Literature DB >> 21577739

Poly[diaqua-(μ(2)-5-carboxy-pyridine-3-carboxyl-ato-κN:O)hemi(μ(2)-oxalato-κO,O:O,O)(μ(4)-pyridine-3,5-dicarboxyl-ato-κN:O:O:O)silver(I)terbium(III)].

Hai-Fu Guo1, Liang Qin, Xiang-Ying Hao.   

Abstract

In the title coordination polymer, [AgTb(C(7)H(3)NO(4))(C(7)H(4)NO(4))(C(2)O(4))(0.5)(H(2)O)(2)](n), the Tb(III) ion is eight-coordinated by three O atoms from three different pydc (H(2)pydc = pyridine-3,5-dicarboxylic acid) ligands, one O atom from one Hpydc ligand, two O atoms from one oxalate ligand and two water mol-ecules in a distorted square-anti-prismatic geometry. The Ag(I) ion is coordinated in an almost linear fashion by two pyridyl N atoms from one pydc and one Hpydc ligand and has weak inter-actions with two carboxyl-ate O atoms. The carboxyl-ate groups of pydc and Hpydc ligands link Tb centers, forming a one-dimensional chain. The oxalate adopts a tetra-dentate bis-chelating coordination mode, connecting the chains into a two-dimensional layer. These layers are further assembled via [Ag(pydc)(Hpydc)] pillars and O-H⋯O and C-H⋯O hydrogen bonds into a three-dimensional coordination framework.

Entities:  

Year:  2009        PMID： 21577739      PMCID： PMC2970247          DOI： 10.1107/S1600536809036393

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


Related literature

For general background to transition metal–lanthanide complexes, see: Barbour (2006 ▶); Kepert (2006 ▶); Kong et al. (2008 ▶); Rao et al. (2004 ▶); Wu et al. (2008 ▶); Zhang et al. (2005 ▶).

