Poly[μ-aqua-aqua-μ4-naphthalene-1,8-dicarboxyl-ato-barium]: a layer structure.

The title compound, [Ba(C12H6O4)(H2O)2] n , is represented by a layer-like structure built of BaO8 polyhedra. The asymmetric unit contains a Ba(2+) ion, half a coordinating water mol-ecule and half a μ4-bridging naphthalene-1,8-dicarboxyl-ate (1,8-nap) ligand, the whole structure being generated by twofold rotational symmetry. The carboxyl-ate groups of the 1,8-nap ligands act as bridges linking four Ba(2+) ions, while each Ba(2+) ion is eight-coordinated by O atoms from four 1,8-nap ligands and two coordinating water mol-ecules. In the crystal, there are O-H⋯O hydrogen bonds involving the water mol-ecules and carboxyl-ate O atoms in the BaO8 polyhedra. Each BaO8 polyhedron is connected via corner-sharing water O atoms or edge-sharing ligand O atoms, forming a sheet parallel to the bc plane. These sheets stack along the a-axis direction and are connected via van der Waals forces only. The naphthalene groups protrude above and below the layers of the BaO8 polyhedra and there are voids of ca 208 Å(3) bounded by these groups. No residual electron density was found in this region. The crystal studied was twinned by pseudo-merohedry, with a refined twin component ratio of 0.5261 (1):0.4739 (1).

Related literature

For other compounds based on 1,8-nap ligands, see: Wen et al. (2007 ▶, 2008 ▶); Zhang et al. (2008 ▶); Fu et al. (2011 ▶).

Experimental

Crystal data

[Ba(C12H6O4)(H2O)2]

M = 369.52

Orthorhombic,

a = 8.9643 (11) Å

b = 30.539 (6) Å

c = 8.9625 (12) Å

V = 2453.6 (7) Å3

Z = 8

Mo Kα radiation

μ = 3.25 mm−1

T = 296 K

0.20 × 0.05 × 0.05 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.563, T max = 0.855

7968 measured reflections

1511 independent reflections

1344 reflections with I > 2σ(I)

R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.019

wR(F 2) = 0.043

S = 1.05

1511 reflections

85 parameters

H-atom parameters constrained

Δρmax = 0.54 e Å−3

Δρmin = −0.57 e Å−3

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: Mercury (Macrae et al., 2008 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813006259/su2556sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813006259/su2556Isup2.hkl

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

[Ba(C12H6O4)(H2O)2]	F(000) = 1408
Mr = 369.52	Dx = 2.001 Mg m−3
Orthorhombic, Ibca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2c	Cell parameters from 2836 reflections
a = 8.9643 (11) Å	θ = 2.7–27.1°
b = 30.539 (6) Å	µ = 3.25 mm−1
c = 8.9625 (12) Å	T = 296 K
V = 2453.6 (7) Å3	Prism, colourless
Z = 8	0.20 × 0.05 × 0.05 mm

Bruker APEXII CCD area-detector diffractometer	1511 independent reflections
Radiation source: fine-focus sealed tube	1344 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
Detector resolution: 83.33 pixels mm-1	θmax = 28.4°, θmin = 1.3°
ω scans	h = −11→5
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −40→38
Tmin = 0.563, Tmax = 0.855	l = −11→10
7968 measured reflections

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)] = 0.019	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.043	H-atom parameters constrained
S = 1.05	w = 1/[σ2(Fo2) + (0.0197P)2 + 0.1976P] where P = (Fo2 + 2Fc2)/3
1511 reflections	(Δ/σ)max = 0.001
85 parameters	Δρmax = 0.54 e Å−3
0 restraints	Δρmin = −0.57 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
Ba1	0.61452 (2)	0.0000	0.2500	0.02892 (7)
O1	0.4190 (2)	0.05878 (6)	0.5240 (3)	0.0360 (5)
C1	0.3754 (3)	0.07360 (9)	0.4035 (4)	0.0236 (6)
O2	0.3671 (2)	0.05119 (7)	0.2858 (2)	0.0341 (5)
C2	0.3410 (3)	0.12190 (9)	0.3935 (3)	0.0253 (6)
O3	0.7500	−0.04396 (9)	0.0000	0.0418 (8)
H3	0.7197	−0.0594	−0.0742	0.050*
C3	0.2500	0.14342 (12)	0.5000	0.0239 (8)
C4	0.2500	0.19041 (12)	0.5000	0.0324 (10)
C5	0.3323 (4)	0.21277 (11)	0.3902 (5)	0.0486 (10)
H5	0.3325	0.2432	0.3899	0.058*
C6	0.4105 (4)	0.19121 (11)	0.2860 (4)	0.0527 (10)
H6	0.4610	0.2067	0.2123	0.063*
C7	0.4163 (4)	0.14507 (10)	0.2877 (3)	0.0386 (8)
H7	0.4720	0.1303	0.2160	0.046*

