Bis[trans-dichloridobis(propane-1,3-diamine-κ(2)N,N')chromium(III)] tetra-chloridozincate determined using synchrotron radiation.

In the title compound, [CrCl(2)(C(3)H(10)N(2))(2)](2)[ZnCl(4)], the Cr(III) atom is coordinated by four N atoms of propane-1,3-diamine (tn) and two Cl atoms in a trans arrangement, displaying a distorted octa-hedral geometry with crystallographic inversion symmetry; the Zn atom in the [ZnCl(4)](2-) anion lies on a -4 axis. The orientations of the two six-membered chelate rings in the complex cation are in an anti chair-chair conformation with respect to each other. The Cr-N bond lengths are 2.087 (6) and 2.097 (6) Å. The Cr-Cl and Zn-Cl bond lengths are 2.3151 (16) and 2.3255 (13) Å, respectively. Weak inter-molecular hydrogen bonds involving the tn NH(2) groups as donors and chloride ligands of the anion and cation as acceptors are observed.

Related literature

For the synthesis, see: House (1970 ▶). For the structures of trans-[Cr(tn)2 L 2]ClO4 (L = F, Cl, Br), see: Vaughn & Rogers (1985 ▶); Choi & Clegg (2011 ▶); Choi et al. (2012 ▶). For the structures of trans-[Cr(Me2tn)2Cl2]ClO4 and trans-[Cr(Me2tn)2Cl2]2ZnCl4, see: Choi et al. (2008 ▶, 2011 ▶).

Experimental

Crystal data

[CrCl2(C3H10N2)2]2[ZnCl4]

M = 749.49

Tetragonal,

a = 15.141 (2) Å

c = 6.4220 (13) Å

V = 1472.2 (4) Å3

Z = 2

Synchrotron radiation, λ = 0.90000 Å

μ = 4.26 mm−1

T = 95 K

0.16 × 0.02 × 0.02 mm

Data collection

ADSC Q210 CCD area-detector diffractometer

Absorption correction: multi-scan (HKL-3000 SCALEPACK; Otwinowski & Minor, 1997 ▶) T min = 0.549, T max = 0.920

7735 measured reflections

1225 independent reflections

1157 reflections with I > 2σ(I)

R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.066

wR(F 2) = 0.198

S = 1.11

1225 reflections

73 parameters

H-atom parameters constrained

Δρmax = 2.55 e Å−3

Δρmin = −1.30 e Å−3

Data collection: PAL ADSC Quantum-210 ADX Program (Arvai & Nielsen, 1983 ▶); cell refinement: HKL-3000 (Otwinowski & Minor, 1997 ▶); data reduction: HKL-3000; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOn class="Chemical">ND (Brandenburg, 2012 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812023355/nk2158sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812023355/nk2158Isup2.hkl

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

[CrCl2(C3H10N2)2]2[ZnCl4]	Dx = 1.691 Mg m−3
Mr = 749.49	Synchrotron radiation, λ = 0.90000 Å
Tetragonal, P42/n	Cell parameters from 16475 reflections
a = 15.141 (2) Å	θ = 1.0–33.7°
c = 6.4220 (13) Å	µ = 4.26 mm−1
V = 1472.2 (4) Å3	T = 95 K
Z = 2	Needle, pale blue
F(000) = 764	0.16 × 0.02 × 0.02 mm

ADSC Q210 CCD area-detector diffractometer	1225 independent reflections
Radiation source: PLSII 2D bending magnet	1157 reflections with I > 2σ(I)
Si(111) double crystal monochromator	Rint = 0.030
ω and kappa scan	θmax = 32.0°, θmin = 2.4°
Absorption correction: multi-scan (HKL-3000SCALEPACK; Otwinowski & Minor, 1997)	h = −17→17
Tmin = 0.549, Tmax = 0.920	k = −17→17
7735 measured reflections	l = −7→7

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)] = 0.066	H-atom parameters constrained
wR(F2) = 0.198	w = 1/[σ2(Fo2) + (0.1185P)2 + 13.7893P] where P = (Fo2 + 2Fc2)/3
S = 1.11	(Δ/σ)max < 0.001
1225 reflections	Δρmax = 2.55 e Å−3
73 parameters	Δρmin = −1.30 e Å−3
0 restraints	Extinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.010 (2)

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
Cr1	0.5000	0.5000	0.5000	0.0176 (6)
Cl1	0.42602 (11)	0.55586 (11)	0.7867 (2)	0.0219 (6)
N1	0.4440 (4)	0.3768 (4)	0.5622 (10)	0.0250 (14)
H1A	0.4141	0.3811	0.6865	0.030*
H1B	0.4027	0.3657	0.4605	0.030*
N2	0.6077 (4)	0.4700 (4)	0.6928 (9)	0.0214 (13)
H2A	0.6528	0.5081	0.6592	0.026*
H2B	0.5914	0.4822	0.8277	0.026*
C1	0.5033 (5)	0.2982 (5)	0.5752 (11)	0.0249 (16)
H1C	0.5309	0.2880	0.4375	0.030*
H1D	0.4676	0.2454	0.6100	0.030*
C2	0.5748 (5)	0.3093 (5)	0.7361 (11)	0.0244 (16)
H2C	0.6049	0.2518	0.7544	0.029*
H2D	0.5465	0.3245	0.8705	0.029*
C3	0.6441 (5)	0.3786 (5)	0.6887 (11)	0.0240 (15)
H3A	0.6923	0.3740	0.7922	0.029*
H3B	0.6696	0.3669	0.5494	0.029*
Zn1	0.2500	0.2500	0.2500	0.0223 (6)
Cl2	0.37601 (8)	0.28336 (9)	0.0585 (2)	0.0115 (5)

	U11	U22	U33	U12	U13	U23
Cr1	0.0199 (9)	0.0192 (9)	0.0138 (9)	−0.0007 (5)	−0.0008 (6)	−0.0002 (6)
Cl1	0.0230 (9)	0.0287 (10)	0.0141 (9)	0.0025 (6)	0.0014 (6)	−0.0007 (6)
N1	0.026 (3)	0.024 (3)	0.025 (3)	0.000 (2)	−0.001 (3)	0.002 (3)
N2	0.024 (3)	0.024 (3)	0.016 (3)	−0.002 (2)	0.000 (2)	−0.001 (2)
C1	0.031 (4)	0.020 (3)	0.023 (4)	0.001 (3)	−0.002 (3)	−0.002 (3)
C2	0.027 (4)	0.021 (3)	0.025 (4)	−0.001 (3)	−0.002 (3)	0.004 (3)
C3	0.021 (3)	0.029 (4)	0.022 (3)	0.002 (3)	−0.002 (3)	0.003 (3)
Zn1	0.0223 (7)	0.0223 (7)	0.0222 (9)	0.000	0.000	0.000
Cl2	0.0087 (8)	0.0138 (8)	0.0119 (8)	−0.0024 (5)	0.0055 (5)	−0.0009 (5)

Cr1—N1	2.087 (6)	C1—C2	1.505 (10)
Cr1—N1i	2.087 (6)	C1—H1C	0.9900
Cr1—N2	2.097 (6)	C1—H1D	0.9900
Cr1—N2i	2.097 (6)	C2—C3	1.515 (10)
Cr1—Cl1i	2.3151 (16)	C2—H2C	0.9900
Cr1—Cl1	2.3151 (16)	C2—H2D	0.9900
N1—C1	1.494 (9)	C3—H3A	0.9900
N1—H1A	0.9200	C3—H3B	0.9900
N1—H1B	0.9200	Zn1—Cl2ii	2.3255 (13)
N2—C3	1.489 (9)	Zn1—Cl2iii	2.3255 (13)
N2—H2A	0.9200	Zn1—Cl2iv	2.3255 (13)
N2—H2B	0.9200	Zn1—Cl2	2.3255 (13)
N1—Cr1—N1i	179.999 (1)	H2A—N2—H2B	107.1
N1—Cr1—N2	90.5 (2)	N1—C1—C2	112.4 (6)
N1i—Cr1—N2	89.5 (2)	N1—C1—H1C	109.1
N1—Cr1—N2i	89.5 (2)	C2—C1—H1C	109.1
N1i—Cr1—N2i	90.5 (2)	N1—C1—H1D	109.1
N2—Cr1—N2i	179.999 (1)	C2—C1—H1D	109.1
N1—Cr1—Cl1i	91.27 (18)	H1C—C1—H1D	107.9
N1i—Cr1—Cl1i	88.73 (18)	C1—C2—C3	115.9 (6)
N2—Cr1—Cl1i	90.80 (16)	C1—C2—H2C	108.3
N2i—Cr1—Cl1i	89.20 (16)	C3—C2—H2C	108.3
N1—Cr1—Cl1	88.73 (18)	C1—C2—H2D	108.3
N1i—Cr1—Cl1	91.27 (18)	C3—C2—H2D	108.3
N2—Cr1—Cl1	89.20 (16)	H2C—C2—H2D	107.4
N2i—Cr1—Cl1	90.80 (16)	N2—C3—C2	112.5 (6)
Cl1i—Cr1—Cl1	180.0	N2—C3—H3A	109.1
C1—N1—Cr1	118.6 (4)	C2—C3—H3A	109.1
C1—N1—H1A	107.7	N2—C3—H3B	109.1
Cr1—N1—H1A	107.7	C2—C3—H3B	109.1
C1—N1—H1B	107.7	H3A—C3—H3B	107.8
Cr1—N1—H1B	107.7	Cl2ii—Zn1—Cl2iii	106.24 (3)
H1A—N1—H1B	107.1	Cl2ii—Zn1—Cl2iv	106.25 (3)
C3—N2—Cr1	118.6 (4)	Cl2iii—Zn1—Cl2iv	116.14 (7)
C3—N2—H2A	107.7	Cl2ii—Zn1—Cl2	116.14 (7)
Cr1—N2—H2A	107.7	Cl2iii—Zn1—Cl2	106.24 (3)
C3—N2—H2B	107.7	Cl2iv—Zn1—Cl2	106.25 (3)
Cr1—N2—H2B	107.7

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1B···Cl2	0.92	2.90	3.678 (6)	144
N1—H1A···Cl2v	0.92	2.87	3.636 (6)	142
N1—H1B···Cl2iv	0.92	2.82	3.529 (6)	134
N2—H2A···Cl2vi	0.92	2.72	3.641 (6)	179
N2—H2B···Cl1vii	0.92	2.56	3.404 (6)	154

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1B⋯Cl2	0.92	2.90	3.678 (6)	144
N1—H1A⋯Cl2i	0.92	2.87	3.636 (6)	142
N1—H1B⋯Cl2ii	0.92	2.82	3.529 (6)	134
N2—H2A⋯Cl2iii	0.92	2.72	3.641 (6)	179
N2—H2B⋯Cl1iv	0.92	2.56	3.404 (6)	154

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