(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_4027076
_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         'C22 H16 N4 S6, C5 H12'
_chemical_formula_sum            'C27 H28 N4 S6'
_chemical_formula_weight         600.89
_chemical_name_systematic
; 
 ? 
;
_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                 111.723(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5105(5)
_cell_length_b                   13.5453(6)
_cell_length_c                   15.6906(5)
_cell_measurement_reflns_used    3621
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.45
_cell_measurement_theta_min      4.63
_cell_volume                     2864.96(19)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13282
_diffrn_reflns_theta_full        70.45
_diffrn_reflns_theta_max         70.45
_diffrn_reflns_theta_min         4.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.601
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (SADABS, 1997)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.075
_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     170
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0523P)^2^+2.8244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                2283
_reflns_number_total             2692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300004p_si_003.cif
_cod_data_source_block           wim54
_cod_original_cell_volume        2864.96(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4027076