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The La atom is ten-coordinate in a capped square–antiprismatic geometry in the title polymeric chain structure, {[La(C6H5N2O2S)3(H2O)2]·3H2O}n. Adjacent chains are linked by hydrogen bonds to give a layer structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805028096/xu6055sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805028096/xu6055Isup2.hkl
Contains datablock I

CCDC reference: 287765

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.044
  • wR factor = 0.110
  • Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT731_ALERT_1_B Bond Calc 0.86(5), Rep 0.850(10) ...... 5.00 su-Rat O4W -H4W2 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat O5W -H5W1 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat O5W -H5W2 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.850(10) ...... 5.00 su-Rat O4W -H8# 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat O5W -H9# 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat O5W -H10# 1.555 1.555
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.56 Ratio PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O2W -H2W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O2W -H2W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.850(10) ...... 4.00 su-Rat O3W -H3W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.850(10) ...... 4.00 su-Rat O3W -H3W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat O4W -H4W1 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(5), Rep 110(2) ...... 2.50 su-Rat H3W1 -O3W -H3W2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 111(5), Rep 110(2) ...... 2.50 su-Rat H5W1 -O5W -H5W2 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O2W -H3# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O2W -H4# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.850(10) ...... 4.00 su-Rat O3W -H5# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.850(10) ...... 4.00 su-Rat O3W -H6# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat O4W -H7# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.92(3), Rep 1.920(10) ...... 3.00 su-Rat H1# -O3W 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.04(5), Rep 2.03(2) ...... 2.50 su-Rat H6# -O3 1.555 3.566 PLAT736_ALERT_1_C H...A Calc 2.08(6), Rep 2.09(2) ...... 3.00 su-Rat H9# -O3W 1.555 3.576 PLAT736_ALERT_1_C H...A Calc 2.07(5), Rep 2.08(2) ...... 2.50 su-Rat H10# -N4 1.555 3.666
0 ALERT level A = In general: serious problem 6 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 26 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

We have reported several metal derivatives of the 4-pyridylthioacetic acid (Fang et al., 2004; Huang, Zhang, Chen & Ng, 2004; Huang, Zhang, Chen, Zhou et al., 2004; Zhang et al., 2003, 2004a,b); the pyridyl N atom in these complexes typically interact through hydrogen bonds. The studies continue with the 2-pyrimidinyl analog of this heteroarylthioacetic acid; few metal derivatives of this carboxylic acid have been reported (Ng et al., 1993; Ma et al., 2004). The present lanthanum(III) derivative, (I), is chelated by the carboxylate portion of the pyrimidin-2-ylsulfanylacetate, but coordination by water molecules as well as two bridging interactions lead to a ten-coordinate environment of the metal atom (Fig. 1). The geometry is better regarded as a capped square–antiprism (Fig. 2); the capping O atoms are farthest away compared with the other eight O atoms that comprise the square–antiprism (Table 1). The compound adopts a chain motif arising from carboxylate bridging (Fig. 3); adjacent chains are linked through hydrogen bonds involving the lattice water molecules (Table 2) in layers.

Experimental top

Pyrimidin-2-ylsulfanylacetic acid (102 mg, 0.6 mmol) was suspended in a small volume of water–ethanol (2:1 (v/v) and ammonium hydroxide was added dropwise until it dissolved completely. Lanthanum nitrate (86 mg, 0.2 mmol) was added and the mixture was transferred into a Teflon-lined Parr bomb. The bomb was heated at 413 K for 100 h. The cooled contents were filtered; colorless plates separated after two weeks. Elemental analysis found (calculated) for C18H25LaN6O11S3: C 29.26 (29.35), H 3.40 (3.42), N 11.32% (11.41%). IR (KBr): 3410, 1601, 1535, 1487, 1426, 622, 550, 472 cm−1. {Bill/David: de we remove the IR data, no assignments]

Refinement top

The methylene and aromatic H atoms were generated geometrically (C—H = 0.97 and 0.93 Å) and were included in the refinement in the riding-model approximation, with Uiso(H) values set at 1.2 times Ueq(C). The water H atoms were located in difference Fourier maps and were refined with distance restraints of O—H = 0.85 (1) Å and H···H = 1.39 (1) Å; their displacement parameters were similarly tied to those of the parent atoms. The final difference Fourier map has a large peak at about 1 Å from atom La1.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. ORTEPII (Johnson, 1976) plot of a portion of the polymeric structure of (I). Displacement ellipsoids are drawn at the 50% probability level and H atoms as spheres of arbitrary radii. [Symmetry codes: (i) 1 − x, 1 − y, 1 − z; (ii) −x, 1 − y, 1 − z.]
