On the sequence of three related phases of [Ni(H₂O)₂(15-crown-5)](HSO₄)₂ in the temperature range 110–295 K

Attempts to prepare the compound [Ni(H₂O)₂(15-crown-5)](X)₂ were eventually successful with X = NO provided that a synthetic route aimed at restricting water was followed. Application of this method was extended to make the analogous compound with X = HSO, for which three symmetry-related phases were isolated between 295 and 110 K: a room-temperature phase with Z′ = ½ [phase (I)], an intermediate-temperature phase with Z′ = 1 [phase (II)] and a low-temperature phase with Z′ = 2 [phase (III)]. The phases are related by two reversible solid–solid phase transitions, and both transitions take place without a significant loss of crystallinity. In the phase sequence (I) ↔ (II) ↔ (III) (Z′: ½ ↔ 1 ↔ 2), the crystal packing remains remarkably similar but the degree of order in the crystal changes significantly; the structure is very disordered at room and intermediate temperatures but is ordered at 110 K. The compound [Ni(H₂O)₂(15-crown-5)](HSO₄)₂ has a complicated hydrogen-bonding network, which contains O—H...O bonds between the counterions. Structural changes are largest along some face-diagonal directions in the sequence (I) ↔ (II) ↔ (III).

Computing details

For all structures, data collection: COLLECT (Nonius, 1999); cell refinement: PEAKREF (Schreurs, 2005); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003).

'diaqua(15-crown-5)nickel(II) hydrogen sulfate' (I)

Crystal data

C10H24NiO7·2(HO4S)	F(000) = 1064
Mr = 509.14	Dx = 1.711 Mg m^−3
Orthorhombic, Cmc21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 6073 reflections
a = 17.8301 (2) Å	θ = 2.3–27.5°
b = 7.4833 (1) Å	µ = 1.26 mm^−1
c = 14.8133 (5) Å	T = 295 K
V = 1976.51 (8) Å^3	Tabular, yellow
Z = 4	0.34 × 0.14 × 0.12 mm

Data collection

Nonius KappaCCD diffractometer	2161 independent reflections
Radiation source: rotating anode	2017 reflections with I > 2sσ(I)
Graphite monochromator	Rint = 0.019
φ and ω scans	θmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	h = −23→21
Tmin = 0.77, Tmax = 0.86	k = −7→9
10012 measured reflections	l = −19→16

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.021	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.048	w = 1/[σ^2(Fo^2) + (0.0228P)^2 + 0.614P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.001
2161 reflections	Δρmax = 0.16 e Å^−3
256 parameters	Δρmin = −0.22 e Å^−3
296 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.004 (12)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ni1	0.5000	0.4064 (4)	0.49376 (11)	0.0316 (4)	0.646 (7)
Ni1'	0.5000	0.4515 (5)	0.5079 (3)	0.0316 (4)	0.354 (7)
C1	0.5437 (5)	0.0639 (10)	0.4194 (6)	0.0695 (19)	0.50
H1A	0.5392	0.0035	0.4771	0.083*	0.50
H1B	0.5732	−0.0104	0.3792	0.083*	0.50
C2	0.4700 (5)	0.0967 (11)	0.3811 (5)	0.070 (2)	0.50
H2A	0.4745	0.1519	0.3221	0.085*	0.50
H2B	0.4427	−0.0146	0.3747	0.085*	0.50
C3	0.3601 (4)	0.2580 (8)	0.4165 (5)	0.0741 (16)	0.50
H3A	0.3293	0.1513	0.4139	0.089*	0.50
H3B	0.3608	0.3116	0.3569	0.089*	0.50
C4	0.3284 (7)	0.3825 (15)	0.4804 (10)	0.054 (2)	0.50
H4A	0.2920	0.4580	0.4503	0.065*	0.50
H4B	0.3028	0.3174	0.5279	0.065*	0.50
C5	0.3619 (6)	0.6524 (14)	0.5587 (8)	0.0449 (17)	0.50
H5A	0.3151	0.6338	0.5907	0.054*	0.50
H5B	0.3539	0.7424	0.5126	0.054*	0.50
C6	0.4209 (6)	0.711 (2)	0.6222 (9)	0.052 (2)	0.50
H6A	0.4117	0.8337	0.6410	0.062*	0.50
H6B	0.4210	0.6359	0.6754	0.062*	0.50
C7	0.5566 (6)	0.721 (2)	0.6314 (10)	0.060 (3)	0.50
H7A	0.5546	0.6414	0.6830	0.072*	0.50
H7B	0.5600	0.8432	0.6532	0.072*	0.50
C8	0.6210 (7)	0.6787 (17)	0.5748 (10)	0.066 (3)	0.50
H8A	0.6237	0.7609	0.5243	0.079*	0.50
H8B	0.6670	0.6890	0.6094	0.079*	0.50
C9	0.6709 (8)	0.4249 (13)	0.4927 (9)	0.062 (3)	0.50
H9A	0.7173	0.4301	0.5268	0.074*	0.50
H9B	0.6777	0.4902	0.4368	0.074*	0.50
C10	0.6502 (3)	0.2315 (8)	0.4730 (4)	0.0570 (14)	0.50
H10A	0.6870	0.1774	0.4333	0.068*	0.50
H10B	0.6480	0.1630	0.5285	0.068*	0.50
O1	0.5790 (5)	0.2357 (17)	0.4309 (9)	0.063 (2)	0.50
O2	0.4321 (6)	0.2124 (15)	0.4414 (8)	0.054 (2)	0.50
O3	0.3862 (8)	0.4907 (15)	0.5188 (6)	0.0434 (18)	0.50
O4	0.4917 (10)	0.6992 (4)	0.5765 (2)	0.051 (2)	0.50
O5	0.6120 (8)	0.5002 (16)	0.5430 (6)	0.050 (2)	0.50
O6	0.5000	0.5629 (5)	0.3841 (2)	0.0702 (9)
H6	0.5342 (15)	0.603 (4)	0.360 (2)	0.105*
O7	0.5000	0.2807 (3)	0.61257 (16)	0.0492 (6)
H7	0.4637 (12)	0.261 (4)	0.6423 (19)	0.074*
S1	0.3281 (2)	0.7620 (5)	0.2505 (5)	0.0381 (11)	0.613 (4)
O8	0.3688 (2)	0.6671 (6)	0.3154 (3)	0.0892 (14)	0.613 (4)
O9	0.37679 (17)	0.8561 (4)	0.1849 (2)	0.0610 (9)	0.613 (4)
O10	0.2669 (4)	0.6670 (9)	0.2100 (5)	0.065 (2)	0.613 (4)
O11	0.28854 (19)	0.9086 (5)	0.3041 (2)	0.0656 (10)	0.613 (4)
H11	0.2610	0.9657	0.2704	0.098*	0.613 (4)
S1'	0.3298 (4)	0.7621 (8)	0.2608 (9)	0.0351 (14)	0.387 (4)
O8'	0.4013 (2)	0.6824 (6)	0.2555 (3)	0.0537 (12)	0.387 (4)
O9'	0.3068 (3)	0.7980 (7)	0.3534 (3)	0.0589 (14)	0.387 (4)
O10'	0.2836 (7)	0.6451 (17)	0.2070 (8)	0.077 (3)	0.387 (4)
O11'	0.3355 (3)	0.9379 (6)	0.2111 (4)	0.0617 (15)	0.387 (4)
H11'	0.3209	1.0189	0.2439	0.093*	0.387 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.02984 (15)	0.0374 (9)	0.0277 (6)	0.000	0.000	0.0039 (6)
Ni1'	0.02984 (15)	0.0374 (9)	0.0277 (6)	0.000	0.000	0.0039 (6)
C1	0.083 (4)	0.049 (3)	0.077 (5)	0.017 (3)	0.011 (4)	−0.012 (4)
C2	0.086 (4)	0.057 (4)	0.069 (4)	−0.010 (3)	0.008 (3)	−0.021 (3)
C3	0.058 (3)	0.086 (4)	0.079 (4)	−0.013 (3)	−0.024 (3)	−0.018 (3)
C4	0.023 (3)	0.082 (5)	0.057 (4)	−0.016 (3)	−0.012 (3)	−0.007 (4)
C5	0.038 (4)	0.051 (3)	0.046 (4)	0.018 (3)	0.000 (3)	0.001 (3)
C6	0.060 (6)	0.046 (3)	0.050 (4)	0.014 (4)	0.001 (4)	−0.013 (3)
C7	0.059 (6)	0.062 (4)	0.057 (5)	−0.025 (4)	−0.009 (4)	−0.011 (3)
C8	0.047 (6)	0.082 (6)	0.067 (6)	−0.025 (4)	−0.006 (4)	−0.003 (4)
C9	0.028 (4)	0.107 (6)	0.051 (4)	0.000 (4)	0.003 (4)	0.026 (5)
C10	0.039 (2)	0.093 (4)	0.039 (3)	0.033 (3)	0.007 (2)	0.009 (3)
O1	0.039 (3)	0.083 (4)	0.066 (4)	0.015 (3)	0.015 (3)	0.007 (3)
O2	0.046 (3)	0.066 (4)	0.049 (3)	−0.003 (2)	−0.010 (3)	−0.020 (3)
O3	0.027 (2)	0.053 (3)	0.049 (4)	0.0011 (18)	−0.005 (3)	−0.011 (3)
O4	0.056 (7)	0.0487 (13)	0.0491 (14)	−0.011 (3)	−0.007 (3)	−0.0077 (11)
O5	0.030 (3)	0.073 (4)	0.048 (4)	−0.015 (3)	−0.001 (3)	0.017 (3)
O6	0.0364 (12)	0.117 (3)	0.0573 (16)	0.000	0.000	0.0518 (16)
O7	0.0290 (10)	0.0780 (16)	0.0407 (13)	0.000	0.000	0.0265 (11)
S1	0.0290 (13)	0.0368 (16)	0.048 (2)	0.0089 (10)	−0.0036 (8)	0.0008 (8)
O8	0.058 (2)	0.106 (3)	0.103 (3)	0.0152 (19)	−0.027 (2)	0.049 (2)
O9	0.0574 (17)	0.0463 (15)	0.079 (2)	0.0042 (13)	0.0362 (16)	0.0050 (14)
O10	0.048 (3)	0.050 (2)	0.097 (5)	−0.0115 (18)	−0.034 (3)	0.017 (2)
O11	0.069 (2)	0.082 (2)	0.0451 (17)	0.0254 (17)	0.0166 (13)	−0.0061 (16)
S1'	0.028 (2)	0.038 (3)	0.039 (2)	−0.0105 (16)	0.0013 (12)	0.0016 (11)
O8'	0.041 (2)	0.076 (3)	0.044 (2)	0.024 (2)	0.0032 (19)	0.005 (2)
O9'	0.055 (3)	0.080 (3)	0.042 (2)	0.005 (2)	0.0131 (19)	−0.002 (2)
O10'	0.065 (6)	0.097 (7)	0.069 (5)	−0.046 (5)	0.025 (4)	−0.042 (5)
O11'	0.059 (3)	0.048 (3)	0.078 (3)	−0.001 (2)	0.017 (2)	0.028 (2)

Geometric parameters (Å, º)

Ni1—Ni1'	0.398 (3)	C6—H6B	0.9700
Ni1—O7	1.996 (3)	C7—O4	1.425 (10)
Ni1—O6	2.002 (3)	C7—C8	1.456 (10)
Ni1—O2	2.043 (11)	C7—H7A	0.9700
Ni1—O2^i	2.043 (11)	C7—H7B	0.9700
Ni1—O1^i	2.117 (12)	C8—O5	1.426 (11)
Ni1—O1	2.117 (12)	C8—H8A	0.9700
Ni1—O3^i	2.157 (14)	C8—H8B	0.9700
Ni1—O3	2.157 (14)	C9—O5	1.405 (10)
Ni1—O4	2.515 (5)	C9—C10	1.522 (10)
Ni1—O5	2.239 (13)	C9—H9A	0.9700
Ni1—O5^i	2.239 (13)	C9—H9B	0.9700
Ni1'—O7	2.009 (4)	C10—O1	1.415 (10)
Ni1'—O6	2.014 (4)	C10—H10A	0.9700
Ni1'—O3^i	2.057 (14)	C10—H10B	0.9700
Ni1'—O3	2.057 (14)	O1—O2^i	0.31 (2)
Ni1'—O5	2.095 (14)	O1—C3^i	1.119 (12)
Ni1'—O5^i	2.095 (14)	O1—C2^i	1.545 (14)
Ni1'—O4^i	2.118 (5)	O2—O1^i	0.31 (2)
Ni1'—O4	2.118 (5)	O2—C1^i	1.235 (14)
Ni1'—O2	2.375 (11)	O2—C10^i	1.547 (12)
Ni1'—O2^i	2.375 (11)	O3—O5^i	0.366 (15)
C1—O1	1.441 (11)	O3—C9^i	1.19 (2)
C1—C2	1.453 (8)	O3—C8^i	1.638 (19)
C1—H1A	0.9700	O4—O4^i	0.30 (4)
C1—H1B	0.9700	O4—C7^i	1.20 (3)
C2—O2	1.415 (9)	O4—C6^i	1.70 (3)
C2—H2A	0.9700	O5—O3^i	0.366 (15)
C2—H2B	0.9700	O5—C5^i	1.25 (2)
C3—O2	1.379 (10)	O5—C4^i	1.66 (2)
C3—C4	1.444 (11)	O6—H6	0.767 (19)
C3—H3A	0.9700	O7—H7	0.797 (17)
C3—H3B	0.9700	S1—O8	1.399 (7)
C4—O3	1.428 (10)	S1—O10	1.432 (7)
C4—H4A	0.9700	S1—O9	1.482 (7)
C4—H4B	0.9700	S1—O11	1.527 (6)
C5—O3	1.414 (10)	O11—H11	0.8200
C5—C6	1.477 (9)	S1'—O8'	1.410 (7)
C5—H5A	0.9700	S1'—O10'	1.442 (10)
C5—H5B	0.9700	S1'—O9'	1.456 (12)
C6—O4	1.436 (10)	S1'—O11'	1.511 (9)
C6—H6A	0.9700	O11'—H11'	0.8200
Ni1'—Ni1—O7	86.3 (8)	C3—C4—H4B	109.6
Ni1'—Ni1—O6	86.1 (8)	H4A—C4—H4B	108.1
O7—Ni1—O6	172.3 (2)	O3—C5—C6	107.7 (9)
Ni1'—Ni1—O2	143.5 (3)	O3—C5—H5A	110.2
O7—Ni1—O2	90.0 (4)	C6—C5—H5A	110.2
O6—Ni1—O2	96.2 (4)	O3—C5—H5B	110.2
Ni1'—Ni1—O2^i	143.5 (3)	C6—C5—H5B	110.2
O7—Ni1—O2^i	90.0 (4)	H5A—C5—H5B	108.5
O6—Ni1—O2^i	96.2 (4)	O4—C6—C5	107.9 (11)
O2—Ni1—O2^i	72.6 (5)	O4—C6—H6A	110.1
Ni1'—Ni1—O1^i	138.1 (3)	C5—C6—H6A	110.1
O7—Ni1—O1^i	95.9 (4)	O4—C6—H6B	110.1
O6—Ni1—O1^i	89.8 (4)	C5—C6—H6B	110.1
O2—Ni1—O1^i	8.2 (6)	H6A—C6—H6B	108.4
O2^i—Ni1—O1^i	78.3 (2)	O4—C7—C8	106.6 (12)
Ni1'—Ni1—O1	138.1 (3)	O4—C7—H7A	110.4
O7—Ni1—O1	95.9 (4)	C8—C7—H7A	110.4
O6—Ni1—O1	89.8 (4)	O4—C7—H7B	110.4
O2—Ni1—O1	78.3 (2)	C8—C7—H7B	110.4
O2^i—Ni1—O1	8.2 (6)	H7A—C7—H7B	108.6
O1^i—Ni1—O1	83.4 (5)	O5—C8—C7	107.8 (10)
Ni1'—Ni1—O3^i	70.2 (3)	O5—C8—H8A	110.1
O7—Ni1—O3^i	89.2 (3)	C7—C8—H8A	110.1
O6—Ni1—O3^i	88.2 (3)	O5—C8—H8B	110.1
O2—Ni1—O3^i	146.1 (4)	C7—C8—H8B	110.1
O2^i—Ni1—O3^i	73.5 (4)	H8A—C8—H8B	108.5
O1^i—Ni1—O3^i	151.4 (4)	O5—C9—C10	107.6 (9)
O1—Ni1—O3^i	68.1 (4)	O5—C9—H9A	110.2
Ni1'—Ni1—O3	70.2 (3)	C10—C9—H9A	110.2
O7—Ni1—O3	89.2 (3)	O5—C9—H9B	110.2
O6—Ni1—O3	88.2 (3)	C10—C9—H9B	110.2
O2—Ni1—O3	73.5 (4)	H9A—C9—H9B	108.5
O2^i—Ni1—O3	146.1 (4)	O1—C10—C9	106.4 (8)
O1^i—Ni1—O3	68.1 (4)	O1—C10—H10A	110.5
O1—Ni1—O3	151.4 (4)	C9—C10—H10A	110.5
O3^i—Ni1—O3	140.3 (6)	O1—C10—H10B	110.5
Ni1'—Ni1—O5	64.0 (3)	C9—C10—H10B	110.5
O7—Ni1—O5	82.0 (3)	H10A—C10—H10B	108.6
O6—Ni1—O5	94.6 (3)	O2^i—O1—C3^i	144 (5)
O2—Ni1—O5	151.0 (4)	O2^i—O1—C10	110 (5)
O2^i—Ni1—O5	79.5 (4)	C3^i—O1—C1	122.2 (11)
O1^i—Ni1—O5	157.8 (4)	C10—O1—C1	115.1 (10)
O1—Ni1—O5	74.9 (4)	O2^i—O1—C2^i	60 (4)
O3^i—Ni1—O5	9.3 (4)	C3^i—O1—C2^i	123.9 (10)
O3—Ni1—O5	133.7 (2)	C10—O1—C2^i	134.6 (10)
Ni1'—Ni1—O5^i	64.0 (3)	O2^i—O1—Ni1	72 (4)
O7—Ni1—O5^i	82.0 (3)	C3^i—O1—Ni1	129.7 (8)
O6—Ni1—O5^i	94.6 (3)	C10—O1—Ni1	114.6 (7)
O2—Ni1—O5^i	79.5 (4)	C1—O1—Ni1	107.5 (7)
O2^i—Ni1—O5^i	151.0 (4)	C2^i—O1—Ni1	103.9 (6)
O1^i—Ni1—O5^i	74.9 (4)	O1^i—O2—C1^i	127 (4)
O1—Ni1—O5^i	157.8 (4)	C1^i—O2—C3	118.5 (9)
O3^i—Ni1—O5^i	133.7 (2)	O1^i—O2—C2	110 (4)
O3—Ni1—O5^i	9.3 (4)	C3—O2—C2	115.3 (9)
O5—Ni1—O5^i	126.2 (6)	O1^i—O2—C10^i	59 (4)
Ni1—Ni1'—O7	82.3 (8)	C1^i—O2—C10^i	119.6 (10)
Ni1—Ni1'—O6	82.6 (8)	C2—O2—C10^i	134.4 (9)
O7—Ni1'—O6	164.9 (2)	O1^i—O2—Ni1	100 (4)
Ni1—Ni1'—O3^i	99.4 (3)	C1^i—O2—Ni1	122.2 (8)
O7—Ni1'—O3^i	91.7 (3)	C3—O2—Ni1	118.5 (7)
O6—Ni1'—O3^i	90.7 (3)	C2—O2—Ni1	113.1 (7)
Ni1—Ni1'—O3	99.4 (3)	C10^i—O2—Ni1	112.4 (5)
O7—Ni1'—O3	91.7 (3)	O1^i—O2—Ni1'	96 (4)
O6—Ni1'—O3	90.7 (3)	C1^i—O2—Ni1'	127.6 (8)
O3^i—Ni1'—O3	161.3 (6)	C3—O2—Ni1'	113.5 (6)
Ni1—Ni1'—O5	106.2 (3)	C2—O2—Ni1'	118.7 (7)
O7—Ni1'—O5	85.4 (3)	C10^i—O2—Ni1'	106.7 (5)
O6—Ni1'—O5	98.8 (3)	O5^i—O3—C9^i	118 (5)
O3^i—Ni1'—O5	10.1 (4)	O5^i—O3—C5	57 (4)
O3—Ni1'—O5	153.7 (3)	C9^i—O3—C5	103.1 (11)
Ni1—Ni1'—O5^i	106.2 (3)	O5^i—O3—C4	124 (4)
O7—Ni1'—O5^i	85.4 (3)	C5—O3—C4	115.5 (9)
O6—Ni1'—O5^i	98.8 (3)	O5^i—O3—C8^i	49 (3)
O3^i—Ni1'—O5^i	153.7 (3)	C9^i—O3—C8^i	116.8 (13)
O3—Ni1'—O5^i	10.1 (4)	C4—O3—C8^i	129.2 (11)
O5—Ni1'—O5^i	144.8 (6)	O5^i—O3—Ni1'	91 (4)
Ni1—Ni1'—O4^i	174.9 (7)	C9^i—O3—Ni1'	139.1 (9)
O7—Ni1'—O4^i	100.79 (19)	C5—O3—Ni1'	117.2 (8)
O6—Ni1'—O4^i	94.3 (2)	C4—O3—Ni1'	126.8 (8)
O3^i—Ni1'—O4^i	76.6 (6)	C8^i—O3—Ni1'	103.9 (7)
O3—Ni1'—O4^i	84.6 (5)	O5^i—O3—Ni1	98 (4)
O5—Ni1'—O4^i	70.3 (5)	C9^i—O3—Ni1	128.7 (9)
O5^i—Ni1'—O4^i	78.2 (6)	C5—O3—Ni1	127.6 (8)
Ni1—Ni1'—O4	174.9 (7)	C4—O3—Ni1	116.3 (7)
O7—Ni1'—O4	100.79 (19)	C8^i—O3—Ni1	114.3 (8)
O6—Ni1'—O4	94.3 (2)	O4^i—O4—C7^i	136.0 (8)
O3^i—Ni1'—O4	84.6 (5)	C7^i—O4—C7	100.4 (11)
O3—Ni1'—O4	76.6 (6)	O4^i—O4—C6	151.6 (6)
O5—Ni1'—O4	78.2 (6)	C7—O4—C6	116.0 (5)
O5^i—Ni1'—O4	70.3 (5)	C7^i—O4—C6^i	112.4 (6)
O4^i—Ni1'—O4	8.0 (9)	C6—O4—C6^i	127.9 (9)
Ni1—Ni1'—O2	30.8 (2)	O4^i—O4—Ni1'	86.0 (5)
O7—Ni1'—O2	80.8 (4)	C7^i—O4—Ni1'	119.8 (10)
O6—Ni1'—O2	86.2 (4)	C7—O4—Ni1'	108.5 (10)
O3^i—Ni1'—O2	130.0 (4)	C6—O4—Ni1'	110.1 (9)
O3—Ni1'—O2	68.7 (4)	C6^i—O4—Ni1'	100.0 (7)
O5—Ni1'—O2	136.0 (4)	O3^i—O5—C5^i	109 (4)
O5^i—Ni1'—O2	75.4 (4)	O3^i—O5—C9	49 (4)
O4^i—Ni1'—O2	153.4 (5)	C5^i—O5—C9	100.7 (10)
O4—Ni1'—O2	145.4 (5)	O3^i—O5—C8	120 (4)
Ni1—Ni1'—O2^i	30.8 (2)	C9—O5—C8	117.8 (10)
O7—Ni1'—O2^i	80.8 (4)	O3^i—O5—C4^i	45 (4)
O6—Ni1'—O2^i	86.2 (4)	C5^i—O5—C4^i	110.4 (12)
O3^i—Ni1'—O2^i	68.7 (3)	C8—O5—C4^i	127.5 (11)
O3—Ni1'—O2^i	130.0 (4)	O3^i—O5—Ni1'	79 (4)
O5—Ni1'—O2^i	75.4 (4)	C5^i—O5—Ni1'	124.0 (11)
O5^i—Ni1'—O2^i	136.0 (4)	C9—O5—Ni1'	120.7 (8)
O4^i—Ni1'—O2^i	145.4 (5)	C8—O5—Ni1'	110.6 (9)
O4—Ni1'—O2^i	153.4 (5)	C4^i—O5—Ni1'	112.3 (7)
O2—Ni1'—O2^i	61.3 (4)	O3^i—O5—Ni1	73 (4)
O1—C1—C2	106.8 (8)	C5^i—O5—Ni1	132.7 (11)
O1—C1—H1A	110.4	C9—O5—Ni1	111.6 (7)
C2—C1—H1A	110.4	C8—O5—Ni1	120.2 (9)
O1—C1—H1B	110.4	C4^i—O5—Ni1	102.9 (7)
C2—C1—H1B	110.4	Ni1—O6—H6	127 (3)
H1A—C1—H1B	108.6	Ni1'—O6—H6	126 (3)
O2—C2—C1	106.8 (9)	Ni1—O7—H7	125 (2)
O2—C2—H2A	110.4	Ni1'—O7—H7	123 (2)
C1—C2—H2A	110.4	O8—S1—O10	115.6 (4)
O2—C2—H2B	110.4	O8—S1—O9	112.8 (3)
C1—C2—H2B	110.4	O10—S1—O9	114.0 (6)
H2A—C2—H2B	108.6	O8—S1—O11	104.3 (5)
O2—C3—C4	110.4 (8)	O10—S1—O11	102.9 (4)
O2—C3—H3A	109.6	O9—S1—O11	105.7 (3)
C4—C3—H3A	109.6	O8'—S1'—O10'	103.3 (8)
O2—C3—H3B	109.6	O8'—S1'—O9'	112.6 (8)
C4—C3—H3B	109.6	O10'—S1'—O9'	118.2 (7)
H3A—C3—H3B	108.1	O8'—S1'—O11'	106.2 (6)
O3—C4—C3	110.2 (9)	O10'—S1'—O11'	107.3 (9)
O3—C4—H4A	109.6	O9'—S1'—O11'	108.5 (6)
C3—C4—H4A	109.6	S1'—O11'—H11'	109.5
O3—C4—H4B	109.6
O6—Ni1—Ni1'—O7	180.0	Ni1—Ni1'—O3—C4	−2.3 (14)
O2—Ni1—Ni1'—O7	84.9 (13)	O7—Ni1'—O3—C4	−84.8 (10)
O2^i—Ni1—Ni1'—O7	−84.9 (13)	O6—Ni1'—O3—C4	80.3 (11)
O1^i—Ni1—Ni1'—O7	94.7 (11)	O3^i—Ni1'—O3—C4	174.6 (14)
O1—Ni1—Ni1'—O7	−94.7 (11)	O5—Ni1'—O3—C4	−167.9 (11)
O3^i—Ni1—Ni1'—O7	−90.5 (4)	O5^i—Ni1'—O3—C4	−136 (4)
O3—Ni1—Ni1'—O7	90.5 (4)	O4^i—Ni1'—O3—C4	174.5 (11)
O5—Ni1—Ni1'—O7	−82.9 (4)	O4—Ni1'—O3—C4	174.5 (11)
O5^i—Ni1—Ni1'—O7	82.9 (4)	O2—Ni1'—O3—C4	−5.4 (10)
O7—Ni1—Ni1'—O6	180.0	O2^i—Ni1'—O3—C4	−5.4 (13)
O2—Ni1—Ni1'—O6	−95.1 (13)	Ni1—Ni1'—O3—C8^i	−178.7 (11)
O2^i—Ni1—Ni1'—O6	95.1 (13)	O7—Ni1'—O3—C8^i	98.8 (8)
O1^i—Ni1—Ni1'—O6	−85.3 (11)	O6—Ni1'—O3—C8^i	−96.1 (8)
O1—Ni1—Ni1'—O6	85.3 (11)	O3^i—Ni1'—O3—C8^i	−2 (2)
O3^i—Ni1—Ni1'—O6	89.5 (4)	O5—Ni1'—O3—C8^i	15.7 (10)
O3—Ni1—Ni1'—O6	−89.5 (4)	O5^i—Ni1'—O3—C8^i	48 (3)
O5—Ni1—Ni1'—O6	97.1 (4)	O4^i—Ni1'—O3—C8^i	−1.9 (8)
O5^i—Ni1—Ni1'—O6	−97.1 (4)	O4—Ni1'—O3—C8^i	−1.9 (7)
O7—Ni1—Ni1'—O3^i	90.5 (4)	O2—Ni1'—O3—C8^i	178.3 (9)
O6—Ni1—Ni1'—O3^i	−89.5 (4)	O2^i—Ni1'—O3—C8^i	178.3 (8)
O2—Ni1—Ni1'—O3^i	175.4 (12)	O7—Ni1'—O3—Ni1	−82.5 (8)
O2^i—Ni1—Ni1'—O3^i	5.6 (16)	O6—Ni1'—O3—Ni1	82.6 (8)
O1^i—Ni1—Ni1'—O3^i	−174.8 (10)	O3^i—Ni1'—O3—Ni1	177 (2)
O1—Ni1—Ni1'—O3^i	−4.2 (14)	O5—Ni1'—O3—Ni1	−165.6 (13)
O3—Ni1—Ni1'—O3^i	−179.0 (8)	O5^i—Ni1'—O3—Ni1	−133 (4)
O5—Ni1—Ni1'—O3^i	7.6 (6)	O4^i—Ni1'—O3—Ni1	176.8 (9)
O5^i—Ni1—Ni1'—O3^i	173.4 (6)	O4—Ni1'—O3—Ni1	176.8 (9)
O7—Ni1—Ni1'—O3	−90.5 (4)	O2—Ni1'—O3—Ni1	−3.1 (9)
O6—Ni1—Ni1'—O3	89.5 (4)	O2^i—Ni1'—O3—Ni1	−3.0 (8)
O2—Ni1—Ni1'—O3	−5.6 (16)	Ni1'—Ni1—O3—O5^i	−47 (4)
O2^i—Ni1—Ni1'—O3	−175.4 (12)	O7—Ni1—O3—O5^i	39 (4)
O1^i—Ni1—Ni1'—O3	4.2 (14)	O6—Ni1—O3—O5^i	−134 (4)
O1—Ni1—Ni1'—O3	174.8 (10)	O2—Ni1—O3—O5^i	129 (4)
O3^i—Ni1—Ni1'—O3	179.0 (8)	O2^i—Ni1—O3—O5^i	128 (4)
O5—Ni1—Ni1'—O3	−173.4 (6)	O1^i—Ni1—O3—O5^i	136 (4)
O5^i—Ni1—Ni1'—O3	−7.6 (6)	O1—Ni1—O3—O5^i	140 (3)
O7—Ni1—Ni1'—O5	82.9 (4)	O3^i—Ni1—O3—O5^i	−49 (4)
O6—Ni1—Ni1'—O5	−97.1 (4)	O5—Ni1—O3—O5^i	−39 (4)
O2—Ni1—Ni1'—O5	167.8 (11)	Ni1'—Ni1—O3—C9^i	176.3 (15)
O2^i—Ni1—Ni1'—O5	−2.0 (17)	O7—Ni1—O3—C9^i	−97.3 (12)
O1^i—Ni1—Ni1'—O5	177.6 (9)	O6—Ni1—O3—C9^i	89.9 (12)
O1—Ni1—Ni1'—O5	−11.8 (15)	O2—Ni1—O3—C9^i	−7.1 (12)
O3^i—Ni1—Ni1'—O5	−7.6 (6)	O2^i—Ni1—O3—C9^i	−8.5 (17)
O3—Ni1—Ni1'—O5	173.4 (6)	O1^i—Ni1—O3—C9^i	−0.6 (12)
O5^i—Ni1—Ni1'—O5	165.8 (9)	O1—Ni1—O3—C9^i	3.6 (19)
O7—Ni1—Ni1'—O5^i	−82.9 (4)	O3^i—Ni1—O3—C9^i	174.9 (8)
O6—Ni1—Ni1'—O5^i	97.1 (4)	O5—Ni1—O3—C9^i	−175.5 (13)
O2—Ni1—Ni1'—O5^i	2.0 (17)	O5^i—Ni1—O3—C9^i	−136 (5)
O2^i—Ni1—Ni1'—O5^i	−167.8 (11)	Ni1'—Ni1—O3—C5	6.8 (12)
O1^i—Ni1—Ni1'—O5^i	11.8 (15)	O7—Ni1—O3—C5	93.1 (8)
O1—Ni1—Ni1'—O5^i	−177.6 (9)	O6—Ni1—O3—C5	−79.7 (9)
O3^i—Ni1—Ni1'—O5^i	−173.4 (6)	O2—Ni1—O3—C5	−176.6 (10)
O3—Ni1—Ni1'—O5^i	7.6 (6)	O2^i—Ni1—O3—C5	−178.1 (9)
O5—Ni1—Ni1'—O5^i	−165.8 (9)	O1^i—Ni1—O3—C5	−170.2 (10)
O7—Ni1—Ni1'—O2	−84.9 (13)	O1—Ni1—O3—C5	−165.9 (10)
O6—Ni1—Ni1'—O2	95.1 (13)	O3^i—Ni1—O3—C5	5.3 (15)
O2^i—Ni1—Ni1'—O2	−170 (3)	O5—Ni1—O3—C5	15.0 (8)
O3^i—Ni1—Ni1'—O2	−175.4 (12)	O5^i—Ni1—O3—C5	54 (3)
O3—Ni1—Ni1'—O2	5.6 (16)	Ni1'—Ni1—O3—C4	177.9 (13)
O5—Ni1—Ni1'—O2	−167.8 (11)	O7—Ni1—O3—C4	−95.8 (9)
O5^i—Ni1—Ni1'—O2	−2.0 (17)	O6—Ni1—O3—C4	91.5 (9)
O7—Ni1—Ni1'—O2^i	84.9 (13)	O2—Ni1—O3—C4	−5.5 (9)
O6—Ni1—Ni1'—O2^i	−95.1 (13)	O2^i—Ni1—O3—C4	−6.9 (14)
O2—Ni1—Ni1'—O2^i	170 (3)	O1^i—Ni1—O3—C4	1.0 (9)
O3^i—Ni1—Ni1'—O2^i	−5.6 (16)	O1—Ni1—O3—C4	5.2 (16)
O3—Ni1—Ni1'—O2^i	175.4 (12)	O3^i—Ni1—O3—C4	176.4 (7)
O5—Ni1—Ni1'—O2^i	2.0 (17)	O5—Ni1—O3—C4	−173.9 (9)
O5^i—Ni1—Ni1'—O2^i	167.8 (11)	O5^i—Ni1—O3—C4	−135 (4)
O1—C1—C2—O2	−57.2 (11)	Ni1'—Ni1—O3—C8^i	1.4 (12)
O2—C3—C4—O3	30.5 (15)	O7—Ni1—O3—C8^i	87.7 (9)
O3—C5—C6—O4	47.4 (12)	O6—Ni1—O3—C8^i	−85.1 (9)
O4—C7—C8—O5	−58.5 (15)	O2—Ni1—O3—C8^i	178.0 (10)
O5—C9—C10—O1	54.5 (11)	O2^i—Ni1—O3—C8^i	176.5 (9)
C9—C10—O1—O2^i	−124 (4)	O1^i—Ni1—O3—C8^i	−175.5 (10)
C9—C10—O1—C3^i	78.4 (10)	O1—Ni1—O3—C8^i	−171.3 (10)
C9—C10—O1—C1	−170.6 (9)	O3^i—Ni1—O3—C8^i	−0.1 (15)
C9—C10—O1—C2^i	169.3 (12)	O5—Ni1—O3—C8^i	9.6 (8)
C9—C10—O1—Ni1	−45.2 (10)	O5^i—Ni1—O3—C8^i	49 (3)
C2—C1—O1—O2^i	83 (6)	O7—Ni1—O3—Ni1'	86.3 (9)
C2—C1—O1—C3^i	−140.4 (12)	O6—Ni1—O3—Ni1'	−86.5 (9)
C2—C1—O1—C10	176.3 (8)	O2—Ni1—O3—Ni1'	176.5 (10)
C2—C1—O1—C2^i	−38.4 (10)	O2^i—Ni1—O3—Ni1'	175.1 (12)
C2—C1—O1—Ni1	47.3 (9)	O1^i—Ni1—O3—Ni1'	−177.0 (10)
Ni1'—Ni1—O1—O2^i	135 (4)	O1—Ni1—O3—Ni1'	−172.7 (14)
O7—Ni1—O1—O2^i	44 (4)	O3^i—Ni1—O3—Ni1'	−1.5 (11)
O6—Ni1—O1—O2^i	−141 (4)	O5—Ni1—O3—Ni1'	8.2 (8)
O2—Ni1—O1—O2^i	−45 (4)	O5^i—Ni1—O3—Ni1'	47 (4)
O1^i—Ni1—O1—O2^i	−52 (5)	C8—C7—O4—O4^i	−6.0 (6)
O3^i—Ni1—O1—O2^i	130 (4)	C8—C7—O4—C7^i	174.0 (6)
O3—Ni1—O1—O2^i	−56 (5)	C8—C7—O4—C6	172.1 (13)
O5—Ni1—O1—O2^i	124 (4)	C8—C7—O4—C6^i	1 (5)
O5^i—Ni1—O1—O2^i	−40 (5)	C8—C7—O4—Ni1'	47.6 (13)
Ni1'—Ni1—O1—C3^i	−12 (2)	C5—C6—O4—O4^i	−167.2 (6)
O7—Ni1—O1—C3^i	−103.0 (13)	C5—C6—O4—C7^i	−177 (6)
O6—Ni1—O1—C3^i	71.9 (13)	C5—C6—O4—C7	−169.6 (13)
O2—Ni1—O1—C3^i	168.2 (17)	C5—C6—O4—C6^i	−167.2 (6)
O2^i—Ni1—O1—C3^i	−147 (5)	C5—C6—O4—Ni1'	−45.9 (11)
O1^i—Ni1—O1—C3^i	161.7 (10)	O7—Ni1'—O4—O4^i	90.77 (9)
O3^i—Ni1—O1—C3^i	−16.3 (12)	O6—Ni1'—O4—O4^i	−90.30 (4)
O3—Ni1—O1—C3^i	157.7 (10)	O3^i—Ni1'—O4—O4^i	0.0 (3)
O5—Ni1—O1—C3^i	−23.0 (13)	O3—Ni1'—O4—O4^i	180.0 (3)
O5^i—Ni1—O1—C3^i	173.6 (10)	O5—Ni1'—O4—O4^i	7.9 (3)
Ni1'—Ni1—O1—C10	30.3 (18)	O5^i—Ni1'—O4—O4^i	171.8 (3)
O7—Ni1—O1—C10	−60.7 (8)	O2—Ni1'—O4—O4^i	−179.8 (7)
O6—Ni1—O1—C10	114.1 (8)	O2^i—Ni1'—O4—O4^i	−0.3 (9)
O2—Ni1—O1—C10	−149.5 (12)	O7—Ni1'—O4—C7^i	−51.5 (11)
O2^i—Ni1—O1—C10	−104 (5)	O6—Ni1'—O4—C7^i	127.4 (10)
O1^i—Ni1—O1—C10	−156.1 (5)	O3^i—Ni1'—O4—C7^i	−142.3 (11)
O3^i—Ni1—O1—C10	26.0 (7)	O3—Ni1'—O4—C7^i	37.7 (11)
O3—Ni1—O1—C10	−160.1 (7)	O5—Ni1'—O4—C7^i	−134.5 (11)
O5—Ni1—O1—C10	19.3 (8)	O5^i—Ni1'—O4—C7^i	29.5 (11)
O5^i—Ni1—O1—C10	−144.1 (9)	O4^i—Ni1'—O4—C7^i	−142.3 (11)
Ni1'—Ni1—O1—C1	159.5 (13)	O2—Ni1'—O4—C7^i	37.9 (13)
O7—Ni1—O1—C1	68.5 (8)	O2^i—Ni1'—O4—C7^i	−142.6 (13)
O6—Ni1—O1—C1	−116.6 (8)	O7—Ni1'—O4—C7	62.7 (9)
O2—Ni1—O1—C1	−20.3 (5)	O6—Ni1'—O4—C7	−118.3 (8)
O2^i—Ni1—O1—C1	25 (4)	O3^i—Ni1'—O4—C7	−28.0 (9)
O1^i—Ni1—O1—C1	−26.8 (11)	O3—Ni1'—O4—C7	151.9 (9)
O3^i—Ni1—O1—C1	155.2 (10)	O5—Ni1'—O4—C7	−20.2 (9)
O3—Ni1—O1—C1	−30.8 (16)	O5^i—Ni1'—O4—C7	143.8 (9)
O5—Ni1—O1—C1	148.5 (9)	O4^i—Ni1'—O4—C7	−28.0 (8)
O5^i—Ni1—O1—C1	−14.9 (18)	O2—Ni1'—O4—C7	152.2 (10)
Ni1'—Ni1—O1—C2^i	−174.3 (13)	O2^i—Ni1'—O4—C7	−28.3 (12)
O7—Ni1—O1—C2^i	94.7 (7)	O7—Ni1'—O4—C6	−65.2 (8)
O6—Ni1—O1—C2^i	−90.4 (7)	O6—Ni1'—O4—C6	113.8 (7)
O2—Ni1—O1—C2^i	5.9 (4)	O3^i—Ni1'—O4—C6	−155.9 (8)
O2^i—Ni1—O1—C2^i	51 (4)	O3—Ni1'—O4—C6	24.0 (8)
O1^i—Ni1—O1—C2^i	−0.6 (10)	O5—Ni1'—O4—C6	−148.1 (8)
O3^i—Ni1—O1—C2^i	−178.6 (9)	O5^i—Ni1'—O4—C6	15.9 (8)
O3—Ni1—O1—C2^i	−4.6 (15)	O4^i—Ni1'—O4—C6	−155.9 (8)
O5—Ni1—O1—C2^i	174.7 (9)	O2—Ni1'—O4—C6	24.3 (10)
O5^i—Ni1—O1—C2^i	11.3 (18)	O2^i—Ni1'—O4—C6	−156.2 (11)
C4—C3—O2—O1^i	−92 (7)	O7—Ni1'—O4—C6^i	71.6 (5)
C4—C3—O2—C1^i	151.4 (11)	O6—Ni1'—O4—C6^i	−109.4 (5)
C4—C3—O2—C2	−177.3 (10)	O3^i—Ni1'—O4—C6^i	−19.1 (6)
C4—C3—O2—C10^i	49.8 (8)	O3—Ni1'—O4—C6^i	160.8 (6)
C4—C3—O2—Ni1	−38.7 (13)	O5—Ni1'—O4—C6^i	−11.3 (6)
C4—C3—O2—Ni1'	−35.6 (12)	O5^i—Ni1'—O4—C6^i	152.7 (6)
C1—C2—O2—O1^i	150 (5)	O4^i—Ni1'—O4—C6^i	−19.1 (5)
C1—C2—O2—C1^i	−75.9 (16)	O2—Ni1'—O4—C6^i	161.1 (8)
C1—C2—O2—C3	−179.5 (10)	O2^i—Ni1'—O4—C6^i	−19.4 (10)
C1—C2—O2—C10^i	−144.1 (12)	C10—C9—O5—O3^i	−78 (5)
C1—C2—O2—Ni1	39.7 (10)	C10—C9—O5—C5^i	176.2 (11)
C1—C2—O2—Ni1'	40.9 (11)	C10—C9—O5—C8	175.9 (11)
Ni1'—Ni1—O2—O1^i	53 (5)	C10—C9—O5—C4^i	−12 (5)
O7—Ni1—O2—O1^i	137 (4)	C10—C9—O5—Ni1'	−43.1 (12)
O6—Ni1—O2—O1^i	−39 (4)	C10—C9—O5—Ni1	−39.0 (11)
O2^i—Ni1—O2—O1^i	−133 (4)	C7—C8—O5—O3^i	129 (5)
O1—Ni1—O2—O1^i	−127 (5)	C7—C8—O5—C5^i	−176 (5)
O3^i—Ni1—O2—O1^i	−135 (4)	C7—C8—O5—C9	−174.8 (11)
O3—Ni1—O2—O1^i	47 (4)	C7—C8—O5—C4^i	−176.5 (13)
O5—Ni1—O2—O1^i	−150 (4)	C7—C8—O5—Ni1'	40.4 (12)
O5^i—Ni1—O2—O1^i	55 (4)	C7—C8—O5—Ni1	43.2 (13)
Ni1'—Ni1—O2—C1^i	−160.6 (15)	Ni1—Ni1'—O5—O3^i	48 (4)
O7—Ni1—O2—C1^i	−76.9 (10)	O7—Ni1'—O5—O3^i	129 (4)
O6—Ni1—O2—C1^i	107.7 (10)	O6—Ni1'—O5—O3^i	−36 (4)
O2^i—Ni1—O2—C1^i	13.1 (13)	O3—Ni1'—O5—O3^i	−146 (4)
O1^i—Ni1—O2—C1^i	146 (5)	O5^i—Ni1'—O5—O3^i	−156 (3)
O1—Ni1—O2—C1^i	19.2 (7)	O4^i—Ni1'—O5—O3^i	−128 (4)
O3^i—Ni1—O2—C1^i	11.7 (16)	O4—Ni1'—O5—O3^i	−129 (4)
O3—Ni1—O2—C1^i	−166.1 (12)	O2—Ni1'—O5—O3^i	57 (4)
O5—Ni1—O2—C1^i	−3.6 (17)	O2^i—Ni1'—O5—O3^i	47 (4)
O5^i—Ni1—O2—C1^i	−158.7 (11)	Ni1—Ni1'—O5—C5^i	153.9 (12)
Ni1'—Ni1—O2—C3	30 (2)	O7—Ni1'—O5—C5^i	−125.5 (10)
O7—Ni1—O2—C3	113.7 (9)	O6—Ni1'—O5—C5^i	69.1 (10)
O6—Ni1—O2—C3	−61.8 (9)	O3^i—Ni1'—O5—C5^i	106 (4)
O2^i—Ni1—O2—C3	−156.3 (7)	O3—Ni1'—O5—C5^i	−40.9 (12)
O1^i—Ni1—O2—C3	−23 (4)	O5^i—Ni1'—O5—C5^i	−50.2 (17)
O1—Ni1—O2—C3	−150.3 (13)	O4^i—Ni1'—O5—C5^i	−22.3 (9)
O3^i—Ni1—O2—C3	−157.8 (7)	O4—Ni1'—O5—C5^i	−23.4 (9)
O3—Ni1—O2—C3	24.5 (9)	O2—Ni1'—O5—C5^i	162.8 (9)
O5—Ni1—O2—C3	−173.1 (7)	O2^i—Ni1'—O5—C5^i	152.8 (11)
O5^i—Ni1—O2—C3	31.8 (9)	Ni1—Ni1'—O5—C9	22.5 (13)
Ni1'—Ni1—O2—C2	169.4 (15)	O7—Ni1'—O5—C9	103.1 (9)
O7—Ni1—O2—C2	−106.9 (8)	O6—Ni1'—O5—C9	−62.3 (10)
O6—Ni1—O2—C2	77.6 (8)	O3^i—Ni1'—O5—C9	−26 (3)
O2^i—Ni1—O2—C2	−16.9 (11)	O3—Ni1'—O5—C9	−172.3 (11)
O1^i—Ni1—O2—C2	116 (5)	O5^i—Ni1'—O5—C9	178.4 (7)
O1—Ni1—O2—C2	−10.9 (5)	O4^i—Ni1'—O5—C9	−153.7 (10)
O3^i—Ni1—O2—C2	−18.4 (14)	O4—Ni1'—O5—C9	−154.8 (10)
O3—Ni1—O2—C2	163.9 (10)	O2—Ni1'—O5—C9	31.4 (13)
O5—Ni1—O2—C2	−33.7 (15)	O2^i—Ni1'—O5—C9	21.4 (9)
O5^i—Ni1—O2—C2	171.2 (9)	Ni1—Ni1'—O5—C8	166.0 (11)
Ni1'—Ni1—O2—C10^i	−7.7 (19)	O7—Ni1'—O5—C8	−113.3 (7)
O7—Ni1—O2—C10^i	76.0 (7)	O6—Ni1'—O5—C8	81.3 (8)
O6—Ni1—O2—C10^i	−99.4 (7)	O3^i—Ni1'—O5—C8	118 (4)
O2^i—Ni1—O2—C10^i	166.0 (5)	O3—Ni1'—O5—C8	−28.8 (10)
O1^i—Ni1—O2—C10^i	−61 (4)	O5^i—Ni1'—O5—C8	−38.1 (15)
O1—Ni1—O2—C10^i	172.1 (12)	O4^i—Ni1'—O5—C8	−10.1 (7)
O3^i—Ni1—O2—C10^i	164.6 (6)	O4—Ni1'—O5—C8	−11.3 (7)
O3—Ni1—O2—C10^i	−13.1 (7)	O2—Ni1'—O5—C8	175.0 (8)
O5—Ni1—O2—C10^i	149.3 (6)	O2^i—Ni1'—O5—C8	165.0 (8)
O5^i—Ni1—O2—C10^i	−5.8 (7)	Ni1—Ni1'—O5—C4^i	17.0 (13)
O7—Ni1—O2—Ni1'	83.7 (15)	O7—Ni1'—O5—C4^i	97.7 (8)
O6—Ni1—O2—Ni1'	−91.7 (15)	O6—Ni1'—O5—C4^i	−67.7 (9)
O2^i—Ni1—O2—Ni1'	173.7 (17)	O3^i—Ni1'—O5—C4^i	−31 (3)
O1^i—Ni1—O2—Ni1'	−53 (5)	O3—Ni1'—O5—C4^i	−177.8 (10)
O1—Ni1—O2—Ni1'	179.8 (15)	O5^i—Ni1'—O5—C4^i	172.9 (8)
O3^i—Ni1—O2—Ni1'	172 (2)	O4^i—Ni1'—O5—C4^i	−159.1 (9)
O3—Ni1—O2—Ni1'	−5.5 (16)	O4—Ni1'—O5—C4^i	−160.3 (9)
O5—Ni1—O2—Ni1'	157 (2)	O2—Ni1'—O5—C4^i	26.0 (12)
O5^i—Ni1—O2—Ni1'	1.9 (15)	O2^i—Ni1'—O5—C4^i	16.0 (8)
Ni1—Ni1'—O2—O1^i	−128 (5)	O7—Ni1'—O5—Ni1	80.6 (9)
O7—Ni1'—O2—O1^i	142 (4)	O6—Ni1'—O5—Ni1	−84.8 (9)
O6—Ni1'—O2—O1^i	−46 (4)	O3^i—Ni1'—O5—Ni1	−48 (4)
O3^i—Ni1'—O2—O1^i	−134 (4)	O3—Ni1'—O5—Ni1	165.2 (13)
O3—Ni1'—O2—O1^i	46 (4)	O5^i—Ni1'—O5—Ni1	155.9 (16)
O5—Ni1'—O2—O1^i	−145 (4)	O4^i—Ni1'—O5—Ni1	−176.2 (9)
O5^i—Ni1'—O2—O1^i	54 (4)	O4—Ni1'—O5—Ni1	−177.3 (10)
O4^i—Ni1'—O2—O1^i	46 (5)	O2—Ni1'—O5—Ni1	8.9 (8)
O4—Ni1'—O2—O1^i	46 (5)	O2^i—Ni1'—O5—Ni1	−1.1 (9)
O2^i—Ni1'—O2—O1^i	−134 (4)	Ni1'—Ni1—O5—O3^i	−130 (4)
Ni1—Ni1'—O2—C1^i	20.8 (16)	O7—Ni1—O5—O3^i	140 (4)
O7—Ni1'—O2—C1^i	−69.6 (11)	O6—Ni1—O5—O3^i	−46 (4)
O6—Ni1'—O2—C1^i	102.6 (11)	O2—Ni1—O5—O3^i	65 (4)
O3^i—Ni1'—O2—C1^i	14.9 (14)	O2^i—Ni1—O5—O3^i	49 (4)
O3—Ni1'—O2—C1^i	−165.1 (13)	O1^i—Ni1—O5—O3^i	54 (4)
O5—Ni1'—O2—C1^i	3.8 (15)	O1—Ni1—O5—O3^i	42 (4)
O5^i—Ni1'—O2—C1^i	−157.2 (12)	O3—Ni1—O5—O3^i	−138 (4)
O4^i—Ni1'—O2—C1^i	−165.4 (7)	O5^i—Ni1—O5—O3^i	−146 (3)
O4—Ni1'—O2—C1^i	−165.4 (8)	Ni1'—Ni1—O5—C5^i	−29.8 (14)
O2^i—Ni1'—O2—C1^i	14.9 (13)	O7—Ni1—O5—C5^i	−119.5 (11)
Ni1—Ni1'—O2—C3	−151.4 (19)	O6—Ni1—O5—C5^i	53.6 (11)
O7—Ni1'—O2—C3	118.2 (9)	O2—Ni1—O5—C5^i	165.2 (11)
O6—Ni1'—O2—C3	−69.6 (9)	O2^i—Ni1—O5—C5^i	149.0 (12)
O3^i—Ni1'—O2—C3	−157.3 (8)	O1^i—Ni1—O5—C5^i	154.4 (13)
O3—Ni1'—O2—C3	22.7 (8)	O1—Ni1—O5—C5^i	142.1 (12)
O5—Ni1'—O2—C3	−168.4 (7)	O3^i—Ni1—O5—C5^i	100 (4)
O5^i—Ni1'—O2—C3	30.6 (8)	O3—Ni1—O5—C5^i	−38.4 (11)
O4^i—Ni1'—O2—C3	22.4 (15)	O5^i—Ni1—O5—C5^i	−45.6 (15)
O4—Ni1'—O2—C3	22.4 (13)	Ni1'—Ni1—O5—C9	−159.3 (12)
O2^i—Ni1'—O2—C3	−157.3 (7)	O7—Ni1—O5—C9	111.0 (8)
Ni1—Ni1'—O2—C2	−11.2 (16)	O6—Ni1—O5—C9	−76.0 (8)
O7—Ni1'—O2—C2	−101.6 (9)	O2—Ni1—O5—C9	35.7 (14)
O6—Ni1'—O2—C2	70.7 (9)	O2^i—Ni1—O5—C9	19.5 (9)
O3^i—Ni1'—O2—C2	−17.1 (12)	O1^i—Ni1—O5—C9	24.9 (17)
O3—Ni1'—O2—C2	162.9 (11)	O1—Ni1—O5—C9	12.6 (9)
O5—Ni1'—O2—C2	−28.1 (13)	O3^i—Ni1—O5—C9	−29 (3)
O5^i—Ni1'—O2—C2	170.8 (10)	O3—Ni1—O5—C9	−167.9 (9)
O4^i—Ni1'—O2—C2	162.6 (6)	O5^i—Ni1—O5—C9	−175.1 (6)
O4—Ni1'—O2—C2	162.7 (6)	Ni1'—Ni1—O5—C8	−15.1 (12)
O2^i—Ni1'—O2—C2	−17.1 (11)	O7—Ni1—O5—C8	−104.9 (8)
Ni1—Ni1'—O2—C10^i	172.6 (18)	O6—Ni1—O5—C8	68.2 (8)
O7—Ni1'—O2—C10^i	82.2 (7)	O2—Ni1—O5—C8	179.9 (10)
O6—Ni1'—O2—C10^i	−105.5 (7)	O2^i—Ni1—O5—C8	163.6 (9)
O3^i—Ni1'—O2—C10^i	166.7 (6)	O1^i—Ni1—O5—C8	169.0 (13)
O3—Ni1'—O2—C10^i	−13.3 (6)	O1—Ni1—O5—C8	156.7 (9)
O5—Ni1'—O2—C10^i	155.7 (6)	O3^i—Ni1—O5—C8	115 (4)
O5^i—Ni1'—O2—C10^i	−5.4 (7)	O3—Ni1—O5—C8	−23.7 (8)
O4^i—Ni1'—O2—C10^i	−13.6 (14)	O5^i—Ni1—O5—C8	−31.0 (12)
O4—Ni1'—O2—C10^i	−13.5 (12)	Ni1'—Ni1—O5—C4^i	−163.9 (12)
O2^i—Ni1'—O2—C10^i	166.7 (5)	O7—Ni1—O5—C4^i	106.4 (8)
O7—Ni1'—O2—Ni1	−90.4 (15)	O6—Ni1—O5—C4^i	−80.5 (8)
O6—Ni1'—O2—Ni1	81.8 (15)	O2—Ni1—O5—C4^i	31.1 (13)
O3^i—Ni1'—O2—Ni1	−5.9 (15)	O2^i—Ni1—O5—C4^i	14.9 (8)
O3—Ni1'—O2—Ni1	174.1 (17)	O1^i—Ni1—O5—C4^i	20.3 (17)
O5—Ni1'—O2—Ni1	−16.9 (15)	O1—Ni1—O5—C4^i	8.0 (8)
O5^i—Ni1'—O2—Ni1	−178.0 (17)	O3^i—Ni1—O5—C4^i	−34 (3)
O4^i—Ni1'—O2—Ni1	173.8 (18)	O3—Ni1—O5—C4^i	−172.5 (8)
O4—Ni1'—O2—Ni1	173.9 (17)	O5^i—Ni1—O5—C4^i	−179.7 (5)
O2^i—Ni1'—O2—Ni1	−5.9 (16)	O7—Ni1—O5—Ni1'	−89.7 (9)
C6—C5—O3—O5^i	44 (5)	O6—Ni1—O5—Ni1'	83.3 (9)
C6—C5—O3—C9^i	159.0 (11)	O2—Ni1—O5—Ni1'	−165.0 (13)
C6—C5—O3—C4	159.4 (11)	O2^i—Ni1—O5—Ni1'	178.8 (10)
C6—C5—O3—C8^i	−9 (4)	O1^i—Ni1—O5—Ni1'	−175.8 (16)
C6—C5—O3—Ni1'	−28.0 (11)	O1—Ni1—O5—Ni1'	171.9 (10)
C6—C5—O3—Ni1	−29.4 (12)	O3^i—Ni1—O5—Ni1'	130 (4)
C3—C4—O3—O5^i	−134 (5)	O3—Ni1—O5—Ni1'	−8.6 (8)
C3—C4—O3—C9^i	162 (7)	O5^i—Ni1—O5—Ni1'	−15.9 (10)
C3—C4—O3—C5	160.3 (9)	O2—Ni1—O6—Ni1'	143.4 (2)
C3—C4—O3—C8^i	164.0 (12)	O2^i—Ni1—O6—Ni1'	−143.4 (2)
C3—C4—O3—Ni1'	−11.5 (16)	O1^i—Ni1—O6—Ni1'	138.3 (3)
C3—C4—O3—Ni1	−11.9 (14)	O1—Ni1—O6—Ni1'	−138.3 (3)
Ni1—Ni1'—O3—O5^i	133 (4)	O3^i—Ni1—O6—Ni1'	−70.2 (3)
O7—Ni1'—O3—O5^i	51 (4)	O3—Ni1—O6—Ni1'	70.2 (3)
O6—Ni1'—O3—O5^i	−144 (4)	O5—Ni1—O6—Ni1'	−63.5 (3)
O3^i—Ni1'—O3—O5^i	−50 (5)	O5^i—Ni1—O6—Ni1'	63.5 (3)
O5—Ni1'—O3—O5^i	−32 (4)	O3^i—Ni1'—O6—Ni1	99.3 (3)
O4^i—Ni1'—O3—O5^i	−50 (4)	O3—Ni1'—O6—Ni1	−99.3 (3)
O4—Ni1'—O3—O5^i	−50 (4)	O5—Ni1'—O6—Ni1	105.3 (3)
O2—Ni1'—O3—O5^i	130 (4)	O5^i—Ni1'—O6—Ni1	−105.3 (3)
O2^i—Ni1'—O3—O5^i	130 (4)	O4^i—Ni1'—O6—Ni1	176.0 (5)
Ni1—Ni1'—O3—C9^i	−4.4 (19)	O4—Ni1'—O6—Ni1	−176.0 (5)
O7—Ni1'—O3—C9^i	−86.9 (15)	O2—Ni1'—O6—Ni1	−30.7 (2)
O6—Ni1'—O3—C9^i	78.2 (16)	O2^i—Ni1'—O6—Ni1	30.7 (2)
O3^i—Ni1'—O3—C9^i	172.5 (12)	O2—Ni1—O7—Ni1'	−143.7 (2)
O5—Ni1'—O3—C9^i	−170.0 (16)	O2^i—Ni1—O7—Ni1'	143.7 (2)
O5^i—Ni1'—O3—C9^i	−138 (5)	O1^i—Ni1—O7—Ni1'	−138.0 (3)
O4^i—Ni1'—O3—C9^i	172.4 (16)	O1—Ni1—O7—Ni1'	138.0 (3)
O4—Ni1'—O3—C9^i	172.4 (16)	O3^i—Ni1—O7—Ni1'	70.2 (3)
O2—Ni1'—O3—C9^i	−7.4 (15)	O3—Ni1—O7—Ni1'	−70.2 (3)
O2^i—Ni1'—O3—C9^i	−7.4 (18)	O5—Ni1—O7—Ni1'	64.3 (3)
Ni1—Ni1'—O3—C5	−173.9 (11)	O5^i—Ni1—O7—Ni1'	−64.3 (3)
O7—Ni1'—O3—C5	103.5 (7)	O6—Ni1'—O7—Ni1	0.000 (4)
O6—Ni1'—O3—C5	−91.4 (7)	O3^i—Ni1'—O7—Ni1	−99.2 (3)
O3^i—Ni1'—O3—C5	3 (2)	O3—Ni1'—O7—Ni1	99.2 (3)
O5—Ni1'—O3—C5	20.4 (9)	O5—Ni1'—O7—Ni1	−107.0 (3)
O5^i—Ni1'—O3—C5	53 (3)	O5^i—Ni1'—O7—Ni1	107.0 (3)
O4^i—Ni1'—O3—C5	2.9 (7)	O4^i—Ni1'—O7—Ni1	−175.9 (5)
O4—Ni1'—O3—C5	2.9 (7)	O4—Ni1'—O7—Ni1	175.9 (5)
O2—Ni1'—O3—C5	−177.0 (9)	O2—Ni1'—O7—Ni1	31.1 (2)
O2^i—Ni1'—O3—C5	−177.0 (8)	O2^i—Ni1'—O7—Ni1	−31.1 (2)

Symmetry code: (i) −x+1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6···O8^i	0.77 (2)	1.91 (2)	2.667 (3)	168 (4)
O6—H6···O8′^i	0.77 (2)	2.02 (2)	2.743 (4)	157 (4)
O7—H7···O9^ii	0.80 (2)	1.89 (2)	2.650 (3)	159 (3)
O7—H7···O8′^ii	0.80 (2)	2.06 (2)	2.767 (5)	149 (3)
O11—H11···O10^iii	0.82	1.82	2.581 (8)	153
O11—H11···O10′^iii	0.82	1.82	2.619 (14)	164

Symmetry codes: (i) −x+1, y, z; (ii) x, −y+1, z+1/2; (iii) −x+1/2, y+1/2, z.

'diaqua(15-crown-5)nickel(II) hydrogen sulfate' (II)

Crystal data

C10H24NiO7·2(HO4S)	F(000) = 1064
Mr = 509.14	Dx = 1.727 Mg m^−3
Orthorhombic, Pbc21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2b	Cell parameters from 7007 reflections
a = 17.7219 (5) Å	θ = 1.8–27.5°
b = 7.5069 (3) Å	µ = 1.28 mm^−1
c = 14.7170 (4) Å	T = 210 K
V = 1957.90 (11) Å^3	Tabular, yellow
Z = 4	0.34 × 0.14 × 0.12 mm

Data collection

Nonius KappaCCD diffractometer	4460 independent reflections
Radiation source: rotating anode	3394 reflections with I > 2sσ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	h = −22→22
Tmin = 0.76, Tmax = 0.86	k = −9→9
15576 measured reflections	l = −18→19

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.026	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.069	w = 1/[σ^2(Fo^2) + (0.026P)^2 + 0.7333P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.001
4460 reflections	Δρmax = 0.37 e Å^−3
476 parameters	Δρmin = −0.26 e Å^−3
668 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.004 (11)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
O6	0.25112 (10)	0.7895 (4)	0.23526 (17)	0.0473 (6)
H6W1	0.2871 (14)	0.836 (5)	0.214 (3)	0.071*
H6W2	0.2135 (14)	0.837 (5)	0.216 (3)	0.071*
O7	0.24987 (10)	0.5280 (3)	0.47065 (14)	0.0371 (5)
H7W1	0.2861 (13)	0.508 (5)	0.500 (2)	0.056*
H7W2	0.2112 (13)	0.497 (4)	0.495 (2)	0.056*
Ni1	0.25080 (7)	0.64310 (17)	0.34863 (6)	0.01851 (18)	0.689 (3)
O1	0.3308 (3)	0.4735 (8)	0.2903 (5)	0.0417 (12)	0.689 (3)
O2	0.1799 (3)	0.4454 (6)	0.2953 (5)	0.0375 (10)	0.689 (3)
O3	0.1366 (3)	0.7319 (7)	0.3721 (3)	0.0293 (10)	0.689 (3)
O4	0.2430 (3)	0.9427 (7)	0.4273 (4)	0.0331 (11)	0.689 (3)
O5	0.3609 (3)	0.7402 (10)	0.3972 (4)	0.0364 (11)	0.689 (3)
C1	0.2968 (3)	0.3063 (7)	0.2770 (5)	0.0554 (13)	0.689 (3)
H1A	0.2936	0.2426	0.3350	0.066*	0.689 (3)
H1B	0.3273	0.2349	0.2351	0.066*	0.689 (3)
C2	0.2225 (4)	0.3308 (7)	0.2402 (4)	0.0527 (13)	0.689 (3)
H2A	0.2263	0.3809	0.1789	0.063*	0.689 (3)
H2B	0.1970	0.2152	0.2357	0.063*	0.689 (3)
C3	0.1120 (3)	0.5052 (7)	0.2653 (4)	0.0484 (11)	0.689 (3)
H3A	0.0785	0.4040	0.2533	0.058*	0.689 (3)
H3B	0.1186	0.5714	0.2085	0.058*	0.689 (3)
C4	0.0782 (3)	0.6219 (8)	0.3348 (5)	0.0379 (12)	0.689 (3)
H4A	0.0388	0.6964	0.3074	0.045*	0.689 (3)
H4B	0.0551	0.5499	0.3829	0.045*	0.689 (3)
C5	0.1129 (3)	0.8957 (8)	0.4110 (4)	0.0357 (12)	0.689 (3)
H5A	0.0645	0.8806	0.4421	0.043*	0.689 (3)
H5B	0.1070	0.9865	0.3637	0.043*	0.689 (3)
C6	0.1727 (4)	0.9504 (9)	0.4771 (5)	0.0394 (13)	0.689 (3)
H6A	0.1633	1.0714	0.4993	0.047*	0.689 (3)
H6B	0.1739	0.8689	0.5291	0.047*	0.689 (3)
C7	0.3083 (3)	0.9663 (11)	0.4836 (6)	0.0436 (14)	0.689 (3)
H7A	0.3058	0.8882	0.5368	0.052*	0.689 (3)
H7B	0.3120	1.0901	0.5044	0.052*	0.689 (3)
C8	0.3736 (4)	0.9198 (11)	0.4265 (7)	0.0482 (15)	0.689 (3)
H8A	0.3770	1.0001	0.3741	0.058*	0.689 (3)
H8B	0.4205	0.9281	0.4614	0.058*	0.689 (3)
C9	0.4234 (3)	0.6655 (8)	0.3460 (5)	0.0433 (13)	0.689 (3)
H9A	0.4704	0.6728	0.3810	0.052*	0.689 (3)
H9B	0.4302	0.7291	0.2884	0.052*	0.689 (3)
C10	0.4023 (3)	0.4780 (7)	0.3296 (4)	0.0490 (11)	0.689 (3)
H10A	0.4390	0.4219	0.2890	0.059*	0.689 (3)
H10B	0.4019	0.4122	0.3871	0.059*	0.689 (3)
Ni1'	0.25060 (19)	0.6901 (3)	0.36243 (15)	0.01851 (18)	0.311 (3)
O1'	0.1709 (6)	0.4939 (15)	0.2984 (12)	0.0360 (19)	0.311 (3)
O2'	0.3135 (6)	0.4546 (18)	0.3019 (11)	0.0360 (18)	0.311 (3)
O3'	0.3659 (7)	0.735 (2)	0.3742 (10)	0.0300 (19)	0.311 (3)
O4'	0.2617 (6)	0.9624 (16)	0.4394 (11)	0.0335 (18)	0.311 (3)
O5'	0.1375 (6)	0.7617 (16)	0.3990 (8)	0.0312 (18)	0.311 (3)
C1'	0.1986 (6)	0.3143 (14)	0.2823 (9)	0.0438 (19)	0.311 (3)
H1'1	0.1644	0.2492	0.2418	0.053*	0.311 (3)
H1'2	0.2030	0.2486	0.3396	0.053*	0.311 (3)
C2'	0.2724 (7)	0.3374 (16)	0.2401 (9)	0.0414 (19)	0.311 (3)
H2'1	0.2675	0.3920	0.1799	0.050*	0.311 (3)
H2'2	0.2982	0.2226	0.2338	0.050*	0.311 (3)
C3'	0.3856 (5)	0.4981 (13)	0.2654 (7)	0.0350 (17)	0.311 (3)
H3'1	0.3813	0.5704	0.2102	0.042*	0.311 (3)
H3'2	0.4154	0.3911	0.2523	0.042*	0.311 (3)
C4'	0.4187 (8)	0.6035 (17)	0.3434 (11)	0.034 (2)	0.311 (3)
H4'1	0.4313	0.5228	0.3935	0.041*	0.311 (3)
H4'2	0.4653	0.6623	0.3235	0.041*	0.311 (3)
C5'	0.3916 (8)	0.888 (2)	0.4170 (14)	0.035 (2)	0.311 (3)
H5'1	0.4021	0.9793	0.3713	0.042*	0.311 (3)
H5'2	0.4387	0.8614	0.4491	0.042*	0.311 (3)
C6'	0.3347 (7)	0.956 (3)	0.4831 (13)	0.040 (2)	0.311 (3)
H6'1	0.3326	0.8783	0.5364	0.048*	0.311 (3)
H6'2	0.3491	1.0760	0.5034	0.048*	0.311 (3)
C7'	0.1954 (7)	0.982 (2)	0.4878 (12)	0.036 (2)	0.311 (3)
H7'1	0.1913	1.1053	0.5093	0.043*	0.311 (3)
H7'2	0.1965	0.9039	0.5411	0.043*	0.311 (3)
C8'	0.1291 (8)	0.9383 (18)	0.4312 (12)	0.038 (2)	0.311 (3)
H8'1	0.0828	0.9486	0.4673	0.046*	0.311 (3)
H8'2	0.1256	1.0212	0.3799	0.046*	0.311 (3)
C9'	0.0778 (7)	0.6844 (15)	0.3467 (11)	0.033 (2)	0.311 (3)
H9'1	0.0734	0.7454	0.2881	0.040*	0.311 (3)
H9'2	0.0297	0.6966	0.3791	0.040*	0.311 (3)
C10'	0.0960 (5)	0.4883 (12)	0.3321 (7)	0.0314 (16)	0.311 (3)
H10C	0.0932	0.4215	0.3892	0.038*	0.311 (3)
H10D	0.0616	0.4344	0.2877	0.038*	0.311 (3)
S1_1	0.07993 (15)	1.0299 (3)	0.11067 (15)	0.0224 (2)	0.882 (3)
O8_1	0.12121 (16)	0.9271 (4)	0.1748 (2)	0.0585 (9)	0.882 (3)
O9_1	0.12521 (13)	1.1162 (3)	0.04162 (19)	0.0415 (7)	0.882 (3)
O10_1	0.0291 (2)	0.9015 (6)	0.0553 (2)	0.0521 (10)	0.882 (3)
O11_1	0.03006 (15)	1.1527 (3)	0.15493 (19)	0.0457 (7)	0.882 (3)
H11_1	−0.0074	1.1703	0.1224	0.069*	0.882 (3)
S1'_1	0.0769 (12)	1.031 (2)	0.1200 (14)	0.0224 (2)	0.118 (3)
O8'_1	0.1485 (9)	0.9337 (17)	0.1152 (13)	0.028 (3)	0.118 (3)
O9'_1	0.0578 (9)	1.0492 (19)	0.2170 (11)	0.033 (4)	0.118 (3)
O10'_1	0.0162 (18)	0.926 (5)	0.076 (2)	0.0521 (10)	0.118 (3)
O11'_1	0.0845 (8)	1.2049 (19)	0.0763 (13)	0.033 (4)	0.118 (3)
H11'_1	0.0499	1.2713	0.0935	0.050*	0.118 (3)
S2_2	0.4218 (7)	1.0189 (14)	0.1109 (7)	0.0235 (5)	0.536 (4)
O8_2	0.3834 (2)	0.9151 (6)	0.1782 (3)	0.0529 (13)	0.536 (4)
O9_2	0.3720 (2)	1.1081 (5)	0.0473 (3)	0.0393 (11)	0.536 (4)
O10_2	0.4715 (8)	0.909 (3)	0.0561 (14)	0.035 (2)	0.536 (4)
O11_2	0.4645 (2)	1.1600 (5)	0.1632 (3)	0.0411 (11)	0.536 (4)
H11_2	0.5051	1.1812	0.1373	0.062*	0.536 (4)
S2'_2	0.4225 (8)	1.0055 (17)	0.1171 (8)	0.0235 (5)	0.464 (4)
O8'_2	0.3486 (2)	0.9292 (5)	0.1108 (4)	0.0337 (10)	0.464 (4)
O9'_2	0.4450 (3)	1.0404 (6)	0.2109 (3)	0.0398 (12)	0.464 (4)
O10'_2	0.4857 (10)	0.920 (4)	0.0708 (17)	0.035 (2)	0.464 (4)
O11'_2	0.4119 (3)	1.1914 (5)	0.0708 (4)	0.0392 (12)	0.464 (4)
H11'_2	0.4491	1.2550	0.0818	0.059*	0.464 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O6	0.0233 (10)	0.0779 (17)	0.0406 (12)	0.0039 (11)	0.0014 (11)	0.0379 (12)
O7	0.0196 (9)	0.0629 (14)	0.0287 (11)	−0.0044 (10)	−0.0021 (9)	0.0227 (9)
Ni1	0.02021 (14)	0.0181 (5)	0.0172 (3)	0.0011 (4)	0.0000 (3)	0.0004 (3)
O1	0.031 (2)	0.057 (2)	0.037 (2)	0.0182 (17)	0.007 (2)	−0.0012 (18)
O2	0.0427 (18)	0.033 (2)	0.0365 (19)	−0.0068 (15)	0.0044 (16)	−0.015 (2)
O3	0.0189 (14)	0.031 (2)	0.038 (3)	0.0034 (13)	−0.0024 (17)	−0.0097 (15)
O4	0.044 (2)	0.0288 (18)	0.027 (2)	−0.0163 (16)	−0.0108 (17)	−0.0102 (13)
O5	0.0182 (16)	0.0490 (18)	0.042 (3)	−0.0076 (14)	0.0017 (18)	0.0196 (19)
C1	0.064 (3)	0.042 (2)	0.060 (3)	0.018 (2)	0.012 (3)	−0.006 (2)
C2	0.065 (3)	0.042 (2)	0.051 (3)	0.001 (2)	0.005 (3)	−0.019 (2)
C3	0.042 (2)	0.052 (2)	0.051 (3)	−0.0121 (18)	−0.013 (2)	−0.008 (2)
C4	0.0173 (18)	0.059 (3)	0.037 (3)	−0.010 (2)	−0.0069 (18)	0.000 (3)
C5	0.031 (3)	0.039 (3)	0.038 (3)	0.016 (2)	0.005 (2)	−0.004 (2)
C6	0.054 (3)	0.028 (3)	0.036 (3)	0.005 (2)	0.002 (3)	−0.0131 (19)
C7	0.049 (3)	0.044 (3)	0.038 (2)	−0.029 (3)	−0.018 (3)	−0.005 (2)
C8	0.037 (3)	0.059 (3)	0.048 (3)	−0.028 (3)	−0.015 (3)	0.008 (3)
C9	0.0149 (18)	0.071 (3)	0.044 (3)	−0.001 (2)	0.005 (2)	0.027 (3)
C10	0.029 (2)	0.062 (3)	0.056 (3)	0.0207 (19)	0.012 (2)	0.017 (2)
Ni1'	0.02021 (14)	0.0181 (5)	0.0172 (3)	0.0011 (4)	0.0000 (3)	0.0004 (3)
O1'	0.030 (3)	0.037 (4)	0.040 (4)	−0.014 (3)	−0.002 (3)	−0.018 (4)
O2'	0.026 (3)	0.050 (3)	0.032 (4)	0.010 (3)	0.007 (3)	−0.015 (3)
O3'	0.019 (3)	0.039 (3)	0.033 (5)	−0.007 (2)	0.008 (3)	0.006 (3)
O4'	0.041 (4)	0.025 (3)	0.034 (4)	−0.007 (3)	−0.008 (3)	−0.011 (3)
O5'	0.017 (3)	0.039 (4)	0.037 (5)	0.010 (2)	−0.004 (3)	−0.010 (3)
C1'	0.052 (4)	0.039 (4)	0.040 (4)	−0.011 (3)	0.003 (4)	−0.019 (4)
C2'	0.047 (4)	0.035 (4)	0.042 (4)	0.002 (3)	−0.002 (4)	−0.011 (3)
C3'	0.027 (3)	0.051 (4)	0.027 (4)	0.012 (3)	0.008 (3)	0.004 (3)
C4'	0.018 (3)	0.049 (4)	0.034 (4)	0.004 (3)	0.008 (3)	0.008 (4)
C5'	0.027 (4)	0.043 (4)	0.035 (4)	−0.013 (3)	−0.007 (4)	0.009 (3)
C6'	0.042 (5)	0.044 (4)	0.035 (4)	−0.015 (5)	−0.013 (4)	−0.004 (3)
C7'	0.050 (4)	0.023 (4)	0.035 (4)	0.011 (4)	−0.006 (4)	−0.014 (3)
C8'	0.037 (4)	0.035 (4)	0.043 (5)	0.017 (4)	0.000 (4)	−0.008 (4)
C9'	0.016 (3)	0.047 (4)	0.037 (5)	−0.001 (3)	−0.007 (4)	0.009 (4)
C10'	0.022 (3)	0.047 (3)	0.025 (4)	−0.019 (3)	−0.007 (3)	0.000 (3)
S1_1	0.0179 (4)	0.0212 (2)	0.0282 (7)	0.0021 (2)	0.0015 (4)	−0.0001 (6)
O8_1	0.0415 (16)	0.0581 (17)	0.076 (2)	0.0084 (13)	−0.0219 (16)	0.0279 (16)
O9_1	0.0377 (13)	0.0297 (11)	0.0569 (16)	0.0019 (10)	0.0247 (13)	0.0018 (11)
O10_1	0.064 (2)	0.0564 (18)	0.036 (2)	−0.0299 (16)	−0.0051 (16)	−0.0063 (14)
O11_1	0.0499 (16)	0.0431 (13)	0.0442 (16)	0.0230 (12)	0.0203 (12)	0.0067 (11)
S1'_1	0.0179 (4)	0.0212 (2)	0.0282 (7)	0.0021 (2)	0.0015 (4)	−0.0001 (6)
O8'_1	0.042 (5)	0.022 (6)	0.019 (8)	0.015 (5)	0.005 (6)	−0.001 (7)
O9'_1	0.043 (10)	0.030 (8)	0.027 (5)	−0.016 (7)	0.018 (6)	−0.014 (5)
O10'_1	0.064 (2)	0.0564 (18)	0.036 (2)	−0.0299 (16)	−0.0051 (16)	−0.0063 (14)
O11'_1	0.012 (6)	0.036 (5)	0.053 (8)	0.003 (4)	0.003 (6)	0.019 (6)
S2_2	0.0182 (3)	0.0231 (12)	0.0291 (10)	−0.0016 (7)	−0.0010 (6)	0.0056 (9)
O8_2	0.041 (3)	0.061 (3)	0.057 (3)	−0.013 (2)	0.014 (2)	0.024 (2)
O9_2	0.035 (2)	0.034 (2)	0.049 (3)	0.0028 (16)	−0.024 (2)	0.0015 (17)
O10_2	0.028 (5)	0.040 (3)	0.037 (6)	0.010 (4)	−0.003 (4)	0.000 (3)
O11_2	0.046 (2)	0.051 (2)	0.026 (2)	−0.0170 (18)	−0.0112 (18)	−0.0055 (18)
S2'_2	0.0182 (3)	0.0231 (12)	0.0291 (10)	−0.0016 (7)	−0.0010 (6)	0.0056 (9)
O8'_2	0.0262 (19)	0.044 (2)	0.031 (2)	−0.0136 (16)	−0.0010 (19)	0.007 (2)
O9'_2	0.040 (3)	0.052 (3)	0.027 (2)	−0.004 (2)	−0.0093 (19)	−0.004 (2)
O10'_2	0.028 (5)	0.040 (3)	0.037 (6)	0.010 (4)	−0.003 (4)	0.000 (3)
O11'_2	0.034 (3)	0.028 (2)	0.055 (3)	−0.0008 (18)	−0.011 (2)	0.0144 (19)

Geometric parameters (Å, º)

O6—Ni1	1.998 (2)	O1'—C1'	1.453 (12)
O6—Ni1'	2.015 (3)	O2'—C3'	1.425 (12)
O6—H6W1	0.79 (2)	O2'—C2'	1.460 (14)
O6—H6W2	0.81 (2)	O3'—C5'	1.386 (15)
O7—Ni1	1.993 (2)	O3'—C4'	1.432 (14)
O7—Ni1'	2.005 (3)	O4'—C7'	1.382 (15)
O7—H7W1	0.79 (2)	O4'—C6'	1.445 (13)
O7—H7W2	0.81 (2)	O5'—C8'	1.416 (13)
Ni1—O1	2.090 (5)	O5'—C9'	1.430 (13)
Ni1—O2	2.097 (5)	C1'—C2'	1.459 (13)
Ni1—O3	2.158 (5)	C1'—H1'1	0.9800
Ni1—O4	2.534 (4)	C1'—H1'2	0.9800
Ni1—O5	2.201 (6)	C2'—H2'1	0.9800
O1—C10	1.392 (7)	C2'—H2'2	0.9800
O1—C1	1.407 (7)	C3'—C4'	1.513 (15)
O2—C3	1.358 (7)	C3'—H3'1	0.9800
O2—C2	1.403 (7)	C3'—H3'2	0.9800
O3—C5	1.419 (6)	C4'—H4'1	0.9800
O3—C4	1.434 (6)	C4'—H4'2	0.9800
O4—C7	1.435 (6)	C5'—C6'	1.492 (15)
O4—C6	1.447 (7)	C5'—H5'1	0.9800
O5—C8	1.433 (8)	C5'—H5'2	0.9800
O5—C9	1.453 (8)	C6'—H6'1	0.9800
C1—C2	1.435 (8)	C6'—H6'2	0.9800
C1—H1A	0.9800	C7'—C8'	1.478 (14)
C1—H1B	0.9800	C7'—H7'1	0.9800
C2—H2A	0.9800	C7'—H7'2	0.9800
C2—H2B	0.9800	C8'—H8'1	0.9800
C3—C4	1.475 (8)	C8'—H8'2	0.9800
C3—H3A	0.9800	C9'—C10'	1.523 (12)
C3—H3B	0.9800	C9'—H9'1	0.9800
C4—H4A	0.9800	C9'—H9'2	0.9800
C4—H4B	0.9800	C10'—H10C	0.9800
C5—C6	1.496 (7)	C10'—H10D	0.9800
C5—H5A	0.9800	S1_1—O8_1	1.422 (3)
C5—H5B	0.9800	S1_1—O11_1	1.433 (3)
C6—H6A	0.9800	S1_1—O9_1	1.448 (3)
C6—H6B	0.9800	S1_1—O10_1	1.550 (3)
C7—C8	1.472 (9)	O11_1—H11_1	0.8300
C7—H7A	0.9800	S1'_1—O11'_1	1.461 (14)
C7—H7B	0.9800	S1'_1—O8'_1	1.466 (15)
C8—H8A	0.9800	S1'_1—O9'_1	1.473 (15)
C8—H8B	0.9800	S1'_1—O10'_1	1.484 (15)
C9—C10	1.477 (7)	O11'_1—H11'_1	0.8300
C9—H9A	0.9800	S2_2—O8_2	1.433 (11)
C9—H9B	0.9800	S2_2—O9_2	1.451 (10)
C10—H10A	0.9800	S2_2—O10_2	1.452 (11)
C10—H10B	0.9800	S2_2—O11_2	1.512 (10)
Ni1'—O3'	2.078 (13)	O11_2—H11_2	0.8300
Ni1'—O5'	2.144 (11)	S2'_2—O8'_2	1.431 (12)
Ni1'—O1'	2.248 (11)	S2'_2—O10'_2	1.458 (12)
Ni1'—O2'	2.272 (12)	S2'_2—O9'_2	1.461 (11)
Ni1'—O4'	2.345 (10)	S2'_2—O11'_2	1.564 (12)
O1'—C10'	1.418 (13)	O11'_2—H11'_2	0.8300
Ni1—O6—H6W1	125 (3)	O3'—Ni1'—O2'	71.1 (4)
Ni1'—O6—H6W1	122 (3)	O5'—Ni1'—O2'	138.8 (4)
Ni1—O6—H6W2	122 (3)	O1'—Ni1'—O2'	68.5 (3)
Ni1'—O6—H6W2	119 (3)	O7—Ni1'—O4'	98.4 (4)
H6W1—O6—H6W2	109 (3)	O6—Ni1'—O4'	97.2 (4)
Ni1—O7—H7W1	125 (2)	O3'—Ni1'—O4'	74.7 (4)
Ni1'—O7—H7W1	123 (2)	O5'—Ni1'—O4'	74.9 (4)
Ni1—O7—H7W2	122 (2)	O1'—Ni1'—O4'	145.8 (4)
Ni1'—O7—H7W2	122 (2)	O2'—Ni1'—O4'	145.7 (4)
H7W1—O7—H7W2	113 (4)	C10'—O1'—C1'	110.2 (10)
O7—Ni1—O6	172.33 (14)	C10'—O1'—Ni1'	117.5 (7)
O7—Ni1—O1	96.4 (2)	C1'—O1'—Ni1'	117.7 (8)
O6—Ni1—O1	89.4 (2)	C3'—O2'—C2'	110.5 (11)
O7—Ni1—O2	91.5 (2)	C3'—O2'—Ni1'	114.2 (8)
O6—Ni1—O2	94.5 (2)	C2'—O2'—Ni1'	117.9 (8)
O1—Ni1—O2	79.73 (19)	C5'—O3'—C4'	119.9 (11)
O7—Ni1—O3	88.99 (17)	C5'—O3'—Ni1'	119.6 (9)
O6—Ni1—O3	88.06 (17)	C4'—O3'—Ni1'	120.4 (9)
O1—Ni1—O3	152.87 (19)	C7'—O4'—C6'	122.3 (12)
O2—Ni1—O3	73.55 (17)	C7'—O4'—Ni1'	105.7 (7)
O7—Ni1—O5	81.9 (2)	C6'—O4'—Ni1'	105.3 (9)
O6—Ni1—O5	95.0 (2)	C8'—O5'—C9'	118.9 (10)
O1—Ni1—O5	74.6 (2)	C8'—O5'—Ni1'	114.6 (8)
O2—Ni1—O5	152.5 (2)	C9'—O5'—Ni1'	117.1 (7)
O3—Ni1—O5	132.57 (19)	O1'—C1'—C2'	105.2 (10)
C10—O1—C1	118.0 (6)	O1'—C1'—H1'1	110.7
C10—O1—Ni1	115.6 (4)	C2'—C1'—H1'1	110.7
C1—O1—Ni1	108.0 (3)	O1'—C1'—H1'2	110.7
C3—O2—C2	119.4 (6)	C2'—C1'—H1'2	110.7
C3—O2—Ni1	114.7 (3)	H1'1—C1'—H1'2	108.8
C2—O2—Ni1	109.2 (4)	C1'—C2'—O2'	104.7 (9)
C5—O3—C4	116.1 (4)	C1'—C2'—H2'1	110.8
C5—O3—Ni1	127.5 (3)	O2'—C2'—H2'1	110.8
C4—O3—Ni1	116.0 (3)	C1'—C2'—H2'2	110.8
C7—O4—C6	113.4 (5)	O2'—C2'—H2'2	110.8
C8—O5—C9	113.5 (5)	H2'1—C2'—H2'2	108.9
C8—O5—Ni1	123.3 (5)	O2'—C3'—C4'	100.5 (9)
C9—O5—Ni1	112.3 (4)	O2'—C3'—H3'1	111.7
O1—C1—C2	109.4 (5)	C4'—C3'—H3'1	111.7
O1—C1—H1A	109.8	O2'—C3'—H3'2	111.7
C2—C1—H1A	109.8	C4'—C3'—H3'2	111.7
O1—C1—H1B	109.8	H3'1—C3'—H3'2	109.4
C2—C1—H1B	109.8	O3'—C4'—C3'	110.3 (11)
H1A—C1—H1B	108.2	O3'—C4'—H4'1	109.6
O2—C2—C1	110.7 (5)	C3'—C4'—H4'1	109.6
O2—C2—H2A	109.5	O3'—C4'—H4'2	109.6
C1—C2—H2A	109.5	C3'—C4'—H4'2	109.6
O2—C2—H2B	109.5	H4'1—C4'—H4'2	108.1
C1—C2—H2B	109.5	O3'—C5'—C6'	111.2 (12)
H2A—C2—H2B	108.1	O3'—C5'—H5'1	109.4
O2—C3—C4	109.3 (5)	C6'—C5'—H5'1	109.4
O2—C3—H3A	109.8	O3'—C5'—H5'2	109.4
C4—C3—H3A	109.8	C6'—C5'—H5'2	109.4
O2—C3—H3B	109.8	H5'1—C5'—H5'2	108.0
C4—C3—H3B	109.8	O4'—C6'—C5'	109.0 (12)
H3A—C3—H3B	108.3	O4'—C6'—H6'1	109.9
O3—C4—C3	108.3 (4)	C5'—C6'—H6'1	109.9
O3—C4—H4A	110.0	O4'—C6'—H6'2	109.9
C3—C4—H4A	110.0	C5'—C6'—H6'2	109.9
O3—C4—H4B	110.0	H6'1—C6'—H6'2	108.3
C3—C4—H4B	110.0	O4'—C7'—C8'	111.2 (11)
H4A—C4—H4B	108.4	O4'—C7'—H7'1	109.4
O3—C5—C6	106.9 (4)	C8'—C7'—H7'1	109.4
O3—C5—H5A	110.3	O4'—C7'—H7'2	109.4
C6—C5—H5A	110.3	C8'—C7'—H7'2	109.4
O3—C5—H5B	110.3	H7'1—C7'—H7'2	108.0
C6—C5—H5B	110.3	O5'—C8'—C7'	108.3 (10)
H5A—C5—H5B	108.6	O5'—C8'—H8'1	110.0
O4—C6—C5	105.6 (5)	C7'—C8'—H8'1	110.0
O4—C6—H6A	110.6	O5'—C8'—H8'2	110.0
C5—C6—H6A	110.6	C7'—C8'—H8'2	110.0
O4—C6—H6B	110.6	H8'1—C8'—H8'2	108.4
C5—C6—H6B	110.6	O5'—C9'—C10'	108.2 (9)
H6A—C6—H6B	108.7	O5'—C9'—H9'1	110.1
O4—C7—C8	105.9 (5)	C10'—C9'—H9'1	110.1
O4—C7—H7A	110.6	O5'—C9'—H9'2	110.1
C8—C7—H7A	110.6	C10'—C9'—H9'2	110.1
O4—C7—H7B	110.6	H9'1—C9'—H9'2	108.4
C8—C7—H7B	110.6	O1'—C10'—C9'	102.7 (9)
H7A—C7—H7B	108.7	O1'—C10'—H10C	111.2
O5—C8—C7	105.7 (5)	C9'—C10'—H10C	111.2
O5—C8—H8A	110.6	O1'—C10'—H10D	111.2
C7—C8—H8A	110.6	C9'—C10'—H10D	111.2
O5—C8—H8B	110.6	H10C—C10'—H10D	109.1
C7—C8—H8B	110.6	O8_1—S1_1—O11_1	111.4 (2)
H8A—C8—H8B	108.7	O8_1—S1_1—O9_1	115.0 (2)
O5—C9—C10	105.0 (5)	O11_1—S1_1—O9_1	111.9 (2)
O5—C9—H9A	110.7	O8_1—S1_1—O10_1	108.1 (3)
C10—C9—H9A	110.7	O11_1—S1_1—O10_1	106.3 (2)
O5—C9—H9B	110.7	O9_1—S1_1—O10_1	103.4 (2)
C10—C9—H9B	110.7	O11'_1—S1'_1—O8'_1	110.2 (14)
H9A—C9—H9B	108.8	O11'_1—S1'_1—O9'_1	111.5 (15)
O1—C10—C9	108.8 (5)	O8'_1—S1'_1—O9'_1	107.0 (15)
O1—C10—H10A	109.9	O11'_1—S1'_1—O10'_1	111 (2)
C9—C10—H10A	109.9	O8'_1—S1'_1—O10'_1	109.9 (19)
O1—C10—H10B	109.9	O9'_1—S1'_1—O10'_1	107.7 (17)
C9—C10—H10B	109.9	S1'_1—O11'_1—H11'_1	109.5
H10A—C10—H10B	108.3	O8_2—S2_2—O9_2	114.0 (8)
O7—Ni1'—O6	164.33 (16)	O8_2—S2_2—O10_2	111.2 (13)
O7—Ni1'—O3'	92.2 (5)	O9_2—S2_2—O10_2	105.9 (10)
O6—Ni1'—O3'	90.8 (5)	O8_2—S2_2—O11_2	105.5 (7)
O7—Ni1'—O5'	87.0 (4)	O9_2—S2_2—O11_2	108.0 (7)
O6—Ni1'—O5'	98.3 (4)	O10_2—S2_2—O11_2	112.3 (9)
O3'—Ni1'—O5'	149.1 (4)	O8'_2—S2'_2—O10'_2	119.8 (12)
O7—Ni1'—O1'	86.0 (5)	O8'_2—S2'_2—O9'_2	112.5 (9)
O6—Ni1'—O1'	81.7 (5)	O10'_2—S2'_2—O9'_2	108.1 (12)
O3'—Ni1'—O1'	139.3 (4)	O8'_2—S2'_2—O11'_2	102.7 (8)
O5'—Ni1'—O1'	71.5 (4)	O10'_2—S2'_2—O11'_2	106.2 (15)
O7—Ni1'—O2'	80.9 (5)	O9'_2—S2'_2—O11'_2	106.5 (8)
O6—Ni1'—O2'	85.5 (5)	S2'_2—O11'_2—H11'_2	109.5
Ni1'—O7—Ni1—O1	137.5 (7)	O6—Ni1'—O1'—C10'	−117.5 (11)
Ni1'—O7—Ni1—O2	−142.7 (7)	O3'—Ni1'—O1'—C10'	161.0 (10)
Ni1'—O7—Ni1—O3	−69.2 (7)	O5'—Ni1'—O1'—C10'	−15.8 (10)
Ni1'—O7—Ni1—O5	64.1 (7)	O2'—Ni1'—O1'—C10'	154.1 (14)
Ni1'—O6—Ni1—O1	−137.8 (7)	O4'—Ni1'—O1'—C10'	−26.8 (19)
Ni1'—O6—Ni1—O2	142.6 (7)	O7—Ni1'—O1'—C1'	−63.1 (12)
Ni1'—O6—Ni1—O3	69.2 (7)	O6—Ni1'—O1'—C1'	107.0 (12)
Ni1'—O6—Ni1—O5	−63.3 (7)	O3'—Ni1'—O1'—C1'	25.6 (19)
O7—Ni1—O1—C10	−63.2 (5)	O5'—Ni1'—O1'—C1'	−151.3 (14)
O6—Ni1—O1—C10	111.8 (5)	O2'—Ni1'—O1'—C1'	18.6 (12)
O2—Ni1—O1—C10	−153.5 (6)	O4'—Ni1'—O1'—C1'	−162.3 (11)
O3—Ni1—O1—C10	−163.6 (4)	O7—Ni1'—O2'—C3'	−124.4 (11)
O5—Ni1—O1—C10	16.5 (5)	O6—Ni1'—O2'—C3'	63.4 (11)
O7—Ni1—O1—C1	71.5 (5)	O3'—Ni1'—O2'—C3'	−28.9 (11)
O6—Ni1—O1—C1	−113.5 (5)	O5'—Ni1'—O2'—C3'	160.9 (9)
O2—Ni1—O1—C1	−18.8 (5)	O1'—Ni1'—O2'—C3'	146.3 (14)
O3—Ni1—O1—C1	−28.8 (10)	O4'—Ni1'—O2'—C3'	−32.8 (19)
O5—Ni1—O1—C1	151.2 (6)	O7—Ni1'—O2'—C2'	103.2 (12)
O7—Ni1—O2—C3	117.4 (5)	O6—Ni1'—O2'—C2'	−68.9 (12)
O6—Ni1—O2—C3	−57.7 (5)	O3'—Ni1'—O2'—C2'	−161.3 (14)
O1—Ni1—O2—C3	−146.3 (6)	O5'—Ni1'—O2'—C2'	28.5 (18)
O3—Ni1—O2—C3	28.9 (5)	O1'—Ni1'—O2'—C2'	13.9 (11)
O5—Ni1—O2—C3	−167.5 (5)	O4'—Ni1'—O2'—C2'	−165.2 (11)
O7—Ni1—O2—C2	−105.4 (5)	O7—Ni1'—O3'—C5'	−98.3 (14)
O6—Ni1—O2—C2	79.4 (5)	O6—Ni1'—O3'—C5'	97.1 (14)
O1—Ni1—O2—C2	−9.2 (5)	O5'—Ni1'—O3'—C5'	−11 (2)
O3—Ni1—O2—C2	166.1 (6)	O1'—Ni1'—O3'—C5'	175.3 (13)
O5—Ni1—O2—C2	−30.3 (10)	O2'—Ni1'—O3'—C5'	−177.9 (16)
O7—Ni1—O3—C5	91.5 (5)	O4'—Ni1'—O3'—C5'	−0.2 (14)
O6—Ni1—O3—C5	−81.4 (5)	O7—Ni1'—O3'—C4'	77.9 (13)
O1—Ni1—O3—C5	−166.4 (6)	O6—Ni1'—O3'—C4'	−86.7 (13)
O2—Ni1—O3—C5	−176.7 (6)	O5'—Ni1'—O3'—C4'	165.6 (11)
O5—Ni1—O3—C5	13.5 (7)	O1'—Ni1'—O3'—C4'	−8.5 (19)
O7—Ni1—O3—C4	−96.2 (4)	O2'—Ni1'—O3'—C4'	−1.7 (13)
O6—Ni1—O3—C4	90.9 (4)	O4'—Ni1'—O3'—C4'	176.0 (15)
O1—Ni1—O3—C4	5.9 (8)	O7—Ni1'—O4'—C7'	−65.9 (10)
O2—Ni1—O3—C4	−4.4 (5)	O6—Ni1'—O4'—C7'	115.4 (10)
O5—Ni1—O3—C4	−174.1 (4)	O3'—Ni1'—O4'—C7'	−155.8 (12)
O7—Ni1—O5—C8	−105.1 (6)	O5'—Ni1'—O4'—C7'	18.7 (10)
O6—Ni1—O5—C8	67.8 (6)	O1'—Ni1'—O4'—C7'	29.5 (17)
O1—Ni1—O5—C8	155.9 (7)	O2'—Ni1'—O4'—C7'	−152.0 (12)
O2—Ni1—O5—C8	177.5 (7)	O7—Ni1'—O4'—C6'	64.9 (11)
O3—Ni1—O5—C8	−24.1 (8)	O6—Ni1'—O4'—C6'	−113.9 (10)
O7—Ni1—O5—C9	113.1 (5)	O3'—Ni1'—O4'—C6'	−25.1 (11)
O6—Ni1—O5—C9	−73.9 (5)	O5'—Ni1'—O4'—C6'	149.4 (12)
O1—Ni1—O5—C9	14.1 (5)	O1'—Ni1'—O4'—C6'	160.2 (12)
O2—Ni1—O5—C9	35.8 (9)	O2'—Ni1'—O4'—C6'	−21.3 (17)
O3—Ni1—O5—C9	−165.8 (4)	O7—Ni1'—O5'—C8'	110.9 (10)
C10—O1—C1—C2	177.2 (5)	O6—Ni1'—O5'—C8'	−83.9 (10)
Ni1—O1—C1—C2	43.8 (7)	O3'—Ni1'—O5'—C8'	21.7 (18)
C3—O2—C2—C1	170.7 (6)	O1'—Ni1'—O5'—C8'	−162.3 (12)
Ni1—O2—C2—C1	35.9 (7)	O2'—Ni1'—O5'—C8'	−176.6 (11)
O1—C1—C2—O2	−54.4 (8)	O4'—Ni1'—O5'—C8'	11.3 (10)
C2—O2—C3—C4	179.7 (6)	O7—Ni1'—O5'—C9'	−103.0 (10)
Ni1—O2—C3—C4	−47.8 (7)	O6—Ni1'—O5'—C9'	62.2 (10)
C5—O3—C4—C3	155.6 (5)	O3'—Ni1'—O5'—C9'	167.9 (12)
Ni1—O3—C4—C3	−17.6 (7)	O1'—Ni1'—O5'—C9'	−16.2 (10)
O2—C3—C4—O3	40.8 (7)	O2'—Ni1'—O5'—C9'	−30.5 (15)
C4—O3—C5—C6	156.9 (6)	O4'—Ni1'—O5'—C9'	157.5 (12)
Ni1—O3—C5—C6	−30.7 (7)	C10'—O1'—C1'—C2'	174.7 (11)
C7—O4—C6—C5	−171.5 (6)	Ni1'—O1'—C1'—C2'	−46.9 (15)
O3—C5—C6—O4	51.6 (6)	O1'—C1'—C2'—O2'	53.2 (15)
C6—O4—C7—C8	169.1 (6)	C3'—O2'—C2'—C1'	−176.1 (12)
C9—O5—C8—C7	−174.9 (7)	Ni1'—O2'—C2'—C1'	−42.2 (15)
Ni1—O5—C8—C7	43.8 (9)	C2'—O2'—C3'—C4'	−175.3 (12)
O4—C7—C8—O5	−57.9 (8)	Ni1'—O2'—C3'—C4'	48.9 (13)
C8—O5—C9—C10	175.1 (6)	C5'—O3'—C4'—C3'	−154.3 (14)
Ni1—O5—C9—C10	−39.2 (7)	Ni1'—O3'—C4'—C3'	29.5 (18)
C1—O1—C10—C9	−174.0 (6)	O2'—C3'—C4'—O3'	−48.5 (16)
Ni1—O1—C10—C9	−44.0 (7)	C4'—O3'—C5'—C6'	−150.8 (16)
O5—C9—C10—O1	52.8 (7)	Ni1'—O3'—C5'—C6'	25 (2)
Ni1—O7—Ni1'—O6	0.9 (3)	C7'—O4'—C6'—C5'	165.4 (13)
Ni1—O7—Ni1'—O3'	−99.7 (8)	Ni1'—O4'—C6'—C5'	45.0 (16)
Ni1—O7—Ni1'—O5'	111.2 (7)	O3'—C5'—C6'—O4'	−48 (2)
Ni1—O7—Ni1'—O1'	39.6 (7)	C6'—O4'—C7'—C8'	−165.4 (14)
Ni1—O7—Ni1'—O2'	−29.3 (7)	Ni1'—O4'—C7'—C8'	−45.3 (14)
Ni1—O7—Ni1'—O4'	−174.6 (8)	C9'—O5'—C8'—C7'	176.3 (13)
Ni1—O6—Ni1'—O7	−0.9 (3)	Ni1'—O5'—C8'—C7'	−38.3 (15)
Ni1—O6—Ni1'—O3'	99.9 (8)	O4'—C7'—C8'—O5'	57.5 (17)
Ni1—O6—Ni1'—O5'	−109.7 (7)	C8'—O5'—C9'—C10'	−172.3 (12)
Ni1—O6—Ni1'—O1'	−39.9 (7)	Ni1'—O5'—C9'—C10'	43.1 (14)
Ni1—O6—Ni1'—O2'	29.0 (7)	C1'—O1'—C10'—C9'	178.7 (12)
Ni1—O6—Ni1'—O4'	174.6 (8)	Ni1'—O1'—C10'—C9'	40.2 (13)
O7—Ni1'—O1'—C10'	72.3 (11)	O5'—C9'—C10'—O1'	−50.8 (14)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6W1···O8_2	0.79 (2)	1.88 (2)	2.663 (4)	168 (4)
O6—H6W1···O8′_2	0.79 (2)	2.00 (3)	2.728 (5)	154 (4)
O6—H6W2···O8_1	0.81 (2)	1.87 (2)	2.676 (3)	174 (3)
O6—H6W2···O8′_1	0.81 (2)	2.01 (3)	2.757 (16)	153 (4)
O7—H7W1···O9_2^i	0.79 (2)	1.89 (2)	2.645 (4)	161 (4)
O7—H7W1···O8′_2^i	0.79 (2)	2.02 (3)	2.724 (5)	148 (3)
O7—H7W2···O9_1^i	0.81 (2)	1.87 (2)	2.672 (3)	170 (4)
O7—H7W2···O8′_1^i	0.81 (2)	2.15 (4)	2.799 (18)	137 (3)
O11_1—H11_1···O10_1^ii	0.83	2.03	2.596 (5)	125
O11′_1—H11′_1···O10′_1^ii	0.83	1.67	2.44 (3)	153
O11_2—H11_2···O10_2^iii	0.83	2.12	2.69 (2)	126
O11′_2—H11′_2···O10′_2^iii	0.83	1.70	2.50 (2)	160

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) −x, y+1/2, z; (iii) −x+1, y+1/2, z.

'diaqua(15-crown-5)nickel(II) hydrogen sulfate' (III)

Crystal data

C10H24NiO7·2(HO4S)	F(000) = 2128
Mr = 509.14	Dx = 1.745 Mg m^−3
Orthorhombic, Pbn21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2ab	Cell parameters from 12771 reflections
a = 17.8198 (3) Å	θ = 2.3–27.5°
b = 14.8945 (1) Å	µ = 1.29 mm^−1
c = 14.6052 (7) Å	T = 110 K
V = 3876.5 (2) Å^3	Tabular, yellow
Z = 8	0.34 × 0.14 × 0.12 mm

Data collection

Nonius KappaCCD diffractometer	8722 independent reflections
Radiation source: rotating anode	5725 reflections with I > 2sσ(I)
Graphite monochromator	Rint = 0.032
φ and ω scans	θmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	h = −22→23
Tmin = 0.76, Tmax = 0.86	k = −19→19
35233 measured reflections	l = −18→18

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.031	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.071	w = 1/[σ^2(Fo^2) + (0.0256P)^2 + 0.7006P] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.001
8722 reflections	Δρmax = 0.55 e Å^−3
541 parameters	Δρmin = −0.42 e Å^−3
17 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.005 (9)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ni1_1	0.250859 (17)	0.31713 (3)	0.34322 (3)	0.00989 (12)
O1_1	0.33252 (11)	0.23676 (13)	0.28346 (13)	0.0133 (5)
O2_1	0.18515 (11)	0.21224 (13)	0.29518 (12)	0.0127 (5)
O3_1	0.13681 (11)	0.35711 (13)	0.36725 (14)	0.0138 (5)
O4_1	0.23764 (11)	0.47315 (16)	0.42259 (15)	0.0152 (5)
O5_1	0.35800 (12)	0.37425 (13)	0.39090 (14)	0.0139 (5)
O6_1	0.24525 (11)	0.38556 (17)	0.22520 (18)	0.0189 (6)
H6W1_1	0.2038 (12)	0.4109 (19)	0.214 (2)	0.028*
H6W2_1	0.2787 (12)	0.409 (2)	0.200 (2)	0.028*
O7_1	0.25539 (10)	0.25192 (18)	0.46247 (16)	0.0148 (6)
H7W1_1	0.2882 (12)	0.259 (2)	0.496 (2)	0.022*
H7W2_1	0.2147 (11)	0.238 (2)	0.488 (2)	0.022*
C1_1	0.30325 (17)	0.14645 (18)	0.2729 (2)	0.0189 (7)
H1A_1	0.3001	0.1160	0.3330	0.023*
H1B_1	0.3360	0.1106	0.2321	0.023*
C2_1	0.22707 (18)	0.1571 (2)	0.2320 (2)	0.0178 (7)
H2A_1	0.2304	0.1865	0.1713	0.021*
H2B_1	0.2026	0.0978	0.2244	0.021*
C3_1	0.11233 (15)	0.23950 (19)	0.26075 (19)	0.0149 (6)
H3A_1	0.0802	0.1864	0.2493	0.018*
H3B_1	0.1178	0.2735	0.2029	0.018*
C4_1	0.07868 (16)	0.29803 (19)	0.3345 (2)	0.0151 (7)
H4A_1	0.0364	0.3334	0.3094	0.018*
H4B_1	0.0595	0.2604	0.3853	0.018*
C5_1	0.10938 (17)	0.43745 (19)	0.4094 (2)	0.0152 (7)
H5A_1	0.0622	0.4251	0.4429	0.018*
H5B_1	0.0993	0.4838	0.3625	0.018*
C6_1	0.16895 (17)	0.4693 (2)	0.4746 (2)	0.0176 (7)
H6A_1	0.1561	0.5294	0.4989	0.021*
H6B_1	0.1741	0.4271	0.5265	0.021*
C7_1	0.30264 (17)	0.4902 (2)	0.4776 (2)	0.0179 (7)
H7A_1	0.3018	0.4528	0.5336	0.022*
H7B_1	0.3048	0.5542	0.4957	0.022*
C8_1	0.36851 (18)	0.4662 (2)	0.4187 (2)	0.0178 (7)
H8A_1	0.3708	0.5060	0.3645	0.021*
H8B_1	0.4158	0.4727	0.4537	0.021*
C9_1	0.42152 (16)	0.33754 (19)	0.3427 (2)	0.0167 (7)
H9A_1	0.4679	0.3447	0.3793	0.020*
H9B_1	0.4284	0.3684	0.2833	0.020*
C10_1	0.40461 (16)	0.24010 (19)	0.3280 (2)	0.0172 (7)
H10A_1	0.4435	0.2120	0.2890	0.021*
H10B_1	0.4029	0.2079	0.3873	0.021*
Ni2_2	0.254502 (18)	0.43221 (3)	0.84509 (3)	0.01270 (12)
O1_2	0.33311 (11)	0.51637 (13)	0.78679 (13)	0.0146 (5)
O2_2	0.18487 (11)	0.53779 (13)	0.79569 (13)	0.0150 (5)
O3_2	0.13838 (12)	0.39096 (13)	0.86732 (14)	0.0151 (5)
O4_2	0.24037 (11)	0.27884 (17)	0.92315 (16)	0.0169 (5)
O5_2	0.36090 (12)	0.37809 (13)	0.89288 (13)	0.0144 (5)
O6_2	0.25097 (10)	0.36411 (17)	0.72730 (18)	0.0196 (7)
H6W1_2	0.2907 (12)	0.343 (2)	0.700 (2)	0.029*
H6W2_2	0.2154 (12)	0.3324 (19)	0.710 (2)	0.029*
O7_2	0.25547 (10)	0.49821 (18)	0.96385 (16)	0.0149 (6)
H7W1_2	0.2855 (13)	0.483 (2)	1.0072 (19)	0.022*
H7W2_2	0.2142 (11)	0.505 (2)	0.987 (2)	0.022*
C1_2	0.30264 (17)	0.60515 (19)	0.7766 (2)	0.0201 (7)
H1A_2	0.3353	0.6422	0.7369	0.024*
H1B_2	0.2981	0.6349	0.8370	0.024*
C2_2	0.22667 (19)	0.5933 (2)	0.7337 (2)	0.0217 (7)
H2A_2	0.2017	0.6521	0.7256	0.026*
H2B_2	0.2312	0.5640	0.6731	0.026*
C3_2	0.11368 (15)	0.50696 (19)	0.75974 (19)	0.0163 (6)
H3A_2	0.1212	0.4714	0.7032	0.020*
H3B_2	0.0805	0.5584	0.7456	0.020*
C4_2	0.08054 (16)	0.4501 (2)	0.8337 (2)	0.0168 (7)
H4A_2	0.0616	0.4885	0.8840	0.020*
H4B_2	0.0381	0.4146	0.8092	0.020*
C5_2	0.11211 (18)	0.3110 (2)	0.9107 (2)	0.0182 (8)
H5A_2	0.1024	0.2637	0.8645	0.022*
H5B_2	0.0650	0.3230	0.9444	0.022*
C6_2	0.17254 (17)	0.2816 (2)	0.9754 (2)	0.0197 (8)
H6A_2	0.1773	0.3247	1.0267	0.024*
H6B_2	0.1609	0.2216	1.0008	0.024*
C7_2	0.30614 (18)	0.2616 (2)	0.9774 (2)	0.0202 (8)
H7A_2	0.3084	0.1974	0.9950	0.024*
H7B_2	0.3056	0.2985	1.0337	0.024*
C8_2	0.37207 (18)	0.2858 (2)	0.9187 (2)	0.0200 (8)
H8A_2	0.4195	0.2788	0.9533	0.024*
H8B_2	0.3741	0.2469	0.8637	0.024*
C9_2	0.42369 (16)	0.41787 (19)	0.8455 (2)	0.0188 (7)
H9A_2	0.4315	0.3881	0.7856	0.023*
H9B_2	0.4701	0.4117	0.8822	0.023*
C10_2	0.40480 (15)	0.51449 (19)	0.83220 (19)	0.0162 (6)
H10A_2	0.4019	0.5457	0.8920	0.019*
H10B_2	0.4434	0.5444	0.7942	0.019*
S1_3	0.07441 (4)	0.50174 (5)	0.10386 (5)	0.01118 (18)
O8_3	0.10831 (11)	0.44672 (13)	0.17337 (15)	0.0238 (5)
O9_3	0.12732 (11)	0.54713 (12)	0.04452 (14)	0.0202 (5)
O10_3	0.01760 (13)	0.45416 (13)	0.05085 (15)	0.0232 (6)
O11_3	0.03334 (11)	0.57611 (13)	0.15912 (13)	0.0187 (5)
H11_3	0.0191 (17)	0.6132 (19)	0.1195 (19)	0.028*
S2_4	0.42112 (4)	0.50473 (5)	0.11612 (5)	0.00978 (18)
O8_4	0.34690 (11)	0.46401 (12)	0.10966 (12)	0.0155 (4)
O9_4	0.44362 (10)	0.52305 (12)	0.20898 (13)	0.0172 (5)
O10_4	0.47675 (13)	0.45440 (13)	0.06450 (14)	0.0204 (5)
O11_4	0.41041 (12)	0.59605 (12)	0.06514 (14)	0.0172 (5)
H11_4	0.4463 (14)	0.6299 (18)	0.073 (2)	0.026*
S3_5	0.07877 (4)	0.24382 (5)	0.60611 (5)	0.01108 (18)
O8_5	0.11785 (11)	0.29505 (13)	0.67485 (15)	0.0239 (5)
O9_5	0.12695 (11)	0.19800 (13)	0.54147 (15)	0.0237 (5)
O10_5	0.02134 (12)	0.29662 (13)	0.55923 (14)	0.0194 (5)
O11_5	0.03798 (11)	0.17001 (13)	0.66194 (14)	0.0197 (5)
H11_5	0.0207 (16)	0.1368 (19)	0.6175 (18)	0.030*
S4_6	0.42329 (4)	0.25153 (5)	0.61055 (5)	0.01150 (18)
O8_6	0.35054 (11)	0.29546 (13)	0.60367 (14)	0.0212 (5)
O9_6	0.44724 (11)	0.23838 (14)	0.70365 (14)	0.0252 (5)
O10_6	0.47927 (12)	0.29407 (13)	0.55259 (15)	0.0208 (5)
O11_6	0.40774 (12)	0.15777 (13)	0.56734 (15)	0.0213 (5)
H11_6	0.4488 (14)	0.129 (2)	0.570 (2)	0.032*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1_1	0.0095 (2)	0.0107 (2)	0.0094 (3)	0.00037 (12)	0.00022 (13)	0.0011 (2)
O1_1	0.0083 (11)	0.0137 (11)	0.0179 (11)	0.0013 (9)	−0.0014 (9)	−0.0003 (9)
O2_1	0.0116 (11)	0.0131 (12)	0.0133 (11)	−0.0002 (9)	−0.0009 (9)	−0.0031 (8)
O3_1	0.0058 (11)	0.0140 (11)	0.0216 (12)	0.0002 (9)	0.0000 (9)	−0.0055 (9)
O4_1	0.0133 (11)	0.0162 (13)	0.0160 (12)	−0.0006 (9)	0.0017 (9)	−0.0009 (10)
O5_1	0.0081 (11)	0.0136 (11)	0.0201 (11)	−0.0028 (9)	0.0028 (9)	−0.0014 (9)
O6_1	0.0138 (15)	0.0239 (16)	0.0189 (15)	0.0016 (9)	0.0023 (9)	0.0125 (12)
O7_1	0.0093 (14)	0.0233 (15)	0.0118 (14)	−0.0032 (9)	−0.0037 (8)	0.0048 (11)
C1_1	0.0210 (18)	0.0094 (16)	0.0263 (17)	0.0028 (13)	0.0034 (15)	−0.0073 (14)
C2_1	0.0197 (17)	0.0130 (16)	0.0207 (18)	−0.0007 (16)	−0.0016 (16)	−0.0096 (14)
C3_1	0.0118 (16)	0.0183 (16)	0.0147 (16)	0.0023 (13)	−0.0039 (13)	−0.0012 (12)
C4_1	0.0096 (15)	0.0200 (17)	0.0156 (15)	−0.0032 (14)	−0.0038 (14)	−0.0021 (14)
C5_1	0.0120 (17)	0.0133 (17)	0.0202 (16)	0.0036 (14)	0.0041 (13)	−0.0035 (13)
C6_1	0.0194 (19)	0.0158 (17)	0.0177 (16)	0.0016 (14)	0.0035 (14)	−0.0048 (13)
C7_1	0.0237 (19)	0.0120 (16)	0.0181 (16)	−0.0066 (15)	−0.0037 (14)	−0.0030 (13)
C8_1	0.0148 (18)	0.0162 (17)	0.0226 (17)	−0.0077 (14)	−0.0015 (14)	−0.0009 (14)
C9_1	0.0073 (15)	0.0237 (18)	0.0190 (16)	0.0033 (13)	0.0032 (14)	0.0043 (15)
C10_1	0.0118 (16)	0.0190 (16)	0.0210 (17)	0.0051 (13)	−0.0001 (13)	0.0025 (14)
Ni2_2	0.0104 (2)	0.0168 (3)	0.0109 (3)	−0.00342 (14)	0.00181 (16)	−0.0046 (2)
O1_2	0.0120 (12)	0.0157 (11)	0.0160 (11)	−0.0029 (9)	0.0005 (9)	−0.0004 (9)
O2_2	0.0137 (12)	0.0154 (12)	0.0159 (11)	−0.0013 (9)	−0.0022 (9)	0.0033 (9)
O3_2	0.0110 (12)	0.0155 (12)	0.0187 (11)	−0.0012 (9)	0.0004 (9)	0.0019 (9)
O4_2	0.0166 (12)	0.0165 (13)	0.0176 (13)	−0.0008 (9)	−0.0002 (9)	0.0020 (11)
O5_2	0.0112 (12)	0.0154 (12)	0.0167 (11)	0.0011 (9)	0.0012 (9)	−0.0023 (9)
O6_2	0.0131 (15)	0.0278 (17)	0.0178 (16)	−0.0060 (9)	0.0014 (8)	−0.0140 (12)
O7_2	0.0129 (14)	0.0220 (15)	0.0100 (13)	0.0025 (10)	−0.0001 (8)	−0.0048 (11)
C1_2	0.0243 (19)	0.0124 (16)	0.0235 (17)	−0.0032 (14)	0.0039 (15)	0.0028 (14)
C2_2	0.0243 (19)	0.0195 (18)	0.0213 (19)	−0.0030 (17)	0.0071 (17)	0.0080 (15)
C3_2	0.0117 (16)	0.0225 (17)	0.0147 (15)	0.0018 (13)	−0.0026 (13)	0.0013 (13)
C4_2	0.0106 (15)	0.0261 (19)	0.0136 (15)	0.0006 (14)	−0.0027 (14)	−0.0016 (14)
C5_2	0.0166 (18)	0.0188 (18)	0.0192 (17)	−0.0067 (15)	0.0048 (14)	0.0010 (14)
C6_2	0.021 (2)	0.0159 (18)	0.0217 (17)	−0.0032 (14)	0.0072 (15)	0.0038 (14)
C7_2	0.026 (2)	0.0156 (17)	0.0195 (17)	0.0046 (15)	−0.0070 (15)	0.0040 (13)
C8_2	0.0166 (18)	0.0207 (18)	0.0228 (18)	0.0089 (15)	−0.0057 (15)	−0.0020 (14)
C9_2	0.0082 (15)	0.029 (2)	0.0189 (17)	−0.0010 (14)	0.0051 (15)	−0.0035 (15)
C10_2	0.0104 (15)	0.0228 (17)	0.0155 (15)	−0.0047 (13)	0.0015 (13)	−0.0036 (14)
S1_3	0.0100 (4)	0.0103 (4)	0.0133 (4)	0.0010 (3)	0.0007 (3)	−0.0001 (3)
O8_3	0.0219 (12)	0.0213 (12)	0.0282 (12)	0.0087 (10)	−0.0041 (10)	0.0089 (10)
O9_3	0.0169 (12)	0.0144 (11)	0.0295 (12)	0.0013 (9)	0.0138 (10)	−0.0013 (10)
O10_3	0.0291 (14)	0.0196 (13)	0.0210 (13)	−0.0084 (11)	−0.0034 (11)	0.0029 (10)
O11_3	0.0204 (12)	0.0228 (12)	0.0128 (11)	0.0096 (10)	0.0046 (10)	0.0031 (9)
S2_4	0.0094 (4)	0.0097 (4)	0.0103 (4)	0.0007 (3)	0.0005 (3)	0.0016 (3)
O8_4	0.0135 (11)	0.0184 (11)	0.0145 (11)	−0.0036 (9)	−0.0027 (8)	0.0043 (9)
O9_4	0.0191 (12)	0.0182 (11)	0.0143 (10)	−0.0001 (9)	−0.0044 (9)	0.0022 (9)
O10_4	0.0217 (13)	0.0209 (12)	0.0188 (12)	0.0091 (10)	0.0044 (10)	0.0017 (9)
O11_4	0.0132 (11)	0.0134 (11)	0.0250 (12)	−0.0034 (9)	−0.0052 (9)	0.0061 (9)
S3_5	0.0097 (4)	0.0095 (4)	0.0141 (4)	−0.0008 (3)	−0.0007 (3)	0.0005 (3)
O8_5	0.0208 (12)	0.0190 (11)	0.0318 (13)	−0.0037 (10)	−0.0107 (10)	−0.0036 (10)
O9_5	0.0199 (13)	0.0207 (12)	0.0305 (13)	0.0003 (10)	0.0100 (10)	−0.0016 (10)
O10_5	0.0218 (13)	0.0178 (12)	0.0187 (13)	0.0061 (10)	−0.0068 (10)	−0.0002 (9)
O11_5	0.0217 (12)	0.0209 (12)	0.0166 (11)	−0.0093 (9)	−0.0007 (10)	0.0008 (9)
S4_6	0.0092 (4)	0.0121 (4)	0.0131 (4)	−0.0005 (3)	−0.0015 (3)	−0.0027 (3)
O8_6	0.0217 (12)	0.0213 (11)	0.0206 (11)	0.0072 (10)	−0.0013 (10)	−0.0040 (9)
O9_6	0.0225 (13)	0.0329 (13)	0.0203 (12)	0.0037 (10)	−0.0060 (10)	−0.0024 (10)
O10_6	0.0189 (13)	0.0203 (12)	0.0233 (13)	−0.0081 (10)	0.0056 (10)	−0.0043 (10)
O11_6	0.0204 (13)	0.0170 (12)	0.0265 (12)	−0.0023 (10)	−0.0005 (10)	−0.0070 (10)

Geometric parameters (Å, º)

Ni1_1—O7_1	1.996 (2)	O2_2—C3_2	1.448 (3)
Ni1_1—O6_1	2.005 (2)	O3_2—C5_2	1.428 (3)
Ni1_1—O2_1	2.0746 (19)	O3_2—C4_2	1.442 (3)
Ni1_1—O1_1	2.0766 (19)	O4_2—C6_2	1.430 (4)
Ni1_1—O3_1	2.147 (2)	O4_2—C7_2	1.438 (4)
Ni1_1—O5_1	2.203 (2)	O5_2—C8_2	1.439 (3)
Ni1_1—O4_1	2.607 (2)	O5_2—C9_2	1.443 (3)
O1_1—C10_1	1.441 (3)	O6_2—H6W1_2	0.87 (2)
O1_1—C1_1	1.451 (3)	O6_2—H6W2_2	0.83 (2)
O2_1—C2_1	1.444 (3)	O7_2—H7W1_2	0.86 (2)
O2_1—C3_1	1.450 (3)	O7_2—H7W2_2	0.82 (2)
O3_1—C5_1	1.432 (3)	C1_2—C2_2	1.502 (4)
O3_1—C4_1	1.441 (3)	C1_2—H1A_2	0.9900
O4_1—C7_1	1.432 (3)	C1_2—H1B_2	0.9900
O4_1—C6_1	1.441 (3)	C2_2—H2A_2	0.9900
O5_1—C9_1	1.441 (3)	C2_2—H2B_2	0.9900
O5_1—C8_1	1.441 (3)	C3_2—C4_2	1.494 (4)
O6_1—H6W1_1	0.85 (2)	C3_2—H3A_2	0.9900
O6_1—H6W2_1	0.78 (2)	C3_2—H3B_2	0.9900
O7_1—H7W1_1	0.77 (2)	C4_2—H4A_2	0.9900
O7_1—H7W2_1	0.84 (2)	C4_2—H4B_2	0.9900
C1_1—C2_1	1.492 (4)	C5_2—C6_2	1.499 (4)
C1_1—H1A_1	0.9900	C5_2—H5A_2	0.9900
C1_1—H1B_1	0.9900	C5_2—H5B_2	0.9900
C2_1—H2A_1	0.9900	C6_2—H6A_2	0.9900
C2_1—H2B_1	0.9900	C6_2—H6B_2	0.9900
C3_1—C4_1	1.510 (4)	C7_2—C8_2	1.499 (4)
C3_1—H3A_1	0.9900	C7_2—H7A_2	0.9900
C3_1—H3B_1	0.9900	C7_2—H7B_2	0.9900
C4_1—H4A_1	0.9900	C8_2—H8A_2	0.9900
C4_1—H4B_1	0.9900	C8_2—H8B_2	0.9900
C5_1—C6_1	1.502 (4)	C9_2—C10_2	1.491 (4)
C5_1—H5A_1	0.9900	C9_2—H9A_2	0.9900
C5_1—H5B_1	0.9900	C9_2—H9B_2	0.9900
C6_1—H6A_1	0.9900	C10_2—H10A_2	0.9900
C6_1—H6B_1	0.9900	C10_2—H10B_2	0.9900
C7_1—C8_1	1.498 (4)	S1_3—O8_3	1.438 (2)
C7_1—H7A_1	0.9900	S1_3—O9_3	1.448 (2)
C7_1—H7B_1	0.9900	S1_3—O10_3	1.458 (2)
C8_1—H8A_1	0.9900	S1_3—O11_3	1.554 (2)
C8_1—H8B_1	0.9900	O11_3—H11_3	0.84 (2)
C9_1—C10_1	1.498 (4)	S2_4—O9_4	1.440 (2)
C9_1—H9A_1	0.9900	S2_4—O10_4	1.454 (2)
C9_1—H9B_1	0.9900	S2_4—O8_4	1.458 (2)
C10_1—H10A_1	0.9900	S2_4—O11_4	1.562 (2)
C10_1—H10B_1	0.9900	O11_4—H11_4	0.82 (2)
Ni2_2—O7_2	1.994 (2)	S3_5—O8_5	1.440 (2)
Ni2_2—O6_2	1.998 (2)	S3_5—O9_5	1.447 (2)
Ni2_2—O1_2	2.064 (2)	S3_5—O10_5	1.461 (2)
Ni2_2—O2_2	2.129 (2)	S3_5—O11_5	1.550 (2)
Ni2_2—O5_2	2.175 (2)	O11_5—H11_5	0.87 (2)
Ni2_2—O3_2	2.183 (2)	S4_6—O9_6	1.438 (2)
Ni2_2—O4_2	2.566 (2)	S4_6—O10_6	1.454 (2)
O1_2—C1_2	1.437 (3)	S4_6—O8_6	1.456 (2)
O1_2—C10_2	1.440 (3)	S4_6—O11_6	1.557 (2)
O2_2—C2_2	1.435 (3)	O11_6—H11_6	0.85 (2)
O7_1—Ni1_1—O6_1	178.46 (11)	O5_2—Ni2_2—O3_2	132.40 (8)
O7_1—Ni1_1—O2_1	87.22 (9)	O7_2—Ni2_2—O4_2	93.05 (9)
O6_1—Ni1_1—O2_1	93.66 (9)	O6_2—Ni2_2—O4_2	85.85 (10)
O7_1—Ni1_1—O1_1	93.32 (9)	O1_2—Ni2_2—O4_2	142.27 (7)
O6_1—Ni1_1—O1_1	88.09 (9)	O2_2—Ni2_2—O4_2	138.68 (7)
O2_1—Ni1_1—O1_1	79.59 (8)	O5_2—Ni2_2—O4_2	67.23 (7)
O7_1—Ni1_1—O3_1	91.75 (8)	O3_2—Ni2_2—O4_2	65.81 (7)
O6_1—Ni1_1—O3_1	87.27 (8)	C1_2—O1_2—C10_2	113.6 (2)
O2_1—Ni1_1—O3_1	74.33 (7)	C1_2—O1_2—Ni2_2	110.18 (16)
O1_1—Ni1_1—O3_1	153.13 (8)	C10_2—O1_2—Ni2_2	113.61 (16)
O7_1—Ni1_1—O5_1	82.94 (8)	C2_2—O2_2—C3_2	114.1 (2)
O6_1—Ni1_1—O5_1	96.82 (8)	C2_2—O2_2—Ni2_2	109.69 (17)
O2_1—Ni1_1—O5_1	152.47 (8)	C3_2—O2_2—Ni2_2	113.54 (16)
O1_1—Ni1_1—O5_1	75.41 (7)	C5_2—O3_2—C4_2	115.2 (2)
O3_1—Ni1_1—O5_1	131.43 (8)	C5_2—O3_2—Ni2_2	127.70 (18)
O7_1—Ni1_1—O4_1	92.83 (9)	C4_2—O3_2—Ni2_2	117.07 (16)
O6_1—Ni1_1—O4_1	85.68 (9)	C6_2—O4_2—C7_2	113.6 (3)
O2_1—Ni1_1—O4_1	140.40 (7)	C6_2—O4_2—Ni2_2	107.12 (18)
O1_1—Ni1_1—O4_1	139.80 (7)	C7_2—O4_2—Ni2_2	108.92 (18)
O3_1—Ni1_1—O4_1	66.08 (7)	C8_2—O5_2—C9_2	114.2 (2)
O5_1—Ni1_1—O4_1	66.02 (7)	C8_2—O5_2—Ni2_2	123.95 (18)
C10_1—O1_1—C1_1	113.6 (2)	C9_2—O5_2—Ni2_2	111.70 (16)
C10_1—O1_1—Ni1_1	114.53 (16)	Ni2_2—O6_2—H6W1_2	123.1 (19)
C1_1—O1_1—Ni1_1	109.10 (16)	Ni2_2—O6_2—H6W2_2	125 (2)
C2_1—O2_1—C3_1	113.6 (2)	H6W1_2—O6_2—H6W2_2	106 (3)
C2_1—O2_1—Ni1_1	110.67 (16)	Ni2_2—O7_2—H7W1_2	121 (2)
C3_1—O2_1—Ni1_1	114.30 (16)	Ni2_2—O7_2—H7W2_2	115 (2)
C5_1—O3_1—C4_1	114.1 (2)	H7W1_2—O7_2—H7W2_2	106 (3)
C5_1—O3_1—Ni1_1	128.71 (17)	O1_2—C1_2—C2_2	106.0 (2)
C4_1—O3_1—Ni1_1	117.19 (16)	O1_2—C1_2—H1A_2	110.5
C7_1—O4_1—C6_1	113.5 (2)	C2_2—C1_2—H1A_2	110.5
C7_1—O4_1—Ni1_1	109.53 (17)	O1_2—C1_2—H1B_2	110.5
C6_1—O4_1—Ni1_1	106.01 (18)	C2_2—C1_2—H1B_2	110.5
C9_1—O5_1—C8_1	113.4 (2)	H1A_2—C1_2—H1B_2	108.7
C9_1—O5_1—Ni1_1	112.32 (16)	O2_2—C2_2—C1_2	105.8 (2)
C8_1—O5_1—Ni1_1	124.67 (18)	O2_2—C2_2—H2A_2	110.6
Ni1_1—O6_1—H6W1_1	116 (2)	C1_2—C2_2—H2A_2	110.6
Ni1_1—O6_1—H6W2_1	126 (2)	O2_2—C2_2—H2B_2	110.6
H6W1_1—O6_1—H6W2_1	112 (3)	C1_2—C2_2—H2B_2	110.6
Ni1_1—O7_1—H7W1_1	121 (2)	H2A_2—C2_2—H2B_2	108.7
Ni1_1—O7_1—H7W2_1	118 (2)	O2_2—C3_2—C4_2	105.3 (2)
H7W1_1—O7_1—H7W2_1	114 (3)	O2_2—C3_2—H3A_2	110.7
O1_1—C1_1—C2_1	105.8 (2)	C4_2—C3_2—H3A_2	110.7
O1_1—C1_1—H1A_1	110.6	O2_2—C3_2—H3B_2	110.7
C2_1—C1_1—H1A_1	110.6	C4_2—C3_2—H3B_2	110.7
O1_1—C1_1—H1B_1	110.6	H3A_2—C3_2—H3B_2	108.8
C2_1—C1_1—H1B_1	110.6	O3_2—C4_2—C3_2	108.0 (2)
H1A_1—C1_1—H1B_1	108.7	O3_2—C4_2—H4A_2	110.1
O2_1—C2_1—C1_1	105.9 (2)	C3_2—C4_2—H4A_2	110.1
O2_1—C2_1—H2A_1	110.5	O3_2—C4_2—H4B_2	110.1
C1_1—C2_1—H2A_1	110.5	C3_2—C4_2—H4B_2	110.1
O2_1—C2_1—H2B_1	110.5	H4A_2—C4_2—H4B_2	108.4
C1_1—C2_1—H2B_1	110.5	O3_2—C5_2—C6_2	106.7 (2)
H2A_1—C2_1—H2B_1	108.7	O3_2—C5_2—H5A_2	110.4
O2_1—C3_1—C4_1	105.6 (2)	C6_2—C5_2—H5A_2	110.4
O2_1—C3_1—H3A_1	110.6	O3_2—C5_2—H5B_2	110.4
C4_1—C3_1—H3A_1	110.6	C6_2—C5_2—H5B_2	110.4
O2_1—C3_1—H3B_1	110.6	H5A_2—C5_2—H5B_2	108.6
C4_1—C3_1—H3B_1	110.6	O4_2—C6_2—C5_2	106.2 (2)
H3A_1—C3_1—H3B_1	108.7	O4_2—C6_2—H6A_2	110.5
O3_1—C4_1—C3_1	107.7 (2)	C5_2—C6_2—H6A_2	110.5
O3_1—C4_1—H4A_1	110.2	O4_2—C6_2—H6B_2	110.5
C3_1—C4_1—H4A_1	110.2	C5_2—C6_2—H6B_2	110.5
O3_1—C4_1—H4B_1	110.2	H6A_2—C6_2—H6B_2	108.7
C3_1—C4_1—H4B_1	110.2	O4_2—C7_2—C8_2	106.3 (2)
H4A_1—C4_1—H4B_1	108.5	O4_2—C7_2—H7A_2	110.5
O3_1—C5_1—C6_1	107.2 (2)	C8_2—C7_2—H7A_2	110.5
O3_1—C5_1—H5A_1	110.3	O4_2—C7_2—H7B_2	110.5
C6_1—C5_1—H5A_1	110.3	C8_2—C7_2—H7B_2	110.5
O3_1—C5_1—H5B_1	110.3	H7A_2—C7_2—H7B_2	108.7
C6_1—C5_1—H5B_1	110.3	O5_2—C8_2—C7_2	105.7 (2)
H5A_1—C5_1—H5B_1	108.5	O5_2—C8_2—H8A_2	110.6
O4_1—C6_1—C5_1	106.2 (2)	C7_2—C8_2—H8A_2	110.6
O4_1—C6_1—H6A_1	110.5	O5_2—C8_2—H8B_2	110.6
C5_1—C6_1—H6A_1	110.5	C7_2—C8_2—H8B_2	110.6
O4_1—C6_1—H6B_1	110.5	H8A_2—C8_2—H8B_2	108.7
C5_1—C6_1—H6B_1	110.5	O5_2—C9_2—C10_2	106.5 (2)
H6A_1—C6_1—H6B_1	108.7	O5_2—C9_2—H9A_2	110.4
O4_1—C7_1—C8_1	105.6 (2)	C10_2—C9_2—H9A_2	110.4
O4_1—C7_1—H7A_1	110.6	O5_2—C9_2—H9B_2	110.4
C8_1—C7_1—H7A_1	110.6	C10_2—C9_2—H9B_2	110.4
O4_1—C7_1—H7B_1	110.6	H9A_2—C9_2—H9B_2	108.6
C8_1—C7_1—H7B_1	110.6	O1_2—C10_2—C9_2	106.2 (2)
H7A_1—C7_1—H7B_1	108.7	O1_2—C10_2—H10A_2	110.5
O5_1—C8_1—C7_1	106.7 (2)	C9_2—C10_2—H10A_2	110.5
O5_1—C8_1—H8A_1	110.4	O1_2—C10_2—H10B_2	110.5
C7_1—C8_1—H8A_1	110.4	C9_2—C10_2—H10B_2	110.5
O5_1—C8_1—H8B_1	110.4	H10A_2—C10_2—H10B_2	108.7
C7_1—C8_1—H8B_1	110.4	O8_3—S1_3—O9_3	114.53 (13)
H8A_1—C8_1—H8B_1	108.6	O8_3—S1_3—O10_3	112.93 (12)
O5_1—C9_1—C10_1	106.2 (2)	O9_3—S1_3—O10_3	111.17 (13)
O5_1—C9_1—H9A_1	110.5	O8_3—S1_3—O11_3	103.74 (12)
C10_1—C9_1—H9A_1	110.5	O9_3—S1_3—O11_3	106.54 (11)
O5_1—C9_1—H9B_1	110.5	O10_3—S1_3—O11_3	107.17 (13)
C10_1—C9_1—H9B_1	110.5	S1_3—O11_3—H11_3	105 (2)
H9A_1—C9_1—H9B_1	108.7	O9_4—S2_4—O10_4	113.35 (12)
O1_1—C10_1—C9_1	106.1 (2)	O9_4—S2_4—O8_4	113.09 (12)
O1_1—C10_1—H10A_1	110.5	O10_4—S2_4—O8_4	111.74 (12)
C9_1—C10_1—H10A_1	110.5	O9_4—S2_4—O11_4	108.53 (11)
O1_1—C10_1—H10B_1	110.5	O10_4—S2_4—O11_4	106.57 (12)
C9_1—C10_1—H10B_1	110.5	O8_4—S2_4—O11_4	102.73 (11)
H10A_1—C10_1—H10B_1	108.7	S2_4—O11_4—H11_4	112 (2)
O7_2—Ni2_2—O6_2	178.37 (9)	O8_5—S3_5—O9_5	114.69 (13)
O7_2—Ni2_2—O1_2	93.07 (9)	O8_5—S3_5—O10_5	112.34 (12)
O6_2—Ni2_2—O1_2	88.54 (9)	O9_5—S3_5—O10_5	111.32 (13)
O7_2—Ni2_2—O2_2	86.31 (9)	O8_5—S3_5—O11_5	103.64 (12)
O6_2—Ni2_2—O2_2	93.71 (9)	O9_5—S3_5—O11_5	106.68 (12)
O1_2—Ni2_2—O2_2	78.88 (8)	O10_5—S3_5—O11_5	107.44 (13)
O7_2—Ni2_2—O5_2	84.03 (8)	S3_5—O11_5—H11_5	100 (2)
O6_2—Ni2_2—O5_2	96.64 (8)	O9_6—S4_6—O10_6	113.97 (13)
O1_2—Ni2_2—O5_2	76.46 (8)	O9_6—S4_6—O8_6	112.99 (13)
O2_2—Ni2_2—O5_2	152.92 (8)	O10_6—S4_6—O8_6	112.03 (12)
O7_2—Ni2_2—O3_2	91.01 (8)	O9_6—S4_6—O11_6	108.29 (13)
O6_2—Ni2_2—O3_2	87.44 (8)	O10_6—S4_6—O11_6	106.08 (12)
O1_2—Ni2_2—O3_2	151.14 (8)	O8_6—S4_6—O11_6	102.51 (12)
O2_2—Ni2_2—O3_2	72.89 (8)	S4_6—O11_6—H11_6	106 (2)
O7_1—Ni1_1—O1_1—C10_1	−61.22 (18)	O7_2—Ni2_2—O1_2—C1_2	−66.15 (18)
O6_1—Ni1_1—O1_1—C10_1	118.15 (18)	O6_2—Ni2_2—O1_2—C1_2	113.56 (19)
O2_1—Ni1_1—O1_1—C10_1	−147.77 (18)	O2_2—Ni2_2—O1_2—C1_2	19.49 (18)
O3_1—Ni1_1—O1_1—C10_1	−161.72 (19)	O5_2—Ni2_2—O1_2—C1_2	−149.25 (19)
O5_1—Ni1_1—O1_1—C10_1	20.60 (17)	O3_2—Ni2_2—O1_2—C1_2	31.5 (3)
O4_1—Ni1_1—O1_1—C10_1	37.1 (2)	O4_2—Ni2_2—O1_2—C1_2	−165.15 (17)
O7_1—Ni1_1—O1_1—C1_1	67.38 (18)	O7_2—Ni2_2—O1_2—C10_2	62.65 (18)
O6_1—Ni1_1—O1_1—C1_1	−113.26 (18)	O6_2—Ni2_2—O1_2—C10_2	−117.65 (18)
O2_1—Ni1_1—O1_1—C1_1	−19.18 (17)	O2_2—Ni2_2—O1_2—C10_2	148.28 (18)
O3_1—Ni1_1—O1_1—C1_1	−33.1 (3)	O5_2—Ni2_2—O1_2—C10_2	−20.46 (17)
O5_1—Ni1_1—O1_1—C1_1	149.19 (18)	O3_2—Ni2_2—O1_2—C10_2	160.35 (18)
O4_1—Ni1_1—O1_1—C1_1	165.74 (16)	O4_2—Ni2_2—O1_2—C10_2	−36.4 (2)
O7_1—Ni1_1—O2_1—C2_1	−107.25 (18)	O7_2—Ni2_2—O2_2—C2_2	107.46 (19)
O6_1—Ni1_1—O2_1—C2_1	74.02 (18)	O6_2—Ni2_2—O2_2—C2_2	−74.18 (18)
O1_1—Ni1_1—O2_1—C2_1	−13.36 (18)	O1_2—Ni2_2—O2_2—C2_2	13.59 (18)
O3_1—Ni1_1—O2_1—C2_1	160.14 (19)	O5_2—Ni2_2—O2_2—C2_2	38.2 (3)
O5_1—Ni1_1—O2_1—C2_1	−38.3 (3)	O3_2—Ni2_2—O2_2—C2_2	−160.35 (19)
O4_1—Ni1_1—O2_1—C2_1	161.66 (17)	O4_2—Ni2_2—O2_2—C2_2	−162.11 (18)
O7_1—Ni1_1—O2_1—C3_1	122.96 (18)	O7_2—Ni2_2—O2_2—C3_2	−123.52 (18)
O6_1—Ni1_1—O2_1—C3_1	−55.77 (18)	O6_2—Ni2_2—O2_2—C3_2	54.84 (18)
O1_1—Ni1_1—O2_1—C3_1	−143.15 (17)	O1_2—Ni2_2—O2_2—C3_2	142.62 (17)
O3_1—Ni1_1—O2_1—C3_1	30.35 (17)	O5_2—Ni2_2—O2_2—C3_2	167.27 (18)
O5_1—Ni1_1—O2_1—C3_1	−168.12 (18)	O3_2—Ni2_2—O2_2—C3_2	−31.32 (17)
O4_1—Ni1_1—O2_1—C3_1	31.9 (2)	O4_2—Ni2_2—O2_2—C3_2	−33.1 (2)
O7_1—Ni1_1—O3_1—C5_1	91.9 (2)	O7_2—Ni2_2—O3_2—C5_2	−91.3 (2)
O6_1—Ni1_1—O3_1—C5_1	−86.9 (2)	O6_2—Ni2_2—O3_2—C5_2	88.2 (2)
O2_1—Ni1_1—O3_1—C5_1	178.5 (2)	O1_2—Ni2_2—O3_2—C5_2	170.5 (2)
O1_1—Ni1_1—O3_1—C5_1	−167.2 (2)	O2_2—Ni2_2—O3_2—C5_2	−177.1 (2)
O5_1—Ni1_1—O3_1—C5_1	9.8 (3)	O5_2—Ni2_2—O3_2—C5_2	−8.4 (3)
O4_1—Ni1_1—O3_1—C5_1	−0.4 (2)	O4_2—Ni2_2—O3_2—C5_2	1.6 (2)
O7_1—Ni1_1—O3_1—C4_1	−90.5 (2)	O7_2—Ni2_2—O3_2—C4_2	89.6 (2)
O6_1—Ni1_1—O3_1—C4_1	90.7 (2)	O6_2—Ni2_2—O3_2—C4_2	−90.9 (2)
O2_1—Ni1_1—O3_1—C4_1	−3.86 (18)	O1_2—Ni2_2—O3_2—C4_2	−8.7 (3)
O1_1—Ni1_1—O3_1—C4_1	10.4 (3)	O2_2—Ni2_2—O3_2—C4_2	3.73 (18)
O5_1—Ni1_1—O3_1—C4_1	−172.60 (16)	O5_2—Ni2_2—O3_2—C4_2	172.40 (17)
O4_1—Ni1_1—O3_1—C4_1	177.2 (2)	O4_2—Ni2_2—O3_2—C4_2	−177.5 (2)
O7_1—Ni1_1—O4_1—C7_1	61.28 (18)	O7_2—Ni2_2—O4_2—C6_2	59.31 (18)
O6_1—Ni1_1—O4_1—C7_1	−119.13 (18)	O6_2—Ni2_2—O4_2—C6_2	−119.48 (18)
O2_1—Ni1_1—O4_1—C7_1	150.34 (17)	O1_2—Ni2_2—O4_2—C6_2	158.32 (17)
O1_1—Ni1_1—O4_1—C7_1	−37.3 (2)	O2_2—Ni2_2—O4_2—C6_2	−28.6 (2)
O3_1—Ni1_1—O4_1—C7_1	151.9 (2)	O5_2—Ni2_2—O4_2—C6_2	141.5 (2)
O5_1—Ni1_1—O4_1—C7_1	−19.70 (17)	O3_2—Ni2_2—O4_2—C6_2	−30.43 (17)
O7_1—Ni1_1—O4_1—C6_1	−61.51 (18)	O7_2—Ni2_2—O4_2—C7_2	−63.93 (19)
O6_1—Ni1_1—O4_1—C6_1	118.07 (18)	O6_2—Ni2_2—O4_2—C7_2	117.28 (19)
O2_1—Ni1_1—O4_1—C6_1	27.5 (2)	O1_2—Ni2_2—O4_2—C7_2	35.1 (3)
O1_1—Ni1_1—O4_1—C6_1	−160.05 (17)	O2_2—Ni2_2—O4_2—C7_2	−151.82 (17)
O3_1—Ni1_1—O4_1—C6_1	29.15 (17)	O5_2—Ni2_2—O4_2—C7_2	18.29 (18)
O5_1—Ni1_1—O4_1—C6_1	−142.50 (19)	O3_2—Ni2_2—O4_2—C7_2	−153.7 (2)
O7_1—Ni1_1—O5_1—C9_1	106.24 (19)	O7_2—Ni2_2—O5_2—C8_2	111.3 (2)
O6_1—Ni1_1—O5_1—C9_1	−75.29 (19)	O6_2—Ni2_2—O5_2—C8_2	−67.2 (2)
O2_1—Ni1_1—O5_1—C9_1	36.3 (3)	O1_2—Ni2_2—O5_2—C8_2	−154.0 (2)
O1_1—Ni1_1—O5_1—C9_1	10.93 (17)	O2_2—Ni2_2—O5_2—C8_2	−178.9 (2)
O3_1—Ni1_1—O5_1—C9_1	−167.67 (16)	O3_2—Ni2_2—O5_2—C8_2	25.4 (3)
O4_1—Ni1_1—O5_1—C9_1	−157.46 (19)	O4_2—Ni2_2—O5_2—C8_2	15.5 (2)
O7_1—Ni1_1—O5_1—C8_1	−110.1 (2)	O7_2—Ni2_2—O5_2—C9_2	−105.49 (19)
O6_1—Ni1_1—O5_1—C8_1	68.3 (2)	O6_2—Ni2_2—O5_2—C9_2	76.01 (19)
O2_1—Ni1_1—O5_1—C8_1	179.95 (19)	O1_2—Ni2_2—O5_2—C9_2	−10.86 (17)
O1_1—Ni1_1—O5_1—C8_1	154.6 (2)	O2_2—Ni2_2—O5_2—C9_2	−35.8 (3)
O3_1—Ni1_1—O5_1—C8_1	−24.0 (3)	O3_2—Ni2_2—O5_2—C9_2	168.61 (16)
O4_1—Ni1_1—O5_1—C8_1	−13.8 (2)	O4_2—Ni2_2—O5_2—C9_2	158.66 (19)
C10_1—O1_1—C1_1—C2_1	176.2 (2)	C10_2—O1_2—C1_2—C2_2	−176.6 (2)
Ni1_1—O1_1—C1_1—C2_1	47.1 (3)	Ni2_2—O1_2—C1_2—C2_2	−47.8 (3)
C3_1—O2_1—C2_1—C1_1	172.4 (2)	C3_2—O2_2—C2_2—C1_2	−170.8 (2)
Ni1_1—O2_1—C2_1—C1_1	42.2 (3)	Ni2_2—O2_2—C2_2—C1_2	−42.2 (3)
O1_1—C1_1—C2_1—O2_1	−58.5 (3)	O1_2—C1_2—C2_2—O2_2	59.1 (3)
C2_1—O2_1—C3_1—C4_1	−178.4 (2)	C2_2—O2_2—C3_2—C4_2	179.2 (2)
Ni1_1—O2_1—C3_1—C4_1	−50.1 (2)	Ni2_2—O2_2—C3_2—C4_2	52.5 (2)
C5_1—O3_1—C4_1—C3_1	157.1 (2)	C5_2—O3_2—C4_2—C3_2	−156.8 (2)
Ni1_1—O3_1—C4_1—C3_1	−20.9 (3)	Ni2_2—O3_2—C4_2—C3_2	22.4 (3)
O2_1—C3_1—C4_1—O3_1	43.1 (3)	O2_2—C3_2—C4_2—O3_2	−45.9 (3)
C4_1—O3_1—C5_1—C6_1	155.0 (2)	C4_2—O3_2—C5_2—C6_2	−154.8 (2)
Ni1_1—O3_1—C5_1—C6_1	−27.3 (3)	Ni2_2—O3_2—C5_2—C6_2	26.0 (3)
C7_1—O4_1—C6_1—C5_1	−171.6 (2)	C7_2—O4_2—C6_2—C5_2	173.3 (2)
Ni1_1—O4_1—C6_1—C5_1	−51.4 (2)	Ni2_2—O4_2—C6_2—C5_2	53.0 (3)
O3_1—C5_1—C6_1—O4_1	51.9 (3)	O3_2—C5_2—C6_2—O4_2	−51.7 (3)
C6_1—O4_1—C7_1—C8_1	164.4 (2)	C6_2—O4_2—C7_2—C8_2	−164.7 (2)
Ni1_1—O4_1—C7_1—C8_1	46.2 (3)	Ni2_2—O4_2—C7_2—C8_2	−45.5 (3)
C9_1—O5_1—C8_1—C7_1	−172.9 (2)	C9_2—O5_2—C8_2—C7_2	172.4 (2)
Ni1_1—O5_1—C8_1—C7_1	43.8 (3)	Ni2_2—O5_2—C8_2—C7_2	−45.2 (3)
O4_1—C7_1—C8_1—O5_1	−56.5 (3)	O4_2—C7_2—C8_2—O5_2	56.9 (3)
C8_1—O5_1—C9_1—C10_1	174.1 (2)	C8_2—O5_2—C9_2—C10_2	−174.9 (2)
Ni1_1—O5_1—C9_1—C10_1	−38.0 (3)	Ni2_2—O5_2—C9_2—C10_2	38.1 (3)
C1_1—O1_1—C10_1—C9_1	−173.6 (2)	C1_2—O1_2—C10_2—C9_2	174.2 (2)
Ni1_1—O1_1—C10_1—C9_1	−47.3 (3)	Ni2_2—O1_2—C10_2—C9_2	47.1 (2)
O5_1—C9_1—C10_1—O1_1	53.8 (3)	O5_2—C9_2—C10_2—O1_2	−54.2 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6_1—H6W1_1···O8_3	0.85 (2)	1.88 (2)	2.712 (3)	168 (3)
O6_1—H6W2_1···O8_4	0.78 (2)	1.97 (2)	2.738 (3)	165 (3)
O7_1—H7W1_1···O8_6	0.77 (2)	1.99 (2)	2.748 (3)	164 (3)
O7_1—H7W2_1···O9_5	0.84 (2)	1.85 (2)	2.686 (3)	176 (3)
O6_2—H6W1_2···O8_6	0.87 (2)	1.91 (2)	2.730 (3)	158 (3)
O6_2—H6W2_2···O8_5	0.83 (2)	1.89 (2)	2.697 (3)	162 (3)
O7_2—H7W1_2···O8_4^i	0.86 (2)	1.88 (2)	2.729 (3)	173 (3)
O7_2—H7W2_2···O9_3^i	0.82 (2)	1.87 (2)	2.671 (3)	167 (3)
O11_3—H11_3···O10_5^ii	0.84 (2)	1.76 (2)	2.583 (3)	166 (3)
O11_4—H11_4···O10_6^iii	0.82 (2)	1.77 (2)	2.565 (3)	163 (3)
O11_5—H11_5···O10_4^iv	0.87 (2)	1.75 (2)	2.579 (3)	158 (3)
O11_6—H11_6···O10_3^v	0.85 (2)	1.76 (2)	2.583 (3)	161 (3)

Symmetry codes: (i) x, y, z+1; (ii) −x, −y+1, z−1/2; (iii) −x+1, −y+1, z−1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z+1/2.