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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 68| Part 4| April 2012| Pages m451-m452
doi:10.1107/S1600536812011269

Poly[[di­aqua­bis­­[μ4-5-nitro­isophthalato-κ4O1:O1:O3:O3′]bis­­[μ3-pyridine-4-carboxyl­ato-κ3O:O′:N]tricobalt(II)] tetra­hydrate]

Xia Yin,a Jun Fan,a* Jingling Xin,a Shengrun Zhenga and Weiguang Zhanga

aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510006, People's Republic of China
*Correspondence e-mail: fanj@scnu.edu.cn

(Received 5 March 2012; accepted 14 March 2012; online 21 March 2012)

The title compound, {[Co3(C6H4NO2)2(C8H3NO6)2(H2O)2]·4H2O}n, exhibits a two-dimensional layer-like structure in which the CoII ions exhibit two kinds of coordination geometries. One nearly octa­hedral CoII ion with crystallographic inversion symmetry is coordinated to six carboxyl­ate O atoms from four bridging 5-nitro­isophthalate (NIPH) ligands and two isonicotinate (IN) anions, while the other type of CoII ion binds with one N atom and one carboxyl­ate O atom from two IN anions, two carboxyl­ate O atoms from two different NIPH anions and one ligated water mol­ecule, displaying a distorted square-pyramidal coordination geometry. Three adjacent CoII ions are bridged by six carboxyl­ate groups from four NIPH ligands and two IN anions to form a linear trinuclear secondary building unit (SBU). Every trinuclear SBU is linked to its nearest neighbours in the ab plane, resulting in a two-dimensional layer-like structure perpendicular to the c axis. Along the a-axis direction neighbouring mol­ecules are connected through carboxyl­ate and pyridyl units of the IN anions, along the b axis through carboxyl­ate groups of the NIPH ligands. The H atoms of one free water mol­ecule are disordered in the crystal in a 1:1 ratio. Typical O—H⋯O hydrogen bonds are observed in the lattice, which include the following contacts: (a) between coordinated water mol­ecules and carboxyl­ate O atoms of the NIPH anions, (b) between lattice water mol­ecules and carboxyl­ate O atoms of the NIPH anions, and (c) between coordinated and lattice water mol­ecules. These inter­molecular hydrogen bonds connect the two-dimensional layers to form a three-dimensional supra­molecular structure.

Related literature

For general background to the design and synthesis of coordination polymers, see: Jiang et al. (2010[Jiang, H. L., Tatsu, Y., Lu, Z. H. & Xu, Q. (2010). J. Am. Chem. Soc. 132, 5586-5587.]); Ma et al. (2009[Ma, S. Q., Sun, D. F., Yuan, D. Q., Wang, X. S. & Zhou, H. C. (2009). J. Am. Chem. Soc. 131, 6445-6451.]); Natarajan & Mahata (2009[Natarajan, S. & Mahata, P. (2009). Chem. Soc. Rev. 38, 2304-2318.]); Zang et al. (2006[Zang, S. Q., Su, Y., Li, Y. Z., Ni, Z. P. & Meng, Q. J. (2006). Inorg. Chem. 45, 174-180.]). For complexes with isonicotinate, see: Amo-Ochoa et al. (2010[Amo-Ochoa, P., Welte, L., Gonzalez-Prieto, R., Sanz Miguel, P. J., Gomez-Garcia, C. J., Mateo-Marti, E., Delgado, S., Gomez-Herrero, J. & Zamora, F. (2010). Chem. Commun. 46, 3262-3264.]). For complexes with 5-nitro­isophthalate, see: Chen et al. (2006[Chen, H. J., Zhang, J., Feng, W. L. & Fu, M. (2006). Inorg. Chem. Commun. 9, 300-303.], 2010[Chen, S. P., Ren, Y. X., Wang, W. T. & Gao, S. L. (2010). Dalton Trans. 39, 1552-1557.]); Sun et al. (2010[Sun, D., Luo, G. G., Zhang, N., Wei, Z. H., Yang, C. F., Xu, Q. J., Huang, R. B. & Zheng, L. S. (2010). J. Mol. Struct. 967, 147-152.]). For related compounds, see: Du et al. (2008[Du, M., Zhang, Z. H., You, Y. P. & Zhao, X. J. (2008). CrystEngComm, 10, 306-321.]); Luo et al. (2003[Luo, J. H., Hong, M. C., Wang, R. H., Cao, R., Han, L., Yuan, D. Q., Lin, Z. Z. & Zhou, Y. F. (2003). Inorg. Chem. 42, 4486-4488.]); Wang et al. (2009[Wang, H.-D., Li, M.-M. & He, H.-Y. (2009). Acta Cryst. E65, m510.]).

[Scheme 1]

Experimental

Crystal data

  • [Co3(C6H4NO2)2(C8H3NO6)2(H2O)2]·4H2O

  • Mr = 947.32

  • Triclinic, [P \overline 1]

  • a = 9.1890 (18) Å

  • b = 9.3548 (19) Å

  • c = 10.390 (2) Å

  • α = 78.74 (3)°

  • β = 88.64 (3)°

  • γ = 73.68 (3)°

  • V = 840.2 (3) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.57 mm−1

  • T = 298 K

  • 0.35 × 0.28 × 0.16 mm
Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2002[Bruker (2002). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.610, Tmax = 0.788

  • 4357 measured reflections

  • 2976 independent reflections

  • 2667 reflections with I > 2σ(I)

  • Rint = 0.012
Refinement

  • R[F2 > 2σ(F2)] = 0.027

  • wR(F2) = 0.071

  • S = 1.02

  • 2976 reflections

  • 271 parameters

  • 10 restraints

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

  • Δρmax = 0.40 e Å−3

  • Δρmin = −0.40 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O1W—H1W⋯O3i 0.84 2.05 2.861 (3) 160
O1W—H2W⋯O2Wii 0.85 1.93 2.773 (3) 173
O3W—H5W⋯O2iii 0.82 2.01 2.820 (2) 168
O3W—H6W⋯O1Wiv 0.83 1.83 2.648 (3) 167
O2W—H4WA⋯O2v 0.85 (2) 2.27 (2) 3.098 (4) 165 (8)
O2W—H3WA⋯O6vi 0.83 (2) 2.38 (6) 3.055 (3) 138 (8)
O2W—H3WB⋯O2Wii 0.87 (2) 2.49 (3) 3.297 (6) 154 (6)
O2W—H4WB⋯O6vi 0.89 (5) 2.54 (5) 3.055 (4) 118 (3)
O2W—H4WB⋯O2v 0.89 (5) 2.54 (5) 3.098 (3) 121 (4)
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, -y, -z; (iii) -x, -y+1, -z+2; (iv) x-1, y, z+1; (v) -x, -y+1, -z+1; (vi) x+1, y-1, z.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: APEX2; data reduction: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); 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: 10.1107/S1600536812011269/zl2461sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812011269/zl2461Isup2.hkl

checkCIF report


Comment top

Over the past decades, rational design and construction of metal coordination polymers with aromatic carboxylates have become an attractive area in coordination and supramolecular chemistry, due to the fascinating network topologies they exhibit (Natarajan & Mahata, 2009) and due to industrially focused applications in gas storage, adsorption and separation (Ma et al., 2009), nonlinear optical devices (Zang et al., 2006), and fluorescence (Jiang et al., 2010), etc. Due to versatile coordination modes and easy formation of secondary building units, 5-nitroisophthalate (NIPH) has been widely employed to construct coordination polymers (Chen et al., 2010; Du et al., 2008; Sun et al., 2010).

Most cobalt complexes with 5-nitroisophthalate (NIPH) and aromatic N-donor coligands (pyridine, bipyridine, and imidazole) possess low-dimensional structure characteristics, namely, ladder, loop-like chain, zigzag chain, layer, and grid, etc (Chen et al., 2006; Du et al., 2008; Luo et al., 2003). Cobalt complexes based on NIPH ligand and other carboxylates have been less developed (Wang et al., 2009). In this work, we selected isonicotinic acid (HIN) as the coligand based on the following considerations: (1) it possesses the bifunctional bridging groups with both oxygen and nitrogen donors as a potential linkers and (2) it can adopt various coordination modes in high-dimensional heterometallic frameworks (Amo-Ochoa et al., 2010). Herein, synthesis and crystal structure of a new cobalt compound is presented, which was prepared by hydrothermal reaction of Co(CH3COO)2.4 H2O with 5-nitroisophthalic acid and isonicotinic acid.

The title compound exhibits a two-dimensional layer-like framework. As illustrated in Fig.1, each asymmetric unit contains one and a half CoII ions, one 5-nitroisophthalate (NIPH) anion, an isonicotinate (IN) anion, one ligated and two lattice water molecules, as the Co1II ion lies on a crystallographic inversion centre. In the structure, the Co1II ion is six-coordinated in an O6 donor set with the coordination geometry of a slightly distorted octahedron by four carboxylate oxygen atoms [O1, O1i, O4ii, O4iii, symmetry codes: (i) -x, 1 - y, 1 - z; (ii) x, -1 + y, z; (iii) -x, 2 - y, 1 - z] from four bridging NIPH ligands in the equatorial plane, and the others [O8 and O8i, symmetry code: (i) -x, 1 - y, 1 - z] from two IN anions at the axial sites; the Co2II ion coordinates with one N2iv atom [symmetry code: (iv) -1 + x, y, z] and one carboxylate O7 atom from two IN anions, two carboxylate oxygen atoms [O3ii and O7, symmetry code: (ii) x, -1 + y, z] from two different NIPH anions and one ligated water molecules, displaying a distorted square pyramidal coordination geometry. If the weak Co—O interaction between Co2 and O2 (2.4908 (6) Å) was considered, the coordination configuration of the Co2 ion could also be described as a severely distorted octahedron. The Co—O bond distances are in the range of 2.0206 (18)–2.1624 (16) Å, and the Co—N bond length is equal to 2.1465 (19) Å, all of which are in the normal ranges (Du et al., 2008).

The NIPH ligand acts as µ4-bridge to link four different CoII ions through two carboxylate groups and the IN anion adopts a tridentate-bridging mode to connect three CoII ions. Thus, one Co1II and two Co2II ions are bridged by six carboxylate groups from four NIPH ligands (two carboxylate groups in bis-monodentate mode and two in monodentate bridged mode) and two IN anions (the carboxylate groups in bis-monodentate mode) to form a linear trinuclear secondary building unit (SBU), [Co3(NIPH)2(IN)2(H2O)2] with a Co···Co separation of 3.5086 (10) Å. Every trinuclear SBU is in turn linked to its nearest neighbors in the ab plane, resulting in a two-dimensional layer like structure perpendicular to the c-axis (Fig. 2). Along the a-axis direction neighboring molecules are connected through carboxylate and pyridyl units of the IN anions, along the b-axis through carboxylate groups of the NIPH ligands. Topologically, the trinuclear CoII units can be seen as four-connected nodes and the organic ligands (the NIPH and IN anions) act as two-connected rods. On the basis of this simplification, this two-dimensional structure can be described as a (4,4)-topological network.

