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Acta Crystallogr Sect E Struct Rep Online. 2009 February 1; 65(Pt 2): m237.
Published online 2009 January 28. doi:  10.1107/S1600536809002864
PMCID: PMC2968397

Poly[diaqua-μ4-biphenyl-4,4′-dicarboxyl­ato-magnesium(II)]

Abstract

The solvothermal reaction of magnesium nitrate with bi­phenyl-4,4′-dicarboxylic acid in N,N-dimethyl­formamide and water leads to the formation of crystals of the title complex, [Mg(C14H8O4)(H2O)2]n. In the crystal structure, the Mg cations are coordinated by six O atoms from two water mol­ecules and four symmetry-related biphenyl-4,4′-dicarboxyl­ate anions within slightly distorted octa­hedra. The Mg cations are located on a center of inversion, the biphenyl-4,4′-dicarboxyl­ate anions around a twofold rotation axis and the water mol­ecule in a general position. The Mg cations are linked by the anions into a three-dimensional framework.

Related literature

For related structures, see: Kitagawa et al. (2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m237-scheme1.jpg

Experimental

Crystal data

  • [Mg(C14H8O4)(H2O)2]
  • M r = 150.27
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m237-efi5.jpg
  • a = 6.5913 (10) Å
  • b = 7.2900 (9) Å
  • c = 26.759 (4) Å
  • V = 1285.8 (3) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 0.16 mm−1
  • T = 295 (2) K
  • 0.15 × 0.10 × 0.05 mm

Data collection

  • Bruker APEXII CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2007 [triangle]) T min = 0.976, T max = 0.995
  • 5950 measured reflections
  • 1589 independent reflections
  • 1048 reflections with I > 2σ(I)
  • R int = 0.048

Refinement

  • R[F 2 > 2σ(F 2)] = 0.041
  • wR(F 2) = 0.106
  • S = 1.02
  • 1589 reflections
  • 97 parameters
  • H-atom parameters constrained
  • Δρmax = 0.30 e Å−3
  • Δρmin = −0.30 e Å−3

Data collection: APEX2 (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809002864/nc2132sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809002864/nc2132Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This research was supported by the National Science Council, Taiwan (grant No. NSC97-2113-M-033–003-MY2), and Chung-Yuan Christian University, Taiwan, under grant No. CYCU-97-CR-CH.

supplementary crystallographic information

Comment

The synthesis of coordination polymers, or so-called metal-organic frameworks (MOF), has been a subject of intense research owing to their interesting structural chemistry and potential applications in gas storage, separation, catalysis, magnetism, luminescence. A large number of these compounds have been synthesized by solvothermal reactions with organic carboxyl acids (Kitagawa et al., 2004). Here we report on the new metal organic framework bis(aqua)-biphenyl-4,4'-dicarboxylate magnesium (II). In the crystal structure the Mg cations are sorrounded by two O atoms from two symmetry related water molecules and four O atoms of four symmetry related anions (Fig. 1). The coordination polyhedron around the Mg cations can be described as a slightly distorted octahedron. The Mg cations are linked via the anions into a three-dimensional network (Fig. 2).

Experimental

The reaction was carried out under solvothermal conditions in a teflon-lined autoclav with an inner volume of 23 ml. A single-phase product consisting of transparent colorless crystals was obtained by heating a mixture of Mg(NO3)2˙6H2O, (0.1281 g, 0.5 mmol), biphenyl-4,4'-dicarboxylic acid (C14H10O4, 0.0290 g, 0.125 mmol), N,N-dimethylformamide (10.0 ml), and H2O (2.0 ml)at 423 K for 2 d followed by slow cooling at 6 K/h to room temperature.

Refinement

The C—H H atoms were positioned with idealized geometry and were refined isotropic using a riding model with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C). The H atoms at the water molecule were found in difference map and were refined with varying coordinates isotropic.

Figures

Fig. 1.
Crystal structure of the title compound with labeling and displacement ellipsoids drawn at the 50% probability level. [symmetry codes: (i) -x + 2,-y + 1,-z; (ii) -x + 3/2,y - 1/2,z; (iii) x + 1/2,-y + 3/2,-z; (iv) -x + 2,y,-z + 1/2.].
Fig. 2.
Crystal structure of the title compound with view along the a axis.

Crystal data

[Mg(C14H8O4)(H2O)2]Dx = 1.553 Mg m3
Mr = 150.27Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcnCell parameters from 1007 reflections
a = 6.5913 (10) Åθ = 3.1–25.2°
b = 7.2900 (9) ŵ = 0.16 mm1
c = 26.759 (4) ÅT = 295 K
V = 1285.8 (3) Å3Lamellar, colorless
Z = 80.15 × 0.10 × 0.05 mm
F(000) = 624

Data collection

Bruker APEXII CCD diffractometer1589 independent reflections
Radiation source: fine-focus sealed tube1048 reflections with I > 2σ(I)
graphiteRint = 0.048
[var phi] and ω scansθmax = 28.4°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −7→8
Tmin = 0.976, Tmax = 0.995k = −9→9
5950 measured reflectionsl = −22→35

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.106H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0448P)2 + 0.3401P] where P = (Fo2 + 2Fc2)/3
1589 reflections(Δ/σ)max < 0.001
97 parametersΔρmax = 0.30 e Å3
0 restraintsΔρmin = −0.30 e Å3

Special details

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)

xyzUiso*/Ueq
Mg11.00000.50000.00000.0159 (2)
C10.7888 (3)0.7850 (2)0.06884 (7)0.0162 (4)
C20.8503 (3)0.7715 (3)0.12262 (7)0.0184 (4)
C30.7124 (3)0.8132 (3)0.16000 (7)0.0245 (5)
H30.57960.84400.15170.029*
C40.7715 (4)0.8092 (3)0.20963 (7)0.0259 (5)
H40.67750.83800.23430.031*
C50.9691 (3)0.7629 (3)0.22334 (7)0.0211 (5)
C61.1051 (3)0.7183 (3)0.18550 (7)0.0261 (5)
H61.23720.68540.19380.031*
C71.0476 (3)0.7220 (3)0.13581 (8)0.0242 (5)
H71.14090.69150.11110.029*
O10.9201 (2)0.74253 (17)0.03552 (5)0.0194 (3)
O1W0.7228 (2)0.48848 (18)−0.03619 (5)0.0221 (3)
H1WA0.63060.5799−0.04120.080*
H1WB0.63350.4082−0.02930.080*
O20.6164 (2)0.8454 (2)0.05857 (5)0.0233 (4)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mg10.0166 (5)0.0205 (4)0.0107 (4)0.0010 (4)0.0010 (4)−0.0006 (4)
C10.0195 (11)0.0161 (9)0.0129 (9)0.0000 (8)0.0000 (8)0.0002 (7)
C20.0214 (12)0.0218 (10)0.0121 (9)0.0017 (8)−0.0020 (8)0.0004 (8)
C30.0214 (12)0.0352 (12)0.0171 (10)0.0075 (10)−0.0001 (9)0.0004 (9)
C40.0271 (13)0.0388 (11)0.0116 (9)0.0057 (10)0.0022 (9)−0.0003 (9)
C50.0240 (12)0.0272 (10)0.0120 (10)0.0006 (9)−0.0017 (9)−0.0002 (8)
C60.0202 (12)0.0416 (12)0.0166 (10)0.0029 (10)−0.0037 (9)0.0012 (9)
C70.0216 (12)0.0369 (12)0.0141 (10)0.0042 (10)0.0010 (8)−0.0005 (9)
O10.0221 (8)0.0232 (7)0.0129 (7)0.0025 (6)0.0012 (6)−0.0015 (6)
O1W0.0165 (8)0.0279 (7)0.0221 (7)0.0001 (6)−0.0011 (6)0.0012 (6)
O20.0200 (8)0.0346 (8)0.0152 (7)0.0065 (7)−0.0015 (7)0.0041 (6)

Geometric parameters (Å, °)

Mg1—O1Wi2.0696 (14)C3—H30.9300
Mg1—O1W2.0696 (14)C4—C51.395 (3)
Mg1—O12.0753 (12)C4—H40.9300
Mg1—O1i2.0753 (12)C5—C61.391 (3)
Mg1—O2ii2.0774 (13)C5—C5iv1.484 (4)
Mg1—O2iii2.0774 (13)C6—C71.383 (3)
C1—O21.249 (2)C6—H60.9300
C1—O11.281 (2)C7—H70.9300
C1—C21.498 (3)O1W—H1WA0.9119
C2—C31.385 (3)O1W—H1WB0.8502
C2—C71.395 (3)O2—Mg1v2.0774 (13)
C3—C41.384 (3)
O1Wi—Mg1—O1W180.00 (10)C4—C3—C2120.2 (2)
O1Wi—Mg1—O188.58 (5)C4—C3—H3119.9
O1W—Mg1—O191.42 (5)C2—C3—H3119.9
O1Wi—Mg1—O1i91.42 (5)C3—C4—C5121.3 (2)
O1W—Mg1—O1i88.58 (5)C3—C4—H4119.3
O1—Mg1—O1i180.00 (6)C5—C4—H4119.3
O1Wi—Mg1—O2ii89.72 (5)C6—C5—C4117.84 (18)
O1W—Mg1—O2ii90.28 (5)C6—C5—C5iv121.5 (2)
O1—Mg1—O2ii91.31 (5)C4—C5—C5iv120.6 (2)
O1i—Mg1—O2ii88.69 (5)C7—C6—C5121.3 (2)
O1Wi—Mg1—O2iii90.28 (5)C7—C6—H6119.4
O1W—Mg1—O2iii89.72 (5)C5—C6—H6119.4
O1—Mg1—O2iii88.69 (5)C6—C7—C2120.2 (2)
O1i—Mg1—O2iii91.31 (5)C6—C7—H7119.9
O2ii—Mg1—O2iii180.00 (8)C2—C7—H7119.9
O2—C1—O1123.14 (17)C1—O1—Mg1134.15 (12)
O2—C1—C2118.73 (17)Mg1—O1W—H1WA128.9
O1—C1—C2118.03 (17)Mg1—O1W—H1WB122.5
C3—C2—C7119.06 (18)H1WA—O1W—H1WB94.2
C3—C2—C1120.10 (18)C1—O2—Mg1v133.89 (13)
C7—C2—C1120.82 (18)

Symmetry codes: (i) −x+2, −y+1, −z; (ii) −x+3/2, y−1/2, z; (iii) x+1/2, −y+3/2, −z; (iv) −x+2, y, −z+1/2; (v) x−1/2, −y+3/2, −z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NC2132).

References

  • Bruker (2007). SADABS, SAINT and APEX2 Bruker AXS Inc., Madison, Wisconsin, USA.
  • Kitagawa, S., Kitaura, R. & Noro, S. (2004). Angew. Chem. Int. Ed.43, 2334–2375. [PubMed]
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography