Poly[tetra­aqua­bis(μ-hydrogen maleato)barium(II)]

In the title compound, [Ba(C₄H₃O₄)₂(H₂O)₄]_n, the barium(II) cation is coordinated by five O atoms from four different hydrogen maleate ions and four O atoms from water mol­ecules in a tricapped trigonal prismatic geometry. The coordination polyhedra are connected by edge-sharing to form zigzag chains, which are linked by hydrogen bonds into an extended three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.011 Å
• R factor = 0.037
• wR factor = 0.089
• Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C
ABSTM02_ALERT_3_C  The ratio of Tmax/Tmin expected RT(exp) is > 1.10
            Absorption corrections should be applied.
            Tmin and Tmax expected:      0.697     0.774
            RT(exp) =      1.110
PLAT057_ALERT_3_C Correction for Absorption Required   RT(exp) ...       1.11
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.22 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O6
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Ba1
PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ...         11
PLAT417_ALERT_2_C Short Inter D-H..H-D       H2W1   ..  H4W1    ..       2.14 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          8
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.17 Ratio

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         12

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: TEXRAY (Molecular Structure Corporation, 1999); cell refinement: TEXRAY; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX (McArdle, 1995); software used to prepare material for publication: SHELXL97.

Poly[tetraaquabis(µ-hydrogen maleato)barium(II)]

Crystal data

[Ba(C4H3O4)2(H2O)4]	F(000) = 856
Mr = 439.53	Dx = 2.049 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3263 reflections
a = 6.528 (2) Å	θ = 12–18°
b = 19.009 (7) Å	µ = 2.85 mm^−1
c = 11.493 (5) Å	T = 293 K
β = 92.345 (16)°	Block, colourless
V = 1425.0 (9) Å^3	0.13 × 0.11 × 0.09 mm
Z = 4

Data collection

Rigaku Weissenberg IP diffractometer	3054 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.037
Graphite monochromator	θmax = 27.5°, θmin = 3.1°
ω scans	h = −8→8
13762 measured reflections	k = −24→24
3263 independent reflections	l = −14→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.089	H atoms treated by a mixture of independent and constrained refinement
S = 1.33	w = 1/[σ^2(Fo^2) + (0.0151P)^2 + 5.031P] where P = (Fo^2 + 2Fc^2)/3
3263 reflections	(Δ/σ)max < 0.001
198 parameters	Δρmax = 1.07 e Å^−3
12 restraints	Δρmin = −1.19 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ba1	0.47288 (7)	0.509334 (19)	0.70287 (3)	0.02775 (14)
O1	0.3262 (9)	0.6462 (3)	0.6174 (4)	0.0357 (12)
O7	0.2080 (9)	0.1889 (3)	0.9582 (5)	0.0371 (12)
O4	0.2413 (9)	0.7701 (3)	0.6380 (4)	0.0364 (12)
H4	0.274 (14)	0.7284 (16)	0.635 (8)	0.05 (3)*
O2W	0.8426 (9)	0.4428 (3)	0.7756 (5)	0.0446 (13)
H2W1	0.9294	0.4718	0.8057	0.067*
H2W2	0.8047	0.4132	0.8252	0.067*
O5	0.2934 (10)	0.3125 (3)	0.9505 (5)	0.0403 (13)
H5	0.247 (16)	0.272 (2)	0.953 (9)	0.06 (3)*
O2	0.4084 (9)	0.5743 (3)	0.4768 (5)	0.0392 (12)
O3W	0.1134 (9)	0.4539 (3)	0.5822 (5)	0.0466 (14)
H3W1	0.0160	0.4519	0.6282	0.070*
H3W2	0.1340	0.4134	0.5537	0.070*
O8	0.1973 (9)	0.0993 (3)	0.8355 (6)	0.0472 (14)
O3	0.1832 (10)	0.8608 (3)	0.5241 (5)	0.0463 (14)
O6	0.3577 (11)	0.3908 (3)	0.8162 (6)	0.0550 (17)
O1W	0.6097 (14)	0.5537 (4)	0.9264 (6)	0.077 (2)
H1W1	0.6183	0.5977	0.9425	0.116*
H1W2	0.6441	0.5239	0.9787	0.116*
O4W	0.1388 (10)	0.5530 (4)	0.8273 (7)	0.0604 (18)
H4W1	0.0642	0.5730	0.7799	0.091*
H4W2	0.1291	0.5763	0.8917	0.091*
C1	0.3473 (11)	0.6326 (3)	0.5099 (6)	0.0287 (14)
C2	0.3023 (11)	0.6874 (4)	0.4190 (6)	0.0299 (14)
H2	0.3095	0.6718	0.3426	0.036*
C3	0.2538 (11)	0.7545 (4)	0.4304 (6)	0.0306 (14)
H3	0.2368	0.7788	0.3605	0.037*
C4	0.2220 (11)	0.7978 (4)	0.5357 (6)	0.0316 (15)
C5	0.3050 (11)	0.3314 (4)	0.8430 (7)	0.0336 (15)
C6	0.2560 (13)	0.2799 (4)	0.7488 (6)	0.0384 (17)
H6	0.2503	0.2988	0.6741	0.046*
C7	0.2077 (10)	0.1635 (4)	0.8558 (7)	0.0310 (15)
C8	0.2190 (12)	0.2113 (4)	0.7538 (6)	0.0372 (17)
H8	0.1964	0.1897	0.6819	0.045*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ba1	0.0377 (2)	0.0219 (2)	0.0236 (2)	−0.00063 (17)	−0.00011 (15)	0.00014 (15)
O1	0.050 (3)	0.033 (3)	0.025 (3)	0.005 (2)	0.003 (2)	0.0028 (19)
O7	0.044 (3)	0.038 (3)	0.029 (3)	0.000 (2)	0.003 (2)	0.006 (2)
O4	0.052 (3)	0.033 (3)	0.024 (2)	0.006 (2)	0.003 (2)	−0.002 (2)
O2W	0.051 (3)	0.040 (3)	0.042 (3)	−0.006 (3)	−0.002 (3)	0.008 (2)
O5	0.056 (4)	0.033 (3)	0.031 (3)	−0.004 (3)	0.000 (3)	−0.002 (2)
O2	0.056 (3)	0.030 (3)	0.032 (3)	0.006 (2)	−0.001 (2)	−0.003 (2)
O3W	0.040 (3)	0.062 (4)	0.038 (3)	0.001 (3)	0.005 (3)	−0.010 (3)
O8	0.038 (3)	0.032 (3)	0.072 (4)	−0.001 (2)	0.000 (3)	−0.006 (3)
O3	0.069 (4)	0.030 (3)	0.040 (3)	0.010 (3)	0.001 (3)	−0.002 (2)
O6	0.068 (4)	0.034 (3)	0.062 (4)	−0.007 (3)	−0.002 (3)	0.014 (3)
O1W	0.114 (7)	0.074 (5)	0.043 (4)	−0.010 (5)	−0.008 (4)	−0.022 (3)
O4W	0.047 (4)	0.063 (4)	0.072 (5)	−0.005 (3)	0.011 (3)	−0.027 (4)
C1	0.031 (3)	0.028 (3)	0.026 (3)	−0.002 (3)	−0.003 (3)	0.000 (3)
C2	0.033 (4)	0.035 (4)	0.021 (3)	0.003 (3)	−0.001 (3)	−0.001 (3)
C3	0.038 (4)	0.032 (3)	0.022 (3)	0.001 (3)	−0.001 (3)	0.002 (3)
C4	0.034 (4)	0.031 (3)	0.029 (4)	0.002 (3)	0.000 (3)	−0.002 (3)
C5	0.032 (4)	0.032 (4)	0.036 (4)	0.000 (3)	−0.003 (3)	0.006 (3)
C6	0.044 (4)	0.049 (4)	0.022 (3)	0.000 (4)	0.000 (3)	0.007 (3)
C7	0.020 (3)	0.033 (3)	0.040 (4)	0.002 (3)	0.001 (3)	−0.001 (3)
C8	0.041 (4)	0.048 (4)	0.023 (3)	0.000 (3)	0.000 (3)	−0.006 (3)

Geometric parameters (Å, º)

Ba1—O6	2.725 (6)	O3W—H3W1	0.8445
Ba1—O2^i	2.743 (5)	O3W—H3W2	0.8482
Ba1—O4W	2.783 (6)	O8—C7	1.242 (9)
Ba1—O8^ii	2.799 (6)	O8—Ba1^iii	2.799 (6)
Ba1—O1W	2.815 (7)	O3—C4	1.230 (9)
Ba1—O2W	2.821 (6)	O6—C5	1.223 (9)
Ba1—O3W	2.877 (6)	O1W—H1W1	0.8573
Ba1—O2	2.892 (5)	O1W—H1W2	0.8496
Ba1—O1	2.927 (5)	O4W—H4W1	0.8101
Ba1—C1	3.306 (7)	O4W—H4W2	0.8670
Ba1—Ba1^i	4.704 (2)	C1—C2	1.496 (9)
O1—C1	1.275 (8)	C2—C3	1.322 (10)
O7—C7	1.273 (9)	C2—H2	0.9300
O4—C4	1.290 (9)	C3—C4	1.485 (10)
O4—H4	0.82 (4)	C3—H3	0.9300
O2W—H2W1	0.8540	C5—C6	1.485 (11)
O2W—H2W2	0.8454	C6—C8	1.328 (11)
O5—C5	1.292 (9)	C6—H6	0.9300
O5—H5	0.83 (5)	C7—C8	1.488 (10)
O2—C1	1.241 (8)	C8—H8	0.9300
O2—Ba1^i	2.743 (5)
O6—Ba1—O2^i	88.41 (19)	O3W—Ba1—Ba1^i	65.64 (12)
O6—Ba1—O4W	76.3 (2)	O2—Ba1—Ba1^i	32.42 (10)
O2^i—Ba1—O4W	144.22 (19)	O1—Ba1—Ba1^i	76.77 (10)
O6—Ba1—O8^ii	144.11 (19)	C1—Ba1—Ba1^i	54.21 (12)
O2^i—Ba1—O8^ii	89.59 (18)	C1—O1—Ba1	95.7 (4)
O4W—Ba1—O8^ii	121.51 (18)	C4—O4—H4	112 (7)
O6—Ba1—O1W	84.0 (2)	Ba1—O2W—H2W1	112.1
O2^i—Ba1—O1W	140.5 (2)	Ba1—O2W—H2W2	103.2
O4W—Ba1—O1W	70.6 (2)	H2W1—O2W—H2W2	111.3
O8^ii—Ba1—O1W	75.1 (2)	C5—O5—H5	109 (8)
O6—Ba1—O2W	74.75 (19)	C1—O2—Ba1^i	148.4 (5)
O2^i—Ba1—O2W	72.45 (17)	C1—O2—Ba1	98.2 (4)
O4W—Ba1—O2W	131.3 (2)	Ba1^i—O2—Ba1	113.15 (17)
O8^ii—Ba1—O2W	70.51 (16)	Ba1—O3W—H3W1	109.5
O1W—Ba1—O2W	68.2 (2)	Ba1—O3W—H3W2	112.3
O6—Ba1—O3W	72.0 (2)	H3W1—O3W—H3W2	109.7
O2^i—Ba1—O3W	71.02 (17)	C7—O8—Ba1^iii	126.4 (5)
O4W—Ba1—O3W	73.51 (18)	C5—O6—Ba1	165.9 (6)
O8^ii—Ba1—O3W	139.95 (18)	Ba1—O1W—H1W1	120.3
O1W—Ba1—O3W	140.5 (2)	Ba1—O1W—H1W2	120.7
O2W—Ba1—O3W	130.52 (17)	H1W1—O1W—H1W2	119.0
O6—Ba1—O2	138.60 (19)	Ba1—O4W—H4W1	104.8
O2^i—Ba1—O2	66.85 (17)	Ba1—O4W—H4W2	132.6
O4W—Ba1—O2	104.2 (2)	H4W1—O4W—H4W2	105.8
