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 4| April 2010| Pages m483-m484

Penta­aqua­tri-μ3-hydroxido-tris­­(imino­di­acetato)-μ3-oxido-tetra­hedro-calcium(II)tricobalt(III) 2.54-hydrate

aDepartment of Chemistry, Faculty of Science, Kochi University, Akebono-cho 2-5-1, Kochi 780-8520, Japan
*Correspondence e-mail: tomama@cc.kochi-u.ac.jp

(Received 18 March 2010; accepted 24 March 2010; online 31 March 2010)

In the title compound, [CaCo3(C4H5NO4)3(OH)3O(H2O)5]·2.54H2O, the Co atom is octa­hedrally coordinated by one imino­diacetate (ida) dianion as a facial O,N,O′-tridentate ligand, two μ3-OH groups and one μ3-O ligand, forming an partial Co3O4 cubane cluster. This unit coordinates to a CaII cation in an O,O′,O′′-tridentate fashion, generating a distorted CaCo3O4 cubane-type cluster. The Ca—μ3-O distances [2.429 (5)–2.572 (6) Å] are much longer than the Co—μ3—O bonds [1.895 (5)–1.941 (5) Å]. The CaII cation is also coord­inated by five water mol­ecules with Ca—O distances in the range 2.355 (6)–2.543 (6) Å. There are three additional uncoordinated water mol­ecules in the asymmetric unit, the occupancy of which refined to 0.54 (3). In H2O (or D2O), the title complex hydrolyses to Ca2+aq cations and [Co3(ida)3(μ2-OH)3(μ3-O)]2− anions.

Related literature

For the synthesis and chemistry of partial Co3O4 cubane clusters, see: Ama et al. (1997[Ama, T., Shiro, M., Takeuchi, A., Yonemura, T., Kawaguchi, H. & Yasui, T. (1997). Bull. Chem. Soc. Jpn, 70, 2685-1692.], 2000[Ama, T., Rashid, Md. M., Yonemura, T., Kawaguchi, H. & Yasui, T. (2000). Coord. Chem. Rev. 198, 101-116.], 2001[Ama, T., Rashid, Md. M., Sarker, A. K., Miyakawa, H., Yonemura, T., Kawaguchi, H. & Yasui, T. (2001). Bull. Chem. Soc. Jpn, 74, 2327-2333.], 2006[Ama, T., Yonemura, T. & Yamaguchi, M. (2006). Bull. Chem. Soc. Jpn, 79, 1063-1065.]). For the chemistry and structure of CaMn4O4 clusters in the OEC (oxygen evolution center) of plants, see: Barber & Murray (2008[Barber, J. & Murray, J. W. (2008). Coord. Chem. Rev. 252, 233-243.]); Rappaport & Diner (2008[Rappaport, F. & Diner, B. A. (2008). Coord. Chem. Rev. 252, 259-272.]); Sauer et al. (2008[Sauer, K., Yano, J. & Yachandra, V. K. (2008). Coord. Chem. Rev. 252, 318-335.]); Yocum (2008[Yocum, C. F. (2008). Coord. Chem. Rev. 252, 296-305.]). For a related structure, see: Ama et al. (1995[Ama, T., Miyazaki, J., Hamada, K., Okamoto, K., Yonemura, T., Kawaguchi, H. & Yasui, T. (1995). Chem. Lett. pp. 267-268.]).

[Scheme 1]

Experimental

Crystal data
  • [CaCo3(C4H5NO4)3(OH)3O(H2O)5]·2.54H2O

  • Mr = 812.92

  • Triclinic, [P \overline 1]

  • a = 10.474 (3) Å

  • b = 11.303 (7) Å

  • c = 12.588 (5) Å

  • α = 75.88 (4)°

  • β = 100.92 (3)°

  • γ = 104.58 (3)°

  • V = 1385.6 (10) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.06 mm−1

  • T = 296 K

  • 0.40 × 0.40 × 0.05 mm

Data collection
  • Rigaku AFC-7S diffractometer

  • Absorption correction: ψ scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.673, Tmax = 0.902

  • 6713 measured reflections

  • 6360 independent reflections

  • 3290 reflections with F2 > 2σ(F2)

  • Rint = 0.076

  • 3 standard reflections every 150 reflections intensity decay: 4.8%

Refinement
  • R[F2 > 2σ(F2)] = 0.060

  • wR(F2) = 0.207

  • S = 1.00

  • 6360 reflections

  • 389 parameters

  • H-atom parameters constrained

  • Δρmax = 1.17 e Å−3

  • Δρmin = −1.13 e Å−3

Table 1
Selected bond lengths (Å)

Co1—O1 1.877 (5)
Co1—O2 1.903 (5)
Co1—O4 1.941 (5)
Co2—O1 1.888 (4)
Co2—O2 1.907 (5)
Co2—O3 1.895 (5)
Co3—O1 1.866 (5)
Co3—O3 1.915 (5)
Co3—O4 1.921 (5)
Ca1—O2 2.572 (6)
Ca1—O3 2.527 (6)
Ca1—O4 2.429 (5)
Ca1—O17 2.355 (6)
Ca1—O18 2.411 (6)
Ca1—O19 2.543 (6)
Ca1—O20 2.406 (6)
Ca1—O21 2.471 (8)

Data collection: WinAFC (Rigaku/MSC, 2000[Rigaku/MSC (2000). WinAFC. Rigaku/MSC, The Woodlands,Texas, USA.]); cell refinement: WinAFC; data reduction: CrystalStructure (Rigaku/MSC, 2007[Rigaku/MSC (2007). CrystalStructure. Rigaku Americas, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.]); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999[Beurskens, P. T., Admiraal, G., Beurskens, G., Bosman, W. P., Garcia-Granda, S., Gould, R. O., Smits, J. M. M. & Smykalla, C. (1999). DIRDIF99. University of Nijmegen, The Netherlands.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2007[Rigaku/MSC (2007). CrystalStructure. Rigaku Americas, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.]).

