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The title compound, [Ni(en)(TETA)][GeF6] or [Ni(C2H8N2)(C6H18N4)][GeF6], was synthesized under mild solvothermal conditions in the presence of triethyl­enetetr­amine (TETA) as a base. It is a new salt composed of [GeF6]2− anions and [Ni(en)(TETA)]2+ cations. The ions are linked together by hydrogen bonding between F atoms and N—H groups. The complex cation and anion lie on twofold axes of the space group Pccn.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804009791/na6318sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804009791/na6318Isup2.hkl
Contains datablock I

CCDC reference: 239119

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.053
  • wR factor = 0.126
  • Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1B ... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 2 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: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SMART (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL.

(Ethylenediamine-κ2N)(triethylenetetramine-κ4N)nickel hexafluorogermanate top
Crystal data top
[Ni(C2H8N2)(C6H18N4)][GeF6]F(000) = 920
Mr = 451.65Dx = 1.967 Mg m3
Orthorhombic, PccnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2acCell parameters from 2958 reflections
a = 8.9029 (2) Åθ = 2.2–25.0°
b = 9.4731 (3) ŵ = 3.27 mm1
c = 18.0856 (2) ÅT = 293 K
V = 1525.30 (6) Å3Prism, purple
Z = 40.22 × 0.12 × 0.10 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
1315 independent reflections
Radiation source: fine-focus sealed tube1216 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
φ and ω scansθmax = 25.0°, θmin = 3.1°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 810
Tmin = 0.630, Tmax = 0.721k = 1110
7696 measured reflectionsl = 1921
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)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.126H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0415P)2 + 11.3515P]
where P = (Fo2 + 2Fc2)/3
1315 reflections(Δ/σ)max < 0.001
101 parametersΔρmax = 1.03 e Å3
0 restraintsΔρmin = 0.56 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
Ge0.75000.75000.34232 (4)0.0141 (3)
F10.5913 (4)0.8645 (3)0.3406 (2)0.0297 (9)
F20.6654 (4)0.6449 (3)0.27071 (18)0.0236 (8)
F30.6636 (5)0.6400 (4)0.41024 (19)0.0305 (9)
Ni0.25000.75000.16241 (5)0.0098 (3)
N10.0487 (5)0.6278 (5)0.1585 (3)0.0194 (10)
H1A0.07190.53570.15400.023*
H1B0.00300.63920.20090.023*
N20.1410 (5)0.8607 (4)0.0767 (2)0.0152 (10)
H2C0.15270.95490.08480.018*
N30.1635 (5)0.8710 (4)0.2484 (2)0.0157 (10)
H3A0.17970.96320.23940.019*
H3B0.06380.85710.25210.019*
C10.0442 (7)0.6720 (6)0.0958 (3)0.0198 (13)
H1C0.14940.65560.10690.024*
H1D0.01820.61710.05240.024*
C20.0188 (7)0.8272 (7)0.0806 (3)0.0228 (13)
H2A0.06650.85240.03430.027*
H2B0.06490.88260.11960.027*
C30.2158 (7)0.8241 (6)0.0057 (3)0.0196 (13)
H3C0.29440.89240.00400.024*
H3D0.14290.83060.03400.024*
C40.2371 (7)0.8300 (6)0.3172 (3)0.0214 (12)
H4A0.17480.85620.35900.026*
H4B0.33250.87860.32170.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ge0.0134 (4)0.0067 (4)0.0221 (4)0.0005 (3)0.0000.000
F10.0165 (17)0.0139 (17)0.059 (2)0.0033 (14)0.0085 (16)0.0002 (16)
F20.0234 (18)0.0165 (16)0.0311 (18)0.0004 (14)0.0052 (15)0.0038 (14)
F30.038 (2)0.0175 (18)0.036 (2)0.0059 (17)0.0091 (16)0.0013 (14)
Ni0.0108 (5)0.0073 (5)0.0111 (5)0.0000 (4)0.0000.000
N10.014 (2)0.016 (2)0.028 (3)0.0029 (19)0.001 (2)0.002 (2)
N20.018 (2)0.007 (2)0.020 (2)0.0012 (19)0.0012 (19)0.0020 (18)
N30.015 (2)0.012 (2)0.020 (2)0.0016 (18)0.0027 (19)0.0012 (18)
C10.009 (3)0.019 (3)0.032 (3)0.000 (2)0.005 (2)0.005 (2)
C20.021 (3)0.023 (3)0.024 (3)0.000 (3)0.006 (2)0.004 (2)
C30.030 (4)0.014 (3)0.015 (3)0.002 (3)0.001 (2)0.002 (2)
C40.018 (3)0.030 (3)0.017 (3)0.000 (3)0.001 (2)0.004 (2)
Geometric parameters (Å, º) top
Ge—F11.781 (3)N2—C31.486 (7)
Ge—F1i1.781 (3)N2—H2C0.9100
Ge—F3i1.785 (3)N3—C41.459 (7)
Ge—F31.785 (3)N3—H3A0.9000
Ge—F21.799 (3)N3—H3B0.9000
Ge—F2i1.799 (3)C1—C21.512 (8)
Ni—N3ii2.080 (4)C1—H1C0.9700
Ni—N32.080 (4)C1—H1D0.9700
Ni—N2ii2.108 (5)C2—H2A0.9700
Ni—N22.108 (5)C2—H2B0.9700
Ni—N12.135 (5)C3—C3ii1.530 (11)
Ni—N1ii2.135 (5)C3—H3C0.9700
N1—C11.465 (7)C3—H3D0.9700
N1—H1A0.9000C4—C4ii1.532 (12)
N1—H1B0.9000C4—H4A0.9700
N2—C21.459 (7)C4—H4B0.9700
F1—Ge—F1i178.0 (3)C2—N2—C3115.3 (4)
F1—Ge—F3i89.93 (17)C2—N2—Ni107.7 (3)
F1i—Ge—F3i91.46 (17)C3—N2—Ni108.2 (3)
F1—Ge—F391.46 (17)C2—N2—H2C108.5
F1i—Ge—F389.93 (17)C3—N2—H2C108.5
F3i—Ge—F393.0 (2)Ni—N2—H2C108.5
F1—Ge—F289.56 (16)C4—N3—Ni108.9 (3)
F1i—Ge—F288.98 (16)C4—N3—H3A109.9
F3i—Ge—F2177.40 (16)Ni—N3—H3A109.9
F3—Ge—F289.54 (16)C4—N3—H3B109.9
F1—Ge—F2i88.98 (16)Ni—N3—H3B109.9
F1i—Ge—F2i89.56 (16)H3A—N3—H3B108.3
F3i—Ge—F2i89.54 (16)N1—C1—C2109.5 (5)
F3—Ge—F2i177.40 (16)N1—C1—H1C109.8
F2—Ge—F2i87.9 (2)C2—C1—H1C109.8
N3ii—Ni—N383.2 (2)N1—C1—H1D109.8
N3ii—Ni—N2ii96.04 (17)C2—C1—H1D109.8
N3—Ni—N2ii173.95 (18)H1C—C1—H1D108.2
N3ii—Ni—N2173.95 (18)N2—C2—C1111.5 (5)
N3—Ni—N296.04 (17)N2—C2—H2A109.3
N2ii—Ni—N285.3 (2)C1—C2—H2A109.3
N3ii—Ni—N192.10 (18)N2—C2—H2B109.3
N3—Ni—N190.72 (18)C1—C2—H2B109.3
N2ii—Ni—N195.31 (18)H2A—C2—H2B108.0
N2—Ni—N181.90 (18)N2—C3—C3ii113.1 (3)
N3ii—Ni—N1ii90.72 (18)N2—C3—H3C109.0
N3—Ni—N1ii92.10 (18)C3ii—C3—H3C109.0
N2ii—Ni—N1ii81.90 (18)N2—C3—H3D109.0
N2—Ni—N1ii95.31 (18)C3ii—C3—H3D109.0
N1—Ni—N1ii176.2 (3)H3C—C3—H3D107.8
C1—N1—Ni110.2 (4)N3—C4—C4ii109.3 (4)
C1—N1—H1A109.6N3—C4—H4A109.8
Ni—N1—H1A109.6C4ii—C4—H4A109.8
C1—N1—H1B109.6N3—C4—H4B109.8
Ni—N1—H1B109.6C4ii—C4—H4B109.8
H1A—N1—H1B108.1H4A—C4—H4B108.3
Symmetry codes: (i) x+3/2, y+3/2, z; (ii) x+1/2, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···F3iii0.902.193.005 (6)151
N1—H1A···F2iii0.902.343.064 (6)138
N2—H2C···F1iv0.912.253.035 (5)145
N2—H2C···F3v0.912.403.176 (6)143
N3—H3A···F2v0.902.213.028 (6)150
N3—H3A···F1iv0.902.323.046 (5)138
N3—H3B···F2ii0.902.072.960 (6)171
C4—H4B···F10.972.333.198 (7)148
Symmetry codes: (ii) x+1/2, y+3/2, z; (iii) x1/2, y+1, z+1/2; (iv) x1/2, y+2, z+1/2; (v) x+1, y+1/2, z+1/2.
 

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