#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:41:58 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252627 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240600.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_7240600 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 '0.5(C30 H36 O30 Tb4)' _chemical_formula_sum 'C15 H18 O15 Tb2' _chemical_formula_weight 756.13 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 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 106.131(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.7575(9) _cell_length_b 7.9696(7) _cell_length_c 12.8428(15) _cell_measurement_reflns_used 1947 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.4310 _cell_measurement_theta_min 4.1780 _cell_volume 959.38(17) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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 293.15 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0355 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 88.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 -150.0000 53 #__ type_ start__ end____ width___ exp.time_ 2 omega 32.00 88.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 -178.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 3 omega -25.00 55.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 -99.0000 -30.0000 80 #__ type_ start__ end____ width___ exp.time_ 4 omega -1.00 83.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 57.0000 60.0000 84 #__ type_ start__ end____ width___ exp.time_ 5 omega 35.00 88.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 -90.0000 53 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0699517000 _diffrn_orient_matrix_UB_12 -0.0284866000 _diffrn_orient_matrix_UB_13 -0.0260865000 _diffrn_orient_matrix_UB_21 -0.0284136000 _diffrn_orient_matrix_UB_22 0.0759157000 _diffrn_orient_matrix_UB_23 0.0139123000 _diffrn_orient_matrix_UB_31 0.0044624000 _diffrn_orient_matrix_UB_32 0.0365710000 _diffrn_orient_matrix_UB_33 -0.0493804000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.710 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_unetI/netI 0.0729 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 6009 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.214 _diffrn_reflns_theta_max 26.342 _diffrn_reflns_theta_min 3.299 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 7.395 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.18691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) 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 2.