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The title compound, {(C9H14N)4[Pb3I10]}n, crystallizes as an organic–inorganic hybrid. As such, the structure consists of a two-dimensional inorganic layer of [Pb3I10]n4n ions extending along [100]. The asymmetric unit contains two independent Pb atoms, viz. one in a general position and the other on an inversion centre. Each Pb atom is octa­hedrally coordinated by six iodide ions and exhibits both face- and corner-sharing with adjacent atoms in the inorganic layer. These anionic layers alternate with 3-phenyl­propyl­ammonium cations, which hydrogen bond to the iodides. Simple face-to-edge σ–π stacking inter­actions are observed between the aromatic rings that stabilize the overall three-dimensional structure. This net structure has only been observed five times previously.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106009127/fg3008sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106009127/fg3008Isup2.hkl
Contains datablock I

CCDC reference: 609394

Comment top

In recent years, a significant number of organic–inorganic hybrid materials based on lead and tin halide units have been prepared and studied. For reviews see Papavassiliou (1997) and Mitzi (1999 or? 2001). Haloplumbates in particular have demonstrated a propensity for forming a great variety of crystalline structures. This diversity is a result of the metal–halide octahedra joining in different combinations of face-, edge- and corner-sharing octahedra. As a result, the MX6 (X = Br and I, and M = Sn and Pb) octahedra building blocks become severely distorted. One of the possible structural motifs forms two-dimensional layers, where chains of two or three trans face-sharing octahedra are connected via four halides on both ends. This can be summarized by the formula (MnX3n + 1)(n + 1)-. To our knowledge, only one structure with n = 2 has been reported, which has isolated I anions between the lead iodide layers (Krautscheid et al., 1998).

The case with n = 3 has been observed with both lead bromide in [PhMe3N]4[Pb3Br10] (Wiest et al., 1999) and tin iodide [PhMe3N]4[Sn3I10] (Lode & Krautscheid, 2001). We present here the synthesis and crystal structure of the n = 3 case that has [Pb3I10]4− two-dimensional layers separated by the cation C6H5C3H6NH3+.

The atomic numbering scheme of (I) is shown in Fig. 1. The building block [Pb3I10]4− has two crystallographically independent Pb atoms, Pb1 and Pb2. Pb2 is the central Pb atom and sits on an inversion centre through which the third Pb atom, Pb1(−x + 3/2, y + 1/2, z), is generated to complete the simplest repeating unit. The three Pb atoms are connected by sharing trans faces made up of µ2-I bridges, with atoms I3, I4 and I5 and their inversion equivalents related through Pb2. The outer octahedra on either end connect to adjacent [Pb3I10]4− units via I2 µ2 bridges which are far from linear [Pb1i—I2—Pb1 = 142.51 (3)°], in contrast to the almost linear bridges found in [Sn3I10]4− with an angle of 169.87 (3)° (Lode & Krautscheid, 2001) (see Fig. 2). The resulting inorganic layer sits in the ab plane and is corrugated as the trimeric units connect in an alternating trans fashion (see Fig. 3) as seen in [C6H5NH3]4[Cd3Br10] (Ishihara et al., 1994) and [C6H5CH2SC(NH2)2]4[Pb3I10] (Raptopoulou et al., 2002). The other two n = 3 structures mentioned above have the individual building blocks cis related.

The Pb atoms show different degrees of distortion. The central Pb2 atom has three almost equal bond lengths to the I atoms with bond lengths of 3.2006 (7)–3.2090 (7) Å. This uniformity is due to the identical face-sharing that occurs with the neighbouring Pb1 atoms. The outer Pb1 octahedra are more distorted, with long Pb—I bond lengths of 3.2288 (8)–3.3381 (9) Å when the I atoms are involved in face-sharing and short bond lengths to the corner-sharing iodide I2 and the terminal non-bridging I1 (see Table 1).

Sandwiched between the inorganic nets are two unique organic aromatic amines, cat1 and cat2. Fig. 3 clearly shows the bidimemsional arrangement of the cations. Both propylammonium groups have an all-trans conformation and deviate by 9.3 (11) and 14.2 (11)° from the normal to the aromatic rings, respectively. The two ammonium groups display the same hydrogen-bonding scheme, viz. one bifurcated and two normal hydrogen bonds. The bifurcated bond distances are similiar for atoms N1 and N2 as they both bond to atoms I4 (2.95 and 2.94 Å) and I2 (3.11 and 3.07 Å). Atom N1 has a long hydrogen bond and a short normal hydrogen bond (2.95 and 2.66 Å) as it bonds to an equatorial (I3) and axial (I5) I atom, respectively. Atom N2, however, has two similiar hydrogen bonds (2.82 and 2.84 Å) as they both bond to the axial atom I1, which is not involved in any bridging (see Fig. 4).

Between the aromatic rings of cat1 and cat2, a face-to-edge σπ interaction, C14—H14···Cg1(1 − x,1 − y,1 − z), occurs with a distance of 2.920 Å and an angle of 143.00°. This interaction is between two cations that hydrogen bond to adjacent two-dimensional nets and so form a three-dimensional system (see Fig. 3).

Experimental top

PbO (0.184 g, 0.824 mmol) and C6H5C3H6NH2 (0.167 g, 1.23 mmol) were dissolved in HI (3 ml) and then heated to form a clear solution. Upon slow cooling to room temperature, yellow crystals formed. A single-crystal suitable for X-ray diffraction was selected and mounted on a glass fibre. Analysis calculated for C36H56I10N4Pb3: C 17.75, H 2.32, N 2.30%; found: C 18.96, H 2.55, N 2.55%.

Refinement top

All H atoms were refined in idealized positions in the riding-model approximation, with their Uiso values fixed to 1.2Ueq of the atom to which they are bonded.

Computing details top

Data collection: SMART-NT (Bruker, 1998); cell refinement: SMART-NT; data reduction: SAINT-Plus (Bruker, 1999) and SHELXTL (Bruker, 1997); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I) and some adjacent atoms, showing the atomic numbering scheme. Displacement ellipsoids are shown at the 50% probability level. Atoms labelled with superscript a are at the symmetry position (−x, −y, −z).
[Figure 2] Fig. 2. Fiure 2. An illustration of the [Pb3I10]n4n two-dimensional net.
[Figure 3] Fig. 3. Packing diagram of (I) viewed along the b axis. Solid lines show the face-to-edge σπ interaction between cat1 and cat2 which forms a three-dimensional system.
[Figure 4] Fig. 4. Hydrogen bridging interactions (dashed lines) between the ammonium heads and the halogen atoms of (I).
catena-Poly[tetrakis(3-phenylpropylammonium) [iodoplumbate(II)-tri-µ-iodo-plumbate(II)-tri-µ-iodo- iodoplumbate(II)-di-µ-iodo]] top
Crystal data top
(C9H14N)4[Pb3I10]F(000) = 4304
Mr = 2435.42Dx = 2.74 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 903 reflections
a = 20.777 (3) Åθ = 4.6–56.5°
b = 8.4689 (11) ŵ = 13.79 mm1
c = 33.550 (5) ÅT = 173 K
V = 5903.3 (14) Å3Rectangular block, yellow
Z = 40.37 × 0.21 × 0.07 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
5479 reflections with I > 2σ(I)
ϕ and ω scansRint = 0.075
Absorption correction: integration
?
θmax = 28°, θmin = 1.6°
Tmin = 0.073, Tmax = 0.393h = 2727
27663 measured reflectionsk = 1011
7120 independent reflectionsl = 4430
Refinement top
Refinement on F2162 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.049 w = 1/[σ2(Fo2) + (0.0228P)2 + 63.008P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.094(Δ/σ)max = 0.001
S = 1.14Δρmax = 1.49 e Å3
7120 reflectionsΔρmin = 2.10 e Å3
217 parameters
Crystal data top
(C9H14N)4[Pb3I10]V = 5903.3 (14) Å3
Mr = 2435.42Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 20.777 (3) ŵ = 13.79 mm1
b = 8.4689 (11) ÅT = 173 K