O8^ii—Ba1—O2	71.45 (18)	O2—C1—O1	121.7 (6)
O1W—Ba1—O2	136.1 (2)	O2—C1—C2	117.6 (6)
O2W—Ba1—O2	123.30 (17)	O1—C1—C2	120.6 (6)
O3W—Ba1—O2	68.75 (17)	O2—C1—Ba1	60.0 (4)
O6—Ba1—O1	143.38 (19)	O1—C1—Ba1	61.8 (4)
O2^i—Ba1—O1	111.17 (15)	C2—C1—Ba1	176.5 (5)
O4W—Ba1—O1	69.82 (19)	C3—C2—C1	130.1 (6)
O8^ii—Ba1—O1	69.34 (16)	C3—C2—H2	115.0
O1W—Ba1—O1	97.3 (2)	C1—C2—H2	115.0
O2W—Ba1—O1	139.63 (16)	C2—C3—C4	131.1 (7)
O3W—Ba1—O1	85.10 (17)	C2—C3—H3	114.4
O2—Ba1—O1	44.38 (14)	C4—C3—H3	114.4
O6—Ba1—C1	147.3 (2)	O3—C4—O4	120.5 (7)
O2^i—Ba1—C1	88.62 (17)	O3—C4—C3	119.1 (7)
O4W—Ba1—C1	87.4 (2)	O4—C4—C3	120.3 (6)
O8^ii—Ba1—C1	68.43 (17)	O6—C5—O5	121.7 (7)
O1W—Ba1—C1	117.4 (2)	O6—C5—C6	118.6 (7)
O2W—Ba1—C1	134.59 (17)	O5—C5—C6	119.7 (6)
O3W—Ba1—C1	76.19 (18)	C8—C6—C5	130.5 (7)
O2—Ba1—C1	21.82 (15)	C8—C6—H6	114.8
O1—Ba1—C1	22.57 (15)	C5—C6—H6	114.8
O6—Ba1—Ba1^i	116.42 (15)	O8—C7—O7	123.0 (7)
O2^i—Ba1—Ba1^i	34.42 (11)	O8—C7—C8	117.2 (7)
O4W—Ba1—Ba1^i	128.62 (16)	O7—C7—C8	119.8 (6)
O8^ii—Ba1—Ba1^i	78.48 (14)	C6—C8—C7	130.6 (7)
O1W—Ba1—Ba1^i	153.31 (18)	C6—C8—H8	114.7
O2W—Ba1—Ba1^i	99.31 (12)	C7—C8—H8	114.7

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y+1/2, −z+3/2; (iii) −x+1, y−1/2, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H4···O1	0.82 (4)	1.61 (4)	2.434 (7)	175 (10)
O2W—H2W1···O4W^iv	0.85	2.07	2.896 (9)	163
O2W—H2W2···O3^iii	0.85	2.00	2.790 (8)	156
O5—H5···O7	0.83 (5)	1.61 (3)	2.416 (8)	168 (12)
O3W—H3W1···O2W^v	0.84	2.08	2.904 (9)	164
O3W—H3W2···O7^vi	0.85	2.30	3.139 (8)	173
O1W—H1W1···O5^vii	0.86	2.17	2.966 (9)	155
O4W—H4W2···O3^viii	0.87	1.96	2.798 (9)	164

Symmetry codes: (iii) −x+1, y−1/2, −z+3/2; (iv) x+1, y, z; (v) x−1, y, z; (vi) x, −y+1/2, z−1/2; (vii) −x+1, −y+1, −z+2; (viii) x, −y+3/2, z+1/2.