(μ-Ethane-1,1,2,2-tetra-carboxyl-ato)bis-[tetra-aqua-manganese(II)].

In the centrosymmetric title molecule, [Mn(2)(C(6)H(2)O(8))(H(2)O)(8)], the Mn(II) atom is in an octa-hedral environment coordinated by six O-atom donors from water mol-ecules and ethane-1,1,2,2-tetra-carboxyl-ate ligands. The crystal structure features a three-dimensional hydrogen-bonding network based on a strong and distinctive pattern of O-H⋯O hydrogen-bonding inter-actions.

Related literature

For related literature on metal–organic frameworks, see: Chen et al. (2007 ▶); Fan & Zhu (2006 ▶); Li & Yang (2006 ▶). For related literature on hydrogen bonding, see: Forster & Cheetham (2002 ▶); Kim & Jung (2000 ▶).

Experimental

Crystal data

[Mn2(C6H2O8)(H2O)8]

M = 456.08

Triclinic,

a = 6.2901 (12) Å

b = 8.0212 (15) Å

c = 8.0769 (15) Å

α = 108.522 (3)°

β = 95.068 (3)°

γ = 97.086 (3)°

V = 379.92 (12) Å3

Z = 1

Mo Kα radiation

μ = 1.75 mm−1

T = 293 K

0.30 × 0.26 × 0.24 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.785, T max = 0.823

1956 measured reflections

1379 independent reflections

1309 reflections with I > 2σ(I)

R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 0.069

S = 1.05

1379 reflections

144 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.30 e Å−3

Δρmin = −0.30 e Å−3

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SMART; data reduction: SAINT (Bruker, 2000 ▶); program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811008063/pb2059sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811008063/pb2059Isup2.hkl

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

[Mn2(C6H2O8)(H2O)8]	Z = 1
Mr = 456.08	F(000) = 232.0
Triclinic, P1	Dx = 1.993 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.2901 (12) Å	Cell parameters from 924 reflections
b = 8.0212 (15) Å	θ = 2.2–20.2°
c = 8.0769 (15) Å	µ = 1.75 mm−1
α = 108.522 (3)°	T = 293 K
β = 95.068 (3)°	Block, brown
γ = 97.086 (3)°	0.30 × 0.26 × 0.24 mm
V = 379.92 (12) Å3

Bruker SMART CCD area-detector diffractometer	1379 independent reflections
Radiation source: fine-focus sealed tube	1309 reflections with I > 2σ(I)
graphite	Rint = 0.044
φ and ω scans	θmax = 25.5°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −6→7
Tmin = 0.785, Tmax = 0.823	k = −9→9
1956 measured reflections	l = −9→9

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ2(Fo2) + (0.0451P)2] where P = (Fo2 + 2Fc2)/3
1379 reflections	(Δ/σ)max = 0.001
144 parameters	Δρmax = 0.30 e Å−3
0 restraints	Δρmin = −0.30 e Å−3

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
Mn1	0.30762 (4)	0.25813 (4)	0.70315 (3)	0.02040 (14)
O1	−0.0280 (3)	0.2382 (3)	0.6000 (2)	0.0407 (4)
O2	0.6555 (2)	0.3118 (2)	0.8276 (2)	0.0249 (3)
O3	0.3825 (3)	0.5167 (2)	0.6758 (2)	0.0388 (4)
O4	0.3632 (3)	0.1354 (2)	0.43505 (19)	0.0293 (3)
O5	0.2172 (2)	0.34158 (18)	0.96515 (17)	0.0238 (3)
O6	0.2933 (2)	−0.00729 (18)	0.72542 (18)	0.0246 (3)
O7	0.1900 (2)	0.28929 (19)	1.21579 (17)	0.0282 (3)
O8	0.3028 (2)	−0.1656 (2)	0.90616 (19)	0.0297 (3)
C1	0.1621 (3)	0.2406 (2)	1.0530 (2)	0.0186 (4)
C2	0.0577 (3)	0.0477 (2)	0.9454 (2)	0.0184 (4)
H9	−0.050 (3)	0.053 (3)	0.853 (3)	0.022*
C3	0.2319 (3)	−0.0512 (2)	0.8542 (2)	0.0192 (4)
H3	0.685 (4)	0.421 (5)	0.890 (4)	0.046 (8)*
H4	0.669 (4)	0.260 (4)	0.883 (4)	0.036 (8)*
H7	0.292 (4)	0.177 (4)	0.373 (3)	0.034 (7)*
H8	0.475 (6)	0.111 (5)	0.400 (5)	0.077 (12)*
H5	0.519 (9)	0.581 (8)	0.691 (7)	0.15 (2)*
H1	−0.108 (7)	0.278 (6)	0.663 (6)	0.100 (15)*
H2	−0.092 (6)	0.175 (5)	0.510 (5)	0.067 (11)*
H6	0.332 (6)	0.591 (6)	0.719 (5)	0.077 (13)*