There are multiple O–H···O hydrogen bonds in the complex, which include the following types of contacts: (a) between coordinated water molecule and carboxylate oxygen atoms of the NIPH anions [O···O, 2.820 (3) Å], (b) between lattice water molecule and carboxylate oxygen atoms of the NIPH anions [O···O, 2.861 (3) – 3.098 (4) Å] and (c) between coordinated and lattice water molecules [O···O, 2.648 (3) – 3.297 (6) Å]. Thus, these two-dimensional layers are further extended to a three-dimensional supramolecular network (Fig. 3).

The IR spectrum shows characteristic absorptions for the carboxylate stretching vibrations and the coordination of organic carboxylate anions (NIPH and IN) to CoII was confirmed by the absence of υ(COOH) absorption bands of the organic ligands at around 1700 cm-1. The characteristic vibrations of the carboxylate groups are seen in the range 1607–1541 cm-1 for asymmetric stretching and 1461–1360 cm-1 for symmetric stretching. The broad absorption band observed at 3412 cm-1 can be assigned to the O–H stretching vibration, indicating the presence of water molecules.

In summary, a new (4, 4)–two-dimensional layer-like polynuclear CoII coordination polymer was constructed by hydrothermal reaction between Co(II) ions and mixed carboxylate ligands, which is further extended to a three-dimensional supramolecular network through intermolecular hydrogen bonding.

Related literature top

For general background to the design and synthesis of coordination polymers, see: Jiang et al. (2010); Ma et al. (2009); Natarajan & Mahata (2009); Zang et al. (2006). For complexes with isonicotinate, see: Amo-Ochoa et al. (2010). For complexes with 5-nitroisophthalate, see: Chen et al. (2006, 2010); Sun et al. (2010). For related compounds, see: Du et al. (2008); Luo et al. (2003); Wang et al. (2009).

Experimental top

A mixture of Co(CH3COO)2.4 H2O (0.1245 g, 0.50 mmol), 5-nitroisophthalic acid (0.0503 g, 0.25 mmol) and isonicotinic acid (0.0310 g, 0.25 mmol) in 8 ml H2O were sealed in a 15 ml Teflon-lined stainless steel reactor and kept under autogenous pressure at 393 K for three days. After the sample was cooled to room temperature at a rate of 5 K/h, pink block-shaped crystals of the title compound were collected and washed with ethanol and water (yield, 45%). IR (KBr pellet, ν, cm-1): 3412 (br), 3102 (s), 1607 (s), 1587 (s), 1541 (s), 1461 (m), 1420 (m), 1403 (s), 1360 (m), 1342 (m), 1163 (w), 1088 (m), 1065 (m), 1024 (m), 933 (m), 921 (w), 862 (m), 792 (m), 781 (m), 724 (m), 714 (s), 691 (m), 592 (w), 562 (w).

Refinement top

The disordered hydrogen atoms (H3W and H4W) of lattice water molecule O2W are, due to a close contact of O2W with one of its symmetry equivalent counterparts across an inversion center, disordered in a 1:1 mode in the crystal. In one of the alternative orientations O2W is hydrogen bonding via H3WB to O2Wii and via H4WB to both O2v and O5vi. In the other orientation, with O2W acting as the acceptor of a hydrogen bond from O2Wii, the water molecule hydrogen bonds via H3WA and H3WB to O6vi and O2v (see Table 1 for symmetry operators). All hydrogen atoms of water molecules were located in electron difference density Fourier maps. The disordered hydrogen atoms (H3W and H4W) of lattice water molecule O2W were refined in a 1:1 disordered mode with O—H distance restraints of 0.85 (2) Å, and H···H distance restraints of 1.37 (2) Å. The other hydrogen atoms were placed geometrically and refined as riding atoms [C—H = 0.93 Å (aromatic C—H), O–H = 0.83 Å (coordinated H2O) and 0.85 Å (lattice water molecules)]. All H atoms were refined with isotropic thermal factors Uiso (H) = 1.2 Ueq (C), or Uiso (H) = 1.5 Ueq(O)].

Structure description top

Over the past decades, rational design and construction of metal coordination polymers with aromatic carboxylates have become an attractive area in coordination and supramolecular chemistry, due to the fascinating network topologies they exhibit (Natarajan & Mahata, 2009) and due to industrially focused applications in gas storage, adsorption and separation (Ma et al., 2009), nonlinear optical devices (Zang et al., 2006), and fluorescence (Jiang et al., 2010), etc. Due to versatile coordination modes and easy formation of secondary building units, 5-nitroisophthalate (NIPH) has been widely employed to construct coordination polymers (Chen et al., 2010; Du et al., 2008; Sun et al., 2010).

Most cobalt complexes with 5-nitroisophthalate (NIPH) and aromatic N-donor coligands (pyridine, bipyridine, and imidazole) possess low-dimensional structure characteristics, namely, ladder, loop-like chain, zigzag chain, layer, and grid, etc (Chen et al., 2006; Du et al., 2008; Luo et al., 2003). Cobalt complexes based on NIPH ligand and other carboxylates have been less developed (Wang et al., 2009). In this work, we selected isonicotinic acid (HIN) as the coligand based on the following considerations: (1) it possesses the bifunctional bridging groups with both oxygen and nitrogen donors as a potential linkers and (2) it can adopt various coordination modes in high-dimensional heterometallic frameworks (Amo-Ochoa et al., 2010). Herein, synthesis and crystal structure of a new cobalt compound is presented, which was prepared by hydrothermal reaction of Co(CH3COO)2.4 H2O with 5-nitroisophthalic acid and isonicotinic acid.