Supporting information


Comment top

We have previously reported on the structures of some [Co3(L)32-OH)33-O)]n+ (L: tridentate ligand) complexes which form incomplete cubane Co3O4 clusters (Ama et al., 1997, 2000,2001, 2006). While many such cationic [Co3(L)32-OH)33-O)]n+ complexes are known, we could find no mention of an anionic complex in our survey of the literature. The title compound was formed during an attempt to prepare the anionic complex [Co3(ida)32-OH)33-O)]2-.

Investigations of the CaMn3O4 cluster are important to gain an understanding of the chemistry of O2 evolution centers (OEC) in plants (Yocum, 2008; Sauer et al., 2008; Barber & Murray, 2008; Rappaport & Diner, 2008). The Mn clusters in the OEC are of interest due to their unique structure, photoreaction mechanisms, and redox chemistry. Moreover, as the covalent radius of Co (1.33 Å) is similar to that of Mn (1.35 Å), we were interested in the preparation of the cobalt analogue, CaCo3O4, as a model of OEC.

In the title complex, each Co atom is coordinated by one ida (iminodiacetato) molecule which acts as a facial tridentate (O,N,O') ligand, two µ2-OH groups and one µ3-O ligand, forming a Co3O4 cluster. This cluster further coordinates to CaII in a tridentate manner generating a distorted CaCo3O4 cubane-type cluster. The µ2-O—Co distances are 1.895 (5) - 1.941 (5)Å and the Co—µ2-O—Co' angles are 94.5 (2) – 95.8 (2)°. In the T1 isomer (Ama et al., 1995) of [Co3(edma)32-OH)33-O)]+ (edma: ethylenediaminemonoacetato), the corresponding distances and angles are 1.899 (3) -1.923 (2)Å and 95.0 (1) - 96.2 (1)°. Hence the structure of the Co3O4 cluster in the title compound resembles that of [Co3(edma)32-OH)33-O)]+ cation. As the Ca2+ cation is coordinated by the three µ3-OH ligands of the Co3O4 cluster, the CaCo3O4 cluster can be considered to be a distorted cubane cluster. The Ca—µ3-O distances (2.429 (5) – 2.572 (6) Å) are much longer than Co—µ3-O (1.895 (5) - 1.921 (5) Å). The µ3-O—Ca—µ3-O' angles (59.84 (16) - 63.09 (16)) are smaller than those involving cobalt, µ3-O—Co—µ3-O' (84.0 (2) - 85.6 (2)°) and Co—µ3-O—Co' (94.5 (2) - 95.8 (2)) in the Co3O4 cluster. There are three additional uncoordinated water molecules in the asymmetric unit, the occupancy of one of these solvates that has the largest Ueq value refines to 0.54 (3).

Related literature top

For the synthesis and chemistry of partial Co3O4 cubane clusters, see: Ama et al. (1997, 2000, 2001, 2006). For the chemistry and structure of CaMn4O4 clusters in the OEC (oxygen evolution center) of plants, see: Barber & Murray (2008); Rappaport & Diner (2008); Sauer et al. (2008); Yocum (2008). For a related structure, see: Ama et al. (1995).

Experimental top

To a suspension of 7.0 g of KHCO3 in 10 cm3 of water, a solution 2.38 g of cobalt(II) chloride hexahydrate and 4 cm3 of 30% H2O2 in 10 cm3 of water was added dropwise with stirring at below 0° C. After the solution was stirred for 15 min, 10 cm3 of H2O containing 1.3 g of H2ida was added and then stirred overnight. The solution was acidified to pH 1.0 with 30% HClO4, stirred for 30 min, pH adjusted to 8.3 with 2 mol dm-3 KOH aqueous solution and then stirred for 2.5 h at 45°C. Filtering off the insoluble white-brown precipitate, the filtrate was loaded onto a QAE-Sephadex column (Cl- form). The adsorbed band was developed with 0.2 mol dm-3 KCl Solution. The eluate from the fifth brown band was collected and concentrated to a small volume and then methanol was added to deposit KCl. After removing the KCl by filtration, potassium salt (K2[Co3(ida)32-OH)33-O)] 3.25 H2O) was obtained by standing the filtrate in a refrigerator. Yield: 76 mg. (Anal. Found: C, 18.45; H, 3.21; N, 5.34%. Calcd for C12H24.5N3O19.25K2Co3 (K2[Co3(ida)32-OH)(µ3-O)] 3.25 H2O): C, 18.62; H, 3.19; N, 5.43%. This potassium salt was dissolved in a small amount of water, which was loaded to a QAE-Sephadex column (Cl- form; ø 6.5 cm × 3.5 cm) and then eluted with 500 cm3 of water to remove the K+ ion in the solution. The adsorbed brown band was eluted out with 0.5 mol dm-3 of CaCl2. The eluted solution was concentrated to a few cm3 and then ethanol and diethylether were added. As the solution was separated into a brown and an uncolored layers, the colorless layer was removed by decantation. After these procedures were repeated several times, a large amount of ethanol was added and the solution allowed to stand overnight at room temperature. The resulting brown precipitate was collected and washed with ethanol. This crude solid was recrystallized from water by adding ethanol. Anal. Found: C, 17.84; H, 4.04; N, 5.11%. Calcd for C12H33.08N3O23.54CaCo3 ([Ca(H2O)5Co3(ida)3(µ-OH)33-O)] 2.54 H2O): C, 17.73; H, 4.09; N, 5.17%. 1H NMR: (δ=4.22 and 3.24ppm; Jgem=17.6 Hz) and (δ=4.03 and 3.24ppm; Jgem=17.2 Hz).

