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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 \overline{4}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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806033186/wm2042sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806033186/wm2042Isup2.hkl
Contains datablock I

CCDC reference: 621520

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.011 Å
  • H-atom completeness 35%
  • Disorder in main residue
  • R factor = 0.023
  • wR factor = 0.068
  • Data-to-parameter ratio = 11.8

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
Author Response: Inorganic structure; there is only an ammonium cation.

Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O1 PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2W .. 2.69 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2W .. 2.69 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2W .. 2.69 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2W .. 2.69 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.123 0.199 Tmin and Tmax expected: 0.046 0.092 RR = 1.234 Please check that your absorption correction is appropriate. CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 470.38 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 4.00 48.04 H 1.01 4.00 4.03 N 14.01 1.00 14.01 O 16.00 11.72 187.51 Bi 208.98 1.00 208.98 Calculated formula weight 462.57 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 470.38 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.18 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.46 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O1W PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O2W PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C4 H11.74 Bi1 N1 O11.72 Atom count from _chemical_formula_moiety:C4 H11.44 Bi1 N1 O11.72 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C4 H11.74 Bi1 N1 O11.72 Atom count from the _atom_site data: C4 H4 Bi1 N1 O11.72 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 0.462 Tmax scaled 0.092 Tmin scaled 0.057 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C4 H11.74 Bi N O11.72 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 16.00 16.00 0.00 H 46.96 16.00 30.96 Bi 4.00 4.00 0.00 N 4.00 4.00 0.00 O 46.88 46.88 0.00
1 ALERT level A = In general: serious problem 5 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 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 (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]·3.72H2ODx = 2.477 Mg m3
Mr = 470.38Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/amdCell parameters from 2126 reflections
Hall symbol: -I 4bd 2θ = 2.6–28.0°
a = 11.674 (1) ŵ = 14.04 mm1
c = 9.2545 (8) ÅT = 295 K
V = 1261.2 (2) Å3Block, colourless
Z = 40.24 × 0.20 × 0.17 mm
F(000) = 878
Data collection top
Bruker APEX area-detector
diffractometer
401 independent reflections
Radiation source: fine-focus sealed tube365 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 27.5°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1315
Tmin = 0.123, Tmax = 0.199k = 1114
3231 measured reflectionsl = 612
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: isomorphous structure methods
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H 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 parametersΔρmax = 0.76 e Å3
14 restraintsΔρmin = 0.49 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Bi10.50000.25000.62500.0298 (2)
O10.2966 (5)0.25000.5729 (7)0.071 (2)
O20.1202 (5)0.25000.6607 (6)0.059 (2)
O1w0.25000.25000.25000.19 (2)0.62
O2w0.203 (3)0.047 (3)0.37500.22 (1)0.62
C10.2260 (7)0.25000.6738 (8)0.046 (2)
N10.00000.25000.37500.090 (9)
H10.0596 (4)0.25000.427 (2)0.108*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.0315 (2)0.0315 (2)0.0264 (3)0.0000.0000.000
O10.039 (3)0.139 (7)0.034 (3)0.0000.002 (3)0.000
O20.034 (3)0.112 (6)0.030 (2)0.0000.003 (2)0.000
O1w0.19 (2)0.20 (2)0.17 (2)0.0000.01 (1)0.000
O2w0.22 (1)0.22 (1)0.22 (2)0.01 (1)0.022 (6)0.022 (6)
C10.034 (4)0.078 (5)0.028 (3)0.0000.002 (3)0.000
N10.12 (1)0.12 (1)0.029 (8)0.0000.0000.000
Geometric parameters (Å, º) top
Bi1—O12.423 (6)Bi1—O2vi2.429 (6)
Bi1—O1i2.423 (6)Bi1—O2vii2.429 (6)
Bi1—O1ii2.423 (6)O1—C11.25 (1)
Bi1—O1iii2.423 (6)O2—C11.24 (1)
Bi1—O2iv2.429 (6)C1—C1vii1.52 (2)
Bi1—O2v2.429 (6)N1—H10.85 (1)
O1i—Bi1—O1ii92.3 (1)O1—Bi1—O2vii66.2 (2)
O1i—Bi1—O192.3 (1)O1iii—Bi1—O2vii80.7 (1)
O1ii—Bi1—O1157.0 (3)O2vi—Bi1—O2vii131.8 (2)
O1i—Bi1—O1iii157.0 (3)O2iv—Bi1—O2vii70.6 (3)
O1ii—Bi1—O1iii92.27 (6)O1i—Bi1—O2v136.8 (2)
O1—Bi1—O1iii92.27 (6)O1ii—Bi1—O2v80.7 (1)
O1i—Bi1—O2vi66.2 (2)O1—Bi1—O2v80.65 (12)
O1ii—Bi1—O2vi80.7 (1)O1iii—Bi1—O2v66.2 (2)
O1—Bi1—O2vi80.7 (1)O2vi—Bi1—O2v70.6 (3)
O1iii—Bi1—O2vi136.8 (2)O2iv—Bi1—O2v131.8 (2)
O1i—Bi1—O2iv80.7 (1)O2vii—Bi1—O2v131.8 (2)
O1ii—Bi1—O2iv66.2 (2)C1—O1—Bi1120.0 (5)
O1—Bi1—O2iv136.8 (2)C1—O2—Bi1vii119.7 (5)
O1iii—Bi1—O2iv80.7 (1)O2—C1—O1125.9 (8)
O2vi—Bi1—O2iv131.8 (2)O2—C1—C1vii117.3 (9)
O1i—Bi1—O2vii80.7 (1)O1—C1—C1vii116.8 (9)
O1ii—Bi1—O2vii136.8 (2)
O1i—Bi1—O1—C178.8 (1)O2v—Bi1—O1—C1144.2 (1)
O1ii—Bi1—O1—C1180.0Bi1vii—O2—C1—O1180.0
O1iii—Bi1—O1—C178.8 (1)Bi1vii—O2—C1—C1vii0.0
O2vi—Bi1—O1—C1144.2 (1)Bi1—O1—C1—O2180.0
O2iv—Bi1—O1—C10.0Bi1—O1—C1—C1vii0.0
O2vii—Bi1—O1—C10.0
Symmetry codes: (i) y+1/4, x1/4, 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, z1/4; (vi) y+3/4, x+1/4, z1/4; (vii) x+1/2, y+1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O20.85 (1)2.27 (2)2.996 (3)143 (1)
 

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