catena-Poly[[diaqua-cobalt(II)]-μ(2)-7-oxa-bicyclo-[2.2.1]heptane-2,3-dicarboxyl-ato-κO,O,O:O].

The polymeric title complex, [Co(C(8)H(8)O(5))(H(2)O)(2)](n) was synthesized by reaction of cobalt acetate with 7-oxabicyclo-[2,2,1]heptane-2,3-dicarb-oxy-lic anhydride. The Co(II) ion is six-coordinated in a distorted octa-hedral environment, binding to two water O atoms, to the ether O atom of the bicyclo-heptane unit, to two carboxyl-ate O atoms from two different carboxyl-ate groups of the same anion and to one carboxyl-ate O atom from a symmetry-related anion. The bridging character of the dianion leads to the formation of ribbons along [001]. The ribbons are linked into a layered network parallel to (010) by several O-H⋯O hydrogen-bonding inter-actions involving the coordinating water mol-ecules as donors and the carboxyl-ate O atoms of neighbouring ribbons as acceptors. The crystal under investigation was an inversion twin.

Related literature

For background to the applications of norcantharidin [systematic name: 7-oxabicyclo­(2.2.1)heptane-2,3-dicarb­oxy­lic anhydride], see: Yang et al. (2002 ▶). For the isotypic Cu analogue, see: Wang et al. (2009a ▶), and for a related Ni complex with monoclinic symmetry, see: Wang et al. (2009b ▶).

Experimental

Crystal data

[Co(C8H8O5)(H2O)2]

M = 279.11

Orthorhombic,

a = 10.3794 (10) Å

b = 18.983 (3) Å

c = 10.5021 (12) Å

V = 2069.3 (5) Å3

Z = 8

Mo Kα radiation

μ = 1.68 mm−1

T = 296 K

0.22 × 0.15 × 0.10 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2006 ▶) T min = 0.742, T max = 0.851

13174 measured reflections

1837 independent reflections

1821 reflections with I > 2σ(I)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.029

wR(F 2) = 0.088

S = 1.00

1837 reflections

146 parameters

7 restraints

H-atom parameters constrained

Δρmax = 0.32 e Å−3

Δρmin = −0.77 e Å−3

Absolute structure: Flack (1983 ▶), 860 Friedel pairs

Flack parameter: 0.12 (3)

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; 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: SHELXL97.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812000554/wm2580sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812000554/wm2580Isup2.hkl

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

[Co(C8H8O5)(H2O)2]	F(000) = 1144
Mr = 279.11	Dx = 1.792 Mg m−3
Orthorhombic, Iba2	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: I 2 -2c	Cell parameters from 9954 reflections
a = 10.3794 (10) Å	θ = 2.2–25.0°
b = 18.983 (3) Å	µ = 1.68 mm−1
c = 10.5021 (12) Å	T = 296 K
V = 2069.3 (5) Å3	Block, red
Z = 8	0.22 × 0.15 × 0.10 mm

Bruker APEXII area-detector diffractometer	1837 independent reflections
Radiation source: fine-focus sealed tube	1821 reflections with I > 2σ(I)
graphite	Rint = 0.025
ω scans	θmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2006)	h = −12→9
Tmin = 0.742, Tmax = 0.851	k = −22→22
13174 measured reflections	l = −12→12

