Dichloro­bis(N-methyl­aniline)palladium(II)

The title complex, [PdCl₂(C₇H₉N)₂], has crystallographic inversion symmetry. It forms a layered structure through N—H...Cl hydrogen bonds. The Pd^II ion is in a square-planar coordination.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.020 Å
• R factor = 0.074
• wR factor = 0.193
• Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C7
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.03
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         20

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   3 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
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Siemens, 1994)); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Dichlorobis(N-methylaniline)palladium(II)

Crystal data

[PdCl2(C7H9N)2]	F(000) = 392
Mr = 391.62	Dx = 1.654 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2765 reflections
a = 6.1411 (11) Å	θ = 2.6–25.0°
b = 15.501 (3) Å	µ = 1.51 mm^−1
c = 8.5024 (17) Å	T = 293 K
β = 103.685 (3)°	Prism, yellow
V = 786.4 (3) Å^3	0.35 × 0.22 × 0.10 mm
Z = 2

Data collection

Bruker SMART 1K diffractometer	1373 independent reflections
Radiation source: fine-focus sealed tube	888 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.070
φ and ω scans	θmax = 25.0°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −5→7
Tmin = 0.678, Tmax = 0.860	k = −18→10
2765 measured reflections	l = −9→10

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)] = 0.074	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.193	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0909P)^2 + 3.5006P] where P = (Fo^2 + 2Fc^2)/3
1373 reflections	(Δ/σ)max < 0.001
88 parameters	Δρmax = 1.38 e Å^−3
0 restraints	Δρmin = −1.18 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.5000	0.5000	0.5000	0.0344 (4)
Cl1	0.7372 (5)	0.5564 (2)	0.3535 (3)	0.0505 (8)
N1	0.2287 (15)	0.4923 (6)	0.3025 (10)	0.039 (2)
H1A	0.1064	0.4931	0.3455	0.047*
C2	0.1966 (18)	0.5685 (8)	0.1873 (13)	0.044 (3)
H2A	0.0666	0.5590	0.1008	0.066*
H2B	0.3263	0.5745	0.1435	0.066*
H2C	0.1767	0.6201	0.2447	0.066*
C3	0.2149 (19)	0.4107 (7)	0.2171 (13)	0.039 (3)
C4	0.343 (3)	0.3143 (9)	0.0408 (15)	0.062 (4)
H4A	0.4455	0.3014	−0.0206	0.074*
C5	0.368 (2)	0.3894 (8)	0.1277 (15)	0.054 (3)
H5A	0.4877	0.4260	0.1267	0.065*
C6	0.047 (2)	0.3541 (8)	0.2221 (16)	0.056 (3)
H6A	−0.0530	0.3666	0.2860	0.067*
C7	0.022 (3)	0.2781 (9)	0.133 (2)	0.084 (5)
H7A	−0.0963	0.2407	0.1351	0.100*
C8	0.175 (3)	0.2583 (10)	0.0411 (18)	0.075 (5)
H8A	0.1610	0.2076	−0.0190	0.090*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.0354 (7)	0.0411 (7)	0.0227 (6)	0.0054 (7)	−0.0010 (4)	0.0023 (6)
Cl1	0.0441 (16)	0.068 (2)	0.0377 (15)	0.0051 (16)	0.0057 (12)	0.0153 (15)
N1	0.043 (5)	0.042 (5)	0.027 (4)	0.004 (5)	−0.005 (4)	0.010 (4)
C2	0.046 (7)	0.049 (7)	0.030 (6)	0.002 (6)	−0.006 (5)	0.008 (5)
C3	0.050 (7)	0.035 (6)	0.026 (6)	0.007 (6)	−0.006 (5)	0.009 (5)
C4	0.077 (9)	0.067 (9)	0.037 (7)	0.007 (8)	0.005 (7)	−0.018 (7)
C5	0.063 (8)	0.049 (8)	0.046 (7)	0.009 (7)	0.006 (6)	0.004 (6)
C6	0.062 (8)	0.052 (8)	0.054 (8)	0.000 (7)	0.014 (7)	0.004 (7)
C7	0.109 (13)	0.039 (8)	0.082 (12)	−0.023 (9)	−0.020 (10)	0.010 (8)
C8	0.116 (14)	0.051 (9)	0.050 (9)	0.010 (10)	0.005 (9)	−0.005 (7)

Geometric parameters (Å, º)

Pd1—N1^i	2.070 (8)	C3—C5	1.382 (17)
Pd1—N1	2.070 (8)	C4—C8	1.35 (2)
Pd1—Cl1	2.302 (3)	C4—C5	1.368 (17)
Pd1—Cl1^i	2.302 (3)	C4—H4A	0.9300
N1—C3	1.452 (14)	C5—H5A	0.9300
N1—C2	1.516 (13)	C6—C7	1.389 (18)
N1—H1A	0.9100	C6—H6A	0.9300
C2—H2A	0.9600	C7—C8	1.39 (2)
C2—H2B	0.9600	C7—H7A	0.9300
C2—H2C	0.9600	C8—H8A	0.9300
C3—C6	1.363 (16)
N1^i—Pd1—N1	180.000 (1)	C6—C3—C5	118.9 (11)
N1^i—Pd1—Cl1	85.8 (3)	C6—C3—N1	120.0 (11)
N1—Pd1—Cl1	94.2 (3)	C5—C3—N1	121.0 (11)
N1^i—Pd1—Cl1^i	94.2 (3)	C8—C4—C5	122.3 (14)
N1—Pd1—Cl1^i	85.8 (3)	C8—C4—H4A	118.9
Cl1—Pd1—Cl1^i	180.00 (16)	C5—C4—H4A	118.9
C3—N1—C2	111.9 (8)	C4—C5—C3	119.7 (13)
C3—N1—Pd1	113.3 (6)	C4—C5—H5A	120.1
C2—N1—Pd1	115.8 (7)	C3—C5—H5A	120.1
C3—N1—H1A	104.8	C3—C6—C7	121.1 (13)
C2—N1—H1A	104.8	C3—C6—H6A	119.5
Pd1—N1—H1A	104.8	C7—C6—H6A	119.5
N1—C2—H2A	109.5	C6—C7—C8	119.3 (14)
N1—C2—H2B	109.5	C6—C7—H7A	120.3
H2A—C2—H2B	109.5	C8—C7—H7A	120.3
N1—C2—H2C	109.5	C4—C8—C7	118.6 (14)
H2A—C2—H2C	109.5	C4—C8—H8A	120.7
H2B—C2—H2C	109.5	C7—C8—H8A	120.7

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1^ii	0.91	2.49	3.302 (10)	149

Symmetry code: (ii) x−1, y, z.