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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 12| December 2010| Pages m1566-m1567
https://doi.org/10.1107/S1600536810046143

Tetra­aqua­di­azido­cobalt(II) 3,3′-dicarb­­oxy­l­ato-1,1′-ethyl­enedipyridinium

Yan-Qing Wen,a Chun-Yan Tiana and En-Qing Gaoa*

aShanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, East China Normal University, Shanghai 200062, People's Republic of China
*Correspondence e-mail: eqgao@chem.ecnu.edu.cn

(Received 21 October 2010; accepted 9 November 2010; online 13 November 2010)

The asymmetric unit of the title compound, [Co(N3)2(H2O)4]·C14H12N2O4, comprises half of the cobalt(II) complex mol­ecule and a half of the 3,3′-dicarboxyl­ato-1,1′-ethyl­enedipyridinium mol­ecule. The CoII atom is located on an inversion centre and hence the complex mol­ecule adopts a centrosymmetric trans-octa­hedral geometry. The zwitterionic organic mol­ecule is also centrosymmetric with the centre of the C—C bond of the ethyl­ene moiety coinciding with an inversion centre. The adduct of metal complex and organic mol­ecule is associated into a three-dimenional network through O—H⋯O hydrogen bonds.

Related literature

For background to hydrogen bonds, see: Braga & Grepioni (2000[Braga, D. & Grepioni, F. (2000). Acc. Chem. Res. 33, 601-608.]); Fabbiani et al. (2010[Fabbiani, P. A. F., Levendis, C. D., Buth, G., Kuhs, F. W., Shanklandd, N. & Sowa, H. (2010). CrystEngComm, 12, 2354-2360.]); Salitros et al. (2010[Salitros, I., Pavlik, J., Boca, R., Fuhr, O., Rajaduraia, C. & Ruben, M. (2010). CrystEngComm, 12, 2361-2368.]); Schultheis et al. (2010[Schultheis, N., Bethune, S. & Henck, J. O. (2010). CrystEngComm, 12, 2436-2442.]). For the synthesis of the ligand, see: Loeb et al. (2006[Loeb, S. J., Tiburcio, J., Vella, S. J. & Wisner, J. A. (2006). Org. Biomol. Chem. 4, 667-680.]). For hydrogen-bond motifs, see: Bernstein et al. (1995[Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N. L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555-1573.]); Etter (1990[Etter, M. C. (1990). Acc. Chem. Res. 23, 120-126.]).

[Scheme 1]

Experimental

Crystal data

  • [Co(N3)2(H2O)4]·C14H12N2O4

  • Mr = 487.31

  • Triclinic, [P \overline 1]

  • a = 7.4309 (6) Å

  • b = 7.7507 (7) Å

  • c = 8.5582 (7) Å

  • α = 95.463 (2)°

  • β = 90.586 (2)°

  • γ = 95.011 (2)°

  • V = 488.71 (7) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 0.94 mm−1

  • T = 296 K

  • 0.25 × 0.20 × 0.15 mm
Data collection

  • Bruker APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.799, Tmax = 0.872

  • 6091 measured reflections

  • 1907 independent reflections

  • 1889 reflections with I > 2σ(I)

  • Rint = 0.015
Refinement

  • R[F2 > 2σ(F2)] = 0.024

  • wR(F2) = 0.074

  • S = 1.12

  • 1907 reflections

  • 154 parameters

  • 9 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.28 e Å−3

  • Δρmin = −0.28 e Å−3

Table 1
Selected bond lengths (Å)

Co1—O4 2.0780 (12)
Co1—N2 2.0958 (15)
Co1—O3 2.1431 (12)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O3—H3B⋯O1i 0.84 (2) 2.01 (2) 2.8180 (18) 163 (2)
O3—H3C⋯O1ii 0.84 (2) 1.91 (2) 2.7395 (17) 172 (2)
O4—H4C⋯O2iii 0.86 (2) 1.84 (2) 2.6901 (18) 173 (3)
O4—H4B⋯O2 0.81 (2) 2.03 (2) 2.8028 (18) 159 (2)
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x, y-1, z; (iii) -x, -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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810046143/kp2284sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810046143/kp2284Isup2.hkl

