Literature DB >> 21582717

Poly[diethyl-enetriammonium [aquadi-μ(2)-sulfato-sulfatolanthanum(III)]].

Yuan-Rui Wang1, Yong-Sheng Hu, Cui-Li Shi, Dan-Ping Li, Ya-Feng Li.   

Abstract

In the title compound, {(C(4)H(16)N(3))[La(SO(4))(3)(H(2)O)]}(n), the La atom adopts an irregular LaO(9) coordination geometry, including one bonded water mol-ecule. The three sulfate groups adopt both monodentate and bidentate coordination to the metal ions. Two of the sulfate groups serve as bridges in the (100) and (010) directions, yielding infinite sheets, whereas the third is pendant to one La(3+) cation. The protonated organic species inter-acts with the layers by way of N-H⋯O hydrogen bonds, and O-H⋯O hydrogen bonds involving aqua ligands also occur.

Entities:  

Year:  2009        PMID: 21582717      PMCID: PMC2969472          DOI: 10.1107/S1600536809022272

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For related lanthanide sulfate structures, see: Bataille & Louër (2004 ▶); Dan et al. (2004 ▶); Liu et al. (2005 ▶); Rao et al. (2006 ▶); Wickleder (2002 ▶); Xing et al. (2003 ▶).

Experimental

Crystal data

(C4H16N3)[La(SO4)3(H2O)] M = 551.33 Monoclinic, a = 6.7128 (13) Å b = 10.442 (2) Å c = 11.103 (2) Å β = 93.94 (3)° V = 776.4 (3) Å3 Z = 2 Mo Kα radiation μ = 3.23 mm−1 T = 293 K 0.45 × 0.31 × 0.06 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.317, T max = 0.830 7574 measured reflections 3429 independent reflections 3312 reflections with I > 2σ(I) R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.021 wR(F 2) = 0.049 S = 1.17 3429 reflections 225 parameters 4 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.35 e Å−3 Δρmin = −0.61 e Å−3 Absolute structure: Flack (1983 ▶), 1552 Friedel pairs Flack parameter: −0.098 (11) Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2000 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809022272/hb2997sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809022272/hb2997Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C4H16N3)[La(SO4)3(H2O)]F(000) = 544
Mr = 551.33Dx = 2.358 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 2000 reflections
a = 6.7128 (13) Åθ = 3.0–27.5°
b = 10.442 (2) ŵ = 3.23 mm1
c = 11.103 (2) ÅT = 293 K
β = 93.94 (3)°Rod, colourless
V = 776.4 (3) Å30.45 × 0.31 × 0.06 mm
Z = 2
Rigaku R-AXIS RAPID diffractometer3429 independent reflections
Radiation source: fine-focus sealed tube3312 reflections with I > 2σ(I)
graphiteRint = 0.028
Detector resolution: 10.00 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = −8→7
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)k = −13→13
Tmin = 0.317, Tmax = 0.830l = −14→14
7574 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.049w = 1/[σ2(Fo2) + (0.0089P)2] where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max = 0.006
3429 reflectionsΔρmax = 0.35 e Å3
