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The crystal structure of dipotassium iron(III) {hydrogen bis[hydrogenphosphate(V)]} difluoride, K2Fe[H(HPO4)2]F2, obtained by hydrothermal synthesis, was determined from single-crystal X-ray diffraction data. The structure is characterized by K+ cations and hydrogen-bonded {[Fe[H(HPO4)2]F2]2-}n chains, which consist of centrosymmetric Fe[F2O4] octahedra linked to their four neighbouring phosphate tetrahedra via common O corners, developing a three-dimensional structure.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (P-O) = 0.002 Å
- R factor = 0.023
- wR factor = 0.064
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.
dipotassium iron(III) {hydrogen bis[hydrogenphosphate(V)]} difluoride
top
Crystal data top
K2Fe[H(HPO4)2]F2 | F(000) = 358 |
Mr = 365.01 | Dx = 2.873 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4590 reflections |
a = 4.7586 (10) Å | θ = 3–28.3° |
b = 8.2530 (17) Å | µ = 3.21 mm−1 |
c = 10.758 (2) Å | T = 295 K |
β = 92.845 (2)° | Prism, pale pink |
V = 421.97 (15) Å3 | 0.33 × 0.26 × 0.08 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1012 independent reflections |
Radiation source: fine-focus sealed tube | 1011 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ω scans | θmax = 28.3°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −6→6 |
Tmin = 0.417, Tmax = 0.783 | k = −10→10 |
4590 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.023 | Only H-atom displacement parameters refined |
wR(F2) = 0.064 | w = 1/[σ2(Fo2) + (0.0241P)2 + 0.5078P] where P = (Fo2 + 2Fc2)/3 |
S = 1.27 | (Δ/σ)max = 0.001 |
1012 reflections | Δρmax = 0.33 e Å−3 |
73 parameters | Δρmin = −0.32 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.035 (3) |
Special details top
Experimental. 2400 images,Δω=0.3°, Exp time: 20 s. |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.5000 | 0.0000 | 0.0000 | 0.01019 (15) | |
P1 | 0.98546 (10) | 0.75976 (6) | 0.91368 (5) | 0.01088 (16) | |
K1 | 0.50465 (11) | 0.10069 (6) | 0.33248 (5) | 0.02184 (16) | |
F1 | 0.3227 (3) | 0.09144 (15) | 0.85181 (11) | 0.0159 (3) | |
O1 | 0.2445 (3) | 0.80846 (18) | 0.98918 (14) | 0.0145 (3) | |
O2 | 0.7682 (3) | 0.88937 (18) | 0.89246 (14) | 0.0143 (3) | |
O3 | 0.8489 (3) | 0.61110 (18) | 0.96974 (16) | 0.0179 (3) | |
O4 | 0.0946 (3) | 0.7080 (2) | 0.78368 (15) | 0.0203 (3) | |
H1 | −0.0280 | 0.6572 | 0.7383 | 0.023 (7)* | |
H2 | 0.9460 | 0.5261 | 0.9938 | 0.023 (16)* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0107 (2) | 0.0103 (2) | 0.0094 (2) | 0.00032 (13) | −0.00137 (14) | 0.00040 (13) |
P1 | 0.0109 (3) | 0.0099 (3) | 0.0118 (3) | −0.00015 (17) | −0.00008 (19) | −0.00124 (17) |
K1 | 0.0254 (3) | 0.0234 (3) | 0.0165 (3) | 0.00490 (18) | −0.00089 (19) | −0.00102 (18) |
F1 | 0.0169 (6) | 0.0178 (6) | 0.0127 (6) | 0.0022 (5) | −0.0032 (5) | 0.0034 (5) |
O1 | 0.0138 (7) | 0.0131 (7) | 0.0161 (7) | −0.0017 (5) | −0.0034 (5) | 0.0000 (5) |
O2 | 0.0149 (7) | 0.0147 (7) | 0.0133 (7) | 0.0034 (5) | 0.0000 (6) | 0.0008 (5) |
O3 | 0.0152 (7) | 0.0120 (7) | 0.0265 (8) | −0.0019 (5) | 0.0010 (6) | 0.0041 (6) |
O4 | 0.0168 (7) | 0.0280 (9) | 0.0162 (8) | −0.0020 (6) | 0.0028 (6) | −0.0098 (7) |
Geometric parameters (Å, º) top
Fe1—F1i | 1.9208 (12) | K1—O3xii | 2.7785 (18) |
Fe1—F1ii | 1.9208 (12) | K1—O1xii | 2.7963 (16) |
Fe1—O2iii | 1.9867 (15) | K1—O4iii | 2.8156 (18) |
Fe1—O2iv | 1.9867 (15) | K1—O4vi | 3.2362 (19) |
Fe1—O1iii | 1.9942 (15) | K1—P1iii | 3.6284 (8) |
Fe1—O1iv | 1.9942 (15) | K1—Fe1xiii | 3.7567 (8) |
Fe1—K1 | 3.6710 (9) | K1—P1xiv | 3.7961 (9) |
Fe1—K1v | 3.6710 (9) | F1—Fe1xv | 1.9208 (12) |
Fe1—K1vi | 3.7567 (8) | F1—K1x | 2.6957 (15) |
Fe1—K1vii | 3.7567 (8) | F1—K1i | 2.6984 (14) |
P1—O1viii | 1.4970 (15) | O1—P1xvi | 1.4970 (15) |
P1—O2 | 1.4974 (15) | O1—Fe1xvii | 1.9942 (15) |
P1—O3 | 1.5265 (16) | O1—K1xviii | 2.7963 (16) |
P1—O4viii | 1.5748 (16) | O2—Fe1xvii | 1.9867 (15) |
P1—K1iii | 3.6284 (9) | O2—K1iii | 2.6900 (16) |
P1—K1ix | 3.7961 (9) | O3—K1x | 2.7711 (17) |
P1—K1x | 3.8274 (9) | O3—K1xviii | 2.7785 (18) |
P1—K1xi | 3.8554 (9) | O3—H2 | 0.8722 |
K1—O2iii | 2.6900 (16) | O4—P1xvi | 1.5748 (16) |
K1—F1vi | 2.6957 (15) | O4—K1iii | 2.8156 (18) |
K1—F1i | 2.6984 (14) | O4—K1x | 3.2362 (19) |
K1—O3vi | 2.7711 (17) | O4—H1 | 0.8521 |
| | | |
F1i—Fe1—F1ii | 180.00 (8) | O3vi—K1—O3xii | 88.61 (5) |
F1i—Fe1—O2iii | 88.03 (6) | O2iii—K1—O1xii | 140.27 (5) |
F1ii—Fe1—O2iii | 91.97 (6) | F1vi—K1—O1xii | 59.79 (4) |
F1i—Fe1—O2iv | 91.97 (6) | F1i—K1—O1xii | 136.82 (5) |
F1ii—Fe1—O2iv | 88.03 (6) | O3vi—K1—O1xii | 78.48 (5) |
O2iii—Fe1—O2iv | 180.00 (9) | O3xii—K1—O1xii | 73.13 (5) |
F1i—Fe1—O1iii | 91.23 (6) | O2iii—K1—O4iii | 83.74 (5) |
F1ii—Fe1—O1iii | 88.77 (6) | F1vi—K1—O4iii | 74.51 (5) |
O2iii—Fe1—O1iii | 90.52 (6) | F1i—K1—O4iii | 76.45 (5) |
O2iv—Fe1—O1iii | 89.48 (6) | O3vi—K1—O4iii | 101.23 (5) |
F1i—Fe1—O1iv | 88.77 (6) | O3xii—K1—O4iii | 140.51 (5) |
F1ii—Fe1—O1iv | 91.23 (6) | O1xii—K1—O4iii | 71.65 (5) |
O2iii—Fe1—O1iv | 89.48 (6) | O2iii—K1—O4vi | 67.53 (4) |
O2iv—Fe1—O1iv | 90.52 (6) | F1vi—K1—O4vi | 124.13 (4) |
O1iii—Fe1—O1iv | 180.00 (10) | F1i—K1—O4vi | 67.75 (4) |
F1i—Fe1—K1 | 45.50 (4) | O3vi—K1—O4vi | 85.73 (5) |
F1ii—Fe1—K1 | 134.50 (4) | O3xii—K1—O4vi | 76.43 (5) |
O2iii—Fe1—K1 | 45.70 (4) | O1xii—K1—O4vi | 145.85 (5) |
O2iv—Fe1—K1 | 134.30 (4) | O4iii—K1—O4vi | 141.79 (3) |
O1iii—Fe1—K1 | 77.85 (4) | O2iii—K1—P1iii | 21.53 (3) |
O1iv—Fe1—K1 | 102.15 (4) | F1vi—K1—P1iii | 63.88 (3) |
F1i—Fe1—K1v | 134.50 (4) | F1i—K1—P1iii | 81.86 (3) |
F1ii—Fe1—K1v | 45.50 (4) | O3vi—K1—P1iii | 158.54 (4) |
O2iii—Fe1—K1v | 134.30 (4) | O3xii—K1—P1iii | 99.06 (4) |
O2iv—Fe1—K1v | 45.70 (4) | O1xii—K1—P1iii | 122.90 (4) |
O1iii—Fe1—K1v | 102.15 (4) | O4iii—K1—P1iii | 85.59 (4) |
O1iv—Fe1—K1v | 77.85 (4) | O4vi—K1—P1iii | 76.76 (3) |
K1—Fe1—K1v | 180.0 | O2iii—K1—Fe1 | 31.91 (3) |
F1i—Fe1—K1vi | 136.89 (4) | F1vi—K1—Fe1 | 107.58 (3) |
F1ii—Fe1—K1vi | 43.11 (4) | F1i—K1—Fe1 | 30.51 (3) |
O2iii—Fe1—K1vi | 84.00 (5) | O3vi—K1—Fe1 | 110.56 (4) |
O2iv—Fe1—K1vi | 96.00 (5) | O3xii—K1—Fe1 | 141.12 (4) |
O1iii—Fe1—K1vi | 46.73 (4) | O1xii—K1—Fe1 | 142.10 (4) |
O1iv—Fe1—K1vi | 133.27 (4) | O4iii—K1—Fe1 | 70.49 (3) |
K1—Fe1—K1vi | 105.601 (12) | O4vi—K1—Fe1 | 71.90 (3) |
K1v—Fe1—K1vi | 74.399 (12) | P1iii—K1—Fe1 | 52.280 (14) |
F1i—Fe1—K1vii | 43.11 (4) | O2iii—K1—Fe1xiii | 113.00 (4) |
F1ii—Fe1—K1vii | 136.89 (4) | F1vi—K1—Fe1xiii | 29.14 (3) |
O2iii—Fe1—K1vii | 96.00 (5) | F1i—K1—Fe1xiii | 151.31 (3) |
O2iv—Fe1—K1vii | 84.00 (5) | O3vi—K1—Fe1xiii | 108.37 (4) |
O1iii—Fe1—K1vii | 133.27 (4) | O3xii—K1—Fe1xiii | 65.63 (3) |
O1iv—Fe1—K1vii | 46.73 (4) | O1xii—K1—Fe1xiii | 31.28 (3) |
K1—Fe1—K1vii | 74.399 (12) | O4iii—K1—Fe1xiii | 75.01 (4) |
K1v—Fe1—K1vii | 105.601 (12) | O4vi—K1—Fe1xiii | 138.64 (3) |
K1vi—Fe1—K1vii | 180.000 (8) | P1iii—K1—Fe1xiii | 93.026 (17) |
O1viii—P1—O2 | 115.76 (9) | Fe1—K1—Fe1xiii | 131.766 (15) |
O1viii—P1—O3 | 110.90 (9) | O2iii—K1—P1xiv | 154.07 (4) |
O2—P1—O3 | 109.27 (9) | F1vi—K1—P1xiv | 79.33 (3) |
O1viii—P1—O4viii | 104.82 (9) | F1i—K1—P1xiv | 121.65 (3) |
O2—P1—O4viii | 108.30 (9) | O3vi—K1—P1xiv | 59.67 (4) |
O3—P1—O4viii | 107.37 (10) | O3xii—K1—P1xiv | 80.10 (4) |
O1viii—P1—K1iii | 142.45 (7) | O1xii—K1—P1xiv | 19.69 (3) |
O3—P1—K1iii | 105.82 (7) | O4iii—K1—P1xiv | 72.69 (4) |
O4viii—P1—K1iii | 70.50 (7) | O4vi—K1—P1xiv | 138.39 (3) |
O2—P1—K1ix | 140.23 (6) | P1iii—K1—P1xiv | 141.260 (18) |
O3—P1—K1ix | 72.98 (7) | Fe1—K1—P1xiv | 138.757 (18) |
O4viii—P1—K1ix | 108.54 (7) | Fe1xiii—K1—P1xiv | 50.972 (12) |
K1iii—P1—K1ix | 178.257 (16) | Fe1xv—F1—K1x | 107.74 (5) |
O1viii—P1—K1x | 143.06 (7) | Fe1xv—F1—K1i | 103.99 (5) |
O2—P1—K1x | 96.89 (6) | K1x—F1—K1i | 112.74 (5) |
O4viii—P1—K1x | 78.83 (7) | P1xvi—O1—Fe1xvii | 136.70 (10) |
K1iii—P1—K1x | 74.027 (15) | P1xvi—O1—K1xviii | 121.30 (8) |
K1ix—P1—K1x | 104.413 (19) | Fe1xvii—O1—K1xviii | 101.99 (6) |
O1viii—P1—K1xi | 76.30 (6) | P1—O2—Fe1xvii | 134.28 (10) |
O2—P1—K1xi | 97.77 (6) | P1—O2—K1iii | 117.24 (8) |
O3—P1—K1xi | 143.73 (7) | Fe1xvii—O2—K1iii | 102.39 (6) |
K1iii—P1—K1xi | 78.90 (2) | P1—O3—K1x | 123.26 (9) |
K1ix—P1—K1xi | 101.29 (2) | P1—O3—K1xviii | 127.82 (9) |
K1x—P1—K1xi | 117.703 (18) | K1x—O3—K1xviii | 91.39 (5) |
O2iii—K1—F1vi | 84.15 (4) | P1—O3—H2 | 122.27 (14) |
O2iii—K1—F1i | 60.53 (4) | K1x—O3—H2 | 86.63 (11) |
F1vi—K1—F1i | 136.16 (3) | K1xviii—O3—H2 | 94.58 (12) |
O2iii—K1—O3vi | 138.14 (5) | P1xvi—O4—K1iii | 120.17 (9) |
F1vi—K1—O3vi | 137.48 (4) | P1xvi—O4—K1x | 106.99 (8) |
F1i—K1—O3vi | 80.06 (5) | K1iii—O4—K1x | 95.58 (5) |
O2iii—K1—O3xii | 113.85 (5) | P1xvi—O4—H1 | 113.31 (14) |
F1vi—K1—O3xii | 72.71 (4) | K1iii—O4—H1 | 118.76 (13) |
F1i—K1—O3xii | 143.02 (5) | K1x—O4—H1 | 95.49 (13) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x, y, z−1; (iii) −x+1, −y+1, −z+1; (iv) x, y−1, z−1; (v) −x+1, −y, −z; (vi) x, −y+1/2, z−1/2; (vii) −x+1, y−1/2, −z+1/2; (viii) x+1, y, z; (ix) −x+2, y+1/2, −z+3/2; (x) x, −y+1/2, z+1/2; (xi) −x+2, −y+1, −z+1; (xii) −x+1, y−1/2, −z+3/2; (xiii) −x+1, y+1/2, −z+1/2; (xiv) −x+2, y−1/2, −z+3/2; (xv) x, y, z+1; (xvi) x−1, y, z; (xvii) x, y+1, z+1; (xviii) −x+1, y+1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H1···F1xix | 0.852 | 1.751 | 2.589 (2) | 168 |
O3—H2···O3xx | 0.872 | 1.533 | 2.400 (2) | 172 |
Symmetry codes: (xix) −x, y+1/2, −z+3/2; (xx) −x+2, −y+1, −z+2. |
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