Literature DB >> 22259367

Bis-(μ-pyridine-2,3-dicarboxyl-ato)bis-[aqua-(3-carb-oxy-pyridine-2-carboxyl-ato)indium(III)] tetra-hydrate.

H Eshtiagh-Hosseini, M Mirzaei, A Mousavinezhad, M Necas, J T Mague.   

Abstract

In the binuclear centrosymmetric title compound, [In(2)(C(7)H(3)NO(4))(2)(C(7)H(4)NO(4))(2)(H(2)O)(2)]·4H(2)O, which contains both pyridine-2,3-dicarboxyl-ate and 3-carb-oxy-pyridine-2-carboxyl-ate ligands, the In(III) atom is six-coordinated in a distorted octa-hedral geometry. One pyridine ligand is N,O-chelated while the other is N,O-chelated and at the same time bridging to the other via the second carboxyl group. In the crystal, an extensive O-H⋯O hydrogen-bonding network, involving the coordinated and lattice water mol-ecules and the carboxyl groups of the ligands, together with C-H⋯O and π-π inter-actions [centroid-centroid distance = 3.793 (1) Å], leads to the formation of a three-dimensional structure.

Entities:  

Year:  2011        PMID： 22259367      PMCID： PMC3254334          DOI： 10.1107/S1600536811053566

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For metal complexes with polycarboxyl­ate ligands, see: Aghabozorg, Daneshvar et al. (2007 ▶); Aghabozorg, Khadivi et al. (2008 ▶); Aghabozorg, Ramezanipour et al. (2006 ▶); Eshtiagh-Hosseini et al. (2010 ▶); Mirzaei et al. (2011 ▶). For examples of self-assembly, see: Kondo et al. (1999 ▶); Beobide et al. (2006 ▶). For a discussion of hard–soft acid base concepts, see: Schlemper et al. (1967 ▶). For examples of π–π stacking, see: Janiak (2000 ▶). For three-dimensional network structures, see: Krygowski et al. (1998 ▶).

Experimental

Crystal data

[In2(C7H3NO4)2(C7H4NO4)2(H2O)2]·4H2O M = 1000.17 Triclinic, a = 8.0166 (3) Å b = 10.0890 (4) Å c = 11.9838 (5) Å α = 110.069 (4)° β = 96.236 (3)° γ = 109.076 (3)° V = 833.36 (6) Å3 Z = 1 Mo Kα radiation μ = 1.49 mm−1 T = 120 K 0.40 × 0.30 × 0.30 mm

Data collection

Oxford Diffraction Xcalibur diffractometer with a Sapphire2 detector Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009 ▶) T min = 0.588, T max = 0.664 10774 measured reflections 3373 independent reflections 3168 reflections with I > 2σ(I) R int = 0.013