225 parametersΔρmin = −0.60 e Å3
4 restraintsAbsolute structure: Flack (1983), 1552 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.098 (11)
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.
xyzUiso*/Ueq
La10.53138 (2)0.36394 (2)0.180431 (16)0.00943 (6)
S1−0.00721 (14)0.31013 (9)0.24266 (10)0.0156 (2)
S20.42405 (15)0.58541 (9)0.36244 (10)0.0176 (2)
S30.42773 (14)0.02938 (9)0.06143 (10)0.0167 (2)
O10.4541 (4)0.1705 (3)0.0573 (3)0.0236 (7)
O20.6123 (4)−0.0363 (3)0.0235 (3)0.0234 (7)
O30.4904 (4)0.4531 (3)0.3940 (3)0.0241 (7)
O40.3862 (5)−0.0119 (3)0.1833 (3)0.0287 (7)
O5−0.1328 (4)0.4210 (3)0.2793 (3)0.0226 (6)
O60.4374 (4)0.5935 (3)0.2274 (3)0.0220 (7)
O70.1623 (3)0.3571 (4)0.1758 (2)0.0233 (6)
O8−0.1464 (4)0.2337 (3)0.1610 (3)0.0217 (7)
O90.2667 (4)−0.0115 (3)−0.0290 (3)0.0226 (7)
O100.0654 (5)0.2351 (3)0.3473 (3)0.0333 (8)
O110.5666 (5)0.6790 (3)0.4210 (3)0.0285 (7)
O120.2219 (4)0.6107 (3)0.3958 (3)0.0320 (8)
O1W0.5151 (5)0.1920 (3)0.3288 (3)0.0242 (7)
H1F0.478 (6)0.119 (3)0.303 (4)0.029*
H1G0.554 (7)0.188 (4)0.403 (2)0.029*
N11.0903 (5)0.6434 (3)0.0681 (4)0.0267 (8)
H1A1.16670.66200.00810.032*
H1B0.99600.58810.04220.032*
H1C1.16510.60890.12900.032*
N20.7510 (5)0.8376 (3)0.2587 (4)0.0270 (10)
H2A0.67140.86870.19700.032*
H2B0.67140.80810.31450.032*
N31.0998 (5)1.0100 (3)0.4815 (4)0.0265 (9)
H3A1.18930.98220.53840.032*
H3B0.99831.04640.51590.032*
H3C1.15671.06710.43520.032*
C10.9941 (7)0.7643 (4)0.1105 (5)0.0280 (10)
H1D0.91150.80280.04510.034*
H1E1.09520.82570.13870.034*
C20.8674 (6)0.7262 (4)0.2127 (4)0.0221 (9)
H2C0.77490.65950.18470.027*
H2D0.95320.69150.27860.027*
C30.8728 (7)0.9459 (4)0.3132 (5)0.0293 (11)
H3D0.93840.99000.25000.035*
H3E0.78491.00660.34920.035*
C41.0257 (7)0.9011 (4)0.4067 (5)0.0339 (12)
H4A0.96790.83730.45730.041*
H4B1.13590.86180.36820.041*
U11U22U33U12U13U23
La10.00845 (8)0.00909 (8)0.01059 (9)−0.00017 (11)−0.00037 (6)−0.00017 (12)
S10.0125 (4)0.0176 (4)0.0165 (5)−0.0001 (4)−0.0004 (4)0.0015 (4)
S20.0180 (5)0.0177 (5)0.0169 (5)−0.0002 (4)0.0002 (4)−0.0024 (4)
S30.0182 (5)0.0156 (4)0.0161 (5)−0.0013 (4)0.0002 (4)−0.0022 (4)
O10.0310 (17)0.0163 (14)0.0238 (18)−0.0007 (13)0.0034 (14)−0.0025 (12)
O20.0223 (16)0.0224 (14)0.0253 (18)0.0088 (12)0.0006 (13)−0.0037 (13)
O30.0279 (17)0.0219 (14)0.0226 (18)0.0050 (13)0.0023 (14)0.0011 (13)
O40.0431 (19)0.0273 (16)0.0161 (18)−0.0080 (15)0.0038 (14)−0.0004 (13)
O50.0148 (14)0.0283 (14)0.0247 (17)0.0027 (13)0.0012 (13)−0.0069 (13)
O60.0255 (16)0.0225 (14)0.0175 (17)0.0009 (13)−0.0028 (13)−0.0019 (12)
O70.0146 (11)0.0317 (14)0.0243 (14)0.0013 (18)0.0053 (10)0.010 (2)
O80.0191 (14)0.0188 (14)0.0268 (18)−0.0017 (12)−0.0004 (13)−0.0053 (12)
O90.0210 (15)0.0258 (15)0.0204 (18)0.0016 (13)−0.0035 (12)−0.0051 (13)
O100.0318 (18)0.0370 (18)0.030 (2)0.0032 (16)−0.0058 (15)0.0145 (15)
O110.0305 (17)0.0313 (16)0.0228 (18)−0.0111 (14)−0.0037 (14)−0.0056 (14)
O120.0224 (15)0.0356 (17)0.039 (2)0.0066 (14)0.0108 (15)−0.0046 (16)
O1W0.0368 (17)0.0208 (15)0.0153 (17)−0.0009 (15)0.0034 (14)0.0021 (13)
N10.0235 (19)0.033 (2)0.024 (2)−0.0013 (17)0.0031 (16)0.0009 (17)
N20.0222 (16)0.027 (3)0.031 (2)0.0017 (15)−0.0033 (15)−0.0011 (16)
N30.030 (2)0.0243 (18)0.024 (2)−0.0041 (17)−0.0034 (17)0.0005 (16)
C10.028 (2)0.026 (2)0.030 (3)−0.0006 (19)0.000 (2)0.004 (2)
C20.023 (2)0.020 (2)0.024 (2)0.0011 (17)0.0016 (18)0.0003 (18)
C30.035 (3)0.0159 (19)0.036 (3)−0.0007 (19)−0.008 (2)−0.0034 (19)
C40.050 (3)0.022 (2)0.028 (3)0.007 (2)−0.011 (2)−0.0010 (18)
La1—O1W2.445 (3)N1—C11.508 (6)
La1—O12.474 (3)N1—H1A0.8900
La1—O72.475 (2)N1—H1B0.8900
La1—O5i2.510 (3)N1—H1C0.8900
La1—O62.542 (3)N2—C31.498 (5)
La1—O8i2.577 (3)N2—C21.510 (5)
La1—O32.580 (3)N2—H2A0.9000
La1—O9ii2.583 (3)N2—H2B0.9000
La1—O2ii2.615 (3)N3—C41.474 (5)
S1—O101.457 (3)N3—H3A0.8900
S1—O71.484 (3)N3—H3B0.8900
S1—O81.488 (3)N3—H3C0.8900
S1—O51.504 (3)C1—C21.517 (6)
S2—O121.455 (3)C1—H1D0.9700
S2—O111.486 (3)C1—H1E0.9700
S2—O31.486 (3)C2—H2C0.9700
S2—O61.511 (3)C2—H2D0.9700
S3—O41.465 (3)C3—C41.485 (6)
S3—O11.485 (3)C3—H3D0.9700
S3—O91.486 (3)C3—H3E0.9700
S3—O21.501 (3)C4—H4A0.9700
O1W—H1F0.841 (19)C4—H4B0.9700
O1W—H1G0.850 (18)
O1W—La1—O175.84 (11)S3—O1—La1144.5 (2)
O1W—La1—O784.36 (11)S3—O2—La1iii99.36 (14)
O1—La1—O778.07 (11)S2—O3—La199.67 (16)
O1W—La1—O5i87.70 (11)S1—O5—La1iv101.69 (14)
O1—La1—O5i125.67 (9)S2—O6—La1100.57 (14)
O7—La1—O5i152.06 (10)S1—O7—La1143.12 (17)
O1W—La1—O6122.10 (10)S1—O8—La1iv99.29 (14)
O1—La1—O6146.90 (10)S3—O9—La1iii101.23 (14)
O7—La1—O676.67 (11)La1—O1W—H1F117 (3)
O5i—La1—O685.11 (9)La1—O1W—H1G132 (3)
O1W—La1—O8i75.26 (11)H1F—O1W—H1G110 (3)
O1—La1—O8i70.62 (9)C1—N1—H1A109.5
O7—La1—O8i145.87 (10)C1—N1—H1B109.5
O5i—La1—O8i55.10 (9)H1A—N1—H1B109.5
O6—La1—O8i137.43 (9)C1—N1—H1C109.5
O1W—La1—O368.48 (10)H1A—N1—H1C109.5
O1—La1—O3140.45 (10)H1B—N1—H1C109.5
O7—La1—O381.93 (10)C3—N2—C2115.9 (3)
O5i—La1—O370.24 (10)C3—N2—H2A108.3
O6—La1—O355.07 (9)C2—N2—H2A108.3
O8i—La1—O3114.26 (10)C3—N2—H2B108.3
O1W—La1—O9ii149.15 (10)C2—N2—H2B108.3
O1—La1—O9ii98.68 (10)H2A—N2—H2B107.4
O7—La1—O9ii124.77 (10)C4—N3—H3A109.5
O5i—La1—O9ii70.70 (10)C4—N3—H3B109.5
O6—La1—O9ii78.89 (10)H3A—N3—H3B109.5
O8i—La1—O9ii74.33 (10)C4—N3—H3C109.5
O3—La1—O9ii120.71 (10)H3A—N3—H3C109.5
O1W—La1—O2ii147.69 (10)H3B—N3—H3C109.5
O1—La1—O2ii78.24 (10)N1—C1—C2106.8 (4)
O7—La1—O2ii71.61 (9)N1—C1—H1D110.4
O5i—La1—O2ii123.41 (9)C2—C1—H1D110.4
O6—La1—O2ii73.73 (10)N1—C1—H1E110.4
O8i—La1—O2ii113.54 (10)C2—C1—H1E110.4
O3—La1—O2ii126.54 (10)H1D—C1—H1E108.6
O9ii—La1—O2ii54.16 (9)N2—C2—C1112.4 (3)
O10—S1—O7110.52 (18)N2—C2—H2C109.1
O10—S1—O8111.06 (19)C1—C2—H2C109.1
O7—S1—O8110.06 (18)N2—C2—H2D109.1
O10—S1—O5111.2 (2)C1—C2—H2D109.1
O7—S1—O5110.1 (2)H2C—C2—H2D107.9
O8—S1—O5103.72 (16)C4—C3—N2112.1 (3)
O12—S2—O11110.7 (2)C4—C3—H3D109.2
O12—S2—O3112.23 (19)N2—C3—H3D109.2
O11—S2—O3109.55 (19)C4—C3—H3E109.2
O12—S2—O6111.26 (19)N2—C3—H3E109.2
O11—S2—O6108.49 (18)H3D—C3—H3E107.9
O3—S2—O6104.40 (17)N3—C4—C3109.9 (4)
O4—S3—O1110.57 (18)N3—C4—H4A109.7
O4—S3—O9111.30 (18)C3—C4—H4A109.7
O1—S3—O9110.28 (18)N3—C4—H4B109.7
O4—S3—O2109.77 (19)C3—C4—H4B109.7
O1—S3—O2109.99 (18)H4A—C4—H4B108.2
O9—S3—O2104.78 (17)
O4—S3—O1—La120.4 (4)O11—S2—O6—La1121.73 (16)
O4—S3—O1—La120.4 (4)O3—S2—O6—La14.98 (17)
O9—S3—O1—La1144.0 (3)O1W—La1—O6—S211.55 (19)
O2—S3—O1—La1−101.0 (3)O1—La1—O6—S2127.22 (17)
La1iii—S3—O1—La1−159.2 (2)O7—La1—O6—S286.02 (15)
O1W—La1—O1—S3−4.8 (3)O5i—La1—O6—S2−72.65 (15)
O7—La1—O1—S3−91.9 (3)O8i—La1—O6—S2−92.26 (18)
O5i—La1—O1—S371.8 (3)O3—La1—O6—S2−3.38 (12)
O6—La1—O1—S3−132.8 (3)O9ii—La1—O6—S2−143.91 (15)
O8i—La1—O1—S374.3 (3)O2ii—La1—O6—S2160.44 (16)
O3—La1—O1—S3−30.7 (4)S1i—La1—O6—S2−79.21 (14)
O9ii—La1—O1—S3144.2 (3)S3ii—La1—O6—S2−170.95 (15)
O2ii—La1—O1—S3−165.3 (3)O10—S1—O7—La1−4.0 (4)
S1i—La1—O1—S371.8 (3)O8—S1—O7—La1−127.0 (3)
S2—La1—O1—S3−76.5 (4)O5—S1—O7—La1119.3 (4)
S3ii—La1—O1—S3169.9 (3)La1iv—S1—O7—La1174.6 (2)
O4—S3—O2—La1iii125.92 (15)O1W—La1—O7—S116.6 (4)
O4—S3—O2—La1iii125.92 (15)O1—La1—O7—S193.2 (4)
O1—S3—O2—La1iii−112.21 (16)O5i—La1—O7—S1−57.7 (5)
O9—S3—O2—La1iii6.31 (17)O6—La1—O7—S1−108.3 (4)
O12—S2—O3—La1115.73 (19)O8i—La1—O7—S169.6 (4)
O11—S2—O3—La1−120.90 (17)O3—La1—O7—S1−52.4 (4)
O11—S2—O3—La1−120.90 (17)O9ii—La1—O7—S1−174.4 (3)
O6—S2—O3—La1−4.89 (17)O2ii—La1—O7—S1174.7 (4)
O1W—La1—O3—S2−163.00 (19)S1i—La1—O7—S115.3 (6)
O1—La1—O3—S2−135.94 (15)S2—La1—O7—S1−79.7 (4)
O7—La1—O3—S2−75.91 (16)S3ii—La1—O7—S1−178.3 (4)
O5i—La1—O3—S2101.50 (16)O10—S1—O8—La1iv115.43 (17)
O6—La1—O3—S23.43 (12)O7—S1—O8—La1iv−121.86 (17)
O8i—La1—O3—S2135.54 (13)O5—S1—O8—La1iv−4.05 (18)
O9ii—La1—O3—S249.94 (18)O4—S3—O9—La1iii−125.00 (16)
O2ii—La1—O3—S2−16.0 (2)O4—S3—O9—La1iii−125.00 (16)
S1i—La1—O3—S2119.34 (14)O1—S3—O9—La1iii111.89 (16)
S3ii—La1—O3—S218.23 (18)O2—S3—O9—La1iii−6.43 (18)
O1—S3—O4—O40.00 (18)O12—S2—O11—O110.0 (3)
O9—S3—O4—O40.00 (10)O3—S2—O11—O110.0 (3)
O2—S3—O4—O40.00 (13)O6—S2—O11—O110.0 (4)
La1iii—S3—O4—O40.00 (5)La1—S2—O11—O110.0 (4)
O10—S1—O5—La1iv−115.22 (18)C3—N2—C2—C1−62.8 (5)
O7—S1—O5—La1iv121.94 (14)N1—C1—C2—N2−176.3 (3)
O8—S1—O5—La1iv4.19 (18)C2—N2—C3—C4−51.4 (6)
O12—S2—O6—La1−116.29 (17)N2—C3—C4—N3−163.4 (4)
O11—S2—O6—La1121.73 (16)
D—H···AD—HH···AD···AD—H···A
O1W—H1F···O40.84 (2)1.98 (2)2.775 (5)157 (4)
O1W—H1G···O11v0.85 (2)2.17 (4)2.872 (5)140 (4)
N1—H1A···O8ii0.892.022.762 (5)141
N1—H1B···O9ii0.892.042.900 (5)161
N1—H1C···O6i0.892.072.874 (5)150
N2—H2B···O110.901.962.798 (5)155
N2—H2A···O2vi0.902.183.015 (5)154
N2—H2A···O4vi0.902.282.981 (5)134
N3—H3A···O5vii0.892.182.809 (5)127
N3—H3A···O3viii0.892.253.051 (5)150
N3—H3B···O12vii0.891.952.834 (5)174
N3—H3C···O10ix0.892.082.784 (5)135
Table 1

