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Lead fluoride iodide adopts the matlockite (PbFCl) structure type and is isotypic with other fluoride halides MFX (M = Ca, Sr, Ba, Sm, Eu, Pb; X = Cl, Br, I). The Pb and I atoms are situated on positions with site symmetry 4mm and the F atom on a position with site symmetry \overline 4m2. The Pb atom is surrounded by four F atoms and four I atoms at the vertices of a square antiprism with distances of d(Pb-F) = 2.5631 (5) Å and d(Pb-I) = 3.3613 (7) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801013678/bt6076sup1.cif
Contains datablocks I, PbFI

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801013678/bt6076Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Pb-F) = 0.001 Å
  • R factor = 0.041
  • wR factor = 0.098
  • Data-to-parameter ratio = 16.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.107 PLAT_030 Alert C Refined Extinction parameter within range .... 2.67 Sigma PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio PB -PB 1.555 1.655 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio PB -PB 1.555 1.455 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio PB -PB 1.555 1.565 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio PB -PB 1.555 1.545 PLAT_731 Alert C Bond Calc 4.9523(11), Rep 4.9523(4) .... 2.75 s.u-Ratio PB -F 1.555 9.555 PLAT_731 Alert C Bond Calc 4.9523(11), Rep 4.9523(4) .... 2.75 s.u-Ratio PB -F 1.555 1.445 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio I -I 1.555 1.565 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio I -I 1.555 1.655 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio I -I 1.555 1.455 PLAT_731 Alert C Bond Calc 4.2374(10), Rep 4.2374(3) .... 3.33 s.u-Ratio I -I 1.555 1.545 PLAT_731 Alert C Bond Calc 4.9523(11), Rep 4.9523(4) .... 2.75 s.u-Ratio F -PB 1.555 9.555 PLAT_731 Alert C Bond Calc 4.9523(11), Rep 4.9523(4) .... 2.75 s.u-Ratio F -PB 1.555 1.665 PLAT_731 Alert C Bond Calc 4.9523(11), Rep 4.9523(4) .... 2.75 s.u-Ratio F -PB 1.555 1.545 PLAT_731 Alert C Bond Calc 4.9523(11), Rep 4.9523(4) .... 2.75 s.u-Ratio F -PB 1.555 9.765 General Notes
ABSTM_02 The ratio of expected to reported Tmax/Tmin(RR) is > 2.00 Tmin and Tmax reported: 0.023 0.611 Tmin and Tmax expected: 0.000 0.730 RR = 79.809 Please check that your absorption correction is appropriate.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
16 Alert Level C = Please check

Comment top

Compounds of the matlockite (PbFCl) structure type are technologically interesting materials. For example, Sm2+– or Eu2+-doped BaFX (X = Cl, Br, I) crystals are well established optical luminophores (Takahashi et al., 1985) or can be used as X-ray phosphors in imaging plate systems (Tanaka et al., 1990; Sato et al., 1992). Many isotypic representatives MFX of divalent lead, the larger alkaline earth ions (M = Ca, Sr, Ba) and of stable divalent rare earth elements (M = Sm, Eu) have been synthesized in the past and their structures determined from single-crystal or powder data.

Focusing on the system PbFX, the structures of PbFCl (Nieuwenkamp & Bijvoet, 1932a) and PbFBr (Nieuwenkamp & Bijvoet, 1932b) were the first to be characterized by X-ray diffraction techniques within this structure family. Synthesis and lattice parameters of microcrystalline PbFI have already been described by Rulmont (1973) and Aurivillius (1976), but no structure parameters of this compound were published up to now, although high quality powder refinements had been previously performed (Haberkorn, 1988).

The crystal structure of PbFI consists of a lattice of alternating coplanar layers with a sequence I–Pb–F–Pb–I–(I–Pb–F–Pb–I)- -extending along [001] (Fig. 1). The coordination polyhedron around the Pb atom is a square antiprism with four short Pb—F bonds and four longer Pb—I bonds (Fig. 2). In contrast to the other lead halide fluorides, PbFCl and PbFBr, where an appreciable interaction between the metal atom and the neighbouring halide layers was observed (and which results in a [4 + 4+1] coordination with a monocapped square antiprism as corresponding coordination figure) only very weak interactions between the Pb atom and the more distant iodine layers [d(Pb—I) ca 4.4 Å] can be found. Between two adjacent iodine layers [distance layer-layer = 2.8681 Å, d(I—I) within a layer = 4.2374 (3) Å, d(I—I) between two I atoms of different layers = 4.1478 (17) Å] only van der Waals interactions stabilize the structure. This corresponds to the very easy cleavage of the crystals along [001].

