Rapid and facile one-step microwave synthesis of macrobicyclic cryptands.
Baisch, Ulrich; Scicluna, Marie Christine; Vella-Zarb, Liana; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 448–451; doi:10.1107/S2056989025003044

data_2023483
_publ_section_title
;
 Rapid and facile one-step microwave synthesis of macrobicyclic cryptands.
;
_journal_coeditor_code           NX2023
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              448
_journal_page_last               451
_journal_paper_doi               10.1107/S2056989025003044
_journal_volume                  81
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C36 H42 N8, 6H2 O'
_chemical_formula_moiety         'C36 H42 N8, 6(H2 O)'
_chemical_formula_sum            'C36 H54 N8 O6'
_chemical_formula_weight         694.87
_chemical_name_systematic
'6,16,25(1,4)-Tribenzena-1,4,8,11,14,18,23,27-octaazabicyclo[9.9.9]nonacosaphane-4,7,14,17,23,26-hexaene hexahydrate'
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
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_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
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_cell_angle_gamma                120
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_cell_length_a                   14.5942(2)
_cell_length_b                   14.5942(2)
_cell_length_c                   15.4565(2)
_cell_measurement_reflns_used    4384
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.9610
_cell_measurement_theta_min      1.8680
_cell_volume                     2851.03(7)
_computing_cell_refinement
;
CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)
;
_computing_data_reduction
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CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
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_computing_publication_material
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Olex2 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
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ShelXL (Sheldrick, 2015b)
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_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
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_diffrn_ambient_temperature      120
_diffrn_detector                 'Pilatus 2M'
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_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device       'Kappa CCD diffractometer at BM01 ESRF'
_diffrn_measurement_device_type  'Kappa CCD diffractometer at BM01 ESRF'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.64066
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4982
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_diffrn_reflns_theta_max         25.954
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74689
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_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2018)
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_density_diffrn    1.214
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_exptl_crystal_size_max          0.12
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_refine_diff_density_max         0.262
_refine_diff_density_min         -0.158
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 691 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                1553
_reflns_number_total             1565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nx2023.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023483.cif.'
_cod_original_cell_volume        2851.03(9)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               2023483
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.993