supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers buy article online

zl2078 scheme

Acta Cryst. (2007). E63, m3110    [ doi:10.1107/S1600536807057765 ]

Poly[diaquatris([mu]4-benzene-1,3-dicarboxylato)diterbium(III)]

Z. Rong-Hua

Abstract top

The title terbium coordination polymer, {[Tb2(C8H4O4)3(H2O)2]}n, was obtained by the hydrothermal reaction of Tb(NO3)3 with benzene-1,3-dicarboxylic acid (1,3-BDC) in alkaline aqueous solution. In the asymmetric unit, there are two crystallographically independent TbIII ions: one seven-coordinate Tb centre is coordinated by six O atoms from six 1,3-BDC ligands and one water molecule, and the other Tb centre is eight-coordinate and surrounded by seven O atoms from six 1,3-BDC ligands and one water molecule. The bridging ligands link the metal centres, forming a three-dimensional network which is further stabilized by hydrogen-bonding interactions. One benzene ring is disordered over two positions with site occupancies of 0.60 (3) and 0.40 (3).

Comment top

As a building block, benzene-1,3-dicarboxylic acid (1,3-BDC) is an excellent candidate for the construction of supramolecular complexes (De Bettencourt-Dias, 2005; Zhang et al., 2003). Recently, we obtained the title coordination polymer by the reaction of Tb(NO3)3 with benzene-1,3-dicarboxylic acid in alkaline aqueous solution, and its crystal structure is reported here.

In the asymmetric unit of the title complex, there are two crystallographically independent TbIII ions: one seven-coordinate Tb centre is coordinated by six oxygen atoms from six 1,3-BDC ligands and one water molecule, and the other Tb centre is eight-coordinate and surrounded by seven oxygen atoms from six 1,3-BDC ligands and one water molecules (Fig. 1). The adjacent Tb···Tb separations are 4.690 (4) and 4.698 (5) Å, respectively. The carboxylate groups of 1,3-BDC ligands are distinct, one of which acts as bis(monodentate) bridge, the other acts as chelate and monodentate bridge. They cross-link the metal ions to form a three-dimensional network (Fig. 2). The crystal structure is stabilized by intra/intermolecular O—H···O and C—H····O hydrogen bonding interactions (Table 1).

Related literature top

De Bettencourt-Dias (2005) and Zhang et al. (2003) have described the use of benzene-1,3-dicarboxylic acid (1,3-BDC) in the construction of supramolecular complexes.

Experimental top

A mixture of Tb(NO3)3 (0.5 mmol, 0.172 g), benzenedicarboxylic acid (0.75 mmol, 0.125 g), NaOH (1.5 mmol; 0.06 g) and H2O (12 ml) was placed in a 23 ml Teflon reactor, which was heated to 433 K for three days and then cooled to room temperature at a rate of 10 K h−1. The crystals obtained were washed with water and dryed in air.

Refinement top

One of the phenyl rings was found to be split into two positions and the occupancy ratio refined to 0.60 (3) to 0.40 (3). Due to the significant overlap of the disordered atoms the following restraints were applied: The phenyl ring C10 C11 C12 C13 C14 C15 and its disordered counterpart were each restrained to be flat and their equivalent bond distances were restrained to be the same within a standard deviation of 0.01 Å. All water H atoms were tentatively located in difference density Fourier maps and were refined with O–H distance restraints of 0.82 (1) Å and with Uiso(H) = 1.5 Ueq(O). Carbon-bound H atoms were placed at calculated positions and were treated as riding on the parent C atoms with C—H = 0.93 Å, and with Uiso(H) = 1.2 Ueq(C).

Computing details top

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

Figures top
[Figure 1] Fig. 1. The molecular structure showing the atomic-numbering scheme and displacement ellipsoids drawn at the 30% probability level.
[Figure 2] Fig. 2. The molecular packing showing the intermolecular hydrogen bonding interactions as broken lines. The minor moieties of the disordered phenyl rings were omitted for clarity.
Poly[diaquatris(m4-benzene-1,3-dicarboxylato)diterbium(III)] top
Crystal data top
[Tb2(C8H4O4)3(H2O)2]F000 = 1608
Mr = 846.21Dx = 2.245 Mg m−3
Monoclinic, P21/nMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4289 reflections
a = 13.2647 (3) Åθ = 1.7–28.0º
b = 14.3741 (3) ŵ = 5.68 mm−1
c = 13.5323 (3) ÅT = 296 (2) K
β = 103.9440 (10)ºBlock, colorless
V = 2504.14 (9) Å30.15 × 0.14 × 0.11 mm
Z = 4
Data collection top
Bruker APEX-II area-detector
diffractometer		5182 independent reflections
Radiation source: fine-focus sealed tube3834 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.077
T = 296(2) Kθmax = 26.5º
φ and ω scanθmin = 1.9º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −16→16
Tmin = 0.445, Tmax = 0.538k = −17→18
35926 measured reflectionsl = −16→16
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.073  w = 1/[σ2(Fo2) + (0.0245P)2 + 8.8675P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
5182 reflectionsΔρmax = 2.21 e Å−3
410 parametersΔρmin = −1.08 e Å−3
66 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Tb2(C8H4O4)3(H2O)2]V = 2504.14 (9) Å3
Mr = 846.21Z = 4
Monoclinic, P21/nMo Kα
a = 13.2647 (3) ŵ = 5.68 mm−1
b = 14.3741 (3) ÅT = 296 (2) K
c = 13.5323 (3) Å0.15 × 0.14 × 0.11 mm
β = 103.9440 (10)º
Data collection top
Bruker APEX-II area-detector
diffractometer		5182 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		3834 reflections with I > 2σ(I)
Tmin = 0.445, Tmax = 0.538Rint = 0.077
35926 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03466 restraints
wR(F2) = 0.073H atoms treated by a mixture of
independent and constrained refinement
S = 1.02Δρmax = 2.21 e Å−3
5182 reflectionsΔρmin = −1.08 e Å−3
410 parameters
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)
C10.8731 (5)0.1394 (4)0.1428 (4)0.0231 (14)
C20.9120 (5)0.2379 (4)0.1428 (5)0.0273 (15)
