In the title compound, [Ni(H
2O)
6]Cl
2·2C
6H
12N
4·4H
2O, the Ni
II atom lies on a center of inversion, and is coordinated by six O atoms from six water molecules, in a slightly distorted octahedral geometry. In the crystal structure, O, N and Cl atoms act as acceptors (
A) to form intermolecular O—H
A hydrogen bonds, giving a three-dimensional network.
Supporting information
CCDC reference: 225679
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Ni-O) = 0.002 Å
- R factor = 0.031
- wR factor = 0.089
- Data-to-parameter ratio = 11.9
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.98
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Ni1
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 49.00 A 3
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Crystal data top
[Ni(H2O)6]Cl2·2C6H12N4·4H2O | Z = 1 |
Mr = 590.14 | F(000) = 314 |
Triclinic, P1 | Dx = 1.411 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.330 (6) Å | Cell parameters from 2777 reflections |
b = 9.411 (6) Å | θ = 2.5–26.3° |
c = 9.446 (6) Å | µ = 0.95 mm−1 |
α = 119.551 (7)° | T = 293 K |
β = 94.192 (8)° | Block, blue |
γ = 100.990 (8)° | 0.46 × 0.32 × 0.18 mm |
V = 694.6 (8) Å3 | |
Data collection top
Bruker SMART-CCD area-detector diffractometer | 2418 independent reflections |
Radiation source: fine-focus sealed tube | 2216 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
φ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→11 |
Tmin = 0.670, Tmax = 0.848 | k = −10→11 |
3644 measured reflections | l = −11→10 |
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)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.089 | w = 1/[σ2(Fo2) + (0.0606P)2 + 0.0662P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
2418 reflections | Δρmax = 0.35 e Å−3 |
204 parameters | Δρmin = −0.49 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.059 (5) |
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. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.02892 (16) | |
O1 | 0.3831 (2) | 0.6342 (2) | 0.4429 (2) | 0.0450 (4) | |
H1 | 0.380 (3) | 0.723 (4) | 0.510 (4) | 0.053 (8)* | |
H2 | 0.305 (3) | 0.595 (3) | 0.369 (4) | 0.059 (8)* | |
O2 | 0.6415 (2) | 0.5275 (2) | 0.3532 (2) | 0.0520 (4) | |
H3 | 0.632 (4) | 0.579 (4) | 0.314 (4) | 0.076 (10)* | |
H4 | 0.684 (4) | 0.456 (4) | 0.288 (4) | 0.080 (10)* | |
O3 | 0.6186 (2) | 0.7235 (2) | 0.69897 (19) | 0.0515 (4) | |
H5 | 0.613 (3) | 0.746 (4) | 0.797 (4) | 0.065 (8)* | |
H6 | 0.671 (3) | 0.790 (4) | 0.699 (4) | 0.059 (9)* | |
N1 | 0.6580 (2) | 1.0478 (2) | 0.3272 (2) | 0.0379 (4) | |
N2 | 0.6660 (2) | 0.7597 (2) | 0.2449 (2) | 0.0391 (4) | |
N3 | 0.88469 (19) | 0.9576 (2) | 0.2560 (2) | 0.0402 (4) | |
N4 | 0.6640 (2) | 0.8457 (2) | 0.0398 (2) | 0.0390 (4) | |
C1 | 0.6077 (2) | 0.9045 (3) | 0.3516 (3) | 0.0411 (5) | |
H11 | 0.4998 | 0.8690 | 0.3268 | 0.041 (6)* | |
H12 | 0.6407 | 0.9410 | 0.4669 | 0.049 (6)* | |
C2 | 0.8220 (2) | 1.0986 (3) | 0.3625 (3) | 0.0435 (5) | |
H13 | 0.8582 | 1.1379 | 0.4780 | 0.055 (7)* | |
H14 | 0.8561 | 1.1918 | 0.3451 | 0.044 (6)* | |
C3 | 0.6057 (2) | 0.9880 (3) | 0.1507 (3) | 0.0403 (5) | |
H15 | 0.4977 | 0.9528 | 0.1249 | 0.041 (6)* | |
H16 | 0.6374 | 1.0805 | 0.1317 | 0.036 (5)* | |
C4 | 0.8296 (2) | 0.8163 (3) | 0.2823 (3) | 0.0433 (5) | |
H17 | 0.8691 | 0.7222 | 0.2120 | 0.048 (6)* | |
H18 | 0.8656 | 0.8519 | 0.3968 | 0.038 (6)* | |
C5 | 0.8272 (2) | 0.9006 (3) | 0.0816 (3) | 0.0435 (5) | |
H19 | 0.8614 | 0.9925 | 0.0623 | 0.046 (6)* | |
H20 | 0.8668 | 0.8075 | 0.0093 | 0.042 (6)* | |
C6 | 0.6137 (2) | 0.7066 (3) | 0.0710 (3) | 0.0410 (5) | |
H21 | 0.5057 | 0.6698 | 0.0448 | 0.045 (6)* | |
H22 | 0.6510 | 0.6113 | −0.0013 | 0.050 (6)* | |
Cl1 | 0.81052 (7) | 0.32527 (8) | 0.06497 (8) | 0.0593 (2) | |
O4 | 0.1488 (3) | 0.5523 (4) | 0.2005 (3) | 0.0813 (7) | |
H7 | 0.165 (5) | 0.585 (5) | 0.129 (6) | 0.114 (15)* | |
H8 | 0.068 (5) | 0.496 (6) | 0.174 (5) | 0.106 (16)* | |
O5 | 0.8033 (2) | 0.9976 (2) | 0.7221 (2) | 0.0518 (4) | |
H9 | 0.889 (4) | 1.002 (4) | 0.732 (4) | 0.061 (9)* | |
H10 | 0.800 (4) | 1.078 (5) | 0.812 (5) | 0.089 (12)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0391 (2) | 0.0253 (2) | 0.0249 (2) | 0.01100 (14) | 0.00910 (14) | 0.01362 (15) |
O1 | 0.0572 (10) | 0.0356 (9) | 0.0394 (8) | 0.0216 (7) | 0.0015 (7) | 0.0153 (7) |
O2 | 0.0749 (12) | 0.0528 (10) | 0.0612 (10) | 0.0366 (9) | 0.0443 (9) | 0.0426 (9) |
O3 | 0.0754 (12) | 0.0348 (9) | 0.0287 (8) | −0.0069 (8) | 0.0047 (7) | 0.0131 (7) |
N1 | 0.0456 (10) | 0.0344 (9) | 0.0338 (8) | 0.0174 (7) | 0.0070 (7) | 0.0154 (7) |
N2 | 0.0481 (10) | 0.0385 (9) | 0.0441 (9) | 0.0191 (8) | 0.0193 (8) | 0.0272 (8) |
N3 | 0.0405 (9) | 0.0386 (9) | 0.0393 (9) | 0.0119 (7) | 0.0089 (7) | 0.0180 (8) |
N4 | 0.0471 (10) | 0.0366 (9) | 0.0311 (8) | 0.0058 (7) | 0.0076 (7) | 0.0176 (7) |
C1 | 0.0472 (12) | 0.0502 (12) | 0.0377 (10) | 0.0228 (10) | 0.0187 (9) | 0.0266 (10) |
C2 | 0.0469 (12) | 0.0343 (11) | 0.0383 (10) | 0.0107 (9) | 0.0014 (9) | 0.0116 (9) |
C3 | 0.0458 (12) | 0.0390 (11) | 0.0407 (10) | 0.0100 (9) | 0.0029 (9) | 0.0251 (9) |
C4 | 0.0505 (12) | 0.0461 (12) | 0.0468 (11) | 0.0258 (10) | 0.0171 (10) | 0.0283 (10) |
C5 | 0.0529 (13) | 0.0410 (12) | 0.0389 (11) | 0.0093 (9) | 0.0180 (9) | 0.0222 (10) |
C6 | 0.0479 (12) | 0.0314 (10) | 0.0408 (10) | 0.0069 (9) | 0.0133 (9) | 0.0171 (9) |
Cl1 | 0.0655 (4) | 0.0484 (4) | 0.0601 (4) | 0.0163 (3) | 0.0287 (3) | 0.0226 (3) |
O4 | 0.0682 (15) | 0.0957 (17) | 0.0812 (15) | 0.0066 (13) | −0.0120 (12) | 0.0552 (14) |
O5 | 0.0442 (10) | 0.0488 (10) | 0.0489 (10) | 0.0023 (7) | 0.0079 (8) | 0.0191 (9) |
Geometric parameters (Å, º) top
Ni1—O3i | 2.0227 (18) | N3—C4 | 1.476 (3) |
Ni1—O3 | 2.0227 (18) | N4—C5 | 1.467 (3) |
Ni1—O1 | 2.0460 (17) | N4—C3 | 1.471 (3) |
Ni1—O1i | 2.0460 (17) | N4—C6 | 1.478 (3) |
Ni1—O2 | 2.0554 (18) | C1—H11 | 0.9700 |
Ni1—O2i | 2.0554 (18) | C1—H12 | 0.9700 |
O1—H1 | 0.77 (3) | C2—H13 | 0.9700 |
O1—H2 | 0.85 (3) | C2—H14 | 0.9700 |
O2—H3 | 0.76 (4) | C3—H15 | 0.9700 |
O2—H4 | 0.84 (4) | C3—H16 | 0.9700 |
O3—H5 | 0.85 (3) | C4—H17 | 0.9700 |
O3—H6 | 0.71 (3) | C4—H18 | 0.9700 |
N1—C2 | 1.474 (3) | C5—H19 | 0.9700 |
N1—C1 | 1.474 (3) | C5—H20 | 0.9700 |
N1—C3 | 1.479 (3) | C6—H21 | 0.9700 |
N2—C4 | 1.472 (3) | C6—H22 | 0.9700 |
N2—C6 | 1.472 (3) | O4—H7 | 0.88 (5) |
N2—C1 | 1.475 (3) | O4—H8 | 0.77 (5) |
N3—C5 | 1.476 (3) | O5—H9 | 0.79 (3) |
N3—C2 | 1.476 (3) | O5—H10 | 0.82 (4) |
| | | |
O3i—Ni1—O3 | 180.000 (1) | N1—C1—H11 | 109.2 |
O3i—Ni1—O1 | 92.61 (9) | N2—C1—H11 | 109.2 |
O3—Ni1—O1 | 87.39 (9) | N1—C1—H12 | 109.2 |
O3i—Ni1—O1i | 87.39 (9) | N2—C1—H12 | 109.2 |
O3—Ni1—O1i | 92.61 (9) | H11—C1—H12 | 107.9 |
O1—Ni1—O1i | 180.000 (1) | N1—C2—N3 | 111.96 (16) |
O3i—Ni1—O2 | 89.24 (9) | N1—C2—H13 | 109.2 |
O3—Ni1—O2 | 90.76 (9) | N3—C2—H13 | 109.2 |
O1—Ni1—O2 | 86.66 (8) | N1—C2—H14 | 109.2 |
O1i—Ni1—O2 | 93.34 (8) | N3—C2—H14 | 109.2 |
O3i—Ni1—O2i | 90.76 (9) | H13—C2—H14 | 107.9 |
O3—Ni1—O2i | 89.24 (9) | N4—C3—N1 | 111.71 (16) |
O1—Ni1—O2i | 93.34 (8) | N4—C3—H15 | 109.3 |
O1i—Ni1—O2i | 86.66 (8) | N1—C3—H15 | 109.3 |
O2—Ni1—O2i | 180.000 (1) | N4—C3—H16 | 109.3 |
Ni1—O1—H1 | 121 (2) | N1—C3—H16 | 109.3 |
Ni1—O1—H2 | 127.3 (18) | H15—C3—H16 | 107.9 |
H1—O1—H2 | 106 (3) | N2—C4—N3 | 112.02 (16) |
Ni1—O2—H3 | 121 (3) | N2—C4—H17 | 109.2 |
Ni1—O2—H4 | 127 (2) | N3—C4—H17 | 109.2 |
H3—O2—H4 | 104 (3) | N2—C4—H18 | 109.2 |
Ni1—O3—H5 | 121 (2) | N3—C4—H18 | 109.2 |
Ni1—O3—H6 | 127 (2) | H17—C4—H18 | 107.9 |
H5—O3—H6 | 112 (3) | N4—C5—N3 | 112.04 (16) |
C2—N1—C1 | 108.67 (15) | N4—C5—H19 | 109.2 |
C2—N1—C3 | 108.16 (17) | N3—C5—H19 | 109.2 |
C1—N1—C3 | 107.79 (16) | N4—C5—H20 | 109.2 |
C4—N2—C6 | 108.33 (16) | N3—C5—H20 | 109.2 |
C4—N2—C1 | 108.53 (17) | H19—C5—H20 | 107.9 |
C6—N2—C1 | 108.04 (16) | N2—C6—N4 | 111.60 (16) |
C5—N3—C2 | 107.84 (17) | N2—C6—H21 | 109.3 |
C5—N3—C4 | 108.05 (16) | N4—C6—H21 | 109.3 |
C2—N3—C4 | 108.34 (17) | N2—C6—H22 | 109.3 |
C5—N4—C3 | 108.55 (16) | N4—C6—H22 | 109.3 |
C5—N4—C6 | 108.52 (16) | H21—C6—H22 | 108.0 |
C3—N4—C6 | 108.11 (17) | H7—O4—H8 | 109 (4) |
N1—C1—N2 | 111.89 (16) | H9—O5—H10 | 102 (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 |
O1—H1···N1ii | 0.77 (3) | 2.06 (3) | 2.823 (3) | 172 (3) |
O1—H2···O4 | 0.85 (3) | 1.90 (3) | 2.739 (3) | 166 (3) |
O2—H3···N2 | 0.76 (4) | 2.08 (4) | 2.814 (3) | 164 (3) |
O2—H4···Cl1 | 0.84 (4) | 2.39 (4) | 3.191 (2) | 158 (3) |
O3—H5···N4iii | 0.85 (3) | 1.98 (3) | 2.799 (3) | 161 (3) |
O3—H6···O5 | 0.71 (3) | 2.00 (3) | 2.714 (3) | 172 (3) |
O4—H7···Cl1iv | 0.88 (5) | 2.37 (5) | 3.253 (3) | 176 (4) |
O4—H8···Cl1v | 0.77 (5) | 2.44 (5) | 3.210 (3) | 173 (4) |
O5—H9···N3vi | 0.79 (3) | 2.05 (3) | 2.838 (3) | 170 (3) |
O5—H10···Cl1vii | 0.82 (4) | 2.35 (4) | 3.168 (3) | 174 (3) |
Symmetry codes: (ii) −x+1, −y+2, −z+1; (iii) x, y, z+1; (iv) −x+1, −y+1, −z; (v) x−1, y, z; (vi) −x+2, −y+2, −z+1; (vii) x, y+1, z+1. |