catena-Poly[bis(dimethylazanium) [[chloridocopper(II)]-di-μ-chlorido-[chloridocopper(II)]-di-μ-azido-κN:N]].

The crystal structure of the title complex, {(C(2)H(8)N)[CuCl(2)(N(3))]}(n), exhibits inorganic chains consisting of Cu(II) cations as well azide and chloride anions. The chains, made up from Cu-Cl-Cu-N-Cu linkages, are aligned parallel to the c axis. This architecture is further stabilized by a number of N-H⋯Cl hydrogen bonds involving the protonated charge-compensating dimethyl-amine cations and chloride atoms.

Related literature

For background to polynuclear complexes, see Goher et al. (2000 ▶); Liu et al. (2008 ▶); Ribas et al. (1994 ▶); Saha et al. (2005 ▶); Vicente et al. (1993 ▶); Wang et al. (2008 ▶). For di- or polyalkyl­amines as templates, see: Cheetham et al. (1999 ▶); Hagrman et al. (1999 ▶). For related copper(II) complexes, see: Mautner et al. (1999 ▶).

Experimental

Crystal data

(C2H8N)[CuCl2(N3)]

M = 222.57

Monoclinic,

a = 15.348 (5) Å

b = 11.089 (2) Å

c = 10.729 (2) Å

β = 119.73 (2)°

V = 1585.7 (7) Å3

Z = 8

Mo Kα radiation

μ = 3.35 mm−1

T = 298 K

0.14 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ▶) T min = 0.651, T max = 0.775

3510 measured reflections

1811 independent reflections

1251 reflections with I > 2σ(I)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.027

wR(F 2) = 0.066

S = 0.94

1811 reflections

85 parameters

13 restraints

H-atom parameters constrained

Δρmax = 0.41 e Å−3

Δρmin = −0.38 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811050537/zb2020sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811050537/zb2020Isup2.hkl

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

(C2H8N)[CuCl2(N3)]	F(000) = 888
Mr = 222.57	Dx = 1.865 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.348 (5) Å	Cell parameters from 1037 reflections
b = 11.089 (2) Å	θ = 2.6–24.6°
c = 10.729 (2) Å	µ = 3.35 mm−1
β = 119.73 (2)°	T = 298 K
V = 1585.7 (7) Å3	Block, green
Z = 8	0.14 × 0.10 × 0.08 mm

Bruker APEXII CCD diffractometer	1811 independent reflections
Radiation source: fine-focus sealed tube	1251 reflections with I > 2σ(I)
graphite	Rint = 0.025
phi and ω scans	θmax = 27.5°, θmin = 3.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −19→19
Tmin = 0.651, Tmax = 0.775	k = −14→14
3510 measured reflections	l = −13→13

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)] = 0.027	H-atom parameters constrained
wR(F2) = 0.066	w = 1/[σ2(Fo2) + (0.0361P)2] where P = (Fo2 + 2Fc2)/3
S = 0.94	(Δ/σ)max = 0.012
1811 reflections	Δρmax = 0.41 e Å−3
85 parameters	Δρmin = −0.38 e Å−3
13 restraints	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0036 (3)

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.

	x	y	z	Uiso*/Ueq
Cu1	−0.03408 (2)	0.39407 (3)	0.06367 (3)	0.03133 (14)
Cl1	−0.14064 (5)	0.39423 (5)	0.15347 (8)	0.03677 (18)
Cl2	−0.03672 (5)	0.19228 (5)	0.03779 (7)	0.0404 (2)
N1	−0.04383 (19)	0.57303 (19)	0.0352 (3)	0.0409 (6)
N2	−0.08322 (18)	0.64469 (19)	0.0760 (3)	0.0388 (6)
N3	−0.1205 (2)	0.7121 (2)	0.1134 (3)	0.0659 (9)
N4	−0.1737 (2)	0.1071 (2)	0.1860 (3)	0.0492 (6)
H1	−0.2164	0.1291	0.0834	0.059*
H2	−0.1180	0.1479	0.2287	0.059*
C1	−0.1482 (3)	−0.0211 (3)	0.1877 (4)	0.0631 (9)
H1A	−0.1133	−0.0496	0.2850	0.095*
H1B	−0.1062	−0.0303	0.1455	0.095*
H1C	−0.2087	−0.0669	0.1337	0.095*
C2	−0.2303 (3)	0.1339 (3)	0.2608 (4)	0.0579 (8)
H2A	−0.2921	0.0894	0.2167	0.087*
H2B	−0.2446	0.2186	0.2544	0.087*
H2C	−0.1911	0.1110	0.3598	0.087*

