Neodymium(III) molybdenum(VI) borate, NdBO(2)MoO(4).

Single crystals of NdBO(2)MoO(4) were obtained from a molybdenum oxide-boron oxide flux under an air atmosphere. The structure features double chains of edge- and face-sharing distorted [NdO(10)] bicapped square-anti-prisms, which are linked by rows of isolated [MoO(4)] tetra-hedra and by zigzag chains of corner-sharing [BO(3)] groups, all of them running along the b axis. The chains of [NdO(10)], chains of [BO(3)] and rows of [MoO(4)] groups are arranged in layers parallel to the bc plane.

Related literature

A rough investigation of subsolidus phase relations in the pseudo-ternary system Nd2O3 – B2O3 – MoO3 has been reported by Lysanova et al. (1983 ▶) and Dzhurinskii & Lysanova (1998 ▶). X-ray powder diffraction data of LnBO2MoO4 (Ln = La, Ce, Pr, Nd) are given by Lysanova et al. (1983 ▶). The occurrence of a structural phase transition of LaBO2MoO4 was reported by Becker et al. (2008 ▶). For determinations of related structures, see: Palkina et al. (1979 ▶); Zhao et al. (2008 ▶, 2009 ▶) for LaBO2MoO4; Zhao et al. (2008 ▶) for CeBO2MoO4.

Experimental

Crystal data

NdMoBO6

M = 346.99

Monoclinic,

a = 10.1218 (19) Å

b = 4.1420 (5) Å

c = 11.896 (3) Å

β = 116.897 (14)°

V = 444.78 (16) Å3

Z = 4

Mo Kα radiation

μ = 14.30 mm−1

T = 292 K

0.30 × 0.20 × 0.15 mm

Data collection

Enraf–Nonius CAD-4/MACH3 diffractometer

Absorption correction: ψ scan (MolEN; Fair, 1990 ▶) T min = 0.487, T max = 0.998

5004 measured reflections

1344 independent reflections

1268 reflections with I > 2σ(I)

R int = 0.035

3 standard reflections every 100 reflections intensity decay: 2.1%

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.063

S = 1.22

1344 reflections

83 parameters

Δρmax = 2.24 e Å−3

Δρmin = −1.61 e Å−3

Data collection: MACH3 (Enraf–Nonius, 1993 ▶); cell refinement: MACH3; data reduction: MolEN (Fair, 1990 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ATOMS (Dowty, 2002 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811017806/fi2107sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811017806/fi2107Isup2.hkl

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

NdMoBO6	F(000) = 620
Mr = 346.99	Dx = 5.182 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 10.1218 (19) Å	θ = 12.1–21.2°
b = 4.1420 (5) Å	µ = 14.30 mm−1
c = 11.896 (3) Å	T = 292 K
β = 116.897 (14)°	Prism, light violet
V = 444.78 (16) Å3	0.30 × 0.20 × 0.15 mm
Z = 4

Enraf–Nonius CAD4/MACH3 diffractometer	1268 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.035
graphite	θmax = 30.4°, θmin = 2.3°
ω/2θ scans	h = −14→14
Absorption correction: ψ scan (MolEN; Fair, 1990)	k = −5→5
Tmin = 0.487, Tmax = 0.998	l = −16→16
5004 measured reflections	3 standard reflections every 100 reflections
1344 independent reflections	intensity decay: 2.1%

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025	w = 1/[σ2(Fo2) + (0.0304P)2 + 1.8082P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.063	(Δ/σ)max < 0.001
S = 1.22	Δρmax = 2.24 e Å−3
1344 reflections	Δρmin = −1.61 e Å−3
83 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraints	Extinction coefficient: 0.0428 (13)

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 is done 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 >2 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.

	x	y	z	Uiso*/Ueq
Nd	0.19204 (2)	0.21132 (6)	−0.47183 (2)	0.00919 (11)
Mo	0.64536 (4)	0.30466 (8)	−0.31742 (3)	0.00668 (12)
B	−0.0028 (7)	0.3290 (12)	−0.3083 (5)	0.0182 (10)
O1	−0.0326 (4)	0.6580 (8)	−0.3013 (3)	0.0120 (6)
O2	−0.0035 (3)	0.2247 (7)	−0.4150 (3)	0.0099 (5)
O3	0.6616 (4)	0.7223 (8)	−0.3016 (4)	0.0173 (7)
O4	0.2605 (4)	−0.2856 (7)	−0.3501 (3)	0.0124 (6)
O5	0.4556 (4)	0.2256 (9)	−0.3956 (3)	0.0156 (6)
O6	0.7424 (4)	0.2194 (9)	−0.4084 (4)	0.0190 (7)

