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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 71| Part 6| June 2015| Pages 709-711

Crystal structure of poly[(2,2′-bi­pyridine-κ2N,N′)tetra­kis­(μ-cyanido-κ2N:C)dinickel(II)]

aCollege of Chemistry and Chemical Engineering, Mu Danjiang Normal University, Mu Danjiang 157012, People's Republic of China
*Correspondence e-mail: cuisx981@163.com

Edited by M. Weil, Vienna University of Technology, Austria (Received 11 May 2015; accepted 20 May 2015; online 28 May 2015)

The polymeric title complex, [Ni2(CN)4(C10H8N2)]n, was obtained serendipitously under hydro­thermal conditions. The asymmetric unit consists of one half of an [Ni(CN)4]2− anion with the Ni2+ cation situated on an inversion centre, and one half of an [Ni(2,2′-bpy)]2+ cation (2,2′-bpy is 2,2′-bi­pyridine), with the second Ni2+ cation situated on a twofold rotation axis. The two Ni2+ cations exhibit different coordination spheres. Whereas the coordination of the metal in the anion is that of a slightly distorted square defined by four C-bound cyanide ligands, the coordination in the cation is that of a distorted octa­hedron defined by four N-bound cyanide ligands and two N atoms from the chelating 2,2′-bpy ligand. The two different Ni2+ cations are alternately bridged by the cyanide ligands, resulting in a two-dimensional structure extending parallel to (010). Within the sheets, ππ inter­actions between pyridine rings of neighbouring 2,2′-bpy ligands, with a centroid-to-centroid distance of 3.687 (3) Å, are present. The crystal packing is dominated by van der Waals forces. A weak C—H⋯N inter­action between adjacent sheets is also observed.

1. Chemical context

Coordination metal complexes have been the subject of intensive investigation not only due to their potential application to material science as catalytic, conductive, luminescent, magnetic, porous, chiral or non-linear optical materials (Janiak et al., 2003[Janiak, C. (2003). Dalton Trans. pp. 2781-2894.]), but also because of their intriguing structural diversity (Kong et al., 2008[Kong, X. J., Ren, Y. P., Chen, W. X., Long, L. S., Zheng, Z., Huang, R. B. & Zheng, L. S. (2008). Angew. Chem. Int. Ed. 47, 2398-2401.]). The assembly of functional mol­ecular building blocks into crystalline polymeric materials through coordination bonds or other weak inter­actions has many advantages over traditional stepwise syntheses and was demonstrated to be an effective approach to fabricating new materials (Kopotkov et al., 2014[Kopotkov, V. A., Yagubskii, E. B., Simonov, S. V., Zorina, L. V., Starichenko, D. V., Korolyov, A. V., Ustinov, V. V. & Shvachko, Y. N. (2014). New J. Chem. 38, 4167-4176.]). Using this approach, numerous materials with inter­esting structures and properties have been prepared through the reactions of cyanidometallate building blocks (Cui et al., 2011[Cui, S., Zuo, M., Zhang, J., Zhao, Y., Tan, R., Liu, S. & Su, S. (2011). Acta Cryst. E67, m1706-m1707.]; Zhang & Lachgar, 2015[Zhang, J. J. & Lachgar, A. (2015). Inorg. Chem. 54, 1082-1090.]). These compounds show novel functionalities due to strong inter­actions mediated by the linear cyanide bridges. The probably oldest and most inter­esting example is the Prussian blue framework, Fe4[Fe(CN)6]3·14H2O, and its analogues derived from the assembly of hexa­cyanidometalate anions [M(CN)6]n and transition-metal ions (Li et al., 2008[Li, D. F., Clérac, R., Roubeau, O., Harté, E., Mathonière, C., Le Bris, R. & Holmes, S. M. (2008). J. Am. Chem. Soc. 130, 252-258.]). For instance, cyanide-bridged bimetallic assemblies were obtained from K3[Fe(CN)6] as a source of cyanidometalate anions, metal cations, and aromatic nitro­gen-containing ligands. These compounds show inter­esting magnetic and other properties that can be affected through the careful choice of the building-block components (Shen et al., 2014[Shen, X. P., Zhou, H. B., Yan, J. H., Li, Y. F. & Zhou, H. (2014). Inorg. Chem. 53, 116-127.]).

