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Hexa­aqua­manganese(II) tetra­aqua­bis­(2-amino­pyrazine-κN4)manganese(II) di­sulfate dihydrate

aCollege of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, People's Republic of China, and bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 27 October 2009; accepted 29 October 2009; online 4 November 2009)

The reaction of manganese(II) sulfate and 2-amino­pyrazine affords the title salt, [Mn(H2O)6][Mn(C4H5N3)2(H2O)4](SO4)2·2H2O. The metal atoms in the tetra­aqua-coordinated and hexa­aqua-coordinated cations lie on centers of inversion in octa­hedral geometries. The cations, anions and solvent water mol­ecules 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[Kang, W., Huo, L.-H., Gao, S. & Ng, S. W. (2009). Acta Cryst. E65, m1503.]).

[Scheme 1]

Experimental

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

  • Mr = 708.43

  • Triclinic, [P \overline 1]

  • 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[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.670, Tmax = 0.821

  • 6866 measured reflections

  • 3159 independent reflections

  • 2874 reflections with I > 2σ(I)

  • Rint = 0.025

Refinement
  • R[F2 > 2σ(F2)] = 0.041

  • wR(F2) = 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

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA 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) x, y-1, z; (ii) x+1, y, z; (iii) x-1, y, z; (iv) -x+1, -y+1, -z+2; (v) -x, -y+1, -z+2; (vi) -x+1, -y+3, -z+1.

Data collection: RAPID-AUTO (Rigaku, 1998[Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002[Rigaku/MSC (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2009[Westrip, S. P. (2009). publCIF. In preparation.]).

Supporting information


Related literature top

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

Experimental top

To an aqueous solution of 3-aminopyrazine (0.19 g, 2 mmol) was added manganese(II) sulfate tetrahydrate (0.45 g, 2 mmol). Colorless crystals of the salt separated from the solution after a few days. CH&N elemental analysis. Calc. for C8H34N6O20S2Mn2: C 13.56, H 4.84, N 11.86%; found: C 13.52, H 4.80, N 11.85%.

Refinement top

Carbon-bound H-atoms were placed in calculated positions (C—H 0.93 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2U(C). The amino and water H-atoms were located in a difference Fourier map, and were refined with a distance restraint of N–H = O–H = 0.85±0.01 Å; their temperature factors were refined.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); 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).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of [Mn(H2O)6] [Mn(H2O)4(C4H5N3)2] 2[SO4].2H2O at the 50% probability level; hydrogen atoms are drawn as spheres of arbitrary radius.
Hexaaquamanganese(II) tetraaquabis(2-aminopyrazine-κN4)manganese(II) disulfate dihydrate top
Crystal data top
[Mn(H2O)6][Mn(C4H5N3)2(H2O)4](SO4)2·2H2OZ = 1
Mr = 708.43F(000) = 366
Triclinic, P1Dx = 1.685 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.6242 (3) ÅCell parameters from 6492 reflections
b = 8.4639 (4) Åθ = 3.2–27.5°
c = 13.2719 (8) ŵ = 1.14 mm1
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
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3159 independent reflections
Radiation source: fine-focus sealed tube2874 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 88
Tmin = 0.670, Tmax = 0.821k = 1010
6866 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H 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 parametersΔρmax = 0.74 e Å3
14 restraintsΔρmin = 0.40 e Å3
Crystal data top
[Mn(H2O)6][Mn(C4H5N3)2(H2O)4](SO4)2·2H2Oγ = 78.834 (2)°
Mr = 708.43V = 697.95 (6) Å3
Triclinic, P1Z = 1
a = 6.6242 (3) ÅMo Kα radiation
b = 8.4639 (4) ŵ = 1.14 mm1
c = 13.2719 (8) ÅT = 293 K
α = 75.654 (2)°0.38 × 0.20 × 0.18 mm
β = 78.364 (2)°
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3159 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
2874 reflections with I > 2σ(I)
Tmin = 0.670, Tmax = 0.821Rint = 0.025
6866 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04114 restraints
wR(F2) = 0.129H atoms treated by a mixture of independent and constrained refinement
S = 1.15Δρmax = 0.74 e Å3
3159 reflectionsΔρmin = 0.40 e Å3
231 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn11.00001.00000.50000.02349 (17)
Mn20.00000.50001.00000.02867 (18)
S10.47994 (10)0.88750 (9)0.80279 (5)0.02457 (18)
O10.4091 (3)0.9828 (3)0.70435 (17)0.0322 (5)
O20.5386 (4)0.7129 (3)0.7978 (2)0.0444 (6)
O30.6644 (3)0.9501 (3)0.81657 (17)0.0318 (5)
O40.3121 (4)0.9084 (4)0.89137 (19)0.0441 (6)
O1W0.7084 (4)0.9110 (3)0.53580 (19)0.0335 (5)
O2W1.0209 (4)0.9617 (3)0.66525 (17)0.0345 (5)
O3W0.2937 (4)0.4732 (3)0.8939 (2)0.0471 (7)
O4W0.1480 (4)0.4748 (3)0.8707 (2)0.0429 (6)
O5W0.0400 (4)0.2353 (3)1.0577 (2)0.0456 (6)
O6W0.6189 (4)0.2200 (3)0.9081 (2)0.0399 (6)
N10.8363 (4)1.2689 (3)0.4980 (2)0.0301 (5)
N20.7098 (4)1.6040 (3)0.4930 (2)0.0344 (6)
N30.7810 (6)1.6587 (4)0.3104 (3)0.0482 (8)
C10.8414 (5)1.3800 (4)0.4078 (3)0.0334 (7)
H10.88991.34470.34500.040*
C20.7760 (5)1.5496 (4)0.4039 (3)0.0325 (6)
C30.7019 (5)1.4892 (4)0.5836 (3)0.0376 (7)
H30.65321.52370.64660.045*
C40.7623 (5)1.3238 (4)0.5874 (3)0.0348 (7)
H40.75221.24910.65210.042*
H1W10.614 (5)0.948 (5)0.581 (3)0.048 (12)*
H1W20.715 (7)0.817 (3)0.521 (4)0.053 (13)*
H2W10.919 (4)0.972 (5)0.714 (2)0.028 (9)*
H2W21.135 (4)0.967 (5)0.683 (3)0.044 (11)*
H3W10.357 (7)0.556 (4)0.866 (4)0.066 (15)*
H3W20.391 (5)0.392 (3)0.901 (3)0.039 (11)*
H4W10.195 (8)0.386 (4)0.876 (4)0.073 (17)*
H4W20.247 (5)0.554 (4)0.859 (4)0.063 (15)*
H5W10.126 (6)0.160 (4)1.089 (3)0.059 (14)*
H5W20.072 (5)0.194 (7)1.074 (5)0.081 (18)*
H6W10.624 (9)0.148 (5)0.873 (4)0.079 (18)*
H6W20.641 (9)0.170 (6)0.9698 (19)0.072 (17)*
H3N10.831 (7)1.629 (6)0.252 (2)0.062 (15)*
H3N20.738 (8)1.7613 (19)0.308 (4)0.060 (14)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0217 (3)0.0225 (3)0.0255 (3)0.0022 (2)0.0054 (2)0.0034 (2)
Mn20.0218 (3)0.0271 (3)0.0341 (3)0.0032 (2)0.0067 (2)0.0002 (2)
S10.0209 (3)0.0257 (3)0.0260 (3)0.0046 (3)0.0066 (2)0.0004 (3)
O10.0289 (11)0.0353 (12)0.0302 (11)0.0007 (9)0.0115 (9)0.0009 (9)
