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The title compound, {(C3H12N2)[Al(OH)(HPO3)2]·H2O}n, has been prepared using a hydro­thermal technique and characterized by X-ray diffraction data. The Al atoms are in a distorted octa­hedral environment. Anions and cations are linked through O—H...O and N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807040512/bt2443sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807040512/bt2443Isup2.hkl
Contains datablock I

CCDC reference: 660152

Key indicators

  • Single-crystal X-ray study
  • T = 170 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.026
  • wR factor = 0.080
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.24 PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A .. O1# .. 2.66 Ang. PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6 O2 -AL1 -O3 -P1 -28.00 11.00 2.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 16 O7 -AL1 -O4 -P2 -170.00 2.00 2.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 18 O5 -AL1 -O5 -AL1 -118.60 1.00 2.655 1.555 1.555 2.645 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.19 Ratio
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C3 H17 Al1 N2 O8 P2 Atom count from _chemical_formula_moiety:C3 H17 Al1 N2 O8 P6 PLAT793_ALERT_1_G Check the Absolute Configuration of C2 = ... R PLAT794_ALERT_5_G Check Predicted Bond Valency for Al1 (3) 2.82 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

At present, it is well known that a remarkable range of compositions and structures of organically templated inorganic framework solids have been synthesized and studied, because of their potential applications in many fields (Cheetham et al., 1999; Harrison, 2002). There are also lots of studies about the synthesis and characterization of metal phosphates containing V, Zn, Co, etc. (Yamase et al., 1997) and most of the known metal–phosphite compounds have been prepared by various solvent-volatilizing methods. However, only a few organically templated aluminophosphites have been reported. In our present work, we have hydrothermally synthesized and characterized the title compound (Fig. 1).

As seen in Figs. 2 and 3, its structure consists of aluminophosphite lines constructed from AlO6 distorted octahedrons and HPO3 pyramids. Each AlO6 octahedron shares two opposite hydroxy groups with two adjacent AlO6 octahedra to construct an infinte Al—O—Al chain running along the [100] direction. Each P atom shares two oxygen atoms with adjacent Al atoms.

The propane-1,2-diammonium cations and water molecules link Al—O—Al chains via numerous N—H···O and O—H···O hydrogen bonds (Table 1 and Fig. 4).

Related literature top

For related literature, see: Cheetham et al. (1999); Harrison (2002); Yamase et al. (1997).

Experimental top

All reagents were used as purchased without further purification. The synthesis was carried out in a rational way from a mixture of [(CH3)2CHO]3Al, C3N2H10, H3PO3 and H2O in a molar ratio of 1:1:2:250. The mixture was loaded in a Teflon-lined autoclave (23 ml capacity) and was heated at 443k for 4 d under autogenous pressure. The solid product was collected by filtration, washed with water and dried at room temperature. Colorless crystals of the title compound were isolated.

Refinement top

All H atoms were located in a difference Fourier map. Those bonded to C and N were refined using a riding model with C—H ranging from 0.96 to 0.97Å and N—H = 0.89Å and U(H)= 1.2 Ueq(C,N). The other H atoms were isotropically refined. The distance O5—H1 was restrained to 0.82 (2) Å.

Structure description top

At present, it is well known that a remarkable range of compositions and structures of organically templated inorganic framework solids have been synthesized and studied, because of their potential applications in many fields (Cheetham et al., 1999; Harrison, 2002). There are also lots of studies about the synthesis and characterization of metal phosphates containing V, Zn, Co, etc. (Yamase et al., 1997) and most of the known metal–phosphite compounds have been prepared by various solvent-volatilizing methods. However, only a few organically templated aluminophosphites have been reported. In our present work, we have hydrothermally synthesized and characterized the title compound (Fig. 1).

As seen in Figs. 2 and 3, its structure consists of aluminophosphite lines constructed from AlO6 distorted octahedrons and HPO3 pyramids. Each AlO6 octahedron shares two opposite hydroxy groups with two adjacent AlO6 octahedra to construct an infinte Al—O—Al chain running along the [100] direction. Each P atom shares two oxygen atoms with adjacent Al atoms.

The propane-1,2-diammonium cations and water molecules link Al—O—Al chains via numerous N—H···O and O—H···O hydrogen bonds (Table 1 and Fig. 4).

For related literature, see: Cheetham et al. (1999); Harrison (2002); Yamase et al. (1997).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO (Rigaku, 2004); data reduction: RAPID-AUTO (Rigaku, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 1999).

Figures top
[Figure 1] Fig. 1. The structure of the title compound, with displacement ellipsoids drawn at the 50% probability level. H atoms shown as arbitrary spheres.
[Figure 2] Fig. 2. View of the infinite Al—O—Al chain.
[Figure 3] Fig. 3. A polyhedral respresentation of the one-dimensional Al—O—Al chain of the title compound.
[Figure 4] Fig. 4. A packing diagram of the title compound, viewed along the a axis. Dashed lines indicate hydrogen bonds.
Poly[propane-1,2-diammonium [µ2-hydroxido-di-µ2-phosphonato-aluminium(III)] monohydrate] top
Crystal data top
(C3H12N2)[Al(OH)(HPO3)2]·H2OF(000) = 624
Mr = 298.11Dx = 1.701 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.059 (2) ÅCell parameters from 10198 reflections
b = 6.9782 (14) Åθ = 3.0–27.5°
c = 15.319 (3) ŵ = 0.48 mm1
β = 100.01 (3)°T = 170 K
V = 1164.2 (4) Å3Chunk, colorless
Z = 40.58 × 0.27 × 0.18 mm
Data collection top
Rigaku R-AXIS SPIDER
diffractometer
2513 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.021
Graphite monochromatorθmax = 27.5°, θmin = 3.2°
ω oscillation scansh = 1414
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
k = 98
Tmin = 0.856, Tmax = 0.917l = 1919
10911 measured reflections2 standard reflections every 150 reflections
2654 independent reflections intensity decay: none
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)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0531P)2 + 0.5902P]
where P = (Fo2 + 2Fc2)/3
2654 reflections(Δ/σ)max = 0.001
169 parametersΔρmax = 0.26 e Å3
1 restraintΔρmin = 0.51 e Å3
Crystal data top
(C3H12N2)[Al(OH)(HPO3)2]·H2OV = 1164.2 (4) Å3
Mr = 298.11Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.059 (2) ŵ = 0.48 mm1
b = 6.9782 (14) ÅT = 170 K
c = 15.319 (3) Å0.58 × 0.27 × 0.18 mm
β = 100.01 (3)°
Data collection top
Rigaku R-AXIS SPIDER
diffractometer
2513 reflections with I > 2σ(I)
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
Rint = 0.021
Tmin = 0.856, Tmax = 0.9172 standard reflections every 150 reflections
10911 measured reflections intensity decay: none
2654 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0261 restraint
wR(F2) = 0.080H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 0.26 e Å3
2654 reflectionsΔρmin = 0.51 e Å3
169 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
P10.95407 (3)0.19849 (4)0.19018 (2)0.00995 (10)
P20.78292 (3)0.20388 (4)0.42460 (2)0.00997 (10)
Al10.75189 (3)0.45005 (4)0.24929 (2)0.00802 (10)
O11.09179 (9)0.19119 (13)0.19924 (8)0.0202 (2)
O20.90558 (8)0.01902 (12)0.22963 (6)0.01556 (19)
O30.90834 (8)0.38056 (12)0.22784 (6)0.0160 (2)
O40.80156 (8)0.38466 (12)0.37257 (6)0.01461 (19)
O50.68994 (8)0.20026 (11)0.22253 (6)0.00947 (18)
O60.86642 (9)0.20370 (13)0.51352 (6)0.0186 (2)
O70.79587 (9)0.01972 (12)0.37372 (6)0.0165 (2)
C11.11228 (12)0.30966 (18)0.42461 (9)0.0162 (3)
H1D1.05360.40740.40030.019*
H1E1.08670.18980.39500.019*
C21.23836 (11)0.36369 (19)0.40522 (9)0.0159 (3)
C31.32693 (15)0.1959 (2)0.41037 (11)0.0267 (3)
H3A1.40430.23970.39770.040*
H3B1.29370.10020.36790.040*
H3C1.33870.14170.46890.040*
N11.11006 (11)0.28876 (14)0.52071 (7)0.0143 (2)
H1A1.03480.25650.52840.022*
H1B1.13130.39940.54810.022*
H1C1.16280.19790.54330.022*
N21.21957 (10)0.44677 (16)0.31407 (7)0.0163 (2)
H2A1.29180.48070.30070.024*
H2B1.17130.54940.31180.024*
H2C1.18440.35980.27530.024*
OW10.90717 (12)0.20990 (16)0.68934 (8)0.0274 (3)
HW1B0.951 (2)0.136 (4)0.7146 (17)0.049 (7)*
HW1A0.887 (2)0.181 (3)0.6364 (19)0.049 (7)*
H10.6189 (14)0.201 (3)0.2196 (14)0.026 (5)*
H21.2722 (16)0.463 (3)0.4441 (12)0.026 (4)*
H30.6632 (16)0.207 (2)0.4384 (11)0.015 (4)*
H40.9074 (16)0.193 (2)0.1039 (12)0.019 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.00979 (17)0.00724 (17)0.01291 (17)0.00029 (10)0.00221 (12)0.00012 (10)
P20.01221 (17)0.00701 (17)0.01020 (17)0.00064 (10)0.00061 (12)0.00013 (10)
Al10.00911 (18)0.00394 (17)0.01038 (18)0.00018 (12)0.00004 (13)0.00020 (12)
O10.0118 (4)0.0137 (5)0.0367 (6)0.0001 (3)0.0089 (4)0.0039 (4)
O20.0106 (4)0.0076 (4)0.0287 (5)0.0002 (3)0.0038 (3)0.0037 (3)
O30.0126 (4)0.0070 (4)0.0292 (5)0.0002 (3)0.0063 (4)0.0025 (3)
O40.0233 (5)0.0067 (4)0.0120 (4)0.0028 (3)0.0021 (3)0.0005 (3)
O50.0082 (4)0.0048 (4)0.0146 (4)0.0001 (3)0.0003 (3)0.0002 (3)
O60.0250 (5)0.0188 (5)0.0101 (4)0.0025 (4)0.0021 (4)0.0008 (3)
O70.0287 (5)0.0066 (4)0.0121 (4)0.0021 (4)0.0028 (3)0.0005 (3)
C10.0159 (6)0.0196 (6)0.0128 (6)0.0022 (5)0.0015 (5)0.0002 (4)
C20.0150 (6)0.0152 (6)0.0170 (6)0.0014 (5)0.0017 (4)0.0012 (5)
C30.0242 (7)0.0284 (8)0.0271 (8)0.0112 (6)0.0036 (6)0.0038 (6)
N10.0180 (5)0.0113 (5)0.0132 (5)0.0001 (4)0.0013 (4)0.0010 (4)
N20.0149 (5)0.0133 (5)0.0215 (5)0.0009 (4)0.0058 (4)0.0024 (4)
OW10.0371 (6)0.0265 (6)0.0164 (5)0.0170 (5)0.0019 (5)0.0001 (4)
Geometric parameters (Å, º) top
P1—O11.5060 (10)C1—N11.4837 (17)
P1—O31.5179 (9)C1—C21.5226 (18)
P1—O21.5276 (9)C1—H1D0.9700
P1—H41.333 (18)C1—H1E0.9700
P2—O61.5070 (11)C2—N21.4928 (16)
P2—O71.5225 (9)C2—C31.5199 (19)
P2—O41.5252 (9)C2—H20.946 (19)
P2—H31.376 (17)C3—H3A0.9600
Al1—O31.8799 (10)C3—H3B0.9600
Al1—O5i1.8847 (9)C3—H3C0.9600
Al1—O2i1.8879 (10)N1—H1A0.8900
Al1—O51.8916 (9)N1—H1B0.8900
Al1—O41.9277 (10)N1—H1C0.8900
Al1—O7i1.9288 (10)N2—H2A0.8900
O2—Al1ii1.8879 (10)N2—H2B0.8900
O5—Al1ii1.8847 (9)N2—H2C0.8900
O5—H10.779 (15)OW1—HW1B0.77 (3)
O7—Al1ii1.9288 (10)OW1—HW1A0.83 (3)
O1—P1—O3113.06 (5)P2—O7—Al1ii132.74 (6)
O1—P1—O2110.78 (5)N1—C1—C2113.05 (11)
O3—P1—O2111.89 (6)N1—C1—H1D109.0
O1—P1—H4107.5 (8)C2—C1—H1D109.0
O3—P1—H4107.8 (7)N1—C1—H1E109.0
O2—P1—H4105.3 (7)C2—C1—H1E109.0
O6—P2—O7111.38 (5)H1D—C1—H1E107.8
O6—P2—O4110.84 (5)N2—C2—C3109.36 (11)
O7—P2—O4113.42 (6)N2—C2—C1107.18 (10)
O6—P2—H3108.4 (7)C3—C2—C1113.75 (12)
O7—P2—H3105.7 (7)N2—C2—H2106.4 (11)
O4—P2—H3106.7 (7)C3—C2—H2110.4 (11)
O3—Al1—O5i89.49 (4)C1—C2—H2109.5 (11)
O3—Al1—O2i179.72 (4)C2—C3—H3A109.5
O5i—Al1—O2i90.74 (4)C2—C3—H3B109.5
O3—Al1—O591.95 (4)H3A—C3—H3B109.5
O5i—Al1—O5178.48 (2)C2—C3—H3C109.5
O2i—Al1—O587.82 (4)H3A—C3—H3C109.5
O3—Al1—O489.77 (5)H3B—C3—H3C109.5
O5i—Al1—O488.11 (4)C1—N1—H1A109.5
O2i—Al1—O490.40 (5)C1—N1—H1B109.5
O5—Al1—O491.43 (4)H1A—N1—H1B109.5
O3—Al1—O7i89.91 (5)C1—N1—H1C109.5
O5i—Al1—O7i90.85 (4)H1A—N1—H1C109.5
O2i—Al1—O7i89.93 (5)H1B—N1—H1C109.5
O5—Al1—O7i89.61 (4)C2—N2—H2A109.5
O4—Al1—O7i178.92 (4)C2—N2—H2B109.5
P1—O2—Al1ii132.40 (6)H2A—N2—H2B109.5
P1—O3—Al1131.29 (6)C2—N2—H2C109.5
P2—O4—Al1131.79 (5)H2A—N2—H2C109.5
Al1ii—O5—Al1135.05 (5)H2B—N2—H2C109.5
Al1ii—O5—H1108.5 (13)HW1B—OW1—HW1A111 (2)
Al1—O5—H1109.5 (13)
O1—P1—O2—Al1ii172.54 (7)O2i—Al1—O4—P282.63 (8)
O3—P1—O2—Al1ii45.39 (10)O5—Al1—O4—P25.19 (8)
O1—P1—O3—Al1170.02 (7)O7i—Al1—O4—P2170 (2)
O2—P1—O3—Al144.11 (10)O3—Al1—O5—Al1ii43.65 (7)
O5i—Al1—O3—P1172.71 (8)O5i—Al1—O5—Al1ii118.6 (10)
O2i—Al1—O3—P128 (11)O2i—Al1—O5—Al1ii136.52 (7)
O5—Al1—O3—P17.75 (8)O4—Al1—O5—Al1ii46.17 (7)
O4—Al1—O3—P199.18 (8)O7i—Al1—O5—Al1ii133.54 (7)
O7i—Al1—O3—P181.86 (8)O6—P2—O7—Al1ii163.64 (7)
O6—P2—O4—Al1165.35 (7)O4—P2—O7—Al1ii37.76 (10)
O7—P2—O4—Al139.19 (10)N1—C1—C2—N2160.17 (10)
O3—Al1—O4—P297.14 (8)N1—C1—C2—C378.82 (14)
O5i—Al1—O4—P2173.36 (8)
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) x+3/2, y1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O60.891.872.7425 (16)165
N1—H1B···O4iii0.892.002.8751 (14)169
N1—H1C···O7iv0.891.982.7833 (14)149
N2—H2A···O1v0.891.952.7295 (15)145
N2—H2A···OW1vi0.892.663.2446 (18)124
N2—H2B···OW1iii0.891.892.7716 (16)171
N2—H2C···O10.891.842.7218 (16)172
OW1—HW1B···O2iv0.77 (3)1.98 (3)2.7363 (16)167 (3)
OW1—HW1A···O60.83 (3)1.86 (3)2.6528 (16)159 (2)
O5—H1···OW1vii0.78 (2)2.39 (2)3.1429 (17)163 (2)
Symmetry codes: (iii) x+2, y+1, z+1; (iv) x+2, y, z+1; (v) x+5/2, y+1/2, z+1/2; (vi) x+1/2, y+1/2, z1/2; (vii) x1/2, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula(C3H12N2)[Al(OH)(HPO3)2]·H2O
Mr298.11
Crystal system, space groupMonoclinic, P21/n
Temperature (K)170
a, b, c (Å)11.059 (2), 6.9782 (14), 15.319 (3)
β (°) 100.01 (3)
V3)1164.2 (4)
Z4
Radiation typeMo Kα
µ (mm1)0.48
Crystal size (mm)0.58 × 0.27 × 0.18
Data collection
DiffractometerRigaku R-AXIS SPIDER
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.856, 0.917
No. of measured, independent and
observed [I > 2σ(I)] reflections
10911, 2654, 2513
Rint0.021
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.080, 1.01
No. of reflections2654
No. of parameters169
No. of restraints1
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.26, 0.51

Computer programs: RAPID-AUTO (Rigaku, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O60.891.872.7425 (16)165.2
N1—H1B···O4i0.892.002.8751 (14)168.8
N1—H1C···O7ii0.891.982.7833 (14)149.1
N2—H2A···O1iii0.891.952.7295 (15)144.8
N2—H2A···OW1iv0.892.663.2446 (18)124.4
N2—H2B···OW1i0.891.892.7716 (16)170.7
N2—H2C···O10.891.842.7218 (16)172.2
OW1—HW1B···O2ii0.77 (3)1.98 (3)2.7363 (16)167 (3)
OW1—HW1A···O60.83 (3)1.86 (3)2.6528 (16)159 (2)
O5—H1···OW1v0.779 (15)2.390 (16)3.1429 (17)163.0 (18)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+2, y, z+1; (iii) x+5/2, y+1/2, z+1/2; (iv) x+1/2, y+1/2, z1/2; (v) x1/2, y+1/2, z1/2.
 

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