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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102002834/bk1640sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102002834/bk1640Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102002834/bk1640IIsup3.hkl
Contains datablock II

CCDC references: 184462; 184463

Computing details top

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·CH4OF(000) = 1520
Mr = 723.42Dx = 1.410 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.803 (1) ÅCell parameters from 16736 reflections
b = 25.951 (2) Åθ = 1.6–28.1°
c = 12.310 (1) ŵ = 0.63 mm1
β = 115.31 (1)°T = 298 K
V = 3408.4 (4) Å3Plates, pale violet
Z = 40.40 × 0.30 × 0.12 mm
Data collection top
CCD area detector
diffractometer
7275 independent reflections
Radiation source: fine-focus sealed tube4648 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
φ and ω scansθmax = 27.0°, θmin = 1.6°
Absorption correction: empirical (using intensity measurements) from intensities
SADABS in SAINT-NT (Bruker, 2000)
h = 1414
Tmin = 0.84, Tmax = 0.93k = 3132
16404 measured reflectionsl = 1115
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.056Hydrogen site location: geom+difmap
wR(F2) = 0.163H 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 parametersΔρmax = 0.70 e Å3
10 restraintsΔρmin = 0.52 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.34455 (4)0.891896 (14)0.22967 (4)0.04620 (16)
O1W0.5272 (3)0.89432 (11)0.2410 (3)0.0654 (7)
H1WA0.588 (4)0.9050 (19)0.298 (4)0.15 (2)*
H1WB0.556 (4)0.8683 (14)0.221 (4)0.108 (18)*
O2W0.3704 (3)0.96657 (10)0.2986 (3)0.0651 (7)
H2WA0.326 (3)0.974 (2)0.331 (4)0.13 (2)*
H2WB0.442 (2)0.9693 (14)0.343 (3)0.056 (13)*
N1A0.2736 (2)0.92184 (10)0.0589 (2)0.0483 (6)
N2A0.1559 (3)0.89823 (9)0.1926 (3)0.0492 (6)
C1A0.3339 (3)0.93302 (13)0.0076 (3)0.0593 (9)
H1A0.42050.92920.02750.071*
C2A0.2770 (4)0.95008 (14)0.1260 (3)0.0648 (10)
C3A0.1486 (4)0.95613 (13)0.1805 (3)0.0620 (9)
C4A0.0810 (3)0.94589 (11)0.1109 (3)0.0520 (8)
C5A0.0513 (3)0.95371 (12)0.1522 (3)0.0589 (9)
H5A0.09760.96630.22940.071*
C6A0.1100 (3)0.94340 (12)0.0829 (3)0.0590 (9)
H6A0.19570.94940.11320.071*
C7A0.0459 (3)0.92360 (11)0.0355 (3)0.0516 (8)
C8A0.1045 (3)0.90950 (13)0.1104 (4)0.0609 (9)
C9A0.0316 (4)0.89113 (14)0.2240 (4)0.0675 (10)
C10A0.0989 (4)0.88634 (12)0.2614 (3)0.0596 (9)
H10A0.14750.87420.33860.072*
C11A0.0841 (3)0.91630 (11)0.0805 (3)0.0463 (7)
C12A0.1472 (3)0.92866 (11)0.0072 (3)0.0460 (7)
C13A0.3603 (4)0.9605 (2)0.1885 (4)0.0936 (14)
H13A0.33280.94010.26030.140*
H13B0.44520.95180.13590.140*
H13C0.35560.99640.20920.140*
C14A0.0822 (4)0.97219 (18)0.3091 (4)0.0892 (14)
H14A0.13980.98990.33250.134*
H14B0.01410.99480.31870.134*
H14C0.05020.94230.35870.134*
C15A0.2441 (4)0.91467 (18)0.0668 (5)0.0887 (14)
H15A0.27560.93920.00240.133*
H15B0.26240.92620.13160.133*
H15C0.28310.88190.03860.133*
C16A0.0845 (5)0.8739 (2)0.3113 (5)0.0967 (15)
H16A0.13270.90140.32280.145*
H16B0.01680.86510.38700.145*
H16C0.13720.84440.27930.145*
N1B0.4086 (2)0.85478 (9)0.3941 (2)0.0504 (7)
N2B0.3270 (2)0.81590 (10)0.1745 (2)0.0499 (6)
C1B0.4566 (3)0.87434 (13)0.5047 (3)0.0558 (9)
H1B0.45790.91000.51230.067*
C2B0.5054 (3)0.84504 (14)0.6103 (3)0.0617 (9)
C3B0.5026 (4)0.79205 (14)0.6020 (3)0.0645 (10)
C4B0.4560 (3)0.77028 (13)0.4860 (3)0.0595 (9)
C5B0.4535 (4)0.71559 (14)0.4645 (4)0.0750 (12)
H5B0.47980.69300.52930.090*
C6B0.4144 (4)0.69670 (14)0.3534 (4)0.0803 (13)
H6B0.41630.66120.34380.096*
C7B0.3700 (3)0.72834 (12)0.2494 (3)0.0600 (9)
C8B0.3272 (4)0.71017 (14)0.1299 (4)0.0682 (10)
C9B0.2840 (4)0.74465 (15)0.0373 (4)0.0694 (10)
C10B0.2853 (3)0.79697 (14)0.0647 (3)0.0587 (9)
H10B0.25460.82010.00100.070*
C11B0.3681 (3)0.78172 (11)0.2666 (3)0.0488 (8)
C12B0.4113 (3)0.80223 (12)0.3855 (3)0.0499 (8)
C13B0.5609 (4)0.87319 (17)0.7291 (3)0.0854 (13)
H13D0.55520.90970.71490.128*
H13E0.64730.86360.77270.128*
H13F0.51560.86420.77510.128*
C14B0.5463 (5)0.75900 (18)0.7131 (4)0.0926 (14)
H14D0.59520.77950.78240.139*
H14E0.59670.73120.70640.139*
H14F0.47500.74520.72150.139*
C15B0.3306 (5)0.65298 (15)0.1046 (5)0.1036 (17)
H15D0.27370.64590.02280.155*
H15E0.30630.63350.15750.155*
H15F0.41400.64340.11760.155*
C16B0.2341 (5)0.73004 (18)0.0939 (4)0.0963 (15)
H16D0.30220.71940.11160.144*
H16E0.19300.75920.14270.144*
H16F0.17530.70230.11060.144*
N1C0.7013 (3)0.98115 (13)0.4829 (3)0.0645 (8)
O1C0.7260 (3)0.94835 (12)0.4254 (3)0.0927 (9)
O2C0.5966 (3)1.00031 (16)0.4404 (4)0.1426 (17)
O3C0.7730 (3)1.00221 (18)0.5705 (3)0.1498 (19)
N1D0.4405 (5)0.1931 (2)0.9591 (5)0.1074 (14)
O1D0.3995 (3)0.18804 (15)0.8538 (3)0.1099 (11)
O2D0.5117 (4)0.16122 (19)1.0266 (4)0.1329 (14)
O3D0.4273 (9)0.2314 (3)1.0060 (5)0.286 (5)
O1X0.6846 (10)0.6840 (4)0.0233 (11)0.140 (3)*0.401 (8)
C1X0.716 (2)0.6730 (10)0.138 (2)0.140 (3)*0.401 (8)
O1Y0.6240 (16)0.6798 (6)0.1494 (16)0.140 (3)*0.294 (9)
C1Y0.742 (2)0.6734 (11)0.217 (2)0.140 (3)*0.294 (9)
O1Z0.674 (4)0.6672 (15)0.104 (4)0.140 (3)*0.151 (9)
C1Z0.764 (4)0.6970 (19)0.175 (5)0.140 (3)*0.151 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0555 (3)0.0376 (2)0.0446 (3)0.00071 (18)0.0205 (2)0.00038 (17)
O1W0.0573 (15)0.0677 (17)0.0687 (19)0.0022 (14)0.0244 (14)0.0111 (14)
O2W0.077 (2)0.0460 (13)0.0694 (18)0.0021 (14)0.0279 (18)0.0074 (13)
N1A0.0518 (16)0.0452 (14)0.0505 (16)0.0048 (12)0.0243 (13)0.0077 (12)
N2A0.0584 (17)0.0411 (14)0.0531 (17)0.0050 (12)0.0287 (14)0.0044 (12)
C1A0.062 (2)0.058 (2)0.065 (2)0.0080 (17)0.0331 (19)0.0100 (18)
C2A0.078 (3)0.061 (2)0.068 (2)0.0178 (19)0.043 (2)0.0196 (18)
C3A0.081 (3)0.0519 (19)0.054 (2)0.0080 (18)0.030 (2)0.0077 (17)
C4A0.065 (2)0.0367 (16)0.051 (2)0.0065 (15)0.0215 (17)0.0018 (14)
C5A0.063 (2)0.0420 (18)0.059 (2)0.0017 (16)0.0133 (19)0.0003 (16)
C6A0.052 (2)0.0461 (18)0.070 (2)0.0021 (15)0.0179 (19)0.0077 (17)
C7A0.054 (2)0.0343 (15)0.066 (2)0.0057 (14)0.0256 (17)0.0117 (15)
C8A0.061 (2)0.0470 (18)0.080 (3)0.0062 (16)0.035 (2)0.0105 (18)
C9A0.076 (3)0.059 (2)0.085 (3)0.0131 (19)0.052 (2)0.012 (2)
C10A0.075 (2)0.0523 (19)0.057 (2)0.0051 (17)0.0333 (19)0.0011 (16)
C11A0.0542 (19)0.0329 (15)0.0516 (19)0.0033 (13)0.0225 (16)0.0060 (14)
C12A0.058 (2)0.0339 (15)0.0469 (18)0.0032 (14)0.0232 (16)0.0006 (13)
C13A0.103 (3)0.115 (4)0.082 (3)0.022 (3)0.057 (3)0.032 (3)
C14A0.101 (3)0.097 (3)0.066 (3)0.014 (3)0.032 (2)0.026 (2)
C15A0.061 (2)0.094 (3)0.117 (4)0.008 (2)0.043 (3)0.007 (3)
C16A0.100 (3)0.116 (4)0.100 (4)0.012 (3)0.068 (3)0.003 (3)
N1B0.0637 (17)0.0380 (13)0.0485 (16)0.0039 (12)0.0231 (14)0.0020 (12)
N2B0.0583 (17)0.0458 (14)0.0469 (16)0.0029 (12)0.0237 (13)0.0069 (12)
C1B0.070 (2)0.0463 (17)0.048 (2)0.0058 (16)0.0224 (18)0.0030 (15)
C2B0.071 (2)0.064 (2)0.049 (2)0.0124 (18)0.0232 (18)0.0019 (17)
C3B0.082 (3)0.064 (2)0.052 (2)0.020 (2)0.033 (2)0.0127 (18)
C4B0.076 (2)0.0482 (19)0.060 (2)0.0121 (17)0.034 (2)0.0089 (16)
C5B0.114 (3)0.0422 (19)0.078 (3)0.011 (2)0.050 (3)0.0146 (19)
C6B0.123 (4)0.0338 (18)0.092 (3)0.004 (2)0.053 (3)0.0027 (19)
C7B0.079 (2)0.0390 (17)0.067 (2)0.0026 (16)0.036 (2)0.0078 (16)
C8B0.088 (3)0.0451 (19)0.081 (3)0.0068 (19)0.045 (2)0.0161 (19)
C9B0.082 (3)0.065 (2)0.067 (3)0.005 (2)0.036 (2)0.022 (2)
C10B0.069 (2)0.058 (2)0.049 (2)0.0024 (17)0.0248 (18)0.0080 (16)
C11B0.059 (2)0.0389 (16)0.0535 (19)0.0014 (14)0.0285 (16)0.0029 (14)
C12B0.064 (2)0.0387 (16)0.0504 (19)0.0030 (14)0.0271 (17)0.0001 (14)
C13B0.111 (4)0.087 (3)0.046 (2)0.015 (3)0.022 (2)0.005 (2)
C14B0.128 (4)0.091 (3)0.062 (3)0.037 (3)0.044 (3)0.031 (2)
C15B0.154 (5)0.054 (2)0.110 (4)0.009 (3)0.063 (3)0.033 (2)
C16B0.125 (4)0.092 (3)0.070 (3)0.001 (3)0.040 (3)0.035 (3)
N1C0.061 (2)0.070 (2)0.0529 (19)0.0087 (17)0.0159 (17)0.0011 (16)
O1C0.103 (2)0.082 (2)0.089 (2)0.0252 (17)0.0369 (18)0.0079 (17)
O2C0.075 (2)0.164 (4)0.172 (4)0.012 (2)0.036 (2)0.098 (3)
O3C0.087 (2)0.208 (5)0.099 (3)0.030 (3)0.012 (2)0.070 (3)
N1D0.145 (4)0.116 (4)0.083 (3)0.024 (3)0.069 (3)0.012 (3)
O1D0.134 (3)0.128 (3)0.070 (2)0.010 (2)0.046 (2)0.004 (2)
O2D0.131 (3)0.153 (4)0.120 (3)0.016 (3)0.060 (3)0.032 (3)
O3D0.478 (12)0.248 (7)0.155 (5)0.185 (8)0.158 (6)0.016 (5)
Geometric parameters (Å, º) top
Ni1—N1A2.054 (3)N1B—C1B1.330 (4)
Ni1—N2B2.067 (3)N1B—C12B1.369 (4)
Ni1—N1B2.071 (3)N2B—C10B1.320 (4)
Ni1—N2A2.079 (3)N2B—C11B1.355 (4)
Ni1—O2W2.085 (3)C1B—C2B1.400 (5)
Ni1—O1W2.100 (3)C1B—H1B0.9300
O1W—H1WA0.81 (3)C2B—C3B1.378 (5)
O1W—H1WB0.84 (3)C2B—C13B1.511 (5)
O2W—H2WA0.80 (3)C3B—C4B1.411 (5)
O2W—H2WB0.79 (2)C3B—C14B1.507 (5)
N1A—C1A1.326 (4)C4B—C12B1.392 (4)
N1A—C12A1.360 (4)C4B—C5B1.442 (5)
N2A—C10A1.323 (4)C5B—C6B1.335 (5)
N2A—C11A1.357 (4)C5B—H5B0.9300
C1A—C2A1.390 (5)C6B—C7B1.419 (5)
C1A—H1A0.9300C6B—H6B0.9300
C2A—C3A1.379 (5)C7B—C11B1.403 (4)
C2A—C13A1.510 (5)C7B—C8B1.417 (5)
C3A—C4A1.424 (5)C8B—C9B1.365 (5)
C3A—C14A1.494 (5)C8B—C15B1.520 (5)
C4A—C12A1.397 (4)C9B—C10B1.398 (5)
C4A—C5A1.435 (5)C9B—C16B1.511 (5)
C5A—C6A1.335 (5)C10B—H10B0.9300
C5A—H5A0.9300C11B—C12B1.431 (4)
C6A—C7A1.421 (5)C13B—H13D0.9600
C6A—H6A0.9300C13B—H13E0.9600
C7A—C11A1.404 (4)C13B—H13F0.9600
C7A—C8A1.416 (5)C14B—H14D0.9600
C8A—C9A1.376 (5)C14B—H14E0.9600
C8A—C15A1.505 (5)C14B—H14F0.9600
C9A—C10A1.413 (5)C15B—H15D0.9600
C9A—C16A1.522 (6)C15B—H15E0.9600
C10A—H10A0.9300C15B—H15F0.9600
C11A—C12A1.431 (4)C16B—H16D0.9600
C13A—H13A0.9600C16B—H16E0.9600
C13A—H13B0.9600C16B—H16F0.9600
C13A—H13C0.9600N1C—O3C1.182 (4)
C14A—H14A0.9600N1C—O1C1.220 (4)
C14A—H14B0.9600N1C—O2C1.223 (4)
C14A—H14C0.9600N1D—O1D1.180 (5)
C15A—H15A0.9600N1D—O3D1.194 (6)
C15A—H15B0.9600N1D—O2D1.218 (5)
C15A—H15C0.9600O1X—C1X1.32 (2)
C16A—H16A0.9600O1Y—C1Y1.30 (2)
C16A—H16B0.9600O1Z—C1Z1.30 (2)
C16A—H16C0.9600
N1A—Ni1—N2B94.88 (10)H15B—C15A—H15C109.5
N1A—Ni1—N1B174.33 (10)C9A—C16A—H16A109.5
N2B—Ni1—N1B79.67 (10)C9A—C16A—H16B109.5
N1A—Ni1—N2A79.39 (11)H16A—C16A—H16B109.5
N2B—Ni1—N2A93.21 (10)C9A—C16A—H16C109.5
N1B—Ni1—N2A99.21 (11)H16A—C16A—H16C109.5
N1A—Ni1—O2W89.41 (11)H16B—C16A—H16C109.5
N2B—Ni1—O2W175.63 (11)C1B—N1B—C12B116.4 (3)
N1B—Ni1—O2W96.06 (10)C1B—N1B—Ni1129.8 (2)
N2A—Ni1—O2W88.41 (12)C12B—N1B—Ni1113.5 (2)
N1A—Ni1—O1W90.83 (11)C10B—N2B—C11B117.2 (3)
N2B—Ni1—O1W90.36 (11)C10B—N2B—Ni1129.2 (2)
N1B—Ni1—O1W90.78 (11)C11B—N2B—Ni1113.6 (2)
N2A—Ni1—O1W169.84 (11)N1B—C1B—C2B124.7 (3)
O2W—Ni1—O1W88.72 (13)N1B—C1B—H1B117.7
Ni1—O1W—H1WA125 (4)C2B—C1B—H1B117.7
Ni1—O1W—H1WB119 (3)C3B—C2B—C1B119.1 (3)
H1WA—O1W—H1WB102 (3)C3B—C2B—C13B122.7 (4)
Ni1—O2W—H2WA114 (4)C1B—C2B—C13B118.2 (3)
Ni1—O2W—H2WB107 (3)C2B—C3B—C4B117.5 (3)
H2WA—O2W—H2WB112 (3)C2B—C3B—C14B120.9 (4)
C1A—N1A—C12A117.0 (3)C4B—C3B—C14B121.7 (3)
C1A—N1A—Ni1128.5 (2)C12B—C4B—C3B119.8 (3)
C12A—N1A—Ni1114.4 (2)C12B—C4B—C5B116.9 (3)
C10A—N2A—C11A117.6 (3)C3B—C4B—C5B123.3 (3)
C10A—N2A—Ni1129.1 (3)C6B—C5B—C4B121.4 (4)
C11A—N2A—Ni1113.3 (2)C6B—C5B—H5B119.3
N1A—C1A—C2A124.8 (3)C4B—C5B—H5B119.3
N1A—C1A—H1A117.6C5B—C6B—C7B122.9 (3)
C2A—C1A—H1A117.6C5B—C6B—H6B118.5
C3A—C2A—C1A119.0 (3)C7B—C6B—H6B118.5
C3A—C2A—C13A123.4 (4)C11B—C7B—C8B117.6 (3)
C1A—C2A—C13A117.6 (4)C11B—C7B—C6B117.3 (3)
C2A—C3A—C4A117.9 (3)C8B—C7B—C6B125.1 (3)
C2A—C3A—C14A121.2 (4)C9B—C8B—C7B119.3 (3)
C4A—C3A—C14A121.0 (4)C9B—C8B—C15B120.2 (4)
C12A—C4A—C3A118.5 (3)C7B—C8B—C15B120.6 (4)
C12A—C4A—C5A117.0 (3)C8B—C9B—C10B118.3 (3)
C3A—C4A—C5A124.4 (3)C8B—C9B—C16B124.3 (4)
C6A—C5A—C4A121.9 (3)C10B—C9B—C16B117.4 (4)
C6A—C5A—H5A119.1N2B—C10B—C9B124.7 (4)
C4A—C5A—H5A119.1N2B—C10B—H10B117.6
C5A—C6A—C7A122.3 (3)C9B—C10B—H10B117.6
C5A—C6A—H6A118.9N2B—C11B—C7B122.9 (3)
C7A—C6A—H6A118.9N2B—C11B—C12B117.1 (3)
C11A—C7A—C8A117.6 (3)C7B—C11B—C12B120.0 (3)
C11A—C7A—C6A117.8 (3)N1B—C12B—C4B122.5 (3)
C8A—C7A—C6A124.6 (3)N1B—C12B—C11B116.1 (3)
C9A—C8A—C7A119.0 (3)C4B—C12B—C11B121.4 (3)
C9A—C8A—C15A120.4 (4)C2B—C13B—H13D109.5
C7A—C8A—C15A120.6 (4)C2B—C13B—H13E109.5
C8A—C9A—C10A118.8 (4)H13D—C13B—H13E109.5
C8A—C9A—C16A123.6 (4)C2B—C13B—H13F109.5
C10A—C9A—C16A117.6 (4)H13D—C13B—H13F109.5
N2A—C10A—C9A123.6 (4)H13E—C13B—H13F109.5
N2A—C10A—H10A118.2C3B—C14B—H14D109.5
C9A—C10A—H10A118.2C3B—C14B—H14E109.5
N2A—C11A—C7A123.4 (3)H14D—C14B—H14E109.5
N2A—C11A—C12A116.9 (3)C3B—C14B—H14F109.5
C7A—C11A—C12A119.8 (3)H14D—C14B—H14F109.5
N1A—C12A—C4A122.9 (3)H14E—C14B—H14F109.5
N1A—C12A—C11A116.0 (3)C8B—C15B—H15D109.5
C4A—C12A—C11A121.1 (3)C8B—C15B—H15E109.5
C2A—C13A—H13A109.5H15D—C15B—H15E109.5
C2A—C13A—H13B109.5C8B—C15B—H15F109.5
H13A—C13A—H13B109.5H15D—C15B—H15F109.5
C2A—C13A—H13C109.5H15E—C15B—H15F109.5
H13A—C13A—H13C109.5C9B—C16B—H16D109.5
H13B—C13A—H13C109.5C9B—C16B—H16E109.5
C3A—C14A—H14A109.5H16D—C16B—H16E109.5
C3A—C14A—H14B109.5C9B—C16B—H16F109.5
H14A—C14A—H14B109.5H16D—C16B—H16F109.5
C3A—C14A—H14C109.5H16E—C16B—H16F109.5
H14A—C14A—H14C109.5O3C—N1C—O1C126.6 (4)
H14B—C14A—H14C109.5O3C—N1C—O2C113.6 (4)
C8A—C15A—H15A109.5O1C—N1C—O2C119.0 (4)
C8A—C15A—H15B109.5O1D—N1D—O3D123.1 (6)
H15A—C15A—H15B109.5O1D—N1D—O2D120.9 (5)
C8A—C15A—H15C109.5O3D—N1D—O2D115.5 (6)
H15A—C15A—H15C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O1C0.81 (3)2.05 (3)2.842 (5)166 (7)
O1W—H1WB···O1Di0.84 (3)1.92 (3)2.746 (5)169 (5)
O2W—H2WA···O3Cii0.79 (3)2.12 (3)2.907 (6)173 (5)
O2W—H2WB···O2C0.79 (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)2·3H2OF(000) = 1248
Mr = 603.16Dx = 1.574 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
a = 12.328 (2) ÅCell parameters from 7432 reflections
b = 14.851 (3) Åθ = 2.2–28.1°
c = 14.124 (3) ŵ = 0.84 mm1
β = 100.06 (3)°T = 298 K
V = 2546.0 (8) Å3Blocks, green
Z = 40.38 × 0.26 × 0.18 mm
Data collection top
Bruker CCD area-detector
diffractometer
3955 independent reflections
Radiation source: fine-focus sealed tube3550 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
φ and ω scansθmax = 27.0°, θmin = 2.2°
Absorption correction: empirical (using intensity measurements) from intensities
SADABS in SAINT_NT (Bruker, 2000)
h = 815
Tmin = 0.76, Tmax = 0.83k = 1818
7312 measured reflectionsl = 1717
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H 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 reflectionsΔρmax = 0.54 e Å3
402 parametersΔρmin = 0.30 e Å3
21 restraintsAbsolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methodsAbsolute 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
xyzUiso*/Ueq
Ni10.21167 (7)0.77296 (2)0.25179 (6)0.03233 (11)
O1W0.2663 (4)0.7798 (2)0.1201 (3)0.0470 (9)
H1WA0.290 (3)0.7272 (11)0.101 (2)0.023 (9)*
H1WB0.304 (3)0.8249 (15)0.098 (3)0.045 (13)*
O2W0.1609 (3)0.77046 (19)0.3837 (2)0.0412 (8)
H2WA0.157 (6)0.7139 (18)0.405 (5)0.13 (3)*
H2WB0.100 (3)0.802 (3)0.388 (4)0.083 (19)*
O3W0.2097 (4)0.90789 (13)0.2570 (3)0.0542 (7)
H3WA0.184 (3)0.942 (2)0.2053 (16)0.035 (10)*
H3WB0.197 (6)0.933 (3)0.3119 (16)0.15 (3)*
N10.0489 (4)0.7416 (2)0.1766 (3)0.0341 (9)
N20.2145 (4)0.64052 (14)0.2478 (3)0.0317 (5)
N30.3724 (4)0.7415 (2)0.3239 (3)0.0325 (9)
N40.1179 (3)0.5064 (2)0.2071 (3)0.0355 (8)
N50.3054 (3)0.5047 (2)0.2901 (3)0.0368 (9)
N60.2949 (3)0.3236 (2)0.3018 (3)0.0387 (9)
C10.0314 (5)0.7979 (3)0.1365 (4)0.0387 (11)
H10.02120.85950.14570.046*
C20.1284 (5)0.7676 (3)0.0822 (4)0.0390 (13)
H20.18110.80830.05310.047*
C30.1461 (4)0.6778 (3)0.0716 (3)0.0412 (11)
H30.21180.65670.03600.049*
C40.0650 (4)0.6168 (3)0.1144 (3)0.0398 (11)
H40.07580.55480.10930.048*
C50.0310 (4)0.6527 (3)0.1642 (3)0.0335 (10)
C60.1235 (4)0.5952 (3)0.2077 (3)0.0340 (10)
C70.2106 (5)0.46443 (17)0.2474 (4)0.0334 (6)
C80.3008 (4)0.5941 (3)0.2880 (3)0.0300 (9)
C90.3936 (4)0.6514 (3)0.3335 (3)0.0322 (10)
C100.4923 (4)0.6181 (3)0.3832 (3)0.0397 (11)
H100.50450.55630.38820.048*
C110.5712 (4)0.6768 (3)0.4244 (3)0.0443 (12)
H110.63770.65580.45860.053*
C120.5509 (5)0.7690 (3)0.4149 (4)0.0408 (13)
H120.60370.81050.44230.049*
C130.4511 (4)0.7975 (3)0.3639 (4)0.0370 (11)
H130.43840.85910.35720.044*
C140.2097 (5)0.36407 (18)0.2460 (4)0.0355 (6)
C150.2943 (6)0.2327 (3)0.3020 (4)0.0501 (15)
H150.35180.20240.34050.060*
C160.2121 (7)0.1830 (2)0.2474 (5)0.0535 (9)
H160.21490.12040.24900.064*
C170.1271 (6)0.2256 (3)0.1913 (4)0.0539 (17)
H170.07110.19270.15420.065*
C180.1251 (5)0.3179 (4)0.1901 (4)0.0490 (13)
H180.06760.34880.15230.059*
N1A0.6697 (3)0.4419 (2)0.5525 (3)0.0501 (9)
O1A0.6169 (4)0.3723 (3)0.5772 (3)0.0806 (11)
O2A0.7716 (4)0.4345 (3)0.5326 (3)0.0874 (12)
O3A0.6241 (4)0.5130 (2)0.5455 (3)0.0950 (13)
N1B0.1623 (3)0.5408 (2)0.4476 (2)0.0501 (8)
O1B0.2548 (3)0.5029 (2)0.4344 (3)0.0695 (10)
O2B0.1015 (3)0.5280 (2)0.3897 (3)0.0725 (9)
O3B0.1340 (3)0.5896 (2)0.5182 (2)0.0737 (10)
O4W0.3732 (4)0.4967 (2)0.5991 (3)0.0691 (9)
H4WA0.329 (3)0.509 (3)0.557 (3)0.051 (15)*
H4WB0.4447 (15)0.492 (5)0.574 (4)0.13 (3)*
O5W0.5015 (3)0.3779 (2)0.4124 (3)0.0635 (8)
H5WA0.567 (2)0.381 (3)0.373 (3)0.068 (15)*
H5WB0.512 (5)0.369 (6)0.4735 (17)0.19 (4)*
O6W0.1224 (4)0.5990 (2)0.4423 (3)0.0773 (11)
H6WA0.166 (2)0.5504 (16)0.451 (3)0.020 (9)*
H6WB0.0500 (13)0.588 (3)0.426 (7)0.15 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0324 (2)0.02447 (16)0.03680 (18)0.0023 (3)0.00307 (14)0.0006 (3)
O1W0.057 (2)0.0383 (18)0.0468 (19)0.0002 (15)0.0118 (18)0.0039 (13)
O2W0.041 (2)0.0420 (19)0.0382 (17)0.0066 (14)0.0003 (15)0.0019 (12)
O3W0.0827 (18)0.0259 (9)0.0449 (14)0.001 (2)0.0140 (13)0.0014 (18)
N10.031 (2)0.0291 (18)0.038 (2)0.0017 (19)0.0033 (18)0.0004 (17)
N20.0308 (12)0.0254 (9)0.0356 (11)0.002 (2)0.0030 (9)0.004 (2)
N30.030 (2)0.0295 (18)0.036 (2)0.0026 (19)0.0008 (18)0.0001 (17)
N40.031 (2)0.0294 (18)0.0424 (19)0.0031 (17)0.0049 (16)0.0054 (15)
N50.044 (2)0.0255 (17)0.0390 (17)0.0015 (18)0.0022 (17)0.0021 (15)
N60.046 (2)0.0250 (17)0.045 (2)0.0009 (17)0.0049 (18)0.0018 (15)
C10.037 (3)0.036 (2)0.041 (3)0.007 (2)0.000 (2)0.006 (2)
C20.031 (3)0.039 (3)0.043 (3)0.006 (2)0.006 (2)0.0073 (18)
C30.026 (3)0.050 (3)0.041 (2)0.003 (2)0.011 (2)0.002 (2)
C40.029 (3)0.040 (2)0.043 (3)0.001 (2)0.0119 (19)0.0031 (19)
C50.035 (3)0.028 (2)0.033 (2)0.0064 (19)0.0057 (19)0.0023 (17)
C60.039 (3)0.032 (2)0.028 (2)0.001 (2)0.0026 (19)0.0017 (17)
C70.0370 (15)0.0273 (11)0.0343 (13)0.004 (3)0.0014 (11)0.002 (2)
C80.025 (2)0.028 (2)0.036 (2)0.0011 (19)0.0030 (18)0.0000 (18)
C90.031 (2)0.034 (2)0.032 (2)0.0053 (19)0.0045 (19)0.0010 (18)
C100.042 (3)0.033 (2)0.042 (3)0.004 (2)0.003 (2)0.0030 (18)
C110.041 (3)0.048 (3)0.042 (2)0.008 (2)0.002 (2)0.003 (2)
C120.034 (3)0.050 (3)0.038 (3)0.010 (2)0.004 (2)0.0062 (19)
C130.035 (3)0.033 (2)0.041 (3)0.001 (2)0.002 (2)0.001 (2)
C140.0396 (16)0.0294 (12)0.0373 (16)0.005 (3)0.0058 (13)0.008 (2)
C150.066 (4)0.032 (3)0.055 (3)0.013 (2)0.018 (3)0.006 (2)
C160.074 (2)0.0284 (13)0.063 (2)0.012 (4)0.0236 (19)0.014 (3)
C170.063 (4)0.036 (3)0.062 (4)0.005 (2)0.007 (3)0.010 (2)
C180.053 (3)0.040 (2)0.052 (3)0.010 (2)0.003 (2)0.006 (2)
N1A0.057 (3)0.0408 (18)0.0537 (19)0.0020 (18)0.0139 (18)0.0008 (15)
O1A0.073 (3)0.077 (2)0.094 (3)0.019 (2)0.021 (2)0.0273 (19)
O2A0.061 (3)0.095 (3)0.106 (3)0.011 (2)0.015 (2)0.005 (2)
O3A0.134 (4)0.0559 (19)0.095 (3)0.036 (2)0.020 (3)0.0024 (18)
N1B0.059 (2)0.0331 (15)0.0541 (19)0.0130 (17)0.0011 (18)0.0006 (14)
O1B0.068 (2)0.0593 (19)0.076 (2)0.0071 (18)0.0007 (19)0.0014 (17)
O2B0.076 (2)0.068 (2)0.077 (2)0.0053 (19)0.0211 (19)0.0126 (17)
O3B0.082 (2)0.0614 (17)0.071 (2)0.0062 (18)0.0064 (18)0.0286 (16)
O4W0.081 (3)0.0565 (19)0.0599 (19)0.006 (2)0.014 (2)0.0062 (16)
O5W0.0490 (19)0.0659 (19)0.071 (2)0.0174 (16)0.0034 (16)0.0086 (16)
O6W0.071 (3)0.058 (2)0.103 (3)0.011 (2)0.013 (2)0.0302 (19)
Geometric parameters (Å, º) top
Ni1—N21.968 (2)C5—C61.471 (6)
Ni1—O3W2.006 (2)C7—C141.491 (4)
Ni1—O1W2.088 (4)C8—C91.480 (6)
Ni1—O2W2.067 (4)C9—C101.386 (6)
Ni1—N32.116 (4)C10—C111.359 (7)
Ni1—N12.151 (4)C10—H100.9300
O1W—H1WA0.89 (3)C11—C121.394 (8)
O1W—H1WB0.90 (3)C11—H110.9300
O2W—H2WA0.90 (4)C12—C131.379 (8)
O2W—H2WB0.90 (4)C12—H120.9300
O3W—H3WA0.90 (3)C13—H130.9300
O3W—H3WB0.90 (4)C14—C181.376 (8)
N1—C11.343 (7)C15—C161.376 (9)
N1—C51.345 (5)C15—H150.9300
N2—C81.311 (6)C16—C171.354 (10)
N2—C61.345 (6)C16—H160.9300
N3—C131.327 (6)C17—C181.372 (8)
N3—C91.365 (5)C17—H170.9300
N4—C61.321 (5)C18—H180.9300
N4—C71.339 (6)N1A—O3A1.207 (5)
N5—C81.329 (5)N1A—O1A1.239 (5)
N5—C71.357 (6)N1A—O2A1.243 (5)
N6—C141.341 (7)N1B—O2B1.217 (5)
N6—C151.351 (7)N1B—O3B1.233 (4)
C1—C21.379 (8)N1B—O1B1.256 (5)
C1—H10.9300O4W—H4WA0.90 (4)
C2—C31.355 (7)O4W—H4WB0.89 (3)
C2—H20.9300O5W—H5WA0.90 (3)
C3—C41.406 (6)O5W—H5WB0.90 (3)
C3—H30.9300O6W—H6WA0.90 (3)
C4—C51.374 (6)O6W—H6WB0.90 (4)
C4—H40.9300
N2—Ni1—O3W179.5 (2)C4—C5—C6121.6 (4)
N2—Ni1—O1W90.75 (16)N4—C6—N2122.8 (4)
O3W—Ni1—O1W89.53 (17)N4—C6—C5122.7 (4)
N2—Ni1—O2W91.00 (16)N2—C6—C5114.5 (4)
O3W—Ni1—O2W88.71 (16)N4—C7—N5126.1 (2)
O1W—Ni1—O2W177.87 (15)N4—C7—C14117.1 (5)
N2—Ni1—N376.90 (18)N5—C7—C14116.8 (5)
O3W—Ni1—N3102.67 (18)N2—C8—N5124.3 (4)
O1W—Ni1—N391.08 (16)N2—C8—C9113.1 (3)
O2W—Ni1—N388.13 (14)N5—C8—C9122.6 (4)
N2—Ni1—N177.83 (18)N3—C9—C10122.5 (5)
O3W—Ni1—N1102.60 (18)N3—C9—C8113.6 (4)
O1W—Ni1—N189.37 (16)C10—C9—C8123.9 (4)
O2W—Ni1—N192.19 (15)C11—C10—C9119.1 (4)
N3—Ni1—N1154.73 (8)C11—C10—H10120.5
Ni1—O1W—H1WA114 (2)C9—C10—H10120.4
Ni1—O1W—H1WB128 (2)C10—C11—C12119.1 (4)
H1WA—O1W—H1WB109 (2)C10—C11—H11120.4
Ni1—O2W—H2WA111 (4)C12—C11—H11120.5
Ni1—O2W—H2WB116 (4)C11—C12—C13118.7 (5)
H2WA—O2W—H2WB111 (3)C11—C12—H12120.6
Ni1—O3W—H3WA122 (2)C13—C12—H12120.7
Ni1—O3W—H3WB117 (3)N3—C13—C12123.4 (5)
H3WA—O3W—H3WB112 (3)N3—C13—H13118.3
C1—N1—C5117.6 (5)C12—C13—H13118.3
C1—N1—Ni1129.0 (3)N6—C14—C18123.5 (3)
C5—N1—Ni1113.3 (3)N6—C14—C7115.9 (5)
C8—N2—C6118.3 (2)C18—C14—C7120.6 (5)
C8—N2—Ni1122.0 (3)N6—C15—C16122.6 (5)
C6—N2—Ni1119.6 (3)N6—C15—H15118.7
C13—N3—C9117.3 (5)C16—C15—H15118.7
C13—N3—Ni1128.4 (3)C17—C16—C15119.7 (3)
C9—N3—Ni1114.3 (3)C17—C16—H16120.1
C6—N4—C7114.9 (3)C15—C16—H16120.1
C8—N5—C7113.6 (3)C18—C17—C16119.0 (5)
C14—N6—C15116.4 (4)C18—C17—H17120.5
N1—C1—C2122.3 (5)C16—C17—H17120.5
N1—C1—H1118.8C17—C18—C14118.7 (5)
C2—C1—H1118.9C17—C18—H18120.6
C1—C2—C3119.4 (5)C14—C18—H18120.6
C1—C2—H2120.3O3A—N1A—O1A121.6 (5)
C3—C2—H2120.3O3A—N1A—O2A121.7 (5)
C2—C3—C4119.8 (4)O1A—N1A—O2A116.7 (4)
C2—C3—H3120.0O2B—N1B—O3B121.0 (4)
C4—C3—H3120.1O2B—N1B—O1B118.7 (4)
C5—C4—C3117.0 (4)O3B—N1B—O1B120.3 (4)
C5—C4—H4121.5H4WA—O4W—H4WB115 (3)
C3—C4—H4121.5H5WA—O5W—H5WB110 (3)
N1—C5—C4123.7 (4)H6WA—O6W—H6WB115 (3)
N1—C5—C6114.6 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O1Ai0.89 (3)1.93 (3)2.801 (6)163 (4)
O1W—H1WB···O3Bii0.90 (3)1.94 (3)2.821 (5)165 (4)
O2W—H2WA···O6W0.90 (4)1.86 (4)2.744 (5)170 (7)
O2W—H2WB···O5Wiii0.90 (4)1.76 (5)2.647 (5)168 (7)
O3W—H3WA···O4Wii0.90 (3)1.79 (3)2.689 (6)176 (4)
O3W—H3WB···O1Biii0.90 (4)2.02 (4)2.842 (6)152 (7)
O4W—H4WA···O1B0.90 (4)2.10 (4)2.957 (8)161 (5)
O4W—H4WB···O3A0.89 (3)2.20 (3)3.062 (8)162 (7)
O5W—H5WA···N6iv0.90 (3)2.01 (3)2.832 (6)152 (5)
O5W—H5WB···O1A0.90 (3)2.12 (4)2.933 (6)150 (6)
O6W—H6WA···O2Av0.90 (3)2.14 (3)2.953 (7)151 (4)
O6W—H6WB···O2B0.90 (4)2.05 (4)2.926 (7)165 (7)
Symmetry codes: (i) x+1, y+1, z1/2; (ii) x+1/2, y+3/2, z1/2; (iii) x+1/2, y+1/2, z; (iv) x1, y, z; (v) x+1, y, z.
 

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