Pentane-1,5-diammonium tetra-chlorido-palladate(II).

In the title compound, [NH(3)(CH(2))(5)NH(3)][PdCl(4)], the square-planar [PdCl(4)](2-) anions are centrosymmetric while the diammonium cation lies in a general position. In addition to electrostatic inter-actions, the two species are linked through N-H⋯Cl hydrogen bonds to form a three-dimensional network.

Related literature

The title compound is isostructural with its tetra­chlorido- and tetra­bromido­cuprate(II) analogues (Garland et al., 1990 ▶). For similar tetra­chlorido­palladate(II) compounds, see: Willett & Willett (1977 ▶); Berg & Søtofte (1976 ▶); Maris et al. (1996 ▶).

Experimental

Crystal data

(C5H16N2)[PdCl4]

M = 352.40

Monoclinic,

a = 8.091 (2) Å

b = 7.276 (2) Å

c = 20.843 (5) Å

β = 98.279 (2)°

V = 1214.2 (5) Å3

Z = 4

Mo Kα radiation

μ = 2.37 mm−1

T = 298 K

0.19 × 0.15 × 0.08 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: integration (Blessing; 1989 ▶) T min = 0.662, T max = 0.833

2816 measured reflections

2783 independent reflections

2771 reflections with I > 2σ(I)

R int = 0.025

5 standard reflections frequency: 60 min intensity decay: none

Refinement

R[F 2 > 2σ(F 2)] = 0.036

wR(F 2) = 0.089

S = 0.99

2783 reflections

112 parameters

H-atom parameters constrained

Δρmax = 0.74 e Å−3

Δρmin = −0.69 e Å−3

Data collection: CAD-4-PC Software (Enraf–Nonius, 1992 ▶); cell refinement: CAD-4-PC Software; data reduction: modified version of NRC-2/NRC2A (Ahmed et al., 1973 ▶); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: ATOMS (Dowty, 2003 ▶) and Materials Studio (Accelrys, 2002 ▶); software used to prepare material for publication: UdMX (Maris, 2004 ▶) and publCIF (Westrip, 2007 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807061430/sj2439sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807061430/sj2439Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C5H16N2)[PdCl4]	F000 = 696
Mr = 352.40	Dx = 1.928 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 8.091 (2) Å	θ = 7.5–16.8º
b = 7.276 (2) Å	µ = 2.37 mm−1
c = 20.843 (5) Å	T = 298 K
β = 98.279 (2)º	Plate, dark red
V = 1214.2 (5) Å3	0.19 × 0.15 × 0.08 mm
Z = 4

Enraf–Nonius CAD-4 diffractometer	Rint = 0.025
Radiation source: fine-focus sealed tube	θmax = 27.4º
Monochromator: graphite	θmin = 2.0º
T = 298 K	h = −10→10
ω/2θ scans	k = 0→9
Absorption correction: integration(Blessing; 1989)	l = 0→26
Tmin = 0.662, Tmax = 0.833	5 standard reflections
2816 measured reflections	every 60 min
2783 independent reflections	intensity decay: none
2771 reflections with I > 2σ(I)

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)] = 0.036	H-atom parameters constrained
wR(F2) = 0.089	w = 1/[σ2(Fo2) + (0.0883P)2] where P = (Fo2 + 2Fc2)/3
S = 0.99	(Δ/σ)max = 0.003
2783 reflections	Δρmax = 0.74 e Å−3
112 parameters	Δρmin = −0.68 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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 > 2σ(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.

