Sodium samarium tetra-kis-(poly-phosphate), NaSm(PO(3))(4).

NaSm(PO(3))(4) has been prepared by solid state reactions. It belongs to type II of the structural family of M(I)Ln(III)(PO(3))(4) compounds (M(I) = alkali metal and Ln(III) = rare earth metal) and is composed of (∞)(PO(3))(n)](n-) polyphosphate chains with a repeating unit of four PO(4) tetra-hedra. The chains extend parallel to [100] and share O atoms with irregular SmO(8) polyhedra, forming a three-dimensional framework which delimits tunnels occupied by Na(+) cations in a distorted octa-hedral environment.

Related literature

The unit cell of NaSm(PO3)4, derived from X-ray powder data, was reported by Ferid et al. (1984 ▶). For classification of M I Ln III(PO3)4 structures, see: Palkina et al. (1981 ▶); Durif (1995 ▶). Structures, properties and applications of other members of this family were discussed by Ettis et al. (2003 ▶); Parreu et al. (2007 ▶); Zhao et al. (2008 ▶, 2010 ▶); Zhu et al. (2009 ▶).

Experimental

Crystal data

NaSm(PO3)4

M = 489.22

Monoclinic,

a = 7.1924 (13) Å

b = 13.091 (2) Å

c = 9.8480 (17) Å

β = 90.396 (10)°

V = 927.2 (3) Å3

Z = 4

Mo Kα radiation

μ = 7.14 mm−1

T = 293 K

0.20 × 0.02 × 0.02 mm

Data collection

Rigaku Mercury70 CCD diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.329, T max = 0.870

7036 measured reflections

2111 independent reflections

1868 reflections with I > 2σ(I)

R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.037

wR(F 2) = 0.068

S = 1.15

2111 reflections

163 parameters

Δρmax = 2.38 e Å−3

Δρmin = −0.80 e Å−3

Data collection: CrystalClear (Rigaku, 2004 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶) and PLATON (Spek, 2009 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2004 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810022543/wm2360sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810022543/wm2360Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

NaSm(PO3)4	F(000) = 916
Mr = 489.22	Dx = 3.504 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2180 reflections
a = 7.1924 (13) Å	θ = 2.1–27.5°
b = 13.091 (2) Å	µ = 7.14 mm−1
c = 9.8480 (17) Å	T = 293 K
β = 90.396 (10)°	Prism, yellow
V = 927.2 (3) Å3	0.20 × 0.02 × 0.02 mm
Z = 4

Rigaku Mercury70 CCD diffractometer	2111 independent reflections
Radiation source: fine-focus sealed tube	1868 reflections with I > 2σ(I)
Rigaku Graphite Monochromator DIFFRACTOMETER TYPE	Rint = 0.041
Detector resolution: 14.6306 pixels mm-1	θmax = 27.5°, θmin = 2.6°
ω scans	h = −9→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −15→17
Tmin = 0.329, Tmax = 0.870	l = −12→12
7036 measured reflections

Refinement on F2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.037	Secondary atom site location: difference Fourier map
wR(F2) = 0.068	w = 1/[σ2(Fo2) + (0.0639P)2] where P = (Fo2 + 2Fc2)/3
S = 1.15	(Δ/σ)max < 0.001
2111 reflections	Δρmax = 2.38 e Å−3
163 parameters	Δρmin = −0.80 e Å−3

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 F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > σ(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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	Uiso*/Ueq
Na1	−0.0002 (4)	0.7220 (2)	0.5648 (3)	0.0210 (6)
Sm1	0.51300 (4)	0.71807 (2)	0.47634 (3)	0.00716 (10)
P1	0.2493 (2)	0.60065 (11)	0.74392 (15)	0.0064 (3)
P2	0.8781 (2)	0.61480 (12)	0.26404 (15)	0.0063 (3)
P3	0.2690 (2)	0.59026 (12)	0.19783 (15)	0.0065 (3)
P4	0.6463 (2)	0.62775 (12)	0.80511 (15)	0.0065 (3)
O1	0.2374 (6)	0.6610 (3)	0.0824 (4)	0.0117 (9)
O2	0.7180 (5)	0.7105 (3)	0.8947 (4)	0.0099 (9)
O3	0.2829 (6)	0.4784 (3)	0.1343 (4)	0.0091 (9)
O4	0.8029 (6)	0.6454 (3)	0.3976 (4)	0.0095 (9)
O5	0.0936 (6)	0.6652 (3)	0.7951 (4)	0.0103 (9)
O6	0.0886 (6)	0.5804 (3)	0.2895 (4)	0.0105 (9)
O7	0.2159 (6)	0.4860 (3)	0.7898 (4)	0.0098 (9)
O8	0.6799 (6)	0.6328 (3)	0.6572 (4)	0.0100 (9)
O9	0.8672 (6)	0.6896 (3)	0.1519 (4)	0.0105 (9)
O10	0.2860 (6)	0.6073 (3)	0.5963 (4)	0.0102 (9)
O11	0.4284 (6)	0.6243 (3)	0.8331 (4)	0.0082 (9)
O12	0.4293 (6)	0.6102 (3)	0.2901 (4)	0.0135 (9)

	U11	U22	U33	U12	U13	U23
Na1	0.0172 (14)	0.0309 (16)	0.0149 (12)	0.0063 (13)	−0.0028 (11)	0.0029 (12)
Sm1	0.00640 (16)	0.00857 (15)	0.00651 (15)	−0.00002 (13)	0.00033 (11)	−0.00033 (13)
P1	0.0049 (7)	0.0065 (7)	0.0078 (7)	−0.0001 (6)	−0.0001 (6)	−0.0006 (6)
P2	0.0055 (7)	0.0053 (7)	0.0082 (7)	0.0002 (6)	0.0012 (6)	0.0002 (6)
P3	0.0046 (7)	0.0064 (7)	0.0084 (7)	0.0013 (6)	0.0000 (6)	−0.0001 (6)
P4	0.0053 (7)	0.0059 (7)	0.0084 (7)	−0.0007 (6)	0.0001 (6)	−0.0007 (6)
O1	0.010 (2)	0.013 (2)	0.012 (2)	0.0027 (18)	0.0012 (18)	0.0029 (18)
O2	0.005 (2)	0.009 (2)	0.016 (2)	−0.0013 (17)	−0.0032 (17)	−0.0044 (18)
O3	0.014 (2)	0.005 (2)	0.009 (2)	0.0016 (17)	−0.0019 (17)	−0.0014 (17)
O4	0.007 (2)	0.012 (2)	0.009 (2)	0.0009 (17)	0.0012 (17)	−0.0007 (17)
O5	0.005 (2)	0.013 (2)	0.013 (2)	0.0014 (17)	0.0020 (17)	−0.0007 (18)
O6	0.008 (2)	0.015 (2)	0.008 (2)	−0.0019 (18)	0.0034 (17)	0.0022 (18)
O7	0.014 (2)	0.005 (2)	0.011 (2)	−0.0042 (17)	−0.0001 (18)	−0.0013 (16)
O8	0.010 (2)	0.013 (2)	0.0064 (19)	0.0015 (18)	0.0028 (17)	0.0026 (17)
O9	0.011 (2)	0.008 (2)	0.012 (2)	0.0023 (17)	0.0018 (18)	0.0028 (17)
O10	0.012 (2)	0.010 (2)	0.009 (2)	−0.0015 (18)	0.0019 (18)	−0.0004 (17)
O11	0.007 (2)	0.010 (2)	0.0076 (19)	−0.0012 (17)	−0.0028 (17)	−0.0021 (16)
O12	0.008 (2)	0.015 (2)	0.017 (2)	−0.0020 (18)	−0.0044 (18)	−0.0047 (18)

