Efficient post-macrocyclization functionalizations of oxacalix[2]arene[2]pyrimidines.
Van Rossom, Wim; Maes, Wouter; Kishore, Lingam; Ovaere, Margriet; Van Meervelt, Luc; Dehaen, Wim; Organic letters 10 (2008) 585–588; doi:10.1021/ol702864y

data_1504520
_publ_section_title
;
 Efficient post-macrocyclization functionalizations of
 oxacalix[2]arene[2]pyrimidines.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              585
_journal_page_last               588
_journal_paper_doi               10.1021/ol702864y
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C40 H34 N4 O10, 3(C H Cl3)'
_chemical_formula_sum            'C43 H37 Cl9 N4 O10'
_chemical_formula_weight         1088.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.407(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6155(12)
_cell_length_b                   22.549(2)
_cell_length_c                   14.7003(12)
_cell_measurement_reflns_used    2176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.6
_cell_measurement_theta_min      3.63
_cell_volume                     4765.0(7)
_computing_cell_refinement       'Bruker SAINT (SAINT, 1997)'
_computing_data_collection       'Bruker SMART (SMART, 1997)'
_computing_data_reduction        'Bruker SAINT (SAINT, 1997)'
_computing_molecular_graphics    'PLUTON (Spek, 1998)'
_computing_publication_material  'PLATON (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'omega and phi scan'
_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  0.1310
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39263
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         3.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.354
_exptl_absorpt_correction_T_max  0.585
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (SADABS, 1997)'
_exptl_crystal_colour            transparant
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2223.8
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         8387
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1147P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2216
_reflns_number_gt                5118
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol702864y-file001.cif
_cod_data_source_block           wim68
_cod_original_cell_volume        4764.9(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1504520