Buy article online - an online subscription or single-article purchase is required to access this article.
The title compound, [Ni(C
9H
4INO
6S)
2(H
2O)
6]·4H
2O, is isomorphous with the corresponding cobalt(II) complex of ferron. Two inversion-related ligands and two Ni
II atoms form a cage-like dimer. Both ligands of the dimer are bridged by a pair of inversion-related Ni—O(sulfonate) bonds. The octahedral coordination geometry of nickel(II) is made up of the ring N atom, the deprotonated quinolinol O atom (the usual bidentate chelation), one of the sulfonate O atoms, and three water molecules. The ligands in the dimer are stacked over one another. This architecture is further stabilized by a number of O—H
O hydrogen bonds involving the deprotonated quinolinol O atom, sulfonate O atoms, and uncoordinated and coordinated water molecules.
Supporting information
CCDC reference: 187221
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.005 Å
- R factor = 0.026
- wR factor = 0.095
- Data-to-parameter ratio = 11.1
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level A:
PLAT_731 Alert A Bond Calc 0.9(3), Rep 0.95(3) .... 9.90 su-Ratio
O1W -H12 1.555 1.555
PLAT_734 Alert A Contact Calc 2.1(3), Rep 2.15(3) .... 9.90 su-Ratio
O4 -H12 1.555 5.555
PLAT_734 Alert A Contact Calc 2.1(3), Rep 2.15(3) .... 9.90 su-Ratio
H12 -O4 1.555 5.445
PLAT_734 Alert A Contact Calc 1.9(4), Rep 1.91(4) .... 9.90 su-Ratio
H52 -O4W 1.555 3.665
PLAT_735 Alert A D-H Calc 0.9(3), Rep 0.95(3) .... 9.90 su-Ratio
O1W -H12 1.555 1.555
PLAT_736 Alert A H...A Calc 2.1(3), Rep 2.15(3) .... 9.90 su-Ratio
H12 -O4 1.555 5.445
PLAT_736 Alert A H...A Calc 1.9(4), Rep 1.91(4) .... 9.90 su-Ratio
H52 -O4W 1.555 3.665
Alert Level B:
PLAT_731 Alert B Bond Calc 0.9(3), Rep 0.94(4) .... 7.50 su-Ratio
O5W -H52 1.555 1.555
PLAT_731 Alert B Bond Calc 0.9(3), Rep 0.93(4) .... 7.50 su-Ratio
O5W -H51 1.555 1.555
PLAT_732 Alert B Angle Calc 109(20), Rep 110(4) .... 5.00 su-Ratio
H51 -O5W -H52 1.555 1.555 1.555
PLAT_734 Alert B Contact Calc 3.0(3), Rep 2.96(4) .... 7.50 su-Ratio
I1 -H51 1.555 3.665
PLAT_734 Alert B Contact Calc 3.1(2), Rep 3.13(4) .... 5.00 su-Ratio
S1 -H12 1.555 5.555
PLAT_734 Alert B Contact Calc 1.9(4), Rep 1.91(5) .... 8.00 su-Ratio
O4W -H52 1.555 3.665
PLAT_734 Alert B Contact Calc 2.9(3), Rep 2.89(6) .... 5.00 su-Ratio
O5W -H52 1.555 2.654
PLAT_734 Alert B Contact Calc 3.0(3), Rep 2.95(4) .... 7.50 su-Ratio
C8 -H51 1.555 3.665
PLAT_734 Alert B Contact Calc 3.1(2), Rep 3.13(4) .... 5.00 su-Ratio
H12 -S1 1.555 5.445
PLAT_734 Alert B Contact Calc 2.4(4), Rep 2.42(7) .... 5.71 su-Ratio
H41 -H52 1.555 3.665
PLAT_734 Alert B Contact Calc 1.1(4), Rep 1.14(6) .... 6.67 su-Ratio
H42 -H52 1.555 3.665
PLAT_734 Alert B Contact Calc 3.0(3), Rep 2.96(4) .... 7.50 su-Ratio
H51 -I1 1.555 3.665
PLAT_734 Alert B Contact Calc 3.0(3), Rep 2.95(4) .... 7.50 su-Ratio
H51 -C8 1.555 3.665
PLAT_734 Alert B Contact Calc 2.4(3), Rep 2.42(6) .... 5.00 su-Ratio
H52 -H41 1.555 3.665
PLAT_734 Alert B Contact Calc 1.1(4), Rep 1.14(6) .... 6.67 su-Ratio
H52 -H42 1.555 3.665
PLAT_735 Alert B D-H Calc 0.9(3), Rep 0.93(4) .... 7.50 su-Ratio
O5W -H51 1.555 1.555
PLAT_735 Alert B D-H Calc 0.9(3), Rep 0.93(4) .... 7.50 su-Ratio
O5W -H51 1.555 1.555
PLAT_735 Alert B D-H Calc 0.9(3), Rep 0.94(4) .... 7.50 su-Ratio
O5W -H52 1.555 1.555
PLAT_736 Alert B H...A Calc 3.0(3), Rep 2.96(4) .... 7.50 su-Ratio
H51 -I1 1.555 3.665
Alert Level C:
ABSTY_02 Alert C An _exptl_absorpt_correction_type has been given without
a literature citation. This should be contained in the
_exptl_absorpt_process_details field.
Absorption correction given as \y scan
PLAT_213 Alert C Atom C8 has ADP max/min Ratio ........... 3.10 oblate
PLAT_213 Alert C Atom C10 has ADP max/min Ratio ........... 3.50 prolate
PLAT_732 Alert C Angle Calc 99(7), Rep 99(3) .... 2.33 su-Ratio
NI -O1W -H12 1.555 1.555 1.555
PLAT_734 Alert C Contact Calc 2.06(19), Rep 2.04(5) .... 3.80 su-Ratio
O1 -H51 1.555 3.665
PLAT_734 Alert C Contact Calc 2.20(17), Rep 2.21(7) .... 2.43 su-Ratio
H31 -H51 1.555 1.555
PLAT_734 Alert C Contact Calc 2.48(16), Rep 2.48(7) .... 2.29 su-Ratio
H32 -H52 1.555 3.665
PLAT_734 Alert C Contact Calc 2.20(17), Rep 2.21(7) .... 2.43 su-Ratio
H51 -H31 1.555 1.555
PLAT_734 Alert C Contact Calc 2.1(2), Rep 2.04(5) .... 4.00 su-Ratio
H51 -O1 1.555 3.665
PLAT_734 Alert C Contact Calc 2.9(2), Rep 2.89(6) .... 3.33 su-Ratio
H52 -O5W 1.555 2.654
PLAT_734 Alert C Contact Calc 2.4(3), Rep 2.37(9) .... 3.33 su-Ratio
H52 -H52 1.555 2.654
PLAT_736 Alert C H...A Calc 2.1(2), Rep 2.04(5) .... 4.00 su-Ratio
H51 -O1 1.555 3.665
7 Alert Level A = Potentially serious problem
19 Alert Level B = Potential problem
12 Alert Level C = Please check
Data collection: Kuma KM4CCD software (Kuma, 1999); cell refinement: KM-4 CCD Software (Kuma, 1999); data reduction: KM-4 CCD Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXS97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON.
Crystal data top
[Ni(C9H4INO6S)2(H2O)6]·4H2O | F(000) = 1952 |
Mr = 995.74 | Dx = 2.304 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 10072 reflections |
a = 22.053 (4) Å | θ = 3.5–25.1° |
b = 10.009 (2) Å | µ = 3.69 mm−1 |
c = 13.241 (3) Å | T = 120 K |
β = 100.760 (3)° | Cuboid, green |
V = 2871.3 (10) Å3 | 0.35 × 0.30 × 0.20 mm |
Z = 4 | |
Data collection top
Kuma KM4CCD diffractometer | 2539 independent reflections |
Radiation source: fine-focus sealed tube | 2405 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
ω scans | θmax = 25.1°, θmin = 3.5° |
Absorption correction: ψ scan | h = −26→26 |
Tmin = 0.236, Tmax = 0.465 | k = −11→11 |
10398 measured reflections | l = −15→13 |
Refinement top
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.83 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
2539 reflections | (Δ/σ)max = 0.001 |
229 parameters | Δρmax = 0.76 e Å−3 |
15 restraints | Δρmin = −0.94 e Å−3 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Refinement. Refinement on F2 for ALL reflections except those flagged by the user
for potential systematic errors. Weighted R-factors wR
and all goodnesses of fit S are based on F2,
conventional R-factors R are based on F, with F
set to zero for negative F2. The observed criterion of F2 >
σ(F2) is used only for calculating -R-factor-obs
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 (Å2) top | x | y | z | Uiso*/Ueq | |
I1 | 0.67525 (1) | 0.70989 (2) | 0.06225 (2) | 0.0131 (1) | |
Ni | 0.58563 (2) | 0.22877 (4) | 0.08990 (4) | 0.0079 (2) | |
S1 | 0.89526 (4) | 0.39410 (9) | 0.14371 (6) | 0.0083 (2) | |
O1 | 0.62124 (11) | 0.4156 (2) | 0.08144 (18) | 0.0104 (7) | |
O1W | 0.54774 (12) | 0.0407 (3) | 0.09759 (19) | 0.0128 (8) | |
O2 | 0.91679 (11) | 0.3500 (3) | 0.25029 (19) | 0.0115 (7) | |
O2W | 0.57927 (14) | 0.2580 (3) | 0.2437 (2) | 0.0199 (9) | |
O3 | 0.91217 (12) | 0.2961 (2) | 0.0716 (2) | 0.0095 (8) | |
O3W | 0.49737 (13) | 0.2859 (2) | 0.0390 (2) | 0.0127 (8) | |
O4 | 0.91470 (11) | 0.5295 (2) | 0.12565 (19) | 0.0120 (7) | |
N1 | 0.67700 (14) | 0.1801 (3) | 0.1257 (2) | 0.0098 (9) | |
C2 | 0.70223 (17) | 0.0613 (4) | 0.1441 (3) | 0.0103 (10) | |
C3 | 0.76622 (17) | 0.0413 (4) | 0.1573 (3) | 0.0120 (11) | |
C4 | 0.80447 (16) | 0.1474 (4) | 0.1526 (3) | 0.0102 (10) | |
C5 | 0.81364 (16) | 0.3971 (4) | 0.1260 (3) | 0.0088 (10) | |
C6 | 0.78343 (16) | 0.5175 (4) | 0.1071 (2) | 0.0093 (10) | |
C7 | 0.71902 (16) | 0.5255 (4) | 0.0932 (3) | 0.0095 (10) | |
C8 | 0.68206 (16) | 0.4137 (4) | 0.0972 (3) | 0.0094 (10) | |
C9 | 0.71379 (18) | 0.2889 (3) | 0.1195 (3) | 0.0093 (11) | |
C10 | 0.77854 (18) | 0.2783 (3) | 0.1334 (3) | 0.0076 (10) | |
O4W | 0.43091 (12) | 0.4751 (3) | 0.1230 (2) | 0.0150 (8) | |
O5W | 0.45865 (12) | 0.3903 (3) | −0.1560 (2) | 0.0147 (8) | |
H2 | 0.6768 | −0.0118 | 0.1485 | 0.0120* | |
H3 | 0.7825 | −0.0441 | 0.1692 | 0.0140* | |
H4 | 0.8469 | 0.1348 | 0.1618 | 0.0120* | |
H6 | 0.8062 | 0.5949 | 0.1036 | 0.0110* | |
H11 | 0.561 (2) | −0.022 (5) | 0.150 (3) | 0.0500* | |
H12 | 0.508 (13) | 0.066 (5) | 0.108 (4) | 0.0500* | |
H21 | 0.581 (3) | 0.196 (4) | 0.299 (3) | 0.0500* | |
H22 | 0.569 (3) | 0.338 (3) | 0.275 (4) | 0.0500* | |
H31 | 0.489 (3) | 0.304 (5) | −0.0324 (16) | 0.0500* | |
H32 | 0.471 (2) | 0.346 (5) | 0.067 (3) | 0.0500* | |
H41 | 0.412 (2) | 0.509 (5) | 0.058 (2) | 0.0500* | |
H42 | 0.459 (2) | 0.542 (4) | 0.152 (4) | 0.0500* | |
H51 | 0.426 (16) | 0.433 (5) | −0.138 (4) | 0.0500* | |
H52 | 0.488 (19) | 0.453 (4) | −0.166 (5) | 0.0500* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0127 (2) | 0.0082 (2) | 0.0188 (2) | 0.0011 (1) | 0.0039 (1) | 0.0015 (1) |
Ni | 0.0076 (3) | 0.0075 (3) | 0.0086 (3) | 0.0002 (2) | 0.0012 (2) | 0.0003 (2) |
S1 | 0.0075 (4) | 0.0089 (4) | 0.0084 (4) | −0.0006 (3) | 0.0013 (3) | −0.0005 (3) |
O1 | 0.0091 (12) | 0.0106 (13) | 0.0115 (12) | −0.0011 (10) | 0.0020 (10) | −0.0023 (10) |
O1W | 0.0133 (13) | 0.0109 (13) | 0.0141 (13) | −0.0012 (10) | 0.0022 (10) | 0.0036 (10) |
O2 | 0.0116 (12) | 0.0141 (13) | 0.0080 (12) | −0.0014 (10) | −0.0001 (10) | 0.0023 (10) |
O2W | 0.0370 (18) | 0.0107 (13) | 0.0136 (15) | 0.0022 (14) | 0.0086 (13) | 0.0017 (12) |
O3 | 0.0073 (13) | 0.0112 (13) | 0.0104 (13) | 0.0015 (9) | 0.0024 (10) | −0.0033 (9) |
O3W | 0.0101 (14) | 0.0154 (15) | 0.0130 (14) | 0.0015 (9) | 0.0029 (11) | 0.0000 (10) |
O4 | 0.0111 (12) | 0.0085 (13) | 0.0168 (13) | −0.0006 (10) | 0.0036 (10) | 0.0000 (10) |
N1 | 0.0129 (16) | 0.0117 (15) | 0.0050 (15) | −0.0018 (12) | 0.0020 (12) | −0.0030 (12) |
C2 | 0.0157 (19) | 0.0095 (18) | 0.0059 (17) | −0.0009 (14) | 0.0023 (13) | 0.0012 (14) |
C3 | 0.0147 (19) | 0.0085 (18) | 0.0117 (18) | 0.0025 (14) | 0.0000 (14) | −0.0002 (14) |
C4 | 0.0112 (17) | 0.0127 (19) | 0.0067 (17) | 0.0037 (14) | 0.0017 (14) | −0.0023 (14) |
C5 | 0.0066 (16) | 0.0116 (18) | 0.0078 (17) | 0.0008 (14) | 0.0000 (13) | −0.0003 (14) |
C6 | 0.0116 (17) | 0.0098 (17) | 0.0054 (17) | −0.0036 (14) | −0.0009 (13) | 0.0009 (13) |
C7 | 0.0110 (17) | 0.0087 (17) | 0.0089 (18) | 0.0006 (14) | 0.0019 (14) | −0.0008 (13) |
C8 | 0.0135 (18) | 0.0126 (18) | 0.0021 (16) | 0.0013 (14) | 0.0016 (13) | −0.0021 (14) |
C9 | 0.0142 (19) | 0.0091 (19) | 0.0047 (17) | −0.0023 (13) | 0.0017 (15) | −0.0003 (13) |
C10 | 0.0132 (18) | 0.0081 (18) | 0.0012 (16) | 0.0023 (13) | 0.0003 (14) | −0.0002 (12) |
O4W | 0.0177 (14) | 0.0114 (14) | 0.0153 (14) | 0.0011 (11) | 0.0015 (11) | 0.0016 (10) |
O5W | 0.0109 (13) | 0.0164 (14) | 0.0174 (14) | −0.0001 (11) | 0.0041 (11) | 0.0004 (11) |
Geometric parameters (Å, º) top
I1—C7 | 2.088 (4) | O4W—H41 | 0.95 (3) |
Ni—O1 | 2.039 (2) | O5W—H52 | 0.94 (4) |
Ni—O1W | 2.070 (3) | O5W—H51 | 0.93 (4) |
Ni—O2W | 2.088 (3) | N1—C9 | 1.370 (5) |
Ni—O3W | 2.020 (3) | N1—C2 | 1.316 (5) |
Ni—N1 | 2.041 (3) | C2—C3 | 1.404 (5) |
Ni—O3i | 2.162 (3) | C3—C4 | 1.365 (6) |
S1—O2 | 1.470 (3) | C4—C10 | 1.433 (5) |
S1—O3 | 1.465 (3) | C5—C6 | 1.377 (6) |
S1—O4 | 1.455 (2) | C5—C10 | 1.432 (5) |
S1—C5 | 1.771 (4) | C6—C7 | 1.400 (5) |
O1—C8 | 1.318 (4) | C7—C8 | 1.391 (5) |
O1W—H11 | 0.94 (4) | C8—C9 | 1.435 (5) |
O1W—H12 | 0.95 (3) | C9—C10 | 1.409 (6) |
O2W—H22 | 0.95 (4) | C2—H2 | 0.930 |
O2W—H21 | 0.96 (4) | C3—H3 | 0.929 |
O3W—H32 | 0.96 (5) | C4—H4 | 0.929 |
O3W—H31 | 0.95 (2) | C6—H6 | 0.929 |
O4W—H42 | 0.94 (5) | | |
| | | |
I1···O1 | 3.205 (2) | C4···O3 | 3.156 (5) |
I1···C2ii | 3.696 (4) | C4···O2 | 3.275 (5) |
I1···C6iii | 3.750 (4) | C5···C2i | 3.552 (6) |
I1···O4Wiv | 3.575 (3) | C5···C2v | 3.534 (6) |
I1···O5Wiv | 3.555 (3) | C6···C3i | 3.517 (5) |
I1···I1iii | 4.0325 (10) | C6···I1iii | 3.751 (4) |
I1···C4v | 3.771 (4) | C6···C3v | 3.502 (5) |
I1···H51iv | 2.96 (4) | C6···C2i | 3.490 (5) |
I1···H41iv | 3.15 (4) | C6···C2v | 3.280 (5) |
I1···H2ii | 3.008 | C7···C3v | 3.262 (6) |
I1···H6iii | 3.0237 | C7···C3i | 3.458 (6) |
Ni···H41iv | 3.28 (4) | C8···C4i | 3.431 (6) |
Ni···H51iv | 3.46 (5) | C8···C3v | 3.481 (6) |
S1···H4 | 2.833 | C9···C10i | 3.450 (6) |
S1···H12vi | 3.13 (4) | C10···C9i | 3.451 (6) |
S1···H11v | 2.85 (4) | C10···C10i | 3.567 (6) |
S1···H21v | 3.14 (4) | C5···H2v | 3.091 |
O1···I1 | 3.205 (2) | C8···H41iv | 2.74 (4) |
O1···O4Wiv | 2.947 (4) | C8···H3v | 3.075 |
O1···O5Wiv | 2.916 (4) | C8···H51iv | 2.95 (4) |
O1W···O1Wvii | 3.122 (4) | H2···H11 | 2.560 |
O1W···O4viii | 3.027 (4) | H2···C5ix | 3.091 |
O1W···O2ix | 2.779 (4) | H2···I1xviii | 3.008 |
O2···C4 | 3.275 (5) | H2···O1W | 2.849 |
O2···O1Wv | 2.779 (4) | H3···C8ix | 3.075 |
O2···O5Wx | 2.784 (4) | H4···O2 | 2.777 |
O2W···O4Wxi | 2.835 (4) | H4···O3 | 2.597 |
O2W···O4ix | 2.856 (4) | H4···S1 | 2.833 |
O3···C4 | 3.156 (5) | H4···H41xvi | 2.505 |
O3W···O4W | 2.753 (4) | H4···O4Wxvi | 2.570 |
O3W···O5W | 2.768 (4) | H6···I1iii | 3.024 |
O4···O1Wvi | 3.027 (4) | H6···O4 | 2.445 |
O4···O2Wv | 2.856 (4) | H11···O2ix | 1.84 (4) |
O4W···O5Wiv | 2.746 (4) | H11···S1ix | 2.85 (4) |
O4W···O5Wxii | 3.175 (4) | H11···H2 | 2.560 |
O4W···O3W | 2.753 (4) | H12···S1viii | 3.13 (4) |
O4W···O2Wxi | 2.835 (4) | H12···O4viii | 2.15 (3) |
O4W···O1iv | 2.947 (4) | H21···O4ix | 1.94 (4) |
O4W···I1iv | 3.575 (3) | H21···S1ix | 3.14 (4) |
O4W···C4xiii | 3.363 (5) | H22···H42xi | 2.39 (6) |
O5W···O1iv | 2.916 (4) | H22···H32xi | 2.42 (7) |
O5W···O2xiv | 2.784 (4) | H22···O4Wxi | 1.93 (4) |
O5W···O4Wiv | 2.746 (4) | H31···O5W | 1.86 (3) |
O5W···O3W | 2.768 (4) | H31···H51 | 2.21 (7) |
O5W···I1iv | 3.555 (3) | H31···H52 | 2.31 (7) |
O5W···O4Wxv | 3.175 (4) | H32···H52iv | 2.48 (7) |
O1···H41iv | 2.00 (3) | H32···H22xi | 2.42 (7) |
O1···H51iv | 2.04 (5) | H32···O4W | 1.80 (5) |
O1W···H2 | 2.849 | H32···H41 | 2.08 (7) |
O2···H11v | 1.84 (5) | H32···H42 | 2.30 (6) |
O2···H4 | 2.777 | H41···Niiv | 3.28 (4) |
O3···H4 | 2.597 | H41···O1iv | 2.00 (3) |
O3···H42xvi | 2.87 (4) | H41···C8iv | 2.74 (4) |
O3···H41xvi | 2.88 (5) | H41···H52iv | 2.42 (7) |
O4···H12vi | 2.15 (3) | H41···O3xiii | 2.88 (5) |
O4···H6 | 2.445 | H41···H32 | 2.08 (7) |
O4···H21v | 1.94 (4) | H41···I1iv | 3.15 (4) |
O4W···H4xiii | 2.570 | H41···H4xiii | 2.505 |
O4W···H52iv | 1.91 (5) | H42···O5Wiv | 1.93 (4) |
O4W···H22xi | 1.93 (4) | H42···H52iv | 1.14 (6) |
O4W···H32 | 1.80 (5) | H42···H52xii | 2.38 (8) |
O5W···H42iv | 1.93 (4) | H42···O3xiii | 2.87 (4) |
O5W···H31 | 1.86 (3) | H42···O5Wxii | 2.63 (5) |
O5W···H42xv | 2.63 (5) | H42···H32 | 2.30 (6) |
O5W···H52xvii | 2.89 (6) | H42···H22xi | 2.39 (6) |
C2···C6i | 3.490 (5) | H51···H31 | 2.21 (7) |
C2···C5i | 3.552 (6) | H51···I1iv | 2.96 (4) |
C2···I1xviii | 3.696 (4) | H51···Niiv | 3.46 (5) |
C2···C5ix | 3.534 (6) | H51···O1iv | 2.04 (5) |
C2···C6ix | 3.280 (5) | H51···C8iv | 2.95 (4) |
C3···C7ix | 3.262 (6) | H52···H31 | 2.31 (7) |
C3···C8ix | 3.481 (6) | H52···O5Wxvii | 2.89 (6) |
C3···C6i | 3.517 (5) | H52···H52xvii | 2.37 (9) |
C3···C6ix | 3.502 (5) | H52···O4Wiv | 1.91 (4) |
C3···C7i | 3.458 (6) | H52···H32iv | 2.48 (7) |
C4···O4Wxvi | 3.363 (5) | H52···H41iv | 2.42 (6) |
C4···I1ix | 3.770 (4) | H52···H42iv | 1.14 (6) |
C4···C8i | 3.431 (6) | H52···H42xv | 2.38 (8) |
| | | |
O1—Ni—O1W | 178.86 (10) | H41—O4W—H42 | 105 (4) |
O1—Ni—O2W | 91.25 (11) | H51—O5W—H52 | 110 (4) |
O1—Ni—O3W | 94.53 (9) | Ni—N1—C9 | 111.5 (2) |
O1—Ni—N1 | 81.84 (11) | Ni—N1—C2 | 128.6 (3) |
O1—Ni—O3i | 88.35 (9) | C2—N1—C9 | 119.7 (3) |
O1W—Ni—O2W | 88.75 (11) | N1—C2—C3 | 122.2 (4) |
O1W—Ni—O3W | 84.33 (10) | C2—C3—C4 | 119.9 (4) |
O1W—Ni—N1 | 99.30 (11) | C3—C4—C10 | 119.3 (3) |
O1W—Ni—O3i | 91.59 (9) | S1—C5—C6 | 118.9 (3) |
O2W—Ni—O3W | 92.85 (11) | C6—C5—C10 | 119.3 (3) |
O2W—Ni—N1 | 92.87 (11) | S1—C5—C10 | 121.7 (3) |
O2W—Ni—O3i | 177.09 (11) | C5—C6—C7 | 121.2 (4) |
O3W—Ni—N1 | 173.29 (11) | C6—C7—C8 | 122.4 (4) |
O3i—Ni—O3W | 84.30 (10) | I1—C7—C6 | 119.8 (3) |
O3i—Ni—N1 | 89.93 (10) | I1—C7—C8 | 117.8 (3) |
O2—S1—O3 | 110.41 (16) | O1—C8—C7 | 124.6 (3) |
O2—S1—O4 | 112.66 (16) | C7—C8—C9 | 116.2 (3) |
O2—S1—C5 | 105.68 (17) | O1—C8—C9 | 119.2 (3) |
O3—S1—O4 | 113.45 (14) | N1—C9—C10 | 122.0 (3) |
O3—S1—C5 | 107.52 (17) | N1—C9—C8 | 115.6 (3) |
O4—S1—C5 | 106.61 (17) | C8—C9—C10 | 122.4 (3) |
Ni—O1—C8 | 111.6 (2) | C5—C10—C9 | 118.4 (3) |
Nii—O3—S1 | 141.00 (14) | C4—C10—C9 | 116.9 (3) |
Ni—O1W—H11 | 125 (3) | C4—C10—C5 | 124.6 (4) |
Ni—O1W—H12 | 99 (3) | N1—C2—H2 | 119 |
H11—O1W—H12 | 104 (4) | C3—C2—H2 | 119 |
Ni—O2W—H21 | 131 (3) | C4—C3—H3 | 120 |
Ni—O2W—H22 | 128 (3) | C2—C3—H3 | 120 |
H21—O2W—H22 | 101 (4) | C3—C4—H4 | 120 |
Ni—O3W—H31 | 113 (4) | C10—C4—H4 | 120 |
H31—O3W—H32 | 104 (4) | C7—C6—H6 | 119 |
Ni—O3W—H32 | 132 (3) | C5—C6—H6 | 119 |
| | | |
O2W—Ni—O1—C8 | 95.6 (2) | O2—S1—C5—C6 | 115.7 (3) |
O3W—Ni—O1—C8 | −171.4 (2) | O2—S1—C5—C10 | −62.7 (4) |
N1—Ni—O1—C8 | 2.9 (2) | O3—S1—C5—C6 | −126.4 (3) |
O3i—Ni—O1—C8 | −87.3 (2) | O3—S1—C5—C10 | 55.2 (4) |
O1—Ni—N1—C2 | −177.8 (3) | O4—S1—C5—C6 | −4.4 (3) |
O1—Ni—N1—C9 | −3.9 (2) | O4—S1—C5—C10 | 177.2 (3) |
O1W—Ni—N1—C2 | 2.1 (3) | O2—S1—O3—Nii | −170.0 (2) |
O1W—Ni—N1—C9 | 176.0 (2) | O4—S1—O3—Nii | −42.4 (3) |
O2W—Ni—N1—C2 | 91.3 (3) | Ni—O1—C8—C7 | 178.1 (3) |
O2W—Ni—N1—C9 | −94.8 (2) | Ni—O1—C8—C9 | −1.5 (4) |
O3i—Ni—N1—C2 | −89.5 (3) | Ni—N1—C2—C3 | 173.2 (3) |
O3i—Ni—N1—C9 | 84.4 (2) | C9—N1—C2—C3 | −0.3 (5) |
O1—Ni—O3i—S1i | 136.1 (3) | Ni—N1—C9—C8 | 4.3 (4) |
O1W—Ni—O3i—S1i | −45.1 (3) | Ni—N1—C9—C10 | −175.3 (3) |
O3W—Ni—O3i—S1i | −129.2 (3) | C2—N1—C9—C8 | 178.8 (3) |
N1—Ni—O3i—S1i | 54.2 (3) | C2—N1—C9—C10 | −0.7 (5) |
O3i—Ni—O3W—H31 | −14 (3) | N1—C2—C3—C4 | 0.9 (6) |
O3i—Ni—O3W—H32 | −151 (4) | C2—C3—C4—C10 | −0.5 (6) |
O3i—Ni—O1W—H12 | −112 (3) | C3—C4—C10—C5 | −179.5 (4) |
O1—Ni—O2W—H21 | −152 (5) | C3—C4—C10—C9 | −0.5 (6) |
O1—Ni—O2W—H22 | 36 (5) | S1—C5—C6—C7 | −179.6 (3) |
O1W—Ni—O2W—H21 | 30 (5) | C10—C5—C6—C7 | −1.1 (5) |
O1W—Ni—O2W—H22 | −142 (5) | S1—C5—C10—C4 | −1.7 (6) |
O3W—Ni—O2W—H21 | 114 (5) | S1—C5—C10—C9 | 179.3 (3) |
O3W—Ni—O2W—H22 | −58 (5) | C6—C5—C10—C9 | 0.9 (5) |
N1—Ni—O2W—H21 | −70 (5) | C6—C5—C10—C4 | 179.9 (4) |
O2W—Ni—O1W—H11 | −48 (3) | C5—C6—C7—C8 | −0.2 (5) |
O2W—Ni—O1W—H12 | 66 (3) | C5—C6—C7—I1 | −179.0 (3) |
O3W—Ni—O1W—H11 | −141 (3) | C6—C7—C8—O1 | −177.8 (3) |
O3W—Ni—O1W—H12 | −27 (3) | I1—C7—C8—O1 | 1.0 (5) |
N1—Ni—O1W—H11 | 44 (3) | I1—C7—C8—C9 | −179.5 (3) |
N1—Ni—O1W—H12 | 158 (3) | C6—C7—C8—C9 | 1.8 (6) |
O3i—Ni—O1W—H11 | 134 (3) | C7—C8—C9—C10 | −2.0 (6) |
O2W—Ni—O3W—H32 | 29 (4) | C7—C8—C9—N1 | 178.5 (3) |
N1—Ni—O2W—H22 | 118 (5) | O1—C8—C9—N1 | −2.0 (5) |
O1—Ni—O3W—H31 | 74 (3) | O1—C8—C9—C10 | 177.6 (3) |
O1—Ni—O3W—H32 | −63 (4) | N1—C9—C10—C5 | −179.8 (3) |
O1W—Ni—O3W—H31 | −106 (3) | C8—C9—C10—C4 | −178.4 (4) |
O1W—Ni—O3W—H32 | 117 (4) | C8—C9—C10—C5 | 0.7 (6) |
O2W—Ni—O3W—H31 | 165 (3) | N1—C9—C10—C4 | 1.1 (6) |
C5—S1—O3—Nii | 75.2 (3) | | |
Symmetry codes: (i) −x+3/2, −y+1/2, −z; (ii) x, y+1, z; (iii) −x+3/2, −y+3/2, −z; (iv) −x+1, −y+1, −z; (v) −x+3/2, y+1/2, −z+1/2; (vi) x+1/2, y+1/2, z; (vii) −x+1, −y, −z; (viii) x−1/2, y−1/2, z; (ix) −x+3/2, y−1/2, −z+1/2; (x) x+1/2, −y+1/2, z+1/2; (xi) −x+1, y, −z+1/2; (xii) x, −y+1, z+1/2; (xiii) x−1/2, y+1/2, z; (xiv) x−1/2, −y+1/2, z−1/2; (xv) x, −y+1, z−1/2; (xvi) x+1/2, y−1/2, z; (xvii) −x+1, y, −z−1/2; (xviii) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11···O2ix | 0.94 (4) | 1.84 (4) | 2.779 (4) | 177 (5) |
O1W—H12···O4viii | 0.95 (3) | 2.15 (3) | 3.027 (4) | 155 (4) |
O2W—H21···O4ix | 0.96 (4) | 1.94 (4) | 2.856 (4) | 161 (3) |
O2W—H22···O4Wxi | 0.95 (4) | 1.93 (4) | 2.835 (4) | 160 (4) |
O3W—H31···O5W | 0.95 (2) | 1.86 (3) | 2.768 (4) | 160 (5) |
O3W—H32···O4W | 0.96 (5) | 1.80 (5) | 2.753 (4) | 172 (4) |
O4W—H41···O1iv | 0.95 (3) | 2.00 (3) | 2.947 (4) | 175 (4) |
O4W—H42···O5Wiv | 0.94 (5) | 1.93 (4) | 2.746 (4) | 143 (4) |
O5W—H51···I1iv | 0.93 (4) | 2.96 (4) | 3.555 (3) | 123 (4) |
O5W—H51···O1iv | 0.93 (4) | 2.04 (5) | 2.916 (4) | 156 (4) |
O5W—H52···O4Wiv | 0.94 (4) | 1.91 (4) | 2.746 (4) | 148 (5) |
C2—H2···I1xviii | 0.93 | 3.01 | 3.696 (4) | 132 |
C4—H4···O3 | 0.93 | 2.60 | 3.156 (5) | 119 |
C4—H4···O4Wxvi | 0.93 | 2.57 | 3.363 (5) | 144 |
C6—H6···O4 | 0.93 | 2.45 | 2.862 (4) | 107 |
C6—H6···I1iii | 0.93 | 3.02 | 3.751 (4) | 136 |
Symmetry codes: (iii) −x+3/2, −y+3/2, −z; (iv) −x+1, −y+1, −z; (viii) x−1/2, y−1/2, z; (ix) −x+3/2, y−1/2, −z+1/2; (xi) −x+1, y, −z+1/2; (xvi) x+1/2, y−1/2, z; (xviii) x, y−1, z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.