checkCIF report


Comment top

Hydrogen bonds play a key role in biological systems and materials, and they have been widely used as a putative supramolecular tool for engineering organic and metal-organic solids (Fabbiani et al., 2010; Salitros et al., 2010; Schultheis et al., 2010; Braga & Grepioni, 2000). In this paper, we report the structure of the title compound, (I), which contains a neutral metal complex molecule, [Co(N3)2(H2O)4], and a zwitterionic dicarboxylate, 1,2-bis(3-carboxylatopyridinium)ethane (Fig. 1). The metal complex molecule is centrosymmetric, with the octahedral-coordinated CoII by two azide anions and four water molecules in a trans arrangement (Fig. 1, Table 1). Two opposite Co—O distances are longer than the Co—N and other Co—O ones, defining an axially elongated geometry. The zwitterionic molecule is also centrosymmetric (Fig.1 ). The inorganic complex molecules and the carboxylate groups are associated into a sheet through O—H···O hydrogen bonds involving the coordinated aqua ligands (O3 and O4) and the carboxylate oxygen atoms (O1 and O2) (Fig. 2, Table 2). The two O4 aqua ligands from symmetry related complex molecules and two O2 atoms from symmetry related organic molecules form a hydrogen-bonded ring which can be denoted by the graph set R42(8) (Bernstein et al., 1995; Etter, 1990). Similar hydrogen-bonded rings are formed by O1 and O3. The carboxylate group forms a R22(8) hydrogen-bonded ring with two aqua ligands from the same complex molecule. Besides, a large hydrogen-bonded ring [R44(16)] is formed by two carboxylate groups and four aqua ligands from two complex molecules. The organic ligands interlink the hydrogen-bonded sheets of the metal complexes into the three-dimensional structure (Fig. 3).

Related literature top

For background to hydrogen bonds, see: Braga & Grepioni (2000); Fabbiani et al. (2010); Salitros et al. (2010); Schultheis et al. (2010). For the synthesis of the ligand, see: Loeb et al. (2006). For hydrogen-bond motifs, see: Bernstein et al. (1995); Etter (1990).

Experimental top

The zwitterionic ligand ([H2L1]Br2) was synthesised from 1,2-dibromoethane and ethyl nicotinate according to the published procedure (Loeb et al., 2006). An aqueous solution (4 mL) of [H2L1]Br2 (0.1 mmol) and NaN3 (1 mmol) was added to a DMF solution (1.5 mL) of Co(ClO4)2.6H2O (0.2 mmol) with stirring. The resulting solution was allowed to evaporate slowly at room temperature, yielding light-red block crystals of (I) in three days. Yield: 75%. Anal. calcd (found) (%) for CoC14H20N8O8: C, 34.79 (34.51); H, 4.39 (4.14); N, 22.87 (23.00). Main IR bands (KBr, ν/cm-1): 3427m, 3097w, 2042 s, 1637 s, 1606 s, 1392m, 765m, 688m.

Refinement top

All hydrogen atoms attached to carbon atoms were placed at calculated positions and refined with the riding model using AFIX 43 and AFIX 23 instructions for aromatic C—H and secondary CH2. The water hydrogen atoms were initially located from difference Fourier maps and refined isotropically with restraints on O—H distance (0.85 Å) and H—O—H angle, and Uiso(H) = 1.5Ueq(O). The 'rigid-bond' restraint was applied on the azide moiety (N2—N3—N4) using the SHELXL DELU instruction.

Structure description top

Hydrogen bonds play a key role in biological systems and materials, and they have been widely used as a putative supramolecular tool for engineering organic and metal-organic solids (Fabbiani et al., 2010; Salitros et al., 2010; Schultheis et al., 2010; Braga & Grepioni, 2000). In this paper, we report the structure of the title compound, (I), which contains a neutral metal complex molecule, [Co(N3)2(H2O)4], and a zwitterionic dicarboxylate, 1,2-bis(3-carboxylatopyridinium)ethane (Fig. 1). The metal complex molecule is centrosymmetric, with the octahedral-coordinated CoII by two azide anions and four water molecules in a trans arrangement (Fig. 1, Table 1). Two opposite Co—O distances are longer than the Co—N and other Co—O ones, defining an axially elongated geometry. The zwitterionic molecule is also centrosymmetric (Fig.1 ). The inorganic complex molecules and the carboxylate groups are associated into a sheet through O—H···O hydrogen bonds involving the coordinated aqua ligands (O3 and O4) and the carboxylate oxygen atoms (O1 and O2) (Fig. 2, Table 2). The two O4 aqua ligands from symmetry related complex molecules and two O2 atoms from symmetry related organic molecules form a hydrogen-bonded ring which can be denoted by the graph set R42(8) (Bernstein et al., 1995; Etter, 1990). Similar hydrogen-bonded rings are formed by O1 and O3. The carboxylate group forms a R22(8) hydrogen-bonded ring with two aqua ligands from the same complex molecule. Besides, a large hydrogen-bonded ring [R44(16)] is formed by two carboxylate groups and four aqua ligands from two complex molecules. The organic ligands interlink the hydrogen-bonded sheets of the metal complexes into the three-dimensional structure (Fig. 3).

