Cerium copper diantimonide, CeCu_0.93(1)Sb₂

CeCu_0.93(1)Sb₂, synthesized in the presence of an Sn flux, crystallizes in the ZrCuSi₂-type structure, but with a partial occupancy of the Cu site.

Key indicators

• Single-crystal X-ray study
• T = 120 K
• Mean [sigma](e-Sb) = 0.002 Å
• Disorder in main residue
• R factor = 0.045
• wR factor = 0.119
• Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT301_ALERT_3_B Main Residue  Disorder .........................      41.00 Perc.

Alert level C
DIFMX01_ALERT_2_C  The maximum difference density is > 0.1*ZMAX*0.75
            _refine_diff_density_max given =      4.365
            Test value =      4.350
DIFMX02_ALERT_1_C  The minimum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
PLAT031_ALERT_4_C Refined Extinction Parameter within Range ......       3.00 Sigma
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   4 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
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXL97.

Cerium copper diantimonide

Crystal data

CeCu0.93Sb2	Dx = 7.629 Mg m^−3
Mr = 442.71	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/nmm	Cell parameters from 154 reflections
Hall symbol: -P 4a 2a	θ = 2.0–26.6°
a = 4.3424 (15) Å	µ = 30.26 mm^−1
c = 10.221 (7) Å	T = 120 K
V = 192.73 (16) Å^3	Block, silver
Z = 2	0.04 × 0.04 × 0.03 mm
F(000) = 374

Data collection

Bruker SMART APEX diffractometer	154 independent reflections
Radiation source: fine-focus sealed tube	133 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.056
Detector resolution: 8.3 pixels mm^-1	θmax = 26.6°, θmin = 2.0°
ω scans	h = −5→3
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	k = −5→5
Tmin = 0.328, Tmax = 0.404	l = −7→12
958 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.045	w = 1/[σ^2(Fo^2) + (0.0679P)^2 + 5.731P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.120	(Δ/σ)max < 0.001
S = 1.14	Δρmax = 4.37 e Å^−3
154 reflections	Δρmin = −2.95 e Å^−3
12 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.006 (2)

Special details

Experimental. Data collection is performed with four batch runs at φ = 0.00 ° (300 frames), at φ = 90.00 ° (300 frames), at φ = 180.00 ° (300 frames), and at φ = 270.00 (300 frames). Frame width = 0.60 \& in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections.

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	Occ. (<1)
Ce	0.2500	0.2500	0.24968 (19)	0.0091 (7)
Sb1	0.2500	0.2500	0.8484 (3)	0.0097 (8)
Sb2	0.7500	0.2500	0.5000	0.0109 (8)
Cu	0.7500	0.2500	0.0000	0.0092 (12)	0.93 (1)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ce	0.0077 (9)	0.0077 (9)	0.0119 (14)	0.000	0.000	0.000
Sb1	0.0078 (9)	0.0078 (9)	0.0133 (16)	0.000	0.000	0.000
Sb2	0.0091 (9)	0.0091 (9)	0.0145 (16)	0.000	0.000	0.000
Cu	0.0087 (16)	0.0087 (16)	0.010 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Ce—Sb1^i	3.2299 (14)	Sb2—Ce^iv	3.356 (2)
Ce—Sb1^ii	3.2299 (14)	Sb2—Ce^x	3.356 (2)
Ce—Sb1^iii	3.2299 (14)	Cu—Sb1^ii	2.6675 (18)
Ce—Sb1^iv	3.2299 (14)	Cu—Sb1^xi	2.6675 (18)
Ce—Cu^v	3.351 (2)	Cu—Sb1^iv	2.6675 (18)
Ce—Cu^vi	3.351 (2)	Cu—Sb1^xii	2.6675 (18)
Ce—Cu	3.351 (2)	Cu—Ce^x	3.351 (2)
Ce—Cu^vii	3.351 (2)	Cu—Ce^v	3.351 (2)
Ce—Sb2^ii	3.356 (2)	Cu—Ce^vii	3.351 (2)
Ce—Sb2	3.356 (2)	Sb1—Cu^ii	2.6676 (18)
Ce—Sb2^iv	3.356 (2)	Sb1—Cu^xiii	2.6676 (18)
Ce—Sb2^vi	3.356 (2)	Sb1—Cu^iv	2.6676 (18)
Sb2—Sb2^viii	3.0705 (11)	Sb1—Cu^xiv	2.6676 (18)
Sb2—Sb2^iv	3.0705 (11)	Sb1—Ce^i	3.2299 (14)
Sb2—Sb2^ii	3.0705 (11)	Sb1—Ce^ii	3.2299 (15)
Sb2—Sb2^ix	3.0705 (11)	Sb1—Ce^iv	3.2299 (14)
Sb2—Ce^ii	3.356 (2)	Sb1—Ce^iii	3.2299 (15)
Sb1^i—Ce—Sb1^ii	143.85 (11)	Sb2^ix—Sb2—Ce^ii	117.228 (18)
Sb1^i—Ce—Sb1^iii	84.48 (3)	Sb2^viii—Sb2—Ce^iv	117.228 (18)
Sb1^ii—Ce—Sb1^iii	84.48 (3)	Sb2^iv—Sb2—Ce^iv	62.772 (18)
Sb1^i—Ce—Sb1^iv	84.48 (3)	Sb2^ii—Sb2—Ce^iv	117.228 (19)
Sb1^ii—Ce—Sb1^iv	84.48 (3)	Sb2^ix—Sb2—Ce^iv	62.772 (19)
Sb1^iii—Ce—Sb1^iv	143.85 (11)	Ce^ii—Sb2—Ce^iv	80.64 (6)
Sb1^i—Ce—Cu^v	47.79 (4)	Sb2^viii—Sb2—Ce^x	62.772 (18)
Sb1^ii—Ce—Cu^v	101.50 (7)	Sb2^iv—Sb2—Ce^x	117.228 (18)
Sb1^iii—Ce—Cu^v	101.50 (7)	Sb2^ii—Sb2—Ce^x	117.228 (19)
Sb1^iv—Ce—Cu^v	47.79 (4)	Sb2^ix—Sb2—Ce^x	62.772 (19)
Sb1^i—Ce—Cu^vi	47.79 (4)	Ce^ii—Sb2—Ce^x	125.54 (4)
Sb1^ii—Ce—Cu^vi	101.50 (7)	Ce^iv—Sb2—Ce^x	125.54 (4)
Sb1^iii—Ce—Cu^vi	47.79 (4)	Sb2^viii—Sb2—Ce	117.228 (19)
Sb1^iv—Ce—Cu^vi	101.50 (7)	Sb2^iv—Sb2—Ce	62.772 (19)
Cu^v—Ce—Cu^vi	54.54 (4)	Sb2^ii—Sb2—Ce	62.772 (19)
Sb1^i—Ce—Cu	101.50 (7)	Sb2^ix—Sb2—Ce	117.228 (19)
Sb1^ii—Ce—Cu	47.79 (4)	Ce^ii—Sb2—Ce	125.54 (4)
Sb1^iii—Ce—Cu	101.50 (7)	Ce^iv—Sb2—Ce	125.54 (4)
Sb1^iv—Ce—Cu	47.79 (4)	Ce^x—Sb2—Ce	80.64 (6)
Cu^v—Ce—Cu	54.54 (4)	Sb1^ii—Cu—Sb1^xi	109.73 (5)
Cu^vi—Ce—Cu	80.78 (6)	Sb1^ii—Cu—Sb1^iv	108.96 (10)
Sb1^i—Ce—Cu^vii	101.50 (7)	Sb1^xi—Cu—Sb1^iv	109.73 (5)
Sb1^ii—Ce—Cu^vii	47.79 (4)	Sb1^ii—Cu—Sb1^xii	109.73 (5)
Sb1^iii—Ce—Cu^vii	47.79 (4)	Sb1^xi—Cu—Sb1^xii	108.96 (10)
Sb1^iv—Ce—Cu^vii	101.50 (7)	Sb1^iv—Cu—Sb1^xii	109.73 (5)
Cu^v—Ce—Cu^vii	80.78 (6)	Sb1^ii—Cu—Ce	63.74 (4)
Cu^vi—Ce—Cu^vii	54.54 (4)	Sb1^xi—Cu—Ce	85.13 (7)
Cu—Ce—Cu^vii	54.54 (4)	Sb1^iv—Cu—Ce	63.74 (4)
Sb1^i—Ce—Sb2^ii	132.18 (5)	Sb1^xii—Cu—Ce	165.91 (5)
Sb1^ii—Ce—Sb2^ii	78.56 (5)	Sb1^ii—Cu—Ce^x	63.74 (4)
Sb1^iii—Ce—Sb2^ii	78.56 (5)	Sb1^xi—Cu—Ce^x	165.91 (5)
Sb1^iv—Ce—Sb2^ii	132.18 (5)	Sb1^iv—Cu—Ce^x	63.74 (4)
Cu^v—Ce—Sb2^ii	179.93 (4)	Sb1^xii—Cu—Ce^x	85.13 (7)
Cu^vi—Ce—Sb2^ii	125.50 (3)	Ce—Cu—Ce^x	80.78 (6)
Cu—Ce—Sb2^ii	125.50 (3)	Sb1^ii—Cu—Ce^v	165.91 (5)
Cu^vii—Ce—Sb2^ii	99.29 (4)	Sb1^xi—Cu—Ce^v	63.74 (4)
Sb1^i—Ce—Sb2	132.18 (5)	Sb1^iv—Cu—Ce^v	85.13 (7)
Sb1^ii—Ce—Sb2	78.56 (5)	Sb1^xii—Cu—Ce^v	63.74 (4)
Sb1^iii—Ce—Sb2	132.18 (5)	Ce—Cu—Ce^v	125.46 (4)
Sb1^iv—Ce—Sb2	78.56 (5)	Ce^x—Cu—Ce^v	125.46 (4)
Cu^v—Ce—Sb2	125.50 (3)	Sb1^ii—Cu—Ce^vii	85.13 (7)
Cu^vi—Ce—Sb2	179.93 (4)	Sb1^xi—Cu—Ce^vii	63.74 (4)
Cu—Ce—Sb2	99.29 (4)	Sb1^iv—Cu—Ce^vii	165.91 (5)
Cu^vii—Ce—Sb2	125.50 (3)	Sb1^xii—Cu—Ce^vii	63.74 (4)
Sb2^ii—Ce—Sb2	54.46 (4)	Ce—Cu—Ce^vii	125.46 (4)
Sb1^i—Ce—Sb2^iv	78.56 (5)	Ce^x—Cu—Ce^vii	125.46 (4)
Sb1^ii—Ce—Sb2^iv	132.18 (5)	Ce^v—Cu—Ce^vii	80.78 (6)
Sb1^iii—Ce—Sb2^iv	132.18 (5)	Cu^ii—Sb1—Cu^xiii	70.27 (5)
Sb1^iv—Ce—Sb2^iv	78.56 (5)	Cu^ii—Sb1—Cu^iv	108.96 (10)
Cu^v—Ce—Sb2^iv	99.29 (4)	Cu^xiii—Sb1—Cu^iv	70.27 (5)
Cu^vi—Ce—Sb2^iv	125.50 (3)	Cu^ii—Sb1—Cu^xiv	70.27 (5)
Cu—Ce—Sb2^iv	125.50 (3)	Cu^xiii—Sb1—Cu^xiv	108.96 (10)
Cu^vii—Ce—Sb2^iv	179.93 (4)	Cu^iv—Sb1—Cu^xiv	70.27 (5)
Sb2^ii—Ce—Sb2^iv	80.64 (6)	Cu^ii—Sb1—Ce^i	136.67 (4)
Sb2—Ce—Sb2^iv	54.46 (4)	Cu^xiii—Sb1—Ce^i	136.67 (4)
Sb1^i—Ce—Sb2^vi	78.56 (5)	Cu^iv—Sb1—Ce^i	68.48 (4)
Sb1^ii—Ce—Sb2^vi	132.18 (5)	Cu^xiv—Sb1—Ce^i	68.48 (4)
Sb1^iii—Ce—Sb2^vi	78.56 (5)	Cu^ii—Sb1—Ce^ii	68.48 (4)
Sb1^iv—Ce—Sb2^vi	132.18 (5)	Cu^xiii—Sb1—Ce^ii	68.48 (4)
Cu^v—Ce—Sb2^vi	125.50 (3)	Cu^iv—Sb1—Ce^ii	136.67 (4)
Cu^vi—Ce—Sb2^vi	99.29 (4)	Cu^xiv—Sb1—Ce^ii	136.67 (4)
Cu—Ce—Sb2^vi	179.93 (4)	Ce^i—Sb1—Ce^ii	143.85 (11)
Cu^vii—Ce—Sb2^vi	125.50 (3)	Cu^ii—Sb1—Ce^iv	136.67 (4)
Sb2^ii—Ce—Sb2^vi	54.46 (4)	Cu^xiii—Sb1—Ce^iv	68.48 (4)
Sb2—Ce—Sb2^vi	80.64 (6)	Cu^iv—Sb1—Ce^iv	68.48 (4)
Sb2^iv—Ce—Sb2^vi	54.46 (4)	Cu^xiv—Sb1—Ce^iv	136.67 (4)
Sb2^viii—Sb2—Sb2^iv	180.0	Ce^i—Sb1—Ce^iv	84.48 (3)
Sb2^viii—Sb2—Sb2^ii	90.0	Ce^ii—Sb1—Ce^iv	84.48 (3)
Sb2^iv—Sb2—Sb2^ii	90.0	Cu^ii—Sb1—Ce^iii	68.48 (4)
Sb2^viii—Sb2—Sb2^ix	90.0	Cu^xiii—Sb1—Ce^iii	136.67 (4)
Sb2^iv—Sb2—Sb2^ix	90.0	Cu^iv—Sb1—Ce^iii	136.67 (4)
Sb2^ii—Sb2—Sb2^ix	180.0	Cu^xiv—Sb1—Ce^iii	68.48 (4)
Sb2^viii—Sb2—Ce^ii	62.772 (19)	Ce^i—Sb1—Ce^iii	84.48 (3)
Sb2^iv—Sb2—Ce^ii	117.228 (19)	Ce^ii—Sb1—Ce^iii	84.48 (3)
Sb2^ii—Sb2—Ce^ii	62.772 (18)	Ce^iv—Sb1—Ce^iii	143.85 (11)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+1; (iv) −x+1, −y, −z+1; (v) −x+1, −y, −z; (vi) x−1, y, z; (vii) −x+1, −y+1, −z; (viii) −x+2, −y+1, −z+1; (ix) −x+2, −y, −z+1; (x) x+1, y, z; (xi) x, y, z−1; (xii) x+1, y, z−1; (xiii) x, y, z+1; (xiv) x−1, y, z+1.