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 compound, [Ni(C14H16N8O2)2(H2O)4](CH3COO)2, is isostructural with the published CoII complex. The Ni atom occupies an inversion centre and is octahedrally coordinated by four aqua ligands and two mol­ecules of the Schiff base.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804012425/ng6031sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804012425/ng6031Isup2.hkl
Contains datablock I

CCDC reference: 242286

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.038
  • wR factor = 0.077
  • Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 609.40 Ang-3 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C2 H3 O2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear (Rigaku, 1999); data reduction: CrystalStructure (Rigaku/MSC, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ni(C14H16N8O2)2(H2O)4](C2H3O2)2Z = 1
Mr = 577.21F(000) = 302
Triclinic, P1Dx = 1.573 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 7.8498 (19) ÅCell parameters from 2857 reflections
b = 8.836 (2) Åθ = 3.3–27.5°
c = 10.2711 (17) ŵ = 0.87 mm1
α = 65.822 (15)°T = 193 K
β = 69.678 (16)°Block, green
γ = 82.14 (2)°0.56 × 0.21 × 0.10 mm
V = 609.4 (2) Å3
Data collection top
Rigaku Mercury CCD
diffractometer
2731 independent reflections
Radiation source: fine-focus sealed tube2567 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
Detector resolution: 7.31 pixels mm-1θmax = 27.5°, θmin = 3.7°
ω scansh = 1010
Absorption correction: multi-scan
(Jacobson, 1998)
k = 1111
Tmin = 0.643, Tmax = 0.918l = 1311
6785 measured reflections
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.077H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0234P)2 + 0.4761P]
where P = (Fo2 + 2Fc2)/3
2731 reflections(Δ/σ)max = 0.001
198 parametersΔρmax = 0.29 e Å3
0 restraintsΔρmin = 0.27 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.50000.50000.50000.01550 (11)
O11.37861 (19)1.20067 (17)0.02653 (16)0.0248 (3)
O20.25190 (19)0.47181 (19)0.48349 (18)0.0231 (3)
O30.6289 (2)0.51561 (19)0.28078 (16)0.0204 (3)
O40.9793 (2)0.4510 (2)0.18607 (19)0.0316 (4)
O51.05363 (19)0.60590 (18)0.28327 (16)0.0255 (3)
N10.4678 (2)0.7599 (2)0.41767 (18)0.0190 (3)
N20.9296 (2)1.0631 (2)0.17038 (19)0.0222 (4)
N31.0764 (2)1.1672 (2)0.0907 (2)0.0256 (4)
N41.2605 (3)0.9399 (2)0.0947 (2)0.0251 (4)
C10.3062 (3)0.8327 (3)0.4540 (2)0.0236 (4)
H10.20040.76490.51100.028*
C20.2882 (3)1.0023 (3)0.4116 (2)0.0268 (4)
H2A0.17181.05000.43780.032*
C30.4415 (3)1.1019 (3)0.3306 (2)0.0250 (4)
H3A0.43201.21850.30260.030*
C40.6094 (3)1.0296 (2)0.2904 (2)0.0200 (4)
C50.6148 (3)0.8577 (2)0.3352 (2)0.0198 (4)
H50.72870.80750.30570.024*
C60.7752 (3)1.1301 (2)0.2085 (2)0.0219 (4)
H60.76831.24640.18320.026*
C71.2461 (3)1.1033 (2)0.0500 (2)0.0205 (4)
C81.0929 (3)0.5264 (2)0.1986 (2)0.0195 (4)
C91.2899 (3)0.5237 (3)0.1074 (3)0.0283 (5)
H9A1.30490.44960.05470.042*
H9B1.36370.48370.17470.042*
H9C1.32930.63610.03350.042*
H2B0.217 (4)0.524 (4)0.408 (3)0.048 (8)*
H2C0.155 (4)0.447 (4)0.563 (4)0.056 (9)*
H3B1.068 (3)1.262 (3)0.078 (3)0.024 (6)*
H3C0.743 (4)0.500 (4)0.261 (3)0.045 (8)*
H3D0.618 (4)0.599 (4)0.214 (4)0.060 (10)*
H4A1.168 (4)0.876 (3)0.152 (3)0.035 (7)*
H4B1.371 (4)0.896 (3)0.073 (3)0.035 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01304 (17)0.01516 (18)0.01659 (18)0.00265 (12)0.00259 (13)0.00549 (14)
O10.0204 (7)0.0192 (7)0.0268 (8)0.0041 (6)0.0027 (6)0.0042 (6)
O20.0163 (7)0.0294 (8)0.0206 (7)0.0043 (6)0.0053 (6)0.0062 (6)
O30.0174 (7)0.0217 (8)0.0183 (7)0.0001 (6)0.0035 (6)0.0058 (6)
O40.0201 (7)0.0377 (9)0.0449 (10)0.0004 (6)0.0059 (7)0.0272 (8)
O50.0218 (7)0.0301 (8)0.0250 (8)0.0035 (6)0.0029 (6)0.0137 (6)
N10.0185 (8)0.0185 (8)0.0190 (8)0.0013 (6)0.0051 (6)0.0066 (7)
N20.0232 (8)0.0184 (8)0.0226 (9)0.0042 (7)0.0040 (7)0.0071 (7)
N30.0231 (9)0.0142 (9)0.0335 (10)0.0040 (7)0.0033 (8)0.0072 (8)
N40.0226 (9)0.0173 (9)0.0298 (10)0.0018 (7)0.0035 (8)0.0073 (8)
C10.0187 (9)0.0252 (11)0.0238 (10)0.0014 (8)0.0043 (8)0.0083 (8)
C20.0218 (10)0.0255 (11)0.0298 (11)0.0058 (8)0.0067 (9)0.0107 (9)
C30.0282 (11)0.0178 (10)0.0264 (11)0.0039 (8)0.0099 (9)0.0065 (8)
C40.0231 (10)0.0172 (9)0.0186 (9)0.0013 (7)0.0064 (8)0.0056 (8)
C50.0197 (9)0.0191 (10)0.0194 (9)0.0011 (7)0.0042 (8)0.0075 (8)
C60.0267 (10)0.0140 (9)0.0230 (10)0.0016 (8)0.0074 (8)0.0053 (8)
C70.0223 (9)0.0207 (10)0.0178 (9)0.0008 (8)0.0059 (8)0.0070 (8)
C80.0169 (9)0.0195 (10)0.0193 (9)0.0008 (7)0.0053 (8)0.0054 (8)
C90.0213 (10)0.0306 (12)0.0300 (11)0.0001 (9)0.0035 (9)0.0130 (9)
Geometric parameters (Å, º) top
Ni1—O22.0689 (15)N2—N31.364 (2)
Ni1—O2i2.0689 (15)N3—H3B0.79 (2)
Ni1—O32.0770 (15)N4—H4A0.86 (3)
Ni1—O3i2.0770 (15)N4—H4B0.89 (3)
Ni1—N1i2.1098 (17)C1—C21.381 (3)
Ni1—N12.1098 (17)C1—H10.9500
C7—O11.250 (2)C2—C31.381 (3)
O2—H2B0.84 (3)C2—H2A0.9500
O2—H2C0.87 (3)C3—C41.387 (3)
O3—H3C0.85 (3)C3—H3A0.9500
O3—H3D0.79 (4)C4—C51.394 (3)
C8—O41.252 (2)C4—C61.461 (3)
C8—O51.265 (2)C5—H50.9500
C5—N11.338 (2)C6—H60.9500
N1—C11.344 (3)C8—C91.507 (3)
C6—N21.279 (3)C9—H9A0.9800
C7—N31.367 (3)C9—H9B0.9800
C7—N41.326 (3)C9—H9C0.9800
O2—Ni1—O2i180.0N1—C1—C2122.47 (19)
O2—Ni1—O390.14 (6)N1—C1—H1118.8
O2i—Ni1—O389.86 (6)C2—C1—H1118.8
O2—Ni1—O3i89.86 (6)C1—C2—C3119.23 (19)
O2i—Ni1—O3i90.14 (6)C1—C2—H2A120.4
O3—Ni1—O3i180.0C3—C2—H2A120.4
O2—Ni1—N190.34 (6)C2—C3—C4119.28 (19)
O2—Ni1—N1i89.66 (6)C2—C3—H3A120.4
O2i—Ni1—N1i90.34 (6)C4—C3—H3A120.4
O3—Ni1—N189.83 (6)C3—C4—C5117.69 (18)
O3—Ni1—N1i90.17 (6)C3—C4—C6120.93 (18)
O3i—Ni1—N1i89.83 (6)C5—C4—C6121.35 (18)
O2i—Ni1—N189.66 (6)N1—C5—C4123.43 (18)
O3i—Ni1—N190.17 (6)N1—C5—H5118.3
N1i—Ni1—N1180.0C4—C5—H5118.3
Ni1—O2—H2B126 (2)N2—C6—C4120.71 (18)
Ni1—O2—H2C120 (2)N2—C6—H6119.6
H2B—O2—H2C107 (3)C4—C6—H6119.6
Ni1—O3—H3C113.0 (19)O1—C7—N4123.52 (19)
Ni1—O3—H3D118 (2)O1—C7—N3118.87 (18)
H3C—O3—H3D105 (3)N4—C7—N3117.61 (18)
C5—N1—C1117.85 (17)O4—C8—O5124.30 (18)
C5—N1—Ni1119.32 (13)O4—C8—C9118.62 (18)
C1—N1—Ni1122.64 (13)O5—C8—C9117.09 (17)
C6—N2—N3116.60 (17)C8—C9—H9A109.5
N2—N3—C7119.62 (17)C8—C9—H9B109.5
N2—N3—H3B121.2 (17)H9A—C9—H9B109.5
C7—N3—H3B118.5 (17)C8—C9—H9C109.5
C7—N4—H4A121.1 (18)H9A—C9—H9C109.5
C7—N4—H4B118.6 (17)H9B—C9—H9C109.5
H4A—N4—H4B120 (2)
O2—Ni1—N1—C5148.10 (14)C1—C2—C3—C41.6 (3)
O2i—Ni1—N1—C531.90 (14)C2—C3—C4—C50.3 (3)
O3—Ni1—N1—C557.96 (14)C2—C3—C4—C6178.24 (19)
O3i—Ni1—N1—C5122.04 (14)C1—N1—C5—C42.5 (3)
O2—Ni1—N1—C137.12 (16)Ni1—N1—C5—C4172.54 (15)
O2i—Ni1—N1—C1142.88 (16)C3—C4—C5—N11.8 (3)
O3—Ni1—N1—C1127.26 (16)C6—C4—C5—N1176.11 (18)
O3i—Ni1—N1—C152.74 (16)N3—N2—C6—C4178.32 (17)
C6—N2—N3—C7178.21 (19)C3—C4—C6—N2179.32 (19)
C5—N1—C1—C21.1 (3)C5—C4—C6—N22.8 (3)
Ni1—N1—C1—C2173.78 (16)N2—N3—C7—O1178.03 (17)
N1—C1—C2—C30.9 (3)N2—N3—C7—N42.0 (3)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2b···O5ii0.84 (3)1.98 (3)2.789 (2)160 (3)
N3—H3b···O4iii0.79 (2)2.27 (2)2.966 (2)147 (2)
O3—H3c···O40.85 (3)1.81 (3)2.647 (2)166 (3)
N4—H4a···O50.86 (3)2.33 (3)3.089 (3)147 (2)
Symmetry codes: (ii) x1, y, z; (iii) x, y+1, z.
 

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