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

The reaction of manganese(II) sulfate and 2-amino-pyrazine affords the title salt, [Mn(H(2)O)(6)][Mn(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 cations lie on centers of inversion in octa-hedral geometries. The cations, anions and solvent water mol-ecules are linked by O-H⋯O, N-H⋯O and O-H⋯N hydrogen bonds into a three-dimensional network.

Related literature

For the isostructural cobalt(II) analog, see: Kang et al. (2009 ▶).

Experimental

Crystal data

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

M = 708.43

Triclinic,

a = 6.6242 (3) Å

b = 8.4639 (4) Å

c = 13.2719 (8) Å

α = 75.654 (2)°

β = 78.364 (2)°

γ = 78.834 (2)°

V = 697.95 (6) Å3

Z = 1

Mo Kα radiation

μ = 1.14 mm−1

T = 293 K

0.38 × 0.20 × 0.18 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.670, T max = 0.821

6866 measured reflections

3159 independent reflections

2874 reflections with I > 2σ(I)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.041

wR(F 2) = 0.129

S = 1.15

3159 reflections

231 parameters

14 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.74 e Å−3

Δρmin = −0.40 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/S1600536809045322/xu2658sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045322/xu2658Isup2.hkl

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

[Mn(H2O)6][Mn(C4H5N3)2(H2O)4](SO4)2·2H2O	Z = 1
Mr = 708.43	F(000) = 366
Triclinic, P1	Dx = 1.685 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.6242 (3) Å	Cell parameters from 6492 reflections
b = 8.4639 (4) Å	θ = 3.2–27.5°
c = 13.2719 (8) Å	µ = 1.14 mm−1
α = 75.654 (2)°	T = 293 K
β = 78.364 (2)°	Prism, colorless
γ = 78.834 (2)°	0.38 × 0.20 × 0.18 mm
V = 697.95 (6) Å3

Rigaku R-AXIS RAPID IP diffractometer	3159 independent reflections
Radiation source: fine-focus sealed tube	2874 reflections with I > 2σ(I)
graphite	Rint = 0.025
ω scans	θmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −8→8
Tmin = 0.670, Tmax = 0.821	k = −10→10
6866 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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129	H atoms treated by a mixture of independent and constrained refinement
S = 1.15	w = 1/[σ2(Fo2) + (0.0556P)2 + 1.1503P] where P = (Fo2 + 2Fc2)/3
3159 reflections	(Δ/σ)max = 0.001
231 parameters	Δρmax = 0.74 e Å−3
14 restraints	Δρmin = −0.40 e Å−3

