Dirubidium sodium manganate(V), Rb₂NaMnO₄

Rb₂NaMnO₄ has been obtained from a redox reaction in silver crucibles. The crystal structure contains isolated [MnO₄] units, which are slightly distorted from ideal tetra­hedral symmetry. Rb₂NaMnO₄ crystallizes isotypic with Cs₂NaVO₄ and Cs₂NaAsO₄.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](n-O) = 0.005 Å
• R factor = 0.036
• wR factor = 0.074
• Data-to-parameter ratio = 14.6

checkCIF/PLATON results

No syntax errors found



Alert level C
RINTA01_ALERT_3_C  The value of Rint is greater than 0.10
            Rint given   0.107
PLAT020_ALERT_3_C The value of Rint is greater than 0.10 .........       0.11
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   3 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
   2 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: IPDS (Stoe, 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, 2005); software used to prepare material for publication: CIF-Editor (Wieczorrek, 2004).

Dirubidium sodium manganate(V)

Crystal data

Rb2Na(MnO4)	F(000) = 284
Mr = 312.87	Dx = 3.701 Mg m^−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 2665 reflections
a = 5.9078 (13) Å	θ = 2.6–28.1°
b = 5.9821 (13) Å	µ = 19.57 mm^−1
c = 7.9503 (19) Å	T = 293 K
β = 92.22 (3)°	Irregular bloc, green-blue
V = 280.76 (11) Å^3	0.30 × 0.15 × 0.10 mm
Z = 2

Data collection

Stoe IPDS-I diffractometer	670 independent reflections
Radiation source: fine-focus sealed tube	556 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.107
Detector resolution: not measured pixels mm^-1	θmax = 27.0°, θmin = 2.6°
φ scans	h = −7→7
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	k = −7→7
Tmin = 0.027, Tmax = 0.086	l = −10→10
2023 measured reflections

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)] = 0.036	Secondary atom site location: difference Fourier map
wR(F^2) = 0.074	w = 1/[σ^2(Fo^2) + (0.0291P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max < 0.001
670 reflections	Δρmax = 1.01 e Å^−3
46 parameters	Δρmin = −1.51 e Å^−3

Special details

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 100 frames (0 < φ < 200°, Δφ = 2°, exposure time of 15 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 atomic parameters for the two crystallographic independent Rb atoms have been extracted from Direct Methods. All other atomic parameters have been obtained from Difference Fourier Synthesis and used for full matrix least squares refinements. 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 (Ų)

	x	y	z	Uiso*/Ueq
Rb1	0.29985 (10)	0.2500	0.50484 (10)	0.0229 (2)
Rb2	0.85438 (13)	0.2500	0.82005 (11)	0.0321 (2)
Mn1	0.78706 (16)	0.2500	0.25549 (15)	0.0165 (3)
Na	0.3668 (5)	0.2500	0.0259 (4)	0.0232 (6)
O1	0.7983 (7)	0.2500	0.4681 (7)	0.0213 (11)
O2	0.0524 (8)	0.2500	0.1793 (8)	0.0330 (13)
O3	0.6402 (6)	0.0223 (6)	0.1813 (5)	0.0318 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rb1	0.0215 (3)	0.0201 (3)	0.0272 (5)	0.000	0.0019 (2)	0.000
Rb2	0.0410 (4)	0.0331 (4)	0.0225 (5)	0.000	0.0037 (3)	0.000
Mn1	0.0179 (5)	0.0143 (4)	0.0176 (7)	0.000	0.0027 (4)	0.000
Na	0.0227 (13)	0.0223 (13)	0.025 (2)	0.000	0.0016 (11)	0.000
O1	0.018 (2)	0.026 (2)	0.020 (3)	0.000	0.0019 (19)	0.000
O2	0.023 (2)	0.053 (3)	0.023 (4)	0.000	0.005 (2)	0.000
O3	0.044 (2)	0.0191 (16)	0.031 (3)	−0.0039 (14)	−0.0101 (18)	−0.0020 (14)

Geometric parameters (Å, º)

