Hexakis­(di­methyl sulfoxide)­nickel(II) dinitrate di­methyl sulfoxide disolvate

The title compound, [Ni(C₂H₆OS)₆](NO₃)₂·2C₂H₆OS, comprises centrosymmetric [Ni(dmso)₆]²⁺ cations, nitrate anions and non-coordinated di­methyl sulfoxide solvent mol­ecules. The octahedral geometry of the cation is very regular, with Ni—O interatomic distances and O—Ni—O interatomic angles falling within narrow ranges 2.0485 (9)–2.0665 (9) Å and 89.12 (4)–93.27 (4)°, respectively. Two weak C—H...O hydrogen-bonding contacts link cations and anions to form a chain which lies along the [111] direction.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](O-N) = 0.002 Å
• R factor = 0.021
• wR factor = 0.057
• Data-to-parameter ratio = 21.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level B:



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           28.65
         From the CIF: _reflns_number_total               4251
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         4850
         Completeness (_total/calc)             87.65%
          Alert B: < 90% complete (theta max?)

Author response: The data collection is 96% complete to theta = 27.5 degrees

 Alert Level C:



ABSTM_02  Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.703     0.769
          Tmin and Tmax expected:      0.638     0.769
          RR =      1.102
          Please check that your absorption correction is appropriate.


 0 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 1 Alert Level C = Please check

---

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT and SHELXTL (Bruker, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CAMERON (Watkin et al., 1996) and SHELXTL; software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2001).

(I)

Crystal data

[Ni(C2H6OS)6](NO3)2·2C2H6OS	F(000) = 426
Mr = 807.75	Dx = 1.421 Mg m^−3
Triclinic, P1	Melting point: unknown K
a = 9.6907 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.3119 (10) Å	Cell parameters from 3076 reflections
c = 11.2549 (11) Å	θ = 2.9–28.4°
α = 63.954 (1)°	µ = 1.01 mm^−1
β = 70.282 (1)°	T = 150 K
γ = 87.414 (2)°	Irregular block, pale green
V = 944.1 (3) Å^3	0.46 × 0.38 × 0.26 mm
Z = 1

Data collection

Bruker SMART1000 CCD area-detector diffractometer	4251 independent reflections
Radiation source: fine-focus sealed tube	3931 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.010
ω scans	θmax = 28.7°, θmin = 2.2°
Absorption correction: multi-scan (Bruker, 2001)	h = −12→12
Tmin = 0.703, Tmax = 0.769	k = −13→13
8316 measured reflections	l = −14→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.021	Hydrogen site location: difference Fourier map
wR(F^2) = 0.057	See text
S = 1.03	w = 1/[σ^2(Fo^2) + (0.03P)^2 + 0.318P] where P = (Fo^2 + 2Fc^2)/3
4251 reflections	(Δ/σ)max = 0.001
195 parameters	Δρmax = 0.46 e Å^−3
0 restraints	Δρmin = −0.26 e Å^−3

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	1.0000	0.0000	0.0000	0.01745 (6)
S2	0.78750 (3)	0.00711 (4)	0.27089 (3)	0.02406 (8)
O21	0.83301 (10)	−0.08810 (9)	0.19528 (9)	0.02316 (18)
C21	0.71013 (18)	−0.12312 (19)	0.45239 (15)	0.0388 (3)
H21A	0.6359	−0.1904	0.4636	0.058*
H21B	0.6663	−0.0740	0.5089	0.058*
H21C	0.7865	−0.1749	0.4823	0.058*
C22	0.62080 (15)	0.07256 (17)	0.24653 (16)	0.0319 (3)
H22A	0.6397	0.1321	0.1477	0.048*
H22B	0.5848	0.1291	0.2969	0.048*
H22C	0.5482	−0.0083	0.2819	0.048*
S3	0.98916 (3)	0.33603 (3)	−0.13943 (3)	0.02341 (7)
O31	0.89903 (10)	0.18525 (9)	−0.05682 (9)	0.02306 (18)
C31	0.87042 (17)	0.44236 (16)	−0.06938 (18)	0.0366 (3)
H31A	0.7739	0.4290	−0.0713	0.055*
H31B	0.9098	0.5432	−0.1255	0.055*
H31C	0.8637	0.4121	0.0263	0.055*
C32	0.9686 (2)	0.40786 (18)	−0.30762 (16)	0.0462 (4)
H32A	1.0231	0.3570	−0.3589	0.069*
H32B	1.0057	0.5094	−0.3600	0.069*
H32C	0.8660	0.3958	−0.2945	0.069*
S4	1.14408 (3)	−0.01084 (3)	0.20775 (3)	0.02129 (7)
O41	1.12934 (10)	0.08882 (9)	0.06542 (9)	0.02320 (18)
C41	1.17323 (18)	0.10991 (16)	0.27420 (16)	0.0334 (3)
H41A	1.2550	0.1825	0.2048	0.050*
H41B	1.1943	0.0561	0.3593	0.050*
H41C	1.0860	0.1561	0.2943	0.050*
C42	1.32564 (15)	−0.06283 (16)	0.16676 (16)	0.0305 (3)
H42A	1.3323	−0.1239	0.1212	0.046*
H42B	1.3462	−0.1151	0.2523	0.046*
H42C	1.3961	0.0225	0.1047	0.046*
S5	0.58901 (4)	−0.39685 (4)	0.10727 (4)	0.03077 (8)
O51	0.49020 (14)	−0.30443 (12)	0.03385 (12)	0.0421 (3)
C51	0.59168 (18)	−0.34312 (18)	0.23703 (17)	0.0372 (3)
H51A	0.6427	−0.2467	0.1909	0.056*
H51B	0.6415	−0.4093	0.2954	0.056*
H51C	0.4922	−0.3444	0.2947	0.056*
C52	0.4844 (2)	−0.57128 (16)	0.22546 (19)	0.0416 (4)
H52A	0.3900	−0.5600	0.2825	0.062*
H52B	0.5365	−0.6301	0.2854	0.062*
H52C	0.4702	−0.6176	0.1721	0.062*
N1	0.77919 (14)	0.26263 (13)	0.41714 (13)	0.0323 (3)
O11	0.65450 (14)	0.19040 (16)	0.48674 (13)	0.0560 (3)
O12	0.87791 (15)	0.23567 (15)	0.46961 (14)	0.0574 (4)
O13	0.80691 (14)	0.35810 (14)	0.29336 (12)	0.0506 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.01913 (11)	0.01742 (11)	0.01557 (10)	0.00208 (8)	−0.00694 (8)	−0.00663 (8)
S2	0.02090 (15)	0.02986 (16)	0.02386 (15)	−0.00030 (12)	−0.00524 (12)	−0.01583 (13)
O21	0.0257 (4)	0.0232 (4)	0.0188 (4)	0.0001 (3)	−0.0043 (3)	−0.0104 (4)
C21	0.0388 (8)	0.0551 (10)	0.0193 (6)	0.0048 (7)	−0.0081 (6)	−0.0153 (7)
C22	0.0250 (7)	0.0370 (8)	0.0314 (7)	0.0067 (6)	−0.0082 (6)	−0.0151 (6)
S3	0.02403 (15)	0.01924 (15)	0.02381 (15)	0.00253 (11)	−0.00841 (12)	−0.00706 (12)
O31	0.0233 (4)	0.0185 (4)	0.0245 (4)	0.0027 (3)	−0.0087 (4)	−0.0071 (4)
C31	0.0378 (8)	0.0264 (7)	0.0459 (9)	0.0059 (6)	−0.0100 (7)	−0.0202 (7)
C32	0.0767 (13)	0.0298 (8)	0.0259 (7)	−0.0033 (8)	−0.0227 (8)	−0.0031 (6)
S4	0.02274 (15)	0.02270 (15)	0.01910 (14)	0.00065 (11)	−0.00957 (11)	−0.00820 (12)
O41	0.0270 (5)	0.0223 (4)	0.0202 (4)	0.0003 (3)	−0.0116 (4)	−0.0068 (4)
C41	0.0451 (8)	0.0336 (7)	0.0302 (7)	0.0026 (6)	−0.0174 (6)	−0.0186 (6)
C42	0.0258 (7)	0.0346 (7)	0.0347 (7)	0.0076 (5)	−0.0153 (6)	−0.0158 (6)
S5	0.03384 (18)	0.02589 (17)	0.03046 (17)	0.00486 (13)	−0.01040 (14)	−0.01173 (14)
O51	0.0580 (7)	0.0301 (5)	0.0422 (6)	0.0110 (5)	−0.0291 (6)	−0.0120 (5)
C51	0.0386 (8)	0.0376 (8)	0.0433 (8)	0.0067 (6)	−0.0186 (7)	−0.0221 (7)
C52	0.0511 (10)	0.0251 (7)	0.0476 (9)	0.0002 (6)	−0.0258 (8)	−0.0090 (7)
N1	0.0363 (6)	0.0263 (6)	0.0296 (6)	−0.0019 (5)	−0.0097 (5)	−0.0094 (5)
O11	0.0437 (7)	0.0660 (9)	0.0389 (6)	−0.0238 (6)	−0.0069 (5)	−0.0099 (6)
O12	0.0487 (7)	0.0508 (7)	0.0539 (8)	−0.0009 (6)	−0.0280 (6)	0.0003 (6)
O13	0.0540 (7)	0.0467 (7)	0.0328 (6)	−0.0097 (6)	−0.0155 (5)	−0.0007 (5)

Geometric parameters (Å, º)

Ni1—O21	2.0625 (9)	C22—H22A	0.96
Ni1—O31	2.0485 (9)	C22—H22B	0.96
Ni1—O41	2.0665 (9)	C22—H22C	0.96
S2—O21	1.5245 (9)	C51—H51A	0.96
S2—C22	1.7827 (14)	C51—H51B	0.96
S2—C21	1.7852 (15)	C51—H51C	0.96
S3—O31	1.5329 (9)	C52—H52A	0.96
S3—C31	1.7834 (15)	C52—H52B	0.96
S3—C32	1.7837 (15)	C52—H52C	0.96
S4—O41	1.5291 (9)	C31—H31A	0.96
S4—C42	1.7833 (14)	C31—H31B	0.96
S4—C41	1.7838 (14)	C31—H31C	0.96
S5—O51	1.5059 (11)	C32—H32A	0.96
S5—C51	1.7827 (16)	C32—H32B	0.96
S5—C52	1.7851 (16)	C32—H32C	0.96
N1—O11	1.2484 (17)	C41—H41A	0.96
N1—O12	1.2467 (17)	C41—H41B	0.96
N1—O13	1.2446 (16)	C41—H41C	0.96
C21—H21A	0.96	C42—H42A	0.96
C21—H21B	0.96	C42—H42B	0.96
C21—H21C	0.96	C42—H42C	0.96
O21—Ni1—O31	89.12 (4)	H51A—C51—H51B	109.5
O21—Ni1—O41	93.27 (4)	S5—C51—H51C	109.5
O31—Ni1—O41	90.45 (4)	H51A—C51—H51C	109.5
O21—S2—C22	106.41 (6)	H51B—C51—H51C	109.5
O21—S2—C21	102.82 (7)	S5—C52—H52A	109.5
C22—S2—C21	98.26 (7)	S5—C52—H52B	109.5
S2—O21—Ni1	117.56 (5)	H52A—C52—H52B	109.5
O51—S5—C51	107.23 (7)	S5—C52—H52C	109.5
O51—S5—C52	106.11 (7)	H52A—C52—H52C	109.5
C51—S5—C52	97.68 (8)	H52B—C52—H52C	109.5
O31—S3—C31	102.96 (6)	S3—C31—H31A	109.5
O31—S3—C32	104.03 (7)	S3—C31—H31B	109.5
C31—S3—C32	98.54 (9)	H31A—C31—H31B	109.5
S3—O31—Ni1	121.03 (5)	S3—C31—H31C	109.5
O41—S4—C42	105.70 (6)	H31A—C31—H31C	109.5
O41—S4—C41	104.45 (6)	H31B—C31—H31C	109.5
C42—S4—C41	98.17 (7)	S3—C32—H32A	109.5
S4—O41—Ni1	116.09 (5)	S3—C32—H32B	109.5
O13—N1—O12	119.80 (13)	H32A—C32—H32B	109.5
O13—N1—O11	120.07 (13)	S3—C32—H32C	109.5
O12—N1—O11	120.08 (13)	H32A—C32—H32C	109.5
S2—C21—H21A	109.5	H32B—C32—H32C	109.5
S2—C21—H21B	109.5	S4—C41—H41A	109.5
H21A—C21—H21B	109.5	S4—C41—H41B	109.5
S2—C21—H21C	109.5	H41A—C41—H41B	109.5
H21A—C21—H21C	109.5	S4—C41—H41C	109.5
H21B—C21—H21C	109.5	H41A—C41—H41C	109.5
S2—C22—H22A	109.5	H41B—C41—H41C	109.5
S2—C22—H22B	109.5	S4—C42—H42A	109.5
H22A—C22—H22B	109.5	S4—C42—H42B	109.5
S2—C22—H22C	109.5	H42A—C42—H42B	109.5
H22A—C22—H22C	109.5	S4—C42—H42C	109.5
H22B—C22—H22C	109.5	H42A—C42—H42C	109.5
S5—C51—H51A	109.5	H42B—C42—H42C	109.5
S5—C51—H51B	109.5