The title complex, [Ni(C4H6N2)6]Cl2·2H2O, is a mononuclear complex in which the NiII ion, lying on a centre of inversion, is coordinated by six 1-methylimidazole ligands that define an octahedral geometry.
Supporting information
CCDC reference: 601258
Key indicators
- Single-crystal X-ray study
- T = 290 K
- Mean (C-C) = 0.006 Å
- R factor = 0.043
- wR factor = 0.115
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
| Author Response: The diffractive ability of crystal isn't strong enough, though its
quality is good. The software used to data collection was DIFRAC and the
range of 2\q was 2\% to 50\%. When the number of reflections reached to
2860, the CAD4 device automatically stopped collecting. After data reduction
by NRCVAX, we found that the independent reflections number was 2714, which
was less than the theoretic one.
|
PLAT093_ALERT_1_A No su's on H-atoms, but refinement reported as . mixed
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3
N1 -NI1 -N1 -C1 14.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8
N1 -NI1 -N1 -C3 4.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 15
N3 -NI1 -N3 -C7 12.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 20
N3 -NI1 -N3 -C5 7.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 21
N5 -NI1 -N5 -C11 17.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 26
N5 -NI1 -N5 -C9 1.00 0.00 3.555 1.555 1.555 1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 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
7 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: DIFRAC (Gabe & White, 1993); cell refinement: DIFRAC; data reduction: NRCVAX (Gabe et al., 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and
Mercury (Version 1.2; Bruno et al., 2002); software used to prepare material for publication: SHELXL97.
Hexakis(1-methyl-1
H-imidazole-
κN3)nickel(II) dichloride
dihydrate
top
Crystal data top
[Ni(C4H6N2)6]Cl2·2H2O | F(000) = 692 |
Mr = 658.29 | Dx = 1.376 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 27 reflections |
a = 8.065 (4) Å | θ = 4.5–7.4° |
b = 13.238 (5) Å | µ = 0.82 mm−1 |
c = 15.029 (7) Å | T = 290 K |
β = 98.07 (4)° | Block, blue |
V = 1588.7 (12) Å3 | 0.25 × 0.25 × 0.23 mm |
Z = 2 | |
Data collection top
Enraf–Nonius CAD-4 diffractometer | Rint = 0.012 |
Radiation source: fine-focus sealed tube | θmax = 25.0°, θmin = 2.7° |
Graphite monochromator | h = −8→9 |
ω/2θ scans | k = 0→15 |
2860 measured reflections | l = −9→17 |
2714 independent reflections | 3 standard reflections every 300 reflections |
1829 reflections with I > 2σ(I) | intensity decay: 1.0% |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.115 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.061P)2 + 0.0104P] where P = (Fo2 + 2Fc2)/3 |
2714 reflections | (Δ/σ)max < 0.001 |
194 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.39 e Å−3 |
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 | 0 | 0 | 0.03065 (19) | |
Cl1 | 0.20308 (14) | 0.37906 (7) | −0.06939 (7) | 0.0555 (3) | |
OW | 0.0189 (5) | 0.4199 (2) | 0.1014 (2) | 0.0815 (11) | |
N1 | 0.1827 (3) | 0.0812 (2) | 0.08774 (19) | 0.0366 (7) | |
N2 | 0.3137 (4) | 0.2023 (2) | 0.1700 (2) | 0.0434 (8) | |
N3 | 0.1692 (3) | −0.12726 (19) | 0.01010 (19) | 0.0339 (7) | |
N4 | 0.2915 (4) | −0.2749 (2) | 0.0430 (2) | 0.0450 (8) | |
N5 | 0.1068 (3) | 0.0450 (2) | −0.11445 (18) | 0.0333 (6) | |
N6 | 0.2633 (4) | 0.1215 (2) | −0.2030 (2) | 0.0401 (7) | |
C1 | 0.1907 (5) | 0.1787 (3) | 0.1044 (2) | 0.0407 (9) | |
H1 | 0.1186 | 0.2260 | 0.0739 | 0.046 (3)* | |
C2 | 0.3881 (5) | 0.1143 (3) | 0.1989 (3) | 0.0527 (10) | |
H2 | 0.4769 | 0.1063 | 0.2450 | 0.046 (3)* | |
C3 | 0.3088 (5) | 0.0412 (3) | 0.1483 (3) | 0.0496 (10) | |
H3 | 0.3354 | −0.0271 | 0.1534 | 0.046 (3)* | |
C4 | 0.3621 (6) | 0.3043 (3) | 0.2011 (3) | 0.0754 (15) | |
H4A | 0.4508 | 0.3282 | 0.1701 | 0.133 (7)* | |
H4B | 0.3998 | 0.3029 | 0.2645 | 0.133 (7)* | |
H4C | 0.2674 | 0.3486 | 0.1889 | 0.133 (7)* | |
C5 | 0.3221 (5) | −0.1296 (3) | −0.0204 (3) | 0.0460 (10) | |
H5 | 0.3667 | −0.0768 | −0.0503 | 0.046 (3)* | |
C6 | 0.3988 (5) | −0.2193 (3) | −0.0009 (3) | 0.0513 (10) | |
H6 | 0.5030 | −0.2392 | −0.0145 | 0.046 (3)* | |
C7 | 0.1568 (5) | −0.2170 (2) | 0.0473 (3) | 0.0415 (9) | |
H7 | 0.0645 | −0.2376 | 0.0735 | 0.046 (3)* | |
C8 | 0.3183 (6) | −0.3794 (3) | 0.0752 (4) | 0.0745 (15) | |
H8A | 0.3925 | −0.3795 | 0.1311 | 0.133 (7)* | |
H8B | 0.3669 | −0.4183 | 0.0316 | 0.133 (7)* | |
H8C | 0.2129 | −0.4087 | 0.0841 | 0.133 (7)* | |
C9 | 0.1046 (5) | −0.0086 (3) | −0.1926 (2) | 0.0420 (9) | |
H9 | 0.0454 | −0.0683 | −0.2061 | 0.046 (3)* | |
C10 | 0.2005 (5) | 0.0373 (3) | −0.2472 (3) | 0.0442 (9) | |
H10 | 0.2198 | 0.0157 | −0.3037 | 0.046 (3)* | |
C11 | 0.2040 (4) | 0.1232 (2) | −0.1243 (2) | 0.0386 (8) | |
H11 | 0.2284 | 0.1737 | −0.0814 | 0.046 (3)* | |
C12 | 0.3670 (6) | 0.2000 (3) | −0.2368 (3) | 0.0684 (14) | |
H12A | 0.3368 | 0.2649 | −0.2155 | 0.133 (7)* | |
H12B | 0.3491 | 0.1996 | −0.3013 | 0.133 (7)* | |
H12C | 0.4829 | 0.1869 | −0.2158 | 0.133 (7)* | |
H1W | 0.0546 | 0.4117 | 0.0466 | 0.130 (17)* | |
H2W | −0.0254 | 0.4814 | 0.1021 | 0.130 (17)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0325 (4) | 0.0270 (3) | 0.0322 (3) | −0.0018 (3) | 0.0038 (2) | 0.0000 (3) |
Cl1 | 0.0628 (7) | 0.0383 (5) | 0.0706 (7) | 0.0038 (5) | 0.0272 (6) | 0.0055 (5) |
OW | 0.109 (3) | 0.0667 (19) | 0.076 (2) | 0.0220 (19) | 0.038 (2) | 0.0245 (17) |
N1 | 0.0379 (18) | 0.0336 (15) | 0.0377 (18) | −0.0050 (13) | 0.0030 (14) | −0.0029 (13) |
N2 | 0.0410 (19) | 0.0460 (17) | 0.0410 (19) | −0.0110 (14) | −0.0020 (15) | −0.0066 (15) |
N3 | 0.0303 (17) | 0.0324 (14) | 0.0380 (18) | 0.0016 (12) | 0.0016 (13) | 0.0001 (13) |
N4 | 0.0419 (19) | 0.0367 (15) | 0.056 (2) | 0.0027 (14) | 0.0045 (16) | −0.0002 (14) |
N5 | 0.0372 (17) | 0.0299 (13) | 0.0335 (17) | 0.0027 (13) | 0.0081 (13) | −0.0012 (12) |
N6 | 0.0433 (19) | 0.0391 (16) | 0.0403 (18) | 0.0012 (14) | 0.0143 (15) | −0.0013 (14) |
C1 | 0.042 (2) | 0.041 (2) | 0.037 (2) | −0.0065 (17) | −0.0014 (17) | 0.0002 (17) |
C2 | 0.043 (2) | 0.063 (3) | 0.047 (2) | 0.003 (2) | −0.0146 (19) | −0.001 (2) |
C3 | 0.047 (2) | 0.0427 (19) | 0.055 (3) | 0.0056 (19) | −0.008 (2) | 0.006 (2) |
C4 | 0.085 (4) | 0.059 (3) | 0.074 (3) | −0.025 (3) | −0.014 (3) | −0.025 (2) |
C5 | 0.041 (2) | 0.045 (2) | 0.053 (3) | 0.0001 (18) | 0.0116 (19) | 0.0067 (18) |
C6 | 0.035 (2) | 0.058 (2) | 0.063 (3) | 0.0082 (19) | 0.015 (2) | 0.001 (2) |
C7 | 0.033 (2) | 0.0397 (19) | 0.052 (2) | −0.0004 (16) | 0.0055 (17) | −0.0008 (18) |
C8 | 0.063 (3) | 0.041 (2) | 0.117 (4) | 0.006 (2) | 0.005 (3) | 0.018 (3) |
C9 | 0.050 (2) | 0.0336 (18) | 0.042 (2) | 0.0014 (17) | 0.0069 (17) | −0.0050 (17) |
C10 | 0.050 (2) | 0.047 (2) | 0.038 (2) | 0.0080 (18) | 0.0113 (18) | −0.0071 (17) |
C11 | 0.041 (2) | 0.0370 (18) | 0.039 (2) | −0.0020 (17) | 0.0105 (17) | −0.0032 (16) |
C12 | 0.077 (3) | 0.066 (3) | 0.071 (3) | −0.023 (2) | 0.045 (3) | −0.004 (2) |
Geometric parameters (Å, º) top
Ni1—N1 | 2.126 (3) | N6—C12 | 1.469 (4) |
Ni1—N3 | 2.160 (3) | C1—H1 | 0.9300 |
Ni1—N5 | 2.115 (3) | C2—C3 | 1.337 (5) |
Ni1—N5i | 2.115 (3) | C2—H2 | 0.9300 |
Ni1—N1i | 2.126 (3) | C3—H3 | 0.9300 |
Ni1—N3i | 2.160 (3) | C4—H4A | 0.9600 |
OW—H1W | 0.9165 | C4—H4B | 0.9600 |
OW—H2W | 0.8895 | C4—H4C | 0.9600 |
N1—C1 | 1.314 (4) | C5—C6 | 1.351 (5) |
N1—C3 | 1.373 (4) | C5—H5 | 0.9300 |
N2—C1 | 1.334 (4) | C6—H6 | 0.9300 |
N2—C2 | 1.353 (5) | C7—H7 | 0.9300 |
N2—C4 | 1.463 (4) | C8—H8A | 0.9600 |
N3—C7 | 1.323 (4) | C8—H8B | 0.9600 |
N3—C5 | 1.375 (4) | C8—H8C | 0.9600 |
N4—C7 | 1.339 (4) | C9—C10 | 1.349 (5) |
N4—C6 | 1.374 (5) | C9—H9 | 0.9300 |
N4—C8 | 1.472 (4) | C10—H10 | 0.9300 |
N5—C11 | 1.319 (4) | C11—H11 | 0.9300 |
N5—C9 | 1.371 (4) | C12—H12A | 0.9600 |
N6—C11 | 1.336 (4) | C12—H12B | 0.9600 |
N6—C10 | 1.359 (4) | C12—H12C | 0.9600 |
| | | |
N1—Ni1—N3 | 88.57 (11) | C2—C3—N1 | 110.4 (3) |
N1—Ni1—N3i | 91.43 (11) | C2—C3—H3 | 124.8 |
N5—Ni1—N1 | 92.07 (11) | N1—C3—H3 | 124.8 |
N5—Ni1—N1i | 87.93 (11) | N2—C4—H4A | 109.5 |
N5—Ni1—N3 | 87.23 (10) | N2—C4—H4B | 109.5 |
N5—Ni1—N3i | 92.77 (10) | H4A—C4—H4B | 109.5 |
N5i—Ni1—N1 | 87.93 (11) | N2—C4—H4C | 109.5 |
N5i—Ni1—N1i | 92.07 (11) | H4A—C4—H4C | 109.5 |
N1—Ni1—N1i | 180.0 | H4B—C4—H4C | 109.5 |
N5i—Ni1—N3i | 87.23 (10) | C6—C5—N3 | 110.7 (3) |
N1i—Ni1—N3i | 88.57 (11) | C6—C5—H5 | 124.7 |
N5i—Ni1—N3 | 92.77 (10) | N3—C5—H5 | 124.7 |
N1i—Ni1—N3 | 91.43 (11) | C5—C6—N4 | 106.0 (3) |
N5—Ni1—N5i | 180.0 | C5—C6—H6 | 127.0 |
N3i—Ni1—N3 | 180.0 | N4—C6—H6 | 127.0 |
H1W—OW—H2W | 107.3 | N3—C7—N4 | 112.6 (3) |
C1—N1—C3 | 103.9 (3) | N3—C7—H7 | 123.7 |
C1—N1—Ni1 | 128.8 (3) | N4—C7—H7 | 123.7 |
C3—N1—Ni1 | 126.9 (2) | N4—C8—H8A | 109.5 |
C1—N2—C2 | 106.6 (3) | N4—C8—H8B | 109.5 |
C1—N2—C4 | 126.1 (3) | H8A—C8—H8B | 109.5 |
C2—N2—C4 | 127.2 (3) | N4—C8—H8C | 109.5 |
C7—N3—C5 | 104.2 (3) | H8A—C8—H8C | 109.5 |
C7—N3—Ni1 | 130.2 (2) | H8B—C8—H8C | 109.5 |
C5—N3—Ni1 | 125.6 (2) | C10—C9—N5 | 110.4 (3) |
C7—N4—C6 | 106.6 (3) | C10—C9—H9 | 124.8 |
C7—N4—C8 | 127.2 (3) | N5—C9—H9 | 124.8 |
C6—N4—C8 | 126.1 (3) | C9—C10—N6 | 106.1 (3) |
C11—N5—C9 | 104.3 (3) | C9—C10—H10 | 126.9 |
C11—N5—Ni1 | 129.0 (2) | N6—C10—H10 | 126.9 |
C9—N5—Ni1 | 126.4 (2) | N5—C11—N6 | 112.2 (3) |
C11—N6—C10 | 106.9 (3) | N5—C11—H11 | 123.9 |
C11—N6—C12 | 125.9 (3) | N6—C11—H11 | 123.9 |
C10—N6—C12 | 127.0 (3) | N6—C12—H12A | 109.5 |
N1—C1—N2 | 112.5 (3) | N6—C12—H12B | 109.5 |
N1—C1—H1 | 123.8 | H12A—C12—H12B | 109.5 |
N2—C1—H1 | 123.8 | N6—C12—H12C | 109.5 |
C3—C2—N2 | 106.6 (3) | H12A—C12—H12C | 109.5 |
C3—C2—H2 | 126.7 | H12B—C12—H12C | 109.5 |
N2—C2—H2 | 126.7 | | |
| | | |
N5—Ni1—N1—C1 | 78.2 (3) | N3—Ni1—N5—C9 | 61.5 (3) |
N5i—Ni1—N1—C1 | −101.8 (3) | C3—N1—C1—N2 | 0.8 (4) |
N1i—Ni1—N1—C1 | −135 (45) | Ni1—N1—C1—N2 | 173.7 (2) |
N3i—Ni1—N1—C1 | −14.6 (3) | C2—N2—C1—N1 | −1.3 (4) |
N3—Ni1—N1—C1 | 165.4 (3) | C4—N2—C1—N1 | 176.2 (4) |
N5—Ni1—N1—C3 | −110.4 (3) | C1—N2—C2—C3 | 1.2 (4) |
N5i—Ni1—N1—C3 | 69.6 (3) | C4—N2—C2—C3 | −176.3 (4) |
N1i—Ni1—N1—C3 | 36 (100) | N2—C2—C3—N1 | −0.7 (5) |
N3i—Ni1—N1—C3 | 156.8 (3) | C1—N1—C3—C2 | 0.0 (4) |
N3—Ni1—N1—C3 | −23.2 (3) | Ni1—N1—C3—C2 | −173.1 (3) |
N5—Ni1—N3—C7 | −155.1 (3) | C7—N3—C5—C6 | −0.4 (4) |
N5i—Ni1—N3—C7 | 24.9 (3) | Ni1—N3—C5—C6 | 177.9 (3) |
N1—Ni1—N3—C7 | 112.8 (3) | N3—C5—C6—N4 | 0.0 (5) |
N1i—Ni1—N3—C7 | −67.2 (3) | C7—N4—C6—C5 | 0.4 (4) |
N3i—Ni1—N3—C7 | −117 (100) | C8—N4—C6—C5 | 178.0 (4) |
N5—Ni1—N3—C5 | 27.1 (3) | C5—N3—C7—N4 | 0.6 (4) |
N5i—Ni1—N3—C5 | −152.9 (3) | Ni1—N3—C7—N4 | −177.6 (2) |
N1—Ni1—N3—C5 | −65.0 (3) | C6—N4—C7—N3 | −0.6 (4) |
N1i—Ni1—N3—C5 | 115.0 (3) | C8—N4—C7—N3 | −178.2 (4) |
N3i—Ni1—N3—C5 | 65 (100) | C11—N5—C9—C10 | 0.4 (4) |
N5i—Ni1—N5—C11 | −166 (100) | Ni1—N5—C9—C10 | −173.1 (2) |
N1—Ni1—N5—C11 | −21.9 (3) | N5—C9—C10—N6 | −0.3 (4) |
N1i—Ni1—N5—C11 | 158.1 (3) | C11—N6—C10—C9 | 0.1 (4) |
N3i—Ni1—N5—C11 | 69.6 (3) | C12—N6—C10—C9 | −176.0 (4) |
N3—Ni1—N5—C11 | −110.4 (3) | C9—N5—C11—N6 | −0.4 (4) |
N5i—Ni1—N5—C9 | 6 (100) | Ni1—N5—C11—N6 | 172.9 (2) |
N1—Ni1—N5—C9 | 150.0 (3) | C10—N6—C11—N5 | 0.2 (4) |
N1i—Ni1—N5—C9 | −30.0 (3) | C12—N6—C11—N5 | 176.4 (3) |
N3i—Ni1—N5—C9 | −118.5 (3) | | |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—H1W···Cl1 | 0.92 | 2.29 | 3.187 (3) | 166 |
OW—H2W···Cl1ii | 0.89 | 2.35 | 3.205 (3) | 162 |
Symmetry code: (ii) −x, −y+1, −z. |