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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 69| Part 7| July 2013| Page m371
https://doi.org/10.1107/S1600536813015262

Poly[[di­aqua­tris­(μ2-4,4′-bi­pyridine)­bis­[μ2-2-(carb­oxylato­methyl­sulfan­yl)nicotinato]dicobalt(II)] 1.3-hydrate]

Rui-Qin Li,a Xiao-Juan Wanga and Yun-Long Fenga*

aZhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, College of Chemistry and Life Science, Zhejiang Normal University, Jinhua, Zhejiang 321004, People's Republic of China
*Correspondence e-mail: sky37@zjnu.cn

(Received 15 May 2013; accepted 2 June 2013; online 8 June 2013)

The title complex, [Co2(C8H5NO4S)2(C10H8N2)3(H2O)2]·1.3H2O, was synthesized under hydro­thermal conditions. The CoII ion is six-coordinated in a slightly distorted octa­hedral environment resulting from two carboxyl­ate O atoms of two 2-carb­oxy­methyl­sulfanyl nicotinate (2-CMSN2−) anions, one water mol­ecule and three N atoms of three 4,4′-bi­pyridine ligands, with one 4,4′-bi­pyridine ligand situated on a centre of inversion. Two neighboring CoII ions are linked by two anions, giving a dinuclear [Co2(2-CMSN)2] subunit with a Co⋯Co separation of 6.8600 (3) Å. The dinuclear subunits are joined by bridging 4,4′-bi­pyridine linkers, generating a three-dimensional network structure. Disordered water mol­ecules are situated in the free space of this network. O—H⋯O hydrogen bonding within and between the subunits enhances the stability of the structure.

Related literature

For general background to coordination polymers, see: Wang et al. (2004[Wang, X.-L., Qin, C., Wang, E.-B., Xu, L., Su, Z.-M. & Hu, C.-W. (2004). Angew. Chem. Int. Ed. 43, 5036-5040.]). For crystal structures of related compounds based on 2-mercaptonicotinic acid, see: Sun et al. (2011[Sun, D., Wang, D.-F., Han, X.-G., Zhang, N., Huang, R.-B. & Zheng, L.-S. (2011). Chem. Commun. 47, 746-748.]). For complexes derived from the 2-H2CMSN ligand, see: Jiang et al. (2010[Jiang, X.-R., Wang, X.-J. & Feng, Y.-L. (2010). Acta Cryst. E66, o3308.], 2012[Jiang, X.-R., Wang, X.-J. & Feng, Y.-L. (2012). Inorg. Chim. Acta, 383, 38-45.]).

[Scheme 1]

Experimental

Crystal data

  • [Co2(C8H5NO4S)2(C10H8N2)3(H2O)2]·1.3H2O

  • Mr = 534.13

  • Monoclinic, P 21 /c

  • a = 10.2211 (1) Å

  • b = 17.1355 (2) Å

  • c = 16.4142 (2) Å

  • β = 125.484 (1)°

  • V = 2340.92 (5) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.87 mm−1

  • T = 296 K

  • 0.34 × 0.20 × 0.11 mm
Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2006[Bruker (2006). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.814, Tmax = 0.912

  • 38093 measured reflections

  • 5439 independent reflections

  • 4772 reflections with I > 2σ(I)

  • Rint = 0.025
Refinement

  • R[F2 > 2σ(F2)] = 0.033

  • wR(F2) = 0.093

  • S = 1.05

  • 5439 reflections

  • 315 parameters

  • 3 restraints

  • H-atom parameters constrained

  • Δρmax = 0.68 e Å−3

  • Δρmin = −0.53 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O1W—H1WA⋯O3i 0.85 1.89 2.663 (2) 150
O1W—H1WB⋯O2 0.85 1.90 2.682 (2) 152
Symmetry code: (i) -x, -y-1, -z.

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). APEX2, SAINT and SADABS. 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: DIAMOND (Brandenburg, 2008[Brandenburg, K. (2008). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S1600536813015262/wm2744sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536813015262/wm2744Isup2.hkl

checkCIF report


Comment top

The construction of coordination polymers has aroused attention due to their potential applications, fascinating topologies and entanglement motifs (Wang et al., 2004).

2-Mercaptonanicotinic acid (2-H2MN) is a multifunctional ligand containing one carboxyl group, one thiol group and a pyridyl N donor atom. Some complexes based on the 2-MN2- ligand have been previously investigated, e.g. by Sun et al. (2011). Recently, on the basis of the 2-H2MN ligand, we have designed a new multi-carboxylate ligand, 2-carboxymethylsulfanyl nicotinic acid (2-H2CMSN) to construct novel complexes (Jiang et al., 2010; 2012). The 2-H2CMSN ligand is interesting because of its potential versatile coordination behavior, resulting from one rigid and one flexible carboxyl group. Due to the flexible carboxyl group, it is favorable for constructing novel network structures. Here we report the structure of the new title compound, [Co(2-CMSN)(4,4'-bipy)1.5(H2O)].0.65H2O, (I).

Complex (I) is isostructural to [Ni(2-CMSN)(4,4'-bipy)1.5(H2O)].0.75H2O (Jiang et al., 2012). The asymmetric unit of (I) contains one CoII ion, one 2-CMSN2- ligand, one and a half 4,4-bipy molecules (the other half being completed by inversion symmetry), one coordination water molecule and disordered lattice water molecules with an overall occupancy of 0.65. The coordination environment of the CoII ion is illustrated in Fig. 1. The CoII ion is six-coordinated in a slightly distorted octahedral CoN3O3 environment: two O atoms originate from one flexible carboxyl group and one rigid carboxyl group of two symmetry-related 2-CMSN2- ligands, three N atoms from three 4,4'-bipy molecules and one O atom from the water molecule. Two adjacent CoII ions are linked by two 2-CMSN2- ligands to give a dinuclear [Co2(2-CMSN)2] subunit with a Co···Co distance of 6.8600 (3) Å (Fig. 2). The dinuclear [Co2(2-CMSN)2] subunits are further bridged by 4,4'-bipy linkers to generate a final three-dimensional structure (Fig. 2). The disordered water molecules are situated in the free space of the resulting network. The 4,4'-bipy molecule that is situated on a centre of inversion is exactly planar, whereas the other has a dihedral angle between the two pyridyl rings [N2,C9—C13] and [N3, C14—C18] of 33.16 (7)°.

In the crystal, intra- and inter-subunit O—H···O hydrogen bonds (Table 1) between the coordinating water molecule and carboxylate O atoms enhance the stability of the structure. Although the H atom position of the lattice water molecules could not be located, the O2W···O2 and O3W···S1 contacts of 2.864 (5) Å and 3.724 (9) Å, respectively, suggest also participation of these molecules in hydrogen bonding.

Related literature top

For general background to coordination polymers, see: Wang et al. (2004). For crystal structures of related complexes based on 2-mercaptonicotinic acid, see: Sun et al. (2011). For complexes derived from the 2-H2CMSN ligand, see: Jiang et al. (2010, 2012).

Experimental top

A mixture of 2-H2CMSN (0.4 mmol, 0.086 g), CoCl2 (0.4 mmol, 0.095 g) and 4,4'-bipy (0.4 mmol, 0.062 g) in CH3CH2OH (2 ml)/H2O (18 ml) was stirred for 1 h. The pH value was adjusted to around 6.0 by sodium carbonate solution in the entire process. Then the mixture was placed in a 25 ml stainless steel reactor and heated at 383 K for 24 h, and then cooled to room temperature for 24 h gave red crystals (yield 46%).

Refinement top

The carbon-bound H-atoms were placed in idealized positions [(C—H = 0.93 or 0.97 Å, Uiso(H) = 1.2Ueq(C)]. The coordinating water H-atoms were located in a different Fourier map and were refined with an O—H distance restrained to 0.85 (2) Å [Uiso(H) = 1.2Ueq(O)]. The two lattice water molecules are occupationally disordered (occupancies of 0.4 for OW2 and 0.25 for OW3). No reasonable H positions could be determined from Fourier maps for these atoms. Therefore the H atoms of OW2 and OW3 were omitted from refinement, but included in the final chemical formula.

Structure description top

The construction of coordination polymers has aroused attention due to their potential applications, fascinating topologies and entanglement motifs (Wang et al., 2004).

