Thermodynamics of cation (alkali-metal) complexation by 5,11,17,23-tetra-tert-butyl[25,26,27,28-tetrakis(2-pyridylmethyl)oxy]- calix(4)arene and the crystal structure‒superstructure of its 1:1 complex with sodium and acetonitrile
Danil de Namor, Angela F.; Castellano, Eduardo E.; Pulcha Salazar, Lupe E.; Piro, Oscar E.; Jafou, Olga; Physical Chemistry Chemical Physics 1 (1999) 285–; doi:10.1039/a806902f

data_7217110
_publ_section_title
;
 Thermodynamics of cation (alkali-metal) complexation by
 5,11,17,23-tetra-tert-butyl[25,26,27,28-tetrakis(2-pyridylmethyl)oxy]-
 calix(4)arene and the crystal structure--superstructure of its 1:1
 complex with sodium and acetonitrile
;
_journal_issue                   2
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              285
_journal_paper_doi               10.1039/a806902f
_journal_volume                  1
_journal_year                    1999
_chemical_formula_sum            'C70 H79 Cl N5 Na O8'
_chemical_formula_weight         1176.82
_chemical_name_systematic
; 
 sodium p-tert-butyl[25,26,27-28-tetrakis(2-pyridylmethyl)oxy]    
 calix(4)arene monoacetonitrile perchlorate 
;
_space_group_IT_number           103
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2c'
_symmetry_space_group_name_H-M   'P 4 c c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.791(2)
_cell_length_b                   21.791(2)
_cell_length_c                   26.958(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.12
_cell_measurement_theta_min      13.4
_cell_volume                     12801(2)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'SDP (Frenz, 1983)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2*theta-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4505
_diffrn_reflns_theta_max         60.02
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       prism
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.214
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.272
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_obs          0.1029
_refine_ls_shift/esd_max         2.722
_refine_ls_shift/esd_mean        0.161
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2344P)^2^+5.4326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3382
_refine_ls_wR_factor_obs         0.2940
_reflns_number_observed          2777
_reflns_number_total             4505
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806902f.txt
_cod_data_source_block           s93
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2344P)^2^+5.4326P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2344P)^2^+5.4326P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4cc
_cod_database_code               7217110