C30.8840 (5)0.3000 (4)0.2099 (5)0.0292 (15)
H30.84300.28010.25280.035*
C40.9166 (5)0.3912 (4)0.2132 (5)0.0285 (15)
C50.9762 (6)0.4214 (5)0.1484 (6)0.0418 (19)
H50.99740.48320.14980.050*
C61.0044 (7)0.3588 (5)0.0808 (6)0.051 (2)
H61.04430.37880.03700.061*
C70.9728 (6)0.2667 (5)0.0792 (6)0.0382 (18)
H70.99250.22450.03530.046*
C80.8853 (5)0.4571 (4)0.2847 (5)0.0272 (15)
C90.6369 (6)0.4092 (5)0.1246 (5)0.0339 (17)
C100.6583 (6)0.4838 (5)0.0566 (5)0.0377 (18)
C110.6834 (13)0.5728 (7)0.0950 (9)0.021 (7)0.40 (3)
H110.67390.58900.15870.025*0.40 (3)
C130.738 (2)0.6150 (13)−0.0580 (11)0.026 (5)0.40 (3)
H130.76780.6582−0.09320.032*0.40 (3)
C140.708 (3)0.5288 (13)−0.1007 (15)0.041 (6)0.40 (3)
H140.70830.5155−0.16770.049*0.40 (3)
C150.677 (2)0.4638 (14)−0.0398 (12)0.039 (6)0.40 (3)
H150.66700.4029−0.06340.047*0.40 (3)
C11'0.7033 (11)0.5661 (6)0.1000 (7)0.022 (4)0.60 (3)
H11'0.72030.57360.17030.026*0.60 (3)
C13'0.6938 (16)0.6260 (9)−0.0677 (7)0.033 (4)0.60 (3)
H13'0.70370.6746−0.10970.040*0.60 (3)
C14'0.6506 (17)0.5431 (9)−0.1100 (10)0.039 (4)0.60 (3)
H14'0.63620.5353−0.18020.047*0.60 (3)
C15'0.6286 (15)0.4723 (9)−0.0504 (7)0.033 (4)0.60 (3)
H15'0.59520.4185−0.07950.040*0.60 (3)
C120.7224 (5)0.6369 (4)0.0379 (5)0.0312 (16)
C160.7631 (5)0.7280 (4)0.0848 (5)0.0226 (14)
C170.6837 (5)0.0910 (4)−0.0429 (4)0.0225 (14)
C180.7180 (5)0.1586 (4)−0.1142 (5)0.0258 (15)
C190.6553 (6)0.2320 (5)−0.1574 (5)0.0332 (16)
H190.58970.2385−0.14500.040*
C200.6886 (6)0.2954 (5)−0.2183 (5)0.0378 (18)
H200.64450.3427−0.24970.045*
C210.7881 (5)0.2886 (5)−0.2329 (5)0.0341 (17)
H210.81190.3332−0.27160.041*
C220.8525 (5)0.2159 (4)−0.1901 (5)0.0270 (15)
C230.8166 (5)0.1504 (5)−0.1316 (4)0.0256 (15)
H230.85890.1006−0.10380.031*
C240.9607 (5)0.2067 (5)−0.2044 (5)0.0279 (15)
O10.7873 (3)0.1236 (3)0.1631 (3)0.0279 (10)
O20.9288 (4)0.0743 (3)0.1211 (4)0.0335 (11)
O30.9080 (4)0.5415 (3)0.2778 (4)0.0390 (12)
O40.8359 (4)0.4262 (3)0.3473 (4)0.0364 (12)
O50.6263 (4)0.3265 (3)0.0916 (4)0.0436 (13)
O60.6325 (4)0.4317 (3)0.2125 (4)0.0423 (13)
O70.7630 (3)0.7967 (3)0.0277 (3)0.0290 (11)
O80.7966 (4)0.7328 (3)0.1800 (3)0.0311 (11)
O90.6139 (3)0.1186 (3)−0.0012 (3)0.0301 (11)
O100.7277 (3)0.0131 (3)−0.0287 (3)0.0275 (10)
O111.0184 (4)0.1465 (3)−0.1523 (3)0.0329 (11)
O120.9859 (4)0.2601 (3)−0.2675 (4)0.0360 (12)
O1W0.4451 (4)0.1564 (5)0.0500 (4)0.0564 (17)
H1W0.387 (3)0.178 (6)0.048 (6)0.085*
H2W0.436 (6)0.121 (5)0.002 (5)0.085*
O2W0.8967 (4)−0.0717 (4)−0.0413 (4)0.0432 (13)
H3W0.948 (3)−0.075 (6)−0.066 (5)0.065*
H4W0.849 (3)−0.059 (6)−0.091 (3)0.065*
Tb10.61128 (2)0.18274 (2)0.15619 (2)0.02036 (8)
Tb20.82716 (2)−0.06625 (2)0.11562 (2)0.02429 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.022 (4)0.025 (3)0.022 (3)0.002 (3)0.004 (3)−0.006 (3)
C20.026 (4)0.023 (4)0.035 (4)−0.004 (3)0.011 (3)−0.002 (3)
C30.029 (4)0.025 (4)0.036 (4)−0.004 (3)0.013 (3)−0.010 (3)
C40.027 (4)0.021 (3)0.041 (4)0.001 (3)0.016 (3)−0.004 (3)
C50.058 (5)0.017 (4)0.058 (5)−0.009 (4)0.031 (4)−0.006 (3)
C60.066 (6)0.034 (5)0.069 (6)−0.012 (4)0.051 (5)−0.008 (4)
C70.046 (5)0.029 (4)0.048 (4)−0.001 (3)0.028 (4)−0.008 (3)
C80.021 (4)0.024 (4)0.039 (4)0.000 (3)0.012 (3)−0.007 (3)
C90.039 (5)0.030 (4)0.031 (4)−0.005 (3)0.003 (3)0.008 (3)
C100.053 (5)0.024 (4)0.034 (4)−0.010 (3)0.007 (4)0.005 (3)
C110.013 (8)0.018 (9)0.026 (10)0.006 (7)−0.006 (6)−0.001 (7)
C130.028 (10)0.020 (8)0.031 (8)0.002 (7)0.008 (7)−0.002 (6)
C140.055 (11)0.040 (9)0.030 (8)0.003 (8)0.016 (8)−0.009 (7)
C150.040 (11)0.033 (9)0.046 (9)−0.007 (8)0.012 (7)−0.006 (7)
C11'0.028 (7)0.019 (7)0.019 (6)0.001 (5)0.006 (5)0.004 (5)
C13'0.039 (8)0.025 (6)0.032 (6)−0.001 (6)0.001 (5)0.004 (5)
C14'0.050 (9)0.033 (7)0.032 (6)−0.005 (6)0.006 (6)0.001 (5)
C15'0.034 (8)0.027 (6)0.038 (6)−0.009 (6)0.006 (5)−0.003 (5)
C120.042 (4)0.022 (4)0.029 (4)−0.004 (3)0.007 (3)0.001 (3)
C160.016 (3)0.024 (4)0.028 (3)−0.002 (3)0.005 (3)−0.002 (3)
C170.015 (3)0.030 (4)0.022 (3)−0.003 (3)0.003 (3)−0.001 (3)
C180.024 (4)0.026 (4)0.030 (3)−0.003 (3)0.012 (3)−0.002 (3)
C190.024 (4)0.038 (4)0.038 (4)0.007 (3)0.010 (3)0.001 (3)
C200.031 (4)0.034 (4)0.049 (4)0.011 (3)0.010 (3)0.010 (3)
C210.032 (4)0.030 (4)0.042 (4)0.006 (3)0.014 (3)0.007 (3)
C220.026 (4)0.025 (4)0.032 (4)0.005 (3)0.013 (3)0.003 (3)
C230.025 (4)0.031 (4)0.023 (3)0.000 (3)0.009 (3)0.002 (3)
C240.027 (4)0.030 (4)0.028 (3)0.004 (3)0.009 (3)0.007 (3)
O10.021 (3)0.031 (3)0.033 (3)−0.006 (2)0.010 (2)−0.006 (2)
O20.029 (3)0.022 (3)0.052 (3)−0.002 (2)0.015 (2)−0.009 (2)
O30.051 (3)0.021 (3)0.050 (3)−0.003 (2)0.023 (3)−0.009 (2)
O40.040 (3)0.026 (3)0.049 (3)−0.004 (2)0.023 (2)−0.009 (2)
O50.063 (4)0.020 (3)0.048 (3)−0.010 (2)0.014 (3)0.005 (2)
O60.063 (4)0.028 (3)0.036 (3)−0.016 (3)0.011 (2)0.006 (2)
O70.036 (3)0.017 (2)0.033 (2)−0.004 (2)0.008 (2)0.0023 (19)
O80.030 (3)0.035 (3)0.028 (2)−0.004 (2)0.008 (2)−0.004 (2)
O90.028 (3)0.037 (3)0.029 (2)0.002 (2)0.013 (2)−0.001 (2)
O100.029 (3)0.025 (3)0.034 (3)0.004 (2)0.017 (2)0.003 (2)
O110.028 (3)0.034 (3)0.041 (3)0.002 (2)0.018 (2)0.009 (2)
O120.029 (3)0.041 (3)0.043 (3)0.003 (2)0.019 (2)0.016 (2)
O1W0.023 (3)0.088 (5)0.055 (4)0.007 (3)0.003 (3)−0.038 (3)
O2W0.043 (3)0.049 (3)0.045 (3)0.006 (3)0.025 (2)0.003 (3)
Tb10.02051 (17)0.01598 (16)0.02636 (16)−0.00013 (13)0.00914 (12)−0.00032 (12)
Tb20.02325 (18)0.01728 (16)0.03264 (18)−0.00032 (13)0.00735 (13)0.00021 (13)
Geometric parameters (Å, °) top
C1—O11.255 (7)C17—O101.256 (7)
C1—O21.269 (7)C17—O91.259 (7)
C1—C21.507 (9)C17—C181.515 (8)
C2—C71.377 (9)C18—C191.383 (9)
C2—C31.387 (9)C18—C231.388 (9)
C3—C41.378 (9)C19—C201.371 (10)
C3—H30.9300C19—H190.9300
C4—C51.385 (9)C20—C211.384 (10)
C4—C81.483 (9)C20—H200.9300
C5—C61.397 (10)C21—C221.385 (9)
C5—H50.9300C21—H210.9300
C6—C71.388 (10)C22—C231.386 (9)
C6—H60.9300C22—C241.500 (9)
C7—H70.9300C23—H230.9300
C8—O31.259 (7)C24—O121.251 (7)
C8—O41.269 (8)C24—O111.254 (7)
C9—O61.248 (8)O1—Tb12.465 (4)
C9—O51.265 (8)O1—Tb22.882 (4)
C9—C101.484 (9)O2—Tb22.420 (4)
C10—C11'1.390 (10)O3—Tb1i2.258 (4)
C10—C111.390 (11)O4—Tb2i2.338 (5)
C10—C151.413 (13)O5—Tb12.271 (4)
C10—C15'1.417 (11)O6—Tb2i2.258 (5)
C11—C121.382 (11)O7—Tb2ii2.352 (4)
C11—H110.9300O8—Tb1i2.370 (4)
C13—C141.384 (13)O9—Tb12.329 (4)
C13—C121.396 (12)O10—Tb22.369 (4)
C13—H130.9300O11—Tb2iii2.299 (5)
C14—C151.372 (14)O12—Tb1iv2.310 (4)
C14—H140.9300O1W—Tb12.354 (5)
C15—H150.9300O1W—H1W0.818 (10)
C11'—C121.381 (10)O1W—H2W0.819 (10)
C11'—H11'0.9300O2W—Tb22.513 (5)
C13'—C14'1.385 (12)O2W—H3W0.823 (10)
C13'—C121.395 (11)O2W—H4W0.822 (10)
C13'—H13'0.9300Tb1—O3v2.258 (4)
C14'—C15'1.373 (13)Tb1—O12vi2.310 (4)
C14'—H14'0.9300Tb1—O8v2.370 (4)
C15'—H15'0.9300Tb2—O6v2.258 (5)
C12—C161.499 (9)Tb2—O11iii2.299 (5)
C16—O71.253 (7)Tb2—O4v2.338 (5)
C16—O81.260 (7)Tb2—O7vii2.352 (4)
O1—C1—O2121.8 (6)C20—C21—C22120.4 (7)
O1—C1—C2119.9 (6)C20—C21—H21119.8
O2—C1—C2118.3 (6)C22—C21—H21119.8
C7—C2—C3120.4 (6)C21—C22—C23119.4 (6)
C7—C2—C1122.3 (6)C21—C22—C24121.6 (6)
C3—C2—C1117.3 (6)C23—C22—C24119.0 (6)
C4—C3—C2120.1 (6)C22—C23—C18120.4 (6)
C4—C3—H3119.9C22—C23—H23119.8
C2—C3—H3119.9C18—C23—H23119.8
C3—C4—C5120.0 (6)O12—C24—O11125.5 (6)
C3—C4—C8119.5 (6)O12—C24—C22117.1 (6)
C5—C4—C8120.4 (6)O11—C24—C22117.4 (6)
C4—C5—C6119.8 (6)C1—O1—Tb1146.1 (4)
C4—C5—H5120.1C1—O1—Tb284.1 (4)
C6—C5—H5120.1Tb1—O1—Tb2122.75 (16)
C7—C6—C5119.8 (7)C1—O2—Tb2105.8 (4)
C7—C6—H6120.1C8—O3—Tb1i141.7 (5)
C5—C6—H6120.1C8—O4—Tb2i141.2 (4)
C2—C7—C6119.8 (7)C9—O5—Tb1137.0 (5)
C2—C7—H7120.1C9—O6—Tb2i158.7 (5)
C6—C7—H7120.1C16—O7—Tb2ii113.7 (4)
O3—C8—O4123.9 (6)C16—O8—Tb1i156.2 (4)
O3—C8—C4117.2 (6)C17—O9—Tb1135.2 (4)
O4—C8—C4118.9 (6)C17—O10—Tb2134.5 (4)
O6—C9—O5123.6 (6)C24—O11—Tb2iii149.2 (4)
O6—C9—C10117.6 (6)C24—O12—Tb1iv149.6 (4)
O5—C9—C10118.8 (6)Tb1—O1W—H1W134 (5)
C11'—C10—C15114.3 (11)Tb1—O1W—H2W122 (5)
C11—C10—C15117.0 (11)H1W—O1W—H2W104.0 (17)
C11'—C10—C15'121.1 (8)Tb2—O2W—H3W148 (5)
C11—C10—C15'118.2 (8)Tb2—O2W—H4W108 (5)
C11'—C10—C9118.7 (7)H3W—O2W—H4W103.3 (17)
C11—C10—C9119.9 (7)O3v—Tb1—O5178.18 (19)
C15—C10—C9121.7 (10)O3v—Tb1—O12vi88.87 (17)
C15'—C10—C9120.1 (7)O5—Tb1—O12vi89.33 (18)
C12—C11—C10119.5 (9)O3v—Tb1—O991.95 (17)
C12—C11—H11120.3O5—Tb1—O989.20 (17)
C10—C11—H11120.3O12vi—Tb1—O9136.12 (16)
C14—C13—C12119.9 (15)O3v—Tb1—O1W85.3 (2)
C14—C13—H13120.1O5—Tb1—O1W93.9 (2)
C12—C13—H13120.1O12vi—Tb1—O1W70.16 (17)
C15—C14—C13117.2 (18)O9—Tb1—O1W66.20 (17)
C15—C14—H14121.4O3v—Tb1—O8v89.16 (16)
C13—C14—H14121.4O5—Tb1—O8v90.58 (16)
C14—C15—C10124.0 (17)O12vi—Tb1—O8v74.82 (16)
C14—C15—H15118.0O9—Tb1—O8v149.05 (16)
C10—C15—H15118.0O1W—Tb1—O8v144.62 (18)
C12—C11'—C10119.6 (8)O3v—Tb1—O182.62 (16)
C12—C11'—H11'120.2O5—Tb1—O199.09 (17)
C10—C11'—H11'120.2O12vi—Tb1—O1152.00 (15)
C14'—C13'—C12120.2 (11)O9—Tb1—O171.07 (15)
C14'—C13'—H13'119.9O1W—Tb1—O1135.00 (16)
C12—C13'—H13'119.9O8v—Tb1—O178.42 (15)
C15'—C14'—C13'121.4 (12)O6v—Tb2—O11iii78.07 (17)
C15'—C14'—H14'119.3O6v—Tb2—O4v77.30 (18)
C13'—C14'—H14'119.3O11iii—Tb2—O4v138.85 (15)
C14'—C15'—C10117.9 (11)O6v—Tb2—O7vii118.50 (16)
C14'—C15'—H15'121.1O11iii—Tb2—O7vii83.35 (16)
C10—C15'—H15'121.1O4v—Tb2—O7vii80.15 (16)
C11'—C12—C13'119.7 (8)O6v—Tb2—O10143.33 (16)