The title compound exhibits a two-dimensional layer-like framework. As illustrated in Fig.1, each asymmetric unit contains one and a half CoII ions, one 5-nitroisophthalate (NIPH) anion, an isonicotinate (IN) anion, one ligated and two lattice water molecules, as the Co1II ion lies on a crystallographic inversion centre. In the structure, the Co1II ion is six-coordinated in an O6 donor set with the coordination geometry of a slightly distorted octahedron by four carboxylate oxygen atoms [O1, O1i, O4ii, O4iii, symmetry codes: (i) -x, 1 - y, 1 - z; (ii) x, -1 + y, z; (iii) -x, 2 - y, 1 - z] from four bridging NIPH ligands in the equatorial plane, and the others [O8 and O8i, symmetry code: (i) -x, 1 - y, 1 - z] from two IN anions at the axial sites; the Co2II ion coordinates with one N2iv atom [symmetry code: (iv) -1 + x, y, z] and one carboxylate O7 atom from two IN anions, two carboxylate oxygen atoms [O3ii and O7, symmetry code: (ii) x, -1 + y, z] from two different NIPH anions and one ligated water molecules, displaying a distorted square pyramidal coordination geometry. If the weak Co—O interaction between Co2 and O2 (2.4908 (6) Å) was considered, the coordination configuration of the Co2 ion could also be described as a severely distorted octahedron. The Co—O bond distances are in the range of 2.0206 (18)–2.1624 (16) Å, and the Co—N bond length is equal to 2.1465 (19) Å, all of which are in the normal ranges (Du et al., 2008).

The NIPH ligand acts as µ4-bridge to link four different CoII ions through two carboxylate groups and the IN anion adopts a tridentate-bridging mode to connect three CoII ions. Thus, one Co1II and two Co2II ions are bridged by six carboxylate groups from four NIPH ligands (two carboxylate groups in bis-monodentate mode and two in monodentate bridged mode) and two IN anions (the carboxylate groups in bis-monodentate mode) to form a linear trinuclear secondary building unit (SBU), [Co3(NIPH)2(IN)2(H2O)2] with a Co···Co separation of 3.5086 (10) Å. Every trinuclear SBU is in turn linked to its nearest neighbors in the ab plane, resulting in a two-dimensional layer like structure perpendicular to the c-axis (Fig. 2). Along the a-axis direction neighboring molecules are connected through carboxylate and pyridyl units of the IN anions, along the b-axis through carboxylate groups of the NIPH ligands. Topologically, the trinuclear CoII units can be seen as four-connected nodes and the organic ligands (the NIPH and IN anions) act as two-connected rods. On the basis of this simplification, this two-dimensional structure can be described as a (4,4)-topological network.

There are multiple O–H···O hydrogen bonds in the complex, which include the following types of contacts: (a) between coordinated water molecule and carboxylate oxygen atoms of the NIPH anions [O···O, 2.820 (3) Å], (b) between lattice water molecule and carboxylate oxygen atoms of the NIPH anions [O···O, 2.861 (3) – 3.098 (4) Å] and (c) between coordinated and lattice water molecules [O···O, 2.648 (3) – 3.297 (6) Å]. Thus, these two-dimensional layers are further extended to a three-dimensional supramolecular network (Fig. 3).

The IR spectrum shows characteristic absorptions for the carboxylate stretching vibrations and the coordination of organic carboxylate anions (NIPH and IN) to CoII was confirmed by the absence of υ(COOH) absorption bands of the organic ligands at around 1700 cm-1. The characteristic vibrations of the carboxylate groups are seen in the range 1607–1541 cm-1 for asymmetric stretching and 1461–1360 cm-1 for symmetric stretching. The broad absorption band observed at 3412 cm-1 can be assigned to the O–H stretching vibration, indicating the presence of water molecules.

In summary, a new (4, 4)–two-dimensional layer-like polynuclear CoII coordination polymer was constructed by hydrothermal reaction between Co(II) ions and mixed carboxylate ligands, which is further extended to a three-dimensional supramolecular network through intermolecular hydrogen bonding.

