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The crystal structure of [Cd(NH3)3Ni(CN)4] has been solved and refined as an incommensurate structure in four-dimensional superspace. The Xcalibur point-detector diffractometer was used for data collection up to the third-order satellites. The structure was refined from 3496 observed reflections to a final R value of 0.0371. The modulation strongly affects all the atoms of the structure. The dominating feature of the modulation is the incommensurate alternation between octahedrally and tetrahedrally coordinated Cd atoms in the electroneutral chains [—Cd(NH3)n—NC—Ni(CN)2—CN—] (n alternates between 2 and 4). The chain is propagated along the a axis, in which the [Cd(NH3)n]2+ cations are linked by square [Ni(CN)4]2− anions. The atomic positional modulations, having mainly a transversal character in the c-direction, exhibit a switching character that can be described by the crenel and sawtooth functions. The effectively pentagonal coordinated cadmium positions were detected in the intermediate regions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105012632/sn5017sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768105012632/sn5017sup2.hkl
Supplementary material

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768105012632/sn5017sup3.pdf
Supplementary material

Computing details top

Data reduction: (Jana2000; Petricek and Dusek, 2000); program(s) used to solve structure: IR97 (Altomare et al., 1997); program(s) used to refine structure: Jana2000 (Petricek and Dusek, 2000); software used to prepare material for publication: (Jana2000; Petricek and Dusek, 2000).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(I) top
Crystal data top
C4H9CdN7NiO0F(000) = 620
Mr = 326.3Dx = 2.105 Mg m3
Monoclinic, C2/c(α0γ)0sMo Kα radiation, λ = 0.71069 Å
q = 0.43650a* + 0.13070c*Cell parameters from 30 reflections
a = 8.4867 (14) Åθ = 9.1–16.3°
b = 15.951 (3) ŵ = 3.86 mm1
c = 7.604 (3) ÅT = 260 K
β = 90.48 (2)°Irregular, gold-yellow
V = 1029.3 (4) Å30.35 × 0.09 × 0.07 mm
Z = 4
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, 1/2−x3, 1/2−x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, 1/2+x3, 1/2+x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, 1/2−x3, 1/2−x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, 1/2+x3, 1/2+x4.

Data collection top
Oxford Diffraction point detector
diffractometer
Rint = 0.086
θ/2θ scansθmax = 27.1°, θmin = 1.5°
Absorption correction: gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
h = 012
Tmin = 0.660, Tmax = 0.807k = 2020
15484 measured reflectionsl = 1010
7894 independent reflections3 standard reflections every 100 reflections
3496 reflections with I > 3σ(I) intensity decay: 1.4%
Refinement top
Refinement on FRestrained
R[F2 > 2σ(F2)] = 0.037Weighting scheme based on measured s.u.'s w = 1/[σ2(F) + 0.0001F2]
wR(F2) = 0.043(Δ/σ)max < 0.001
S = 1.78Δρmax = 0.95 e Å3
3496 reflectionsΔρmin = 0.99 e Å3
275 parameters
Crystal data top
C4H9CdN7NiO0β = 90.48 (2)°
Mr = 326.3V = 1029.3 (4) Å3
Monoclinic, C2/c(α0γ)0sZ = 4
q = 0.43650a* + 0.13070c*Mo Kα radiation
a = 8.4867 (14) ŵ = 3.86 mm1
b = 15.951 (3) ÅT = 260 K
c = 7.604 (3) Å0.35 × 0.09 × 0.07 mm
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, 1/2−x3, 1/2−x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, 1/2+x3, 1/2+x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, 1/2−x3, 1/2−x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, 1/2+x3, 1/2+x4.

Data collection top
Oxford Diffraction point detector
diffractometer
3496 reflections with I > 3σ(I)
Absorption correction: gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
Rint = 0.086
Tmin = 0.660, Tmax = 0.8073 standard reflections every 100 reflections
15484 measured reflections intensity decay: 1.4%
7894 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037275 parameters
wR(F2) = 0.043Restrained
S = 1.78Δρmax = 0.95 e Å3
3496 reflectionsΔρmin = 0.99 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cd110.20155 (4)0.250.0247 (2)
Cd210.14519 (4)0.250.0367 (2)
Ni0.50.01073 (3)0.250.02530 (17)
C10.6550 (4)0.07102 (18)0.2481 (4)0.0282 (9)
N10.7525 (3)0.12053 (17)0.2469 (4)0.0371 (9)
C20.6550 (4)0.09278 (19)0.2478 (4)0.0311 (10)
N20.7485 (4)0.1440 (2)0.2471 (4)0.0455 (11)
N40.9962 (6)0.0300 (3)0.4583 (7)0.0480 (16)
N30.9982 (4)0.23658 (17)0.0019 (4)0.0381 (9)
H310.921 (4)0.209 (3)0.036 (7)0.149 (16)*
H321.081 (4)0.217 (3)0.046 (7)0.149 (16)*
H330.987 (7)0.2854 (14)0.032 (7)0.149 (16)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0283 (6)0.0237 (3)0.0221 (3)00.0006 (3)0
Cd20.0253 (3)0.0415 (4)0.0434 (4)00.0008 (2)0
Ni0.0195 (3)0.0215 (3)0.0350 (3)00.0007 (2)0
C10.0249 (14)0.0247 (15)0.0350 (17)0.0026 (12)0.0009 (13)0.0001 (12)
N10.0316 (14)0.0337 (16)0.0461 (18)0.0038 (12)0.0002 (12)0.0000 (12)
C20.0272 (17)0.0325 (17)0.0337 (18)0.0003 (13)0.0004 (13)0.0006 (12)
N20.0404 (17)0.045 (2)0.0507 (19)0.0115 (15)0.0001 (14)0.0012 (15)
N40.050 (3)0.047 (2)0.047 (3)0.0017 (19)0.001 (2)0.0165 (19)
N30.0392 (17)0.0393 (15)0.0358 (16)0.0007 (12)0.0003 (13)0.0026 (12)
Geometric parameters (Å, º) top
AverageMinimumMaximum
Cd1—N12.28 (3)2.23 (3)2.38 (2)
Cd1—N32.187 (19)2.046 (19)2.25 (2)
Cd1—N2i3.03 (3)2.70 (3)3.33 (3)
Cd2—N12.39 (2)2.249 (15)2.470 (17)
Cd2—N32.305 (18)2.222 (17)2.516 (17)
Cd2—N42.40 (2)2.320 (18)2.596 (18)
Ni—C11.85 (2)1.78 (3)1.89 (3)
Ni—C21.865 (19)1.687 (19)2.065 (19)
N1—C11.15 (3)1.12 (2)1.18 (4)
N2—C21.15 (3)1.11 (3)1.20 (3)
N3—N2ii3.22 (2)3.11 (2)3.38 (2)
N3—N2iii3.22 (2)3.11 (2)3.38 (2)
N1—Cd1—N1iv101.6 (12)99.7 (15)102.8 (12)
N1—Cd1—N398.6 (9)95.0 (8)102.3 (10)
N1—Cd1—N3iv99.4 (9)92.1 (7)106.0 (11)
N1—Cd1—N2i170.6 (11)162.9 (8)174.6 (10)
N1—Cd1—N2v87.5 (7)80.4 (6)93.4 (9)
N3—Cd1—N3iv150.3 (14)148.8 (13)152.6 (19)
N3—Cd1—N2i79.0 (8)75.4 (7)82.3 (8)
N3—Cd1—N2v79.4 (8)76.7 (7)81.6 (8)
N2i—Cd1—N2v83.4 (8)83.1 (7)83.7 (10)
N1—Cd2—N1iv165.1 (10)155.0 (10)172.7 (12)
N1—Cd2—N393.7 (7)91.4 (7)96.1 (9)
N1—Cd2—N3iv95.2 (7)85.7 (6)109.0 (9)
N1—Cd2—N485.5 (9)78.4 (7)88.3 (9)
N1—Cd2—N4iv85.3 (8)82.7 (8)86.8 (8)
N3—Cd2—N3iv100.6 (8)95.4 (10)109.5 (7)
N3—Cd2—N4169.3 (8)152.7 (7)175.6 (11)
N3—Cd2—N4iv90.2 (7)82.5 (5)96.0 (6)
N4—Cd2—N4iv83.0 (10)77.8 (8)86.4 (12)
Cd1—N1—C1175 (2)167.9 (14)178 (2)
Cd2—N1—C1140.8 (18)135.9 (14)145.4 (14)
Ni—C1—N1178 (2)177 (2)179.4 (17)
Cd1vi—N2—C298.9 (14)90.3 (13)108.9 (14)
Ni—C2—N2176.1 (18)168.5 (17)179.9 (18)
Symmetry codes: (i) x1+1/2, x2+1/2, x3, x4; (ii) x1+2, x2, x3, x4; (iii) x1, x2, x31/2, x1/2; (iv) x1+2, x2, x3+1/2, x1/2; (v) x1+3/2, x2+1/2, x3+1/2, x1/2; (vi) x11/2, x21/2, x3, x4.

Experimental details

Crystal data
Chemical formulaC4H9CdN7NiO0
Mr326.3
Crystal system, space groupMonoclinic, C2/c(α0γ)0s
Temperature (K)260
Wave vectorsq = 0.43650a* + 0.13070c*
a, b, c (Å)8.4867 (14), 15.951 (3), 7.604 (3)
β (°) 90.48 (2)
V3)1029.3 (4)
Z4
Radiation typeMo Kα
µ (mm1)3.86
Crystal size (mm)0.35 × 0.09 × 0.07
Data collection
DiffractometerOxford Diffraction point detector
Absorption correctionGaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
Tmin, Tmax0.660, 0.807
No. of measured, independent and
observed [I > 3σ(I)] reflections
15484, 7894, 3496
Rint0.086
(sin θ/λ)max1)0.641
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.043, 1.78
No. of reflections3496
No. of parameters275
No. of restraints?
H-atom treatmentRestrained
Δρmax, Δρmin (e Å3)0.95, 0.99

† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, 1/2−x3, 1/2−x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, 1/2+x3, 1/2+x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, 1/2−x3, 1/2−x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, 1/2+x3, 1/2+x4.

Computer programs: (Jana2000; Petricek and Dusek, 2000), IR97 (Altomare et al., 1997), Jana2000 (Petricek and Dusek, 2000).

Selected geometric parameters (Å, º) top
AverageMinimumMaximum
Cd1—N12.28 (3)2.23 (3)2.38 (2)
Cd1—N32.187 (19)2.046 (19)2.25 (2)
Cd1—N2i3.03 (3)2.70 (3)3.33 (3)
Cd2—N12.39 (2)2.249 (15)2.470 (17)
Cd2—N32.305 (18)2.222 (17)2.516 (17)
Cd2—N42.40 (2)2.320 (18)2.596 (18)
Ni—C11.85 (2)1.78 (3)1.89 (3)
Ni—C21.865 (19)1.687 (19)2.065 (19)
N1—C11.15 (3)1.12 (2)1.18 (4)
N2—C21.15 (3)1.11 (3)1.20 (3)
N3—N2ii3.22 (2)3.11 (2)3.38 (2)
N3—N2iii3.22 (2)3.11 (2)3.38 (2)
N1—Cd1—N1iv101.6 (12)99.7 (15)102.8 (12)
N1—Cd1—N398.6 (9)95.0 (8)102.3 (10)
N1—Cd1—N3iv99.4 (9)92.1 (7)106.0 (11)
N1—Cd1—N2i170.6 (11)162.9 (8)174.6 (10)
N1—Cd1—N2v87.5 (7)80.4 (6)93.4 (9)
N3—Cd1—N3iv150.3 (14)148.8 (13)152.6 (19)
N3—Cd1—N2i79.0 (8)75.4 (7)82.3 (8)
N3—Cd1—N2v79.4 (8)76.7 (7)81.6 (8)
N2i—Cd1—N2v83.4 (8)83.1 (7)83.7 (10)
N1—Cd2—N1iv165.1 (10)155.0 (10)172.7 (12)
N1—Cd2—N393.7 (7)91.4 (7)96.1 (9)
N1—Cd2—N3iv95.2 (7)85.7 (6)109.0 (9)
N1—Cd2—N485.5 (9)78.4 (7)88.3 (9)
N1—Cd2—N4iv85.3 (8)82.7 (8)86.8 (8)
N3—Cd2—N3iv100.6 (8)95.4 (10)109.5 (7)
N3—Cd2—N4169.3 (8)152.7 (7)175.6 (11)
N3—Cd2—N4iv90.2 (7)82.5 (5)96.0 (6)
N4—Cd2—N4iv83.0 (10)77.8 (8)86.4 (12)
Cd1—N1—C1175 (2)167.9 (14)178 (2)
Cd2—N1—C1140.8 (18)135.9 (14)145.4 (14)
Ni—C1—N1178 (2)177 (2)179.4 (17)
Cd1vi—N2—C298.9 (14)90.3 (13)108.9 (14)
Ni—C2—N2176.1 (18)168.5 (17)179.9 (18)
Symmetry codes: (i) x1+1/2, x2+1/2, x3, x4; (ii) x1+2, x2, x3, x4; (iii) x1, x2, x31/2, x1/2; (iv) x1+2, x2, x3+1/2, x1/2; (v) x1+3/2, x2+1/2, x3+1/2, x1/2; (vi) x11/2, x21/2, x3, x4.
 

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