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A zinc(II) coordination discrete complex, [Zn4(pydc)4(H2O)8] (pydc = 2,5-pyridine­di­carboxyl­ate, C7H3NO4), has been pre­pared from the hydro­thermal reaction of [Zn(CH3COO)2]·2H2O and H2pydc in H2O. The complex exhibits a rectangular structure formed from four zinc(II) and four pydc bridging ligands. The rectangular structure is interconnected by hydrogen bonds to form a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801004184/bt6022sup1.cif
Contains datablocks Zn4-2, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801004184/bt6022Isup2.hkl
Contains datablock I

CCDC reference: 156029

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.041
  • wR factor = 0.121
  • Data-to-parameter ratio = 10.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry
Yellow Alert Alert Level C:
PLAT_731 Alert C Bond Calc 0.94(5), Rep 0.94(2) .... 2.50 s.u-Ratio O1 -H1B 1.555 1.555 PLAT_731 Alert C Bond Calc 0.96(5), Rep 0.95(2) .... 2.50 s.u-Ratio O3 -H3A 1.555 1.555 PLAT_731 Alert C Bond Calc 0.94(5), Rep 0.94(2) .... 2.50 s.u-Ratio O4 -H4A 1.555 1.555 PLAT_731 Alert C Bond Calc 0.94(5), Rep 0.94(2) .... 2.50 s.u-Ratio O4 -H4B 1.555 1.555 PLAT_735 Alert C D-H Calc 0.94(5), Rep 0.94(2) .... 2.50 s.u-Ratio O1 -H1B 1.555 1.555 General Notes
GOODF_01 _refine_ls_goodness_of_fit_obs is an old dataname which has been superseded by _refine_ls_goodness_of_fit_ref RFACG_01 _refine_ls_R_factor_obs is an old dataname which has been superseded by _refine_ls_R_factor_gt
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
5 Alert Level C = Please check

Comment top

In the last few years, much effort has been devoted to the use of transition metal ions with exo-bidentate ligands, such as polypyridyl or pyrazines and 1,4-benzenedicarboxylate, to generate polymeric metal–organic coordination polymers with two- or three-dimensional networks. Very recently, Goodgame and Williams reported a new type of metal–organic large-pore zeotype, i.e. [Zn(dimto)2]n.nDMF [dimto = 2,4,6-tri(1-imidazolyl)-1,3,5-triazin-2-one], which was generated from zinc bromide and 2,4,6-tri(1-imidazolyl)-1,3,5-triazine (timt) (Goodgame et al., 1999). Li et al. (1999) reported a porous polymer, [{Zn4O(bdc)3}(dmf)8(C6H5Cl)]n (bdc = 1,4-benzenedicarboxylate), which could absorb and disabsorb nitrogen gas. Several infinite two- and three-dimensional coordination polymers with 1,4-benzenedicarboxylate as a bridging ligand have been prepared (Hagrman et al., 1999; Li et al., 1998; Groenman et al., 1999). However, reports on coordination polymers based on a metal cluster framework have not received much attention in this respect, although several three-dimensional polymers consisting of a metal oxide interconnected by organic molecules have been reported (Liang et al., 2000). Herein we report a coordination complex, [Zn4(pydc)4(H2O)8] (pydc = pyridine-2,4-dicarboxylate), (I), prepared from hydrothermal reaction of [Zn(CH3COO)2]·2H2O and H2pydc in H2O.

Crystallographic analysis reveals that the compound is a discrete [Zn4(pydc)4((H2O)8)] molecule, in which the four Zn atoms are connected by four pydc ligands through bridges forming a rectangular structure, as shown in Fig. 1. The molecules are connected by hydrogen-bonding interactions involving the carboxylate groups and H2O, with an average O···O distance of 2.708 Å, to form a three-dimensional network, as shown in Fig. 2. The coordination environment of the zinc centre in the complex is distorted bipyramidal {ZnO4N}, of which one N atom and two O atoms are from the pydc ligand and the other two O atoms are from water molecules. Zn—O bond lengths are in the range 1.985 (4)–2.107 (3) Å and the Zn—N distances range from 2.070 (4) to 2.113 (3) Å.

Experimental top

A mixture of [Zn(CH3COO)2]·2H2O (0.220 g, 1.0 mmol), H2pydc (0.167 g, 1.0 mmol), and H2O (16 ml) in a molar ratio of ca 1:1:890 was sealed in a 25 ml stainless-steel reactor with a Teflon liner. The reaction system was heated at 443 K for 72 h. Slow cooling to room temperature yielded prismatic colourless crystals of the complex, which were collected by filtration.

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXTL (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The structure of [Zn4(pydc)4(H2O)8]. Displacement ellipsoids are plotted at the 50% probability level.
[Figure 2] Fig. 2. Packing diagram of [Zn4(pydc)4(H2O)8].
Tetra(2,4-pyridinedicarboxylate)terazinc(II) octa-hydtate top
Crystal data top
[Zn4(C7H3NO4)4(H2O)8]Z = 1
Mr = 1066.02F(000) = 536
Triclinic, P1Dx = 2.061 Mg m3
a = 7.0512 (6) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.3853 (6) ÅCell parameters from 423 reflections
c = 18.4652 (14) Åθ = 8.1–19.6°
α = 90.022 (1)°µ = 2.87 mm1
β = 96.985 (1)°T = 293 K
γ = 115.630 (1)°Prism, colorless
V = 859.02 (12) Å30.36 × 0.18 × 0.12 mm
Data collection top
SMART CCD
diffractometer
3021 independent reflections
Radiation source: fine-focus sealed tube2472 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 25.0°, θmin = 1.1°
Absorption correction: empirical (using intensity measurements)
(SHELXTL; Sheldrick, 1997)
h = 88
Tmin = 0.350, Tmax = 0.709k = 88
4717 measured reflectionsl = 2115
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0701P)2 + 0.0949P]
where P = (Fo2 + 2Fc2)/3
3021 reflections(Δ/σ)max < 0.001
303 parametersΔρmax = 0.56 e Å3
8 restraintsΔρmin = 1.22 e Å3
Crystal data top
[Zn4(C7H3NO4)4(H2O)8]γ = 115.630 (1)°
Mr = 1066.02V = 859.02 (12) Å3
Triclinic, P1Z = 1
a = 7.0512 (6) ÅMo Kα radiation
b = 7.3853 (6) ŵ = 2.87 mm1
c = 18.4652 (14) ÅT = 293 K
α = 90.022 (1)°0.36 × 0.18 × 0.12 mm
β = 96.985 (1)°
Data collection top
SMART CCD
diffractometer
3021 independent reflections
Absorption correction: empirical (using intensity measurements)
(SHELXTL; Sheldrick, 1997)
2472 reflections with I > 2σ(I)
Tmin = 0.350, Tmax = 0.709Rint = 0.028
4717 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0418 restraints
wR(F2) = 0.121H-atom parameters constrained
S = 1.07Δρmax = 0.56 e Å3
3021 reflectionsΔρmin = 1.22 e Å3
303 parameters
Special details top

Experimental. Empirical, from equivalent reflections (XEMP in SHELXTL; Sheldrick, 1997)

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
Zn10.27843 (9)0.13833 (7)0.05025 (3)0.02636 (18)
Zn20.57964 (9)0.79994 (8)0.39562 (3)0.02935 (19)
N10.2795 (6)0.1124 (5)0.16422 (18)0.0219 (8)
N20.7047 (6)0.9451 (5)0.30478 (19)0.0253 (8)
O10.7844 (6)0.7231 (6)0.45521 (18)0.0416 (9)
H1A0.785 (12)0.716 (11)0.5062 (13)0.09 (2)*
H1B0.799 (10)0.614 (6)0.435 (3)0.057 (18)*
O20.3144 (6)0.7370 (5)0.44082 (18)0.0395 (9)
H2A0.211 (9)0.601 (4)0.439 (4)0.08 (2)*
H2B0.322 (9)0.780 (8)0.4903 (14)0.052 (17)*
O30.5901 (5)0.3039 (5)0.04700 (17)0.0307 (7)
H3A0.627 (11)0.272 (11)0.002 (2)0.08 (2)*
H3B0.647 (10)0.443 (4)0.061 (3)0.07 (2)*
O40.1629 (5)0.3482 (5)0.03985 (17)0.0287 (7)
H4A0.025 (5)0.267 (8)0.016 (3)0.07 (2)*
H4B0.184 (10)0.440 (8)0.079 (2)0.07 (2)*
O110.2355 (5)0.1605 (4)0.06091 (16)0.0282 (7)
O120.1757 (6)0.3988 (4)0.14164 (17)0.0346 (8)
O130.4206 (6)0.5477 (5)0.32736 (17)0.0371 (8)
O140.2449 (7)0.3192 (5)0.40287 (18)0.0494 (10)
O210.6866 (6)1.1036 (5)0.43001 (17)0.0350 (8)
O220.8344 (6)1.4171 (5)0.39177 (19)0.0441 (9)
O230.8197 (6)0.9530 (5)0.05646 (16)0.0339 (8)
O240.6767 (7)0.6620 (5)0.11002 (18)0.0464 (10)
C110.2133 (7)0.2254 (6)0.1247 (2)0.0238 (9)
C120.2323 (7)0.0770 (6)0.1846 (2)0.0211 (9)
C130.2049 (7)0.1326 (6)0.2554 (2)0.0247 (9)
H13A0.17290.26380.26760.030*
C140.2260 (7)0.0119 (7)0.3079 (2)0.0279 (10)
H14A0.20240.02270.35560.033*
C150.2826 (7)0.2077 (6)0.2887 (2)0.0233 (9)
C160.3079 (7)0.2515 (6)0.2163 (2)0.0226 (9)
H16A0.34620.38330.20340.027*
C170.3199 (7)0.3703 (7)0.3452 (2)0.0257 (10)
C210.7631 (7)1.2324 (7)0.3825 (2)0.0284 (10)
C220.7662 (7)1.1460 (6)0.3084 (2)0.0237 (9)
C230.8207 (8)1.2586 (7)0.2488 (2)0.0283 (10)
H23A0.86001.39610.25250.034*
C240.8167 (7)1.1657 (6)0.1832 (2)0.0259 (10)
H24A0.85221.23980.14210.031*
C250.7590 (7)0.9604 (6)0.1794 (2)0.0219 (9)
C260.7034 (7)0.8561 (6)0.2419 (2)0.0215 (9)
H26A0.66370.71840.23980.026*
C270.7501 (7)0.8464 (7)0.1098 (2)0.0254 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0400 (3)0.0193 (3)0.0189 (3)0.0111 (2)0.0082 (2)0.0004 (2)
Zn20.0468 (4)0.0257 (3)0.0198 (3)0.0182 (3)0.0104 (2)0.0007 (2)
N10.0238 (19)0.0204 (18)0.0225 (19)0.0097 (16)0.0071 (15)0.0027 (14)
N20.030 (2)0.0221 (19)0.0244 (19)0.0116 (16)0.0064 (15)0.0015 (15)
O10.068 (3)0.045 (2)0.0269 (19)0.039 (2)0.0076 (17)0.0002 (16)
O20.055 (2)0.0274 (19)0.0306 (19)0.0087 (18)0.0211 (17)0.0044 (15)
O30.0380 (19)0.0250 (17)0.0269 (18)0.0104 (15)0.0099 (14)0.0001 (14)
O40.0324 (19)0.0255 (17)0.0287 (17)0.0124 (15)0.0063 (14)0.0036 (14)
O110.043 (2)0.0199 (15)0.0228 (16)0.0135 (15)0.0102 (14)0.0012 (12)
O120.059 (2)0.0181 (17)0.0318 (18)0.0193 (16)0.0131 (16)0.0024 (13)
O130.061 (2)0.0226 (17)0.0258 (17)0.0140 (17)0.0159 (16)0.0021 (13)
O140.073 (3)0.039 (2)0.0266 (19)0.012 (2)0.0233 (18)0.0019 (16)
O210.051 (2)0.0284 (18)0.0263 (17)0.0155 (16)0.0140 (15)0.0031 (14)
O220.069 (3)0.0249 (18)0.040 (2)0.0176 (18)0.0211 (18)0.0048 (15)
O230.052 (2)0.0257 (17)0.0174 (15)0.0099 (16)0.0089 (14)0.0002 (13)
O240.078 (3)0.0236 (19)0.0313 (19)0.0126 (19)0.0226 (18)0.0009 (14)
C110.026 (2)0.021 (2)0.024 (2)0.0103 (19)0.0026 (18)0.0022 (18)
C120.020 (2)0.015 (2)0.027 (2)0.0068 (17)0.0036 (17)0.0016 (16)
C130.029 (2)0.020 (2)0.027 (2)0.0113 (19)0.0070 (18)0.0046 (17)
C140.034 (3)0.030 (2)0.021 (2)0.014 (2)0.0059 (19)0.0051 (19)
C150.025 (2)0.021 (2)0.023 (2)0.0094 (19)0.0043 (17)0.0012 (17)
C160.028 (2)0.020 (2)0.021 (2)0.0103 (19)0.0077 (17)0.0007 (17)
C170.031 (3)0.028 (2)0.020 (2)0.014 (2)0.0043 (18)0.0022 (18)
C210.031 (3)0.027 (2)0.029 (2)0.013 (2)0.0076 (19)0.0027 (19)
C220.024 (2)0.022 (2)0.028 (2)0.0111 (19)0.0070 (18)0.0014 (18)
C230.035 (3)0.020 (2)0.031 (3)0.011 (2)0.010 (2)0.0021 (18)
C240.027 (2)0.023 (2)0.028 (2)0.0085 (19)0.0112 (19)0.0062 (18)
C250.022 (2)0.023 (2)0.019 (2)0.0075 (18)0.0036 (16)0.0025 (17)
C260.026 (2)0.021 (2)0.019 (2)0.0107 (19)0.0075 (17)0.0005 (17)
C270.031 (3)0.023 (2)0.021 (2)0.011 (2)0.0064 (18)0.0002 (18)
Geometric parameters (Å, º) top
Zn1—O32.009 (3)O14—C171.233 (5)
Zn1—O23i2.020 (3)O21—C211.280 (6)
Zn1—O42.039 (3)O22—C211.236 (5)
Zn1—O112.107 (3)O23—C271.270 (5)
Zn1—N12.113 (3)O23—Zn1i2.020 (3)
Zn2—O11.985 (4)O24—C271.230 (5)
Zn2—O22.010 (4)C11—C121.510 (6)
Zn2—O132.040 (3)C12—C131.380 (6)
Zn2—N22.070 (4)C13—C141.389 (6)
Zn2—O212.103 (3)C13—H13A0.9300
N1—C161.340 (5)C14—C151.383 (6)
N1—C121.355 (5)C14—H14A0.9300
N2—C261.331 (5)C15—C161.389 (6)
N2—C221.353 (6)C15—C171.504 (6)
O1—H1A0.94 (2)C16—H16A0.9300
O1—H1B0.94 (2)C21—C221.517 (6)
O2—H2A0.95 (2)C22—C231.369 (6)
O2—H2B0.95 (2)C23—C241.384 (6)
O3—H3A0.95 (2)C23—H23A0.9300
O3—H3B0.95 (2)C24—C251.389 (6)
O4—H4A0.94 (2)C24—H24A0.9300
O4—H4B0.94 (2)C25—C261.389 (6)
O11—C111.274 (5)C25—C271.517 (6)
O12—C111.239 (5)C26—H26A0.9300
O13—C171.258 (5)
O3—Zn1—O23i99.90 (14)O12—C11—O11126.0 (4)
O3—Zn1—O4102.40 (13)O12—C11—C12117.4 (4)
O23i—Zn1—O491.22 (13)O11—C11—C12116.6 (4)
O3—Zn1—O11106.09 (13)N1—C12—C13122.9 (4)
O23i—Zn1—O1183.20 (12)N1—C12—C11115.5 (4)
O4—Zn1—O11151.49 (14)C13—C12—C11121.5 (4)
O3—Zn1—N199.89 (13)C12—C13—C14118.5 (4)
O23i—Zn1—N1156.01 (14)C12—C13—H13A120.7
O4—Zn1—N197.65 (13)C14—C13—H13A120.7
O11—Zn1—N178.38 (12)C15—C14—C13119.2 (4)
O1—Zn2—O2113.39 (16)C15—C14—H14A120.4
O1—Zn2—O1399.80 (15)C13—C14—H14A120.4
O2—Zn2—O1389.91 (14)C14—C15—C16118.7 (4)
O1—Zn2—N2110.78 (16)C14—C15—C17120.6 (4)
O2—Zn2—N2135.66 (16)C16—C15—C17120.7 (4)
O13—Zn2—N286.40 (13)N1—C16—C15122.9 (4)
O1—Zn2—O21102.65 (15)N1—C16—H16A118.5
O2—Zn2—O2188.50 (14)C15—C16—H16A118.5
O13—Zn2—O21156.16 (14)O14—C17—O13126.3 (4)
N2—Zn2—O2178.25 (13)O14—C17—C15118.0 (4)
C16—N1—C12117.6 (4)O13—C17—C15115.7 (4)
C16—N1—Zn1129.2 (3)O22—C21—O21126.3 (4)
C12—N1—Zn1113.1 (3)O22—C21—C22118.1 (4)
C26—N2—C22118.7 (4)O21—C21—C22115.6 (4)
C26—N2—Zn2125.8 (3)N2—C22—C23122.0 (4)
C22—N2—Zn2114.9 (3)N2—C22—C21114.5 (4)
Zn2—O1—H1A120 (5)C23—C22—C21123.6 (4)
Zn2—O1—H1B115 (4)C22—C23—C24119.3 (4)
H1A—O1—H1B111 (6)C22—C23—H23A120.3
Zn2—O2—H2A119 (4)C24—C23—H23A120.3
Zn2—O2—H2B121 (4)C23—C24—C25119.1 (4)
H2A—O2—H2B101 (5)C23—C24—H24A120.4
Zn1—O3—H3A110 (4)C25—C24—H24A120.4
Zn1—O3—H3B117 (4)C26—C25—C24118.1 (4)
H3A—O3—H3B115 (6)C26—C25—C27119.2 (4)
Zn1—O4—H4A100 (4)C24—C25—C27122.6 (4)
Zn1—O4—H4B121 (4)N2—C26—C25122.7 (4)
H4A—O4—H4B120 (5)N2—C26—H26A118.7
C11—O11—Zn1115.9 (3)C25—C26—H26A118.7
C17—O13—Zn2127.2 (3)O24—C27—O23126.4 (4)
C21—O21—Zn2116.2 (3)O24—C27—C25117.6 (4)
C27—O23—Zn1i125.3 (3)O23—C27—C25115.9 (4)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O140.94 (2)3.53 (6)3.687 (6)92 (4)

Experimental details

Crystal data
Chemical formula[Zn4(C7H3NO4)4(H2O)8]
Mr1066.02
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.0512 (6), 7.3853 (6), 18.4652 (14)
α, β, γ (°)90.022 (1), 96.985 (1), 115.630 (1)
V3)859.02 (12)
Z1
Radiation typeMo Kα
µ (mm1)2.87
Crystal size (mm)0.36 × 0.18 × 0.12
Data collection
DiffractometerSMART CCD
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SHELXTL; Sheldrick, 1997)
Tmin, Tmax0.350, 0.709
No. of measured, independent and
observed [I > 2σ(I)] reflections
4717, 3021, 2472
Rint0.028
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.121, 1.07
No. of reflections3021
No. of parameters303
No. of restraints8
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.56, 1.22

Computer programs: SMART (Siemens, 1994), SMART, SHELXS97 (Sheldrick, 1990), SHELXTL (Sheldrick, 1997), SHELXTL.

Selected geometric parameters (Å, º) top
Zn1—O32.009 (3)Zn2—O11.985 (4)
Zn1—O23i2.020 (3)Zn2—O22.010 (4)
Zn1—O42.039 (3)Zn2—O132.040 (3)
Zn1—O112.107 (3)Zn2—N22.070 (4)
Zn1—N12.113 (3)Zn2—O212.103 (3)
O3—Zn1—O23i99.90 (14)O1—Zn2—O2113.39 (16)
O3—Zn1—O4102.40 (13)O1—Zn2—O1399.80 (15)
O23i—Zn1—O491.22 (13)O2—Zn2—O1389.91 (14)
O3—Zn1—O11106.09 (13)O1—Zn2—N2110.78 (16)
O23i—Zn1—O1183.20 (12)O2—Zn2—N2135.66 (16)
O4—Zn1—O11151.49 (14)O13—Zn2—N286.40 (13)
O3—Zn1—N199.89 (13)O1—Zn2—O21102.65 (15)
O23i—Zn1—N1156.01 (14)O2—Zn2—O2188.50 (14)
O4—Zn1—N197.65 (13)O13—Zn2—O21156.16 (14)
O11—Zn1—N178.38 (12)N2—Zn2—O2178.25 (13)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O140.94 (2)3.53 (6)3.687 (6)92 (4)
 

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