Tuning the Selectivity/Specificity of Fluorescent Metal Ion Sensors Based on N2S2 Pyridine-Containing Macrocyclic Ligands by Changing the Fluorogenic Subunit: Spectrofluorimetric and Metal Ion Binding Studies
M. Carla Aragoni; Massimiliano Arca; Andrea Bencini; Alexander J. Blake; Claudia Caltagirone; Greta De Filippo; Francesco A. Devillanova; Alessandra Garau; Thomas Gelbrich; Michael B. Hursthouse; Francesco Isaia; Vito Lippolis; Marta Mameli; Palma Mariani; Barbara Valtancoli; Claire Wilson; Inorganic Chemistry 46 (2007) 4548–4559; doi:10.1021/ic070169e

data_4308166
_publ_section_title
;
Tuning the Selectivity/Specificity of Fluorescent Metal Ion Sensors Based
on N2S2 Pyridine-Containing Macrocyclic Ligands by Changing the Fluorogenic
Subunit: Spectrofluorimetric and Metal Ion Binding Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4548
_journal_page_last               4559
_journal_paper_doi               10.1021/ic070169e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'Cu(C21 H22 Cl N3 O1 S2)2 2+,2(BF4-),2(C H3N O2)'
_chemical_formula_sum            'C44 H50 B2 Cl2 Cu F8 N8 O6 S4'
_chemical_formula_weight         1223.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.38(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.7570(17)
_cell_length_b                   25.205(6)
_cell_length_c                   15.048(4)
_cell_measurement_reflns_used    4338
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.91
_cell_volume                     2520.9(11)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1355
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25640
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.8577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV Acta Cryst. A51 (1995) 33-37'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0034(8)
_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   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          1.425
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+3.7535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                3022
_reflns_number_total             4750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070169e_si_5.cif
_cod_data_source_block           s92
_cod_database_code               4308166