Poly[[tris-(μ(3)-2-oxidopyridinium-3-carboxyl-ato)manganese(II)sodium(I)] monohydrate].

In the crystal structure of the title compound, {[MnNa(C(6)H(4)NO(3))(3)]·H(2)O}(n), the Mn(II) cation is located on a threefold rotation axis and is chelated by three 2-oxidopyridinium-3-carboxyl-ate (opc) anions in an octa-hedal coordination. The Na(I) cation is located on a threefold rotation axis and is surrounded by six O atoms from three opc anions. The opc anions link the Mn and Na cations, forming a three-dimensional polymeric structure. The uncoordinated water mol-ecule, located on a threefold rotation axis, is equally disordered over two sites. The three-dimensional network is consolidated by N-H⋯O hydrogen bonds.

Related literature

For related NiII and CoII complexes, see: Zhang et al. (2009a ▶,b ▶). For comparison C—O bond distances in 2-oxidopyridinium-3-carboxyl­ate and 2-hydroxy­pyridine­carboxyl­ate complexes, see: Yao et al. (2004 ▶); Yan & Hu (2007a ▶,b ▶); Wen & Liu (2007 ▶); Quintal et al. (2002 ▶). For comparison C—O bond distances in 2-hydroxy­benzoic acid and 2-hydroxy­benzoate complexes, see: Munshi & Guru Row (2006 ▶); Su & Xu (2005 ▶); Li et al. (2005 ▶).

Experimental

Crystal data

[MnNa(C6H4NO3)3]·H2O

M = 510.25

Trigonal,

a = 10.1478 (18) Å

c = 37.420 (13) Å

V = 3337.1 (15) Å3

Z = 6

Mo Kα radiation

μ = 0.67 mm−1

T = 294 K

0.33 × 0.28 × 0.26 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.822, T max = 0.840

6825 measured reflections

1315 independent reflections

1236 reflections with I > 2σ(I)

R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.099

S = 1.16

1315 reflections

103 parameters

1 restraint

H-atom parameters constrained

Δρmax = 0.35 e Å−3

Δρmin = −0.49 e Å−3

Absolute structure: Flack (1983 ▶), 649 Friedel pairs

Flack parameter: −0.01 (3)

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810002953/ng2724sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810002953/ng2724Isup2.hkl

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

[MnNa(C6H4NO3)3]·H2O	Dx = 1.523 Mg m−3
Mr = 510.25	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 1286 reflections
Hall symbol: R 3 -2"c	θ = 2.6–25.0°
a = 10.1478 (18) Å	µ = 0.67 mm−1
c = 37.420 (13) Å	T = 294 K
V = 3337.1 (15) Å3	Prism, brown
Z = 6	0.33 × 0.28 × 0.26 mm
F(000) = 1554

Rigaku R-AXIS RAPID IP diffractometer	1315 independent reflections
Radiation source: fine-focus sealed tube	1236 reflections with I > 2σ(I)
graphite	Rint = 0.027
Detector resolution: 10.00 pixels mm-1	θmax = 25.2°, θmin = 2.6°
ω scan	h = −11→11
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −11→11
Tmin = 0.822, Tmax = 0.840	l = −44→44
6825 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033	H-atom parameters constrained
wR(F2) = 0.099	w = 1/[σ2(Fo2) + (0.0683P)2 + 0.0175P] where P = (Fo2 + 2Fc2)/3
S = 1.16	(Δ/σ)max = 0.001
1315 reflections	Δρmax = 0.35 e Å−3
103 parameters	Δρmin = −0.49 e Å−3
1 restraint	Absolute structure: Flack (1983), 649 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: −0.01 (3)

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn	0.6667	0.3333	0.87519 (2)	0.0258 (2)
Na1	0.6667	0.3333	0.96375 (5)	0.0283 (5)
N1	0.7336 (3)	0.0138 (3)	0.93953 (7)	0.0401 (6)
H1N	0.7655	0.0750	0.9589	0.048*
O1	0.4925 (3)	−0.1044 (3)	0.82611 (6)	0.0464 (6)
O2	0.5735 (3)	0.1281 (3)	0.84538 (6)	0.0377 (6)
O3	0.6999 (3)	0.1941 (3)	0.91404 (6)	0.0425 (6)
C1	0.5566 (3)	−0.0028 (3)	0.84910 (7)	0.0292 (6)
C2	0.6173 (3)	−0.0412 (3)	0.88206 (8)	0.0321 (6)
C3	0.6828 (3)	0.0635 (3)	0.91133 (8)	0.0293 (6)
C4	0.7283 (6)	−0.1207 (4)	0.94099 (12)	0.0596 (12)
H4	0.7664	−0.1454	0.9609	0.072*
C5	0.6677 (6)	−0.2210 (4)	0.91359 (12)	0.0689 (13)
H5	0.6651	−0.3139	0.9141	0.083*
C6	0.6092 (6)	−0.1799 (4)	0.88440 (12)	0.0581 (12)
H6	0.5631	−0.2494	0.8659	0.070*
O1W	0.6667	0.3333	0.6735 (14)	0.26 (3)	0.50
H1W	0.5895	0.3288	0.6601	0.310*	0.6667
O2W	0.6667	0.3333	0.6459 (14)	0.30 (3)	0.50

	U11	U22	U33	U12	U13	U23
Mn	0.0289 (3)	0.0289 (3)	0.0195 (4)	0.01446 (13)	0.000	0.000
Na1	0.0312 (7)	0.0312 (7)	0.0225 (11)	0.0156 (4)	0.000	0.000
N1	0.0555 (16)	0.0401 (14)	0.0283 (13)	0.0266 (13)	−0.0171 (12)	−0.0075 (10)
O1	0.0624 (15)	0.0393 (12)	0.0297 (12)	0.0195 (12)	−0.0221 (12)	−0.0113 (10)
O2	0.0536 (14)	0.0337 (13)	0.0250 (11)	0.0213 (9)	−0.0148 (10)	−0.0030 (10)
O3	0.0703 (17)	0.0398 (13)	0.0283 (12)	0.0358 (13)	−0.0199 (12)	−0.0107 (11)
C1	0.0288 (14)	0.0302 (16)	0.0235 (13)	0.0110 (12)	−0.0031 (12)	−0.0034 (12)
C2	0.0360 (14)	0.0296 (14)	0.0269 (15)	0.0135 (13)	−0.0089 (12)	−0.0046 (12)
C3	0.0348 (15)	0.0314 (15)	0.0238 (13)	0.0180 (13)	−0.0069 (11)	−0.0005 (11)
C4	0.094 (3)	0.050 (2)	0.044 (2)	0.043 (2)	−0.031 (2)	−0.0023 (17)
C5	0.113 (4)	0.042 (2)	0.063 (2)	0.047 (3)	−0.041 (2)	−0.011 (2)
C6	0.091 (3)	0.0422 (19)	0.048 (2)	0.038 (2)	−0.034 (2)	−0.0189 (17)
O1W	0.31 (4)	0.31 (4)	0.16 (4)	0.15 (2)	0.000	0.000
O2W	0.34 (5)	0.34 (5)	0.23 (6)	0.17 (2)	0.000	0.000

