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In the title compound, [Pb(ClO4)2(C15H11N3)]n, two mol­ecules occupy general positions while the third lies on a crystallographic twofold axis, giving a total of two and a half mol­ecules per asymmetric unit. Each metal centre is coordinated equatorially by three 2,2′:6′,2′′-terpyridine (terpy) N-donor atoms and axially by two perchlorate O-donor atoms. The distorted penta­gonal bipyramidal geometry is completed by two equatorial O-donor atoms from two perchlorate anions which bridge to two different adjacent metal centres. The coordination about each metal centre is very similar to that seen at the unique PbII centre in the previously published polymorph [Engelhardt, Harrowfield, Miyamae, Patrick, Skelton, Soudi & White (1996). Aust. J. Chem. 49, 1135–1146], but the new polymorph differs from it by the insertion on each side of an existing [bis­(perchlorato)(terpy)lead(II)] mol­ecule of two additional such units. Pairs of asymmetrically bridging perchlorate anions link irregularly spaced PbII centres into undulating chains parallel to [201] which exhibit a repeat distance of 26.280 (4) Å. The significance of this new polymorph lies in the fact that, while it is chemically identical to the known polymorph, it is structurally distinct from it.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108042236/fg3072sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108042236/fg3072Isup2.hkl
Contains datablock I

CCDC reference: 718111

Comment top

Polydentate analogues of the pyridine molecule have played an important role in the development of coordination chemistry and continue to be of considerable interest, in particular the metal complexes of N,N'-bidentate aromatic ligands such as 2,2'-bipyridine (bipy), 1,10-phenanthroline (phen) and the tridentate analogue 2,2':6',2''-terpyridine (terpy). This interest stems not only from the similarity of these ligands to biologically important nitrogen-containing heterocyclic ligands such as porphyrins and purines, but also from their use as building blocks in the construction of supramolecular systems, macromolecules, metallo-oligomers and polymers exhibiting a wide variety of chromophoric, electrochemical, luminescent and magnetic properties (Sauvage et al., 1994; Kaes et al., 2000; Chelucci & Thummel, 2002; Hofmeier et al., 2004; Baronoff et al., 2004; Eryazici et al., 2008; Glasson et al., 2008; Constable, 2007, 2008). In particular, 2,2':6',2''-terpyridine (terpy) is a ligand with a very extensive coordination chemistry. In principle, it can exhibit a variety of coordination modes towards metals, i.e. monodentate, bidentate, terdentate and bridging, but, in practice, it almost invariably acts as a planar tridentate ligand forming 1:1 and 1:2 (metal to ligand) five- or six-coordinate complexes with divalent transition and post-transition metal ions (Brandt et al., 1954; Cargill Thompson, 1997). Particularly interesting from a structural point of view are the 1:1 complexes in which the coordination sphere of the metal ion is completed by solvent or adventitious oxygenated ligands which can also function as bridging ligands, resulting in extended polynuclear architectures of different dimensionalities. In this paper, we report the crystal structure of a new polymorph of [Pb(terpy)(ClO4)2] obtained by reacting a 1:1 molar ratio of Pb(ClO4)2 and terpy in acetonitrile.

In the title compound (I), the molecules containing Pb1 (Fig. 1) and Pb2 occupy general positions while Pb3 lies on a crystallographic twofold axis that also passes through the middle of the central pyridyl ring (atoms N7, C38 and H38). Each metal centre is coordinated by all three N pyridyl donors from its terpy ligand [Pb—N 2.494 (8)–2.540 (9) Å; Table 1] in the equatorial plane and by two axial perchlorate O donors at distances of 2.532 (10)–2.626 (10) Å. Considering only these linkages, the anions may be regarded as unidentate with respect to any one metal centre; an alternative description as strongly asymmetrically bidentate (see below) would involve the consideration of a wide range of much longer Pb—O distances of 3.151 (12)–3.404 (14) Å. The seven coordination at each of the three metal centres in (I) is completed by two equatorial O atoms [Pb—O 2.969 (11)–3.024 (11) Å; Table 1] from two anions bridging to two different adjacent metal centres (Fig. 2). The significant deviations of these O donors in opposing directions out of the equatorial plane represent the principal distortion from pentagonal bipyramidal geometry at each metal centre.

Other notable features of the coordination geometry are the markedly nonlinear O(axial)—Pb—O(axial) angles (Table 1) which have values of around 150°, and the dihedral angles between the outer rings of the terpy ligands which adopt a narrow range of values, namely 11.8 (5), 6.9 (4) and 4.7 (4) ° for Pb1, Pb2 and Pb3, respectively.

The pairs of asymmetrically bridging perchlorate anions described above lead to an extended structure wherein the PbII centres are linked into undulating chains which run parallel to the [201] direction (Fig. 3a) and which are significantly interdigitated. The spacing of the PbII centres is irregular [Pb1···Pb2 5.5835 (10), Pb2···Pb2 6.2364 (11), Pb1···Pb3 6.0004 (10) Å] and this can be traced to variations in the Pb—O—Cl angles associated with the perchlorate bridges: for the shortest Pb1···Pb2 distance, these range between 110.1 (6) and 116.9 (6) °, averaging 114 °; for the longest Pb2···Pb2 distance, the angles are much wider [121.4 (4) and 134.7 (5), average 128 °]; while for the intermediate Pb1···Pb3 distance, the angles [118.8 (5)–129.4 (6), average 124°] are correspondingly intermediate. In the literature, the main distribution of M—O—Cl angles in perchlorate bridges covers a wide range (115–140°, with a few examples extending this range to between 105 and 150 °; Allen, 2002). We believe that this flexibility in the coordination geometry of the perchlorate anion is the prime factor that allows different polymorphs to exist. We have every reason to suspect the existence of other polymorphs based on different proportions of perchlorate geometries. Fig. 3(b) shows alternating regions of hydrophilic perchlorate and hydrophobic terpy units along the b axis.

