Selective synthesis of functionalized thia- and oxacalix[2]arene[2]pyrimidines.
Maes, Wouter; Van Rossom, Wim; Van Hecke, Kristof; Van Meervelt, Luc; Dehaen, Wim; Organic letters 8 (2006) 4161–4164; doi:10.1021/ol0617446

data_1506188
_publ_section_title
;
 Selective synthesis of functionalized thia- and
 oxacalix[2]arene[2]pyrimidines.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4161
_journal_page_last               4164
_journal_paper_doi               10.1021/ol0617446
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C34 H24 N4 O4'
_chemical_formula_sum            'C34 H24 N4 O4'
_chemical_formula_weight         552.57
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 129.9540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.2904(6)
_cell_length_b                   4.64990(10)
_cell_length_c                   21.8825(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2596.60(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11670
_diffrn_reflns_theta_full        70.86
_diffrn_reflns_theta_max         70.86
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+2.0491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                2214
_reflns_number_total             2447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0617446si20060717_031001.cif
_cod_data_source_block           wdb06
_cod_original_cell_volume        2596.61(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1506188