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The title compound, [Tb2(C24H12F9O6S3)2(C8H6N4)]·C4H8O2, has two terbium(III) centers bridged by the polyazine ligand 2,2′-bipyrimidine (bpm), which is distorted from planarity by 7.0 (2)°. The terminal ligand 4,4,4-trifluoro-1-(2-thienyl)­butane-1,3-dione (tta) is bidentate, coordinating through the two O atoms, while the bridging ligand is bis-bidentate, coordinating through four equivalent N atoms. Both the complex and the ethyl acetate solvent mol­ecules are dis­ordered. The structure was refined as a non-merohedral twin.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106008389/ga1121sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106008389/ga1121Isup2.hkl
Contains datablock I

CCDC reference: 609549

Comment top

Terbium(III) ions and their complexes have been extensively used as probes for proteins and nucleic acids due, in part, to their long-lived (millisecond) excited-state lifetimes (Fu et al., 1999; Klakamp & Horrocks, 1990). β-Diketonates are used as antenna ligands to overcome the forbidden 4f–4f transitions of lanthanide metals, thereby increasing the emission intensity of these complexes. Bridging ligands such as 2,2'-bipyrimidine (bpm) have been primarily used to link transition metals through coordination by equivalent N atoms (Balzani et al., 1996). Heteronuclear bimetallic lanthanide/transition metal complexes bridged by bpm have been synthesized and structurally characterized (Shavaleev et al., 2005). In these mixed-metal complexes, the planarity of the bpm bridging ligand is maintained and electronic communication between the two metal centers is observed. Examples of homodinuclear lanthanide complexes bridged by bpm are sparse (Sultan et al., 2006). We present here the title compound, (I), i the first structural report of a homodinuclear TbIII complex bridged by the polyazine ligand bpm.

The molecular structure of (I) is illustrated in Fig. 1. Each TbIII ion is eight-coordinate and the complex is neutral. Lanthanide(III) complexes, and particularly TbIII complexes, are very often eight-coordinate due to the large ionic radius of the metal. The coordination sphere around each TbIII ion consists of six O atoms from three 4,4,4-trifluoro-1-(2-thienyl)butane-1,3-dione (tta) ligands and two N atoms from the bpm ligand. Selected bond lengths and angles are given in Table 1. Both Tb centers are in a distorted square-antiprismatic geometry, a coordination geometry previously reported in heteronuclear bimetallic lanthanide/transition metal complexes bridged by bpm (Shavaleev et al., 2005). The approximate square planes at the Tb1 center are comprised of atoms O5, O6, N1 and N4, where the average deviation of these atoms from the mean plane is 0.306 (2) Å, and atoms O1, O2, O3 and O4, where the average deviation of these atoms from the mean plane is 0.300 (2) Å. The corresponding approximate square planes at Tb2 are comprised of atoms O9, O10, N2 and N3, with an average deviation of 0.131 (2) Å, and atoms O7, O8, O11 and O12, with an average deviation of 0.045 (2) Å (Fig. 1). These mean planes at the metal centers are nearly orthogonal, with a dihedral angle of 83.24(0.06)° at Tb1, while the corresponding value at Tb2 is 89.87 (7)°.

The intramolecular Tb1···Tb2 distance across the bridging bpm ligand is 6.7596 (5) Å. The only other relevant LnIII···LnIII distance documented to date is in the EuIII···EuIII bipyrimidine-bridged complex reported by Fernandes et al. (2005), which has a metal–metal distance of 6.856 (1) Å. The longer distance in the EuIII complex is consistent with the larger ionic radius of EuIII compared with TbIII, due to lanthanide contraction.

The individual bpm rings are planar, with a mean deviation of 0.003 (3) Å for atoms N1, C1, C2, C3, N2 and C4, and of 0.007 (3) Å for atoms N4, C5, N3, C6, C7 and C8; they are rotated from planarity by 7.0 (2)°. In lanthanide–transition metal complexes bridged by bipyrimidine, the bridging ligand is planar (Shavaleev et al., 2005). The unusual non-planarity observed in this complex is due most likely to the steric crowding of the bulky TbIII ions forcing a slight torsional twist of the bridging ligand.

Part of both the solvate and the complex are positionally disordered, as described in the Experimental section. Atom O13 of the solvate interacts weakly with the π system of the bpm ligand, based on the close O13···C4 and O13···C5 distances of 2.909 (7) and 2.799 (7) Å, respectively.

Experimental top

Synthesis of the TbIII complex was accomplished as described previously by Sultan et al. (2006), by mixing the appropriate stoichiometries of an aqueous solution of TbCl3 with a basic ethanolic solution containing bpm and tta. X-ray quality crystals were obtained by diffusion of hexanes into an ethyl acetate solution of the TbIII complex, (I), at room temperature.

Refinement top

The refinement of the structure was complicated by twinning. The structure was identified as a non-merohedral twin using RLATT (Bruker, 1998). Two p4p files were written (GEMINI; Bruker, 2000) and combined into one twinp4p file that could be read by SAINT (Bruker, 2003). SAINT integrates with both orientation matrices and separates the twin components. Corrections for absorption and decay were applied using TWINABS. The twinning law is a 180° rotation about (001). The final refinements were performed with all unique reflections using HKLF 5 format in SHELXTL (Sheldrick, 2003). A partial structure solution was obtained by direct methods and the remaining non-H atoms were located with difference Fourier techniques. Two thiophene rings of the six tta ligands show positional disorder, which can be described as 180° rotations about the C—C bonds C27—C28 and C35—C36. The occupancies refined to 0.80:0.20 for the ring S3/C28–C31 and 0.50:0.50 for the ring S4/C36–C39. Concomitantly, we find atoms of different elements (S and C) sharing almost the same site. SADI and EADP constraints were used to achieve a stable refinement for this disorder. Furthermore, four out of six tta-CF3 groups could be modeled as disordered groups. The refined model contained two or three positions for each of the F atoms with the following occupancies: F7/F8/F9 0.50:0.25:0.25; F10/F11/F12 0.55:0.45; F13/F14/F15 0.50:0.25:0.25; and F16/F17/F18 0.55:0.45. One SADI constraint was required for a stable refinement (C40—F10A and C40—F10B). Additionally, the ethyl acetate solvate molecule exhibits a 0.70:0.30 disorder of the terminal methyl group.

All non-disordered non-H atoms were refined with anisotropic atomic displacement parameters and disordered atoms were refined isotropically. The H atoms were calculated in idealized positions, with C—H distances in the range 0.95–0.99 Å, and included in the refinement as restrained atoms with appropriate occupancies, with Uiso(H) = 1.2Ueq(C). [Please check added text]

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1]
Fig. 1. The molecular structure of the title compound, showing the atom-numbering scheme for a single component of the disordered structure. For clarity, C and F atoms have not been labeled. Displacement ellipsoids are drawn at the 20% probability level for C and F, and 50% for all others. H atoms and the solvate molecule have been omitted for clarity.

