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The title complex, [Hg2Br4(C14H14S2)], has a dinuclear structure with one 1,2-bis(phenylsulfanyl)ethane ligand linking two HgBr2 units, in which the HgII center adopts a near T-shape coordination geometry formed by two Br− anions and one S atom of 1,2-bis(phenylsulfanyl)ethane. There is a crystallographic inversion center at the mid-point of the central C—C bond. In the crystal structure, when the Hg—Br weak interactions are considered, the dinuclear structure expands into a three-dimensional framework.
Supporting information
CCDC reference: 601130
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.011 Å
- R factor = 0.037
- wR factor = 0.098
- Data-to-parameter ratio = 19.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
Alert level G
ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.284 1.000
Tmin(prime) and Tmax expected: 0.009 0.024
RR(prime) = 0.775
Please check that your absorption correction is appropriate.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
5 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
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT and SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[µ-1,2-Bis(phenylsulfanyl)ethane-
κ2S:
S']bis[dibromomercury(II)]
top
Crystal data top
[Hg2Br4(C14H14S2)] | F(000) = 1720 |
Mr = 967.20 | Dx = 3.181 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3720 reflections |
a = 22.0328 (13) Å | θ = 2.8–27.3° |
b = 11.6648 (7) Å | µ = 23.30 mm−1 |
c = 8.0759 (4) Å | T = 293 K |
β = 103.313 (4)° | Block, colorless |
V = 2019.8 (2) Å3 | 0.18 × 0.16 × 0.16 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1987 independent reflections |
Radiation source: fine-focus sealed tube | 1772 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
φ and ω scans | θmax = 26.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −27→27 |
Tmin = 0.284, Tmax = 1.000 | k = −14→11 |
8500 measured reflections | l = −9→9 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.098 | w = 1/[σ2(Fo2) + (0.0351P)2 + 9.9952P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.001 |
1987 reflections | Δρmax = 2.52 e Å−3 |
101 parameters | Δρmin = −1.62 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00211 (15) |
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 | |
Hg1 | 0.583722 (15) | 0.58533 (3) | 0.18613 (4) | 0.05131 (19) | |
Br1 | 0.64832 (3) | 0.44047 (6) | 0.36648 (9) | 0.0378 (2) | |
Br2 | 0.49153 (3) | 0.67061 (6) | 0.00078 (9) | 0.0421 (2) | |
S1 | 0.67986 (8) | 0.75966 (14) | 0.2550 (2) | 0.0349 (4) | |
C1 | 0.6530 (3) | 0.8976 (5) | 0.2970 (8) | 0.0317 (14) | |
C2 | 0.6894 (3) | 0.9923 (6) | 0.2831 (9) | 0.0370 (15) | |
H2A | 0.7273 | 0.9825 | 0.2528 | 0.044* | |
C3 | 0.6700 (4) | 1.1008 (6) | 0.3137 (10) | 0.0447 (18) | |
H3A | 0.6952 | 1.1638 | 0.3077 | 0.054* | |
C4 | 0.6125 (4) | 1.1154 (7) | 0.3537 (10) | 0.0427 (16) | |
H4A | 0.5981 | 1.1888 | 0.3687 | 0.051* | |
C5 | 0.5768 (4) | 1.0215 (7) | 0.3711 (10) | 0.0469 (18) | |
H5A | 0.5393 | 1.0314 | 0.4036 | 0.056* | |
C6 | 0.5961 (4) | 0.9128 (6) | 0.3408 (10) | 0.0408 (17) | |
H6A | 0.5712 | 0.8498 | 0.3496 | 0.049* | |
C7 | 0.7213 (3) | 0.7142 (5) | 0.4663 (9) | 0.0368 (15) | |
H7A | 0.6936 | 0.7200 | 0.5436 | 0.044* | |
H7B | 0.7334 | 0.6345 | 0.4621 | 0.044* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Hg1 | 0.0409 (3) | 0.0615 (3) | 0.0464 (3) | 0.01361 (13) | −0.00061 (15) | 0.00668 (13) |
Br1 | 0.0357 (4) | 0.0330 (4) | 0.0434 (4) | −0.0010 (3) | 0.0063 (3) | 0.0065 (3) |
Br2 | 0.0329 (4) | 0.0452 (4) | 0.0449 (4) | 0.0070 (3) | 0.0019 (3) | 0.0000 (3) |
S1 | 0.0331 (10) | 0.0306 (8) | 0.0354 (9) | −0.0010 (6) | −0.0036 (6) | −0.0039 (6) |
C1 | 0.032 (4) | 0.028 (3) | 0.034 (3) | −0.002 (3) | 0.004 (3) | 0.004 (2) |
C2 | 0.036 (4) | 0.030 (3) | 0.047 (4) | −0.006 (3) | 0.014 (3) | 0.001 (3) |
C3 | 0.052 (5) | 0.034 (4) | 0.046 (4) | −0.010 (3) | 0.007 (4) | 0.004 (3) |
C4 | 0.042 (5) | 0.040 (4) | 0.043 (4) | 0.007 (3) | 0.004 (3) | −0.004 (3) |
C5 | 0.030 (4) | 0.057 (5) | 0.053 (5) | 0.003 (3) | 0.009 (3) | −0.007 (4) |
C6 | 0.027 (4) | 0.042 (4) | 0.052 (4) | −0.010 (3) | 0.006 (3) | 0.001 (3) |
C7 | 0.035 (4) | 0.027 (3) | 0.041 (4) | 0.000 (3) | −0.005 (3) | 0.001 (3) |
Geometric parameters (Å, º) top
Hg1—Br2 | 2.4404 (8) | C3—H3A | 0.9300 |
Hg1—Br1 | 2.4592 (7) | C4—C5 | 1.374 (12) |
Hg1—S1 | 2.8963 (17) | C4—H4A | 0.9300 |
S1—C1 | 1.774 (7) | C5—C6 | 1.377 (11) |
S1—C7 | 1.819 (7) | C5—H5A | 0.9300 |
C1—C2 | 1.384 (9) | C6—H6A | 0.9300 |
C1—C6 | 1.391 (10) | C7—C7i | 1.508 (13) |
C2—C3 | 1.377 (10) | C7—H7A | 0.9700 |
C2—H2A | 0.9300 | C7—H7B | 0.9700 |
C3—C4 | 1.389 (11) | | |
| | | |
Br2—Hg1—Br1 | 158.41 (3) | C5—C4—C3 | 120.0 (7) |
Br1—Hg1—S1 | 94.05 (4) | C5—C4—H4A | 120.0 |
Br2—Hg1—S1 | 107.47 (4) | C3—C4—H4A | 120.0 |
C1—S1—C7 | 101.7 (3) | C4—C5—C6 | 120.5 (7) |
C1—S1—Hg1 | 114.4 (2) | C4—C5—H5A | 119.7 |
C7—S1—Hg1 | 99.4 (2) | C6—C5—H5A | 119.7 |
C2—C1—C6 | 119.5 (6) | C5—C6—C1 | 119.8 (6) |
C2—C1—S1 | 118.9 (5) | C5—C6—H6A | 120.1 |
C6—C1—S1 | 121.6 (5) | C1—C6—H6A | 120.1 |
C3—C2—C1 | 120.6 (7) | C7i—C7—S1 | 112.0 (6) |
C3—C2—H2A | 119.7 | C7i—C7—H7A | 109.2 |
C1—C2—H2A | 119.7 | S1—C7—H7A | 109.2 |
C2—C3—C4 | 119.5 (7) | C7i—C7—H7B | 109.2 |
C2—C3—H3A | 120.2 | S1—C7—H7B | 109.2 |
C4—C3—H3A | 120.2 | H7A—C7—H7B | 107.9 |
| | | |
Br2—Hg1—S1—C1 | 42.2 (2) | S1—C1—C2—C3 | 179.6 (6) |
Br1—Hg1—S1—C1 | −136.0 (2) | C1—C2—C3—C4 | −2.0 (12) |
Br2—Hg1—S1—C7 | 149.7 (2) | C2—C3—C4—C5 | 3.4 (12) |
Br1—Hg1—S1—C7 | −28.6 (2) | C3—C4—C5—C6 | −3.3 (12) |
C7—S1—C1—C2 | 92.4 (6) | C4—C5—C6—C1 | 1.9 (12) |
Hg1—S1—C1—C2 | −161.6 (5) | C2—C1—C6—C5 | −0.5 (11) |
C7—S1—C1—C6 | −88.6 (7) | S1—C1—C6—C5 | −179.5 (6) |
Hg1—S1—C1—C6 | 17.4 (7) | C1—S1—C7—C7i | −66.8 (8) |
C6—C1—C2—C3 | 0.6 (11) | Hg1—S1—C7—C7i | 175.8 (7) |
Symmetry code: (i) −x+3/2, −y+3/2, −z+1. |
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