metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 1| January 2010| Pages m54-m55

Bis(μ-4-hy­droxy­benzoato-κ2O:O′)bis­­[tri­aqua­bis­(4-hy­droxy­benzoato)-κO;κ2O,O′-terbium(III)] deca­hydrate

aMOE Key Laboratory of Bioinorganic and Synthetic Chemistry, School of Chemistry & Chemical Engineering, Sun Yat-Sen University, Guangzhou 510275, People's Republic of China, and bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 6 December 2009; accepted 7 December 2009; online 12 December 2009)

The title dinuclear compound, [Tb2(C7H5O3)6(H2O)6]·10H2O, lies on a center of inversion and the two TbIII atoms are bridged by two 4-hydroxy­benzoate anions; each metal atom is further coordinated by one monodentate anion and chelated by the third anion. The eight-coordinate geometry approximates a square anti­prism. Hydrogen bonds of the O—H⋯O type connect the uncoordinated water mol­ecules to the dinuclear species, forming a three-dimensional network.

Related literature

For a related structure, Tb2(H2O)2(DMF)2(C7H5O3)6, see: Zhou et al. (2008[Zhou, Y.-X., Shen, X.-Q., Zhang, H.-Y., Du, C.-X. & Hou, H.-W. (2008). J. Coord. Chem. 61, 3981-3992.]).

[Scheme 1]

Experimental

Crystal data
  • [Tb2(C7H5O3)6(H2O)6]·10H2O

  • Mr = 1428.76

  • Triclinic, [P \overline 1]

  • a = 10.8308 (5) Å

  • b = 11.3337 (6) Å

  • c = 11.5128 (6) Å

  • α = 90.463 (1)°

  • β = 101.690 (1)°

  • γ = 105.249 (1)°

  • V = 1332.37 (12) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 2.73 mm−1

  • T = 173 K

  • 0.47 × 0.30 × 0.19 mm

Data collection
  • Bruker SMART area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.360, Tmax = 0.625

  • 12836 measured reflections

  • 5756 independent reflections

  • 5391 reflections with I > 2σ(I)

  • Rint = 0.018

Refinement
  • R[F2 > 2σ(F2)] = 0.018

  • wR(F2) = 0.059

  • S = 1.09

  • 5756 reflections

  • 409 parameters

  • 27 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.67 e Å−3

  • Δρmin = −0.64 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H3⋯O7wi 0.84 (1) 1.82 (2) 2.612 (3) 158 (3)
O6—H6⋯O6wii 0.83 (1) 1.87 (1) 2.678 (3) 165 (4)
O9—H9⋯O4wiii 0.84 (1) 1.98 (2) 2.763 (3) 156 (3)
O1w—H11⋯O4w 0.84 (1) 2.04 (1) 2.870 (3) 171 (3)
O1w—H12⋯O9iv 0.83 (1) 1.96 (1) 2.766 (3) 164 (3)
O2w—H22⋯O5w 0.83 (1) 1.86 (1) 2.678 (3) 167 (3)
O2w—H21⋯O5wv 0.84 (1) 2.20 (2) 2.952 (3) 150 (3)
O3w—H31⋯O3ii 0.84 (1) 1.95 (1) 2.777 (3) 171 (3)
O3w—H32⋯O7vi 0.84 (1) 2.25 (2) 2.916 (2) 137 (3)
O4w—H41⋯O8wvii 0.84 (1) 1.94 (1) 2.753 (3) 163 (3)
O4w—H42⋯O5viii 0.84 (1) 2.10 (1) 2.927 (3) 169 (3)
O5w—H52⋯O7w 0.85 (1) 2.01 (2) 2.811 (3) 157 (3)
O5w—H51⋯O8wix 0.86 (1) 1.96 (1) 2.791 (3) 163 (3)
O6w—H61⋯O2 0.85 (1) 1.90 (1) 2.743 (2) 172 (3)
O6w—H62⋯O5 0.84 (1) 1.95 (1) 2.785 (2) 171 (3)
O7w—H71⋯O6w 0.84 (1) 1.90 (1) 2.732 (3) 172 (3)
O7w—H72⋯O5x 0.83 (1) 1.89 (1) 2.725 (3) 175 (3)
O8w—H81⋯O1xi 0.84 (1) 2.10 (2) 2.818 (3) 144 (3)
O8w—H82⋯O6 0.84 (1) 1.90 (1) 2.713 (3) 164 (3)
Symmetry codes: (i) -x+2, -y+1, -z; (ii) x-1, y, z; (iii) x+1, y+1, z; (iv) -x+2, -y+1, -z+1; (v) -x+1, -y+1, -z; (vi) -x+1, -y+1, -z+1; (vii) -x, -y, -z+1; (viii) -x+1, -y, -z+1; (ix) -x, -y, -z; (x) -x+1, -y, -z; (xi) x-1, y-1, z.