	U11	U22	U33	U12	U13	U23
Mn1	0.0220 (2)	0.02101 (19)	0.01841 (19)	0.00202 (12)	0.00384 (12)	0.00706 (13)
O1	0.0267 (9)	0.0621 (12)	0.0257 (9)	0.0078 (8)	0.0007 (7)	0.0045 (8)
O2	0.0274 (8)	0.0220 (8)	0.0251 (8)	0.0022 (6)	0.0024 (6)	0.0086 (7)
O3	0.0508 (11)	0.0237 (8)	0.0427 (10)	0.0047 (8)	0.0128 (8)	0.0110 (7)
O4	0.0338 (9)	0.0375 (9)	0.0210 (7)	0.0145 (7)	0.0088 (7)	0.0114 (7)
O5	0.0331 (8)	0.0176 (7)	0.0200 (7)	0.0006 (6)	0.0069 (6)	0.0059 (5)
O6	0.0310 (8)	0.0234 (7)	0.0234 (7)	0.0073 (6)	0.0126 (6)	0.0098 (6)
O7	0.0389 (8)	0.0245 (7)	0.0180 (7)	−0.0011 (6)	0.0012 (6)	0.0057 (6)
O8	0.0345 (8)	0.0312 (8)	0.0317 (8)	0.0145 (6)	0.0116 (6)	0.0168 (6)
C1	0.0167 (9)	0.0192 (9)	0.0200 (9)	0.0048 (7)	0.0041 (7)	0.0056 (7)
C2	0.0196 (9)	0.0184 (9)	0.0177 (9)	0.0023 (7)	0.0031 (7)	0.0067 (7)
C3	0.0216 (9)	0.0163 (9)	0.0173 (9)	0.0006 (7)	0.0024 (7)	0.0032 (7)

Mn1—O3	2.1541 (18)	O3—H6	0.71 (4)
Mn1—O4	2.1552 (15)	O4—H7	0.82 (3)
Mn1—O5	2.1578 (13)	O4—H8	0.80 (4)
Mn1—O1	2.1674 (18)	O5—C1	1.273 (2)
Mn1—O6	2.1845 (14)	O6—C3	1.275 (2)
Mn1—O2	2.2557 (16)	O7—C1	1.236 (2)
O1—H1	0.77 (4)	O8—C3	1.237 (2)
O1—H2	0.78 (4)	C1—C2	1.541 (3)
O2—H3	0.85 (3)	C2—C2i	1.515 (3)
O2—H4	0.71 (3)	C2—C3	1.536 (2)
O3—H5	0.92 (6)	C2—H9	0.98 (2)
O3—Mn1—O4	89.71 (7)	Mn1—O3—H5	126 (3)
O3—Mn1—O5	98.50 (6)	Mn1—O3—H6	123 (3)
O4—Mn1—O5	170.75 (6)	H5—O3—H6	96 (4)
O3—Mn1—O1	90.76 (8)	Mn1—O4—H7	107.7 (18)
O4—Mn1—O1	87.24 (7)	Mn1—O4—H8	128 (3)
O5—Mn1—O1	88.40 (6)	H7—O4—H8	113 (3)
O3—Mn1—O6	169.57 (7)	C1—O5—Mn1	126.22 (12)
O4—Mn1—O6	86.03 (6)	C3—O6—Mn1	125.18 (11)
O5—Mn1—O6	86.55 (5)	O7—C1—O5	123.56 (17)
O1—Mn1—O6	98.54 (7)	O7—C1—C2	120.04 (16)
O3—Mn1—O2	84.27 (8)	O5—C1—C2	116.39 (16)
O4—Mn1—O2	96.98 (6)	C2i—C2—C3	112.65 (19)
O5—Mn1—O2	88.12 (6)	C2i—C2—C1	112.95 (19)
O1—Mn1—O2	173.45 (7)	C3—C2—C1	108.56 (14)
O6—Mn1—O2	86.79 (6)	C2i—C2—H9	107.6 (13)
Mn1—O1—H1	120 (3)	C3—C2—H9	107.4 (13)
Mn1—O1—H2	129 (3)	C1—C2—H9	107.4 (15)
H1—O1—H2	109 (4)	O8—C3—O6	124.24 (16)
Mn1—O2—H3	107.8 (18)	O8—C3—C2	120.15 (16)
Mn1—O2—H4	110 (2)	O6—C3—C2	115.61 (16)
H3—O2—H4	109 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H3···O5ii	0.85 (3)	1.88 (3)	2.726 (2)	174 (3)
O2—H4···O8iii	0.71 (3)	2.07 (3)	2.765 (2)	166 (3)
O4—H7···O7iv	0.82 (3)	1.89 (3)	2.689 (2)	167 (2)
O4—H8···O6v	0.80 (4)	1.97 (4)	2.757 (2)	167 (4)
O3—H5···O7ii	0.92 (6)	1.95 (6)	2.847 (2)	165 (5)
O1—H1···O2vi	0.77 (4)	2.07 (4)	2.818 (2)	164 (5)
O1—H2···O6vii	0.78 (4)	2.14 (4)	2.914 (2)	175 (4)
O3—H6···O8viii	0.71 (4)	2.10 (4)	2.771 (2)	158 (4)