The mixed-metal nitridophosphate Na3TiN(PO3)3

Zatovsky, I.V.; Vorobjova, T.V.; Domasevitch, K.V.; Ogorodnyk, I.V.; Slobodyanik, N.S.

doi:10.1107/S1600536806002376

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The mixed-metal nitridophosphate Na₃TiN(PO₃)₃

I. V. Zatovsky, T. V. Vorobjova, K. V. Domasevitch, I. V. Ogorodnyk and N. S. Slobodyanik

The title compound, trisodium titanium nitride tris(phosphate), is built up from Ti^IIIO₆ octahedra linked together via [N(PO₃)₃] groups, the latter arising from three PO₃N tetrahedra sharing an N vertex. Three sodium cations complete the structure, which is also found for Na₃AlN(PO₃)₃. All the metal cations and the N atom occupy special positions with site symmetry 3.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806002376/hb2002sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806002376/hb2002Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (P-N) = 0.004 Å
R factor = 0.032
wR factor = 0.079
Data-to-parameter ratio = 7.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT089_ALERT_3_C Poor Data / Parameter Ratio (Zmax .LT. 18) .....       7.87

Alert level G
REFLT03_ALERT_4_G  WARNING: Large fraction of Friedel related reflns may
                     be needed to determine absolute structure
           From the CIF: _diffrn_reflns_theta_max           27.96
           From the CIF: _reflns_number_total                409
           Count of symmetry unique reflns          409
           Completeness (_total/calc)            100.00%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured         0
           Fraction of Friedel pairs measured     0.000
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   1 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
   0 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: PROFIT (Streltsov & Zavodnik, 1989); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).

trisodium titanium nitride tris(phosphate) top

Crystal data top

Na₃TiN(PO₃)₃	D_x = 2.851 Mg m⁻³
M_r = 367.79	Mo Kα radiation, λ = 0.71073 Å
Cubic, P2₁3	Cell parameters from 25 reflections
Hall symbol: P 2ac 2ab 3	θ = 3.0–28°
a = 9.4984 (10) Å	µ = 1.75 mm⁻¹
V = 856.94 (16) Å³	T = 298 K
Z = 4	Tetrahedron, violet
F(000) = 716	0.10 × 0.10 × 0.10 mm

Data collection top

Enraf–Nonius CAD-4 diffractometer	R_int = 0.075
Graphite monochromator	θ_max = 28.0°, θ_min = 3.0°
non–profiled ω/2θ scans	h = 0→12
Absorption correction: analytical (Alcock, 1970)	k = 0→12
T_min = 0.758, T_max = 0.812	l = 0→12
1209 measured reflections	2 standard reflections every 122 reflections
409 independent reflections	intensity decay: 1%
338 reflections with I > 2σ(I)

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0319P)²] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.032	(Δ/σ)_max < 0.001
wR(F²) = 0.079	Δρ_max = 0.47 e Å⁻³
S = 1.06	Δρ_min = −0.52 e Å⁻³
409 reflections	Absolute structure: Flack (1983), xxx Friedel pairs
52 parameters	Absolute structure parameter: 0.11 (10)

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Na1	−0.2614 (3)	0.7386 (3)	0.7386 (3)	0.0255 (9)
Na2	0.1423 (2)	0.6423 (2)	0.8577 (2)	0.0181 (8)
Na3	−0.0518 (3)	0.9482 (3)	0.9482 (3)	0.0290 (11)
Ti1	0.33070 (9)	0.83070 (9)	0.66930 (9)	0.0109 (3)
P1	0.00415 (13)	0.83568 (14)	0.58270 (13)	0.0092 (3)
N1	0.0515 (4)	0.9485 (4)	0.4485 (4)	0.0087 (14)
O1	−0.0986 (4)	0.7293 (4)	0.5200 (4)	0.0154 (8)
O2	0.1372 (4)	0.7568 (4)	0.6237 (4)	0.0124 (8)
O3	−0.0615 (4)	0.9181 (4)	0.7002 (4)	0.0170 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.0255 (9)	0.0255 (9)	0.0255 (9)	0.0050 (11)	0.0050 (11)	0.0050 (11)
Na2	0.0181 (8)	0.0181 (8)	0.0181 (8)	−0.0031 (8)	0.0031 (8)	0.0031 (8)
Na3	0.0290 (11)	0.0290 (11)	0.0290 (11)	−0.0026 (10)	−0.0026 (10)	−0.0026 (10)
Ti1	0.0109 (3)	0.0109 (3)	0.0109 (3)	0.0002 (4)	−0.0002 (4)	−0.0002 (4)
P1	0.0096 (5)	0.0105 (6)	0.0076 (6)	−0.0004 (5)	0.0006 (5)	0.0005 (6)
N1	0.0087 (14)	0.0087 (14)	0.0087 (14)	−0.0031 (15)	−0.0031 (15)	0.0031 (15)
O1	0.0168 (17)	0.0179 (18)	0.0114 (17)	−0.0051 (17)	−0.0003 (15)	0.0016 (15)
O2	0.0124 (18)	0.0094 (16)	0.0155 (18)	−0.0009 (13)	−0.0012 (14)	0.0010 (14)
O3	0.0225 (19)	0.0162 (18)	0.0123 (18)	0.0050 (18)	0.0054 (15)	−0.0012 (16)

Geometric parameters (Å, º) top

Na1—O3ⁱ	2.578 (5)	Na3—O1^ix	3.043 (5)
Na1—O3ⁱⁱ	2.578 (5)	Na3—O2^viii	3.117 (5)
Na1—O3	2.578 (5)	Na3—O2^vi	3.117 (5)
Na1—O1ⁱ	2.590 (5)	Na3—O2^ix	3.117 (5)
Na1—O1ⁱⁱ	2.590 (5)	Ti1—O1^x	2.002 (4)
Na1—O1	2.590 (5)	Ti1—O1^xi	2.002 (4)
Na1—N1ⁱⁱⁱ	3.078 (5)	Ti1—O1^xii	2.002 (4)
Na2—O3^iv	2.330 (4)	Ti1—O2^vi	2.015 (4)
Na2—O3ⁱⁱ	2.330 (4)	Ti1—O2^vii	2.015 (4)
Na2—O3^v	2.330 (4)	Ti1—O2	2.015 (4)
Na2—O2^vi	2.475 (4)	P1—O3	1.499 (4)
Na2—O2^vii	2.475 (4)	P1—O2	1.520 (4)
Na2—O2	2.475 (4)	P1—O1	1.526 (4)
Na2—N1^v	3.188 (4)	P1—N1	1.725 (4)
Na3—O3ⁱ	2.375 (5)	N1—P1^xi	1.725 (4)
Na3—O3ⁱⁱ	2.375 (5)	N1—P1^xiii	1.725 (4)
Na3—O3	2.375 (5)	O1—Ti1ⁱⁱⁱ	2.002 (4)
Na3—O1^viii	3.043 (5)	O3—Na2^ix	2.330 (4)
Na3—O1^vi	3.043 (5)

O3ⁱ—Na1—O3ⁱⁱ	73.21 (16)	O3ⁱ—Na3—O2^viii	83.44 (14)
O3ⁱ—Na1—O3	73.21 (16)	O3ⁱⁱ—Na3—O2^viii	75.64 (14)
O3ⁱⁱ—Na1—O3	73.21 (16)	O3—Na3—O2^viii	153.25 (16)
O3ⁱ—Na1—O1ⁱ	57.96 (13)	O1^viii—Na3—O2^viii	47.07 (11)
O3ⁱⁱ—Na1—O1ⁱ	129.78 (17)	O1^vi—Na3—O2^viii	77.09 (12)
O3—Na1—O1ⁱ	101.00 (14)	O1^ix—Na3—O2^viii	103.76 (13)
O3ⁱ—Na1—O1ⁱⁱ	101.00 (14)	O3ⁱ—Na3—O2^vi	153.25 (16)
O3ⁱⁱ—Na1—O1ⁱⁱ	57.96 (13)	O3ⁱⁱ—Na3—O2^vi	83.44 (14)
O3—Na1—O1ⁱⁱ	129.78 (17)	O3—Na3—O2^vi	75.64 (14)
O1ⁱ—Na1—O1ⁱⁱ	118.13 (6)	O1^viii—Na3—O2^vi	103.76 (13)
O3ⁱ—Na1—O1	129.78 (17)	O1^vi—Na3—O2^vi	47.07 (11)
O3ⁱⁱ—Na1—O1	101.00 (14)	O1^ix—Na3—O2^vi	77.09 (12)
O3—Na1—O1	57.96 (13)	O2^viii—Na3—O2^vi	113.19 (13)
O1ⁱ—Na1—O1	118.13 (6)	O3ⁱ—Na3—O2^ix	75.64 (14)
O1ⁱⁱ—Na1—O1	118.13 (6)	O3ⁱⁱ—Na3—O2^ix	153.25 (16)
O3ⁱ—Na1—N1ⁱⁱⁱ	136.50 (15)	O3—Na3—O2^ix	83.44 (14)
O3ⁱⁱ—Na1—N1ⁱⁱⁱ	136.50 (15)	O1^viii—Na3—O2^ix	77.09 (12)
O3—Na1—N1ⁱⁱⁱ	136.50 (15)	O1^vi—Na3—O2^ix	103.76 (13)
O1ⁱ—Na1—N1ⁱⁱⁱ	82.08 (13)	O1^ix—Na3—O2^ix	47.07 (11)
O1ⁱⁱ—Na1—N1ⁱⁱⁱ	82.08 (13)	O2^viii—Na3—O2^ix	113.19 (13)
O1—Na1—N1ⁱⁱⁱ	82.08 (13)	O2^vi—Na3—O2^ix	113.19 (13)
O3^iv—Na2—O3ⁱⁱ	89.55 (16)	O1^x—Ti1—O1^xi	92.86 (16)
O3^iv—Na2—O3^v	89.55 (16)	O1^x—Ti1—O1^xii	92.86 (16)
O3ⁱⁱ—Na2—O3^v	89.55 (16)	O1^xi—Ti1—O1^xii	92.86 (16)
O3^iv—Na2—O2^vi	100.06 (13)	O1^x—Ti1—O2^vi	88.90 (14)
O3ⁱⁱ—Na2—O2^vi	100.56 (12)	O1^xi—Ti1—O2^vi	90.78 (15)
O3^v—Na2—O2^vi	166.02 (17)	O1^xii—Ti1—O2^vi	175.87 (17)
O3^iv—Na2—O2^vii	100.56 (12)	O1^x—Ti1—O2^vii	90.78 (15)
O3ⁱⁱ—Na2—O2^vii	166.02 (17)	O1^xi—Ti1—O2^vii	175.87 (17)
O3^v—Na2—O2^vii	100.06 (13)	O1^xii—Ti1—O2^vii	88.90 (14)
O2^vi—Na2—O2^vii	68.36 (15)	O2^vi—Ti1—O2^vii	87.34 (16)
O3^iv—Na2—O2	166.02 (17)	O1^x—Ti1—O2	175.87 (17)
O3ⁱⁱ—Na2—O2	100.06 (13)	O1^xi—Ti1—O2	88.90 (14)
O3^v—Na2—O2	100.56 (12)	O1^xii—Ti1—O2	90.78 (15)
O2^vi—Na2—O2	68.36 (15)	O2^vi—Ti1—O2	87.34 (16)
O2^vii—Na2—O2	68.36 (15)	O2^vii—Ti1—O2	87.34 (16)
O3^iv—Na2—N1^v	54.43 (12)	O3—P1—O2	114.4 (2)
O3ⁱⁱ—Na2—N1^v	54.43 (12)	O3—P1—O1	111.7 (2)
O3^v—Na2—N1^v	54.43 (12)	O2—P1—O1	107.8 (2)
O2^vi—Na2—N1^v	139.54 (13)	O3—P1—N1	109.5 (2)
O2^vii—Na2—N1^v	139.54 (13)	O2—P1—N1	106.2 (2)
O2—Na2—N1^v	139.54 (13)	O1—P1—N1	106.8 (2)
O3ⁱ—Na3—O3ⁱⁱ	80.7 (2)	P1^xi—N1—P1^xiii	115.35 (17)
O3ⁱ—Na3—O3	80.7 (2)	P1^xi—N1—P1	115.35 (17)
O3ⁱⁱ—Na3—O3	80.7 (2)	P1^xiii—N1—P1	115.35 (17)
O3ⁱ—Na3—O1^viii	102.84 (15)	P1—O1—Ti1ⁱⁱⁱ	138.9 (2)
O3ⁱⁱ—Na3—O1^viii	120.77 (16)	P1—O1—Na1	92.66 (19)
O3—Na3—O1^viii	158.54 (17)	Ti1ⁱⁱⁱ—O1—Na1	122.0 (2)
O3ⁱ—Na3—O1^vi	158.54 (17)	P1—O2—Ti1	129.9 (2)
O3ⁱⁱ—Na3—O1^vi	102.84 (15)	P1—O2—Na2	117.6 (2)
O3—Na3—O1^vi	120.77 (16)	Ti1—O2—Na2	86.69 (14)
O1^viii—Na3—O1^vi	56.94 (11)	P1—O3—Na2^ix	116.0 (2)
O3ⁱ—Na3—O1^ix	120.77 (16)	P1—O3—Na3	141.7 (2)
O3ⁱⁱ—Na3—O1^ix	158.54 (17)	Na2^ix—O3—Na3	97.87 (16)
O3—Na3—O1^ix	102.84 (15)	P1—O3—Na1	93.80 (19)
O1^viii—Na3—O1^ix	56.94 (11)	Na2^ix—O3—Na1	113.29 (17)
O1^vi—Na3—O1^ix	56.94 (11)	Na3—O3—Na1	88.16 (15)

O3—Na1—O1—Ti1ⁱⁱⁱ	−145.0 (2)	Ti1ⁱⁱⁱ—O1—P1—O3	130.7 (4)
O3ⁱⁱ—Na1—O1—Ti1ⁱⁱⁱ	153.0 (2)	Na1—O1—P1—O3	−18.5 (2)
O3ⁱ—Na1—O1—Ti1ⁱⁱⁱ	−129.8 (2)	Ti1ⁱⁱⁱ—O1—P1—O2	−102.8 (4)
O1ⁱ—Na1—O1—Ti1ⁱⁱⁱ	−59.6 (3)	Na1—O1—P1—O2	108.00 (18)
O1ⁱⁱ—Na1—O1—Ti1ⁱⁱⁱ	93.6 (2)	Ti1ⁱⁱⁱ—O1—P1—N1	11.0 (4)
O3^v—Na2—O2—P1	92.1 (2)	Na1—O1—P1—N1	−138.3 (3)
O3^iv—Na2—O2—P1	−132.2 (5)	P1^xi—N1—P1—O3	56.9 (4)
O3ⁱⁱ—Na2—O2—P1	0.6 (2)	P1^xiii—N1—P1—O3	−81.6 (4)
O2^vi—Na2—O2—P1	−96.8 (3)	P1^xi—N1—P1—O2	−67.1 (4)
O2^vii—Na2—O2—P1	−171.2 (3)	P1^xiii—N1—P1—O2	154.4 (3)
O3^v—Na2—O2—Ti1	−133.91 (14)	P1^xi—N1—P1—O1	178.1 (3)
O3^iv—Na2—O2—Ti1	1.8 (6)	P1^xiii—N1—P1—O1	39.6 (4)
O3ⁱⁱ—Na2—O2—Ti1	134.65 (14)	P1—O2—Ti1—O1^xii	−103.7 (3)
O2^vi—Na2—O2—Ti1	37.19 (13)	Na2—O2—Ti1—O1^xii	132.59 (13)
O2^vii—Na2—O2—Ti1	−37.19 (13)	P1—O2—Ti1—O1^xi	−10.8 (3)
O3ⁱ—Na3—O3—P1	−134.7 (4)	Na2—O2—Ti1—O1^xi	−134.56 (15)
O3ⁱⁱ—Na3—O3—P1	−52.8 (5)	P1—O2—Ti1—O2^vii	167.5 (3)
O3ⁱ—Na3—O3—Na2^ix	72.3 (2)	Na2—O2—Ti1—O2^vii	43.73 (7)
O3ⁱⁱ—Na3—O3—Na2^ix	154.23 (14)	P1—O2—Ti1—O2^vi	80.0 (4)
O3ⁱ—Na3—O3—Na1	−40.99 (8)	Na2—O2—Ti1—O2^vi	−43.73 (7)
O3ⁱⁱ—Na3—O3—Na1	40.99 (8)	O3^v—Na2—Ti1—O1^xii	−1.08 (16)
O3ⁱⁱ—Na1—O3—P1	103.2 (3)	O3^iv—Na2—Ti1—O1^xii	118.92 (16)
O3ⁱ—Na1—O3—P1	−179.7 (2)	O3ⁱⁱ—Na2—Ti1—O1^xii	−121.08 (16)
O1ⁱ—Na1—O3—P1	−128.31 (19)	O2^vi—Na2—Ti1—O1^xii	178.38 (19)
O1—Na1—O3—P1	−11.88 (15)	O2^vii—Na2—Ti1—O1^xii	58.38 (19)
O1ⁱⁱ—Na1—O3—P1	89.8 (2)	O2—Na2—Ti1—O1^xii	−61.62 (19)
O3ⁱⁱ—Na1—O3—Na2^ix	−136.29 (15)	O3^v—Na2—Ti1—O1^x	−121.08 (16)
O3ⁱ—Na1—O3—Na2^ix	−59.2 (2)	O3^iv—Na2—Ti1—O1^x	−1.08 (16)
O1ⁱ—Na1—O3—Na2^ix	−7.8 (2)	O3ⁱⁱ—Na2—Ti1—O1^x	118.92 (16)
O1—Na1—O3—Na2^ix	108.62 (19)	O2^vi—Na2—Ti1—O1^x	58.38 (19)
O1ⁱⁱ—Na1—O3—Na2^ix	−149.70 (18)	O2^vii—Na2—Ti1—O1^x	−61.62 (19)
O3ⁱⁱ—Na1—O3—Na3	−38.52 (14)	O2—Na2—Ti1—O1^x	178.38 (19)
O3ⁱ—Na1—O3—Na3	38.52 (14)	O3^v—Na2—Ti1—O1^xi	118.92 (16)
O1ⁱ—Na1—O3—Na3	89.96 (15)	O3^iv—Na2—Ti1—O1^xi	−121.08 (16)
O1—Na1—O3—Na3	−153.62 (17)	O3ⁱⁱ—Na2—Ti1—O1^xi	−1.08 (16)
O1ⁱⁱ—Na1—O3—Na3	−51.9 (2)	O2^vi—Na2—Ti1—O1^xi	−61.62 (19)
P1ⁱ—Na1—O3—Na3	67.20 (10)	O2^vii—Na2—Ti1—O1^xi	178.38 (19)
P1—Na1—O3—Na3	−141.7 (2)	O2—Na2—Ti1—O1^xi	58.38 (19)
P1ⁱⁱ—Na1—O3—Na3	−38.65 (12)	O3^v—Na2—Ti1—O2	60.55 (17)
Na2^ix—O3—P1—O2	137.5 (2)	O3^iv—Na2—Ti1—O2	−179.45 (17)
Na3—O3—P1—O2	−12.4 (5)	O3ⁱⁱ—Na2—Ti1—O2	−59.45 (17)
Na1—O3—P1—O2	−104.2 (2)	O2^vi—Na2—Ti1—O2	−120.0 (2)
Na2^ix—O3—P1—O1	−99.6 (2)	O2^vii—Na2—Ti1—O2	120.0 (2)
Na3—O3—P1—O1	110.4 (4)	O3^v—Na2—Ti1—O2^vii	−59.45 (17)
Na1—O3—P1—O1	18.6 (2)	O3^iv—Na2—Ti1—O2^vii	60.55 (17)
Na2^ix—O3—P1—N1	18.5 (3)	O3ⁱⁱ—Na2—Ti1—O2^vii	−179.45 (17)
Na3—O3—P1—N1	−131.4 (4)	O2^vi—Na2—Ti1—O2^vii	120.0 (2)
Na1—O3—P1—N1	136.80 (12)	O2—Na2—Ti1—O2^vii	−120.0 (2)
Ti1—O2—P1—O3	−70.9 (3)	O3^v—Na2—Ti1—O2^vi	−179.45 (17)
Na2—O2—P1—O3	39.7 (3)	O3^iv—Na2—Ti1—O2^vi	−59.45 (17)
Ti1—O2—P1—O1	164.1 (3)	O3ⁱⁱ—Na2—Ti1—O2^vi	60.55 (17)
Na2—O2—P1—O1	−85.3 (2)	O2^vii—Na2—Ti1—O2^vi	−120.0 (2)
Ti1—O2—P1—N1	49.9 (3)	O2—Na2—Ti1—O2^vi	120.0 (2)
Na2—O2—P1—N1	160.5 (2)

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

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