486 0.14580 = 0.10089 0.02804 0.02020 0.04433 AFIX 43 H10 2 0.024111 0.369512 0.797508 11.00000 -1.20000 AFIX 65 C11 1 0.086387 0.438582 0.674630 11.00000 0.05584 0.08766 = 0.08860 0.01235 0.01311 0.03476 AFIX 43 H11 2 0.113975 0.427989 0.682314 11.00000 -1.20000 AFIX 0 C12 1 -0.066568 0.380495 0.808680 11.00000 0.06561 0.33129 = 0.16750 0.00736 0.03817 0.07948 AFIX 137 H12A 2 -0.077454 0.341762 0.783506 11.00000 -1.50000 H12B 2 -0.093710 0.389085 0.757806 11.00000 -1.50000 H12C 2 -0.065421 0.385862 0.933484 11.00000 -1.50000 AFIX 0 C13 1 0.297998 0.451994 0.673233 11.00000 0.08252 0.06856 = 0.03688 -0.00572 -0.00128 0.02893 C14 1 0.271168 0.392645 0.637123 11.00000 0.10226 0.07079 = 0.04977 -0.00159 -0.00396 0.04325 C15 1 0.223412 0.363216 0.540719 11.00000 0.06969 0.06185 = 0.10731 -0.00099 0.01079 0.03310 AFIX 43 H15 2 0.203837 0.380998 0.501188 11.00000 -1.20000 AFIX 0 C16 1 0.203810 0.307482 0.501173 11.00000 0.13892 0.06893 = 0.11795 -0.02324 -0.01757 0.04258 AFIX 43 H16 2 0.173189 0.289108 0.424833 11.00000 -1.20000 AFIX 0 C17 1 0.227690 0.277560 0.570093 11.00000 0.12686 0.05579 = 0.08714 0.00680 -0.00767 0.04126 C18 1 0.275734 0.307830 0.665864 11.00000 0.16327 0.07992 = 0.12306 0.00730 -0.04143 0.06123 AFIX 43 H18 2 0.295274 0.290047 0.705712 11.00000 -1.20000 AFIX 0 C19 1 0.295540 0.362090 0.704094 11.00000 0.18442 0.08941 = 0.08387 0.00011 -0.03706 0.08253 AFIX 43 H19 2 0.326782 0.380389 0.778180 11.00000 -1.20000 AFIX 0 C20 1 0.204711 0.215467 0.530360 11.00000 0.23208 0.09052 = 0.11700 -0.01120 -0.01912 0.09334 AFIX 137 H20A 2 0.229902 0.211472 0.450902 11.00000 -1.50000 H20B 2 0.167836 0.199932 0.477591 11.00000 -1.50000 H20C 2 0.201777 0.195496 0.637308 11.00000 -1.50000 AFIX 0 C21 1 0.394167 0.822447 -0.016079 11.00000 0.13318 0.09612 = 0.08950 0.01828 -0.02431 0.04152 AFIX 137 H21A 2 0.396214 0.812418 -0.135599 11.00000 -1.50000 H21B 2 0.430027 0.854256 0.017733 11.00000 -1.50000 H21C 2 0.365016 0.832379 -0.005425 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in R3 REM R1 = 0.0383 for 3415 Fo > 4sig(Fo) and 0.0384 for all 3426 data REM 267 parameters refined using 10 restraints END WGHT 0.0531 0.0000 REM Highest difference peak 0.793, deepest hole -0.570, 1-sigma level 0.081 Q1 1 0.3575 0.7127 0.0742 11.00000 0.05 0.79 Q2 1 0.3110 0.6902 0.0872 11.00000 0.05 0.79 Q3 1 0.1838 0.3597 0.5082 11.00000 0.05 0.43 Q4 1 0.1476 0.3021 0.4463 11.00000 0.05 0.42 Q5 1 0.1674 0.2620 0.4965 11.00000 0.05 0.41 ; _shelx_res_checksum 44131 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 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 Tb1 Tb 0.333333 0.666667 0.08413(5) 0.02899(17) Uani 1 3 d S T P O1 O 0.3072(3) 0.5949(2) 0.2953(8) 0.0486(14) Uani 1 1 d . . . O2 O 0.2338(4) 0.5077(3) 0.2619(9) 0.068(2) Uani 1 1 d . . . H2 H 0.237165 0.507641 0.153286 0.103 Uiso 1 1 d R U . O3 O 0.2551(3) 0.5017(3) 0.9498(8) 0.0612(18) Uani 1 1 d . . . O4 O 0.3013(3) 0.5940(3) 0.8825(8) 0.0582(17) Uani 1 1 d . . . O5 O 0.1935(2) 0.5132(2) 0.5838(8) 0.0437(13) Uani 1 1 d . . . O6 O 0.1722(5) 0.5726(4) 0.4481(14) 0.086(3) Uani 1 1 d . . . O7 O 0.2624(4) 0.4740(3) 0.6178(11) 0.054(2) Uani 1 1 d . . . O8 O 0.3423(5) 0.4806(4) 0.7414(14) 0.094(3) Uani 1 1 d . . . O9 O 0.3810(4) 0.7748(3) 0.0967(11) 0.077(2) Uani 1 1 d . . . H9 H 0.394012 0.787484 0.209831 0.116 Uiso 1 1 calc R U . C1 C 0.2657(4) 0.5520(3) 0.3494(10) 0.044(2) Uani 1 1 d . . . C2 C 0.2526(3) 0.5509(3) 0.5430(10) 0.0405(18) Uani 1 1 d . . . H2A H 0.262779 0.589352 0.579867 0.049 Uiso 1 1 calc R U . C3 C 0.2853(4) 0.5314(5) 0.6519(13) 0.046(2) Uani 1 1 d . . . H3 H 0.325384 0.551933 0.616906 0.056 Uiso 1 1 calc R U . C4 C 0.2800(4) 0.5431(4) 0.8465(11) 0.0454(19) Uani 1 1 d . . . C5 C 0.1559(6) 0.5296(5) 0.5351(16) 0.057(3) Uani 1 1 d . . . C6 C 0.0990(3) 0.4895(3) 0.5941(13) 0.063(3) Uani 1 1 d G . . C7 C 0.0578(4) 0.5053(4) 0.5826(16) 0.114(6) Uani 1 1 d G . . H7 H 0.066196 0.539316 0.528782 0.137 Uiso 1 1 calc R U . C8 C 0.0039(4) 0.4702(6) 0.6517(18) 0.135(7) Uani 1 1 d G U . H8 H -0.023668 0.480837 0.643976 0.161 Uiso 1 1 calc R U . C9 C -0.0087(3) 0.4194(5) 0.7322(16) 0.127(6) Uani 1 1 d DG U . C10 C 0.0325(3) 0.4035(4) 0.7436(14) 0.108(5) Uani 1 1 d G . . H10 H 0.024111 0.369512 0.797508 0.129 Uiso 1 1 calc R U . C11 C 0.0864(3) 0.4386(3) 0.6746(13) 0.078(3) Uani 1 1 d G . . H11 H 0.113975 0.427989 0.682314 0.093 Uiso 1 1 calc R U . C12 C -0.0666(6) 0.3805(12) 0.809(4) 0.197(13) Uani 1 1 d D . . H12A H -0.077454 0.341762 0.783506 0.295 Uiso 1 1 calc R U . H12B H -0.093710 0.389085 0.757806 0.295 Uiso 1 1 calc R U . H12C H -0.065421 0.385862 0.933484 0.295 Uiso 1 1 calc R U . C13 C 0.2980(6) 0.4520(5) 0.6732(15) 0.067(3) Uani 1 1 d . . . C14 C 0.2712(6) 0.3926(5) 0.6371(16) 0.074(3) Uani 1 1 d . . . C15 C 0.2234(6) 0.3632(5) 0.541(2) 0.080(4) Uani 1 1 d . . . H15 H 0.203837 0.380998 0.501188 0.095 Uiso 1 1 calc R U . C16 C 0.2038(9) 0.3075(7) 0.501(3) 0.113(6) Uani 1 1 d . . . H16 H 0.173189 0.289108 0.424833 0.135 Uiso 1 1 calc R U . C17 C 0.2277(7) 0.2776(5) 0.570(2) 0.092(4) Uani 1 1 d D . . C18 C 0.2757(9) 0.3078(7) 0.666(3) 0.122(6) Uani 1 1 d . . . H18 H 0.295274 0.290047 0.705712 0.146 Uiso 1 1 calc R U . C19 C 0.2955(9) 0.3621(7) 0.704(2) 0.113(6) Uani 1 1 d . . . H19 H 0.326782 0.380389 0.778180 0.136 Uiso 1 1 calc R U . C20 C 0.2047(11) 0.2155(6) 0.530(3) 0.141(8) Uani 1 1 d D . . H20A H 0.229902 0.211472 0.450902 0.211 Uiso 1 1 calc R U . H20B H 0.167836 0.199932 0.477591 0.211 Uiso 1 1 calc R U . H20C H 0.201777 0.195496 0.637308 0.211 Uiso 1 1 calc R U . C21 C 0.3942(8) 0.8224(7) -0.016(2) 0.113(6) Uani 1 1 d . . . H21A H 0.396214 0.812418 -0.135599 0.170 Uiso 1 1 calc R U . H21B H 0.430027 0.854256 0.017733 0.170 Uiso 1 1 calc R U . H21C H 0.365016 0.832379 -0.005425 0.170 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 0.0359(2) 0.0359(2) 0.0152(2) 0.000 0.000 0.01794(10) O1 0.057(3) 0.040(3) 0.030(3) 0.012(2) -0.002(3) 0.011(3) O2 0.089(5) 0.049(4) 0.024(3) -0.007(3) 0.009(3) 0.002(3) O3 0.094(5) 0.051(4) 0.026(3) 0.001(3) 0.002(3) 0.027(3) O4 0.082(5) 0.046(3) 0.029(3) -0.012(3) -0.015(3) 0.019(3) O5 0.049(3) 0.049(3) 0.032(3) 0.006(2) 0.002(2) 0.023(3) O6 0.108(8) 0.089(6) 0.078(7) 0.031(6) 0.006(6) 0.061(6) O7 0.072(5) 0.055(4) 0.033(4) -0.002(3) -0.009(4) 0.030(4) O8 0.104(7) 0.104(7) 0.089(7) 0.001(5) -0.023(6) 0.064(6) O9 0.097(6) 0.066(5) 0.059(5) 0.004(4) -0.001(4) 0.033(4) C1 0.062(5) 0.037(4) 0.024(4) 0.004(3) -0.005(4) 0.017(4) C2 0.051(5) 0.032(4) 0.025(4) -0.001(3) 0.000(3) 0.010(3) C3 0.049(5) 0.056(6) 0.027(5) -0.004(4) -0.001(4) 0.021(5) C4 0.056(5) 0.046(5) 0.027(4) -0.006(4) -0.010(4) 0.020(4) C5 0.076(8) 0.055(7) 0.034(6) -0.001(5) -0.011(5) 0.027(6) C6 0.048(6) 0.071(7) 0.069(8) -0.009(6) -0.005(5) 0.029(5) C7 0.096(11) 0.167(18) 0.123(15) 0.021(13) 0.009(10) 0.098(13) C8 0.093(10) 0.24(2) 0.121(13) 0.003(13) 0.003(10) 0.117(13) C9 0.086(9) 0.22(2) 0.099(12) -0.003(12) 0.012(8) 0.098(12) C10 0.065(8) 0.146(14) 0.101(13) 0.028(10) 0.020(7) 0.044(9) C11 0.056(6) 0.088(8) 0.089(9) 0.012(7) 0.013(6) 0.035(6) C12 0.066(10) 0.33(4) 0.17(2) 0.01(2) 0.038(12) 0.079(16) C13 0.083(8) 0.069(7) 0.037(6) -0.006(5) -0.001(6) 0.029(6) C14 0.102(9) 0.071(7) 0.050(7) -0.002(5) -0.004(6) 0.043(7) C15 0.070(9) 0.062(8) 0.107(12) -0.001(8) 0.011(8) 0.033(8) C16 0.139(15) 0.069(10) 0.118(15) -0.023(9) -0.018(12) 0.043(11) C17 0.127(12) 0.056(7) 0.087(10) 0.007(7) -0.008(9) 0.041(8) C18 0.163(16) 0.080(10) 0.123(15) 0.007(9) -0.041(13) 0.061(11) C19 0.184(17) 0.089(10) 0.084(11) 0.000(8) -0.037(11) 0.083(11) C20 0.23(2) 0.091(11) 0.117(15) -0.011(10) -0.019(15) 0.093(14) C21 0.133(14) 0.096(11) 0.089(12) 0.018(9) -0.024(11) 0.042(10) 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 O4 Tb1 O4 80.3(2) 1_554 2_664 O4 Tb1 O4 80.3(2) 1_554 3_564 O4 Tb1 O4 80.3(2) 2_664 3_564 O4 Tb1 O1 133.3(2) 1_554 3_565 O4 Tb1 O1 140.2(2) 2_664 3_565 O4 Tb1 O1 85.2(2) 3_564 3_565 O4 Tb1 O1 140.2(2) 1_554 2_665 O4 Tb1 O1 85.3(2) 2_664 2_665 O4 Tb1 O1 133.3(2) 3_564 2_665 O1 Tb1 O1 78.2(2) 3_565 2_665 O4 Tb1 O1 85.3(2) 1_554 . O4 Tb1 O1 133.3(2) 2_664 . O4 Tb1 O1 140.2(2) 3_564 . O1 Tb1 O1 78.2(2) 3_565 . O1 Tb1 O1 78.2(2) 2_665 . O4 Tb1 O9 69.7(3) 1_554 2_665 O4 Tb1 O9 140.3(3) 2_664 2_665 O4 Tb1 O9 69.7(3) 3_564 2_665 O1 Tb1 O9 63.7(2) 3_565 2_665 O1 Tb1 O9 134.4(2) 2_665 2_665 O1 Tb1 O9 70.6(3) . 2_665 O4 Tb1 O9 140.3(3) 1_554 . O4 Tb1 O9 69.7(3) 2_664 . O4 Tb1 O9 69.7(3) 3_564 . O1 Tb1 O9 70.6(2) 3_565 . O1 Tb1 O9 63.7(2) 2_665 . O1 Tb1 O9 134.4(2) . . O9 Tb1 O9 119.86(3) 2_665 . O4 Tb1 O9 69.7(3) 1_554 3_565 O4 Tb1 O9 69.7(3) 2_664 3_565 O4 Tb1 O9 140.3(3) 3_564 3_565 O1 Tb1 O9 134.4(2) 3_565 3_565 O1 Tb1 O9 70.6(3) 2_665 3_565 O1 Tb1 O9 63.7(2) . 3_565 O9 Tb1 O9 119.86(3) 2_665 3_565 O9 Tb1 O9 119.86(3) . 3_565 C1 O1 Tb1 141.0(6) . . C1 O2 H2 120.1 . . C4 O4 Tb1 150.9(6) . 1_556 C5 O5 C2 117.5(8) . . C3 O7 C13 113.5(9) . . C21 O9 Tb1 140.1(9) . . C21 O9 H9 110.0 . . Tb1 O9 H9 110.0 . . O1 C1 O2 126.7(8) . . O1 C1 C2 116.4(7) . . O2 C1 C2 116.8(7) . . O5 C2 C3 106.1(7) . . O5 C2 C1 113.1(6) . . C3 C2 C1 111.8(7) . . O5 C2 H2A 108.6 . . C3 C2 H2A 108.6 . . C1 C2 H2A 108.6 . . O7 C3 C2 106.4(8) . . O7 C3 C4 112.2(9) . . C2 C3 C4 109.1(8) . . O7 C3 H3 109.7 . . C2 C3 H3 109.7 . . C4 C3 H3 109.7 . . O4 C4 O3 127.2(8) . . O4 C4 C3 113.9(8) . . O3 C4 C3 118.8(8) . . O6 C5 O5 119.6(13) . . O6 C5 C6 129.0(13) . . O5 C5 C6 111.4(9) . . C7 C6 C11 120.0 . . C7 C6 C5 118.1(7) . . C11 C6 C5 121.7(7) . . C8 C7 C6 120.0 . . C8 C7 H7 120.0 . . C6 C7 H7 120.0 . . C9 C8 C7 120.0 . . C9 C8 H8 120.0 . . C7 C8 H8 120.0 . . C8 C9 C10 120.0 . . C8 C9 C12 121.3(13) . . C10 C9 C12 118.7(13) . . C11 C10 C9 120.0 . . C11 C10 H10 120.0 . . C9 C10 H10 120.0 . . C10 C11 C6 120.0 . . C10 C11 H11 120.0 . . C6 C11 H11 120.0 . . C9 C12 H12A 109.5 . . C9 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . C9 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . O8 C13 C14 127.5(13) . . O8 C13 O7 122.3(11) . . C14 C13 O7 110.3(11) . . C15 C14 C19 116.7(12) . . C15 C14 C13 124.8(13) . . C19 C14 C13 118.5(13) . . C14 C15 C16 120.2(15) . . C14 C15 H15 119.9 . . C16 C15 H15 119.9 . . C15 C16 C17 122.4(17) . . C15 C16 H16 118.8 . . C17 C16 H16 118.8 . . C18 C17 C16 116.3(12) . . C18 C17 C20 121.4(15) . . C16 C17 C20 122.1(16) . . C19 C18 C17 121.7(16) . . C19 C18 H18 119.2 . . C17 C18 H18 119.2 . . C18 C19 C14 122.3(16) . . C18 C19 H19 118.9 . . C14 C19 H19 118.9 . . C17 C20 H20A 109.5 . . C17 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . C17 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . O9 C21 H21A 109.5 . . O9 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . O9 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Tb1 O4 2.302(6) 1_554 Tb1 O4 2.302(6) 2_664 Tb1 O4 2.302(6) 3_564 Tb1 O1 2.347(5) 3_565 Tb1 O1 2.347(5) 2_665 Tb1 O1 2.347(5) . Tb1 O9 2.554(8) 2_665 Tb1 O9 2.554(8) . Tb1 O9 2.554(8) 3_565 O1 C1 1.220(10) . O2 C1 1.267(11) . O2 H2 0.8324 . O3 C4 1.258(11) . O4 C4 1.235(10) . O5 C5 1.356(15) . O5 C2 1.441(10) . O6 C5 1.218(15) . O7 C3 1.384(13) . O7 C13 1.432(16) . O8 C13 1.178(15) . O9 C21 1.442(17) . O9 H9 0.9300 . C1 C2 1.514(11) . C2 C3 1.495(13) . C2 H2A 0.9800 . C3 C4 1.539(12) . C3 H3 0.9800 . C5 C6 1.449(15) . C6 C7 1.3900 . C6 C11 1.3900 . C7 C8 1.3900 . C7 H7 0.9300 . C8 C9 1.3900 . C8 H8 0.9300 . C9 C10 1.3900 . C9 C12 1.507(12) . C10 C11 1.3900 . C10 H10 0.9300 . C11 H11 0.9300 . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C13 C14 1.426(17) . C14 C15 1.35(2) . C14 C19 1.39(2) . C15 C16 1.365(19) . C15 H15 0.9300 . C16 C17 1.37(2) . C16 H16 0.9300 . C17 C18 1.36(2) . C17 C20 1.509(12) . C18 C19 1.33(2) . C18 H18 0.9300 . C19 H19 0.9300 . C20 H20A 0.9600 . C20 H20B 0.9600 . C20 H20C 0.9600 . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 . 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 O9 H9 O6 0.93 2.08 2.960(14) 156.8 3_565 O2 H2 O3 0.83 1.66 2.471(9) 165.5 1_554