The synthesis, X-ray structure, and substitution lability of chloro(2,3,7,8,12,13,17,18-octaethylporphinato)(triphenylphosphine)rhodium(III)

1986 ◽  
Vol 64 (12) ◽  
pp. 2440-2446 ◽  
Author(s):  
David C. Thackray ◽  
Sara Ariel ◽  
Tak W. Leung ◽  
Kusum Menon ◽  
Brian R. James ◽  
...  
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Thermodynamic Data ◽  
Crystal Data ◽  
X Ray ◽  
Thermal Reactions ◽  
Photochemical Processes ◽  
Rhodium Atom ◽  
Ring Nitrogen ◽  
The Mean

The rhodium(III) octaethylporphyrin complex Rh(OEP)(PPh3)Cl (1) has been synthesized via Rh(III) or Rh(I) precursors, and fully characterized both by spectroscopy and single crystal data. The crystals, available as a bis(chloroform) solvate are triclinic, P1, a = 13.478(5), b = 14.300(5), c = 15.346(4) Å, α = 102.33(2), β = 102.89(2), γ = 90.56(3)°, Z = 2, Dx = 1.384 g cm−3. The structure was determined from Mo diffractometer data and refined by least-squares methods to R = 0.095, Rw = 0.068 for 5189 reflections. The octahedrally coordinated rhodium atom is displaced by 0.077 Å from the mean plane of the four N atoms, towards the triphenylphosphine group. The average Rh – ring nitrogen distance is 2.024 Å, Rh—P is 2.306(3) Å and Rh—Cl, 2.442(2) Å. Solution equilibria studies on 1 describe formation of Rh(OEP)L2+ (L = PPh3, PnBu3) via thermal reactions (including thermodynamic data for the PPh3 system), and formation of Rh(OEP)Cl(L′) species (L′ = CO, THF, MeCN) via photochemical processes.

Crystal structure of Hydroxyimino(N,N'-dimethyl)malonamide

1977 ◽  
Vol 30 (9) ◽  
pp. 1929 ◽  
Author(s):  
SR Hall ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Direct Methods ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Independent Molecules

The crystal structure of the title compound, namely hydroxyimino(N,N?- dimethyl)malonamide (MeNHCOC(=NOH)CONHMe), has been determined by single-crystal X-ray diffraction with diffractometer data at 295 K. The structure was solved by direct methods and refined by least squares to a residual of 0.055 for 1477 observed reflections. ��� Crystal data: monoclinic, P21/n, a 15.508(3), b 10.544(2), c 9.377(1) Ǻ, β 103.15(2)�, Z 8. ��� The two crystallographically independent molecules exhibit little conjugation throughout the C-C-C skeleton (<C-C> 1.50 Ǻ), the molecule being non-planar. <C=O> is 1.234, <N-CH3> 1.443, <OC-N> 1.323, <C-NO> 1.278 and (N-O) 1.375 Ǻ. The geometry is compared with those observed for several related derivatives.

Hereroite and vladkrivovichevite: two novel lead oxychlorides from the Kombat mine, Namibia

2012 ◽  
Vol 76 (4) ◽  
pp. 883-890 ◽  
Author(s):  
R. Turner ◽  
O. I. Siidra ◽  
M. S. Rumsey ◽  
S. V. Krivovichev ◽  
C. J. Stanley ◽  
...  
Keyword(s):  
Single Crystal ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Crystal Data ◽  
Powder Diffraction Data ◽  
Calculated Density ◽  
X Ray ◽  
Conchoidal Fracture ◽  
The Mean

AbstractTwo new lead oxychloride minerals, hereroite [Pb32(O, ☐)21](AsO4)2((Si,As,V,Mo)O4)2Cl10 and vladkrivovichevite [Pb32O18][Pb4Mn2O]Cl14(BO3)8·2H2O occur in association with asisite, damaraite, kombatite, sahlinite, copper, quartz, barysilite, Mn silicates and a number of Mn oxyhydroxide minerals on a specimen from the Kombat mine in Namibia. The minerals formed as late-stage products of hydrothermal reworking of primary sulfide minerals.Hereroite is monoclinic, C2/c with a = 23.14(1), b = 22.65(1), c = 12.39(1) Å, β = 102.00(5)°, V = 6351.6(41) Å3 from powder-diffraction data and a = 23.139(4), b = 22.684(4), c = 12.389(2) Å, β = 102.090(3)°, V = 6358.8(18) Å3 from single-crystal data. It is bright orange, with white streak and adamantine lustre. It is brittle with no observed parting or cleavage and has a conchoidal fracture. The calculated density is 8.15 g cm–3. The mean refractive index in air at 589 nm is 2.38. The six strongest reflections in the X-ray powder diffraction pattern [d in Å, (I), (hkl)] are as follows: 2.982(100)(51); 2.795(47)(80); 1.986(24)(8); 1.641(24)(11..); 3.512(23)(61); 3.901(21)(511). Hereroite is named for the Herero people, one of the indigenous tribal groupings in the region where the Kombat mine is located.Vladkrivovichevite is orthorhombic, Pmmn with a = 12.87(5), b = 27.7(4), c = 11.46(3) Å, V = 4080.1(5) Å3, from powder-diffraction data and a = 12.759(1), b = 27.169(4), c = 11.515(1) Å, V = 3992.0(9) Å3, Z = 2, from single-crystal data. It is pale greenish yellow, with white streak and adamantine lustre. It is brittle with no observed parting or cleavage and has a conchoidal fracture. The calculated density is 7.40 g cm–3. The mean refractive indices in air at 589 nm are 2.30 and 2.34. The six strongest reflections in the X-ray powder diffraction pattern [d in Å, (I), (hkl)] are as follows: 2.860(100)(370); 2.733(84)(073); 3.707(49)(073); 3.068(37)(401); 2.075(32)(473); 1.601(32)(3.14.3). Vladkrivovichevite is named in honour of Prof. Dr Vladimir Gerasimovich Krivovichev (b. 24.04.1946), Head of the Department of Mineralogy, Geological Faculty, St Petersburg State University.The crystal structures of hereroite and vladkrivovichevite consist of alternating litharge-like O – Pb double layers and chlorine sheets and both are structurally related to other layered lead oxychlorides. In hereroite, tetrahedral AsO4 and (Si, As, V, Mo)O4 groups locate in defects within the O – Pb block, which combines square 'symesite-type' and double-square 'kombatite-type' cavities in its crystal structure. The structure of vladkrivovichevite is based on O – Pb derivative blocks with the interlayer occupied by Cl– anions and oxocentred OPb4Mn2 octahedra whose eight triangular faces are capped by triangular borate anions, BO33–.

Crystal structures of rac- and meso-o-Phenylenebis(iodomethylarsine), the latter as its lattice complex with the methiodide of 1,3-Dimethyl-1,3-dihydro-2,1,3-benzoxadiarsole

1977 ◽  
Vol 30 (11) ◽  
pp. 2417 ◽  
Author(s):  
K Henrick ◽  
CL Raston ◽  
AH White ◽  
SB Wild
Keyword(s):  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Iodine Species ◽  
Iodide Anion ◽  
The Mean

The crystal structures of the title compounds, o-C6H4(AsMeI)2 (1), and o- C6H4(AsMeI)2- [o-C6H4(AsMe)(As+Me2)O] I- (2), have been determined at 295 K by single-crystal X-ray diffraction and refined by least squares to residuals of 0.037 and 0.067 for 2095 and 2913 reflections respectively. Crystals of (1) are triclinic, Pī, a 9.865(5), b 9.837(7), c 7.765(4) Ǻ, α 98.89(5), β 96.71(4), γ 60.72(4)�, Z 2. <As- I> is 2.585 Ǻ and <As-C> 1.97 Ǻ. The angles about the arsenic differ only trivially, the mean being 98.4�. Crystals of (2) are monoclinic, P21/n, a 15.315(4), b 21.511(8), c 7.952(2) Ǻ, β 98.19(2)�, Z 4. In the cation As-O distances are unequal [1.75(1) (quaternary As), 1.86(2) Ǻ]; As-O-As is very small being 115.8(8)�. Charge-transfer interactions between iodine species are present in both derivatives; in (2), there is an interaction between the tertiary arsenics of the meso molecule and the iodide anion, As...I being 3.307(3), 3.551(3) Ǻ, with the geometry of the arsenics approaching that of a tetrahedral disposition. Within the cation, the geometry about the quaternary arsenic is typical of arsenic(v), the bond lengths being shorter than those about the ternary arsenic.

Die Röntgenstrukturanalyse von (CO)9Co3CΟΒΒr2Ν(C5)3. X-ray Structure Analysis of (CO)9Co3COBBr2N(C2H5)3

1976 ◽  
Vol 31 (3) ◽  
pp. 342-344 ◽  
Author(s):  
Volker Bätzel
Keyword(s):  
Least Squares ◽  
Structure Analysis ◽  
Reliability Index ◽  
Three Dimensional ◽  
Diagonal Matrix ◽  
Crystal Data ◽  
Block Diagonal Matrix ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray

Using three dimensional X-ray data collected on a four circle diffractometer, the structure of (CO)9Co3COBBr2N(C2H5)3 was solved by Patterson and Fourier methods. Least squares refinement with a block-diagonal matrix leads to a reliability index of R = 10.7%. Crystal data: α = 13.277(6) Å, b = 10.17(1) Å, c = 9.22(2) Å; α = 91.12(6)°, β = 87.61(4)°, γ = 98.79(2)°; space group P1̅; Z = 2; V = 1229,7 Å3; Dx = 1.97 gcm-3.

scholarly journals Intermetallic REPtZn Compounds with TiNiSi-type Structure

2011 ◽  
Vol 66 (7) ◽  
pp. 671-676 ◽  
Author(s):  
Trinath Mishra ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Coordination Number ◽  
High Frequency ◽  
Three Dimensional ◽  
Type Structure ◽  
Rare Earth Compounds ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray

The equiatomic rare earth compounds REPtZn (RE = Y, Pr, Nd, Gd-Tm) were synthesized from the elements in sealed tantalum tubes by high-frequency melting at 1500 K followed by annealing at 1120 K and quenching. The samples were characterized by powder X-ray diffraction. The structures of four crystals were refined from single-crystal diffractometer data: TiNiSi type, Pnma, a = 707.1(1), b = 430.0(1), c = 812.4(1) pm, wR2 = 0.066, 602 F2, 21 variables for PrPt1.056Zn0.944; a = 695.2(1), b = 419.9(1), c = 804.8(1) pm, wR2 = 0.041, 522 F2, 21 variables for GdPt0.941Zn1.059; a = 688.2(1), b = 408.1(1), c = 812.5(1) pm, wR2 = 0.041, 497 F2, 22 variables for HoPt1.055Zn0.945; a = 686.9(1), b = 407.8(1), c = 810.4(1) pm, wR2 = 0.061, 779 F2, 20 variables for ErPtZn. The single-crystal data indicate small homogeneity ranges REPt1±xZn1±x. The platinum and zinc atoms build up three-dimensional [PtZn] networks (265 - 269 pm Pt-Zn in ErPtZn) in which the erbium atoms fill cages with coordination number 16 (6 Pt + 6 Zn + 4 Er). Bonding of the erbium atoms to the [PtZn] network proceeds via shorter RE-Pt distances, i. e. 288 - 293 pm in ErPtZn.

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

Single-crystal Data of Ternary Germanides RE2Nb3Ge4 (RE = Sc, Y, Gd–Er, Lu) and Sc2Ta3Ge4 with Ordered Sm5Ge4-type Structure

2013 ◽  
Vol 68 (5-6) ◽  
pp. 625-634 ◽  
Author(s):  
Bastian Reker ◽  
Samir F. Matar ◽  
Ute Ch. Rodewald ◽  
Rolf-Dieter Hoffmann ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Coordination Number ◽  
Electronic Structure Calculations ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Arc Melting ◽  
Structure Calculations ◽  
The Rare Earth

Small single crystals of the Sm5Ge4-type (space group Pnma) germanides RE2Nb3Ge4 (RE = Sc, Y, Gd-Er, Lu) and Sc2Ta3Ge4 were synthesized by arc-melting of the respective elements. The samples were characterized by powder and single-crystal X-ray diffraction. In all structures, except for Sc2.04Nb2.96Ge4 and Sc2.19Ta2.81Ge4, the rare earth and niobium atoms show full ordering on the three crystallographically independent samarium sites of the Sm5Ge4 type. Two sites with coordination number 6 are occupied by niobium, while the slightly larger site with coordination number 7 is filled with the rare earth element. Small homogeneity ranges with RE=Nb and RE=Ta mixing can be expected for all compounds. The ordered substitution of two rare earth sites by niobium or tantalum has drastic effects on the coordination number and chemical bonding. This was studied for the pair Y5Ge4/Y2Nb3Ge4. Electronic structure calculations show larger charge transfer from yttrium to germanium for Y5Ge4, contrary to Y2Nb3Ge4 which shows stronger covalent bonding due to the presence of Nb replacing Y at two sites

Crystal structure of ab-Bis(3-methylpyridine)-dc,fe-bis(pentane-2,3,4-trione 3-oximato)iron(II)

1978 ◽  
Vol 31 (11) ◽  
pp. 2431 ◽  
Author(s):  
BN Figgis ◽  
CL Raston ◽  
RP Sharma ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chelate Ligands

The crystal structure of the title compound has been determined at 295 K by single-crystal X-ray diffraction and refined by least squares to a residual of 0.062. Crystals are monoclinic, P2/c, a 19.102(8), b 8.117(4), c 16.610(8) Ǻ, β 111.90(3)°, Z. Unlike the tris(α-oxyimino ketonato)iron(II) complexes which are fac, the present derivative is based upon substitution of the two picoline moieties into a mer derivative, trans to the nitrogen atoms of the chelate ligands. <Fe- N(picoline)> is 2.020; <Fe-N, O(chelate)> 1.880, 1.952 Ǻ.

The Molecular Geometry of Diastereoisomeric Bis[α-(9-anthryl)ethyl] Ethers

1985 ◽  
Vol 38 (9) ◽  
pp. 1417 ◽  
Author(s):  
H Becker ◽  
VA Patrick ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Dihedral Angle ◽  
Molecular Geometry ◽  
Dihedral Angles ◽  
Methyl Groups ◽  
X Ray Diffraction ◽  
X Ray ◽  
Meso Form ◽  
Aromatic Systems

The crystal structures of racemic bis [α-(9-anthryl)] ether and its meso form have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.053 and 0.041 for 1868 and 3568 independent 'observed' reflections respectively. Crystals of the racemate are orthorhombic, Pcab, a 23.07(1), b 19.85(2), c 10.241(8) Ǻ, Z 8. Crystals of the meso form are triclinic, Pī , a 19.032(12), b 14.207(11), c 9.451(8) Ǻ, α 79.46(6), β 89.68(6), γ 68.97(5)°, Z 4. In the racemate , the dihedral angle between the methyl groups along the ether bonds is 12°, and the short axes of the anthracene moieties lie at an angle of about 120°. In the meso compound, for the two molecules the dihedral angles between the methyl groups along the ether bonds are 90 and 93°, the angle between the two anthracene moieties is 90°, and the interplanar angles between the partly overlapping aromatic systems are 46 and 43°.

Redetermination of Co4Nb2O9 by single-crystal X-ray methods

2006 ◽  
Vol 62 (5) ◽  
pp. i117-i119 ◽  
Author(s):  
María A. Castellanos R. ◽  
Sylvain Bernès ◽  
Marina Vega-González
Keyword(s):  
Single Crystal ◽  
High Precision ◽  
Cation Distribution ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Ray Methods

A high-precision structure of tetracobalt diniobium nonaoxide, Co4Nb2O9, is presented, based on X-ray single-crystal data. The space group and cation distribution previously obtained from powder data [Bertaut, Corliss, Forrat, Aleonard & Pauthenet (1961). J. Phys. Chem. Solids, 21, 234–251] are confirmed.

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