The double molybdate Na₉Sc(MoO₄)₆ refined from powder XRD data

Na₉Sc(MoO₄)₆ {nona­sodium scandium hexa­kis­[tetra­oxido­molybdate(II)]} was synthesised by a solid-state method. The basic structure units are polyhedral clusters composed of an ScO₆ octa­hedron and three NaO₆ octa­hedra sharing total edges. The clusters are connected by sharing vertices with bridging MoO₄ tetra­hedra, forming a three-dimensional framework where the cavities are occupied by the other two crystallographically independent Na atoms.

Computing details

Data collection: SMART (Bruker, 2002); cell refinement: GSAS (Larson & Von Dreele, 1994); data reduction: GSAS (Larson & Von Dreele, 1994); program(s) used to solve structure: GSAS (Larson & Von Dreele, 1994); program(s) used to refine structure: GSAS (Larson & Von Dreele, 1994); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999).

Nonasodium scandium hexakis[tetraoxidomolybdate(II)]

Crystal data

Na9Sc(MoO4)6	Z = 6
Mr = 1211.48	Dx = 3.224 Mg m^−3
Trigonal, R3	CuKα1, CuKα2 radiation, λ = 1.540562, 1.544390 Å
a = 15.0087 (3) Å	T = 295 K
c = 19.1943 (4) Å	white
V = 3744.5 (2) Å^3

Data collection

Bruker D8 ADVANCE diffractometer	Data collection mode: reflection
Radiation source: X-ray tube	Scan method: step
Secondary graphite monochromator	2θmin = 7°, 2θmax = 100°, 2θstep = 0.021°
Specimen mounting: packed powder pellet

Refinement

Least-squares matrix: full with fixed elements per cycle	Profile function: CW Profile function number 3 with 19 terms Pseudo-Voigt profile coefficients as parameterized in P. Thompson, D. E. Cox & J. B. Hastings (1987). J. Appl. Cryst. 20, 79–83. Asymmetry correction of L. W. Finger, D. E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst. 27, 892–900. #1(GU) = 0.000 #2(GV) = -4.046 #3(GW) = 5.017 #4(GP) = 0.000 #5(LX) = 2.919 #6(LY) = 5.208 #7(S/L) = 0.0005 #8(H/L) = 0.0243 #9(trns) = 1.30 #10(shft)= -1.4855 #11(stec)= 5.47 #12(ptec)= -0.69 #13(sfec)= 0.00 #14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000 #17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.036	62 parameters
Rwp = 0.046	Weighting scheme based on measured s.u.'s
Rexp = 0.015	(Δ/σ)max = 0.004
R(F^2) = 0.05044	Background function: GSAS Background function number 1 with 14 terms. Shifted Chebyshev function of 1st kind 1: 2896.21 2: -1969.52 3: 1220.07 4: -623.347 5: 281.467 6: -101.028 7: 37.6638 8: -13.9996 9: -22.4161 10: 44.5336 11: -33.2340 12: -24.8908 13: 83.9862 14: -56.2952
4477 data points

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sc	0	0	0.2600 (5)	0.0146 (19)*
Na1	0.0055 (11)	0.2270 (7)	0.2568 (8)	0.040 (3)*
Na2	0.0130 (8)	0.2304 (8)	0.0486 (6)	0.039 (4)*
Na3	0.0164 (7)	0.2428 (8)	0.4469 (6)	0.032 (3)*
Mo1	0.5269 (2)	0.8610 (2)	0.0272 (1)	0.0205 (7)*
Mo2	0.5144 (2)	0.6476 (2)	0.5248 (1)	0.0331 (9)*
O1	0.5738 (16)	0.7833 (16)	0.0354 (9)	0.042 (3)*
O2	0.5030 (11)	0.8880 (12)	0.1099 (9)	0.032 (4)*
O3	0.6082 (16)	0.9696 (17)	−0.0121 (11)	0.042 (5)*
O4	0.4062 (14)	0.8060 (14)	−0.0180 (8)	0.028 (3)*
O5	0.5855 (15)	0.7828 (15)	0.5247 (8)	0.042 (3)*
O6	0.4693 (12)	0.5950 (12)	0.6092 (9)	0.042 (5)*
O7	0.6058 (15)	0.6161 (11)	0.4968 (11)	0.032 (4)*
O8	0.4021 (13)	0.6027 (12)	0.4681 (8)	0.028 (3)*

Geometric parameters (Å, º)

Sc—O4^i	2.100 (17)	Na2—O6^xi	2.312 (19)
Sc—O4^ii	2.100 (17)	Na2—O7^viii	2.75 (2)
Sc—O4^iii	2.100 (17)	Na3—O1^ii	2.42 (2)
Sc—O8^iv	2.089 (16)	Na3—O2^vi	2.361 (19)
Sc—O8^v	2.089 (16)	Na3—O2^i	2.478 (18)
Sc—O8^vi	2.089 (16)	Na3—O3^vii	2.52 (2)
Na1—O1^ii	2.75 (2)	Na3—O7^ix	2.510 (18)
Na1—O3^vii	2.47 (2)	Mo1—O1	1.64 (2)
Na1—O4^i	2.312 (19)	Mo1—O2	1.720 (17)
Na1—O5^vi	2.85 (2)	Mo1—O3	1.65 (2)
Na1—O7^viii	2.39 (2)	Mo1—O4	1.795 (19)
Na1—O8^iv	2.397 (19)	Mo2—O5	1.76 (2)
Na2—O1^ix	2.95 (2)	Mo2—O6	1.780 (18)
Na2—O3^x	2.46 (2)	Mo2—O7	1.74 (2)
Na2—O5^vi	2.47 (2)	Mo2—O8	1.830 (16)
Na2—O6^iv	2.318 (17)
O4^i—Sc—O4^ii	96.7 (7)	O5^vi—Na2—O7^viii	76.3 (7)
O4^iii—Sc—O4^i	96.7 (7)	O6^iv—Na2—O6^xi	99.0 (8)
O4^ii—Sc—O4^iii	96.7 (7)	O6^iv—Na2—O7^viii	85.1 (6)
O4^i—Sc—O8^iv	87.6 (3)	O6^xi—Na2—O7^viii	170.3 (8)
O4^i—Sc—O8^v	175.4 (8)	O1^ii—Na3—O2^vi	101.9 (7)
O4^i—Sc—O8^vi	84.3 (3)	O1^ii—Na3—O2^i	111.3 (7)
O4^ii—Sc—O8^iv	84.3 (3)	O1^ii—Na3—O3^vii	82.5 (8)
O4^ii—Sc—O8^v	87.6 (3)	O1^ii—Na3—O7^ix	120.9 (8)
O4^ii—Sc—O8^vi	175.4 (8)	O2^vi—Na3—O2^i	100.3 (7)
O4^iii—Sc—O8^iv	175.4 (8)	O2^vi—Na3—O3^vii	157.0 (7)
O4^iii—Sc—O8^v	84.3 (3)	O2^vi—Na3—O7^ix	82.9 (7)
O4^iii—Sc—O8^vi	87.6 (3)	O2^i—Na3—O3^vii	99.0 (6)
O8^iv—Sc—O8^v	91.3 (7)	O2^i—Na3—O7^ix	125.8 (7)
O8^iv—Sc—O8^vi	91.3 (7)	O3^vii—Na3—O7^ix	75.6 (5)
O8^v—Sc—O8^vi	91.3 (7)	O1—Mo1—O2	107.0 (7)
O3^vii—Na1—O4^i	95.0 (9)	O1—Mo1—O3	112.2 (9)
O3^vii—Na1—O7^viii	104.0 (4)	O1—Mo1—O4	114.4 (9)
O3^vii—Na1—O8^iv	163.9 (10)	O2—Mo1—O3	109.1 (8)
O4^i—Na1—O7^viii	159.9 (9)	O2—Mo1—O4	105.8 (7)
O4^i—Na1—O8^iv	76.0 (3)	O3—Mo1—O4	108.1 (9)
O7^viii—Na1—O8^iv	86.9 (8)	O5—Mo2—O6	113.0 (7)
O3^x—Na2—O5^vi	125.3 (8)	O5—Mo2—O7	101.9 (8)
O3^x—Na2—O6^iv	109.7 (8)	O5—Mo2—O8	109.9 (8)
O3^x—Na2—O6^xi	98.0 (8)	O6—Mo2—O7	109.7 (8)
O3^x—Na2—O7^viii	72.2 (5)	O6—Mo2—O8	107.5 (8)
O5^vi—Na2—O6^iv	110.8 (8)	O7—Mo2—O8	114.9 (9)
O5^vi—Na2—O6^xi	110.1 (6)

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