Intermolecular distance measurements in supramolecular solids: 13C‒19F REDOR NMR spectroscopy of p-tert-butylcalix[4]arene‒fluorobenzene
Brouwer, Eric B.; Gougeon, Regis D. M.; Hirschinger, Je´rôme; Udachin, Kostantin A.; Harris, Robin K.; Ripmeester, John A.; Physical Chemistry Chemical Physics 1 (1999) 4043–; doi:10.1039/a904189c

data_7217113
_publ_section_title
;
 Intermolecular distance measurements in supramolecular solids: 13C--19F
 REDOR NMR spectroscopy of p-tert-butylcalix[4]arene--fluorobenzene
;
_journal_issue                   17
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              4043
_journal_paper_doi               10.1039/a904189c
_journal_volume                  1
_journal_year                    1999
_chemical_formula_sum            'C50 H61 F O4'
_chemical_formula_weight         744.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8581(2)
_cell_length_b                   12.8581(2)
_cell_length_c                   13.2833(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2196.14(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13945
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.072
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         2666
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+0.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                2024
_reflns_number_total             2666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904189c.txt
_cod_data_source_block           koss28
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+0.0740P] 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^)+(0.0995P)^2^+0.0740P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7217113