Sodium ytterbium carbonate difluoride, NaYb(CO₃)F₂

The title compound was obtained by microwave-assisted hydro­thermal synthesis at 463 K. It is isostructural with the mineral horváthite, NaY(CO₃)F₂. The structure is built up from (010) infinite [NaYbCO₃]²⁺ layers inter­spersed by fluoride ions. All the atoms except F have site symmetry m.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](O-C) = 0.012 Å
• R factor = 0.030
• wR factor = 0.077
• Data-to-parameter ratio = 13.2

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound ..          ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.10

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   2 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
   1 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

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Computing details

Data collection: STADI4 (Stoe & Cie, 1998); cell refinement: STADI4; data reduction: X-RED32 (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: enCIFer (Version 1.0; Allen et al., 2004).

Sodium ytterbium carbonate difluoride, NaYb(CO₃)F₂

Crystal data

NaYb(CO3)F2	F(000) = 516
Mr = 294.04	Dx = 4.973 Mg m^−3 Dm = 4.95 (1) Mg m^−3 Dm measured by pycnometery
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 32 reflections
a = 6.243 (1) Å	θ = 28–32°
b = 6.892 (2) Å	µ = 23.86 mm^−1
c = 9.127 (2) Å	T = 298 K
V = 392.71 (16) Å^3	Parallelepiped, colorless
Z = 4	0.15 × 0.10 × 0.04 mm

Data collection

Siemens AED2 diffractometer	523 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.000
Graphite monochromator	θmax = 30.0°, θmin = 3.7°
2θ/ω scans	h = 0→8
Absorption correction: gaussian (SHELX76; Sheldrick, 1976)	k = 0→9
Tmin = 0.07, Tmax = 0.39	l = 0→12
609 measured reflections	3 standard reflections every 120 min
609 independent reflections	intensity decay: 15%

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.030	Secondary atom site location: difference Fourier map
wR(F^2) = 0.077	w = 1/[σ^2(Fo^2) + (0.046P)^2 + 2.2577P] where P = (Fo^2 + 2Fc^2)/3
S = 1.13	(Δ/σ)max < 0.001
609 reflections	Δρmax = 2.15 e Å^−3
46 parameters	Δρmin = −2.32 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Na	0.1691 (7)	0.2500	0.2173 (5)	0.0208 (11)
Yb	0.01201 (5)	0.2500	0.57782 (4)	0.00582 (15)
C	0.4582 (15)	0.2500	0.5622 (11)	0.0093 (17)
O1	0.3673 (11)	0.2500	0.6888 (7)	0.0106 (14)
O2	0.6586 (12)	0.2500	0.5451 (9)	0.022 (2)
O3	0.3346 (11)	0.2500	0.4501 (8)	0.0174 (18)
F	−0.0432 (7)	0.4407 (7)	0.3710 (5)	0.0138 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na	0.0145 (19)	0.035 (3)	0.013 (2)	0.000	0.0026 (16)	0.000
Yb	0.0063 (2)	0.0045 (2)	0.0066 (2)	0.000	0.00015 (13)	0.000
C	0.005 (3)	0.009 (5)	0.014 (4)	0.000	0.004 (3)	0.000
O1	0.012 (3)	0.016 (4)	0.004 (3)	0.000	0.001 (2)	0.000
O2	0.008 (3)	0.046 (6)	0.013 (4)	0.000	0.000 (3)	0.000
O3	0.009 (3)	0.035 (5)	0.008 (3)	0.000	−0.001 (2)	0.000
F	0.0196 (19)	0.009 (2)	0.0134 (18)	−0.0014 (18)	−0.0016 (16)	−0.0003 (16)

Geometric parameters (Å, º)

Na—F	2.336 (6)	Yb—F	2.326 (4)
Na—F^i	2.336 (6)	Yb—O3	2.327 (7)
Na—O3	2.363 (9)	Yb—O1	2.439 (7)
Na—F^ii	2.367 (6)	C—O2	1.261 (11)
Na—F^iii	2.367 (6)	C—O3	1.282 (12)
Na—O2^iv	2.395 (10)	C—O1	1.287 (11)
Na—O3^iv	2.587 (9)	O1—Yb^ix	2.314 (7)
Yb—F^v	2.191 (5)	O2—Yb^x	2.227 (8)
Yb—F^vi	2.191 (5)	O2—Na^ii	2.395 (10)
Yb—O2^vii	2.227 (8)	O3—Na^ii	2.587 (9)
Yb—O1^viii	2.314 (7)	F—Yb^v	2.191 (5)
Yb—F^i	2.326 (4)	F—Na^iv	2.367 (6)
F—Na—F^i	68.5 (2)	F^i—Yb—F	68.8 (2)
F—Na—O3	73.0 (2)	F^v—Yb—O3	91.71 (12)
F^i—Na—O3	73.0 (2)	F^vi—Yb—O3	91.71 (12)
F—Na—F^ii	108.8 (2)	O2^vii—Yb—O3	142.2 (3)
F^i—Na—F^ii	161.4 (3)	O1^viii—Yb—O3	143.0 (3)
O3—Na—F^ii	88.5 (2)	F^i—Yb—O3	73.84 (18)
F—Na—F^iii	161.4 (3)	F—Yb—O3	73.84 (18)
F^i—Na—F^iii	108.83 (19)	F^v—Yb—O1	80.25 (12)
O3—Na—F^iii	88.5 (2)	F^vi—Yb—O1	80.25 (12)
F^ii—Na—F^iii	67.5 (3)	O2^vii—Yb—O1	163.2 (3)
F—Na—O2^iv	125.8 (2)	O1^viii—Yb—O1	88.44 (12)
F^i—Na—O2^iv	125.8 (2)	F^i—Yb—O1	118.16 (17)
O3—Na—O2^iv	155.7 (3)	F—Yb—O1	118.16 (17)
F^ii—Na—O2^iv	71.4 (2)	O3—Yb—O1	54.6 (3)
F^iii—Na—O2^iv	71.4 (2)	O2—C—O3	119.9 (9)
F—Na—O3^iv	84.1 (2)	O2—C—O1	123.3 (10)
F^i—Na—O3^iv	84.1 (2)	O3—C—O1	116.8 (8)
O3—Na—O3^iv	152.1 (3)	C—O1—Yb^ix	130.9 (6)
F^ii—Na—O3^iv	114.3 (2)	C—O1—Yb	91.6 (6)
F^iii—Na—O3^iv	114.3 (2)	Yb^ix—O1—Yb	137.5 (3)
O2^iv—Na—O3^iv	52.2 (3)	C—O2—Yb^x	165.1 (8)
F^v—Yb—F^vi	153.3 (2)	C—O2—Na^ii	98.7 (7)
F^v—Yb—O2^vii	96.70 (12)	Yb^x—O2—Na^ii	96.1 (3)
F^vi—Yb—O2^vii	96.70 (12)	C—O3—Yb	97.0 (6)
F^v—Yb—O1^viii	80.71 (12)	C—O3—Na	168.9 (7)
F^vi—Yb—O1^viii	80.71 (12)	Yb—O3—Na	94.1 (3)
O2^vii—Yb—O1^viii	74.7 (3)	C—O3—Na^ii	89.2 (6)
F^v—Yb—F^i	137.39 (13)	Yb—O3—Na^ii	173.9 (4)
F^vi—Yb—F^i	68.66 (18)	Na—O3—Na^ii	79.7 (2)
O2^vii—Yb—F^i	75.2 (2)	Yb^v—F—Yb	111.34 (18)
O1^viii—Yb—F^i	133.57 (16)	Yb^v—F—Na	128.7 (2)
F^v—Yb—F	68.66 (18)	Yb—F—Na	94.91 (19)
F^vi—Yb—F	137.39 (13)	Yb^v—F—Na^iv	132.9 (2)
O2^vii—Yb—F	75.2 (2)	Yb—F—Na^iv	94.30 (18)
O1^viii—Yb—F	133.57 (15)	Na—F—Na^iv	85.04 (15)

Symmetry codes: (i) x, −y+1/2, z; (ii) x+1/2, y, −z+1/2; (iii) x+1/2, −y+1/2, −z+1/2; (iv) x−1/2, y, −z+1/2; (v) −x, −y+1, −z+1; (vi) −x, y−1/2, −z+1; (vii) x−1, y, z; (viii) x−1/2, y, −z+3/2; (ix) x+1/2, y, −z+3/2; (x) x+1, y, z.