The charge distribution has been determined by multipole refinements against single-crystal X-ray diffraction data. In the refinements a comparison was made between the densities based on H-atom parameters from X-ray and neutron data, respectively. X-ray study: λ(Mo Kα) = 0.71073 Å, F(000) = 408; at 30 K: R(F) = 0.015 for 6686 reflections; at 295 K: R(F) = 0.022 for 4630 reflections. The nickel ion is octahedrally surrounded by four water molecules and two chloride ions, forming a locally neutral Ni(H2O)4Cl2 complex. Two of the water molecules are coordinated to nickel approximately in one of the tetrahedral (`lone-pair') directions; the other two are trigonally coordinated. At 30 K one H atom in one of the trigonally coordinated water molecules is disordered, with equal occupation of two different positions. Owing to the polarizing influence of the nickel ion there are two peaks in the lone-pair plane of the water molecules when these are tetrahedrally coordinated; for those trigonally coordinated there is just one peak. The individual (`partial') charge densities, calculated from the deformation functions of only nickel or the separate water molecules, have also been calculated to study the effects of superposition of the individual densities. In the individual density of nickel an excess is observed in the diagonal directions and a deficiency in the ligand directions. However, owing to the influence of the whole crystalline environment, the maxima around nickel are not found in the planes defined by nickel and the six ligands.
Supporting information
| Crystallographic Information File (CIF) Contains datablocks text, 1, 2, 3, 4 |
| Portable Document Format (PDF) file Supplementary material |
| Portable Document Format (PDF) file Supplementary material |
| Structure factor file (SHELXL table format) Supplementary material |
| Structure factor file (SHELXL table format) Supplementary material |
Data collection: STOE 4-circle Diffractometer Control Program for (1), (3); Diffractometer Control Program D9 for (2), (4). Cell refinement: STOE 4-circle Diffractometer Control Program for (1), (3); Diffractometer Control Program D9 for (2), (4). Data reduction: DATRED Lundgren (1982) for (1), (3); Wilkinson, Khamis, Stansfield & McIntyre (1988) for (2), (4). For all compounds, program(s) used to refine structure: UPALS Lundgren (1982).
Crystal data top
Cl2Ni·4(H2O) | Z = 4 |
Mr = 201.7 | Dx = 2.240 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 20 reflections |
a = 5.985 (3) Å | θ = 15–25° |
b = 9.291 (5) Å | µ = 4.05 mm−1 |
c = 10.931 (6) Å | T = 295 K |
β = 100.32 (3)° | Prism with 21 faces, light green |
V = 598 (1) Å3 | 0.23 × 0.20 × 0.09 mm |
Data collection top
Stoe four-circle diffractometer | Rint = 0.024 |
ω–2θ scans | θmax = 50.8° |
Absorption correction: gaussian (Coppens, Leiserowitz & Rabinovich, 1965) | h = −6→13 |
Tmin = 0.481, Tmax = 0.564 | k = 0→20 |
6710 measured reflections | l = −23→23 |
6137 independent reflections | 6 standard reflections every 240 min |
4630 reflections with Fo2 > 3σ(Fo2) | intensity decay: none |
Refinement top
Refinement on F2 | w = 1/[σ2(Fo2) + k2Fo4] |
R[F2 > 2σ(F2)] = 0.028 | (Δ/σ)max = 0.005 |
wR(F2) = 0.0341 | Δρmax = 0.15 e Å−3 |
S = 1.31 | Δρmin = −0.15 e Å−3 |
4630 reflections | Extinction correction: Gaussian type I isotropic (Becker & Coppens, 1974, 1975) |
164 parameters | Extinction coefficient: 4.92E4 |
H atoms:placed at positions found by neutron diffraction, see text | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni | 0.01357 (2) | 0.16902 (1) | 0.26396 (1) | 0.0144 (1) | |
Cl1 | −0.02924 (2) | 0.36300 (2) | 0.12066 (1) | 0.0207 (1) | |
Cl2 | 0.09642 (2) | 0.30579 (2) | 0.42923 (1) | 0.0227 (1) | |
O1 | 0.34593 (11) | 0.22553 (6) | 0.33707 (5) | 0.0208 (2) | |
O2 | −0.32321 (8) | 0.11558 (6) | 0.19534 (7) | 0.0202 (3) | |
O3 | 0.12495 (11) | 0.04131 (7) | 0.13162 (6) | 0.0286 (4) | |
O4 | 0.03767 (9) | −0.01607 (9) | 0.36810 (6) | 0.0283 (3) | |
H41 | 0.178 (2) | −0.064 (2) | 0.388 (1) | 0.053 (5) | |
H42 | −0.086 (3) | −0.057 (2) | 0.393 (1) | 0.112 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.01329 (5) | 0.01487 (5) | 0.01521 (5) | −0.00012 (4) | 0.00292 (3) | 0.00014 (5) |
Cl1 | 0.02421 (8) | 0.01902 (7) | 0.01909 (7) | −0.00090 (4) | 0.00308 (4) | 0.00318 (5) |
Cl2 | 0.02446 (8) | 0.02470 (8) | 0.01900 (7) | 0.00333 (5) | 0.00526 (5) | −0.00395 (5) |
O1 | 0.0152 (2) | 0.0272 (3) | 0.0201 (2) | 0.0001 (2) | 0.0020 (2) | 0.0021 (2) |
O2 | 0.0171 (2) | 0.0206 (2) | 0.0229 (2) | −0.0027 (2) | 0.0008 (2) | 0.0006 (2) |
O3 | 0.0359 (4) | 0.0232 (3) | 0.0269 (3) | 0.0035 (2) | 0.0145 (3) | −0.0018 (2) |
O4 | 0.0237 (3) | 0.0245 (3) | 0.0368 (4) | 0.0038 (2) | 0.0080 (2) | 0.0132 (3) |
Geometric parameters (Å, º) top
Ni—O1 | 2.074 (1) | O1—H12 | 0.889 (8) |
Ni—O2 | 2.081 (1) | O2—H21 | 0.951 (8) |
Ni—O3 | 2.071 (1) | O2—H22 | 0.959 (8) |
Ni—O4 | 2.053 (1) | O3—H31 | 0.931 (9) |
Ni—Cl1 | 2.371 (1) | O3—H32 | 0.957 (9) |
Ni—Cl2 | 2.395 (1) | O4—H41 | 0.945 (9) |
O1—H11 | 0.974 (8) | O4—H42 | 0.921 (17) |
