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The title compound, [La(C10H8O6)Cl(H2O)2]n, was synthesized from lanthanum(III) chloride and p-phenyl­enedioxy­diacetic acid under hydro­thermal conditions. The ligands are bridging through carboxyl­ate groups, forming a coordination polymer with ten-coordinate lanthanum(III) ions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806029473/cf2038sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806029473/cf2038Isup2.hkl
Contains datablock I

CCDC reference: 620725

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.023
  • wR factor = 0.054
  • Data-to-parameter ratio = 14.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.92 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.19 Ratio
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.918 Tmax scaled 0.477 Tmin scaled 0.327
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker,2001; data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
C10H12ClLaO8F(000) = 840
Mr = 434.56Dx = 2.221 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1554 reflections
a = 13.8892 (11) Åθ = 2.2–23.5°
b = 6.2703 (5) ŵ = 3.53 mm1
c = 14.9800 (11) ÅT = 193 K
β = 95.151 (1)°Block, colorless
V = 1299.33 (17) Å30.37 × 0.23 × 0.21 mm
Z = 4
Data collection top
Bruker APEX CCD area-detector
diffractometer
2532 independent reflections
Radiation source: fine-focus sealed tube2379 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
φ and ω scansθmax = 26.0°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1517
Tmin = 0.356, Tmax = 0.519k = 77
6619 measured reflectionsl = 1817
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.054H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0272P)2 + 0.4094P]
where P = (Fo2 + 2Fc2)/3
2532 reflections(Δ/σ)max = 0.001
181 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.79 e Å3
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
La1.138184 (11)1.09493 (3)0.436381 (10)0.01426 (7)
C10.6725 (2)1.0209 (5)0.3851 (2)0.0203 (6)
C20.6310 (2)0.8631 (5)0.43504 (19)0.0190 (7)
C30.5340 (2)0.8306 (5)0.4268 (2)0.0243 (7)
H3A0.50730.72470.46030.029*
C40.4744 (2)0.9554 (5)0.3682 (2)0.0259 (7)
H4A0.40780.93420.36290.031*
C50.5144 (3)1.1096 (6)0.3184 (2)0.0309 (8)
H5A0.47461.19310.27920.037*
C60.6145 (2)1.1432 (6)0.3257 (2)0.0286 (8)
H6A0.64151.24650.29100.034*
C70.8226 (2)1.1560 (6)0.3383 (2)0.0237 (7)
H7A0.79261.29340.32480.028*
H7B0.82161.07490.28310.028*
C80.9254 (2)1.1866 (5)0.37804 (19)0.0163 (6)
C90.6663 (2)0.5422 (5)0.5215 (2)0.0273 (7)
H9A0.63550.46680.47010.033*
H9B0.61980.55620.56570.033*
C100.7534 (2)0.4170 (5)0.5610 (2)0.0187 (6)
O10.77111 (15)1.0445 (4)0.40184 (14)0.0247 (5)
O20.98854 (15)1.2448 (4)0.32818 (14)0.0237 (5)
O30.94608 (15)1.1493 (3)0.45982 (13)0.0199 (5)
O40.69626 (14)0.7500 (3)0.49452 (14)0.0213 (5)
O50.74356 (15)0.2214 (3)0.56684 (15)0.0253 (5)
O60.82866 (15)0.5198 (4)0.58612 (15)0.0243 (5)
O1W1.11229 (16)1.3236 (4)0.57702 (14)0.0283 (5)
H1WA1.05831.31060.59840.034*
H1WB1.15791.33100.61820.034*
O2W1.05304 (14)0.7884 (3)0.34788 (13)0.0206 (5)
H2WA1.04090.77990.29110.025*
H2WB1.08950.68420.36520.025*
Cl11.23005 (6)1.14155 (14)0.27192 (5)0.02917 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La0.01447 (11)0.01393 (11)0.01391 (10)0.00159 (6)0.00138 (7)0.00132 (6)
C10.0169 (15)0.0244 (17)0.0190 (15)0.0005 (13)0.0024 (11)0.0007 (13)
C20.0152 (16)0.0206 (16)0.0203 (16)0.0023 (12)0.0037 (12)0.0015 (12)
C30.0206 (16)0.0242 (17)0.0277 (17)0.0043 (14)0.0009 (13)0.0007 (14)
C40.0120 (15)0.035 (2)0.0296 (18)0.0000 (13)0.0036 (13)0.0030 (15)
C50.0254 (18)0.036 (2)0.0289 (19)0.0064 (15)0.0082 (14)0.0061 (15)
C60.0212 (17)0.034 (2)0.0294 (19)0.0012 (14)0.0035 (14)0.0115 (15)
C70.0228 (17)0.0301 (18)0.0174 (16)0.0057 (14)0.0033 (12)0.0084 (13)
C80.0174 (15)0.0119 (15)0.0191 (15)0.0014 (12)0.0004 (11)0.0020 (12)
C90.0223 (17)0.0175 (17)0.041 (2)0.0047 (13)0.0020 (14)0.0047 (15)
C100.0222 (16)0.0149 (16)0.0189 (15)0.0000 (12)0.0015 (12)0.0006 (12)
O10.0133 (11)0.0346 (14)0.0256 (12)0.0034 (9)0.0025 (9)0.0145 (10)
O20.0187 (11)0.0318 (13)0.0205 (11)0.0029 (9)0.0005 (8)0.0055 (9)
O30.0189 (11)0.0247 (12)0.0155 (11)0.0016 (9)0.0014 (8)0.0039 (9)
O40.0159 (10)0.0201 (12)0.0266 (11)0.0031 (9)0.0046 (8)0.0094 (9)
O50.0217 (11)0.0153 (12)0.0382 (13)0.0029 (9)0.0017 (9)0.0021 (10)
O60.0231 (12)0.0188 (12)0.0297 (12)0.0014 (9)0.0050 (9)0.0025 (10)
O1W0.0241 (12)0.0352 (14)0.0258 (12)0.0031 (10)0.0029 (9)0.0084 (10)
O2W0.0222 (11)0.0225 (12)0.0163 (10)0.0024 (9)0.0032 (8)0.0017 (9)
Cl10.0342 (5)0.0314 (5)0.0224 (4)0.0004 (4)0.0052 (3)0.0025 (3)
Geometric parameters (Å, º) top
La—O6i2.488 (2)C7—O11.424 (4)
La—O3i2.541 (2)C7—C81.509 (4)
La—O5ii2.578 (2)C7—H7A0.970
La—O4i2.622 (2)C7—H7B0.970
La—O22.688 (2)C8—O31.255 (3)
La—O32.744 (2)C8—O21.256 (4)
La—O1i2.771 (2)C9—O41.436 (4)
La—O1W2.600 (2)C9—C101.517 (4)
La—O2W2.563 (2)C9—H9A0.970
La—Cl12.8892 (8)C9—H9B0.970
C1—O11.378 (4)C10—O51.238 (3)
C1—C61.378 (4)C10—O61.257 (4)
C1—C21.396 (4)O1—Lai2.771 (2)
C2—C31.357 (4)O3—Lai2.541 (2)
C2—O41.405 (3)O4—Lai2.622 (2)
C3—C41.392 (5)O5—Laii2.578 (2)
C3—H3A0.930O6—Lai2.488 (2)
C4—C51.369 (5)O1W—H1WA0.845
C4—H4A0.930O1W—H1WB0.845
C5—C61.402 (5)O2W—H2WA0.854
C5—H5A0.930O2W—H2WB0.853
C6—H6A0.930
O6i—La—O3i140.26 (7)C1—C2—O4115.1 (2)
O6i—La—O2W137.78 (7)C2—C3—C4120.2 (3)
O3i—La—O2W69.40 (7)C2—C3—H3A119.9
O6i—La—O5ii128.20 (7)C4—C3—H3A119.9
O3i—La—O5ii82.94 (7)C5—C4—C3119.5 (3)
O2W—La—O5ii71.25 (7)C5—C4—H4A120.2
O6i—La—O1W67.35 (8)C3—C4—H4A120.2
O3i—La—O1W74.44 (7)C4—C5—C6120.8 (3)
O2W—La—O1W137.88 (7)C4—C5—H5A119.6
O5ii—La—O1W125.04 (7)C6—C5—H5A119.6
O6i—La—O4i61.78 (6)C1—C6—C5119.0 (3)
O3i—La—O4i114.68 (6)C1—C6—H6A120.5
O2W—La—O4i146.07 (7)C5—C6—H6A120.5
O5ii—La—O4i75.82 (7)O1—C7—C8108.2 (2)
O1W—La—O4i69.87 (7)O1—C7—H7A110.1
O6i—La—O273.82 (7)C8—C7—H7A110.1
O3i—La—O2101.89 (6)O1—C7—H7B110.1
O2W—La—O269.78 (7)C8—C7—H7B110.1
O5ii—La—O2135.81 (7)H7A—C7—H7B108.4
