metal-organic compounds
In the crystal structure of the title compound, poly[ammonium di-μ2-oxalato-bismuthate(III) 3.72-hydrate], NH4[Bi(C2O4)2]·3.72H2O, the Bi3+ ion and the centre of the [NH4]+ ion lie on different special positions of m2 site symmetry, and the oxalate group and one water molecule on different special positions of m site symmetry; the second water molecule lies on a special position of 2/m site symmetry. The Bi atom is eight-coordinate in a slightly distorted dodecahedral environment. This single-crystal redetermination improves the precision of the previous powder diffraction study [Vanhoyland et al. (2004). Inorg. Chem. 43, 785–789], as all non-H atoms have been refined anisotropically.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806033186/wm2042sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806033186/wm2042Isup2.hkl |
CCDC reference: 621520
Computing details top
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: atomic coordinates taken from published structure; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.
poly[ammonium di-µ2-oxalato-bismuthate(III) 3.72-hydrate] top
Crystal data top
NH4[Bi(C2O4)2]·3.72H2O | Dx = 2.477 Mg m−3 |
Mr = 470.38 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/amd | Cell parameters from 2126 reflections |
Hall symbol: -I 4bd 2 | θ = 2.6–28.0° |
a = 11.674 (1) Å | µ = 14.04 mm−1 |
c = 9.2545 (8) Å | T = 295 K |
V = 1261.2 (2) Å3 | Block, colourless |
Z = 4 | 0.24 × 0.20 × 0.17 mm |
F(000) = 878 |
Data collection top
Bruker APEX area-detector diffractometer | 401 independent reflections |
Radiation source: fine-focus sealed tube | 365 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
φ and ω scans | θmax = 27.5°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→15 |
Tmin = 0.123, Tmax = 0.199 | k = −11→14 |
3231 measured reflections | l = −6→12 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: isomorphous structure methods |
R[F2 > 2σ(F2)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.068 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0476P)2 + 3.0591P] where P = (Fo2 + 2Fc2)/3 |
401 reflections | (Δ/σ)max = 0.001 |
34 parameters | Δρmax = 0.76 e Å−3 |
14 restraints | Δρmin = −0.49 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Bi1 | 0.5000 | 0.2500 | 0.6250 | 0.0298 (2) | |
O1 | 0.2966 (5) | 0.2500 | 0.5729 (7) | 0.071 (2) | |
O2 | 0.1202 (5) | 0.2500 | 0.6607 (6) | 0.059 (2) | |
O1w | 0.2500 | 0.2500 | 0.2500 | 0.19 (2) | 0.62 |
O2w | 0.203 (3) | 0.047 (3) | 0.3750 | 0.22 (1) | 0.62 |
C1 | 0.2260 (7) | 0.2500 | 0.6738 (8) | 0.046 (2) | |
N1 | 0.0000 | 0.2500 | 0.3750 | 0.090 (9) | |
H1 | 0.0596 (4) | 0.2500 | 0.427 (2) | 0.108* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Bi1 | 0.0315 (2) | 0.0315 (2) | 0.0264 (3) | 0.000 | 0.000 | 0.000 |
O1 | 0.039 (3) | 0.139 (7) | 0.034 (3) | 0.000 | −0.002 (3) | 0.000 |
O2 | 0.034 (3) | 0.112 (6) | 0.030 (2) | 0.000 | −0.003 (2) | 0.000 |
O1w | 0.19 (2) | 0.20 (2) | 0.17 (2) | 0.000 | −0.01 (1) | 0.000 |
O2w | 0.22 (1) | 0.22 (1) | 0.22 (2) | −0.01 (1) | −0.022 (6) | −0.022 (6) |
C1 | 0.034 (4) | 0.078 (5) | 0.028 (3) | 0.000 | −0.002 (3) | 0.000 |
N1 | 0.12 (1) | 0.12 (1) | 0.029 (8) | 0.000 | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Bi1—O1 | 2.423 (6) | Bi1—O2vi | 2.429 (6) |
Bi1—O1i | 2.423 (6) | Bi1—O2vii | 2.429 (6) |
Bi1—O1ii | 2.423 (6) | O1—C1 | 1.25 (1) |
Bi1—O1iii | 2.423 (6) | O2—C1 | 1.24 (1) |
Bi1—O2iv | 2.429 (6) | C1—C1vii | 1.52 (2) |
Bi1—O2v | 2.429 (6) | N1—H1 | 0.85 (1) |
O1i—Bi1—O1ii | 92.3 (1) | O1—Bi1—O2vii | 66.2 (2) |
O1i—Bi1—O1 | 92.3 (1) | O1iii—Bi1—O2vii | 80.7 (1) |
O1ii—Bi1—O1 | 157.0 (3) | O2vi—Bi1—O2vii | 131.8 (2) |
O1i—Bi1—O1iii | 157.0 (3) | O2iv—Bi1—O2vii | 70.6 (3) |
O1ii—Bi1—O1iii | 92.27 (6) | O1i—Bi1—O2v | 136.8 (2) |
O1—Bi1—O1iii | 92.27 (6) | O1ii—Bi1—O2v | 80.7 (1) |
O1i—Bi1—O2vi | 66.2 (2) | O1—Bi1—O2v | 80.65 (12) |
O1ii—Bi1—O2vi | 80.7 (1) | O1iii—Bi1—O2v | 66.2 (2) |
O1—Bi1—O2vi | 80.7 (1) | O2vi—Bi1—O2v | 70.6 (3) |
O1iii—Bi1—O2vi | 136.8 (2) | O2iv—Bi1—O2v | 131.8 (2) |
O1i—Bi1—O2iv | 80.7 (1) | O2vii—Bi1—O2v | 131.8 (2) |
O1ii—Bi1—O2iv | 66.2 (2) | C1—O1—Bi1 | 120.0 (5) |
O1—Bi1—O2iv | 136.8 (2) | C1—O2—Bi1vii | 119.7 (5) |
O1iii—Bi1—O2iv | 80.7 (1) | O2—C1—O1 | 125.9 (8) |
O2vi—Bi1—O2iv | 131.8 (2) | O2—C1—C1vii | 117.3 (9) |
O1i—Bi1—O2vii | 80.7 (1) | O1—C1—C1vii | 116.8 (9) |
O1ii—Bi1—O2vii | 136.8 (2) | ||
O1i—Bi1—O1—C1 | 78.8 (1) | O2v—Bi1—O1—C1 | −144.2 (1) |
O1ii—Bi1—O1—C1 | 180.0 | Bi1vii—O2—C1—O1 | 180.0 |
O1iii—Bi1—O1—C1 | −78.8 (1) | Bi1vii—O2—C1—C1vii | 0.0 |
O2vi—Bi1—O1—C1 | 144.2 (1) | Bi1—O1—C1—O2 | 180.0 |
O2iv—Bi1—O1—C1 | 0.0 | Bi1—O1—C1—C1vii | 0.0 |
O2vii—Bi1—O1—C1 | 0.0 |
Symmetry codes: (i) y+1/4, x−1/4, −z+5/4; (ii) −x+1, y, z; (iii) y+1/4, −x+3/4, −z+5/4; (iv) x+1/2, −y+1/2, −z+3/2; (v) −y+3/4, x+1/4, z−1/4; (vi) −y+3/4, −x+1/4, z−1/4; (vii) −x+1/2, −y+1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O2 | 0.85 (1) | 2.27 (2) | 2.996 (3) | 143 (1) |