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In the title compound, [PdCl
2(C
6H
4N
2)
2], the Pd
II cations occupy crystallographic inversion centres and adopt a slightly distorted square-planar coordination geometry. Adjacent molecules are linked into one-dimensional chains
via long-range pairwise Pd
Cl interactions.
Supporting information
CCDC reference: 193696
Key indicators
- Single-crystal synchrotron study
- T = 150 K
- Mean (C-C) = 0.005 Å
- R factor = 0.037
- wR factor = 0.088
- Data-to-parameter ratio = 20.9
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level B:
REFLT_03
From the CIF: _diffrn_reflns_theta_max 29.12
From the CIF: _reflns_number_total 1856
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 2118
Completeness (_total/calc) 87.63%
Alert B: < 90% complete (theta max?)
| Author response: ...
The dataset is >97% complete to 2theta = 55 degrees.
|
Alert Level C:
PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C(4) - C(7) = 1.45 Ang.
General Notes
ABSMU_01 Radiation type not identified. Calculation of
_exptl_absorpt_correction_mu not performed.
ABSTM_02 When printed, the submitted absorption T values will be replaced
by the scaled T values. Since the ratio of scaled T's is
identical to the ratio of reported T values, the scaling does
not imply a change to the absorption corrections used in the
study.
Ratio of Tmax expected/reported 1.698
Tmax scaled 0.935 Tmin scaled 0.570
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Bruker, 1998); cell refinement: LSCELL (Clegg, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1994); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2002).
Palladium(II)-transdichlorobis(4-cyanopyridine)
top
Crystal data top
[PdCl2(C6H4N2)2] | F(000) = 376 |
Mr = 385.52 | Dx = 1.800 Mg m−3 |
Monoclinic, P21/n | Synchrotron radiation, λ = 0.6890 Å |
a = 3.8983 (13) Å | Cell parameters from 2761 reflections |
b = 25.651 (14) Å | θ = 3.0–29.0° |
c = 7.256 (4) Å | µ = 1.67 mm−1 |
β = 101.33 (5)° | T = 150 K |
V = 711.4 (6) Å3 | Needle, yellow-orange |
Z = 2 | 0.90 × 0.04 × 0.04 mm |
Data collection top
Bruker SMART CCD diffractometer | 1856 independent reflections |
Radiation source: Daresbury SRS station 9.8 | 1452 reflections with I > 2σ(I) |
Silicon 111 monochromator | Rint = 0.040 |
ω rotation with narrow frames scans | θmax = 29.1°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −5→5 |
Tmin = 0.336, Tmax = 0.551 | k = −19→35 |
3314 measured reflections | l = −9→4 |
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) = 0.088 | w = 1/[σ2(Fo2) + (0.0428P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.93 | (Δ/σ)max = 0.001 |
1856 reflections | Δρmax = 0.86 e Å−3 |
89 parameters | Δρmin = −1.03 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: 0.008 (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 | |
Pd1 | 0.0000 | 0.0000 | 0.5000 | 0.01541 (13) | |
Cl1 | −0.3703 (2) | 0.04335 (3) | 0.26048 (10) | 0.02030 (18) | |
N1 | 0.0619 (7) | 0.06633 (10) | 0.6538 (4) | 0.0167 (5) | |
C2 | 0.1814 (9) | 0.11030 (13) | 0.5851 (5) | 0.0200 (7) | |
H2A | 0.2365 | 0.1094 | 0.4633 | 0.024* | |
C3 | 0.2265 (9) | 0.15651 (13) | 0.6852 (5) | 0.0217 (7) | |
H3A | 0.3083 | 0.1870 | 0.6335 | 0.026* | |
C4 | 0.1478 (8) | 0.15677 (13) | 0.8651 (5) | 0.0210 (7) | |
C5 | 0.0288 (9) | 0.11185 (14) | 0.9374 (5) | 0.0228 (7) | |
H5A | −0.0237 | 0.1117 | 1.0599 | 0.027* | |
C6 | −0.0126 (9) | 0.06697 (13) | 0.8278 (4) | 0.0193 (6) | |
H6A | −0.0952 | 0.0360 | 0.8764 | 0.023* | |
C7 | 0.1915 (10) | 0.20401 (15) | 0.9777 (6) | 0.0311 (8) | |
N8 | 0.2255 (12) | 0.24088 (16) | 1.0702 (6) | 0.0498 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pd1 | 0.01917 (18) | 0.01314 (17) | 0.01467 (18) | −0.00058 (13) | 0.00512 (12) | 0.00041 (13) |
Cl1 | 0.0225 (4) | 0.0201 (3) | 0.0186 (3) | 0.0009 (3) | 0.0048 (3) | 0.0026 (3) |
N1 | 0.0192 (13) | 0.0143 (12) | 0.0179 (12) | 0.0017 (10) | 0.0063 (10) | 0.0009 (10) |
C2 | 0.0215 (15) | 0.0190 (16) | 0.0206 (15) | −0.0014 (12) | 0.0070 (13) | 0.0022 (12) |
C3 | 0.0205 (15) | 0.0162 (15) | 0.0294 (17) | −0.0012 (12) | 0.0075 (14) | −0.0002 (13) |
C4 | 0.0179 (15) | 0.0185 (16) | 0.0267 (16) | 0.0014 (12) | 0.0042 (13) | −0.0073 (13) |
C5 | 0.0235 (16) | 0.0249 (18) | 0.0198 (15) | 0.0016 (13) | 0.0039 (13) | 0.0009 (14) |
C6 | 0.0216 (15) | 0.0217 (16) | 0.0154 (13) | 0.0019 (12) | 0.0051 (12) | 0.0046 (12) |
C7 | 0.0296 (18) | 0.0239 (18) | 0.041 (2) | −0.0018 (14) | 0.0094 (17) | −0.0065 (16) |
N8 | 0.054 (2) | 0.036 (2) | 0.061 (3) | −0.0053 (18) | 0.015 (2) | −0.0241 (19) |
Geometric parameters (Å, º) top
Pd1—N1 | 2.023 (3) | C4—C7 | 1.453 (5) |
Pd1—Cl1 | 2.3141 (14) | C5—C6 | 1.391 (5) |
Pd1—Cl1i | 3.4580 (16) | C7—N8 | 1.152 (5) |
N1—C6 | 1.350 (4) | C2—H2A | 0.9500 |
N1—C2 | 1.352 (4) | C3—H3A | 0.9500 |
C2—C3 | 1.383 (5) | C5—H5A | 0.9500 |
C3—C4 | 1.398 (5) | C6—H6A | 0.9500 |
C4—C5 | 1.384 (5) | | |
| | | |
N1—Pd1—Cl1 | 89.96 (9) | C4—C5—C6 | 118.8 (3) |
N1—Pd1—Cl1ii | 90.04 (9) | N1—C6—C5 | 121.5 (3) |
N1—Pd1—Cl1iii | 90.74 (8) | N8—C7—C4 | 178.6 (5) |
Cl1—Pd1—Cl1i | 82.40 (4) | N1—C2—H2A | 118.7 |
C6—N1—C2 | 119.2 (3) | C3—C2—H2A | 118.7 |
Pd1—N1—C6 | 120.1 (2) | C2—C3—H3A | 121.1 |
Pd1—N1—C2 | 120.7 (2) | C4—C3—H3A | 121.1 |
N1—C2—C3 | 122.6 (3) | C4—C5—H5A | 120.6 |
C2—C3—C4 | 117.8 (3) | C6—C5—H5A | 120.6 |
C5—C4—C3 | 120.1 (3) | N1—C6—H6A | 119.2 |
C5—C4—C7 | 119.5 (3) | C5—C6—H6A | 119.2 |
C3—C4—C7 | 120.4 (3) | | |
Symmetry codes: (i) x+1, y, z; (ii) −x, −y, −z+1; (iii) −x−1, −y, −z+1. |
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