An Integrated Approach (Thermodynamic, Structural, and Computational) to the Study of Complexation of Alkali-Metal Cations by a Lower-Rim Calix[4]arene Amide Derivative in Acetonitrile
Gordan Horvat; Vladimir Stilinović; Tomica Hrenar; Branko Kaitner; Leo Frkanec; Vladislav Tomišić; Inorganic Chemistry 51 (2012) 6264–6278; doi:10.1021/ic300474s

data_4329358
_publ_section_title
;
 An Integrated Approach (Thermodynamic, Structural, and Computational) to
 the Study of Complexation of Alkali-Metal Cations by a Lower-Rim
 Calix[4]arene Amide Derivative in Acetonitrile
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6264
_journal_page_last               6278
_journal_paper_doi               10.1021/ic300474s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C76 H116 N4 Na O8, C8 H11 N2 O3, C2 H6 O, C2 H3 N, 3(H2 O)'
_chemical_formula_sum            'C88 H142 N7 Na O15'
_chemical_formula_weight         1561.09
_chemical_name_systematic
;
5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrakis(N-hexylaminocarbonylmethoxy)
calix[4]arene-sodium 5,5-diethylbarbiturate acetonitrile, ethanol solvate 
trihydrete
;
_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_date             2011-02-03T13:45:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.404(3)
_cell_angle_beta                 90.787(3)
_cell_angle_gamma                106.426(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1464(4)
_cell_length_b                   16.8767(6)
_cell_length_c                   22.1602(8)
_cell_measurement_reflns_used    214
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.6
_cell_volume                     4657.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35524
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.82
_diffrn_standards_number         27
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.833
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         15632
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.1054
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.302
_refine_ls_wR_factor_ref         0.3246
_reflns_number_gt                8850
_reflns_number_total             15632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300474s_si_002_5.cif
_cod_data_source_block           calix_Na_barb
_cod_database_code               4329358