Reinvestigation of Ni₃TeO₆

The crystal structure of the title compound, trinickel(II) tellurium(VI) hexa­oxide, has been reinvestigated [Newnham & Meagher (1967). Mater. Res. Bull. 2, 549-554] and confirmed to much higher precision. The structure is of the corundum (Al₂O₃) type, with Ni and Te replacing Al in an ordered manner. All the metal atoms occupy special positions with site symmetry 3.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• Mean [sigma](i-O) = 0.006 Å
• R factor = 0.024
• wR factor = 0.059
• Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT112_ALERT_2_A ADDSYM Detects Additional (Pseudo) Symm. Elem...          n

Author Response: The n glides would give rise to a C centring and 335 reflexes, some as strong as above 60 sigma, breake this symmetry.

PLAT112_ALERT_2_A ADDSYM Detects Additional (Pseudo) Symm. Elem...          n

Author Response: The n glides would give rise to a C centring and 335 reflexes, some as strong as above 60 sigma, breake this symmetry.

PLAT112_ALERT_2_A ADDSYM Detects Additional (Pseudo) Symm. Elem...          n

Author Response: The n glides would give rise to a C centring and 335 reflexes, some as strong as above 60 sigma, breake this symmetry.

PLAT113_ALERT_2_A ADDSYM Suggests Possible Pseudo/New Spacegroup .       R-3c

Author Response: The c centring is not possible due to the present 335 reflexes that breaks this symmetry. The centrosymmetry can not exist as two of the Ni atoms can not relate and merge into a single one.

Alert level B
PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry .....        100 PerFi

Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.77
PLAT850_ALERT_2_C Check Flack Parameter Exact Value 0.00 and su ..       0.02

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           32.87
           From the CIF: _reflns_number_total                514
           Count of symmetry unique reflns          269
           Completeness (_total/calc)            191.08%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       245
           Fraction of Friedel pairs measured     0.911
           Are heavy atom types Z>Si present        yes

   4 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   2 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
   7 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
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.

Trinickel(II) tellurium(VI) hexaoxide

Crystal data

Ni3TeO6	Dx = 6.399 Mg m^−3
Mr = 399.73	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3	Cell parameters from 2232 reflections
Hall symbol: R 3	θ = 4.4–32.9°
a = 5.1087 (8) Å	µ = 20.31 mm^−1
c = 13.767 (2) Å	T = 292 K
V = 311.17 (8) Å^3	Prism, green
Z = 3	0.09 × 0.06 × 0.04 mm
F(000) = 552

Data collection

Oxford Xcalibur diffractometer	514 independent reflections
Radiation source: fine-focus sealed tube, Oxford diffraction Xcalibur3	506 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.079
ω scans	θmax = 32.9°, θmin = 4.4°
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	h = −7→7
Tmin = 0.500, Tmax = 1.000	k = −7→7
2232 measured reflections	l = −20→20

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.028P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.024	(Δ/σ)max < 0.001
wR(F^2) = 0.059	Δρmax = 3.46 e Å^−3
S = 1.08	Δρmin = −0.92 e Å^−3
514 reflections	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
33 parameters	Extinction coefficient: 0.0070 (8)
1 restraint	Absolute structure: Flack (1983), with 245 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.000 (17)

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
Te1	0.3333	0.6667	0.37517 (8)	0.00413 (17)
Ni1	0.3333	0.6667	0.17325 (6)	0.0040 (3)
Ni2	1.0000	1.0000	0.2144 (3)	0.0093 (5)
Ni3	0.6667	0.3333	0.34602 (9)	0.0064 (3)
O1	0.6298 (12)	0.6699 (11)	0.2845 (3)	0.0041 (9)
O2	−0.0070 (10)	0.6347 (13)	0.4453 (4)	0.0066 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Te1	0.00376 (19)	0.00376 (19)	0.0049 (3)	0.00188 (9)	0.000	0.000
Ni1	0.0046 (4)	0.0046 (4)	0.0027 (6)	0.00231 (18)	0.000	0.000
Ni2	0.0049 (3)	0.0049 (3)	0.0182 (13)	0.00244 (14)	0.000	0.000
Ni3	0.0041 (4)	0.0041 (4)	0.0111 (8)	0.00205 (18)	0.000	0.000
O1	0.0015 (17)	0.006 (2)	0.0038 (16)	0.0007 (16)	−0.0004 (12)	0.0005 (13)
O2	0.007 (2)	0.006 (2)	0.0068 (15)	0.0036 (17)	−0.0021 (14)	−0.0032 (14)

Geometric parameters (Å, º)

Te1—O2^i	1.923 (5)	Ni2—O1^vi	2.040 (6)
Te1—O2	1.923 (5)	Ni2—O1	2.040 (6)
Te1—O2^ii	1.923 (5)	Ni2—O1^vii	2.040 (6)
Te1—O1^i	1.956 (5)	Ni2—O2^iv	2.139 (7)
Te1—O1^ii	1.956 (5)	Ni2—O2^viii	2.139 (7)
Te1—O1	1.956 (5)	Ni2—O2^ix	2.139 (7)
Ni1—O2^iii	2.032 (6)	Ni3—O1^x	2.008 (6)
Ni1—O2^iv	2.032 (6)	Ni3—O1^xi	2.008 (6)
Ni1—O2^v	2.032 (6)	Ni3—O1	2.008 (6)
Ni1—O1^ii	2.148 (5)	Ni3—O2^xii	2.110 (5)
Ni1—O1	2.148 (5)	Ni3—O2^xiii	2.110 (5)
Ni1—O1^i	2.148 (5)	Ni3—O2^ii	2.110 (5)
O2^i—Te1—O2	97.00 (16)	O1^vi—Ni2—O2^viii	87.9 (3)
O2^i—Te1—O2^ii	97.00 (16)	O1—Ni2—O2^viii	166.9 (3)
O2—Te1—O2^ii	97.00 (16)	O1^vii—Ni2—O2^viii	89.9 (2)
O2^i—Te1—O1^i	169.85 (18)	O2^iv—Ni2—O2^viii	81.2 (3)
O2—Te1—O1^i	86.8 (2)	O1^vi—Ni2—O2^ix	166.9 (3)
O2^ii—Te1—O1^i	91.8 (2)	O1—Ni2—O2^ix	89.9 (2)
O2^i—Te1—O1^ii	86.8 (2)	O1^vii—Ni2—O2^ix	87.9 (3)
O2—Te1—O1^ii	91.8 (2)	O2^iv—Ni2—O2^ix	81.2 (3)
O2^ii—Te1—O1^ii	169.85 (18)	O2^viii—Ni2—O2^ix	81.2 (3)
O1^i—Te1—O1^ii	83.6 (2)	O1^x—Ni3—O1^xi	103.49 (17)
O2^i—Te1—O1	91.8 (2)	O1^x—Ni3—O1	103.49 (17)
O2—Te1—O1	169.85 (18)	O1^xi—Ni3—O1	103.49 (17)
O2^ii—Te1—O1	86.8 (2)	O1^x—Ni3—O2^xii	162.8 (3)
O1^i—Te1—O1	83.6 (2)	O1^xi—Ni3—O2^xii	80.65 (12)
O1^ii—Te1—O1	83.6 (2)	O1—Ni3—O2^xii	91.52 (18)
O2^iii—Ni1—O2^iv	103.96 (18)	O1^x—Ni3—O2^xiii	80.65 (12)
O2^iii—Ni1—O2^v	103.96 (18)	O1^xi—Ni3—O2^xiii	91.52 (17)
O2^iv—Ni1—O2^v	103.96 (18)	O1—Ni3—O2^xiii	162.8 (3)
O2^iii—Ni1—O1^ii	87.87 (13)	O2^xii—Ni3—O2^xiii	82.6 (2)
O2^iv—Ni1—O1^ii	89.53 (19)	O1^x—Ni3—O2^ii	91.52 (18)
O2^v—Ni1—O1^ii	159.0 (3)	O1^xi—Ni3—O2^ii	162.8 (3)
O2^iii—Ni1—O1	159.0 (3)	O1—Ni3—O2^ii	80.65 (12)
O2^iv—Ni1—O1	87.87 (13)	O2^xii—Ni3—O2^ii	82.6 (2)
O2^v—Ni1—O1	89.53 (19)	O2^xiii—Ni3—O2^ii	82.6 (2)
O1^ii—Ni1—O1	74.8 (2)	Te1—O1—Ni3	97.3 (2)
O2^iii—Ni1—O1^i	89.53 (19)	Te1—O1—Ni2	134.6 (3)
O2^iv—Ni1—O1^i	159.0 (3)	Te1—O1—Ni1	85.1 (3)
O2^v—Ni1—O1^i	87.87 (13)	Ni3—O1—Ni2	117.5 (3)
O1^ii—Ni1—O1^i	74.8 (2)	Ni3—O1—Ni1	131.4 (2)
O1—Ni1—O1^i	74.8 (2)	Ni2—O1—Ni1	91.6 (3)
O1^vi—Ni2—O1	99.5 (2)	Te1—O2—Ni1^xiv	122.0 (3)
O1^vi—Ni2—O1^vii	99.5 (2)	Te1—O2—Ni3^xv	95.0 (2)
O1—Ni2—O1^vii	99.5 (2)	Te1—O2—Ni2^xvi	137.6 (3)
O1^vi—Ni2—O2^iv	89.90 (19)	Ni1^xiv—O2—Ni3^xv	125.7 (2)
O1—Ni2—O2^iv	87.9 (3)	Ni1^xiv—O2—Ni2^xvi	92.1 (3)
O1^vii—Ni2—O2^iv	166.9 (3)	Ni3^xv—O2—Ni2^xvi	81.65 (18)

Symmetry codes: (i) −x+y, −x+1, z; (ii) −y+1, x−y+1, z; (iii) −x+y−2/3, −x+2/3, z−1/3; (iv) −y+4/3, x−y+5/3, z−1/3; (v) x+1/3, y−1/3, z−1/3; (vi) −x+y+1, −x+2, z; (vii) −y+2, x−y+1, z; (viii) x+4/3, y+2/3, z−1/3; (ix) −x+y+1/3, −x+2/3, z−1/3; (x) −y+1, x−y, z; (xi) −x+y+1, −x+1, z; (xii) x+1, y, z; (xiii) −x+y, −x, z; (xiv) x−1/3, y+1/3, z+1/3; (xv) x−1, y, z; (xvi) x−4/3, y−2/3, z+1/3.