Mercury(I) actetate, [Hg(C2H3O2)]n, crystallizes as centrosymmetric dimers, CH3COO-Hg-Hg-OOCCH3, with an Hg-Hg distance of 2.5202 (15) Å and an Hg-O distance of 2.152 (12) Å. The dimers are assembled into infinite ribbons by long, weaker Hg-O bonds [Hg-O = 2.6802 (12) Å]. There are no strong intermolecular forces between the ribbons.
Supporting information
CCDC reference: 282309
Key indicators
- Single-crystal synchrotron study
- T = 150 K
- Mean (C-C) = 0.017 Å
- R factor = 0.043
- wR factor = 0.109
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
Alert level C
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2
| Author Response:
Inspection of the ORTEP plot suggests there is no serious problem
with the atomic displacement parameter for O2.
|
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 17
| Author Response:
Diffraction is dominated by scattering from mercury (80 electrons).
The precision with which light atoms are located will be moderate.
|
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: APEXII (Bruker, 2004); cell refinement: APEXII; data reduction: APEXII; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Version 1.164; Farrugia, 1999); software used to prepare material for publication: SHELXL97.
Crystal data top
[Hg(C2H3O2)] | F(000) = 444 |
Mr = 259.63 | Dx = 4.763 Mg m−3 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.84640 Å |
Hall symbol: -C 2y | Cell parameters from 1173 reflections |
a = 5.133 (3) Å | θ = 4.0–32.4° |
b = 5.866 (3) Å | µ = 79.55 mm−1 |
c = 12.202 (6) Å | T = 150 K |
β = 99.779 (7)° | Plate, colourless |
V = 362.1 (3) Å3 | 0.02 × 0.02 × 0.01 mm |
Z = 4 | |
Data collection top
Bruker D8 diffractometer | 404 independent reflections |
Radiation source: Daresbury SRS, Station 16.2SMX | 395 reflections with I > 2σ(I) |
Silicon 111 monochromator | Rint = 0.046 |
ω rotation with narrow frame scans | θmax = 32.4°, θmin = 4.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −6→6 |
Tmin = 0.204, Tmax = 0.672 | k = −7→7 |
1173 measured reflections | l = −15→15 |
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) = 0.109 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0852P)2] where P = (Fo2 + 2Fc2)/3 |
404 reflections | (Δ/σ)max < 0.001 |
33 parameters | Δρmax = 2.89 e Å−3 |
24 restraints | Δρmin = −5.57 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 | Occ. (<1) |
Hg1 | −0.38573 (10) | 0.0000 | 0.09993 (4) | 0.0116 (4) | |
O1 | −0.177 (2) | 0.0000 | 0.2686 (10) | 0.019 (3) | |
C1 | 0.063 (2) | 0.0000 | 0.2661 (9) | 0.004 (2) | |
O2 | 0.1553 (19) | 0.0000 | 0.1768 (9) | 0.027 (3) | |
C2 | 0.246 (3) | 0.0000 | 0.3761 (10) | 0.008 (2) | |
H2A | 0.1809 | −0.1070 | 0.4268 | 0.012* | 0.50 |
H2B | 0.2544 | 0.1536 | 0.4081 | 0.012* | 0.50 |
H2C | 0.4236 | −0.0466 | 0.3652 | 0.012* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Hg1 | 0.0098 (5) | 0.0144 (5) | 0.0094 (5) | 0.000 | −0.0018 (3) | 0.000 |
O1 | 0.015 (5) | 0.035 (5) | 0.008 (5) | 0.000 | 0.005 (4) | 0.000 |
C1 | 0.003 (2) | 0.003 (2) | 0.004 (2) | 0.000 | 0.0001 (10) | 0.000 |
O2 | 0.012 (5) | 0.056 (7) | 0.016 (5) | 0.000 | 0.006 (4) | 0.000 |
C2 | 0.008 (5) | 0.010 (4) | 0.005 (5) | 0.000 | −0.002 (4) | 0.000 |
Geometric parameters (Å, º) top
Hg1—O1 | 2.152 (12) | C1—C2 | 1.503 (16) |
Hg1—Hg1i | 2.5202 (15) | C2—H2A | 0.9800 |
O1—C1 | 1.239 (15) | C2—H2B | 0.9800 |
C1—O2 | 1.259 (15) | C2—H2C | 0.9800 |
| | | |
O1—Hg1—Hg1i | 178.0 (3) | C1—C2—H2B | 109.5 |
C1—O1—Hg1 | 108.2 (9) | H2A—C2—H2B | 109.5 |
O1—C1—O2 | 122.9 (11) | C1—C2—H2C | 109.5 |
O1—C1—C2 | 117.0 (11) | H2A—C2—H2C | 109.5 |
O2—C1—C2 | 120.2 (9) | H2B—C2—H2C | 109.5 |
C1—C2—H2A | 109.5 | | |
Symmetry code: (i) −x−1, −y, −z. |