Potassium aqua-terbium(III) oxalate sulfate.

Single crystals of KTb(C(2)O(4))(SO(4))(H(2)O), potassium aqua-terbium(III) oxalate sulfate, were obtained under hydro-thermal conditions. In the crystal structure, the Tb(III) atom is coordinated by four O atoms from two oxalate anions, three O atoms from three sulfate anions and one O atom from a water mol-ecule within a TbO(8) distorted square antiprismatic coordination. The potassium and terbium(III) atoms are bridged by the oxalate and sulfate groups, forming a three-dimensional structure. The coordination mode of the oxalate has not yet been reported. O-H⋯O hydrogen bonding between the water molecules and the oxygen atoms of oxalate and sulfate anions is also observed.

Related literature

For oxaltes and their coordination modes, see: Audebrand et al. (2003 ▶); Dean et al. (2004 ▶); Lu et al. (2004 ▶).

Experimental

Crystal data

KTb(C2O4)(SO4)(H2O)

M = 400.14

Monoclinic,

a = 6.5274 (13) Å

b = 8.5072 (17) Å

c = 14.591 (4) Å

β = 112.65 (3)°

V = 747.7 (3) Å3

Z = 4

Mo Kα radiation

μ = 10.32 mm−1

T = 113 K

0.06 × 0.04 × 0.02 mm

Data collection

Bruker SMART 1000 CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ▶) T min = 0.576, T max = 0.820

4812 measured reflections

1317 independent reflections

1079 reflections with I > 2σ(I)

R int = 0.057

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.051

S = 1.05

1317 reflections

127 parameters

24 restraints

H-atom parameters constrained

Δρmax = 0.92 e Å−3

Δρmin = −0.78 e Å−3

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2001 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1998 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809019679/br2105sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809019679/br2105Isup2.hkl

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

KTb(C2O4)(SO4)(H2O)	F(000) = 744
Mr = 400.14	Dx = 3.554 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1317 reflections
a = 6.5274 (13) Å	θ = 2.8–27.2°
b = 8.5072 (17) Å	µ = 10.32 mm−1
c = 14.591 (4) Å	T = 113 K
β = 112.65 (3)°	Block, colorless
V = 747.7 (3) Å3	0.06 × 0.04 × 0.02 mm
Z = 4

Bruker SMART 1000 CCD diffractometer	1317 independent reflections
Radiation source: rotating anode	1079 reflections with I > 2σ(I)
confocal	Rint = 0.057
ω scans	θmax = 25.0°, θmin = 2.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −7→7
Tmin = 0.576, Tmax = 0.820	k = −9→10
4812 measured reflections	l = −17→17

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.051	H-atom parameters constrained
S = 1.05	w = 1/[σ2(Fo2) + (0.0171P)2] where P = (Fo2 + 2Fc2)/3
1317 reflections	(Δ/σ)max = 0.001
127 parameters	Δρmax = 0.92 e Å−3
24 restraints	Δρmin = −0.78 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
Tb1	0.33208 (4)	0.24112 (3)	0.086605 (17)	0.00425 (11)
K1	0.9670 (2)	−0.15405 (14)	0.19899 (9)	0.0144 (3)
S1	0.7406 (2)	0.16467 (15)	−0.02448 (9)	0.0057 (3)
O1	0.2682 (6)	0.1255 (4)	0.2251 (3)	0.0079 (8)
O2	0.6044 (6)	0.4446 (4)	0.1557 (2)	0.0074 (8)
O3	0.2189 (6)	0.4466 (4)	0.1717 (2)	0.0079 (8)
O4	0.6523 (6)	0.1083 (4)	0.1984 (3)	0.0065 (8)
O5	0.5568 (7)	0.2364 (4)	−0.0040 (3)	0.0077 (8)
O6	0.7540 (6)	−0.0053 (4)	−0.0015 (3)	0.0080 (8)
O7	0.9493 (7)	0.2388 (4)	0.0409 (3)	0.0096 (9)
O8	0.7035 (7)	0.1876 (5)	−0.1285 (3)	0.0119 (9)
O9	0.1774 (6)	0.4070 (4)	−0.0544 (3)	0.0072 (8)
H9A	0.285 (8)	0.475 (6)	−0.063 (5)	0.04 (2)*
H9B	0.047 (6)	0.448 (9)	−0.107 (5)	0.13 (4)*
C1	0.4137 (9)	0.0364 (6)	0.2801 (4)	0.0043 (11)
C2	0.3644 (9)	0.5312 (6)	0.2329 (4)	0.0052 (11)

	U11	U22	U33	U12	U13	U23
Tb1	0.00438 (17)	0.00457 (17)	0.00411 (16)	0.00031 (11)	0.00197 (12)	0.00024 (10)
K1	0.0141 (8)	0.0162 (7)	0.0164 (7)	−0.0038 (6)	0.0099 (6)	−0.0061 (5)
S1	0.0054 (8)	0.0063 (7)	0.0061 (7)	−0.0002 (6)	0.0029 (6)	−0.0010 (5)
O1	0.006 (2)	0.009 (2)	0.010 (2)	0.0033 (17)	0.0045 (18)	0.0001 (15)
O2	0.010 (2)	0.0070 (19)	0.008 (2)	−0.0028 (17)	0.0067 (18)	−0.0041 (16)
O3	0.008 (2)	0.009 (2)	0.006 (2)	−0.0019 (17)	0.0013 (18)	−0.0020 (15)
O4	0.0068 (12)	0.0062 (11)	0.0066 (11)	−0.0001 (9)	0.0028 (9)	−0.0002 (8)
O5	0.011 (2)	0.0047 (19)	0.013 (2)	0.0011 (16)	0.0096 (18)	−0.0002 (14)
O6	0.011 (2)	0.0035 (19)	0.010 (2)	−0.0010 (17)	0.0048 (17)	−0.0014 (14)
O7	0.008 (2)	0.009 (2)	0.012 (2)	0.0002 (17)	0.0041 (18)	0.0008 (16)
O8	0.016 (3)	0.014 (2)	0.008 (2)	−0.0015 (19)	0.0071 (19)	0.0010 (16)
O9	0.0063 (12)	0.0077 (12)	0.0083 (11)	−0.0003 (9)	0.0036 (9)	0.0017 (8)
C1	0.0048 (14)	0.0036 (14)	0.0043 (13)	0.0005 (9)	0.0015 (10)	−0.0011 (9)
C2	0.0052 (14)	0.0046 (14)	0.0057 (14)	0.0003 (9)	0.0019 (10)	0.0010 (9)

Tb1—O6i	2.311 (4)	S1—O5	1.476 (3)
Tb1—O5	2.323 (3)	S1—O6	1.480 (4)
Tb1—O7ii	2.325 (4)	O1—C1	1.238 (6)
Tb1—O9	2.375 (4)	O1—K1vii	2.900 (3)
Tb1—O4	2.382 (4)	O1—K1ii	3.016 (4)
Tb1—O2	2.406 (4)	O2—C1vii	1.261 (5)
Tb1—O3	2.419 (3)	O2—K1viii	2.909 (4)
Tb1—O1	2.423 (3)	O3—C2	1.250 (6)
K1—O8iii	2.733 (4)	O3—K1vii	2.744 (3)
K1—O3iv	2.744 (3)	O4—C2iv	1.238 (6)
K1—O1iv	2.900 (3)	O4—K1viii	3.105 (4)
K1—O9i	2.903 (4)	O6—Tb1i	2.311 (4)
K1—O2v	2.909 (4)	O7—Tb1vi	2.325 (4)
K1—O6	2.992 (4)	O8—K1iii	2.733 (4)
K1—O1vi	3.016 (4)	O9—K1i	2.903 (4)
K1—O4	3.032 (4)	O9—H9A	0.96 (6)
K1—O4v	3.105 (4)	O9—H9B	0.97 (6)
K1—C2iv	3.132 (5)	C1—O2iv	1.261 (5)
K1—C1vi	3.141 (6)	C1—C2iv	1.532 (7)
K1—S1iii	3.7251 (18)	C2—O4vii	1.238 (6)
S1—O8	1.455 (4)	C2—C1vii	1.532 (7)
S1—O7	1.470 (4)
O6i—Tb1—O5	75.84 (12)	O1vi—K1—O4	80.09 (10)
O6i—Tb1—O7ii	80.00 (13)	O8iii—K1—O4v	60.90 (11)
O5—Tb1—O7ii	132.93 (13)	O3iv—K1—O4v	110.83 (11)
O6i—Tb1—O9	96.65 (12)	O1iv—K1—O4v	80.67 (10)
O5—Tb1—O9	70.62 (12)	O9i—K1—O4v	80.98 (10)
O7ii—Tb1—O9	72.86 (12)	O2v—K1—O4v	57.98 (10)
O5—Tb1—O4	78.58 (12)	O6—K1—O4v	136.94 (9)
O7ii—Tb1—O4	138.98 (12)	O1vi—K1—O4v	95.21 (11)
O9—Tb1—O4	147.42 (11)	O4—K1—O4v	153.72 (5)
O6i—Tb1—O2	146.78 (11)	O8—S1—O7	111.1 (2)
O5—Tb1—O2	74.00 (11)	O8—S1—O5	109.5 (2)
O7ii—Tb1—O2	131.70 (12)	O7—S1—O5	108.3 (2)
O9—Tb1—O2	86.26 (13)	O8—S1—O6	109.8 (2)
O4—Tb1—O2	75.09 (13)	O7—S1—O6	108.2 (2)
O6i—Tb1—O3	147.54 (12)	O5—S1—O6	109.9 (2)
O5—Tb1—O3	133.59 (11)	C1—O1—Tb1	117.0 (3)
O7ii—Tb1—O3	69.30 (12)	C1—O1—K1vii	122.4 (3)
O4—Tb1—O3	110.60 (12)	Tb1—O1—K1vii	110.02 (12)
O2—Tb1—O3	65.64 (12)	C1—O1—K1ii	84.2 (3)
O6i—Tb1—O1	90.64 (12)	Tb1—O1—K1ii	121.87 (14)
O5—Tb1—O1	144.76 (13)	K1vii—O1—K1ii	98.21 (10)
O9—Tb1—O1	144.20 (12)	C1vii—O2—Tb1	119.4 (3)
O4—Tb1—O1	67.90 (12)	C1vii—O2—K1viii	88.6 (3)
O2—Tb1—O1	106.20 (11)	Tb1—O2—K1viii	116.49 (13)
O3—Tb1—O1	71.38 (11)	C2—O3—Tb1	119.0 (3)
O8iii—K1—O3iv	155.77 (13)	C2—O3—K1vii	96.0 (3)
O8iii—K1—O1iv	133.26 (11)	Tb1—O3—K1vii	115.52 (14)
O3iv—K1—O1iv	59.99 (10)	C2iv—O4—Tb1	118.6 (3)
O8iii—K1—O9i	74.43 (11)	C2iv—O4—K1	83.0 (3)
O3iv—K1—O9i	128.67 (11)	Tb1—O4—K1	139.97 (14)
O1iv—K1—O9i	74.15 (10)	C2iv—O4—K1viii	105.0 (3)
O8iii—K1—O2v	68.22 (11)	Tb1—O4—K1viii	110.44 (12)
O3iv—K1—O2v	87.98 (11)	K1—O4—K1viii	93.58 (10)
O1iv—K1—O2v	114.22 (11)	S1—O5—Tb1	149.7 (2)
O9i—K1—O2v	134.04 (11)	S1—O6—Tb1i	138.2 (2)
O8iii—K1—O6	79.21 (11)	S1—O6—K1	126.8 (2)
O3iv—K1—O6	112.22 (11)	Tb1i—O6—K1	94.79 (12)
O1iv—K1—O6	122.12 (12)	S1—O7—Tb1vi	144.5 (2)
O9i—K1—O6	72.82 (10)	S1—O8—K1iii	122.7 (2)
O2v—K1—O6	123.02 (10)	Tb1—O9—K1i	95.73 (12)
O8iii—K1—O1vi	63.92 (11)	Tb1—O9—H9A	113 (4)
O3iv—K1—O1vi	96.12 (11)	K1i—O9—H9A	113 (4)
O1iv—K1—O1vi	151.31 (6)	Tb1—O9—H9B	149 (4)
O9i—K1—O1vi	133.59 (10)	K1i—O9—H9B	75 (6)
O2v—K1—O1vi	44.18 (10)	H9A—O9—H9B	97.7 (13)
O6—K1—O1vi	79.92 (11)	O1—C1—O2iv	126.4 (5)
O8iii—K1—O4	134.96 (11)	O1—C1—C2iv	117.6 (4)
O3iv—K1—O4	45.03 (10)	O2iv—C1—C2iv	116.0 (5)
O1iv—K1—O4	91.10 (10)	O4vii—C2—O3	127.1 (5)
O9i—K1—O4	120.90 (11)	O4vii—C2—C1vii	117.8 (5)
O2v—K1—O4	104.49 (11)	O3—C2—C1vii	115.0 (4)
O6—K1—O4	68.10 (9)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O2ix	0.96 (6)	1.88 (4)	2.731 (4)	145 (5)
O9—H9B···O3x	0.96 (6)	1.86 (3)	2.787 (5)	160 (9)
O9—H9B···O7ix	0.97 (6)	2.83 (9)	3.149 (5)	100 (6)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H9A⋯O2i	0.96 (6)	1.88 (4)	2.731 (4)	145 (5)
O9—H9B⋯O3ii	0.96 (6)	1.86 (3)	2.787 (5)	160 (9)
O9—H9B⋯O7i	0.97 (6)	2.83 (9)	3.149 (5)	100 (6)

Symmetry codes: (i) ; (ii) .