Hexaaqua-cobalt(II) tetra-aqua-bis(2-amino-pyrazine-κN)cobalt(II) disulfate dihydrate.

The reaction of cobalt(II) sulfate and 2-amino-pyrazine affords the title salt, [Co(H(2)O)(6)][Co(C(4)H(5)N(3))(2)(H(2)O)(4)](SO(4))(2)·2H(2)O. The metal atoms in the tetra-aqua-coordinated and hexa-aqua-coordinated complex cations lie on centers of inversion in slightly distorted octa-hedral geometries. The cations, anions and solvent water mol-ecules are linked by O-H⋯O, O-H⋯N and N-H⋯O hydrogen bonds into a three-dimensional network.

Related literature

The reaction of cobalt(II) chloride and 3-amino­pyrazine yields tetra­kis(3-amino­pyrazine)dichloridocobalt(II); see: Csöregh et al. (2000 ▶); Kang et al. (2009 ▶).

Experimental

Crystal data

[Co(H2O)6][Co(C4H5N3)2(H2O)4](SO4)2·2H2O

M = 716.40

Triclinic,

a = 6.5722 (3) Å

b = 8.3264 (4) Å

c = 13.2337 (7) Å

α = 75.732 (2)°

β = 78.571 (1)°

γ = 78.795 (1)°

V = 679.81 (6) Å3

Z = 1

Mo Kα radiation

μ = 1.47 mm−1

T = 293 K

0.30 × 0.20 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.668, T max = 0.758

6692 measured reflections

3071 independent reflections

2762 reflections with I > 2σ(I)

R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.031

wR(F 2) = 0.085

S = 1.05

3071 reflections

231 parameters

14 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.47 e Å−3

Δρmin = −0.33 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2009 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809045310/xu2657sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045310/xu2657Isup2.hkl

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

[Co(H2O)6][Co(C4H5N3)2(H2O)4](SO4)2·2H2O	Z = 1
Mr = 716.40	F(000) = 370
Triclinic, P1	Dx = 1.750 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.5722 (3) Å	Cell parameters from 6326 reflections
b = 8.3264 (4) Å	θ = 3.2–27.5°
c = 13.2337 (7) Å	µ = 1.47 mm−1
α = 75.732 (2)°	T = 293 K
β = 78.571 (1)°	Prism, red
γ = 78.795 (1)°	0.30 × 0.20 × 0.20 mm
V = 679.81 (6) Å3

Rigaku RAXIS-RAPID IP diffractometer	3071 independent reflections
Radiation source: fine-focus sealed tube	2762 reflections with I > 2σ(I)
graphite	Rint = 0.027
ω scans	θmax = 27.4°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −7→8
Tmin = 0.668, Tmax = 0.758	k = −10→10
6692 measured reflections	l = −17→17

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ2(Fo2) + (0.0511P)2 + 0.1887P] where P = (Fo2 + 2Fc2)/3
3071 reflections	(Δ/σ)max = 0.001
231 parameters	Δρmax = 0.47 e Å−3
14 restraints	Δρmin = −0.33 e Å−3

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.

	x	y	z	Uiso*/Ueq
Co1	1.0000	1.0000	0.5000	0.02058 (10)
Co2	0.0000	0.5000	1.0000	0.02713 (11)
S1	0.48109 (7)	0.88842 (5)	0.80066 (3)	0.02386 (12)
O1	0.4133 (2)	0.98162 (18)	0.70001 (10)	0.0309 (3)
O2	0.5369 (3)	0.70948 (18)	0.79992 (14)	0.0439 (4)
O3	0.6685 (2)	0.95119 (18)	0.81446 (11)	0.0317 (3)
O4	0.3094 (2)	0.9161 (2)	0.88747 (12)	0.0410 (4)
O1W	0.7178 (2)	0.91396 (17)	0.53377 (11)	0.0295 (3)
O2W	1.0213 (2)	0.96509 (18)	0.66021 (11)	0.0305 (3)
O3W	0.2836 (2)	0.4730 (2)	0.90039 (14)	0.0435 (4)
O4W	−0.1433 (3)	0.4747 (2)	0.87641 (13)	0.0399 (4)
O5W	0.0399 (2)	0.23895 (19)	1.05544 (14)	0.0421 (4)
O6W	0.6169 (3)	0.2195 (2)	0.91230 (13)	0.0397 (3)
N1	0.8413 (2)	1.25974 (19)	0.49825 (13)	0.0257 (3)
N2	0.7121 (3)	1.6016 (2)	0.49242 (14)	0.0302 (3)
N3	0.7876 (3)	1.6554 (2)	0.30956 (16)	0.0423 (4)
C1	0.8491 (3)	1.3722 (2)	0.40789 (15)	0.0289 (4)
H1	0.9012	1.3361	0.3452	0.035*
C2	0.7812 (3)	1.5450 (2)	0.40335 (16)	0.0283 (4)
C3	0.7021 (3)	1.4852 (3)	0.58309 (16)	0.0317 (4)
H3	0.6516	1.5207	0.6461	0.038*
C4	0.7624 (3)	1.3170 (2)	0.58746 (15)	0.0306 (4)
H4	0.7489	1.2415	0.6523	0.037*
H1W1	0.615 (3)	0.941 (3)	0.5778 (16)	0.039 (7)*
H1W2	0.708 (4)	0.822 (2)	0.521 (2)	0.043 (7)*
H2W1	0.924 (3)	0.961 (3)	0.7118 (14)	0.038 (7)*
H2W2	1.136 (3)	0.983 (4)	0.671 (2)	0.058 (9)*
H3W1	0.348 (5)	0.556 (3)	0.872 (3)	0.072 (10)*
H3W2	0.376 (3)	0.387 (2)	0.906 (2)	0.050 (8)*
H4W1	−0.199 (5)	0.387 (3)	0.886 (3)	0.068 (10)*
H4W2	−0.234 (3)	0.558 (2)	0.856 (2)	0.043 (7)*
H5W1	0.135 (3)	0.176 (3)	1.0881 (19)	0.046 (8)*
H5W2	−0.062 (4)	0.185 (4)	1.076 (2)	0.066 (9)*
H6W1	0.637 (6)	0.145 (4)	0.876 (3)	0.094 (13)*
H6W2	0.625 (5)	0.164 (4)	0.9747 (12)	0.065 (10)*
H3N1	0.830 (5)	1.618 (4)	0.2538 (15)	0.062 (9)*
H3N2	0.751 (5)	1.7602 (15)	0.307 (3)	0.064 (9)*

	U11	U22	U33	U12	U13	U23
Co1	0.02009 (17)	0.01865 (17)	0.02239 (18)	−0.00235 (12)	−0.00307 (13)	−0.00400 (12)
Co2	0.02194 (19)	0.02479 (19)	0.0323 (2)	−0.00440 (14)	−0.00566 (14)	0.00002 (14)
S1	0.0220 (2)	0.0245 (2)	0.0240 (2)	−0.00519 (17)	−0.00492 (16)	−0.00072 (16)
O1	0.0285 (7)	0.0353 (7)	0.0270 (7)	−0.0006 (6)	−0.0095 (5)	−0.0022 (5)
O2	0.0429 (9)	0.0237 (7)	0.0623 (10)	−0.0039 (6)	−0.0138 (8)	−0.0005 (7)
O3	0.0241 (6)	0.0394 (8)	0.0336 (7)	−0.0094 (6)	−0.0057 (5)	−0.0074 (6)
O4	0.0292 (7)	0.0610 (10)	0.0311 (7)	−0.0127 (7)	0.0028 (6)	−0.0080 (7)
O1W	0.0249 (7)	0.0264 (7)	0.0383 (8)	−0.0067 (5)	0.0030 (6)	−0.0134 (6)
O2W	0.0266 (7)	0.0413 (8)	0.0242 (7)	−0.0062 (6)	−0.0044 (5)	−0.0069 (6)
O3W	0.0280 (8)	0.0322 (8)	0.0594 (10)	−0.0041 (6)	0.0049 (7)	0.0007 (7)
O4W	0.0383 (8)	0.0344 (8)	0.0493 (9)	−0.0060 (7)	−0.0199 (7)	−0.0029 (7)
O5W	0.0314 (8)	0.0290 (8)	0.0618 (10)	−0.0075 (6)	−0.0170 (7)	0.0077 (7)
O6W	0.0501 (9)	0.0321 (8)	0.0387 (9)	−0.0050 (7)	−0.0107 (7)	−0.0089 (7)
N1	0.0231 (7)	0.0206 (7)	0.0326 (8)	−0.0019 (6)	−0.0050 (6)	−0.0053 (6)
N2	0.0271 (8)	0.0234 (8)	0.0425 (9)	−0.0026 (6)	−0.0079 (7)	−0.0104 (7)
N3	0.0564 (12)	0.0247 (9)	0.0399 (11)	0.0015 (8)	−0.0053 (9)	−0.0040 (8)
C1	0.0305 (9)	0.0241 (9)	0.0318 (10)	−0.0029 (7)	−0.0039 (8)	−0.0072 (7)
C2	0.0244 (9)	0.0224 (9)	0.0378 (10)	−0.0034 (7)	−0.0059 (7)	−0.0052 (7)
C3	0.0290 (9)	0.0318 (10)	0.0361 (10)	0.0005 (8)	−0.0061 (8)	−0.0138 (8)
C4	0.0305 (10)	0.0296 (10)	0.0294 (9)	−0.0018 (8)	−0.0040 (8)	−0.0052 (7)

