1,4-Diazo-niabicyclo-[2.2.2]octane hexa-aqua-magnesium bis-(sulfate).

In the title compound, (C(6)H(14)N(2))[Mg(H(2)O)(6)](SO(4))(2), the Mg(II) ion, lying on an inversion center, is coordinated by six water mol-ecules in a slightly distorted octa-hedral geometry. The 1,4-diazo-niabicyclo-[2.2.2]octane cation is located about a twofold rotation axis. Inter-molecular N-H⋯O and O-H⋯O hydrogen bonds link the cations and the anions into a three-dimensional network.

Related literature

For the properties and applications of amide salt compounds, see: Fu et al. (2007 ▶, 2008 ▶, 2009 ▶); Fu & Xiong (2008 ▶).

Experimental

Crystal data

(C6H14N2)[Mg(H2O)6](SO4)2

M = 438.74

Monoclinic,

a = 14.968 (3) Å

b = 9.1860 (18) Å

c = 14.334 (3) Å

β = 117.12 (3)°

V = 1754.2 (8) Å3

Z = 4

Mo Kα radiation

μ = 0.41 mm−1

T = 298 K

0.40 × 0.30 × 0.20 mm

Data collection

Rigaku SCXmini CCD diffractometer

Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T min = 0.89, T max = 0.95

8747 measured reflections

2014 independent reflections

1839 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.065

wR(F 2) = 0.169

S = 1.26

2014 reflections

116 parameters

H-atom parameters constrained

Δρmax = 1.30 e Å−3

Δρmin = −1.08 e Å−3

Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811005368/hy2403sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811005368/hy2403Isup2.hkl

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

(C6H14N2)[Mg(H2O)6](SO4)2	F(000) = 928
Mr = 438.74	Dx = 1.661 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2014 reflections
a = 14.968 (3) Å	θ = 3.1–27.5°
b = 9.1860 (18) Å	µ = 0.41 mm−1
c = 14.334 (3) Å	T = 298 K
β = 117.12 (3)°	Block, colorless
V = 1754.2 (8) Å3	0.40 × 0.30 × 0.20 mm
Z = 4

Rigaku SCXmini CCD diffractometer	2014 independent reflections
Radiation source: fine-focus sealed tube	1839 reflections with I > 2σ(I)
graphite	Rint = 0.022
Detector resolution: 13.6612 pixels mm-1	θmax = 27.5°, θmin = 3.1°
ω scans	h = −19→19
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	k = −11→11
Tmin = 0.89, Tmax = 0.95	l = −18→18
8747 measured reflections

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)] = 0.065	H-atom parameters constrained
wR(F2) = 0.169	w = 1/[σ2(Fo2) + (0.0899P)2 + 2.4679P] where P = (Fo2 + 2Fc2)/3
S = 1.26	(Δ/σ)max < 0.001
2014 reflections	Δρmax = 1.30 e Å−3
116 parameters	Δρmin = −1.08 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: 0.045 (4)

	x	y	z	Uiso*/Ueq
S1	0.61852 (4)	0.24340 (6)	0.11814 (4)	0.0233 (3)
O1W	0.17086 (15)	0.3991 (2)	0.04379 (17)	0.0371 (5)
H1WA	0.1091	0.3776	0.0197	0.056*
H1WB	0.1876	0.4636	0.0913	0.056*
Mg1	0.2500	0.2500	0.0000	0.0216 (3)
O2W	0.37984 (14)	0.3255 (2)	0.11889 (15)	0.0352 (5)
H2WA	0.4372	0.3244	0.1203	0.053*
H2WB	0.3855	0.3321	0.1805	0.053*
O1	0.68789 (16)	0.1296 (2)	0.18242 (15)	0.0383 (5)
O3W	0.23727 (17)	0.1023 (2)	0.10262 (15)	0.0397 (5)
H3WA	0.2082	0.0203	0.0839	0.059*
H3WB	0.2606	0.1142	0.1684	0.059*
O2	0.58702 (19)	0.3346 (3)	0.18142 (17)	0.0490 (7)
N1	−0.02189 (19)	0.2779 (3)	0.15657 (17)	0.0352 (6)
H1	−0.0387	0.2783	0.0870	0.042*
O3	0.52895 (16)	0.1720 (3)	0.03471 (16)	0.0450 (6)
O4	0.66399 (19)	0.3290 (2)	0.06522 (19)	0.0472 (6)
C1	0.0764 (3)	0.2074 (5)	0.2138 (3)	0.0538 (9)
H1B	0.1276	0.2641	0.2066	0.065*
H1C	0.0748	0.1110	0.1855	0.065*
C2	−0.1004 (3)	0.1967 (5)	0.1718 (3)	0.0569 (10)
H2A	−0.1012	0.0955	0.1522	0.068*
H2B	−0.1660	0.2382	0.1283	0.068*
C3	−0.0189 (4)	0.4288 (4)	0.1915 (3)	0.0575 (10)
H3A	−0.0855	0.4713	0.1572	0.069*
H3B	0.0254	0.4863	0.1734	0.069*

	U11	U22	U33	U12	U13	U23
S1	0.0256 (4)	0.0261 (4)	0.0189 (4)	−0.0006 (2)	0.0108 (3)	−0.00084 (19)
O1W	0.0286 (10)	0.0394 (11)	0.0437 (11)	−0.0001 (8)	0.0166 (9)	−0.0157 (9)
Mg1	0.0226 (6)	0.0232 (6)	0.0179 (6)	0.0001 (4)	0.0085 (5)	−0.0008 (4)
O2W	0.0254 (9)	0.0532 (13)	0.0245 (9)	−0.0056 (8)	0.0091 (8)	−0.0064 (8)
O1	0.0425 (11)	0.0411 (11)	0.0247 (9)	0.0132 (9)	0.0095 (8)	0.0013 (8)
O3W	0.0609 (14)	0.0335 (11)	0.0253 (10)	−0.0144 (9)	0.0203 (10)	−0.0001 (8)
O2	0.0632 (15)	0.0555 (15)	0.0317 (11)	0.0207 (12)	0.0247 (11)	−0.0024 (10)
N1	0.0370 (13)	0.0521 (15)	0.0166 (10)	0.0083 (11)	0.0122 (10)	0.0022 (9)
O3	0.0314 (11)	0.0643 (16)	0.0304 (11)	−0.0149 (10)	0.0064 (9)	−0.0022 (10)
O4	0.0637 (15)	0.0410 (13)	0.0503 (13)	−0.0170 (11)	0.0378 (13)	−0.0022 (10)
C1	0.052 (2)	0.073 (2)	0.0464 (19)	0.0296 (18)	0.0312 (17)	0.0097 (18)
C2	0.0463 (19)	0.078 (3)	0.0433 (19)	−0.0272 (19)	0.0174 (15)	−0.0236 (18)
C3	0.080 (3)	0.0389 (18)	0.064 (2)	0.0159 (17)	0.042 (2)	0.0226 (16)

