Download citation
Download citation
link to html
The title compound, di­aqua­(pyridine-2,6-di­carboxyl­ato)(6-carboxy­pyridine-2-carboxyl­ato)­lanthanum(III) dihydrate ethanol solvate, [LaIII(C7H4NO4)(C7H3NO4)(H2O)2]·2H2O·C2H5OH, is a polynuclear complex in which neighbouring LaIII ions are bridged by the carboxyl­ate O atoms of the anionic ligand mol­ecules. The central LaIII atom is coordin­ated by two N,O,O'-tridentate dipicolinic acid ligands, and two water O atoms. The coordination number of the LaIII ion is nine.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802007596/bt6140sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802007596/bt6140Isup2.hkl
Contains datablock I

CCDC reference: 185757

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.031
  • wR factor = 0.109
  • Data-to-parameter ratio = 16.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_360 Alert C Short C(sp3)-C(sp3) Bond C(16) - C(17) = 1.41 Ang.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

Dipicolinic acid (dipic; pyridine-2,6-dicarboxylic acid) is a component of bacterial spores (Powell, 1953). It can induce apoptosis in leukemia HL-60 cells which is cell-death characterized by DNA fragmentation (Ogata et al., 2000). It forms complexes with many bivalent and monovalent metals, such as CaII, TiII, MnII, FeII, NiII, CuII, ZnII, SrII, AgII and LiI (Odoko et al., 2002). Here, we aimed to clarify the structure of the rare earth metal complexes of dipicolinic acid, since rare earth metals are known to have antitumor activity (Zhou et al., 2001). In this study, the structure of the LaIII complex (I) has been determined.

The structure of (I) is shown in Fig. 1. It has a unique polynuclear chain structure consisting of the [LaIII(dipic)2(H2O)2] coordination unit, in which the central LaIII atom is bonded to four O atoms and two N atoms of the two N,O,O'-tridentate dipicolinates and to two water O atoms. The LaIII ions in the coordination units are linked together by the carboxylate O atom of the dianionic dipicolinate ligand, forming a polynuclear chain structure. One of the ligand molecules is dianionic and another is monoanionic. The total charge of the title compound is neutral. In the [LaIII(dipic)2] unit, LaIII has a distorted nine-coordinate geometry. Selected geometric parameters are listed in Table 1.

Experimental top

Colorless prismatic crystals of (I) were obtained by slow evaporation from a 50% ethanol–water solution of dipicolinic acid (pyridine-2-carboxylic acid) and LaCl3·7H2O (2:1 molar ratio).

Refinement top

All H atoms were located from difference Fourier maps and included in the refinement using the riding-model approximation.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation and Rigaku, 1999); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation and Rigaku, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) and DIRDIF94 (Beurskens et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.

Figures top
[Figure 1] Fig. 1. ORTEPII (Johnson, 1976) drawing of the title compound with the atomic numbering scheme. Ellipsoids for non-H atoms correspond to the 50% probability level.
(I) top
Crystal data top
[La(C7H4NO4)(C7H3NO4)(H2O)2]·2H2O·C2H6OF(000) = 1168.0
Mr = 588.26Dx = 1.863 Mg m3
Monoclinic, P21/aMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2yabCell parameters from 25 reflections
a = 13.037 (4) Åθ = 14.6–15.0°
b = 11.003 (3) ŵ = 2.11 mm1
c = 14.851 (3) ÅT = 296 K
β = 100.12 (2)°Pillar, colorless
V = 2097.2 (10) Å30.20 × 0.10 × 0.10 mm
Z = 4
Data collection top
Rigaku AFC-5R
diffractometer
Rint = 0.025
ω–2θ scansθmax = 27.5°
Absorption correction: ψ scan
(North et al., 1968)
h = 016
Tmin = 0.773, Tmax = 0.810k = 014
5275 measured reflectionsl = 1918
4811 independent reflections3 standard reflections every 150 reflections
3623 reflections with I > 2σ(I) intensity decay: 0.4%
Refinement top
Refinement on F2H-atom parameters not refined
R[F2 > 2σ(F2)] = 0.031 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.109(Δ/σ)max = 0.003
S = 0.80Δρmax = 0.98 e Å3
4811 reflectionsΔρmin = 0.91 e Å3
289 parameters
Crystal data top
[La(C7H4NO4)(C7H3NO4)(H2O)2]·2H2O·C2H6OV = 2097.2 (10) Å3
Mr = 588.26Z = 4
Monoclinic, P21/aMo Kα radiation
a = 13.037 (4) ŵ = 2.11 mm1
b = 11.003 (3) ÅT = 296 K
c = 14.851 (3) Å0.20 × 0.10 × 0.10 mm
β = 100.12 (2)°
Data collection top
Rigaku AFC-5R
diffractometer
3623 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.025
Tmin = 0.773, Tmax = 0.8103 standard reflections every 150 reflections
5275 measured reflections intensity decay: 0.4%
4811 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.031289 parameters
wR(F2) = 0.109H-atom parameters not refined
S = 0.80Δρmax = 0.98 e Å3
4811 reflectionsΔρmin = 0.91 e Å3
Special details top

Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
La10.15477 (2)0.19317 (2)0.27207 (1)0.01921 (9)
O10.1296 (3)0.4954 (3)0.4822 (2)0.0388 (8)
O20.1405 (3)0.3850 (3)0.3591 (2)0.0338 (7)
O30.1299 (3)0.1397 (3)0.4671 (3)0.0422 (8)
O40.1374 (3)0.0192 (3)0.3469 (2)0.0349 (7)
O50.2093 (2)0.1700 (3)0.2259 (2)0.0324 (7)
O60.0414 (2)0.2097 (3)0.2798 (2)0.0292 (7)
O70.2070 (3)0.1112 (3)0.0684 (3)0.0427 (9)
O80.2172 (2)0.0606 (3)0.1510 (2)0.0327 (7)
O90.3338 (3)0.1324 (4)0.3589 (3)0.0423 (9)
O100.0690 (3)0.3164 (3)0.1374 (3)0.0385 (8)
O110.1136 (4)0.3191 (4)0.3674 (3)0.064 (1)
O120.6134 (3)0.0584 (4)0.9958 (3)0.061 (1)
O130.3601 (3)0.1915 (3)0.0538 (3)0.0372 (8)
N10.1338 (3)0.1783 (3)0.4481 (3)0.0256 (7)
N20.0204 (3)0.0465 (3)0.1692 (2)0.0224 (7)
C20.1314 (4)0.2803 (4)0.4962 (3)0.0274 (9)
C30.1252 (5)0.2788 (5)0.5883 (4)0.042 (1)
C40.1243 (6)0.1673 (6)0.6313 (4)0.053 (2)
C50.1272 (4)0.0611 (5)0.5813 (3)0.042 (1)
C60.1316 (3)0.0713 (4)0.4906 (3)0.0280 (9)
C70.1334 (3)0.3960 (4)0.4423 (3)0.0266 (9)
C80.1337 (3)0.0352 (4)0.4282 (3)0.0301 (9)
C90.0812 (3)0.0476 (4)0.1748 (3)0.0217 (8)
C100.1508 (3)0.0397 (4)0.1341 (3)0.0286 (9)
C110.1124 (4)0.1333 (5)0.0874 (4)0.036 (1)
C120.0086 (4)0.1352 (4)0.0805 (3)0.034 (1)
C130.0555 (3)0.0426 (4)0.1211 (3)0.0249 (8)
C140.1139 (3)0.1509 (4)0.2305 (3)0.0226 (8)
C150.1696 (3)0.0311 (4)0.1126 (3)0.0267 (9)
C160.023 (1)0.401 (1)0.2188 (9)0.179 (8)
C170.107 (2)0.340 (1)0.2731 (10)0.151 (5)
H10.13820.19380.43110.0633*
H30.12200.35070.62050.0520*
H40.12160.16370.69330.0660*
H50.12610.01470.60900.0527*
H9A0.33860.08640.40280.2247*
H9B0.38930.16410.35410.2247*
H100.22110.03550.13800.0357*
H10A0.00560.31400.13560.2247*
H10B0.08370.34240.08950.2247*
H110.15660.19480.06080.0451*
H120.01810.19760.04920.0422*
H12A0.59590.01190.98890.2247*
H12B0.66620.07950.97860.2247*
H130.11780.38440.39440.0955*
H13A0.31850.14380.06730.2247*
H13B0.34040.24670.01970.2247*
H16A0.01060.47650.24790.2217*
H16B0.03930.41780.15940.2217*
H16C0.03810.35130.21250.2217*
H17A0.17050.38400.26600.1872*
H17B0.11280.26080.24480.1872*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.0159 (1)0.0202 (1)0.0222 (1)0.00145 (9)0.00523 (8)0.00013 (9)
O10.056 (2)0.027 (2)0.034 (2)0.000 (2)0.010 (2)0.008 (1)
O20.048 (2)0.024 (2)0.031 (2)0.004 (1)0.011 (1)0.002 (1)
O30.054 (2)0.026 (2)0.049 (2)0.001 (2)0.013 (2)0.010 (2)
O40.046 (2)0.028 (2)0.032 (2)0.004 (1)0.010 (1)0.001 (1)
O50.016 (1)0.040 (2)0.043 (2)0.004 (1)0.010 (1)0.008 (1)
O60.017 (1)0.035 (2)0.035 (2)0.000 (1)0.005 (1)0.009 (1)
O70.034 (2)0.041 (2)0.058 (2)0.003 (2)0.021 (2)0.018 (2)
O80.024 (1)0.034 (2)0.042 (2)0.006 (1)0.015 (1)0.016 (1)
O90.024 (2)0.054 (2)0.048 (2)0.001 (2)0.003 (1)0.025 (2)
O100.028 (2)0.042 (2)0.044 (2)0.002 (1)0.003 (1)0.017 (2)
O110.102 (4)0.032 (2)0.055 (3)0.003 (2)0.008 (3)0.006 (2)
O120.052 (2)0.056 (3)0.083 (3)0.004 (2)0.035 (2)0.026 (2)
O130.030 (2)0.042 (2)0.040 (2)0.005 (1)0.009 (1)0.001 (2)
N10.023 (2)0.025 (2)0.029 (2)0.000 (1)0.007 (1)0.003 (1)
N20.019 (2)0.023 (2)0.026 (2)0.000 (1)0.007 (1)0.001 (1)
C20.026 (2)0.029 (2)0.028 (2)0.004 (2)0.007 (2)0.000 (2)
C30.053 (3)0.047 (3)0.027 (2)0.004 (2)0.013 (2)0.003 (2)
C40.075 (4)0.057 (4)0.029 (3)0.003 (3)0.016 (3)0.007 (2)
C50.051 (3)0.043 (3)0.034 (3)0.001 (2)0.012 (2)0.014 (2)
C60.022 (2)0.028 (2)0.034 (2)0.000 (2)0.007 (2)0.010 (2)
C70.028 (2)0.023 (2)0.028 (2)0.003 (2)0.003 (2)0.003 (2)
C80.028 (2)0.024 (2)0.039 (2)0.004 (2)0.008 (2)0.009 (2)
C90.016 (2)0.024 (2)0.024 (2)0.001 (1)0.003 (1)0.001 (2)
C100.018 (2)0.031 (2)0.037 (2)0.003 (2)0.004 (2)0.001 (2)
C110.025 (2)0.032 (2)0.049 (3)0.005 (2)0.002 (2)0.014 (2)
C120.032 (2)0.030 (2)0.039 (3)0.000 (2)0.007 (2)0.010 (2)
C130.024 (2)0.023 (2)0.029 (2)0.004 (2)0.007 (2)0.000 (2)
C140.017 (2)0.026 (2)0.026 (2)0.001 (2)0.007 (1)0.003 (2)
C150.024 (2)0.030 (2)0.028 (2)0.004 (2)0.009 (2)0.004 (2)
C160.32 (2)0.071 (7)0.103 (8)0.015 (10)0.09 (1)0.012 (6)
C170.23 (2)0.095 (9)0.12 (1)0.04 (1)0.01 (1)0.022 (7)
Geometric parameters (Å, º) top
La1—O22.499 (3)N1—C21.334 (6)
La1—O42.615 (3)N1—C61.338 (6)
La1—O5i2.511 (3)N2—C91.341 (5)
La1—O62.586 (3)N2—C131.340 (6)
La1—O82.557 (4)C2—C31.385 (7)
La1—O92.549 (3)C2—C71.506 (6)
La1—O102.511 (4)C3—C41.383 (9)
La1—N12.681 (4)C3—H30.929
La1—N22.659 (3)C4—C51.388 (8)
O1—C71.250 (6)C4—H40.929
O2—C71.261 (6)C5—C61.364 (7)
O3—C81.291 (6)C5—H50.930
O3—H10.820C6—C81.497 (7)
O4—C81.229 (6)C9—C101.386 (6)
O5—C141.251 (5)C9—C141.510 (6)
O6—C141.267 (5)C10—C111.384 (7)
O7—C151.248 (6)C10—H100.930
O8—C151.266 (5)C11—C121.375 (7)
O9—H9A0.820C11—H110.930
O9—H9B0.817C12—C131.387 (6)
O10—H10A0.823C12—H120.929
O10—H10B0.819C13—C151.520 (6)
O11—C171.41 (2)C16—C171.41 (2)
O11—H130.820C16—H16A0.961
O12—H12A0.808C16—H16B0.961
O12—H12B0.809C16—H16C0.957
O13—H13A0.804C17—H17A0.986
O13—H13B0.804C17—H17B0.977
La1···O42.615 (3)O5···O13vii3.238 (5)
La1···O5i2.511 (3)O5···O8vii3.251 (4)
La1···O62.586 (3)O6···O9vii2.778 (5)
La1···O82.557 (4)O6···O13vii3.547 (5)
La1···O92.549 (3)O7···O12viii2.741 (6)
La1···O102.511 (4)O7···O13ix2.865 (5)
La1···N12.681 (4)O7···C10x3.400 (6)
La1···N22.659 (3)O10···O12xi2.660 (6)
O1···O11ii2.644 (6)O10···O13vii2.789 (5)
O1···O9iii2.770 (5)O10···C16ii3.43 (1)
O1···C8iii3.157 (6)O11···C7xii3.321 (6)
O1···C6iii3.180 (6)O11···C3vi3.323 (9)
O1···O3iii3.432 (5)O11···C4v3.417 (9)
O1···O1iv3.513 (8)O11···C3v3.521 (8)
O1···C5iii3.538 (7)O11···C4vi3.526 (9)
O1···C17ii3.56 (1)O11···C5v3.582 (8)
O2···O11ii3.279 (5)O12···O13viii2.883 (6)
O2···C17ii3.28 (1)O12···O12xiii3.247 (9)
O2···C16ii3.33 (1)O12···C16iii3.39 (1)
O2···C5iii3.574 (6)O12···C15viii3.505 (7)
O3···C7v3.167 (6)O12···C10xiv3.551 (6)
O3···C2v3.188 (6)O13···C12xv3.566 (6)
O3···C4vi3.392 (8)O13···C11x3.586 (6)
O3···C5vi3.413 (7)C4···C17iii3.55 (2)
