Literature DB >> 21836851

Poly[tri-μ(2)-aqua-(μ(3)-pyridine-2,4-dicarboxyl-ato-κN,O:O:O)barium].

Hoda Pasdar, Shadi Siabi, Behrouz Notash, Hossein Aghabozorg, Naser Foroughifar.   

Abstract

In the polymeric title compound, [Ba(C(7)H(3)NO(4))(H(2)O)(3)](n), the Ba(II) ion is ten-coordinated in an NO(9) environment by one N atom and three O atoms from three pyridine-2,4-dicarboxyl-ate (pydc) ligands and six water mol-ecules. The μ(3)-pydc ligands and the bridging water mol-ecules connect the Ba atoms into a layer parallel to (100). The crystal packing is stabilized by O-H⋯O and C-H⋯O hydrogen bonds.

Entities:  

Year:  2011        PMID： 21836851      PMCID： PMC3151937          DOI： 10.1107/S1600536811020204

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


Related literature

For related compounds with pyridine dicarb­oxy­lic acid deriv­atives, see: Aghabozorg et al. (2008 ▶, 2011a ▶,b ▶,c ▶,d ▶); Noro et al. (2005 ▶); Pasdar et al. (2011a ▶,b ▶); Wang et al. (2007 ▶).

Experimental

Crystal data

[Ba(C7H3NO4)(H2O)3] M = 356.48 Monoclinic, a = 11.079 (2) Å b = 13.714 (3) Å c = 6.5961 (13) Å β = 94.13 (3)° V = 999.6 (3) Å3 Z = 4 Mo Kα radiation μ = 4.00 mm−1 T = 298 K 0.39 × 0.38 × 0.33 mm

Data collection

Stoe IPDS-2T diffractometer Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005 ▶) T min = 0.410, T max = 0.460 7321 measured reflections 2681 independent reflections 2515 reflections with I > 2σ(I) R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.023 wR(F 2) = 0.057 S = 1.10 2681 reflections 170 parameters 1 restraint H atoms treated by a mixture of independent and constrained refinement Δρmax = 2.20 e Å−3 Δρmin = −0.60 e Å−3 Data collection: X-AREA (Stoe & Cie, 2005 ▶); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811020204/hy2431sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811020204/hy2431Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ba(C7H3NO4)(H2O)3]F(000) = 680
Mr = 356.48Dx = 2.369 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2681 reflections
a = 11.079 (2) Åθ = 2.4–29.1°
b = 13.714 (3) ŵ = 4.00 mm−1
c = 6.5961 (13) ÅT = 298 K
β = 94.13 (3)°Block, colorless
V = 999.6 (3) Å30.39 × 0.38 × 0.33 mm
Z = 4
Stoe IPDS-2T diffractometer2681 independent reflections
Radiation source: fine-focus sealed tube2515 reflections with I > 2σ(I)
graphiteRint = 0.041
ω scansθmax = 29.1°, θmin = 2.4°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005)h = −15→13
Tmin = 0.410, Tmax = 0.460k = −18→18
7321 measured reflectionsl = −9→9
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.057w = 1/[σ2(Fo2) + (0.0343P)2 + 0.2871P] where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.002
2681 reflectionsΔρmax = 2.20 e Å−3
170 parametersΔρmin = −0.60 e Å−3
1 restraintExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0182 (7)
xyzUiso*/Ueq
H6B−0.211 (3)0.577 (3)−0.019 (6)0.045 (11)*
O6−0.16582 (16)0.54989 (14)0.0517 (3)0.0245 (3)
O7−0.09028 (16)0.75423 (14)−0.1846 (3)0.0234 (3)
O50.02949 (17)0.45857 (14)0.2957 (3)0.0233 (3)
Ba10.074526 (10)0.638147 (8)0.073630 (17)0.01506 (7)
C20.4566 (2)0.63768 (15)0.5688 (4)0.0179 (4)
H20.46720.65080.70730.021*
N10.32012 (18)0.61649 (17)0.2709 (3)0.0223 (4)
C10.3411 (2)0.63417 (14)0.4713 (4)0.0166 (4)
C50.4167 (2)0.6023 (2)0.1646 (4)0.0290 (5)
H50.40400.59070.02580.035*
O10.13032 (15)0.66224 (14)0.4870 (3)0.0227 (3)
O20.24279 (19)0.65068 (17)0.7766 (3)0.0341 (5)
C60.2301 (2)0.64984 (16)0.5894 (4)0.0175 (4)
C70.6829 (2)0.62030 (18)0.5578 (4)0.0206 (4)
C30.5562 (2)0.62132 (17)0.4560 (4)0.0186 (4)
C40.5348 (2)0.6037 (2)0.2492 (4)0.0268 (5)
H40.59900.59300.16850.032*
O30.69566 (19)0.64657 (16)0.7382 (3)0.0340 (5)
O40.76764 (15)0.59321 (15)0.4537 (3)0.0278 (4)
H5A−0.019 (4)0.438 (3)0.361 (6)0.047 (11)*
H5B0.087 (4)0.448 (3)0.364 (6)0.048 (12)*
H7B−0.116 (4)0.792 (3)−0.116 (6)0.039 (10)*
H6A−0.209 (4)0.550 (3)0.164 (6)0.043 (10)*
H7A−0.155 (4)0.723 (3)−0.215 (7)0.060 (13)*
U11U22U33U12U13U23
O60.0208 (8)0.0317 (9)0.0211 (8)0.0043 (7)0.0026 (7)0.0017 (7)
O70.0204 (8)0.0251 (8)0.0246 (8)−0.0010 (7)0.0016 (7)−0.0014 (7)
O50.0192 (8)0.0316 (9)0.0191 (8)0.0005 (7)0.0014 (7)0.0040 (7)
Ba10.01347 (9)0.01844 (9)0.01335 (10)0.00009 (4)0.00141 (5)−0.00001 (4)
C20.0153 (10)0.0255 (11)0.0128 (10)−0.0002 (7)0.0004 (8)0.0007 (7)
N10.0169 (9)0.0350 (10)0.0148 (9)0.0023 (8)−0.0012 (7)−0.0034 (8)
C10.0128 (9)0.0217 (10)0.0156 (10)0.0007 (7)0.0026 (8)0.0003 (7)
C50.0177 (10)0.0535 (16)0.0157 (10)0.0048 (11)0.0003 (8)−0.0053 (11)
O10.0135 (7)0.0330 (8)0.0218 (8)0.0041 (6)0.0017 (6)0.0010 (7)
O20.0216 (9)0.0644 (14)0.0170 (9)−0.0006 (8)0.0052 (7)−0.0048 (8)
C60.0138 (9)0.0202 (9)0.0189 (10)−0.0006 (7)0.0042 (8)−0.0010 (8)
C70.0137 (9)0.0240 (9)0.0237 (11)−0.0005 (8)−0.0013 (8)0.0044 (9)
C30.0146 (9)0.0227 (9)0.0182 (10)0.0006 (8)0.0002 (8)0.0014 (8)
C40.0160 (10)0.0466 (15)0.0179 (11)0.0017 (10)0.0026 (8)−0.0032 (10)
O30.0237 (10)0.0518 (12)0.0252 (10)0.0041 (8)−0.0065 (8)−0.0064 (8)
O40.0156 (7)0.0406 (10)0.0272 (9)0.0030 (7)0.0023 (6)0.0028 (8)
O6—H6B0.75 (3)C2—C11.391 (3)
O6—H6A0.91 (4)C2—C31.393 (3)
O7—H7B0.75 (4)C2—H20.9300
O7—H7A0.85 (5)N1—C51.336 (3)
O5—H5A0.77 (5)N1—C11.347 (3)
O5—H5B0.77 (5)C1—C61.518 (3)
Ba1—O12.7720 (19)C5—C41.385 (3)
Ba1—O2i2.805 (2)C5—H50.9300
Ba1—O1ii2.8728 (19)O1—C61.265 (3)
Ba1—O7iii2.9111 (18)O2—C61.233 (3)
Ba1—O72.8846 (19)C7—O31.242 (3)
Ba1—O6iv2.9115 (19)C7—O41.258 (3)
Ba1—O5iv2.935 (2)C7—C31.511 (3)
Ba1—O52.9263 (19)C3—C41.389 (3)
Ba1—N12.945 (2)C4—H40.9300
Ba1—O62.9190 (19)
Ba1iv—O6—Ba192.69 (5)O7—Ba1—N1147.33 (6)
Ba1iv—O6—H6B119 (3)O7iii—Ba1—N1113.88 (6)
Ba1—O6—H6B113 (3)O6iv—Ba1—N172.99 (6)
Ba1iv—O6—H6A117 (2)O6—Ba1—N1142.22 (6)
Ba1—O6—H6A119 (2)O5—Ba1—N183.07 (6)
H6B—O6—H6A98 (4)O5iv—Ba1—N1128.03 (6)
Ba1—O7—Ba1ii102.01 (6)O1—Ba1—C6ii77.88 (6)
Ba1—O7—H7B106 (3)O2i—Ba1—C6ii66.76 (6)
Ba1ii—O7—H7B105 (3)O1ii—Ba1—C6ii21.45 (5)
Ba1—O7—H7A110 (3)O7—Ba1—C6ii80.97 (6)
Ba1ii—O7—H7A133 (3)O7iii—Ba1—C6ii83.42 (5)
H7B—O7—H7A98 (4)O6iv—Ba1—C6ii125.75 (5)
Ba1—O5—Ba1iv92.06 (5)O6—Ba1—C6ii145.09 (5)
Ba1—O5—H5A138 (3)O5—Ba1—C6ii144.49 (6)
Ba1iv—O5—H5A93 (3)O5iv—Ba1—C6ii125.70 (5)
Ba1—O5—H5B107 (3)N1—Ba1—C6ii67.67 (6)
Ba1iv—O5—H5B131 (3)O1—Ba1—Ba1iv112.92 (4)
H5A—O5—H5B101 (4)O2i—Ba1—Ba1iv99.38 (5)
O1—Ba1—O2i124.57 (6)O1ii—Ba1—Ba1iv153.68 (4)
O1—Ba1—O1ii92.64 (5)O7—Ba1—Ba1iv98.00 (4)
O2i—Ba1—O1ii68.86 (6)O7iii—Ba1—Ba1iv109.33 (4)
O1—Ba1—O7127.00 (5)O6iv—Ba1—Ba1iv43.72 (4)
O2i—Ba1—O788.74 (6)O6—Ba1—Ba1iv43.58 (4)
O1ii—Ba1—O759.52 (5)O5—Ba1—Ba1iv44.06 (4)
O1—Ba1—O7iii60.32 (5)O5iv—Ba1—Ba1iv43.89 (4)
O2i—Ba1—O7iii145.70 (6)N1—Ba1—Ba1iv110.18 (5)
O1ii—Ba1—O7iii77.19 (5)C1—C2—C3119.0 (2)
O7—Ba1—O7iii69.42 (3)C1—C2—H2120.5
O1—Ba1—O6iv109.12 (5)C3—C2—H2120.5
O2i—Ba1—O6iv66.05 (6)C5—N1—C1116.9 (2)
O1ii—Ba1—O6iv134.70 (5)C5—N1—Ba1122.17 (16)
O7—Ba1—O6iv122.63 (6)C1—N1—Ba1120.28 (14)
O7iii—Ba1—O6iv148.11 (5)N1—C1—C2123.3 (2)
O1—Ba1—O6103.66 (6)N1—C1—C6116.1 (2)
O2i—Ba1—O6129.84 (6)C2—C1—C6120.7 (2)
O1ii—Ba1—O6126.43 (5)N1—C5—C4123.8 (2)
O7—Ba1—O670.32 (5)N1—C5—H5118.1
O7iii—Ba1—O668.38 (5)C4—C5—H5118.1
O6iv—Ba1—O687.31 (5)C6—O1—Ba1129.32 (14)
O1—Ba1—O569.02 (5)C6—O1—Ba1iii102.37 (14)
O2i—Ba1—O5123.15 (6)Ba1—O1—Ba1iii105.86 (6)
O1ii—Ba1—O5161.49 (5)C6—O2—Ba1v131.70 (16)
O7—Ba1—O5129.53 (5)O2—C6—O1124.5 (2)
O7iii—Ba1—O590.93 (5)O2—C6—C1118.5 (2)
O6iv—Ba1—O558.13 (5)O1—C6—C1117.0 (2)
O6—Ba1—O559.20 (6)O2—C6—Ba1iii92.52 (15)
O1—Ba1—O5iv156.43 (5)O1—C6—Ba1iii56.18 (12)
O2i—Ba1—O5iv71.89 (6)C1—C6—Ba1iii122.45 (13)
O1ii—Ba1—O5iv110.05 (5)O3—C7—O4124.8 (2)
O7—Ba1—O5iv64.24 (6)O3—C7—C3117.5 (2)
O7iii—Ba1—O5iv117.35 (5)O4—C7—C3117.8 (2)
O6iv—Ba1—O5iv59.19 (5)C4—C3—C2117.8 (2)
O6—Ba1—O5iv57.95 (5)C4—C3—C7121.5 (2)
O5—Ba1—O5iv87.94 (5)C2—C3—C7120.7 (2)
O1—Ba1—N156.21 (6)C5—C4—C3119.2 (2)
O2i—Ba1—N171.07 (6)C5—C4—H4120.4
O1ii—Ba1—N188.79 (6)C3—C4—H4120.4
