Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100014967/qa0417sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100014967/qa0417Isup2.hkl |
CCDC reference: 156192
1-Methyl-2-{[N-ethyl-N-(2-hydroxy-5-methylbenzyl)amino]methyl}-1H-benzimidazole (L; 0.224 g, 0.725 mmol) dissolved in methanol (7 ml) was added slowly to a suspension of NiBr2 (0.231 g, 0.966 mmol) in refluxing methanol. Heating was continued until dissolution of the nickel salt was complete, affording a clear green solution. Sodium acetate (0.277 g, 0.203 mmol) dissolved in methanol (5 ml) was added to the green solution. The solvent was removed under vacuum, resulting in a crude green product. This material was dissolved in acetonitrile and the solution filtered and evaporated to dryness. Recrystallization from methanol/2-propanol resulted in crystals of suitable quality for X-ray structure determination.
The coordinates of the two H atoms of the water molecule O8 could not be reliably located and were not included in the refinement.
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1994); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1992-1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: Xtal3.4 CRYLSQ (Hall et al., 1995); software used to prepare material for publication: Xtal3.4 BONDLA CIFIO.
[Ni3(C18H22N3O)2(C2H3O2)4(H2O)2]·4H2O | Z = 1 |
Mr = 1137.15 | F(000) = 598 |
Triclinic, P1 | Dx = 1.419 Mg m−3 |
Hall symbol: -P 1 | Cu Kα radiation, λ = 1.5418 Å |
a = 11.130 (2) Å | Cell parameters from 25 reflections |
b = 11.732 (2) Å | θ = 17.2–26.1° |
c = 12.258 (2) Å | µ = 1.83 mm−1 |
α = 99.66 (2)° | T = 193 K |
β = 110.34 (1)° | Plate, colourless |
γ = 110.23 (1)° | 0.12 × 0.12 × 0.02 mm |
V = 1330.6 (5) Å3 |
Rigaku AFC-6R diffractometer | 2872 reflections with F > 2.5σ(Fo)' |
Radiation source: Rigaku rotating anode | Rint = 0.031 |
Graphite monochromator | θmax = 60.0°, θmin = 4.1° |
ω–2θ scans | h = −11→12 |
Absorption correction: ψ scan (North et al., 1968) | k = −12→13 |
Tmin = 0.873, Tmax = 0.965 | l = −13→0 |
4152 measured reflections | 3 standard reflections every 150 reflections |
3940 independent reflections | intensity decay: 0.8% |
Refinement on F | 0 restraints |
Least-squares matrix: full | 0 constraints |
R[F2 > 2σ(F2)] = 0.058 | H-atom parameters not refined |
wR(F2) = 0.047 | Weighting scheme based on measured s.u.'s w = 1/σ2(Fo) |
S = 1.93 | (Δ/σ)max < 0.001 |
2865 reflections | Δρmax = 0.64 e Å−3 |
322 parameters | Δρmin = −0.68 e Å−3 |
[Ni3(C18H22N3O)2(C2H3O2)4(H2O)2]·4H2O | γ = 110.23 (1)° |
Mr = 1137.15 | V = 1330.6 (5) Å3 |
Triclinic, P1 | Z = 1 |
a = 11.130 (2) Å | Cu Kα radiation |
b = 11.732 (2) Å | µ = 1.83 mm−1 |
c = 12.258 (2) Å | T = 193 K |
α = 99.66 (2)° | 0.12 × 0.12 × 0.02 mm |
β = 110.34 (1)° |
Rigaku AFC-6R diffractometer | 2872 reflections with F > 2.5σ(Fo)' |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.031 |
Tmin = 0.873, Tmax = 0.965 | θmax = 60.0° |
4152 measured reflections | 3 standard reflections every 150 reflections |
3940 independent reflections | intensity decay: 0.8% |
R[F2 > 2σ(F2)] = 0.058 | 0 restraints |
wR(F2) = 0.047 | H-atom parameters not refined |
S = 1.93 | Δρmax = 0.64 e Å−3 |
2865 reflections | Δρmin = −0.68 e Å−3 |
322 parameters |
Experimental. The scan width was (1.30 + 0.30tanθ)° with an ω scan speed of 8° per minute (up to 5 scans to achieve I/σ(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 ° on a AFC6R diffractometer when the evacuated beam tunnel in used. Mass attenuation coefficients for absorption from International Tables for X-ray Crystallography, Vol IV (1974) Table 2.1 C. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.50000 | 0.50000 | 0.50000 | 0.0280 (5) | |
Ni2 | 0.22639 (9) | 0.43520 (8) | 0.27164 (8) | 0.0255 (4) | |
O1 | 0.2877 (3) | 0.4391 (3) | 0.4497 (3) | 0.0255 (14) | |
O2 | 0.4235 (3) | 0.4344 (3) | 0.3044 (3) | 0.0268 (14) | |
O3 | 0.4009 (4) | 0.3737 (4) | 0.1152 (4) | 0.054 (2) | |
O4 | 0.3253 (4) | 0.6325 (3) | 0.3253 (3) | 0.0318 (14) | |
O5 | 0.5077 (4) | 0.6745 (3) | 0.5028 (3) | 0.0317 (14) | |
O6 | 0.1834 (4) | 0.4333 (3) | 0.0903 (3) | 0.0351 (15) | |
O7 | 0.6989 (5) | 0.3011 (4) | 0.8865 (4) | 0.060 (2) | |
O8 | 0.4650 (6) | 0.3269 (5) | 0.9188 (5) | 0.094 (3) | |
N1 | 0.0252 (4) | 0.4320 (4) | 0.2479 (4) | 0.0277 (17) | |
N2 | 0.1040 (4) | 0.2378 (4) | 0.2049 (4) | 0.0271 (17) | |
N3 | −0.1131 (4) | 0.0769 (4) | 0.1210 (4) | 0.0331 (17) | |
C1 | 0.0239 (6) | 0.4472 (5) | 0.3700 (5) | 0.031 (2) | |
C2 | 0.0534 (5) | 0.3531 (5) | 0.4308 (5) | 0.026 (2) | |
C3 | −0.0503 (6) | 0.2653 (5) | 0.4522 (5) | 0.034 (2) | |
C4 | −0.0245 (6) | 0.1869 (5) | 0.5193 (6) | 0.038 (2) | |
C5 | 0.1137 (7) | 0.1984 (5) | 0.5673 (6) | 0.041 (3) | |
C6 | 0.2193 (6) | 0.2813 (5) | 0.5465 (5) | 0.036 (2) | |
C7 | 0.1909 (5) | 0.3581 (4) | 0.4766 (5) | 0.027 (2) | |
C8 | −0.1390 (7) | 0.0966 (6) | 0.5421 (6) | 0.058 (3) | |
C9 | 0.0038 (6) | 0.5371 (5) | 0.2030 (5) | 0.035 (2) | |
C10 | −0.1321 (6) | 0.5488 (5) | 0.1896 (5) | 0.038 (2) | |
C11 | −0.0900 (6) | 0.3038 (5) | 0.1578 (5) | 0.034 (2) | |
C12 | −0.0324 (6) | 0.2073 (5) | 0.1631 (5) | 0.029 (2) | |
C13 | 0.1175 (6) | 0.1244 (5) | 0.1937 (5) | 0.028 (2) | |
C14 | 0.2345 (6) | 0.0986 (5) | 0.2246 (5) | 0.034 (2) | |
C15 | 0.2117 (6) | −0.0292 (5) | 0.1950 (5) | 0.041 (3) | |
C16 | 0.0735 (7) | −0.1296 (5) | 0.1362 (5) | 0.040 (2) | |
C17 | −0.0452 (6) | −0.1069 (5) | 0.1078 (5) | 0.041 (2) | |
C18 | −0.0215 (6) | 0.0210 (5) | 0.1383 (5) | 0.032 (2) | |
C19 | −0.2693 (6) | 0.0097 (6) | 0.0699 (7) | 0.058 (3) | |
C20 | 0.4626 (6) | 0.3920 (5) | 0.2281 (5) | 0.032 (2) | |
C21 | 0.5876 (6) | 0.3604 (5) | 0.2738 (5) | 0.040 (2) | |
C22 | 0.4327 (6) | 0.7073 (5) | 0.4248 (6) | 0.033 (2) | |
C23 | 0.4759 (7) | 0.8493 (5) | 0.4513 (7) | 0.060 (3) | |
H1a | −0.06681 | 0.43970 | 0.36020 | 0.03700* | |
H1b | 0.09490 | 0.53120 | 0.42350 | 0.03700* | |
H3 | −0.14409 | 0.26000 | 0.41800 | 0.04100* | |
H5 | 0.13620 | 0.14750 | 0.61600 | 0.05000* | |
H6 | 0.31250 | 0.28630 | 0.57981 | 0.04300* | |
H06a | 0.26790 | 0.42250 | 0.10041 | 0.05400* | |
H06b | 0.19770 | 0.51930 | 0.08110 | 0.05400* | |
H8b | −0.10330 | 0.04850 | 0.58800 | 0.07000* | |
H8c | −0.21779 | 0.03950 | 0.46580 | 0.07000* | |
H8a | −0.17050 | 0.14440 | 0.58741 | 0.07000* | |
H9a | 0.00509 | 0.52391 | 0.12471 | 0.04200* | |
H9b | 0.08261 | 0.61610 | 0.25940 | 0.04200* | |
H10b | −0.21209 | 0.46881 | 0.13810 | 0.04600* | |
H10c | −0.13060 | 0.57210 | 0.26780 | 0.04600* | |
H10a | −0.13880 | 0.61310 | 0.15250 | 0.04600* | |
H11a | −0.12069 | 0.30931 | 0.07701 | 0.04100* | |
H11b | −0.16751 | 0.27900 | 0.17830 | 0.04100* | |
H14 | 0.32801 | 0.16610 | 0.26470 | 0.04000* | |
H15 | 0.29090 | −0.04889 | 0.21511 | 0.04800* | |
H16 | 0.06221 | −0.21560 | 0.11590 | 0.04700* | |
H17 | −0.13810 | −0.17500 | 0.06890 | 0.04900* | |
H19b | −0.30200 | −0.07760 | 0.02391 | 0.06900* | |
H19c | −0.29709 | 0.01261 | 0.13520 | 0.06900* | |
H19a | −0.31130 | 0.05030 | 0.01741 | 0.06900* | |
H21b | 0.58490 | 0.32460 | 0.33741 | 0.04900* | |
H21c | 0.67321 | 0.43560 | 0.30381 | 0.04900* | |
H21a | 0.58110 | 0.29870 | 0.20761 | 0.04900* | |
H23b | 0.46200 | 0.86860 | 0.37661 | 0.07300* | |
H23c | 0.57319 | 0.89540 | 0.50820 | 0.07300* | |
H23a | 0.41900 | 0.87250 | 0.48430 | 0.07300* | |
H7a | 0.66025 | 0.29930 | 0.80648 | 0.08600* | |
H7b | 0.61827 | 0.27783 | 0.89958 | 0.08600* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0249 (7) | 0.0222 (7) | 0.0267 (8) | 0.0057 (6) | 0.0077 (6) | 0.0022 (6) |
Ni2 | 0.0250 (5) | 0.0181 (5) | 0.0248 (5) | 0.0036 (4) | 0.0103 (4) | 0.0012 (4) |
O1 | 0.025 (2) | 0.022 (2) | 0.028 (2) | 0.0075 (16) | 0.0141 (18) | 0.0057 (17) |
O2 | 0.021 (2) | 0.026 (2) | 0.024 (2) | 0.0041 (16) | 0.0102 (18) | −0.0001 (17) |
O3 | 0.056 (3) | 0.085 (3) | 0.028 (3) | 0.042 (3) | 0.018 (2) | 0.006 (2) |
O4 | 0.029 (2) | 0.021 (2) | 0.030 (2) | 0.0042 (17) | 0.007 (2) | 0.0008 (17) |
O5 | 0.028 (2) | 0.0202 (19) | 0.034 (2) | 0.0076 (17) | 0.0049 (19) | 0.0044 (17) |
O6 | 0.036 (2) | 0.031 (2) | 0.032 (2) | 0.0102 (18) | 0.014 (2) | 0.0076 (18) |
O7 | 0.072 (3) | 0.053 (3) | 0.050 (3) | 0.024 (3) | 0.025 (3) | 0.017 (2) |
O8 | 0.112 (5) | 0.124 (5) | 0.078 (4) | 0.067 (4) | 0.061 (4) | 0.029 (4) |
N1 | 0.031 (3) | 0.022 (2) | 0.029 (3) | 0.010 (2) | 0.013 (2) | 0.007 (2) |
N2 | 0.027 (3) | 0.019 (2) | 0.024 (3) | 0.003 (2) | 0.009 (2) | 0.002 (2) |
N3 | 0.026 (2) | 0.022 (2) | 0.031 (3) | −0.002 (2) | 0.009 (2) | −0.002 (2) |
C1 | 0.030 (3) | 0.030 (3) | 0.029 (3) | 0.011 (3) | 0.012 (3) | 0.002 (3) |
C2 | 0.027 (3) | 0.021 (3) | 0.024 (3) | 0.005 (2) | 0.014 (3) | −0.001 (2) |
C3 | 0.032 (3) | 0.032 (3) | 0.029 (3) | 0.010 (3) | 0.016 (3) | −0.002 (3) |
C4 | 0.050 (4) | 0.026 (3) | 0.041 (4) | 0.010 (3) | 0.030 (3) | 0.008 (3) |
C5 | 0.055 (4) | 0.031 (3) | 0.046 (4) | 0.022 (3) | 0.029 (3) | 0.014 (3) |
C6 | 0.043 (4) | 0.036 (3) | 0.038 (4) | 0.020 (3) | 0.026 (3) | 0.015 (3) |
C7 | 0.031 (3) | 0.018 (3) | 0.026 (3) | 0.008 (2) | 0.014 (3) | −0.004 (2) |
C8 | 0.072 (5) | 0.044 (4) | 0.070 (5) | 0.017 (4) | 0.051 (4) | 0.019 (4) |
C9 | 0.034 (3) | 0.031 (3) | 0.037 (4) | 0.014 (3) | 0.014 (3) | 0.007 (3) |
C10 | 0.041 (3) | 0.037 (3) | 0.041 (4) | 0.021 (3) | 0.020 (3) | 0.013 (3) |
C11 | 0.030 (3) | 0.033 (3) | 0.028 (3) | 0.006 (3) | 0.012 (3) | 0.002 (3) |
C12 | 0.032 (3) | 0.021 (3) | 0.024 (3) | 0.004 (3) | 0.012 (3) | −0.001 (2) |
C13 | 0.035 (3) | 0.016 (3) | 0.021 (3) | 0.001 (2) | 0.012 (3) | −0.000 (2) |
C14 | 0.035 (3) | 0.023 (3) | 0.037 (4) | 0.008 (3) | 0.015 (3) | 0.006 (3) |
C15 | 0.054 (4) | 0.036 (3) | 0.037 (4) | 0.025 (3) | 0.018 (3) | 0.015 (3) |
C16 | 0.052 (4) | 0.016 (3) | 0.033 (4) | 0.005 (3) | 0.012 (3) | 0.001 (3) |
C17 | 0.046 (4) | 0.022 (3) | 0.031 (4) | −0.002 (3) | 0.011 (3) | −0.000 (3) |
C18 | 0.034 (3) | 0.025 (3) | 0.026 (3) | 0.006 (3) | 0.009 (3) | 0.003 (3) |
C19 | 0.034 (4) | 0.042 (4) | 0.068 (5) | −0.003 (3) | 0.016 (4) | 0.003 (4) |
C20 | 0.029 (3) | 0.029 (3) | 0.032 (4) | 0.004 (3) | 0.015 (3) | 0.006 (3) |
C21 | 0.035 (3) | 0.045 (4) | 0.040 (4) | 0.015 (3) | 0.022 (3) | 0.006 (3) |
C22 | 0.031 (3) | 0.025 (3) | 0.041 (4) | 0.010 (3) | 0.019 (3) | 0.009 (3) |
C23 | 0.048 (4) | 0.019 (3) | 0.074 (5) | 0.010 (3) | −0.003 (4) | 0.002 (3) |
Ni1—O5 | 2.014 (4) | C5—H5 | 0.946 (7) |
Ni1—O5i | 2.014 (4) | C5—C6 | 1.376 (10) |
Ni1—O1i | 2.036 (4) | C6—H6 | 0.950 (7) |
Ni1—O1 | 2.036 (4) | C6—C7 | 1.383 (9) |
Ni1—O2i | 2.138 (4) | C8—H8b | 0.948 (8) |
Ni1—O2 | 2.138 (4) | C8—H8c | 0.952 (5) |
Ni2—O1 | 2.035 (4) | C8—H8a | 0.955 (9) |
Ni2—O4 | 2.056 (3) | C9—H9a | 0.951 (7) |
Ni2—N2 | 2.073 (4) | C9—H9b | 0.952 (4) |
Ni2—O2 | 2.092 (4) | C9—C10 | 1.521 (10) |
Ni2—O6 | 2.099 (4) | C10—H10c | 0.944 (7) |
Ni2—N1 | 2.142 (5) | C10—H10b | 0.951 (4) |
O1—C7 | 1.348 (7) | C10—H10a | 0.955 (7) |
O2—C20 | 1.260 (9) | C11—H11b | 0.945 (7) |
O3—C20 | 1.254 (7) | C11—H11a | 0.950 (6) |
O4—C22 | 1.260 (5) | C11—C12 | 1.482 (9) |
O5—C22 | 1.245 (8) | C13—C14 | 1.378 (9) |
O6—H06a | 0.961 (5) | C13—C18 | 1.421 (6) |
O6—H06b | 0.998 (4) | C14—H14 | 0.947 (5) |
O7—H7a | 0.917 (5) | C14—C15 | 1.391 (9) |
O7—H7b | 0.922 (6) | C15—H15 | 0.949 (8) |
N1—C1 | 1.483 (8) | C15—C16 | 1.402 (7) |
N1—C9 | 1.490 (8) | C16—H16 | 0.949 (6) |
N1—C11 | 1.500 (5) | C16—C17 | 1.375 (11) |
N2—C12 | 1.310 (7) | C17—H17 | 0.945 (5) |
N2—C13 | 1.380 (8) | C17—C18 | 1.390 (8) |
N3—C18 | 1.368 (9) | C19—H19b | 0.951 (6) |
N3—C12 | 1.370 (6) | C19—H19c | 0.953 (9) |
N3—C19 | 1.472 (7) | C19—H19a | 0.953 (8) |
C1—H1a | 0.945 (7) | C20—C21 | 1.507 (10) |
C1—H1b | 0.954 (4) | C21—H21c | 0.942 (5) |
C1—C2 | 1.496 (9) | C21—H21b | 0.950 (7) |
C2—C3 | 1.393 (8) | C21—H21a | 0.955 (7) |
C2—C7 | 1.412 (8) | C22—C23 | 1.506 (8) |
C3—H3 | 0.955 (6) | C23—H23c | 0.946 (5) |
C3—C4 | 1.371 (9) | C23—H23a | 0.949 (9) |
C4—C5 | 1.389 (10) | C23—H23b | 0.953 (8) |
C4—C8 | 1.496 (10) | ||
O5—Ni1—O5i | 180.0000 | C5—C6—C7 | 120.4 (6) |
O5—Ni1—O1i | 93.77 (15) | O1—C7—C6 | 123.9 (5) |
O5—Ni1—O1 | 86.23 (15) | O1—C7—C2 | 117.3 (5) |
O5—Ni1—O2i | 87.40 (15) | C6—C7—C2 | 118.8 (6) |
O5—Ni1—O2 | 92.60 (15) | H8b—C8—H8c | 109.4 (6) |
O5i—Ni1—O1i | 86.23 (15) | H8b—C8—H8a | 109.2 (8) |
O5i—Ni1—O1 | 93.77 (15) | H8b—C8—C4 | 109.9 (7) |
O5i—Ni1—O2i | 92.60 (15) | H8c—C8—H8a | 108.8 (8) |
O5i—Ni1—O2 | 87.40 (15) | H8c—C8—C4 | 109.9 (7) |
O1i—Ni1—O1 | 180.0000 | H8a—C8—C4 | 109.6 (6) |
O1i—Ni1—O2i | 80.99 (15) | H9a—C9—H9b | 109.1 (6) |
O1i—Ni1—O2 | 99.01 (15) | H9a—C9—N1 | 107.3 (6) |
O1—Ni1—O2i | 99.01 (15) | H9a—C9—C10 | 108.3 (5) |
O1—Ni1—O2 | 80.99 (15) | H9b—C9—N1 | 107.3 (5) |
O2i—Ni1—O2 | 180.0000 | H9b—C9—C10 | 108.0 (6) |
O1—Ni2—O4 | 91.58 (14) | N1—C9—C10 | 116.7 (5) |
O1—Ni2—N2 | 92.33 (16) | H10c—C10—H10b | 110.0 (7) |
O1—Ni2—O2 | 82.14 (16) | H10c—C10—H10a | 109.5 (7) |
O1—Ni2—O6 | 174.29 (18) | H10c—C10—C9 | 109.9 (5) |
O1—Ni2—N1 | 94.44 (18) | H10b—C10—H10a | 109.0 (5) |
O4—Ni2—N2 | 172.96 (18) | H10b—C10—C9 | 109.3 (6) |
O4—Ni2—O2 | 88.72 (15) | H10a—C10—C9 | 109.1 (6) |
O4—Ni2—O6 | 87.65 (15) | H11b—C11—H11a | 110.0 (5) |
O4—Ni2—N1 | 92.56 (17) | H11b—C11—C12 | 109.5 (6) |
N2—Ni2—O2 | 97.61 (18) | H11b—C11—N1 | 109.7 (5) |
N2—Ni2—O6 | 89.04 (16) | H11a—C11—C12 | 109.3 (6) |
N2—Ni2—N1 | 81.30 (18) | H11a—C11—N1 | 109.4 (5) |
O2—Ni2—O6 | 92.18 (17) | C12—C11—N1 | 109.0 (4) |
O2—Ni2—N1 | 176.38 (19) | N2—C12—N3 | 111.8 (5) |
O6—Ni2—N1 | 91.25 (18) | N2—C12—C11 | 123.1 (4) |
C7—O1—Ni2 | 117.5 (3) | N3—C12—C11 | 125.0 (5) |
C7—O1—Ni1 | 135.6 (4) | C14—C13—N2 | 132.4 (4) |
Ni2—O1—Ni1 | 98.05 (19) | C14—C13—C18 | 119.6 (5) |
C20—O2—Ni2 | 128.7 (3) | N2—C13—C18 | 108.1 (5) |
C20—O2—Ni1 | 137.6 (4) | H14—C14—C13 | 120.9 (6) |
Ni2—O2—Ni1 | 93.17 (18) | H14—C14—C15 | 120.8 (7) |
C22—O4—Ni2 | 126.7 (4) | C13—C14—C15 | 118.3 (5) |
C22—O5—Ni1 | 130.5 (3) | H15—C15—C14 | 119.6 (5) |
H06a—O6—H06b | 108.7 (4) | H15—C15—C16 | 119.3 (6) |
H06a—O6—Ni2 | 89.0 (3) | C14—C15—C16 | 121.1 (7) |
H06b—O6—Ni2 | 112.5 (3) | H16—C16—C17 | 119.5 (5) |
H7a—O7—H7b | 99.5 (4) | H16—C16—C15 | 118.6 (7) |
C1—N1—C9 | 109.9 (5) | C17—C16—C15 | 121.9 (6) |
C1—N1—C11 | 110.0 (4) | H17—C17—C16 | 121.6 (6) |
C1—N1—Ni2 | 106.6 (3) | H17—C17—C18 | 121.8 (7) |
C9—N1—C11 | 110.1 (4) | C16—C17—C18 | 116.6 (5) |
C9—N1—Ni2 | 112.1 (4) | N3—C18—C17 | 131.9 (5) |
C11—N1—Ni2 | 108.1 (4) | N3—C18—C13 | 105.7 (5) |
C12—N2—C13 | 107.0 (4) | C17—C18—C13 | 122.4 (6) |
C12—N2—Ni2 | 111.8 (4) | H19b—C19—H19c | 109.2 (7) |
C13—N2—Ni2 | 141.1 (4) | H19b—C19—H19a | 109.3 (6) |
C18—N3—C12 | 107.4 (4) | H19b—C19—N3 | 109.9 (7) |
C18—N3—C19 | 126.4 (5) | H19c—C19—H19a | 109.0 (8) |
C12—N3—C19 | 126.2 (6) | H19c—C19—N3 | 109.7 (5) |
H1a—C1—H1b | 109.6 (7) | H19a—C19—N3 | 109.7 (6) |
H1a—C1—N1 | 107.9 (5) | O3—C20—O2 | 122.7 (6) |
H1a—C1—C2 | 107.9 (6) | O3—C20—C21 | 118.4 (7) |
H1b—C1—N1 | 107.6 (5) | O2—C20—C21 | 118.9 (5) |
H1b—C1—C2 | 107.6 (5) | H21c—C21—H21b | 110.1 (5) |
N1—C1—C2 | 116.1 (5) | H21c—C21—H21a | 109.7 (7) |
C3—C2—C7 | 118.2 (5) | H21c—C21—C20 | 109.7 (6) |
C3—C2—C1 | 121.1 (6) | H21b—C21—H21a | 109.1 (7) |
C7—C2—C1 | 120.5 (5) | H21b—C21—C20 | 109.0 (7) |
H3—C3—C4 | 118.7 (6) | H21a—C21—C20 | 109.3 (5) |
H3—C3—C2 | 117.8 (6) | O5—C22—O4 | 125.9 (5) |
C4—C3—C2 | 123.5 (6) | O5—C22—C23 | 116.8 (4) |
C3—C4—C5 | 116.5 (6) | O4—C22—C23 | 117.3 (6) |
C3—C4—C8 | 121.3 (6) | H23c—C23—H23a | 110.0 (7) |
C5—C4—C8 | 122.2 (6) | H23c—C23—H23b | 109.5 (7) |
H5—C5—C6 | 118.7 (7) | H23c—C23—C22 | 109.4 (7) |
H5—C5—C4 | 119.0 (7) | H23a—C23—H23b | 109.3 (7) |
C6—C5—C4 | 122.4 (6) | H23a—C23—C22 | 109.5 (6) |
H6—C6—C5 | 120.4 (7) | H23b—C23—C22 | 109.2 (6) |
H6—C6—C7 | 119.2 (6) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ni3(C18H22N3O)2(C2H3O2)4(H2O)2]·4H2O |
Mr | 1137.15 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 193 |
a, b, c (Å) | 11.130 (2), 11.732 (2), 12.258 (2) |
α, β, γ (°) | 99.66 (2), 110.34 (1), 110.23 (1) |
V (Å3) | 1330.6 (5) |
Z | 1 |
Radiation type | Cu Kα |
µ (mm−1) | 1.83 |
Crystal size (mm) | 0.12 × 0.12 × 0.02 |
Data collection | |
Diffractometer | Rigaku AFC-6R diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.873, 0.965 |
No. of measured, independent and observed [F > 2.5σ(Fo)'] reflections | 4152, 3940, 2872 |
Rint | 0.031 |
θmax (°) | 60.0 |
(sin θ/λ)max (Å−1) | 0.562 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.058, 0.047, 1.93 |
No. of reflections | 2865 |
No. of parameters | 322 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.64, −0.68 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1994), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1992-1997), SIR92 (Altomare et al., 1994), Xtal3.4 CRYLSQ (Hall et al., 1995), Xtal3.4 BONDLA CIFIO.
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