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Rb[NaCd3O4] presents, to the best of our knowledge, the first example of a 4d transition metal oxide in this A[(MO)4] structure type. The structure consists of a three-dimensional network of edge- and corner-linked distorted tetra­hedral [MO4] entities, with M = Na+ and Cd2+ in a 1:3 ratio sharing a common site set on Wyckoff position 8h in space group I4/m. The large cavities are occupied by A = Rb+ in an almost cubic coordination (4/m symmetry), giving rise to one-dimensional chains of face-sharing [RbO8] polyhedra along [001].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034489/wm2046sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034489/wm2046Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma]() = 0.000 Å
  • Disorder in main residue
  • R factor = 0.041
  • wR factor = 0.098
  • Data-to-parameter ratio = 12.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT301_ALERT_3_B Main Residue Disorder ......................... 35.00 Perc.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M RB M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M RB M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M RB M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M RB M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M M O PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M M O PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M M O PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M M O PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M M M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M M M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M O M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M O M PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M RB M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O M O PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O M O PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O M O PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O M O PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O M O PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M O M O PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O M PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... M M O RB
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 68 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 70 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 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: IPDS (Stoe & Cie, 1997); cell refinement: IPDS; data reduction: X-RED32 (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: CIF-Editor (Wieczorrek, 1999).

Rubidium sodiotricadmate top
Crystal data top
Rb[NaCd3O4]Dx = 5.712 Mg m3
Mr = 509.69Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4/mCell parameters from 1489 reflections
Hall symbol: -I 4θ = 4.6–27.9°
a = 8.957 (2) ŵ = 18.82 mm1
c = 3.6939 (14) ÅT = 293 K
V = 296.35 (15) Å3Irregular block, orange-red
Z = 20.27 × 0.15 × 0.10 mm
F(000) = 448
Data collection top
Stoe IPDS-I
diffractometer
203 independent reflections
Radiation source: fine-focus sealed tube192 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
φ scansθmax = 27.8°, θmin = 3.2°
Absorption correction: numerical
[XRED32 (Stoe & Cie, 2001), after optimizing the crystal shape using XSHAPE (Stoe & Cie, 1999)]
h = 1111
Tmin = 0.026, Tmax = 0.145k = 1111
1250 measured reflectionsl = 44
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)] = 0.041 w = 1/[σ2(Fo2) + (0.052P)2 + 3.5767P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.098(Δ/σ)max < 0.001
S = 1.21Δρmax = 2.03 e Å3
203 reflectionsΔρmin = 1.87 e Å3
16 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.012 (2)
Special details top

Experimental. A suitable single-crystal was carefully selected in a golve box with an attached microscope and mounted in a glass capillary. The scattering intensities were collected on an imaging plate diffractometer (IPDS I, Stoe & Cie) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 30 mA. Intensity data for the title compound were collected at room temperature by φ-scans in 125 frames (0 < φ < 250°, Δφ = 2°, exposure time of 25 min) in the 2 θ range 3.8 to 56.3°. Structure solution and refinement were carried out using the programs SHELXS and SHELXL (Sheldrick, 1997). A numerical absorption correction (X-RED (Stoe & Cie, 2001)) was applied after optimization of the crystal shape (X-SHAPE (Stoe & Cie, 1999)). The last cycles of refinement included atomic positions and anisotropic parameters for all atoms. The final difference maps were free of any chemically significant features. The refinement was based on F2 for ALL reflections.