[Figure 2] Fig. 2. ORTEPII (Johnson, 1976) plot of the capped square–antiprismatic geometry of La in (I). [Symmetry codes: (i) 1 − x, 1 − y, 1 − z; (ii) −x, 1 − y, 1 − z.]
[Figure 3] Fig. 3. ORTEPII (Johnson, 1976) of the chain structure. The lattice water molecules have been omitted.
catena-Poly[[[diaqua(pyrimidin-2-ylsulfanylacetato)lanthanum(III)]-di- µ-pyrimidin-2-ylsulfanylacetato] trihydrate] top
Crystal data top
[La(C6H5N2O2S)3(H2O)2]·3H2OF(000) = 1472
Mr = 736.53Dx = 1.827 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7684 reflections
a = 8.8145 (3) Åθ = 2.3–28.6°
b = 11.8211 (5) ŵ = 1.90 mm1
c = 25.887 (1) ÅT = 295 K
β = 97.046 (1)°Block, colorless
V = 2677.0 (2) Å30.50 × 0.22 × 0.14 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
6110 independent reflections
Radiation source: fine-focus sealed tube5749 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
ϕ and ω scansθmax = 27.5°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 911
Tmin = 0.504, Tmax = 0.777k = 1512
15909 measured reflectionsl = 3332
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.110H atoms treated by a mixture of independent and constrained refinement
S = 1.16 w = 1/[σ2(Fo2) + (0.0499P)2 + 4.1463P]
where P = (Fo2 + 2Fc2)/3
6110 reflections(Δ/σ)max = 0.001
382 parametersΔρmax = 1.19 e Å3
15 restraintsΔρmin = 0.75 e Å3
Crystal data top
[La(C6H5N2O2S)3(H2O)2]·3H2OV = 2677.0 (2) Å3
Mr = 736.53Z = 4
Monoclinic, P21/cMo Kα radiation
a = 8.8145 (3) ŵ = 1.90 mm1
b = 11.8211 (5) ÅT = 295 K
c = 25.887 (1) Å0.50 × 0.22 × 0.14 mm
β = 97.046 (1)°
Data collection top
Bruker APEX area-detector
diffractometer
6110 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5749 reflections with I > 2σ(I)
Tmin = 0.504, Tmax = 0.777Rint = 0.029
15909 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04415 restraints
wR(F2) = 0.110H atoms treated by a mixture of independent and constrained refinement
S = 1.16Δρmax = 1.19 e Å3
6110 reflectionsΔρmin = 0.75 e Å3
382 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
La10.24487 (2)0.48747 (2)0.49842 (1)0.0217 (1)
S10.5311 (2)0.3943 (1)0.69500 (4)0.0470 (3)
S20.4673 (2)0.0804 (1)0.55240 (5)0.0476 (3)
S30.0317 (2)0.2167 (1)0.34125 (4)0.0404 (3)
O10.3454 (3)0.4736 (3)0.5965 (1)0.035 (1)
O20.5419 (3)0.4989 (2)0.5547 (1)0.031 (1)
O30.1503 (3)0.3031 (2)0.5376 (1)0.035 (1)
O40.3790 (3)0.2962 (2)0.5139 (1)0.035 (1)
O50.0392 (3)0.4333 (2)0.4558 (1)0.026 (1)
O60.1484 (3)0.3640 (3)0.4188 (1)0.035 (1)
O1w0.3398 (3)0.6877 (3)0.5214 (1)0.037 (1)
O2w0.1468 (3)0.6245 (3)0.4276 (1)0.038 (1)
O3w0.0981 (4)0.8355 (3)0.5042 (1)0.050 (1)
O4w0.0958 (4)0.5996 (3)0.3534 (1)0.049 (1)
O5w0.1230 (6)1.0288 (4)0.4489 (2)0.077 (1)
N10.7112 (5)0.2556 (4)0.6491 (2)0.046 (1)
N20.6024 (5)0.1919 (4)0.7227 (2)0.058 (1)
N30.3869 (4)0.0388 (3)0.6313 (1)0.035 (1)
N40.5952 (4)0.1016 (3)0.5896 (1)0.040 (1)
N50.0257 (4)0.4134 (3)0.2969 (1)0.037 (1)
N60.1111 (5)0.2424 (4)0.2629 (2)0.053 (1)
C10.4845 (4)0.4851 (3)0.5959 (1)0.025 (1)
C20.5888 (5)0.4845 (4)0.6462 (2)0.035 (1)
C30.6261 (5)0.2679 (4)0.6867 (2)0.037 (1)
C40.7790 (7)0.1555 (5)0.6472 (2)0.060 (1)
C50.7640 (7)0.0724 (5)0.6819 (2)0.060 (1)
C60.6737 (7)0.0952 (5)0.7191 (2)0.065 (2)
C70.2768 (4)0.2565 (3)0.5380 (2)0.031 (1)
C80.3067 (5)0.1532 (4)0.5705 (2)0.041 (1)
C90.4812 (5)0.0313 (3)0.5962 (2)0.032 (1)
C100.4121 (5)0.1244 (4)0.6640 (2)0.039 (1)
C110.5247 (6)0.2007 (4)0.6611 (2)0.040 (1)
C120.6136 (5)0.1871 (4)0.6220 (2)0.043 (1)
C130.0111 (4)0.3731 (3)0.4219 (1)0.025 (1)
C140.1050 (5)0.3133 (4)0.3845 (2)0.034 (1)
C150.0412 (5)0.3026 (4)0.2959 (2)0.035 (1)
C160.0885 (6)0.4681 (5)0.2604 (2)0.049 (1)
C170.1640 (7)0.4162 (5)0.2243 (2)0.056 (1)
C180.1719 (7)0.3016 (5)0.2273 (2)0.059 (2)
H1w10.275 (3)0.740 (3)0.512 (2)0.044*
H1w20.425 (2)0.707 (3)0.512 (2)0.044*
H2w10.211 (3)0.656 (4)0.410 (1)0.045*
H2w20.064 (3)0.612 (4)0.408 (1)0.045*
H3w10.117 (6)0.890 (3)0.485 (2)0.059*
H3w20.041 (6)0.788 (3)0.487 (2)0.059*
H4w10.184 (3)0.588 (4)0.363 (2)0.059*
H4w20.082 (5)0.553 (4)0.329 (2)0.059*
H5w10.064 (6)1.080 (4)0.458 (3)0.092*
H5w20.203 (4)1.058 (5)0.439 (3)0.092*
H2a0.59670.56110.65970.041*
H2b0.69000.46160.63910.041*
H40.83930.14220.62070.072*
H50.81330.00320.68030.072*
H60.66120.03920.74340.078*
H8a0.21790.10410.56590.049*
H8b0.32540.17430.60690.049*
H100.34960.13250.69020.046*
H110.54090.26010.68470.048*
H120.68940.24010.61820.052*
H14a0.16510.36980.36400.041*
H14b0.17360.27250.40440.041*
H160.08050.54660.25930.059*
H170.20760.45670.19910.067*
H180.22240.26300.20310.071*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.0157 (1)0.0270 (1)0.0231 (1)0.0040 (1)0.0054 (1)0.0029 (1)
S10.0490 (7)0.0660 (8)0.0281 (5)0.0167 (6)0.0127 (5)0.0101 (5)
S20.0511 (7)0.0480 (7)0.0480 (7)0.0256 (6)0.0237 (5)0.0187 (5)
S30.0508 (7)0.0374 (6)0.0350 (5)0.0092 (5)0.0135 (5)0.0091 (4)
O10.022 (1)0.057 (2)0.028 (1)0.003 (1)0.008 (1)0.006 (1)
O20.023 (1)0.043 (2)0.027 (1)0.003 (1)0.010 (1)0.004 (1)
O30.023 (1)0.034 (2)0.050 (2)0.007 (1)0.009 (1)0.010 (1)
O40.028 (2)0.034 (2)0.047 (2)0.008 (1)0.013 (1)0.008 (1)
O50.021 (1)0.031 (1)0.026 (1)0.004 (1)0.008 (1)0.002 (1)
O60.022 (1)0.046 (2)0.037 (2)0.004 (1)0.008 (1)0.012 (1)
O1w0.022 (1)0.034 (2)0.056 (2)0.002 (1)0.011 (1)0.001 (1)
O2w0.028 (2)0.048 (2)0.037 (2)0.004 (1)0.004 (1)0.014 (1)
O3w0.043 (2)0.035 (2)0.071 (2)0.000 (2)0.013 (2)0.006 (2)
O4w0.047 (2)0.063 (2)0.040 (2)0.004 (2)0.015 (2)0.006 (2)
O5w0.073 (3)0.066 (3)0.101 (4)0.012 (2)0.048 (3)0.023 (3)
N10.051 (2)0.047 (2)0.041 (2)0.006 (2)0.014 (2)0.005 (2)
N20.058 (3)0.068 (3)0.050 (2)0.003 (2)0.013 (2)0.019 (2)
N30.032 (2)0.036 (2)0.038 (2)0.007 (2)0.009 (2)0.005 (2)
N40.044 (2)0.038 (2)0.041 (2)0.017 (2)0.014 (2)0.007 (2)
N50.037 (2)0.042 (2)0.033 (2)0.003 (2)0.006 (2)0.002 (2)
N60.067 (3)0.049 (2)0.047 (2)0.005 (2)0.028 (2)0.013 (2)
C10.025 (2)0.026 (2)0.026 (2)0.0049 (14)0.007 (2)0.000 (1)
C20.036 (2)0.039 (2)0.027 (2)0.002 (2)0.000 (2)0.001 (2)
C30.032 (2)0.047 (3)0.030 (2)0.005 (2)0.002 (2)0.006 (2)
C40.072 (4)0.056 (3)0.057 (3)0.009 (3)0.023 (3)0.000 (3)
C50.064 (4)0.047 (3)0.067 (4)0.004 (3)0.003 (3)0.002 (3)
C60.073 (4)0.053 (3)0.066 (4)0.007 (3)0.003 (3)0.022 (3)
C70.025 (2)0.030 (2)0.038 (2)0.002 (2)0.004 (2)0.002 (2)
C80.038 (2)0.040 (2)0.046 (2)0.015 (2)0.018 (2)0.013 (2)
C90.037 (2)0.029 (2)0.032 (2)0.008 (2)0.007 (2)0.000 (2)
C100.035 (2)0.043 (2)0.039 (2)0.001 (2)0.009 (2)0.006 (2)
C110.051 (3)0.034 (2)0.035 (2)0.008 (2)0.005 (2)0.008 (2)
C120.043 (3)0.038 (2)0.050 (3)0.019 (2)0.008 (2)0.003 (2)
C130.025 (2)0.026 (2)0.026 (2)0.004 (1)0.007 (1)0.002 (1)
C140.027 (2)0.046 (2)0.031 (2)0.006 (2)0.007 (2)0.008 (2)
C150.033 (2)0.044 (2)0.027 (2)0.004 (2)0.003 (2)0.009 (2)
C160.057 (3)0.046 (3)0.044 (3)0.007 (2)0.005 (2)0.000 (2)
C170.062 (3)0.067 (4)0.043 (3)0.023 (3)0.021 (2)0.001 (2)
