Crystal data, data collection and structure refinement details for 1, 2 and 3 are summarized in Table 1 . Diffraction data were obtained at 100(1) K using a Bruker SMART CCD 1000 (1 and 2) or a Bruker X8 Kappa APEXII (3) diffractometer from crystals mounted on glass fibers. Data were corrected for Lorentz and polarization effects and for absorption following multi-scan type.29 The structures were solved by direct methods and subsequent difference Fourier maps30 (link) and refined on F2 by a full-matrix least-squares procedure using anisotropic displacement parameters.30 (link) Hydrogen atoms attached to carbon and nitrogen atoms were placed in geometrically idealized positions and were refined with isotropic displacement parameters constrained to 1.2/1.5 Ueq of the carrier atoms. Molecular graphics were generated with DIAMOND.31 For each structure peculiarities of the refinement are indicated in ESI (S1–S3).†
X8 kappa apex 2
Manufactured by Bruker
The X8 Kappa Apex II is a single-crystal X-ray diffraction system designed for high-performance crystallographic analysis. It features a kappa goniometer and a high-flux microfocus X-ray source, providing advanced structural determination capabilities.
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7 protocols using x8 kappa apex 2
1
Crystal Structure Determination Protocol
2
X-ray Crystallographic Structural Analysis
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X-ray diffraction data were collected on a Bruker X8 Kappa Apex II diffractometer using Mo Kα radiation (1–3 , 6 ), a Bruker D8 VENTURE diffractometer using Mo Kα radiation (5 ), or a Bruker D8 VENTURE diffractometer using Cu Kα radiation (7 and 11 ). Crystal data, data collection and refinement parameters are summarized in Table S1 . The structures were solved using direct methods and standard difference map techniques, and were refined by full-matrix least-squares procedures on F2 with SHELXTL (Sheldrick, 1981 , 2015 (link)). All hydrogen atoms bound to carbon were placed in calculated positions and refined with a riding model [Uiso(H) = 1.2–1.5Ueq(C)], while hydrogen atoms bound to boron were located on the difference map and freely refined. For 3 , some carbon-bound hydrogen atoms involved in sigma interactions with potassium were also located on the difference map and freely refined. Database: CCDC Nos. 2159079-2159084 (1 -3 and 5 -7 ) and 2192622 (11 ) contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/retrieving.html, or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: (+44) 1223-336-033; or e-mail: deposit@ccdc.cam.ac.uk.
3
X-ray Diffraction Structural Determination
4
Crystallization of Compound 5
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Crystals of 5 were
obtained from the saturated solution of the chloroform/hexane solvent
system. The X-ray structure was obtained using a Bruker X8 KAPPA APEX
II diffractometer using a wavelength of 0.71 Å.
obtained from the saturated solution of the chloroform/hexane solvent
system. The X-ray structure was obtained using a Bruker X8 KAPPA APEX
II diffractometer using a wavelength of 0.71 Å.
5
Synthesis and Crystallographic Analysis of 2,4-dimethoxy-THPQs
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Single crystals of 2,4-dimethoxy-THPQs 4(a–d) are grown by recrystallisation method using a mixture of 20 mL dichloromethane and 2 mL methanol. The X-ray intensity measurements were taken at 296(2) K using Mo Kα radiation with a wavelength of 0.71073 on a Bruker X8 Kappa APEX II diffractometer with an X-ray generator operating at 50 kV and 30 mA. The Bruker SAINT software suite was used to collect intensity data and correct frames using a narrow-frame algorithm. The empirical absorption correction (multiscan) was performed on each structure using SADABS. SHELXL-2014/7, which is part of the Sheldrick-2014 programme suite, was used to solve the structure using direct methods. The positional and anisotropic temperature parameters of non-hydrogen atoms were refined by the full-matrix least-squares method on F2 using the SHELXL-2014/7. Crystallography tools PLATON, ORTEP and MERCURY were used for structure analysis and demonstration of results. Details of data collection, crystal parameters and structure refinement process of 4(a–d) are given in Table 3 .
6
Single Crystal X-ray Diffraction Analysis
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X-ray diffraction data were collected on a Bruker X8 Kappa Apex II diffractometer using Mo Kα radiation (for 1) or on a Bruker D8 VENTURE diffractometer using Cu Kα radiation (for 2 and 3). Crystal data, data collection and refinement parameters are summarized in Table S1 (ESI† ). The structures were solved using a dual-space method and standard difference map techniques and were refined by full-matrix least-squares procedures on F2 with SHELXTL.23 All hydrogen atoms bound to carbon were placed in calculated positions and refined with a riding model [Uiso(H) = 1.2 − 1.5Ueq(C)]. The hydrogen atom bound to nitrogen was located on the difference map and refined freely or with an N–H distance restraint (for 3) [Uiso(H) = 1.2Ueq(N)].
7
X-ray Crystallographic Analysis Protocol
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Diffraction
data were obtained at 100.0(1) K on a Bruker X8 KappaAPEXII diffractometer
from yellow crystals of1 –3 mounted
on glass fibers. Graphite monochromated MoK(α) radiation (λ
= 0.71073 Å) was used throughout. The data were processed with
APEX232 and corrected for absorption using
SADABS.33 The structures were solved by
direct methods34 (link) and refined by full-matrix
least-squares techniques against F2.34 (link) Positional and anisotropic atomic displacement
parameters were refined for all non-hydrogen atoms. Hydrogen atoms
attached to carbon were located in difference Fourier maps or placed
in geometrically idealized positions. The O–H and N–H
hydrogen atoms were located from difference maps. All hydrogen atoms
were refined using a riding model. Molecular graphics were generated
with DIAMOND.35 Details on the particularity
in the resolution of each structure are collected inSupporting Information , and the crystal data, experimental
details, and refinement results are summarized inTable 1 .
data were obtained at 100.0(1) K on a Bruker X8 KappaAPEXII diffractometer
from yellow crystals of
on glass fibers. Graphite monochromated MoK(α) radiation (λ
= 0.71073 Å) was used throughout. The data were processed with
APEX232 and corrected for absorption using
SADABS.33 The structures were solved by
direct methods34 (link) and refined by full-matrix
least-squares techniques against F2.34 (link) Positional and anisotropic atomic displacement
parameters were refined for all non-hydrogen atoms. Hydrogen atoms
attached to carbon were located in difference Fourier maps or placed
in geometrically idealized positions. The O–H and N–H
hydrogen atoms were located from difference maps. All hydrogen atoms
were refined using a riding model. Molecular graphics were generated
with DIAMOND.35 Details on the particularity
in the resolution of each structure are collected in
details, and refinement results are summarized in
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