	U11	U22	U33	U12	U13	U23
Nd	0.00733 (14)	0.00900 (16)	0.00992 (14)	−0.00094 (6)	0.00274 (10)	−0.00205 (7)
Mo	0.00602 (17)	0.0087 (2)	0.00546 (17)	−0.00022 (10)	0.00270 (13)	−0.00094 (10)
B	0.040 (3)	0.007 (2)	0.013 (2)	0.0020 (19)	0.017 (2)	−0.0003 (17)
O1	0.0259 (16)	0.0056 (13)	0.0050 (12)	−0.0010 (11)	0.0074 (12)	−0.0004 (10)
O2	0.0108 (13)	0.0118 (14)	0.0084 (13)	−0.0018 (10)	0.0055 (11)	−0.0021 (10)
O3	0.0203 (16)	0.0125 (15)	0.0199 (16)	0.0003 (12)	0.0099 (14)	−0.0002 (12)
O4	0.0173 (15)	0.0091 (14)	0.0067 (13)	−0.0007 (10)	0.0018 (12)	−0.0017 (10)
O5	0.0066 (12)	0.0235 (17)	0.0137 (15)	−0.0009 (11)	0.0019 (11)	−0.0008 (12)
O6	0.0271 (18)	0.0192 (17)	0.0207 (17)	−0.0024 (13)	0.0197 (15)	−0.0039 (13)

Nd—O2	2.364 (3)	B—O2	1.338 (6)
Nd—O5	2.399 (3)	B—O1ix	1.381 (6)
Nd—O4	2.431 (3)	B—O1	1.406 (6)
Nd—O4i	2.452 (3)	B—Ndii	3.099 (6)
Nd—O1ii	2.498 (3)	B—Ndiii	3.315 (6)
Nd—O2iii	2.528 (3)	O1—Bx	1.381 (6)
Nd—O6iv	2.551 (3)	O1—Ndii	2.498 (3)
Nd—O3v	2.901 (4)	O2—Ndiii	2.528 (3)
Nd—O2ii	2.930 (3)	O2—Ndii	2.930 (3)
Nd—O6vi	2.981 (4)	O3—Moi	2.419 (3)
Mo—O3	1.740 (4)	O3—Ndvii	2.901 (4)
Mo—O5	1.745 (3)	O4—Mov	1.816 (3)
Mo—O6	1.795 (3)	O4—Ndviii	2.452 (3)
Mo—O4vii	1.816 (3)	O6—Ndiv	2.551 (3)
Mo—O3viii	2.419 (3)	O6—Ndvi	2.981 (4)
Mo—Ndvii	3.5017 (8)
O2—Nd—O5	145.40 (12)	O4vii—Mo—Ndvi	128.02 (11)
O2—Nd—O4	84.21 (11)	O3viii—Mo—Ndvi	120.27 (9)
O5—Nd—O4	80.04 (12)	Ndvii—Mo—Ndvi	103.052 (17)
O2—Nd—O4i	81.98 (11)	Ndv—Mo—Ndvi	135.816 (15)
O5—Nd—O4i	77.71 (12)	O3—Mo—Nd	99.98 (12)
O4—Nd—O4i	116.06 (13)	O5—Mo—Nd	7.61 (12)
O2—Nd—O1ii	95.08 (11)	O6—Mo—Nd	121.06 (13)
O5—Nd—O1ii	117.89 (12)	O4vii—Mo—Nd	113.32 (11)
O4—Nd—O1ii	134.27 (11)	O3viii—Mo—Nd	87.93 (9)
O4i—Nd—O1ii	109.02 (10)	Ndvii—Mo—Nd	114.650 (15)
O2—Nd—O2iii	68.97 (12)	Ndv—Mo—Nd	105.813 (15)
O5—Nd—O2iii	131.40 (11)	Ndvi—Mo—Nd	116.653 (16)
O4—Nd—O2iii	69.84 (11)	O3—Mo—Ndiv	122.17 (12)
O4i—Nd—O2iii	149.91 (11)	O5—Mo—Ndiv	102.87 (12)
O1ii—Nd—O2iii	67.44 (11)	O6—Mo—Ndiv	20.25 (12)
O2—Nd—O6iv	129.71 (11)	O4vii—Mo—Ndiv	113.64 (11)
O5—Nd—O6iv	72.70 (12)	O3viii—Mo—Ndiv	60.20 (9)
O4—Nd—O6iv	70.40 (12)	Ndvii—Mo—Ndiv	134.533 (16)
O4i—Nd—O6iv	148.09 (12)	Ndv—Mo—Ndiv	94.773 (16)
O1ii—Nd—O6iv	75.67 (12)	Ndvi—Mo—Ndiv	60.259 (12)
O2iii—Nd—O6iv	61.79 (10)	Nd—Mo—Ndiv	110.359 (15)
O2—Nd—O3v	75.40 (11)	O2—B—O1ix	128.1 (4)
O5—Nd—O3v	70.07 (11)	O2—B—O1	117.4 (4)
O4—Nd—O3v	58.78 (10)	O1ix—B—Ndii	155.4 (4)
O4i—Nd—O3v	57.31 (10)	O1ix—B—Ndiii	102.0 (3)
O1ii—Nd—O3v	163.84 (10)	O1—B—Ndiii	129.6 (4)
O2iii—Nd—O3v	119.20 (10)	Ndii—B—Ndiii	80.37 (14)
O6iv—Nd—O3v	120.47 (11)	O1ix—B—Nd	120.0 (3)
O2—Nd—O2ii	69.96 (11)	O1—B—Nd	111.8 (3)
O5—Nd—O2ii	122.40 (10)	Ndii—B—Nd	84.34 (13)
O4—Nd—O2ii	154.13 (10)	Ndiii—B—Nd	74.17 (11)
O4i—Nd—O2ii	62.95 (10)	O2—B—Ndxi	144.1 (4)
O1ii—Nd—O2ii	50.40 (10)	O1—B—Ndxi	90.2 (3)
O2iii—Nd—O2ii	98.46 (10)	Ndii—B—Ndxi	142.25 (16)
O6iv—Nd—O2ii	125.50 (11)	Ndiii—B—Ndxi	132.90 (16)
O3v—Nd—O2ii	113.50 (9)	Nd—B—Ndxi	117.93 (18)
O2—Nd—O6vi	120.96 (10)	Bx—O1—B	125.6 (3)
O5—Nd—O6vi	73.22 (11)	Bx—O1—Ndii	132.3 (3)
O4—Nd—O6vi	152.84 (11)	B—O1—Ndii	101.4 (3)
O4i—Nd—O6vi	62.98 (10)	Bx—O1—Ndxi	57.4 (2)
O1ii—Nd—O6vi	59.13 (11)	B—O1—Ndxi	68.4 (3)
O2iii—Nd—O6vi	126.02 (10)	Ndii—O1—Ndxi	169.04 (12)
O6iv—Nd—O6vi	96.66 (11)	Bx—O1—Nd	137.1 (3)
O3v—Nd—O6vi	114.35 (10)	B—O1—Nd	49.7 (3)
O2ii—Nd—O6vi	52.35 (9)	Ndii—O1—Nd	78.20 (8)
O3—Mo—O5	105.76 (17)	Ndxi—O1—Nd	96.89 (8)
O3—Mo—O6	102.12 (17)	B—O2—Nd	129.3 (3)
O5—Mo—O6	114.36 (17)	B—O2—Ndiii	114.5 (3)
O3—Mo—O4vii	96.26 (16)	Nd—O2—Ndiii	111.03 (12)
O5—Mo—O4vii	116.79 (16)	B—O2—Ndii	84.3 (3)
O6—Mo—O4vii	117.52 (17)	Nd—O2—Ndii	110.04 (11)
O3—Mo—O3viii	169.5 (2)	Ndiii—O2—Ndii	98.46 (10)
O5—Mo—O3viii	82.75 (15)	Mo—O3—Moi	169.5 (2)
O6—Mo—O3viii	79.30 (15)	Mo—O3—Ndvii	94.65 (15)
O4vii—Mo—O3viii	74.10 (13)	Moi—O3—Ndvii	94.88 (12)
O3—Mo—Ndvii	55.67 (13)	Mo—O3—Ndvi	92.60 (14)
O5—Mo—Ndvii	121.91 (12)	Moi—O3—Ndvi	84.42 (10)
O6—Mo—Ndvii	123.02 (13)	Ndvii—O3—Ndvi	131.41 (12)
O4vii—Mo—Ndvii	40.63 (10)	Mov—O4—Nd	110.25 (14)
O3viii—Mo—Ndvii	114.71 (9)	Mov—O4—Ndviii	133.69 (16)
O3—Mo—Ndv	123.03 (13)	Nd—O4—Ndviii	116.06 (13)
O5—Mo—Ndv	105.84 (12)	Mov—O4—Ndiii	117.45 (14)
O6—Mo—Ndv	106.15 (13)	Nd—O4—Ndiii	71.19 (8)
O4vii—Mo—Ndv	26.80 (10)	Ndviii—O4—Ndiii	78.89 (8)
O3viii—Mo—Ndv	47.32 (9)	Mo—O5—Nd	166.9 (2)
Ndvii—Mo—Ndv	67.430 (16)	Mo—O6—Ndiv	145.65 (19)
O3—Mo—Ndvi	62.27 (12)	Mo—O6—Ndvi	115.69 (16)
O5—Mo—Ndvi	114.60 (12)	Ndiv—O6—Ndvi	96.66 (11)
O6—Mo—Ndvi	41.02 (12)