Literature DB >> 22064850

Calcium platinum aluminium, CaPtAl.

Patrice Kenfack Tsobnang, Daniel Fotio, Siméon Ponou, Charles Fon Abi.

Abstract

A preliminary X-ray study of CaPtAl has been reported previously by Hulliger [J. Alloys Compd (1993), 196, 225-228] based on X-ray powder diffraction data without structure refinement. With the present single-crystal X-ray study, we confirm the assignment of the TiNiSi type for CaPtAl, in a fully ordered inverse structure. All three atoms of the asymmetric unit have .m. site symmetry. The structure features a (∞) (3)[AlPt] open framework with a fourfold coordination of Pt by Al atoms and vice versa. The Ca atoms are located in the large channels of the structure.

Entities: Chemical Disease Species

Year: 2011 PMID： 22064850 PMCID： PMC3201391 DOI： 10.1107/S1600536811036749

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For a previous X-ray powder diffraction study of CaPtAl, see: Hulliger (1993 ▶). For related compounds, see: Dascoulidou-Gritner & Schuster (1994 ▶); Merlo et al. (1996 ▶). For structural systematics and properties of the TiNiSi structure type, see: Kussmann et al. (1998) ▶; Hoffmann & Pöttgen (2001 ▶); Nuspl et al. (1996 ▶); Evers et al. (1992 ▶). For related compounds of the TiNiSi structure type, see: Ponou & Lidin (2008 ▶); Ponou (2010 ▶); Banenzoué et al. (2009 ▶). For atomic radii, see: Pauling (1960 ▶).

Experimental

Crystal data

CaPtAl M = 262.15 Orthorhombic, a = 7.1581 (14) Å b = 4.2853 (15) Å c = 7.7536 (9) Å V = 237.84 (10) Å3 Z = 4 Mo Kα radiation μ = 61.08 mm−1 T = 293 K 0.15 × 0.08 × 0.05 mm

Data collection

Oxford Diffraction Xcalibur diffractometer with Sapphire3 CCD Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007 ▶) T min = 0.004, T max = 0.047 4413 measured reflections 511 independent reflections 435 reflections with I > 2σ(I) R int = 0.091

Refinement

R[F 2 > 2σ(F 2)] = 0.028 wR(F 2) = 0.064 S = 1.03 511 reflections 20 parameters Δρmax = 2.61 e Å−3 Δρmin = −2.95 e Å−3 Data collection: CrysAlis CCD (Oxford Diffraction, 2007 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2007 ▶); data reduction: CrysAlis CCD; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811036749/wm2532sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811036749/wm2532Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

CaPtAl	F(000) = 444
M_r = 262.15	D_x = 7.321 Mg m⁻³
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2105 reflections
a = 7.1581 (14) Å	θ = 2.6–33.7°
b = 4.2853 (15) Å	µ = 61.08 mm⁻¹
c = 7.7536 (9) Å	T = 293 K
V = 237.84 (10) Å³	Irregular block, metallic grey
Z = 4	0.15 × 0.08 × 0.05 mm

Oxford Diffraction Xcalibur diffractometer with Sapphire3 CCD	511 independent reflections
graphite	435 reflections with I > 2σ(I)
Detector resolution: 16.1829 pixels mm^-1	R_int = 0.091
ω and φ scans	θ_max = 33.8°, θ_min = 3.9°
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	h = −10→11
T_min = 0.004, T_max = 0.047	k = −6→6
4413 measured reflections	l = −11→12

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.028	w = 1/[σ²(F_o²) + (0.0326P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.064	(Δ/σ)_max < 0.001
S = 1.03	Δρ_max = 2.61 e Å⁻³
511 reflections	Δρ_min = −2.95 e Å⁻³
20 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008)
0 restraints	Extinction coefficient: 0.0027 (5)

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.

	x	y	z	U_iso*/U_eq
Pt1	0.78928 (5)	0.25	0.38355 (4)	0.01029 (15)
Al1	0.1446 (5)	0.25	0.4346 (4)	0.0103 (6)
Ca1	0.4796 (3)	0.75	0.3234 (2)	0.0106 (4)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.00775 (19)	0.0118 (2)	0.0113 (2)	0	0.00104 (12)	0
Al1	0.0087 (13)	0.0127 (15)	0.0094 (11)	0	0.0001 (11)	0
Ca1	0.0088 (8)	0.0129 (10)	0.0102 (8)	0	−0.0011 (6)	0