Fig. 2. Please provide caption.
µ-2,2'-bipyrimidine-1κ2N1,N1':2κ2N3,N3'- bis{tris[4,4,4-trifluoro-1-(2-thienyl)butane-1,3-dionato-κ2O,O']terbium(III)} ethyl acetate solvate top
Crystal data top
[Tb2(C24H12F9O6S3)2(C8H6N4)]·C4H8O2F(000) = 1852
Mr = 1891.14Dx = 1.806 Mg m3
Triclinic, P1Melting point = 536–538 K
a = 10.0301 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.1408 (11) ÅCell parameters from 4046 reflections
c = 24.9919 (9) Åθ = 2.3–27.9°
α = 85.820 (2)°µ = 2.31 mm1
β = 86.556 (2)°T = 140 K
γ = 80.066 (2)°Columnar, pale-yellow
V = 3478.2 (4) Å30.38 × 0.12 × 0.10 mm
Z = 2
Data collection top
Bruker SMART 6000 CCD area-detector
diffractometer
23700 independent reflections
Radiation source: fine-focus sealed tube23095 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
ω scansθmax = 27.9°, θmin = 0.8°
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2002; Blessing, 1995)
h = 1313
Tmin = 0.62, Tmax = 0.79k = 1717
23700 measured reflectionsl = 032
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121H-atom parameters constrained
S = 1.18 w = 1/[σ2(Fo2) + (0.0577P)2 + 15.0158P]
where P = (Fo2 + 2Fc2)/3
23700 reflections(Δ/σ)max = 0.003
944 parametersΔρmax = 2.01 e Å3
4 restraintsΔρmin = 0.97 e Å3
Crystal data top
[Tb2(C24H12F9O6S3)2(C8H6N4)]·C4H8O2γ = 80.066 (2)°
Mr = 1891.14V = 3478.2 (4) Å3
Triclinic, P1Z = 2
a = 10.0301 (8) ÅMo Kα radiation
b = 14.1408 (11) ŵ = 2.31 mm1
c = 24.9919 (9) ÅT = 140 K
α = 85.820 (2)°0.38 × 0.12 × 0.10 mm
β = 86.556 (2)°
Data collection top
Bruker SMART 6000 CCD area-detector
diffractometer
23700 independent reflections
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2002; Blessing, 1995)
23095 reflections with I > 2σ(I)
Tmin = 0.62, Tmax = 0.79Rint = 0.000
23700 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0424 restraints
wR(F2) = 0.121H-atom parameters constrained
S = 1.18 w = 1/[σ2(Fo2) + (0.0577P)2 + 15.0158P]
where P = (Fo2 + 2Fc2)/3
23700 reflectionsΔρmax = 2.01 e Å3
944 parametersΔρmin = 0.97 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Tb10.72239 (2)1.233100 (16)0.656112 (9)0.01852 (6)
Tb21.05073 (2)0.889387 (16)0.826229 (9)0.01908 (6)
S10.95900 (15)1.47143 (12)0.73977 (8)0.0419 (4)
S21.08648 (13)0.96614 (10)0.59354 (7)0.0320 (3)
S3A0.3863 (2)1.52036 (14)0.58724 (8)0.0327 (4)*0.80
C29A0.5605 (9)1.6057 (6)0.5332 (4)0.031 (2)*0.80
H29A0.64361.62090.51760.038*0.80
S3B0.5872 (9)1.6196 (7)0.5264 (4)0.038 (2)*0.20
C29B0.4144 (16)1.5470 (18)0.5871 (9)0.031 (2)*0.20
H29B0.37871.51760.61890.038*0.20
S4A0.7046 (3)1.0476 (3)0.95515 (14)0.0270 (8)*0.50
C37A0.8487 (19)1.1577 (13)1.0028 (8)0.028 (3)*0.50
H37A0.92191.18341.01520.034*0.50
S4B0.8630 (6)1.1703 (4)1.0019 (3)0.0491 (15)*0.50
C37B0.7094 (14)1.0724 (10)0.9550 (6)0.028 (3)*0.50
H37B0.67641.03690.92930.034*0.50
S51.41821 (17)0.61028 (12)0.87158 (8)0.0467 (4)
S60.78335 (15)0.80783 (13)0.67773 (6)0.0389 (3)
O20.7778 (3)1.3522 (2)0.70639 (15)0.0231 (7)
O10.5322 (3)1.2854 (2)0.71083 (15)0.0240 (7)
O30.5654 (4)1.1623 (3)0.61674 (16)0.0294 (8)
O40.8396 (3)1.0963 (2)0.61590 (15)0.0240 (7)
O50.8910 (3)1.2904 (2)0.60195 (15)0.0250 (8)
O60.6173 (3)1.3698 (2)0.60740 (15)0.0256 (8)
O80.9446 (4)0.9803 (3)0.89452 (15)0.0271 (8)
O71.2104 (3)0.9679 (3)0.86062 (15)0.0270 (8)
O101.1703 (4)0.7444 (3)0.86192 (16)0.0301 (8)
O90.8953 (4)0.8006 (2)0.87069 (15)0.0258 (8)
O120.9863 (4)0.8247 (3)0.75161 (15)0.0267 (8)
O111.2443 (3)0.8548 (3)0.76883 (15)0.0260 (8)
O140.7931 (6)0.3256 (3)0.8748 (2)0.0549 (13)
O130.8399 (7)0.1950 (4)0.8284 (2)0.0733 (17)
N10.7052 (4)1.0935 (3)0.72767 (17)0.0202 (8)
N40.9361 (4)1.1662 (3)0.70751 (17)0.0201 (8)
N20.8170 (4)0.9786 (3)0.79154 (17)0.0205 (8)
N31.0528 (4)1.0402 (3)0.76405 (16)0.0199 (8)
C10.5902 (5)1.0598 (4)0.7403 (2)0.0259 (11)
H10.51121.08810.72210.031*
C20.5812 (5)0.9861 (4)0.7785 (2)0.0276 (11)
H20.49810.96350.78710.033*
C30.6982 (5)0.9463 (4)0.8040 (2)0.0237 (10)
H30.69560.89520.83080.028*
C40.8138 (4)1.0506 (3)0.75443 (19)0.0177 (9)
C50.9424 (5)1.0878 (3)0.74077 (19)0.0190 (9)
C61.1683 (5)1.0755 (4)0.7524 (2)0.0242 (10)
H61.24991.04310.76740.029*
C71.1714 (5)1.1575 (4)0.7192 (2)0.0268 (11)
H71.25271.18280.71170.032*
C81.0522 (5)1.2008 (4)0.6978 (2)0.0257 (11)
H81.05151.25780.67510.031*
C90.4931 (5)1.3686 (4)0.7289 (2)0.0252 (11)
C100.5671 (5)1.4368 (4)0.7379 (2)0.0286 (11)
H100.52141.49600.75070.034*
C110.7105 (5)1.4235 (3)0.7290 (2)0.0228 (10)
C120.7866 (5)1.4929 (4)0.7487 (2)0.0243 (10)
C130.7375 (5)1.5779 (3)0.7770 (2)0.0205 (10)
H130.64581.60140.78740.025*
C140.8531 (7)1.6206 (4)0.7867 (3)0.0392 (14)
H140.84511.67940.80370.047*
C150.9737 (6)1.5710 (4)0.7700 (3)0.0385 (14)
H151.05801.59050.77480.046*
C160.3398 (6)1.3873 (4)0.7439 (3)0.0417 (16)
C170.5714 (5)1.0875 (4)0.5912 (2)0.0256 (11)
C180.6805 (5)1.0228 (4)0.5757 (2)0.0279 (11)
H180.66730.97080.55570.033*
C190.8145 (5)1.0310 (3)0.5885 (2)0.0216 (10)
C200.9301 (5)0.9616 (3)0.5695 (2)0.0238 (10)
C210.9383 (5)0.8926 (3)0.5313 (2)0.0261 (11)
H210.86350.87920.51330.031*
C221.0740 (6)0.8457 (4)0.5235 (3)0.0353 (13)
H221.10020.79670.49900.042*
C231.1629 (6)0.8765 (4)0.5539 (3)0.0358 (14)
H231.25710.85130.55330.043*
C240.4308 (6)1.0719 (5)0.5765 (3)0.0394 (15)
C250.8971 (5)1.3751 (4)0.5810 (2)0.0259 (11)
C260.7944 (5)1.4485 (4)0.5706 (2)0.0329 (13)
H260.81601.50720.55450.040*
C270.6565 (5)1.4420 (4)0.5825 (2)0.0275 (11)
C280.5508 (5)1.5229 (4)0.5667 (2)0.0266 (11)
C300.4296 (6)1.6656 (4)0.5249 (3)0.0403 (14)
H300.41341.72450.50350.048*
C310.3356 (7)1.6230 (5)0.5529 (3)0.0436 (15)
H310.24241.65110.55290.052*
C321.0433 (6)1.3897 (5)0.5661 (2)0.0340 (13)
C331.2040 (5)1.0310 (4)0.8943 (2)0.0288 (11)
C341.0964 (5)1.0699 (4)0.9266 (2)0.0290 (12)
H341.10851.11640.95070.035*
C350.9679 (5)1.0424 (4)0.9250 (2)0.0253 (11)
C360.8533 (5)1.0868 (4)0.9589 (2)0.0271 (11)
C380.6287 (6)1.1239 (5)0.9987 (2)0.0419 (16)
H380.53421.12981.00740.050*
C390.7049 (7)1.1770 (5)1.0214 (3)0.0472 (16)
H390.67001.22261.04700.057*
C401.3370 (6)1.0714 (5)0.8945 (3)0.0410 (15)
C410.9057 (6)0.7298 (4)0.9049 (2)0.0286 (11)
C421.0204 (6)0.6666 (4)0.9186 (2)0.0291 (12)
H421.01360.61620.94540.035*
C431.1492 (5)0.6754 (4)0.8934 (2)0.0254 (11)
C441.2669 (6)0.6010 (4)0.9052 (2)0.0310 (12)
C451.2785 (6)0.5188 (4)0.9429 (3)0.0394 (14)
H451.20710.50050.96590.047*
C461.4135 (8)0.4697 (5)0.9402 (4)0.058 (2)
H461.44320.41300.96200.070*
C471.4978 (7)0.5093 (5)0.9042 (3)0.0519 (18)
H471.59090.48340.89800.062*
C480.7729 (6)0.7166 (5)0.9340 (3)0.0405 (14)
C491.2709 (5)0.7996 (4)0.7305 (2)0.0299 (12)
C501.1832 (5)0.7595 (4)0.7028 (2)0.0321 (12)
H501.21940.71530.67660.039*
C511.0419 (5)0.7809 (4)0.7116 (2)0.0250 (10)
C520.9511 (6)0.7552 (4)0.6738 (2)0.0320 (12)
C530.9789 (7)0.6929 (5)0.6314 (3)0.0434 (16)
H531.06510.65690.62200.052*
C540.8563 (8)0.6927 (6)0.6047 (3)0.0512 (19)
H540.85290.65510.57490.061*
C550.7477 (7)0.7492 (6)0.6248 (3)0.0495 (18)
H550.66000.75600.61110.059*
C561.4202 (6)0.7822 (5)0.7123 (3)0.0399 (14)
C570.6099 (9)0.2547 (7)0.8550 (4)0.075 (3)
H57A0.58890.20080.83640.112*
H57B0.56250.31540.83870.112*
H57C0.58040.24830.89300.112*
C580.7576 (9)0.2543 (5)0.8504 (3)0.0518 (18)
C59A0.9347 (10)0.3294 (6)0.8742 (4)0.072 (2)
H59A0.97090.34360.83730.093*0.70
H59B0.98630.26790.88900.093*0.70
C60A0.9417 (16)0.4120 (10)0.9104 (6)0.079 (4)*0.70
H60A0.85440.42900.93010.119*0.70
H60B0.96230.46810.88820.119*0.70
H60C1.01300.39120.93600.119*0.70
H59C0.96410.32590.83580.093*0.30
H59D0.97420.26650.89160.093*0.30
C60B1.017 (4)0.398 (3)0.8941 (16)0.087 (11)*0.30
H60D1.10780.38730.87680.131*0.30
H60E1.02290.38720.93320.131*0.30
H60F0.97250.46430.88540.131*0.30
F10.3071 (4)1.3234 (4)0.78192 (19)0.0658 (13)
F20.2694 (4)1.3763 (3)0.70222 (19)0.0559 (11)
F30.2961 (4)1.4737 (3)0.7602 (3)0.092 (2)
F40.3779 (4)1.1381 (3)0.5394 (2)0.0737 (15)
F50.3464 (4)1.0757 (4)0.6198 (2)0.0742 (16)
F60.4293 (4)0.9875 (3)0.55660 (18)0.0552 (11)
F7A1.0971 (11)1.3518 (8)0.5269 (5)0.040 (3)*0.50
F8A1.0516 (11)1.4856 (8)0.5526 (5)0.028 (3)*0.50
F9A1.1244 (9)1.3632 (8)0.6073 (4)0.023 (2)*0.50
F7B1.0783 (18)1.3434 (14)0.5162 (7)0.030 (4)*0.25
F8B1.054 (2)1.4909 (15)0.5648 (8)0.035 (6)*0.25
F9B1.1311 (16)1.3377 (12)0.5971 (7)0.033 (5)*0.25
F7C1.1111 (15)1.3114 (11)0.5329 (6)0.031 (3)*0.25
F8C1.0674 (15)1.4598 (11)0.5391 (6)0.032 (4)*0.25
F9C1.1076 (16)1.3877 (12)0.6141 (7)0.028 (5)*0.25
F10A1.4441 (8)1.0158 (7)0.8984 (4)0.044 (3)*0.55
F11A1.3289 (7)1.1448 (5)0.9294 (3)0.0359 (16)*0.55
F12A1.3647 (9)1.1145 (6)0.8480 (3)0.036 (2)*0.55
F10B1.4467 (8)0.9898 (7)0.8964 (4)0.032 (2)*0.45
F11B1.3529 (8)1.1101 (6)0.9398 (3)0.0323 (18)*0.45
F12B1.3372 (11)1.1372 (8)0.8485 (4)0.039 (3)*0.45
F13A0.6715 (8)0.7269 (7)0.8962 (3)0.0380 (18)*0.50
F14A0.7723 (8)0.6309 (6)0.9596 (4)0.0412 (18)*0.50
F15A0.7351 (9)0.7853 (7)0.9686 (4)0.0447 (19)*0.50
F13B0.6619 (17)0.7584 (13)0.9140 (8)0.047 (4)*0.25
F14B0.7547 (14)0.6186 (10)0.9379 (7)0.033 (3)*0.25
F15B0.7652 (19)0.7401 (16)0.9849 (8)0.060 (5)*0.25
F13C0.6989 (17)0.7978 (11)0.9486 (7)0.042 (4)*0.25
F15C0.7860 (16)0.6605 (13)0.9809 (7)0.047 (4)*0.25
F14C0.699 (2)0.6818 (15)0.9067 (8)0.061 (5)*0.25
F16A1.4611 (7)0.6971 (5)0.6910 (3)0.0409 (17)*0.55
F17A1.4537 (9)0.8504 (6)0.6812 (4)0.044 (2)*0.55
F18A1.5006 (7)0.7747 (6)0.7586 (3)0.0324 (18)*0.55
F16B1.4517 (9)0.7237 (7)0.6711 (4)0.046 (2)*0.45
F17B1.4550 (10)0.8720 (8)0.6924 (4)0.042 (3)*0.45
F18B1.4957 (12)0.7521 (9)0.7482 (5)0.056 (3)*0.45
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb10.01408 (11)0.01832 (11)0.02337 (12)0.00201 (8)0.00318 (9)0.00261 (10)
Tb20.01533 (11)0.02011 (11)0.02205 (12)0.00443 (8)0.00096 (9)0.00038 (10)
S10.0255 (7)0.0402 (8)0.0628 (11)0.0093 (6)0.0001 (7)0.0147 (8)
S20.0201 (6)0.0294 (7)0.0475 (9)0.0029 (5)0.0055 (6)0.0084 (6)
S50.0336 (8)0.0393 (8)0.0625 (11)0.0009 (6)0.0022 (8)0.0071 (8)
S60.0278 (7)0.0567 (10)0.0351 (8)0.0126 (7)0.0009 (6)0.0101 (7)
O20.0173 (17)0.0233 (17)0.0291 (19)0.0021 (13)0.0026 (14)0.0058 (15)
O10.0192 (17)0.0217 (17)0.031 (2)0.0028 (13)0.0014 (14)0.0014 (15)
O30.0187 (18)0.032 (2)0.040 (2)0.0048 (15)0.0072 (15)0.0117 (17)
O40.0154 (16)0.0240 (18)0.034 (2)0.0019 (13)0.0039 (14)0.0092 (15)
O50.0181 (17)0.0259 (18)0.030 (2)0.0016 (14)0.0006 (14)0.0006 (15)
O60.0214 (18)0.0253 (18)0.029 (2)0.0021 (14)0.0034 (15)0.0034 (15)
O80.0210 (18)0.033 (2)0.031 (2)0.0091 (15)0.0017 (15)0.0091 (16)
O70.0205 (18)0.035 (2)0.0267 (19)0.0080 (15)0.0039 (14)0.0011 (16)
O100.0223 (19)0.0302 (19)0.036 (2)0.0050 (15)0.0012 (16)0.0069 (16)
O90.0211 (18)0.0239 (18)0.032 (2)0.0052 (14)0.0005 (15)0.0001 (15)
O120.0207 (18)0.034 (2)0.0261 (19)0.0068 (15)0.0025 (15)0.0067 (16)
O110.0206 (18)0.0260 (18)0.031 (2)0.0042 (14)0.0013 (15)0.0018 (15)
O140.079 (4)0.037 (3)0.051 (3)0.012 (2)0.011 (3)0.006 (2)
O130.107 (5)0.062 (3)0.052 (3)0.013 (3)0.011 (3)0.024 (3)
N10.0160 (19)0.0195 (19)0.026 (2)0.0024 (15)0.0004 (16)0.0086 (16)
N40.018 (2)0.0185 (19)0.025 (2)0.0038 (15)0.0054 (16)0.0002 (16)
N20.0168 (19)0.021 (2)0.024 (2)0.0038 (15)0.0003 (16)0.0031 (16)
N30.0167 (19)0.023 (2)0.021 (2)0.0053 (16)0.0010 (15)0.0003 (16)
C10.015 (2)0.029 (3)0.034 (3)0.0003 (19)0.003 (2)0.004 (2)
C20.014 (2)0.031 (3)0.038 (3)0.005 (2)0.003 (2)0.000 (2)
C30.018 (2)0.026 (2)0.027 (3)0.0060 (19)0.0017 (19)0.002 (2)
C40.014 (2)0.016 (2)0.023 (2)0.0022 (17)0.0001 (18)0.0058 (18)
C50.019 (2)0.020 (2)0.019 (2)0.0045 (18)0.0017 (18)0.0055 (18)
C60.019 (2)0.023 (2)0.030 (3)0.0027 (19)0.005 (2)0.003 (2)
C70.016 (2)0.026 (3)0.039 (3)0.007 (2)0.000 (2)0.001 (2)
C80.024 (3)0.023 (2)0.030 (3)0.006 (2)0.006 (2)0.002 (2)
C90.017 (2)0.028 (3)0.029 (3)0.0003 (19)0.003 (2)0.000 (2)
C100.019 (2)0.027 (3)0.040 (3)0.002 (2)0.003 (2)0.014 (2)
C110.024 (3)0.021 (2)0.024 (3)0.0050 (19)0.001 (2)0.0015 (19)
C120.016 (2)0.026 (3)0.031 (3)0.0050 (19)0.001 (2)0.004 (2)
C130.017 (2)0.013 (2)0.034 (3)0.0059 (17)0.007 (2)0.0040 (19)
C140.046 (4)0.030 (3)0.045 (4)0.015 (3)0.001 (3)0.008 (3)
C150.029 (3)0.037 (3)0.054 (4)0.016 (2)0.002 (3)0.006 (3)
C160.023 (3)0.038 (3)0.067 (5)0.007 (2)0.000 (3)0.017 (3)
C170.020 (2)0.033 (3)0.028 (3)0.012 (2)0.007 (2)0.002 (2)
C180.026 (3)0.025 (3)0.036 (3)0.009 (2)0.002 (2)0.010 (2)
C190.022 (2)0.019 (2)0.025 (3)0.0084 (19)0.0004 (19)0.0005 (19)
C200.022 (2)0.020 (2)0.030 (3)0.0054 (19)0.001 (2)0.001 (2)
C210.022 (3)0.021 (2)0.033 (3)0.0017 (19)0.005 (2)0.002 (2)
C220.036 (3)0.023 (3)0.045 (4)0.002 (2)0.006 (3)0.009 (2)
C230.019 (3)0.025 (3)0.061 (4)0.000 (2)0.003 (3)0.005 (3)
