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_4308162
_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
'C51 H47 Cl3 Cu3 N7 O3 S4, 3(Cl O4), 7.5(H2 O)'
_chemical_formula_sum            'C51 H62 Cl6 Cu3 N7 O22.5 S4'
_chemical_formula_weight         1664.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                116.069(4)
_cell_angle_beta                 104.143(4)
_cell_angle_gamma                91.725(4)
_cell_formula_units_Z            2
_cell_length_a                   12.297(3)
_cell_length_b                   17.199(4)
_cell_length_c                   17.234(4)
_cell_measurement_reflns_used    2404
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.3
_cell_volume                     3135.1(13)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    ' ?'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.124
_diffrn_reflns_av_sigmaI/netI    0.164
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19956
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
A void volume of 410 A**3 containing 150 electrons was assigned to
15 solvent water molecules/unit cell. These are not included in the 
refinement model but are accounted for in the formula, formula weight,
density, mu and F(000).
;
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.61
_refine_diff_density_rms         0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.84
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         8960
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      0.85
_refine_ls_R_factor_all          0.139
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.089P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.156
_refine_ls_wR_factor_ref         0.175
_reflns_number_gt                4114
_reflns_number_total             8960
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic070169e_si_1.cif
_cod_data_source_block           cunscn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C51 H62 Cl6 Cu3 N7 O22.50 S4'
_cod_database_code               4308162