Rubidium sodotricadmate, Rb[NaCd3O4]

Kerp, O.; Möller, A.

doi:10.1107/S1600536806034489

Buy article online - an online subscription or single-article purchase is required to access this article.

Rubidium sodotricadmate, Rb[NaCd₃O₄]

O. Kerp and A. Möller

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].

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034489/wm2046sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034489/wm2046Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean () = 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]	D_x = 5.712 Mg m⁻³
M_r = 509.69	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4/m	Cell parameters from 1489 reflections
Hall symbol: -I 4	θ = 4.6–27.9°
a = 8.957 (2) Å	µ = 18.82 mm⁻¹
c = 3.6939 (14) Å	T = 293 K
V = 296.35 (15) Å³	Irregular block, orange-red
Z = 2	0.27 × 0.15 × 0.10 mm
F(000) = 448

Data collection top

Stoe IPDS-I diffractometer	203 independent reflections
Radiation source: fine-focus sealed tube	192 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.058
φ scans	θ_max = 27.8°, θ_min = 3.2°
Absorption correction: numerical [XRED32 (Stoe & Cie, 2001), after optimizing the crystal shape using XSHAPE (Stoe & Cie, 1999)]	h = −11→11
T_min = 0.026, T_max = 0.145	k = −11→11
1250 measured reflections	l = −4→4

Refinement top

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)] = 0.041	w = 1/[σ²(F_o²) + (0.052P)² + 3.5767P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.098	(Δ/σ)_max < 0.001
S = 1.21	Δρ_max = 2.03 e Å⁻³
203 reflections	Δρ_min = −1.87 e Å⁻³
16 parameters	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Rb	0.0000	0.0000	0.0000	0.0241 (6)
Cd	0.81832 (12)	0.63076 (12)	0.0000	0.0238 (5)	0.75
Na	0.81832 (12)	0.63076 (12)	0.0000	0.0238 (5)	0.25
O	0.7648 (11)	0.3999 (9)	0.0000	0.0303 (18)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb	0.0255 (8)	0.0255 (8)	0.0213 (10)	0.000	0.000	0.000
Cd	0.0331 (7)	0.0192 (7)	0.0192 (6)	−0.0015 (4)	0.000	0.000
Na	0.0331 (7)	0.0192 (7)	0.0192 (6)	−0.0015 (4)	0.000	0.000
O	0.042 (5)	0.018 (4)	0.030 (4)	0.001 (3)	0.000	0.000

Geometric parameters (Å, º) top

Rb—Oⁱ	3.137 (8)	M—O^ix	2.196 (5)
Rb—Oⁱⁱ	3.137 (8)	M—O^x	2.196 (5)
Rb—Oⁱⁱⁱ	3.137 (8)	M—O^xi	2.294 (9)
Rb—O^iv	3.137 (8)	M—M^xii	3.0777 (17)
Rb—O^v	3.137 (8)	M—M^xiii	3.0777 (17)
Rb—O^vi	3.137 (8)	O—M^xiv	2.196 (5)
Rb—O^vii	3.137 (8)	O—M^xv	2.196 (5)
Rb—O^viii	3.137 (8)	O—M^xvi	2.294 (9)
Rb—Mⁱⁱⁱ	3.5934 (12)	O—Rb^xvii	3.137 (8)
Rb—M^iv	3.5934 (12)	O—Rb^xviii	3.137 (8)
Rb—Mⁱ	3.5934 (12)	O—O^xix	3.270 (14)
Rb—M^vi	3.5934 (12)	O—O^xx	3.270 (14)
M—O	2.123 (9)

Oⁱ—Rb—Oⁱⁱ	180.0 (2)	Oⁱⁱⁱ—Rb—Mⁱ	99.82 (13)
Oⁱ—Rb—Oⁱⁱⁱ	69.72 (11)	O^iv—Rb—Mⁱ	80.18 (13)
Oⁱⁱ—Rb—Oⁱⁱⁱ	110.28 (11)	O^v—Rb—Mⁱ	78.22 (13)
Oⁱ—Rb—O^iv	110.28 (11)	O^vi—Rb—Mⁱ	140.88 (16)
Oⁱⁱ—Rb—O^iv	69.72 (11)	O^vii—Rb—Mⁱ	101.78 (13)
Oⁱⁱⁱ—Rb—O^iv	180.0 (4)	Mⁱⁱⁱ—Rb—Mⁱ	74.682 (13)
Oⁱ—Rb—O^v	72.1 (2)	M^iv—Rb—Mⁱ	105.318 (13)
Oⁱⁱ—Rb—O^v	107.9 (2)	Oⁱ—Rb—M^vi	80.18 (13)
Oⁱⁱⁱ—Rb—O^v	110.28 (11)	Oⁱⁱ—Rb—M^vi	99.82 (13)
O^iv—Rb—O^v	69.72 (11)	Oⁱⁱⁱ—Rb—M^vi	78.22 (13)
Oⁱ—Rb—O^vi	110.28 (11)	O^iv—Rb—M^vi	101.78 (13)
Oⁱⁱ—Rb—O^vi	69.72 (11)	O^vii—Rb—M^vi	140.88 (16)
Oⁱⁱⁱ—Rb—O^vi	72.1 (2)	O^viii—Rb—M^vi	144.04 (15)
O^iv—Rb—O^vi	107.9 (2)	Mⁱⁱⁱ—Rb—M^vi	61.86 (3)
O^v—Rb—O^vi	69.72 (11)	M^iv—Rb—M^vi	118.14 (3)
Oⁱ—Rb—O^vii	107.9 (2)	Mⁱ—Rb—M^vi	105.318 (13)
Oⁱⁱ—Rb—O^vii	72.1 (2)	O—M—O^ix	119.4 (3)
Oⁱⁱⁱ—Rb—O^vii	69.72 (11)	O—M—O^x	119.4 (3)
O^iv—Rb—O^vii	110.28 (11)	O^ix—M—O^x	114.5 (4)
O^v—Rb—O^vii	180.0 (2)	O—M—O^xi	108.5 (5)
O^vi—Rb—O^vii	110.28 (11)	O^ix—M—O^xi	93.5 (2)
Oⁱ—Rb—O^viii	69.72 (11)	O^x—M—O^xi	93.5 (2)
Oⁱⁱ—Rb—O^viii	110.28 (11)	M—O—M^xiv	103.2 (3)
Oⁱⁱⁱ—Rb—O^viii	107.9 (2)	M—O—M^xv	103.2 (3)
O^iv—Rb—O^viii	72.1 (2)	M^xiv—O—M^xv	114.5 (4)
O^v—Rb—O^viii	110.28 (11)	M—O—M^xv	103.2 (3)
O^vi—Rb—O^viii	180.0 (2)	M—O—M^xvi	161.5 (5)
O^vii—Rb—O^viii	69.72 (11)	M^xiv—O—M^xvi	86.5 (2)
Oⁱⁱ—Rb—Mⁱⁱⁱ	140.88 (16)	M^xv—O—M^xvi	86.5 (2)
O^iv—Rb—Mⁱⁱⁱ	144.04 (15)	M—O—M^xvi	161.5 (5)
O^v—Rb—Mⁱⁱⁱ	80.18 (13)	M^xiv—O—M^xvi	86.5 (2)
O^vi—Rb—Mⁱⁱⁱ	78.22 (13)	M^xv—O—M^xvi	86.5 (2)
O^vii—Rb—Mⁱⁱⁱ	99.82 (13)	M—O—Rb^xvii	83.8 (2)
O^viii—Rb—Mⁱⁱⁱ	101.78 (13)	M^xiv—O—Rb^xvii	155.9 (4)
Oⁱ—Rb—M^iv	140.88 (16)	M^xv—O—Rb^xvii	85.52 (12)
Oⁱⁱⁱ—Rb—M^iv	144.04 (15)	M^xvi—O—Rb^xvii	81.2 (2)
O^v—Rb—M^iv	99.82 (13)	M—O—Rb^xviii	83.8 (2)
O^vi—Rb—M^iv	101.78 (13)	M^xiv—O—Rb^xviii	85.52 (12)
O^vii—Rb—M^iv	80.18 (13)	M^xv—O—Rb^xviii	155.9 (4)
O^viii—Rb—M^iv	78.22 (13)	M^xvi—O—Rb^xviii	81.2 (2)
Mⁱⁱⁱ—Rb—M^iv	180.00 (2)	Rb^xvii—O—Rb^xviii	72.1 (2)
Oⁱⁱ—Rb—Mⁱ	144.04 (16)

Symmetry codes: (i) −y+1/2, x−1/2, z+1/2; (ii) y−1/2, −x+1/2, −z−1/2; (iii) x−1/2, y−1/2, z+1/2; (iv) −x+1/2, −y+1/2, −z−1/2; (v) −y+1/2, x−1/2, z−1/2; (vi) x−1/2, y−1/2, z−1/2; (vii) y−1/2, −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, −z−1/2; (xi) −y+1, x, z; (xii) −x+3/2, −y+3/2, −z+1/2; (xiii) −x+3/2, −y+3/2, −z−1/2; (xiv) −y+3/2, x−1/2, z+1/2; (xv) −y+3/2, x−1/2, z−1/2; (xvi) y, −x+1, −z; (xvii) x+1/2, y+1/2, z−1/2; (xviii) x+1/2, y+1/2, z+1/2; (xix) −x+3/2, −y+1/2, −z−1/2; (xx) −x+3/2, −y+1/2, −z+1/2.

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.

E-mail address*
Repeat e-mail address* (for error checking)

Format*	PDF (US $40)
	HTML (US $40)
	PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number (non-UK EC countries only)
Country*

Terms and conditions of use
Contact us

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page