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_4329356
_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 H119 N4 O8, H2 O, C2 H3 N'
_chemical_formula_sum            'C78 H121 N5 O9'
_chemical_formula_weight         1272.8
_chemical_name_systematic
;
5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrakis(N-hexylaminocarbonylmethoxy)
calix[4]arene acetonitrile solvate monohydrate
;
_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             2011-02-02T13:28:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                65.402(16)
_cell_angle_beta                 74.233(13)
_cell_angle_gamma                79.578(13)
_cell_formula_units_Z            2
_cell_length_a                   11.6750(16)
_cell_length_b                   18.183(3)
_cell_length_c                   20.382(3)
_cell_measurement_reflns_used    619
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.6
_cell_volume                     3774.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.1019
_diffrn_reflns_av_unetI/netI     0.5591
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18772
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.75
_diffrn_standards_number         27
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.623
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         11994
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.623
_refine_ls_R_factor_all          0.2523
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                2591
_reflns_number_total             11994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300474s_si_002_3.cif
_cod_data_source_block           calix_MeCN
_cod_original_cell_volume        3774.8(10)
_cod_database_code               4329356