O20.0423 (14)0.0252 (11)0.0645 (17)0.0035 (10)0.0175 (12)0.0014 (11)
O30.0224 (10)0.0385 (12)0.0356 (11)0.0062 (9)0.0079 (8)0.0062 (9)
O40.0313 (12)0.0672 (17)0.0317 (12)0.0132 (12)0.0012 (10)0.0078 (11)
O1W0.0277 (11)0.0325 (12)0.0423 (13)0.0092 (9)0.0038 (9)0.0157 (10)
O2W0.0258 (11)0.0521 (14)0.0264 (10)0.0058 (10)0.0080 (9)0.0068 (10)
O3W0.0281 (12)0.0356 (14)0.0671 (18)0.0064 (11)0.0055 (12)0.0012 (12)
O4W0.0395 (14)0.0380 (14)0.0542 (15)0.0039 (11)0.0212 (12)0.0059 (12)
O5W0.0318 (13)0.0320 (12)0.0679 (17)0.0074 (10)0.0194 (12)0.0096 (12)
O6W0.0477 (14)0.0317 (12)0.0413 (14)0.0016 (11)0.0131 (11)0.0086 (10)
N10.0269 (12)0.0226 (12)0.0390 (14)0.0011 (10)0.0063 (10)0.0044 (10)
N20.0293 (13)0.0255 (12)0.0498 (16)0.0013 (10)0.0095 (12)0.0109 (11)
N30.063 (2)0.0285 (15)0.0451 (18)0.0031 (15)0.0061 (16)0.0039 (13)
C10.0347 (16)0.0256 (15)0.0380 (16)0.0001 (12)0.0061 (13)0.0069 (12)
C20.0289 (15)0.0238 (14)0.0435 (17)0.0014 (12)0.0071 (13)0.0060 (12)
C30.0337 (16)0.0391 (18)0.0425 (18)0.0019 (14)0.0073 (14)0.0182 (14)
C40.0318 (16)0.0335 (16)0.0352 (16)0.0037 (13)0.0075 (13)0.0051 (13)
Geometric parameters (Å, º) top
Mn1—O1W2.131 (2)O3W—H3W10.849 (10)
Mn1—O1Wi2.131 (2)O3W—H3W20.849 (10)
Mn1—O2Wi2.165 (2)O4W—H4W10.848 (10)
Mn1—O2W2.165 (2)O4W—H4W20.850 (10)
Mn1—N12.320 (2)O5W—H5W10.849 (10)
Mn1—N1i2.320 (2)O5W—H5W20.850 (10)
Mn2—O3W2.168 (3)O6W—H6W10.850 (10)
Mn2—O3Wii2.168 (3)O6W—H6W20.850 (10)
Mn2—O4W2.212 (3)N1—C11.325 (4)
Mn2—O4Wii2.212 (3)N1—C41.347 (4)
Mn2—O5Wii2.163 (2)N2—C21.337 (4)
Mn2—O5W2.163 (2)N2—C31.344 (5)
S1—O41.466 (2)N3—C21.350 (5)
S1—O21.468 (3)N3—H3N10.855 (10)
S1—O11.468 (2)N3—H3N20.854 (10)
S1—O31.482 (2)C1—C21.408 (4)
O1W—H1W10.844 (10)C1—H10.9300
O1W—H1W20.851 (10)C3—C41.371 (5)
O2W—H2W10.846 (10)C3—H30.9300
O2W—H2W20.852 (10)C4—H40.9300
O1W—Mn1—O1Wi180.000 (1)Mn1—O1W—H1W1118 (3)
O1W—Mn1—O2Wi87.90 (9)Mn1—O1W—H1W2114 (3)
O1Wi—Mn1—O2Wi92.10 (9)H1W1—O1W—H1W2123 (4)
O1W—Mn1—O2W92.10 (9)Mn1—O2W—H2W1125 (3)
O1Wi—Mn1—O2W87.90 (9)Mn1—O2W—H2W2120 (3)
O2Wi—Mn1—O2W180.000 (1)H2W1—O2W—H2W2112 (4)
O1W—Mn1—N191.71 (9)Mn2—O3W—H3W1120 (4)
O1Wi—Mn1—N188.29 (9)Mn2—O3W—H3W2126 (3)
O2Wi—Mn1—N189.32 (10)H3W1—O3W—H3W2104 (4)
O2W—Mn1—N190.68 (10)Mn2—O4W—H4W1119 (4)
O1W—Mn1—N1i88.29 (9)Mn2—O4W—H4W2110 (3)
O1Wi—Mn1—N1i91.71 (9)H4W1—O4W—H4W2107 (5)
O2Wi—Mn1—N1i90.68 (10)Mn2—O5W—H5W1139 (3)
O2W—Mn1—N1i89.32 (10)Mn2—O5W—H5W2115 (4)
N1—Mn1—N1i180.000 (1)H5W1—O5W—H5W2103 (5)
O5Wii—Mn2—O5W180.000 (1)H6W1—O6W—H6W2108 (5)
O5Wii—Mn2—O3W90.64 (10)C1—N1—C4117.4 (3)
O5W—Mn2—O3W89.36 (10)C1—N1—Mn1119.9 (2)
O5Wii—Mn2—O3Wii89.36 (10)C4—N1—Mn1121.9 (2)
O5W—Mn2—O3Wii90.64 (10)C2—N2—C3116.8 (3)
O3W—Mn2—O3Wii180.000 (1)C2—N3—H3N1122 (3)
O5Wii—Mn2—O4W89.84 (10)C2—N3—H3N2121 (3)
O5W—Mn2—O4W90.16 (10)H3N1—N3—H3N2117 (5)
O3W—Mn2—O4W86.45 (11)N1—C1—C2122.2 (3)
O3Wii—Mn2—O4W93.55 (11)N1—C1—H1118.9
O5Wii—Mn2—O4Wii90.16 (10)C2—C1—H1118.9
O5W—Mn2—O4Wii89.84 (10)N2—C2—N3119.4 (3)
O3W—Mn2—O4Wii93.55 (11)N2—C2—C1120.2 (3)
O3Wii—Mn2—O4Wii86.45 (11)N3—C2—C1120.4 (3)
O4W—Mn2—O4Wii180.000 (1)N2—C3—C4123.1 (3)
O4—S1—O2110.85 (17)N2—C3—H3118.4
O4—S1—O1109.03 (14)C4—C3—H3118.4
O2—S1—O1109.60 (15)N1—C4—C3120.3 (3)
O4—S1—O3109.10 (14)N1—C4—H4119.9
O2—S1—O3109.02 (14)C3—C4—H4119.9
O1—S1—O3109.22 (13)
Symmetry codes: (i) x+2, y+2, z+1; (ii) x, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O10.84 (1)1.95 (2)2.779 (3)167 (4)
O1w—H1w2···N2iii0.85 (1)1.94 (1)2.792 (3)176 (5)
O2w—H2w1···O30.85 (1)1.95 (1)2.775 (3)166 (4)
O2w—H2w2···O1iv0.85 (1)1.92 (1)2.770 (3)172 (4)
O3w—H3w1···O20.85 (1)1.90 (1)2.744 (4)170 (5)
O3w—H3w2···O6w0.85 (1)1.88 (1)2.728 (4)175 (4)
O4w—H4w1···O6wv0.85 (1)1.96 (2)2.780 (4)162 (5)
O4w—H4w2···O2v0.85 (1)1.92 (2)2.744 (4)164 (5)
O5w—H5w1···O3vi0.84 (1)2.00 (2)2.813 (3)159 (5)
O5w—H5w2···O4ii0.85 (1)1.88 (1)2.726 (4)177 (6)
O6w—H6w1···O3iii0.85 (1)1.95 (2)2.783 (3)167 (6)
O6w—H6w2···O4vi0.85 (1)1.87 (1)2.709 (4)172 (6)
N3—H3n2···O1vii0.85 (1)2.18 (1)3.026 (4)172 (5)
Symmetry codes: (ii) x, y+1, z+2; (iii) x, y1, z; (iv) x+1, y, z; (v) x1, y, z; (vi) x+1, y+1, z+2; (vii) x+1, y+3, z+1.

Experimental details

Crystal data
Chemical formula[Mn(H2O)6][Mn(C4H5N3)2(H2O)4](SO4)2·2H2O
Mr708.43
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)6.6242 (3), 8.4639 (4), 13.2719 (8)
α, β, γ (°)75.654 (2), 78.364 (2), 78.834 (2)
V3)697.95 (6)
Z1
Radiation typeMo Kα
µ (mm1)1.14
Crystal size (mm)0.38 × 0.20 × 0.18
Data collection
DiffractometerRigaku R-AXIS RAPID IP
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.670, 0.821
No. of measured, independent and
observed [I > 2σ(I)] reflections
6866, 3159, 2874
Rint0.025
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.129, 1.15
No. of reflections3159
No. of parameters231
No. of restraints14
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.74, 0.40

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalClear (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O10.84 (1)1.95 (2)2.779 (3)167 (4)
O1w—H1w2···N2i0.85 (1)1.94 (1)2.792 (3)176 (5)
O2w—H2w1···O30.85 (1)1.95 (1)2.775 (3)166 (4)
O2w—H2w2···O1ii0.85 (1)1.92 (1)2.770 (3)172 (4)
O3w—H3w1···O20.85 (1)1.90 (1)2.744 (4)170 (5)
O3w—H3w2···O6w0.85 (1)1.88 (1)2.728 (4)175 (4)
O4w—H4w1···O6wiii0.85 (1)1.96 (2)2.780 (4)162 (5)
O4w—H4w2···O2iii0.85 (1)1.92 (2)2.744 (4)164 (5)
O5w—H5w1···O3iv0.84 (1)2.00 (2)2.813 (3)159 (5)
O5w—H5w2···O4v0.85 (1)1.88 (1)2.726 (4)177 (6)
O6w—H6w1···O3i0.85 (1)1.95 (2)2.783 (3)167 (6)
O6w—H6w2···O4iv0.85 (1)1.87 (1)2.709 (4)172 (6)
N3—H3n2···O1vi0.85 (1)2.18 (1)3.026 (4)172 (5)
Symmetry codes: (i) x, y1, z; (ii) x+1, y, z; (iii) x1, y, z; (iv) x+1, y+1, z+2; (v) x, y+1, z+2; (vi) x+1, y+3, z+1.
 

Acknowledgements

We thank the Natural Science Foundation of Heilongjiang Province (No. B200501), Heilongjiang University, China, and the University of Malaya for supporting this study.

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