Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title complex, [Ni(C6H8N2)4]Cl2, consists of a centrosymmetric octahedral six-coordinate nickel(II) coordination complex cation and two chloride ions. The Ni atom sits on a crystallographic inversion center. Two of the 1,2-di­amino­benzene ligands are chelating and the other two are monodentate. The chelating ligands define an equatorial plane and the monodentate ligands are axially trans. In addition to one hydrogen bond between the non-coordinated N atom of the monodentate ligand and an adjacent metal complex, there is extensive hydrogen bonding to the chloride ions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804033574/bv6007sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804033574/bv6007Isup2.hkl
Contains datablock I

CCDC reference: 262294

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.062
  • wR factor = 0.110
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT420_ALERT_2_C D-H Without Acceptor N4 - H15 ... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 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 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius 2000); cell refinement: DENZO and SCALEPACK; data reduction: DENZO and SCALEPACK (Version 1.96.2; Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: TEXSAN for Windows (Version 1.06; MSC, 1999); software used to prepare material for publication: TEXSAN for Windows.

(I) top
Crystal data top
[Ni(C6H8N2)4]Cl2F(000) = 588.00
Mr = 562.18Dx = 1.468 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 2903 reflections
a = 12.8062 (7) Åθ = 2.5–27.5°
b = 8.1242 (4) ŵ = 1.00 mm1
c = 12.4333 (8) ÅT = 100 K
β = 100.610 (2)°Parallelpiped, violet
V = 1271.45 (11) Å30.15 × 0.12 × 0.10 mm
Z = 2
Data collection top
KappaCCD (with an Oxford Cryosystems Cryostream cooler)
diffractometer
2919 independent reflections
Radiation source: fine-focus sealed tube2077 reflections with I > 3.00σ(I)
Graphite monochromatorRint = 0.032
ω scans with κ offsetsθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
h = 016
Tmin = 0.854, Tmax = 0.905k = 1010
12286 measured reflectionsl = 1615
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullH-atom parameters not refined
R[F2 > 2σ(F2)] = 0.063Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.00140625|Fo|2]
wR(F2) = 0.110(Δ/σ)max = 0.000186
S = 0.98Δρmax = 0.85 e Å3
2077 reflectionsΔρmin = 0.68 e Å3
161 parametersExtinction correction: Zachariasen
0 restraintsExtinction coefficient: 0.69306
Special details top

Geometry. Ni1 is located on an inversion center. H15 and H16, the hydrogen atoms associated with N4 were found in difference maps, but not refined.

Refinement. Refinement of F2. The weighted R-factor wR and goodness of fit are based on F2, conventional R-factors R are based on F. R-factors based on F2 are statistically about twice as large as those based on F. H15 and H15, the hydrogen atoms associated with N4, were found in difference maps, but not refined. All of the hydrogen atoms are assigned thermal parameters 1.2 times larger than the atoms to which they are bound.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.00000.00001.00000.0170 (1)
Cl10.02434 (6)0.02883 (8)0.64912 (5)0.0222 (2)
N10.1157 (2)0.1838 (3)0.9975 (2)0.0201 (6)
N20.0987 (2)0.0677 (3)0.8517 (2)0.0193 (6)
N30.0890 (2)0.1656 (3)0.9071 (2)0.0197 (6)
N40.2344 (2)0.0545 (3)0.8315 (2)0.0234 (6)
C10.2053 (2)0.1529 (3)0.9096 (2)0.0205 (7)
C20.3000 (2)0.2409 (3)0.9005 (2)0.0225 (7)
C30.3852 (2)0.2050 (4)0.8174 (2)0.0249 (8)
C40.3754 (2)0.0812 (4)0.7432 (2)0.0262 (8)
C50.2823 (2)0.0086 (3)0.7523 (2)0.0230 (7)
C60.1967 (2)0.0262 (3)0.8363 (2)0.0187 (7)
C70.2014 (2)0.1862 (3)0.9384 (2)0.0199 (7)
C80.2413 (2)0.3113 (3)1.0115 (2)0.0220 (7)
C90.3499 (2)0.3302 (3)1.0474 (2)0.0259 (8)
C100.4198 (2)0.2286 (4)1.0070 (3)0.0275 (8)
C110.3816 (2)0.1058 (4)0.9327 (2)0.0242 (8)
C120.2729 (2)0.0805 (3)0.8986 (2)0.0216 (7)
H10.13960.18411.06540.024*
H20.08550.28790.98640.024*
H30.30630.32580.95150.027*
H40.44970.26490.81150.030*
H50.43320.05780.68550.031*
H60.27660.09390.70140.028*
H70.11470.18170.85350.023*
H80.06300.04630.79260.023*
H90.07650.12640.83390.024*
H100.05860.27190.90920.024*
H110.19340.38451.03710.026*
H120.37590.41271.09970.031*
H130.49420.24291.03000.033*
H140.43050.03750.90460.029*
H150.29200.11000.80510.019*
H160.17540.03140.77280.019*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0205 (3)0.0138 (3)0.0167 (3)0.0010 (2)0.0032 (2)0.0003 (2)
Cl10.0295 (4)0.0191 (4)0.0181 (3)0.0026 (3)0.0044 (3)0.0004 (2)
N10.025 (1)0.0154 (11)0.0203 (11)0.0011 (9)0.0057 (10)0.0011 (9)
N20.023 (1)0.0148 (11)0.0201 (11)0.0001 (9)0.0049 (9)0.0006 (9)
N30.0228 (13)0.0145 (11)0.0221 (11)0.0025 (9)0.0048 (9)0.0005 (9)
N40.026 (1)0.0214 (12)0.0239 (12)0.0026 (10)0.0081 (10)0.0026 (10)
C10.022 (2)0.0173 (13)0.0228 (13)0.0007 (11)0.0054 (11)0.0019 (11)
C20.027 (2)0.0156 (13)0.026 (2)0.0016 (11)0.0091 (12)0.0045 (11)
C30.021 (2)0.023 (2)0.031 (2)0.0024 (12)0.0050 (12)0.0062 (12)
C40.026 (2)0.024 (2)0.027 (2)0.0019 (12)0.0007 (12)0.0048 (12)
C50.027 (2)0.021 (1)0.020 (1)0.0013 (12)0.0028 (12)0.0010 (11)
C60.020 (2)0.019 (1)0.0190 (13)0.0001 (11)0.0070 (11)0.0042 (10)
C70.024 (2)0.0161 (13)0.0206 (13)0.0001 (11)0.0057 (11)0.0041 (10)
C80.025 (2)0.0176 (13)0.024 (1)0.0011 (11)0.0046 (12)0.0023 (11)
C90.029 (2)0.0172 (13)0.030 (2)0.0023 (12)0.0031 (13)0.0013 (12)
C100.022 (2)0.024 (2)0.035 (2)0.0008 (12)0.0039 (13)0.0059 (13)
C110.024 (2)0.021 (1)0.029 (1)0.0032 (12)0.0064 (12)0.0033 (12)
C120.031 (2)0.016 (1)0.0189 (13)0.0003 (11)0.0068 (12)0.0020 (11)
Geometric parameters (Å, º) top
Ni1—N12.100 (2)C9—C101.379 (4)
Ni1—N1i2.100 (2)C10—C111.386 (4)
Ni1—N22.108 (2)C11—C121.394 (4)