C11—C12—C13'116.9 (8)O11iii—Tb2—O10135.23 (15)
C11'—C12—C13119.2 (10)O4v—Tb2—O1080.73 (15)
C11—C12—C13121.8 (10)O7vii—Tb2—O1085.66 (15)
C11'—C12—C16119.1 (6)O6v—Tb2—O289.27 (17)
C11—C12—C16119.4 (7)O11iii—Tb2—O287.20 (15)
C13'—C12—C16120.9 (7)O4v—Tb2—O2124.72 (16)
C13—C12—C16118.3 (9)O7vii—Tb2—O2147.76 (15)
O7—C16—O8122.3 (6)O10—Tb2—O279.58 (15)
O7—C16—C12118.7 (5)O6v—Tb2—O2W145.73 (19)
O8—C16—C12118.9 (6)O11iii—Tb2—O2W71.18 (17)
O10—C17—O9125.3 (6)O4v—Tb2—O2W136.65 (17)
O10—C17—C18118.0 (6)O7vii—Tb2—O2W73.04 (17)
O9—C17—C18116.7 (6)O10—Tb2—O2W64.10 (16)
C19—C18—C23119.2 (6)O2—Tb2—O2W74.73 (17)
C19—C18—C17121.1 (6)O6v—Tb2—O178.07 (14)
C23—C18—C17119.6 (6)O11iii—Tb2—O1128.96 (14)
C20—C19—C18120.9 (7)O4v—Tb2—O176.53 (14)
C20—C19—H19119.6O7vii—Tb2—O1147.41 (14)
C18—C19—H19119.6O10—Tb2—O168.43 (13)
C19—C20—C21119.7 (7)O2—Tb2—O148.19 (14)
C19—C20—H20120.2O2W—Tb2—O1110.02 (16)
C21—C20—H20120.2
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (ii) x, y+1, z; (iii) −x+2, −y, −z; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) x−1/2, −y+1/2, z+1/2; (vii) x, y−1, z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O7viii0.818 (10)2.04 (4)2.789 (7)151 (7)
O1W—H2W···O4ix0.819 (10)2.29 (4)3.020 (7)149 (7)
O2W—H3W···O2iii0.823 (10)1.959 (14)2.780 (7)176 (9)
C3—H3···O8v0.932.353.257 (8)164
C11'—H11'···O1i0.932.393.284 (10)161
Symmetry codes: (viii) −x+1, −y+1, −z; (ix) x−1/2, −y+1/2, z−1/2; (iii) −x+2, −y, −z; (v) −x+3/2, y−1/2, −z+1/2; (i) −x+3/2, y+1/2, −z+1/2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O7i0.818 (10)2.04 (4)2.789 (7)151 (7)
O1W—H2W···O4ii0.819 (10)2.29 (4)3.020 (7)149 (7)
O2W—H3W···O2iii0.823 (10)1.959 (14)2.780 (7)176 (9)
C3—H3···O8iv0.932.353.257 (8)164
C11'—H11'···O1v0.932.393.284 (10)161
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+2, −y, −z; (iv) −x+3/2, y−1/2, −z+1/2; (v) −x+3/2, y+1/2, −z+1/2.
Acknowledgements top

The authors acknowledge South China Normal University for supporting this work.

references
References top

Bruker (2004). APEX2 (Version 6.12) and SMART (Version 6.12). Bruker AXS Inc, Madison, Wisconsin, USA.

De Bettencourt-Dias, A. (2005). Inorg. Chem. 44, 2734–2741.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Zhang, L.-P., Wan, Y.-H. & Jin, L.-P. (2003). Polyhedron, 22, 981–987.