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The title compound, [La(C6H4NO2)3(C12H8N2)2(H2O)2]·3H2O, consists of a mononuclear complex and three non-coordinated water mol­ecules. The La atom is coordinated by five O atoms of three nicotinate groups and two coordinated water mol­ecules, and four N atoms of two bidentate phenanthroline mol­ecules, in a tricapped trigonal–prismatic coordination geometry. The complex mol­ecule and water mol­ecules are linked into layers through O—H...O and O—H...N hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502725X/hb6254sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680502725X/hb6254Isup2.hkl
Contains datablock I

CCDC reference: 287561

Key indicators

  • Single-crystal X-ray study
  • T = 290 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.020
  • wR factor = 0.054
  • Data-to-parameter ratio = 22.5

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

The title compound, (I), is isostructural with its [M(C6H4NO2)3(C12H8N2)2(H2O)2]·3H2O [M = Pr (Yue et al., 2004), Nd (Liu & Wang, 2004) and Ce (Liu et al., 2004)] analogues. It consists of a mononuclear [La(C6H4NO2)3(C12H8N2)2(H2O)2] neutral molecule and three uncoordinated water molecules (Fig. 1). The La atom possesses trigonal prismatic coordination geometry (Table 1), in which the La—O bond distances range from 2.4199 (10) to 2.5416 (10) Å and the La—N bond distances range from 2.7565 (12) to 2.7757 (11) Å, which is similar to the previously reported isostructural complexes. In (I), the uncoordinated water molecules participate in the extensive hydrogen-bonding interactions formed between the water molecules and the N and O atoms of the nicotinate groups (Table 2), resulting in a layered structure.

Experimental top

1,10-Phenanthroline monohydrate (0.0198 g, 0.10 mmol) and nicotinic acid (0.0123 g, 0.10 mmol) were completely dissolved in CH3OH/H2O (30 ml, 1:1 v/v); La(CH3COO)3·3H2O (0.0158 g) was added andthe mixture was stirred for 40 min. The resulting white slurry was filtered and the filtrate was left to stand at room temperature. Crystals of (I) suitable for X-ray analysis were obtained after two weeks (yield ca 35%).

Refinement top

H atoms attached to C atoms were included at calculated positions and treated as riding atoms [C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C)]. The water H atoms were found in a diffrence map, relocated in idealized posiitons (O—H = 0.85 Å) and refined as riding with Uiso(H) = 1.2Ueq(O).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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. The asymmetric unit of (I), showing 35% probability displacement ellipsoids (arbitrary spheres for H atoms).
Diaquatris(nicotinato-kO)bis(1,10-phenanthroline-k2N,N')lanthanum(III) trihydrate top
Crystal data top
[La(C6H4NO2)3(C12H8N2)2(H2O)2]·3H2OZ = 2
Mr = 955.70F(000) = 968
Triclinic, P1Dx = 1.537 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.0676 (1) ÅCell parameters from 985 reflections
b = 12.9618 (2) Åθ = 3.3–26.7°
c = 17.9351 (3) ŵ = 1.10 mm1
α = 84.998 (1)°T = 290 K
β = 80.800 (1)°Block, colorless
γ = 84.190 (1)°0.20 × 0.20 × 0.18 mm
V = 2064.73 (5) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
12414 independent reflections
Radiation source: fine-focus sealed tube11284 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
ϕ and ω scansθmax = 30.7°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1212
Tmin = 0.791, Tmax = 0.811k = 1817
45880 measured reflectionsl = 2523
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difmap (O-H) and geom (others)
R[F2 > 2σ(F2)] = 0.020H-atom parameters constrained
wR(F2) = 0.054 w = 1/[σ2(Fo2) + (0.0318P)2 + 0.2509P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.005
12414 reflectionsΔρmax = 0.50 e Å3
552 parametersΔρmin = 0.26 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0010 (2)
Crystal data top
[La(C6H4NO2)3(C12H8N2)2(H2O)2]·3H2Oγ = 84.190 (1)°
Mr = 955.70V = 2064.73 (5) Å3
Triclinic, P1Z = 2
a = 9.0676 (1) ÅMo Kα radiation
b = 12.9618 (2) ŵ = 1.10 mm1
c = 17.9351 (3) ÅT = 290 K
α = 84.998 (1)°0.20 × 0.20 × 0.18 mm
β = 80.800 (1)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
12414 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
11284 reflections with I > 2σ(I)
Tmin = 0.791, Tmax = 0.811Rint = 0.020
45880 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0200 restraints
wR(F2) = 0.054H-atom parameters constrained
S = 1.04Δρmax = 0.50 e Å3
12414 reflectionsΔρmin = 0.26 e Å3
552 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
La0.583247 (7)0.741098 (5)0.735662 (4)0.02918 (3)
N10.68513 (13)0.90575 (8)0.63803 (7)0.0370 (2)
N20.50559 (14)0.77384 (10)0.59248 (7)0.0416 (3)
C10.76622 (17)0.97387 (11)0.65973 (9)0.0433 (3)
H1A0.77330.97280.71100.052*
C20.84199 (19)1.04749 (12)0.61017 (10)0.0504 (4)
H2A0.89701.09390.62840.060*
C30.83383 (19)1.04989 (12)0.53496 (10)0.0494 (4)
H3A0.88391.09780.50100.059*
