Crystal structure of the mixed-metal tris­ulfide BaCu1/3Ta2/3S3

Bu, K.; He, J.; Wang, D.; Zheng, C.; Huang, F.

doi:10.1107/S2056989017005266

Crystal structure of the mixed-metal trisulfide BaCu_1/3Ta_2/3S₃

K. Bu, J. He, D. Wang, C. Zheng and F. Huang

In the structure of BaCu_1/3Ta_2/3S₃, the Cu and Ta atoms are occupationally disordered on the same site in a ratio of 1/3:2/3.

Keywords: crystal structure; quasi-one-dimensional structure; mixed-metal trisulfide.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989017005266/wm5362sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989017005266/wm5362Isup3.hkl Contains datablock I

CCDC reference: 1542709

checkCIF report

Key indicators

Structure: I

Single-crystal X-ray study
T = 297 K
Mean () = 0.000 Å
Disorder in main residue
R factor = 0.043
wR factor = 0.113
Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..     Please Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of          S Check
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......     10.408 Check
PLAT971_ALERT_2_C Check Calcd Residual Density  1.03A From      Ta       1.58 eA-3
PLAT972_ALERT_2_C Check Calcd Residual Density  1.86A From       S      -1.61 eA-3

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       0.50 Check
PLAT068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
PLAT171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ta     --  S       ..        9.7 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cu     --  S       ..        9.7 s.u.
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1)..         21 % Note
PLAT811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          ! Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          2 Note

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

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX3 (Bruker, 2015); cell refinement: SAINT (Bruker, 2015); data reduction: SAINT (Bruker, 2015); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg, 2007); software used to prepare material for publication: publCIF (Westrip, 2010).

Barium copper(II) tantalum(V) trisulfide top

Crystal data top

BaCu_0.33Ta_0.67S₃	D_x = 5.280 Mg m⁻³
M_r = 375.14	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃/mmc	Cell parameters from 1738 reflections
a = 6.8350 (6) Å	θ = 3.4–25.9°
c = 5.8318 (5) Å	µ = 26.34 mm⁻¹
V = 235.94 (5) Å³	T = 297 K
Z = 2	Plate, black
F(000) = 325	0.04 × 0.03 × 0.01 mm

Data collection top

Bruker D8 QUEST diffractometer	106 reflections with I > 2σ(I)
Detector resolution: 10.4167 pixels mm^-1	R_int = 0.042
phi and ω scans	θ_max = 27.3°, θ_min = 3.4°
Absorption correction: multi-scan (SADABS; Bruker, 2015)	h = −8→8
T_min = 0.44, T_max = 0.86	k = −8→8
4312 measured reflections	l = −7→6
125 independent reflections

Refinement top

Refinement on F²	11 parameters
Least-squares matrix: full	2 restraints
R[F² > 2σ(F²)] = 0.043	w = 1/[σ²(F_o²) + (0.0503P)² + 4.8137P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.113	(Δ/σ)_max < 0.001
S = 1.25	Δρ_max = 1.50 e Å⁻³
125 reflections	Δρ_min = −1.50 e Å⁻³

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ba	0.6667	0.3333	0.75	0.0341 (7)
Ta	0	0	0.5	0.0707 (12)	0.6666 (8)
Cu	0	0	0.5	0.0707 (12)	0.3334 (18)
S	0.1689 (4)	0.3378 (8)	0.75	0.0449 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba	0.0246 (7)	0.0246 (7)	0.0529 (13)	0.0123 (4)	0	0
Ta	0.0306 (8)	0.0306 (8)	0.151 (3)	0.0153 (4)	0	0
Cu	0.0306 (8)	0.0306 (8)	0.151 (3)	0.0153 (4)	0	0
S	0.0217 (18)	0.015 (2)	0.096 (4)	0.0074 (10)	0	0