Data collection: SMART (Bruker, 2001[Bruker (2001). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2009[Westrip, S. P. (2009). publCIF. In preparation.]).

Supporting information


Related literature top

For a related structure, Tb2(H2O)2(DMF)2(C7H5O3)6, see: Zhou et al. (2008).

Experimental top

4-Hydroxybenzoic acid (0.3 mmol) and sodium hydroxide (0.3 mmol) were dissolved in water (5 ml) and this was mixed with a solution of terbium chloride (0.1 mmol) dissolved in water (5 ml). The white precipitate that formed was removed by filtration. Colorless crystals were isolated from the filtrated after two weeks.

Refinement top

Carbon-bound hydrogen atoms were generated geometrically and were constrained to ride on their parent atoms [C–H = 0.95, Uiso(H) = 1.2Ueq(C)]. The hydroxy and water H-atoms were located in a difference Fourier map, and were refined with distance restraints of O–H 0.84±0.01 Å and H···H 1.37±0.01 Å. Their temperature factors were tied by a factor of 1.5.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of Tb2(H2O)6(C7H5O3)6.10H2O at the 70% probability level; hydrogen atoms are drawn as sphere of arbitrary radius.
[Figure 2] Fig. 2. Detail of the coordination environment of the terbium(III) atom.
Bis(µ-4-hydroxybenzoato-κ2O:O')bis[triaquabis(4- hydroxybenzoato)-κO;κ2O,O'-terbium(III)] decahydrate top
Crystal data top
[Tb2(C7H5O3)6(H2O)6]·10H2OZ = 1
Mr = 1428.76F(000) = 716
Triclinic, P1Dx = 1.781 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.8308 (5) ÅCell parameters from 5392 reflections
b = 11.3337 (6) Åθ = 2.3–27.0°
c = 11.5128 (6) ŵ = 2.73 mm1
α = 90.463 (1)°T = 173 K
β = 101.690 (1)°Block, colorless
γ = 105.249 (1)°0.47 × 0.30 × 0.19 mm
V = 1332.37 (12) Å3
Data collection top
Bruker SMART area-detector
diffractometer
5756 independent reflections
Radiation source: fine-focus sealed tube5391 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
ϕ and ω scansθmax = 27.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.360, Tmax = 0.625k = 1314
12836 measured reflectionsl = 1414
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)] = 0.018Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0407P)2 + 0.0925P]
where P = (Fo2 + 2Fc2)/3
5756 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.67 e Å3
27 restraintsΔρmin = 0.64 e Å3
Crystal data top
[Tb2(C7H5O3)6(H2O)6]·10H2Oγ = 105.249 (1)°
Mr = 1428.76V = 1332.37 (12) Å3
Triclinic, P1Z = 1
a = 10.8308 (5) ÅMo Kα radiation