Refinement

R[F 2 > 2σ(F 2)] = 0.016 wR(F 2) = 0.039 S = 1.10 3373 reflections 254 parameters H-atom parameters constrained Δρmax = 0.38 e Å−3 Δρmin = −0.31 e Å−3 Data collection: CrysAlis CCD (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2009 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811053566/su2349sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811053566/su2349Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[In2(C7H3NO4)2(C7H4NO4)2(H2O)2]·4H2OZ = 1
Mr = 1000.17F(000) = 496
Triclinic, P1Dx = 1.993 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.0166 (3) ÅCell parameters from 8569 reflections
b = 10.0890 (4) Åθ = 2.8–27.2°
c = 11.9838 (5) ŵ = 1.49 mm−1
α = 110.069 (4)°T = 120 K
β = 96.236 (3)°Block, colourless
γ = 109.076 (3)°0.40 × 0.30 × 0.30 mm
V = 833.36 (6) Å3
Oxford Diffraction Xcalibur diffractometer with a Sapphire2 detector3373 independent reflections
Radiation source: Enhance (Mo) X-ray Source3168 reflections with I > 2σ(I)
graphiteRint = 0.013
Detector resolution: 8.4353 pixels mm-1θmax = 27.2°, θmin = 3.3°
ω scanh = −8→10
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009)k = −12→12
Tmin = 0.588, Tmax = 0.664l = −15→15
10774 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.016H-atom parameters constrained
wR(F2) = 0.039w = 1/[σ2(Fo2) + (0.0197P)2 + 0.3217P] where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.002
3373 reflectionsΔρmax = 0.38 e Å−3
254 parametersΔρmin = −0.31 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0083 (5)
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.
xyzUiso*/Ueq
In10.716069 (17)0.792788 (13)0.730349 (10)0.00941 (5)
O10.81082 (17)0.78122 (15)0.57022 (11)0.0132 (3)
O20.77166 (18)0.81433 (15)0.39645 (11)0.0165 (3)
O30.43118 (19)0.60530 (14)0.22385 (11)0.0154 (3)
O40.38691 (19)0.80920 (15)0.21595 (11)0.0179 (3)
H4O0.38700.77210.14160.021*
O50.64775 (17)0.86624 (14)0.90207 (10)0.0127 (3)
O60.73152 (19)1.05169 (15)1.08983 (11)0.0171 (3)
O70.92356 (19)1.40964 (15)1.17662 (11)0.0165 (3)
O81.10615 (18)1.31541 (14)1.24362 (11)0.0144 (3)
O90.50749 (18)0.56958 (14)0.66940 (11)0.0168 (3)
H910.39720.55390.64730.020*
H920.53250.51800.70570.020*
N10.5111 (2)0.83155 (16)0.61329 (13)0.0105 (3)
N20.9159 (2)1.03454 (17)0.83361 (13)0.0104 (3)
C10.5347 (2)0.80161 (19)0.49914 (15)0.0101 (4)
C20.4018 (3)0.78340 (19)0.40403 (16)0.0120 (4)
C30.2455 (3)0.8044 (2)0.43128 (17)0.0159 (4)
H30.15270.79380.36850.019*
C40.2254 (3)0.8406 (2)0.54992 (17)0.0165 (4)
H40.12090.85830.56990.020*
C50.3595 (3)0.8508 (2)0.63908 (16)0.0135 (4)
H50.34420.87170.72000.016*
C60.7195 (2)0.79807 (19)0.48430 (15)0.0107 (4)
C70.4120 (3)0.7255 (2)0.27281 (16)0.0124 (4)
C80.9017 (3)1.0999 (2)0.94915 (15)0.0100 (3)
C91.0201 (3)1.2475 (2)1.02728 (15)0.0113 (4)
C101.1540 (3)1.3289 (2)0.98329 (16)0.0153 (4)
H101.23611.43051.03480.018*
C111.1667 (3)1.2612 (2)0.86462 (16)0.0158 (4)
H111.25701.31540.83350.019*
C121.0452 (3)1.1130 (2)0.79220 (16)0.0131 (4)
H121.05371.06550.71070.016*
C130.7493 (3)1.0014 (2)0.98602 (15)0.0113 (4)
C141.0119 (3)1.3270 (2)1.15813 (15)0.0121 (4)
O100.39345 (18)0.69562 (15)−0.00496 (11)0.0167 (3)
H1010.47040.7512−0.02930.020*
H1020.29440.6616−0.05720.020*
O110.83456 (19)0.48403 (16)0.39983 (12)0.0217 (3)
H1110.89430.56680.46090.026*
H1120.88490.47550.34130.026*
U11U22U33U12U13U23
In10.00961 (8)0.01133 (8)0.00717 (7)0.00362 (6)0.00213 (5)0.00400 (5)
O10.0104 (7)0.0217 (7)0.0097 (6)0.0077 (6)0.0033 (5)0.0072 (5)
O20.0164 (8)0.0241 (7)0.0127 (6)0.0077 (6)0.0072 (6)0.0105 (6)
O30.0209 (8)0.0118 (6)0.0123 (6)0.0055 (6)0.0014 (6)0.0050 (5)
O40.0275 (9)0.0184 (7)0.0112 (6)0.0112 (6)0.0027 (6)0.0084 (5)
O50.0112 (7)0.0143 (6)0.0108 (6)0.0026 (6)0.0040 (5)0.0049 (5)
O60.0181 (8)0.0196 (7)0.0113 (6)0.0046 (6)0.0074 (6)0.0049 (5)
O70.0191 (8)0.0186 (7)0.0129 (6)0.0119 (6)0.0014 (6)0.0039 (5)
O80.0164 (8)0.0191 (7)0.0098 (6)0.0102 (6)0.0018 (5)0.0055 (5)
O90.0132 (7)0.0150 (7)0.0218 (7)0.0033 (6)−0.0003 (6)0.0106 (6)
N10.0104 (8)0.0097 (7)0.0111 (7)0.0032 (6)0.0033 (6)0.0046 (6)
N20.0103 (8)0.0124 (7)0.0098 (7)0.0047 (7)0.0026 (6)0.0054 (6)
C10.0104 (10)0.0068 (8)0.0122 (8)0.0017 (7)0.0028 (7)0.0044 (7)
C20.0130 (10)0.0083 (8)0.0135 (8)0.0021 (8)0.0013 (7)0.0056 (7)
C30.0128 (10)0.0173 (9)0.0183 (9)0.0062 (8)0.0001 (8)0.0087 (8)
C40.0124 (10)0.0161 (9)0.0238 (10)0.0074 (8)0.0067 (8)0.0089 (8)
C50.0145 (10)0.0109 (9)0.0158 (9)0.0048 (8)0.0068 (8)0.0057 (7)
C60.0100 (10)0.0088 (8)0.0100 (8)0.0015 (7)0.0013 (7)0.0023 (7)
C70.0072 (9)0.0135 (9)0.0136 (8)0.0008 (8)−0.0013 (7)0.0063 (7)
C80.0104 (10)0.0131 (9)0.0094 (8)0.0063 (8)0.0027 (7)0.0062 (7)
C90.0115 (10)0.0142 (9)0.0100 (8)0.0068 (8)0.0012 (7)0.0058 (7)
C100.0149 (11)0.0139 (9)0.0139 (8)0.0027 (8)0.0007 (8)0.0054 (7)
C110.0147 (11)0.0171 (9)0.0153 (9)0.0027 (8)0.0056 (8)0.0090 (8)
C120.0142 (10)0.0158 (9)0.0107 (8)0.0057 (8)0.0050 (7)0.0065 (7)
C130.0104 (10)0.0148 (9)0.0113 (8)0.0070 (8)0.0017 (7)0.0067 (7)
C140.0103 (10)0.0110 (9)0.0115 (8)0.0009 (8)0.0015 (7)0.0038 (7)
O100.0133 (7)0.0224 (7)0.0134 (6)0.0027 (6)0.0014 (5)0.0106 (6)
O110.0204 (8)0.0215 (7)0.0203 (7)0.0069 (6)0.0059 (6)0.0061 (6)
In1—O8i2.1153 (12)C1—C21.390 (2)
In1—O12.1199 (12)C1—C61.522 (2)
In1—O92.1319 (13)C2—C31.392 (3)
In1—O52.1324 (11)C2—C71.500 (2)
In1—N22.2339 (15)C3—C41.383 (3)
In1—N12.2618 (14)C3—H30.9500
O1—C61.289 (2)C4—C51.383 (3)
O2—C61.216 (2)C4—H40.9500
O3—C71.221 (2)C5—H50.9500
O4—C71.302 (2)C8—C91.386 (3)
O4—H4O0.8401C8—C131.517 (3)
O5—C131.300 (2)C9—C101.396 (3)
O6—C131.216 (2)C9—C141.517 (2)
O7—C141.240 (2)C10—C111.382 (2)
O8—C141.268 (2)C10—H100.9500
O8—In1i2.1152 (12)C11—C121.383 (3)
O9—H910.8400C11—H110.9500
O9—H920.8400C12—H120.9500
N1—C51.343 (2)O10—H1010.8400
N1—C11.345 (2)O10—H1020.8400
N2—C121.339 (2)O11—H1110.8400
N2—C81.350 (2)O11—H1120.8400
O8i—In1—O183.58 (5)C2—C3—H3120.0
O8i—In1—O984.44 (5)C5—C4—C3119.06 (17)
O1—In1—O9101.63 (5)C5—C4—H4120.5
O8i—In1—O5104.07 (5)C3—C4—H4120.5
O1—In1—O5165.16 (5)N1—C5—C4121.17 (16)
O9—In1—O591.87 (5)N1—C5—H5119.4
O8i—In1—N297.32 (5)C4—C5—H5119.4
O1—In1—N291.20 (5)O2—C6—O1125.21 (17)
O9—In1—N2167.17 (5)O2—C6—C1119.13 (15)
O5—In1—N275.36 (5)O1—C6—C1115.64 (14)
O8i—In1—N1153.16 (5)O3—C7—O4124.16 (16)
O1—In1—N175.34 (5)O3—C7—C2121.80 (15)
O9—In1—N183.75 (5)O4—C7—C2113.89 (15)
O5—In1—N1100.33 (5)N2—C8—C9121.27 (16)
N2—In1—N199.52 (5)N2—C8—C13115.55 (15)
C6—O1—In1119.19 (11)C9—C8—C13123.18 (15)
C7—O4—H4O112.4C8—C9—C10118.45 (16)
C13—O5—In1118.93 (11)C8—C9—C14123.82 (16)
C14—O8—In1i140.24 (11)C10—C9—C14117.73 (16)
In1—O9—H91121.2C11—C10—C9119.83 (18)
In1—O9—H92112.4C11—C10—H10120.1
H91—O9—H92117.5C9—C10—H10120.1
C5—N1—C1120.12 (15)C10—C11—C12118.58 (18)
C5—N1—In1126.80 (11)C10—C11—H11120.7
C1—N1—In1111.76 (11)C12—C11—H11120.7
C12—N2—C8119.97 (16)N2—C12—C11121.89 (16)
C12—N2—In1126.11 (11)N2—C12—H12119.1
C8—N2—In1113.89 (12)C11—C12—H12119.1
N1—C1—C2121.65 (16)O6—C13—O5124.90 (17)
N1—C1—C6115.19 (15)O6—C13—C8119.05 (16)
C2—C1—C6123.09 (15)O5—C13—C8116.05 (14)
C1—C2—C3118.00 (16)O7—C14—O8123.27 (15)
C1—C2—C7122.31 (16)O7—C14—C9117.88 (15)
C3—C2—C7119.33 (16)O8—C14—C9118.63 (15)
C4—C3—C2119.91 (17)H101—O10—H102105.0
C4—C3—H3120.0H111—O11—H112111.8
O8i—In1—O1—C6162.67 (13)C2—C3—C4—C5−2.0 (3)
O9—In1—O1—C679.72 (13)C1—N1—C5—C4−0.1 (3)
O5—In1—O1—C6−75.3 (2)In1—N1—C5—C4−165.89 (13)
N2—In1—O1—C6−100.10 (13)C3—C4—C5—N12.5 (3)
N1—In1—O1—C6−0.57 (12)In1—O1—C6—O2169.57 (14)
O8i—In1—O5—C1389.72 (12)In1—O1—C6—C1−8.69 (19)
O1—In1—O5—C13−30.0 (2)N1—C1—C6—O2−159.83 (16)
O9—In1—O5—C13174.45 (12)C2—C1—C6—O216.9 (3)
N2—In1—O5—C13−4.31 (11)N1—C1—C6—O118.5 (2)
N1—In1—O5—C13−101.56 (12)C2—C1—C6—O1−164.68 (16)
O8i—In1—N1—C5138.04 (14)C1—C2—C7—O353.6 (3)
O1—In1—N1—C5177.42 (15)C3—C2—C7—O3−119.3 (2)
O9—In1—N1—C573.64 (15)C1—C2—C7—O4−130.59 (18)
O5—In1—N1—C5−17.12 (15)C3—C2—C7—O456.5 (2)
N2—In1—N1—C5−93.83 (15)C12—N2—C8—C9−0.6 (2)
O8i—In1—N1—C1−28.73 (19)In1—N2—C8—C9177.46 (12)
O1—In1—N1—C110.65 (11)C12—N2—C8—C13179.38 (15)
O9—In1—N1—C1−93.12 (12)In1—N2—C8—C13−2.56 (18)
O5—In1—N1—C1176.11 (12)N2—C8—C9—C100.9 (2)
N2—In1—N1—C199.40 (12)C13—C8—C9—C10−179.06 (16)
O8i—In1—N2—C1278.74 (14)N2—C8—C9—C14−179.73 (16)
O1—In1—N2—C12−4.94 (14)C13—C8—C9—C140.3 (3)
O9—In1—N2—C12175.85 (19)C8—C9—C10—C11−0.5 (3)
O5—In1—N2—C12−178.56 (15)C14—C9—C10—C11−179.94 (16)
N1—In1—N2—C12−80.27 (14)C9—C10—C11—C12−0.1 (3)
O8i—In1—N2—C8−99.18 (12)C8—N2—C12—C11−0.1 (3)
O1—In1—N2—C8177.14 (12)In1—N2—C12—C11−177.90 (13)
O9—In1—N2—C8−2.1 (3)C10—C11—C12—N20.4 (3)
O5—In1—N2—C83.52 (11)In1—O5—C13—O6−174.77 (13)
N1—In1—N2—C8101.80 (12)In1—O5—C13—C84.34 (18)
C5—N1—C1—C2−2.7 (3)N2—C8—C13—O6178.18 (15)
In1—N1—C1—C2165.07 (13)C9—C8—C13—O6−1.8 (3)
C5—N1—C1—C6174.13 (15)N2—C8—C13—O5−1.0 (2)
In1—N1—C1—C6−18.10 (17)C9—C8—C13—O5179.00 (15)
N1—C1—C2—C33.0 (3)In1i—O8—C14—O7−176.98 (13)
C6—C1—C2—C3−173.52 (16)In1i—O8—C14—C9−2.6 (3)
N1—C1—C2—C7−169.95 (16)C8—C9—C14—O7−93.8 (2)
C6—C1—C2—C713.5 (3)C10—C9—C14—O785.6 (2)
C1—C2—C3—C4−0.7 (3)C8—C9—C14—O891.5 (2)
C7—C2—C3—C4172.56 (17)C10—C9—C14—O8−89.1 (2)
D—H···AD—HH···AD···AD—H···A
O9—H91···O11ii0.841.752.5938 (19)178
O9—H92···O3ii0.841.802.6402 (17)175
O11—H112···O7iii0.841.952.7595 (18)162
O10—H101···O5iv0.841.972.8065 (18)175
O10—H102···O7v0.841.882.7237 (19)178
O4—H4O···O100.841.672.5124 (17)178
C4—H4···O1vi0.952.353.231 (2)154
C5—H5···O6vii0.952.363.293 (2)168
C11—H11···O3viii0.952.613.495 (2)156
C12—H12···O2viii0.952.332.993 (2)126
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O9—H91⋯O11i0.841.752.5938 (19)178
O9—H92⋯O3i0.841.802.6402 (17)175
O11—H112⋯O7ii0.841.952.7595 (18)162
O10—H101⋯O5iii0.841.972.8065 (18)175
O10—H102⋯O7iv0.841.882.7237 (19)178
O4—H4O⋯O100.841.672.5124 (17)178
C4—H4⋯O1v0.952.353.231 (2)154
C5—H5⋯O6vi0.952.363.293 (2)168
C11—H11⋯O3vii0.952.613.495 (2)156
C12—H12⋯O2vii0.952.332.993 (2)126

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

  3 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Supramolecular architectures and magnetic properties of coordination polymers based on pyrazinedicarboxylato ligands showing embedded water clusters.

Authors:  Garikoitz Beobide; Oscar Castillo; Antonio Luque; Urko García-Couceiro; Juan P García-Terán; Pascual Román
Journal:  Inorg Chem       Date:  2006-07-10       Impact factor: 5.165

3.  Poly[propane-1,3-diammonium [cuprate(II)-bis-(μ(2)-pyridine-2,3-dicarboxyl-ato)] trihydrate].

Authors:  Hossein Aghabozorg; Ramona Khadivi; Mohammad Ghadermazi; Hoda Pasdar; Shabnam Hooshmand
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-01-04
  3 in total

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