Crystals of the previously published polymorph were prepared by a different synthetic route (cf. Experimental): hot equimolar solutions of Pb(ClO4)2.3H2O in water and terpyridine in MeOH were combined and the mixture boiled before being allowed to cool overnight (Engelhardt et al., 1996). The resulting structure is considerably simpler, with a single unique PbII centre: this lies on a crystallographic twofold axis, with pairs of symmetry-related perchlorate anions linking successive PbII centres into a one-dimensional polymeric chain. The authors characterize each perchlorate as a highly asymmetric O,O'-bidentate ligand [Pb—O 2.554 (5) and 3.258 (9) Å] to one metal centre while another O atom forms one of the links to the adjacent metal. The same paper reports closely similar chain structures for complexes with other small oxoanions (nitrate and nitrite). The structure of the current polymorph may be formally converted into that of the original one by removal of the [bis(perchlorato)(terpy)lead(II)] units centred on Pb1 and Pb2 and linking Pb3-centred units directly via pairwise perchlorate bridges. The unique repeat distance along the chain in the original polymorph is 6.0670 (6) Å, while in the current structure the Pb3···Pb3 distance is 26.280 (4) Å. Because of the irregularity of the Pb···Pb distances (see above), this considerably longer distance must be regarded as the fundamental repeat distance along the chain. Interestingly, similar undulating chains of doubly-bridged [(terpy)lead(II)] units are observed in the extended structures of {[Pb(C15H11N3)(NO3)2]} (Engelhardt et al., 1996) and {[Pb(C15H11N3)(SCN)2]} (Engelhardt et al., 1989), with Pb···Pb repeat distances of 6.892 (3) and 6.018 (4) Å, respectively.

Related literature top

For related literature, see: Allen (2002); Baronoff et al. (2004); Brandt et al. (1954); Cargill Thompson (1997); Chelucci & Thummel (2002); Constable (2007, 2008); Engelhardt et al. (1989, 1996); Eryazici et al. (2008); Glasson et al. (2008); Hofmeier & Schubert (2004); Kaes et al. (2000); Sauvage et al. (1994).

Experimental top

The title salt was prepared by reaction of Pb(ClO4)2.3H2O (5 mg, 0.0215 mmol) and terpyridine (9.9 mg, 0.0215 mmol) in MeCN (5 ml). Crystals were grown by diffusion of diethyl ether into the reaction mixture. Analysis found (calculated for C15H11Cl2N3O8Pb): C 28.10 (28.18), H 1.80 (1.73), N 6.55 (6.57).

Refinement top

H atoms were placed geometrically and refined riding at a distance of 0.95 Å from their parent C atoms with Uiso(H) = 1.2Ueq(C). Rigid bond restraints were applied to all anisotropic displacement parameters.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: enCIFer (Allen et al., 2004), PLATON (Spek, 2003), publCIF (Westrip, 2008).

Figures top
[Figure 1] Fig. 1. Views of the two and a half independent molecules of the title compound in each asymmetric unit, showing the atom numbering scheme and with displacement ellipsoids drawn at the 30% probability level. For clarity, coordination of Pb by anions primarily bonded to other PbII centres is not shown. The molecules containing Pb1 (a) and Pb2 (b) occupy general positions while Pb3 (c) lies on a crystallographic twofold axis which also bisects the central ring of the ligand. Atoms whose labels include the suffix A are related to their unsuffixed equivalents by the symmetry operation (1 - x, y, 1/2 - z).
[Figure 2] Fig. 2. A view of the asymmetric unit, extended to complete the coordination sphere around Pb2 and Pb3, and showing the distorted N3O4 coordination at each metal centre. The unlabelled N atoms, shown as blue circles in the online version, are shaded bottom left to top right. Atoms whose labels include the suffices A and B are related to their unsuffixed equivalents by the symmetry operations (1 - x, y, 1/2 - z) and (-x, 1 - y, -z), respectively.
[Figure 3] Fig. 3. (a) A view approximately along the b axis, showing chains of molecules running along the [201] direction. The atoms shown as purple spheres in the central chain are Pb3 and two of its symmetry equivalents. The shortest Pb3···Pb3 separation along the chain is 26.280 (4) Å and represents the fundamental repeat distance. (b) An orthogonal view, showing the alternation of hydrophilic (perchlorate) and hydrophobic (terpy) regions along the b axis.
poly[bis(µ2-perchlorato-κ2O:O')(2,2':6',2''-terpyridine- κ3N,N',N'')lead(II)] top
Crystal data top
[Pb(ClO4)2(C15H11N3)]F(000) = 6040
Mr = 639.36Dx = 2.359 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2817 reflections
a = 25.440 (4) Åθ = 2.5–27.9°
b = 16.333 (3) ŵ = 9.72 mm1
c = 21.916 (4) ÅT = 150 K
β = 98.671 (2)°Column, colourless
V = 9002 (4) Å30.25 × 0.08 × 0.05 mm
Z = 20
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
8832 independent reflections
Radiation source: sealed tube4705 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
ω scansθmax = 26.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 3230
Tmin = 0.514, Tmax = 1.000k = 1221
27358 measured reflectionsl = 2427
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.126H-atom parameters constrained
S = 1.03 w = 1/[σ^2^(Fo^2^) + (0.027P)^2^ + 69.73P]
where P = (Fo^2^ + 2Fc^2^)/3
8832 reflections(Δ/σ)max = 0.003
655 parametersΔρmax = 2.07 e Å3
220 restraintsΔρmin = 2.43 e Å3
Crystal data top
[Pb(ClO4)2(C15H11N3)]V = 9002 (4) Å3
Mr = 639.36Z = 20
Monoclinic, C2/cMo Kα radiation
a = 25.440 (4) ŵ = 9.72 mm1
b = 16.333 (3) ÅT = 150 K
c = 21.916 (4) Å0.25 × 0.08 × 0.05 mm
β = 98.671 (2)°
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
8832 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
4705 reflections with I > 2σ(I)
Tmin = 0.514, Tmax = 1.000Rint = 0.052
27358 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.045220 restraints
wR(F2) = 0.126H-atom parameters constrained
S = 1.03 w = 1/[σ^2^(Fo^2^) + (0.027P)^2^ + 69.73P]
where P = (Fo^2^ + 2Fc^2^)/3
8832 reflectionsΔρmax = 2.07 e Å3
655 parametersΔρmin = 2.43 e Å3
Special details top

Geometry. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

23.5451 (0.0492) x + 1.7226 (0.0859) y + 4.8224 (0.1106) z = 9.1427 (0.0561)

* 0.0033 (0.0088) N3 * 0.0025 (0.0089) C11 * -0.0014 (0.0090) C12 * -0.0049 (0.0092) C13 * 0.0107 (0.0096) C14 * -0.0101 (0.0092) C15 - 0.4850 (0.0196) Pb1

Rms deviation of fitted atoms = 0.0066

23.5313 (0.0506) x - 1.6446 (0.0850) y + 4.8831 (0.1126) z = 6.4665 (0.0630)

Angle to previous plane (with approximate e.s.d.) = 11.83 (0.48)

* -0.0214 (0.0082) N1 * 0.0286 (0.0090) C1 * -0.0173 (0.0099) C2 * -0.0006 (0.0103) C3 * 0.0068 (0.0096) C4 * 0.0040 (0.0089) C5 0.2393 (0.0198) Pb1

Rms deviation of fitted atoms = 0.0165

24.0082 (0.0420) x - 0.7988 (0.0824) y + 3.9689 (0.1077) z = 2.4376 (0.0345)

Angle to previous plane (with approximate e.s.d.) = 3.88 (0.49)

* -0.0160 (0.0081) N4 * 0.0038 (0.0087) C26 * 0.0021 (0.0095) C27 * 0.0029 (0.0095) C28 * -0.0141 (0.0089) C29 * 0.0212 (0.0087) C30 0.0065 (0.0192) Pb2

Rms deviation of fitted atoms = 0.0124

24.0055 (0.0418) x + 1.1685 (0.0899) y + 3.8852 (0.1065) z = 2.9174 (0.0326)

Angle to previous plane (with approximate e.s.d.) = 6.91 (0.44)

* 0.0014 (0.0085) N6 * -0.0042 (0.0090) C16 * 0.0097 (0.0089) C17 * -0.0118 (0.0091) C18 * 0.0083 (0.0090) C19 * -0.0034 (0.0089) C20 0.3427 (0.0191) Pb2

Rms deviation of fitted atoms = 0.0074

24.0996 (0.0400) x - 0.6892 (0.1045) y + 3.7494 (0.1053) z = 12.8401 (0.0432)

Angle to previous plane (with approximate e.s.d.) = 6.53 (0.43)

* 0.0110 (0.0067) N8 * -0.0050 (0.0037) C32 * -0.0050 (0.0037) C32 * 0.0093 (0.0099) C33 * 0.0014 (0.0086) C34 * -0.0116 (0.0086) C35 - 0.1401 (0.0209) Pb3

Rms deviation of fitted atoms = 0.0081

24.1132 (0.0401) x + 0.6461 (0.0816) y + 3.7202 (0.1065) z = 13.1264 (0.0266)

Angle to previous plane (with approximate e.s.d.) = 4.69 (0.42)

* -0.0156 (0.0080) N8_$1 * 0.0089 (0.0086) C31_$1 * 0.0029 (0.0087) C32_$1 * -0.0076 (0.0088) C33_$1 * 0.0008 (0.0089) C34_$1 * 0.0107 (0.0084) C35_$1

Rms deviation of fitted atoms = 0.0092

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.29584 (2)0.58101 (3)0.14318 (2)0.0274 (1)
Pb20.10584 (2)0.41745 (3)0.05993 (2)0.0204 (1)
Pb30.500000.41658 (5)0.250000.0265 (2)
Cl10.36484 (14)0.4067 (2)0.26047 (12)0.0301 (10)
Cl20.23748 (13)0.4117 (3)0.03496 (12)0.0300 (9)
Cl30.16410 (13)0.5837 (3)0.16825 (11)0.0300 (10)
Cl40.43245 (12)0.5844 (2)0.13279 (11)0.0257 (9)
Cl50.03225 (12)0.4109 (2)0.06172 (11)0.0243 (9)
O10.4021 (4)0.3798 (7)0.2208 (4)0.052 (3)
O20.3876 (4)0.4700 (7)0.2983 (5)0.062 (4)
O30.3162 (4)0.4330 (7)0.2227 (4)0.041 (3)
O40.3533 (5)0.3375 (8)0.2960 (5)0.083 (5)
O50.2041 (4)0.3644 (6)0.0685 (4)0.044 (3)
O60.2881 (4)0.4250 (7)0.0713 (4)0.044 (3)
O70.2113 (4)0.4887 (8)0.0218 (5)0.069 (4)
O80.2434 (5)0.3708 (10)0.0191 (5)0.105 (5)
O90.1980 (4)0.6303 (7)0.1360 (4)0.047 (3)
O100.1597 (5)0.6207 (10)0.2234 (5)0.109 (6)
O110.1867 (4)0.5058 (8)0.1775 (6)0.077 (4)
O120.1125 (4)0.5753 (7)0.1328 (4)0.040 (3)
O130.3941 (4)0.6119 (7)0.1706 (4)0.051 (3)
O140.4106 (5)0.5172 (8)0.0973 (6)0.081 (5)
O150.4404 (5)0.6522 (8)0.0951 (5)0.085 (5)
O160.4804 (4)0.5653 (7)0.1720 (4)0.045 (3)
O170.0441 (4)0.3410 (6)0.0940 (4)0.043 (3)
O180.0116 (4)0.4752 (6)0.1035 (4)0.036 (3)
O190.0074 (3)0.3918 (6)0.0233 (3)0.034 (2)
O200.0793 (3)0.4383 (6)0.0218 (4)0.035 (3)
N10.3101 (4)0.6465 (7)0.0433 (4)0.026 (2)
N20.2996 (5)0.7336 (5)0.1448 (5)0.0292 (19)
N30.2904 (5)0.6446 (8)0.2461 (4)0.033 (2)
N40.0867 (4)0.3526 (7)0.1596 (4)0.027 (2)
N50.1002 (4)0.2645 (7)0.0590 (4)0.023 (2)
N60.1118 (4)0.3524 (7)0.0421 (4)0.026 (2)
N70.500000.2636 (9)0.250000.025 (3)
N80.4883 (4)0.3527 (7)0.3517 (4)0.025 (2)
C10.3186 (5)0.5980 (9)0.0050 (5)0.032 (4)
C20.3302 (5)0.6293 (9)0.0584 (5)0.032 (4)
C30.3375 (6)0.7111 (10)0.0635 (6)0.040 (4)
C40.3317 (6)0.7632 (9)0.0146 (6)0.033 (3)
C50.3173 (5)0.7264 (9)0.0384 (5)0.027 (3)
C60.3087 (5)0.7767 (8)0.0939 (5)0.026 (3)
C70.3099 (5)0.8620 (9)0.0928 (6)0.031 (4)
C80.3005 (7)0.9038 (7)0.1461 (6)0.034 (3)
C90.2912 (6)0.8619 (9)0.1969 (6)0.037 (4)
C100.2904 (5)0.7757 (9)0.1953 (5)0.028 (3)
C110.2838 (5)0.7267 (9)0.2503 (5)0.026 (3)
C120.2705 (5)0.7600 (9)0.3029 (5)0.030 (3)
C130.2632 (6)0.7119 (10)0.3538 (6)0.034 (4)
C140.2710 (6)0.6279 (9)0.3477 (5)0.037 (4)
C150.2837 (5)0.5989 (9)0.2937 (5)0.031 (4)
C160.1166 (5)0.4016 (9)0.0889 (4)0.032 (4)
C170.1273 (5)0.3707 (9)0.1456 (5)0.029 (3)
C180.1320 (5)0.2886 (9)0.1522 (5)0.031 (4)
C190.1270 (6)0.2348 (9)0.1020 (5)0.035 (4)
C200.1163 (5)0.2725 (8)0.0471 (5)0.025 (3)
C210.1087 (5)0.2215 (8)0.0074 (5)0.023 (3)
C220.1090 (5)0.1389 (9)0.0050 (5)0.029 (3)
C230.0998 (5)0.0969 (10)0.0579 (5)0.031 (4)
C240.0900 (6)0.1373 (9)0.1100 (5)0.030 (4)
C250.0909 (5)0.2230 (8)0.1091 (5)0.025 (3)
C260.0835 (5)0.2717 (8)0.1648 (5)0.021 (3)
C270.0731 (6)0.2342 (9)0.2189 (5)0.033 (4)
C280.0666 (6)0.2840 (9)0.2689 (5)0.032 (4)
C290.0697 (5)0.3687 (9)0.2634 (5)0.028 (3)
C300.0810 (5)0.3989 (8)0.2073 (4)0.025 (3)
C310.4813 (5)0.3994 (8)0.3996 (5)0.029 (3)
C320.4721 (5)0.3689 (9)0.4554 (5)0.031 (4)
C330.4697 (6)0.2843 (9)0.4623 (5)0.032 (4)
C340.4757 (5)0.2349 (9)0.4110 (5)0.028 (3)
C350.4848 (5)0.2696 (8)0.3568 (5)0.026 (3)
C360.4922 (5)0.2216 (8)0.3015 (5)0.027 (3)
C370.4911 (5)0.1354 (9)0.3029 (6)0.033 (4)
C380.500000.0928 (13)0.250000.033 (5)
H10.316400.540200.000900.0380*
H20.333200.594200.092300.0380*
H30.346600.733000.100600.0480*
H40.337300.820500.017000.0400*
H70.316800.890900.057200.0370*
H80.300600.962000.146700.0410*
H90.285300.890400.233100.0440*
H120.266000.817600.305100.0360*
H130.253600.735000.390300.0420*
H140.267500.591600.380800.0440*
H150.288000.541400.290000.0370*
H160.112700.459000.084100.0380*
H170.131200.406700.178700.0350*
H180.138600.266700.190500.0370*
H190.130600.177200.105300.0430*
H220.115100.110600.031100.0340*
H230.100400.038700.057900.0370*
H240.082900.108200.145400.0360*
H270.070500.176300.221500.0400*
H280.060000.260200.306600.0390*
H290.064400.404300.296200.0340*
H300.084800.456400.203300.0300*
H310.482900.457100.394900.0350*
H320.467500.404500.488400.0370*
H330.464100.260600.500400.0380*
H340.473300.177000.414200.0330*
H370.484500.106900.338800.0390*
H380.500000.034600.250000.0400*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0347 (2)0.0180 (2)0.0335 (2)0.0002 (3)0.0177 (2)0.0009 (2)
Pb20.0282 (2)0.0172 (3)0.0177 (2)0.0010 (2)0.0092 (2)0.0001 (2)
Pb30.0382 (4)0.0152 (4)0.0297 (3)0.00000.0172 (3)0.0000
Cl10.0349 (17)0.029 (2)0.0261 (12)0.0061 (17)0.0039 (12)0.0002 (12)
Cl20.0287 (16)0.036 (2)0.0258 (12)0.0015 (18)0.0060 (11)0.0054 (14)