Ni1—N2i2.108 (2)N1—H10.950
Ni1—N32.220 (2)N1—H20.950
Ni1—N3i2.220 (2)N2—H70.950
N1—C11.453 (4)N2—H80.950
N2—C61.451 (4)N3—H90.950
N3—C71.431 (4)N3—H100.950
N4—C121.411 (4)N4—H150.972
C1—C21.395 (4)N4—H160.967
C1—C61.393 (4)C2—H30.950
C2—C31.388 (4)C3—H40.950
C3—C41.387 (4)C4—H50.950
C4—C51.385 (4)C5—H60.950
C5—C61.396 (4)C8—H110.950
C7—C81.396 (4)C9—H120.950
C7—C121.409 (4)C10—H130.950
C8—C91.389 (4)C11—H140.950
N4···C3ii3.506 (4)N4···C2ii3.562 (4)
N1—Ni1—N1i180.00Ni1—N1—H2109.28
N1—Ni1—N282.21 (9)C1—N1—H1109.29
N1—Ni1—N2i97.79 (9)C1—N1—H2109.29
N1—Ni1—N389.42 (8)H1—N1—H2109.46
N1—Ni1—N3i90.58 (8)Ni1—N2—H7109.33
N2—Ni1—N2i180.00Ni1—N2—H8109.33
N2—Ni1—N389.18 (8)C6—N2—H7109.33
N2—Ni1—N3i90.82 (8)C6—N2—H8109.33
N3—Ni1—N3i180.00H7—N2—H8109.46
Ni1—N1—C1110.2 (2)Ni1—N3—H9106.48
Ni1—N2—C6110.1 (2)Ni1—N3—H10106.48
Ni1—N3—C7121.1 (2)C7—N3—H9106.48
N1—C1—C2121.8 (3)C7—N3—H10106.48
N1—C1—C6118.3 (2)H9—N3—H10109.46
C2—C1—C6119.9 (3)C12—N4—H15110.82
C1—C2—C3120.3 (3)C12—N4—H16115.78
C2—C3—C4119.6 (3)H15—N4—H16111.79
C3—C4—C5120.6 (3)C1—C2—H3119.84
C4—C5—C6120.0 (3)C3—C2—H3119.84
N2—C6—C1118.2 (2)C2—C3—H4120.21
N2—C6—C5122.2 (2)C4—C3—H4120.21
C1—C6—C5119.6 (3)C3—C4—H5119.70
N3—C7—C8119.4 (2)C5—C4—H5119.70
N3—C7—C12121.3 (2)C4—C5—H6120.00
C8—C7—C12119.3 (3)C6—C5—H6120.00
C7—C8—C9120.9 (3)C7—C8—H11119.53
C8—C9—C10119.7 (3)C9—C8—H11119.53
C9—C10—C11120.1 (3)C8—C9—H12120.15
C10—C11—C12121.3 (3)C10—C9—H12120.15
N4—C12—C7120.1 (3)C9—C10—H13119.97
N4—C12—C11121.0 (3)C11—C10—H13119.98
C7—C12—C11118.7 (3)C10—C11—H14119.36
Ni1—N1—H1109.29C12—C11—H14119.36
Ni1—N1—C1—C2169.6 (2)N2—C6—C1—C2177.1 (2)
Ni1—N1—C1—C67.2 (3)N2—C6—C5—C4178.0 (2)
Ni1—N1i—C1i—C2i169.6 (2)N3—Ni1—N1—C197.8 (2)
Ni1—N1i—C1i—C6i7.2 (3)N3—Ni1—N1i—C1i82.2 (2)
Ni1—N2—C6—C17.4 (3)N3—Ni1—N2—C698.1 (2)
Ni1—N2—C6—C5171.5 (2)N3—Ni1—N2i—C6i81.9 (2)
Ni1—N2i—C6i—C1i7.4 (3)N3—C7—C8—C9177.1 (2)
Ni1—N2i—C6i—C5i171.5 (2)N3—C7—C12—N43.7 (4)
Ni1—N3—C7—C890.7 (3)N3—C7—C12—C11179.4 (2)
Ni1—N3—C7—C1288.0 (3)N4—C12—C7—C8175.0 (2)
Ni1—N3i—C7i—C8i90.7 (3)N4—C12—C11—C10173.7 (3)
Ni1—N3i—C7i—C12i88.0 (3)C1—C2—C3—C40.1 (4)
N1—Ni1—N2—C68.6 (2)C1—C6—C5—C40.9 (4)
N1—Ni1—N2i—C6i171.4 (2)C2—C1—C6—C51.9 (4)
N1—Ni1—N3—C7134.3 (2)C2—C3—C4—C51.1 (4)
N1—Ni1—N3i—C7i45.7 (2)C3—C2—C1—C61.3 (4)
N1—C1—C2—C3178.1 (3)C3—C4—C5—C60.6 (4)
N1—C1—C6—N20.2 (4)C7—C8—C9—C102.8 (4)
N1—C1—C6—C5178.8 (2)C7—C12—C11—C102.0 (4)
N2—Ni1—N1—C18.5 (2)C8—C7—C12—C110.8 (4)
N2—Ni1—N1i—C1i171.5 (2)C8—C9—C10—C111.5 (4)
N2—Ni1—N3—C7143.4 (2)C9—C8—C7—C121.6 (4)
N2—Ni1—N3i—C7i36.6 (2)C9—C10—C11—C120.9 (4)
Symmetry codes: (i) x, y, z+2; (ii) x, y1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···N4i0.952.193.021 (3)145
N1—H2···Cl1iii0.952.693.313 (2)124
N2—H7···Cl1ii0.952.623.414 (2)141
N2—H8···Cl10.952.353.302 (2)176
N3—H9···Cl10.952.413.351 (2)174
N3—H10···Cl1iv0.952.393.306 (2)161
N4—H16···Cl10.972.293.254 (3)173
Symmetry codes: (i) x, y, z+2; (ii) x, y1/2, z+3/2; (iii) x, y+1/2, z+1/2; (iv) x, y+1/2, z+3/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds