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

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ISSN: 2056-9890

Poly[di-μ4-benzene-1,4-di­carboxyl­ato-μ6-succinato-diholmium(III)]

aDepartment of Chemistry, Xuchang University, Xuchang 461000, People's Republic of China
*Correspondence e-mail: qhe.xcu@163.com

(Received 25 October 2007; accepted 14 December 2007; online 21 December 2007)

The title compound, [Ho2(C4H4O4)(C8H4O4)2]n, was synthesized hydro­thermally. The Ho atom is coordinated by four O atoms from four benzene-1,4-dicarboxyl­ate (BDC) anions and four O atoms from three succinate anions, in a distorted square-anti­prismatic coordination geometry. The anti­prisms are bridged by the benzene-1,4-dicarboxyl­ate and succinate anions, into a three-dimensional coordination network. The succinate anions are located on centres of inversion.

Related literature

For related literature, see: Li & Wang (2005[Li, Z.-F. & Wang, C.-X. (2005). Acta Cryst. E61, m2689-m2690.]); Li et al. (2006[Li, Z.-F., Wang, C.-X., Li, Y., Cai, D.-J. & Xiao, Y.-J. (2006). Acta Cryst. E62, m251-m252.]); Wang & Li (2005[Wang, C.-X. & Li, Z.-F. (2005). Acta Cryst. E61, m2212-m2213.]); He et al. (2006[He, Q., Zi, J.-F. & Zhang, F.-J. (2006). Acta Cryst. E62, m997-m998.]).

[Scheme 1]

Experimental

Crystal data
  • [Ho2(C4H4O4)(C8H4O4)2]

  • Mr = 387.08

  • Orthorhombic, P b c a

  • a = 13.8147 (3) Å

  • b = 6.7850 (2) Å

  • c = 21.7103 (5) Å

  • V = 2034.97 (9) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 7.79 mm−1

  • T = 291 (2) K

  • 0.18 × 0.15 × 0.05 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.245, Tmax = 0.682

  • 11598 measured reflections

  • 2411 independent reflections

  • 2140 reflections with I > 2σ(I)

  • Rint = 0.019

Refinement
  • R[F2 > 2σ(F2)] = 0.015

  • wR(F2) = 0.042

  • S = 1.06

  • 2411 reflections

  • 155 parameters

  • H-atom parameters constrained

  • Δρmax = 0.94 e Å−3

  • Δρmin = −0.60 e Å−3

Table 1
Selected bond lengths (Å)

Ho—O1 2.2899 (17)
Ho—O2i 2.2320 (17)
Ho—O3ii 2.3208 (16)
Ho—O4iii 2.3013 (16)
Ho—O5 2.4753 (16)
Ho—O5iv 2.4015 (18)
Ho—O6v 2.4633 (17)
Ho—O6 2.5230 (16)
Symmetry codes: (i) -x+2, -y+2, -z+1; (ii) [x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]; (iii) [-x+{\script{3\over 2}}, -y+2, z+{\script{1\over 2}}]; (iv) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z]; (v) [-x+{\script{3\over 2}}, y-{\script{1\over 2}}, z].

Data collection: SMART (Bruker, 1998[Bruker (1998). SMART (Version 5.16), SAINT (Version 6.01) and SHELXTL (Version 6.14). Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SMART; data reduction: SAINT (Bruker, 1998[Bruker (1998). SMART (Version 5.16), SAINT (Version 6.01) and SHELXTL (Version 6.14). Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); molecular graphics: SHELXTL (Bruker, 1998[Bruker (1998). SMART (Version 5.16), SAINT (Version 6.01) and SHELXTL (Version 6.14). Bruker AXS Inc., Madison, Wisconsin, USA.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The title compound, (I), is isostructural with its [M2(C8H4O4)2(C4H4O4)]n [M = Gd (Wang & Li, 2005), Dy ((Li & Wang, 2005), Nd (Li et al., 2006) and Er (He et al., 2006)] analogues. The Ho3+ ion is located at the center of a distorted square antiprism and is coordinated by four oxygen atoms from four benzene-1,4-dicarboxylate anions and four oxygen atoms from three succinate anions (Fig. 1). The Ho—O bond distances ranging from 2.2851 (2) to 2.5764 (16) Å.

The succinate anions are located on centres of inversion and acts as a bis-chelating ligands for each two symmetry related Ho atoms. Each of the four oxygen atom are additionally connected by Ho atoms into layers which are parallel to the (001) plane. These layers are connected via the benzene-1,4-dicarboxylate anions into a three-dimensional coordination network.

Related literature top

For related literature, see: Li & Wang (2005); Li et al. (2006); Wang & Li (2005); He et al. (2006).

Experimental top

A mixture of HoCl3.6H2O (2.00 mmol, 0.74 g), benzene-1,4-dicarboxylic acid (1.0 mmol, 0.16 g), succinic acid (1.0 mmol, 0.10 g), NaOH (6.0 ml, 1 mol/L) and H2O (20.0 ml) was heated in a 35 ml stainless steel reactor with a Teflon liner at 453 K for 48 h. The column-like crystals were filtered and washed with ethanol. Yield: 30% based on Ho.

Refinement top

H atoms were included at calculated positions and treated as riding atoms, with C—H distances of 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C)].

Structure description top

The title compound, (I), is isostructural with its [M2(C8H4O4)2(C4H4O4)]n [M = Gd (Wang & Li, 2005), Dy ((Li & Wang, 2005), Nd (Li et al., 2006) and Er (He et al., 2006)] analogues. The Ho3+ ion is located at the center of a distorted square antiprism and is coordinated by four oxygen atoms from four benzene-1,4-dicarboxylate anions and four oxygen atoms from three succinate anions (Fig. 1). The Ho—O bond distances ranging from 2.2851 (2) to 2.5764 (16) Å.

The succinate anions are located on centres of inversion and acts as a bis-chelating ligands for each two symmetry related Ho atoms. Each of the four oxygen atom are additionally connected by Ho atoms into layers which are parallel to the (001) plane. These layers are connected via the benzene-1,4-dicarboxylate anions into a three-dimensional coordination network.

For related literature, see: Li & Wang (2005); Li et al. (2006); Wang & Li (2005); He et al. (2006).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).

Figures top
[Figure 1] Fig. 1. The coordination environment of the Ho atom, with the atom-numbering scheme, showing displacement ellipsoids drawn at the 50% probability level. Symmetry codes: (i) 2 - x, 2 - y, 1 - z; (ii) x, 3/2 - y, z + 1/2; (iii) 3/2 - x, 2 - y, z + 1/2; (iv) 3/2 - x, y + 1/2, z; (v) 3/2 - x, y - 1/2, z; (vi) 1 - x, 2 - y, 1 - z.
Poly[di-µ4-benzene-1,4-dicarboxylato-µ6-succinato-diholmium(III)] top
Crystal data top
[Ho2(C4H4O4)(C8H4O4)2]F(000) = 1448
Mr = 387.08Dx = 2.527 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 254 reflections
a = 13.8147 (3) Åθ = 2.1–27.1°
b = 6.7850 (2) ŵ = 7.79 mm1
c = 21.7103 (5) ÅT = 291 K
V = 2034.97 (9) Å3Column, orange
Z = 80.18 × 0.15 × 0.05 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2411 independent reflections
Radiation source: fine-focus sealed tube2140 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 28.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1716
Tmin = 0.245, Tmax = 0.682k = 78
11598 measured reflectionsl = 2825
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)] = 0.015H-atom parameters constrained
wR(F2) = 0.042 w = 1/[σ2(Fo2) + (0.0238P)2 + 0.923P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.002
2411 reflectionsΔρmax = 0.94 e Å3
155 parametersΔρmin = 0.60 e Å3
0 restraintsExtinction correction: SHELXTL (Bruker, 1998), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00060 (5)
Crystal data top
[Ho2(C4H4O4)(C8H4O4)2]V = 2034.97 (9) Å3
Mr = 387.08Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 13.8147 (3) ŵ = 7.79 mm1
b = 6.7850 (2) ÅT = 291 K
c = 21.7103 (5) Å0.18 × 0.15 × 0.05 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2411 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2140 reflections with I > 2σ(I)
Tmin = 0.245, Tmax = 0.682Rint = 0.019
11598 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0150 restraints
wR(F2) = 0.042H-atom parameters constrained
S = 1.06Δρmax = 0.94 e Å3
2411 reflectionsΔρmin = 0.60 e Å3
155 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*/Ueq
Ho0.830676 (8)1.016049 (15)0.554834 (5)0.01275 (6)
O10.86282 (15)1.0368 (2)0.45156 (8)0.0198 (4)
O21.01131 (12)0.9282 (3)0.43269 (7)0.0206 (3)
C10.92600 (17)0.9674 (3)0.41630 (11)0.0148 (4)
C20.89870 (17)0.9259 (3)0.35070 (10)0.0177 (5)
C30.96527 (18)0.8440 (4)0.31009 (11)0.0257 (5)
H3A1.02740.81430.32370.031*
C40.93977 (19)0.8064 (4)0.24966 (11)0.0276 (6)
H4A0.98460.75100.22280.033*
C50.84715 (17)0.8514 (3)0.22885 (11)0.0208 (5)
C60.81879 (18)0.8035 (3)0.16377 (11)0.0213 (5)
C70.78017 (19)0.9332 (4)0.26926 (11)0.0259 (5)
H7A0.71810.96340.25550.031*
C80.8056 (2)0.9698 (4)0.32984 (13)0.0244 (5)
H8A0.76051.02400.35680.029*
O30.87624 (13)0.6998 (3)0.13253 (8)0.0284 (4)
O40.73920 (13)0.8685 (3)0.14403 (7)0.0265 (4)
O50.66712 (11)0.8691 (3)0.54719 (8)0.0229 (4)
O60.67647 (11)1.1742 (2)0.51694 (8)0.0205 (4)
C90.6257 (2)1.0274 (3)0.53160 (14)0.0240 (6)
C100.5157 (2)1.0403 (4)0.53093 (15)0.0313 (6)
H10A0.48830.96270.56410.038*
H10B0.49481.17600.53560.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ho0.01198 (8)0.01651 (7)0.00977 (8)0.00044 (3)0.00010 (4)0.00131 (3)
O10.0203 (10)0.0274 (9)0.0118 (9)0.0012 (7)0.0002 (7)0.0009 (6)
O20.0158 (9)0.0311 (8)0.0149 (8)0.0020 (7)0.0033 (7)0.0017 (7)
C10.0166 (12)0.0170 (10)0.0108 (11)0.0019 (8)0.0003 (9)0.0010 (8)
C20.0190 (12)0.0229 (11)0.0112 (11)0.0006 (9)0.0022 (9)0.0021 (8)
C30.0203 (13)0.0393 (14)0.0175 (13)0.0050 (10)0.0054 (10)0.0067 (10)
C40.0250 (14)0.0385 (14)0.0193 (13)0.0056 (11)0.0008 (10)0.0087 (11)
C50.0278 (13)0.0224 (11)0.0123 (12)0.0005 (9)0.0051 (10)0.0036 (9)
C60.0302 (14)0.0206 (11)0.0131 (12)0.0036 (9)0.0049 (10)0.0017 (9)
C70.0228 (13)0.0364 (13)0.0186 (13)0.0066 (11)0.0097 (11)0.0037 (11)
C80.0210 (13)0.0356 (13)0.0167 (13)0.0063 (10)0.0022 (11)0.0065 (10)
O30.0338 (10)0.0312 (9)0.0203 (10)0.0021 (8)0.0054 (8)0.0088 (7)
O40.0264 (10)0.0378 (10)0.0154 (8)0.0011 (8)0.0072 (7)0.0012 (7)
O50.0173 (9)0.0174 (8)0.0341 (11)0.0002 (6)0.0071 (7)0.0010 (7)
O60.0189 (9)0.0188 (8)0.0238 (10)0.0010 (6)0.0022 (7)0.0019 (7)
C90.0197 (14)0.0212 (12)0.0310 (16)0.0020 (9)0.0089 (12)0.0025 (10)
C100.0376 (18)0.0236 (12)0.0326 (17)0.0037 (11)0.0005 (14)0.0019 (11)
Geometric parameters (Å, º) top
Ho—O12.2899 (17)C4—C51.391 (3)
Ho—O2i2.2320 (17)C4—H4A0.9300
Ho—O3ii2.3208 (16)C5—C71.391 (3)
Ho—O4iii2.3013 (16)C5—C61.502 (3)
Ho—O52.4753 (16)C6—O31.259 (3)
Ho—O5iv2.4015 (18)C6—O41.260 (3)
Ho—O6v2.4633 (17)C7—C81.384 (4)
Ho—O62.5230 (16)C7—H7A0.9300
O1—C11.253 (3)C8—H8A0.9300
O2—C11.259 (3)O5—C91.263 (3)
C1—C21.500 (3)O6—C91.259 (3)
C2—C31.390 (3)C9—C101.523 (4)
C2—C81.395 (4)C10—C10vi1.514 (6)
C3—C41.382 (3)C10—H10A0.9700
C3—H3A0.9300C10—H10B0.9700
O2i—Ho—O185.34 (7)C3—C2—C8119.3 (2)
O2i—Ho—O4iii104.50 (6)C3—C2—C1120.7 (2)
O1—Ho—O4iii152.17 (6)C8—C2—C1120.0 (2)
O2i—Ho—O3ii75.73 (6)C4—C3—C2120.5 (2)
O1—Ho—O3ii134.25 (7)C4—C3—H3A119.8
O4iii—Ho—O3ii73.56 (7)C2—C3—H3A119.8
O2i—Ho—O5iv80.03 (6)C3—C4—C5120.2 (2)
O1—Ho—O5iv82.44 (6)C3—C4—H4A119.9
O4iii—Ho—O5iv73.97 (6)C5—C4—H4A119.9
O3ii—Ho—O5iv132.55 (6)C7—C5—C4119.7 (2)
O2i—Ho—O6v103.85 (6)C7—C5—C6120.4 (2)
O1—Ho—O6v74.86 (6)C4—C5—C6119.9 (2)
O4iii—Ho—O6v125.79 (6)O3—C6—O4124.2 (2)
O3ii—Ho—O6v70.08 (6)O3—C6—C5117.6 (2)
O5iv—Ho—O6v156.47 (6)O4—C6—C5118.2 (2)
O2i—Ho—O5165.74 (6)C8—C7—C5120.1 (2)
O1—Ho—O597.82 (7)C8—C7—H7A119.9
O4iii—Ho—O579.09 (6)C5—C7—H7A119.9
O3ii—Ho—O592.42 (6)C7—C8—C2120.3 (2)
O5iv—Ho—O5114.12 (5)C7—C8—H8A119.9
O6v—Ho—O564.00 (6)C2—C8—H8A119.9
O2i—Ho—O6142.50 (6)C6—O3—Hovii124.97 (15)
O1—Ho—O679.54 (6)C6—O4—Hoviii140.49 (16)
O4iii—Ho—O677.02 (6)C9—O5—Hov150.76 (16)
O3ii—Ho—O6137.25 (6)C9—O5—Ho95.09 (15)
O5iv—Ho—O664.15 (5)Hov—O5—Ho112.68 (6)
O6v—Ho—O6104.93 (5)C9—O6—Hoiv129.67 (17)
O5—Ho—O651.58 (6)C9—O6—Ho92.94 (15)
O2i—Ho—C9168.32 (6)Hoiv—O6—Ho108.99 (6)
O1—Ho—C991.01 (8)O6—C9—O5119.2 (2)
O4iii—Ho—C974.08 (8)O6—C9—C10120.5 (2)
O3ii—Ho—C9114.28 (7)O5—C9—C10120.2 (2)
O5iv—Ho—C988.50 (6)O6—C9—Ho61.15 (13)
O6v—Ho—C985.82 (6)O5—C9—Ho58.99 (13)
O5—Ho—C925.92 (6)C10—C9—Ho170.3 (2)
O6—Ho—C925.91 (6)C10vi—C10—C9105.9 (3)
C1—O1—Ho135.25 (16)C10vi—C10—H10A110.6
C1—O2—Hoi156.02 (15)C9—C10—H10A110.6
O1—C1—O2124.0 (2)C10vi—C10—H10B110.6
O1—C1—C2118.4 (2)C9—C10—H10B110.6
O2—C1—C2117.6 (2)H10A—C10—H10B108.7
Symmetry codes: (i) x+2, y+2, z+1; (ii) x, y+3/2, z+1/2; (iii) x+3/2, y+2, z+1/2; (iv) x+3/2, y+1/2, z; (v) x+3/2, y1/2, z; (vi) x+1, y+2, z+1; (vii) x, y+3/2, z1/2; (viii) x+3/2, y+2, z1/2.

Experimental details

Crystal data
Chemical formula[Ho2(C4H4O4)(C8H4O4)2]
Mr387.08
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)291
a, b, c (Å)13.8147 (3), 6.7850 (2), 21.7103 (5)
V3)2034.97 (9)
Z8
Radiation typeMo Kα
µ (mm1)7.79
Crystal size (mm)0.18 × 0.15 × 0.05
Data collection
DiffractometerBruker SMART CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.245, 0.682
No. of measured, independent and
observed [I > 2σ(I)] reflections
11598, 2411, 2140
Rint0.019
(sin θ/λ)max1)0.660
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.015, 0.042, 1.06
No. of reflections2411
No. of parameters155
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.94, 0.60

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998).

Selected bond lengths (Å) top
Ho—O12.2899 (17)Ho—O52.4753 (16)
Ho—O2i2.2320 (17)Ho—O5iv2.4015 (18)
Ho—O3ii2.3208 (16)Ho—O6v2.4633 (17)
Ho—O4iii2.3013 (16)Ho—O62.5230 (16)
Symmetry codes: (i) x+2, y+2, z+1; (ii) x, y+3/2, z+1/2; (iii) x+3/2, y+2, z+1/2; (iv) x+3/2, y+1/2, z; (v) x+3/2, y1/2, z.
 

References

First citationBruker (1998). SMART (Version 5.16), SAINT (Version 6.01) and SHELXTL (Version 6.14). Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationHe, Q., Zi, J.-F. & Zhang, F.-J. (2006). Acta Cryst. E62, m997–m998.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationLi, Z.-F. & Wang, C.-X. (2005). Acta Cryst. E61, m2689–m2690.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationLi, Z.-F., Wang, C.-X., Li, Y., Cai, D.-J. & Xiao, Y.-J. (2006). Acta Cryst. E62, m251–m252.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.  Google Scholar
First citationWang, C.-X. & Li, Z.-F. (2005). Acta Cryst. E61, m2212–m2213.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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