C240.023 (3)0.055 (4)0.045 (4)0.012 (3)0.001 (2)0.021 (3)
C250.023 (3)0.036 (3)0.019 (2)0.008 (2)0.0017 (19)0.003 (2)
C260.024 (3)0.034 (3)0.041 (3)0.011 (2)0.011 (2)0.016 (2)
C270.027 (3)0.030 (3)0.026 (3)0.006 (2)0.009 (2)0.003 (2)
C280.024 (3)0.028 (3)0.027 (3)0.004 (2)0.000 (2)0.001 (2)
C300.056 (4)0.025 (3)0.036 (3)0.003 (3)0.001 (3)0.001 (2)
C310.037 (3)0.046 (4)0.039 (4)0.011 (3)0.003 (3)0.004 (3)
C320.028 (3)0.049 (4)0.025 (3)0.010 (3)0.003 (2)0.006 (3)
C330.026 (3)0.036 (3)0.027 (3)0.012 (2)0.008 (2)0.003 (2)
C340.028 (3)0.035 (3)0.028 (3)0.012 (2)0.006 (2)0.006 (2)
C350.021 (2)0.030 (3)0.026 (3)0.010 (2)0.002 (2)0.001 (2)
C360.028 (3)0.030 (3)0.023 (3)0.004 (2)0.000 (2)0.006 (2)
C380.026 (3)0.061 (4)0.035 (4)0.004 (3)0.001 (3)0.008 (3)
C390.049 (4)0.047 (4)0.045 (4)0.002 (3)0.002 (3)0.015 (3)
C400.031 (3)0.065 (4)0.034 (3)0.023 (3)0.002 (2)0.014 (3)
C410.035 (3)0.023 (3)0.032 (3)0.014 (2)0.001 (2)0.005 (2)
C420.028 (3)0.027 (3)0.032 (3)0.009 (2)0.002 (2)0.006 (2)
C430.029 (3)0.018 (2)0.029 (3)0.005 (2)0.002 (2)0.002 (2)
C440.028 (3)0.030 (3)0.035 (3)0.005 (2)0.004 (2)0.003 (2)
C450.032 (3)0.028 (3)0.054 (4)0.002 (2)0.005 (3)0.010 (3)
C460.050 (4)0.041 (4)0.076 (6)0.005 (3)0.010 (4)0.023 (4)
C470.033 (3)0.039 (4)0.081 (6)0.000 (3)0.010 (3)0.005 (4)
C480.029 (3)0.038 (3)0.054 (4)0.010 (3)0.007 (3)0.003 (3)
C490.021 (3)0.024 (3)0.041 (3)0.000 (2)0.006 (2)0.003 (2)
C500.023 (3)0.037 (3)0.035 (3)0.001 (2)0.006 (2)0.014 (2)
C510.023 (3)0.028 (3)0.025 (3)0.007 (2)0.003 (2)0.004 (2)
C520.024 (3)0.035 (3)0.041 (3)0.013 (2)0.004 (2)0.010 (2)
C530.039 (3)0.061 (4)0.036 (3)0.024 (3)0.010 (3)0.015 (3)
C540.058 (4)0.071 (5)0.035 (4)0.033 (4)0.007 (3)0.026 (3)
C550.040 (4)0.080 (5)0.038 (4)0.035 (4)0.002 (3)0.009 (3)
C560.024 (3)0.048 (4)0.047 (4)0.005 (3)0.005 (3)0.007 (3)
C570.083 (6)0.070 (6)0.077 (6)0.033 (5)0.023 (5)0.019 (5)
C580.076 (5)0.036 (4)0.044 (4)0.011 (3)0.009 (4)0.004 (3)
C59A0.081 (6)0.052 (5)0.082 (7)0.015 (4)0.018 (5)0.013 (4)
F10.034 (2)0.101 (4)0.063 (3)0.022 (2)0.015 (2)0.002 (3)
F20.0229 (18)0.071 (3)0.074 (3)0.0046 (17)0.0122 (18)0.005 (2)
F30.023 (2)0.063 (3)0.194 (6)0.0025 (19)0.020 (3)0.074 (4)
F40.046 (3)0.069 (3)0.110 (4)0.008 (2)0.049 (3)0.002 (3)
F50.029 (2)0.131 (4)0.077 (3)0.039 (2)0.021 (2)0.059 (3)
F60.0268 (19)0.072 (3)0.077 (3)0.0213 (18)0.0043 (18)0.038 (2)
Geometric parameters (Å, º) top
Tb1—O32.307 (3)C18—C191.425 (7)
Tb1—O52.321 (3)C18—H180.9500
Tb1—O12.325 (3)C19—C201.464 (7)
Tb1—O22.332 (3)C20—C211.401 (7)
Tb1—O62.332 (3)C21—C221.417 (7)
Tb1—O42.343 (3)C21—H210.9500
Tb1—N42.568 (4)C22—C231.351 (9)
Tb1—N12.586 (4)C22—H220.9500
Tb2—O82.308 (4)C23—H230.9500
Tb2—O122.309 (4)C24—F61.330 (7)
Tb2—O102.335 (4)C24—F51.330 (7)
Tb2—O72.336 (3)C24—F41.334 (8)
Tb2—O92.346 (3)C25—C261.352 (8)
Tb2—O112.347 (4)C25—C321.535 (7)
Tb2—N32.547 (4)C26—C271.415 (7)
Tb2—N22.628 (4)C26—H260.9500
S1—C151.678 (6)C27—C281.467 (7)
S1—C121.708 (5)C30—C311.341 (9)
S2—C231.712 (6)C30—H300.9500
S2—C201.726 (5)C31—H310.9500
S3A—C311.649 (6)C32—F7A1.205 (12)
S3A—C281.704 (6)C32—F8C1.209 (16)
C29A—C281.404 (10)C32—F9B1.301 (17)
C29A—C301.452 (10)C32—F9A1.342 (11)
C29A—H29A0.9500C32—F8A1.389 (13)
S3B—C301.604 (9)C32—F9C1.392 (17)
S3B—C281.715 (12)C32—F7B1.448 (19)
C29B—C281.424 (13)C32—F8B1.45 (2)
C29B—C311.472 (13)C32—F7C1.478 (16)
C29B—H29B0.9500C33—C341.369 (8)
S4A—C381.649 (7)C33—C401.540 (7)
S4A—C361.688 (6)C34—C351.413 (7)
C37A—C391.47 (2)C34—H340.9500
C37A—C361.533 (19)C35—C361.463 (7)
C37A—H37A0.9500C38—C391.335 (9)
S4B—C391.620 (10)C38—H380.9500
S4B—C361.672 (8)C39—H390.9500
C37B—C381.479 (15)C40—F10A1.221 (10)
C37B—C361.502 (15)C40—F12A1.311 (10)
C37B—H37B0.9500C40—F11B1.321 (10)
S5—C471.690 (7)C40—F11A1.392 (9)
S5—C441.711 (6)C40—F12B1.426 (12)
S6—C551.698 (7)C40—F10B1.451 (11)
S6—C521.718 (6)C41—C421.374 (8)
O2—C111.263 (6)C41—C481.513 (8)
O1—C91.280 (6)C42—C431.424 (7)
O3—C171.266 (6)C42—H420.9500
O4—C191.257 (6)C43—C441.468 (8)
O5—C251.282 (6)C44—C451.434 (8)
O6—C271.265 (6)C45—C461.412 (9)
O8—C351.264 (6)C45—H450.9500
O7—C331.261 (7)C46—C471.355 (11)
O10—C431.247 (6)C46—H460.9500
O9—C411.263 (6)C47—H470.9500
O12—C511.265 (6)C48—F14C1.22 (2)
O11—C491.267 (7)C48—F13B1.279 (18)
O14—C581.323 (8)C48—F13C1.318 (17)
O14—C59A1.430 (10)C48—F14A1.328 (10)
O13—C581.209 (9)C48—F15B1.33 (2)
N1—C11.335 (6)C48—F15A1.338 (11)
N1—C41.342 (6)C48—F15C1.366 (17)
N4—C51.331 (6)C48—F13A1.413 (11)
N4—C81.342 (6)C48—F14B1.425 (15)
N2—C41.323 (6)C49—C501.370 (8)
N2—C31.360 (6)C49—C561.522 (7)
N3—C51.334 (6)C50—C511.404 (7)
N3—C61.348 (6)C50—H500.9500
C1—C21.373 (7)C51—C521.457 (7)
C1—H10.9500C52—C531.411 (8)
C2—C31.382 (7)C53—C541.434 (9)
C2—H20.9500C53—H530.9500
C3—H30.9500C54—C551.330 (10)
C4—C51.488 (6)C54—H540.9500
C6—C71.379 (7)C55—H550.9500
C6—H60.9500C56—F18B1.215 (13)
C7—C81.367 (7)C56—F17A1.274 (10)
C7—H70.9500C56—F16A1.342 (9)
C8—H80.9500C56—F16B1.357 (11)
C9—C101.353 (7)C56—F17B1.422 (12)
C9—C161.543 (8)C56—F18A1.437 (10)
C10—C111.424 (7)C57—C581.478 (12)
C10—H100.9500C57—H57A0.9800
C11—C121.470 (7)C57—H57B0.9800
C12—C131.436 (7)C57—H57C0.9800
C13—C141.436 (7)C59A—C60A1.541 (17)
C13—H130.9500C59A—H59A0.9900
C14—C151.349 (9)C59A—H59B0.9900
C14—H140.9500C60A—H60A0.9800
C15—H150.9500C60A—H60B0.9800
C16—F31.309 (7)C60A—H60C0.9800
C16—F21.326 (8)C60B—H60D0.9800
C16—F11.328 (8)C60B—H60E0.9800
C17—C181.357 (8)C60B—H60F0.9800
C17—C241.534 (7)
O3—Tb1—O5118.87 (14)F4—C24—C17111.6 (5)
O3—Tb1—O180.58 (13)O5—C25—C26128.7 (5)
O5—Tb1—O1141.60 (12)O5—C25—C32112.4 (5)
O3—Tb1—O2151.17 (12)C26—C25—C32118.9 (5)
O5—Tb1—O277.60 (13)C25—C26—C27123.3 (5)
O1—Tb1—O273.30 (12)C25—C26—H26118.4
O3—Tb1—O682.44 (13)C27—C26—H26118.4
O5—Tb1—O673.40 (12)O6—C27—C26123.5 (5)
O1—Tb1—O677.38 (13)O6—C27—C28116.8 (5)
O2—Tb1—O680.18 (12)C26—C27—C28119.7 (5)
O3—Tb1—O472.42 (12)C29A—C28—C29B99.7 (10)
O5—Tb1—O476.00 (12)C29A—C28—C27129.8 (6)
O1—Tb1—O4142.06 (12)C29B—C28—C27129.9 (8)
O2—Tb1—O4136.39 (12)C29A—C28—S3A110.4 (5)
O6—Tb1—O4123.35 (13)C27—C28—S3A119.7 (4)
O3—Tb1—N4133.52 (13)C29B—C28—S3B107.3 (8)
O5—Tb1—N477.70 (13)C27—C28—S3B121.8 (5)
O1—Tb1—N4114.17 (13)C31—C30—C29A107.7 (6)
O2—Tb1—N470.31 (12)C31—C30—S3B120.8 (6)
O6—Tb1—N4142.31 (12)C31—C30—H30126.2
O4—Tb1—N470.56 (12)C29A—C30—H30126.2
O3—Tb1—N181.29 (13)S3B—C30—H30113.0
O5—Tb1—N1137.33 (12)C30—C31—C29B104.2 (9)
O1—Tb1—N174.34 (12)C30—C31—S3A118.1 (5)
O2—Tb1—N1102.70 (13)C30—C31—H31121.0
O6—Tb1—N1149.25 (12)C29B—C31—H31133.4
O4—Tb1—N175.62 (13)S3A—C31—H31121.0
N4—Tb1—N163.12 (12)F7A—C32—F9A108.2 (9)
O8—Tb2—O12136.74 (13)F7A—C32—F8A101.4 (9)
O8—Tb2—O10110.11 (14)F9A—C32—F8A105.7 (8)
O12—Tb2—O1095.03 (14)F8C—C32—F9C107.0 (11)
O8—Tb2—O771.98 (12)F9B—C32—F7B100.4 (12)
O12—Tb2—O7145.66 (13)F9B—C32—F8B111.5 (12)
O10—Tb2—O788.27 (13)F7B—C32—F8B116.1 (12)
O8—Tb2—O973.42 (13)F8C—C32—F7C101.2 (11)
O12—Tb2—O982.59 (13)F9C—C32—F7C110.7 (10)
O10—Tb2—O971.52 (12)F7A—C32—C25116.7 (7)
O7—Tb2—O9130.29 (13)F8C—C32—C25121.5 (9)
O8—Tb2—O11146.73 (12)F9B—C32—C25112.9 (9)
O12—Tb2—O1172.64 (13)F9A—C32—C25111.8 (6)
O10—Tb2—O1174.68 (13)F8A—C32—C25112.1 (6)
O7—Tb2—O1175.37 (13)F9C—C32—C25106.8 (8)
O9—Tb2—O11135.69 (12)F7B—C32—C25104.9 (8)
O8—Tb2—N390.97 (13)F8B—C32—C25110.6 (10)
O12—Tb2—N384.49 (13)F7C—C32—C25109.3 (7)
O10—Tb2—N3147.92 (13)O7—C33—C34129.4 (5)
O7—Tb2—N375.23 (13)O7—C33—C40112.1 (5)
O9—Tb2—N3139.59 (12)C34—C33—C40118.4 (5)
O11—Tb2—N374.60 (13)C33—C34—C35121.5 (5)
O8—Tb2—N272.95 (13)C33—C34—H34119.2
O12—Tb2—N266.81 (13)C35—C34—H34119.2
O10—Tb2—N2145.55 (12)O8—C35—C34122.8 (5)
O7—Tb2—N2123.57 (12)O8—C35—C36116.6 (4)
O9—Tb2—N277.05 (12)C34—C35—C36120.6 (5)
O11—Tb2—N2122.41 (13)C35—C36—C37B124.7 (7)
N3—Tb2—N262.67 (12)C35—C36—C37A130.0 (8)
C15—S1—C1292.1 (3)C35—C36—S4B124.0 (4)
C23—S2—C2091.2 (3)C37B—C36—S4B111.0 (7)
C31—S3A—C2891.3 (3)C35—C36—S4A117.2 (4)
C28—C29A—C30112.6 (7)C37A—C36—S4A112.5 (8)
C28—C29A—H29A123.7C39—C38—C37B109.3 (8)
C30—C29A—H29A123.7C39—C38—S4A117.5 (5)
C30—S3B—C2891.3 (6)C39—C38—H38121.2
C28—C29B—C31111.8 (11)C37B—C38—H38128.8
C28—C29B—H29B124.1S4A—C38—H38121.2
C31—C29B—H29B124.1C38—C39—C37A113.2 (9)
C38—S4A—C3691.8 (3)C38—C39—S4B119.3 (6)
C39—C37A—C36104.3 (11)C38—C39—H39123.4
C39—C37A—H37A127.8C37A—C39—H39123.4
C36—C37A—H37A127.8S4B—C39—H39117.2
C39—S4B—C3692.4 (4)F10A—C40—F12A97.9 (7)
