Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680100753X/ob6038sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680100753X/ob6038Isup2.hkl |
CCDC reference: 170736
Key indicators
- Single-crystal X-ray study
- T = 301 K
- Mean (C-C) = 0.005 Å
- R factor = 0.032
- wR factor = 0.085
- Data-to-parameter ratio = 15.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
To a solution of N, N'-bis(salicylidene)-1,3-propanediamine (2.82 g, 0.1 mol) in hot ethanol (50 ml), 20% ammonia solution (10 ml) was added and the mixture was heated to boiling point. Then a solution of NiCl2·6H2O (2.38 g, 0.1 mol) in hot water (30 ml) was added and the resulting mixture set aside. After 2 h, the light-green Ni complex was filtered and dried at 423 K for 3 h. 0.339 g (1 mmol) of this complex was dissolved in 60 ml hot dimethylformamide and the temperature of the solution was increased to 383 K. Dropwise addition of Cu(CH3COO)2·H2O (0.100 g, 0.5 mmol) dissolved in 20 ml hot ethanol resulted in the formation of crystals of (I) after 24 h.
H atoms were placed geometrically from their parent atoms and a riding model was used with Ueq(H) = 1.2Ueq(C).
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1993); cell refinement: SHELXL97 (Sheldrick, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: SHELXL97.
[CuNi2(C17H16N2O2)2(C2H3O2)2(C3H7NO)2] | V = 1131.5 (2) Å3 |
Mr = 1005.88 | Z = 1 |
Triclinic, P1 | Dx = 1.476 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.5802 (12) Å | Cell parameters from 25 reflections |
b = 10.6920 (13) Å | θ = 2.5–25.7° |
c = 12.2069 (11) Å | µ = 1.35 mm−1 |
α = 112.203 (3)° | T = 301 K |
β = 101.145 (5)° | Parallelpiped, blue green |
γ = 90.376 (3)° | 0.25 × 0.20 × 0.15 mm |
CAD-4 EXPRESS diffractometer | Rint = 0.013 |
ω/2θ scans | θmax = 25.7° |
Absorption correction: ψ scan (Fair, 1990) | h = −11→11 |
Tmin = 0.729, Tmax = 0.823 | k = 0→13 |
4526 measured reflections | l = −14→13 |
4282 independent reflections | 3 standard reflections every 120 min |
3386 reflections with I > 2σ(I) | intensity decay: 0.1% |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | H-atom parameters constrained |
S = 0.93 | w = 1/[σ2(Fo2) + (0.0725P)2 + 2.0204P] where P = (Fo2 + 2Fc2)/3 |
4282 reflections | (Δ/σ)max = 0.001 |
286 parameters | Δρmax = 0.43 e Å−3 |
0 restraints | Δρmin = −0.34 e Å−3 |
[CuNi2(C17H16N2O2)2(C2H3O2)2(C3H7NO)2] | γ = 90.376 (3)° |
Mr = 1005.88 | V = 1131.5 (2) Å3 |
Triclinic, P1 | Z = 1 |
a = 9.5802 (12) Å | Mo Kα radiation |
b = 10.6920 (13) Å | µ = 1.35 mm−1 |
c = 12.2069 (11) Å | T = 301 K |