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.036 _refine_diff_density_max 3.150 _refine_diff_density_min -2.629 _refine_diff_density_rms 0.339 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 2081 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0613 _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^)+(0.0560P)^2^+25.4418P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1448 _refine_ls_wR_factor_ref 0.1534 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1783 _reflns_number_total 2081 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 150615_BQB_Tb in P21/m CELL 0.71 9.757451 7.969565 12.842813 90 106.1311 90 ZERR 2 0.000865 0.000654 0.001462 0 0.0106 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H O Tb UNIT 30 36 30 4 EADP O2 O1 C1 C2 C3 EADP O6 C7 C8 C9 EADP O8 O7 O9 L.S. 100 PLAN 10 SIZE 0.036 0.38 0.42 TEMP 20 htab BOND $H CONF MORE -1 fmap 2 acta SHEL 999 0.8 OMIT -2 6 2 OMIT -2 4 2 OMIT -6 4 6 OMIT 3 6 2 OMIT -1 5 3 OMIT 0 5 4 OMIT 0 7 4 OMIT -7 4 5 OMIT -3 4 1 OMIT 4 5 0 OMIT -7 6 2 OMIT -5 5 7 OMIT -2 8 2 OMIT 3 3 6 OMIT -1 8 3 REM REM REM WGHT 0.056000 25.441799 FVAR 3.80767 TB1 4 0.490551 0.750000 0.133106 10.50000 0.01790 0.01328 = 0.01343 0.00000 0.00624 0.00000 TB2 4 0.896856 0.250000 0.505955 10.50000 0.01674 0.02738 = 0.01283 0.00000 0.00646 0.00000 O3 3 0.657259 0.571089 0.087816 11.00000 0.02782 0.01437 = 0.03285 -0.00785 0.02080 -0.00108 O2 3 0.719205 0.422946 0.412681 11.00000 0.03289 0.02937 = 0.04029 0.00856 0.00525 0.00277 O6 3 0.840893 0.078258 0.645579 11.00000 0.05320 0.01675 = 0.02329 0.00131 0.01459 0.00276 O1 3 0.583938 0.565455 0.275494 11.00000 0.03289 0.02937 = 0.04029 0.00856 0.00525 0.00277 O8 3 0.322423 0.750000 0.240202 10.50000 0.03309 0.01685 = 0.02718 0.00000 0.00925 0.00000 AFIX 3 0.8600 H8A 2 0.316613 0.676910 0.288062 10.50000 -1.50000 H8B 2 0.254093 0.820420 0.235112 10.50000 -1.50000 AFIX 0 O7 3 0.451602 0.750000 -0.065091 10.50000 0.03309 0.01685 = 0.02718 0.00000 0.00925 0.00000 AFIX 3 0.8600 H7A 2 0.391162 0.822550 -0.100461 10.50000 -1.50000 H7B 2 0.420142 0.657190 -0.097051 10.50000 -1.50000 AFIX 0 O9 3 1.135158 0.250000 0.618912 10.50000 0.03309 0.01685 = 0.02718 0.00000 0.00925 0.00000 AFIX 3 0.8600 H9A 2 1.200748 0.177920 0.618932 10.50000 -1.50000 H9B 2 1.187488 0.311830 0.669372 10.50000 -1.50000 AFIX 0 O4 3 0.681400 0.457218 -0.064784 11.00000 0.03382 0.02921 = 0.02548 -0.01195 0.01236 -0.00794 O5 3 0.993071 -0.075162 0.594377 11.00000 0.05188 0.03559 = 0.03807 0.00085 0.03738 -0.00472 C1 1 0.599610 0.449987 0.343296 11.00000 0.03289 0.02937 = 0.04029 0.00856 0.00525 0.00277 C4 1 0.720310 0.558179 0.014893 11.00000 0.01910 0.00672 = 0.02884 0.00461 0.00291 0.00165 C9 1 1.059713 -0.250000 0.808609 10.50000 0.05320 0.01675 = 0.02329 0.00131 0.01459 0.00276 AFIX 23 H9C 2 1.093418 -0.249996 0.887134 10.50000 -1.20000 H9D 2 1.134517 -0.250004 0.772208 10.50000 -1.20000 AFIX 0 C8 1 0.926695 -0.153973 0.756967 11.00000 0.05320 0.01675 = 0.02329 0.00131 0.01459 0.00276 AFIX 13 H8 2 0.881361 -0.103747 0.808689 11.00000 -1.20000 AFIX 0 C2 1 0.474496 0.345749 0.345320 11.00000 0.03289 0.02937 = 0.04029 0.00856 0.00525 0.00277 AFIX 13 H2 2 0.383365 0.394478 0.304069 11.00000 -1.20000 AFIX 0 C3 1 0.464613 0.250000 0.441721 10.50000 0.03289 0.02937 = 0.04029 0.00856 0.00525 0.00277 AFIX 23 H3A 2 0.547407 0.250002 0.504510 10.50000 -1.20000 H3B 2 0.373657 0.249998 0.458545 10.50000 -1.20000 AFIX 0 C7 1 0.921415 -0.047546 0.661663 11.00000 0.05320 0.01675 = 0.02329 0.00131 0.01459 0.00276 C6 1 0.925601 0.750000 0.121123 10.50000 0.02473 0.02895 = 0.01820 0.00000 0.00030 0.00000 AFIX 23 H6A 2 1.029081 0.750002 0.143715 10.50000 -1.20000 H6B 2 0.881677 0.749999 0.180239 10.50000 -1.20000 AFIX 0 C5 1 0.853291 0.652313 0.021918 11.00000 0.02230 0.01304 = 0.02000 -0.00261 0.00920 0.00439 AFIX 13 H5 2 0.917437 0.600210 -0.015391 11.00000 -1.20000 AFIX 0 HKLF 4 REM 150615_BQB_Tb in P21/m REM R1 = 0.0613 for 1783 Fo > 4sig(Fo) and 0.0709 for all 2081 data REM 111 parameters refined using 0 restraints END WGHT 0.0560 25.4276 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y+1/2, -z+1 HTAB O8 O6_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB O8 O6_$2 EQIV $3 -x+1, y+1/2, -z HTAB O7 O3_$3 EQIV $4 -x+1, -y+1, -z HTAB O7 O3_$4 EQIV $5 -x+2, y-1/2, -z+1 HTAB O9 O2_$5 HTAB O9 O1_$5 EQIV $6 -x+2, -y+1, -z+1 HTAB O9 O2_$6 HTAB O9 O1_$6 REM Highest difference peak 3.150, deepest hole -2.629, 1-sigma level 0.339 Q1 1 0.9499 0.2500 0.4610 10.50000 0.05 3.15 Q2 1 0.4386 0.7500 0.1774 10.50000 0.05 2.92 Q3 1 0.5380 0.7500 0.0894 10.50000 0.05 2.79 Q4 1 0.8511 0.2500 0.5591 10.50000 0.05 2.54 Q5 1 0.9157 0.7500 0.2424 10.50000 0.05 2.34 Q6 1 0.7159 -0.1704 0.8610 11.00000 0.05 1.94 Q7 1 0.9584 0.1409 0.5624 11.00000 0.05 1.67 Q8 1 0.5618 0.6381 0.1954 11.00000 0.05 1.64 Q9 1 0.8400 0.1493 0.4592 11.00000 0.05 1.60 Q10 1 0.4221 0.8622 0.0771 11.00000 0.05 1.52 REM The information below was added by Olex2. REM REM R1 = 0.0613 for 1783 Fo > 4sig(Fo) and 0.0709 for all 6518 data REM n/a parameters refined using n/a restraints REM Highest difference peak 3.15, deepest hole -2.63 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0709 REM R1_gt = 0.0613 REM wR_ref = 0.1534 REM GOOF = 1.087 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 6518 REM Reflections_gt = 1783 REM Parameters = n/a REM Hole = -2.63 REM Peak = 3.15 REM Flack = n/a ; _cod_data_source_file d0ce00583e2.cif _cod_data_source_block cpdc-Tb _cod_original_cell_volume 959.37(17) _cod_database_code 7240600 _shelxl_version_number 2013-2 _chemical_oxdiff_formula 'C H N O 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. ; _shelx_estimated_absorpt_t_max 0.777 _shelx_estimated_absorpt_t_min 0.147 _reflns_odcompleteness_completeness 99.62 _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(O2) = Uanis(O1) = Uanis(C1) = Uanis(C2) = Uanis(C3) Uanis(O6) = Uanis(C7) = Uanis(C8) = Uanis(C9) Uanis(O8) = Uanis(O7) = Uanis(O9) 3. Others Fixed Sof: H8A(0.5) H8B(0.5) H7A(0.5) H7B(0.5) H9A(0.5) H9B(0.5) 4.a Riding coordinates: O8(H8A,H8B), O7(H7A,H7B), O9(H9A,H9B) 4.b Ternary CH refined with riding coordinates: C8(H8), C2(H2), C5(H5) 4.c Secondary CH2 refined with riding coordinates: C9(H9C,H9D), C3(H3A,H3B), C6(H6A,H6B) ; _olex2_date_sample_data_collection 2015-06-14 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.49055(7) 0.7500 0.13311(6) 0.0145(2) Uani 1 2 d S T P . . Tb2 Tb 0.89686(8) 0.2500 0.50595(6) 0.0185(2) Uani 1 2 d S T P . . O3 O 0.6573(8) 0.5711(11) 0.0878(7) 0.0225(18) Uani 1 1 d . . . . . O2 O 0.7192(9) 0.4229(13) 0.4127(8) 0.0352(13) Uani 1 1 d . . . . . O6 O 0.8409(10) 0.0783(12) 0.6456(7) 0.0303(14) Uani 1 1 d . . . . . O1 O 0.5839(9) 0.5655(13) 0.2755(8) 0.0352(13) Uani 1 1 d . . . . . O8 O 0.3224(13) 0.7500 0.2402(10) 0.0255(15) Uani 1 2 d S T P . . H8A H 0.3166 0.6769 0.2881 0.038 Uiso 0.5 1 d R . . . . H8B H 0.2541 0.8204 0.2351 0.038 Uiso 0.5 1 d R . . . . O7 O 0.4516(13) 0.7500 -0.0651(10) 0.0255(15) Uani 1 2 d S T P . . H7A H 0.3912 0.8225 -0.1005 0.038 Uiso 0.5 1 d R . . . . H7B H 0.4201 0.6572 -0.0971 0.038 Uiso 0.5 1 d R . . . . O9 O 1.1352(13) 0.2500 0.6189(10) 0.0255(15) Uani 1 2 d S T P . . H9A H 1.2007 0.1779 0.6189 0.038 Uiso 0.5 1 d R . . . . H9B H 1.1875 0.3118 0.6694 0.038 Uiso 0.5 1 d R . . . . O4 O 0.6814(9) 0.4572(12) -0.0648(7) 0.029(2) Uani 1 1 d . . . . . O5 O 0.9931(10) -0.0752(13) 0.5944(8) 0.037(2) Uani 1 1 d . . . . . C1 C 0.5996(14) 0.4500(19) 0.3433(12) 0.0352(13) Uani 1 1 d . . . . . C4 C 0.7203(11) 0.5582(14) 0.0149(9) 0.019(2) Uani 1 1 d . . . . . C9 C 1.060(2) -0.2500 