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metal-organic compounds
Tetrakis{μ3-2-[(2-hydroxyethyl)amino]ethanolato}tetrakis[chloridonickel(II)] methanol solvate
aDepartment of Chemistry and Environmental Engineering, Anyang Institute of Technology, Henan 455000, People's Republic of China, and bCollege of Chemistry and Chemical Engineering, Liaocheng University, Shandong 252059, People's Republic of China
*Correspondence e-mail: lidacheng@lcu.edu.cn
The complex molecule of the title compound, [Ni4(C4H10NO2)4Cl4]·CH3OH, consists of a cubane-like {Ni4O4} core in which each nickel(II) atom is six-coordinated in a distorted octahedral geometry by one N and four O atoms of three mono-deprotonated diethanolamine ligands and by a chloride anion. The molecular conformation is stabilized by intramolecular O—H⋯Cl bonds. In the complex molecules and methanol solvent molecules are linked into a three-dimensional network by N—H⋯Cl, N—H⋯O and O—H⋯Cl hydrogen-bonding interactions.
Related literature
For the magnetic properties and structures of related compounds, see: Cadiou et al. (2001); Ferguson et al. (2008
).
Experimental
Crystal data
|
Refinement
|
|
Data collection: SMART (Siemens, 1996); cell SAINT (Siemens, 1996
); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008
); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008
); molecular graphics: SHELXTL (Sheldrick, 2008
); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536810024384/rz2468sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536810024384/rz2468Isup2.hkl
To a stirred methanol solution (15 ml) of NiCl2.6H2O (2 mmol, 475 mg) was added diethanolamine (4 mmol, 421 mg) in 5 ml methanol. After 10 min NaOAc was added and the mixture stirred for 6 h. The resulting blue solution was filtrated and was allowed to stand at room temperature for about one week, whereupon blue block crystals suitable for X-ray
were obtained.All H atoms were placed in geometrically idealized positions and treated as riding on their parent atoms, with C—H = 0.96-0.97 Å, N—H = 0.91 Å, O—H = 0.82 Å, and with Uiso(H) = 1.2Ueq(C, N) or 1.5Ueq(C, O) for methyl and hydroxy H atoms.
Data collection: SMART (Siemens, 1996); cell
SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008). ![]() | Fig. 1. The molecular structure of the title compound, with atom labels and 30% probability displacement ellipsoids. Hydrogen atoms are omitted for clarity. |
[Ni4(C4H10NO2)4Cl4]·CH4O | Z = 2 |
Mr = 825.20 | F(000) = 852 |
Triclinic, P1 | Dx = 1.773 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.8244 (12) Å | Cell parameters from 2996 reflections |
b = 11.5609 (13) Å | θ = 2.4–28.3° |
c = 13.2797 (17) Å | µ = 2.79 mm−1 |
α = 91.741 (1)° | T = 298 K |
β = 91.845 (1)° | Block, blue |
γ = 111.283 (2)° | 0.39 × 0.25 × 0.15 mm |
V = 1546.1 (3) Å3 |
Bruker SMART 1000 CCD diffractometer | 5352 independent reflections |
Radiation source: fine-focus sealed tube | 3889 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
phi and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→12 |
Tmin = 0.409, Tmax = 0.680 | k = −13→13 |
8045 measured reflections | l = −13→15 |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.141 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.085P)2] where P = (Fo2 + 2Fc2)/3 |
5352 reflections | (Δ/σ)max = 0.001 |
344 parameters | Δρmax = 1.01 e Å−3 |
0 restraints | Δρmin = −0.74 e Å−3 |
[Ni4(C4H10NO2)4Cl4]·CH4O | γ = 111.283 (2)° |
Mr = 825.20 | V = 1546.1 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.8244 (12) Å | Mo Kα radiation |
b = 11.5609 (13) Å | µ = 2.79 mm−1 |
c = 13.2797 (17) Å | T = 298 K |
α = 91.741 (1)° | 0.39 × 0.25 × 0.15 mm |
β = 91.845 (1)° |
Bruker SMART 1000 CCD diffractometer | 5352 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3889 reflections with I > 2σ(I) |
Tmin = 0.409, Tmax = 0.680 | Rint = 0.025 |
8045 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 0 restraints |
wR(F2) = 0.141 | H-atom parameters constrained |
S = 1.01 | Δρmax = 1.01 e Å−3 |
5352 reflections | Δρmin = −0.74 e Å−3 |
344 parameters |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.28194 (7) | 0.64164 (6) | 0.10224 (5) | 0.0256 (2) | |
Ni2 | 0.35928 (7) | 0.55768 (6) | 0.30672 (5) | 0.0258 (2) | |
Ni3 | 0.25126 (7) | 0.77201 (6) | 0.31177 (5) | 0.0250 (2) | |
Ni4 | 0.52684 (7) | 0.82657 (6) | 0.22639 (5) | 0.0252 (2) | |
Cl4 | 0.65383 (15) | 0.88748 (14) | 0.08011 (11) | 0.0391 (4) | |
Cl1 | 0.17830 (15) | 0.43190 (14) | 0.03338 (12) | 0.0399 (4) | |
Cl3 | 0.30181 (15) | 0.98516 (14) | 0.36147 (11) | 0.0381 (4) | |
Cl2 | 0.28239 (14) | 0.49380 (14) | 0.47358 (11) | 0.0375 (4) | |
O1 | 0.3416 (3) | 0.8145 (3) | 0.1730 (3) | 0.0234 (8) | |
O3 | 0.2025 (3) | 0.5972 (3) | 0.2474 (3) | 0.0238 (8) | |
O7 | 0.4270 (3) | 0.7491 (3) | 0.3498 (2) | 0.0228 (8) | |
O5 | 0.4480 (3) | 0.6348 (3) | 0.1788 (3) | 0.0252 (8) | |
O4 | 0.1916 (4) | 0.7173 (4) | 0.4608 (3) | 0.0370 (10) | |
H4 | 0.2120 | 0.6559 | 0.4656 | 0.055* | |
O8 | 0.5626 (4) | 1.0166 (4) | 0.2700 (3) | 0.0379 (10) | |
H8 | 0.4914 | 1.0069 | 0.2950 | 0.057* | |
O2 | 0.4041 (4) | 0.6984 (4) | −0.0261 (3) | 0.0351 (10) | |
H2 | 0.4681 | 0.7497 | 0.0051 | 0.053* | |
N1 | 0.1626 (5) | 0.7099 (4) | 0.0125 (3) | 0.0319 (11) | |
H1 | 0.0760 | 0.6598 | 0.0164 | 0.038* | |
N3 | 0.5163 (5) | 0.4904 (4) | 0.3159 (4) | 0.0346 (12) | |
H3 | 0.5644 | 0.5204 | 0.3747 | 0.042* | |
C2 | 0.1813 (5) | 0.8351 (5) | 0.0534 (4) | 0.0330 (14) | |
H2A | 0.1120 | 0.8292 | 0.0997 | 0.040* | |
H2B | 0.1725 | 0.8856 | −0.0014 | 0.040* | |
C13 | 0.5074 (5) | 0.7992 (5) | 0.4385 (4) | 0.0304 (13) | |
H13A | 0.4723 | 0.7465 | 0.4942 | 0.036* | |
H13B | 0.5065 | 0.8811 | 0.4553 | 0.036* | |
O6 | 0.2621 (4) | 0.3722 (4) | 0.2390 (3) | 0.0406 (10) | |
H6 | 0.2429 | 0.3795 | 0.2975 | 0.061* | |
C10 | 0.6016 (6) | 0.5390 (6) | 0.2315 (5) | 0.0361 (14) | |
H10A | 0.6386 | 0.4784 | 0.2089 | 0.043* | |
H10B | 0.6746 | 0.6141 | 0.2544 | 0.043* | |
C9 | 0.5254 (6) | 0.5683 (5) | 0.1428 (4) | 0.0302 (13) | |
H9A | 0.5875 | 0.6174 | 0.0955 | 0.036* | |
H9B | 0.4684 | 0.4916 | 0.1080 | 0.036* | |
C1 | 0.3169 (5) | 0.8993 (5) | 0.1086 (4) | 0.0281 (13) | |
H1A | 0.3857 | 0.9264 | 0.0601 | 0.034* | |
H1B | 0.3174 | 0.9718 | 0.1476 | 0.034* | |
C16 | 0.7654 (6) | 1.0042 (6) | 0.3340 (5) | 0.0452 (17) | |
H16A | 0.8152 | 1.0312 | 0.2741 | 0.054* | |
H16B | 0.8278 | 1.0264 | 0.3919 | 0.054* | |
C8 | −0.0011 (6) | 0.7483 (6) | 0.3952 (5) | 0.0368 (15) | |
H8A | −0.0974 | 0.7151 | 0.3936 | 0.044* | |
H8B | 0.0290 | 0.8364 | 0.4134 | 0.044* | |
N4 | 0.6958 (5) | 0.8668 (5) | 0.3262 (4) | 0.0351 (12) | |
H4AA | 0.7511 | 0.8319 | 0.2995 | 0.042* | |
N2 | 0.0443 (4) | 0.7305 (4) | 0.2953 (3) | 0.0320 (11) | |
H2AA | 0.0296 | 0.7855 | 0.2535 | 0.038* | |
C12 | 0.4551 (6) | 0.3542 (6) | 0.3186 (5) | 0.0414 (16) | |
H12A | 0.4176 | 0.3316 | 0.3838 | 0.050* | |
H12B | 0.5224 | 0.3181 | 0.3098 | 0.050* | |
C4 | 0.2032 (6) | 0.7055 (6) | −0.0929 (4) | 0.0411 (16) | |
H4A | 0.1636 | 0.7514 | −0.1346 | 0.049* | |
H4B | 0.1705 | 0.6199 | −0.1189 | 0.049* | |
C14 | 0.6484 (6) | 0.8081 (6) | 0.4222 (4) | 0.0335 (14) | |
H14A | 0.7062 | 0.8568 | 0.4778 | 0.040* | |
H14B | 0.6522 | 0.7256 | 0.4213 | 0.040* | |
C6 | −0.0179 (5) | 0.6034 (5) | 0.2479 (5) | 0.0353 (14) | |
H6A | −0.0319 | 0.6093 | 0.1760 | 0.042* | |
H6B | −0.1039 | 0.5624 | 0.2758 | 0.042* | |
C3 | 0.3516 (6) | 0.7598 (6) | −0.0988 (4) | 0.0405 (16) | |
H3A | 0.3773 | 0.7455 | −0.1660 | 0.049* | |
H3B | 0.3845 | 0.8486 | −0.0832 | 0.049* | |
C7 | 0.0525 (6) | 0.6830 (6) | 0.4735 (5) | 0.0420 (16) | |
H7A | 0.0370 | 0.7080 | 0.5409 | 0.050* | |
H7B | 0.0083 | 0.5937 | 0.4643 | 0.050* | |
C5 | 0.0676 (5) | 0.5254 (5) | 0.2648 (5) | 0.0356 (14) | |
H5A | 0.0602 | 0.4979 | 0.3334 | 0.043* | |
H5B | 0.0367 | 0.4524 | 0.2192 | 0.043* | |
O9 | 0.9349 (6) | 0.8985 (7) | 0.1774 (5) | 0.093 (2) | |
H9 | 0.8969 | 0.8687 | 0.1230 | 0.139* | |
C15 | 0.6687 (6) | 1.0703 (6) | 0.3450 (5) | 0.0432 (16) | |
H15A | 0.6339 | 1.0601 | 0.4120 | 0.052* | |
H15B | 0.7128 | 1.1584 | 0.3353 | 0.052* | |
C11 | 0.3460 (7) | 0.3024 (6) | 0.2354 (5) | 0.0480 (17) | |
H11A | 0.3850 | 0.3088 | 0.1701 | 0.058* | |
H11B | 0.2952 | 0.2155 | 0.2454 | 0.058* | |
C17 | 1.0282 (9) | 1.0283 (9) | 0.1646 (9) | 0.107 (4) | |
H17A | 0.9832 | 1.0850 | 0.1766 | 0.161* | |
H17B | 1.0587 | 1.0360 | 0.0972 | 0.161* | |
H17C | 1.1027 | 1.0476 | 0.2119 | 0.161* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0271 (4) | 0.0258 (4) | 0.0237 (4) | 0.0097 (3) | −0.0053 (3) | 0.0029 (3) |
Ni2 | 0.0257 (4) | 0.0264 (4) | 0.0259 (4) | 0.0104 (3) | −0.0030 (3) | 0.0056 (3) |
Ni3 | 0.0233 (4) | 0.0267 (4) | 0.0253 (4) | 0.0095 (3) | −0.0015 (3) | 0.0032 (3) |
Ni4 | 0.0235 (4) | 0.0268 (4) | 0.0242 (4) | 0.0079 (3) | −0.0019 (3) | 0.0042 (3) |
Cl4 | 0.0358 (8) | 0.0429 (9) | 0.0354 (9) | 0.0092 (7) | 0.0057 (6) | 0.0124 (7) |
Cl1 | 0.0437 (9) | 0.0325 (8) | 0.0408 (9) | 0.0122 (7) | −0.0117 (7) | −0.0032 (6) |
Cl3 | 0.0429 (9) | 0.0321 (8) | 0.0403 (9) | 0.0155 (7) | 0.0002 (7) | −0.0022 (6) |
Cl2 | 0.0353 (8) | 0.0430 (9) | 0.0355 (9) | 0.0148 (7) | 0.0023 (6) | 0.0154 (7) |
O1 | 0.027 (2) | 0.021 (2) | 0.022 (2) | 0.0098 (16) | −0.0031 (15) | 0.0010 (15) |
O3 | 0.0181 (18) | 0.026 (2) | 0.028 (2) | 0.0089 (16) | −0.0026 (15) | 0.0007 (15) |
O7 | 0.0215 (19) | 0.028 (2) | 0.0189 (19) | 0.0087 (16) | −0.0013 (14) | 0.0032 (15) |
O5 | 0.026 (2) | 0.029 (2) | 0.022 (2) | 0.0116 (17) | −0.0022 (15) | 0.0061 (15) |
O4 | 0.035 (2) | 0.041 (3) | 0.037 (2) | 0.015 (2) | 0.0031 (18) | 0.0088 (19) |
O8 | 0.034 (2) | 0.037 (2) | 0.039 (2) | 0.0086 (19) | −0.0036 (18) | −0.0017 (19) |
O2 | 0.039 (2) | 0.040 (3) | 0.028 (2) | 0.016 (2) | −0.0029 (17) | 0.0030 (18) |
N1 | 0.030 (3) | 0.031 (3) | 0.035 (3) | 0.012 (2) | −0.006 (2) | 0.007 (2) |
N3 | 0.040 (3) | 0.035 (3) | 0.035 (3) | 0.022 (2) | −0.008 (2) | 0.001 (2) |
C2 | 0.028 (3) | 0.035 (3) | 0.038 (4) | 0.015 (3) | −0.005 (2) | 0.008 (3) |
C13 | 0.027 (3) | 0.038 (3) | 0.023 (3) | 0.008 (3) | −0.001 (2) | 0.005 (2) |
O6 | 0.049 (3) | 0.033 (2) | 0.040 (3) | 0.017 (2) | −0.009 (2) | −0.0011 (19) |
C10 | 0.031 (3) | 0.038 (4) | 0.044 (4) | 0.020 (3) | −0.006 (3) | 0.001 (3) |
C9 | 0.036 (3) | 0.034 (3) | 0.031 (3) | 0.026 (3) | 0.008 (2) | 0.002 (2) |
C1 | 0.034 (3) | 0.027 (3) | 0.027 (3) | 0.016 (3) | −0.005 (2) | 0.007 (2) |
C16 | 0.035 (4) | 0.042 (4) | 0.048 (4) | 0.002 (3) | −0.005 (3) | 0.003 (3) |
C8 | 0.029 (3) | 0.044 (4) | 0.043 (4) | 0.019 (3) | 0.010 (3) | 0.005 (3) |
N4 | 0.028 (3) | 0.043 (3) | 0.036 (3) | 0.015 (2) | −0.001 (2) | 0.004 (2) |
N2 | 0.028 (3) | 0.037 (3) | 0.034 (3) | 0.014 (2) | −0.001 (2) | 0.010 (2) |
C12 | 0.048 (4) | 0.039 (4) | 0.047 (4) | 0.027 (3) | 0.001 (3) | 0.012 (3) |
C4 | 0.053 (4) | 0.046 (4) | 0.027 (3) | 0.022 (3) | −0.015 (3) | 0.000 (3) |
C14 | 0.035 (3) | 0.043 (4) | 0.025 (3) | 0.018 (3) | −0.008 (2) | −0.003 (3) |
C6 | 0.024 (3) | 0.035 (4) | 0.045 (4) | 0.009 (3) | −0.006 (3) | 0.004 (3) |
C3 | 0.058 (4) | 0.043 (4) | 0.024 (3) | 0.022 (3) | −0.001 (3) | 0.007 (3) |
C7 | 0.035 (4) | 0.051 (4) | 0.040 (4) | 0.015 (3) | 0.012 (3) | 0.006 (3) |
C5 | 0.025 (3) | 0.030 (3) | 0.044 (4) | 0.001 (3) | −0.008 (3) | 0.000 (3) |
O9 | 0.086 (5) | 0.126 (6) | 0.090 (5) | 0.066 (4) | −0.002 (4) | 0.016 (4) |
C15 | 0.047 (4) | 0.034 (4) | 0.039 (4) | 0.005 (3) | −0.008 (3) | −0.006 (3) |
C11 | 0.062 (5) | 0.035 (4) | 0.050 (4) | 0.022 (3) | −0.005 (3) | 0.001 (3) |
C17 | 0.053 (6) | 0.089 (8) | 0.171 (12) | 0.015 (5) | 0.022 (6) | 0.001 (7) |
Ni1—O1 | 2.050 (3) | O6—H6 | 0.8200 |
Ni1—O5 | 2.064 (4) | C10—C9 | 1.530 (8) |
Ni1—N1 | 2.100 (4) | C10—H10A | 0.9700 |
Ni1—O3 | 2.137 (4) | C10—H10B | 0.9700 |
Ni1—O2 | 2.160 (4) | C9—H9A | 0.9700 |
Ni1—Cl1 | 2.4081 (16) | C9—H9B | 0.9700 |
Ni2—O5 | 2.044 (3) | C1—H1A | 0.9700 |
Ni2—O3 | 2.052 (3) | C1—H1B | 0.9700 |
Ni2—N3 | 2.112 (5) | C16—N4 | 1.489 (8) |
Ni2—O7 | 2.117 (4) | C16—C15 | 1.511 (9) |
Ni2—O6 | 2.168 (4) | C16—H16A | 0.9700 |
Ni2—Cl2 | 2.4331 (16) | C16—H16B | 0.9700 |
Ni3—O3 | 2.045 (4) | C8—N2 | 1.463 (7) |
Ni3—O7 | 2.063 (3) | C8—C7 | 1.522 (8) |
Ni3—O1 | 2.101 (3) | C8—H8A | 0.9700 |
Ni3—N2 | 2.116 (4) | C8—H8B | 0.9700 |
Ni3—O4 | 2.144 (4) | N4—C14 | 1.480 (7) |
Ni3—Cl3 | 2.3888 (16) | N4—H4AA | 0.9100 |
Ni4—O7 | 2.039 (3) | N2—C6 | 1.486 (7) |
Ni4—O1 | 2.059 (3) | N2—H2AA | 0.9100 |
Ni4—N4 | 2.123 (5) | C12—C11 | 1.529 (9) |
Ni4—O5 | 2.133 (4) | C12—H12A | 0.9700 |
Ni4—O8 | 2.145 (4) | C12—H12B | 0.9700 |
Ni4—Cl4 | 2.3898 (16) | C4—C3 | 1.503 (9) |
O1—C1 | 1.411 (6) | C4—H4A | 0.9700 |
O3—C5 | 1.424 (6) | C4—H4B | 0.9700 |
O7—C13 | 1.416 (6) | C14—H14A | 0.9700 |
O5—C9 | 1.412 (6) | C14—H14B | 0.9700 |
O4—C7 | 1.428 (7) | C6—C5 | 1.525 (8) |
O4—H4 | 0.8200 | C6—H6A | 0.9700 |
O8—C15 | 1.438 (7) | C6—H6B | 0.9700 |
O8—H8 | 0.8200 | C3—H3A | 0.9700 |
O2—C3 | 1.435 (7) | C3—H3B | 0.9700 |
O2—H2 | 0.8200 | C7—H7A | 0.9700 |
N1—C4 | 1.485 (7) | C7—H7B | 0.9700 |
N1—C2 | 1.471 (7) | C5—H5A | 0.9700 |
N1—H1 | 0.9100 | C5—H5B | 0.9700 |
N3—C12 | 1.472 (7) | O9—C17 | 1.492 (10) |
N3—C10 | 1.467 (7) | O9—H9 | 0.8200 |
N3—H3 | 0.9100 | C15—H15A | 0.9700 |
C2—C1 | 1.533 (7) | C15—H15B | 0.9700 |
C2—H2A | 0.9700 | C11—H11A | 0.9700 |
C2—H2B | 0.9700 | C11—H11B | 0.9700 |
C13—C14 | 1.515 (7) | C17—H17A | 0.9600 |
C13—H13A | 0.9700 | C17—H17B | 0.9600 |
C13—H13B | 0.9700 | C17—H17C | 0.9600 |
O6—C11 | 1.417 (7) | ||
O1—Ni1—O5 | 82.68 (14) | O7—C13—H13A | 109.7 |
O1—Ni1—N1 | 83.49 (16) | C14—C13—H13A | 109.7 |
O5—Ni1—N1 | 159.63 (17) | O7—C13—H13B | 109.7 |
O1—Ni1—O3 | 78.70 (14) | C14—C13—H13B | 109.7 |
O5—Ni1—O3 | 80.83 (13) | H13A—C13—H13B | 108.2 |
N1—Ni1—O3 | 110.95 (16) | C11—O6—Ni2 | 113.3 (4) |
O1—Ni1—O2 | 96.07 (14) | C11—O6—H6 | 109.5 |
O5—Ni1—O2 | 87.03 (14) | Ni2—O6—H6 | 66.2 |
N1—Ni1—O2 | 79.64 (16) | N3—C10—C9 | 112.0 (5) |
O3—Ni1—O2 | 167.27 (14) | N3—C10—H10A | 109.2 |
O1—Ni1—Cl1 | 170.51 (11) | C9—C10—H10A | 109.2 |
O5—Ni1—Cl1 | 102.11 (11) | N3—C10—H10B | 109.2 |
N1—Ni1—Cl1 | 93.83 (14) | C9—C10—H10B | 109.2 |
O3—Ni1—Cl1 | 93.87 (10) | H10A—C10—H10B | 107.9 |
O2—Ni1—Cl1 | 92.38 (11) | O5—C9—C10 | 109.6 (4) |
O5—Ni2—O3 | 83.39 (14) | O5—C9—H9A | 109.7 |
O5—Ni2—N3 | 83.37 (17) | C10—C9—H9A | 109.7 |
O3—Ni2—N3 | 159.85 (17) | O5—C9—H9B | 109.7 |
O5—Ni2—O7 | 79.11 (14) | C10—C9—H9B | 109.7 |
O3—Ni2—O7 | 81.33 (13) | H9A—C9—H9B | 108.2 |
N3—Ni2—O7 | 110.89 (16) | O1—C1—C2 | 108.8 (4) |
O5—Ni2—O6 | 95.49 (15) | O1—C1—H1A | 109.9 |
O3—Ni2—O6 | 86.76 (15) | C2—C1—H1A | 109.9 |
N3—Ni2—O6 | 79.46 (17) | O1—C1—H1B | 109.9 |
O7—Ni2—O6 | 167.40 (14) | C2—C1—H1B | 109.9 |
O5—Ni2—Cl2 | 170.64 (11) | H1A—C1—H1B | 108.3 |
O3—Ni2—Cl2 | 100.80 (11) | N4—C16—C15 | 111.5 (5) |
N3—Ni2—Cl2 | 94.61 (14) | N4—C16—H16A | 109.3 |
O7—Ni2—Cl2 | 93.16 (10) | C15—C16—H16A | 109.3 |
O6—Ni2—Cl2 | 93.12 (12) | N4—C16—H16B | 109.3 |
O3—Ni3—O7 | 82.80 (13) | C15—C16—H16B | 109.3 |
O3—Ni3—O1 | 79.64 (14) | H16A—C16—H16B | 108.0 |
O7—Ni3—O1 | 81.65 (13) | N2—C8—C7 | 110.4 (5) |
O3—Ni3—N2 | 83.21 (16) | N2—C8—H8A | 109.6 |
O7—Ni3—N2 | 158.91 (17) | C7—C8—H8A | 109.6 |
O1—Ni3—N2 | 111.15 (16) | N2—C8—H8B | 109.6 |
O3—Ni3—O4 | 97.16 (15) | C7—C8—H8B | 109.6 |
O7—Ni3—O4 | 87.04 (14) | H8A—C8—H8B | 108.1 |
O1—Ni3—O4 | 168.54 (14) | C16—N4—C14 | 115.2 (5) |
N2—Ni3—O4 | 79.14 (16) | C16—N4—Ni4 | 107.8 (4) |
O3—Ni3—Cl3 | 171.15 (11) | C14—N4—Ni4 | 107.2 (3) |
O7—Ni3—Cl3 | 101.82 (11) | C16—N4—H4AA | 108.8 |
O1—Ni3—Cl3 | 93.46 (10) | C14—N4—H4AA | 108.8 |
N2—Ni3—Cl3 | 94.26 (14) | Ni4—N4—H4AA | 108.8 |
O4—Ni3—Cl3 | 90.66 (12) | C8—N2—C6 | 115.5 (5) |
O7—Ni4—O1 | 83.25 (14) | C8—N2—Ni3 | 107.0 (3) |
O7—Ni4—N4 | 83.12 (16) | C6—N2—Ni3 | 107.9 (3) |
O1—Ni4—N4 | 159.57 (17) | C8—N2—H2AA | 108.7 |
O7—Ni4—O5 | 78.83 (14) | C6—N2—H2AA | 108.7 |
O1—Ni4—O5 | 80.81 (13) | Ni3—N2—H2AA | 108.7 |
N4—Ni4—O5 | 111.26 (17) | N3—C12—C11 | 110.6 (5) |
O7—Ni4—O8 | 97.15 (15) | N3—C12—H12A | 109.5 |
O1—Ni4—O8 | 87.13 (14) | C11—C12—H12A | 109.5 |
N4—Ni4—O8 | 79.56 (17) | N3—C12—H12B | 109.5 |
O5—Ni4—O8 | 167.63 (14) | C11—C12—H12B | 109.5 |
O7—Ni4—Cl4 | 170.45 (11) | H12A—C12—H12B | 108.1 |
O1—Ni4—Cl4 | 101.52 (11) | N1—C4—C3 | 111.3 (5) |
N4—Ni4—Cl4 | 94.28 (14) | N1—C4—H4A | 109.4 |
O5—Ni4—Cl4 | 93.67 (10) | C3—C4—H4A | 109.4 |
O8—Ni4—Cl4 | 91.39 (12) | N1—C4—H4B | 109.4 |
C1—O1—Ni4 | 124.9 (3) | C3—C4—H4B | 109.4 |
C1—O1—Ni1 | 110.1 (3) | H4A—C4—H4B | 108.0 |
Ni4—O1—Ni1 | 98.59 (14) | N4—C14—C13 | 111.1 (4) |
C1—O1—Ni3 | 122.1 (3) | N4—C14—H14A | 109.4 |
Ni4—O1—Ni3 | 95.45 (14) | C13—C14—H14A | 109.4 |
Ni1—O1—Ni3 | 101.20 (15) | N4—C14—H14B | 109.4 |
C5—O3—Ni3 | 109.6 (3) | C13—C14—H14B | 109.4 |
C5—O3—Ni2 | 123.2 (3) | H14A—C14—H14B | 108.0 |
Ni3—O3—Ni2 | 98.34 (14) | N2—C6—C5 | 112.1 (4) |
C5—O3—Ni1 | 125.0 (3) | N2—C6—H6A | 109.2 |
Ni3—O3—Ni1 | 100.17 (15) | C5—C6—H6A | 109.2 |
Ni2—O3—Ni1 | 95.53 (14) | N2—C6—H6B | 109.2 |
C13—O7—Ni4 | 109.8 (3) | C5—C6—H6B | 109.2 |
C13—O7—Ni3 | 125.5 (3) | H6A—C6—H6B | 107.9 |
Ni4—O7—Ni3 | 97.27 (14) | O2—C3—C4 | 106.3 (5) |
C13—O7—Ni2 | 122.4 (3) | O2—C3—H3A | 110.5 |
Ni4—O7—Ni2 | 101.27 (14) | C4—C3—H3A | 110.5 |
Ni3—O7—Ni2 | 95.75 (14) | O2—C3—H3B | 110.5 |
C9—O5—Ni2 | 109.5 (3) | C4—C3—H3B | 110.5 |
C9—O5—Ni1 | 124.0 (3) | H3A—C3—H3B | 108.7 |
Ni2—O5—Ni1 | 98.06 (15) | O4—C7—C8 | 107.8 (5) |
C9—O5—Ni4 | 124.0 (3) | O4—C7—H7A | 110.1 |
Ni2—O5—Ni4 | 100.56 (15) | C8—C7—H7A | 110.1 |
Ni1—O5—Ni4 | 95.85 (14) | O4—C7—H7B | 110.1 |
C7—O4—Ni3 | 114.0 (3) | C8—C7—H7B | 110.1 |
C7—O4—H4 | 109.5 | H7A—C7—H7B | 108.5 |
Ni3—O4—H4 | 101.4 | O3—C5—C6 | 109.7 (5) |
C15—O8—Ni4 | 114.3 (4) | O3—C5—H5A | 109.7 |
C15—O8—H8 | 109.5 | C6—C5—H5A | 109.7 |
Ni4—O8—H8 | 98.8 | O3—C5—H5B | 109.7 |
C3—O2—Ni1 | 113.2 (3) | C6—C5—H5B | 109.7 |
C3—O2—H2 | 109.5 | H5A—C5—H5B | 108.2 |
Ni1—O2—H2 | 96.3 | C17—O9—H9 | 109.5 |
C4—N1—C2 | 114.6 (5) | O8—C15—C16 | 107.7 (5) |
C4—N1—Ni1 | 106.8 (3) | O8—C15—H15A | 110.2 |
C2—N1—Ni1 | 107.4 (3) | C16—C15—H15A | 110.2 |
C4—N1—H1 | 109.3 | O8—C15—H15B | 110.2 |
C2—N1—H1 | 109.3 | C16—C15—H15B | 110.2 |
Ni1—N1—H1 | 109.3 | H15A—C15—H15B | 108.5 |
C12—N3—C10 | 116.2 (5) | O6—C11—C12 | 108.3 (5) |
C12—N3—Ni2 | 106.7 (4) | O6—C11—H11A | 110.0 |
C10—N3—Ni2 | 107.6 (3) | C12—C11—H11A | 110.0 |
C12—N3—H3 | 108.7 | O6—C11—H11B | 110.0 |
C10—N3—H3 | 108.7 | C12—C11—H11B | 110.0 |
Ni2—N3—H3 | 108.7 | H11A—C11—H11B | 108.4 |
N1—C2—C1 | 112.7 (4) | O9—C17—H17A | 109.5 |
N1—C2—H2A | 109.1 | O9—C17—H17B | 109.5 |
C1—C2—H2A | 109.1 | H17A—C17—H17B | 109.5 |
N1—C2—H2B | 109.1 | O9—C17—H17C | 109.5 |
C1—C2—H2B | 109.1 | H17A—C17—H17C | 109.5 |
H2A—C2—H2B | 107.8 | H17B—C17—H17C | 109.5 |
O7—C13—C14 | 109.9 (4) | ||
O7—Ni4—O1—C1 | 147.4 (4) | O3—Ni2—O5—Ni4 | 85.98 (15) |
N4—Ni4—O1—C1 | 99.0 (6) | N3—Ni2—O5—Ni4 | −109.24 (18) |
O5—Ni4—O1—C1 | −132.9 (4) | O7—Ni2—O5—Ni4 | 3.58 (13) |
O8—Ni4—O1—C1 | 49.9 (4) | O6—Ni2—O5—Ni4 | 172.07 (15) |
Cl4—Ni4—O1—C1 | −41.0 (4) | O1—Ni1—O5—C9 | −149.1 (4) |
O7—Ni4—O1—Ni1 | −90.62 (15) | N1—Ni1—O5—C9 | −101.5 (6) |
N4—Ni4—O1—Ni1 | −139.1 (4) | O3—Ni1—O5—C9 | 131.2 (4) |
O5—Ni4—O1—Ni1 | −10.90 (14) | O2—Ni1—O5—C9 | −52.6 (4) |
O8—Ni4—O1—Ni1 | 171.83 (16) | Cl1—Ni1—O5—C9 | 39.2 (4) |
Cl4—Ni4—O1—Ni1 | 81.00 (13) | O1—Ni1—O5—Ni2 | 90.81 (15) |
O7—Ni4—O1—Ni3 | 11.61 (14) | N1—Ni1—O5—Ni2 | 138.4 (4) |
N4—Ni4—O1—Ni3 | −36.8 (5) | O3—Ni1—O5—Ni2 | 11.15 (14) |
O5—Ni4—O1—Ni3 | 91.33 (14) | O2—Ni1—O5—Ni2 | −172.67 (16) |
O8—Ni4—O1—Ni3 | −85.94 (15) | Cl1—Ni1—O5—Ni2 | −80.87 (13) |
Cl4—Ni4—O1—Ni3 | −176.77 (9) | O1—Ni1—O5—Ni4 | −10.76 (14) |
O5—Ni1—O1—C1 | 143.4 (3) | N1—Ni1—O5—Ni4 | 36.9 (5) |
N1—Ni1—O1—C1 | −21.6 (3) | O3—Ni1—O5—Ni4 | −90.42 (14) |
O3—Ni1—O1—C1 | −134.6 (3) | O2—Ni1—O5—Ni4 | 85.76 (15) |
O2—Ni1—O1—C1 | 57.2 (3) | Cl1—Ni1—O5—Ni4 | 177.56 (9) |
O5—Ni1—O1—Ni4 | 11.22 (14) | O7—Ni4—O5—C9 | −126.0 (4) |
N1—Ni1—O1—Ni4 | −153.78 (18) | O1—Ni4—O5—C9 | 149.1 (4) |
O3—Ni1—O1—Ni4 | 93.28 (15) | N4—Ni4—O5—C9 | −48.0 (4) |
O2—Ni1—O1—Ni4 | −74.98 (16) | O8—Ni4—O5—C9 | 162.0 (6) |
O5—Ni1—O1—Ni3 | −86.13 (15) | Cl4—Ni4—O5—C9 | 48.0 (4) |
N1—Ni1—O1—Ni3 | 108.87 (18) | O7—Ni4—O5—Ni2 | −3.72 (14) |
O3—Ni1—O1—Ni3 | −4.07 (13) | O1—Ni4—O5—Ni2 | −88.59 (15) |
O2—Ni1—O1—Ni3 | −172.33 (15) | N4—Ni4—O5—Ni2 | 74.29 (19) |
O3—Ni3—O1—C1 | 126.8 (4) | O8—Ni4—O5—Ni2 | −75.7 (7) |
O7—Ni3—O1—C1 | −149.0 (4) | Cl4—Ni4—O5—Ni2 | 170.32 (12) |
N2—Ni3—O1—C1 | 48.3 (4) | O7—Ni4—O5—Ni1 | 95.63 (15) |
O4—Ni3—O1—C1 | −158.5 (7) | O1—Ni4—O5—Ni1 | 10.76 (14) |
Cl3—Ni3—O1—C1 | −47.6 (4) | N4—Ni4—O5—Ni1 | 173.64 (16) |
O3—Ni3—O1—Ni4 | −95.66 (14) | O8—Ni4—O5—Ni1 | 23.6 (7) |
O7—Ni3—O1—Ni4 | −11.51 (14) | Cl4—Ni4—O5—Ni1 | −90.33 (11) |
N2—Ni3—O1—Ni4 | −174.14 (15) | O3—Ni3—O4—C7 | −81.7 (4) |
O4—Ni3—O1—Ni4 | −21.0 (8) | O7—Ni3—O4—C7 | −164.1 (4) |
Cl3—Ni3—O1—Ni4 | 89.94 (11) | O1—Ni3—O4—C7 | −154.7 (6) |
O3—Ni3—O1—Ni1 | 4.24 (14) | N2—Ni3—O4—C7 | −0.1 (4) |
O7—Ni3—O1—Ni1 | 88.39 (15) | Cl3—Ni3—O4—C7 | 94.1 (4) |
N2—Ni3—O1—Ni1 | −74.24 (19) | O7—Ni4—O8—C15 | 77.5 (4) |
O4—Ni3—O1—Ni1 | 78.9 (7) | O1—Ni4—O8—C15 | 160.3 (4) |
Cl3—Ni3—O1—Ni1 | −170.16 (12) | N4—Ni4—O8—C15 | −4.1 (4) |
O7—Ni3—O3—C5 | 140.1 (3) | O5—Ni4—O8—C15 | 147.6 (6) |
O1—Ni3—O3—C5 | −137.1 (3) | Cl4—Ni4—O8—C15 | −98.2 (4) |
N2—Ni3—O3—C5 | −24.1 (3) | O1—Ni1—O2—C3 | −77.4 (4) |
O4—Ni3—O3—C5 | 54.0 (3) | O5—Ni1—O2—C3 | −159.7 (4) |
O7—Ni3—O3—Ni2 | 10.35 (14) | N1—Ni1—O2—C3 | 4.8 (4) |
O1—Ni3—O3—Ni2 | 93.13 (15) | O3—Ni1—O2—C3 | −142.3 (6) |
N2—Ni3—O3—Ni2 | −153.84 (18) | Cl1—Ni1—O2—C3 | 98.3 (4) |
O4—Ni3—O3—Ni2 | −75.73 (16) | O1—Ni1—N1—C4 | 119.8 (4) |
O7—Ni3—O3—Ni1 | −86.84 (14) | O5—Ni1—N1—C4 | 72.3 (6) |
O1—Ni3—O3—Ni1 | −4.06 (13) | O3—Ni1—N1—C4 | −165.0 (3) |
N2—Ni3—O3—Ni1 | 108.97 (17) | O2—Ni1—N1—C4 | 22.4 (4) |
O4—Ni3—O3—Ni1 | −172.92 (14) | Cl1—Ni1—N1—C4 | −69.3 (4) |
O5—Ni2—O3—C5 | 149.8 (4) | O1—Ni1—N1—C2 | −3.6 (3) |
N3—Ni2—O3—C5 | 100.6 (6) | O5—Ni1—N1—C2 | −51.1 (7) |
O7—Ni2—O3—C5 | −130.2 (4) | O3—Ni1—N1—C2 | 71.6 (4) |
O6—Ni2—O3—C5 | 53.9 (4) | O2—Ni1—N1—C2 | −101.0 (4) |
Cl2—Ni2—O3—C5 | −38.6 (4) | Cl1—Ni1—N1—C2 | 167.3 (3) |
O5—Ni2—O3—Ni3 | −90.06 (15) | O5—Ni2—N3—C12 | −123.0 (4) |
N3—Ni2—O3—Ni3 | −139.3 (4) | O3—Ni2—N3—C12 | −73.8 (6) |
O7—Ni2—O3—Ni3 | −10.12 (14) | O7—Ni2—N3—C12 | 161.4 (3) |
O6—Ni2—O3—Ni3 | 174.03 (16) | O6—Ni2—N3—C12 | −26.1 (4) |
Cl2—Ni2—O3—Ni3 | 81.47 (13) | Cl2—Ni2—N3—C12 | 66.2 (4) |
O5—Ni2—O3—Ni1 | 11.09 (14) | O5—Ni2—N3—C10 | 2.4 (3) |
N3—Ni2—O3—Ni1 | −38.1 (5) | O3—Ni2—N3—C10 | 51.7 (7) |
O7—Ni2—O3—Ni1 | 91.03 (14) | O7—Ni2—N3—C10 | −73.2 (4) |
O6—Ni2—O3—Ni1 | −84.82 (15) | O6—Ni2—N3—C10 | 99.3 (4) |
Cl2—Ni2—O3—Ni1 | −177.38 (9) | Cl2—Ni2—N3—C10 | −168.4 (3) |
O1—Ni1—O3—C5 | 127.0 (4) | C4—N1—C2—C1 | −91.7 (6) |
O5—Ni1—O3—C5 | −148.7 (4) | Ni1—N1—C2—C1 | 26.7 (5) |
N1—Ni1—O3—C5 | 48.5 (4) | Ni4—O7—C13—C14 | −42.6 (5) |
O2—Ni1—O3—C5 | −166.3 (6) | Ni3—O7—C13—C14 | −157.5 (3) |
Cl1—Ni1—O3—C5 | −47.1 (4) | Ni2—O7—C13—C14 | 75.8 (5) |
O1—Ni1—O3—Ni3 | 4.17 (13) | O5—Ni2—O6—C11 | 82.6 (4) |
O5—Ni1—O3—Ni3 | 88.47 (15) | O3—Ni2—O6—C11 | 165.6 (4) |
N1—Ni1—O3—Ni3 | −74.28 (19) | N3—Ni2—O6—C11 | 0.4 (4) |
O2—Ni1—O3—Ni3 | 70.9 (7) | O7—Ni2—O6—C11 | 146.5 (6) |
Cl1—Ni1—O3—Ni3 | −169.87 (11) | Cl2—Ni2—O6—C11 | −93.8 (4) |
O1—Ni1—O3—Ni2 | −95.35 (15) | C12—N3—C10—C9 | 93.9 (6) |
O5—Ni1—O3—Ni2 | −11.05 (14) | Ni2—N3—C10—C9 | −25.6 (5) |
N1—Ni1—O3—Ni2 | −173.80 (16) | Ni2—O5—C9—C10 | −42.5 (5) |
O2—Ni1—O3—Ni2 | −28.6 (7) | Ni1—O5—C9—C10 | −157.2 (3) |
Cl1—Ni1—O3—Ni2 | 90.60 (11) | Ni4—O5—C9—C10 | 75.7 (5) |
O1—Ni4—O7—C13 | −143.7 (3) | N3—C10—C9—O5 | 46.3 (6) |
N4—Ni4—O7—C13 | 21.0 (3) | Ni4—O1—C1—C2 | 157.8 (3) |
O5—Ni4—O7—C13 | 134.4 (3) | Ni1—O1—C1—C2 | 41.1 (5) |
O8—Ni4—O7—C13 | −57.5 (3) | Ni3—O1—C1—C2 | −77.2 (5) |
O1—Ni4—O7—Ni3 | −11.87 (14) | N1—C2—C1—O1 | −46.1 (6) |
N4—Ni4—O7—Ni3 | 152.88 (18) | C15—C16—N4—C14 | −75.9 (6) |
O5—Ni4—O7—Ni3 | −93.78 (15) | C15—C16—N4—Ni4 | 43.7 (6) |
O8—Ni4—O7—Ni3 | 74.37 (16) | O7—Ni4—N4—C16 | −119.7 (4) |
O1—Ni4—O7—Ni2 | 85.51 (15) | O1—Ni4—N4—C16 | −71.3 (6) |
N4—Ni4—O7—Ni2 | −109.74 (18) | O5—Ni4—N4—C16 | 165.1 (3) |
O5—Ni4—O7—Ni2 | 3.60 (13) | O8—Ni4—N4—C16 | −21.1 (4) |
O8—Ni4—O7—Ni2 | 171.75 (15) | Cl4—Ni4—N4—C16 | 69.5 (4) |
O3—Ni3—O7—C13 | −147.1 (4) | O7—Ni4—N4—C14 | 4.9 (3) |
O1—Ni3—O7—C13 | 132.3 (4) | O1—Ni4—N4—C14 | 53.3 (7) |
N2—Ni3—O7—C13 | −98.4 (6) | O5—Ni4—N4—C14 | −70.3 (4) |
O4—Ni3—O7—C13 | −49.5 (4) | O8—Ni4—N4—C14 | 103.5 (4) |
Cl3—Ni3—O7—C13 | 40.5 (4) | Cl4—Ni4—N4—C14 | −165.9 (3) |
O3—Ni3—O7—Ni4 | 92.20 (15) | C7—C8—N2—C6 | 71.9 (6) |
O1—Ni3—O7—Ni4 | 11.67 (14) | C7—C8—N2—Ni3 | −48.3 (5) |
N2—Ni3—O7—Ni4 | 141.0 (4) | O3—Ni3—N2—C8 | 124.7 (4) |
O4—Ni3—O7—Ni4 | −170.20 (15) | O7—Ni3—N2—C8 | 76.0 (6) |
Cl3—Ni3—O7—Ni4 | −80.14 (12) | O1—Ni3—N2—C8 | −159.2 (3) |
O3—Ni3—O7—Ni2 | −9.97 (13) | O4—Ni3—N2—C8 | 26.0 (4) |
O1—Ni3—O7—Ni2 | −90.50 (14) | Cl3—Ni3—N2—C8 | −63.8 (4) |
N2—Ni3—O7—Ni2 | 38.8 (5) | O3—Ni3—N2—C6 | −0.2 (4) |
O4—Ni3—O7—Ni2 | 87.63 (15) | O7—Ni3—N2—C6 | −48.9 (6) |
Cl3—Ni3—O7—Ni2 | 177.69 (9) | O1—Ni3—N2—C6 | 75.9 (4) |
O5—Ni2—O7—C13 | −126.1 (4) | O4—Ni3—N2—C6 | −98.9 (4) |
O3—Ni2—O7—C13 | 149.0 (4) | Cl3—Ni3—N2—C6 | 171.2 (3) |
N3—Ni2—O7—C13 | −47.6 (4) | C10—N3—C12—C11 | −71.7 (6) |
O6—Ni2—O7—C13 | 168.3 (6) | Ni2—N3—C12—C11 | 48.3 (6) |
Cl2—Ni2—O7—C13 | 48.5 (3) | C2—N1—C4—C3 | 71.2 (6) |
O5—Ni2—O7—Ni4 | −3.75 (14) | Ni1—N1—C4—C3 | −47.6 (6) |
O3—Ni2—O7—Ni4 | −88.63 (15) | C16—N4—C14—C13 | 91.4 (6) |
N3—Ni2—O7—Ni4 | 74.76 (19) | Ni4—N4—C14—C13 | −28.6 (5) |
O6—Ni2—O7—Ni4 | −69.3 (7) | O7—C13—C14—N4 | 48.2 (6) |
Cl2—Ni2—O7—Ni4 | 170.92 (12) | C8—N2—C6—C5 | −96.5 (6) |
O5—Ni2—O7—Ni3 | 94.86 (15) | Ni3—N2—C6—C5 | 23.2 (6) |
O3—Ni2—O7—Ni3 | 9.98 (13) | Ni1—O2—C3—C4 | −30.4 (5) |
N3—Ni2—O7—Ni3 | 173.37 (16) | N1—C4—C3—O2 | 51.8 (6) |
O6—Ni2—O7—Ni3 | 29.3 (7) | Ni3—O4—C7—C8 | −24.9 (6) |
Cl2—Ni2—O7—Ni3 | −90.47 (11) | N2—C8—C7—O4 | 48.8 (7) |
O3—Ni2—O5—C9 | −142.0 (3) | Ni3—O3—C5—C6 | 43.0 (5) |
N3—Ni2—O5—C9 | 22.8 (3) | Ni2—O3—C5—C6 | 157.7 (4) |
O7—Ni2—O5—C9 | 135.6 (3) | Ni1—O3—C5—C6 | −75.5 (5) |
O6—Ni2—O5—C9 | −55.9 (3) | N2—C6—C5—O3 | −44.6 (7) |
O3—Ni2—O5—Ni1 | −11.55 (14) | Ni4—O8—C15—C16 | 27.9 (6) |
N3—Ni2—O5—Ni1 | 153.23 (19) | N4—C16—C15—O8 | −47.4 (7) |
O7—Ni2—O5—Ni1 | −93.95 (15) | Ni2—O6—C11—C12 | 24.7 (6) |
O6—Ni2—O5—Ni1 | 74.54 (16) | N3—C12—C11—O6 | −48.9 (7) |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4···Cl2 | 0.82 | 2.27 | 3.087 (4) | 176 |
O8—H8···Cl3 | 0.82 | 2.19 | 3.013 (4) | 179 |
O2—H2···Cl4 | 0.82 | 2.24 | 3.058 (4) | 175 |
O6—H6···Cl2 | 0.82 | 2.60 | 3.346 (4) | 153 |
N1—H1···Cl1i | 0.91 | 2.62 | 3.476 (5) | 157 |
N3—H3···Cl2ii | 0.91 | 2.62 | 3.448 (5) | 152 |
N4—H4AA···O9 | 0.91 | 2.52 | 3.228 (9) | 135 |
N2—H2AA···O9iii | 0.91 | 2.18 | 3.060 (10) | 162 |
O9—H9···Cl4 | 0.82 | 2.76 | 3.224 (7) | 118 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Ni4(C4H10NO2)4Cl4]·CH4O |
Mr | 825.20 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 10.8244 (12), 11.5609 (13), 13.2797 (17) |
α, β, γ (°) | 91.741 (1), 91.845 (1), 111.283 (2) |
V (Å3) | 1546.1 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.79 |
Crystal size (mm) | 0.39 × 0.25 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.409, 0.680 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8045, 5352, 3889 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.141, 1.01 |
No. of reflections | 5352 |
No. of parameters | 344 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.01, −0.74 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4···Cl2 | 0.82 | 2.27 | 3.087 (4) | 175.9 |
O8—H8···Cl3 | 0.82 | 2.19 | 3.013 (4) | 178.8 |
O2—H2···Cl4 | 0.82 | 2.24 | 3.058 (4) | 175.2 |
O6—H6···Cl2 | 0.82 | 2.60 | 3.346 (4) | 152.8 |
N1—H1···Cl1i | 0.91 | 2.62 | 3.476 (5) | 157.1 |
N3—H3···Cl2ii | 0.91 | 2.62 | 3.448 (5) | 152.4 |
N4—H4AA···O9 | 0.91 | 2.52 | 3.228 (9) | 135 |
N2—H2AA···O9iii | 0.91 | 2.18 | 3.060 (10) | 162 |
O9—H9···Cl4 | 0.82 | 2.76 | 3.224 (7) | 118 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z. |
Acknowledgements
This work was supported by the Natural Science Foundation of China (grant No. 20971063)
References
Cadiou, C., Murrie, M., Paulsen, C., Villar, V., Wernsdorfer, W. & Winpenny, R. E. P. (2001). Chem. Commun. pp. 2666–2667. Web of Science CrossRef Google Scholar
Ferguson, A., Lawrence, J., Parkin, A., Sanchez-Benitez, J., Kamenev, K. V., Brechin, E. K., Wernsdorfer, W., Hill, S. & Murrie, M. (2008). Dalton Trans. pp. 6409–6414. Web of Science CSD CrossRef Google Scholar
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Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The potential of the nickel(II) was highlighted when a few Ni-containing complexes have been reported for their 'single molecule magnetism' (SMM) behaviour. (Cadiou et al., 2001). We report here the synthesis and structure of the title compound.
In the title complex (Fig. 1), each nickel(II) metal atom is six-coordinated by three µ3-O donors derived from the alkoxide groups of three mono-deprotonated diethanolamine ligands, one hydroxy O and one amine N atom of the same ligand, and by a Cl anion, forming a distorted octahedron. Bond lengths and angles are typical and are comparable with those observed in the related acetonitrile solvate octadecahydrate complexes (Ferguson et al., 2008). The conformation of the complex molecule is stabilized by intramolecular O—H···Cl bonds (Table 1). In the crystal structure, complex molecules and solvent molecules are linked through intermolecular N—H···Cl, N—H···O and O—H···Cl hydrogen bonds (Table 1) into a three-dimensional network.