[Scheme 1]

Our own efforts are focused to assemble metallic complexes and the achievement of tuning their properties by crystal engineering of the terminal/bridging ligands. However, the hydro­thermal reaction of Ni(acetate)2, 2,2′-bi­pyridine and K3[Fe(CN)6] did not yield the expected bimetallic system analogous to coordinated iron ions which were reported in literature (Colacio et al., 2003[Colacio, E., Domínguez-Vera, J. M., Lloret, F., Moreno Sánchez, J. M., Kivekäs, R., Rodríguez, A. & Sillanpää, R. (2003). Inorg. Chem. 42, 4209-4214.]), but to the serendipitous formation of the polymeric complex (I)[link], [Ni2(CN)4(C10H8N2)]n, the crystal structure of which is reported here.

2. Structural commentary

The asymmetric unit of the structure of (I)[link] contains formally one half of an [Ni(CN)4]2− (Ni1) anion, and one half of an [Ni(2,2′-bpy)]2+ (Ni2) cation (2,2′-bpy is 2,2′-bi­pyridine). The anion is completed by inversion symmetry, whereas the cation is completed by a twofold rotation axis (Fig. 1[link]). The Ni1 atom shows a slightly distorted square-planar geometry through coordination by four C atoms (C6 and C6i, C7 and C7i) [symmetry code: (i)x + 2, −y, −z + 1] from four cyanide groups, bridging Ni1 to four adjacent Ni2 atoms. The latter exhibits an overall distorted octa­hedral environment, being defined by four N atoms (N3, N3ii, N2ii, N2iii) [symmetry codes: (ii) −x + 1, y, −z + [{3\over 2}]; (iii) x − 1, y, z] from four [Ni(CN)4]2− groups, and two N atoms (N1 and N1ii) of one 2,2′-bpy ligand. The corresponding N1—Ni2—N1 bite angle is 77.32 (13)°. Relevant bond lengths involving the two metal cations are compiled in Table 1[link]. As depicted in Fig. 2[link], the cyanide groups bridge nickel cations, forming undulating sheets of composition [Ni2(CN)4(2,2′-bpy)2] parallel to (010), constituted by alternation of Ni1 and Ni2 ions.

Table 1
Selected bond lengths (Å)

Ni1—C6 1.863 (3) Ni2—N1 2.102 (2)
Ni1—C7 1.871 (3) Ni2—N2i 2.116 (2)
Ni2—N3 2.071 (2)    
Symmetry code: (i) x-1, y, z.
[Figure 1]
Figure 1
The principal building units of complex (I)[link], showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity. For symmetry codes, see text.
[Figure 2]
Figure 2
A view of the polymeric sheet of complex (I)[link]. Ni atoms are represented by hatched green spheres, C atoms are grey, N atoms blue and H atoms green.

3. Supra­molecular features

Within a sheet, ππ inter­actions between pyridine rings with a centroid-to-centroid distance of 3.687 (3) Å are present. The adhesion of the sheets in the crystal packing is dominated by van der Waals forces. However, a weak non-classical C—H⋯N inter­action (Table 2[link]) between neighbouring sheets may participate in the stabilization of the crystal packing.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C1—H1⋯N3 0.96 (3) 2.54 (3) 3.129 (3) 120 (2)

4. Synthesis and crystallization

Ni(acetate)2 (0.159 g, 0.64 mmol), 2,2′-bi­pyridine (0.047 g, 0.3 mmol) and K3[Fe(CN)6] (0.21 g, 0.64 mmol) dissolved in aqueous solution of 1M NaCl (8 ml) were added to a 15 ml Teflon-lined autoclave and heated at 433 K for 3 d. The autoclave was then cooled to room temperature. Green block-shaped crystals of (I)[link] deposited on the wall of the container and were collected and air-dried.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3[link]. Hydrogen atoms bound to carbon were found in a difference map and were refined with Uiso(H) = 1.2Ueq(C).

Table 3
Experimental details

Crystal data
Chemical formula [Ni2(CN)4(C10H8N2)]
Mr 377.68
Crystal system, space group Monoclinic, C2/c
Temperature (K) 293
a, b, c (Å) 6.519 (5), 16.698 (5), 12.019 (5)
β (°) 90.852 (5)
V3) 1308.2 (12)
Z 4
Radiation type Mo Kα
μ (mm−1) 2.88
Crystal size (mm) 0.40 × 0.10 × 0.06
 
Data collection
Diffractometer Siemens SMART CCD
No. of measured, independent and observed [I > 2σ(I)] reflections 3858, 1156, 1039
Rint 0.032
(sin θ/λ)max−1) 0.594
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.074, 1.10
No. of reflections 1156
No. of parameters 118
H-atom treatment H atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3) 0.71, −0.40
Computer programs: SMART and SAINT (Bruker, 2007[Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]), SHELXS97, SHELXL97and XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Chemical context top

Coordination metal complexes have been the subject of intensive investigation not only due to their potential application to material science as catalytic, conductive, luminescent, magnetic, porous, chiral or non-linear optical materials (Janiak et al., 2003), but also because of their intriguing structural diversity (Kong et al., 2008). The assembly of functional molecular building blocks into crystalline polymeric materials through coordination bonds or other weak inter­actions has many advantages over traditional stepwise syntheses and was demonstrated to be an effective approach to fabricating new materials (Kopotkov et al., 2014). Using this approach, numerous materials with inter­esting structures and properties have been prepared through the reactions of cyanidometallate building blocks (Cui et al., 2011; Zhang & Lachgar, 2015). These compounds show novel functionalities due to strong inter­actions mediated by the linear cyanide bridges. The probably oldest and most inter­esting example is the Prussian blue framework, Fe4[Fe(CN)6]3·14H2O, and its analogues derived from the assembly of hexacyanidometalate anions [M(CN)6]n and transition-metal ions (Li et al., 2008). For instance, cyanide-bridged bimetallic assemblies were obtained from K3[Fe(CN)6] as a source of cyanidometalate anions, metal cations, and aromatic nitro­gen-containing ligands. These compounds show inter­esting magnetic and other properties that can be affected through the careful choice of the building-block components (Shen et al., 2014).

Our own efforts are focused to assemble metallic complexes and the achievement of tuning their properties by crystal engineering of the terminal/bridging ligands. However, the hydro­thermal reaction of Ni(acetate)2, 2,2'-bi­pyridine and K3[Fe(CN)6] did not yield the expected bimetallic system analogous to coordinated iron ions which were reported in literature (Colacio et al., 2003), but to the serendipitous formation of the polymeric complex (I), [Ni2(CN)4(C10H8N2)]n, the crystal structure of which is reported here.

Structural commentary top

The asymmetric unit of the structure of (I) contains formally one half of an [Ni(CN)4]2- (Ni1) anion, and one half of an [Ni(2,2'-bpy)]2+ (Ni2) cation (2,2'-bpy is 2,2'-bi­pyridine). The anion is completed by inversion symmetry, whereas the cation is completed by a twofold rotation axis (Fig. 1). The Ni1 atom shows a slightly distorted square-planar geometry through coordination by four C atoms (C6 and C6i, C7 and C7i) [symmetry code: (i)x + 2, -y, -z + 1] from four cyanide groups, bridging Ni1 to four adjacent Ni2 atoms. The latter exhibits an overall distorted o­cta­hedral environment, being defined by four N atoms (N3, N3ii, N2ii, N2iii) [symmetry codes: (ii) -x + 1, y, -z + 3/2; (iii) x - 1, y, z] from four [Ni(CN)4]2- groups, and two N atoms (N1 and N1ii) of one 2,2'-bpy ligand. The corresponding N1—Ni2—N1 bite angle is 77.32 (13)°. Relevant bond lengths involving the two metal cations are compiled in Table 1. As depicted in Fig. 2, the cyanide groups bridge nickel cations, forming undulating sheets of composition [Ni4(CN)4(bpy)2] parallel to (010), constituted by alternation of Ni1 and Ni2 ions.

Supra­molecular features top

Within a sheet, ππ inter­actions between pyridine rings with a centroid-to-centroid distance of 3.687 (3) Å are present. The adhesion of the sheets in the crystal packing is dominated by van der Waals forces. However, a weak non-classical C—H···N inter­action (Table 2) between neighbouring sheets may participate in the stabilization of the crystal packing.

Synthesis and crystallization top

Ni(acetate)2 (0.159 g, 0.64 mmol), 2,2'-bi­pyridine (0.047 g, 0.3 mmol) and K3[Fe(CN)6] (0.21 g, 0.64 mmol) dissolved in aqueous solution of 1M NaCl (8 ml) were added to a 15 ml Teflon-lined autoclave and heated at 433 K for 3 d. The autoclave was then cooled to room temperature. Green block-shaped crystals of (I) deposited on the wall of the container and were collected and air-dried.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 3. Hydrogen atoms bound to carbon were found in a difference map and were refined with Uiso(H) = 1.2Ueq(C).

Related literature top

For related literature, see: Colacio et al. (2003); Cui et al. (2011); Janiak (2003); Kong et al. (2008); Kopotkov et al. (2014); Li et al. (2008); Shen et al. (2014); Zhang & Lachgar (2015).

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The principal building units of complex (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity. For symmetry codes, see text.
[Figure 2] Fig. 2. A view of the polymeric sheet of complex (I). Ni atoms are represented by hatched green spheres, C atoms are grey, N atoms blue and H atoms green.
Poly[(2,2'-bipyridine-κ2N,N')tetrakis(µ-cyanido-κ2N:C)dinickel(II)] top
Crystal data top
[Ni2(CN)4(C10H8N2)]F(000) = 760
Mr = 377.68Dx = 1.918 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 3858 reflections
a = 6.519 (5) Åθ = 1.0–25.0°
b = 16.698 (5) ŵ = 2.88 mm1
c = 12.019 (5) ÅT = 293 K
β = 90.852 (5)°Block, green
V = 1308.2 (12) Å30.40 × 0.10 × 0.06 mm
Z = 4
Data collection top
Siemens SMART CCD
diffractometer
1039 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.032
Graphite monochromatorθmax = 25.0°, θmin = 3.4°
Detector resolution: 9 pixels mm-1h = 77
ω scansk = 1916
3858 measured reflectionsl = 1410
1156 independent reflections
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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H atoms treated by a mixture of independent and constrained refinement
S = 1.10 w = 1/[σ2(Fo2) + (0.0374P)2 + 0.9543P]
where P = (Fo2 + 2Fc2)/3
1156 reflections(Δ/σ)max < 0.001
118 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.40 e Å3
Crystal data top
[Ni2(CN)4(C10H8N2)]V = 1308.2 (12) Å3
Mr = 377.68Z = 4
Monoclinic, C2/cMo Kα radiation
a = 6.519 (5) ŵ = 2.88 mm1
b = 16.698 (5) ÅT = 293 K
c = 12.019 (5) Å0.40 × 0.10 × 0.06 mm
β = 90.852 (5)°
Data collection top
Siemens SMART CCD
diffractometer
1039 reflections with I > 2σ(I)
3858 measured reflectionsRint = 0.032
1156 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.074H atoms treated by a mixture of independent and constrained refinement
S = 1.10Δρmax = 0.71 e Å3
1156 reflectionsΔρmin = 0.40 e Å3
118 parameters
Special details top

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.