Refinement top

All H atoms of the fragment containing CaCo3O4 cluster were positioned geometrically (C—H = 0.95 Å, N—H = 0.91 Å and O—H = 0.84 Å) and refined as riding, with Uiso(H)= 1.2 Ueq of the parent atom. The H atoms of the solvate water molecules were found in the difference Fourier synthesis, constrained to O—H = 0.84Å and then refined as riding.

Computing details top

Data collection: WinAFC (Rigaku/MSC, 2000); cell refinement: WinAFC (Rigaku/MSC, 2000); data reduction: CrystalStructure (Rigaku/MSC, 2007); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2007).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound showing the atom-labeling scheme and with 50% probability displacement ellipsoids.
Pentaaquatri-µ3-hydroxido-tris(iminodiacetato)-µ3-oxido- tetrahedro-calcium(II)tricobalt(III) 2.54-hydrate top
Crystal data top
[CaCo3(C4H5NO4)3(OH)3O(H2O)5]·2.54H2OZ = 2
Mr = 812.92F(000) = 830.80
Triclinic, P1Dx = 1.948 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 10.474 (3) ÅCell parameters from 12 reflections
b = 11.303 (7) Åθ = 15.1–15.8°
c = 12.588 (5) ŵ = 2.06 mm1
α = 75.88 (4)°T = 296 K
β = 100.92 (3)°Plate, brown
γ = 104.58 (3)°0.40 × 0.40 × 0.05 mm
V = 1385.6 (10) Å3
Data collection top
Rigaku AFC-7S
diffractometer
Rint = 0.076
ω–2θ scansθmax = 27.5°
Absorption correction: ψ scan
(North et al., 1968)
h = 013
Tmin = 0.673, Tmax = 0.902k = 1414
6713 measured reflectionsl = 1616
6360 independent reflections3 standard reflections every 150 reflections
3290 reflections with F2 > 2σ(F2) intensity decay: 4.8%
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.060 w = 1/[σ2(Fo2) + (0.1052P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.207(Δ/σ)max < 0.0001
S = 1.00Δρmax = 1.17 e Å3
6360 reflectionsΔρmin = 1.13 e Å3
389 parameters
Crystal data top
[CaCo3(C4H5NO4)3(OH)3O(H2O)5]·2.54H2Oγ = 104.58 (3)°
Mr = 812.92V = 1385.6 (10) Å3
Triclinic, P1Z = 2
a = 10.474 (3) ÅMo Kα radiation
b = 11.303 (7) ŵ = 2.06 mm1
c = 12.588 (5) ÅT = 296 K
α = 75.88 (4)°0.40 × 0.40 × 0.05 mm
β = 100.92 (3)°
Data collection top
Rigaku AFC-7S
diffractometer
3290 reflections with F2 > 2σ(F2)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.076
Tmin = 0.673, Tmax = 0.9023 standard reflections every 150 reflections
6713 measured reflections intensity decay: 4.8%
6360 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.060389 parameters
wR(F2) = 0.207H-atom parameters constrained
S = 1.00Δρmax = 1.17 e Å3
6360 reflectionsΔρmin = 1.13 e Å3
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co(1)0.71696 (10)0.72533 (9)0.93041 (8)0.0137 (2)
Co(2)0.73172 (10)0.93813 (9)0.75658 (8)0.0141 (2)
Co(3)0.51954 (10)0.72856 (9)0.74180 (8)0.0140 (2)
Ca(1)0.81420 (15)0.67221 (15)0.69882 (13)0.0190 (3)
O(1)0.6046 (4)0.8286 (4)0.8436 (4)0.0141 (10)
O(2)0.8387 (5)0.8207 (4)0.8306 (4)0.0176 (11)
O(3)0.6625 (5)0.8240 (4)0.6610 (4)0.0154 (10)
O(4)0.6435 (5)0.6261 (4)0.8183 (4)0.0160 (10)
O(5)0.8438 (5)0.6279 (5)1.0143 (4)0.0224 (12)
O(6)1.0147 (6)0.6325 (6)1.1499 (5)0.0377 (16)
O(7)0.5867 (5)0.6299 (5)1.0215 (4)0.0227 (12)
O(8)0.4950 (6)0.6300 (6)1.1655 (5)0.0327 (14)
O(9)0.8615 (5)1.0388 (5)0.6638 (4)0.0256 (12)
O(10)0.8934 (7)1.2014 (6)0.5255 (6)0.052 (2)
