Lower Rim 1,3-Di{4-antipyrine}amide Conjugate of Calix[4]arene: Synthesis, Characterization, and Selective Recognition of Hg2+ and Its Sensitivity toward Pyrimidine Bases
Jayaraman Dessingou; Khatija Tabbasum; Atanu Mitra; Vijaya Kumar Hinge; Chebrolu P. Rao; Journal of Organic Chemistry 77 (2012) 1406–1413; doi:10.1021/jo2022372

data_4026923
_publ_section_title
;
 Lower Rim 1,3-Di{4-antipyrine}amide Conjugate of Calix[4]arene:
 Synthesis, Characterization, and Selective Recognition of Hg2+ and Its
 Sensitivity toward Pyrimidine Bases
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1406
_journal_page_last               1413
_journal_paper_doi               10.1021/jo2022372
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C72 H90 N6 O10'
_chemical_formula_weight         1199.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.797(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.4499(7)
_cell_length_b                   11.9982(3)
_cell_length_c                   25.5576(8)
_cell_measurement_reflns_used    20359
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.7054
_cell_measurement_theta_min      2.9385
_cell_volume                     6554.7(4)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55285
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_correction_T_min  0.9714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         11527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0334P)^2^+3.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                8377
_reflns_number_total             11527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2022372_si_002.cif
_cod_data_source_block           cpr021
_cod_original_cell_volume        6554.7(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4026923