Diaqua­tetra­kis­(1,3-di-4-pyridylpropane-κN)­manganese(II) bis­(perchlorate) ses­qui­hydrate

Hai-Wei Kuai; Xiao-Chun Cheng

doi:10.1107/S1600536811041511

. 2011 Oct 22;67(Pt 11):m1543. doi: 10.1107/S1600536811041511

Diaquatetrakis(1,3-di-4-pyridylpropane-κN)manganese(II) bis(perchlorate) sesquihydrate

Hai-Wei Kuai ^a,^*, Xiao-Chun Cheng ^a

PMCID: PMC3246966 PMID: 22219786

Abstract

In the title complex, [Mn(C₁₃H₁₄N₂)₄(H₂O)₂](ClO₄)₂·1.5H₂O, the Mn^II ion is coordinated by four N atoms from four different 1,3-di-4-pyridylpropane molecules and two O atoms from two coordinated water molecules, leading to a distorted MnN₄O₂ octahedral geometry. Each 1,3-di-4-pyridylpropane ligand displays a monodentate coordinating mode. In the crystal, there exist O—H⋯O, O—H⋯N and C—H⋯O hydrogen bonds. The perchlorate anions and the coordinated and lattice water molecules play an important role in the formation of these hydrogen bonds. One of the two lattice water molecules shows half-occupancy.

Related literature

For a related structure, see: Zheng et al. (2007 ▶).

Experimental

Crystal data

[Mn(C₁₃H₁₄N₂)₄(H₂O)₂](ClO₄)₂·1.5H₂O
M _r = 1108.94
Orthorhombic,
a = 19.0755 (10) Å
b = 15.9409 (9) Å
c = 37.533 (2) Å
V = 11412.9 (11) Å³
Z = 8
Mo Kα radiation
μ = 0.39 mm⁻¹
T = 293 K
0.30 × 0.30 × 0.10 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.892, T _max = 0.962
61756 measured reflections
10065 independent reflections
6106 reflections with I > 2.σ(I)
R _int = 0.113

Refinement

R[F ² > 2σ(F ²)] = 0.057
wR(F ²) = 0.188
S = 1.01
10065 reflections
676 parameters
H-atom parameters constrained
Δρ_max = 0.66 e Å⁻³
Δρ_min = −0.47 e Å⁻³

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2000 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811041511/pv2456sup1.cif

e-67-m1543-sup1.cif^{(39.3KB, cif)}

Supplementary material file. DOI: 10.1107/S1600536811041511/pv2456Isup2.cdx

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811041511/pv2456Isup3.hkl

e-67-m1543-Isup3.hkl^{(492.3KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3W—H3WA⋯N8ⁱ	0.92	1.86	2.753 (4)	162
O3W—H3W⋯N5ⁱⁱ	0.88	1.87	2.738 (4)	167
O2W—H2WA⋯O3Wⁱⁱⁱ	0.85	1.88	2.723 (3)	178
O2W—H2W⋯N7^iv	0.86	1.98	2.844 (4)	174
O1W—H1W⋯N6^v	0.81	2.08	2.824 (4)	153
O4W—H4W⋯O4	0.85	2.22	2.975 (9)	147
O1W—H1WA⋯O3W	0.80	1.91	2.684 (3)	163
O4W—H4WA⋯O6	0.85	2.43	3.035 (14)	129
C23—H23⋯O4^iv	0.93	2.53	3.379 (6)	152
C28—H28⋯O5^vi	0.93	2.43	3.255 (11)	148
C39—H39⋯O8	0.93	2.52	3.214 (9)	132

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

Acknowledgments

The authors gratefully acknowledge the Natural Science Foundation of Jiangsu Province of China (BK2008195) for financial support of this work.

supplementary crystallographic information

Comment

Flexible compounds, e.g., 1,3-di-4-pyridylpropane, are often used as ligands to synthesize complexes for their variable conformations. Herein, we report the crystal structure of thr title complex.

The asymmetric unit of the title complex consists of one manganese ion, four 1,3-di-4-pyridylpropane molecules, two coordinated water molecules, and sesqui crystallization water molecule. The Mn ion is coordinated by four N atoms from four different 1,3-di-4-pyridylpropane molecules and two O atoms from two coordinated water molecules, displaying a distorted MnN₄O₂ octahedral geometry (Fig. 1). Each 1,3-di-4-pyridylpropane displays a monodentate coordinating mode. In the crystal structure, there exist O—H···O, O—H···N and C—H···O hydrogen bonds (Table 1). Perchlorate anions and water molecules including coordinated water molecule and lattice water molecule, play very important roles in the formation of these hydrogen bonding interactions.

Experimental

Reaction mixture of Mn(ClO₄)₂.6H₂O (72.3 mg, 0.2 mmol), 1,3-di-4-pyridylpropane (39.6 mg, 0.2 mmol), 4-((1H-benzo[d]imidazol-1-yl)methyl)benzoic acid (50.4 mg, 0.2 mmol) and potassium hydroxide (11.2 mg, 0.2 mmol) in 12 ml H₂O was sealed in a 16 ml Teflon-lined stainless steel container and heated to 373 K for 3 days. After cooling to room temperature, colorless block crystals of the title complex were obtained.