	U11	U22	U33	U12	U13	U23
Cu1	0.0392 (2)	0.02505 (19)	0.0368 (2)	0.00100 (14)	0.02419 (17)	0.00218 (13)
Cl1	0.0405 (4)	0.0355 (4)	0.0434 (4)	0.0016 (3)	0.0277 (3)	0.0042 (3)
Cl2	0.0520 (5)	0.0270 (3)	0.0459 (5)	−0.0020 (3)	0.0271 (4)	−0.0012 (3)
N1	0.0609 (17)	0.0280 (11)	0.0535 (16)	0.0035 (10)	0.0433 (14)	0.0048 (10)
N2	0.0495 (15)	0.0285 (12)	0.0501 (16)	0.0050 (10)	0.0336 (13)	0.0062 (10)
N3	0.087 (2)	0.0483 (17)	0.092 (2)	0.0157 (15)	0.067 (2)	0.0034 (14)
N4	0.0569 (14)	0.0425 (11)	0.0524 (14)	−0.0084 (10)	0.0303 (11)	−0.0003 (9)
C1	0.0676 (17)	0.0421 (14)	0.0641 (17)	−0.0036 (14)	0.0208 (15)	0.0025 (13)
C2	0.0592 (17)	0.0641 (15)	0.0575 (17)	−0.0108 (14)	0.0342 (14)	0.0001 (13)

Cu1—N1i	1.987 (2)	N4—C1	1.471 (4)
Cu1—N1	2.002 (2)	N4—C2	1.477 (4)
Cu1—Cl2	2.2527 (8)	N4—H1	0.9931
Cu1—Cl1	2.2729 (9)	N4—H2	0.8693
Cu1—Cl1ii	2.8860 (13)	C1—H1A	0.9600
Cu1—Cu1i	3.1460 (7)	C1—H1B	0.9600
Cl1—Cu1ii	2.8860 (13)	C1—H1C	0.9600
N1—N2	1.205 (3)	C2—H2A	0.9600
N1—Cu1i	1.987 (2)	C2—H2B	0.9600
N2—N3	1.129 (3)	C2—H2C	0.9600
N1i—Cu1—N1	75.87 (10)	N3—N2—N1	179.6 (3)
N1i—Cu1—Cl2	95.48 (7)	C1—N4—C2	114.3 (2)
N1—Cu1—Cl2	166.02 (7)	C1—N4—H1	106.0
N1i—Cu1—Cl1	167.54 (7)	C2—N4—H1	108.0
N1—Cu1—Cl1	92.79 (7)	C1—N4—H2	108.1
Cl2—Cu1—Cl1	94.60 (3)	C2—N4—H2	107.4
N1i—Cu1—Cl1ii	94.01 (8)	H1—N4—H2	113.1
N1—Cu1—Cl1ii	96.89 (7)	N4—C1—H1A	109.5
Cl2—Cu1—Cl1ii	94.63 (2)	N4—C1—H1B	109.5
Cl1—Cu1—Cl1ii	92.46 (3)	H1A—C1—H1B	109.5
N1i—Cu1—Cu1i	38.11 (6)	N4—C1—H1C	109.5
N1—Cu1—Cu1i	37.76 (7)	H1A—C1—H1C	109.5
Cl2—Cu1—Cu1i	132.67 (3)	H1B—C1—H1C	109.5
Cl1—Cu1—Cu1i	130.36 (2)	N4—C2—H2A	109.5
Cl1ii—Cu1—Cu1i	96.92 (2)	N4—C2—H2B	109.5
Cu1—Cl1—Cu1ii	87.54 (3)	H2A—C2—H2B	109.5
N2—N1—Cu1i	128.05 (19)	N4—C2—H2C	109.5
N2—N1—Cu1	127.70 (19)	H2A—C2—H2C	109.5
Cu1i—N1—Cu1	104.13 (10)	H2B—C2—H2C	109.5

D—H···A	D—H	H···A	D···A	D—H···A
N4—H1···Cl1iii	0.99	2.41	3.331 (3)	154.
N4—H2···Cl2ii	0.87	2.50	3.257 (3)	146.
N4—H2···Cl1	0.87	2.82	3.270 (2)	114.
N4—H2···Cl2	0.87	2.92	3.340 (3)	112.

Table 1

Selected bond lengths (Å)

Cu1—N1i	1.987 (2)
Cu1—N1	2.002 (2)
Cu1—Cl2	2.2527 (8)
Cu1—Cl1	2.2729 (9)
Cu1—Cl1ii	2.8860 (13)
Cu1—Cu1i	3.1460 (7)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N4—H1⋯Cl1iii	0.99	2.41	3.331 (3)	154
N4—H2⋯Cl2ii	0.87	2.50	3.257 (3)	146
N4—H2⋯Cl1	0.87	2.82	3.270 (2)	114
N4—H2⋯Cl2	0.87	2.92	3.340 (3)	112

Symmetry codes: (ii) ; (iii) .