Tetra-kis(pyridazine-κN)bis-(thio-cyanato-κN)nickel(II) pyridazine disolvate.

The reaction of nickel(II) thio-cyanate with an excess of pyridazine leads to single crystals of the title compound, [Ni(NCS)(2)(C(4)H(4)N(2))(4)]·2C(4)H(4)N(2). The Ni(II) cations are coordinated by two terminal N-bonded thio-cyanate anions (trans) and four pyridazine ligands in a slightly distorted octa-hedral geometry. The discrete complexes are arranged into layers parallel to the ab plane which are separated by additional non-coordinated pyridazine ligands.

Related literature

For related pyridazine coordination compounds, see: Boeckmann et al. (2011 ▶); Lloret et al. (1998 ▶); Yi et al. (2006 ▶); Wriedt & Näther (2009 ▶, 2011 ▶).

Experimental

Crystal data

[Ni(NCS)2(C4H4N2)4]·2C4H4N2

M = 655.42

Triclinic,

a = 11.2111 (9) Å

b = 12.033 (1) Å

c = 12.5409 (10) Å

α = 62.287 (9)°

β = 88.983 (10)°

γ = 88.949 (10)°

V = 1497.4 (2) Å3

Z = 2

Mo Kα radiation

μ = 0.83 mm−1

T = 200 K

0.06 × 0.04 × 0.03 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.916, T max = 0.973

11937 measured reflections

6400 independent reflections

4719 reflections with I > 2σ(I)

R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.084

S = 0.97

6400 reflections

389 parameters

H-atom parameters constrained

Δρmax = 0.39 e Å−3

Δρmin = −0.40 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 and PLATON (Spek, 2009 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812023306/bt5930sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812023306/bt5930Isup2.hkl

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

[Ni(NCS)2(C4H4N2)4]·2C4H4N2	Z = 2
Mr = 655.42	F(000) = 676
Triclinic, P1	Dx = 1.454 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.2111 (9) Å	Cell parameters from 11937 reflections
b = 12.033 (1) Å	θ = 2.6–27.0°
c = 12.5409 (10) Å	µ = 0.83 mm−1
α = 62.287 (9)°	T = 200 K
β = 88.983 (10)°	Block, light-green
γ = 88.949 (10)°	0.06 × 0.04 × 0.03 mm
V = 1497.4 (2) Å3

Stoe IPDS-1 diffractometer	6400 independent reflections
Radiation source: fine-focus sealed tube	4719 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
phi scan	θmax = 27.0°, θmin = 2.6°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −14→14
Tmin = 0.916, Tmax = 0.973	k = −15→15
11937 measured reflections	l = −16→16

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)] = 0.032	H-atom parameters constrained
wR(F2) = 0.084	w = 1/[σ2(Fo2) + (0.0504P)2] where P = (Fo2 + 2Fc2)/3
S = 0.97	(Δ/σ)max = 0.001
6400 reflections	Δρmax = 0.39 e Å−3
389 parameters	Δρmin = −0.40 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: 0.0149 (15)

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	0.752765 (19)	0.75179 (2)	0.993234 (18)	0.01640 (8)
N2	0.85894 (13)	0.65700 (14)	1.14111 (13)	0.0237 (3)
C2	0.93634 (15)	0.60587 (16)	1.20694 (14)	0.0195 (3)
S2	1.04648 (4)	0.53396 (5)	1.29882 (4)	0.03462 (13)
N1	0.64734 (13)	0.84717 (14)	0.84542 (13)	0.0241 (3)
C1	0.56476 (16)	0.89404 (16)	0.78585 (14)	0.0204 (4)
S1	0.44826 (5)	0.95934 (5)	0.70169 (5)	0.03734 (14)
N10	0.69744 (12)	0.57958 (14)	0.99727 (12)	0.0212 (3)
N11	0.65668 (14)	0.48848 (14)	1.10237 (14)	0.0281 (3)
C11	0.62296 (18)	0.38099 (18)	1.10720 (19)	0.0332 (4)
H11	0.5923	0.3180	1.1815	0.040*
C12	0.62968 (18)	0.3551 (2)	1.0107 (2)	0.0365 (5)
H12	0.6056	0.2765	1.0180	0.044*
C13	0.67269 (19)	0.4479 (2)	0.9041 (2)	0.0398 (5)
H13	0.6806	0.4359	0.8346	0.048*
C14	0.70445 (17)	0.5607 (2)	0.90134 (17)	0.0301 (4)
H14	0.7323	0.6269	0.8275	0.036*
N20	0.61071 (12)	0.74611 (13)	1.11065 (12)	0.0185 (3)
N21	0.54160 (13)	0.85064 (14)	1.06923 (12)	0.0221 (3)
C21	0.45590 (16)	0.85656 (18)	1.14045 (16)	0.0267 (4)
H21	0.4084	0.9309	1.1115	0.032*
C22	0.43142 (18)	0.7605 (2)	1.25495 (17)	0.0329 (5)
H22	0.3682	0.7680	1.3027	0.039*
C23	0.50158 (17)	0.65455 (18)	1.29662 (16)	0.0287 (4)
H23	0.4887	0.5855	1.3740	0.034*
C24	0.59298 (16)	0.65231 (16)	1.22036 (14)	0.0223 (4)
H24	0.6444	0.5809	1.2481	0.027*
N30	0.80605 (12)	0.92471 (14)	0.98921 (13)	0.0210 (3)
N31	0.83861 (14)	1.02153 (14)	0.88415 (14)	0.0278 (3)
C31	0.86974 (18)	1.12832 (19)	0.88297 (19)	0.0336 (4)
H31	0.8940	1.1960	0.8084	0.040*
C32	0.86879 (19)	1.1465 (2)	0.9847 (2)	0.0382 (5)
H32	0.8915	1.2242	0.9804	0.046*
C33	0.83376 (19)	1.0480 (2)	1.0911 (2)	0.0387 (5)
H33	0.8298	1.0549	1.1635	0.046*
C34	0.80415 (17)	0.93705 (19)	1.08911 (17)	0.0290 (4)
H34	0.7815	0.8669	1.1627	0.035*
N40	0.89770 (12)	0.75517 (13)	0.87968 (12)	0.0192 (3)
N41	0.96253 (13)	0.64770 (14)	0.92420 (12)	0.0228 (3)
C41	1.05424 (16)	0.64035 (18)	0.85962 (16)	0.0266 (4)
H41	1.0987	0.5640	0.8902	0.032*
C42	1.08890 (17)	0.7384 (2)	0.74940 (17)	0.0316 (4)
H42	1.1567	0.7303	0.7069	0.038*
C43	1.02254 (18)	0.84661 (19)	0.70416 (16)	0.0298 (4)
H43	1.0420	0.9163	0.6291	0.036*
C44	0.92462 (16)	0.85029 (17)	0.77327 (15)	0.0236 (4)
H44	0.8756	0.9236	0.7429	0.028*
N50	0.70575 (16)	1.39686 (16)	0.45667 (15)	0.0364 (4)
N51	0.61715 (16)	1.33478 (17)	0.43752 (15)	0.0374 (4)
C51	0.6319 (2)	1.2132 (2)	0.47219 (19)	0.0387 (5)
H51	0.5686	1.1701	0.4587	0.046*
C52	0.7336 (2)	1.1454 (2)	0.5268 (2)	0.0403 (5)
H52	0.7403	1.0583	0.5501	0.048*
C53	0.82377 (19)	1.2079 (2)	0.54582 (19)	0.0371 (5)
H53	0.8959	1.1666	0.5831	0.044*
C54	0.80526 (19)	1.3355 (2)	0.50801 (18)	0.0339 (5)
H54	0.8675	1.3812	0.5197	0.041*
N60	1.18977 (17)	1.12073 (18)	0.50816 (18)	0.0425 (4)
N61	1.12255 (18)	1.1575 (2)	0.57472 (19)	0.0497 (5)
C61	1.1514 (3)	1.2601 (3)	0.5806 (2)	0.0525 (7)
H61	1.1019	1.2854	0.6279	0.063*
C62	1.2485 (3)	1.3331 (2)	0.5228 (3)	0.0559 (7)
H62	1.2665	1.4061	0.5301	0.067*
C63	1.3172 (2)	1.2955 (2)	0.4547 (3)	0.0535 (7)
H63	1.3855	1.3411	0.4120	0.064*
C64	1.2832 (2)	1.1884 (2)	0.4506 (2)	0.0444 (6)
H64	1.3301	1.1613	0.4030	0.053*

	U11	U22	U33	U12	U13	U23
Ni1	0.01669 (12)	0.01298 (12)	0.01687 (12)	0.00196 (7)	0.00033 (7)	−0.00480 (8)
N2	0.0236 (7)	0.0211 (8)	0.0227 (7)	0.0033 (6)	−0.0016 (6)	−0.0072 (6)
C2	0.0225 (8)	0.0150 (8)	0.0199 (7)	−0.0005 (7)	0.0014 (7)	−0.0073 (7)
S2	0.0301 (3)	0.0309 (3)	0.0348 (3)	0.0052 (2)	−0.0147 (2)	−0.0082 (2)
N1	0.0249 (8)	0.0231 (8)	0.0215 (7)	0.0036 (6)	−0.0018 (6)	−0.0081 (6)
C1	0.0262 (9)	0.0146 (8)	0.0191 (7)	−0.0016 (7)	0.0019 (7)	−0.0068 (7)
S1	0.0335 (3)	0.0295 (3)	0.0393 (3)	0.0034 (2)	−0.0174 (2)	−0.0074 (2)
N10	0.0193 (7)	0.0183 (8)	0.0248 (7)	−0.0001 (6)	0.0008 (6)	−0.0090 (6)
N11	0.0330 (8)	0.0186 (8)	0.0301 (8)	−0.0047 (7)	0.0069 (7)	−0.0091 (7)
C11	0.0324 (10)	0.0206 (10)	0.0431 (11)	−0.0054 (8)	0.0038 (9)	−0.0118 (9)
C12	0.0315 (10)	0.0283 (11)	0.0568 (13)	−0.0053 (8)	−0.0018 (9)	−0.0256 (10)
C13	0.0416 (12)	0.0464 (14)	0.0484 (12)	−0.0086 (10)	−0.0005 (10)	−0.0361 (11)
C14	0.0308 (10)	0.0336 (11)	0.0295 (9)	−0.0064 (8)	0.0011 (8)	−0.0175 (8)
N20	0.0192 (7)	0.0154 (7)	0.0195 (6)	0.0027 (6)	0.0004 (5)	−0.0070 (6)
N21	0.0226 (7)	0.0183 (8)	0.0222 (7)	0.0053 (6)	0.0007 (6)	−0.0070 (6)
C21	0.0270 (9)	0.0252 (10)	0.0286 (9)	0.0076 (8)	0.0008 (7)	−0.0136 (8)
C22	0.0325 (10)	0.0377 (12)	0.0293 (9)	0.0027 (9)	0.0093 (8)	−0.0168 (9)
C23	0.0337 (10)	0.0272 (10)	0.0204 (8)	0.0000 (8)	0.0055 (7)	−0.0071 (8)
C24	0.0260 (9)	0.0181 (9)	0.0203 (8)	0.0013 (7)	0.0006 (7)	−0.0068 (7)
N30	0.0185 (7)	0.0172 (7)	0.0260 (7)	0.0019 (6)	−0.0016 (6)	−0.0089 (6)
N31	0.0319 (8)	0.0174 (8)	0.0314 (8)	−0.0033 (6)	0.0060 (7)	−0.0093 (7)
C31	0.0341 (10)	0.0224 (10)	0.0412 (11)	−0.0069 (8)	0.0062 (9)	−0.0123 (9)
C32	0.0348 (11)	0.0295 (11)	0.0588 (13)	−0.0059 (9)	−0.0007 (10)	−0.0275 (11)
C33	0.0408 (12)	0.0428 (13)	0.0445 (11)	−0.0090 (10)	−0.0011 (9)	−0.0302 (11)
C34	0.0325 (10)	0.0276 (10)	0.0281 (9)	−0.0054 (8)	−0.0010 (8)	−0.0138 (8)
N40	0.0194 (7)	0.0157 (7)	0.0205 (6)	0.0001 (6)	0.0011 (5)	−0.0068 (6)
N41	0.0234 (7)	0.0181 (8)	0.0240 (7)	0.0045 (6)	0.0023 (6)	−0.0075 (6)
C41	0.0260 (9)	0.0260 (10)	0.0278 (9)	0.0054 (8)	0.0025 (7)	−0.0127 (8)
C42	0.0292 (10)	0.0374 (12)	0.0289 (9)	0.0002 (8)	0.0104 (8)	−0.0164 (9)
C43	0.0363 (10)	0.0280 (10)	0.0205 (8)	−0.0062 (8)	0.0080 (7)	−0.0076 (8)
C44	0.0311 (9)	0.0159 (9)	0.0200 (8)	0.0015 (7)	0.0013 (7)	−0.0053 (7)
N50	0.0455 (10)	0.0223 (9)	0.0359 (9)	−0.0048 (8)	−0.0030 (8)	−0.0086 (7)
N51	0.0394 (10)	0.0320 (10)	0.0333 (9)	−0.0052 (8)	−0.0048 (7)	−0.0086 (8)
C51	0.0455 (13)	0.0367 (12)	0.0370 (10)	−0.0160 (10)	0.0042 (9)	−0.0192 (10)
C52	0.0516 (14)	0.0242 (11)	0.0462 (12)	−0.0015 (10)	0.0107 (10)	−0.0176 (10)
C53	0.0339 (11)	0.0377 (12)	0.0352 (10)	0.0051 (9)	0.0074 (8)	−0.0137 (9)
C54	0.0351 (11)	0.0321 (11)	0.0322 (10)	−0.0095 (9)	0.0004 (8)	−0.0127 (9)
N60	0.0403 (10)	0.0337 (10)	0.0583 (12)	−0.0004 (8)	−0.0048 (9)	−0.0254 (9)
N61	0.0437 (11)	0.0400 (12)	0.0573 (12)	0.0049 (9)	0.0056 (9)	−0.0163 (10)
C61	0.0640 (17)	0.0532 (16)	0.0474 (13)	0.0264 (14)	−0.0112 (12)	−0.0299 (13)
C62	0.0652 (17)	0.0297 (13)	0.0843 (19)	0.0167 (12)	−0.0445 (15)	−0.0353 (14)
C63	0.0351 (12)	0.0342 (13)	0.0771 (18)	−0.0056 (10)	−0.0074 (12)	−0.0136 (13)
C64	0.0445 (13)	0.0424 (14)	0.0494 (13)	0.0022 (11)	0.0042 (10)	−0.0242 (11)

