Two new nickel nitrates, diaquabis(3,4,7,8-tetramethyl-1,10-phenanthroline-κ2N,N′)nickel(II) dinitrate methanol solvate, [Ni(C16H16N2)2(H2O)2](NO3)2·CH4O, (I), and triaqua[2,4,6-tris(2-pyridyl)-1,3,5-triazine-κ3N1,N2,N6]nickel(II) dinitrate trihydrate, [Ni(C18H12N6)(H2O)3](NO3)2·3H2O, (II), are reported. In both structures, the cation is octahedrally coordinated, to two bidentate 3,4,7,8-tetramethyl-1,10-phenanthroline (tmp) and two water molecules in (I), and to one tridentate 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tpt) and three water molecules in (II). Both structures are stabilized by extensive hydrogen-bonding interactions.
Supporting information
CCDC references: 184462; 184463
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: XP in SHELXTL/PC (Sheldrick, 1994). Software used to prepare material for publication: SHELXL97 for (I); SHELXL97 (Sheldrick, 1997) for (II).
(I) Diaqua-bis(3,4,7,8-Tetramethyl-1,10-phenanthroline-N,
N')nickel(II)
dinitrate, methanol solvate
top
Crystal data top
[Ni(C16H16N2)2(H2O)2](NO3)2·CH4O | F(000) = 1520 |
Mr = 723.42 | Dx = 1.410 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.803 (1) Å | Cell parameters from 16736 reflections |
b = 25.951 (2) Å | θ = 1.6–28.1° |
c = 12.310 (1) Å | µ = 0.63 mm−1 |
β = 115.31 (1)° | T = 298 K |
V = 3408.4 (4) Å3 | Plates, pale violet |
Z = 4 | 0.40 × 0.30 × 0.12 mm |
Data collection top
CCD area detector diffractometer | 7275 independent reflections |
Radiation source: fine-focus sealed tube | 4648 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 27.0°, θmin = 1.6° |
Absorption correction: empirical (using intensity measurements) from intensities SADABS in SAINT-NT (Bruker, 2000) | h = −14→14 |
Tmin = 0.84, Tmax = 0.93 | k = −31→32 |
16404 measured reflections | l = −11→15 |
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)] = 0.056 | Hydrogen site location: geom+difmap |
wR(F2) = 0.163 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.95 | w = 1/[σ2(Fo2) + (0.104P)2] where P = (Fo2 + 2Fc2)/3 |
7275 reflections | (Δ/σ)max = 0.006 |
472 parameters | Δρmax = 0.70 e Å−3 |
10 restraints | Δρmin = −0.52 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 0.34455 (4) | 0.891896 (14) | 0.22967 (4) | 0.04620 (16) | |
O1W | 0.5272 (3) | 0.89432 (11) | 0.2410 (3) | 0.0654 (7) | |
H1WA | 0.588 (4) | 0.9050 (19) | 0.298 (4) | 0.15 (2)* | |
H1WB | 0.556 (4) | 0.8683 (14) | 0.221 (4) | 0.108 (18)* | |
O2W | 0.3704 (3) | 0.96657 (10) | 0.2986 (3) | 0.0651 (7) | |
H2WA | 0.326 (3) | 0.974 (2) | 0.331 (4) | 0.13 (2)* | |
H2WB | 0.442 (2) | 0.9693 (14) | 0.343 (3) | 0.056 (13)* | |
N1A | 0.2736 (2) | 0.92184 (10) | 0.0589 (2) | 0.0483 (6) | |
N2A | 0.1559 (3) | 0.89823 (9) | 0.1926 (3) | 0.0492 (6) | |
C1A | 0.3339 (3) | 0.93302 (13) | −0.0076 (3) | 0.0593 (9) | |
H1A | 0.4205 | 0.9292 | 0.0275 | 0.071* | |
C2A | 0.2770 (4) | 0.95008 (14) | −0.1260 (3) | 0.0648 (10) | |
C3A | 0.1486 (4) | 0.95613 (13) | −0.1805 (3) | 0.0620 (9) | |
C4A | 0.0810 (3) | 0.94589 (11) | −0.1109 (3) | 0.0520 (8) | |
C5A | −0.0513 (3) | 0.95371 (12) | −0.1522 (3) | 0.0589 (9) | |
H5A | −0.0976 | 0.9663 | −0.2294 | 0.071* | |
C6A | −0.1100 (3) | 0.94340 (12) | −0.0829 (3) | 0.0590 (9) | |
H6A | −0.1957 | 0.9494 | −0.1132 | 0.071* | |
C7A | −0.0459 (3) | 0.92360 (11) | 0.0355 (3) | 0.0516 (8) | |
C8A | −0.1045 (3) | 0.90950 (13) | 0.1104 (4) | 0.0609 (9) | |
C9A | −0.0316 (4) | 0.89113 (14) | 0.2240 (4) | 0.0675 (10) | |
C10A | 0.0989 (4) | 0.88634 (12) | 0.2614 (3) | 0.0596 (9) | |
H10A | 0.1475 | 0.8742 | 0.3386 | 0.072* | |
C11A | 0.0841 (3) | 0.91630 (11) | 0.0805 (3) | 0.0463 (7) | |
C12A | 0.1472 (3) | 0.92866 (11) | 0.0072 (3) | 0.0460 (7) | |
C13A | 0.3603 (4) | 0.9605 (2) | −0.1885 (4) | 0.0936 (14) | |
H13A | 0.3328 | 0.9401 | −0.2603 | 0.140* | |
H13B | 0.4452 | 0.9518 | −0.1359 | 0.140* | |
H13C | 0.3556 | 0.9964 | −0.2092 | 0.140* | |
C14A | 0.0822 (4) | 0.97219 (18) | −0.3091 (4) | 0.0892 (14) | |
H14A | 0.1398 | 0.9899 | −0.3325 | 0.134* | |
H14B | 0.0141 | 0.9948 | −0.3187 | 0.134* | |
H14C | 0.0502 | 0.9423 | −0.3587 | 0.134* | |
C15A | −0.2441 (4) | 0.91467 (18) | 0.0668 (5) | 0.0887 (14) | |
H15A | −0.2756 | 0.9392 | 0.0024 | 0.133* | |
H15B | −0.2624 | 0.9262 | 0.1316 | 0.133* | |
H15C | −0.2831 | 0.8819 | 0.0386 | 0.133* | |
C16A | −0.0845 (5) | 0.8739 (2) | 0.3113 (5) | 0.0967 (15) | |
H16A | −0.1327 | 0.9014 | 0.3228 | 0.145* | |
H16B | −0.0168 | 0.8651 | 0.3870 | 0.145* | |
H16C | −0.1372 | 0.8444 | 0.2793 | 0.145* | |
N1B | 0.4086 (2) | 0.85478 (9) | 0.3941 (2) | 0.0504 (7) | |
N2B | 0.3270 (2) | 0.81590 (10) | 0.1745 (2) | 0.0499 (6) | |
C1B | 0.4566 (3) | 0.87434 (13) | 0.5047 (3) | 0.0558 (9) | |
H1B | 0.4579 | 0.9100 | 0.5123 | 0.067* | |
C2B | 0.5054 (3) | 0.84504 (14) | 0.6103 (3) | 0.0617 (9) | |
C3B | 0.5026 (4) | 0.79205 (14) | 0.6020 (3) | 0.0645 (10) | |
C4B | 0.4560 (3) | 0.77028 (13) | 0.4860 (3) | 0.0595 (9) | |
C5B | 0.4535 (4) | 0.71559 (14) | 0.4645 (4) | 0.0750 (12) | |
H5B | 0.4798 | 0.6930 | 0.5293 | 0.090* | |
C6B | 0.4144 (4) | 0.69670 (14) | 0.3534 (4) | 0.0803 (13) | |
H6B | 0.4163 | 0.6612 | 0.3438 | 0.096* | |
C7B | 0.3700 (3) | 0.72834 (12) | 0.2494 (3) | 0.0600 (9) | |
C8B | 0.3272 (4) | 0.71017 (14) | 0.1299 (4) | 0.0682 (10) | |
C9B | 0.2840 (4) | 0.74465 (15) | 0.0373 (4) | 0.0694 (10) | |
C10B | 0.2853 (3) | 0.79697 (14) | 0.0647 (3) | 0.0587 (9) | |
H10B | 0.2546 | 0.8201 | 0.0010 | 0.070* | |
C11B | 0.3681 (3) | 0.78172 (11) | 0.2666 (3) | 0.0488 (8) | |
C12B | 0.4113 (3) | 0.80223 (12) | 0.3855 (3) | 0.0499 (8) | |
C13B | 0.5609 (4) | 0.87319 (17) | 0.7291 (3) | 0.0854 (13) | |
H13D | 0.5552 | 0.9097 | 0.7149 | 0.128* | |
H13E | 0.6473 | 0.8636 | 0.7727 | 0.128* | |
H13F | 0.5156 | 0.8642 | 0.7751 | 0.128* | |
C14B | 0.5463 (5) | 0.75900 (18) | 0.7131 (4) | 0.0926 (14) | |
H14D | 0.5952 | 0.7795 | 0.7824 | 0.139* | |
H14E | 0.5967 | 0.7312 | 0.7064 | 0.139* | |
H14F | 0.4750 | 0.7452 | 0.7215 | 0.139* | |
C15B | 0.3306 (5) | 0.65298 (15) | 0.1046 (5) | 0.1036 (17) | |
H15D | 0.2737 | 0.6459 | 0.0228 | 0.155* | |
H15E | 0.3063 | 0.6335 | 0.1575 | 0.155* | |
H15F | 0.4140 | 0.6434 | 0.1176 | 0.155* | |
C16B | 0.2341 (5) | 0.73004 (18) | −0.0939 (4) | 0.0963 (15) | |
H16D | 0.3022 | 0.7194 | −0.1116 | 0.144* | |
H16E | 0.1930 | 0.7592 | −0.1427 | 0.144* | |
H16F | 0.1753 | 0.7023 | −0.1106 | 0.144* | |
N1C | 0.7013 (3) | 0.98115 (13) | 0.4829 (3) | 0.0645 (8) | |
O1C | 0.7260 (3) | 0.94835 (12) | 0.4254 (3) | 0.0927 (9) | |
O2C | 0.5966 (3) | 1.00031 (16) | 0.4404 (4) | 0.1426 (17) | |
O3C | 0.7730 (3) | 1.00221 (18) | 0.5705 (3) | 0.1498 (19) | |
N1D | 0.4405 (5) | 0.1931 (2) | 0.9591 (5) | 0.1074 (14) | |
O1D | 0.3995 (3) | 0.18804 (15) | 0.8538 (3) | 0.1099 (11) | |
O2D | 0.5117 (4) | 0.16122 (19) | 1.0266 (4) | 0.1329 (14) | |
O3D | 0.4273 (9) | 0.2314 (3) | 1.0060 (5) | 0.286 (5) | |
O1X | 0.6846 (10) | 0.6840 (4) | 0.0233 (11) | 0.140 (3)* | 0.401 (8) |
C1X | 0.716 (2) | 0.6730 (10) | 0.138 (2) | 0.140 (3)* | 0.401 (8) |
O1Y | 0.6240 (16) | 0.6798 (6) | 0.1494 (16) | 0.140 (3)* | 0.294 (9) |
C1Y | 0.742 (2) | 0.6734 (11) | 0.217 (2) | 0.140 (3)* | 0.294 (9) |
O1Z | 0.674 (4) | 0.6672 (15) | 0.104 (4) | 0.140 (3)* | 0.151 (9) |
C1Z | 0.764 (4) | 0.6970 (19) | 0.175 (5) | 0.140 (3)* | 0.151 (9) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0555 (3) | 0.0376 (2) | 0.0446 (3) | 0.00071 (18) | 0.0205 (2) | 0.00038 (17) |
O1W | 0.0573 (15) | 0.0677 (17) | 0.0687 (19) | −0.0022 (14) | 0.0244 (14) | −0.0111 (14) |
O2W | 0.077 (2) | 0.0460 (13) | 0.0694 (18) | −0.0021 (14) | 0.0279 (18) | −0.0074 (13) |
N1A | 0.0518 (16) | 0.0452 (14) | 0.0505 (16) | 0.0048 (12) | 0.0243 (13) | 0.0077 (12) |
N2A | 0.0584 (17) | 0.0411 (14) | 0.0531 (17) | −0.0050 (12) | 0.0287 (14) | −0.0044 (12) |
C1A | 0.062 (2) | 0.058 (2) | 0.065 (2) | 0.0080 (17) | 0.0331 (19) | 0.0100 (18) |
C2A | 0.078 (3) | 0.061 (2) | 0.068 (2) | 0.0178 (19) | 0.043 (2) | 0.0196 (18) |
C3A | 0.081 (3) | 0.0519 (19) | 0.054 (2) | 0.0080 (18) | 0.030 (2) | 0.0077 (17) |
C4A | 0.065 (2) | 0.0367 (16) | 0.051 (2) | 0.0065 (15) | 0.0215 (17) | 0.0018 (14) |
C5A | 0.063 (2) | 0.0420 (18) | 0.059 (2) | 0.0017 (16) | 0.0133 (19) | −0.0003 (16) |
C6A | 0.052 (2) | 0.0461 (18) | 0.070 (2) | −0.0021 (15) | 0.0179 (19) | −0.0077 (17) |
C7A | 0.054 (2) | 0.0343 (15) | 0.066 (2) | −0.0057 (14) | 0.0256 (17) | −0.0117 (15) |
C8A | 0.061 (2) | 0.0470 (18) | 0.080 (3) | −0.0062 (16) | 0.035 (2) | −0.0105 (18) |
C9A | 0.076 (3) | 0.059 (2) | 0.085 (3) | −0.0131 (19) | 0.052 (2) | −0.012 (2) |
C10A | 0.075 (2) | 0.0523 (19) | 0.057 (2) | −0.0051 (17) | 0.0333 (19) | −0.0011 (16) |
C11A | 0.0542 (19) | 0.0329 (15) | 0.0516 (19) | −0.0033 (13) | 0.0225 (16) | −0.0060 (14) |
C12A | 0.058 (2) | 0.0339 (15) | 0.0469 (18) | 0.0032 (14) | 0.0232 (16) | −0.0006 (13) |
C13A | 0.103 (3) | 0.115 (4) | 0.082 (3) | 0.022 (3) | 0.057 (3) | 0.032 (3) |
C14A | 0.101 (3) | 0.097 (3) | 0.066 (3) | 0.014 (3) | 0.032 (2) | 0.026 (2) |
C15A | 0.061 (2) | 0.094 (3) | 0.117 (4) | −0.008 (2) | 0.043 (3) | −0.007 (3) |
C16A | 0.100 (3) | 0.116 (4) | 0.100 (4) | −0.012 (3) | 0.068 (3) | 0.003 (3) |
N1B | 0.0637 (17) | 0.0380 (13) | 0.0485 (16) | 0.0039 (12) | 0.0231 (14) | −0.0020 (12) |
N2B | 0.0583 (17) | 0.0458 (14) | 0.0469 (16) | −0.0029 (12) | 0.0237 (13) | −0.0069 (12) |
C1B | 0.070 (2) | 0.0463 (17) | 0.048 (2) | 0.0058 (16) | 0.0224 (18) | −0.0030 (15) |
C2B | 0.071 (2) | 0.064 (2) | 0.049 (2) | 0.0124 (18) | 0.0232 (18) | −0.0019 (17) |
C3B | 0.082 (3) | 0.064 (2) | 0.052 (2) | 0.020 (2) | 0.033 (2) | 0.0127 (18) |
C4B | 0.076 (2) | 0.0482 (19) | 0.060 (2) | 0.0121 (17) | 0.034 (2) | 0.0089 (16) |
C5B | 0.114 (3) | 0.0422 (19) | 0.078 (3) | 0.011 (2) | 0.050 (3) | 0.0146 (19) |
C6B | 0.123 (4) | 0.0338 (18) | 0.092 (3) | 0.004 (2) | 0.053 (3) | 0.0027 (19) |
C7B | 0.079 (2) | 0.0390 (17) | 0.067 (2) | −0.0026 (16) | 0.036 (2) | −0.0078 (16) |
C8B | 0.088 (3) | 0.0451 (19) | 0.081 (3) | −0.0068 (19) | 0.045 (2) | −0.0161 (19) |
C9B | 0.082 (3) | 0.065 (2) | 0.067 (3) | −0.005 (2) | 0.036 (2) | −0.022 (2) |
C10B | 0.069 (2) | 0.058 (2) | 0.049 (2) | −0.0024 (17) | 0.0248 (18) | −0.0080 (16) |
C11B | 0.059 (2) | 0.0389 (16) | 0.0535 (19) | −0.0014 (14) | 0.0285 (16) | −0.0029 (14) |
C12B | 0.064 (2) | 0.0387 (16) | 0.0504 (19) | 0.0030 (14) | 0.0271 (17) | 0.0001 (14) |
C13B | 0.111 (4) | 0.087 (3) | 0.046 (2) | 0.015 (3) | 0.022 (2) | −0.005 (2) |
C14B | 0.128 (4) | 0.091 (3) | 0.062 (3) | 0.037 (3) | 0.044 (3) | 0.031 (2) |
C15B | 0.154 (5) | 0.054 (2) | 0.110 (4) | −0.009 (3) | 0.063 (3) | −0.033 (2) |
C16B | 0.125 (4) | 0.092 (3) | 0.070 (3) | −0.001 (3) | 0.040 (3) | −0.035 (3) |
N1C | 0.061 (2) | 0.070 (2) | 0.0529 (19) | 0.0087 (17) | 0.0159 (17) | −0.0011 (16) |
O1C | 0.103 (2) | 0.082 (2) | 0.089 (2) | 0.0252 (17) | 0.0369 (18) | −0.0079 (17) |
O2C | 0.075 (2) | 0.164 (4) | 0.172 (4) | −0.012 (2) | 0.036 (2) | −0.098 (3) |
O3C | 0.087 (2) | 0.208 (5) | 0.099 (3) | 0.030 (3) | −0.012 (2) | −0.070 (3) |
N1D | 0.145 (4) | 0.116 (4) | 0.083 (3) | 0.024 (3) | 0.069 (3) | 0.012 (3) |
O1D | 0.134 (3) | 0.128 (3) | 0.070 (2) | 0.010 (2) | 0.046 (2) | −0.004 (2) |
O2D | 0.131 (3) | 0.153 (4) | 0.120 (3) | 0.016 (3) | 0.060 (3) | 0.032 (3) |
O3D | 0.478 (12) | 0.248 (7) | 0.155 (5) | 0.185 (8) | 0.158 (6) | −0.016 (5) |
Geometric parameters (Å, º) top
Ni1—N1A | 2.054 (3) | N1B—C1B | 1.330 (4) |
Ni1—N2B | 2.067 (3) | N1B—C12B | 1.369 (4) |
Ni1—N1B | 2.071 (3) | N2B—C10B | 1.320 (4) |
Ni1—N2A | 2.079 (3) | N2B—C11B | 1.355 (4) |
Ni1—O2W | 2.085 (3) | C1B—C2B | 1.400 (5) |
Ni1—O1W | 2.100 (3) | C1B—H1B | 0.9300 |
O1W—H1WA | 0.81 (3) | C2B—C3B | 1.378 (5) |
O1W—H1WB | 0.84 (3) | C2B—C13B | 1.511 (5) |
O2W—H2WA | 0.80 (3) | C3B—C4B | 1.411 (5) |
O2W—H2WB | 0.79 (2) | C3B—C14B | 1.507 (5) |
N1A—C1A | 1.326 (4) | C4B—C12B | 1.392 (4) |
N1A—C12A | 1.360 (4) | C4B—C5B | 1.442 (5) |
N2A—C10A | 1.323 (4) | C5B—C6B | 1.335 (5) |
N2A—C11A | 1.357 (4) | C5B—H5B | 0.9300 |
C1A—C2A | 1.390 (5) | C6B—C7B | 1.419 (5) |
C1A—H1A | 0.9300 | C6B—H6B | 0.9300 |
C2A—C3A | 1.379 (5) | C7B—C11B | 1.403 (4) |
C2A—C13A | 1.510 (5) | C7B—C8B | 1.417 (5) |
C3A—C4A | 1.424 (5) | C8B—C9B | 1.365 (5) |
C3A—C14A | 1.494 (5) | C8B—C15B | 1.520 (5) |
C4A—C12A | 1.397 (4) | C9B—C10B | 1.398 (5) |
C4A—C5A | 1.435 (5) | C9B—C16B | 1.511 (5) |
C5A—C6A | 1.335 (5) | C10B—H10B | 0.9300 |
C5A—H5A | 0.9300 | C11B—C12B | 1.431 (4) |
C6A—C7A | 1.421 (5) | C13B—H13D | 0.9600 |
C6A—H6A | 0.9300 | C13B—H13E | 0.9600 |
C7A—C11A | 1.404 (4) | C13B—H13F | 0.9600 |
C7A—C8A | 1.416 (5) | C14B—H14D | 0.9600 |
C8A—C9A | 1.376 (5) | C14B—H14E | 0.9600 |
C8A—C15A | 1.505 (5) | C14B—H14F | 0.9600 |
C9A—C10A | 1.413 (5) | C15B—H15D | 0.9600 |
C9A—C16A | 1.522 (6) | C15B—H15E | 0.9600 |
C10A—H10A | 0.9300 | C15B—H15F | 0.9600 |
C11A—C12A | 1.431 (4) | C16B—H16D | 0.9600 |
C13A—H13A | 0.9600 | C16B—H16E | 0.9600 |
C13A—H13B | 0.9600 | C16B—H16F | 0.9600 |
C13A—H13C | 0.9600 | N1C—O3C | 1.182 (4) |
C14A—H14A | 0.9600 | N1C—O1C | 1.220 (4) |
C14A—H14B | 0.9600 | N1C—O2C | 1.223 (4) |
C14A—H14C | 0.9600 | N1D—O1D | 1.180 (5) |
C15A—H15A | 0.9600 | N1D—O3D | 1.194 (6) |
C15A—H15B | 0.9600 | N1D—O2D | 1.218 (5) |
C15A—H15C | 0.9600 | O1X—C1X | 1.32 (2) |
C16A—H16A | 0.9600 | O1Y—C1Y | 1.30 (2) |
C16A—H16B | 0.9600 | O1Z—C1Z | 1.30 (2) |
C16A—H16C | 0.9600 | | |
| | | |
N1A—Ni1—N2B | 94.88 (10) | H15B—C15A—H15C | 109.5 |
N1A—Ni1—N1B | 174.33 (10) | C9A—C16A—H16A | 109.5 |
N2B—Ni1—N1B | 79.67 (10) | C9A—C16A—H16B | 109.5 |
N1A—Ni1—N2A | 79.39 (11) | H16A—C16A—H16B | 109.5 |
N2B—Ni1—N2A | 93.21 (10) | C9A—C16A—H16C | 109.5 |
N1B—Ni1—N2A | 99.21 (11) | H16A—C16A—H16C | 109.5 |
N1A—Ni1—O2W | 89.41 (11) | H16B—C16A—H16C | 109.5 |
N2B—Ni1—O2W | 175.63 (11) | C1B—N1B—C12B | 116.4 (3) |
N1B—Ni1—O2W | 96.06 (10) | C1B—N1B—Ni1 | 129.8 (2) |
N2A—Ni1—O2W | 88.41 (12) | C12B—N1B—Ni1 | 113.5 (2) |
N1A—Ni1—O1W | 90.83 (11) | C10B—N2B—C11B | 117.2 (3) |
N2B—Ni1—O1W | 90.36 (11) | C10B—N2B—Ni1 | 129.2 (2) |
N1B—Ni1—O1W | 90.78 (11) | C11B—N2B—Ni1 | 113.6 (2) |
N2A—Ni1—O1W | 169.84 (11) | N1B—C1B—C2B | 124.7 (3) |
O2W—Ni1—O1W | 88.72 (13) | N1B—C1B—H1B | 117.7 |
Ni1—O1W—H1WA | 125 (4) | C2B—C1B—H1B | 117.7 |
Ni1—O1W—H1WB | 119 (3) | C3B—C2B—C1B | 119.1 (3) |
H1WA—O1W—H1WB | 102 (3) | C3B—C2B—C13B | 122.7 (4) |
Ni1—O2W—H2WA | 114 (4) | C1B—C2B—C13B | 118.2 (3) |
Ni1—O2W—H2WB | 107 (3) | C2B—C3B—C4B | 117.5 (3) |
H2WA—O2W—H2WB | 112 (3) | C2B—C3B—C14B | 120.9 (4) |
C1A—N1A—C12A | 117.0 (3) | C4B—C3B—C14B | 121.7 (3) |
C1A—N1A—Ni1 | 128.5 (2) | C12B—C4B—C3B | 119.8 (3) |
C12A—N1A—Ni1 | 114.4 (2) | C12B—C4B—C5B | 116.9 (3) |
C10A—N2A—C11A | 117.6 (3) | C3B—C4B—C5B | 123.3 (3) |
C10A—N2A—Ni1 | 129.1 (3) | C6B—C5B—C4B | 121.4 (4) |
C11A—N2A—Ni1 | 113.3 (2) | C6B—C5B—H5B | 119.3 |
N1A—C1A—C2A | 124.8 (3) | C4B—C5B—H5B | 119.3 |
N1A—C1A—H1A | 117.6 | C5B—C6B—C7B | 122.9 (3) |
C2A—C1A—H1A | 117.6 | C5B—C6B—H6B | 118.5 |
C3A—C2A—C1A | 119.0 (3) | C7B—C6B—H6B | 118.5 |
C3A—C2A—C13A | 123.4 (4) | C11B—C7B—C8B | 117.6 (3) |
C1A—C2A—C13A | 117.6 (4) | C11B—C7B—C6B | 117.3 (3) |
C2A—C3A—C4A | 117.9 (3) | C8B—C7B—C6B | 125.1 (3) |
C2A—C3A—C14A | 121.2 (4) | C9B—C8B—C7B | 119.3 (3) |
C4A—C3A—C14A | 121.0 (4) | C9B—C8B—C15B | 120.2 (4) |
C12A—C4A—C3A | 118.5 (3) | C7B—C8B—C15B | 120.6 (4) |
C12A—C4A—C5A | 117.0 (3) | C8B—C9B—C10B | 118.3 (3) |
C3A—C4A—C5A | 124.4 (3) | C8B—C9B—C16B | 124.3 (4) |
C6A—C5A—C4A | 121.9 (3) | C10B—C9B—C16B | 117.4 (4) |
C6A—C5A—H5A | 119.1 | N2B—C10B—C9B | 124.7 (4) |
C4A—C5A—H5A | 119.1 | N2B—C10B—H10B | 117.6 |
C5A—C6A—C7A | 122.3 (3) | C9B—C10B—H10B | 117.6 |
C5A—C6A—H6A | 118.9 | N2B—C11B—C7B | 122.9 (3) |
C7A—C6A—H6A | 118.9 | N2B—C11B—C12B | 117.1 (3) |
C11A—C7A—C8A | 117.6 (3) | C7B—C11B—C12B | 120.0 (3) |
C11A—C7A—C6A | 117.8 (3) | N1B—C12B—C4B | 122.5 (3) |
C8A—C7A—C6A | 124.6 (3) | N1B—C12B—C11B | 116.1 (3) |
C9A—C8A—C7A | 119.0 (3) | C4B—C12B—C11B | 121.4 (3) |
C9A—C8A—C15A | 120.4 (4) | C2B—C13B—H13D | 109.5 |
C7A—C8A—C15A | 120.6 (4) | C2B—C13B—H13E | 109.5 |
C8A—C9A—C10A | 118.8 (4) | H13D—C13B—H13E | 109.5 |
C8A—C9A—C16A | 123.6 (4) | C2B—C13B—H13F | 109.5 |
C10A—C9A—C16A | 117.6 (4) | H13D—C13B—H13F | 109.5 |
N2A—C10A—C9A | 123.6 (4) | H13E—C13B—H13F | 109.5 |
N2A—C10A—H10A | 118.2 | C3B—C14B—H14D | 109.5 |
C9A—C10A—H10A | 118.2 | C3B—C14B—H14E | 109.5 |
N2A—C11A—C7A | 123.4 (3) | H14D—C14B—H14E | 109.5 |
N2A—C11A—C12A | 116.9 (3) | C3B—C14B—H14F | 109.5 |
C7A—C11A—C12A | 119.8 (3) | H14D—C14B—H14F | 109.5 |
N1A—C12A—C4A | 122.9 (3) | H14E—C14B—H14F | 109.5 |
N1A—C12A—C11A | 116.0 (3) | C8B—C15B—H15D | 109.5 |
C4A—C12A—C11A | 121.1 (3) | C8B—C15B—H15E | 109.5 |
C2A—C13A—H13A | 109.5 | H15D—C15B—H15E | 109.5 |
C2A—C13A—H13B | 109.5 | C8B—C15B—H15F | 109.5 |
H13A—C13A—H13B | 109.5 | H15D—C15B—H15F | 109.5 |
C2A—C13A—H13C | 109.5 | H15E—C15B—H15F | 109.5 |
H13A—C13A—H13C | 109.5 | C9B—C16B—H16D | 109.5 |
H13B—C13A—H13C | 109.5 | C9B—C16B—H16E | 109.5 |
C3A—C14A—H14A | 109.5 | H16D—C16B—H16E | 109.5 |
C3A—C14A—H14B | 109.5 | C9B—C16B—H16F | 109.5 |
H14A—C14A—H14B | 109.5 | H16D—C16B—H16F | 109.5 |
C3A—C14A—H14C | 109.5 | H16E—C16B—H16F | 109.5 |
H14A—C14A—H14C | 109.5 | O3C—N1C—O1C | 126.6 (4) |
H14B—C14A—H14C | 109.5 | O3C—N1C—O2C | 113.6 (4) |
C8A—C15A—H15A | 109.5 | O1C—N1C—O2C | 119.0 (4) |
C8A—C15A—H15B | 109.5 | O1D—N1D—O3D | 123.1 (6) |
H15A—C15A—H15B | 109.5 | O1D—N1D—O2D | 120.9 (5) |
C8A—C15A—H15C | 109.5 | O3D—N1D—O2D | 115.5 (6) |
H15A—C15A—H15C | 109.5 | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O1C | 0.81 (3) | 2.05 (3) | 2.842 (5) | 166 (7) |
O1W—H1WB···O1Di | 0.84 (3) | 1.92 (3) | 2.746 (5) | 169 (5) |
O2W—H2WA···O3Cii | 0.79 (3) | 2.12 (3) | 2.907 (6) | 173 (5) |
O2W—H2WB···O2C | 0.79 (3) | 1.88 (3) | 2.638 (5) | 160 (4) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+2, −z+1. |
(II) Triaqua-(2,4,6-tris(2-Pyridyl)-1,3,5-triazine-N,
N',
N")nickel(II),
dinitrate, trihydrate
top
Crystal data top
[Ni(C18H12N6)(H2O)3](NO3)2·3H2O | F(000) = 1248 |
Mr = 603.16 | Dx = 1.574 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
a = 12.328 (2) Å | Cell parameters from 7432 reflections |
b = 14.851 (3) Å | θ = 2.2–28.1° |
c = 14.124 (3) Å | µ = 0.84 mm−1 |
β = 100.06 (3)° | T = 298 K |
V = 2546.0 (8) Å3 | Blocks, green |
Z = 4 | 0.38 × 0.26 × 0.18 mm |
Data collection top
Bruker CCD area-detector diffractometer | 3955 independent reflections |
Radiation source: fine-focus sealed tube | 3550 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
φ and ω scans | θmax = 27.0°, θmin = 2.2° |
Absorption correction: empirical (using intensity measurements) from intensities SADABS in SAINT_NT (Bruker, 2000) | h = −8→15 |
Tmin = 0.76, Tmax = 0.83 | k = −18→18 |
7312 measured reflections | l = −17→17 |
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)] = 0.037 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.092 | w = 1/[σ2(Fo2) + (0.0747P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.008 |
3955 reflections | Δρmax = 0.54 e Å−3 |
402 parameters | Δρmin = −0.30 e Å−3 |
21 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.087 (16) |
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 | 0.21167 (7) | 0.77296 (2) | 0.25179 (6) | 0.03233 (11) | |
O1W | 0.2663 (4) | 0.7798 (2) | 0.1201 (3) | 0.0470 (9) | |
H1WA | 0.290 (3) | 0.7272 (11) | 0.101 (2) | 0.023 (9)* | |
H1WB | 0.304 (3) | 0.8249 (15) | 0.098 (3) | 0.045 (13)* | |
O2W | 0.1609 (3) | 0.77046 (19) | 0.3837 (2) | 0.0412 (8) | |
H2WA | 0.157 (6) | 0.7139 (18) | 0.405 (5) | 0.13 (3)* | |
H2WB | 0.100 (3) | 0.802 (3) | 0.388 (4) | 0.083 (19)* | |
O3W | 0.2097 (4) | 0.90789 (13) | 0.2570 (3) | 0.0542 (7) | |
H3WA | 0.184 (3) | 0.942 (2) | 0.2053 (16) | 0.035 (10)* | |
H3WB | 0.197 (6) | 0.933 (3) | 0.3119 (16) | 0.15 (3)* | |
N1 | 0.0489 (4) | 0.7416 (2) | 0.1766 (3) | 0.0341 (9) | |
N2 | 0.2145 (4) | 0.64052 (14) | 0.2478 (3) | 0.0317 (5) | |
N3 | 0.3724 (4) | 0.7415 (2) | 0.3239 (3) | 0.0325 (9) | |
N4 | 0.1179 (3) | 0.5064 (2) | 0.2071 (3) | 0.0355 (8) | |
N5 | 0.3054 (3) | 0.5047 (2) | 0.2901 (3) | 0.0368 (9) | |
N6 | 0.2949 (3) | 0.3236 (2) | 0.3018 (3) | 0.0387 (9) | |
C1 | −0.0314 (5) | 0.7979 (3) | 0.1365 (4) | 0.0387 (11) | |
H1 | −0.0212 | 0.8595 | 0.1457 | 0.046* | |
C2 | −0.1284 (5) | 0.7676 (3) | 0.0822 (4) | 0.0390 (13) | |
H2 | −0.1811 | 0.8083 | 0.0531 | 0.047* | |
C3 | −0.1461 (4) | 0.6778 (3) | 0.0716 (3) | 0.0412 (11) | |
H3 | −0.2118 | 0.6567 | 0.0360 | 0.049* | |
C4 | −0.0650 (4) | 0.6168 (3) | 0.1144 (3) | 0.0398 (11) | |
H4 | −0.0758 | 0.5548 | 0.1093 | 0.048* | |
C5 | 0.0310 (4) | 0.6527 (3) | 0.1642 (3) | 0.0335 (10) | |
C6 | 0.1235 (4) | 0.5952 (3) | 0.2077 (3) | 0.0340 (10) | |
C7 | 0.2106 (5) | 0.46443 (17) | 0.2474 (4) | 0.0334 (6) | |
C8 | 0.3008 (4) | 0.5941 (3) | 0.2880 (3) | 0.0300 (9) | |
C9 | 0.3936 (4) | 0.6514 (3) | 0.3335 (3) | 0.0322 (10) | |
C10 | 0.4923 (4) | 0.6181 (3) | 0.3832 (3) | 0.0397 (11) | |
H10 | 0.5045 | 0.5563 | 0.3882 | 0.048* | |
C11 | 0.5712 (4) | 0.6768 (3) | 0.4244 (3) | 0.0443 (12) | |
H11 | 0.6377 | 0.6558 | 0.4586 | 0.053* | |
C12 | 0.5509 (5) | 0.7690 (3) | 0.4149 (4) | 0.0408 (13) | |
H12 | 0.6037 | 0.8105 | 0.4423 | 0.049* | |
C13 | 0.4511 (4) | 0.7975 (3) | 0.3639 (4) | 0.0370 (11) | |
H13 | 0.4384 | 0.8591 | 0.3572 | 0.044* | |
C14 | 0.2097 (5) | 0.36407 (18) | 0.2460 (4) | 0.0355 (6) | |
C15 | 0.2943 (6) | 0.2327 (3) | 0.3020 (4) | 0.0501 (15) | |
H15 | 0.3518 | 0.2024 | 0.3405 | 0.060* | |
C16 | 0.2121 (7) | 0.1830 (2) | 0.2474 (5) | 0.0535 (9) | |
H16 | 0.2149 | 0.1204 | 0.2490 | 0.064* | |
C17 | 0.1271 (6) | 0.2256 (3) | 0.1913 (4) | 0.0539 (17) | |
H17 | 0.0711 | 0.1927 | 0.1542 | 0.065* | |
C18 | 0.1251 (5) | 0.3179 (4) | 0.1901 (4) | 0.0490 (13) | |
H18 | 0.0676 | 0.3488 | 0.1523 | 0.059* | |
N1A | −0.6697 (3) | 0.4419 (2) | 0.5525 (3) | 0.0501 (9) | |
O1A | −0.6169 (4) | 0.3723 (3) | 0.5772 (3) | 0.0806 (11) | |
O2A | −0.7716 (4) | 0.4345 (3) | 0.5326 (3) | 0.0874 (12) | |
O3A | −0.6241 (4) | 0.5130 (2) | 0.5455 (3) | 0.0950 (13) | |
N1B | −0.1623 (3) | 0.5408 (2) | 0.4476 (2) | 0.0501 (8) | |
O1B | −0.2548 (3) | 0.5029 (2) | 0.4344 (3) | 0.0695 (10) | |
O2B | −0.1015 (3) | 0.5280 (2) | 0.3897 (3) | 0.0725 (9) | |
O3B | −0.1340 (3) | 0.5896 (2) | 0.5182 (2) | 0.0737 (10) | |
O4W | −0.3732 (4) | 0.4967 (2) | 0.5991 (3) | 0.0691 (9) | |
H4WA | −0.329 (3) | 0.509 (3) | 0.557 (3) | 0.051 (15)* | |
H4WB | −0.4447 (15) | 0.492 (5) | 0.574 (4) | 0.13 (3)* | |
O5W | −0.5015 (3) | 0.3779 (2) | 0.4124 (3) | 0.0635 (8) | |
H5WA | −0.567 (2) | 0.381 (3) | 0.373 (3) | 0.068 (15)* | |
H5WB | −0.512 (5) | 0.369 (6) | 0.4735 (17) | 0.19 (4)* | |
O6W | 0.1224 (4) | 0.5990 (2) | 0.4423 (3) | 0.0773 (11) | |
H6WA | 0.166 (2) | 0.5504 (16) | 0.451 (3) | 0.020 (9)* | |
H6WB | 0.0500 (13) | 0.588 (3) | 0.426 (7) | 0.15 (4)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0324 (2) | 0.02447 (16) | 0.03680 (18) | 0.0023 (3) | −0.00307 (14) | −0.0006 (3) |
O1W | 0.057 (2) | 0.0383 (18) | 0.0468 (19) | −0.0002 (15) | 0.0118 (18) | 0.0039 (13) |
O2W | 0.041 (2) | 0.0420 (19) | 0.0382 (17) | 0.0066 (14) | 0.0003 (15) | 0.0019 (12) |
O3W | 0.0827 (18) | 0.0259 (9) | 0.0449 (14) | −0.001 (2) | −0.0140 (13) | 0.0014 (18) |
N1 | 0.031 (2) | 0.0291 (18) | 0.038 (2) | −0.0017 (19) | −0.0033 (18) | 0.0004 (17) |
N2 | 0.0308 (12) | 0.0254 (9) | 0.0356 (11) | −0.002 (2) | −0.0030 (9) | −0.004 (2) |
N3 | 0.030 (2) | 0.0295 (18) | 0.036 (2) | −0.0026 (19) | 0.0008 (18) | −0.0001 (17) |
N4 | 0.031 (2) | 0.0294 (18) | 0.0424 (19) | −0.0031 (17) | −0.0049 (16) | −0.0054 (15) |
N5 | 0.044 (2) | 0.0255 (17) | 0.0390 (17) | 0.0015 (18) | 0.0022 (17) | −0.0021 (15) |
N6 | 0.046 (2) | 0.0250 (17) | 0.045 (2) | −0.0009 (17) | 0.0049 (18) | 0.0018 (15) |
C1 | 0.037 (3) | 0.036 (2) | 0.041 (3) | 0.007 (2) | 0.000 (2) | 0.006 (2) |
C2 | 0.031 (3) | 0.039 (3) | 0.043 (3) | 0.006 (2) | −0.006 (2) | 0.0073 (18) |
C3 | 0.026 (3) | 0.050 (3) | 0.041 (2) | 0.003 (2) | −0.011 (2) | 0.002 (2) |
C4 | 0.029 (3) | 0.040 (2) | 0.043 (3) | −0.001 (2) | −0.0119 (19) | −0.0031 (19) |
C5 | 0.035 (3) | 0.028 (2) | 0.033 (2) | 0.0064 (19) | −0.0057 (19) | 0.0023 (17) |
C6 | 0.039 (3) | 0.032 (2) | 0.028 (2) | −0.001 (2) | −0.0026 (19) | −0.0017 (17) |
C7 | 0.0370 (15) | 0.0273 (11) | 0.0343 (13) | 0.004 (3) | 0.0014 (11) | −0.002 (2) |
C8 | 0.025 (2) | 0.028 (2) | 0.036 (2) | 0.0011 (19) | 0.0030 (18) | 0.0000 (18) |
C9 | 0.031 (2) | 0.034 (2) | 0.032 (2) | 0.0053 (19) | 0.0045 (19) | 0.0010 (18) |
C10 | 0.042 (3) | 0.033 (2) | 0.042 (3) | 0.004 (2) | 0.003 (2) | 0.0030 (18) |
C11 | 0.041 (3) | 0.048 (3) | 0.042 (2) | 0.008 (2) | 0.002 (2) | 0.003 (2) |
C12 | 0.034 (3) | 0.050 (3) | 0.038 (3) | −0.010 (2) | 0.004 (2) | −0.0062 (19) |
C13 | 0.035 (3) | 0.033 (2) | 0.041 (3) | −0.001 (2) | 0.002 (2) | 0.001 (2) |
C14 | 0.0396 (16) | 0.0294 (12) | 0.0373 (16) | 0.005 (3) | 0.0058 (13) | 0.008 (2) |
C15 | 0.066 (4) | 0.032 (3) | 0.055 (3) | 0.013 (2) | 0.018 (3) | 0.006 (2) |
C16 | 0.074 (2) | 0.0284 (13) | 0.063 (2) | −0.012 (4) | 0.0236 (19) | −0.014 (3) |
C17 | 0.063 (4) | 0.036 (3) | 0.062 (4) | −0.005 (2) | 0.007 (3) | −0.010 (2) |
C18 | 0.053 (3) | 0.040 (2) | 0.052 (3) | −0.010 (2) | 0.003 (2) | −0.006 (2) |
N1A | 0.057 (3) | 0.0408 (18) | 0.0537 (19) | −0.0020 (18) | 0.0139 (18) | 0.0008 (15) |
O1A | 0.073 (3) | 0.077 (2) | 0.094 (3) | 0.019 (2) | 0.021 (2) | 0.0273 (19) |
O2A | 0.061 (3) | 0.095 (3) | 0.106 (3) | −0.011 (2) | 0.015 (2) | 0.005 (2) |
O3A | 0.134 (4) | 0.0559 (19) | 0.095 (3) | −0.036 (2) | 0.020 (3) | −0.0024 (18) |
N1B | 0.059 (2) | 0.0331 (15) | 0.0541 (19) | 0.0130 (17) | −0.0011 (18) | 0.0006 (14) |
O1B | 0.068 (2) | 0.0593 (19) | 0.076 (2) | −0.0071 (18) | 0.0007 (19) | 0.0014 (17) |
O2B | 0.076 (2) | 0.068 (2) | 0.077 (2) | 0.0053 (19) | 0.0211 (19) | −0.0126 (17) |
O3B | 0.082 (2) | 0.0614 (17) | 0.071 (2) | 0.0062 (18) | −0.0064 (18) | −0.0286 (16) |
O4W | 0.081 (3) | 0.0565 (19) | 0.0599 (19) | −0.006 (2) | −0.014 (2) | −0.0062 (16) |
O5W | 0.0490 (19) | 0.0659 (19) | 0.071 (2) | 0.0174 (16) | −0.0034 (16) | −0.0086 (16) |
O6W | 0.071 (3) | 0.058 (2) | 0.103 (3) | 0.011 (2) | 0.013 (2) | 0.0302 (19) |
Geometric parameters (Å, º) top
Ni1—N2 | 1.968 (2) | C5—C6 | 1.471 (6) |
Ni1—O3W | 2.006 (2) | C7—C14 | 1.491 (4) |
Ni1—O1W | 2.088 (4) | C8—C9 | 1.480 (6) |
Ni1—O2W | 2.067 (4) | C9—C10 | 1.386 (6) |
Ni1—N3 | 2.116 (4) | C10—C11 | 1.359 (7) |
Ni1—N1 | 2.151 (4) | C10—H10 | 0.9300 |
O1W—H1WA | 0.89 (3) | C11—C12 | 1.394 (8) |
O1W—H1WB | 0.90 (3) | C11—H11 | 0.9300 |
O2W—H2WA | 0.90 (4) | C12—C13 | 1.379 (8) |
O2W—H2WB | 0.90 (4) | C12—H12 | 0.9300 |
O3W—H3WA | 0.90 (3) | C13—H13 | 0.9300 |
O3W—H3WB | 0.90 (4) | C14—C18 | 1.376 (8) |
N1—C1 | 1.343 (7) | C15—C16 | 1.376 (9) |
N1—C5 | 1.345 (5) | C15—H15 | 0.9300 |
N2—C8 | 1.311 (6) | C16—C17 | 1.354 (10) |
N2—C6 | 1.345 (6) | C16—H16 | 0.9300 |
N3—C13 | 1.327 (6) | C17—C18 | 1.372 (8) |
N3—C9 | 1.365 (5) | C17—H17 | 0.9300 |
N4—C6 | 1.321 (5) | C18—H18 | 0.9300 |
N4—C7 | 1.339 (6) | N1A—O3A | 1.207 (5) |
N5—C8 | 1.329 (5) | N1A—O1A | 1.239 (5) |
N5—C7 | 1.357 (6) | N1A—O2A | 1.243 (5) |
N6—C14 | 1.341 (7) | N1B—O2B | 1.217 (5) |
N6—C15 | 1.351 (7) | N1B—O3B | 1.233 (4) |
C1—C2 | 1.379 (8) | N1B—O1B | 1.256 (5) |
C1—H1 | 0.9300 | O4W—H4WA | 0.90 (4) |
C2—C3 | 1.355 (7) | O4W—H4WB | 0.89 (3) |
C2—H2 | 0.9300 | O5W—H5WA | 0.90 (3) |
C3—C4 | 1.406 (6) | O5W—H5WB | 0.90 (3) |
C3—H3 | 0.9300 | O6W—H6WA | 0.90 (3) |
C4—C5 | 1.374 (6) | O6W—H6WB | 0.90 (4) |
C4—H4 | 0.9300 | | |
| | | |
N2—Ni1—O3W | 179.5 (2) | C4—C5—C6 | 121.6 (4) |
N2—Ni1—O1W | 90.75 (16) | N4—C6—N2 | 122.8 (4) |
O3W—Ni1—O1W | 89.53 (17) | N4—C6—C5 | 122.7 (4) |
N2—Ni1—O2W | 91.00 (16) | N2—C6—C5 | 114.5 (4) |
O3W—Ni1—O2W | 88.71 (16) | N4—C7—N5 | 126.1 (2) |
O1W—Ni1—O2W | 177.87 (15) | N4—C7—C14 | 117.1 (5) |
N2—Ni1—N3 | 76.90 (18) | N5—C7—C14 | 116.8 (5) |
O3W—Ni1—N3 | 102.67 (18) | N2—C8—N5 | 124.3 (4) |
O1W—Ni1—N3 | 91.08 (16) | N2—C8—C9 | 113.1 (3) |
O2W—Ni1—N3 | 88.13 (14) | N5—C8—C9 | 122.6 (4) |
N2—Ni1—N1 | 77.83 (18) | N3—C9—C10 | 122.5 (5) |
O3W—Ni1—N1 | 102.60 (18) | N3—C9—C8 | 113.6 (4) |
O1W—Ni1—N1 | 89.37 (16) | C10—C9—C8 | 123.9 (4) |
O2W—Ni1—N1 | 92.19 (15) | C11—C10—C9 | 119.1 (4) |
N3—Ni1—N1 | 154.73 (8) | C11—C10—H10 | 120.5 |
Ni1—O1W—H1WA | 114 (2) | C9—C10—H10 | 120.4 |
Ni1—O1W—H1WB | 128 (2) | C10—C11—C12 | 119.1 (4) |
H1WA—O1W—H1WB | 109 (2) | C10—C11—H11 | 120.4 |
Ni1—O2W—H2WA | 111 (4) | C12—C11—H11 | 120.5 |
Ni1—O2W—H2WB | 116 (4) | C11—C12—C13 | 118.7 (5) |
H2WA—O2W—H2WB | 111 (3) | C11—C12—H12 | 120.6 |
Ni1—O3W—H3WA | 122 (2) | C13—C12—H12 | 120.7 |
Ni1—O3W—H3WB | 117 (3) | N3—C13—C12 | 123.4 (5) |
H3WA—O3W—H3WB | 112 (3) | N3—C13—H13 | 118.3 |
C1—N1—C5 | 117.6 (5) | C12—C13—H13 | 118.3 |
C1—N1—Ni1 | 129.0 (3) | N6—C14—C18 | 123.5 (3) |
C5—N1—Ni1 | 113.3 (3) | N6—C14—C7 | 115.9 (5) |
C8—N2—C6 | 118.3 (2) | C18—C14—C7 | 120.6 (5) |
C8—N2—Ni1 | 122.0 (3) | N6—C15—C16 | 122.6 (5) |
C6—N2—Ni1 | 119.6 (3) | N6—C15—H15 | 118.7 |
C13—N3—C9 | 117.3 (5) | C16—C15—H15 | 118.7 |
C13—N3—Ni1 | 128.4 (3) | C17—C16—C15 | 119.7 (3) |
C9—N3—Ni1 | 114.3 (3) | C17—C16—H16 | 120.1 |
C6—N4—C7 | 114.9 (3) | C15—C16—H16 | 120.1 |
C8—N5—C7 | 113.6 (3) | C18—C17—C16 | 119.0 (5) |
C14—N6—C15 | 116.4 (4) | C18—C17—H17 | 120.5 |
N1—C1—C2 | 122.3 (5) | C16—C17—H17 | 120.5 |
N1—C1—H1 | 118.8 | C17—C18—C14 | 118.7 (5) |
C2—C1—H1 | 118.9 | C17—C18—H18 | 120.6 |
C1—C2—C3 | 119.4 (5) | C14—C18—H18 | 120.6 |
C1—C2—H2 | 120.3 | O3A—N1A—O1A | 121.6 (5) |
C3—C2—H2 | 120.3 | O3A—N1A—O2A | 121.7 (5) |
C2—C3—C4 | 119.8 (4) | O1A—N1A—O2A | 116.7 (4) |
C2—C3—H3 | 120.0 | O2B—N1B—O3B | 121.0 (4) |
C4—C3—H3 | 120.1 | O2B—N1B—O1B | 118.7 (4) |
C5—C4—C3 | 117.0 (4) | O3B—N1B—O1B | 120.3 (4) |
C5—C4—H4 | 121.5 | H4WA—O4W—H4WB | 115 (3) |
C3—C4—H4 | 121.5 | H5WA—O5W—H5WB | 110 (3) |
N1—C5—C4 | 123.7 (4) | H6WA—O6W—H6WB | 115 (3) |
N1—C5—C6 | 114.6 (4) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O1Ai | 0.89 (3) | 1.93 (3) | 2.801 (6) | 163 (4) |
O1W—H1WB···O3Bii | 0.90 (3) | 1.94 (3) | 2.821 (5) | 165 (4) |
O2W—H2WA···O6W | 0.90 (4) | 1.86 (4) | 2.744 (5) | 170 (7) |
O2W—H2WB···O5Wiii | 0.90 (4) | 1.76 (5) | 2.647 (5) | 168 (7) |
O3W—H3WA···O4Wii | 0.90 (3) | 1.79 (3) | 2.689 (6) | 176 (4) |
O3W—H3WB···O1Biii | 0.90 (4) | 2.02 (4) | 2.842 (6) | 152 (7) |
O4W—H4WA···O1B | 0.90 (4) | 2.10 (4) | 2.957 (8) | 161 (5) |
O4W—H4WB···O3A | 0.89 (3) | 2.20 (3) | 3.062 (8) | 162 (7) |
O5W—H5WA···N6iv | 0.90 (3) | 2.01 (3) | 2.832 (6) | 152 (5) |
O5W—H5WB···O1A | 0.90 (3) | 2.12 (4) | 2.933 (6) | 150 (6) |
O6W—H6WA···O2Av | 0.90 (3) | 2.14 (3) | 2.953 (7) | 151 (4) |
O6W—H6WB···O2B | 0.90 (4) | 2.05 (4) | 2.926 (7) | 165 (7) |
Symmetry codes: (i) x+1, −y+1, z−1/2; (ii) x+1/2, −y+3/2, z−1/2; (iii) x+1/2, y+1/2, z; (iv) x−1, y, z; (v) x+1, y, z. |