b = 11.3337 (6) ŵ = 2.73 mm1
c = 11.5128 (6) ÅT = 173 K
α = 90.463 (1)°0.47 × 0.30 × 0.19 mm
β = 101.690 (1)°
Data collection top
Bruker SMART area-detector
diffractometer
5756 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5391 reflections with I > 2σ(I)
Tmin = 0.360, Tmax = 0.625Rint = 0.018
12836 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01827 restraints
wR(F2) = 0.059H atoms treated by a mixture of independent and constrained refinement
S = 1.09Δρmax = 0.67 e Å3
5756 reflectionsΔρmin = 0.64 e Å3
409 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Tb10.521099 (9)0.392335 (9)0.316629 (8)0.01393 (5)
O10.68247 (16)0.52500 (16)0.22113 (15)0.0219 (4)
O20.71938 (16)0.35118 (15)0.28025 (15)0.0189 (3)
O31.25530 (17)0.60503 (18)0.13235 (17)0.0243 (4)
H31.262 (3)0.6687 (19)0.095 (3)0.036*
O40.44616 (17)0.20553 (16)0.21445 (16)0.0233 (4)
O50.44536 (17)0.00991 (16)0.21119 (16)0.0236 (4)
O60.15974 (18)0.03603 (17)0.16884 (18)0.0280 (4)
H60.192 (3)0.023 (2)0.171 (3)0.042*
O70.66267 (16)0.51402 (16)0.47709 (14)0.0207 (3)
O80.65933 (16)0.66801 (16)0.59555 (15)0.0209 (4)
O91.23480 (17)0.85877 (17)0.50180 (16)0.0220 (4)
H91.262 (3)0.9320 (13)0.529 (3)0.033*
O1w0.56576 (17)0.25542 (17)0.47360 (16)0.0241 (4)
H110.509 (2)0.206 (2)0.502 (3)0.036*
H120.6353 (16)0.234 (3)0.487 (3)0.036*
O2w0.40382 (18)0.41807 (17)0.12181 (15)0.0233 (4)
H210.405 (3)0.4895 (13)0.102 (2)0.035*
H220.426 (3)0.380 (2)0.071 (2)0.035*
O3w0.44922 (17)0.57723 (16)0.32029 (15)0.0201 (3)
H310.397 (2)0.593 (3)0.2625 (14)0.030*
H320.428 (3)0.593 (3)0.3838 (13)0.030*
O4w0.39635 (19)0.08545 (18)0.59456 (16)0.0267 (4)
H410.358 (3)0.130 (3)0.624 (2)0.040*
H420.450 (3)0.066 (3)0.6490 (19)0.040*
O5w0.4872 (2)0.3305 (2)0.05591 (17)0.0309 (4)
H510.421 (2)0.294 (3)0.111 (2)0.046*
H520.530 (3)0.278 (2)0.037 (3)0.046*
O6w0.69870 (17)0.12258 (17)0.18465 (16)0.0235 (4)
H610.711 (3)0.1957 (12)0.211 (3)0.035*
H620.6246 (17)0.082 (2)0.194 (3)0.035*
O7w0.6606 (2)0.18314 (17)0.04660 (16)0.0286 (4)
H710.676 (3)0.160 (3)0.0230 (11)0.043*
H720.627 (3)0.1215 (18)0.0936 (19)0.043*
O8w0.30680 (19)0.22701 (18)0.26414 (18)0.0301 (4)
H810.280 (3)0.2897 (17)0.276 (3)0.045*
H820.249 (2)0.172 (2)0.242 (3)0.045*
C10.7539 (2)0.4523 (2)0.2315 (2)0.0169 (5)
C20.8802 (2)0.4855 (2)0.19285 (19)0.0163 (4)
C30.9139 (2)0.5908 (2)0.1316 (2)0.0190 (5)
H3A0.85130.63520.10570.023*
C41.0383 (2)0.6307 (2)0.1084 (2)0.0186 (5)
H41.06090.70200.06600.022*
