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

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Poly[(μ5-5-amino­isophthalato)aqua­barium]

aDepartment of Chemistry, Chung-Yuan Christian University, Chung-Li 320, Taiwan
*Correspondence e-mail: chiaher@cycu.edu.tw

(Received 2 September 2011; accepted 16 September 2011; online 30 September 2011)

In the title compound, [Ba(C8H5NO4)(H2O)]n, the BaII ion is eight-coordinated by six O atoms and one N atom from five 5-amino­isophthalate ligands and one water mol­ecule in a distorted dodeca­hedral geometry. The BaII ions are connected via the ligands into a layer parallel to (011). The layers are linked by N—H⋯O hydrogen bonds. The coordinated water mol­ecule is involved in intra­layer O—H⋯O hydrogen bonds.

Related literature

For general background to metal coordination polymers, see: Kitagawa et al. (2004[Kitagawa, S., Kitaura, R. & Noro, S. (2004). Angew. Chem. Int. Ed. 43, 2334-2375.]). For related structures, see: Kongshaug & Fjellvåg (2006[Kongshaug, K. O. & Fjellvåg, H. (2006). Inorg. Chem. 45, 2424-2429.]); Wu & Lin (2010[Wu, C.-Y. & Lin, C.-H. (2010). Acta Cryst. E66, m1437.]); Zeng et al. (2007[Zeng, R.-H., Fang, Z.-Q., Sun, F., Jiang, L.-S. & Tang, Y.-W. (2007). Acta Cryst. E63, m1813-m1814.]).

[Scheme 1]

Experimental

Crystal data
  • [Ba(C8H5NO4)(H2O)]

  • Mr = 334.48

  • Triclinic, [P \overline 1]

  • a = 7.7621 (1) Å

  • b = 7.9652 (1) Å

  • c = 8.3416 (1) Å

  • α = 79.618 (1)°

  • β = 65.574 (1)°

  • γ = 83.575 (1)°

  • V = 461.48 (1) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 4.30 mm−1

  • T = 295 K

  • 0.50 × 0.30 × 0.30 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.232, Tmax = 0.275

  • 7950 measured reflections

  • 2283 independent reflections

  • 2230 reflections with I > 2σ(I)

  • Rint = 0.019

Refinement
  • R[F2 > 2σ(F2)] = 0.015

  • wR(F2) = 0.040

  • S = 1.12

  • 2283 reflections

  • 136 parameters

  • H-atom parameters constrained

  • Δρmax = 0.48 e Å−3

  • Δρmin = −0.79 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1W—H1WA⋯O3i 0.89 1.90 2.770 (2) 165
O1W—H1WB⋯O2ii 0.83 1.95 2.770 (2) 167
N1—H1A⋯O2iii 0.96 2.16 3.067 (2) 157
N1—H1B⋯O4iv 0.99 2.19 3.176 (2) 175
Symmetry codes: (i) -x, -y+1, -z+1; (ii) -x, -y+1, -z; (iii) -x+1, -y, -z; (iv) -x+1, -y-1, -z+1.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. 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: DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Comment top

The increasingly rapid development of metal coordination polymers over the past two decades has attracted considerable attention due to their structural diversity and important applications (Kitagawa et al., 2004). 5-Aminoisophthalic acid has been successively reported as sodium (Zeng et al., 2007), zinc (Kongshaug & Fjellvåg, 2006) and magnesium complexes (Wu & Lin, 2010). In our continuous investigations in metal coordination polymers, we report here the structure of a new Ba(II) coordination polymer based on the 5-aminoisophthalate ligand.

In the title compound (Fig. 1), the BaII ion is eight-coordinated by six O atoms and one N atom from five 5-aminoisophthalate ligands and one water molecule in a distorted dodecahedral geometry. The Ba—O distances range from 2.6808 (16) to 2.8813 (17) Å. The Ba—N distance is 2.918 (2) Å. The BaO7N dodecahedra are connected via the anionic ligands into a layer parallel to ( 0 1 1). The coordinated water molecule is involved in intralayer O—H···O hydrogen bonds (Table 1 , Fig. 2). These layers are linked by interlayer N—H···O hydrogen bonds (Fig. 3).

