Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802006116/bt6133sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802006116/bt6133Isup2.hkl |
CCDC reference: 185750
All hydrogen atoms of the ligands were placed in idealized positions and refined as riding atoms with with fixed individual displacement parameters [U(H) = 1.2 Ueq(N), U(H) = 1.2 Ueq(C)]. Hydrogen atoms of the water molecules were located from the difference Fourier map. Their coordinates were not refined but their displacement parameters.
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998 ); software used to prepare material for publication: SHELXTL.
[Ni(C4H13N3)(C6H8N3O2)]I·H2O | F(000) = 920 |
Mr = 460.95 | Dx = 1.775 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 9.384 (5) Å | Cell parameters from 813 reflections |
b = 15.323 (7) Å | θ = 2.9–25.3° |
c = 12.667 (6) Å | µ = 2.93 mm−1 |
β = 108.758 (8)° | T = 293 K |
V = 1724.6 (14) Å3 | Block, purple |
Z = 4 | 0.50 × 0.41 × 0.29 mm |
CCD area detector diffractometer | 3673 independent reflections |
Radiation source: fine-focus sealed tube | 3280 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
phi and ω scans | θmax = 27.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS: Sheldrick, 1996; Blessing, 1995) | h = −11→7 |
Tmin = 0.322, Tmax = 0.483 | k = −19→17 |
9823 measured reflections | l = −16→16 |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.051 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0191P)2 + 1.0794P] where P = (Fo2 + 2Fc2)/3 |
3673 reflections | (Δ/σ)max = 0.002 |
192 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.68 e Å−3 |
[Ni(C4H13N3)(C6H8N3O2)]I·H2O | V = 1724.6 (14) Å3 |
Mr = 460.95 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.384 (5) Å | µ = 2.93 mm−1 |
b = 15.323 (7) Å | T = 293 K |
c = 12.667 (6) Å | 0.50 × 0.41 × 0.29 mm |
β = 108.758 (8)° |
CCD area detector diffractometer | 3673 independent reflections |
Absorption correction: multi-scan (SADABS: Sheldrick, 1996; Blessing, 1995) | 3280 reflections with I > 2σ(I) |
Tmin = 0.322, Tmax = 0.483 | Rint = 0.018 |
9823 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.051 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | Δρmax = 0.60 e Å−3 |
3673 reflections | Δρmin = −0.68 e Å−3 |
192 parameters |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) 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. |
x | y | z | Uiso*/Ueq | ||
I1 | 0.363034 (18) | 0.103023 (10) | 0.688563 (14) | 0.04352 (6) | |
Ni1 | 0.79822 (3) | 0.915238 (16) | 0.75632 (2) | 0.02584 (7) | |
N1 | 0.9742 (2) | 0.98089 (12) | 0.71850 (14) | 0.0328 (4) | |
H1C | 1.0181 | 1.0197 | 0.7738 | 0.039* | |
N2 | 0.6680 (2) | 0.97424 (13) | 0.60666 (15) | 0.0380 (4) | |
H2C | 0.6568 | 0.9379 | 0.5488 | 0.046* | |
H2D | 0.5762 | 0.9882 | 0.6097 | 0.046* | |
N3 | 0.8878 (2) | 0.80687 (12) | 0.69617 (15) | 0.0336 (4) | |
H3C | 0.9263 | 0.7686 | 0.7520 | 0.040* | |
H3D | 0.8140 | 0.7799 | 0.6425 | 0.040* | |
N4 | 0.7454 (2) | 1.01534 (11) | 0.85211 (14) | 0.0306 (4) | |
H4C | 0.8137 | 1.0586 | 0.8647 | 0.037* | |
H4D | 0.6537 | 1.0375 | 0.8167 | 0.037* | |
N5 | 0.4510 (2) | 0.74343 (13) | 0.75751 (18) | 0.0442 (5) | |
H5B | 0.3929 | 0.6999 | 0.7305 | 0.053* | |
N6 | 0.6226 (2) | 0.84410 (12) | 0.77719 (15) | 0.0337 (4) | |
C1 | 0.9110 (3) | 1.02831 (16) | 0.61223 (19) | 0.0418 (5) | |
H1A | 0.9166 | 0.9918 | 0.5512 | 0.050* | |
H1B | 0.9698 | 1.0805 | 0.6132 | 0.050* | |
C2 | 0.7500 (3) | 1.05306 (17) | 0.5943 (2) | 0.0459 (6) | |
H2A | 0.7448 | 1.0966 | 0.6485 | 0.055* | |
H2B | 0.7055 | 1.0775 | 0.5203 | 0.055* | |
C3 | 1.0063 (3) | 0.83522 (16) | 0.6509 (2) | 0.0428 (5) | |
H3A | 0.9622 | 0.8497 | 0.5726 | 0.051* | |
H3B | 1.0780 | 0.7883 | 0.6574 | 0.051* | |
C4 | 1.0854 (3) | 0.91398 (16) | 0.7147 (2) | 0.0424 (5) | |
H4A | 1.1437 | 0.8970 | 0.7900 | 0.051* | |
H4B | 1.1539 | 0.9378 | 0.6789 | 0.051* | |
C5 | 0.7486 (2) | 0.97372 (13) | 0.95797 (16) | 0.0303 (4) | |
H5A | 0.7617 | 1.0192 | 1.0147 | 0.036* | |
C6 | 0.8836 (2) | 0.91176 (12) | 0.99501 (17) | 0.0293 (4) | |
C7 | 0.6011 (3) | 0.92577 (16) | 0.94445 (19) | 0.0381 (5) | |
H7A | 0.6054 | 0.9024 | 1.0166 | 0.046* | |
H7B | 0.5201 | 0.9682 | 0.9235 | 0.046* | |
C8 | 0.5610 (2) | 0.85304 (14) | 0.86167 (18) | 0.0326 (4) | |
C9 | 0.5533 (3) | 0.77723 (15) | 0.71655 (19) | 0.0397 (5) | |
H9A | 0.5731 | 0.7565 | 0.6537 | 0.048* | |
C10 | 0.4551 (3) | 0.79035 (16) | 0.8500 (2) | 0.0439 (6) | |
H10A | 0.3967 | 0.7811 | 0.8960 | 0.053* | |
O1 | 0.93527 (18) | 0.88474 (10) | 0.91983 (12) | 0.0350 (3) | |
O2 | 0.9352 (2) | 0.89227 (10) | 1.09468 (12) | 0.0395 (4) | |
O1W | 0.1850 (2) | 0.78154 (13) | 0.99661 (15) | 0.0572 (5) | |
HW1 | 0.0993 | 0.8123 | 0.9720 | 0.087 (12)* | |
HW2 | 0.1524 | 0.7352 | 0.9496 | 0.085 (12)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
I1 | 0.03620 (9) | 0.04348 (10) | 0.04843 (10) | 0.00282 (6) | 0.01021 (7) | −0.00072 (6) |
Ni1 | 0.02600 (14) | 0.02975 (13) | 0.02187 (13) | −0.00023 (10) | 0.00783 (10) | −0.00186 (9) |
N1 | 0.0315 (9) | 0.0380 (10) | 0.0280 (9) | −0.0049 (8) | 0.0084 (7) | −0.0035 (7) |
N2 | 0.0326 (10) | 0.0525 (12) | 0.0260 (9) | 0.0051 (9) | 0.0056 (8) | 0.0006 (8) |
N3 | 0.0340 (10) | 0.0349 (10) | 0.0324 (9) | 0.0008 (8) | 0.0113 (8) | −0.0032 (7) |
N4 | 0.0322 (9) | 0.0282 (8) | 0.0276 (9) | 0.0038 (7) | 0.0046 (7) | 0.0007 (7) |
