Di-μ-sulfato-κO:O'-bis-[diaqua-(1H-imidazo[4,5-f][1,10]phenanthroline-κN,N)cobalt(II)] dihydrate.

In the centrosymmetric dinuclear title compound, [Co(2)(SO(4))(2)(C(13)H(8)N(4))(2)(H(2)O)(4)]·2H(2)O, the Co(II) atom is coord-in-ated by two N atoms from two 1H-imidazo[4,5-f][1,10]phenanthroline ligands, two O atoms from two sulfate anions and two O atoms from water mol-ecules in a distorted octa-hedral geometry. The Co⋯Co separation is 5.1167 (7) Å. The coordinated and uncoordinated water mol-ecules engage in N-H⋯O and O-H⋯O hydrogen-bonding inter-actions.

Related literature

For related compounds, see: Jing et al. (2000 ▶, 2004 ▶); Nagababu & Satyanarayana (2007 ▶); Selvi & Palaniandavar (2002 ▶); Shavaleev et al. (2007 ▶); Wang et al. (2008 ▶); Wu et al. (1997 ▶).

Experimental

Crystal data

[Co2(SO4)2(C13H8N4)2(H2O)4]·2H2O

M = 858.54

Monoclinic,

a = 10.3160 (13) Å

b = 9.0716 (10) Å

c = 16.8549 (17) Å

β = 99.1040 (10)°

V = 1557.5 (3) Å3

Z = 2

Mo Kα radiation

μ = 1.29 mm−1

T = 298 K

0.43 × 0.36 × 0.22 mm

Data collection

Siemens SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.581, T max = 0.754

7558 measured reflections

2742 independent reflections

2329 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.027

wR(F 2) = 0.073

S = 1.07

2742 reflections

235 parameters

H-atom parameters constrained

Δρmax = 0.63 e Å−3

Δρmin = −0.36 e Å−3

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; 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 global, I. DOI: 10.1107/S1600536809024295/ng2604sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809024295/ng2604Isup2.hkl

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

[Co2(SO4)2(C13H8N4)2(H2O)4]·2H2O	F(000) = 876
Mr = 858.54	Dx = 1.831 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 7558 reflections
a = 10.3160 (13) Å	θ = 2.0–25.0°
b = 9.0716 (10) Å	µ = 1.29 mm−1
c = 16.8549 (17) Å	T = 298 K
β = 99.104 (1)°	Block, brown
V = 1557.5 (3) Å3	0.43 × 0.36 × 0.22 mm
Z = 2

Siemens SMART CCD area-detector diffractometer	2742 independent reflections
Radiation source: fine-focus sealed tube	2329 reflections with I > 2σ(I)
graphite	Rint = 0.020
φ and ω scans	θmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→8
Tmin = 0.581, Tmax = 0.754	k = −10→10
7558 measured reflections	l = −19→20

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073	H-atom parameters constrained
S = 1.07	w = 1/[σ2(Fo2) + (0.0289P)2 + 1.5148P] where P = (Fo2 + 2Fc2)/3
2742 reflections	(Δ/σ)max < 0.001
235 parameters	Δρmax = 0.63 e Å−3
0 restraints	Δρmin = −0.36 e Å−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 > 2sigma(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
Co1	0.68903 (3)	0.31926 (4)	0.04124 (2)	0.02494 (12)
N1	0.8745 (2)	0.3237 (2)	0.11677 (12)	0.0266 (5)
N2	0.75649 (19)	0.0980 (2)	0.03284 (12)	0.0254 (5)
N3	1.2464 (2)	−0.0127 (2)	0.20274 (13)	0.0326 (5)
H3	1.3069	0.0380	0.2315	0.039*
N4	1.1436 (2)	−0.2056 (2)	0.13930 (13)	0.0339 (5)
O1	0.53904 (16)	0.29041 (18)	−0.05637 (10)	0.0302 (4)
O2	0.63548 (17)	0.53058 (18)	0.07489 (11)	0.0339 (4)
O3	0.56078 (16)	0.51259 (19)	−0.13340 (10)	0.0307 (4)
O4	0.40919 (19)	0.3224 (2)	−0.18590 (11)	0.0399 (5)
O5	0.79510 (17)	0.4343 (2)	−0.03947 (10)	0.0323 (4)
H5A	0.7307	0.4726	−0.0703	0.039*
H5B	0.8276	0.3690	−0.0667	0.039*
O6	0.5767 (2)	0.2368 (2)	0.12221 (12)	0.0472 (5)
H6A	0.5151	0.2917	0.1330	0.057*
H6B	0.5745	0.1555	0.1470	0.057*
O7	0.5866 (3)	0.9854 (2)	0.20115 (13)	0.0658 (7)
H7A	0.5836	0.8952	0.1873	0.079*
H7B	0.5822	0.9896	0.2510	0.079*
S1	0.46794 (6)	0.39915 (6)	−0.11220 (4)	0.02442 (15)
C1	0.9322 (3)	0.4409 (3)	0.15383 (16)	0.0312 (6)
H1	0.8867	0.5298	0.1501	0.037*
C2	1.0586 (3)	0.4365 (3)	0.19832 (16)	0.0335 (6)
H2	1.0963	0.5212	0.2232	0.040*
C3	1.1263 (3)	0.3062 (3)	0.20491 (16)	0.0322 (6)
H3A	1.2097	0.3008	0.2352	0.039*
C4	1.0685 (2)	0.1811 (3)	0.16548 (14)	0.0255 (5)
C5	0.9415 (2)	0.1946 (3)	0.12104 (14)	0.0239 (5)
C6	0.8762 (2)	0.0708 (3)	0.07713 (14)	0.0231 (5)
C7	0.9348 (2)	−0.0701 (3)	0.08041 (14)	0.0247 (5)
C8	0.8635 (3)	−0.1852 (3)	0.03828 (16)	0.0304 (6)
H8	0.8987	−0.2797	0.0390	0.036*
C9	0.7410 (3)	−0.1567 (3)	−0.00397 (16)	0.0333 (6)
H9	0.6916	−0.2323	−0.0310	0.040*
C10	0.6914 (2)	−0.0137 (3)	−0.00605 (15)	0.0305 (6)
H10	0.6092	0.0044	−0.0359	0.037*
C11	1.1259 (2)	0.0376 (3)	0.16564 (15)	0.0265 (5)
C12	1.0637 (2)	−0.0818 (3)	0.12648 (15)	0.0260 (5)
C13	1.2505 (3)	−0.1568 (3)	0.18502 (17)	0.0378 (7)
H13	1.3222	−0.2167	0.2033	0.045*

	U11	U22	U33	U12	U13	U23
Co1	0.02401 (19)	0.02377 (19)	0.0260 (2)	0.00539 (14)	0.00088 (13)	0.00188 (14)
N1	0.0291 (11)	0.0243 (11)	0.0257 (11)	0.0054 (9)	0.0026 (9)	0.0006 (9)
N2	0.0233 (11)	0.0275 (11)	0.0246 (11)	0.0037 (9)	0.0015 (8)	0.0013 (9)
N3	0.0276 (11)	0.0378 (12)	0.0288 (12)	0.0042 (10)	−0.0068 (9)	−0.0011 (10)
N4	0.0355 (12)	0.0316 (12)	0.0328 (13)	0.0118 (10)	0.0004 (10)	0.0020 (10)
O1	0.0297 (9)	0.0255 (9)	0.0323 (10)	0.0025 (7)	−0.0046 (8)	0.0043 (8)
O2	0.0317 (10)	0.0241 (9)	0.0478 (11)	0.0049 (8)	0.0117 (8)	−0.0021 (8)
O3	0.0310 (9)	0.0289 (9)	0.0325 (10)	0.0035 (8)	0.0061 (8)	0.0049 (8)
O4	0.0504 (12)	0.0338 (10)	0.0302 (10)	0.0044 (9)	−0.0102 (9)	−0.0075 (8)
O5	0.0311 (10)	0.0350 (10)	0.0307 (10)	0.0052 (8)	0.0044 (8)	0.0005 (8)
O6	0.0587 (13)	0.0317 (10)	0.0586 (14)	0.0165 (10)	0.0318 (11)	0.0167 (10)
O7	0.129 (2)	0.0306 (11)	0.0426 (13)	0.0143 (13)	0.0287 (14)	0.0071 (10)
S1	0.0258 (3)	0.0217 (3)	0.0239 (3)	0.0051 (2)	−0.0016 (2)	−0.0010 (2)
C1	0.0388 (15)	0.0237 (13)	0.0308 (14)	0.0034 (11)	0.0046 (11)	−0.0012 (11)
C2	0.0372 (15)	0.0291 (14)	0.0335 (15)	−0.0045 (12)	0.0029 (12)	−0.0052 (11)
C3	0.0273 (13)	0.0356 (15)	0.0315 (15)	−0.0006 (11)	−0.0023 (11)	−0.0032 (12)
C4	0.0254 (13)	0.0284 (13)	0.0224 (13)	0.0026 (11)	0.0025 (10)	0.0003 (10)
C5	0.0257 (13)	0.0232 (12)	0.0228 (13)	0.0039 (10)	0.0037 (10)	0.0014 (10)
C6	0.0246 (12)	0.0233 (12)	0.0211 (12)	0.0029 (10)	0.0029 (10)	0.0020 (10)
C7	0.0275 (13)	0.0249 (12)	0.0219 (13)	0.0021 (10)	0.0046 (10)	0.0035 (10)
C8	0.0370 (14)	0.0219 (13)	0.0320 (14)	0.0029 (11)	0.0051 (11)	0.0001 (11)
C9	0.0349 (15)	0.0283 (14)	0.0349 (15)	−0.0056 (11)	0.0002 (12)	−0.0039 (12)
C10	0.0245 (13)	0.0341 (14)	0.0309 (14)	0.0003 (11)	−0.0015 (10)	−0.0023 (12)
C11	0.0245 (12)	0.0303 (13)	0.0240 (13)	0.0058 (11)	0.0014 (10)	0.0030 (11)
C12	0.0284 (13)	0.0267 (13)	0.0230 (13)	0.0071 (10)	0.0047 (10)	0.0029 (10)
C13	0.0368 (16)	0.0401 (16)	0.0341 (16)	0.0169 (13)	−0.0021 (12)	0.0036 (12)

Co1—N1	2.124 (2)	O7—H7A	0.8500
Co1—N2	2.137 (2)	O7—H7B	0.8500
Co1—O6	2.0654 (19)	S1—O2i	1.4671 (18)
Co1—O1	2.0889 (17)	C1—C2	1.398 (4)
Co1—O2	2.0978 (17)	C1—H1	0.9300
Co1—O5	2.1468 (18)	C2—C3	1.369 (4)
N1—C1	1.326 (3)	C2—H2	0.9300
N1—C5	1.356 (3)	C3—C4	1.400 (3)
N2—C10	1.330 (3)	C3—H3A	0.9300
N2—C6	1.360 (3)	C4—C5	1.408 (3)
N3—C13	1.343 (3)	C4—C11	1.430 (3)
N3—C11	1.378 (3)	C5—C6	1.451 (3)
N3—H3	0.8600	C6—C7	1.411 (3)
N4—C13	1.318 (4)	C7—C8	1.404 (3)
N4—C12	1.390 (3)	C7—C12	1.433 (3)
O1—S1	1.4758 (17)	C8—C9	1.373 (4)
O2—S1i	1.4671 (18)	C8—H8	0.9300
O3—S1	1.4873 (18)	C9—C10	1.393 (4)
O4—S1	1.4689 (18)	C9—H9	0.9300
O5—H5A	0.8500	C10—H10	0.9300
O5—H5B	0.8501	C11—C12	1.374 (3)
O6—H6A	0.8499	C13—H13	0.9300
O6—H6B	0.8499
O6—Co1—O1	92.97 (8)	N1—C1—C2	122.7 (2)
O6—Co1—O2	87.31 (7)	N1—C1—H1	118.6
O1—Co1—O2	97.67 (7)	C2—C1—H1	118.6
O6—Co1—N1	99.04 (8)	C3—C2—C1	119.3 (2)
O1—Co1—N1	163.56 (8)	C3—C2—H2	120.4
O2—Co1—N1	94.09 (7)	C1—C2—H2	120.4
O6—Co1—N2	85.76 (8)	C2—C3—C4	119.2 (2)
O1—Co1—N2	92.21 (7)	C2—C3—H3A	120.4
O2—Co1—N2	168.21 (8)	C4—C3—H3A	120.4
N1—Co1—N2	77.62 (7)	C3—C4—C5	118.2 (2)
O6—Co1—O5	172.06 (7)	C3—C4—C11	126.3 (2)
O1—Co1—O5	87.15 (7)	C5—C4—C11	115.5 (2)
O2—Co1—O5	84.80 (7)	N1—C5—C4	121.8 (2)
N1—Co1—O5	82.50 (7)	N1—C5—C6	116.8 (2)
N2—Co1—O5	102.17 (7)	C4—C5—C6	121.4 (2)
C1—N1—C5	118.7 (2)	N2—C6—C7	122.1 (2)
C1—N1—Co1	126.32 (17)	N2—C6—C5	116.6 (2)
C5—N1—Co1	114.74 (16)	C7—C6—C5	121.3 (2)
C10—N2—C6	118.4 (2)	C8—C7—C6	117.8 (2)
C10—N2—Co1	127.18 (16)	C8—C7—C12	125.9 (2)
C6—N2—Co1	114.27 (16)	C6—C7—C12	116.3 (2)
C13—N3—C11	106.2 (2)	C9—C8—C7	119.2 (2)
C13—N3—H3	126.9	C9—C8—H8	120.4
C11—N3—H3	126.9	C7—C8—H8	120.4
C13—N4—C12	103.9 (2)	C8—C9—C10	119.6 (2)
S1—O1—Co1	130.53 (10)	C8—C9—H9	120.2
S1i—O2—Co1	138.89 (11)	C10—C9—H9	120.2
Co1—O5—H5A	99.1	N2—C10—C9	122.8 (2)
Co1—O5—H5B	106.7	N2—C10—H10	118.6
H5A—O5—H5B	107.0	C9—C10—H10	118.6
Co1—O6—H6A	116.5	C12—C11—N3	106.0 (2)
Co1—O6—H6B	134.5	C12—C11—C4	123.7 (2)
H6A—O6—H6B	108.9	N3—C11—C4	130.2 (2)
H7A—O7—H7B	108.0	C11—C12—N4	110.0 (2)
O2i—S1—O4	109.74 (11)	C11—C12—C7	121.7 (2)
O2i—S1—O1	109.81 (11)	N4—C12—C7	128.4 (2)
O4—S1—O1	108.62 (10)	N4—C13—N3	113.8 (2)
O2i—S1—O3	109.99 (10)	N4—C13—H13	123.1
O4—S1—O3	108.67 (11)	N3—C13—H13	123.1
O1—S1—O3	109.98 (10)
O6—Co1—N1—C1	−100.4 (2)	Co1—N1—C5—C6	−2.7 (3)
O1—Co1—N1—C1	123.2 (3)	C3—C4—C5—N1	−1.0 (4)
O2—Co1—N1—C1	−12.5 (2)	C11—C4—C5—N1	178.9 (2)
N2—Co1—N1—C1	176.0 (2)	C3—C4—C5—C6	178.7 (2)
O5—Co1—N1—C1	71.7 (2)	C11—C4—C5—C6	−1.5 (4)
O6—Co1—N1—C5	84.93 (18)	C10—N2—C6—C7	2.5 (4)
O1—Co1—N1—C5	−51.5 (3)	Co1—N2—C6—C7	178.45 (18)
O2—Co1—N1—C5	172.86 (17)	C10—N2—C6—C5	−177.7 (2)
N2—Co1—N1—C5	1.34 (17)	Co1—N2—C6—C5	−1.7 (3)
O5—Co1—N1—C5	−102.94 (18)	N1—C5—C6—N2	3.0 (3)
O6—Co1—N2—C10	75.6 (2)	C4—C5—C6—N2	−176.7 (2)
O1—Co1—N2—C10	−17.2 (2)	N1—C5—C6—C7	−177.2 (2)
O2—Co1—N2—C10	129.8 (3)	C4—C5—C6—C7	3.1 (4)
N1—Co1—N2—C10	175.8 (2)	N2—C6—C7—C8	−2.2 (4)
O5—Co1—N2—C10	−104.8 (2)	C5—C6—C7—C8	178.0 (2)
O6—Co1—N2—C6	−99.96 (17)	N2—C6—C7—C12	177.3 (2)
O1—Co1—N2—C6	167.22 (17)	C5—C6—C7—C12	−2.5 (3)
O2—Co1—N2—C6	−45.8 (4)	C6—C7—C8—C9	0.0 (4)
N1—Co1—N2—C6	0.26 (16)	C12—C7—C8—C9	−179.4 (3)
O5—Co1—N2—C6	79.66 (17)	C7—C8—C9—C10	1.7 (4)
O6—Co1—O1—S1	117.94 (15)	C6—N2—C10—C9	−0.6 (4)
O2—Co1—O1—S1	30.25 (15)	Co1—N2—C10—C9	−176.0 (2)
N1—Co1—O1—S1	−105.0 (3)	C8—C9—C10—N2	−1.5 (4)
N2—Co1—O1—S1	−156.20 (15)	C13—N3—C11—C12	−0.4 (3)
O5—Co1—O1—S1	−54.11 (15)	C13—N3—C11—C4	178.7 (3)
O6—Co1—O2—S1i	−21.15 (18)	C3—C4—C11—C12	179.2 (3)
O1—Co1—O2—S1i	71.49 (18)	C5—C4—C11—C12	−0.7 (4)
N1—Co1—O2—S1i	−120.03 (18)	C3—C4—C11—N3	0.2 (5)
N2—Co1—O2—S1i	−75.2 (4)	C5—C4—C11—N3	−179.7 (2)
O5—Co1—O2—S1i	157.89 (18)	N3—C11—C12—N4	0.4 (3)
Co1—O1—S1—O2i	−80.84 (16)	C4—C11—C12—N4	−178.8 (2)
Co1—O1—S1—O4	159.15 (14)	N3—C11—C12—C7	−179.6 (2)
Co1—O1—S1—O3	40.34 (17)	C4—C11—C12—C7	1.2 (4)
C5—N1—C1—C2	−1.1 (4)	C13—N4—C12—C11	−0.2 (3)
Co1—N1—C1—C2	−175.59 (19)	C13—N4—C12—C7	179.7 (3)
N1—C1—C2—C3	−0.5 (4)	C8—C7—C12—C11	179.9 (2)
C1—C2—C3—C4	1.4 (4)	C6—C7—C12—C11	0.4 (4)
C2—C3—C4—C5	−0.7 (4)	C8—C7—C12—N4	−0.1 (4)
C2—C3—C4—C11	179.5 (3)	C6—C7—C12—N4	−179.5 (2)
C1—N1—C5—C4	1.8 (4)	C12—N4—C13—N3	0.0 (3)
Co1—N1—C5—C4	176.97 (18)	C11—N3—C13—N4	0.3 (3)
C1—N1—C5—C6	−177.8 (2)

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3···O4ii	0.86	2.05	2.886 (3)	165
N3—H3···S1ii	0.86	2.94	3.709 (2)	150
O5—H5A···O3	0.85	1.94	2.764 (2)	165
O5—H5A···S1	0.85	2.77	3.4184 (19)	134
O6—H6B···O7iii	0.85	1.79	2.634 (3)	174
O7—H7B···O3iv	0.85	2.00	2.843 (3)	176
O7—H7B···S1iv	0.85	2.93	3.703 (3)	152

Table 1

Selected bond lengths (Å)

Co1—N1	2.124 (2)
Co1—N2	2.137 (2)
Co1—O6	2.0654 (19)
Co1—O1	2.0889 (17)
Co1—O2	2.0978 (17)
Co1—O5	2.1468 (18)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H3⋯O4i	0.86	2.05	2.886 (3)	165
O5—H5A⋯O3	0.85	1.94	2.764 (2)	165
O6—H6B⋯O7ii	0.85	1.79	2.634 (3)	174
O7—H7B⋯O3iii	0.85	2.00	2.843 (3)	176

Symmetry codes: (i) ; (ii) ; (iii) .