Bis(1,4-diazo-niabi-cyclo-[2.2.2]octa-ne) di-μ-chlorido-bis-[tetra-chlorido-anti-monate(III)] dihydrate.

The title salt, (C6H14N2)2[Sb2Cl10]·2H2O, was obtained by slow evaporation of an acidic solution of 1,4-di-aza-bicyclo-[2.2.2]octane and SbCl3. The crystal structure consists of (C6H14N2)(2+) cations, [Sb2Cl10](4-) double octa-hedra and lattice water mol-ecules. All mol-ecular components are situated on special positions. The cation and the lattice water mol-ecule exhibit mirror symmetry, whereas the anion has site symmetry 2/m. The cations, anions and water mol-ecules are alternately arranged into columns along [010]. Individual columns are joined into layers extending along (001). Intra-layer N-H⋯O and inter-layer N-H⋯Cl hydrogen-bonding inter-actions lead to the formation of a three-dimensional network.

Related literature

For background to this class of compounds, see: Pietraszko et al. (2001 ▶); Feng et al. (2007 ▶); Bujak & Zaleski (1999 ▶); Knodler et al. (1988 ▶); Baker & Williams (1978 ▶). For a related structure, see: Qu & Sun (2005 ▶).

Experimental

Crystal data

(C6H14N2)2[Sb2Cl10]·2H2O

M = 862.46

Orthorhombic,

a = 9.162 (1) Å

b = 20.869 (7) Å

c = 7.566 (2) Å

V = 1446.8 (7) Å3

Z = 2

Mo Kα radiation

μ = 2.81 mm−1

T = 298 K

0.50 × 0.43 × 0.36 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.334, T max = 0.431

2797 measured reflections

1700 independent reflections

1488 reflections with I > 2σ(I)

R int = 0.029

2 standard reflections every 120 min intensity decay: 1%

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.061

S = 1.08

1700 reflections

82 parameters

H-atom parameters constrained

Δρmax = 0.59 e Å−3

Δρmin = −0.37 e Å−3

Data collection: CAD-4 EXPRESS (Duisenberg, 1992 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681301307X/wm2740sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681301307X/wm2740Isup2.hkl

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

(C6H14N2)2[Sb2Cl10]·2H2O	Dx = 1.980 Mg m−3
Mr = 862.46	Melting point: 571 K
Orthorhombic, Pnnm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2 2n	Cell parameters from 1700 reflections
a = 9.162 (1) Å	θ = 2.4–27.0°
b = 20.869 (7) Å	µ = 2.81 mm−1
c = 7.566 (2) Å	T = 298 K
V = 1446.8 (7) Å3	Prism, colourless
Z = 2	0.50 × 0.43 × 0.36 mm
F(000) = 840

Enraf–Nonius CAD-4 diffractometer	1488 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 27.0°, θmin = 2.4°
non–profiled ω/2θ scans	h = −1→11
Absorption correction: ψ scan (North et al., 1968)	k = −26→1
Tmin = 0.334, Tmax = 0.431	l = −9→3
2797 measured reflections	2 standard reflections every 120 min
1700 independent reflections	intensity decay: 1%

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)] = 0.023	H-atom parameters constrained
wR(F2) = 0.061	w = 1/[σ2(Fo2) + (0.0268P)2 + 1.1425P] where P = (Fo2 + 2Fc2)/3
S = 1.08	(Δ/σ)max = 0.001
1700 reflections	Δρmax = 0.59 e Å−3
82 parameters	Δρmin = −0.37 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0099 (5)

Experimental. Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied.

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	Occ. (<1)
Sb	0.40193 (3)	0.407356 (11)	0.5000	0.03327 (11)
Cl1	0.16885 (14)	0.46510 (7)	0.5000	0.0678 (4)
Cl2	0.62462 (11)	0.31027 (6)	0.5000	0.0471 (3)
Cl3	0.30372 (8)	0.33776 (3)	0.26053 (10)	0.04669 (19)
Cl4	0.5000	0.5000	0.23812 (14)	0.0534 (3)
N1	0.3554 (4)	0.20234 (16)	0.5000	0.0406 (8)
H1	0.3861	0.2438	0.5000	0.049*
N2	0.2710 (4)	0.09024 (15)	0.5000	0.0443 (8)
H2	0.2394	0.0489	0.5000	0.053*
C1	0.1931 (4)	0.20125 (18)	0.5000	0.0433 (9)
H1A	0.1563	0.2231	0.3961	0.052*	0.50
H1B	0.1563	0.2231	0.6039	0.052*	0.50
C2	0.1428 (5)	0.1332 (2)	0.5000	0.0537 (12)
H2A	0.0836	0.1251	0.6039	0.064*	0.50
H2B	0.0836	0.1251	0.3961	0.064*	0.50
C3	0.4100 (3)	0.17034 (16)	0.6617 (5)	0.0535 (8)
H3A	0.3730	0.1921	0.7657	0.064*
H3B	0.5158	0.1720	0.6646	0.064*
C4	0.3595 (4)	0.10141 (15)	0.6615 (5)	0.0541 (8)
H4A	0.4432	0.0729	0.6626	0.065*
H4B	0.3013	0.0929	0.7660	0.065*
O	0.3071 (4)	−0.04203 (13)	0.5000	0.0522 (8)

	U11	U22	U33	U12	U13	U23
Sb	0.03290 (16)	0.02973 (15)	0.03718 (16)	−0.00263 (10)	0.000	0.000
Cl1	0.0468 (6)	0.0716 (8)	0.0850 (9)	0.0239 (6)	0.000	0.000
Cl2	0.0379 (5)	0.0543 (6)	0.0492 (6)	0.0080 (4)	0.000	0.000
Cl3	0.0517 (4)	0.0401 (4)	0.0483 (4)	−0.0104 (3)	−0.0131 (3)	0.0003 (3)
Cl4	0.0639 (7)	0.0548 (6)	0.0414 (5)	0.0027 (5)	0.000	0.000
N1	0.0392 (17)	0.0292 (15)	0.053 (2)	−0.0064 (13)	0.000	0.000
N2	0.050 (2)	0.0268 (15)	0.056 (2)	0.0011 (14)	0.000	0.000
C1	0.036 (2)	0.0315 (18)	0.062 (3)	0.0061 (16)	0.000	0.000
C2	0.0314 (19)	0.039 (2)	0.091 (4)	−0.0053 (18)	0.000	0.000
C3	0.0447 (16)	0.0601 (19)	0.0557 (19)	−0.0037 (14)	−0.0143 (15)	−0.0024 (16)
C4	0.0640 (19)	0.0475 (16)	0.0508 (18)	0.0084 (14)	−0.0059 (17)	0.0100 (15)
O	0.0487 (17)	0.0359 (15)	0.072 (2)	−0.0019 (13)	0.000	0.000

Sb—Cl1	2.4520 (12)	N2—H2	0.9100
Sb—Cl3i	2.4904 (7)	C1—C2	1.492 (6)
Sb—Cl3	2.4904 (7)	C1—H1A	0.9700
Sb—Cl2	2.8755 (11)	C1—H1B	0.9700
Sb—Cl4	2.9107 (8)	C2—H2A	0.9700
N1—C3	1.481 (4)	C2—H2B	0.9700
N1—C3i	1.481 (4)	C3—C4	1.511 (4)
N1—C1	1.487 (5)	C3—H3A	0.9700
N1—H1	0.9100	C3—H3B	0.9700
N2—C2	1.478 (5)	C4—H4A	0.9700
N2—C4i	1.485 (4)	C4—H4B	0.9700
N2—C4	1.485 (4)
Cl1—Sb—Cl3i	88.39 (3)	N1—C1—H1A	109.9
Cl1—Sb—Cl3	88.39 (3)	C2—C1—H1A	109.9
Cl3i—Sb—Cl3	93.37 (3)	N1—C1—H1B	109.9
Cl1—Sb—Cl2	164.64 (4)	C2—C1—H1B	109.9
Cl3i—Sb—Cl2	81.11 (2)	H1A—C1—H1B	108.3
Cl3—Sb—Cl2	81.11 (2)	N2—C2—C1	109.4 (3)
Cl4—Sb—Cl3	90.19 (1)	N2—C2—H2A	109.8
Cl4—Sb—Cl3i	173.84 (1)	C1—C2—H2A	109.8
Cl4—Sb—Cl1	86.69 (4)	N2—C2—H2B	109.8
Cl4—Sb—Cl2	104.42 (1)	C1—C2—H2B	109.8
C3—N1—C3i	111.4 (3)	H2A—C2—H2B	108.2
C3—N1—C1	109.3 (2)	N1—C3—C4	109.0 (3)
C3i—N1—C1	109.3 (2)	N1—C3—H3A	109.9
C3—N1—H1	108.9	C4—C3—H3A	109.9
C3i—N1—H1	108.9	N1—C3—H3B	109.9
C1—N1—H1	108.9	C4—C3—H3B	109.9
C2—N2—C4i	109.8 (2)	H3A—C3—H3B	108.3
C2—N2—C4	109.8 (2)	N2—C4—C3	108.5 (3)
C4i—N2—C4	110.8 (4)	N2—C4—H4A	110.0
C2—N2—H2	108.8	C3—C4—H4A	110.0
C4i—N2—H2	108.8	N2—C4—H4B	110.0
C4—N2—H2	108.8	C3—C4—H4B	110.0
N1—C1—C2	108.9 (3)	H4A—C4—H4B	108.4

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Cl2	0.91	2.59	3.340 (4)	140
N1—H1···Cl3	0.91	2.77	3.390 (3)	126
N1—H1···Cl3i	0.91	2.77	3.390 (3)	126
N2—H2···O	0.91	2.00	2.780 (4)	143

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯Cl2	0.91	2.59	3.340 (4)	140
N1—H1⋯Cl3	0.91	2.77	3.390 (3)	126
N1—H1⋯Cl3i	0.91	2.77	3.390 (3)	126
N2—H2⋯O	0.91	2.00	2.780 (4)	143

Symmetry code: (i) .