N5 | 0.0399 (11) | 0.0397 (11) | 0.0529 (12) | −0.0138 (9) | 0.0146 (10) | −0.0089 (9) |
N6 | 0.0350 (10) | 0.0339 (9) | 0.0359 (10) | −0.0054 (8) | 0.0167 (8) | −0.0082 (7) |
C1 | 0.0495 (14) | 0.0435 (13) | 0.0353 (12) | −0.0054 (11) | 0.0177 (11) | 0.0057 (10) |
C2 | 0.0555 (16) | 0.0473 (14) | 0.0346 (12) | 0.0079 (12) | 0.0141 (11) | 0.0117 (10) |
C3 | 0.0431 (14) | 0.0470 (14) | 0.0455 (13) | 0.0049 (11) | 0.0242 (11) | −0.0046 (11) |
C4 | 0.0285 (12) | 0.0525 (14) | 0.0485 (14) | −0.0011 (10) | 0.0156 (10) | −0.0015 (11) |
C5 | 0.0366 (11) | 0.0286 (10) | 0.0248 (10) | 0.0021 (8) | 0.0089 (9) | −0.0058 (8) |
C6 | 0.0345 (11) | 0.0249 (10) | 0.0264 (10) | −0.0023 (8) | 0.0067 (9) | −0.0019 (7) |
C7 | 0.0397 (13) | 0.0446 (12) | 0.0359 (12) | 0.0025 (10) | 0.0203 (10) | −0.0063 (10) |
C8 | 0.0292 (11) | 0.0370 (11) | 0.0339 (11) | 0.0013 (9) | 0.0135 (9) | −0.0013 (9) |
C9 | 0.0418 (13) | 0.0386 (12) | 0.0403 (12) | −0.0067 (10) | 0.0156 (11) | −0.0099 (10) |
C10 | 0.0391 (13) | 0.0486 (14) | 0.0497 (14) | −0.0061 (11) | 0.0224 (11) | −0.0012 (11) |
O1 | 0.0381 (8) | 0.0399 (8) | 0.0259 (7) | 0.0117 (7) | 0.0087 (6) | 0.0024 (6) |
O2 | 0.0531 (10) | 0.0373 (8) | 0.0240 (7) | 0.0041 (7) | 0.0067 (7) | 0.0033 (6) |
O1W | 0.0542 (11) | 0.0668 (13) | 0.0436 (10) | 0.0238 (10) | 0.0060 (9) | 0.0018 (9) |
Ni1—N6 | 2.0621 (19) | C1—C2 | 1.503 (4) |
Ni1—N2 | 2.1011 (19) | C1—H1A | 0.9700 |
Ni1—O1 | 2.1092 (17) | C1—H1B | 0.9700 |
Ni1—N4 | 2.1111 (18) | C2—H2A | 0.9700 |
Ni1—N3 | 2.1111 (19) | C2—H2B | 0.9700 |
Ni1—N1 | 2.1162 (19) | C3—C4 | 1.508 (3) |
N1—C4 | 1.474 (3) | C3—H3A | 0.9700 |
N1—C1 | 1.476 (3) | C3—H3B | 0.9700 |
N1—H1C | 0.9100 | C4—H4A | 0.9700 |
N2—C2 | 1.467 (3) | C4—H4B | 0.9700 |
N2—H2C | 0.9000 | C5—C7 | 1.527 (3) |
N2—H2D | 0.9000 | C5—C6 | 1.531 (3) |
N3—C3 | 1.471 (3) | C5—H5A | 0.9800 |
N3—H3C | 0.9000 | C6—O2 | 1.235 (3) |
N3—H3D | 0.9000 | C6—O1 | 1.269 (3) |
N4—C5 | 1.476 (3) | C7—C8 | 1.493 (3) |
N4—H4C | 0.9000 | C7—H7A | 0.9700 |
N4—H4D | 0.9000 | C7—H7B | 0.9700 |
N5—C9 | 1.334 (3) | C8—C10 | 1.356 (3) |
N5—C10 | 1.365 (3) | C9—H9A | 0.9300 |
N5—H5B | 0.8600 | C10—H10A | 0.9300 |
N6—C9 | 1.320 (3) | O1W—HW1 | 0.8967 |
N6—C8 | 1.377 (3) | O1W—HW2 | 0.9144 |
N6—Ni1—N2 | 94.94 (8) | N1—C1—H1B | 109.5 |
N6—Ni1—O1 | 90.98 (7) | C2—C1—H1B | 109.5 |
N2—Ni1—O1 | 167.26 (7) | H1A—C1—H1B | 108.1 |
N6—Ni1—N4 | 88.03 (7) | N2—C2—C1 | 108.2 (2) |
N2—Ni1—N4 | 91.72 (8) | N2—C2—H2A | 110.1 |
O1—Ni1—N4 | 77.19 (7) | C1—C2—H2A | 110.1 |
N6—Ni1—N3 | 93.31 (8) | N2—C2—H2B | 110.1 |
N2—Ni1—N3 | 101.33 (8) | C1—C2—H2B | 110.1 |
O1—Ni1—N3 | 89.56 (7) | H2A—C2—H2B | 108.4 |
N4—Ni1—N3 | 166.71 (7) | N3—C3—C4 | 109.31 (18) |
N6—Ni1—N1 | 173.81 (7) | N3—C3—H3A | 109.8 |
N2—Ni1—N1 | 82.02 (8) | C4—C3—H3A | 109.8 |
O1—Ni1—N1 | 93.09 (7) | N3—C3—H3B | 109.8 |
N4—Ni1—N1 | 97.42 (8) | C4—C3—H3B | 109.8 |
N3—Ni1—N1 | 82.06 (8) | H3A—C3—H3B | 108.3 |
C4—N1—C1 | 113.19 (18) | N1—C4—C3 | 110.04 (19) |
C4—N1—Ni1 | 106.77 (14) | N1—C4—H4A | 109.7 |
C1—N1—Ni1 | 109.06 (14) | C3—C4—H4A | 109.7 |
C4—N1—H1C | 109.2 | N1—C4—H4B | 109.7 |
C1—N1—H1C | 109.2 | C3—C4—H4B | 109.7 |
Ni1—N1—H1C | 109.2 | H4A—C4—H4B | 108.2 |
C2—N2—Ni1 | 106.12 (14) | N4—C5—C7 | 110.67 (17) |
C2—N2—H2C | 110.5 | N4—C5—C6 | 108.62 (16) |
Ni1—N2—H2C | 110.5 | C7—C5—C6 | 111.52 (18) |
C2—N2—H2D | 110.5 | N4—C5—H5A | 108.7 |
Ni1—N2—H2D | 110.5 | C7—C5—H5A | 108.7 |
H2C—N2—H2D | 108.7 | C6—C5—H5A | 108.7 |
C3—N3—Ni1 | 110.30 (14) | O2—C6—O1 | 124.7 (2) |
C3—N3—H3C | 109.6 | O2—C6—C5 | 118.49 (19) |
Ni1—N3—H3C | 109.6 | O1—C6—C5 | 116.77 (17) |
C3—N3—H3D | 109.6 | C8—C7—C5 | 116.89 (18) |
Ni1—N3—H3D | 109.6 | C8—C7—H7A | 108.1 |
H3C—N3—H3D | 108.1 | C5—C7—H7A | 108.1 |
C5—N4—Ni1 | 105.55 (12) | C8—C7—H7B | 108.1 |
C5—N4—H4C | 110.6 | C5—C7—H7B | 108.1 |
Ni1—N4—H4C | 110.6 | H7A—C7—H7B | 107.3 |
C5—N4—H4D | 110.6 | C10—C8—N6 | 108.74 (19) |
Ni1—N4—H4D | 110.6 | C10—C8—C7 | 128.0 (2) |
H4C—N4—H4D | 108.8 | N6—C8—C7 | 123.10 (19) |
C9—N5—C10 | 107.7 (2) | N6—C9—N5 | 110.9 (2) |
C9—N5—H5B | 126.1 | N6—C9—H9A | 124.5 |
C10—N5—H5B | 126.1 | N5—C9—H9A | 124.5 |
C9—N6—C8 | 106.13 (18) | C8—C10—N5 | 106.5 (2) |
C9—N6—Ni1 | 126.91 (15) | C8—C10—H10A | 126.8 |
C8—N6—Ni1 | 126.83 (14) | N5—C10—H10A | 126.8 |
N1—C1—C2 | 110.61 (18) | C6—O1—Ni1 | 113.91 (14) |
N1—C1—H1A | 109.5 | HW1—O1W—HW2 | 96.1 |
C2—C1—H1A | 109.5 | ||
N2—Ni1—N1—C4 | −123.43 (15) | Ni1—N2—C2—C1 | 49.1 (2) |
O1—Ni1—N1—C4 | 68.40 (14) | N1—C1—C2—N2 | −52.4 (3) |
N4—Ni1—N1—C4 | 145.87 (14) | Ni1—N3—C3—C4 | 31.7 (2) |
N3—Ni1—N1—C4 | −20.73 (14) | C1—N1—C4—C3 | −75.7 (2) |
N2—Ni1—N1—C1 | −0.79 (14) | Ni1—N1—C4—C3 | 44.3 (2) |
O1—Ni1—N1—C1 | −168.97 (14) | N3—C3—C4—N1 | −51.5 (3) |
N4—Ni1—N1—C1 | −91.49 (15) | Ni1—N4—C5—C7 | −81.26 (17) |
N3—Ni1—N1—C1 | 101.91 (15) | Ni1—N4—C5—C6 | 41.48 (17) |
N6—Ni1—N2—C2 | 158.90 (15) | N4—C5—C6—O2 | 157.18 (18) |
O1—Ni1—N2—C2 | 41.5 (4) | C7—C5—C6—O2 | −80.6 (2) |
N4—Ni1—N2—C2 | 70.73 (15) | N4—C5—C6—O1 | −22.2 (2) |
N3—Ni1—N2—C2 | −106.72 (15) | C7—C5—C6—O1 | 100.0 (2) |
N1—Ni1—N2—C2 | −26.53 (15) | N4—C5—C7—C8 | 61.2 (3) |
N6—Ni1—N3—C3 | 169.71 (15) | C6—C5—C7—C8 | −59.8 (3) |
N2—Ni1—N3—C3 | 74.00 (16) | C9—N6—C8—C10 | 0.2 (3) |
O1—Ni1—N3—C3 | −99.34 (15) | Ni1—N6—C8—C10 | −175.82 (16) |
N4—Ni1—N3—C3 | −94.8 (3) | C9—N6—C8—C7 | −175.4 (2) |
N1—Ni1—N3—C3 | −6.16 (15) | Ni1—N6—C8—C7 | 8.5 (3) |
N6—Ni1—N4—C5 | 55.03 (13) | C5—C7—C8—C10 | 165.6 (2) |
N2—Ni1—N4—C5 | 149.92 (13) | C5—C7—C8—N6 | −19.6 (3) |
O1—Ni1—N4—C5 | −36.42 (13) | C8—N6—C9—N5 | 0.2 (3) |
N3—Ni1—N4—C5 | −41.0 (4) | Ni1—N6—C9—N5 | 176.22 (16) |
N1—Ni1—N4—C5 | −127.91 (13) | C10—N5—C9—N6 | −0.5 (3) |
N2—Ni1—N6—C9 | 69.6 (2) | N6—C8—C10—N5 | −0.5 (3) |
O1—Ni1—N6—C9 | −121.7 (2) | C7—C8—C10—N5 | 174.9 (2) |
N4—Ni1—N6—C9 | 161.2 (2) | C9—N5—C10—C8 | 0.6 (3) |
N3—Ni1—N6—C9 | −32.1 (2) | O2—C6—O1—Ni1 | 170.75 (17) |
N2—Ni1—N6—C8 | −115.15 (19) | C5—C6—O1—Ni1 | −9.9 (2) |
O1—Ni1—N6—C8 | 53.55 (19) | N6—Ni1—O1—C6 | −60.92 (15) |
N4—Ni1—N6—C8 | −23.60 (18) | N2—Ni1—O1—C6 | 56.8 (4) |
N3—Ni1—N6—C8 | 143.16 (18) | N4—Ni1—O1—C6 | 26.84 (14) |
C4—N1—C1—C2 | 146.7 (2) | N3—Ni1—O1—C6 | −154.22 (15) |
Ni1—N1—C1—C2 | 28.0 (2) | N1—Ni1—O1—C6 | 123.76 (15) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.91 | 2.08 | 2.968 (3) | 165 |
N2—H2C···I1ii | 0.90 | 3.02 | 3.843 (3) | 153 |
N2—H2D···I1iii | 0.90 | 3.06 | 3.882 (2) | 152 |
N3—H3C···I1iv | 0.90 | 3.15 | 3.894 (2) | 141 |
N4—H4C···O2i | 0.90 | 2.37 | 3.184 (3) | 151 |
N4—H4D···I1iii | 0.90 | 2.87 | 3.767 (2) | 176 |
N5—H5B···O2v | 0.86 | 2.36 | 2.899 (3) | 121 |
N5—H5B···I1vi | 0.86 | 3.26 | 3.882 (2) | 132 |
O1W—HW1···O1vii | 0.90 | 1.84 | 2.733 (3) | 174 |
O1W—HW2···I1vi | 0.91 | 2.65 | 3.537 (2) | 164 |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) −x+3/2, y+1/2, −z+3/2; (v) x−1/2, −y+3/2, z−1/2; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Ni(C4H13N3)(C6H8N3O2)]I·H2O |
Mr | 460.95 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 9.384 (5), 15.323 (7), 12.667 (6) |
β (°) | 108.758 (8) |
V (Å3) | 1724.6 (14) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.93 |
Crystal size (mm) | 0.50 × 0.41 × 0.29 |
Data collection | |
Diffractometer | CCD area detector diffractometer |
Absorption correction | Multi-scan (SADABS: Sheldrick, 1996; Blessing, 1995) |
Tmin, Tmax | 0.322, 0.483 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9823, 3673, 3280 |
Rint | 0.018 |
(sin θ/λ)max (Å−1) | 0.638 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.051, 1.08 |
No. of reflections | 3673 |
No. of parameters | 192 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.60, −0.68 |
Computer programs: SMART (Bruker, 1998), SMART, SAINT-Plus (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998 ), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.91 | 2.08 | 2.968 (3) | 165.4 |
N2—H2C···I1ii | 0.90 | 3.02 | 3.843 (3) | 153.4 |
N2—H2D···I1iii | 0.90 | 3.06 | 3.882 (2) | 152.3 |
N3—H3C···I1iv | 0.90 | 3.15 | 3.894 (2) | 140.7 |
N4—H4C···O2i | 0.90 | 2.37 | 3.184 (3) | 151.0 |
N4—H4D···I1iii | 0.90 | 2.87 | 3.767 (2) | 175.7 |
N5—H5B···O2v | 0.86 | 2.36 | 2.899 (3) | 121.4 |
N5—H5B···I1vi | 0.86 | 3.26 | 3.882 (2) | 131.7 |
O1W—HW1···O1vii | 0.90 | 1.84 | 2.733 (3) | 174.1 |
O1W—HW2···I1vi | 0.91 | 2.65 | 3.537 (2) | 163.7 |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) −x+3/2, y+1/2, −z+3/2; (v) x−1/2, −y+3/2, z−1/2; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x−1, y, z. |
Previously we have reported the crystal structures of a series of amino acidato complexes with the formula [M(N4)(amino acidato)]n+, where N4 = triethylenetetraamine (trien) or tris(2-aminoethyl)amine (tren), M = Co3+, n = 2+ and M = Ni2+, n = 1+ (Cai et al., 2000, 2001, 2002; Hu et al., 2001). Their interesting packing arrangements directed by intermolecular hydrogen bonds were also discussed. Compared with the cobalt(III) analogues, structures of Ni(II) amino acidato complexes are less well documented (Cai et al., 2002).
In the title compound, Ni(II) is six-coordinated by three nitrogen atoms of the diethylenetriamine (dien) ligand, two N atoms and one O atom of the histidine ligand, as shown in Fig.1. Histidine is a potential multidentate ligand displaying varying coordination modes in different chemical environments. In the reported compond [Co(trien)(histidinato)](ClO4)2·2H2O (Hu et al., 2001), histidine is coordinated to Co(III) through one of the imidazol nitrogen atoms and the amino N atom. There are only two structures in the Cambridge Structural Database (Allen & Kennard, 1993) showing the tridentate coordination mode of histidine with Ni(II), namely [Ni(histidinato)(SCN)(H2O)2]·H2O (Shvelashvili et al., 1980, 1984; Sakurai et al., 1978) and [Ni(histidinato)2]·H2O (Shvelashvili et al., 1984; Sakurai et al., 1978). The bond lengths and angles of the Ni(II) coordination geometry in (I) are in agreement with these structures. The C–O bond lengths of the carboxylate group are 1.269 (3) and 1.235 (3) Å respectively, indicative of conjugated bonds.
As shown in Fig.2, the catonic complex is connected to another one, related by an inversion center, through complementary hydrogen bonds, formed by the free carboxylate oxygen atoms and the amino hydrogen atoms of both the dien and histidine ligands, leading to racemic pairs. These racemic pairs are further linked to each other via hydrogen bonds formed by the free carboxylate oxygen and the imidazol amino hydrogen and form an extended two-dimensional network along the bc plane. Both the crystalline water molecule and I- are involved in extensive hydrogen bonding with the cation, as shown in Table 1.