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_4329354
_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 O8'
_chemical_formula_sum            'C76 H116 N4 O8'
_chemical_formula_weight         1213.73
_chemical_name_systematic
;
5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrakis(N-hexylaminocarbonylmethoxy)
calix[4]arene
;
_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_date             2011-02-22T11:34:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.575(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.981(2)
_cell_length_b                   24.792(2)
_cell_length_c                   18.5200(17)
_cell_measurement_reflns_used    421
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.6
_cell_volume                     14683(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.1742
_diffrn_reflns_av_unetI/netI     0.3005
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45804
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.69
_diffrn_standards_number         27
_exptl_absorpt_coefficient_mu    0.07
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         12065
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.2762
_refine_ls_R_factor_gt           0.1292
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3294
_refine_ls_wR_factor_ref         0.367
_reflns_number_gt                3617
_reflns_number_total             12065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300474s_si_002_1.cif
_cod_data_source_block           calix
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4329354