Whole-mol­ecule disorder of the heterometallic complex di­aqua-1κ2O-di­chlorido-2κ2Cl-(μ-2-formyl-6-meth­oxy­phenolato-1κ2O1,O2:2κO6){μ-2-meth­oxy-6-[(methyl­imino)­meth­yl]phenolato-1κ2N,O1:2κO6}lead(II)nickel(II)

Vassilyeva, O.Y.; Kokozay, V.N.; Goreshnik, E.

doi:10.1107/S2056989025005857

research communications

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ISSN: 2056-9890

Volume 81| Part 8| August 2025| Pages 667-671

https://doi.org/10.1107/S2056989025005857

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Whole-molecule disorder of the heterometallic complex diaqua-1κ²O-dichlorido-2κ²Cl-(μ-2-formyl-6-methoxyphenolato-1κ²O¹,O²:2κO⁶){μ-2-methoxy-6-[(methylimino)methyl]phenolato-1κ²N,O¹:2κO⁶}lead(II)nickel(II)

Olga Yu. Vassilyeva,^a ^* Vladimir N. Kokozay ^a and Evgeny Goreshnik ^b

^aDepartment of Chemistry, Taras Shevchenko National University of Kyiv, 12, Hetman Pavlo Skoropadskyi str., 01601 Kyiv, Ukraine, and ^bDepartment of Inorganic Chemistry and Technology, Jozef Stefan Institute, Jamova 39, 1000 Ljubljana, Slovenia
^*Correspondence e-mail: [email protected]

Edited by N. Alvarez Failache, Universidad de la Repüblica, Uruguay (Received 22 May 2025; accepted 27 June 2025; online 1 July 2025)

The new molecular complex [NiPb(C₉H₁₀NO₂)(C₈H₇NO₃)Cl₂(H₂O)₂] with the Schiff base 2-methoxy-6-[(methylimino)methyl]phenol and ortho-vanillin ligands, both deprotonated, crystallizes in the monoclinic space group P2₁/c with one molecule per asymmetric unit. The heterometallic molecule exhibits a whole-molecule orientational disorder [occupancy ratio 0.711 (6): 0.289 (6)] about a pseudo-twofold rotation axis that roughly bisects the molecule along the Ni–Pb axis. The Ni centre coordination is distorted octahedral [Ni—N/O_eq = 1.996 (8)–2.021 (7) Å, major component] with two water molecules in the apexes [2.088 (6) and 2.090 (5) Å]. The Pb atom is six-coordinate in a highly distorted tetragonal–bipyramidal geometry. Two phenolato and two methoxo O atoms from the deprotonated ligand moieties are nearly coplanar with the metal centre [Pb–O 2.301 (8)–2.740 (10) Å, major component], while the two chlorides are located on opposite sides of the plane [Pb—Cl = 2.821 (5) and 2.868 (5) Å]. The Ni–Pb pair of metals is bridged by two phenolato O atoms enabling a metal–metal separation of 3.441 (3)/3.477 (7) Å. Two intramolecular O–H⋯Cl hydrogen bonds between coordinated aqua and chloride ligands appear to be a reason for the Cl–Pb–Cl and O–Ni–O angles being far from 180°. In the solid state, the well-separated heterometallic molecules are interlinked by π–π stacking and weak O—H⋯Cl and C—H⋯Cl/O hydrogen bonds. The molecules show no significant intermolecular interactions: the minimal M⋯M distance in the crystal is about 7.65 Å (Ni⋯Pb).

Keywords: crystal structure; heterometallic complex; Schiff base ligand; o-vanillin; methylamine.

CCDC reference: 2467901

1. Chemical context

Heterometallic complexes comprising metals of different kinds are attractive objects of research in several important fields of scientific interest such as bioinorganic, medicinal and materials chemistry (Becker, 2024 ). Studying synthetic heterometallic compounds helps to understand the structure, bonding, and reaction mechanisms of natural metalloenzymes that feature multinuclear active sites, containing dissimilar metal ions. Ensued practical applications may lead to low-molecular catalysts that are significantly more active, selective, or capable of mediating reactions impossible with single-metal catalysts (Campos, 2020 ). Heterometallic drugs that integrate traceability and therapy in one system (theranostic agents) have emerged as a promising alternative to conventional metallodrugs (Redrado et al., 2021 ). Theranostic agents are becoming increasingly important in cancer research. Cooperativity of different metals within a single molecular entity is crucial for developing new materials like single-molecule magnets (SMMs), where interactions between different types of spin carriers (e.g., transition metals and lanthanides) are engineered to achieve high magnetic anisotropy and slow relaxation of magnetization (Shukla et al., 2023 ). The combination of distinct metal centres in proximity creates unique electronic structures and enables fine-tuning of light absorption and emission properties (Bonfiglio et al., 2022 ). Selective assembly of several different metal ions into a well-defined structure is often synthetically challenging. Overcoming these challenges drives innovation in synthetic methodologies and coordination chemistry.

We have recently reported two novel heterometallic mixed-ligand mixed-anion complexes [CuCdClL(o-Van)(OAc)]·3H₂O and [Cu₂ZnCl₂L₂(o-Van)(OAc)] (GOQHIG and NOTGUB, respectively; Vassilyeva et al., 2025 ) synthesized by reacting a fine copper powder and Cd^II or Zn^II acetate with a methanol solution of the Schiff base ligand HL formed in situ from 2-hydroxy-3-methoxy-benzaldehyde (ortho-vanillin, o-VanH) and CH₃NH₂·HCl. The Cu/Cd complex demonstrated slow magnetic relaxation under an external magnetic field, a very rarely observable effect in the Cu^II coordination compounds.

To continue the series of heterometallics with the 2-methoxy-6-[(methylimino)methyl]phenol ligand, we report herein on the synthesis and crystal structure of [NiPbCl₂L(o-Van)(H₂O)₂], (I), prepared using a zerovalent nickel powder and PbCl₂ as starting materials. Similar to the Cu/Cd and Cu/Zn analogues, the reaction conditions did not favour complete amine-aldehyde condensation, yielding a combination of two kinds of aromatic ligands in complex (I). It is worth noting that the use of two salts in a parallel synthesis did not enable crystallization of a desired hetetometallic product. In the crystal, (I) exhibits full-molecule disorder [occupancy ratio 0.711 (6): 0.289 (6)], generated by a false twofold rotation about the shorter, Ni–Pb, axis of the molecule.

2. Structural commentary

Complex (I) crystallizes in the monoclinic space group P2₁/c; the neutral molecule contains two metal centres, the Schiff base and ortho-vanillin ligands, both deprotonated, as well as the chloride and aqua ligands. The molecule exhibits a whole-molecule orientational disorder [occupancy ratio 0.711 (6): 0.289 (6)] about a pseudo-twofold rotation axis that roughly bisects the molecule along the Ni–Pb axis (Figs. 1, 2). The major and minor components slightly differ in bond lengths and angles (Table 1).

Table 1
Selected geometric parameters (Å, °)

Pb1—Ni2	3.441 (3)	Pb1B—Ni2B	3.477 (7)
Pb1—Cl1	2.821 (5)	Pb1B—Cl1B	2.821 (13)
Pb1—Cl2	2.868 (5)	Pb1B—Cl2B	2.875 (12)
Pb1—O1	2.740 (10)	Pb1B—O1B	2.762 (19)
Pb1—O2	2.375 (9)	Pb1B—O2B	2.410 (18)
Pb1—O4	2.663 (9)	Pb1B—O4B	2.647 (19)
Pb1—O5	2.301 (8)	Pb1B—O5B	2.302 (18)
Ni2—O2	2.005 (7)	Ni2B—O2B	1.991 (15)
Ni2—O3	2.021 (7)	Ni2B—O3B	2.009 (15)
Ni2—O5	2.008 (7)	Ni2B—O5B	2.016 (16)
Ni2—O6	2.088 (6)	Ni2B—O6B	2.085 (13)
Ni2—O7	2.090 (5)	Ni2B—O7B	2.079 (11)
Ni2—N1	1.996 (8)	Ni2B—N1B	2.003 (14)

Cl1—Pb1—Cl2	166.0 (2)	Cl1B—Pb1B—Cl2B	164.7 (5)
O1—Pb1—Cl1	88.5 (4)	O1B—Pb1B—Cl1B	84.9 (11)
O1—Pb1—Cl2	96.9 (4)	O1B—Pb1B—Cl2B	94.7 (9)
O2—Pb1—Cl1	84.8 (4)	O2B—Pb1B—Cl1B	83.2 (9)
O2—Pb1—Cl2	86.7 (3)	O2B—Pb1B—Cl2B	83.5 (8)
O2—Pb1—O1	60.8 (3)	O2B—Pb1B—O1B	59.5 (5)
O2—Pb1—O4	132.5 (3)	O2B—Pb1B—O4B	132.0 (6)
O4—Pb1—Cl1	85.5 (4)	O4B—Pb1B—Cl1B	88.7 (11)
O4—Pb1—Cl2	92.2 (4)	O4B—Pb1B—Cl2B	94.8 (10)
O4—Pb1—O1	164.6 (3)	O4B—Pb1B—O1B	165.9 (7)
O5—Pb1—Cl1	84.2 (3)	O5B—Pb1B—Cl1B	84.5 (9)
O5—Pb1—Cl2	82.4 (3)	O5B—Pb1B—Cl2B	83.6 (8)
O5—Pb1—O1	129.4 (3)	O5B—Pb1B—O1B	126.7 (6)
O5—Pb1—O2	68.7 (2)	O5B—Pb1B—O2B	67.4 (4)
O5—Pb1—O4	64.1 (2)	O5B—Pb1B—O4B	64.8 (6)
O2—Ni2—O3	91.6 (3)	O2B—Ni2B—O3B	94.0 (7)
O2—Ni2—O5	82.3 (2)	O2B—Ni2B—O5B	81.5 (5)
O2—Ni2—O6	92.0 (5)	O2B—Ni2B—O6B	92.7 (13)
O2—Ni2—O7	83.3 (4)	O2B—Ni2B—O7B	83.5 (9)
O3—Ni2—O6	92.6 (6)	O2B—Ni2B—N1B	172.6 (8)
O3—Ni2—O7	87.8 (3)	O3B—Ni2B—O5B	175.3 (8)
O5—Ni2—O3	173.8 (3)	O3B—Ni2B—O6B	92.9 (14)
O5—Ni2—O6	86.7 (6)	O3B—Ni2B—O7B	88.1 (8)
O5—Ni2—O7	92.4 (4)	O5B—Ni2B—O6B	85.8 (14)
O6—Ni2—O7	175.4 (5)	O5B—Ni2B—O7B	92.9 (10)
N1—Ni2—O2	173.9 (4)	O7B—Ni2B—O6B	176.1 (10)
N1—Ni2—O3	94.3 (3)	N1B—Ni2B—O3B	92.8 (7)
N1—Ni2—O5	91.8 (4)	N1B—Ni2B—O5B	91.7 (7)
N1—Ni2—O6	89.1 (6)	N1B—Ni2B—O6B	89.7 (14)
N1—Ni2—O7	95.4 (3)	N1B—Ni2B—O7B	94.0 (9)

Figure 1
Molecular structure of the major component of the disordered complex [NiPbCl₂L(o-Van)(H₂O)₂], (I)

, with atom labelling and displacement ellipsoids drawn at the 50% probability level.

Figure 2
Disposition of the major and minor components of (I)

with the minor component shaded in pink.

The coordination around the Ni centre is distorted octahedral with the four Ni—N/O equatorial bond lengths for the major component falling in the range 1.996 (8)–2.021 (7) Å and the two axial distances to water molecules being slightly longer, 2.088 (6) and 2.090 (5) Å (Table 1). Cis bond angles at the metal atom of the major component vary from 82.3 (2) to 92.6 (6)° and the trans angles fall in the range 173.8 (3)–175.4 (5)° (Table 1). The Pb atom is six-coordinate in a highly distorted tetragonal–bipyramidal geometry, the four oxygen atoms from the two ligands are nearly coplanar with the metal centre [Pb—O = 2.301 (8)–2.740 (10) Å] while the two chlorides are located on opposite sides of the plane at Pb—Cl distances of 2.821 (5) and 2.868 (5) Å (major component, Table 1). The cis and trans bond angles at the metal atom vary in the ranges 60.8 (3)–129.4 (3) and 132.5 (3)–166.0 (2)°.

The Ni–Pb pair of metals is bridged by two phenolato oxygen atoms, O2/O2B and O5/O5B, from the two ligands enabling a metal–metal separation of 3.441 (3)/3.477 (7) Å. Most of the molecule, except for the coordinated Cl atoms and water molecules, is nearly planar with the Pb1 atom showing the largest deviation of 0.249 (1) Å from the mean plane defined by the 22 atoms of the major component. The structural configuration of (I) resembles that of GOQHIG, showing similar arrangement of the deprotonated Schiff base and ortho-vanillin ligands around the metal centres (Vassilyeva et al., 2025). The intramolecular O—H⋯Cl hydrogen bonds involving coordinated H₂O and chloride ligands appear to be a reason for non-linearity of the axial axes of the Ni and Pb polyhedra (Table 2).

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H2⋯Cl2	0.87	2.27	3.127 (7)	166
O6—H6⋯Cl2ⁱ	0.87	2.36	3.169 (17)	154
O7—H1⋯Cl1	0.88	2.31	3.152 (8)	162
O7—H7⋯Cl1ⁱⁱ	0.88	2.43	3.183 (10)	145
O6B—H6BB⋯Cl2Bⁱ	0.87	2.14	2.99 (4)	167
C14B—H14B⋯O6Bⁱⁱⁱ	0.95	2.50	3.26 (6)	138
C18B—H18D⋯O3B	0.98	2.27	2.96 (3)	127
Symmetry codes: (i) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) ; (iii) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

3. Supramolecular features

In the solid state, the heterometallic molecules pack loosely (Fig. 3) and the structure shows no significant intermolecular contacts; the minimal M⋯M distance is about 7.65 Å (Ni⋯Pb). The parallel o-vanillin rings of the adjacent molecules of (I) display π–π stacking with a ring centroid separation of 3.486 (2) Å (major component). In Fig. 3, it can be seen that for the major component the molecular packing features O—H⋯Cl and C—H⋯Cl/O hydrogen-bonding interactions (Table 2) that consolidate an extended supramolecular 3D network structure.

Figure 3
Fragment of the crystal packing of the major component of (I)

. Green and grey polyhedra denote Ni and Pb atoms, respectively, O atoms are red, N atoms are dark blue, H atoms are light blue, C atoms are grey. Hydrogen bonds are shown as blue dashed lines.

4. Database survey

A search in the Cambridge Structural Database for HL and its complexes (CSD; Groom et al., 2016 ) via the WebCSD interface in May 2025 revealed 54 original crystal structures, including the structure of the ligand itself. The majority of the homometallic compounds are polynuclear complexes with nuclearity ranging from 2 to 7. Four dimeric (Co, Ni, Cu, Mo), two tetrameric complexes with cubane- (Mn) or open-cubane type cores (Co), two hexametallic Dy compounds with the metal sites adopting a chair-like configuration, and 19 heptanuclear hexagonal disc-like clusters (Mn, Co, Ni, Zn) have been reported (Meally et al., 2012 ). The formation of polymetallic complexes with L⁻ of higher nuclearity is usually supported by the presence of other bridging ligands, such as OH⁻, MeO⁻, oxo, acetato or carbamato groups. Mononuclear complexes that possess molecular (Mn, Co, Mo, Cd and Pt) or polymeric structures (Mn, Co) show a higher metal-to-L⁻ ratio (1:2 and 1:3). The Schiff base is also able to act as a cation by protonation, counter-balanced by tetrachlorocobaltate(II) in [H₂L]₂CoCl₄ (KOZQOI; Vassilyeva et al., 2023 ).

The heterometallic 1s–3d examples comprise four structures of Na/M (M = Fe, Ni) complexes formed in the presence of sodium salts and/or NaOH in the reaction media (Meally et al., 2013 ). We have employed the neutral CoL₃ metalloligand to generate a series of heterometallic and mixed-valent [Co^IIIM^IIL₃Cl₂]·Solv (M = Mn, Co, Zn, Cd; Solv = H₂O, CH₃OH) complexes in the absence of other bridging ligands (Nesterova et al., 2018 ; Kokozay et al., 2022 ). In contrast, the neutral NiL₂ units required an additional bridging MeO⁻ group to construct the heterometallic dimer [NiZnL₂(OMe)Cl]₂ (ILIMOI; Vassilyeva et al., 2021 ). Similar to (I), the copper-based heterometallics [CuCdClL(o-Van)(OAc)]·3H₂O and [Cu₂ZnCl₂L₂(o-Van)(OAc)] (Vassilyeva et al., 2025) use the deprotonated o-vanillin molecule to support their integrity.

5. Synthesis and crystallization

o-Vanillin (0.23 g, 1.5 mmol), CH₃NH₂·HCl (0.10 g, 1.5 mmol) and 2-dimethylaminoethanol (0.1 ml, 0.1 mmol) were dissolved in 10 ml of ethanol in a 50 ml conical flask. PbCl₂ (0.14 g, 0.5 mmol) and Ni powder (0.03 g, 0.5 mmol) were added to the flask under continuous stirring at 333 K. The mixture was stirred magnetically for 2.5 h in the open air until the complete dissolution of the nickel powder and lead salt was observed. The brown solution was filtered and left to evaporate at room temperature. Green plate-like crystals of (I) suitable for X-ray crystallography precipitated the next day. They were filtered off, washed with PrⁱOH and dried in air. An additional amount of the product formed in the mother liquor over several days. Yield: 53%. Analysis calculated for C₁₇H₂₁Cl₂NNiO₇Pb (688.15): C 29.67, H 3.08, N 2.04%. Found: C 29.43, H 2.65, N 1.98%. IR (ν/cm⁻¹): 3340br, 3062, 2959, 2922, 2877, 2841, 2792, 1638s, 1605, 1553, 1472, 1455s, 1441s, 1416, 1311, 1290s, 1220s, 1210s, 1106, 1077, 1020, 953, 850, 790, 749, 730, 632, 584, 481, 436.

6. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3. The heterometallic molecule was modelled as being disordered over two sets of sites with site occupancies refined to 0.711 (6) and its complement. Rigid body restrains (RIGU) were applied to the minor component during refinement. The anisotropic displacement parameters for corresponding atoms in the major and minor components were constrained to be equal. Anisotropic displacement parameters were employed for the non-hydrogen atoms. The water hydrogen atoms were located from the experimental data and refined as rotating groups. Other hydrogen atoms were added at calculated positions and refined as riding with isotropic displacement parameters based on those of the parent atom [C—H = 0.95 Å, U_iso(H) = 1.2U_eqC for CH; C—H = 0.98 Å, U_iso(H) = 1.5U_eqC for CH₃]. The idealized methyl groups of the major component were refined as rotating groups.

Table 3
Experimental details

Crystal data
Chemical formula	[NiPb(C₉H₁₀NO₂)(C₈H₇NO₃)Cl₂(H₂O)₂]
M_r	688.15
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	150
a, b, c (Å)	14.2171 (6), 9.7678 (3), 16.1291 (6)
β (°)	108.006 (4)
V (Å³)	2130.15 (14)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	9.07
Crystal size (mm)	0.44 × 0.15 × 0.06

Data collection
Diffractometer	New Gemini, Dual, Cu at home/near, Atlas
Absorption correction	Analytical (CrysAlis PRO; Rigaku OD, 2023 $[Rigaku OD (2023). CrysAlis PRO. Rigaku Oxford Diffraction Ltd, Yarnton, England.]$ )
T_min, T_max	0.190, 0.603
No. of measured, independent and observed [I > 2σ(I)] reflections	13267, 4662, 3785
R_int	0.045
(sin θ/λ)_max (Å⁻¹)	0.681

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.082, 1.03
No. of reflections	4662
No. of parameters	437
No. of restraints	461
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.40, −1.55
Computer programs: CrysAlis PRO (Rigaku OD, 2023 $[Rigaku OD (2023). CrysAlis PRO. Rigaku Oxford Diffraction Ltd, Yarnton, England.]$ ), SHELXT2014/4 (Sheldrick, 2015a ), SHELXL2016/6 (Sheldrick, 2015b ), Mercury (Macrae et al., 2020 ) and OLEX2 (Dolomanov et al., 2009 ).

Supporting information

CCDC reference: 2467901

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2056989025005857/ny2013sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989025005857/ny2013Isup2.hkl

checkCIF report

Computing details top

Diaqua-1κ²O-dichlorido-2κ²Cl-(µ-2-formyl-6-methoxyphenolato-1κ²O¹,O²:2κO⁶)(µ-2-methoxy-6-[(methylimino)methyl]phenolato-1κ²N,O¹:2κO⁶)lead(II)nickel(II) top

Crystal data top

[NiPb(C₉H₁₀NO₂)(C₈H₇NO₃)Cl₂(H₂O)₂]	F(000) = 1320
M_r = 688.15	D_x = 2.146 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 14.2171 (6) Å	Cell parameters from 6907 reflections
b = 9.7678 (3) Å	θ = 3.1–28.4°
c = 16.1291 (6) Å	µ = 9.07 mm⁻¹
β = 108.006 (4)°	T = 150 K
V = 2130.15 (14) Å³	Plate, green
Z = 4	0.44 × 0.15 × 0.06 mm

Data collection top

New Gemini, Dual, Cu at home/near, Atlas diffractometer	3785 reflections with I > 2σ(I)
Detector resolution: 10.6426 pixels mm^-1	R_int = 0.045
ω scans	θ_max = 29.0°, θ_min = 2.5°
Absorption correction: analytical (CrysAlisPro; Rigaku OD, 2023)	h = −18→17
T_min = 0.190, T_max = 0.603	k = −11→12
13267 measured reflections	l = −21→19
4662 independent reflections

