metal-organic compounds
In the crystal structure of the yellow copper(I) compound, {[Cu2(SO4)(C10H8N2)2]·4H2O}n, one [(C10H8N2)2Cu]n chain is stacked over another [CuCu = 3.180 (1) Å]; the two chains are bridged by SO4 groups through two Cu—O bonds into a double-chain motif. The SO4 groups are located alternately on opposite sides of the double chain and lie on twofold rotation axes. The disordered solvent water molecules occupy the space between the double chains. The CuI atom exists in a T-shaped environment.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804014801/bt6475sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804014801/bt6475Isup2.hkl |
CCDC reference: 245151
Computing details top
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; 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.
Crystal data top
[Cu2(SO4)(C10H8N2)2]·4H2O | F(000) = 1240 |
Mr = 607.57 | Dx = 1.587 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2789 reflections |
a = 10.825 (1) Å | θ = 2.3–24.7° |
b = 17.316 (1) Å | µ = 1.81 mm−1 |
c = 14.428 (1) Å | T = 298 K |
β = 109.907 (1)° | Block, yellow |
V = 2542.8 (4) Å3 | 0.30 × 0.15 × 0.10 mm |
Z = 4 |
Data collection top
Bruker APEX area-detector diffractometer | 2234 independent reflections |
Radiation source: fine-focus sealed tube | 1449 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
φ and ω scans | θmax = 25.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −12→12 |
Tmin = 0.675, Tmax = 0.840 | k = −20→20 |
11348 measured reflections | l = −17→17 |
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)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.221 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.1121P)2 + 9.1371P] where P = (Fo2 + 2Fc2)/3 |
2234 reflections | (Δ/σ)max = 0.001 |
177 parameters | Δρmax = 1.27 e Å−3 |
48 restraints | Δρmin = −0.41 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.59148 (8) | 0.04495 (5) | 0.18403 (6) | 0.0691 (5) | |
S1 | 0.5000 | 0.2225 (2) | 0.2500 | 0.112 (2) | |
O1 | 0.5777 (6) | 0.1736 (4) | 0.2079 (6) | 0.135 (3) | |
O2 | 0.4114 (6) | 0.2698 (4) | 0.1726 (7) | 0.141 (3) | |
O1w | 0.142 (1) | 0.2934 (9) | 0.156 (1) | 0.125 (5) | 0.50 |
O2w | −0.041 (2) | 0.242 (1) | −0.028 (2) | 0.165 (7) | 0.50 |
O1w' | 0.143 (2) | 0.2463 (9) | 0.066 (1) | 0.146 (7) | 0.50 |
O2w' | −0.272 (2) | 0.2515 (9) | −0.108 (2) | 0.148 (6) | 0.50 |
N1 | 0.7690 (5) | 0.0297 (3) | 0.2672 (4) | 0.057 (1) | |
N2 | 1.4256 (5) | −0.0257 (3) | 0.5863 (4) | 0.061 (2) | |
C1 | 0.8478 (6) | 0.0901 (4) | 0.3077 (5) | 0.072 (2) | |
C2 | 0.9770 (6) | 0.0811 (4) | 0.3657 (6) | 0.071 (2) | |
C3 | 1.0321 (6) | 0.0086 (3) | 0.3877 (4) | 0.050 (2) | |
C4 | 0.9518 (6) | −0.0528 (3) | 0.3466 (5) | 0.061 (2) | |
C5 | 0.8226 (6) | −0.0414 (3) | 0.2884 (5) | 0.061 (2) | |
C6 | 1.3748 (7) | 0.0452 (4) | 0.5632 (6) | 0.069 (2) | |
C7 | 1.2503 (6) | 0.0580 (4) | 0.4990 (6) | 0.071 (2) | |
C8 | 1.1689 (6) | −0.0027 (3) | 0.4527 (4) | 0.051 (2) | |
C9 | 1.2250 (7) | −0.0745 (4) | 0.4728 (6) | 0.081 (3) | |
C10 | 1.3492 (7) | −0.0847 (4) | 0.5382 (6) | 0.083 (3) | |
H1 | 0.8131 | 0.1398 | 0.2958 | 0.087* | |
H2 | 1.0282 | 0.1245 | 0.3905 | 0.085* | |
H4 | 0.9850 | −0.1028 | 0.3582 | 0.073* | |
H5 | 0.7704 | −0.0842 | 0.2628 | 0.074* | |
H6 | 1.4265 | 0.0875 | 0.5919 | 0.083* | |
H7 | 1.2196 | 0.1084 | 0.4862 | 0.085* | |
H9 | 1.1773 | −0.1173 | 0.4412 | 0.097* | |
H10 | 1.3826 | −0.1346 | 0.5500 | 0.099* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0440 (6) | 0.0751 (7) | 0.0585 (6) | −0.0026 (4) | −0.0212 (4) | 0.0032 (4) |
S1 | 0.0493 (15) | 0.0331 (13) | 0.188 (4) | 0.000 | −0.0438 (19) | 0.000 |
O1 | 0.086 (4) | 0.060 (4) | 0.188 (7) | 0.010 (3) | −0.045 (4) | −0.029 (4) |
O2 | 0.066 (4) | 0.079 (4) | 0.226 (8) | 0.010 (3) | −0.017 (4) | 0.057 (5) |
O1w | 0.088 (9) | 0.11 (1) | 0.17 (1) | −0.007 (8) | 0.032 (9) | 0.02 (1) |
O2w | 0.20 (2) | 0.12 (1) | 0.16 (1) | −0.059 (11) | 0.05 (1) | 0.00 (1) |
O1w' | 0.14 (1) | 0.11 (1) | 0.17 (1) | −0.003 (9) | 0.02 (1) | 0.05 (1) |
O2w' | 0.17 (1) | 0.10 (1) | 0.16 (1) | 0.02 (1) | 0.03 (1) | −0.003 (9) |
N1 | 0.046 (3) | 0.059 (3) | 0.044 (3) | 0.002 (2) | −0.013 (2) | −0.006 (2) |
N2 | 0.049 (3) | 0.064 (3) | 0.049 (3) | 0.010 (3) | −0.011 (3) | −0.004 (3) |
C1 | 0.056 (4) | 0.051 (4) | 0.078 (5) | 0.015 (3) | −0.018 (3) | −0.010 (4) |
C2 | 0.049 (4) | 0.051 (4) | 0.081 (5) | 0.004 (3) | −0.020 (3) | −0.014 (4) |
C3 | 0.048 (3) | 0.049 (3) | 0.037 (3) | 0.009 (3) | −0.005 (3) | −0.007 (3) |
C4 | 0.053 (4) | 0.045 (4) | 0.064 (4) | 0.006 (3) | −0.008 (3) | −0.004 (3) |
C5 | 0.053 (4) | 0.052 (4) | 0.057 (4) | 0.001 (3) | −0.010 (3) | −0.002 (3) |
C6 | 0.050 (4) | 0.058 (4) | 0.071 (5) | −0.003 (3) | −0.017 (3) | −0.003 (3) |
C7 | 0.057 (4) | 0.054 (4) | 0.070 (5) | 0.005 (3) | −0.020 (3) | −0.002 (3) |
C8 | 0.043 (3) | 0.053 (4) | 0.039 (3) | 0.011 (3) | −0.009 (3) | −0.005 (3) |
C9 | 0.061 (4) | 0.053 (4) | 0.086 (5) | 0.009 (3) | −0.030 (4) | −0.020 (4) |
C10 | 0.069 (5) | 0.055 (4) | 0.083 (5) | 0.023 (4) | −0.030 (4) | −0.015 (4) |
Geometric parameters (Å, º) top
Cu1—N1 | 1.905 (5) | C3—C8 | 1.471 (8) |
Cu1—N2i | 1.897 (5) | C4—C5 | 1.378 (7) |
Cu1—O1 | 2.266 (6) | C6—C7 | 1.369 (7) |
S1—O1 | 1.463 (8) | C7—C8 | 1.388 (7) |
S1—O1ii | 1.463 (8) | C8—C9 | 1.370 (7) |
S1—O2 | 1.452 (7) | C9—C10 | 1.365 (7) |
S1—O2ii | 1.452 (7) | C1—H1 | 0.93 |
N1—C1 | 1.350 (7) | C2—H2 | 0.93 |
N1—C5 | 1.351 (6) | C4—H4 | 0.93 |
N2—C6 | 1.339 (7) | C5—H5 | 0.93 |
N2—C10 | 1.349 (7) | C6—H6 | 0.93 |
C1—C2 | 1.373 (7) | C7—H7 | 0.93 |
C2—C3 | 1.381 (7) | C9—H9 | 0.93 |
C3—C4 | 1.373 (7) | C10—H10 | 0.93 |
N1—Cu1—N2i | 160.0 (2) | N2—C6—C7 | 122.9 (6) |
N1—Cu1—O1 | 98.3 (2) | C6—C7—C8 | 121.4 (6) |
N2i—Cu1—O1 | 101.0 (2) | C9—C8—C7 | 114.9 (5) |
O2ii—S1—O2 | 111.3 (7) | C9—C8—C3 | 122.2 (5) |
O2ii—S1—O1ii | 109.2 (5) | C7—C8—C3 | 122.9 (5) |
O2—S1—O1ii | 108.9 (4) | C10—C9—C8 | 121.7 (6) |
O2ii—S1—O1 | 108.9 (4) | N2—C10—C9 | 122.9 (6) |
O2—S1—O1 | 109.2 (5) | N1—C1—H1 | 118.7 |
O1ii—S1—O1 | 109.2 (7) | C2—C1—H1 | 118.7 |
S1—O1—Cu1 | 135.2 (5) | C1—C2—H2 | 119.5 |
C1—N1—C5 | 116.6 (5) | C3—C2—H2 | 119.5 |
C1—N1—Cu1 | 121.2 (4) | C3—C4—H4 | 119.5 |
C5—N1—Cu1 | 122.2 (4) | C5—C4—H4 | 119.5 |
C6—N2—C10 | 116.0 (6) | N1—C5—H5 | 118.7 |
C6—N2—Cu1iii | 123.4 (4) | C4—C5—H5 | 118.7 |
C10—N2—Cu1iii | 120.6 (4) | N2—C6—H6 | 118.6 |
N1—C1—C2 | 122.6 (6) | C7—C6—H6 | 118.6 |
C1—C2—C3 | 120.9 (6) | C6—C7—H7 | 119.3 |
C4—C3—C2 | 116.4 (5) | C8—C7—H7 | 119.3 |
C4—C3—C8 | 121.7 (5) | C10—C9—H9 | 119.1 |
C2—C3—C8 | 122.0 (5) | C8—C9—H9 | 119.1 |
C3—C4—C5 | 120.9 (6) | N2—C10—H10 | 118.5 |
N1—C5—C4 | 122.5 (6) | C9—C10—H10 | 118.5 |
O2ii—S1—O1—Cu1 | 124.9 (6) | Cu1—N1—C5—C4 | 178.4 (6) |
O2—S1—O1—Cu1 | −113.3 (6) | C3—C4—C5—N1 | 1 (1) |
O1ii—S1—O1—Cu1 | 5.6 (3) | C10—N2—C6—C7 | 4 (1) |
N2i—Cu1—O1—S1 | 68.1 (6) | Cu1iii—N2—C6—C7 | −174.0 (6) |
N1—Cu1—O1—S1 | −116.9 (6) | N2—C6—C7—C8 | −1 (1) |
N2i—Cu1—N1—C1 | 157.2 (7) | C6—C7—C8—C9 | −3 (1) |
O1—Cu1—N1—C1 | −8.3 (7) | C6—C7—C8—C3 | 176.5 (7) |
N2i—Cu1—N1—C5 | −23 (1) | C4—C3—C8—C9 | 3 (1) |
O1—Cu1—N1—C5 | 171.9 (6) | C2—C3—C8—C9 | −178.4 (8) |
C5—N1—C1—C2 | 2 (1) | C4—C3—C8—C7 | −176.8 (7) |
Cu1—N1—C1—C2 | −178.2 (7) | C2—C3—C8—C7 | 2 (1) |
N1—C1—C2—C3 | −2 (1) | C7—C8—C9—C10 | 4 (1) |
C1—C2—C3—C4 | 2 (1) | C3—C8—C9—C10 | −175.8 (8) |
C1—C2—C3—C8 | −177.6 (7) | C6—N2—C10—C9 | −3 (1) |
C2—C3—C4—C5 | −1 (1) | Cu1iii—N2—C10—C9 | 174.8 (7) |
C8—C3—C4—C5 | 177.9 (7) | C8—C9—C10—N2 | −1 (1) |
C1—N1—C5—C4 | −1 (1) |
Symmetry codes: (i) x−1, −y, z−1/2; (ii) −x+1, y, −z+1/2; (iii) x+1, −y, z+1/2. |