C180.064 (4)0.075 (4)0.045 (3)0.009 (3)0.030 (3)0.016 (3)
Geometric parameters (Å, º) top
La1—O12.590 (3)N2—C61.314 (8)
La1—O22.838 (3)N2—C31.329 (6)
La1—O2i2.466 (3)N3—C91.309 (5)
La1—O32.584 (3)N3—C101.319 (5)
La1—O42.560 (3)N4—C121.311 (6)
La1—O52.687 (3)N4—C91.331 (5)
La1—O5ii2.469 (2)N5—C151.317 (6)
La1—O62.583 (3)N5—C161.323 (6)
La1—O1w2.556 (3)N6—C151.322 (5)
La1—O2w2.518 (3)N6—C181.321 (7)
S1—C31.740 (5)C1—C21.498 (5)
S1—C21.775 (4)C4—C51.349 (8)
S2—C91.734 (4)C5—C61.348 (9)
S2—C81.769 (4)C7—C81.488 (6)
S3—C151.734 (4)C10—C111.351 (6)
S3—C141.776 (4)C11—C121.362 (6)
O1—C11.236 (5)C13—C141.496 (5)
O2—C11.247 (5)C16—C171.358 (7)
O3—C71.243 (5)C17—C181.359 (8)
O4—C71.249 (5)C2—H2a0.97
O5—C131.254 (4)C2—H2b0.97
O6—C131.227 (4)C4—H40.93
O1w—H1w10.85 (1)C5—H50.93
O1w—H1w20.85 (1)C6—H60.93
O2w—H2w10.85 (1)C8—H8a0.97
O2w—H2w20.85 (1)C8—H8b0.97
O3w—H3w10.85 (1)C10—H100.93
O3w—H3w20.85 (1)C11—H110.93
O4w—H4w10.85 (1)C12—H120.93
O4w—H4w20.85 (1)C14—H14a0.97
O5w—H5w10.85 (1)C14—H14b0.97
O5w—H5w20.85 (1)C16—H160.93
N1—C31.308 (6)C17—H170.93
N1—C41.329 (7)C18—H180.93
O1—La1—O246.9 (1)N1—C3—N2126.9 (5)
O1—La1—O2i111.0 (1)N1—C3—S1121.1 (3)
O1—La1—O369.5 (1)N2—C3—S1112.0 (4)
O1—La1—O472.2 (1)N1—C4—C5122.8 (5)
O1—La1—O5125.2 (1)C4—C5—C6116.4 (6)
O1—La1—O5ii74.7 (1)N2—C6—C5123.6 (5)
O1—La1—O6141.8 (1)O4—C7—O3122.1 (4)
O1—La1—O1w76.6 (1)O4—C7—C8120.1 (4)
O1—La1—O2w143.1 (1)O3—C7—C8117.7 (4)
O2—La1—O2i64.2 (1)C7—C8—S2110.0 (3)
O2—La1—O399.2 (1)N3—C9—N4126.9 (4)
O2—La1—O465.3 (1)N3—C9—S2120.4 (3)
O2—La1—O5167.5 (1)N4—C9—S2112.7 (3)
O2—La1—O5ii114.9 (1)N3—C10—C11123.0 (4)
O2—La1—O6129.0 (1)C10—C11—C12117.1 (4)
O2—La1—O1w65.3 (1)N4—C12—C11121.9 (4)
O2—La1—O2w123.8 (1)O6—C13—O5122.1 (4)
O2i—La1—O3125.35 (1)O6—C13—C14121.3 (3)
O2i—La1—O477.1 (1)O5—C13—C14116.6 (3)
O2i—La1—O5ii153.8 (1)C13—C14—S3116.0 (3)
O2i—La1—O5121.5 (1)N5—C15—N6127.3 (4)
O2i—La1—O677.9 (1)N5—C15—S3121.3 (3)
O2i—La1—O1w79.6 (1)N6—C15—S3111.3 (4)
O2i—La1—O2w76.7 (1)N5—C16—C17123.6 (5)
O3—La1—O450.1 (1)C16—C17—C18116.0 (5)
O3—La1—O568.3 (1)N6—C18—C17123.0 (5)
O3—La1—O5ii80.8 (1)La1—O1w—H1w1114 (3)
O3—La1—O675.3 (1)La1—O1w—H1w2117 (3)
O3—La1—O1w143.3 (1)H1w1—O1w—H1w2109 (2)
O3—La1—O2w136.8 (1)La1—O2w—H2w1118 (3)
O4—La1—O5104.1 (1)La1—O2w—H2w2121 (3)
O4—La1—O5ii127.8 (1)H2w1—O2w—H2w2110 (2)
O4—La1—O674.1 (1)H3w1—O3w—H3w2110 (2)
O4—La1—O1w130.5 (1)H4w1—O4w—H4w2109 (2)
O4—La1—O2w142.4 (1)H5w1—O5w—H5w2110 (2)
O5—La1—O5ii65.5 (1)C1—C2—H2a108.5
O5—La1—O648.6 (1)S1—C2—H2a108.5
O5—La1—O1w125.3 (1)C1—C2—H2b108.5
O5—La1—O2w68.6 (1)S1—C2—H2b108.5
O5ii—La1—O6114.1 (1)H2a—C2—H2b107.5
O5ii—La1—O1w77.0 (1)N1—C4—H4118.6
O5ii—La1—O2w84.2 (1)C5—C4—H4118.6
O6—La1—O1w140.8 (1)C4—C5—H5121.8
O6—La1—O2w74.5 (1)C6—C5—H5121.8
O1w—La1—O2w69.3 (1)N2—C6—H6118.2
C3—S1—C2104.1 (2)C5—C6—H6118.2
C9—S2—C8101.1 (2)C7—C8—H8a109.7
C15—S3—C14104.1 (2)S2—C8—H8a109.7
C1—O1—La1101.6 (2)C7—C8—H8b109.7
C1—O2—La1i154.5 (3)S2—C8—H8b109.7
C1—O2—La189.3 (2)H8a—C8—H8b108.2
La1i—O2—La1115.82 (10)N3—C10—H10118.5
C7—O3—La192.6 (2)C11—C10—H10118.5
C7—O4—La193.6 (2)C10—C11—H11121.4
C13—O5—La1ii153.6 (2)C12—C11—H11121.4
C13—O5—La191.8 (2)N4—C12—H12119.0
La1ii—O5—La1114.49 (9)C11—C12—H12119.0
C13—O6—La197.5 (2)C13—C14—H14a108.3
C3—N1—C4115.4 (4)S3—C14—H14a108.3
C6—N2—C3114.8 (5)C13—C14—H14b108.3
C9—N3—C10115.2 (4)S3—C14—H14b108.3
C12—N4—C9115.8 (4)H14a—C14—H14b107.4
C15—N5—C16114.8 (4)N5—C16—H16118.2
C15—N6—C18115.3 (5)C17—C16—H16118.2
O1—C1—O2122.2 (4)C16—C17—H17122.0
O1—C1—C2119.5 (4)C18—C17—H17122.0
O2—C1—C2118.3 (4)N6—C18—H18118.5
C1—C2—S1115.0 (3)C17—C18—H18118.5
O2i—La1—O1—C14.6 (3)O2w—La1—O6—C1376.2 (2)
O5ii—La1—O1—C1148.5 (3)O1w—La1—O6—C1399.3 (3)
O2w—La1—O1—C191.2 (3)O4—La1—O6—C13124.7 (3)
O1w—La1—O1—C168.5 (2)O3—La1—O6—C1372.6 (2)
O4—La1—O1—C172.6 (2)O1—La1—O6—C1395.8 (3)
O3—La1—O1—C1125.8 (3)O5—La1—O6—C131.3 (2)
O6—La1—O1—C1101.8 (3)O2—La1—O6—C13162.6 (2)
O5—La1—O1—C1167.5 (2)La1—O1—C1—O20.1 (4)
O2—La1—O1—C10.1 (2)La1—O1—C1—C2178.9 (3)
O2i—La1—O2—C1175.4 (3)La1i—O2—C1—O1170.2 (4)
O5ii—La1—O2—C133.7 (2)La1—O2—C1—O10.1 (4)
O2w—La1—O2—C1133.8 (2)La1i—O2—C1—C210.8 (8)
O1w—La1—O2—C194.6 (2)La1—O2—C1—C2178.9 (3)
O4—La1—O2—C188.3 (2)O1—C1—C2—S133.9 (5)
O3—La1—O2—C150.5 (2)O2—C1—C2—S1147.1 (3)
O6—La1—O2—C1129.0 (2)C3—S1—C2—C193.1 (3)
O1—La1—O2—C10.0 (2)C4—N1—C3—N20.7 (7)
O5—La1—O2—C155.3 (4)C4—N1—C3—S1179.4 (4)
O5ii—La1—O2—La1i151.0 (1)C6—N2—C3—N10.0 (8)
O2w—La1—O2—La1i50.9 (2)C6—N2—C3—S1178.8 (4)
O1w—La1—O2—La1i90.1 (1)C2—S1—C3—N12.7 (4)
O4—La1—O2—La1i87.1 (1)C2—S1—C3—N2176.2 (3)
O3—La1—O2—La1i124.9 (1)C3—N1—C4—C51.1 (8)
O6—La1—O2—La1i46.4 (2)N1—C4—C5—C60.9 (9)
O1—La1—O2—La1i175.3 (2)C3—N2—C6—C50.3 (9)
O5—La1—O2—La1i120.0 (3)C4—C5—C6—N20.2 (9)
O2i—La1—O3—C725.3 (3)La1—O4—C7—O313.4 (4)
O5ii—La1—O3—C7153.4 (3)La1—O4—C7—C8163.7 (4)
O2w—La1—O3—C7135.4 (2)La1—O3—C7—O413.3 (4)
O1w—La1—O3—C7100.1 (3)La1—O3—C7—C8163.9 (3)
O4—La1—O3—C77.1 (2)O4—C7—C8—S218.4 (5)
O6—La1—O3—C788.5 (2)O3—C7—C8—S2164.4 (3)
O1—La1—O3—C776.4 (2)C9—S2—C8—C7178.3 (3)
O5—La1—O3—C7139.4 (3)C10—N3—C9—N41.6 (7)
O2—La1—O3—C739.5 (3)C10—N3—C9—S2177.2 (3)
O2i—La1—O4—C7171.9 (3)C12—N4—C9—N30.2 (7)
O5ii—La1—O4—C717.5 (3)C12—N4—C9—S2179.0 (4)
O2w—La1—O4—C7125.3 (2)C8—S2—C9—N32.2 (4)
O1w—La1—O4—C7124.3 (2)C8—S2—C9—N4178.8 (4)
O3—La1—O4—C77.1 (2)C9—N3—C10—C111.4 (7)
O6—La1—O4—C791.0 (2)N3—C10—C11—C120.5 (7)
O1—La1—O4—C770.8 (2)C9—N4—C12—C112.3 (7)
O5—La1—O4—C752.2 (3)C10—C11—C12—N42.5 (7)
O2—La1—O4—C7120.8 (3)La1—O6—C13—O52.5 (4)
O2i—La1—O5—C1331.2 (2)La1—O6—C13—C14178.3 (3)
O5ii—La1—O5—C13177.5 (3)La1ii—O5—C13—O6177.3 (4)
O2w—La1—O5—C1389.1 (2)La1—O5—C13—O62.4 (4)
O1w—La1—O5—C13131.2 (2)La1ii—O5—C13—C143.4 (7)
O4—La1—O5—C1352.1 (2)La1—O5—C13—C14178.4 (3)
O3—La1—O5—C1388.0 (2)O6—C13—C14—S37.3 (5)
O6—La1—O5—C131.3 (2)O5—C13—C14—S3173.4 (3)
O1—La1—O5—C13130.1 (2)C15—S3—C14—C1374.9 (4)
O2—La1—O5—C1382.8 (4)C16—N5—C15—N60.1 (7)
O2i—La1—O5—La1ii151.3 (1)C16—N5—C15—S3179.2 (3)
O2w—La1—O5—La1ii93.4 (1)C18—N6—C15—N50.2 (7)
O1w—La1—O5—La1ii51.3 (2)C18—N6—C15—S3179.2 (4)
O4—La1—O5—La1ii125.4 (1)C14—S3—C15—N54.2 (4)
O3—La1—O5—La1ii89.6 (1)C14—S3—C15—N6175.2 (3)
O6—La1—O5—La1ii178.8 (2)C15—N5—C16—C170.2 (7)
O1—La1—O5—La1ii47.5 (2)N5—C16—C17—C180.3 (9)
O2—La1—O5—La1ii94.8 (3)C15—N6—C18—C170.0 (8)
O2i—La1—O6—C13155.6 (3)C16—C17—C18—N60.2 (9)
O5ii—La1—O6—C130.1 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O3w0.85 (1)1.92 (1)2.749 (5)165 (4)
O1w—H1w2···O4i0.85 (1)1.93 (2)2.751 (4)164 (4)
O2w—H2w1···N1i0.85 (1)2.05 (2)2.852 (5)158 (4)
O2w—H2w2···O4w0.85 (1)1.88 (2)2.709 (5)167 (4)
O3w—H3w1···O5w0.85 (1)1.89 (2)2.718 (5)166 (6)
O3w—H3w2···O3ii0.85 (1)2.03 (2)2.840 (5)158 (5)
O4w—H4w1···O1ii0.85 (1)2.01 (2)2.823 (4)160 (5)
O4w—H4w2···N50.85 (1)2.13 (3)2.918 (5)154 (5)
O5w—H5w1···O3wiii0.85 (1)2.09 (2)2.903 (6)162 (6)
O5w—H5w2···N4i0.85 (1)2.08 (2)2.918 (6)169 (6)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y+2, z+1.

Experimental details

Crystal data
Chemical formula[La(C6H5N2O2S)3(H2O)2]·3H2O
Mr736.53
Crystal system, space groupMonoclinic, P21/c
Temperature (K)295
a, b, c (Å)8.8145 (3), 11.8211 (5), 25.887 (1)
β (°) 97.046 (1)
V3)2677.0 (2)
Z4
Radiation typeMo Kα
µ (mm1)1.90
Crystal size (mm)0.50 × 0.22 × 0.14
Data collection
DiffractometerBruker APEX area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.504, 0.777
No. of measured, independent and
observed [I > 2σ(I)] reflections
15909, 6110, 5749
Rint0.029
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.110, 1.16
No. of reflections6110
No. of parameters382
No. of restraints15
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.19, 0.75

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
La1—O12.590 (3)La1—O52.687 (3)
La1—O22.838 (3)La1—O5ii2.469 (2)
La1—O2i2.466 (3)La1—O62.583 (3)
La1—O32.584 (3)La1—O1w2.556 (3)
La1—O42.560 (3)La1—O2w2.518 (3)
O1—La1—O246.9 (1)O2i—La1—O2w76.7 (1)
O1—La1—O2i111.0 (1)O3—La1—O450.1 (1)
O1—La1—O369.5 (1)O3—La1—O568.3 (1)
O1—La1—O472.2 (1)O3—La1—O5ii80.8 (1)
O1—La1—O5125.2 (1)O3—La1—O675.3 (1)
O1—La1—O5ii74.7 (1)O3—La1—O1w143.3 (1)
O1—La1—O6141.8 (1)O3—La1—O2w136.8 (1)
O1—La1—O1w76.6 (1)O4—La1—O5104.1 (1)
O1—La1—O2w143.1 (1)O4—La1—O5ii127.8 (1)
O2—La1—O2i64.2 (1)O4—La1—O674.1 (1)
O2—La1—O399.2 (1)O4—La1—O1w130.5 (1)
O2—La1—O465.3 (1)O4—La1—O2w142.4 (1)
O2—La1—O5167.5 (1)O5—La1—O5ii65.5 (1)
O2—La1—O5ii114.9 (1)O5—La1—O648.6 (1)
O2—La1—O6129.0 (1)O5—La1—O1w125.3 (1)
O2—La1—O1w65.3 (1)O5—La1—O2w68.6 (1)
O2—La1—O2w123.8 (1)O5ii—La1—O6114.1 (1)
O2i—La1—O3125.35 (1)O5ii—La1—O1w77.0 (1)
O2i—La1—O477.1 (1)O5ii—La1—O2w84.2 (1)
O2i—La1—O5ii153.8 (1)O6—La1—O1w140.8 (1)
O2i—La1—O5121.5 (1)O6—La1—O2w74.5 (1)
O2i—La1—O677.9 (1)O1w—La1—O2w69.3 (1)
O2i—La1—O1w79.6 (1)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O3w0.85 (1)1.92 (1)2.749 (5)165 (4)
O1w—H1w2···O4i0.85 (1)1.93 (2)2.751 (4)164 (4)
O2w—H2w1···N1i0.85 (1)2.05 (2)2.852 (5)158 (4)
O2w—H2w2···O4w0.85 (1)1.88 (2)2.709 (5)167 (4)
O3w—H3w1···O5w0.85 (1)1.89 (2)2.718 (5)166 (6)
O3w—H3w2···O3ii0.85 (1)2.03 (2)2.840 (5)158 (5)
O4w—H4w1···O1ii0.85 (1)2.01 (2)2.823 (4)160 (5)
O4w—H4w2···N50.85 (1)2.13 (3)2.918 (5)154 (5)
O5w—H5w1···O3wiii0.85 (1)2.09 (2)2.903 (6)162 (6)
O5w—H5w2···N4i0.85 (1)2.08 (2)2.918 (6)169 (6)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y+2, z+1.
 

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