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Acta Crystallographica Section E: Crystallographic Communications logoLink to Acta Crystallographica Section E: Crystallographic Communications
. 2025 Jan 1;81(Pt 1):85–89. doi: 10.1107/S2056989024012349

Crystal structure of di-μ-acetato-κ4O:O′-bis{(acetato-κ2O,O′)tetra­aqua­[1-(pyridin-2-yl­methylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate

Mbossé Ndiaye-Gueye a, Bocar Traoré a, Ibrahima Elhadji Thiam a,*, Ousmane Diouf a, Emmanuel Wenger b, Abdou Salam Sall a, Claude Lecomte b, Mohamed Gaye a
Editor: S Parkinc
PMCID: PMC11701776  PMID: 39776632

In the title Schiff base binuclear lanthanum(III) complex, the two metal ions have the same environment and the LaIII ion is coordinated by three soft nitro­gen atoms from the Schiff base ligand, four hard oxygen atoms from carboxyl­ate co-ligands and two water oxygen atoms. Each LaIII ion is nine coordinate and its environment is best described as a tricapped trigonal–prismatic geometry.

Keywords: lanthanum; crystal structure; 2-hydrazino­pyridine,hydrazone

Abstract

In the binuclear title complex, [La2(C2H3O2)4(C11H10N4)(H2O)4](NO3)2·0.5H2O, the two lanthanum ions are nine coordinate in a distorted trigonal–prismatic geometry. Each LaIII ion is bonded to three N atoms of the Schiff base, 1-(pyridin-2-yl)-2-(pyridin-2-yl­methyl­ene)hydrazine and is coordinated by one acetate group, which acts in η2-bidentate mode and two acetate groups that act in μ2-mode between the two LaIII ions. Two η1-water mol­ecules complete the coordination sphere. All bond lengths in the coordination environment of the LaIII ion are slightly larger than those observed in the isostructural NdIII and SmIII complexes. The LaIII⋯LaIII distance is 4.6696 (6) Å. In the crystal, extensive O—H⋯O hydrogen-bonding inter­actions involving the coordinated water mol­ecules and the non-coordinating nitrate anions, as well as the oxygen atoms of the acetate groups, generate an overall three-dimensional supra­molecular network.

1. Chemical context

Lanthanide–Schiff base complexes are widely used in applied and fundamental sciences. Chemists continue to pay much attention in the preparation of functional Schiff bases and their lanthanide complexes, which can be used in many fields such as catalysis (Bell et al., 2022), radiopharmaceuticals (Hu & Wilson, 2022), fluoro­immuno assay reagents (Wu et al., 2024; Dong et al., 2023), diagnostic tools in biology (Liu et al., 2020; Zapolotsky et al., 2022), and in laser development (Lapaev et al., 2019). The use of acyclic Schiff bases allows the introduction of two identical or different metal ions (Geng et al., 2022; Bryleva et al., 2023). The presence of multiple coordination sites and the versatile coordination modes provide several possible structures with lanthanide ions (Le Fur et al., 2018; Kariaka et al., 2019). Organic ligands that are used as precursors for the structural design of complexes can have hard and/or soft sites such as oxygen, nitro­gen or sulfur atoms. Through proper design, the mol­ecular structure of the ligand can be controlled to have suitable sites to coordinate metal ions to generate specific architectures. The introduction of co-ligands offers multiple possibilities to develop original structures. Carboxyl­ate groups are versatile co-ligands, which can adopt various coordination modes, to generate different structures with the same ligand (Grebenyuk et al., 2021; Wang et al., 2012). However, lanthanides can have high and variable coordination numbers, depending on the synthesis conditions of the complexes. Indeed, the synthesis of these compounds is considerably influenced by the reaction procedures and conditions such as the nature of the solvent, pH, temperature and/or reaction time (Sinchow et al., 2019). This provides a versatility in coordination geometries that makes it difficult to predict the structures and properties of lanthanide com­pounds. In this context, for the synthesis of lanthanide(III) complexes, the Schiff base 1-(pyridin-2-yl­methyl­idene)-2-(pyridin-2-yl)hydrazine (HL), which provides three soft donor N atoms from two pyridine rings and an azomethine unit, was used in the presence of acetate anions as co-ligands, which provide hard donor O atoms. Several complexes from the ligand HL have been reported by our group (Gueye, Dieng et al., 2017; Ndiaye-Gueye, Dieng, Thiam, Sow et al., 2017; Sarr et al., 2018). In all of these complexes, the acetate group is either bidentate chelating η2-OOCH3, bridging μ2-OOCH3 or bidentate bridging η2:μ2-OOCH3. This report presents the synthesis, characterization, and X-ray structure of a lanthanum (III) complex derived from 1-(pyrydin-2­yl)-2-(pyridine-2-yl­methyl­ene)hydrazine (HL) and an acetate group as co-ligand.1.