O1W—La—O298.05 (7)O3—C8—O2121.6 (3)
O4i—La—O2135.36 (7)O3—C8—C7119.2 (3)
O6i—La—O395.20 (7)O2—C8—C7119.3 (3)
O3i—La—O359.34 (8)O4—C9—C10109.8 (2)
O2W—La—O375.55 (6)O4—C9—H9A109.7
O5ii—La—O3136.59 (7)C10—C9—H9A109.7
O1W—La—O367.72 (6)O4—C9—H9B109.7
O4i—La—O3137.04 (7)C10—C9—H9B109.7
O2—La—O347.59 (6)H9A—C9—H9B108.2
O6i—La—O1i110.47 (7)O5—C10—O6125.5 (3)
O3i—La—O1i58.20 (6)O5—C10—C9116.8 (3)
O2W—La—O1i111.61 (7)O6—C10—C9117.6 (3)
O5ii—La—O1i62.18 (7)C1—O1—C7118.8 (2)
O1W—La—O1i63.28 (7)C1—O1—Lai119.49 (17)
O4i—La—O1i57.17 (6)C7—O1—Lai121.56 (16)
O2—La—O1i154.69 (6)C8—O2—La94.79 (17)
O3—La—O1i107.36 (6)C8—O3—Lai129.18 (18)
O6i—La—Cl171.64 (6)C8—O3—La92.21 (17)
O3i—La—Cl1147.73 (5)Lai—O3—La120.66 (8)
O2W—La—Cl181.57 (5)C2—O4—C9116.7 (2)
O5ii—La—Cl174.40 (5)C2—O4—Lai123.79 (18)
O1W—La—Cl1137.64 (6)C9—O4—Lai119.39 (17)
O4i—La—Cl181.97 (5)C10—O5—Laii133.3 (2)
O2—La—Cl180.05 (5)C10—O6—Lai128.08 (19)
O3—La—Cl1127.27 (4)La—O1W—H1WA116.5
O1i—La—Cl1125.23 (5)La—O1W—H1WB118.2
O1—C1—C6124.9 (3)H1WA—O1W—H1WB111.1
O1—C1—C2115.5 (3)La—O2W—H2WA127.0
C6—C1—C2119.7 (3)La—O2W—H2WB100.6
C3—C2—C1120.8 (3)H2WA—O2W—H2WB108.3
C3—C2—O4124.1 (3)
O1—C1—C2—C3177.5 (3)O2—C8—O3—Lai153.8 (2)
C6—C1—C2—C30.9 (5)C7—C8—O3—Lai24.8 (4)
O1—C1—C2—O40.6 (4)O2—C8—O3—La20.2 (3)
C6—C1—C2—O4179.1 (3)C7—C8—O3—La158.4 (3)
C1—C2—C3—C40.2 (5)O6i—La—O3—C873.19 (17)
O4—C2—C3—C4177.8 (3)O3i—La—O3—C8139.3 (2)
C2—C3—C4—C50.6 (5)O2W—La—O3—C864.92 (17)
C3—C4—C5—C60.0 (5)O5ii—La—O3—C8105.86 (18)
O1—C1—C6—C5176.7 (3)O1W—La—O3—C8136.12 (18)
C2—C1—C6—C51.5 (5)O4i—La—O3—C8126.39 (17)
C4—C5—C6—C11.1 (6)O2—La—O3—C810.72 (16)
O1—C7—C8—O312.0 (4)O1i—La—O3—C8173.46 (17)
O1—C7—C8—O2166.7 (3)Cl1—La—O3—C82.36 (19)
O4—C9—C10—O5162.8 (3)O6i—La—O3—Lai147.53 (9)
O4—C9—C10—O618.1 (4)O3i—La—O3—Lai0.0
C6—C1—O1—C718.9 (5)O2W—La—O3—Lai74.36 (9)
C2—C1—O1—C7162.7 (3)O5ii—La—O3—Lai33.42 (14)
C6—C1—O1—Lai155.9 (3)O1W—La—O3—Lai84.60 (10)
C2—C1—O1—Lai22.4 (4)O4i—La—O3—Lai94.33 (11)
C8—C7—O1—C1172.1 (3)O2—La—O3—Lai150.00 (13)
C8—C7—O1—Lai2.7 (3)O1i—La—O3—Lai34.18 (11)
O3—C8—O2—La20.7 (3)Cl1—La—O3—Lai141.63 (6)
C7—C8—O2—La158.0 (3)C3—C2—O4—C924.6 (4)
O6i—La—O2—C8123.88 (18)C1—C2—O4—C9157.4 (3)
O3i—La—O2—C815.34 (18)C3—C2—O4—Lai152.1 (3)
O2W—La—O2—C877.91 (18)C1—C2—O4—Lai26.0 (4)
O5ii—La—O2—C8107.42 (18)C10—C9—O4—C2162.9 (3)
O1W—La—O2—C860.36 (18)C10—C9—O4—Lai20.4 (3)
O4i—La—O2—C8129.79 (17)O6—C10—O5—Laii29.9 (5)
O3—La—O2—C810.74 (16)C9—C10—O5—Laii151.0 (2)
O1i—La—O2—C820.1 (3)O5—C10—O6—Lai173.1 (2)
Cl1—La—O2—C8162.51 (18)C9—C10—O6—Lai7.8 (4)
Symmetry codes: (i) x+2, y+2, z+1; (ii) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2Wi0.841.912.738 (3)166
O1W—H1WB···Cl1iii0.842.433.223 (2)156
O2W—H2WA···O2iv0.851.812.663 (3)176
O2W—H2WB···O6ii0.851.822.668 (3)173
O2W—H2WB···O5ii0.852.522.995 (3)116
Symmetry codes: (i) x+2, y+2, z+1; (ii) x+2, y+1, z+1; (iii) x, y+5/2, z+1/2; (iv) x+2, y1/2, z+1/2.
 

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