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The title compound, [PdBr2(C6H12N3)2] or [PdBr2(PTA)2] (where PTA is 1,3,5-triaza-7-phosphaadamantane), was found to be isostructural with the previously reported trans-[PtI2(PTA)2]. The Pd atom lies on an inversion centre, resulting in a trans-square-planar geometry. Selected geometrical parameters are Pd1—P1 and Pd1—Br1 distances of 2.320 (1) and 2.427 (1) Å, respectively, and a P—Pd—Br angle of 90.6 (3)°. The effective cone angle for the PTA ligands was calculated as 114.0°.
Supporting information
CCDC reference: 200729
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.006 Å
- R factor = 0.039
- wR factor = 0.084
- Data-to-parameter ratio = 23.1
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level A:
PLAT_701 Alert A Bond Calc 2.3199(12), Rep 2.3120(10), Dev. 6.58 Sigma
PD1 -P1 1.555 1.555
PLAT_701 Alert A Bond Calc 2.3199(12), Rep 2.3120(10), Dev. 6.58 Sigma
PD1 -P1 1.555 3.556
General Notes
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 1.162
Tmax scaled 0.708 Tmin scaled 0.518
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check
Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXL97.
trans-Dibromobis(1,3,5-triaza-7-phosphaadamantane)palladium(II)
top
Crystal data top
[PdBr2(C6H12N3)2] | F(000) = 568 |
Mr = 580.53 | Dx = 2.184 Mg m−3 Dm = 2.177 Mg m−3 Dm measured by flotation in CH2I2/C6H6 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 7.276 (2) Å | Cell parameters from 2112 reflections |
b = 11.808 (2) Å | θ = 2.6–27.9° |
c = 10.317 (2) Å | µ = 5.77 mm−1 |
β = 94.99 (3)° | T = 293 K |
V = 883.0 (3) Å3 | Rectangle, yellow |
Z = 2 | 0.18 × 0.09 × 0.06 mm |
Data collection top
Siemens SMART CCD diffractometer | 2475 independent reflections |
Radiation source: rotating anode | 1629 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
ω scans | θmax = 29.6°, θmin = 2.6° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −10→9 |
Tmin = 0.446, Tmax = 0.609 | k = −16→16 |
8979 measured reflections | l = −12→14 |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.084 | H-atom parameters constrained |
S = 0.94 | w = 1/[σ2(Fo2) + (0.038P)2] where P = (Fo2 + 2Fc2)/3 |
2475 reflections | (Δ/σ)max = 0.001 |
107 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −1.34 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. The intensity data were collected on a Siemens SMART CCD diffractometer
using an exposure time of 20 s/frame. A total of 1940 frames were collected
with a frame width of 0.25 ° being used covering up to θ = 29.57° with a
completeness of 99.8% being achieved. The first 50 frames were recollected at
the end of the data collection to check for decay. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pd1 | 0.0000 | 0.0000 | 0.5000 | 0.02038 (12) | |
Br1 | 0.24015 (7) | −0.04574 (4) | 0.35938 (5) | 0.03753 (15) | |
P1 | 0.13587 (14) | 0.17448 (8) | 0.54797 (11) | 0.0218 (2) | |
N1 | 0.3616 (5) | 0.2889 (3) | 0.7321 (4) | 0.0273 (8) | |
N3 | 0.1182 (5) | 0.4004 (3) | 0.6106 (3) | 0.0255 (8) | |
N2 | 0.3900 (5) | 0.3393 (3) | 0.5020 (4) | 0.0290 (9) | |
C1 | 0.2746 (6) | 0.1785 (3) | 0.7055 (4) | 0.0309 (10) | |
H1A | 0.1961 | 0.1609 | 0.7742 | 0.039 (4)* | |
H1B | 0.3697 | 0.1209 | 0.7065 | 0.039 (4)* | |
C3 | −0.0011 (6) | 0.3040 (3) | 0.5678 (5) | 0.0286 (10) | |
H3A | −0.0696 | 0.3226 | 0.4856 | 0.039 (4)* | |
H3B | −0.0892 | 0.2904 | 0.6313 | 0.039 (4)* | |
C2 | 0.3068 (6) | 0.2343 (4) | 0.4463 (5) | 0.0329 (11) | |
H2A | 0.4033 | 0.1790 | 0.4371 | 0.039 (4)* | |
H2B | 0.2477 | 0.2502 | 0.3603 | 0.039 (4)* | |
C4 | 0.2226 (6) | 0.3779 (4) | 0.7348 (5) | 0.0317 (10) | |
H4A | 0.1368 | 0.3570 | 0.7976 | 0.039 (4)* | |
H4B | 0.2833 | 0.4473 | 0.7652 | 0.039 (4)* | |
C5 | 0.2486 (6) | 0.4264 (3) | 0.5128 (5) | 0.0317 (10) | |
H5A | 0.1797 | 0.4357 | 0.4286 | 0.039 (4)* | |
H5B | 0.3090 | 0.4979 | 0.5352 | 0.039 (4)* | |
C6 | 0.4836 (6) | 0.3187 (4) | 0.6307 (5) | 0.0321 (11) | |
H6A | 0.5526 | 0.3861 | 0.6581 | 0.039 (4)* | |
H6B | 0.5717 | 0.2577 | 0.6240 | 0.039 (4)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pd1 | 0.0204 (2) | 0.0172 (2) | 0.0232 (2) | 0.00008 (18) | 0.00011 (17) | −0.00444 (19) |
Br1 | 0.0391 (3) | 0.0288 (3) | 0.0472 (3) | 0.0026 (2) | 0.0185 (2) | −0.0075 (2) |
P1 | 0.0203 (5) | 0.0183 (5) | 0.0268 (6) | −0.0011 (4) | 0.0020 (5) | −0.0040 (4) |
N1 | 0.031 (2) | 0.0189 (17) | 0.030 (2) | −0.0061 (15) | −0.0073 (17) | −0.0010 (15) |
N3 | 0.0249 (18) | 0.0163 (17) | 0.035 (2) | 0.0013 (14) | 0.0015 (16) | −0.0026 (14) |
N2 | 0.028 (2) | 0.0237 (19) | 0.036 (2) | −0.0079 (15) | 0.0085 (18) | −0.0027 (16) |
C1 | 0.034 (2) | 0.021 (2) | 0.037 (3) | −0.0068 (18) | −0.004 (2) | 0.0069 (19) |
C3 | 0.022 (2) | 0.024 (2) | 0.039 (3) | 0.0041 (17) | −0.002 (2) | −0.0033 (19) |
C2 | 0.036 (3) | 0.034 (2) | 0.031 (3) | −0.005 (2) | 0.012 (2) | −0.0109 (19) |
C4 | 0.039 (3) | 0.024 (2) | 0.032 (3) | −0.0047 (19) | 0.002 (2) | −0.0097 (19) |
C5 | 0.035 (2) | 0.022 (2) | 0.037 (3) | −0.0022 (19) | 0.000 (2) | 0.0061 (19) |
C6 | 0.020 (2) | 0.021 (2) | 0.054 (3) | −0.0010 (17) | −0.003 (2) | 0.003 (2) |
Geometric parameters (Å, º) top
Pd1—P1 | 2.312 (1) | N2—C5 | 1.466 (5) |
Pd1—P1i | 2.312 (1) | N2—C2 | 1.473 (5) |
Pd1—Br1 | 2.427 (1) | C1—H1A | 0.9700 |
Pd1—Br1i | 2.427 (1) | C1—H1B | 0.9700 |
P1—C2 | 1.836 (4) | C3—H3A | 0.9700 |
P1—C1 | 1.838 (5) | C3—H3B | 0.9700 |
P1—C3 | 1.847 (4) | C2—H2A | 0.9700 |
N1—C4 | 1.460 (5) | C2—H2B | 0.9700 |
N1—C1 | 1.465 (5) | C4—H4A | 0.9700 |
N1—C6 | 1.472 (6) | C4—H4B | 0.9700 |
N3—C4 | 1.456 (6) | C5—H5A | 0.9700 |
N3—C3 | 1.476 (5) | C5—H5B | 0.9700 |
N3—C5 | 1.477 (5) | C6—H6A | 0.9700 |
N2—C6 | 1.459 (6) | C6—H6B | 0.9700 |
| | | |
P1—Pd1—P1i | 180.0 | P1—C3—H3A | 109.4 |
P1—Pd1—Br1 | 90.55 (3) | N3—C3—H3B | 109.4 |
P1i—Pd1—Br1 | 89.45 (3) | P1—C3—H3B | 109.4 |
P1—Pd1—Br1i | 89.45 (3) | H3A—C3—H3B | 108.0 |
P1i—Pd1—Br1i | 90.55 (3) | N2—C2—P1 | 112.1 (3) |
Br1—Pd1—Br1i | 180.0 | N2—C2—H2A | 109.2 |
C2—P1—C1 | 98.5 (2) | P1—C2—H2A | 109.2 |
C2—P1—C3 | 98.2 (2) | N2—C2—H2B | 109.2 |
C1—P1—C3 | 98.1 (2) | P1—C2—H2B | 109.2 |
C2—P1—Pd1 | 121.1 (1) | H2A—C2—H2B | 107.9 |
C1—P1—Pd1 | 113.8 (1) | N3—C4—N1 | 115.1 (3) |
C3—P1—Pd1 | 122.4 (1) | N3—C4—H4A | 108.5 |
C4—N1—C1 | 110.8 (3) | N1—C4—H4A | 108.5 |
C4—N1—C6 | 107.7 (3) | N3—C4—H4B | 108.5 |
C1—N1—C6 | 110.9 (3) | N1—C4—H4B | 108.5 |
C4—N3—C3 | 111.8 (3) | H4A—C4—H4B | 107.5 |
C4—N3—C5 | 108.8 (3) | N2—C5—N3 | 113.7 (3) |
C3—N3—C5 | 110.6 (3) | N2—C5—H5A | 108.8 |
C6—N2—C5 | 108.8 (3) | N3—C5—H5A | 108.8 |
C6—N2—C2 | 111.0 (3) | N2—C5—H5B | 108.8 |
C5—N2—C2 | 110.7 (3) | N3—C5—H5B | 108.8 |
N1—C1—P1 | 112.6 (3) | H5A—C5—H5B | 107.7 |
N1—C1—H1A | 109.1 | N2—C6—N1 | 115.1 (3) |
P1—C1—H1A | 109.1 | N2—C6—H6A | 108.5 |
N1—C1—H1B | 109.1 | N1—C6—H6A | 108.5 |
P1—C1—H1B | 109.1 | N2—C6—H6B | 108.5 |
H1A—C1—H1B | 107.8 | N1—C6—H6B | 108.5 |
N3—C3—P1 | 111.3 (3) | H6A—C6—H6B | 107.5 |
N3—C3—H3A | 109.4 | | |
| | | |
Br1—Pd1—P1—C1 | −100.2 (2) | Br1—Pd1—P1—C3 | 142.4 (2) |
Br1—Pd1—P1—C2 | 16.9 (2) | | |
Symmetry code: (i) −x, −y, −z+1. |
Comparative geometrical parameters (Å) for selected
trans-[PdBr2(L)2] (L = tertiary phosphine ligand) complexes topL | Pd—P | Pd—Br |
PTAa | 2.320 (1) | 2.427 (1) |
PPh2(o-Cl-Ph)b | 2.350 (2) | 2.423 (1) |
DDEPc | 2.325 (3) | 2.412 (1) |
DPAd | 2.322 (2) | 2.447 (1) |
ppqe | 2.318 (1) | 2.435 (1) |
DMPPf | 2.319 (2) | 2.433 (1) |
| 2.313 (2) | 2.435 (1) |
PPh3g | 2.34 (4) | 2.42 (4) |
P(o-Tol)3h | 2.370 (1) | 2.445 (2) |
Notes: (a) this work;
(b) Coalter et al. (2000);
(c) Ganguly et al. (1992) [DDEP is 2-(diphenylphosphino)ethanephosphonate];
(d) Podlahova et al. (1979) (DPA is diphenylphosphinoacetic acid);
(e) Sembiring et al. (1995) (ppq is p-quinonyldiphenylphosphine);
(f) Wilson et al. (1996) (DMPP is 1-phenyl-3,4-dimethylphosphole);
(g) Stark et al. (1997);
(h) Vicente et al. (1997). |
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