Refinement top

Refinement on F²	461 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.036	H-atom parameters constrained
wR(F²) = 0.082	w = 1/[σ²(F_o²) + (0.0386P)² + 2.0045P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.001
4662 reflections	Δρ_max = 1.40 e Å⁻³
437 parameters	Δρ_min = −1.55 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.71331 (18)	0.6780 (2)	0.32661 (18)	0.0192 (2)	0.711 (6)
Ni2	0.75011 (17)	0.3361 (2)	0.37762 (17)	0.0181 (4)	0.711 (6)
Cl1	0.9003 (6)	0.7086 (7)	0.4530 (9)	0.0322 (16)	0.711 (6)
Cl2	0.5382 (4)	0.5785 (8)	0.1987 (5)	0.0273 (12)	0.711 (6)
O1	0.6280 (12)	0.7362 (11)	0.4534 (9)	0.034 (3)	0.711 (6)
O2	0.6904 (9)	0.4990 (8)	0.4181 (6)	0.0210 (13)	0.711 (6)
O3	0.7134 (6)	0.2123 (7)	0.4632 (5)	0.028 (2)	0.711 (6)
O4	0.8114 (10)	0.6915 (7)	0.2104 (9)	0.0322 (16)	0.711 (6)
O5	0.7776 (9)	0.4748 (8)	0.2961 (7)	0.0253 (13)	0.711 (6)
O6	0.6187 (10)	0.2941 (8)	0.2788 (12)	0.0292 (18)	0.711 (6)
H2	0.587543	0.370418	0.260097	0.044*	0.711 (6)
H6	0.579202	0.249284	0.301012	0.044*	0.711 (6)
O7	0.8760 (4)	0.3922 (6)	0.4790 (4)	0.0284 (15)	0.711 (6)
H1	0.895129	0.474209	0.469416	0.043*	0.711 (6)
H7	0.925460	0.339213	0.478427	0.043*	0.711 (6)
N1	0.8164 (7)	0.1881 (8)	0.3310 (6)	0.026 (2)	0.711 (6)
C1	0.6042 (15)	0.8686 (12)	0.4776 (13)	0.055 (5)	0.711 (6)
H1A	0.533645	0.872297	0.472176	0.083*	0.711 (6)
H1B	0.619084	0.937315	0.439202	0.083*	0.711 (6)
H1C	0.643401	0.887320	0.538090	0.083*	0.711 (6)
C2	0.6248 (16)	0.6294 (9)	0.5103 (10)	0.027 (2)	0.711 (6)
C3	0.6581 (16)	0.5046 (13)	0.4869 (11)	0.023 (3)	0.711 (6)
C4	0.6574 (10)	0.3902 (10)	0.5398 (7)	0.0229 (19)	0.711 (6)
C5	0.6239 (10)	0.4051 (14)	0.6130 (7)	0.033 (3)	0.711 (6)
H5	0.624201	0.327941	0.648941	0.040*	0.711 (6)
C6	0.5913 (11)	0.5275 (13)	0.6333 (8)	0.040 (3)	0.711 (6)
H6A	0.569212	0.535901	0.682916	0.048*	0.711 (6)
C7	0.5906 (15)	0.6420 (13)	0.5799 (10)	0.035 (3)	0.711 (6)
H7A	0.566384	0.727548	0.592567	0.042*	0.711 (6)
C8	0.6845 (10)	0.2540 (11)	0.5231 (7)	0.030 (3)	0.711 (6)
H8	0.679333	0.186511	0.563935	0.036*	0.711 (6)
C10	0.8366 (11)	0.8138 (9)	0.1702 (7)	0.032 (2)	0.711 (6)
H10A	0.908445	0.827325	0.190738	0.048*	0.711 (6)
H10B	0.803940	0.893497	0.186018	0.048*	0.711 (6)
H10C	0.814463	0.803010	0.106642	0.048*	0.711 (6)
C11	0.8501 (13)	0.5696 (10)	0.1957 (11)	0.0256 (19)	0.711 (6)
C12	0.8302 (15)	0.4586 (11)	0.2421 (11)	0.022 (3)	0.711 (6)
C13	0.8688 (9)	0.3288 (10)	0.2283 (7)	0.025 (2)	0.711 (6)
C14	0.9206 (9)	0.3185 (11)	0.1681 (8)	0.032 (3)	0.711 (6)
H14	0.944187	0.231385	0.157457	0.039*	0.711 (6)
C15	0.9384 (10)	0.4283 (13)	0.1242 (9)	0.037 (3)	0.711 (6)
H15	0.975374	0.417545	0.084642	0.044*	0.711 (6)
C16	0.9029 (15)	0.5565 (12)	0.1365 (11)	0.038 (3)	0.711 (6)
H16	0.914497	0.633701	0.105225	0.045*	0.711 (6)
C17	0.8558 (9)	0.2032 (11)	0.2714 (7)	0.028 (3)	0.711 (6)
H17	0.879937	0.122232	0.252393	0.034*	0.711 (6)
C18	0.8092 (9)	0.0480 (8)	0.3637 (7)	0.051 (3)	0.711 (6)
H18A	0.739425	0.023298	0.351565	0.077*	0.711 (6)
H18B	0.842460	0.044881	0.426688	0.077*	0.711 (6)
H18C	0.840936	−0.016942	0.334396	0.077*	0.711 (6)
Pb1B	0.7023 (5)	0.6866 (6)	0.3317 (4)	0.0192 (2)	0.289 (6)
Ni2B	0.7554 (5)	0.3385 (6)	0.3531 (4)	0.0181 (4)	0.289 (6)
Cl1B	0.8901 (18)	0.7087 (17)	0.458 (2)	0.0322 (16)	0.289 (6)
Cl2B	0.5250 (12)	0.588 (2)	0.2051 (14)	0.0273 (12)	0.289 (6)
O1B	0.804 (3)	0.724 (2)	0.212 (2)	0.0322 (16)	0.289 (6)
O2B	0.777 (2)	0.4950 (18)	0.2822 (17)	0.0253 (13)	0.289 (6)
O3B	0.8189 (18)	0.2010 (18)	0.2947 (14)	0.032 (5)	0.289 (6)
O4B	0.621 (3)	0.711 (2)	0.458 (2)	0.033 (5)	0.289 (6)
O5B	0.690 (2)	0.4866 (18)	0.4033 (16)	0.0210 (13)	0.289 (6)
O6B	0.614 (2)	0.3004 (19)	0.268 (3)	0.0292 (18)	0.289 (6)
H6BA	0.600144	0.312202	0.211792	0.044*	0.289 (6)
H6BB	0.579774	0.229360	0.273079	0.044*	0.289 (6)
O7B	0.8960 (9)	0.3888 (13)	0.4338 (10)	0.0284 (15)	0.289 (6)
H7BA	0.944470	0.347727	0.416687	0.043*	0.289 (6)
H7BB	0.906628	0.353907	0.488206	0.043*	0.289 (6)
N1B	0.732 (2)	0.1992 (16)	0.4358 (15)	0.026 (4)	0.289 (6)
C1B	0.835 (3)	0.854 (2)	0.193 (2)	0.032 (2)	0.289 (6)
H1BA	0.798451	0.925365	0.213586	0.048*	0.289 (6)
H1BB	0.905674	0.864531	0.222595	0.048*	0.289 (6)
H1BC	0.821185	0.862747	0.130096	0.048*	0.289 (6)
C2B	0.847 (4)	0.609 (2)	0.188 (3)	0.0256 (19)	0.289 (6)
C3B	0.829 (3)	0.488 (2)	0.226 (3)	0.018 (5)	0.289 (6)
C4B	0.869 (3)	0.365 (2)	0.206 (2)	0.025 (2)	0.289 (6)
C5B	0.931 (3)	0.367 (3)	0.152 (3)	0.042 (9)	0.289 (6)
H5B	0.965558	0.286775	0.144337	0.050*	0.289 (6)
C6B	0.940 (4)	0.485 (3)	0.112 (3)	0.043 (7)	0.289 (6)
H6B	0.971557	0.485048	0.067657	0.052*	0.289 (6)
C7B	0.903 (3)	0.609 (3)	0.134 (3)	0.031 (6)	0.289 (6)
H7B	0.917774	0.692505	0.111268	0.038*	0.289 (6)
C8B	0.857 (2)	0.231 (3)	0.2385 (18)	0.027 (6)	0.289 (6)
H8B	0.881052	0.156929	0.213134	0.033*	0.289 (6)
C10B	0.576 (4)	0.833 (3)	0.484 (4)	0.055 (5)	0.289 (6)
H10D	0.578590	0.909605	0.445666	0.083*	0.289 (6)