	U11	U22	U33	U12	U13	U23
Ba1	0.01894 (11)	0.03182 (12)	0.03599 (14)	0.000	0.000	0.00999 (13)
O1	0.0321 (12)	0.0315 (11)	0.0445 (13)	0.0027 (9)	−0.0065 (10)	0.0124 (10)
C1	0.0140 (12)	0.0213 (14)	0.0356 (16)	−0.0012 (10)	0.0042 (11)	−0.0009 (12)
O2	0.0330 (11)	0.0314 (11)	0.0380 (14)	−0.0029 (8)	0.0096 (8)	−0.0132 (9)
C2	0.0279 (15)	0.0225 (15)	0.0255 (15)	−0.0033 (12)	−0.0016 (11)	−0.0004 (12)
O3	0.0412 (19)	0.0472 (18)	0.037 (2)	0.000	−0.0162 (15)	0.000
C3	0.025 (2)	0.0220 (19)	0.025 (2)	0.000	−0.0046 (16)	0.000
C4	0.034 (2)	0.022 (2)	0.041 (3)	0.000	−0.0010 (19)	0.000
C5	0.061 (2)	0.0203 (17)	0.065 (3)	−0.0016 (16)	0.0042 (19)	0.0087 (16)
C6	0.067 (2)	0.0326 (18)	0.058 (3)	−0.0034 (16)	0.0213 (19)	0.0164 (15)
C7	0.0463 (18)	0.0366 (17)	0.033 (2)	−0.0007 (14)	0.0128 (13)	0.0060 (13)

