Azocalix[4]arene Strapped Calix[4]pyrrole: A Confirmable Fluoride Sensor.
Thiampanya, Preecha; Muangsin, Nongnuj; Pulpoka, Buncha; Organic letters 14 (2012) 4050–4053; doi:10.1021/ol301684r

data_1508322
_publ_section_title
;
 Azocalix[4]arene Strapped Calix[4]pyrrole: A Confirmable Fluoride Sensor.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4050
_journal_page_last               4053
_journal_paper_doi               10.1021/ol301684r
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C68 H66 N6 O16, C H Cl3'
_chemical_formula_sum            'C69 H67 Cl3 N6 O16'
_chemical_formula_weight         1342.64
_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
_audit_update_record
;
2012-04-24 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.7260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9165(5)
_cell_length_b                   16.5501(4)
_cell_length_c                   22.8972(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.440
_cell_volume                     6647.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42038
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   NONE
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         13657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1697
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.489
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+6.1652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.3053
_reflns_number_gt                6538
_reflns_number_total             13657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol301684r_si_002.cif
_cod_data_source_block           ajbuncha-precha
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1508322