2-Mercaptonanicotinic acid (2-H2MN) is a multifunctional ligand containing one carboxyl group, one thiol group and a pyridyl N donor atom. Some complexes based on the 2-MN2- ligand have been previously investigated, e.g. by Sun et al. (2011). Recently, on the basis of the 2-H2MN ligand, we have designed a new multi-carboxylate ligand, 2-carboxymethylsulfanyl nicotinic acid (2-H2CMSN) to construct novel complexes (Jiang et al., 2010; 2012). The 2-H2CMSN ligand is interesting because of its potential versatile coordination behavior, resulting from one rigid and one flexible carboxyl group. Due to the flexible carboxyl group, it is favorable for constructing novel network structures. Here we report the structure of the new title compound, [Co(2-CMSN)(4,4'-bipy)1.5(H2O)].0.65H2O, (I).

Complex (I) is isostructural to [Ni(2-CMSN)(4,4'-bipy)1.5(H2O)].0.75H2O (Jiang et al., 2012). The asymmetric unit of (I) contains one CoII ion, one 2-CMSN2- ligand, one and a half 4,4-bipy molecules (the other half being completed by inversion symmetry), one coordination water molecule and disordered lattice water molecules with an overall occupancy of 0.65. The coordination environment of the CoII ion is illustrated in Fig. 1. The CoII ion is six-coordinated in a slightly distorted octahedral CoN3O3 environment: two O atoms originate from one flexible carboxyl group and one rigid carboxyl group of two symmetry-related 2-CMSN2- ligands, three N atoms from three 4,4'-bipy molecules and one O atom from the water molecule. Two adjacent CoII ions are linked by two 2-CMSN2- ligands to give a dinuclear [Co2(2-CMSN)2] subunit with a Co···Co distance of 6.8600 (3) Å (Fig. 2). The dinuclear [Co2(2-CMSN)2] subunits are further bridged by 4,4'-bipy linkers to generate a final three-dimensional structure (Fig. 2). The disordered water molecules are situated in the free space of the resulting network. The 4,4'-bipy molecule that is situated on a centre of inversion is exactly planar, whereas the other has a dihedral angle between the two pyridyl rings [N2,C9—C13] and [N3, C14—C18] of 33.16 (7)°.

In the crystal, intra- and inter-subunit O—H···O hydrogen bonds (Table 1) between the coordinating water molecule and carboxylate O atoms enhance the stability of the structure. Although the H atom position of the lattice water molecules could not be located, the O2W···O2 and O3W···S1 contacts of 2.864 (5) Å and 3.724 (9) Å, respectively, suggest also participation of these molecules in hydrogen bonding.

