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Each La3+ ion in the title complex, tetra-μ-2-fluorobenzoato-κ10O:O′;O:O,O′;O:O′;O,O′:O′-bis[aqua(4,4′-bipy­ridine-κN)(2-fluorobenzoato-κO)lanthanum(II)], [La(C7H4FO2)6(C10H8N2)2(H2O)2], is coordinated by six O atoms from the carboxyl­ate groups of five 2-fluoro­benzoate ligands, one O atom from a water mol­ecule and one N atom from a 4,4′-bi­pyridine mol­ecule, thus forming a dimeric mol­ecule. An infinite one-dimensional dimeric supramolecular chain is formed via intermolecular hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103029470/av1158sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103029470/av1158Isup2.hkl
Contains datablock I

CCDC reference: 235313

Comment top

Rare earth carboxylate complexes with aromatic diamines, such as 1,10-phenanthroline and 2,2'-bipyridine, have been studied extensively. These lanthanide complexes display a variety of structural types, high stability and intense fluorescence characteristics. However, few rare earth carboxylate complexes with 4,4'-bipyridine have been reported. This paper reports the structure of the title complex, determined by single-crystal X-ray diffraction analysis.

Each La3+ ion is coordinated by seven O atoms and one N atom from a 4,4'-bipyridine molecule, where six of the O atoms (O1, O1A, O2A, O3, O4A and O5) are from different 2-fluorobenzoate groups and the seventh (O7) is from the water molecule. Carboxylate groups adopt three coordination modes, viz. unidentate, bidentate-bridging and bidentate-chelating. Two La3+ ions form a dimeric molecule with four bridging carboxylate groups. The O5/C15/O6 carboxylate groups are in the unidentate mode, with one atom (O5) coordinated to the La3+ ion. The O3/C8/O4 groups are in the bridging mode, in which two O atoms coordinate to two different La3+ ions. The O1/C1/O2 groups are in the chelating-bridging mode, in which two O atoms chelate one La3+ ion and one of the O atoms is linked to another La3+ ion. La—Ocarboxy distances in the title complex range from 2.471 (2) to 2.942 (3) Å [mean 2.569 Å]. The O—La—O angles range from 71.51 (9) to 143.64 (8)°. One N atom from a 4,4'-bipyridine molecule is coordinated to the La3+ ion; this conformation contrasts with that of the [Eu(DBM)3.1/2(4,4'-bipy)] complex, in which two N atoms from 4,4'-bipyridine link two Eu3+ ions to result in an infinite polymeric chain (Wang et al., 1995). The La1—N1 bond distance is 2.852 (3) Å. Each La3+ ion is also coordinated by a water molecule, the La—Owater bond distance being 2.572 (3) Å.

Hydrogen bonds exist between two dimeric molecules, involving the non-coordinated N atom of the 4,4'-bipyridine group of one dimeric molecule and the H atom of the coordinated water molecule of another dimer. (O—H···N = 2.019 Å and O—H···N = 167.9°). An infinite one-dimensional dimeric supramolecular chain is formed, linked by the hydrogen bonds.

Experimental top

LaCl3·6H2O (0.5 mmol), 2-fluorobenzoic acid (1.5 mmol) and 4,4'-bipyridine (0.5 mmol) were dissolved separately in appropriate amounts of ethanol. The ethanol solution of 2-fluorobenzoic acid was controlled to pH 6–7 with an aqueous solution of NaOH (2 mol dm−3), and then the ethanol solutions of 4,4'-bipyridine and LaCl3 were added dropwise. The mixture was heated under reflux with stirring for 2 h, and the resulting white minor precipitate was filtered off. Single crystals were obtained from the mother liquor after one month at room temperature.

Refinement top

H atoms were placed at calculated positions, with C—H distances of 0.93 Å and O—Hwater distance of 0.85 Å. Please check computer programs used.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART); data reduction: SAINT (Bruker, 1997; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of complex (I), with the atom-numbering scheme. Displacement ellipsoids are shown at the 30% probability level.
Diaquatris-bis[(µ-2-Fluorobenzoato-o,o':o')(µ-2-Fluorobenzoato-o,o' (2-Fluorobenzoato-o)(4,4'-bipyridine-N)-lanthanum(III)] top
Crystal data top
[La(C7H4FO2)6(C10H8N2)2(H2O)2]Z = 2
Mr = 730.42F(000) = 724
Triclinic, P1Dx = 1.698 Mg m3
a = 9.746 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.780 (7) ÅCell parameters from 986 reflections
c = 13.315 (7) Åθ = 3.2–28.0°
α = 113.132 (9)°µ = 1.57 mm1
β = 104.763 (9)°T = 293 K
γ = 96.916 (9)°Prism, white
V = 1428.6 (13) Å30.20 × 0.18 × 0.12 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
6871 independent reflections
Radiation source: fine-focus sealed tube5931 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ϕ and ω scansθmax = 28.4°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1213
Tmin = 0.728, Tmax = 0.834k = 1516
13305 measured reflectionsl = 1716
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0392P)2]
where P = (Fo2 + 2Fc2)/3
6871 reflections(Δ/σ)max = 0.002
397 parametersΔρmax = 0.77 e Å3
0 restraintsΔρmin = 1.02 e Å3
Crystal data top
[La(C7H4FO2)6(C10H8N2)2(H2O)2]γ = 96.916 (9)°
Mr = 730.42V = 1428.6 (13) Å3
Triclinic, P1Z = 2
a = 9.746 (5) ÅMo Kα radiation
b = 12.780 (7) ŵ = 1.57 mm1
c = 13.315 (7) ÅT = 293 K
α = 113.132 (9)°0.20 × 0.18 × 0.12 mm
β = 104.763 (9)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
6871 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5931 reflections with I > 2σ(I)
Tmin = 0.728, Tmax = 0.834Rint = 0.032
13305 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.080H-atom parameters constrained
S = 1.08Δρmax = 0.77 e Å3
6871 reflectionsΔρmin = 1.02 e Å3
397 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
La10.270721 (16)0.462748 (14)0.474272 (14)0.01955 (6)
C10.5566 (3)0.7307 (3)0.5589 (3)0.0267 (6)
C20.4994 (3)0.8372 (3)0.5770 (3)0.0267 (6)
C30.5894 (4)0.9501 (3)0.6337 (3)0.0356 (8)
C40.5366 (4)1.0488 (3)0.6504 (4)0.0454 (9)
H40.60031.12320.68860.055*
C50.3877 (5)1.0351 (4)0.6096 (4)0.0504 (10)
H50.35001.10070.62010.061*
C60.2943 (4)0.9246 (4)0.5532 (4)0.0489 (10)
H60.19370.91570.52560.059*
C70.3493 (3)0.8275 (3)0.5378 (3)0.0374 (8)
H70.28490.75350.50020.045*
C80.5667 (3)0.4954 (3)0.7183 (3)0.0260 (6)
C90.5893 (3)0.4608 (3)0.8161 (3)0.0277 (7)
C100.7051 (4)0.5192 (4)0.9196 (3)0.0411 (9)
C110.7232 (5)0.4870 (4)1.0083 (4)0.0556 (11)
H110.80090.52941.07720.067*
C120.6252 (5)0.3915 (4)0.9941 (4)0.0574 (12)
H120.63760.36801.05300.069*
C130.5093 (5)0.3307 (4)0.8935 (4)0.0588 (12)
H130.44320.26590.88420.071*
C140.4903 (4)0.3657 (3)0.8054 (3)0.0422 (9)
H140.41010.32490.73810.051*
C150.0091 (3)0.6065 (3)0.4011 (3)0.0234 (6)
C160.0020 (3)0.6741 (3)0.3320 (3)0.0255 (6)
C170.0702 (4)0.7648 (3)0.3408 (3)0.0376 (8)
C180.0586 (5)0.8265 (4)0.2762 (4)0.0523 (11)
H180.10550.88690.28290.063*
C190.0215 (5)0.7987 (4)0.2027 (4)0.0499 (10)
H190.02920.84020.15980.060*
C200.0906 (4)0.7093 (4)0.1927 (3)0.0463 (9)
H200.14530.69050.14300.056*
C210.0791 (3)0.6470 (3)0.2561 (3)0.0332 (7)
H210.12580.58640.24820.040*
C220.0008 (4)0.2862 (3)0.1763 (3)0.0398 (8)
H220.03150.35670.17440.048*
C230.1093 (4)0.1992 (3)0.0790 (3)0.0421 (9)
H230.14830.21200.01460.050*
C240.1592 (4)0.0927 (3)0.0788 (3)0.0355 (8)
C250.0939 (4)0.0806 (3)0.1780 (4)0.0469 (10)
H250.12280.01060.18190.056*
C260.0135 (4)0.1721 (3)0.2707 (3)0.0444 (9)
H260.05590.16140.33580.053*
C270.5196 (4)0.0661 (4)0.1615 (3)0.0477 (10)
H270.59660.04690.20270.057*
C280.3986 (4)0.0242 (3)0.0806 (3)0.0422 (9)
H280.39530.10130.06890.051*
C290.2835 (4)0.0022 (3)0.0179 (3)0.0393 (8)
C300.2942 (5)0.1199 (4)0.0431 (4)0.0616 (13)
H300.21820.14260.00510.074*
C310.4198 (5)0.2026 (4)0.1256 (4)0.0678 (14)
H310.42540.28080.14120.081*
F10.7359 (2)0.9671 (2)0.6771 (3)0.0684 (8)
F20.8003 (3)0.6157 (3)0.9376 (2)0.0808 (10)
F30.1461 (3)0.8002 (3)0.4148 (3)0.0728 (8)
N10.0599 (3)0.2759 (2)0.2716 (2)0.0344 (6)
N20.5319 (4)0.1780 (3)0.1835 (3)0.0544 (9)
O10.4742 (3)0.63668 (19)0.5411 (2)0.0348 (5)
O20.6865 (2)0.7367 (2)0.5615 (2)0.0451 (7)
O30.4358 (2)0.4812 (2)0.6617 (2)0.0367 (6)
O40.6770 (2)0.5342 (2)0.69945 (19)0.0334 (5)
O50.0632 (2)0.5309 (2)0.3915 (2)0.0323 (5)
O60.0876 (2)0.6291 (2)0.4651 (2)0.0323 (5)
O70.2306 (2)0.6321 (2)0.6405 (2)0.0421 (6)
H7A0.29300.69520.69150.063*
H7B0.14870.62920.65210.063*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.01654 (8)0.02040 (9)0.02189 (9)0.00551 (6)0.00559 (6)0.00969 (7)
C10.0306 (15)0.0216 (15)0.0230 (16)0.0047 (12)0.0033 (12)0.0089 (13)
C20.0269 (14)0.0245 (16)0.0282 (16)0.0079 (12)0.0075 (12)0.0117 (13)
C30.0313 (16)0.0267 (17)0.044 (2)0.0072 (13)0.0090 (14)0.0131 (15)
C40.051 (2)0.0247 (18)0.054 (2)0.0108 (16)0.0135 (18)0.0133 (17)
C50.059 (2)0.039 (2)0.057 (3)0.0292 (19)0.018 (2)0.022 (2)
C60.0383 (19)0.049 (2)0.055 (3)0.0221 (18)0.0062 (17)0.021 (2)
C70.0288 (16)0.0347 (19)0.040 (2)0.0079 (14)0.0034 (14)0.0125 (16)
C80.0284 (14)0.0274 (16)0.0214 (15)0.0094 (12)0.0086 (12)0.0091 (13)
C90.0293 (15)0.0324 (17)0.0234 (16)0.0127 (13)0.0103 (12)0.0118 (13)
C100.0366 (18)0.052 (2)0.0305 (19)0.0040 (16)0.0062 (15)0.0192 (17)
C110.055 (2)0.080 (3)0.031 (2)0.014 (2)0.0047 (18)0.030 (2)
C120.076 (3)0.079 (3)0.049 (3)0.037 (3)0.031 (2)0.048 (3)
C130.067 (3)0.060 (3)0.070 (3)0.015 (2)0.029 (2)0.044 (3)
C140.0419 (19)0.043 (2)0.043 (2)0.0046 (16)0.0116 (16)0.0242 (18)
C150.0173 (12)0.0259 (16)0.0243 (15)0.0041 (11)0.0018 (11)0.0120 (13)
C160.0228 (13)0.0277 (16)0.0269 (16)0.0053 (12)0.0033 (12)0.0164 (13)
C170.0377 (17)0.043 (2)0.044 (2)0.0172 (16)0.0159 (16)0.0272 (18)
C180.063 (3)0.052 (3)0.068 (3)0.027 (2)0.024 (2)0.047 (2)
C190.058 (2)0.056 (3)0.051 (2)0.010 (2)0.016 (2)0.042 (2)
C200.049 (2)0.058 (3)0.041 (2)0.0101 (19)0.0191 (18)0.029 (2)
C210.0334 (16)0.0365 (19)0.0333 (18)0.0093 (14)0.0122 (14)0.0180 (15)
C220.0447 (19)0.035 (2)0.0325 (19)0.0035 (15)0.0073 (15)0.0145 (16)
C230.045 (2)0.044 (2)0.0290 (19)0.0007 (16)0.0064 (15)0.0156 (17)
C240.0330 (16)0.0293 (18)0.0322 (19)0.0047 (14)0.0066 (14)0.0052 (15)
C250.046 (2)0.0275 (19)0.053 (2)0.0004 (16)0.0043 (18)0.0187 (18)
C260.0420 (19)0.034 (2)0.042 (2)0.0015 (16)0.0069 (16)0.0177 (17)
C270.043 (2)0.055 (3)0.028 (2)0.0016 (18)0.0034 (16)0.0098 (18)
C280.045 (2)0.043 (2)0.0271 (19)0.0019 (16)0.0065 (15)0.0100 (16)
C290.0357 (17)0.0340 (19)0.0337 (19)0.0030 (15)0.0069 (14)0.0050 (15)
C300.046 (2)0.037 (2)0.067 (3)0.0091 (18)0.002 (2)0.003 (2)
C310.062 (3)0.027 (2)0.071 (3)0.0022 (19)0.003 (2)0.007 (2)
F10.0302 (11)0.0322 (12)0.115 (2)0.0022 (9)0.0051 (12)0.0180 (13)
F20.0689 (17)0.093 (2)0.0478 (16)0.0325 (15)0.0131 (13)0.0336 (15)
F30.0911 (19)0.083 (2)0.102 (2)0.0613 (17)0.0645 (18)0.0655 (18)
N10.0325 (14)0.0311 (16)0.0324 (16)0.0024 (12)0.0055 (12)0.0117 (13)
N20.051 (2)0.049 (2)0.0313 (18)0.0053 (16)0.0070 (15)0.0042 (15)
O10.0450 (13)0.0224 (11)0.0365 (13)0.0027 (10)0.0174 (11)0.0115 (10)
O20.0258 (11)0.0282 (13)0.0698 (19)0.0080 (10)0.0063 (12)0.0159 (13)
O30.0274 (11)0.0529 (16)0.0337 (13)0.0130 (10)0.0072 (10)0.0238 (12)
O40.0283 (11)0.0468 (15)0.0255 (12)0.0056 (10)0.0085 (9)0.0178 (11)
O50.0352 (11)0.0376 (13)0.0368 (13)0.0206 (10)0.0148 (10)0.0236 (11)
O60.0308 (11)0.0343 (13)0.0435 (14)0.0128 (9)0.0202 (10)0.0226 (11)
O70.0297 (11)0.0370 (14)0.0438 (15)0.0060 (10)0.0160 (11)0.0007 (11)
Geometric parameters (Å, º) top
La1—O52.471 (2)C15—O61.260 (4)
La1—O12.480 (2)C15—C161.497 (4)
La1—O6i2.488 (2)C16—C171.384 (5)
La1—O32.504 (2)C16—C211.402 (4)
La1—O4ii2.506 (2)C17—F31.351 (4)
La1—O2ii2.510 (3)C17—C181.391 (5)
La1—O72.572 (3)C18—C191.370 (6)
La1—N12.852 (3)C18—H180.9300
La1—O1ii2.942 (3)C19—C201.374 (6)
La1—C1ii3.108 (3)C19—H190.9300
C1—O21.250 (4)C20—C211.383 (5)
C1—O11.262 (4)C20—H200.9300
C1—C21.489 (4)C21—H210.9300
C1—La1ii3.108 (3)C22—N11.321 (4)
C2—C31.386 (4)C22—C231.385 (5)
C2—C71.395 (4)C22—H220.9300
C3—F11.351 (4)C23—C241.388 (5)
C3—C41.378 (5)C23—H230.9300
C4—C51.376 (5)C24—C251.389 (5)
C4—H40.9300C24—C291.490 (5)
C5—C61.377 (6)C25—C261.378 (5)
C5—H50.9300C25—H250.9300
C6—C71.372 (5)C26—N11.343 (5)
C6—H60.9300C26—H260.9300
C7—H70.9300C27—N21.326 (6)
C8—O41.253 (4)C27—C281.389 (5)
C8—O31.255 (4)C27—H270.9300
C8—C91.507 (4)C28—C291.381 (5)
C9—C101.388 (5)C28—H280.9300
C9—C141.392 (5)C29—C301.390 (6)
C10—F21.348 (4)C30—C311.383 (6)
C10—C111.375 (5)C30—H300.9300
C11—C121.371 (6)C31—N21.315 (6)
C11—H110.9300C31—H310.9300
C12—C131.368 (6)O1—La1ii2.942 (3)
C12—H120.9300O2—La1ii2.510 (3)
C13—C141.391 (6)O4—La1ii2.506 (2)
C13—H130.9300O6—La1i2.488 (2)
C14—H140.9300O7—H7A0.8497
C15—O51.248 (4)O7—H7B0.8506
O5—La1—O199.84 (9)C12—C11—C10119.2 (4)
O5—La1—O6i83.20 (8)C12—C11—H11120.4
O1—La1—O6i143.64 (8)C10—C11—H11120.4
O5—La1—O3142.72 (8)C13—C12—C11120.3 (4)
O1—La1—O375.43 (8)C13—C12—H12119.9
O6i—La1—O380.53 (8)C11—C12—H12119.9
O5—La1—O4ii78.17 (8)C12—C13—C14120.0 (4)
O1—La1—O4ii71.69 (8)C12—C13—H13120.0
O6i—La1—O4ii143.01 (8)C14—C13—H13120.0
O3—La1—O4ii131.59 (8)C13—C14—C9121.2 (4)
O5—La1—O2ii133.53 (8)C13—C14—H14119.4
O1—La1—O2ii122.16 (8)C9—C14—H14119.4
O6i—La1—O2ii74.58 (8)O5—C15—O6124.1 (3)
O3—La1—O2ii73.03 (9)O5—C15—C16117.8 (3)
O4ii—La1—O2ii95.77 (9)O6—C15—C16118.1 (3)
