The title compound, [Ni(C14H16N8O2)2(H2O)4](CH3COO)2, is isostructural with the published CoII complex. The Ni atom occupies an inversion centre and is octahedrally coordinated by four aqua ligands and two molecules of the Schiff base.
Supporting information
CCDC reference: 242286
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.003 Å
- R factor = 0.038
- wR factor = 0.077
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 609.40 Ang-3
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
C2 H3 O2
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear (Rigaku, 1999); data reduction: CrystalStructure (Rigaku/MSC, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXTL.
Crystal data top
[Ni(C14H16N8O2)2(H2O)4](C2H3O2)2 | Z = 1 |
Mr = 577.21 | F(000) = 302 |
Triclinic, P1 | Dx = 1.573 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71070 Å |
a = 7.8498 (19) Å | Cell parameters from 2857 reflections |
b = 8.836 (2) Å | θ = 3.3–27.5° |
c = 10.2711 (17) Å | µ = 0.87 mm−1 |
α = 65.822 (15)° | T = 193 K |
β = 69.678 (16)° | Block, green |
γ = 82.14 (2)° | 0.56 × 0.21 × 0.10 mm |
V = 609.4 (2) Å3 | |
Data collection top
Rigaku Mercury CCD diffractometer | 2731 independent reflections |
Radiation source: fine-focus sealed tube | 2567 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
Detector resolution: 7.31 pixels mm-1 | θmax = 27.5°, θmin = 3.7° |
ω scans | h = −10→10 |
Absorption correction: multi-scan (Jacobson, 1998) | k = −11→11 |
Tmin = 0.643, Tmax = 0.918 | l = −13→11 |
6785 measured reflections | |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.077 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0234P)2 + 0.4761P] where P = (Fo2 + 2Fc2)/3 |
2731 reflections | (Δ/σ)max = 0.001 |
198 parameters | Δρmax = 0.29 e Å−3 |
0 restraints | Δρmin = −0.27 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.01550 (11) | |
O1 | 1.37861 (19) | 1.20067 (17) | −0.02653 (16) | 0.0248 (3) | |
O2 | 0.25190 (19) | 0.47181 (19) | 0.48349 (18) | 0.0231 (3) | |
O3 | 0.6289 (2) | 0.51561 (19) | 0.28078 (16) | 0.0204 (3) | |
O4 | 0.9793 (2) | 0.4510 (2) | 0.18607 (19) | 0.0316 (4) | |
O5 | 1.05363 (19) | 0.60590 (18) | 0.28327 (16) | 0.0255 (3) | |
N1 | 0.4678 (2) | 0.7599 (2) | 0.41767 (18) | 0.0190 (3) | |
N2 | 0.9296 (2) | 1.0631 (2) | 0.17038 (19) | 0.0222 (4) | |
N3 | 1.0764 (2) | 1.1672 (2) | 0.0907 (2) | 0.0256 (4) | |
N4 | 1.2605 (3) | 0.9399 (2) | 0.0947 (2) | 0.0251 (4) | |
C1 | 0.3062 (3) | 0.8327 (3) | 0.4540 (2) | 0.0236 (4) | |
H1 | 0.2004 | 0.7649 | 0.5110 | 0.028* | |
C2 | 0.2882 (3) | 1.0023 (3) | 0.4116 (2) | 0.0268 (4) | |
H2A | 0.1718 | 1.0500 | 0.4378 | 0.032* | |
C3 | 0.4415 (3) | 1.1019 (3) | 0.3306 (2) | 0.0250 (4) | |
H3A | 0.4320 | 1.2185 | 0.3026 | 0.030* | |
C4 | 0.6094 (3) | 1.0296 (2) | 0.2904 (2) | 0.0200 (4) | |
C5 | 0.6148 (3) | 0.8577 (2) | 0.3352 (2) | 0.0198 (4) | |
H5 | 0.7287 | 0.8075 | 0.3057 | 0.024* | |
C6 | 0.7752 (3) | 1.1301 (2) | 0.2085 (2) | 0.0219 (4) | |
H6 | 0.7683 | 1.2464 | 0.1832 | 0.026* | |
C7 | 1.2461 (3) | 1.1033 (2) | 0.0500 (2) | 0.0205 (4) | |
C8 | 1.0929 (3) | 0.5264 (2) | 0.1986 (2) | 0.0195 (4) | |
C9 | 1.2899 (3) | 0.5237 (3) | 0.1074 (3) | 0.0283 (5) | |
H9A | 1.3049 | 0.4496 | 0.0547 | 0.042* | |
H9B | 1.3637 | 0.4837 | 0.1747 | 0.042* | |
H9C | 1.3293 | 0.6361 | 0.0335 | 0.042* | |
H2B | 0.217 (4) | 0.524 (4) | 0.408 (3) | 0.048 (8)* | |
H2C | 0.155 (4) | 0.447 (4) | 0.563 (4) | 0.056 (9)* | |
H3B | 1.068 (3) | 1.262 (3) | 0.078 (3) | 0.024 (6)* | |
H3C | 0.743 (4) | 0.500 (4) | 0.261 (3) | 0.045 (8)* | |
H3D | 0.618 (4) | 0.599 (4) | 0.214 (4) | 0.060 (10)* | |
H4A | 1.168 (4) | 0.876 (3) | 0.152 (3) | 0.035 (7)* | |
H4B | 1.371 (4) | 0.896 (3) | 0.073 (3) | 0.035 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.01304 (17) | 0.01516 (18) | 0.01659 (18) | −0.00265 (12) | −0.00259 (13) | −0.00549 (14) |
O1 | 0.0204 (7) | 0.0192 (7) | 0.0268 (8) | −0.0041 (6) | −0.0027 (6) | −0.0042 (6) |
O2 | 0.0163 (7) | 0.0294 (8) | 0.0206 (7) | −0.0043 (6) | −0.0053 (6) | −0.0062 (6) |
O3 | 0.0174 (7) | 0.0217 (8) | 0.0183 (7) | −0.0001 (6) | −0.0035 (6) | −0.0058 (6) |
O4 | 0.0201 (7) | 0.0377 (9) | 0.0449 (10) | −0.0004 (6) | −0.0059 (7) | −0.0272 (8) |
O5 | 0.0218 (7) | 0.0301 (8) | 0.0250 (8) | −0.0035 (6) | −0.0029 (6) | −0.0137 (6) |
N1 | 0.0185 (8) | 0.0185 (8) | 0.0190 (8) | −0.0013 (6) | −0.0051 (6) | −0.0066 (7) |
N2 | 0.0232 (8) | 0.0184 (8) | 0.0226 (9) | −0.0042 (7) | −0.0040 (7) | −0.0071 (7) |
N3 | 0.0231 (9) | 0.0142 (9) | 0.0335 (10) | −0.0040 (7) | −0.0033 (8) | −0.0072 (8) |
N4 | 0.0226 (9) | 0.0173 (9) | 0.0298 (10) | −0.0018 (7) | −0.0035 (8) | −0.0073 (8) |
C1 | 0.0187 (9) | 0.0252 (11) | 0.0238 (10) | −0.0014 (8) | −0.0043 (8) | −0.0083 (8) |
C2 | 0.0218 (10) | 0.0255 (11) | 0.0298 (11) | 0.0058 (8) | −0.0067 (9) | −0.0107 (9) |
C3 | 0.0282 (11) | 0.0178 (10) | 0.0264 (11) | 0.0039 (8) | −0.0099 (9) | −0.0065 (8) |
C4 | 0.0231 (10) | 0.0172 (9) | 0.0186 (9) | −0.0013 (7) | −0.0064 (8) | −0.0056 (8) |
C5 | 0.0197 (9) | 0.0191 (10) | 0.0194 (9) | −0.0011 (7) | −0.0042 (8) | −0.0075 (8) |
C6 | 0.0267 (10) | 0.0140 (9) | 0.0230 (10) | −0.0016 (8) | −0.0074 (8) | −0.0053 (8) |
C7 | 0.0223 (9) | 0.0207 (10) | 0.0178 (9) | −0.0008 (8) | −0.0059 (8) | −0.0070 (8) |
C8 | 0.0169 (9) | 0.0195 (10) | 0.0193 (9) | 0.0008 (7) | −0.0053 (8) | −0.0054 (8) |
C9 | 0.0213 (10) | 0.0306 (12) | 0.0300 (11) | −0.0001 (9) | −0.0035 (9) | −0.0130 (9) |
Geometric parameters (Å, º) top
Ni1—O2 | 2.0689 (15) | N2—N3 | 1.364 (2) |
Ni1—O2i | 2.0689 (15) | N3—H3B | 0.79 (2) |
Ni1—O3 | 2.0770 (15) | N4—H4A | 0.86 (3) |
Ni1—O3i | 2.0770 (15) | N4—H4B | 0.89 (3) |
Ni1—N1i | 2.1098 (17) | C1—C2 | 1.381 (3) |
Ni1—N1 | 2.1098 (17) | C1—H1 | 0.9500 |
C7—O1 | 1.250 (2) | C2—C3 | 1.381 (3) |
O2—H2B | 0.84 (3) | C2—H2A | 0.9500 |
O2—H2C | 0.87 (3) | C3—C4 | 1.387 (3) |
O3—H3C | 0.85 (3) | C3—H3A | 0.9500 |
O3—H3D | 0.79 (4) | C4—C5 | 1.394 (3) |
C8—O4 | 1.252 (2) | C4—C6 | 1.461 (3) |
C8—O5 | 1.265 (2) | C5—H5 | 0.9500 |
C5—N1 | 1.338 (2) | C6—H6 | 0.9500 |
N1—C1 | 1.344 (3) | C8—C9 | 1.507 (3) |
C6—N2 | 1.279 (3) | C9—H9A | 0.9800 |
C7—N3 | 1.367 (3) | C9—H9B | 0.9800 |
C7—N4 | 1.326 (3) | C9—H9C | 0.9800 |
| | | |
O2—Ni1—O2i | 180.0 | N1—C1—C2 | 122.47 (19) |
O2—Ni1—O3 | 90.14 (6) | N1—C1—H1 | 118.8 |
O2i—Ni1—O3 | 89.86 (6) | C2—C1—H1 | 118.8 |
O2—Ni1—O3i | 89.86 (6) | C1—C2—C3 | 119.23 (19) |
O2i—Ni1—O3i | 90.14 (6) | C1—C2—H2A | 120.4 |
O3—Ni1—O3i | 180.0 | C3—C2—H2A | 120.4 |
O2—Ni1—N1 | 90.34 (6) | C2—C3—C4 | 119.28 (19) |
O2—Ni1—N1i | 89.66 (6) | C2—C3—H3A | 120.4 |
O2i—Ni1—N1i | 90.34 (6) | C4—C3—H3A | 120.4 |
O3—Ni1—N1 | 89.83 (6) | C3—C4—C5 | 117.69 (18) |
O3—Ni1—N1i | 90.17 (6) | C3—C4—C6 | 120.93 (18) |
O3i—Ni1—N1i | 89.83 (6) | C5—C4—C6 | 121.35 (18) |
O2i—Ni1—N1 | 89.66 (6) | N1—C5—C4 | 123.43 (18) |
O3i—Ni1—N1 | 90.17 (6) | N1—C5—H5 | 118.3 |
N1i—Ni1—N1 | 180.0 | C4—C5—H5 | 118.3 |
Ni1—O2—H2B | 126 (2) | N2—C6—C4 | 120.71 (18) |
Ni1—O2—H2C | 120 (2) | N2—C6—H6 | 119.6 |
H2B—O2—H2C | 107 (3) | C4—C6—H6 | 119.6 |
Ni1—O3—H3C | 113.0 (19) | O1—C7—N4 | 123.52 (19) |
Ni1—O3—H3D | 118 (2) | O1—C7—N3 | 118.87 (18) |
H3C—O3—H3D | 105 (3) | N4—C7—N3 | 117.61 (18) |
C5—N1—C1 | 117.85 (17) | O4—C8—O5 | 124.30 (18) |
C5—N1—Ni1 | 119.32 (13) | O4—C8—C9 | 118.62 (18) |
C1—N1—Ni1 | 122.64 (13) | O5—C8—C9 | 117.09 (17) |
C6—N2—N3 | 116.60 (17) | C8—C9—H9A | 109.5 |
N2—N3—C7 | 119.62 (17) | C8—C9—H9B | 109.5 |
N2—N3—H3B | 121.2 (17) | H9A—C9—H9B | 109.5 |
C7—N3—H3B | 118.5 (17) | C8—C9—H9C | 109.5 |
C7—N4—H4A | 121.1 (18) | H9A—C9—H9C | 109.5 |
C7—N4—H4B | 118.6 (17) | H9B—C9—H9C | 109.5 |
H4A—N4—H4B | 120 (2) | | |
| | | |
O2—Ni1—N1—C5 | −148.10 (14) | C1—C2—C3—C4 | 1.6 (3) |
O2i—Ni1—N1—C5 | 31.90 (14) | C2—C3—C4—C5 | −0.3 (3) |
O3—Ni1—N1—C5 | −57.96 (14) | C2—C3—C4—C6 | −178.24 (19) |
O3i—Ni1—N1—C5 | 122.04 (14) | C1—N1—C5—C4 | 2.5 (3) |
O2—Ni1—N1—C1 | 37.12 (16) | Ni1—N1—C5—C4 | −172.54 (15) |
O2i—Ni1—N1—C1 | −142.88 (16) | C3—C4—C5—N1 | −1.8 (3) |
O3—Ni1—N1—C1 | 127.26 (16) | C6—C4—C5—N1 | 176.11 (18) |
O3i—Ni1—N1—C1 | −52.74 (16) | N3—N2—C6—C4 | 178.32 (17) |
C6—N2—N3—C7 | 178.21 (19) | C3—C4—C6—N2 | −179.32 (19) |
C5—N1—C1—C2 | −1.1 (3) | C5—C4—C6—N2 | 2.8 (3) |
Ni1—N1—C1—C2 | 173.78 (16) | N2—N3—C7—O1 | 178.03 (17) |
N1—C1—C2—C3 | −0.9 (3) | N2—N3—C7—N4 | −2.0 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2b···O5ii | 0.84 (3) | 1.98 (3) | 2.789 (2) | 160 (3) |
N3—H3b···O4iii | 0.79 (2) | 2.27 (2) | 2.966 (2) | 147 (2) |
O3—H3c···O4 | 0.85 (3) | 1.81 (3) | 2.647 (2) | 166 (3) |
N4—H4a···O5 | 0.86 (3) | 2.33 (3) | 3.089 (3) | 147 (2) |
Symmetry codes: (ii) x−1, y, z; (iii) x, y+1, z. |