Facile synthesis of a <i>C</i><sub>4</sub>-symmetrical inherently chiral calix[4]arene.
Hodson, Luke; Visagie, Kevin J.; Smith, Michael-Phillip; Loots, Leigh; Kuter, David; Snayer, Trégen M; Arnott, Gareth E.; Chemical communications (Cambridge, England) 57 (2021) 11045–11048; doi:10.1039/d1cc04607a

data_7129038
_publ_section_title
;
 Facile synthesis of a <i>C</i><sub>4</sub>-symmetrical inherently chiral
 calix[4]arene.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11045
_journal_page_last               11048
_journal_paper_doi               10.1039/d1cc04607a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H80 Br4 N4 O12, C H3 O'
_chemical_formula_sum            'C61 H83 Br4 N4 O13'
_chemical_formula_weight         1399.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual-space
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-19 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.935(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.982(2)
_cell_length_b                   23.272(4)
_cell_length_c                   20.029(3)
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.28
_cell_volume                     6493.1(17)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2018)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2018)'
_computing_molecular_graphics
'X-Seed (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX II DUO CCD'
_diffrn_measurement_method       '\f and w\ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            145346
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.692
_diffrn_reflns_theta_min         1.344
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.541
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2016/2'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       lath
_exptl_crystal_F_000             2884
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         15072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+16.0409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10703
_reflns_number_total             15072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04607a2.cif
_cod_data_source_block           3b
_cod_depositor_comments          'Adding full bibliography for 7129038.cif.'
_cod_original_cell_volume        6493.3(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7129038
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              36950
_shelx_hkl_checksum              86397