0.8086(15) 0.0303(14) Uani 1 2 d S T P . . H9C H 1.0934 -0.2500 0.8871 0.036 Uiso 1 2 calc RS T P . . H9D H 1.1345 -0.2500 0.7722 0.036 Uiso 1 2 calc RS T P . . C8 C 0.9267(15) -0.1540(16) 0.7570(10) 0.0303(14) Uani 1 1 d . . . . . H8 H 0.8814 -0.1037 0.8087 0.036 Uiso 1 1 calc R . . . . C2 C 0.4745(14) 0.3457(18) 0.3453(12) 0.0352(13) Uani 1 1 d . . . . . H2 H 0.3834 0.3945 0.3041 0.042 Uiso 1 1 calc R . . . . C3 C 0.465(2) 0.2500 0.4417(17) 0.0352(13) Uani 1 2 d S T P . . H3A H 0.5474 0.2500 0.5045 0.042 Uiso 1 2 calc RS T P . . H3B H 0.3737 0.2500 0.4585 0.042 Uiso 1 2 calc RS T P . . C7 C 0.9214(15) -0.0475(17) 0.6617(10) 0.0303(14) Uani 1 1 d . . . . . C6 C 0.9256(18) 0.7500 0.1211(14) 0.025(4) Uani 1 2 d S T P . . H6A H 1.0291 0.7500 0.1437 0.030 Uiso 1 2 calc RS T P . . H6B H 0.8817 0.7500 0.1802 0.030 Uiso 1 2 calc RS T P . . C5 C 0.8533(11) 0.6523(14) 0.0219(9) 0.018(2) Uani 1 1 d . . . . . H5 H 0.9174 0.6002 -0.0154 0.021 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 0.0179(4) 0.0133(4) 0.0134(4) 0.000 0.0062(3) 0.000 Tb2 0.0167(4) 0.0274(5) 0.0128(4) 0.000 0.0065(3) 0.000 O3 0.028(4) 0.014(4) 0.033(5) -0.008(4) 0.021(4) -0.001(3) O2 0.033(3) 0.029(3) 0.040(3) 0.009(3) 0.005(2) 0.003(2) O6 0.053(4) 0.017(3) 0.023(3) 0.001(3) 0.015(3) 0.003(3) O1 0.033(3) 0.029(3) 0.040(3) 0.009(3) 0.005(2) 0.003(2) O8 0.033(4) 0.017(4) 0.027(4) 0.000 0.009(3) 0.000 O7 0.033(4) 0.017(4) 0.027(4) 0.000 0.009(3) 0.000 O9 0.033(4) 0.017(4) 0.027(4) 0.000 0.009(3) 0.000 O4 0.034(5) 0.029(5) 0.025(5) -0.012(4) 0.012(4) -0.008(4) O5 0.052(6) 0.036(6) 0.038(5) 0.001(5) 0.037(5) -0.005(5) C1 0.033(3) 0.029(3) 0.040(3) 0.009(3) 0.005(2) 0.003(2) C4 0.019(5) 0.007(5) 0.029(6) 0.005(5) 0.003(5) 0.002(4) C9 0.053(4) 0.017(3) 0.023(3) 0.001(3) 0.015(3) 0.003(3) C8 0.053(4) 0.017(3) 0.023(3) 0.001(3) 0.015(3) 0.003(3) C2 0.033(3) 0.029(3) 0.040(3) 0.009(3) 0.005(2) 0.003(2) C3 0.033(3) 0.029(3) 0.040(3) 0.009(3) 0.005(2) 0.003(2) C7 0.053(4) 0.017(3) 0.023(3) 0.001(3) 0.015(3) 0.003(3) C6 0.025(8) 0.029(10) 0.018(8) 0.000 0.000(7) 0.000 C5 0.022(5) 0.013(6) 0.020(5) -0.003(5) 0.009(4) 0.004(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 74.5(4) 4_575 . ? O3 Tb1 O8 140.0(2) 4_575 . ? O3 Tb1 O8 140.0(2) . . ? O3 Tb1 O7 70.4(3) . . ? O3 Tb1 O7 70.4(3) 4_575 . ? O1 Tb1 O3 115.5(3) 4_575 . ? O1 Tb1 O3 70.4(3) 4_575 4_575 ? O1 Tb1 O3 115.5(3) . 4_575 ? O1 Tb1 O3 70.4(3) . . ? O1 Tb1 O1 78.4(5) 4_575 . ? O1 Tb1 O8 74.5(3) . . ? O1 Tb1 O8 74.5(3) 4_575 . ? O1 Tb1 O7 136.5(3) 4_575 . ? O1 Tb1 O7 136.5(3) . . ? O1 Tb1 O4 145.4(3) . 