For background to hydrogen bonds, see: Braga & Grepioni (2000); Fabbiani et al. (2010); Salitros et al. (2010); Schultheis et al. (2010). For the synthesis of the ligand, see: Loeb et al. (2006). For hydrogen-bond motifs, see: Bernstein et al. (1995); Etter (1990).

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: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry code: (i) -x, -y, 1 - z; (ii) 1 - x, -y, -z].
[Figure 2] Fig. 2. Two-dimensional layer structure connected through intermolecula O—H···O hydrogen bonds. [Symmetry code: (i) -x + 1, -y + 1, -z + 1; (ii) x, y - 1, z; (iii)-x, -y + 1, -z + 1].
[Figure 3] Fig. 3. Three dimensional structure connected by the organic ligands interlinking the hydrogen-bonded sheets.
Tetraaquadiazidocobalt(II) 3,3'-dicarboxylato-1,1'-ethylenedipyridinium top
Crystal data top
[Co(N3)2(H2O)4]·C14H12N2O4Z = 1
Mr = 487.31F(000) = 251
Triclinic, P1Dx = 1.656 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4309 (6) ÅCell parameters from 15377 reflections
b = 7.7507 (7) Åθ = 3.4–27.5°
c = 8.5582 (7) ŵ = 0.94 mm−1
α = 95.463 (2)°T = 296 K
β = 90.586 (2)°Block, red
γ = 95.011 (2)°0.25 × 0.20 × 0.15 mm
V = 488.71 (7) Å3
Data collection top
Bruker APEXII CCD area-detector
diffractometer		1907 independent reflections
Radiation source: fine-focus sealed tube1889 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.015
phi and ω scansθmax = 26.1°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)		h = −9→9
Tmin = 0.799, Tmax = 0.872k = −9→8
6091 measured reflectionsl = −10→10
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)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0411P)2 + 0.2239P]
where P = (Fo2 + 2Fc2)/3
1907 reflections(Δ/σ)max < 0.001
154 parametersΔρmax = 0.28 e Å−3
9 restraintsΔρmin = −0.28 e Å−3
Crystal data top
[Co(N3)2(H2O)4]·C14H12N2O4γ = 95.011 (2)°
Mr = 487.31V = 488.71 (7) Å3
Triclinic, P1Z = 1
a = 7.4309 (6) ÅMo Kα radiation
b = 7.7507 (7) ŵ = 0.94 mm−1
c = 8.5582 (7) ÅT = 296 K
α = 95.463 (2)°0.25 × 0.20 × 0.15 mm
β = 90.586 (2)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		1907 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2008)		1889 reflections with I > 2σ(I)
Tmin = 0.799, Tmax = 0.872Rint = 0.015
6091 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0249 restraints
wR(F2) = 0.074H atoms treated by a mixture of independent and constrained refinement
S = 1.12Δρmax = 0.28 e Å−3
1907 reflectionsΔρmin = −0.28 e Å−3
154 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.00000.00000.50000.02282 (12)
C10.3729 (2)0.5896 (2)0.3420 (2)0.0283 (3)
C20.5025 (2)0.4708 (2)0.26023 (19)0.0258 (3)
C30.6822 (2)0.5278 (2)0.2423 (2)0.0335 (4)
H3A0.72340.64240.27510.040*
C40.4437 (2)0.3011 (2)0.20731 (19)0.0255 (3)
H4A0.32280.26130.21530.031*
