Poly[[μ2-aqua-aqua­(μ3-3,5-dinitro­salicylato)barium(II)] monohydrate]

Song, W.-D.; Fan, R.-Z.; Gu, C.-S.; Hao, X.-M.

doi:10.1107/S1600536808006338

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 4| April 2008| Page m551

doi:10.1107/S1600536808006338

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Poly[[μ₂-aqua-aqua(μ₃-3,5-dinitrosalicylato)barium(II)] monohydrate]

Wen-Dong Song,^a ^* Run-Zhen Fan,^a Chang-Sheng Gu ^a and Xiao-Min Hao ^a

^aCollege of Science, Guang Dong Ocean University, Zhanjiang 524088, People's Republic of China
^*Correspondence e-mail: songwd60@126.com

(Received 7 December 2007; accepted 7 March 2008; online 14 March 2008)

In the title coordination polymer, {[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O}_n, the Ba^II atom is ten-coordinated by seven O atoms from four 3,5-dinitrosalicylatate ligands, two μ₂-bridging aqua ligands and one water molecule. The coordination mode is best described as a bicapped square-antiprismatic 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 supramolecular network through intermolecular O—H⋯O hydrogen-bonding interactions between O atoms of 3,5-dinitrosalicylatate ligands and water molecules.

Related literature

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

Experimental

Crystal data

[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O
M_r = 417.49
Monoclinic, P 2₁ /c
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[F² > 2σ(F²)] = 0.026
wR(F²) = 0.067
S = 1.05
2374 reflections
199 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.03 e Å⁻³
Δρ_min = −1.30 e Å⁻³

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⋯N1^iv	0.83 (3)	2.69 (4)	3.340 (4)	137 (4)
O2W—H4W⋯O4^iv	0.83 (3)	2.55 (4)	3.080 (4)	123 (3)
O2W—H4W⋯O5^iv	0.83 (3)	2.25 (3)	2.993 (4)	150 (5)
O2W—H3W⋯O3^v	0.83 (3)	2.01 (2)	2.730 (4)	145 (4)
O1W—H1W⋯O3W^v	0.83 (3)	1.991 (16)	2.798 (4)	164 (4)
O1W—H2W⋯O3W^vi	0.83 (3)	1.90 (3)	2.725 (4)	171 (4)
Symmetry codes: (i) x-1, y, z; (ii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) -x+1, -y+2, -z; (iv) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (v) -x+1, -y+1, -z; (vi) x+1, y-1, z.

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.

Supporting information

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

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

checkCIF report

Comment top

In the structural investigation of 3,5-dinitrosalicylatato complexes, it has been found that the 3,5-dinitrosalicylatato moiety functions as a multidentate ligand (Song et al., 2007) with versatile binding and coordination modes. In this paper, we report the crystal structure of the title compound, (I), a new Ba complex obtained by the reaction of 3,5-dinitrosalicylic acid and barium chloride in alkaline aqueous solution.

As illustrated in Figure 1, the Ba^II atom displays a bicapped square antiprismatic coordination environment, defined by seven O atoms from four 3,5-dinitrosalicylatato ligands, two µ₂-bridging aqua ligands and one water molecule. The 3,5-dinitrosalicylatato ligands link barium ions to form infinite chains, which are further self-assembled into a supramolecular network through intermolecular O—H···O hydrogen bonding interactions (Table 1) involving the uncoordinating water molecules, coordinating water molecules as donors and O atoms of 3,5-dinitrosalicylatato ligands as acceptors (Fig. 2).

Related literature top

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

Experimental top

A mixture of barium chloride (1 mmol), 3,5-dinitrosalicylic acid (1 mmol), NaOH (1.5 mmol) and H₂O (12 ml) was placed in a 23 ml Teflon reactor, which was heated to 433 K for three days and then cooled to room temperature at a rate of 10 K h^-1. The obtained crystals obtained were washed with water and dryed in air.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. The structure of (I), showing the atomic numbering scheme. Non-H atoms are shown with 30% probability displacement ellipsoids.
	Fig. 2. A packing view of the title compound. The intermolecluar hydrogen bonds are shown as dashed lines.

Poly[[µ₂-aqua-aqua(µ₃-3,5-dinitrosalicylato)barium(II)] monohydrate] top

Crystal data top

[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O	F(000) = 800
M_r = 417.49	D_x = 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 = 2.8–27.9°
b = 4.1866 (2) Å	µ = 3.27 mm⁻¹
c = 26.121 (1) Å	T = 296 K
β = 109.332 (3)°	Block, yellow
V = 1234.7 (1) Å³	0.30 × 0.26 × 0.23 mm
Z = 4

Data collection top

Bruker APEXII area-detector diffractometer	2374 independent reflections
Radiation source: fine-focus sealed tube	2189 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.041
ϕ and ω scans	θ_max = 26.0°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→14
T_min = 0.392, T_max = 0.472	k = −4→4
8615 measured reflections	l = −31→32

Refinement top

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.067	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0339P)² + 1.4739P] where P = (F_o² + 2F_c²)/3
2374 reflections	(Δ/σ)_max = 0.001
199 parameters	Δρ_max = 1.03 e Å⁻³
9 restraints	Δρ_min = −1.30 e Å⁻³

Crystal data top

[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O	V = 1234.7 (1) Å³
M_r = 417.49	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.9649 (6) Å	µ = 3.27 mm⁻¹
b = 4.1866 (2) Å	T = 296 K
c = 26.121 (1) Å	0.30 × 0.26 × 0.23 mm
β = 109.332 (3)°

Data collection top

Bruker APEXII area-detector diffractometer	2374 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2189 reflections with I > 2σ(I)
T_min = 0.392, T_max = 0.472	R_int = 0.041
8615 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	9 restraints
wR(F²) = 0.067	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	Δρ_max = 1.03 e Å⁻³
2374 reflections	Δρ_min = −1.30 e Å⁻³
199 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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	4.1866 (2)	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—Ba1^iv	2.706 (2)	C6—C7	1.431 (5)
O2—C1	1.254 (4)	O1W—Ba1^iv	2.966 (3)
O2—Ba1^iv	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—Ba1^iv	130.8 (2)
O1ⁱ—Ba1—O2W	122.52 (7)	Ba1—O1—Ba1^iv	102.07 (8)
O2ⁱ—Ba1—O2W	146.64 (8)	C1—O2—Ba1^iv	134.8 (2)
O1W—Ba1—O2W	71.15 (8)	C1—O2—Ba1ⁱⁱⁱ	99.6 (2)
O3ⁱⁱ—Ba1—O2W	56.60 (7)	Ba1^iv—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—Ba1^iv	93.55 (7)
O1—Ba1—Ba1ⁱ	140.79 (5)	Ba1—O1W—H2W	121 (3)
O1ⁱ—Ba1—Ba1ⁱ	38.72 (5)	Ba1^iv—O1W—H2W	107 (3)
O2ⁱ—Ba1—Ba1ⁱ	86.11 (5)	Ba1—O1W—H1W	113 (3)
O1W—Ba1—Ba1ⁱ	135.00 (5)	Ba1^iv—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)

Symmetry codes: (i) x, y+1, z; (ii) −x+1, −y+1, −z; (iii) −x+1, −y, −z; (iv) x, y−1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3W—H6W···O7^v	0.82 (3)	2.27 (3)	2.916 (4)	135 (4)
O3W—H5W···O5^vi	0.82 (4)	2.60 (4)	2.985 (4)	110 (3)
O3W—H5W···O2W^vii	0.82 (4)	2.04 (3)	2.755 (4)	145 (4)
O2W—H4W···N1^viii	0.83 (3)	2.69 (4)	3.340 (4)	137 (4)
O2W—H4W···O4^viii	0.83 (3)	2.55 (4)	3.080 (4)	123 (3)
O2W—H4W···O5^viii	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)	1.99 (2)	2.798 (4)	164 (4)
O1W—H2W···O3W^ix	0.83 (3)	1.90 (3)	2.725 (4)	171 (4)

Symmetry codes: (ii) −x+1, −y+1, −z; (v) x−1, y, z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x+1, −y+2, −z; (viii) x, −y+1/2, z−1/2; (ix) x+1, y−1, z.

Experimental details

Crystal data
Chemical formula	[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O
M_r	417.49
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	11.9649 (6), 4.1866 (2), 26.121 (1)
β (°)	109.332 (3)
V (Å³)	1234.7 (1)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.27
Crystal size (mm)	0.30 × 0.26 × 0.23

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.392, 0.472
No. of measured, independent and observed [I > 2σ(I)] reflections	8615, 2374, 2189
R_int	0.041
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.067, 1.05
No. of reflections	2374
No. of parameters	199
No. of restraints	9
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.03, −1.30

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

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···N1^iv	0.83 (3)	2.69 (4)	3.340 (4)	137 (4)
O2W—H4W···O4^iv	0.83 (3)	2.55 (4)	3.080 (4)	123 (3)
O2W—H4W···O5^iv	0.83 (3)	2.25 (3)	2.993 (4)	150 (5)
O2W—H3W···O3^v	0.83 (3)	2.01 (2)	2.730 (4)	145 (4)
O1W—H1W···O3W^v	0.83 (3)	1.991 (16)	2.798 (4)	164 (4)
O1W—H2W···O3W^vi	0.83 (3)	1.90 (3)	2.725 (4)	171 (4)

Symmetry codes: (i) x−1, y, z; (ii) −x+1, y+1/2, −z+1/2; (iii) −x+1, −y+2, −z; (iv) x, −y+1/2, z−1/2; (v) −x+1, −y+1, −z; (vi) x+1, y−1, z.

Acknowledgements

The authors acknowledge Guang Dong Ocean University for supporting this work.

References

Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Song, W.-D., Guo, X.-X. & Zhang, C.-H. (2007). Acta Cryst. E63, m399–m401. Web of Science CSD CrossRef IUCr Journals Google Scholar