α = 112.203 (3)° | 0.25 × 0.20 × 0.15 mm |
β = 101.145 (5)° |
CAD-4 EXPRESS diffractometer | 3386 reflections with I > 2σ(I) |
Absorption correction: ψ scan (Fair, 1990) | Rint = 0.013 |
Tmin = 0.729, Tmax = 0.823 | 3 standard reflections every 120 min |
4526 measured reflections | intensity decay: 0.1% |
4282 independent reflections |
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.085 | H-atom parameters constrained |
S = 0.93 | Δρmax = 0.43 e Å−3 |
4282 reflections | Δρmin = −0.34 e Å−3 |
286 parameters |
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 | ||
Cu | 0.5000 | 0.0000 | 0.5000 | 0.02907 (13) | |
Ni | 0.70801 (4) | −0.09668 (4) | 0.66884 (3) | 0.02955 (12) | |
N1 | 0.8975 (3) | −0.0060 (3) | 0.7809 (2) | 0.0351 (5) | |
N2 | 0.7223 (3) | −0.2796 (2) | 0.6795 (2) | 0.0348 (5) | |
N3 | 0.5103 (3) | 0.1376 (3) | 0.9489 (2) | 0.0469 (7) | |
O1 | 0.6637 (2) | 0.08068 (19) | 0.65178 (18) | 0.0339 (4) | |
O2 | 0.5113 (2) | −0.1553 (2) | 0.56369 (18) | 0.0342 (4) | |
O3 | 0.3439 (2) | 0.0838 (2) | 0.59676 (18) | 0.0385 (5) | |
O4 | 0.1925 (2) | 0.1570 (2) | 0.47378 (19) | 0.0407 (5) | |
O5 | 0.6266 (2) | −0.0279 (2) | 0.8354 (2) | 0.0445 (5) | |
C1 | 0.6988 (3) | 0.1994 (3) | 0.7411 (3) | 0.0327 (6) | |
C2 | 0.6134 (4) | 0.3075 (3) | 0.7480 (3) | 0.0439 (7) | |
C3 | 0.6473 (4) | 0.4324 (3) | 0.8426 (3) | 0.0536 (9) | |
C4 | 0.7689 (4) | 0.4561 (3) | 0.9323 (3) | 0.0569 (9) | |
C5 | 0.8564 (4) | 0.3537 (3) | 0.9264 (3) | 0.0485 (8) | |
C6 | 0.8231 (3) | 0.2239 (3) | 0.8340 (3) | 0.0368 (7) | |
C7 | 0.9199 (3) | 0.1222 (3) | 0.8398 (3) | 0.0386 (7) | |
C8 | 1.0111 (3) | −0.0911 (4) | 0.7999 (3) | 0.0473 (8) | |
C9 | 0.9556 (4) | −0.2107 (4) | 0.8226 (3) | 0.0510 (9) | |
C10 | 0.8632 (3) | −0.3219 (3) | 0.7130 (3) | 0.0460 (8) | |
C11 | 0.6132 (3) | −0.3627 (3) | 0.6549 (3) | 0.0385 (7) | |
C12 | 0.4650 (3) | −0.3429 (3) | 0.6168 (3) | 0.0361 (6) | |
C13 | 0.3612 (4) | −0.4343 (3) | 0.6204 (3) | 0.0475 (8) | |
C14 | 0.2176 (4) | −0.4261 (4) | 0.5857 (3) | 0.0529 (9) | |
C15 | 0.1736 (4) | −0.3280 (4) | 0.5413 (3) | 0.0498 (8) | |
C16 | 0.2714 (3) | −0.2385 (3) | 0.5330 (3) | 0.0408 (7) | |
C17 | 0.4191 (3) | −0.2416 (3) | 0.5717 (3) | 0.0332 (6) | |
C18 | 0.2319 (3) | 0.1337 (3) | 0.5678 (3) | 0.0404 (7) | |
C19 | 0.1309 (5) | 0.1673 (7) | 0.6537 (4) | 0.0966 (19) | |
C20 | 0.5242 (3) | 0.0411 (3) | 0.8461 (3) | 0.0421 (7) | |
C21 | 0.6226 (4) | 0.1801 (4) | 1.0550 (3) | 0.0638 (11) | |
C22 | 0.3870 (6) | 0.2149 (6) | 0.9553 (5) | 0.1008 (19) | |
H2 | 0.5306 | 0.2944 | 0.6863 | 0.053* | |
H3 | 0.5864 | 0.5029 | 0.8462 | 0.064* | |
H4 | 0.7915 | 0.5422 | 0.9973 | 0.068* | |
H5 | 0.9418 | 0.3710 | 0.9863 | 0.058* | |
H7 | 1.0103 | 0.1543 | 0.8934 | 0.046* | |
H8A | 1.0867 | −0.0356 | 0.8700 | 0.057* | |
H8B | 1.0542 | −0.1252 | 0.7276 | 0.057* | |
H9A | 1.0384 | −0.2513 | 0.8544 | 0.061* | |
H9B | 0.8993 | −0.1763 | 0.8864 | 0.061* | |
H10A | 0.9113 | −0.3461 | 0.6438 | 0.055* | |
H10B | 0.8523 | −0.4037 | 0.7313 | 0.055* | |
H11 | 0.6314 | −0.4466 | 0.6625 | 0.046* | |
H13 | 0.3914 | −0.5039 | 0.6478 | 0.057* | |
H14 | 0.1496 | −0.4867 | 0.5919 | 0.064* | |
H15 | 0.0744 | −0.3222 | 0.5163 | 0.060* | |
H16 | 0.2384 | −0.1735 | 0.5006 | 0.049* | |
H19A | 0.1713 | 0.1452 | 0.7236 | 0.145* | |
H19B | 0.0388 | 0.1143 | 0.6120 | 0.145* | |
H19C | 0.1170 | 0.2642 | 0.6811 | 0.145* | |
H20 | 0.4508 | 0.0242 | 0.7763 | 0.050* | |
H21A | 0.5920 | 0.2524 | 1.1214 | 0.096* | |
H21B | 0.7079 | 0.2141 | 1.0381 | 0.096* | |
H21C | 0.6448 | 0.1030 | 1.0782 | 0.096* | |
H22A | 0.3955 | 0.2816 | 1.0381 | 0.151* | |
H22B | 0.3004 | 0.1536 | 0.9325 | 0.151* | |
H22C | 0.3815 | 0.2618 | 0.8997 | 0.151* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu | 0.0288 (2) | 0.0302 (3) | 0.0287 (2) | 0.0140 (2) | 0.00190 (18) | 0.00402 (19) |
Ni | 0.0290 (2) | 0.0301 (2) | 0.0306 (2) | 0.01298 (15) | 0.00597 (14) | 0.00510 (14) |
N1 | 0.0303 (12) | 0.0404 (14) | 0.0333 (12) | 0.0138 (11) | 0.0044 (10) | 0.0064 (10) |
N2 | 0.0376 (13) | 0.0356 (13) | 0.0351 (13) | 0.0173 (11) | 0.0088 (10) | 0.0106 (11) |
N3 | 0.0506 (16) | 0.0448 (16) | 0.0419 (15) | 0.0109 (13) | 0.0139 (13) | 0.0125 (13) |
O1 | 0.0350 (10) | 0.0290 (10) | 0.0332 (10) | 0.0104 (8) | 0.0001 (8) | 0.0026 (8) |
O2 | 0.0296 (10) | 0.0324 (10) | 0.0423 (11) | 0.0192 (9) | 0.0016 (8) | −0.0003 (8) |
O3 | 0.0377 (11) | 0.0446 (12) | 0.0349 (11) | 0.0171 (9) | 0.0078 (9) | 0.0075 (9) |
O4 | 0.0400 (11) | 0.0501 (13) | 0.0383 (11) | 0.0211 (10) | 0.0140 (9) | 0.0139 (10) |
O5 | 0.0464 (12) | 0.0489 (13) | 0.0442 (12) | 0.0199 (10) | 0.0194 (10) | 0.0152 (10) |
C1 | 0.0372 (15) | 0.0290 (14) | 0.0329 (14) | 0.0129 (12) | 0.0079 (12) | −0.0019 (12) |
C2 | 0.0494 (18) | 0.0352 (17) | 0.0446 (18) | 0.0162 (14) | 0.0025 (14) | 0.0045 (14) |
C3 | 0.068 (2) | 0.0323 (17) | 0.054 (2) | 0.0122 (15) | 0.0078 (18) | 0.0118 (16) |
C4 | 0.075 (3) | 0.0314 (17) | 0.050 (2) | 0.0039 (15) | 0.0040 (18) | 0.0019 (17) |
C5 | 0.053 (2) | 0.0428 (19) | 0.0417 (18) | 0.0119 (15) | −0.0002 (15) | −0.0069 (15) |
C6 | 0.0404 (16) | 0.0343 (16) | 0.0350 (16) | 0.0131 (13) | 0.0070 (13) | −0.0005 (13) |
C7 | 0.0329 (15) | 0.0474 (18) | 0.0316 (15) | 0.0139 (13) | 0.0015 (12) | −0.0021 (13) |
