Poly[[μ(2)-aqua-aqua-(μ(3)-3,5-dinitro-salicylato)barium(II)] monohydrate].

In the title coordination polymer, {[Ba(C(7)H(2)N(2)O(7))(H(2)O)(2)]·H(2)O}(n), the Ba(II) atom is ten-coordinated by seven O atoms from four 3,5-dinitro-salicylatate ligands, two μ(2)-bridging aqua ligands and one water mol-ecule. The coordination mode is best described as a bicapped square-anti-prismatic geometry. The 3,5-dinitrosalicylatate ligands bridge three Ba atoms. Centrosymmetrically related dinuclear barium units, with a Ba⋯Ba separation of 4.767 (5) Å, form infinite chains, which are further self-assembled into a supra-molecular network through inter-molecular O-H⋯O hydrogen-bonding inter-actions between O atoms of 3,5-dinitro-salicylatate ligands and water mol-ecules.

Related literature

For related literature, see: Song et al. (2007 ▶).

Experimental

Crystal data

[Ba(C7H2N2O7)(H2O)2]·H2O

M = 417.49

Monoclinic,

a = 11.9649 (6) Å

b = 4.1866 (2) Å

c = 26.121 (1) Å

β = 109.332 (3)°

V = 1234.7 (1) Å3

Z = 4

Mo Kα radiation

μ = 3.27 mm−1

T = 296 (2) K

0.30 × 0.26 × 0.23 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.392, T max = 0.471

8615 measured reflections

2374 independent reflections

2189 reflections with I > 2σ(I)

R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 0.067

S = 1.05

2374 reflections

199 parameters

9 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 1.03 e Å−3

Δρmin = −1.30 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808006338/im2052sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808006338/im2052Isup2.hkl

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

[Ba(C7H2N2O7)(H2O)2]·H2O	F000 = 800
Mr = 417.49	Dx = 2.246 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5837 reflections
a = 11.9649 (6) Å	θ = 2.8–27.9º
b = 4.1866 (2) Å	µ = 3.27 mm−1
c = 26.121 (1) Å	T = 296 (2) K
β = 109.332 (3)º	Block, yellow
V = 1234.7 (1) Å3	0.30 × 0.26 × 0.23 mm
Z = 4

Bruker APEXII area-detector diffractometer	2374 independent reflections
Radiation source: fine-focus sealed tube	2189 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.041
T = 296(2) K	θmax = 26.0º
φ and ω scans	θmin = 1.7º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −14→14
Tmin = 0.392, Tmax = 0.472	k = −4→4
8615 measured reflections	l = −31→32

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)] = 0.026	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.067	w = 1/[σ2(Fo2) + (0.0339P)2 + 1.4739P] where P = (Fo2 + 2Fc2)/3
S = 1.05	(Δ/σ)max = 0.001
2374 reflections	Δρmax = 1.03 e Å−3
199 parameters	Δρmin = −1.30 e Å−3
9 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

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	0.698106 (16)	0.59849 (4)	0.002749 (8)	0.01250 (10)
O1	0.7177 (2)	0.1028 (5)	0.06998 (10)	0.0150 (5)
O2	0.5320 (2)	−0.3574 (6)	0.05297 (11)	0.0211 (6)
O3	0.4012 (2)	−0.0694 (6)	0.07602 (11)	0.0190 (6)
O4	0.5934 (3)	0.0066 (8)	0.28282 (12)	0.0311 (7)
O5	0.7491 (3)	0.3054 (8)	0.31157 (12)	0.0359 (7)
O6	0.9954 (3)	0.3764 (8)	0.19294 (14)	0.0416 (9)
O7	0.8915 (2)	0.5460 (7)	0.11347 (12)	0.0251 (6)
N1	0.6755 (3)	0.1544 (8)	0.27501 (14)	0.0245 (7)
N2	0.9007 (3)	0.4015 (7)	0.15565 (14)	0.0205 (7)
C1	0.5067 (3)	−0.1530 (8)	0.08248 (14)	0.0116 (7)
C2	0.6052 (3)	−0.0051 (9)	0.12815 (14)	0.0129 (7)
C3	0.5950 (3)	0.0128 (9)	0.17862 (15)	0.0167 (7)
H3	0.5270	−0.0629	0.1844	0.020*
C4	0.6874 (3)	0.1461 (9)	0.22201 (15)	0.0178 (8)
C5	0.7878 (3)	0.2691 (9)	0.21433 (15)	0.0191 (8)
H5	0.8488	0.3552	0.2431	0.023*
C6	0.7951 (3)	0.2603 (9)	0.16271 (14)	0.0158 (7)
C7	0.7074 (3)	0.1200 (8)	0.11687 (15)	0.0146 (8)
O1W	0.8608 (2)	0.1295 (6)	0.00092 (12)	0.0205 (6)
H2W	0.922 (2)	0.101 (10)	0.0272 (9)	0.031*
H1W	0.881 (3)	0.137 (10)	−0.0265 (9)	0.031*
O2W	0.7483 (2)	0.6467 (6)	−0.09980 (12)	0.0223 (6)
H3W	0.688 (2)	0.758 (8)	−0.1068 (17)	0.033*
H4W	0.732 (3)	0.484 (6)	−0.1189 (16)	0.033*
O3W	0.0565 (2)	0.9715 (8)	0.08622 (12)	0.0255 (6)
H5W	0.110 (3)	1.093 (8)	0.1033 (15)	0.038*
H6W	0.047 (4)	0.837 (8)	0.1074 (13)	0.038*

	U11	U22	U33	U12	U13	U23
Ba1	0.01402 (13)	0.01055 (14)	0.01455 (15)	−0.00009 (7)	0.00690 (10)	−0.00038 (8)
O1	0.0191 (13)	0.0156 (14)	0.0133 (13)	−0.0010 (9)	0.0091 (11)	−0.0007 (10)
O2	0.0199 (13)	0.0222 (15)	0.0235 (15)	−0.0031 (10)	0.0105 (12)	−0.0089 (11)
O3	0.0142 (12)	0.0185 (15)	0.0238 (15)	0.0005 (10)	0.0055 (11)	−0.0015 (11)
O4	0.0331 (16)	0.0413 (17)	0.0244 (16)	−0.0037 (14)	0.0167 (13)	0.0019 (15)
O5	0.0411 (18)	0.0464 (19)	0.0186 (16)	−0.0102 (15)	0.0077 (14)	−0.0100 (15)
O6	0.0227 (16)	0.066 (3)	0.033 (2)	−0.0138 (14)	0.0056 (15)	0.0021 (16)
O7	0.0248 (14)	0.0226 (15)	0.0300 (17)	−0.0044 (11)	0.0117 (12)	0.0052 (13)
N1	0.0296 (18)	0.0263 (18)	0.0184 (18)	0.0037 (14)	0.0089 (15)	−0.0003 (14)
N2	0.0151 (15)	0.0223 (19)	0.0230 (19)	−0.0046 (12)	0.0049 (14)	−0.0040 (14)
C1	0.0132 (16)	0.0130 (18)	0.0082 (17)	−0.0010 (13)	0.0030 (14)	0.0023 (13)
C2	0.0163 (16)	0.0102 (17)	0.0128 (18)	0.0025 (14)	0.0056 (14)	0.0018 (14)
C3	0.0178 (17)	0.0153 (18)	0.0178 (19)	0.0006 (15)	0.0071 (15)	0.0015 (16)
C4	0.0214 (18)	0.021 (2)	0.0116 (18)	0.0022 (14)	0.0060 (15)	−0.0015 (15)
C5	0.0190 (17)	0.018 (2)	0.0166 (19)	−0.0003 (15)	0.0013 (15)	−0.0030 (16)
C6	0.0129 (16)	0.016 (2)	0.0181 (19)	−0.0012 (14)	0.0042 (14)	−0.0002 (15)
C7	0.0184 (18)	0.0121 (19)	0.0146 (19)	0.0044 (13)	0.0074 (15)	0.0040 (13)
O1W	0.0156 (13)	0.0291 (16)	0.0186 (15)	0.0036 (10)	0.0079 (11)	0.0005 (12)
O2W	0.0290 (15)	0.0188 (15)	0.0222 (15)	0.0010 (11)	0.0126 (13)	−0.0019 (11)
O3W	0.0206 (14)	0.0334 (17)	0.0235 (16)	−0.0020 (12)	0.0086 (12)	0.0046 (13)

Ba1—O1	2.678 (2)	O5—N1	1.237 (4)
Ba1—O1i	2.706 (2)	O6—N2	1.230 (5)
Ba1—O2i	2.726 (3)	O7—N2	1.230 (4)
Ba1—O1W	2.777 (3)	N1—C4	1.438 (5)
Ba1—O3ii	2.813 (3)	N2—C6	1.462 (4)
Ba1—O2iii	2.840 (3)	C1—C2	1.505 (5)
Ba1—O2W	2.940 (3)	C1—Ba1iii	3.290 (3)
Ba1—O1Wi	2.966 (3)	C2—C3	1.366 (5)
Ba1—O3iii	2.989 (3)	C2—C7	1.447 (5)
Ba1—O7	3.056 (3)	C3—C4	1.410 (5)
Ba1—C1iii	3.290 (3)	C3—H3	0.9300
Ba1—Ba1i	4.18660 (19)	C4—C5	1.382 (5)
Ba1—H3W	2.90 (5)	C5—C6	1.380 (5)
O1—C7	1.273 (4)	C5—H5	0.9300
O1—Ba1iv	2.706 (2)	C6—C7	1.431 (5)
O2—C1	1.254 (4)	O1W—Ba1iv	2.966 (3)
O2—Ba1iv	2.726 (3)	O1W—H2W	0.83 (4)
O2—Ba1iii	2.840 (3)	O1W—H1W	0.83 (4)
O3—C1	1.266 (4)	O2W—H3W	0.83 (4)
O3—Ba1ii	2.813 (3)	O2W—H4W	0.83 (4)
O3—Ba1iii	2.989 (3)	O3W—H5W	0.82 (4)
O4—N1	1.233 (4)	O3W—H6W	0.83 (4)
O1—Ba1—O1i	102.07 (8)	O7—Ba1—Ba1i	94.12 (5)
O1—Ba1—O2i	69.92 (8)	C1iii—Ba1—Ba1i	124.53 (6)
O1i—Ba1—O2i	63.59 (7)	O1—Ba1—H3W	142.3 (6)
O1—Ba1—O1W	63.49 (7)	O1i—Ba1—H3W	115.3 (6)
O1i—Ba1—O1W	130.70 (8)	O2i—Ba1—H3W	131.3 (3)
O2i—Ba1—O1W	133.10 (8)	O1W—Ba1—H3W	86.9 (3)
O1—Ba1—O3ii	161.23 (8)	O3ii—Ba1—H3W	41.2 (3)
O1i—Ba1—O3ii	81.53 (7)	O2iii—Ba1—H3W	81.9 (7)
O2i—Ba1—O3ii	96.08 (8)	O2W—Ba1—H3W	16.3 (6)
O1W—Ba1—O3ii	127.72 (8)	O1Wi—Ba1—H3W	68.0 (7)
O1—Ba1—O2iii	85.43 (8)	O3iii—Ba1—H3W	67.3 (7)
O1i—Ba1—O2iii	118.10 (7)	O7—Ba1—H3W	136.2 (6)
O2i—Ba1—O2iii	62.17 (9)	C1iii—Ba1—H3W	71.6 (7)
O1W—Ba1—O2iii	107.83 (7)	Ba1i—Ba1—H3W	76.7 (6)
O3ii—Ba1—O2iii	76.78 (8)	C7—O1—Ba1	124.9 (2)
O1—Ba1—O2W	130.60 (7)	C7—O1—Ba1iv	130.8 (2)
O1i—Ba1—O2W	122.52 (7)	Ba1—O1—Ba1iv	102.07 (8)
O2i—Ba1—O2W	146.64 (8)	C1—O2—Ba1iv	134.8 (2)
O1W—Ba1—O2W	71.15 (8)	C1—O2—Ba1iii	99.6 (2)
O3ii—Ba1—O2W	56.60 (7)	Ba1iv—O2—Ba1iii	117.83 (9)
O2iii—Ba1—O2W	90.76 (8)	C1—O3—Ba1ii	116.9 (2)
O1—Ba1—O1Wi	132.52 (7)	C1—O3—Ba1iii	92.2 (2)
O1i—Ba1—O1Wi	60.61 (7)	Ba1ii—O3—Ba1iii	92.33 (8)
O2i—Ba1—O1Wi	122.95 (7)	N2—O7—Ba1	134.3 (2)
O1W—Ba1—O1Wi	93.55 (7)	O4—N1—O5	122.1 (3)
O3ii—Ba1—O1Wi	65.38 (7)	O4—N1—C4	119.0 (3)
O2iii—Ba1—O1Wi	142.04 (8)	O5—N1—C4	118.9 (3)
O2W—Ba1—O1Wi	66.46 (8)	O7—N2—O6	122.5 (3)
O1—Ba1—O3iii	78.80 (7)	O7—N2—C6	119.2 (3)
O1i—Ba1—O3iii	162.60 (7)	O6—N2—C6	118.3 (3)
O2i—Ba1—O3iii	101.22 (7)	O2—C1—O3	122.7 (3)
O1W—Ba1—O3iii	65.50 (7)	O2—C1—C2	118.9 (3)
O3ii—Ba1—O3iii	92.33 (8)	O3—C1—C2	118.5 (3)
O2iii—Ba1—O3iii	44.50 (7)	O2—C1—Ba1iii	58.32 (18)
O2W—Ba1—O3iii	65.05 (7)	O3—C1—Ba1iii	65.18 (18)
O1Wi—Ba1—O3iii	131.14 (7)	C2—C1—Ba1iii	169.1 (2)
O1—Ba1—O7	56.58 (7)	C3—C2—C7	121.9 (3)
O1i—Ba1—O7	64.28 (8)	C3—C2—C1	119.4 (3)
O2i—Ba1—O7	89.64 (8)	C7—C2—C1	118.7 (3)
O1W—Ba1—O7	69.50 (8)	C2—C3—C4	120.0 (3)
O3ii—Ba1—O7	138.31 (7)	C2—C3—H3	120.0
O2iii—Ba1—O7	139.60 (8)	C4—C3—H3	120.0
O2W—Ba1—O7	123.25 (7)	C5—C4—C3	121.3 (3)
O1Wi—Ba1—O7	76.92 (7)	C5—C4—N1	119.9 (3)
O3iii—Ba1—O7	127.03 (7)	C3—C4—N1	118.8 (3)
O1—Ba1—C1iii	83.60 (8)	C6—C5—C4	118.1 (3)
O1i—Ba1—C1iii	140.04 (8)	C6—C5—H5	121.0
O2i—Ba1—C1iii	82.29 (8)	C4—C5—H5	121.0
O1W—Ba1—C1iii	87.53 (8)	C5—C6—C7	124.2 (3)
O3ii—Ba1—C1iii	82.12 (8)	C5—C6—N2	116.7 (3)
O2iii—Ba1—C1iii	22.07 (8)	C7—C6—N2	119.1 (3)
O2W—Ba1—C1iii	75.72 (8)	O1—C7—C6	123.4 (3)
O1Wi—Ba1—C1iii	139.44 (8)	O1—C7—C2	122.2 (3)
O3iii—Ba1—C1iii	22.61 (8)	C6—C7—C2	114.4 (3)
O7—Ba1—C1iii	139.53 (8)	Ba1—O1W—Ba1iv	93.55 (7)
O1—Ba1—Ba1i	140.79 (5)	Ba1—O1W—H2W	121 (3)
O1i—Ba1—Ba1i	38.72 (5)	Ba1iv—O1W—H2W	107 (3)
O2i—Ba1—Ba1i	86.11 (5)	Ba1—O1W—H1W	113 (3)
O1W—Ba1—Ba1i	135.00 (5)	Ba1iv—O1W—H1W	115 (3)
O3ii—Ba1—Ba1i	45.50 (5)	H2W—O1W—H1W	106.4 (17)
O2iii—Ba1—Ba1i	110.82 (5)	Ba1—O2W—H3W	79 (3)
O2W—Ba1—Ba1i	86.06 (5)	Ba1—O2W—H4W	114 (4)
O1Wi—Ba1—Ba1i	41.45 (5)	H3W—O2W—H4W	108 (4)
O3iii—Ba1—Ba1i	137.83 (5)	H5W—O3W—H6W	108 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O3W—H6W···O7v	0.82 (3)	2.27 (3)	2.916 (4)	135 (4)
O3W—H5W···O5vi	0.82 (4)	2.60 (4)	2.985 (4)	110 (3)
O3W—H5W···O2Wvii	0.82 (4)	2.04 (3)	2.755 (4)	145 (4)
O2W—H4W···N1viii	0.83 (3)	2.69 (4)	3.340 (4)	137 (4)
O2W—H4W···O4viii	0.83 (3)	2.55 (4)	3.080 (4)	123 (3)
O2W—H4W···O5viii	0.83 (3)	2.25 (3)	2.993 (4)	150 (5)
O2W—H3W···O3ii	0.83 (3)	2.01 (2)	2.730 (4)	145 (4)
O1W—H1W···O3Wii	0.83 (3)	1.991 (16)	2.798 (4)	164 (4)
O1W—H2W···O3Wix	0.83 (3)	1.90 (3)	2.725 (4)	171 (4)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3W—H6W⋯O7i	0.82 (3)	2.27 (3)	2.916 (4)	135 (4)
O3W—H5W⋯O5ii	0.82 (4)	2.60 (4)	2.985 (4)	110 (3)
O3W—H5W⋯O2Wiii	0.82 (4)	2.04 (3)	2.755 (4)	145 (4)
O2W—H4W⋯N1iv	0.83 (3)	2.69 (4)	3.340 (4)	137 (4)
O2W—H4W⋯O4iv	0.83 (3)	2.55 (4)	3.080 (4)	123 (3)
O2W—H4W⋯O5iv	0.83 (3)	2.25 (3)	2.993 (4)	150 (5)
O2W—H3W⋯O3v	0.83 (3)	2.01 (2)	2.730 (4)	145 (4)
O1W—H1W⋯O3Wv	0.83 (3)	1.991 (16)	2.798 (4)	164 (4)
O1W—H2W⋯O3Wvi	0.83 (3)	1.90 (3)	2.725 (4)	171 (4)

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