2_655 ? O1 Tb1 O4 86.1(3) 4_575 2_655 ? O1 Tb1 O4 145.4(3) 4_575 3_665 ? O1 Tb1 O4 86.1(3) . 3_665 ? O8 Tb1 O7 130.8(4) . . ? O4 Tb1 O3 87.3(3) 3_665 . ? O4 Tb1 O3 143.7(3) 2_655 . ? O4 Tb1 O3 143.7(3) 3_665 4_575 ? O4 Tb1 O3 87.3(3) 2_655 4_575 ? O4 Tb1 O8 71.6(3) 3_665 . ? O4 Tb1 O8 71.6(3) 2_655 . ? O4 Tb1 O7 74.0(3) 2_655 . ? O4 Tb1 O7 74.0(3) 3_665 . ? O4 Tb1 O4 89.6(5) 3_665 2_655 ? O2 Tb2 O2 74.5(5) 4_565 . ? O2 Tb2 O6 115.7(3) 4_565 4_565 ? O2 Tb2 O6 115.7(3) . . ? O2 Tb2 O6 75.7(3) 4_565 . ? O2 Tb2 O6 75.7(3) . 4_565 ? O2 Tb2 O9 142.6(3) 4_565 . ? O2 Tb2 O9 142.6(3) . . ? O2 Tb2 O5 117.9(4) 4_565 2_756 ? O2 Tb2 O5 117.9(4) . 3_756 ? O2 Tb2 O5 75.5(3) 4_565 3_756 ? O2 Tb2 O5 77.3(3) 4_565 . ? O2 Tb2 O5 150.4(3) . . ? O2 Tb2 O5 150.4(3) 4_565 4_565 ? O2 Tb2 O5 75.5(3) . 2_756 ? O2 Tb2 O5 77.3(3) . 4_565 ? O6 Tb2 O6 68.4(4) . 4_565 ? O6 Tb2 O5 47.1(3) 4_565 4_565 ? O6 Tb2 O5 109.3(3) . 4_565 ? O6 Tb2 O5 47.1(3) . . ? O6 Tb2 O5 109.3(3) 4_565 . ? O9 Tb2 O6 86.1(3) . 4_565 ? O9 Tb2 O6 86.1(3) . . ? O9 Tb2 O5 66.6(2) . 4_565 ? O9 Tb2 O5 66.6(2) . . ? O5 Tb2 O6 165.2(3) 2_756 . ? O5 Tb2 O6 107.5(3) 3_756 . ? O5 Tb2 O6 107.5(3) 2_756 4_565 ? O5 Tb2 O6 165.2(3) 3_756 4_565 ? O5 Tb2 O9 79.4(3) 2_756 . ? O5 Tb2 O9 79.4(3) 3_756 . ? O5 Tb2 O5 62.2(3) 2_756 4_565 ? O5 Tb2 O5 126.95(19) 3_756 4_565 ? O5 Tb2 O5 62.2(3) 3_756 . ? O5 Tb2 O5 72.7(5) 3_756 2_756 ? O5 Tb2 O5 128.3(4) 4_565 . ? O5 Tb2 O5 126.95(19) 2_756 . ? C4 O3 Tb1 138.3(8) . . ? C1 O2 Tb2 152.3(10) . . ? C7 O6 Tb2 108.2(8) . . ? C1 O1 Tb1 163.9(9) . . ? Tb1 O8 H8A 126.6 . . ? Tb1 O8 H8B 126.3 . . ? H8A O8 H8B 107.0 . . ? Tb1 O7 H7A 115.6 . . ? Tb1 O7 H7B 115.1 . . ? H7A O7 H7B 103.0 . . ? Tb2 O9 H9A 127.1 . . ? Tb2 O9 H9B 137.4 . . ? H9A O9 H9B 95.5 . . ? C4 O4 Tb1 140.2(8) . 3_665 ? Tb2 O5 Tb2 117.8(3) 3_756 . ? C7 O5 Tb2 153.6(9) . 3_756 ? C7 O5 Tb2 86.1(8) . . ? O2 C1 C2 119.4(13) . . ? O1 C1 O2 121.6(13) . . ? O1 C1 C2 118.9(12) . . ? O3 C4 O4 123.4(10) . . ? O3 C4 C5 121.0(10) . . ? O4 C4 C5 115.5(10) . . ? H9C C9 H9D 114.7 . . ? C8 C9 H9C 117.6 4 . ? C8 C9 H9C 117.6 . . ? C8 C9 H9D 117.6 4 . ? C8 C9 H9D 117.6 . . ? C8 C9 C8 61.6(13) . 4 ? C9 C8 C8 59.2(6) . 4 ? C9 C8 H8 114.1 . . ? C8 C8 H8 114.1 4 . ? C7 C8 C9 119.2(12) . . ? C7 C8 C8 125.0(7) . 4 ? C7 C8 H8 114.1 . . ? C1 C2 C2 124.1(8) . 4_565 ? C1 C2 H2 113.3 . . ? C2 C2 H2 113.3 4_565 . ? C3 C2 C1 123.3(13) . . ? C3 C2 C2 59.0(7) . 4_565 ? C3 C2 H2 113.3 . . ? C2 C3 C2 62.1(14) 4_565 . ? C2 C3 H3A 117.6 4_565 . ? C2 C3 H3A 117.6 . . ? C2 C3 H3B 117.6 4_565 . ? C2 C3 H3B 117.6 . . ? H3A C3 H3B 114.6 . . ? O6 C7 O5 117.6(12) . . ? O6 C7 C8 118.1(11) . . ? O5 C7 C8 124.3(12) . . ? H6A C6 H6B 114.5 . . ? C5 C6 H6A 117.5 . . ? C5 C6 H6A 117.5 4_575 . ? C5 C6 H6B 117.5 . . ? C5 C6 H6B 117.5 4_575 . ? C5 C6 C5 62.9(11) . 4_575 ? C4 C5 C6 121.0(11) . . ? C4 C5 C5 120.5(6) . 4_575 ? C4 C5 H5 115.1 . . ? C6 C5 C5 58.6(5) . 4_575 ? C6 C5 H5 115.1 . . ? C5 C5 H5 115.1 4_575 . ? 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 2.354(8) 4_575 ? Tb1 O3 2.354(8) . ? Tb1 O1 2.326(9) . ? Tb1 O1 2.326(9) 4_575 ? Tb1 O8 2.416(12) . ? Tb1 O7 2.467(12) . ? Tb1 O4 2.344(9) 2_655 ? Tb1 O4 2.344(9) 3_665 ? Tb2 O2 2.277(9) 4_565 ? Tb2 O2 2.277(9) . ? Tb2 O6 2.435(9) . ? Tb2 O6 2.435(9) 4_565 ? Tb2 O9 2.374(12) . ? Tb2 O5 2.350(9) 3_756 ? Tb2 O5 2.880(11) 4_565 ? Tb2 O5 2.880(11) . ? Tb2 O5 2.350(9) 2_756 ? O3 C4 1.259(14) . ? O2 C1 1.275(16) . ? O6 C7 1.255(16) . ? O1 C1 1.247(17) . ? O8 H8A 0.8600 . ? O8 H8B 0.8600 . ? O7 H7A 0.8600 . ? O7 H7B 0.8601 . ? O9 H9A 0.8599 . ? O9 H9B 0.8600 . ? O4 Tb1 2.344(9) 3_665 ? O4 C4 1.274(14) . ? O5 Tb2 2.350(9) 3_756 ? O5 C7 1.273(15) . ? C1 C2 1.483(19) . ? C4 C5 1.480(15) . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C9 C8 1.49(2) . ? C9 C8 1.49(2) 4 ? C8 C8 1.53(3) 4 ? C8 H8 0.9800 . ? C8 C7 1.478(17) . ? C2 C2 1.53(3) 4_565 ? C2 H2 0.9800 . ? C2 C3 1.48(2) . ? C3 C2 1.48(2) 4_565 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C5 1.493(17) . ? C6 C5 1.493(17) 4_575 ? C5 C5 1.56(2) 4_575 ? C5 H5 0.9800 . ? 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 C4 O4 -100.1(14) . . . . ? Tb1 O3 C4 C5 84.8(14) . . . . ? Tb1 O1 C1 O2 178(3) . . . . ? Tb1 O1 C1 C2 -4(5) . . . . ? Tb1 O4 C4 O3 -2(2) 3_665 . . . ? Tb1 O4 C4 C5 173.4(8) 3_665 . . . ? Tb2 O2 C1 O1 -134.6(17) . . . . ? Tb2 O2 C1 C2 48(3) . . . . ? Tb2 O6 C7 O5 -11.5(15) . . . . ? Tb2 O6 C7 C8 168.7(10) . . . . ? Tb2 O5 C7 O6 -146.6(16) 3_756 . . . ? Tb2 O5 C7 O6 9.2(12) . . . . ? Tb2 O5 C7 C8 -170.9(13) . . . . ? Tb2 O5 C7 C8 33(3) 3_756 . . . ? O3 C4 C5 C6 7.0(16) . . . . ? O3 C4 C5 C5 -62.4(12) . . . 4_575 ? O2 C1 C2 C2 -52.0(17) . . . 4_565 ? O2 C1 C2 C3 21(2) . . . . ? O1 C1 C2 C2 130.1(11) . . . 4_565 ? O1 C1 C2 C3 -157.4(14) . . . . ? O4 C4 C5 C6 -168.5(10) . . . . ? O4 C4 C5 C5 122.1(8) . . . 4_575 ? C1 C2 C3 C2 -112.8(12) . . . 4_565 ? C9 C8 C7 O6 -151.9(12) . . . . ? C9 C8 C7 O5 28(2) . . . . ? C8 C9 C8 C7 -115.6(11) 4 . . . ? C8 C8 C7 O6 137.0(9) 4 . . . ? C8 C8 C7 O5 -42.8(17) 4 . . . ? C5 C6 C5 C4 -109.0(9) 4_575 . . . ?