Synthesis, Single-crystal Structure and Raman Spectrum of Cu[N(CN)2]2 · 2 NH3

Transparent blue crystals of Cu[N(CN)2]2 · 2 NH3 were obtained by blending solutions of Na[N(CN)2] and Cu(NO3)2 · 2.5 H2O in aqueous ammonia and subsequent evaporation of the solvent under ambient conditions. Cu[N(CN)2]2 · 2 NH3 crystallizes in space group P1̄ (no. 2, Z = 2) with the cell parameters a = 746:1(4), b = 747:8(4) and c = 894:4(5) pm, and the angles α = 68:94(2), β = 75:52(1) and γ = 68:22(4)°. The presence of the dicyanamide anion and the ammonia molecules was verified by Raman spectroscopy.

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Synthesis, single-crystal structure determination and Raman spectrum of Cu[C(CN)3]2·2 NH3

Zeitschrift für Naturforschung B ◽

10.1515/znb-2014-0242 ◽

2015 ◽

Vol 70 (3) ◽

pp. 177-181

Author(s):

Olaf Reckeweg ◽

Armin Schulz ◽

Francis J. DiSalvo

Keyword(s):

Crystal Structure ◽

Raman Spectroscopy ◽

Raman Spectrum ◽

Single Crystals ◽

Structure Determination ◽

Aqueous Ammonia ◽

Ambient Conditions ◽

Light Blue ◽

Cell Parameters ◽

First Time

AbstractTransparent, light blue crystals of Cu[C(CN)3]2·2 NH3 were obtained by dissolving Cu[C(CN)3]2 in aqueous ammonia and subsequent evaporation of the solvent under ambient conditions. Cu[C(CN)3]2·2 NH3 crystallizes in the space group C2/c (no. 15, Z = 4) with the cell parameters a = 1291.9(3), b = 753.18(15) and c = 1200.8(2) pm, and β = 92.68(3)°. The nature of the tricyanomethanide anion and the ammonia molecules were verified by Raman spectroscopy. Single crystals of Ag[C(CN)3] and Cu[C(CN)3]2 were synthesized, the known structures were confirmed and their Raman spectra were recorded for the first time for comparison.

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Synthesis, single-crystal structure determination and Raman spectra of the tricyanomelaminates NaA5[C6N9]2 · 4 H2O (A = Rb, Cs)

Zeitschrift für Naturforschung B ◽

10.1515/znb-2016-0024 ◽

2016 ◽

Vol 71 (4) ◽

pp. 327-332 ◽

Cited By ~ 1

Author(s):

Olaf Reckeweg ◽

Armin Schulz ◽

Francis J. DiSalvo

Keyword(s):

Crystal Structure ◽

Aqueous Solutions ◽

Single Crystal ◽

Raman Spectra ◽

Structure Determination ◽

Single Crystal Structure ◽

Crystal Structure Determination ◽

Ambient Conditions ◽

Space Group ◽

Cell Parameters

AbstractTransparent colorless crystals of NaA5[C6N9]2 · 4 H2O (A = Rb, Cs) were obtained by blending aqueous solutions of Na3[C6N9] and RbF or CsF, respectively, and subsequent evaporation of the water under ambient conditions. Both compounds crystallize in the space group P21/m (no. 11) with the cell parameters a = 815.56(16), b = 1637.7(4) and c = 1036.4(3) pm, and β = 110.738(12)° for NaRb5[C6N9]2 · 4 H2O and a = 843.32(6), b = 1708.47(11) and c = 1052.42(7) pm, and β = 112.034(2)° for NaCs5[C6N9]2 · 4 H2O, respectively. Raman spectra of the title compounds complement our results.

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X-Ray and Raman Investigations on Cyanides ofMono- and DivalentMetals and Synthesis, Crystal Structure and Raman Spectrum of Tl5(CO3)2(CN)

Zeitschrift für Naturforschung B ◽

10.1515/znb-2002-0809 ◽

2002 ◽

Vol 57 (8) ◽

pp. 895-900 ◽

Cited By ~ 11

Author(s):

Olaf Reckeweg ◽

Arndt Simon

Keyword(s):

Crystal Structure ◽

Raman Spectroscopy ◽

Raman Spectrum ◽

Single Crystal ◽

Aqueous Ammonia ◽

Ammonia Solution ◽

Aqueous Ammonia Solution ◽

Divalent Metals ◽

X Ray ◽

First Time

Pseudobinary cyanides of monovalent and divalent metals were synthesized, and X-ray and Raman data of the cyanides were measured. Single crystal X-ray structure analyses were performed on Zn(CN)2 (Pn3̄m (No. 224), a = 591.32(7) pm), Hg(CN)2 (I4̄2d (No. 122), a = 969.22(14) and c = 890,15(18) pm) and for the first time on AgCN (I4̄2d (No. 166), a = 600.58(8) and c = 526.28(11) pm). The data are compared with literature data. The reaction of TlF and NaCN in 25% aqueous ammonia solution in air led to Tl5(CO3)2(CN) which was characterized by X-ray (Cmca (No. 64), 1468.1(3), 1171.6(2) and 1266.0(3) pm) and Raman spectroscopy.

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Synthesis and single-crystal structure of the pseudo-ternary compounds LiA[N(CN)2]2 (A = K or Rb)

Zeitschrift für Naturforschung B ◽

10.1515/znb-2015-0174 ◽

2016 ◽

Vol 71 (2) ◽

pp. 157-160 ◽

Cited By ~ 5

Author(s):

Olaf Reckeweg ◽

Francis J. DiSalvo

Keyword(s):

Crystal Structure ◽

Alkali Metal ◽

Single Crystal ◽

Title Compound ◽

Single Crystal Structure ◽

Rectangular Plates ◽

Atmospheric Conditions ◽

Space Group ◽

Cell Parameters ◽

Ternary Compounds

AbstractCrystals of LiA[N(CN)2]2 were obtained from the reaction of LiCl and ACl (A = K or Rb) with Ag[N(CN)2] in water and subsequent evaporation of the filtered solution at 80 °C under normal atmospheric conditions. Crystals of the title compound form thin rectangular plates that are transparent, colorless, and very fragile. Single-crystal structure analyses have shown that both compounds are isotypic and adopt the tetragonal space group I4/mcm (no. 140, Z = 4) with the cell parameters a = 701.53(12) and c = 1413.7(5) pm for LiK[N(CN)2]2 and a = 730.34(10) and c = 1414.4(4) pm for LiRb[N(CN)2]2. The crystal structure is described and compared to that of the pseudo-binary alkali metal dicyanamides.

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Crystal chemistry of natural layered double hydroxides. 5. Single-crystal structure refinement of hydrotalcite, [Mg6Al2(OH)16](CO3)(H2O)4

Mineralogical Magazine ◽

10.1180/mgm.2018.145 ◽

2018 ◽

Vol 83 (02) ◽

pp. 269-280 ◽

Cited By ~ 7

Author(s):