Cl30.0326 (17)0.035 (2)0.0239 (12)0.0066 (18)0.0092 (11)0.0030 (14)
Cl40.0277 (15)0.025 (2)0.0250 (12)0.0010 (17)0.0060 (11)0.0018 (13)
Cl50.0324 (16)0.0214 (19)0.0200 (11)0.0065 (16)0.0072 (10)0.0021 (12)
O10.036 (4)0.071 (8)0.048 (4)0.019 (4)0.005 (3)0.026 (4)
O20.055 (7)0.060 (6)0.065 (6)0.016 (5)0.008 (5)0.042 (5)
O30.039 (5)0.040 (7)0.041 (5)0.012 (5)0.003 (4)0.003 (4)
O40.083 (9)0.082 (8)0.081 (7)0.005 (7)0.004 (6)0.054 (6)
O50.025 (3)0.044 (6)0.061 (5)0.000 (3)0.003 (3)0.022 (4)
O60.033 (4)0.036 (7)0.058 (5)0.006 (4)0.007 (4)0.009 (5)
O70.044 (6)0.066 (6)0.102 (8)0.016 (5)0.028 (6)0.059 (5)
O80.063 (8)0.187 (13)0.069 (6)0.020 (8)0.026 (5)0.082 (7)
O90.032 (3)0.056 (6)0.054 (4)0.007 (3)0.013 (3)0.020 (4)
O100.064 (8)0.220 (14)0.046 (5)0.022 (8)0.022 (4)0.071 (7)
O110.036 (6)0.056 (5)0.139 (10)0.001 (5)0.014 (6)0.050 (6)
O120.027 (4)0.043 (7)0.049 (4)0.002 (4)0.006 (3)0.013 (4)
O130.031 (3)0.086 (8)0.036 (4)0.015 (4)0.005 (3)0.018 (4)
O140.055 (8)0.063 (7)0.119 (9)0.007 (6)0.008 (6)0.062 (6)
O150.086 (9)0.094 (8)0.074 (7)0.016 (7)0.008 (6)0.059 (6)
O160.032 (4)0.057 (8)0.044 (5)0.011 (5)0.001 (4)0.003 (4)
O170.062 (6)0.035 (5)0.034 (4)0.004 (4)0.019 (4)0.009 (3)
O180.039 (6)0.031 (5)0.037 (4)0.002 (4)0.001 (4)0.007 (3)
O190.026 (3)0.048 (6)0.029 (3)0.004 (3)0.010 (2)0.001 (3)
O200.028 (4)0.039 (6)0.036 (4)0.004 (4)0.001 (3)0.001 (3)
N10.023 (5)0.022 (4)0.034 (3)0.005 (5)0.005 (3)0.000 (3)
N20.029 (4)0.021 (3)0.038 (3)0.002 (4)0.006 (4)0.000 (3)
N30.036 (5)0.028 (4)0.037 (3)0.002 (6)0.012 (3)0.003 (3)
N40.038 (5)0.020 (4)0.023 (3)0.004 (5)0.006 (3)0.003 (3)
N50.023 (5)0.022 (3)0.025 (3)0.002 (3)0.004 (4)0.002 (3)
N60.033 (5)0.023 (4)0.023 (3)0.001 (5)0.008 (3)0.005 (3)
N70.020 (7)0.019 (4)0.040 (5)0.00000.019 (6)0.0000
N80.022 (5)0.022 (4)0.035 (3)0.005 (5)0.014 (3)0.003 (3)
C10.037 (8)0.028 (6)0.031 (4)0.005 (6)0.007 (5)0.000 (4)
C20.030 (8)0.034 (6)0.031 (4)0.003 (6)0.004 (5)0.000 (4)
C30.041 (9)0.037 (7)0.046 (6)0.001 (7)0.018 (6)0.005 (5)
C40.029 (7)0.025 (6)0.047 (5)0.008 (6)0.013 (5)0.005 (4)
C50.020 (7)0.022 (4)0.038 (4)0.001 (6)0.004 (5)0.003 (3)
C60.022 (8)0.018 (3)0.037 (4)0.004 (6)0.000 (4)0.001 (3)
C70.022 (8)0.019 (4)0.053 (6)0.002 (6)0.007 (5)0.003 (4)
C80.033 (6)0.012 (4)0.057 (6)0.014 (8)0.004 (5)0.001 (4)
C90.033 (9)0.022 (4)0.055 (6)0.008 (7)0.007 (6)0.003 (4)
C100.020 (7)0.022 (4)0.043 (4)0.010 (6)0.009 (5)0.006 (3)
C110.016 (7)0.027 (4)0.036 (4)0.000 (6)0.003 (4)0.004 (3)
C120.024 (7)0.028 (6)0.038 (5)0.004 (6)0.005 (5)0.008 (4)
C130.030 (8)0.038 (7)0.036 (5)0.005 (7)0.008 (5)0.004 (5)
C140.044 (9)0.037 (6)0.028 (4)0.004 (7)0.000 (5)0.003 (5)
C150.032 (8)0.027 (6)0.033 (4)0.006 (6)0.003 (5)0.004 (4)
C160.044 (8)0.032 (6)0.022 (4)0.004 (7)0.014 (5)0.002 (3)
C170.023 (7)0.038 (6)0.028 (4)0.011 (6)0.012 (5)0.003 (4)
C180.028 (8)0.039 (7)0.026 (4)0.011 (6)0.009 (5)0.005 (4)
C190.052 (10)0.032 (6)0.022 (4)0.002 (7)0.005 (5)0.009 (4)
C200.027 (8)0.024 (4)0.025 (4)0.001 (6)0.006 (4)0.009 (3)
C210.017 (7)0.022 (3)0.030 (4)0.005 (5)0.006 (4)0.005 (3)
C220.024 (8)0.023 (4)0.039 (5)0.000 (6)0.004 (5)0.002 (4)
C230.033 (9)0.021 (6)0.039 (5)0.007 (6)0.010 (5)0.006 (4)
C240.032 (9)0.023 (4)0.035 (5)0.005 (6)0.006 (5)0.001 (4)
C250.022 (7)0.020 (3)0.033 (4)0.008 (6)0.007 (4)0.005 (3)
C260.015 (7)0.019 (4)0.029 (4)0.005 (5)0.005 (4)0.006 (3)
C270.044 (9)0.027 (6)0.030 (4)0.011 (6)0.008 (5)0.013 (4)
C280.037 (9)0.034 (6)0.026 (4)0.005 (7)0.009 (5)0.011 (4)
C290.025 (7)0.033 (6)0.028 (4)0.003 (6)0.012 (4)0.002 (4)
C300.028 (7)0.023 (5)0.024 (4)0.000 (6)0.006 (4)0.004 (3)
C310.030 (7)0.023 (5)0.035 (4)0.002 (6)0.010 (5)0.003 (4)
C320.034 (8)0.032 (6)0.023 (4)0.004 (6)0.006 (5)0.000 (4)
C330.034 (8)0.035 (6)0.027 (4)0.002 (6)0.005 (5)0.013 (4)
C340.018 (6)0.025 (6)0.043 (5)0.002 (5)0.011 (5)0.006 (4)
C350.022 (7)0.022 (4)0.036 (4)0.002 (6)0.009 (5)0.003 (3)
C360.024 (7)0.018 (4)0.041 (5)0.000 (6)0.011 (5)0.004 (3)
C370.022 (8)0.018 (4)0.061 (7)0.000 (6)0.017 (6)0.002 (4)
C380.024 (10)0.011 (7)0.069 (9)0.00000.022 (8)0.0000
Geometric parameters (Å, º) top
Pb1—O32.980 (11)C6—C71.39 (2)
Pb1—O62.987 (11)C7—C81.404 (19)
Pb1—O92.598 (10)C8—C91.358 (19)
Pb1—O132.532 (10)C9—C101.41 (2)
Pb1—N12.511 (9)C10—C111.477 (17)
Pb1—N22.494 (8)C11—C121.363 (17)
Pb1—N32.506 (10)C12—C131.400 (19)
Pb2—O52.626 (10)C13—C141.40 (2)
Pb2—O123.024 (11)C14—C151.358 (17)
Pb2—O192.547 (8)C16—C171.405 (15)
Pb2—O20i2.975 (9)C17—C181.36 (2)
Pb2—N42.540 (9)C18—C191.429 (18)
Pb2—N52.502 (11)C19—C201.414 (17)
Pb2—N62.501 (9)C20—C211.493 (17)
Pb3—O12.548 (10)C21—C221.35 (2)
Pb3—O162.969 (11)C22—C231.397 (17)
Pb3—N72.499 (15)C23—C241.374 (18)
Pb3—N82.519 (9)C24—C251.40 (2)
Cl1—O11.448 (10)C25—C261.493 (16)
Cl1—O21.395 (12)C26—C271.395 (17)
Cl1—O31.446 (10)C27—C281.394 (18)
Cl1—O41.428 (13)C28—C291.39 (2)
Cl2—O51.431 (10)C29—C301.394 (15)
Cl2—O61.425 (10)C31—C321.373 (16)
Cl2—O71.432 (13)C32—C331.39 (2)
Cl2—O81.388 (13)C33—C341.411 (18)
Cl3—O91.417 (11)C34—C351.367 (16)
Cl3—O101.371 (13)C35—C361.479 (16)
Cl3—O111.398 (14)C36—C371.41 (2)
Cl3—O121.428 (10)C37—C381.400 (17)
Cl4—O131.444 (10)C1—H10.9500
Cl4—O141.410 (13)C2—H20.9500
Cl4—O151.414 (13)C3—H30.9500
Cl4—O161.417 (10)C4—H40.9500
Cl5—O171.400 (10)C7—H70.9500
Cl5—O181.440 (10)C8—H80.9500
Cl5—O191.442 (8)C9—H90.9500
Cl5—O201.443 (9)C12—H120.9500
N1—C11.365 (16)C13—H130.9500
N1—C51.324 (19)C14—H140.9500
N2—C61.368 (16)C15—H150.9500
N2—C101.353 (16)C16—H160.9500
N3—C111.36 (2)C17—H170.9500
N3—C151.315 (16)C18—H180.9500
N4—C261.330 (17)C19—H190.9500
N4—C301.316 (14)C22—H220.9500
N5—C211.376 (15)C23—H230.9500
N5—C251.341 (15)C24—H240.9500
N6—C161.323 (15)C27—H270.9500
N6—C201.316 (17)C28—H280.9500
N7—C361.361 (14)C29—H290.9500
N7—C36ii1.361 (14)C30—H300.9500
N8—C311.331 (15)C31—H310.9500
N8—C351.366 (17)C32—H320.9500
C1—C21.350 (17)C33—H330.9500
C2—C31.36 (2)C34—H340.9500
C3—C41.39 (2)C37—H370.9500
C4—C51.405 (18)C38—H380.9500
C5—C61.511 (17)
O3—Pb1—O666.9 (3)Pb3—N8—C35120.1 (7)
O3—Pb1—O9111.6 (3)C31—N8—C35119.1 (10)
O3—Pb1—O1386.8 (3)N1—C1—C2122.2 (13)
O3—Pb1—N1145.1 (3)C1—C2—C3119.7 (12)
O3—Pb1—N2143.1 (3)C2—C3—C4120.4 (13)
O3—Pb1—N380.7 (3)C3—C4—C5116.5 (13)
O6—Pb1—O9104.2 (3)N1—C5—C4123.0 (12)
O6—Pb1—O13106.2 (3)N1—C5—C6115.6 (10)
O6—Pb1—N184.9 (3)C4—C5—C6121.4 (13)
O6—Pb1—N2149.3 (3)N2—C6—C5116.1 (11)
O6—Pb1—N3145.1 (3)N2—C6—C7122.4 (11)
O9—Pb1—O13148.8 (4)C5—C6—C7121.6 (11)
O9—Pb1—N194.5 (3)C6—C7—C8117.7 (12)
O9—Pb1—N274.1 (4)C7—C8—C9120.6 (12)
O9—Pb1—N375.2 (3)C8—C9—C10119.2 (12)
O13—Pb1—N181.7 (3)N2—C10—C9121.7 (11)
O13—Pb1—N276.3 (4)N2—C10—C11116.6 (12)
O13—Pb1—N383.7 (4)C9—C10—C11121.6 (11)
N1—Pb1—N265.0 (4)N3—C11—C10116.7 (10)
N1—Pb1—N3130.0 (4)N3—C11—C12120.1 (12)
N2—Pb1—N365.2 (4)C10—C11—C12123.2 (13)
O5—Pb2—O12105.5 (3)C11—C12—C13122.0 (14)
O5—Pb2—O19148.1 (3)C12—C13—C14116.0 (12)
O5—Pb2—O20i115.6 (3)C13—C14—C15118.8 (12)
O5—Pb2—N496.0 (3)N3—C15—C14124.7 (14)
O5—Pb2—N574.0 (3)N6—C16—C17121.3 (13)
O5—Pb2—N674.8 (3)C16—C17—C18118.8 (12)
O12—Pb2—O19106.3 (3)C17—C18—C19120.4 (11)
O12—Pb2—O20i68.4 (3)C18—C19—C20116.0 (13)
O12—Pb2—N484.5 (3)N6—C20—C19122.2 (11)
O12—Pb2—N5148.7 (3)N6—C20—C21117.6 (10)
O12—Pb2—N6145.9 (3)C19—C20—C21120.2 (12)
O19—Pb2—O20i79.5 (3)N5—C21—C20115.4 (11)
O19—Pb2—N484.0 (3)N5—C21—C22123.0 (11)
O19—Pb2—N577.3 (3)C20—C21—C22121.6 (10)
O19—Pb2—N680.7 (3)C21—C22—C23117.1 (12)
O20i—Pb2—N4142.4 (3)C22—C23—C24121.9 (14)
O20i—Pb2—N5141.1 (3)C23—C24—C25117.6 (12)
O20i—Pb2—N680.6 (3)N5—C25—C24121.5 (11)
N4—Pb2—N564.7 (3)N5—C25—C26117.4 (11)
N4—Pb2—N6129.6 (4)C24—C25—C26121.1 (10)
N5—Pb2—N665.2 (3)N4—C26—C25116.3 (10)
O1—Pb3—O1688.6 (3)N4—C26—C27122.1 (11)
O1—Pb3—N776.4 (3)C25—C26—C27121.7 (12)
O1—Pb3—N883.3 (3)C26—C27—C28118.2 (13)
O1—Pb3—O1ii152.7 (4)C27—C28—C29119.8 (11)
O1—Pb3—O16ii114.2 (3)C28—C29—C30116.7 (11)
O1—Pb3—N8ii85.5 (3)N4—C30—C29124.0 (12)
O16—Pb3—N7144.9 (2)N8—C31—C32123.8 (12)
O16—Pb3—N8144.7 (3)C31—C32—C33118.2 (11)
O16—Pb3—O16ii70.2 (3)C32—C33—C34118.0 (11)
O16—Pb3—N8ii82.0 (3)C33—C34—C35120.6 (13)
N7—Pb3—N865.5 (3)N8—C35—C34120.3 (11)
N8—Pb3—N8ii131.1 (4)N8—C35—C36116.2 (10)
O1—Cl1—O2109.3 (6)C34—C35—C36123.5 (12)
O1—Cl1—O3109.1 (5)N7—C36—C35117.7 (12)
O1—Cl1—O4107.1 (7)N7—C36—C37121.9 (11)
O2—Cl1—O3111.3 (7)C35—C36—C37120.4 (11)
O2—Cl1—O4111.3 (7)C36—C37—C38118.2 (13)
O3—Cl1—O4108.6 (7)C37—C38—C37ii120.4 (17)
O5—Cl2—O6110.6 (6)N1—C1—H1119.00
O5—Cl2—O7106.5 (6)C2—C1—H1119.00
O5—Cl2—O8109.1 (8)C1—C2—H2120.00
O6—Cl2—O7109.4 (7)C3—C2—H2120.00
O6—Cl2—O8110.2 (7)C2—C3—H3120.00
O7—Cl2—O8111.0 (8)C4—C3—H3120.00
O9—Cl3—O10109.9 (8)C3—C4—H4122.00
O9—Cl3—O11107.1 (7)C5—C4—H4122.00
O9—Cl3—O12111.1 (6)C6—C7—H7121.00
O10—Cl3—O11111.1 (8)C8—C7—H7121.00
O10—Cl3—O12109.4 (7)C7—C8—H8120.00
O11—Cl3—O12108.4 (7)C9—C8—H8120.00
O13—Cl4—O14108.3 (7)C8—C9—H9120.00
O13—Cl4—O15105.1 (7)C10—C9—H9120.00
O13—Cl4—O16108.4 (5)C11—C12—H12119.00
O14—Cl4—O15111.5 (7)C13—C12—H12119.00
O14—Cl4—O16113.3 (7)C12—C13—H13122.00
O15—Cl4—O16109.9 (7)C14—C13—H13122.00
O17—Cl5—O18111.1 (5)C13—C14—H14121.00
O17—Cl5—O19110.0 (6)C15—C14—H14121.00
O17—Cl5—O20109.7 (6)N3—C15—H15118.00
