catena-Poly[[triaqua-nickel(II)]-μ-5-carb-oxy-benzene-1,3-dicarboxyl-ato-κO:O].

In the title compound, [Ni(C(9)H(4)O(6))(H(2)O)(3)](n), the Ni(II) ion has a distorted NiO(5) square-pyramidal geometry, the maximum deviation from the least-squares plane formed by the basal atoms being 0.9351 (13) Å. The basal plane is formed by two O atoms from carboxyl-ate residues of the 5-carb-oxy-benzene-1,3-dicarboxyl-ate ligand and by two O atoms from water mol-ecules. The O atom of the third water mol-ecule is axially positioned, 1.7890 (19) Å perpendicular to the basal plane. The 5-carb-oxy-benzene-1,3-dicarboxyl-ate ligand bridges the metal atoms, forming a polymeric chain along the b axis. O-H⋯O hydrogen bonds between the water mol-ecules and carboxyl-ate groups stabilize the crystal structure.

Related literature

For the applications and stuctures of related metal complexes of 1,3,5-benzene­tricarb­oxy­lic acid, see: Xia et al. (2004 ▶); Modec & Brencic (2005 ▶); Wei & Han (2005 ▶); Han & Wei (2005 ▶); Wang et al. (2005 ▶); Che et al. (2008 ▶); He et al. (2008 ▶); Li et al. (2008 ▶); Gao et al. (2009 ▶). For bond-length data, see: Allen et al. (1987 ▶).

Experimental

Crystal data

[Ni(C9H4O6)(H2O)3]

M = 320.88

Monoclinic,

a = 6.838 (2) Å

b = 18.809 (5) Å

c = 10.705 (3) Å

β = 126.901 (14)°

V = 1101.0 (5) Å3

Z = 4

Mo Kα radiation

μ = 1.81 mm−1

T = 296 K

0.30 × 0.25 × 0.20 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.613, T max = 0.714

7973 measured reflections

1938 independent reflections

1864 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.102

S = 1.01

1938 reflections

173 parameters

H-atom parameters constrained

Δρmax = 0.32 e Å−3

Δρmin = −0.38 e Å−3

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; 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 datablock(s) global, I. DOI: 10.1107/S1600536811035227/go2022sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811035227/go2022Isup2.hkl

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

[Ni(C9H4O6)(H2O)3]	F(000) = 656
Mr = 320.88	Dx = 1.936 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6807 reflections
a = 6.838 (2) Å	θ = 2.6–27.8°
b = 18.809 (5) Å	µ = 1.81 mm−1
c = 10.705 (3) Å	T = 296 K
β = 126.901 (14)°	Block, green
V = 1101.0 (5) Å3	0.30 × 0.25 × 0.20 mm
Z = 4

Bruker SMART APEXII CCD area-detector diffractometer	1938 independent reflections
Radiation source: fine-focus sealed tube	1864 reflections with I > 2σ(I)
graphite	Rint = 0.021
φ and ω scans	θmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −8→8
Tmin = 0.613, Tmax = 0.714	k = −22→21
7973 measured reflections	l = −10→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)] = 0.023	H-atom parameters constrained
wR(F2) = 0.102	w = 1/[σ2(Fo2) + (0.0942P)2 + 0.090P] where P = (Fo2 + 2Fc2)/3
S = 1.01	(Δ/σ)max = 0.002
1938 reflections	Δρmax = 0.32 e Å−3
173 parameters	Δρmin = −0.38 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: 0.036 (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 takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused 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 andgoodness of fit S are based on F2, conventional R-factors R are basedon F, with F set to zero for negative F2. The threshold expression ofF2 > σ(F2) is used only for calculating R-factors(gt) etc. and isnot relevant to the choice of reflections for refinement. R-factors basedon 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	0.1199 (3)	0.63000 (10)	0.3748 (2)	0.0228 (4)
C2	0.2227 (3)	0.56454 (10)	0.4747 (2)	0.0203 (4)
C3	0.3935 (3)	0.57173 (10)	0.6364 (2)	0.0213 (4)
H3	0.4431	0.6168	0.6806	0.026*
C4	0.4892 (3)	0.51227 (11)	0.7312 (2)	0.0220 (4)
C5	0.4154 (3)	0.44487 (11)	0.6640 (2)	0.0231 (4)
H5	0.4805	0.4047	0.7273	0.028*
C6	0.2465 (3)	0.43711 (10)	0.5040 (2)	0.0196 (4)
C7	0.1480 (3)	0.49745 (10)	0.4085 (2)	0.0209 (4)
H7	0.0327	0.4925	0.3010	0.025*
C8	0.6645 (4)	0.51904 (11)	0.9031 (2)	0.0281 (5)
C9	0.1625 (3)	0.36441 (10)	0.4346 (2)	0.0214 (4)
Ni1	0.11091 (4)	0.773616 (12)	0.32089 (3)	0.01894 (19)
O1	0.2116 (3)	0.68864 (7)	0.44634 (16)	0.0274 (4)
O2	−0.0451 (3)	0.62603 (8)	0.23299 (18)	0.0408 (4)
O3	0.7481 (3)	0.58432 (8)	0.95119 (18)	0.0371 (4)
H3A	0.8391	0.5853	1.0470	0.056*
O4	0.7292 (4)	0.47053 (9)	0.99436 (19)	0.0532 (6)
O5	0.2577 (3)	0.31100 (8)	0.51934 (18)	0.0314 (4)
O6	−0.0066 (3)	0.36214 (7)	0.28913 (17)	0.0304 (4)
O1W	−0.1375 (4)	0.78863 (9)	0.3587 (2)	0.0448 (5)
H1W	−0.0823	0.8266	0.4123	0.067*
H2W	−0.1097	0.7563	0.4230	0.067*
O2W	0.3070 (3)	0.74742 (11)	0.2478 (2)	0.0430 (4)
H4W	0.4388	0.7241	0.3076	0.065*
H3W	0.3268	0.7712	0.1886	0.065*
O3W	0.4158 (3)	0.82950 (8)	0.53994 (18)	0.0394 (4)
H5W	0.4312	0.8744	0.5432	0.059*
H6W	0.5507	0.8132	0.5647	0.059*

	U11	U22	U33	U12	U13	U23
C1	0.0263 (9)	0.0193 (10)	0.0166 (9)	0.0008 (7)	0.0096 (7)	−0.0008 (8)
C2	0.0241 (9)	0.0153 (10)	0.0193 (9)	−0.0015 (7)	0.0119 (8)	0.0002 (7)
C3	0.0246 (9)	0.0140 (10)	0.0209 (9)	−0.0032 (7)	0.0113 (8)	−0.0021 (8)
C4	0.0240 (10)	0.0193 (9)	0.0181 (10)	−0.0005 (8)	0.0103 (8)	−0.0008 (8)
C5	0.0285 (9)	0.0155 (10)	0.0227 (10)	0.0014 (7)	0.0141 (8)	0.0032 (7)
C6	0.0238 (9)	0.0163 (10)	0.0192 (9)	−0.0016 (7)	0.0132 (8)	−0.0018 (7)
C7	0.0239 (9)	0.0194 (10)	0.0181 (9)	−0.0020 (8)	0.0119 (8)	−0.0025 (8)
C8	0.0316 (10)	0.0233 (11)	0.0215 (10)	−0.0010 (8)	0.0117 (9)	−0.0021 (8)
C9	0.0246 (9)	0.0170 (10)	0.0243 (10)	−0.0003 (7)	0.0157 (8)	−0.0014 (8)
Ni1	0.0249 (2)	0.0112 (3)	0.0160 (3)	0.00245 (7)	0.00978 (19)	0.00329 (7)
O1	0.0346 (8)	0.0141 (7)	0.0212 (7)	−0.0010 (5)	0.0102 (6)	0.0009 (6)
O2	0.0520 (10)	0.0239 (9)	0.0193 (8)	0.0012 (7)	0.0070 (7)	0.0010 (7)
O3	0.0508 (10)	0.0231 (8)	0.0189 (8)	−0.0080 (7)	0.0111 (7)	−0.0034 (6)
O4	0.0761 (13)	0.0245 (9)	0.0189 (8)	−0.0031 (8)	0.0072 (8)	0.0062 (7)
O5	0.0348 (8)	0.0179 (8)	0.0331 (8)	−0.0015 (6)	0.0159 (7)	0.0024 (6)
O6	0.0358 (8)	0.0196 (7)	0.0222 (7)	−0.0037 (6)	0.0102 (6)	−0.0057 (6)
O1W	0.0583 (11)	0.0283 (8)	0.0682 (13)	0.0123 (9)	0.0489 (11)	0.0156 (9)
O2W	0.0453 (10)	0.0524 (11)	0.0384 (9)	0.0201 (9)	0.0289 (9)	0.0161 (9)
O3W	0.0399 (8)	0.0279 (9)	0.0331 (8)	−0.0027 (7)	0.0126 (7)	−0.0066 (7)

