Diaqua­tris(nitrato-κ²O,O′)bis­(4-pyridone-κO)lanthanum(III)

In the mononuclear title compound, [La(NO₃)₃(C₅H₅NO)₂(H₂O)₂], the La^III atom is ten-coordinate, with a coordination polyhedron made up of the O atoms of two 4-pyridone ligands, six O atoms of three O,O′-chelating nitrate groups and two water mol­ecules, the polyhedron approximating a dodeca­hedron. The mol­ecule lies on a twofold rotation axis. A three-dimensional network structure is formed by hydrogen-bonding and π–π stacking inter­actions.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.016
• wR factor = 0.040
• Data-to-parameter ratio = 15.5

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  La1    -   O2      ..      11.44 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  La1    -   O4      ..      13.06 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  La1    -   O5      ..      14.10 su

Alert level C
PLAT213_ALERT_2_C Atom O3      has ADP max/min Ratio .............       3.10 prolat
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        La1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N2
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

   0 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Diaquatris(nitrato-κ²O,O')bis(4-pyridone-κO)lanthanum(III)

Crystal data

[La(NO3)3(C5H5NO)2(H2O)2]	F(000) = 1080
Mr = 551.17	Dx = 1.949 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 8926 reflections
a = 11.051 (2) Å	θ = 3.1–27.5°
b = 8.9055 (18) Å	µ = 2.35 mm^−1
c = 19.203 (4) Å	T = 295 K
β = 96.31 (3)°	Prism, colorless
V = 1878.4 (7) Å^3	0.36 × 0.25 × 0.19 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer	2150 independent reflections
Radiation source: fine-focus sealed tube	2106 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.015
Detector resolution: 10 pixels mm^-1	θmax = 27.5°, θmin = 3.1°
ω scan	h = −14→14
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −11→11
Tmin = 0.494, Tmax = 0.645	l = −24→24
8972 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.016	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.040	H atoms treated by a mixture of independent and constrained refinement
S = 1.24	w = 1/[σ^2(Fo^2) + (0.0228P)^2 + 0.6564P] where P = (Fo^2 + 2Fc^2)/3
2150 reflections	(Δ/σ)max = 0.001
139 parameters	Δρmax = 0.34 e Å^−3
3 restraints	Δρmin = −0.67 e Å^−3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
La1	0.5000	0.298597 (13)	0.7500	0.02360 (5)
O1W	0.26861 (13)	0.31347 (16)	0.73382 (12)	0.0540 (5)
O1	0.48238 (15)	0.3808 (2)	0.63123 (7)	0.0539 (4)
O2	0.59694 (11)	0.57592 (14)	0.74747 (8)	0.0424 (3)
O3	0.5000	0.7841 (2)	0.7500	0.0931 (14)
O4	0.40621 (13)	0.07622 (16)	0.66863 (8)	0.0460 (3)
O5	0.60148 (13)	0.07647 (18)	0.68054 (8)	0.0505 (4)
O6	0.5027 (2)	−0.0645 (3)	0.60190 (12)	0.0901 (8)
N1	0.27223 (18)	0.4560 (2)	0.44933 (10)	0.0533 (5)
N2	0.5000	0.6495 (2)	0.7500	0.0383 (5)
N3	0.50433 (18)	0.0269 (2)	0.64929 (10)	0.0499 (4)
C1	0.2532 (2)	0.5356 (3)	0.50592 (14)	0.0573 (6)
C2	0.3222 (2)	0.5141 (3)	0.56839 (12)	0.0493 (5)
C3	0.41439 (17)	0.4043 (2)	0.57403 (9)	0.0381 (4)
C4	0.4282 (2)	0.3218 (2)	0.51276 (12)	0.0447 (4)
C5	0.3573 (2)	0.3496 (3)	0.45223 (11)	0.0504 (5)
H1W1	0.227 (2)	0.3943 (18)	0.7288 (17)	0.081*
H1W2	0.222 (2)	0.241 (2)	0.7420 (18)	0.081*
H1	0.1916	0.6072	0.5027	0.069*
H2	0.3084	0.5717	0.6071	0.059*
H4	0.4871	0.2470	0.5140	0.054*
H5	0.3680	0.2941	0.4123	0.061*
H6	0.2288	0.4737	0.4102	0.064*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
La1	0.01880 (7)	0.02110 (7)	0.03051 (8)	0.000	0.00102 (5)	0.000
O1W	0.0204 (6)	0.0337 (7)	0.1075 (15)	−0.0007 (5)	0.0053 (8)	0.0087 (8)
O1	0.0548 (9)	0.0666 (11)	0.0393 (7)	−0.0012 (8)	0.0008 (6)	0.0183 (7)
O2	0.0223 (6)	0.0285 (6)	0.0764 (9)	0.0018 (5)	0.0055 (6)	0.0005 (6)
O3	0.0457 (15)	0.0226 (11)	0.214 (5)	0.000	0.029 (2)	0.000
O4	0.0392 (7)	0.0413 (7)	0.0555 (8)	0.0045 (6)	−0.0039 (6)	−0.0149 (6)
O5	0.0394 (7)	0.0522 (9)	0.0582 (8)	0.0095 (7)	−0.0027 (6)	−0.0170 (7)
O6	0.0826 (14)	0.0916 (15)	0.0912 (14)	0.0239 (12)	−0.0119 (11)	−0.0644 (13)
N1	0.0491 (10)	0.0605 (12)	0.0468 (9)	−0.0097 (9)	−0.0099 (8)	0.0074 (8)
N2	0.0250 (10)	0.0240 (10)	0.0656 (14)	0.000	0.0033 (9)	0.000
N3	0.0515 (10)	0.0451 (10)	0.0504 (9)	0.0122 (8)	−0.0059 (8)	−0.0181 (8)
C1	0.0448 (12)	0.0531 (13)	0.0721 (16)	0.0089 (10)	−0.0019 (11)	0.0054 (12)
C2	0.0483 (11)	0.0507 (12)	0.0491 (11)	0.0053 (10)	0.0064 (9)	−0.0044 (9)
C3	0.0382 (9)	0.0395 (9)	0.0371 (8)	−0.0056 (8)	0.0058 (7)	0.0094 (8)
C4	0.0461 (11)	0.0401 (10)	0.0491 (11)	0.0010 (8)	0.0105 (9)	0.0028 (8)
C5	0.0553 (13)	0.0533 (12)	0.0427 (10)	−0.0099 (10)	0.0056 (9)	−0.0046 (9)

