Poly[[triaqua(butane-1,2,3,4-tetra-carboxyl-ato)dimanganese(II)] mono-hydrate].

The asymmetric unit of the title Mn(II) coordination polymer, {[Mn(2)(C(8)H(6)O(8))(H(2)O)(3)]·H(2)O}(n), contains two crystallographic-ally independent Mn(II) cations, two half butane-1,2,3,4-tetra-carboxyl-ato anions, each lying on a centre of inversion, and four water mol-ecules. The Mn(II) cation has a distorted octa-hedral coordination environment. One Mn centre is coordinated by four carboxyl-ate O atoms from two different anions and two water O atoms. The other Mn centre is coordinated by five carboxyl-ate O atoms from four different anions and one water O atom. One water mol-ecule does not coordinate to a Mn centre. The crystal packing is stabilized by several O-H⋯O hydrogen bonds, forming a three-dimensional framework.

Related literature

For multicarboxyl­ate ligands in the construction of coordin­ation polymers, see: Yang et al. (2008 ▶). For butane-1,2,3,4-tetracarboxylic acid in coordination chemistry, see: Liu et al. (2008 ▶).

Experimental

Crystal data

[Mn2(C8H6O8)(H2O)3]·H2O

M = 824.14

Monoclinic,

a = 8.1962 (4) Å

b = 12.3291 (7) Å

c = 12.9758 (6) Å

β = 97.760 (5)°

V = 1299.22 (11) Å3

Z = 2

Mo Kα radiation

μ = 2.01 mm−1

T = 293 K

0.33 × 0.21 × 0.17 mm

Data collection

Bruker APEX CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.764, T max = 0.852

7085 measured reflections

3031 independent reflections

1990 reflections with I > 2σ(I)

R int = 0.040

Refinement

R[F 2 > 2σ(F 2)] = 0.041

wR(F 2) = 0.106

S = 0.88

3031 reflections

227 parameters

12 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.63 e Å−3

Δρmin = −0.83 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809042998/bt5105sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809042998/bt5105Isup2.hkl

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

[Mn2(C8H6O8)(H2O)3]·H2O	F(000) = 832
Mr = 824.14	Dx = 2.107 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3031 reflections
a = 8.1962 (4) Å	θ = 3.0–29.1°
b = 12.3291 (7) Å	µ = 2.01 mm−1
c = 12.9758 (6) Å	T = 293 K
β = 97.760 (5)°	Block, colorless
V = 1299.22 (11) Å3	0.33 × 0.21 × 0.17 mm
Z = 2

Bruker APEX CCD area-detector diffractometer	3031 independent reflections
Radiation source: fine-focus sealed tube	1990 reflections with I > 2σ(I)
graphite	Rint = 0.040
ω scans	θmax = 29.1°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→7
Tmin = 0.764, Tmax = 0.852	k = −12→15
7085 measured reflections	l = −17→17

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.106	H atoms treated by a mixture of independent and constrained refinement
S = 0.88	w = 1/[σ2(Fo2) + (0.0651P)2] where P = (Fo2 + 2Fc2)/3
3031 reflections	(Δ/σ)max < 0.001
227 parameters	Δρmax = 0.63 e Å−3
12 restraints	Δρmin = −0.83 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
C1	1.1879 (4)	0.8429 (3)	0.8558 (3)	0.0198 (8)
C2	1.0480 (4)	0.8783 (3)	0.9135 (3)	0.0271 (9)
H2A	1.0241	0.8197	0.9590	0.033*
H2B	0.9507	0.8893	0.8630	0.033*
C3	1.0781 (4)	0.9804 (3)	0.9778 (3)	0.0205 (7)
H3	1.1109	1.0378	0.9325	0.025*
C4	1.2178 (4)	0.9664 (3)	1.0691 (3)	0.0193 (8)
C5	0.9481 (4)	0.5441 (3)	0.8594 (3)	0.0193 (8)
C6	0.9556 (4)	0.4695 (3)	0.9522 (2)	0.0220 (8)
H6	1.0203	0.4052	0.9395	0.026*
C7	0.7837 (5)	0.4336 (3)	0.9692 (3)	0.0306 (9)
H7A	0.7915	0.3939	1.0343	0.037*
H7B	0.7172	0.4976	0.9760	0.037*
C8	0.6978 (5)	0.3639 (3)	0.8845 (3)	0.0275 (9)
O1	1.0249 (3)	0.5178 (2)	0.78555 (18)	0.0248 (6)
O2	0.8740 (3)	0.6329 (2)	0.85773 (19)	0.0263 (6)
O1W	1.0570 (4)	0.2456 (3)	0.8215 (3)	0.0391 (8)
O3	1.1646 (3)	0.7613 (2)	0.7983 (2)	0.0287 (6)
O2W	0.9047 (4)	0.2290 (3)	0.5915 (3)	0.0425 (8)
HW22	0.969 (4)	0.181 (3)	0.575 (4)	0.064*
O4	1.3228 (3)	0.8944 (2)	0.87012 (19)	0.0253 (6)
O3W	1.1264 (4)	0.6245 (3)	0.6096 (2)	0.0357 (7)
HW31	1.129 (6)	0.5569 (10)	0.597 (3)	0.054*
O5	0.7513 (3)	0.3496 (2)	0.7980 (2)	0.0317 (7)
O4W	1.0955 (15)	0.0359 (7)	0.6785 (11)	0.192 (4)
HW41	1.181 (13)	0.011 (12)	0.654 (14)	0.288*
HW42	1.06 (2)	−0.021 (8)	0.705 (14)	0.288*
O6	0.5696 (4)	0.3186 (3)	0.9039 (3)	0.0458 (9)
O7	1.2229 (3)	0.8806 (2)	1.12238 (19)	0.0268 (6)
O8	1.3177 (3)	1.0437 (2)	1.08580 (19)	0.0253 (6)
Mn1	0.96260 (7)	0.36380 (5)	0.70273 (4)	0.02057 (16)
Mn2	0.95382 (6)	0.68692 (4)	0.70684 (4)	0.01775 (15)
HW11	0.979 (4)	0.205 (3)	0.835 (4)	0.064 (18)*
HW12	1.129 (4)	0.203 (3)	0.802 (4)	0.065 (18)*
HW21	0.812 (2)	0.198 (3)	0.592 (4)	0.041 (14)*
HW32	1.102 (6)	0.654 (3)	0.5505 (18)	0.063 (18)*

	U11	U22	U33	U12	U13	U23
C1	0.0179 (17)	0.025 (2)	0.0152 (16)	0.0031 (16)	−0.0039 (14)	0.0026 (15)
C2	0.0181 (18)	0.032 (2)	0.0288 (19)	0.0020 (17)	−0.0043 (16)	−0.0103 (17)
C3	0.0188 (17)	0.0238 (19)	0.0173 (16)	0.0020 (16)	−0.0032 (14)	−0.0006 (15)
C4	0.0162 (16)	0.023 (2)	0.0180 (16)	0.0050 (16)	−0.0016 (14)	−0.0002 (16)
C5	0.0191 (17)	0.021 (2)	0.0153 (16)	−0.0061 (16)	−0.0080 (14)	−0.0003 (14)
C6	0.0279 (18)	0.0190 (19)	0.0169 (16)	−0.0047 (17)	−0.0054 (15)	−0.0017 (15)
C7	0.035 (2)	0.030 (2)	0.0261 (19)	−0.010 (2)	−0.0026 (17)	0.0011 (18)
C8	0.026 (2)	0.017 (2)	0.036 (2)	0.0032 (17)	−0.0059 (18)	−0.0048 (17)
O1	0.0317 (14)	0.0231 (14)	0.0188 (12)	−0.0017 (12)	0.0005 (11)	−0.0016 (11)
O2	0.0284 (14)	0.0264 (16)	0.0232 (13)	0.0014 (12)	0.0005 (11)	0.0024 (12)
O1W	0.0288 (16)	0.0375 (19)	0.0508 (19)	0.0121 (16)	0.0045 (15)	0.0166 (16)
O3	0.0197 (13)	0.0327 (16)	0.0328 (14)	−0.0037 (12)	0.0006 (11)	−0.0140 (13)
O2W	0.0367 (17)	0.0322 (18)	0.061 (2)	−0.0119 (15)	0.0148 (16)	−0.0229 (16)
O4	0.0191 (12)	0.0246 (15)	0.0323 (14)	−0.0045 (11)	0.0040 (11)	−0.0093 (12)
O3W	0.0359 (17)	0.0418 (19)	0.0312 (16)	−0.0032 (15)	0.0116 (14)	−0.0101 (14)
O5	0.0291 (15)	0.0325 (17)	0.0296 (15)	0.0015 (13)	−0.0098 (12)	−0.0031 (13)
O4W	0.179 (9)	0.162 (8)	0.243 (11)	0.014 (6)	0.060 (8)	0.014 (8)
O6	0.0260 (15)	0.047 (2)	0.065 (2)	−0.0131 (15)	0.0074 (15)	−0.0301 (17)
O7	0.0205 (12)	0.0259 (16)	0.0313 (14)	0.0006 (11)	−0.0070 (11)	0.0080 (12)
O8	0.0227 (13)	0.0288 (16)	0.0226 (12)	−0.0054 (12)	−0.0035 (10)	0.0006 (11)
Mn1	0.0198 (3)	0.0200 (3)	0.0207 (3)	−0.0005 (2)	−0.0016 (2)	0.0007 (2)
Mn2	0.0165 (3)	0.0188 (3)	0.0166 (3)	0.0002 (2)	−0.0029 (2)	0.0014 (2)

C1—O3	1.252 (4)	O1—Mn2	2.360 (3)
C1—O4	1.267 (4)	O2—Mn2	2.247 (2)
C1—C2	1.515 (5)	O1W—Mn1	2.185 (3)
C2—C3	1.512 (5)	O1W—HW11	0.850 (10)
C2—H2A	0.9700	O1W—HW12	0.854 (10)
C2—H2B	0.9700	O3—Mn2	2.163 (3)
C3—C4	1.542 (5)	O2W—Mn1	2.211 (3)
C3—C3i	1.549 (7)	O2W—HW22	0.843 (10)
C3—H3	0.9800	O2W—HW21	0.845 (10)
C4—O8	1.257 (4)	O4—Mn1iii	2.140 (2)
C4—O7	1.262 (4)	O3W—Mn2	2.160 (3)
C5—O2	1.251 (4)	O3W—HW31	0.850 (10)
C5—O1	1.258 (4)	O3W—HW32	0.849 (10)
C5—C6	1.510 (5)	O5—Mn1	2.267 (3)
C6—C7	1.521 (5)	O4W—HW41	0.86 (12)
C6—C6ii	1.546 (7)	O4W—HW42	0.85 (13)
C6—H6	0.9800	O6—Mn2iv	2.160 (3)
C7—C8	1.494 (6)	O7—Mn2v	2.217 (3)
C7—H7A	0.9700	O8—Mn1v	2.127 (3)
C7—H7B	0.9700	Mn1—O8vi	2.127 (3)
C8—O6	1.245 (5)	Mn1—O4vii	2.140 (2)
C8—O5	1.271 (5)	Mn2—O6viii	2.160 (3)
O1—Mn1	2.207 (3)	Mn2—O7vi	2.217 (3)
O3—C1—O4	123.3 (3)	C1—O3—Mn2	135.5 (2)
O3—C1—C2	117.5 (3)	Mn1—O2W—HW22	128 (3)
O4—C1—C2	119.2 (3)	Mn1—O2W—HW21	116 (3)
C1—C2—C3	115.7 (3)	HW22—O2W—HW21	106.4 (17)
C1—C2—H2A	108.3	C1—O4—Mn1iii	126.9 (2)
C3—C2—H2A	108.3	Mn2—O3W—HW31	120 (3)
C1—C2—H2B	108.3	Mn2—O3W—HW32	106 (3)
C3—C2—H2B	108.3	HW31—O3W—HW32	104.9 (16)
H2A—C2—H2B	107.4	C8—O5—Mn1	148.3 (3)
C2—C3—C4	112.3 (3)	HW41—O4W—HW42	101 (13)
C2—C3—C3i	112.5 (4)	C8—O6—Mn2iv	101.8 (2)
C4—C3—C3i	108.3 (3)	C4—O7—Mn2v	123.3 (2)
C2—C3—H3	107.8	C4—O8—Mn1v	144.9 (2)
C4—C3—H3	107.8	O8vi—Mn1—O4vii	90.20 (9)
C3i—C3—H3	107.8	O8vi—Mn1—O1W	166.12 (11)
O8—C4—O7	124.7 (3)	O4vii—Mn1—O1W	101.26 (10)
O8—C4—C3	116.5 (3)	O8vi—Mn1—O1	87.51 (10)
O7—C4—C3	118.8 (3)	O4vii—Mn1—O1	85.02 (10)
O2—C5—O1	120.3 (3)	O1W—Mn1—O1	101.15 (11)
O2—C5—C6	120.9 (3)	O8vi—Mn1—O2W	83.53 (12)
O1—C5—C6	118.7 (3)	O4vii—Mn1—O2W	87.77 (11)
C5—C6—C7	110.8 (3)	O1W—Mn1—O2W	89.06 (14)
C5—C6—C6ii	107.9 (4)	O1—Mn1—O2W	168.48 (11)
C7—C6—C6ii	111.8 (4)	O8vi—Mn1—O5	92.08 (10)
C5—C6—H6	108.8	O4vii—Mn1—O5	171.42 (10)
C7—C6—H6	108.8	O1W—Mn1—O5	77.75 (11)
C6ii—C6—H6	108.8	O1—Mn1—O5	86.81 (9)
C8—C7—C6	114.5 (3)	O2W—Mn1—O5	100.70 (11)
C8—C7—H7A	108.6	O3W—Mn2—O6viii	83.43 (13)
C6—C7—H7A	108.6	O3W—Mn2—O3	86.20 (11)
C8—C7—H7B	108.6	O6viii—Mn2—O3	92.23 (12)
C6—C7—H7B	108.6	O3W—Mn2—O7vi	99.22 (11)
H7A—C7—H7B	107.6	O6viii—Mn2—O7vi	87.70 (12)
O6—C8—O5	121.2 (4)	O3—Mn2—O7vi	174.53 (10)
O6—C8—C7	115.8 (3)	O3W—Mn2—O2	133.95 (12)
O5—C8—C7	123.0 (4)	O6viii—Mn2—O2	142.39 (11)
C5—O1—Mn1	119.0 (2)	O3—Mn2—O2	87.30 (10)
C5—O1—Mn2	89.0 (2)	O7vi—Mn2—O2	89.42 (10)
Mn1—O1—Mn2	121.45 (11)	O3W—Mn2—O1	78.19 (11)
C5—O2—Mn2	94.4 (2)	O6viii—Mn2—O1	161.24 (11)
Mn1—O1W—HW11	110 (3)	O3—Mn2—O1	90.28 (10)
Mn1—O1W—HW12	114 (4)	O7vi—Mn2—O1	91.54 (10)
HW11—O1W—HW12	104.7 (16)	O2—Mn2—O1	56.30 (9)

