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Single crystals of the lanthanide-containing iridate, disamarium sodium iridium hexaoxide, Sm2NaIrO6, were prepared via high-temperature flux growth and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n and is a double perovskite, consisting of a 1:1 ordered rock-salt-type lattice of corner-shared NaO6 and IrO6 distorted octahedra. Samarium occupies the eightfold coordination site generated by the connectivity of the octahedra.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031836/wm6042sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031836/wm6042Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](m-O) = 0.004 Å
  • R factor = 0.026
  • wR factor = 0.052
  • Data-to-parameter ratio = 22.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART NT (Bruker, 2001); cell refinement: SAINT-Plus NT (Bruker, 2001); data reduction: SAINT-Plus NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.

disamarium sodium iridium hexaoxide top
Crystal data top
Sm2NaIrO6F(000) = 520
Mr = 611.89Dx = 8.024 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3184 reflections
a = 5.4656 (2) Åθ = 2.6–35.0°
b = 5.8880 (2) ŵ = 49.13 mm1
c = 7.8714 (3) ÅT = 294 K
β = 91.097 (1)°Prism, black
V = 253.27 (2) Å30.06 × 0.04 × 0.04 mm
Z = 2
Data collection top
Bruker SMART APEX CCD
diffractometer
1112 independent reflections
Radiation source: fine-focus sealed tube1049 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scansθmax = 35.1°, θmin = 4.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 88
Tmin = 0.075, Tmax = 0.140k = 98
4588 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026 w = 1/[σ2(Fo2) + (0.0142P)2 + 3.1589P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.052(Δ/σ)max < 0.001
S = 1.13Δρmax = 2.08 e Å3
1112 reflectionsΔρmin = 1.74 e Å3
50 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0085 (4)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sm10.47863 (5)0.07291 (5)0.25378 (4)0.01000 (9)
Na10.00000.00000.00000.0091 (6)
Ir10.50000.50000.00000.00730 (8)
O10.2037 (8)0.3260 (7)0.0533 (5)0.0115 (7)
O20.6253 (8)0.4450 (7)0.2320 (5)0.0106 (7)
O30.3389 (8)0.7825 (8)0.0719 (5)0.0123 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.01074 (14)0.00799 (14)0.01126 (13)0.00048 (9)0.00014 (9)0.00022 (9)
Na10.0092 (15)0.0102 (15)0.0078 (13)0.0013 (10)0.0035 (11)0.0008 (11)
Ir10.00742 (13)0.00669 (14)0.00777 (12)0.00014 (8)0.00000 (9)0.00014 (9)
O10.0153 (19)0.0057 (18)0.0135 (17)0.0026 (13)0.0027 (14)0.0001 (14)
O20.0094 (18)0.0124 (19)0.0101 (16)0.0016 (14)0.0002 (13)0.0003 (14)
O30.0139 (19)0.0091 (18)0.0137 (17)0.0044 (14)0.0023 (14)0.0025 (14)
Geometric parameters (Å, º) top
Sm1—O2i2.293 (4)Na1—Sm1x3.5373 (3)
Sm1—O1ii2.339 (4)Na1—Sm1xi3.5373 (3)
Sm1—O22.340 (4)Ir1—O2v1.965 (4)
Sm1—O3iii2.348 (4)Ir1—O21.965 (4)
Sm1—O3ii2.552 (5)Ir1—O11.968 (4)
Sm1—O12.623 (4)Ir1—O1v1.968 (4)
Sm1—O1iv2.705 (4)Ir1—O3v1.970 (4)
Sm1—O3v2.896 (4)Ir1—O31.970 (4)
Sm1—Na1vi3.1757 (3)Ir1—Sm1v3.2150 (3)
Sm1—Ir13.2151 (3)Ir1—Sm1vi3.3133 (3)
Sm1—Na13.2891 (3)Ir1—Sm1xii3.3133 (3)
Sm1—Ir1ii3.3133 (3)Ir1—Sm1xiii3.4423 (3)
Na1—O2vii2.254 (4)Ir1—Sm1vii3.4423 (3)
Na1—O2ii2.254 (4)O1—Sm1vi2.339 (4)
Na1—O12.254 (4)O1—Sm1vii2.705 (4)
Na1—O1viii2.255 (4)O2—Na1vi2.254 (4)
Na1—O3ix2.313 (4)O2—Sm1xiii2.293 (4)
Na1—O3iii2.313 (4)O3—Na1xiv2.313 (4)
Na1—Sm1ii3.1757 (3)O3—Sm1xiv2.348 (4)
Na1—Sm1vii3.1757 (3)O3—Sm1vi2.552 (5)
Na1—Sm1viii3.2891 (3)O3—Sm1v2.896 (4)
O2i—Sm1—O1ii100.24 (15)O3ix—Na1—O3iii180.0
O2i—Sm1—O289.24 (9)O2v—Ir1—O2180.0 (3)
O1ii—Sm1—O2141.28 (15)O2v—Ir1—O190.60 (18)
O2i—Sm1—O3iii94.94 (15)O2—Ir1—O189.40 (18)
O1ii—Sm1—O3iii78.79 (15)O2v—Ir1—O1v89.40 (18)
O2—Sm1—O3iii138.14 (15)O2—Ir1—O1v90.60 (18)
O2i—Sm1—O3ii141.63 (14)O1—Ir1—O1v180.0
O1ii—Sm1—O3ii69.44 (14)O2v—Ir1—O3v91.26 (18)
O2—Sm1—O3ii79.87 (14)O2—Ir1—O3v88.74 (18)
O3iii—Sm1—O3ii117.62 (9)O1—Ir1—O3v89.76 (18)
O2i—Sm1—O1138.22 (14)O1v—Ir1—O3v90.24 (18)
O1ii—Sm1—O1119.83 (8)O2v—Ir1—O388.74 (18)
O2—Sm1—O167.49 (14)O2—Ir1—O391.26 (18)
O3iii—Sm1—O182.60 (14)O1—Ir1—O390.24 (18)
O3ii—Sm1—O170.17 (13)O1v—Ir1—O389.76 (18)
O2i—Sm1—O1iv67.46 (14)O3v—Ir1—O3180.0 (2)
O1ii—Sm1—O1iv76.29 (16)Ir1—O1—Na1144.0 (2)
O2—Sm1—O1iv72.97 (14)Ir1—O1—Sm1vi100.23 (17)
O3iii—Sm1—O1iv145.98 (14)Na1—O1—Sm1vi115.80 (18)
O3ii—Sm1—O1iv74.18 (13)Ir1—O1—Sm187.69 (16)
O1—Sm1—O1iv130.18 (6)Na1—O1—Sm184.45 (13)
O2i—Sm1—O3v78.40 (13)Sm1vi—O1—Sm1102.07 (15)
O1ii—Sm1—O3v156.28 (14)Ir1—O1—Sm1vii93.55 (15)
O2—Sm1—O3v62.34 (13)Na1—O1—Sm1vii79.06 (13)
O3iii—Sm1—O3v77.75 (16)Sm1vi—O1—Sm1vii103.71 (16)
O3ii—Sm1—O3v125.67 (9)Sm1—O1—Sm1vii153.54 (17)
O1—Sm1—O3v60.23 (12)Ir1—O2—Na1vi137.7 (2)
O1iv—Sm1—O3v123.26 (13)Ir1—O2—Sm1xiii107.64 (18)
O2vii—Na1—O2ii180.0 (3)Na1vi—O2—Sm1xiii102.16 (16)
O2vii—Na1—O183.92 (16)Ir1—O2—Sm196.23 (17)
O2ii—Na1—O196.08 (16)Na1vi—O2—Sm187.45 (15)
O2vii—Na1—O1viii96.08 (16)Sm1xiii—O2—Sm1128.9 (2)
O2ii—Na1—O1viii83.92 (16)Ir1—O3—Na1xiv139.2 (2)
O1—Na1—O1viii180.0Ir1—O3—Sm1xiv130.4 (2)
O2vii—Na1—O3ix87.01 (15)Na1xiv—O3—Sm1xiv89.74 (15)
O2ii—Na1—O3ix92.99 (15)Ir1—O3—Sm1vi93.35 (17)
O1—Na1—O3ix87.96 (16)Na1xiv—O3—Sm1vi81.34 (14)
O1viii—Na1—O3ix92.04 (16)Sm1xiv—O3—Sm1vi103.93 (16)
O2vii—Na1—O3iii92.99 (15)Ir1—O3—Sm1v80.25 (14)
O2ii—Na1—O3iii87.01 (15)Na1xiv—O3—Sm1v84.75 (13)
O1—Na1—O3iii92.04 (16)Sm1xiv—O3—Sm1v102.25 (16)
O1viii—Na1—O3iii87.96 (16)Sm1vi—O3—Sm1v150.17 (18)
Symmetry codes: (i) x+3/2, y1/2, z+1/2; (ii) x+1/2, y1/2, z+1/2; (iii) x, y1, z; (iv) x+1/2, y+1/2, z+1/2; (v) x+1, y+1, z; (vi) x+1/2, y+1/2, z+1/2; (vii) x1/2, y+1/2, z1/2; (viii) x, y, z; (ix) x, y+1, z; (x) x+1, y, z; (xi) x1, y, z; (xii) x+1/2, y+1/2, z1/2; (xiii) x+3/2, y+1/2, z+1/2; (xiv) x, y+1, z.
 

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