Mn—O2	2.123 (3)	N1—H1N	0.9033
Mn—O2i	2.123 (3)	O1—C1	1.247 (4)
Mn—O2ii	2.123 (3)	O2—C1	1.260 (4)
Mn—O3	2.168 (2)	O3—C3	1.251 (4)
Mn—O3i	2.168 (2)	C1—C2	1.514 (4)
Mn—O3ii	2.168 (2)	C2—C6	1.370 (4)
Mn—Na1	3.314 (2)	C2—C3	1.437 (4)
Na1—O1iii	2.331 (2)	C4—C5	1.356 (6)
Na1—O1iv	2.331 (3)	C4—H4	0.9300
Na1—O1v	2.331 (2)	C5—C6	1.403 (6)
Na1—O3	2.459 (3)	C5—H5	0.9300
Na1—O3i	2.459 (3)	C6—H6	0.9300
Na1—O3ii	2.459 (3)	O1W—H1W	0.9106
N1—C4	1.339 (5)	O2W—H1W	0.9294
N1—C3	1.376 (4)
O2—Mn—O2i	94.91 (9)	O3—Na1—O3ii	69.00 (10)
O2—Mn—O2ii	94.91 (9)	O3i—Na1—O3ii	69.00 (10)
O2i—Mn—O2ii	94.91 (9)	O1iii—Na1—Mn	117.77 (8)
O2—Mn—O3	81.45 (8)	O1iv—Na1—Mn	117.77 (8)
O2i—Mn—O3	105.70 (10)	O1v—Na1—Mn	117.77 (8)
O2ii—Mn—O3	159.28 (9)	O3—Na1—Mn	40.85 (6)
O2—Mn—O3i	159.28 (9)	O3i—Na1—Mn	40.85 (6)
O2i—Mn—O3i	81.45 (8)	O3ii—Na1—Mn	40.85 (6)
O2ii—Mn—O3i	105.70 (10)	C4—N1—C3	125.0 (3)
O3—Mn—O3i	79.96 (10)	C4—N1—H1N	119.0
O2—Mn—O3ii	105.70 (11)	C3—N1—H1N	115.8
O2i—Mn—O3ii	159.28 (9)	C1—O1—Na1vi	163.8 (2)
O2ii—Mn—O3ii	81.45 (8)	C1—O2—Mn	137.3 (2)
O3—Mn—O3ii	79.96 (10)	C3—O3—Mn	130.64 (19)
O3i—Mn—O3ii	79.96 (10)	C3—O3—Na1	133.1 (2)
O2—Mn—Na1	121.71 (7)	Mn—O3—Na1	91.26 (9)
O2i—Mn—Na1	121.71 (7)	O1—C1—O2	122.4 (3)
O2ii—Mn—Na1	121.71 (7)	O1—C1—C2	117.4 (3)
O3—Mn—Na1	47.89 (6)	O2—C1—C2	120.3 (3)
O3i—Mn—Na1	47.89 (7)	C6—C2—C3	118.6 (3)
O3ii—Mn—Na1	47.89 (6)	C6—C2—C1	119.5 (3)
O1iii—Na1—O1iv	100.04 (10)	C3—C2—C1	121.8 (2)
O1iii—Na1—O1v	100.04 (10)	O3—C3—N1	116.6 (3)
O1iv—Na1—O1v	100.04 (10)	O3—C3—C2	127.8 (3)
O1iii—Na1—O3	149.83 (11)	N1—C3—C2	115.6 (2)
O1iv—Na1—O3	109.27 (10)	N1—C4—C5	120.4 (4)
O1v—Na1—O3	82.12 (8)	N1—C4—H4	119.8
O1iii—Na1—O3i	82.12 (8)	C5—C4—H4	119.8
O1iv—Na1—O3i	149.83 (11)	C4—C5—C6	117.8 (3)
O1v—Na1—O3i	109.27 (10)	C4—C5—H5	121.1
O3—Na1—O3i	69.00 (10)	C6—C5—H5	121.1
O1iii—Na1—O3ii	109.27 (10)	C2—C6—C5	122.5 (4)
O1iv—Na1—O3ii	82.12 (8)	C2—C6—H6	118.7
O1v—Na1—O3ii	149.83 (11)	C5—C6—H6	118.7

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···O1v	0.90	2.12	2.983 (4)	161
N1—H1N···O2v	0.90	2.37	3.113 (4)	140

Table 1

Selected bond lengths (Å)

Mn—O2	2.123 (3)
Mn—O3	2.168 (2)
Na1—O1i	2.331 (2)
Na1—O3	2.459 (3)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1N⋯O1ii	0.90	2.12	2.983 (4)	161
N1—H1N⋯O2ii	0.90	2.37	3.113 (4)	140

Symmetry code: (ii) .