C51.1296 (2)0.5662 (2)0.1474 (2)0.0177 (5)
C61.0956 (2)0.4574 (2)0.2042 (2)0.0188 (5)
H6A1.15720.41120.22680.023*
C70.9713 (2)0.4181 (2)0.22698 (19)0.0178 (5)
H70.94750.34460.26610.021*
C80.3871 (2)0.0935 (2)0.2068 (2)0.0184 (5)
C90.2416 (2)0.0589 (2)0.1919 (2)0.0168 (4)
C100.1763 (2)0.0536 (2)0.2258 (2)0.0206 (5)
H100.22370.11090.25420.025*
C110.0414 (2)0.0831 (2)0.2184 (2)0.0224 (5)
H11A0.00270.15920.24400.027*
C120.0276 (2)0.0015 (2)0.1740 (2)0.0201 (5)
C130.0352 (2)0.1103 (2)0.1364 (2)0.0214 (5)
H130.01350.16510.10340.026*
C140.1704 (2)0.1410 (2)0.1477 (2)0.0207 (5)
H140.21460.21850.12510.025*
C150.7152 (2)0.6180 (2)0.53115 (19)0.0159 (4)
C160.8513 (2)0.6851 (2)0.52099 (19)0.0153 (4)
C170.9058 (2)0.8072 (2)0.56448 (19)0.0167 (4)
H170.85500.84940.59820.020*
C181.0337 (2)0.8673 (2)0.5587 (2)0.0187 (5)
H181.07040.95030.58830.022*
C191.1080 (2)0.8052 (2)0.5093 (2)0.0177 (5)
C201.0543 (2)0.6841 (2)0.4635 (2)0.0187 (5)
H201.10450.64270.42820.022*
C210.9260 (2)0.6245 (2)0.4702 (2)0.0176 (5)
H21A0.88900.54180.43980.021*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb10.01190 (7)0.01180 (7)0.01807 (7)0.00220 (4)0.00446 (4)0.00005 (4)
O10.0188 (8)0.0190 (9)0.0318 (9)0.0082 (7)0.0104 (7)0.0067 (7)
O20.0174 (8)0.0138 (8)0.0276 (8)0.0042 (6)0.0098 (6)0.0035 (6)
O30.0152 (8)0.0248 (10)0.0348 (10)0.0051 (7)0.0099 (7)0.0120 (8)
O40.0198 (8)0.0152 (9)0.0338 (9)0.0032 (7)0.0051 (7)0.0029 (7)
O50.0186 (8)0.0183 (9)0.0343 (9)0.0062 (7)0.0049 (7)0.0008 (7)
O60.0173 (9)0.0201 (10)0.0484 (11)0.0055 (7)0.0105 (8)0.0042 (8)
O70.0160 (8)0.0188 (9)0.0244 (8)0.0005 (7)0.0032 (6)0.0025 (7)
O80.0174 (8)0.0170 (9)0.0302 (9)0.0039 (7)0.0105 (7)0.0001 (7)
O90.0134 (8)0.0204 (9)0.0321 (9)0.0023 (7)0.0079 (7)0.0027 (7)
O1w0.0184 (8)0.0241 (10)0.0337 (9)0.0082 (7)0.0108 (7)0.0114 (7)
O2w0.0316 (10)0.0196 (9)0.0203 (8)0.0097 (8)0.0058 (7)0.0005 (7)
O3w0.0237 (9)0.0198 (9)0.0195 (8)0.0093 (7)0.0065 (7)0.0013 (7)
O4w0.0262 (10)0.0251 (10)0.0301 (9)0.0082 (8)0.0067 (7)0.0042 (8)
O5w0.0298 (10)0.0359 (12)0.0292 (10)0.0122 (9)0.0072 (8)0.0007 (8)
O6w0.0200 (9)0.0194 (9)0.0330 (10)0.0057 (7)0.0092 (7)0.0001 (7)
O7w0.0404 (11)0.0183 (9)0.0272 (9)0.0055 (8)0.0109 (8)0.0021 (7)
O8w0.0293 (10)0.0204 (10)0.0427 (11)0.0062 (8)0.0128 (8)0.0068 (8)
C10.0153 (11)0.0168 (11)0.0172 (10)0.0023 (9)0.0030 (8)0.0022 (9)
C20.0156 (10)0.0159 (11)0.0170 (10)0.0029 (9)0.0047 (8)0.0000 (8)
C30.0185 (11)0.0181 (12)0.0224 (11)0.0074 (9)0.0057 (9)0.0039 (9)
C40.0207 (11)0.0155 (11)0.0206 (11)0.0047 (9)0.0066 (9)0.0040 (9)
C50.0162 (11)0.0183 (12)0.0185 (11)0.0028 (9)0.0057 (8)0.0004 (9)
C60.0180 (11)0.0180 (12)0.0222 (11)0.0066 (9)0.0055 (9)0.0046 (9)
C70.0190 (11)0.0155 (11)0.0182 (10)0.0028 (9)0.0046 (8)0.0029 (9)
C80.0181 (11)0.0172 (12)0.0189 (10)0.0026 (9)0.0044 (8)0.0012 (9)
C90.0185 (11)0.0136 (11)0.0185 (10)0.0046 (9)0.0039 (8)0.0004 (8)
C100.0203 (11)0.0158 (12)0.0276 (12)0.0078 (9)0.0054 (9)0.0029 (9)
C110.0222 (12)0.0147 (12)0.0318 (13)0.0040 (10)0.0102 (10)0.0027 (10)
C120.0186 (11)0.0184 (12)0.0230 (11)0.0036 (9)0.0055 (9)0.0021 (9)
C130.0215 (12)0.0185 (12)0.0247 (12)0.0082 (10)0.0023 (9)0.0034 (9)
C140.0216 (12)0.0156 (12)0.0245 (11)0.0032 (10)0.0064 (9)0.0022 (9)
C150.0141 (10)0.0166 (11)0.0176 (10)0.0052 (9)0.0031 (8)0.0036 (8)
C160.0147 (10)0.0166 (11)0.0142 (10)0.0043 (9)0.0021 (8)0.0016 (8)
C170.0163 (11)0.0163 (11)0.0189 (10)0.0055 (9)0.0051 (8)0.0024 (9)
C180.0188 (11)0.0148 (11)0.0221 (11)0.0030 (9)0.0053 (9)0.0008 (9)
C190.0121 (10)0.0209 (12)0.0200 (11)0.0036 (9)0.0040 (8)0.0051 (9)
C200.0175 (11)0.0190 (12)0.0217 (11)0.0070 (9)0.0064 (9)0.0001 (9)
C210.0163 (11)0.0161 (11)0.0189 (10)0.0026 (9)0.0028 (8)0.0008 (9)
Geometric parameters (Å, º) top
Tb1—O42.2791 (17)O8w—H810.836 (10)
Tb1—O72.3162 (16)O8w—H820.840 (10)
Tb1—O8i2.3276 (16)C1—C21.480 (3)
Tb1—O2w2.4042 (17)C2—C31.394 (3)
Tb1—O3w2.4227 (18)C2—C71.398 (3)
Tb1—O22.4276 (16)C3—C41.385 (3)
Tb1—O12.4388 (17)C3—H3A0.9500
Tb1—O1w2.4482 (17)C4—C51.386 (3)
O1—C11.262 (3)C4—H40.9500
O2—C11.280 (3)C5—C61.398 (3)
O3—C51.364 (3)C6—C71.383 (3)
O3—H30.837 (10)C6—H6A0.9500
O4—C81.256 (3)C7—H70.9500
O5—C81.265 (3)C8—C91.494 (3)
O6—C121.370 (3)C9—C101.387 (3)
O6—H60.833 (10)C9—C141.395 (4)
O7—C151.262 (3)C10—C111.395 (3)
O8—C151.262 (3)C10—H100.9500
O8—Tb1i2.3276 (16)C11—C121.375 (4)
O9—C191.368 (3)C11—H11A0.9500
O9—H90.841 (10)C12—C131.389 (4)
O1w—H110.839 (10)C13—C141.392 (3)
O1w—H120.834 (10)C13—H130.9500
O2w—H210.838 (10)C14—H140.9500
O2w—H220.832 (10)C15—C161.499 (3)
O3w—H310.835 (10)C16—C211.395 (3)
O3w—H320.840 (10)C16—C171.397 (3)
O4w—H410.837 (10)C17—C181.389 (3)
O4w—H420.840 (10)C17—H170.9500
O5w—H510.861 (10)C18—C191.394 (3)
O5w—H520.852 (10)C18—H180.9500
O6w—H610.846 (10)C19—C201.394 (3)
O6w—H620.841 (10)C20—C211.394 (3)
O7w—H710.842 (10)C20—H200.9500
O7w—H720.833 (10)C21—H21A0.9500
O4—Tb1—O7147.98 (6)C4—C3—H3A119.9
O4—Tb1—O8i86.52 (6)C2—C3—H3A119.9
O7—Tb1—O8i97.15 (6)C3—C4—C5119.7 (2)
O4—Tb1—O2w71.93 (6)C3—C4—H4120.2
O7—Tb1—O2w138.23 (6)C5—C4—H4120.2
O8i—Tb1—O2w97.25 (6)O3—C5—C4122.0 (2)
O4—Tb1—O3w136.40 (6)O3—C5—C6117.2 (2)
O7—Tb1—O3w74.94 (6)C4—C5—C6120.8 (2)
O8i—Tb1—O3w77.43 (6)C7—C6—C5119.1 (2)
O2w—Tb1—O3w70.33 (6)C7—C6—H6A120.4
O4—Tb1—O276.79 (6)C5—C6—H6A120.4
O7—Tb1—O283.64 (6)C6—C7—C2120.5 (2)
O8i—Tb1—O2147.37 (6)C6—C7—H7119.8
O2w—Tb1—O2103.72 (6)C2—C7—H7119.8
O3w—Tb1—O2133.16 (6)O4—C8—O5122.9 (2)
O4—Tb1—O1108.71 (6)O4—C8—C9117.9 (2)
O7—Tb1—O178.16 (6)O5—C8—C9119.2 (2)
O8i—Tb1—O1158.46 (6)C10—C9—C14119.2 (2)
O2w—Tb1—O174.23 (6)C10—C9—C8120.3 (2)
O3w—Tb1—O181.06 (6)C14—C9—C8120.4 (2)
O2—Tb1—O153.69 (6)C9—C10—C11120.4 (2)
O4—Tb1—O1w78.28 (6)C9—C10—H10119.8
O7—Tb1—O1w73.07 (6)C11—C10—H10119.8
O8i—Tb1—O1w70.82 (6)C12—C11—C10119.7 (2)
O2w—Tb1—O1w148.59 (6)C12—C11—H11A120.2
O3w—Tb1—O1w130.93 (6)C10—C11—H11A120.2
O2—Tb1—O1w78.37 (6)O6—C12—C11116.8 (2)
O1—Tb1—O1w126.13 (6)O6—C12—C13122.2 (2)
C1—O1—Tb193.28 (14)C11—C12—C13121.0 (2)
C1—O2—Tb193.32 (14)C14—C13—C12119.1 (2)
C5—O3—H3107 (2)C14—C13—H13120.5
C8—O4—Tb1150.98 (16)C12—C13—H13120.5
C12—O6—H6114 (2)C13—C14—C9120.6 (2)
C15—O7—Tb1150.17 (16)C13—C14—H14119.7
C15—O8—Tb1i136.88 (15)C9—C14—H14119.7
C19—O9—H9113 (2)O8—C15—O7123.1 (2)
Tb1—O1w—H11125.7 (19)O8—C15—C16117.9 (2)
Tb1—O1w—H12121.8 (19)O7—C15—C16119.0 (2)
H11—O1w—H12109.2 (16)C21—C16—C17119.4 (2)
Tb1—O2w—H21118 (2)C21—C16—C15119.8 (2)
Tb1—O2w—H22110 (2)C17—C16—C15120.8 (2)
H21—O2w—H22110.7 (16)C18—C17—C16120.3 (2)
Tb1—O3w—H31121 (2)C18—C17—H17119.8
Tb1—O3w—H32114.7 (19)C16—C17—H17119.8
H31—O3w—H32109.5 (16)C17—C18—C19119.7 (2)
H41—O4w—H42108.8 (16)C17—C18—H18120.1
H51—O5w—H52105.4 (15)C19—C18—H18120.1
H61—O6w—H62108.3 (16)O9—C19—C18122.6 (2)
H71—O7w—H72108.9 (16)O9—C19—C20116.8 (2)
H81—O8w—H82109.5 (16)C18—C19—C20120.6 (2)
O1—C1—O2119.7 (2)C21—C20—C19119.2 (2)
O1—C1—C2120.5 (2)C21—C20—H20120.4
O2—C1—C2119.7 (2)C19—C20—H20120.4
C3—C2—C7119.6 (2)C20—C21—C16120.7 (2)
C3—C2—C1120.0 (2)C20—C21—H21A119.7
C7—C2—C1120.2 (2)C16—C21—H21A119.7
C4—C3—C2120.2 (2)
O4—Tb1—O1—C156.96 (14)C3—C4—C5—C63.5 (3)
O7—Tb1—O1—C190.56 (14)O3—C5—C6—C7176.6 (2)
O8i—Tb1—O1—C1169.90 (15)C4—C5—C6—C73.4 (3)
O2w—Tb1—O1—C1121.11 (14)C5—C6—C7—C20.5 (3)
O3w—Tb1—O1—C1166.92 (14)C3—C2—C7—C62.3 (3)
O2—Tb1—O1—C10.22 (12)C1—C2—C7—C6171.8 (2)
O1w—Tb1—O1—C131.99 (16)Tb1—O4—C8—O5108.1 (3)
O4—Tb1—O2—C1125.77 (14)Tb1—O4—C8—C972.0 (4)
O7—Tb1—O2—C179.74 (13)O4—C8—C9—C10156.2 (2)
O8i—Tb1—O2—C1173.07 (12)O5—C8—C9—C1023.8 (3)
