inorganic compounds
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.
Keywords: crystal structure; double molybdate; polyhedral clusters; ScO6 octahedron; NaO6 octahedron; MoO4 tetrahedron; powder diffraction.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827011302862X/cu3037sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827011302862X/cu3037Isup2.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S010827011302862X/cu3037Isup3.rtv |
CCDC reference: 967055
Computing details top
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)] top
Crystal data top
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) Å3 |
Data collection top
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 top
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(F2) = 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 (Å2) top
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) top
Sc—O4i | 2.100 (17) | Na2—O6xi | 2.312 (19) |
Sc—O4ii | 2.100 (17) | Na2—O7viii | 2.75 (2) |
Sc—O4iii | 2.100 (17) | Na3—O1ii | 2.42 (2) |
Sc—O8iv | 2.089 (16) | Na3—O2vi | 2.361 (19) |
Sc—O8v | 2.089 (16) | Na3—O2i | 2.478 (18) |
Sc—O8vi | 2.089 (16) | Na3—O3vii | 2.52 (2) |
Na1—O1ii | 2.75 (2) | Na3—O7ix | 2.510 (18) |
Na1—O3vii | 2.47 (2) | Mo1—O1 | 1.64 (2) |
Na1—O4i | 2.312 (19) | Mo1—O2 | 1.720 (17) |
Na1—O5vi | 2.85 (2) | Mo1—O3 | 1.65 (2) |
Na1—O7viii | 2.39 (2) | Mo1—O4 | 1.795 (19) |
Na1—O8iv | 2.397 (19) | Mo2—O5 | 1.76 (2) |
Na2—O1ix | 2.95 (2) | Mo2—O6 | 1.780 (18) |
Na2—O3x | 2.46 (2) | Mo2—O7 | 1.74 (2) |
Na2—O5vi | 2.47 (2) | Mo2—O8 | 1.830 (16) |
Na2—O6iv | 2.318 (17) | ||
O4i—Sc—O4ii | 96.7 (7) | O5vi—Na2—O7viii | 76.3 (7) |
O4iii—Sc—O4i | 96.7 (7) | O6iv—Na2—O6xi | 99.0 (8) |
O4ii—Sc—O4iii | 96.7 (7) | O6iv—Na2—O7viii | 85.1 (6) |
O4i—Sc—O8iv | 87.6 (3) | O6xi—Na2—O7viii | 170.3 (8) |
O4i—Sc—O8v | 175.4 (8) | O1ii—Na3—O2vi | 101.9 (7) |
O4i—Sc—O8vi | 84.3 (3) | O1ii—Na3—O2i | 111.3 (7) |
O4ii—Sc—O8iv | 84.3 (3) | O1ii—Na3—O3vii | 82.5 (8) |
O4ii—Sc—O8v | 87.6 (3) | O1ii—Na3—O7ix | 120.9 (8) |
O4ii—Sc—O8vi | 175.4 (8) | O2vi—Na3—O2i | 100.3 (7) |
O4iii—Sc—O8iv | 175.4 (8) | O2vi—Na3—O3vii | 157.0 (7) |
O4iii—Sc—O8v | 84.3 (3) | O2vi—Na3—O7ix | 82.9 (7) |
O4iii—Sc—O8vi | 87.6 (3) | O2i—Na3—O3vii | 99.0 (6) |
O8iv—Sc—O8v | 91.3 (7) | O2i—Na3—O7ix | 125.8 (7) |
O8iv—Sc—O8vi | 91.3 (7) | O3vii—Na3—O7ix | 75.6 (5) |
O8v—Sc—O8vi | 91.3 (7) | O1—Mo1—O2 | 107.0 (7) |
O3vii—Na1—O4i | 95.0 (9) | O1—Mo1—O3 | 112.2 (9) |
O3vii—Na1—O7viii | 104.0 (4) | O1—Mo1—O4 | 114.4 (9) |
O3vii—Na1—O8iv | 163.9 (10) | O2—Mo1—O3 | 109.1 (8) |
O4i—Na1—O7viii | 159.9 (9) | O2—Mo1—O4 | 105.8 (7) |
O4i—Na1—O8iv | 76.0 (3) | O3—Mo1—O4 | 108.1 (9) |
O7viii—Na1—O8iv | 86.9 (8) | O5—Mo2—O6 | 113.0 (7) |
O3x—Na2—O5vi | 125.3 (8) | O5—Mo2—O7 | 101.9 (8) |
O3x—Na2—O6iv | 109.7 (8) | O5—Mo2—O8 | 109.9 (8) |
O3x—Na2—O6xi | 98.0 (8) | O6—Mo2—O7 | 109.7 (8) |
O3x—Na2—O7viii | 72.2 (5) | O6—Mo2—O8 | 107.5 (8) |
O5vi—Na2—O6iv | 110.8 (8) | O7—Mo2—O8 | 114.9 (9) |
O5vi—Na2—O6xi | 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. |
Bond lengths (Å) and angles (°) for Na9Sc(MoO4)6 top
ScO6 octahedron | ||||||
Sc | O4i | O4ii | O4iii | O8iv | O8v | O8vi |
O4i | 2.100 (17) | 96.7 (7) | 96.7 (7) | 87.6 (3) | 175.4 (8) | 84.3 (3) |
O4ii | 2.100 (17) | 96.7 (7) | 84.3 (3) | 87.6 (3) | 175.4 (8) | |
O4iii | 2.100 (17) | 175.4 (8) | 84.3 (3) | 87.6 (3) | ||
O8iv | 2.089 (16) | 91.3 (7) | 91.3 (7) | |||
O8v | 2.089 (16) | 91.3 (7) | ||||
O8vi | 2.089 (16) | |||||
Na1O6 octahedron | ||||||
Na1 | O1ii | O3vii | O4i | O5vi | O7viii | O8iv |
O1ii | 2.75 (2) | 77.1 (8) | 69.9 (7) | 154.4 (5) | 120.3 (7) | 87.1 (7) |
O3vii | 2.47 (2) | 95.0 (9) | 120.5 (8) | 104.0 (4) | 163.9 (10) | |
O4i | 2.312 (19) | 89.0 (7) | 159.9 (9) | 76.0 (3) | ||
O5vi | 2.85 (2) | 75.7 (7) | 73.2 (6) | |||
O7viii | 2.39 (2) | 86.9 (8) | ||||
O8iv | 2.397 (19) | |||||
Na2O6 octahedron | ||||||
Na2 | O1ix | O3x | O5vi | O6iv | O6xi | O7viii |
O1ix | 2.95 (2) | 73.2 (7) | 67.8 (6) | 176.6 (7) | 78.8 (6) | 120.3 (7) |
O3x | 2.46 (2) | 125.3 (8) | 109.7 (8) | 98.0 (8) | 72.2 (5) | |
O5vi | 2.47 (2) | 110.8 (8) | 110.1 (6) | 76.3 (7) | ||
O6iv | 2.318 (17) | 99.0 (8) | 85.1 (6) | |||
O6xi | 2.312 (19) | 170.3 (8) | ||||
O7viii | 2.75 (2) | |||||
Na3O5 polyhedron | ||||||
Na3 | O1ii | O2vi | O2i | O3vii | O7ix | |
O1ii | 2.42 (2) | 101.9 (7) | 111.3 (7) | 82.5 (8) | 120.9 (8) | |
O2vi | 2.361 (19) | 100.3 (7) | 157.0 (7) | 82.9 (7) | ||
O2i | 2.478 (18) | 99.0 (6) | 125.8 (7) | |||
O3vii | 2.52 (2) | 75.6 (5) | ||||
O7ix | 2.510 (18) | |||||
Mo1O4 tetrahedron | ||||||
Mo1 | O1 | O2 | O3 | O4 | ||
O1 | 1.64 (2) | 107.0 (7) | 112.2 (9) | 114.4 (9) | ||
O2 | 1.720 (17) | 109.1 (8) | 105.8 (7) | |||
O3 | 1.65 (2) | 108.1 (9) | ||||
O4 | 1.795 (19) | |||||
Mo2O4 tetrahedron | ||||||
Mo2 | O5 | O6 | O7 | O8 | ||
O5 | 1.76 (2) | 113.0 (7) | 101.9 (8) | 109.9 (8) | ||
O6 | 1.780 (18) | 109.7 (8) | 107.5 (8) | |||
O7 | 1.74 (2) | 114.9 (9) | ||||
O8 | 1.830 (16) |
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. |