Literature DB >> 21582354

catena-Poly[[[diaqua-thulium(III)]-μ-6-carboxy-nicotinato-μ-pyridine-2,5-di-carboxyl-ato] dihydrate].

Sheng Li, Yue Chen, Hong-Mei He, Yuan-Fang Ma.   

Abstract

The title compound, {[Tm(C(7)H(3)NO(4))(C(7)H(4)n class="Chemical">NO(4))(H(2)O)(2)]·2H(2)O}(n), is isotypic with the analogous Tb(III) compound [Li et al. (2009 ▶). Acta Cryst. E65, m410]. All interatomic distances and angles and the hydrogen-bond geometries are very similar for the two structures. The refined Flack parameter of 0.49 (2) suggests inversion twinning.

Entities:  

Year:  2009        PMID： 21582354      PMCID： PMC2968913          DOI： 10.1107/S1600536809008836

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


Related literature

For the isotypic TbIII compound, see Li et al. (2009 ▶). For other related structures, see: Huang et al. (2007 ▶).

Experimental

Crystal data

[Tm(C7H3NO4)(C7H4NO4)(H2O)2]·2H2O M = 572.21 Tetragonal, a = 15.1286 (12) Å c = 14.849 (2) Å V = 3398.6 (6) Å3 Z = 8 Mo Kα radiation μ = 5.30 mm−1 T = 298 K 0.12 × 0.11 × 0.09 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.569, T max = 0.647 7093 measured reflections 3085 independent reflections 2977 reflections with I > 2σ(I) R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.043 wR(F 2) = 0.111 S = 1.07 3085 reflections 263 parameters H-atom parameters constrained Δρmax = 6.96 e Å−3 Δρmin = −1.18 e Å−3 Absolute structure: Flack (1983 ▶), with 1444 Friedel pairs Flack parameter: 0.49 (2) Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809008836/bi2347sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809008836/bi2347Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Tm(C7H3NO4)(C7H4NO4)(H2O)2]·2H2ODx = 2.237 Mg m−3
Mr = 572.21Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4Cell parameters from 3085 reflections
Hall symbol: I -4θ = 1.9–25.5°
a = 15.1286 (12) ŵ = 5.30 mm−1
c = 14.849 (2) ÅT = 298 K
V = 3398.6 (6) Å3Block, colorless
Z = 80.12 × 0.11 × 0.09 mm
F(000) = 2224
Bruker APEXII CCD diffractometer3085 independent reflections
Radiation source: fine-focus sealed tube2977 reflections with I > 2σ(I)
graphiteRint = 0.031
φ and ω scansθmax = 25.5°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −18→16
Tmin = 0.569, Tmax = 0.647k = −18→15
7093 measured reflectionsl = −17→16
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.111w = 1/[σ2(Fo2) + (0.0703P)2 + 51.4546P] where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
3085 reflectionsΔρmax = 6.96 e Å−3
263 parametersΔρmin = −1.18 e Å−3
0 restraintsAbsolute structure: Flack (1983), 1444 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.49 (2)
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Tm10.30232 (3)0.22523 (3)0.22714 (3)0.01768 (14)
C10.1831 (5)0.4107 (6)0.1942 (6)0.0111 (18)
C20.1327 (6)0.4765 (6)0.1551 (6)0.0164 (19)
H2A0.11150.52290.19000.020*
C30.1140 (6)0.4732 (6)0.0642 (6)0.0156 (18)
H3A0.08160.51850.03760.019*
C40.1428 (6)0.4034 (6)0.0126 (6)0.0132 (17)
C50.1880 (6)0.3365 (6)0.0577 (7)0.0170 (19)
H5A0.20410.28640.02530.020*
C60.2156 (6)0.4129 (6)0.2916 (5)0.0115 (19)
C70.1298 (6)0.3968 (6)−0.0877 (7)0.017 (2)
C80.1188 (6)0.1237 (6)0.1724 (6)0.0133 (18)
C90.0969 (5)0.1481 (5)0.2698 (7)0.0091 (15)
C100.0232 (6)0.1189 (6)0.3171 (7)0.0160 (18)
H10A−0.01960.08560.28760.019*
C110.0128 (6)0.1380 (6)0.4051 (7)0.0160 (19)
H11A−0.03580.11620.43640.019*
C120.0768 (6)0.1922 (6)0.4506 (6)0.0103 (16)
C130.1453 (6)0.2202 (6)0.3982 (6)0.0136 (18)
H13A0.18680.25710.42510.016*
C140.0689 (6)0.2110 (7)0.5496 (6)0.016 (2)
N10.1582 (5)0.1994 (5)0.3117 (6)0.0152 (16)
N20.2099 (5)0.3404 (5)0.1464 (5)0.0117 (15)
O10.2739 (4)0.3555 (4)0.3098 (5)0.0170 (14)
H10.30590.36470.35590.025*
O20.1850 (6)0.4687 (6)0.3432 (5)0.0315 (18)
O30.1614 (5)0.3285 (4)−0.1275 (5)0.0191 (14)
O40.0916 (5)0.4563 (5)−0.1268 (5)0.0221 (15)
O50.1938 (4)0.1458 (4)0.1461 (5)0.0177 (14)
O60.0627 (5)0.0860 (5)0.1274 (5)0.0221 (15)
O70.0051 (5)0.1854 (6)0.5920 (5)0.0281 (17)
O80.1335 (4)0.2552 (5)0.5835 (5)0.0215 (15)
O90.3709 (5)0.0809 (4)0.2010 (4)0.0189 (14)
H910.38270.06910.25560.028*
H920.42270.08400.17900.028*
O100.4516 (4)0.2745 (5)0.2619 (5)0.0217 (15)
H1010.46530.28770.20800.033*
H1020.48870.23360.27270.033*
O110.2679 (7)0.0199 (6)0.0226 (6)0.042 (2)
H1110.24630.05710.05940.063*
H1120.28230.0234−0.03260.063*
O120.1257 (6)−0.0911 (6)0.0638 (6)0.041 (2)
H1210.0724−0.09000.08210.061*
H1220.1146−0.08310.00830.061*
U11U22U33U12U13U23
Tm10.0186 (2)0.0188 (2)0.0156 (2)−0.00011 (16)−0.00025 (17)0.00017 (17)
C10.006 (4)0.014 (4)0.013 (5)0.002 (3)−0.006 (3)0.001 (3)
C20.018 (4)0.014 (4)0.017 (5)0.000 (4)0.004 (4)−0.006 (4)
C30.012 (4)0.016 (4)0.019 (4)0.008 (3)−0.002 (4)0.002 (4)
C40.011 (4)0.016 (4)0.013 (4)−0.004 (3)−0.005 (3)0.001 (3)
C50.022 (5)0.012 (4)0.017 (5)0.010 (4)−0.001 (4)−0.004 (4)
C60.016 (4)0.015 (4)0.003 (5)−0.001 (3)0.002 (3)−0.006 (3)
C70.017 (5)0.019 (5)0.017 (5)−0.001 (4)0.001 (4)−0.009 (4)
C80.024 (5)0.013 (4)0.003 (4)0.006 (4)−0.004 (4)−0.005 (3)
C90.013 (4)0.010 (4)0.004 (4)−0.002 (3)−0.005 (4)0.005 (3)
C100.016 (4)0.019 (4)0.013 (4)0.000 (3)−0.002 (4)−0.002 (4)
C110.013 (4)0.015 (4)0.021 (5)0.000 (3)−0.001 (4)0.002 (4)
C120.012 (4)0.012 (4)0.007 (4)0.005 (3)0.004 (3)0.000 (3)
C130.016 (4)0.015 (4)0.009 (4)−0.002 (3)0.000 (3)−0.003 (3)
C140.014 (4)0.024 (5)0.011 (5)0.001 (4)−0.003 (4)−0.001 (4)
N10.017 (4)0.017 (4)0.011 (4)−0.002 (3)0.000 (3)−0.007 (3)
N20.015 (4)0.014 (4)0.006 (4)0.003 (3)−0.002 (3)0.000 (3)
O10.022 (3)0.015 (3)0.015 (3)−0.003 (3)−0.005 (3)0.000 (3)
O20.047 (5)0.036 (4)0.012 (3)0.021 (4)−0.004 (3)−0.005 (3)
O30.026 (4)0.017 (3)0.014 (3)0.009 (3)−0.001 (3)−0.004 (3)
O40.031 (4)0.022 (4)0.013 (3)0.014 (3)−0.007 (3)0.000 (3)
O50.018 (3)0.017 (3)0.018 (4)−0.003 (3)0.006 (3)0.000 (3)
O60.019 (3)0.025 (4)0.022 (4)−0.008 (3)−0.003 (3)−0.006 (3)
O70.030 (4)0.038 (4)0.016 (4)−0.012 (3)0.007 (3)−0.007 (3)
O80.016 (3)0.034 (4)0.015 (3)−0.008 (3)0.003 (3)−0.007 (3)
O90.021 (3)0.022 (3)0.014 (3)0.003 (3)0.007 (3)0.002 (3)
O100.016 (3)0.032 (4)0.017 (4)0.001 (3)0.001 (3)−0.001 (3)
O110.061 (6)0.036 (5)0.029 (4)0.002 (4)0.015 (4)−0.007 (4)
O120.044 (5)0.041 (5)0.036 (5)0.019 (4)0.002 (4)0.012 (4)
Tm1—O12.361 (7)C8—C91.529 (13)
Tm1—O8i2.363 (7)C9—N11.360 (12)
Tm1—O52.364 (7)C9—C101.390 (13)
Tm1—O3ii2.371 (7)C10—C111.347 (15)
Tm1—O102.434 (7)C10—H10A0.930
Tm1—O92.448 (7)C11—C121.438 (13)
Tm1—N22.536 (8)C11—H11A0.930
Tm1—N12.546 (8)C12—C131.363 (13)
C1—N21.341 (12)C12—C141.502 (13)
C1—C21.381 (13)C13—N11.338 (13)
C1—C61.528 (12)C13—H13A0.930
C2—C31.380 (14)C14—O71.215 (13)
C2—H2A0.930C14—O81.287 (12)
C3—C41.376 (13)O1—H10.850
C3—H3A0.930O3—Tm1i2.371 (7)
C4—C51.392 (13)O8—Tm1ii2.363 (7)
C4—C71.506 (14)O9—H910.850
C5—N21.359 (13)O9—H920.850
C5—H5A0.930O10—H1010.850
C6—O21.230 (12)O10—H1020.850
C6—O11.268 (11)O11—H1110.850
C7—O41.217 (13)O11—H1120.850
C7—O31.284 (12)O12—H1210.850
C8—O61.221 (12)O12—H1220.850
C8—O51.246 (12)
O1—Tm1—O8i116.1 (3)O1—C6—C1114.3 (8)
O1—Tm1—O5124.3 (2)O4—C7—O3123.6 (9)
O8i—Tm1—O583.6 (2)O4—C7—C4119.1 (9)
O1—Tm1—O3ii81.6 (2)O3—C7—C4117.4 (9)
O8i—Tm1—O3ii140.4 (2)O6—C8—O5126.0 (9)
O5—Tm1—O3ii116.7 (2)O6—C8—C9118.6 (9)
O1—Tm1—O1078.6 (2)O5—C8—C9115.4 (8)
O8i—Tm1—O1076.8 (2)N1—C9—C10119.8 (9)
O5—Tm1—O10155.2 (2)N1—C9—C8115.0 (8)
O3ii—Tm1—O1072.4 (2)C10—C9—C8125.1 (8)
O1—Tm1—O9154.7 (2)C11—C10—C9121.0 (9)
O8i—Tm1—O978.1 (2)C11—C10—H10A119.5
O5—Tm1—O976.1 (2)C9—C10—H10A119.5
O3ii—Tm1—O975.0 (2)C10—C11—C12120.0 (9)
O10—Tm1—O985.1 (2)C10—C11—H11A120.0
O1—Tm1—N264.7 (2)C12—C11—H11A120.0
O8i—Tm1—N273.3 (3)C13—C12—C11114.9 (8)
O5—Tm1—N274.1 (3)C13—C12—C14124.1 (8)
O3ii—Tm1—N2142.5 (2)C11—C12—C14120.9 (8)
O10—Tm1—N2113.6 (3)N1—C13—C12125.9 (9)
O9—Tm1—N2140.5 (2)N1—C13—H13A117.0
O1—Tm1—N173.5 (3)C12—C13—H13A117.0
O8i—Tm1—N1144.7 (3)O7—C14—O8124.5 (9)
O5—Tm1—N165.1 (3)O7—C14—C12120.7 (9)
O3ii—Tm1—N172.3 (3)O8—C14—C12114.8 (8)
O10—Tm1—N1137.5 (3)C13—N1—C9118.3 (8)
O9—Tm1—N1107.7 (2)C13—N1—Tm1124.2 (6)
N2—Tm1—N182.3 (3)C9—N1—Tm1116.5 (7)
N2—C1—C2121.0 (8)C1—N2—C5118.3 (8)
N2—C1—C6114.9 (7)C1—N2—Tm1117.5 (6)
C2—C1—C6124.0 (8)C5—N2—Tm1124.2 (6)
C3—C2—C1119.9 (8)C6—O1—Tm1126.0 (6)
C3—C2—H2A120.0C6—O1—H1117.1
C1—C2—H2A120.0Tm1—O1—H1116.9
C4—C3—C2120.4 (8)C7—O3—Tm1i141.4 (6)
C4—C3—H3A119.8C8—O5—Tm1127.5 (6)
C2—C3—H3A119.8C14—O8—Tm1ii136.9 (6)
C3—C4—C5116.5 (8)Tm1—O9—H9197.2
C3—C4—C7124.0 (9)Tm1—O9—H92113.8
C5—C4—C7119.5 (8)H91—O9—H92100.6
N2—C5—C4123.6 (8)Tm1—O10—H10195.7
N2—C5—H5A118.2Tm1—O10—H102115.4
C4—C5—H5A118.2H101—O10—H102100.8
O2—C6—O1126.8 (8)H111—O11—H112132.5
O2—C6—C1119.0 (8)H121—O12—H12296.9
N2—C1—C2—C3−4.1 (14)O3ii—Tm1—N1—C9−127.0 (7)
C6—C1—C2—C3173.5 (8)O10—Tm1—N1—C9−162.2 (6)
C1—C2—C3—C42.0 (14)O9—Tm1—N1—C9−59.8 (7)
C2—C3—C4—C52.3 (13)N2—Tm1—N1—C980.9 (6)
C2—C3—C4—C7−176.5 (9)C2—C1—N2—C51.6 (13)
C3—C4—C5—N2−5.0 (14)C6—C1—N2—C5−176.2 (8)
C7—C4—C5—N2173.9 (9)C2—C1—N2—Tm1179.9 (7)
N2—C1—C6—O2−170.7 (9)C6—C1—N2—Tm12.1 (10)
C2—C1—C6—O211.5 (14)C4—C5—N2—C13.1 (14)
N2—C1—C6—O110.3 (11)C4—C5—N2—Tm1−175.1 (7)
C2—C1—C6—O1−167.5 (8)O1—Tm1—N2—C1−7.8 (6)
C3—C4—C7—O40.1 (14)O8i—Tm1—N2—C1−138.3 (7)
C5—C4—C7—O4−178.7 (9)O5—Tm1—N2—C1133.7 (7)
C3—C4—C7—O3178.9 (9)O3ii—Tm1—N2—C120.3 (9)
C5—C4—C7—O30.2 (13)O10—Tm1—N2—C1−71.3 (7)
O6—C8—C9—N1−172.2 (8)O9—Tm1—N2—C1176.1 (6)
O5—C8—C9—N17.3 (11)N1—Tm1—N2—C167.5 (7)
O6—C8—C9—C1010.7 (13)O1—Tm1—N2—C5170.3 (8)
O5—C8—C9—C10−169.9 (9)O8i—Tm1—N2—C539.8 (8)
N1—C9—C10—C11−2.3 (13)O5—Tm1—N2—C5−48.2 (8)
C8—C9—C10—C11174.7 (8)O3ii—Tm1—N2—C5−161.6 (7)
C9—C10—C11—C122.3 (14)O10—Tm1—N2—C5106.8 (8)
C10—C11—C12—C13−0.2 (13)O9—Tm1—N2—C5−5.7 (10)
C10—C11—C12—C14−177.1 (9)N1—Tm1—N2—C5−114.3 (8)
C11—C12—C13—N1−2.1 (14)O2—C6—O1—Tm1161.1 (8)
C14—C12—C13—N1174.7 (9)C1—C6—O1—Tm1−20.0 (11)
C13—C12—C14—O7178.6 (9)O8i—Tm1—O1—C669.8 (7)
C11—C12—C14—O7−4.8 (14)O5—Tm1—O1—C6−30.8 (8)
C13—C12—C14—O8−1.2 (13)O3ii—Tm1—O1—C6−147.5 (7)
C11—C12—C14—O8175.4 (8)O10—Tm1—O1—C6138.9 (7)
C12—C13—N1—C92.2 (14)O9—Tm1—O1—C6−170.2 (6)
C12—C13—N1—Tm1−166.1 (7)N2—Tm1—O1—C615.6 (7)
C10—C9—N1—C130.1 (13)N1—Tm1—O1—C6−73.6 (7)
C8—C9—N1—C13−177.2 (8)O4—C7—O3—Tm1i14.3 (17)
C10—C9—N1—Tm1169.3 (6)C4—C7—O3—Tm1i−164.4 (7)
C8—C9—N1—Tm1−8.0 (9)O6—C8—O5—Tm1176.6 (7)
O1—Tm1—N1—C13−44.8 (7)C9—C8—O5—Tm1−2.8 (11)
O8i—Tm1—N1—C13−156.8 (7)O1—Tm1—O5—C8−46.8 (8)
O5—Tm1—N1—C13173.4 (8)O8i—Tm1—O5—C8−164.2 (8)
O3ii—Tm1—N1—C1341.5 (7)O3ii—Tm1—O5—C851.6 (8)
O10—Tm1—N1—C136.3 (9)O10—Tm1—O5—C8158.1 (7)
O9—Tm1—N1—C13108.7 (7)O9—Tm1—O5—C8116.5 (8)
N2—Tm1—N1—C13−110.6 (8)N2—Tm1—O5—C8−89.7 (7)
O1—Tm1—N1—C9146.7 (7)N1—Tm1—O5—C8−0.9 (7)
O8i—Tm1—N1—C934.7 (9)O7—C14—O8—Tm1ii23.9 (16)
O5—Tm1—N1—C94.9 (6)C12—C14—O8—Tm1ii−156.4 (6)
D—H···AD—HH···AD···AD—H···A
O1—H1···O12iii0.851.972.788 (11)162
O9—H91···O4ii0.851.832.679 (10)180
O9—H92···O4iv0.851.992.842 (10)180
O10—H101···O7i0.851.832.675 (11)179
O10—H102···O9iii0.852.142.996 (10)179
O11—H111···O50.852.022.872 (11)179
O11—H112···O2i0.851.912.763 (11)180
O12—H121···O6v0.852.153.004 (12)179
O12—H122···O6vi0.852.082.933 (12)179
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H1⋯O12i0.851.972.788 (11)162
O9—H91⋯O4ii0.851.832.679 (10)180
O9—H92⋯O4iii0.851.992.842 (10)180
O10—H101⋯O7iv0.851.832.675 (11)179
O10—H102⋯O9i0.852.142.996 (10)179
O11—H111⋯O50.852.022.872 (11)179
O11—H112⋯O2iv0.851.912.763 (11)180
O12—H121⋯O6v0.852.153.004 (12)179
O12—H122⋯O6vi0.852.082.933 (12)179

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

  3 in total

1.  New lanthanide hybrid as clustered infinite nanotunnel with 3D Ln-O-Ln framework and (3,4)-connected net.

Authors:  You-gui Huang; Ben-lai Wu; Da-qiang Yuan; Yan-qing Xu; Fei-long Jiang; Mao-chun Hong
Journal:  Inorg Chem       Date:  2007-02-19       Impact factor: 5.165

2.  A short history of SHELX.

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

3.  catena-Poly[[[diaqua-terbium(III)]-μ-6-carboxy-nicotinato-μ-pyridine-2,5-di-carboxyl-ato] dihydrate].

Authors:  Sheng Li; Fu-Li Zhang; Shou-Bin Wang; Hui-Ling Bai
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-03-19
  3 in total
  3 in total

1.  catena-Poly[[[diaqua-terbium(III)]-μ-6-carboxy-nicotinato-μ-pyridine-2,5-di-carboxyl-ato] dihydrate].

Authors:  Sheng Li; Fu-Li Zhang; Shou-Bin Wang; Hui-Ling Bai
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-03-19

2.  Retraction of articles.

Authors: 
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-06-13

3.  catena-Poly[diimidazolium [bis-(μ-pyridine-2,5-dicarboxyl-ato)bis-[diaqua-praseodymate(III)]]-bis-(μ-pyridine-2,5-dicarboxyl-ato)].

Authors:  Wenjun Zhang; Yanmei Chen; Tao Lei; Yahong Li; Wu Li
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-04-13
  3 in total

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