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In the title compound, [CdCl
2(C
5H
5NS)
2], the Cd
II atom (site symmetry 2) is coordinated by the S atoms of two zwitterionic pyridine-2-thione ligands and two Cl atoms in distorted tetrahedral geometry [Cd—S = 2.5068 (8) Å and Cd—Cl = 2.4684 (8) Å]. The molecules are linked
via N—H
Cl, C—H
Cl and C—H
S interactions into an extended network.
Supporting information
CCDC reference: 252050
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.018
- wR factor = 0.041
- Data-to-parameter ratio = 20.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3A .. CL .. 2.87 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
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 27.04
From the CIF: _reflns_number_total 1579
Count of symmetry unique reflns 850
Completeness (_total/calc) 185.76%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 729
Fraction of Friedel pairs measured 0.858
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 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
0 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: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Dichlorobis(pyridinium-2-thiolato)cadmium(II)
top
Crystal data top
[CdCl2(C5H5NS)2] | F(000) = 1584 |
Mr = 405.62 | Dx = 1.873 Mg m−3 |
Orthorhombic, Fdd2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: F 2 -2d | Cell parameters from 2850 reflections |
a = 12.837 (3) Å | θ = 1.9–27.0° |
b = 27.526 (6) Å | µ = 2.16 mm−1 |
c = 8.140 (2) Å | T = 293 K |
V = 2876.3 (12) Å3 | Rod, light yellow |
Z = 8 | 0.15 × 0.07 × 0.06 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1579 independent reflections |
Radiation source: fine-focus sealed tube | 1520 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω scans | θmax = 27.0°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −13→16 |
Tmin = 0.834, Tmax = 0.879 | k = −34→27 |
4192 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)] = 0.018 | H-atom parameters constrained |
wR(F2) = 0.041 | w = 1/[σ2(Fo2) + (0.0224P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.029 |
1579 reflections | Δρmax = 0.30 e Å−3 |
78 parameters | Δρmin = −0.30 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 729 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.04 (2) |
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 | 0.53742 (4) | 0.04074 (8) | |
S | 0.17690 (5) | 0.32170 (3) | 0.68829 (10) | 0.05179 (18) | |
Cl | 0.40241 (5) | 0.27564 (2) | 0.37412 (9) | 0.05074 (16) | |
N | 0.29346 (18) | 0.39272 (8) | 0.8027 (3) | 0.0427 (5) | |
H0A | 0.2479 | 0.4105 | 0.7540 | 0.051* | |
C1 | 0.4375 (2) | 0.33858 (13) | 0.9549 (4) | 0.0593 (8) | |
H1A | 0.4876 | 0.3196 | 1.0069 | 0.071* | |
C2 | 0.4437 (2) | 0.38833 (14) | 0.9646 (4) | 0.0627 (9) | |
H2A | 0.4969 | 0.4032 | 1.0236 | 0.075* | |
C3 | 0.3709 (3) | 0.41508 (11) | 0.8864 (4) | 0.0578 (8) | |
H3A | 0.3740 | 0.4488 | 0.8899 | 0.069* | |
C4 | 0.28371 (19) | 0.34418 (9) | 0.7915 (4) | 0.0375 (5) | |
C5 | 0.3593 (2) | 0.31667 (10) | 0.8702 (4) | 0.0486 (6) | |
H5A | 0.3563 | 0.2829 | 0.8650 | 0.058* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd | 0.04312 (13) | 0.03507 (12) | 0.04404 (12) | −0.00578 (13) | 0.000 | 0.000 |
S | 0.0375 (3) | 0.0533 (4) | 0.0646 (4) | 0.0073 (3) | −0.0152 (3) | −0.0191 (3) |
Cl | 0.0496 (4) | 0.0413 (3) | 0.0613 (4) | −0.0102 (3) | 0.0109 (3) | −0.0007 (3) |
N | 0.0506 (12) | 0.0357 (11) | 0.0416 (12) | 0.0036 (9) | 0.0017 (12) | −0.0048 (11) |
C1 | 0.0473 (17) | 0.075 (2) | 0.0554 (18) | 0.0097 (15) | −0.0139 (16) | −0.0099 (17) |
C2 | 0.0457 (17) | 0.086 (3) | 0.0566 (19) | −0.0132 (16) | −0.0072 (15) | −0.0235 (18) |
C3 | 0.065 (2) | 0.0493 (16) | 0.0593 (19) | −0.0159 (15) | 0.0104 (18) | −0.0196 (15) |
C4 | 0.0343 (11) | 0.0416 (13) | 0.0366 (12) | 0.0014 (10) | 0.0014 (11) | −0.0041 (12) |
C5 | 0.0458 (15) | 0.0441 (14) | 0.0559 (16) | 0.0043 (12) | −0.0117 (13) | −0.0016 (13) |
Geometric parameters (Å, º) top
Cd—S | 2.5068 (8) | C1—C5 | 1.359 (4) |
Cd—Cl | 2.4684 (8) | C1—C2 | 1.374 (5) |
Cd—Si | 2.5068 (8) | C1—H1A | 0.9300 |
Cd—Cli | 2.4684 (8) | C2—C3 | 1.349 (5) |
S—C4 | 1.723 (3) | C2—H2A | 0.9300 |
N—C4 | 1.345 (3) | C3—H3A | 0.9300 |
N—C3 | 1.353 (4) | C4—C5 | 1.387 (4) |
N—H0A | 0.8600 | C5—H5A | 0.9300 |
| | | |
Si—Cd—S | 121.33 (4) | C3—C2—C1 | 118.5 (3) |
Cli—Cd—Cl | 114.83 (4) | C3—C2—H2A | 120.8 |
Cli—Cd—Si | 109.60 (3) | C1—C2—H2A | 120.8 |
Cl—Cd—Si | 101.08 (3) | C2—C3—N | 119.9 (3) |
Cli—Cd—S | 101.08 (3) | C2—C3—H3A | 120.1 |
Cl—Cd—S | 109.60 (3) | N—C3—H3A | 120.1 |
C4—S—Cd | 102.92 (9) | N—C4—C5 | 116.5 (3) |
C4—N—C3 | 123.7 (3) | N—C4—S | 117.6 (2) |
C4—N—H0A | 118.2 | C5—C4—S | 125.8 (2) |
C3—N—H0A | 118.2 | C1—C5—C4 | 120.6 (3) |
C5—C1—C2 | 121.0 (3) | C1—C5—H5A | 119.7 |
C5—C1—H1A | 119.5 | C4—C5—H5A | 119.7 |
C2—C1—H1A | 119.5 | | |
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 |
C1—H1A···Sii | 0.93 | 2.84 | 3.643 (3) | 145 |
C3—H3A···Cliii | 0.93 | 2.87 | 3.619 (3) | 139 |
N—H0A···Cliv | 0.86 | 2.39 | 3.231 (2) | 167 |
Symmetry codes: (ii) x+1/2, y, z+1/2; (iii) −x+3/4, y+1/4, z+3/4; (iv) x−1/4, −y+3/4, z+1/4. |
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