O5—La1—O771.51 (9)C17—C16—C21117.7 (3)
O1—La1—O772.89 (8)C17—C16—C15123.0 (3)
O6i—La1—O773.90 (8)C21—C16—C15119.3 (3)
O3—La1—O771.81 (9)F3—C17—C16122.0 (3)
O4ii—La1—O7127.77 (9)F3—C17—C18117.0 (3)
O2ii—La1—O7135.76 (10)C16—C17—C18121.0 (3)
O5—La1—N168.32 (9)C19—C18—C17120.3 (4)
O1—La1—N1142.92 (8)C19—C18—H18119.8
O6i—La1—N171.99 (9)C17—C18—H18119.8
O3—La1—N1135.31 (9)C18—C19—C20119.8 (4)
O4ii—La1—N171.49 (9)C18—C19—H19120.1
O2ii—La1—N166.16 (9)C20—C19—H19120.1
O7—La1—N1129.38 (8)C19—C20—C21120.3 (4)
O5—La1—O1ii151.13 (7)C19—C20—H20119.9
O1—La1—O1ii76.33 (9)C21—C20—H20119.9
O6i—La1—O1ii117.06 (7)C20—C21—C16120.9 (3)
O3—La1—O1ii64.85 (8)C20—C21—H21119.5
O4ii—La1—O1ii73.46 (7)C16—C21—H21119.5
O2ii—La1—O1ii46.53 (7)N1—C22—C23124.5 (3)
O7—La1—O1ii131.64 (7)N1—C22—H22117.8
N1—La1—O1ii97.23 (8)C23—C22—H22117.8
O5—La1—C1ii148.13 (8)C22—C23—C24119.2 (4)
O1—La1—C1ii99.86 (9)C22—C23—H23120.4
O6i—La1—C1ii95.35 (9)C24—C23—H23120.4
O3—La1—C1ii67.12 (8)C23—C24—C25116.6 (3)
O4ii—La1—C1ii84.57 (8)C23—C24—C29122.9 (3)
O2ii—La1—C1ii22.67 (8)C25—C24—C29120.4 (3)
O7—La1—C1ii138.75 (9)C26—C25—C24120.1 (3)
N1—La1—C1ii80.90 (9)C26—C25—H25119.9
O1ii—La1—C1ii23.87 (7)C24—C25—H25119.9
O2—C1—O1121.3 (3)N1—C26—C25123.3 (4)
O2—C1—C2118.7 (3)N1—C26—H26118.4
O1—C1—C2120.0 (3)C25—C26—H26118.4
O2—C1—La1ii50.69 (16)N2—C27—C28123.9 (4)
O1—C1—La1ii70.64 (18)N2—C27—H27118.0
C2—C1—La1ii169.4 (2)C28—C27—H27118.0
C3—C2—C7116.4 (3)C29—C28—C27119.0 (4)
C3—C2—C1123.0 (3)C29—C28—H28120.5
C7—C2—C1120.7 (3)C27—C28—H28120.5
F1—C3—C4117.0 (3)C28—C29—C30117.2 (3)
F1—C3—C2120.0 (3)C28—C29—C24120.9 (3)
C4—C3—C2123.0 (3)C30—C29—C24121.7 (4)
C5—C4—C3118.7 (3)C31—C30—C29118.9 (4)
C5—C4—H4120.7C31—C30—H30120.6
C3—C4—H4120.7C29—C30—H30120.6
C4—C5—C6120.2 (4)N2—C31—C30124.5 (4)
C4—C5—H5119.9N2—C31—H31117.8
C6—C5—H5119.9C30—C31—H31117.8
C7—C6—C5120.1 (4)C22—N1—C26116.3 (3)
C7—C6—H6119.9C22—N1—La1123.3 (2)
C5—C6—H6119.9C26—N1—La1120.4 (2)
C6—C7—C2121.6 (3)C31—N2—C27116.5 (3)
C6—C7—H7119.2C1—O1—La1166.6 (2)
C2—C7—H7119.2C1—O1—La1ii85.49 (19)
O4—C8—O3125.7 (3)La1—O1—La1ii103.67 (9)
O4—C8—C9118.6 (3)C1—O2—La1ii106.6 (2)
O3—C8—C9115.6 (3)C8—O3—La1143.8 (2)
C10—C9—C14116.5 (3)C8—O4—La1ii135.3 (2)
C10—C9—C8123.7 (3)C15—O5—La1150.2 (2)
C14—C9—C8119.9 (3)C15—O6—La1i143.4 (2)
F2—C10—C11117.8 (3)La1—O7—H7A127.7
F2—C10—C9119.3 (3)La1—O7—H7B121.6
C11—C10—C9122.8 (4)H7A—O7—H7B110.6
O2—C1—C2—C322.4 (5)O6i—La1—N1—C22134.1 (3)
O1—C1—C2—C3157.8 (3)O3—La1—N1—C22171.0 (3)
La1ii—C1—C2—C323.9 (13)O4ii—La1—N1—C2239.9 (3)
O2—C1—C2—C7158.3 (3)O2ii—La1—N1—C22145.2 (3)
O1—C1—C2—C721.5 (5)O7—La1—N1—C2284.2 (3)
La1ii—C1—C2—C7156.8 (10)O1ii—La1—N1—C22109.8 (3)
C7—C2—C3—F1178.2 (3)C1ii—La1—N1—C22127.2 (3)
C1—C2—C3—F11.1 (5)O5—La1—N1—C26133.3 (3)
C7—C2—C3—C40.7 (5)O1—La1—N1—C26149.4 (3)
C1—C2—C3—C4180.0 (3)O6i—La1—N1—C2643.6 (3)
F1—C3—C4—C5178.6 (4)O3—La1—N1—C2611.3 (3)
C2—C3—C4—C50.3 (6)O4ii—La1—N1—C26142.4 (3)
C3—C4—C5—C60.0 (6)O2ii—La1—N1—C2637.1 (3)
C4—C5—C6—C70.2 (7)O7—La1—N1—C2693.5 (3)
C5—C6—C7—C20.6 (6)O1ii—La1—N1—C2672.6 (3)
C3—C2—C7—C60.8 (5)C1ii—La1—N1—C2655.1 (3)
C1—C2—C7—C6179.8 (4)C30—C31—N2—C271.5 (8)
O4—C8—C9—C1035.4 (5)C28—C27—N2—C311.4 (6)
O3—C8—C9—C10145.2 (3)O2—C1—O1—La1133.9 (8)
O4—C8—C9—C14144.9 (3)C2—C1—O1—La145.9 (11)
O3—C8—C9—C1434.6 (4)La1ii—C1—O1—La1133.7 (9)
C14—C9—C10—F2176.6 (4)O2—C1—O1—La1ii0.1 (3)
C8—C9—C10—F23.2 (6)C2—C1—O1—La1ii179.7 (3)
C14—C9—C10—C110.3 (6)O5—La1—O1—C118.6 (9)
C8—C9—C10—C11179.4 (4)O6i—La1—O1—C1110.5 (9)
F2—C10—C11—C12177.8 (4)O3—La1—O1—C1160.7 (9)
C9—C10—C11—C121.6 (7)O4ii—La1—O1—C155.3 (9)
C10—C11—C12—C131.3 (7)O2ii—La1—O1—C1140.6 (9)
C11—C12—C13—C140.1 (7)O7—La1—O1—C185.6 (9)
C12—C13—C14—C91.4 (7)N1—La1—O1—C148.3 (10)
C10—C9—C14—C131.1 (6)O1ii—La1—O1—C1132.2 (10)
C8—C9—C14—C13179.1 (4)C1ii—La1—O1—C1136.2 (9)
O5—C15—C16—C17176.0 (3)O5—La1—O1—La1ii150.76 (8)
O6—C15—C16—C174.1 (4)O6i—La1—O1—La1ii117.35 (11)
O5—C15—C16—C212.8 (4)O3—La1—O1—La1ii67.13 (8)
O6—C15—C16—C21177.1 (3)O4ii—La1—O1—La1ii76.81 (8)
C21—C16—C17—F3177.5 (3)O2ii—La1—O1—La1ii8.43 (12)
C15—C16—C17—F31.4 (5)O7—La1—O1—La1ii142.21 (10)
C21—C16—C17—C180.1 (5)N1—La1—O1—La1ii83.86 (14)
C15—C16—C17—C18178.9 (3)O1ii—La1—O1—La1ii0.0
F3—C17—C18—C19177.4 (4)C1ii—La1—O1—La1ii4.06 (9)
C16—C17—C18—C190.3 (6)O1—C1—O2—La1ii0.2 (4)
C17—C18—C19—C200.1 (7)C2—C1—O2—La1ii179.6 (2)
C18—C19—C20—C210.2 (6)O4—C8—O3—La118.3 (6)
C19—C20—C21—C160.4 (6)C9—C8—O3—La1161.2 (3)
C17—C16—C21—C200.2 (5)O5—La1—O3—C8135.0 (4)
C15—C16—C21—C20178.7 (3)O1—La1—O3—C847.8 (4)
N1—C22—C23—C240.5 (6)O6i—La1—O3—C8159.7 (4)
C22—C23—C24—C250.7 (6)O4ii—La1—O3—C80.5 (4)
C22—C23—C24—C29174.9 (3)O2ii—La1—O3—C883.0 (4)
C23—C24—C25—C260.6 (6)O7—La1—O3—C8124.3 (4)
C29—C24—C25—C26175.1 (4)N1—La1—O3—C8107.6 (4)
C24—C25—C26—N10.5 (7)O1ii—La1—O3—C833.7 (4)
N2—C27—C28—C290.5 (6)C1ii—La1—O3—C859.7 (4)
C27—C28—C29—C302.2 (6)O3—C8—O4—La1ii26.9 (5)
C27—C28—C29—C24173.1 (3)C9—C8—O4—La1ii152.5 (2)
C23—C24—C29—C2832.6 (5)O6—C15—O5—La169.7 (5)
C25—C24—C29—C28142.8 (4)C16—C15—O5—La1110.4 (4)
C23—C24—C29—C30152.3 (4)O1—La1—O5—C1552.3 (4)
C25—C24—C29—C3032.3 (6)O6i—La1—O5—C1591.0 (4)
C28—C29—C30—C312.2 (7)O3—La1—O5—C1526.5 (5)
C24—C29—C30—C31173.1 (4)O4ii—La1—O5—C15121.1 (4)
C29—C30—C31—N20.3 (8)O2ii—La1—O5—C15152.2 (4)
C23—C22—N1—C261.6 (6)O7—La1—O5—C1515.8 (4)
C23—C22—N1—La1176.2 (3)N1—La1—O5—C15164.3 (4)
C25—C26—N1—C221.6 (6)O1ii—La1—O5—C15131.8 (4)
C25—C26—N1—La1176.3 (3)C1ii—La1—O5—C15179.8 (4)
O5—La1—N1—C2244.3 (3)O5—C15—O6—La1i44.0 (5)
O1—La1—N1—C2232.9 (3)C16—C15—O6—La1i135.9 (3)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···N2iii0.852.022.855 (4)168
O7—H7B···O5i0.852.503.158 (4)135
C5—H5···F3iv0.932.523.379 (5)153
C26—H26···O2ii0.932.442.950 (4)115
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y+1, z+1; (iv) x, y+2, z+1.

Experimental details

Crystal data
Chemical formula[La(C7H4FO2)6(C10H8N2)2(H2O)2]
Mr730.42
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.746 (5), 12.780 (7), 13.315 (7)
α, β, γ (°)113.132 (9), 104.763 (9), 96.916 (9)
V3)1428.6 (13)
Z2
Radiation typeMo Kα
µ (mm1)1.57
Crystal size (mm)0.20 × 0.18 × 0.12
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.728, 0.834
No. of measured, independent and
observed [I > 2σ(I)] reflections
13305, 6871, 5931
Rint0.032
(sin θ/λ)max1)0.669
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.080, 1.08
No. of reflections6871
No. of parameters397
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.77, 1.02

Computer programs: SMART (Bruker, 1997), SMART), SAINT (Bruker, 1997, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···N2i0.852.022.855 (4)168
O7—H7B···O5ii0.852.503.158 (4)135
C5—H5···F3iii0.932.523.379 (5)153
C26—H26···O2iv0.932.442.950 (4)115
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y+2, z+1; (iv) x+1, y+1, z+1.
 

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