data_compound8 #===================================================================== # corresponding information _publ_contact_author_name 'Professor Dr. Guo-Cong Guo & Ming-Sheng Wang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_phone '+86 591 8370 5882' _publ_contact_author_fax '+86 591 8371 4946' _publ_contact_author_email 'mswang@fjirsm.ac.cn & gcguo@fjirsm.ac.cn' #===================================================================== _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'H8 N3 O13 Tb, C7 H7 N5' _chemical_formula_sum 'C7 H15 N8 O13 Tb' _chemical_formula_weight 578.19 _chemical_melting_point ? 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' 'N' 'N' 0.0061 0.0033 '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' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 6.5400(4) _cell_length_b 10.7434(6) _cell_length_c 13.3014(9) _cell_angle_alpha 90.105(5) _cell_angle_beta 92.035(5) _cell_angle_gamma 100.717(6) _cell_volume 917.67(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7413 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.1400 _cell_measurement_theta_min 2.5830 _exptl_absorpt_coefficient_mu 3.938 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.39117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 564 _exptl_crystal_preparation Fiber _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 9165 _diffrn_reflns_theta_full 27.10 _diffrn_reflns_theta_max 27.10 _diffrn_reflns_theta_min 2.45 _diffrn_ambient_temperature 298(2) _diffrn_detector PILT _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measurement_device_type 'Rigaku Pilatus 200K' _diffrn_measurement_method CCD_Profile_fitting _diffrn_measurement_specimen_support Fiber _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Rotating Anode' _diffrn_source_current 80.0 _diffrn_source_power 4.0 _diffrn_source_voltage 50.0 _diffrn_special_details ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3713 _reflns_number_total 4065 _reflns_odcompleteness_completeness 96.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.04 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015) ; _computing_data_collection ; CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear-SM Expert 2.1 b45 (Rigaku, 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-97 (Sheldrick, 1990)' _refine_diff_density_max 0.718 _refine_diff_density_min -1.407 _refine_diff_density_rms 0.234 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 4065 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0280 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.0764 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances O17-H17B = O17-H17A = O16-H16A = O16-H16B = O15-H15A = O15-H15B = O14-H14A = O14-H14B 0.85 with sigma of 0.01 3.a Aromatic/amide H refined with riding coordinates: C23(H23), C24(H24), C25(H25), C26(H26) 3.b Idealised Me refined as rotating group: C27(H27A,H27B,H27C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn N11 N 0.2280(5) 0.5991(3) 0.3545(2) 0.0358(7) Uani 1 d . . . N12 N 0.3470(6) 0.5123(3) 0.1078(3) 0.0431(8) Uani 1 d . . . N13 N 0.2712(5) 0.8721(3) 0.0506(2) 0.0372(7) Uani 1 d . . . O11A O 0.4204(4) 0.6212(3) 0.3730(2) 0.0433(6) Uani 1 d . . . O11B O 0.1654(4) 0.6543(3) 0.27752(19) 0.0354(6) Uani 1 d . . . O11C O 0.1065(6) 0.5294(4) 0.4055(3) 0.0677(10) Uani 1 d . . . O12A O 0.4640(6) 0.5243(3) 0.1867(3) 0.0552(8) Uani 1 d . . . O12B O 0.3100(6) 0.6119(3) 0.0710(2) 0.0585(8) Uani 1 d . . . O12C O 0.2780(7) 0.4065(3) 0.0735(3) 0.0740(11) Uani 1 d . . . O13A O 0.2136(5) 0.8537(3) 0.1410(2) 0.0422(6) Uani 1 d . . . O13B O 0.4507(4) 0.8605(3) 0.0326(2) 0.0448(6) Uani 1 d . . . O13C O 0.1474(5) 0.8982(4) -0.0149(3) 0.0656(10) Uani 1 d . . . O14 O 0.7808(4) 0.7189(3) 0.1091(2) 0.0517(8) Uani 1 d . . D H14B H 0.766(9) 0.676(5) 0.054(3) 0.077 Uiso 1 d . . DR H14A H 0.893(5) 0.763(5) 0.090(4) 0.077 Uiso 1 d . . DR O15 O 0.7227(5) 0.9591(3) 0.1884(2) 0.0425(6) Uani 1 d . . D H15B H 0.732(8) 0.999(4) 0.133(2) 0.064 Uiso 1 d . . DR H15A H 0.794(7) 1.003(4) 0.235(3) 0.064 Uiso 1 d . . DR O16 O 0.8022(4) 0.7453(3) 0.3148(2) 0.0458(7) Uani 1 d . . D H16A H 0.835(8) 0.772(5) 0.3744(17) 0.069 Uiso 1 d . . DR H16B H 0.906(6) 0.717(5) 0.294(4) 0.069 Uiso 1 d . . DR O17 O 0.4445(4) 0.8921(2) 0.3459(2) 0.0388(6) Uani 1 d . . D H17B H 0.347(5) 0.883(5) 0.387(3) 0.058 Uiso 1 d . . DR H17A H 0.530(7) 0.958(3) 0.365(4) 0.058 Uiso 1 d . . DR Tb1 Tb 0.50527(2) 0.757349(12) 0.213015(10) 0.02463(8) Uani 1 d . . . C21 C 0.9090(5) 0.8319(3) 0.6042(3) 0.0269(7) Uani 1 d . . . C22 C 0.7129(5) 0.7850(3) 0.6524(3) 0.0285(7) Uani 1 d . . . C23 C 0.6777(6) 0.8281(4) 0.7481(3) 0.0374(8) Uani 1 d . . . H23 H 0.7770 0.8895 0.7807 0.045 Uiso 1 calc . . R C24 C 0.4964(6) 0.7795(4) 0.7938(3) 0.0404(9) Uani 1 d . . . H24 H 0.4740 0.8081 0.8578 0.048 Uiso 1 calc . . R C25 C 0.3778(6) 0.6485(4) 0.6553(3) 0.0386(8) Uani 1 d . . . H25 H 0.2748 0.5881 0.6241 0.046 Uiso 1 calc . . R C26 C 0.5581(6) 0.6941(3) 0.6065(3) 0.0343(8) Uani 1 d . . . H26 H 0.5767 0.6640 0.5425 0.041 Uiso 1 calc . . R C27 C 0.1606(7) 0.6378(5) 0.8026(4) 0.0518(11) Uani 1 d . . . H27A H 0.0862 0.5642 0.7672 0.078 Uiso 1 calc . . GR H27B H 0.0731 0.7000 0.8067 0.078 Uiso 1 calc . . GR H27C H 0.1994 0.6143 0.8692 0.078 Uiso 1 calc . . GR N21 N 0.9479(5) 0.8101(3) 0.5085(2) 0.0335(6) Uani 1 d . . . N22 N 1.1438(5) 0.8676(3) 0.4970(2) 0.0355(7) Uani 1 d . . . N23 N 1.2207(5) 0.9223(3) 0.5823(3) 0.0374(7) Uani 1 d . . . N24 N 1.0761(5) 0.9015(3) 0.6513(2) 0.0334(6) Uani 1 d . . . N25 N 0.3502(5) 0.6913(3) 0.7481(3) 0.0360(7) Uani 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 N11 0.0354(17) 0.0393(15) 0.0310(16) 0.0049(12) 0.0054(13) 0.0017(13) N12 0.056(2) 0.0366(15) 0.0369(18) -0.0061(13) 0.0149(16) 0.0056(15) N13 0.0330(17) 