Lower rim calix(4)arene ketone derivatives and their interaction with alkali metal cations. Structural and thermodynamic (solution and complexation) characterisation of the tetraphenyl ketone derivative and its sodium complex
Danil de Namor, Angela F.; Kowalska, Dorota; Castellano, Eduardo E.; Piro, Oscar E.; Sueros Velarde, Felix J.; Villanueva Salas, Jose; Physical Chemistry Chemical Physics 3 (2001) 4010–; doi:10.1039/b104355m

data_7204902
_publ_contact_author
;
Angela F. Danil de Namor
Laboratory of Thermochemistry
Department of Chemistry
University of Surrey
Guildford, Surrey, GU2 5XH
England
;
_publ_section_title
;
 Lower rim calix(4)arene ketone derivatives and their interaction with
 alkali metal cations. Structural and thermodynamic (solution and
 complexation) characterisation of the tetraphenyl ketone derivative
 and its sodium complex
;
_journal_issue                   18
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              4010
_journal_paper_doi               10.1039/b104355m
_journal_volume                  3
_journal_year                    2001
_chemical_formula_sum            'C80 H91 Cl N Na O14'
_chemical_formula_weight         1348.98
_chemical_name_systematic
;
sodium 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetra(benzoyl)methoxy
calix(4)arene monoacetonitrile perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.422(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8693(9)
_cell_length_b                   13.4590(5)
_cell_length_c                   30.405(2)
_cell_measurement_reflns_used    17881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.1
_cell_volume                     7714.3(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.506
_diffrn_measured_fraction_theta_max 0.506
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w'
_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  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            17881
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.116
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         9054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.1066
_refine_ls_shift/su_max          1.040
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3058
_refine_ls_wR_factor_ref         0.3416
_reflns_number_gt                6117
_reflns_number_total             9054
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            program.txt
_cod_data_source_block           s97
_cod_depositor_comments
;
The following automatic conversions were performed:
'_publ_contact_autor' tag replaced with '_publ_contact_author'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=3D(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=3D1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7714.4(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7204902