C40.74891 (17)0.97928 (11)0.50904 (8)0.0422 (3)
C50.7338 (2)0.97814 (14)0.43089 (9)0.0523 (4)
H5A0.78421.02390.39520.063*
C60.6482 (2)0.91222 (14)0.40835 (9)0.0537 (4)
H6A0.64120.91240.35720.064*
C70.56706 (18)0.84125 (12)0.46156 (8)0.0449 (3)
C80.4698 (2)0.77548 (15)0.44079 (10)0.0578 (4)
H8C0.45930.77390.39020.069*
C90.3904 (2)0.71375 (16)0.49480 (11)0.0632 (5)
H9C0.32240.67190.48180.076*
C100.4126 (2)0.71430 (14)0.56997 (10)0.0536 (4)
H10C0.35960.67070.60620.064*
C110.58103 (15)0.83852 (11)0.53909 (8)0.0372 (3)
C120.67429 (15)0.90862 (10)0.56325 (8)0.0354 (3)
N30.49510 (14)0.70097 (10)0.88894 (7)0.0421 (3)
N40.74812 (13)0.59505 (9)0.81828 (7)0.0393 (2)
C130.37536 (19)0.75361 (14)0.92443 (10)0.0543 (4)
H13A0.31230.79500.89570.065*
C140.3396 (2)0.74943 (17)1.00397 (12)0.0676 (5)
H14A0.25610.78911.02690.081*
C150.4271 (3)0.68774 (18)1.04654 (11)0.0682 (5)
H15A0.40390.68441.09910.082*
C160.5522 (2)0.62890 (15)1.01191 (9)0.0546 (4)
C170.6469 (3)0.55723 (18)1.05357 (10)0.0678 (6)
H17A0.62600.55101.10620.081*
C180.7631 (3)0.49989 (16)1.01882 (11)0.0642 (5)
H18A0.82010.45291.04730.077*
C190.80165 (19)0.50957 (13)0.93811 (10)0.0501 (4)
C200.9241 (2)0.45098 (15)0.89952 (13)0.0644 (5)
H20A0.98210.40210.92610.077*
C210.9572 (2)0.46590 (16)0.82352 (12)0.0669 (5)
H21A1.03860.42800.79720.080*
C220.86718 (19)0.53947 (14)0.78475 (10)0.0540 (4)
H22A0.89250.54980.73250.065*
C240.58411 (17)0.63903 (11)0.93208 (8)0.0404 (3)
O10.59043 (16)0.96134 (10)0.86802 (8)0.0646 (3)
O20.73590 (11)0.83138 (8)0.81291 (6)0.0416 (2)
N70.9590 (2)0.77728 (19)1.00024 (12)0.0895 (6)
C230.71386 (16)0.58049 (11)0.89471 (8)0.0391 (3)
C250.69444 (17)0.89200 (11)0.86703 (8)0.0409 (3)
C260.77693 (18)0.87694 (12)0.93379 (8)0.0440 (3)
C270.7390 (2)0.94261 (17)0.99230 (11)0.0635 (5)
H27A0.66390.99680.99040.076*
C280.8161 (3)0.9252 (2)1.05367 (12)0.0743 (7)
H28A0.79570.96921.09300.089*
C290.9213 (3)0.8436 (3)1.05567 (14)0.0748 (9)
H29A0.97050.83241.09770.090*
C300.8868 (2)0.79661 (16)0.94004 (11)0.0615 (5)
H30A0.91250.75340.90040.074*
O31.02074 (13)0.75971 (11)0.59165 (7)0.0583 (3)
O40.81618 (11)0.69314 (8)0.65496 (6)0.0418 (2)
C340.7637 (3)0.54783 (18)0.46312 (13)0.0783 (6)
H34A0.69720.49750.46380.094*
C310.91118 (15)0.70821 (11)0.59570 (8)0.0385 (3)
C320.88553 (16)0.66012 (11)0.52625 (8)0.0406 (3)
C330.9566 (2)0.69361 (16)0.45572 (10)0.0592 (4)
H33A1.02380.74390.45320.071*
N50.9350 (2)0.65827 (16)0.39077 (9)0.0778 (5)
C350.8422 (3)0.58503 (19)0.39578 (12)0.0769 (6)
H35A0.82910.55710.35150.092*
C360.7848 (2)0.58590 (14)0.52952 (11)0.0585 (4)
H36A0.73240.56220.57570.070*
O50.30850 (13)0.51845 (10)0.73377 (10)0.0674 (4)
O60.54465 (11)0.55922 (7)0.70809 (6)0.0429 (2)
N60.7016 (2)0.25106 (12)0.74967 (10)0.0669 (4)
C370.44594 (16)0.49545 (11)0.72525 (8)0.0402 (3)
C380.49871 (17)0.38246 (11)0.73889 (8)0.0410 (3)
C390.64924 (19)0.34868 (12)0.73132 (10)0.0502 (4)
H39A0.71830.39650.71240.060*
C400.5987 (3)0.18318 (14)0.77480 (12)0.0736 (6)
H40A0.63260.11480.78780.088*
C410.4488 (3)0.20853 (14)0.78231 (13)0.0729 (6)
H41A0.38230.15840.79940.087*
C420.3964 (2)0.30960 (13)0.76430 (11)0.0572 (4)
H42A0.29390.32880.76910.069*
O70.43149 (12)0.91033 (9)0.76985 (7)0.0503 (3)
O80.30437 (11)0.71789 (8)0.75547 (7)0.0514 (3)
O90.14993 (15)0.00103 (11)0.76982 (9)0.0662 (3)
O100.03720 (12)0.82433 (10)0.73077 (7)0.0555 (3)
O111.01842 (18)0.19971 (12)0.74285 (9)0.0777 (4)
H7B0.34340.93910.76850.050*
H8B0.21950.74930.74980.050*
H9B0.10560.06000.75870.050*
H9A0.10320.04460.75450.050*
H8A0.28650.65620.74990.050*
H7A0.48080.93320.80040.050*
H10B0.04800.81840.75760.050*
H11B1.03740.23800.70220.050*
H11A0.92410.21290.75390.050*
H10A0.03800.80820.68580.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La0.03010 (4)0.02807 (4)0.02927 (4)0.00298 (2)0.00568 (2)0.00103 (2)
N10.0434 (6)0.0318 (5)0.0354 (6)0.0034 (4)0.0068 (4)0.0023 (4)
N20.0459 (6)0.0418 (6)0.0393 (6)0.0085 (5)0.0144 (5)0.0051 (5)
C10.0535 (8)0.0357 (7)0.0415 (7)0.0067 (6)0.0095 (6)0.0001 (6)
C20.0582 (9)0.0384 (7)0.0549 (9)0.0136 (6)0.0054 (7)0.0000 (7)
C30.0557 (9)0.0380 (7)0.0508 (9)0.0096 (6)0.0026 (7)0.0052 (6)
C40.0462 (7)0.0359 (7)0.0404 (7)0.0004 (5)0.0004 (6)0.0053 (5)
C50.0623 (10)0.0521 (9)0.0369 (8)0.0027 (7)0.0009 (7)0.0093 (7)
C60.0645 (10)0.0615 (10)0.0324 (7)0.0009 (8)0.0073 (7)0.0051 (7)
C70.0524 (8)0.0465 (8)0.0353 (7)0.0042 (6)0.0127 (6)0.0008 (6)
C80.0706 (11)0.0640 (11)0.0432 (9)0.0019 (8)0.0249 (8)0.0031 (8)
C90.0736 (12)0.0646 (11)0.0613 (11)0.0185 (9)0.0359 (9)0.0011 (9)
C100.0605 (9)0.0544 (9)0.0510 (9)0.0172 (7)0.0217 (7)0.0062 (7)
C110.0403 (6)0.0361 (6)0.0342 (6)0.0028 (5)0.0090 (5)0.0016 (5)
C120.0385 (6)0.0306 (6)0.0347 (6)0.0020 (5)0.0044 (5)0.0026 (5)
N30.0437 (6)0.0427 (6)0.0373 (6)0.0056 (5)0.0012 (5)0.0002 (5)
N40.0414 (6)0.0392 (6)0.0357 (6)0.0007 (4)0.0074 (5)0.0038 (5)
C130.0512 (9)0.0546 (9)0.0513 (9)0.0022 (7)0.0077 (7)0.0040 (7)
C140.0693 (12)0.0719 (12)0.0552 (11)0.0089 (9)0.0186 (9)0.0176 (9)
C150.0866 (14)0.0781 (13)0.0385 (9)0.0214 (11)0.0060 (9)0.0088 (9)
C160.0724 (11)0.0608 (10)0.0328 (7)0.0234 (8)0.0051 (7)0.0019 (7)
C170.0978 (15)0.0773 (13)0.0344 (8)0.0281 (12)0.0240 (9)0.0109 (8)
C180.0809 (13)0.0677 (12)0.0498 (10)0.0376 (10)0.0315 (9)0.0156 (9)
C190.0571 (9)0.0479 (8)0.0497 (9)0.0139 (7)0.0243 (7)0.0132 (7)
C200.0574 (10)0.0575 (10)0.0784 (13)0.0034 (8)0.0282 (9)0.0179 (9)
C210.0525 (9)0.0650 (11)0.0759 (13)0.0187 (8)0.0107 (9)0.0099 (10)
C220.0510 (8)0.0530 (9)0.0514 (9)0.0115 (7)0.0039 (7)0.0076 (7)
C240.0497 (7)0.0411 (7)0.0320 (6)0.0156 (6)0.0062 (5)0.0018 (5)
O10.0824 (9)0.0480 (7)0.0695 (8)0.0144 (6)0.0361 (7)0.0160 (6)
O20.0454 (5)0.0434 (5)0.0389 (5)0.0078 (4)0.0132 (4)0.0030 (4)
N70.0940 (14)0.1076 (16)0.0698 (12)0.0225 (12)0.0435 (11)0.0022 (11)
C230.0461 (7)0.0374 (6)0.0360 (7)0.0109 (5)0.0127 (5)0.0055 (5)
C250.0525 (8)0.0349 (6)0.0389 (7)0.0112 (5)0.0166 (6)0.0030 (5)
C260.0518 (8)0.0445 (8)0.0379 (7)0.0078 (6)0.0126 (6)0.0002 (6)
C270.0716 (12)0.0707 (12)0.0520 (10)0.0014 (9)0.0196 (9)0.0159 (9)
C280.0733 (17)0.116 (2)0.0490 (11)0.0024 (14)0.0207 (11)0.0267 (12)
C290.0733 (17)0.142 (3)0.0545 (13)0.0086 (17)0.0398 (12)0.0077 (14)
C300.0656 (11)0.0661 (11)0.0558 (10)0.0074 (9)0.0247 (9)0.0071 (9)
O30.0508 (6)0.0791 (9)0.0470 (6)0.0275 (6)0.0008 (5)0.0062 (6)
O40.0410 (5)0.0433 (5)0.0370 (5)0.0032 (4)0.0031 (4)0.0025 (4)
C340.1066 (17)0.0650 (12)0.0710 (14)0.0374 (12)0.0148 (12)0.0117 (10)
C310.0380 (6)0.0386 (7)0.0366 (7)0.0023 (5)0.0018 (5)0.0025 (5)
C320.0430 (7)0.0384 (7)0.0383 (7)0.0032 (5)0.0021 (5)0.0003 (5)
C330.0686 (11)0.0689 (11)0.0410 (8)0.0267 (9)0.0002 (8)0.0002 (8)
N50.1009 (14)0.0941 (14)0.0404 (8)0.0313 (11)0.0031 (8)0.0050 (8)
C350.1045 (17)0.0810 (15)0.0514 (11)0.0241 (13)0.0157 (11)0.0139 (10)
C360.0755 (11)0.0491 (9)0.0513 (9)0.0223 (8)0.0018 (8)0.0001 (7)
O50.0428 (6)0.0450 (6)0.1154 (12)0.0083 (5)0.0113 (7)0.0082 (7)
O60.0428 (5)0.0329 (5)0.0531 (6)0.0080 (4)0.0059 (4)0.0004 (4)
N60.0772 (11)0.0470 (8)0.0698 (11)0.0134 (7)0.0034 (8)0.0028 (7)
C370.0448 (7)0.0341 (6)0.0425 (7)0.0068 (5)0.0070 (6)0.0027 (5)
C380.0525 (8)0.0329 (6)0.0368 (7)0.0084 (5)0.0004 (6)0.0050 (5)
C390.0562 (9)0.0395 (7)0.0523 (9)0.0025 (6)0.0027 (7)0.0011 (6)
C400.1142 (18)0.0333 (8)0.0647 (12)0.0023 (9)0.0038 (12)0.0019 (8)
C410.1016 (17)0.0368 (9)0.0731 (13)0.0197 (9)0.0151 (12)0.0010 (8)
C420.0667 (10)0.0407 (8)0.0610 (11)0.0157 (7)0.0082 (8)0.0066 (7)
O70.0448 (5)0.0431 (6)0.0644 (7)0.0063 (4)0.0147 (5)0.0125 (5)