| | | |
Ni···Nii | 5.985 (3) | Ni···Niv | 5.593 (3) |
Ni···Niii | 5.985 (3) | Ni···Nivi | 5.593 (3) |
Ni···Niiii | 5.935 (3) | Ni···Nivii | 5.477 (3) |
Ni···Niiv | 5.935 (3) | Ni···Nivi | 5.477 (3) |
| | | |
O1—Ni—O2 | 178.18 (3) | Cl1—Ni—Cl2 | 94.77 (4) |
O1—Ni—O3 | 90.44 (4) | Cl1—Ni—O3 | 89.10 (4) |
O1—Ni—O4 | 91.79 (3) | Cl2—Ni—O4 | 91.60 (4) |
O1—Ni—Cl1 | 92.56 (3) | Nii—Ni—Niii | 180 |
O1—Ni—Cl2 | 87.10 (3) | Nii—Ni—Niiv | 109.83 (3) |
O2—Ni—O3 | 91.36 (4) | Nii—Ni—Niv | 56.34 (2) |
O2—Ni—O4 | 88.13 (3) | Nii—Ni—Nivi | 121.78 (2) |
O3—Ni—O4 | 84.72 (4) | Nii—Ni—Niviii | 56.34 (2) |
O2—Ni—Cl1 | 87.71 (3) | Nii—Ni—Nivii | 121.78 (2) |
O2—Ni—Cl2 | 91.10 (4) | Nii—Ni—Niiii | 70.17 (3) |
Cl1—Ni—O4 | 172.47 (2) | Nivi—Ni—Niviii | 173.51 (1) |
Cl2—Ni—O3 | 175.49 (2) | Nivii—Ni—Niv | 173.51 (1) |
Symmetry codes: (i) x−1, y, z; (ii) x+1, y, z; (iii) x−1/2, −y+1/2, z−1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) −x−1/2, y−1/2, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, y+1/2, −z+1/2; (viii) −x−1/2, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | H···A | D···A | D—H···A |
O1—H11···Cl1iv | 2.19 (1) | 3.165 (2) | 176 (1) |
O1—H12···O2ii | 2.02 (1) | 2.909 (1) | 174 (1) |
O2—H21···Cl2vi | 2.27 (1) | 3.157 (2) | 154 (1) |
O2—H22···Cl2iii | 2.30 (1) | 3.184 (1) | 153 (1) |
O3—H31···Cl2ix | 2.40 (1) | 3.319 (1) | 170 (1) |
O3—H32···O1vi | 2.02 (1) | 2.955 (2) | 167 (1) |
O4—H41···Cl1vi | 2.22 (1) | 3.131 (2) | 161 (1) |
O4—H42···Cl1v | 2.39 (2) | 3.266 (2) | 158 (1.3) |
Symmetry codes: (ii) x+1, y, z; (iii) x−1/2, −y+1/2, z−1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) −x−1/2, y−1/2, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (ix) −x+3/2, y−1/2, −z+1/2. |
Crystal data top
Cl2Ni·4(H2O) | Z = 4 |
Mr = 201.7 | Dx = 2.211 Mg m−3 |
Monoclinic, P21/n | Neutron radiation, λ = 0.8405 Å |
Hall symbol: -P 2yn | Cell parameters from 175 reflections |
a = 6.006 (3) Å | θ = 3–40° |
b = 9.338 (5) Å | µ = 0.24 mm−1 |
c = 10.986 (5) Å | T = 295 K |
β = 100.45 (3)° | Prism 10 faces, light green |
V = 606 (1) Å3 | 4.0 × 2.0 × 1.7 mm |
Data collection top
D9 diffractometer | θmax = 40° |
ω–xθ scans | h = 0→9 |
Absorption correction: gaussian (Coppens, Leiserowitz & Rabinovich, 1965) | k = 0→14 |
Tmin = 0.644, Tmax = 0.738 | l = −16→16 |
2292 measured reflections | 1 standard reflections every 120 min |
2292 independent reflections | intensity decay: none |
2237 reflections with unaffected by pyrasite peaks | |
Refinement top
Refinement on F2 | H atoms refined |
R[F2 > 2σ(F2)] = 0.18 | w = 1/[σ2(Fo2) + k2Fo4] |
wR(F2) = 0.17 | (Δ/σ)max = 0.03 |
S = 2.34 | Extinction correction: no correction |
2237 reflections | Extinction coefficient: 0 |
136 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni | 0.0139 (3) | 0.1694 (2) | 0.2639 (2) | 0.019 (1) | |
Cl1 | −0.0288 (4) | 0.3625 (2) | 0.1208 (2) | 0.024 (1) | |
Cl2 | −0.0949 (4) | 0.3053 (2) | 0.4292 (2) | 0.028 (1) | |
O1 | 0.3513 (7) | 0.2252 (4) | 0.3366 (4) | 0.026 (2) | |
O2 | −0.3244 (7) | 0.1164 (4) | 0.1953 (4) | 0.026 (2) | |
O3 | 0.1225 (8) | 0.0419 (5) | 0.1315 (4) | 0.035 (2) | |
O4 | 0.0358 (8) | −0.0174 (5) | 0.3672 (4) | 0.033 (2) | |
H11 | 0.387 (2) | 0.194 (2) | 0.423 (1) | 0.050 (4) | |
H12 | 0.454 (2) | 0.192 (2) | 0.299 (1) | 0.051 (5) | |
H21 | −0.360 (1) | 0.152 (3) | 0.113 (1) | 0.056 (5) | |
H22 | −0.346 (1) | 0.014 (2) | 0.187 (1) | 0.053 (5) | |
H31 | 0.192 (1) | 0.076 (3) | 0.067 (1) | 0.057 (5) | |
H32 | 0.159 (2) | −0.058 (2) | 0.146 (1) | 0.051 (5) | |
H41 | 0.178 (2) | −0.064 (2) | 0.388 (1) | 0.053 (5) | |
H42 | −0.086 (3) | −0.057 (2) | 0.393 (1) | 0.112 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.016 (1) | 0.020 (1) | 0.020 (1) | −0.000 (1) | 0.004 (1) | −0.000 (1) |
Cl1 | 0.028 (1) | 0.024 (1) | 0.021 (1) | −0.002 (1) | 0.001 (1) | 0.002 (1) |
Cl2 | 0.034 (1) | 0.028 (1) | 0.021 (1) | 0.005 (1) | 0.003 (1) | −0.004 (1) |
O1 | 0.027 (2) | 0.027 (2) | 0.025 (2) | −0.004 (1) | −0.004 (1) | 0.005 (1) |
O2 | 0.028 (2) | 0.022 (2) | 0.026 (2) | −0.004 (1) | 0.001 (1) | −0.002 (1) |
O3 | 0.046 (2) | 0.032 (2) | 0.026 (2) | 0.006 (2) | 0.006 (2) | −0.004 (2) |
O4 | 0.029 (2) | 0.033 (2) | 0.036 (2) | 0.004 (2) | 0.006 (2) | 0.009 (2) |
H11 | 0.070 (5) | 0.046 (4) | 0.033 (4) | −0.005 (4) | 0.001 (3) | −0.005 (3) |
H12 | 0.045 (5) | 0.075 (6) | 0.033 (4) | −0.004 (4) | 0.000 (3) | 0.003 (4) |
H21 | 0.052 (5) | 0.078 (7) | 0.036 (4) | 0.002 (4) | 0.000 (3) | 0.009 (4) |
H22 | 0.035 (4) | 0.030 (4) | 0.093 (7) | −0.008 (3) | −0.009 (4) | 0.003 (4) |
H31 | 0.044 (5) | 0.071 (6) | 0.055 (5) | 0.001 (4) | 0.021 (4) | 0.004 (4) |
H32 | 0.057 (5) | 0.038 (4) | 0.059 (5) | 0.014 (4) | 0.006 (4) | −0.004 (4) |
H41 | 0.047 (5) | 0.046 (4) | 0.065 (5) | 0.018 (4) | 0.001 (4) | 0.013 (4) |
H42 | 0.153 (15) | 0.052 (6) | 0.131 (13) | 0.002 (7) | 0.087 (12) | 0.036 (7) |
Crystal data top
Cl2Ni·4(H2O) | Z = 4 |
Mr = 201.7 | Dx = 2.260 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 20 reflections |
a = 5.961 (3) Å | θ = 15–25° |
b = 9.273 (5) Å | µ = 4.09 mm−1 |
c = 10.891 (7) Å | T = 30 K |
β = 100.02 (5)° | Prism with 9 faces, light green |
V = 593 (1) Å3 | 0.21 × 0.20 × 0.08 mm |
Data collection top
Huber-Aracor 400 mm diameter four-circle diffractometer | Rint = 0.019 |
ω–2θ scans | θmax = 52.6° |
Absorption correction: gaussian (Coppens, Leiserowitz & Rabinovich, 1965) | h = −13→13 |
Tmin = 0.430, Tmax = 0.635 | k = −20→20 |
7534 measured reflections | l = −5→24 |
6686 independent reflections | 6 standard reflections every 240 min |
6686 reflections with Fo2 > 3σ(Fo2) | intensity decay: none |
Refinement top
Refinement on F2 | w = 1/[σ2(Fo2) + k2Fo4] |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max = 0.006 |
wR(F2) = 0.0327 | Δρmax = 0.15 e Å−3 |
S = 1.42 | Δρmin = −0.15 e Å−3 |
6686 reflections | Extinction correction: Gaussian type I isotropic (Becker & Coppens, 1974, 1975) |
164 parameters | Extinction coefficient: 1.11E3 |
H atoms:placed at positions found by neutron diffraction, see text | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni | 0.01461 (1) | 0.16986 (1) | 0.26586 (1) | 0.00333 (2) | |
Cl1 | −0.02658 (2) | 0.36338 (1) | 0.12080 (1) | 0.00779 (4) | |
Cl2 | −0.09570 (2) | 0.31012 (1) | 0.43076 (1) | 0.00556 (4) | |
O1 | 0.34847 (7) | 0.22745 (4) | 0.33802 (3) | 0.0067 (1) | |
O2 | −0.32509 (6) | 0.11736 (4) | 0.19799 (4) | 0.0070 (1) | |
O3 | 0.12182 (7) | 0.03982 (4) | 0.13301 (4) | 0.0084 (1) | |
O4 | 0.03855 (6) | −0.01465 (5) | 0.37314 (4) | 0.0097 (1) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.00305 (2) | 0.00317 (2) | 0.00377 (2) | 0.00001 (2) | 0.00074 (2) | 0.00002 (2) |
Cl1 | 0.01344 (5) | 0.00453 (3) | 0.00542 (3) | −0.00101 (3) | 0.00170 (3) | 0.00047 (3) |
Cl2 | 0.00585 (4) | 0.00535 (3) | 0.00550 (3) | 0.00076 (2) | 0.00154 (3) | −0.00050 (3) |
O1 | 0.0047 (1) | 0.0084 (1) | 0.0068 (1) | 0.0001 (1) | 0.0009 (1) | −0.0006 (1) |
O2 | 0.0054 (1) | 0.0071 (1) | 0.0084 (1) | −0.0007 (1) | 0.0006 (1) | −0.0014 (1) |
O3 | 0.0101 (1) | 0.0067 (1) | 0.0084 (1) | 0.0008 (1) | 0.0043 (1) | −0.0005 (1) |
O4 | 0.0069 (1) | 0.0074 (1) | 0.0149 (2) | −0.0003 (1) | −0.0007 (1) | 0.0049 (1) |
Geometric parameters (Å, º) top
Ni—O1 | 2.078 (1) | O1—H11 | 0.992 (7) |
Ni—O2 | 2.089 (1) | O1—H12 | 0.985 (8) |
Ni—O3 | 2.068 (1) | O2—H21 | 0.972 (8) |
Ni—O4 | 2.063 (1) | O2—H22 | 0.976 (8) |
Ni—Cl1 | 2.375 (1) | O3—H31 | 0.981 (8) |
Ni—Cl2 | 2.400 (1) | O3—H32 | 0.970 (8) |
| | | |
Ni···Nii | 5.961 (2) | Ni···Niv | 5.585 (2) |
Ni···Niii | 5.961 (2) | Ni···Nivi | 5.585 (2) |
Ni···Niiii | 5.924 (2) | Ni···Nivii | 5.461 (2) |
Ni···Niiv | 5.924 (2) | Ni···Nivi | 5.461 (2) |
| | | |
O1—Ni—O2 | 177.86 (2) | Cl1—Ni—Cl2 | 94.49 (4) |
O1—Ni—O3 | 91.27 (4) | H11—O1—H12 | 103.4 (7) |
O1—Ni—O4 | 91.81 (4) | H21—O2—H22 | 102.6 (8) |
O1—Ni—Cl1 | 92.23 (4) | H31—O3—H32 | 108.9 (7) |
O1—Ni—Cl2 | 86.95 (4) | Nii—Ni—Niii | 180 |
O2—Ni—O3 | 90.86 (4) | Nii—Ni—Niiv | 110.07 (5) |
O2—Ni—O4 | 88.53 (4) | Nii—Ni—Niv | 56.35 (2) |
O3—Ni—O4 | 85.03 (5) | Nii—Ni—Nivi | 121.66 (2) |
O2—Ni—Cl1 | 87.64 (4) | Nii—Ni—Niviii | 56.35 (2) |
O2—Ni—Cl2 | 90.92 (4) | Nii—Ni—Nivii | 121.66 (2) |
Cl1—Ni—O4 | 172.93 (1) | Nii—Ni—Niiii | 69.93 (5) |
Cl2—Ni—O3 | 176.07 (2) | Nivi—Ni—Niviii | 172.66 (1) |
Cl1—Ni—O3 | 89.08 (5) | Nivii—Ni—Niv | 172.66 (1) |
Cl2—Ni—O4 | 91.52 (4) | | |
Symmetry codes: (i) x−1, y, z; (ii) x+1, y, z; (iii) x−1/2, −y+1/2, z−1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) −x−1/2, y−1/2, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, y+1/2, −z+1/2; (viii) −x−1/2, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | H···A | D···A | D—H···A |
O1—H11···Cl1iv | 2.17 (1) | 3.154 (2) | 174 (1) |
O1—H12···O2ii | 1.88 (1) | 2.861 (1) | 174 (1) |
O2—H21···Cl2vi | 2.22 (1) | 3.145 (2) | 159 (1) |
O2—H22···Cl2iii | 2.28 (1) | 3.174 (1) | 153 (1) |
O3—H31···Cl2ix | 2.34 (1) | 3.304 (2) | 169 (1) |
O3—H32···O1vi | 1.96 (1) | 2.916 (2) | 169 (1) |
O4—H41···Cl1vi | 2.20 (1) | 3.111 (1) | 165 (1) |
O4—H421···Cl1v | 2.33 (3) | 3.266 (2) | 163 (2) |
O4—H422···O4x | 2.02 (3) | 2.893 (2) | 157 (2) |
Symmetry codes: (ii) x+1, y, z; (iii) x−1/2, −y+1/2, z−1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) −x−1/2, y−1/2, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (ix) −x+3/2, y−1/2, −z+1/2; (x) −x, −y, −z+1. |
Crystal data top
Cl2Ni·4(H2O) | Z = 4 |
Mr = 201.7 | Dx = 2.254 Mg m−3 |
Monoclinic, P21/n | Neutron radiation, λ = 0.8405 Å |
Hall symbol: -P 2yn | Cell parameters from 233 reflections |
a = 5.968 (2) Å | θ = 3–40° |
b = 9.283 (3) Å | µ = 0.24 mm−1 |
c = 10.897 (3) Å | T = 30 K |
β = 100.08 (2)° | Prism 10 faces, light green |
V = 594 (1) Å3 | 4.0 × 2.0 × 1.7 mm |
Data collection top
D9 four-circle diffractometer | θmax = 40° |
ω–xθ scans | h = 0→9 |
Absorption correction: gaussian (Coppens, Leiserowitz & Rabinovich, 1965) | k = 0→14 |
Tmin = 0.681, Tmax = 0.748 | l = −16→16 |
1566 measured reflections | 1 standard reflections every 120 min |
1566 independent reflections | intensity decay: none |
1503 reflections with unaffected by parasite peaks | |
Refinement top
Refinement on F2 | H atoms refined |
R[F2 > 2σ(F2)] = 0.126 | w = 1/[σ2(Fo2) + k2Fo4] |
wR(F2) = 0.142 | (Δ/σ)max = 0.03 |
S = 2.99 | Extinction correction: no correction |
1503 reflections | Extinction coefficient: 0 |
136 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni | 0.0144 (4) | 0.1700 (2) | 0.2660 (2) | 0.005 (1) | |
Cl1 | −0.0260 (4) | 0.3635 (2) | 0.1209 (2) | 0.009 (1) | |
Cl2 | −0.0948 (4) | 0.3101 (2) | 0.4312 (2) | 0.007 (1) | |
O1 | 0.3499 (7) | 0.2281 (4) | 0.3385 (3) | 0.008 (2) | |
O2 | −0.3263 (7) | 0.1170 (4) | 0.1987 (3) | 0.009 (2) | |
O3 | 0.1210 (7) | 0.0400 (4) | 0.1333 (3) | 0.008 (2) | |
O4 | 0.0405 (10) | −0.0164 (4) | 0.3739 (3) | 0.011 (2) | |
H11 | 0.399 (1) | 0.199 (1) | 0.426 (1) | 0.028 (4) | |
H12 | 0.468 (1) | 0.188 (1) | 0.296 (1) | 0.019 (3) | |
H21 | −0.375 (2) | 0.154 (1) | 0.114 (1) | 0.038 (5) | |
H22 | −0.352 (2) | 0.014 (1) | 0.187 (1) | 0.036 (4) | |
H31 | 0.192 (2) | 0.076 (1) | 0.064 (1) | 0.032 (4) | |
H32 | 0.153 (2) | −0.062 (1) | 0.143 (1) | 0.032 (4) | |
H41 | 0.175 (2) | −0.065 (1) | 0.383 (1) | 0.035 (5) | |
H421 | −0.097 (4) | −0.070 (2) | 0.376 (2) | 0.037 (13) | 0.52 (5) |
H422 | −0.019 (4) | −0.021 (2) | 0.446 (2) | 0.027 (12) | 0.48 (5) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.005 (1) | 0.006 (1) | 0.004 (1) | 0.000 (1) | −0.000 (1) | 0.001 (1) |
Cl1 | 0.015 (1) | 0.006 (1) | 0.005 (1) | −0.002 (1) | 0.001 (1) | 0.001 (1) |
Cl2 | 0.010 (1) | 0.007 (1) | 0.004 (1) | 0.001 (1) | 0.002 (1) | −0.001 (1) |
O1 | 0.006 (2) | 0.011 (2) | 0.006 (1) | −0.001 (2) | 0.000 (2) | −0.002 (1) |
O2 | 0.010 (2) | 0.008 (2) | 0.009 (1) | −0.003 (2) | −0.000 (2) | −0.002 (1) |
O3 | 0.011 (2) | 0.007 (2) | 0.006 (1) | −0.003 (2) | 0.002 (2) | −0.001 (1) |
O4 | 0.009 (2) | 0.011 (2) | 0.013 (2) | −0.002 (2) | −0.003 (2) | 0.006 (1) |
H11 | 0.045 (5) | 0.025 (3) | 0.013 (3) | 0.004 (4) | −0.001 (3) | 0.002 (2) |
H12 | 0.014 (4) | 0.034 (4) | 0.009 (3) | 0.004 (3) | 0.001 (3) | −0.011 (2) |
H21 | 0.038 (5) | 0.060 (6) | 0.018 (3) | 0.006 (5) | −0.003 (3) | 0.007 (3) |
H22 | 0.032 (5) | 0.011 (3) | 0.065 (5) | −0.004 (4) | −0.003 (4) | −0.007 (3) |
H31 | 0.046 (6) | 0.029 (4) | 0.021 (3) | 0.003 (4) | 0.022 (4) | 0.006 (3) |
H32 | 0.045 (5) | 0.018 (3) | 0.032 (3) | 0.005 (4) | 0.012 (4) | 0.006 (3) |
H41 | 0.048 (6) | 0.023 (4) | 0.035 (4) | 0.013 (4) | 0.005 (4) | −0.002 (3) |
H421 | 0.034 (14) | 0.021 (9) | 0.056 (16) | −0.012 (9) | 0.011 (10) | 0.015 (9) |
H422 | 0.021 (11) | 0.027 (9) | 0.035 (14) | 0.000 (8) | 0.008 (10) | −0.001 (8) |