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Single crystals of lead(II) chloride perrhenate(VII), (I), were obtained from a reaction of PbCl2 and Pb(ReO4)2. Its structure can be considered as an alternation of lead-chlorine slices, [Pb2Cl2]2+, formed of edge-sharing ClPb4 tetra­hedra, and double layers of perrhenate anions, [ReO4-]2. Except for one O atom, all other atoms in (I) are situated on mirror planes. The arrangement is derived from a distorted matlockite (PbFCl) structure by replacing F with Cl, and introducing the ReO4 group instead of Cl. The structure of (I) is the first PbFCl derivative containing tetra­hedral anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805042613/wm6124sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805042613/wm6124Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](e-O) = 0.014 Å
  • R factor = 0.035
  • wR factor = 0.089
  • Data-to-parameter ratio = 12.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.58
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 28.28 From the CIF: _reflns_number_total 518 Count of symmetry unique reflns 363 Completeness (_total/calc) 142.70% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 155 Fraction of Friedel pairs measured 0.427 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.

Lead(II) perrhenate(VII) chloride top
Crystal data top
PbCl(ReO4)ClF(000) = 412
Mr = 492.84Dx = 6.837 Mg m3
Orthorhombic, Pmn21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac -2Cell parameters from 2115 reflections
a = 5.6800 (3) Åθ = 4.2–32.6°
b = 9.4389 (5) ŵ = 60.82 mm1
c = 4.4656 (2) ÅT = 173 K
V = 239.41 (2) Å3Prism, black
Z = 20.07 × 0.06 × 0.03 mm
Data collection top
Bruker–Nonius X8 Apex CCD area-detector
diffractometer
518 independent reflections
Radiation source: fine-focus sealed tube517 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 25 pixels mm-1θmax = 28.3°, θmin = 5.1°
φ scansh = 77
Absorption correction: numerical
(XPREP in SHELXTL; Bruker, 2004)
k = 1212
Tmin = 0.016, Tmax = 0.163l = 55
1798 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0539P)2 + 0.5031P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.035(Δ/σ)max < 0.001
wR(F2) = 0.089Δρmax = 5.68 e Å3
S = 1.27Δρmin = 2.20 e Å3
518 reflectionsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
41 parametersExtinction coefficient: 0.109 (7)
1 restraintAbsolute structure: Flack (1983), 160 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.07 (2)
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.

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
Re0.00000.13176 (7)0.24821 (17)0.0087 (3)
Pb0.50000.32266 (9)0.2844 (3)0.0198 (4)
Cl0.50000.5359 (5)0.1625 (14)0.0175 (11)
O10.00000.0433 (16)0.143 (4)0.013 (3)
O20.2526 (16)0.2225 (11)0.139 (3)0.021 (3)
O30.00000.133 (2)0.622 (5)0.026 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re0.0099 (4)0.0044 (5)0.0119 (5)0.0000.0000.0009 (5)
Pb0.0271 (5)0.0122 (5)0.0200 (7)0.0000.0000.0005 (5)
Cl0.0196 (19)0.010 (2)0.022 (3)0.0000.0000.003 (2)
O10.017 (4)0.007 (4)0.015 (5)0.0000.0000.004 (4)
O20.015 (4)0.024 (7)0.024 (7)0.006 (4)0.001 (5)0.007 (5)
O30.032 (8)0.015 (8)0.029 (12)0.0000.0000.010 (9)
Geometric parameters (Å, º) top
Re—O31.67 (2)Pb—O2v3.084 (13)
Re—O11.718 (15)Pb—Clvi3.147 (2)
Re—O21.741 (10)Pb—Clvii3.147 (2)
Re—O2i1.741 (10)Pb—Cliv3.186 (6)
Pb—O2ii2.537 (12)Cl—Pbviii3.147 (2)
Pb—O22.537 (12)Cl—Pbix3.147 (2)
Pb—O1iii2.657 (16)Cl—Pbx3.186 (6)
Pb—Cl2.834 (6)O1—Pbxi2.657 (16)
Pb—O2iv3.084 (13)O2—Pbx3.084 (13)
O3—Re—O1106.3 (9)O2v—Pb—Clvi69.9 (2)
O3—Re—O2106.1 (6)O2ii—Pb—Clvii135.6 (3)
O1—Re—O2113.3 (5)O2—Pb—Clvii73.4 (2)
O3—Re—O2i106.1 (6)O1iii—Pb—Clvii114.34 (10)
O1—Re—O2i113.3 (5)Cl—Pb—Clvii75.63 (6)
O2—Re—O2i111.0 (7)O2iv—Pb—Clvii69.9 (2)
O2ii—Pb—O267.3 (5)O2v—Pb—Clvii118.6 (2)
O2ii—Pb—O1iii73.8 (4)Clvi—Pb—Clvii128.95 (17)
O2—Pb—O1iii73.8 (4)O2ii—Pb—Cliv144.4 (2)
O2ii—Pb—Cl75.0 (3)O2—Pb—Cliv144.4 (2)
O2—Pb—Cl75.0 (3)O1iii—Pb—Cliv122.1 (4)
O1iii—Pb—Cl142.3 (4)Cl—Pb—Cliv95.58 (15)
O2ii—Pb—O2iv139.5 (4)O2iv—Pb—Cliv63.0 (2)
O2—Pb—O2iv104.8 (3)O2v—Pb—Cliv63.0 (2)
O1iii—Pb—O2iv66.0 (4)Clvi—Pb—Cliv70.95 (7)
Cl—Pb—O2iv143.7 (2)Clvii—Pb—Cliv70.95 (7)
O2ii—Pb—O2v104.8 (3)Pb—Cl—Pbviii110.75 (11)
O2—Pb—O2v139.5 (4)Pb—Cl—Pbix110.75 (11)
O1iii—Pb—O2v66.0 (4)Pbviii—Cl—Pbix128.95 (17)
Cl—Pb—O2v143.7 (2)Pb—Cl—Pbx95.58 (15)
O2iv—Pb—O2v54.2 (4)Pbviii—Cl—Pbx102.10 (12)
O2ii—Pb—Clvi73.4 (2)Pbix—Cl—Pbx102.10 (12)
O2—Pb—Clvi135.6 (3)Re—O1—Pbxi157.1 (9)
O1iii—Pb—Clvi114.32 (10)Re—O2—Pb148.1 (7)
Cl—Pb—Clvi75.63 (6)Re—O2—Pbx106.9 (6)
O2iv—Pb—Clvi118.6 (2)Pb—O2—Pbx104.8 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x+1/2, y, z1/2; (iv) x, y, z1; (v) x+1, y, z1; (vi) x+3/2, y+1, z1/2; (vii) x+1/2, y+1, z1/2; (viii) x+3/2, y+1, z+1/2; (ix) x+1/2, y+1, z+1/2; (x) x, y, z+1; (xi) x+1/2, y, z+1/2.
 

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