	x	y	z	Uiso*/Ueq
Mn1	1.0000	1.0000	0.5000	0.02349 (17)
Mn2	0.0000	0.5000	1.0000	0.02867 (18)
S1	0.47994 (10)	0.88750 (9)	0.80279 (5)	0.02457 (18)
O1	0.4091 (3)	0.9828 (3)	0.70435 (17)	0.0322 (5)
O2	0.5386 (4)	0.7129 (3)	0.7978 (2)	0.0444 (6)
O3	0.6644 (3)	0.9501 (3)	0.81657 (17)	0.0318 (5)
O4	0.3121 (4)	0.9084 (4)	0.89137 (19)	0.0441 (6)
O1W	0.7084 (4)	0.9110 (3)	0.53580 (19)	0.0335 (5)
O2W	1.0209 (4)	0.9617 (3)	0.66525 (17)	0.0345 (5)
O3W	0.2937 (4)	0.4732 (3)	0.8939 (2)	0.0471 (7)
O4W	−0.1480 (4)	0.4748 (3)	0.8707 (2)	0.0429 (6)
O5W	0.0400 (4)	0.2353 (3)	1.0577 (2)	0.0456 (6)
O6W	0.6189 (4)	0.2200 (3)	0.9081 (2)	0.0399 (6)
N1	0.8363 (4)	1.2689 (3)	0.4980 (2)	0.0301 (5)
N2	0.7098 (4)	1.6040 (3)	0.4930 (2)	0.0344 (6)
N3	0.7810 (6)	1.6587 (4)	0.3104 (3)	0.0482 (8)
C1	0.8414 (5)	1.3800 (4)	0.4078 (3)	0.0334 (7)
H1	0.8899	1.3447	0.3450	0.040*
C2	0.7760 (5)	1.5496 (4)	0.4039 (3)	0.0325 (6)
C3	0.7019 (5)	1.4892 (4)	0.5836 (3)	0.0376 (7)
H3	0.6532	1.5237	0.6466	0.045*
C4	0.7623 (5)	1.3238 (4)	0.5874 (3)	0.0348 (7)
H4	0.7522	1.2491	0.6521	0.042*
H1W1	0.614 (5)	0.948 (5)	0.581 (3)	0.048 (12)*
H1W2	0.715 (7)	0.817 (3)	0.521 (4)	0.053 (13)*
H2W1	0.919 (4)	0.972 (5)	0.714 (2)	0.028 (9)*
H2W2	1.135 (4)	0.967 (5)	0.683 (3)	0.044 (11)*
H3W1	0.357 (7)	0.556 (4)	0.866 (4)	0.066 (15)*
H3W2	0.391 (5)	0.392 (3)	0.901 (3)	0.039 (11)*
H4W1	−0.195 (8)	0.386 (4)	0.876 (4)	0.073 (17)*
H4W2	−0.247 (5)	0.554 (4)	0.859 (4)	0.063 (15)*
H5W1	0.126 (6)	0.160 (4)	1.089 (3)	0.059 (14)*
H5W2	−0.072 (5)	0.194 (7)	1.074 (5)	0.081 (18)*
H6W1	0.624 (9)	0.148 (5)	0.873 (4)	0.079 (18)*
H6W2	0.641 (9)	0.170 (6)	0.9698 (19)	0.072 (17)*
H3N1	0.831 (7)	1.629 (6)	0.252 (2)	0.062 (15)*
H3N2	0.738 (8)	1.7613 (19)	0.308 (4)	0.060 (14)*

	U11	U22	U33	U12	U13	U23
Mn1	0.0217 (3)	0.0225 (3)	0.0255 (3)	−0.0022 (2)	−0.0054 (2)	−0.0034 (2)
Mn2	0.0218 (3)	0.0271 (3)	0.0341 (3)	−0.0032 (2)	−0.0067 (2)	0.0002 (2)
S1	0.0209 (3)	0.0257 (3)	0.0260 (3)	−0.0046 (3)	−0.0066 (2)	−0.0004 (3)
O1	0.0289 (11)	0.0353 (12)	0.0302 (11)	−0.0007 (9)	−0.0115 (9)	−0.0009 (9)
O2	0.0423 (14)	0.0252 (11)	0.0645 (17)	−0.0035 (10)	−0.0175 (12)	−0.0014 (11)
O3	0.0224 (10)	0.0385 (12)	0.0356 (11)	−0.0062 (9)	−0.0079 (8)	−0.0062 (9)
O4	0.0313 (12)	0.0672 (17)	0.0317 (12)	−0.0132 (12)	0.0012 (10)	−0.0078 (11)
O1W	0.0277 (11)	0.0325 (12)	0.0423 (13)	−0.0092 (9)	0.0038 (9)	−0.0157 (10)
O2W	0.0258 (11)	0.0521 (14)	0.0264 (10)	−0.0058 (10)	−0.0080 (9)	−0.0068 (10)
O3W	0.0281 (12)	0.0356 (14)	0.0671 (18)	−0.0064 (11)	0.0055 (12)	−0.0012 (12)
O4W	0.0395 (14)	0.0380 (14)	0.0542 (15)	−0.0039 (11)	−0.0212 (12)	−0.0059 (12)
O5W	0.0318 (13)	0.0320 (12)	0.0679 (17)	−0.0074 (10)	−0.0194 (12)	0.0096 (12)
O6W	0.0477 (14)	0.0317 (12)	0.0413 (14)	−0.0016 (11)	−0.0131 (11)	−0.0086 (10)
N1	0.0269 (12)	0.0226 (12)	0.0390 (14)	−0.0011 (10)	−0.0063 (10)	−0.0044 (10)
N2	0.0293 (13)	0.0255 (12)	0.0498 (16)	−0.0013 (10)	−0.0095 (12)	−0.0109 (11)
N3	0.063 (2)	0.0285 (15)	0.0451 (18)	0.0031 (15)	−0.0061 (16)	−0.0039 (13)
C1	0.0347 (16)	0.0256 (15)	0.0380 (16)	0.0001 (12)	−0.0061 (13)	−0.0069 (12)
C2	0.0289 (15)	0.0238 (14)	0.0435 (17)	−0.0014 (12)	−0.0071 (13)	−0.0060 (12)
C3	0.0337 (16)	0.0391 (18)	0.0425 (18)	0.0019 (14)	−0.0073 (14)	−0.0182 (14)
C4	0.0318 (16)	0.0335 (16)	0.0352 (16)	0.0037 (13)	−0.0075 (13)	−0.0051 (13)

Mn1—O1W	2.131 (2)	O3W—H3W1	0.849 (10)
Mn1—O1Wi	2.131 (2)	O3W—H3W2	0.849 (10)
Mn1—O2Wi	2.165 (2)	O4W—H4W1	0.848 (10)
Mn1—O2W	2.165 (2)	O4W—H4W2	0.850 (10)
Mn1—N1	2.320 (2)	O5W—H5W1	0.849 (10)
Mn1—N1i	2.320 (2)	O5W—H5W2	0.850 (10)
Mn2—O3W	2.168 (3)	O6W—H6W1	0.850 (10)
Mn2—O3Wii	2.168 (3)	O6W—H6W2	0.850 (10)
Mn2—O4W	2.212 (3)	N1—C1	1.325 (4)
Mn2—O4Wii	2.212 (3)	N1—C4	1.347 (4)
Mn2—O5Wii	2.163 (2)	N2—C2	1.337 (4)
Mn2—O5W	2.163 (2)	N2—C3	1.344 (5)
S1—O4	1.466 (2)	N3—C2	1.350 (5)
S1—O2	1.468 (3)	N3—H3N1	0.855 (10)
S1—O1	1.468 (2)	N3—H3N2	0.854 (10)
S1—O3	1.482 (2)	C1—C2	1.408 (4)
O1W—H1W1	0.844 (10)	C1—H1	0.9300
O1W—H1W2	0.851 (10)	C3—C4	1.371 (5)
O2W—H2W1	0.846 (10)	C3—H3	0.9300
O2W—H2W2	0.852 (10)	C4—H4	0.9300
O1W—Mn1—O1Wi	180.000 (1)	Mn1—O1W—H1W1	118 (3)
O1W—Mn1—O2Wi	87.90 (9)	Mn1—O1W—H1W2	114 (3)
O1Wi—Mn1—O2Wi	92.10 (9)	H1W1—O1W—H1W2	123 (4)
O1W—Mn1—O2W	92.10 (9)	Mn1—O2W—H2W1	125 (3)
O1Wi—Mn1—O2W	87.90 (9)	Mn1—O2W—H2W2	120 (3)
O2Wi—Mn1—O2W	180.000 (1)	H2W1—O2W—H2W2	112 (4)
O1W—Mn1—N1	91.71 (9)	Mn2—O3W—H3W1	120 (4)
O1Wi—Mn1—N1	88.29 (9)	Mn2—O3W—H3W2	126 (3)
O2Wi—Mn1—N1	89.32 (10)	H3W1—O3W—H3W2	104 (4)
O2W—Mn1—N1	90.68 (10)	Mn2—O4W—H4W1	119 (4)
O1W—Mn1—N1i	88.29 (9)	Mn2—O4W—H4W2	110 (3)
O1Wi—Mn1—N1i	91.71 (9)	H4W1—O4W—H4W2	107 (5)
O2Wi—Mn1—N1i	90.68 (10)	Mn2—O5W—H5W1	139 (3)
O2W—Mn1—N1i	89.32 (10)	Mn2—O5W—H5W2	115 (4)
N1—Mn1—N1i	180.000 (1)	H5W1—O5W—H5W2	103 (5)
O5Wii—Mn2—O5W	180.000 (1)	H6W1—O6W—H6W2	108 (5)
O5Wii—Mn2—O3W	90.64 (10)	C1—N1—C4	117.4 (3)
O5W—Mn2—O3W	89.36 (10)	C1—N1—Mn1	119.9 (2)
O5Wii—Mn2—O3Wii	89.36 (10)	C4—N1—Mn1	121.9 (2)
O5W—Mn2—O3Wii	90.64 (10)	C2—N2—C3	116.8 (3)
O3W—Mn2—O3Wii	180.000 (1)	C2—N3—H3N1	122 (3)
O5Wii—Mn2—O4W	89.84 (10)	C2—N3—H3N2	121 (3)
O5W—Mn2—O4W	90.16 (10)	H3N1—N3—H3N2	117 (5)
O3W—Mn2—O4W	86.45 (11)	N1—C1—C2	122.2 (3)
O3Wii—Mn2—O4W	93.55 (11)	N1—C1—H1	118.9
O5Wii—Mn2—O4Wii	90.16 (10)	C2—C1—H1	118.9