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 > σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni11.00000.00000.50000.01983 (19)
Ni20.50000.12867 (3)0.75000.01682 (18)
C60.8027 (4)0.02639 (16)0.6043 (2)0.0207 (6)
C10.8426 (4)0.22353 (19)0.6347 (3)0.0275 (7)
N30.6828 (3)0.04836 (14)0.6654 (2)0.0242 (5)
N10.6675 (3)0.22697 (13)0.6906 (2)0.0198 (5)
C50.5950 (4)0.29952 (16)0.7170 (2)0.0207 (6)
C71.1817 (4)0.07283 (17)0.5669 (2)0.0220 (6)
C40.6937 (5)0.36889 (18)0.6855 (3)0.0305 (7)
N21.2931 (3)0.11329 (14)0.6143 (2)0.0240 (5)
C30.8723 (5)0.3640 (2)0.6262 (3)0.0343 (8)
C20.9471 (5)0.29004 (19)0.6008 (3)0.0317 (7)
H21.062 (5)0.284 (2)0.562 (3)0.043 (10)*
H40.636 (4)0.4223 (19)0.711 (3)0.031 (8)*
H10.892 (5)0.171 (2)0.616 (3)0.033 (9)*
H30.940 (5)0.409 (2)0.608 (3)0.038 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0146 (3)0.0249 (3)0.0202 (3)0.00164 (17)0.0062 (2)0.0069 (2)
Ni20.0146 (3)0.0183 (3)0.0177 (3)0.0000.0058 (2)0.000
C60.0184 (13)0.0189 (14)0.0248 (16)0.0028 (11)0.0033 (12)0.0031 (12)
C10.0244 (15)0.0288 (17)0.0297 (18)0.0016 (12)0.0091 (13)0.0005 (13)
N30.0212 (12)0.0240 (13)0.0275 (15)0.0002 (9)0.0066 (11)0.0042 (11)
N10.0186 (11)0.0217 (12)0.0192 (13)0.0020 (9)0.0026 (9)0.0021 (10)
C50.0217 (14)0.0197 (15)0.0208 (16)0.0016 (10)0.0013 (12)0.0022 (11)
C70.0176 (13)0.0254 (15)0.0233 (16)0.0018 (11)0.0084 (12)0.0024 (12)
C40.0314 (17)0.0264 (17)0.034 (2)0.0035 (12)0.0005 (14)0.0030 (13)
N20.0187 (12)0.0289 (13)0.0245 (15)0.0021 (10)0.0054 (10)0.0033 (11)
C30.0331 (18)0.0323 (19)0.037 (2)0.0125 (14)0.0004 (15)0.0098 (15)
C20.0241 (16)0.0390 (19)0.0323 (19)0.0083 (13)0.0084 (14)0.0054 (15)
Geometric parameters (Å, º) top
Ni1—C6i1.863 (3)C1—C21.368 (4)
Ni1—C61.863 (3)C1—H10.95 (3)
Ni1—C7i1.871 (3)N1—C51.340 (3)
Ni1—C71.871 (3)C5—C41.381 (4)
Ni2—N3ii2.071 (2)C5—C5ii1.480 (5)
Ni2—N32.071 (2)C7—N21.139 (4)
Ni2—N12.102 (2)C4—C31.377 (5)
Ni2—N1ii2.102 (2)C4—H41.02 (3)
Ni2—N2iii2.116 (2)N2—Ni2v2.116 (2)
Ni2—N2iv2.116 (2)C3—C21.364 (5)
C6—N31.140 (4)C3—H30.90 (4)
C1—N11.335 (4)C2—H20.89 (4)
C6i—Ni1—C6180.0N1—C1—C2123.3 (3)
C6i—Ni1—C7i89.76 (12)N1—C1—H1117 (2)
C6—Ni1—C7i90.24 (12)C2—C1—H1120 (2)
C6i—Ni1—C790.24 (12)C6—N3—Ni2158.3 (2)
C6—Ni1—C789.76 (12)C1—N1—C5117.7 (2)
C7i—Ni1—C7180.00 (13)C1—N1—Ni2126.15 (19)
N3ii—Ni2—N399.29 (14)C5—N1—Ni2116.02 (18)
N3ii—Ni2—N1167.94 (10)N1—C5—C4121.7 (3)
N3—Ni2—N191.91 (10)N1—C5—C5ii115.32 (15)
N3ii—Ni2—N1ii91.91 (10)C4—C5—C5ii122.95 (18)
N3—Ni2—N1ii167.94 (10)N2—C7—Ni1174.8 (3)
N1—Ni2—N1ii77.32 (13)C3—C4—C5119.6 (3)
N3ii—Ni2—N2iii86.28 (10)C3—C4—H4122.1 (18)
N3—Ni2—N2iii84.71 (10)C5—C4—H4118.2 (18)
N1—Ni2—N2iii99.29 (9)C7—N2—Ni2v148.4 (2)
N1ii—Ni2—N2iii91.61 (9)C2—C3—C4118.5 (3)
N3ii—Ni2—N2iv84.71 (10)C2—C3—H3122 (2)
N3—Ni2—N2iv86.28 (10)C4—C3—H3120 (2)
N1—Ni2—N2iv91.61 (9)C3—C2—C1119.1 (3)
N1ii—Ni2—N2iv99.29 (9)C3—C2—H2122 (2)
N2iii—Ni2—N2iv166.06 (13)C1—C2—H2119 (2)
N3—C6—Ni1174.8 (2)
N3ii—Ni2—N3—C6173.2 (7)N3—Ni2—N1—C5174.8 (2)
N1—Ni2—N3—C611.3 (6)N1ii—Ni2—N1—C50.33 (14)
N1ii—Ni2—N3—C615.2 (9)N2iii—Ni2—N1—C589.9 (2)
N2iii—Ni2—N3—C687.8 (6)N2iv—Ni2—N1—C598.8 (2)
N2iv—Ni2—N3—C6102.8 (6)C1—N1—C5—C41.7 (4)
C2—C1—N1—C51.9 (5)Ni2—N1—C5—C4178.3 (2)
C2—C1—N1—Ni2178.2 (2)C1—N1—C5—C5ii177.6 (3)
N3ii—Ni2—N1—C1149.5 (4)Ni2—N1—C5—C5ii0.9 (4)
N3—Ni2—N1—C18.8 (2)N1—C5—C4—C30.6 (5)
N1ii—Ni2—N1—C1176.7 (3)C5ii—C5—C4—C3178.6 (3)
N2iii—Ni2—N1—C193.7 (2)C5—C4—C3—C20.3 (5)
N2iv—Ni2—N1—C177.5 (2)C4—C3—C2—C10.1 (5)
N3ii—Ni2—N1—C526.9 (5)N1—C1—C2—C31.0 (5)
Symmetry codes: (i) x+2, y, z+1; (ii) x+1, y, z+3/2; (iii) x1, y, z; (iv) x+2, y, z+3/2; (v) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···N30.96 (3)2.54 (3)3.129 (3)120 (2)
Selected bond lengths (Å) top
Ni1—C61.863 (3)Ni2—N12.102 (2)
Ni1—C71.871 (3)Ni2—N2i2.116 (2)
Ni2—N32.071 (2)
Symmetry code: (i) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···N30.96 (3)2.54 (3)3.129 (3)120 (2)

Experimental details

Crystal data
Chemical formula[Ni2(CN)4(C10H8N2)]
Mr377.68
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)6.519 (5), 16.698 (5), 12.019 (5)
β (°) 90.852 (5)
V3)1308.2 (12)
Z4
Radiation typeMo Kα
µ (mm1)2.88
Crystal size (mm)0.40 × 0.10 × 0.06
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
3858, 1156, 1039
Rint0.032
(sin θ/λ)max1)0.594
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.074, 1.10
No. of reflections1156
No. of parameters118
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.71, 0.40

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

 

Acknowledgements

This research was supported by the Natural Science Foundation of Heilongjiang Province (QC2014C009).

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Volume 71| Part 6| June 2015| Pages 709-711
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