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The HfIV atoms in the centrosymmetric title compound, (C4H12N)2][Hf2F10(H2O)2], are bridged by two F atoms. The HfIV atoms show penta­gonal–bipyramidal coordination. The dianions are linked by water–fluorine hydrogen bonds into layers.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805042479/bv6041sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805042479/bv6041Isup2.hkl
Contains datablock I

CCDC reference: 298379

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](N-C) = 0.007 Å
  • R factor = 0.021
  • wR factor = 0.055
  • Data-to-parameter ratio = 18.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.72
Alert level C CRYSR01_ALERT_1_C _exptl_crystal_size_rad not in the CIF when expected. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Hf1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1 PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.850(10) ...... 4.00 su-Rat O1 -H1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat O1 -H2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.850(10) ...... 4.00 su-Rat O1 -H1 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat O1 -H2 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.84(5), Rep 1.84(2) ...... 2.50 su-Rat H1 -F4 1.555 4.566
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 8 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXS97.

Bis(tetramethylammonium) di-µ-fluoro-bis[aquatetrafluorohafnate(IV)] top
Crystal data top
(C4H12N)2][Hf2F10(H2O)2]F(000) = 1360
Mr = 731.30Dx = 2.572 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 754 reflections
a = 9.919 (1) Åθ = 27.0–44.7°
b = 9.687 (1) ŵ = 11.08 mm1
c = 19.656 (2) ÅT = 295 K
V = 1888.6 (4) Å3Sphere, colourless
Z = 40.16 × 0.16 × 0.16 mm
Data collection top
Bruker SMART 1000 area-detector
diffractometer
2168 independent reflections
Radiation source: fine-focus sealed tube1942 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
Detector resolution: 8.33 pixels mm-1θmax = 27.6°, θmin = 2.9°
φ and ω scansh = 1212
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1212
Tmin = 0.141, Tmax = 0.170l = 2025
11359 measured reflections
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)] = 0.021H-atom parameters constrained
wR(F2) = 0.055 w = 1/[σ2(Fo2) + (0.0221P)2 + 3.7908P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
2168 reflectionsΔρmax = 0.91 e Å3
118 parametersΔρmin = 0.81 e Å3
3 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0026 (1)
Special details top

Experimental. The crystal was measured up to a 2θmax of 90°; the cell was refined from 754 reflections in the 27.0 to 44.7° range as the cell would be more accurately determined from higher angle reflections. However, the refinement used only those below the 55° maximum.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Hf10.53921 (2)0.59702 (2)0.42352 (1)0.01665 (8)
F10.5859 (3)0.5589 (3)0.5282 (1)0.0306 (6)
F20.4156 (3)0.5306 (3)0.3519 (1)0.0372 (6)
F30.5968 (3)0.7156 (3)0.3463 (1)0.0333 (6)
F40.4054 (3)0.7374 (3)0.4540 (2)0.0364 (6)
F50.6708 (3)0.4487 (3)0.4010 (2)0.0379 (7)
O10.7045 (3)0.7357 (3)0.4587 (2)0.0356 (8)
N10.0513 (4)0.5903 (4)0.3353 (2)0.0278 (8)
C10.0895 (6)0.6159 (7)0.3122 (3)0.056 (2)
C20.1360 (6)0.7132 (5)0.3213 (3)0.043 (1)
C30.1079 (6)0.4701 (5)0.2976 (3)0.044 (1)
C40.0508 (8)0.5613 (8)0.4094 (3)0.056 (2)
H10.755 (5)0.730 (5)0.494 (2)0.06 (2)*
H20.730 (5)0.803 (3)0.434 (2)0.03 (1)*
H1a0.08960.63590.26430.084*
H1b0.12640.69300.33660.084*
H1c0.14340.53540.32060.084*
H2a0.13530.73240.27340.064*
H2b0.22680.69550.33590.064*
H2c0.10070.79120.34560.064*
H3a0.10790.48970.24970.067*
H3b0.05360.38990.30620.067*
H3c0.19850.45320.31250.067*
H4a0.00400.48160.41830.084*
H4b0.01470.63930.43330.084*
H4c0.14130.54410.42450.084*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Hf10.0165 (1)0.0167 (1)0.0168 (1)0.0003 (1)0.0000 (1)0.0024 (1)
F10.035 (1)0.036 (1)0.021 (1)0.019 (1)0.008 (1)0.007 (1)
F20.045 (2)0.042 (2)0.025 (1)0.014 (1)0.011 (1)0.005 (1)
F30.035 (1)0.040 (1)0.025 (1)0.008 (1)0.000 (1)0.012 (1)
F40.035 (2)0.030 (1)0.044 (2)0.010 (1)0.014 (1)0.003 (1)
F50.041 (2)0.030 (1)0.043 (2)0.018 (1)0.010 (1)0.008 (1)
O10.038 (2)0.039 (2)0.031 (2)0.024 (2)0.010 (1)0.014 (2)
N10.029 (2)0.028 (2)0.026 (2)0.000 (2)0.0013 (1)0.000 (2)
C10.025 (3)0.091 (5)0.053 (3)0.009 (3)0.003 (2)0.002 (3)
C20.050 (3)0.025 (2)0.054 (3)0.004 (2)0.001 (2)0.004 (2)
C30.047 (3)0.033 (3)0.053 (3)0.003 (2)0.000 (2)0.012 (2)
C40.078 (5)0.061 (4)0.028 (3)0.011 (3)0.002 (3)0.000 (3)
Geometric parameters (Å, º) top
Hf1—F12.141 (2)C1—H1a0.96
Hf1—F1i2.173 (2)C1—H1b0.96
Hf1—F21.975 (3)C1—H1c0.96
Hf1—F31.987 (2)C2—H2a0.96
Hf1—F51.991 (2)C2—H2b0.96
Hf1—F41.992 (2)C2—H2c0.96
Hf1—O12.230 (3)C3—H3a0.96
N1—C21.482 (6)C3—H3b0.96
N1—C41.483 (7)C3—H3c0.96
N1—C11.490 (6)C4—H4a0.96
N1—C31.491 (6)C4—H4b0.96
O1—H10.85 (1)C4—H4c0.96
O1—H20.85 (1)
F1—Hf1—F1i65.4 (1)Hf1—O1—H1130 (3)
F1—Hf1—F2139.7 (1)Hf1—O1—H2120 (3)
F1—Hf1—F3140.5 (1)H1—O1—H2109 (2)
F1—Hf1—F488.5 (1)N1—C1—H1a109.5
F1—Hf1—F587.0 (1)N1—C1—H1b109.5
F1—Hf1—O169.3 (1)H1a—C1—H1b109.5
F1i—Hf1—F274.4 (1)N1—C1—H1c109.5
F1i—Hf1—F3154.1 (1)H1a—C1—H1c109.5
F1i—Hf1—F487.8 (1)H1b—C1—H1c109.5
F1i—Hf1—F588.3 (1)N1—C2—H2a109.5
F1i—Hf1—O1134.7 (1)N1—C2—H2b109.5
F2—Hf1—F379.8 (1)H2a—C2—H2b109.5
F2—Hf1—F491.3 (1)N1—C2—H2c109.5
F2—Hf1—F590.7 (1)H2a—C2—H2c109.5
F2—Hf1—O1150.9 (1)H2b—C2—H2c109.5
F3—Hf1—F491.5 (1)N1—C3—H3a109.5
F3—Hf1—F593.4 (1)N1—C3—H3b109.5
F3—Hf1—O171.2 (1)H3a—C3—H3b109.5
F5—Hf1—F4175.0 (1)N1—C3—H3c109.5
F4—Hf1—O189.2 (1)H3a—C3—H3c109.5
F5—Hf1—O191.3 (1)H3b—C3—H3c109.5
Hf1—F1—Hf1i114.6 (1)N1—C4—H4a109.5
C2—N1—C4109.7 (4)N1—C4—H4b109.5
C2—N1—C1110.0 (4)H4a—C4—H4b109.5
C4—N1—C1109.2 (5)N1—C4—H4c109.5
C2—N1—C3108.8 (4)H4a—C4—H4c109.5
C4—N1—C3109.9 (4)H4b—C4—H4c109.5
C1—N1—C3109.3 (4)
F2—Hf1—F1—Hf1i1.9 (3)F4—Hf1—F1—Hf1i88.3 (2)
F3—Hf1—F1—Hf1i178.9 (1)O1—Hf1—F1—Hf1i178.0 (2)
F5—Hf1—F1—Hf1i89.5 (2)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···F4ii0.85 (1)1.84 (2)2.643 (4)156 (5)
O1—H2···F5iii0.85 (1)1.84 (2)2.660 (4)162 (4)
Symmetry codes: (ii) x+1/2, y+3/2, z+1; (iii) x+3/2, y+1/2, z.
 

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