Download citation
Download citation
link to html
The title complex is coordinated by two acetyl­acetonate, one 1H-imidazole, one nitrate and one water ligand. The mol­ecular plane of the imidazole ligand is almost parallel to that of the nitrate anion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S205698901701461X/vn2131sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205698901701461X/vn2131Isup2.hkl
Contains datablock I

CCDC reference: 1579078

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.016
  • wR factor = 0.040
  • Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of O43 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of La1 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C22 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C24 Check PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min). 6 Note PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 4 Report PLAT923_ALERT_1_C S values in the CIF and FCF Differ by ....... -0.011 Check
Alert level G PLAT005_ALERT_5_G No Embedded Refinement Details found in the CIF Please Do ! PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 1 Report PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K) 293 Check PLAT200_ALERT_1_G Reported _diffrn_ambient_temperature ..... (K) 293 Check PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O11W .. 5.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O12 .. 6.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O12W .. 5.1 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O22 .. 5.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O24 .. 7.1 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O42 .. 17.3 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 -- O43 .. 7.0 s.u. PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 3 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 5 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 7 ALERT level C = Check. Ensure it is not caused by an omission or oversight 13 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check
checkCIF publication errors
Alert level A PUBL024_ALERT_1_A The number of authors is greater than 5. Please specify the role of each of the co-authors for your paper.
1 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2006); cell refinement: CrystalClear (Rigaku/MSC, 2006); data reduction: CrystalClear (Rigaku/MSC, 2006) and SORTAV (Blessing, 1995); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012).

Diaqua(1H-imidazole-κN3)(nitrato-κ2O,O')bis(4-oxopent-2-en-2-olato-κ2O,O')lanthanum(III) top
Crystal data top
[La(C5H7O2)2(NO3)(C3H4N2)(H2O)2]F(000) = 1000
Mr = 503.24Dx = 1.686 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 19036 reflections
a = 9.8233 (9) Åθ = 3–27.5°
b = 12.4719 (12) ŵ = 2.20 mm1
c = 16.4432 (16) ÅT = 293 K
β = 100.184 (7)°Prism, colorless
V = 1982.8 (3) Å30.42 × 0.39 × 0.12 mm
Z = 4
Data collection top
XTALAB-MINI
diffractometer
4543 independent reflections
Radiation source: sealed x-ray tube4317 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 10 pixels mm-1θmax = 27.5°, θmin = 3.0°
phi or ω oscillation scansh = 1212
Absorption correction: multi-scan
(REQAB; Rigaku, 1998)
k = 1616
Tmin = 0.456, Tmax = 0.772l = 2121
19723 measured reflections
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)] = 0.016Hydrogen site location: mixed
wR(F2) = 0.040H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0179P)2 + 0.8453P]
where P = (Fo2 + 2Fc2)/3
4543 reflections(Δ/σ)max < 0.001
251 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.54 e Å3
0 constraints
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
La10.49302 (2)0.06987 (2)0.73872 (2)0.02341 (4)
C110.3206 (3)0.1406 (2)0.94575 (16)0.0675 (7)
H11A0.26570.18850.90760.101*
H11B0.2720.12380.98990.101*
H11C0.40710.17420.96790.101*
C120.3473 (2)0.03887 (17)0.90146 (12)0.0416 (4)
O120.40186 (14)0.05003 (10)0.83749 (8)0.0404 (3)
C130.3101 (2)0.05849 (17)0.93181 (13)0.0489 (5)
H130.26680.05660.97770.059*
C140.33217 (18)0.15900 (16)0.89926 (11)0.0395 (4)
O140.38770 (15)0.17374 (10)0.83705 (8)0.0454 (3)
C150.2866 (2)0.2580 (2)0.93995 (16)0.0622 (6)
H15A0.24680.30830.89830.093*
H15B0.36510.290.97450.093*
H15C0.21910.23860.9730.093*
C210.8806 (3)0.2748 (2)0.8716 (2)0.0910 (11)
H21A0.82630.31930.90110.136*
H21B0.89830.31220.82350.136*
H21C0.96680.25780.90670.136*
C220.80297 (19)0.17260 (16)0.84555 (12)0.0424 (4)
O220.67656 (13)0.18282 (10)0.81634 (9)0.0448 (3)
C230.8740 (2)0.07563 (17)0.85616 (14)0.0456 (5)
H230.96790.07840.8780.055*
C240.81648 (19)0.02525 (16)0.83686 (12)0.0425 (4)
O240.69227 (13)0.04257 (11)0.80450 (9)0.0446 (3)
C250.9079 (3)0.1227 (2)0.8548 (2)0.0856 (10)
H25A0.86620.17260.88750.128*
H25B0.99680.10140.88470.128*
H25C0.9190.15610.80380.128*
N310.22279 (15)0.07647 (12)0.67424 (10)0.0367 (3)
C320.1625 (2)0.07834 (15)0.59247 (12)0.0411 (4)
H320.21010.07680.54840.049*
C330.0238 (2)0.08279 (17)0.58553 (14)0.0481 (5)
H330.04090.08530.53690.058*
N340.00239 (16)0.08292 (14)0.66351 (12)0.0496 (4)
H340.08260.08520.67760.06*
C350.1190 (2)0.07876 (18)0.71465 (13)0.0483 (5)
H350.12890.07760.77190.058*
N410.62511 (15)0.09036 (12)0.57886 (9)0.0329 (3)
O420.49735 (12)0.08624 (10)0.57207 (8)0.0374 (3)
O430.69523 (14)0.08635 (14)0.65120 (8)0.0545 (4)
O440.68294 (15)0.09930 (13)0.51860 (8)0.0491 (3)
O11W0.45059 (16)0.26240 (10)0.68241 (9)0.0411 (3)
H11X0.389 (3)0.303 (2)0.6897 (16)0.062*
H11Y0.499 (3)0.311 (2)0.6723 (16)0.062*
O12W0.45109 (17)0.10477 (11)0.65529 (9)0.0453 (3)
H12Y0.425 (3)0.100 (2)0.6035 (17)0.068*
H12X0.438 (3)0.160 (2)0.6658 (17)0.068*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.02352 (5)0.02229 (5)0.02468 (6)0.00018 (3)0.00500 (3)0.00149 (3)
C110.0832 (18)0.0650 (15)0.0637 (15)0.0058 (13)0.0387 (14)0.0254 (12)
C120.0416 (10)0.0513 (11)0.0344 (9)0.0007 (8)0.0134 (8)0.0079 (8)
O120.0528 (8)0.0354 (7)0.0377 (7)0.0031 (6)0.0208 (6)0.0043 (5)
C130.0549 (12)0.0635 (14)0.0332 (10)0.0012 (10)0.0214 (9)0.0042 (9)
C140.0319 (9)0.0516 (11)0.0362 (9)0.0029 (8)0.0087 (7)0.0183 (8)
O140.0577 (9)0.0372 (7)0.0476 (7)0.0012 (6)0.0263 (7)0.0107 (6)
C150.0545 (13)0.0666 (15)0.0713 (15)0.0042 (11)0.0267 (12)0.0364 (12)
C210.0437 (13)0.0679 (18)0.153 (3)0.0129 (12)0.0071 (16)0.0437 (19)
C220.0306 (9)0.0505 (11)0.0451 (10)0.0057 (8)0.0042 (8)0.0153 (8)
O220.0336 (7)0.0409 (7)0.0553 (8)0.0023 (5)0.0043 (6)0.0132 (6)
C230.0250 (8)0.0615 (13)0.0485 (12)0.0006 (8)0.0016 (8)0.0030 (9)
C240.0326 (9)0.0486 (11)0.0463 (11)0.0071 (8)0.0069 (8)0.0125 (9)
O240.0350 (7)0.0363 (7)0.0592 (9)0.0022 (5)0.0008 (6)0.0087 (6)
C250.0454 (13)0.0614 (16)0.143 (3)0.0176 (12)0.0008 (16)0.0247 (17)
N310.0256 (7)0.0463 (9)0.0378 (8)0.0009 (6)0.0046 (6)0.0008 (6)
C320.0393 (10)0.0477 (11)0.0365 (10)0.0002 (8)0.0074 (8)0.0017 (8)
C330.0360 (10)0.0576 (13)0.0457 (12)0.0011 (9)0.0067 (9)0.0005 (9)
N340.0239 (7)0.0671 (12)0.0586 (11)0.0023 (7)0.0093 (7)0.0053 (8)
C350.0340 (10)0.0740 (15)0.0381 (10)0.0028 (9)0.0096 (8)0.0022 (9)
N410.0332 (7)0.0373 (8)0.0294 (7)0.0018 (6)0.0085 (6)0.0029 (6)
O420.0294 (6)0.0460 (7)0.0364 (7)0.0021 (5)0.0048 (5)0.0011 (5)
O430.0291 (7)0.1049 (13)0.0294 (7)0.0024 (7)0.0049 (5)0.0017 (7)
O440.0501 (8)0.0691 (9)0.0326 (7)0.0106 (7)0.0198 (6)0.0067 (6)
O11W0.0485 (8)0.0256 (6)0.0502 (8)0.0026 (5)0.0113 (6)0.0023 (5)
O12W0.0726 (10)0.0261 (6)0.0336 (7)0.0018 (6)0.0002 (7)0.0023 (5)
Geometric parameters (Å, º) top
La1—O142.4402 (12)C22—O221.256 (2)
La1—O222.4597 (12)C22—C231.392 (3)
La1—O122.4880 (12)C23—C241.393 (3)
La1—O242.4939 (13)C23—H230.93
La1—O12W2.5682 (13)C24—O241.261 (2)
La1—O11W2.5808 (13)C24—C251.510 (3)
La1—O432.6589 (14)C25—H25A0.96
La1—N312.6800 (15)C25—H25B0.96
La1—O422.7556 (13)C25—H25C0.96
C11—C121.509 (3)N31—C351.312 (2)
C11—H11A0.96N31—C321.370 (3)
C11—H11B0.96C32—C331.348 (3)
C11—H11C0.96C32—H320.93
C12—O121.270 (2)C33—N341.352 (3)
C12—C131.386 (3)C33—H330.93
C13—C141.395 (3)N34—C351.333 (3)
C13—H130.93N34—H340.86
C14—O141.255 (2)C35—H350.93
C14—C151.509 (3)N41—O441.2311 (19)
C15—H15A0.96N41—O421.2413 (18)
C15—H15B0.96N41—O431.266 (2)
C15—H15C0.96O11W—H11X0.81 (3)
C21—C221.508 (3)O11W—H11Y0.81 (3)
C21—H21A0.96O12W—H12Y0.85 (3)
C21—H21B0.96O12W—H12X0.73 (3)
C21—H21C0.96
O14—La1—O2273.14 (5)C14—C15—H15B109.5
O14—La1—O1269.07 (4)H15A—C15—H15B109.5
O22—La1—O12108.72 (5)C14—C15—H15C109.5
O14—La1—O24113.79 (5)H15A—C15—H15C109.5
O22—La1—O2469.51 (5)H15B—C15—H15C109.5
O12—La1—O2474.00 (5)C22—C21—H21A109.5
O14—La1—O12W139.24 (5)C22—C21—H21B109.5
O22—La1—O12W142.79 (5)H21A—C21—H21B109.5
O12—La1—O12W78.27 (5)C22—C21—H21C109.5
O24—La1—O12W78.12 (5)H21A—C21—H21C109.5
O14—La1—O11W71.54 (5)H21B—C21—H21C109.5
O22—La1—O11W73.17 (5)O22—C22—C23125.16 (17)
O12—La1—O11W137.69 (5)O22—C22—C21116.06 (19)
O24—La1—O11W138.02 (5)C23—C22—C21118.78 (19)
O12W—La1—O11W126.65 (5)C22—O22—La1136.44 (12)
O14—La1—O43139.68 (5)C22—C23—C24125.62 (18)
O22—La1—O4371.78 (5)C22—C23—H23117.2
O12—La1—O43142.12 (5)C24—C23—H23117.2
O24—La1—O4370.97 (5)O24—C24—C23125.06 (18)
O12W—La1—O4380.85 (5)O24—C24—C25116.3 (2)
O11W—La1—O4379.79 (5)C23—C24—C25118.66 (19)
O14—La1—N3174.90 (5)C24—O24—La1135.53 (12)
O22—La1—N31140.50 (4)C24—C25—H25A109.5
O12—La1—N3180.27 (5)C24—C25—H25B109.5
O24—La1—N31146.66 (4)H25A—C25—H25B109.5
O12W—La1—N3176.15 (5)C24—C25—H25C109.5
O11W—La1—N3175.15 (5)H25A—C25—H25C109.5
O43—La1—N31124.47 (5)H25B—C25—H25C109.5
O14—La1—O42134.63 (4)C35—N31—C32104.87 (16)
O22—La1—O42109.56 (4)C35—N31—La1127.18 (13)
O12—La1—O42139.84 (4)C32—N31—La1127.95 (12)
O24—La1—O42108.91 (4)C33—C32—N31109.82 (18)
O12W—La1—O4263.95 (4)C33—C32—H32125.1
O11W—La1—O4266.69 (4)N31—C32—H32125.1
O43—La1—O4246.51 (4)C32—C33—N34106.18 (18)
N31—La1—O4278.03 (4)C32—C33—H33126.9
C12—C11—H11A109.5N34—C33—H33126.9
C12—C11—H11B109.5C35—N34—C33107.42 (17)
H11A—C11—H11B109.5C35—N34—H34126.3
C12—C11—H11C109.5C33—N34—H34126.3
H11A—C11—H11C109.5N31—C35—N34111.71 (19)
H11B—C11—H11C109.5N31—C35—H35124.1
O12—C12—C13124.82 (18)N34—C35—H35124.1
O12—C12—C11116.26 (19)O44—N41—O42122.31 (15)
C13—C12—C11118.91 (18)O44—N41—O43120.53 (15)
C12—O12—La1136.74 (12)O42—N41—O43117.15 (14)
C12—C13—C14125.47 (18)N41—O42—La196.13 (10)
C12—C13—H13117.3N41—O43—La1100.21 (10)
C14—C13—H13117.3La1—O11W—H11X127.1 (18)
O14—C14—C13124.32 (17)La1—O11W—H11Y135.3 (18)
O14—C14—C15116.57 (19)H11X—O11W—H11Y92 (2)
C13—C14—C15119.11 (18)La1—O12W—H12Y117.7 (18)
C14—O14—La1139.35 (12)La1—O12W—H12X134 (2)
C14—C15—H15A109.5H12Y—O12W—H12X106 (3)
C13—C12—O12—La16.4 (3)C23—C24—O24—La110.7 (3)
C11—C12—O12—La1174.35 (15)C25—C24—O24—La1168.80 (18)
O12—C12—C13—C143.0 (4)C35—N31—C32—C330.6 (2)
C11—C12—C13—C14177.8 (2)La1—N31—C32—C33179.32 (13)
C12—C13—C14—O140.9 (4)N31—C32—C33—N340.4 (2)
C12—C13—C14—C15179.5 (2)C32—C33—N34—C350.1 (2)
C13—C14—O14—La12.3 (3)C32—N31—C35—N340.6 (2)
C15—C14—O14—La1178.08 (15)La1—N31—C35—N34179.36 (12)
C23—C22—O22—La114.8 (3)C33—N34—C35—N310.3 (3)
C21—C22—O22—La1166.00 (19)O44—N41—O42—La1179.37 (15)
O22—C22—C23—C240.6 (4)O43—N41—O42—La10.25 (16)
C21—C22—C23—C24178.6 (2)O44—N41—O43—La1179.40 (14)
C22—C23—C24—O242.3 (4)O42—N41—O43—La10.26 (17)
C22—C23—C24—C25178.2 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N34—H34···O43i0.862.152.942 (2)153
O11W—H11X···O24ii0.81 (3)2.10 (3)2.8353 (19)152 (2)
O11W—H11Y···O12ii0.81 (3)2.00 (3)2.8014 (19)168 (3)
O12W—H12Y···O44iii0.85 (3)2.10 (3)2.930 (2)167 (3)
O12W—H12X···O22iv0.73 (3)2.30 (3)3.0025 (19)161 (3)
Symmetry codes: (i) x1, y, z; (ii) x+1, y+1/2, z+3/2; (iii) x+1, y, z+1; (iv) x+1, y1/2, z+3/2.
 

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