Ba1ii—O7—Ba1—O1108.60 (7)C5—N1—C1—C2−0.2 (4)
Ba1ii—O7—Ba1—O2i−25.36 (7)Ba1—N1—C1—C2−171.43 (15)
Ba1ii—O7—Ba1—O1ii40.72 (5)C5—N1—C1—C6−179.8 (2)
Ba1ii—O7—Ba1—O7iii127.63 (8)Ba1—N1—C1—C69.0 (3)
Ba1ii—O7—Ba1—O6iv−85.61 (7)C3—C2—C1—N1−0.6 (3)
Ba1ii—O7—Ba1—O6−158.86 (7)C3—C2—C1—C6178.93 (19)
Ba1ii—O7—Ba1—O5−159.07 (5)C1—N1—C5—C40.7 (4)
Ba1ii—O7—Ba1—O5iv−95.80 (7)Ba1—N1—C5—C4171.8 (2)
Ba1ii—O7—Ba1—N125.18 (13)O2i—Ba1—O1—C6−24.9 (2)
Ba1ii—O7—Ba1—C6ii41.31 (6)O1ii—Ba1—O1—C6−90.95 (18)
Ba1ii—O7—Ba1—Ba1iv−124.66 (5)O7—Ba1—O1—C6−144.00 (18)
Ba1iv—O6—Ba1—O1−109.03 (5)O7iii—Ba1—O1—C6−164.6 (2)
Ba1iv—O6—Ba1—O2i55.35 (9)O6iv—Ba1—O1—C648.6 (2)
Ba1iv—O6—Ba1—O1ii147.19 (5)O6—Ba1—O1—C6140.52 (19)
Ba1iv—O6—Ba1—O7126.16 (6)O5—Ba1—O1—C691.6 (2)
Ba1iv—O6—Ba1—O7iii−158.90 (7)O5iv—Ba1—O1—C6104.5 (2)
Ba1iv—O6—Ba1—O6iv0.0N1—Ba1—O1—C6−4.18 (18)
Ba1iv—O6—Ba1—O5−54.04 (5)C6ii—Ba1—O1—C6−75.3 (2)
Ba1iv—O6—Ba1—O5iv54.86 (5)Ba1iv—Ba1—O1—C695.48 (19)
Ba1iv—O6—Ba1—N1−57.40 (10)O2i—Ba1—O1—Ba1iii96.43 (7)
Ba1iv—O6—Ba1—C6ii162.67 (7)O1ii—Ba1—O1—Ba1iii30.42 (8)
Ba1iv—O5—Ba1—O1174.89 (6)O7—Ba1—O1—Ba1iii−22.64 (8)
Ba1iv—O5—Ba1—O2i−66.73 (8)O7iii—Ba1—O1—Ba1iii−43.21 (5)
Ba1iv—O5—Ba1—O1ii166.78 (13)O6iv—Ba1—O1—Ba1iii170.00 (5)
Ba1iv—O5—Ba1—O753.60 (8)O6—Ba1—O1—Ba1iii−98.11 (6)
Ba1iv—O5—Ba1—O7iii117.34 (5)O5—Ba1—O1—Ba1iii−147.01 (7)
Ba1iv—O5—Ba1—O6iv−54.46 (5)O5iv—Ba1—O1—Ba1iii−134.14 (11)
Ba1iv—O5—Ba1—O653.36 (6)N1—Ba1—O1—Ba1iii117.19 (8)
Ba1iv—O5—Ba1—O5iv0.0C6ii—Ba1—O1—Ba1iii46.08 (6)
Ba1iv—O5—Ba1—N1−128.71 (6)Ba1iv—Ba1—O1—Ba1iii−143.15 (4)
Ba1iv—O5—Ba1—C6ii−162.71 (6)Ba1v—O2—C6—O114.9 (4)
O1—Ba1—N1—C5−174.1 (2)Ba1v—O2—C6—C1−165.84 (15)
O2i—Ba1—N1—C5−12.0 (2)Ba1v—O2—C6—Ba1iii64.7 (2)
O1ii—Ba1—N1—C5−80.1 (2)Ba1—O1—C6—O2−170.54 (18)
O7—Ba1—N1—C5−66.7 (3)Ba1iii—O1—C6—O266.7 (3)
O7iii—Ba1—N1—C5−155.5 (2)Ba1—O1—C6—C110.2 (3)
O6iv—Ba1—N1—C557.8 (2)Ba1iii—O1—C6—C1−112.54 (17)
O6—Ba1—N1—C5119.5 (2)Ba1—O1—C6—Ba1iii122.77 (18)
O5—Ba1—N1—C5116.6 (2)N1—C1—C6—O2168.6 (2)
O5iv—Ba1—N1—C534.7 (2)C2—C1—C6—O2−11.0 (3)
C6ii—Ba1—N1—C5−84.0 (2)N1—C1—C6—O1−12.2 (3)
Ba1iv—Ba1—N1—C581.3 (2)C2—C1—C6—O1168.2 (2)
O1—Ba1—N1—C1−3.35 (16)N1—C1—C6—Ba1iii−77.6 (2)
O2i—Ba1—N1—C1158.68 (19)C2—C1—C6—Ba1iii102.8 (2)
O1ii—Ba1—N1—C190.65 (18)C1—C2—C3—C41.0 (3)
O7—Ba1—N1—C1103.99 (18)C1—C2—C3—C7−177.42 (19)
O7iii—Ba1—N1—C115.24 (19)O3—C7—C3—C4172.7 (3)
O6iv—Ba1—N1—C1−131.43 (19)O4—C7—C3—C4−7.1 (4)
O6—Ba1—N1—C1−69.8 (2)O3—C7—C3—C2−8.9 (3)
O5—Ba1—N1—C1−72.70 (18)O4—C7—C3—C2171.3 (2)
O5iv—Ba1—N1—C1−154.60 (16)N1—C5—C4—C3−0.4 (5)
C6ii—Ba1—N1—C186.74 (18)C2—C3—C4—C5−0.5 (4)
Ba1iv—Ba1—N1—C1−108.02 (17)C7—C3—C4—C5177.9 (3)
D—H···AD—HH···AD···AD—H···A
C5—H5···O2i0.932.483.161 (3)130
O5—H5A···O1vi0.77 (5)2.14 (4)2.881 (3)162 (4)
O5—H5B···O4vii0.77 (5)2.02 (5)2.785 (3)174 (4)
O6—H6A···O4viii0.91 (4)2.03 (4)2.865 (3)151 (3)
O6—H6B···O3ix0.76 (4)2.08 (4)2.816 (3)167 (4)
O7—H7A···O3ix0.85 (5)1.96 (5)2.809 (3)175 (4)
O7—H7B···O4x0.75 (4)2.11 (4)2.810 (3)155 (4)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C5—H5⋯O2i0.932.483.161 (3)130
O5—H5A⋯O1ii0.77 (5)2.14 (4)2.881 (3)162 (4)
O5—H5B⋯O4iii0.77 (5)2.02 (5)2.785 (3)174 (4)
O6—H6A⋯O4iv0.91 (4)2.03 (4)2.865 (3)151 (3)
O6—H6B⋯O3v0.76 (4)2.08 (4)2.816 (3)167 (4)
O7—H7A⋯O3v0.85 (5)1.96 (5)2.809 (3)175 (4)
O7—H7B⋯O4vi0.75 (4)2.11 (4)2.810 (3)155 (4)

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

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Authors:  Hossein Aghabozorg; Saba Goodarzi; Masoud Mirzaei; Behrouz Notash
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-29

5.  Poly[aqua-(dimethyl sulfoxide)(μ(4)-pyridine-2,5-dicarboxyl-ato)calcium(II)].

Authors:  Hoda Pasdar; Zahra Safari; Hossein Aghabozorg; Behrouz Notash; Masoud Mirzaei
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15

6.  2,2'-Azanediyl-diethanaminium pyridine-2,5-dicarboxyl-ate.

Authors:  Hossein Aghabozorg; Maryam Saemi; Zeynab Khazaei; Vahid Amani; Behrouz Notash
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-08

7.  Bis(1-methyl-4-oxoimidazolidin-2-iminium) diaqua-bis-(pyridine-2,4-dicarboxyl-ato-κN,O)zincate(II) dihydrate.

Authors:  Hossein Aghabozorg; Fatemeh Jafarbak; Masoud Mirzaei; Behrouz Notash
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-03-12

8.  Propane-1,3-diaminium pyridine-2,5-di-carboxyl-ate dimethyl sulfoxide mono-solvate.

Authors:  Hossein Aghabozorg; Minoo Bayan; Masoud Mirzaei; Behrouz Notash
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-02-12
  8 in total

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