Literature DB >> 21583755

catena-Poly[[(2,2'-bipyridine-κN,N')cobalt(II)]-μ-oxalato-κO,O:O,O].

Pei-Zhou Li1, Qiang Xu.   

Abstract

In the one-dimensional title coordination polymer, [Co(C(2)O(4))(C(10)H(8)N(2))](n), the Co(II) atom is coordinated in a distorted octa-hedral geometry by two N atoms from one 2,2'-bipyridine ligand and four O atoms belonging to two chelating oxalate ligands. Two neighboring Co centers are bridged by an oxalate ligand, forming a one-dimensional chain structure.

Entities:  

Year:  2009        PMID： 21583755      PMCID： PMC2977569          DOI： 10.1107/S1600536809012690

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


Related literature

For general background to metal–oxalate compounds, see: Coronado et al. (2001 ▶); Decurtins et al. (1994 ▶). For related structures, see: Fun et al. (1999 ▶); Lin et al. (2006 ▶).

Experimental

Crystal data

[Co(C2O4)(C10H8N2)] M = 303.13 Orthorhombic, a = 9.2333 (18) Å b = 9.2163 (18) Å c = 14.101 (3) Å V = 1199.9 (4) Å3 Z = 4 Mo Kα radiation μ = 1.44 mm−1 T = 293 K 0.16 × 0.14 × 0.08 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.800, T max = 0.892 10848 measured reflections 2692 independent reflections 1887 reflections with I > 2σ(I) R int = 0.064

Refinement

R[F 2 > 2σ(F 2)] = 0.052 wR(F 2) = 0.136 S = 1.09 2692 reflections 172 parameters 1 restraint H-atom parameters constrained Δρmax = 0.38 e Å−3 Δρmin = −0.90 e Å−3 Absolute structure: Flack (1983 ▶); 1283 Friedel pairs Flack parameter: 0.03 (4) Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶) and ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: publCIF (Westrip, 2009 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809012690/hy2191sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809012690/hy2191Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C2O4)(C10H8N2)]F(000) = 612
Mr = 303.13Dx = 1.678 Mg m−3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 2143 reflections
a = 9.2333 (18) Åθ = 3.4–26.5°
b = 9.2163 (18) ŵ = 1.44 mm−1
c = 14.101 (3) ÅT = 293 K
V = 1199.9 (4) Å3Plate, brown
Z = 40.16 × 0.14 × 0.08 mm
Rigaku R-AXIS RAPID diffractometer2692 independent reflections
Radiation source: rotating anode1887 reflections with I > 2σ(I)
graphiteRint = 0.064
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −10→11
Tmin = 0.800, Tmax = 0.892k = −11→11
10848 measured reflectionsl = −18→18
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.052H-atom parameters constrained
wR(F2) = 0.136w = 1/[σ2(Fo2) + (0.0501P)2 + 1.1682P] where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
2692 reflectionsΔρmax = 0.38 e Å−3
172 parametersΔρmin = −0.89 e Å−3
1 restraintAbsolute structure: Flack (1983); 1283 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.03 (4)
xyzUiso*/Ueq
O20.5044 (5)1.2574 (5)0.3939 (3)0.0580 (13)
O40.4266 (4)1.3874 (4)0.2309 (3)0.0507 (10)
C120.3425 (7)1.2932 (7)0.2640 (4)0.0463 (14)
Co10.11792 (7)1.08924 (7)0.30925 (11)0.0484 (2)
C110.3876 (6)1.2177 (7)0.3569 (4)0.0441 (13)
O10.3038 (5)1.1224 (4)0.3891 (3)0.0504 (10)
O30.2237 (5)1.2560 (5)0.2294 (3)0.0543 (12)
C50.1633 (8)0.7791 (7)0.2550 (5)0.0494 (15)
C60.0832 (8)0.7718 (7)0.3458 (5)0.0519 (16)
N10.1983 (6)0.9123 (6)0.2254 (4)0.0482 (12)
N20.0502 (6)0.9010 (5)0.3861 (4)0.0485 (12)
C10.2749 (8)0.9265 (8)0.1462 (5)0.0628 (18)
H10.30121.01890.12620.075*
C10−0.0191 (8)0.9026 (8)0.4686 (5)0.0630 (17)
H10−0.04020.99160.49640.076*
C40.2031 (9)0.6552 (8)0.2047 (6)0.066 (2)
H40.17760.56340.22640.079*
C9−0.0611 (9)0.7770 (9)0.5146 (5)0.074 (2)
H9−0.10830.78190.57280.088*
C70.0401 (9)0.6451 (8)0.3887 (6)0.069 (2)
H70.06040.55690.35960.083*
C20.3166 (9)0.8083 (11)0.0928 (6)0.078 (2)
H20.36860.82090.03690.094*
C8−0.0327 (10)0.6461 (9)0.4741 (6)0.078 (2)
H8−0.06150.56010.50310.094*
C30.2799 (10)0.6717 (9)0.1236 (6)0.080 (2)
H30.30770.59070.08880.096*
U11U22U33U12U13U23
O20.058 (3)0.056 (3)0.060 (3)−0.010 (2)−0.018 (3)0.017 (2)
O40.057 (2)0.046 (2)0.049 (2)−0.0021 (19)−0.005 (2)0.0123 (19)
C120.059 (3)0.035 (3)0.045 (3)0.008 (3)−0.003 (3)0.002 (3)
Co10.0518 (4)0.0394 (3)0.0541 (4)0.0005 (4)−0.0009 (5)−0.0032 (5)
C110.058 (4)0.034 (3)0.040 (3)0.004 (3)−0.007 (3)0.001 (2)
O10.060 (2)0.043 (2)0.048 (2)−0.0009 (19)−0.007 (2)0.0121 (19)
O30.058 (3)0.055 (3)0.050 (3)−0.009 (2)−0.014 (2)0.009 (2)
C50.054 (3)0.040 (3)0.054 (4)0.007 (3)−0.004 (4)0.000 (3)
C60.066 (4)0.038 (3)0.052 (4)−0.007 (3)−0.015 (4)0.005 (3)
N10.057 (3)0.044 (3)0.044 (3)0.006 (2)0.005 (2)−0.003 (2)
N20.053 (3)0.046 (3)0.046 (3)−0.002 (2)0.007 (3)−0.003 (2)
C10.073 (4)0.064 (4)0.051 (4)0.009 (4)0.011 (4)−0.001 (3)
C100.073 (4)0.054 (4)0.062 (4)−0.011 (3)0.006 (4)−0.006 (3)
C40.080 (5)0.046 (4)0.073 (5)0.008 (3)−0.003 (4)−0.013 (3)
C90.089 (5)0.082 (5)0.050 (4)−0.023 (4)0.013 (4)0.004 (4)
C70.086 (5)0.051 (4)0.070 (5)−0.013 (4)0.006 (4)−0.007 (4)
C20.083 (5)0.090 (6)0.062 (5)0.015 (5)0.022 (5)−0.010 (4)
C80.102 (6)0.062 (5)0.071 (5)−0.023 (4)0.000 (5)0.009 (4)
C30.094 (6)0.063 (5)0.082 (6)0.027 (4)0.006 (5)−0.024 (4)
O2—C111.252 (7)C6—C71.374 (10)
O2—Co1i2.126 (4)N1—C11.328 (8)
O4—C121.254 (7)N2—C101.327 (9)
O4—Co1i2.095 (4)C1—C21.379 (10)
C12—O31.248 (7)C1—H10.9300
C12—C111.541 (6)C10—C91.383 (10)
Co1—O12.076 (4)C10—H100.9300
Co1—O4ii2.095 (4)C4—C31.355 (12)
Co1—O2ii2.126 (4)C4—H40.9300
Co1—N22.139 (5)C9—C81.360 (11)
Co1—O32.142 (4)C9—H90.9300
Co1—N12.146 (5)C7—C81.379 (11)
C11—O11.256 (7)C7—H70.9300
C5—N11.336 (8)C2—C31.375 (12)
C5—C41.393 (10)C2—H20.9300
C5—C61.480 (8)C8—H80.9300
C6—N21.354 (8)C3—H30.9300
C11—O2—Co1i112.6 (4)C1—N1—C5118.7 (6)
C12—O4—Co1i113.4 (4)C1—N1—Co1124.9 (5)
O3—C12—O4126.0 (6)C5—N1—Co1116.3 (4)
O3—C12—C11116.5 (5)C10—N2—C6119.1 (6)
O4—C12—C11117.5 (5)C10—N2—Co1125.1 (5)
O1—Co1—O4ii165.57 (14)C6—N2—Co1115.8 (4)
O1—Co1—O2ii90.30 (17)N1—C1—C2122.1 (7)
O4ii—Co1—O2ii79.14 (16)N1—C1—H1119.0
O1—Co1—N294.94 (18)C2—C1—H1119.0
O4ii—Co1—N295.99 (19)N2—C10—C9122.5 (7)
O2ii—Co1—N296.4 (2)N2—C10—H10118.8
O1—Co1—O378.61 (16)C9—C10—H10118.8
O4ii—Co1—O391.91 (17)C3—C4—C5118.4 (7)
O2ii—Co1—O392.47 (16)C3—C4—H4120.8
N2—Co1—O3169.12 (18)C5—C4—H4120.8
O1—Co1—N197.18 (19)C8—C9—C10119.4 (8)
O4ii—Co1—N194.55 (18)C8—C9—H9120.3
O2ii—Co1—N1169.92 (18)C10—C9—H9120.3
N2—Co1—N176.34 (17)C6—C7—C8121.3 (8)
O3—Co1—N195.6 (2)C6—C7—H7119.3
O2—C11—O1125.7 (6)C8—C7—H7119.3
O2—C11—C12117.1 (5)C3—C2—C1118.8 (8)
O1—C11—C12117.2 (5)C3—C2—H2120.6
C11—O1—Co1114.6 (4)C1—C2—H2120.6
C12—O3—Co1113.1 (4)C9—C8—C7117.8 (7)
N1—C5—C4122.0 (7)C9—C8—H8121.1
N1—C5—C6115.6 (6)C7—C8—H8121.1
C4—C5—C6122.3 (7)C4—C3—C2119.9 (7)
N2—C6—C7119.8 (7)C4—C3—H3120.1
N2—C6—C5115.8 (6)C2—C3—H3120.1
C7—C6—C5124.3 (7)
Co1i—O4—C12—O3−178.1 (5)O3—Co1—N1—C1−5.9 (6)
Co1i—O4—C12—C113.1 (6)O1—Co1—N1—C597.1 (5)
Co1i—O2—C11—O1175.8 (5)O4ii—Co1—N1—C5−91.3 (5)
Co1i—O2—C11—C12−4.6 (6)O2ii—Co1—N1—C5−40.5 (14)
O3—C12—C11—O2−177.8 (7)N2—Co1—N1—C53.7 (5)
O4—C12—C11—O21.1 (7)O3—Co1—N1—C5176.3 (5)
O3—C12—C11—O11.8 (7)C7—C6—N2—C102.4 (10)
O4—C12—C11—O1−179.2 (6)C5—C6—N2—C10−178.7 (5)
O2—C11—O1—Co1178.8 (5)C7—C6—N2—Co1−178.0 (6)
C12—C11—O1—Co1−0.8 (6)C5—C6—N2—Co10.9 (7)
O4ii—Co1—O1—C11−49.8 (10)O1—Co1—N2—C1081.0 (6)
O2ii—Co1—O1—C11−92.5 (4)O4ii—Co1—N2—C10−89.6 (5)
N2—Co1—O1—C11171.1 (4)O2ii—Co1—N2—C10−9.9 (6)
O3—Co1—O1—C110.0 (4)O3—Co1—N2—C10134.1 (10)
N1—Co1—O1—C1194.3 (4)N1—Co1—N2—C10177.2 (5)
O4—C12—O3—Co1179.4 (5)O1—Co1—N2—C6−98.6 (5)
C11—C12—O3—Co1−1.8 (6)O4ii—Co1—N2—C690.9 (5)
O1—Co1—O3—C121.1 (4)O2ii—Co1—N2—C6170.6 (5)
O4ii—Co1—O3—C12170.1 (4)O3—Co1—N2—C6−45.5 (13)
O2ii—Co1—O3—C1290.9 (4)N1—Co1—N2—C6−2.4 (5)
N2—Co1—O3—C12−53.3 (13)C5—N1—C1—C21.4 (11)
N1—Co1—O3—C12−95.1 (5)Co1—N1—C1—C2−176.3 (6)
N1—C5—C6—N22.4 (7)C6—N2—C10—C9−1.0 (10)
C4—C5—C6—N2−179.2 (8)Co1—N2—C10—C9179.5 (6)
N1—C5—C6—C7−178.8 (8)N1—C5—C4—C30.2 (11)
C4—C5—C6—C7−0.3 (9)C6—C5—C4—C3−178.2 (7)
C4—C5—N1—C1−0.9 (10)N2—C10—C9—C8−0.9 (12)
C6—C5—N1—C1177.6 (6)N2—C6—C7—C8−2.1 (12)
C4—C5—N1—Co1177.1 (5)C5—C6—C7—C8179.1 (7)
C6—C5—N1—Co1−4.5 (7)N1—C1—C2—C3−1.3 (12)
O1—Co1—N1—C1−85.1 (6)C10—C9—C8—C71.2 (13)
O4ii—Co1—N1—C186.5 (6)C6—C7—C8—C90.2 (13)
O2ii—Co1—N1—C1137.3 (11)C5—C4—C3—C20.0 (12)
N2—Co1—N1—C1−178.4 (6)C1—C2—C3—C40.5 (13)
Table 1