O18—Cl5—O19108.0 (6)C14—C15—H15118.00
O18—Cl5—O20110.4 (6)N6—C16—H16119.00
O19—Cl5—O20107.6 (5)C17—C16—H16119.00
Pb3—O1—Cl1118.8 (5)C16—C17—H17121.00
Pb1—O3—Cl1129.4 (6)C18—C17—H17121.00
Pb2—O5—Cl2114.7 (5)C17—C18—H18120.00
Pb1—O6—Cl2114.0 (6)C19—C18—H18120.00
Pb1—O9—Cl3116.9 (6)C18—C19—H19122.00
Pb2—O12—Cl3110.1 (6)C20—C19—H19122.00
Pb1—O13—Cl4122.0 (5)C21—C22—H22121.00
Pb3—O16—Cl4125.7 (6)C23—C22—H22121.00
Pb2—O19—Cl5121.4 (4)C22—C23—H23119.00
Pb2—O20i—Cl5i134.7 (5)C24—C23—H23119.00
Pb1—N1—C1119.3 (9)C23—C24—H24121.00
Pb1—N1—C5122.0 (7)C25—C24—H24121.00
C1—N1—C5118.0 (10)C26—C27—H27121.00
Pb1—N2—C6120.9 (8)C28—C27—H27121.00
Pb1—N2—C10120.6 (8)C27—C28—H28120.00
C6—N2—C10118.5 (10)C29—C28—H28120.00
Pb1—N3—C11119.7 (7)C28—C29—H29122.00
Pb1—N3—C15120.7 (10)C30—C29—H29121.00
C11—N3—C15118.4 (11)N4—C30—H30118.00
Pb2—N4—C26120.7 (7)C29—C30—H30118.00
Pb2—N4—C30120.1 (8)N8—C31—H31118.00
C26—N4—C30119.2 (10)C32—C31—H31118.00
Pb2—N5—C21120.0 (8)C31—C32—H32121.00
Pb2—N5—C25121.0 (8)C33—C32—H32121.00
C21—N5—C25118.9 (11)C32—C33—H33121.00
Pb2—N6—C16117.4 (9)C34—C33—H33121.00
Pb2—N6—C20120.9 (7)C33—C34—H34120.00
C16—N6—C20121.2 (10)C35—C34—H34120.00
Pb3—N7—C36120.3 (8)C36—C37—H37121.00
Pb3—N7—C36ii120.3 (8)C38—C37—H37121.00
C36—N7—C36ii119.5 (13)C37—C38—H38120.00
Pb3—N8—C31120.5 (8)C37ii—C38—H38120.00
C5—N1—C1—C24.8 (18)C9—C10—C11—C1210 (2)
C1—N1—C5—C41.9 (19)N3—C11—C12—C130 (2)
C1—N1—C5—C6178.5 (11)C10—C11—C12—C13178.4 (13)
C10—N2—C6—C5178.5 (11)C11—C12—C13—C141 (2)
C10—N2—C6—C71.4 (19)C12—C13—C14—C151 (2)
C6—N2—C10—C91 (2)C13—C14—C15—N31 (2)
C6—N2—C10—C11176.7 (12)N6—C16—C17—C180.9 (19)
C15—N3—C11—C10178.6 (12)C16—C17—C18—C191.0 (19)
C15—N3—C11—C120.1 (19)C17—C18—C19—C201 (2)
C11—N3—C15—C141 (2)C18—C19—C20—N61 (2)
C30—N4—C26—C25179.4 (11)C18—C19—C20—C21178.1 (12)
C30—N4—C26—C271.5 (19)N6—C20—C21—N53.1 (17)
C26—N4—C30—C292.5 (19)N6—C20—C21—C22175.4 (12)
C25—N5—C21—C20177.4 (11)C19—C20—C21—N5178.0 (12)
C25—N5—C21—C221.1 (18)C19—C20—C21—C223.5 (19)
C21—N5—C25—C240.4 (18)N5—C21—C22—C230.4 (19)
C21—N5—C25—C26178.2 (11)C20—C21—C22—C23178.0 (12)
C20—N6—C16—C170.7 (19)C21—C22—C23—C241.0 (19)
C16—N6—C20—C190.7 (19)C22—C23—C24—C252 (2)
C16—N6—C20—C21178.2 (11)C23—C24—C25—N51 (2)
C36ii—N7—C36—C35179.0 (10)C23—C24—C25—C26176.8 (12)
C36ii—N7—C36—C371.0 (15)N5—C25—C26—N40.2 (17)
C35—N8—C31—C321.9 (19)N5—C25—C26—C27179.3 (12)
C31—N8—C35—C341.8 (18)C24—C25—C26—N4178.0 (12)
C31—N8—C35—C36179.1 (11)C24—C25—C26—C273 (2)
N1—C1—C2—C35 (2)N4—C26—C27—C281 (2)
C1—C2—C3—C42 (2)C25—C26—C27—C28179.9 (13)
C2—C3—C4—C51 (2)C26—C27—C28—C291 (2)
C3—C4—C5—N11 (2)C27—C28—C29—C302 (2)
C3—C4—C5—C6178.7 (12)C28—C29—C30—N42.7 (19)
N1—C5—C6—N26.1 (17)N8—C31—C32—C330 (2)
N1—C5—C6—C7173.7 (12)C31—C32—C33—C341 (2)
C4—C5—C6—N2174.2 (13)C32—C33—C34—C352 (2)
C4—C5—C6—C76.0 (19)C33—C34—C35—N80.1 (19)
N2—C6—C7—C81 (2)C33—C34—C35—C36179.1 (12)
C5—C6—C7—C8178.8 (13)N8—C35—C36—N72.2 (16)
C6—C7—C8—C91 (2)N8—C35—C36—C37177.8 (11)
C7—C8—C9—C101 (2)C34—C35—C36—N7178.8 (11)
C8—C9—C10—N21 (2)C34—C35—C36—C371.2 (19)
C8—C9—C10—C11176.2 (14)N7—C36—C37—C382.0 (17)
N2—C10—C11—N33.4 (18)C35—C36—C37—C38178.0 (10)
N2—C10—C11—C12175.0 (12)C36—C37—C38—C37ii1.0 (15)
C9—C10—C11—N3171.8 (13)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3···O4iii0.952.573.263 (17)130
C3—H3···O9iv0.952.573.101 (19)116
C13—H13···O5v0.952.483.061 (18)120
C14—H14···O8vi0.952.443.104 (16)126
C15—H15···O30.952.483.292 (17)144
C16—H16···O20i0.952.403.213 (16)144
C17—H17···O10iii0.952.413.107 (16)130
C22—H22···O14vii0.952.573.382 (19)144
C31—H31···O16ii0.952.563.349 (17)141
C37—H37···O18viii0.952.543.317 (17)139
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1/2; (iii) x, y+1, z1/2; (iv) x+1/2, y+3/2, z; (v) x+1/2, y+1/2, z+1/2; (vi) x, y+1, z+1/2; (vii) x+1/2, y+1/2, z; (viii) x+1/2, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Pb(ClO4)2(C15H11N3)]
Mr639.36
Crystal system, space groupMonoclinic, C2/c
Temperature (K)150
a, b, c (Å)25.440 (4), 16.333 (3), 21.916 (4)
β (°) 98.671 (2)
V3)9002 (4)
Z20
Radiation typeMo Kα
µ (mm1)9.72
Crystal size (mm)0.25 × 0.08 × 0.05
Data collection
DiffractometerBruker SMART APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.514, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
27358, 8832, 4705
Rint0.052
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.126, 1.03
No. of reflections8832
No. of parameters655
No. of restraints220
H-atom treatmentH-atom parameters constrained
w = 1/[σ^2^(Fo^2^) + (0.027P)^2^ + 69.73P]
where P = (Fo^2^ + 2Fc^2^)/3
Δρmax, Δρmin (e Å3)2.07, 2.43

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), enCIFer (Allen et al., 2004), PLATON (Spek, 2003), publCIF (Westrip, 2008).

Selected geometric parameters (Å, º) top
Pb1—O32.980 (11)Pb2—O192.547 (8)
Pb1—O62.987 (11)Pb2—O20i2.975 (9)
Pb1—O92.598 (10)Pb2—N42.540 (9)
Pb1—O132.532 (10)Pb2—N52.502 (11)
Pb1—N12.511 (9)Pb2—N62.501 (9)
Pb1—N22.494 (8)Pb3—O12.548 (10)
Pb1—N32.506 (10)Pb3—O162.969 (11)
Pb2—O52.626 (10)Pb3—N72.499 (15)
Pb2—O123.024 (11)Pb3—N82.519 (9)
O9—Pb1—O13148.8 (4)Pb1—O9—Cl3116.9 (6)
O5—Pb2—O19148.1 (3)Pb2—O12—Cl3110.1 (6)
O1—Pb3—O1ii152.7 (4)Pb1—O13—Cl4122.0 (5)
Pb3—O1—Cl1118.8 (5)Pb3—O16—Cl4125.7 (6)
Pb1—O3—Cl1129.4 (6)Pb2—O19—Cl5121.4 (4)
Pb2—O5—Cl2114.7 (5)Pb2—O20i—Cl5i134.7 (5)
Pb1—O6—Cl2114.0 (6)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z+1/2.
 

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