Experimental

Crystal data

[AgTb(C7H3NO4)(C7H4NO4)(C2O4)0.5(H2O)2] M = 678.05 Triclinic, a = 7.592 (3) Å b = 8.249 (3) Å c = 14.241 (6) Å α = 98.956 (4)° β = 99.556 (4)° γ = 95.839 (5)° V = 861.3 (6) Å3 Z = 2 Mo Kα radiation μ = 5.29 mm−1 T = 293 K 0.30 × 0.24 × 0.19 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.251, T max = 0.378 4416 measured reflections 3032 independent reflections 2862 reflections with I > 2σ(I) R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.023 wR(F 2) = 0.062 S = 1.09 3032 reflections 284 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.85 e Å−3 Δρmin = −0.79 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I. DOI: 10.1107/S1600536809036393/hy2227sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809036393/hy2227Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[AgTb(C7H3NO4)(C7H4NO4)(C2O4)0.5(H2O)2]Z = 2
Mr = 678.05F(000) = 646
Triclinic, P1Dx = 2.615 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.592 (3) ÅCell parameters from 3600 reflections
b = 8.249 (3) Åθ = 1.4–28°
c = 14.241 (6) ŵ = 5.29 mm−1
α = 98.956 (4)°T = 293 K
β = 99.556 (4)°Block, colorless
γ = 95.839 (5)°0.30 × 0.24 × 0.19 mm
V = 861.3 (6) Å3
Bruker APEXII CCD diffractometer3032 independent reflections
Radiation source: fine-focus sealed tube2862 reflections with I > 2σ(I)
graphiteRint = 0.018
φ and ω scansθmax = 25.2°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −9→6
Tmin = 0.251, Tmax = 0.378k = −9→9
4416 measured reflectionsl = −16→17
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.062H atoms treated by a mixture of independent and constrained refinement
S = 1.09w = 1/[σ2(Fo2) + (0.0323P)2] where P = (Fo2 + 2Fc2)/3
3032 reflections(Δ/σ)max = 0.049
284 parametersΔρmax = 0.85 e Å−3
0 restraintsΔρmin = −0.79 e Å−3
xyzUiso*/Ueq
Tb10.80756 (3)0.29706 (2)0.080761 (13)0.01369 (8)
Ag10.17209 (6)0.40250 (5)0.53284 (3)0.03343 (12)
O10.4372 (5)0.2187 (4)0.2009 (2)0.0305 (8)
O1W0.7121 (5)0.5291 (4)0.0096 (2)0.0278 (8)
H1W0.77420.5573−0.03020.042*
H2W0.63160.59040.01650.042*
O20.6205 (4)0.4300 (4)0.1747 (2)0.0255 (7)
O2W1.0914 (4)0.1769 (4)0.0759 (2)0.0253 (7)
H3W1.10700.13930.02000.038*
H4W1.18760.19050.11660.038*
O30.4778 (6)0.9748 (5)0.2896 (3)0.0449 (10)
O40.3416 (5)1.0334 (4)0.4169 (2)0.0346 (8)
O51.0531 (4)0.5114 (3)0.1239 (2)0.0203 (7)
O90.5031 (4)0.2064 (3)−0.0119 (2)0.0209 (7)
N10.3034 (5)0.5246 (4)0.4335 (3)0.0234 (8)
N20.8987 (5)0.7556 (4)0.3678 (2)0.0192 (8)
C10.3576 (6)0.4244 (5)0.3627 (3)0.0231 (10)
H10.33770.31060.36010.028*
C20.4420 (6)0.4845 (5)0.2934 (3)0.0188 (9)
C30.4629 (6)0.6531 (5)0.2942 (3)0.0204 (9)
H30.51620.69650.24760.025*
C40.4032 (6)0.7568 (5)0.3654 (3)0.0200 (9)
C50.3273 (6)0.6886 (5)0.4347 (3)0.0208 (10)
H50.29170.75870.48380.025*
C60.5041 (6)0.3688 (5)0.2177 (3)0.0216 (10)
C70.4047 (6)0.9388 (6)0.3621 (3)0.0246 (10)
C80.9565 (6)0.6777 (5)0.2901 (3)0.0165 (9)
H80.96580.56520.28490.020*
C91.0023 (6)0.7592 (5)0.2182 (3)0.0169 (9)
C100.9849 (6)0.9277 (5)0.2249 (3)0.0168 (9)
H101.01420.98480.17700.020*
C110.9234 (6)1.0091 (5)0.3038 (3)0.0166 (9)
C120.8845 (6)0.9188 (5)0.3740 (3)0.0201 (9)
H120.84690.97320.42790.024*
C131.0667 (6)0.6684 (5)0.1333 (3)0.0151 (9)
C150.4376 (6)0.0595 (5)−0.0196 (3)0.0168 (9)
O61.1310 (4)0.7500 (3)0.0780 (2)0.0211 (7)
C140.9003 (6)1.1915 (5)0.3113 (3)0.0202 (10)
O70.8768 (5)1.2673 (4)0.3899 (2)0.0328 (8)
O100.2771 (4)−0.0028 (3)−0.0543 (2)0.0219 (7)
O80.9101 (5)1.2520 (4)0.2359 (2)0.0262 (8)
H3A0.461 (9)1.076 (8)0.276 (4)0.056 (18)*
U11U22U33U12U13U23
Tb10.01701 (13)0.01146 (12)0.01419 (12)0.00272 (8)0.00639 (8)0.00282 (8)
Ag10.0419 (3)0.0381 (2)0.0290 (2)0.00612 (19)0.01825 (17)0.01948 (17)
O10.049 (2)0.0185 (16)0.0251 (17)0.0037 (16)0.0116 (15)0.0024 (13)
O1W0.033 (2)0.0227 (16)0.0388 (19)0.0149 (15)0.0194 (16)0.0180 (14)
O20.0281 (19)0.0287 (17)0.0241 (16)0.0080 (15)0.0150 (14)0.0039 (13)
O2W0.0241 (19)0.0321 (17)0.0215 (16)0.0081 (15)0.0070 (13)0.0039 (13)
O30.067 (3)0.0275 (19)0.055 (2)0.018 (2)0.035 (2)0.0209 (18)
O40.045 (2)0.0241 (17)0.0375 (19)0.0126 (17)0.0136 (17)0.0024 (15)
O50.0284 (18)0.0129 (14)0.0208 (15)0.0011 (13)0.0096 (13)0.0029 (11)
O90.0192 (17)0.0147 (14)0.0288 (16)0.0013 (13)0.0027 (13)0.0063 (12)
N10.031 (2)0.025 (2)0.0207 (19)0.0084 (17)0.0136 (17)0.0089 (15)
N20.022 (2)0.0199 (18)0.0191 (18)0.0048 (16)0.0083 (15)0.0085 (14)
C10.027 (3)0.019 (2)0.028 (2)0.005 (2)0.011 (2)0.0102 (18)
C20.019 (2)0.023 (2)0.016 (2)0.0047 (19)0.0063 (17)0.0045 (17)
C30.020 (2)0.023 (2)0.020 (2)0.0026 (19)0.0065 (18)0.0074 (17)
C40.016 (2)0.017 (2)0.027 (2)0.0037 (18)0.0038 (18)0.0054 (17)
C50.022 (3)0.025 (2)0.017 (2)0.0078 (19)0.0061 (18)0.0011 (17)
C60.027 (3)0.022 (2)0.017 (2)0.008 (2)0.0038 (19)0.0046 (17)
C70.019 (3)0.026 (2)0.028 (2)0.003 (2)0.0013 (19)0.008 (2)
C80.015 (2)0.017 (2)0.018 (2)0.0021 (17)0.0017 (17)0.0056 (16)
C90.019 (2)0.018 (2)0.014 (2)0.0030 (18)0.0041 (17)0.0033 (16)
C100.020 (2)0.016 (2)0.016 (2)0.0018 (18)0.0057 (17)0.0056 (16)
C110.018 (2)0.018 (2)0.015 (2)0.0034 (18)0.0038 (17)0.0042 (16)
C120.023 (3)0.023 (2)0.015 (2)0.0060 (19)0.0040 (18)0.0027 (17)
C130.017 (2)0.016 (2)0.0119 (19)0.0015 (17)0.0021 (16)0.0009 (16)
C150.021 (2)0.015 (2)0.014 (2)0.0039 (19)0.0058 (17)0.0000 (16)
O60.0315 (19)0.0181 (15)0.0161 (14)0.0030 (14)0.0113 (13)0.0034 (12)
C140.025 (3)0.017 (2)0.019 (2)0.0035 (19)0.0048 (18)0.0037 (17)
O70.058 (3)0.0231 (17)0.0228 (17)0.0110 (17)0.0220 (16)0.0011 (13)
O100.0198 (18)0.0157 (14)0.0303 (16)0.0015 (13)0.0053 (13)0.0041 (12)
O80.045 (2)0.0196 (15)0.0179 (15)0.0103 (15)0.0109 (14)0.0071 (12)
Tb1—O22.346 (3)N2—C81.352 (5)
Tb1—O52.364 (3)N2—C121.351 (5)
Tb1—O6i2.365 (3)N2—Ag1iv2.162 (4)
Tb1—O8ii2.317 (3)C1—C21.388 (6)
Tb1—O92.444 (3)C1—H10.9300
Tb1—O10iii2.401 (3)C2—C31.382 (6)
Tb1—O1W2.421 (3)C2—C61.494 (6)
Tb1—O2W2.468 (3)C3—C41.388 (6)
Ag1—N12.172 (4)C3—H30.9300
Ag1—N2iv2.162 (4)C4—C51.386 (6)
Ag1—O7v2.772 (3)C4—C71.508 (6)
Ag1—O7vi2.859 (3)C5—H50.9300
Ag1—Ag1vii3.2867 (12)C8—C91.381 (6)
O1—C61.260 (5)C8—H80.9300
O1W—H1W0.8401C9—C101.400 (6)
O1W—H2W0.8400C9—C131.500 (6)
O2—C61.263 (6)C10—C111.391 (6)
O2W—H3W0.8402C10—H100.9300
O2W—H4W0.8400C11—C121.388 (6)
O3—C71.309 (6)C11—C141.522 (6)
O3—H3A0.90 (6)C12—H120.9300
O4—C71.207 (5)C13—O61.241 (5)
O5—C131.273 (5)C15—O101.260 (5)
O9—C151.244 (5)C15—C15iii1.535 (8)
N1—C51.343 (6)C14—O71.244 (5)
N1—C11.348 (5)C14—O81.262 (5)
O8ii—Tb1—O275.61 (11)C8—N2—Ag1iv114.8 (3)
O8ii—Tb1—O6i141.96 (11)C12—N2—Ag1iv127.0 (3)
O2—Tb1—O6i142.34 (10)N1—C1—C2122.6 (4)
O8ii—Tb1—O582.16 (11)N1—C1—H1118.7
O2—Tb1—O596.02 (11)C2—C1—H1118.7
O6i—Tb1—O589.03 (10)C3—C2—C1118.6 (4)
O8ii—Tb1—O10iii81.37 (10)C3—C2—C6120.7 (4)
O2—Tb1—O10iii109.81 (11)C1—C2—C6120.7 (4)
O6i—Tb1—O10iii85.00 (10)C2—C3—C4119.1 (4)
O5—Tb1—O10iii144.60 (10)C2—C3—H3120.5
O8ii—Tb1—O1W135.70 (10)C4—C3—H3120.5
O2—Tb1—O1W71.23 (11)C5—C4—C3119.0 (4)
O6i—Tb1—O1W74.71 (10)C5—C4—C7120.2 (4)
O5—Tb1—O1W73.14 (11)C3—C4—C7120.6 (4)
O10iii—Tb1—O1W137.38 (11)N1—C5—C4122.3 (4)
O8ii—Tb1—O9125.23 (12)N1—C5—H5118.9
O2—Tb1—O975.56 (11)C4—C5—H5118.9
O6i—Tb1—O979.71 (11)O1—C6—O2124.7 (4)
O5—Tb1—O9146.28 (10)O1—C6—C2118.4 (4)
O10iii—Tb1—O966.38 (9)O2—C6—C2116.9 (4)
O1W—Tb1—O973.25 (11)O4—C7—O3126.2 (4)
O8ii—Tb1—O2W73.67 (11)O4—C7—C4124.1 (4)
O2—Tb1—O2W147.82 (10)O3—C7—C4109.6 (4)
O6i—Tb1—O2W68.50 (10)N2—C8—C9122.3 (4)
O5—Tb1—O2W70.60 (11)N2—C8—H8118.8
O10iii—Tb1—O2W74.76 (11)C9—C8—H8118.8
O1W—Tb1—O2W127.82 (11)C8—C9—C10118.9 (4)
O9—Tb1—O2W131.32 (10)C8—C9—C13120.7 (4)
N2iv—Ag1—N1164.83 (14)C10—C9—C13120.4 (4)
N2iv—Ag1—Ag1vii108.80 (10)C11—C10—C9119.4 (4)
N1—Ag1—Ag1vii86.10 (10)C11—C10—H10120.3
N2iv—Ag1—O7v93.85 (11)C9—C10—H10120.3
N1—Ag1—O7v92.40 (13)C12—C11—C10117.9 (4)
N1—Ag1—O7vi83.19 (11)C12—C11—C14122.0 (4)
N2iv—Ag1—O7vi107.77 (11)C10—C11—C14120.1 (4)
O7v—Ag1—O7vi108.60 (9)N2—C12—C11123.2 (4)
Tb1—O1W—H1W113.8N2—C12—H12118.4
Tb1—O1W—H2W134.5C11—C12—H12118.4
H1W—O1W—H2W111.6O6—C13—O5124.4 (4)
C6—O2—Tb1129.6 (3)O6—C13—C9118.5 (3)
Tb1—O2W—H3W114.5O5—C13—C9117.1 (4)
Tb1—O2W—H4W131.1O9—C15—O10126.9 (4)
H3W—O2W—H4W111.7O9—C15—C15iii117.3 (5)
C7—O3—H3A113 (4)O10—C15—C15iii115.7 (4)
C13—O5—Tb1133.9 (3)C13—O6—Tb1i137.7 (3)
C15—O9—Tb1118.8 (3)O7—C14—O8126.2 (4)
C5—N1—C1118.3 (4)O7—C14—C11118.2 (4)
C5—N1—Ag1125.6 (3)O8—C14—C11115.6 (4)
C1—N1—Ag1116.1 (3)C15—O10—Tb1iii120.5 (2)
C8—N2—C12118.2 (4)C14—O8—Tb1viii155.4 (3)
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O5i0.842.082.820 (5)147
O1W—H1W···O2Wi0.842.553.221 (5)138
O1W—H2W···O9ix0.842.052.855 (4)159
O2W—H3W···O10x0.842.132.839 (4)142
O2W—H4W···O1x0.842.042.873 (5)173
O3—H3A···O1viii0.90 (6)1.71 (7)2.554 (5)154 (6)
C10—H10···O2Wviii0.932.403.314 (6)169
Table 1

Selected bond lengths (Å)

Tb1—O22.346 (3)
Tb1—O52.364 (3)
Tb1—O6i2.365 (3)
Tb1—O8ii2.317 (3)
Tb1—O92.444 (3)
Tb1—O10iii2.401 (3)
Tb1—O1W2.421 (3)
Tb1—O2W2.468 (3)
Ag1—N12.172 (4)
Ag1—N2iv2.162 (4)
Ag1—O7v2.772 (3)
Ag1—O7vi2.859 (3)

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

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1W⋯O5i0.842.082.820 (5)147
O1W—H1W⋯O2Wi0.842.553.221 (5)138
O1W—H2W⋯O9vii0.842.052.855 (4)159
O2W—H3W⋯O10viii0.842.132.839 (4)142
O2W—H4W⋯O1viii0.842.042.873 (5)173
O3—H3A⋯O1ix0.90 (6)1.71 (7)2.554 (5)154 (6)
C10—H10⋯O2Wix0.932.403.314 (6)169

Symmetry codes: (i) ; (vii) ; (viii) ; (ix) .

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