O80.0345 (5)0.0436 (6)0.0783 (8)0.0020 (4)0.0127 (5)0.0097 (5)
O90.0579 (7)0.0618 (8)0.0851 (10)0.0084 (6)0.0316 (7)0.0183 (7)
O100.0405 (5)0.0649 (7)0.0644 (7)0.0026 (5)0.0147 (5)0.0141 (6)
O110.0789 (9)0.0736 (9)0.0728 (10)0.0107 (7)0.0076 (7)0.0114 (7)
Geometric parameters (Å, º) top
La—O42.4199 (10)C21—C221.403 (2)
La—O62.5200 (10)C21—H21A0.9300
La—O22.5355 (10)C22—H22A0.9300
La—O72.5367 (10)C24—C231.437 (2)
La—O82.5416 (10)O1—C251.2342 (19)
La—N22.7565 (12)O2—C251.2873 (18)
La—N32.7566 (12)N7—C301.343 (2)
La—N42.7678 (11)N7—C291.351 (3)
La—N12.7757 (11)C25—C261.499 (2)
N1—C11.3247 (18)C26—C301.377 (2)
N1—C121.3574 (18)C26—C271.387 (2)
N2—C101.328 (2)C27—C281.386 (3)
N2—C111.3617 (18)C27—H27A0.9300
C1—C21.401 (2)C28—C291.354 (4)
C1—H1A0.9300C28—H28A0.9300
C2—C31.360 (2)C29—H29A0.9300
C2—H2A0.9300C30—H30A0.9300
C3—C41.406 (2)O3—C311.2412 (18)
C3—H3A0.9300O4—C311.2708 (16)
C4—C121.4149 (18)C34—C351.375 (3)
C4—C51.431 (2)C34—C361.376 (3)
C5—C61.338 (3)C34—H34A0.9300
C5—H5A0.9300C31—C321.501 (2)
C6—C71.434 (2)C32—C331.380 (2)
C6—H6A0.9300C32—C361.383 (2)
C7—C81.399 (2)C33—N51.338 (2)
C7—C111.413 (2)C33—H33A0.9300
C8—C91.362 (3)N5—C351.320 (3)
C8—H8C0.9300C35—H35A0.9300
C9—C101.395 (2)C36—H36A0.9300
C9—H9C0.9300O5—C371.2399 (18)
C10—H10C0.9300O6—C371.2634 (16)
C11—C121.439 (2)N6—C391.338 (2)
N3—C131.325 (2)N6—C401.345 (3)
N3—C241.3619 (19)C37—C381.506 (2)
N4—C221.325 (2)C38—C391.380 (2)
N4—C231.3571 (18)C38—C421.388 (2)
C13—C141.409 (3)C39—H39A0.9300
C13—H13A0.9300C40—C411.354 (3)
C14—C151.345 (3)C40—H40A0.9300
C14—H14A0.9300C41—C421.377 (3)
C15—C161.392 (3)C41—H41A0.9300
C15—H15A0.9300C42—H42A0.9300
C16—C241.412 (2)O7—H7B0.8498
C16—C171.443 (3)O7—H7A0.8497
C17—C181.328 (3)O8—H8B0.8497
C17—H17A0.9300O8—H8A0.8495
C18—C191.431 (3)O9—H9B0.8498
C18—H18A0.9300O9—H9A0.8494
C19—C201.401 (3)O10—H10B0.8496
C19—C231.418 (2)O10—H10A0.8498
C20—C211.349 (3)O11—H11B0.8495
C20—H20A0.9300O11—H11A0.8498
O4—La—O678.67 (3)C24—C16—C17119.30 (18)
O4—La—O287.40 (4)C18—C17—C16121.76 (17)
O6—La—O2139.00 (3)C18—C17—H17A119.1
O4—La—O7135.61 (4)C16—C17—H17A119.1
O6—La—O7139.88 (3)C17—C18—C19120.78 (17)
O2—La—O773.61 (3)C17—C18—H18A119.6
O4—La—O8142.05 (4)C19—C18—H18A119.6
O6—La—O870.36 (3)C20—C19—C23118.00 (15)
O2—La—O8130.48 (4)C20—C19—C18122.39 (16)
O7—La—O869.63 (4)C23—C19—C18119.60 (17)
O4—La—N277.16 (4)C21—C20—C19119.55 (15)
O6—La—N278.56 (4)C21—C20—H20A120.2
O2—La—N2135.62 (3)C19—C20—H20A120.2
O7—La—N288.87 (4)C20—C21—C22119.05 (17)
O8—La—N275.68 (4)C20—C21—H21A120.5
O4—La—N3130.98 (4)C22—C21—H21A120.5
O6—La—N392.29 (4)N4—C22—C21123.81 (17)
O2—La—N368.38 (4)N4—C22—H22A118.1
O7—La—N378.83 (4)C21—C22—H22A118.1
O8—La—N372.84 (4)N3—C24—C16122.48 (15)
N2—La—N3148.49 (4)N3—C24—C23118.62 (12)
O4—La—N472.59 (3)C16—C24—C23118.89 (14)
O6—La—N469.06 (4)C25—O2—La130.85 (9)
O2—La—N470.00 (3)C30—N7—C29116.3 (2)
O7—La—N4132.05 (4)N4—C23—C19122.02 (14)
O8—La—N4113.97 (4)N4—C23—C24118.41 (12)
N2—La—N4139.07 (4)C19—C23—C24119.57 (14)
N3—La—N459.39 (4)O1—C25—O2124.44 (13)
O4—La—N167.43 (3)O1—C25—C26117.61 (14)
O6—La—N1129.96 (3)O2—C25—C26117.94 (13)
O2—La—N176.40 (3)C30—C26—C27118.63 (16)
O7—La—N169.21 (4)C30—C26—C25121.48 (15)
O8—La—N1117.91 (4)C27—C26—C25119.84 (15)
N2—La—N159.23 (3)C28—C27—C26118.2 (2)
N3—La—N1137.74 (4)C28—C27—H27A120.9
N4—La—N1128.12 (3)C26—C27—H27A120.9
C1—N1—C12117.60 (12)C29—C28—C27119.3 (2)
C1—N1—La121.35 (9)C29—C28—H28A120.4
C12—N1—La120.17 (8)C27—C28—H28A120.4
C10—N2—C11117.76 (13)N7—C29—C28123.9 (2)
C10—N2—La120.73 (10)N7—C29—H29A118.0
C11—N2—La120.52 (9)C28—C29—H29A118.0
N1—C1—C2123.96 (15)N7—C30—C26123.62 (19)
N1—C1—H1A118.0N7—C30—H30A118.2
C2—C1—H1A118.0C26—C30—H30A118.2
C3—C2—C1118.89 (15)C31—O4—La151.35 (9)
C3—C2—H2A120.6C35—C34—C36119.22 (19)
C1—C2—H2A120.6C35—C34—H34A120.4
C2—C3—C4119.37 (14)C36—C34—H34A120.4
C2—C3—H3A120.3O3—C31—O4124.76 (14)
C4—C3—H3A120.3O3—C31—C32118.85 (13)
C3—C4—C12117.91 (14)O4—C31—C32116.38 (12)
C3—C4—C5122.44 (14)C33—C32—C36117.60 (16)
C12—C4—C5119.65 (15)C33—C32—C31120.28 (14)
C6—C5—C4120.99 (15)C36—C32—C31122.01 (14)
C6—C5—H5A119.5N5—C33—C32124.12 (17)
C4—C5—H5A119.5N5—C33—H33A117.9
C5—C6—C7121.32 (15)C32—C33—H33A117.9
C5—C6—H6A119.3C35—N5—C33116.95 (17)
C7—C6—H6A119.3N5—C35—C34123.37 (19)
C8—C7—C11117.51 (15)N5—C35—H35A118.3
C8—C7—C6122.97 (15)C34—C35—H35A118.3
C11—C7—C6119.50 (15)C34—C36—C32118.67 (17)
C9—C8—C7119.92 (16)C34—C36—H36A120.7
C9—C8—H8C120.0C32—C36—H36A120.7
C7—C8—H8C120.0C37—O6—La138.33 (9)
C8—C9—C10118.98 (16)C39—N6—C40116.62 (18)
C8—C9—H9C120.5O5—C37—O6125.39 (14)
C10—C9—H9C120.5O5—C37—C38116.97 (13)
N2—C10—C9123.46 (16)O6—C37—C38117.62 (13)
N2—C10—H10C118.3C39—C38—C42117.71 (15)
C9—C10—H10C118.3C39—C38—C37121.61 (13)
N2—C11—C7122.31 (14)C42—C38—C37120.56 (15)
N2—C11—C12118.47 (12)N6—C39—C38123.73 (16)
C7—C11—C12119.19 (13)N6—C39—H39A118.1
N1—C12—C4122.26 (13)C38—C39—H39A118.1
N1—C12—C11118.41 (12)N6—C40—C41123.83 (18)
C4—C12—C11119.32 (13)N6—C40—H40A118.1
C13—N3—C24117.69 (14)C41—C40—H40A118.1
C13—N3—La120.28 (11)C40—C41—C42118.98 (19)
C24—N3—La121.30 (9)C40—C41—H41A120.5
C22—N4—C23117.53 (13)C42—C41—H41A120.5
C22—N4—La120.99 (10)C41—C42—C38119.1 (2)
C23—N4—La121.43 (9)C41—C42—H42A120.5
N3—C13—C14122.70 (18)C38—C42—H42A120.5
N3—C13—H13A118.7La—O7—H7B138.5
C14—C13—H13A118.7La—O7—H7A102.7
C15—C14—C13119.56 (18)H7B—O7—H7A116.5
C15—C14—H14A120.2La—O8—H8B142.8
C13—C14—H14A120.2La—O8—H8A112.7
C14—C15—C16119.96 (17)H8B—O8—H8A99.3
C14—C15—H15A120.0H9B—O9—H9A107.0
C16—C15—H15A120.0H10B—O10—H10A111.5
C15—C16—C24117.56 (17)H11B—O11—H11A101.5
C15—C16—C17123.12 (17)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O10.851.772.612 (2)172
O7—H7B···O9i0.851.852.701 (2)178
O8—H8A···O50.851.822.643 (2)163
O8—H8B···O100.851.902.744 (2)176
O9—H9A···O10ii0.851.962.786 (2)164
O9—H9B···O11iii0.851.922.763 (2)173
O10—H10A···O3iii0.851.892.731 (2)172
O10—H10B···O2iii0.852.052.886 (2)169
O11—H11A···N60.852.042.868 (2)165
O11—H11B···N5iv0.852.052.894 (2)174
Symmetry codes: (i) x, y+1, z; (ii) x, y1, z; (iii) x1, y, z; (iv) x+2, y+1, z+1.

Experimental details

Crystal data
Chemical formula[La(C6H4NO2)3(C12H8N2)2(H2O)2]·3H2O
Mr955.70
Crystal system, space groupTriclinic, P1
Temperature (K)290
a, b, c (Å)9.0676 (1), 12.9618 (2), 17.9351 (3)
α, β, γ (°)84.998 (1), 80.800 (1), 84.190 (1)
V3)2064.73 (5)
Z2
Radiation typeMo Kα
µ (mm1)1.10
Crystal size (mm)0.20 × 0.20 × 0.18
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.791, 0.811
No. of measured, independent and
observed [I > 2σ(I)] reflections
45880, 12414, 11284
Rint0.020
(sin θ/λ)max1)0.718
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.054, 1.04
No. of reflections12414
No. of parameters552
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.26

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

Selected bond lengths (Å) top
La—O42.4199 (10)La—N22.7565 (12)
La—O62.5200 (10)La—N32.7566 (12)
La—O22.5355 (10)La—N42.7678 (11)
La—O72.5367 (10)La—N12.7757 (11)
La—O82.5416 (10)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O10.851.772.612 (2)172
O7—H7B···O9i0.851.852.701 (2)178
O8—H8A···O50.851.822.643 (2)163
O8—H8B···O100.851.902.744 (2)176
O9—H9A···O10ii0.851.962.786 (2)164
O9—H9B···O11iii0.851.922.763 (2)173
O10—H10A···O3iii0.851.892.731 (2)172
O10—H10B···O2iii0.852.052.886 (2)169
O11—H11A···N60.852.042.868 (2)165
O11—H11B···N5iv0.852.052.894 (2)174
Symmetry codes: (i) x, y+1, z; (ii) x, y1, z; (iii) x1, y, z; (iv) x+2, y+1, z+1.
 

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