Synthesis and crystal structures of 5,17-dibromo-26,28-dihydroxy-25,27-dipropynyloxycalix[4]arene, 5,17-dibromo-26,28-dipropoxy-25,27-dipropynyloxycalix[4]arene and 25,27-bis(2-azidoethoxy)-5,17-dibromo-26,28-dihydroxycalix[4]arene
Gorbunov, Alexander; Bezzubov, Stanislav; Malakhova, Maria; Kovalev, Vladimir; Vatsouro, Ivan; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024003785

data_2023116
_publ_section_title
;
 Synthesis and crystal structures of
 5,17-dibromo-26,28-dihydroxy-25,27-dipropynyloxycalix[4]arene,
 5,17-dibromo-26,28-dipropoxy-25,27-dipropynyloxycalix[4]arene and
 25,27-bis(2-azidoethoxy)-5,17-dibromo-26,28-dihydroxycalix[4]arene
;
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024003785
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C32 H28 Br2 N6 O4'
_chemical_formula_moiety         'C32 H28 Br2 N6 O4'
_chemical_formula_sum            'C32 H28 Br2 N6 O4'
_chemical_formula_weight         720.42
_chemical_name_systematic
;
25,27-Bis(2-azidoethoxy)-5,17-dibromo-26,28-dihydroxycalix[4]arene
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   36.3261(7)
_cell_length_b                   36.3261(7)
_cell_length_c                   12.1054(4)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.311
_cell_measurement_theta_min      2.243
_cell_volume                     13834.0(6)
_computing_cell_refinement
;
APEX3 (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON III CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45251
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.499
_diffrn_reflns_theta_min         1.802
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.685
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             6552
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7804
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+55.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                6043
_reflns_number_total             7804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5716.cif
_cod_data_source_block           3
_cod_original_cell_volume        13834.0(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2023116
_shelx_estimated_absorpt_t_min   0.437
_shelx_estimated_absorpt_t_max   0.775
_shelx_hkl_checksum              27373
_shelx_res_checksum              72674
_shelx_fab_checksum              62141