O(11)0.7888 (5)1.0409 (4)0.8634 (4)0.0176 (11)
O(12)0.7064 (8)1.1589 (7)0.9394 (5)0.051 (2)
O(13)0.4431 (5)0.6281 (5)0.6339 (4)0.0228 (12)
O(14)0.2633 (7)0.4911 (7)0.5851 (6)0.051 (2)
O(15)0.4032 (5)0.8393 (5)0.6783 (4)0.0203 (11)
O(16)0.2518 (6)0.9176 (6)0.7259 (5)0.0399 (16)
O(17)0.9506 (7)0.8551 (6)0.6103 (6)0.050 (2)
O(18)0.6561 (6)0.6337 (6)0.5383 (5)0.0358 (16)
O(19)0.7455 (5)0.4350 (6)0.7370 (5)0.0348 (15)
O(20)0.9788 (6)0.6105 (6)0.8499 (5)0.0313 (14)
O(21)0.9474 (6)0.5947 (6)0.5991 (5)0.0395 (16)
O(22)0.0992 (5)0.9178 (6)0.8899 (5)0.0315 (14)
O(23)0.6372 (6)0.8910 (6)0.4401 (5)0.0411 (17)
O(24)0.8213 (16)0.7798 (16)0.3566 (14)0.068 (4)0.54 (3)
N(1)0.7746 (6)0.8266 (5)1.0404 (5)0.0168 (12)
N(2)0.6218 (5)1.0576 (5)0.6830 (5)0.0149 (12)
N(3)0.3720 (6)0.6372 (5)0.8218 (5)0.0167 (12)
C(1)0.9207 (8)0.6772 (7)1.0912 (6)0.0236 (17)
C(2)0.5724 (7)0.6812 (7)1.0984 (6)0.0195 (15)
C(3)0.8963 (8)0.7956 (8)1.1112 (7)0.0279 (18)
C(4)0.6595 (8)0.8098 (7)1.0997 (7)0.0251 (17)
C(5)0.8276 (9)1.1327 (8)0.5968 (7)0.0300 (19)
C(6)0.7038 (9)1.1044 (7)0.8667 (6)0.0253 (17)
C(7)0.6939 (9)1.1555 (8)0.6011 (7)0.031 (2)
C(8)0.5893 (8)1.1025 (7)0.7744 (6)0.0213 (16)
C(9)0.3283 (8)0.5566 (8)0.6488 (7)0.0266 (18)
C(10)0.3213 (7)0.8398 (7)0.7426 (6)0.0217 (16)
C(11)0.2752 (8)0.5578 (7)0.7508 (7)0.0246 (17)
C(12)0.3138 (8)0.7343 (7)0.8439 (6)0.0237 (17)
H(1)0.79470.90791.00480.020*
H(2)0.54521.01720.64760.018*
H(3)0.40150.58890.88640.020*
H(4)0.88590.78411.18670.033*
H(5)0.97020.86231.09440.033*
H(6)0.60910.87111.06370.030*
H(7)0.69040.81831.17380.030*
H(8)0.70571.23400.62070.037*
H(9)0.64231.15670.53030.037*
H(10)0.51171.04790.80140.026*
H(11)0.57321.18440.74780.026*
H(12)0.19620.58970.72940.030*
H(13)0.25510.47490.79230.030*
H(14)0.36320.76420.90710.028*
H(15)0.22370.70090.85580.028*
H(16)0.91660.84980.85860.021*
H(17)0.64080.85540.59400.018*
H(18)0.61070.55000.84130.019*
H(19)0.93470.91790.62580.060*
H(20)1.01150.86820.57100.060*
H(21)0.68030.58620.50780.043*
H(22)0.58060.59970.55770.043*
H(23)0.78390.40560.79910.042*
H(24)0.66260.41300.73650.042*
H(25)0.94100.56900.90480.038*
H(26)1.02090.56660.83100.038*
H(27)0.89770.53870.56770.047*
H(28)0.98230.65400.55140.047*
H(29)0.13830.87070.94020.038*
H(30)0.13400.89160.84780.038*
H(31)0.66830.83790.42290.049*
H(32)0.67650.95000.39520.049*
H(33)0.81620.71090.38780.079*0.54
H(34)0.87080.82150.39780.079*0.54
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co(1)0.0127 (4)0.0144 (5)0.0121 (4)0.0010 (3)0.0026 (3)0.0006 (3)
Co(2)0.0116 (4)0.0139 (5)0.0152 (4)0.0011 (3)0.0034 (3)0.0007 (3)
Co(3)0.0110 (4)0.0161 (5)0.0135 (4)0.0006 (3)0.0026 (3)0.0024 (3)
Ca(1)0.0147 (7)0.0214 (8)0.0208 (7)0.0042 (6)0.0039 (6)0.0027 (6)
O(1)0.012 (2)0.014 (2)0.018 (2)0.003 (2)0.0010 (19)0.008 (2)
O(2)0.013 (2)0.016 (2)0.020 (2)0.002 (2)0.000 (2)0.001 (2)
O(3)0.018 (2)0.015 (2)0.013 (2)0.003 (2)0.004 (2)0.001 (2)
O(4)0.018 (2)0.012 (2)0.018 (2)0.004 (2)0.005 (2)0.003 (2)
O(5)0.025 (2)0.018 (2)0.023 (2)0.008 (2)0.001 (2)0.000 (2)
O(6)0.032 (3)0.039 (3)0.038 (3)0.019 (3)0.007 (2)0.001 (3)
O(7)0.020 (2)0.018 (2)0.024 (2)0.004 (2)0.007 (2)0.001 (2)
O(8)0.029 (3)0.034 (3)0.032 (3)0.003 (2)0.017 (2)0.002 (2)
