Poly[tetra-kis-(seleno-cyanato-κN)bis-(methanol-κO)tris-(μ-pyrimidine-κN:N')dicobalt(II)].

In the title compound, [Co(2)(NCSe)(4)(C(4)H(4)N(2))(3)(CH(3)OH)(2)](n), the Co(II) ion is coordinated by three N-bonded pyrimidine ligands, two N-bonded seleno-cyanate anions and one O-bonded methanol mol-ecule in an octa-hedral coordination mode. The asymmetric unit consists of one Co(II) ion, one pyrimidine ligand, two seleno-cyanate anions and one methanol mol-ecule in general positions as well as one pyrimidine ligand located around a twofold rotation axis. In the crystal structure, the pyrimidine ligands bridge [Co(CNSe)(2)(CH(3)OH)] units into zigzag-like chains, which are further connected by pyrimidine ligands into layers parallel to (010).

Related literature

For general background, see: Wriedt & Näther (2009a ▶,b ▶); Wriedt, Sellmer & Näther (2009a ▶,b ▶). For the isotypic structure of a nickel thio­cyanato complex, see: Wriedt et al. (2009 ▶).

Experimental

Crystal data

[Co2(CNSe)4(C4H4N2)3(CH4O)2]

M = 421.07

Orthorhombic,

a = 20.4069 (8) Å

b = 33.0633 (15) Å

c = 8.3750 (3) Å

V = 5650.8 (4) Å3

Z = 16

Mo Kα radiation

μ = 6.36 mm−1

T = 293 K

0.16 × 0.11 × 0.02 mm

Data collection

Stoe IPDS-2 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2002 ▶) T min = 0.431, T max = 0.885

18545 measured reflections

3391 independent reflections

3067 reflections with I > 2σ(I)

R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.069

S = 1.16

3391 reflections

164 parameters

1 restraint

H-atom parameters constrained

Δρmax = 0.55 e Å−3

Δρmin = −0.35 e Å−3

Absolute structure: Flack (1983 ▶), 1579 Friedel pairs

Flack parameter: 0.057 (13)

Data collection: X-AREA (Stoe & Cie, 2002 ▶); 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: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681002060X/hy2313sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053681002060X/hy2313Isup2.hkl

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

[Co2(CNSe)4(C4H4N2)3(CH4O)2]	F(000) = 3232
Mr = 421.07	Dx = 1.980 Mg m−3
Orthorhombic, Fdd2	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: F 2 -2d	Cell parameters from 18545 reflections
a = 20.4069 (8) Å	θ = 2.4–28.0°
b = 33.0633 (15) Å	µ = 6.36 mm−1
c = 8.3750 (3) Å	T = 293 K
V = 5650.8 (4) Å3	Block, light pink
Z = 16	0.16 × 0.11 × 0.02 mm

Stoe IPDS-2 diffractometer	3391 independent reflections
Radiation source: fine-focus sealed tube	3067 reflections with I > 2σ(I)
graphite	Rint = 0.044
ω scans	θmax = 28.0°, θmin = 2.4°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2002)	h = −26→26
Tmin = 0.431, Tmax = 0.885	k = −43→43
18545 measured reflections	l = −11→10

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)] = 0.038	H-atom parameters constrained
wR(F2) = 0.069	w = 1/[σ2(Fo2) + (0.0286P)2 + 8.8704P] where P = (Fo2 + 2Fc2)/3
S = 1.16	(Δ/σ)max < 0.001
3391 reflections	Δρmax = 0.55 e Å−3
164 parameters	Δρmin = −0.35 e Å−3
1 restraint	Absolute structure: Flack (1983), 1579 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.057 (13)

	x	y	z	Uiso*/Ueq
Co1	0.60574 (2)	0.227474 (17)	0.78759 (6)	0.03270 (12)
N1	0.55104 (15)	0.27269 (10)	0.6504 (4)	0.0360 (8)
N2	0.47521 (15)	0.28919 (10)	0.4458 (5)	0.0382 (7)
C1	0.50711 (17)	0.26316 (13)	0.5388 (6)	0.0374 (9)
H1	0.4979	0.2358	0.5246	0.045*
C2	0.4883 (2)	0.32854 (13)	0.4677 (6)	0.0412 (9)
H2	0.4672	0.3477	0.4048	0.049*
C3	0.5320 (2)	0.34078 (14)	0.5813 (6)	0.0459 (11)
H3	0.5410	0.3681	0.5959	0.055*
C4	0.5623 (2)	0.31226 (13)	0.6730 (6)	0.0434 (10)
H4	0.5912	0.3204	0.7526	0.052*
N11	0.69371 (15)	0.24124 (11)	0.6493 (4)	0.0352 (8)
C11	0.7500	0.2500	0.7228 (7)	0.0372 (12)
H11	0.7500	0.2500	0.8339	0.045*
C13	0.7500	0.2500	0.4059 (8)	0.061 (2)
H13	0.7500	0.2500	0.2948	0.074*
C14	0.6944 (2)	0.24140 (17)	0.4914 (6)	0.0499 (12)
H14	0.6559	0.2355	0.4366	0.060*
N21	0.57994 (17)	0.18287 (12)	0.6270 (5)	0.0434 (8)
C21	0.56005 (17)	0.15562 (13)	0.5553 (5)	0.0381 (9)
Se21	0.53008 (3)	0.114405 (17)	0.44108 (7)	0.06121 (16)
N31	0.63231 (16)	0.26940 (12)	0.9575 (5)	0.0428 (8)
C31	0.63448 (17)	0.29139 (13)	1.0643 (5)	0.0373 (9)
Se31	0.63665 (3)	0.324181 (19)	1.23170 (7)	0.06461 (17)
O41	0.66187 (15)	0.18255 (10)	0.9111 (4)	0.0522 (8)
C41	0.6758 (4)	0.1790 (2)	1.0749 (8)	0.085 (2)
H41A	0.6359	0.1747	1.1328	0.127*
H41B	0.6964	0.2034	1.1118	0.127*
H41C	0.7048	0.1566	1.0918	0.127*
H1O4	0.6862	0.1792	0.8352	0.127*

	U11	U22	U33	U12	U13	U23
Co1	0.0252 (2)	0.0341 (3)	0.0388 (3)	−0.0009 (2)	−0.0010 (2)	−0.0043 (2)
N1	0.0287 (15)	0.0336 (18)	0.046 (2)	−0.0015 (13)	−0.0036 (13)	0.0000 (15)
N2	0.0294 (14)	0.0376 (17)	0.048 (2)	−0.0013 (14)	−0.0020 (14)	0.0017 (17)
C1	0.0270 (16)	0.036 (2)	0.049 (2)	0.0006 (15)	−0.0018 (18)	−0.0026 (19)
C2	0.045 (2)	0.033 (2)	0.045 (2)	0.0008 (17)	−0.0001 (19)	0.0031 (19)
C3	0.059 (3)	0.029 (2)	0.049 (3)	−0.0082 (19)	0.003 (2)	−0.0002 (19)
C4	0.048 (2)	0.039 (2)	0.043 (2)	−0.0022 (18)	−0.0087 (19)	−0.0029 (19)
N11	0.0268 (14)	0.0419 (19)	0.037 (2)	−0.0028 (13)	−0.0005 (13)	0.0017 (14)
C11	0.029 (2)	0.050 (3)	0.032 (3)	0.000 (2)	0.000	0.000
C13	0.046 (4)	0.108 (7)	0.030 (4)	−0.001 (4)	0.000	0.000
C14	0.0295 (19)	0.075 (3)	0.045 (3)	−0.005 (2)	−0.0032 (18)	−0.003 (2)
N21	0.0422 (18)	0.040 (2)	0.048 (2)	0.0000 (16)	−0.0047 (16)	−0.0091 (17)
C21	0.0304 (16)	0.043 (2)	0.042 (2)	0.0029 (16)	0.0016 (17)	0.002 (2)
Se21	0.0661 (3)	0.0505 (3)	0.0670 (4)	−0.0056 (2)	−0.0100 (3)	−0.0199 (3)
N31	0.0419 (18)	0.045 (2)	0.042 (2)	−0.0081 (16)	0.0024 (16)	−0.0071 (18)
C31	0.0276 (17)	0.039 (2)	0.046 (3)	−0.0020 (15)	0.0036 (16)	0.003 (2)
Se31	0.0715 (3)	0.0632 (4)	0.0592 (3)	−0.0041 (3)	0.0086 (3)	−0.0256 (3)
O41	0.0456 (16)	0.054 (2)	0.057 (2)	0.0146 (15)	−0.0044 (15)	0.0063 (16)
C41	0.101 (5)	0.071 (4)	0.082 (5)	0.002 (4)	−0.047 (4)	0.007 (3)

