catena-Poly[[diaqua-nickel(II)]-μ-7-oxabicyclo-[2.2.1]heptane-2,3-di-carboxyl-ato].

In the crystal structure of the title compound, [Ni(C(8)H(8)O(5))(H(2)O)(2)](n), the Ni(II) cation is in a Jahn-Teller-distorted octahedral coordination environment binding to two O atoms from water molecules, the bridging O atom of the bicycloheptane unit, two carboxylate O atoms from different carboxylate groups and one carboxylate O atom from a symmetry-related bridging ligand. The crystal structure is made up from layers propagating parallel to the bc plane.

Related literature

For the structure of the Cu(II) analogue, see: Wang et al. (2009 ▶).

Experimental

Crystal data

[Ni(C8H8O5)(H2O)2]

M = 278.89

Monoclinic,

a = 10.9145 (2) Å

b = 8.6281 (2) Å

c = 10.8581 (2) Å

β = 107.351 (1)°

V = 975.99 (3) Å3

Z = 4

Mo Kα radiation

μ = 2.01 mm−1

T = 296 K

0.27 × 0.20 × 0.10 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.618, T max = 0.817

7972 measured reflections

2213 independent reflections

1961 reflections with I > 2σ(I)

R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.059

S = 1.02

2213 reflections

157 parameters

6 restraints

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: 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: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809021771/at2793sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809021771/at2793Isup2.hkl

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

[Ni(C8H8O5)(H2O)2]	F(000) = 576
Mr = 278.89	Dx = 1.898 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4375 reflections
a = 10.9145 (2) Å	θ = 2.0–27.5°
b = 8.6281 (2) Å	µ = 2.01 mm−1
c = 10.8581 (2) Å	T = 296 K
β = 107.351 (1)°	Block, green
V = 975.99 (3) Å3	0.27 × 0.20 × 0.10 mm
Z = 4

Bruker APEXII area-detector diffractometer	2213 independent reflections
Radiation source: fine-focus sealed tube	1961 reflections with I > 2σ(I)
graphite	Rint = 0.019
ω scans	θmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→14
Tmin = 0.618, Tmax = 0.817	k = −11→6
7972 measured reflections	l = −12→14

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)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ2(Fo2) + (0.032P)2 + 0.4246P] where P = (Fo2 + 2Fc2)/3
2213 reflections	(Δ/σ)max = 0.001
157 parameters	Δρmax = 0.30 e Å−3
6 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
C1	0.73787 (15)	−0.1019 (2)	0.71021 (15)	0.0214 (3)
H1A	0.7710	−0.2053	0.7005	0.026*
C2	0.75289 (16)	0.0067 (2)	0.60404 (16)	0.0234 (3)
H2A	0.6816	0.0008	0.5240	0.028*
C3	0.88388 (17)	−0.0131 (2)	0.58426 (19)	0.0329 (4)
H3A	0.8888	0.0402	0.5072	0.039*
H3B	0.9048	−0.1216	0.5789	0.039*
C4	0.97214 (18)	0.0632 (3)	0.7078 (2)	0.0375 (5)
H4A	1.0324	−0.0110	0.7599	0.045*
H4B	1.0192	0.1498	0.6872	0.045*
C5	0.87589 (15)	0.1175 (2)	0.77610 (17)	0.0265 (4)
H5A	0.9073	0.2034	0.8363	0.032*
C6	0.82547 (16)	−0.0207 (2)	0.83620 (16)	0.0234 (3)
H6A	0.8966	−0.0891	0.8805	0.028*
C7	0.59962 (14)	−0.1119 (2)	0.71114 (15)	0.0202 (3)
C8	0.75095 (16)	0.0292 (2)	0.92900 (15)	0.0242 (4)
O1W	0.69190 (12)	0.44064 (15)	0.74994 (13)	0.0289 (3)
H1WA	0.711 (2)	0.473 (3)	0.6846 (18)	0.043*
H1WB	0.643 (2)	0.505 (2)	0.765 (2)	0.043*
O1	0.56501 (12)	−0.23749 (14)	0.74852 (12)	0.0244 (3)
O2W	0.51314 (14)	0.29376 (19)	0.53124 (13)	0.0383 (3)
H2WA	0.557 (2)	0.322 (3)	0.486 (2)	0.057*
H2WB	0.4472 (17)	0.342 (3)	0.512 (2)	0.057*
O2	0.75780 (15)	−0.05131 (17)	1.02529 (12)	0.0389 (3)
O3	0.52811 (11)	0.00446 (14)	0.67765 (13)	0.0272 (3)
O4	0.68270 (12)	0.15134 (16)	0.89954 (11)	0.0302 (3)
O5	0.76514 (11)	0.15762 (14)	0.66735 (11)	0.0236 (3)
Ni1	0.601796 (19)	0.22532 (2)	0.714683 (19)	0.01937 (8)

	U11	U22	U33	U12	U13	U23
C1	0.0213 (8)	0.0212 (8)	0.0245 (8)	0.0010 (6)	0.0109 (6)	−0.0017 (6)
C2	0.0216 (8)	0.0296 (9)	0.0221 (8)	−0.0007 (7)	0.0111 (6)	−0.0032 (7)
C3	0.0287 (9)	0.0413 (11)	0.0364 (10)	0.0019 (8)	0.0217 (8)	−0.0008 (8)
C4	0.0218 (9)	0.0503 (13)	0.0452 (11)	−0.0038 (8)	0.0172 (8)	0.0003 (10)
C5	0.0196 (8)	0.0318 (10)	0.0285 (9)	−0.0051 (7)	0.0080 (7)	−0.0037 (7)
C6	0.0194 (7)	0.0285 (9)	0.0225 (8)	0.0031 (7)	0.0066 (6)	0.0014 (7)
C7	0.0218 (8)	0.0217 (8)	0.0194 (8)	−0.0035 (6)	0.0098 (6)	−0.0058 (6)
C8	0.0240 (8)	0.0299 (9)	0.0181 (8)	−0.0004 (7)	0.0053 (6)	−0.0013 (7)
O1W	0.0290 (7)	0.0249 (7)	0.0357 (7)	0.0008 (5)	0.0145 (6)	−0.0014 (5)
O1	0.0236 (6)	0.0228 (6)	0.0306 (6)	−0.0026 (5)	0.0138 (5)	0.0003 (5)
O2W	0.0377 (8)	0.0566 (10)	0.0238 (7)	0.0112 (7)	0.0144 (6)	0.0103 (6)
O2	0.0555 (9)	0.0399 (8)	0.0258 (7)	0.0123 (7)	0.0187 (6)	0.0097 (6)
O3	0.0220 (6)	0.0209 (6)	0.0421 (7)	−0.0007 (5)	0.0145 (5)	−0.0011 (5)
O4	0.0364 (7)	0.0357 (8)	0.0218 (6)	0.0119 (6)	0.0137 (5)	0.0046 (5)
O5	0.0234 (6)	0.0249 (6)	0.0254 (6)	0.0001 (5)	0.0118 (5)	0.0019 (5)
Ni1	0.02056 (12)	0.02009 (13)	0.01992 (12)	0.00083 (8)	0.00979 (9)	0.00170 (8)

C1—C7	1.514 (2)	C6—H6A	0.9800
C1—C2	1.532 (2)	C7—O1	1.254 (2)
C1—C6	1.580 (2)	C7—O3	1.257 (2)
C1—H1A	0.9800	C8—O2	1.239 (2)
C2—O5	1.460 (2)	C8—O4	1.275 (2)
C2—C3	1.517 (2)	O1W—Ni1	2.0834 (13)
C2—H2A	0.9800	O1W—H1WA	0.841 (15)
C3—C4	1.546 (3)	O1W—H1WB	0.822 (15)
C3—H3A	0.9700	O1—Ni1i	2.0027 (12)
C3—H3B	0.9700	O2W—Ni1	2.0255 (13)
C4—C5	1.529 (2)	O2W—H2WA	0.824 (16)
C4—H4A	0.9700	O2W—H2WB	0.802 (16)
C4—H4B	0.9700	O3—Ni1	2.0608 (12)
C5—O5	1.457 (2)	O4—Ni1	2.0393 (12)
C5—C6	1.538 (2)	O5—Ni1	2.0809 (11)
C5—H5A	0.9800	Ni1—O1ii	2.0027 (12)
C6—C8	1.533 (2)
C7—C1—C2	111.72 (13)	C1—C6—H6A	110.1
C7—C1—C6	111.48 (13)	O1—C7—O3	124.24 (14)
C2—C1—C6	101.96 (13)	O1—C7—C1	116.61 (15)
C7—C1—H1A	110.5	O3—C7—C1	119.13 (15)
C2—C1—H1A	110.5	O2—C8—O4	123.98 (16)
C6—C1—H1A	110.5	O2—C8—C6	119.16 (16)
O5—C2—C3	102.07 (14)	O4—C8—C6	116.85 (14)
O5—C2—C1	101.93 (12)	Ni1—O1W—H1WA	110.9 (17)
C3—C2—C1	110.77 (14)	Ni1—O1W—H1WB	109.8 (17)
O5—C2—H2A	113.6	H1WA—O1W—H1WB	106.5 (19)
C3—C2—H2A	113.6	C7—O1—Ni1i	125.62 (11)
C1—C2—H2A	113.6	Ni1—O2W—H2WA	119.0 (17)
C2—C3—C4	101.47 (14)	Ni1—O2W—H2WB	122.3 (17)
C2—C3—H3A	111.5	H2WA—O2W—H2WB	109 (2)
C4—C3—H3A	111.5	C7—O3—Ni1	120.63 (11)
C2—C3—H3B	111.5	C8—O4—Ni1	123.69 (11)
C4—C3—H3B	111.5	C5—O5—C2	96.15 (13)
H3A—C3—H3B	109.3	C5—O5—Ni1	115.54 (9)
C5—C4—C3	102.17 (14)	C2—O5—Ni1	113.69 (9)
C5—C4—H4A	111.3	O1ii—Ni1—O2W	87.33 (6)
C3—C4—H4A	111.3	O1ii—Ni1—O4	90.36 (5)
C5—C4—H4B	111.3	O2W—Ni1—O4	177.14 (6)
C3—C4—H4B	111.3	O1ii—Ni1—O3	82.07 (5)
H4A—C4—H4B	109.2	O2W—Ni1—O3	91.92 (6)
O5—C5—C4	101.75 (14)	O4—Ni1—O3	86.09 (5)
O5—C5—C6	102.27 (13)	O1ii—Ni1—O5	172.30 (5)
C4—C5—C6	110.67 (16)	O2W—Ni1—O5	91.84 (5)
O5—C5—H5A	113.7	O4—Ni1—O5	90.22 (5)
C4—C5—H5A	113.7	O3—Ni1—O5	90.31 (5)
C6—C5—H5A	113.7	O1ii—Ni1—O1W	103.17 (5)
C8—C6—C5	112.87 (15)	O2W—Ni1—O1W	88.95 (6)
C8—C6—C1	113.00 (13)	O4—Ni1—O1W	93.22 (5)
C5—C6—C1	100.21 (13)	O3—Ni1—O1W	174.73 (5)
C8—C6—H6A	110.1	O5—Ni1—O1W	84.46 (5)
C5—C6—H6A	110.1
C7—C1—C2—O5	85.11 (15)	C6—C8—O4—Ni1	28.8 (2)
C6—C1—C2—O5	−34.06 (14)	C4—C5—O5—C2	56.04 (15)
C7—C1—C2—C3	−166.92 (14)	C6—C5—O5—C2	−58.43 (14)
C6—C1—C2—C3	73.92 (16)	C4—C5—O5—Ni1	176.00 (11)
O5—C2—C3—C4	35.96 (17)	C6—C5—O5—Ni1	61.53 (14)
C1—C2—C3—C4	−71.93 (18)	C3—C2—O5—C5	−57.44 (14)
C2—C3—C4—C5	−1.3 (2)	C1—C2—O5—C5	57.12 (13)
C3—C4—C5—O5	−33.65 (19)	C3—C2—O5—Ni1	−178.84 (10)
C3—C4—C5—C6	74.44 (18)	C1—C2—O5—Ni1	−64.27 (13)
O5—C5—C6—C8	−84.19 (16)	C8—O4—Ni1—O1ii	133.87 (14)
C4—C5—C6—C8	168.06 (15)	C8—O4—Ni1—O2W	97.8 (11)
O5—C5—C6—C1	36.27 (15)	C8—O4—Ni1—O3	51.85 (14)
C4—C5—C6—C1	−71.48 (16)	C8—O4—Ni1—O5	−38.45 (14)
C7—C1—C6—C8	−0.2 (2)	C8—O4—Ni1—O1W	−122.91 (14)
C2—C1—C6—C8	119.17 (15)	C7—O3—Ni1—O1ii	−141.13 (13)
C7—C1—C6—C5	−120.54 (14)	C7—O3—Ni1—O2W	131.83 (12)
C2—C1—C6—C5	−1.20 (15)	C7—O3—Ni1—O4	−50.22 (12)
C2—C1—C7—O1	149.60 (15)	C7—O3—Ni1—O5	39.98 (12)
C6—C1—C7—O1	−97.04 (17)	C7—O3—Ni1—O1W	32.4 (6)
C2—C1—C7—O3	−31.8 (2)	C5—O5—Ni1—O1ii	−105.7 (4)
C6—C1—C7—O3	81.59 (18)	C2—O5—Ni1—O1ii	4.1 (4)
C5—C6—C8—O2	−145.66 (17)	C5—O5—Ni1—O2W	170.59 (12)
C1—C6—C8—O2	101.50 (19)	C2—O5—Ni1—O2W	−79.56 (11)
C5—C6—C8—O4	35.8 (2)	C5—O5—Ni1—O4	−11.38 (12)
C1—C6—C8—O4	−77.0 (2)	C2—O5—Ni1—O4	98.46 (11)
O3—C7—O1—Ni1i	−8.3 (2)	C5—O5—Ni1—O3	−97.47 (11)
C1—C7—O1—Ni1i	170.29 (10)	C2—O5—Ni1—O3	12.37 (10)
O1—C7—O3—Ni1	145.58 (13)	C5—O5—Ni1—O1W	81.83 (12)
C1—C7—O3—Ni1	−32.95 (18)	C2—O5—Ni1—O1W	−168.33 (11)
O2—C8—O4—Ni1	−149.69 (15)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O2iii	0.84 (2)	2.06 (2)	2.9027 (19)	180 (3)
O1W—H1WB···O3ii	0.82 (2)	2.13 (2)	2.7953 (17)	137 (2)
O1W—H1WB···O1iv	0.82 (2)	2.37 (2)	3.1013 (17)	149 (2)
O2W—H2WA···O4iii	0.82 (2)	1.89 (2)	2.6967 (19)	167 (3)
O2W—H2WB···O2ii	0.80 (2)	2.34 (2)	3.135 (2)	170 (2)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯O2i	0.841 (15)	2.062 (15)	2.9027 (19)	180 (3)
O1W—H1WB⋯O3ii	0.822 (15)	2.135 (18)	2.7953 (17)	137 (2)
O1W—H1WB⋯O1iii	0.822 (15)	2.366 (19)	3.1013 (17)	149 (2)
O2W—H2WA⋯O4i	0.824 (16)	1.888 (16)	2.6967 (19)	167 (3)
O2W—H2WB⋯O2ii	0.802 (16)	2.341 (16)	3.135 (2)	170 (2)

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