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The crystal structure of the title compound, [Ni(C2H8N2)3][MoO4], is composed of tetra­hedral [MoO4]2- anions and octa­hedral [Ni(en)3]2+ cations (en is ethyl­enediamine), both ions lying on special positions of site symmetry 2. The components are held together in a three-dimensional network by hydrogen-bonding inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806004971/ng2003sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806004971/ng2003Isup2.hkl
Contains datablock I

CCDC reference: 601220

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.040
  • wR factor = 0.153
  • Data-to-parameter ratio = 21.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - N2 .. 11.13 su
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni - N1 .. 6.98 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni - N3 .. 9.42 su PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1D ... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2D ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H2D .. O1 .. 2.64 Ang. PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 5 N1 -NI -N1 -C1 -28.01 0.18 4.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7 N3 -NI -N2 -C2 -25.60 0.60 4.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 12 N2 -NI -N3 -C3 -36.30 0.60 4.555 1.555 1.555 1.555
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 27.99 From the CIF: _reflns_number_total 1785 From the CIF: _diffrn_reflns_limit_ max hkl 18. 21. 13. From the CIF: _diffrn_reflns_limit_ min hkl -18. -21. -13. TEST1: Expected hkl limits for theta max Calculated maximum hkl 21. 21. 13. Calculated minimum hkl -21. -21. -13.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 9 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 5 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 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1987); cell refinement: TEXSAN (Molecular Structure Corporation, 1987); data reduction: TEXSAN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

Tris(ethylenediamine)nickel(II) tetraoxomolybdate(VI) top
Crystal data top
[Ni(C2H8N2)3][MoO4]Dx = 1.799 Mg m3
Mr = 398.96Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3c1Cell parameters from 200 reflections
Hall symbol: -P 3 2"cθ = 10–20°
a = 16.0024 (16) ŵ = 2.15 mm1
c = 9.9608 (19) ÅT = 291 K
V = 2209.0 (5) Å3Block, violet
Z = 60.20 × 0.12 × 0.08 mm
F(000) = 1224
Data collection top
Rigaku AFC-5R
diffractometer
1538 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.037
Graphite monochromatorθmax = 28.0°, θmin = 2.6°
ω–2θ scansh = 1818
Absorption correction: ψ scan
(North et al., 1968)
k = 2121
Tmin = 0.674, Tmax = 0.847l = 1313
5355 measured reflections3 standard reflections every 150 reflections
1785 independent reflections intensity decay: 0.2%
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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.153H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0867P)2 + 1.4958P]
where P = (Fo2 + 2Fc2)/3
1785 reflections(Δ/σ)max = 0.001
83 parametersΔρmax = 0.94 e Å3
0 restraintsΔρmin = 0.53 e Å3
Special details top

Experimental. crystal coated in epoxy glue

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
Ni0.33135 (2)0.33135 (2)0.25000.0317 (2)
Mo0.00000.334817 (15)0.25000.0356 (2)
O10.07418 (13)0.43261 (13)0.15839 (17)0.0483 (5)
O20.06951 (12)0.31208 (13)0.36123 (16)0.0431 (4)
N10.40297 (17)0.27074 (17)0.3637 (3)0.0428 (5)
H1C0.39570.27610.45240.051*
H1D0.37820.20790.34360.051*
N20.4603 (2)0.38995 (19)0.1322 (3)0.0493 (6)
H2C0.44580.38130.04420.059*
H2D0.49770.45360.14810.059*
N30.25274 (18)0.20474 (19)0.1309 (3)0.0475 (6)
H3C0.25740.22060.04340.057*
H3D0.27680.16500.14220.057*
C10.5037 (2)0.3249 (3)0.3269 (3)0.0513 (7)
H1A0.53720.28900.35530.062*
H1B0.53690.38680.36910.062*
C20.5113 (2)0.3377 (2)0.1724 (3)0.0460 (6)
H2A0.57850.37420.14560.055*
H2B0.48200.27510.12880.055*
C30.1560 (2)0.1590 (2)0.1721 (3)0.0436 (6)
H3A0.12040.09420.13560.052*
H3B0.12550.19520.14270.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0324 (3)0.0324 (3)0.0306 (4)0.01642 (19)0.00001 (6)0.00001 (6)
Mo0.0365 (2)0.0363 (2)0.0340 (3)0.01827 (12)0.00001 (9)0.00000 (4)
O10.0501 (10)0.0460 (10)0.0460 (9)0.0219 (8)0.0011 (8)0.0002 (7)
O20.0445 (9)0.0446 (9)0.0416 (8)0.0233 (8)0.0011 (7)0.0006 (7)
N10.0439 (12)0.0447 (11)0.0417 (12)0.0235 (10)0.0011 (9)0.0007 (9)
N20.0506 (14)0.0502 (13)0.0481 (14)0.0259 (11)0.0026 (10)0.0013 (10)
N30.0464 (12)0.0460 (13)0.0476 (13)0.0213 (10)0.0018 (10)0.0021 (10)
C10.0492 (15)0.0560 (17)0.0506 (16)0.0277 (13)0.0011 (12)0.0010 (13)
C20.0437 (14)0.0510 (15)0.0450 (15)0.0249 (12)0.0024 (11)0.0003 (12)
C30.0413 (13)0.0421 (13)0.0443 (14)0.0185 (11)0.0019 (11)0.0021 (10)
Geometric parameters (Å, º) top
Ni—N1i2.156 (2)N2—H2C0.9000
Ni—N2i2.140 (3)N2—H2D0.9000
Ni—N32.132 (3)N3—C31.403 (4)
Ni—N3i2.132 (3)N3—H3C0.9000
Ni—N22.140 (3)N3—H3D0.9000
Ni—N12.156 (2)C1—C21.550 (5)
Mo—O1ii1.6832 (18)C1—H1A1.0022
Mo—O11.6832 (18)C1—H1B0.9560
Mo—O2ii1.7326 (17)C2—H2A0.9700
Mo—O21.7326 (17)C2—H2B0.9700
N1—C11.445 (4)C3—C3i1.553 (5)
N1—H1C0.9000C3—H3A0.9700
N1—H1D0.9000C3—H3B0.9700
N2—C21.485 (4)
N3—Ni—N3i79.28 (14)Ni—N2—H2C110.4
N3—Ni—N2i170.85 (11)C2—N2—H2D110.4
N3i—Ni—N2i95.32 (11)Ni—N2—H2D110.4
N3—Ni—N295.32 (11)H2C—N2—H2D108.6
N3i—Ni—N2170.85 (11)C3—N3—Ni107.80 (19)
N2i—Ni—N290.95 (15)C3—N3—H3C110.1
N3—Ni—N1i90.24 (10)Ni—N3—H3C110.1
N3i—Ni—N1i93.36 (11)C3—N3—H3D110.1
N2i—Ni—N1i82.65 (12)Ni—N3—H3D110.1
N2—Ni—N1i94.05 (10)H3C—N3—H3D108.5
N3—Ni—N193.36 (11)N1—C1—C2108.7 (2)
N3i—Ni—N190.24 (10)N1—C1—H1A109.9
N2i—Ni—N194.05 (10)C2—C1—H1A109.1
N2—Ni—N182.65 (12)N1—C1—H1B112.6
N1i—Ni—N1175.32 (13)C2—C1—H1B109.5
O1ii—Mo—O1109.50 (13)H1A—C1—H1B107.0
O1ii—Mo—O2ii108.27 (9)N2—C2—C1108.3 (2)
O1—Mo—O2ii107.42 (8)N2—C2—H2A110.0
O1ii—Mo—O2107.42 (8)C1—C2—H2A110.0
O1—Mo—O2108.27 (9)N2—C2—H2B110.0
O2ii—Mo—O2115.85 (11)C1—C2—H2B110.0
C1—N1—Ni106.35 (19)H2A—C2—H2B108.4
C1—N1—H1C110.5N3—C3—C3i105.4 (2)
Ni—N1—H1C110.5N3—C3—H3A110.7
C1—N1—H1D110.5C3i—C3—H3A110.7
Ni—N1—H1D110.5N3—C3—H3B110.7
H1C—N1—H1D108.7C3i—C3—H3B110.7
C2—N2—Ni106.63 (18)H3A—C3—H3B108.8
C2—N2—H2C110.4
N3—Ni—N1—C1112.3 (2)N3i—Ni—N3—C318.12 (14)
N3i—Ni—N1—C1168.41 (18)N2i—Ni—N3—C336.3 (6)
N2i—Ni—N1—C173.1 (2)N2—Ni—N3—C3169.35 (19)
N2—Ni—N1—C117.38 (17)N1i—Ni—N3—C375.3 (2)
N1i—Ni—N1—C128.01 (18)N1—Ni—N3—C3107.7 (2)
N3—Ni—N2—C279.0 (2)Ni—N1—C1—C244.5 (3)
N3i—Ni—N2—C225.6 (6)Ni—N2—C2—C141.0 (3)
N2i—Ni—N2—C2107.7 (2)N1—C1—C2—N259.5 (4)
N1i—Ni—N2—C2169.60 (18)Ni—N3—C3—C3i47.5 (3)
N1—Ni—N2—C213.74 (17)
Symmetry codes: (i) y, x, z+1/2; (ii) x, x+y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O2iii0.902.193.028 (3)154
N2—H2C···O1iv0.902.042.934 (3)170
N2—H2D···O1v0.902.643.510 (3)164
N3—H3C···O2vi0.902.423.236 (3)152
N3—H3D···O2i0.901.882.765 (3)169
Symmetry codes: (i) y, x, z+1/2; (iii) y, x+y, z+1; (iv) y, x+y, z; (v) y+1, xy+1, z; (vi) x+y, y, z1/2.
 

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