O2w—Tb1—O2—C158.44 (14)O4—C8—C9—C1421.5 (3)
O3w—Tb1—O2—C117.32 (16)O5—C8—C9—C14158.5 (2)
O1—Tb1—O2—C10.22 (12)C14—C9—C10—C111.5 (4)
O1w—Tb1—O2—C1153.71 (14)C8—C9—C10—C11176.2 (2)
O7—Tb1—O4—C866.9 (4)C9—C10—C11—C121.9 (4)
O8i—Tb1—O4—C831.0 (3)C10—C11—C12—O6179.8 (2)
O2w—Tb1—O4—C8129.8 (3)C10—C11—C12—C130.1 (4)
O3w—Tb1—O4—C898.7 (3)O6—C12—C13—C14178.0 (2)
O2—Tb1—O4—C8120.8 (3)C11—C12—C13—C142.1 (4)
O1—Tb1—O4—C8164.6 (3)C12—C13—C14—C92.4 (4)
O1w—Tb1—O4—C840.1 (3)C10—C9—C14—C130.7 (4)
O4—Tb1—O7—C15169.6 (3)C8—C9—C14—C13178.4 (2)
O8i—Tb1—O7—C1595.6 (3)Tb1i—O8—C15—O714.8 (4)
O2w—Tb1—O7—C1513.8 (3)Tb1i—O8—C15—C16163.99 (16)
O3w—Tb1—O7—C1520.7 (3)Tb1—O7—C15—O881.1 (4)
O2—Tb1—O7—C15117.3 (3)Tb1—O7—C15—C16100.2 (3)
O1—Tb1—O7—C1563.1 (3)O8—C15—C16—C21167.8 (2)
O1w—Tb1—O7—C15163.0 (3)O7—C15—C16—C2111.1 (3)
Tb1—O1—C1—O20.4 (2)O8—C15—C16—C1710.6 (3)
Tb1—O1—C1—C2176.78 (18)O7—C15—C16—C17170.5 (2)
Tb1—O2—C1—O10.4 (2)C21—C16—C17—C180.9 (3)
Tb1—O2—C1—C2176.80 (18)C15—C16—C17—C18177.6 (2)
O1—C1—C2—C37.7 (3)C16—C17—C18—C190.0 (3)
O2—C1—C2—C3175.1 (2)C17—C18—C19—O9179.5 (2)
O1—C1—C2—C7166.3 (2)C17—C18—C19—C201.2 (4)
O2—C1—C2—C710.8 (3)O9—C19—C20—C21179.2 (2)
C7—C2—C3—C42.3 (3)C18—C19—C20—C211.5 (4)
C1—C2—C3—C4171.8 (2)C19—C20—C21—C160.5 (3)
C2—C3—C4—C50.6 (4)C17—C16—C21—C200.6 (3)
C3—C4—C5—O3176.5 (2)C15—C16—C21—C20177.8 (2)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O7wii0.84 (1)1.82 (2)2.612 (3)158 (3)
O6—H6···O6wiii0.83 (1)1.87 (1)2.678 (3)165 (4)
O9—H9···O4wiv0.84 (1)1.98 (2)2.763 (3)156 (3)
O1w—H11···O4w0.84 (1)2.04 (1)2.870 (3)171 (3)
O1w—H12···O9v0.83 (1)1.96 (1)2.766 (3)164 (3)
O2w—H22···O5w0.83 (1)1.86 (1)2.678 (3)167 (3)
O2w—H21···O5wvi0.84 (1)2.20 (2)2.952 (3)150 (3)
O3w—H31···O3iii0.84 (1)1.95 (1)2.777 (3)171 (3)
O3w—H32···O7i0.84 (1)2.25 (2)2.916 (2)137 (3)
O4w—H41···O8wvii0.84 (1)1.94 (1)2.753 (3)163 (3)
O4w—H42···O5viii0.84 (1)2.10 (1)2.927 (3)169 (3)
O5w—H52···O7w0.85 (1)2.01 (2)2.811 (3)157 (3)
O5w—H51···O8wix0.86 (1)1.96 (1)2.791 (3)163 (3)
O6w—H61···O20.85 (1)1.90 (1)2.743 (2)172 (3)
O6w—H62···O50.84 (1)1.95 (1)2.785 (2)171 (3)
O7w—H71···O6w0.84 (1)1.90 (1)2.732 (3)172 (3)
O7w—H72···O5x0.83 (1)1.89 (1)2.725 (3)175 (3)
O8w—H81···O1xi0.84 (1)2.10 (2)2.818 (3)144 (3)
O8w—H82···O60.84 (1)1.90 (1)2.713 (3)164 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z; (iii) x1, y, z; (iv) x+1, y+1, z; (v) x+2, y+1, z+1; (vi) x+1, y+1, z; (vii) x, y, z+1; (viii) x+1, y, z+1; (ix) x, y, z; (x) x+1, y, z; (xi) x1, y1, z.

Experimental details

Crystal data
Chemical formula[Tb2(C7H5O3)6(H2O)6]·10H2O
Mr1428.76
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)10.8308 (5), 11.3337 (6), 11.5128 (6)
α, β, γ (°)90.463 (1), 101.690 (1), 105.249 (1)
V3)1332.37 (12)
Z1
Radiation typeMo Kα
µ (mm1)2.73
Crystal size (mm)0.47 × 0.30 × 0.19
Data collection
DiffractometerBruker SMART area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.360, 0.625
No. of measured, independent and
observed [I > 2σ(I)] reflections
12836, 5756, 5391
Rint0.018
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.018, 0.059, 1.09
No. of reflections5756
No. of parameters409
No. of restraints27
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.67, 0.64

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O7wi0.84 (1)1.82 (2)2.612 (3)158 (3)
O6—H6···O6wii0.83 (1)1.87 (1)2.678 (3)165 (4)
O9—H9···O4wiii0.84 (1)1.98 (2)2.763 (3)156 (3)
O1w—H11···O4w0.84 (1)2.04 (1)2.870 (3)171 (3)
O1w—H12···O9iv0.83 (1)1.96 (1)2.766 (3)164 (3)
O2w—H22···O5w0.83 (1)1.86 (1)2.678 (3)167 (3)
O2w—H21···O5wv0.84 (1)2.20 (2)2.952 (3)150 (3)
O3w—H31···O3ii0.84 (1)1.95 (1)2.777 (3)171 (3)
O3w—H32···O7vi0.84 (1)2.25 (2)2.916 (2)137 (3)
O4w—H41···O8wvii0.84 (1)1.94 (1)2.753 (3)163 (3)
O4w—H42···O5viii0.84 (1)2.10 (1)2.927 (3)169 (3)
O5w—H52···O7w0.85 (1)2.01 (2)2.811 (3)157 (3)
O5w—H51···O8wix0.86 (1)1.96 (1)2.791 (3)163 (3)
O6w—H61···O20.85 (1)1.90 (1)2.743 (2)172 (3)
O6w—H62···O50.84 (1)1.95 (1)2.785 (2)171 (3)
O7w—H71···O6w0.84 (1)1.90 (1)2.732 (3)172 (3)
O7w—H72···O5x0.83 (1)1.89 (1)2.725 (3)175 (3)
O8w—H81···O1xi0.84 (1)2.10 (2)2.818 (3)144 (3)
O8w—H82···O60.84 (1)1.90 (1)2.713 (3)164 (3)
Symmetry codes: (i) x+2, y+1, z; (ii) x1, y, z; (iii) x+1, y+1, z; (iv) x+2, y+1, z+1; (v) x+1, y+1, z; (vi) x+1, y+1, z+1; (vii) x, y, z+1; (viii) x+1, y, z+1; (ix) x, y, z; (x) x+1, y, z; (xi) x1, y1, z.
 

Acknowledgements

This work was supported by Sun Yat-Sen University and the University of Malaya.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
First citationBruker (2001). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWestrip, S. P. (2009). publCIF. In preparation.  Google Scholar
First citationZhou, Y.-X., Shen, X.-Q., Zhang, H.-Y., Du, C.-X. & Hou, H.-W. (2008). J. Coord. Chem. 61, 3981–3992.  Web of Science CSD CrossRef CAS Google Scholar

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Volume 66| Part 1| January 2010| Pages m54-m55
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