Ba1—O1i	2.723 (2)	C2—C7	1.362 (4)
Ba1—O1ii	2.723 (2)	C2—C3	1.417 (3)
Ba1—O2iii	2.7324 (19)	O3—Ba1viii	2.8806 (14)
Ba1—O2	2.7324 (19)	O3—H3	0.8587
Ba1—O2iv	2.7703 (19)	C3—C2ix	1.417 (3)
Ba1—O2v	2.7703 (19)	C3—C4	1.435 (5)
Ba1—O3vi	2.8806 (14)	C4—C5ix	1.407 (4)
Ba1—O3	2.8806 (14)	C4—C5	1.407 (4)
O1—C1	1.234 (4)	C5—C6	1.341 (5)
O1—Ba1ii	2.723 (2)	C5—H5	0.9300
C1—O2	1.259 (4)	C6—C7	1.410 (4)
C1—C2	1.509 (4)	C6—H6	0.9300
O2—Ba1vii	2.7703 (19)	C7—H7	0.9300
O1i—Ba1—O1ii	167.34 (9)	O2iv—Ba1—Ba1vii	144.82 (4)
O1i—Ba1—O2iii	101.55 (6)	O2v—Ba1—Ba1vii	144.82 (4)
O1ii—Ba1—O2iii	67.71 (6)	O3vi—Ba1—Ba1vii	114.937 (13)
O1i—Ba1—O2	67.71 (6)	O3—Ba1—Ba1vii	114.937 (13)
O1ii—Ba1—O2	101.55 (6)	C1iii—Ba1—Ba1vii	50.87 (4)
O2iii—Ba1—O2	71.48 (8)	C1—Ba1—Ba1vii	50.87 (4)
O1i—Ba1—O2iv	68.40 (6)	O1i—Ba1—Ba1iv	96.33 (4)
O1ii—Ba1—O2iv	123.25 (6)	O1ii—Ba1—Ba1iv	96.33 (4)
O2iii—Ba1—O2iv	166.59 (9)	O2iii—Ba1—Ba1iv	144.26 (4)
O2—Ba1—O2iv	110.74 (7)	O2—Ba1—Ba1iv	144.26 (4)
O1i—Ba1—O2v	123.25 (6)	O2iv—Ba1—Ba1iv	35.18 (4)
O1ii—Ba1—O2v	68.40 (6)	O2v—Ba1—Ba1iv	35.18 (4)
O2iii—Ba1—O2v	110.74 (7)	O3vi—Ba1—Ba1iv	65.063 (13)
O2—Ba1—O2v	166.59 (9)	O3—Ba1—Ba1iv	65.063 (13)
O2iv—Ba1—O2v	70.35 (8)	C1iii—Ba1—Ba1iv	129.13 (4)
O1i—Ba1—O3vi	108.54 (7)	C1—Ba1—Ba1iv	129.13 (4)
O1ii—Ba1—O3vi	77.00 (7)	Ba1vii—Ba1—Ba1iv	180.0
O2iii—Ba1—O3vi	134.45 (5)	C1—O1—Ba1ii	149.05 (19)
O2—Ba1—O3vi	89.09 (5)	O1—C1—O2	123.5 (3)
O2iv—Ba1—O3vi	58.83 (5)	O1—C1—C2	118.3 (3)
O2v—Ba1—O3vi	80.11 (6)	O2—C1—C2	118.0 (3)
O1i—Ba1—O3	77.00 (7)	O1—C1—Ba1	84.93 (16)
O1ii—Ba1—O3	108.54 (7)	O2—C1—Ba1	48.58 (13)
O2iii—Ba1—O3	89.09 (5)	C2—C1—Ba1	138.71 (18)
O2—Ba1—O3	134.45 (5)	C1—O2—Ba1	111.20 (16)
O2iv—Ba1—O3	80.11 (6)	C1—O2—Ba1vii	116.85 (16)
O2v—Ba1—O3	58.83 (5)	Ba1—O2—Ba1vii	109.08 (7)
O3vi—Ba1—O3	130.13 (3)	C7—C2—C3	120.9 (3)
O1i—Ba1—C1iii	93.75 (7)	C7—C2—C1	116.6 (3)
O1ii—Ba1—C1iii	78.20 (7)	C3—C2—C1	122.1 (3)
O2iii—Ba1—C1iii	20.22 (6)	Ba1viii—O3—Ba1	124.44 (10)
O2—Ba1—C1iii	85.06 (6)	Ba1viii—O3—H3	77.7
O2iv—Ba1—C1iii	147.38 (7)	Ba1—O3—H3	136.4
O2v—Ba1—C1iii	100.91 (6)	C2—C3—C2ix	124.8 (3)
O3vi—Ba1—C1iii	152.80 (6)	C2—C3—C4	117.62 (17)
O3—Ba1—C1iii	69.07 (6)	C2ix—C3—C4	117.62 (17)
O1i—Ba1—C1	78.20 (7)	C5ix—C4—C5	121.9 (4)
O1ii—Ba1—C1	93.75 (7)	C5ix—C4—C3	119.0 (2)
O2iii—Ba1—C1	85.06 (6)	C5—C4—C3	119.0 (2)
O2—Ba1—C1	20.22 (6)	C6—C5—C4	121.6 (3)
O2iv—Ba1—C1	100.91 (6)	C6—C5—H5	119.2
O2v—Ba1—C1	147.38 (7)	C4—C5—H5	119.2
O3vi—Ba1—C1	69.07 (6)	C5—C6—C7	120.2 (3)
O3—Ba1—C1	152.80 (6)	C5—C6—H6	119.9
C1iii—Ba1—C1	101.74 (9)	C7—C6—H6	119.9
O1i—Ba1—Ba1vii	83.67 (4)	C2—C7—C6	120.5 (3)
O1ii—Ba1—Ba1vii	83.67 (4)	C2—C7—H7	119.7
O2iii—Ba1—Ba1vii	35.74 (4)	C6—C7—H7	119.7
O2—Ba1—Ba1vii	35.74 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O2x	0.86	2.07	2.777 (2)	140

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O2i	0.86	2.07	2.777 (2)	140

Symmetry code: (i) .