(Thio)ureido Anion Receptors Based on a 1,3-Alternate Oxacalix[2]arene[2]pyrimidine Scaffold
Wim Van Rossom; Jef Caers; Koen Robeyns; Luc Van Meervelt; Wouter Maes; Wim Dehaen; Journal of Organic Chemistry 77 (2012) 2791–2797; doi:10.1021/jo300004p

data_4027075
_publ_section_title
;
 (Thio)ureido Anion Receptors Based on a 1,3-Alternate
 Oxacalix[2]arene[2]pyrimidine Scaffold
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2791
_journal_page_last               2797
_journal_paper_doi               10.1021/jo300004p
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C24 H20 N4 O4 S2, C1 H1 Cl3'
_chemical_formula_sum            'C25 H21 Cl3 N4 O4 S2'
_chemical_formula_weight         611.93
_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                116.859(5)
_cell_angle_beta                 100.003(6)
_cell_angle_gamma                93.089(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7931(13)
_cell_length_b                   11.7407(12)
_cell_length_c                   12.4871(12)
_cell_measurement_reflns_used    1814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.72
_cell_measurement_theta_min      4.07
_cell_volume                     1374.3(3)
_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, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       '/w and /f 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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12469
_diffrn_reflns_theta_full        67.70
_diffrn_reflns_theta_max         69.72
_diffrn_reflns_theta_min         4.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.778
_exptl_absorpt_correction_T_max  0.385
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (SADABS, 1997)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+0.1644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                3285
_reflns_number_total             4861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300004p_si_002.cif
_cod_data_source_block           wim53
_cod_database_code               4027075