Synthesis and structural characterization, by spectroscopic and computational methods, of two fluorescent 3-hydroxy-4-pyridinone chelators bearing sulphorhodamine B and naphthalene
Rangel, Maria; Moniz, Tania; Coimbra, João T. S.; Bras, Natercia Fernandes; Cunha-Silva, Luis; Ramos, Maria Joao; Fernandes, Pedro Alexandrino; de Castro, Baltazar; RSC Adv.  (2015) –; doi:10.1039/C5RA23217A

data_7223630
_publ_section_title
;
 Synthesis and structural characterization, by spectroscopic and
 computational methods, of two fluorescent 3-hydroxy-4-pyridinone
 chelators bearing sulphorhodamine B and naphthalene
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA23217A
_journal_year                    2015
_chemical_formula_moiety         'C35 H41 N4 O8 S2, Cl, 5(H2 O)'
_chemical_formula_sum            'C35 H51 Cl N4 O13 S2'
_chemical_formula_weight         835.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             '02 November 2015'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_audit_update_record
;
2015-11-02 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                77.945(4)
_cell_angle_beta                 87.615(4)
_cell_angle_gamma                86.940(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5844(6)
_cell_length_b                   12.4376(9)
_cell_length_c                   19.9706(14)
_cell_measurement_reflns_used    7284
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.85
_cell_volume                     2081.2(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.713
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       prism
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+3.4986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5286
_reflns_number_total             7259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra23217a2.cif
_cod_data_source_block           T93-comp2
_cod_database_code               7223630
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              48339