C8 | 0.0344 (16) | 0.052 (2) | 0.0489 (19) | 0.0158 (16) | 0.0024 (14) | 0.0101 (14) |
C9 | 0.0475 (19) | 0.059 (2) | 0.0489 (19) | 0.0282 (17) | 0.0012 (15) | 0.0161 (16) |
C10 | 0.0426 (17) | 0.0436 (18) | 0.058 (2) | 0.0262 (16) | 0.0101 (15) | 0.0149 (14) |
C11 | 0.0494 (18) | 0.0332 (15) | 0.0399 (16) | 0.0195 (13) | 0.0141 (14) | 0.0098 (13) |
C12 | 0.0408 (16) | 0.0332 (15) | 0.0357 (15) | 0.0125 (12) | 0.0134 (12) | 0.0019 (12) |
C13 | 0.059 (2) | 0.0390 (18) | 0.0504 (19) | 0.0212 (15) | 0.0179 (16) | 0.0002 (15) |
C14 | 0.051 (2) | 0.049 (2) | 0.058 (2) | 0.0172 (17) | 0.0174 (17) | −0.0130 (16) |
C15 | 0.0385 (17) | 0.052 (2) | 0.055 (2) | 0.0147 (17) | 0.0128 (15) | −0.0039 (15) |
C16 | 0.0359 (16) | 0.0384 (17) | 0.0470 (18) | 0.0159 (14) | 0.0076 (13) | 0.0002 (13) |
C17 | 0.0366 (15) | 0.0301 (14) | 0.0312 (14) | 0.0088 (12) | 0.0100 (12) | −0.0003 (12) |
C18 | 0.0410 (17) | 0.0494 (18) | 0.0345 (16) | 0.0181 (14) | 0.0124 (13) | 0.0083 (14) |
C19 | 0.076 (3) | 0.182 (6) | 0.072 (3) | 0.077 (4) | 0.045 (3) | 0.067 (4) |
C20 | 0.0444 (18) | 0.0463 (18) | 0.0356 (16) | 0.0144 (14) | 0.0116 (14) | 0.0074 (15) |
C21 | 0.069 (3) | 0.070 (3) | 0.0406 (19) | 0.0088 (18) | 0.0090 (18) | −0.009 (2) |
C22 | 0.089 (4) | 0.100 (4) | 0.089 (4) | 0.006 (3) | 0.025 (3) | 0.054 (3) |
Cu—Ni | 3.0556 (5) | C10—N2 | 1.459 (4) |
Cui—O1 | 2.0705 (19) | C10—H10A | 0.99 |
Cu—O1 | 2.0705 (19) | C10—H10B | 0.99 |
Cu—O2 | 2.0782 (19) | C11—N2 | 1.280 (4) |
Cui—O2 | 2.0782 (19) | C11—C12 | 1.449 (4) |
Cui—O3 | 2.082 (2) | C11—H11 | 0.95 |
Cu—O3 | 2.082 (2) | C12—C13 | 1.408 (4) |
Ni—N1 | 2.030 (2) | C12—C17 | 1.426 (4) |
Ni—N2 | 2.012 (2) | C13—C14 | 1.372 (5) |
Ni—O2 | 2.0082 (19) | C13—H13 | 0.95 |
Ni—O1 | 2.024 (2) | C14—C15 | 1.384 (5) |
Nii—O4 | 2.039 (2) | C14—H14 | 0.95 |
Ni—O5 | 2.186 (2) | C15—C16 | 1.379 (4) |
O4—Nii | 2.039 (2) | C15—H15 | 0.95 |
C1—O1 | 1.311 (3) | C16—C17 | 1.408 (4) |
C1—C2 | 1.407 (4) | C16—H16 | 0.95 |
C1—C6 | 1.422 (4) | C17—O2 | 1.316 (3) |
C2—C3 | 1.380 (5) | C18—O3 | 1.250 (4) |
C2—H2 | 0.95 | C18—O4 | 1.253 (4) |
C3—C4 | 1.384 (5) | C18—C19 | 1.509 (5) |
C3—H3 | 0.95 | C19—H19A | 0.98 |
C4—C5 | 1.372 (5) | C19—H19B | 0.98 |
C4—H4 | 0.95 | C19—H19C | 0.98 |
C5—C6 | 1.404 (4) | C20—O5 | 1.229 (4) |
C5—H5 | 0.95 | C20—N3 | 1.321 (4) |
C6—C7 | 1.447 (4) | C20—H20 | 0.95 |
C7—N1 | 1.278 (4) | C21—N3 | 1.433 (5) |
C7—H7 | 0.95 | C21—H21A | 0.98 |
C8—N1 | 1.463 (4) | C21—H21B | 0.98 |
C8—C9 | 1.521 (5) | C21—H21C | 0.98 |
C8—H8A | 0.99 | C22—N3 | 1.444 (5) |
C8—H8B | 0.99 | C22—H22A | 0.98 |
C9—C10 | 1.521 (5) | C22—H22B | 0.98 |
C9—H9A | 0.99 | C22—H22C | 0.98 |
C9—H9B | 0.99 | ||
O1—Cu—O2 | 78.89 (8) | C10—C9—C8 | 115.5 (3) |
O1—Cu—O3 | 92.92 (8) | C10—C9—H9A | 108.4 |
O2—Cu—O3 | 90.94 (8) | C8—C9—H9A | 108.4 |
C7—N1—C8 | 118.4 (3) | C10—C9—H9B | 108.4 |
C7—N1—Ni | 122.7 (2) | C8—C9—H9B | 108.4 |
C8—N1—Ni | 118.8 (2) | H9A—C9—H9B | 107.5 |
C11—N2—C10 | 118.1 (3) | N2—C10—C9 | 111.7 (3) |
C11—N2—Ni | 122.9 (2) | N2—C10—H10A | 109.3 |
C10—N2—Ni | 118.9 (2) | C9—C10—H10A | 109.3 |
C20—N3—C21 | 121.8 (3) | N2—C10—H10B | 109.3 |
C20—N3—C22 | 121.0 (3) | C9—C10—H10B | 109.3 |
C21—N3—C22 | 116.8 (3) | H10A—C10—H10B | 107.9 |
O2—Ni—N2 | 90.85 (9) | N2—C11—C12 | 127.2 (3) |
O2—Ni—O1 | 81.65 (8) | N2—C11—H11 | 116.4 |
N2—Ni—O1 | 171.98 (9) | C12—C11—H11 | 116.4 |
O2—Ni—N1 | 170.60 (9) | C13—C12—C17 | 118.7 (3) |
N2—Ni—N1 | 97.95 (10) | C13—C12—C11 | 117.0 (3) |
O1—Ni—N1 | 89.38 (9) | C17—C12—C11 | 124.2 (3) |
O2—Ni—O5 | 92.73 (9) | C14—C13—C12 | 122.1 (3) |
N2—Ni—O5 | 88.15 (9) | C14—C13—H13 | 119.0 |
O1—Ni—O5 | 89.36 (8) | C12—C13—H13 | 119.0 |
N1—Ni—O5 | 84.29 (9) | C13—C14—C15 | 119.0 (3) |
C1—O1—Ni | 123.34 (18) | C13—C14—H14 | 120.5 |
C1—O1—Cu | 135.37 (18) | C15—C14—H14 | 120.5 |
Ni—O1—Cu | 96.55 (8) | C16—C15—C14 | 121.0 (3) |
C17—O2—Ni | 124.41 (18) | C16—C15—H15 | 119.5 |
C17—O2—Cu | 136.00 (18) | C14—C15—H15 | 119.5 |
Ni—O2—Cu | 96.78 (8) | C15—C16—C17 | 121.3 (3) |
C18—O3—Cu | 130.8 (2) | C15—C16—H16 | 119.3 |
C20—O5—Ni | 121.0 (2) | C17—C16—H16 | 119.3 |
O1—C1—C2 | 120.6 (3) | O2—C17—C16 | 120.7 (3) |
O1—C1—C6 | 121.8 (3) | O2—C17—C12 | 121.5 (3) |
C2—C1—C6 | 117.6 (3) | C16—C17—C12 | 117.8 (3) |
C3—C2—C1 | 121.3 (3) | O3—C18—O4 | 127.2 (3) |
C3—C2—H2 | 119.3 | O3—C18—C19 | 116.9 (3) |
C1—C2—H2 | 119.3 | O4—C18—C19 | 115.9 (3) |
C2—C3—C4 | 120.8 (3) | C18—C19—H19A | 109.5 |
C2—C3—H3 | 119.6 | C18—C19—H19B | 109.5 |
C4—C3—H3 | 119.6 | H19A—C19—H19B | 109.5 |
C5—C4—C3 | 119.2 (3) | C18—C19—H19C | 109.5 |
C5—C4—H4 | 120.4 | H19A—C19—H19C | 109.5 |
C3—C4—H4 | 120.4 | H19B—C19—H19C | 109.5 |
C4—C5—C6 | 121.7 (3) | O5—C20—N3 | 123.8 (3) |
C4—C5—H5 | 119.1 | O5—C20—H20 | 118.1 |
C6—C5—H5 | 119.1 | N3—C20—H20 | 118.1 |
C5—C6—C1 | 119.3 (3) | N3—C21—H21A | 109.5 |
C5—C6—C7 | 116.9 (3) | N3—C21—H21B | 109.5 |
C1—C6—C7 | 123.8 (3) | H21A—C21—H21B | 109.5 |
N1—C7—C6 | 127.3 (3) | N3—C21—H21C | 109.5 |
N1—C7—H7 | 116.4 | H21A—C21—H21C | 109.5 |
C6—C7—H7 | 116.4 | H21B—C21—H21C | 109.5 |
N1—C8—C9 | 111.8 (3) | N3—C22—H22A | 109.5 |
N1—C8—H8A | 109.3 | N3—C22—H22B | 109.5 |
C9—C8—H8A | 109.3 | H22A—C22—H22B | 109.5 |
N1—C8—H8B | 109.3 | N3—C22—H22C | 109.5 |
C9—C8—H8B | 109.3 | H22A—C22—H22C | 109.5 |
H8A—C8—H8B | 107.9 | H22B—C22—H22C | 109.5 |
N2—Ni—O2—C17 | 32.3 (2) | C9—C8—N1—Ni | −45.6 (3) |
O1—Ni—O2—C17 | −144.8 (2) | C12—C11—N2—C10 | −178.3 (3) |
O5—Ni—O2—C17 | −55.8 (2) | C9—C10—N2—C11 | −134.8 (3) |
N2—Ni—O2—Cu | −164.02 (9) | C9—C10—N2—Ni | 47.0 (3) |
O1—Ni—O2—Cu | 18.84 (8) | O5—C20—N3—C21 | 7.0 (5) |
O5—Ni—O2—Cu | 107.79 (9) | O5—C20—N3—C22 | −179.8 (4) |
O1—Cu—O2—C17 | 141.9 (3) | C11—N2—Ni—O2 | −18.4 (2) |
O3—Cu—O2—C17 | 49.1 (3) | C10—N2—Ni—O2 | 159.6 (2) |
O1—Cu—O2—Ni | −18.56 (8) | C11—N2—Ni—N1 | 158.2 (2) |
O3—Cu—O2—Ni | −111.35 (9) | C10—N2—Ni—N1 | −23.7 (2) |
O4—C18—O3—Cu | −7.4 (5) | C11—N2—Ni—O5 | 74.3 (2) |
C19—C18—O3—Cu | 171.3 (3) | C10—N2—Ni—O5 | −107.7 (2) |
O1—Cu—O3—C18 | 142.7 (3) | C7—N1—Ni—N2 | −153.9 (2) |
O2—Cu—O3—C18 | −138.4 (3) | C8—N1—Ni—N2 | 23.0 (2) |
N3—C20—O5—Ni | −145.5 (3) | C7—N1—Ni—O1 | 22.8 (2) |
O2—Ni—O5—C20 | −45.7 (3) | C8—N1—Ni—O1 | −160.2 (2) |
N2—Ni—O5—C20 | −136.4 (3) | C7—N1—Ni—O5 | −66.6 (2) |
O1—Ni—O5—C20 | 35.9 (3) | C8—N1—Ni—O5 | 110.3 (2) |
N1—Ni—O5—C20 | 125.4 (3) | C2—C1—O1—Ni | −148.4 (2) |
O1—C1—C2—C3 | 178.8 (3) | C6—C1—O1—Ni | 31.5 (4) |
C4—C5—C6—C7 | −177.3 (3) | C6—C1—O1—Cu | −179.2 (2) |
O1—C1—C6—C5 | 179.0 (3) | O2—Ni—O1—C1 | 140.0 (2) |
C2—C1—C6—C7 | 179.1 (3) | N1—Ni—O1—C1 | −37.2 (2) |
C5—C6—C7—N1 | 165.4 (3) | O5—Ni—O1—C1 | 47.1 (2) |
C1—C6—C7—N1 | −14.8 (5) | O2—Ni—O1—Cu | −18.90 (8) |
N1—C8—C9—C10 | 71.9 (4) | N1—Ni—O1—Cu | 163.95 (9) |
C8—C9—C10—N2 | −72.7 (4) | O5—Ni—O1—Cu | −111.76 (9) |
N2—C11—C12—C13 | −166.4 (3) | O2—Cu—O1—C1 | −136.2 (3) |
N2—C11—C12—C17 | 16.4 (5) | O3—Cu—O1—C1 | −45.9 (3) |
C11—C12—C13—C14 | −179.5 (3) | O2—Cu—O1—Ni | 18.40 (8) |
C15—C16—C17—O2 | −179.7 (3) | O3—Cu—O1—Ni | 108.78 (9) |
C13—C12—C17—O2 | −178.5 (3) | C16—C17—O2—Ni | 154.7 (2) |
C11—C12—C17—C16 | 177.2 (3) | C12—C17—O2—Ni | −26.8 (4) |
C6—C7—N1—C8 | 179.6 (3) | C12—C17—O2—Cu | 176.9 (2) |
C9—C8—N1—C7 | 131.5 (3) |
Symmetry code: (i) −x+1, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [CuNi2(C17H16N2O2)2(C2H3O2)2(C3H7NO)2] |
Mr | 1005.88 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 301 |
a, b, c (Å) | 9.5802 (12), 10.6920 (13), 12.2069 (11) |
α, β, γ (°) | 112.203 (3), 101.145 (5), 90.376 (3) |
V (Å3) | 1131.5 (2) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.35 |
Crystal size (mm) | 0.25 × 0.20 × 0.15 |
Data collection | |
Diffractometer | CAD-4 EXPRESS diffractometer |
Absorption correction | ψ scan (Fair, 1990) |
Tmin, Tmax | 0.729, 0.823 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4526, 4282, 3386 |
Rint | 0.013 |
(sin θ/λ)max (Å−1) | 0.609 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.085, 0.93 |
No. of reflections | 4282 |
No. of parameters | 286 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.43, −0.34 |
Computer programs: CAD-4 EXPRESS (Enraf-Nonius, 1993), SHELXL97 (Sheldrick, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97, PLATON (Spek, 2000).
Cu—Ni | 3.0556 (5) | Ni—N2 | 2.012 (2) |
Cu—O1 | 2.0705 (19) | Ni—O2 | 2.0082 (19) |
Cu—O2 | 2.0782 (19) | Ni—O1 | 2.024 (2) |
Cu—O3 | 2.082 (2) | Nii—O4 | 2.039 (2) |
Ni—N1 | 2.030 (2) | Ni—O5 | 2.186 (2) |
O1—Cu—O2 | 78.89 (8) | O1—Ni—N1 | 89.38 (9) |
O1—Cu—O3 | 92.92 (8) | O2—Ni—O5 | 92.73 (9) |
O2—Cu—O3 | 90.94 (8) | N2—Ni—O5 | 88.15 (9) |
O2—Ni—N2 | 90.85 (9) | O1—Ni—O5 | 89.36 (8) |
O2—Ni—O1 | 81.65 (8) | N1—Ni—O5 | 84.29 (9) |
N2—Ni—O1 | 171.98 (9) | Ni—O1—Cu | 96.55 (8) |
O2—Ni—N1 | 170.60 (9) | Ni—O2—Cu | 96.78 (8) |
N2—Ni—N1 | 97.95 (10) |
Symmetry code: (i) −x+1, −y, −z+1. |
Trinuclear linear homo- or heteronuclear complexes based on Schiff base ligands are of interest because of their magnetic super-exchange interactions between bridged metal ions (Fukuhara et al., 1990). In these complexes, various combinations of metal ions in the central and terminal locations, as well as the µ-bridges, such as acetate or nitrite anions, are possible. Among the trinuclear complexes with similar formula reported from this laboratory previously (Ülkü et al., 1997; Tahir et al., 1998; Atakol et al., 1999, and references therein), the title complex, (I), resembles [CdNi2(C17H16N2O2)2(C2H3O2)2(C3H7NO)2] (Ülkü et al., 1997), (II), more than any other trinuclear complex. The crystal data indicate that (I) and (II) are isomorphous.
The central metal ions, i.e. Cu2+ in (I) and Cd2+ in (II), have irregular octahedral environments consisting of four bridging O atoms from two SALPD2- ligands [O1, O2, O1i, O2i; symmetry code: (i) -x, -y, -z; Fig. 1] and two O atoms from two bridging acetate groups (O3 and O3i). The terminal metal ion, which is Ni2+ in both (I) and (II), has a distorted octahedral coordination also, involving two N and two O atoms from a SALPD2- ligand and one O atom each from an acetate and a dimethylformamide group. The Cu—O distances in (I) are all shorter than the corresponding Cd—O distances in (II). The corresponding Ni—O and Ni—N distances have almost the same values in these two complexes. As can be seen from Fig. 2, there is an intramolecular close contact between C20—H20 and O3 [H20···O3 2.54 Å, C20···O3 3.389 (4) Å and C20—H20···O3 148.7°].