A New Convergent Strategy for the Synthesis of Calixarenes via a Triple Annulation of Fischer Carbene Complexes
Vijay Gopalsamuthiram; William D. Wulff; Journal of the American Chemical Society 126 (2004) 13936–13937; doi:10.1021/ja0454236

data_4113109
_publ_section_title
;
 A New Convergent Strategy for the Synthesis of Calixarenes via a Triple
 Annulation of Fischer Carbene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13936
_journal_page_last               13937
_journal_paper_doi               10.1021/ja0454236
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C44 H40 O4'
_chemical_formula_weight         632.76
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.699(2)
_cell_length_b                   15.699(2)
_cell_length_c                   16.214(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3996.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.7337
_diffrn_reflns_av_sigmaI/netI    0.4829
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47415
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.066
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_F_000             1344
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.491
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.491
_refine_ls_R_factor_all          0.4427
_refine_ls_R_factor_gt           0.1882
_refine_ls_shift/su_max          5.561
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3515
_refine_ls_wR_factor_ref         0.4135
_reflns_number_gt                1418
_reflns_number_total             4877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0454236rom20040727_021330.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3996.2(11)
_cod_database_code               4113109