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Single crystals of the title compound, Na3Ca2BiO6, were grown from a high-temperature reactive flux solution of Na2CO3. Na3Ca2BiO6 crystallizes as an ordered rock-salt structure (space group Fddd), in which the octa­hedral holes in the oxide array are filled by an ordered 3:2:1 arrangement of Na+, Ca2+ and Bi5+ cations. All atoms except for one O atom lie on special positions; site symmetries are as follows: Bi 222, Ca 2, Na 222 and 2, O 2.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008690/hb2296sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008690/hb2296Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](i-O) = 0.002 Å
  • R factor = 0.013
  • wR factor = 0.032
  • Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ?
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.778 1.000 Tmin and Tmax expected: 0.259 0.417 RR = 1.251 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.26 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.42 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.417 Tmax scaled 0.417 Tmin scaled 0.324
0 ALERT level A = In general: serious problem 8 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART-NT (Bruker, 2003); cell refinement: SAINT-Plus-NT (Bruker, 2003); data reduction: SAINT-Plus-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL.

trisodium dicalcium bismuth hexaoxide top
Crystal data top
Na3Ca2BiO6F(000) = 1632
Mr = 454.11Dx = 4.687 Mg m3
Orthorhombic, FdddMo Kα radiation, λ = 0.71073 Å
Hall symbol: -F 2uv 2vwCell parameters from 2630 reflections
a = 6.7039 (8) Åθ = 3.8–30.0°
b = 9.6251 (11) ŵ = 29.17 mm1
c = 19.947 (2) ÅT = 294 K
V = 1287.1 (3) Å3Cut plate, yellow
Z = 80.05 × 0.04 × 0.03 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
499 independent reflections
Radiation source: fine-focus sealed tube414 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
ω scansθmax = 30.5°, θmin = 3.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
h = 99
Tmin = 0.778, Tmax = 1.000k = 1313
5827 measured reflectionsl = 2828
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.013 w = 1/[σ2(Fo2) + (0.0159P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.032(Δ/σ)max < 0.001
S = 1.08Δρmax = 0.92 e Å3
499 reflectionsΔρmin = 0.65 e Å3
32 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00027 (2)
Special details top

Experimental. Data crystal cleaved from larger plate

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
Bi10.12500.12500.62500.00649 (8)
Ca10.12500.12500.45560 (4)0.00951 (17)
Na10.12500.12500.12500.0161 (6)
Na20.12500.12500.28796 (9)0.0092 (3)
O10.12500.4051 (3)0.12500.0108 (6)
O20.4013 (4)0.1212 (3)0.04863 (11)0.0103 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.00614 (12)0.00677 (11)0.00656 (11)0.0000.0000.000
Ca10.0095 (4)0.0099 (4)0.0092 (4)0.0007 (9)0.0000.000
Na10.0072 (13)0.0288 (15)0.0122 (12)0.0000.0000.000
Na20.0085 (9)0.0096 (8)0.0094 (8)0.0016 (19)0.0000.000
O10.0122 (16)0.0089 (13)0.0113 (14)0.0000.0009 (14)0.000
O20.0081 (11)0.0131 (11)0.0097 (10)0.0001 (12)0.0015 (8)0.0005 (8)
Geometric parameters (Å, º) top
Bi1—O1i2.117 (3)Na1—O1xi2.696 (3)
Bi1—O1ii2.117 (3)Na2—O1vii2.4305 (13)
Bi1—O2iii2.138 (2)Na2—O1viii2.4305 (13)
Bi1—O2iv2.138 (2)Na2—O2xiv2.458 (3)
Bi1—O2v2.138 (2)Na2—O2xv2.458 (3)
Bi1—O2vi2.138 (2)Na2—O2xiii2.533 (3)
Ca1—O1vii2.3404 (7)Na2—O2xii2.533 (3)
Ca1—O1viii2.3404 (7)O1—Bi1xvi2.117 (3)
Ca1—O2ix2.378 (3)O1—Ca1viii2.3404 (7)
Ca1—O2x2.378 (3)O1—Ca1xvii2.3405 (7)
Ca1—O2iv2.386 (2)O1—Na2xvii2.4305 (13)
Ca1—O2iii2.386 (2)O1—Na2viii2.4305 (13)
Na1—O22.398 (2)O2—Bi1xviii2.138 (2)
Na1—O2xi2.398 (2)O2—Ca1x2.378 (3)
Na1—O2xii2.398 (2)O2—Ca1xviii2.386 (2)
Na1—O2xiii2.398 (2)O2—Na2xvii2.458 (3)
Na1—O12.696 (3)O2—Na2xiii2.533 (3)
O1i—Bi1—O1ii180.0O1vii—Na2—O1viii88.82 (6)
O1i—Bi1—O2iii90.98 (7)O1vii—Na2—O2xiv76.73 (10)
O1ii—Bi1—O2iii89.02 (7)O1viii—Na2—O2xiv96.08 (10)
O1i—Bi1—O2iv89.02 (7)O1vii—Na2—O2xv96.08 (10)
O1ii—Bi1—O2iv90.98 (7)O1viii—Na2—O2xv76.73 (10)
O2iii—Bi1—O2iv89.13 (12)O2xiv—Na2—O2xv170.06 (13)
O1i—Bi1—O2v90.98 (7)O1vii—Na2—O2xiii173.28 (9)
O1ii—Bi1—O2v89.02 (7)O1viii—Na2—O2xiii88.92 (5)
O2iii—Bi1—O2v178.04 (14)O2xiv—Na2—O2xiii97.23 (8)
O2iv—Bi1—O2v90.90 (13)O2xv—Na2—O2xiii89.56 (9)
O1i—Bi1—O2vi89.02 (7)O1vii—Na2—O2xii88.92 (5)
O1ii—Bi1—O2vi90.98 (7)O1viii—Na2—O2xii173.28 (9)
O2iii—Bi1—O2vi90.90 (13)O2xiv—Na2—O2xii89.56 (9)
O2iv—Bi1—O2vi178.04 (14)O2xv—Na2—O2xii97.23 (8)
O2v—Bi1—O2vi89.13 (13)O2xiii—Na2—O2xii94.01 (12)
O1vii—Ca1—O1viii93.22 (4)Bi1xvi—O1—Ca1viii97.11 (8)
O1vii—Ca1—O2ix78.42 (10)Bi1xvi—O1—Ca1xvii97.10 (8)
O1viii—Ca1—O2ix98.74 (10)Ca1viii—O1—Ca1xvii165.79 (16)
O1vii—Ca1—O2x98.74 (10)Bi1xvi—O1—Na2xvii96.84 (8)
O1viii—Ca1—O2x78.42 (10)Ca1viii—O1—Na2xvii89.33 (4)
O2ix—Ca1—O2x175.93 (12)Ca1xvii—O1—Na2xvii88.98 (4)
O1vii—Ca1—O2iv94.71 (6)Bi1xvi—O1—Na2viii96.84 (8)
O1viii—Ca1—O2iv170.47 (8)Ca1viii—O1—Na2viii88.98 (4)
O2ix—Ca1—O2iv88.04 (9)Ca1xvii—O1—Na2viii89.33 (4)
O2x—Ca1—O2iv95.13 (9)Na2xvii—O1—Na2viii166.32 (15)
O1vii—Ca1—O2iii170.47 (8)Bi1xvi—O1—Na1180.0
O1viii—Ca1—O2iii94.71 (6)Ca1viii—O1—Na182.89 (8)
O2ix—Ca1—O2iii95.13 (9)Ca1xvii—O1—Na182.90 (8)
O2x—Ca1—O2iii88.04 (9)Na2xvii—O1—Na183.16 (8)
O2iv—Ca1—O2iii77.92 (12)Na2viii—O1—Na183.16 (8)
O2—Na1—O2xi101.13 (11)Bi1xviii—O2—Ca1x95.41 (10)
O2—Na1—O2xii78.89 (11)Bi1xviii—O2—Ca1xviii96.47 (9)
O2xi—Na1—O2xii178.25 (12)Ca1x—O2—Ca1xviii91.96 (9)
O2—Na1—O2xiii178.25 (12)Bi1xviii—O2—Na195.10 (8)
O2xi—Na1—O2xiii78.89 (11)Ca1x—O2—Na188.89 (8)
O2xii—Na1—O2xiii101.13 (11)Ca1xviii—O2—Na1168.26 (11)
O2—Na1—O190.88 (6)Bi1xviii—O2—Na2xvii95.44 (9)
O2xi—Na1—O189.12 (6)Ca1x—O2—Na2xvii169.09 (12)
O2xii—Na1—O189.12 (6)Ca1xviii—O2—Na2xvii87.85 (9)
O2xiii—Na1—O190.88 (6)Na1—O2—Na2xvii89.11 (9)
O2—Na1—O1xi89.12 (6)Bi1xviii—O2—Na2xiii176.96 (13)
O2xi—Na1—O1xi90.88 (6)Ca1x—O2—Na2xiii86.33 (8)
O2xii—Na1—O1xi90.87 (6)Ca1xviii—O2—Na2xiii85.94 (8)
O2xiii—Na1—O1xi89.12 (6)Na1—O2—Na2xiii82.43 (8)
O1—Na1—O1xi180.0Na2xvii—O2—Na2xiii82.77 (8)
Symmetry codes: (i) x+1/4, y+3/4, z+1/2; (ii) x, y1/2, z+1/2; (iii) x1/2, y, z+1/2; (iv) x+3/4, y+1/4, z+1/2; (v) x+3/4, y, z+3/4; (vi) x1/2, y+1/4, z+3/4; (vii) x+1/4, y1/4, z+1/2; (viii) x, y+1/2, z+1/2; (ix) x1/4, y+1/4, z+1/2; (x) x+1/2, y, z+1/2; (xi) x+1/4, y+1/4, z; (xii) x, y+1/4, z+1/4; (xiii) x+1/4, y, z+1/4; (xiv) x1/4, y+1/2, z+1/4; (xv) x+1/2, y1/4, z+1/4; (xvi) x, y+1/2, z1/2; (xvii) x+1/4, y+1/2, z1/4; (xviii) x+1/2, y, z1/2.
 

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