O5W—Mn2—O4Wii	89.84 (10)	N2—C2—N3	119.4 (3)
O3W—Mn2—O4Wii	93.55 (11)	N2—C2—C1	120.2 (3)
O3Wii—Mn2—O4Wii	86.45 (11)	N3—C2—C1	120.4 (3)
O4W—Mn2—O4Wii	180.000 (1)	N2—C3—C4	123.1 (3)
O4—S1—O2	110.85 (17)	N2—C3—H3	118.4
O4—S1—O1	109.03 (14)	C4—C3—H3	118.4
O2—S1—O1	109.60 (15)	N1—C4—C3	120.3 (3)
O4—S1—O3	109.10 (14)	N1—C4—H4	119.9
O2—S1—O3	109.02 (14)	C3—C4—H4	119.9
O1—S1—O3	109.22 (13)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O1	0.84 (1)	1.95 (2)	2.779 (3)	167 (4)
O1w—H1w2···N2iii	0.85 (1)	1.94 (1)	2.792 (3)	176 (5)
O2w—H2w1···O3	0.85 (1)	1.95 (1)	2.775 (3)	166 (4)
O2w—H2w2···O1iv	0.85 (1)	1.92 (1)	2.770 (3)	172 (4)
O3w—H3w1···O2	0.85 (1)	1.90 (1)	2.744 (4)	170 (5)
O3w—H3w2···O6w	0.85 (1)	1.88 (1)	2.728 (4)	175 (4)
O4w—H4w1···O6wv	0.85 (1)	1.96 (2)	2.780 (4)	162 (5)
O4w—H4w2···O2v	0.85 (1)	1.92 (2)	2.744 (4)	164 (5)
O5w—H5w1···O3vi	0.84 (1)	2.00 (2)	2.813 (3)	159 (5)
O5w—H5w2···O4ii	0.85 (1)	1.88 (1)	2.726 (4)	177 (6)
O6w—H6w1···O3iii	0.85 (1)	1.95 (2)	2.783 (3)	167 (6)
O6w—H6w2···O4vi	0.85 (1)	1.87 (1)	2.709 (4)	172 (6)
N3—H3n2···O1vii	0.85 (1)	2.18 (1)	3.026 (4)	172 (5)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H1w1⋯O1	0.84 (1)	1.95 (2)	2.779 (3)	167 (4)
O1w—H1w2⋯N2i	0.85 (1)	1.94 (1)	2.792 (3)	176 (5)
O2w—H2w1⋯O3	0.85 (1)	1.95 (1)	2.775 (3)	166 (4)
O2w—H2w2⋯O1ii	0.85 (1)	1.92 (1)	2.770 (3)	172 (4)
O3w—H3w1⋯O2	0.85 (1)	1.90 (1)	2.744 (4)	170 (5)
O3w—H3w2⋯O6w	0.85 (1)	1.88 (1)	2.728 (4)	175 (4)
O4w—H4w1⋯O6wiii	0.85 (1)	1.96 (2)	2.780 (4)	162 (5)
O4w—H4w2⋯O2iii	0.85 (1)	1.92 (2)	2.744 (4)	164 (5)
O5w—H5w1⋯O3iv	0.84 (1)	2.00 (2)	2.813 (3)	159 (5)
O5w—H5w2⋯O4v	0.85 (1)	1.88 (1)	2.726 (4)	177 (6)
O6w—H6w1⋯O3i	0.85 (1)	1.95 (2)	2.783 (3)	167 (6)
O6w—H6w2⋯O4iv	0.85 (1)	1.87 (1)	2.709 (4)	172 (6)
N3—H3n2⋯O1vi	0.85 (1)	2.18 (1)	3.026 (4)	172 (5)

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