S1—O4	1.458 (2)	O3W—H3WB	0.8502
S1—O2	1.462 (2)	N1—C3	1.467 (5)
S1—O1	1.466 (2)	N1—C1	1.469 (4)
S1—O3	1.482 (2)	N1—C2	1.490 (5)
O1W—Mg1	2.0856 (19)	N1—H1	0.9100
O1W—H1WA	0.8502	C1—C2ii	1.513 (5)
O1W—H1WB	0.8500	C1—H1B	0.9700
Mg1—O2W	2.035 (2)	C1—H1C	0.9700
Mg1—O2Wi	2.035 (2)	C2—C1ii	1.513 (5)
Mg1—O3Wi	2.0728 (19)	C2—H2A	0.9700
Mg1—O3W	2.0728 (19)	C2—H2B	0.9700
Mg1—O1Wi	2.0856 (19)	C3—C3ii	1.506 (8)
O2W—H2WA	0.8499	C3—H3A	0.9700
O2W—H2WB	0.8502	C3—H3B	0.9700
O3W—H3WA	0.8499
O4—S1—O2	111.89 (16)	Mg1—O3W—H3WA	123.8
O4—S1—O1	110.28 (14)	Mg1—O3W—H3WB	125.4
O2—S1—O1	110.80 (12)	H3WA—O3W—H3WB	110.9
O4—S1—O3	106.49 (14)	C3—N1—C1	111.0 (3)
O2—S1—O3	109.00 (14)	C3—N1—C2	109.1 (3)
O1—S1—O3	108.21 (14)	C1—N1—C2	110.7 (3)
Mg1—O1W—H1WA	112.8	C3—N1—H1	108.7
Mg1—O1W—H1WB	134.3	C1—N1—H1	108.7
H1WA—O1W—H1WB	110.8	C2—N1—H1	108.7
O2W—Mg1—O2Wi	180.00 (17)	N1—C1—C2ii	108.5 (3)
O2W—Mg1—O3Wi	90.55 (9)	N1—C1—H1B	110.0
O2Wi—Mg1—O3Wi	89.45 (9)	C2ii—C1—H1B	110.0
O2W—Mg1—O3W	89.45 (9)	N1—C1—H1C	110.0
O2Wi—Mg1—O3W	90.55 (9)	C2ii—C1—H1C	110.0
O3Wi—Mg1—O3W	180.00 (13)	H1B—C1—H1C	108.4
O2W—Mg1—O1Wi	91.10 (8)	N1—C2—C1ii	108.2 (3)
O2Wi—Mg1—O1Wi	88.90 (8)	N1—C2—H2A	110.1
O3Wi—Mg1—O1Wi	88.14 (9)	C1ii—C2—H2A	110.1
O3W—Mg1—O1Wi	91.86 (9)	N1—C2—H2B	110.1
O2W—Mg1—O1W	88.90 (8)	C1ii—C2—H2B	110.1
O2Wi—Mg1—O1W	91.10 (8)	H2A—C2—H2B	108.4
O3Wi—Mg1—O1W	91.86 (9)	N1—C3—C3ii	108.51 (18)
O3W—Mg1—O1W	88.14 (9)	N1—C3—H3A	110.0
O1Wi—Mg1—O1W	180.00 (10)	C3ii—C3—H3A	110.0
Mg1—O2W—H2WA	125.8	N1—C3—H3B	110.0
Mg1—O2W—H2WB	119.9	C3ii—C3—H3B	110.0
H2WA—O2W—H2WB	110.8	H3A—C3—H3B	108.4
C3—N1—C1—C2ii	64.8 (4)	C1—N1—C2—C1ii	65.4 (4)
C2—N1—C1—C2ii	−56.5 (4)	C1—N1—C3—C3ii	−55.0 (5)
C3—N1—C2—C1ii	−57.0 (5)	C2—N1—C3—C3ii	67.3 (5)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O3i	0.91	1.87	2.734 (3)	157
O1W—H1WA···O3i	0.85	1.90	2.751 (3)	179
O1W—H1WB···O1iii	0.85	2.01	2.835 (3)	165
O2W—H2WA···O2	0.85	2.00	2.809 (3)	158
O2W—H2WB···O2iv	0.85	1.83	2.674 (3)	173
O3W—H3WA···O4v	0.85	1.85	2.694 (3)	170
O3W—H3WB···O1iv	0.85	1.92	2.769 (3)	177

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯O3i	0.91	1.87	2.734 (3)	157
O1W—H1WA⋯O3i	0.85	1.90	2.751 (3)	179
O1W—H1WB⋯O1ii	0.85	2.01	2.835 (3)	165
O2W—H2WA⋯O2	0.85	2.00	2.809 (3)	158
O2W—H2WB⋯O2iii	0.85	1.83	2.674 (3)	173
O3W—H3WA⋯O4iv	0.85	1.85	2.694 (3)	170
O3W—H3WB⋯O1iii	0.85	1.92	2.769 (3)	177

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