4-(3-Ammonio-prop-yl)morpholin-4-ium tetra-chloridozincate(II).

In the title compound, (C(7)H(18)N(2)O)[ZnCl(4)], the Zn(II) ion is coordinated by four Cl atoms in a close to tetra-hedral geometry. The crystal packing exhibits C-H⋯Cl, N-H⋯Cl and N-H⋯O hydrogen bonds.

Related literature

For common applications of this material, see: Bringley & Rajeswaran (2006 ▶); Tao et al. (2003 ▶). For structure cohesion, see: Brammer et al. (2002 ▶). For a discussion of Zn—Cl distances and Cl—Zn—Cl bond angles, see: Guo et al. (2007 ▶); Valkonen et al. (2006 ▶). For computational details, see: Prince (1982 ▶); Watkin (1994 ▶).

Experimental

Crystal data

(C7H18N2O)[ZnCl4]

M = 353.42

Monoclinic,

a = 6.2765 (2) Å

b = 14.3552 (4) Å

c = 15.4858 (6) Å

β = 100.759 (4)°

V = 1370.75 (8) Å3

Z = 4

Mo Kα radiation

μ = 2.55 mm−1

T = 293 K

0.17 × 0.09 × 0.08 mm

Data collection

Oxford Diffraction Xcalibur area-detector diffractometer

Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2002 ▶) T min = 0.63, T max = 0.82

13120 measured reflections

3304 independent reflections

2815 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.019

wR(F 2) = 0.020

S = 1.04

2696 reflections

137 parameters

H-atom parameters constrained

Δρmax = 0.27 e Å−3

Δρmin = −0.19 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2002 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2002 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003 ▶); molecular graphics: CAMERON (Watkin et al., 1996 ▶); software used to prepare material for publication: CRYSTALS.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809004346/lx2089sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809004346/lx2089Isup2.hkl

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

(C7H18N2O)[ZnCl4]	F(000) = 720
Mr = 353.42	Dx = 1.712 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybc	Cell parameters from 7336 reflections
a = 6.2765 (2) Å	θ = 2.8–29.2°
b = 14.3552 (4) Å	µ = 2.55 mm−1
c = 15.4858 (6) Å	T = 293 K
β = 100.759 (4)°	Block, colorless
V = 1370.75 (8) Å3	0.17 × 0.09 × 0.08 mm
Z = 4

Oxford Diffraction XCALIBUR area-detector diffractometer	3304 independent reflections
Radiation source: Enhance (Mo) X-ray Source	2815 reflections with I > 2σ(I)
graphite	Rint = 0.021
Detector resolution: 15.9897 pixels mm-1	θmax = 29.3°, θmin = 2.8°
φ and ω scans	h = −8→8
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2002)	k = −18→18
Tmin = 0.63, Tmax = 0.82	l = −18→20
13120 measured reflections

Refinement on F	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.019	Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A0*T0(x) + A1*T1(x) ··· + An-1]*Tn-1(x)] where Ai are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)2]2 Ai are: 8.69 -6.08 5.75
wR(F2) = 0.020	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 0.27 e Å−3
2696 reflections	Δρmin = −0.19 e Å−3
137 parameters	Extinction correction: Larson (1970), Equation 22
0 restraints	Extinction coefficient: 64 (4)
Primary atom site location: structure-invariant direct methods

Refinement. Data with I<3σ(I) were excluded from the refinement.

	x	y	z	Uiso*/Ueq
Zn1	0.37044 (3)	0.371470 (11)	0.756164 (11)	0.0273
Cl1	0.48665 (7)	0.47971 (3)	0.85946 (3)	0.0402
Cl2	0.00747 (6)	0.35230 (3)	0.74949 (3)	0.0367
Cl3	0.51658 (6)	0.22854 (2)	0.79921 (3)	0.0372
Cl4	0.43433 (6)	0.42069 (3)	0.62551 (2)	0.0402
C1	0.2040 (3)	0.73398 (12)	0.47182 (11)	0.0383
C2	0.2358 (3)	0.83554 (14)	0.45739 (12)	0.0468
C3	−0.0795 (3)	0.87396 (11)	0.50847 (11)	0.0441
C4	−0.1308 (2)	0.77313 (10)	0.52356 (10)	0.0319
C5	0.0385 (3)	0.61461 (10)	0.54896 (10)	0.0319
C6	−0.1030 (2)	0.58498 (10)	0.61278 (9)	0.0310
C7	−0.0059 (2)	0.60272 (10)	0.70780 (9)	0.0284
O	0.0323 (2)	0.88265 (8)	0.43720 (8)	0.0456
N1	0.07386 (18)	0.71776 (8)	0.54268 (7)	0.0256
N2	−0.1501 (2)	0.56344 (9)	0.76395 (8)	0.0355
H1	0.1513	0.7371	0.5924	0.0370*
H2	−0.0977	0.5758	0.8191	0.0530*
H3	−0.1610	0.5037	0.7569	0.0543*
H4	−0.2786	0.5881	0.7508	0.0540*
H5	0.3391	0.7034	0.4902	0.0478*
H6	0.1254	0.7059	0.4190	0.0461*
H7	0.3247	0.8625	0.5090	0.0563*
H8	0.3080	0.8410	0.4080	0.0566*
H9	0.0095	0.9001	0.5612	0.0534*
H10	−0.2154	0.9071	0.4938	0.0536*
H11	−0.2037	0.7673	0.5727	0.0386*
H12	−0.2185	0.7468	0.4714	0.0373*
H13	0.1820	0.5879	0.5638	0.0378*
H14	−0.0305	0.5963	0.4896	0.0376*
H15	−0.1224	0.5188	0.6059	0.0375*
H16	−0.2428	0.6161	0.5982	0.0365*
H17	0.1334	0.5740	0.7240	0.0348*
H18	0.0068	0.6679	0.7193	0.0354*

	U11	U22	U33	U12	U13	U23
Zn1	0.02689 (9)	0.02429 (9)	0.02946 (9)	−0.00028 (6)	0.00203 (6)	0.00055 (6)
Cl1	0.0496 (2)	0.03524 (19)	0.03582 (19)	−0.00756 (15)	0.00812 (16)	−0.00963 (14)
Cl2	0.02569 (16)	0.03157 (17)	0.0513 (2)	−0.00010 (12)	0.00342 (14)	0.00177 (15)
Cl3	0.02699 (16)	0.02632 (16)	0.0545 (2)	0.00182 (12)	−0.00201 (15)	0.00397 (15)
Cl4	0.0402 (2)	0.0493 (2)	0.03073 (18)	−0.00006 (16)	0.00604 (15)	0.00497 (15)
C1	0.0350 (8)	0.0496 (9)	0.0336 (8)	0.0016 (7)	0.0147 (6)	0.0046 (7)
C2	0.0456 (9)	0.0538 (10)	0.0415 (9)	−0.0109 (8)	0.0096 (7)	0.0126 (8)
C3	0.0648 (11)	0.0334 (8)	0.0370 (8)	0.0071 (7)	0.0177 (8)	0.0041 (6)
C4	0.0333 (7)	0.0331 (7)	0.0306 (7)	0.0031 (6)	0.0093 (6)	0.0007 (5)
C5	0.0405 (8)	0.0261 (7)	0.0297 (7)	0.0009 (5)	0.0084 (6)	−0.0024 (5)
C6	0.0367 (7)	0.0256 (7)	0.0300 (7)	−0.0060 (5)	0.0047 (6)	−0.0010 (5)
C7	0.0318 (7)	0.0238 (6)	0.0293 (7)	−0.0020 (5)	0.0052 (5)	0.0007 (5)
O	0.0610 (8)	0.0437 (7)	0.0337 (6)	0.0007 (5)	0.0133 (5)	0.0131 (5)
N1	0.0283 (6)	0.0286 (6)	0.0192 (5)	−0.0033 (4)	0.0027 (4)	−0.0002 (4)
N2	0.0441 (7)	0.0331 (6)	0.0310 (6)	−0.0010 (5)	0.0119 (5)	0.0018 (5)

