Diaqua-bis-(seleno-cyanato-κN)bis-(pyrimidine-κN)manganese(II).

In the crystal structure of the title compound, [Mn(NCSe)(2)(C(4)H(4)N(2))(2)(H(2)O)(2)], the manganese(II) cation is coordinated by two N-bonded pyrimidine ligands, two N-bonded seleno-cyanate anions and two O-bonded water mol-ecules in a distorted octa-hedral coordination mode. The asymmetric unit consists of one manganese(II) cation, located on a centre of inversion, as well as one seleno-cyanate anion, one water mol-ecule and one pyrimidine ligand in general positions. The crystal structure consists of discrete building blocks of composition [Mn(NCSe)(2)(pyrimidine)(2)(H(2)O)(2)], which are connected into layers parallel to (101) by strong water-pyrimidine O-H⋯N hydrogen bonds.

Related literature

For a related pyrimidine structure, see: Lipkowski & Soldatov (1993 ▶). For general background to the use of thermal decomposition reactions for the discovery and preparation of new ligand-deficient coordination polymers with defined magnetic properties, see: Wriedt & Näther (2009a ▶,b ▶); Wriedt et al. (2009a ▶,b ▶).

Experimental

Crystal data

[Mn(CNSe)2(C4H4N2)2(H2O)2]

M = 461.12

Monoclinic,

a = 9.2402 (7) Å

b = 9.6012 (6) Å

c = 10.2099 (8) Å

β = 111.505 (8)°

V = 842.74 (11) Å3

Z = 2

Mo Kα radiation

μ = 5.11 mm−1

T = 170 K

0.10 × 0.07 × 0.04 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.653, T max = 0.818

9472 measured reflections

2024 independent reflections

1795 reflections with I > 2σ(I)

R int = 0.043

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 0.064

S = 1.03

2024 reflections

98 parameters

H-atom parameters constrained

Δρmax = 0.50 e Å−3

Δρmin = −0.51 e Å−3

Data collection: X-AREA (Stoe & Cie, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; 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: XCIF in SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810028941/bv2144sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810028941/bv2144Isup2.hkl

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

[Mn(CNSe)2(C4H4N2)2(H2O)2]	F(000) = 446
Mr = 461.12	Dx = 1.817 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 9472 reflections
a = 9.2402 (7) Å	θ = 2.6–28.0°
b = 9.6012 (6) Å	µ = 5.11 mm−1
c = 10.2099 (8) Å	T = 170 K
β = 111.505 (8)°	Block, colourless
V = 842.74 (11) Å3	0.10 × 0.07 × 0.04 mm
Z = 2

Stoe IPDS-1 diffractometer	2024 independent reflections
Radiation source: fine-focus sealed tube	1795 reflections with I > 2σ(I)
graphite	Rint = 0.043
Phi scans	θmax = 28.0°, θmin = 2.6°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −12→12
Tmin = 0.653, Tmax = 0.818	k = −12→12
9472 measured reflections	l = −13→13

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)] = 0.026	H-atom parameters constrained
wR(F2) = 0.064	w = 1/[σ2(Fo2) + (0.0376P)2 + 0.3681P] where P = (Fo2 + 2Fc2)/3
S = 1.03	(Δ/σ)max = 0.002
2024 reflections	Δρmax = 0.50 e Å−3
98 parameters	Δρmin = −0.51 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0110 (14)

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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
Mn1	0.5000	1.0000	0.5000	0.01759 (12)
N1	0.4202 (2)	0.77991 (19)	0.54320 (18)	0.0208 (4)
N2	0.3036 (2)	0.5623 (2)	0.45030 (19)	0.0289 (4)
C1	0.3525 (3)	0.6901 (3)	0.4381 (2)	0.0265 (5)
H1	0.3380	0.7208	0.3456	0.032*
C2	0.3267 (3)	0.5183 (3)	0.5807 (2)	0.0298 (5)
H2	0.2947	0.4271	0.5938	0.036*
C3	0.3961 (3)	0.6023 (3)	0.6969 (2)	0.0299 (5)
H3	0.4128	0.5705	0.7894	0.036*
C4	0.4398 (3)	0.7336 (2)	0.6731 (2)	0.0261 (5)
H4	0.4856	0.7940	0.7511	0.031*
N11	0.7272 (2)	0.9064 (2)	0.5380 (2)	0.0300 (4)
C11	0.8449 (2)	0.8544 (2)	0.5539 (2)	0.0214 (4)
Se11	1.02886 (3)	0.77302 (3)	0.58075 (3)	0.02776 (10)
O1	0.42680 (19)	0.94905 (18)	0.27927 (15)	0.0283 (3)
H1O1	0.4782	0.9061	0.2392	0.042*
H2O1	0.3448	0.9730	0.2134	0.042*

	U11	U22	U33	U12	U13	U23
Mn1	0.0178 (2)	0.0179 (2)	0.0143 (2)	0.00340 (15)	0.00258 (15)	−0.00073 (14)
N1	0.0200 (8)	0.0227 (9)	0.0175 (8)	−0.0008 (7)	0.0044 (7)	−0.0010 (6)
N2	0.0341 (10)	0.0270 (11)	0.0222 (9)	−0.0077 (8)	0.0061 (7)	−0.0039 (7)
C1	0.0300 (11)	0.0291 (12)	0.0185 (10)	−0.0042 (9)	0.0068 (8)	−0.0022 (8)
C2	0.0345 (12)	0.0246 (12)	0.0279 (11)	−0.0045 (9)	0.0086 (9)	0.0002 (9)
C3	0.0381 (12)	0.0285 (12)	0.0200 (10)	−0.0020 (10)	0.0070 (9)	0.0028 (9)
C4	0.0289 (11)	0.0253 (11)	0.0191 (9)	−0.0015 (9)	0.0030 (8)	−0.0021 (8)
N11	0.0230 (9)	0.0297 (11)	0.0367 (10)	0.0060 (8)	0.0101 (8)	0.0036 (8)
C11	0.0218 (9)	0.0218 (10)	0.0205 (9)	−0.0012 (8)	0.0078 (7)	0.0022 (7)
Se11	0.02287 (14)	0.02978 (16)	0.03597 (15)	0.00821 (9)	0.01709 (10)	0.00904 (9)
O1	0.0356 (8)	0.0300 (9)	0.0136 (6)	0.0116 (7)	0.0024 (6)	−0.0026 (6)

Mn1—O1	2.1582 (14)	C1—H1	0.9500
Mn1—O1i	2.1582 (14)	C2—C3	1.383 (3)
Mn1—N11	2.1840 (19)	C2—H2	0.9500
Mn1—N11i	2.1840 (19)	C3—C4	1.372 (3)
Mn1—N1i	2.3328 (18)	C3—H3	0.9500
Mn1—N1	2.3328 (18)	C4—H4	0.9500
N1—C1	1.340 (3)	N11—C11	1.153 (3)
N1—C4	1.347 (3)	C11—Se11	1.798 (2)
N2—C1	1.329 (3)	O1—H1O1	0.8400
N2—C2	1.337 (3)	O1—H2O1	0.8400
O1—Mn1—O1i	180.0	C1—N2—C2	116.70 (19)
O1—Mn1—N11	90.29 (7)	N2—C1—N1	126.4 (2)
O1i—Mn1—N11	89.71 (7)	N2—C1—H1	116.8
O1—Mn1—N11i	89.71 (7)	N1—C1—H1	116.8
O1i—Mn1—N11i	90.29 (7)	N2—C2—C3	121.7 (2)
N11—Mn1—N11i	180.0	N2—C2—H2	119.2
O1—Mn1—N1i	90.44 (6)	C3—C2—H2	119.2
O1i—Mn1—N1i	89.56 (6)	C4—C3—C2	117.2 (2)
N11—Mn1—N1i	93.23 (7)	C4—C3—H3	121.4
N11i—Mn1—N1i	86.77 (7)	C2—C3—H3	121.4
O1—Mn1—N1	89.56 (6)	N1—C4—C3	122.4 (2)
O1i—Mn1—N1	90.44 (6)	N1—C4—H4	118.8
N11—Mn1—N1	86.77 (7)	C3—C4—H4	118.8
N11i—Mn1—N1	93.23 (7)	C11—N11—Mn1	177.7 (2)
N1i—Mn1—N1	180.00 (9)	N11—C11—Se11	179.4 (2)
C1—N1—C4	115.56 (19)	Mn1—O1—H1O1	127.1
C1—N1—Mn1	121.24 (15)	Mn1—O1—H2O1	128.3
C4—N1—Mn1	123.19 (14)	H1O1—O1—H2O1	104.5

D—H···A	D—H	H···A	D···A	D—H···A
O1—H2O1···N2ii	0.84	1.93	2.748 (2)	164

Mn1—O1	2.1582 (14)
Mn1—N11	2.1840 (19)
Mn1—N1	2.3328 (18)

O1—Mn1—O1i	180.0
O1—Mn1—N11	90.29 (7)
O1i—Mn1—N11	89.71 (7)
O1—Mn1—N1i	90.44 (6)
N11—Mn1—N1i	93.23 (7)
N11i—Mn1—N1i	86.77 (7)
O1—Mn1—N1	89.56 (6)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H2O1⋯N2ii	0.84	1.93	2.748 (2)	164

Symmetry code: (ii) .