Related literature top

For general background to metal coordination polymers, see: Kitagawa et al. (2004). For related structures, see: Kongshaug & Fjellvåg (2006); Wu & Lin (2010); Zeng et al. (2007).

Experimental top

Solvothermal reactions were carried out at 423 K for 2 d in a Teflon-lined acid digestion bomb with an internal volume of 23 ml followed by slow cooling at 6 K h-1 to room temperature. A single-phase product consisting of transparent crystals was obtained from a mixture of 5-aminoisophthalic acid (C8H7NO4, 0.145 g, 0.8 mmol), Ba(NO3)2.4H2O (0.105 g, 0.2 mmol), methanol (5.0 ml) and H2O (1.0 ml).

Refinement top

H atoms bound to C atoms were positioned geometrically, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C). H atoms bound to N and O atoms were located in a difference Fourier map and fixed in refinements, with Uiso(H) = 1.5Ueq(O) or 1.2Ueq(N).

Structure description top

The increasingly rapid development of metal coordination polymers over the past two decades has attracted considerable attention due to their structural diversity and important applications (Kitagawa et al., 2004). 5-Aminoisophthalic acid has been successively reported as sodium (Zeng et al., 2007), zinc (Kongshaug & Fjellvåg, 2006) and magnesium complexes (Wu & Lin, 2010). In our continuous investigations in metal coordination polymers, we report here the structure of a new Ba(II) coordination polymer based on the 5-aminoisophthalate ligand.

In the title compound (Fig. 1), the BaII ion is eight-coordinated by six O atoms and one N atom from five 5-aminoisophthalate ligands and one water molecule in a distorted dodecahedral geometry. The Ba—O distances range from 2.6808 (16) to 2.8813 (17) Å. The Ba—N distance is 2.918 (2) Å. The BaO7N dodecahedra are connected via the anionic ligands into a layer parallel to ( 0 1 1). The coordinated water molecule is involved in intralayer O—H···O hydrogen bonds (Table 1 , Fig. 2). These layers are linked by interlayer N—H···O hydrogen bonds (Fig. 3).

For general background to metal coordination polymers, see: Kitagawa et al. (2004). For related structures, see: Kongshaug & Fjellvåg (2006); Wu & Lin (2010); Zeng et al. (2007).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) -x, 1-y, 1-z; (ii) x, 1+y, z; (iii) -x, -y, 1-z; (iv) x, 1+y, -1+z.]
[Figure 2] Fig. 2. The layer structure of the title compound viewed along the a axis. Intralayer O—H···O hydrogen bonds are shown as pink dashed lines.
[Figure 3] Fig. 3. The crystal packing of the title compound viewed along the a axis. Interlayer N—H···O hydrogen bonds are shown as pink dashed lines.
Poly[(µ5-5-aminoisophthalato)aquabarium] top
Crystal data top
[Ba(C8H5NO4)(H2O)]Z = 2
Mr = 334.48F(000) = 316
Triclinic, P1Dx = 2.407 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.7621 (1) ÅCell parameters from 120 reflections
b = 7.9652 (1) Åθ = 2.6–31.8°
c = 8.3416 (1) ŵ = 4.30 mm1
α = 79.618 (1)°T = 295 K
β = 65.574 (1)°Block, colourless
γ = 83.575 (1)°0.50 × 0.30 × 0.30 mm
V = 461.48 (1) Å3
Data collection top
Bruker APEXII CCD
diffractometer
2283 independent reflections
Radiation source: fine-focus sealed tube2230 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 8.3333 pixels mm-1θmax = 28.3°, θmin = 2.6°
φ and ω scansh = 1010
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
k = 1010
Tmin = 0.232, Tmax = 0.275l = 1110
7950 measured reflections
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)] = 0.015Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.040H-atom parameters constrained
S = 1.12 w = 1/[σ2(Fo2) + (0.0203P)2 + 0.2964P]
where P = (Fo2 + 2Fc2)/3
2283 reflections(Δ/σ)max = 0.001
136 parametersΔρmax = 0.48 e Å3
0 restraintsΔρmin = 0.79 e Å3
Crystal data top
[Ba(C8H5NO4)(H2O)]γ = 83.575 (1)°
Mr = 334.48V = 461.48 (1) Å3
Triclinic, P1Z = 2
a = 7.7621 (1) ÅMo Kα radiation
b = 7.9652 (1) ŵ = 4.30 mm1
c = 8.3416 (1) ÅT = 295 K
α = 79.618 (1)°0.50 × 0.30 × 0.30 mm
β = 65.574 (1)°
Data collection top
Bruker APEXII CCD
diffractometer
2283 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
2230 reflections with I > 2σ(I)
Tmin = 0.232, Tmax = 0.275Rint = 0.019
7950 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0150 restraints
wR(F2) = 0.040H-atom parameters constrained
S = 1.12Δρmax = 0.48 e Å3
2283 reflectionsΔρmin = 0.79 e Å3
136 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.047838 (16)0.597922 (13)0.212249 (13)0.01817 (5)
O10.1383 (2)0.32074 (19)0.4588 (2)0.0281 (3)
O1W0.1803 (3)0.8279 (2)0.0982 (2)0.0345 (4)
H1WA0.19190.94110.07940.052*
H1WB0.20530.78470.02670.052*
O20.2226 (3)0.27828 (19)0.18144 (19)0.0286 (3)
O30.2563 (3)0.1752 (2)0.8942 (2)0.0293 (3)
O40.2032 (2)0.42403 (18)0.84296 (19)0.0243 (3)
N10.4296 (3)0.3479 (2)0.1704 (2)0.0222 (3)
H1A0.52460.29310.06220.027*
H1B0.54050.42080.17470.027*
C10.2029 (3)0.2256 (2)0.3391 (3)0.0198 (4)
C20.2556 (3)0.0420 (2)0.3867 (3)0.0184 (4)
C30.2367 (3)0.0217 (2)0.5594 (3)0.0204 (4)
H30.19830.05120.64460.025*
C40.2751 (3)0.1940 (2)0.6051 (3)0.0180 (4)
C50.3385 (3)0.3012 (2)0.4757 (3)0.0191 (4)
H50.36100.41710.50710.023*
C60.3688 (3)0.2373 (2)0.2996 (3)0.0179 (4)
C70.3232 (3)0.0654 (3)0.2571 (3)0.0193 (4)
H70.33820.02210.14110.023*
C80.2440 (3)0.2676 (3)0.7936 (3)0.0191 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.02706 (8)0.01489 (7)0.01284 (7)0.00289 (5)0.00903 (5)0.00259 (4)
O10.0457 (9)0.0188 (7)0.0174 (7)0.0088 (6)0.0116 (7)0.0057 (6)
O1W0.0527 (11)0.0238 (8)0.0411 (10)0.0094 (7)0.0335 (9)0.0103 (7)
O20.0509 (10)0.0182 (7)0.0160 (7)0.0084 (7)0.0156 (7)0.0020 (5)
O30.0511 (10)0.0211 (7)0.0205 (7)0.0045 (7)0.0190 (7)0.0013 (6)
O40.0381 (8)0.0156 (7)0.0187 (7)0.0021 (6)0.0125 (6)0.0016 (5)
N10.0284 (9)0.0191 (8)0.0181 (8)0.0046 (7)0.0081 (7)0.0065 (6)
C10.0266 (10)0.0154 (9)0.0153 (9)0.0024 (7)0.0072 (8)0.0021 (7)
C20.0232 (9)0.0162 (9)0.0150 (9)0.0025 (7)0.0078 (7)0.0018 (7)
C30.0298 (10)0.0159 (9)0.0145 (8)0.0018 (7)0.0085 (8)0.0022 (7)
C40.0211 (9)0.0177 (9)0.0153 (8)0.0002 (7)0.0085 (7)0.0007 (7)
C50.0237 (9)0.0145 (8)0.0181 (9)0.0023 (7)0.0090 (8)0.0005 (7)
C60.0193 (9)0.0178 (9)0.0165 (9)0.0019 (7)0.0070 (7)0.0047 (7)
C70.0250 (9)0.0173 (9)0.0143 (8)0.0022 (7)0.0078 (7)0.0012 (7)
C80.0244 (9)0.0176 (9)0.0149 (9)0.0018 (7)0.0091 (7)0.0001 (7)
Geometric parameters (Å, º) top
Ba1—O1i2.6815 (15)N1—C61.410 (2)
Ba1—O1W2.7266 (16)N1—H1A0.9638
Ba1—O4ii2.7392 (16)N1—H1B0.9930
Ba1—O22.7502 (15)C1—C21.502 (3)
Ba1—O4iii2.8371 (15)C2—C31.390 (3)
Ba1—O3iii2.8807 (16)C2—C71.393 (3)
Ba1—N1iv2.9094 (19)C3—C41.390 (3)
Ba1—O12.9675 (15)C3—H30.9300
O1—C11.263 (2)C4—C51.391 (3)
O1W—H1WA0.8880C4—C81.504 (3)
O1W—H1WB0.8346C5—C61.394 (3)
O2—C11.256 (2)C5—H50.9300
O3—C81.249 (2)C6—C71.395 (3)
O4—C81.272 (2)C7—H70.9300
O1i—Ba1—O1W89.50 (5)O2—Ba1—Ba1v72.77 (3)
O1i—Ba1—O4ii105.30 (5)O4iii—Ba1—Ba1v36.03 (3)
O1W—Ba1—O4ii71.13 (5)O3iii—Ba1—Ba1v76.62 (3)
O1i—Ba1—O2117.46 (4)N1iv—Ba1—Ba1v120.53 (3)
O1W—Ba1—O2143.56 (5)O1—Ba1—Ba1v112.75 (3)
O4ii—Ba1—O277.97 (5)C8iii—Ba1—Ba1v54.33 (4)
O1i—Ba1—O4iii167.63 (5)C1—Ba1—Ba1v91.86 (4)
O1W—Ba1—O4iii78.43 (5)C6iv—Ba1—Ba1v143.55 (3)
O4ii—Ba1—O4iii73.57 (5)C1—O1—Ba1i157.18 (14)
O2—Ba1—O4iii74.63 (4)C1—O1—Ba190.64 (12)
O1i—Ba1—O3iii126.70 (5)Ba1i—O1—Ba1106.97 (5)
O1W—Ba1—O3iii67.04 (5)Ba1—O1W—H1WA134.8
O4ii—Ba1—O3iii110.30 (4)Ba1—O1W—H1WB107.5
O2—Ba1—O3iii107.93 (5)H1WA—O1W—H1WB111.2
O4iii—Ba1—O3iii45.63 (4)C1—O2—Ba1101.23 (12)
O1i—Ba1—N1iv97.88 (5)C8—O3—Ba1vi93.35 (12)
O1W—Ba1—N1iv126.35 (5)C8—O4—Ba1ii129.23 (13)
O4ii—Ba1—N1iv151.39 (5)C8—O4—Ba1vi94.88 (12)
O2—Ba1—N1iv76.55 (5)Ba1ii—O4—Ba1vi106.43 (5)
O4iii—Ba1—N1iv87.26 (5)C6—N1—Ba1vii94.09 (12)
O3iii—Ba1—N1iv66.27 (5)C6—N1—H1A108.9
O1i—Ba1—O173.03 (5)Ba1vii—N1—H1A123.8
O1W—Ba1—O1155.90 (5)C6—N1—H1B110.7
O4ii—Ba1—O197.10 (4)Ba1vii—N1—H1B136.5
O2—Ba1—O145.23 (4)H1A—N1—H1B82.2
O4iii—Ba1—O1119.31 (4)O2—C1—O1122.41 (18)
O3iii—Ba1—O1136.85 (5)O2—C1—C2118.51 (17)
N1iv—Ba1—O173.66 (5)O1—C1—C2119.08 (17)
O1i—Ba1—C8iii147.07 (5)O2—C1—Ba156.41 (10)
O1W—Ba1—C8iii67.76 (5)O1—C1—Ba166.40 (11)
O4ii—Ba1—C8iii90.03 (5)C2—C1—Ba1170.98 (14)
O2—Ba1—C8iii93.92 (5)C3—C2—C7119.75 (18)
O4iii—Ba1—C8iii23.28 (5)C3—C2—C1120.48 (17)
O3iii—Ba1—C8iii22.89 (5)C7—C2—C1119.77 (17)
N1iv—Ba1—C8iii78.98 (5)C4—C3—C2120.14 (18)
O1—Ba1—C8iii134.77 (5)C4—C3—H3119.9
O1i—Ba1—C195.28 (5)C2—C3—H3119.9
O1W—Ba1—C1156.97 (5)C3—C4—C5119.66 (17)
O4ii—Ba1—C185.89 (5)C3—C4—C8121.00 (17)
O2—Ba1—C122.36 (4)C5—C4—C8119.32 (17)
O4iii—Ba1—C196.91 (5)C4—C5—C6120.87 (17)
O3iii—Ba1—C1125.09 (5)C4—C5—H5119.6
N1iv—Ba1—C175.35 (5)C6—C5—H5119.6
O1—Ba1—C122.96 (4)C5—C6—C7118.75 (17)
C8iii—Ba1—C1115.07 (5)C5—C6—N1120.32 (17)
O1i—Ba1—C6iv74.74 (5)C7—C6—N1120.73 (18)
O1W—Ba1—C6iv115.84 (5)C5—C6—Ba1vii107.12 (13)
O4ii—Ba1—C6iv172.98 (5)C7—C6—Ba1vii97.58 (12)
O2—Ba1—C6iv95.71 (5)N1—C6—Ba1vii60.87 (10)
O4iii—Ba1—C6iv107.94 (5)C2—C7—C6120.68 (18)
O3iii—Ba1—C6iv74.39 (5)C2—C7—H7119.7
N1iv—Ba1—C6iv25.04 (4)C6—C7—H7119.7
O1—Ba1—C6iv76.13 (5)O3—C8—O4123.16 (18)
C8iii—Ba1—C6iv93.49 (5)O3—C8—C4119.92 (18)
C1—Ba1—C6iv87.11 (5)O4—C8—C4116.91 (17)
O1i—Ba1—Ba1v141.47 (4)O3—C8—Ba1vi63.76 (11)
O1W—Ba1—Ba1v70.99 (3)O4—C8—Ba1vi61.84 (10)
O4ii—Ba1—Ba1v37.54 (3)C4—C8—Ba1vi162.79 (14)
Symmetry codes: (i) x, y+1, z+1; (ii) x, y, z+1; (iii) x, y+1, z1; (iv) x, y+1, z; (v) x, y+1, z; (vi) x, y1, z+1; (vii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O3i0.891.902.770 (2)165
O1W—H1WB···O2v0.831.952.770 (2)167
N1—H1A···O2viii0.962.163.067 (2)157
N1—H1B···O4ix0.992.193.176 (2)175
Symmetry codes: (i) x, y+1, z+1; (v) x, y+1, z; (viii) x+1, y, z; (ix) x+1, y1, z+1.

Experimental details

Crystal data
Chemical formula[Ba(C8H5NO4)(H2O)]
Mr334.48
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)7.7621 (1), 7.9652 (1), 8.3416 (1)
α, β, γ (°)79.618 (1), 65.574 (1), 83.575 (1)
V3)461.48 (1)
Z2
Radiation typeMo Kα
µ (mm1)4.30
Crystal size (mm)0.50 × 0.30 × 0.30
Data collection
DiffractometerBruker APEXII CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.232, 0.275
No. of measured, independent and
observed [I > 2σ(I)] reflections
7950, 2283, 2230
Rint0.019
(sin θ/λ)max1)0.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.015, 0.040, 1.12
No. of reflections2283
No. of parameters136
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.48, 0.79

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O3i0.891.902.770 (2)165
O1W—H1WB···O2ii0.831.952.770 (2)167
N1—H1A···O2iii0.962.163.067 (2)157
N1—H1B···O4iv0.992.193.176 (2)175
Symmetry codes: (i) x, y+1, z+1; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x+1, y1, z+1.
 

Acknowledgements

This research was supported by National Science Council, Taiwan (NSC99–2113-M-033–005-MY2).

References

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First citationZeng, R.-H., Fang, Z.-Q., Sun, F., Jiang, L.-S. & Tang, Y.-W. (2007). Acta Cryst. E63, m1813–m1814.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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