Literature DB >> 21836844

Poly[dimethyl-ammonium [aquadi-μ(2)-oxalato-yttriate(III)] trihydrate].

Yao-Kang Lv1, Li-Hua Gan, Liang Xu, Hao-Wen Zheng, Cao Liu.   

Abstract

The title complex, {(C(2)H(8)N)[Y(C(2)O(4))(2)(H(2)O)]·3H(2)O}(n), was obtained accidentally under hydro-thermal conditions. The Y(III) atom is chelated by four oxalate ligands and one water mol-ecule resulting in a distorted tricapped trigonal-prismatic geometry. Each oxalate ligand bridges two Y(III) atoms, thus generating a three-dimensional network with cavities in which the ammonium cations and lattice water mol-ecules reside. Various O-H⋯O and N-H⋯O hydrogen-bonding inter-actions stabilize the crystal structure. The title complex is isotypic with the Eu and Dy analogues.

Entities:  

Year:  2011        PMID： 21836844      PMCID： PMC3151934          DOI： 10.1107/S1600536811019209

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


Related literature

For general background to the rational design and synthesis of metal-organic polymers, see: Lv et al. (2010 ▶, 2011 ▶). For related structures, see: Platel et al. (2009 ▶); Gao & Cui (2008 ▶); Deguenon et al. (1990 ▶). The structure of the isotypic EuIII compound was reported by Yang et al. (2005 ▶), and that of the DyIII compound by Ye & Lin (2010 ▶). For decomposition products obtained under hydro­thermal conditions, see: Song et al. (2004 ▶).

Experimental

Crystal data

(C2H8N)[Y(C2O4)2(H2O)]·3H2O M = 383.11 Monoclinic, a = 9.6008 (1) Å b = 11.5422 (2) Å c = 14.2886 (2) Å β = 122.460 (1)° V = 1336.00 (3) Å3 Z = 4 Mo Kα radiation μ = 4.43 mm−1 T = 293 K 0.31 × 0.20 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.36, T max = 0.43 11935 measured reflections 3040 independent reflections 2384 reflections with I > 2σ(I) R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.033 wR(F 2) = 0.082 S = 1.00 3040 reflections 207 parameters 13 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.70 e Å−3 Δρmin = −0.58 e Å−3 Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); 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 & Putz, 2004 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811019209/wm2489sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811019209/wm2489Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C2H8N)[Y(C2O4)2(H2O)]·3H2OF(000) = 776
Mr = 383.11Dx = 1.905 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2287 reflections
a = 9.6008 (1) Åθ = 2.0–28.0°
b = 11.5422 (2) ŵ = 4.43 mm−1
c = 14.2886 (2) ÅT = 293 K
β = 122.460 (1)°Block, colourless
V = 1336.00 (3) Å30.31 × 0.20 × 0.19 mm
Z = 4
Bruker APEXII area-detector diffractometer3040 independent reflections
Radiation source: fine-focus sealed tube2384 reflections with I > 2σ(I)
graphiteRint = 0.044
ω scansθmax = 27.5°, θmin = 2.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −12→12
Tmin = 0.36, Tmax = 0.43k = −14→14
11935 measured reflectionsl = −18→18
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082H atoms treated by a mixture of independent and constrained refinement
S = 1.00w = 1/[σ2(Fo2) + (0.0359P)2 + 1.2217P] where P = (Fo2 + 2Fc2)/3
3040 reflections(Δ/σ)max = 0.001
207 parametersΔρmax = 0.70 e Å−3
13 restraintsΔρmin = −0.58 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.
xyzUiso*/Ueq
Y10.61770 (3)0.98846 (2)0.33257 (2)0.01817 (10)
O10.7049 (3)0.78990 (17)0.34286 (19)0.0270 (5)
O20.6167 (3)0.60733 (18)0.2950 (2)0.0304 (6)
O30.3054 (3)0.68334 (17)0.17013 (18)0.0231 (5)
O40.3959 (3)0.86535 (17)0.20743 (19)0.0259 (5)
O60.5198 (3)0.88268 (18)0.4319 (2)0.0293 (5)
O70.5387 (3)1.11238 (19)0.4367 (2)0.0320 (6)
O80.8892 (3)0.99123 (17)0.35640 (19)0.0245 (5)
O90.8389 (3)0.98964 (18)0.52152 (19)0.0278 (5)
O1W0.6044 (3)0.9808 (2)0.1578 (2)0.0348 (6)
H1WA0.617 (5)1.039 (2)0.129 (3)0.042*
H1WB0.568 (4)0.931 (2)0.122 (3)0.042*
O2W1.3774 (5)0.8468 (3)0.9672 (3)0.0649 (10)
H2WA1.386 (6)0.785 (3)0.946 (4)0.078*
H2WB1.293 (4)0.850 (4)0.965 (5)0.078*
O3W0.8383 (7)0.5082 (4)0.5055 (4)0.1038 (17)
H3WA0.857 (10)0.539 (5)0.457 (5)0.125*
H3WB0.889 (8)0.444 (3)0.512 (6)0.125*
O4W1.0523 (5)0.7844 (3)0.9661 (3)0.0861 (13)
H4WA0.959 (3)0.758 (5)0.936 (4)0.103*
H4WB1.103 (6)0.758 (5)1.030 (2)0.103*
N10.9245 (4)0.6326 (3)0.6962 (3)0.0585 (11)
H1A0.89280.60070.73940.070*
H1B0.88080.58950.63410.070*
C10.5960 (4)0.7148 (2)0.2919 (3)0.0222 (7)
C20.4163 (4)0.7587 (2)0.2166 (3)0.0195 (6)
C30.4947 (4)0.9335 (3)0.4984 (3)0.0243 (7)
C41.0151 (4)1.0005 (2)0.4524 (3)0.0202 (6)
C51.0993 (6)0.6253 (6)0.7531 (5)0.0864 (19)
H5A1.13140.54590.75670.104*
H5B1.14760.65530.82690.104*
H5C1.13700.66990.71410.104*
C60.8547 (8)0.7488 (5)0.6652 (5)0.0897 (19)
H6A0.73650.74420.62540.108*
H6B0.88720.78410.61900.108*
H6C0.89440.79460.73090.108*
U11U22U33U12U13U23
Y10.01775 (15)0.01434 (15)0.01968 (16)−0.00007 (11)0.00824 (12)−0.00024 (11)
O10.0193 (12)0.0194 (11)0.0322 (14)−0.0013 (8)0.0071 (11)−0.0044 (9)
O20.0264 (12)0.0173 (11)0.0332 (14)0.0029 (9)0.0066 (11)−0.0002 (9)
O30.0203 (11)0.0193 (10)0.0265 (13)−0.0017 (8)0.0105 (10)−0.0016 (9)
O40.0232 (12)0.0170 (10)0.0285 (13)0.0016 (8)0.0079 (10)0.0003 (9)
O60.0347 (13)0.0252 (12)0.0331 (15)−0.0039 (9)0.0216 (12)−0.0047 (10)
O70.0424 (14)0.0252 (12)0.0402 (16)0.0045 (10)0.0301 (13)0.0060 (10)
O80.0195 (10)0.0307 (12)0.0205 (11)0.0009 (9)0.0088 (9)−0.0019 (9)
O90.0209 (11)0.0368 (13)0.0265 (12)−0.0014 (9)0.0132 (10)−0.0004 (10)
O1W0.0408 (14)0.0346 (14)0.0265 (14)−0.0076 (12)0.0165 (12)−0.0043 (11)
O2W0.080 (3)0.0390 (17)0.069 (2)0.0025 (16)0.036 (2)0.0072 (16)
O3W0.112 (4)0.095 (3)0.061 (3)0.031 (3)0.017 (3)−0.013 (2)
O4W0.070 (3)0.061 (2)0.069 (3)−0.0094 (19)−0.001 (2)0.0154 (19)
N10.045 (2)0.071 (3)0.058 (3)−0.0039 (18)0.027 (2)0.022 (2)
C10.0233 (16)0.0187 (15)0.0242 (17)0.0003 (11)0.0124 (14)−0.0014 (12)
C20.0236 (17)0.0206 (15)0.0165 (16)−0.0012 (11)0.0121 (14)−0.0026 (12)
C30.0184 (14)0.0272 (17)0.0257 (17)−0.0012 (12)0.0108 (13)−0.0008 (13)
C40.0205 (14)0.0145 (14)0.0222 (16)0.0004 (11)0.0092 (13)−0.0013 (12)
C50.046 (3)0.144 (6)0.066 (4)−0.004 (3)0.028 (3)0.027 (4)
C60.110 (5)0.073 (4)0.103 (5)0.024 (3)0.068 (4)0.029 (3)
Y1—O3i2.374 (2)O2W—H2WA0.805 (19)
Y1—O92.376 (2)O2W—H2WB0.794 (19)
Y1—O42.380 (2)O3W—H3WA0.88 (2)
Y1—O62.413 (2)O3W—H3WB0.86 (2)
Y1—O12.417 (2)O4W—H4WA0.82 (2)
Y1—O2i2.422 (2)O4W—H4WB0.83 (2)
Y1—O1W2.432 (3)N1—C51.421 (6)
Y1—O82.441 (2)N1—C61.458 (6)
Y1—O72.459 (2)N1—H1A0.9000
O1—C11.247 (3)N1—H1B0.9000
O2—C11.254 (3)C1—C21.548 (4)
O2—Y1ii2.422 (2)C3—O7iii1.250 (4)
O3—C21.254 (3)C3—C3iii1.536 (6)
O3—Y1ii2.374 (2)C4—O9iv1.248 (4)
O4—C21.243 (3)C4—C4iv1.535 (6)
O6—C31.246 (4)C5—H5A0.9600
O7—C3iii1.250 (4)C5—H5B0.9600
O8—C41.255 (4)C5—H5C0.9600
O9—C4iv1.248 (4)C6—H6A0.9600
O1W—H1WA0.828 (18)C6—H6B0.9600
O1W—H1WB0.720 (17)C6—H6C0.9600
O3i—Y1—O985.24 (7)C3—O6—Y1120.4 (2)
O3i—Y1—O4135.57 (7)C3iii—O7—Y1119.2 (2)
O9—Y1—O4138.66 (8)C4—O8—Y1118.9 (2)
O3i—Y1—O6135.37 (8)C4iv—O9—Y1121.0 (2)
O9—Y1—O674.17 (8)Y1—O1W—H1WA122 (3)
O4—Y1—O670.48 (8)Y1—O1W—H1WB119 (3)
O3i—Y1—O1143.01 (7)H1WA—O1W—H1WB117 (3)
O9—Y1—O182.37 (7)H2WA—O2W—H2WB110 (3)
O4—Y1—O167.70 (7)H3WA—O3W—H3WB95 (7)
O6—Y1—O173.50 (8)H4WA—O4W—H4WB106 (3)
O3i—Y1—O2i67.82 (7)C5—N1—C6115.9 (5)
O9—Y1—O2i139.01 (8)C5—N1—H1A108.3
O4—Y1—O2i71.18 (7)C6—N1—H1A108.3
O6—Y1—O2i103.39 (8)C5—N1—H1B108.3
O1—Y1—O2i137.25 (7)C6—N1—H1B108.3
O3i—Y1—O1W82.13 (8)H1A—N1—H1B107.4
O9—Y1—O1W133.57 (8)O1—C1—O2126.8 (3)
O4—Y1—O1W70.99 (8)O1—C1—C2116.8 (2)
O6—Y1—O1W139.75 (8)O2—C1—C2116.4 (3)
O1—Y1—O1W81.59 (8)O4—C2—O3126.2 (3)
O2i—Y1—O1W74.46 (9)O4—C2—C1116.8 (3)
O3i—Y1—O870.84 (7)O3—C2—C1117.0 (3)
O9—Y1—O866.75 (7)O6—C3—O7iii126.7 (3)
O4—Y1—O8124.78 (8)O6—C3—C3iii117.1 (4)
O6—Y1—O8130.44 (8)O7iii—C3—C3iii116.2 (4)
O1—Y1—O872.24 (7)O9iv—C4—O8127.1 (3)
O2i—Y1—O8126.06 (8)O9iv—C4—C4iv116.9 (3)
O1W—Y1—O866.89 (8)O8—C4—C4iv116.0 (3)
O3i—Y1—O770.02 (7)N1—C5—H5A109.5
O9—Y1—O771.75 (8)N1—C5—H5B109.5
O4—Y1—O7111.09 (8)H5A—C5—H5B109.5
O6—Y1—O766.06 (8)N1—C5—H5C109.5
O1—Y1—O7136.38 (8)H5A—C5—H5C109.5
O2i—Y1—O770.27 (8)H5B—C5—H5C109.5
O1W—Y1—O7141.16 (8)N1—C6—H6A109.5
O8—Y1—O7124.12 (8)N1—C6—H6B109.5
C1—O1—Y1117.95 (18)H6A—C6—H6B109.5
C1—O2—Y1ii117.94 (19)N1—C6—H6C109.5
C2—O3—Y1ii118.85 (19)H6A—C6—H6C109.5
C2—O4—Y1119.03 (19)H6B—C6—H6C109.5
O3i—Y1—O1—C1−146.8 (2)O3i—Y1—O8—C487.9 (2)
O9—Y1—O1—C1141.7 (2)O9—Y1—O8—C4−5.14 (19)
O4—Y1—O1—C1−9.2 (2)O4—Y1—O8—C4−139.29 (19)
O6—Y1—O1—C166.0 (2)O6—Y1—O8—C4−46.0 (2)
O2i—Y1—O1—C1−26.0 (3)O1—Y1—O8—C4−94.3 (2)
O1W—Y1—O1—C1−82.0 (2)O2i—Y1—O8—C4129.6 (2)
O8—Y1—O1—C1−150.3 (3)O1W—Y1—O8—C4177.4 (2)
O7—Y1—O1—C188.5 (3)O7—Y1—O8—C440.2 (2)
O3i—Y1—O4—C2156.4 (2)O3i—Y1—O9—C4iv−65.9 (2)
O9—Y1—O4—C2−35.0 (3)O4—Y1—O9—C4iv122.1 (2)
O6—Y1—O4—C2−67.7 (2)O6—Y1—O9—C4iv154.1 (2)
O1—Y1—O4—C211.9 (2)O1—Y1—O9—C4iv79.1 (2)
O2i—Y1—O4—C2179.9 (3)O2i—Y1—O9—C4iv−113.6 (2)
O1W—Y1—O4—C2100.4 (2)O1W—Y1—O9—C4iv8.5 (3)
O8—Y1—O4—C258.5 (3)O8—Y1—O9—C4iv5.23 (19)
O7—Y1—O4—C2−121.0 (2)O7—Y1—O9—C4iv−136.5 (2)
O3i—Y1—O6—C32.2 (3)Y1—O1—C1—O2−173.7 (3)
O9—Y1—O6—C368.0 (2)Y1—O1—C1—C26.4 (4)
O4—Y1—O6—C3−133.8 (3)Y1ii—O2—C1—O1−172.3 (3)
O1—Y1—O6—C3154.5 (3)Y1ii—O2—C1—C27.6 (4)
O2i—Y1—O6—C3−69.7 (2)Y1—O4—C2—O3167.4 (2)
O1W—Y1—O6—C3−151.3 (2)Y1—O4—C2—C1−13.2 (4)
O8—Y1—O6—C3106.6 (2)Y1ii—O3—C2—O4165.7 (3)
O7—Y1—O6—C3−8.7 (2)Y1ii—O3—C2—C1−13.8 (4)
O3i—Y1—O7—C3iii−163.4 (3)O1—C1—C2—O44.4 (4)
O9—Y1—O7—C3iii−71.8 (2)O2—C1—C2—O4−175.5 (3)
O4—Y1—O7—C3iii64.3 (3)O1—C1—C2—O3−176.1 (3)
O6—Y1—O7—C3iii8.5 (2)O2—C1—C2—O34.0 (4)
O1—Y1—O7—C3iii−15.1 (3)Y1—O6—C3—O7iii−171.9 (3)
O2i—Y1—O7—C3iii123.9 (3)Y1—O6—C3—C3iii8.3 (5)
O1W—Y1—O7—C3iii149.8 (2)Y1—O8—C4—O9iv−175.3 (2)
O8—Y1—O7—C3iii−115.3 (2)Y1—O8—C4—C4iv4.7 (4)
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2Wiv0.83 (2)1.93 (2)2.742 (4)167 (4)
O1W—H1WB···O2Wv0.72 (2)2.20 (2)2.861 (4)152 (4)
O2W—H2WA···O6vi0.81 (2)2.38 (2)3.143 (4)158 (5)
O2W—H2WA···O7vii0.81 (2)2.45 (5)2.944 (4)121 (5)
O2W—H2WB···O3Wviii0.79 (2)2.38 (3)2.963 (7)131 (4)
O2W—H2WB···O4W0.79 (2)2.44 (3)3.194 (6)159 (5)
O3W—H3WA···O20.88 (2)2.36 (7)2.830 (5)114 (6)
O3W—H3WB···O4Wvii0.86 (2)1.90 (3)2.735 (6)161 (6)
O4W—H4WA···O1ix0.82 (2)2.13 (2)2.943 (4)172 (5)
O4W—H4WB···O3x0.83 (2)2.08 (3)2.857 (4)155 (6)
N1—H1A···O8ix0.902.002.869 (4)163
N1—H1A···O1Wix0.902.543.107 (4)122
N1—H1B···O3W0.901.902.784 (6)166
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1WA⋯O2Wi0.83 (2)1.93 (2)2.742 (4)167 (4)
O1W—H1WB⋯O2Wii0.72 (2)2.20 (2)2.861 (4)152 (4)
O2W—H2WA⋯O6iii0.81 (2)2.38 (2)3.143 (4)158 (5)
O2W—H2WA⋯O7iv0.81 (2)2.45 (5)2.944 (4)121 (5)
O2W—H2WB⋯O3Wv0.79 (2)2.38 (3)2.963 (7)131 (4)
O2W—H2WB⋯O4W0.79 (2)2.44 (3)3.194 (6)159 (5)
O3W—H3WA⋯O20.88 (2)2.36 (7)2.830 (5)114 (6)
O3W—H3WB⋯O4Wiv0.86 (2)1.90 (3)2.735 (6)161 (6)
O4W—H4WA⋯O1vi0.82 (2)2.13 (2)2.943 (4)172 (5)
O4W—H4WB⋯O3vii0.83 (2)2.08 (3)2.857 (4)155 (6)
N1—H1A⋯O8vi0.902.002.869 (4)163
N1—H1A⋯O1Wvi0.902.543.107 (4)122
N1—H1B⋯O3W0.901.902.784 (6)166

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

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