PbCl(ReO₄), a derivative of the matlockite (PbFCl) structure

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.

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

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Computing details

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

Crystal data

PbCl(ReO4)Cl	F(000) = 412
Mr = 492.84	Dx = 6.837 Mg m^−3
Orthorhombic, Pmn21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac -2	Cell parameters from 2115 reflections
a = 5.6800 (3) Å	θ = 4.2–32.6°
b = 9.4389 (5) Å	µ = 60.82 mm^−1
c = 4.4656 (2) Å	T = 173 K
V = 239.41 (2) Å^3	Prism, black
Z = 2	0.07 × 0.06 × 0.03 mm

Data collection

Bruker–Nonius X8 Apex CCD area-detector diffractometer	518 independent reflections
Radiation source: fine-focus sealed tube	517 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
Detector resolution: 25 pixels mm^-1	θmax = 28.3°, θmin = 5.1°
φ scans	h = −7→7
Absorption correction: numerical (XPREP in SHELXTL; Bruker, 2004)	k = −12→12
Tmin = 0.016, Tmax = 0.163	l = −5→5
1798 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0539P)^2 + 0.5031P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.035	(Δ/σ)max < 0.001
wR(F^2) = 0.089	Δρmax = 5.68 e Å^−3
S = 1.27	Δρmin = −2.20 e Å^−3
518 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
41 parameters	Extinction coefficient: 0.109 (7)
1 restraint	Absolute structure: Flack (1983), 160 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.07 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Re	0.0000	0.13176 (7)	0.24821 (17)	0.0087 (3)
Pb	0.5000	0.32266 (9)	−0.2844 (3)	0.0198 (4)
Cl	0.5000	0.5359 (5)	0.1625 (14)	0.0175 (11)
O1	0.0000	−0.0433 (16)	0.143 (4)	0.013 (3)
O2	0.2526 (16)	0.2225 (11)	0.139 (3)	0.021 (3)
O3	0.0000	0.133 (2)	0.622 (5)	0.026 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re	0.0099 (4)	0.0044 (5)	0.0119 (5)	0.000	0.000	0.0009 (5)
Pb	0.0271 (5)	0.0122 (5)	0.0200 (7)	0.000	0.000	−0.0005 (5)
Cl	0.0196 (19)	0.010 (2)	0.022 (3)	0.000	0.000	−0.003 (2)
O1	0.017 (4)	0.007 (4)	0.015 (5)	0.000	0.000	−0.004 (4)
O2	0.015 (4)	0.024 (7)	0.024 (7)	−0.006 (4)	−0.001 (5)	0.007 (5)
O3	0.032 (8)	0.015 (8)	0.029 (12)	0.000	0.000	0.010 (9)

Geometric parameters (Å, º)

Re—O3	1.67 (2)	Pb—O2^v	3.084 (13)
Re—O1	1.718 (15)	Pb—Cl^vi	3.147 (2)
Re—O2	1.741 (10)	Pb—Cl^vii	3.147 (2)
Re—O2^i	1.741 (10)	Pb—Cl^iv	3.186 (6)
Pb—O2^ii	2.537 (12)	Cl—Pb^viii	3.147 (2)
Pb—O2	2.537 (12)	Cl—Pb^ix	3.147 (2)
Pb—O1^iii	2.657 (16)	Cl—Pb^x	3.186 (6)
Pb—Cl	2.834 (6)	O1—Pb^xi	2.657 (16)
Pb—O2^iv	3.084 (13)	O2—Pb^x	3.084 (13)
O3—Re—O1	106.3 (9)	O2^v—Pb—Cl^vi	69.9 (2)
O3—Re—O2	106.1 (6)	O2^ii—Pb—Cl^vii	135.6 (3)
O1—Re—O2	113.3 (5)	O2—Pb—Cl^vii	73.4 (2)
O3—Re—O2^i	106.1 (6)	O1^iii—Pb—Cl^vii	114.34 (10)
O1—Re—O2^i	113.3 (5)	Cl—Pb—Cl^vii	75.63 (6)
O2—Re—O2^i	111.0 (7)	O2^iv—Pb—Cl^vii	69.9 (2)
O2^ii—Pb—O2	67.3 (5)	O2^v—Pb—Cl^vii	118.6 (2)
O2^ii—Pb—O1^iii	73.8 (4)	Cl^vi—Pb—Cl^vii	128.95 (17)
O2—Pb—O1^iii	73.8 (4)	O2^ii—Pb—Cl^iv	144.4 (2)
O2^ii—Pb—Cl	75.0 (3)	O2—Pb—Cl^iv	144.4 (2)
O2—Pb—Cl	75.0 (3)	O1^iii—Pb—Cl^iv	122.1 (4)
O1^iii—Pb—Cl	142.3 (4)	Cl—Pb—Cl^iv	95.58 (15)
O2^ii—Pb—O2^iv	139.5 (4)	O2^iv—Pb—Cl^iv	63.0 (2)
O2—Pb—O2^iv	104.8 (3)	O2^v—Pb—Cl^iv	63.0 (2)
O1^iii—Pb—O2^iv	66.0 (4)	Cl^vi—Pb—Cl^iv	70.95 (7)
Cl—Pb—O2^iv	143.7 (2)	Cl^vii—Pb—Cl^iv	70.95 (7)
O2^ii—Pb—O2^v	104.8 (3)	Pb—Cl—Pb^viii	110.75 (11)
O2—Pb—O2^v	139.5 (4)	Pb—Cl—Pb^ix	110.75 (11)
O1^iii—Pb—O2^v	66.0 (4)	Pb^viii—Cl—Pb^ix	128.95 (17)
Cl—Pb—O2^v	143.7 (2)	Pb—Cl—Pb^x	95.58 (15)
O2^iv—Pb—O2^v	54.2 (4)	Pb^viii—Cl—Pb^x	102.10 (12)
O2^ii—Pb—Cl^vi	73.4 (2)	Pb^ix—Cl—Pb^x	102.10 (12)
O2—Pb—Cl^vi	135.6 (3)	Re—O1—Pb^xi	157.1 (9)
O1^iii—Pb—Cl^vi	114.32 (10)	Re—O2—Pb	148.1 (7)
Cl—Pb—Cl^vi	75.63 (6)	Re—O2—Pb^x	106.9 (6)
O2^iv—Pb—Cl^vi	118.6 (2)	Pb—O2—Pb^x	104.8 (3)

Symmetry codes: (i) −x, y, z; (ii) −x+1, y, z; (iii) −x+1/2, −y, z−1/2; (iv) x, y, z−1; (v) −x+1, y, z−1; (vi) −x+3/2, −y+1, z−1/2; (vii) −x+1/2, −y+1, z−1/2; (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.