C38—C37B—C36107.0 (9)F10A—C40—F11A110.8 (7)
C38—C37B—H37B126.5F12A—C40—F11A102.4 (7)
C36—C37B—H37B126.5F11B—C40—F12B113.4 (7)
C47—S5—C4492.2 (3)F11B—C40—F10B100.4 (7)
C55—S6—C5292.0 (3)F12B—C40—F10B116.6 (7)
C11—O2—Tb1134.5 (3)F10A—C40—C33119.3 (7)
C9—O1—Tb1128.6 (3)F12A—C40—C33111.4 (6)
C17—O3—Tb1134.6 (3)F11B—C40—C33113.5 (6)
C19—O4—Tb1138.5 (3)F11A—C40—C33112.7 (5)
C25—O5—Tb1130.5 (3)F12B—C40—C33105.9 (6)
C27—O6—Tb1135.2 (3)F10B—C40—C33107.1 (6)
C35—O8—Tb2139.8 (3)O9—C41—C42128.2 (5)
C33—O7—Tb2134.0 (3)O9—C41—C48113.7 (5)
C43—O10—Tb2138.7 (3)C42—C41—C48118.0 (5)
C41—O9—Tb2134.0 (3)C41—C42—C43121.2 (5)
C51—O12—Tb2138.3 (3)C41—C42—H42119.4
C49—O11—Tb2131.6 (3)C43—C42—H42119.4
C58—O14—C59A116.9 (7)O10—C43—C42123.9 (5)
C1—N1—C4116.0 (4)O10—C43—C44116.6 (5)
C1—N1—Tb1122.9 (3)C42—C43—C44119.5 (5)
C4—N1—Tb1121.0 (3)C45—C44—C43130.0 (5)
C5—N4—C8116.0 (4)C45—C44—S5111.7 (4)
C5—N4—Tb1121.4 (3)C43—C44—S5118.3 (4)
C8—N4—Tb1122.1 (3)C46—C45—C44108.7 (6)
C4—N2—C3116.5 (4)C46—C45—H45125.6
C4—N2—Tb2119.8 (3)C44—C45—H45125.6
C3—N2—Tb2123.0 (3)C47—C46—C45115.1 (6)
C5—N3—C6116.2 (4)C47—C46—H46122.4
C5—N3—Tb2123.0 (3)C45—C46—H46122.4
C6—N3—Tb2120.8 (3)C46—C47—S5112.2 (5)
N1—C1—C2122.8 (5)C46—C47—H47123.9
N1—C1—H1118.6S5—C47—H47123.9
C2—C1—H1118.6F14C—C48—F13C104.5 (14)
C1—C2—C3117.1 (5)F13B—C48—F15B105.8 (13)
C1—C2—H2121.5F14A—C48—F15A109.4 (8)
C3—C2—H2121.5F14C—C48—F15C106.6 (13)
N2—C3—C2121.3 (5)F13C—C48—F15C103.7 (12)
N2—C3—H3119.4F14A—C48—F13A105.8 (7)
C2—C3—H3119.4F15A—C48—F13A107.2 (7)
N2—C4—N1126.3 (4)F13B—C48—F14B101.6 (11)
N2—C4—C5117.3 (4)F15B—C48—F14B103.9 (12)
N1—C4—C5116.5 (4)F14C—C48—C41113.0 (11)
N4—C5—N3126.3 (4)F13B—C48—C41119.0 (10)
N4—C5—C4117.2 (4)F13C—C48—C41113.5 (8)
N3—C5—C4116.5 (4)F14A—C48—C41115.1 (6)
N3—C6—C7121.8 (5)F15B—C48—C41113.0 (9)
N3—C6—H6119.1F15A—C48—C41110.1 (6)
C7—C6—H6119.1F15C—C48—C41114.5 (8)
C8—C7—C6117.1 (5)F13A—C48—C41108.8 (6)
C8—C7—H7121.4F14B—C48—C41112.0 (7)
C6—C7—H7121.4O11—C49—C50128.5 (5)
N4—C8—C7122.6 (5)O11—C49—C56113.3 (5)
N4—C8—H8118.7C50—C49—C56118.1 (5)
C7—C8—H8118.7C49—C50—C51122.7 (5)
O1—C9—C10129.3 (5)C49—C50—H50118.6
O1—C9—C16112.2 (4)C51—C50—H50118.6
C10—C9—C16118.5 (5)O12—C51—C50122.6 (5)
C9—C10—C11122.8 (5)O12—C51—C52116.3 (5)
C9—C10—H10118.6C50—C51—C52121.1 (5)
C11—C10—H10118.6C53—C52—C51129.9 (5)
O2—C11—C10123.0 (4)C53—C52—S6111.6 (5)
O2—C11—C12117.4 (4)C51—C52—S6118.5 (4)
C10—C11—C12119.6 (4)C52—C53—C54109.1 (6)
C13—C12—C11129.3 (4)C52—C53—H53125.4
C13—C12—S1112.7 (4)C54—C53—H53125.4
C11—C12—S1118.0 (4)C55—C54—C53114.8 (6)
C12—C13—C14107.2 (5)C55—C54—H54122.6
C12—C13—H13126.4C53—C54—H54122.6
C14—C13—H13126.4C54—C55—S6112.5 (5)
C15—C14—C13115.1 (5)C54—C55—H55123.8
C15—C14—H14122.5S6—C55—H55123.8
C13—C14—H14122.5F17A—C56—F16A110.8 (7)
C14—C15—S1112.8 (4)F18B—C56—F16B108.2 (9)
C14—C15—H15123.6F18B—C56—F17B106.5 (8)
S1—C15—H15123.6F16B—C56—F17B105.1 (8)
F3—C16—F2107.8 (6)F17A—C56—F18A106.9 (6)
F3—C16—F1108.5 (6)F16A—C56—F18A102.9 (6)
F2—C16—F1105.1 (5)F18B—C56—C49113.9 (8)
F3—C16—C9113.3 (5)F17A—C56—C49113.0 (6)
F2—C16—C9110.5 (5)F16A—C56—C49113.5 (6)
F1—C16—C9111.3 (5)F16B—C56—C49114.7 (6)
O3—C17—C18129.9 (5)F17B—C56—C49107.9 (6)
O3—C17—C24112.0 (5)F18A—C56—C49109.0 (6)
C18—C17—C24118.1 (5)C58—C57—H57A109.5
C17—C18—C19121.7 (5)C58—C57—H57B109.5
C17—C18—H18119.2H57A—C57—H57B109.5
C19—C18—H18119.2C58—C57—H57C109.5
O4—C19—C18122.8 (5)H57A—C57—H57C109.5
O4—C19—C20117.1 (4)H57B—C57—H57C109.5
C18—C19—C20120.1 (4)O13—C58—O14122.3 (8)
C21—C20—C19130.4 (5)O13—C58—C57125.1 (8)
C21—C20—S2112.0 (4)O14—C58—C57112.6 (7)
C19—C20—S2117.6 (4)O14—C59A—C60A103.6 (9)
C20—C21—C22110.3 (5)O14—C59A—H59A111.0
C20—C21—H21124.9C60A—C59A—H59A111.0
C22—C21—H21124.9O14—C59A—H59B111.0
C23—C22—C21114.2 (5)C60A—C59A—H59B111.0
C23—C22—H22122.9H59A—C59A—H59B109.0
C21—C22—H22122.9C59A—C60A—H60A109.5
C22—C23—S2112.3 (4)C59A—C60A—H60B109.5
C22—C23—H23123.8H60A—C60A—H60B109.5
S2—C23—H23123.8C59A—C60A—H60C109.5
F6—C24—F5106.0 (5)H60A—C60A—H60C109.5
F6—C24—F4105.6 (5)H60B—C60A—H60C109.5
F5—C24—F4108.5 (6)H60D—C60B—H60E109.5
F6—C24—C17114.3 (5)H60D—C60B—H60F109.5
F5—C24—C17110.5 (5)H60E—C60B—H60F109.5

Experimental details

Crystal data
Chemical formula[Tb2(C24H12F9O6S3)2(C8H6N4)]·C4H8O2
Mr1891.14
Crystal system, space groupTriclinic, P1
Temperature (K)140
a, b, c (Å)10.0301 (8), 14.1408 (11), 24.9919 (9)
α, β, γ (°)85.820 (2), 86.556 (2), 80.066 (2)
V3)3478.2 (4)
Z2
Radiation typeMo Kα
µ (mm1)2.31
Crystal size (mm)0.38 × 0.12 × 0.10
Data collection
DiffractometerBruker SMART 6000 CCD area-detector
diffractometer
Absorption correctionMulti-scan
(TWINABS; Sheldrick, 2002; Blessing, 1995)
Tmin, Tmax0.62, 0.79
No. of measured, independent and
observed [I > 2σ(I)] reflections
23700, 23700, 23095
Rint0.000
(sin θ/λ)max1)0.659
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.121, 1.18
No. of reflections23700
No. of parameters944
No. of restraints4
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0577P)2 + 15.0158P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.01, 0.97

Computer programs: SMART (Bruker, 2000), SMART, SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2004), SHELXL97.

Selected geometric parameters (Å, º) top
Tb1—O32.307 (3)Tb2—O82.308 (4)
Tb1—O52.321 (3)Tb2—O122.309 (4)
Tb1—O12.325 (3)Tb2—O102.335 (4)
Tb1—O22.332 (3)Tb2—O72.336 (3)
Tb1—O62.332 (3)Tb2—O92.346 (3)
Tb1—O42.343 (3)Tb2—O112.347 (4)
Tb1—N42.568 (4)Tb2—N32.547 (4)
Tb1—N12.586 (4)Tb2—N22.628 (4)
O1—Tb1—O273.30 (12)O8—Tb2—O771.98 (12)
O5—Tb1—O673.40 (12)O10—Tb2—O971.52 (12)
O3—Tb1—O472.42 (12)O12—Tb2—O1172.64 (13)
N4—Tb1—N163.12 (12)N3—Tb2—N262.67 (12)
 

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