0.0428(16) 0.0332(17) 0.0072(13) -0.0007(14) 0.0007(13) O11A 0.0384(15) 0.0534(16) 0.0367(15) 0.0016(12) -0.0053(12) 0.0059(13) O11B 0.0284(13) 0.0452(13) 0.0329(14) 0.0062(11) 0.0049(11) 0.0072(11) O11C 0.059(2) 0.083(2) 0.055(2) 0.0300(18) 0.0204(17) -0.0051(18) O12A 0.064(2) 0.0513(16) 0.053(2) -0.0167(14) -0.0064(17) 0.0198(15) O12B 0.072(2) 0.0577(18) 0.0431(18) -0.0013(14) -0.0064(16) 0.0057(16) O12C 0.106(3) 0.0519(18) 0.055(2) -0.0247(16) 0.006(2) -0.0097(19) O13A 0.0439(16) 0.0550(16) 0.0313(14) 0.0095(12) 0.0082(12) 0.0170(13) O13B 0.0332(15) 0.0639(17) 0.0350(15) -0.0015(13) 0.0038(12) 0.0024(13) O13C 0.0443(17) 0.097(3) 0.052(2) 0.0364(18) -0.0078(15) 0.0062(17) O14 0.0298(15) 0.078(2) 0.0440(17) -0.0272(15) 0.0092(13) -0.0002(14) O15 0.0464(16) 0.0469(15) 0.0251(14) -0.0039(11) 0.0024(12) -0.0150(13) O16 0.0274(14) 0.083(2) 0.0291(14) -0.0137(14) -0.0049(12) 0.0183(14) O17 0.0362(15) 0.0414(13) 0.0349(15) -0.0144(11) 0.0159(12) -0.0056(11) Tb1 0.01846(11) 0.03281(11) 0.02176(11) -0.00524(7) 0.00199(7) 0.00237(7) C21 0.0273(17) 0.0285(14) 0.0243(16) -0.0023(12) -0.0007(13) 0.0041(12) C22 0.0301(17) 0.0274(14) 0.0281(17) 0.0004(12) 0.0019(14) 0.0057(13) C23 0.037(2) 0.0422(19) 0.032(2) -0.0100(15) 0.0048(16) 0.0043(16) C24 0.040(2) 0.0456(19) 0.036(2) -0.0036(15) 0.0100(18) 0.0088(16) C25 0.0322(19) 0.0400(18) 0.041(2) -0.0020(16) 0.0016(16) 0.0000(15) C26 0.0349(19) 0.0384(17) 0.0277(18) -0.0025(14) 0.0017(15) 0.0015(15) C27 0.038(2) 0.059(3) 0.057(3) 0.009(2) 0.021(2) 0.0037(19) N21 0.0307(15) 0.0425(15) 0.0247(15) -0.0047(12) 0.0031(12) -0.0007(12) N22 0.0297(15) 0.0452(16) 0.0291(16) -0.0020(13) 0.0051(12) -0.0003(13) N23 0.0327(16) 0.0423(16) 0.0331(16) -0.0047(13) 0.0036(13) -0.0040(13) N24 0.0308(16) 0.0382(14) 0.0272(15) -0.0058(11) 0.0032(12) -0.0044(12) N25 0.0322(17) 0.0403(16) 0.0369(18) 0.0052(13) 0.0108(14) 0.0087(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N11 O11A 1.252(4) . ? N11 O11B 1.278(4) . ? N11 O11C 1.212(4) . ? N12 O12A 1.268(5) . ? N12 O12B 1.238(4) . ? N12 O12C 1.223(4) . ? N13 O13A 1.277(4) . ? N13 O13B 1.235(4) . ? N13 O13C 1.236(4) . ? O11A Tb1 2.602(3) . ? O11B Tb1 2.475(2) . ? O12A Tb1 2.490(3) . ? O12B Tb1 2.592(3) . ? O13A Tb1 2.498(3) . ? O13B Tb1 2.685(3) . ? O14 H14B 0.851(10) . ? O14 H14A 0.846(10) . ? O14 Tb1 2.405(3) . ? O15 H15B 0.846(10) . ? O15 H15A 0.850(10) . ? O15 Tb1 2.391(3) . ? O16 H16A 0.850(10) . ? O16 H16B 0.851(10) . ? O16 Tb1 2.351(3) . ? O17 H17B 0.848(10) . ? O17 H17A 0.849(10) . ? O17 Tb1 2.373(2) . ? C21 C22 1.459(5) . ? C21 N21 1.337(4) . ? C21 N24 1.338(4) . ? C22 C23 1.396(5) . ? C22 C26 1.392(5) . ? C23 H23 0.9300 . ? C23 C24 1.367(6) . ? C24 H24 0.9300 . ? C24 N25 1.342(5) . ? C25 H25 0.9300 . ? C25 C26 1.376(5) . ? C25 N25 1.347(5) . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C27 N25 1.481(5) . ? N21 N22 1.329(4) . ? N22 N23 1.316(5) . ? N23 N24 1.330(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 O11A N11 O11B 115.8(3) . . ? O11C N11 O11A 122.9(3) . . ? O11C N11 O11B 121.3(3) . . ? O12B N12 O12A 116.0(3) . . ? O12C N12 O12A 119.6(4) . . ? O12C N12 O12B 124.4(4) . . ? O13B N13 O13A 117.3(3) . . ? O13B N13 O13C 122.8(3) . . ? O13C N13 O13A 119.9(3) . . ? N11 O11A Tb1 94.3(2) . . ? N11 O11B Tb1 99.77(19) . . ? N12 O12A Tb1 99.3(2) . . ? N12 O12B Tb1 95.1(2) . . ? N13 O13A Tb1 100.3(2) . . ? N13 O13B Tb1 92.4(2) . . ? H14B O14 H14A 91(5) . . ? Tb1 O14 H14B 126(4) . . ? Tb1 O14 H14A 135(4) . . ? H15B O15 H15A 111(5) . . ? Tb1 O15 H15B 125(4) . . ? Tb1 O15 H15A 124(4) . . ? H16A O16 H16B 106(5) . . ? Tb1 O16 H16A 130(4) . . ? Tb1 O16 H16B 123(4) . . ? H17B O17 H17A 106(5) . . ? Tb1 O17 H17B 130(3) . . ? Tb1 O17 H17A 124(4) . . ? O11A Tb1 O13B 159.50(10) . . ? O11B Tb1 O11A 49.87(8) . . ? O11B Tb1 O12A 71.42(11) . . ? O11B Tb1 O12B 72.52(10) . . ? O11B Tb1 O13A 68.29(9) . . ? O11B Tb1 O13B 110.18(8) . . ? O12A Tb1 O11A 64.82(10) . . ? O12A Tb1 O12B 49.39(11) . . ? O12A Tb1 O13A 114.87(11) . . ? O12A Tb1 O13B 107.30(10) . . ? O12B Tb1 O11A 102.63(10) . . ? O12B Tb1 O13B 61.89(9) . . ? O13A Tb1 O11A 115.41(9) . . ? O13A Tb1 O12B 70.62(10) . . ? O13A Tb1 O13B 48.76(9) . . ? O14 Tb1 O11A 119.24(11) . . ? O14 Tb1 O11B 142.17(10) . . ? O14 Tb1 O12A 71.97(12) . . ? O14 Tb1 O12B 76.69(11) . . ? O14 Tb1 O13A 120.69(11) . . ? O14 Tb1 O13B 72.38(11) . . ? O15 Tb1 O11A 132.08(9) . . ? O15 Tb1 O11B 143.00(10) . . ? O15 Tb1 O12A 145.55(11) . . ? O15 Tb1 O12B 125.17(10) . . ? O15 Tb1 O13A 86.44(10) . . ? O15 Tb1 O13B 65.52(9) . . ? O15 Tb1 O14 73.85(11) . . ? O16 Tb1 O11A 66.98(10) . . ? O16 Tb1 O11B 116.70(10) . . ? O16 Tb1 O12A 87.40(12) . . ? O16 Tb1 O12B 132.38(11) . . ? O16 Tb1 O13A 156.86(11) . . ? O16 Tb1 O13B 133.11(10) . . ? O16 Tb1 O14 70.55(10) . . ? O16 Tb1 O15 77.27(12) . . ? O16 Tb1 O17 81.79(10) . . ? O17 Tb1 O11A 71.40(9) . . ? O17 Tb1 O11B 75.54(9) . . ? O17 Tb1 O12A 135.66(10) . . ? O17 Tb1 O12B 141.32(11) . . ? O17 Tb1 O13A 77.73(10) . . ? O17 Tb1 O13B 111.39(10) . . ? O17 Tb1 O14 140.47(10) . . ? O17 Tb1 O15 72.88(9) . . ? N21 C21 C22 125.0(3) . . ? N21 C21 N24 110.9(3) . . ? N24 C21 C22 124.1(3) . . ? C23 C22 C21 120.4(3) . . ? C26 C22 C21 121.7(3) . . ? C26 C22 C23 117.8(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23 120.2 . . ? C23 C24 H24 119.4 . . ? N25 C24 C23 121.3(4) . . ? N25 C24 H24 119.4 . . ? C26 C25 H25 119.9 . . ? N25 C25 H25 119.9 . . ? N25 C25 C26 120.2(4) . . ? C22 C26 H26 119.8 . . ? C25 C26 C22 120.4(3) . . ? C25 C26 H26 119.8 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N25 C27 H27A 109.5 . . ? N25 C27 H27B 109.5 . . ? N25 C27 H27C 109.5 . . ? N22 N21 C21 105.1(3) . . ? N23 N22 N21 109.6(3) . . ? N22 N23 N24 109.3(3) . . ? N23 N24 C21 105.1(3) . . ? C24 N25 C25 120.7(3) . . ? C24 N25 C27 119.2(4) . . ? C25 N25 C27 120.1(4) . . ?