Bis(3-aza­niumylpyridin-1-ium) hexa­chloridostannate(IV) dichloride

Megen, M. van; Prömper, S.; Reiss, G.J.

doi:10.1107/S1600536813006806

metal-organic compounds

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Volume 69| Part 4| April 2013| Page m217

doi:10.1107/S1600536813006806

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Bis(3-azaniumylpyridin-1-ium) hexachloridostannate(IV) dichloride

Martin van Megen,^a Stephan Prömper ^a and Guido J. Reiss ^a ^*

^aInstitut für Anorganische Chemie und Strukturchemie, Lehrstuhl II: Material- und Strukturforschung, Heinrich-Heine-Universität Düsseldorf, Universitätsstrasse 1, D-40225 Düsseldorf, Germany
^*Correspondence e-mail: reissg@hhu.de

(Received 4 March 2013; accepted 11 March 2013; online 16 March 2013)

The asymmetric unit of the title compound, (C₅H₈N₂)₂[SnCl₆]Cl₂, consists of one 3-azaniumylpyridin-1-ium dication and one chloride ion in a general position and a hexachloridostannate(IV) dianion lying about a centre of inversion. The [SnCl₆]²⁻ anion exhibits almost perfect octahedral geometry. The 3-azaniumylpyridin-1-ium and chloride ions are connected via medium–strong charge-supported N—H⋯Cl hydrogen bonds, forming undulating layers in the (110) plane. The [SnCl₆]²⁻ ions are located between these layers and occupy cavities formed by two facing layer puckers.

Related literature

For related 3-azaniumylpyridin-1-ium salts, see: Ali et al. (2008 ); Kapoor et al. (2012 ); Rao et al. (2011 ); Sarma et al. (2012 ); Willett et al. (1988 ). For related hexahalogenidometalate salts, see: Reiss (1998 , 2002 ); Reiss & Helmbrecht (2012 ). For spectroscopy of hexachloridostannate(IV) salts, see: Brown et al. (1970 ); Ouasri et al. (2001 ). For graph-set theory and its applications, see: Bernstein et al. (1995 ); Etter et al. (1990 ).

Experimental

Crystal data

(C₅H₈N₂)₂[SnCl₆]Cl₂
M_r = 594.56
Orthorhombic, P b c a
a = 11.9379 (3) Å
b = 10.3704 (3) Å
c = 16.7018 (5) Å
V = 2067.70 (10) Å³
Z = 4
Mo Kα radiation
μ = 2.27 mm⁻¹
T = 290 K
0.14 × 0.12 × 0.06 mm

Data collection

Oxford Diffraction Xcalibur Eos diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]$ ) T_min = 0.853, T_max = 1.000
30476 measured reflections
2364 independent reflections
1875 reflections with I > 2σ(I)
R_int = 0.038

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.044
S = 1.06
2364 reflections
138 parameters
All H-atom parameters refined
Δρ_max = 0.26 e Å⁻³
Δρ_min = −0.22 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H11⋯Cl1	0.94 (2)	2.23 (3)	3.135 (2)	161 (2)
N1—H12⋯Cl2ⁱ	0.91 (3)	2.48 (3)	3.343 (2)	160 (2)
N1—H13⋯Cl1ⁱⁱ	0.92 (3)	2.19 (3)	3.104 (2)	176 (2)
N2—H2⋯Cl1ⁱⁱⁱ	0.86 (2)	2.21 (2)	3.055 (2)	167 (2)
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (iii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CrysAlis PRO (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]$ ); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2012 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536813006806/pk2471sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813006806/pk2471Isup2.hkl

checkCIF report

Comment top

Only a limited number of 3-azaniumylpyridin-1-ium containing compounds has structurally been characterized so far. The majority of these are salts consisting of halogenidometalate anions such as [BiCl₆]^3- (Rao et al., 2011), [CuCl₄]^2- (Willett et al., 1988), [CuBr₄]^2- (Willett et al., 1988) and [HgBr₄]^2- (Ali et al., 2008). Furthermore, the dinitrate (Kapoor et al., 2012) and some complex crown ether compounds (Sarma et al., 2012) have been reported. This study on (C₅H₈N₂)₂[SnCl₆]Cl₂ is part of our long standing interest on the principles of arrangement of simple hexahalogenidometalate salts (dipH = diisopropylaminium): (dipH)₂[SiF₆] (Reiss, 1998); (dipH)₂[IrCl₆] (Reiss, 2002); (dipH)₂[SnCl₆] (Reiss & Helmbrecht, 2012).

The asymmetric unit of the title compound, (C₅H₈N₂)₂[SnCl₆]Cl₂, consists of one 3-azaniumylpyridin-1-ium dication and one chloride ion in general positions and the hexachloridostannate(IV) dianion lying on a centre of inversion (Fig. 1). The C–N and C–C bond lengths and angles of the cation are within the expected ranges. The [SnCl₆]^2- dianion exhibits a nearly perfect octahedral coordination sphere with Sn–Cl bond lengths ranging from 2.4162 (5) to 2.4242 (5) Å and bond angles between 88.03 (2) and 91.97 (2)°. The 3-azaniumylpyridin-1-ium dications and chloride ions are connected by medium strong, charge supported hydrogen bonds (Table 1) forming layers in the [110] plane. The characteristic hydrogen bonding motif is a 18-membered, wavy ring, which is classified as a third level graph-set R₆³(18) (Etter et al., 1990; Fig. 2). In addition to that, the second level graph-set descriptors C₂¹(4) and C₂¹(7) represent the chains, bridging the dications and chloride ions along [010] and [100], respectively. Thereby, the NH₃⁺ group as well as the NH⁺ group of the 3-azaniumylpyridin-1-ium dication acts as a hydrogen bond donor. D···A distances for the NH₃⁺ group range from 3.104 (2) to 3.343 (2) Å and for the NH⁺ group a D···A distance of 3.055 (2) Å is found. The [SnCl₆]^2- dianions are located in cavities between the layers, connected to the 3-azaniumylpyridin-1-ium dications by weak hydrogen bonds (Table 1) between two of their chlorido ligands and neighbouring NH₃⁺groups (Fig. 3). The Raman-active bands (ν₁, ν₂, ν₄ and ν₅) of the [SnCl₆]^2- dianion appear in the Raman spectrum of the title compound (C₅H₈N₂)₂[SnCl₆]Cl₂ (Brown et al., 1970; Ouasri et al., 2001).

Related literature top

For related 3-azaniumylpyridin-1-ium salts, see: Ali et al. (2008); Kapoor et al. (2012); Rao et al. (2011); Sarma et al. (2012); Willett et al. (1988). For related hexahalogenidometalate salts, see: Reiss (1998, 2002); Reiss & Helmbrecht (2012). For spectroscopy of hexachloridostannate(IV) salts, see: Brown et al. (1970); Ouasri et al. (2001). For graph-set theory and its applications, see: Bernstein et al. (1995); Etter et al. (1990).

Experimental top

The title compound, (C₅H₈N₂)₂[SnCl₆]Cl₂, was prepared by dissolving 0.47 g (5.0 mmol) 3-aminopyridine and 0.65 g (2.5 mmol) tin(IV) chloride in 10 ml of concentrated (37%) hydrochloric acid. Within two to three days under ambient conditions colourless, rod-shaped crystals were obtained by slow evaporation of the solvent. The Raman spectrum was measured using a Bruker MULTIRAM spectrometer (Nd:YAG-Laser at 1064 nm; RT-InGaAs-detector); 4000–70 cm^-1: 3082(w), 3049(w), 2954(vw), 1646(w), 1625(w), 1502(w), 1231(w), 1188(w), 1046(m), 1030(m), 815(w), 627(w), 537(w), 324(vs; ν₁, Sn–Cl), 241 (m, br; ν₂, Sn–Cl), 172 (s; ν₄, Sn–Cl), 158 (s; ν₅, Sn–Cl), 98 (m; most likely a lattice mode). - IR spectroscopic data were recorded on a Digilab FT3400 spectrometer using a MIRacle ATR unit (Pike Technologies); 4000–560 cm^-1: 3458(w), 3364(w), 3245(w), 3187(w), 3080(s), 3066(s), 3008(m), 2952(m), 2880(m), 2773(vs), 2739(vs), 2687(s), 2604(s), 2542(vs), 1892(w, br), 1644(w), 1624(w), 1556(s), 1499(s), 1472(w), 1380(m), 1318(m), 1131(m), 1123(m), 1092(w), 1009(w), 998(w), 941(w), 890(w), 798(m), 673(m), 625(w). - Elemental analyses (C, H, N) were performed with a HEKA-Tech Euro EA3000 instrument; SnCl₈N₄C₁₀H₁₆ (594.60): calcd. C 20.20, H 2.71, N 9.42; found C 20.38, H 2.54, N 9.34.

Computing details top

Data collection: CrysAlis PRO (Oxford Diffraction, 2009); cell refinement: CrysAlis PRO (Oxford Diffraction, 2009); data reduction: CrysAlis PRO (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2012); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. The asymmetric unit of the title compound plus the symmetry-related chlorido ligands completing the hexachloridostannate(IV) dianion (displacement ellipsoids are drawn at the 50% probability level; hydrogen atoms are drawn as spheres with arbitrary radii; symmetry code: -x, -y, -z).
	Fig. 2. View on a hydrogen bonded layer of 3-azaniumylpyridin-1-ium dications and chloride anions in the [110] plane (graph-set descriptors R₆³(18), C₂¹(4) and C₂¹(7) are indicated with green, red and blue numbers; symmetry code: ' 0.5 - x, 0.5 + y, z, '' 1 - x, 0.5 + y, 0.5 - z).
	Fig. 3. View along [110] on the title structure. Showing the hydrogen bonded layers consisting of 3-azaniumylpyridin-1-ium and chloride ions (parallel to ab at c = 1/4, 3/4) with the [SnCl₆]^2- dianions (parallel to ab at c = 0, 1/2, 1) located in cavities between them.

Bis(3-azaniumylpyridin-1-ium) hexachloridostannate(IV) dichloride top

Crystal data top

(C₅H₈N₂)₂[SnCl₆]Cl₂	F(000) = 1160
M_r = 594.56	D_x = 1.910 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 11374 reflections
a = 11.9379 (3) Å	θ = 3.6–33.9°
b = 10.3704 (3) Å	µ = 2.27 mm⁻¹
c = 16.7018 (5) Å	T = 290 K
V = 2067.70 (10) Å³	Block, colourless
Z = 4	0.14 × 0.12 × 0.06 mm

Data collection top

Oxford Diffraction Xcalibur Eos diffractometer	2364 independent reflections
Radiation source: fine-focus sealed tube	1875 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
Detector resolution: 16.2711 pixels mm^-1	θ_max = 27.5°, θ_min = 3.6°
ω scans	h = −15→15
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009)	k = −13→13
T_min = 0.853, T_max = 1.000	l = −21→21
30476 measured reflections

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)] = 0.020	Hydrogen site location: difference Fourier map
wR(F²) = 0.044	All H-atom parameters refined
S = 1.06	w = 1/[σ²(F_o²) + (0.0162P)² + 0.6462P] where P = (F_o² + 2F_c²)/3
2364 reflections	(Δ/σ)_max < 0.001
138 parameters	Δρ_max = 0.26 e Å⁻³
0 restraints	Δρ_min = −0.22 e Å⁻³

Crystal data top

(C₅H₈N₂)₂[SnCl₆]Cl₂	V = 2067.70 (10) Å³
M_r = 594.56	Z = 4
Orthorhombic, Pbca	Mo Kα radiation
a = 11.9379 (3) Å	µ = 2.27 mm⁻¹
b = 10.3704 (3) Å	T = 290 K
c = 16.7018 (5) Å	0.14 × 0.12 × 0.06 mm

Data collection top

Oxford Diffraction Xcalibur Eos diffractometer	2364 independent reflections
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009)	1875 reflections with I > 2σ(I)
T_min = 0.853, T_max = 1.000	R_int = 0.038
30476 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	0 restraints
wR(F²) = 0.044	All H-atom parameters refined
S = 1.06	Δρ_max = 0.26 e Å⁻³
2364 reflections	Δρ_min = −0.22 e Å⁻³
138 parameters

Special details top

Experimental. CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

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	U_iso*/U_eq
N1	0.28997 (16)	0.5670 (2)	0.35522 (13)	0.0399 (4)
H11	0.262 (2)	0.496 (2)	0.3270 (14)	0.059 (8)*
H12	0.257 (2)	0.574 (2)	0.4040 (16)	0.076 (9)*
H13	0.273 (2)	0.639 (2)	0.3256 (14)	0.060 (8)*
C1	0.41111 (17)	0.55437 (19)	0.36189 (11)	0.0308 (4)
C2	0.4574 (2)	0.4437 (2)	0.39366 (14)	0.0433 (5)
H2A	0.4103 (19)	0.381 (2)	0.4093 (13)	0.048 (7)*
C3	0.5719 (2)	0.4332 (2)	0.39775 (15)	0.0511 (6)
H3A	0.603 (2)	0.364 (2)	0.4159 (14)	0.061 (8)*
C4	0.6373 (2)	0.5311 (3)	0.37014 (14)	0.0472 (6)
H4A	0.712 (2)	0.529 (2)	0.3692 (14)	0.060 (8)*
N2	0.58917 (16)	0.63570 (19)	0.33931 (10)	0.0395 (4)
H2	0.630 (2)	0.695 (2)	0.3187 (14)	0.061 (8)*
C5	0.47825 (17)	0.65048 (19)	0.33392 (12)	0.0335 (5)
H5A	0.4526 (16)	0.7277 (19)	0.3111 (11)	0.033 (5)*
Cl1	0.25614 (5)	0.31396 (5)	0.25548 (3)	0.04263 (13)
Sn1	0.0000	0.0000	0.0000	0.02235 (6)
Cl2	0.14393 (4)	−0.16245 (5)	0.01538 (3)	0.04262 (13)
Cl3	−0.14685 (4)	−0.15423 (5)	0.02721 (3)	0.04332 (13)
Cl4	0.00932 (5)	0.04893 (7)	0.14177 (3)	0.05529 (16)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
N1	0.0356 (11)	0.0370 (11)	0.0470 (11)	−0.0016 (9)	0.0044 (9)	0.0035 (10)
C1	0.0342 (11)	0.0297 (10)	0.0285 (9)	−0.0009 (9)	0.0042 (8)	−0.0031 (8)
C2	0.0491 (14)	0.0340 (12)	0.0469 (13)	−0.0021 (11)	0.0031 (11)	0.0082 (11)
C3	0.0556 (17)	0.0417 (14)	0.0559 (15)	0.0141 (13)	−0.0052 (12)	0.0085 (12)
C4	0.0357 (13)	0.0564 (15)	0.0493 (13)	0.0017 (12)	−0.0005 (11)	−0.0078 (12)
N2	0.0384 (11)	0.0414 (11)	0.0388 (10)	−0.0095 (9)	0.0066 (8)	−0.0026 (8)
C5	0.0391 (14)	0.0288 (10)	0.0327 (10)	−0.0016 (9)	0.0045 (8)	0.0004 (8)
Cl1	0.0474 (3)	0.0329 (2)	0.0476 (3)	0.0018 (2)	0.0113 (2)	−0.0002 (2)
Sn1	0.01879 (9)	0.02282 (9)	0.02543 (9)	−0.00037 (7)	0.00169 (7)	−0.00180 (6)
Cl2	0.0341 (3)	0.0371 (3)	0.0566 (3)	0.0133 (2)	0.0059 (2)	0.0094 (2)
Cl3	0.0334 (3)	0.0338 (3)	0.0627 (3)	−0.0120 (2)	0.0084 (2)	0.0002 (2)
Cl4	0.0572 (4)	0.0802 (4)	0.0285 (3)	0.0001 (3)	−0.0011 (3)	−0.0142 (3)

Geometric parameters (Å, º) top

N1—C1	1.456 (3)	C4—H4A	0.90 (3)
N1—H11	0.94 (2)	N2—C5	1.336 (3)
N1—H12	0.91 (3)	N2—H2	0.86 (2)
N1—H13	0.92 (3)	C5—H5A	0.938 (19)
C1—C5	1.362 (3)	Sn1—Cl3ⁱ	2.4162 (5)
C1—C2	1.380 (3)	Sn1—Cl3	2.4162 (5)
C2—C3	1.373 (4)	Sn1—Cl2ⁱ	2.4200 (5)
C2—H2A	0.90 (2)	Sn1—Cl2	2.4200 (5)
C3—C4	1.361 (4)	Sn1—Cl4	2.4242 (5)
C3—H3A	0.86 (2)	Sn1—Cl4ⁱ	2.4242 (5)
C4—N2	1.331 (3)

C1—N1—H11	108.4 (16)	C5—N2—H2	117.0 (17)
C1—N1—H12	111.5 (17)	N2—C5—C1	118.4 (2)
H11—N1—H12	111 (2)	N2—C5—H5A	116.7 (12)
C1—N1—H13	109.8 (15)	C1—C5—H5A	124.9 (13)
H11—N1—H13	107 (2)	Cl3ⁱ—Sn1—Cl3	180.00 (3)
H12—N1—H13	109 (2)	Cl3ⁱ—Sn1—Cl2ⁱ	91.968 (19)
C5—C1—C2	120.3 (2)	Cl3—Sn1—Cl2ⁱ	88.032 (19)
C5—C1—N1	119.49 (19)	Cl3ⁱ—Sn1—Cl2	88.032 (19)
C2—C1—N1	120.1 (2)	Cl3—Sn1—Cl2	91.968 (19)
C3—C2—C1	119.0 (2)	Cl2ⁱ—Sn1—Cl2	180.00 (3)
C3—C2—H2A	123.4 (15)	Cl3ⁱ—Sn1—Cl4	90.68 (2)
C1—C2—H2A	117.7 (15)	Cl3—Sn1—Cl4	89.32 (2)
C4—C3—C2	119.7 (2)	Cl2ⁱ—Sn1—Cl4	89.46 (2)
C4—C3—H3A	119.5 (17)	Cl2—Sn1—Cl4	90.54 (2)
C2—C3—H3A	120.8 (17)	Cl3ⁱ—Sn1—Cl4ⁱ	89.32 (2)
N2—C4—C3	119.4 (2)	Cl3—Sn1—Cl4ⁱ	90.68 (2)
N2—C4—H4A	116.1 (16)	Cl2ⁱ—Sn1—Cl4ⁱ	90.54 (2)
C3—C4—H4A	124.5 (16)	Cl2—Sn1—Cl4ⁱ	89.46 (2)
C4—N2—C5	123.2 (2)	Cl4—Sn1—Cl4ⁱ	180.00 (5)
C4—N2—H2	119.7 (17)

Symmetry code: (i) −x, −y, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H11···Cl1	0.94 (2)	2.23 (3)	3.135 (2)	161 (2)
N1—H12···Cl2ⁱⁱ	0.91 (3)	2.48 (3)	3.343 (2)	160 (2)
N1—H13···Cl1ⁱⁱⁱ	0.92 (3)	2.19 (3)	3.104 (2)	176 (2)
N2—H2···Cl1^iv	0.86 (2)	2.21 (2)	3.055 (2)	167 (2)

Symmetry codes: (ii) x, −y+1/2, z+1/2; (iii) −x+1/2, y+1/2, z; (iv) −x+1, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	(C₅H₈N₂)₂[SnCl₆]Cl₂
M_r	594.56
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	290
a, b, c (Å)	11.9379 (3), 10.3704 (3), 16.7018 (5)
V (Å³)	2067.70 (10)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.27
Crystal size (mm)	0.14 × 0.12 × 0.06

Data collection
Diffractometer	Oxford Diffraction Xcalibur Eos diffractometer
Absorption correction	Multi-scan (CrysAlis PRO; Oxford Diffraction, 2009)
T_min, T_max	0.853, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	30476, 2364, 1875
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.044, 1.06
No. of reflections	2364
No. of parameters	138
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	0.26, −0.22

Computer programs: CrysAlis PRO (Oxford Diffraction, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2012), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H11···Cl1	0.94 (2)	2.23 (3)	3.135 (2)	161 (2)
N1—H12···Cl2ⁱ	0.91 (3)	2.48 (3)	3.343 (2)	160 (2)
N1—H13···Cl1ⁱⁱ	0.92 (3)	2.19 (3)	3.104 (2)	176 (2)
N2—H2···Cl1ⁱⁱⁱ	0.86 (2)	2.21 (2)	3.055 (2)	167 (2)

Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1/2, y+1/2, z; (iii) −x+1, y+1/2, −z+1/2.

Acknowledgements

We thank E. Hammes and P. Roloff for technical support. We acknowledge the support for the publication fee by the `Lehrförderfond' of the Heinrich-Heine-Universität Düsseldorf.

References

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