Selected bond lengths (Å)

Co1—O12.076 (4)
Co1—O4i2.095 (4)
Co1—O2i2.126 (4)
Co1—N22.139 (5)
Co1—O32.142 (4)
Co1—N12.146 (5)

Symmetry code: (i) .

  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.  Molecule-based magnets formed by bimetallic three-dimensional oxalate networks and chiral tris(bipyridyl) complex cations. The series [ZII(bpy)3][ClO4][MIICrIII(ox)3] (ZII = Ru, Fe, Co, and Ni; MII = Mn, Fe, Co, Ni, Cu, and Zn; ox = oxalate dianion).

Authors:  E Coronado; J R Galán-Mascarós; C J Gómez-García; J M Martínez-Agudo
Journal:  Inorg Chem       Date:  2001-01-01       Impact factor: 5.165

3.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  3 in total
  2 in total

1.  (μ-Oxalato-κO,O:O,O)bis-[bis-(2,2'-bipyridine-κN,N')cobalt(II)] μ(6)-oxido-dodeca-μ(2)-oxido-hexa-oxido-hexa-tungstate(VI).

Authors:  Congwen Shi; Liming Fan; Peihai Wei; Bin Li; Xiutang Zhang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-06-18

2.  Tris(2,2'-bipyridine)-cobalt(II) μ(6)-oxido-dodeca-μ(2)-oxido-hexa-oxidohexa-molydate(VI).

Authors:  Ying Liu; Xianxi Zhang; Zechun Xue; Jian Sheng
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-06-05
  2 in total

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