Steric Modification of M-P Bond Lengths: Crystal and Molecular-Structures of the Platinum(II) Complexes trans-(PPrI3)2ClnH2-nPtII (N = 0-2)

1986 ◽  
Vol 39 (10) ◽  
pp. 1495 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker ◽  
WA Wickramasinghe
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Room Temperature ◽  
Platinum Complexes ◽  
Molecular Structures ◽  
Crystal And Molecular Structures ◽  
Anionic Ligand ◽  
Trans Bond ◽  
Square Planar ◽  
Ligand Conformation

Crystal structure analyses of the square-planar platinum complexes trans-(PPri3)2ClnH2-nPtII(n = 0-2) (C), (B), (A) are described. Diffraction data were recorded at room temperature with a Picker FACS-1 diffractometer. Convergence R values, for reflection numbers given in parentheses, are 0.020 (2373), (A), 0.021 (5771), (B) and 0.018 (1982), (C). The ligand conformation about the Pt-P bonds is perpendicular for (A) and (B) and eclipsed for (C). The Pt-P distances decrease systematically with increasing hydride content [2.339(1)Ǻ, (A); 2.286(1)Ǻ, (B); 2.252(1)Ǻ, (C)]. The decrease reflects the low steric requirement of hydride vis a vis chloride ligands and concomitant changes in anionic ligand/phosphine substituent non-bonding interactions. The trans-bond lengthening of the Pt- Cl bond in (B)(due to trans hydride) is 0.092(1)Ǻ.

scholarly journals Preparation and Crystal Structure of a Platinum(II) Complex of [CH2N(CH2COOH)CH2CONH2]2, the Hydrolysis Product of an Anti-Tumour Bis(3,5-Dioxopiperazin-1-YL)Alkane

1994 ◽  
Vol 1 (4) ◽  
pp. 321-328 ◽  
Author(s):  
Kevin B. Nolan ◽  
Leo P. Ryan ◽  
Colm J. Campbell ◽  
Patrick McArdle ◽  
Desmond Cunningham ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Hydrolysis Product ◽  
Molecular Structures ◽  
3 Dimensional ◽  
Crystal And Molecular Structures ◽  
Dimensional Network ◽  
Square Planar ◽  
Ligand Bond ◽  
Hydrogen Bonded

The synthesis and crystal and molecular structures of the platinum(II) complex Pt(HL)Cl where H2L is the diacid diamide –[CH2N(CH2COOH)CH2CONH2]2, a hydrolytic metabolite of an antitumour active bis(3,5-dioxopiperazin-1-yl)alkane are reported. The complex is square planar and contains HL− as a tridentate 2N (amino), O (carboxylate) donor. The metal to ligand bond distances are Pt-Cl 2.287(1) Å, Pt-O 2.002 (1) Å, Pt-Ntrans Cl 2.014(1) Å and Pt-Ntrans O 2.073 Å. There is extensive hydrogen bonding, each molecule of Pt(HL)Cl being intermolecularly hydrogen bonded to ten others giving a 3-dimensional network. There is also one intramolecular H-bond.

Purine complexes of platinum: synthesis, nmr, and crystal and molecular structures of cis-chloro(caffeine)bis(triethylphosphine)platinum(II) fluoroborate and cis-bis(isocaffeine)bis(triethylphosphine)platinum (II) fluoroborate

1983 ◽  
Vol 61 (6) ◽  
pp. 1132-1141 ◽  
Author(s):  
Gordon William Bushnell ◽  
Roderick James Densmore ◽  
Keith Roger Dixon ◽  
Arthur Charles Ralfs
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Molecular Structures ◽  
Platinum Drugs ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Antitumour Agents ◽  
Crystal And Molecular Structures ◽  
Square Planar

Synthesis and 31P nmr spectra of the complex cations, cis-[PtCl(L)(PEt3)2]+, L= theophylline, caffeine, or isocaffeine, and cis[Pt(isocaff)2(PEt3)2]2+ are reported. The crystal structure of cis-[PtCl(caffeine)(PEt3)2][BF4] is determined, space group [Formula: see text], a = 1.1766(6), b = 1.4428(5), c = 0.9002(4) nm, α = 97.28(4)°, β = 97.69(4)°, γ = 100.96(5)°, Dm = 1.649 g cm−1, the bond lengths are Pt—Cl= 233.4(4) pm, Pt—N = 215(1) pm, Pt—P = 225.4(5) pm (mean), and the residual R = 0.071. The crystal structure of cis-[Pt(isocaffeine)2(PEt3)2][BF4]2 is orthorhombic, space group Pbca, a = 2.317(3), b = 1.717(3), c = 2.130(3) nm, Dm = 1.574 g cm−3, with an opposing isocaffeine conformation, bond lengths Pt—N = 211(2) pm, Pt—P = 227.6(9) pm (mean), and R = 0.073. Both crystal structures contain approximately square planar Pt(II) coordination with the purine coordinated via an imidazole nitrogen. The structures are discussed as models for the possible involvement of [Formula: see text] chelation of guanine to platinum when platinum drugs act as antitumour agents, but there is no evidence that isocaffeine acts as an [Formula: see text] chelate.

Crystal structure and diffraction data for a polymorph of voglibose (C10H21NO7)

2010 ◽  
Vol 25 (S1) ◽  
pp. S28-S30
Author(s):  
G. Q. Zhang ◽  
G. L. Lv
Keyword(s):  
Crystal Structure ◽  
Simulated Annealing ◽  
Rigid Body ◽  
Rietveld Refinement ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Molecular Structures ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Crystal And Molecular Structures

X-ray powder diffraction data of voglibose are reported, and its crystal and molecular structures were determined by simulated annealing and rigid-body Rietveld refinement methods. Voglibose was found to be crystallized in triclinic symmetry with space group P-1. The lattice parameters were determined to be a=6.1974(6) Å, b=6.9918(5) Å, c=7.3955(9) Å, α=70.8628(3), β=103.5312(4), γ=94.3867(5)°, V=294.2(2) Å3, and ρcal=1.495 g/cm3. The crystal structure contains isolated C10H21NO7 molecular.

Cluster chemistry. V. Reactions between [Ru3(CO)11(CNBut)] and [Pt(η-C2H4)(PPh3)2] and related chemistry : Crystal and molecular structures of Di-μ-carbonyl-[μ-carbonyl-bis {(triphenylphosphine)platinum}]dicarbonyl(triphenylphosphine)ruthenium(2Ru-Pt)(Pt-Pt), [RuPt2(CO)5(PPh3)3], and its benzene solvate

1982 ◽  
Vol 35 (4) ◽  
pp. 687 ◽  
Author(s):  
MI Bruce ◽  
JG Matisons ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Cluster Chemistry ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Analogous Compound ◽  
Benzene Solvate ◽  
Unstable Intermediate

The reaction between [Ru3(CO)11(CNBut)] and [Pt(η-C2H4)(PPh3)2] at -30° affords a thermally unstable intermediate complex (A), which decomposes at room temperature affording, inter alia, [Ru2Pt(CO)7(PPhd3)3 (1), [RuPt2(CO)5(PPh3)3] (2), [RuPt2(CO)6(CNBut)(PPh3)] (5) and [Ru2Pt2- (CO)9(CNBut)(PPh3)] (6). The hexanuclear complexes [Ru2Pt4(CO)5-n(CNBut)(PPh3)4+n] [n = 0 (17) and 1 (18)] are obtained, with [Ru2Pt(CO)5(CNBut)(PPh3)4] (16), from reactions at 80°. Related Ru2Pt and RuPt, complexes are obtained from reactions between complex (A) and CO, CNBut, Pme3, P(C6H4Me-p)3, or P(OMe)3; related reactions between [Ru3(CO)11(CNBut)] and [Pt{P(C6H4Me-p)3}4], and between [Ru3(CO)10(CNBut)2] and [Pt(η-C2H4)(PPh3)2, are also described. The crystal structure of [RuPt2(CO)5(PPh3)3] has been determined by single-crystal X-ray diffraction methods at 295(1) K and refined by least squares to a residual of 0.035 for 6774 'observed' reflections. Crystals are triclinic, P 1, a 15.893(5), b 15.400(5), c 12.651(4) Ǻ, α 57.04(2), β 77.09(3), γ 84.10(3)°, Z 2. Crystals of the dibenzene solvate of the complex are monoclinic, P 21/c, a 11.868(4), b 18.647(8), c 29.24(1) A, β 98.35(3)°, Z 4, the structure being refined to a residual of 0.057 for 4530 'observed' reflections. Ligand dispositions are compared in detail with those observed in the analogous compound previously described with the methyldiphenylphosphine Iigand.

N,N′-methylenedipyridinium Pt(II) and Pt(IV) hybrid salts: synthesis, crystal and molecular structures of [(C5H5N)2CH2] · [PtCl4] and [(C5H5N)2CH2] · [PtCl6]

2012 ◽  
Vol 66 (11) ◽  
Author(s):  
Mahmoud Al-Ktaifani ◽  
Mwaffak Rukiah
Keyword(s):  
Crystal Structure ◽  
Molecular Structures ◽  
Planar Geometry ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Ionic Compounds ◽  
Methylene Group

AbstractThe highly insoluble organic-inorganic hybrid ionic compounds N,N′-methylenedipyridinium tetrachloroplatinate(II) [(C5H5N)2CH2] · [PtCl4] and N,N′-methylenedipyridinium hexachloroplatinate(IV) [(C5H5N)2CH2] · [PtCl6] were obtained by the treatment of N,N′-methylenedipyridinium dichloride monohydrate [(C5H5N)2CH2]Cl2 · H2O with K2[PtCl4] or (NH4)2[PtCl6], respectively, in an aqueous solution. Both complexes were isolated, purified, characterised by elemental analysis, and their molecular structures were confirmed by powder X-ray diffraction. The crystal structure of both compounds consists of separated discrete dications [(C5H5N)2CH2]2+ and anions [PtCln]2− (n = 4 or 6). As anticipated, the dications formed a butterfly shape consisting of two pyridine rings bound to the methylene group via their N atoms, while the Pt centre had a square planar geometry in [(C5H5N)2CH2] · [PtCl4] and an octahedral coordination in [(C5H5N)2CH2] · [PtCl6]. Interestingly, both crystal structures are stabilised by intermolecular C-H…Cl non-standard hydrogen bonds, π-π ring interactions between two pyridine rings of adjacent dications, and also by Cl-π interactions.

Synthesis and crystal structure analyses of tri-substituted guanidine-based copper(II) complexes

2021 ◽  
Vol 76 (3-4) ◽  
pp. 193-199
Author(s):  
Muhammad Said ◽  
Sadia Rehman ◽  
Muhammad Ikram ◽  
Hizbullah Khan ◽  
Carola Schulzke
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Molecular Structures ◽  
Hydroxyl Groups ◽  
Synthesis And Crystal Structure ◽  
Pyramidal Geometry ◽  
Tautomeric Forms ◽  
Square Planar ◽  
Nitrogen Donor ◽  
Square Pyramidal Geometry

Abstract Three guanidine-derived tri-substituted ligands viz. N-pivaloyl-N′,N″-bis-(2-methoxyphenyl)guanidine (L1), N-pivaloyl-N′-(2-methoxyphenyl)-N″-phenylguanidine (L2) and N-pivaloyl-N′-(2-methoxyphenyl)-N″-(2-tolyl)guanidine (L3) were reacted with Cu(II) acetate to produce the corresponding complexes. The significance of the substituent on N″ for the resulting molecular structures and their packing in the solid state has been studied with respect to the structural specifics of the corresponding Cu(II) complexes. The key characteristic of the guanidine-based metal complexation with Cu(II) is the formation of an essentially square planar core with an N2O2 donor set. As an exception, in the complex of L1, the substituent’s methoxy moiety also interacts with the Cu(II) center to generate a square-pyramidal geometry. The hydroxyl groups of the imidic acid tautomeric forms of L1–L3, in addition to N″, are also bonded to Cu(II) in all three complexes rather than the nitrogen donor of the guanidine motif.

scholarly journals Comparison of molecular structures of cis-bis[8-(dimethylphosphanyl)quinoline]nickel(II) and -platinum(II) complex cations

2020 ◽  
Vol 76 (12) ◽  
pp. 1813-1817
Author(s):  
Masatoshi Mori ◽  
Takayoshi Suzuki
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Steric Hindrance ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Donor Group ◽  
Bending Deformation ◽  
Bond Lengths ◽  
Square Planar ◽  
Chelate Ligands

The crystal structures of the complexes (SP-4-2)-cis-bis[8-(dimethylphosphanyl)quinoline-κ2 N,P]nickel(II) bis(perchlorate) nitromethane monosolvate, [Ni(C11H12NP)2](ClO4)2·CH3NO2 (1), and (SP-4-2)-cis-bis[8-(dimethylphosphanyl)quinoline-κ2 N,P]platinum(II) bis(tetrafluoroborate) acetonitrile monosolvate, [Pt(C11H12NP)2](BF4)2·C2H3N (2), are reported. In both complex cations, two phosphanylquinolines act as bidentate P,N-donating chelate ligands and form the mutually cis configuration in the square-planar coordination geometry. The strong trans influence of the dimethylphosphanyl donor group is confirmed by the Ni—N bond lengths in 1, 1.970 (2) and 1.982 (2) Å and, the Pt—N bond lengths of 2, 2.123 (4) and 2.132 (4) Å, which are relatively long as compared to those in the analogous 8-(diphenylphosphanyl)quinoline complexes. Mutually cis-positioned quinoline donor groups would give a severe steric hindrance between their ortho-H atoms. In order to reduce such a steric congestion, the NiII complex in 1 shows a tetrahedral distortion of the coordination geometry, as parameterized by τ4 = 0.199 (1)°, while the PtII complex in 2 exhibits a typical square-planar coordination geometry [τ4 = 0.014 (1)°] with a large bending deformation of the ideally planar Me2Pqn chelate planes. In the crystal structure of 2, three F atoms of one of the BF4 − anions are disordered over two sets of positions with refined occupancies of 0.573 (10) and 0.427 (10).

scholarly journals Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

scholarly journals The caesium phosphates Cs3(H1.5PO4)2(H2O)2, Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3

2020 ◽  
Vol 151 (9) ◽  
pp. 1317-1328
Author(s):  
Matthias Weil ◽  
Berthold Stöger
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Single Crystal ◽  
Diffraction Data ◽  
Room Temperature ◽  
Structure Type ◽  
Solid State Reactions ◽  
X Ray Diffraction ◽  
Hydrogen Phosphate ◽  
X Ray

Abstract The caesium phosphates Cs3(H1.5PO4)2(H2O)2 and Cs3(H1.5PO4)2 were obtained from aqueous solutions, and Cs4P2O7(H2O)4 and CsPO3 from solid state reactions, respectively. Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3 were fully structurally characterized for the first time on basis of single-crystal X-ray diffraction data recorded at − 173 °C. Monoclinic Cs3(H1.5PO4)2 (Z = 2, C2/m) represents a new structure type and comprises hydrogen phosphate groups involved in the formation of a strong non-symmetrical hydrogen bond (accompanied by a disordered H atom over a twofold rotation axis) and a very strong symmetric hydrogen bond (with the H atom situated on an inversion centre) with symmetry-related neighbouring anions. Triclinic Cs4P2O7(H2O)4 (Z = 2, P$$\bar{1}$$ 1 ¯ ) crystallizes also in a new structure type and is represented by a diphosphate group with a P–O–P bridging angle of 128.5°. Although H atoms of the water molecules were not modelled, O···O distances point to hydrogen bonds of medium strengths in the crystal structure. CsPO3 is monoclinic (Z = 4, P21/n) and belongs to the family of catena-polyphosphates (MPO3)n with a repetition period of 2. It is isotypic with the room-temperature modification of RbPO3. The crystal structure of Cs3(H1.5PO4)2(H2O)2 was re-evaluated on the basis of single-crystal X-ray diffraction data at − 173 °C, revealing that two adjacent hydrogen phosphate anions are connected by a very strong and non-symmetrical hydrogen bond, in contrast to the previously described symmetrical bonding situation derived from room temperature X-ray diffraction data. In the four title crystal structures, coordination numbers of the caesium cations range from 7 to 12. Graphic abstract

The Crystal and Molecular Structure of Pentane-2,4-dionato-(2,3,5,6-tetrahepto-2,3-dicarbomethoxo[2.2.1]bicycloheptadiene)rhodium(I), Rh(C5H7O2) (C7H6(CO2CH3)2)

1975 ◽  
Vol 53 (18) ◽  
pp. 2707-2713 ◽  
Author(s):  
Debbie Allen ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
John Powell
Keyword(s):  
Crystal And Molecular Structure ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Rhodium Atom

The crystal and molecular structures of pentane-2,4-dionato-(2,3,5,6-tetrahapto-2,3-dicarbomethoxo[2.2.1]bicycloheptadienerhodium(I), Rh(C5H7O2)(C7H6(CO2CH3)2), have been measured by single crystal X-ray diffraction. The orange crystals are monoclinic, space group P21/c, Z = 4, a = 9.245(4), b = 9.003(4), c = 21.680(15) Å, β = 113.41(5)°. The calculated and observed densities are 1.645 and 1.642(5) respectively. Intensity data were collected on a Syntex [Formula: see text] diffractometer and a full matrix least squares refinement on 3010 observed reflections leads to a conventional R = 0.0660. The structure can be considered as a roughly square planar arrangement of ligands around the rhodium atom composed of two β-ketoenolate oxygen atoms (Rh—O, 2.037(5) and 2.025(5) Å ) and the centers of the two ethylenic groups. The Rh—C distances for the olefin group attached to the two carbomethoxo groups, 2.117(8), 2.108(8) Å, appear to be slightly larger than those for the other olefinic group, 2.087(7), 2.082(6), and the corresponding C=C distances of 1.375(10) and 1.410(9) Å are different at the 95% confidence level.

Sign in / Sign up

Export Citation Format

Share Document