Selected bond lengths (Å)

La1—O1W2.445 (3)
La1—O12.474 (3)
La1—O72.475 (2)
La1—O5i2.510 (3)
La1—O62.542 (3)
La1—O8i2.577 (3)
La1—O32.580 (3)
La1—O9ii2.583 (3)
La1—O2ii2.615 (3)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O1W—H1F⋯O40.841 (19)1.98 (2)2.775 (5)157 (4)
O1W—H1G⋯O11iii0.850 (18)2.17 (4)2.872 (5)140 (4)
N1—H1A⋯O8ii0.892.022.762 (5)141
N1—H1B⋯O9ii0.892.042.900 (5)161
N1—H1C⋯O6i0.892.072.874 (5)150
N2—H2B⋯O110.901.962.798 (5)155
N2—H2A⋯O2iv0.902.183.015 (5)154
N2—H2A⋯O4iv0.902.282.981 (5)134
N3—H3A⋯O5v0.892.182.809 (5)127
N3—H3A⋯O3vi0.892.253.051 (5)150
N3—H3B⋯O12v0.891.952.834 (5)174
N3—H3C⋯O10vii0.892.082.784 (5)135

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

  3 in total

1.  Inorganic lanthanide compounds with complex anions.

Authors:  Mathias S Wickleder
Journal:  Chem Rev       Date:  2002-06       Impact factor: 60.622

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Organically-templated metal sulfates, selenites and selenates.

Authors:  C N R Rao; J N Behera; Meenakshi Dan
Journal:  Chem Soc Rev       Date:  2006-01-30       Impact factor: 54.564

  3 in total
  1 in total

1.  Bis(1,10-phenanthroline-κN,N')(sulfato-κO,O')cobalt(II) propane-1,3-diol solvate.

Authors:  Kai-Long Zhong
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-02-03
  1 in total

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