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)] = 0.029	H-atom parameters constrained
wR(F2) = 0.088	w = 1/[σ2(Fo2) + (0.0734P)2 + 1.6545P] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max = 0.001
1837 reflections	Δρmax = 0.32 e Å−3
146 parameters	Δρmin = −0.77 e Å−3
7 restraints	Absolute structure: Flack (1983), 860 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.12 (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
Co1	0.23966 (4)	0.966647 (19)	0.74932 (8)	0.02813 (16)
O1W	0.1588 (3)	0.91672 (15)	0.5806 (2)	0.0429 (6)
H1WA	0.2080	0.9431	0.5369	0.064*
H1WB	0.0843	0.8987	0.5727	0.064*
O1	0.3221 (2)	0.99510 (11)	0.9348 (2)	0.0248 (4)
O2W	0.1226 (2)	1.06142 (12)	0.7759 (2)	0.0374 (6)
H2WA	0.0483	1.0731	0.8026	0.056*
H2WB	0.1121	1.0858	0.7089	0.056*
O2	0.3530 (2)	0.96635 (11)	1.1378 (2)	0.0257 (5)
O3	0.1138 (2)	0.90091 (11)	0.8609 (2)	0.0303 (5)
O4	0.0868 (2)	0.85747 (12)	1.0548 (2)	0.0309 (5)
O5	0.37724 (17)	0.87420 (9)	0.76172 (19)	0.0215 (4)
C1	0.4783 (3)	0.87921 (15)	0.8584 (3)	0.0242 (6)
H1	0.5346	0.9202	0.8480	0.029*
C2	0.4010 (3)	0.87971 (14)	0.9824 (3)	0.0201 (6)
H2	0.4522	0.8587	1.0510	0.024*
C3	0.2838 (3)	0.82969 (15)	0.9480 (3)	0.0217 (6)
H3	0.2852	0.7878	1.0023	0.026*
C4	0.3196 (3)	0.80965 (14)	0.8104 (3)	0.0258 (6)
H4	0.2465	0.7927	0.7597	0.031*
C5	0.4367 (4)	0.75899 (17)	0.8103 (4)	0.0389 (8)
H5A	0.4272	0.7223	0.8738	0.047*
H5B	0.4492	0.7376	0.7273	0.047*
C6	0.5475 (3)	0.80918 (18)	0.8437 (3)	0.0351 (7)
H6A	0.5895	0.7953	0.9224	0.042*
H6B	0.6110	0.8110	0.7760	0.042*
C7	0.3557 (2)	0.95301 (15)	1.0216 (3)	0.0179 (6)
C8	0.1514 (3)	0.86588 (14)	0.9561 (3)	0.0211 (6)

	U11	U22	U33	U12	U13	U23
Co1	0.0293 (2)	0.0306 (3)	0.0245 (2)	−0.00025 (14)	0.0007 (2)	0.0048 (2)
O1W	0.0397 (14)	0.0645 (17)	0.0247 (11)	−0.0249 (12)	−0.0039 (11)	0.0043 (12)
O1	0.0329 (11)	0.0223 (10)	0.0191 (9)	0.0030 (8)	0.0000 (9)	0.0004 (8)
O2W	0.0309 (12)	0.0419 (12)	0.0394 (14)	0.0150 (10)	0.0098 (10)	0.0125 (10)
O2	0.0236 (12)	0.0331 (10)	0.0203 (10)	0.0057 (8)	−0.0002 (9)	−0.0052 (7)
O3	0.0186 (10)	0.0394 (12)	0.0329 (12)	0.0013 (9)	0.0023 (9)	0.0144 (10)
O4	0.0272 (11)	0.0399 (12)	0.0257 (11)	0.0020 (9)	0.0057 (9)	0.0035 (9)
O5	0.0231 (9)	0.0226 (9)	0.0187 (10)	0.0008 (7)	0.0006 (8)	−0.0003 (8)
C1	0.0195 (13)	0.0282 (14)	0.0249 (15)	0.0029 (11)	0.0012 (12)	−0.0046 (11)
C2	0.0196 (13)	0.0224 (14)	0.0183 (13)	0.0023 (11)	−0.0012 (11)	−0.0008 (11)
C3	0.0240 (13)	0.0184 (13)	0.0227 (14)	−0.0009 (12)	−0.0005 (12)	0.0036 (11)
C4	0.0310 (16)	0.0205 (13)	0.0259 (14)	−0.0007 (11)	−0.0011 (13)	−0.0034 (11)
C5	0.051 (2)	0.0250 (15)	0.0408 (18)	0.0140 (14)	0.0077 (17)	−0.0045 (13)
C6	0.0303 (16)	0.0438 (17)	0.0312 (17)	0.0170 (14)	0.0038 (15)	−0.0048 (14)
C7	0.0125 (12)	0.0237 (13)	0.0174 (14)	−0.0020 (10)	−0.0001 (11)	−0.0046 (11)
C8	0.0200 (14)	0.0196 (13)	0.0238 (14)	−0.0038 (10)	−0.0011 (12)	−0.0001 (11)