For general background to coordination polymers, see: Wang et al. (2004). For crystal structures of related complexes based on 2-mercaptonicotinic acid, see: Sun et al. (2011). For complexes derived from the 2-H2CMSN ligand, see: Jiang et al. (2010, 2012).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The coordination environment of the Co2+ ion in the title compound and the bridging character of the ligand. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i)-x, -y - 1, -z; (ii) x + 1, -y - 1/2, z + 1/2; (iv) -x, -y - 1, -z + 1; (vi) -x-1, y-1/2, -z-1/2.]
[Figure 2] Fig. 2. The dinuclear [Co2(2-CMSN)2] subunit (left), and the three-dimensional network of the title compound (right) viewed approximately down [001].
Poly[[diaquatris(µ2-4,4'-bipyridine)bis[µ2-2-(carboxylatomethylsulfanyl)nicotinato]dicobalt(II)] 1.3-hydrate] top
Crystal data top
[Co2(C8H5NO4S)2(C10H8N2)3(H2O)2]·1.3H2OF(000) = 1092.9
Mr = 1068.26V=2340.92(5)Å3
Monoclinic, P21/cDx = 1.516 Mg m−3
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 10.2211 (1) Åθ = 1.9–27.6°
b = 17.1355 (2) ŵ = 0.87 mm−1
c = 16.4142 (2) ÅT = 296 K
β = 125.484 (1)°Block, red
V = 2340.92 (5) Å30.34 × 0.20 × 0.11 mm
Z = 2
Data collection top
Bruker APEXII CCD
diffractometer		5439 independent reflections
Radiation source: fine-focus sealed tube4772 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ω scansθmax = 27.6°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2006)		h = −13→13
Tmin = 0.814, Tmax = 0.912k = −22→22
38093 measured reflectionsl = −21→21
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)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0477P)2 + 1.3453P]
where P = (Fo2 + 2Fc2)/3
5439 reflections(Δ/σ)max = 0.001
315 parametersΔρmax = 0.68 e Å−3
3 restraintsΔρmin = −0.53 e Å−3
Crystal data top
[Co2(C8H5NO4S)2(C10H8N2)3(H2O)2]·1.3H2OV = 2340.92 (5) Å3
Mr = 1068.26Z = 2
Monoclinic, P21/cMo Kα radiation
a = 10.2211 (1) ŵ = 0.87 mm−1
b = 17.1355 (2) ÅT = 296 K
c = 16.4142 (2) Å0.34 × 0.20 × 0.11 mm
β = 125.484 (1)°
Data collection top
Bruker APEXII CCD
diffractometer		5439 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2006)		4772 reflections with I > 2σ(I)
Tmin = 0.814, Tmax = 0.912Rint = 0.025
38093 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0333 restraints
wR(F2) = 0.093H-atom parameters constrained
S = 1.05Δρmax = 0.68 e Å−3
5439 reflectionsΔρmin = −0.53 e Å−3
315 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*/UeqOcc. (<1)
Co10.22673 (3)−0.467750 (13)0.253178 (16)0.02436 (8)
S1−0.26808 (6)−0.54790 (4)0.03145 (4)0.04356 (14)
N1−0.3385 (2)−0.68541 (12)−0.05863 (14)0.0512 (5)
N20.04982 (18)−0.38323 (9)0.15601 (11)0.0316 (3)
N3−0.60092 (18)−0.12730 (9)−0.15781 (11)0.0317 (3)
N40.14149 (18)−0.47934 (10)0.34767 (11)0.0324 (3)
O10.06128 (15)−0.55683 (8)0.16874 (10)0.0366 (3)
O20.20011 (18)−0.66643 (9)0.23590 (11)0.0506 (4)
O3−0.54191 (18)−0.48099 (12)−0.24881 (12)0.0595 (5)
O4−0.29489 (15)−0.53055 (8)−0.15622 (10)0.0327 (3)
O1W0.41017 (15)−0.55208 (8)0.34497 (9)0.0344 (3)
H1WB0.3686−0.59730.32680.041*
H1WA0.4812−0.54820.33360.041*
O2W0.3056 (6)−0.8235 (3)0.2968 (4)0.0716 (13)*0.40
O3W−0.7292 (11)−0.3553 (6)−0.2320 (7)0.082 (2)*0.25
C1−0.0421 (3)−0.75259 (13)0.07695 (19)0.0537 (6)
H1A0.0564−0.77620.12290.064*
C2−0.1648 (4)−0.79492 (14)−0.0044 (2)0.0737 (9)
H2A−0.1496−0.8467−0.01410.088*
C3−0.3083 (4)−0.75831 (15)−0.0694 (2)0.0661 (8)
H3A−0.3895−0.7863−0.12450.079*
C4−0.2204 (2)−0.64420 (12)0.01904 (13)0.0350 (4)
C5−0.0664 (2)−0.67566 (11)0.08956 (14)0.0345 (4)
C60.0760 (2)−0.62946 (11)0.17223 (13)0.0314 (4)
C7−0.4499 (3)−0.52819 (15)−0.09011 (16)0.0474 (5)
H7A−0.5211−0.5727−0.11030.057*
H7B−0.5031−0.4837−0.08470.057*
C8−0.4259 (2)−0.51158 (12)−0.17142 (14)0.0347 (4)
C9−0.1027 (3)−0.26859 (15)0.12914 (17)0.0637 (8)
H9A−0.1169−0.22450.15630.076*
C100.0229 (3)−0.31873 (14)0.18932 (16)0.0563 (7)
H10A0.0930−0.30690.25700.068*
C11−0.0478 (2)−0.39688 (11)0.05773 (13)0.0334 (4)
H11A−0.0282−0.44030.03230.040*
C12−0.1767 (2)−0.34941 (11)−0.00793 (13)0.0346 (4)
H12A−0.2421−0.3614−0.07580.042*
C13−0.2083 (2)−0.28423 (11)0.02741 (14)0.0369 (4)
C14−0.4239 (3)−0.19437 (14)−0.00281 (15)0.0474 (5)
H14A−0.3913−0.20300.06240.057*
C15−0.3472 (2)−0.23228 (11)−0.03857 (14)0.0359 (4)
C16−0.5485 (2)−0.14378 (13)−0.06392 (14)0.0421 (5)
H16A−0.5990−0.1197−0.03830.051*
C17−0.5296 (3)−0.16573 (12)−0.19305 (15)0.0422 (5)
H17A−0.5660−0.1568−0.25900.051*
C18−0.4046 (3)−0.21800 (12)−0.13694 (15)0.0439 (5)
H18A−0.3595−0.2434−0.16520.053*
C19−0.0124 (3)−0.46731 (18)0.31159 (16)0.0580 (7)
H19A−0.0828−0.45230.24500.070*
C20−0.0725 (2)−0.47589 (19)0.36765 (16)0.0623 (8)
H20A−0.1810−0.46730.33840.075*
C210.1870 (2)−0.51257 (11)0.50404 (14)0.0342 (4)
H21A0.2596−0.52900.56980.041*
C220.2363 (2)−0.50319 (11)0.44222 (14)0.0334 (4)
H22A0.3429−0.51430.46840.040*
C230.0286 (2)−0.49728 (11)0.46761 (13)0.0319 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01954 (12)0.02930 (13)0.02172 (12)0.00108 (8)0.01053 (10)0.00026 (8)
S10.0376 (3)0.0610 (3)0.0279 (2)0.0119 (2)0.0166 (2)−0.0005 (2)
N10.0453 (10)0.0565 (11)0.0372 (9)−0.0174 (9)0.0156 (8)−0.0018 (8)
N20.0287 (7)0.0332 (7)0.0277 (7)0.0085 (6)0.0133 (6)0.0012 (6)
N30.0272 (7)0.0340 (8)0.0269 (7)0.0054 (6)0.0118 (6)0.0025 (6)
N40.0243 (7)0.0467 (9)0.0270 (7)−0.0038 (6)0.0153 (6)−0.0027 (6)
O10.0280 (7)0.0316 (6)0.0355 (7)−0.0012 (5)0.0100 (6)−0.0022 (5)
O20.0419 (8)0.0390 (8)0.0445 (8)0.0039 (6)0.0101 (7)0.0102 (6)
O30.0285 (8)0.1104 (15)0.0385 (8)0.0196 (8)0.0188 (7)0.0218 (9)
O40.0257 (6)0.0449 (7)0.0285 (6)0.0045 (5)0.0163 (5)−0.0001 (5)
O1W0.0265 (6)0.0432 (7)0.0298 (6)0.0052 (5)0.0142 (5)0.0048 (5)
C10.0587 (14)0.0325 (10)0.0540 (13)−0.0024 (10)0.0237 (12)0.0045 (9)
C20.095 (2)0.0312 (11)0.0711 (18)−0.0167 (13)0.0345 (17)−0.0085 (11)
C30.0711 (18)0.0491 (14)0.0481 (13)−0.0264 (13)0.0174 (13)−0.0067 (11)
C40.0346 (10)0.0435 (10)0.0276 (8)−0.0089 (8)0.0184 (8)0.0004 (7)
C50.0379 (10)0.0326 (9)0.0317 (9)−0.0069 (7)0.0196 (8)0.0025 (7)
C60.0324 (9)0.0345 (9)0.0262 (8)−0.0014 (7)0.0164 (7)0.0043 (7)
C70.0287 (10)0.0808 (16)0.0351 (10)0.0118 (10)0.0198 (9)0.0087 (10)
