X-ray diffraction data was collected on an Oxford Diffraction SuperNova diffractometer with Mo/Cu microfocus X-ray source with mirror optics and an Atlas detector at 150(2) K. The structures were solved in Olex2 graphical user interface43 by direct methods implemented in SHELXT and refined by a full-matrix least-squares procedure based on F2 using SHELXL.120 (link) All non-hydrogen atoms were refined anisotropically. The hydrogen atoms were placed at calculated positions and treated using appropriate riding models. Additional details on structural properties and refinement details are given in the ESI (Tables S2 and S3† ).
Diffraction supernova
Manufactured by Rigaku
The Diffraction SuperNova is a high-performance X-ray diffraction system designed for advanced materials analysis. It features a micro-focus X-ray source and a high-efficiency detector, providing exceptional data quality and resolution. The system is capable of performing a wide range of X-ray diffraction experiments, including phase identification, structural analysis, and in-situ studies.
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Lab products found in correlation
5 protocols using diffraction supernova
1
Structural Determination by X-ray Diffraction
2
Powder X-ray Diffraction Measurements
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Powder X-ray diffraction measurements were recorded on an Oxford Diffraction Supernova in capillary mode using Cu Kα radiation, with a CCD detector at 77 mm from the samples and an exposure time of 66 s. The recorded 2D diffraction images were integrated to produce a 1D diffraction spectrum. The powder samples were packed in 0.7- or 0.5-mm diameter glass capillaries sealed with silicone grease under argon.
3
X-ray Crystallographic Structural Analysis
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X-ray diffraction data were collected using an Oxford Diffraction SuperNova diffractometer with a Mo/Cu microfocus X-ray source (Kα radiation, λMo = 0.71073 Å, λCu = 1.54184 Å) with mirror optics and an Atlas detector at 150(2) K. Structures were solved in Olex2 graphical user interface [41 (link)] by direct methods implemented in SHELXT and refined by a full-matrix least-squares procedure based on F2 using SHELXL [42 (link)]. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed at calculated positions and treated using appropriate riding models. The crystal structure has been submitted to CCDC and has been assigned the deposition numbers 2235957–2235958. Additional crystallographic data (Table S1 ) and photographs of the analyzed crystals (Figure S14 ) are included in the Supplementary information file .
4
Synthesis and Characterization of Rhenium Complexes
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All chemicals were used as received. Syntheses were carried out under aerobic conditions using CH 3 CN dried over 3 Å molecular sieves. (NBu 4 ) 2 [ReCl 6 ] was prepared as described previously. 6, 26 Crystals of the six compounds were collected and left open to air before use in further analysis. Elemental analyses (C, H, N) were performed by MEDAC Ltd. Direct current (dc) magnetic susceptibility measurements were collected on a Quantum Design MPMS-XL SQUID magnetometer equipped with a 7 T dc magnet in the temperature range 2.0-300 K. Diamagnetic corrections were applied using Pascal's constants. 27 Crystallography Data were measured on Rigaku Oxford Diffraction SuperNova (1, 2, 5, 6) and Rigaku Oxford Diffraction XCalibur (3, 4) X-ray diffractometers using Mo-K α radiation. Structures were solved with olex2.solve (1, 2, 6) 28 or ShelXS (3, 4, 5) 29 and refined by full-matrix least-squares on F-squared using ShelXL, interfaced through Olex2. 30 In 1 C( 18) is disordered over two positions with partial occupancies 0.74 and 0.26. In 3, one vinyl-group is disorder over two positioned with partial occupancies 0.72 and 0.28. In 4, the -CH 2 CH 3 group of one ligand is disordered over two positions with partial occupancies 0.77 and 0.23. All non-hydrogen atoms were refined anisotropically. CCDC 1550271-1550276. †
5
Single-Crystal X-Ray Diffraction Analysis
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Single-crystals
of all compounds
suitable for X-ray analyses were grown via the liquid–vapor
diffusion method using dichloromethane and n-hexane
as solvents. The X-ray diffraction measurements were carried out on
a Rigaku Oxford Diffraction SuperNova instrument equipped with a microfocus
Cu X-ray source. During the measurements, crystals were maintained
at low temperature with the use of a Oxford Cryosystems nitrogen gas-flow
device. Unit-cell parameter determination and raw diffraction image
processing were performed with the native diffractometer software.53 All structures were solved using an intrinsic
phasing method implemented in the SHELXT program54 (link) and refined with the SHELXL module of the SHELX package55 (link) (with an aid of the OLEX2 suite56 (link)) within the independent atom model approximation. Scattering
factors, in their analytical form, were taken from the International
Tables for Crystallography.57 Final crystal,
data collection, and refinement parameters for all compounds are summarized
in the associated CIF files, which are present in theSupporting Information , or can be retrieved from
the Cambridge Structural Database58 (link),59 (link) (deposition
numbers: CCDC 2004139-43).
of all compounds
suitable for X-ray analyses were grown via the liquid–vapor
diffusion method using dichloromethane and n-hexane
as solvents. The X-ray diffraction measurements were carried out on
a Rigaku Oxford Diffraction SuperNova instrument equipped with a microfocus
Cu X-ray source. During the measurements, crystals were maintained
at low temperature with the use of a Oxford Cryosystems nitrogen gas-flow
device. Unit-cell parameter determination and raw diffraction image
processing were performed with the native diffractometer software.53 All structures were solved using an intrinsic
phasing method implemented in the SHELXT program54 (link) and refined with the SHELXL module of the SHELX package55 (link) (with an aid of the OLEX2 suite56 (link)) within the independent atom model approximation. Scattering
factors, in their analytical form, were taken from the International
Tables for Crystallography.57 Final crystal,
data collection, and refinement parameters for all compounds are summarized
in the associated CIF files, which are present in the
the Cambridge Structural Database58 (link),59 (link) (deposition
numbers: CCDC 2004139-43).
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