Synthesis of deep-cavity fluorous calix[4]arenes as molecular recognition scaffolds.
Osipov, Maksim; Chu, Qianli; Geib, Steven J.; Curran, Dennis P.; Weber, Stephen G.; Beilstein journal of organic chemistry 4 (2008) 36–; doi:10.3762/bjoc.4.36

data_4029806
_publ_section_title
;
 Synthesis of deep-cavity fluorous calix[4]arenes as molecular recognition
 scaffolds.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              36
_journal_paper_doi               10.3762/bjoc.4.36
_journal_volume                  4
_journal_year                    2008
_chemical_formula_sum            'C74 H44 F68 I4 O4.5'
_chemical_formula_weight         2804.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.915(2)
_cell_angle_beta                 92.614(2)
_cell_angle_gamma                91.654(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9956(10)
_cell_length_b                   19.4176(16)
_cell_length_c                   39.769(3)
_cell_measurement_temperature    173(2)
_cell_volume                     9248.3(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            67528
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.533
_exptl_absorpt_correction_T_max  0.7390
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker sadabs'
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5392
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         5.869
_refine_diff_density_min         -2.006
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.789
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1287
_refine_ls_number_reflns         29023
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.791
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.1364
_refine_ls_shift/su_max          1.064
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3055
_refine_ls_wR_factor_ref         0.3243
_reflns_number_gt                16192
_reflns_number_total             29023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-4-36-S2.txt
_cod_data_source_block           max1030
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C74 H44 F68 I4 O4.50'
_cod_database_code               4029806