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*/UeqOcc. (<1)
Rb0.00000.00000.00000.0241 (6)
Cd0.81832 (12)0.63076 (12)0.00000.0238 (5)0.75
Na0.81832 (12)0.63076 (12)0.00000.0238 (5)0.25
O0.7648 (11)0.3999 (9)0.00000.0303 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb0.0255 (8)0.0255 (8)0.0213 (10)0.0000.0000.000
Cd0.0331 (7)0.0192 (7)0.0192 (6)0.0015 (4)0.0000.000
Na0.0331 (7)0.0192 (7)0.0192 (6)0.0015 (4)0.0000.000
O0.042 (5)0.018 (4)0.030 (4)0.001 (3)0.0000.000
Geometric parameters (Å, º) top
Rb—Oi3.137 (8)M—Oix2.196 (5)
Rb—Oii3.137 (8)M—Ox2.196 (5)
Rb—Oiii3.137 (8)M—Oxi2.294 (9)
Rb—Oiv3.137 (8)M—Mxii3.0777 (17)
Rb—Ov3.137 (8)M—Mxiii3.0777 (17)
Rb—Ovi3.137 (8)O—Mxiv2.196 (5)
Rb—Ovii3.137 (8)O—Mxv2.196 (5)
Rb—Oviii3.137 (8)O—Mxvi2.294 (9)
Rb—Miii3.5934 (12)O—Rbxvii3.137 (8)
Rb—Miv3.5934 (12)O—Rbxviii3.137 (8)
Rb—Mi3.5934 (12)O—Oxix3.270 (14)
Rb—Mvi3.5934 (12)O—Oxx3.270 (14)
M—O2.123 (9)
Oi—Rb—Oii180.0 (2)Oiii—Rb—Mi99.82 (13)
Oi—Rb—Oiii69.72 (11)Oiv—Rb—Mi80.18 (13)
Oii—Rb—Oiii110.28 (11)Ov—Rb—Mi78.22 (13)
Oi—Rb—Oiv110.28 (11)Ovi—Rb—Mi140.88 (16)
Oii—Rb—Oiv69.72 (11)Ovii—Rb—Mi101.78 (13)
Oiii—Rb—Oiv180.0 (4)Miii—Rb—Mi74.682 (13)
Oi—Rb—Ov72.1 (2)Miv—Rb—Mi105.318 (13)
Oii—Rb—Ov107.9 (2)Oi—Rb—Mvi80.18 (13)
Oiii—Rb—Ov110.28 (11)Oii—Rb—Mvi99.82 (13)
Oiv—Rb—Ov69.72 (11)Oiii—Rb—Mvi78.22 (13)
Oi—Rb—Ovi110.28 (11)Oiv—Rb—Mvi101.78 (13)
Oii—Rb—Ovi69.72 (11)Ovii—Rb—Mvi140.88 (16)
Oiii—Rb—Ovi72.1 (2)Oviii—Rb—Mvi144.04 (15)
Oiv—Rb—Ovi107.9 (2)Miii—Rb—Mvi61.86 (3)
Ov—Rb—Ovi69.72 (11)Miv—Rb—Mvi118.14 (3)
Oi—Rb—Ovii107.9 (2)Mi—Rb—Mvi105.318 (13)
Oii—Rb—Ovii72.1 (2)O—M—Oix119.4 (3)
Oiii—Rb—Ovii69.72 (11)O—M—Ox119.4 (3)
Oiv—Rb—Ovii110.28 (11)Oix—M—Ox114.5 (4)
Ov—Rb—Ovii180.0 (2)O—M—Oxi108.5 (5)
Ovi—Rb—Ovii110.28 (11)Oix—M—Oxi93.5 (2)
Oi—Rb—Oviii69.72 (11)Ox—M—Oxi93.5 (2)
Oii—Rb—Oviii110.28 (11)M—O—Mxiv103.2 (3)
Oiii—Rb—Oviii107.9 (2)M—O—Mxv103.2 (3)
Oiv—Rb—Oviii72.1 (2)Mxiv—O—Mxv114.5 (4)
Ov—Rb—Oviii110.28 (11)M—O—Mxv103.2 (3)
Ovi—Rb—Oviii180.0 (2)M—O—Mxvi161.5 (5)
Ovii—Rb—Oviii69.72 (11)Mxiv—O—Mxvi86.5 (2)
Oii—Rb—Miii140.88 (16)Mxv—O—Mxvi86.5 (2)
Oiv—Rb—Miii144.04 (15)M—O—Mxvi161.5 (5)
Ov—Rb—Miii80.18 (13)Mxiv—O—Mxvi86.5 (2)
Ovi—Rb—Miii78.22 (13)Mxv—O—Mxvi86.5 (2)
Ovii—Rb—Miii99.82 (13)M—O—Rbxvii83.8 (2)
Oviii—Rb—Miii101.78 (13)Mxiv—O—Rbxvii155.9 (4)
Oi—Rb—Miv140.88 (16)Mxv—O—Rbxvii85.52 (12)
Oiii—Rb—Miv144.04 (15)Mxvi—O—Rbxvii81.2 (2)
Ov—Rb—Miv99.82 (13)M—O—Rbxviii83.8 (2)
Ovi—Rb—Miv101.78 (13)Mxiv—O—Rbxviii85.52 (12)
Ovii—Rb—Miv80.18 (13)Mxv—O—Rbxviii155.9 (4)
Oviii—Rb—Miv78.22 (13)Mxvi—O—Rbxviii81.2 (2)
Miii—Rb—Miv180.00 (2)Rbxvii—O—Rbxviii72.1 (2)
Oii—Rb—Mi144.04 (16)
Symmetry codes: (i) y+1/2, x1/2, z+1/2; (ii) y1/2, x+1/2, z1/2; (iii) x1/2, y1/2, z+1/2; (iv) x+1/2, y+1/2, z1/2; (v) y+1/2, x1/2, z1/2; (vi) x1/2, y1/2, z1/2; (vii) y1/2, x+1/2, z+1/2; (viii) x+1/2, y+1/2, z+1/2; (ix) y+1/2, x+3/2, z+1/2; (x) y+1/2, x+3/2, z1/2; (xi) y+1, x, z; (xii) x+3/2, y+3/2, z+1/2; (xiii) x+3/2, y+3/2, z1/2; (xiv) y+3/2, x1/2, z+1/2; (xv) y+3/2, x1/2, z1/2; (xvi) y, x+1, z; (xvii) x+1/2, y+1/2, z1/2; (xviii) x+1/2, y+1/2, z+1/2; (xix) x+3/2, y+1/2, z1/2; (xx) x+3/2, y+1/2, z+1/2.
 

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