Geometric parameters (Å, º)

La1—O1W	2.5452 (15)	O2—N2	1.2612 (17)
La1—O1	2.3830 (14)	O3—N2	1.199 (3)
La1—O2	2.6946 (14)	O4—N3	1.263 (2)
La1—O4	2.6612 (14)	O5—N3	1.251 (2)
La1—O5	2.6978 (15)	O6—N3	1.219 (2)
O1—C3	1.278 (2)	N1—C5	1.331 (3)
C1—C2	1.362 (3)	N1—C1	1.333 (3)
C4—C5	1.351 (3)	N1—H6	0.8600
La1—O1W^i	2.5452 (15)	N2—O2^i	1.2612 (17)
La1—O1^i	2.3830 (14)	C1—H1	0.9300
La1—O2^i	2.6946 (14)	C2—C3	1.408 (3)
La1—O4^i	2.6612 (14)	C2—H2	0.9300
La1—O5^i	2.6978 (15)	C3—C4	1.409 (3)
O1W—H1W1	0.854 (10)	C4—H4	0.9300
O1W—H1W2	0.847 (10)	C5—H5	0.9300
O1W^i—La1—O1W	174.03 (7)	O1^i—La1—O4^i	71.41 (6)
O1W—La1—O2	110.25 (4)	O1^i—La1—O5	134.74 (6)
O1W—La1—O2^i	63.80 (4)	O1^i—La1—O5^i	75.34 (6)
O1W—La1—O4^i	115.57 (5)	O1—C3—C2	122.13 (19)
O1W—La1—O4	69.26 (5)	O1—C3—C4	121.7 (2)
O1W—La1—O5	116.39 (5)	O2^i—La1—O5^i	118.39 (5)
O1W—La1—O5^i	68.40 (5)	O2^i—La1—O5	150.30 (5)
O1^i—La1—O1	144.20 (9)	O2^i—N2—O2	117.4 (2)
O1—La1—O1W	83.79 (7)	O3—N2—O2	121.30 (10)
O1—La1—O1W^i	94.37 (7)	O3—N2—O2^i	121.30 (10)
O1—La1—O2	72.05 (6)	O4^i—La1—O2	124.24 (5)
O1—La1—O2^i	75.21 (6)	O4^i—La1—O2^i	143.27 (5)
O1—La1—O4^i	140.92 (6)	O4^i—La1—O5^i	47.18 (5)
O1—La1—O4	71.41 (6)	O4^i—La1—O5	65.69 (5)
O1—La1—O5^i	134.74 (6)	O5—N3—O4	117.09 (16)
O1—La1—O5	75.34 (6)	O6—N3—O4	120.58 (19)
O2—La1—O2^i	47.15 (5)	O6—N3—O5	122.33 (19)
O2—La1—O5	118.39 (5)	N1—C1—C2	121.3 (2)
O2—La1—O5^i	150.30 (5)	N1—C1—H1	119.3
O4—La1—O2^i	124.24 (5)	N1—C5—C4	120.4 (2)
O4—La1—O2	143.27 (5)	N1—C5—H5	119.8
O4—La1—O4^i	83.82 (7)	N2—O2—La1	97.73 (11)
O4—La1—O5	47.18 (5)	N3—O4—La1	98.04 (11)
O4—La1—O5^i	65.69 (5)	N3—O5—La1	96.57 (11)
O5—La1—O5^i	85.69 (8)	C1—C2—C3	119.7 (2)
La1—O1W—H1W1	125.4 (18)	C1—C2—H2	120.1
La1—O1W—H1W2	124.0 (19)	C1—N1—H6	119.4
O1W^i—La1—O2^i	110.25 (4)	C2—C1—H1	119.3
O1W^i—La1—O2	63.80 (4)	C2—C3—C4	116.20 (18)
O1W^i—La1—O4	115.57 (5)	C3—C2—H2	120.1
O1W^i—La1—O4^i	69.26 (5)	C3—C4—H4	119.4
O1W^i—La1—O5^i	116.39 (5)	C3—O1—La1	148.35 (14)
O1W^i—La1—O5	68.40 (5)	C4—C5—H5	119.8
O1^i—La1—O1W^i	83.79 (7)	C5—C4—C3	121.1 (2)
O1^i—La1—O1W	94.37 (7)	C5—C4—H4	119.4
O1^i—La1—O2^i	72.05 (6)	C5—N1—C1	121.2 (2)
O1^i—La1—O2	75.21 (6)	C5—N1—H6	119.4
O1^i—La1—O4	140.92 (6)	H1W1—O1W—H1W2	109.3 (16)
O1^i—La1—O1—C3	−101.4 (3)	O5^i—La1—O4—N3	−113.85 (13)
O1W^i—La1—O1—C3	173.2 (3)	O1^i—La1—O5—N3	130.94 (13)
O1W—La1—O1—C3	−12.5 (3)	O1—La1—O5—N3	−71.99 (14)
O4—La1—O1—C3	57.7 (3)	O1W^i—La1—O5—N3	−172.84 (15)
O4^i—La1—O1—C3	111.2 (3)	O1W—La1—O5—N3	3.26 (15)
O2—La1—O1—C3	−126.2 (3)	O4—La1—O5—N3	6.07 (12)
O2^i—La1—O1—C3	−77.0 (3)	O4^i—La1—O5—N3	110.99 (14)
O5—La1—O1—C3	106.9 (3)	O2—La1—O5—N3	−131.76 (13)
O5^i—La1—O1—C3	38.5 (3)	O2^i—La1—O5—N3	−79.56 (16)
O1^i—La1—O2—N2	−79.06 (9)	O5^i—La1—O5—N3	66.54 (13)
O1—La1—O2—N2	86.24 (9)	La1—O2—N2—O3	180.0
O1W^i—La1—O2—N2	−169.37 (11)	La1—O2—N2—O2^i	0.0
O1W—La1—O2—N2	10.16 (10)	La1—O5—N3—O6	169.1 (2)
O4—La1—O2—N2	92.31 (10)	La1—O5—N3—O4	−10.6 (2)
O4^i—La1—O2—N2	−133.71 (8)	La1—O4—N3—O6	−168.9 (2)
O2^i—La1—O2—N2	0.0	La1—O4—N3—O5	10.8 (2)
O5—La1—O2—N2	147.72 (7)	C5—N1—C1—C2	1.9 (4)
O5^i—La1—O2—N2	−71.49 (12)	N1—C1—C2—C3	−1.0 (4)
O1^i—La1—O4—N3	−118.44 (13)	La1—O1—C3—C2	65.6 (4)
O1—La1—O4—N3	80.96 (13)	La1—O1—C3—C4	−114.7 (3)
O1W^i—La1—O4—N3	−4.92 (14)	C1—C2—C3—O1	179.3 (2)
O1W—La1—O4—N3	171.27 (14)	C1—C2—C3—C4	−0.4 (3)
O4^i—La1—O4—N3	−68.38 (12)	O1—C3—C4—C5	−178.7 (2)
O2—La1—O4—N3	74.87 (14)	C2—C3—C4—C5	0.9 (3)
O2^i—La1—O4—N3	137.26 (12)	C1—N1—C5—C4	−1.3 (3)
O5—La1—O4—N3	−6.04 (12)	C3—C4—C5—N1	−0.1 (3)

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W1···O5^ii	0.85 (1)	2.27 (1)	3.087 (2)	161 (3)
O1W—H1W2···O2^iii	0.85 (1)	2.03 (1)	2.873 (2)	171 (3)
O1W—H1W2···O3^iii	0.85 (1)	2.51 (3)	3.0296 (16)	121 (2)
N1—H6···O4^iv	0.86	2.05	2.849 (2)	153

Symmetry codes: (ii) x−1/2, y+1/2, z; (iii) x−1/2, y−1/2, z; (iv) −x+1/2, −y+1/2, −z+1.