Solvent-free synthesis of calix[4]resorcinarenes
Brett A. Roberts; Gareth W. V. Cave; Colin L. Raston; Janet L. Scott; Green Chem. 3 () 280–284; doi:10.1039/b104430n

data_7204165
_publ_section_title
;
 Solvent-free synthesis of calix[4]resorcinarenes
;
_journal_issue                   6
_journal_name_full               'Green Chem.'
_journal_page_first              280
_journal_page_last               284
_journal_paper_doi               10.1039/b104430n
_journal_volume                  3
_chemical_formula_moiety         ' C68H70O12.2(C3H8NO).2(C3H6O)'
_chemical_formula_sum            'C80 H98 N2 O16'
_chemical_formula_weight         1343.60
_chemical_name_common
'2,8,14,20-tetra(p-butoxy-phenyl)resorcinarene DMF/acetone solvate '
_chemical_name_systematic
; 
2,8,14,20-tetra(p-butoxy-phenyl)pentacyclo-[19.3.1.13,7.19,13.115,19]octacosa-
1-(25),3,5,7(28),9,11,13(27),15,17,19(26),21,23-dodecaene-
4,6,10,12,16,18,22,24-octaol 
;
_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                90.7340(10)
_cell_angle_beta                 110.9560(10)
_cell_angle_gamma                112.2100(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2391(2)
_cell_length_b                   12.8890(2)
_cell_length_c                   14.4780(4)
_cell_volume                     1786.49(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Enraf-nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '1 degree, phi and omega scans'
_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  0.0984
_diffrn_reflns_av_sigmaI/netI    0.1415
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30522
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.086
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8752
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.2155
_refine_ls_R_factor_gt           0.0979
_refine_ls_shift/su_max          0.183
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1140P)^2^+3.8815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2877
_reflns_number_gt                3850
_reflns_number_total             8752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104430n.txt
_cod_data_source_block           3c
_cod_original_cell_volume        1786.48(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204165