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_4113110
_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
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.899(3)
_cell_length_b                   16.405(3)
_cell_length_c                   15.888(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3332.4(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37057
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.079
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             1344
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0030(3)
_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   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         7755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.140
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.4333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                4170
_reflns_number_total             7755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0454236rom20040727_021348.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3332.3(12)
_cod_database_code               4113110