Ni1—N1	2.0494 (15)	C32—C33	1.366 (3)
Ni1—N2	2.0538 (15)	C32—H32	0.9500
Ni1—N40	2.1298 (13)	C33—C34	1.393 (3)
Ni1—N20	2.1299 (13)	C33—H33	0.9500
Ni1—N10	2.1516 (15)	C34—H34	0.9500
Ni1—N30	2.1530 (15)	N40—C44	1.327 (2)
N2—C2	1.160 (2)	N40—N41	1.3494 (19)
C2—S2	1.6387 (18)	N41—C41	1.325 (2)
N1—C1	1.161 (2)	C41—C42	1.391 (3)
C1—S1	1.6362 (18)	C41—H41	0.9500
N10—C14	1.325 (2)	C42—C43	1.365 (3)
N10—N11	1.342 (2)	C42—H42	0.9500
N11—C11	1.328 (3)	C43—C44	1.399 (2)
C11—C12	1.384 (3)	C43—H43	0.9500
C11—H11	0.9500	C44—H44	0.9500
C12—C13	1.369 (3)	N50—C54	1.326 (3)
C12—H12	0.9500	N50—N51	1.343 (3)
C13—C14	1.394 (3)	N51—C51	1.326 (3)
C13—H13	0.9500	C51—C52	1.382 (3)
C14—H14	0.9500	C51—H51	0.9500
N20—C24	1.327 (2)	C52—C53	1.360 (3)
N20—N21	1.3502 (19)	C52—H52	0.9500
N21—C21	1.324 (2)	C53—C54	1.393 (3)
C21—C22	1.388 (3)	C53—H53	0.9500
C21—H21	0.9500	C54—H54	0.9500
C22—C23	1.370 (3)	N60—C64	1.318 (3)
C22—H22	0.9500	N60—N61	1.331 (3)
C23—C24	1.398 (2)	N61—C61	1.316 (3)
C23—H23	0.9500	C61—C62	1.378 (4)
C24—H24	0.9500	C61—H61	0.9500
N30—C34	1.328 (2)	C62—C63	1.360 (4)
N30—N31	1.341 (2)	C62—H62	0.9500
N31—C31	1.331 (3)	C63—C64	1.375 (4)
C31—C32	1.391 (3)	C63—H63	0.9500
C31—H31	0.9500	C64—H64	0.9500
N1—Ni1—N2	179.71 (7)	N31—C31—H31	118.1
N1—Ni1—N40	90.25 (6)	C32—C31—H31	118.1
N2—Ni1—N40	89.64 (6)	C33—C32—C31	117.2 (2)
N1—Ni1—N20	91.20 (6)	C33—C32—H32	121.4
N2—Ni1—N20	88.90 (6)	C31—C32—H32	121.4
N40—Ni1—N20	178.54 (6)	C32—C33—C34	117.37 (19)
N1—Ni1—N10	88.37 (6)	C32—C33—H33	121.3
N2—Ni1—N10	91.90 (6)	C34—C33—H33	121.3
N40—Ni1—N10	87.95 (5)	N30—C34—C33	123.06 (18)
N20—Ni1—N10	92.16 (5)	N30—C34—H34	118.5
N1—Ni1—N30	91.25 (6)	C33—C34—H34	118.5
N2—Ni1—N30	88.48 (6)	C44—N40—N41	120.64 (14)
N40—Ni1—N30	92.57 (5)	C44—N40—Ni1	125.54 (12)
N20—Ni1—N30	87.33 (5)	N41—N40—Ni1	113.81 (10)
N10—Ni1—N30	179.36 (5)	C41—N41—N40	118.32 (14)
C2—N2—Ni1	165.91 (13)	N41—C41—C42	123.54 (17)
N2—C2—S2	179.46 (15)	N41—C41—H41	118.2
C1—N1—Ni1	161.54 (13)	C42—C41—H41	118.2
N1—C1—S1	179.63 (17)	C43—C42—C41	117.98 (16)
C14—N10—N11	119.91 (16)	C43—C42—H42	121.0
C14—N10—Ni1	122.41 (13)	C41—C42—H42	121.0
N11—N10—Ni1	117.67 (11)	C42—C43—C44	117.04 (16)
C11—N11—N10	118.70 (15)	C42—C43—H43	121.5
N11—C11—C12	124.07 (19)	C44—C43—H43	121.5
N11—C11—H11	118.0	N40—C44—C43	122.43 (16)
C12—C11—H11	118.0	N40—C44—H44	118.8
C13—C12—C11	116.88 (19)	C43—C44—H44	118.8
C13—C12—H12	121.6	C54—N50—N51	119.27 (18)
C11—C12—H12	121.6	C51—N51—N50	118.58 (19)
C12—C13—C14	117.59 (18)	N51—C51—C52	124.1 (2)
C12—C13—H13	121.2	N51—C51—H51	117.9
C14—C13—H13	121.2	C52—C51—H51	117.9
N10—C14—C13	122.82 (18)	C53—C52—C51	117.5 (2)
N10—C14—H14	118.6	C53—C52—H52	121.2
C13—C14—H14	118.6	C51—C52—H52	121.2
C24—N20—N21	120.47 (13)	C52—C53—C54	116.8 (2)
C24—N20—Ni1	124.29 (11)	C52—C53—H53	121.6
N21—N20—Ni1	115.09 (10)	C54—C53—H53	121.6
C21—N21—N20	118.35 (14)	N50—C54—C53	123.7 (2)
N21—C21—C22	123.81 (17)	N50—C54—H54	118.1
N21—C21—H21	118.1	C53—C54—H54	118.1
C22—C21—H21	118.1	C64—N60—N61	118.7 (2)
C23—C22—C21	117.67 (16)	C61—N61—N60	119.0 (2)
C23—C22—H22	121.2	N61—C61—C62	124.4 (2)
C21—C22—H22	121.2	N61—C61—H61	117.8
C22—C23—C24	117.13 (17)	C62—C61—H61	117.8
C22—C23—H23	121.4	C63—C62—C61	116.7 (2)
C24—C23—H23	121.4	C63—C62—H62	121.7
N20—C24—C23	122.52 (16)	C61—C62—H62	121.7
N20—C24—H24	118.7	C62—C63—C64	116.9 (2)
C23—C24—H24	118.7	C62—C63—H63	121.6
C34—N30—N31	119.93 (16)	C64—C63—H63	121.6
C34—N30—Ni1	120.60 (12)	N60—C64—C63	124.4 (2)
N31—N30—Ni1	119.45 (11)	N60—C64—H64	117.8
C31—N31—N30	118.68 (16)	C63—C64—H64	117.8
N31—C31—C32	123.75 (19)