C50.8009 (2)0.4148 (3)0.1756 (3)0.0392 (4)
H5A0.92150.45300.16250.047*
C60.7382 (2)0.2466 (2)0.1293 (2)0.0339 (4)
H6A0.81730.16850.08750.041*
C70.5003 (2)0.0111 (2)0.08913 (19)0.0286 (3)
H7A0.3795−0.01770.12650.034*
H7B0.5803−0.06670.13030.034*
N10.56206 (18)0.19334 (17)0.14405 (16)0.0257 (3)
N20.0817 (2)−0.0222 (2)0.26583 (18)0.0399 (4)
N3−0.0146 (2)−0.1006 (2)0.16704 (17)0.0320 (3)
N4−0.1073 (3)−0.1740 (2)0.0672 (2)0.0461 (4)
O10.43867 (18)0.73681 (16)0.39597 (19)0.0435 (4)
O20.21281 (17)0.52889 (16)0.35044 (18)0.0405 (3)
O30.27781 (16)−0.00456 (16)0.56790 (15)0.0319 (3)
H3B0.347 (3)0.086 (2)0.569 (3)0.048*
H3C0.321 (3)−0.082 (2)0.508 (3)0.048*
O40.02796 (18)0.26995 (16)0.50991 (18)0.0379 (3)
H4B0.090 (3)0.323 (3)0.449 (3)0.057*
H4C−0.053 (3)0.334 (3)0.547 (3)0.057*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02008 (17)0.02004 (17)0.02747 (17)−0.00003 (11)0.00302 (11)−0.00082 (11)
C10.0273 (8)0.0202 (7)0.0363 (8)0.0007 (6)0.0062 (7)−0.0031 (6)
C20.0247 (8)0.0210 (7)0.0305 (8)0.0009 (6)0.0035 (6)−0.0024 (6)
C30.0282 (9)0.0247 (8)0.0445 (10)−0.0047 (7)0.0040 (7)−0.0067 (7)
C40.0220 (7)0.0230 (8)0.0301 (8)0.0002 (6)0.0040 (6)−0.0026 (6)
C50.0231 (8)0.0348 (9)0.0565 (12)−0.0035 (7)0.0081 (8)−0.0077 (8)
C60.0247 (8)0.0311 (9)0.0447 (10)0.0045 (7)0.0068 (7)−0.0056 (7)
C70.0331 (8)0.0179 (7)0.0336 (9)0.0000 (6)0.0054 (7)−0.0030 (6)
N10.0256 (7)0.0203 (6)0.0297 (7)0.0006 (5)0.0035 (5)−0.0043 (5)
N20.0335 (8)0.0555 (10)0.0297 (8)−0.0006 (7)0.0064 (6)0.0028 (7)
N30.0314 (8)0.0343 (8)0.0318 (8)0.0069 (6)0.0117 (7)0.0059 (6)
N40.0475 (10)0.0485 (10)0.0398 (9)−0.0053 (8)0.0032 (8)−0.0011 (8)
O10.0330 (7)0.0226 (6)0.0701 (10)−0.0026 (5)0.0105 (6)−0.0159 (6)
O20.0282 (6)0.0241 (6)0.0665 (9)−0.0017 (5)0.0160 (6)−0.0082 (6)
O30.0230 (6)0.0274 (6)0.0434 (7)0.0016 (5)0.0014 (5)−0.0067 (5)
O40.0356 (7)0.0210 (6)0.0575 (8)0.0026 (5)0.0178 (6)0.0028 (5)
Geometric parameters (Å, º) top
Co1—O42.0780 (12)C5—C61.366 (3)
Co1—O4i2.0780 (12)C5—H5A0.9300
Co1—N22.0958 (15)C6—N11.349 (2)
Co1—N2i2.0958 (15)C6—H6A0.9300
Co1—O3i2.1431 (12)C7—N11.478 (2)
Co1—O32.1431 (12)C7—C7ii1.519 (3)
C1—O11.245 (2)C7—H7A0.9700
C1—O21.246 (2)C7—H7B0.9700
C1—C21.521 (2)N2—N31.188 (2)
C2—C41.381 (2)N3—N41.164 (2)
C2—C31.384 (2)O3—H3B0.836 (15)
C3—C51.386 (3)O3—H3C0.839 (15)
C3—H3A0.9300O4—H4B0.813 (16)
C4—N11.348 (2)O4—H4C0.856 (16)
C4—H4A0.9300
O4—Co1—O4i180.0N1—C4—H4A120.1
O4—Co1—N291.41 (6)C2—C4—H4A120.1
O4i—Co1—N288.59 (6)C6—C5—C3119.02 (16)
O4—Co1—N2i88.59 (6)C6—C5—H5A120.5
O4i—Co1—N2i91.41 (6)C3—C5—H5A120.5
N2—Co1—N2i180.0N1—C6—C5120.23 (16)
O4—Co1—O3i88.83 (5)N1—C6—H6A119.9
O4i—Co1—O3i91.17 (5)C5—C6—H6A119.9
N2—Co1—O3i92.17 (6)N1—C7—C7ii109.09 (16)
N2i—Co1—O3i87.83 (6)N1—C7—H7A109.9
O4—Co1—O391.17 (5)C7ii—C7—H7A109.9
O4i—Co1—O388.83 (5)N1—C7—H7B109.9