Co1—O2i	2.091 (2)	C1—C6	1.519 (4)
Co1—O3	2.154 (2)	C1—C2	1.529 (4)
Co1—O1W	2.178 (3)	C1—H1	0.9800
Co1—O2W	2.188 (2)	C2—C7	1.525 (4)
Co1—O1	2.194 (2)	C2—C3	1.585 (4)
Co1—O5	2.2664 (18)	C2—H2	0.9800
O1W—H1WA	0.8500	C3—C8	1.539 (4)
O1W—H1WB	0.8500	C3—C4	1.540 (4)
O1—C7	1.262 (4)	C3—H3	0.9800
O2W—H2WA	0.8501	C4—C5	1.550 (4)
O2W—H2WB	0.8499	C4—H4	0.9800
O2—C7	1.246 (4)	C5—C6	1.534 (5)
O2—Co1ii	2.091 (2)	C5—H5A	0.9700
O3—C8	1.262 (4)	C5—H5B	0.9700
O4—C8	1.244 (4)	C6—H6A	0.9700
O5—C4	1.456 (3)	C6—H6B	0.9700
O5—C1	1.462 (4)
O2i—Co1—O3	176.84 (9)	C1—C2—C3	101.8 (2)
O2i—Co1—O1W	91.46 (10)	C7—C2—H2	109.9
O3—Co1—O1W	87.54 (10)	C1—C2—H2	109.9
O2i—Co1—O2W	83.31 (9)	C3—C2—H2	109.9
O3—Co1—O2W	94.03 (8)	C8—C3—C4	112.2 (2)
O1W—Co1—O2W	104.34 (11)	C8—C3—C2	113.9 (2)
O2i—Co1—O1	97.37 (9)	C4—C3—C2	100.2 (2)
O3—Co1—O1	84.03 (9)	C8—C3—H3	110.0
O1W—Co1—O1	168.35 (9)	C4—C3—H3	110.0
O2W—Co1—O1	84.31 (9)	C2—C3—H3	110.0
O2i—Co1—O5	98.56 (8)	O5—C4—C3	102.7 (2)
O3—Co1—O5	84.39 (7)	O5—C4—C5	101.5 (2)
O1W—Co1—O5	87.28 (10)	C3—C4—C5	110.1 (2)
O2W—Co1—O5	168.22 (10)	O5—C4—H4	113.8
O1—Co1—O5	83.92 (8)	C3—C4—H4	113.8
Co1—O1W—H1WA	87.2	C5—C4—H4	113.8
Co1—O1W—H1WB	127.2	C6—C5—C4	101.7 (2)
H1WA—O1W—H1WB	137.0	C6—C5—H5A	111.4
C7—O1—Co1	126.40 (17)	C4—C5—H5A	111.4
Co1—O2W—H2WA	139.4	C6—C5—H5B	111.4
Co1—O2W—H2WB	114.5	C4—C5—H5B	111.4
H2WA—O2W—H2WB	90.8	H5A—C5—H5B	109.3
C7—O2—Co1ii	133.2 (2)	C1—C6—C5	102.2 (3)
C8—O3—Co1	123.30 (19)	C1—C6—H6A	111.3
C4—O5—C1	96.1 (2)	C5—C6—H6A	111.3
C4—O5—Co1	114.38 (16)	C1—C6—H6B	111.3
C1—O5—Co1	116.19 (14)	C5—C6—H6B	111.3
O5—C1—C6	102.2 (2)	H6A—C6—H6B	109.2
O5—C1—C2	102.4 (2)	O2—C7—O1	124.9 (3)
C6—C1—C2	109.8 (2)	O2—C7—C2	117.2 (2)
O5—C1—H1	113.7	O1—C7—C2	117.9 (2)
C6—C1—H1	113.7	O4—C8—O3	124.1 (3)
C2—C1—H1	113.7	O4—C8—C3	118.0 (3)
C7—C2—C1	113.4 (2)	O3—C8—C3	117.8 (3)
C7—C2—C3	111.8 (2)
O2i—Co1—O1—C7	−134.4 (2)	C7—C2—C3—C4	122.2 (2)
O3—Co1—O1—C7	48.5 (2)	C1—C2—C3—C4	0.9 (3)
O1W—Co1—O1—C7	4.6 (6)	C1—O5—C4—C3	57.7 (2)
O2W—Co1—O1—C7	143.1 (2)	Co1—O5—C4—C3	−64.7 (2)
O5—Co1—O1—C7	−36.5 (2)	C1—O5—C4—C5	−56.1 (2)
O1W—Co1—O3—C8	131.9 (2)	Co1—O5—C4—C5	−178.54 (17)
O2W—Co1—O3—C8	−123.9 (2)	C8—C3—C4—O5	85.4 (3)
O1—Co1—O3—C8	−40.0 (2)	C2—C3—C4—O5	−35.8 (3)
O5—Co1—O3—C8	44.4 (2)	C8—C3—C4—C5	−167.1 (2)
O2i—Co1—O5—C4	−167.10 (18)	C2—C3—C4—C5	71.7 (3)
O3—Co1—O5—C4	11.75 (19)	O5—C4—C5—C6	34.5 (3)
O1W—Co1—O5—C4	−76.03 (19)	C3—C4—C5—C6	−73.8 (3)
O2W—Co1—O5—C4	94.6 (4)	O5—C1—C6—C5	−35.0 (3)
O1—Co1—O5—C4	96.32 (19)	C2—C1—C6—C5	73.2 (3)
O2i—Co1—O5—C1	82.24 (18)	C4—C5—C6—C1	0.3 (3)
O3—Co1—O5—C1	−98.90 (18)	Co1ii—O2—C7—O1	27.9 (4)
O1W—Co1—O5—C1	173.31 (19)	Co1ii—O2—C7—C2	−151.0 (2)
O2W—Co1—O5—C1	−16.1 (5)	Co1—O1—C7—O2	−149.7 (2)
O1—Co1—O5—C1	−14.33 (18)	Co1—O1—C7—C2	29.1 (3)
C4—O5—C1—C6	57.0 (3)	C1—C2—C7—O2	−144.6 (3)
Co1—O5—C1—C6	178.01 (18)	C3—C2—C7—O2	101.0 (3)
C4—O5—C1—C2	−56.8 (2)	C1—C2—C7—O1	36.5 (3)
Co1—O5—C1—C2	64.2 (2)	C3—C2—C7—O1	−77.9 (3)
O5—C1—C2—C7	−86.2 (3)	Co1—O3—C8—O4	142.1 (2)
C6—C1—C2—C7	165.7 (2)	Co1—O3—C8—C3	−39.6 (3)
O5—C1—C2—C3	34.1 (3)	C4—C3—C8—O4	149.2 (3)
C6—C1—C2—C3	−74.0 (3)	C2—C3—C8—O4	−97.8 (3)
C7—C2—C3—C8	2.2 (3)	C4—C3—C8—O3	−29.2 (3)
C1—C2—C3—C8	−119.1 (2)	C2—C3—C8—O3	83.8 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O1i	0.85	1.98	2.832 (3)	180
O2W—H2WB···O4i	0.85	1.96	2.811 (3)	180
O1W—H1WB···O4iii	0.85	1.95	2.800 (3)	180
O2W—H2WA···O3iv	0.85	1.86	2.708 (3)	180

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯O1i	0.85	1.98	2.832 (3)	180
O2W—H2WB⋯O4i	0.85	1.96	2.811 (3)	180
O1W—H1WB⋯O4ii	0.85	1.95	2.800 (3)	180
O2W—H2WA⋯O3iii	0.85	1.86	2.708 (3)	180

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