Single crystal X-ray diffractions of bulk NbOCl2 and NbOI2 crystals are measured using a four circles goniometer Kappa geometry, Bruker AXS D8 Venture, equipped with a Photon 100 CMOS active pixel sensor detector. A molybdenum monochromatized (λ = 0.71073 Å) X-Ray radiation is used for the measurement. The frames are integrated with the Bruker SAINT software using a narrow-frame algorithm. Data are corrected for absorption effects using the Multi-Scan method (SADABS). The structures are solved in the monoclinic unit cell and refined using the SHELXT, VERSION 2014/5 Software. The final anisotropic refinement of the structures is performed by least squares procedures on weighted F2 values using the SHELXL-2014/7 (Sheldrick, 2014) included in the APEX3 v2016, 9.0, AXS Bruker program.
Axs d8 venture
Manufactured by Bruker
The Bruker AXS D8 Venture is a single-crystal X-ray diffractometer. It is designed for the analysis of crystalline materials and structures.
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11 protocols using axs d8 venture
1
Single Crystal X-ray Diffraction of NbOCl2 and NbOI2
2
Monoclinic Crystalline Structure Analysis
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C26H22N5OS+Cl–, Mr = 487.99, red plate, 0.038 × 0.164 × 0.293 mm, monoclinic, space group Cc, a = 4.4070(7), b = 27.253(4), c = 22.678(3) Å, β= 94.224(5)°, V = 2716.3(7) Å3, Z = 4, Dc = 1.193 g·cm–3, F(000) = 1016, Bruker AXS D8 VENTURE, MoKα radiation, λ = 0.71073 Å, T = 293(2) K, 2θmax = 55.38°, 32,586 reflections collected, 5911 unique (Rint = 0.081). The structure was solved and refined using the XT, VERSION 2018/2 and SHELXL-2019/1 [50 ] programs, respectively. Final GooF = 1.13, R = 0.105, wR = 0.248, R indices based on 4025 reflections with I > 2σ(I) (refinement on F2), 328 parameters, 0 restraints. Lp and absorption corrections applied, μ = 0.24 mm–1.
3
Inert Synthesis of Organometallic Compounds
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All manipulations were carried out under an argon inert gas atmosphere (argon 5.0), using either Schlenk line techniques or a glovebox. Aluminum trichloride and aluminum tribromide were purchased from Sigma Aldrich and used as received. The other starting materials, Me2C[1]magnesocenophane[12] , lithium diphenylphosphide (obtained as a yellow highly air‐sensitive solid from the reaction of n‐butyllithium and diphenylphosphane)[13] , NHCs[14] and thione[14] were synthesized following literature established procedures. NMR spectra were recorded on a Bruker Avance III 400 spectrometer. The 1H and 13C NMR spectra were referenced using the solvent signals[15] (δ1H(C6HD5)=7.16; δ13C(C6D6)=128.06). 27Al and 31P NMR spectra were referenced using external standards (δ 27Al(AlCl3 in D2O)=0) (δ 31P(85 % H3PO4 in D2O)=0). Elemental analysis was performed on an Elementar vario MICROcube®. Single crystal X‐ray diffraction analysis were carried out at low temperatures on Bruker AXS X8 Apex CCD and Bruker AXS D8 Venture diffractometers. Structure solution and refinement was performed using SHELX[16] .
4
Structural Characterization of Gold-Platinum and Gold-Palladium Clusters
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The data were collected at 263 K (for Au4Pt2(SR)8) and 100 K (for Au4Pd2(SR)8) using a four circles goniometer Kappa geometry, Bruker AXS D8 Venture, equipped with a Photon 100 CMOS active pixel sensor detector. A Molybdenum monochromatized (λ = 0.71073 Å) X-Ray radiation was used for the measurement. Data were corrected for absorption effects using the Multi-Scan method SADABS. The atomic structure of single crystal was solved by direct methods and further refined by full matrix least squares using the SHELXTL 6.1 bundled software package.
5
X-ray Crystallography of BPTA and Re-BPTA
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Crystal data were collected at 193K using MoKα radiation (wavelength = 0.71073 Å) on a Bruker AXS D8-Venture diffractometer equipped with a Mo Kα sealed tube (λ = 0.71073 Å), a multilayer TRIUMPH X-ray mirror, a Photon III-C14 detector and an Oxford Instruments Cryostream 700+ Series low-temperature device. Phi-and omega-scans were used. The space group was determined on the basis of systematic absences and intensity statistics. Semi-empirical absorption correction was employed. 53 The structures were solved using an intrinsic phasing method (ShelXT). 54 All non-hydrogen atoms were refined anisotropically using the least-square method on F 2 . 55 Hydrogen atoms were refined isotropically at calculated positions using a riding model with their isotropic displacement parameters constrained to be equal to 1.5 times the equivalent isotropic displacement parameters of their pivot atoms for terminal sp3 carbon and 1.2 times for all other carbon atoms. CCDC 2212965 (BPTA) and CCDC 2212966 (Re-BPTA) † contain the supplementary crystallographic data for this paper. Selected crystallographic data are collected in Table 3.
6
Single-Crystal Structural Analysis of Compounds
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The structures of 1-3 were determined at 173 K on a Bruker AXS D8 Venture single-crystal diffractometer equipped with graphite-monochromatized Cu Kα radiation (λ = 1.542 Å). The structures were determined with the ShelXT 24 structure solution program using the Intrinsic Phasing solution method and by using Olex2 25, 26 as the graphical interface. The model was refined with a version of ShelXL 24 using Least Squares minimisation. All non-hydrogen atoms were refined anisotropically. Most hydrogen atom positions were calculated geometrically and refined using the riding model, but some hydrogen atoms were refined freely.
7
X-ray Crystallographic Structure Determination
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X-ray data
for1 (Table 6 ) was collected using a Bruker AXS D8 VENTURE diffractometer
equipped with Mo (Kα) (λ = 0.71073 Å) radiation and
a PHOTON II area detector. The unit cell was determined53 (link),75 (link) by collecting reflections, and then, intensity data for determining
the structure of1 was collected, as described in refs (53 (link)) and (75 (link)). In brief, the frames
were integrated using the program APEX3-SAINT,55 absorption correction was performed using the program SADABS,55 SHELXT-201856 was
used to solve the structure, and it was refined by SHELXL-2018,56 a computer program incorporated in the WinGX
system version v2018.3. ORTEP357 (link) was used
to draw the molecular graphics. Other details are as described in
refs (53 (link)) and (75 (link)).
for
equipped with Mo (Kα) (λ = 0.71073 Å) radiation and
a PHOTON II area detector. The unit cell was determined53 (link),75 (link) by collecting reflections, and then, intensity data for determining
the structure of
were integrated using the program APEX3-SAINT,55 absorption correction was performed using the program SADABS,55 SHELXT-201856 was
used to solve the structure, and it was refined by SHELXL-2018,56 a computer program incorporated in the WinGX
system version v2018.3. ORTEP357 (link) was used
to draw the molecular graphics. Other details are as described in
refs (53 (link)) and (75 (link)).
8
Synthesis and Structural Characterization of C19H15ClN2OS
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C19H15ClN2OS, Mr = 354.85, red-brown block, 0.081 × 0.132 × 0.259 mm, monoclinic, space group P21/c, a = 9.445(4), b = 13.847(5),c = 12.819(5) Å, β = 100.51(1)°, V = 1648(1) Å3, Z = 2, Dc = 1.430 g/cm3, F000 = 736, Bruker AXS D8 VENTURE, MoKα radiation, λ = 0.71073 Å, T = 293(2) K, 2θmax = 55.06°, 40,268 reflections collected, 3711 unique (Rint = 0.047). The structure was solved and refined using the programs XT, VERSION 2018/2 [59 (link)] and SHELXL-2019/1 [60 (link)], respectively. Final GooF = 1.09, R = 0.05, wR = 0.125, R indices based on 3119 reflections with I > 2σ(I) (refinement on F2), 211 parameters, 0 restraints. Lp and absorption corrections applied, μ = 0.366 mm−1. CCDC deposition number 2178985.
9
Structural Characterization of Briavioid A
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Suitable, colorless prisms of briavioid A (9 ) were obtained from a mixture of MeOH/acetone (10:1). The crystal (0.400 × 0.050 × 0.025 mm3) was identified as of the monoclinic system, space group P21 (#4), with a = 9.8798(6) Å, b = 31.107(2) Å, c = 10.4985(7) Å, V = 2871.5(3) Å3, Z = 4, Dcalculated = 1.348 Mg/m3 and λ (Cu Kα) = 1.54178 Å. Intensity data were obtained on a crystal diffractometer (Bruker, AXS D8 Venture, Photon III_C28) up to a θmax of 77.86°. All measurement data from 60,292 reflections were collected, of which 10,314 were independent. The structure was solved by direct methods and refined by a full-matrix least-squares on F2 procedure [15 (link),16 ]. The refined structural model converged to a final R1 = 0.0427; wR2 = 0.1145 for 9539 observed reflections [I > 2σ(I)] and 759 variable parameters. The absolute configuration was established from the Flack parameter x = 0.01(5) [17 (link),18 (link)]. Crystallographic data for the structure of briavioid D (9 ) were deposited at the Cambridge Crystallographic Data Center (CCDC) as supplementary publication number CCDC 2224010 [19 ].
10
X-Ray Structural Analysis of Compounds
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The structures of 1 and 2 were determined at 173 K on a Bruker AXS D8 Venture single-crystal diffractometer equipped with graphite-monochromatized Cu Kα radiation (λ = 1.542 Å) and graphite-monochromatized Mo Kα radiation (λ = 0.71073 Å). The structures were determined with the ShelXT 40 structure solution program using the Intrinsic Phasing solution method and by using Olex2 41, 42 as the graphical interface. The model was refined with a version of ShelXL 40 using Least Squares minimisation. All non-hydrogen atoms were refined anisotropically. Most hydrogen atom positions were calculated geometrically and refined using the riding model, but some hydrogen atoms were refined freely.
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