metal-organic compounds
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Redetermination of chlorido(2,2′:6′,2′′-terpyridine-κ3N,N′,N′′)gold(I) dichloride trihydrate at 173 K
aSchool of Chemistry, University of KwaZulu-Natal, Westville Campus, Private Bag X54001, Durban 4000, South Africa
*Correspondence e-mail: maguireg@ukzn.ac.za
The redetermined structure of the title compound, [AuCl(C15H11N3)]Cl2·3H2O, at 173 (2) K is reported. The structure displays O—H⋯Cl and O—H⋯O hydrogen bonding. The distance of one of the chloride ions from the gold(I) atom [5.047 (1) Å] differs from that determined previously.
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2005); cell SAINT-NT (Bruker, 2005); data reduction: SAINT-NT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536808027943/ez2137sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808027943/ez2137Isup2.hkl
A mixture of AuCl4.3H2O (0.100 g, 0.29 mmol) and terpyridine (0.072 g, 0.31 mmol) was placed in 10 ml of deionized water in a round-bottom flask. The solution pH was adjusted to 3.0 with 1 M NaOH, and the resulting mixture refluxed at 100°C for 24 h. The red mixture was then cooled to room temperature and filtered to remove small amounts of a purple solid. The filtrate obtained was allowed to stand at room temperature to induce precipitation of the crystalline product. The crystals were filtered off and air-dried to yield the title compound. (0.013 g, 7.5%), mp 503 K. 1H NMR [DMSO, 600 MHz]: δ = 8.07 (t, 2H), 8.13 (t, 1H), 8.47 (d, 2H), 8.66 (t, 2H), 8.67 (d, 2H), 8.71 (d, 2H). IR (KBr, cm-1): 3341, 1604, 1584, 1035. 13C NMR [DMSO, 150 MHz]: δ = 151.8, 151.5, 146.8, 141.5, 139.7, 126.0, 122.8, 122.7.
Hydrogen atoms were positioned geometrically and allowed to ride on their respective parent atoms, with C—H bond lengths of 0.93 Å (CH) in a riding model with Uiso(H) = 1.2Ueq(X) for X = CH.
Data collection: APEX2 (Bruker, 2005); cell
SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. The asymmetric unit of I. Displacement ellipsoids are drawn at the 40% probability level. The labelling of atoms is as shown, and is identical to that of Hollis & Lippard. The two chloride counter ions and the three water molecules associated with I are evident, present above and below the plane of the molecule. | |
Fig. 2. Intermolecular hydrogen bonding present in I, shown by the dashed lines. Hanging dashed lines indicate bonding to an adjacent unit cell. Displacement ellipsoids are drawn at the 40% probability level. Protons belonging to individual molecules have been omitted for purposes of clarity. The water and the chloride ions are seen to be found between the individual molecules of I. |
[AuCl(C15H11N3)]Cl2·3H2O | F(000) = 1128 |
Mr = 590.63 | Dx = 2.142 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8408 reflections |
a = 8.4486 (1) Å | θ = 3.8–28.3° |
b = 6.9766 (1) Å | µ = 8.49 mm−1 |
c = 31.1581 (6) Å | T = 173 K |
β = 94.392 (1)° | Block, brown |
V = 1831.14 (5) Å3 | 0.41 × 0.31 × 0.30 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 4386 independent reflections |
Radiation source: fine-focus sealed tube | 4157 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
ϕ and ω scans | θmax = 28.0°, θmin = 3.5° |
Absorption correction: integration [Face-indexed absorption corrections carried out with XPREP (Bruker, 2005)] | h = −11→11 |
Tmin = 0.128, Tmax = 0.185 | k = −9→8 |
13022 measured reflections | l = −41→39 |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.37 | w = 1/[σ2(Fo2) + (0.0093P)2 + 4.719P] where P = (Fo2 + 2Fc2)/3 |
4386 reflections | (Δ/σ)max = 0.001 |
226 parameters | Δρmax = 1.32 e Å−3 |
0 restraints | Δρmin = −2.24 e Å−3 |
[AuCl(C15H11N3)]Cl2·3H2O | V = 1831.14 (5) Å3 |
Mr = 590.63 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.4486 (1) Å | µ = 8.49 mm−1 |
b = 6.9766 (1) Å | T = 173 K |
c = 31.1581 (6) Å | 0.41 × 0.31 × 0.30 mm |
β = 94.392 (1)° |
Bruker APEXII CCD area-detector diffractometer | 4386 independent reflections |
Absorption correction: integration [Face-indexed absorption corrections carried out with XPREP (Bruker, 2005)] | 4157 reflections with I > 2σ(I) |
Tmin = 0.128, Tmax = 0.185 | Rint = 0.034 |
13022 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.37 | Δρmax = 1.32 e Å−3 |
4386 reflections | Δρmin = −2.24 e Å−3 |
226 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 | ||
C1 | −0.0770 (6) | 0.2047 (7) | 0.02507 (15) | 0.0253 (10) | |
H1 | −0.0237 | 0.2331 | 0.0001 | 0.030* | |
C2 | −0.2269 (6) | 0.1252 (7) | 0.02079 (17) | 0.0298 (11) | |
H2 | −0.2766 | 0.0986 | −0.0069 | 0.036* | |
C3 | −0.3033 (6) | 0.0848 (7) | 0.05707 (17) | 0.0298 (11) | |
H3 | −0.4064 | 0.0297 | 0.0545 | 0.036* | |
C4 | −0.2298 (5) | 0.1246 (7) | 0.09735 (16) | 0.0248 (10) | |
H4 | −0.2823 | 0.0976 | 0.1225 | 0.030* | |
C5 | −0.0803 (5) | 0.2036 (6) | 0.10059 (15) | 0.0204 (9) | |
C6 | 0.0097 (5) | 0.2552 (6) | 0.14095 (14) | 0.0196 (9) | |
C7 | −0.0305 (5) | 0.2284 (7) | 0.18273 (15) | 0.0261 (10) | |
H7 | −0.1293 | 0.1721 | 0.1882 | 0.031* | |
C8 | 0.0750 (6) | 0.2845 (8) | 0.21643 (16) | 0.0290 (11) | |
H8 | 0.0478 | 0.2669 | 0.2452 | 0.035* | |
C9 | 0.2201 (6) | 0.3663 (7) | 0.20891 (15) | 0.0265 (10) | |
H9 | 0.2926 | 0.4037 | 0.2322 | 0.032* | |
C10 | 0.2570 (5) | 0.3922 (6) | 0.16673 (15) | 0.0203 (9) | |
C11 | 0.4020 (5) | 0.4747 (6) | 0.15124 (15) | 0.0209 (9) | |
C12 | 0.5251 (5) | 0.5513 (7) | 0.17706 (17) | 0.0272 (10) | |
H12 | 0.5194 | 0.5570 | 0.2074 | 0.033* | |
C13 | 0.6570 (5) | 0.6197 (7) | 0.15853 (18) | 0.0305 (11) | |
H13 | 0.7427 | 0.6729 | 0.1762 | 0.037* | |
C14 | 0.6651 (5) | 0.6113 (7) | 0.11450 (18) | 0.0287 (11) | |
H14 | 0.7564 | 0.6564 | 0.1016 | 0.034* | |
C15 | 0.5375 (5) | 0.5358 (7) | 0.08946 (17) | 0.0250 (10) | |
H15 | 0.5408 | 0.5313 | 0.0591 | 0.030* | |
Cl1 | 0.28844 (15) | 0.3714 (2) | 0.00827 (4) | 0.0321 (3) | |
Cl2 | 0.06873 (13) | 0.75596 (17) | 0.08334 (4) | 0.0268 (2) | |
Cl3 | 0.56001 (14) | 0.06210 (19) | 0.19728 (4) | 0.0298 (3) | |
Au1 | 0.211462 (19) | 0.35966 (2) | 0.076389 (5) | 0.01864 (6) | |
N1 | −0.0062 (4) | 0.2421 (5) | 0.06372 (12) | 0.0206 (8) | |
N2 | 0.1517 (4) | 0.3343 (5) | 0.13536 (11) | 0.0162 (7) | |
N3 | 0.4098 (4) | 0.4693 (5) | 0.10746 (12) | 0.0200 (8) | |
O1W | 0.3810 (4) | −0.0056 (6) | 0.10320 (13) | 0.0384 (9) | |
H1A | 0.3000 | −0.0750 | 0.1021 | 0.058* | |
H1B | 0.4060 | 0.0050 | 0.1296 | 0.058* | |
O2W | 0.0068 (4) | 0.7688 (7) | 0.18143 (12) | 0.0422 (10) | |
H2A | 0.0261 | 0.7780 | 0.1555 | 0.063* | |
H2B | 0.0931 | 0.7980 | 0.1949 | 0.063* | |
O3W | 0.2720 (4) | 0.8576 (6) | 0.23548 (13) | 0.0449 (10) | |
H3A | 0.3421 | 0.9059 | 0.2213 | 0.067* | |
H3B | 0.3221 | 0.7749 | 0.2508 | 0.067* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.027 (2) | 0.028 (3) | 0.021 (2) | −0.0037 (19) | 0.0037 (18) | 0.002 (2) |
C2 | 0.028 (2) | 0.028 (3) | 0.033 (3) | −0.006 (2) | −0.003 (2) | −0.004 (2) |
C3 | 0.024 (2) | 0.026 (3) | 0.039 (3) | −0.0032 (19) | 0.002 (2) | −0.002 (2) |
C4 | 0.021 (2) | 0.021 (2) | 0.033 (3) | −0.0039 (18) | 0.0076 (18) | −0.001 (2) |
C5 | 0.021 (2) | 0.015 (2) | 0.025 (2) | 0.0008 (16) | 0.0039 (17) | 0.0019 (18) |
C6 | 0.0170 (19) | 0.017 (2) | 0.026 (2) | 0.0012 (16) | 0.0065 (17) | 0.0039 (18) |
C7 | 0.024 (2) | 0.030 (3) | 0.025 (2) | −0.0022 (19) | 0.0101 (19) | 0.001 (2) |
C8 | 0.033 (3) | 0.035 (3) | 0.019 (2) | 0.001 (2) | 0.0074 (19) | 0.002 (2) |
C9 | 0.027 (2) | 0.031 (3) | 0.021 (2) | 0.002 (2) | 0.0013 (18) | −0.001 (2) |
C10 | 0.021 (2) | 0.016 (2) | 0.024 (2) | 0.0010 (16) | 0.0032 (17) | 0.0017 (18) |
C11 | 0.020 (2) | 0.018 (2) | 0.025 (2) | 0.0020 (16) | 0.0048 (17) | 0.0004 (18) |
C12 | 0.023 (2) | 0.026 (3) | 0.032 (3) | 0.0007 (19) | −0.0009 (19) | 0.000 (2) |
C13 | 0.018 (2) | 0.024 (3) | 0.049 (3) | −0.0013 (18) | −0.001 (2) | −0.001 (2) |
C14 | 0.018 (2) | 0.020 (3) | 0.048 (3) | −0.0018 (17) | 0.008 (2) | 0.001 (2) |
C15 | 0.022 (2) | 0.021 (2) | 0.033 (3) | −0.0013 (18) | 0.0076 (19) | 0.001 (2) |
Cl1 | 0.0363 (6) | 0.0386 (7) | 0.0230 (6) | −0.0093 (5) | 0.0120 (5) | −0.0003 (5) |
Cl2 | 0.0285 (5) | 0.0258 (6) | 0.0260 (6) | 0.0037 (4) | 0.0015 (4) | 0.0004 (5) |
Cl3 | 0.0263 (5) | 0.0290 (6) | 0.0344 (6) | −0.0015 (5) | 0.0044 (5) | 0.0023 (5) |
Au1 | 0.01834 (8) | 0.01925 (9) | 0.01896 (9) | −0.00206 (7) | 0.00558 (6) | 0.00098 (7) |
N1 | 0.0188 (17) | 0.019 (2) | 0.024 (2) | −0.0018 (14) | 0.0045 (15) | 0.0004 (16) |
N2 | 0.0180 (16) | 0.0136 (18) | 0.0175 (17) | 0.0029 (13) | 0.0040 (13) | 0.0000 (14) |
N3 | 0.0181 (17) | 0.0163 (19) | 0.026 (2) | −0.0003 (14) | 0.0027 (15) | 0.0003 (16) |
O1W | 0.0303 (19) | 0.043 (2) | 0.042 (2) | −0.0015 (17) | 0.0029 (16) | 0.0090 (19) |
O2W | 0.0289 (18) | 0.068 (3) | 0.030 (2) | −0.0122 (19) | 0.0052 (15) | −0.003 (2) |
O3W | 0.0305 (19) | 0.061 (3) | 0.042 (2) | −0.0077 (19) | −0.0007 (17) | 0.013 (2) |
C1—N1 | 1.329 (6) | C11—N3 | 1.371 (6) |
C1—C2 | 1.380 (6) | C11—C12 | 1.373 (7) |
C1—H1 | 0.9500 | C12—C13 | 1.379 (7) |
C2—C3 | 1.373 (7) | C12—H12 | 0.9500 |
C2—H2 | 0.9500 | C13—C14 | 1.380 (8) |
C3—C4 | 1.385 (7) | C13—H13 | 0.9500 |
C3—H3 | 0.9500 | C14—C15 | 1.386 (7) |
C4—C5 | 1.375 (6) | C14—H14 | 0.9500 |
C4—H4 | 0.9500 | C15—N3 | 1.336 (5) |
C5—N1 | 1.376 (6) | C15—H15 | 0.9500 |
C5—C6 | 1.463 (6) | Cl1—Au1 | 2.2686 (11) |
C6—N2 | 1.345 (5) | Au1—N2 | 1.950 (3) |
C6—C7 | 1.383 (6) | Au1—N3 | 2.021 (4) |
C7—C8 | 1.381 (7) | Au1—N1 | 2.025 (4) |
C7—H7 | 0.9500 | O1W—H1A | 0.8369 |
C8—C9 | 1.388 (7) | O1W—H1B | 0.8373 |
C8—H8 | 0.9500 | O2W—H2A | 0.8388 |
C9—C10 | 1.386 (6) | O2W—H2B | 0.8381 |
C9—H9 | 0.9500 | O3W—H3A | 0.8361 |
C10—N2 | 1.333 (6) | O3W—H3B | 0.8423 |
C10—C11 | 1.468 (6) | ||
N1—C1—C2 | 120.8 (4) | C12—C11—C10 | 125.0 (4) |
N1—C1—H1 | 119.6 | C11—C12—C13 | 119.3 (5) |
C2—C1—H1 | 119.6 | C11—C12—H12 | 120.3 |
C3—C2—C1 | 119.3 (5) | C13—C12—H12 | 120.3 |
C3—C2—H2 | 120.4 | C12—C13—C14 | 120.3 (5) |
C1—C2—H2 | 120.4 | C12—C13—H13 | 119.8 |
C2—C3—C4 | 119.9 (5) | C14—C13—H13 | 119.8 |
C2—C3—H3 | 120.1 | C13—C14—C15 | 118.7 (4) |
C4—C3—H3 | 120.1 | C13—C14—H14 | 120.7 |
C5—C4—C3 | 119.5 (4) | C15—C14—H14 | 120.7 |
C5—C4—H4 | 120.2 | N3—C15—C14 | 120.9 (5) |
C3—C4—H4 | 120.2 | N3—C15—H15 | 119.5 |
C4—C5—N1 | 119.4 (4) | C14—C15—H15 | 119.5 |
C4—C5—C6 | 125.1 (4) | N2—Au1—N3 | 81.25 (15) |
N1—C5—C6 | 115.5 (4) | N2—Au1—N1 | 81.39 (15) |
N2—C6—C7 | 117.6 (4) | N3—Au1—N1 | 162.64 (15) |
N2—C6—C5 | 113.6 (4) | N2—Au1—Cl1 | 176.48 (11) |
C7—C6—C5 | 128.9 (4) | N3—Au1—Cl1 | 98.51 (11) |
C8—C7—C6 | 119.2 (4) | N1—Au1—Cl1 | 98.82 (11) |
C8—C7—H7 | 120.4 | C1—N1—C5 | 121.1 (4) |
C6—C7—H7 | 120.4 | C1—N1—Au1 | 126.5 (3) |
C7—C8—C9 | 121.0 (4) | C5—N1—Au1 | 112.4 (3) |
C7—C8—H8 | 119.5 | C10—N2—C6 | 125.6 (4) |
C9—C8—H8 | 119.5 | C10—N2—Au1 | 117.2 (3) |
C10—C9—C8 | 118.7 (4) | C6—N2—Au1 | 117.2 (3) |
C10—C9—H9 | 120.7 | C15—N3—C11 | 120.7 (4) |
C8—C9—H9 | 120.7 | C15—N3—Au1 | 126.7 (3) |
N2—C10—C9 | 118.0 (4) | C11—N3—Au1 | 112.7 (3) |
N2—C10—C11 | 113.9 (4) | H1A—O1W—H1B | 103.6 |
C9—C10—C11 | 128.1 (4) | H2A—O2W—H2B | 103.8 |
N3—C11—C12 | 120.1 (4) | H3A—O3W—H3B | 103.3 |
N3—C11—C10 | 114.9 (4) | ||
N1—C1—C2—C3 | 0.1 (8) | N2—Au1—N1—C1 | 178.4 (4) |
C1—C2—C3—C4 | 0.2 (8) | N3—Au1—N1—C1 | 178.2 (4) |
C2—C3—C4—C5 | −0.3 (7) | Cl1—Au1—N1—C1 | −5.1 (4) |
C3—C4—C5—N1 | 0.1 (7) | N2—Au1—N1—C5 | −0.9 (3) |
C3—C4—C5—C6 | 179.1 (4) | N3—Au1—N1—C5 | −1.1 (7) |
C4—C5—C6—N2 | −178.5 (4) | Cl1—Au1—N1—C5 | 175.6 (3) |
N1—C5—C6—N2 | 0.5 (6) | C9—C10—N2—C6 | 1.3 (7) |
C4—C5—C6—C7 | 3.4 (8) | C11—C10—N2—C6 | −179.6 (4) |
N1—C5—C6—C7 | −177.6 (5) | C9—C10—N2—Au1 | −176.8 (3) |
N2—C6—C7—C8 | 0.5 (7) | C11—C10—N2—Au1 | 2.3 (5) |
C5—C6—C7—C8 | 178.5 (5) | C7—C6—N2—C10 | −1.1 (7) |
C6—C7—C8—C9 | −0.2 (8) | C5—C6—N2—C10 | −179.4 (4) |
C7—C8—C9—C10 | 0.5 (8) | C7—C6—N2—Au1 | 177.0 (3) |
C8—C9—C10—N2 | −1.0 (7) | C5—C6—N2—Au1 | −1.3 (5) |
C8—C9—C10—C11 | −179.9 (5) | N3—Au1—N2—C10 | −0.6 (3) |
N2—C10—C11—N3 | −3.5 (6) | N1—Au1—N2—C10 | 179.5 (3) |
C9—C10—C11—N3 | 175.5 (4) | N3—Au1—N2—C6 | −178.9 (3) |
N2—C10—C11—C12 | 177.3 (4) | N1—Au1—N2—C6 | 1.2 (3) |
C9—C10—C11—C12 | −3.7 (8) | C14—C15—N3—C11 | 0.2 (7) |
N3—C11—C12—C13 | −0.9 (7) | C14—C15—N3—Au1 | 178.7 (3) |
C10—C11—C12—C13 | 178.2 (4) | C12—C11—N3—C15 | 0.9 (7) |
C11—C12—C13—C14 | 0.0 (7) | C10—C11—N3—C15 | −178.4 (4) |
C12—C13—C14—C15 | 1.0 (7) | C12—C11—N3—Au1 | −177.8 (4) |
C13—C14—C15—N3 | −1.1 (7) | C10—C11—N3—Au1 | 2.9 (5) |
C2—C1—N1—C5 | −0.3 (7) | N2—Au1—N3—C15 | −179.9 (4) |
C2—C1—N1—Au1 | −179.6 (4) | N1—Au1—N3—C15 | −179.7 (4) |
C4—C5—N1—C1 | 0.2 (7) | Cl1—Au1—N3—C15 | 3.6 (4) |
C6—C5—N1—C1 | −178.9 (4) | N2—Au1—N3—C11 | −1.4 (3) |
C4—C5—N1—Au1 | 179.5 (3) | N1—Au1—N3—C11 | −1.1 (7) |
C6—C5—N1—Au1 | 0.5 (5) | Cl1—Au1—N3—C11 | −177.8 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···Cl2i | 0.84 | 2.32 | 3.140 (4) | 167 |
O1W—H1B···Cl3 | 0.84 | 2.42 | 3.229 (4) | 161 |
O2W—H2A···Cl2 | 0.84 | 2.31 | 3.141 (4) | 172 |
O2W—H2B···O3W | 0.84 | 1.94 | 2.768 (5) | 169 |
O3W—H3A···Cl3ii | 0.84 | 2.31 | 3.133 (4) | 167 |
O3W—H3B···Cl3iii | 0.84 | 2.36 | 3.194 (4) | 171 |
Symmetry codes: (i) x, y−1, z; (ii) x, y+1, z; (iii) −x+1, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [AuCl(C15H11N3)]Cl2·3H2O |
Mr | 590.63 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 173 |
a, b, c (Å) | 8.4486 (1), 6.9766 (1), 31.1581 (6) |
β (°) | 94.392 (1) |
V (Å3) | 1831.14 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 8.49 |
Crystal size (mm) | 0.41 × 0.31 × 0.30 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector diffractometer |
Absorption correction | Integration [Face-indexed absorption corrections carried out with XPREP (Bruker, 2005)] |
Tmin, Tmax | 0.128, 0.185 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13022, 4386, 4157 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.661 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.061, 1.37 |
No. of reflections | 4386 |
No. of parameters | 226 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.32, −2.24 |
Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXTL (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···Cl2i | 0.84 | 2.32 | 3.140 (4) | 167 |
O1W—H1B···Cl3 | 0.84 | 2.42 | 3.229 (4) | 161 |
O2W—H2A···Cl2 | 0.84 | 2.31 | 3.141 (4) | 172 |
O2W—H2B···O3W | 0.84 | 1.94 | 2.768 (5) | 169 |
O3W—H3A···Cl3ii | 0.84 | 2.31 | 3.133 (4) | 167 |
O3W—H3B···Cl3iii | 0.84 | 2.36 | 3.194 (4) | 171 |
Symmetry codes: (i) x, y−1, z; (ii) x, y+1, z; (iii) −x+1, y+1/2, −z+1/2. |
Acknowledgements
We thank Dr Manuel Fernandes of the Jan Boeyens Structural Chemistry Laboratory at the University of the Witwatersrand for his assistance in the acquisition and solution of the crystallographic data.
References
Bruker (2005). APEX2 and SAINT-NT (includes XPREP and SADABS). Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Hollis, L. S. & Lippard, S. J. (1983). J. Am. Chem. Soc. 105, 4293–4299. CSD CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The title compound (I, Scheme 1) was synthesized as part of an ongoing study of the DNA binding and intercalation properties of metalloterpyridine complexes.
The asymmetric unit (Fig. 1) consists of the planar terpyridine-AuCl complex with one water molecule and one chloride ion above the plane of the complex, and the remaining two water molecules and a chloride ion below the plane.
A search of the literature revealed that the crystal structure of this compound was previously reported by Hollis & Lippard (1983). The reported structure possesses almost identical crystal parameters to the structure reported here in terms of space group, and unit-cell dimensions and angles. In addition, the coordination sphere parameters appear to closely match those obtained previously. However, the collection of data at 173 K, in comparison to 296 K as reported by Hollis & Lippard, results in some notable conclusions in addition to yielding more accurate data.
The water molecules and chloride ions are involved in extensive intermolecular hydrogen bonding. Fig. 2 illustrates these interactions which extend throughout the crystal structure. The atoms and interaction distances involved in the hydrogen bonding are very similar to those proposed by Hollis & Lippard, and the redetermined hydrogen bonding network confirms the proposed hydrogen bonds.
Additionally, Cl3 is orientated differently here than in the previously determined structure. With reference to the gold centre, Cl3 is found 5.047 (1) Å from the metal atom while the structure reported by Hollis & Lippard shows this distance to be 5.016 Å.