The presented single-crystal results are in good agreement with the results obtained from powder data (Haberkorn, 1988).

Experimental top

Single crystals of PbFI were synthesized under hydrothermal conditions, starting from stoichiometric amounts of PbI2 (Riedel-de Haën, pure) and PbF2 (Aldrich, 99+%). The materials were homogenized by grinding and filled in a 5 ml teflon inlay which was two-thirds filled with demineralized water. The teflon inlay then was closed, placed in a steel autoclave and heated in a laboratory furnace. The heating rate was 298 523 K [2 h], 523 K [10 d], 523 298 K [10 h]. Very thin crystals with plate-like habit and light yellow colour of the title compound were obtained. Microcrystalline samples of PbFI were prepared by reaction of PbI2 and PbF2 in sealed and evacuated silica ampoules at 653 K for one week.

Computing details top

Data collection: PW1100 Operation Software (Philips, 1980); cell refinement: PW1100 Operation Software; data reduction: PW1100 Operation Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS for Windows (Dowty, 1998); software used to prepare material for publication: SHELX97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. Projection of the structure along [100]. The stacking sequence of coplanar layers along [001] is given. Weaker interactions between Pb and I atoms of neighbouring layers are denoted with dashed lines.
[Figure 2] Fig. 2. Coordination around the Pb atom (yellow) with anisotropic displacement ellipsoids drawn at the 99% probability level. F atoms are blue and I atoms are purple.
Lead(II) fluoride iodide top
Crystal data top
PbFIDx = 7.422 Mg m3
Mr = 353.09Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/nmmCell parameters from 21 reflections
a = 4.2374 (3) Åθ = 6.8–21.8°
c = 8.800 (2) ŵ = 62.89 mm1
V = 158.00 (4) Å3T = 293 K
Z = 2Plate, light yellow
F(000) = 2880.17 × 0.15 × 0.01 mm
Data collection top
Philips PW1100
diffractometer
143 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.107
Graphite monochromatorθmax = 29.5°, θmin = 4.6°
θ/2θ scansh = 55
Absorption correction: numerical
(SHELXTL; Siemens, 1995)
k = 55
Tmin = 0.023, Tmax = 0.611l = 1212
1724 measured reflections3 standard reflections every 120 min
162 independent reflections intensity decay: none
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)] = 0.041 w = 1/[σ2(Fo2) + (0.0613P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.098(Δ/σ)max < 0.001
S = 1.13Δρmax = 5.98 e Å3
162 reflectionsΔρmin = 2.37 e Å3
10 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.008 (3)
Crystal data top
PbFIZ = 2
Mr = 353.09Mo Kα radiation
Tetragonal, P4/nmmµ = 62.89 mm1
a = 4.2374 (3) ÅT = 293 K
c = 8.800 (2) Å0.17 × 0.15 × 0.01 mm
V = 158.00 (4) Å3
Data collection top
Philips PW1100
diffractometer
143 reflections with I > 2σ(I)
Absorption correction: numerical
(SHELXTL; Siemens, 1995)
Rint = 0.107
Tmin = 0.023, Tmax = 0.6113 standard reflections every 120 min
1724 measured reflections intensity decay: none
162 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04110 parameters
wR(F2) = 0.0980 restraints
S = 1.13Δρmax = 5.98 e Å3
162 reflectionsΔρmin = 2.37 e Å3
Special details top

Experimental. the measured distances of indexed crystal faces have been used for numerical absorption correction using the program SHELXTL (Siemens, 1995).

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb0.25000.25000.16392 (9)0.0225 (5)
I0.25000.25000.66297 (13)0.0177 (5)
F0.75000.25000.00000.022 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb0.0178 (5)0.0178 (5)0.0318 (7)0.0000.0000.000
I0.0147 (5)0.0147 (5)0.0237 (8)0.0000.0000.000
F0.017 (3)0.017 (3)0.032 (6)0.0000.0000.000
Geometric parameters (Å, º) top
Pb—Fi2.5631 (5)I—Fxv3.6448 (11)
Pb—Fii2.5631 (5)I—Fvii3.6448 (11)
Pb—Fiii2.5631 (5)I—Fxvi3.6448 (11)
Pb—F2.5631 (5)I—Iv4.1478 (17)
Pb—Iiv3.3613 (7)I—Ivi4.1478 (17)
Pb—Iv3.3613 (7)I—Ivii4.1478 (17)
Pb—Ivi3.3613 (7)I—Iiv4.1478 (17)
Pb—Ivii3.3613 (7)I—Ixi4.2374 (3)
Pb—Pbviii4.1594 (12)I—Ix4.2374 (3)
Pb—Pbix4.1594 (12)I—Iii4.2374 (3)
Pb—Pbi4.1594 (12)I—Ixii4.2374 (3)
Pb—Pbiii4.1594 (12)I—Pbxv4.4082 (18)
Pb—Pbx4.2374 (3)I—Fxvii5.5893 (8)
Pb—Pbii4.2374 (3)I—Fxviii5.5893 (8)
Pb—Pbxi4.2374 (3)F—Pbi2.5631 (5)
Pb—Pbxii4.2374 (3)F—Pbx2.5631 (5)
Pb—I4.3915 (18)F—Pbiii2.5631 (5)
Pb—Ixiii4.4082 (18)F—Iiv3.6448 (11)
Pb—Fviii4.9523 (4)F—Ixiii3.6448 (11)
Pb—Fxiv4.9523 (4)F—Ivii3.6448 (11)
I—Pbiv3.3613 (7)F—Ixix3.6448 (11)
I—Pbv3.3613 (7)F—Pbviii4.9523 (4)
I—Pbvi3.3613 (7)F—Pbxx4.9523 (4)
I—Pbvii3.3613 (7)F—Pbxii4.9523 (4)
I—Fiv3.6448 (11)F—Pbxxi4.9523 (4)
Fi—Pb—Fii71.535 (15)Fxv—I—Iv149.271 (15)
Fi—Pb—Fiii111.50 (3)Fvii—I—Iv105.411 (17)
Fii—Pb—Fiii71.535 (15)Fxvi—I—Iv105.411 (17)
Fi—Pb—F71.535 (15)Pbiv—I—Ivi108.263 (10)
Fii—Pb—F111.50 (3)Pbv—I—Ivi108.263 (10)
Fiii—Pb—F71.535 (15)Pbvi—I—Ivi70.697 (19)
Fi—Pb—Iiv140.903 (8)Pbvii—I—Ivi163.20 (4)
Fii—Pb—Iiv140.903 (8)Fiv—I—Ivi105.411 (18)
Fiii—Pb—Iiv74.574 (17)Fxv—I—Ivi149.271 (15)
F—Pb—Iiv74.574 (17)Fvii—I—Ivi149.271 (15)
Fi—Pb—Iv74.574 (18)Fxvi—I—Ivi105.411 (17)
Fii—Pb—Iv74.574 (18)Iv—I—Ivi61.43 (3)
Fiii—Pb—Iv140.903 (8)Pbiv—I—Ivii108.263 (10)
F—Pb—Iv140.903 (8)Pbv—I—Ivii108.263 (10)
Iiv—Pb—Iv126.10 (4)Pbvi—I—Ivii163.20 (4)
Fi—Pb—Ivi140.903 (8)Pbvii—I—Ivii70.697 (19)
Fii—Pb—Ivi74.574 (18)Fiv—I—Ivii149.271 (15)
Fiii—Pb—Ivi74.574 (18)Fxv—I—Ivii105.411 (18)
F—Pb—Ivi140.903 (8)Fvii—I—Ivii105.411 (18)
Iiv—Pb—Ivi78.149 (18)Fxvi—I—Ivii149.271 (15)
Iv—Pb—Ivi78.149 (18)Iv—I—Ivii61.43 (3)
Fi—Pb—Ivii74.574 (18)Ivi—I—Ivii92.50 (5)
Fii—Pb—Ivii140.903 (8)Pbiv—I—Iiv70.697 (19)
Fiii—Pb—Ivii140.903 (8)Pbv—I—Iiv163.20 (4)
F—Pb—Ivii74.574 (18)Pbvi—I—Iiv108.263 (10)
Iiv—Pb—Ivii78.149 (18)Pbvii—I—Iiv108.263 (10)
Iv—Pb—Ivii78.149 (18)Fiv—I—Iiv105.411 (18)
Ivi—Pb—Ivii126.10 (4)Fxv—I—Iiv105.411 (18)
Fi—Pb—Pbviii35.768 (8)Fvii—I—Iiv149.271 (15)
Fii—Pb—Pbviii35.768 (8)Fxvi—I—Iiv149.271 (15)
Fiii—Pb—Pbviii91.76 (3)Iv—I—Iiv92.50 (5)
F—Pb—Pbviii91.76 (3)Ivi—I—Iiv61.43 (3)
Iiv—Pb—Pbviii163.03 (3)Ivii—I—Iiv61.43 (3)
Iv—Pb—Pbviii70.86 (2)Pbiv—I—Ixi50.926 (9)
Ivi—Pb—Pbviii108.320 (13)Pbv—I—Ixi129.074 (9)
Ivii—Pb—Pbviii108.320 (13)Pbvi—I—Ixi50.926 (9)
Fi—Pb—Pbix91.76 (3)Pbvii—I—Ixi129.074 (9)
Fii—Pb—Pbix35.768 (8)Fiv—I—Ixi54.458 (13)
Fiii—Pb—Pbix35.768 (8)Fxv—I—Ixi90.0
F—Pb—Pbix91.76 (3)Fvii—I—Ixi125.542 (13)
Iiv—Pb—Pbix108.320 (13)Fxvi—I—Ixi90.0
Iv—Pb—Pbix108.320 (13)Iv—I—Ixi120.717 (14)
Ivi—Pb—Pbix70.86 (2)Ivi—I—Ixi59.283 (14)
Ivii—Pb—Pbix163.03 (3)Ivii—I—Ixi120.717 (14)
Pbviii—Pb—Pbix61.244 (19)Iiv—I—Ixi59.283 (14)
Fi—Pb—Pbi35.768 (8)Pbiv—I—Ix50.926 (9)
Fii—Pb—Pbi91.76 (3)Pbv—I—Ix129.074 (9)
Fiii—Pb—Pbi91.76 (3)Pbvi—I—Ix129.074 (9)
F—Pb—Pbi35.768 (8)Pbvii—I—Ix50.926 (9)
Iiv—Pb—Pbi108.320 (13)Fiv—I—Ix90.0
Iv—Pb—Pbi108.320 (13)Fxv—I—Ix54.458 (13)
Ivi—Pb—Pbi163.03 (3)Fvii—I—Ix90.0
Ivii—Pb—Pbi70.86 (2)Fxvi—I—Ix125.542 (13)
Pbviii—Pb—Pbi61.244 (19)Iv—I—Ix120.717 (14)
Pbix—Pb—Pbi92.17 (3)Ivi—I—Ix120.717 (14)
Fi—Pb—Pbiii91.76 (3)Ivii—I—Ix59.283 (14)
Fii—Pb—Pbiii91.76 (3)Iiv—I—Ix59.283 (14)
Fiii—Pb—Pbiii35.768 (8)Ixi—I—Ix90.0
F—Pb—Pbiii35.768 (8)Pbiv—I—Iii129.074 (9)
Iiv—Pb—Pbiii70.86 (2)Pbv—I—Iii50.926 (9)
Iv—Pb—Pbiii163.03 (3)Pbvi—I—Iii50.926 (9)
Ivi—Pb—Pbiii108.320 (13)Pbvii—I—Iii129.074 (9)
Ivii—Pb—Pbiii108.320 (13)Fiv—I—Iii90.0
Pbviii—Pb—Pbiii92.17 (3)Fxv—I—Iii125.542 (13)
Pbix—Pb—Pbiii61.244 (19)Fvii—I—Iii90.0
Pbi—Pb—Pbiii61.244 (19)Fxvi—I—Iii54.458 (13)
Fi—Pb—Pbx90.0Iv—I—Iii59.283 (14)
Fii—Pb—Pbx145.752 (16)Ivi—I—Iii59.283 (14)
Fiii—Pb—Pbx90.0Ivii—I—Iii120.717 (14)
F—Pb—Pbx34.248 (16)Iiv—I—Iii120.717 (14)
Iiv—Pb—Pbx50.926 (9)Ixi—I—Iii90.0
Iv—Pb—Pbx129.074 (9)Ix—I—Iii180.00 (6)
Ivi—Pb—Pbx129.074 (9)Pbiv—I—Ixii129.074 (9)
Ivii—Pb—Pbx50.926 (9)Pbv—I—Ixii50.926 (9)
Pbviii—Pb—Pbx120.622 (10)Pbvi—I—Ixii129.074 (9)
Pbix—Pb—Pbx120.622 (10)Pbvii—I—Ixii50.926 (9)
Pbi—Pb—Pbx59.378 (10)Fiv—I—Ixii125.542 (13)
Pbiii—Pb—Pbx59.378 (10)Fxv—I—Ixii90.0
Fi—Pb—Pbii90.0Fvii—I—Ixii54.458 (13)
Fii—Pb—Pbii34.248 (16)Fxvi—I—Ixii90.0
Fiii—Pb—Pbii90.0Iv—I—Ixii59.283 (14)
F—Pb—Pbii145.752 (16)Ivi—I—Ixii120.717 (14)
Iiv—Pb—Pbii129.074 (9)Ivii—I—Ixii59.283 (14)
Iv—Pb—Pbii50.926 (9)Iiv—I—Ixii120.717 (14)
Ivi—Pb—Pbii50.926 (9)Ixi—I—Ixii180.00 (6)
Ivii—Pb—Pbii129.074 (9)Ix—I—Ixii90.0
Pbviii—Pb—Pbii59.378 (10)Iii—I—Ixii90.0
Pbix—Pb—Pbii59.378 (10)Pbiv—I—Pb116.95 (2)
Pbi—Pb—Pbii120.622 (10)Pbv—I—Pb116.95 (2)
Pbiii—Pb—Pbii120.622 (10)Pbvi—I—Pb116.95 (2)
Pbx—Pb—Pbii180.00 (4)Pbvii—I—Pb116.95 (2)
Fi—Pb—Pbxi145.752 (16)Fiv—I—Pb144.458 (13)
Fii—Pb—Pbxi90.0Fxv—I—Pb144.458 (13)
Fiii—Pb—Pbxi34.248 (16)Fvii—I—Pb144.458 (13)
F—Pb—Pbxi90.0Fxvi—I—Pb144.458 (13)
Iiv—Pb—Pbxi50.926 (9)Iv—I—Pb46.25 (2)
Iv—Pb—Pbxi129.074 (9)Ivi—I—Pb46.25 (2)
Ivi—Pb—Pbxi50.926 (9)Ivii—I—Pb46.25 (2)
Ivii—Pb—Pbxi129.074 (9)Iiv—I—Pb46.25 (2)
Pbviii—Pb—Pbxi120.622 (10)Ixi—I—Pb90.0
Pbix—Pb—Pbxi59.378 (10)Ix—I—Pb90.0
Pbi—Pb—Pbxi120.622 (10)Iii—I—Pb90.0
Pbiii—Pb—Pbxi59.378 (10)Ixii—I—Pb90.0
Pbx—Pb—Pbxi90.0Pbiv—I—Pbxv63.05 (2)
Pbii—Pb—Pbxi90.0Pbv—I—Pbxv63.05 (2)
Fi—Pb—Pbxii34.248 (16)Pbvi—I—Pbxv63.05 (2)
Fii—Pb—Pbxii90.0Pbvii—I—Pbxv63.05 (2)
Fiii—Pb—Pbxii145.752 (16)Fiv—I—Pbxv35.542 (13)
F—Pb—Pbxii90.0Fxv—I—Pbxv35.542 (13)
Iiv—Pb—Pbxii129.074 (9)Fvii—I—Pbxv35.542 (13)
Iv—Pb—Pbxii50.926 (9)Fxvi—I—Pbxv35.542 (13)
Ivi—Pb—Pbxii129.074 (9)Iv—I—Pbxv133.75 (2)
Ivii—Pb—Pbxii50.926 (9)Ivi—I—Pbxv133.75 (2)
Pbviii—Pb—Pbxii59.378 (10)Ivii—I—Pbxv133.75 (2)
Pbix—Pb—Pbxii120.622 (10)Iiv—I—Pbxv133.75 (2)
Pbi—Pb—Pbxii59.378 (10)Ixi—I—Pbxv90.0
Pbiii—Pb—Pbxii120.622 (10)Ix—I—Pbxv90.0
Pbx—Pb—Pbxii90.0Iii—I—Pbxv90.0
Pbii—Pb—Pbxii90.0Ixii—I—Pbxv90.0
Pbxi—Pb—Pbxii180.00 (4)Pb—I—Pbxv180.0
Fi—Pb—I124.248 (16)Pbiv—I—Fxvii16.810 (6)
Fii—Pb—I124.248 (16)Pbv—I—Fxvii118.45 (3)
Fiii—Pb—I124.248 (16)Pbvi—I—Fxvii89.912 (18)
F—Pb—I124.248 (16)Pbvii—I—Fxvii61.354 (11)
Iiv—Pb—I63.05 (2)Fiv—I—Fxvii49.300 (9)
Iv—Pb—I63.05 (2)Fxv—I—Fxvii29.255 (2)
Ivi—Pb—I63.05 (2)Fvii—I—Fxvii77.795 (18)
Ivii—Pb—I63.05 (2)Fxvi—I—Fxvii90.51 (2)
Pbviii—Pb—I133.915 (17)Iv—I—Fxvii161.40 (2)
Pbix—Pb—I133.915 (17)Ivi—I—Fxvii124.093 (6)
Pbi—Pb—I133.915 (17)Ivii—I—Fxvii99.979 (11)
Pbiii—Pb—I133.915 (17)Iiv—I—Fxvii77.646 (19)
Pbx—Pb—I90.0Ixi—I—Fxvii67.724 (3)
Pbii—Pb—I90.0Ix—I—Fxvii40.700 (9)
Pbxi—Pb—I90.0Iii—I—Fxvii139.300 (9)
Pbxii—Pb—I90.0Ixii—I—Fxvii112.276 (3)
Fi—Pb—Ixiii55.752 (16)Pb—I—Fxvii122.047 (12)
Fii—Pb—Ixiii55.752 (16)Pbxv—I—Fxvii57.953 (12)
Fiii—Pb—Ixiii55.752 (16)Pbiv—I—Fxviii16.810 (6)
F—Pb—Ixiii55.752 (16)Pbv—I—Fxviii118.45 (3)
Iiv—Pb—Ixiii116.95 (2)Pbvi—I—Fxviii61.354 (11)
Iv—Pb—Ixiii116.95 (2)Pbvii—I—Fxviii89.912 (18)
Ivi—Pb—Ixiii116.95 (2)Fiv—I—Fxviii29.255 (2)
Ivii—Pb—Ixiii116.95 (2)Fxv—I—Fxviii49.300 (9)
Pbviii—Pb—Ixiii46.085 (17)Fvii—I—Fxviii90.51 (2)
Pbix—Pb—Ixiii46.085 (17)Fxvi—I—Fxviii77.795 (18)
Pbi—Pb—Ixiii46.085 (17)Iv—I—Fxviii161.40 (2)
Pbiii—Pb—Ixiii46.085 (17)Ivi—I—Fxviii99.979 (11)
Pbx—Pb—Ixiii90.0Ivii—I—Fxviii124.093 (5)
Pbii—Pb—Ixiii90.0Iiv—I—Fxviii77.646 (19)
Pbxi—Pb—Ixiii90.0Ixi—I—Fxviii40.700 (9)
Pbxii—Pb—Ixiii90.0Ix—I—Fxviii67.724 (3)
I—Pb—Ixiii180.0Iii—I—Fxviii112.276 (3)
Fi—Pb—Fviii58.831 (5)Ixii—I—Fxviii139.300 (9)
Fii—Pb—Fviii29.401 (2)Pb—I—Fxviii122.047 (12)
Fiii—Pb—Fviii100.936 (14)Pbxv—I—Fxviii57.953 (12)
F—Pb—Fviii122.91 (2)Fxvii—I—Fxviii31.095 (4)
Iiv—Pb—Fviii160.221 (12)Pbi—F—Pbx108.465 (15)
Iv—Pb—Fviii47.390 (19)Pbi—F—Pbiii111.50 (3)
Ivi—Pb—Fviii82.087 (8)Pbx—F—Pbiii108.465 (15)
Ivii—Pb—Fviii113.683 (4)Pbi—F—Pb108.465 (15)
Pbviii—Pb—Fviii31.153 (5)Pbx—F—Pb111.50 (3)
Pbix—Pb—Fviii65.169 (6)Pbiii—F—Pb108.465 (15)
Pbi—Pb—Fviii90.911 (14)Pbi—F—Iiv159.790 (17)
Pbiii—Pb—Fviii116.86 (3)Pbx—F—Iiv62.746 (14)
Pbx—Pb—Fviii148.831 (5)Pbiii—F—Iiv88.71 (2)
Pbii—Pb—Fviii31.169 (5)Pb—F—Iiv62.746 (14)
Pbxi—Pb—Fviii115.329 (1)Pbi—F—Ixiii62.746 (14)
Pbxii—Pb—Fviii64.671 (1)Pbx—F—Ixiii159.790 (17)
I—Pb—Fviii106.934 (9)Pbiii—F—Ixiii62.746 (14)
Ixiii—Pb—Fviii73.066 (9)Pb—F—Ixiii88.71 (2)
Fi—Pb—Fxiv29.401 (2)Iiv—F—Ixiii131.460 (16)
Fii—Pb—Fxiv58.831 (5)Pbi—F—Ivii88.71 (2)
Fiii—Pb—Fxiv122.91 (2)Pbx—F—Ivii62.746 (14)
F—Pb—Fxiv100.936 (14)Pbiii—F—Ivii159.790 (17)
Iiv—Pb—Fxiv160.221 (12)Pb—F—Ivii62.746 (14)
Iv—Pb—Fxiv47.390 (19)Iiv—F—Ivii71.08 (3)
Ivi—Pb—Fxiv113.683 (4)Ixiii—F—Ivii131.460 (16)
Ivii—Pb—Fxiv82.087 (8)Pbi—F—Ixix62.746 (14)
Pbviii—Pb—Fxiv31.153 (5)Pbx—F—Ixix88.71 (2)
Pbix—Pb—Fxiv90.911 (14)Pbiii—F—Ixix62.746 (14)
Pbi—Pb—Fxiv65.169 (6)Pb—F—Ixix159.790 (17)
Pbiii—Pb—Fxiv116.86 (3)Iiv—F—Ixix131.460 (16)
Pbx—Pb—Fxiv115.329 (1)Ixiii—F—Ixix71.08 (3)
Pbii—Pb—Fxiv64.671 (1)Ivii—F—Ixix131.460 (16)
Pbxi—Pb—Fxiv148.831 (5)Pbi—F—Pbviii58.831 (5)
Pbxii—Pb—Fxiv31.169 (5)Pbx—F—Pbviii150.599 (1)
I—Pb—Fxiv106.934 (9)Pbiii—F—Pbviii100.936 (14)
Ixiii—Pb—Fxiv73.066 (9)Pb—F—Pbviii57.09 (2)
Fviii—Pb—Fxiv35.218 (2)Iiv—F—Pbviii119.058 (7)
Pbiv—I—Pbv126.10 (4)Ixiii—F—Pbviii42.744 (11)
Pbiv—I—Pbvi78.149 (18)Ivii—F—Pbviii89.331 (12)
Pbv—I—Pbvi78.149 (18)Ixix—F—Pbviii105.092 (17)
Pbiv—I—Pbvii78.149 (18)Pbi—F—Pbxx150.599 (1)
Pbv—I—Pbvii78.149 (18)Pbx—F—Pbxx58.831 (5)
Pbvi—I—Pbvii126.10 (4)Pbiii—F—Pbxx57.09 (2)
Pbiv—I—Fiv42.679 (13)Pb—F—Pbxx100.936 (14)
Pbv—I—Fiv89.87 (3)Iiv—F—Pbxx42.744 (11)
Pbvi—I—Fiv42.680 (13)Ixiii—F—Pbxx119.058 (7)
Pbvii—I—Fiv89.87 (3)Ivii—F—Pbxx105.092 (17)
Pbiv—I—Fxv42.679 (13)Ixix—F—Pbxx89.331 (12)
Pbv—I—Fxv89.87 (3)Pbviii—F—Pbxx144.782 (2)
Pbvi—I—Fxv89.87 (3)Pbi—F—Pbxii57.09 (2)
Pbvii—I—Fxv42.679 (13)Pbx—F—Pbxii100.936 (14)
Fiv—I—Fxv48.540 (16)Pbiii—F—Pbxii150.599 (2)
Pbiv—I—Fvii89.87 (3)Pb—F—Pbxii58.831 (5)
Pbv—I—Fvii42.680 (13)Iiv—F—Pbxii105.092 (17)
Pbvi—I—Fvii89.87 (3)Ixiii—F—Pbxii89.331 (12)
Pbvii—I—Fvii42.679 (13)Ivii—F—Pbxii42.744 (11)
Fiv—I—Fvii71.08 (3)Ixix—F—Pbxii119.058 (7)
Fxv—I—Fvii48.540 (16)Pbviii—F—Pbxii49.663 (12)
Pbiv—I—Fxvi89.87 (3)Pbxx—F—Pbxii146.131 (19)
Pbv—I—Fxvi42.680 (13)Pbi—F—Pbxxi100.936 (14)
Pbvi—I—Fxvi42.679 (13)Pbx—F—Pbxxi57.09 (2)
Pbvii—I—Fxvi89.87 (3)Pbiii—F—Pbxxi58.831 (5)
Fiv—I—Fxvi48.540 (16)Pb—F—Pbxxi150.599 (2)
Fxv—I—Fxvi71.08 (3)Iiv—F—Pbxxi89.331 (12)
Fvii—I—Fxvi48.540 (16)Ixiii—F—Pbxxi105.092 (17)
Pbiv—I—Iv163.20 (4)Ivii—F—Pbxxi119.058 (7)
Pbv—I—Iv70.697 (19)Ixix—F—Pbxxi42.744 (11)
Pbvi—I—Iv108.263 (10)Pbviii—F—Pbxxi146.131 (19)
Pbvii—I—Iv108.263 (10)Pbxx—F—Pbxxi49.663 (12)
Fiv—I—Iv149.271 (15)Pbxii—F—Pbxxi144.782 (2)
Symmetry codes: (i) x+1, y, z; (ii) x1, y, z; (iii) x+1, y+1, z; (iv) x+1, y+1, z+1; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1, y, z+1; (viii) x, y, z; (ix) x, y+1, z; (x) x+1, y, z; (xi) x, y+1, z; (xii) x, y1, z; (xiii) x, y, z1; (xiv) x1, y1, z; (xv) x, y, z+1; (xvi) x1, y, z+1; (xvii) x+2, y+1, z+1; (xviii) x, y+1, z+1; (xix) x+1, y, z1; (xx) x+1, y+1, z; (xxi) x+2, y+1, z.

Experimental details

Crystal data
Chemical formulaPbFI
Mr353.09
Crystal system, space groupTetragonal, P4/nmm
Temperature (K)293
a, c (Å)4.2374 (3), 8.800 (2)
V3)158.00 (4)
Z2
Radiation typeMo Kα
µ (mm1)62.89
Crystal size (mm)0.17 × 0.15 × 0.01
Data collection
DiffractometerPhilips PW1100
diffractometer
Absorption correctionNumerical
(SHELXTL; Siemens, 1995)
Tmin, Tmax0.023, 0.611
No. of measured, independent and
observed [I > 2σ(I)] reflections
1724, 162, 143
Rint0.107
(sin θ/λ)max1)0.692
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.098, 1.13
No. of reflections162
No. of parameters10
Δρmax, Δρmin (e Å3)5.98, 2.37

Computer programs: PW1100 Operation Software (Philips, 1980), PW1100 Operation Software, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ATOMS for Windows (Dowty, 1998), SHELX97 (Sheldrick, 1997).

Selected bond lengths (Å) top
Pb—Fi2.5631 (5)Pb—I4.3915 (18)
Pb—Iii3.3613 (7)Pb—Iiii4.4082 (18)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z+1; (iii) x, y, z1.
 

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