Bis(dicyanamido-κN)tetra-kis-(pyridazine-κN)nickel(II).

Reaction of nickel(II) chloride with sodium dicyanamide and pyridazine leads to single crystals of the title compound, [Ni{N(CN)(2)}(2)(C(4)H(4)N(2))(4)], in which the Ni(II) cation is octa-hedrally coordinated by two dicyanamide anions and four pyridazine ligands into a discrete complex that is located on a center of inversion.

Related literature

For the synthesis, structures and properties of dicyanamide coordination compounds, see: Wriedt & Näther (2011 ▶).

Experimental

Crystal data

[Ni(C2N3)2(C4H4N2)4]

M = 511.18

Triclinic,

a = 8.1796 (12) Å

b = 8.4125 (12) Å

c = 8.9643 (11) Å

α = 81.364 (16)°

β = 66.027 (15)°

γ = 84.879 (17)°

V = 556.97 (13) Å3

Z = 1

Mo Kα radiation

μ = 0.91 mm−1

T = 170 K

0.10 × 0.08 × 0.06 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.783, T max = 0.927

4159 measured reflections

2142 independent reflections

1582 reflections with I > 2σ(I)

R int = 0.068

Refinement

R[F 2 > 2σ(F 2)] = 0.048

wR(F 2) = 0.097

S = 1.01

2142 reflections

161 parameters

H-atom parameters constrained

Δρmax = 0.51 e Å−3

Δρmin = −0.52 e Å−3

Data collection: X-AREA (Stoe & Cie, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; 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 ▶) and DIAMOND (Brandenburg, 2011 ▶).; software used to prepare material for publication: XCIF in SHELXTL.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812018363/bt5900sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812018363/bt5900Isup2.hkl

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

[Ni(C2N3)2(C4H4N2)4]	Z = 1
Mr = 511.18	F(000) = 262
Triclinic, P1	Dx = 1.524 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.1796 (12) Å	Cell parameters from 4159 reflections
b = 8.4125 (12) Å	θ = 2.5–26.0°
c = 8.9643 (11) Å	µ = 0.91 mm−1
α = 81.364 (16)°	T = 170 K
β = 66.027 (15)°	Block, green
γ = 84.879 (17)°	0.10 × 0.08 × 0.06 mm
V = 556.97 (13) Å3

Stoe IPDS-1 diffractometer	2142 independent reflections
Radiation source: fine-focus sealed tube	1582 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.068
phi scan	θmax = 26.0°, θmin = 2.5°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −10→10
Tmin = 0.783, Tmax = 0.927	k = −10→10
4159 measured reflections	l = −11→11

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.048	H-atom parameters constrained
wR(F2) = 0.097	w = 1/[σ2(Fo2) + (0.0348P)2] where P = (Fo2 + 2Fc2)/3
S = 1.01	(Δ/σ)max < 0.001
2142 reflections	Δρmax = 0.51 e Å−3
161 parameters	Δρmin = −0.52 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.025 (4)

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.

	x	y	z	Uiso*/Ueq
Ni1	0.0000	0.5000	0.5000	0.0161 (2)
N1	0.1088 (4)	0.7246 (3)	0.4952 (4)	0.0190 (6)
N2	0.0726 (4)	0.7802 (4)	0.6384 (4)	0.0249 (7)
C1	0.1491 (5)	0.9151 (5)	0.6353 (5)	0.0295 (9)
H1	0.1204	0.9557	0.7366	0.035*
C2	0.2687 (6)	0.9998 (5)	0.4919 (6)	0.0336 (10)
H2	0.3228	1.0941	0.4945	0.040*
C3	0.3045 (6)	0.9406 (5)	0.3470 (5)	0.0333 (9)
H3	0.3853	0.9920	0.2449	0.040*
C4	0.2185 (5)	0.8030 (4)	0.3549 (5)	0.0254 (8)
H4	0.2391	0.7628	0.2550	0.031*
N11	0.2622 (4)	0.4283 (3)	0.3430 (4)	0.0184 (6)
N12	0.3917 (4)	0.4485 (4)	0.3946 (4)	0.0250 (7)
C11	0.5593 (5)	0.4051 (5)	0.3036 (5)	0.0264 (8)
H11	0.6503	0.4227	0.3390	0.032*
C12	0.6091 (5)	0.3350 (5)	0.1588 (5)	0.0295 (9)
H12	0.7298	0.3030	0.0984	0.035*
C13	0.4777 (5)	0.3144 (4)	0.1079 (5)	0.0273 (8)
H13	0.5035	0.2669	0.0107	0.033*
C14	0.3019 (4)	0.3658 (4)	0.2037 (4)	0.0201 (7)
H14	0.2092	0.3556	0.1680	0.024*
N21	0.0470 (4)	0.4009 (4)	0.7037 (4)	0.0223 (7)
C21	0.0896 (5)	0.3404 (4)	0.8065 (5)	0.0263 (8)
N22	0.1310 (7)	0.2874 (5)	0.9320 (5)	0.0581 (13)
C22	0.1948 (5)	0.1418 (5)	0.9515 (5)	0.0300 (9)
N23	0.2467 (6)	0.0160 (5)	0.9879 (5)	0.0480 (10)

	U11	U22	U33	U12	U13	U23
Ni1	0.0151 (4)	0.0195 (4)	0.0144 (4)	−0.0010 (3)	−0.0066 (3)	−0.0020 (3)
N1	0.0177 (14)	0.0215 (15)	0.0193 (16)	0.0027 (12)	−0.0090 (12)	−0.0047 (12)
N2	0.0227 (16)	0.0314 (17)	0.0223 (17)	−0.0058 (13)	−0.0082 (13)	−0.0083 (13)
C1	0.032 (2)	0.029 (2)	0.033 (2)	0.0018 (17)	−0.0151 (18)	−0.0137 (17)
C2	0.037 (2)	0.0228 (19)	0.047 (3)	−0.0085 (17)	−0.021 (2)	−0.0029 (18)
C3	0.033 (2)	0.028 (2)	0.032 (2)	−0.0079 (17)	−0.0069 (18)	0.0039 (17)
C4	0.029 (2)	0.0245 (18)	0.021 (2)	−0.0027 (16)	−0.0087 (16)	0.0008 (15)
N11	0.0157 (15)	0.0224 (15)	0.0174 (16)	−0.0012 (12)	−0.0062 (12)	−0.0043 (12)
N12	0.0211 (16)	0.0290 (17)	0.0291 (18)	0.0023 (13)	−0.0131 (14)	−0.0083 (14)
C11	0.0145 (17)	0.032 (2)	0.033 (2)	−0.0030 (15)	−0.0085 (16)	−0.0050 (17)
C12	0.0207 (19)	0.030 (2)	0.031 (2)	0.0018 (16)	−0.0031 (16)	−0.0047 (17)
C13	0.0249 (19)	0.028 (2)	0.021 (2)	−0.0026 (16)	0.0003 (15)	−0.0065 (16)
C14	0.0172 (17)	0.0242 (18)	0.0162 (19)	−0.0016 (14)	−0.0036 (14)	−0.0025 (14)
N21	0.0219 (16)	0.0263 (16)	0.0191 (18)	−0.0035 (13)	−0.0079 (14)	−0.0034 (13)
C21	0.035 (2)	0.028 (2)	0.018 (2)	−0.0030 (16)	−0.0129 (17)	−0.0034 (15)
N22	0.113 (4)	0.037 (2)	0.053 (3)	0.007 (2)	−0.065 (3)	−0.0054 (19)
C22	0.037 (2)	0.035 (2)	0.024 (2)	−0.0021 (19)	−0.0190 (18)	−0.0022 (17)
N23	0.059 (3)	0.050 (2)	0.043 (2)	0.020 (2)	−0.030 (2)	−0.0134 (19)

Ni1—N21	2.058 (3)	C4—H4	0.9500
Ni1—N21i	2.058 (3)	N11—C14	1.333 (4)
Ni1—N11i	2.125 (3)	N11—N12	1.349 (4)
Ni1—N11	2.125 (3)	N12—C11	1.330 (5)
Ni1—N1i	2.147 (3)	C11—C12	1.399 (5)
Ni1—N1	2.147 (3)	C11—H11	0.9500
N1—C4	1.327 (5)	C12—C13	1.359 (5)
N1—N2	1.342 (4)	C12—H12	0.9500
N2—C1	1.336 (5)	C13—C14	1.410 (5)
C1—C2	1.394 (6)	C13—H13	0.9500
C1—H1	0.9500	C14—H14	0.9500
C2—C3	1.372 (6)	N21—C21	1.148 (5)
C2—H2	0.9500	C21—N22	1.308 (5)
C3—C4	1.385 (5)	N22—C22	1.304 (6)
C3—H3	0.9500	C22—N23	1.155 (6)
N21—Ni1—N21i	180.00 (8)	C2—C3—H3	121.2
N21—Ni1—N11i	89.44 (11)	C4—C3—H3	121.2
N21i—Ni1—N11i	90.56 (11)	N1—C4—C3	123.2 (3)
N21—Ni1—N11	90.56 (11)	N1—C4—H4	118.4
N21i—Ni1—N11	89.44 (11)	C3—C4—H4	118.4
N11i—Ni1—N11	180.0	C14—N11—N12	120.5 (3)
N21—Ni1—N1i	88.23 (11)	C14—N11—Ni1	124.5 (2)
N21i—Ni1—N1i	91.77 (11)	N12—N11—Ni1	115.0 (2)
N11i—Ni1—N1i	87.48 (11)	C11—N12—N11	118.6 (3)
N11—Ni1—N1i	92.52 (10)	N12—C11—C12	123.7 (3)
N21—Ni1—N1	91.77 (11)	N12—C11—H11	118.1
N21i—Ni1—N1	88.23 (11)	C12—C11—H11	118.1
N11i—Ni1—N1	92.52 (10)	C13—C12—C11	117.3 (3)
N11—Ni1—N1	87.48 (11)	C13—C12—H12	121.3
N1i—Ni1—N1	180.0	C11—C12—H12	121.3
C4—N1—N2	120.1 (3)	C12—C13—C14	117.9 (3)
C4—N1—Ni1	121.1 (2)	C12—C13—H13	121.0
N2—N1—Ni1	118.7 (2)	C14—C13—H13	121.0
C1—N2—N1	118.4 (3)	N11—C14—C13	121.9 (3)
N2—C1—C2	123.8 (3)	N11—C14—H14	119.1
N2—C1—H1	118.1	C13—C14—H14	119.1
C2—C1—H1	118.1	C21—N21—Ni1	173.1 (3)
C3—C2—C1	116.9 (3)	N21—C21—N22	173.1 (4)
C3—C2—H2	121.6	C22—N22—C21	122.1 (4)
C1—C2—H2	121.6	N23—C22—N22	171.8 (4)
C2—C3—C4	117.6 (4)