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_4113111
_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            'C36 H39 N O6'
_chemical_formula_weight         581.68
_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                104.68(3)
_cell_angle_beta                 101.53(3)
_cell_angle_gamma                92.22(3)
_cell_formula_units_Z            2
_cell_length_a                   10.817(2)
_cell_length_b                   10.839(2)
_cell_length_c                   13.945(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1542.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9671
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.085
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_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          0.1618
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                5382
_reflns_number_total             6813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0454236rom20040727_021439.cif
_cod_data_source_block           wulff05
_cod_original_cell_volume        1542.7(5)
_cod_database_code               4113111