catena-Poly[[[aqua­(1,10-phenanthro­line)manganese(II)]-μ-adamantane-1,3-dicarboxyl­ato] monohydrate]

Jian-Qiang Liu; Yun-Sheng Huang

doi:10.1107/S1600536811041900

. 2011 Oct 12;67(Pt 11):m1541–m1542. doi: 10.1107/S1600536811041900

catena-Poly[[[aqua(1,10-phenanthroline)manganese(II)]-μ-adamantane-1,3-dicarboxylato] monohydrate]

Jian-Qiang Liu ^a,^*, Yun-Sheng Huang ^a

PMCID: PMC3246965 PMID: 22219785

Abstract

In the title coordination polymer, {[Mn(C₁₂H₁₄O₄)(C₁₂H₈N₂)(H₂O)]·H₂O}_n, the Mn^II atom has a highly distorted cis-MnN₂O₄ octahedral geometry arising from its coordination by a bidentate phenanthroline ligand, a water molecule and monodentate and bidentate adamantane-1,3-dicarboxylate dianions. The bridging dianion leads to [001] chains in the crystal. The chains are linked by O—H⋯O hydrogen bonds, involving both the coordinated and uncoordinated water molecules, thereby forming a two-dimensional network.

Related literature

For related structures, see: Liu & Wu (2010 ▶); Chen & Liu (2002 ▶). For background to the synthesis of functionalized adamantane compounds, see: Seidel & Stang (2002 ▶).

Experimental

Crystal data

[Mn(C₁₂H₁₄O₄)(C₁₂H₈N₂)(H₂O)]·H₂O
M _r = 493.41
Monoclinic,
a = 13.248 (2) Å
b = 18.345 (3) Å
c = 9.3908 (17) Å
β = 105.283 (3)°
V = 2201.6 (6) Å³
Z = 4
Mo Kα radiation
μ = 0.64 mm⁻¹
T = 298 K
0.30 × 0.22 × 0.17 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T _min = 0.830, T _max = 0.898
10943 measured reflections
3918 independent reflections
2393 reflections with I > 2σ(I)
R _int = 0.046

Refinement

R[F ² > 2σ(F ²)] = 0.040
wR(F ²) = 0.116
S = 0.83
3918 reflections
310 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.28 e Å⁻³
Δρ_min = −0.26 e Å⁻³

Data collection: SMART (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: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811041900/hb6433sup1.cif

e-67-m1541-sup1.cif^{(21.3KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811041900/hb6433Isup2.hkl

e-67-m1541-Isup2.hkl^{(192.1KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Mn2—O3ⁱ	2.140 (2)
Mn2—O5	2.170 (2)
Mn2—O2	2.224 (2)
Mn2—N1	2.244 (2)
Mn2—O1	2.271 (2)
Mn2—N2	2.282 (2)

Open in a new tab

O2—Mn2—O1

57.92 (7)

Open in a new tab

Symmetry code: (i) Inline graphic .

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5WA⋯O2ⁱⁱ	0.84 (1)	1.88 (1)	2.711 (3)	173 (5)
O5—H5WB⋯O4ⁱ	0.83 (1)	1.76 (1)	2.582 (3)	172 (5)
O6—H6WA⋯O3ⁱⁱⁱ	0.84 (1)	2.60 (6)	3.062 (4)	116 (5)
O6—H6WB⋯O1^iv	0.84 (1)	2.22 (4)	2.914 (4)	140 (5)

Open in a new tab

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

Acknowledgments

The authors gratefully acknowledge financial support of this work by Guangdong Medical College (B2010009).

supplementary crystallographic information

Comment

Adamantane-1,3-dicarboxylate (H₂L), is a dicarboxylaic acid and one of the most stable hydrocarbons, which was discovered in the 1930s. As a consequence of its stability, it can be produced catalytically from a wide various precursor organic substances (Seidel & Stang, 2002). In our recent work, we have studied the supramolecular chemistry based on L and 2,2-bipy (Liu et al., 2010). With this background in mind, we continued to our investigation and chose L as a bridging ligand and phenanthroline (phen) ligand to react with the d-block metal ions. Herein, we are interested in self-assembly reactions of Mn^II with H₂L and phen, which led to the title compound, (I).

The title compound, {[Mn(L)(phen)(H₂O)].H₂O} is comprised of a Mn^II, one adamantane-1,3-dicarboxylate dianion and one phen ligand, one coordinated water molecule and one free water molecule. As illustrated in Fig. 1. the Mn^II has a highly distorted octahedral coordination sphere (Table 1) comprising two N atoms from one different phen ligand, three one oxygen atoms from the adjacent L ligands and one coordinated water molecule. In title compound, the Mn^II ions are linked by L ligands to form chains along the c axis (Fig. 2), and the resulting chains are further held together based on O—H···O hydrogen bonds interactions, shaping 2D supramolecular sheet parallel to [010] (Table 2).

Compared to the title compound and {[Mn^II(L)(2,2'-bipy).H₂O]}n, the L exhibits bridging bidentate and chelated-bidentate modes in the latter compoud (Liu & Wu, 2010). Moreover, a dinuclear unit Mn^II was also shaped due to the different coordinated mode. Thus, the assistant ligand could induce the separated fomration of structures (Chen & Liu., 2002).

Experimental

A mixture of Mn(ac)₂.H₂O (25 mg, 0.1 mmol), H₂L (21 mg, 0.1 mmol), phen (18 mg, 0.1 mmol), NaOH (0.1mmol) and 8 ml H₂O and CH₃OH (3ml) was stirred for 1h, and then the mixture was transferred to an 25-ml Teflon-lined reactor and kept under autogenous pressure at 435 K for 3 days,then cooled down to room temperature. Colourless blocks of (I) were obtained.