trans-Di­bromo­bis(1,3,5-tri­aza-7-phosphaadamantane-κP)­palladium(II)

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°.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](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

---

Computing details

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)

Crystal data

[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) Å^3	Rectangle, yellow
Z = 2	0.18 × 0.09 × 0.06 mm

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.084	H-atom parameters constrained
S = 0.94	w = 1/[σ^2(Fo^2) + (0.038P)^2] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Pd1—P1	2.312 (1)	N2—C5	1.466 (5)
Pd1—P1^i	2.312 (1)	N2—C2	1.473 (5)
Pd1—Br1	2.427 (1)	C1—H1A	0.9700
Pd1—Br1^i	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—P1^i	180.0	P1—C3—H3A	109.4
P1—Pd1—Br1	90.55 (3)	N3—C3—H3B	109.4
P1^i—Pd1—Br1	89.45 (3)	P1—C3—H3B	109.4
P1—Pd1—Br1^i	89.45 (3)	H3A—C3—H3B	108.0
P1^i—Pd1—Br1^i	90.55 (3)	N2—C2—P1	112.1 (3)
Br1—Pd1—Br1^i	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.