2. Structural commentary

A mixture of the ligand HL [1-(pyridin-2-yl)-2-(pyridin-2-yl­methyl­ene)hydrazine], lanthanum nitrate, and acetate salts in a 1:1:3 ratio yields the title compound, which crystallographic studies reveal to be a dicationic binuclear complex with a 1:1:2 stoichiometric ratio. The crystal structure exhibits disorder involving both the ligand and the nitrate group. The site occupancy factors (SOFs) for the two disordered parts of the ligand refine to 0.547 (9) and 0.453 (9). For the nitrate group, the SOFs refine to 0.826 (9) and 0.174 (9). The following analysis of the crystal structure focuses on the major disorder components. The structure of the lanthanum acetato-bridged complex is built from two identical entities {La(HL)(η2-OOCH3)(η1-HO2)2} bridged by two acetate anions acting in μ2-OOCH3 mode, yielding a binuclear dianionic complex containing two uncoordinated nitrate anions and a partial occupancy non-coordinating water mol­ecule (Figs. 1 and 2). Each LaIII ion is coordinated by one HL ligand coordinated through two 2-pyridyl nitro­gen atoms and one azomethine nitro­gen atom. The coordination of the Schiff base forms two five-membered rings (LaNCNN) and (LaNCCN) with bite angles of 59.99 (9) and 59.43 (10)°, respectively, in the major disorder component. Additionally, each LaIII ion is coordinated by one chelating-bidentate acetate group acting in η2-OOCH3 mode and two chelating-monodentate water mol­ecules acting in η1-HO2 mode. Thus, the LaIII ions are nine coordinate and their environments are best described as a strongly distorted tricapped trigonal–prismatic geometry. The atoms N4/N3/O5 and O2/O3/O4 define the slanted base faces of the trigonal–tricapped environment. These two planes are twisted and form a dihedral angle of 57.37 (2)°. The three caps are occupied by O1, N1 and N2 atoms. The lanthanum cation is situated 1.320 (4) Å out of the plane defined by the caps O1, N1 and N2 of the polyhedron. The La—N distances (Table 1) are slightly longer than those found for the analogous complex of the NdIII ion with the same ligand [2.675 (3), 2.637 (2) and 2.639 (2) Å] (Ndiaye-Gueye, Dieng, Thiam, Sow et al., 2017; Ndiaye-Gueye, Dieng, Thiam, Lo et al., 2017; Gueye, Dieng et al., 2017; Gueye, et al. 2021). The La—O distances s fall in the range reported for other carboxyl­ate complexes (Gueye, Moussa et al., 2017; Bag et al., 2013; Chen et al., 2014). The distances for La—OH2 are comparable to the values in the complex [{Ln(HL(η2-OOCH3)2(η1-H2O)2}{μ2-OOCH3)2}{Ln(HL)(η2-OOCH3)2}(η1-H2O)2]·2NO3, (where Ln = Nd or Sm) (Ndiaye-Gueye, Dieng, Thiam, Lo, et al., 2017). The LaIII⋯LaIII distance is 4.6696 (6) Å and the value of the bridging angle O3— La1—O10 is 109.21 (5)°. The C6—N3 distance of 1.289 (7) Å is consistent with double-bond character. The bond lengths in the chain C—CH=N—NH—C bridging two pyridine rings are [1.443 (6) Å for PyC—C, 1.289 (7) Å for CH=N, 1.346 (6) Å for N—N and 1.377 (6) Å C—CPy] and are significantly different from the corresponding mean values for this ligand found in the CSD [1.450 (17), 1.283 (15), 1.349 (12) and 1.376 (16) Å, respectively].

Figure 1.

Figure 1

A view of the title compound, showing the atom-numbering scheme for the asymmetric unit. Displacement ellipsoids are drawn at the 30% probability level.

Figure 2.

Figure 2

The nature of disorder of the ligand and nitrate anion.

Table 1. Selected bond lengths (Å).

La1—O1 2.5659 (14) La1—O10 2.4814 (14)
La1—O2 2.5395 (15) La1—N1 2.626 (8)
La1—O3 2.5184 (16) La1—N3 2.683 (7)
La1—O4 2.5653 (15) La1—N4 2.768 (6)
La1—O5 2.6073 (16)    

3. Supra­molecular features

The title complex [{La(HL)(η2-OOCH3)(η1-H2O)2}{(μ2-OOCH3)2}{La(HL)(η2-OOCH3)(η1-H2O)2}]·2NO3·0.5(H2O) features both coordinated and solvent water mol­ecules. The unbound solvent water is present at partial occupancy. An intra­molecular hydrogen bond is formed between the OH group of a coordinated water mol­ecule, acting as donor, and an oxygen atom (O7) of a free nitrate group, acting as acceptor (O1—H1B⋯O7). In addition, inter­molecular hydrogen bonds involving the OH groups of coordinated water mol­ecules are significant in the construction of the structure. These OH groups act as donors to the nitrate oxygen atoms of free nitrate groups (O1—H1A⋯O8i and O2—H2B⋯O7i; symmetry codes as in Table 1) and to oxygen atoms of bidentate chelating acetate groups (O2—H2A⋯O4ii). The NH group of the hydrazine moiety inter­acts with an oxygen atom of a bidentate chelating acetate group, further consolidating the structure through the hydrogen bond N2—H2⋯O5iii. Weak inter­molecular C—H⋯O hydrogen bonds are also observed between CH groups and oxygen atoms of the bidentate chelating acetate groups, as summarized in Table 1. These hydrogen bonds collectively connect the mol­ecules of the complex into a three-dimensional network (Table 2, Fig. 3).

Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A D—H H⋯A DA D—H⋯A
O1—H1A⋯O6 0.76 (1) 2.27 (2) 2.994 (3) 158 (3)
O1—H1A⋯O7 0.76 (1) 2.59 (2) 3.273 (6) 151 (2)
O1—H1A⋯O6′ 0.76 (1) 2.19 (2) 2.901 (14) 154 (2)
O1—H1B⋯O8i 0.76 (1) 2.03 (2) 2.793 (4) 176 (3)
O1—H1B⋯O8′i 0.76 (1) 1.97 (3) 2.73 (2) 171 (3)
O2—H2A⋯O4ii 0.76 (1) 1.95 (2) 2.6971 (19) 168 (3)
O2—H2B⋯O7i 0.76 (1) 2.03 (2) 2.786 (4) 171 (3)
O2—H2B⋯N5′i 0.76 (1) 2.68 (2) 3.419 (16) 164 (3)
O2—H2B⋯O7′i 0.76 (1) 1.79 (3) 2.54 (2) 167 (3)
C13—H13A⋯O7iii 0.96 2.53 3.483 (5) 170
C13—H13A⋯O7′iii 0.96 2.33 3.27 (3) 167
C13—H13C⋯O7iv 0.96 2.65 3.544 (6) 155
C15—H15A⋯O9 0.96 2.62 3.350 (10) 133
C2—H2⋯O6v 0.93 2.57 3.420 (6) 153
N2—H2C⋯O5iv 0.86 2.13 2.898 (7) 149
C11—H11⋯O9 0.93 2.57 3.150 (10) 121
N2′—H2′A⋯O5iv 0.86 2.30 3.028 (7) 142
C6′—H6′⋯O5iv 0.93 2.32 3.067 (9) 138
C10′—H10′⋯O6′v 0.93 2.34 3.260 (18) 170
O9—H9A⋯O6vi 0.76 (2) 2.66 (14) 3.062 (9) 115 (13)
O9—H9B⋯O8vi 0.76 (2) 2.57 (10) 3.241 (11) 147 (16)

Symmetry codes: (i) Inline graphic; (ii) Inline graphic; (iii) Inline graphic; (iv) Inline graphic; (v) Inline graphic; (vi) Inline graphic.

Figure 3.

Figure 3

A partial packing plot showing diperiodic sheets that extend parallel to the bc plane.

4. Database survey

A search of the Cambridge Structural Database (CSD version 5.44, updates of September 2023; Groom et al., 2016) indicated 27 compounds incorporating the ligand 1-(pyridin-2-yl­methyl­idene)-2-(pyridin-2-yl)hydrazine, which has been widely used in coordination chemistry. Seven examples of complexes of the above ligand with f-block metal ions are known from the literature: BEHFUS and TESXOH (Gueye, Dieng et al., 2017), PCPHYB (Baraniak et al., 1976), TIKDAV and TIKCUO (Ndiaye-Gueye, Dieng, Thiam, Lo, et al., 2017), ZEFJOM (Gueye, Moussa et al., 2017), GIJYAD (Ndiaye-Gueye et al., 2022). Three structures are available for the Ca2+ metal ion: NIWLEM, NIWLIQ and NIWLOW (Vantomme, Hafezi et al., 2014). One Co2+ (PAPCOC10; Gerloch, 1966) and two Mn2+ [PEQMAC (Sarr et al., 2018), SIZPID01 (Diop et al., 2019)] structures are reported in the CSD. Nine entries for Cu2+ are found: DIMLEQ10 and DIMLIU01 (Rojo et al., 1988), JAWRII (Mesa et al., 1988), SAHDOU (Mesa et al., 1989), REJMEY and REJMIC (Ainscough et al., 1996), QUJTIZ (Chowdhury et al., 2009) TUSWEK (Mukherjee et al., 2010), FAFZOF (U-wang et al., 2020). Five Zn2+ structures: GECWAP and GECWIX (Vantomme, Jiang et al., 2014), SAVQAI and SAVQEM (Dumitru et al., 2005), SIZPOJ01 (Diop et al., 2019) are also reported in the CSD.

5. Synthesis and crystallization

A mixture of 2-hydrazino­pyridine (1 mmol) and 2-pyridine­carbaldehyde (1 mmol) in ethanol (15 mL) was stirred under reflux for 30 min. A mixture of sodium acetate (3 mmol) and La(NO3)3·6H2O (1 mmol) in ethanol (10 mL) was added to the solution. The mixture was stirred for 30 min and the resulting yellow solution was filtered and the filtrate was kept at 298 K. A yellow powder appeared after one day and was collected by filtration. Recrystallization by slow evaporation of an ethanol solution gave X-ray quality crystals of the compound [C30H40LaN8O12]·2NO3·0.5H2O. Yield 65%. Analysis calculated C, 32.30; H, 3.70; N, 12.56. Found: C, 32.27; H, 3.73; N, 12.52. %.

6. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3. Hydrogen atoms were found in difference-Fourier maps, but subsequently included in the refinement using riding models, with constrained distances set to 0.93 Å (Csp2—H), 0.96 Å (RCH3) and 0.86 Å (Nsp2—H). Water hydrogen atoms were refined using 1,2 and 1,3 distance restraints. Uiso(H) parameters were set to values of either 1.2Ueq or 1.5Ueq (RCH3 and H2O only) of the attached atom. To ensure satisfactory refinement for disordered groups in the structure, a combination of constraints and restraints was employed. Constraints (SHELXL command EADP) were used to fix Uij of overlapping fragments. Restraints were used to ensure the integrity of ill-defined or disordered groups (SHELXL commands SAME, DFIX, CHIV, SIMU, and RIGU).

Table 3. Experimental details.

Crystal data
Chemical formula [La2(C2H3O2)4(C11H10N4)(H2O)4](NO3)2·0.5H2O
M r 1115.55
Crystal system, space group Monoclinic, P21/c
Temperature (K) 293
a, b, c (Å) 11.1170 (11), 17.8366 (19), 11.8094 (12)
β (°) 114.213 (3)
V3) 2135.7 (4)
Z 2
Radiation type Mo Kα
μ (mm−1) 2.06
Crystal size (mm) 0.2 × 0.2 × 0.1
 
Data collection
Diffractometer Bruker X8
Absorption correction Numerical (SADABS; Krause et al., 2015)
Tmin, Tmax 0.215, 0.424
No. of measured, independent and observed [I > 2σ(I)] reflections 72063, 10392, 7368
R int 0.084
(sin θ/λ)max−1) 0.836
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.064, 1.04
No. of reflections 10392
No. of parameters 451
No. of restraints 781
H-atom treatment H atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3) 1.26, −0.95

Computer programs: APEX5 (Bruker, 2023), SHELXT (Sheldrick, 2015a), SHELXL (Sheldrick, 2015b) and OLEX2 (Dolomanov et al., 2009).

Supplementary Material

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989024012349/pk2715sup1.cif

e-81-00085-sup1.cif (2.1MB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989024012349/pk2715Isup2.hkl

e-81-00085-Isup2.hkl (824.6KB, hkl)

CCDC reference: 2412041

Additional supporting information: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the PMD2X X-ray diffraction facility of the CRM2 laboratory, Université de Lorraine, for the X-ray diffraction measurements, data processing and analysis, and providing of reports for publication: https://crm2.univ-lorraine.fr/plateformes/pmd2x.

supplementary crystallographic information

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Crystal data

[La2(C2H3O2)4(C11H10N4)(H2O)4](NO3)2·0.5H2O F(000) = 1106
Mr = 1115.55 Dx = 1.735 Mg m3
Monoclinic, P21/c Mo Kα radiation, λ = 0.71073 Å
a = 11.1170 (11) Å Cell parameters from 21184 reflections
b = 17.8366 (19) Å θ = 2.7–29.4°
c = 11.8094 (12) Å µ = 2.06 mm1
β = 114.213 (3)° T = 293 K
V = 2135.7 (4) Å3 Block, metallic yellowish yellow
Z = 2 0.2 × 0.2 × 0.1 mm

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Data collection

Bruker X8 diffractometer 7368 reflections with I > 2σ(I)
Detector resolution: 10 pixels mm-1 Rint = 0.084
Single crystals were positioned at 35, 40, 35, and 28 mm from the detector scans θmax = 36.4°, θmin = 2.2°
Absorption correction: numerical (SADABS; Krause et al., 2015) h = −16→18
Tmin = 0.215, Tmax = 0.424 k = −29→29
72063 measured reflections l = −19→19
10392 independent reflections

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Refinement

Refinement on F2 Hydrogen site location: mixed
Least-squares matrix: full H atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.039 w = 1/[σ2(Fo2) + (0.0112P)2 + 1.5461P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.064 (Δ/σ)max = 0.003
S = 1.04 Δρmax = 1.26 e Å3
10392 reflections Δρmin = −0.94 e Å3
451 parameters Extinction correction: SHELXL (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
781 restraints Extinction coefficient: 0.00071 (13)

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Special details

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.

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x y z Uiso*/Ueq Occ. (<1)
La1 0.56737 (2) 0.95905 (2) 0.20467 (2) 0.01520 (3)
O1 0.71353 (15) 0.84746 (8) 0.31638 (13) 0.0207 (3)
H1A 0.737 (2) 0.8335 (14) 0.3831 (15) 0.031*
H1B 0.753 (2) 0.8249 (13) 0.289 (2) 0.031*
O2 0.52181 (16) 0.84992 (8) 0.05463 (13) 0.0247 (3)
H2A 0.490 (2) 0.8580 (14) −0.0147 (14) 0.037*
H2B 0.574 (2) 0.8205 (13) 0.062 (2) 0.037*
O3 0.77181 (16) 0.96048 (9) 0.16251 (13) 0.0295 (3)
O4 0.57600 (14) 1.10181 (8) 0.18261 (12) 0.0218 (3)
O5 0.46089 (19) 1.06485 (10) 0.28544 (14) 0.0360 (4)
C12 0.5029 (2) 1.11655 (12) 0.23852 (17) 0.0263 (5)
C13 0.4664 (3) 1.19661 (14) 0.2475 (2) 0.0449 (7)
H13A 0.431738 1.218889 0.166320 0.067*
H13B 0.543322 1.223772 0.300997 0.067*
H13C 0.400921 1.198418 0.280778 0.067*
O10 0.37451 (14) 0.99521 (9) 0.01294 (13) 0.0248 (3)
C14 0.2633 (2) 1.02384 (12) −0.05024 (18) 0.0207 (4)
C15 0.1712 (3) 1.04094 (18) 0.0093 (2) 0.0452 (7)
H15A 0.104232 1.002998 −0.012831 0.068*
H15B 0.130825 1.088904 −0.018859 0.068*
H15C 0.219407 1.041944 0.097847 0.068*
N1 0.7389 (8) 1.0127 (6) 0.4165 (8) 0.0154 (11) 0.547 (8)
C1 0.8351 (10) 1.0594 (7) 0.4194 (8) 0.0221 (14) 0.547 (8)
H1 0.837759 1.072530 0.344276 0.026* 0.547 (8)
C2 0.9305 (7) 1.0891 (5) 0.5271 (6) 0.0234 (12) 0.547 (8)
H2 0.993945 1.122342 0.524696 0.028* 0.547 (8)
C3 0.9276 (6) 1.0672 (4) 0.6394 (5) 0.0228 (10) 0.547 (8)
H3 0.990764 1.085119 0.714130 0.027* 0.547 (8)
C4 0.8317 (6) 1.0194 (3) 0.6390 (5) 0.0207 (10) 0.547 (8)
H4 0.828457 1.004507 0.713141 0.025* 0.547 (8)
C5 0.7388 (6) 0.9932 (4) 0.5261 (5) 0.0123 (9) 0.547 (8)
N2 0.6401 (5) 0.9460 (4) 0.5246 (6) 0.0156 (10) 0.547 (8)
H2C 0.637201 0.932701 0.593393 0.019* 0.547 (8)
N3 0.5482 (6) 0.9206 (4) 0.4163 (6) 0.0154 (10) 0.547 (8)
C6 0.4571 (7) 0.8775 (4) 0.4207 (6) 0.0175 (10) 0.547 (8)
H6 0.455719 0.865341 0.496698 0.021* 0.547 (8)
C7 0.3572 (5) 0.8483 (3) 0.3071 (5) 0.0192 (9) 0.547 (8)
C8 0.2639 (6) 0.7974 (3) 0.3128 (6) 0.0279 (11) 0.547 (8)
H8 0.266593 0.781473 0.388808 0.034* 0.547 (8)
C9 0.1675 (5) 0.7714 (3) 0.2022 (7) 0.0344 (13) 0.547 (8)
H9 0.104301 0.737475 0.202871 0.041* 0.547 (8)
C10 0.1663 (5) 0.7966 (3) 0.0905 (6) 0.0344 (12) 0.547 (8)
H10 0.101955 0.780214 0.015203 0.041* 0.547 (8)
C11 0.2632 (6) 0.8466 (4) 0.0937 (6) 0.0273 (12) 0.547 (8)
H11 0.262204 0.863073 0.018597 0.033* 0.547 (8)
N4 0.3581 (6) 0.8727 (3) 0.1988 (5) 0.0187 (9) 0.547 (8)
N1' 0.3780 (8) 0.8785 (5) 0.2388 (6) 0.0239 (13) 0.453 (8)
C1' 0.2781 (9) 0.8502 (5) 0.1387 (7) 0.0324 (15) 0.453 (8)
H1' 0.271747 0.863508 0.060346 0.039* 0.453 (8)
C2' 0.1839 (8) 0.8019 (5) 0.1470 (8) 0.0418 (16) 0.453 (8)
H2' 0.113781 0.784576 0.076477 0.050* 0.453 (8)
C3' 0.1993 (8) 0.7806 (4) 0.2654 (9) 0.0414 (16) 0.453 (8)
H3' 0.140352 0.746774 0.274681 0.050* 0.453 (8)
C4' 0.2991 (7) 0.8087 (4) 0.3674 (8) 0.0328 (14) 0.453 (8)
H4' 0.308199 0.795176 0.446545 0.039* 0.453 (8)
C5' 0.3880 (7) 0.8582 (4) 0.3514 (7) 0.0202 (11) 0.453 (8)
N2' 0.4887 (7) 0.8877 (4) 0.4527 (6) 0.0202 (12) 0.453 (8)
H2'A 0.493246 0.878841 0.525905 0.024* 0.453 (8)
N3' 0.5807 (7) 0.9306 (5) 0.4385 (7) 0.0145 (12) 0.453 (8)
C6' 0.6765 (8) 0.9552 (6) 0.5382 (8) 0.0174 (13) 0.453 (8)
H6' 0.680870 0.941845 0.615935 0.021* 0.453 (8)
C7' 0.7762 (7) 1.0032 (5) 0.5286 (7) 0.0178 (13) 0.453 (8)
C8' 0.8745 (7) 1.0334 (4) 0.6364 (6) 0.0236 (13) 0.453 (8)
H8' 0.879996 1.020580 0.714666 0.028* 0.453 (8)
C9' 0.9619 (8) 1.0821 (4) 0.6225 (7) 0.0286 (14) 0.453 (8)
H9' 1.027339 1.103938 0.691992 0.034* 0.453 (8)
C10' 0.9537 (9) 1.0992 (6) 0.5056 (8) 0.0290 (16) 0.453 (8)
H10' 1.013469 1.131946 0.495294 0.035* 0.453 (8)
C11' 0.8542 (12) 1.0663 (8) 0.4037 (10) 0.0228 (17) 0.453 (8)
H11' 0.848158 1.078181 0.324895 0.027* 0.453 (8)
N4' 0.7676 (9) 1.0191 (7) 0.4134 (9) 0.0162 (14) 0.453 (8)
N5 0.8120 (3) 0.7717 (2) 0.6227 (3) 0.0278 (7) 0.826 (9)
O6 0.8757 (3) 0.8140 (3) 0.5847 (4) 0.0629 (13) 0.826 (9)
O7 0.6941 (4) 0.7636 (2) 0.5548 (5) 0.0405 (8) 0.826 (9)
O8 0.8623 (4) 0.7415 (2) 0.7271 (3) 0.0445 (10) 0.826 (9)
N5' 0.8000 (16) 0.7501 (9) 0.5993 (15) 0.0278 (7) 0.174 (9)
O6' 0.8688 (15) 0.7717 (12) 0.5480 (17) 0.0629 (13) 0.174 (9)
O7' 0.6816 (18) 0.7484 (13) 0.543 (3) 0.0405 (8) 0.174 (9)
O8' 0.854 (2) 0.7191 (12) 0.7010 (16) 0.0445 (10) 0.174 (9)
O9 0.0421 (9) 0.8898 (6) −0.1673 (8) 0.062 (3) 0.25
H9A 0.016 (14) 0.907 (8) −0.232 (6) 0.093* 0.25
H9B −0.010 (11) 0.861 (7) −0.170 (13) 0.093* 0.25

