Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802019128/br6064sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802019128/br6064Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (As-O) = 0.002 Å
- R factor = 0.019
- wR factor = 0.039
- Data-to-parameter ratio = 12.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.406 0.508 Tmin and Tmax expected: 0.286 0.445 RR = 1.243 Please check that your absorption correction is appropriate. General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.875 Tmax scaled 0.445 Tmin scaled 0.355 REFLT_03 From the CIF: _diffrn_reflns_theta_max 29.88 From the CIF: _reflns_number_total 216 From the CIF: _diffrn_reflns_limit_ max hkl 17. 17. 10. From the CIF: _diffrn_reflns_limit_ min hkl 0. 0. 0. TEST1: Expected hkl limits for theta max Calculated maximum hkl 17. 17. 17. Calculated minimum hkl -17. -17. -17. ALERT: Expected hkl max differ from CIF values
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
The title compound was prepared as previously described by Schwarz & Schmidt (1972), starting from reagent-grade Na2CO3 (Fluka, 99%), (NH4)2Cr2O7 (Prolabo, 99%) and As2O3 (Hoping & Williams, 99.5%) mixed in stoichiometric ratios. The sample was heated first at 773 K for 6 h and the at 1173 K for 60 h and finally quenched to room temperature.
Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4(Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Na3Cr2(AsO4)3 | Dx = 4.327 Mg m−3 |
Mr = 589.73 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, Ia3d | Cell parameters from 25 reflections |
Hall symbol: -I 4bd 2c 3 | θ = 10–14° |
a = 12.188 (2) Å | µ = 13.50 mm−1 |
V = 1810.6 (5) Å3 | T = 293 K |
Z = 8 | Polyhedral, green |
F(000) = 1104 | 0.1 × 0.08 × 0.06 mm |
Enarf-Nonius CAD-4 diffractometer | 194 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.021 |
Graphite monochromator | θmax = 29.9°, θmin = 4.1° |
ω/2θ scans | h = 0→17 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→17 |
Tmin = 0.406, Tmax = 0.508 | l = 0→10 |
735 measured reflections | 2 standard reflections every 120 min |
216 independent reflections | intensity decay: 1.0% |
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)] = 0.019 | w = 1/[σ2(Fo2) + (0.0156P)2 + 7.0122P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.039 | (Δ/σ)max < 0.001 |
S = 1.14 | Δρmax = 0.33 e Å−3 |
216 reflections | Δρmin = −0.40 e Å−3 |
18 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00326 (17) |
Na3Cr2(AsO4)3 | Z = 8 |
Mr = 589.73 | Mo Kα radiation |
Cubic, Ia3d | µ = 13.50 mm−1 |
a = 12.188 (2) Å | T = 293 K |
V = 1810.6 (5) Å3 | 0.1 × 0.08 × 0.06 mm |
Enarf-Nonius CAD-4 diffractometer | 194 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.021 |
Tmin = 0.406, Tmax = 0.508 | 2 standard reflections every 120 min |
735 measured reflections | intensity decay: 1.0% |
216 independent reflections |
R[F2 > 2σ(F2)] = 0.019 | 18 parameters |
wR(F2) = 0.039 | 0 restraints |
S = 1.14 | Δρmax = 0.33 e Å−3 |
216 reflections | Δρmin = −0.40 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 F2 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 > 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 | ||
As1 | 0.3750 | 0.0000 | 0.2500 | 0.00339 (18) | |
Cr1 | 0.2500 | 0.2500 | 0.2500 | 0.0034 (2) | |
Na1 | 0.1250 | 0.0000 | 0.2500 | 0.0112 (4) | |
O1 | 0.28819 (14) | −0.09814 (12) | 0.29743 (13) | 0.0064 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
As1 | 0.0037 (2) | 0.0032 (2) | 0.0032 (2) | 0.000 | 0.000 | 0.000 |
Cr1 | 0.0034 (2) | 0.0034 (2) | 0.0034 (2) | 0.00020 (16) | 0.00020 (16) | 0.00020 (16) |
Na1 | 0.0064 (9) | 0.0136 (6) | 0.0136 (6) | 0.000 | 0.000 | 0.0011 (7) |
O1 | 0.0076 (8) | 0.0046 (7) | 0.0071 (8) | −0.0016 (6) | 0.0017 (6) | 0.0002 (5) |
As1—O1i | 1.6983 (16) | Cr1—O1viii | 1.9942 (15) |
As1—O1ii | 1.6983 (16) | Na1—O1ix | 2.3919 (17) |
As1—O1 | 1.6984 (16) | Na1—O1x | 2.3919 (17) |
As1—O1iii | 1.6984 (16) | Na1—O1iii | 2.3919 (17) |
Cr1—O1iv | 1.9941 (15) | Na1—O1 | 2.3919 (17) |
Cr1—O1v | 1.9941 (15) | Na1—O1xi | 2.5337 (17) |
Cr1—O1vi | 1.9942 (15) | Na1—O1xii | 2.5337 (17) |
Cr1—O1iii | 1.9942 (15) | Na1—O1xiii | 2.5337 (17) |
Cr1—O1vii | 1.9942 (15) | Na1—O1viii | 2.5337 (17) |
O1i—As1—O1ii | 102.93 (11) | O1x—Na1—O1 | 116.73 (7) |
O1i—As1—O1 | 112.84 (6) | O1iii—Na1—O1 | 67.48 (7) |
O1ii—As1—O1 | 112.84 (6) | O1ix—Na1—O1xi | 123.39 (3) |
O1i—As1—O1iii | 112.84 (6) | O1x—Na1—O1xi | 70.40 (7) |
O1ii—As1—O1iii | 112.84 (6) | O1iii—Na1—O1xi | 92.07 (4) |
O1—As1—O1iii | 102.93 (11) | O1—Na1—O1xi | 75.46 (6) |
O1iv—Cr1—O1v | 180.0 | O1ix—Na1—O1xii | 70.40 (7) |
O1iv—Cr1—O1vi | 90.87 (7) | O1x—Na1—O1xii | 123.39 (3) |
O1v—Cr1—O1vi | 89.13 (7) | O1iii—Na1—O1xii | 75.46 (6) |
O1iv—Cr1—O1iii | 89.13 (7) | O1—Na1—O1xii | 92.07 (4) |
O1v—Cr1—O1iii | 90.87 (7) | O1xi—Na1—O1xii | 165.15 (7) |
O1vi—Cr1—O1iii | 180.00 (9) | O1ix—Na1—O1xiii | 92.07 (4) |
O1iv—Cr1—O1vii | 90.87 (7) | O1x—Na1—O1xiii | 75.46 (6) |
O1v—Cr1—O1vii | 89.13 (7) | O1iii—Na1—O1xiii | 123.39 (3) |
O1vi—Cr1—O1vii | 90.87 (7) | O1—Na1—O1xiii | 70.40 (7) |
O1iii—Cr1—O1vii | 89.13 (7) | O1xi—Na1—O1xiii | 112.01 (8) |
O1iv—Cr1—O1viii | 89.13 (7) | O1xii—Na1—O1xiii | 70.04 (8) |
O1v—Cr1—O1viii | 90.87 (7) | O1ix—Na1—O1viii | 75.46 (6) |
O1vi—Cr1—O1viii | 89.13 (7) | O1x—Na1—O1viii | 92.07 (4) |
O1iii—Cr1—O1viii | 90.87 (7) | O1iii—Na1—O1viii | 70.40 (7) |
O1vii—Cr1—O1viii | 180.00 (9) | O1—Na1—O1viii | 123.39 (3) |
O1ix—Na1—O1x | 67.48 (7) | O1xi—Na1—O1viii | 70.04 (8) |
O1ix—Na1—O1iii | 116.73 (7) | O1xii—Na1—O1viii | 112.01 (8) |
O1x—Na1—O1iii | 158.94 (7) | O1xiii—Na1—O1viii | 165.15 (7) |
O1ix—Na1—O1 | 158.94 (7) |
Symmetry codes: (i) −x+3/4, z−1/4, −y+1/4; (ii) −x+3/4, −z+1/4, y+1/4; (iii) x, −y, −z+1/2; (iv) z, −x+1/2, y+1/2; (v) −z+1/2, x, −y; (vi) −x+1/2, y+1/2, z; (vii) y+1/2, z, −x+1/2; (viii) −y, −z+1/2, x; (ix) −x+1/4, z−1/4, y+1/4; (x) −x+1/4, −z+1/4, −y+1/4; (xi) y+1/4, x−1/4, −z+3/4; (xii) y+1/4, −x+1/4, z−1/4; (xiii) −y, z−1/2, −x+1/2. |
Experimental details
Crystal data | |
Chemical formula | Na3Cr2(AsO4)3 |
Mr | 589.73 |
Crystal system, space group | Cubic, Ia3d |
Temperature (K) | 293 |
a (Å) | 12.188 (2) |
V (Å3) | 1810.6 (5) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 13.50 |
Crystal size (mm) | 0.1 × 0.08 × 0.06 |
Data collection | |
Diffractometer | Enarf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.406, 0.508 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 735, 216, 194 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.701 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.019, 0.039, 1.14 |
No. of reflections | 216 |
No. of parameters | 18 |
Δρmax, Δρmin (e Å−3) | 0.33, −0.40 |
Computer programs: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992), CAD-4 EXPRESS, XCAD4(Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1998).
As1—O1i | 1.6983 (16) | Cr1—O1iii | 1.9942 (15) |
As1—O1 | 1.6984 (16) | Na1—O1iv | 2.3919 (17) |
Cr1—O1ii | 1.9941 (15) | Na1—O1v | 2.5337 (17) |
Symmetry codes: (i) −x+3/4, z−1/4, −y+1/4; (ii) z, −x+1/2, y+1/2; (iii) −x+1/2, y+1/2, z; (iv) −x+1/4, z−1/4, y+1/4; (v) y+1/4, x−1/4, −z+3/4. |
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Until now, in the system Na2O–Cr2O3–As2O5, only the structure compounds lying in the limiting binary system have been studied: NaCrO2 (Ruedorff & Becker, 1977), CrAsO4 (Attfield et al., 1987), Na2As4O11 (Driss et al., 1988), NaAsO3 (Liebau, 1956), Na4As2O7 (Leung & Calvo, 1973) and Na3AsO4 (Palazzi & Remy, 1971).
To our knowledge, only one ternary compound, viz. Na3Cr2(AsO4)3 (Schwarz & Schmidt, 1972), has been reported, but its structure has not been determined. On investigating this system, we synthesized this arsenate and report here the synthesis and crystal structure determination.