metal-organic compounds
Bis(dicyanamido-κN)tetrakis(pyridine-κN)nickel(II)
aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany, and bDepartement of Chemistry, Texas A&M University, College Station, Texas 77843, USA
*Correspondence e-mail: swoehlert@ac.uni-kiel.de
In the 2N3)2(C5H5N)4], the NiII cations are coordinated by four pyridine ligands and two dicyanamide anions into discrete complexes. The shortest Ni⋯Ni separation is 8.1068 (10) Å. The structure is pseudo-centrosymmetric and can also be refined in the C2/c in which both anionic ligands are strongly disordered and the leads to significantly poorer reliability factors.
of the title compound, [Ni(CRelated literature
For related structures, see: Boeckmann & Näther (2010, 2011); Wriedt & Näther (2011); Wu et al. (2004). For a description of the Cambridge Structural Database, see: Allen (2002).
Experimental
Crystal data
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Data collection: X-AREA (Stoe & Cie, 2008); cell 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.
Supporting information
10.1107/S1600536812019691/bt5887sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812019691/bt5887Isup2.hkl
Nickel(II) chloride hexahydrate (NiCl2x6H2O), sodium dicyanamide (NaN(CN)2) and pyridine were obtained from Alfa Aesar. All chemicals were used without further purification. 0.125 mmol (29.7 mg) NiCl2x6H2O, 0.25 mmol (22.3 mg) Na(N(CN)2) were reacted in 2.5 ml pyridine. Light-green single-crystal of the title compound were obtained after three days.
All H atoms were located in difference map but were positioned with idealized geometry and were refined isotropic with Ueq(H) = 1.2 Ueq(C) of the parent atom using a riding model with C—H = 0.95 Å. The structure is pseudo-centrosymmetric and can also be refined in the centrosymmetric
C2/c. However, in C2/c the complexes are located on centres of inversion and the anionic ligands are strongly disorderd which is not the case in Cc. Moreover, in C2/c the reliability factors are very poor and no reasonable structure model can be found. Therefore, Cc was selected, in which the structure can be very easily refined. In this case the cannot be determined presumable, because of the pseudo-symmetry and therefore, a twin for racemic was performed leading to an BASF parameter of 0.53 (2).Data collection: X-AREA (Stoe & Cie, 2008); cell
X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); 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 (Sheldrick, 2008).[Ni(C2N3)2(C5H5N)4] | F(000) = 1048 |
Mr = 507.21 | Dx = 1.415 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 11154 reflections |
a = 13.0439 (6) Å | θ = 3.0–28.1° |
b = 12.8557 (8) Å | µ = 0.85 mm−1 |
c = 15.1294 (7) Å | T = 170 K |
β = 110.191 (5)° | Block, light green |
V = 2381.1 (2) Å3 | 0.05 × 0.04 × 0.04 mm |
Z = 4 |
Stoe IPDS-1 diffractometer | 5386 independent reflections |
Radiation source: fine-focus sealed tube | 4554 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
phi scan | θmax = 28.1°, θmin = 3.0° |
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) | h = −17→17 |
Tmin = 0.911, Tmax = 0.973 | k = −16→16 |
11154 measured reflections | l = −19→19 |
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)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.092 | w = 1/[σ2(Fo2) + (0.0593P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.98 | (Δ/σ)max < 0.001 |
5386 reflections | Δρmax = 0.35 e Å−3 |
318 parameters | Δρmin = −0.44 e Å−3 |
2 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: 0.0106 (6) |
[Ni(C2N3)2(C5H5N)4] | V = 2381.1 (2) Å3 |
Mr = 507.21 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 13.0439 (6) Å | µ = 0.85 mm−1 |
b = 12.8557 (8) Å | T = 170 K |
c = 15.1294 (7) Å | 0.05 × 0.04 × 0.04 mm |
β = 110.191 (5)° |
Stoe IPDS-1 diffractometer | 5386 independent reflections |
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) | 4554 reflections with I > 2σ(I) |
Tmin = 0.911, Tmax = 0.973 | Rint = 0.035 |
11154 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 2 restraints |
wR(F2) = 0.092 | H-atom parameters constrained |
S = 0.98 | Δρmax = 0.35 e Å−3 |
5386 reflections | Δρmin = −0.44 e Å−3 |
318 parameters |
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 | 0.53427 (5) | 0.75512 (3) | 0.65840 (5) | 0.01803 (10) | |
N1 | 0.5772 (2) | 0.68096 (18) | 0.7947 (2) | 0.0204 (6) | |
C1 | 0.5414 (3) | 0.7163 (3) | 0.8622 (3) | 0.0254 (7) | |
H1 | 0.4997 | 0.7786 | 0.8508 | 0.031* | |
C2 | 0.5620 (3) | 0.6669 (3) | 0.9474 (3) | 0.0314 (8) | |
H2 | 0.5360 | 0.6956 | 0.9935 | 0.038* | |
C3 | 0.6207 (3) | 0.5749 (3) | 0.9651 (3) | 0.0332 (8) | |
H3 | 0.6345 | 0.5385 | 1.0227 | 0.040* | |
C4 | 0.6587 (3) | 0.5376 (3) | 0.8962 (3) | 0.0338 (8) | |
H4 | 0.6992 | 0.4747 | 0.9057 | 0.041* | |
C5 | 0.6369 (3) | 0.5932 (2) | 0.8131 (3) | 0.0280 (7) | |
H5 | 0.6655 | 0.5682 | 0.7672 | 0.034* | |
N11 | 0.6453 (2) | 0.88091 (19) | 0.7206 (2) | 0.0230 (6) | |
C11 | 0.7525 (3) | 0.8647 (3) | 0.7619 (3) | 0.0364 (9) | |
H11 | 0.7792 | 0.7954 | 0.7664 | 0.044* | |
C12 | 0.8266 (4) | 0.9446 (3) | 0.7983 (4) | 0.0512 (12) | |
H12 | 0.9024 | 0.9299 | 0.8262 | 0.061* | |
C13 | 0.7897 (4) | 1.0450 (3) | 0.7938 (4) | 0.0480 (11) | |
H13 | 0.8391 | 1.1008 | 0.8188 | 0.058* | |
C14 | 0.6809 (4) | 1.0628 (3) | 0.7529 (3) | 0.0416 (10) | |
H14 | 0.6527 | 1.1315 | 0.7484 | 0.050* | |
C15 | 0.6115 (3) | 0.9793 (2) | 0.7179 (3) | 0.0331 (8) | |
H15 | 0.5355 | 0.9929 | 0.6903 | 0.040* | |
N21 | 0.4158 (2) | 0.63412 (19) | 0.5948 (2) | 0.0223 (6) | |
C21 | 0.4425 (3) | 0.5333 (2) | 0.6051 (3) | 0.0285 (8) | |
H21 | 0.5166 | 0.5153 | 0.6378 | 0.034* | |
C22 | 0.3677 (4) | 0.4536 (3) | 0.5706 (3) | 0.0403 (10) | |
H22 | 0.3902 | 0.3829 | 0.5799 | 0.048* | |
C23 | 0.2604 (4) | 0.4788 (3) | 0.5226 (3) | 0.0419 (10) | |
H23 | 0.2071 | 0.4259 | 0.4988 | 0.050* | |
C24 | 0.2317 (3) | 0.5822 (3) | 0.5098 (3) | 0.0406 (9) | |
H24 | 0.1585 | 0.6020 | 0.4756 | 0.049* | |
C25 | 0.3110 (3) | 0.6567 (3) | 0.5475 (3) | 0.0297 (8) | |
H25 | 0.2901 | 0.7279 | 0.5393 | 0.036* | |
N31 | 0.4925 (2) | 0.81948 (19) | 0.5191 (2) | 0.0228 (6) | |
C31 | 0.5106 (3) | 0.7632 (3) | 0.4508 (3) | 0.0269 (7) | |
H31 | 0.5396 | 0.6950 | 0.4657 | 0.032* | |
C32 | 0.4890 (3) | 0.7998 (3) | 0.3597 (3) | 0.0359 (8) | |
H32 | 0.5032 | 0.7575 | 0.3138 | 0.043* | |
C33 | 0.4467 (3) | 0.8983 (3) | 0.3369 (3) | 0.0368 (9) | |
H33 | 0.4307 | 0.9249 | 0.2750 | 0.044* | |
C34 | 0.4282 (4) | 0.9574 (3) | 0.4057 (3) | 0.0384 (9) | |
H34 | 0.4000 | 1.0260 | 0.3924 | 0.046* | |
C35 | 0.4513 (3) | 0.9153 (3) | 0.4948 (3) | 0.0326 (8) | |
H35 | 0.4371 | 0.9565 | 0.5414 | 0.039* | |
N41 | 0.6587 (2) | 0.67389 (19) | 0.6335 (2) | 0.0241 (6) | |
C41 | 0.7342 (3) | 0.6558 (2) | 0.6128 (2) | 0.0234 (7) | |
N42 | 0.8215 (3) | 0.6277 (3) | 0.5954 (3) | 0.0398 (8) | |
C42 | 0.8367 (3) | 0.6685 (3) | 0.5206 (3) | 0.0445 (10) | |
N43 | 0.8561 (4) | 0.6974 (3) | 0.4559 (3) | 0.0723 (14) | |
N51 | 0.4106 (2) | 0.8376 (2) | 0.6812 (2) | 0.0248 (6) | |
C51 | 0.3343 (3) | 0.8681 (2) | 0.6955 (2) | 0.0198 (6) | |
N52 | 0.2530 (3) | 0.9113 (2) | 0.7117 (2) | 0.0304 (6) | |
C52 | 0.1669 (3) | 0.8567 (2) | 0.7082 (2) | 0.0266 (6) | |
N53 | 0.0854 (3) | 0.8178 (3) | 0.7044 (3) | 0.0512 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.01894 (14) | 0.01636 (15) | 0.02019 (15) | 0.00311 (14) | 0.00853 (10) | −0.00008 (15) |
N1 | 0.0215 (15) | 0.0189 (11) | 0.0215 (17) | 0.0028 (9) | 0.0083 (13) | 0.0001 (10) |
C1 | 0.0266 (16) | 0.0255 (15) | 0.0252 (19) | 0.0042 (13) | 0.0103 (15) | 0.0020 (14) |
C2 | 0.0326 (18) | 0.0417 (18) | 0.0224 (18) | 0.0036 (14) | 0.0127 (15) | −0.0012 (14) |
C3 | 0.037 (2) | 0.0382 (18) | 0.024 (2) | 0.0060 (14) | 0.0090 (17) | 0.0072 (14) |
C4 | 0.043 (2) | 0.0283 (15) | 0.030 (2) | 0.0167 (14) | 0.0136 (17) | 0.0102 (13) |
C5 | 0.0342 (18) | 0.0260 (14) | 0.0257 (18) | 0.0106 (12) | 0.0127 (15) | 0.0035 (12) |
N11 | 0.0242 (15) | 0.0221 (12) | 0.0234 (16) | 0.0002 (10) | 0.0093 (13) | −0.0014 (10) |
C11 | 0.033 (2) | 0.0281 (16) | 0.044 (3) | −0.0006 (13) | 0.0074 (19) | −0.0027 (14) |
C12 | 0.033 (2) | 0.044 (2) | 0.061 (3) | −0.0111 (17) | −0.003 (2) | −0.008 (2) |
C13 | 0.051 (3) | 0.0321 (18) | 0.060 (3) | −0.0195 (17) | 0.019 (2) | −0.0114 (18) |
C14 | 0.048 (2) | 0.0229 (15) | 0.055 (3) | −0.0078 (15) | 0.018 (2) | −0.0056 (15) |
C15 | 0.035 (2) | 0.0189 (14) | 0.047 (2) | −0.0006 (13) | 0.0160 (18) | −0.0047 (14) |
N21 | 0.0225 (15) | 0.0185 (11) | 0.0259 (16) | −0.0004 (9) | 0.0084 (13) | −0.0028 (10) |
C21 | 0.0280 (17) | 0.0188 (13) | 0.038 (2) | 0.0029 (12) | 0.0106 (16) | −0.0011 (12) |
C22 | 0.048 (2) | 0.0187 (15) | 0.052 (3) | −0.0014 (14) | 0.014 (2) | −0.0050 (14) |
C23 | 0.035 (2) | 0.0349 (18) | 0.050 (3) | −0.0111 (15) | 0.0068 (19) | −0.0073 (16) |
C24 | 0.0274 (19) | 0.0347 (18) | 0.050 (3) | −0.0043 (14) | 0.0009 (18) | −0.0037 (16) |
C25 | 0.0222 (16) | 0.0257 (14) | 0.034 (2) | 0.0013 (12) | 0.0006 (15) | −0.0023 (13) |
N31 | 0.0239 (15) | 0.0220 (12) | 0.0221 (17) | 0.0011 (10) | 0.0075 (13) | 0.0024 (10) |
C31 | 0.0275 (16) | 0.0328 (17) | 0.0208 (18) | 0.0002 (13) | 0.0089 (14) | −0.0039 (13) |
C32 | 0.0334 (19) | 0.053 (2) | 0.023 (2) | −0.0027 (16) | 0.0118 (16) | −0.0039 (15) |
C33 | 0.033 (2) | 0.051 (2) | 0.026 (2) | −0.0024 (15) | 0.0106 (17) | 0.0107 (15) |
C34 | 0.043 (2) | 0.0395 (19) | 0.030 (2) | 0.0065 (15) | 0.0077 (18) | 0.0153 (15) |
C35 | 0.040 (2) | 0.0297 (15) | 0.029 (2) | 0.0076 (13) | 0.0123 (17) | 0.0056 (12) |
N41 | 0.0250 (15) | 0.0243 (12) | 0.0258 (17) | 0.0077 (10) | 0.0122 (14) | 0.0019 (10) |
C41 | 0.0243 (16) | 0.0230 (14) | 0.0232 (18) | −0.0021 (11) | 0.0085 (14) | −0.0037 (11) |
N42 | 0.0305 (17) | 0.0533 (19) | 0.045 (2) | 0.0087 (14) | 0.0245 (15) | −0.0011 (14) |
C42 | 0.048 (2) | 0.0416 (18) | 0.060 (3) | −0.0219 (16) | 0.039 (2) | −0.0256 (17) |
N43 | 0.103 (3) | 0.067 (3) | 0.082 (3) | −0.046 (2) | 0.076 (3) | −0.033 (2) |
N51 | 0.0223 (15) | 0.0225 (12) | 0.0307 (18) | 0.0055 (10) | 0.0106 (14) | −0.0014 (10) |
C51 | 0.0244 (15) | 0.0164 (12) | 0.0168 (15) | 0.0023 (10) | 0.0048 (12) | −0.0002 (10) |
N52 | 0.0295 (14) | 0.0243 (13) | 0.0441 (18) | 0.0036 (11) | 0.0213 (13) | −0.0051 (11) |
C52 | 0.0266 (15) | 0.0241 (13) | 0.0324 (18) | 0.0097 (11) | 0.0144 (13) | 0.0082 (11) |
N53 | 0.0377 (17) | 0.0438 (17) | 0.079 (3) | 0.0064 (14) | 0.0294 (18) | 0.0222 (17) |
Ni1—N51 | 2.057 (3) | N21—C25 | 1.338 (5) |
Ni1—N41 | 2.071 (3) | C21—C22 | 1.386 (5) |
Ni1—N31 | 2.152 (3) | C21—H21 | 0.9500 |
Ni1—N11 | 2.158 (3) | C22—C23 | 1.375 (6) |
Ni1—N1 | 2.162 (3) | C22—H22 | 0.9500 |
Ni1—N21 | 2.169 (3) | C23—C24 | 1.377 (6) |
N1—C1 | 1.341 (4) | C23—H23 | 0.9500 |
N1—C5 | 1.344 (4) | C24—C25 | 1.381 (5) |
C1—C2 | 1.377 (5) | C24—H24 | 0.9500 |
C1—H1 | 0.9500 | C25—H25 | 0.9500 |
C2—C3 | 1.383 (5) | N31—C35 | 1.343 (4) |
C2—H2 | 0.9500 | N31—C31 | 1.348 (5) |
C3—C4 | 1.385 (5) | C31—C32 | 1.391 (5) |
C3—H3 | 0.9500 | C31—H31 | 0.9500 |
C4—C5 | 1.388 (5) | C32—C33 | 1.376 (6) |
C4—H4 | 0.9500 | C32—H32 | 0.9500 |
C5—H5 | 0.9500 | C33—C34 | 1.376 (6) |
N11—C15 | 1.336 (4) | C33—H33 | 0.9500 |
N11—C11 | 1.337 (5) | C34—C35 | 1.385 (5) |
C11—C12 | 1.388 (6) | C34—H34 | 0.9500 |
C11—H11 | 0.9500 | C35—H35 | 0.9500 |
C12—C13 | 1.371 (6) | N41—C41 | 1.154 (4) |
C12—H12 | 0.9500 | C41—N42 | 1.306 (4) |
C13—C14 | 1.358 (7) | N42—C42 | 1.322 (5) |
C13—H13 | 0.9500 | C42—N43 | 1.154 (5) |
C14—C15 | 1.386 (5) | N51—C51 | 1.157 (4) |
C14—H14 | 0.9500 | C51—N52 | 1.294 (4) |
C15—H15 | 0.9500 | N52—C52 | 1.309 (4) |
N21—C21 | 1.337 (4) | C52—N53 | 1.159 (4) |
N51—Ni1—N41 | 178.96 (15) | N11—C15—C14 | 123.8 (4) |
N51—Ni1—N31 | 91.03 (12) | N11—C15—H15 | 118.1 |
N41—Ni1—N31 | 88.00 (11) | C14—C15—H15 | 118.1 |
N51—Ni1—N11 | 89.29 (11) | C21—N21—C25 | 116.7 (3) |
N41—Ni1—N11 | 90.40 (11) | C21—N21—Ni1 | 121.8 (3) |
N31—Ni1—N11 | 92.51 (11) | C25—N21—Ni1 | 121.4 (2) |
N51—Ni1—N1 | 91.56 (11) | N21—C21—C22 | 123.5 (4) |
N41—Ni1—N1 | 89.43 (11) | N21—C21—H21 | 118.3 |
N31—Ni1—N1 | 176.39 (11) | C22—C21—H21 | 118.3 |
N11—Ni1—N1 | 90.04 (11) | C23—C22—C21 | 118.7 (3) |
N51—Ni1—N21 | 87.97 (11) | C23—C22—H22 | 120.6 |
N41—Ni1—N21 | 92.33 (11) | C21—C22—H22 | 120.6 |
N31—Ni1—N21 | 86.59 (11) | C22—C23—C24 | 118.6 (4) |
N11—Ni1—N21 | 177.09 (12) | C22—C23—H23 | 120.7 |
N1—Ni1—N21 | 90.98 (11) | C24—C23—H23 | 120.7 |
C1—N1—C5 | 117.1 (3) | C23—C24—C25 | 118.9 (4) |
C1—N1—Ni1 | 122.3 (2) | C23—C24—H24 | 120.5 |
C5—N1—Ni1 | 120.5 (2) | C25—C24—H24 | 120.5 |
N1—C1—C2 | 123.3 (3) | N21—C25—C24 | 123.5 (3) |
N1—C1—H1 | 118.3 | N21—C25—H25 | 118.2 |
C2—C1—H1 | 118.3 | C24—C25—H25 | 118.2 |
C1—C2—C3 | 119.5 (3) | C35—N31—C31 | 116.2 (3) |
C1—C2—H2 | 120.3 | C35—N31—Ni1 | 124.3 (2) |
C3—C2—H2 | 120.3 | C31—N31—Ni1 | 119.5 (2) |
C2—C3—C4 | 117.9 (3) | N31—C31—C32 | 123.3 (4) |
C2—C3—H3 | 121.1 | N31—C31—H31 | 118.3 |
C4—C3—H3 | 121.1 | C32—C31—H31 | 118.3 |
C3—C4—C5 | 119.3 (3) | C33—C32—C31 | 119.1 (4) |
C3—C4—H4 | 120.3 | C33—C32—H32 | 120.5 |
C5—C4—H4 | 120.3 | C31—C32—H32 | 120.5 |
N1—C5—C4 | 122.8 (3) | C32—C33—C34 | 118.6 (4) |
N1—C5—H5 | 118.6 | C32—C33—H33 | 120.7 |
C4—C5—H5 | 118.6 | C34—C33—H33 | 120.7 |
C15—N11—C11 | 116.3 (3) | C33—C34—C35 | 118.9 (4) |
C15—N11—Ni1 | 122.1 (3) | C33—C34—H34 | 120.5 |
C11—N11—Ni1 | 121.6 (2) | C35—C34—H34 | 120.5 |
N11—C11—C12 | 122.9 (4) | N31—C35—C34 | 123.9 (4) |
N11—C11—H11 | 118.5 | N31—C35—H35 | 118.1 |
C12—C11—H11 | 118.5 | C34—C35—H35 | 118.1 |
C13—C12—C11 | 119.5 (5) | C41—N41—Ni1 | 161.0 (3) |
C13—C12—H12 | 120.2 | N41—C41—N42 | 174.3 (4) |
C11—C12—H12 | 120.2 | C41—N42—C42 | 117.5 (4) |
C14—C13—C12 | 118.4 (4) | N43—C42—N42 | 174.2 (5) |
C14—C13—H13 | 120.8 | C51—N51—Ni1 | 168.7 (3) |
C12—C13—H13 | 120.8 | N51—C51—N52 | 174.3 (3) |
C13—C14—C15 | 119.1 (4) | C51—N52—C52 | 120.7 (3) |
C13—C14—H14 | 120.5 | N53—C52—N52 | 173.2 (3) |
C15—C14—H14 | 120.5 |
Experimental details
Crystal data | |
Chemical formula | [Ni(C2N3)2(C5H5N)4] |
Mr | 507.21 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 170 |
a, b, c (Å) | 13.0439 (6), 12.8557 (8), 15.1294 (7) |
β (°) | 110.191 (5) |
V (Å3) | 2381.1 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.85 |
Crystal size (mm) | 0.05 × 0.04 × 0.04 |
Data collection | |
Diffractometer | Stoe IPDS1 diffractometer |
Absorption correction | Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) |
Tmin, Tmax | 0.911, 0.973 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11154, 5386, 4554 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.662 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.092, 0.98 |
No. of reflections | 5386 |
No. of parameters | 318 |
No. of restraints | 2 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.35, −0.44 |
Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), XCIF in SHELXTL (Sheldrick, 2008).
Acknowledgements
We gratefully acknowledge financial support by the DFG (project No. NA 720/3–1) and the State of Schleswig–Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facility.
References
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Recently we have reported on the thermal and magnetic properties of coordination polymers based on paramagnetic transition metal thio- and selenocyanato compounds in which the cations are linked by thio- or selenocyanato anions (Boeckmann & Näther; 2010; Boeckmann & Näther, 2011). The bridging compounds with e.g. pyridine can be prepared by thermal decomposition of discrete complexes with terminal bonded anionic ligands. In the course of systematic investigations we also started to investigated similar compounds based on dicyanamide (Wriedt & Näther, 2011). Within this project crystals of the title compound were obtained, which were characterized by single-crystal X-ray diffraction. In the crystal structure of the title compound each nickel(II) cation is six-coordinated by two dicyanamido anions and four pyridine ligands in a slightly distorted octehedral geometry (Fig. 1). The NiN6 distances ranges from 2.057 (3) Å to 2.169 (3) Å and the angles are between 86.59 (11) ° and 178.96 (15)°. In the crystal structure, the discrete complexes are connected through intermolecular N—HC hydrogen bonds with an N···H distances of 2.559 Å (Fig. 2). The shortest nickel(II)—nickel(II) distance between the complexes is 9.157 Å.
It must be noted that a discrete nickel(II) dicyanamide complex is reported (Wu et al., 2004) with 1,10-phenanthroline as co-ligands in which all ligands are cis-coordinated.