Na1—O4i	2.386 (5)	P2—O6vii	1.598 (4)
Na1—O1ii	2.438 (5)	P3—O1	1.482 (4)
Na1—O2iii	2.468 (5)	P3—O12	1.486 (4)
Na1—O5	2.475 (5)	P3—O6	1.591 (4)
Na1—O10	2.565 (5)	P3—O3	1.596 (4)
Na1—O8i	2.741 (5)	P4—O8	1.479 (4)
Na1—O9ii	3.005 (5)	P4—O2	1.487 (4)
Sm1—O9ii	2.362 (4)	P4—O11	1.594 (4)
Sm1—O12	2.389 (4)	P4—O3vi	1.595 (4)
Sm1—O8	2.415 (4)	O1—Na1iv	2.438 (5)
Sm1—O5iv	2.423 (4)	O1—Sm1iii	2.486 (4)
Sm1—O4	2.424 (4)	O2—Sm1v	2.449 (4)
Sm1—O2iii	2.449 (4)	O2—Na1v	2.468 (5)
Sm1—O1v	2.486 (4)	O3—P4vi	1.595 (4)
Sm1—O10	2.488 (4)	O4—Na1vii	2.386 (5)
P1—O10	1.482 (4)	O5—Sm1ii	2.423 (4)
P1—O5	1.494 (4)	O6—P2i	1.598 (4)
P1—O11	1.584 (4)	O7—P2vi	1.574 (4)
P1—O7	1.586 (4)	O8—Na1vii	2.741 (5)
P2—O9	1.477 (4)	O9—Sm1iv	2.362 (4)
P2—O4	1.481 (4)	O9—Na1iv	3.005 (5)
P2—O7vi	1.574 (4)
O4i—Na1—O1ii	81.77 (16)	O10—P1—O5	115.9 (2)
O4i—Na1—O2iii	93.40 (16)	O10—P1—O11	112.5 (2)
O1ii—Na1—O2iii	108.62 (17)	O5—P1—O11	108.1 (2)
O4i—Na1—O5	131.55 (19)	O10—P1—O7	111.3 (2)
O1ii—Na1—O5	109.24 (16)	O5—P1—O7	108.9 (2)
O2iii—Na1—O5	123.97 (17)	O11—P1—O7	98.7 (2)
O4i—Na1—O10	108.05 (17)	O9—P2—O4	117.8 (2)
O1ii—Na1—O10	168.60 (18)	O9—P2—O7vi	106.5 (2)
O2iii—Na1—O10	77.17 (15)	O4—P2—O7vi	111.6 (2)
O5—Na1—O10	60.02 (14)	O9—P2—O6vii	110.5 (2)
O4i—Na1—O8i	63.56 (14)	O4—P2—O6vii	106.8 (2)
O1ii—Na1—O8i	65.92 (15)	O7vi—P2—O6vii	102.8 (2)
O2iii—Na1—O8i	156.55 (17)	O1—P3—O12	118.2 (3)
O5—Na1—O8i	78.01 (15)	O1—P3—O6	111.4 (2)
O10—Na1—O8i	112.69 (17)	O12—P3—O6	107.4 (2)
O4i—Na1—O9ii	151.14 (16)	O1—P3—O3	106.4 (2)
O1ii—Na1—O9ii	114.66 (17)	O12—P3—O3	110.5 (2)
O2iii—Na1—O9ii	59.56 (14)	O6—P3—O3	101.6 (2)
O5—Na1—O9ii	67.70 (14)	O8—P4—O2	119.5 (3)
O10—Na1—O9ii	59.17 (13)	O8—P4—O11	109.8 (2)
O8i—Na1—O9ii	143.89 (15)	O2—P4—O11	104.8 (2)
P1—Na1—O9ii	60.64 (10)	O8—P4—O3vi	110.7 (2)
O9ii—Sm1—O12	138.95 (15)	O2—P4—O3vi	107.7 (2)
O9ii—Sm1—O8	85.27 (14)	O11—P4—O3vi	102.9 (2)
O12—Sm1—O8	114.50 (15)	P3—O1—Sm1iii	144.7 (2)
O9ii—Sm1—O5iv	109.05 (14)	Na1iv—O1—Sm1iii	94.05 (16)
O12—Sm1—O5iv	82.37 (15)	P4—O2—Sm1v	140.3 (2)
O8—Sm1—O5iv	135.61 (14)	P4—O2—Na1v	116.4 (2)
O9ii—Sm1—O4	145.34 (14)	Sm1v—O2—Na1v	101.18 (16)
O12—Sm1—O4	74.63 (14)	P4vi—O3—P3	132.3 (3)
O8—Sm1—O4	68.31 (13)	P2—O4—Na1vii	120.5 (2)
O5iv—Sm1—O4	78.51 (14)	P2—O4—Sm1	135.3 (2)
O9ii—Sm1—O2iii	69.92 (14)	Na1vii—O4—Sm1	97.01 (16)
O12—Sm1—O2iii	76.16 (14)	P1—O5—Sm1ii	142.1 (2)
O8—Sm1—O2iii	147.54 (13)	P1—O5—Na1	93.5 (2)
O5iv—Sm1—O2iii	74.25 (14)	Sm1ii—O5—Na1	114.88 (18)
O4—Sm1—O2iii	142.17 (13)	P3—O6—P2i	131.6 (3)
O9ii—Sm1—O1v	69.91 (14)	P2vi—O7—P1	139.8 (3)
O12—Sm1—O1v	149.17 (14)	P4—O8—Sm1	131.5 (2)
O8—Sm1—O1v	70.50 (14)	P4—O8—Na1vii	119.3 (2)
O5iv—Sm1—O1v	75.54 (14)	Sm1—O8—Na1vii	88.43 (14)
O4—Sm1—O1v	80.05 (14)	P2—O9—Sm1iv	149.9 (3)
O2iii—Sm1—O1v	116.94 (14)	P2—O9—Na1iv	120.7 (2)
O9ii—Sm1—O10	69.79 (14)	Sm1iv—O9—Na1iv	89.30 (14)
O12—Sm1—O10	81.81 (14)	P1—O10—Sm1	128.5 (2)
O8—Sm1—O10	72.84 (14)	P1—O10—Na1	90.3 (2)
O5iv—Sm1—O10	151.45 (14)	Sm1—O10—Na1	97.49 (15)
O4—Sm1—O10	119.46 (14)	P1—O11—P4	135.0 (3)
O2iii—Sm1—O10	78.97 (14)	P3—O12—Sm1	139.8 (3)
O1v—Sm1—O10	126.71 (13)

Table 1

Selected bond lengths (Å)

P1—O10	1.482 (4)
P1—O5	1.494 (4)
P1—O11	1.584 (4)
P1—O7	1.586 (4)
P2—O9	1.477 (4)
P2—O4	1.481 (4)
P2—O7i	1.574 (4)
P2—O6ii	1.598 (4)
P3—O1	1.482 (4)
P3—O12	1.486 (4)
P3—O6	1.591 (4)
P3—O3	1.596 (4)
P4—O8	1.479 (4)
P4—O2	1.487 (4)
P4—O11	1.594 (4)
P4—O3i	1.595 (4)

Symmetry codes: (i) ; (ii) .