The intensities for the X-ray determinations were collected at room temperature on a BRÜKER APEX II duo for HL3FPh, HL4ClPh, HL5NO2Ph and HL6Al; and on a STOE IPDS 2T diffractometer at 200 K for the Au1 and Au2 complexes, both instruments equipped with Mo-Kα radiation (λ = 0.71073 Å). Standard procedures were applied for data reduction and absorption correction [35 ,36 ]. The structures were predicted by direct methods using SHELXS97 [37 (link)] or SHELXT [38 (link)] and refined by using SHELXL2016 [39 (link)], programs included in the OLEX2 program package [40 (link)]. The positions of the hydrogen atoms were calculated at idealized positions and treated with the “riding model” option of the SHELXL2016 program [39 (link)]. The details regarding structure refinement can be found in Table 1 , with the exception of HL4ClPh, whose data were not adequate. Since Au1 crystallized together with disordered solvent molecules (partially close to special positions), the refinement of its structure was undertaken with the removal of the disordered solvent molecules using the solvent mask option of OLEX2. Details are given in the Supplementary Materials . The representations of molecular and crystalline structures were prepared with the programs Mercury 4.3.1. [41 (link)] and DIAMOND 4 [42 ].
Ipds 2t
Manufactured by STOE
Sourced in Germany
The IPDS 2T is a compact and versatile lab equipment designed for precision measurements. It functions as a high-resolution imaging system capable of capturing detailed images and data. The core function of the IPDS 2T is to provide accurate and reliable data acquisition for various research and analytical applications.
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Lab products found in correlation
6 protocols using ipds 2t
1
X-ray Analysis of Metal Complexes
2
X-Ray Structural Analysis of 2c Crystal
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A suitable
single crystal of2c was mounted on a thin glass fiber
coated with paraffin oil. X-ray single-crystal structural data were
collected at low temperature (170 K) using a STOE IPDS 2T diffractometer
equipped with a normal-focus, 2.4 kW, sealed-tube X-ray source with
graphite-monochromated Mo Kα radiation (λ = 0.71073 Å).
The program X-Area was used for integration of the diffraction profiles;
numerical absorption correction was made with the programs X-shape
and X-red32; all from STOE 2010. The structure was solved by SHELXT-201426 (link) and refined by full-matrix least-squares methods
using SHELXL-2013.27 (link) The nonhydrogen atoms
were refined anisotropically. Hydrogen atoms were refined isotropically
on calculated positions using a riding model with their Uiso values
constrained to 1.2 Ueq of their pivot atoms. All calculations were
carried out using SHELX-201327 (link) and the
WinGX GUI, ver2013.2.28 (link) The crystallographic
data are summarized inTable 4 .
The crystallographic data were deposited with the
Cambridge Crystallographic
Data Centre (CCDC) 12 Union Road, Cambridge CB21EZ, U.K. These data
can be obtained free of charge on quoting the depository number CCDC
1544200 by FAX (+44-1223-336-033), e-mail (deposit@ccdc.cam.ac.uk ), or their web interface (at http://www.ccdc.cam.ac.uk ).
single crystal of
coated with paraffin oil. X-ray single-crystal structural data were
collected at low temperature (170 K) using a STOE IPDS 2T diffractometer
equipped with a normal-focus, 2.4 kW, sealed-tube X-ray source with
graphite-monochromated Mo Kα radiation (λ = 0.71073 Å).
The program X-Area was used for integration of the diffraction profiles;
numerical absorption correction was made with the programs X-shape
and X-red32; all from STOE 2010. The structure was solved by SHELXT-201426 (link) and refined by full-matrix least-squares methods
using SHELXL-2013.27 (link) The nonhydrogen atoms
were refined anisotropically. Hydrogen atoms were refined isotropically
on calculated positions using a riding model with their Uiso values
constrained to 1.2 Ueq of their pivot atoms. All calculations were
carried out using SHELX-201327 (link) and the
WinGX GUI, ver2013.2.28 (link) The crystallographic
data are summarized in
The crystallographic data were deposited with the
Cambridge Crystallographic
Data Centre (CCDC) 12 Union Road, Cambridge CB21EZ, U.K. These data
can be obtained free of charge on quoting the depository number CCDC
1544200 by FAX (+44-1223-336-033), e-mail (
3
Single Crystal Structure of Compound 6
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Single crystals of 6 were crystallized from acetonitrile by slow evaporation. A suitable crystal was selected and was mounted on a loop in oil on a Stoe IPDS2T diffractometer. The crystallographic data of the single crystal were collected with Cu Kα1 radiation (λ = 1.54186 Å). The crystal was kept at 250(2) K during data collection by an Oxford Cryosystem open-flow cryostat. Using Olex2 [30 (link)], the structure was solved with the ShelXT [31 (link)] structure solution program using Intrinsic Phasing and refined with the ShelXL [31 (link)] refinement package using Least Squares minimization.
