Poly[di-μ-cis-cyclo­hexane-1,4-dicarboxyl­ato-μ-trans-cyclo­hexane-1,4-dicarboxyl­ato-bis­[dipyrido[3,2-a:2′,3′-c]phenazine]trimanganese(II)]

Wen-Zhi Zhang; Xiao-Huan Yuan

doi:10.1107/S1600536808012737

. 2008 May 7;64(Pt 6):m781–m782. doi: 10.1107/S1600536808012737

Poly[di-μ-cis-cyclohexane-1,4-dicarboxylato-μ-trans-cyclohexane-1,4-dicarboxylato-bis[dipyrido[3,2-a:2′,3′-c]phenazine]trimanganese(II)]

Wen-Zhi Zhang ^a,^*, Xiao-Huan Yuan ^b

PMCID: PMC2961629 PMID: 21202471

Abstract

In the title compound, [Mn₃(C₈H₁₀O₄)₃(C₁₈H₁₀N₄)₂], one Mn atom and one cyclohexane-1,4-dicarboxylate (chdc) ligand are located on centres of inversion. One of the two independent Mn atoms is seven-coordinate, binding to five carboxylate O atoms from different chdc ligands and two phenanthrene N atoms from a dipyrido[3,2-a:2′,3′-c]phenazine (L) ligand, while the second Mn atom is six-coordinate, binding to six carboxylate O atoms from different chdc ligands. The cis-chdc ligands bridge the trinuclear Mn^II clusters, forming chains, which are further linked into a three-dimensional network.

Related literature

For related structures, see: De (2007 ▶); Li (2007 ▶).

Experimental

Crystal data

[Mn₃(C₈H₁₀O₄)₃(C₁₈H₁₀N₄)₂]
M _r = 1239.90
Triclinic,
a = 8.5730 (17) Å
b = 10.614 (2) Å
c = 14.846 (3) Å
α = 77.34 (3)°
β = 81.99 (3)°
γ = 82.67 (3)°
V = 1298.6 (4) Å³
Z = 1
Mo Kα radiation
μ = 0.80 mm⁻¹
T = 293 (2) K
0.33 × 0.22 × 0.19 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.762, T _max = 0.863
12776 measured reflections
5830 independent reflections
3707 reflections with I > 2σ(I)
R _int = 0.061

Refinement

R[F ² > 2σ(F ²)] = 0.060
wR(F ²) = 0.176
S = 1.05
5830 reflections
376 parameters
H-atom parameters constrained
Δρ_max = 0.64 e Å⁻³
Δρ_min = −0.74 e Å⁻³

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL-Plus (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808012737/bt2704sup1.cif

e-64-0m781-sup1.cif^{(23.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808012737/bt2704Isup2.hkl

e-64-0m781-Isup2.hkl^{(279.6KB, hkl)}

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

Acknowledgments

The work was supported by the Program for Young Academic Backbone in Heilongjiang Provincial University (No. 1152 G053).

supplementary crystallographic information

Comment

1,4-Cyclohexanedicarboxylic acid (H₂chdc), as a flexible multidentate ligand, has been extensively studied in the chemistry of coordination polymers (De, 2007; Li, 2007). Here, we report a new Mn^II coordination polymer with chdc ligand, namely [Mn₃(cis-chdc)₃(trans-chdc)(L)₂] (I), where L = dipyrido[3,2-a:2',3'-c]-phenazine.

In (I) the Mn1 atom is seven-coordinate binding to five carboxylate O atoms from different chdc ligands, and two phenanthrene N atoms from L ligand (Fig. 1 and Table 1). The Mn2 atom is six-coordinate binding to six carboxylate O atoms from different chdc ligands (Fig. 1 and Table 1). Interestingly, the chdc ligands bridge neighboring Mn^II atoms to give a trinuclear Mn^II cluster. The cis-chdc ligands bridge the trinuclear Mn^II clusters to form a chain structure, which are further linked into a 3D network structure (Fig. 2). One Mn atom and one 1,4-cyclohexanedicarboxylate molecule are located on a centre of inversion.

Experimental

A mixture of Mn(NO₃)₂^.2H₂O (1 mmol), H₂chdc (1 mmol) and L (1 mmol) was dissolved in 12 ml distilled water, followed by addition of triethylamine until the pH value of the system was approximately 5.5. The resulting solution was sealed in a 23-ml Teflon-lined stainless steel autoclave and heated at 175°C for 8 days under autogenous pressure. The reaction vessel was then slowly cooled to room temperature. Pale yellow block-like crystals of (I) suitable for single-crystal X-ray diffraction analysis were obtained from the resulting solution.