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Acta Crystallogr Sect E Struct Rep Online. 2009 December 1; 65(Pt 12): m1502.
Published online 2009 November 4. doi:  10.1107/S1600536809045309
PMCID: PMC2972178

Tetra­kis(2-amino­pyrazine-κN 4)dichlorido­cobalt(II)

Abstract

The CoII atom in the title complex, [CoCl2(C4H5N3)4], exists in an all-trans Cl2N4Co octa­hedral geometry. The CoII atom lies on a special position of 2 site symmetry. Adjacent mol­ecules are linked by N—H(...)N and N—H(...)Cl hydrogen bonds into a three-dimensional network.

Related literature

For the triclinic modification, see: Csöregh et al. (2000 [triangle]).

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Object name is e-65-m1502-scheme1.jpg

Experimental

Crystal data

  • [CoCl2(C4H5N3)4]
  • M r = 510.27
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1502-efi1.jpg
  • a = 7.6347 (2) Å
  • b = 15.7341 (4) Å
  • c = 18.6074 (4) Å
  • V = 2235.22 (9) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.04 mm−1
  • T = 293 K
  • 0.30 × 0.20 × 0.15 mm

Data collection

  • Rigaku R-AXIS RAPID IP diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.746, T max = 0.860
  • 20053 measured reflections
  • 2553 independent reflections
  • 2234 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.025
  • wR(F 2) = 0.074
  • S = 1.06
  • 2553 reflections
  • 157 parameters
  • 4 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.29 e Å−3
  • Δρmin = −0.25 e Å−3

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

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809045309/xu2656sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045309/xu2656Isup2.hkl

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

Acknowledgments

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

supplementary crystallographic information

Experimental

Cobalt(II) chloride hexahydrate (0.48 g, 2 mmol) and 2-aminopyrazine (0.19 g, 2 mmol) were dissolved in a small volume of water. Red crystals of the adduct separated from the filtered solution after several days. CH&N elemental analysis. Calc. for C16H20Cl2N12Co: C 37.66, H 3.95, N 32.94%; found: C 37.63, H 3.89, N 32.97%.

Refinement

Amino-H atoms were located in a difference Fourier map and refined isotropically with a distance restraint of N–H = 0.86±0.01 Å. 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 Uiso(H) set to 1.2Ueq(C).

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of CoCl2(C2H5N3)4 at the 50% probability level; hydrogen atoms are drawn as spheres of arbitrary radius.

Crystal data

[CoCl2(C4H5N3)4]F(000) = 1044
Mr = 510.27Dx = 1.516 Mg m3
Orthorhombic, PccnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2acCell parameters from 15790 reflections
a = 7.6347 (2) Åθ = 2.3–27.5°
b = 15.7341 (4) ŵ = 1.04 mm1
c = 18.6074 (4) ÅT = 293 K
V = 2235.22 (9) Å3Block, red
Z = 40.30 × 0.20 × 0.15 mm

Data collection

Rigaku RAXIS-RAPID IP diffractometer2553 independent reflections
Radiation source: fine-focus sealed tube2234 reflections with I > 2σ(I)
graphiteRint = 0.024
ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −9→9
Tmin = 0.746, Tmax = 0.860k = −20→20
20053 measured reflectionsl = −24→24

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.0439P)2 + 0.4514P] where P = (Fo2 + 2Fc2)/3
2553 reflections(Δ/σ)max = 0.001
157 parametersΔρmax = 0.28 e Å3
4 restraintsΔρmin = −0.25 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Co10.75000.25000.103443 (12)0.02794 (9)
Cl10.98632 (5)0.14744 (2)0.103952 (17)0.03970 (11)
N10.61989 (16)0.17473 (8)0.01880 (6)0.0348 (3)
N20.46194 (19)0.08976 (11)−0.09614 (7)0.0553 (4)
N30.1968 (2)0.09877 (14)−0.03954 (8)0.0686 (5)
N40.88907 (16)0.31841 (7)0.18890 (6)0.0339 (3)
N51.03169 (17)0.40550 (8)0.30631 (6)0.0387 (3)
N60.9535 (2)0.53209 (8)0.25231 (7)0.0527 (4)
C10.45050 (19)0.15892 (9)0.01846 (7)0.0357 (3)
H1A0.38230.17710.05690.043*
C20.3693 (2)0.11475 (10)−0.03920 (7)0.0413 (3)
C30.6338 (2)0.10573 (14)−0.09351 (9)0.0625 (6)
H3A0.70270.0878−0.13180.075*
C40.7141 (2)0.14683 (13)−0.03790 (9)0.0509 (4)
H4A0.83450.1557−0.03910.061*
C50.88843 (19)0.40188 (8)0.19189 (6)0.0319 (3)
H50.83950.43240.15410.038*
C60.96002 (18)0.44673 (8)0.25094 (7)0.0325 (3)
C71.0327 (2)0.32043 (10)0.30155 (8)0.0453 (4)
H71.08230.28960.33900.054*
C80.9645 (2)0.27664 (10)0.24459 (8)0.0452 (4)
H80.97000.21760.24400.054*
H10.136 (3)0.1094 (14)−0.0022 (8)0.078 (7)*
H20.155 (3)0.0704 (11)−0.0753 (8)0.063 (6)*
H30.978 (3)0.5580 (12)0.2913 (7)0.060 (6)*
H40.909 (2)0.5583 (11)0.2164 (8)0.061 (6)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.03367 (16)0.02901 (14)0.02114 (14)−0.00229 (9)0.0000.000
Cl10.0462 (2)0.0432 (2)0.02968 (18)0.01013 (15)0.00662 (13)0.00476 (12)
N10.0337 (6)0.0435 (6)0.0271 (5)−0.0030 (5)0.0015 (5)−0.0079 (5)
N20.0407 (8)0.0851 (11)0.0401 (7)−0.0055 (7)0.0052 (6)−0.0322 (7)
N30.0366 (8)0.1287 (16)0.0407 (8)−0.0134 (9)0.0027 (6)−0.0368 (9)
N40.0428 (7)0.0326 (5)0.0262 (5)−0.0011 (5)−0.0058 (5)0.0003 (4)
N50.0447 (7)0.0433 (6)0.0281 (5)−0.0005 (5)−0.0095 (5)−0.0004 (5)
N60.0912 (12)0.0339 (6)0.0331 (6)−0.0092 (7)−0.0211 (7)0.0002 (5)
C10.0359 (7)0.0464 (7)0.0248 (6)0.0013 (6)0.0028 (5)−0.0084 (6)
C20.0352 (8)0.0588 (9)0.0300 (6)−0.0012 (7)0.0005 (6)−0.0124 (6)
C30.0416 (9)0.1031 (16)0.0429 (9)−0.0042 (10)0.0106 (7)−0.0368 (9)
C40.0340 (8)0.0789 (12)0.0398 (8)−0.0060 (7)0.0075 (6)−0.0206 (8)
C50.0399 (7)0.0323 (6)0.0236 (6)−0.0039 (5)−0.0055 (5)0.0036 (5)
C60.0376 (7)0.0349 (6)0.0251 (6)−0.0057 (5)−0.0034 (5)0.0008 (5)
C70.0582 (10)0.0450 (8)0.0326 (7)0.0103 (7)−0.0151 (7)0.0028 (6)
C80.0650 (11)0.0335 (7)0.0371 (7)0.0090 (7)−0.0136 (7)0.0015 (6)

Geometric parameters (Å, °)

Co1—N1i2.2068 (11)N5—C61.3348 (18)
Co1—N12.2068 (11)N5—C71.341 (2)
Co1—N42.1941 (11)N6—C61.3441 (18)
Co1—N4i2.1941 (11)N6—H30.852 (9)
Co1—Cl1i2.4206 (4)N6—H40.856 (9)
Co1—Cl12.4206 (4)C1—C21.4207 (19)
N1—C11.3170 (19)C1—H1A0.9300
N1—C41.3501 (19)C3—C41.366 (2)
N2—C21.3332 (19)C3—H3A0.9300
N2—C31.337 (2)C4—H4A0.9300
N3—C21.341 (2)C5—C61.4157 (18)
N3—H10.853 (9)C5—H50.9300
N3—H20.864 (9)C7—C81.367 (2)
N4—C51.3145 (17)C7—H70.9300
N4—C81.3556 (18)C8—H80.9300
N4—Co1—N4i87.12 (6)C6—N6—H4118.8 (14)
N4—Co1—N1i92.07 (4)H3—N6—H4121 (2)
N4i—Co1—N1i176.67 (4)N1—C1—C2121.63 (13)
N4—Co1—N1176.67 (4)N1—C1—H1A119.2
N4i—Co1—N192.07 (4)C2—C1—H1A119.2
N1i—Co1—N188.93 (6)N2—C2—N3117.51 (14)
N4—Co1—Cl1i91.77 (3)N2—C2—C1120.88 (15)
N4i—Co1—Cl1i87.91 (3)N3—C2—C1121.59 (13)
N1i—Co1—Cl1i88.89 (3)N2—C3—C4123.88 (15)
N1—Co1—Cl1i91.43 (3)N2—C3—H3A118.1
N4—Co1—Cl187.91 (3)C4—C3—H3A118.1
N4i—Co1—Cl191.77 (3)N1—C4—C3120.47 (15)
N1i—Co1—Cl191.43 (3)N1—C4—H4A119.8
N1—Co1—Cl188.89 (3)C3—C4—H4A119.8
Cl1i—Co1—Cl1179.552 (18)N4—C5—C6121.97 (12)
C1—N1—C4117.25 (12)N4—C5—H5119.0
C1—N1—Co1123.15 (9)C6—C5—H5119.0
C4—N1—Co1119.50 (10)N5—C6—N6119.10 (12)
C2—N2—C3115.85 (13)N5—C6—C5121.00 (12)
C2—N3—H1119.6 (16)N6—C6—C5119.89 (12)
C2—N3—H2117.9 (14)N5—C7—C8123.50 (13)
H1—N3—H2122 (2)N5—C7—H7118.2
C5—N4—C8116.97 (12)C8—C7—H7118.2
C5—N4—Co1121.27 (9)N4—C8—C7120.67 (14)
C8—N4—Co1121.45 (10)N4—C8—H8119.7
C6—N5—C7115.87 (12)C7—C8—H8119.7
C6—N6—H3119.0 (14)
N4i—Co1—N1—C145.73 (12)C3—N2—C2—N3−179.1 (2)
N1i—Co1—N1—C1−131.09 (13)C3—N2—C2—C12.7 (3)
Cl1i—Co1—N1—C1−42.23 (11)N1—C1—C2—N2−1.9 (2)
Cl1—Co1—N1—C1137.45 (11)N1—C1—C2—N3−179.93 (17)
N4i—Co1—N1—C4−138.03 (13)C2—N2—C3—C4−1.6 (3)
N1i—Co1—N1—C445.15 (12)C1—N1—C4—C31.4 (3)
Cl1i—Co1—N1—C4134.01 (13)Co1—N1—C4—C3−175.03 (16)
Cl1—Co1—N1—C4−46.30 (13)N2—C3—C4—N1−0.5 (4)
N4i—Co1—N4—C5−124.52 (13)C8—N4—C5—C6−1.1 (2)
N1i—Co1—N4—C552.25 (11)Co1—N4—C5—C6172.58 (10)
Cl1i—Co1—N4—C5−36.70 (11)C7—N5—C6—N6179.54 (15)
Cl1—Co1—N4—C5143.61 (11)C7—N5—C6—C50.7 (2)
N4i—Co1—N4—C848.91 (11)N4—C5—C6—N50.1 (2)
N1i—Co1—N4—C8−134.32 (13)N4—C5—C6—N6−178.74 (15)
Cl1i—Co1—N4—C8136.73 (12)C6—N5—C7—C8−0.5 (3)
Cl1—Co1—N4—C8−42.96 (12)C5—N4—C8—C71.4 (2)
C4—N1—C1—C2−0.3 (2)Co1—N4—C8—C7−172.29 (13)
Co1—N1—C1—C2176.01 (11)N5—C7—C8—N4−0.6 (3)

Symmetry codes: (i) −x+3/2, −y+1/2, z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N3—H1···Cl1ii0.85 (1)2.36 (1)3.209 (2)175 (2)
N3—H2···N5iii0.86 (1)2.43 (2)3.134 (2)140 (2)
N6—H3···Cl1iv0.85 (1)2.42 (1)3.265 (1)171 (2)
N6—H4···N2v0.86 (1)2.33 (2)3.045 (2)142 (2)

Symmetry codes: (ii) x−1, y, z; (iii) x−1, −y+1/2, z−1/2; (iv) −x+2, y+1/2, −z+1/2; (v) x+1/2, y+1/2, −z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU2656).

References

  • Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.
  • Csöregh, I., Kennessey, G., Wadsten, T., Liptay, G. & Carson, B. R. (2000). Z. Kristallogr. 215, 547–552.
  • Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
  • Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
  • Rigaku/MSC (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2009). publCIF. In preparation.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography