Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008690/hb2296sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008690/hb2296Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (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
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.
Na3Ca2BiO6 | F(000) = 1632 |
Mr = 454.11 | Dx = 4.687 Mg m−3 |
Orthorhombic, Fddd | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -F 2uv 2vw | Cell parameters from 2630 reflections |
a = 6.7039 (8) Å | θ = 3.8–30.0° |
b = 9.6251 (11) Å | µ = 29.17 mm−1 |
c = 19.947 (2) Å | T = 294 K |
V = 1287.1 (3) Å3 | Cut plate, yellow |
Z = 8 | 0.05 × 0.04 × 0.03 mm |
Bruker SMART APEX CCD diffractometer | 499 independent reflections |
Radiation source: fine-focus sealed tube | 414 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
ω scans | θmax = 30.5°, θmin = 3.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2003) | h = −9→9 |
Tmin = 0.778, Tmax = 1.000 | k = −13→13 |
5827 measured reflections | l = −28→28 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.08 | Δρmax = 0.92 e Å−3 |
499 reflections | Δρmin = −0.65 e Å−3 |
32 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00027 (2) |
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. |
x | y | z | Uiso*/Ueq | ||
Bi1 | 0.1250 | 0.1250 | 0.6250 | 0.00649 (8) | |
Ca1 | 0.1250 | 0.1250 | 0.45560 (4) | 0.00951 (17) | |
Na1 | 0.1250 | 0.1250 | 0.1250 | 0.0161 (6) | |
Na2 | 0.1250 | 0.1250 | 0.28796 (9) | 0.0092 (3) | |
O1 | 0.1250 | 0.4051 (3) | 0.1250 | 0.0108 (6) | |
O2 | 0.4013 (4) | 0.1212 (3) | 0.04863 (11) | 0.0103 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Bi1 | 0.00614 (12) | 0.00677 (11) | 0.00656 (11) | 0.000 | 0.000 | 0.000 |
Ca1 | 0.0095 (4) | 0.0099 (4) | 0.0092 (4) | −0.0007 (9) | 0.000 | 0.000 |
Na1 | 0.0072 (13) | 0.0288 (15) | 0.0122 (12) | 0.000 | 0.000 | 0.000 |
Na2 | 0.0085 (9) | 0.0096 (8) | 0.0094 (8) | −0.0016 (19) | 0.000 | 0.000 |
O1 | 0.0122 (16) | 0.0089 (13) | 0.0113 (14) | 0.000 | −0.0009 (14) | 0.000 |
O2 | 0.0081 (11) | 0.0131 (11) | 0.0097 (10) | −0.0001 (12) | −0.0015 (8) | −0.0005 (8) |
Bi1—O1i | 2.117 (3) | Na1—O1xi | 2.696 (3) |
Bi1—O1ii | 2.117 (3) | Na2—O1vii | 2.4305 (13) |
Bi1—O2iii | 2.138 (2) | Na2—O1viii | 2.4305 (13) |
Bi1—O2iv | 2.138 (2) | Na2—O2xiv | 2.458 (3) |
Bi1—O2v | 2.138 (2) | Na2—O2xv | 2.458 (3) |
Bi1—O2vi | 2.138 (2) | Na2—O2xiii | 2.533 (3) |
Ca1—O1vii | 2.3404 (7) | Na2—O2xii | 2.533 (3) |
Ca1—O1viii | 2.3404 (7) | O1—Bi1xvi | 2.117 (3) |
Ca1—O2ix | 2.378 (3) | O1—Ca1viii | 2.3404 (7) |
Ca1—O2x | 2.378 (3) | O1—Ca1xvii | 2.3405 (7) |
Ca1—O2iv | 2.386 (2) | O1—Na2xvii | 2.4305 (13) |
Ca1—O2iii | 2.386 (2) | O1—Na2viii | 2.4305 (13) |
Na1—O2 | 2.398 (2) | O2—Bi1xviii | 2.138 (2) |
Na1—O2xi | 2.398 (2) | O2—Ca1x | 2.378 (3) |
Na1—O2xii | 2.398 (2) | O2—Ca1xviii | 2.386 (2) |
Na1—O2xiii | 2.398 (2) | O2—Na2xvii | 2.458 (3) |
Na1—O1 | 2.696 (3) | O2—Na2xiii | 2.533 (3) |
O1i—Bi1—O1ii | 180.0 | O1vii—Na2—O1viii | 88.82 (6) |
O1i—Bi1—O2iii | 90.98 (7) | O1vii—Na2—O2xiv | 76.73 (10) |
O1ii—Bi1—O2iii | 89.02 (7) | O1viii—Na2—O2xiv | 96.08 (10) |
O1i—Bi1—O2iv | 89.02 (7) | O1vii—Na2—O2xv | 96.08 (10) |
O1ii—Bi1—O2iv | 90.98 (7) | O1viii—Na2—O2xv | 76.73 (10) |
O2iii—Bi1—O2iv | 89.13 (12) | O2xiv—Na2—O2xv | 170.06 (13) |
O1i—Bi1—O2v | 90.98 (7) | O1vii—Na2—O2xiii | 173.28 (9) |
O1ii—Bi1—O2v | 89.02 (7) | O1viii—Na2—O2xiii | 88.92 (5) |
O2iii—Bi1—O2v | 178.04 (14) | O2xiv—Na2—O2xiii | 97.23 (8) |
O2iv—Bi1—O2v | 90.90 (13) | O2xv—Na2—O2xiii | 89.56 (9) |
O1i—Bi1—O2vi | 89.02 (7) | O1vii—Na2—O2xii | 88.92 (5) |
O1ii—Bi1—O2vi | 90.98 (7) | O1viii—Na2—O2xii | 173.28 (9) |
O2iii—Bi1—O2vi | 90.90 (13) | O2xiv—Na2—O2xii | 89.56 (9) |
O2iv—Bi1—O2vi | 178.04 (14) | O2xv—Na2—O2xii | 97.23 (8) |
O2v—Bi1—O2vi | 89.13 (13) | O2xiii—Na2—O2xii | 94.01 (12) |
O1vii—Ca1—O1viii | 93.22 (4) | Bi1xvi—O1—Ca1viii | 97.11 (8) |
O1vii—Ca1—O2ix | 78.42 (10) | Bi1xvi—O1—Ca1xvii | 97.10 (8) |
O1viii—Ca1—O2ix | 98.74 (10) | Ca1viii—O1—Ca1xvii | 165.79 (16) |
O1vii—Ca1—O2x | 98.74 (10) | Bi1xvi—O1—Na2xvii | 96.84 (8) |
O1viii—Ca1—O2x | 78.42 (10) | Ca1viii—O1—Na2xvii | 89.33 (4) |
O2ix—Ca1—O2x | 175.93 (12) | Ca1xvii—O1—Na2xvii | 88.98 (4) |
O1vii—Ca1—O2iv | 94.71 (6) | Bi1xvi—O1—Na2viii | 96.84 (8) |
O1viii—Ca1—O2iv | 170.47 (8) | Ca1viii—O1—Na2viii | 88.98 (4) |
O2ix—Ca1—O2iv | 88.04 (9) | Ca1xvii—O1—Na2viii | 89.33 (4) |
O2x—Ca1—O2iv | 95.13 (9) | Na2xvii—O1—Na2viii | 166.32 (15) |
O1vii—Ca1—O2iii | 170.47 (8) | Bi1xvi—O1—Na1 | 180.0 |
O1viii—Ca1—O2iii | 94.71 (6) | Ca1viii—O1—Na1 | 82.89 (8) |
O2ix—Ca1—O2iii | 95.13 (9) | Ca1xvii—O1—Na1 | 82.90 (8) |
O2x—Ca1—O2iii | 88.04 (9) | Na2xvii—O1—Na1 | 83.16 (8) |
O2iv—Ca1—O2iii | 77.92 (12) | Na2viii—O1—Na1 | 83.16 (8) |
O2—Na1—O2xi | 101.13 (11) | Bi1xviii—O2—Ca1x | 95.41 (10) |
O2—Na1—O2xii | 78.89 (11) | Bi1xviii—O2—Ca1xviii | 96.47 (9) |
O2xi—Na1—O2xii | 178.25 (12) | Ca1x—O2—Ca1xviii | 91.96 (9) |
O2—Na1—O2xiii | 178.25 (12) | Bi1xviii—O2—Na1 | 95.10 (8) |
O2xi—Na1—O2xiii | 78.89 (11) | Ca1x—O2—Na1 | 88.89 (8) |
O2xii—Na1—O2xiii | 101.13 (11) | Ca1xviii—O2—Na1 | 168.26 (11) |
O2—Na1—O1 | 90.88 (6) | Bi1xviii—O2—Na2xvii | 95.44 (9) |
O2xi—Na1—O1 | 89.12 (6) | Ca1x—O2—Na2xvii | 169.09 (12) |
O2xii—Na1—O1 | 89.12 (6) | Ca1xviii—O2—Na2xvii | 87.85 (9) |
O2xiii—Na1—O1 | 90.88 (6) | Na1—O2—Na2xvii | 89.11 (9) |
O2—Na1—O1xi | 89.12 (6) | Bi1xviii—O2—Na2xiii | 176.96 (13) |
O2xi—Na1—O1xi | 90.88 (6) | Ca1x—O2—Na2xiii | 86.33 (8) |
O2xii—Na1—O1xi | 90.87 (6) | Ca1xviii—O2—Na2xiii | 85.94 (8) |
O2xiii—Na1—O1xi | 89.12 (6) | Na1—O2—Na2xiii | 82.43 (8) |
O1—Na1—O1xi | 180.0 | Na2xvii—O2—Na2xiii | 82.77 (8) |
Symmetry codes: (i) −x+1/4, −y+3/4, z+1/2; (ii) x, y−1/2, z+1/2; (iii) x−1/2, y, z+1/2; (iv) −x+3/4, −y+1/4, z+1/2; (v) −x+3/4, y, −z+3/4; (vi) x−1/2, −y+1/4, −z+3/4; (vii) x+1/4, y−1/4, −z+1/2; (viii) −x, −y+1/2, −z+1/2; (ix) x−1/4, 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) x−1/4, −y+1/2, z+1/4; (xv) −x+1/2, y−1/4, z+1/4; (xvi) x, y+1/2, z−1/2; (xvii) x+1/4, −y+1/2, z−1/4; (xviii) x+1/2, y, z−1/2. |