4
X-ray Structural Analysis Protocol
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The data for the X-ray structural analyses were collected at T = 100.0 K with Mo-Kα-radiation (λ = 0.71073 Å) on area detector systems Stoe IPDS/2T for X, Y, and Z and with Cu-Kα-radiation (λ = 1.54186 Å) for X, Y, Z on an area detector system Stoe StadiVari. The structures were solved by methods of SHELXT from SHELXL-2018/136, and refined by full-matrix least-squares methods against F2 with the SHELXL52 program using Olex2 v1.3.0 software53 (link). All hydrogen atoms were kept riding on calculated positions with isotropic displacement parameters U = 1.2 Ueq of the bonding partners. The crystal data and experimental parameters of the structure determination are collected in Supplementary Tables 3 –8 . Supplementary structural images are shown in Supplementary Figs. 13 –26 . Figures were created with Diamond 454 .
5
Structure Determination via X-ray Crystallography
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X-ray data were collected on a STOE IPDS-2T (STOE, Darmstadt, Germany) or Bruker CCD instruments (Bruker, Billerica, MA, USA) with Mo/Kα radiation. SADABS or X-RED32 were used for absorption correction [129 ,130 ]. The SHELX programs [131 (link),132 (link)] included in the WinGX [133 (link)] or OLEX2 [134 (link)] program packages were used for structure solution and refinement. The ‘riding model’ option of SHELXL was used to treat the hydrogen atoms. Diffuse and/or strongly disordered solvent molecules were treated using the SQUEEZE option installed in the program PLATON or the solvent mask option of OLEX2. Details are outlined in the Supplementary Materials . Molecular graphics were produced with the program DIAMOND, vers. 5.0 [135 ].
6
Chiral HPLC Separation and Characterization of (14S/15R)-14-deoxyoxacyclododecindione
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Analytical, chiral HPLC was performed on a Daicel chiralpak AD-H column, 250 × 4.6 mm i.D., flow 1.0 mL min -1 . Solvent system heptanes : ethanol : methanol 5 : 1 : 1. R t ((+)-4) = 6.2 min, R t ((-)-4) = 4.5 min. Preparative, chiral HPLC was performed on a chiralpak AD-H column, 250 × 30 mm i.D., flow 30 mL min -1 . Solvent system heptane : ethanol : methanol 5 : 1 : 1.
The polarimeter values were measured with a Perkin-Elmer 241 polarimeter at 546 nm and 578 nm. The data were extrapolated to a wavelength of λ = 589 nm by using the Drude equation. 23 Crystallization was performed by the solvent diffusion method using ethyl acetate and petroleum ether.
X-ray crystallography of (+)-4 was performed on a STOE IPDS 2T with Mo-K α radiation (graphite monochromator).
CCDC 1454207 contains the supplementary crystallographic data for (14S/15R)-14-deoxyoxacyclododecindione (+)-4.
The polarimeter values were measured with a Perkin-Elmer 241 polarimeter at 546 nm and 578 nm. The data were extrapolated to a wavelength of λ = 589 nm by using the Drude equation. 23 Crystallization was performed by the solvent diffusion method using ethyl acetate and petroleum ether.
X-ray crystallography of (+)-4 was performed on a STOE IPDS 2T with Mo-K α radiation (graphite monochromator).
CCDC 1454207 contains the supplementary crystallographic data for (14S/15R)-14-deoxyoxacyclododecindione (+)-4.
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