O(9)0.020 (2)0.021 (2)0.034 (3)0.001 (2)0.015 (2)0.002 (2)
O(10)0.058 (4)0.040 (4)0.057 (4)0.018 (3)0.039 (4)0.025 (3)
O(11)0.020 (2)0.017 (2)0.015 (2)0.000 (2)0.002 (2)0.009 (2)
O(12)0.067 (5)0.073 (5)0.033 (3)0.046 (4)0.014 (3)0.033 (3)
O(13)0.015 (2)0.031 (3)0.019 (2)0.007 (2)0.009 (2)0.006 (2)
O(14)0.035 (3)0.069 (5)0.052 (4)0.022 (3)0.012 (3)0.045 (4)
O(15)0.016 (2)0.023 (2)0.021 (2)0.007 (2)0.002 (2)0.001 (2)
O(16)0.034 (3)0.038 (3)0.050 (4)0.019 (3)0.020 (3)0.008 (3)
O(17)0.041 (4)0.034 (3)0.083 (5)0.003 (3)0.043 (4)0.005 (3)
O(18)0.028 (3)0.048 (4)0.045 (3)0.006 (3)0.010 (2)0.033 (3)
O(19)0.020 (3)0.033 (3)0.047 (3)0.002 (2)0.006 (2)0.002 (3)
O(20)0.030 (3)0.036 (3)0.030 (3)0.009 (2)0.004 (2)0.009 (2)
O(21)0.040 (3)0.029 (3)0.051 (4)0.003 (2)0.025 (3)0.007 (3)
O(22)0.020 (2)0.039 (3)0.037 (3)0.002 (2)0.002 (2)0.016 (2)
O(23)0.039 (3)0.053 (4)0.029 (3)0.020 (3)0.009 (3)0.010 (3)
O(24)0.063 (10)0.071 (11)0.066 (10)0.016 (9)0.003 (8)0.009 (9)
N(1)0.021 (3)0.015 (3)0.015 (3)0.003 (2)0.006 (2)0.004 (2)
N(2)0.013 (2)0.013 (2)0.017 (3)0.001 (2)0.003 (2)0.001 (2)
N(3)0.015 (3)0.017 (3)0.016 (3)0.004 (2)0.000 (2)0.001 (2)
C(1)0.023 (4)0.018 (4)0.029 (4)0.004 (3)0.010 (3)0.001 (3)
C(2)0.015 (3)0.019 (3)0.023 (3)0.003 (2)0.001 (3)0.002 (3)
C(3)0.026 (4)0.034 (4)0.028 (4)0.008 (3)0.002 (3)0.014 (3)
C(4)0.024 (4)0.022 (4)0.027 (4)0.004 (3)0.009 (3)0.006 (3)
C(5)0.028 (4)0.025 (4)0.037 (5)0.002 (3)0.014 (3)0.008 (3)
C(6)0.038 (4)0.021 (4)0.023 (4)0.014 (3)0.005 (3)0.008 (3)
C(7)0.036 (4)0.023 (4)0.034 (4)0.018 (3)0.012 (4)0.013 (3)
C(8)0.029 (4)0.025 (4)0.015 (3)0.010 (3)0.005 (3)0.007 (3)
C(9)0.019 (3)0.029 (4)0.031 (4)0.000 (3)0.005 (3)0.009 (3)
C(10)0.016 (3)0.021 (4)0.025 (4)0.003 (3)0.001 (3)0.003 (3)
C(11)0.019 (3)0.023 (4)0.035 (4)0.005 (3)0.009 (3)0.016 (3)
C(12)0.022 (4)0.022 (4)0.027 (4)0.004 (3)0.011 (3)0.000 (3)
Geometric parameters (Å, º) top
Co(1)—O(1)1.877 (5)N(3)—C(11)1.491 (10)
Co(1)—O(2)1.903 (5)N(3)—C(12)1.484 (12)
Co(1)—O(4)1.941 (5)C(1)—C(3)1.511 (14)
Co(1)—O(5)1.932 (5)C(2)—C(4)1.511 (10)
Co(1)—O(7)1.894 (5)C(5)—C(7)1.499 (14)
Co(1)—N(1)1.923 (6)C(6)—C(8)1.503 (11)
Co(2)—O(1)1.888 (4)C(9)—C(11)1.498 (14)
Co(2)—O(2)1.907 (5)C(10)—C(12)1.518 (10)
Co(2)—O(3)1.895 (5)O(2)—H(16)0.842
Co(2)—O(9)1.918 (5)O(3)—H(17)0.843
Co(2)—O(11)1.904 (5)O(4)—H(18)0.842
Co(2)—N(2)1.943 (6)O(17)—H(19)0.841
Co(3)—Ca(1)3.466 (2)O(17)—H(20)0.844
Co(3)—O(1)1.866 (5)O(18)—H(21)0.840
Co(3)—O(3)1.915 (5)O(18)—H(22)0.840
Co(3)—O(4)1.921 (5)O(19)—H(23)0.840
Co(3)—O(13)1.913 (6)O(19)—H(24)0.839
Co(3)—O(15)1.897 (5)O(20)—H(25)0.840
Co(3)—N(3)1.936 (6)O(20)—H(26)0.840
Ca(1)—O(2)2.572 (6)O(21)—H(27)0.840
Ca(1)—O(3)2.527 (6)O(21)—H(28)0.840
Ca(1)—O(4)2.429 (5)O(22)—H(29)0.837
Ca(1)—O(17)2.355 (6)O(22)—H(30)0.839
Ca(1)—O(18)2.411 (6)O(23)—H(31)0.837
Ca(1)—O(19)2.543 (6)O(23)—H(32)0.836
Ca(1)—O(20)2.406 (6)O(24)—H(33)0.775
Ca(1)—O(21)2.471 (8)O(24)—H(34)0.809
O(5)—C(1)1.280 (9)N(1)—H(1)0.910
O(6)—C(1)1.249 (10)N(2)—H(2)0.910
O(7)—C(2)1.292 (11)N(3)—H(3)0.910
O(8)—C(2)1.220 (10)C(3)—H(4)0.951
O(9)—C(5)1.267 (10)C(3)—H(5)0.951
O(10)—C(5)1.227 (11)C(4)—H(6)0.951
O(11)—C(6)1.288 (12)C(4)—H(7)0.947
O(12)—C(6)1.215 (13)C(7)—H(8)0.951
O(13)—C(9)1.287 (9)C(7)—H(9)0.950
O(14)—C(9)1.219 (12)C(8)—H(10)0.952
O(15)—C(10)1.288 (11)C(8)—H(11)0.950
O(16)—C(10)1.234 (12)C(11)—H(12)0.951
N(1)—C(3)1.477 (10)C(11)—H(13)0.948
N(1)—C(4)1.485 (12)C(12)—H(14)0.951
N(2)—C(7)1.475 (10)C(12)—H(15)0.951
N(2)—C(8)1.489 (12)
O(1)—Co(1)—O(2)83.4 (2)Co(2)—O(11)—C(6)113.5 (4)
O(1)—Co(1)—O(4)82.8 (2)Co(3)—O(13)—C(9)115.3 (6)
O(1)—Co(1)—O(5)175.6 (2)Co(3)—O(15)—C(10)113.6 (4)
O(1)—Co(1)—O(7)93.8 (2)Co(1)—N(1)—C(3)110.3 (6)
O(1)—Co(1)—N(1)93.2 (2)Co(1)—N(1)—C(4)107.1 (4)
O(2)—Co(1)—O(4)85.6 (2)C(3)—N(1)—C(4)115.2 (6)
O(2)—Co(1)—O(5)92.3 (2)Co(2)—N(2)—C(7)109.6 (5)
O(2)—Co(1)—O(7)176.1 (2)Co(2)—N(2)—C(8)104.6 (4)
O(2)—Co(1)—N(1)97.0 (2)C(7)—N(2)—C(8)115.1 (6)
O(4)—Co(1)—O(5)97.9 (2)Co(3)—N(3)—C(11)108.5 (5)
O(4)—Co(1)—O(7)91.4 (2)Co(3)—N(3)—C(12)105.2 (4)
O(4)—Co(1)—N(1)175.0 (2)C(11)—N(3)—C(12)111.8 (6)
O(5)—Co(1)—O(7)90.5 (2)O(5)—C(1)—O(6)123.4 (8)
O(5)—Co(1)—N(1)86.3 (2)O(5)—C(1)—C(3)117.9 (7)
O(7)—Co(1)—N(1)85.8 (2)O(6)—C(1)—C(3)118.7 (7)
O(1)—Co(2)—O(2)82.9 (2)O(7)—C(2)—O(8)122.9 (7)
O(1)—Co(2)—O(3)82.7 (2)O(7)—C(2)—C(4)114.9 (6)
O(1)—Co(2)—O(9)175.7 (2)O(8)—C(2)—C(4)122.2 (8)
O(1)—Co(2)—O(11)91.0 (2)N(1)—C(3)—C(1)110.2 (7)
O(1)—Co(2)—N(2)96.5 (2)N(1)—C(4)—C(2)109.2 (7)
O(2)—Co(2)—O(3)84.0 (2)O(9)—C(5)—O(10)124.4 (9)
O(2)—Co(2)—O(9)94.7 (2)O(9)—C(5)—C(7)117.0 (7)
O(2)—Co(2)—O(11)94.9 (2)O(10)—C(5)—C(7)118.4 (8)
O(2)—Co(2)—N(2)179.2 (2)O(11)—C(6)—O(12)125.5 (8)
O(3)—Co(2)—O(9)93.4 (2)O(11)—C(6)—C(8)115.3 (8)
O(3)—Co(2)—O(11)173.8 (2)O(12)—C(6)—C(8)119.1 (9)
O(3)—Co(2)—N(2)96.4 (2)N(2)—C(7)—C(5)111.7 (7)
O(9)—Co(2)—O(11)92.8 (2)N(2)—C(8)—C(6)109.6 (7)
O(9)—Co(2)—N(2)86.0 (2)O(13)—C(9)—O(14)123.7 (9)
O(11)—Co(2)—N(2)84.6 (2)O(13)—C(9)—C(11)116.2 (7)
Ca(1)—Co(3)—O(1)93.60 (17)O(14)—C(9)—C(11)120.2 (7)
Ca(1)—Co(3)—O(3)45.55 (17)O(15)—C(10)—O(16)124.6 (7)
Ca(1)—Co(3)—O(4)42.59 (16)O(15)—C(10)—C(12)114.8 (7)
Ca(1)—Co(3)—O(13)82.93 (19)O(16)—C(10)—C(12)120.6 (8)
Ca(1)—Co(3)—O(15)139.35 (16)N(3)—C(11)—C(9)112.4 (6)
Ca(1)—Co(3)—N(3)136.5 (2)N(3)—C(12)—C(10)107.0 (7)
O(1)—Co(3)—O(3)82.8 (2)Co(1)—O(2)—H(16)117.0
O(1)—Co(3)—O(4)83.6 (2)Co(2)—O(2)—H(16)116.9
O(1)—Co(3)—O(13)176.3 (2)Ca(1)—O(2)—H(16)117.0
O(1)—Co(3)—O(15)90.4 (2)Co(2)—O(3)—H(17)116.3
O(1)—Co(3)—N(3)96.7 (2)Co(3)—O(3)—H(17)116.2
O(3)—Co(3)—O(4)85.1 (2)Ca(1)—O(3)—H(17)116.2
O(3)—Co(3)—O(13)93.8 (2)Co(1)—O(4)—H(18)116.3
O(3)—Co(3)—O(15)95.2 (2)Co(3)—O(4)—H(18)116.3
O(3)—Co(3)—N(3)177.9 (2)Ca(1)—O(4)—H(18)116.4
O(4)—Co(3)—O(13)94.6 (2)Ca(1)—O(17)—H(19)109.5
O(4)—Co(3)—O(15)174.0 (2)Ca(1)—O(17)—H(20)133.3
O(4)—Co(3)—N(3)96.9 (2)H(19)—O(17)—H(20)117.1
O(13)—Co(3)—O(15)91.3 (2)Ca(1)—O(18)—H(21)109.5
O(13)—Co(3)—N(3)86.8 (2)Ca(1)—O(18)—H(22)109.5
O(15)—Co(3)—N(3)82.8 (2)H(21)—O(18)—H(22)109.4
Co(3)—Ca(1)—O(2)64.34 (12)Ca(1)—O(19)—H(23)109.4
Co(3)—Ca(1)—O(3)32.76 (10)Ca(1)—O(19)—H(24)109.4
Co(3)—Ca(1)—O(4)32.37 (12)H(23)—O(19)—H(24)109.6
Co(3)—Ca(1)—O(17)111.7 (2)Ca(1)—O(20)—H(25)109.5
Co(3)—Ca(1)—O(18)74.12 (19)Ca(1)—O(20)—H(26)109.5
Co(3)—Ca(1)—O(19)97.28 (16)H(25)—O(20)—H(26)109.5
Co(3)—Ca(1)—O(20)121.95 (18)Ca(1)—O(21)—H(27)109.4
Co(3)—Ca(1)—O(21)153.06 (16)Ca(1)—O(21)—H(28)109.4
O(2)—Ca(1)—O(3)59.84 (16)H(27)—O(21)—H(28)109.5
O(2)—Ca(1)—O(4)62.91 (17)H(29)—O(22)—H(30)84.2
O(2)—Ca(1)—O(17)78.2 (2)H(31)—O(23)—H(32)93.0
O(2)—Ca(1)—O(18)132.2 (2)H(33)—O(24)—H(34)105.7
O(2)—Ca(1)—O(19)128.8 (2)Co(1)—N(1)—H(1)108.0
O(2)—Ca(1)—O(20)75.0 (2)C(3)—N(1)—H(1)108.1
O(2)—Ca(1)—O(21)141.50 (19)C(4)—N(1)—H(1)107.9
O(3)—Ca(1)—O(4)63.09 (16)Co(2)—N(2)—H(2)109.1
O(3)—Ca(1)—O(17)79.3 (2)C(7)—N(2)—H(2)109.1
O(3)—Ca(1)—O(18)72.5 (2)C(8)—N(2)—H(2)109.2
O(3)—Ca(1)—O(19)126.86 (18)Co(3)—N(3)—H(3)110.4
O(3)—Ca(1)—O(20)134.5 (2)C(11)—N(3)—H(3)110.3
O(3)—Ca(1)—O(21)139.57 (19)C(12)—N(3)—H(3)110.5
O(4)—Ca(1)—O(17)135.4 (2)N(1)—C(3)—H(4)109.3
O(4)—Ca(1)—O(18)93.7 (2)N(1)—C(3)—H(5)109.3
O(4)—Ca(1)—O(19)76.6 (2)C(1)—C(3)—H(4)109.3
O(4)—Ca(1)—O(20)92.9 (2)C(1)—C(3)—H(5)109.3
O(4)—Ca(1)—O(21)148.6 (2)H(4)—C(3)—H(5)109.4
O(17)—Ca(1)—O(18)97.1 (2)N(1)—C(4)—H(6)109.5
O(17)—Ca(1)—O(19)148.0 (2)N(1)—C(4)—H(7)109.7
O(17)—Ca(1)—O(20)97.6 (2)C(2)—C(4)—H(6)109.3
O(17)—Ca(1)—O(21)76.0 (2)C(2)—C(4)—H(7)109.5
O(18)—Ca(1)—O(19)77.4 (2)H(6)—C(4)—H(7)109.6
O(18)—Ca(1)—O(20)151.5 (2)N(2)—C(7)—H(8)108.7
O(18)—Ca(1)—O(21)79.4 (2)N(2)—C(7)—H(9)108.8
O(19)—Ca(1)—O(20)77.2 (2)C(5)—C(7)—H(8)109.0
O(19)—Ca(1)—O(21)72.0 (2)C(5)—C(7)—H(9)109.1
O(20)—Ca(1)—O(21)80.6 (2)H(8)—C(7)—H(9)109.4
Co(1)—O(1)—Co(2)97.1 (2)N(2)—C(8)—H(10)109.5
Co(1)—O(1)—Co(3)98.6 (2)N(2)—C(8)—H(11)109.6
Co(2)—O(1)—Co(3)97.7 (2)C(6)—C(8)—H(10)109.4
Co(1)—O(2)—Co(2)95.6 (2)C(6)—C(8)—H(11)109.5
Co(1)—O(2)—Ca(1)101.5 (2)H(10)—C(8)—H(11)109.3
Co(2)—O(2)—Ca(1)105.8 (2)N(3)—C(11)—H(12)108.6
Co(2)—O(3)—Co(3)95.8 (2)N(3)—C(11)—H(13)108.8
Co(2)—O(3)—Ca(1)107.9 (2)C(9)—C(11)—H(12)108.7
Co(3)—O(3)—Ca(1)101.7 (2)C(9)—C(11)—H(13)108.8
Co(1)—O(4)—Co(3)94.5 (2)H(12)—C(11)—H(13)109.6
Co(1)—O(4)—Ca(1)105.5 (2)N(3)—C(12)—H(14)110.2
Co(3)—O(4)—Ca(1)105.0 (2)N(3)—C(12)—H(15)110.3
Co(1)—O(5)—C(1)113.7 (5)C(10)—C(12)—H(14)110.0
Co(1)—O(7)—C(2)115.1 (4)C(10)—C(12)—H(15)110.0
Co(2)—O(9)—C(5)115.6 (6)H(14)—C(12)—H(15)109.4
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O(2)—H(16)···O(22)i0.841.882.707 (7)168
O(3)—H(17)···O(23)0.841.882.677 (7)159
O(4)—H(18)···O(8)ii0.842.072.870 (7)158
O(17)—H(19)···O(9)0.841.922.744 (11)168
O(17)—H(20)···O(10)iii0.842.102.850 (13)148
O(18)—H(21)···O(14)iv0.841.872.699 (12)168
O(18)—H(22)···O(13)0.842.002.708 (9)141
O(19)—H(23)···O(6)v0.842.212.829 (9)131
O(19)—H(24)···O(8)ii0.842.142.863 (9)145
O(20)—H(25)···O(5)0.842.172.787 (9)130
O(20)—H(26)···O(6)v0.842.152.765 (10)130
O(21)—H(27)···O(14)iv0.842.343.043 (9)142
O(21)—H(28)···O(10)iii0.841.992.801 (9)164
O(22)—H(29)···O(12)vi0.842.042.800 (9)152
O(22)—H(30)···O(16)0.842.072.840 (10)153
O(23)—H(31)···O(18)0.842.402.909 (10)120
O(23)—H(31)···O(24)0.842.243.01 (2)153
O(23)—H(32)···O(16)vii0.841.972.802 (8)172
O(24)—H(33)···O(14)iv0.782.192.912 (18)156
O(24)—H(34)···O(10)iii0.812.533.054 (18)124
N(1)—H(1)···O(11)0.912.032.857 (7)150
N(1)—H(1)···O(22)vi0.912.553.121 (9)122
N(2)—H(2)···O(15)0.912.182.917 (7)138
N(2)—H(2)···O(23)vii0.912.362.977 (9)125
N(3)—H(3)···O(7)0.912.363.038 (7)132
N(3)—H(3)···O(7)ii0.912.493.259 (8)143
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z+2; (iii) x+2, y+2, z+1; (iv) x+1, y+1, z+1; (v) x+2, y+1, z+2; (vi) x+1, y+2, z+2; (vii) x+1, y+2, z+1.

Experimental details

Crystal data
Chemical formula[CaCo3(C4H5NO4)3(OH)3O(H2O)5]·2.54H2O
Mr812.92
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)10.474 (3), 11.303 (7), 12.588 (5)
α, β, γ (°)75.88 (4), 100.92 (3), 104.58 (3)
V3)1385.6 (10)
Z2
Radiation typeMo Kα
µ (mm1)2.06
Crystal size (mm)0.40 × 0.40 × 0.05
Data collection
DiffractometerRigaku AFC-7S
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.673, 0.902
No. of measured, independent and
observed [F2 > 2σ(F2)] reflections
6713, 6360, 3290
Rint0.076
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.060, 0.207, 1.00
No. of reflections6360
No. of parameters389
No. of restraints?
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.17, 1.13

Computer programs: WinAFC (Rigaku/MSC, 2000), CrystalStructure (Rigaku/MSC, 2007), DIRDIF99 (Beurskens et al., 1999), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997).

Selected geometric parameters (Å, º) top
Co(1)—O(1)1.877 (5)Ca(1)—O(2)2.572 (6)
Co(1)—O(2)1.903 (5)Ca(1)—O(3)2.527 (6)
Co(1)—O(4)1.941 (5)Ca(1)—O(4)2.429 (5)
Co(2)—O(1)1.888 (4)Ca(1)—O(17)2.355 (6)
Co(2)—O(2)1.907 (5)Ca(1)—O(18)2.411 (6)
Co(2)—O(3)1.895 (5)Ca(1)—O(19)2.543 (6)
Co(3)—O(1)1.866 (5)Ca(1)—O(20)2.406 (6)
Co(3)—O(3)1.915 (5)Ca(1)—O(21)2.471 (8)
Co(3)—O(4)1.921 (5)
O(1)—Co(1)—O(2)83.4 (2)Co(1)—O(1)—Co(2)97.1 (2)
O(1)—Co(1)—O(4)82.8 (2)Co(1)—O(1)—Co(3)98.6 (2)
O(2)—Co(1)—O(4)85.6 (2)Co(2)—O(1)—Co(3)97.7 (2)
O(1)—Co(2)—O(2)82.9 (2)Co(1)—O(2)—Co(2)95.6 (2)
O(1)—Co(2)—O(3)82.7 (2)Co(1)—O(2)—Ca(1)101.5 (2)
O(2)—Co(2)—O(3)84.0 (2)Co(2)—O(2)—Ca(1)105.8 (2)
O(1)—Co(3)—O(3)82.8 (2)Co(2)—O(3)—Co(3)95.8 (2)
O(1)—Co(3)—O(4)83.6 (2)Co(2)—O(3)—Ca(1)107.9 (2)
O(3)—Co(3)—O(4)85.1 (2)Co(3)—O(3)—Ca(1)101.7 (2)
O(2)—Ca(1)—O(3)59.84 (16)Co(1)—O(4)—Co(3)94.5 (2)
O(2)—Ca(1)—O(4)62.91 (17)Co(1)—O(4)—Ca(1)105.5 (2)
O(3)—Ca(1)—O(4)63.09 (16)Co(3)—O(4)—Ca(1)105.0 (2)
 

Acknowledgements

The authors are grateful to Kochi University for financial support.

References

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Volume 66| Part 4| April 2010| Pages m483-m484
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