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Na3[OsO4(OH)2] contains osmium(VII) coordinated octa­hedrally by four oxide and two hydroxide groups. The OsO4(OH)2 octa­hedra form zigzag chains parallel to [010], linked by hydrogen bridges. Two O atoms, one Na and the Os atom lie on a mirror plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005034/wm6135sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005034/wm6135Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](s-O) = 0.005 Å
  • R factor = 0.023
  • wR factor = 0.053
  • Data-to-parameter ratio = 15.3

checkCIF/PLATON results

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Alert level C 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 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART32 (Bruker, 2000); cell refinement: SAINT32 (Bruker, 2000); data reduction: SAINT32; 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: SHELXL97.

Trisodium dihydroxotetraoxoosmate(VII) top
Crystal data top
Na3OsO4(OH)2F(000) = 318
Mr = 357.19Dx = 4.223 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 1930 reflections
a = 5.7605 (5) Åθ = 3.9–34.4°
b = 9.2995 (7) ŵ = 22.89 mm1
c = 5.9485 (5) ÅT = 293 K
β = 118.168 (2)°Block, black
V = 280.92 (4) Å30.25 × 0.13 × 0.08 mm
Z = 2
Data collection top
Bruker SMART APEX CCD
diffractometer
871 independent reflections
Radiation source: fine-focus sealed tube814 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.065
ω scansθmax = 30.0°, θmin = 3.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1998)
h = 88
Tmin = 0.042, Tmax = 0.160k = 1313
3488 measured reflectionsl = 88
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024All H-atom parameters refined
wR(F2) = 0.053 w = 1/[σ2(Fo2) + (0.0209P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
871 reflectionsΔρmax = 1.94 e Å3
57 parametersΔρmin = 1.62 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0032 (9)
Special details top

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
xyzUiso*/Ueq
Na10.0207 (6)0.25000.0150 (6)0.0293 (7)
Na20.4553 (4)0.0719 (2)0.7497 (4)0.0242 (4)
Os0.78102 (5)0.25000.38101 (4)0.01551 (11)
O11.1298 (10)0.25000.5210 (10)0.0227 (10)
O20.4624 (10)0.25000.1089 (10)0.0278 (12)
O30.7415 (7)0.1095 (4)0.5701 (7)0.0242 (8)
O40.8200 (7)0.0850 (4)0.1473 (7)0.0217 (7)
H0.958 (13)0.039 (6)0.241 (11)0.019 (15)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0198 (14)0.044 (2)0.0265 (14)0.0000.0132 (12)0.000
Na20.0204 (10)0.0277 (11)0.0229 (9)0.0027 (8)0.0088 (8)0.0002 (8)
Os0.01277 (14)0.01910 (18)0.01401 (14)0.0000.00579 (10)0.000
O10.017 (2)0.024 (3)0.023 (2)0.0000.0059 (19)0.000
O20.018 (2)0.037 (3)0.023 (2)0.0000.006 (2)0.000
O30.0270 (19)0.025 (2)0.0245 (16)0.0002 (15)0.0153 (15)0.0052 (15)
O40.0179 (16)0.0245 (19)0.0184 (15)0.0004 (15)0.0050 (13)0.0036 (14)
Geometric parameters (Å, º) top
Os—O11.775 (5)Na2—O4x2.436 (5)
Os—O21.784 (5)Na2—O2ix2.689 (5)
Os—O31.807 (4)Na2—Na2xi3.078 (4)
Os—O3i1.807 (4)Na2—Osx3.228 (2)
Os—O42.152 (4)Na2—Na2i3.313 (4)
Os—O4i2.152 (4)Na2—Na1xii3.318 (3)
O4—H0.84 (6)Na2—Na2x3.510 (4)
O4—O3ii2.910 (5)Na2—O3iv3.744 (4)
Na1—O22.291 (6)Os—Na1xii3.183 (3)
Na1—O4iii2.383 (5)Os—Na2x3.228 (2)
Na1—O4iv2.383 (5)Os—Na2xiii3.228 (2)
Na1—O3v2.577 (5)Os—Na1xiv3.244 (3)
Na1—O3vi2.577 (5)O1—Na2xv2.388 (4)
Na1—O1iv2.945 (6)O1—Na2xiv2.388 (4)
Na1—Osv3.183 (3)O1—Na1xiv2.945 (6)
Na1—Osiv3.244 (3)O2—Na2viii2.689 (5)
Na1—Na2v3.318 (3)O2—Na2vii2.689 (5)
Na1—Na2vi3.318 (3)O3—Na2x2.390 (5)
Na1—Na2vii3.779 (4)O3—Na1xii2.577 (5)
Na1—Na2viii3.779 (4)O3—O4ii2.910 (5)
Na2—O4ix2.309 (4)O4—Na2viii2.309 (4)
Na2—O32.376 (5)O4—Na1xiv2.383 (5)
Na2—O1iv2.388 (4)O4—Na2x2.436 (5)
Na2—O3x2.390 (5)
O2—Na1—O4iii123.19 (16)O1—Os—O2151.3 (3)
O2—Na1—O4iv123.19 (16)O3—Os—O4i178.54 (15)
O4iii—Na1—O4iv80.2 (2)O3i—Os—O4178.54 (15)
O2—Na1—O3v113.86 (17)O1—Os—O3i98.92 (17)
O4iii—Na1—O3v120.79 (18)O2—Os—O3i100.76 (17)
O4iv—Na1—O3v81.88 (14)O1—Os—O398.92 (17)
O2—Na1—O3vi113.86 (17)O2—Os—O3100.76 (17)
O4iii—Na1—O3vi81.88 (14)O3i—Os—O392.6 (3)
O4iv—Na1—O3vi120.79 (18)O1—Os—O482.13 (16)
O3v—Na1—O3vi60.96 (18)O2—Os—O477.90 (16)
O2—Na1—O1iv90.84 (19)O3—Os—O488.19 (18)
O4iii—Na1—O1iv57.14 (12)O1—Os—O4i82.13 (16)
O4iv—Na1—O1iv57.14 (12)O2—Os—O4i77.90 (16)
O3v—Na1—O1iv139.02 (13)O3i—Os—O4i88.19 (18)
O3vi—Na1—O1iv139.02 (13)O4—Os—O4i91.0 (2)
O2—Na1—Osv100.80 (16)O1—Os—Na1xii71.24 (18)
O4iii—Na1—Osv115.00 (12)O2—Os—Na1xii137.41 (19)
O4iv—Na1—Osv115.00 (12)O3i—Os—Na1xii54.02 (13)
O3v—Na1—Osv34.58 (9)O3—Os—Na1xii54.02 (13)
O3vi—Na1—Osv34.58 (9)O4—Os—Na1xii127.39 (10)
O1iv—Na1—Osv168.36 (15)O4i—Os—Na1xii127.39 (10)
O2—Na1—Osiv123.72 (17)O1—Os—Na2x111.61 (4)
O4iii—Na1—Osiv41.53 (10)O2—Os—Na2x69.22 (4)
O4iv—Na1—Osiv41.53 (10)O3i—Os—Na2x131.14 (14)
O3v—Na1—Osiv114.11 (13)O3—Os—Na2x46.89 (13)
O3vi—Na1—Osiv114.11 (13)O4—Os—Na2x49.00 (11)
O1iv—Na1—Osiv32.87 (11)O4i—Os—Na2x131.78 (11)
Osv—Na1—Osiv135.48 (10)Na1xii—Os—Na2x100.42 (4)
O2—Na1—Na2v148.86 (7)O1—Os—Na2xiii111.61 (4)
O4iii—Na1—Na2v85.69 (13)O2—Os—Na2xiii69.22 (4)
O4iv—Na1—Na2v44.10 (10)O3i—Os—Na2xiii46.89 (13)
O3v—Na1—Na2v45.42 (10)O3—Os—Na2xiii131.14 (14)
O3vi—Na1—Na2v78.73 (12)O4—Os—Na2xiii131.78 (11)
O1iv—Na1—Na2v97.00 (12)O4i—Os—Na2xiii49.00 (11)
Osv—Na1—Na2v72.99 (7)Na1xii—Os—Na2xiii100.42 (4)
Osiv—Na1—Na2v68.70 (7)Na2x—Os—Na2xiii136.06 (8)
O2—Na1—Na2vi148.86 (7)O1—Os—Na1xiv64.24 (18)
O4iii—Na1—Na2vi44.10 (10)O2—Os—Na1xiv87.1 (2)
O4iv—Na1—Na2vi85.69 (13)O3i—Os—Na1xiv132.34 (13)
O3v—Na1—Na2vi78.73 (12)O3—Os—Na1xiv132.34 (13)
O3vi—Na1—Na2vi45.42 (10)O4—Os—Na1xiv47.25 (11)
O1iv—Na1—Na2vi97.00 (12)O4i—Os—Na1xiv47.25 (11)
Osv—Na1—Na2vi72.99 (7)Na1xii—Os—Na1xiv135.48 (11)
Osiv—Na1—Na2vi68.70 (7)Na2x—Os—Na1xiv95.78 (4)
Na2v—Na1—Na2vi59.90 (9)Na2xiii—Os—Na1xiv95.78 (4)
O2—Na1—Na2vii44.74 (12)Os—O1—Na2xv132.68 (14)
O4iii—Na1—Na2vii113.64 (10)Os—O1—Na2xiv132.68 (14)
O4iv—Na1—Na2vii164.91 (13)Na2xv—O1—Na2xiv87.8 (2)
O3v—Na1—Na2vii95.20 (12)Na2xv—O1—O3137.4 (2)
O3vi—Na1—Na2vii69.26 (11)Na2xiv—O1—O394.01 (14)
O1iv—Na1—Na2vii124.14 (12)Na2xv—O1—O3i94.01 (14)
Osv—Na1—Na2vii65.93 (6)Na2xiv—O1—O3i137.4 (2)
Osiv—Na1—Na2vii148.47 (7)O3—O1—O3i57.4 (2)
Na2v—Na1—Na2vii138.83 (11)Os—O1—Na1xiv82.89 (19)
Na2vi—Na1—Na2vii108.36 (8)Na2xv—O1—Na1xiv109.00 (18)
O2—Na1—Na2viii44.74 (12)Na2xiv—O1—Na1xiv109.00 (17)
O4iii—Na1—Na2viii164.91 (13)O3—O1—Na1xiv110.48 (17)
O4iv—Na1—Na2viii113.64 (10)O3i—O1—Na1xiv110.48 (17)
O3v—Na1—Na2viii69.26 (11)Os—O2—Na1143.4 (3)
O3vi—Na1—Na2viii95.20 (12)Os—O2—Na2viii110.1 (2)
O1iv—Na1—Na2viii124.14 (12)Na1—O2—Na2viii98.41 (16)
Osv—Na1—Na2viii65.93 (6)Os—O2—Na2vii110.1 (2)
Osiv—Na1—Na2viii148.47 (7)Na1—O2—Na2vii98.41 (16)
Na2v—Na1—Na2viii108.36 (8)Na2viii—O2—Na2vii76.06 (17)
Na2vi—Na1—Na2viii138.83 (11)Na1—O2—O3i110.9 (2)
Na2vii—Na1—Na2viii52.00 (8)Na2viii—O2—O3i149.6 (2)
O4ix—Na2—O387.93 (15)Na2vii—O2—O3i106.30 (12)
O4ix—Na2—O1iv129.55 (16)Na1—O2—O3110.9 (2)
O3—Na2—O1iv99.61 (18)Na2viii—O2—O3106.30 (12)
O4ix—Na2—O3x135.49 (16)Na2vii—O2—O3149.6 (2)
O3—Na2—O3x85.13 (15)O3i—O2—O356.38 (19)
O1iv—Na2—O3x94.94 (15)Os—O3—Hii119.9 (18)
O4ix—Na2—O4x99.18 (14)Os—O3—Na2134.8 (2)
O3—Na2—O4x150.84 (16)Hii—O3—Na2103.8 (17)
O1iv—Na2—O4x97.44 (17)Os—O3—Na2x99.60 (17)
O3x—Na2—O4x69.93 (14)Hii—O3—Na2x85.6 (16)
O4ix—Na2—O2ix59.20 (15)Na2—O3—Na2x94.87 (15)
O3—Na2—O2ix120.88 (16)Os—O3—Na1xii91.39 (16)
O1iv—Na2—O2ix74.85 (15)Hii—O3—Na1xii80.5 (16)
O3x—Na2—O2ix152.98 (17)Na2—O3—Na1xii84.01 (15)
O4x—Na2—O2ix86.37 (14)Na2x—O3—Na1xii165.34 (19)
O4ix—Na2—Na2xi51.39 (12)Hii—O3—O3i131.5 (17)
O3—Na2—Na2xi131.62 (15)Na2—O3—O3i98.46 (11)
O1iv—Na2—Na2xi125.47 (18)Na2x—O3—O3i134.88 (10)
O3x—Na2—Na2xi105.27 (14)Na1xii—O3—O3i59.52 (9)
O4x—Na2—Na2xi47.79 (10)Hii—O3—O181.9 (18)
O2ix—Na2—Na2xi64.27 (10)Na2—O3—O1153.9 (2)
O4ix—Na2—Osx111.85 (12)Na2x—O3—O1111.01 (18)
O3—Na2—Osx109.35 (12)Na1xii—O3—O171.72 (15)
O1iv—Na2—Osx112.19 (11)O3i—O3—O161.31 (10)
O3x—Na2—Osx33.51 (10)Os—O3—O451.03 (13)
O4x—Na2—Osx41.80 (9)Hii—O3—O489.1 (17)
O2ix—Na2—Osx127.54 (12)Na2—O3—O4147.40 (19)
Na2xi—Na2—Osx71.89 (8)Na2x—O3—O455.82 (12)
O4ix—Na2—Na2i86.96 (11)Na1xii—O3—O4128.07 (18)
O3—Na2—Na2i81.54 (11)O3i—O3—O494.71 (11)
O1iv—Na2—Na2i46.08 (10)O1—O3—O456.43 (15)
O3x—Na2—Na2i134.88 (10)Hii—O3—O2142.6 (17)
O4x—Na2—Na2i126.80 (11)Na2—O3—O2108.26 (19)
O2ix—Na2—Na2i51.97 (9)Na2x—O3—O273.07 (12)
Na2xi—Na2—Na2i115.75 (8)Na1xii—O3—O2121.20 (16)
Osx—Na2—Na2i158.03 (4)O3i—O3—O261.81 (10)
O4ix—Na2—Na1xii45.91 (11)O1—O3—O277.84 (18)
O3—Na2—Na1xii50.57 (11)O4—O3—O253.51 (15)
O1iv—Na2—Na1xii104.15 (12)Os—O3—O4ii118.62 (18)
O3x—Na2—Na1xii133.67 (13)Na2—O3—O4ii104.26 (15)
O4x—Na2—Na1xii144.96 (12)Na2x—O3—O4ii88.71 (16)
O2ix—Na2—Na1xii73.35 (13)Na1xii—O3—O4ii77.46 (12)
Na2xi—Na2—Na1xii97.24 (10)O3i—O3—O4ii128.43 (11)
Osx—Na2—Na1xii141.54 (8)O1—O3—O4ii80.06 (14)
Na2i—Na2—Na1xii60.05 (5)O4—O3—O4ii90.25 (15)
O4ix—Na2—Na2x117.46 (14)O2—O3—O4ii143.71 (19)
O3—Na2—Na2x42.72 (11)Os—O4—Na2viii112.19 (17)
O1iv—Na2—Na2x99.88 (16)Os—O4—Na1xiv91.22 (15)
O3x—Na2—Na2x42.41 (10)Na2viii—O4—Na1xiv89.99 (15)
O4x—Na2—Na2x110.95 (13)Os—O4—Na2x89.20 (14)
O2ix—Na2—Na2x162.54 (15)Na2viii—O4—Na2x80.82 (14)
Na2xi—Na2—Na2x128.98 (14)Na1xiv—O4—Na2x170.22 (19)
Osx—Na2—Na2x69.92 (7)Na2viii—O4—O3118.40 (18)
Na2i—Na2—Na2x112.39 (7)Na1xiv—O4—O3129.37 (17)
Na1xii—Na2—Na2x92.30 (10)Na2x—O4—O354.25 (12)
O4ix—Na2—O3iv129.26 (13)Os—O4—O3ii113.37 (15)
O3—Na2—O3iv139.43 (15)Na2viii—O4—O3ii132.90 (18)
O1iv—Na2—O3iv46.49 (13)Na1xiv—O4—O3ii100.33 (16)
O3x—Na2—O3iv78.13 (14)Na2x—O4—O3ii88.45 (15)
O4x—Na2—O3iv50.98 (12)O3—O4—O3ii89.75 (15)
O2ix—Na2—O3iv76.82 (14)Os—O4—H107 (4)
Na2xi—Na2—O3iv88.65 (11)Na2viii—O4—H140 (4)
Osx—Na2—O3iv74.72 (8)Na1xiv—O4—H96 (4)
Na2i—Na2—O3iv84.64 (7)Na2x—O4—H93 (4)
Na1xii—Na2—O3iv143.21 (10)O3—O4—H87 (4)
Na2x—Na2—O3iv111.97 (10)
Symmetry codes: (i) x, y+1/2, z; (ii) x+2, y, z+1; (iii) x1, y+1/2, z; (iv) x1, y, z; (v) x1, y, z1; (vi) x1, y+1/2, z1; (vii) x, y+1/2, z1; (viii) x, y, z1; (ix) x, y, z+1; (x) x+1, y, z+1; (xi) x+1, y, z+2; (xii) x+1, y, z+1; (xiii) x+1, y+1/2, z+1; (xiv) x+1, y, z; (xv) x+1, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H···O3ii0.84 (6)2.08 (6)2.910 (5)169
Symmetry code: (ii) x+2, y, z+1.
 

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