Growth and characterization of a new inorganic metal–halide crystal structure, InPb₂Cl₅

A new solid-state inorganic compound, InPb₂Cl₅, was synthesized by melting InCl and PbCl₂ in a vacuum-sealed quartz ampoule. Bulk InPb₂Cl₅ was separated from PbCl2 and characterized by single-crystal X-ray diffraction.

Key indicators

Structure: I

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](b-Cl) = 0.001 Å
• R factor = 0.021
• wR factor = 0.042
• Data-to-parameter ratio = 36.5

checkCIF/PLATON results

No syntax errors found



Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Pb1       (II)      .       2.27 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Pb2       (II)      .       2.15 Info
PLAT794_ALERT_5_G Tentative Bond Valency for In1       (I)       .       1.05 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         10 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   0 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   5 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   4 ALERT type 5 Informative message, check

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Computing details

Cell refinement: APEX2 (Bruker, 2012); data reduction: SAINT (Bruker, 2012); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: CrystalMaker (Palmer, 2014); software used to prepare material for publication: WinGX (Farrugia, 2012) and publCIF (Westrip, 2010).

Indium dilead pentachloride

Crystal data

In2Pb4Cl10	F(000) = 1192
Mr = 1412.9	Dx = 5.297 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9997 reflections
a = 8.9681 (11) Å	θ = 2.3–30.5°
b = 7.9033 (9) Å	µ = 41.91 mm^−1
c = 12.4980 (16) Å	T = 298 K
β = 90.254 (6)°	Transparent square, colourless
V = 885.82 (19) Å^3	0.22 × 0.18 × 0.13 mm
Z = 2

Data collection

Bruker APEXII CCD diffractometer	2699 independent reflections
Radiation source: sealed X-ray tube, Incoatec Iµs	2423 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.051
Detector resolution: 7.9 pixels mm^-1	θmax = 30.6°, θmin = 2.3°
φ and ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	k = −11→11
Tmin = 0.378, Tmax = 0.746	l = −17→17
20682 measured reflections

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.021	w = 1/[σ^2(Fo^2) + (0.0083P)^2 + 1.8133P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.042	(Δ/σ)max = 0.002
S = 1.08	Δρmax = 1.22 e Å^−3
2699 reflections	Δρmin = −1.13 e Å^−3
74 parameters	Extinction correction: SHELXL-2018/3 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00232 (8)

Special details

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cl1	0.04109 (12)	0.67574 (15)	0.41739 (11)	0.0316 (3)
Cl2	0.45758 (11)	0.66555 (13)	0.40434 (9)	0.0226 (2)
Cl3	0.27835 (14)	0.65746 (14)	0.68735 (10)	0.0304 (3)
Cl4	0.72918 (12)	0.68702 (14)	0.72264 (9)	0.0252 (2)
Cl5	0.28105 (12)	0.45943 (14)	1.00167 (9)	0.0232 (2)
In1	0.98678 (5)	0.45346 (6)	0.83468 (4)	0.04410 (11)
Pb1	0.24664 (2)	0.43551 (2)	0.50647 (2)	0.02229 (6)
Pb2	0.49498 (2)	0.48805 (2)	0.82509 (2)	0.02538 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cl1	0.0194 (5)	0.0309 (6)	0.0445 (7)	0.0009 (4)	0.0017 (5)	0.0137 (5)
Cl2	0.0192 (5)	0.0201 (4)	0.0285 (6)	−0.0008 (4)	−0.0002 (4)	0.0059 (4)
Cl3	0.0364 (6)	0.0283 (5)	0.0263 (6)	0.0084 (5)	−0.0081 (5)	−0.0063 (4)
Cl4	0.0259 (5)	0.0254 (5)	0.0243 (6)	−0.0027 (4)	0.0021 (4)	0.0025 (4)
Cl5	0.0251 (5)	0.0240 (5)	0.0205 (5)	0.0004 (4)	0.0005 (4)	0.0009 (4)
In1	0.0418 (2)	0.0432 (2)	0.0472 (3)	0.00874 (18)	−0.00359 (19)	−0.00495 (19)
Pb1	0.01876 (9)	0.02412 (9)	0.02399 (10)	−0.00042 (6)	−0.00025 (6)	−0.00142 (6)
Pb2	0.02614 (10)	0.02526 (9)	0.02473 (10)	−0.00304 (7)	0.00037 (7)	0.00179 (6)

Geometric parameters (Å, º)

Cl1—Pb1	2.8677 (12)	Cl3—Pb2	2.9156 (12)
Cl1—Pb1^i	2.8912 (11)	Cl4—Pb2	2.9236 (11)
Cl2—Pb1	2.9214 (10)	Cl4—Pb1^iii	3.0314 (12)
Cl2—Pb2^ii	2.9311 (10)	Cl5—Pb2	2.9394 (11)
Cl2—Pb1^iii	2.9817 (11)	Cl5—Pb2^iv	2.9760 (12)
Cl3—Pb1	2.8744 (12)
Pb1—Cl1—Pb1^i	104.12 (4)	Cl2—Pb1—Cl2^iii	75.72 (3)
Pb1—Cl2—Pb2^ii	143.53 (4)	Cl1—Pb1—Cl4^iii	83.88 (4)
Pb1—Cl2—Pb1^iii	104.28 (3)	Cl3—Pb1—Cl4^iii	158.52 (3)
Pb2^ii—Cl2—Pb1^iii	105.88 (3)	Cl1^i—Pb1—Cl4^iii	106.34 (4)
Pb1—Cl3—Pb2	104.33 (4)	Cl2—Pb1—Cl4^iii	74.75 (3)
Pb2—Cl4—Pb1^iii	107.24 (4)	Cl2^iii—Pb1—Cl4^iii	101.55 (3)
Pb2—Cl5—Pb2^iv	95.44 (3)	Cl3—Pb2—Cl4	88.42 (4)
Cl1—Pb1—Cl3	87.85 (4)	Cl3—Pb2—Cl2^v	72.16 (3)
Cl1—Pb1—Cl1^i	75.88 (4)	Cl4—Pb2—Cl2^v	74.28 (3)
Cl3—Pb1—Cl1^i	90.69 (4)	Cl3—Pb2—Cl5	92.48 (3)
Cl1—Pb1—Cl2	80.49 (3)	Cl4—Pb2—Cl5	147.44 (3)
Cl3—Pb1—Cl2	84.37 (4)	Cl2^v—Pb2—Cl5	75.06 (3)
Cl1^i—Pb1—Cl2	156.02 (3)	Cl3—Pb2—Cl5^iv	144.23 (3)
Cl1—Pb1—Cl2^iii	153.09 (3)	Cl4—Pb2—Cl5^iv	76.10 (3)
Cl3—Pb1—Cl2^iii	77.57 (3)	Cl2^v—Pb2—Cl5^iv	72.65 (3)
Cl1^i—Pb1—Cl2^iii	126.11 (3)	Cl5—Pb2—Cl5^iv	84.56 (3)

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