Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802009005/br6050sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802009005/br6050Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Co-O) = 0.004 Å
- R factor = 0.043
- wR factor = 0.115
- Data-to-parameter ratio = 23.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level B:
DIFMX_01 Alert B The maximum difference density is > 0.1*ZMAX*1.00 _refine_diff_density_max given = 6.370 Test value = 5.600
Author response: Not great, but we assign this to a difficult shaped (needle) crystal and a less than perfect absorption correction. Attempts to model a split-site Ba species were unsuccessful. |
Alert Level C:
DIFMX_02 Alert C The minimum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. General Notes
ABSTM_02 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 1.143 Tmax scaled 0.688 Tmin scaled 0.034
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Shape Software, 1999); software used to prepare material for publication: SHELXL97.
Ba2Co(SeO3)2Cl2 | F(000) = 578 |
Mr = 658.44 | Dx = 4.746 Mg m−3 |
Orthorhombic, Pnnm | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2 2n | Cell parameters from 2656 reflections |
a = 6.7635 (4) Å | θ = 3.2–32.5° |
b = 12.6454 (7) Å | µ = 18.70 mm−1 |
c = 5.3866 (3) Å | T = 293 K |
V = 460.70 (5) Å3 | Needle, pale purple |
Z = 2 | 0.48 × 0.02 × 0.02 mm |
Bruker SMART1000 CCD diffractometer | 902 independent reflections |
Radiation source: fine-focus sealed tube | 837 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
ω scans | θmax = 32.5°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | h = −10→10 |
Tmin = 0.030, Tmax = 0.602 | k = −17→19 |
3658 measured reflections | l = −8→4 |
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)] = 0.044 | w = 1/[σ2(Fo2) + (0.0817P)2 + 0.2871P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.115 | (Δ/σ)max < 0.001 |
S = 1.13 | Δρmax = 6.37 e Å−3 |
902 reflections | Δρmin = −2.51 e Å−3 |
39 parameters | Extinction correction: SHELXL (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0066 (13) |
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 | ||
Ba1 | 0.29903 (6) | 0.26908 (3) | 0.5000 | 0.01271 (19) | |
Co1 | 0.0000 | 0.0000 | 0.5000 | 0.0107 (3) | |
Se1 | 0.25482 (11) | 0.07257 (5) | 0.0000 | 0.0108 (2) | |
O1 | 0.1015 (5) | 0.1079 (3) | 0.2392 (6) | 0.0135 (7) | |
O2 | 0.4136 (9) | 0.1752 (4) | 0.0000 | 0.0193 (10) | |
Cl1 | 0.3234 (3) | −0.10316 (16) | 0.5000 | 0.0179 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.0109 (3) | 0.0097 (3) | 0.0176 (3) | −0.00136 (12) | 0.000 | 0.000 |
Co1 | 0.0130 (6) | 0.0068 (5) | 0.0123 (5) | −0.0017 (4) | 0.000 | 0.000 |
Se1 | 0.0118 (4) | 0.0063 (3) | 0.0142 (3) | 0.0014 (2) | 0.000 | 0.000 |
O1 | 0.0171 (18) | 0.0109 (14) | 0.0124 (14) | −0.0005 (13) | 0.0040 (11) | 0.0013 (11) |
O2 | 0.013 (2) | 0.020 (2) | 0.024 (2) | −0.006 (2) | 0.000 | 0.000 |
Cl1 | 0.0169 (8) | 0.0155 (7) | 0.0213 (7) | 0.0021 (6) | 0.000 | 0.000 |
Ba1—O2i | 2.700 (6) | Co1—O1ii | 2.075 (3) |
Ba1—O1 | 2.813 (3) | Co1—O1ix | 2.075 (3) |
Ba1—O1ii | 2.813 (3) | Co1—O1 | 2.075 (3) |
Ba1—O1iii | 2.875 (4) | Co1—O1x | 2.075 (3) |
Ba1—O1iv | 2.875 (4) | Co1—Cl1x | 2.5465 (19) |
Ba1—O2 | 3.043 (3) | Co1—Cl1 | 2.5465 (19) |
Ba1—O2v | 3.043 (3) | Se1—O2 | 1.685 (6) |
Ba1—Cl1vi | 3.2480 (12) | Se1—O1xi | 1.713 (3) |
Ba1—Cl1vii | 3.2480 (12) | Se1—O1 | 1.713 (3) |
Ba1—Cl1viii | 3.305 (2) | ||
O2i—Ba1—O1 | 74.36 (13) | O2—Ba1—Cl1viii | 63.63 (10) |
O2i—Ba1—O1ii | 74.36 (13) | O2v—Ba1—Cl1viii | 63.63 (10) |
O1—Ba1—O1ii | 59.92 (13) | Cl1vi—Ba1—Cl1viii | 120.84 (4) |
O2i—Ba1—O1iii | 123.09 (12) | Cl1vii—Ba1—Cl1viii | 120.84 (4) |
O1—Ba1—O1iii | 162.52 (12) | O1ii—Co1—O1ix | 180.00 (14) |
O1ii—Ba1—O1iii | 120.41 (6) | O1ii—Co1—O1 | 85.21 (18) |
O2i—Ba1—O1iv | 123.09 (12) | O1ix—Co1—O1 | 94.79 (18) |
O1—Ba1—O1iv | 120.41 (6) | O1ii—Co1—O1x | 94.79 (18) |
O1ii—Ba1—O1iv | 162.52 (12) | O1ix—Co1—O1x | 85.21 (18) |
O1iii—Ba1—O1iv | 53.25 (13) | O1—Co1—O1x | 180.00 (14) |
O2i—Ba1—O2 | 110.33 (13) | O1ii—Co1—Cl1x | 86.98 (11) |
O1—Ba1—O2 | 52.87 (12) | O1ix—Co1—Cl1x | 93.02 (11) |
O1ii—Ba1—O2 | 106.28 (12) | O1—Co1—Cl1x | 86.98 (11) |
O1iii—Ba1—O2 | 115.24 (12) | O1x—Co1—Cl1x | 93.02 (11) |
O1iv—Ba1—O2 | 68.48 (12) | O1ii—Co1—Cl1 | 93.02 (11) |
O2i—Ba1—O2v | 110.33 (13) | O1ix—Co1—Cl1 | 86.98 (11) |
O1—Ba1—O2v | 106.28 (12) | O1—Co1—Cl1 | 93.02 (11) |
O1ii—Ba1—O2v | 52.87 (12) | O1x—Co1—Cl1 | 86.98 (11) |
O1iii—Ba1—O2v | 68.48 (12) | Cl1x—Co1—Cl1 | 180.0 |
O1iv—Ba1—O2v | 115.24 (12) | O2—Se1—O1xi | 100.65 (17) |
O2—Ba1—O2v | 124.5 (2) | O2—Se1—O1 | 100.65 (17) |
O2i—Ba1—Cl1vi | 67.93 (6) | O1xi—Se1—O1 | 97.5 (2) |
O1—Ba1—Cl1vi | 130.81 (8) | Se1—O1—Co1 | 122.54 (18) |
O1ii—Ba1—Cl1vi | 79.94 (7) | Se1—O1—Ba1 | 106.09 (16) |
O1iii—Ba1—Cl1vi | 62.65 (7) | Co1—O1—Ba1 | 107.19 (12) |
O1iv—Ba1—Cl1vi | 106.49 (8) | Se1—O1—Ba1xii | 103.58 (14) |
O2—Ba1—Cl1vi | 173.06 (10) | Co1—O1—Ba1xii | 115.07 (15) |
O2v—Ba1—Cl1vi | 61.64 (10) | Ba1—O1—Ba1xii | 99.77 (10) |
O2i—Ba1—Cl1vii | 67.93 (6) | Se1—O2—Ba1xiii | 144.7 (3) |
O1—Ba1—Cl1vii | 79.94 (7) | Se1—O2—Ba1 | 97.94 (14) |
O1ii—Ba1—Cl1vii | 130.81 (8) | Ba1xiii—O2—Ba1 | 98.29 (12) |
O1iii—Ba1—Cl1vii | 106.49 (8) | Se1—O2—Ba1xiv | 97.94 (14) |
O1iv—Ba1—Cl1vii | 62.65 (7) | Ba1xiii—O2—Ba1xiv | 98.29 (12) |
O2—Ba1—Cl1vii | 61.64 (10) | Ba1—O2—Ba1xiv | 124.5 (2) |
O2v—Ba1—Cl1vii | 173.06 (10) | Co1—Cl1—Ba1xv | 92.06 (4) |
Cl1vi—Ba1—Cl1vii | 112.04 (6) | Co1—Cl1—Ba1xvi | 92.06 (4) |
O2i—Ba1—Cl1viii | 155.71 (13) | Ba1xv—Cl1—Ba1xvi | 112.04 (6) |
O1—Ba1—Cl1viii | 84.66 (8) | Co1—Cl1—Ba1viii | 171.41 (8) |
O1ii—Ba1—Cl1viii | 84.66 (8) | Ba1xv—Cl1—Ba1viii | 83.17 (4) |
O1iii—Ba1—Cl1viii | 78.09 (8) | Ba1xvi—Cl1—Ba1viii | 83.17 (4) |
O1iv—Ba1—Cl1viii | 78.09 (8) |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x, y, −z+1; (iii) x+1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, −z+1/2; (v) x, y, z+1; (vi) −x+1/2, y+1/2, −z+3/2; (vii) −x+1/2, y+1/2, −z+1/2; (viii) −x+1, −y, −z+1; (ix) −x, −y, z; (x) −x, −y, −z+1; (xi) x, y, −z; (xii) x−1/2, −y+1/2, z−1/2; (xiii) x+1/2, −y+1/2, z−1/2; (xiv) x, y, z−1; (xv) −x+1/2, y−1/2, −z+1/2; (xvi) −x+1/2, y−1/2, −z+3/2. |