Tetra­aqua­{1-[(1H-1,2,3-benzotriazol-1-yl)meth­yl]-1H-imidazole}­sulfato­manganese(II) dihydrate

Ying Wang; Ying-Ying Sun

doi:10.1107/S1600536811022197

. 2011 Jun 18;67(Pt 7):m920. doi: 10.1107/S1600536811022197

Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-imidazole}sulfatomanganese(II) dihydrate

Ying Wang ^a,^*, Ying-Ying Sun ^b

PMCID: PMC3151900 PMID: 21836905

Abstract

In the title complex, [Mn(SO₄)(C₁₀H₉N₅)(H₂O)₄]·2H₂O, the Mn²⁺ cation is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-imidazole ligand and five O atoms from one monodentate sulfate ligand and four water molecules in a distorted octahedral geometry. In the crystal, adjacent molecules are linked through O—H⋯O and O—H⋯N hydrogen bonds into a three-dimensional network.

Related literature

For background to complexes based on flexible organic ligands, see: Ma et al. (2011 ▶); Meng et al. (2009 ▶); Sanchez et al. (2002 ▶).

Experimental

Crystal data

[Mn(SO₄)(C₁₀H₉N₅)(H₂O)₄]·2H₂O
M _r = 458.32
Triclinic,
a = 7.5824 (15) Å
b = 8.5237 (17) Å
c = 15.972 (3) Å
α = 98.33 (3)°
β = 91.11 (3)°
γ = 115.21 (3)°
V = 920.3 (3) Å³
Z = 2
Mo Kα radiation
μ = 0.89 mm⁻¹
T = 293 K
0.20 × 0.18 × 0.15 mm

Data collection

Rigaku Saturn diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006 ▶) T _min = 0.842, T _max = 0.878
11432 measured reflections
4337 independent reflections
3890 reflections with I > 2σ(I)
R _int = 0.022

Refinement

R[F ² > 2σ(F ²)] = 0.038
wR(F ²) = 0.087
S = 1.03
4337 reflections
244 parameters
H-atom parameters constrained
Δρ_max = 0.88 e Å⁻³
Δρ_min = −0.42 e Å⁻³

Data collection: CrystalClear (Rigaku/MSC, 2006 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811022197/wm2495sup1.cif

e-67-0m920-sup1.cif^{(20.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811022197/wm2495Isup2.hkl

e-67-0m920-Isup2.hkl^{(212.5KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Mn1—O5	2.1543 (16)
Mn1—O8	2.1854 (15)
Mn1—O7	2.1860 (16)
Mn1—N1	2.2043 (17)
Mn1—O6	2.2142 (17)
Mn1—O1	2.2269 (16)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H1W⋯O10	0.85	1.79	2.634 (2)	173
O5—H2W⋯O3	0.85	1.92	2.729 (3)	159
O9—H9W⋯O4	0.85	2.02	2.843 (3)	163
O6—H3W⋯O9ⁱ	0.85	1.98	2.824 (2)	170
O8—H8W⋯O1ⁱ	0.85	2.04	2.885 (2)	176
O7—H6W⋯O4ⁱ	0.85	2.03	2.855 (3)	163
O6—H4W⋯O4ⁱⁱ	0.85	1.96	2.805 (2)	173
O7—H5W⋯O9ⁱⁱ	0.85	1.99	2.813 (2)	162
O8—H7W⋯O2ⁱⁱⁱ	0.85	1.87	2.712 (2)	172
O10—H11W⋯O2ⁱⁱⁱ	0.85	2.08	2.842 (3)	150
O10—H12W⋯N5^iv	0.85	1.99	2.840 (3)	173
O9—H10W⋯O1^v	0.85	2.24	3.083 (2)	173

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) .

supplementary crystallographic information

Comment

A large number of metal-organic frameworks based on flexible organic ligands have been reported since they are good linkers and can influence the structural diversification of the products, including the formation of supramolecular isomers (Ma et al., 2011; Meng et al., 2009; Sanchez et al., 2002). In order to further explore complexes with novel structures, in this work, through the reaction of 1-[1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,3-imidazole (bmi) with manganese sulfate at room temperature, we obtained the title complex, [Mn(SO₄)(C₁₀H₉N₅)(H₂O)₄](H₂O)₂, which is reported here.

As shown in Figure 1, the Mn(II) ion features a distorted octahedral coordination geometry and is surrounded by five oxygen atoms from four water molecules and one monodentate sulfate ligand as well as one nitrogen atom from the bmi ligand. Atoms O1, O5, O6, O7 form the equatorial plane, whereas O8 and N1 atoms are located in the apical positions. The bond angle of O(8)—Mn(1)—N(1) is 176.71 (6) °. Intramolecular O—H···O hydrogen bonds stabilize the molecular configuration and O—H···O, O—H···N hydrogen bonds between adjacent molecules consolidate the crystal packing (Fig. 2).

Experimental

The ligand 1-[1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,3-imidazole (0.1 mmol) in methanol (4 ml) was added dropwise to an aqueous solution (2 ml) of manganese sulfate (0.1 mmol). The resulting solution was allowed to stand at room temperature. After four weeks colorless crystals with good quality were obtained from the filtrate and dried in air.