Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020453/wm6078sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020453/wm6078Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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).
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) Å3 | 0.30 × 0.15 × 0.10 mm |
Z = 2 |
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 on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.036 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.074 | w = 1/[σ2(Fo2) + (0.0291P)2] where P = (Fo2 + 2Fc2)/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 |
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. |
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) |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
Rb1—O2 | 2.923 (6) | Mn1—Rb2xii | 3.4999 (17) |
Rb1—O1i | 2.966 (4) | Mn1—Rb1xi | 3.5556 (16) |
Rb1—O1 | 2.971 (4) | Mn1—Rb1iv | 3.5939 (10) |
Rb1—O3ii | 2.989 (4) | Mn1—Rb1iii | 3.5939 (10) |
Rb1—O3iii | 2.989 (4) | Mn1—Rb2xiii | 3.7273 (10) |
Rb1—O1iii | 3.0560 (11) | Mn1—Rb2ix | 3.7273 (10) |
Rb1—O1iv | 3.0560 (11) | Na—O2 | 2.262 (6) |
Rb1—Mn1i | 3.5556 (16) | Na—O3xiv | 2.316 (4) |
Rb1—Mn1 | 3.5576 (16) | Na—O3xv | 2.316 (4) |
Rb1—O3v | 3.594 (5) | Na—O3v | 2.415 (4) |
Rb1—O3 | 3.594 (5) | Na—O3 | 2.415 (4) |
Rb1—Mn1iv | 3.5939 (10) | Na—Rb2xii | 3.368 (3) |
Rb2—O1 | 2.805 (6) | Na—Rb2xvi | 3.386 (3) |
Rb2—O2iv | 3.0413 (11) | Na—Naxvii | 3.412 (3) |
Rb2—O2iii | 3.0413 (11) | Na—Naxiv | 3.412 (3) |
Rb2—O2vi | 3.045 (6) | Na—Rb2iii | 3.5039 (17) |
Rb2—O3iii | 3.345 (4) | Na—Rb2iv | 3.5039 (17) |
Rb2—O3ii | 3.345 (4) | O1—Rb1xi | 2.966 (4) |
Rb2—Navii | 3.368 (3) | O1—Rb1iii | 3.0560 (11) |
Rb2—Navi | 3.386 (3) | O1—Rb1iv | 3.0560 (11) |
Rb2—O3viii | 3.402 (4) | O2—Mn1i | 1.702 (5) |
Rb2—O3ix | 3.402 (4) | O2—Rb2iv | 3.0413 (11) |
Rb2—O3x | 3.462 (5) | O2—Rb2iii | 3.0413 (11) |
Rb2—O3vii | 3.462 (5) | O2—Rb2xvi | 3.045 (6) |
Mn1—O1 | 1.689 (6) | O3—Naxiv | 2.316 (4) |
Mn1—O2xi | 1.702 (5) | O3—Rb1iii | 2.989 (4) |
Mn1—O3 | 1.708 (3) | O3—Rb2iii | 3.345 (4) |
Mn1—O3v | 1.708 (3) | O3—Rb2ix | 3.402 (4) |
Mn1—Na | 3.024 (3) | O3—Rb2xii | 3.462 (5) |
O2—Rb1—O1i | 56.58 (16) | O3ii—Rb2—O3vii | 81.20 (8) |