c = 33.550 (5) Å0.37 × 0.21 × 0.07 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
7120 independent reflections
Absorption correction: integration
?
5479 reflections with I > 2σ(I)
Tmin = 0.073, Tmax = 0.393Rint = 0.075
27663 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.049162 restraints
wR(F2) = 0.094H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0228P)2 + 63.008P]
where P = (Fo2 + 2Fc2)/3
7120 reflectionsΔρmax = 1.49 e Å3
217 parametersΔρmin = 2.10 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.6953 (4)0.3247 (11)0.14757 (17)0.037 (2)
C20.6425 (4)0.2523 (11)0.1653 (2)0.051 (3)
H20.61180.19830.14930.061*
C30.6345 (4)0.2588 (13)0.2064 (2)0.066 (4)
H30.59850.20920.21850.079*
C40.6794 (5)0.3378 (13)0.22978 (17)0.069 (4)
H40.6740.34230.25790.083*
C50.7322 (5)0.4103 (12)0.2121 (3)0.069 (4)
H50.76280.46430.22810.083*
C60.7401 (4)0.4038 (11)0.1710 (3)0.055 (3)
H60.77620.45330.15890.066*
C70.7014 (6)0.3223 (16)0.1033 (3)0.044 (3)
H7A0.69020.21580.09340.053*
H7B0.74660.34420.09590.053*
C80.6569 (5)0.4463 (13)0.0830 (3)0.028 (2)
H8A0.61270.43720.09390.034*
H8B0.67290.55410.08880.034*
C90.6558 (6)0.4191 (14)0.0386 (3)0.038 (2)
H9A0.64650.30660.0330.045*
H9B0.69840.4450.02710.045*
C100.5499 (4)0.6487 (11)0.25952 (18)0.045 (2)
C110.5086 (4)0.5749 (10)0.2863 (2)0.052 (3)
H110.47660.50410.27680.062*
C120.5142 (4)0.6048 (11)0.3269 (2)0.056 (3)
H120.48590.55440.34520.067*
C130.5610 (4)0.7085 (12)0.34071 (18)0.057 (3)
H130.56480.72890.36850.068*
C140.6023 (4)0.7822 (11)0.3140 (3)0.058 (3)
H140.63430.8530.32340.069*
C150.5967 (4)0.7523 (11)0.2734 (2)0.052 (3)
H150.6250.80280.25510.063*
C160.5475 (7)0.6088 (17)0.2156 (4)0.049 (3)
H16A0.50630.55480.20980.058*
H16B0.54850.7080.20.058*
C170.6029 (6)0.5036 (17)0.2021 (3)0.044 (3)
H17A0.59920.39930.21520.053*
H17B0.64420.55170.21030.053*
C180.6025 (6)0.4821 (16)0.1582 (4)0.044 (3)
H18A0.5610.4350.14990.053*
H18B0.60660.58630.14510.053*
N10.6043 (4)0.5228 (11)0.0198 (3)0.032 (2)
H1A0.60380.50670.00710.048*
H1B0.61320.6260.02490.048*
H1C0.56520.49760.03020.048*
N20.6565 (5)0.3776 (12)0.1450 (3)0.040 (2)
H2A0.65520.36630.11810.06*
H2B0.69470.42160.15220.06*
H2C0.65240.28120.15680.06*
I10.67125 (4)0.05002 (10)0.16238 (2)0.03461 (18)
I20.78375 (3)0.11079 (9)0.06215 (2)0.02979 (16)
I30.51744 (3)0.25984 (8)0.06872 (2)0.02690 (15)
I40.55761 (3)0.25593 (8)0.060842 (19)0.02525 (15)
I50.64396 (3)0.06978 (9)0.029021 (18)0.02584 (15)
Pb10.649813 (17)0.06022 (5)0.070380 (11)0.02068 (9)
Pb20.5000.02125 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.042 (5)0.032 (6)0.035 (4)0.002 (4)0.003 (3)0.012 (4)
C20.052 (6)0.064 (8)0.036 (4)0.014 (6)0.004 (4)0.016 (6)
C30.076 (8)0.086 (10)0.036 (5)0.005 (7)0.004 (5)0.024 (6)
C40.107 (10)0.068 (9)0.032 (5)0.017 (7)0.012 (5)0.004 (6)
C50.090 (9)0.055 (9)0.063 (5)0.001 (7)0.035 (6)0.007 (7)
C60.053 (7)0.046 (8)0.065 (5)0.006 (5)0.017 (5)0.009 (6)
C70.046 (6)0.049 (7)0.037 (4)0.024 (5)0.008 (4)0.011 (5)
C80.031 (5)0.022 (5)0.033 (4)0.001 (4)0.003 (4)0.007 (4)
C90.047 (6)0.032 (6)0.035 (4)0.009 (5)0.004 (5)0.008 (5)
C100.044 (6)0.041 (6)0.051 (4)0.001 (4)0.009 (4)0.004 (4)
C110.050 (7)0.049 (7)0.058 (5)0.014 (5)0.018 (5)0.010 (6)
C120.052 (7)0.062 (8)0.054 (5)0.007 (5)0.027 (5)0.002 (6)
C130.055 (7)0.073 (9)0.042 (5)0.001 (6)0.014 (5)0.011 (6)
C140.056 (7)0.057 (8)0.060 (6)0.011 (6)0.008 (5)0.004 (6)
C150.047 (6)0.055 (8)0.055 (5)0.013 (5)0.014 (5)0.003 (6)
C160.049 (6)0.044 (7)0.053 (5)0.007 (5)0.010 (5)0.002 (5)
C170.051 (6)0.045 (7)0.036 (4)0.003 (5)0.001 (5)0.010 (5)
C180.047 (6)0.047 (7)0.039 (5)0.001 (5)0.004 (5)0.004 (5)
N10.041 (5)0.024 (5)0.032 (4)0.004 (4)0.000 (4)0.002 (4)
N20.038 (5)0.042 (6)0.040 (5)0.009 (4)0.006 (4)0.003 (4)
I10.0384 (4)0.0438 (5)0.0216 (3)0.0010 (4)0.0053 (3)0.0004 (3)
I20.0265 (3)0.0268 (4)0.0361 (4)0.0106 (3)0.0042 (3)0.0005 (3)
I30.0206 (3)0.0248 (4)0.0353 (3)0.0036 (3)0.0035 (3)0.0083 (3)
I40.0299 (3)0.0189 (3)0.0269 (3)0.0001 (3)0.0018 (3)0.0042 (3)
I50.0237 (3)0.0270 (4)0.0269 (3)0.0023 (3)0.0032 (2)0.0009 (3)
Pb10.01873 (16)0.01992 (19)0.02340 (17)0.00006 (15)0.00114 (14)0.00033 (16)
Pb20.0195 (2)0.0185 (3)0.0257 (2)0.0013 (2)0.0040 (2)0.0010 (2)
Geometric parameters (Å, º) top
C1—C21.39C14—H140.95
C1—C61.39C15—H150.95
C1—C71.490 (13)C16—C171.523 (18)
C2—C31.39C16—H16A0.99
C2—H20.95C16—H16B0.99
C3—C41.39C17—C181.483 (16)
C3—H30.95C17—H17A0.99
C4—C51.39C17—H17B0.99
C4—H40.95C18—N21.496 (16)
C5—C61.39C18—H18A0.99
C5—H50.95C18—H18B0.99
C6—H60.95N1—H1A0.91
C7—C81.556 (15)N1—H1B0.91
C7—H7A0.99N1—H1C0.91
C7—H7B0.99N2—H2A0.91
C8—C91.508 (15)N2—H2B0.91
C8—H8A0.99N2—H2C0.91
C8—H8B0.99I1—Pb13.1197 (9)
C9—N11.521 (14)I2—Pb1i3.1217 (8)
C9—H9A0.99I2—Pb13.1492 (8)
C9—H9B0.99I3—Pb23.2078 (7)
C10—C111.39I3—Pb13.2288 (8)
C10—C151.39I4—Pb23.2090 (7)
C10—C161.513 (14)I4—Pb13.3077 (8)
C11—C121.39I5—Pb23.2006 (7)
C11—H110.95I5—Pb13.3381 (9)
C12—C131.39Pb1—I2ii3.1217 (8)
C12—H120.95Pb2—I5iii3.2006 (7)
C13—C141.39Pb2—I3iii3.2078 (7)
C13—H130.95Pb2—I4iii3.2090 (7)
C14—C151.39
C2—C1—C6120H16A—C16—H16B107.7
C2—C1—C7119.1 (8)C18—C17—C16111.3 (11)
C6—C1—C7120.8 (8)C18—C17—H17A109.4
C1—C2—C3120C16—C17—H17A109.4
C1—C2—H2120C18—C17—H17B109.4
C3—C2—H2120C16—C17—H17B109.4
C4—C3—C2120H17A—C17—H17B108
C4—C3—H3120C17—C18—N2111.3 (10)
C2—C3—H3120C17—C18—H18A109.4
C5—C4—C3120N2—C18—H18A109.4
C5—C4—H4120C17—C18—H18B109.4
C3—C4—H4120N2—C18—H18B109.4
C4—C5—C6120H18A—C18—H18B108
C4—C5—H5120C9—N1—H1A109.5
C6—C5—H5120C9—N1—H1B109.5
C5—C6—C1120H1A—N1—H1B109.5
C5—C6—H6120C9—N1—H1C109.5
C1—C6—H6120H1A—N1—H1C109.5
C1—C7—C8112.1 (9)H1B—N1—H1C109.5
C1—C7—H7A109.2C18—N2—H2A109.5
C8—C7—H7A109.2C18—N2—H2B109.5
C1—C7—H7B109.2H2A—N2—H2B109.5
C8—C7—H7B109.2C18—N2—H2C109.5
H7A—C7—H7B107.9H2A—N2—H2C109.5
C9—C8—C7109.7 (9)H2B—N2—H2C109.5
C9—C8—H8A109.7Pb1i—I2—Pb1142.51 (3)
C7—C8—H8A109.7Pb2—I3—Pb175.488 (16)
C9—C8—H8B109.7Pb2—I4—Pb174.385 (17)
C7—C8—H8B109.7Pb2—I5—Pb174.076 (15)
H8A—C8—H8B108.2I1—Pb1—I2ii92.82 (2)
C8—C9—N1109.4 (9)I1—Pb1—I287.01 (2)
C8—C9—H9A109.8I2ii—Pb1—I290.685 (15)
N1—C9—H9A109.8I1—Pb1—I398.81 (2)
C8—C9—H9B109.8I2ii—Pb1—I384.71 (2)
N1—C9—H9B109.8I2—Pb1—I3172.73 (2)
H9A—C9—H9B108.2I1—Pb1—I498.97 (2)
C11—C10—C15120I2ii—Pb1—I4165.93 (2)
C11—C10—C16120.6 (7)I2—Pb1—I497.53 (2)
C15—C10—C16119.3 (7)I3—Pb1—I485.92 (2)
C12—C11—C10120I1—Pb1—I5173.87 (2)
C12—C11—H11120I2ii—Pb1—I584.61 (2)
C10—C11—H11120I2—Pb1—I587.460 (19)
C11—C12—C13120I3—Pb1—I586.508 (19)
C11—C12—H12120I4—Pb1—I584.370 (18)
C13—C12—H12120I5—Pb2—I5iii180.00 (3)
C14—C13—C12120I5—Pb2—I3iii90.778 (17)
C14—C13—H13120I5iii—Pb2—I3iii89.222 (17)
C12—C13—H13120I5—Pb2—I389.222 (17)
C15—C14—C13120I5iii—Pb2—I390.778 (17)
C15—C14—H14120I3iii—Pb2—I3180.000 (17)
C13—C14—H14120I5—Pb2—I488.259 (18)
C14—C15—C10120I5iii—Pb2—I491.741 (18)
C14—C15—H15120I3iii—Pb2—I492.06 (2)
C10—C15—H15120I3—Pb2—I487.94 (2)
C10—C16—C17113.3 (11)I5—Pb2—I4iii91.741 (18)
C10—C16—H16A108.9I5iii—Pb2—I4iii88.259 (18)
C17—C16—H16A108.9I3iii—Pb2—I4iii87.94 (2)
C10—C16—H16B108.9I3—Pb2—I4iii92.06 (2)
C17—C16—H16B108.9I4—Pb2—I4iii180.00 (3)
C6—C1—C2—C30Pb2—I3—Pb1—I2ii126.658 (19)
C7—C1—C2—C3177.4 (9)Pb2—I3—Pb1—I275.76 (18)
C1—C2—C3—C40Pb2—I3—Pb1—I442.838 (16)
C2—C3—C4—C50Pb2—I3—Pb1—I541.757 (17)
C3—C4—C5—C60Pb2—I4—Pb1—I1141.383 (19)
C4—C5—C6—C10Pb2—I4—Pb1—I2ii5.23 (9)
C2—C1—C6—C50Pb2—I4—Pb1—I2130.470 (18)
C7—C1—C6—C5177.3 (9)Pb2—I4—Pb1—I343.095 (16)
C2—C1—C7—C878.1 (12)Pb2—I4—Pb1—I543.791 (16)
C6—C1—C7—C899.3 (11)Pb2—I5—Pb1—I1167.4 (2)
C1—C7—C8—C9169.8 (10)Pb2—I5—Pb1—I2ii127.228 (18)
C7—C8—C9—N1171.0 (9)Pb2—I5—Pb1—I2141.84 (2)
C15—C10—C11—C120Pb2—I5—Pb1—I342.219 (18)
C16—C10—C11—C12175.7 (10)Pb2—I5—Pb1—I444.019 (16)
C10—C11—C12—C130Pb1—I5—Pb2—I5iii35 (16)
C11—C12—C13—C140Pb1—I5—Pb2—I3iii137.533 (18)
C12—C13—C14—C150Pb1—I5—Pb2—I342.467 (18)
C13—C14—C15—C100Pb1—I5—Pb2—I445.492 (17)
C11—C10—C15—C140Pb1—I5—Pb2—I4iii134.508 (18)
C16—C10—C15—C14175.8 (10)Pb1—I3—Pb2—I543.897 (18)
C11—C10—C16—C17104.2 (11)Pb1—I3—Pb2—I5iii136.103 (18)
C15—C10—C16—C1771.5 (12)Pb1—I3—Pb2—I3iii0.00 (4)
C10—C16—C17—C18173.8 (11)Pb1—I3—Pb2—I444.389 (17)
C16—C17—C18—N2179.4 (10)Pb1—I3—Pb2—I4iii135.611 (17)
Pb1i—I2—Pb1—I177.26 (5)Pb1—I4—Pb2—I545.940 (17)
Pb1i—I2—Pb1—I2ii170.04 (3)Pb1—I4—Pb2—I5iii134.060 (17)
Pb1i—I2—Pb1—I3139.36 (15)Pb1—I4—Pb2—I3iii136.656 (16)
Pb1i—I2—Pb1—I421.41 (5)Pb1—I4—Pb2—I343.344 (16)
Pb1i—I2—Pb1—I5105.39 (4)Pb1—I4—Pb2—I4iii111.137 (12)
Pb2—I3—Pb1—I1141.30 (2)
Symmetry codes: (i) x+3/2, y1/2, z; (ii) x+3/2, y+1/2, z; (iii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···I40.912.953.655 (9)136
N1—H1A···I2i0.913.113.676 (9)122
N1—H1B···I5iv0.912.663.561 (9)172
N1—H1C···I3iii0.912.953.750 (10)148
N2—H2A···I40.912.943.641 (9)135
N2—H2A···I2i0.913.073.629 (10)122
N2—H2B···I1i0.912.823.677 (9)159
N2—H2C···I10.912.843.680 (11)155
Symmetry codes: (i) x+3/2, y1/2, z; (iii) x+1, y, z; (iv) x, y1, z.

Experimental details

Crystal data
Chemical formula(C9H14N)4[Pb3I10]
Mr2435.42
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)173
a, b, c (Å)20.777 (3), 8.4689 (11), 33.550 (5)
V3)5903.3 (14)
Z4
Radiation typeMo Kα
µ (mm1)13.79
Crystal size (mm)0.37 × 0.21 × 0.07
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionIntegration
Tmin, Tmax0.073, 0.393
No. of measured, independent and
observed [I > 2σ(I)] reflections
27663, 7120, 5479
Rint0.075
(sin θ/λ)max1)0.661
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.094, 1.14
No. of reflections7120
No. of parameters217
No. of restraints162
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0228P)2 + 63.008P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.49, 2.10

Computer programs: SMART-NT (Bruker, 1998), SMART-NT, SAINT-Plus (Bruker, 1999) and SHELXTL (Bruker, 1997), SHELXTL, SHELXL97 (Sheldrick, 1997).

Selected bond lengths (Å) top
C1—C71.490 (13)I2—Pb1i3.1217 (8)
C7—C81.556 (15)I2—Pb13.1492 (8)
C8—C91.508 (15)I3—Pb23.2078 (7)
C9—N11.521 (14)I3—Pb13.2288 (8)
C10—C161.513 (14)I4—Pb23.2090 (7)
C16—C171.523 (18)I4—Pb13.3077 (8)
C17—C181.483 (16)I5—Pb23.2006 (7)
C18—N21.496 (16)I5—Pb13.3381 (9)
I1—Pb13.1197 (9)
Symmetry code: (i) x+3/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···I40.912.953.655 (9)136
N1—H1A···I2i0.913.113.676 (9)122
N1—H1B···I5ii0.912.663.561 (9)172
N1—H1C···I3iii0.912.953.750 (10)148
N2—H2A···I40.912.943.641 (9)135
N2—H2A···I2i0.913.073.629 (10)122
N2—H2B···I1i0.912.823.677 (9)159
N2—H2C···I10.912.843.680 (11)155
Symmetry codes: (i) x+3/2, y1/2, z; (ii) x, y1, z; (iii) x+1, y, z.
 

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