In the title compound, [CdBr
2(C
5H
5NS)
2], the Cd
II cation (site symmetry 2) is coordinated by the S atoms of two pyridine-2-thione ligands and two Br
− ions in a distorted tetrahedral geometry [Cd—S = 2.5171 (10) Å and Cd—Br = 2.5911 (6) Å]. The molecules are linked
via N—H
Br, C—H
Br and C—H
S interactions into an extended network.
Supporting information
CCDC reference: 258703
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.020
- wR factor = 0.047
- Data-to-parameter ratio = 20.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd - Br .. 8.30 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd - S1 .. 5.56 su
PLAT480_ALERT_4_C Long H...A H-Bond Reported H5A .. BR .. 3.00 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3A .. S1 .. 2.90 Ang.
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.00
From the CIF: _reflns_number_total 1622
Count of symmetry unique reflns 877
Completeness (_total/calc) 184.95%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 745
Fraction of Friedel pairs measured 0.849
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXTL97.
Dibromobis(pyridinium-2-thiolato-
κS)cadmium(II)
top
Crystal data top
[CdBr2(C5H5NS)2] | F(000) = 1872 |
Mr = 494.54 | Dx = 2.189 Mg m−3 |
Orthorhombic, Fdd2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: F 2 -2d | Cell parameters from 2990 reflections |
a = 13.050 (3) Å | θ = 2.9–27.0° |
b = 28.521 (6) Å | µ = 7.04 mm−1 |
c = 8.065 (2) Å | T = 293 K |
V = 3001.8 (12) Å3 | Rod, light yellow |
Z = 8 | 0.18 × 0.07 × 0.06 mm |
Data collection top
Bruker SMART CCD diffractometer | 1622 independent reflections |
Radiation source: fine-focus sealed tube | 1535 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ω scans | θmax = 27.0°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −16→7 |
Tmin = 0.559, Tmax = 0.656 | k = −36→35 |
4357 measured reflections | l = −10→10 |
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)] = 0.020 | H-atom parameters constrained |
wR(F2) = 0.047 | w = 1/[σ2(Fo2) + (0.0271P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max = 0.026 |
1622 reflections | Δρmax = 0.43 e Å−3 |
78 parameters | Δρmin = −0.38 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 745 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.060 (8) |
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 | |
Cd | 0.2500 | 0.2500 | 0.85297 (4) | 0.03911 (9) | |
Br | 0.09238 (2) | 0.224412 (12) | 0.67982 (5) | 0.04781 (11) | |
S1 | 0.31925 (6) | 0.17996 (4) | 1.00629 (14) | 0.0506 (2) | |
N1 | 0.2034 (2) | 0.11077 (11) | 1.1159 (4) | 0.0427 (6) | |
H1A | 0.2488 | 0.0939 | 1.0667 | 0.051* | |
C1 | 0.2127 (2) | 0.15796 (11) | 1.1060 (5) | 0.0348 (6) | |
C2 | 0.1365 (3) | 0.18372 (13) | 1.1843 (6) | 0.0463 (8) | |
H2A | 0.1380 | 0.2163 | 1.1789 | 0.056* | |
C3 | 0.0599 (3) | 0.16222 (16) | 1.2684 (6) | 0.0549 (10) | |
H3A | 0.0105 | 0.1801 | 1.3221 | 0.066* | |
C4 | 0.0548 (3) | 0.11370 (17) | 1.2749 (6) | 0.0592 (11) | |
H4A | 0.0020 | 0.0988 | 1.3315 | 0.071* | |
C5 | 0.1277 (4) | 0.08858 (14) | 1.1978 (6) | 0.0549 (10) | |
H5A | 0.1259 | 0.0560 | 1.2010 | 0.066* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd | 0.03775 (17) | 0.03658 (16) | 0.04301 (18) | −0.00597 (15) | 0.000 | 0.000 |
Br | 0.04280 (19) | 0.04144 (18) | 0.0592 (2) | −0.00889 (15) | −0.01097 (18) | −0.00022 (18) |
S1 | 0.0318 (4) | 0.0554 (5) | 0.0646 (6) | 0.0068 (4) | 0.0123 (4) | 0.0207 (5) |
N1 | 0.0475 (15) | 0.0379 (13) | 0.0427 (16) | 0.0025 (12) | −0.0016 (15) | 0.0043 (15) |
C1 | 0.0324 (15) | 0.0367 (15) | 0.0352 (15) | 0.0020 (13) | −0.0001 (15) | 0.0039 (15) |
C2 | 0.0430 (17) | 0.0430 (18) | 0.053 (2) | 0.0068 (15) | 0.0056 (18) | −0.0006 (18) |
C3 | 0.041 (2) | 0.069 (3) | 0.054 (2) | 0.0069 (19) | 0.0086 (19) | 0.006 (2) |
C4 | 0.046 (2) | 0.077 (3) | 0.055 (2) | −0.015 (2) | 0.002 (2) | 0.023 (2) |
C5 | 0.066 (2) | 0.0445 (19) | 0.054 (2) | −0.0144 (19) | −0.010 (2) | 0.0148 (19) |
Geometric parameters (Å, º) top
Cd—S1i | 2.5171 (10) | C1—C2 | 1.389 (5) |
Cd—S1 | 2.5171 (10) | C2—C3 | 1.354 (6) |
Cd—Br | 2.5911 (6) | C2—H2A | 0.9300 |
Cd—Bri | 2.5911 (6) | C3—C4 | 1.387 (6) |
S1—C1 | 1.724 (3) | C3—H3A | 0.9300 |
N1—C5 | 1.347 (5) | C4—C5 | 1.343 (7) |
N1—C1 | 1.354 (4) | C4—H4A | 0.9300 |
N1—H1A | 0.8600 | C5—H5A | 0.9300 |
| | | |
S1i—Cd—S1 | 121.16 (6) | C3—C2—C1 | 121.1 (3) |
S1i—Cd—Br | 101.73 (2) | C3—C2—H2A | 119.4 |
S1—Cd—Br | 109.04 (3) | C1—C2—H2A | 119.4 |
S1i—Cd—Bri | 109.04 (3) | C2—C3—C4 | 120.4 (4) |
S1—Cd—Bri | 101.73 (2) | C2—C3—H3A | 119.8 |
Br—Cd—Bri | 114.77 (3) | C4—C3—H3A | 119.8 |
C1—S1—Cd | 103.22 (11) | C5—C4—C3 | 118.7 (4) |
C5—N1—C1 | 124.2 (3) | C5—C4—H4A | 120.6 |
C5—N1—H1A | 117.9 | C3—C4—H4A | 120.6 |
C1—N1—H1A | 117.9 | C4—C5—N1 | 119.7 (4) |
N1—C1—C2 | 115.8 (3) | C4—C5—H5A | 120.1 |
N1—C1—S1 | 117.5 (3) | N1—C5—H5A | 120.1 |
C2—C1—S1 | 126.7 (3) | | |
Symmetry code: (i) −x+1/2, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C5—H5A···Brii | 0.93 | 3.00 | 3.776 (4) | 142 |
C3—H3A···S1iii | 0.93 | 2.90 | 3.715 (4) | 147 |
N1—H1A···Briv | 0.86 | 2.55 | 3.382 (3) | 163 |
Symmetry codes: (ii) −x+1/4, y−1/4, z+3/4; (iii) x−1/2, y, z+1/2; (iv) x+1/4, −y+1/4, z+1/4. |