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
La1 0.01924 (6) 0.01380 (5) 0.01228 (5) 0.00382 (5) 0.00618 (4) 0.00176 (4)
O1 0.0285 (8) 0.0184 (7) 0.0151 (6) 0.0072 (6) 0.0089 (6) 0.0030 (5)
O2 0.0375 (9) 0.0191 (7) 0.0136 (6) 0.0035 (6) 0.0064 (6) 0.0031 (5)
O3 0.0304 (8) 0.0409 (9) 0.0196 (7) 0.0064 (7) 0.0127 (6) 0.0083 (7)
O4 0.0318 (8) 0.0186 (7) 0.0125 (6) 0.0045 (6) 0.0064 (6) 0.0011 (5)
O5 0.0626 (12) 0.0311 (9) 0.0273 (8) 0.0265 (8) 0.0317 (8) 0.0145 (7)
C12 0.0427 (13) 0.0244 (11) 0.0113 (8) 0.0151 (10) 0.0105 (8) 0.0025 (7)
C13 0.083 (2) 0.0246 (13) 0.0345 (13) 0.0207 (13) 0.0311 (14) 0.0021 (10)
O10 0.0201 (7) 0.0258 (8) 0.0238 (7) 0.0059 (6) 0.0043 (6) 0.0010 (6)
C14 0.0190 (9) 0.0258 (11) 0.0193 (9) 0.0010 (8) 0.0098 (8) 0.0030 (7)
C15 0.0315 (13) 0.078 (2) 0.0347 (13) 0.0181 (14) 0.0220 (11) 0.0165 (14)
N1 0.015 (3) 0.019 (2) 0.0153 (16) −0.002 (2) 0.0085 (18) −0.0007 (13)
C1 0.025 (3) 0.027 (3) 0.018 (2) −0.004 (2) 0.0123 (18) 0.0013 (18)
C2 0.022 (3) 0.023 (3) 0.026 (2) −0.0031 (18) 0.0110 (18) −0.0020 (18)
C3 0.018 (3) 0.026 (3) 0.0196 (19) −0.0020 (19) 0.0038 (17) −0.0042 (18)
C4 0.019 (2) 0.025 (2) 0.0144 (16) −0.0004 (18) 0.0029 (17) −0.0022 (15)
C5 0.011 (2) 0.015 (2) 0.0098 (14) 0.0023 (17) 0.0035 (17) −0.0005 (13)
N2 0.017 (2) 0.019 (2) 0.012 (2) −0.0026 (18) 0.0074 (19) 0.0022 (15)
N3 0.016 (3) 0.014 (2) 0.015 (2) 0.0019 (17) 0.0041 (18) −0.0014 (15)
C6 0.020 (3) 0.018 (2) 0.017 (3) −0.0020 (19) 0.010 (2) 0.0026 (19)
C7 0.017 (2) 0.0185 (19) 0.022 (2) −0.0021 (15) 0.0081 (18) −0.0042 (17)
C8 0.027 (3) 0.026 (2) 0.033 (3) −0.0114 (19) 0.014 (2) −0.003 (2)
C9 0.025 (2) 0.035 (3) 0.043 (3) −0.0134 (19) 0.013 (2) −0.006 (2)
C10 0.025 (2) 0.034 (2) 0.039 (3) −0.0091 (18) 0.008 (2) −0.006 (2)
C11 0.021 (2) 0.030 (2) 0.023 (2) −0.0069 (17) 0.001 (2) −0.003 (2)
N4 0.019 (2) 0.0191 (19) 0.017 (2) −0.0019 (15) 0.0071 (19) −0.0002 (19)
N1' 0.027 (3) 0.024 (2) 0.019 (3) 0.003 (2) 0.008 (2) −0.003 (2)
C1' 0.031 (3) 0.039 (3) 0.025 (3) −0.003 (2) 0.009 (3) −0.002 (3)
C2' 0.035 (3) 0.046 (4) 0.038 (3) −0.010 (3) 0.009 (3) −0.006 (3)
C3' 0.035 (4) 0.041 (4) 0.046 (4) −0.013 (3) 0.015 (3) −0.003 (3)
C4' 0.030 (3) 0.032 (3) 0.038 (3) −0.006 (2) 0.015 (3) −0.001 (3)
C5' 0.021 (3) 0.020 (2) 0.022 (3) 0.0015 (19) 0.011 (2) 0.000 (2)
N2' 0.020 (3) 0.025 (3) 0.016 (3) −0.002 (2) 0.007 (2) 0.000 (2)
N3' 0.015 (3) 0.016 (3) 0.012 (3) 0.001 (2) 0.005 (2) 0.0004 (19)
C6' 0.018 (3) 0.023 (3) 0.0060 (19) 0.002 (2) −0.001 (2) −0.0032 (19)
C7' 0.013 (3) 0.017 (3) 0.020 (2) 0.002 (2) 0.004 (2) −0.0022 (17)
C8' 0.018 (3) 0.030 (3) 0.0148 (19) −0.005 (2) −0.002 (2) −0.005 (2)
C9' 0.022 (3) 0.025 (3) 0.030 (3) −0.004 (2) 0.002 (2) −0.006 (2)
C10' 0.026 (3) 0.023 (3) 0.033 (3) −0.002 (2) 0.007 (2) −0.002 (2)
C11' 0.021 (3) 0.021 (3) 0.026 (3) −0.003 (2) 0.010 (2) −0.001 (2)
N4' 0.014 (3) 0.018 (3) 0.015 (2) 0.004 (2) 0.005 (2) −0.0002 (17)
N5 0.0304 (12) 0.0219 (16) 0.0343 (15) 0.0066 (12) 0.0165 (12) 0.0098 (12)
O6 0.0440 (13) 0.064 (3) 0.090 (2) 0.0082 (16) 0.0369 (15) 0.050 (2)
O7 0.0407 (14) 0.025 (2) 0.0347 (14) −0.0131 (11) −0.0054 (11) 0.0036 (14)
O8 0.0282 (11) 0.059 (3) 0.0363 (16) −0.0100 (16) 0.0031 (13) 0.0233 (15)
N5' 0.0304 (12) 0.0219 (16) 0.0343 (15) 0.0066 (12) 0.0165 (12) 0.0098 (12)
O6' 0.0440 (13) 0.064 (3) 0.090 (2) 0.0082 (16) 0.0369 (15) 0.050 (2)
O7' 0.0407 (14) 0.025 (2) 0.0347 (14) −0.0131 (11) −0.0054 (11) 0.0036 (14)
O8' 0.0282 (11) 0.059 (3) 0.0363 (16) −0.0100 (16) 0.0031 (13) 0.0233 (15)
O9 0.047 (5) 0.069 (7) 0.047 (5) 0.007 (5) −0.004 (4) −0.017 (4)

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Geometric parameters (Å, º)

La1—O1 2.5659 (14) C7—C8 1.400 (7)
La1—O2 2.5395 (15) C7—N4 1.355 (6)
La1—O3 2.5184 (16) C8—H8 0.9300
La1—O4 2.5653 (15) C8—C9 1.386 (6)
La1—O5 2.6073 (16) C9—H9 0.9300
La1—O10 2.4814 (14) C9—C10 1.388 (7)
La1—N1 2.626 (8) C10—H10 0.9300
La1—N3 2.683 (7) C10—C11 1.388 (7)
La1—N4 2.768 (6) C11—H11 0.9300
La1—N1' 2.712 (8) C11—N4 1.339 (6)
La1—N3' 2.752 (8) N1'—C1' 1.345 (8)
La1—N4' 2.771 (9) N1'—C5' 1.338 (7)
O1—H1A 0.763 (14) C1'—H1' 0.9300
O1—H1B 0.760 (14) C1'—C2' 1.389 (10)
O2—H2A 0.761 (14) C2'—H2' 0.9300
O2—H2B 0.761 (14) C2'—C3' 1.390 (9)
O3—C14i 1.251 (2) C3'—H3' 0.9300
O4—C12 1.267 (3) C3'—C4' 1.356 (8)
O5—C12 1.260 (3) C4'—H4' 0.9300
C12—C13 1.500 (3) C4'—C5' 1.394 (8)
C13—H13A 0.9600 C5'—N2' 1.365 (6)
C13—H13B 0.9600 N2'—H2'A 0.8600
C13—H13C 0.9600 N2'—N3' 1.340 (8)
O10—C14 1.261 (2) N3'—C6' 1.298 (7)
C14—C15 1.491 (3) C6'—H6' 0.9300
C15—H15A 0.9600 C6'—C7' 1.441 (8)
C15—H15B 0.9600 C7'—C8' 1.401 (8)
C15—H15C 0.9600 C7'—N4' 1.355 (10)
N1—C1 1.345 (7) C8'—H8' 0.9300
N1—C5 1.340 (8) C8'—C9' 1.363 (8)
C1—H1 0.9300 C9'—H9' 0.9300
C1—C2 1.385 (9) C9'—C10' 1.379 (9)
C2—H2 0.9300 C10'—H10' 0.9300
C2—C3 1.396 (7) C10'—C11' 1.386 (11)
C3—H3 0.9300 C11'—H11' 0.9300
C3—C4 1.364 (6) C11'—N4' 1.319 (9)
C4—H4 0.9300 N5—O6 1.238 (3)
C4—C5 1.390 (6) N5—O7 1.233 (4)
C5—N2 1.377 (6) N5—O8 1.248 (3)
N2—H2C 0.8600 N5'—O6' 1.216 (14)
N2—N3 1.346 (6) N5'—O7' 1.208 (15)
N3—C6 1.289 (7) N5'—O8' 1.231 (15)
C6—H6 0.9300 O9—H9A 0.761 (16)
C6—C7 1.443 (6) O9—H9B 0.762 (16)
O1—La1—O5 131.31 (5) N1—C1—C2 124.2 (6)
O1—La1—N1 74.6 (2) C2—C1—H1 117.9
O1—La1—N3 66.31 (17) C1—C2—H2 121.4
O1—La1—N4 85.96 (14) C1—C2—C3 117.2 (5)
O1—La1—N1' 83.07 (18) C3—C2—H2 121.4
O1—La1—N3' 65.1 (2) C2—C3—H3 120.2
O1—La1—N4' 74.6 (3) C4—C3—C2 119.6 (5)
O2—La1—O1 70.56 (5) C4—C3—H3 120.2
O2—La1—O4 134.03 (4) C3—C4—H4 120.5
O2—La1—O5 145.03 (6) C3—C4—C5 119.1 (5)
O2—La1—N1 143.4 (2) C5—C4—H4 120.5
O2—La1—N3 112.63 (15) N1—C5—C4 123.0 (5)
O2—La1—N4 68.32 (13) N1—C5—N2 117.5 (5)
O2—La1—N1' 75.71 (16) N2—C5—C4 119.5 (5)
O2—La1—N3' 118.17 (18) C5—N2—H2C 119.7
O2—La1—N4' 140.7 (3) N3—N2—C5 120.5 (5)
O3—La1—O1 71.15 (5) N3—N2—H2C 119.7
O3—La1—O2 78.91 (6) N2—N3—La1 118.6 (4)
O3—La1—O4 84.00 (5) C6—N3—La1 123.6 (4)
O3—La1—O5 130.31 (6) C6—N3—N2 117.8 (6)
O3—La1—N1 79.82 (16) N3—C6—H6 120.1
O3—La1—N3 127.56 (15) N3—C6—C7 119.8 (5)
O3—La1—N4 144.90 (14) C7—C6—H6 120.1
O3—La1—N1' 148.59 (18) C8—C7—C6 119.5 (5)
O3—La1—N3' 121.26 (17) N4—C7—C6 117.4 (4)
O3—La1—N4' 73.2 (2) N4—C7—C8 123.1 (4)
O4—La1—O1 141.26 (5) C7—C8—H8 120.9
O4—La1—O5 50.23 (5) C9—C8—C7 118.2 (5)
O4—La1—N1 72.1 (2) C9—C8—H8 120.9
O4—La1—N3 111.64 (16) C8—C9—H9 120.3
O4—La1—N4 128.03 (14) C8—C9—C10 119.4 (5)
O4—La1—N1' 127.18 (18) C10—C9—H9 120.3
O4—La1—N3' 107.23 (19) C9—C10—H10 120.8
O4—La1—N4' 69.9 (2) C9—C10—C11 118.5 (5)
O5—La1—N1 69.4 (2) C11—C10—H10 120.8
O5—La1—N3 67.84 (17) C10—C11—H11 118.1
O5—La1—N4 84.78 (14) N4—C11—C10 123.8 (5)
O5—La1—N1' 80.33 (18) N4—C11—H11 118.1
O5—La1—N3' 67.2 (2) C7—N4—La1 119.1 (3)
O5—La1—N4' 73.4 (2) C11—N4—La1 123.4 (4)
O10—La1—O1 143.00 (5) C11—N4—C7 117.1 (5)
O10—La1—O2 73.27 (5) C1'—N1'—La1 118.7 (5)
O10—La1—O3 109.21 (5) C5'—N1'—La1 122.6 (4)
O10—La1—O4 72.76 (5) C5'—N1'—C1' 118.2 (7)
O10—La1—O5 78.09 (5) N1'—C1'—H1' 118.5
O10—La1—N1 142.4 (2) N1'—C1'—C2' 123.0 (7)
O10—La1—N3 123.20 (15) C2'—C1'—H1' 118.5
O10—La1—N4 73.67 (12) C1'—C2'—H2' 121.5
O10—La1—N1' 80.82 (16) C1'—C2'—C3' 117.1 (6)
O10—La1—N3' 129.37 (18) C3'—C2'—H2' 121.5
O10—La1—N4' 142.2 (3) C2'—C3'—H3' 119.6
N1—La1—N3 60.63 (17) C4'—C3'—C2' 120.7 (6)
N1—La1—N4 120.08 (16) C4'—C3'—H3' 119.6
N3—La1—N4 59.61 (13) C3'—C4'—H4' 120.6
N1'—La1—N3' 58.56 (16) C3'—C4'—C5' 118.8 (6)
N1'—La1—N4' 117.50 (19) C5'—C4'—H4' 120.6
N3'—La1—N4' 59.0 (2) N1'—C5'—C4' 122.1 (6)
La1—O1—H1A 131.3 (18) N1'—C5'—N2' 118.0 (6)
La1—O1—H1B 123.4 (18) N2'—C5'—C4' 119.9 (6)
H1A—O1—H1B 105 (2) C5'—N2'—H2'A 119.8
La1—O2—H2A 118.5 (19) N3'—N2'—C5' 120.3 (6)
La1—O2—H2B 122 (2) N3'—N2'—H2'A 119.8
H2A—O2—H2B 105 (2) N2'—N3'—La1 120.0 (4)
C14i—O3—La1 107.31 (13) C6'—N3'—La1 122.3 (6)
C12—O4—La1 95.42 (13) C6'—N3'—N2' 117.6 (7)
C12—O5—La1 93.60 (13) N3'—C6'—H6' 120.0
O4—C12—C13 118.9 (2) N3'—C6'—C7' 120.1 (7)
O5—C12—O4 120.66 (19) C7'—C6'—H6' 120.0
O5—C12—C13 120.4 (2) C8'—C7'—C6' 119.7 (6)
C12—C13—H13A 109.5 N4'—C7'—C6' 117.6 (6)
C12—C13—H13B 109.5 N4'—C7'—C8' 122.6 (6)
C12—C13—H13C 109.5 C7'—C8'—H8' 121.1
H13A—C13—H13B 109.5 C9'—C8'—C7' 117.7 (6)
H13A—C13—H13C 109.5 C9'—C8'—H8' 121.1
H13B—C13—H13C 109.5 C8'—C9'—H9' 119.9
La1—O10—La1i 116.24 (6) C8'—C9'—C10' 120.2 (6)
C14—O10—La1i 83.51 (11) C10'—C9'—H9' 119.9
C14—O10—La1 156.33 (14) C9'—C10'—H10' 120.8
O3i—C14—La1i 50.25 (10) C9'—C10'—C11' 118.5 (7)
O3i—C14—O10 121.44 (19) C11'—C10'—H10' 120.8
O3i—C14—C15 118.55 (19) C10'—C11'—H11' 118.5
O10—C14—La1i 72.88 (11) N4'—C11'—C10' 123.1 (8)
O10—C14—C15 120.00 (19) N4'—C11'—H11' 118.5
C15—C14—La1i 161.51 (17) C7'—N4'—La1 120.9 (5)
C14—C15—H15A 109.5 C11'—N4'—La1 121.2 (6)
C14—C15—H15B 109.5 C11'—N4'—C7' 117.9 (8)
C14—C15—H15C 109.5 O6—N5—O8 122.0 (3)
H15A—C15—H15B 109.5 O7—N5—O6 116.7 (3)
H15A—C15—H15C 109.5 O7—N5—O8 121.2 (4)
H15B—C15—H15C 109.5 O6'—N5'—O8' 118.5 (17)
C1—N1—La1 120.6 (5) O7'—N5'—O6' 120.1 (19)
C5—N1—La1 122.5 (4) O7'—N5'—O8' 120.4 (19)
C5—N1—C1 116.8 (6) H9A—O9—H9B 104 (3)
N1—C1—H1 117.9
La1—O4—C12—O5 3.1 (2) C7—C8—C9—C10 −0.2 (8)
La1—O4—C12—C13 −176.59 (19) C8—C7—N4—La1 −172.4 (4)
La1—O5—C12—O4 −3.0 (2) C8—C7—N4—C11 0.8 (9)
La1—O5—C12—C13 176.64 (19) C8—C9—C10—C11 0.6 (9)
La1—O10—C14—La1i 148.0 (3) C9—C10—C11—N4 −0.4 (10)
La1i—O10—C14—O3i 13.4 (2) C10—C11—N4—La1 172.5 (5)
La1—O10—C14—O3i 161.5 (2) C10—C11—N4—C7 −0.3 (10)
La1i—O10—C14—C15 −165.5 (2) N4—C7—C8—C9 −0.6 (8)
La1—O10—C14—C15 −17.4 (5) N1'—C1'—C2'—C3' −2.6 (13)
La1—N1—C1—C2 −178.9 (9) N1'—C5'—N2'—N3' −5.7 (11)
La1—N1—C5—C4 177.9 (5) C1'—N1'—C5'—C4' 0.3 (11)
La1—N1—C5—N2 −3.2 (10) C1'—N1'—C5'—N2' −179.3 (7)
La1—N3—C6—C7 −1.0 (9) C1'—C2'—C3'—C4' 2.6 (12)
La1—N1'—C1'—C2' 173.1 (7) C2'—C3'—C4'—C5' −1.3 (11)
La1—N1'—C5'—C4' −171.4 (5) C3'—C4'—C5'—N1' −0.2 (11)
La1—N1'—C5'—N2' 9.0 (9) C3'—C4'—C5'—N2' 179.4 (7)
La1—N3'—C6'—C7' 4.1 (12) C4'—C5'—N2'—N3' 174.7 (8)
N1—C1—C2—C3 1.8 (15) C5'—N1'—C1'—C2' 1.2 (13)
N1—C5—N2—N3 0.3 (10) C5'—N2'—N3'—La1 −0.2 (10)
C1—N1—C5—C4 0.5 (12) C5'—N2'—N3'—C6' −177.8 (8)
C1—N1—C5—N2 179.4 (8) N2'—N3'—C6'—C7' −178.3 (8)
C1—C2—C3—C4 −1.1 (11) N3'—C6'—C7'—C8' 175.9 (9)
C2—C3—C4—C5 0.3 (9) N3'—C6'—C7'—N4' −2.0 (13)
C3—C4—C5—N1 0.1 (10) C6'—C7'—C8'—C9' −176.0 (7)
C3—C4—C5—N2 −178.8 (6) C6'—C7'—N4'—La1 −1.0 (12)
C4—C5—N2—N3 179.3 (6) C6'—C7'—N4'—C11' 176.2 (10)
C5—N1—C1—C2 −1.5 (15) C7'—C8'—C9'—C10' −1.3 (11)
C5—N2—N3—La1 2.5 (8) C8'—C7'—N4'—La1 −178.9 (6)
C5—N2—N3—C6 −179.0 (7) C8'—C7'—N4'—C11' −1.7 (15)
N2—N3—C6—C7 −179.4 (6) C8'—C9'—C10'—C11' 0.7 (14)
N3—C6—C7—C8 175.6 (6) C9'—C10'—C11'—N4' −0.6 (18)
N3—C6—C7—N4 −5.1 (9) C10'—C11'—N4'—La1 178.2 (10)
C6—C7—C8—C9 178.7 (5) C10'—C11'—N4'—C7' 1.0 (18)
C6—C7—N4—La1 8.3 (7) N4'—C7'—C8'—C9' 1.8 (12)
C6—C7—N4—C11 −178.5 (6)

Symmetry code: (i) −x+1, −y+2, −z.

Di-µ-acetato-κ4O:O'-bis{(acetato-κ2O,O')tetraaqua[1-(pyridin-2-ylmethylidene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]lanthanum(III)} dinitrate hemihydrate . Hydrogen-bond geometry (Å, º)

D—H···A D—H H···A D···A D—H···A
O1—H1A···O6 0.76 (1) 2.27 (2) 2.994 (3) 158 (3)
O1—H1A···O7 0.76 (1) 2.59 (2) 3.273 (6) 151 (2)
O1—H1A···O6′ 0.76 (1) 2.19 (2) 2.901 (14) 154 (2)
O1—H1B···O8ii 0.76 (1) 2.03 (2) 2.793 (4) 176 (3)
O1—H1B···O8′ii 0.76 (1) 1.97 (3) 2.73 (2) 171 (3)
O2—H2A···O4i 0.76 (1) 1.95 (2) 2.6971 (19) 168 (3)
O2—H2B···O7ii 0.76 (1) 2.03 (2) 2.786 (4) 171 (3)
O2—H2B···N5′ii 0.76 (1) 2.68 (2) 3.419 (16) 164 (3)
O2—H2B···O7′ii 0.76 (1) 1.79 (3) 2.54 (2) 167 (3)
C13—H13A···O7iii 0.96 2.53 3.483 (5) 170
C13—H13A···O7′iii 0.96 2.33 3.27 (3) 167
C13—H13C···O7iv 0.96 2.65 3.544 (6) 155
C15—H15A···O9 0.96 2.62 3.350 (10) 133
C2—H2···O6v 0.93 2.57 3.420 (6) 153
N2—H2C···O5iv 0.86 2.13 2.898 (7) 149
C11—H11···O9 0.93 2.57 3.150 (10) 121
N2′—H2′A···O5iv 0.86 2.30 3.028 (7) 142
C6′—H6′···O5iv 0.93 2.32 3.067 (9) 138
C10′—H10′···O6′v 0.93 2.34 3.260 (18) 170
O9—H9A···O6vi 0.76 (2) 2.66 (14) 3.062 (9) 115 (13)
O9—H9B···O8vi 0.76 (2) 2.57 (10) 3.241 (11) 147 (16)

Symmetry codes: (i) −x+1, −y+2, −z; (ii) x, −y+3/2, z−1/2; (iii) −x+1, y+1/2, −z+1/2; (iv) −x+1, −y+2, −z+1; (v) −x+2, −y+2, −z+1; (vi) x−1, y, z−1.

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989024012349/pk2715sup1.cif

e-81-00085-sup1.cif (2.1MB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989024012349/pk2715Isup2.hkl

e-81-00085-Isup2.hkl (824.6KB, hkl)

CCDC reference: 2412041

Additional supporting information: crystallographic information; 3D view; checkCIF report


Articles from Acta Crystallographica Section E: Crystallographic Communications are provided here courtesy of International Union of Crystallography

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