Synthesis and structural characterisation of the first bis(bora)calixarene: a selective, bidentate, fluorescent fluoride sensor
Arimori, Susumu; Davidson, Matthew G.; Fyles, Thomas M.; Hibbert, Thomas G.; James, Tony D.; Kociok-Köhn, Gabriele I.; Chemical Communications (Cambridge, United Kingdom)  (2004) 1640–1641; doi:10.1039/b404937c

data_7110322
_publ_section_title
;
 Synthesis and structural characterisation of the first bis(bora)calixarene:
 a selective, bidentate, fluorescent fluoride sensor
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   14
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom) 
;
_journal_page_first              1640
_journal_page_last               1641
_journal_paper_doi               10.1039/b404937c
_journal_year                    2004
_chemical_formula_moiety         '[(C56 H62 B2 O4)(C H3 C N)1.5]'
_chemical_formula_sum            'C59 H66.5 B2 N1.5 O4'
_chemical_formula_weight         882.26
_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                 100.5070(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0360(5)
_cell_length_b                   21.5750(10)
_cell_length_c                   22.0480(13)
_cell_measurement_temperature    150(2)
_cell_volume                     5161.6(5)
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material  'SHELX97-2, G. M. Sheldrick'
_computing_structure_refinement
;
SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick,
Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4,
D-3400 Gottingen, Germany, 1998.
;
_computing_structure_solution
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \f-rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1449
_diffrn_reflns_av_sigmaI/netI    0.1268
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24829
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_correction_T_min  0.9863
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.010(2)
_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   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.2036
_refine_ls_R_factor_gt           0.1028
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2723
_refine_ls_wR_factor_ref         0.3238
_reflns_number_gt                3308
_reflns_number_total             7101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b404937csup1.cif
_cod_data_source_block           k00tgh3
_cod_original_formula_sum        'C59 H66.50 B2 N1.50 O4'
_cod_database_code               7110322