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catena-Poly[[[tetraaquanickel(II)]-μ-4,4′-bipyridine-κ2N:N′] thiosulfate dihydrate], {[Ni(C10H8N2)(H2O)4]S2O3·2H2O}n, (I), and catena-poly[[[tetraaquanickel(II)]-μ-4,4′-bipyridine-κ2N:N′] sulfate methanol solvate monohydrate], {[Ni(C10H8N2)(H2O)4]SO4·CH4O·H2O}n, (II), are built up of {[Ni(4,4′-bipy)(H2O)4]2+}n chains (4,4′-bipy is 4,4′-bipyridine) interwoven in an unusual P31 fashion. Voids are filled by the corresponding counter-anions and solvate molecules, defining a complex three-dimensional network surrounding them. In both structures, the cationic chains evolve around a set of twofold axes passing through the NiII ions and bisecting the aromatic amines through their N (and their opposite C) atoms.
Supporting information
CCDC references: 645513; 645514
For both compounds, data collection: SMART-NT (Bruker, 2001); cell refinement: SAINT-NT (Bruker, 2000); data reduction: SAINT-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-NT (Sheldrick, 2000); software used to prepare material for publication: SHELXTL-NT and PLATON (Spek, 2003).
(I)
catena-Poly[[[tetraaquanickel(II)]-µ-4,4'-bipyridine-
κ2N:
N'] thiosulfate dihydrate]
top
Crystal data top
[Ni(C10H8N2)(H2O)4]S2O3·2H2O | F(000) = 678 |
Mr = 435.11 | Dx = 1.746 Mg m−3 |
Hexagonal, P3121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 31 2" | µ = 1.47 mm−1 |
a = 11.3363 (9) Å | T = 274 K |
c = 11.1523 (13) Å | Needles, colourless |
V = 1241.2 (2) Å3 | 0.18 × 0.08 × 0.06 mm |
Z = 3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1907 independent reflections |
Radiation source: fine-focus sealed tube | 1725 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
φ and ω scans | θmax = 28.0°, θmin = 2.1° |
Absorption correction: multi-scan SADABS (Sheldrick, 2001) | h = −14→14 |
Tmin = 0.78, Tmax = 0.92 | k = −14→14 |
10484 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.082 | w = 1/[σ2(Fo2) + (0.0412P)2 + 0.57P] where P = (Fo2 + 2Fc2)/3 |
S = 0.98 | (Δ/σ)max = 0.004 |
1907 reflections | Δρmax = 0.52 e Å−3 |
153 parameters | Δρmin = −0.31 e Å−3 |
15 restraints | Absolute structure: Flack (1983), with how many Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (2) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 1.0000 | 0.60675 (4) | 1.1667 | 0.02801 (14) | |
O1W | 1.1959 (2) | 0.6991 (2) | 1.1020 (2) | 0.0395 (5) | |
H1WB | 1.209 (4) | 0.649 (3) | 1.055 (3) | 0.066 (13)* | |
H1WA | 1.269 (2) | 0.742 (4) | 1.142 (3) | 0.058 (13)* | |
O2W | 1.0791 (2) | 0.6516 (2) | 1.33982 (19) | 0.0415 (5) | |
H2WB | 1.153 (2) | 0.726 (2) | 1.346 (3) | 0.067 (13)* | |
H2WA | 1.067 (3) | 0.613 (3) | 1.4072 (17) | 0.051 (11)* | |
O3W | 0.6763 (3) | 0.4299 (4) | 0.7414 (3) | 0.0827 (11) | |
H3WB | 0.649 (4) | 0.476 (4) | 0.781 (4) | 0.088 (18)* | |
H3WA | 0.756 (2) | 0.488 (4) | 0.719 (5) | 0.107 (19)* | |
N1 | 1.0000 | 0.7946 (3) | 1.1667 | 0.0312 (7) | |
N2 | 1.0000 | 1.4214 (3) | 1.1667 | 0.0319 (7) | |
C1 | 0.8852 (3) | 0.8001 (3) | 1.1688 (3) | 0.0430 (8) | |
H1 | 0.8031 | 0.7182 | 1.1701 | 0.052* | |
C2 | 0.8805 (3) | 0.9185 (3) | 1.1693 (3) | 0.0413 (7) | |
H2 | 0.7968 | 0.9150 | 1.1715 | 0.050* | |
C3 | 1.0000 | 1.0435 (3) | 1.1667 | 0.0322 (9) | |
C4 | 1.0000 | 1.1750 (4) | 1.1667 | 0.0342 (9) | |
C5 | 0.8901 (3) | 1.1831 (3) | 1.1244 (3) | 0.0406 (7) | |
H5 | 0.8138 | 1.1061 | 1.0948 | 0.049* | |
C6 | 0.8947 (3) | 1.3074 (3) | 1.1267 (3) | 0.0412 (7) | |
H6 | 0.8193 | 1.3110 | 1.0984 | 0.049* | |
S1 | 0.98833 (19) | 0.44014 (16) | 0.69163 (13) | 0.0388 (4)* | 0.50 |
S2 | 0.9882 (2) | 0.60284 (18) | 0.62674 (14) | 0.0477 (4) | 0.50 |
O1 | 0.9453 (7) | 0.4222 (6) | 0.8165 (4) | 0.078 (2) | 0.50 |
O2 | 1.1256 (9) | 0.4590 (16) | 0.6800 (11) | 0.078 (4) | 0.50 |
O3 | 0.8935 (9) | 0.3208 (9) | 0.6206 (8) | 0.044 (2) | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0303 (3) | 0.02351 (18) | 0.0325 (2) | 0.01516 (15) | −0.0027 (2) | −0.00133 (12) |
O1W | 0.0394 (12) | 0.0334 (12) | 0.0460 (12) | 0.0184 (10) | 0.0053 (10) | −0.0006 (10) |
O2W | 0.0447 (13) | 0.0362 (12) | 0.0329 (12) | 0.0123 (11) | −0.0058 (9) | −0.0011 (9) |
O3W | 0.0427 (16) | 0.102 (3) | 0.0642 (19) | 0.0069 (18) | 0.0019 (14) | −0.0308 (19) |
N1 | 0.039 (2) | 0.0268 (12) | 0.0322 (17) | 0.0193 (10) | 0.0010 (16) | 0.0005 (8) |
N2 | 0.0353 (19) | 0.0257 (12) | 0.0380 (18) | 0.0177 (10) | −0.0083 (14) | −0.0042 (7) |
C1 | 0.0390 (17) | 0.0300 (16) | 0.062 (2) | 0.0191 (13) | −0.0019 (14) | 0.0019 (14) |
C2 | 0.0375 (17) | 0.0308 (16) | 0.059 (2) | 0.0195 (13) | −0.0029 (14) | −0.0010 (14) |
C3 | 0.040 (2) | 0.0277 (15) | 0.033 (2) | 0.0199 (12) | −0.0058 (17) | −0.0029 (8) |
C4 | 0.042 (2) | 0.0308 (16) | 0.033 (2) | 0.0211 (11) | −0.0058 (16) | −0.0029 (8) |
C5 | 0.0377 (17) | 0.0273 (14) | 0.0577 (19) | 0.0169 (13) | −0.0173 (15) | −0.0110 (13) |
C6 | 0.0418 (17) | 0.0331 (16) | 0.0556 (19) | 0.0239 (14) | −0.0163 (14) | −0.0087 (14) |
S2 | 0.0513 (10) | 0.0433 (8) | 0.0521 (9) | 0.0263 (8) | 0.0103 (10) | 0.0113 (7) |
O1 | 0.152 (7) | 0.053 (3) | 0.043 (3) | 0.062 (4) | 0.004 (3) | −0.001 (2) |
O2 | 0.049 (5) | 0.069 (8) | 0.132 (11) | 0.041 (5) | −0.015 (6) | −0.016 (7) |
O3 | 0.044 (3) | 0.042 (4) | 0.037 (3) | 0.016 (3) | 0.005 (2) | −0.001 (2) |
Geometric parameters (Å, º) top
Ni1—O1Wi | 2.055 (2) | N2—Ni1iii | 2.101 (3) |
Ni1—O1W | 2.055 (2) | C1—C2 | 1.370 (5) |
Ni1—O2W | 2.082 (2) | C1—H1 | 0.9300 |
Ni1—O2Wi | 2.082 (2) | C2—C3 | 1.388 (4) |
Ni1—N2ii | 2.101 (3) | C2—H2 | 0.9300 |
Ni1—N1 | 2.129 (3) | C3—C2i | 1.388 (4) |
O1W—H1WA | 0.85 (4) | C3—C4 | 1.490 (5) |
O1W—H1WB | 0.85 (4) | C4—C5i | 1.377 (4) |
O2W—H2WA | 0.85 (2) | C4—C5 | 1.377 (4) |
O2W—H2WB | 0.85 (2) | C5—C6 | 1.384 (4) |
O3W—H3WA | 0.85 (5) | C5—H5 | 0.9300 |
O3W—H3WB | 0.85 (5) | C6—H6 | 0.9300 |
N1—C1i | 1.334 (4) | S1—O1 | 1.456 (5) |
N1—C1 | 1.334 (4) | S1—O2 | 1.466 (6) |
N2—C6i | 1.324 (4) | S1—O3 | 1.470 (6) |
N2—C6 | 1.324 (4) | S1—S2 | 1.982 (2) |
| | | |
O1Wi—Ni1—O1W | 176.44 (13) | C6i—N2—Ni1iii | 121.69 (19) |
O2W—Ni1—O2Wi | 176.68 (14) | C6—N2—Ni1iii | 121.69 (19) |
N2ii—Ni1—N1 | 180.000 | N1—C1—C2 | 124.3 (3) |
O1Wi—Ni1—O2W | 91.43 (9) | N1—C1—H1 | 117.9 |
O1W—Ni1—O2Wi | 91.42 (9) | C2—C1—H1 | 117.9 |
O1W—Ni1—O2W | 88.68 (9) | C1—C2—C3 | 120.3 (3) |
O1Wi—Ni1—O2Wi | 88.68 (9) | C1—C2—H2 | 119.9 |
O1W—Ni1—N2ii | 88.22 (6) | C3—C2—H2 | 119.9 |
O1Wi—Ni1—N2ii | 88.22 (6) | C2—C3—C2i | 115.5 (4) |
O2W—Ni1—N2ii | 91.66 (7) | C2—C3—C4 | 122.2 (2) |
O2Wi—Ni1—N2ii | 91.66 (7) | C2i—C3—C4 | 122.2 (2) |
O1W—Ni1—N1 | 91.78 (6) | C5i—C4—C5 | 117.4 (4) |
O1Wi—Ni1—N1 | 91.78 (6) | C5i—C4—C3 | 121.28 (19) |
O2W—Ni1—N1 | 88.34 (7) | C5—C4—C3 | 121.28 (19) |
O2Wi—Ni1—N1 | 88.34 (7) | C4—C5—C6 | 119.2 (3) |
Ni1—O1W—H1WB | 113 (3) | C4—C5—H5 | 120.4 |
Ni1—O1W—H1WA | 127 (3) | C6—C5—H5 | 120.4 |
H1WB—O1W—H1WA | 106 (2) | N2—C6—C5 | 123.8 (3) |
Ni1—O2W—H2WB | 115 (2) | N2—C6—H6 | 118.1 |
Ni1—O2W—H2WA | 139 (2) | C5—C6—H6 | 118.1 |
H2WB—O2W—H2WA | 105 (2) | O1—S1—O2 | 111.2 (5) |
H3WB—O3W—H3WA | 104 (2) | O1—S1—O3 | 110.3 (4) |
C1i—N1—C1 | 115.4 (4) | O2—S1—O3 | 108.7 (4) |
C1i—N1—Ni1 | 122.31 (19) | O1—S1—S2 | 108.8 (2) |
C1—N1—Ni1 | 122.3 (2) | O2—S1—S2 | 109.0 (5) |
C6i—N2—C6 | 116.6 (4) | O3—S1—S2 | 108.6 (6) |
Symmetry codes: (i) −x+2, −x+y+1, −z+7/3; (ii) x, y−1, z; (iii) x, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O1iv | 0.85 (4) | 2.13 (2) | 2.835 (7) | 140 (4) |
O1W—H1WB···O3Wv | 0.85 (4) | 1.85 (2) | 2.681 (4) | 167 (4) |
O2W—H2WA···O1i | 0.85 (2) | 1.91 (2) | 2.710 (5) | 156 (3) |
O2W—H2WA···S2vi | 0.85 (2) | 2.59 (2) | 3.322 (3) | 146 (3) |
O2W—H2WB···O2vii | 0.85 (2) | 1.88 (2) | 2.723 (7) | 169 (4) |
O2W—H2WB···O3iv | 0.85 (2) | 1.93 (2) | 2.776 (7) | 174 (3) |
O3W—H3WA···S2 | 0.85 (5) | 2.50 (2) | 3.324 (4) | 164 (4) |
O3W—H3WA···S2viii | 0.85 (5) | 2.51 (2) | 3.322 (4) | 160 (5) |
O3W—H3WB···O3ix | 0.85 (5) | 2.16 (2) | 2.862 (13) | 140 (5) |
O3W—H3WB···O2x | 0.85 (5) | 2.39 (2) | 3.037 (14) | 134 (5) |
O3W—H3WB···O1x | 0.85 (5) | 2.37 (2) | 3.196 (8) | 164 (5) |
Symmetry codes: (i) −x+2, −x+y+1, −z+7/3; (iv) y+1, x, −z+2; (v) x−y+1, −y+1, −z+5/3; (vi) x, y, z+1; (vii) −x+y+2, −x+2, z+2/3; (viii) −x+2, −x+y+1, −z+4/3; (ix) −y+1, x−y, z+1/3; (x) x−y, −y+1, −z+5/3. |
(II)
catena-poly[[[tetraaquanickel(II)]-µ-4,4'-bipyridine-
κ2N:
N'] sulfate methanol solvate monohydrate
top
Crystal data top
[Ni(C10H8N2)(H2O)4]SO4·CH4O·H2O | Dx = 1.652 Mg m−3 |
Mr = 433.08 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P3121 | Cell parameters from 2570 reflections |
Hall symbol: P 31 2" | θ = 2.3–21.6° |
a = 11.2916 (10) Å | µ = 1.29 mm−1 |
c = 23.660 (3) Å | T = 273 K |
V = 2612.5 (5) Å3 | Block, green |
Z = 6 | 0.16 × 0.12 × 0.10 mm |
F(000) = 1356 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 3968 independent reflections |
Radiation source: fine-focus sealed tube | 2906 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.076 |
φ and ω scans | θmax = 28.4°, θmin = 2.1° |
Absorption correction: multi-scan SADABS (Sheldrick, 2001) | h = −14→7 |
Tmin = 0.82, Tmax = 0.88 | k = 0→14 |
21995 measured reflections | l = 0→31 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.068 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.144 | w = 1/[σ2(Fo2) + (0.0429P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.017 |
3968 reflections | Δρmax = 0.92 e Å−3 |
265 parameters | Δρmin = −0.49 e Å−3 |
27 restraints | Absolute structure: Flack (1983), with how many Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.01 (3) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.47361 (8) | 0.47361 (8) | 0.0000 | 0.0259 (2) | |
Ni2 | 1.0000 | 0.61953 (8) | 0.1667 | 0.0287 (3) | |
O1W | 0.5759 (4) | 0.3648 (4) | 0.01093 (17) | 0.0382 (10) | |
H1WA | 0.597 (6) | 0.341 (5) | −0.0203 (11) | 0.046* | |
H1WB | 0.559 (6) | 0.309 (5) | 0.0364 (15) | 0.046* | |
O2W | 0.4537 (4) | 0.4910 (4) | 0.08618 (15) | 0.0351 (9) | |
H2WA | 0.498 (5) | 0.469 (5) | 0.1086 (13) | 0.042* | |
H2WB | 0.459 (6) | 0.566 (4) | 0.0975 (14) | 0.042* | |
O3W | 1.1013 (4) | 0.6746 (5) | 0.09014 (16) | 0.0415 (10) | |
H3WA | 1.185 (2) | 0.702 (6) | 0.0928 (16) | 0.050* | |
H3WB | 1.061 (4) | 0.613 (4) | 0.0656 (14) | 0.050* | |
O4W | 0.8229 (4) | 0.5262 (4) | 0.12045 (16) | 0.0338 (9) | |
H4WA | 0.822 (4) | 0.470 (4) | 0.0978 (18) | 0.041* | |
H4WB | 0.750 (2) | 0.500 (5) | 0.1379 (16) | 0.041* | |
N1 | 0.2874 (6) | 0.2874 (6) | 0.0000 | 0.0303 (16) | |
N2 | −0.3394 (5) | −0.3394 (5) | 0.0000 | 0.0265 (14) | |
C1 | 0.2636 (6) | 0.1858 (6) | 0.0362 (2) | 0.0355 (14) | |
H1 | 0.3317 | 0.1999 | 0.0619 | 0.043* | |
C2 | 0.1443 (6) | 0.0629 (6) | 0.0370 (2) | 0.0327 (13) | |
H2 | 0.1334 | −0.0048 | 0.0623 | 0.039* | |
C3 | 0.0395 (7) | 0.0395 (7) | 0.0000 | 0.0273 (17) | |
C4 | −0.0910 (7) | −0.0910 (7) | 0.0000 | 0.0280 (18) | |
C5 | −0.0949 (6) | −0.2149 (6) | 0.0046 (3) | 0.0394 (15) | |
H5 | −0.0142 | −0.2175 | 0.0084 | 0.047* | |
C6 | −0.2181 (6) | −0.3336 (6) | 0.0037 (3) | 0.0371 (15) | |
H6 | −0.2178 | −0.4157 | 0.0058 | 0.045* | |
N3 | 1.0000 | 0.4318 (6) | 0.1667 | 0.0308 (16) | |
N4 | 1.0000 | −0.1937 (5) | 0.1667 | 0.0265 (15) | |
C7 | 0.8866 (6) | 0.3138 (6) | 0.1775 (3) | 0.0366 (14) | |
H7 | 0.8065 | 0.3151 | 0.1850 | 0.044* | |
C8 | 0.8827 (6) | 0.1901 (6) | 0.1782 (3) | 0.0373 (14) | |
H8 | 0.8014 | 0.1102 | 0.1864 | 0.045* | |
C9 | 1.0000 | 0.1848 (7) | 0.1667 | 0.0313 (18) | |
C10 | 1.0000 | 0.0532 (7) | 0.1667 | 0.0301 (19) | |
C11 | 0.8860 (6) | −0.0673 (6) | 0.1504 (2) | 0.0343 (14) | |
H11 | 0.8072 | −0.0679 | 0.1386 | 0.041* | |
C12 | 0.8910 (6) | −0.1869 (6) | 0.1518 (2) | 0.0344 (14) | |
H12 | 0.8126 | −0.2677 | 0.1418 | 0.041* | |
S1 | 0.47343 (15) | 0.81912 (15) | 0.11549 (6) | 0.0339 (3) | |
O1 | 0.5609 (5) | 0.9420 (4) | 0.08333 (18) | 0.0541 (13) | |
O2 | 0.3578 (5) | 0.7229 (5) | 0.07953 (18) | 0.0521 (13) | |
O3 | 0.5473 (5) | 0.7520 (5) | 0.1335 (2) | 0.0536 (12) | |
O4 | 0.4162 (5) | 0.8533 (5) | 0.16479 (18) | 0.0513 (13) | |
O1M | 0.4572 (6) | 0.9252 (6) | −0.0248 (2) | 0.0597 (14) | |
H1M | 0.500 (7) | 0.928 (8) | 0.005 (2) | 0.072* | |
C1M | 0.3325 (11) | 0.9186 (12) | −0.0222 (3) | 0.102 (4) | |
H1MA | 0.3460 | 1.0090 | −0.0173 | 0.153* | |
H1MB | 0.2812 | 0.8624 | 0.0092 | 0.153* | |
H1MC | 0.2830 | 0.8799 | −0.0566 | 0.153* | |
O5W | 0.5600 (8) | 1.1908 (6) | 0.0927 (2) | 0.0737 (18) | |
H5WA | 0.541 (9) | 1.215 (8) | 0.1242 (18) | 0.088* | |
H5WB | 0.569 (9) | 1.121 (6) | 0.099 (3) | 0.088* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0226 (4) | 0.0226 (4) | 0.0302 (5) | 0.0096 (4) | −0.0006 (2) | 0.0006 (2) |
Ni2 | 0.0298 (6) | 0.0231 (4) | 0.0353 (6) | 0.0149 (3) | 0.0011 (4) | 0.0005 (2) |
O1W | 0.044 (3) | 0.041 (3) | 0.038 (2) | 0.028 (2) | 0.008 (2) | 0.008 (2) |
O2W | 0.041 (3) | 0.036 (2) | 0.030 (2) | 0.021 (2) | −0.0067 (18) | −0.0042 (17) |
O3W | 0.041 (3) | 0.045 (3) | 0.042 (2) | 0.024 (2) | 0.004 (2) | 0.003 (2) |
O4W | 0.034 (2) | 0.030 (2) | 0.041 (2) | 0.0182 (19) | −0.0034 (18) | −0.0089 (18) |
N1 | 0.030 (3) | 0.030 (3) | 0.033 (4) | 0.016 (3) | −0.0024 (14) | 0.0024 (14) |
N2 | 0.023 (2) | 0.023 (2) | 0.031 (3) | 0.009 (3) | −0.0037 (14) | 0.0037 (14) |
C1 | 0.030 (3) | 0.035 (3) | 0.037 (3) | 0.013 (3) | −0.001 (2) | 0.003 (3) |
C2 | 0.030 (3) | 0.031 (3) | 0.038 (3) | 0.016 (3) | 0.001 (3) | 0.007 (2) |
C3 | 0.025 (3) | 0.025 (3) | 0.035 (4) | 0.014 (4) | 0.0019 (17) | −0.0019 (17) |
C4 | 0.024 (3) | 0.024 (3) | 0.029 (4) | 0.007 (4) | 0.0009 (17) | −0.0009 (17) |
C5 | 0.026 (3) | 0.033 (3) | 0.062 (4) | 0.017 (3) | 0.000 (3) | 0.000 (3) |
C6 | 0.032 (3) | 0.025 (3) | 0.057 (4) | 0.015 (3) | −0.003 (3) | 0.000 (3) |
N3 | 0.035 (4) | 0.022 (3) | 0.039 (4) | 0.018 (2) | 0.007 (3) | 0.0036 (16) |
N4 | 0.026 (4) | 0.023 (2) | 0.032 (4) | 0.0128 (19) | 0.006 (3) | 0.0030 (13) |
C7 | 0.029 (3) | 0.031 (3) | 0.055 (4) | 0.018 (3) | 0.005 (3) | −0.003 (3) |
C8 | 0.033 (3) | 0.025 (3) | 0.055 (4) | 0.015 (3) | 0.005 (3) | 0.002 (3) |
C9 | 0.037 (5) | 0.027 (3) | 0.034 (4) | 0.019 (2) | 0.002 (4) | 0.0012 (18) |
C10 | 0.036 (5) | 0.031 (3) | 0.026 (4) | 0.018 (2) | 0.010 (3) | 0.0052 (17) |
C11 | 0.035 (3) | 0.027 (3) | 0.045 (4) | 0.018 (3) | 0.001 (3) | −0.002 (3) |
C12 | 0.036 (3) | 0.026 (3) | 0.041 (3) | 0.015 (3) | −0.001 (3) | −0.004 (3) |
S1 | 0.0326 (8) | 0.0312 (8) | 0.0369 (8) | 0.0151 (6) | 0.0022 (6) | −0.0004 (6) |
O1 | 0.054 (3) | 0.041 (3) | 0.063 (3) | 0.020 (2) | 0.022 (3) | 0.008 (2) |
O2 | 0.047 (3) | 0.058 (3) | 0.050 (3) | 0.025 (2) | −0.009 (2) | −0.029 (2) |
O3 | 0.048 (3) | 0.054 (3) | 0.064 (3) | 0.030 (3) | −0.001 (2) | 0.007 (2) |
O4 | 0.043 (3) | 0.048 (3) | 0.043 (3) | 0.007 (2) | 0.007 (2) | −0.016 (2) |
O1M | 0.080 (4) | 0.077 (4) | 0.048 (3) | 0.059 (3) | 0.014 (3) | 0.011 (3) |
C1M | 0.132 (9) | 0.166 (12) | 0.059 (5) | 0.113 (9) | 0.031 (6) | 0.037 (6) |
O5W | 0.137 (6) | 0.073 (4) | 0.046 (3) | 0.079 (4) | 0.019 (3) | 0.014 (3) |
Geometric parameters (Å, º) top
Ni1—O2Wi | 2.072 (4) | C4—C5 | 1.382 (7) |
Ni1—O2W | 2.072 (4) | C5—C6 | 1.367 (9) |
Ni1—O1W | 2.081 (4) | C5—H5 | 0.9300 |
Ni1—O1Wi | 2.081 (4) | C6—H6 | 0.9300 |
Ni1—N1 | 2.103 (6) | N3—C7 | 1.332 (6) |
Ni1—N2ii | 2.112 (6) | N3—C7iii | 1.332 (6) |
Ni2—O4Wiii | 2.049 (4) | N4—C12iii | 1.319 (7) |
Ni2—O4W | 2.049 (4) | N4—C12 | 1.319 (7) |
Ni2—O3Wiii | 2.064 (4) | C7—C8 | 1.376 (8) |
Ni2—O3W | 2.064 (4) | C7—H7 | 0.9300 |
Ni2—N4iv | 2.109 (6) | C8—C9 | 1.383 (7) |
Ni2—N3 | 2.120 (6) | C8—H8 | 0.9300 |
O1W—H1WA | 0.86 (4) | C9—C8iii | 1.383 (7) |
O1W—H1WB | 0.82 (4) | C9—C10 | 1.486 (11) |
O2W—H2WA | 0.85 (4) | C10—C11iii | 1.380 (7) |
O2W—H2WB | 0.86 (4) | C10—C11 | 1.380 (7) |
O3W—H3WA | 0.83 (4) | C11—C12 | 1.380 (8) |
O3W—H3WB | 0.84 (4) | C11—H11 | 0.9300 |
O4W—H4WA | 0.82 (4) | C12—H12 | 0.9300 |
O4W—H4WB | 0.83 (4) | S1—O3 | 1.444 (5) |
N1—C1i | 1.347 (6) | S1—O1 | 1.452 (4) |
N1—C1 | 1.347 (6) | S1—O4 | 1.475 (4) |
N2—C6 | 1.341 (7) | S1—O2 | 1.480 (4) |
N2—C6i | 1.341 (6) | O1M—C1M | 1.374 (10) |
C1—C2 | 1.368 (7) | O1M—H1M | 0.84 (5) |
C1—H1 | 0.9300 | C1M—H1MA | 0.9600 |
C2—C3 | 1.387 (7) | C1M—H1MB | 0.9600 |
C2—H2 | 0.9300 | C1M—H1MC | 0.9600 |
C3—C2i | 1.387 (7) | O5W—H5WA | 0.86 (5) |
C3—C4 | 1.474 (10) | O5W—H5WB | 0.86 (5) |
C4—C5i | 1.382 (7) | | |
| | | |
O2Wi—Ni1—O2W | 179.2 (2) | C1—C2—H2 | 120.1 |
O2Wi—Ni1—O1W | 86.98 (15) | C3—C2—H2 | 120.1 |
O2W—Ni1—O1W | 93.01 (15) | C2—C3—C2i | 117.1 (7) |
O2Wi—Ni1—O1Wi | 93.01 (15) | C2—C3—C4 | 121.4 (4) |
O2W—Ni1—O1Wi | 86.98 (15) | C2i—C3—C4 | 121.4 (4) |
O1W—Ni1—O1Wi | 178.0 (2) | C5i—C4—C5 | 117.1 (7) |
O2Wi—Ni1—N1 | 89.61 (11) | C5i—C4—C3 | 121.4 (4) |
O2W—Ni1—N1 | 89.61 (11) | C5—C4—C3 | 121.4 (4) |
O1W—Ni1—N1 | 88.99 (12) | C6—C5—C4 | 119.5 (6) |
O1Wi—Ni1—N1 | 88.99 (12) | C6—C5—H5 | 120.2 |
O2Wi—Ni1—N2ii | 90.39 (11) | C4—C5—H5 | 120.2 |
O2W—Ni1—N2ii | 90.39 (11) | N2—C6—C5 | 124.2 (6) |
O1W—Ni1—N2ii | 91.01 (12) | N2—C6—H6 | 117.9 |
O1Wi—Ni1—N2ii | 91.01 (12) | C5—C6—H6 | 117.9 |
N1—Ni1—N2ii | 180.0 | C7—N3—C7iii | 117.4 (7) |
O4Wiii—Ni2—O4W | 177.0 (2) | C7—N3—Ni2 | 121.3 (4) |
O4Wiii—Ni2—O3Wiii | 86.45 (16) | C7iii—N3—Ni2 | 121.3 (4) |
O4W—Ni2—O3Wiii | 93.63 (16) | C12iii—N4—C12 | 116.6 (7) |
O4Wiii—Ni2—O3W | 93.63 (16) | C12iii—N4—Ni2vi | 121.7 (4) |
O4W—Ni2—O3W | 86.45 (16) | C12—N4—Ni2vi | 121.7 (4) |
O3Wiii—Ni2—O3W | 177.2 (2) | N3—C7—C8 | 123.0 (6) |
O4Wiii—Ni2—N4iv | 91.51 (11) | N3—C7—H7 | 118.5 |
O4W—Ni2—N4iv | 91.51 (11) | C8—C7—H7 | 118.5 |
O3Wiii—Ni2—N4iv | 88.61 (12) | C7—C8—C9 | 119.7 (6) |
O3W—Ni2—N4iv | 88.61 (12) | C7—C8—H8 | 120.1 |
O4Wiii—Ni2—N3 | 88.49 (11) | C9—C8—H8 | 120.1 |
O4W—Ni2—N3 | 88.49 (11) | C8—C9—C8iii | 117.1 (8) |
O3Wiii—Ni2—N3 | 91.39 (12) | C8—C9—C10 | 121.5 (4) |
O3W—Ni2—N3 | 91.39 (12) | C8iii—C9—C10 | 121.5 (4) |
N4iv—Ni2—N3 | 180.000 (2) | C11iii—C10—C11 | 117.4 (8) |
Ni1—O1W—H1WA | 114 (2) | C11iii—C10—C9 | 121.3 (4) |
Ni1—O1W—H1WB | 124 (3) | C11—C10—C9 | 121.3 (4) |
H1WA—O1W—H1WB | 112 (5) | C12—C11—C10 | 118.9 (6) |
Ni1—O2W—H2WA | 118 (3) | C12—C11—H11 | 120.5 |
Ni1—O2W—H2WB | 116 (3) | C10—C11—H11 | 120.5 |
H2WA—O2W—H2WB | 109 (5) | N4—C12—C11 | 124.0 (6) |
Ni2—O3W—H3WA | 114 (3) | N4—C12—H12 | 118.0 |
Ni2—O3W—H3WB | 111 (3) | C11—C12—H12 | 118.0 |
H3WA—O3W—H3WB | 114 (5) | O3—S1—O1 | 111.1 (3) |
Ni2—O4W—H4WA | 112 (3) | O3—S1—O4 | 110.3 (3) |
Ni2—O4W—H4WB | 117 (3) | O1—S1—O4 | 110.0 (3) |
H4WA—O4W—H4WB | 115 (5) | O3—S1—O2 | 108.3 (3) |
C1i—N1—C1 | 116.6 (7) | O1—S1—O2 | 109.2 (3) |
C1i—N1—Ni1 | 121.7 (3) | O4—S1—O2 | 107.8 (3) |
C1—N1—Ni1 | 121.7 (3) | C1M—O1M—H1M | 121 (6) |
C6—N2—C6i | 115.3 (7) | O1M—C1M—H1MA | 109.5 |
C6—N2—Ni1v | 122.3 (3) | O1M—C1M—H1MB | 109.5 |
C6i—N2—Ni1v | 122.3 (3) | H1MA—C1M—H1MB | 109.5 |
N1—C1—C2 | 123.3 (6) | O1M—C1M—H1MC | 109.5 |
N1—C1—H1 | 118.4 | H1MA—C1M—H1MC | 109.5 |
C2—C1—H1 | 118.4 | H1MB—C1M—H1MC | 109.5 |
C1—C2—C3 | 119.9 (6) | H5WA—O5W—H5WB | 108 (5) |
Symmetry codes: (i) y, x, −z; (ii) x+1, y+1, z; (iii) −x+2, −x+y+1, −z+1/3; (iv) x, y+1, z; (v) x−1, y−1, z; (vi) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2i | 0.86 (4) | 1.93 (4) | 2.734 (6) | 154 (6) |
O1W—H1WB···O5Wvi | 0.82 (4) | 1.89 (4) | 2.699 (6) | 168 (5) |
O2W—H2WA···O4vii | 0.85 (4) | 1.85 (4) | 2.687 (5) | 168 (4) |
O2W—H2WB···O3 | 0.86 (4) | 2.01 (4) | 2.818 (6) | 156 (5) |
O3W—H3WA···O2viii | 0.83 (4) | 1.87 (4) | 2.678 (6) | 161 (5) |
O3W—H3WB···O1Mi | 0.84 (4) | 1.92 (4) | 2.736 (7) | 163 (4) |
O4W—H4WA···O1Mi | 0.82 (4) | 2.13 (4) | 2.822 (6) | 141 (5) |
O4W—H4WB···O4vii | 0.83 (4) | 1.79 (4) | 2.623 (6) | 174 (4) |
O1M—H1M···O1 | 0.84 (5) | 1.96 (5) | 2.781 (7) | 164 (8) |
O5W—H5WA···O3ix | 0.86 (5) | 2.02 (5) | 2.846 (7) | 161 (8) |
O5W—H5WB···O1 | 0.86 (5) | 2.01 (5) | 2.823 (7) | 158 (7) |
Symmetry codes: (i) y, x, −z; (vi) x, y−1, z; (vii) −x+1, −x+y, −z+1/3; (viii) x+1, y, z; (ix) −x+1, −x+y+1, −z+1/3. |
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