Pt1—Al1ⁱ	2.574 (3)	Al1—Ca1^xi	3.160 (3)
Pt1—Al1ⁱⁱ	2.6084 (17)	Al1—Ca1^ix	3.160 (3)
Pt1—Al1ⁱⁱⁱ	2.6084 (17)	Al1—Ca1ⁱⁱ	3.280 (4)
Pt1—Al1^iv	2.675 (3)	Al1—Ca1	3.329 (3)
Pt1—Ca1ⁱⁱ	2.978 (2)	Al1—Ca1^vi	3.329 (3)
Pt1—Ca1^v	3.0037 (14)	Ca1—Pt1ⁱⁱ	2.978 (2)
Pt1—Ca1^iv	3.0037 (14)	Ca1—Pt1^ix	3.0037 (14)
Pt1—Ca1^vi	3.1179 (16)	Ca1—Pt1^xii	3.0037 (14)
Pt1—Ca1	3.1179 (16)	Ca1—Pt1^xiii	3.1179 (16)
Pt1—Ca1^vii	3.791 (2)	Ca1—Al1^xiv	3.143 (3)
Al1—Pt1^viii	2.574 (3)	Ca1—Al1^iv	3.160 (3)
Al1—Pt1ⁱⁱ	2.6084 (17)	Ca1—Al1^xv	3.160 (3)
Al1—Pt1ⁱⁱⁱ	2.6084 (17)	Ca1—Al1ⁱⁱ	3.280 (4)
Al1—Pt1^ix	2.675 (3)	Ca1—Al1^xiii	3.329 (3)
Al1—Ca1^x	3.143 (3)	Ca1—Ca1^xvi	3.489 (3)