	x	y	z	Uiso*/Ueq
Pd1	0.0000	0.0000	0.0000	0.01948 (10)
Cl1	0.09323 (3)	0.01856 (2)	0.110313 (8)	0.03247 (10)
Cl2	−0.195673 (16)	−0.21942 (2)	0.017283 (7)	0.02727 (10)
Pd2	0.5000	0.5000	0.0000	0.01998 (10)
Cl3	0.711649 (16)	0.285055 (19)	0.022152 (8)	0.02908 (10)
Cl4	0.51179 (2)	0.46485 (3)	−0.109913 (8)	0.03058 (10)
N1	0.07248 (18)	0.49394 (9)	0.10015 (5)	0.0386 (2)
H1A	0.0198	0.5472	0.0645	0.058*
H1B	0.0736	0.3727	0.0945	0.058*
H1C	0.1769	0.5355	0.1080	0.058*
C2	−0.01184 (11)	0.53613 (14)	0.15356 (5)	0.03569 (19)
H2A	−0.1260	0.4924	0.1441	0.043*
H2B	−0.0157	0.6686	0.1583	0.043*
C3	0.06862 (13)	0.45279 (14)	0.21793 (4)	0.0467 (2)
H3A	−0.0062	0.4706	0.2498	0.056*
H3B	0.0809	0.3215	0.2121	0.056*
C4	0.23397 (14)	0.5307 (2)	0.24383 (5)	0.0461 (3)
H4A	0.2259	0.6637	0.2437	0.055*
H4B	0.3137	0.4964	0.2154	0.055*
C5	0.29934 (12)	0.46619 (13)	0.31257 (4)	0.04003 (19)
H5A	0.2217	0.5039	0.3415	0.048*
H5B	0.3047	0.3330	0.3132	0.048*
C6	0.46483 (13)	0.54043 (14)	0.33643 (4)	0.0408 (2)
H6A	0.4639	0.6727	0.3306	0.049*
H6B	0.5461	0.4890	0.3115	0.049*
N7	0.51365 (16)	0.49611 (10)	0.40599 (6)	0.0420 (2)
H7A	0.6148	0.5415	0.4195	0.063*
H7B	0.5151	0.3747	0.4112	0.063*
H7C	0.4403	0.5456	0.4289	0.063*

	U11	U22	U33	U12	U13	U23
Pd1	0.01015 (15)	0.01755 (17)	0.03049 (14)	−0.00113 (1)	0.00208 (12)	−0.00208 (2)
Cl1	0.02387 (16)	0.04333 (16)	0.02952 (15)	−0.00249 (6)	0.00153 (11)	0.00146 (5)
Cl2	0.01297 (15)	0.02395 (15)	0.04395 (15)	−0.00589 (4)	0.00088 (10)	0.00250 (5)
Pd2	0.01077 (15)	0.01766 (17)	0.03179 (14)	0.00019 (1)	0.00401 (12)	−0.00195 (2)
Cl3	0.01415 (15)	0.02303 (15)	0.04964 (15)	0.00526 (5)	0.00317 (10)	−0.00050 (5)
Cl4	0.02803 (16)	0.03239 (15)	0.03202 (15)	−0.00018 (7)	0.00674 (10)	0.00025 (5)
N1	0.0377 (5)	0.0413 (5)	0.0359 (4)	−0.0059 (2)	0.0023 (4)	−0.0095 (2)
C2	0.0383 (5)	0.0295 (3)	0.0379 (4)	0.0061 (3)	0.0008 (3)	−0.0068 (3)
C3	0.0466 (5)	0.0525 (5)	0.0396 (4)	−0.0105 (4)	0.0016 (3)	0.0077 (4)
C4	0.0370 (5)	0.0562 (5)	0.0433 (5)	−0.0005 (4)	−0.0005 (4)	0.0053 (4)
C5	0.0324 (5)	0.0496 (4)	0.0390 (4)	−0.0051 (3)	0.0082 (3)	0.0042 (3)
C6	0.0456 (5)	0.0268 (3)	0.0465 (4)	−0.0104 (4)	−0.0055 (4)	0.0088 (3)
N7	0.0300 (5)	0.0518 (5)	0.0443 (5)	−0.0080 (2)	0.0057 (5)	0.0125 (3)

Pd1—Cl2	2.3129 (4)	C3—C4	1.4814 (13)
Pd1—Cl2i	2.3129 (4)	C3—H3A	0.9700
Pd1—Cl1	2.3183 (6)	C3—H3B	0.9700
Pd1—Cl1i	2.3183 (6)	C4—C5	1.5279 (16)
Pd2—Cl3ii	2.3160 (4)	C4—H4A	0.9700
Pd2—Cl3	2.3160 (4)	C4—H4B	0.9700
Pd2—Cl4	2.3207 (6)	C5—C6	1.4629 (13)
Pd2—Cl4ii	2.3207 (6)	C5—H5A	0.9700
N1—C2	1.4205 (14)	C5—H5B	0.9700
N1—H1A	0.8900	C6—N7	1.4822 (14)
N1—H1B	0.8900	C6—H6A	0.9700
N1—H1C	0.8900	C6—H6B	0.9700
C2—C3	1.5298 (13)	N7—H7A	0.8900
C2—H2A	0.9700	N7—H7B	0.8900
C2—H2B	0.9700	N7—H7C	0.8900
Pd1···Cl3iii	3.2044 (9)	Pd2···Cl2v	3.1788 (9)
Pd1···Cl3iv	3.2044 (9)	Pd2···Cl2vi	3.1789 (9)
Cl2—Pd1—Cl2i	180.0	C4—C3—H3B	108.6
Cl2—Pd1—Cl1	91.031 (9)	C2—C3—H3B	108.6
Cl2i—Pd1—Cl1	88.970 (10)	H3A—C3—H3B	107.6
Cl2—Pd1—Cl1i	88.969 (10)	C3—C4—C5	113.37 (10)
Cl2i—Pd1—Cl1i	91.030 (10)	C3—C4—H4A	108.9
Cl1—Pd1—Cl1i	180.000 (3)	C5—C4—H4A	108.9
Cl3ii—Pd2—Cl3	180.0	C3—C4—H4B	108.9
Cl3ii—Pd2—Cl4	90.681 (8)	C5—C4—H4B	108.9
Cl3—Pd2—Cl4	89.317 (8)	H4A—C4—H4B	107.7
Cl3ii—Pd2—Cl4ii	89.320 (9)	C6—C5—C4	112.44 (8)
Cl3—Pd2—Cl4ii	90.682 (8)	C6—C5—H5A	109.1
Cl4—Pd2—Cl4ii	180.0	C4—C5—H5A	109.1
C2—N1—H1A	109.5	C6—C5—H5B	109.1
C2—N1—H1B	109.5	C4—C5—H5B	109.1
H1A—N1—H1B	109.5	H5A—C5—H5B	107.8
C2—N1—H1C	109.5	C5—C6—N7	110.74 (8)
H1A—N1—H1C	109.5	C5—C6—H6A	109.5
H1B—N1—H1C	109.5	N7—C6—H6A	109.5
N1—C2—C3	114.20 (9)	C5—C6—H6B	109.5
N1—C2—H2A	108.7	N7—C6—H6B	109.5
C3—C2—H2A	108.7	H6A—C6—H6B	108.1
N1—C2—H2B	108.7	C6—N7—H7A	109.5
C3—C2—H2B	108.7	C6—N7—H7B	109.5
H2A—C2—H2B	107.6	H7A—N7—H7B	109.5
C4—C3—C2	114.57 (9)	C6—N7—H7C	109.5
C4—C3—H3A	108.6	H7A—N7—H7C	109.5
C2—C3—H3A	108.6	H7B—N7—H7C	109.5
N1—C2—C3—C4	67.86 (12)	C3—C4—C5—C6	178.30 (9)
C2—C3—C4—C5	171.37 (9)	C4—C5—C6—N7	172.18 (9)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1B···Cl2i	0.89	2.88	3.4171 (11)	120
N1—H1C···Cl4ii	0.89	2.51	3.3539 (17)	158
N1—H1A···Cl2vii	0.89	2.53	3.3107 (13)	147
N1—H1B···Cl1	0.89	2.60	3.4680 (12)	165
N7—H7A···Cl1viii	0.89	2.53	3.2512 (15)	138
N7—H7B···Cl4ix	0.89	2.51	3.3702 (12)	163
N7—H7C···Cl3viii	0.89	2.44	3.2821 (13)	158
N7—H7A···Cl2x	0.89	2.70	3.4614 (13)	145
N7—H7B···Cl3ix	0.89	2.86	3.3907 (11)	120

Table 1

Selected bond lengths (Å)

Pd1—Cl2	2.3129 (4)
Pd1—Cl1	2.3183 (6)
Pd2—Cl3	2.3160 (4)
Pd2—Cl4	2.3207 (6)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1B⋯Cl2i	0.89	2.88	3.4171 (11)	120
N1—H1C⋯Cl4ii	0.89	2.51	3.3539 (17)	158
N1—H1A⋯Cl2iii	0.89	2.53	3.3107 (13)	147
N1—H1B⋯Cl1	0.89	2.60	3.4680 (12)	165
N7—H7A⋯Cl1iv	0.89	2.53	3.2512 (15)	138
N7—H7B⋯Cl4v	0.89	2.51	3.3702 (12)	163
N7—H7C⋯Cl3iv	0.89	2.44	3.2821 (13)	158
N7—H7A⋯Cl2vi	0.89	2.70	3.4614 (13)	145
N7—H7B⋯Cl3v	0.89	2.86	3.3907 (11)	120

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .