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The title compound, (C3H5N2)2[NiNa2Mo6O18(OH)6]·2H2O, features inversion-generated hexa­molybdonickelate anions (Ni site symmetry \overline{1}). The anions are linked by the octa­hedrally coordinated sodium cations into a three-dimensional network containing one-dimensional channels. The imidazolium cations are embedded in the channels and inter­act with the inorganic framework by way of N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045168/hb2183sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045168/hb2183Isup2.hkl
Contains datablock I

CCDC reference: 629832

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C)= 0.008 Å
  • R factor = 0.028
  • wR factor = 0.069
  • Data-to-parameter ratio = 13.7

checkCIF/PLATON results

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Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Poly[bis(imidazolium) hexahydroxooctadecaoxodisodiohexamolybdonickelate dihydrate] top
Crystal data top
(C3H5N2)2[NiNa2Mo6O18(OH)6]·2H2OF(000) = 1188
Mr = 1244.57Dx = 2.879 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 6347 reflections
a = 7.1305 (7) Åθ = 1.8–26.1°
b = 14.0039 (14) ŵ = 3.32 mm1
c = 14.7479 (15) ÅT = 296 K
β = 102.874 (1)°Prism, green
V = 1435.6 (2) Å30.25 × 0.21 × 0.14 mm
Z = 2
Data collection top
Bruker SMART APEX-II CCD
diffractometer
2814 independent reflections
Radiation source: fine-focus sealed tube2703 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
not measured scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 88
Tmin = 0.445, Tmax = 0.630k = 1517
7331 measured reflectionsl = 1815
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-atom parameters constrained
wR(F2) = 0.069 w = 1/[σ2(Fo2) + (0.0206P)2 + 9.957P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max < 0.001
2814 reflectionsΔρmax = 0.80 e Å3
206 parametersΔρmin = 0.92 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0231 (5)
Special details top

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*/Ueq
Ni0.00000.50000.50000.01257 (17)
Mo10.07365 (5)0.67175 (3)0.65600 (3)0.01292 (12)
Mo20.36732 (5)0.48311 (3)0.68195 (3)0.01291 (13)
Mo30.29397 (5)0.31256 (3)0.52397 (2)0.01282 (13)
Na10.3929 (3)0.22653 (13)0.77766 (13)0.0206 (4)
O10.2235 (4)0.4171 (2)0.4324 (2)0.0135 (6)
H10.29060.38790.45910.016*
O20.1519 (4)0.4263 (2)0.4211 (2)0.0139 (6)
H20.22130.46450.39620.017*
O30.1214 (4)0.5968 (2)0.4025 (2)0.0130 (6)
H30.02840.62440.37790.016*
O40.4567 (4)0.4169 (2)0.5843 (2)0.0161 (6)
O50.4354 (5)0.2801 (2)0.4485 (2)0.0219 (7)
O60.2697 (4)0.7470 (2)0.6856 (2)0.0185 (6)
O70.3416 (5)0.2294 (2)0.6111 (2)0.0223 (7)
O80.4016 (5)0.3987 (2)0.7687 (2)0.0223 (7)
O90.1722 (4)0.5572 (2)0.7252 (2)0.0162 (6)
O100.0700 (5)0.7060 (2)0.7285 (2)0.0224 (7)
O110.5614 (5)0.5578 (2)0.7125 (2)0.0216 (7)
O120.0467 (4)0.7347 (2)0.5427 (2)0.0162 (6)
O13w0.1901 (5)0.6633 (3)0.3528 (3)0.0428 (11)
H1w0.19830.70340.31080.051*
H2w0.26040.61430.34800.051*
N10.7968 (7)0.0464 (3)0.5884 (3)0.0298 (10)
H1n0.82660.04570.64820.036*
N20.7288 (8)0.0959 (4)0.4490 (3)0.0402 (12)
H2n0.70700.13360.40170.048*
C10.7723 (9)0.1226 (4)0.5367 (4)0.0365 (13)
H1a0.78370.18520.55810.044*
C20.7241 (9)0.0017 (5)0.4454 (4)0.0381 (13)
H2a0.69580.03920.39210.046*
C30.7676 (9)0.0322 (4)0.5325 (4)0.0341 (12)
H3a0.77650.09550.55200.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0134 (4)0.0104 (4)0.0131 (4)0.0018 (3)0.0011 (3)0.0008 (3)
Mo10.0128 (2)0.0117 (2)0.0138 (2)0.00080 (13)0.00198 (14)0.00316 (14)
Mo20.0141 (2)0.0100 (2)0.0131 (2)0.00057 (13)0.00020 (14)0.00008 (13)
Mo30.0149 (2)0.01111 (19)0.0122 (2)0.00333 (13)0.00245 (14)0.00013 (13)
Na10.0191 (9)0.0184 (9)0.0247 (10)0.0000 (7)0.0056 (7)0.0038 (7)
O10.0135 (14)0.0124 (14)0.0158 (15)0.0006 (11)0.0057 (11)0.0006 (12)
O20.0152 (14)0.0105 (14)0.0162 (15)0.0024 (11)0.0038 (12)0.0006 (12)
O30.0124 (14)0.0117 (14)0.0153 (14)0.0012 (11)0.0039 (11)0.0000 (12)
O40.0122 (14)0.0172 (15)0.0189 (15)0.0003 (12)0.0034 (12)0.0015 (12)
O50.0237 (17)0.0244 (17)0.0192 (17)0.0070 (14)0.0081 (13)0.0015 (14)
O60.0186 (15)0.0163 (15)0.0198 (16)0.0014 (12)0.0023 (12)0.0051 (13)
O70.0305 (18)0.0156 (16)0.0188 (17)0.0037 (13)0.0014 (14)0.0048 (13)
O80.0287 (18)0.0154 (16)0.0199 (17)0.0036 (13)0.0006 (14)0.0044 (13)
O90.0214 (16)0.0165 (15)0.0108 (14)0.0026 (12)0.0038 (12)0.0003 (12)
O100.0216 (17)0.0247 (17)0.0220 (17)0.0016 (14)0.0073 (13)0.0097 (14)
O110.0225 (17)0.0153 (16)0.0249 (17)0.0034 (13)0.0010 (13)0.0042 (13)
O120.0192 (15)0.0099 (14)0.0179 (16)0.0011 (12)0.0007 (12)0.0007 (12)
O13w0.025 (2)0.057 (3)0.050 (3)0.0097 (18)0.0152 (18)0.033 (2)
N10.043 (3)0.029 (2)0.018 (2)0.002 (2)0.0075 (18)0.0015 (18)
N20.057 (3)0.038 (3)0.025 (2)0.007 (2)0.008 (2)0.015 (2)
C10.053 (4)0.022 (3)0.038 (3)0.002 (2)0.017 (3)0.001 (2)
C20.041 (3)0.045 (3)0.027 (3)0.002 (3)0.006 (2)0.012 (3)
C30.051 (3)0.017 (2)0.034 (3)0.000 (2)0.007 (3)0.001 (2)
Geometric parameters (Å, º) top
Ni—O32.024 (3)Mo3—O22.276 (3)
Ni—O22.037 (3)Na1—O10ii2.302 (4)
Ni—O12.043 (3)Na1—O6iii2.363 (4)
Ni—O3i2.024 (3)Na1—O11iii2.386 (4)
Ni—O2i2.037 (3)Na1—O72.402 (4)
Ni—O1i2.043 (3)Na1—O82.417 (4)
Mo1—O101.705 (3)Na1—O5iv2.471 (4)
Mo1—O61.727 (3)O1—H10.7976
Mo1—O121.915 (3)O2—H20.8645
Mo1—O91.947 (3)O3—H30.9106
Mo1—O2i2.225 (3)O13w—H1w0.8474
Mo1—O1i2.238 (3)O13w—H2w0.8624
Mo2—O111.713 (3)N1—C11.300 (7)
Mo2—O81.719 (3)N1—C31.363 (7)
Mo2—O41.936 (3)N1—H1n0.8600
Mo2—O91.953 (3)N2—C11.315 (8)
Mo2—O3i2.215 (3)N2—C21.367 (8)
Mo2—O1i2.253 (3)N2—H2n0.8600
Mo3—O71.711 (3)C1—H1a0.9300
Mo3—O51.722 (3)C2—C31.324 (8)
Mo3—O12i1.934 (3)C2—H2a0.9300
Mo3—O41.953 (3)C3—H3a0.9300
Mo3—O3i2.213 (3)
O3i—Ni—O3180.0O3i—Mo3—O273.21 (11)
O3i—Ni—O2i97.54 (12)O10ii—Na1—O6iii169.29 (15)
O3—Ni—O2i82.46 (12)O10ii—Na1—O11iii90.04 (13)
O3i—Ni—O282.46 (12)O6iii—Na1—O11iii89.32 (13)
O3—Ni—O297.54 (12)O10ii—Na1—O792.23 (13)
O2i—Ni—O2180.0O6iii—Na1—O798.48 (13)
O3i—Ni—O1i82.53 (12)O11iii—Na1—O793.80 (13)
O3—Ni—O1i97.47 (12)O10ii—Na1—O899.20 (13)
O2i—Ni—O1i83.65 (12)O6iii—Na1—O881.61 (12)
O2—Ni—O1i96.35 (12)O11iii—Na1—O8170.76 (14)
O3i—Ni—O197.47 (12)O7—Na1—O885.84 (12)
O3—Ni—O182.53 (12)O10ii—Na1—O5iv85.97 (13)
O2i—Ni—O196.35 (12)O6iii—Na1—O5iv83.32 (12)
O2—Ni—O183.65 (12)O11iii—Na1—O5iv85.24 (13)
O1i—Ni—O1180.0O7—Na1—O5iv177.96 (14)
O10—Mo1—O6103.56 (15)O8—Na1—O5iv95.40 (13)
O10—Mo1—O12101.66 (15)Ni—O1—Mo1i100.28 (12)
O6—Mo1—O1296.89 (14)Ni—O1—Mo2i100.86 (12)
O10—Mo1—O995.77 (15)Mo1i—O1—Mo2i96.08 (11)
O6—Mo1—O9101.12 (14)Ni—O1—H1122.6
O12—Mo1—O9151.19 (13)Mo1i—O1—H1114.9
O10—Mo1—O2i91.59 (14)Mo2i—O1—H1117.7
O6—Mo1—O2i163.33 (13)Ni—O2—Mo1i100.90 (12)
O12—Mo1—O2i72.89 (12)Ni—O2—Mo3100.86 (12)
O9—Mo1—O2i83.96 (12)Mo1i—O2—Mo394.15 (11)
O10—Mo1—O1i162.28 (14)Ni—O2—H2111.0
O6—Mo1—O1i91.28 (13)Mo1i—O2—H2125.5
O12—Mo1—O1i85.83 (12)Mo3—O2—H2120.3
O9—Mo1—O1i71.55 (11)Ni—O3—Mo3i103.46 (12)
O2i—Mo1—O1i75.14 (11)Ni—O3—Mo2i102.77 (12)
O11—Mo2—O8104.54 (16)Mo3i—O3—Mo2i96.23 (11)
O11—Mo2—O496.16 (14)Ni—O3—H3109.5
O8—Mo2—O4102.06 (15)Mo3i—O3—H3119.0
O11—Mo2—O9100.51 (14)Mo2i—O3—H3123.1
O8—Mo2—O996.64 (15)Mo2—O4—Mo3115.88 (15)
O4—Mo2—O9150.90 (13)Mo3—O5—Na1v135.45 (18)
O11—Mo2—O3i161.51 (14)Mo1—O6—Na1vi135.16 (17)
O8—Mo2—O3i92.01 (14)Mo3—O7—Na1137.64 (18)
O4—Mo2—O3i71.96 (11)Mo2—O8—Na1136.51 (18)
O9—Mo2—O3i85.40 (12)Mo1—O9—Mo2117.83 (15)
O11—Mo2—O1i91.41 (14)Mo1—O10—Na1vii138.20 (19)
O8—Mo2—O1i161.63 (14)Mo2—O11—Na1vi135.40 (18)
O4—Mo2—O1i84.87 (12)Mo1—O12—Mo3i117.82 (15)
O9—Mo2—O1i71.11 (11)H1w—O13w—H2w109.5
O3i—Mo2—O1i73.80 (11)C1—N1—C3109.0 (5)
O7—Mo3—O5105.01 (16)C1—N1—H1n125.5
O7—Mo3—O12i98.91 (15)C3—N1—H1n125.5
O5—Mo3—O12i100.35 (15)C1—N2—C2108.7 (5)
O7—Mo3—O499.72 (15)C1—N2—H2n125.7
O5—Mo3—O496.79 (15)C2—N2—H2n125.7
O12i—Mo3—O4150.40 (13)N1—C1—N2108.4 (5)
O7—Mo3—O3i93.53 (14)N1—C1—H1a125.8
O5—Mo3—O3i159.77 (14)N2—C1—H1a125.8
O12i—Mo3—O3i84.38 (12)C3—C2—N2106.7 (5)
O4—Mo3—O3i71.71 (11)C3—C2—H2a126.7
O7—Mo3—O2163.97 (14)N2—C2—H2a126.7
O5—Mo3—O289.54 (14)C2—C3—N1107.3 (5)
O12i—Mo3—O271.38 (11)C2—C3—H3a126.4
O4—Mo3—O284.88 (12)N1—C3—H3a126.4
O3i—Ni—O1—Mo1i80.20 (12)O9—Mo1—O6—Na1vi31.9 (3)
O3—Ni—O1—Mo1i99.80 (12)O2i—Mo1—O6—Na1vi74.5 (5)
O2i—Ni—O1—Mo1i178.69 (12)O1i—Mo1—O6—Na1vi39.5 (2)
O2—Ni—O1—Mo1i1.31 (12)O5—Mo3—O7—Na1138.6 (3)
O3i—Ni—O1—Mo2i178.50 (11)O12i—Mo3—O7—Na1118.1 (3)
O3—Ni—O1—Mo2i1.50 (11)O4—Mo3—O7—Na138.8 (3)
O2i—Ni—O1—Mo2i83.00 (12)O3i—Mo3—O7—Na133.3 (3)
O2—Ni—O1—Mo2i97.00 (12)O2—Mo3—O7—Na166.8 (6)
O3i—Ni—O2—Mo1i97.12 (13)O10ii—Na1—O7—Mo389.8 (3)
O3—Ni—O2—Mo1i82.88 (13)O6iii—Na1—O7—Mo390.2 (3)
O1i—Ni—O2—Mo1i178.68 (12)O11iii—Na1—O7—Mo3179.9 (3)
O1—Ni—O2—Mo1i1.32 (12)O8—Na1—O7—Mo39.3 (3)
O3i—Ni—O2—Mo30.69 (11)O11—Mo2—O8—Na1131.5 (3)
O3—Ni—O2—Mo3179.31 (11)O4—Mo2—O8—Na131.8 (3)
O1i—Ni—O2—Mo382.26 (12)O9—Mo2—O8—Na1125.8 (3)
O1—Ni—O2—Mo397.74 (12)O3i—Mo2—O8—Na140.2 (3)
O7—Mo3—O2—Ni34.5 (5)O1i—Mo2—O8—Na178.9 (5)
O5—Mo3—O2—Ni169.93 (15)O10ii—Na1—O8—Mo287.1 (3)
O12i—Mo3—O2—Ni88.99 (14)O6iii—Na1—O8—Mo2103.7 (3)
O4—Mo3—O2—Ni73.07 (13)O7—Na1—O8—Mo24.5 (3)
O3i—Mo3—O2—Ni0.65 (11)O5iv—Na1—O8—Mo2173.9 (3)
O7—Mo3—O2—Mo1i67.4 (5)O10—Mo1—O9—Mo2176.37 (18)
O5—Mo3—O2—Mo1i88.13 (14)O6—Mo1—O9—Mo271.29 (19)
O12i—Mo3—O2—Mo1i12.95 (11)O12—Mo1—O9—Mo256.4 (3)
O4—Mo3—O2—Mo1i175.01 (12)O2i—Mo1—O9—Mo292.64 (17)
O3i—Mo3—O2—Mo1i102.59 (12)O1i—Mo1—O9—Mo216.32 (14)
O2i—Ni—O3—Mo3i0.72 (12)O11—Mo2—O9—Mo171.6 (2)
O2—Ni—O3—Mo3i179.28 (12)O8—Mo2—O9—Mo1177.81 (18)
O1i—Ni—O3—Mo3i81.82 (13)O4—Mo2—O9—Mo152.3 (3)
O1—Ni—O3—Mo3i98.18 (13)O3i—Mo2—O9—Mo190.69 (17)
O2i—Ni—O3—Mo2i98.99 (13)O1i—Mo2—O9—Mo116.25 (14)
O2—Ni—O3—Mo2i81.01 (13)O6—Mo1—O10—Na1vii141.2 (3)
O1i—Ni—O3—Mo2i178.47 (11)O12—Mo1—O10—Na1vii41.1 (3)
O1—Ni—O3—Mo2i1.53 (11)O9—Mo1—O10—Na1vii115.9 (3)
O11—Mo2—O4—Mo3176.75 (17)O2i—Mo1—O10—Na1vii31.8 (3)
O8—Mo2—O4—Mo370.41 (19)O1i—Mo1—O10—Na1vii72.7 (6)
O9—Mo2—O4—Mo358.4 (3)O8—Mo2—O11—Na1vi132.8 (3)
O3i—Mo2—O4—Mo317.77 (14)O4—Mo2—O11—Na1vi123.0 (3)
O1i—Mo2—O4—Mo392.38 (16)O9—Mo2—O11—Na1vi33.1 (3)
O7—Mo3—O4—Mo272.72 (19)O3i—Mo2—O11—Na1vi74.2 (5)
O5—Mo3—O4—Mo2179.28 (17)O1i—Mo2—O11—Na1vi38.0 (3)
O12i—Mo3—O4—Mo255.6 (3)O10—Mo1—O12—Mo3i70.7 (2)
O3i—Mo3—O4—Mo217.81 (14)O6—Mo1—O12—Mo3i176.16 (17)
O2—Mo3—O4—Mo291.80 (16)O9—Mo1—O12—Mo3i55.3 (3)
O7—Mo3—O5—Na1v139.4 (2)O2i—Mo1—O12—Mo3i17.33 (15)
O12i—Mo3—O5—Na1v37.1 (3)O1i—Mo1—O12—Mo3i93.05 (17)
O4—Mo3—O5—Na1v118.6 (2)C3—N1—C1—N20.2 (7)
O3i—Mo3—O5—Na1v64.8 (5)C2—N2—C1—N10.5 (7)
O2—Mo3—O5—Na1v33.8 (2)C1—N2—C2—C30.6 (7)
O10—Mo1—O6—Na1vi130.7 (2)N2—C2—C3—N10.5 (7)
O12—Mo1—O6—Na1vi125.5 (2)C1—N1—C3—C20.2 (7)
Symmetry codes: (i) x, y+1, z+1; (ii) x, y1/2, z+3/2; (iii) x+1, y1/2, z+3/2; (iv) x, y+1/2, z+1/2; (v) x, y+1/2, z1/2; (vi) x+1, y+1/2, z+3/2; (vii) x, y+1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O13w0.911.772.659 (5)166
O13w—H2w···O4viii0.862.092.725 (5)130
O13w—H1w···O6ix0.852.142.932 (5)156
O13w—H1w···O10ix0.852.392.938 (5)123
N1—H1n···O9iii0.861.872.712 (5)165
N2—H2n···O6viii0.862.142.965 (6)161
Symmetry codes: (iii) x+1, y1/2, z+3/2; (viii) x+1, y+1, z+1; (ix) x, y+3/2, z1/2.
 

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