Co1—O1W	2.0451 (13)	O3W—H3W1	0.846 (10)
Co1—O1Wi	2.0451 (13)	O3W—H3W2	0.846 (10)
Co1—O2Wi	2.0970 (13)	O4W—H4W1	0.847 (10)
Co1—O2W	2.0970 (13)	O4W—H4W2	0.850 (10)
Co1—N1i	2.2076 (15)	O5W—H5W1	0.849 (10)
Co1—N1	2.2076 (15)	O5W—H5W2	0.840 (10)
Co2—O3W	2.0670 (16)	O6W—H6W1	0.849 (10)
Co2—O3Wii	2.0670 (16)	O6W—H6W2	0.847 (10)
Co2—O5W	2.0977 (15)	N1—C1	1.324 (2)
Co2—O5Wii	2.0977 (15)	N1—C4	1.352 (3)
Co2—O4W	2.1128 (16)	N2—C2	1.340 (3)
Co2—O4Wii	2.1128 (16)	N2—C3	1.343 (3)
S1—O2	1.4656 (16)	N3—C2	1.349 (3)
S1—O4	1.4703 (15)	N3—H3N1	0.849 (10)
S1—O1	1.4717 (13)	N3—H3N2	0.852 (10)
S1—O3	1.4866 (14)	C1—C2	1.411 (3)
O1W—H1W1	0.836 (10)	C1—H1	0.9300
O1W—H1W2	0.846 (10)	C3—C4	1.370 (3)
O2W—H2W1	0.838 (10)	C3—H3	0.9300
O2W—H2W2	0.843 (10)	C4—H4	0.9300
O1W—Co1—O1Wi	180.0	Co1—O1W—H1W1	126.4 (17)
O1W—Co1—O2Wi	87.43 (6)	Co1—O1W—H1W2	120.7 (18)
O1Wi—Co1—O2Wi	92.57 (6)	H1W1—O1W—H1W2	110 (2)
O1W—Co1—O2W	92.57 (6)	Co1—O2W—H2W1	128.2 (18)
O1Wi—Co1—O2W	87.43 (6)	Co1—O2W—H2W2	114 (2)
O2Wi—Co1—O2W	180.000 (1)	H2W1—O2W—H2W2	116 (3)
O1W—Co1—N1i	88.71 (6)	Co2—O3W—H3W1	121 (2)
O1Wi—Co1—N1i	91.29 (6)	Co2—O3W—H3W2	125.2 (19)
O2Wi—Co1—N1i	90.16 (6)	H3W1—O3W—H3W2	107 (3)
O2W—Co1—N1i	89.84 (6)	Co2—O4W—H4W1	117 (2)
O1W—Co1—N1	91.29 (6)	Co2—O4W—H4W2	114.2 (18)
O1Wi—Co1—N1	88.71 (6)	H4W1—O4W—H4W2	107 (3)
O2Wi—Co1—N1	89.84 (6)	Co2—O5W—H5W1	128.5 (19)
O2W—Co1—N1	90.16 (6)	Co2—O5W—H5W2	122 (2)
N1i—Co1—N1	180.000 (1)	H5W1—O5W—H5W2	103 (3)
O3W—Co2—O3Wii	180.0	H6W1—O6W—H6W2	104 (3)
O3W—Co2—O5W	88.95 (7)	C1—N1—C4	117.08 (16)
O3Wii—Co2—O5W	91.05 (7)	C1—N1—Co1	119.42 (13)
O3W—Co2—O5Wii	91.05 (7)	C4—N1—Co1	122.75 (13)
O3Wii—Co2—O5Wii	88.95 (7)	C2—N2—C3	116.49 (17)
O5W—Co2—O5Wii	180.0	C2—N3—H3N1	118 (2)
O3W—Co2—O4W	87.20 (7)	C2—N3—H3N2	121 (2)
O3Wii—Co2—O4W	92.80 (7)	H3N1—N3—H3N2	121 (3)
O5W—Co2—O4W	89.82 (7)	N1—C1—C2	122.25 (18)
O5Wii—Co2—O4W	90.18 (7)	N1—C1—H1	118.9