H10E	0.506607	0.812876	0.478702	0.083*	0.289 (6)
H10F	0.611659	0.856925	0.544445	0.083*	0.289 (6)
C11B	0.625 (4)	0.594 (3)	0.504 (3)	0.027 (2)	0.289 (6)
C12B	0.668 (5)	0.482 (3)	0.477 (3)	0.026 (7)	0.289 (6)
C13B	0.675 (3)	0.358 (2)	0.5260 (19)	0.0229 (19)	0.289 (6)
C14B	0.641 (3)	0.358 (3)	0.598 (2)	0.029 (6)	0.289 (6)
H14B	0.644962	0.275687	0.630598	0.035*	0.289 (6)
C15B	0.603 (3)	0.471 (3)	0.6244 (19)	0.031 (7)	0.289 (6)
H15B	0.582672	0.467078	0.674989	0.037*	0.289 (6)
C16B	0.594 (4)	0.592 (2)	0.579 (2)	0.031 (6)	0.289 (6)
H16B	0.568552	0.671354	0.597384	0.038*	0.289 (6)
C17B	0.708 (3)	0.229 (2)	0.5026 (19)	0.021 (6)	0.289 (6)
H17B	0.711178	0.155661	0.542537	0.025*	0.289 (6)
C18B	0.760 (2)	0.0553 (17)	0.4322 (16)	0.051 (3)	0.289 (6)
H18D	0.778343	0.039607	0.379049	0.077*	0.289 (6)
H18E	0.816853	0.034000	0.483302	0.077*	0.289 (6)
H18F	0.704401	−0.003753	0.431792	0.077*	0.289 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.0219 (6)	0.0110 (3)	0.0250 (3)	0.0038 (3)	0.0079 (3)	0.0001 (2)
Ni2	0.0202 (5)	0.0119 (3)	0.0219 (12)	−0.0008 (3)	0.0059 (8)	0.0037 (7)
Cl1	0.025 (2)	0.0201 (7)	0.0484 (18)	−0.0036 (9)	0.0074 (19)	−0.0006 (7)
Cl2	0.0245 (18)	0.0245 (13)	0.0312 (14)	0.0086 (13)	0.0061 (15)	0.0001 (10)
O1	0.044 (6)	0.024 (5)	0.033 (5)	0.008 (5)	0.008 (4)	0.004 (4)
O2	0.029 (2)	0.015 (2)	0.018 (4)	−0.0023 (19)	0.004 (3)	−0.003 (2)
O3	0.038 (5)	0.019 (3)	0.024 (7)	−0.008 (3)	0.004 (5)	0.004 (3)
O4	0.034 (3)	0.020 (4)	0.042 (3)	0.004 (4)	0.011 (2)	0.010 (4)
O5	0.030 (2)	0.009 (3)	0.042 (4)	0.000 (2)	0.019 (3)	0.005 (2)
O6	0.026 (2)	0.020 (2)	0.037 (5)	−0.0025 (18)	0.002 (2)	−0.002 (2)
O7	0.024 (3)	0.022 (2)	0.037 (4)	−0.003 (2)	0.006 (3)	0.004 (3)
N1	0.020 (4)	0.016 (4)	0.037 (6)	0.000 (3)	0.003 (4)	−0.002 (4)
C1	0.086 (14)	0.032 (7)	0.046 (5)	0.019 (8)	0.020 (7)	−0.006 (6)
C2	0.031 (3)	0.025 (5)	0.020 (4)	−0.002 (7)	−0.001 (3)	−0.010 (5)
C3	0.016 (7)	0.034 (7)	0.015 (6)	−0.010 (6)	−0.001 (5)	−0.001 (5)
C4	0.021 (6)	0.027 (5)	0.021 (5)	−0.001 (4)	0.007 (3)	0.000 (4)
C5	0.040 (11)	0.044 (10)	0.018 (6)	−0.008 (9)	0.010 (5)	−0.003 (7)
C6	0.032 (6)	0.068 (10)	0.025 (5)	−0.008 (7)	0.015 (4)	−0.020 (6)
C7	0.025 (6)	0.050 (8)	0.029 (5)	−0.002 (8)	0.005 (4)	−0.011 (6)
C8	0.028 (7)	0.036 (6)	0.024 (6)	−0.009 (5)	0.006 (5)	0.007 (5)
C10	0.031 (4)	0.024 (5)	0.039 (7)	−0.004 (5)	0.009 (5)	0.001 (4)
C11	0.023 (3)	0.023 (5)	0.027 (5)	0.003 (6)	0.002 (3)	0.007 (6)
C12	0.023 (6)	0.019 (5)	0.024 (7)	−0.006 (5)	0.004 (6)	0.004 (4)
C13	0.019 (3)	0.023 (5)	0.027 (7)	0.000 (5)	0.000 (4)	0.000 (4)
C14	0.017 (5)	0.036 (6)	0.041 (7)	0.000 (5)	0.005 (4)	−0.009 (5)
C15	0.037 (7)	0.047 (10)	0.028 (8)	0.008 (9)	0.012 (5)	0.001 (8)
C16	0.049 (7)	0.033 (8)	0.029 (6)	0.001 (8)	0.009 (5)	0.007 (7)
C17	0.025 (6)	0.024 (6)	0.027 (8)	0.015 (5)	−0.004 (5)	−0.007 (5)
C18	0.074 (7)	0.014 (4)	0.068 (6)	0.005 (4)	0.027 (5)	−0.001 (4)
Pb1B	0.0219 (6)	0.0110 (3)	0.0250 (3)	0.0038 (3)	0.0079 (3)	0.0001 (2)
Ni2B	0.0202 (5)	0.0119 (3)	0.0219 (12)	−0.0008 (3)	0.0059 (8)	0.0037 (7)
Cl1B	0.025 (2)	0.0201 (7)	0.0484 (18)	−0.0036 (9)	0.0074 (19)	−0.0006 (7)
Cl2B	0.0245 (18)	0.0245 (13)	0.0312 (14)	0.0086 (13)	0.0061 (15)	0.0001 (10)
O1B	0.034 (3)	0.020 (4)	0.042 (3)	0.004 (4)	0.011 (2)	0.010 (4)
O2B	0.030 (2)	0.009 (3)	0.042 (4)	0.000 (2)	0.019 (3)	0.005 (2)
O3B	0.045 (12)	0.013 (7)	0.047 (12)	0.010 (7)	0.027 (10)	0.005 (7)
O4B	0.044 (14)	0.019 (7)	0.041 (12)	−0.002 (8)	0.019 (10)	−0.012 (6)
O5B	0.029 (2)	0.015 (2)	0.018 (4)	−0.0023 (19)	0.004 (3)	−0.003 (2)
O6B	0.026 (2)	0.020 (2)	0.037 (5)	−0.0025 (18)	0.002 (2)	−0.002 (2)
O7B	0.024 (3)	0.022 (2)	0.037 (4)	−0.003 (2)	0.006 (3)	0.004 (3)
N1B	0.051 (14)	0.012 (6)	0.016 (9)	−0.009 (6)	0.010 (7)	−0.003 (6)
C1B	0.031 (4)	0.024 (5)	0.039 (7)	−0.004 (5)	0.009 (5)	0.001 (4)
C2B	0.023 (3)	0.023 (5)	0.027 (5)	0.003 (6)	0.002 (3)	0.007 (6)
C3B	0.013 (11)	0.022 (7)	0.014 (12)	0.007 (10)	−0.006 (8)	0.007 (8)
C4B	0.019 (3)	0.023 (5)	0.027 (7)	0.000 (5)	0.000 (4)	0.000 (4)
C5B	0.052 (18)	0.032 (15)	0.05 (2)	0.000 (15)	0.028 (15)	0.003 (13)
C6B	0.058 (19)	0.038 (15)	0.036 (17)	−0.009 (14)	0.017 (13)	0.000 (13)
C7B	0.026 (12)	0.033 (14)	0.033 (12)	−0.013 (14)	0.006 (9)	0.002 (13)
C8B	0.022 (12)	0.024 (8)	0.038 (15)	0.007 (9)	0.012 (12)	0.004 (9)
C10B	0.086 (14)	0.032 (7)	0.046 (5)	0.019 (8)	0.020 (7)	−0.006 (6)
C11B	0.031 (3)	0.025 (5)	0.020 (4)	−0.002 (7)	−0.001 (3)	−0.010 (5)
C12B	0.04 (2)	0.017 (7)	0.018 (10)	−0.004 (9)	0.008 (11)	−0.007 (7)
C13B	0.021 (6)	0.027 (5)	0.021 (5)	−0.001 (4)	0.007 (3)	0.000 (4)
C14B	0.025 (14)	0.036 (13)	0.030 (11)	−0.003 (13)	0.015 (9)	−0.007 (11)
C15B	0.037 (18)	0.029 (14)	0.033 (14)	−0.008 (14)	0.019 (11)	−0.011 (12)
C16B	0.037 (16)	0.029 (13)	0.026 (10)	−0.007 (14)	0.007 (9)	−0.014 (11)
C17B	0.032 (16)	0.017 (8)	0.014 (13)	−0.003 (9)	0.006 (12)	0.006 (8)
C18B	0.074 (7)	0.014 (4)	0.068 (6)	0.005 (4)	0.027 (5)	−0.001 (4)

Geometric parameters (Å, º) top

Pb1—Ni2	3.441 (3)	Pb1B—Cl1B	2.821 (13)
Pb1—Cl1	2.821 (5)	Pb1B—Cl2B	2.875 (12)
Pb1—Cl2	2.868 (5)	Pb1B—O1B	2.762 (19)
Pb1—O1	2.740 (10)	Pb1B—O2B	2.410 (18)
Pb1—O2	2.375 (9)	Pb1B—O4B	2.647 (19)
Pb1—O4	2.663 (9)	Pb1B—O5B	2.302 (18)
Pb1—O5	2.301 (8)	Ni2B—O2B	1.991 (15)
Ni2—O2	2.005 (7)	Ni2B—O3B	2.009 (15)
Ni2—O3	2.021 (7)	Ni2B—O5B	2.016 (16)
Ni2—O5	2.008 (7)	Ni2B—O6B	2.085 (13)
Ni2—O6	2.088 (6)	Ni2B—O7B	2.079 (11)
Ni2—O7	2.090 (5)	Ni2B—N1B	2.003 (14)
Ni2—N1	1.996 (8)	Cl1B—O7B	3.152 (15)
Cl1—O7	3.152 (8)	Cl1B—O7Bⁱ	3.15 (2)
Cl2—O6	3.127 (7)	Cl2B—O6B	3.123 (15)
O1—C1	1.422 (14)	Cl2B—O6Bⁱⁱ	2.99 (4)
O1—C2	1.399 (13)	O1B—C1B	1.41 (2)
O2—C3	1.327 (12)	O1B—C2B	1.39 (2)
O3—C8	1.231 (12)	O2B—C3B	1.33 (2)
O4—C10	1.457 (12)	O3B—C8B	1.224 (19)
O4—C11	1.363 (11)	O4B—C10B	1.47 (2)
O5—C12	1.323 (12)	O4B—C11B	1.36 (2)
O6—H2	0.8719	O5B—C12B	1.32 (2)
O6—H6	0.8718	O6B—H6BA	0.8700
O7—H1	0.8752	O6B—H6BB	0.8700
O7—H7	0.8751	O7B—H7BA	0.9111
N1—C17	1.262 (14)	O7B—H7BB	0.9090
N1—C18	1.481 (11)	N1B—C17B	1.26 (2)
C1—H1A	0.9800	N1B—C18B	1.468 (18)
C1—H1B	0.9800	C1B—H1BA	0.9800
C1—H1C	0.9800	C1B—H1BB	0.9800
C2—C3	1.401 (14)	C1B—H1BC	0.9800
C2—C7	1.361 (15)	C2B—C3B	1.39 (2)
C3—C4	1.407 (13)	C2B—C7B	1.35 (2)
C4—C5	1.410 (13)	C3B—C4B	1.41 (2)
C4—C8	1.434 (13)	C4B—C5B	1.42 (2)
C5—H5	0.9500	C4B—C8B	1.438 (19)
C5—C6	1.358 (15)	C5B—H5B	0.9500
C6—H6A	0.9500	C5B—C6B	1.35 (2)
C6—C7	1.408 (16)	C6B—H6B	0.9500
C7—H7A	0.9500	C6B—C7B	1.41 (2)
C8—H8	0.9500	C7B—H7B	0.9500
C10—H10A	0.9800	C8B—H8B	0.9500
C10—H10B	0.9800	C10B—H10D	0.9800
C10—H10C	0.9800	C10B—H10E	0.9800
C11—C12	1.395 (12)	C10B—H10F	0.9800
C11—C16	1.390 (15)	C11B—C12B	1.39 (2)
C12—C13	1.425 (13)	C11B—C16B	1.39 (2)
C13—C14	1.392 (14)	C12B—C13B	1.43 (2)
C13—C17	1.450 (14)	C13B—C14B	1.39 (2)
C14—H14	0.9500	C13B—C17B	1.44 (2)
C14—C15	1.350 (15)	C14B—H14B	0.9500
C15—H15	0.9500	C14B—C15B	1.35 (2)
C15—C16	1.387 (15)	C15B—H15B	0.9500
C16—H16	0.9500	C15B—C16B	1.37 (2)
C17—H17	0.9500	C16B—H16B	0.9500
C18—H18A	0.9800	C17B—H17B	0.9500
C18—H18B	0.9800	C18B—H18D	0.9800
C18—H18C	0.9800	C18B—H18E	0.9800
Pb1B—Ni2B	3.477 (7)	C18B—H18F	0.9800