N2—Co1—O387.83 (6)C7ii—C7—H7B109.9
N2i—Co1—O392.17 (6)H7A—C7—H7B108.3
O3i—Co1—O3180.0C4—N1—C6121.82 (14)
O1—C1—O2126.73 (15)C4—N1—C7120.05 (13)
O1—C1—C2116.50 (14)C6—N1—C7118.13 (14)
O2—C1—C2116.75 (14)N3—N2—Co1120.05 (12)
C4—C2—C3118.77 (14)N4—N3—N2178.01 (19)
C4—C2—C1120.22 (14)Co1—O3—H3B119.4 (17)
C3—C2—C1120.97 (14)Co1—O3—H3C107.1 (17)
C2—C3—C5120.26 (16)H3B—O3—H3C108.0 (19)
C2—C3—H3A119.9Co1—O4—H4B122.9 (18)
C5—C3—H3A119.9Co1—O4—H4C123.1 (17)
N1—C4—C2119.85 (14)H4B—O4—H4C109 (2)
O1—C1—C2—C4175.22 (17)C2—C4—N1—C6−0.5 (3)
O2—C1—C2—C4−3.6 (2)C2—C4—N1—C7179.21 (14)
O1—C1—C2—C3−2.5 (3)C5—C6—N1—C4−1.6 (3)
O2—C1—C2—C3178.67 (17)C5—C6—N1—C7178.70 (17)
C4—C2—C3—C5−1.5 (3)C7ii—C7—N1—C4108.4 (2)
C1—C2—C3—C5176.28 (18)C7ii—C7—N1—C6−71.9 (2)
C3—C2—C4—N12.0 (2)O4—Co1—N2—N3−122.40 (16)
C1—C2—C4—N1−175.75 (15)O4i—Co1—N2—N357.60 (16)
C2—C3—C5—C6−0.6 (3)O3i—Co1—N2—N3−33.51 (16)
C3—C5—C6—N12.1 (3)O3—Co1—N2—N3146.49 (16)
Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3B···O1iii0.84 (2)2.01 (2)2.8180 (18)163 (2)
O3—H3C···O1iv0.84 (2)1.91 (2)2.7395 (17)172 (2)
O4—H4C···O2v0.86 (2)1.84 (2)2.6901 (18)173 (3)
O4—H4B···O20.81 (2)2.03 (2)2.8028 (18)159 (2)
Symmetry codes: (iii) −x+1, −y+1, −z+1; (iv) x, y−1, z; (v) −x, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula[Co(N3)2(H2O)4]·C14H12N2O4
Mr487.31
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)7.4309 (6), 7.7507 (7), 8.5582 (7)
α, β, γ (°)95.463 (2), 90.586 (2), 95.011 (2)
V (Å3)488.71 (7)
Z1
Radiation typeMo Kα
µ (mm−1)0.94
Crystal size (mm)0.25 × 0.20 × 0.15
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2008)
Tmin, Tmax0.799, 0.872
No. of measured, independent and
observed [I > 2σ(I)] reflections		6091, 1907, 1889
Rint0.015
(sin θ/λ)max (Å−1)0.619
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.074, 1.12
No. of reflections1907
No. of parameters154
No. of restraints9
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.28, −0.28

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

Selected bond lengths (Å) top
Co1—O42.0780 (12)Co1—O32.1431 (12)
Co1—N22.0958 (15)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3B···O1i0.836 (15)2.007 (17)2.8180 (18)163 (2)
O3—H3C···O1ii0.839 (15)1.906 (16)2.7395 (17)172 (2)
O4—H4C···O2iii0.856 (16)1.839 (16)2.6901 (18)173 (3)
O4—H4B···O20.813 (16)2.030 (19)2.8028 (18)159 (2)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y−1, z; (iii) −x, −y+1, −z+1.
 

Acknowledgements

We are thankful for financial support from the Shanghai Leading Academic Discipline Project (B409).

References

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ISSN: 2056-9890
Volume 66| Part 12| December 2010| Pages m1566-m1567
https://doi.org/10.1107/S1600536810046143
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