Sodium perchlorate in the space group Pnma

The first example of Na⁺ClO₄⁻ in the ortho­rhom­bic system in space group Pnma at room temperature is reported. The Na, Cl and two O atoms are located on positions of site symmetry m.

Key indicators

• Single-crystal X-ray study
• T = 571 K
• Mean [sigma](l-O) = 0.006 Å
• R factor = 0.075
• wR factor = 0.200
• Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cl1

   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: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Sodium perchlorate

Crystal data

Na^+·ClO4^−	F(000) = 240
Mr = 122.44	Dx = 2.036 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 184 reflections
a = 9.236 (7) Å	θ = 3.6–25.0°
b = 5.809 (4) Å	µ = 0.93 mm^−1
c = 7.444 (6) Å	T = 571 K
V = 399.4 (5) Å^3	Block, colorless
Z = 4	0.28 × 0.23 × 0.19 mm

Data collection

Bruker APEX area-detector diffractometer	387 independent reflections
Radiation source: fine-focus sealed tube	342 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
φ and ω scans	θmax = 25.0°, θmin = 3.5°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −10→6
Tmin = 0.782, Tmax = 0.844	k = −6→6
1882 measured reflections	l = −8→8

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)] = 0.075	Secondary atom site location: difference Fourier map
wR(F^2) = 0.200	w = 1/[σ^2(Fo^2) + (0.1006P)^2 + 2.6942P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max < 0.001
387 reflections	Δρmax = 0.53 e Å^−3
34 parameters	Δρmin = −0.92 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
Na1	0.3191 (7)	0.7500	0.3323 (8)	0.102 (2)
Cl1	0.56799 (18)	0.2500	0.1917 (2)	0.0292 (8)
O1	0.5798 (4)	0.4507 (8)	0.3039 (5)	0.0421 (12)
O2	0.4314 (6)	0.2500	0.1033 (10)	0.060 (2)
O3	0.6852 (7)	0.2500	0.0656 (8)	0.0491 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na1	0.103 (4)	0.105 (5)	0.098 (4)	0.000	−0.003 (3)	0.000
Cl1	0.0312 (11)	0.0288 (12)	0.0277 (11)	0.000	−0.0009 (7)	0.000
O1	0.049 (2)	0.034 (2)	0.044 (2)	0.0021 (18)	0.0019 (18)	−0.0092 (18)
O2	0.044 (4)	0.068 (5)	0.068 (4)	0.000	−0.026 (3)	0.000
O3	0.058 (4)	0.053 (4)	0.036 (3)	0.000	0.018 (3)	0.000

Geometric parameters (Å, º)

Cl1—O1	1.438 (4)	Na1—O1^iv	2.989 (7)
Cl1—O1^i	1.438 (4)	Na1—O1^v	3.093 (7)
Cl1—O2	1.423 (6)	Na1—O1^vi	3.093 (7)
Cl1—O3	1.433 (6)	Na1—O2^vii	3.070 (9)
Na1—O1	2.977 (7)	Na1—O3^viii	2.962 (8)
Na1—O1^ii	2.977 (7)	O1—Na1^ix	2.989 (7)
Na1—O1^iii	2.989 (7)	O3—Na1^viii	2.962 (8)
O3^viii—Na1—O1	86.6 (2)	O2—Cl1—O3	111.5 (4)
O3^viii—Na1—O1^ii	86.6 (2)	O2—Cl1—O1	109.6 (2)
O3^viii—Na1—O1^iii	69.57 (18)	O3—Cl1—O1	108.8 (2)
O3^viii—Na1—O1^iv	69.57 (18)	O2—Cl1—O1^i	109.6 (2)
O1^ii—Na1—O1	71.5 (2)	O3—Cl1—O1^i	108.8 (2)
O1^ii—Na1—O1^iii	156.0 (2)	O1—Cl1—O1^i	108.3 (3)
O1—Na1—O1^iii	103.55 (15)	Cl1—O1—Na1	116.9 (2)
O1^ii—Na1—O1^iv	103.55 (15)	Cl1—O1—Na1^ix	109.3 (2)
O1—Na1—O1^iv	156.0 (2)	Na1—O1—Na1^ix	106.40 (15)
O1^iii—Na1—O1^iv	71.1 (2)	Cl1—O3—Na1^viii	130.2 (4)
O2—Cl1—O1—Na1	5.1 (4)	O1^iv—Na1—O1—Cl1	−57.4 (5)
O3—Cl1—O1—Na1	127.3 (3)	O3^viii—Na1—O1—Na1^ix	70.97 (19)
O1^i—Cl1—O1—Na1	−114.5 (3)	O1^ii—Na1—O1—Na1^ix	−16.55 (15)
O2—Cl1—O1—Na1^ix	−115.9 (3)	O1^iii—Na1—O1—Na1^ix	139.0 (3)
O3—Cl1—O1—Na1^ix	6.4 (3)	O1^iv—Na1—O1—Na1^ix	65.1 (5)
O1^i—Cl1—O1—Na1^ix	124.6 (2)	O2—Cl1—O3—Na1^viii	0.0
O3^viii—Na1—O1—Cl1	−51.4 (3)	O1—Cl1—O3—Na1^viii	−121.1 (2)
O1^ii—Na1—O1—Cl1	−139.0 (2)	O1^i—Cl1—O3—Na1^viii	121.1 (2)
O1^iii—Na1—O1—Cl1	16.6 (3)

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