C1—O2	1.236 (3)	C9—O5	1.244 (2)
C1—O1	1.273 (2)	C9—O6	1.266 (3)
C1—C2	1.500 (3)	Ni1—O6i	1.9129 (15)
C2—C7	1.386 (3)	Ni1—O1	1.9292 (14)
C2—C3	1.397 (3)	Ni1—O2W	1.9781 (17)
C3—C4	1.383 (3)	Ni1—O1W	1.9884 (18)
C3—H3	0.9300	Ni1—O3W	2.2536 (16)
C4—C5	1.394 (3)	O3—H3A	0.8200
C4—C8	1.480 (3)	O6—Ni1ii	1.9129 (15)
C5—C6	1.383 (3)	O1W—H1W	0.8501
C5—H5	0.9300	O1W—H2W	0.8500
C6—C7	1.400 (3)	O2W—H4W	0.8501
C6—C9	1.496 (3)	O2W—H3W	0.8500
C7—H7	0.9300	O3W—H5W	0.8501
C8—O4	1.210 (3)	O3W—H6W	0.8500
C8—O3	1.321 (3)
O2—C1—O1	123.25 (18)	O5—C9—C6	119.96 (17)
O2—C1—C2	121.17 (17)	O6—C9—C6	115.87 (16)
O1—C1—C2	115.58 (16)	O6i—Ni1—O1	174.25 (7)
C7—C2—C3	119.92 (18)	O6i—Ni1—O2W	93.67 (7)
C7—C2—C1	120.79 (17)	O1—Ni1—O2W	91.48 (7)
C3—C2—C1	119.28 (17)	O6i—Ni1—O1W	87.32 (7)
C4—C3—C2	120.44 (18)	O1—Ni1—O1W	88.13 (7)
C4—C3—H3	119.8	O2W—Ni1—O1W	168.69 (8)
C2—C3—H3	119.8	O6i—Ni1—O3W	90.27 (6)
C3—C4—C5	119.43 (18)	O1—Ni1—O3W	86.65 (6)
C3—C4—C8	121.08 (18)	O2W—Ni1—O3W	96.01 (8)
C5—C4—C8	119.48 (17)	O1W—Ni1—O3W	95.25 (8)
C6—C5—C4	120.64 (18)	C1—O1—Ni1	117.27 (12)
C6—C5—H5	119.7	C8—O3—H3A	109.5
C4—C5—H5	119.7	C9—O6—Ni1ii	120.96 (13)
C5—C6—C7	119.76 (18)	Ni1—O1W—H1W	99.8
C5—C6—C9	119.82 (18)	Ni1—O1W—H2W	105.1
C7—C6—C9	120.37 (16)	H1W—O1W—H2W	105.1
C2—C7—C6	119.80 (17)	Ni1—O2W—H4W	119.7
C2—C7—H7	120.1	Ni1—O2W—H3W	127.8
C6—C7—H7	120.1	H4W—O2W—H3W	105.1
O4—C8—O3	121.55 (19)	Ni1—O3W—H5W	121.4
O4—C8—C4	124.72 (19)	Ni1—O3W—H6W	108.0
O3—C8—C4	113.73 (18)	H5W—O3W—H6W	105.1
O5—C9—O6	124.16 (18)
O2—C1—C2—C7	4.9 (3)	C3—C4—C8—O4	169.1 (2)
O1—C1—C2—C7	−176.04 (17)	C5—C4—C8—O4	−9.6 (3)
O2—C1—C2—C3	−174.3 (2)	C3—C4—C8—O3	−10.9 (3)
O1—C1—C2—C3	4.8 (3)	C5—C4—C8—O3	170.43 (19)
C7—C2—C3—C4	0.2 (3)	C5—C6—C9—O5	−5.2 (3)
C1—C2—C3—C4	179.35 (17)	C7—C6—C9—O5	177.22 (18)
C2—C3—C4—C5	0.6 (3)	C5—C6—C9—O6	174.46 (18)
C2—C3—C4—C8	−178.15 (18)	C7—C6—C9—O6	−3.1 (3)
C3—C4—C5—C6	−0.6 (3)	O2—C1—O1—Ni1	−7.3 (3)
C8—C4—C5—C6	178.15 (19)	C2—C1—O1—Ni1	173.69 (13)
C4—C5—C6—C7	−0.1 (3)	O2W—Ni1—O1—C1	−72.99 (16)
C4—C5—C6—C9	−177.68 (17)	O1W—Ni1—O1—C1	95.70 (16)
C3—C2—C7—C6	−0.8 (3)	O3W—Ni1—O1—C1	−168.93 (15)
C1—C2—C7—C6	179.97 (17)	O5—C9—O6—Ni1ii	−6.8 (3)
C5—C6—C7—C2	0.8 (3)	C6—C9—O6—Ni1ii	173.52 (12)
C9—C6—C7—C2	178.38 (17)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3A···O2iii	0.82	1.81	2.568 (2)	152.
O1W—H1W···O3iv	0.85	2.21	2.869 (3)	134.
O1W—H2W···O5v	0.85	1.94	2.680 (2)	145.
O2W—H4W···O5vi	0.85	1.89	2.715 (2)	165.
O3W—H5W···O4vii	0.85	2.03	2.778 (2)	147.
O3W—H6W···O2viii	0.85	2.49	3.068 (3)	126.
O2W—H3W···O1ix	0.85	2.34	3.123 (2)	154.

Table 1

Selected bond lengths (Å)

Ni1—O1	1.9292 (14)
Ni1—O2W	1.9781 (17)
Ni1—O1W	1.9884 (18)
Ni1—O3W	2.2536 (16)
O6—Ni1i	1.9129 (15)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3A⋯O2ii	0.82	1.81	2.568 (2)	152
O1W—H1W⋯O3iii	0.85	2.21	2.869 (3)	134
O1W—H2W⋯O5iv	0.85	1.94	2.680 (2)	145
O2W—H4W⋯O5v	0.85	1.89	2.715 (2)	165
O3W—H5W⋯O4vi	0.85	2.03	2.778 (2)	147
O3W—H6W⋯O2vii	0.85	2.49	3.068 (3)	126
O2W—H3W⋯O1viii	0.85	2.34	3.123 (2)	154

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .