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The title compound, (H3O)[Ni(C2H6N4O2)3]I3 or (H3O)[Ni(H2oxado)3]I3, where H2oxado = oxamide dioxime, contains six [Ni(H2oxado)3]2+ cations, six H3O+ cations and eighteen I anions in the unit cell. The Ni atom lies on a position of site symmetry 32 and the hydronium cation is disordered on a position of site symmetry \overline{3}. The crystal packing is consolidated by O—H...O hydrogen bonds that link the cations along c into positively charged pillars. The proton balancing the charge of the iodide ions is attached to the water mol­ecule of crystallization, thus forming a hydro­nium ion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680603621X/om2032sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680603621X/om2032Isup2.hkl
Contains datablock I

CCDC reference: 624958

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.027
  • wR factor = 0.059
  • Data-to-parameter ratio = 26.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H1 .. H3 .. 2.01 Ang.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT031_ALERT_4_C Refined Extinction Parameter within Range ...... 3.20 Sigma PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O2 PLAT733_ALERT_1_C Torsion Calc 44.4(4), Rep 44.38(16) ...... 2.50 su-Ra N1 -NI -N1 -C 5.555 1.555 1.555 1.555
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 35.08 From the CIF: _reflns_number_total 1557 From the CIF: _diffrn_reflns_limit_ max hkl 24. 25. 23. From the CIF: _diffrn_reflns_limit_ min hkl -24. -25. -23. TEST1: Expected hkl limits for theta max Calculated maximum hkl 26. 26. 23. Calculated minimum hkl -26. -26. -23.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 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: WinXpose (Stoe & Cie, 2002); cell refinement: RECIPE (Stoe & Cie, 2002); data reduction: INTEGRATE (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97 and DIAMOND.

Hydronium tris(oxamide dioxime-κ2N,N')nickel(II) triiodide top
Crystal data top
(H3O)[Ni(C2H6N2O2)3]I3Dx = 2.488 Mg m3
Mr = 812.76Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3cCell parameters from 2000 reflections
Hall symbol: -R 3 2"cθ = 2.0–35.1°
a = 16.105 (2) ŵ = 5.22 mm1
c = 14.488 (3) ÅT = 100 K
V = 3254.4 (9) Å3Hexagonal, pink–red
Z = 60.11 × 0.09 × 0.05 mm
F(000) = 2304
Data collection top
Stoe IPDS-II
diffractometer
1557 independent reflections
Radiation source: fine-focus sealed tube1461 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
ω scansθmax = 35.1°, θmin = 4.1°
Absorption correction: numerical
[X-RED32 (Stoe & Cie, 2001); crystal description using FACEIT (Stoe & Cie, 2002); optimization using equivalent reflections (X-SHAPE; Stoe & Cie, 1999)]
h = 2424
Tmin = 0.450, Tmax = 0.678k = 2525
13652 measured reflectionsl = 2323
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.059 w = [1-exp(-10(sinθ/λ)2)]/ [σ2(Fo2) + 30.9996*P + (0.0144P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max = 0.001
1557 reflectionsΔρmax = 1.49 e Å3
60 parametersΔρmin = 1.19 e Å3
4 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00016 (5)
Special details top

Experimental. collection of intensity data: φ = 0 and ω oscillation scans, Δω = 0.8°, crystal to detector distance (60 mm), lattice parameters from Stoe IPDS-II diffraction data using Mo Kα radiation

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*/UeqOcc. (<1)
I0.452326 (12)0.452326 (12)0.25000.01007 (7)
Ni0.00000.00000.25000.00642 (12)
N10.07560 (14)0.12434 (14)0.32316 (11)0.0082 (3)
N20.22242 (15)0.26688 (15)0.33919 (13)0.0116 (3)
H2A0.207 (3)0.278 (3)0.397 (2)0.014*
H2B0.2846 (19)0.300 (3)0.321 (3)0.014*
O10.05674 (13)0.14547 (13)0.41334 (10)0.0102 (3)
H10.013 (3)0.159 (3)0.406 (3)0.015*
O20.00000.00000.50000.0114 (7)
H30.034 (6)0.002 (8)0.452 (4)0.017*0.50
C0.16157 (15)0.18706 (15)0.29531 (13)0.0071 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I0.00996 (9)0.00996 (9)0.01000 (9)0.00477 (7)0.00081 (3)0.00081 (3)
Ni0.00634 (17)0.00634 (17)0.0066 (2)0.00317 (9)0.0000.000
N10.0084 (7)0.0091 (7)0.0061 (6)0.0037 (6)0.0021 (5)0.0014 (5)
N20.0102 (8)0.0097 (8)0.0114 (7)0.0022 (6)0.0017 (6)0.0025 (6)
O10.0116 (7)0.0124 (7)0.0068 (6)0.0062 (6)0.0025 (5)0.0011 (5)
O20.0126 (9)0.0126 (9)0.0090 (10)0.0063 (4)0.0000.000
C0.0080 (8)0.0067 (8)0.0070 (7)0.0040 (7)0.0005 (6)0.0002 (6)
Geometric parameters (Å, º) top
Ni—N12.0440 (19)N1—O11.421 (2)
Ni—N1i2.0440 (18)N2—C1.326 (3)
Ni—N1ii2.0440 (18)N2—H2A0.92 (2)
Ni—N1iii2.0440 (19)N2—H2B0.91 (3)
Ni—N1iv2.0440 (18)O1—H10.84 (3)
Ni—N1v2.0440 (18)O2—H30.89 (3)
N1—C1.305 (3)C—Ciii1.493 (4)
N1—Ni—N1i167.85 (11)N1iii—Ni—N1v167.85 (11)
N1—Ni—N1ii94.02 (11)N1iv—Ni—N1v95.55 (7)
N1i—Ni—N1ii95.55 (7)C—N1—O1111.73 (17)
N1—Ni—N1iii76.06 (10)C—N1—Ni118.68 (14)
N1i—Ni—N1iii95.55 (7)O1—N1—Ni128.14 (13)
N1ii—Ni—N1iii95.55 (7)C—N2—H2A119 (3)
N1—Ni—N1iv95.55 (7)C—N2—H2B120 (3)
N1i—Ni—N1iv76.06 (10)H2A—N2—H2B119 (4)
N1ii—Ni—N1iv167.85 (11)N1—O1—H1105 (3)
N1iii—Ni—N1iv94.02 (11)N1—C—N2125.90 (19)
N1—Ni—N1v95.55 (7)N1—C—Ciii112.98 (11)
N1i—Ni—N1v94.02 (11)N2—C—Ciii121.12 (12)
N1ii—Ni—N1v76.06 (10)
N1i—Ni—N1—C44.38 (16)N1iii—Ni—N1—O1167.8 (2)
N1ii—Ni—N1—C97.49 (17)N1iv—Ni—N1—O175.04 (13)
N1iii—Ni—N1—C2.77 (11)N1v—Ni—N1—O121.10 (17)
N1iv—Ni—N1—C90.0 (2)O1—N1—C—N26.6 (3)
N1v—Ni—N1—C173.85 (17)Ni—N1—C—N2173.99 (18)
N1i—Ni—N1—O1120.67 (17)O1—N1—C—Ciii174.4 (2)
N1ii—Ni—N1—O197.46 (18)Ni—N1—C—Ciii7.0 (3)
Symmetry codes: (i) xy, y, z+1/2; (ii) x, x+y, z+1/2; (iii) y, x, z+1/2; (iv) x+y, x, z; (v) y, xy, z.
Selected bond distances (Å) involving non H atoms in (I)* top
Ni—N1i-v2.044 (2)[2.055 (5)]
N1—C1.304 (3)[1.293 (8)]
N1—O11.420 (2)[1.416 (7)]
N2—C1.325 (3)[1.310 (9)]
C—Ciii1.494 (4)[1.502 (8)]
* Values in brackets are from [Endres, 1985]

Symmetry codes: (i) -y, x-y, z (ii) -x+y, -x, z (iii) y, x, -z-1/2 (iv) x-y, -y, -z-1/2 (v) -x, -x+y, -z-1/2.
Atomic coordinates and isotropic displacement parameters (Ueq / Å2 × 104) for all H atoms in (I) top
AtomxyzUiso
H10.013 (3)0.159 (3)0.406 (3)150
H2A0.207 (3)0.278 (3)0.397 (2)140
H2B0.285 (2)0.300 (3)0.321 (3)140
H30.034 (6)-0.002 (8)0.452 (4)170
Selected torsion angles (°) for (I) top
O1—N1—C—N2-6.6 (3)
Ni—N1—C—N2-174.0 (2)
O1—N1—C—Ciii174.4 (2)
Ni—N1—C—Ciii6.97 (3)
Symmetry code: (iii) y, x, -z-1/2.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···Ivi0.92 (2)2.83 (3)3.717 (2)164 (4)
N2—H2B···I0.91 (3)2.78 (3)3.639 (2)158 (4)
O2—H3···O1vii0.89 (3)1.64 (6)2.400 (2)142 (9)
Symmetry codes: (vi) -y+2/3, x-y+1/3, z+1/3 (vii) -x+y, -x, z.
 

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