Al1ⁱ—Pt1—Al1ⁱⁱ	74.79 (9)	Ca1^xi—Al1—Ca1	122.80 (9)
Al1ⁱ—Pt1—Al1ⁱⁱⁱ	74.79 (8)	Ca1^ix—Al1—Ca1	70.67 (4)
Al1ⁱⁱ—Pt1—Al1ⁱⁱⁱ	110.46 (10)	Ca1ⁱⁱ—Al1—Ca1	63.73 (7)
Al1ⁱ—Pt1—Al1^iv	121.62 (9)	Pt1^viii—Al1—Ca1^vi	132.22 (7)
Al1ⁱⁱ—Pt1—Al1^iv	124.66 (5)	Pt1ⁱⁱ—Al1—Ca1^vi	122.54 (12)
Al1ⁱⁱⁱ—Pt1—Al1^iv	124.66 (5)	Pt1ⁱⁱⁱ—Al1—Ca1^vi	58.71 (5)
Al1ⁱ—Pt1—Ca1ⁱⁱ	121.43 (7)	Pt1^ix—Al1—Ca1^vi	58.83 (6)
Al1ⁱⁱ—Pt1—Ca1ⁱⁱ	72.83 (7)	Ca1^x—Al1—Ca1^vi	116.88 (8)
Al1ⁱⁱⁱ—Pt1—Ca1ⁱⁱ	72.83 (7)	Ca1^xi—Al1—Ca1^vi	70.67 (4)
Al1^iv—Pt1—Ca1ⁱⁱ	116.96 (8)	Ca1^ix—Al1—Ca1^vi	122.80 (9)
Al1ⁱ—Pt1—Ca1^v	68.52 (5)	Ca1ⁱⁱ—Al1—Ca1^vi	63.73 (7)
Al1ⁱⁱ—Pt1—Ca1^v	142.42 (8)	Ca1—Al1—Ca1^vi	80.12 (9)
Al1ⁱⁱⁱ—Pt1—Ca1^v	67.70 (7)	Pt1ⁱⁱ—Ca1—Pt1^ix	96.57 (5)
Al1^iv—Pt1—Ca1^v	71.52 (6)	Pt1ⁱⁱ—Ca1—Pt1^xii	96.57 (5)
Ca1ⁱⁱ—Pt1—Ca1^v	134.49 (3)	Pt1^ix—Ca1—Pt1^xii	91.01 (6)
Al1ⁱ—Pt1—Ca1^iv	68.52 (5)	Pt1ⁱⁱ—Ca1—Pt1^xiii	110.21 (5)
Al1ⁱⁱ—Pt1—Ca1^iv	67.70 (7)	Pt1^ix—Ca1—Pt1^xiii	153.20 (7)
Al1ⁱⁱⁱ—Pt1—Ca1^iv	142.42 (8)	Pt1^xii—Ca1—Pt1^xiii	84.96 (3)
Al1^iv—Pt1—Ca1^iv	71.52 (6)	Pt1ⁱⁱ—Ca1—Pt1	110.21 (5)
Ca1ⁱⁱ—Pt1—Ca1^iv	134.49 (3)	Pt1^ix—Ca1—Pt1	84.96 (3)
Ca1^v—Pt1—Ca1^iv	91.01 (6)	Pt1^xii—Ca1—Pt1	153.20 (7)
Al1ⁱ—Pt1—Ca1^vi	136.51 (3)	Pt1^xiii—Ca1—Pt1	86.82 (5)
Al1ⁱⁱ—Pt1—Ca1^vi	140.75 (8)	Pt1ⁱⁱ—Ca1—Al1^xiv	123.30 (9)
Al1ⁱⁱⁱ—Pt1—Ca1^vi	69.23 (7)	Pt1^ix—Ca1—Al1^xiv	50.15 (4)
Al1^iv—Pt1—Ca1^vi	65.60 (6)	Pt1^xii—Ca1—Al1^xiv	50.15 (4)
Ca1ⁱⁱ—Pt1—Ca1^vi	69.79 (5)	Pt1^xiii—Ca1—Al1^xiv	110.15 (6)
Ca1^v—Pt1—Ca1^vi	75.66 (3)	Pt1—Ca1—Al1^xiv	110.15 (6)
Ca1^iv—Pt1—Ca1^vi	137.12 (3)	Pt1ⁱⁱ—Ca1—Al1^iv	136.43 (5)
Al1ⁱ—Pt1—Ca1	136.51 (3)	Pt1^ix—Ca1—Al1^iv	49.29 (6)
Al1ⁱⁱ—Pt1—Ca1	69.23 (7)	Pt1^xii—Ca1—Al1^iv	108.36 (7)
Al1ⁱⁱⁱ—Pt1—Ca1	140.74 (8)	Pt1^xiii—Ca1—Al1^iv	107.15 (8)
Al1^iv—Pt1—Ca1	65.60 (6)	Pt1—Ca1—Al1^iv	50.44 (6)
Ca1ⁱⁱ—Pt1—Ca1	69.79 (5)	Al1^xiv—Ca1—Al1^iv	59.91 (8)
Ca1^v—Pt1—Ca1	137.12 (3)	Pt1ⁱⁱ—Ca1—Al1^xv	136.43 (5)
Ca1^iv—Pt1—Ca1	75.66 (3)	Pt1^ix—Ca1—Al1^xv	108.36 (7)
Ca1^vi—Pt1—Ca1	86.82 (5)	Pt1^xii—Ca1—Al1^xv	49.29 (6)
Al1ⁱ—Pt1—Ca1^vii	55.28 (7)	Pt1^xiii—Ca1—Al1^xv	50.44 (6)
Al1ⁱⁱ—Pt1—Ca1^vii	55.55 (5)	Pt1—Ca1—Al1^xv	107.15 (8)
Al1ⁱⁱⁱ—Pt1—Ca1^vii	55.55 (5)	Al1^xiv—Ca1—Al1^xv	59.91 (8)
Al1^iv—Pt1—Ca1^vii	176.90 (8)	Al1^iv—Ca1—Al1^xv	85.38 (9)
Ca1ⁱⁱ—Pt1—Ca1^vii	66.144 (17)	Pt1ⁱⁱ—Ca1—Al1ⁱⁱ	95.37 (7)
Ca1^v—Pt1—Ca1^vii	106.42 (4)	Pt1^ix—Ca1—Al1ⁱⁱ	132.66 (3)
Ca1^iv—Pt1—Ca1^vii	106.42 (4)	Pt1^xii—Ca1—Al1ⁱⁱ	132.66 (3)
Ca1^vi—Pt1—Ca1^vii	116.41 (5)	Pt1^xiii—Ca1—Al1ⁱⁱ	48.04 (3)
Ca1—Pt1—Ca1^vii	116.41 (5)	Pt1—Ca1—Al1ⁱⁱ	48.04 (3)
Pt1^viii—Al1—Pt1ⁱⁱ	105.21 (8)	Al1^xiv—Ca1—Al1ⁱⁱ	141.34 (12)
Pt1^viii—Al1—Pt1ⁱⁱⁱ	105.21 (8)	Al1^iv—Ca1—Al1ⁱⁱ	93.19 (5)
Pt1ⁱⁱ—Al1—Pt1ⁱⁱⁱ	110.46 (10)	Al1^xv—Ca1—Al1ⁱⁱ	93.19 (5)
Pt1^viii—Al1—Pt1^ix	103.93 (10)	Pt1ⁱⁱ—Ca1—Al1	48.46 (5)
Pt1ⁱⁱ—Al1—Pt1^ix	115.36 (8)	Pt1^ix—Ca1—Al1	49.65 (5)
Pt1ⁱⁱⁱ—Al1—Pt1^ix	115.36 (8)	Pt1^xii—Ca1—Al1	105.70 (8)
Pt1^viii—Al1—Ca1^x	82.41 (9)	Pt1^xiii—Ca1—Al1	156.29 (8)
Pt1ⁱⁱ—Al1—Ca1^x	62.14 (6)	Pt1—Ca1—Al1	91.78 (5)
Pt1ⁱⁱⁱ—Al1—Ca1^x	62.14 (6)	Al1^xiv—Ca1—Al1	92.55 (6)
Pt1^ix—Al1—Ca1^x	173.66 (14)	Al1^iv—Ca1—Al1	89.81 (6)
Pt1^viii—Al1—Ca1^xi	62.19 (7)	Al1^xv—Ca1—Al1	150.39 (11)
Pt1ⁱⁱ—Al1—Ca1^xi	165.23 (11)	Al1ⁱⁱ—Ca1—Al1	116.27 (7)
Pt1ⁱⁱⁱ—Al1—Ca1^xi	81.55 (4)	Pt1ⁱⁱ—Ca1—Al1^xiii	48.46 (5)
Pt1^ix—Al1—Ca1^xi	63.96 (6)	Pt1^ix—Ca1—Al1^xiii	105.70 (8)
Ca1^x—Al1—Ca1^xi	120.09 (8)	Pt1^xii—Ca1—Al1^xiii	49.65 (5)
Pt1^viii—Al1—Ca1^ix	62.19 (7)	Pt1^xiii—Ca1—Al1^xiii	91.78 (5)
Pt1ⁱⁱ—Al1—Ca1^ix	81.55 (4)	Pt1—Ca1—Al1^xiii	156.29 (8)
Pt1ⁱⁱⁱ—Al1—Ca1^ix	165.23 (11)	Al1^xiv—Ca1—Al1^xiii	92.55 (6)
Pt1^ix—Al1—Ca1^ix	63.96 (6)	Al1^iv—Ca1—Al1^xiii	150.39 (10)
Ca1^x—Al1—Ca1^ix	120.09 (8)	Al1^xv—Ca1—Al1^xiii	89.81 (6)
Ca1^xi—Al1—Ca1^ix	85.38 (9)	Al1ⁱⁱ—Ca1—Al1^xiii	116.27 (7)
Pt1^viii—Al1—Ca1ⁱⁱ	153.94 (11)	Al1—Ca1—Al1^xiii	80.12 (9)
Pt1ⁱⁱ—Al1—Ca1ⁱⁱ	62.73 (6)	Pt1ⁱⁱ—Ca1—Ca1^xvi	56.99 (5)
Pt1ⁱⁱⁱ—Al1—Ca1ⁱⁱ	62.73 (6)	Pt1^ix—Ca1—Ca1^xvi	153.54 (10)
Pt1^ix—Al1—Ca1ⁱⁱ	102.13 (11)	Pt1^xii—Ca1—Ca1^xvi	91.10 (3)
Ca1^x—Al1—Ca1ⁱⁱ	71.53 (6)	Pt1^xiii—Ca1—Ca1^xvi	53.22 (4)
Ca1^xi—Al1—Ca1ⁱⁱ	131.96 (7)	Pt1—Ca1—Ca1^xvi	104.19 (8)
Ca1^ix—Al1—Ca1ⁱⁱ	131.96 (7)	Al1^xiv—Ca1—Ca1^xvi	140.93 (5)
Pt1^viii—Al1—Ca1	132.22 (7)	Al1^iv—Ca1—Ca1^xvi	151.87 (11)
Pt1ⁱⁱ—Al1—Ca1	58.71 (5)	Al1^xv—Ca1—Ca1^xvi	92.82 (5)
Pt1ⁱⁱⁱ—Al1—Ca1	122.54 (12)	Al1ⁱⁱ—Ca1—Ca1^xvi	58.83 (7)
Pt1^ix—Al1—Ca1	58.83 (6)	Al1—Ca1—Ca1^xvi	104.61 (9)
Ca1^x—Al1—Ca1	116.88 (8)	Al1^xiii—Ca1—Ca1^xvi	57.44 (6)

3 in total

1. The Four-Connected Net in the CeCu(2) Structure and Its Ternary Derivatives. Its Electronic and Structural Properties.

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Journal: Inorg Chem Date: 1996-11-20 Impact factor: 5.165

2. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

3. Non-isovalent substitution in a Zintl phase with the TiNiSi type structure, CaMg(1-x)Ag(x)Ge [x = 0.13 (3)].

Authors: Charles Banenzoué; Siméon Ponou; John Ngolui Lambi
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-11-21

3 in total