Selective mono-O-acylation of C2V-symmetrical calix[4]arenediols with acylisocyanates.
Yakovenko, Anton V.; Boyko, Vyacheslav I.; Kushnir, Oleg V.; Tsymbal, Ivan F.; Lipkowski, Janusz; Shivanyuk, Alexander; Kalchenko, Vitaly I.; Organic letters 6 (2004) 2769–2772; doi:10.1021/ol049030n

data_1507056
_publ_section_title
;
 Selective mono-O-acylation of C2V-symmetrical calix[4]arenediols with
 acylisocyanates.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              2769
_journal_page_last               2772
_journal_paper_doi               10.1021/ol049030n
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C53 H66 Cl3 N3 O6'
_chemical_formula_weight         947.44
_chemical_name_common            calixarene
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.750(3)
_cell_length_b                   12.540(2)
_cell_length_c                   33.750(7)
_cell_measurement_temperature    293(2)
_cell_volume                     5324.3(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            16489
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.0240(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1741P)^2^+6.2184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2916
_reflns_number_gt                7136
_reflns_number_total             10567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol049030nsi20040526_020210.cif
_cod_data_source_block           cal99x
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1507056