O3W—Co2—O4Wii	92.80 (7)	C2—C1—H1	118.9
O3Wii—Co2—O4Wii	87.20 (7)	N2—C2—N3	119.21 (18)
O5W—Co2—O4Wii	90.18 (7)	N2—C2—C1	120.28 (18)
O5Wii—Co2—O4Wii	89.82 (7)	N3—C2—C1	120.50 (19)
O4W—Co2—O4Wii	180.0	N2—C3—C4	123.26 (19)
O2—S1—O4	110.72 (10)	N2—C3—H3	118.4
O2—S1—O1	109.81 (9)	C4—C3—H3	118.4
O4—S1—O1	108.83 (9)	N1—C4—C3	120.53 (18)
O2—S1—O3	108.89 (9)	N1—C4—H4	119.7
O4—S1—O3	109.26 (9)	C3—C4—H4	119.7
O1—S1—O3	109.31 (8)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O1	0.84 (1)	1.93 (1)	2.755 (2)	168 (3)
O1w—H1w2···N2iii	0.85 (1)	1.95 (1)	2.795 (2)	175 (3)
O2w—H2w1···O3	0.84 (1)	1.94 (1)	2.769 (2)	170 (2)
O2w—H2w2···O1iv	0.84 (1)	1.93 (1)	2.765 (2)	170 (3)
O3w—H3w1···O2	0.85 (1)	1.91 (1)	2.743 (2)	169 (3)
O3w—H3w2···O6w	0.85 (1)	1.89 (1)	2.730 (2)	170 (3)
O4w—H4w1···O6wv	0.85 (1)	1.95 (1)	2.781 (2)	168 (3)
O4w—H4w2···O2v	0.85 (1)	1.91 (1)	2.745 (2)	167 (2)
O5w—H5w1···O3vi	0.85 (1)	1.98 (1)	2.816 (2)	170 (3)
O5w—H5w2···O4ii	0.84 (1)	1.90 (1)	2.737 (2)	174 (3)
O6w—H6w1···O3iii	0.85 (1)	1.94 (1)	2.782 (2)	171 (4)
O6w—H6w2···O4vi	0.85 (1)	1.89 (1)	2.711 (2)	164 (3)
N3—H3n2···O1vii	0.85 (1)	2.20 (1)	3.036 (2)	168 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H1w1⋯O1	0.84 (1)	1.93 (1)	2.755 (2)	168 (3)
O1w—H1w2⋯N2i	0.85 (1)	1.95 (1)	2.795 (2)	175 (3)
O2w—H2w1⋯O3	0.84 (1)	1.94 (1)	2.769 (2)	170 (2)
O2w—H2w2⋯O1ii	0.84 (1)	1.93 (1)	2.765 (2)	170 (3)
O3w—H3w1⋯O2	0.85 (1)	1.91 (1)	2.743 (2)	169 (3)
O3w—H3w2⋯O6w	0.85 (1)	1.89 (1)	2.730 (2)	170 (3)
O4w—H4w1⋯O6wiii	0.85 (1)	1.95 (1)	2.781 (2)	168 (3)
O4w—H4w2⋯O2iii	0.85 (1)	1.91 (1)	2.745 (2)	167 (2)
O5w—H5w1⋯O3iv	0.85 (1)	1.98 (1)	2.816 (2)	170 (3)
O5w—H5w2⋯O4v	0.84 (1)	1.90 (1)	2.737 (2)	174 (3)
O6w—H6w1⋯O3i	0.85 (1)	1.94 (1)	2.782 (2)	171 (4)
O6w—H6w2⋯O4iv	0.85 (1)	1.89 (1)	2.711 (2)	164 (3)
N3—H3n2⋯O1vi	0.85 (1)	2.20 (1)	3.036 (2)	168 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .