Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801016403/na6097sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801016403/na6097Isup2.hkl |
CCDC reference: 177173
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (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
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).
[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) Å3 | 0.46 × 0.38 × 0.26 mm |
Z = 1 |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.057 | See text |
S = 1.03 | w = 1/[σ2(Fo2) + (0.03P)2 + 0.318P] where P = (Fo2 + 2Fc2)/3 |
4251 reflections | (Δ/σ)max = 0.001 |
195 parameters | Δρmax = 0.46 e Å−3 |
0 restraints | Δρmin = −0.26 e Å−3 |
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. |
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) |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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 |