Charge density in NiCl₂.4H₂O at 295 and 30 K

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.

Computing details

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).

(1)

Crystal data

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) Å^3	0.23 × 0.20 × 0.09 mm

Data collection

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 Fo^2 > 3σ(Fo^2)	intensity decay: none

Refinement

Refinement on F^2	w = 1/[σ^2(Fo^2) + k^2Fo^4]
R[F^2 > 2σ(F^2)] = 0.028	(Δ/σ)max = 0.005
wR(F^2) = 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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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···Ni^i	5.985 (3)	Ni···Ni^v	5.593 (3)
Ni···Ni^ii	5.985 (3)	Ni···Ni^vi	5.593 (3)
Ni···Ni^iii	5.935 (3)	Ni···Ni^vii	5.477 (3)
Ni···Ni^iv	5.935 (3)	Ni···Ni^vi	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)	Ni^i—Ni—Ni^ii	180
O1—Ni—Cl2	87.10 (3)	Ni^i—Ni—Ni^iv	109.83 (3)
O2—Ni—O3	91.36 (4)	Ni^i—Ni—Ni^v	56.34 (2)
O2—Ni—O4	88.13 (3)	Ni^i—Ni—Ni^vi	121.78 (2)
O3—Ni—O4	84.72 (4)	Ni^i—Ni—Ni^viii	56.34 (2)
O2—Ni—Cl1	87.71 (3)	Ni^i—Ni—Ni^vii	121.78 (2)
O2—Ni—Cl2	91.10 (4)	Ni^i—Ni—Ni^iii	70.17 (3)
Cl1—Ni—O4	172.47 (2)	Ni^vi—Ni—Ni^viii	173.51 (1)
Cl2—Ni—O3	175.49 (2)	Ni^vii—Ni—Ni^v	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)

D—H···A	H···A	D···A	D—H···A
O1—H11···Cl1^iv	2.19 (1)	3.165 (2)	176 (1)
O1—H12···O2^ii	2.02 (1)	2.909 (1)	174 (1)
O2—H21···Cl2^vi	2.27 (1)	3.157 (2)	154 (1)
O2—H22···Cl2^iii	2.30 (1)	3.184 (1)	153 (1)
O3—H31···Cl2^ix	2.40 (1)	3.319 (1)	170 (1)
O3—H32···O1^vi	2.02 (1)	2.955 (2)	167 (1)
O4—H41···Cl1^vi	2.22 (1)	3.131 (2)	161 (1)
O4—H42···Cl1^v	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.

(2)

Crystal data

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) Å^3	4.0 × 2.0 × 1.7 mm

Data collection

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

Refinement on F^2	H atoms refined
R[F^2 > 2σ(F^2)] = 0.18	w = 1/[σ^2(Fo^2) + k^2Fo^4]
wR(F^2) = 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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

(3)

Crystal data

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) Å^3	0.21 × 0.20 × 0.08 mm

Data collection

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 Fo^2 > 3σ(Fo^2)	intensity decay: none

Refinement

Refinement on F^2	w = 1/[σ^2(Fo^2) + k^2Fo^4]
R[F^2 > 2σ(F^2)] = 0.022	(Δ/σ)max = 0.006
wR(F^2) = 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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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···Ni^i	5.961 (2)	Ni···Ni^v	5.585 (2)
Ni···Ni^ii	5.961 (2)	Ni···Ni^vi	5.585 (2)
Ni···Ni^iii	5.924 (2)	Ni···Ni^vii	5.461 (2)
Ni···Ni^iv	5.924 (2)	Ni···Ni^vi	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)	Ni^i—Ni—Ni^ii	180
O2—Ni—O3	90.86 (4)	Ni^i—Ni—Ni^iv	110.07 (5)
O2—Ni—O4	88.53 (4)	Ni^i—Ni—Ni^v	56.35 (2)
O3—Ni—O4	85.03 (5)	Ni^i—Ni—Ni^vi	121.66 (2)
O2—Ni—Cl1	87.64 (4)	Ni^i—Ni—Ni^viii	56.35 (2)
O2—Ni—Cl2	90.92 (4)	Ni^i—Ni—Ni^vii	121.66 (2)
Cl1—Ni—O4	172.93 (1)	Ni^i—Ni—Ni^iii	69.93 (5)
Cl2—Ni—O3	176.07 (2)	Ni^vi—Ni—Ni^viii	172.66 (1)
Cl1—Ni—O3	89.08 (5)	Ni^vii—Ni—Ni^v	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)

D—H···A	H···A	D···A	D—H···A
O1—H11···Cl1^iv	2.17 (1)	3.154 (2)	174 (1)
O1—H12···O2^ii	1.88 (1)	2.861 (1)	174 (1)
O2—H21···Cl2^vi	2.22 (1)	3.145 (2)	159 (1)
O2—H22···Cl2^iii	2.28 (1)	3.174 (1)	153 (1)
O3—H31···Cl2^ix	2.34 (1)	3.304 (2)	169 (1)
O3—H32···O1^vi	1.96 (1)	2.916 (2)	169 (1)
O4—H41···Cl1^vi	2.20 (1)	3.111 (1)	165 (1)
O4—H421···Cl1^v	2.33 (3)	3.266 (2)	163 (2)
O4—H422···O4^x	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.

(4)

Crystal data

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) Å^3	4.0 × 2.0 × 1.7 mm

Data collection

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

Refinement on F^2	H atoms refined
R[F^2 > 2σ(F^2)] = 0.126	w = 1/[σ^2(Fo^2) + k^2Fo^4]
wR(F^2) = 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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)