D—H···A	D—H	H···A	D···A	D—H···A
O2W—HW22···O6ix	0.84 (1)	2.46 (5)	2.998 (4)	122 (4)
O2W—HW22···O4W	0.84 (1)	2.39 (4)	2.985 (10)	128 (4)
O3W—HW31···O4vii	0.85 (1)	2.08 (2)	2.874 (4)	156 (4)
O4W—HW41···O1vii	0.86 (12)	2.43 (14)	3.091 (12)	133 (16)
O4W—HW42···O6iv	0.85 (13)	2.58 (14)	3.124 (11)	123 (14)
O1W—HW11···O7ii	0.85 (1)	2.10 (1)	2.944 (4)	173 (4)
O1W—HW12···O3vii	0.85 (1)	2.39 (4)	2.935 (4)	123 (3)
O2W—HW21···O2iv	0.85 (1)	1.92 (2)	2.731 (4)	161 (4)
O3W—HW32···O2Wx	0.85 (1)	2.33 (2)	3.155 (5)	163 (5)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2W—HW22⋯O6i	0.843 (10)	2.46 (5)	2.998 (4)	122 (4)
O2W—HW22⋯O4W	0.843 (10)	2.39 (4)	2.985 (10)	128 (4)
O3W—HW31⋯O4ii	0.850 (10)	2.075 (19)	2.874 (4)	156 (4)
O4W—HW41⋯O1ii	0.86 (12)	2.43 (14)	3.091 (12)	133 (16)
O4W—HW42⋯O6iii	0.85 (13)	2.58 (14)	3.124 (11)	123 (14)
O1W—HW11⋯O7iv	0.850 (10)	2.098 (11)	2.944 (4)	173 (4)
O1W—HW12⋯O3ii	0.854 (10)	2.39 (4)	2.935 (4)	123 (3)
O2W—HW21⋯O2iii	0.845 (10)	1.919 (18)	2.731 (4)	161 (4)
O3W—HW32⋯O2Wv	0.849 (10)	2.333 (17)	3.155 (5)	163 (5)

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