Propane-1,3-diammonium dichromate(VI).

The title compound, (C(3)H(12)N(2))[Cr(2)O(7)], consists of a discrete dichromate anion with an eclipsed conformation and a propane-1,3-diammonium cation. Both kinds of ions have a mirror plane passing through the bridging O atom and the central methyl-ene C atom of the Cr(2)O(7) (2-) and C(3)H(12)N(2) (2+) moieties, respectively. Anions and cations are alternately stacked to form columns parallel to the b axis. Ions are linked by intra- and inter-column hydrogen bonds of types N-H⋯O and C-H⋯O, involving O atoms of the dichromate anions as acceptors, and ammonium or methyl-ene groups as donors.

Related literature

For related structures, see: Akriche & Rzaigui (2009 ▶); Sieroń (2007 ▶); Khadhrani et al. (2006 ▶); Kallel et al. (1980 ▶); Pritchard et al. (1992 ▶). For a discussion on hydrogen bonding, see: Brown (1976 ▶); Blessing (1986 ▶). For background on CrVI species as industrial waste, see: Wani et al. (2007 ▶).

Experimental

Crystal data

(C3H12N2)[Cr2O7]

M = 292.15

Orthorhombic,

a = 8.818 (2) Å

b = 13.764 (2) Å

c = 7.918 (2) Å

V = 961.1 (4) Å3

Z = 4

Ag Kα radiation

λ = 0.56083 Å

μ = 1.18 mm−1

T = 293 K

0.30 × 0.15 × 0.10 mm

Data collection

Enraf–Nonius CAD4 diffractometer

4877 measured reflections

2430 independent reflections

1811 reflections with I > 2σ(I)

R int = 0.020

2 standard reflections every 120 min intensity decay: 3%

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.096

S = 1.10

2430 reflections

69 parameters

H-atom parameters constrained

Δρmax = 0.79 e Å−3

Δρmin = −0.61 e Å−3

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1994 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812031042/bh2445sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812031042/bh2445Isup2.hkl

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

(C3H12N2)[Cr2O7]	F(000) = 592
Mr = 292.15	Dx = 2.019 Mg m−3
Orthorhombic, Pnma	Ag Kα radiation, λ = 0.56083 Å
Hall symbol: -P 2ac 2n	Cell parameters from 25 reflections
a = 8.818 (2) Å	θ = 9–11°
b = 13.764 (2) Å	µ = 1.18 mm−1
c = 7.918 (2) Å	T = 293 K
V = 961.1 (4) Å3	Prism, orange
Z = 4	0.30 × 0.15 × 0.10 mm

Enraf–Nonius CAD4 diffractometer	Rint = 0.020
Radiation source: fine-focus sealed tube	θmax = 28.0°, θmin = 2.3°
Graphite monochromator	h = −14→3
non–profiled ω scans	k = −23→3
4877 measured reflections	l = −3→13
2430 independent reflections	2 standard reflections every 120 min
1811 reflections with I > 2σ(I)	intensity decay: 3%

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)] = 0.032	H-atom parameters constrained
wR(F2) = 0.096	w = 1/[σ2(Fo2) + (0.0502P)2 + 0.243P] where P = (Fo2 + 2Fc2)/3
S = 1.10	(Δ/σ)max = 0.001
2430 reflections	Δρmax = 0.79 e Å−3
69 parameters	Δρmin = −0.61 e Å−3
0 restraints	Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 constraints	Extinction coefficient: 0.024 (2)
Primary atom site location: structure-invariant direct methods

	x	y	z	Uiso*/Ueq
Cr	0.58026 (3)	0.131997 (16)	0.65346 (3)	0.01952 (8)
O2	0.59121 (13)	0.05330 (8)	0.80635 (15)	0.0271 (2)
O4	0.72115 (14)	0.11753 (9)	0.52532 (16)	0.0324 (3)
O3	0.42366 (14)	0.11686 (10)	0.55239 (19)	0.0388 (3)
O1	0.5853 (2)	0.2500	0.7434 (2)	0.0322 (4)
N1	0.66136 (15)	0.07105 (9)	0.16706 (17)	0.0263 (2)
H1A	0.7277	0.0716	0.0824	0.039*
H1B	0.6016	0.0192	0.1578	0.039*
H1C	0.7109	0.0687	0.2649	0.039*
C2	0.6661 (2)	0.2500	0.1633 (3)	0.0237 (3)
H2A	0.7327	0.2500	0.0658	0.028*
H2B	0.7285	0.2500	0.2642	0.028*
C1	0.56785 (16)	0.16037 (11)	0.16067 (19)	0.0231 (2)
H1D	0.4995	0.1615	0.2567	0.028*
H1E	0.5070	0.1601	0.0586	0.028*

	U11	U22	U33	U12	U13	U23
Cr	0.02104 (11)	0.01893 (11)	0.01860 (11)	−0.00012 (7)	−0.00096 (8)	0.00048 (7)
O2	0.0335 (5)	0.0232 (4)	0.0245 (4)	−0.0013 (4)	−0.0003 (4)	0.0043 (4)
O4	0.0308 (6)	0.0386 (6)	0.0277 (5)	0.0028 (4)	0.0079 (5)	0.0010 (5)
O3	0.0285 (6)	0.0481 (7)	0.0398 (7)	−0.0008 (5)	−0.0122 (5)	−0.0022 (6)
O1	0.0481 (10)	0.0202 (6)	0.0282 (7)	0.000	0.0002 (7)	0.000
N1	0.0279 (6)	0.0220 (5)	0.0289 (6)	0.0000 (5)	0.0022 (5)	0.0018 (5)
C2	0.0207 (8)	0.0216 (7)	0.0287 (9)	0.000	0.0028 (7)	0.000
C1	0.0206 (6)	0.0235 (6)	0.0252 (6)	−0.0010 (4)	−0.0002 (5)	−0.0005 (5)

Cr—O3	1.6096 (13)	N1—H1C	0.8900
Cr—O4	1.6165 (13)	C2—C1	1.5077 (19)
Cr—O2	1.6274 (12)	C2—C1i	1.5077 (19)
Cr—O1	1.7740 (8)	C2—H2A	0.9700
O1—Cri	1.7740 (8)	C2—H2B	0.9700
N1—C1	1.481 (2)	C1—H1D	0.9700
N1—H1A	0.8900	C1—H1E	0.9700
N1—H1B	0.8900
O3—Cr—O4	109.35 (8)	C1—C2—C1i	109.83 (17)
O3—Cr—O2	109.55 (7)	C1—C2—H2A	109.7
O4—Cr—O2	109.84 (6)	C1i—C2—H2A	109.7
O3—Cr—O1	109.85 (8)	C1—C2—H2B	109.7
O4—Cr—O1	110.21 (8)	C1i—C2—H2B	109.7
O2—Cr—O1	108.02 (7)	H2A—C2—H2B	108.2
Cr—O1—Cri	132.57 (11)	N1—C1—C2	111.03 (13)
C1—N1—H1A	109.5	N1—C1—H1D	109.4
C1—N1—H1B	109.5	C2—C1—H1D	109.4
H1A—N1—H1B	109.5	N1—C1—H1E	109.4
C1—N1—H1C	109.5	C2—C1—H1E	109.4
H1A—N1—H1C	109.5	H1D—C1—H1E	108.0
H1B—N1—H1C	109.5

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O2ii	0.89	2.51	2.9326 (19)	110
N1—H1A···O3iii	0.89	2.12	2.9609 (19)	156
N1—H1B···O2iv	0.89	1.99	2.8168 (19)	154
N1—H1C···O4	0.89	2.17	2.955 (2)	147
N1—H1C···O2v	0.89	2.44	2.9844 (19)	120
C1—H1D···O3	0.97	2.51	3.405 (2)	153
C1—H1E···O2ii	0.97	2.59	3.176 (2)	119

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O3i	0.89	2.12	2.9609 (19)	156
N1—H1B⋯O2ii	0.89	1.99	2.8168 (19)	154
N1—H1C⋯O4	0.89	2.17	2.955 (2)	147
N1—H1C⋯O2iii	0.89	2.44	2.9844 (19)	120
C1—H1D⋯O3	0.97	2.51	3.405 (2)	153
C1—H1E⋯O2iv	0.97	2.59	3.176 (2)	119

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