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In the title complex, [Cu(C6H4FN2O4)2(H2O)4]·4H2O, the Cu atom is located in the centre of a distorted octahedral geometry. The coordination atoms are six O atoms provided by two carboxylate groups [coordinated in a monodentate mode, with Cu-O = 1.9551 (10) Å] and four water molecules [Cu-O = 1.9241 (13) and 2.5771 (14) Å]. In addition, one intramolecular hydrogen bond and ten intermolecular hydrogen bonds make up a three-dimensional network.
Supporting information
CCDC reference: 153927
Data collection: CAD-4-PC (Enraf-Nonius, 1989); cell refinement: CAD-4-PC; data reduction: TEXSAN (Molecular Structure Corporation, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
Tetraaqua(5-fluoro-uracil-1-acetato-O)-copper (II) tetrahydrate
top
Crystal data top
[Cu(C6H4FN2O4)2(H2O)4]·4H2O | F(000) = 598 |
Mr = 581.89 | Dx = 1.745 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 8.304 (1) Å | Cell parameters from 150 reflections |
b = 12.044 (2) Å | θ = 16.1–16.9° |
c = 11.082 (2) Å | µ = 1.09 mm−1 |
β = 92.47 (1)° | T = 293 K |
V = 1107.3 (3) Å3 | Prismatic, blue |
Z = 2 | 0.30 × 0.15 × 0.10 mm |
Data collection top
Enraf-nonius CAD-4 diffractometer | 1838 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.0 |
Graphite monochromator | θmax = 25.0°, θmin = 2.5° |
ω/2θ scans | h = −9→9 |
Absorption correction: ψ scan (TEXSAN; Molecular Structure Corporation, 1989) | k = 0→14 |
Tmin = 0.851, Tmax = 0.897 | l = 0→13 |
1941 measured reflections | 3 standard reflections every 400 reflections |
1941 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)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.056 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.020P)2 + 0.444P] where P = (Fo2 + 2Fc2)/3 |
1941 reflections | (Δ/σ)max < 0.001 |
160 parameters | Δρmax = 0.29 e Å−3 |
34 restraints | Δρmin = −0.34 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu | 0.5000 | 0.0000 | 0.0000 | 0.02271 (10) | |
O1 | 0.38908 (15) | 0.10354 (12) | 0.18221 (11) | 0.0403 (3) | |
H1A | 0.310 (2) | 0.122 (2) | 0.158 (2) | 0.060* | |
H1B | 0.380 (3) | 0.083 (2) | 0.2383 (15) | 0.060* | |
O2 | 0.39173 (16) | −0.13307 (11) | 0.04805 (12) | 0.0411 (3) | |
H2A | 0.395 (3) | −0.1775 (17) | 0.007 (2) | 0.062* | |
H2B | 0.3063 (19) | −0.122 (2) | 0.051 (2) | 0.062* | |
O3 | 0.67913 (12) | −0.03487 (9) | 0.11398 (9) | 0.0267 (2) | |
O4 | 0.85492 (13) | −0.10260 (10) | −0.01351 (9) | 0.0349 (3) | |
O5 | 0.97799 (14) | 0.11773 (9) | 0.29680 (10) | 0.0339 (3) | |
O6 | 0.67100 (17) | 0.03682 (10) | 0.61472 (11) | 0.0439 (3) | |
N1 | 0.87716 (14) | −0.05803 (10) | 0.30885 (10) | 0.0230 (3) | |
N2 | 0.82678 (15) | 0.07368 (10) | 0.45618 (11) | 0.0264 (3) | |
H2 | 0.8433 | 0.1392 | 0.4850 | 0.032* | |
F | 0.62339 (16) | −0.17610 (10) | 0.52978 (12) | 0.0625 (4) | |
C1 | 0.81274 (16) | −0.07439 (11) | 0.08810 (12) | 0.0207 (3) | |
C2 | 0.93783 (17) | −0.08952 (13) | 0.19217 (12) | 0.0250 (3) | |
H2C | 0.9712 | −0.1667 | 0.1954 | 0.030* | |
H2D | 1.0320 | −0.0449 | 0.1766 | 0.030* | |
C3 | 0.89914 (17) | 0.04936 (12) | 0.34906 (12) | 0.0227 (3) | |
C4 | 0.7316 (2) | 0.00494 (12) | 0.52158 (14) | 0.0291 (3) | |
C5 | 0.7137 (2) | −0.10399 (13) | 0.47033 (16) | 0.0339 (4) | |
C6 | 0.78282 (19) | −0.13151 (13) | 0.36918 (14) | 0.0301 (3) | |
H6 | 0.7671 | −0.2026 | 0.3380 | 0.036* | |
O7 | 0.87955 (14) | 0.21563 (10) | 0.06382 (10) | 0.0304 (2) | |
H7A | 0.867 (2) | 0.2082 (18) | 0.1282 (13) | 0.046* | |
H7B | 0.950 (2) | 0.1856 (17) | 0.0536 (19) | 0.046* | |
O8 | 0.37913 (18) | −0.23677 (12) | 0.25723 (12) | 0.0450 (3) | |
H8A | 0.343 (3) | −0.1991 (19) | 0.298 (2) | 0.068* | |
H8B | 0.458 (2) | −0.249 (2) | 0.287 (2) | 0.068* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu | 0.01960 (14) | 0.02279 (15) | 0.02554 (15) | 0.00225 (9) | −0.00148 (10) | 0.00515 (9) |
O1 | 0.0378 (7) | 0.0507 (8) | 0.0322 (6) | −0.0040 (6) | 0.0007 (5) | 0.0129 (6) |
O2 | 0.0419 (7) | 0.0391 (7) | 0.0413 (7) | −0.0105 (6) | −0.0092 (6) | 0.0115 (5) |
O3 | 0.0231 (5) | 0.0343 (6) | 0.0227 (5) | 0.0086 (4) | 0.0007 (4) | 0.0001 (4) |
O4 | 0.0342 (6) | 0.0483 (7) | 0.0221 (5) | 0.0099 (5) | −0.0003 (4) | −0.0069 (5) |
O5 | 0.0437 (6) | 0.0303 (6) | 0.0286 (5) | −0.0078 (5) | 0.0111 (5) | 0.0054 (5) |
O6 | 0.0649 (8) | 0.0339 (6) | 0.0352 (7) | 0.0055 (6) | 0.0273 (6) | 0.0032 (5) |
N1 | 0.0259 (6) | 0.0227 (6) | 0.0202 (6) | 0.0036 (5) | −0.0006 (5) | 0.0002 (5) |
N2 | 0.0384 (7) | 0.0188 (6) | 0.0226 (6) | −0.0014 (5) | 0.0062 (5) | −0.0008 (5) |
F | 0.0824 (9) | 0.0397 (6) | 0.0686 (8) | −0.0246 (6) | 0.0396 (7) | 0.0015 (6) |
C1 | 0.0256 (7) | 0.0158 (6) | 0.0207 (7) | −0.0007 (5) | 0.0016 (5) | 0.0009 (5) |
C2 | 0.0251 (7) | 0.0275 (8) | 0.0227 (7) | 0.0069 (6) | 0.0024 (6) | −0.0036 (6) |
C3 | 0.0261 (7) | 0.0220 (7) | 0.0197 (6) | 0.0023 (6) | −0.0016 (5) | 0.0018 (5) |
C4 | 0.0333 (8) | 0.0273 (8) | 0.0270 (8) | 0.0008 (6) | 0.0047 (6) | 0.0062 (6) |
C5 | 0.0383 (9) | 0.0233 (8) | 0.0411 (9) | −0.0084 (6) | 0.0128 (7) | 0.0051 (7) |
C6 | 0.0359 (8) | 0.0208 (7) | 0.0337 (8) | −0.0038 (6) | 0.0016 (6) | −0.0008 (6) |
O7 | 0.0341 (6) | 0.0312 (6) | 0.0262 (5) | 0.0029 (5) | 0.0058 (5) | 0.0059 (5) |
O8 | 0.0581 (8) | 0.0416 (8) | 0.0358 (7) | 0.0087 (6) | 0.0069 (6) | 0.0045 (6) |
Geometric parameters (Å, º) top
Cu—O2 | 1.9241 (13) | N1—C2 | 1.4580 (18) |
Cu—O2i | 1.9241 (13) | N2—C4 | 1.373 (2) |
Cu—O3i | 1.9551 (10) | N2—C3 | 1.3847 (19) |
Cu—O3 | 1.9551 (10) | N2—H2 | 0.8600 |
Cu—O1 | 2.5771 (14) | F—C5 | 1.3391 (18) |
O1—H1A | 0.734 (14) | C1—C2 | 1.5295 (19) |
O1—H1B | 0.675 (14) | C2—H2C | 0.9700 |
O2—H2A | 0.705 (14) | C2—H2D | 0.9700 |
O2—H2B | 0.725 (14) | C4—C5 | 1.435 (2) |
O3—C1 | 1.2519 (17) | C5—C6 | 1.323 (2) |
O4—C1 | 1.2409 (17) | C6—H6 | 0.9300 |
O5—C3 | 1.2144 (18) | O7—H7A | 0.732 (14) |
O6—C4 | 1.229 (2) | O7—H7B | 0.698 (14) |
N1—C6 | 1.374 (2) | O8—H8A | 0.718 (14) |
N1—C3 | 1.378 (2) | O8—H8B | 0.738 (14) |
| | | |
O2—Cu—O2i | 180.00 (4) | O4—C1—O3 | 126.84 (13) |
O2—Cu—O3i | 90.35 (5) | O4—C1—C2 | 116.26 (12) |
O2i—Cu—O3i | 89.65 (5) | O3—C1—C2 | 116.90 (12) |
O2—Cu—O3 | 89.65 (5) | N1—C2—C1 | 112.85 (11) |
O2i—Cu—O3 | 90.35 (5) | N1—C2—H2C | 109.0 |
O3i—Cu—O3 | 180.00 (8) | C1—C2—H2C | 109.0 |
O2—Cu—O1 | 89.95 (5) | N1—C2—H2D | 109.0 |
O2i—Cu—O1 | 90.05 (5) | C1—C2—H2D | 109.0 |
O3i—Cu—O1 | 96.58 (4) | H2C—C2—H2D | 107.8 |
O3—Cu—O1 | 83.42 (4) | O5—C3—N1 | 123.29 (13) |
Cu—O1—H1A | 101.8 (19) | O5—C3—N2 | 121.89 (13) |
Cu—O1—H1B | 127 (2) | N1—C3—N2 | 114.81 (12) |
H1A—O1—H1B | 109 (2) | O6—C4—N2 | 121.38 (14) |
Cu—O2—H2A | 115 (2) | O6—C4—C5 | 125.38 (15) |
Cu—O2—H2B | 109 (2) | N2—C4—C5 | 113.23 (14) |
H2A—O2—H2B | 104 (2) | C6—C5—F | 121.79 (15) |
C1—O3—Cu | 126.21 (9) | C6—C5—C4 | 121.54 (14) |
C6—N1—C3 | 121.16 (12) | F—C5—C4 | 116.67 (14) |
C6—N1—C2 | 119.33 (12) | C5—C6—N1 | 121.87 (14) |
C3—N1—C2 | 119.02 (12) | C5—C6—H6 | 119.1 |
C4—N2—C3 | 127.30 (13) | N1—C6—H6 | 119.1 |
C4—N2—H2 | 116.3 | H7A—O7—H7B | 104 (2) |
C3—N2—H2 | 116.3 | H8A—O8—H8B | 103 (2) |
| | | |
O2—Cu—O3—C1 | 102.87 (13) | C2—N1—C3—N2 | 175.26 (11) |
O2i—Cu—O3—C1 | −77.13 (13) | C4—N2—C3—O5 | 178.02 (15) |
O3i—Cu—O3—C1 | −116.00 (10) | C4—N2—C3—N1 | −3.3 (2) |
O1—Cu—O3—C1 | −167.14 (12) | C3—N2—C4—O6 | −178.49 (15) |
Cu—O3—C1—O4 | −2.8 (2) | C3—N2—C4—C5 | 2.0 (2) |
Cu—O3—C1—C2 | 177.08 (9) | O6—C4—C5—C6 | 179.79 (17) |
C6—N1—C2—C1 | 80.72 (16) | N2—C4—C5—C6 | −0.7 (2) |
C3—N1—C2—C1 | −91.41 (15) | O6—C4—C5—F | −0.1 (3) |
O4—C1—C2—N1 | −178.05 (13) | N2—C4—C5—F | 179.47 (15) |
O3—C1—C2—N1 | 2.05 (18) | F—C5—C6—N1 | −179.18 (15) |
C6—N1—C3—O5 | −178.02 (14) | C4—C5—C6—N1 | 1.0 (3) |
C2—N1—C3—O5 | −6.0 (2) | C3—N1—C6—C5 | −2.4 (2) |
C6—N1—C3—N2 | 3.28 (19) | C2—N1—C6—C5 | −174.35 (15) |
Symmetry code: (i) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O5 | 0.73 (1) | 2.32 (2) | 2.9228 (16) | 141 (2) |
O1—H1A···O4i | 0.73 (1) | 2.08 (2) | 2.6971 (17) | 143 (3) |
O1—H1B···O6ii | 0.68 (1) | 2.23 (2) | 2.8753 (17) | 160 (3) |
O2—H2A···Fiii | 0.71 (1) | 2.59 (2) | 3.0096 (19) | 120 (2) |
O2—H2B···O7i | 0.73 (1) | 2.26 (2) | 2.7128 (17) | 121 (2) |
N2—H2···O7iv | 0.86 | 1.97 | 2.8300 (17) | 176 |
O7—H7A···O8v | 0.73 (1) | 2.54 (2) | 3.0402 (18) | 127 (2) |
O7—H7B···O4vi | 0.70 (1) | 1.97 (1) | 2.6706 (16) | 176 (2) |
O8—H8A···O6ii | 0.72 (1) | 2.18 (2) | 2.8350 (19) | 151 (3) |
O8—H8A···O7vii | 0.72 (1) | 2.65 (2) | 3.0402 (18) | 116 (2) |
O8—H8B···O1vii | 0.74 (1) | 2.20 (2) | 2.783 (2) | 137 (3) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y, −z+1; (iii) x, −y−1/2, z−1/2; (iv) x, −y+1/2, z+1/2; (v) −x+1, y+1/2, −z+1/2; (vi) −x+2, −y, −z; (vii) −x+1, y−1/2, −z+1/2. |
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