Limits...
Crystal structure of trans-(1,8-dibutyl-1,3,6,8,10,13-hexa-aza-cyclo-tetra-decane-κ(4) N (3),N (6),N (10),N (13))bis-(thio-cyanato-κN)nickel(II) from synchrotron data.

Kim DW, Kim JJ, Shin JW, Kim JH, Moon D - Acta Crystallogr E Crystallogr Commun (2015)

Bottom Line: Only half of the macrocyclic ligand N-H groups are involved in hydrogen bonding.The complex mol-ecules are connected via inter-molecular N-H⋯S hydrogen bonds into two symmetry-independent one-dimensional polymeric structures extending along the b-axis direction.One of the n-butyl substituents of the macrocycle exhibits conformational disorder with a refined occupancy ratio of 0.630:0.370.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University, Daegu, 702-701, Republic of Korea.

ABSTRACT
The crystal structure of the title compound, [Ni(NCS)2(C16H38N6)], has been determined from synchrotron data. The asymmetric unit consists of two halves of the complex mol-ecules which have their Ni(II) atoms located on inversion centres. The Ni(II) ions show a tetra-gonally distorted octa-hedral coordination geometry, with four secondary amine N atoms of the aza-macrocyclic ligand in the equatorial plane and two N atoms of the thio-cyanate anions in the axial positions. The average equatorial Ni-N bond length [2.070 (5) Å] is shorter than the average axial Ni-N bond length [2.107 (18) Å]. Only half of the macrocyclic ligand N-H groups are involved in hydrogen bonding. The complex mol-ecules are connected via inter-molecular N-H⋯S hydrogen bonds into two symmetry-independent one-dimensional polymeric structures extending along the b-axis direction. One of the n-butyl substituents of the macrocycle exhibits conformational disorder with a refined occupancy ratio of 0.630:0.370.

No MeSH data available.


Related in: MedlinePlus

View of the mol­ecular structure of the title compound, showing the atom-labelling scheme, with displacement ellipsoids drawn at the 30% probability level. H atoms have been omitted for clarity. The minor position of the n-butyl substituent in the A mol­ecule is not shown.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
getmorefigures.php?uid=PMC4518977&req=5

fig1: View of the mol­ecular structure of the title compound, showing the atom-labelling scheme, with displacement ellipsoids drawn at the 30% probability level. H atoms have been omitted for clarity. The minor position of the n-butyl substituent in the A mol­ecule is not shown.

Mentions: The title compound (I) contains two crystallographically independent complex mol­ecules that are centrosymmetric. Each NiII ion lies on an inversion centre and is coordinated by four secondary amine N atoms of the aza­macrocyclic ligand in a square-planar fashion in the equatorial plane, and by two N atoms from the thio­cyanate anions at the axial positions, resulting in a tetra­gonally distorted octa­hedral geometry, as shown in Fig. 1 ▸. The average equatorial bond lengths, Ni1A—Neq and Ni1B—Neq, are 2.070 (8) and 2.070 (3) Å, respectively. The axial bond lengths, Ni1A—Nax and Ni1B—Nax are 2.119 (1) and 2.093 (1) Å, respectively. The axial bonds are longer than the equatorial bonds, which can be attributed either to a large Jahn–Teller distortion effect of the NiII ion and/or to a ring contraction of the aza­macrocyclic ligand (Halcrow, 2013 ▸; Kim et al., 2015 ▸). The average N—C and C—S bond lengths of the thiocyanate ligands are 1.157 (1) and 1.627 (11) Å, respectively. The former is very similar to a C N triple-bond length, while the latter is slightly shorter than reported C—S single-bond lengths (Bradforth et al., 1993 ▸; Shin et al., 2010 ▸). The six-membered chelate rings involving C2A, C3A and C2B, C3B atoms adopt a chair conformation, whereas the five-membered chelate rings involving C1A, C4A and C1B, C4B assume a gauche conformation (Min & Suh, 2001 ▸; Kim et al., 2015 ▸).


Crystal structure of trans-(1,8-dibutyl-1,3,6,8,10,13-hexa-aza-cyclo-tetra-decane-κ(4) N (3),N (6),N (10),N (13))bis-(thio-cyanato-κN)nickel(II) from synchrotron data.

Kim DW, Kim JJ, Shin JW, Kim JH, Moon D - Acta Crystallogr E Crystallogr Commun (2015)

View of the mol­ecular structure of the title compound, showing the atom-labelling scheme, with displacement ellipsoids drawn at the 30% probability level. H atoms have been omitted for clarity. The minor position of the n-butyl substituent in the A mol­ecule is not shown.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4518977&req=5

fig1: View of the mol­ecular structure of the title compound, showing the atom-labelling scheme, with displacement ellipsoids drawn at the 30% probability level. H atoms have been omitted for clarity. The minor position of the n-butyl substituent in the A mol­ecule is not shown.
Mentions: The title compound (I) contains two crystallographically independent complex mol­ecules that are centrosymmetric. Each NiII ion lies on an inversion centre and is coordinated by four secondary amine N atoms of the aza­macrocyclic ligand in a square-planar fashion in the equatorial plane, and by two N atoms from the thio­cyanate anions at the axial positions, resulting in a tetra­gonally distorted octa­hedral geometry, as shown in Fig. 1 ▸. The average equatorial bond lengths, Ni1A—Neq and Ni1B—Neq, are 2.070 (8) and 2.070 (3) Å, respectively. The axial bond lengths, Ni1A—Nax and Ni1B—Nax are 2.119 (1) and 2.093 (1) Å, respectively. The axial bonds are longer than the equatorial bonds, which can be attributed either to a large Jahn–Teller distortion effect of the NiII ion and/or to a ring contraction of the aza­macrocyclic ligand (Halcrow, 2013 ▸; Kim et al., 2015 ▸). The average N—C and C—S bond lengths of the thiocyanate ligands are 1.157 (1) and 1.627 (11) Å, respectively. The former is very similar to a C N triple-bond length, while the latter is slightly shorter than reported C—S single-bond lengths (Bradforth et al., 1993 ▸; Shin et al., 2010 ▸). The six-membered chelate rings involving C2A, C3A and C2B, C3B atoms adopt a chair conformation, whereas the five-membered chelate rings involving C1A, C4A and C1B, C4B assume a gauche conformation (Min & Suh, 2001 ▸; Kim et al., 2015 ▸).

Bottom Line: Only half of the macrocyclic ligand N-H groups are involved in hydrogen bonding.The complex mol-ecules are connected via inter-molecular N-H⋯S hydrogen bonds into two symmetry-independent one-dimensional polymeric structures extending along the b-axis direction.One of the n-butyl substituents of the macrocycle exhibits conformational disorder with a refined occupancy ratio of 0.630:0.370.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University, Daegu, 702-701, Republic of Korea.

ABSTRACT
The crystal structure of the title compound, [Ni(NCS)2(C16H38N6)], has been determined from synchrotron data. The asymmetric unit consists of two halves of the complex mol-ecules which have their Ni(II) atoms located on inversion centres. The Ni(II) ions show a tetra-gonally distorted octa-hedral coordination geometry, with four secondary amine N atoms of the aza-macrocyclic ligand in the equatorial plane and two N atoms of the thio-cyanate anions in the axial positions. The average equatorial Ni-N bond length [2.070 (5) Å] is shorter than the average axial Ni-N bond length [2.107 (18) Å]. Only half of the macrocyclic ligand N-H groups are involved in hydrogen bonding. The complex mol-ecules are connected via inter-molecular N-H⋯S hydrogen bonds into two symmetry-independent one-dimensional polymeric structures extending along the b-axis direction. One of the n-butyl substituents of the macrocycle exhibits conformational disorder with a refined occupancy ratio of 0.630:0.370.

No MeSH data available.


Related in: MedlinePlus