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The title compound, cis-[Ni(C2H8N2)2(H2O)2](C8H4O4)·H2O, was obtained by a reaction of nickel chloride hexahydrate, terephthalic acid, ethyl­enedi­amine and NaOH (molar ratio 2:1:4:2). The compound contains a six-coordinate NiII cation, with four ethyl­enedi­amine N atoms and two water O atoms attached to the Ni atom, one benzene-1,4-di­carboxyl­ate anion, and one water molecule of solvation. A C2 axis passes through the Ni atom, the anion and the water O atom. Intermolecular hydrogen-bonding interactions are present, linking the nickel complex cations, organic anions and uncoordinated water mol­ecules in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803028988/cv6254sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803028988/cv6254Isup2.hkl
Contains datablock I

CCDC reference: 231838

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.033
  • wR factor = 0.097
  • Data-to-parameter ratio = 20.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 1 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O1 = 6.76 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N1 = 7.54 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N2 = 5.01 su PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.84 PLAT751_ALERT_4_C Bond Calc 2.09650, Rep 2.0965(11) ...... Senseless su NI1 -N2 1.555 1.555 PLAT751_ALERT_4_C Bond Calc 2.09650, Rep 2.0965(11) ...... Senseless su NI1 -N2 1.555 2.656 PLAT751_ALERT_4_C Bond Calc 1.47733, Rep 1.477(2) ...... Senseless su N2 -C2 1.555 1.555 PLAT752_ALERT_4_C Angle Calc 94.69, Rep 94.69(4) ...... Senseless su N2 -NI1 -N1 1.555 1.555 1.555 PLAT752_ALERT_4_C Angle Calc 167.68, Rep 167.68(4) ...... Senseless su N2 -NI1 -O1 1.555 1.555 1.555 PLAT752_ALERT_4_C Angle Calc 107.82, Rep 107.82(9) ...... Senseless su C2 -N2 -NI1 1.555 1.555 1.555 PLAT757_ALERT_4_C D...A Calc 3.00307, Rep 3.003(2) ...... Senseless su N2 -O4 1.555 1.555 PLAT757_ALERT_4_C D...A Calc 2.91901, Rep 2.919(3) ...... Senseless su N2 -O2 1.555 5.667
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C12 H26 N4 Ni1 O7 Atom count from _chemical_formula_moiety:C12 H26 N4 Ni1 O9
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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 8 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ni(C2H8N2)2(H2O)2](C8H4O4)·H2OF(000) = 840
Mr = 397.08Dx = 1.443 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3931 reflections
a = 12.489 (1) Åθ = 2.5–25°
b = 20.4936 (16) ŵ = 1.10 mm1
c = 8.4365 (6) ÅT = 295 K
β = 122.191 (1)°Columnar, blue
V = 1827.3 (2) Å30.60 × 0.40 × 0.30 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
2269 independent reflections
Radiation source: fine-focus sealed tube2024 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
φ and ω scansθmax = 28.3°, θmin = 2.0°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1995)
h = 1316
Tmin = 0.620, Tmax = 0.718k = 2722
6464 measured reflectionsl = 1110
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)] = 0.033Hydrogen site location: difference Fourier map
wR(F2) = 0.097H-atom parameters not refined
S = 1.07 w = 1/[σ2(Fo2) + (0.0632P)2 + 0.0602P]
where P = (Fo2 + 2Fc2)/3
2269 reflections(Δ/σ)max = 0.001
110 parametersΔρmax = 0.37 e Å3
0 restraintsΔρmin = 0.32 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
Ni10.50000.595504 (11)0.75000.03685 (11)
O10.36711 (10)0.52091 (5)0.59740 (14)0.0492 (3)
H1A0.33350.50940.65390.059*
H1B0.31560.53060.48600.059*
O20.18596 (18)0.35714 (9)0.7373 (2)0.0980 (6)
O30.24480 (12)0.45756 (7)0.72807 (17)0.0648 (4)
O40.50000.79167 (10)0.75000.0987 (9)
H4A0.55240.81640.73910.118*
N10.47423 (9)0.59892 (4)0.97726 (14)0.0507 (3)
H1C0.43380.56280.97880.061*
H1D0.54970.60111.08600.061*
N20.64459 (9)0.66553 (4)0.86145 (14)0.0465 (3)
H2A0.61250.70540.85620.056*
H2B0.70260.65620.98200.056*
C10.3986 (2)0.65715 (9)0.9542 (3)0.0630 (5)
H1E0.45230.69550.99650.076*
H1F0.36100.65291.02890.076*
C20.70362 (18)0.66435 (11)0.7493 (3)0.0645 (5)
H2C0.76240.62810.78830.077*
H2D0.75020.70450.76820.077*
C30.04189 (16)0.35018 (9)0.3456 (2)0.0547 (4)
H3A0.06910.31080.41000.066*
C40.08581 (15)0.40847 (8)0.4425 (2)0.0457 (4)
C50.04392 (15)0.46678 (9)0.3461 (2)0.0480 (4)
H5A0.07450.50610.40970.058*
C60.17865 (18)0.40756 (9)0.6520 (2)0.0540 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.03501 (16)0.04103 (17)0.02896 (16)0.0000.01331 (12)0.000
O10.0459 (6)0.0557 (6)0.0323 (5)0.0087 (5)0.0116 (5)0.0008 (5)
O20.0963 (11)0.1083 (12)0.0415 (8)0.0294 (10)0.0045 (7)0.0250 (8)
O30.0595 (7)0.0904 (9)0.0287 (6)0.0192 (7)0.0130 (5)0.0005 (6)
O40.1116 (19)0.0499 (11)0.160 (3)0.0000.090 (2)0.000
N10.0556 (9)0.0558 (8)0.0412 (8)0.0000 (6)0.0261 (7)0.0014 (5)
N20.0409 (6)0.0491 (7)0.0396 (7)0.0034 (5)0.0148 (6)0.0005 (5)
C10.0743 (12)0.0696 (11)0.0567 (11)0.0094 (9)0.0427 (10)0.0021 (9)
C20.0548 (10)0.0789 (12)0.0639 (12)0.0160 (9)0.0343 (9)0.0044 (10)
C30.0493 (9)0.0586 (10)0.0436 (9)0.0000 (8)0.0163 (8)0.0058 (7)
C40.0351 (7)0.0660 (10)0.0297 (8)0.0024 (6)0.0130 (6)0.0042 (6)
C50.0438 (8)0.0606 (9)0.0305 (8)0.0043 (7)0.0138 (7)0.0041 (6)
C60.0409 (8)0.0804 (13)0.0303 (8)0.0054 (7)0.0120 (7)0.0077 (7)
Geometric parameters (Å, º) top
Ni1—N22.0965 (11)N2—H2A0.9000
Ni1—N2i2.0965 (11)N2—H2B0.9000
Ni1—N12.1076 (10)C1—C2i1.505 (3)
Ni1—N1i2.1076 (10)C1—H1E0.9700
Ni1—O12.1148 (10)C1—H1F0.9700
Ni1—O1i2.1148 (10)C2—C1i1.505 (3)
O1—H1A0.8200C2—H2C0.9700
O1—H1B0.8323C2—H2D0.9700
O2—C61.235 (2)C3—C3ii1.378 (3)
O3—C61.257 (2)C3—C41.385 (2)
O4—H4A0.8705C3—H3A0.9300
N1—C11.469 (2)C4—C51.382 (2)
N1—H1C0.9000C4—C61.511 (2)
N1—H1D0.9000C5—C5ii1.392 (3)
N2—C21.477 (2)C5—H5A0.9300
N2—Ni1—N2i93.60 (5)C2—N2—H2B110.1
N2—Ni1—N194.69 (4)Ni1—N2—H2B110.1
N2i—Ni1—N182.69 (4)H2A—N2—H2B108.5
N2—Ni1—N1i82.69 (4)N1—C1—C2i108.99 (14)
N2i—Ni1—N1i94.69 (4)N1—C1—H1E109.9
N1—Ni1—N1i176.19 (5)C2i—C1—H1E109.9
N2—Ni1—O1167.68 (4)N1—C1—H1F109.9
N2i—Ni1—O190.73 (4)C2i—C1—H1F109.9
N1—Ni1—O197.31 (4)H1E—C1—H1F108.3
N1i—Ni1—O185.46 (4)N2—C2—C1i108.84 (14)
N2—Ni1—O1i90.73 (4)N2—C2—H2C109.9
N2i—Ni1—O1i167.68 (4)C1i—C2—H2C109.9
N1—Ni1—O1i85.46 (4)N2—C2—H2D109.9
N1i—Ni1—O1i97.31 (4)C1i—C2—H2D109.9
O1—Ni1—O1i87.42 (6)H2C—C2—H2D108.3
Ni1—O1—H1A109.5C3ii—C3—C4120.40 (9)
Ni1—O1—H1B113.5C3ii—C3—H3A119.8
H1A—O1—H1B113.5C4—C3—H3A119.8
C1—N1—Ni1107.79 (9)C5—C4—C3119.44 (15)
C1—N1—H1C110.1C5—C4—C6120.87 (15)
Ni1—N1—H1C110.1C3—C4—C6119.70 (15)
C1—N1—H1D110.1C4—C5—C5ii120.14 (9)
Ni1—N1—H1D110.1C4—C5—H5A119.9
H1C—N1—H1D108.5C5ii—C5—H5A119.9
C2—N2—Ni1107.82 (9)O2—C6—O3124.08 (17)
C2—N2—H2A110.1O2—C6—C4117.67 (16)
Ni1—N2—H2A110.1O3—C6—C4118.24 (15)
Symmetry codes: (i) x+1, y, z+3/2; (ii) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O30.821.872.651 (2)160
O1—H1B···O3iii0.831.882.677 (2)161
N2—H2A···O40.902.143.003 (2)161
N2—H2B···O2iv0.902.032.919 (3)171
O4—H4A···O2v0.871.872.733 (3)170
Symmetry codes: (iii) x, y+1, z1/2; (iv) x+1, y+1, z+2; (v) x+1/2, y+1/2, z.
 

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