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In the title compound, [Cu(C5H4ClNO)2(C4H4N2)(H2O)2](ClO4)2, the Cu atom, which lies on an inversion centre, has an octahedral environment. The pyrazine ligand also lies about an inversion centre and links adjacent Cu atoms into a chain running along the b axis; perchlorate anions occupy the space between the chains, and the chains use the coordinated water molecules to link to the anions, resulting in a hydrogen-bonded ribbon structure. The donor 5-chloro-2-hydroxypyridine ligand exists in the zwitterionic form, i.e. 5-chloropyridinium-2-olate.
Supporting information
CCDC reference: 184484
Data collection: R3m Software (Siemens, 1990); cell refinement: R3m Software; data reduction: R3m Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[[[diaquabis(5-chloropyridinium-2-olato-
κO)copper(II)]-µ-pyrazine-
κ2N:
N'] diperchlorate]
top
Crystal data top
[Cu(C5H4ClNO)2(C4H4N2)(H2O)2](ClO4)2 | F(000) = 1284 |
Mr = 637.65 | Dx = 1.820 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 22.247 (8) Å | Cell parameters from 25 reflections |
b = 6.888 (2) Å | θ = 7–15° |
c = 15.211 (4) Å | µ = 1.47 mm−1 |
β = 93.07 (1)° | T = 298 K |
V = 2328 (1) Å3 | Block, blue |
Z = 4 | 0.46 × 0.42 × 0.36 mm |
Data collection top
Siemens R3m four-circle diffractometer | 2251 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.025 |
Graphite monochromator | θmax = 29.0°, θmin = 3.1° |
ω scans | h = 0→27 |
Absorption correction: empirical (using intensity measurements) via ψ scan (North et al., 1968) | k = 0→9 |
Tmin = 0.515, Tmax = 0.590 | l = −20→20 |
3006 measured reflections | 2 standard reflections every 150 reflections |
2941 independent reflections | intensity decay: none |
Refinement top
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0648P)2 + 3.7085P] where P = (Fo2 + 2Fc2)/3 |
2941 reflections | (Δ/σ)max < 0.001 |
172 parameters | Δρmax = 0.43 e Å−3 |
3 restraints | Δρmin = −0.76 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.2500 | 0.2500 | 0.0000 | 0.0270 (1) | |
Cl1 | −0.06134 (4) | 0.2108 (2) | 0.12793 (8) | 0.0663 (3) | |
Cl2 | 0.13731 (4) | 0.7126 (1) | 0.19823 (5) | 0.0461 (2) | |
O1 | 0.1651 (1) | 0.2547 (3) | −0.0431 (1) | 0.033 (1) | |
O2 | 0.1772 (2) | 0.5729 (5) | 0.2414 (2) | 0.087 (1) | |
O3 | 0.1558 (2) | 0.9000 (5) | 0.2278 (3) | 0.100 (1) | |
O4 | 0.0773 (2) | 0.6824 (8) | 0.2202 (2) | 0.111 (2) | |
O5 | 0.1401 (1) | 0.6942 (6) | 0.1062 (2) | 0.082 (1) | |
O1W | 0.2281 (1) | 0.2607 (3) | 0.1518 (1) | 0.041 (1) | |
N1 | 0.1109 (1) | 0.1914 (4) | 0.0776 (2) | 0.040 (1) | |
N2 | 0.2508 (1) | 0.5480 (3) | −0.0018 (1) | 0.029 (1) | |
C1 | 0.1143 (1) | 0.2426 (4) | −0.0080 (2) | 0.030 (1) | |
C2 | 0.0586 (1) | 0.2775 (4) | −0.0558 (2) | 0.039 (1) | |
C3 | 0.0052 (1) | 0.2667 (4) | −0.0153 (2) | 0.041 (1) | |
C4 | 0.0056 (1) | 0.2203 (4) | 0.0746 (2) | 0.042 (1) | |
C5 | 0.0583 (1) | 0.1805 (5) | 0.1195 (2) | 0.045 (1) | |
C6 | 0.2178 (1) | 0.6496 (4) | −0.0620 (2) | 0.032 (1) | |
C7 | 0.2831 (1) | 0.6474 (4) | 0.0601 (2) | 0.031 (1) | |
H1W1 | 0.216 (2) | 0.358 (3) | 0.180 (2) | 0.04 (1)* | |
H1W2 | 0.257 (1) | 0.218 (6) | 0.184 (2) | 0.06 (1)* | |
H1N1 | 0.14391) | 0.161 (6) | 0.107 (2) | 0.06 (1)* | |
H2 | 0.0585 | 0.3080 | −0.1154 | 0.046* | |
H3 | −0.0310 | 0.2899 | −0.0470 | 0.049* | |
H5 | 0.0586 | 0.1459 | 0.1787 | 0.054* | |
H6 | 0.1951 | 0.5841 | −0.1057 | 0.038* | |
H7 | 0.3064 | 0.5802 | 0.1025 | 0.037* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0222 (2) | 0.0220 (2) | 0.0365 (2) | −0.0004 (2) | 0.0004 (2) | −0.0009 (2) |
Cl1 | 0.0359 (5) | 0.0923 (8) | 0.0725 (6) | 0.0012 (4) | 0.0186 (4) | 0.0042 (5) |
Cl2 | 0.0435 (4) | 0.0580 (5) | 0.0364 (4) | 0.0060 (3) | −0.0022 (3) | 0.0037 (3) |
O1 | 0.025 (1) | 0.036 (1) | 0.040 (1) | −0.002 (1) | 0.000 (1) | −0.001 (1) |
O2 | 0.127 (3) | 0.069 (2) | 0.061 (2) | 0.047 (2) | −0.038 (2) | −0.012 (1) |
O3 | 0.126 (3) | 0.057 (2) | 0.110 (3) | 0.001 (2) | −0.055 (2) | 0.006 (2) |
O4 | 0.067 (2) | 0.198 (4) | 0.071 (2) | −0.027 (3) | 0.022 (2) | 0.002 (3) |
O5 | 0.058 (2) | 0.153 (3) | 0.036 (1) | 0.019 (2) | 0.002 (1) | 0.009 (2) |
O1W | 0.039 (1) | 0.047 (1) | 0.037 (1) | 0.003 (1) | −0.003 (1) | −0.004 (1) |
N1 | 0.029 (1) | 0.053 (2) | 0.038 (1) | 0.003 (1) | −0.004 (1) | 0.006 (1) |
N2 | 0.029 (1) | 0.022 (1) | 0.036 (1) | −0.001 (1) | 0.000 (1) | −0.001 (1) |
C1 | 0.026 (1) | 0.026 (1) | 0.038 (1) | 0.001 (1) | 0.000 (1) | −0.002 (1) |
C2 | 0.030 (1) | 0.045 (2) | 0.040 (2) | 0.005 (1) | −0.004 (1) | 0.001 (1) |
C3 | 0.029 (1) | 0.049 (2) | 0.045 (2) | 0.005 (1) | −0.006 (1) | −0.003 (1) |
C4 | 0.030 (2) | 0.046 (2) | 0.050 (2) | −0.001 (1) | 0.007 (1) | −0.002 (1) |
C5 | 0.036 (2) | 0.061 (2) | 0.039 (2) | 0.001 (1) | 0.004 (1) | 0.009 (2) |
C6 | 0.034 (1) | 0.025 (1) | 0.036 (1) | −0.001 (1) | −0.004 (1) | −0.003 (1) |
C7 | 0.031 (1) | 0.027 (1) | 0.033 (1) | 0.000 (1) | −0.004 (1) | 0.000 (1) |
Geometric parameters (Å, º) top
Cu1—O1 | 1.967 (2) | C1—C2 | 1.423 (4) |
Cu1—N2 | 2.053 (2) | C2—C3 | 1.370 (4) |
Cu1—O1W | 2.387 (2) | C3—C4 | 1.403 (5) |
Cl1—C4 | 1.736 (3) | C4—C5 | 1.352 (4) |
Cl2—O2 | 1.444 (3) | C6—C7i | 1.399 (4) |
Cl2—O3 | 1.420 (3) | O1W—H1W1 | 0.85 (3) |
Cl2—O4 | 1.409 (3) | O1W—H1W2 | 0.84 (3) |
Cl2—O5 | 1.410 (3) | N1—H1N1 | 0.85 (1) |
O1—C1 | 1.279 (3) | C2—H2 | 0.9300 |
N1—C1 | 1.353 (4) | C3—H3 | 0.9300 |
N1—C5 | 1.365 (4) | C5—H5 | 0.9300 |
N2—C6 | 1.339 (3) | C6—H6 | 0.9300 |
N2—C7 | 1.342 (3) | C7—H7 | 0.9300 |
| | | |
O1—Cu1—O1ii | 180.0 (1) | C2—C3—C4 | 119.3 (3) |
O1—Cu1—O1W | 94.6 (1) | C5—C4—C3 | 120.0 (3) |
O1—Cu1—O1Wii | 85.4 (1) | C5—C4—Cl1 | 119.9 (3) |
O1—Cu1—N2 | 89.3 (1) | C3—C4—Cl1 | 120.2 (2) |
O1—Cu1—N2ii | 90.7 (1) | C4—C5—N1 | 119.5 (3) |
O1W—Cu1—O1Wii | 180.0 (2) | N2—C6—C7i | 121.1 (2) |
O1W—Cu1—N2 | 89.1 (1) | N2—C7—C6i | 121.1 (2) |
O1W—Cu1—N2ii | 90.9 (1) | Cu1—O1W—H1W1 | 126 (2) |
O5—Cl2—O4 | 108.3 (2) | Cu1—O1W—H1W2 | 112 (3) |
O5—Cl2—O3 | 111.6 (2) | H1W1—O1W—H1W2 | 104 (4) |
O4—Cl2—O3 | 108.7 (3) | C1—N1—H1N1 | 119 (3) |
O5—Cl2—O2 | 109.5 (2) | C5—N1—H1N1 | 117 (3) |
O4—Cl2—O2 | 111.2 (3) | C3—C2—H2 | 119.6 |
O3—Cl2—O2 | 107.5 (2) | C1—C2—H2 | 119.6 |
C1—O1—Cu1 | 135.5 (2) | C2—C3—H3 | 120.3 |
C1—N1—C5 | 123.9 (3) | C4—C3—H3 | 120.3 |
C6—N2—C7 | 117.8 (2) | C4—C5—H5 | 120.2 |
C6—N2—Cu1 | 121.8 (2) | N1—C5—H5 | 120.2 |
C7—N2—Cu1 | 120.4 (2) | N2—C6—H6 | 119.5 |
O1—C1—N1 | 121.0 (2) | C7i—C6—H6 | 119.5 |
O1—C1—C2 | 122.6 (3) | N2—C7—H7 | 119.4 |
N1—C1—C2 | 116.3 (3) | C6i—C7—H7 | 119.4 |
C3—C2—C1 | 120.8 (3) | | |
| | | |
N2ii—Cu1—O1—C1 | 82.8 (2) | C5—N1—C1—O1 | 178.3 (3) |
N2—Cu1—O1—C1 | −97.2 (2) | C5—N1—C1—C2 | −2.9 (4) |
O1Wii—Cu1—O1—C1 | 171.8 (2) | O1—C1—C2—C3 | −178.7 (3) |
O1W—Cu1—O1—C1 | −8.2 (2) | N1—C1—C2—C3 | 2.5 (4) |
O1ii—Cu1—N2—C6 | 146.9 (2) | C1—C2—C3—C4 | −0.1 (4) |
O1—Cu1—N2—C6 | −33.1 (2) | C2—C3—C4—C5 | −2.2 (5) |
O1Wii—Cu1—N2—C6 | 52.3 (2) | C2—C3—C4—Cl1 | 178.7 (2) |
O1W—Cu1—N2—C6 | −127.7 (2) | C3—C4—C5—N1 | 1.9 (5) |
O1ii—Cu1—N2—C7 | −35.7 (2) | Cl1—C4—C5—N1 | −178.9 (3) |
O1—Cu1—N2—C7 | 144.3 (2) | C1—N1—C5—C4 | 0.7 (5) |
O1Wii—Cu1—N2—C7 | −130.3 (2) | C7—N2—C6—C7i | −0.2 (4) |
O1W—Cu1—N2—C7 | 49.7 (2) | Cu1—N2—C6—C7i | 177.3 (2) |
Cu1—O1—C1—N1 | −10.2 (4) | C6—N2—C7—C6i | 0.2 (4) |
Cu1—O1—C1—C2 | 171.1 (2) | Cu1—N2—C7—C6i | −177.4 (2) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z; (ii) −x+1/2, −y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2 | 0.85 (3) | 1.97 (3) | 2.816 (4) | 172 (3) |
O1W—H1W2···O2iii | 0.84 (3) | 2.06 (3) | 2.895 (4) | 172 (4) |
N1—H1N1···O1W | 0.85 (1) | 2.10 (3) | 2.826 (3) | 144 (4) |
C7—H7···O1ii | 0.93 | 2.57 | 3.017 (3) | 110 |
Symmetry codes: (ii) −x+1/2, −y+1/2, −z; (iii) −x+1/2, y−1/2, −z+1/2. |
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