Co1—N1	2.191 (3)	N11—C11	1.335 (4)
Co1—N2i	2.188 (3)	C11—N11ii	1.335 (4)
Co1—N11	2.184 (3)	C11—H11	0.9300
Co1—N21	2.064 (4)	C13—C14	1.372 (6)
Co1—N31	2.059 (4)	C13—C14ii	1.372 (6)
Co1—O41	2.142 (3)	C13—H13	0.9300
N1—C1	1.333 (5)	C14—H14	0.9300
N1—C4	1.342 (5)	N21—C21	1.157 (5)
N2—C1	1.331 (5)	C21—Se21	1.774 (5)
N2—C2	1.341 (5)	N31—C31	1.154 (5)
C1—H1	0.9300	C31—Se31	1.773 (4)
C2—C3	1.366 (6)	O41—C41	1.405 (7)
C2—H2	0.9300	O41—H1O4	0.8139
C3—C4	1.364 (7)	C41—H41A	0.9600
C3—H3	0.9300	C41—H41B	0.9600
C4—H4	0.9300	C41—H41C	0.9600
N11—C14	1.323 (6)
N31—Co1—N21	176.69 (16)	C2—C3—H3	120.6
N31—Co1—O41	89.55 (15)	N1—C4—C3	121.2 (4)
N21—Co1—O41	87.46 (14)	N1—C4—H4	119.4
N31—Co1—N11	90.55 (13)	C3—C4—H4	119.4
N21—Co1—N11	90.75 (14)	C14—N11—C11	116.8 (4)
O41—Co1—N11	87.77 (13)	C14—N11—Co1	122.6 (3)
N31—Co1—N2i	87.12 (14)	C11—N11—Co1	120.5 (3)
N21—Co1—N2i	91.27 (14)	N11—C11—N11ii	125.1 (5)
O41—Co1—N2i	86.37 (13)	N11—C11—H11	117.5
N11—Co1—N2i	173.71 (13)	N11ii—C11—H11	117.5
N31—Co1—N1	92.13 (14)	C14—C13—C14ii	117.1 (6)
N21—Co1—N1	90.91 (14)	C14—C13—H13	121.5
O41—Co1—N1	177.16 (14)	C14ii—C13—H13	121.5
N11—Co1—N1	89.92 (12)	N11—C14—C13	122.1 (4)
N2i—Co1—N1	96.00 (13)	N11—C14—H14	118.9
C1—N1—C4	116.4 (4)	C13—C14—H14	118.9
C1—N1—Co1	123.3 (3)	C21—N21—Co1	169.9 (4)
C4—N1—Co1	120.3 (3)	N21—C21—Se21	178.7 (4)
C1—N2—C2	116.8 (4)	C31—N31—Co1	166.0 (3)
C1—N2—Co1iii	124.1 (3)	N31—C31—Se31	178.4 (4)
C2—N2—Co1iii	118.5 (3)	C41—O41—Co1	129.6 (4)
N2—C1—N1	125.9 (4)	C41—O41—H1O4	128.9
N2—C1—H1	117.0	Co1—O41—H1O4	92.4
N1—C1—H1	117.0	O41—C41—H41A	109.5
N2—C2—C3	120.8 (4)	O41—C41—H41B	109.5
N2—C2—H2	119.6	H41A—C41—H41B	109.5
C3—C2—H2	119.6	O41—C41—H41C	109.5
C4—C3—C2	118.9 (4)	H41A—C41—H41C	109.5
C4—C3—H3	120.6	H41B—C41—H41C	109.5

Table 1

Selected bond lengths (Å)

Co1—N1	2.191 (3)
Co1—N2i	2.188 (3)
Co1—N11	2.184 (3)
Co1—N21	2.064 (4)
Co1—N31	2.059 (4)
Co1—O41	2.142 (3)

Symmetry code: (i) .