O2—Rb1—O1 | 112.14 (15) | O3viii—Rb2—O3vii | 122.69 (7) |
O1i—Rb1—O1 | 168.7 (2) | O3ix—Rb2—O3vii | 99.40 (10) |
O2—Rb1—O3ii | 141.09 (8) | O3x—Rb2—O3vii | 46.33 (12) |
O1i—Rb1—O3ii | 99.66 (12) | O1—Mn1—O2xi | 110.8 (2) |
O1—Rb1—O3ii | 89.78 (12) | O1—Mn1—O3 | 110.21 (17) |
O2—Rb1—O3iii | 141.09 (9) | O2xi—Mn1—O3 | 109.86 (18) |
O1i—Rb1—O3iii | 99.66 (12) | O1—Mn1—O3v | 110.21 (17) |
O1—Rb1—O3iii | 89.78 (12) | O2xi—Mn1—O3v | 109.86 (18) |
O3ii—Rb1—O3iii | 66.04 (14) | O3—Mn1—O3v | 105.8 (2) |
O2—Rb1—O1iii | 88.42 (10) | O2—Na—O3xiv | 113.03 (16) |
O1i—Rb1—O1iii | 79.36 (8) | O2—Na—O3xv | 113.03 (16) |
O1—Rb1—O1iii | 101.45 (8) | O3xiv—Na—O3xv | 89.4 (2) |
O3ii—Rb1—O1iii | 119.43 (13) | O2—Na—O3v | 105.73 (19) |
O3iii—Rb1—O1iii | 54.87 (12) | O3xiv—Na—O3v | 138.90 (14) |
O2—Rb1—O1iv | 88.42 (10) | O3xv—Na—O3v | 87.74 (14) |
O1i—Rb1—O1iv | 79.36 (8) | O2—Na—O3 | 105.73 (19) |
O1—Rb1—O1iv | 101.45 (8) | O3xiv—Na—O3 | 87.74 (14) |
O3ii—Rb1—O1iv | 54.87 (12) | O3xv—Na—O3 | 138.90 (14) |
O3iii—Rb1—O1iv | 119.43 (13) | O3v—Na—O3 | 68.65 (17) |
O1iii—Rb1—O1iv | 156.34 (17) | Mn1—O1—Rb2 | 175.5 (2) |
O2—Rb1—O3v | 68.95 (12) | Mn1—O1—Rb1xi | 95.69 (19) |
O1i—Rb1—O3v | 120.93 (11) | Rb2—O1—Rb1xi | 79.80 (12) |
O1—Rb1—O3v | 49.11 (11) | Mn1—O1—Rb1 | 95.60 (18) |
O3ii—Rb1—O3v | 109.84 (10) | Rb2—O1—Rb1 | 88.92 (15) |
O3iii—Rb1—O3v | 138.80 (6) | Rb1xi—O1—Rb1 | 168.7 (2) |
O1iii—Rb1—O3v | 122.30 (11) | Mn1—O1—Rb1iii | 94.02 (10) |
O1iv—Rb1—O3v | 78.02 (11) | Rb2—O1—Rb1iii | 86.86 (10) |
Mn1i—Rb1—O3v | 95.12 (6) | Rb1xi—O1—Rb1iii | 100.64 (8) |
Mn1—Rb1—O3v | 27.62 (6) | Rb1—O1—Rb1iii | 78.55 (8) |
O2—Rb1—O3 | 68.95 (12) | Mn1—O1—Rb1iv | 94.03 (10) |
O1i—Rb1—O3 | 120.93 (11) | Rb2—O1—Rb1iv | 86.86 (10) |
O1—Rb1—O3 | 49.11 (11) | Rb1xi—O1—Rb1iv | 100.64 (8) |
O3ii—Rb1—O3 | 138.80 (6) | Rb1—O1—Rb1iv | 78.55 (8) |
O3iii—Rb1—O3 | 109.84 (9) | Rb1iii—O1—Rb1iv | 156.34 (17) |
O1iii—Rb1—O3 | 78.02 (11) | Mn1i—O2—Na | 168.2 (3) |
O1iv—Rb1—O3 | 122.30 (12) | Mn1i—O2—Rb1 | 97.0 (3) |
O3v—Rb1—O3 | 44.55 (11) | Na—O2—Rb1 | 94.83 (18) |
O1—Rb2—O2iv | 90.91 (12) | Mn1i—O2—Rb2iv | 99.71 (10) |
O1—Rb2—O2iii | 90.91 (12) | Na—O2—Rb2iv | 81.27 (10) |
O2iv—Rb2—O2iii | 159.13 (18) | Rb1—O2—Rb2iv | 85.08 (10) |
O1—Rb2—O2vi | 164.20 (14) | Mn1i—O2—Rb2iii | 99.71 (10) |
O2iv—Rb2—O2vi | 86.30 (12) | Na—O2—Rb2iii | 81.27 (10) |
O2iii—Rb2—O2vi | 86.30 (12) | Rb1—O2—Rb2iii | 85.08 (10) |
O1—Rb2—O3iii | 85.84 (11) | Rb2iv—O2—Rb2iii | 159.13 (18) |
O2iv—Rb2—O3iii | 129.58 (11) | Mn1i—O2—Rb2xvi | 90.5 (2) |
O2iii—Rb2—O3iii | 71.29 (11) | Na—O2—Rb2xvi | 77.75 (19) |
O2vi—Rb2—O3iii | 107.87 (12) | Rb1—O2—Rb2xvi | 172.6 (2) |
O1—Rb2—O3ii | 85.84 (11) | Rb2iv—O2—Rb2xvi | 93.70 (12) |
O2iv—Rb2—O3ii | 71.29 (11) | Rb2iii—O2—Rb2xvi | 93.70 (12) |
O2iii—Rb2—O3ii | 129.58 (11) | Mn1—O3—Naxiv | 143.3 (3) |
O2vi—Rb2—O3ii | 107.87 (12) | Mn1—O3—Na | 92.72 (15) |
O3iii—Rb2—O3ii | 58.29 (12) | Naxiv—O3—Na | 92.26 (14) |
O1—Rb2—O3viii | 93.81 (11) | Mn1—O3—Rb1iii | 95.98 (17) |
O2iv—Rb2—O3viii | 50.96 (11) | Naxiv—O3—Rb1iii | 102.05 (13) |
O2iii—Rb2—O3viii | 108.18 (11) | Na—O3—Rb1iii | 142.13 (19) |
O2vi—Rb2—O3viii | 72.40 (11) | Mn1—O3—Rb2iii | 145.3 (2) |
O3iii—Rb2—O3viii | 179.35 (11) | Naxiv—O3—Rb2iii | 70.34 (11) |
O3ii—Rb2—O3viii | 122.24 (10) | Na—O3—Rb2iii | 72.92 (10) |
O1—Rb2—O3ix | 93.81 (11) | Rb1iii—O3—Rb2iii | 79.20 (10) |
O2iv—Rb2—O3ix | 108.18 (11) | Mn1—O3—Rb2ix | 87.06 (14) |
O2iii—Rb2—O3ix | 50.96 (11) | Naxiv—O3—Rb2ix | 69.67 (12) |
O2vi—Rb2—O3ix | 72.40 (11) | Na—O3—Rb2ix | 146.92 (19) |
O3iii—Rb2—O3ix | 122.24 (10) | Rb1iii—O3—Rb2ix | 70.49 (8) |
O3ii—Rb2—O3ix | 179.35 (11) | Rb2iii—O3—Rb2ix | 122.24 (10) |
O3viii—Rb2—O3ix | 57.22 (12) | Mn1—O3—Rb2xii | 77.03 (15) |
O1—Rb2—O3x | 142.63 (9) | Naxiv—O3—Rb2xii | 71.55 (13) |
O2iv—Rb2—O3x | 71.57 (13) | Na—O3—Rb2xii | 67.20 (12) |
O2iii—Rb2—O3x | 117.23 (13) | Rb1iii—O3—Rb2xii | 150.63 (13) |
O2vi—Rb2—O3x | 50.29 (10) | Rb2iii—O3—Rb2xii | 122.42 (11) |
O3iii—Rb2—O3x | 81.20 (8) | Rb2ix—O3—Rb2xii | 80.60 (10) |
O3ii—Rb2—O3x | 57.58 (11) | Mn1—O3—Rb1 | 75.02 (15) |
O3viii—Rb2—O3x | 99.40 (10) | Naxiv—O3—Rb1 | 141.32 (16) |
O3ix—Rb2—O3x | 122.69 (7) | Na—O3—Rb1 | 76.75 (13) |
O1—Rb2—O3vii | 142.63 (9) | Rb1iii—O3—Rb1 | 70.16 (9) |
O2iv—Rb2—O3vii | 117.23 (13) | Rb2iii—O3—Rb1 | 70.98 (9) |
O2iii—Rb2—O3vii | 71.57 (13) | Rb2ix—O3—Rb1 | 134.37 (12) |
O2vi—Rb2—O3vii | 50.29 (11) | Rb2xii—O3—Rb1 | 132.63 (10) |
O3iii—Rb2—O3vii | 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. |