Literature DB >> 21522514

Dipotassium hexa-aqua-nickel(II) bis-[hexa-fluoridozirconate(IV)].

Abdelghani Oudahmane1, Noura Mnaouer, Malika El-Ghozzi, Daniel Avignant.   

Abstract

Single crystals of the title compound, K(2)[Ni(H(2)O)(6)][ZrF(6)](2), were grown by slow evaporation of a 40% aqueous HF solution in which a stoichiometric mixture of NiCl(2)·6H(2)O, ZrF(4) and KCl was dissolved. The monoclinic structure is isotypic with its K(2)Cu, K(2)Zn, Cs(2)Zn and Cs(2)Cu analogues. The structure is built up from isolated, slightly elongated octa-hedral [Ni(H(2)O)(6)](2+) complex cations (symmetry ) and dimeric [Zr(2)F(12)](4-) complex anions (symmetry ) that are also isolated from each other. The [Zr(2)F(12)](4-) anion results from the association of two distorted penta-gonal-bipyramidal [ZrF(7)] coordination polyhedra by sharing an equatorial edge passing through an inversion center of the unit cell. Both isolated [Ni(H(2)O)(6)](2+) and [Zr(2)F(12)](4-) complex ions are situated in planes parallel to (010). They are connected by the eight-coordinated K(+) ions into a three-dimensional structure. An intricate O-H⋯F hydrogen-bonding network consolidates the structure.

Entities:  

Year:  2010        PMID： 21522514      PMCID： PMC3050341          DOI： 10.1107/S160053681005350X

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For isotypic structures, see: Fischer & Weiss (1973 ▶); Bukvetskii et al. (1993 ▶); Hitchman et al. (2002 ▶). For a review on the stereochemistry of zirconium and hafnium fluorido complexes, see: Davidovich (1998 ▶). For background to distortion indices, see: Momma & Izumi (2008 ▶).

Experimental

Crystal data

K2[Ni(H2O)6][ZrF6]2 M = 655.45 Monoclinic, a = 6.6090 (1) Å b = 10.0398 (1) Å c = 11.7843 (1) Å β = 95.897 (1)° V = 777.79 (2) Å3 Z = 2 Mo Kα radiation μ = 3.20 mm−1 T = 296 K 0.28 × 0.14 × 0.09 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.613, T max = 0.748 17267 measured reflections 4436 independent reflections 3858 reflections with I > 2σ(I) R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.023 wR(F 2) = 0.052 S = 1.06 4436 reflections 131 parameters All H-atom parameters refined Δρmax = 0.63 e Å−3 Δρmin = −0.57 e Å−3 Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶) and ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681005350X/wm2439sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053681005350X/wm2439Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
K2[Ni(H2O)6][ZrF6]2F(000) = 628
Mr = 655.45Dx = 2.799 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7940 reflections
a = 6.6090 (1) Åθ = 3.7–38.7°
b = 10.0398 (1) ŵ = 3.20 mm−1
c = 11.7843 (1) ÅT = 296 K
β = 95.897 (1)°Block, green
V = 777.79 (2) Å30.28 × 0.14 × 0.09 mm
Z = 2
Bruker APEXII CCD diffractometer4436 independent reflections
Radiation source: fine-focus sealed tube3858 reflections with I > 2σ(I)
graphiteRint = 0.028
Detector resolution: 8.3333 pixels mm-1θmax = 38.8°, θmin = 4.2°
ω and φ scansh = −11→11
Absorption correction: multi-scan (SADABS; Bruker, 2008)k = −17→12
Tmin = 0.613, Tmax = 0.748l = −18→20
17267 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023All H-atom parameters refined
wR(F2) = 0.052w = 1/[σ2(Fo2) + (0.0182P)2 + 0.3179P] where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.032
4436 reflectionsΔρmax = 0.63 e Å−3
131 parametersΔρmin = −0.57 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 constraintsExtinction coefficient: 0.0068 (4)
Primary atom site location: structure-invariant direct methods
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.
xyzUiso*/Ueq
Zr−0.462200 (17)0.984514 (11)0.350424 (9)0.01376 (3)
Ni0.00000.00000.00000.01508 (4)
K0.47534 (5)0.71630 (3)0.08423 (3)0.02839 (7)
O10.21314 (15)−0.11683 (10)−0.06747 (9)0.02154 (17)
O2−0.23852 (15)−0.12500 (10)−0.05901 (9)0.02039 (17)
O3−0.04437 (19)−0.88871 (12)−0.14701 (9)0.0293 (2)
F10.53736 (16)0.11314 (9)0.49592 (7)0.0300 (2)
F2−0.53154 (14)0.78950 (8)0.31006 (7)0.02440 (16)
F3−0.17901 (13)0.93040 (11)0.39692 (9)0.0346 (2)
F4−0.46635 (13)0.97177 (8)0.17481 (7)0.02228 (15)
F5−0.35001 (14)0.16232 (8)0.30407 (8)0.02609 (17)
F6−0.75507 (12)0.03609 (11)0.31945 (8)0.02759 (18)
H110.159 (4)−0.169 (3)−0.111 (2)0.044 (6)*
H120.289 (4)−0.072 (3)−0.103 (2)0.044 (6)*
H21−0.196 (3)−0.178 (2)−0.099 (2)0.041 (6)*
H22−0.327 (3)−0.084 (2)−0.0981 (19)0.038 (6)*
H310.028 (4)−0.829 (3)−0.163 (2)0.046 (7)*
H32−0.086 (4)−0.925 (3)−0.205 (2)0.048 (7)*
U11U22U33U12U13U23
Zr0.01662 (5)0.01302 (5)0.01144 (5)−0.00068 (3)0.00044 (3)0.00045 (3)
Ni0.01666 (9)0.01442 (9)0.01395 (9)−0.00119 (6)0.00064 (7)−0.00028 (6)
K0.03371 (15)0.02741 (14)0.02299 (14)−0.00580 (11)−0.00224 (11)0.00113 (10)
O10.0229 (4)0.0194 (4)0.0230 (5)−0.0021 (3)0.0058 (4)−0.0031 (3)
O20.0207 (4)0.0186 (4)0.0213 (4)−0.0003 (3)−0.0007 (3)−0.0024 (3)
O30.0407 (6)0.0279 (5)0.0175 (5)−0.0127 (4)−0.0053 (4)0.0056 (4)
F10.0579 (6)0.0175 (4)0.0158 (4)−0.0105 (4)0.0091 (4)−0.0021 (3)
F20.0394 (5)0.0162 (3)0.0173 (4)−0.0029 (3)0.0014 (3)−0.0013 (3)
F30.0216 (4)0.0442 (6)0.0365 (5)0.0060 (4)−0.0048 (3)0.0052 (4)
F40.0280 (4)0.0239 (4)0.0152 (3)−0.0041 (3)0.0037 (3)−0.0007 (3)
F50.0367 (4)0.0181 (4)0.0247 (4)−0.0067 (3)0.0091 (3)0.0002 (3)
F60.0193 (4)0.0350 (5)0.0280 (5)0.0055 (3)0.0004 (3)−0.0062 (3)
Zr—F31.9717 (9)K—F3xi3.1685 (12)
Zr—F6i2.0006 (8)O1—Kxii2.8929 (11)
Zr—F5i2.0293 (8)O1—H110.79 (3)
Zr—F22.0554 (8)O1—H120.82 (3)
Zr—F42.0708 (8)O2—Kxiii3.1015 (11)
Zr—F1ii2.1467 (8)O2—H210.78 (2)
Zr—F1iii2.1614 (8)O2—H220.82 (2)
Ni—O1iv2.0548 (10)O3—Nixii2.0570 (11)
Ni—O12.0548 (10)O3—H310.80 (3)
Ni—O3v2.0570 (11)O3—H320.80 (3)
Ni—O3i2.0570 (11)F1—Zrxiv2.1467 (8)
Ni—O2iv2.0781 (9)F1—Zriii2.1614 (8)
Ni—O22.0781 (9)F2—Kxv2.7658 (9)
K—F6vi2.6497 (9)F3—Kxvi2.7603 (10)
K—F5vii2.7365 (10)F3—Kvii3.1685 (12)
K—F3viii2.7603 (10)F4—Kxv2.7896 (9)
K—F2ix2.7658 (9)F5—Zrxii2.0293 (8)
K—F4ix2.7896 (9)F5—Kxi2.7365 (10)
K—O1i2.8929 (11)F6—Zrxii2.0006 (8)
K—O2x3.1015 (11)F6—Kxvii2.6497 (9)
F3—Zr—F6i174.24 (4)F5vii—K—F2ix72.14 (3)
F3—Zr—F5i87.40 (4)F3viii—K—F2ix150.45 (3)
F6i—Zr—F5i95.54 (4)F6vi—K—F4ix121.62 (3)
F3—Zr—F289.11 (4)F5vii—K—F4ix85.15 (3)
F6i—Zr—F290.90 (4)F3viii—K—F4ix145.26 (3)
F5i—Zr—F2148.71 (3)F2ix—K—F4ix53.33 (2)
F3—Zr—F4100.10 (4)F6vi—K—O1i109.85 (3)
F6i—Zr—F485.44 (4)F5vii—K—O1i150.10 (3)
F5i—Zr—F475.70 (3)F3viii—K—O1i70.50 (3)
F2—Zr—F474.34 (3)F2ix—K—O1i111.88 (3)
F3—Zr—F1ii91.31 (4)F4ix—K—O1i75.79 (3)
F6i—Zr—F1ii84.80 (4)F6vi—K—O2x167.54 (3)
F5i—Zr—F1ii73.52 (3)F5vii—K—O2x77.96 (3)
F2—Zr—F1ii137.67 (3)F3viii—K—O2x92.00 (3)
F4—Zr—F1ii146.55 (3)F2ix—K—O2x117.28 (3)
F3—Zr—F1iii86.30 (4)F4ix—K—O2x70.61 (3)
F6i—Zr—F1iii88.22 (4)O1i—K—O2x74.11 (3)
F5i—Zr—F1iii138.27 (3)F6vi—K—F3xi66.39 (3)
F2—Zr—F1iii72.35 (3)F5vii—K—F3xi55.25 (2)
F4—Zr—F1iii145.96 (3)F3viii—K—F3xi72.07 (3)
F1ii—Zr—F1iii65.45 (4)F2ix—K—F3xi102.83 (3)
F3—Zr—Zrxviii88.57 (3)F4ix—K—F3xi139.92 (3)
F6i—Zr—Zrxviii85.86 (3)O1i—K—F3xi142.29 (3)
F5i—Zr—Zrxviii106.09 (3)O2x—K—F3xi103.01 (3)
F2—Zr—Zrxviii104.90 (2)F6vi—K—Zrxi89.24 (2)
F4—Zr—Zrxviii171.25 (2)F5vii—K—Zrxi28.097 (18)
F1ii—Zr—Zrxviii32.85 (2)F3viii—K—Zrxi93.88 (2)
F1iii—Zr—Zrxviii32.60 (2)F2ix—K—Zrxi93.56 (2)
F3—Zr—Kvii51.84 (3)F4ix—K—Zrxi112.72 (2)
F6i—Zr—Kvii129.16 (3)O1i—K—Zrxi151.51 (2)
F5i—Zr—Kvii39.43 (3)O2x—K—Zrxi83.09 (2)
F2—Zr—Kvii139.29 (3)F3xi—K—Zrxi29.294 (16)
F4—Zr—Kvii99.03 (2)F6vi—K—Zrix97.85 (2)
F1ii—Zr—Kvii63.98 (3)F5vii—K—Zrix75.428 (19)
F1iii—Zr—Kvii110.72 (3)F3viii—K—Zrix163.11 (2)
Zrxviii—Zr—Kvii87.200 (6)F2ix—K—Zrix26.431 (17)
F3—Zr—Kxv92.84 (3)F4ix—K—Zrix27.023 (17)
F6i—Zr—Kxv90.62 (3)O1i—K—Zrix95.67 (2)
F5i—Zr—Kxv112.37 (3)O2x—K—Zrix93.42 (2)
F2—Zr—Kxv36.80 (2)F3xi—K—Zrix121.99 (2)
F4—Zr—Kxv37.74 (2)Zrxi—K—Zrix102.640 (7)
F1ii—Zr—Kxv172.94 (3)F6vi—K—Zrxvii20.660 (19)
F1iii—Zr—Kxv109.12 (2)F5vii—K—Zrxvii120.27 (2)
Zrxviii—Zr—Kxv141.547 (7)F3viii—K—Zrxvii67.44 (2)
Kvii—Zr—Kxv123.004 (4)F2ix—K—Zrxvii83.04 (2)
F3—Zr—Kvi148.57 (3)F4ix—K—Zrxvii121.05 (2)
F6i—Zr—Kvi27.86 (3)O1i—K—Zrxvii89.46 (2)
F5i—Zr—Kvi83.54 (3)O2x—K—Zrxvii157.34 (2)
F2—Zr—Kvi113.62 (3)F3xi—K—Zrxvii80.348 (18)
F4—Zr—Kvi106.63 (3)Zrxi—K—Zrxvii106.804 (8)
F1ii—Zr—Kvi57.25 (3)Zrix—K—Zrxvii103.843 (7)
F1iii—Zr—Kvi80.80 (3)F6vi—K—Zrviii65.81 (2)
Zrxviii—Zr—Kvi65.435 (5)F5vii—K—Zrviii137.16 (2)
Kvii—Zr—Kvi106.804 (8)F3viii—K—Zrviii20.89 (2)
Kxv—Zr—Kvi118.448 (4)F2ix—K—Zrviii131.81 (2)
F3—Zr—Kxvi29.95 (3)F4ix—K—Zrviii137.38 (2)
F6i—Zr—Kxvi144.59 (3)O1i—K—Zrviii63.49 (2)
F5i—Zr—Kxvi110.23 (3)O2x—K—Zrviii107.49 (2)
F2—Zr—Kxvi79.65 (3)F3xi—K—Zrviii82.684 (18)
F4—Zr—Kxvi123.50 (3)Zrxi—K—Zrviii109.132 (8)
F1ii—Zr—Kxvi79.97 (3)Zrix—K—Zrviii143.549 (10)
F1iii—Zr—Kxvi56.37 (3)Zrxvii—K—Zrviii50.252 (5)
Zrxviii—Zr—Kxvi64.313 (5)Ni—O1—Kxii118.84 (4)
Kvii—Zr—Kxvi70.868 (8)Ni—O1—H11110.3 (17)
Kxv—Zr—Kxvi100.955 (4)Kxii—O1—H11102.4 (18)
Kvi—Zr—Kxvi129.748 (5)Ni—O1—H12111.2 (17)
O1iv—Ni—O1180.00 (7)Kxii—O1—H12106.2 (17)
O1iv—Ni—O3v91.62 (5)H11—O1—H12107 (2)
O1—Ni—O3v88.38 (5)Ni—O2—Kxiii127.74 (4)
O1iv—Ni—O3i88.38 (5)Ni—O2—H21107.6 (17)
O1—Ni—O3i91.62 (5)Kxiii—O2—H21105.2 (17)
O3v—Ni—O3i180.0Ni—O2—H22111.1 (16)
O1iv—Ni—O2iv93.00 (4)Kxiii—O2—H2297.1 (15)
O1—Ni—O2iv87.00 (4)H21—O2—H22106 (2)
O3v—Ni—O2iv90.50 (4)Nixii—O3—H31124.4 (17)
O3i—Ni—O2iv89.50 (4)Nixii—O3—H32118.5 (19)
O1iv—Ni—O287.00 (4)H31—O3—H32108 (2)
O1—Ni—O293.00 (4)Zrxiv—F1—Zriii114.55 (4)
O3v—Ni—O289.50 (4)Zr—F2—Kxv116.77 (3)
O3i—Ni—O290.50 (4)Zr—F3—Kxvi129.16 (5)
O2iv—Ni—O2180.00 (5)Zr—F3—Kvii98.87 (4)
F6vi—K—F5vii99.70 (3)Kxvi—F3—Kvii107.93 (3)
F6vi—K—F3viii78.70 (3)Zr—F4—Kxv115.24 (3)
F5vii—K—F3viii121.39 (3)Zrxii—F5—Kxi112.48 (4)
F6vi—K—F2ix72.85 (3)Zrxii—F6—Kxvii131.48 (4)
D—H···AD—HH···AD···AD—H···A
O1—H11···F1xi0.79 (3)2.94 (2)3.3300 (14)112.8 (19)
O1—H11···F2xix0.79 (3)1.92 (3)2.6877 (14)164 (2)
O1—H12···F4xx0.82 (3)1.82 (3)2.6375 (13)177 (2)
O1—H12···F5iv0.82 (3)2.61 (2)3.0526 (13)116 (2)
O2—H21···F1xi0.78 (2)2.59 (2)3.0048 (13)115 (2)
O2—H21···F2xix0.78 (2)1.95 (2)2.7227 (13)167 (2)
O2—H22···F4xxi0.82 (2)1.92 (2)2.7362 (13)173 (2)
O2—H22···F6xxii0.82 (2)2.76 (2)3.1924 (14)114.9 (17)
O3—H31···F1xxiii0.80 (3)2.86 (3)3.2552 (16)113.3 (19)
O3—H31···F5xxiv0.80 (3)1.92 (3)2.7019 (14)168 (2)
O3—H32···F3iv0.80 (3)3.00 (2)3.4527 (16)119 (2)
O3—H32···F6xxv0.80 (3)1.97 (3)2.7427 (15)163 (2)
K2[Ni(H2O)6][ZrF6]2aK2[Cu(H2O)6][ZrF6]2bK2[Zn(H2O)6][ZrF6]2cCs2[Zn(H2O)6][ZrF6]2d
Space groupP21/nP21/cP21/cP21/n
a6.6090 (1)6.631 (6)6.631 (1)6.970 (1)
b10.0398 (1)9.981 (10)10.071 (1)10.515 (2)
c11.7843 (1)12.921 (12)12.952 (1)11.803 (2)
β95.897 (1)114.20 (15)114.96 (2)93.56 (3)
V777.786 (16)780.01 (1)784.16 (2)863.4 (3)
Ni—O1 = 2.0548 (10) (2×)Cu—O1 = 1.966 (4) (2×)Zn—O1 = 2.0856 (2) (2×)Zn—O3 = 2.096 (6) (2×)
Distances MII—ONi—O3 = 2.0570 (11) (2×)Cu—O2 = 2.025 (6) (2×)Zn—O2 = 2.0940 (1) (2×)Zn—O1 = 2.099 (5) (2×)
Ni—O2 = 2.0781 (9) (2×)Cu—O3 = 2.327 (5) (2×)Zn—O3 = 2.1185 (2) (2×)Zn—O2 = 2.105 (5) (2×)
Average MII—O bond length2.0632.1062.0992.100
Polyhedral volume11.68412.33512.31812.341
Distortion index (bond length)0.004830.060890.006070.00156
Quadratic elongation1.00131.01241.00111.0006
Zr—F6 = 1.9718 (9)Zr—F3 = 1.968 (5)Zr—F3 = 1.9727 (3)Zr—F3 = 1.962 (5)
Zr—F5 = 2.0006 (8)Zr—F1 = 2.004 (5)Zr—F1 = 2.0018 (3)Zr—F6 = 1.977 (5)
Zr—F3 = 2.0293 (9)Zr—F5 = 2.029 (4)Zr—F5 = 2.0277 (3)Zr—F5 = 2.037 (5)
Distances Zr—F (Å)Zr—F2 = 2.0554 (8)Zr—F6 = 2.059 (4)Zr—F6 = 2.0570 (3)Zr—F4 = 2.067 (4)
Zr—F1 = 2.0708 (8)Zr—F2 = 2.063 (4)Zr—F2 = 2.0668 (4)Zr—F2 = 2.069 (4)
Zr—F4 = 2.1468 (9)Zr—F4 = 2.156 (5)Zr—F4 = 2.1501 (4)Zr—F1 = 2.156 (4)
Zr—F4 = 2.1614 (8)Zr—F4 = 2.160 (4)Zr—F4 = 2.1628 (4)Zr—F1 = 2.180 (4)
Average Zr—F bond length2.0622.0632.0632.064
Polyhedral volume13.66913.67413.67513.692
Distortion index (bond length)0.026620.026500.026540.02985
K—F5 = 2.6496 (10)K—F1 = 2.668 (5)K—F1 = 2.6506 (3)Cs—F6 = 2.911 (5)
K—F3 = 2.7366 (9)K—F6 = 2.750 (6)K—F2 = 2.7395 (4)Cs—F4 = 3.046 (4)
K—F6 = 2.7603 (11)K—F3 = 2.756 (5)K—F5 = 2.7633 (2)Cs—F2 = 3.057 (4)
Distances K—F/OK—F2 = 2.7658 (9)K—F5 = 2.767 (5)K—F6 = 2.7739 (2)Cs—F3 = 3.065 (5)
K—F1 = 2.7895 (9)K—F2 = 2.799 (5)K—F3 = 2.8094 (2)Cs—F3 = 3.102 (5)
K—O2 = 2.8927 (10)K—O3 = 2.942 (5)K—O1 = 2.8968 (3)Cs—O2 = 3.218 (5)
K—O1 = 3.1012 (10)K—O1 = 2.980 (5)K—O2 = 3.0873 (5)Cs—O1 = 3.236 (5)
K—F6 = 3.1684 (12)K—F3 = 3.1307 (7)K—F3 = 3.1707 (7)Cs—F5 = 3.228 (6)
Average MI—F/O bond length2.8582.8492.8613.118
Polyhedral volume38.45838.15838.56948.130
Distortion index (bond length)0.051460.044290.049840.02627
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H11⋯F1i0.79 (3)2.94 (2)3.3300 (14)112.8 (19)
O1—H11⋯F2ii0.79 (3)1.92 (3)2.6877 (14)164 (2)
O1—H12⋯F4iii0.82 (3)1.82 (3)2.6375 (13)177 (2)
O1—H12⋯F5iv0.82 (3)2.61 (2)3.0526 (13)116 (2)
O2—H21⋯F1i0.78 (2)2.59 (2)3.0048 (13)115 (2)
O2—H21⋯F2ii0.78 (2)1.95 (2)2.7227 (13)167 (2)
O2—H22⋯F4v0.82 (2)1.92 (2)2.7362 (13)173 (2)
O2—H22⋯F6vi0.82 (2)2.76 (2)3.1924 (14)114.9 (17)
O3—H31⋯F1vii0.80 (3)2.86 (3)3.2552 (16)113.3 (19)
O3—H31⋯F5viii0.80 (3)1.92 (3)2.7019 (14)168 (2)
O3—H32⋯F3iv0.80 (3)3.00 (2)3.4527 (16)119 (2)
O3—H32⋯F6ix0.80 (3)1.97 (3)2.7427 (15)163 (2)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

Table 2

Comparison of the geometrical characteristics of the coordination polyhedra in isotypic M I 2[M II(H2O)6][ZrF6]2 structures determined from single-crystal data (Å, °, Å3)

 K2[Ni(H2O)6][ZrF6]2aK2[Cu(H2O)6][ZrF6]2bK2[Zn(H2O)6][ZrF6]2cCs2[Zn(H2O)6][ZrF6]2d
Space groupP21/nP21/cP21/cP21/n
a6.6090 (1)6.631 (6)6.631 (1)6.970 (1)
b10.0398 (1)9.981 (10)10.071 (1)10.515 (2)
c11.7843 (1)12.921 (12)12.952 (1)11.803 (2)
β95.897 (1)114.20 (15)114.96 (2)93.56 (3)
V777.786 (16)780.01 (1)784.16 (2)863.4 (3)
 Ni—O1 = 2.0548 (10) (2×)Cu—O1 = 1.966 (4) (2×)Zn—O1 = 2.0856 (2) (2×)Zn—O3 = 2.096 (6) (2×)
Distances MII—ONi—O3 = 2.0570 (11) (2×)Cu—O2 = 2.025 (6) (2×)Zn—O2 = 2.0940 (1) (2×)Zn—O1 = 2.099 (5) (2×)
 Ni—O2 = 2.0781 (9) (2×)Cu—O3 = 2.327 (5) (2×)Zn—O3 = 2.1185 (2) (2×)Zn—O2 = 2.105 (5) (2×)
Average MII—O bond length2.0632.1062.0992.100
Polyhedral volume11.68412.33512.31812.341
Distortion index (bond length)0.004830.060890.006070.00156
Quadratic elongation1.00131.01241.00111.0006
 Zr—F6 = 1.9718 (9)Zr—F3 = 1.968 (5)Zr—F3 = 1.9727 (3)Zr—F3 = 1.962 (5)
 Zr—F5 = 2.0006 (8)Zr—F1 = 2.004 (5)Zr—F1 = 2.0018 (3)Zr—F6 = 1.977 (5)
 Zr—F3 = 2.0293 (9)Zr—F5 = 2.029 (4)Zr—F5 = 2.0277 (3)Zr—F5 = 2.037 (5)
Distances Zr—F (Å)Zr—F2 = 2.0554 (8)Zr—F6 = 2.059 (4)Zr—F6 = 2.0570 (3)Zr—F4 = 2.067 (4)
 Zr—F1 = 2.0708 (8)Zr—F2 = 2.063 (4)Zr—F2 = 2.0668 (4)Zr—F2 = 2.069 (4)
 Zr—F4 = 2.1468 (9)Zr—F4 = 2.156 (5)Zr—F4 = 2.1501 (4)Zr—F1 = 2.156 (4)
 Zr—F4 = 2.1614 (8)Zr—F4 = 2.160 (4)Zr—F4 = 2.1628 (4)Zr—F1 = 2.180 (4)
Average Zr—F bond length2.0622.0632.0632.064
Polyhedral volume13.66913.67413.67513.692
Distortion index (bond length)0.026620.026500.026540.02985
 K—F5 = 2.6496 (10)K—F1 = 2.668 (5)K—F1 = 2.6506 (3)Cs—F6 = 2.911 (5)
 K—F3 = 2.7366 (9)K—F6 = 2.750 (6)K—F2 = 2.7395 (4)Cs—F4 = 3.046 (4)
 K—F6 = 2.7603 (11)K—F3 = 2.756 (5)K—F5 = 2.7633 (2)Cs—F2 = 3.057 (4)
Distances K—F/OK—F2 = 2.7658 (9)K—F5 = 2.767 (5)K—F6 = 2.7739 (2)Cs—F3 = 3.065 (5)
 K—F1 = 2.7895 (9)K—F2 = 2.799 (5)K—F3 = 2.8094 (2)Cs—F3 = 3.102 (5)
 K—O2 = 2.8927 (10)K—O3 = 2.942 (5)K—O1 = 2.8968 (3)Cs—O2 = 3.218 (5)
 K—O1 = 3.1012 (10)K—O1 = 2.980 (5)K—O2 = 3.0873 (5)Cs—O1 = 3.236 (5)
 K—F6 = 3.1684 (12)K—F3 = 3.1307 (7)K—F3 = 3.1707 (7)Cs—F5 = 3.228 (6)
Average MI—F/O bond length2.8582.8492.8613.118
Polyhedral volume38.45838.15838.56948.130
Distortion index (bond length)0.051460.044290.049840.02627

Notes: (a) this work; (b) Fischer & Weiss (1973 ▶); (c) Bukvetskii et al. (1993 ▶); (d) Hitchman et al. (2002 ▶).

  2 in total

1.  Dynamic behavior of the Jahn-Teller distorted Cu(H(2)O)(6)(2+) ion in Cu(2+) doped Cs(2)[Zn(H(2)O)(6)](ZrF(6))(2) and the crystal structure of the host lattice.

Authors:  Michael A Hitchman; Yurii V Yablokov; Vladimir E Petrashen; Maria A Augustyniak-Jabłokov; Horst Stratemeier; Mark J Riley; Kazimierz Łukaszewicz; Paweł E Tomaszewski; Adam Pietraszko
Journal:  Inorg Chem       Date:  2002-01-28       Impact factor: 5.165

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
  2 in total

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