For general background to the design and synthesis of coordination polymers, see: Jiang et al. (2010); Ma et al. (2009); Natarajan & Mahata (2009); Zang et al. (2006). For complexes with isonicotinate, see: Amo-Ochoa et al. (2010). For complexes with 5-nitroisophthalate, see: Chen et al. (2006, 2010); Sun et al. (2010). For related compounds, see: Du et al. (2008); Luo et al. (2003); Wang et al. (2009).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: APEX2 (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, with displacement ellipsoids drawn at the 30% probability level. All H atoms are drawn as spheres of arbitrary radii. [Symmetry codes: (i): -x, -y + 1, -z + 1; (ii): x - 1, y, z; (iii): -x + 1, -y + 1, -z + 1; (iv): x, y - 1, z; (v): -x, -y + 2, -z - 1]. Disorder of H atoms of O2W is omitted for clarity.
[Figure 2] Fig. 2. (a) A packing diagram along the a-axial direction. (b) A packing diagram, showing the two-dimensional layer-like structure in the ab plane. H atoms are omitted for clarity.
[Figure 3] Fig. 3. A packing diagram of the title compound, showing the three-dimensional supramolecular network driven by intermolecular hydrogen bonds (dashed lines). H atoms are omitted for clarity.
Poly[[diaquabis[µ4-5-nitroisophthalato- κ4O1:O1:O3:O3']bis[µ3-pyridine-4- carboxylato-κ3O:O':N]tricobalt(II)] tetrahydrate] top
Crystal data top
[Co3(C6H4NO2)2(C8H3NO6)2(H2O)2]·4H2OZ = 1
Mr = 947.32F(000) = 479
Triclinic, P1Dx = 1.872 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.1890 (18) ÅCell parameters from 3665 reflections
b = 9.3548 (19) Åθ = 2.0–27.9°
c = 10.390 (2) ŵ = 1.57 mm−1
α = 78.74 (3)°T = 298 K
β = 88.64 (3)°Block, pink
γ = 73.68 (3)°0.35 × 0.28 × 0.16 mm
V = 840.2 (3) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		2976 independent reflections
Radiation source: fine-focus sealed tube2667 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.012
φ and ω scanθmax = 25.3°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)		h = −9→11
Tmin = 0.610, Tmax = 0.788k = −11→11
4357 measured reflectionsl = −12→12
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.0397P)2 + 0.585P]
where P = (Fo2 + 2Fc2)/3
2976 reflections(Δ/σ)max = 0.001
271 parametersΔρmax = 0.40 e Å−3
10 restraintsΔρmin = −0.40 e Å−3
Crystal data top
[Co3(C6H4NO2)2(C8H3NO6)2(H2O)2]·4H2Oγ = 73.68 (3)°
Mr = 947.32V = 840.2 (3) Å3
Triclinic, P1Z = 1
a = 9.1890 (18) ÅMo Kα radiation
b = 9.3548 (19) ŵ = 1.57 mm−1
c = 10.390 (2) ÅT = 298 K
α = 78.74 (3)°0.35 × 0.28 × 0.16 mm
β = 88.64 (3)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		2976 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)		2667 reflections with I > 2σ(I)
Tmin = 0.610, Tmax = 0.788Rint = 0.012
4357 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02710 restraints
wR(F2) = 0.071H atoms treated by a mixture of independent and constrained refinement
S = 1.02Δρmax = 0.40 e Å−3
2976 reflectionsΔρmin = −0.40 e Å−3
271 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)
C1−0.1582 (2)0.6886 (2)0.7129 (2)0.0192 (5)
C2−0.1920 (3)0.8433 (2)0.6267 (2)0.0193 (5)
C3−0.2761 (3)0.8738 (2)0.5103 (2)0.0215 (5)
H3−0.31090.79910.48460.026*
C4−0.3067 (3)1.0182 (3)0.4336 (2)0.0226 (5)
C5−0.2494 (3)1.1290 (3)0.4646 (2)0.0241 (5)
H5−0.26711.22320.40860.029*
C6−0.1647 (3)1.0974 (2)0.5811 (2)0.0194 (5)
C7−0.1408 (3)0.9561 (2)0.6638 (2)0.0212 (5)
H7−0.09020.93700.74450.025*
C90.2058 (2)0.3927 (2)0.7504 (2)0.0201 (5)
C100.3646 (2)0.3974 (2)0.7775 (2)0.0201 (5)
C110.4307 (3)0.3616 (3)0.9022 (2)0.0302 (6)
H110.37690.33390.97530.036*
C120.5780 (3)0.3674 (3)0.9166 (2)0.0291 (5)
H120.62270.33881.00050.035*
C130.5920 (3)0.4501 (3)0.6972 (2)0.0320 (6)
H130.64540.48360.62590.038*
C140.4490 (3)0.4422 (3)0.6743 (2)0.0313 (6)
H140.40850.46720.58890.038*
C8−0.1022 (2)1.2189 (2)0.6151 (2)0.0202 (5)
Co10.00000.50000.50000.01527 (11)
Co2−0.10352 (3)0.39808 (3)0.82492 (3)0.01738 (10)
N20.6596 (2)0.4120 (2)0.81683 (18)0.0218 (4)
N1−0.4063 (2)1.0548 (2)0.3153 (2)0.0297 (5)
O2−0.1492 (2)0.67118 (19)0.83422 (16)0.0285 (4)
O1−0.14157 (17)0.57462 (16)0.65704 (15)0.0192 (3)
O6−0.4433 (3)0.9517 (2)0.2817 (2)0.0474 (5)
O5−0.4506 (3)1.1871 (2)0.2580 (2)0.0484 (5)
O70.11919 (18)0.3888 (2)0.84536 (16)0.0285 (4)
O3−0.07060 (19)1.21068 (17)0.73447 (16)0.0247 (4)
O4−0.08995 (18)1.31976 (17)0.52098 (16)0.0250 (4)
O80.17412 (17)0.39430 (18)0.63366 (15)0.0231 (3)
O1W0.8479 (2)0.0405 (2)0.1145 (2)0.0498 (5)
H1W0.9262−0.02990.14290.075*
H2W0.80170.01090.05990.075*
O3W−0.0897 (2)0.2994 (2)1.01711 (16)0.0356 (4)
H5W−0.01900.31811.05150.053*
H6W−0.10210.21831.05770.053*
O2W0.3255 (3)0.0491 (3)0.0522 (3)0.0676 (7)
H4WA0.271 (8)0.114 (6)0.094 (7)0.101*0.50
H3WA0.386 (8)−0.021 (7)0.103 (6)0.101*0.50
H3WB0.415 (3)−0.006 (6)0.038 (6)0.101*0.50
H4WB0.344 (5)0.096 (5)0.114 (5)0.101*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0180 (11)0.0210 (11)0.0200 (12)−0.0090 (9)−0.0018 (9)−0.0017 (9)
C20.0203 (11)0.0170 (11)0.0211 (12)−0.0057 (9)0.0012 (9)−0.0046 (9)
C30.0245 (12)0.0198 (11)0.0226 (12)−0.0085 (9)0.0000 (9)−0.0067 (9)
C40.0246 (12)0.0229 (12)0.0205 (12)−0.0059 (9)−0.0043 (9)−0.0050 (9)
C50.0285 (13)0.0181 (11)0.0244 (13)−0.0068 (9)0.0002 (10)−0.0009 (9)
C60.0226 (11)0.0168 (10)0.0212 (11)−0.0087 (9)0.0018 (9)−0.0049 (9)
C70.0244 (12)0.0227 (11)0.0185 (11)−0.0095 (9)−0.0006 (9)−0.0044 (9)
C90.0164 (11)0.0186 (11)0.0247 (13)−0.0058 (9)−0.0022 (9)−0.0012 (9)
C100.0165 (11)0.0222 (11)0.0224 (12)−0.0059 (9)−0.0030 (9)−0.0047 (9)
C110.0256 (13)0.0474 (15)0.0193 (12)−0.0183 (11)−0.0009 (10)0.0010 (11)
C120.0247 (13)0.0447 (15)0.0191 (12)−0.0142 (11)−0.0049 (10)−0.0017 (11)
C130.0258 (13)0.0518 (16)0.0201 (13)−0.0196 (12)0.0000 (10)0.0016 (11)
C140.0237 (13)0.0541 (17)0.0186 (13)−0.0191 (12)−0.0043 (10)−0.0003 (11)
C80.0164 (11)0.0173 (11)0.0274 (13)−0.0048 (9)−0.0008 (9)−0.0053 (9)
Co10.0164 (2)0.0163 (2)0.0144 (2)−0.00812 (16)−0.00199 (16)−0.00068 (16)
Co20.01635 (17)0.02053 (17)0.01603 (17)−0.00834 (12)−0.00217 (11)−0.00047 (12)
N20.0185 (10)0.0277 (10)0.0205 (10)−0.0088 (8)−0.0011 (8)−0.0042 (8)
N10.0334 (12)0.0289 (11)0.0256 (11)−0.0078 (9)−0.0075 (9)−0.0031 (9)
O20.0386 (10)0.0315 (9)0.0176 (9)−0.0147 (8)−0.0028 (7)−0.0024 (7)
O10.0226 (8)0.0158 (7)0.0209 (8)−0.0086 (6)0.0011 (6)−0.0028 (6)
O60.0637 (14)0.0393 (11)0.0429 (12)−0.0196 (10)−0.0279 (10)−0.0057 (9)
O50.0636 (14)0.0314 (11)0.0423 (12)−0.0081 (10)−0.0262 (10)0.0072 (9)
O70.0183 (8)0.0470 (10)0.0226 (9)−0.0141 (7)−0.0003 (7)−0.0050 (8)
O30.0308 (9)0.0209 (8)0.0242 (9)−0.0095 (7)−0.0051 (7)−0.0048 (7)
O40.0319 (9)0.0219 (8)0.0254 (9)−0.0163 (7)−0.0005 (7)−0.0013 (7)
O80.0211 (8)0.0282 (8)0.0200 (9)−0.0062 (7)−0.0051 (6)−0.0051 (7)
O1W0.0499 (13)0.0354 (11)0.0605 (14)−0.0130 (10)−0.0197 (11)0.0029 (10)
O3W0.0370 (11)0.0510 (11)0.0227 (9)−0.0284 (9)−0.0097 (8)0.0079 (8)
O2W0.0697 (18)0.0779 (19)0.0591 (16)−0.0224 (14)−0.0130 (14)−0.0186 (14)
Geometric parameters (Å, º) top
C1—O21.241 (3)C8—O41.246 (3)
C1—O11.281 (3)C8—O31.263 (3)
C1—C21.499 (3)Co1—O82.0363 (17)
C2—C31.388 (3)Co1—O8i2.0363 (17)
C2—C71.389 (3)Co1—O4ii2.0506 (15)
C3—C41.384 (3)Co1—O4iii2.0506 (15)
C3—H30.9300Co1—O12.1623 (16)
C4—C51.379 (3)Co1—O1i2.1623 (16)
C4—N11.477 (3)Co2—O3W2.0205 (18)
C5—C61.391 (3)Co2—O72.0383 (16)
C5—H50.9300Co2—O3ii2.0927 (16)
C6—C71.391 (3)Co2—O12.1146 (17)
C6—C81.511 (3)Co2—N2iv2.1468 (19)
C7—H70.9300N2—Co2v2.1468 (19)
C9—O81.250 (3)N1—O61.220 (3)
C9—O71.254 (3)N1—O51.222 (3)
C9—C101.507 (3)O3—Co2vi2.0927 (16)
C10—C141.376 (3)O4—Co1vi2.0506 (15)
C10—C111.384 (3)O1W—H1W0.8406
C11—C121.383 (3)O1W—H2W0.8463
C11—H110.9300O3W—H5W0.8243
C12—N21.334 (3)O3W—H6W0.8285
C12—H120.9300O2W—H4WA0.854 (19)
C13—N21.341 (3)O2W—H3WA0.83 (2)
C13—C141.366 (3)O2W—H3WB0.868 (19)
C13—H130.9300O2W—H4WB0.886 (18)
C14—H140.9300
O2—C1—O1120.9 (2)O8—Co1—O4iii84.51 (7)
O2—C1—C2121.4 (2)O8i—Co1—O4iii95.49 (7)
O1—C1—C2117.69 (19)O4ii—Co1—O4iii180.0
C3—C2—C7120.2 (2)O8—Co1—O189.18 (6)
C3—C2—C1119.64 (19)O8i—Co1—O190.82 (6)
C7—C2—C1120.2 (2)O4ii—Co1—O187.91 (6)
C4—C3—C2118.2 (2)O4iii—Co1—O192.09 (6)
C4—C3—H3120.9O8—Co1—O1i90.82 (6)
C2—C3—H3120.9O8i—Co1—O1i89.18 (6)
C5—C4—C3122.5 (2)O4ii—Co1—O1i92.09 (6)
C5—C4—N1119.0 (2)O4iii—Co1—O1i87.91 (6)
C3—C4—N1118.4 (2)O1—Co1—O1i180.0
C4—C5—C6118.8 (2)O3W—Co2—O786.46 (7)
C4—C5—H5120.6O3W—Co2—O3ii101.78 (7)
C6—C5—H5120.6O7—Co2—O3ii97.35 (7)
C5—C6—C7119.6 (2)O3W—Co2—O1158.16 (7)
C5—C6—C8118.8 (2)O7—Co2—O193.45 (7)
C7—C6—C8121.6 (2)O3ii—Co2—O199.89 (6)
C2—C7—C6120.5 (2)O3W—Co2—N2iv90.42 (8)
C2—C7—H7119.8O7—Co2—N2iv175.95 (7)
C6—C7—H7119.8O3ii—Co2—N2iv85.80 (7)
O8—C9—O7126.8 (2)O1—Co2—N2iv88.50 (7)
O8—C9—C10115.7 (2)C12—N2—C13116.3 (2)
O7—C9—C10117.6 (2)C12—N2—Co2v126.40 (16)
C14—C10—C11117.4 (2)C13—N2—Co2v116.62 (15)
C14—C10—C9119.2 (2)O6—N1—O5123.4 (2)
C11—C10—C9123.4 (2)O6—N1—C4118.2 (2)
C12—C11—C10119.0 (2)O5—N1—C4118.4 (2)
C12—C11—H11120.5C1—O1—Co299.61 (13)
C10—C11—H11120.5C1—O1—Co1132.30 (13)
N2—C12—C11123.7 (2)Co2—O1—Co1110.24 (7)
N2—C12—H12118.2C9—O7—Co2122.97 (15)
C11—C12—H12118.2C8—O3—Co2vi124.57 (14)
N2—C13—C14123.5 (2)C8—O4—Co1vi134.35 (15)
N2—C13—H13118.3C9—O8—Co1138.09 (15)
C14—C13—H13118.3H1W—O1W—H2W108.3
C13—C14—C10120.1 (2)Co2—O3W—H5W107.7
C13—C14—H14120.0Co2—O3W—H6W133.6
C10—C14—H14120.0H5W—O3W—H6W109.9
O4—C8—O3126.6 (2)H4WA—O2W—H3WA111 (4)
O4—C8—C6115.6 (2)H4WA—O2W—H3WB149 (7)
O3—C8—C6117.70 (19)H3WA—O2W—H3WB51 (7)
O8—Co1—O8i180.000 (1)H4WA—O2W—H4WB46 (6)
O8—Co1—O4ii95.49 (7)H3WA—O2W—H4WB77 (6)
O8i—Co1—O4ii84.51 (7)H3WB—O2W—H4WB103 (3)
O2—C1—C2—C3−146.5 (2)C3—C4—N1—O5169.9 (2)
O1—C1—C2—C332.3 (3)O2—C1—O1—Co20.1 (2)
O2—C1—C2—C732.7 (3)C2—C1—O1—Co2−178.70 (16)
O1—C1—C2—C7−148.5 (2)O2—C1—O1—Co1−128.83 (19)
C7—C2—C3—C40.0 (3)C2—C1—O1—Co152.4 (3)
C1—C2—C3—C4179.3 (2)O3W—Co2—O1—C18.5 (2)
C2—C3—C4—C54.0 (3)O7—Co2—O1—C1−80.54 (13)
C2—C3—C4—N1−175.2 (2)O3ii—Co2—O1—C1−178.62 (13)
C3—C4—C5—C6−3.7 (4)N2iv—Co2—O1—C195.91 (13)
N1—C4—C5—C6175.4 (2)O3W—Co2—O1—Co1150.72 (15)
C4—C5—C6—C7−0.5 (3)O7—Co2—O1—Co161.64 (8)
C4—C5—C6—C8−179.9 (2)O3ii—Co2—O1—Co1−36.44 (8)
C3—C2—C7—C6−4.1 (3)N2iv—Co2—O1—Co1−121.91 (8)
C1—C2—C7—C6176.6 (2)O8—Co1—O1—C184.14 (19)
C5—C6—C7—C24.4 (3)O8i—Co1—O1—C1−95.86 (19)
C8—C6—C7—C2−176.2 (2)O4ii—Co1—O1—C1179.66 (19)
O8—C9—C10—C1416.8 (3)O4iii—Co1—O1—C1−0.34 (19)
O7—C9—C10—C14−162.7 (2)O8—Co1—O1—Co2−41.04 (7)
O8—C9—C10—C11−164.6 (2)O8i—Co1—O1—Co2138.96 (7)
O7—C9—C10—C1116.0 (3)O4ii—Co1—O1—Co254.48 (8)
C14—C10—C11—C12−2.2 (4)O4iii—Co1—O1—Co2−125.52 (8)
C9—C10—C11—C12179.2 (2)O8—C9—O7—Co2−4.1 (3)
C10—C11—C12—N22.8 (4)C10—C9—O7—Co2175.29 (14)
N2—C13—C14—C101.9 (4)O3W—Co2—O7—C9157.95 (19)
C11—C10—C14—C130.0 (4)O3ii—Co2—O7—C956.52 (18)
C9—C10—C14—C13178.7 (2)O1—Co2—O7—C9−43.92 (18)
C5—C6—C8—O4−21.3 (3)O4—C8—O3—Co2vi35.3 (3)
C7—C6—C8—O4159.2 (2)C6—C8—O3—Co2vi−143.13 (16)
C5—C6—C8—O3157.3 (2)O3—C8—O4—Co1vi7.4 (4)
C7—C6—C8—O3−22.2 (3)C6—C8—O4—Co1vi−174.15 (14)
C11—C12—N2—C13−1.0 (4)O7—C9—O8—Co143.6 (4)
C11—C12—N2—Co2v−171.6 (2)C10—C9—O8—Co1−135.76 (18)
C14—C13—N2—C12−1.3 (4)O4ii—Co1—O8—C9−101.0 (2)
C14—C13—N2—Co2v170.1 (2)O4iii—Co1—O8—C979.0 (2)
C5—C4—N1—O6172.6 (2)O1—Co1—O8—C9−13.2 (2)
C3—C4—N1—O6−8.3 (3)O1i—Co1—O8—C9166.8 (2)
C5—C4—N1—O5−9.3 (3)
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x, y−1, z; (iii) −x, −y+2, −z+1; (iv) x−1, y, z; (v) x+1, y, z; (vi) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3vii0.842.052.861 (3)160
O1W—H2W···O2Wviii0.851.932.773 (3)173
O3W—H5W···O2ix0.822.012.820 (2)168
O3W—H6W···O1Wx0.831.832.648 (3)167
O2W—H4WA···O2i0.85 (2)2.27 (2)3.098 (4)165 (8)
O2W—H3WA···O6xi0.83 (2)2.38 (6)3.055 (3)138 (8)
O2W—H3WB···O2Wviii0.87 (2)2.49 (3)3.297 (6)154 (6)
O2W—H4WB···O6xi0.89 (5)2.54 (5)3.055 (4)118 (3)
O2W—H4WB···O2i0.89 (5)2.54 (5)3.098 (3)121 (4)
Symmetry codes: (i) −x, −y+1, −z+1; (vii) −x+1, −y+1, −z+1; (viii) −x+1, −y, −z; (ix) −x, −y+1, −z+2; (x) x−1, y, z+1; (xi) x+1, y−1, z.

Experimental details

Crystal data
Chemical formula[Co3(C6H4NO2)2(C8H3NO6)2(H2O)2]·4H2O
Mr947.32
Crystal system, space groupTriclinic, P1
Temperature (K)298
a, b, c (Å)9.1890 (18), 9.3548 (19), 10.390 (2)
α, β, γ (°)78.74 (3), 88.64 (3), 73.68 (3)
V (Å3)840.2 (3)
Z1
Radiation typeMo Kα
µ (mm−1)1.57
Crystal size (mm)0.35 × 0.28 × 0.16
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2002)
Tmin, Tmax0.610, 0.788
No. of measured, independent and
observed [I > 2σ(I)] reflections		4357, 2976, 2667
Rint0.012
(sin θ/λ)max (Å−1)0.600
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.071, 1.02
No. of reflections2976
No. of parameters271
No. of restraints10
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.40, −0.40

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

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3i0.842.052.861 (3)160.4
O1W—H2W···O2Wii0.851.932.773 (3)172.9
O3W—H5W···O2iii0.822.012.820 (2)168.1
O3W—H6W···O1Wiv0.831.832.648 (3)167.4
O2W—H4WA···O2v0.854 (19)2.27 (2)3.098 (4)165 (8)
O2W—H3WA···O6vi0.83 (2)2.38 (6)3.055 (3)138 (8)
O2W—H3WB···O2Wii0.868 (19)2.49 (3)3.297 (6)154 (6)
O2W—H4WB···O6vi0.89 (5)2.54 (5)3.055 (4)118 (3)
O2W—H4WB···O2v0.89 (5)2.54 (5)3.098 (3)121 (4)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z; (iii) −x, −y+1, −z+2; (iv) x−1, y, z+1; (v) −x, −y+1, −z+1; (vi) x+1, y−1, z.
 

Acknowledgements

This work was supported financially by the National Natural Science Foundation of China (grant Nos. 21171059 and 21003053) and Guangdong Science and Technology Department (grant Nos. 2010B090300031 and 2011B010400023).

References

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ISSN: 2056-9890
Volume 68| Part 4| April 2012| Pages m451-m452
doi:10.1107/S1600536812011269
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