C80.0239 (9)0.0502 (11)0.0280 (8)−0.0007 (8)0.0140 (7)−0.0029 (8)
C90.0586 (15)0.0597 (14)0.0353 (11)0.0329 (12)0.0057 (10)−0.0140 (10)
C100.0495 (13)0.0581 (14)0.0293 (10)0.0250 (11)0.0046 (9)−0.0102 (9)
C110.0403 (10)0.0324 (9)0.0287 (8)0.0094 (7)0.0207 (8)0.0026 (7)
C120.0402 (10)0.0353 (9)0.0240 (8)0.0088 (8)0.0162 (8)0.0023 (7)
C130.0360 (10)0.0374 (10)0.0292 (9)0.0131 (8)0.0143 (8)0.0026 (7)
C140.0505 (12)0.0582 (13)0.0276 (9)0.0263 (10)0.0193 (9)0.0095 (9)
C150.0335 (10)0.0350 (9)0.0294 (9)0.0100 (7)0.0127 (8)0.0010 (7)
C160.0421 (11)0.0503 (11)0.0334 (10)0.0189 (9)0.0216 (9)0.0063 (8)
C170.0502 (12)0.0444 (11)0.0301 (9)0.0165 (9)0.0222 (9)0.0083 (8)
C180.0508 (12)0.0454 (11)0.0371 (10)0.0202 (9)0.0265 (10)0.0073 (9)
C190.0243 (10)0.123 (2)0.0231 (9)−0.0001 (11)0.0117 (8)0.0058 (11)
C200.0190 (9)0.137 (3)0.0276 (10)−0.0005 (12)0.0119 (8)0.0040 (12)
C210.0314 (9)0.0408 (10)0.0322 (9)0.0058 (7)0.0195 (8)0.0088 (7)
C220.0272 (9)0.0401 (10)0.0358 (9)0.0055 (7)0.0200 (8)0.0067 (8)
C230.0258 (9)0.0428 (10)0.0286 (8)−0.0074 (7)0.0166 (7)−0.0042 (7)
Geometric parameters (Å, º) top
Co1—O4i2.0752 (13)C5—C61.514 (3)
Co1—O12.0951 (13)C7—C81.518 (3)
Co1—N22.1361 (14)C7—H7A0.9700
Co1—O1W2.1434 (13)C7—H7B0.9700
Co1—N42.1847 (15)C9—C101.375 (3)
Co1—N3ii2.2141 (15)C9—C131.390 (3)
S1—C41.765 (2)C9—H9A0.9300
S1—C71.801 (2)C10—H10A0.9300
N1—C31.323 (4)C11—C121.382 (2)
N1—C41.340 (3)C11—H11A0.9300
N2—C101.331 (2)C12—C131.380 (3)
N2—C111.336 (2)C12—H12A0.9300
N3—C161.335 (2)C13—C151.482 (3)
N3—C171.338 (2)C14—C161.377 (3)
N3—Co1iii2.2141 (14)C14—C151.384 (3)
N4—C221.330 (2)C14—H14A0.9300
N4—C191.336 (3)C15—C181.382 (3)
O1—C61.251 (2)C16—H16A0.9300
O2—C61.251 (2)C17—C181.384 (3)
O3—C81.243 (2)C17—H17A0.9300
O4—C81.254 (2)C18—H18A0.9300
O4—Co1i2.0752 (13)C19—C201.379 (3)
O1W—H1WB0.8500C19—H19A0.9300
O1W—H1WA0.8500C20—C231.388 (3)
C1—C51.379 (3)C20—H20A0.9300
C1—C21.392 (4)C21—C221.379 (2)
C1—H1A0.9300C21—C231.387 (2)
C2—C31.366 (4)C21—H21A0.9300
C2—H2A0.9300C22—H22A0.9300
C3—H3A0.9300C23—C23iv1.484 (3)
C4—C51.412 (3)
O4i—Co1—O189.07 (5)C8—C7—H7B108.6
O4i—Co1—N287.27 (5)S1—C7—H7B108.6
O1—Co1—N289.52 (6)H7A—C7—H7B107.5
O4i—Co1—O1W89.06 (5)O3—C8—O4125.96 (18)
O1—Co1—O1W90.84 (5)O3—C8—C7115.63 (17)
N2—Co1—O1W176.31 (5)O4—C8—C7118.40 (17)
O4i—Co1—N4173.20 (6)C10—C9—C13119.52 (19)
O1—Co1—N484.38 (6)C10—C9—H9A120.2
N2—Co1—N494.48 (6)C13—C9—H9A120.2
O1W—Co1—N489.21 (5)N2—C10—C9123.60 (19)
O4i—Co1—N3ii91.36 (5)N2—C10—H10A118.2
O1—Co1—N3ii179.27 (6)C9—C10—H10A118.2
N2—Co1—N3ii89.91 (6)N2—C11—C12122.98 (16)
O1W—Co1—N3ii89.76 (6)N2—C11—H11A118.5
N4—Co1—N3ii95.21 (6)C12—C11—H11A118.5
C4—S1—C7102.94 (11)C13—C12—C11119.87 (17)
C3—N1—C4118.3 (2)C13—C12—H12A120.1
C10—N2—C11117.00 (16)C11—C12—H12A120.1
C10—N2—Co1122.93 (13)C12—C13—C9116.92 (17)
C11—N2—Co1119.88 (12)C12—C13—C15122.51 (17)
C16—N3—C17116.14 (16)C9—C13—C15120.57 (17)
C16—N3—Co1iii123.35 (12)C16—C14—C15119.91 (18)
C17—N3—Co1iii120.09 (12)C16—C14—H14A120.0
C22—N4—C19115.95 (16)C15—C14—H14A120.0
C22—N4—Co1122.38 (12)C18—C15—C14116.83 (17)
C19—N4—Co1121.55 (13)C18—C15—C13122.48 (18)
C6—O1—Co1131.70 (12)C14—C15—C13120.68 (18)