Rb1—O2	2.923 (6)	Mn1—Rb2^xii	3.4999 (17)
Rb1—O1^i	2.966 (4)	Mn1—Rb1^xi	3.5556 (16)
Rb1—O1	2.971 (4)	Mn1—Rb1^iv	3.5939 (10)
Rb1—O3^ii	2.989 (4)	Mn1—Rb1^iii	3.5939 (10)
Rb1—O3^iii	2.989 (4)	Mn1—Rb2^xiii	3.7273 (10)
Rb1—O1^iii	3.0560 (11)	Mn1—Rb2^ix	3.7273 (10)
Rb1—O1^iv	3.0560 (11)	Na—O2	2.262 (6)
Rb1—Mn1^i	3.5556 (16)	Na—O3^xiv	2.316 (4)
Rb1—Mn1	3.5576 (16)	Na—O3^xv	2.316 (4)
Rb1—O3^v	3.594 (5)	Na—O3^v	2.415 (4)
Rb1—O3	3.594 (5)	Na—O3	2.415 (4)
Rb1—Mn1^iv	3.5939 (10)	Na—Rb2^xii	3.368 (3)
Rb2—O1	2.805 (6)	Na—Rb2^xvi	3.386 (3)
Rb2—O2^iv	3.0413 (11)	Na—Na^xvii	3.412 (3)
Rb2—O2^iii	3.0413 (11)	Na—Na^xiv	3.412 (3)
Rb2—O2^vi	3.045 (6)	Na—Rb2^iii	3.5039 (17)
Rb2—O3^iii	3.345 (4)	Na—Rb2^iv	3.5039 (17)
Rb2—O3^ii	3.345 (4)	O1—Rb1^xi	2.966 (4)
Rb2—Na^vii	3.368 (3)	O1—Rb1^iii	3.0560 (11)
Rb2—Na^vi	3.386 (3)	O1—Rb1^iv	3.0560 (11)
Rb2—O3^viii	3.402 (4)	O2—Mn1^i	1.702 (5)
Rb2—O3^ix	3.402 (4)	O2—Rb2^iv	3.0413 (11)
Rb2—O3^x	3.462 (5)	O2—Rb2^iii	3.0413 (11)
Rb2—O3^vii	3.462 (5)	O2—Rb2^xvi	3.045 (6)
Mn1—O1	1.689 (6)	O3—Na^xiv	2.316 (4)
Mn1—O2^xi	1.702 (5)	O3—Rb1^iii	2.989 (4)
Mn1—O3	1.708 (3)	O3—Rb2^iii	3.345 (4)
Mn1—O3^v	1.708 (3)	O3—Rb2^ix	3.402 (4)
Mn1—Na	3.024 (3)	O3—Rb2^xii	3.462 (5)
O2—Rb1—O1^i	56.58 (16)	O3^ii—Rb2—O3^vii	81.20 (8)
O2—Rb1—O1	112.14 (15)	O3^viii—Rb2—O3^vii	122.69 (7)
O1^i—Rb1—O1	168.7 (2)	O3^ix—Rb2—O3^vii	99.40 (10)
O2—Rb1—O3^ii	141.09 (8)	O3^x—Rb2—O3^vii	46.33 (12)
O1^i—Rb1—O3^ii	99.66 (12)	O1—Mn1—O2^xi	110.8 (2)
O1—Rb1—O3^ii	89.78 (12)	O1—Mn1—O3	110.21 (17)
O2—Rb1—O3^iii	141.09 (9)	O2^xi—Mn1—O3	109.86 (18)
O1^i—Rb1—O3^iii	99.66 (12)	O1—Mn1—O3^v	110.21 (17)
O1—Rb1—O3^iii	89.78 (12)	O2^xi—Mn1—O3^v	109.86 (18)
O3^ii—Rb1—O3^iii	66.04 (14)	O3—Mn1—O3^v	105.8 (2)
O2—Rb1—O1^iii	88.42 (10)	O2—Na—O3^xiv	113.03 (16)
O1^i—Rb1—O1^iii	79.36 (8)	O2—Na—O3^xv	113.03 (16)
O1—Rb1—O1^iii	101.45 (8)	O3^xiv—Na—O3^xv	89.4 (2)
O3^ii—Rb1—O1^iii	119.43 (13)	O2—Na—O3^v	105.73 (19)
O3^iii—Rb1—O1^iii	54.87 (12)	O3^xiv—Na—O3^v	138.90 (14)
O2—Rb1—O1^iv	88.42 (10)	O3^xv—Na—O3^v	87.74 (14)
O1^i—Rb1—O1^iv	79.36 (8)	O2—Na—O3	105.73 (19)
O1—Rb1—O1^iv	101.45 (8)	O3^xiv—Na—O3	87.74 (14)
O3^ii—Rb1—O1^iv	54.87 (12)	O3^xv—Na—O3	138.90 (14)
O3^iii—Rb1—O1^iv	119.43 (13)	O3^v—Na—O3	68.65 (17)
O1^iii—Rb1—O1^iv	156.34 (17)	Mn1—O1—Rb2	175.5 (2)
O2—Rb1—O3^v	68.95 (12)	Mn1—O1—Rb1^xi	95.69 (19)
O1^i—Rb1—O3^v	120.93 (11)	Rb2—O1—Rb1^xi	79.80 (12)
O1—Rb1—O3^v	49.11 (11)	Mn1—O1—Rb1	95.60 (18)
O3^ii—Rb1—O3^v	109.84 (10)	Rb2—O1—Rb1	88.92 (15)
O3^iii—Rb1—O3^v	138.80 (6)	Rb1^xi—O1—Rb1	168.7 (2)
O1^iii—Rb1—O3^v	122.30 (11)	Mn1—O1—Rb1^iii	94.02 (10)
O1^iv—Rb1—O3^v	78.02 (11)	Rb2—O1—Rb1^iii	86.86 (10)
Mn1^i—Rb1—O3^v	95.12 (6)	Rb1^xi—O1—Rb1^iii	100.64 (8)
Mn1—Rb1—O3^v	27.62 (6)	Rb1—O1—Rb1^iii	78.55 (8)
O2—Rb1—O3	68.95 (12)	Mn1—O1—Rb1^iv	94.03 (10)
O1^i—Rb1—O3	120.93 (11)	Rb2—O1—Rb1^iv	86.86 (10)
O1—Rb1—O3	49.11 (11)	Rb1^xi—O1—Rb1^iv	100.64 (8)
O3^ii—Rb1—O3	138.80 (6)	Rb1—O1—Rb1^iv	78.55 (8)
O3^iii—Rb1—O3	109.84 (9)	Rb1^iii—O1—Rb1^iv	156.34 (17)
O1^iii—Rb1—O3	78.02 (11)	Mn1^i—O2—Na	168.2 (3)
O1^iv—Rb1—O3	122.30 (12)	Mn1^i—O2—Rb1	97.0 (3)
O3^v—Rb1—O3	44.55 (11)	Na—O2—Rb1	94.83 (18)
O1—Rb2—O2^iv	90.91 (12)	Mn1^i—O2—Rb2^iv	99.71 (10)
O1—Rb2—O2^iii	90.91 (12)	Na—O2—Rb2^iv	81.27 (10)
O2^iv—Rb2—O2^iii	159.13 (18)	Rb1—O2—Rb2^iv	85.08 (10)
O1—Rb2—O2^vi	164.20 (14)	Mn1^i—O2—Rb2^iii	99.71 (10)
O2^iv—Rb2—O2^vi	86.30 (12)	Na—O2—Rb2^iii	81.27 (10)
O2^iii—Rb2—O2^vi	86.30 (12)	Rb1—O2—Rb2^iii	85.08 (10)
O1—Rb2—O3^iii	85.84 (11)	Rb2^iv—O2—Rb2^iii	159.13 (18)
O2^iv—Rb2—O3^iii	129.58 (11)	Mn1^i—O2—Rb2^xvi	90.5 (2)
O2^iii—Rb2—O3^iii	71.29 (11)	Na—O2—Rb2^xvi	77.75 (19)