Geometric parameters (Å, º) top

Ba—Sⁱ	3.4176 (3)	Ta—S	2.475 (4)
Ba—Sⁱⁱ	3.4176 (3)	Ta—S^xiii	2.475 (4)
Ba—Sⁱⁱⁱ	3.4176 (3)	Ta—S^vii	2.475 (4)
Ba—S^iv	3.4176 (3)	Ta—S^xiv	2.475 (4)
Ba—S	3.4176 (3)	Ta—Ta^xv	2.9159 (3)
Ba—S^v	3.4176 (3)	Ta—Cu^xvi	2.9159 (3)
Ba—S^vi	3.506 (3)	Ta—Cu^xv	2.9159 (3)
Ba—S^vii	3.506 (3)	Ta—Ta^xvi	2.9159 (3)
Ba—S^viii	3.506 (3)	S—Cu^xv	2.475 (4)
Ba—S^ix	3.506 (3)	S—Ta^xv	2.475 (4)
Ba—S^x	3.506 (3)	S—Ba^xvii	3.4176 (3)
Ba—S^xi	3.506 (3)	S—Ba^vi	3.506 (3)
Ta—S^xii	2.475 (4)	S—Ba^ix	3.506 (3)
Ta—Sⁱⁱⁱ	2.475 (4)

Sⁱ—Ba—Sⁱⁱ	60.89 (16)	S^xii—Ta—Sⁱⁱⁱ	180.0
Sⁱ—Ba—Sⁱⁱⁱ	120.0010 (10)	S^xii—Ta—S	91.18 (10)
Sⁱⁱ—Ba—Sⁱⁱⁱ	59.11 (17)	Sⁱⁱⁱ—Ta—S	88.82 (10)
Sⁱ—Ba—S^iv	59.11 (17)	S^xii—Ta—S^xiii	88.82 (10)
Sⁱⁱ—Ba—S^iv	120.0010 (10)	Sⁱⁱⁱ—Ta—S^xiii	91.18 (10)
Sⁱⁱⁱ—Ba—S^iv	179.11 (16)	S—Ta—S^xiii	180.0
Sⁱ—Ba—S	179.11 (17)	S^xii—Ta—S^vii	88.82 (10)
Sⁱⁱ—Ba—S	120.0000 (10)	Sⁱⁱⁱ—Ta—S^vii	91.18 (10)
Sⁱⁱⁱ—Ba—S	60.89 (17)	S—Ta—S^vii	91.18 (10)
S^iv—Ba—S	119.9990 (10)	S^xiii—Ta—S^vii	88.82 (10)
Sⁱ—Ba—S^v	120.0000 (10)	S^xii—Ta—S^xiv	91.18 (10)
Sⁱⁱ—Ba—S^v	179.11 (17)	Sⁱⁱⁱ—Ta—S^xiv	88.82 (10)
Sⁱⁱⁱ—Ba—S^v	119.9990 (10)	S—Ta—S^xiv	88.82 (10)
S^iv—Ba—S^v	60.89 (17)	S^xiii—Ta—S^xiv	91.18 (10)
S—Ba—S^v	59.11 (17)	S^vii—Ta—S^xiv	180.0
Sⁱ—Ba—S^vi	89.75 (5)	S^xii—Ta—Ta^xv	126.10 (7)
Sⁱⁱ—Ba—S^vi	118.88 (3)	Sⁱⁱⁱ—Ta—Ta^xv	53.90 (7)
Sⁱⁱⁱ—Ba—S^vi	118.88 (3)	S—Ta—Ta^xv	53.90 (7)
S^iv—Ba—S^vi	61.40 (8)	S^xiii—Ta—Ta^xv	126.10 (7)
S—Ba—S^vi	89.75 (5)	S^vii—Ta—Ta^xv	126.10 (7)
S^v—Ba—S^vi	61.40 (8)	S^xiv—Ta—Ta^xv	53.90 (7)
Sⁱ—Ba—S^vii	118.88 (3)	S^xii—Ta—Cu^xvi	53.90 (7)
Sⁱⁱ—Ba—S^vii	89.75 (5)	Sⁱⁱⁱ—Ta—Cu^xvi	126.10 (7)
Sⁱⁱⁱ—Ba—S^vii	61.40 (8)	S—Ta—Cu^xvi	126.10 (7)
S^iv—Ba—S^vii	118.88 (3)	S^xiii—Ta—Cu^xvi	53.90 (7)
S—Ba—S^vii	61.40 (8)	S^vii—Ta—Cu^xvi	53.90 (7)
S^v—Ba—S^vii	89.75 (5)	S^xiv—Ta—Cu^xvi	126.10 (7)
S^vi—Ba—S^vii	147.76 (6)	Ta^xv—Ta—Cu^xvi	180.0
Sⁱ—Ba—S^viii	118.88 (3)	S^xii—Ta—Cu^xv	126.10 (7)
Sⁱⁱ—Ba—S^viii	89.75 (5)	Sⁱⁱⁱ—Ta—Cu^xv	53.90 (7)
Sⁱⁱⁱ—Ba—S^viii	61.40 (8)	S—Ta—Cu^xv	53.90 (7)
S^iv—Ba—S^viii	118.88 (3)	S^xiii—Ta—Cu^xv	126.10 (7)
S—Ba—S^viii	61.40 (8)	S^vii—Ta—Cu^xv	126.10 (7)
S^v—Ba—S^viii	89.75 (5)	S^xiv—Ta—Cu^xv	53.90 (7)
S^vi—Ba—S^viii	57.48 (11)	Ta^xv—Ta—Cu^xv	0
S^vii—Ba—S^viii	112.55 (14)	Cu^xvi—Ta—Cu^xv	180.0
Sⁱ—Ba—S^ix	89.75 (5)	S^xii—Ta—Ta^xvi	53.90 (7)
Sⁱⁱ—Ba—S^ix	118.88 (3)	Sⁱⁱⁱ—Ta—Ta^xvi	126.10 (7)
Sⁱⁱⁱ—Ba—S^ix	118.88 (3)	S—Ta—Ta^xvi	126.10 (7)
S^iv—Ba—S^ix	61.40 (8)	S^xiii—Ta—Ta^xvi	53.90 (7)
S—Ba—S^ix	89.75 (5)	S^vii—Ta—Ta^xvi	53.90 (7)
S^v—Ba—S^ix	61.40 (8)	S^xiv—Ta—Ta^xvi	126.10 (7)
S^vi—Ba—S^ix	112.55 (14)	Ta^xv—Ta—Ta^xvi	180.0
S^vii—Ba—S^ix	57.48 (11)	Cu^xvi—Ta—Ta^xvi	0
S^viii—Ba—S^ix	147.76 (6)	Cu^xv—Ta—Ta^xvi	180.0
Sⁱ—Ba—S^x	61.40 (8)	Ta—S—Cu^xv	72.2
Sⁱⁱ—Ba—S^x	61.40 (8)	Ta—S—Ta^xv	72.19 (13)
Sⁱⁱⁱ—Ba—S^x	89.75 (5)	Cu^xv—S—Ta^xv	0
S^iv—Ba—S^x	89.75 (5)	Ta—S—Ba	89.64 (7)
S—Ba—S^x	118.88 (3)	Cu^xv—S—Ba	89.64 (7)
S^v—Ba—S^x	118.88 (3)	Ta^xv—S—Ba	89.64 (7)
S^vi—Ba—S^x	57.48 (11)	Ta—S—Ba^xvii	89.64 (7)
S^vii—Ba—S^x	147.76 (6)	Cu^xv—S—Ba^xvii	89.64 (7)
S^viii—Ba—S^x	57.48 (11)	Ta^xv—S—Ba^xvii	89.64 (7)
S^ix—Ba—S^x	147.76 (6)	Ba—S—Ba^xvii	179.11 (16)
Sⁱ—Ba—S^xi	61.40 (8)	Ta—S—Ba^vi	159.82 (13)
Sⁱⁱ—Ba—S^xi	61.40 (8)	Cu^xv—S—Ba^vi	87.629 (7)
Sⁱⁱⁱ—Ba—S^xi	89.75 (5)	Ta^xv—S—Ba^vi	87.629 (7)
S^iv—Ba—S^xi	89.75 (5)	Ba—S—Ba^vi	90.25 (5)
S—Ba—S^xi	118.88 (3)	Ba^xvii—S—Ba^vi	90.25 (5)
S^v—Ba—S^xi	118.88 (3)	Ta—S—Ba^ix	87.629 (7)
S^vi—Ba—S^xi	147.76 (6)	Cu^xv—S—Ba^ix	159.82 (13)
S^vii—Ba—S^xi	57.48 (11)	Ta^xv—S—Ba^ix	159.82 (13)
S^viii—Ba—S^xi	147.76 (6)	Ba—S—Ba^ix	90.25 (5)
S^ix—Ba—S^xi	57.48 (11)	Ba^xvii—S—Ba^ix	90.25 (5)
S^x—Ba—S^xi	112.55 (13)	Ba^vi—S—Ba^ix	112.55 (13)

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

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Crystal structure of the mixed-metal tris­ulfide BaCu1/3Ta2/3S3

Supporting information

Key indicators

checkCIF/PLATON results

Crystal structure of the mixed-metal trisulfide BaCu_1/3Ta_2/3S₃