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metal-organic compounds
catena-Poly[2,2′,2′′-nitrilotris(ethanaminium) [tri-μ-oxido-tris[dioxidovanadate(V)]] monohydrate]
aDepartment of Chemistry, Haverford College, 370 Lancaster Avenue, Haverford, PA 19041, USA, and bDepartment of Chemistry, Youngstown State University, 1 University Plaza, Youngstown, OH 44555, USA
*Correspondence e-mail: anorquis@haverford.edu
The title compound, {(C6H21N4)[V3O9]·H2O}n, crystallizes as a salt with [trenH3]3+ cations [tren is tris(2-aminoethyl)amine], and one-dimensional anionic {[VVO3]−}n (metavanadate) chains along the c-axis direction. Three crystallographically distinct VV sites and one occluded water molecule are present for every [trenH3]3+ cation in the The {[VVO3]−}n chains are composed of vertex-sharing [VO4] tetrahedra and have a repeat unit of six tetrahedra. Each tetrahedron in the chain contains two terminal and two μ2-bridging oxide ligands. The [trenH3]3+ cations, {[VVO3]−}n anions and occluded water molecules participate in an extensive three-dimensonal hydrogen-bonding network. The three terminal ammonium sites of the [trenH3]3+ cations each form strong N—H⋯O hydrogen bonds to terminal oxide ligands on the {[VVO3]−}n chain. Each occluded water molecule also donates two O—H⋯O hydrogen bonds to the terminal oxide ligands.
CCDC reference: 962516
Related literature
For properties of organically templated metal oxides, see: Cheetham et al. (1999). A host of amine-templated metavanadate chains with connectivities identical to the title compound have been reported previously, for examples, see: Riou & Ferey (1996
); Roman et al. (1991
); Smith et al. (2012
). Metavanadate chains with repeat units of six tetrahedra are known to exist, see: Lin et al. (2003
); Tyrselová et al. (1995
). For details of the H-atom treatment in the see: Cooper et al. (2010
).
Experimental
Crystal data
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Data collection: APEX2 (Bruker, 2009); cell SAINT (Bruker, 2009
); data reduction: SAINT; program(s) used to solve structure: SHELXS86 (Sheldrick, 2008
); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003
); molecular graphics: CAMERON (Watkin et al., 1996
); software used to prepare material for publication: CRYSTALS.
Supporting information
CCDC reference: 962516
10.1107/S1600536813026056/hp2060sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536813026056/hp2060Isup2.hkl
All chemicals (reagent grade) were commercially available and were used as received. Deionized water was used in this synthesis. The title compound was prepared under mild hydrothermal conditions in a 23 mL Teflon-lined stainless-steel autoclave. V2O5 (0.1449 g, 0.7967 mmol), Na2TeO3 (0.0889 g, 0.4012 mmol), tren (0.0620 g, 0.4240 mmol), ethanol (4 ml, 0.069 mol), and H2O (4 ml, 0.22 mol) were mixed to give a reaction mixture with a molar composition ratio of 2:1:1:170:550. The role of Na2TeO3 in this reaction is not understood. Reactions were placed in a 110 °C oven for 5 d. The reactions were then cooled to room temperature at a rate of 6 °C h-1 to promote the growth of large single crystals. Reaction vessels were opened in air, and the title compound was recovered as clear colorless needles in the presence of an unidentified tan powder via vacuum filtration.
While the H atoms were all located in a difference map, they were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularize their geometry (C—H in the range 0.93–0.98, N—H to 0.95, and O—H = 0.95 Å) and Uiso(H) (in the range 1.2–1.5 times Ueq of the parent atom), after which the positions were refined with riding constraints (Cooper et al., 2010).
Data collection: APEX2 (Bruker, 2009); cell
SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: CRYSTALS (Betteridge et al., 2003).(C6H21N4)[V3O9]·H2O | F(000) = 944 |
Mr = 464.09 | Dx = 1.885 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2067 reflections |
a = 9.6624 (14) Å | θ = 2.6–29.5° |
b = 10.9179 (15) Å | µ = 1.73 mm−1 |
c = 15.768 (2) Å | T = 100 K |
β = 100.565 (2)° | Block, colorless |
V = 1635.2 (4) Å3 | 0.26 × 0.20 × 0.16 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 4719 independent reflections |
Radiation source: fine focus sealed tube | 3195 reflections with I > 2.0σ(I) |
Graphite monochromator | Rint = 0.061 |
ω scans | θmax = 30.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | h = −13→13 |
Tmin = 0.623, Tmax = 0.746 | k = −15→15 |
14279 measured reflections | l = −20→22 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.052 | H-atom parameters not refined |
wR(F2) = 0.094 | Method = Modified Sheldrick w = 1/[σ2(F2) + (0.03P)2 + 7.47P] , where P = (max(Fo2,0) + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.0003744 |
2860 reflections | Δρmax = 1.44 e Å−3 |
208 parameters | Δρmin = −0.68 e Å−3 |
0 restraints |
(C6H21N4)[V3O9]·H2O | V = 1635.2 (4) Å3 |
Mr = 464.09 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.6624 (14) Å | µ = 1.73 mm−1 |
b = 10.9179 (15) Å | T = 100 K |
c = 15.768 (2) Å | 0.26 × 0.20 × 0.16 mm |
β = 100.565 (2)° |
Bruker SMART APEX CCD area-detector diffractometer | 4719 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | 3195 reflections with I > 2.0σ(I) |
Tmin = 0.623, Tmax = 0.746 | Rint = 0.061 |
14279 measured reflections |
R[F2 > 2σ(F2)] = 0.052 | 0 restraints |
wR(F2) = 0.094 | H-atom parameters not refined |
S = 1.00 | Δρmax = 1.44 e Å−3 |
2860 reflections | Δρmin = −0.68 e Å−3 |
208 parameters |
x | y | z | Uiso*/Ueq | ||
V1 | 0.92597 (7) | 0.75226 (7) | 0.71937 (5) | 0.0135 | |
V2 | 0.87185 (7) | 0.80317 (7) | 0.49412 (4) | 0.0120 | |
V3 | 0.75379 (8) | 0.58481 (7) | 0.35925 (5) | 0.0152 | |
O1 | 0.8914 (4) | 0.6089 (3) | 0.7288 (2) | 0.0320 | |
O2 | 1.0944 (3) | 0.7734 (3) | 0.7595 (2) | 0.0217 | |
O3 | 0.8219 (5) | 0.8480 (4) | 0.7734 (2) | 0.0498 | |
O4 | 0.8935 (3) | 0.8036 (3) | 0.6095 (2) | 0.0244 | |
O5 | 1.0270 (3) | 0.7839 (3) | 0.4659 (2) | 0.0220 | |
O6 | 0.8112 (4) | 0.9374 (3) | 0.4625 (2) | 0.0379 | |
O7 | 0.7512 (4) | 0.6883 (4) | 0.4472 (2) | 0.0354 | |
O8 | 0.8542 (4) | 0.4695 (4) | 0.4011 (3) | 0.0429 | |
O9 | 0.5943 (3) | 0.5335 (3) | 0.3264 (2) | 0.0233 | |
O10 | 0.6272 (4) | 0.9517 (3) | 0.2942 (2) | 0.0326 | |
N1 | 0.3633 (3) | 0.7571 (3) | 0.4750 (2) | 0.0124 | |
N2 | 0.1483 (4) | 0.5617 (3) | 0.4189 (2) | 0.0186 | |
N3 | 0.2327 (4) | 0.8310 (4) | 0.6220 (2) | 0.0199 | |
N4 | 0.1714 (4) | 0.9305 (3) | 0.3650 (2) | 0.0173 | |
C1 | 0.3965 (4) | 0.6257 (4) | 0.4704 (3) | 0.0144 | |
C2 | 0.2953 (4) | 0.5559 (4) | 0.4031 (3) | 0.0161 | |
C3 | 0.4414 (4) | 0.8077 (4) | 0.5560 (3) | 0.0180 | |
C4 | 0.3751 (4) | 0.7766 (4) | 0.6334 (3) | 0.0178 | |
C5 | 0.4008 (5) | 0.8229 (4) | 0.4007 (3) | 0.0195 | |
C6 | 0.3272 (4) | 0.9449 (4) | 0.3853 (3) | 0.0186 | |
H1 | 0.7169 | 0.9334 | 0.2807 | 0.0389* | |
H2 | 0.5660 | 0.9794 | 0.2437 | 0.0389* | |
H3 | 0.4912 | 0.6178 | 0.4588 | 0.0191* | |
H4 | 0.3936 | 0.5894 | 0.5259 | 0.0187* | |
H5 | 0.2977 | 0.5904 | 0.3470 | 0.0191* | |
H6 | 0.3247 | 0.4713 | 0.4050 | 0.0189* | |
H7 | 0.1445 | 0.5268 | 0.4736 | 0.0240* | |
H8 | 0.0880 | 0.5172 | 0.3752 | 0.0240* | |
H9 | 0.1185 | 0.6447 | 0.4180 | 0.0240* | |
H10 | 0.5379 | 0.7765 | 0.5656 | 0.0209* | |
H11 | 0.4435 | 0.8963 | 0.5511 | 0.0211* | |
H12 | 0.4324 | 0.8092 | 0.6858 | 0.0219* | |
H13 | 0.3682 | 0.6886 | 0.6390 | 0.0222* | |
H14 | 0.1764 | 0.7994 | 0.5709 | 0.0245* | |
H15 | 0.1904 | 0.8116 | 0.6701 | 0.0245* | |
H16 | 0.2399 | 0.9174 | 0.6173 | 0.0245* | |
H17 | 0.3702 | 0.7723 | 0.3497 | 0.0240* | |
H18 | 0.5027 | 0.8342 | 0.4091 | 0.0241* | |
H19 | 0.3508 | 0.9958 | 0.4366 | 0.0226* | |
H20 | 0.3573 | 0.9845 | 0.3373 | 0.0229* | |
H21 | 0.1284 | 1.0088 | 0.3561 | 0.0223* | |
H22 | 0.1465 | 0.8828 | 0.3140 | 0.0223* | |
H23 | 0.1400 | 0.8905 | 0.4115 | 0.0223* |
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0147 (3) | 0.0181 (4) | 0.0087 (3) | 0.0034 (3) | 0.0046 (3) | −0.0010 (3) |
V2 | 0.0124 (3) | 0.0158 (4) | 0.0081 (3) | 0.0005 (3) | 0.0028 (3) | −0.0025 (3) |
V3 | 0.0125 (3) | 0.0188 (4) | 0.0157 (4) | −0.0053 (3) | 0.0062 (3) | −0.0037 (3) |
O1 | 0.032 (2) | 0.025 (2) | 0.036 (2) | −0.0146 (15) | −0.0010 (17) | 0.0016 (16) |
O2 | 0.0239 (17) | 0.0250 (18) | 0.0149 (16) | −0.0088 (13) | 0.0000 (13) | 0.0037 (13) |
O3 | 0.058 (3) | 0.074 (3) | 0.019 (2) | 0.042 (2) | 0.0113 (19) | −0.001 (2) |
O4 | 0.0225 (16) | 0.039 (2) | 0.0122 (15) | 0.0070 (15) | 0.0038 (13) | 0.0007 (15) |
O5 | 0.0161 (15) | 0.034 (2) | 0.0177 (16) | −0.0063 (13) | 0.0081 (13) | −0.0052 (14) |
O6 | 0.056 (3) | 0.031 (2) | 0.025 (2) | 0.0182 (19) | 0.0041 (18) | 0.0015 (16) |
O7 | 0.032 (2) | 0.049 (2) | 0.031 (2) | −0.0281 (18) | 0.0210 (17) | −0.0238 (18) |
O8 | 0.028 (2) | 0.032 (2) | 0.071 (3) | 0.0053 (17) | 0.014 (2) | 0.003 (2) |
O9 | 0.0206 (16) | 0.0303 (19) | 0.0184 (17) | −0.0104 (14) | 0.0023 (13) | −0.0028 (14) |
O10 | 0.0283 (19) | 0.047 (2) | 0.0227 (19) | 0.0063 (17) | 0.0044 (15) | 0.0061 (17) |
N1 | 0.0124 (16) | 0.0120 (16) | 0.0136 (17) | 0.0000 (14) | 0.0043 (13) | 0.0019 (14) |
N2 | 0.0161 (18) | 0.0198 (19) | 0.0188 (19) | −0.0023 (15) | 0.0007 (15) | −0.0005 (16) |
N3 | 0.0159 (18) | 0.028 (2) | 0.0158 (19) | −0.0045 (16) | 0.0041 (15) | 0.0007 (16) |
N4 | 0.0143 (17) | 0.0140 (18) | 0.022 (2) | 0.0004 (14) | 0.0004 (15) | −0.0020 (16) |
C1 | 0.0109 (19) | 0.015 (2) | 0.018 (2) | 0.0030 (16) | 0.0043 (16) | 0.0040 (17) |
C2 | 0.015 (2) | 0.015 (2) | 0.019 (2) | 0.0045 (16) | 0.0043 (17) | 0.0012 (17) |
C3 | 0.0107 (19) | 0.019 (2) | 0.024 (2) | −0.0026 (17) | 0.0016 (17) | 0.0026 (19) |
C4 | 0.016 (2) | 0.017 (2) | 0.018 (2) | −0.0043 (16) | −0.0014 (17) | −0.0005 (17) |
C5 | 0.015 (2) | 0.024 (2) | 0.021 (2) | 0.0039 (18) | 0.0090 (18) | 0.0054 (19) |
C6 | 0.015 (2) | 0.014 (2) | 0.027 (2) | 0.0009 (17) | 0.0046 (18) | 0.0065 (19) |
V1—O1 | 1.613 (3) | N3—H14 | 0.950 |
V1—O2 | 1.651 (3) | N3—H15 | 0.950 |
V1—O3 | 1.773 (4) | N3—H16 | 0.950 |
V1—O4 | 1.793 (3) | N4—C6 | 1.489 (5) |
V2—V3 | 3.2585 (11) | N4—H21 | 0.950 |
V2—O4 | 1.793 (3) | N4—H22 | 0.950 |
V2—O5 | 1.654 (3) | N4—H23 | 0.950 |
V2—O6 | 1.623 (4) | C1—C2 | 1.510 (6) |
V2—O7 | 1.778 (3) | C1—H3 | 0.969 |
V3—O3i | 1.769 (4) | C1—H4 | 0.966 |
V3—O7 | 1.793 (3) | C2—H5 | 0.967 |
V3—O8 | 1.651 (4) | C2—H6 | 0.966 |
V3—O9 | 1.632 (3) | C3—C4 | 1.517 (6) |
O10—H1 | 0.950 | C3—H10 | 0.978 |
O10—H2 | 0.950 | C3—H11 | 0.970 |
N1—C1 | 1.475 (5) | C4—H12 | 0.975 |
N1—C3 | 1.468 (5) | C4—H13 | 0.968 |
N1—C5 | 1.475 (5) | C5—C6 | 1.508 (6) |
N2—C2 | 1.488 (5) | C5—H17 | 0.976 |
N2—H7 | 0.950 | C5—H18 | 0.977 |
N2—H8 | 0.950 | C6—H19 | 0.974 |
N2—H9 | 0.950 | C6—H20 | 0.962 |
N3—C4 | 1.479 (6) | ||
O1—V1—O2 | 107.86 (17) | H15—N3—H16 | 109.5 |
O1—V1—O3 | 112.5 (2) | C6—N4—H21 | 109.5 |
O2—V1—O3 | 109.83 (19) | C6—N4—H22 | 109.2 |
O1—V1—O4 | 112.94 (18) | H21—N4—H22 | 109.5 |
O2—V1—O4 | 108.21 (15) | C6—N4—H23 | 109.6 |
O3—V1—O4 | 105.41 (17) | H21—N4—H23 | 109.5 |
V3—V2—O4 | 128.76 (12) | H22—N4—H23 | 109.5 |
V3—V2—O5 | 87.55 (11) | N1—C1—C2 | 114.0 (3) |
O4—V2—O5 | 109.31 (15) | N1—C1—H3 | 108.5 |
V3—V2—O6 | 113.39 (14) | C2—C1—H3 | 109.6 |
O4—V2—O6 | 106.12 (17) | N1—C1—H4 | 108.2 |
O5—V2—O6 | 109.05 (19) | C2—C1—H4 | 107.9 |
V3—V2—O7 | 24.27 (11) | H3—C1—H4 | 108.6 |
O4—V2—O7 | 111.67 (17) | C1—C2—N2 | 112.1 (3) |
O5—V2—O7 | 110.85 (16) | C1—C2—H5 | 109.0 |
O6—V2—O7 | 109.7 (2) | N2—C2—H5 | 108.7 |
V2—V3—O3i | 93.50 (13) | C1—C2—H6 | 108.2 |
V2—V3—O7 | 24.06 (10) | N2—C2—H6 | 108.7 |
O3i—V3—O7 | 112.99 (19) | H5—C2—H6 | 110.2 |
V2—V3—O8 | 100.80 (15) | N1—C3—C4 | 112.9 (3) |
O3i—V3—O8 | 110.4 (2) | N1—C3—H10 | 109.0 |
O7—V3—O8 | 105.2 (2) | C4—C3—H10 | 109.2 |
V2—V3—O9 | 130.93 (12) | N1—C3—H11 | 108.7 |
O3i—V3—O9 | 111.19 (18) | C4—C3—H11 | 107.8 |
O7—V3—O9 | 108.37 (16) | H10—C3—H11 | 109.1 |
O8—V3—O9 | 108.46 (19) | C3—C4—N3 | 109.4 (4) |
V1—O3—V3ii | 159.3 (2) | C3—C4—H12 | 110.0 |
V2—O4—V1 | 161.2 (2) | N3—C4—H12 | 109.1 |
V3—O7—V2 | 131.66 (19) | C3—C4—H13 | 110.0 |
H1—O10—H2 | 109.5 | N3—C4—H13 | 109.4 |
C1—N1—C3 | 109.1 (3) | H12—C4—H13 | 108.8 |
C1—N1—C5 | 110.3 (3) | N1—C5—C6 | 112.4 (3) |
C3—N1—C5 | 110.2 (3) | N1—C5—H17 | 107.3 |
C2—N2—H7 | 109.4 | C6—C5—H17 | 107.7 |
C2—N2—H8 | 109.6 | N1—C5—H18 | 110.0 |
H7—N2—H8 | 109.5 | C6—C5—H18 | 110.1 |
C2—N2—H9 | 109.5 | H17—C5—H18 | 109.2 |
H7—N2—H9 | 109.5 | C5—C6—N4 | 111.7 (3) |
H8—N2—H9 | 109.5 | C5—C6—H19 | 109.8 |
C4—N3—H14 | 109.4 | N4—C6—H19 | 108.2 |
C4—N3—H15 | 109.9 | C5—C6—H20 | 108.8 |
H14—N3—H15 | 109.5 | N4—C6—H20 | 108.5 |
C4—N3—H16 | 109.1 | H19—C6—H20 | 109.8 |
H14—N3—H16 | 109.5 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H1···O1i | 0.95 | 2.06 | 2.997 (6) | 170 (1) |
O10—H2···O9iii | 0.95 | 1.83 | 2.739 (6) | 160 (1) |
N2—H7···O8iv | 0.95 | 1.97 | 2.864 (6) | 155 (1) |
N2—H8···O1iv | 0.95 | 2.18 | 2.951 (6) | 138 (1) |
N2—H9···O5v | 0.95 | 1.98 | 2.850 (6) | 152 (1) |
C4—H13···O9iv | 0.97 | 2.50 | 3.447 (6) | 167 (1) |
N3—H14···O5v | 0.95 | 2.00 | 2.912 (6) | 162 (1) |
N3—H15···O2v | 0.95 | 1.87 | 2.819 (6) | 176 (1) |
N3—H16···O6vi | 0.95 | 2.03 | 2.853 (6) | 144 (1) |
N3—H16···O10vi | 0.95 | 2.23 | 2.925 (6) | 129 (1) |
C6—H19···O6vi | 0.97 | 2.54 | 3.222 (6) | 127 (1) |
N4—H21···O4vi | 0.95 | 2.14 | 3.013 (6) | 152 (1) |
N4—H22···O2vii | 0.95 | 1.94 | 2.796 (6) | 150 (1) |
N4—H23···O5v | 0.95 | 1.90 | 2.803 (6) | 157 (1) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (iii) −x+1, y+1/2, −z+1/2; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x+1, −y+2, −z+1; (vii) x−1, −y+3/2, z−1/2. |
V1—O1 | 1.613 (3) | V2—O6 | 1.623 (4) |
V1—O2 | 1.651 (3) | V2—O7 | 1.778 (3) |
V1—O3 | 1.773 (4) | V3—O3i | 1.769 (4) |
V1—O4 | 1.793 (3) | V3—O7 | 1.793 (3) |
V2—V3 | 3.2585 (11) | V3—O8 | 1.651 (4) |
V2—O4 | 1.793 (3) | V3—O9 | 1.632 (3) |
V2—O5 | 1.654 (3) |
Symmetry code: (i) x, −y+3/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H1···O1i | 0.950 | 2.058 | 2.997 (6) | 169.49 (14) |
O10—H2···O9ii | 0.950 | 1.828 | 2.739 (6) | 159.72 (15) |
N2—H7···O8iii | 0.950 | 1.974 | 2.864 (6) | 155.08 (16) |
N2—H8···O1iii | 0.950 | 2.177 | 2.951 (6) | 137.77 (13) |
N2—H9···O5iv | 0.950 | 1.976 | 2.850 (6) | 152.05 (14) |
C4—H13···O9iii | 0.968 | 2.497 | 3.447 (6) | 166.90 (12) |
N3—H14···O5iv | 0.950 | 1.995 | 2.912 (6) | 161.64 (15) |
N3—H15···O2iv | 0.950 | 1.871 | 2.819 (6) | 175.82 (15) |
N3—H16···O6v | 0.950 | 2.027 | 2.853 (6) | 144.28 (15) |
N3—H16···O10v | 0.950 | 2.233 | 2.925 (6) | 128.97 (13) |
C6—H19···O6v | 0.974 | 2.535 | 3.222 (6) | 127.44 (14) |
N4—H21···O4v | 0.950 | 2.138 | 3.013 (6) | 152.40 (13) |
N4—H22···O2vi | 0.950 | 1.935 | 2.796 (6) | 149.71 (14) |
N4—H23···O5iv | 0.950 | 1.904 | 2.803 (6) | 156.83 (14) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) −x+1, y+1/2, −z+1/2; (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z; (v) −x+1, −y+2, −z+1; (vi) x−1, −y+3/2, z−1/2. |
Acknowledgements
The authors acknowledge support from the NSF (Award No. CHE-0911121), the Henry Dreyfus Teacher–Scholar Awards Program, and grants to Haverford College from the HHMI Undergraduate Science Education Program. MZ acknowledges support for the purchase of a diffractometer from the NSF Grant 0087210, the Ohio Board of Regents Grant CAP-491, and Youngstown State University.
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Organically templated metal oxides have been the subject of sustained interest for many years, owing to their structural diversity and potential to exhibit technologically desirable physical properties (Cheetham et al., 1999). Amine-templated metavanadate chain compounds are no exception, with a number of different topologies for chains with identical connectivity having been reported. The synthesis and crystal structure of the title compound, [trenH3][VO3]3·H2O, is described here. The three-dimensional packing of the title compound is shown in Fig. 2. The {[VVO3]-}n chains are composed of vertex-sharing [VO4] tetrahedra and have a repeat unit of six tetrahedra. Each tetrahedron in the chain contains two terminal and two µ2-bridging oxide ligands. The V – Oterminal and V – Obridging bond lengths range from 1.613 (4) to 1.653 (3) Å and 1.770 (4) to 1.794 (4) Å, respectively. Several compounds containing amine templated metavanadate chains have been previously reported, see: Riou et al. (1996), Roman et al. (1991), Smith et al. (2012), Lin et al. (2003) and Tyrselová et al. (1995). However, the chain topology of the inorganic anion in the title compound is novel. The [trenH3]3+ cations, {[VVO3]-}n anions and occluded water molecules participate in an extensive three-dimensonal hydrogen-bonding network. The three terminal ammonium sites of the [trenH3]3+ cations each form strong N–H···O hydrogen bonds to terminal oxide atoms on the {[VVO3]-}n chain, with N···O distances ranging from 2.796 (5) to 3.013 (5) Å. Each occluded water molecule also donates two O–H···O hydrogen bonds to the terminal oxide atoms, with O···O distances ranging from 2.738 (4) to 2.996 (5) Å.