Zn1—Cl1	2.2515 (4)	C5—H13	0.966
Zn1—Cl2	2.2779 (4)	C5—H14	0.976
Zn1—Cl3	2.2950 (4)	C6—C7	1.5056 (19)
Zn1—Cl4	2.2486 (4)	C6—H16	0.973
O—C2	1.427 (2)	C6—H15	0.961
O—C3	1.419 (2)	C7—N2	1.4790 (18)
C2—C1	1.494 (2)	C7—H18	0.954
C2—H7	0.966	C7—H17	0.957
C2—H8	0.962	N2—H2	0.875
C1—N1	1.5036 (18)	N2—H3	0.866
C1—H5	0.950	N2—H4	0.869
C1—H6	0.961	C4—C3	1.510 (2)
N1—C5	1.5032 (17)	C4—H11	0.963
N1—C4	1.4922 (18)	C4—H12	0.965
N1—H1	0.875	C3—H9	0.974
C5—C6	1.508 (2)	C3—H10	0.966
Cl1—Zn1—Cl2	107.710 (16)	C5—C6—C7	114.36 (12)
Cl1—Zn1—Cl3	110.593 (17)	C5—C6—H16	109.5
Cl2—Zn1—Cl3	104.316 (14)	C7—C6—H16	109.4
Cl1—Zn1—Cl4	109.501 (17)	C5—C6—H15	106.5
Cl2—Zn1—Cl4	109.997 (17)	C7—C6—H15	107.2
Cl3—Zn1—Cl4	114.428 (17)	H16—C6—H15	109.8
C2—O—C3	109.87 (13)	C6—C7—N2	109.25 (12)
O—C2—C1	110.87 (14)	C6—C7—H18	110.7
O—C2—H7	110.3	N2—C7—H18	107.7
C1—C2—H7	109.9	C6—C7—H17	111.5
O—C2—H8	108.8	N2—C7—H17	108.1
C1—C2—H8	107.1	H18—C7—H17	109.5
H7—C2—H8	109.9	C7—N2—H2	109.7
C2—C1—N1	111.48 (13)	C7—N2—H3	110.2
C2—C1—H5	111.0	H2—N2—H3	109.4
N1—C1—H5	106.6	C7—N2—H4	110.5
C2—C1—H6	110.1	H2—N2—H4	108.0
N1—C1—H6	107.0	H3—N2—H4	109.0
H5—C1—H6	110.5	N1—C4—C3	109.92 (13)
C1—N1—C5	107.86 (11)	N1—C4—H11	108.4
C1—N1—C4	109.72 (11)	C3—C4—H11	110.6
C5—N1—C4	113.91 (11)	N1—C4—H12	107.1
C1—N1—H1	107.7	C3—C4—H12	110.5
C5—N1—H1	108.7	H11—C4—H12	110.3
C4—N1—H1	108.8	C4—C3—O	110.79 (13)
N1—C5—C6	115.63 (11)	C4—C3—H9	110.1
N1—C5—H13	105.3	O—C3—H9	109.2
C6—C5—H13	111.7	C4—C3—H10	107.7
N1—C5—H14	104.5	O—C3—H10	108.4
C6—C5—H14	109.2	H9—C3—H10	110.5
H13—C5—H14	110.3

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2···Oi	0.87	1.95	2.821 (2)	173
N2—H3···Cl2	0.87	2.43	3.209 (2)	150
C1—H6···Cl2ii	0.96	2.72	3.653 (2)	164
C7—H18···Cl2iii	0.95	2.70	3.644 (2)	173
C5—H14···Cl4ii	0.98	2.82	3.657 (2)	144
N2—H4···Cl3iii	0.87	2.54	3.320 (2)	149
N1—H1···Cl3iv	0.88	2.42	3.206 (2)	149
C2—H7···Cl1iv	0.97	2.74	3.677 (2)	165

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2⋯Oi	0.87	1.95	2.821 (2)	173
N2—H3⋯Cl2	0.87	2.43	3.209 (2)	150
C1—H6⋯Cl2ii	0.96	2.72	3.653 (2)	164
C7—H18⋯Cl2iii	0.95	2.70	3.644 (2)	173
C5—H14⋯Cl4ii	0.98	2.82	3.657 (2)	144
N2—H4⋯Cl3iii	0.87	2.54	3.320 (2)	149
N1—H1⋯Cl3iv	0.88	2.42	3.206 (2)	149
C2—H7⋯Cl1iv	0.97	2.74	3.677 (2)	165

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