C8—O4—Co1i130.24 (12)N3—C16—C14123.75 (18)
Co1—O1W—H1WB108.2N3—C16—H16A118.1
Co1—O1W—H1WA107.6C14—C16—H16A118.1
H1WB—O1W—H1WA108.2N3—C17—C18123.70 (18)
C5—C1—C2120.1 (2)N3—C17—H17A118.1
C5—C1—H1A119.9C18—C17—H17A118.1
C2—C1—H1A119.9C15—C18—C17119.59 (18)
C3—C2—C1118.1 (2)C15—C18—H18A120.2
C3—C2—H2A121.0C17—C18—H18A120.2
C1—C2—H2A121.0N4—C19—C20123.60 (19)
N1—C3—C2123.9 (2)N4—C19—H19A118.2
N1—C3—H3A118.1C20—C19—H19A118.2
C2—C3—H3A118.1C19—C20—C23120.19 (19)
N1—C4—C5122.6 (2)C19—C20—H20A119.9
N1—C4—S1116.49 (16)C23—C20—H20A119.9
C5—C4—S1120.88 (14)C22—C21—C23119.62 (17)
C1—C5—C4117.00 (19)C22—C21—H21A120.2
C1—C5—C6118.12 (19)C23—C21—H21A120.2
C4—C5—C6124.70 (17)N4—C22—C21124.35 (17)
O2—C6—O1125.36 (17)N4—C22—H22A117.8
O2—C6—C5117.72 (17)C21—C22—H22A117.8
O1—C6—C5116.86 (16)C21—C23—C20116.18 (17)
C8—C7—S1114.81 (14)C21—C23—C23iv121.7 (2)
C8—C7—H7A108.6C20—C23—C23iv122.1 (2)
S1—C7—H7A108.6
O4i—Co1—N2—C10−135.1 (2)C1—C5—C6—O1164.59 (19)
O1—Co1—N2—C10135.8 (2)C4—C5—C6—O1−10.3 (3)
N4—Co1—N2—C1051.5 (2)C4—S1—C7—C8−75.84 (19)
N3ii—Co1—N2—C10−43.7 (2)Co1i—O4—C8—O3−8.2 (3)
O4i—Co1—N2—C1149.97 (15)Co1i—O4—C8—C7170.55 (14)
O1—Co1—N2—C11−39.12 (15)S1—C7—C8—O3−164.40 (18)
O1W—Co1—N2—C1156.5 (9)S1—C7—C8—O416.8 (3)
N4—Co1—N2—C11−123.44 (15)C11—N2—C10—C93.2 (4)
N3ii—Co1—N2—C11141.34 (15)Co1—N2—C10—C9−171.9 (2)
O4i—Co1—N4—C2299.9 (4)C13—C9—C10—N2−0.7 (5)
O1—Co1—N4—C22115.53 (15)C10—N2—C11—C12−3.0 (3)
N2—Co1—N4—C22−155.40 (15)Co1—N2—C11—C12172.19 (15)
O1W—Co1—N4—C2224.61 (15)N2—C11—C12—C130.5 (3)
N3ii—Co1—N4—C22−65.08 (16)C11—C12—C13—C92.0 (3)
O4i—Co1—N4—C19−76.0 (5)C11—C12—C13—C15−178.22 (19)
O1—Co1—N4—C19−60.33 (19)C10—C9—C13—C12−1.9 (4)
N2—Co1—N4—C1928.75 (19)C10—C9—C13—C15178.3 (3)
O1W—Co1—N4—C19−151.25 (19)C16—C14—C15—C18−1.5 (3)
N3ii—Co1—N4—C19119.06 (19)C16—C14—C15—C13177.3 (2)
O4i—Co1—O1—C685.94 (17)C12—C13—C15—C18−33.7 (3)
N2—Co1—O1—C6173.22 (17)C9—C13—C15—C18146.1 (3)
O1W—Co1—O1—C6−3.11 (17)C12—C13—C15—C14147.5 (2)
N4—Co1—O1—C6−92.23 (17)C9—C13—C15—C14−32.7 (3)
N3ii—Co1—O1—C6−148 (4)C17—N3—C16—C142.8 (3)
C5—C1—C2—C3−0.8 (4)Co1iii—N3—C16—C14−169.71 (18)
C4—N1—C3—C21.9 (4)C15—C14—C16—N3−1.0 (4)
C1—C2—C3—N1−1.3 (5)C16—N3—C17—C18−2.2 (3)
C3—N1—C4—C5−0.4 (3)Co1iii—N3—C17—C18170.62 (18)
C3—N1—C4—S1−178.79 (19)C14—C15—C18—C172.1 (3)
C7—S1—C4—N1−16.68 (17)C13—C15—C18—C17−176.7 (2)
C7—S1—C4—C5164.86 (15)N3—C17—C18—C15−0.3 (4)
C2—C1—C5—C42.1 (3)C22—N4—C19—C202.2 (4)
C2—C1—C5—C6−173.2 (2)Co1—N4—C19—C20178.3 (2)
N1—C4—C5—C1−1.6 (3)N4—C19—C20—C230.8 (5)
S1—C4—C5—C1176.78 (16)C19—N4—C22—C21−2.8 (3)
N1—C4—C5—C6173.38 (18)Co1—N4—C22—C21−178.90 (15)
S1—C4—C5—C6−8.3 (3)C23—C21—C22—N40.6 (3)
Co1—O1—C6—O24.9 (3)C22—C21—C23—C202.4 (3)
Co1—O1—C6—C5−172.18 (12)C22—C21—C23—C23iv−177.0 (2)
C1—C5—C6—O2−12.7 (3)C19—C20—C23—C21−3.0 (4)
C4—C5—C6—O2172.36 (18)C19—C20—C23—C23iv176.3 (3)
Symmetry codes: (i) −x, −y−1, −z; (ii) x+1, −y−1/2, z+1/2; (iii) x−1, −y−1/2, z−1/2; (iv) −x, −y−1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O3i0.851.892.663 (2)150
O1W—H1WB···O20.851.902.682 (2)152
Symmetry code: (i) −x, −y−1, −z.

Experimental details

Crystal data
Chemical formula[Co2(C8H5NO4S)2(C10H8N2)3(H2O)2]·1.3H2O
Mr1068.26
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)10.2211 (1), 17.1355 (2), 16.4142 (2)
β (°) 125.484 (1)
V (Å3)2340.92 (5)
Z2
Radiation typeMo Kα
µ (mm−1)0.87
Crystal size (mm)0.34 × 0.20 × 0.11
Data collection
DiffractometerBruker APEXII CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2006)
Tmin, Tmax0.814, 0.912
No. of measured, independent and
observed [I > 2σ(I)] reflections		38093, 5439, 4772
Rint0.025
(sin θ/λ)max (Å−1)0.652
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.093, 1.05
No. of reflections5439
No. of parameters315
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.68, −0.53

Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O3i0.851.892.663 (2)150.3
O1W—H1WB···O20.851.902.682 (2)152.2
Symmetry code: (i) −x, −y−1, −z.
 

References

First citationBrandenburg, K. (2008). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
 First citationBruker (2006). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationJiang, X.-R., Wang, X.-J. & Feng, Y.-L. (2010). Acta Cryst. E66, o3308.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationJiang, X.-R., Wang, X.-J. & Feng, Y.-L. (2012). Inorg. Chim. Acta, 383, 38–45.  Web of Science CSD CrossRef CAS Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationSun, D., Wang, D.-F., Han, X.-G., Zhang, N., Huang, R.-B. & Zheng, L.-S. (2011). Chem. Commun. 47, 746–748.  Web of Science CSD CrossRef CAS Google Scholar
 First citationWang, X.-L., Qin, C., Wang, E.-B., Xu, L., Su, Z.-M. & Hu, C.-W. (2004). Angew. Chem. Int. Ed. 43, 5036–5040.  Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
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ISSN: 2056-9890
Volume 69| Part 7| July 2013| Page m371
https://doi.org/10.1107/S1600536813015262
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