Elena S. Zhitova ◽

Sergey V. Krivovichev ◽

Igor Pekov ◽

H. Christopher Greenwell

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Crystal Structures ◽

Structure Refinement ◽

Unit Cell ◽

Single Crystal Structure ◽

Unit Cell Parameters ◽

Diagnostic Features ◽

Space Group ◽

Cell Parameters

AbstractHydrotalcite, ideally [Mg6Al2(OH)16](CO3)(H2O)4, was studied in samples from Dypingdal, Snarum, Norway (3R and 2H), Zelentsovskaya pit (2H) and Praskovie–Evgenievskaya pit (2H) (both Southern Urals, Russia), Talnakh, Siberia, Russia (3R), Khibiny, Kola, Russia (3R), and St. Lawrence, New York, USA (3R and 2H). Two polytypes, 3R and 2H (both ‘classical’), were confirmed on the basis of single-crystal and powder X-ray diffraction data. Their chemical composition was studied by electron-microprobe analysis, infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The crystal structure of hydrotalcite-3R was solved by direct methods in the space group R$ {\bar 3} $m on three crystals (two data collections at 290 K and one at 120 K). The unit-cell parameters are as follows (290/290/120 K): a = 3.0728(9)/3.0626(3)/3.0617(4), c = 23.326(9)/23.313(3)/23.203(3) Å and V = 190.7(1)/189.37(4)/188.36(4) Å3. The crystal structures were refined on the basis of 304/150/101 reflections to R1 = 0.075/0.041/0.038. Hydrotalcite-2H crystallises in the P63/mmc space group; unit-cell parameters for two crystals are (data collection at 290 K and 93 K): a = 3.046(1)/3.0521(9), c = 15.447(6)/15.439(4) Å, V = 124.39(8)/124.55(8) Å3. The crystal structures were refined on the basis of 160/142 reflections to R1 = 0.077/0.059. This paper reports the first single-crystal structure data on hydrotalcite. Hydrotalcite distribution in Nature, diagnostic features, polytypism, interlayer topology and localisation of M2+–M3+ cations within metal hydroxide layers are discussed.

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The first pseudo-ternary thiocyanate containing two alkali metals – synthesis and single-crystal structure of LiK2[SCN]3

Zeitschrift für Naturforschung B ◽

10.1515/znb-2015-0175 ◽

2016 ◽

Vol 71 (2) ◽

pp. 161-164 ◽

Cited By ~ 2

Author(s):

Olaf Reckeweg ◽

Francis J. DiSalvo

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Alkali Metals ◽

Single Crystal Structure ◽

Rectangular Plates ◽

X Ray Diffraction ◽

Orthorhombic Space Group ◽

Space Group ◽

X Ray ◽

Cell Parameters

AbstractA procedure was empirically developed to prepare the compound LiK2[SCN]3, which forms colorless, transparent, very fragile, and extremely hygroscopic thin rectangular plates. Its unique crystal structure was determined by single-crystal X-ray diffraction. LiK2[SCN]3 adopts the orthorhombic space group Pna21 (no. 33, Z = 4) with the cell parameters a = 1209.32(9), b = 950.85(9), and c = 849.95(6) pm.

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Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

Zeitschrift für Naturforschung B ◽

10.1515/znb-2014-0250 ◽

2015 ◽

Vol 70 (3) ◽

pp. 191-196 ◽

Cited By ~ 1

Author(s):

Olaf Reckeweg ◽

Francis J. DiSalvo

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Single Crystals ◽

Structure Determination ◽

Monoclinic Space Group ◽

Orthorhombic Space Group ◽

Space Group ◽

Cell Parameters ◽

New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

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Molecular and crystal structure of a copper(II) complex of sildenafil

Zeitschrift für Naturforschung B ◽

10.1515/znb-2021-0145 ◽

2021 ◽

Vol 0 (0) ◽

Author(s):

Akhmatkhodja N. Yunuskhodjayev ◽

Shokhista F. Iskandarova ◽

Vahobjon Kh. Sabirov

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Unit Cell ◽

Monoclinic Space Group ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Piperazine Ring ◽

Space Group ◽

X Ray ◽

Cell Parameters

Abstract The crystal structure of a copper(II) complex of protonated sildenafil, CuCl3C22H31N6O4S⋅2H2O was studied by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n with the unit cell parameters a = 15.4292(2), b = 9.06735(12), c = 21.1752(2) Å, V = 2945.48(7) Å3, Z = 4. The Cu atom is coordinated by the sildenafil ligand via the N2 atom of the pyrazolopyrimidine ring and by three chloride anions. Sildenafil is protonated at the methylated N6 atom of the piperazine ring and it is cation ligand with a 1+ charge.

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