Cl1—Pb1—Ni2	83.70 (15)	O1B—Pb1B—Cl2B	94.7 (9)
Cl1—Pb1—Cl2	166.0 (2)	O2B—Pb1B—Ni2B	33.8 (4)
Cl2—Pb1—Ni2	82.93 (15)	O2B—Pb1B—Cl1B	83.2 (9)
O1—Pb1—Ni2	95.3 (2)	O2B—Pb1B—Cl2B	83.5 (8)
O1—Pb1—Cl1	88.5 (4)	O2B—Pb1B—O1B	59.5 (5)
O1—Pb1—Cl2	96.9 (4)	O2B—Pb1B—O4B	132.0 (6)
O2—Pb1—Ni2	34.57 (18)	O4B—Pb1B—Ni2B	98.4 (5)
O2—Pb1—Cl1	84.8 (4)	O4B—Pb1B—Cl1B	88.7 (11)
O2—Pb1—Cl2	86.7 (3)	O4B—Pb1B—Cl2B	94.8 (10)
O2—Pb1—O1	60.8 (3)	O4B—Pb1B—O1B	165.9 (7)
O2—Pb1—O4	132.5 (3)	O5B—Pb1B—Ni2B	33.7 (4)
O4—Pb1—Ni2	98.17 (16)	O5B—Pb1B—Cl1B	84.5 (9)
O4—Pb1—Cl1	85.5 (4)	O5B—Pb1B—Cl2B	83.6 (8)
O4—Pb1—Cl2	92.2 (4)	O5B—Pb1B—O1B	126.7 (6)
O4—Pb1—O1	164.6 (3)	O5B—Pb1B—O2B	67.4 (4)
O5—Pb1—Ni2	34.18 (18)	O5B—Pb1B—O4B	64.8 (6)
O5—Pb1—Cl1	84.2 (3)	O2B—Ni2B—Pb1B	42.3 (5)
O5—Pb1—Cl2	82.4 (3)	O2B—Ni2B—O3B	94.0 (7)
O5—Pb1—O1	129.4 (3)	O2B—Ni2B—O5B	81.5 (5)
O5—Pb1—O2	68.7 (2)	O2B—Ni2B—O6B	92.7 (13)
O5—Pb1—O4	64.1 (2)	O2B—Ni2B—O7B	83.5 (9)
O2—Ni2—Pb1	42.2 (3)	O2B—Ni2B—N1B	172.6 (8)
O2—Ni2—O3	91.6 (3)	O3B—Ni2B—Pb1B	136.3 (5)
O2—Ni2—O5	82.3 (2)	O3B—Ni2B—O5B	175.3 (8)
O2—Ni2—O6	92.0 (5)	O3B—Ni2B—O6B	92.9 (14)
O2—Ni2—O7	83.3 (4)	O3B—Ni2B—O7B	88.1 (8)
O3—Ni2—Pb1	133.8 (2)	O5B—Ni2B—Pb1B	39.3 (5)
O3—Ni2—O6	92.6 (6)	O5B—Ni2B—O6B	85.8 (14)
O3—Ni2—O7	87.8 (3)	O5B—Ni2B—O7B	92.9 (10)
O5—Ni2—Pb1	40.1 (3)	O6B—Ni2B—Pb1B	88.5 (6)
O5—Ni2—O3	173.8 (3)	O7B—Ni2B—Pb1B	88.2 (4)
O5—Ni2—O6	86.7 (6)	O7B—Ni2B—O6B	176.1 (10)
O5—Ni2—O7	92.4 (4)	N1B—Ni2B—Pb1B	130.9 (5)
O6—Ni2—Pb1	88.5 (2)	N1B—Ni2B—O3B	92.8 (7)
O6—Ni2—O7	175.4 (5)	N1B—Ni2B—O5B	91.7 (7)
O7—Ni2—Pb1	87.88 (16)	N1B—Ni2B—O6B	89.7 (14)
N1—Ni2—Pb1	131.9 (3)	N1B—Ni2B—O7B	94.0 (9)
N1—Ni2—O2	173.9 (4)	Pb1B—Cl1B—O7B	83.7 (4)
N1—Ni2—O3	94.3 (3)	Pb1B—Cl1B—O7Bⁱ	156.0 (10)
N1—Ni2—O5	91.8 (4)	O7Bⁱ—Cl1B—O7B	73.2 (6)
N1—Ni2—O6	89.1 (6)	Pb1B—Cl2B—O6B	83.7 (4)
N1—Ni2—O7	95.4 (3)	O6Bⁱⁱ—Cl2B—O6B	143.0 (9)
Pb1—Cl1—O7	82.82 (18)	C1B—O1B—Pb1B	122.7 (17)
Pb1—Cl2—O6	83.03 (18)	C2B—O1B—Pb1B	117.1 (13)
C1—O1—Pb1	126.3 (8)	C2B—O1B—C1B	118 (2)
C2—O1—Pb1	116.5 (7)	Ni2B—O2B—Pb1B	103.9 (8)
C2—O1—C1	116.0 (10)	C3B—O2B—Pb1B	131.4 (13)
Ni2—O2—Pb1	103.2 (3)	C3B—O2B—Ni2B	124.5 (14)
C3—O2—Pb1	129.7 (7)	C8B—O3B—Ni2B	123.3 (16)
C3—O2—Ni2	126.6 (7)	C10B—O4B—Pb1B	128.6 (18)
C8—O3—Ni2	123.9 (6)	C11B—O4B—Pb1B	113.2 (13)
C10—O4—Pb1	127.5 (6)	C11B—O4B—C10B	118 (2)
C11—O4—Pb1	114.0 (6)	Ni2B—O5B—Pb1B	107.1 (8)
C11—O4—C10	118.1 (9)	C12B—O5B—Pb1B	123.8 (15)
Ni2—O5—Pb1	105.8 (4)	C12B—O5B—Ni2B	127.1 (15)
C12—O5—Pb1	126.0 (6)	Ni2B—O6B—Cl2B	105.4 (6)
C12—O5—Ni2	127.9 (6)	Ni2B—O6B—H6BA	122.0
Ni2—O6—Cl2	105.5 (3)	Ni2B—O6B—H6BB	122.4
Ni2—O6—H2	109.6	Cl2Bⁱⁱⁱ—O6B—Cl2B	116.7 (12)
Ni2—O6—H6	108.8	Cl2B—O6B—H6BA	66.6
Cl2—O6—H2	10.2	Cl2Bⁱⁱⁱ—O6B—H6BA	106.9
Cl2—O6—H6	114.6	Cl2B—O6B—H6BB	124.3
H2—O6—H6	104.4	Cl2Bⁱⁱⁱ—O6B—H6BB	9.1
Ni2—O7—Cl1	104.8 (2)	H6BA—O6B—H6BB	104.5
Ni2—O7—H1	109.8	Ni2B—O7B—Cl1B	104.7 (5)
Ni2—O7—H7	109.5	Ni2B—O7B—H7BA	112.1
Cl1—O7—H1	13.1	Ni2B—O7B—H7BB	110.9
Cl1—O7—H7	117.2	Cl1Bⁱ—O7B—Cl1B	106.8 (6)
H1—O7—H7	104.2	Cl1Bⁱ—O7B—H7BA	49.0
C17—N1—Ni2	125.1 (7)	Cl1B—O7B—H7BA	121.7
C17—N1—C18	118.4 (9)	Cl1B—O7B—H7BB	104.8
C18—N1—Ni2	116.3 (7)	Cl1Bⁱ—O7B—H7BB	60.5
O1—C1—H1A	109.5	H7BA—O7B—H7BB	102.2
O1—C1—H1B	109.5	C17B—N1B—Ni2B	124.1 (16)
O1—C1—H1C	109.5	C17B—N1B—C18B	113.7 (18)
H1A—C1—H1B	109.5	C18B—N1B—Ni2B	121.4 (13)
H1A—C1—H1C	109.5	O1B—C1B—H1BA	109.5
H1B—C1—H1C	109.5	O1B—C1B—H1BB	109.5
O1—C2—C3	113.0 (10)	O1B—C1B—H1BC	109.5
C7—C2—O1	124.5 (10)	H1BA—C1B—H1BB	109.5
C7—C2—C3	122.4 (10)	H1BA—C1B—H1BC	109.5
O2—C3—C2	119.6 (10)	H1BB—C1B—H1BC	109.5
O2—C3—C4	122.9 (10)	O1B—C2B—C3B	114.4 (18)
C2—C3—C4	117.5 (9)	C7B—C2B—O1B	125.7 (18)
C3—C4—C5	119.5 (9)	C7B—C2B—C3B	119.9 (18)
C3—C4—C8	124.8 (9)	O2B—C3B—C2B	117.5 (18)
C5—C4—C8	115.6 (9)	O2B—C3B—C4B	123.5 (18)
C4—C5—H5	119.3	C2B—C3B—C4B	118.9 (17)
C6—C5—C4	121.4 (9)	C3B—C4B—C5B	120.4 (17)
C6—C5—H5	119.3	C3B—C4B—C8B	125.7 (18)
C5—C6—H6A	120.3	C5B—C4B—C8B	113.9 (18)
C5—C6—C7	119.4 (10)	C4B—C5B—H5B	120.8
C7—C6—H6A	120.3	C6B—C5B—C4B	118 (2)
C2—C7—C6	119.7 (11)	C6B—C5B—H5B	120.8
C2—C7—H7A	120.1	C5B—C6B—H6B	119.7
C6—C7—H7A	120.1	C5B—C6B—C7B	121 (2)
O3—C8—C4	129.0 (9)	C7B—C6B—H6B	119.7
O3—C8—H8	115.5	C2B—C7B—C6B	121 (2)
C4—C8—H8	115.5	C2B—C7B—H7B	119.5
O4—C10—H10A	109.5	C6B—C7B—H7B	119.5
O4—C10—H10B	109.5	O3B—C8B—C4B	128 (2)
O4—C10—H10C	109.5	O3B—C8B—H8B	115.8
H10A—C10—H10B	109.5	C4B—C8B—H8B	115.8
H10A—C10—H10C	109.5	O4B—C10B—H10D	109.5
H10B—C10—H10C	109.5	O4B—C10B—H10E	109.5
O4—C11—C12	115.2 (10)	O4B—C10B—H10F	109.5
O4—C11—C16	122.2 (9)	H10D—C10B—H10E	109.5
C16—C11—C12	122.6 (9)	H10D—C10B—H10F	109.5
O5—C12—C11	120.7 (9)	H10E—C10B—H10F	109.5
O5—C12—C13	122.2 (8)	O4B—C11B—C12B	115.8 (19)
C11—C12—C13	117.1 (9)	O4B—C11B—C16B	120.9 (18)
C12—C13—C17	124.4 (9)	C12B—C11B—C16B	123.0 (19)
C14—C13—C12	119.0 (8)	O5B—C12B—C11B	121 (2)
C14—C13—C17	116.6 (9)	O5B—C12B—C13B	122.2 (18)
C13—C14—H14	118.9	C11B—C12B—C13B	116.7 (17)
C15—C14—C13	122.3 (9)	C12B—C13B—C17B	124.8 (18)
C15—C14—H14	118.9	C14B—C13B—C12B	119.0 (17)
C14—C15—H15	119.8	C14B—C13B—C17B	116.1 (18)
C14—C15—C16	120.4 (10)	C13B—C14B—H14B	119.0
C16—C15—H15	119.8	C15B—C14B—C13B	122 (2)
C11—C16—H16	120.7	C15B—C14B—H14B	119.0
C15—C16—C11	118.6 (10)	C14B—C15B—H15B	119.5
C15—C16—H16	120.7	C14B—C15B—C16B	121 (2)
N1—C17—C13	128.1 (9)	C16B—C15B—H15B	119.5
N1—C17—H17	116.0	C11B—C16B—H16B	120.9
C13—C17—H17	116.0	C15B—C16B—C11B	118 (2)
N1—C18—H18A	109.5	C15B—C16B—H16B	120.9
N1—C18—H18B	109.5	N1B—C17B—C13B	128 (2)
N1—C18—H18C	109.5	N1B—C17B—H17B	115.9
H18A—C18—H18B	109.5	C13B—C17B—H17B	115.9
H18A—C18—H18C	109.5	N1B—C18B—H18D	109.5
H18B—C18—H18C	109.5	N1B—C18B—H18E	109.5
Cl1B—Pb1B—Ni2B	82.8 (4)	N1B—C18B—H18F	109.5
Cl1B—Pb1B—Cl2B	164.7 (5)	H18D—C18B—H18E	109.5
Cl2B—Pb1B—Ni2B	81.9 (4)	H18D—C18B—H18F	109.5
O1B—Pb1B—Ni2B	93.2 (4)	H18E—C18B—H18F	109.5
O1B—Pb1B—Cl1B	84.9 (11)

Pb1—O1—C2—C3	−6 (2)	Pb1B—O1B—C2B—C3B	2 (6)
Pb1—O1—C2—C7	176.0 (17)	Pb1B—O1B—C2B—C7B	−177 (4)
Pb1—O2—C3—C2	5 (3)	Pb1B—O2B—C3B—C2B	1 (6)
Pb1—O2—C3—C4	−173.7 (13)	Pb1B—O2B—C3B—C4B	179 (3)
Pb1—O4—C11—C12	1 (2)	Pb1B—O4B—C11B—C12B	−1 (7)
Pb1—O4—C11—C16	179.4 (15)	Pb1B—O4B—C11B—C16B	173 (4)
Pb1—O5—C12—C11	−1 (3)	Pb1B—O5B—C12B—C11B	17 (9)
Pb1—O5—C12—C13	178.8 (12)	Pb1B—O5B—C12B—C13B	−171 (4)
Ni2—O2—C3—C2	175.3 (15)	Ni2B—O2B—C3B—C2B	−173 (3)
Ni2—O2—C3—C4	−3 (3)	Ni2B—O2B—C3B—C4B	4 (6)
Ni2—O3—C8—C4	9.3 (18)	Ni2B—O3B—C8B—C4B	4 (5)
Ni2—O5—C12—C11	−173.8 (13)	Ni2B—O5B—C12B—C11B	179 (5)
Ni2—O5—C12—C13	6 (3)	Ni2B—O5B—C12B—C13B	−9 (9)
Ni2—N1—C17—C13	4.9 (16)	Ni2B—N1B—C17B—C13B	12 (7)
O1—C2—C3—O2	2 (3)	O1B—C2B—C3B—O2B	−2 (7)
O1—C2—C3—C4	−179.7 (18)	O1B—C2B—C3B—C4B	180 (5)
O1—C2—C7—C6	−179.7 (18)	O1B—C2B—C7B—C6B	−178 (5)
O2—C3—C4—C5	178.6 (17)	O2B—C3B—C4B—C5B	−174 (4)
O2—C3—C4—C8	−4 (3)	O2B—C3B—C4B—C8B	3 (7)
O4—C11—C12—O5	0 (3)	O4B—C11B—C12B—O5B	−10 (10)
O4—C11—C12—C13	179.7 (17)	O4B—C11B—C12B—C13B	178 (5)
O4—C11—C16—C15	−178.9 (17)	O4B—C11B—C16B—C15B	−177 (5)
O5—C12—C13—C14	177.7 (16)	O5B—C12B—C13B—C14B	−174 (5)
O5—C12—C13—C17	−1 (3)	O5B—C12B—C13B—C17B	1 (9)
C1—O1—C2—C3	−174.3 (19)	C1B—O1B—C2B—C3B	166 (4)
C1—O1—C2—C7	8 (3)	C1B—O1B—C2B—C7B	−13 (8)
C2—C3—C4—C5	0 (3)	C2B—C3B—C4B—C5B	3 (7)
C2—C3—C4—C8	176.9 (17)	C2B—C3B—C4B—C8B	−179 (4)
C3—C2—C7—C6	2 (3)	C3B—C2B—C7B—C6B	3 (8)
C3—C4—C5—C6	1 (2)	C3B—C4B—C5B—C6B	−8 (7)
C3—C4—C8—O3	1 (2)	C3B—C4B—C8B—O3B	−8 (7)
C4—C5—C6—C7	0 (2)	C4B—C5B—C6B—C7B	11 (8)
C5—C4—C8—O3	178.1 (13)	C5B—C4B—C8B—O3B	170 (4)
C5—C6—C7—C2	−2 (2)	C5B—C6B—C7B—C2B	−9 (8)
C7—C2—C3—O2	180 (2)	C7B—C2B—C3B—O2B	177 (5)
C7—C2—C3—C4	−2 (3)	C7B—C2B—C3B—C4B	−1 (8)
C8—C4—C5—C6	−176.6 (12)	C8B—C4B—C5B—C6B	174 (4)
C10—O4—C11—C12	174.6 (15)	C10B—O4B—C11B—C12B	180 (6)
C10—O4—C11—C16	−7 (3)	C10B—O4B—C11B—C16B	−6 (8)
C11—C12—C13—C14	−2 (2)	C11B—C12B—C13B—C14B	−2 (9)
C11—C12—C13—C17	179.6 (14)	C11B—C12B—C13B—C17B	173 (5)
C12—C11—C16—C15	−1 (3)	C12B—C11B—C16B—C15B	−4 (9)
C12—C13—C14—C15	2 (2)	C12B—C13B—C14B—C15B	−1 (8)
C12—C13—C17—N1	−6 (2)	C12B—C13B—C17B—N1B	−3 (8)
C13—C14—C15—C16	−2 (2)	C13B—C14B—C15B—C16B	1 (8)
C14—C13—C17—N1	176.1 (12)	C14B—C13B—C17B—N1B	173 (5)
C14—C15—C16—C11	1 (3)	C14B—C15B—C16B—C11B	1 (8)
C16—C11—C12—O5	−178 (2)	C16B—C11B—C12B—O5B	176 (6)
C16—C11—C12—C13	2 (3)	C16B—C11B—C12B—C13B	4 (10)
C17—C13—C14—C15	−179.4 (12)	C17B—C13B—C14B—C15B	−176 (4)
C18—N1—C17—C13	178.5 (11)	C18B—N1B—C17B—C13B	−179 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H2···Cl2	0.87	2.27	3.127 (7)	166
O6—H6···Cl2ⁱⁱⁱ	0.87	2.36	3.169 (17)	154
O7—H1···Cl1	0.88	2.31	3.152 (8)	162
O7—H7···Cl1ⁱ	0.88	2.43	3.183 (10)	145
O6B—H6BB···Cl2Bⁱⁱⁱ	0.87	2.14	2.99 (4)	167
C14B—H14B···O6B^iv	0.95	2.50	3.26 (6)	138
C18B—H18D···O3B	0.98	2.27	2.96 (3)	127

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

Acknowledgements

We truly appreciate Professor Sean Parkin's help in modelling the disorder.

Funding information

Funding for this research was provided by: Ministry of Education and Science of Ukraine (grant for the perspective development of the scientific direction "Mathematical sciences and natural sciences" at the Taras Shevchenko National University of Kyiv).

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