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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806003746/tk6306sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806003746/tk6306Isup2.hkl
Contains datablock I

CCDC reference: 601258

Key indicators

  • Single-crystal X-ray study
  • T = 290 K
  • Mean [sigma](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

Computing details top

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-1H-imidazole-κN3)nickel(II) dichloride dihydrate top
Crystal data top
[Ni(C4H6N2)6]Cl2·2H2OF(000) = 692
Mr = 658.29Dx = 1.376 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 27 reflections
a = 8.065 (4) Åθ = 4.5–7.4°
b = 13.238 (5) ŵ = 0.82 mm1
c = 15.029 (7) ÅT = 290 K
β = 98.07 (4)°Block, blue
V = 1588.7 (12) Å30.25 × 0.25 × 0.23 mm
Z = 2
Data collection top
Enraf–Nonius CAD-4
diffractometer
Rint = 0.012
Radiation source: fine-focus sealed tubeθmax = 25.0°, θmin = 2.7°
Graphite monochromatorh = 89
ω/2θ scansk = 015
2860 measured reflectionsl = 917
2714 independent reflections3 standard reflections every 300 reflections
1829 reflections with I > 2σ(I) intensity decay: 1.0%
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H 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 parametersΔρmax = 0.35 e Å3
0 restraintsΔρmin = 0.39 e Å3
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
xyzUiso*/Ueq
Ni10000.03065 (19)
Cl10.20308 (14)0.37906 (7)0.06939 (7)0.0555 (3)
OW0.0189 (5)0.4199 (2)0.1014 (2)0.0815 (11)
N10.1827 (3)0.0812 (2)0.08774 (19)0.0366 (7)
N20.3137 (4)0.2023 (2)0.1700 (2)0.0434 (8)
N30.1692 (3)0.12726 (19)0.01010 (19)0.0339 (7)
N40.2915 (4)0.2749 (2)0.0430 (2)0.0450 (8)
N50.1068 (3)0.0450 (2)0.11445 (18)0.0333 (6)
N60.2633 (4)0.1215 (2)0.2030 (2)0.0401 (7)
C10.1907 (5)0.1787 (3)0.1044 (2)0.0407 (9)
H10.11860.22600.07390.046 (3)*
C20.3881 (5)0.1143 (3)0.1989 (3)0.0527 (10)
H20.47690.10630.24500.046 (3)*
C30.3088 (5)0.0412 (3)0.1483 (3)0.0496 (10)
H30.33540.02710.15340.046 (3)*
C40.3621 (6)0.3043 (3)0.2011 (3)0.0754 (15)
H4A0.45080.32820.17010.133 (7)*
H4B0.39980.30290.26450.133 (7)*
H4C0.26740.34860.18890.133 (7)*
C50.3221 (5)0.1296 (3)0.0204 (3)0.0460 (10)
H50.36670.07680.05030.046 (3)*
C60.3988 (5)0.2193 (3)0.0009 (3)0.0513 (10)
H60.50300.23920.01450.046 (3)*
C70.1568 (5)0.2170 (2)0.0473 (3)0.0415 (9)
H70.06450.23760.07350.046 (3)*
C80.3183 (6)0.3794 (3)0.0752 (4)0.0745 (15)
H8A0.39250.37950.13110.133 (7)*
H8B0.36690.41830.03160.133 (7)*
H8C0.21290.40870.08410.133 (7)*
C90.1046 (5)0.0086 (3)0.1926 (2)0.0420 (9)
H90.04540.06830.20610.046 (3)*
C100.2005 (5)0.0373 (3)0.2472 (3)0.0442 (9)
H100.21980.01570.30370.046 (3)*
C110.2040 (4)0.1232 (2)0.1243 (2)0.0386 (8)
H110.22840.17370.08140.046 (3)*
C120.3670 (6)0.2000 (3)0.2368 (3)0.0684 (14)
H12A0.33680.26490.21550.133 (7)*
H12B0.34910.19960.30130.133 (7)*
H12C0.48290.18690.21580.133 (7)*
H1W0.05460.41170.04660.130 (17)*
H2W0.02540.48140.10210.130 (17)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0325 (4)0.0270 (3)0.0322 (3)0.0018 (3)0.0038 (2)0.0000 (3)
Cl10.0628 (7)0.0383 (5)0.0706 (7)0.0038 (5)0.0272 (6)0.0055 (5)
OW0.109 (3)0.0667 (19)0.076 (2)0.0220 (19)0.038 (2)0.0245 (17)
N10.0379 (18)0.0336 (15)0.0377 (18)0.0050 (13)0.0030 (14)0.0029 (13)
N20.0410 (19)0.0460 (17)0.0410 (19)0.0110 (14)0.0020 (15)0.0066 (15)
N30.0303 (17)0.0324 (14)0.0380 (18)0.0016 (12)0.0016 (13)0.0001 (13)
N40.0419 (19)0.0367 (15)0.056 (2)0.0027 (14)0.0045 (16)0.0002 (14)
N50.0372 (17)0.0299 (13)0.0335 (17)0.0027 (13)0.0081 (13)0.0012 (12)
N60.0433 (19)0.0391 (16)0.0403 (18)0.0012 (14)0.0143 (15)0.0013 (14)
C10.042 (2)0.041 (2)0.037 (2)0.0065 (17)0.0014 (17)0.0002 (17)
C20.043 (2)0.063 (3)0.047 (2)0.003 (2)0.0146 (19)0.001 (2)
C30.047 (2)0.0427 (19)0.055 (3)0.0056 (19)0.008 (2)0.006 (2)
C40.085 (4)0.059 (3)0.074 (3)0.025 (3)0.014 (3)0.025 (2)
C50.041 (2)0.045 (2)0.053 (3)0.0001 (18)0.0116 (19)0.0067 (18)
C60.035 (2)0.058 (2)0.063 (3)0.0082 (19)0.015 (2)0.001 (2)
C70.033 (2)0.0397 (19)0.052 (2)0.0004 (16)0.0055 (17)0.0008 (18)
C80.063 (3)0.041 (2)0.117 (4)0.006 (2)0.005 (3)0.018 (3)
C90.050 (2)0.0336 (18)0.042 (2)0.0014 (17)0.0069 (17)0.0050 (17)
C100.050 (2)0.047 (2)0.038 (2)0.0080 (18)0.0113 (18)0.0071 (17)
C110.041 (2)0.0370 (18)0.039 (2)0.0020 (17)0.0105 (17)0.0032 (16)
C120.077 (3)0.066 (3)0.071 (3)0.023 (2)0.045 (3)0.004 (2)
Geometric parameters (Å, º) top
Ni1—N12.126 (3)N6—C121.469 (4)
Ni1—N32.160 (3)C1—H10.9300
Ni1—N52.115 (3)C2—C31.337 (5)
Ni1—N5i2.115 (3)C2—H20.9300
Ni1—N1i2.126 (3)C3—H30.9300
Ni1—N3i2.160 (3)C4—H4A0.9600
OW—H1W0.9165C4—H4B0.9600
OW—H2W0.8895C4—H4C0.9600
N1—C11.314 (4)C5—C61.351 (5)
N1—C31.373 (4)C5—H50.9300
N2—C11.334 (4)C6—H60.9300
N2—C21.353 (5)C7—H70.9300
N2—C41.463 (4)C8—H8A0.9600
N3—C71.323 (4)C8—H8B0.9600
N3—C51.375 (4)C8—H8C0.9600
N4—C71.339 (4)C9—C101.349 (5)
N4—C61.374 (5)C9—H90.9300
N4—C81.472 (4)C10—H100.9300
N5—C111.319 (4)C11—H110.9300
N5—C91.371 (4)C12—H12A0.9600
N6—C111.336 (4)C12—H12B0.9600
N6—C101.359 (4)C12—H12C0.9600
N1—Ni1—N388.57 (11)C2—C3—N1110.4 (3)
N1—Ni1—N3i91.43 (11)C2—C3—H3124.8
N5—Ni1—N192.07 (11)N1—C3—H3124.8
N5—Ni1—N1i87.93 (11)N2—C4—H4A109.5
N5—Ni1—N387.23 (10)N2—C4—H4B109.5
N5—Ni1—N3i92.77 (10)H4A—C4—H4B109.5
N5i—Ni1—N187.93 (11)N2—C4—H4C109.5
N5i—Ni1—N1i92.07 (11)H4A—C4—H4C109.5
N1—Ni1—N1i180.0H4B—C4—H4C109.5
N5i—Ni1—N3i87.23 (10)C6—C5—N3110.7 (3)
N1i—Ni1—N3i88.57 (11)C6—C5—H5124.7
N5i—Ni1—N392.77 (10)N3—C5—H5124.7
N1i—Ni1—N391.43 (11)C5—C6—N4106.0 (3)
N5—Ni1—N5i180.0C5—C6—H6127.0
N3i—Ni1—N3180.0N4—C6—H6127.0
H1W—OW—H2W107.3N3—C7—N4112.6 (3)
C1—N1—C3103.9 (3)N3—C7—H7123.7
C1—N1—Ni1128.8 (3)N4—C7—H7123.7
C3—N1—Ni1126.9 (2)N4—C8—H8A109.5
C1—N2—C2106.6 (3)N4—C8—H8B109.5
C1—N2—C4126.1 (3)H8A—C8—H8B109.5
C2—N2—C4127.2 (3)N4—C8—H8C109.5
C7—N3—C5104.2 (3)H8A—C8—H8C109.5
C7—N3—Ni1130.2 (2)H8B—C8—H8C109.5
C5—N3—Ni1125.6 (2)C10—C9—N5110.4 (3)
C7—N4—C6106.6 (3)C10—C9—H9124.8
C7—N4—C8127.2 (3)N5—C9—H9124.8
C6—N4—C8126.1 (3)C9—C10—N6106.1 (3)
C11—N5—C9104.3 (3)C9—C10—H10126.9
C11—N5—Ni1129.0 (2)N6—C10—H10126.9
C9—N5—Ni1126.4 (2)N5—C11—N6112.2 (3)
C11—N6—C10106.9 (3)N5—C11—H11123.9
C11—N6—C12125.9 (3)N6—C11—H11123.9
C10—N6—C12127.0 (3)N6—C12—H12A109.5
N1—C1—N2112.5 (3)N6—C12—H12B109.5
N1—C1—H1123.8H12A—C12—H12B109.5
N2—C1—H1123.8N6—C12—H12C109.5
C3—C2—N2106.6 (3)H12A—C12—H12C109.5
C3—C2—H2126.7H12B—C12—H12C109.5
N2—C2—H2126.7
N5—Ni1—N1—C178.2 (3)N3—Ni1—N5—C961.5 (3)
N5i—Ni1—N1—C1101.8 (3)C3—N1—C1—N20.8 (4)
N1i—Ni1—N1—C1135 (45)Ni1—N1—C1—N2173.7 (2)
N3i—Ni1—N1—C114.6 (3)C2—N2—C1—N11.3 (4)
N3—Ni1—N1—C1165.4 (3)C4—N2—C1—N1176.2 (4)
N5—Ni1—N1—C3110.4 (3)C1—N2—C2—C31.2 (4)
N5i—Ni1—N1—C369.6 (3)C4—N2—C2—C3176.3 (4)
N1i—Ni1—N1—C336 (100)N2—C2—C3—N10.7 (5)
N3i—Ni1—N1—C3156.8 (3)C1—N1—C3—C20.0 (4)
N3—Ni1—N1—C323.2 (3)Ni1—N1—C3—C2173.1 (3)
N5—Ni1—N3—C7155.1 (3)C7—N3—C5—C60.4 (4)
N5i—Ni1—N3—C724.9 (3)Ni1—N3—C5—C6177.9 (3)
N1—Ni1—N3—C7112.8 (3)N3—C5—C6—N40.0 (5)
N1i—Ni1—N3—C767.2 (3)C7—N4—C6—C50.4 (4)
N3i—Ni1—N3—C7117 (100)C8—N4—C6—C5178.0 (4)
N5—Ni1—N3—C527.1 (3)C5—N3—C7—N40.6 (4)
N5i—Ni1—N3—C5152.9 (3)Ni1—N3—C7—N4177.6 (2)
N1—Ni1—N3—C565.0 (3)C6—N4—C7—N30.6 (4)
N1i—Ni1—N3—C5115.0 (3)C8—N4—C7—N3178.2 (4)
N3i—Ni1—N3—C565 (100)C11—N5—C9—C100.4 (4)
N5i—Ni1—N5—C11166 (100)Ni1—N5—C9—C10173.1 (2)
N1—Ni1—N5—C1121.9 (3)N5—C9—C10—N60.3 (4)
N1i—Ni1—N5—C11158.1 (3)C11—N6—C10—C90.1 (4)
N3i—Ni1—N5—C1169.6 (3)C12—N6—C10—C9176.0 (4)
N3—Ni1—N5—C11110.4 (3)C9—N5—C11—N60.4 (4)
N5i—Ni1—N5—C96 (100)Ni1—N5—C11—N6172.9 (2)
N1—Ni1—N5—C9150.0 (3)C10—N6—C11—N50.2 (4)
N1i—Ni1—N5—C930.0 (3)C12—N6—C11—N5176.4 (3)
N3i—Ni1—N5—C9118.5 (3)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW—H1W···Cl10.922.293.187 (3)166
OW—H2W···Cl1ii0.892.353.205 (3)162
Symmetry code: (ii) x, y+1, z.
 

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