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_7223629
_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         'C42 H46 N4 O8 S2'
_chemical_formula_sum            'C42 H46 N4 O8 S2'
_chemical_formula_weight         798.95
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                111.715(8)
_cell_angle_beta                 95.652(8)
_cell_angle_gamma                94.106(8)
_cell_formula_units_Z            2
_cell_length_a                   12.0266(19)
_cell_length_b                   13.158(2)
_cell_length_c                   16.691(3)
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.50
_cell_volume                     2425.2(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            73045
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.649
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       prism
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
;
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0734P)^2^+1.2890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7792
_reflns_number_total             9863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra23217a2.cif
_cod_data_source_block           T90-comp1
_cod_original_cell_volume        2425.1(7)
_cod_database_code               7223629
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              39300