O2^vi—Rb2—O3^iii	107.87 (12)	Rb1—O2—Rb2^xvi	172.6 (2)
O1—Rb2—O3^ii	85.84 (11)	Rb2^iv—O2—Rb2^xvi	93.70 (12)
O2^iv—Rb2—O3^ii	71.29 (11)	Rb2^iii—O2—Rb2^xvi	93.70 (12)
O2^iii—Rb2—O3^ii	129.58 (11)	Mn1—O3—Na^xiv	143.3 (3)
O2^vi—Rb2—O3^ii	107.87 (12)	Mn1—O3—Na	92.72 (15)
O3^iii—Rb2—O3^ii	58.29 (12)	Na^xiv—O3—Na	92.26 (14)
O1—Rb2—O3^viii	93.81 (11)	Mn1—O3—Rb1^iii	95.98 (17)
O2^iv—Rb2—O3^viii	50.96 (11)	Na^xiv—O3—Rb1^iii	102.05 (13)
O2^iii—Rb2—O3^viii	108.18 (11)	Na—O3—Rb1^iii	142.13 (19)
O2^vi—Rb2—O3^viii	72.40 (11)	Mn1—O3—Rb2^iii	145.3 (2)
O3^iii—Rb2—O3^viii	179.35 (11)	Na^xiv—O3—Rb2^iii	70.34 (11)
O3^ii—Rb2—O3^viii	122.24 (10)	Na—O3—Rb2^iii	72.92 (10)
O1—Rb2—O3^ix	93.81 (11)	Rb1^iii—O3—Rb2^iii	79.20 (10)
O2^iv—Rb2—O3^ix	108.18 (11)	Mn1—O3—Rb2^ix	87.06 (14)
O2^iii—Rb2—O3^ix	50.96 (11)	Na^xiv—O3—Rb2^ix	69.67 (12)
O2^vi—Rb2—O3^ix	72.40 (11)	Na—O3—Rb2^ix	146.92 (19)
O3^iii—Rb2—O3^ix	122.24 (10)	Rb1^iii—O3—Rb2^ix	70.49 (8)
O3^ii—Rb2—O3^ix	179.35 (11)	Rb2^iii—O3—Rb2^ix	122.24 (10)
O3^viii—Rb2—O3^ix	57.22 (12)	Mn1—O3—Rb2^xii	77.03 (15)
O1—Rb2—O3^x	142.63 (9)	Na^xiv—O3—Rb2^xii	71.55 (13)
O2^iv—Rb2—O3^x	71.57 (13)	Na—O3—Rb2^xii	67.20 (12)
O2^iii—Rb2—O3^x	117.23 (13)	Rb1^iii—O3—Rb2^xii	150.63 (13)
O2^vi—Rb2—O3^x	50.29 (10)	Rb2^iii—O3—Rb2^xii	122.42 (11)
O3^iii—Rb2—O3^x	81.20 (8)	Rb2^ix—O3—Rb2^xii	80.60 (10)
O3^ii—Rb2—O3^x	57.58 (11)	Mn1—O3—Rb1	75.02 (15)
O3^viii—Rb2—O3^x	99.40 (10)	Na^xiv—O3—Rb1	141.32 (16)
O3^ix—Rb2—O3^x	122.69 (7)	Na—O3—Rb1	76.75 (13)
O1—Rb2—O3^vii	142.63 (9)	Rb1^iii—O3—Rb1	70.16 (9)
O2^iv—Rb2—O3^vii	117.23 (13)	Rb2^iii—O3—Rb1	70.98 (9)
O2^iii—Rb2—O3^vii	71.57 (13)	Rb2^ix—O3—Rb1	134.37 (12)
O2^vi—Rb2—O3^vii	50.29 (11)	Rb2^xii—O3—Rb1	132.63 (10)
O3^iii—Rb2—O3^vii	57.58 (11)

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