O3···C3v3.549 (8)C5···C8vi3.391 (7)
O3···O9v3.572 (5)C7···C8iii3.382 (6)
O5···O9vii2.925 (5)C11···C15x3.446 (7)
O5···O10vii2.961 (4)C12···C13x3.539 (6)
O2—La1—O4121.0 (1)C9—N2—C13118.3 (3)
O2—La1—O5i75.8 (1)N1—C2—C3122.0 (4)
O2—La1—O675.7 (1)N1—C2—C7115.0 (4)
O2—La1—O8155.2 (1)C3—C2—C7123.1 (4)
O2—La1—O996.0 (1)C2—C3—C4118.3 (5)
O2—La1—O1083.8 (1)C2—C3—H3120.8
O2—La1—N161.2 (1)C4—C3—H3120.9
O2—La1—N2135.1 (1)C3—C4—C5119.8 (5)
O4—La1—O5i140.4 (1)C3—C4—H4120.0
O4—La1—O683.3 (1)C5—C4—H4120.2
O4—La1—O881.4 (1)C4—C5—C6117.9 (5)
O4—La1—O972.0 (1)C4—C5—H5121.0
O4—La1—O10139.6 (1)C6—C5—H5121.1
O4—La1—N160.0 (1)N1—C6—C5123.1 (4)
O4—La1—N266.71 (10)N1—C6—C8113.2 (4)
O5i—La1—O6136.10 (10)C5—C6—C8123.7 (4)
O5i—La1—O879.8 (1)O1—C7—O2124.4 (4)
O5i—La1—O970.6 (1)O1—C7—C2118.8 (4)
O5i—La1—O1072.2 (1)O2—C7—C2116.9 (4)
O5i—La1—N1120.1 (1)O3—C8—O4125.4 (4)
O5i—La1—N2129.2 (1)O3—C8—C6114.4 (4)
O6—La1—O8120.69 (10)O4—C8—C6120.2 (4)
O6—La1—O9145.2 (1)N2—C9—C10123.0 (4)
O6—La1—O1072.1 (1)N2—C9—C14114.7 (3)
O6—La1—N172.0 (1)C10—C9—C14122.3 (4)
O6—La1—N260.7 (1)C9—C10—C11117.9 (4)
O8—La1—O980.2 (1)C9—C10—H10121.0
O8—La1—O1084.3 (1)C11—C10—H10121.1
O8—La1—N1138.6 (1)C10—C11—C12119.8 (4)
O8—La1—N260.6 (1)C10—C11—H11120.1
O9—La1—O10141.7 (1)C12—C11—H11120.1
O9—La1—N174.5 (1)C11—C12—C13118.8 (5)
O9—La1—N2125.7 (1)C11—C12—H12120.6
O10—La1—N1134.6 (1)C13—C12—H12120.6
O10—La1—N273.4 (1)N2—C13—C12122.2 (4)
N1—La1—N2110.7 (1)N2—C13—C15114.5 (4)
La1—O2—C7127.8 (3)C12—C13—C15123.3 (4)
C8—O3—H1109.5O5—C14—O6125.4 (4)
La1—O4—C8124.6 (3)O5—C14—C9118.0 (3)
La1vii—O5—C14145.9 (3)O6—C14—C9116.5 (4)
La1—O6—C14125.6 (3)O7—C15—O8126.5 (4)
La1—O8—C15125.5 (3)O7—C15—C13117.6 (4)
La1—O9—H9A120.0O8—C15—C13116.0 (4)
La1—O9—H9B126.2C17—C16—H16A109.1
H9A—O9—H9B112.8C17—C16—H16B110.0
La1—O10—H10A108.2C17—C16—H16C109.2
La1—O10—H10B137.8H16A—C16—H16B109.3
H10A—O10—H10B111.7H16A—C16—H16C109.6
C17—O11—H13109.3H16B—C16—H16C109.6
H12A—O12—H12B118.1O11—C17—C16123 (1)
H13A—O13—H13B119.7O11—C17—H17A106.2
La1—N1—C2119.1 (3)O11—C17—H17B106.7
La1—N1—C6121.8 (3)C16—C17—H17A106.8
C2—N1—C6118.9 (4)C16—C17—H17B107.1
La1—N2—C9121.1 (3)H17A—C17—H17B104.8
La1—N2—C13119.8 (3)
La1—O2—C7—O1177.8 (3)O8—La1—O2—C7145.9 (3)
La1—O2—C7—C21.2 (6)O8—La1—O4—C8160.0 (4)
La1—O4—C8—O3176.7 (3)O8—La1—O6—C144.3 (4)
La1—O4—C8—C64.3 (6)O8—La1—N1—C2157.1 (3)
La1—O6—C14—O5170.3 (3)O8—La1—N1—C619.0 (4)
La1—O6—C14—C911.2 (5)O8—La1—N2—C9174.8 (3)
La1—O8—C15—O7164.1 (4)O8—La1—N2—C1315.4 (3)
La1—O8—C15—C1316.6 (5)O8—C15—C13—N20.4 (6)
La1—N1—C2—C3177.1 (4)O8—C15—C13—C12177.8 (4)
La1—N1—C2—C74.1 (5)O9—La1—O2—C766.2 (4)
La1—N1—C6—C5176.0 (4)O9—La1—O4—C877.6 (4)
La1—N1—C6—C84.4 (5)O9—La1—O6—C14116.1 (3)
La1—N2—C9—C10169.2 (3)O9—La1—O8—C15124.1 (3)
La1—N2—C9—C149.8 (4)O9—La1—N1—C2102.8 (3)
La1—N2—C13—C12167.5 (3)O9—La1—N1—C673.4 (3)
La1—N2—C13—C1514.3 (5)O9—La1—N2—C9135.5 (3)
O1—C7—C2—N1178.8 (4)O9—La1—N2—C1334.3 (4)
O1—C7—C2—C30.1 (7)O10—La1—O2—C7152.3 (4)
O2—La1—O4—C88.5 (4)O10—La1—O4—C8129.4 (3)
O2—La1—O6—C14164.0 (3)O10—La1—O6—C1476.0 (3)
O2—La1—O8—C15152.8 (3)O10—La1—O8—C1591.1 (3)
O2—La1—N1—C23.3 (3)O10—La1—N1—C247.6 (4)
O2—La1—N1—C6179.5 (3)O10—La1—N1—C6136.2 (3)
O2—La1—N2—C919.3 (4)O10—La1—N2—C982.0 (3)
O2—La1—N2—C13170.9 (3)O10—La1—N2—C13108.2 (3)
O2—C7—C2—N12.2 (6)N1—La1—O2—C72.3 (3)
O2—C7—C2—C3179.1 (5)N1—La1—O4—C84.5 (3)
O3—C8—C6—N1178.9 (4)N1—La1—O6—C14132.1 (3)
O3—C8—C6—C50.7 (6)N1—La1—O8—C1571.5 (4)
O4—La1—O2—C76.3 (4)N1—La1—N2—C950.1 (3)
O4—La1—O6—C1471.6 (3)N1—La1—N2—C13119.7 (3)
O4—La1—O8—C1551.1 (3)N1—C2—C3—C41.6 (8)
O4—La1—N1—C2179.4 (3)N1—C6—C5—C40.3 (8)
O4—La1—N1—C64.5 (3)N2—La1—O2—C793.4 (4)
O4—La1—N2—C991.9 (3)N2—La1—O4—C8138.4 (4)
O4—La1—N2—C1377.9 (3)N2—La1—O6—C144.6 (3)
O4—C8—C6—N10.2 (6)N2—La1—O8—C1517.0 (3)
O4—C8—C6—C5179.8 (5)N2—La1—N1—C2134.3 (3)
O5—La1vii—O2vii—C7vii134.5 (4)N2—La1—N1—C649.5 (3)
O5—La1vii—O4vii—C8vii97.6 (4)N2—C9—C10—C111.4 (7)
O5—La1vii—O6vii—C14vii113.0 (3)N2—C13—C12—C112.2 (7)
O5—La1vii—O8vii—C15vii164.0 (3)C2—N1—C6—C50.1 (7)
O5—La1vii—N1vii—C2vii46.8 (3)C2—N1—C6—C8179.4 (4)
O5—La1vii—N1vii—C6vii129.4 (3)C2—C3—C4—C51.3 (9)
O5—La1vii—N2vii—C9vii131.1 (3)C3—C2—N1—C60.9 (7)
O5—La1vii—N2vii—C13vii59.1 (3)C3—C4—C5—C60.4 (9)
O5—C14—C9—N2168.0 (4)C4—C3—C2—C7179.8 (5)
O5—C14—C9—C1013.0 (6)C4—C5—C6—C8179.2 (5)
O6—La1—O2—C779.3 (4)C6—N1—C2—C7179.6 (4)
O6—La1—O4—C877.5 (4)C9—N2—C13—C122.6 (6)
O6—La1—O8—C1525.9 (4)C9—N2—C13—C15175.6 (4)
O6—La1—N1—C286.6 (3)C9—C10—C11—C121.9 (7)
O6—La1—N1—C697.2 (3)C10—C9—N2—C130.8 (6)
O6—La1—N2—C93.6 (3)C10—C11—C12—C130.2 (7)
O6—La1—N2—C13173.4 (3)C11—C10—C9—C14177.5 (4)
O6—C14—C9—N213.4 (5)C11—C12—C13—C15175.9 (4)
O6—C14—C9—C10165.7 (4)C13—N2—C9—C14179.8 (4)
O7—C15—C13—N2179.8 (4)C13—N2—C9—C14179.8 (4)
O7—C15—C13—C121.6 (6)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x, y+1, z; (iii) x+1/2, y+1/2, z+1; (iv) x, y+1, z+1; (v) x+1/2, y1/2, z+1; (vi) x, y, z+1; (vii) x1/2, y+1/2, z; (viii) x+1, y, z+1; (ix) x+1/2, y1/2, z; (x) x, y, z; (xi) x1/2, y+1/2, z1; (xii) x, y1, z; (xiii) x+1, y, z+2; (xiv) x+1, y, z+1; (xv) x+1/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula[La(C7H4NO4)(C7H3NO4)(H2O)2]·2H2O·C2H6O
Mr588.26
Crystal system, space groupMonoclinic, P21/a
Temperature (K)296
a, b, c (Å)13.037 (4), 11.003 (3), 14.851 (3)
β (°) 100.12 (2)
V3)2097.2 (10)
Z4
Radiation typeMo Kα
µ (mm1)2.11
Crystal size (mm)0.20 × 0.10 × 0.10
Data collection
DiffractometerRigaku AFC-5R
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.773, 0.810
No. of measured, independent and
observed [I > 2σ(I)] reflections
5275, 4811, 3623
Rint0.025
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.109, 0.80
No. of reflections4811
No. of parameters289
No. of restraints?
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.98, 0.91

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation and Rigaku, 1999), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation and Rigaku, 1999), SHELXS97 (Sheldrick, 1997) and DIRDIF94 (Beurskens et al., 1994), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), TEXSAN.

Selected geometric parameters (Å, º) top
La1—O22.499 (3)N1—C21.334 (6)
La1—O42.615 (3)N1—C61.338 (6)
La1—O5i2.511 (3)N2—C91.341 (5)
La1—O62.586 (3)N2—C131.340 (6)
La1—O82.557 (4)C2—C31.385 (7)
La1—O92.549 (3)C2—C71.506 (6)
La1—O102.511 (4)C3—C41.383 (9)
La1—N12.681 (4)C4—C51.388 (8)
La1—N22.659 (3)C5—C61.364 (7)
O1—C71.250 (6)C6—C81.497 (7)
O2—C71.261 (6)C9—C101.386 (6)
O3—C81.291 (6)C9—C141.510 (6)
O4—C81.229 (6)C10—C111.384 (7)
O5—C141.251 (5)C11—C121.375 (7)
O6—C141.267 (5)C12—C131.387 (6)
O7—C151.248 (6)C13—C151.520 (6)
O8—C151.266 (5)C16—C171.41 (2)
O11—C171.41 (2)
O2—La1—O4121.0 (1)O5i—La1—N1120.1 (1)
O2—La1—O5i75.8 (1)O5i—La1—N2129.2 (1)
O2—La1—O675.7 (1)O6—La1—O8120.69 (10)
O2—La1—O8155.2 (1)O6—La1—O9145.2 (1)
O2—La1—O996.0 (1)O6—La1—O1072.1 (1)
O2—La1—O1083.8 (1)O6—La1—N172.0 (1)
O2—La1—N161.2 (1)O6—La1—N260.7 (1)
O2—La1—N2135.1 (1)O8—La1—O980.2 (1)
O4—La1—O5i140.4 (1)O8—La1—O1084.3 (1)
O4—La1—O683.3 (1)O8—La1—N1138.6 (1)
O4—La1—O881.4 (1)O8—La1—N260.6 (1)
O4—La1—O972.0 (1)O9—La1—O10141.7 (1)
O4—La1—O10139.6 (1)O9—La1—N174.5 (1)
O4—La1—N160.0 (1)O9—La1—N2125.7 (1)
O4—La1—N266.71 (10)O10—La1—N1134.6 (1)
O5i—La1—O6136.10 (10)O10—La1—N273.4 (1)
O5i—La1—O879.8 (1)N1—La1—N2110.7 (1)
O5i—La1—O970.6 (1)La1—O2—C7127.8 (3)
O5i—La1—O1072.2 (1)
Symmetry code: (i) x+1/2, y+1/2, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds