The title compound, [KAuCl4(C10H8N2)]n, is a layer coordination polymer with an AuIII—KI metal–metal bond. The Au and K atoms lie on positions of site symmetry 2/m and 222, respectively, and are arranged alternately to form Au—K—Au—K linear chains along the c axis. In addition, the Au atom is coordinated by four Cl atoms, and the K atom coordinated by two N atoms of bipyridine ligands.
Supporting information
CCDC reference: 232059
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.040
- wR factor = 0.099
- Data-to-parameter ratio = 17.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2 .. CL1 .. 2.90 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.25 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Poly[[terachlorogold(III)potassium(I)(Au—
K)]-µ-4,4'-bipyridine]
top
Crystal data top
[KAuCl4(C10H8N2)] | F(000) = 992 |
Mr = 534.05 | Dx = 2.385 Mg m−3 |
Orthorhombic, Ibam | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -I 2 2c | Cell parameters from 732 reflections |
a = 12.900 (3) Å | θ = 2.7–27.4° |
b = 7.8312 (19) Å | µ = 10.87 mm−1 |
c = 14.722 (4) Å | T = 293 K |
V = 1487.3 (6) Å3 | Slice, yellow |
Z = 4 | 0.30 × 0.20 × 0.20 mm |
Data collection top
Bruker SMART APEX CCD area-detector diffractometer | 848 independent reflections |
Radiation source: sealed tube | 629 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
φ and ω scans | θmax = 27.0°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −16→16 |
Tmin = 0.09, Tmax = 0.11 | k = −9→10 |
4067 measured reflections | l = −18→11 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0588P)2] where P = (Fo2 + 2Fc2)/3 |
848 reflections | (Δ/σ)max < 0.001 |
48 parameters | Δρmax = 1.19 e Å−3 |
1 restraint | Δρmin = −1.08 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. The structure was solved by weight atom method and refined on F2 by
full matrix least squares methods. All the non-hydrogen atoms were refined
anisotropically. 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 | |
K1 | 1.0000 | 0.0000 | 0.2500 | 0.0473 (8) | |
N1 | 0.7666 (7) | 0.0000 | 0.2500 | 0.051 (3) | |
C1 | 0.55645 (19) | 0.0000 | 0.2500 | 0.036 (2) | |
C2 | 0.6098 (6) | 0.0692 (12) | 0.3231 (7) | 0.043 (2) | |
H2 | 0.5746 | 0.1168 | 0.3720 | 0.051* | |
C3 | 0.7190 (6) | 0.0653 (12) | 0.3211 (7) | 0.045 (2) | |
H3 | 0.7571 | 0.1085 | 0.3695 | 0.054* | |
Au1 | 1.0000 | 0.0000 | 0.0000 | 0.0346 (2) | |
Cl1 | 1.15612 (19) | −0.1367 (4) | 0.0000 | 0.0408 (6) | |
Cl2 | 1.0838 (2) | 0.2579 (4) | 0.0000 | 0.0452 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0266 (16) | 0.055 (2) | 0.060 (2) | 0.000 | 0.000 | 0.000 |
N1 | 0.015 (4) | 0.049 (6) | 0.090 (8) | 0.000 | 0.000 | 0.010 (7) |
C1 | 0.025 (5) | 0.032 (5) | 0.051 (6) | 0.000 | 0.000 | 0.008 (6) |
C2 | 0.020 (4) | 0.059 (5) | 0.050 (5) | 0.000 (3) | −0.005 (3) | 0.001 (4) |
C3 | 0.024 (4) | 0.048 (5) | 0.062 (6) | 0.006 (3) | −0.008 (4) | −0.007 (4) |
Au1 | 0.0165 (3) | 0.0388 (3) | 0.0486 (4) | −0.0013 (2) | 0.000 | 0.000 |
Cl1 | 0.0149 (10) | 0.0473 (15) | 0.0601 (18) | 0.0065 (11) | 0.000 | 0.000 |
Cl2 | 0.0246 (12) | 0.0365 (15) | 0.074 (2) | −0.0046 (10) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
K1—N1i | 3.010 (9) | C2—C3 | 1.409 (11) |
K1—N1 | 3.010 (9) | C2—H2 | 0.9300 |
K1—Au1ii | 3.6805 (10) | C3—H3 | 0.9300 |
K1—Au1 | 3.6805 (10) | Au1—Cl1iv | 2.281 (2) |
N1—C3ii | 1.317 (10) | Au1—Cl1 | 2.281 (2) |
N1—C3 | 1.317 (10) | Au1—Cl2 | 2.291 (3) |
C1—C2 | 1.387 (9) | Au1—Cl2iv | 2.291 (3) |
C1—C2ii | 1.387 (9) | Au1—K1iv | 3.6805 (10) |
C1—C1iii | 1.457 (5) | | |
| | | |
N1—K1—N1i | 180.0 | C2—C3—H3 | 120.3 |
N1i—K1—Au1ii | 90.0 | Cl1iv—Au1—Cl1 | 180.00 (14) |
N1—K1—Au1ii | 90.0 | Cl1iv—Au1—Cl2 | 90.16 (11) |
N1i—K1—Au1 | 90.0 | Cl1—Au1—Cl2 | 89.84 (11) |
N1—K1—Au1 | 90.0 | Cl1iv—Au1—Cl2iv | 89.84 (11) |
Au1—K1—Au1ii | 180.0 | Cl1—Au1—Cl2iv | 90.16 (11) |
C3ii—N1—C3 | 124.3 (10) | Cl2—Au1—Cl2iv | 180.00 (14) |
C3ii—N1—K1 | 117.8 (5) | Cl1iv—Au1—K1iv | 90.0 |
C3—N1—K1 | 117.8 (5) | Cl1—Au1—K1iv | 90.0 |
C2—C1—C2ii | 120.5 (7) | Cl2—Au1—K1iv | 90.0 |
C2—C1—C1iii | 119.8 (4) | Cl2iv—Au1—K1iv | 90.0 |
C2ii—C1—C1iii | 119.8 (4) | Cl1iv—Au1—K1 | 90.0 |
C1—C2—C3 | 118.1 (8) | Cl1—Au1—K1 | 90.0 |
C1—C2—H2 | 120.9 | Cl2—Au1—K1 | 90.0 |
C3—C2—H2 | 120.9 | Cl2iv—Au1—K1 | 90.0 |
N1—C3—C2 | 119.4 (9) | K1—Au1—K1iv | 180.0 |
N1—C3—H3 | 120.3 | | |
Symmetry codes: (i) −x+2, −y, z; (ii) x, −y, −z+1/2; (iii) −x+1, −y, z; (iv) −x+2, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···Cl1v | 0.93 | 2.90 | 3.528 (10) | 126 |
Symmetry code: (v) x−1/2, y+1/2, z+1/2. |